#------------------------------------------------------------------------------ #$Date: 2021-07-29 04:49:56 +0300 (Thu, 29 Jul 2021) $ #$Revision: 267793 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/42/1564258.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1564258 loop_ _publ_author_name 'Jia, Xiangqing' 'Nitsch, J\"orn' 'Wu, Zhu' 'Friedrich, Alexandra' 'Krebs, Johannes' 'Krummenacher, Ivo' 'Fantuzzi, Felipe' 'Braunschweig, Holger' 'Moos, Michael' 'Lambert, Christoph' 'Engels, Bernd' 'Marder, Todd B.' _publ_section_title ; One- and Two-Electron Reduction of Triarylborane-Based Helical Donor-Acceptor Compounds ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC02409D _journal_year 2021 _chemical_formula_moiety 'C50 H46 B N, C12 H24 K O6, 3(C4 H8 O)' _chemical_formula_sum 'C74 H94 B K N O9' _chemical_formula_weight 1191.41 _chemical_name_systematic '10-(dimesitylboryl)-N,N-di-p-tolylbenzo[c]phenanthren-4-amine (3-B(Mes)2-[4]helix-9-N(p-Tol)2) monoanion' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-09-30 _audit_creation_method ; Olex2 1.2-ac3 (compiled 2017.03.02 svn.r3394 for Rigaku Oxford Diffraction, GUI svn.r5318) ; _audit_update_record ; 2020-11-13 deposited with the CCDC. 2021-07-27 downloaded from the CCDC. ; _cell_angle_alpha 98.375(2) _cell_angle_beta 90.741(2) _cell_angle_gamma 103.958(2) _cell_formula_units_Z 2 _cell_length_a 12.5786(3) _cell_length_b 16.3020(4) _cell_length_c 16.8804(3) _cell_measurement_reflns_used 24252 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 70.0680 _cell_measurement_theta_min 2.6500 _cell_volume 3319.24(13) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -20.00 57.00 0.50 7.00 -- 50.30 -52.00 -9.00 154 2 \w 4.00 47.00 0.50 7.00 -- 50.30 0.00 -30.00 86 3 \w 97.00 123.00 0.50 27.00 -- 105.75 61.00 60.00 52 4 \w 132.00 170.00 0.50 27.00 -- 105.75 61.00 60.00 76 5 \w 136.00 178.00 0.50 27.00 -- 105.75 52.00 136.00 84 6 \w 114.00 173.00 0.50 27.00 -- 105.75 15.00 60.00 118 7 \w 96.00 123.00 0.50 27.00 -- 105.75 52.00 136.00 54 8 \w 74.00 104.00 0.50 27.00 -- 105.75 0.00 90.00 60 9 \w 46.00 105.00 0.50 7.00 -- 50.30 52.00 136.00 118 10 \w 34.00 70.00 0.50 27.00 -- 105.75 -61.00 0.00 72 11 \w 36.00 108.00 0.50 27.00 -- 105.75-109.00 14.08 144 12 \w 50.00 116.00 0.50 27.00 -- 105.75-131.00 95.07 132 13 \w 47.00 122.00 0.50 27.00 -- 105.75-140.00 -8.93 150 14 \w 83.00 108.00 0.50 27.00 -- 105.75-111.00-123.03 50 15 \w 40.00 111.00 0.50 27.00 -- 105.75-125.00-120.00 142 16 \w 44.00 85.00 0.50 27.00 -- 105.75 -94.00 -90.00 82 17 \w 35.00 111.00 0.50 27.00 -- 105.75-125.00 0.00 152 18 \w 45.00 71.00 0.50 27.00 -- 105.75 -61.00 120.00 52 19 \w 40.00 106.00 0.50 27.00 -- 105.75 -77.00 90.00 132 20 \w 38.00 108.00 0.50 27.00 -- 105.75-107.00 103.59 140 21 \w 68.00 107.00 0.50 27.00 -- 105.75 0.00 -60.00 78 22 \w 105.00 177.00 0.50 27.00 -- 105.75 30.00 -90.00 144 23 \w 57.00 93.00 0.50 27.00 -- 105.75 0.00 -90.00 72 24 \w 58.00 112.00 0.50 27.00 -- 105.75 0.00-150.00 108 25 \w 39.00 71.00 0.50 27.00 -- 105.75-111.00-123.03 64 26 \w 40.00 109.00 0.50 27.00 -- 105.75-114.00 -98.45 138 27 \w 35.00 110.00 0.50 27.00 -- 105.75-125.00-150.00 150 28 \w 16.00 57.00 0.50 7.00 -- 50.30 0.00-180.00 82 29 \w -23.00 20.00 0.50 7.00 -- -50.24 19.00-120.00 86 30 \w -68.00 -13.00 0.50 27.00 -- -84.25 61.00 -60.00 110 31 \w -118.00 -54.00 0.50 7.00 -- -50.24 -52.00 -9.00 128 32 \w -52.00 15.00 0.50 7.00 -- -50.24 52.00 136.00 134 33 \w -49.00 -12.00 0.50 27.00 -- -84.25 52.00 136.00 74 34 \w -121.00 -85.00 0.50 7.00 -- -50.24-125.00 -60.00 72 35 \w -150.00 -75.00 0.50 27.00 -- -84.25 -52.00 -9.00 150 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0183541000 _diffrn_orient_matrix_UB_12 -0.0828862000 _diffrn_orient_matrix_UB_13 -0.0608530000 _diffrn_orient_matrix_UB_21 0.1126616000 _diffrn_orient_matrix_UB_22 -0.0113889000 _diffrn_orient_matrix_UB_23 0.0262247000 _diffrn_orient_matrix_UB_31 -0.0541958000 _diffrn_orient_matrix_UB_32 -0.0520631000 _diffrn_orient_matrix_UB_33 0.0643430000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_unetI/netI 0.0339 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 42082 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.058 _diffrn_reflns_theta_min 2.649 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.149 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.68341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.192 _exptl_crystal_description block _exptl_crystal_F_000 1282 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Tetrahydrofuran' _exptl_crystal_size_max 0.245 _exptl_crystal_size_mid 0.184 _exptl_crystal_size_min 0.056 _refine_diff_density_max 0.741 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.053 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 935 _refine_ls_number_reflns 12455 _refine_ls_number_restraints 586 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0601 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+1.2153P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1716 _refine_ls_wR_factor_ref 0.1818 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10489 _reflns_number_total 12455 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 17.5012\% around [-0.77 -0.50 0.40] (reciprocal) or [-0.89 -0.44 0.15] (direct) ; _cod_data_source_file d1sc02409d2.cif _cod_data_source_block cmpd_1K1 _cod_database_code 1564258 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_usercomment jxq2-27 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.938 _shelx_estimated_absorpt_t_min 0.766 _diffrn_oxdiff_digest_frames ; 019ff81479cd11082f70f10a9a0a2d755103640fffd ; _diffrn_oxdiff_digest_hkl ; 014178addd1f89adc334aefbc36ee7820fde05 ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C9B_1-C10B_1 = C7B_1-C8B_1 = C9A_1-C10A_1 = C7A_1-C8A_1 = C8A_1-C9A_1 = C8B_1- C9B_1 1.52 with sigma of 0.01 O4A_1-C7A_1 = O4A_1-C10A_1 = O4B_1-C7B_1 = O4B_1-C10B_1 1.43 with sigma of 0.01 O4A_1-C8A_1 = O4A_1-C9A_1 = O4B_1-C8B_1 = O4B_1-C9B_1 2.37 with sigma of 0.01 C7A_1-C10A_1 = C7B_1-C10B_1 2.33 with sigma of 0.01 C8A_1-C10A_1 = C7A_1-C9A_1 = C7B_1-C9B_1 = C8B_1-C10B_1 2.36 with sigma of 0.01 C1A_3-C2A_3 = C2A_3-C3A_3 = C3A_3-C4A_3 1.52 with sigma of 0.01 C3A_3-O1A_3 = O1A_3-C2A_3 2.37 with sigma of 0.01 C1A_3-C3A_3 = C2A_3-C4A_3 2.36 with sigma of 0.01 C1A_3-O1A_3 = O1A_3-C4A_3 1.43 with sigma of 0.01 C1A_3-C4A_3 2.33 with sigma of 0.01 C3B_3-C5B_3 = C4B_3-C1B_3 2.36 with sigma of 0.01 O2B_3-C4B_3 = O2B_3-C5B_3 2.37 with sigma of 0.01 C1B_3-O2B_3 = O2B_3-C3B_3 1.43 with sigma of 0.01 C3B_3-C4B_3 = C4B_3-C5B_3 = C5B_3-C1B_3 1.52 with sigma of 0.01 C1B_3-C3B_3 2.33 with sigma of 0.01 O1C_3-C2C_3 = C5C_3-O1C_3 1.43 with sigma of 0.01 C2C_3-C3C_3 = C3C_3-C4C_3 = C4C_3-C5C_3 1.52 with sigma of 0.01 O1C_3-C3C_3 = C4C_3-O1C_3 2.37 with sigma of 0.01 C2C_3-C4C_3 = C3C_3-C5C_3 = C2C_3-C5C_3 2.36 with sigma of 0.01 C2C_3-C5C_3 2.33 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints O4A_1 \\sim C7A_1 \\sim C8A_1 \\sim C9A_1 \\sim C10A_1 \\sim O4B_1 \\sim C8B_1 \\sim C7B_1 \\sim C9B_1 \\sim C10B_1: within 2A with sigma of 0.003 and sigma for terminal atoms of 0.006 C9A_2 \\sim C9B_2: within 2A with sigma of 0.003 and sigma for terminal atoms of 0.006 C1A_3 \\sim C2A_3 \\sim O1A_3 \\sim C4A_3 \\sim C3A_3 \\sim C5B_3 \\sim C1B_3 \\sim O2B_3 \\sim C3B_3 \\sim C4B_3 \\sim C4C_3 \\sim O1C_3 \\sim C2C_3 \\sim C3C_3 \\sim C5C_3: within 2A with sigma of 0.008 and sigma for terminal atoms of 0.016 4. Others 1*[Sof(C1A)+Sof(H1AA)+Sof(H1AB)+Sof(C2A)+Sof(H2AA)+Sof(H2AB)+Sof(O1A)+ Sof(C4A)+Sof(H4A1)+Sof(H4A2)+Sof(C3A)+Sof(H3A1)+Sof(H3A2)]+1*[Sof(C5B)+ Sof(H5B1)+Sof(H5B2)+Sof(C1B)+Sof(H1BA)+Sof(H1BB)+Sof(O2B)+Sof(C3B)+Sof(H3BA)+ Sof(H3BB)+Sof(C4B)+Sof(H4B1)+Sof(H4B2)]+1*[Sof(C4C)+Sof(H4CA)+Sof(H4CB)+ Sof(O1C)+Sof(C2C)+Sof(H2CA)+Sof(H2CB)+Sof(C3C)+Sof(H3CA)+Sof(H3CB)+Sof(C5C)+ Sof(H5CA)+Sof(H5CB)]=1 with esd of 0.0001 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(O1A)=Sof(C4A)= Sof(H4A1)=Sof(H4A2)=Sof(C3A)=Sof(H3A1)=Sof(H3A2)=FVAR(1) Sof(C5B)=Sof(H5B1)=Sof(H5B2)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(O2B)=Sof(C3B)= Sof(H3BA)=Sof(H3BB)=Sof(C4B)=Sof(H4B1)=Sof(H4B2)=FVAR(2) Sof(C4C)=Sof(H4CA)=Sof(H4CB)=Sof(O1C)=Sof(C2C)=Sof(H2CA)=Sof(H2CB)=Sof(C3C)= Sof(H3CA)=Sof(H3CB)=Sof(C5C)=Sof(H5CA)=Sof(H5CB)=FVAR(3) Sof(C9B)=Sof(H9BA)=Sof(H9BB)=1-FVAR(4) Sof(C9A)=Sof(H9AA)=Sof(H9AB)=FVAR(4) Sof(O4B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(C9B)= Sof(H9BA)=Sof(H9BB)=Sof(C10B)=Sof(H10C)=Sof(H10D)=1-FVAR(5) Sof(O4A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)= Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(H10B)=FVAR(5) 5.a Secondary CH2 refined with riding coordinates: C1(H1A,H1AB), C2(H2A,H2AB), C3(H3A,H3AB), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10A,H10B), C8B(H8BA,H8BB), C7B(H7BA,H7BB), C9B(H9BA, H9BB), C10B(H10C,H10D), C5(H5A,H5AB), C6(H6A,H6AB), C4(H4A,H4AB), C1(H1A,H1AB), C2(H2A,H2AB), C3(H3A,H3AB), C5(H5A,H5AB), C6(H6A,H6AB), C7(H7A,H7AB), C9A(H9AA,H9AB), C9B(H9BA,H9BB), C4(H4A,H4AB), C1A(H1AA,H1AB), C2A(H2AA,H2AB), C4A(H4A1,H4A2), C3A(H3A1,H3A2), C5B(H5B1,H5B2), C1B(H1BA,H1BB), C3B(H3BA,H3BB), C4B(H4B1,H4B2), C4C(H4CA,H4CB), C2C(H2CA,H2CB), C3C(H3CA,H3CB), C5C(H5CA,H5CB) 5.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6), C9(H9), C10(H10), C24(H24), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18), C22(H22), C21(H21), C25(H25), C27(H27), C29(H29), C30(H30), C37(H37), C35(H35), C46(H46), C44(H44) 5.c Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C39(H39A,H39B,H39C), C50(H50A,H50B, H50C), C49(H49A,H49B,H49C), C48(H48A,H48B,H48C), C41(H41A,H41B,H41C), C40(H40A, H40B,H40C) ; _shelx_res_file ; TITL AF287_twin_jet_smart_smallcell_twin1_hklf4_a.res in P-1 AF287_twin_jet_smart_smallcell_twin1_hklf4_a.res created by SHELXL-2018/3 at 11:35:00 on 30-Sep-2019 REM Old TITL AF287_twin_jet_smart_smallcell_twin1_hklf4 in P-1 REM SHELXT solution in P-1 REM R1 0.213, Rweak 0.010, Alpha 0.049, Orientation as input REM Formula found by SHELXT: C76 N5 O4 CELL 1.54184 12.5786 16.3020 16.8804 98.375 90.741 103.958 ZERR 2.000 0.0003 0.0004 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H B N O K UNIT 148 188 2 2 18 2 TEMP -173 SIZE 0.056 0.184 0.245 L.S. 10 SHEL 999. 0.82 BOND $H ACTA CONF LIST 4 FMAP 2 PLAN 20 OMIT 0 -4 1 SUMP 1.0 0.0001 1.0 2 1.0 3 1.0 4 WGHT 0.105000 1.215300 FVAR 0.44064 0.37454 0.48175 0.14370 0.40065 0.79302 C1 1 0.970995 0.373769 0.293176 11.00000 0.03702 0.03869 = 0.04951 0.01368 -0.00368 0.01072 N1 4 1.005699 0.434354 0.242243 11.00000 0.03068 0.04485 = 0.06300 0.02526 0.00578 0.01754 B1 3 0.480753 0.851279 0.216478 11.00000 0.03591 0.04224 = 0.03674 0.01436 0.00435 0.01662 C2 1 0.864096 0.353444 0.316371 11.00000 0.04290 0.07517 = 0.06788 0.03867 0.00810 0.02014 AFIX 43 H2 2 0.812570 0.381116 0.297509 11.00000 -1.20000 AFIX 0 C23 1 0.920783 0.726038 0.323668 11.00000 0.02810 0.04480 = 0.04520 0.01662 -0.00040 0.01015 C3 1 0.831189 0.293236 0.366769 11.00000 0.05699 0.10136 = 0.08627 0.05665 0.01591 0.01685 AFIX 43 H3 2 0.757421 0.281279 0.382384 11.00000 -1.20000 AFIX 0 C4 1 0.901900 0.249835 0.395223 11.00000 0.07960 0.05624 = 0.05096 0.02446 -0.00879 0.00553 C5 1 1.008634 0.271897 0.373410 11.00000 0.06855 0.04159 = 0.06144 0.01477 -0.02217 0.01128 AFIX 43 H5 2 1.059813 0.244313 0.392927 11.00000 -1.20000 AFIX 0 C6 1 1.044450 0.332612 0.324213 11.00000 0.04424 0.04485 = 0.07276 0.02265 -0.01035 0.01172 AFIX 43 H6 2 1.119316 0.346600 0.311302 11.00000 -1.20000 AFIX 0 C7 1 0.859872 0.179653 0.445211 11.00000 0.12693 0.07815 = 0.06626 0.04112 -0.00848 0.00049 AFIX 137 H7A 2 0.921913 0.167975 0.473416 11.00000 -1.50000 H7B 2 0.820336 0.127603 0.410132 11.00000 -1.50000 H7C 2 0.810217 0.198045 0.484378 11.00000 -1.50000 AFIX 0 C8 1 1.097409 0.433005 0.192920 11.00000 0.03031 0.04843 = 0.06320 0.02626 0.00504 0.01828 C9 1 1.110721 0.358250 0.147837 11.00000 0.03685 0.04775 = 0.08139 0.02372 0.00962 0.01844 AFIX 43 H9 2 1.060307 0.305262 0.151201 11.00000 -1.20000 AFIX 0 C19 1 0.843176 0.598535 0.224116 11.00000 0.02366 0.03971 = 0.04501 0.01857 0.00471 0.01107 C10 1 1.198082 0.360977 0.097639 11.00000 0.04611 0.06505 = 0.07927 0.02482 0.01347 0.03279 AFIX 43 H10 2 1.206699 0.309447 0.067092 11.00000 -1.20000 AFIX 0 C24 1 0.930726 0.814200 0.352753 11.00000 0.03648 0.04384 = 0.05013 0.01196 -0.01030 0.00564 AFIX 43 H24 2 0.990667 0.844723 0.388644 11.00000 -1.20000 AFIX 0 C11 1 1.272837 0.437513 0.091350 11.00000 0.03760 0.08087 = 0.07167 0.04162 0.00986 0.03188 C12 1 1.258178 0.512062 0.136453 11.00000 0.03229 0.06477 = 0.07692 0.04221 0.00293 0.01347 AFIX 43 H12 2 1.308240 0.565104 0.132707 11.00000 -1.20000 AFIX 0 C13 1 1.171569 0.510277 0.186891 11.00000 0.03716 0.04983 = 0.06498 0.02691 0.00304 0.01593 AFIX 43 H13 2 1.162884 0.561840 0.217333 11.00000 -1.20000 AFIX 0 C14 1 1.369454 0.440478 0.038515 11.00000 0.04458 0.11640 = 0.08357 0.05605 0.02058 0.04172 AFIX 137 H14A 2 1.378940 0.489751 0.009931 11.00000 -1.50000 H14B 2 1.356055 0.387762 -0.000351 11.00000 -1.50000 H14C 2 1.435977 0.445843 0.071726 11.00000 -1.50000 AFIX 0 C15 1 0.927920 0.476900 0.213180 11.00000 0.02785 0.04349 = 0.05327 0.02195 0.00696 0.01448 C16 1 0.869182 0.441350 0.142123 11.00000 0.03456 0.03916 = 0.05660 0.01488 0.00780 0.01550 AFIX 43 H16 2 0.874363 0.386915 0.115842 11.00000 -1.20000 AFIX 0 C17 1 0.801758 0.485406 0.108537 11.00000 0.03234 0.04350 = 0.04877 0.01189 0.00137 0.01335 AFIX 43 H17 2 0.764298 0.462470 0.057954 11.00000 -1.20000 AFIX 0 C18 1 0.789810 0.562082 0.148953 11.00000 0.02678 0.04018 = 0.04721 0.01622 0.00387 0.01352 AFIX 43 H18 2 0.743972 0.591373 0.125286 11.00000 -1.20000 AFIX 0 C20 1 0.918972 0.556236 0.255294 11.00000 0.02695 0.04225 = 0.04532 0.01938 