#------------------------------------------------------------------------------ #$Date: 2019-12-25 03:46:28 +0200 (Wed, 25 Dec 2019) $ #$Revision: 245568 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125694.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_7125694 loop_ _publ_author_name 'Ye, Zecong' 'Wang, Jian' 'Kothapalli, Sudarshana Santhosh Kumar' 'Yang, Zhiyao' 'Chen, Lixi' 'Xu, Weitao' 'Cai, Yimin' 'Zhang, Tinghui' 'Xiao, Xin' 'Deng, Pengchi' 'Feng, Wen' 'Yuan, Lihua' _publ_section_title ; Controlling the selective synthesis of [2]- and [3]rotaxanes by intermolecular steric hindrance between the macrocyclic hosts ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC08253K _journal_year 2020 _chemical_formula_moiety '2(F6 P), C80 H108 N8 O12, C40 H54 N2, 2(C4 H8 O2), 2(C4.5 O2)' _chemical_formula_sum 'C137 H197 F12 N10 O20 P2' _chemical_formula_weight 2593.97 _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 _audit_creation_date 2019-05-10 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-07-12 deposited with the CCDC. 2019-12-12 downloaded from the CCDC. ; _cell_angle_alpha 100.477(3) _cell_angle_beta 97.247(3) _cell_angle_gamma 114.357(4) _cell_formula_units_Z 1 _cell_length_a 14.0229(5) _cell_length_b 16.6854(7) _cell_length_c 17.4200(5) _cell_measurement_reflns_used 8361 _cell_measurement_temperature 200.00(10) _cell_measurement_theta_max 73.2990 _cell_measurement_theta_min 4.3620 _cell_volume 3558.0(3) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 200.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.6525 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _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 -109.00 -16.00 1.00 2.00 -- -40.08 -38.00 -60.00 93 2 \w -110.00 -25.00 1.00 2.00 -- -40.08 -38.00 30.00 85 3 \w -68.00 33.00 1.00 2.00 -- -40.08 57.00-180.00 101 4 \w 1.00 81.00 1.00 2.00 -- 40.08 -99.00 -90.00 80 5 \w 42.00 118.00 1.00 2.00 -- 105.48-125.00 30.00 76 6 \w 103.00 177.00 1.00 2.00 -- 105.48 125.00-180.00 74 7 \w 75.00 118.00 1.00 2.00 -- 105.48-125.00-150.00 43 8 \w 32.00 61.00 1.00 2.00 -- 105.48 -45.00 -90.00 29 9 \w 88.00 130.00 1.00 2.00 -- 105.48 -45.00 -90.00 42 10 \w 33.00 134.00 1.00 2.00 -- 105.48 -61.00 60.00 101 11 \w 78.00 178.00 1.00 2.00 -- 105.48 30.00 150.00 100 12 \w 42.00 153.00 1.00 2.00 -- 105.48 -15.00 120.00 111 13 \w 40.00 135.00 1.00 2.00 -- 105.48 -61.00-180.00 95 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0166680000 _diffrn_orient_matrix_UB_12 0.0932282000 _diffrn_orient_matrix_UB_13 -0.0133239000 _diffrn_orient_matrix_UB_21 -0.1093681000 _diffrn_orient_matrix_UB_22 -0.0459936000 _diffrn_orient_matrix_UB_23 -0.0602720000 _diffrn_orient_matrix_UB_31 -0.0554604000 _diffrn_orient_matrix_UB_32 0.0142240000 _diffrn_orient_matrix_UB_33 0.0686121000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_unetI/netI 0.0308 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 20980 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 66.600 _diffrn_reflns_theta_max 66.600 _diffrn_reflns_theta_min 3.456 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.955 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.79351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 1.211 _exptl_crystal_description block _exptl_crystal_F_000 1387 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.014 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.061 _refine_ls_extinction_coef 0.00077(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 919 _refine_ls_number_reflns 12457 _refine_ls_number_restraints 384 _refine_ls_restrained_S_all 1.101 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0745 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1300P)^2^+2.2684P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2131 _refine_ls_wR_factor_ref 0.2308 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9806 _reflns_number_total 12457 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc08253k2.cif _cod_data_source_block s _cod_original_cell_volume 3558.0(2) _cod_database_code 7125694 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C11 H10 N O' _chemical_oxdiff_usercomment C4A-C2-CaCL2 _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 0.902 _shelx_estimated_absorpt_t_min 0.847 _reflns_odcompleteness_completeness 99.16 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.49 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C38-C39A 1.5 with sigma of 0.02 C38-C39 1.5 with sigma of 0.02 C65-C66 1.5 with sigma of 0.02 C66-O8 1.22 with sigma of 0.02 C66-O9 1.23 with sigma of 0.02 O9-C67 1.35 with sigma of 0.02 C67-C68 1.5 with sigma of 0.02 C66A-O8A 1.25 with sigma of 0.02 C66A-O9 1.25 with sigma of 0.02 C65A-C66A 1.5 with sigma of 0.02 C67A-O9 1.35 with sigma of 0.02 C67A-C68A 1.5 with sigma of 0.02 O8-C65 2.35 with sigma of 0.02 O9-C65 2.35 with sigma of 0.02 O8A-C65A 2.38 with sigma of 0.02 O9-C68A 2.45 with sigma of 0.02 3. Rigid bond restraints O9, C65, C66, O8, C67, C66A, C67A, C68, C65A, O8A, C68A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints F3 \\sim F2A \\sim F2 \\sim F5A \\sim F1 \\sim F4A \\sim F4 \\sim F3A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 O9 \\sim C65 \\sim C66 \\sim O8 \\sim C67 \\sim C66A \\sim C67A \\sim C68 \\sim C65A \\sim O8A \\sim C68A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(F3A) \\sim Ueq, Uanis(P1) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F2A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C64) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C61) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(F1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(C68) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(O9) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(C67A) \\sim Ueq, Uanis(C68A) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C66A) \\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C65A) \\sim Ueq, Uanis(O8A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 5. Others Fixed Sof: F4(0.5) H38A(0.5) H38(0.5) F3(0.5) F2(0.5) F1(0.5) C39A(0.5) H39A(0.5) H39B(0.5) H39C(0.5) C39(0.5) H39D(0.5) H39E(0.5) H39F(0.5) F3A(0.5) F5A(0.5) F4A(0.5) F2A(0.5) C66(0.5) C67(0.5) C68(0.5) O8(0.5) C65A(0.5) C66A(0.5) C67A(0.5) C68A(0.5) O8A(0.5) 