#------------------------------------------------------------------------------ #$Date: 2021-01-04 20:15:54 +0200 (Mon, 04 Jan 2021) $ #$Revision: 260469 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/77/7127752.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_7127752 loop_ _publ_author_name 'Xiao, Tangxin' 'Zhong, Weiwei' 'Yang, Weiwei' 'Qi, Lijie' 'Gao, Yan' 'Sue, Andrew C.-H.' 'Li, Zheng-Yi' 'Sun, Xiao-Qiang' 'Lin, Chen' 'Wang, Leyong' _publ_section_title ; Reversible hydrogen-bonded polymerization regulated by allosteric metal templation. ; _journal_issue 92 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 14385 _journal_page_last 14388 _journal_paper_doi 10.1039/d0cc06381a _journal_volume 56 _journal_year 2020 _chemical_formula_moiety 'C64 H92 F12 K2 N16 O16 P2' _chemical_formula_sum 'C64 H92 F12 K2 N16 O16 P2' _chemical_formula_weight 1709.67 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-10-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-11-01 deposited with the CCDC. 2020-10-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.689(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.5377(3) _cell_length_b 16.9875(3) _cell_length_c 31.4097(5) _cell_measurement_reflns_used 33484 _cell_measurement_temperature 159.99(10) _cell_measurement_theta_max 30.2240 _cell_measurement_theta_min 2.2680 _cell_volume 7748.4(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.43d (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.43d (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)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 159.99(10) _diffrn_detector 'CCD plate' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.827 _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 -48.00 61.00 0.50 11.01 -- -13.65 78.00 -73.00 218 2 \w 39.00 97.00 0.50 11.01 -- 12.17 178.00 120.00 116 3 \w -63.00 29.00 0.50 11.01 -- 12.17 -57.00 -30.00 184 4 \w -22.00 9.00 0.50 11.01 -- -13.65 -99.00 30.00 62 5 \w 36.00 98.00 0.50 11.01 -- 12.17-178.00 150.00 124 6 \w -88.00 21.00 0.50 11.01 -- -13.65 -78.00 162.00 218 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at offset/far, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0193747000 _diffrn_orient_matrix_UB_12 -0.0252477000 _diffrn_orient_matrix_UB_13 0.0151691000 _diffrn_orient_matrix_UB_21 -0.0174429000 _diffrn_orient_matrix_UB_22 -0.0247346000 _diffrn_orient_matrix_UB_23 -0.0167076000 _diffrn_orient_matrix_UB_31 0.0413012000 _diffrn_orient_matrix_UB_32 -0.0222430000 _diffrn_orient_matrix_UB_33 0.0013566000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_unetI/netI 0.0285 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.827 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 89268 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.827 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.169 _diffrn_reflns_theta_min 1.845 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.267 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.75947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.43d (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light