0.00489 0.01267 C22 1 0.994016 0.681713 0.352704 11.00000 0.02703 0.04983 = 0.04552 0.01910 -0.00168 0.00939 AFIX 43 H22 2 1.047563 0.711017 0.393955 11.00000 -1.20000 AFIX 0 C21 1 0.989792 0.598779 0.323297 11.00000 0.02749 0.05178 = 0.04747 0.02381 0.00297 0.01508 AFIX 43 H21 2 1.034069 0.569070 0.348056 11.00000 -1.20000 AFIX 0 C26 1 0.759446 0.810133 0.281849 11.00000 0.03514 0.03804 = 0.04332 0.01182 -0.00308 0.01067 C25 1 0.856445 0.855474 0.330295 11.00000 0.04398 0.03559 = 0.05235 0.00900 -0.00934 0.00881 AFIX 43 H25 2 0.868700 0.915385 0.346854 11.00000 -1.20000 AFIX 0 C28 1 0.574873 0.808246 0.226346 11.00000 0.03296 0.03968 = 0.03847 0.01327 0.00170 0.01452 C27 1 0.677409 0.850947 0.266708 11.00000 0.03936 0.03547 = 0.04298 0.00907 -0.00281 0.01400 AFIX 43 H27 2 0.690898 0.910747 0.284413 11.00000 -1.20000 AFIX 0 C29 1 0.562685 0.718423 0.201949 11.00000 0.02716 0.04010 = 0.03986 0.01119 0.00096 0.01093 AFIX 43 H29 2 0.494780 0.685648 0.176551 11.00000 -1.20000 AFIX 0 C30 1 0.642957 0.677006 0.213027 11.00000 0.02855 0.03370 = 0.04098 0.00983 0.00155 0.01017 AFIX 43 H30 2 0.629025 0.617344 0.194452 11.00000 -1.20000 AFIX 0 C32 1 0.834565 0.681424 0.266137 11.00000 0.02664 0.03749 = 0.04201 0.01505 0.00148 0.00899 C31 1 0.747384 0.720813 0.251772 11.00000 0.03008 0.03709 = 0.03915 0.01327 0.00125 0.01190 C34 1 0.486679 1.012209 0.206146 11.00000 0.03465 0.04477 = 0.04118 0.01380 0.00275 0.01792 C33 1 0.493944 0.949014 0.254697 11.00000 0.03626 0.04488 = 0.03973 0.01184 0.00300 0.01930 C37 1 0.528244 1.064446 0.368796 11.00000 0.06636 0.05441 = 0.03837 0.00673 0.00061 0.02704 AFIX 43 H37 2 0.543396 1.081891 0.424823 11.00000 -1.20000 AFIX 0 C36 1 0.520400 1.125771 0.321456 11.00000 0.05443 0.04541 = 0.04753 0.00903 0.00391 0.02238 C35 1 0.500137 1.097426 0.239745 11.00000 0.04326 0.04287 = 0.04661 0.01534 0.00265 0.01939 AFIX 43 H35 2 0.495278 1.137840 0.205452 11.00000 -1.20000 AFIX 0 C39 1 0.519081 0.918780 0.397679 11.00000 0.08445 0.05815 = 0.03908 0.01301 -0.00040 0.03530 AFIX 137 H39A 2 0.584744 0.942005 0.433484 11.00000 -1.50000 H39B 2 0.521631 0.862521 0.369118 11.00000 -1.50000 H39C 2 0.453588 0.913057 0.429264 11.00000 -1.50000 AFIX 0 C38 1 0.514882 0.978594 0.337755 11.00000 0.05421 0.04986 = 0.04097 0.01308 0.00156 0.02468 C50 1 0.267474 0.818957 0.299431 11.00000 0.04380 0.06255 = 0.04542 0.01934 0.01139 0.02414 AFIX 137 H50A 2 0.297118 0.881041 0.305624 11.00000 -1.50000 H50B 2 0.312057 0.794290 0.332814 11.00000 -1.50000 H50C 2 0.191672 0.806431 0.316159 11.00000 -1.50000 AFIX 0 C49 1 0.059103 0.633529 0.057452 11.00000 0.03127 0.04964 = 0.06389 0.01814 0.00635 0.00849 AFIX 137 H49A 2 0.002218 0.629704 0.096823 11.00000 -1.50000 H49B 2 0.070160 0.576417 0.039322 11.00000 -1.50000 H49C 2 0.036156 0.656711 0.011487 11.00000 -1.50000 AFIX 0 C48 1 0.457477 0.771804 0.037027 11.00000 0.03205 0.04680 = 0.04319 0.00780 0.00572 0.01097 AFIX 137 H48A 2 0.523432 0.803638 0.069798 11.00000 -1.50000 H48B 2 0.444985 0.803904 -0.005513 11.00000 -1.50000 H48C 2 0.467350 0.715840 0.013002 11.00000 -1.50000 AFIX 0 C47 1 0.359588 0.759485 0.089258 11.00000 0.03092 0.03571 = 0.04514 0.01496 0.00570 0.01458 C46 1 0.259878 0.709855 0.052896 11.00000 0.03230 0.03664 = 0.04518 0.01362 0.00429 0.01254 AFIX 43 H46 2 0.256500 0.687760 -0.002603 11.00000 -1.20000 AFIX 0 C45 1 0.165314 0.691836 0.095636 11.00000 0.03045 0.03861 = 0.05452 0.02053 0.00529 0.01401 C44 1 0.172815 0.728254 0.175591 11.00000 0.03164 0.04409 = 0.05193 0.02454 0.01098 0.01728 AFIX 43 H44 2 0.109447 0.717081 0.206146 11.00000 -1.20000 AFIX 0 C43 1 0.269902 0.780591 0.212639 11.00000 0.03636 0.04240 = 0.04359 0.02035 0.00868 0.02142 C42 1 0.368033 0.796565 0.170713 11.00000 0.03185 0.03719 = 0.04300 0.01616 0.00435 0.01829 C41 1 0.468428 0.988166 0.116476 11.00000 0.04567 0.04377 = 0.04266 0.01424 0.00139 0.01539 AFIX 137 H41A 2 0.470220 1.039603 0.092334 11.00000 -1.50000 H41B 2 0.396878 0.947560 0.103775 11.00000 -1.50000 H41C 2 0.526320 0.961702 0.095023 11.00000 -1.50000 AFIX 0 C40 1 0.529958 1.217844 0.357438 11.00000 0.07845 0.04897 = 0.05487 0.00544 0.00256 0.02425 AFIX 137 H40A 2 0.576433 1.255673 0.324734 11.00000 -1.50000 H40B 2 0.562761 1.228453 0.412086 11.00000 -1.50000 H40C 2 0.456879 1.229141 0.358837 11.00000 -1.50000 AFIX 0 RESI 1 CATI K1 6 1.000000 1.000000 0.000000 10.50000 0.03282 0.05073 = 0.09191 0.03991 0.01586 0.01649 C1 1 0.732995 0.851103 -0.022273 11.00000 0.03367 0.05097 = 0.10921 0.02985 0.01734 0.01159 AFIX 23 H1A 2 0.702163 0.893622 0.011745 11.00000 -1.20000 H1AB 2 0.681703 0.794136 -0.024547 11.00000 -1.20000 AFIX 0 O2 5 1.008365 0.914666 0.131076 11.00000 0.04384 0.05425 = 0.10198 0.04376 0.01331 0.01973 C2 1 0.831179 0.827348 0.089037 11.00000 0.05106 0.05604 = 0.08667 0.03689 0.02542 0.00846 AFIX 23 H2A 2 0.782446 0.769463 0.087451 11.00000 -1.20000 H2AB 2 0.800682 0.868327 0.125378 11.00000 -1.20000 AFIX 0 O3 5 1.193542 1.039985 0.098906 11.00000 0.03958 0.05719 = 0.10734 0.04046 0.00554 0.01366 C3 1 0.944469 0.828797 0.119110 11.00000 0.05821 0.05219 = 0.08756 0.04208 0.02285 0.01968 AFIX 23 H3A 2 0.940957 0.805398 0.170205 11.00000 -1.20000 H3AB 2 0.978323 0.793061 0.079564 11.00000 -1.20000 AFIX 0 SIMU_1 0.003 O4A > C10B DFIX_1 1.52 0.01 C9B C10B C7B C8B C9A C10A C7A C8A C8A C9A C8B C9B DFIX_1 1.43 0.01 O4A C7A O4A C10A O4B C7B O4B C10B DFIX_1 2.37 0.01 O4A C8A O4A C9A O4B C8B O4B C9B DFIX_1 2.33 0.01 C7A C10A C7B C10B DFIX_1 2.36 0.01 C8A C10A C7A C9A C7B C9B C8B C10B PART 1 61. O4A 5 0.920663 1.110723 0.109112 61.00000 0.05838 0.08183 = 0.09295 0.02882 0.01952 0.02967 C7A 1 0.843407 1.149808 0.077300 61.00000 0.06187 0.08235 = 0.09328 0.03256 0.01525 0.02934 AFIX 23 H7AA 2 0.805914 1.113679 0.027794 61.00000 -1.20000 H7AB 2 0.881200 1.206406 0.063929 61.00000 -1.20000 AFIX 0 C8A 1 0.763611 1.159596 0.137872 61.00000 0.05991 0.08767 = 0.09179 0.02925 0.01220 0.02872 AFIX 23 H8AA 2 0.689039 1.149600 0.112904 61.00000 -1.20000 H8AB 2 0.783852 1.217328 0.170239 61.00000 -1.20000 AFIX 0 C9A 1 0.770386 1.088454 0.190668 61.00000 0.05578 0.08488 = 0.08416 0.02883 0.01071 0.02827 AFIX 23 H9AA 2 0.747422 1.102683 0.245812 61.00000 -1.20000 H9AB 2 0.725769 1.031466 0.166115 61.00000 -1.20000 AFIX 0 C10A 1 0.890005 1.092999 0.189208 61.00000 0.05907 0.08353 = 0.08485 0.02484 0.00973 0.02651 AFIX 23 H10A 2 0.931469 1.139261 0.230793 61.00000 -1.20000 H10B 2 0.904736 1.038136 0.198625 61.00000 -1.20000 AFIX 0 PART 2 -61. O4B 5 0.873071 1.071217 0.086100 -61.00000 0.06092 0.08276 = 0.08894 0.02823 0.01314 0.02981 C8B 1 0.736363 1.137818 0.130867 -61.00000 0.05964 0.08579 = 0.09044 0.03019 0.01160 0.02688 AFIX 23 H8BA 2 0.665391 1.094453 0.122260 -61.00000 -1.20000 H8BB 2 0.721994 1.195461 0.137441 -61.00000 -1.20000 AFIX 0 C7B 1 0.807635 1.126260 0.062093 -61.00000 0.06009 0.08406 = 0.09098 0.02974 0.01309 0.02965 AFIX 23 H7BA 2 0.762795 1.099000 0.012300 -61.00000 -1.20000 H7BB 2 0.854874 1.181882 0.053175 -61.00000 -1.20000 AFIX 0 C9B 1 0.799270 1.126925 0.203191 -61.00000 0.05877 0.08540 = 0.08735 0.02771 0.01135 0.02782 AFIX 23 H9BA 2 0.755461 1.081199 0.230488 -61.00000 -1.20000 H9BB 2 0.818967 1.180828 0.241676 -61.00000 -1.20000 AFIX 0 C10B 1 0.901625 1.102782 0.170893 -61.00000 0.05935 0.08384 = 0.08755 0.02750 0.01051 0.02836 AFIX 23 H10C 2 0.965166 1.153173 0.177982 -61.00000 -1.20000 H10D 2 0.919530 1.057793 0.198385 -61.00000 -1.20000 AFIX 0 PART 0 C5 1 1.176779 1.013585 0.175325 11.00000 0.04704 0.07202 = 0.11231 0.04978 0.00024 0.01891 AFIX 23 H5A 2 1.134649 1.049187 0.207718 11.00000 -1.20000 H5AB 2 1.248381 1.020919 0.204027 11.00000 -1.20000 AFIX 0 C6 1 1.253097 1.126335 0.104219 11.00000 0.04013 0.05448 = 0.11199 0.03699 0.00198 0.01258 AFIX 23 H6A 2 1.325830 1.134398 0.131520 11.00000 -1.20000 H6AB 2 1.213107 1.164133 0.135959 11.00000 -1.20000 AFIX 0 C4 1 1.115398 0.922092 0.164548 11.00000 0.04643 0.07136 = 0.11814 0.05415 0.00868 0.02531 AFIX 23 H4A 2 1.154306 0.887033 0.128371 11.00000 -1.20000 H4AB 2 1.110236 0.901183 0.216906 11.00000 -1.20000 AFIX 0 O1 5 0.837226 0.850152 0.010860 11.00000 0.03721 0.05368 = 0.08681 0.03480 0.01891 0.01342 RESI 0 RESI 2 CATI K1 6 0.500000 0.500000 0.500000 10.50000 0.04348 0.07662 = 0.05027 0.03463 0.01113 0.02814 C1 1 0.782954 0.483023 0.527113 11.00000 0.04528 0.08853 = 0.06246 0.02435 0.00892 0.03599 AFIX 23 H1A 2 0.861541 0.507107 0.543241 11.00000 -1.20000 H1AB 2 0.777580 0.446782 0.474081 11.00000 -1.20000 AFIX 0 O2 5 0.613100 0.635460 0.431694 11.00000 0.05026 0.06072 = 0.05004 0.02190 0.00587 0.02138 C2 1 0.781064 0.606222 0.468885 11.00000 0.04608 0.07469 = 0.04293 0.01763 0.00650 0.01804 AFIX 23 H2A 2 0.780186 0.573536 0.414541 11.00000 -1.20000 H2AB 2 0.858345 0.632930 0.487347 11.00000 -1.20000 AFIX 0 O3 5 0.381807 0.609707 0.440509 11.00000 0.05180 0.07552 = 0.04698 0.02395 0.00608 0.03187 C3 1 0.719737 0.673535 0.466689 11.00000 0.05617 0.06986 = 0.04116 0.01524 0.00644 0.01816 AFIX 23 H3A 2 0.714758 0.702509 0.521795 11.00000 -1.20000 H3AB 2 0.758999 0.716890 0.434910 11.00000 -1.20000 AFIX 0 O4 5 0.484180 0.427269 0.340417 11.00000 0.05393 0.06556 = 0.06199 0.01473 0.00792 0.01459 C5 1 0.443435 0.651390 0.381480 11.00000 0.06258 0.06103 = 0.04731 0.02295 0.00601 0.03223 AFIX 23 H5A 2 0.405919 0.692586 0.363077 11.00000 -1.20000 H5AB 2 0.449432 0.608740 0.334677 11.00000 -1.20000 AFIX 0 C6 1 0.272045 0.569343 0.412331 11.00000 0.04865 0.08492 = 0.06121 0.02704 0.00219 0.03703 AFIX 23 H6A 2 0.271626 0.532169 0.360371 11.00000 -1.20000 H6AB 2 0.232074 0.613085 0.404160 11.00000 -1.20000 AFIX 0 C7 1 0.393942 0.386915 0.285212 11.00000 0.05279 0.08609 = 0.08425 0.01035 -0.00398 0.03412 AFIX 23 H7A 2 0.358927 0.430050 0.267878 11.00000 -1.20000 H7AB 2 0.338477 0.345850 0.310352 11.00000 -1.20000 AFIX 0 C8 1 0.438612 0.341549 0.215508 11.00000 0.05116 0.05842 = 0.06684 0.01767 -0.00249 0.01713 AFIX 23 H8A 2 0.387527 0.324683 0.167560 11.00000 -1.20000 H8AB 2 0.464012 0.291827 0.228319 11.00000 -1.20000 AFIX 0 C10 1 0.580807 0.444159 0.296332 11.00000 0.05480 0.05178 = 0.07556 0.01203 0.01298 0.00596 AFIX 23 H10A 2 0.630539 0.408205 0.307904 11.00000 -1.20000 H10B 2 0.620766 0.505181 0.307959 11.00000 -1.20000 AFIX 0 SIMU_2 0.003 C9A C9B PART 1 51. C9A 1 0.533124 0.419931 0.209550 51.00000 0.05596 0.07179 = 0.06464 0.01595 0.00867 0.01166 AFIX 23 H9AA 2 0.588050 0.405050 0.172257 51.00000 -1.20000 H9AB 2 0.505836 0.466801 0.191936 51.00000 -1.20000 AFIX 0 PART 2 -51. C9B 1 0.561996 0.386721 0.215737 -51.00000 0.05207 0.07529 = 0.06603 0.01808 0.00788 0.01593 AFIX 23 H9BA 2 0.608021 0.344999 0.211924 -51.00000 -1.20000 H9BB 2 0.577376 0.420475 0.171136 -51.00000 -1.20000 AFIX 0 PART 0 C4 1 0.555185 0.697366 0.416613 11.00000 0.06507 0.05495 = 0.04864 0.01593 0.00857 0.02919 AFIX 23 H4A 2 0.595107 0.733486 0.378855 11.00000 -1.20000 H4AB 2 0.549268 0.734818 0.467235 11.00000 -1.20000 AFIX 0 O1 5 0.730021 0.550374 0.522531 11.00000 0.04451 0.07935 = 0.04915 0.02624 0.01133 0.02991 RESI 0 RESI 3 THF SIMU_3 0.008 C1A > C5C DFIX_3 1.52 0.01 C1A C2A C2A C3A C3A C4A DFIX_3 2.37 0.01 C3A O1A O1A C2A DFIX_3 2.36 0.01 C1A C3A C2A C4A DFIX_3 1.43 0.01 C1A O1A O1A C4A DFIX_3 2.33 0.01 C1A C4A DFIX_3 2.36 0.01 C3B C5B C4B C1B DFIX_3 2.37 0.01 O2B C4B O2B C5B DFIX_3 1.43 0.01 C1B O2B O2B C3B DFIX_3 1.52 0.01 C3B C4B C4B C5B C5B C1B DFIX_3 2.33 0.01 C1B C3B DFIX_3 1.43 0.01 O1C C2C C5C O1C DFIX_3 1.52 0.01 C2C C3C C3C C4C C4C C5C DFIX_3 2.37 0.01 O1C C3C C4C O1C DFIX_3 2.36 0.01 C2C C4C C3C C5C C2C C5C DFIX_3 2.33 0.01 C2C C5C PART 1 21. C1A 1 1.070638 1.055087 0.371621 21.00000 0.07867 0.07232 = 0.09346 0.01795 -0.00978 0.02267 AFIX 23 H1AA 2 1.057376 1.003847 0.329891 21.00000 -1.20000 H1AB 2 1.009078 1.082728 0.368367 21.00000 -1.20000 AFIX 0 C2A 1 1.080938 1.030535 0.454228 21.00000 0.07471 0.07518 = 0.09807 0.01950 -0.01141 0.00961 AFIX 23 H2AA 2 1.026031 0.977296 0.460397 21.00000 -1.20000 H2AB 2 1.074327 1.076944 0.497323 21.00000 -1.20000 AFIX 0 O1A 5 1.169257 1.111564 0.361167 21.00000 0.07365 0.08210 = 0.08436 0.02298 -0.00352 0.02626 C4A 1 1.257544 1.083335 0.406528 21.00000 0.06043 0.05356 = 0.08537 0.01594 0.01098 0.01285 AFIX 23 H4A1 2 1.305850 1.060108 0.368243 21.00000 -1.20000 H4A2 2 1.303123 1.132640 0.443115 21.00000 -1.20000 AFIX 0 C3A 1 1.201012 1.017165 0.452474 21.00000 0.06543 0.06805 = 0.09367 0.02120 -0.01179 0.01177 AFIX 23 H3A1 2 1.234888 1.026049 0.507302 21.00000 -1.20000 H3A2 2 1.201648 0.959230 0.425291 21.00000 -1.20000 AFIX 0 PART 2 31. C5B 1 1.123269 0.975653 0.451111 31.00000 0.04889 0.05152 = 0.08699 0.03137 -0.00141 0.00566 AFIX 23 H5B1 2 1.088131 0.972862 0.503118 31.00000 -1.20000 H5B2 2 1.105102 0.917648 0.419246 31.00000 -1.20000 AFIX 0 C1B 1 1.085256 1.036933 0.406972 31.00000 0.06520 0.06747 = 0.08459 0.03003 -0.01722 0.01563 AFIX 23 H1BA 2 1.077232 1.015029 0.348792 31.00000 -1.20000 H1BB 2 1.013035 1.043688 0.425435 31.00000 -1.20000 AFIX 0 O2B 5 1.167190 1.120551 0.422312 31.00000 0.07858 0.07779 = 0.09702 0.02376 -0.02158 0.01836 C3B 1 1.261811 1.099872 0.460801 31.00000 0.07231 0.06345 = 0.10107 0.03390 -0.02742 0.01075 AFIX 23 H3BA 2 1.327982 1.117709 0.430314 31.00000 -1.20000 H3BB 2 1.276135 1.131760 0.515993 31.00000 -1.20000 AFIX 0 C4B 1 1.239701 1.007825 0.463373 31.00000 0.04713 0.04877 = 0.09060 0.01793 0.00087 0.01359 AFIX 23 H4B1 2 1.277968 0.979690 0.420704 31.00000 -1.20000 H4B2 2 1.264872 0.997294 0.515929 31.00000 -1.20000 AFIX 0 PART 3 41. C4C 1 1.237474 1.103141 0.373279 41.00000 0.06749 0.07230 = 0.09038 0.02450 -0.01306 0.02017 AFIX 23 H4CA 2 1.225533 1.133427 0.328470 41.00000 -1.20000 H4CB 2 1.317101 1.115705 0.387015 41.00000 -1.20000 AFIX 0 O1C 5 1.139047 0.977858 0.421944 41.00000 0.05888 0.05719 = 0.09416 