6.a Ternary CH refined with riding coordinates: C16(H16), C2(H2A), C38(H38A), C38(H38), C33(H33) 6.b Secondary CH2 refined with riding coordinates: C46(H46A,H46B), C13(H13A,H13B), C36(H36A,H36B), C31(H31A,H31B), C5(H5A,H5B), C14(H14A,H14B), C4(H4A,H4B), C37(H37A,H37B), C32(H32A,H32B), C63(H63A,H63B) 6.c Aromatic/amide H refined with riding coordinates: N2(H2), N1(H1), C41(H41), C24(H24), C48(H48), C9(H9), C12(H12), C52(H52), C26(H26), C50(H50), C29(H29), C30(H30), C21(H21), C22(H22), C45(H45), C43(H43), C44(H44) 6.d Idealised Me refined as rotating group: C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C54(H54A,H54B,H54C), C59(H59A,H59B, H59C), C58(H58A,H58B,H58C), C15(H15A,H15B,H15C), C60(H60A,H60B,H60C), C17(H17A, H17B,H17C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C64(H64A,H64B,H64C), C40(H40A, H40B,H40C), C61(H61A,H61B,H61C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C39A(H39A,H39B,H39C), C39(H39D,H39E,H39F) ; _shelx_res_file ; s.res created by SHELXL-2014/7 TITL s_a.res in P-1 REM Old TITL exp_3209S in P-1 REM SHELXT solution in P-1 REM R1 0.262, Rweak 0.017, Alpha 0.061, Orientation as input REM Formula found by SHELXT: C69 N6 O6 P F2 CELL 1.54184 14.0229 16.6854 17.42 100.477 97.247 114.357 ZERR 1 0.0005 0.0007 0.0005 0.003 0.003 0.004 LATT 1 SFAC C H N O P F UNIT 137 197 10 20 2 12 DFIX 1.5 C38 C39A DFIX 1.5 C38 C39 DFIX 1.5 C65 C66 DFIX 1.22 C66 O8 DFIX 1.23 C66 O9 DFIX 1.35 O9 C67 DFIX 1.5 C67 C68 DFIX 1.25 C66A O8A DFIX 1.25 C66A O9 DFIX 1.5 C65A C66A DFIX 1.35 C67A O9 DFIX 1.5 C67A C68A DFIX 2.35 O8 C65 DFIX 2.35 O9 C65 DFIX 2.38 O8A C65A DFIX 2.45 O9 C68A DELU O9 C65 C66 O8 C67 C66A C67A C68 C65A O8A C68A SIMU F3 F2A F2 F5A F1 F4A F4 F3A SIMU O9 C65 C66 O8 C67 C66A C67A C68 C65A O8A C68A ISOR 0.01 0.02 F3A P1 F5 F6 F4 F3 F2 F1 F5A F4A F2A ISOR 0.01 0.02 C64 O6 C62 C63 O7 C61 ISOR 0.001 0.002 F1 ISOR 0.001 0.002 C65 C66 C67 O8 C68 ISOR 0.001 0.002 O9 C65 C66 O8 C67A C68A C67 C66A C68 C65A O8A L.S. 10 0 0 PLAN 20 SIZE 0.18 0.15 0.11 list 4 fmap 2 53 acta REM REM REM WGHT 0.130000 2.268400 EXTI 0.000770 FVAR 0.38405 P1 5 0.140467 0.282388 0.767783 11.00000 0.08255 0.08200 = 0.04460 0.02434 0.02986 0.04540 O3 4 -0.166845 0.305705 0.436422 11.00000 0.03028 0.04186 = 0.03690 0.00380 0.00951 0.01258 O003 4 0.218547 0.486071 0.487517 11.00000 0.03484 0.04158 = 0.03172 0.00375 0.01040 0.00842 O5 4 0.896117 0.736633 0.932027 11.00000 0.03846 0.06664 = 0.02499 0.00697 0.00420 0.02101 O1 4 0.249238 0.337362 0.310615 11.00000 0.03353 0.05590 = 0.02348 0.00472 0.00551 0.01340 O2 4 -0.118719 0.181757 0.176390 11.00000 0.03427 0.04404 = 0.03117 -0.00418 0.00316 0.00509 O4 4 -0.010370 0.459351 0.622073 11.00000 0.03323 0.06173 = 0.03601 0.00500 0.01054 0.01835 N2 3 0.041624 0.408012 0.485971 11.00000 0.03095 0.03946 = 0.02959 0.00391 0.00875 0.01346 AFIX 43 H2 2 -0.005603 0.403175 0.514209 11.00000 -1.20000 AFIX 0 N5 3 0.318946 0.358218 0.552075 11.00000 0.03469 0.02570 = 0.03568 0.00681 0.01196 0.00934 N1 3 0.091903 0.288386 0.222284 11.00000 0.03328 0.04242 = 0.02211 0.00312 0.00435 0.01108 AFIX 43 H1 2 0.060864 0.269011 0.172242 11.00000 -1.20000 AFIX 0 N4 3 0.459518 0.635898 0.833517 11.00000 0.03721 0.04341 = 0.03026 0.00383 0.00761 0.01244 N3 3 0.425364 0.614253 0.758865 11.00000 0.03640 0.04321 = 0.02931 0.00185 0.00681 0.01195 F5 6 0.207003 0.238959 0.723139 11.00000 0.13501 0.09334 = 0.07157 0.02004 0.05199 0.06506 C47 1 0.201963 0.192886 0.488480 11.00000 0.02730 0.02847 = 0.03794 0.00640 0.00925 0.00636 C10 1 -0.108179 0.298183 0.380690 11.00000 0.03290 0.03464 = 0.03367 0.00962 0.00919 0.01465 C11 1 0.003284 0.353758 0.406856 11.00000 0.03364 0.03148 = 0.02912 0.00641 0.00643 0.01277 C7 1 0.026576 0.292021 0.277678 11.00000 0.03359 0.03571 = 0.02709 0.00655 0.00728 0.01305 C18 1 0.144561 0.467126 0.522901 11.00000 0.03256 0.03004 = 0.03182 0.00537 0.00726 0.01299 C41 1 0.368674 0.405187 0.501921 11.00000 0.03461 0.02884 = 0.02866 0.00503 0.00870 0.01143 AFIX 43 H41 2 0.332325 0.391562 0.449216 11.00000 -1.20000 AFIX 0 C6 1 0.197413 0.312367 0.240837 11.00000 0.03417 0.03380 = 0.02583 0.00578 0.00747 0.00908 C42 1 0.473348 0.473586 0.527829 11.00000 0.03603 0.02580 = 0.03009 0.00513 0.00952 0.00857 C19 1 0.169375 0.505899 0.611703 11.00000 0.03493 0.03091 = 0.03043 0.00548 0.00909 0.01413 C8 1 -0.083461 0.236594 0.252839 11.00000 0.03532 0.03384 = 0.02929 0.00359 0.00447 0.01148 C24 1 0.277259 0.548028 0.649071 11.00000 0.03497 0.03300 = 0.03185 0.00403 0.01130 0.01223 AFIX 43 H24 2 0.327449 0.554306 0.617573 11.00000 -1.20000 AFIX 0 C25 1 0.572010 0.664292 0.856858 11.00000 0.03591 0.03704 = 0.03004 0.00460 0.00797 0.01152 C23 1 0.313581 0.581189 0.731300 11.00000 0.03483 0.03673 = 0.03283 0.00345 0.00808 0.01224 C48 1 0.192152 0.133305 0.536883 11.00000 0.03073 0.03546 = 0.03410 0.00961 0.00892 0.00919 AFIX 43 H48 2 0.189732 0.150780 0.590150 11.00000 -1.20000 AFIX 0 C27 1 0.745310 0.691427 0.826336 11.00000 0.03693 0.03210 = 0.02550 0.00360 0.00696 0.01006 C49 1 0.185946 0.047887 0.506182 11.00000 0.03029 0.03494 = 0.04568 0.01240 0.00937 0.01099 C9 1 -0.150891 0.240623 0.304455 11.00000 0.02940 0.03584 = 0.03643 0.00488 0.00457 0.00952 AFIX 43 H9 2 -0.224667 0.204471 0.287427 11.00000 -1.20000 AFIX 0 C12 1 0.068918 0.350699 0.354086 11.00000 0.03013 0.03491 = 0.03120 0.00576 0.00603 0.01058 AFIX 43 H12 2 0.142388 0.388544 0.370169 11.00000 -1.20000 AFIX 0 C28 1 0.790022 0.713555 0.909318 11.00000 0.03660 0.03939 = 0.02730 0.00497 0.00538 0.01336 C52 1 0.205773 0.167880 0.409212 11.00000 0.03421 0.03399 = 0.04069 0.01207 0.01250 0.00879 AFIX 43 H52 2 0.211919 0.208115 0.377397 11.00000 -1.20000 AFIX 0 C26 1 0.637637 0.667823 0.802491 11.00000 0.03682 0.03529 = 0.02454 0.00359 0.00611 0.00994 AFIX 43 H26 2 0.607679 0.653741 0.748158 11.00000 -1.20000 AFIX 0 C20 1 0.094896 0.500151 0.660308 11.00000 0.03587 0.03860 = 0.03479 0.00755 0.00992 0.01641 C46 1 0.205622 0.284700 0.521564 11.00000 0.03074 0.03236 = 0.04662 0.01025 0.01420 0.00879 AFIX 23 H46A 2 0.168885 0.300022 0.479836 11.00000 -1.20000 H46B 2 0.168061 0.281309 0.564869 11.00000 -1.20000 AFIX 0 C51 1 0.200499 0.082856 0.376307 11.00000 0.03584 0.03737 = 0.03884 0.00629 0.01329 0.00986 C50 1 0.190582 0.024936 0.426127 11.00000 0.03948 0.03228 = 0.04654 0.00691 0.01393 0.01334 AFIX 43 H50 2 0.186855 -0.031913 0.405051 11.00000 -1.20000 AFIX 0 C29 1 0.725028 0.711024 0.963817 11.00000 0.04636 0.05194 = 0.02152 0.00356 0.00619 0.02019 AFIX 43 H29 2 0.754410 0.725765 1.018334 11.00000 -1.20000 AFIX 0 C30 1 0.617040 0.686787 0.937751 11.00000 0.04275 0.05055 = 0.02827 0.00379 0.01135 0.01746 AFIX 43 H30 2 0.574557 0.685628 0.974842 11.00000 -1.20000 AFIX 0 C21 1 0.131638 0.536198 0.743040 11.00000 0.04032 0.05301 = 0.03529 0.00341 0.01494 0.01851 AFIX 43 H21 2 0.082361 0.533543 0.774766 11.00000 -1.20000 AFIX 0 C22 1 0.238806 0.575419 0.778490 11.00000 0.04207 0.05081 = 0.02996 0.00231 0.00988 0.01778 AFIX 43 H22 2 0.261675 0.598136 0.833836 11.00000 -1.20000 AFIX 0 C45 1 0.367975 0.375020 0.628475 11.00000 0.04971 0.03574 = 0.03615 0.01102 0.01583 0.01194 AFIX 43 H45 2 0.331926 0.341576 0.661868 11.00000 -1.20000 AFIX 0 C13 1 -0.281689 0.251006 0.412191 11.00000 0.02818 0.04015 = 0.04491 0.00541 0.00657 0.01182 AFIX 23 H13A 2 -0.298761 0.187120 0.394205 11.00000 -1.20000 H13B 2 -0.311414 0.268528 0.368462 11.00000 -1.20000 AFIX 0 C57 1 0.175986 -0.017628 0.559801 11.00000 0.04980 0.04174 = 0.05201 0.02008 0.01151 0.02003 C36 1 0.941126 0.748517 1.015110 11.00000 0.05100 0.06728 = 0.02486 0.00433 0.00300 0.02815 AFIX 23 H36A 2 0.898687 0.695867 1.033143 11.00000 -1.20000 H36B 2 0.941552 0.802025 1.048470 11.00000 -1.20000 AFIX 0 C43 1 0.524637 0.490802 0.606966 11.00000 0.04021 0.03639 = 0.03476 0.00481 0.00413 0.00251 AFIX 43 H43 2 0.595157 0.535634 0.626233 11.00000 -1.20000 AFIX 0 C31 1 -0.093867 0.447028 0.666147 11.00000 0.03610 0.05441 = 0.04345 0.01335 0.01359 0.02237 AFIX 23 H31A 2 -0.156879 0.442743 0.631917 11.00000 -1.20000 H31B 2 -0.069277 0.499404 0.711621 11.00000 -1.20000 AFIX 0 C44 1 0.471573 0.441789 0.657126 11.00000 0.05128 0.04413 = 0.03394 0.00961 0.00625 0.00815 AFIX 43 H44 2 0.505977 0.454025 0.710134 11.00000 -1.20000 AFIX 0 C5 1 -0.224497 0.108814 0.155436 11.00000 0.03036 0.05938 = 0.04971 -0.00876 0.00355 0.00305 AFIX 23 H5A 2 -0.277074 0.132549 0.153648 11.00000 -1.20000 H5B 2 -0.234317 0.073660 0.194948 11.00000 -1.20000 AFIX 0 C14 1 -0.328271 0.266542 0.483587 11.00000 0.03537 0.04596 = 0.05021 0.00591 0.01431 0.01549 AFIX 23 H14A 2 -0.308207 0.331008 0.501916 11.00000 -1.20000 H14B 2 -0.297533 0.248835 0.526689 11.00000 -1.20000 AFIX 0 C53 1 0.200582 0.056144 0.287549 11.00000 0.05720 0.04784 = 0.04097 0.00426 0.01696 0.01480 C16 1 -0.450639 0.213209 0.465277 11.00000 0.03475 0.06054 = 0.06603 0.00940 0.01503 0.01876 AFIX 13 H16 2 -0.481211 0.226374 0.418153 11.00000 -1.20000 AFIX 0 F6 6 0.085230 0.332811 0.814186 11.00000 0.23382 0.28611 = 0.11076 0.10080 0.10331 0.22061 C4 1 -0.239012 0.049343 0.074184 11.00000 0.04089 0.05452 = 0.04359 -0.00937 -0.00106 0.00149 AFIX 23 H4A 2 -0.230673 0.085601 0.035596 11.00000 -1.20000 H4B 2 -0.311900 0.000861 0.058513 11.00000 -1.20000 AFIX 0 C37 1 1.054141 0.759535 1.020660 11.00000 0.04702 0.07080 = 0.03906 0.01077 0.00079 0.02529 AFIX 23 H37A 2 1.089871 0.804139 0.992162 11.00000 -1.20000 H37B 2 1.091799 0.784412 1.076526 11.00000 -1.20000 AFIX 0 PART 2 F4 6 0.198253 0.278084 0.846673 10.50000 0.16280 0.19377 = 0.04334 0.05791 0.05169 0.14175 PART 0 O6 4 0.527174 0.941236 0.876137 11.00000 0.16142 0.09647 = 0.09168 -0.00474 -0.00744 0.06308 C32 1 -0.122953 0.362929 0.694915 11.00000 0.05354 0.05755 = 0.06193 0.01919 0.00773 0.02426 AFIX 23 H32A 2 -0.062245 0.370954 0.734420 11.00000 -1.20000 H32B 2 -0.137353 0.312294 0.650232 11.00000 -1.20000 AFIX 0 C56 1 0.299512 0.128198 0.269020 11.00000 0.07221 0.06817 = 0.05109 0.01589 0.03162 0.02422 AFIX 137 H56A 2 0.302979 0.187325 0.287775 11.00000 -1.50000 H56B 2 0.294278 0.115192 0.212231 11.00000 -1.50000 H56C 2 0.363198 0.127177 0.295457 11.00000 -1.50000 AFIX 0 C2 1 -0.162113 0.006897 0.069425 11.00000 0.06266 0.05294 = 0.06438 -0.01241 0.00775 0.01426 AFIX 13 H2A 2 -0.088841 0.055277 0.091985 11.00000 -1.20000 AFIX 0 O7 4 0.435888 0.898806 0.754344 11.00000 0.09011 0.13596 = 0.10825 0.00228 0.00635 0.01835 C55 1 0.098661 0.050659 0.238174 11.00000 0.07386 0.10249 = 0.04115 0.00510 0.00888 0.03250 AFIX 137 H55A 2 0.036663 0.005210 0.249363 11.00000 -1.50000 H55B 2 0.097666 0.034648 0.182183 11.00000 -1.50000 H55C 2 0.097748 0.108679 0.252016 11.00000 -1.50000 AFIX 0 C54 1 0.202795 -0.035511 0.262972 11.00000 0.10652 0.05443 = 0.06092 0.00221 0.03683 0.02898 AFIX 137 H54A 2 0.265670 -0.033124 0.294506 11.00000 -1.50000 H54B 2 0.204334 -0.048748 0.207284 11.00000 -1.50000 H54C 2 0.139772 -0.082338 0.271661 11.00000 -1.50000 AFIX 0 C59 1 0.099366 -0.015292 0.614400 11.00000 0.08951 0.07276 = 0.08361 0.05067 0.04574 0.04184 AFIX 137 H59A 2 0.128798 0.044122 0.650695 11.00000 -1.50000 H59B 2 0.090149 -0.059901 0.644342 11.00000 -1.50000 H59C 2 0.031061 -0.028632 0.582432 11.00000 -1.50000 AFIX 0 C62 1 0.494845 0.955077 0.809844 11.00000 0.06421 0.09431 = 0.08308 0.00480 0.02323 0.03007 C58 1 0.286399 0.011352 0.610530 11.00000 0.07060 0.10779 = 0.10919 0.06694 0.00955 0.03865 AFIX 137 H58A 2 0.331820 0.001845 0.576727 11.00000 -1.50000 H58B 2 0.280423 -0.024125 0.648911 11.00000 -1.50000 H58C 2 0.316938 0.074706 0.638107 11.00000 -1.50000 AFIX 0 C15 1 -0.494953 0.239942 0.535128 11.00000 0.05270 0.10130 = 0.11716 -0.00116 0.04080 0.02599 AFIX 137 H15A 2 -0.469361 0.223376 0.580571 11.00000 -1.50000 H15B 2 -0.572015 0.208879 0.520809 11.00000 -1.50000 H15C 2 -0.471609 0.304540 0.548337 11.00000 -1.50000 AFIX 0 C60 1 0.129687 -0.116371 0.510230 11.00000 0.17838 0.04454 = 0.07668 0.02887 0.02786 0.04339 AFIX 137 H60A 2 0.065365 -0.130875 0.472218 11.00000 -1.50000 H60B 2 0.113219 -0.156292 0.545098 11.00000 -1.50000 H60C 2 0.181425 -0.123908 0.482267 11.00000 -1.50000 AFIX 0 C17 1 -0.487110 0.109853 0.448205 11.00000 0.05603 0.07130 = 0.13228 0.01042 0.03838 0.01091 AFIX 137 H17A 2 -0.470633 0.089018 0.398832 11.00000 -1.50000 H17B 2 -0.563162 0.078982 0.444019 11.00000 -1.50000 H17C 2 -0.450269 0.097129 0.491120 11.00000 -1.50000 AFIX 0 C38 1 1.065925 0.675774 0.988860 11.00000 0.09299 0.09794 = 0.14004 0.04851 0.05852 0.06479 PART 2 AFIX 13 H38A 2 1.045101 0.639754 1.027811 10.50000 -1.20000 AFIX 13 PART 0 PART 1 H38 2 1.039419 0.663186 0.931058 10.50000 -1.20000 AFIX 0 PART 0 PART 2 F3 6 0.248496 0.379257 0.774115 10.50000 0.13027 0.07282 = 0.13189 0.01872 0.06433 0.02713 PART 0 C1 1 -0.169608 -0.036130 -0.018050 11.00000 0.13072 0.07376 = 0.08187 -0.00390 0.04721 0.03366 AFIX 137 H1A 2 -0.241014 -0.083675 -0.041291 11.00000 -1.50000 H1B 2 -0.119173 -0.061197 -0.020257 11.00000 -1.50000 H1C 2 -0.153331 0.009527 -0.047404 11.00000 -1.50000 AFIX 0 PART 2 F2 6 0.090697 0.298031 0.689890 10.50000 0.13385 0.19962 = 0.05752 0.02529 0.00487 0.10922 PART 0 C33 1 -0.219906 0.339778 0.731616 11.00000 0.08813 0.11293 = 0.12911 0.07222 0.06303 0.04138 AFIX 13 H33 2 -0.278790 0.335296 0.691493 11.00000 -1.20000 AFIX 0 PART 2 F1 6 0.042863 0.205263 0.764663 10.50000 0.16823 0.17158 = 0.17149 0.04864 0.04189 0.06605 PART 0 C3 1 -0.184276 -0.063135 0.118220 11.00000 0.17574 0.09326 = 0.06997 0.00261 -0.00445 0.07160 AFIX 137 H3A 2 -0.174318 -0.033944 0.173438 11.00000 -1.50000 H3B 2 -0.135638 -0.089833 0.113572 11.00000 -1.50000 H3C 2 -0.256864 -0.109836 0.098451 11.00000 -1.50000 AFIX 0 C64 1 0.463391 0.835388 0.952091 11.00000 0.07263 0.11207 = 0.15318 0.01537 0.02899 0.02417 AFIX 137 H64A 2 0.424990 0.771808 0.949354 11.00000 -1.50000 H64B 2 0.420017 0.865397 0.965744 11.00000 -1.50000 H64C 2 0.529077 0.862011 0.992223 11.00000 -1.50000 AFIX 0 C63 1 0.487801 0.845930 0.874639 11.00000 0.15423 0.08833 = 0.13485 0.01866 0.02257 0.06703 AFIX 23 H63A 2 0.541817 0.825680 0.864686 11.00000 -1.20000 H63B 2 0.423683 0.809564 0.832277 11.00000 -1.20000 AFIX 0 C40 1 1.186561 0.701138 0.995468 11.00000 0.12833 0.19323 = 0.28303 0.12313 0.12396 0.12409 AFIX 137 H40A 2 1.211491 0.732065 0.955325 11.00000 -1.50000 H40B 2 1.196202 0.646737 0.987559 11.00000 -1.50000 H40C 2 1.226798 0.740340 1.047616 11.00000 -1.50000 AFIX 0 C61 1 0.538927 1.053915 0.815102 11.00000 0.18134 0.11096 = 0.15774 0.05104 0.07156 0.05709 AFIX 137 H61A 2 0.486885 1.074858 0.827214 11.00000 -1.50000 H61B 2 0.555121 1.064388 0.764847 11.00000 -1.50000 H61C 2 0.603307 1.086467 0.856651 11.00000 -1.50000 AFIX 0 C34 1 -0.254476 0.247676 0.749016 11.00000 0.13992 0.15404 = 0.23019 0.13378 0.07986 0.02648 AFIX 137 H34A 2 -0.283516 0.201019 0.699499 11.00000 -1.50000 H34B 2 -0.308295 0.238234 0.780011 11.00000 -1.50000 H34C 2 -0.193594 0.245225 0.778599 11.00000 -1.50000 AFIX 0 C35 1 -0.205772 0.405287 0.800074 11.00000 0.25968 0.14321 = 0.23494 0.03179 0.19549 0.03433 AFIX 137 H35A 2 -0.133295 0.430917 0.830651 11.00000 -1.50000 H35B 2 -0.254657 0.377483 0.831978 11.00000 -1.50000 H35C 2 -0.219630 0.452568 0.784732 11.00000 -1.50000 AFIX 0 PART 2 C39A 1 1.011707 0.616513 0.917523 10.50000 0.11305 0.06479 = 0.07684 0.00520 0.01976 0.05053 AFIX 137 H39A 2 0.935952 0.594086 0.914397 10.50000 -1.50000 H39B 2 1.029891 0.566537 0.911350 10.50000 -1.50000 H39C 2 1.030427 0.646449 0.875701 10.50000 -1.50000 AFIX 0 PART 0 PART 1 C39 1 1.002982 0.588423 1.004863 10.50000 0.11705 0.08216 = 0.15235 0.01505 0.01768 0.05084 AFIX 137 H39D 2 1.040585 0.583721 1.052550 10.50000 -1.50000 H39E 2 0.992460 0.539857 0.960449 10.50000 -1.50000 H39F 2 0.934495 0.584230 1.012117 10.50000 -1.50000 AFIX 0 C65 1 0.439446 0.256184 0.805866 11.00000 0.20854 0.20914 = 0.21095 0.05123 0.03841 0.09540 F3A 6 0.228322 0.331153 0.842168 10.50000 0.12144 0.16601 = 0.09444 -0.04425 0.00809 0.02481 F5A 6 0.044984 0.214922 0.693785 10.50000 0.09611 0.21429 = 0.09056 -0.00553 -0.01288 0.01099 F4A 6 0.097195 0.196650 0.806507 10.50000 0.16462 0.10535 = 0.11607 0.07546 0.08288 0.06342 F2A 6 0.173240 0.352473 0.722474 10.50000 0.24174 0.09023 = 0.15347 0.08305 0.13251 0.09624 C66 1 0.508122 0.354292 0.853654 10.50000 0.15841 0.15898 = 0.15865 0.04139 0.03588 0.07087 C67 1 0.612398 0.462360 0.990102 10.50000 0.15955 0.15892 = 0.15941 0.04144 0.03571 0.07074 C68 1 0.725649 0.487713 0.991768 10.50000 0.14492 0.14217 = 0.14541 0.03678 0.03180 0.06446 O8 4 0.511935 0.410015 0.824972 10.50000 0.20766 0.20649 = 0.20425 0.06166 0.04304 0.08977 PART 0 O9 4 0.541762 0.368931 0.924368 11.00000 0.14784 0.14740 = 0.14868 0.04003 0.03546 0.06415 PART 2 C65A 1 0.661542 0.484133 1.007045 10.50000 0.11696 0.11318 = 0.11974 0.03262 0.02537 0.05084 C66A 1 0.596277 0.453671 0.928326 10.50000 0.13443 0.13245 = 0.13261 0.03637 0.02950 0.05871 C67A 1 0.463594 0.303793 0.842284 10.50000 0.14974 0.14985 = 0.14936 0.03841 0.03392 0.06677 C68A 1 0.462737 0.219601 0.877135 10.50000 0.18451 0.18150 = 0.18361 0.04819 0.04303 0.08212 O8A 4 0.576293 0.462737 0.859466 10.50000 0.15497 0.15071 = 0.14690 0.04370 0.02972 0.06679 HKLF 4 REM s_a.res in P-1 REM R1 = 0.0745 for 9806 Fo > 4sig(Fo) and 0.0889 for all 12457 data REM 919 parameters refined using 384 restraints END WGHT 0.1303 2.2613 REM Highest difference peak 1.014, deepest hole -0.614, 1-sigma level 0.061 Q1 1 0.4655 0.2543 0.7377 11.00000 0.05 1.01 Q2 1 0.5037 0.3427 0.7785 11.00000 0.05 0.70 Q3 1 -0.4875 0.2813 0.4256 11.00000 0.05 0.59 Q4 1 -0.2955 0.3843 0.7191 11.00000 0.05 0.58 Q5 1 0.5082 0.2566 0.8975 11.00000 0.05 0.49 Q6 1 0.5000 0.5000 1.0000 10.50000 0.05 0.47 Q7 1 0.6349 0.5035 1.0386 11.00000 0.05 0.47 Q8 1 0.0169 0.2575 0.7813 11.00000 0.05 0.46 Q9 1 0.0626 0.1702 0.7408 11.00000 0.05 0.44 Q10 1 0.4014 0.2186 0.8323 11.00000 0.05 0.42 Q11 1 0.6635 0.4764 0.9624 11.00000 0.05 0.41 Q12 1 0.5343 0.4655 0.9398 11.00000 0.05 0.40 Q13 1 0.6926 0.4822 1.0350 11.00000 0.05 0.36 Q14 1 0.1172 0.1985 0.7094 11.00000 0.05 0.32 Q15 1 0.1646 0.3588 0.8373 11.00000 0.05 0.31 Q16 1 0.7194 0.4833 0.9345 11.00000 0.05 0.30 Q17 1 0.4195 0.3174 0.8354 11.00000 0.05 0.28 Q18 1 0.1522 0.2314 0.8252 11.00000 0.05 0.26 Q19 1 0.0560 0.2013 0.7963 11.00000 0.05 0.25 Q20 1 0.5620 0.8792 0.8988 11.00000 0.05 0.24 ; _shelx_res_checksum 74951 _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 1.394 _oxdiff_exptl_absorpt_empirical_full_min 