colourless' _exptl_crystal_density_diffrn 1.466 _exptl_crystal_description block _exptl_crystal_F_000 3568 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.692 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.056 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1138 _refine_ls_number_reflns 18989 _refine_ls_number_restraints 121 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0523 _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^)+(0.0819P)^2^+2.6556P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1491 _refine_ls_wR_factor_ref 0.1666 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12945 _reflns_number_total 18989 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc06381a2.cif _cod_data_source_block yww-czu-1a _cod_database_code 7127752 _shelx_shelxl_version_number 2018/3 _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 0.949 _shelx_estimated_absorpt_t_min 0.936 _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances O1-C43 \\sim O1-C43A with sigma of 0.02 C42-C43 \\sim C42-C43A with sigma of 0.02 C62-C63 \\sim C62-C63A with sigma of 0.02 C63-C64 \\sim C63A-C64A with sigma of 0.02 C62-C64 \\sim C62-C64A with sigma of 0.04 C27-C28 \\sim C27-C28A with sigma of 0.02 C28-C30 \\sim C28A-C30A with sigma of 0.04 C37-C38 \\sim C37-C38A with sigma of 0.02 C39-C38 \\sim C39A-C38A with sigma of 0.02 C39-C40 \\sim C39A-C40A with sigma of 0.02 C37-C39 \\sim C37-C39A with sigma of 0.04 C38-C40 \\sim C38A-C40A with sigma of 0.04 O15-C11 \\sim O15-C11A with sigma of 0.02 C10-C11 \\sim C10-C11A with sigma of 0.02 C5-C6 \\sim C5-C6A with sigma of 0.02 C6-C7 \\sim C6A-C7A with sigma of 0.02 C5-C7 \\sim C5-C7A with sigma of 0.04 C28-C29 \\sim C28A-C29A with sigma of 0.02 C29-C30 \\sim C29A-C30A with sigma of 0.02 C27-C29 \\sim C27-C29A with sigma of 0.04 C3-C5 \\sim C5-C6A \\sim C6A-C7A \\sim C7A-C8A with sigma of 0.01 C8-C7 \\sim C8A-C7A with sigma of 0.02 C6-C8 \\sim C6A-C8A with sigma of 0.04 C35-C37 \\sim C37-C38A \\sim C38A-C39A with sigma of 0.01 3. Rigid body (RIGU) restrains C37, C38A, C38, C39A, C39, C40, C40A with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001 C27, C28, C28A, C29A, C30A, C30, C29 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001 C5, C6, C6A, C7, C7A, C8A, C8 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001 4. Others Sof(H42C)=Sof(H42D)=Sof(C43A)=Sof(H43C)=Sof(H43D)=1-FVAR(1) Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=FVAR(1) Sof(H62C)=Sof(H62D)=Sof(C63A)=Sof(H63C)=Sof(H63D)=Sof(C64A)=Sof(H64D)= Sof(H64E)=Sof(H64F)=1-FVAR(2) Sof(H62A)=Sof(H62B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C64)=Sof(H64A)=Sof(H64B)= Sof(H64C)=FVAR(2) Sof(H27C)=Sof(H27D)=Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)= Sof(H29D)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(3) Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)= Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(3) Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)= Sof(H39D)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(4) Sof(H37A)=Sof(H37B