0.02292 -0.00755 0.01148 C2C 1 1.166399 1.049297 0.487875 41.00000 0.06951 0.06930 = 0.09640 0.02087 -0.01017 0.01261 AFIX 23 H2CA 2 1.236988 1.051517 0.515768 41.00000 -1.20000 H2CB 2 1.108268 1.044763 0.527137 41.00000 -1.20000 AFIX 0 C3C 1 1.174636 1.128562 0.446198 41.00000 0.07342 0.07189 = 0.09515 0.02065 -0.01160 0.01377 AFIX 23 H3CA 2 1.101484 1.135283 0.430453 41.00000 -1.20000 H3CB 2 1.216407 1.181645 0.480038 41.00000 -1.20000 AFIX 0 C5C 1 1.189008 1.008437 0.352258 41.00000 0.05873 0.05759 = 0.08460 0.02444 -0.00707 0.02001 AFIX 23 H5CA 2 1.133408 0.996776 0.307350 41.00000 -1.20000 H5CB 2 1.247108 0.978953 0.335531 41.00000 -1.20000 PART 0 RESI 0 AFIX 0 HKLF 4 REM AF287_twin_jet_smart_smallcell_twin1_hklf4_a.res in P-1 REM wR2 = 0.1818, GooF = S = 1.056, Restrained GooF = 1.087 for all data REM R1 = 0.0601 for 10489 Fo > 4sig(Fo) and 0.0680 for all 12455 data REM 935 parameters refined using 586 restraints END WGHT 0.1050 1.2153 REM Highest difference peak 0.741, deepest hole -0.460, 1-sigma level 0.053 Q1 1 1.2791 1.0750 0.4235 11.00000 0.05 0.74 Q2 1 0.8152 1.0421 0.1621 11.00000 0.05 0.66 Q3 1 0.9675 0.9516 0.0223 11.00000 0.05 0.43 Q4 1 1.2213 1.0884 0.4791 11.00000 0.05 0.40 Q5 1 0.5389 0.5534 0.4796 11.00000 0.05 0.39 Q6 1 0.7510 1.1100 0.0986 11.00000 0.05 0.39 Q7 1 1.2393 1.1676 0.4014 11.00000 0.05 0.38 Q8 1 0.8766 1.1802 0.1209 11.00000 0.05 0.38 Q9 1 1.2237 1.0031 0.4259 11.00000 0.05 0.34 Q10 1 1.1272 1.0795 0.3633 11.00000 0.05 0.34 Q11 1 1.2847 0.9664 0.4611 11.00000 0.05 0.32 Q12 1 1.1744 1.1658 0.3728 11.00000 0.05 0.29 Q13 1 0.8203 1.0505 0.0836 11.00000 0.05 0.28 Q14 1 1.1374 0.9976 0.4668 11.00000 0.05 0.28 Q15 1 0.4138 0.2781 0.2239 11.00000 0.05 0.28 Q16 1 0.8370 0.6388 0.2478 11.00000 0.05 0.27 Q17 1 0.7668 0.7700 0.2548 11.00000 0.05 0.27 Q18 1 0.7469 0.7616 0.2829 11.00000 0.05 0.25 Q19 1 1.1428 0.9721 0.3932 11.00000 0.05 0.24 Q20 1 1.0827 1.0987 0.4415 11.00000 0.05 0.24 ; _shelx_res_checksum 42930 _shelx_hkl_file ; -5 -8 -3 0.51 1.30 0 -7 -13 0.36 1.17 -1 -9 -6 8.75 1.53 -3 -9 -10 1.50 1.44 1 -8 -8 6.99 1.31 -3 -8 -2 6.14 1.16 -6 -4 1 0.75 0.70 1 -8 -9 0.59 1.28 -5 -9 -6 14.41 1.63 -7 -3 1 -0.27 0.58 -8 -7 -5 -0.36 1.13 3 -5 -8 0.49 0.80 -7 -8 -6 1.40 1.27 2 -7 -9 5.06 1.15 -5 -9 -5 1.72 1.44 0 -9 -8 4.69 1.41 -5 -9 -7 5.01 1.51 -5 -2 2 0.46 0.54 -7 -6 -1 7.53 1.09 -6 -8 -3 43.35 1.71 -5 -8 -2 2.94 1.23 -2 -9 -11 -0.99 1.30 -5 -5 1 3.54 0.84 2 -6 -4 5.88 1.06 -7 -5 0 -0.22 0.78 -1 -9 -11 -1.14 1.28 -5 -7 -1 5.34 1.10 -6 -9 -7 7.36 1.40 0 -8 -12 0.04 1.21 -4 -9 -3 9.47 1.49 0 -9 -10 6.30 1.46 -6 -7 -1 -0.15 1.07 1 -8 -11 8.71 1.42 -2 -10 -7 -0.74 1.44 -2 -10 -6 2.42 1.50 1 -8 -6 3.87 1.14 -3 -10 -9 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6 -1 -7 6.79 0.98 5 -4 2 -0.18 1.23 7 -15 2 10.51 1.52 6 -2 -2 9.46 1.34 5 0 -6 1.88 0.88 9 -7 -7 8.14 1.57 10 -11 -4 4.55 1.58 9 -6 -4 7.51 1.46 6 -15 3 10.47 1.43 5 -7 4 6.89 1.21 7 -10 3 13.29 1.56 9 -10 0 1.98 1.58 9 -8 -1 7.23 1.56 7 -2 -6 8.42 1.13 6 -13 4 0.85 1.38 8 -4 -7 0.43 1.26 7 -2 -5 0.23 1.08 6 -5 2 10.23 1.41 5 -11 5 1.56 1.16 10 -8 -6 12.09 1.64 9 -5 -6 13.54 1.61 10 -10 -3 92.42 2.79 7 -5 0 0.60 1.31 10 -9 -4 16.92 1.89 9 -5 -5 1.45 1.43 9 -12 1 10.43 1.71 9 -6 -7 8.95 1.57 4 -11 5 11.02 1.20 9 -8 0 4.91 1.64 8 -3 -6 12.45 1.36 9 -13 1 7.78 1.64 8 -3 -7 14.26 1.37 5 -9 5 -0.73 1.05 10 -8 -3 1.70 1.60 10 -12 -1 1.07 1.51 7 -12 4 1.75 1.39 7 -10 4 12.81 1.50 5 -8 5 159.86 2.34 3 -6 5 698.97 3.52 10 -9 -6 3.11 1.48 7 -13 4 5.38 1.46 3 -10 6 51.24 1.45 9 -12 2 -0.65 1.41 9 -11 2 2.87 1.53 8 -9 3 1.35 1.36 10 -7 -3 7.55 1.68 8 -10 3 -0.68 1.43 1 -15 -2 22.88 1.79 5 -5 -9 142.12 2.87 3 -8 1 370.70 3.34 5 -11 -5 240.94 4.15 2 -12 1 67.27 2.09 2 -14 -1 50.27 2.23 3 -9 1 12.16 1.34 5 -6 -4 11.24 1.35 2 -15 -3 25.21 1.94 5 -5 -5 89.25 2.12 5 -8 -3 57.50 2.00 3 -7 1 31.13 1.43 2 -10 2 13.47 1.18 3 -3 -1 440.19 2.56 3 -10 1 32.28 1.55 5 -10 -4 124.36 2.93 5 -7 -3 1.21 1.23 5 -11 -9 29.09 2.17 5 -7 -11 3.20 1.56 3 -14 -2 39.32 2.19 4 -11 -1 30.46 1.85 4 -2 -5 30.67 1.33 5 -12 -5 26.17 2.22 1 -7 3 517.45 2.89 1 -15 -1 37.14 1.88 5 -6 -11 24.13 1.82 3 -13 -1 15.25 1.77 3 0 -6 23.01 0.90 4 -13 -3 25.97 2.08 5 -5 -4 54.77 1.85 5 -4 -9 154.69 2.64 4 -9 0 21.83 1.51 2 1 -5 858.52 2.18 4 -3 -3 212.96 2.23 4 -12 -2 90.70 2.72 4 -8 0 40.13 1.69 2 -6 2 13.03 0.93 5 -6 -3 273.98 3.19 3 -11 1 15.98 1.42 3 -4 0 129.44 1.56 2 -11 2 37.33 1.55 -1 -8 4 246.98 1.72 1 -10 3 14.56 1.08 4 -14 -4 41.94 2.32 4 -14 -5 39.61 2.25 5 -12 -8 46.58 2.48 5 -8 -2 155.19 2.74 4 -10 0 227.33 3.22 2 -7 2 825.75 4.03 4 -5 -1 470.52 3.36 5 -8 -11 270.94 4.26 -1 -7 4 10.28 0.64 4 -12 -1 68.11 2.37 3 -13 0 45.60 2.09 5 -4 -5 181.83 2.59 5 -9 -11 28.38 2.03 3 -15 -3 28.88 2.01 1 -6 3 1010.73 3.55 2 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48.45 2.18 6 -12 -7 92.23 2.93 0 -8 4 1.14 0.70 5 -11 -1 202.22 3.48 -1 -6 4 350.93 1.45 4 -1 -6 294.34 2.38 6 -9 -6 24.35 2.00 4 -1 -8 116.34 1.72 3 -11 2 38.21 1.62 6 -12 -5 24.45 2.13 5 -12 -2 43.74 2.25 6 -7 -5 377.52 4.20 5 -3 -8 29.91 1.38 6 -10 -5 70.77 2.62 6 -7 -6 20.17 1.60 5 -3 -7 48.70 1.54 5 -3 -5 533.87 3.74 6 -6 -5 0.85 1.21 4 -1 -7 371.10 2.72 5 -5 -2 101.43 2.09 2 -13 2 94.22 2.28 5 -12 -1 235.31 3.85 5 -4 -3 55.84 1.72 1 -5 3 182.88 1.45 5 -14 -3 73.11 2.71 6 -7 -7 61.65 2.25 4 -7 1 96.35 2.03 6 -6 -10 262.87 3.77 0 -7 4 -0.01 0.70 4 -4 -1 303.11 2.51 6 -6 -4 233.26 3.13 2 -10 3 51.67 1.52 6 -6 -7 3.53 1.33 4 -15 -2 56.22 2.35 4 -11 1 81.63 2.21 5 -9 0 493.10 4.47 2 -11 3 21.33 1.27 5 -10 0 52.36 1.94 5 -6 -1 199.71 2.67 4 -2 -3 42.24 1.15 0 -10 4 25.45 0.97 6 -5 -9 40.34 1.77 1 -12 3 17.90 1.21 0 -4 3 662.43 1.89 4 -12 1 64.91 2.14 6 -10 -3 17.24 1.75 1 0 -1 766.68 1.46 6 -6 -8 10.88 1.54 6 -8 -11 27.56 1.87 6 -5 -5 212.73 2.96 6 -9 -11 43.78 2.11 4 -1 -5 397.98 2.62 4 -14 -1 42.93 2.18 5 -13 -2 219.18 3.91 1 -3 2 8.22 0.60 2 -7 3 497.65 3.05 6 -5 -10 191.17 3.12 5 -12 0 134.00 2.98 2 -4 2 4279.29 6.85 6 -5 -7 153.01 2.71 3 -2 -1 314.78 2.04 6 -6 -3 32.29 1.64 6 -13 -3 113.05 3.11 3 -7 2 149.40 2.10 3 -12 2 78.22 2.10 7 -10 -6 75.37 2.70 7 -10 -7 107.61 3.06 4 -13 1 17.07 1.62 5 -15 -3 16.55 1.76 6 -5 -4 18.10 1.37 2 -6 3 1426.69 4.57 6 -7 -2 295.75 3.45 7 -8 -7 170.27 3.38 7 -9 -8 324.65 4.61 3 -13 2 77.53 2.20 3 0 -4 185.12 1.40 4 -10 2 187.38 2.77 3 -6 2 878.16 4.12 3 -1 -2 367.11 2.05 7 -11 -6 26.64 2.03 5 -4 -2 69.85 1.69 7 -11 -7 158.27 3.53 5 -5 -1 78.25 1.79 7 -8 -8 34.61 2.05 6 -14 -4 77.50 2.76 5 -2 -6 569.29 3.73 7 -11 -5 107.17 3.09 2 -12 3 1.02 1.01 3 -15 0 60.47 2.22 4 -11 2 27.58 1.55 3 -9 3 562.73 3.93 7 -10 -4 19.65 1.89 5 -10 1 84.08 2.23 7 -10 -9 23.65 1.93 7 -8 -9 70.49 2.50 7 -12 -6 44.15 2.34 5 -9 1 21.29 1.44 6 -8 -1 0.43 1.26 3 -8 3 230.02 2.52 0 -6 4 342.72 1.72 3 -11 3 265.57 3.13 7 -12 -5 18.97 1.92 6 -4 -5 121.29 2.23 5 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20.65 1.89 4 7 -3 17.99 1.15 -3 3 4 492.36 2.28 4 6 -4 239.98 2.33 2 7 1 1.76 1.24 -1 8 4 6.82 1.31 2 5 1 512.31 3.41 -4 7 5 17.67 1.22 0 10 3 71.35 2.35 0 8 3 74.05 2.04 1 8 2 34.95 1.70 2 6 1 58.96 1.75 3 7 -1 45.44 1.57 1 4 2 140.57 1.76 4 8 -4 226.19 2.75 -3 8 5 67.22 1.92 0 12 1 23.73 1.95 4 8 -5 15.41 1.19 1 2 1 102.99 1.12 3 10 -3 103.34 2.44 -1 15 -1 -1.35 1.60 -6 13 3 66.18 2.29 -2 2 3 3658.35 5.05 4 7 -5 207.54 2.32 3 6 -1 15.62 1.29 4 5 -5 104.02 1.38 2 9 0 24.21 1.51 3 2 -3 1913.98 3.14 -3 14 2 27.23 2.04 1 7 2 167.12 2.57 -4 14 2 20.55 2.00 -3 10 4 1.59 1.31 4 6 -5 189.95 2.00 -7 14 2 24.05 1.72 1 5 2 33.56 1.24 1 10 1 0.59 1.33 2 12 -3 66.24 2.45 1 6 2 188.44 2.49 0 14 -1 39.38 2.42 -1 5 4 407.50 3.10 -2 5 4 785.45 3.98 1 11 0 265.04 3.92 -1 3 3 1538.05 4.25 2 10 -1 66.81 2.15 3 8 -2 48.93 1.69 -3 4 4 335.08 2.27 -7 12 3 25.96 1.65 2 3 0 1594.30 4.34 2 11 -2 36.07 1.90 -2 7 4 114.27 2.20 -5 14 2 75.25 2.60 1 1 0 327.22 1.19 -3 9 4 105.68 2.29 2 8 0 31.54 1.48 -1 16 -3 20.31 1.98 -4 11 4 40.98 1.97 -2 4 4 12.78 0.91 -4 12 3 5.71 1.62 1 9 1 376.60 3.89 -4 4 4 315.56 2.07 0 11 1 28.12 1.81 -1 16 -4 22.86 2.00 3 11 -4 54.16 2.09 -1 15 -2 18.54 2.05 -3 14 1 24.72 2.10 -2 8 4 68.46 1.96 -6 12 3 46.06 1.99 0 1 1 3413.65 3.79 0 12 0 20.28 1.85 -2 9 4 85.98 2.21 -4 9 4 8.56 1.26 2 7 0 101.36 2.04 0 9 2 88.86 2.10 3 5 -1 19.68 1.25 2 9 -1 14.35 1.39 -6 6 4 191.84 1.92 -5 9 4 21.39 1.39 -3 5 4 790.48 3.83 -3 2 3 359.94 1.41 -5 10 4 75.62 2.11 3 11 -5 28.93 1.73 1 8 1 148.21 2.52 -3 12 3 20.95 1.82 1 10 0 92.97 2.43 -6 8 4 216.28 2.56 2 13 -5 71.99 2.46 3 4 -2 267.25 2.07 -3 7 4 147.29 2.27 -7 11 3 143.05 2.67 0 15 -5 59.04 2.50 2 6 0 718.56 4.24 -1 4 3 416.26 2.63 1 12 -2 47.18 2.30 3 8 -3 45.31 1.57 2 10 -2 232.65 3.39 -6 7 4 63.35 1.44 2 4 0 771.75 3.48 0 8 2 109.97 2.25 -4 2 3 39.55 0.44 1 11 -1 62.47 2.16 1 3 1 35.01 1.03 0 14 -3 69.13 2.68 -4 8 4 212.56 2.78 -4 14 1 33.33 2.16 -3 6 4 19.81 1.31 -5 13 2 132.28 3.14 -4 11 3 18.23 1.69 3 9 -3 -0.46 1.15 3 10 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8.47 1.11 3 -10 11 12.13 1.55 3 -9 14 1.94 1.30 6 -10 7 -0.81 1.29 8 -9 5 3.35 1.34 5 -10 8 12.03 1.59 6 -10 13 12.07 1.62 5 -9 5 -0.36 1.01 6 -8 3 3.29 1.03 5 -10 12 2.96 1.51 3 -9 13 0.74 1.25 8 -10 11 0.25 1.36 7 -10 8 -0.88 1.45 10 -9 8 4.92 1.31 7 -10 12 7.40 1.52 7 -10 7 -0.33 1.33 5 -10 11 6.53 1.53 7 -10 9 11.13 1.64 7 -10 11 1.56 1.39 6 -10 9 12.48 1.61 7 -10 10 -1.50 1.45 6 -9 5 134.33 2.42 4 -3 -1 1.27 0.50 8 -9 6 1.01 1.33 4 -9 14 2.48 1.37 4 -9 13 2.21 1.75 10 -8 7 13.03 1.48 5 -8 4 8.05 1.23 1 -8 11 5.77 1.19 0 -6 13 1.59 1.01 7 -8 4 98.52 2.10 1 -7 13 5.58 1.19 7 -5 0 1.41 0.78 0 -6 7 3.49 1.01 3 -9 10 0.68 1.29 5 -9 13 0.58 1.43 2 -8 9 2.50 1.16 7 -9 7 3.27 1.39 9 -8 6 -0.70 1.28 9 -9 9 0.58 1.36 8 -6 2 2.09 0.98 0 -6 12 0.48 1.00 6 -9 13 8.23 1.47 10 -8 8 1.28 1.28 5 -9 8 13.22 1.52 7 -9 12 0.11 1.47 7 -7 3 0.03 0.99 9 -8 5 4.38 1.31 7 -9 6 2.94 1.40 5 -9 9 11.42 1.58 9 -6 3 204.43 3.12 7 -9 11 1.43 1.51 7 -9 9 6.09 1.58 7 -9 10 8.50 1.60 8 -9 10 0.31 1.48 4 -9 10 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1.38 8 -10 3 1.14 1.62 9 -7 5 17.40 1.91 7 -7 5 2.26 1.37 5 -10 -3 1.98 1.19 4 -9 -1 2.39 1.24 7 -11 0 8.62 1.75 1 -4 6 251.34 2.45 2 -11 3 18.34 1.44 3 -11 6 94.74 2.61 7 -12 9 68.25 2.55 0 -5 3 927.50 3.97 6 -14 6 122.12 3.08 6 -9 10 64.76 2.32 5 -2 9 43.87 1.25 7 -13 8 17.10 1.86 2 -11 2 23.32 1.40 1 -7 5 35.77 1.54 5 -14 4 38.64 2.03 6 -11 9 18.17 1.84 0 -3 3 5.88 0.79 2 -9 6 100.62 2.25 0 -4 3 847.91 3.57 8 -12 9 59.35 2.37 4 -1 8 66.06 1.23 1 -9 2 113.21 2.02 4 -13 4 41.68 2.07 6 -15 2 61.40 2.18 2 -11 1 83.14 1.95 1 -9 -1 14.71 0.93 4 -11 7 36.71 1.97 0 -6 1 6.82 0.76 4 -12 6 454.60 5.13 6 -5 10 15.97 1.35 3 -12 3 208.16 3.26 4 -7 9 132.08 2.72 5 -11 8 136.30 3.20 0 -6 2 312.24 2.40 1 -9 1 108.74 1.91 6 -13 7 137.22 3.36 0 -6 -1 185.66 1.53 9 -9 10 26.99 1.68 3 -3 8 179.11 2.23 5 -14 3 149.54 3.13 1 -9 0 2.13 0.89 3 -7 8 669.67 5.13 1 -9 3 2.46 1.06 7 -15 4 83.84 2.63 6 -6 10 292.43 3.66 6 -14 5 76.96 2.71 0 -6 0 292.71 2.04 8 -10 10 15.89 1.65 4 -6 9 26.43 1.50 5 -9 9 10.81 1.60 6 -8 10 194.12 3.47 4 -13 3 151.77 3.02 1 -6 5 97.99 1.91 2 -8 6 214.10 2.98 2 -4 7 25.30 1.35 1 -2 5 2168.89 5.32 2 -3 7 527.14 3.37 3 -12 2 48.91 1.86 7 -5 10 33.87 1.57 1 -8 4 66.89 1.82 5 -7 10 48.10 1.91 5 -12 7 1.92 1.63 8 -8 10 124.11 2.82 3 -9 7 23.28 1.56 4 -13 5 387.35 4.75 5 -13 5 316.55 4.36 8 -11 9 114.72 2.94 4 -12 5 84.63 2.47 7 -7 10 74.82 2.27 2 -9 5 48.67 1.76 4 -13 2 261.19 3.64 4 -5 9 79.20 1.94 2 -1 6 64.56 1.11 1 -5 5 77.19 1.57 0 -5 2 561.83 2.89 6 -14 4 21.36 1.88 6 -13 6 11.12 1.82 4 -4 9 49.63 1.55 1 -3 5 312.49 2.29 6 -7 10 72.44 2.23 3 -6 8 187.33 2.83 4 -10 7 51.95 2.16 4 -11 6 22.67 1.84 2 -7 6 35.21 1.57 7 -6 10 7.26 1.31 8 -12 8 46.71 2.29 7 -14 5 27.36 1.99 4 -8 8 364.42 4.13 1 0 4 615.61 1.99 4 -2 8 125.73 1.79 5 -12 6 152.40 3.38 4 -12 4 66.50 2.39 2 -10 4 57.75 1.81 6 -14 3 82.84 2.61 4 -13 1 22.68 1.55 2 -10 -2 18.65 1.02 0 -4 2 157.52 1.53 0 -5 -2 363.19 1.63 5 -8 9 20.49 1.65 3 -10 5 300.56 3.80 1 -8 3 205.53 2.61 2 -8 5 6.97 1.34 5 -1 8 40.92 1.06 5 -6 9 40.74 1.77 5 -5 9 63.39 1.88 1 -7 4 186.06 2.48 3 -5 8 19.06 1.34 0 -5 0 22.72 0.77 3 -11 3 231.28 3.30 7 -11 8 38.90 2.24 8 -14 5 18.85 1.89 8 -10 9 31.82 2.03 9 -10 9 155.49 3.29 7 -13 6 204.37 4.03 3 -9 6 23.40 1.66 2 -10 1 112.31 2.09 1 -8 -2 9.55 0.84 1 -8 1 49.22 1.48 5 -4 9 21.04 1.28 0 -3 2 1758.54 4.21 5 -9 8 16.01 1.65 6 -14 2 74.70 2.51 3 -1 7 11.16 0.90 2 -10 0 278.36 2.86 5 -13 3 721.12 6.16 6 -10 8 19.75 1.79 8 -13 7 0.89 1.54 5 -11 7 26.35 1.91 4 -12 3 13.37 1.62 6 -8 9 15.28 1.69 0 -1 1 11.23 0.28 1 -1 4 9.44 0.67 3 -11 4 33.27 1.76 1 -8 0 228.12 2.31 5 -12 5 50.68 2.26 2 -10 3 35.71 1.51 4 -3 8 340.49 3.00 7 -3 9 16.90 1.12 3 -4 8 16.68 1.25 1 -8 -1 513.82 3.05 9 -11 8 204.18 3.84 6 -3 9 38.44 1.36 3 -11 2 44.34 1.77 6 -4 9 67.89 1.79 7 -12 7 6.83 1.76 4 -6 8 36.24 1.65 0 -5 1 141.32 1.49 3 -6 7 138.81 2.44 7 -8 9 125.11 2.92 1 -5 4 892.93 4.21 5 -10 7 133.93 3.09 2 -3 6 148.02 1.89 5 -7 9 39.83 1.81 1 -8 2 72.71 1.75 3 -2 7 230.83 2.27 5 -13 2 75.07 2.45 2 -4 6 83.73 1.67 7 -14 3 21.34 1.83 2 -7 5 13.25 1.41 6 -5 9 140.20 2.53 9 -8 9 75.47 2.38 3 -8 6 12.47 1.44 5 -8 8 111.69 2.71 2 0 5 1117.01 3.04 8 -8 9 30.82 1.91 3 -11 -2 235.51 2.66 8 -13 6 6.74 1.67 2 -8 4 480.58 3.99 8 -4 9 418.52 3.82 7 -4 9 61.30 1.79 0 -3 1 1045.70 2.90 4 0 7 385.27 2.19 3 -9 5 47.05 1.83 6 -9 8 39.55 2.01 9 -13 6 62.15 2.41 1 -7 3 520.68 3.60 3 -4 7 243.20 2.74 8 -9 9 198.88 3.71 1 -4 4 1604.98 5.18 3 0 6 22.40 0.82 5 -11 6 92.11 2.75 3 -11 1 15.74 1.33 6 -7 9 91.53 2.42 6 -14 0 17.92 1.57 8 -7 9 82.96 2.41 2 -9 4 461.96 4.01 4 -12 1 30.15 1.65 4 -5 8 102.81 2.07 1 -2 4 1592.46 4.23 7 -5 9 25.71 1.50 8 -10 8 50.55 2.35 6 -11 7 65.47 2.48 0 -2 1 210.87 1.18 2 -9 2 34.32 1.52 3 -11 0 83.29 1.97 8 -5 9 20.69 1.48 0 -4 