0.684 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 P1 P 0.14047(9) 0.28239(7) 0.76778(5) 0.0640(3) Uani 1 1 d . U . . . O3 O -0.16685(14) 0.30571(12) 0.43642(10) 0.0383(4) Uani 1 1 d . . . . . O003 O 0.21855(14) 0.48607(12) 0.48752(10) 0.0396(4) Uani 1 1 d . . . . . O5 O 0.89612(15) 0.73663(14) 0.93203(10) 0.0452(5) Uani 1 1 d . . . . . O1 O 0.24924(14) 0.33736(13) 0.31061(10) 0.0408(4) Uani 1 1 d . . . . . O2 O -0.11872(14) 0.18176(13) 0.17639(10) 0.0433(5) Uani 1 1 d . . . . . O4 O -0.01037(14) 0.45935(14) 0.62207(11) 0.0455(5) Uani 1 1 d . . . . . N2 N 0.04162(16) 0.40801(14) 0.48597(12) 0.0347(5) Uani 1 1 d . . . . . H2 H -0.0056 0.4032 0.5142 0.042 Uiso 1 1 calc R . . . . N5 N 0.31895(16) 0.35822(13) 0.55208(12) 0.0332(5) Uani 1 1 d . . . . . N1 N 0.09190(16) 0.28839(15) 0.22228(12) 0.0356(5) Uani 1 1 d . . . . . H1 H 0.0609 0.2690 0.1722 0.043 Uiso 1 1 calc R . . . . N4 N 0.45952(17) 0.63590(15) 0.83352(12) 0.0397(5) Uani 1 1 d . . . . . N3 N 0.42536(17) 0.61425(15) 0.75886(12) 0.0395(5) Uani 1 1 d . . . . . F5 F 0.2070(2) 0.23896(18) 0.72314(14) 0.0923(8) Uani 1 1 d . U . . . C47 C 0.20196(19) 0.19289(16) 0.48848(15) 0.0335(5) Uani 1 1 d . . . . . C10 C -0.1082(2) 0.29818(17) 0.38069(15) 0.0336(5) Uani 1 1 d . . . . . C11 C 0.00328(19) 0.35376(16) 0.40686(14) 0.0323(5) Uani 1 1 d . . . . . C7 C 0.0266(2) 0.29202(17) 0.27768(14) 0.0332(5) Uani 1 1 d . . . . . C18 C 0.14456(19) 0.46713(16) 0.52290(14) 0.0322(5) Uani 1 1 d . . . . . C41 C 0.36867(19) 0.40519(16) 0.50192(14) 0.0319(5) Uani 1 1 d . . . . . H41 H 0.3323 0.3916 0.4492 0.038 Uiso 1 1 calc R . . . . C6 C 0.19741(19) 0.31237(17) 0.24084(14) 0.0336(5) Uani 1 1 d . . . . . C42 C 0.4733(2) 0.47359(16) 0.52783(14) 0.0326(5) Uani 1 1 d . . . . . C19 C 0.1694(2) 0.50590(16) 0.61170(14) 0.0325(5) Uani 1 1 d . . . . . C8 C -0.0835(2) 0.23659(17) 0.25284(14) 0.0351(5) Uani 1 1 d . . . . . C24 C 0.2773(2) 0.54803(17) 0.64907(15) 0.0346(5) Uani 1 1 d . . . . . H24 H 0.3274 0.5543 0.6176 0.041 Uiso 1 1 calc R . . . . C25 C 0.5720(2) 0.66429(17) 0.85686(15) 0.0365(6) Uani 1 1 d . . . . . C23 C 0.3136(2) 0.58119(17) 0.73130(15) 0.0369(6) Uani 1 1 d . . . . . C48 C 0.19215(19) 0.13331(17) 0.53688(15) 0.0351(5) Uani 1 1 d . . . . . H48 H 0.1897 0.1508 0.5902 0.042 Uiso 1 1 calc R . . . . C27 C 0.7453(2) 0.69143(16) 0.82634(14) 0.0339(5) Uani 1 1 d . . . . . C49 C 0.1859(2) 0.04789(17) 0.50618(16) 0.0379(6) Uani 1 1 d . . . . . C9 C -0.1509(2) 0.24062(17) 0.30445(15) 0.0366(6) Uani 1 1 d . . . . . H9 H -0.2247 0.2045 0.2874 0.044 Uiso 1 1 calc R . . . . C12 C 0.0689(2) 0.35070(17) 0.35409(14) 0.0339(5) Uani 1 1 d . . . . . H12 H 0.1424 0.3885 0.3702 0.041 Uiso 1 1 calc R . . . . C28 C 0.7900(2) 0.71355(18) 0.90932(14) 0.0364(6) Uani 1 1 d . . . . . C52 C 0.2058(2) 0.16788(17) 0.40921(16) 0.0378(6) Uani 1 1 d . . . . . H52 H 0.2119 0.2081 0.3774 0.045 Uiso 1 1 calc R . . . . C26 C 0.6376(2) 0.66782(17) 0.80249(14) 0.0351(5) Uani 1 1 d . . . . . H26 H 0.6077 0.6537 0.7482 0.042 Uiso 1 1 calc R . . . . C20 C 0.0949(2) 0.50015(18) 0.66031(15) 0.0366(6) Uani 1 1 d . . . . . C46 C 0.2056(2) 0.28470(17) 0.52156(16) 0.0379(6) Uani 1 1 d . . . . . H46A H 0.1689 0.3000 0.4798 0.045 Uiso 1 1 calc R . . . . H46B H 0.1681 0.2813 0.5649 0.045 Uiso 1 1 calc R . . . . C51 C 0.2005(2) 0.08286(18) 0.37631(16) 0.0397(6) Uani 1 1 d . . . . . C50 C 0.1906(2) 0.02494(18) 0.42613(16) 0.0404(6) Uani 1 1 d . . . . . H50 H 0.1869 -0.0319 0.4051 0.049 Uiso 1 1 calc R . . . . C29 C 0.7250(2) 0.7110(2) 0.96382(15) 0.0416(6) Uani 1 1 d . . . . . H29 H 0.7544 0.7258 1.0183 0.050 Uiso 1 1 calc R . . . . C30 C 0.6170(2) 0.68679(19) 0.93775(15) 0.0423(6) Uani 1 1 d . . . . . H30 H 0.5746 0.6856 0.9748 0.051 Uiso 1 1 calc R . . . . C21 C 0.1316(2) 0.5362(2) 0.74304(16) 0.0442(6) Uani 1 1 d . . . . . H21 H 0.0824 0.5335 0.7748 0.053 Uiso 1 1 calc R . . . . C22 C 0.2388(2) 0.5754(2) 0.77849(16) 0.0430(6) Uani 1 1 d . . . . . H22 H 0.2617 0.5981 0.8338 0.052 Uiso 1 1 calc R . . . . C45 C 0.3680(2) 0.37502(18) 0.62847(16) 0.0422(6) Uani 1 1 d . . . . . H45 H 0.3319 0.3416 0.6619 0.051 Uiso 1 1 calc R . . . . C13 C -0.2817(2) 0.25101(19) 0.41219(16) 0.0399(6) Uani 1 1 d . . . . . H13A H -0.2988 0.1871 0.3942 0.048 Uiso 1 1 calc R . . . . H13B H -0.3114 0.2685 0.3685 0.048 Uiso 1 1 calc R . . . . C57 C 0.1760(2) -0.0176(2) 0.55980(18) 0.0468(7) Uani 1 1 d . . . . . C36 C 0.9411(2) 0.7485(2) 1.01511(15) 0.0487(7) Uani 1 1 d . . . . . H36A H 0.8987 0.6959 1.0331 0.058 Uiso 1 1 calc R . . . . H36B H 0.9416 0.8020 1.0485 0.058 Uiso 1 1 calc R . . . . C43 C 0.5246(2) 0.49080(18) 0.60697(16) 0.0433(6) Uani 1 1 d . . . . . H43 H 0.5952 0.5356 0.6262 0.052 Uiso 1 1 calc R . . . . C31 C -0.0939(2) 0.4470(2) 0.66615(17) 0.0433(6) Uani 1 1 d . . . . . H31A H -0.1569 0.4427 0.6319 0.052 Uiso 1 1 calc R . . . . H31B H -0.0693 0.4994 0.7116 0.052 Uiso 1 1 calc R . . . . C44 C 0.4716(2) 0.4418(2) 0.65713(17) 0.0481(7) Uani 1 1 d . . . . . H44 H 0.5060 0.4540 0.7101 0.058 Uiso 1 1 calc R . . . . C5 C -0.2245(2) 0.1088(2) 0.15544(19) 0.0563(8) Uani 1 1 d . . . . . H5A H -0.2771 0.1325 0.1536 0.068 Uiso 1 1 calc R . . . . H5B H -0.2343 0.0737 0.1949 0.068 Uiso 1 1 calc R . . . . C14 C -0.3283(2) 0.2665(2) 0.48359(18) 0.0453(7) Uani 1 1 d . . . . . H14A H -0.3082 0.3310 0.5019 0.054 Uiso 1 1 calc R . . . . H14B H -0.2975 0.2488 0.5267 0.054 Uiso 1 1 calc R . . . . C53 C 0.2006(3) 0.0561(2) 0.28755(18) 0.0522(7) Uani 1 1 d . . . . . C16 C -0.4506(2) 0.2132(2) 0.4653(2) 0.0553(8) Uani 1 1 d . . . . . H16 H -0.4812 0.2264 0.4182 0.066 Uiso 1 1 calc R . . . . F6 F 0.0852(4) 0.3328(3) 0.8142(2) 0.1599(18) Uani 1 1 d . U . . . C4 C -0.2390(2) 0.0493(2) 0.07418(18) 0.0575(8) Uani 1 1 d . . . . . H4A H -0.2307 0.0856 0.0356 0.069 Uiso 1 1 calc R . . . . H4B H -0.3119 0.0009 0.0585 0.069 Uiso 1 1 calc R . . . . C37 C 1.0541(2) 0.7595(2) 1.02066(18) 0.0540(8) Uani 1 1 d . . . . . H37A H 1.0899 0.8041 0.9922 0.065 Uiso 1 1 calc R . . . . H37B H 1.0918 0.7844 1.0765 0.065 Uiso 1 1 calc R . . . . F4 F 0.1983(8) 0.2781(8) 0.8467(4) 0.105(3) Uani 0.5 1 d . U P A 2 O6 O 0.5272(4) 0.9412(3) 0.8761(2) 0.1223(13) Uani 1 1 d . U . . . C32 C -0.1230(3) 