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C38)=Sof(H38A)=Sof(H38B)= Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(4) Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=1-FVAR(5) Sof(H10A)=Sof(H10B)=Sof(C11)=Sof(H11A)=Sof(H11B)=FVAR(5) Sof(H5BC)=Sof(H5BD)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)= Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=1-FVAR(6) Sof(H5AA)=Sof(H5AB)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C8)=Sof(H8A)=Sof(H8B)= Sof(H8C)=Sof(C7)=Sof(H7A)=Sof(H7B)=FVAR(6) 5.a Secondary CH2 refined with riding coordinates: C22(H22A,H22B), C21(H21A,H21B), C54(H54A,H54B), C53(H53A,H53B), C20(H20A, H20B), C42(H42A,H42B), C42(H42C,H42D), C10(H10A,H10B), C10(H10C,H10D), C52(H52A,H52B), C61(H61A,H61B), C23(H23A,H23B), C27(H27A,H27B), C27(H27C,H27D), C55(H55A,H55B), C45(H45A,H45B), C13(H13A,H13B), C12(H12A,H12B), C44(H44A, H44B), C62(H62A,H62B), C62(H62C,H62D), C11(H11A,H11B), C28(H28A,H28B), C37(H37A,H37B), C37(H37C,H37D), C5(H5AA,H5AB), C5(H5BC,H5BD), C29(H29A,H29B), C63(H63A,H63B), C39(H39A,H39B), C38(H38A,H38B), C43(H43A,H43B), C6(H6A,H6B), C7(H7A,H7B), C43A(H43C,H43D), C63A(H63C,H63D), C28A(H28C,H28D), C29A(H29C, H29D), C38A(H38C,H38D), C39A(H39C,H39D), C11A(H11C,H11D), C6A(H6AA,H6AB), C7A(H7AA,H7AB) 5.b Aromatic/amide H refined with riding coordinates: N3(H3), N6(H6), N14(H14), N7(H7), N10(H10), N1(H1), N0AA(H0AA), N9(H9), N13(H13), N5(H5), N11(H11), N4(H4), C59(H59), C31(H31), C18(H18), C34(H34), C50(H50), C15(H15), C47(H47), C2(H2), C16(H16), C49(H49), C17(H17), C48(H48) 5.c Idealised Me refined with riding coordinates: C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC) 5.d Idealised Me refined as rotating group: C30(H30A,H30B,H30C), C64(H64A,H64B,H64C), C40(H40A,H40B,H40C), C64A(H64D,H64E, H64F), C30A(H30D,H30E,H30F), C40A(H40D,H40E,H40F) ; _shelx_res_file ; TITL yww-czu-1a_a.res in P2(1)/n yww-czu-1a.res created by SHELXL-2018/3 at 22:31:53 on 26-Oct-2019 REM Old TITL yww-czu-1a_a.res in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.189, Rweak 0.003, Alpha 0.029 REM 0.527 for 567 systematic absences, Orientation as input REM Formula found by SHELXT: C63 F12 K2 N17 O14 P2 CELL 0.71073 14.5377 16.9875 31.4097 90 92.689 90 ZERR 4 0.0003 0.0003 0.0005 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F K N O P UNIT 256 368 48 8 64 64 8 SADI O1 C43 O1 C43A SADI C42 C43 C42 C43A SADI C62 C63 C62 C63A SADI C63 C64 C63A C64A SADI 0.04 C62 C64 C62 C64A SADI C27 C28 C27 C28A SADI 0.04 C28 C30 C28A C30A SADI C37 C38 C37 C38A SADI C39 C38 C39A C38A SADI C39 C40 C39A C40A SADI 0.04 C37 C39 C37 C39A SADI 0.04 C38 C40 C38A C40A SADI O15 C11 O15 C11A SADI C10 C11 C10 C11A SADI C5 C6 C5 C6A SADI C6 C7 C6A C7A SADI 0.04 C5 C7 C5 C7A SADI C28 C29 C28A C29A SADI C29 C30 C29A C30A SADI 0.04 C27 C29 C27 C29A SADI 0.01 C3 C5 C5 C6A C6A C7A C7A C8A SADI C8 C7 C8A C7A SADI 0.04 C6 C8 C6A C8A SADI 0.01 C35 C37 C37 C38A C38A C39A RIGU 0.0001 0.0001 C37 C38A C38 C39A C39 C40 C40A RIGU 0.0001 0.0001 C27 C28 C28A C29A C30A C30 C29 RIGU 0.0001 0.0001 C5 C6 C6A C7 C7A C8A C8 L.S. 10 0 0 PLAN 50 SIZE 0.2 0.2 0.25 FREE K1 