0 378.60 1.89 5 -7 8 78.45 2.20 4 -12 -1 40.64 1.66 8 -14 3 40.64 2.08 8 -13 5 47.83 2.42 7 -14 1 59.90 2.25 2 -6 5 10.41 1.43 4 -10 5 48.10 2.03 2 -2 6 49.00 1.18 0 -4 -3 44.02 0.44 0 -4 1 34.06 0.91 5 -13 0 20.33 1.62 7 -9 8 103.70 2.84 9 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6 136.90 1.33 2 -8 -1 159.33 2.09 4 -5 6 6.31 1.28 8 -7 7 80.53 2.53 11 -8 6 36.06 1.95 4 -7 5 13.63 1.46 6 -6 7 379.56 4.05 10 -5 7 36.01 1.78 10 -6 7 59.51 2.17 3 -8 3 210.39 2.88 4 -10 1 40.72 1.69 5 -4 7 295.60 3.14 1 -6 -1 25.36 0.91 2 -8 -3 35.95 1.09 7 -10 5 55.62 2.49 6 -12 -2 29.89 1.75 7 -1 7 41.64 1.29 2 -8 -2 225.54 2.29 6 -11 4 29.36 2.02 6 -10 4 49.58 2.13 6 -5 7 54.41 1.81 0 -1 0 90.20 0.45 1 -4 2 3592.12 6.77 4 -8 4 40.55 1.79 8 -13 -1 102.28 2.77 9 -11 4 52.94 2.60 10 -10 5 6.48 1.83 8 -12 2 113.89 3.22 7 -12 1 117.38 3.07 6 -12 0 269.73 3.90 2 -7 2 766.19 4.33 4 -4 6 490.63 3.72 1 -6 -4 636.58 2.30 5 -9 4 1204.82 7.23 4 2 5 150.84 0.98 6 -11 2 31.94 1.92 1 -5 1 681.12 3.11 3 -9 0 17.07 1.31 7 -6 7 0.98 1.36 9 -6 7 95.11 2.60 9 -3 7 267.71 3.29 10 -8 6 8.71 1.62 3 -4 5 43.82 1.47 5 -6 6 43.92 1.75 1 -6 -2 546.10 2.59 3 -6 4 274.61 2.99 4 -3 6 55.64 1.60 9 -13 0 83.38 2.64 2 0 4 811.46 2.50 2 -6 3 1581.49 5.87 5 -10 3 64.69 2.15 4 -2 6 38.93 1.35 5 -3 7 115.92 2.06 9 -5 7 25.86 1.72 3 -9 -1 6.88 1.11 1 -6 -3 313.68 1.86 3 0 5 9.07 0.68 2 -5 3 1753.69 5.71 5 -11 -3 41.99 1.65 8 -12 1 146.93 3.45 9 -9 6 98.72 2.88 5 -11 -1 122.61 2.57 4 -10 0 242.44 3.15 4 -1 6 -0.25 0.93 8 -3 7 29.06 1.48 8 -4 7 11.98 1.35 3 -8 2 171.88 2.60 3 -9 -2 518.90 3.66 10 -12 1 27.08 2.04 2 -2 4 2812.94 5.89 4 -9 3 341.57 3.72 6 -11 1 243.22 3.71 3 -9 -3 54.21 1.41 3 -3 5 1044.59 4.42 10 -7 6 0.91 1.41 7 -12 -3 29.20 1.77 6 -3 7 36.28 1.45 2 -1 4 482.80 2.29 4 -10 -3 31.39 1.37 5 -5 6 62.38 1.84 7 -11 2 0.77 1.59 0 -3 -2 1725.20 2.42 7 -11 3 7.01 1.66 2 -7 1 48.82 1.48 8 -5 7 131.07 2.71 1 -5 0 971.49 3.51 7 -12 -1 23.57 1.88 3 -1 5 122.43 1.44 6 -9 4 232.41 3.59 2 -7 0 241.14 2.41 4 -7 4 81.19 2.16 11 -5 6 24.44 1.60 6 -7 6 30.80 1.71 9 -4 7 61.76 2.01 9 -7 6 25.35 1.94 3 -8 1 343.84 3.27 8 -7 6 41.21 2.06 7 -2 7 231.40 2.70 3 -7 3 202.84 2.72 5 -10 1 89.95 2.37 8 -11 3 28.35 2.12 6 -10 3 44.25 2.11 6 -2 7 8.40 0.96 8 -11 2 10.38 1.91 1 -3 2 19.72 0.84 5 -4 6 362.47 3.43 4 -9 1 66.91 1.93 4 -5 5 186.41 2.55 8 -12 -3 26.88 1.81 7 -11 1 245.09 4.12 8 -12 -2 35.40 2.00 7 -7 6 30.25 1.86 6 -10 2 91.46 2.50 2 -4 3 1176.31 4.39 11 -8 5 1.69 1.52 9 -6 6 38.40 2.04 7 -9 4 26.72 1.92 5 0 6 137.70 1.63 10 -3 6 23.61 1.50 10 -12 -2 41.00 2.12 10 -4 6 107.54 2.53 8 -12 -1 52.60 2.38 6 -5 6 45.07 1.70 5 -1 6 317.00 2.60 2 -6 2 15.54 1.11 10 -11 2 69.73 2.67 8 -6 6 211.91 3.50 9 -12 -3 14.07 1.67 2 -7 -1 147.92 1.99 1 -2 2 3051.81 4.96 11 -11 1 18.28 1.90 6 -11 -2 134.53 2.82 5 -6 5 9.94 1.41 5 -2 6 20.33 1.23 6 -11 -1 4.36 1.46 6 -11 0 382.70 4.47 9 -10 3 4.45 1.86 9 -12 -2 23.43 1.88 10 -5 6 11.04 1.57 5 -9 3 178.30 3.07 8 -11 1 6.73 1.76 10 -11 1 251.18 4.43 6 -9 3 466.39 4.80 6 0 6 109.35 1.61 2 -5 2 43.88 1.18 10 -7 5 81.73 2.61 6 -8 4 54.46 2.06 7 -5 6 167.64 2.92 10 -8 5 9.03 1.74 1 -5 -1 39.87 0.93 6 -4 6 233.07 2.99 3 -2 5 3.17 0.82 11 -9 3 27.73 2.08 5 -10 0 42.80 1.82 6 -10 1 41.37 2.01 4 -8 3 38.49 1.77 3 -7 2 160.22 2.36 9 -2 6 58.76 1.84 7 -10 2 19.72 1.73 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18.42 1.09 6 7 8 8.71 1.02 1 3 11 2.28 0.79 5 1 5 94.29 1.17 7 4 5 28.23 1.02 1 8 12 21.37 1.08 -2 8 12 0.75 0.70 1 4 11 28.07 1.04 5 5 9 7.69 1.00 4 5 10 150.22 1.93 -1 7 12 205.20 1.89 5 3 8 16.69 0.93 0 13 11 6.48 0.67 7 6 7 13.77 1.03 -1 2 9 261.57 1.53 0 6 12 8.96 0.94 4 2 8 2.41 0.78 0 7 12 53.39 1.26 4 1 7 119.54 1.30 7 4 4 62.34 1.18 -1 3 10 19.20 0.74 4 0 4 106.26 1.04 6 2 4 14.30 0.75 2 5 11 32.71 1.19 3 0 5 4.90 0.62 4 6 10 32.76 1.22 5 8 9 18.67 1.04 2 13 10 8.07 0.71 2 2 9 28.29 0.93 5 7 9 58.57 1.41 2 3 10 48.73 1.10 7 6 6 7.20 0.91 7 7 6 0.64 0.88 7 4 3 165.37 1.54 0 3 10 2.09 0.65 4 1 6 1364.41 3.60 1 7 12 36.13 1.17 0 9 12 8.03 0.89 6 2 3 672.15 2.50 7 7 5 125.35 1.67 6 3 6 26.06 0.98 0 2 9 50.02 0.92 4 4 9 54.24 1.28 1 5 11 29.68 1.09 0 1 8 104.49 1.09 6 2 2 35.04 0.78 7 4 2 41.29 0.91 5 3 7 83.88 1.32 5 1 3 591.60 2.09 -1 9 12 10.67 0.86 5 2 6 627.73 2.71 2 1 8 15.55 0.85 3 1 7 308.69 1.83 -2 6 11 84.94 1.22 2 8 11 29.75 1.19 5 1 2 438.33 1.71 1 1 8 690.07 2.46 -2 3 9 32.29 0.73 2 4 10 198.00 1.87 5 4 8 51.34 1.26 6 5 7 2.55 0.88 2 7 11 49.58 1.30 1 6 11 93.47 1.54 -2 4 10 0.39 0.55 7 8 5 41.52 1.15 7 6 5 17.73 1.02 4 1 5 621.20 2.38 4 5 9 41.94 1.21 -2 5 11 73.52 1.11 6 5 6 13.75 0.99 6 3 4 40.66 0.95 5 9 8 67.04 1.48 5 6 8 42.07 1.20 7 9 5 9.90 0.89 -1 6 11 164.83 1.72 0 6 11 11.06 0.95 -3 7 11 14.57 0.74 7 6 4 32.27 1.09 1 4 10 8.15 0.82 5 7 8 89.32 1.54 3 1 6 130.75 1.30 4 9 9 131.43 1.85 6 9 6 57.42 1.35 -1 5 11 44.41 1.04 7 6 3 189.94 1.79 -1 4 10 13.93 0.75 4 2 7 259.13 1.86 7 7 4 26.12 1.05 5 4 7 14.02 0.94 0 4 10 12.58 0.79 6 6 6 88.47 1.46 2 5 10 41.03 1.19 4 7 9 45.40 1.37 7 5 1 10.92 0.72 -1 2 8 0.23 0.59 6 8 6 26.12 1.13 6 6 7 55.12 1.31 2 3 9 7.30 0.76 7 8 4 19.54 1.01 1 10 11 37.28 1.19 6 3 3 16.83 0.74 6 2 1 85.14 0.92 -1 3 9 64.31 0.98 7 7 3 63.48 1.27 -1 7 11 96.58 1.47 -2 7 11 52.03 1.10 4 1 4 266.62 1.49 -2 8 11 145.22 1.61 7 6 2 18.08 0.90 5 2 4 181.00 1.46 7 10 3 14.27 0.87 0 8 11 14.36 1.03 5 10 7 11.82 1.04 4 2 6 196.36 1.56 5 3 6 109.63 1.35 0 3 9 304.17 1.86 -1 8 11 8.66 0.92 1 3 9 2.55 0.67 0 9 11 17.61 1.05 6 3 2 89.06 1.07 -3 6 10 52.85 0.96 7 10 2 30.74 0.98 7 7 2 36.52 1.04 1 5 10 28.20 1.03 7 6 1 6.95 0.72 2 10 10 14.15 1.03 2 6 10 19.40 1.10 6 7 6 41.71 1.21 4 5 8 110.57 1.59 7 9 2 12.59 0.88 2 9 10 49.32 1.33 2 11 10 21.58 1.05 2 7 10 79.89 1.50 5 9 7 11.69 1.03 5 6 7 16.99 1.03 2 4 9 -0.16 0.76 -3 8 11 20.45 0.82 3 1 5 1164.76 2.94 7 9 1 23.56 0.93 2 8 10 121.99 1.81 4 10 8 19.91 1.15 3 16 5 8.88 0.63 5 8 7 47.34 1.35 7 7 1 28.68 0.93 5 11 6 11.99 1.00 -1 9 11 26.65 1.08 3 2 7 71.07 1.14 5 5 7 50.92 1.27 7 8 1 7.88 0.82 6 7 5 104.77 1.58 2 2 8 80.04 1.16 6 5 5 1.32 0.77 -2 9 11 0.51 0.77 4 6 8 105.49 1.68 0 5 10 8.89 0.85 3 12 8 24.84 1.09 -2 4 9 99.27 1.09 6 4 3 211.95 1.65 4 2 5 212.13 1.56 4 4 7 106.73 1.45 4 7 8 41.55 1.34 6 10 4 65.26 1.39 4 8 8 32.86 1.26 4 3 7 7.05 0.76 -2 5 10 30.91 0.85 1 4 9 1.75 0.68 -2 6 10 152.65 1.50 -1 5 10 30.59 0.92 5 2 2 106.87 1.06 4 9 8 42.52 1.35 1 7 10 58.46 1.39 2 5 9 8.26 0.90 5 10 6 11.71 1.04 1 2 8 -0.52 0.73 1 9 10 2.97 0.98 1 6 10 81.86 1.47 5 4 6 136.98 1.58 1 8 10 29.08 1.24 -1 6 10 20.39 0.94 5 3 4 1.07 0.69 0 2 8 380.80 1.87 -1 4 9 129.07 1.30 0 4 9 14.69 0.77 6 8 5 44.19 1.26 -3 5 9 144.59 1.22 -1 12 10 -0.83 0.79 6 12 3 17.19 0.89 6 4 2 102.87 1.19 5 9 6 21.36 1.11 -2 3 8 6.34 0.59 4 5 7 23.99 1.03 4 3 6 3.76 0.76 3 5 8 24.12 1.02 6 5 3 72.87 1.20 0 7 10 29.84 1.12 6 9 5 22.77 1.11 2 6 9 52.26 1.23 5 11 5 17.74 1.04 -1 11 10 14.52 0.97 4 10 7 67.01 1.52 6 6 4 7.49 0.87 6 4 1 191.52 1.41 4 2 4 378.52 1.84 0 8 10 166.42 1.85 -2 7 10 13.07 0.86 0 3 8 19.19 0.75 6 3 1 189.59 1.31 -1 7 10 66.85 1.28 1 5 9 1.90 0.80 0 6 10 93.45 1.40 0 14 9 3.19 0.75 6 7 4 38.30 1.14 -3 10 10 25.90 0.96 3 10 8 13.61 1.13 5 12 4 28.55 1.10 6 12 2 9.25 0.81 3 6 8 52.89 1.30 -3 4 8 97.76 0.91 4 9 7 63.37 1.48 6 6 3 3.23 0.84 5 3 3 576.91 2.32 1 2 7 19.49 0.80 5 7 6 46.20 1.26 6 8 4 28.96 1.11 3 9 8 17.06 1.18 4 13 5 9.48 0.93 6 5 2 101.73 1.25 3 3 7 7.58 0.82 3 4 7 6.78 0.79 -1 3 8 26.10 0.77 3 7 8 157.44 1.85 6 9 4 4.41 0.89 0 5 9 40.70 1.02 6 7 3 36.15 1.09 3 2 5 866.88 2.73 -1 8 10 38.81 1.17 0 2 7 77.49 1.02 3 8 8 87.31 1.63 4 11 6 15.90 1.12 3 12 7 22.33 1.12 1 6 9 10.60 0.88 -1 5 9 205.07 1.64 -3 8 10 6.29 0.74 1 4 8 129.26 1.41 -3 6 9 9.07 0.67 -2 5 9 47.82 0.93 4 2 3 586.90 2.11 -2 8 10 126.82 1.56 4 15 2 17.47 0.86 5 5 5 84.21 1.31 5 3 2 83.71 1.02 2 13 7 16.72 1.06 3 11 7 16.58 1.15 6 9 3 8.58 0.95 1 9 9 41.97 1.31 4 4 6 26.18 0.93 5 6 5 58.59 1.28 -1 9 10 1.33 0.90 1 8 9 175.03 1.93 3 5 7 7.45 0.84 4 10 6 31.53 1.28 3 3 6 537.91 2.43 1 10 9 -0.03 0.99 6 7 2 13.78 0.91 1 2 6 25.02 0.74 1 3 7 666.84 2.50 5 5 4 161.92 1.55 0 4 8 101.15 1.23 4 6 6 23.70 0.98 4 13 4 11.83 0.99 5 4 3 207.66 1.57 6 11 0 29.25 1.02 6 9 2 15.57 0.98 -2 6 9 26.56 0.88 -4 8 9 9.75 0.72 2 16 4 7.56 0.77 4 3 4 15.12 0.85 3 10 7 83.62 1.68 4 9 6 127.42 1.87 -1 6 9 23.55 0.89 0 6 9 93.65 1.40 6 6 1 89.65 1.20 5 7 5 26.19 1.07 0 7 9 115.05 1.58 4 8 6 54.11 1.40 1 5 8 55.65 1.10 5 6 4 93.81 1.37 1 16 5 9.18 0.81 6 9 1 75.18 1.33 3 2 4 80.57 0.95 3 9 7 393.68 2.83 2 12 7 18.59 1.14 0 8 9 13.30 1.03 -4 9 9 45.78 1.02 3 12 6 -0.41 0.95 3 7 7 39.73 1.20 0 3 7 92.17 1.13 2 2 5 22.33 0.71 3 6 7 51.01 1.22 3 8 7 183.03 2.03 6 8 1 18.04 0.93 -2 14 8 9.65 0.89 5 10 4 63.39 1.42 -1 7 9 66.02 1.27 -1 3 7 104.83 1.08 0 9 9 48.38 1.39 -2 7 9 9.43 0.82 4 7 6 17.40 1.04 3 13 5 10.00 1.02 5 12 3 14.09 1.01 4 5 5 1.08 0.78 5 4 2 10.33 0.71 0 10 9 25.72 1.16 4 12 4 5.93 1.03 1 6 8 46.88 1.16 4 10 5 82.59 1.57 -3 12 9 14.11 0.90 -2 4 8 404.37 1.85 -3 10 9 2.95 0.87 0 12 8 46.75 1.31 -3 9 9 40.66 1.10 -2 10 9 12.70 0.98 6 8 0 20.52 0.91 -2 17 6 7.09 0.66 -1 4 8 167.25 1.40 5 11 3 120.36 1.74 4 4 4 332.84 1.94 4 3 3 1225.75 3.10 3 4 6 30.39 0.97 4 9 5 25.01 1.11 5 6 3 28.65 0.94 -2 5 8 78.13 1.04 1 9 8 212.40 2.13 5 3 1 84.49 1.00 -1 5 8 46.75 0.94 1 8 8 22.68 1.16 -2 8 9 84.69 1.36 1 7 8 292.58 2.26 6 5 0 13.35 0.67 3 10 6 318.21 2.61 5 9 4 5.51 0.98 -1 9 9 30.38 1.17 2 10 7 0.96 0.96 5 12 2 178.77 1.91 3 5 6 20.39 0.89 -3 8 9 39.11 1.02 4 11 4 144.21 1.95 4 6 5 205.45 1.86 5 4 1 912.25 2.74 1 4 7 136.68 1.35 1 3 6 1233.81 3.13 0 6 8 10.63 0.81 5 5 2 117.69 1.29 3 9 6 93.98 1.66 3 15 2 10.24 0.91 2 12 6 3.23 0.98 -1 14 7 10.45 0.98 3 8 6 168.03 1.91 3 3 4 111.28 1.22 -3 6 8 18.25 0.71 5 12 0 58.71 1.30 3 16 0 8.37 0.81 -2 9 9 41.70 1.16 0 7 8 10.57 0.89 3 4 5 311.60 1.87 5 10 2 66.35 1.42 5 9 3 64.36 1.36 -1 6 8 24.89 0.86 2 3 5 44.24 0.96 4 3 2 1595.02 3.32 4 7 5 56.26 1.22 3 11 5 0.96 1.04 0 8 8 109.25 1.56 5 6 2 68.78 1.14 -2 16 6 13.99 0.88 -2 6 8 25.05 0.84 4 4 3 32.51 0.93 1 15 5 10.24 0.95 3 6 6 23.18 0.94 0 4 7 180.02 1.46 0 10 8 1.42 0.95 2 11 6 24.52 1.23 4 9 4 53.00 1.33 0 3 6 321.80 1.63 5 7 2 10.79 0.82 5 11 1 68.01 1.38 3 5 5 158.49 1.54 5 5 1 0.19 0.65 4 8 5 10.44 0.94 5 12 -1 81.59 1.39 -1 7 8 137.38 1.52 2 15 3 11.36 0.99 0 12 7 5.29 1.07 5 10 1 15.37 1.02 4 10 4 14.33 1.05 -4 8 8 11.11 0.74 3 10 5 40.10 1.26 -3 7 8 109.52 1.28 3 12 4 30.46 1.24 0 17 3 19.77 0.92 -1 8 8 14.85 0.97 -1 4 7 790.00 2.59 -2 7 8 64.89 1.14 1 5 7 250.86 1.82 1 7 7 8.52 0.88 1 4 6 8.81 0.82 2 5 6 40.09 0.99 -2 4 7 70.75 0.92 -4 9 8 6.51 0.77 4 7 4 35.80 1.08 3 13 3 32.83 1.22 3 9 5 187.72 1.95 5 6 1 0.96 0.65 -1 9 8 0.79 0.92 5 9 1 141.94 1.66 4 5 3 222.58 1.64 5 4 0 27.81 0.75 3 4 4 88.02 1.18 -1 13 7 16.22 1.07 2 9 6 -0.27 0.89 -2 8 8 41.52 1.08 0 11 7 120.85 1.80 -4 11 8 1.59 0.81 4 14 0 34.59 1.12 -3 9 8 38.86 1.07 -4 12 8 59.50 1.22 5 8 1 20.11 0.94 5 7 1 8.15 0.76 2 4 5 41.59 0.95 3 6 5 225.64 1.85 3 3 3 35.95 0.77 4 8 4 4.19 0.93 -3 5 7 21.12 0.66 5 11 -1 19.23 1.00 5 10 0 50.80 1.20 4 4 2 319.23 1.72 -1 14 6 26.87 1.18 -1 18 2 9.08 0.78 0 6 7 29.74 0.89 4 6 3 255.59 1.83 4 10 3 79.11 1.51 4 9 3 7.87 0.97 -4 13 7 20.31 1.01 4 14 -2 11.30 0.90 2 17 0 9.26 0.79 4 7 3 1.41 0.78 2 11 5 14.23 1.16 2 14 3 14.16 1.09 -2 9 8 11.43 0.93 4 12 2 23.67 1.12 5 9 0 17.73 0.93 5 6 0 126.55 1.25 0 7 7 37.62 1.04 0 5 7 202.87 1.55 2 6 6 75.37 1.22 0 10 7 36.88 1.28 3 5 4 131.74 1.38 0 9 7 12.57 1.03 -4 6 7 59.56 0.82 0 8 7 24.13 0.97 3 7 5 17.72 0.92 5 10 -1 57.00 1.21 -2 13 7 18.20 1.09 1 14 4 24.45 1.19 5 7 0 21.81 0.84 -4 16 5 9.10 0.83 4 8 3 44.74 1.17 4 11 2 64.52 1.45 4 5 2 200.13 1.49 4 13 -1 2.24 0.90 -4 12 7 15.54 0.97 -1 10 7 13.25 1.03 3 11 4 9.48 1.12 -5 11 7 8.88 0.79 1 12 5 112.23 1.83 3 4 3 82.26 1.11 5 9 -1 133.19 1.48 4 4 1 65.21 0.97 -2 6 7 316.90 1.84 -3 6 7 0.69 0.59 4 12 1 8.95 1.02 -1 7 7 15.00 0.83 4 9 2 82.33 1.38 3 9 4 60.33 1.34 3 10 4 169.14 1.92 -1 5 7 17.49 0.79 4 12 0 23.23 1.10 5 5 0 7.52 0.64 -1 9 7 79.94 1.40 4 6 2 51.47 1.01 -1 13 6 12.32 1.10 -1 8 7 40.34 1.06 5 8 -1 48.45 1.01 0 11 6 7.38 1.08 5 7 -1 88.82 1.11 -3 16 5 16.55 0.96 4 7 2 53.59 1.06 4 8 2 14.81 0.90 4 11 1 11.31 1.02 2 8 5 64.50 1.30 2 4 4 29.11 0.90 -1 14 5 17.98 1.15 -3 11 7 3.84 0.92 3 7 4 232.18 1.86 1 16 1 10.55 0.99 -1 12 6 1.35 0.98 3 12 3 1.57 1.01 5 9 -2 32.87 0.94 4 10 1 32.61 1.14 2 9 5 37.23 1.14 1 18 -3 28.46 0.87 -2 8 7 64.29 1.12 -4 8 7 21.87 0.79 1 17 -1 10.25 0.88 -3 10 7 60.09 1.25 3 5 3 131.24 1.34 0 10 6 21.91 1.11 4 12 -1 -0.31 0.90 0 14 4 15.27 1.11 -4 11 7 24.97 1.01 4 5 1 76.22 1.01 -4 9 7 25.58 0.90 4 11 0 28.35 1.10 5 8 -2 61.91 1.02 3 8 4 10.33 0.90 0 5 6 88.31 1.16 5 7 -2 81.07 1.02 3 11 3 13.05 1.05 -5 13 6 62.03 1.23 3 13 1 2.30 0.98 0 15 3 16.32 1.04 3 14 -1 11.76 1.01 -2 7 7 0.23 0.69 0 9 6 52.60 1.27 -2 9 7 19.07 0.95 3 9 3 2.27 0.84 4 4 0 647.39 2.04 1 10 5 13.43 1.01 -4 7 7 57.07 0.90 -1 11 6 24.56 1.14 3 6 3 501.55 2.30 2 5 4 0.32 0.77 2 7 5 18.19 0.93 -2 13 6 20.11 1.14 5 6 -1 438.21 1.96 0 7 6 13.15 0.80 -2 19 -1 9.31 0.72 4 6 1 665.35 2.48 -4 16 4 12.95 0.91 -3 7 7 46.22 0.93 1 12 4 19.24 1.16 2 12 3 57.83 1.50 4 8 1 230.49 1.83 -1 13 5 12.53 1.11 -5 15 5 10.67 0.86 3 7 3 55.74 1.07 4 12 -2 11.24 0.96 4 7 1 214.55 1.63 3 4 2 12.64 0.68 -2 12 6 0.58 0.96 0 4 5 422.46 1.74 4 10 0 77.26 1.35 -1 10 6 8.78 0.94 2 6 4 726.62 2.71 2 11 4 0.71 0.95 -5 12 6 18.68 0.94 -3 5 6 47.21 0.79 2 8 4 87.37 1.32 -4 19 0 7.96 0.69 0 8 6 6.95 0.84 -3 8 7 13.76 0.81 -1 6 6 156.98 1.35 2 9 4 46.61 1.17 3 8 3 5.94 0.82 2 10 4 0.14 0.93 3 11 2 5.25 0.95 -1 5 6 72.50 1.03 4 5 0 134.35 1.16 4 12 -3 12.24 0.93 0 16 1 8.98 1.04 4 9 0 31.02 1.01 -1 9 6 46.99 1.15 -4 14 5 24.63 1.10 0 6 6 99.47 1.26 3 10 2 37.22 1.14 0 14 