0.3629(2) 0.6949(2) 0.0578(8) Uani 1 1 d . . . . . H32A H -0.0622 0.3710 0.7344 0.069 Uiso 1 1 calc R . . . . H32B H -0.1374 0.3123 0.6502 0.069 Uiso 1 1 calc R . . . . C56 C 0.2995(3) 0.1282(3) 0.2690(2) 0.0645(9) Uani 1 1 d . . . . . H56A H 0.3030 0.1873 0.2878 0.097 Uiso 1 1 calc GR . . . . H56B H 0.2943 0.1152 0.2122 0.097 Uiso 1 1 calc GR . . . . H56C H 0.3632 0.1272 0.2955 0.097 Uiso 1 1 calc GR . . . . C2 C -0.1621(3) 0.0069(2) 0.0694(2) 0.0687(10) Uani 1 1 d . . . . . H2A H -0.0888 0.0553 0.0920 0.082 Uiso 1 1 calc R . . . . O7 O 0.4359(3) 0.8988(3) 0.7543(2) 0.1285(15) Uani 1 1 d . U . . . C55 C 0.0987(3) 0.0507(3) 0.2382(2) 0.0773(11) Uani 1 1 d . . . . . H55A H 0.0367 0.0052 0.2494 0.116 Uiso 1 1 calc GR . . . . H55B H 0.0977 0.0346 0.1822 0.116 Uiso 1 1 calc GR . . . . H55C H 0.0977 0.1087 0.2520 0.116 Uiso 1 1 calc GR . . . . C54 C 0.2028(4) -0.0355(3) 0.2630(2) 0.0764(11) Uani 1 1 d . . . . . H54A H 0.2657 -0.0331 0.2945 0.115 Uiso 1 1 calc GR . . . . H54B H 0.2043 -0.0487 0.2073 0.115 Uiso 1 1 calc GR . . . . H54C H 0.1398 -0.0823 0.2717 0.115 Uiso 1 1 calc GR . . . . C59 C 0.0994(3) -0.0153(3) 0.6144(2) 0.0730(11) Uani 1 1 d . . . . . H59A H 0.1288 0.0441 0.6507 0.110 Uiso 1 1 calc GR . . . . H59B H 0.0901 -0.0599 0.6443 0.110 Uiso 1 1 calc GR . . . . H59C H 0.0311 -0.0286 0.5824 0.110 Uiso 1 1 calc GR . . . . C62 C 0.4948(4) 0.9551(4) 0.8098(3) 0.0844(12) Uani 1 1 d . U . . . C58 C 0.2864(3) 0.0114(3) 0.6105(3) 0.0917(15) Uani 1 1 d . . . . . H58A H 0.3318 0.0018 0.5767 0.138 Uiso 1 1 calc GR . . . . H58B H 0.2804 -0.0241 0.6489 0.138 Uiso 1 1 calc GR . . . . H58C H 0.3169 0.0747 0.6381 0.138 Uiso 1 1 calc GR . . . . C15 C -0.4950(3) 0.2399(3) 0.5351(3) 0.0954(16) Uani 1 1 d . . . . . H15A H -0.4694 0.2234 0.5806 0.143 Uiso 1 1 calc GR . . . . H15B H -0.5720 0.2089 0.5208 0.143 Uiso 1 1 calc GR . . . . H15C H -0.4716 0.3045 0.5483 0.143 Uiso 1 1 calc GR . . . . C60 C 0.1297(5) -0.1164(3) 0.5102(3) 0.1003(17) Uani 1 1 d . . . . . H60A H 0.0654 -0.1309 0.4722 0.150 Uiso 1 1 calc GR . . . . H60B H 0.1132 -0.1563 0.5451 0.150 Uiso 1 1 calc GR . . . . H60C H 0.1814 -0.1239 0.4823 0.150 Uiso 1 1 calc GR . . . . C17 C -0.4871(3) 0.1099(3) 0.4482(3) 0.0933(15) Uani 1 1 d . . . . . H17A H -0.4706 0.0890 0.3988 0.140 Uiso 1 1 calc GR . . . . H17B H -0.5632 0.0790 0.4440 0.140 Uiso 1 1 calc GR . . . . H17C H -0.4503 0.0971 0.4911 0.140 Uiso 1 1 calc GR . . . . C38 C 1.0659(4) 0.6758(4) 0.9889(4) 0.0968(15) Uani 1 1 d D . . . . H38A H 1.0451 0.6398 1.0278 0.116 Uiso 0.5 1 calc R . P B 2 H38 H 1.0394 0.6632 0.9311 0.116 Uiso 0.5 1 calc R . P C 1 F3 F 0.2485(7) 0.3793(5) 0.7741(6) 0.116(3) Uani 0.5 1 d . U P A 2 C1 C -0.1696(5) -0.0361(3) -0.0180(3) 0.1008(17) Uani 1 1 d . . . . . H1A H -0.2410 -0.0837 -0.0413 0.151 Uiso 1 1 calc GR . . . . H1B H -0.1192 -0.0612 -0.0203 0.151 Uiso 1 1 calc GR . . . . H1C H -0.1533 0.0095 -0.0474 0.151 Uiso 1 1 calc GR . . . . F2 F 0.0907(9) 0.2980(10) 0.6899(4) 0.121(3) Uani 0.5 1 d . U P A 2 C33 C -0.2199(4) 0.3398(4) 0.7316(4) 0.1016(16) Uani 1 1 d . . . . . H33 H -0.2788 0.3353 0.6915 0.122 Uiso 1 1 calc R . . . . F1 F 0.0429(9) 0.2053(8) 0.7647(8) 0.173(4) Uani 0.5 1 d . U P A 2 C3 C -0.1843(5) -0.0631(4) 0.1182(3) 0.115(2) Uani 1 1 d . . . . . H3A H -0.1743 -0.0339 0.1734 0.172 Uiso 1 1 calc GR . . . . H3B H -0.1356 -0.0898 0.1136 0.172 Uiso 1 1 calc GR . . . . H3C H -0.2569 -0.1098 0.0985 0.172 Uiso 1 1 calc GR . . . . C64 C 0.4634(4) 0.8354(4) 0.9521(4) 0.121(2) Uani 1 1 d . U . . . H64A H 0.4250 0.7718 0.9494 0.181 Uiso 1 1 calc GR . . . . H64B H 0.4200 0.8654 0.9657 0.181 Uiso 1 1 calc GR . . . . H64C H 0.5291 0.8620 0.9922 0.181 Uiso 1 1 calc GR . . . . C63 C 0.4878(6) 0.8459(4) 0.8746(4) 0.124(2) Uani 1 1 d . U . . . H63A H 0.5418 0.8257 0.8647 0.148 Uiso 1 1 calc R . . . . H63B H 0.4237 0.8096 0.8323 0.148 Uiso 1 1 calc R . . . . C40 C 1.1866(6) 0.7011(6) 0.9955(6) 0.167(3) Uani 1 1 d . . . . . H40A H 1.2115 0.7321 0.9553 0.250 Uiso 1 1 calc GR . . . . H40B H 1.1962 0.6467 0.9876 0.250 Uiso 1 1 calc GR . . . . H40C H 1.2268 0.7403 1.0476 0.250 Uiso 1 1 calc GR . . . . C61 C 0.5389(7) 1.0539(5) 0.8151(5) 0.147(3) Uani 1 1 d . U . . . H61A H 0.4869 1.0749 0.8272 0.221 Uiso 1 1 calc GR . . . . H61B H 0.5551 1.0644 0.7648 0.221 Uiso 1 1 calc GR . . . . H61C H 0.6033 1.0865 0.8567 0.221 Uiso 1 1 calc GR . . . . C34 C -0.2545(6) 0.2477(5) 0.7490(5) 0.173(3) Uani 1 1 d . . . . . H34A H -0.2835 0.2010 0.6995 0.259 Uiso 1 1 calc GR . . . . H34B H -0.3083 0.2382 0.7800 0.259 Uiso 1 1 calc GR . . . . H34C H -0.1936 0.2452 0.7786 0.259 Uiso 1 1 calc GR . . . . C35 C -0.2058(9) 0.4053(6) 0.8001(6) 0.221(6) Uani 1 1 d . . . . . H35A H -0.1333 0.4309 0.8307 0.331 Uiso 1 1 calc GR . . . . H35B H -0.2547 0.3775 0.8320 0.331 Uiso 1 1 calc GR . . . . H35C H -0.2196 0.4526 0.7847 0.331 Uiso 1 1 calc GR . . . . C39A C 1.0117(8) 0.6165(6) 0.9175(5) 0.083(2) Uani 0.5 1 d D . P D 2 H39A H 0.9360 0.5941 0.9144 0.125 Uiso 0.5 1 calc GR . P D 2 H39B H 1.0299 0.5665 0.9114 0.125 Uiso 0.5 1 calc GR . P D 2 H39C H 1.0304 0.6464 0.8757 0.125 Uiso 0.5 1 calc GR . P D 2 C39 C 1.0030(10) 0.5884(7) 1.0049(8) 0.118(4) Uani 0.5 1 d D . P D 1 H39D H 1.0406 0.5837 1.0526 0.178 Uiso 0.5 1 calc GR . P D 1 H39E H 0.9925 0.5399 0.9604 0.178 Uiso 0.5 1 calc GR . P D 1 H39F H 0.9345 0.5842 1.0121 0.178 Uiso 0.5 1 calc GR . P D 1 C65 C 0.4394(10) 0.2562(8) 0.8059(7) 0.210(4) Uani 1 1 d D U . E 1 F3A F 0.2283(8) 0.3312(8) 0.8422(6) 0.154(5) Uani 0.5 1 d . U P A 1 F5A F 0.0450(6) 0.2149(9) 0.6938(5) 0.164(4) Uani 0.5 1 d . U P A 1 F4A F 0.0972(8) 0.1967(5) 0.8065(5) 0.116(2) Uani 0.5 1 d . U P A 1 F2A F 0.1732(13) 0.3525(6) 0.7225(8) 0.138(4) Uani 0.5 1 d . U P A 1 C66 C 0.5081(16) 0.3543(12) 0.8537(9) 0.159(4) Uani 0.5 1 d D U P E 1 C67 C 0.6124(13) 0.4624(12) 0.9901(12) 0.159(5) Uani 0.5 1 d D U P E 1 C68 C 0.7256(13) 0.4877(11) 0.9918(10) 0.144(4) Uani 0.5 1 d D U P E 1 O8 O 0.5119(13) 0.4100(10) 0.8250(9) 0.206(4) Uani 0.5 1 d D U P E 1 O9 O 0.5418(4) 0.3689(4) 0.9244(3) 0.1481(15) Uani 1 1 d D U . . . C65A C 0.6615(13) 0.4841(11) 1.0070(7) 0.117(3) Uani 0.5 1 d D U P E 2 C66A C 0.5963(11) 0.4537(9) 0.9283(9) 