O1 FREE K1 C44 FREE K1 P1 FREE K1 H43d FREE P2 K2 FREE K2 C21 FREE K2 C11A FREE C53 K1 FREE C43A K1 FREE H11d K2 FREE C12 K2 list 4 fmap 2 53 acta OMIT -4 5 3 REM REM REM WGHT 0.081900 2.655600 FVAR 0.12323 0.41607 0.67298 0.79664 0.71815 0.80367 0.67987 K2 4 0.223035 0.609055 0.678308 11.00000 0.03745 0.03297 = 0.03090 -0.00387 0.00331 0.00326 K1 4 0.279111 0.616525 0.321670 11.00000 0.03850 0.03638 = 0.03092 0.00445 0.00362 -0.00135 P1 7 0.353569 0.587125 0.213385 11.00000 0.03459 0.04737 = 0.03766 0.00538 0.00986 0.00505 P2 7 0.147428 0.570395 0.785873 11.00000 0.03545 0.04665 = 0.03672 -0.00421 0.00794 -0.00224 O12 6 0.329037 0.471975 0.686648 11.00000 0.03053 0.03258 = 0.03229 -0.00373 0.00071 0.00199 O4 6 0.168289 0.481297 0.311517 11.00000 0.03573 0.03822 = 0.03252 0.00095 0.00201 -0.00212 F6 3 0.270260 0.632600 0.234029 11.00000 0.04775 0.07012 = 0.05008 0.01347 0.01286 0.02671 F9 3 0.233466 0.614782 0.767062 11.00000 0.04736 0.07058 = 0.05546 -0.01574 0.01309 -0.02314 O5 6 0.425230 0.562044 0.384752 11.00000 0.04526 0.03740 = 0.03491 0.00127 0.00884 -0.00285 O14 6 0.331384 0.748710 0.696127 11.00000 0.05212 0.03016 = 0.04060 -0.00658 -0.00406 -0.00166 O13 6 0.417079 0.616466 0.703854 11.00000 0.03543 0.03249 = 0.04042 -0.00095 -0.00376 -0.00580 O3 6 0.087430 0.631385 0.299163 11.00000 0.03653 0.03747 = 0.04025 0.00051 -0.00440 0.00520 O11 6 0.294899 0.616734 0.601185 11.00000 0.04962 0.03390 = 0.03313 -0.00009 0.00927 -0.00020 O10 6 0.078200 0.553415 0.614551 11.00000 0.04582 0.03672 = 0.03382 -0.00226 0.00858 0.00125 O2 6 0.178755 0.761601 0.306353 11.00000 0.04870 0.03200 = 0.04331 0.00514 -0.00527 0.00370 O16 6 0.210049 0.615000 0.398607 11.00000 0.04972 0.04444 = 0.03231 0.00067 0.00994 -0.00174 O9 6 0.357790 0.355387 0.544140 11.00000 0.06989 0.02903 = 0.03578 -0.00101 0.00655 0.00018 O7 6 0.125964 0.354974 0.450301 11.00000 0.07047 0.03530 = 0.03714 -0.00410 0.00727 -0.00464 F3 3 0.437272 0.540632 0.194696 11.00000 0.06226 0.07961 = 0.06817 0.00074 0.03324 0.02056 N8 5 0.100443 0.520315 0.545564 11.00000 0.02831 0.03205 = 0.02980 0.00156 0.00207 -0.00030 O6 6 0.447820 0.818631 0.455025 11.00000 0.08111 0.03086 = 0.04297 0.00071 0.01186 -0.00853 F11 3 0.142033 0.633725 0.821818 11.00000 0.06818 0.08855 = 0.07191 -0.04073 0.01840 0.00122 F8 3 0.154374 0.505914 0.748723 11.00000 0.06656 0.07811 = 0.07990 -0.04166 0.02618 -0.02676 N2 5 0.400190 0.525319 0.452932 11.00000 0.02931 0.03120 = 0.03063 -0.00232 0.00176 -0.00014 N3 5 0.365381 0.483452 0.520217 11.00000 0.04014 0.02691 = 0.02773 -0.00135 0.00056 0.00163 AFIX 43 H3 2 0.360408 0.532171 0.527188 11.00000 -1.20000 AFIX 0 O8 6 0.081700 0.815481 0.550205 11.00000 0.08294 0.03148 = 0.04825 0.00015 0.01230 0.00715 N15 5 0.162899 0.649710 0.463627 11.00000 0.03172 0.03314 = 0.02843 0.00172 0.00108 -0.00310 N12 5 0.349138 0.652518 0.537537 11.00000 0.03519 0.02858 = 0.02754 -0.00008 0.00045 0.00104 F10 3 0.060693 0.525125 0.802628 11.00000 0.06655 0.09396 = 0.06571 -0.00039 0.03036 -0.02615 N6 5 0.132078 0.481220 0.477311 11.00000 0.03754 0.03123 = 0.02925 0.00025 0.00038 -0.00308 