3 68.94 1.50 -5 14 5 10.09 0.92 -1 12 5 24.29 1.22 2 4 3 9.89 0.66 1 9 5 14.73 0.95 3 13 -1 11.38 1.06 3 5 2 1.39 0.72 2 16 -4 9.84 0.86 3 9 2 99.34 1.41 -2 18 0 10.73 0.88 2 14 1 12.48 1.06 -3 11 6 54.29 1.28 4 11 -2 1.05 0.85 4 10 -1 18.67 1.00 -2 10 6 71.44 1.34 4 8 0 11.66 0.79 -3 17 2 11.60 0.96 3 12 1 2.48 0.99 -2 6 6 1.08 0.67 -2 13 5 97.67 1.68 2 7 4 93.38 1.26 4 6 0 167.30 1.33 2 16 -5 12.56 0.87 -4 6 6 17.91 0.62 2 12 2 40.85 1.30 4 7 0 6.42 0.73 0 5 5 23.46 0.86 3 6 2 181.86 1.46 -3 6 6 64.59 0.92 -2 5 6 682.13 2.27 -2 9 6 11.85 0.88 -3 13 5 37.85 1.23 -2 14 4 1.29 0.97 3 14 -4 34.16 1.12 3 7 2 153.04 1.48 -3 10 6 7.96 0.91 2 11 3 7.48 1.05 -1 11 5 0.33 0.89 3 10 1 189.15 1.82 -5 8 6 16.81 0.69 2 5 3 52.18 0.99 0 17 0 20.16 1.00 -4 16 3 9.81 0.96 -4 11 6 3.87 0.88 4 9 -1 14.42 0.85 -5 9 6 21.00 0.81 4 11 -3 17.09 0.95 -2 12 5 28.16 1.23 -4 10 6 48.54 1.13 2 13 1 45.06 1.35 -5 13 5 14.95 0.98 1 12 3 60.44 1.47 2 9 3 104.46 1.41 0 7 5 3.93 0.76 -2 15 3 23.12 1.18 3 14 -5 9.69 0.89 -2 7 6 187.57 1.51 1 17 -4 8.85 0.87 -5 17 2 9.86 0.88 4 10 -2 28.61 1.02 0 13 3 41.63 1.36 -3 9 6 82.05 1.28 2 8 3 6.24 0.79 -4 19 -1 13.19 0.79 3 11 0 38.16 1.16 -5 10 6 -0.63 0.70 2 6 3 39.44 0.99 2 14 -1 11.66 1.07 -5 11 6 1.79 0.80 3 12 -1 26.31 1.14 -4 8 6 27.79 0.82 1 8 4 51.13 1.06 -5 15 4 24.30 1.05 3 9 1 27.21 1.00 -1 15 2 19.45 1.21 1 7 4 31.45 0.95 -6 12 5 12.02 0.86 4 7 -1 30.22 0.81 1 9 4 28.93 1.03 2 12 1 1.93 0.99 1 6 4 46.05 0.97 0 17 -2 20.65 1.06 2 7 3 50.24 1.01 4 5 -1 67.82 0.90 -3 7 6 6.26 0.67 -2 11 5 22.69 1.07 3 5 1 53.47 0.92 1 13 2 31.01 1.32 4 9 -2 16.55 0.83 -3 15 3 10.00 1.09 4 10 -3 25.68 0.97 -4 14 4 34.23 1.21 -3 12 5 40.59 1.22 -1 5 5 54.37 0.93 3 8 1 12.77 0.78 -5 12 5 16.51 0.99 2 11 2 30.47 1.15 -2 13 4 -0.25 1.05 3 10 0 20.46 0.98 0 16 -1 16.15 1.09 3 6 1 28.89 0.85 -1 6 5 328.99 1.80 3 7 1 63.36 1.05 0 16 0 13.04 1.04 3 13 -4 63.60 1.35 -2 18 -2 16.06 0.99 2 10 2 107.71 1.54 -6 11 5 2.27 0.73 -1 7 5 401.73 2.09 1 14 1 18.65 1.18 -4 17 1 8.71 0.97 4 8 -2 224.77 1.61 2 9 2 34.03 1.03 -2 10 5 17.98 0.96 1 12 2 24.97 1.22 -3 11 5 13.70 0.98 -6 19 -2 12.47 0.74 -1 16 1 11.23 1.08 -2 5 5 20.96 0.74 1 14 0 10.99 1.13 0 15 0 11.42 1.11 -3 8 6 26.34 0.86 -1 16 0 32.94 1.30 -6 14 4 48.49 1.17 2 12 0 39.32 1.19 -2 19 -4 0.80 0.70 2 15 -6 12.89 0.94 0 17 -3 1.39 0.88 -4 15 3 13.91 1.07 0 12 3 1.61 1.02 2 11 1 179.72 1.94 1 16 -4 0.27 0.89 4 6 -1 8.79 0.66 -1 8 5 33.52 0.94 1 11 3 2.36 1.00 -1 18 -4 0.96 0.83 0 14 2 0.80 1.02 -3 19 -3 0.79 0.72 4 11 -4 0.63 0.79 1 10 3 35.87 1.13 -1 9 5 147.01 1.57 1 13 1 56.06 1.49 4 5 -2 155.54 1.09 -5 15 3 7.02 0.95 -5 19 -2 5.38 0.71 4 10 -4 10.56 0.83 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 34496 _olex2_date_sample_data_collection 2019-08-06 _olex2_date_sample_submission 2019-08-05 _olex2_exptl_crystal_mounting_method ; The crystal was immersed in a film of perfluoropolyether oil, mounted on a polyimide microloop (MicroMounts of MiTeGen) and transferred to stream of cold nitrogen (Oxford Cryostream 800).' ; _olex2_submission_original_sample_id jxq2-27 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.424 _oxdiff_exptl_absorpt_empirical_full_min 0.696 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.97100(16) 0.37377(13) 0.29318(13) 0.0408(4) Uani 1 1 d . . . . . N1 N 1.00570(13) 0.43435(11) 0.24224(12) 0.0430(4) Uani 1 1 d . . . . . B1 B 0.48075(18) 0.85128(15) 0.21648(13) 0.0362(4) Uani 1 1 d . . . . . C2 C 0.86410(19) 0.35344(18) 0.31637(16) 0.0581(6) Uani 1 1 d . . . . . H2 H 0.812570 0.381116 0.297509 0.070 Uiso 1 1 calc R U . . . C23 C 0.92078(15) 0.72604(13) 0.32367(12) 0.0382(4) Uani 1 1 d . . . . . C3 C 0.8312(2) 0.2932(2) 0.3668(2) 0.0775(9) Uani 1 1 d . . . . . H3 H 0.757421 0.281279 0.382384 0.093 Uiso 1 1 calc R U . . . C4 C 0.9019(2) 0.24984(17) 0.39522(15) 0.0626(7) Uani 1 1 d . . . . . C5 C 1.0086(2) 0.27190(15) 0.37341(15) 0.0571(6) Uani 1 1 d . . . . . H5 H 1.059813 0.244313 0.392927 0.069 Uiso 1 1 calc R U . . . C6 C 1.04445(19) 0.33261(15) 0.32421(16) 0.0525(6) Uani 1 1 d . . . . . H6 H 1.119316 0.346600 0.311302 0.063 Uiso 1 1 calc R U . . . C7 C 0.8599(4) 0.1797(2) 0.4452(2) 0.0918(11) Uani 1 1 d . . . . . H7A H 0.921913 0.167975 0.473416 0.138 Uiso 1 1 calc R U . . . H7B H 0.820336 0.127603 0.410132 0.138 Uiso 1 1 calc R U . . . H7C H 0.810217 0.198045 0.484378 0.138 Uiso 1 1 calc R U . . . C8 C 1.09741(16) 0.43300(14) 0.19292(14) 0.0440(5) Uani 1 1 d . . . . . C9 C 1.11072(18) 0.35825(15) 0.14784(16) 0.0525(6) Uani 1 1 d . . . . . H9 H 1.060307 0.305262 0.151201 0.063 Uiso 1 1 calc R U . . . C19 C 0.84318(14) 0.59853(12) 0.22412(12) 0.0343(4) Uani 1 1 d . . . . . C10 C 1.1981(2) 0.36098(18) 0.09764(17) 0.0587(6) Uani 1 1 d . . . . . H10 H 1.206699 0.309447 0.067092 0.070 Uiso 1 1 calc R U . . . C24 C 0.93073(17) 0.81420(14) 0.35275(13) 0.0438(5) Uani 1 1 d . . . . . H24 H 0.990667 0.844723 0.388644 0.053 Uiso 1 1 calc R U . . . C11 C 1.27284(18) 0.43751(19) 0.09135(16) 0.0573(6) Uani 1 1 d . . . . . C12 C 1.25818(17) 0.51206(17) 0.13645(16) 0.0545(6) Uani 1 1 d . . . . . H12 H 1.308240 0.565104 0.132707 0.065 Uiso 1 1 calc R U . . . C13 C 1.17157(17) 0.51028(15) 0.18689(15) 0.0479(5) Uani 1 1 d . . . . . H13 H 1.162884 0.561840 0.217333 0.057 Uiso 1 1 calc R U . . . C14 C 1.3695(2) 0.4405(2) 0.03851(19) 0.0734(9) Uani 1 1 d . . . . . H14A H 1.378940 0.489751 0.009931 0.110 Uiso 1 1 calc R U . . . H14B H 1.356055 0.387762 -0.000351 0.110 Uiso 1 1 calc R U . . . H14C H 1.435977 0.445843 0.071726 0.110 Uiso 1 1 calc R U . . . C15 C 0.92792(15) 0.47690(13) 0.21318(13) 0.0390(4) Uani 1 1 d . . . . . C16 C 0.86918(16) 0.44135(13) 0.14212(13) 0.0415(4) Uani 1 1 d . . . . . H16 H 0.874363 0.386915 0.115842 0.050 Uiso 1 1 calc R U . . . C17 C 0.80176(16) 0.48541(13) 0.10854(13) 0.0404(4) Uani 1 1 d . . . . . H17 H 0.764298 0.462470 0.057954 0.048 Uiso 1 1 calc R U . . . C18 C 0.78981(14) 0.56208(13) 0.14895(12) 0.0361(4) Uani 1 1 d . . . . . H18 H 0.743972 0.591373 0.125286 0.043 Uiso 1 1 calc R U . . . C20 C 0.91897(14) 0.55624(13) 0.25529(12) 0.0361(4) Uani 1 1 d . . . . . C22 C 0.99402(15) 0.68171(14) 0.35270(12) 0.0396(4) Uani 1 1 d . . . . . H22 H 1.047563 0.711017 0.393955 0.048 Uiso 1 1 calc R U . . . C21 C 0.98979(15) 0.59878(14) 0.32330(12) 0.0397(4) Uani 1 1 d . . . . . H21 H 1.034069 0.569070 0.348056 0.048 Uiso 1 1 calc R U . . . C26 C 0.75945(16) 0.81013(13) 0.28185(12) 0.0380(4) Uani 1 1 d . . . . . C25 C 0.85644(17) 0.85547(13) 0.33029(13) 0.0440(5) Uani 1 1 d . . . . . H25 H 0.868700 0.915385 0.346854 0.053 Uiso 1 1 calc R U . . . C28 C 0.57487(15) 0.80825(13) 0.22635(11) 0.0353(4) Uani 1 1 d . . . . . C27 C 0.67741(16) 0.85095(13) 0.26671(12) 0.0382(4) Uani 1 1 d . . . . . H27 H 0.690898 0.910747 0.284413 0.046 Uiso 1 1 calc R U . . . C29 C 0.56269(15) 0.71842(13) 0.20195(11) 0.0347(4) Uani 1 1 d . . . . . H29 H 0.494780 0.685648 0.176551 0.042 Uiso 1 1 calc R U . . . C30 C 0.64296(14) 0.67701(12) 0.21303(11) 0.0336(4) Uani 1 1 d . . . . . H30 H 0.629025 0.617344 0.194452 0.040 Uiso 1 1 calc R U . . . C32 C 0.83456(14) 0.68142(12) 0.26614(11) 0.0343(4) Uani 1 1 d . . . . . C31 C 0.74738(15) 0.72081(12) 0.25177(11) 0.0341(4) Uani 1 1 d . . . . . C34 C 0.48668(16) 1.01221(13) 0.20615(12) 0.0380(4) Uani 1 1 d . . . . . C33 C 0.49394(16) 0.94901(13) 0.25470(12) 0.0381(4) Uani 1 1 d . . . . . C37 C 0.5282(2) 1.06445(16) 0.36880(13) 0.0510(5) Uani 1 1 d . . . . . H37 H 0.543396 1.081891 0.424823 0.061 Uiso 1 1 calc R U . . . C36 C 0.52040(19) 1.12577(15) 0.32146(13) 0.0472(5) Uani 1 1 d . . . . . C35 C 0.50014(17) 1.09743(14) 0.23975(13) 0.0419(4) Uani 1 1 d . . . . . H35 H 0.495278 1.137840 0.205452 0.050 Uiso 1 1 calc R U . . . C39 C 0.5191(2) 0.91878(17) 0.39768(14) 0.0569(6) Uani 1 1 d . . . . . H39A H 0.584744 0.942005 0.433484 0.085 Uiso 1 1 calc R U . . . H39B H 0.521631 0.862521 0.369118 0.085 Uiso 1 1 calc R U . . . H39C H 0.453588 0.913057 0.429264 0.085 Uiso 1 1 calc R U . . . C38 C 0.51488(19) 0.97859(15) 0.33776(13) 0.0457(5) Uani 1 1 d . . . . . C50 C 0.26747(18) 0.81896(16) 0.29943(13) 0.0475(5) Uani 1 1 d . . . . . H50A H 0.297118 0.881041 0.305624 0.071 Uiso 1 1 calc R U . . . H50B H 0.312057 0.794290 0.332814 0.071 Uiso 1 1 calc R U . . . H50C H 0.191672 0.806431 0.316159 0.071 Uiso 1 1 calc R U . . . C49 C 0.05910(16) 0.63353(15) 0.05745(15) 0.0475(5) Uani 1 1 d . . . . . H49A H 0.002218 0.629704 0.096823 0.071 Uiso 1 1 calc R U . . . H49B H 0.070160 0.576417 0.039322 0.071 Uiso 1 1 calc R U . . . H49C H 0.036156 0.656711 0.011487 0.071 Uiso 1 1 calc R U . . . C48 C 0.45748(16) 0.77180(14) 0.03703(12) 0.0403(4) Uani 1 1 d . . . . . H48A H 0.523432 0.803638 0.069798 0.060 Uiso 1 1 calc R U . . . H48B H 0.444985 0.803904 -0.005513 0.060 Uiso 1 1 calc R U . . . H48C H 0.467350 0.715840 0.013002 0.060 Uiso 1 1 calc R U . . . C47 C 0.35959(15) 0.75949(12) 0.08926(12) 0.0352(4) Uani 1 1 d . . . . . C46 C 0.25988(15) 0.70985(12) 0.05290(12) 0.0366(4) Uani 1 1 d . . . . . H46 H 0.256500 0.687760 -0.002603 0.044 Uiso 1 1 calc R U . . . C45 C 0.16531(15) 0.69184(13) 0.09564(13) 0.0388(4) Uani 1 1 d . . . . . C44 C 0.17281(15) 0.72825(13) 0.17559(13) 0.0393(4) Uani 1 1 d . . . . . H44 H 0.109447 0.717081 0.206146 0.047 Uiso 1 1 calc R U . . . C43 C 0.26990(16) 0.78059(13) 0.21264(12) 0.0373(4) Uani 1 1 d . . . . . C42 C 0.36803(15) 0.79656(12) 0.17071(11) 0.0346(4) Uani 1 1 d . . . . . C41 C 0.46843(18) 0.98817(14) 0.11648(12) 0.0425(4) Uani 1 1 d . . . . . H41A H 0.470220 1.039603 0.092334 0.064 Uiso 1 1 calc R U . . . H41B H 0.396878 0.947560 0.103775 0.064 Uiso 1 1 calc R U . . . H41C H 0.526320 0.961702 0.095023 0.064 Uiso 1 1 calc R U . . . C40 C 0.5300(2) 1.21784(16) 0.35744(16) 0.0595(6) Uani 1 1 d . . . . . H40A H 0.576433 1.255673 0.324734 0.089 Uiso 1 1 calc R U . . . H40B H 0.562761 1.228453 0.412086 0.089 Uiso 1 1 calc R U . . . H40C H 0.456879 1.229141 0.358837 0.089 Uiso 1 1 calc R U . . . K1_1 K 1.000000 1.000000 0.000000 0.0543(2) Uani 1 2 d S . P . . C1_1 C 0.73300(18) 0.85110(17) -0.0223(2) 0.0625(7) Uani 1 1 d . . . . . H1A_1 H 0.702163 0.893622 0.011745 0.075 Uiso 1 1 calc R U . . . H1AB_1 H 0.681703 0.794136 -0.024547 0.075 Uiso 1 1 calc R U . . . O2_1 O 1.00836(13) 0.91467(11) 0.13108(13) 0.0620(5) Uani 1 1 d . . . . . C2_1 C 0.8312(2) 0.82735(17) 0.08904(18) 0.0625(7) Uani 1 1 d . . . . . H2A_1 H 0.782446 0.769463 0.087451 0.075 Uiso 1 1 calc R U . . . H2AB_1 H 0.800682 0.868327 0.125378 0.075 Uiso 1 1 calc R U . . . O3_1 O 1.19354(13) 1.03998(12) 0.09891(13) 0.0649(5) Uani 1 1 d . . . . . C3_1 C 0.9445(2) 0.82880(17) 0.11911(18) 0.0615(7) Uani 1 1 d . . . . . H3A_1 H 0.940957 0.805398 0.170205 0.074 Uiso 1 1 calc R U . . . H3AB_1 H 0.978323 0.793061 0.079564 0.074 Uiso 1 1 calc R U . . . O4A_1 O 0.9207(3) 1.1107(2) 0.1091(2) 0.0738(7) Uani 0.793(6) 1 d D U P A 1 C7A_1 C 0.8434(4) 1.1498(3) 0.0773(3) 0.0751(8) Uani 0.793(6) 1 d D U P A 1 H7AA_1 H 0.805914 1.113679 0.027794 0.090 Uiso 0.793(6) 1 calc R U P A 1 H7AB_1 H 0.881200 1.206406 0.063929 0.090 Uiso 0.793(6) 1 calc R U P A 1 C8A_1 C 0.7636(3) 1.1596(3) 0.1379(3) 0.0763(8) Uani 0.793(6) 1 d D U P A 1 H8AA_1 H 0.689039 1.149600 0.112904 0.092 Uiso 0.793(6) 1 calc R U P A 1 H8AB_1 H 0.783852 1.217328 0.170239 0.092 Uiso 0.793(6) 1 calc R U P A 1 C9A_1 C 0.7704(3) 1.0885(3) 0.1907(3) 0.0713(8) Uani 0.793(6) 1 d D U P A 1 H9AA_1 H 0.747422 1.102683 0.245812 0.086 Uiso 0.793(6) 1 calc R U P A 1 H9AB_1 H 0.725769 1.031466 0.166115 0.086 Uiso 0.793(6) 1 calc R U P A 1 C10A_1 C 0.8900(3) 1.0930(4) 0.1892(3) 0.0730(8) Uani 0.793(6) 1 d D U P A 1 H10A_1 H 0.931469 1.139261 0.230793 0.088 Uiso 0.793(6) 1 calc R U P A 1 H10B_1 H 0.904736 1.038136 0.198625 0.088 Uiso 0.793(6) 1 calc R U P A 1 O4B_1 O 0.8731(10) 1.0712(8) 0.0861(6) 0.0738(10) Uani 0.207(6) 1 d D U P A 2 C8B_1 C 0.7364(11) 1.1378(13) 0.1309(9) 0.0753(11) Uani 0.207(6) 1 d D U P A 2 H8BA_1 H 0.665391 1.094453 0.122260 0.090 Uiso 0.207(6) 1 calc R U P A 2 H8BB_1 H 0.721994 1.195461 0.137441 0.090 Uiso 0.207(6) 1 calc R U P A 2 C7B_1 C 0.8076(13) 1.1263(12) 0.0621(7) 0.0746(10) Uani 0.207(6) 1 d D U P A 2 H7BA_1 H 0.762795 1.099000 0.012300 0.089 Uiso 0.207(6) 1 calc R U P A 2 H7BB_1 H 0.854874 1.181882 0.053175 0.089 Uiso 0.207(6) 1 calc R U P A 2 C9B_1 C 0.7993(13) 1.1269(13) 0.2032(6) 0.0739(10) Uani 0.207(6) 1 d D U P A 2 H9BA_1 H 0.755461 1.081199 0.230488 0.089 Uiso 0.207(6) 1 calc R U P A 2 H9BB_1 H 0.818967 1.180828 0.241676 0.089 Uiso 0.207(6) 1 calc R U P A 2 C10B_1 C 0.9016(12) 1.1028(14) 0.1709(8) 0.0735(10) Uani 0.207(6) 1 d D U P A 2 H10C_1 H 0.965166 1.153173 0.177982 0.088 Uiso 0.207(6) 1 calc R U P A 2 H10D_1 H 0.919530 1.057793 0.198385 0.088 Uiso 0.207(6) 1 calc R U P A 2 C5_1 C 1.1768(2) 1.0136(2) 0.1753(2) 0.0728(8) Uani 1 1 d . . . . . H5A_1 H 1.134649 1.049187 0.207718 0.087 Uiso 1 1 calc R U . . . H5AB_1 H 1.248381 1.020919 0.204027 0.087 Uiso 1 1 calc R U . . . C6_1 C 1.2531(2) 1.12633(18) 0.1042(2) 0.0662(7) Uani 1 1 d . . . . . H6A_1 H 1.325830 1.134398 0.131520 0.079 Uiso 1 1 calc R U . . . H6AB_1 H 1.213107 1.164133 0.135959 0.079 Uiso 1 1 calc R U . . . C4_1 C 1.1154(2) 0.9221(2) 0.1645(2) 0.0727(9) Uani 1 1 d . . . . . H4A_1 H 1.154306 0.887033 0.128371 0.087 Uiso 1 1 calc R U . . . H4AB_1 H 1.110236 0.901183 0.216906 0.087 Uiso 1 1 calc R U . . . O1_1 O 0.83723(12) 0.85015(11) 0.01086(11) 0.0562(4) Uani 1 1 d . . . . . K1_2 K 0.500000 0.500000 0.500000 0.05184(19) Uani 1 2 d S . P . . C1_2 C 0.7830(2) 0.4830(2) 0.52711(16) 0.0607(7) Uani 1 1 d . . . . . H1A_2 H 0.861541 0.507107 0.543241 0.073 Uiso 1 1 calc R U . . . H1AB_2 H 0.777580 0.446782 0.474081 0.073 Uiso 1 1 calc R U . . . O2_2 O 0.61310(13) 0.63546(11) 0.43169(9) 0.0509(4) Uani 1 1 d . . . . . C2_2 C 0.78106(19) 