0.133(3) Uani 0.5 1 d D U P E 2 C67A C 0.4636(15) 0.3038(12) 0.8423(9) 0.150(4) Uani 0.5 1 d D U P E 2 C68A C 0.4627(16) 0.2196(10) 0.8771(11) 0.183(5) Uani 0.5 1 d D U P E 2 O8A O 0.5763(9) 0.4627(8) 0.8595(7) 0.151(3) Uani 0.5 1 d D U P E 2 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 P1 0.0825(7) 0.0820(7) 0.0446(5) 0.0243(4) 0.0299(4) 0.0454(5) O3 0.0303(9) 0.0419(10) 0.0369(9) 0.0038(8) 0.0095(7) 0.0126(8) O003 0.0348(9) 0.0416(10) 0.0317(9) 0.0037(7) 0.0104(7) 0.0084(8) O5 0.0385(10) 0.0666(13) 0.0250(9) 0.0070(8) 0.0042(7) 0.0210(9) O1 0.0335(9) 0.0559(11) 0.0235(8) 0.0047(8) 0.0055(7) 0.0134(8) O2 0.0343(9) 0.0440(10) 0.0312(9) -0.0042(8) 0.0032(7) 0.0051(8) O4 0.0332(10) 0.0617(12) 0.0360(10) 0.0050(9) 0.0105(8) 0.0183(9) N2 0.0310(10) 0.0395(11) 0.0296(10) 0.0039(9) 0.0088(8) 0.0135(9) N5 0.0347(11) 0.0257(10) 0.0357(11) 0.0068(8) 0.0120(9) 0.0093(8) N1 0.0333(11) 0.0424(12) 0.0221(9) 0.0031(8) 0.0043(8) 0.0111(9) N4 0.0372(12) 0.0434(12) 0.0303(11) 0.0038(9) 0.0076(9) 0.0124(10) N3 0.0364(12) 0.0432(12) 0.0293(11) 0.0018(9) 0.0068(9) 0.0119(10) F5 0.135(2) 0.0933(17) 0.0716(14) 0.0200(12) 0.0520(15) 0.0651(17) C47 0.0273(12) 0.0285(12) 0.0379(13) 0.0064(10) 0.0092(10) 0.0064(10) C10 0.0329(12) 0.0346(13) 0.0337(12) 0.0096(10) 0.0092(10) 0.0146(10) C11 0.0336(12) 0.0315(12) 0.0291(12) 0.0064(9) 0.0064(10) 0.0128(10) C7 0.0336(13) 0.0357(13) 0.0271(12) 0.0066(10) 0.0073(10) 0.0130(10) C18 0.0326(12) 0.0300(12) 0.0318(12) 0.0054(10) 0.0073(10) 0.0130(10) C41 0.0346(12) 0.0288(12) 0.0287(12) 0.0050(9) 0.0087(10) 0.0114(10) C6 0.0342(13) 0.0338(13) 0.0258(12) 0.0058(9) 0.0075(10) 0.0091(10) C42 0.0360(13) 0.0258(11) 0.0301(12) 0.0051(9) 0.0095(10) 0.0086(10) C19 0.0349(13) 0.0309(12) 0.0304(12) 0.0055(9) 0.0091(10) 0.0141(10) C8 0.0353(13) 0.0338(13) 0.0293(12) 0.0036(10) 0.0045(10) 0.0115(10) C24 0.0350(13) 0.0330(12) 0.0319(12) 0.0040(10) 0.0113(10) 0.0122(10) C25 0.0359(13) 0.0370(13) 0.0300(12) 0.0046(10) 0.0080(10) 0.0115(11) C23 0.0348(13) 0.0367(13) 0.0328(13) 0.0035(10) 0.0081(10) 0.0122(11) C48 0.0307(12) 0.0355(13) 0.0341(13) 0.0096(10) 0.0089(10) 0.0092(10) C27 0.0369(13) 0.0321(12) 0.0255(12) 0.0036(9) 0.0070(10) 0.0101(10) C49 0.0303(12) 0.0349(13) 0.0457(15) 0.0124(11) 0.0094(11) 0.0110(10) C9 0.0294(12) 0.0358(13) 0.0364(13) 0.0049(10) 0.0046(10) 0.0095(10) C12 0.0301(12) 0.0349(13) 0.0312(12) 0.0058(10) 0.0060(10) 0.0106(10) C28 0.0366(13) 0.0394(14) 0.0273(12) 0.0050(10) 0.0054(10) 0.0134(11) C52 0.0342(13) 0.0340(13) 0.0407(14) 0.0121(11) 0.0125(11) 0.0088(10) C26 0.0368(13) 0.0353(13) 0.0245(11) 0.0036(10) 0.0061(10) 0.0099(10) C20 0.0359(13) 0.0386(13) 0.0348(13) 0.0075(10) 0.0099(10) 0.0164(11) C46 0.0307(13) 0.0324(13) 0.0466(15) 0.0103(11) 0.0142(11) 0.0088(10) C51 0.0358(13) 0.0374(14) 0.0388(14) 0.0063(11) 0.0133(11) 0.0099(11) C50 0.0395(14) 0.0323(13) 0.0465(15) 0.0069(11) 0.0139(11) 0.0133(11) C29 0.0464(15) 0.0519(16) 0.0215(11) 0.0036(11) 0.0062(10) 0.0202(13) C30 0.0427(15) 0.0506(16) 0.0283(13) 0.0038(11) 0.0114(11) 0.0175(12) C21 0.0403(14) 0.0530(16) 0.0353(14) 0.0034(12) 0.0149(11) 0.0185(13) C22 0.0421(15) 0.0508(16) 0.0300(13) 0.0023(11) 0.0099(11) 0.0178(12) C45 0.0497(16) 0.0357(14) 0.0362(14) 0.0110(11) 0.0158(12) 0.0119(12) C13 0.0282(13) 0.0402(14) 0.0449(15) 0.0054(11) 0.0066(11) 0.0118(11) C57 0.0498(16) 0.0417(15) 0.0520(16) 0.0201(13) 0.0115(13) 0.0200(13) C36 0.0510(17) 0.0673(19) 0.0249(13) 0.0043(12) 0.0030(11) 0.0281(15) C43 0.0402(14) 0.0364(14) 0.0348(13) 0.0048(11) 0.0041(11) 0.0025(11) C31 0.0361(14) 0.0544(17) 0.0435(15) 0.0133(12) 0.0136(11) 0.0224(12) C44 0.0513(17) 0.0441(15) 0.0339(14) 0.0096(12) 0.0063(12) 0.0082(13) C5 0.0304(14) 0.0594(19) 0.0497(17) -0.0088(14) 0.0035(12) 0.0031(13) C14 0.0354(14) 0.0460(16) 0.0502(16) 0.0059(12) 0.0143(12) 0.0155(12) C53 0.0572(18) 0.0478(17) 0.0410(16) 0.0043(13) 0.0170(13) 0.0148(14) C16 0.0347(15) 0.0605(19) 0.066(2) 0.0094(15) 0.0150(14) 0.0188(14) F6 0.234(4) 0.286(5) 0.111(2) 0.101(3) 0.103(3) 0.221(4) C4 0.0409(16) 0.0545(18) 0.0436(16) -0.0094(14) -0.0011(13) 0.0015(14) C37 0.0470(17) 0.071(2) 0.0391(15) 0.0108(14) 0.0008(12) 0.0253(15) F4 0.163(8) 0.194(9) 0.043(3) 0.058(5) 0.052(4) 0.142(8) O6 0.161(4) 0.096(3) 0.092(2) -0.0047(19) -0.007(2) 0.063(2) C32 0.0535(18) 0.0576(19) 0.062(2) 0.0192(15) 0.0077(15) 0.0243(15) C56 0.072(2) 0.068(2) 0.0511(19) 0.0159(16) 0.0316(17) 0.0242(18) C2 0.063(2) 0.053(2) 0.064(2) -0.0124(16) 0.0078(17) 0.0143(16) O7 0.090(3) 0.136(3) 0.108(3) 0.002(2) 0.006(2) 0.018(2) C55 0.074(2) 0.102(3) 0.0412(18) 0.0051(18) 0.0089(17) 0.032(2) C54 0.107(3) 0.054(2) 0.061(2) 0.0022(16) 0.037(2) 0.029(2) C59 0.090(3) 0.073(2) 0.084(3) 0.051(2) 0.046(2) 0.042(2) C62 0.064(2) 0.094(3) 0.083(3) 0.005(2) 0.023(2) 0.030(2) C58 0.071(3) 0.108(4) 0.109(3) 0.067(3) 0.010(2) 0.039(2) C15 0.053(2) 0.101(3) 0.117(4) -0.001(3) 0.041(2) 0.026(2) C60 0.178(5) 0.045(2) 0.077(3) 0.0289(19) 0.028(3) 0.043(3) C17 0.056(2) 0.071(3) 0.132(4) 0.010(3) 0.038(2) 0.0109(19) C38 0.093(3) 0.098(3) 0.140(5) 0.049(3) 0.059(3) 0.065(3) F3 0.130(6) 0.073(4) 0.132(6) 0.019(4) 0.064(5) 0.027(4) C1 0.131(4) 0.074(3) 0.082(3) -0.004(2) 0.047(3) 0.034(3) F2 0.134(7) 0.200(9) 0.058(3) 0.025(5) 0.005(4) 0.109(6) C33 0.088(3) 0.113(4) 0.129(4) 0.072(4) 0.063(3) 0.041(3) F1 0.168(4) 0.172(4) 0.171(4) 0.049(2) 0.042(2) 0.066(2) C3 0.176(6) 0.093(4) 0.070(3) 0.003(3) -0.004(3) 0.072(4) C64 0.073(3) 0.112(4) 0.153(6) 0.015(4) 0.029(3) 0.024(3) C63 0.154(5) 0.088(4) 0.135(5) 0.019(3) 0.023(4) 0.067(4) C40 0.128(5) 0.193(7) 0.283(10) 0.123(7) 0.124(6) 0.124(6) C61 0.181(7) 0.111(5) 0.158(6) 0.051(4) 0.072(5) 0.057(5) C34 0.140(6) 0.154(6) 0.230(9) 0.134(6) 0.080(6) 0.026(5) C35 0.260(11) 0.143(7) 0.235(10) 0.032(7) 0.195(9) 0.034(7) C39A 0.113(7) 0.065(5) 0.077(5) 0.005(4) 0.020(5) 0.051(5) C39 0.117(9) 0.082(7) 0.152(11) 0.015(7) 0.018(8) 0.051(7) C65 0.209(4) 0.209(4) 0.211(4) 0.051(2) 0.038(2) 0.095(2) F3A 0.121(6) 0.166(9) 0.094(7) -0.044(6) 0.008(5) 0.025(6) F5A 0.096(5) 0.214(9) 0.091(5) -0.006(6) -0.013(4) 0.011(5) F4A 0.165(6) 0.105(4) 0.116(5) 0.075(4) 0.083(5) 0.063(5) F2A 0.242(11) 0.090(6) 0.153(8) 0.083(6) 0.133(8) 0.096(6) C66 0.158(4) 0.159(4) 0.159(4) 0.0414(15) 0.0359(13) 0.071(2) C67 0.160(5) 0.159(5) 0.159(5) 0.0414(15) 0.0357(15) 0.071(2) C68 0.145(5) 0.142(5) 0.145(5) 0.037(2) 0.032(2) 0.064(3) O8 0.208(5) 0.206(5) 0.204(5) 0.062(2) 0.043(2) 0.090(3) O9 0.1478(18) 0.1474(17) 0.1487(17) 0.0400(10) 0.0355(10) 0.0641(11) C65A 0.117(4) 0.113(4) 0.120(4) 0.033(2) 0.025(2) 0.051(2) C66A 0.134(4) 0.132(4) 0.133(4) 0.0364(14) 0.0295(13) 0.0587(18) C67A 0.150(4) 0.150(4) 0.149(4) 0.0384(15) 0.0339(14) 0.067(2) C68A 0.185(6) 0.182(5) 0.184(6) 0.048(2) 0.043(2) 0.082(3) O8A 0.155(4) 0.151(4) 0.147(3) 0.044(2) 0.030(2) 0.067(2) 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' 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' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_3 F5 P1 F3 82.1(3) . F5 P1 F4A 88.6(3) . F6 P1 F5 174.8(2) . F6 P1 F3 92.9(3) . F6 P1 F2 87.7(3) . F6 P1 F5A 101.1(5) . F6 P1 F4A 94.6(3) . F4 P1 F5 87.7(3) . F4 P1 F6 90.7(3) . F4 P1 F3 88.0(5) . F4 P1 F2 173.7(7) . F2 P1 F5 93.3(3) . F2 P1 F3 86.1(5) . F1 P1 F5 103.6(5) . F1 P1 F6 81.5(5) . F1 P1 F4 93.6(6) . F1 P1 F3 174.2(6) . F1 P1 F2 92.2(7) . F3A P1 F5 93.3(5) . F3A P1 F6 82.8(5) . F3A P1 F5A 169.8(8) . F3A P1 F4A 87.0(6) . F5A P1 F5 83.3(4) . F5A P1 F4A 83.3(6) . F2A P1 F5 88.0(3) . F2A P1 F6 89.3(3) . F2A P1 F3A 99.5(8) . F2A P1 F5A 90.0(7) . F2A P1 F4A 172.8(6) . C10 O3 C13 117.04(19) . C28 O5 C36 118.8(2) . C8 O2 C5 117.4(2) . C20 O4 C31 121.2(2) . C18 N2 C11 127.3(2) . C41 N5 C46 119.2(2) . C45 N5 C41 121.8(2) . C45 N5 C46 119.0(2) . C6 N1 C7 126.0(2) . N3 N4 C25 113.2(2) . N4 N3 C23 116.2(2) . C48 C47 C46 120.3(2) . C52 C47 C48 120.4(2) . C52 C47 C46 119.3(2) . O3 C10 C11 114.9(2) . O3 C10 C9 124.7(2) . C9 C10 C11 120.4(2) . N2 C11 C10 117.4(2) . C12 C11 N2 123.8(2) . C12 C11 C10 118.8(2) . C8 C7 N1 118.2(2) . C12 C7 N1 122.1(2) . C12 C7 C8 119.7(2) . O003 C18 N2 122.8(2) . O003 C18 C19 119.2(2) . N2 C18 C19 117.8(2) . N5 C41 C42 120.9(2) . O1 C6 N1 122.6(2) . O1 C6 C27 118.9(2) 2_666 N1 C6 C27 118.5(2) 2_666 C41 C42 C42 120.4(3) 2_666 C41 C42 C43 117.4(2) . C43 C42 C42 122.3(3) 2_666 C24 C19 C18 115.3(2) . C24 C19 C20 117.7(2) . C20 C19 C18 127.0(2) . O2 C8 C7 115.9(2) . O2 C8 C9 124.1(2) . C7 C8 C9 120.0(2) . C23 C24 C19 122.8(2) . C26 C25 N4 123.5(2) . C30 C25 N4 117.7(2) . C30 C25 C26 118.8(2) . C24 C23 N3 114.6(2) . C24 C23 C22 118.8(2) . C22 C23 N3 126.6(2) . C49 C48 C47 120.5(2) . C28 C27 C6 126.7(2) 2_666 C26 C27 C6 115.1(2) 2_666 C26 C27 C28 118.2(2) . C48 C49 C50 117.7(2) . C48 C49 C57 120.5(2) . C50 C49 C57 121.8(2) . C10 C9 C8 120.1(2) . C7 C12 C11 121.1(2) . O5 C28 C27 117.6(2) . O5 C28 C29 122.8(2) . C29 C28 C27 119.6(2) . C47 C52 C51 120.8(2) . C27 C26 C25 122.4(2) . O4 C20 C19 116.5(2) . O4 C20 C21 123.9(2) . C21 C20 C19 119.6(2) . N5 C46 C47 111.7(2) . C52 C51 C53 119.3(3) . C50 C51 C52 117.4(2) . C50 C51 C53 123.2(3) . C51 C50 C49 123.2(2) . C30 C29 C28 120.7(2) . C25 C30 C29 120.4(2) . C22 C21 C20 121.3(2) . C21 C22 C23 119.8(2) . N5 C45 C44 119.6(2) . O3 C13 C14 107.7(2) . C59 C57 C49 110.9(2) . C59 C57 C60 106.3(3) . C58 C57 C49 108.3(3) . C58 C57 C59 109.4(3) . C58 C57 C60 110.2(4) . C60 C57 C49 111.6(3) . O5 C36 C37 107.4(2) . C44 C43 C42 120.5(2) . O4 C31 C32 110.9(2) . C45 C44 C43 119.8(3) . O2 C5 C4 108.0(2) . C13 C14 C16 112.9(2) . C51 C53 C56 110.0(2) . C51 C53 C55 108.2(3) . C55 C53 C56 109.4(3) . C54 C53 C51 112.5(3) . C54 C53 C56 107.9(3) . C54 C53 C55 108.9(3) . C14 C16 C17 111.6(3) . C15 C16 C14 111.0(3) . C15 C16 C17 107.5(3) . C5 C4 C2 115.2(3) . C38 C37 C36 116.6(3) . C62 O6 C63 113.7(4) . C31 C32 C33 113.1(3) . C4 C2 C1 110.4(4) . C4 C2 C3 110.9(4) . C3 C2 C1 110.8(4) . O6 C62 C61 111.0(5) . O7 C62 O6 124.9(6) . O7 C62 C61 124.0(6) . C37 C38 C40 109.2(5) . C39A C38 C37 124.5(6) . C39A C38 C40 107.8(6) . C39 C38 C37 123.0(6) . C39 C38 C40 114.7(6) . C34 C33 C32 110.5(5) . C35 C33 C32 114.1(5) . C35 C33 C34 110.3(6) . O6 C63 C64 108.0(5) . O8 C66 C65 118.7(15) . O8 C66 O9 122.0(18) . O9 C66 C65 118.1(14) . C68 C67 O9 108.7(13) . C66 O9 C67 130.3(13) . C66A O9 C67A 118.4(10) . O9 C66A C65A 100.1(12) . O8A C66A O9 106.6(12) . O8A C66A C65A 151.7(14) . O9 C67A C68A 87.0(10) . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 P1 F5 1.593(2) . P1 F6 1.552(3) . P1 F4 1.534(6) . P1 F3 1.671(7) . P1 F2 1.561(6) . P1 F1 1.427(11) . P1 F3A 1.499(9) . P1 F5A 1.586(7) . P1 F4A 1.615(5) . P1 F2A 1.478(6) . O3 C10 1.370(3) . O3 C13 1.442(3) . O003 C18 1.232(3) . O5 C28 1.357(3) . O5 C36 1.447(3) . O1 C6 1.234(3) . O2 C8 1.368(3) . O2 C5 1.424(3) . O4 C20 1.358(3) . O4 C31 1.445(3) . N2 C11 1.402(3) . N2 C18 1.353(3) . N5 C41 1.347(3) . N5 C46 1.501(3) . N5 C45 1.341(3) . N1 C7 1.422(3) . N1 C6 1.341(3) . N4 N3 1.257(3) . N4 C25 1.425(3) . N3 C23 1.412(3) . C47 C48 1.393(4) . C47 C52 1.382(4) . C47 C46 1.513(3) . C10 C11 1.408(3) . C10 C9 1.380(3) . C11 C12 1.389(3) . C7 C8 1.390(3) . C7 C12 1.389(3) . C18 C19 1.499(3) . C41 C42 1.387(3) . C6 C27 1.507(3) 2_666 C42 C42 1.492(5) 2_666 C42 C43 1.391(4) . C19 C24 1.384(3) . C19 C20 1.410(3) . C8 C9 1.397(4) . C24 C23 1.383(3) . C25 C26 1.394(3) . C25 C30 1.383(4) . C23 C22 1.396(4) . C48 C49 1.391(4) . C27 C6 1.507(3) 2_666 C27 C28 1.416(3) . C27 C26 1.378(4) . C49 C50 1.395(4) . C49 C57 1.538(4) . C28 C29 1.391(4) . C52 C51 1.398(4) . C20 C21 1.395(4) . C51 C50 1.390(4) . C51 C53 1.530(4) . C29 C30 1.385(4) . C21 C22 1.370(4) . C45 C44 1.371(4) . C13 C14 1.506(4) . C57 C59 1.530(5) . C57 C58 1.515(5) . C57 C60 1.530(5) . C36 C37 1.506(4) . C43 C44 1.381(4) . C31 C32 1.491(4) . C5 C4 1.510(4) . C14 C16 1.529(4) . C53 C56 1.534(4) . C53 C55 1.531(5) . C53 C54 1.526(5) . C16 C15 1.513(5) . C16 C17 1.540(6) . C4 C2 1.517(5) . C37 C38 1.490(6) . O6 C62 1.282(6) . O6 C63 1.446(7) . C32 C33 1.511(5) . C2 C1 1.532(5) . C2 C3 1.521(7) . O7 C62 1.152(6) . C62 C61 1.483(8) . C38 C40 1.548(7) . C38 C39A 1.340(9) . C38 C39 1.459(11) . C33 C34 1.510(8) . C33 C35 1.394(9) . C64 C63 1.457(8) . C65 C66 1.517(15) . C66 O8 1.119(14) . C66 O9 1.204(14) . C67 C68 1.460(16) . C67 O9 1.585(15) . O9 C66A 1.284(12) . O9 C67A 1.576(15) . C65A C66A 1.422(14) . C66A O8A 1.248(12) . C67A C68A 1.625(16) .