0.60622(18) 0.46889(14) 0.0531(6) Uani 1 1 d . . . . . H2A_2 H 0.780186 0.573536 0.414541 0.064 Uiso 1 1 calc R U . . . H2AB_2 H 0.858345 0.632930 0.487347 0.064 Uiso 1 1 calc R U . . . O3_2 O 0.38181(13) 0.60971(12) 0.44051(9) 0.0538(4) Uani 1 1 d . . . . . C3_2 C 0.7197(2) 0.67354(18) 0.46669(14) 0.0545(6) Uani 1 1 d . . . . . H3A_2 H 0.714758 0.702509 0.521795 0.065 Uiso 1 1 calc R U . . . H3AB_2 H 0.758999 0.716890 0.434910 0.065 Uiso 1 1 calc R U . . . O4_2 O 0.48418(14) 0.42727(12) 0.34042(11) 0.0600(4) Uani 1 1 d . . . . . C5_2 C 0.4434(2) 0.65139(17) 0.38148(14) 0.0525(6) Uani 1 1 d . . . . . H5A_2 H 0.405919 0.692586 0.363077 0.063 Uiso 1 1 calc R U . . . H5AB_2 H 0.449432 0.608740 0.334677 0.063 Uiso 1 1 calc R U . . . C6_2 C 0.2720(2) 0.5693(2) 0.41233(16) 0.0597(6) Uani 1 1 d . . . . . H6A_2 H 0.271626 0.532169 0.360371 0.072 Uiso 1 1 calc R U . . . H6AB_2 H 0.232074 0.613085 0.404160 0.072 Uiso 1 1 calc R U . . . C7_2 C 0.3939(2) 0.3869(2) 0.2852(2) 0.0718(8) Uani 1 1 d . . . . . H7A_2 H 0.358927 0.430050 0.267878 0.086 Uiso 1 1 calc R U . . . H7AB_2 H 0.338477 0.345850 0.310352 0.086 Uiso 1 1 calc R U . . . C8_2 C 0.4386(2) 0.34155(17) 0.21551(16) 0.0574(6) Uani 1 1 d . . . . . H8A_2 H 0.387527 0.324683 0.167560 0.069 Uiso 1 1 calc R U . B 1 H8AB_2 H 0.464012 0.291827 0.228319 0.069 Uiso 1 1 calc R U . B 1 C10_2 C 0.5808(2) 0.44416(17) 0.29633(17) 0.0616(6) Uani 1 1 d . . . . . H10A_2 H 0.630539 0.408205 0.307904 0.074 Uiso 1 1 calc R U . C 1 H10B_2 H 0.620766 0.505181 0.307959 0.074 Uiso 1 1 calc R U . C 1 C9A_2 C 0.5331(8) 0.4199(7) 0.2095(5) 0.0642(16) Uani 0.401(12) 1 d . U P D 1 H9AA_2 H 0.588050 0.405050 0.172257 0.077 Uiso 0.401(12) 1 calc R U P D 1 H9AB_2 H 0.505836 0.466801 0.191936 0.077 Uiso 0.401(12) 1 calc R U P D 1 C9B_2 C 0.5620(5) 0.3867(5) 0.2157(4) 0.0636(13) Uani 0.599(12) 1 d . U P D 2 H9BA_2 H 0.608021 0.344999 0.211924 0.076 Uiso 0.599(12) 1 calc R U P D 2 H9BB_2 H 0.577376 0.420475 0.171136 0.076 Uiso 0.599(12) 1 calc R U P D 2 C4_2 C 0.5552(2) 0.69737(16) 0.41661(14) 0.0528(5) Uani 1 1 d . . . . . H4A_2 H 0.595107 0.733486 0.378855 0.063 Uiso 1 1 calc R U . . . H4AB_2 H 0.549268 0.734818 0.467235 0.063 Uiso 1 1 calc R U . . . O1_2 O 0.73002(13) 0.55037(12) 0.52253(9) 0.0534(4) Uani 1 1 d . . . . . C1A_3 C 1.0706(6) 1.0551(6) 0.3716(5) 0.0804(16) Uani 0.375(2) 1 d D U P E 1 H1AA_3 H 1.057376 1.003847 0.329891 0.096 Uiso 0.375(2) 1 calc R U P E 1 H1AB_3 H 1.009078 1.082728 0.368367 0.096 Uiso 0.375(2) 1 calc R U P E 1 C2A_3 C 1.0809(6) 1.0305(6) 0.4542(5) 0.0837(16) Uani 0.375(2) 1 d D U P E 1 H2AA_3 H 1.026031 0.977296 0.460397 0.100 Uiso 0.375(2) 1 calc R U P E 1 H2AB_3 H 1.074327 1.076944 0.497323 0.100 Uiso 0.375(2) 1 calc R U P E 1 O1A_3 O 1.1693(5) 1.1116(4) 0.3612(4) 0.0778(13) Uani 0.375(2) 1 d D U P E 1 C4A_3 C 1.2575(5) 1.0833(5) 0.4065(6) 0.0660(14) Uani 0.375(2) 1 d D U P E 1 H4A1_3 H 1.305850 1.060108 0.368243 0.079 Uiso 0.375(2) 1 calc R U P E 1 H4A2_3 H 1.303123 1.132640 0.443115 0.079 Uiso 0.375(2) 1 calc R U P E 1 C3A_3 C 1.2010(7) 1.0172(7) 0.4525(7) 0.0758(15) Uani 0.375(2) 1 d D U P E 1 H3A1_3 H 1.234888 1.026049 0.507302 0.091 Uiso 0.375(2) 1 calc R U P E 1 H3A2_3 H 1.201648 0.959230 0.425291 0.091 Uiso 0.375(2) 1 calc R U P E 1 C5B_3 C 1.1233(5) 0.9757(4) 0.4511(4) 0.0615(12) Uani 0.482(3) 1 d D U P F 2 H5B1_3 H 1.088131 0.972862 0.503118 0.074 Uiso 0.482(3) 1 calc R U P F 2 H5B2_3 H 1.105102 0.917648 0.419246 0.074 Uiso 0.482(3) 1 calc R U P F 2 C1B_3 C 1.0853(5) 1.0369(4) 0.4070(5) 0.0708(12) Uani 0.482(3) 1 d D U P F 2 H1BA_3 H 1.077232 1.015029 0.348792 0.085 Uiso 0.482(3) 1 calc R U P F 2 H1BB_3 H 1.013035 1.043688 0.425435 0.085 Uiso 0.482(3) 1 calc R U P F 2 O2B_3 O 1.1672(4) 1.1206(3) 0.4223(4) 0.0838(12) Uani 0.482(3) 1 d D U P F 2 C3B_3 C 1.2618(5) 1.0999(4) 0.4608(5) 0.0781(13) Uani 0.482(3) 1 d D U P F 2 H3BA_3 H 1.327982 1.117709 0.430314 0.094 Uiso 0.482(3) 1 calc R U P F 2 H3BB_3 H 1.276135 1.131760 0.515993 0.094 Uiso 0.482(3) 1 calc R U P F 2 C4B_3 C 1.2397(4) 1.0078(3) 0.4634(4) 0.0611(12) Uani 0.482(3) 1 d D U P F 2 H4B1_3 H 1.277968 0.979690 0.420704 0.073 Uiso 0.482(3) 1 calc R U P F 2 H4B2_3 H 1.264872 0.997294 0.515929 0.073 Uiso 0.482(3) 1 calc R U P F 2 C4C_3 C 1.2375(18) 1.1031(9) 0.3733(11) 0.075(2) Uani 0.144(2) 1 d D U P G 3 H4CA_3 H 1.225533 1.133427 0.328470 0.090 Uiso 0.144(2) 1 calc R U P G 3 H4CB_3 H 1.317101 1.115705 0.387015 0.090 Uiso 0.144(2) 1 calc R U P G 3 O1C_3 O 1.1390(14) 0.9779(8) 0.4219(9) 0.0695(18) Uani 0.144(2) 1 d D U P G 3 C2C_3 C 1.1664(18) 1.0493(11) 0.4879(7) 0.0785(17) Uani 0.144(2) 1 d D U P G 3 H2CA_3 H 1.236988 1.051517 0.515768 0.094 Uiso 0.144(2) 1 calc R U P G 3 H2CB_3 H 1.108268 1.044763 0.527137 0.094 Uiso 0.144(2) 1 calc R U P G 3 C3C_3 C 1.175(2) 1.1286(9) 0.4462(12) 0.0802(18) Uani 0.144(2) 1 d D U P G 3 H3CA_3 H 1.101484 1.135283 0.430453 0.096 Uiso 0.144(2) 1 calc R U P G 3 H3CB_3 H 1.216407 1.181645 0.480038 0.096 Uiso 0.144(2) 1 calc R U P G 3 C5C_3 C 1.1890(14) 1.0084(9) 0.3523(8) 0.0647(17) Uani 0.144(2) 1 d D U P G 3 H5CA_3 H 1.133408 0.996776 0.307350 0.078 Uiso 0.144(2) 1 calc R U P G 3 H5CB_3 H 1.247108 0.978953 0.335531 0.078 Uiso 0.144(2) 1 calc R U P G 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0370(10) 0.0387(10) 0.0495(11) 0.0137(9) -0.0037(8) 0.0107(8) N1 0.0307(8) 0.0448(9) 0.0630(11) 0.0253(8) 0.0058(7) 0.0175(7) B1 0.0359(10) 0.0422(12) 0.0367(10) 0.0144(9) 0.0043(8) 0.0166(9) C2 0.0429(12) 0.0752(17) 0.0679(15) 0.0387(13) 0.0081(10) 0.0201(11) C23 0.0281(9) 0.0448(11) 0.0452(10) 0.0166(9) -0.0004(7) 0.0102(8) C3 0.0570(15) 0.101(2) 0.086(2) 0.0567(19) 0.0159(14) 0.0169(15) C4 0.0796(18) 0.0562(15) 0.0510(13) 0.0245(11) -0.0088(12) 0.0055(13) C5 0.0685(15) 0.0416(12) 0.0614(14) 0.0148(10) -0.0222(12) 0.0113(11) C6 0.0442(12) 0.0448(12) 0.0728(15) 0.0227(11) -0.0103(10) 0.0117(9) C7 0.127(3) 0.078(2) 0.0663(18) 0.0411(16) -0.0085(18) 0.000(2) C8 0.0303(9) 0.0484(12) 0.0632(13) 0.0263(10) 0.0050(9) 0.0183(8) C9 0.0368(11) 0.0478(12) 0.0814(16) 0.0237(12) 0.0096(10) 0.0184(9) C19 0.0237(8) 0.0397(10) 0.0450(10) 0.0186(8) 0.0047(7) 0.0111(7) C10 0.0461(12) 0.0651(15) 0.0793(17) 0.0248(13) 0.0135(11) 0.0328(11) C24 0.0365(10) 0.0438(11) 0.0501(11) 0.0120(9) -0.0103(8) 0.0056(8) C11 0.0376(11) 0.0809(17) 0.0717(15) 0.0416(14) 0.0099(10) 0.0319(11) C12 0.0323(10) 0.0648(15) 0.0769(16) 0.0422(13) 0.0029(10) 0.0135(10) C13 0.0372(10) 0.0498(12) 0.0650(13) 0.0269(10) 0.0030(9) 0.0159(9) C14 0.0446(13) 0.116(2) 0.0836(19) 0.0561(18) 0.0206(12) 0.0417(15) C15 0.0279(9) 0.0435(11) 0.0533(11) 0.0220(9) 0.0070(8) 0.0145(8) C16 0.0346(9) 0.0392(10) 0.0566(12) 0.0149(9) 0.0078(8) 0.0155(8) C17 0.0323(9) 0.0435(11) 0.0488(11) 0.0119(9) 0.0014(8) 0.0133(8) C18 0.0268(8) 0.0402(10) 0.0472(10) 0.0162(8) 0.0039(7) 0.0135(7) C20 0.0270(8) 0.0423(10) 0.0453(10) 0.0194(8) 0.0049(7) 0.0127(7) C22 0.0270(9) 0.0498(12) 0.0455(10) 0.0191(9) -0.0017(7) 0.0094(8) C21 0.0275(9) 0.0518(12) 0.0475(11) 0.0238(9) 0.0030(7) 0.0151(8) C26 0.0351(9) 0.0380(10) 0.0433(10) 0.0118(8) -0.0031(8) 0.0107(8) C25 0.0440(11) 0.0356(10) 0.0523(12) 0.0090(9) -0.0093(9) 0.0088(8) C28 0.0330(9) 0.0397(10) 0.0385(9) 0.0133(8) 0.0017(7) 0.0145(8) C27 0.0394(10) 0.0355(10) 0.0430(10) 0.0091(8) -0.0028(8) 0.0140(8) C29 0.0272(8) 0.0401(10) 0.0399(9) 0.0112(8) 0.0010(7) 0.0109(7) C30 0.0286(8) 0.0337(9) 0.0410(9) 0.0098(7) 0.0015(7) 0.0102(7) C32 0.0266(8) 0.0375(10) 0.0420(10) 0.0150(8) 0.0015(7) 0.0090(7) C31 0.0301(9) 0.0371(10) 0.0392(9) 0.0133(8) 0.0013(7) 0.0119(7) C34 0.0347(9) 0.0448(11) 0.0412(10) 0.0138(8) 0.0027(7) 0.0179(8) C33 0.0363(9) 0.0449(11) 0.0397(10) 0.0118(8) 0.0030(8) 0.0193(8) C37 0.0664(14) 0.0544(13) 0.0384(11) 0.0067(9) 0.0006(10) 0.0270(11) C36 0.0544(12) 0.0454(12) 0.0475(11) 0.0090(9) 0.0039(9) 0.0224(10) C35 0.0433(11) 0.0429(11) 0.0466(11) 0.0153(9) 0.0026(8) 0.0194(9) C39 0.0844(18) 0.0582(14) 0.0391(11) 0.0130(10) -0.0004(11) 0.0353(13) C38 0.0542(12) 0.0499(12) 0.0410(10) 0.0131(9) 0.0016(9) 0.0247(10) C50 0.0438(11) 0.0625(14) 0.0454(11) 0.0193(10) 0.0114(9) 0.0241(10) C49 0.0313(10) 0.0496(12) 0.0639(13) 0.0181(10) 0.0063(9) 0.0085(9) C48 0.0320(9) 0.0468(11) 0.0432(10) 0.0078(8) 0.0057(8) 0.0110(8) C47 0.0309(9) 0.0357(9) 0.0451(10) 0.0150(8) 0.0057(7) 0.0146(7) C46 0.0323(9) 0.0366(10) 0.0452(10) 0.0136(8) 0.0043(8) 0.0125(7) C45 0.0304(9) 0.0386(10) 0.0545(11) 0.0205(9) 0.0053(8) 0.0140(8) C44 0.0316(9) 0.0441(11) 0.0519(11) 0.0245(9) 0.0110(8) 0.0173(8) C43 0.0364(9) 0.0424(10) 0.0436(10) 0.0203(8) 0.0087(8) 0.0214(8) C42 0.0318(9) 0.0372(10) 0.0430(10) 0.0162(8) 0.0044(7) 0.0183(7) C41 0.0457(11) 0.0438(11) 0.0427(11) 0.0142(9) 0.0014(8) 0.0154(9) C40 0.0785(17) 0.0490(13) 0.0549(13) 0.0054(11) 0.0026(12) 0.0243(12) K1_1 0.0328(3) 0.0507(4) 0.0919(5) 0.0399(4) 0.0159(3) 0.0165(3) C1_1 0.0337(11) 0.0510(13) 0.109(2) 0.0298(14) 0.0173(12) 0.0116(10) O2_1 0.0438(8) 0.0543(10) 0.1020(14) 0.0438(10) 0.0133(8) 0.0197(7) C2_1 0.0511(13) 0.0560(14) 0.0867(18) 0.0369(13) 0.0254(13) 0.0085(11) O3_1 0.0396(8) 0.0572(10) 0.1073(15) 0.0405(10) 0.0055(9) 0.0137(7) C3_1 0.0582(14) 0.0522(14) 0.0876(18) 0.0421(13) 0.0228(13) 0.0197(11) O4A_1 0.0584(13) 0.0818(16) 0.0929(14) 0.0288(12) 0.0195(11) 0.0297(12) C7A_1 0.0619(15) 0.0824(18) 0.0933(16) 0.0326(14) 0.0153(13) 0.0293(14) C8A_1 0.0599(15) 0.0877(18) 0.0918(16) 0.0292(14) 0.0122(13) 0.0287(14) C9A_1 0.0558(14) 0.0849(18) 0.0842(15) 0.0288(14) 0.0107(12) 0.0283(13) C10A_1 0.0591(14) 0.0835(17) 0.0849(16) 0.0248(14) 0.0097(13) 0.0265(13) O4B_1 0.0609(17) 0.0828(19) 0.0889(18) 0.0282(17) 0.0131(16) 0.0298(16) C8B_1 0.0596(18) 0.086(2) 0.0904(18) 0.0302(17) 0.0116(16) 0.0269(17) C7B_1 0.0601(18) 0.084(2) 0.0910(18) 0.0297(17) 0.0131(16) 0.0296(17) C9B_1 0.0588(18) 0.085(2) 0.0874(18) 0.0277(17) 0.0113(16) 0.0278(17) C10B_1 0.0593(17) 0.0838(19) 0.0875(18) 0.0275(17) 0.0105(16) 0.0284(17) C5_1 0.0470(13) 0.0720(18) 0.112(2) 0.0498(17) 0.0002(14) 0.0189(12) C6_1 0.0401(12) 0.0545(14) 0.112(2) 0.0370(15) 0.0020(13) 0.0126(10) C4_1 0.0464(13) 0.0714(18) 0.118(2) 0.0542(17) 0.0087(14) 0.0253(12) O1_1 0.0372(8) 0.0537(9) 0.0868(12) 0.0348(9) 0.0189(8) 0.0134(7) K1_2 0.0435(3) 0.0766(5) 0.0503(4) 0.0346(3) 0.0111(3) 0.0281(3) C1_2 0.0453(12) 0.0885(19) 0.0625(14) 0.0244(13) 0.0089(10) 0.0360(13) O2_2 0.0503(9) 0.0607(10) 0.0500(8) 0.0219(7) 0.0059(7) 0.0214(7) C2_2 0.0461(12) 0.0747(16) 0.0429(11) 0.0176(11) 0.0065(9) 0.0180(11) O3_2 0.0518(9) 0.0755(11) 0.0470(8) 0.0240(8) 0.0061(7) 0.0319(8) C3_2 0.0562(13) 0.0699(16) 0.0412(11) 0.0152(11) 0.0064(10) 0.0182(12) O4_2 0.0539(9) 0.0656(11) 0.0620(10) 0.0147(8) 0.0079(8) 0.0146(8) C5_2 0.0626(14) 0.0610(14) 0.0473(12) 0.0230(10) 0.0060(10) 0.0322(12) C6_2 0.0487(13) 0.0849(18) 0.0612(14) 0.0270(13) 0.0022(10) 0.0370(13) C7_2 0.0528(14) 0.086(2) 0.0842(19) 0.0103(16) -0.0040(13) 0.0341(14) C8_2 0.0512(13) 0.0584(14) 0.0668(15) 0.0177(12) -0.0025(11) 0.0171(11) C10_2 0.0548(14) 0.0518(14) 0.0756(17) 0.0120(12) 0.0130(12) 0.0060(11) C9A_2 0.056(4) 0.072(4) 0.065(3) 0.016(3) 0.009(3) 0.012(3) C9B_2 0.052(3) 0.075(4) 0.066(2) 0.018(3) 0.008(2) 0.016(2) C4_2 0.0651(14) 0.0549(13) 0.0486(12) 0.0159(10) 0.0086(10) 0.0292(11) O1_2 0.0445(8) 0.0793(11) 0.0491(8) 0.0262(8) 0.0113(6) 0.0299(8) C1A_3 0.079(3) 0.072(3) 0.093(3) 0.018(3) -0.010(3) 0.023(3) C2A_3 0.075(3) 0.075(3) 0.098(3) 0.020(3) -0.011(3) 0.010(3) O1A_3 0.074(2) 0.082(3) 0.084(3) 0.023(2) -0.004(2) 0.026(2) C4A_3 0.060(2) 0.054(2) 0.085(3) 0.016(3) 0.011(3) 0.013(2) C3A_3 0.065(3) 0.068(2) 0.094(3) 0.021(2) -0.012(3) 0.012(2) C5B_3 0.049(2) 0.052(2) 0.087(3) 0.031(2) -0.001(2) 0.0057(19) C1B_3 0.065(2) 0.067(2) 0.085(3) 0.030(2) -0.017(2) 0.0156(19) O2B_3 0.079(2) 0.078(2) 0.097(3) 0.024(2) -0.022(2) 0.0184(17) C3B_3 0.072(2) 0.063(2) 0.101(3) 0.034(2) -0.027(3) 0.011(2) C4B_3 0.047(2) 0.049(2) 0.091(3) 0.018(2) 0.001(2) 0.014(2) C4C_3 0.067(4) 0.072(4) 0.090(4) 0.025(4) -0.013(4) 0.020(3) O1C_3 0.059(3) 0.057(3) 0.094(4) 0.023(3) -0.008(3) 0.011(3) C2C_3 0.070(3) 0.069(3) 0.096(3) 0.021(3) -0.010(3) 0.013(3) C3C_3 0.073(3) 0.072(3) 0.095(3) 0.021(3) -0.012(3) 0.014(3) C5C_3 0.059(3) 0.058(3) 0.085(3) 0.024(3) -0.007(3) 0.020(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -1 1 0.0762 -4 -7 -3 0.0522 -2 -3 -9 0.0586 -1 -2 0 0.0649 0 -2 -1 0.0344 0 -2 -1 0.0331 0 -1 -1 0.0316 -1 0 0 0.0956 1 -1 0 0.0918 0 0 0 0.1202 0 -1 0 0.0604 0 -1 -1 0.0448 0 1 -1 0.1558 0 -1 0 0.0587 0 -1 1 0.0955 -3 -5 -7 0.0493 0 2 1 0.0214 1 -1 0 0.1029 0 1 1 0.0410 -1 1 -1 0.1078 -1 0 0 0.0962 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 N1 121.56(18) . . ? C2 C1 C6 117.4(2) . . ? N1 C1 C6 121.05(19) . . ? C1 N1 C8 121.91(16) . . ? C1 N1 C15 119.28(16) . . ? C8 N1 C15 114.32(16) . . ? C28 B1 C33 119.97(18) . . ? C28 B1 C42 119.51(18) . . ? C33 B1 C42 120.48(16) . . ? C1 C2 C3 120.8(2) . . ? C1 C2 H2 119.6 . . ? C3 C2 H2 119.6 . . ? C22 C23 C24 120.81(18) . . ? C22 C23 C32 119.81(19) . . ? C24 C23 C32 119.36(17) . . ? C4 C3 C2 122.3(3) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C5 C4 C3 116.5(2) . . ? C5 C4 C7 123.1(3) . . ? C3 C4 C7 120.3(3) . . ? C4 C5 C6 122.6(2) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 120.4(2) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 119.4(2) . . ? C9 C8 N1 122.09(19) . . ? C13 C8 N1 118.5(2) . . ? C8 C9 C10 119.9(2) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C18 C19 C20 117.49(18) . . ? C18 C19 C32 122.74(16) . . ? C20 C19 C32 119.36(17) . . ? C11 C10 C9 121.3(3) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C25 C24 C23 121.38(19) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C10 C11 C12 118.2(2) . . ? C10 C11 C14 121.5(3) . . ? C12 C11 C14 120.3(3) . . ? C13 C12 C11 121.1(2) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C8 120.1(2) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 121.47(17) . . ? C16 C15 N1 118.74(19) . . ? C20 C15 N1 119.66(18) . . ? C15 C16 C17 119.92(19) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 119.8(2) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 122.24(17) . . ? C17 C18 H18 118.9 . . ? C19 C18 H18 118.9 . . ? C15 C20 C21 121.70(17) . . ? C15 C20 C19 118.72(18) . . ? C21 C20 C19 119.33(18) . . ? C21 C22 C23 122.07(19) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C22 C21 C20 120.12(17) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C27 C26 C25 120.73(19) . . ? C27 C26 C31 120.91(18) . . ? C25 C26 C31 118.33(17) . . ? C24 C25 C26 121.13(19) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C28 C29 113.80(16) . . ? C27 C28 B1 123.78(18) . . ? C29 C28 B1 122.17(17) . . ? C26 C27 C28 123.79(18) . . ? C26 C27 H27 118.1 . . ? C28 C27 H27 118.1 . . ? C30 C29 C28 123.93(17) . . ? C30 C29 H29 118.0 . . ? C28 C29 H29 118.0 . . ? C29 C30 C31 122.04(18) . . ? C29 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C23 C32 C31 118.70(18) . . ? C23 C32 C19 116.96(16) . . ? C31 C32 C19 124.32(17) . . ? C32 C31 C30 125.02(17) . . ? C32 C31 C26 119.57(17) . . ? C30 C31 C26 115.30(16) . . ? C35 C34 C33 121.06(18) . . ? C35 C34 C41 118.65(17) . . ? C33 C34 C41 120.25(18) . . ? C38 C33 C34 115.88(19) . . ? C38 C33 B1 122.69(17) . . ? C34 C33 B1 121.43(17) . . ? C36 C37 C38 122.8(2) . . ? C36 C37 H37 118.6 . . ? C38 C37 H37 118.6 . . ? C37 C36 C35 116.4(2) . . ? C37 C36 C40 121.6(2) . . ? C35 C36 C40 121.9(2) . . ? C36 C35 C34 122.60(19) . . ? C36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C38 C33 121.19(19) . . ? C37 C38 C39 116.51(19) . . ? C33 C38 C39 122.3(2) . . ? C43 C50 H50A 109.5 . . ? C43 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C43 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C45 C49 H49A 109.5 . . ? C45 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C45 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C47 C42 121.30(17) . . ? C46 C47 C48 116.84(17) . . ? C42 C47 C48 121.86(17) . . ? C45 C46 C47 121.89(19) . . ? C45 C46 H46 119.1 . . ? C47 C46 H46 119.1 . . ? C44 C45 C46 117.13(18) . . ? C44 C45 C49 121.03(18) . . ? C46 C45 C49 121.83(19) . . ? C45 C44 C43 122.25(17) . . ? C45 C44 H44 118.9 . . ? C43 C44 H44 118.9 . . ? C44 C43 C42 121.19(18) . . ? C44 C43 C50 117.59(17) . . ? C42 C43 C50 121.21(19) . . ? C47 C42 C43 116.14(18) . . ? C47 C42 B1 123.58(16) . . ? C43 C42 B1 120.24(17) . . ? C34 C41 H41A 109.5 . . ? C34 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C34 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36 C40 H40A 109.5 . . ? C36 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C36 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O4A_1 K1_1 O4A_1 180.0 . 2_775 ? O4A_1 K1_1 O2_1 96.69(7) . 2_775 ? O4A_1 K1_1 O2_1 83.31(7) 2_775 2_775 ? O4B_1 K1_1 O2_1 83.3(2) . . ? O4B_1 K1_1 O2_1 96.7(2) 2_775 . ? O4A_1 K1_1 O2_1 83.31(7) . . ? O4A_1 K1_1 O2_1 96.69(7) 2_775 . ? O2_1 K1_1 O2_1 180.0 2_775 . ? O4A_1 K1_1 O1_1 82.09(8) . 2_775 ? O4A_1 K1_1 O1_1 97.91(8) 2_775 2_775 ? O2_1 K1_1 O1_1 60.71(5) 2_775 2_775 ? O2_1 K1_1 O1_1 119.29(5) . 2_775 ? O4B_1 K1_1 O1_1 83.1(3) . . ? O4B_1 K1_1 O1_1 96.9(3) 2_775 . ? O4A_1 K1_1 O1_1 97.91(8) . . ? O4A_1 K1_1 O1_1 82.09(8) 2_775 . ? O2_1 K1_1 O1_1 119.29(5) 2_775 . ? O2_1 K1_1 O1_1 60.71(5) . . ? O1_1 K1_1 O1_1 180.00(5) 2_775 . ? O4B_1 K1_1 O3_1 102.6(3) . . ? O4B_1 K1_1 O3_1 77.4(3) 2_775 . ? O4A_1 K1_1 O3_1 88.02(9) . . ? O4A_1 K1_1 O3_1 91.98(9) 2_775 . ? O2_1 K1_1 O3_1 119.68(5) 2_775 . ? O2_1 K1_1 O3_1 60.32(5) . . ? O1_1 K1_1 O3_1 60.57(5) 2_775 . ? O1_1 K1_1 O3_1 119.43(5) . . ? O4A_1 K1_1 O3_1 91.98(9) . 2_775 ? O4A_1 K1_1 O3_1 88.02(9) 2_775 2_775 ? O2_1 K1_1 O3_1 60.32(5) 2_775 2_775 ? O2_1 K1_1 O3_1 119.68(5) . 2_775 ? O1_1 K1_1 O3_1 119.43(5) 2_775 2_775 ? O1_1 K1_1 O3_1 60.57(5) . 2_775 ? O3_1 K1_1 O3_1 180.0 . 2_775 ? O4A_1 K1_1 C10B_1 165.5(3) . 2_775 ? O4A_1 K1_1 C10B_1 14.5(3) 2_775 2_775 ? O2_1 K1_1 C10B_1 68.9(3) 2_775 2_775 ? O2_1 K1_1 C10B_1 111.1(3) . 2_775 ? O1_1 K1_1 C10B_1 89.3(4) 2_775 2_775 ? O1_1 K1_1 C10B_1 90.7(4) . 2_775 ? O3_1 K1_1 C10B_1 97.9(2) . 2_775 ? O3_1 K1_1 C10B_1 82.1(2) 2_775 2_775 ? O4B_1 K1_1 C10B_1 21.0(3) . . ? O4B_1 K1_1 C10B_1 159.0(3) 2_775 . ? O2_1 K1_1 C10B_1 111.1(3) 2_775 . ? O2_1 K1_1 C10B_1 68.9(3) . . ? O1_1 K1_1 C10B_1 90.7(4) 2_775 . ? O1_1 K1_1 C10B_1 89.3(4) . . ? O3_1 K1_1 C10B_1 82.1(2) . . ? O3_1 K1_1 C10B_1 97.9(2) 2_775 . ? C10B_1 K1_1 C10B_1 180.0 2_775 . ? O1_1 C1_1 C6_1 108.68(19) . 2_775 ? O1_1 C1_1 H1A_1 110.0 . . ? C6_1 C1_1 H1A_1 110.0 2_775 . ? O1_1 C1_1 H1AB_1 110.0 . . ? C6_1 C1_1 H1AB_1 110.0 2_775 . ? H1A_1 C1_1 H1AB_1 108.3 . . ? C3_1 O2_1 C4_1 112.05(19) . . ? C3_1 O2_1 K1_1 114.02(16) . . ? C4_1 O2_1 K1_1 115.43(14) . . ? O1_1 C2_1 C3_1 108.61(19) . . ? O1_1 C2_1 H2A_1 110.0 . . ? C3_1 C2_1 H2A_1 110.0 . . ? O1_1 C2_1 H2AB_1 110.0 . . ? C3_1 C2_1 H2AB_1 110.0 . . ? H2A_1 C2_1 H2AB_1 108.3 . . ? C6_1 O3_1 C5_1 112.5(2) . . ? C6_1 O3_1 K1_1 113.27(14) . . ? C5_1 O3_1 K1_1 113.41(14) . . ? O2_1 C3_1 C2_1 108.67(19) . . ? O2_1 C3_1 H3A_1 110.0 . . ? C2_1 C3_1 H3A_1 110.0 . . ? O2_1 C3_1 H3AB_1 110.0 . . ? C2_1 C3_1 H3AB_1 110.0 . . ? H3A_1 C3_1 H3AB_1 108.3 . . ? C7A_1 O4A_1 C10A_1 109.0(3) . . ? C7A_1 O4A_1 K1_1 115.6(3) . . ? C10A_1 O4A_1 K1_1 123.1(3) . . ? O4A_1 C7A_1 C8A_1 108.0(3) . . ? O4A_1 C7A_1 H7AA_1 110.1 . . ? C8A_1 C7A_1 H7AA_1 110.1 . . ? O4A_1 C7A_1 H7AB_1 110.1 . . ? C8A_1 C7A_1 H7AB_1 110.1 . . ? H7AA_1 C7A_1 H7AB_1 108.4 . . ? C7A_1 C8A_1 C9A_1 103.0(3) . . ? C7A_1 C8A_1 H8AA_1 111.2 . . ? C9A_1 C8A_1 H8AA_1 111.2 . . ? C7A_1 C8A_1 H8AB_1 111.2 . . ? C9A_1 C8A_1 H8AB_1 111.2 . . ? H8AA_1 C8A_1 H8AB_1 109.1 . . ? C10A_1 C9A_1 C8A_1 100.0(3) . . ? C10A_1 C9A_1 H9AA_1 111.8 . . ? C8A_1 C9A_1 H9AA_1 111.8 . . ? C10A_1 C9A_1 H9AB_1 111.8 . . ? C8A_1 C9A_1 H9AB_1 111.8 . . ? H9AA_1 C9A_1 H9AB_1 109.5 . . ? O4A_1 C10A_1 C9A_1 105.1(3) . . ? O4A_1 C10A_1 H10A_1 110.7 . . ? C9A_1 C10A_1 H10A_1 110.7 . . ? O4A_1 C10A_1 H10B_1 110.7 . . ? C9A_1 C10A_1 H10B_1 110.7 . . ? H10A_1 C10A_1 H10B_1 108.8 . . ? C7B_1 O4B_1 C10B_1 104.5(7) . . ? C7B_1 O4B_1 K1_1 127.2(6) . . ? C10B_1 O4B_1 K1_1 120.3(7) . . ? C7B_1 C8B_1 C9B_1 105.5(5) . . ? C7B_1 C8B_1 H8BA_1 110.6 . . ? C9B_1 C8B_1 H8BA_1 110.6 . . ? C7B_1 C8B_1 H8BB_1 110.6 . . ? C9B_1 C8B_1 H8BB_1 110.6 . . ? H8BA_1 C8B_1 H8BB_1 108.8 . . ? O4B_1 C7B_1 C8B_1 104.3(6) . . ? O4B_1 C7B_1 H7BA_1 110.9 . . ? C8B_1 C7B_1 H7BA_1 110.9 . . ? O4B_1 C7B_1 H7BB_1 110.9 . . ? C8B_1 C7B_1 H7BB_1 110.9 . . ? H7BA_1 C7B_1 H7BB_1 108.9 . . ? C8B_1 C9B_1 C10B_1 105.1(5) . . ? C8B_1 C9B_1 H9BA_1 110.7 . . ? C10B_1 C9B_1 H9BA_1 110.7 . . ? C8B_1 C9B_1 H9BB_1 110.7 . . ? C10B_1 C9B_1 H9BB_1 110.7 . . ? H9BA_1 C9B_1 H9BB_1 108.8 . . ? O4B_1 C10B_1 C9B_1 104.2(6) . . ? O4B_1 C10B_1 K1_1 38.7(5) . . ? C9B_1 C10B_1 K1_1 142.2(8) . . ? O4B_1 C10B_1 H10C_1 110.9 . . ? C9B_1 C10B_1 H10C_1 110.9 . . ? K1_1 C10B_1 H10C_1 94.2 . . ? O4B_1 C10B_1 H10D_1 110.9 . . ? C9B_1 C10B_1 H10D_1 110.9 . . ? K1_1 C10B_1 H10D_1 85.3 . . ? H10C_1 C10B_1 H10D_1 108.9 . . ? O3_1 C5_1 C4_1 109.2(3) . . ? O3_1 C5_1 H5A_1 109.8 . . ? C4_1 C5_1 H5A_1 109.8 . . ? O3_1 C5_1 H5AB_1 109.8 . . ? C4_1 C5_1 H5AB_1 109.8 . . ? H5A_1 C5_1 H5AB_1 108.3 . . ? O3_1 C6_1 C1_1 109.2(3) . 2_775 ? O3_1 C6_1 H6A_1 109.8 . . ? C1_1 C6_1 H6A_1 109.8 2_775 . ? O3_1 C6_1 H6AB_1 109.8 . . ? C1_1 C6_1 H6AB_1 109.8 2_775 . ? H6A_1 C6_1 H6AB_1 108.3 . . ? O2_1 C4_1 C5_1 108.7(2) . . ? O2_1 C4_1 H4A_1 109.9 . . ? C5_1 C4_1 H4A_1 109.9 . . ? O2_1 C4_1 H4AB_1 109.9 . . ? C5_1 C4_1 H4AB_1 109.9 . . ? H4A_1 C4_1 H4AB_1 108.3 . . ? C2_1 O1_1 C1_1 112.48(18) . . ? C2_1 O1_1 K1_1 113.47(15) . . ? C1_1 O1_1 K1_1 113.05(13) . . ? O2_2 K1_2 O2_2 180.0 2_666 . ? O2_2 K1_2 O4_2 100.90(5) 2_666 . ? O2_2 K1_2 O4_2 79.10(5) . . ? O2_2 K1_2 O4_2 79.10(5) 2_666 2_666 ? O2_2 K1_2 O4_2 100.90(5) . 2_666 ? O4_2 K1_2 O4_2 180.00(3) . 2_666 ? O2_2 K1_2 O1_2 61.15(5) 2_666 2_666 ? O2_2 K1_2 O1_2 118.85(5) . 2_666 ? O4_2 K1_2 O1_2 81.00(5) . 2_666 ? O4_2 K1_2 O1_2 99.00(5) 2_666 2_666 ? O2_2 K1_2 O1_2 118.85(5) 2_666 . ? O2_2 K1_2 O1_2 61.15(5) . . ? O4_2 K1_2 O1_2 99.00(5) . . ? O4_2 K1_2 O1_2 81.00(5) 2_666 . ? O1_2 K1_2 O1_2 180.0 2_666 . ? O2_2 K1_2 O3_2 118.93(5) 2_666 . ? O2_2 K1_2 O3_2 61.07(5) . . ? O4_2 K1_2 O3_2 82.63(5) . . ? O4_2 K1_2 O3_2 97.37(5) 2_666 . ? O1_2 K1_2 O3_2 59.38(5) 2_666 . ? O1_2 K1_2 O3_2 120.62(5) . . ? O2_2 K1_2 O3_2 61.06(5) 2_666 2_666 ? O2_2 K1_2 O3_2 118.93(5) . 2_666 ? O4_2 K1_2 O3_2 97.37(5) . 2_666 ? O4_2 K1_2 O3_2 82.63(5) 2_666 2_666 ? O1_2 K1_2 O3_2 120.62(5) 2_666 2_666 ? O1_2 K1_2 O3_2 59.38(5) . 2_666 ? O3_2 K1_2 O3_2 180.00(5) . 2_666 ? O1_2 C1_2 C6_2 108.44(19) . 2_666 ? O1_2 C1_2 H1A_2 110.0 . . ? C6_2 C1_2 H1A_2 110.0 2_666 . ? O1_2 C1_2 H1AB_2 110.0 . . ? C6_2 C1_2 H1AB_2 110.0 2_666 . ? H1A_2 C1_2 H1AB_2 108.4 . . ? C3_2 O2_2 C4_2 112.46(19) . . ? C3_2 O2_2 K1_2 114.27(13) . . ? C4_2 O2_2 K1_2 116.96(13) . . ? O1_2 C2_2 C3_2 108.60(18) . . ? O1_2 C2_2 H2A_2 110.0 . . ? C3_2 C2_2 H2A_2 110.0 . . ? O1_2 C2_2 H2AB_2 110.0 . . ? C3_2 C2_2 H2AB_2 110.0 . . ? H2A_2 C2_2 H2AB_2 108.4 . . ? C5_2 O3_2 C6_2 111.98(17) . . ? C5_2 O3_2 K1_2 108.99(12) . . ? C6_2 O3_2 K1_2 114.93(14) . . ? O2_2 C3_2 C2_2 109.4(2) . . ? O2_2 C3_2 H3A_2 109.8 . . ? C2_2 C3_2 H3A_2 109.8 . . ? O2_2 C3_2 H3AB_2 109.8 . . ? C2_2 C3_2 H3AB_2 109.8 . . ? H3A_2 C3_2 H3AB_2 108.2 . . ? C7_2 O4_2 C10_2 108.1(2) . . ? C7_2 O4_2 K1_2 133.34(16) . . ? C10_2 O4_2 K1_2 117.48(15) . . ? O3_2 C5_2 C4_2 109.26(18) . . ? O3_2 C5_2 H5A_2 109.8 . . ? C4_2 C5_2 H5A_2 109.8 . . ? O3_2 C5_2 H5AB_2 109.8 . . ? C4_2 C5_2 H5AB_2 109.8 . . ? H5A_2 C5_2 H5AB_2 108.3 . . ? O3_2 C6_2 C1_2 108.91(19) . 2_666 ? O3_2 C6_2 H6A_2 109.9 . . ? C1_2 C6_2 H6A_2 109.9 2_666 . ? O3_2 C6_2 H6AB_2 109.9 . . ? C1_2 C6_2 H6AB_2 109.9 2_666 . ? H6A_2 C6_2 H6AB_2 108.3 . . ? O4_2 C7_2 C8_2 106.7(2) . . ? O4_2 C7_2 H7A_2 110.4 . . ? C8_2 C7_2 H7A_2 110.4 . . ? O4_2 C7_2 H7AB_2 110.4 . . ? C8_2 C7_2 H7AB_2 110.4 . . ? H7A_2 C7_2 H7AB_2 108.6 . . ? C7_2 C8_2 C9A_2 92.7(4) . . ? C7_2 C8_2 C9B_2 106.4(3) . . ? C7_2 C8_2 H8A_2 113.2 . . ? C9A_2 C8_2 H8A_2 113.2 . . ? C7_2 C8_2 H8AB_2 113.2 . . ? C9A_2 C8_2 H8AB_2 113.2 . . ? H8A_2 C8_2 H8AB_2 110.5 . . ? O4_2 C10_2 C9B_2 109.7(3) . . ? O4_2 C10_2 C9A_2 101.6(4) . . ? O4_2 C10_2 H10A_2 111.4 . . ? C9A_2 C10_2 H10A_2 111.4 . . ? O4_2 C10_2 H10B_2 111.4 . . ? C9A_2 C10_2 H10B_2 111.4 . . ? H10A_2 C10_2 H10B_2 109.3 . . ? C10_2 C9A_2 C8_2 101.8(6) . . ? C10_2 C9A_2 H9AA_2 111.4 . . ? C8_2 C9A_2 H9AA_2 111.4 . . ? C10_2 C9A_2 H9AB_2 111.4 . . ? C8_2 C9A_2 H9AB_2 111.4 . . ? H9AA_2 C9A_2 H9AB_2 109.3 . . ? C10_2 C9B_2 C8_2 102.2(4) . . ? C10_2 C9B_2 H9BA_2 111.3 . . ? C8_2 C9B_2 H9BA_2 111.3 . . ? C10_2 C9B_2 H9BB_2 111.3 . . ? C8_2 C9B_2 H9BB_2 111.3 . . ? H9BA_2 C9B_2 H9BB_2 109.2 . . ? O2_2 C4_2 C5_2 108.5(2) . . ? O2_2 C4_2 H4A_2 110.0 . . ? C5_2 C4_2 H4A_2 110.0 . . ? O2_2 C4_2 H4AB_2 110.0 . . ? C5_2 C4_2 H4AB_2 110.0 . . ? H4A_2 C4_2 H4AB_2 108.4 . . ? C1_2 O1_2 C2_2 112.15(17) . . ? C1_2 O1_2 K1_2 115.61(15) . . ? C2_2 O1_2 K1_2 113.28(12) . . ? O1A_3 C1A_3 C2A_3 106.1(5) . . ? O1A_3 C1A_3 H1AA_3 110.5 . . ? C2A_3 C1A_3 H1AA_3 110.5 . . ? O1A_3 C1A_3 H1AB_3 110.5 . . ? C2A_3 C1A_3 H1AB_3 110.5 . . ? H1AA_3 C1A_3 H1AB_3 108.7 . . ? C1A_3 C2A_3 C3A_3 99.9(5) . . ? C1A_3 C2A_3 H2AA_3 111.8 . . ? C3A_3 C2A_3 H2AA_3 111.8 . . ? C1A_3 C2A_3 H2AB_3 111.8 . . ? C3A_3 C2A_3 H2AB_3 111.8 . . ? H2AA_3 C2A_3 H2AB_3 109.5 . . ? C1A_3 O1A_3 C4A_3 106.0(4) . . ? C3A_3 C4A_3 O1A_3 107.5(4) . . ? C3A_3 C4A_3 H4A1_3 110.2 . . ? O1A_3 C4A_3 H4A1_3 110.2 . . ? C3A_3 C4A_3 H4A2_3 110.2 . . ? O1A_3 C4A_3 H4A2_3 110.2 . . ? H4A1_3 C4A_3 H4A2_3 108.5 . . ? C4A_3 C3A_3 C2A_3 102.5(5) . . ? C4A_3 C3A_3 H3A1_3 111.3 . . ? C2A_3 C3A_3 H3A1_3 111.3 . . ? C4A_3 C3A_3 H3A2_3 111.3 . . ? C2A_3 C3A_3 H3A2_3 111.3 . . ? H3A1_3 C3A_3 H3A2_3 109.2 . . ? C4B_3 C5B_3 C1B_3 105.8(4) . . ? C4B_3 C5B_3 H5B1_3 110.6 . . ? C1B_3 C5B_3 H5B1_3 110.6 . . ? C4B_3 C5B_3 H5B2_3 110.6 . . ? C1B_3 C5B_3 H5B2_3 110.6 . . ? H5B1_3 C5B_3 H5B2_3 108.7 . . ? O2B_3 C1B_3 C5B_3 108.7(4) . . ? O2B_3 C1B_3 H1BA_3 110.0 . . ? C5B_3 C1B_3 H1BA_3 110.0 . . ? O2B_3 C1B_3 H1BB_3 110.0 . . ? C5B_3 C1B_3 H1BB_3 110.0 . . ? H1BA_3 C1B_3 H1BB_3 108.3 . . ? C3B_3 O2B_3 C1B_3 103.1(4) . . ? C4B_3 C3B_3 O2B_3 110.4(4) . . ? C4B_3 C3B_3 H3BA_3 109.6 . . ? O2B_3 C3B_3 H3BA_3 109.6 . . ? C4B_3 C3B_3 H3BB_3 109.6 . . ? O2B_3 C3B_3 H3BB_3 109.6 . . ? H3BA_3 C3B_3 H3BB_3 108.1 . . ? C5B_3 C4B_3 C3B_3 106.0(4) . . ? C5B_3 C4B_3 H4B1_3 110.5 . . ? C3B_3 C4B_3 H4B1_3 110.5 . . ? C5B_3 C4B_3 H4B2_3 110.5 . . ? C3B_3 C4B_3 H4B2_3 110.5 . . ? H4B1_3 C4B_3 H4B2_3 108.7 . . ? C5C_3 C4C_3 C3C_3 103.1(7) . . ? C5C_3 C4C_3 H4CA_3 111.1 . . ? C3C_3 C4C_3 H4CA_3 111.1 . . ? C5C_3 C4C_3 H4CB_3 111.1 . . ? C3C_3 C4C_3 H4CB_3 111.1 . . ? H4CA_3 C4C_3 H4CB_3 109.1 . . ? C5C_3 O1C_3 C2C_3 107.0(6) . . ? O1C_3 C2C_3 C3C_3 103.7(7) . . ? O1C_3 C2C_3 H2CA_3 111.0 . . ? C3C_3 C2C_3 H2CA_3 111.0 . . ? O1C_3 C2C_3 H2CB_3 111.0 . . ? C3C_3 C2C_3 H2CB_3 111.0 . . ? H2CA_3 C2C_3 H2CB_3 109.0 . . ? C4C_3 C3C_3 C2C_3 99.1(7) . . ? C4C_3 C3C_3 H3CA_3 111.9 . . ? C2C_3 C3C_3 H3CA_3 111.9 . . ? C4C_3 C3C_3 H3CB_3 111.9 . . ? C2C_3 C3C_3 H3CB_3 111.9 . . ? H3CA_3 C3C_3 H3CB_3 109.6 . . ? O1C_3 C5C_3 C4C_3 108.1(5) . . ? O1C_3 C5C_3 H5CA_3 110.1 . . ? C4C_3 C5C_3 H5CA_3 110.1 . . ? O1C_3 C5C_3 H5CB_3 110.1 . . ? C4C_3 C5C_3 H5CB_3 110.1 . . ? H5CA_3 C5C_3 H5CB_3 108.4 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.381(3) . ? C1 N1 1.398(3) . ? C1 C6 1.403(3) . ? N1 C8 1.434(3) . ? N1 C15 1.447(2) . ? B1 C28 1.533(3) . ? B1 C33 1.598(3) . ? B1 C42 1.601(3) . ? C2 C3 1.384(4) . ? C2 H2 0.9500 . ? C23 C22 1.423(3) . ? C23 C24 1.424(3) . ? C23 C32 1.426(3) . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? C4 C5 1.373(4) . ? C4 C7 1.517(4) . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.387(3) . ? C8 C13 1.393(3) . ? C9 C10 1.392(3) . ? C9 H9 0.9500 . ? C19 C18 1.407(3) . ? C19 C20 1.439(2) . ? C19 C32 1.461(3) . ? C10 C11 1.388(4) . ? C10 H10 0.9500 . ? C24 C25 1.356(3) . ? C24 H24 0.9500 . ? C11 C12 1.390(4) . ? C11 C14 1.512(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.374(3) . ? C15 C20 1.413(3) . ? C16 C17 1.399(3) . ? C16 H16 0.9500 . ? C17 C18 1.377(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C20 C21 1.427(3) . ? C22 C21 1.359(3) . ? C22 H22 0.9500 . ? C21 H21 0.9500 . ? C26 C27 1.395(3) . ? C26 C25 1.438(3) . ? C26 C31 1.441(3) . ? C25 H25 0.9500 . ? C28 C27 1.421(3) . ? C28 C29 1.432(3) . ? C27 H27 0.9500 . ? C29 C30 1.368(3) . ? C29 H29 0.9500 . ? C30 C31 1.433(3) . ? C30 H30 0.9500 . ? C32 C31 1.432(2) . ? C34 C35 1.391(3) . ? C34 C33 1.425(3) . ? C34 C41 1.507(3) . ? C33 C38 1.414(3) . ? C37 C36 1.388(3) . ? C37 C38 1.390(3) . ? C37 H37 0.9500 . ? C36 C35 1.389(3) . ? C36 C40 1.511(3) . ? C35 H35 0.9500 . ? C39 C38 1.512(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C50 C43 1.511(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C49 C45 1.513(3) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C48 C47 1.515(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C47 C46 1.397(3) . ? C47 C42 1.411(3) . ? C46 C45 1.392(3) . ? C46 H46 0.9500 . ? C45 C44 1.385(3) . ? C44 C43 1.390(3) . ? C44 H44 0.9500 . ? C43 C42 1.419(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? K1_1 O4B_1 2.544(9) . ? K1_1 O4B_1 2.544(9) 2_775 ? K1_1 O4A_1 2.756(3) . ? K1_1 O4A_1 2.756(3) 2_775 ? K1_1 O2_1 2.7934(17) 2_775 ? K1_1 O2_1 2.7934(17) . ? K1_1 O1_1 2.8143(15) 2_775 ? K1_1 O1_1 2.8143(15) . ? K1_1 O3_1 2.8198(18) . ? K1_1 O3_1 2.8198(18) 2_775 ? K1_1 C10B_1 3.514(14) 2_775 ? K1_1 C10B_1 3.514(14) . ? C1_1 O1_1 1.423(3) . ? C1_1 C6_1 1.484(4) 2_775 ? C1_1 H1A_1 0.9900 . ? C1_1 H1AB_1 0.9900 . ? O2_1 C3_1 1.420(3) . ? O2_1 C4_1 1.424(3) . ? C2_1 O1_1 1.420(3) . ? C2_1 C3_1 1.500(4) . ? C2_1 H2A_1 0.9900 . ? C2_1 H2AB_1 0.9900 . ? O3_1 C6_1 1.415(3) . ? O3_1 C5_1 1.421(4) . ? C3_1 H3A_1 0.9900 . ? C3_1 H3AB_1 0.9900 . ? O4A_1 C7A_1 1.423(4) . ? O4A_1 C10A_1 1.461(4) . ? C7A_1 C8A_1 1.461(5) . ? C7A_1 H7AA_1 0.9900 . ? C7A_1 H7AB_1 0.9900 . ? C8A_1 C9A_1 1.579(5) . ? C8A_1 H8AA_1 0.9900 . ? C8A_1 H8AB_1 0.9900 . ? C9A_1 C10A_1 1.489(5) . ? C9A_1 H9AA_1 0.9900 . ? C9A_1 H9AB_1 0.9900 . ? C10A_1 H10A_1 0.9900 . ? C10A_1 H10B_1 0.9900 . ? O4B_1 C7B_1 1.449(9) . ? O4B_1 C10B_1 1.458(9) . ? C8B_1 C7B_1 1.494(9) . ? C8B_1 C9B_1 1.501(9) . ? C8B_1 H8BA_1 0.9900 . ? C8B_1 H8BB_1 0.9900 . ? C7B_1 H7BA_1 0.9900 . ? C7B_1 H7BB_1 0.9900 . ? C9B_1 C10B_1 1.520(9) . ? C9B_1 H9BA_1 0.9900 . ? C9B_1 H9BB_1 0.9900 . ? C10B_1 H10C_1 0.9900 . ? C10B_1 H10D_1 0.9900 . ? C5_1 C4_1 1.489(4) . ? C5_1 H5A_1 0.9900 . ? C5_1 H5AB_1 0.9900 . ? C6_1 H6A_1 0.9900 . ? C6_1 H6AB_1 0.9900 . ? C4_1 H4A_1 0.9900 . ? C4_1 H4AB_1 0.9900 . ? K1_2 O2_2 2.7383(16) 2_666 ? K1_2 O2_2 2.7383(16) . ? K1_2 O4_2 2.7648(18) . ? K1_2 O4_2 2.7648(18) 2_666 ? K1_2 O1_2 2.8151(16) 2_666 ? K1_2 O1_2 2.8151(16) . ? K1_2 O3_2 2.8609(15) . ? K1_2 O3_2 2.8610(15) 2_666 ? C1_2 O1_2 1.425(3) . ? C1_2 C6_2 1.497(4) 2_666 ? C1_2 H1A_2 0.9900 . ? C1_2 H1AB_2 0.9900 . ? O2_2 C3_2 1.416(3) . ? O2_2 C4_2 1.428(3) . ? C2_2 O1_2 1.426(3) . ? C2_2 C3_2 1.490(4) . ? C2_2 H2A_2 0.9900 . ? C2_2 H2AB_2 0.9900 . ? O3_2 C5_2 1.421(3) . ? O3_2 C6_2 1.421(3) . ? C3_2 H3A_2 0.9900 . ? C3_2 H3AB_2 0.9900 . ? O4_2 C7_2 1.422(3) . ? O4_2 C10_2 1.424(3) . ? C5_2 C4_2 1.493(4) . ? C5_2 H5A_2 0.9900 . ? C5_2 H5AB_2 0.9900 . ? C6_2 H6A_2 0.9900 . ? C6_2 H6AB_2 0.9900 . ? C7_2 C8_2 1.487(4) . ? C7_2 H7A_2 0.9900 . ? C7_2 H7AB_2 0.9900 . ? C8_2 C9A_2 1.537(9) . ? C8_2 C9B_2 1.549(6) . ? C8_2 H8A_2 0.9900 . ? C8_2 H8AB_2 0.9900 . ? C10_2 C9B_2 1.516(7) . ? C10_2 C9A_2 1.535(10) . ? C10_2 H10A_2 0.9900 . ? C10_2 H10B_2 0.9900 . ? C9A_2 H9AA_2 0.9900 . ? C9A_2 H9AB_2 0.9900 . ? C9B_2 H9BA_2 0.9900 . ? C9B_2 H9BB_2 0.9900 . ? C4_2 H4A_2 0.9900 . ? C4_2 H4AB_2 0.9900 . ? C1A_3 O1A_3 1.386(7) . ? C1A_3 C2A_3 1.518(8) . ? C1A_3 H1AA_3 0.9900 . ? C1A_3 H1AB_3 0.9900 . ? C2A_3 C3A_3 1.577(8) . ? C2A_3 H2AA_3 0.9900 . ? C2A_3 H2AB_3 0.9900 . ? O1A_3 C4A_3 1.536(7) . ? C4A_3 C3A_3 1.469(8) . ? C4A_3 H4A1_3 0.9900 . ? C4A_3 H4A2_3 0.9900 . ? C3A_3 H3A1_3 0.9900 . ? C3A_3 H3A2_3 0.9900 . ? C5B_3 C4B_3 1.433(6) . ? C5B_3 C1B_3 1.490(6) . ? C5B_3 H5B1_3 0.9900 . ? C5B_3 H5B2_3 0.9900 . ? C1B_3 O2B_3 1.483(6) . ? C1B_3 H1BA_3 0.9900 . ? C1B_3 H1BB_3 0.9900 . ? O2B_3 C3B_3 1.480(6) . ? C3B_3 C4B_3 1.466(6) . ? C3B_3 H3BA_3 0.9900 . ? C3B_3 H3BB_3 0.9900 . ? C4B_3 H4B1_3 0.9900 . ? C4B_3 H4B2_3 0.9900 . ? C4C_3 C5C_3 1.504(9) . ? C4C_3 C3C_3 1.532(10) . ? C4C_3 H4CA_3 0.9900 . ? C4C_3 H4CB_3 0.9900 . ? O1C_3 C5C_3 1.437(8) . ? O1C_3 C2C_3 1.460(9) . ? C2C_3 C3C_3 1.542(10) . ? C2C_3 H2CA_3 0.9900 . ? C2C_3 H2CB_3 0.9900 . ? C3C_3 H3CA_3 0.9900 . ? C3C_3 H3CB_3 0.9900 . ? C5C_3 H5CA_3 0.9900 . ? C5C_3 H5CB_3 0.9900 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 N1 C8 -154.8(2) . . . . ? C6 C1 N1 C8 26.7(3) . . . . ? C2 C1 N1 C15 0.1(3) . . . . ? C6 C1 N1 C15 -178.4(2) . . . . ? N1 C1 C2 C3 179.9(3) . . . . ? C6 C1 C2 C3 -1.5(4) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C2 C3 C4 C5 2.5(5) . . . . ? C2 C3 C4 C7 -175.4(3) . . . . ? C3 C4 C5 C6 -1.5(4) . . . . ? C7 C4 C5 C6 176.3(3) . . . . ? C4 C5 C6 C1 -1.0(4) . . . . ? C2 C1 C6 C5 2.5(4) . . . . ? N1 C1 C6 C5 -178.9(2) . . . . ? C1 N1 C8 C9 46.0(3) . . . . ? C15 N1 C8 C9 -110.1(2) . . . . ? C1 N1 C8 C13 -137.8(2) . . . . ? C15 N1 C8 C13 66.2(3) . . . . ? C13 C8 C9 C10 0.5(3) . . . . ? N1 C8 C9 C10 176.6(2) . . . . ? C8 C9 C10 C11 -0.2(4) . . . . ? C22 C23 C24 C25 -174.8(2) . . . . ? C32 C23 C24 C25 3.7(3) . . . . ? C9 C10 C11 C12 -0.2(4) . . . . ? C9 C10 C11 C14 178.4(2) . . . . ? C10 C11 C12 C13 0.4(3) . . . . ? C14 C11 C12 C13 -178.3(2) . . . . ? C11 C12 C13 C8 -0.1(3) . . . . ? C9 C8 C13 C12 -0.3(3) . . . . ? N1 C8 C13 C12 -176.64(19) . . . . ? C1 N1 C15 C16 -90.8(2) . . . . ? C8 N1 C15 C16 65.9(2) . . . . ? C1 N1 C15 C20 93.2(2) . . . . ? C8 N1 C15 C20 -110.1(2) . . . . ? C20 C15 C16 C17 2.4(3) . . . . ? N1 C15 C16 C17 -173.54(17) . . . . ? C15 C16 C17 C18 -3.5(3) . . . . ? C16 C17 C18 C19 -0.2(3) . . . . ? C20 C19 C18 C17 5.0(3) . . . . ? C32 C19 C18 C17 177.54(17) . . . . ? C16 C15 C20 C21 -171.74(18) . . . . ? N1 C15 C20 C21 4.1(3) . . . . ? C16 C15 C20 C19 2.5(3) . . . . ? N1 C15 C20 C19 178.35(16) . . . . ? C18 C19 C20 C15 -6.0(2) . . . . ? C32 C19 C20 C15 -178.80(16) . . . . ? C18 C19 C20 C21 168.36(17) . . . . ? C32 C19 C20 C21 -4.5(3) . . . . ? C24 C23 C22 C21 -176.78(19) . . . . ? C32 C23 C22 C21 4.7(3) . . . . ? C23 C22 C21 C20 7.2(3) . . . . ? C15 C20 C21 C22 167.00(18) . . . . ? C19 C20 C21 C22 -7.2(3) . . . . ? C23 C24 C25 C26 5.6(3) . . . . ? C27 C26 C25 C24 172.6(2) . . . . ? C31 C26 C25 C24 -5.3(3) . . . . ? C33 B1 C28 C27 -1.6(3) . . . . ? C42 B1 C28 C27 -179.25(17) . . . . ? C33 B1 C28 C29 172.22(17) . . . . ? C42 B1 C28 C29 -5.4(3) . . . . ? C25 C26 C27 C28 -173.43(19) . . . . ? C31 C26 C27 C28 4.3(3) . . . . ? C29 C28 C27 C26 -0.1(3) . . . . ? B1 C28 C27 C26 174.16(18) . . . . ? C27 C28 C29 C30 -2.5(3) . . . . ? B1 C28 C29 C30 -176.92(18) . . . . ? C28 C29 C30 C31 0.9(3) . . . . ? C22 C23 C32 C31 165.57(17) . . . . ? C24 C23 C32 C31 -12.9(3) . . . . ? C22 C23 C32 C19 -15.9(3) . . . . ? C24 C23 C32 C19 165.59(18) . . . . ? C18 C19 C32 C23 -156.75(17) . . . . ? C20 C19 C32 C23 15.7(2) . . . . ? C18 C19 C32 C31 21.7(3) . . . . ? C20 C19 C32 C31 -165.89(17) . . . . ? C23 C32 C31 C30 -162.85(18) . . . . ? C19 C32 C31 C30 18.7(3) . . . . ? C23 C32 C31 C26 13.1(3) . . . . ? C19 C32 C31 C26 -165.32(17) . . . . ? C29 C30 C31 C32 179.28(18) . . . . ? C29 C30 C31 C26 3.2(3) . . . . ? C27 C26 C31 C32 178.00(17) . . . . ? C25 C26 C31 C32 -4.2(3) . . . . ? C27 C26 C31 C30 -5.7(3) . . . . ? C25 C26 C31 C30 172.15(18) . . . . ? C35 C34 C33 C38 0.3(3) . . . . ? C41 C34 C33 C38 177.92(18) . . . . ? C35 C34 C33 B1 -178.88(18) . . . . ? C41 C34 C33 B1 -1.2(3) . . . . ? C28 B1 C33 C38 -59.2(3) . . . . ? C42 B1 C33 C38 118.4(2) . . . . ? C28 B1 C33 C34 119.8(2) . . . . ? C42 B1 C33 C34 -62.5(3) . . . . ? C38 C37 C36 C35 -1.1(4) . . . . ? C38 C37 C36 C40 177.0(2) . . . . ? C37 C36 C35 C34 0.9(3) . . . . ? C40 C36 C35 C34 -177.3(2) . . . . ? C33 C34 C35 C36 -0.5(3) . . . . ? C41 C34 C35 C36 -178.1(2) . . . . ? C36 C37 C38 C33 1.0(4) . . . . ? C36 C37 C38 C39 -176.4(2) . . . . ? C34 C33 C38 C37 -0.5(3) . . . . ? B1 C33 C38 C37 178.6(2) . . . . ? C34 C33 C38 C39 176.8(2) . . . . ? B1 C33 C38 C39 -4.1(3) . . . . ? C42 C47 C46 C45 -2.5(3) . . . . ? C48 C47 C46 C45 177.81(17) . . . . ? C47 C46 C45 C44 2.6(3) . . . . ? C47 C46 C45 C49 -176.10(18) . . . . ? C46 C45 C44 C43 -0.1(3) . . . . ? C49 C45 C44 C43 178.63(18) . . . . ? C45 C44 C43 C42 -2.6(3) . . . . ? C45 C44 C43 C50 178.15(18) . . . . ? C46 C47 C42 C43 -0.2(3) . . . . ? C48 C47 C42 C43 179.48(16) . . . . ? C46 C47 C42 B1 177.79(17) . . . . ? C48 C47 C42 B1 -2.5(3) . . . . ? C44 C43 C42 C47 2.7(3) . . . . ? C50 C43 C42 C47 -178.11(17) . . . . ? C44 C43 C42 B1 -175.39(17) . . . . ? C50 C43 C42 B1 3.8(3) . . . . ? C28 B1 C42 C47 -63.1(2) . . . . ? C33 B1 C42 C47 119.2(2) . . . . ? C28 B1 C42 C43 114.8(2) . . . . ? C33 B1 C42 C43 -62.9(2) . . . . ? C4_1 O2_1 C3_1 C2_1 176.3(2) . . . . ? K1_1 O2_1 C3_1 C2_1 -50.3(2) . . . . ? O1_1 C2_1 C3_1 O2_1 67.4(3) . . . . ? C10A_1 O4A_1 C7A_1 C8A_1 1.5(5) . . . . ? K1_1 O4A_1 C7A_1 C8A_1 145.2(3) . . . . ? O4A_1 C7A_1 C8A_1 C9A_1 -23.9(5) . . . . ? C7A_1 C8A_1 C9A_1 C10A_1 36.5(5) . . . . ? C7A_1 O4A_1 C10A_1 C9A_1 23.2(5) . . . . ? K1_1 O4A_1 C10A_1 C9A_1 -117.2(4) . . . . ? C8A_1 C9A_1 C10A_1 O4A_1 -35.8(5) . . . . ? C10B_1 O4B_1 C7B_1 C8B_1 -40.6(15) . . . . ? K1_1 O4B_1 C7B_1 C8B_1 171.0(11) . . . . ? C9B_1 C8B_1 C7B_1 O4B_1 27.1(18) . . . . ? C7B_1 C8B_1 C9B_1 C10B_1 -4(2) . . . . ? C7B_1 O4B_1 C10B_1 C9B_1 37.7(16) . . . . ? K1_1 O4B_1 C10B_1 C9B_1 -171.3(11) . . . . ? C7B_1 O4B_1 C10B_1 K1_1 -151.0(15) . . . . ? C8B_1 C9B_1 C10B_1 O4B_1 -20.2(19) . . . . ? C8B_1 C9B_1 C10B_1 K1_1 -29(3) . . . . ? C6_1 O3_1 C5_1 C4_1 -179.1(2) . . . . ? K1_1 O3_1 C5_1 C4_1 50.7(2) . . . . ? C5_1 O3_1 C6_1 C1_1 -179.9(2) . . . 2_775 ? K1_1 O3_1 C6_1 C1_1 -49.7(2) . . . 2_775 ? C3_1 O2_1 C4_1 C5_1 -179.9(3) . . . . ? K1_1 O2_1 C4_1 C5_1 47.3(3) . . . . ? O3_1 C5_1 C4_1 O2_1 -65.7(3) . . . . ? C3_1 C2_1 O1_1 C1_1 -179.5(2) . . . . ? C3_1 C2_1 O1_1 K1_1 -49.6(2) . . . . ? C6_1 C1_1 O1_1 C2_1 -178.8(2) 2_775 . . . ? C6_1 C1_1 O1_1 K1_1 51.1(3) 2_775 . . . ? C4_2 O2_2 C3_2 C2_2 -171.23(18) . . . . ? K1_2 O2_2 C3_2 C2_2 52.3(2) . . . . ? O1_2 C2_2 C3_2 O2_2 -66.2(2) . . . . ? C6_2 O3_2 C5_2 C4_2 176.14(19) . . . . ? K1_2 O3_2 C5_2 C4_2 -55.6(2) . . . . ? C5_2 O3_2 C6_2 C1_2 172.2(2) . . . 2_666 ? K1_2 O3_2 C6_2 C1_2 47.1(2) . . . 2_666 ? C10_2 O4_2 C7_2 C8_2 27.2(3) . . . . ? K1_2 O4_2 C7_2 C8_2 -165.42(16) . . . . ? O4_2 C7_2 C8_2 C9A_2 -47.6(5) . . . . ? O4_2 C7_2 C8_2 C9B_2 -23.1(4) . . . . ? C7_2 O4_2 C10_2 C9B_2 -20.7(4) . . . . ? K1_2 O4_2 C10_2 C9B_2 169.6(4) . . . . ? C7_2 O4_2 C10_2 C9A_2 7.2(5) . . . . ? K1_2 O4_2 C10_2 C9A_2 -162.4(5) . . . . ? O4_2 C10_2 C9A_2 C8_2 -37.6(7) . . . . ? C7_2 C8_2 C9A_2 C10_2 50.4(7) . . . . ? O4_2 C10_2 C9B_2 C8_2 5.7(6) . . . . ? C7_2 C8_2 C9B_2 C10_2 10.4(5) . . . . ? C3_2 O2_2 C4_2 C5_2 -178.84(18) . . . . ? K1_2 O2_2 C4_2 C5_2 -43.7(2) . . . . ? O3_2 C5_2 C4_2 O2_2 67.9(2) . . . . ? C6_2 C1_2 O1_2 C2_2 177.0(2) 2_666 . . . ? C6_2 C1_2 O1_2 K1_2 -51.0(2) 2_666 . . . ? C3_2 C2_2 O1_2 C1_2 179.1(2) . . . . ? C3_2 C2_2 O1_2 K1_2 46.0(2) . . . . ? O1A_3 C1A_3 C2A_3 C3A_3 -43.0(9) . . . . ? C2A_3 C1A_3 O1A_3 C4A_3 32.7(9) . . . . ? C1A_3 O1A_3 C4A_3 C3A_3 -8.5(10) . . . . ? O1A_3 C4A_3 C3A_3 C2A_3 -17.9(10) . . . . ? C1A_3 C2A_3 C3A_3 C4A_3 35.6(10) . . . . ? C4B_3 C5B_3 C1B_3 O2B_3 -23.1(8) . . . . ? C5B_3 C1B_3 O2B_3 C3B_3 11.8(8) . . . . ? C1B_3 O2B_3 C3B_3 C4B_3 3.5(9) . . . . ? C1B_3 C5B_3 C4B_3 C3B_3 24.4(9) . . . . ? O2B_3 C3B_3 C4B_3 C5B_3 -17.9(9) . . . . ? C5C_3 O1C_3 C2C_3 C3C_3 31.1(19) . . . . ? C5C_3 C4C_3 C3C_3 C2C_3 37.9(18) . . . . ? O1C_3 C2C_3 C3C_3 C4C_3 -42.5(17) . . . . ? C2C_3 O1C_3 C5C_3 C4C_3 -6(2) . . . . ? C3C_3 C4C_3 C5C_3 O1C_3 -21(2) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.7992 40279 1868 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.2008 40103 1868 nmt 0.9631 -0.0540 -0.1402 0.1223 1.0243 0.2618 0.1283 -0.2604 0.9222 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.5005 -1.0043 1.4984 -0.0171 0.1071 0.1216 -3.5073 -6.9563 -3.4711 0.8522 -0.4069 0.3289 -1.8704 -3.3102 -9.0366 0.8586 -0.4100 -0.3077 -1.0039 -2.0044 0.0006 0.1845 -0.0903 0.1588 0.4937 -2.0015 -1.4981 0.2480 0.0391 -0.0189 -0.0055 -2.0025 -0.9985 0.2268 -0.0040 0.0403 -0.0036 -1.0005 -0.9987 0.1438 -0.0152 -0.0120 -0.5008 0.0006 -0.4993 0.0395 -0.0695 -0.0050 0.9981 -1.0017 -0.0000 0.0647 0.1239 -0.0019 0.4992 0.0010 -0.4996 0.0212 0.0431 -0.0592 0.4973 -1.0011 -0.4994 0.1042 0.0543 -0.0070 0.4956 -0.9995 -1.4983 0.1649 0.0279 -0.0712 0.4995 1.0046 -1.4986 -0.0012 0.0055 -0.1758 -0.0019 -1.0020 0.0002 0.0831 0.0112 0.0523 -0.4995 -1.0046 1.4986 0.0012 -0.0055 0.1758 -2.5749 -4.8470 -7.4009 0.8994 -0.4290 -0.0843 -0.4937 2.0015 1.4981 -0.2480 -0.0391 0.0189 1.4989 -1.0024 0.4993 0.0252 0.1934 0.0031 0.0036 1.0005 0.9987 -0.1438 0.0152 0.0120 -0.5005 1.0043 -1.4984 0.0171 -0.1071 -0.1216 -1.0000 -0.0003 0.0002 0.0184 -0.1127 0.0542