AFIX 43 H6 2 0.141899 0.529879 0.471485 11.00000 -1.20000 AFIX 0 O15 6 0.139373 0.757832 0.680406 11.00000 0.05893 0.04006 = 0.05993 -0.01547 -0.01270 0.01513 O1 6 0.367163 0.767495 0.328090 11.00000 0.05219 0.04717 = 0.07070 0.02236 -0.01457 -0.01081 N14 5 0.112360 0.689231 0.528668 11.00000 0.04463 0.02785 = 0.03198 -0.00086 0.00307 -0.00180 AFIX 43 H14 2 0.107856 0.640241 0.535150 11.00000 -1.20000 AFIX 0 N7 5 0.091302 0.386915 0.526782 11.00000 0.03902 0.03065 = 0.03290 -0.00108 0.00184 -0.00210 AFIX 43 H7 2 0.097721 0.351925 0.507357 11.00000 -1.20000 AFIX 0 N10 5 0.406221 0.692950 0.473944 11.00000 0.04945 0.02609 = 0.02935 0.00116 0.00349 -0.00045 AFIX 43 H10 2 0.407397 0.644200 0.466606 11.00000 -1.20000 AFIX 0 N1 5 0.399779 0.390521 0.468827 11.00000 0.03959 0.02865 = 0.03241 -0.00167 0.00152 -0.00015 AFIX 43 H1 2 0.391189 0.354573 0.487506 11.00000 -1.20000 AFIX 0 F7 3 0.080643 0.619101 0.754903 11.00000 0.06252 0.08360 = 0.09399 0.02436 -0.02357 -0.00271 N0AA 5 0.321357 0.455151 0.588107 11.00000 0.04619 0.03010 = 0.02871 -0.00034 0.00105 -0.00205 AFIX 43 H0AA 2 0.317591 0.505186 0.591815 11.00000 -1.20000 AFIX 0 N9 5 0.457736 0.718952 0.407593 11.00000 0.04955 0.03235 = 0.03308 0.00357 0.00471 -0.00351 AFIX 43 H9 2 0.445435 0.670420 0.402000 11.00000 -1.20000 AFIX 0 F1 3 0.361079 0.652993 0.179550 11.00000 0.07936 0.10860 = 0.10538 0.06734 0.04550 0.02797 N13 5 0.061522 0.713965 0.595355 11.00000 0.04661 0.03273 = 0.03659 -0.00423 0.00518 0.00448 AFIX 43 H13 2 0.071731 0.664977 0.600620 11.00000 -1.20000 AFIX 0 N5 5 0.172844 0.454868 0.408791 11.00000 0.04735 0.03682 = 0.03010 -0.00067 0.00304 0.00117 AFIX 43 H5 2 0.181600 0.504679 0.406232 11.00000 -1.20000 AFIX 0 F4 3 0.342696 0.518457 0.247770 11.00000 0.07433 0.08141 = 0.11198 0.05009 0.04499 0.03387 F12 3 0.215335 0.518671 0.814989 11.00000 0.08630 0.08345 = 0.09184 0.01734 -0.01914 0.01867 N11 5 0.366473 0.787744 0.523505 11.00000 0.06537 0.02694 = 0.03411 -0.00015 0.00630 0.00060 AFIX 43 H11 2 0.384017 0.823313 0.506171 11.00000 -1.20000 AFIX 0 F5 3 0.422848 0.628513 0.245801 11.00000 0.05926 0.10306 = 0.12379 -0.05135 -0.03299 0.02002 N4 5 0.160638 0.784178 0.481165 11.00000 0.05767 0.03186 = 0.03764 -0.00033 0.00431 -0.00903 AFIX 43 H4 2 0.146469 0.819691 0.499239 11.00000 -1.20000 AFIX 0 C25 1 0.389357 0.466629 0.479506 11.00000 0.02665 0.03142 = 0.02912 -0.00229 -0.00094 0.00013 F2 3 0.281888 0.541515 0.183306 11.00000 0.07579 0.12535 = 0.11213 -0.04452 -0.01163 -0.00957 C57 1 0.106917 0.462985 0.517774 11.00000 0.02500 0.03270 = 0.03053 0.00215 -0.00074 -0.00071 C01F 1 0.146091 0.707408 0.490113 11.00000 0.03350 0.03191 = 0.03144 0.00105 -0.00086 -0.00415 C22 1 0.359692 0.407927 0.662035 11.00000 0.03897 0.03063 = 0.02978 0.00065 0.00583 0.00240 AFIX 23 H22A 2 0.357418 0.359598 0.678400 11.00000 -1.20000 H22B 2 0.422837 0.416637 0.654505 11.00000 -1.20000 AFIX 0 C21 1 0.387528 0.486069 0.723810 11.00000 0.03570 0.03593 = 0.02663 0.00087 0.00237 0.00118 AFIX 23 H21A 2 0.415189 0.436801 0.733365 11.00000 -1.20000 H21B 2 0.350789 0.505935 0.746459 11.00000 -1.20000 AFIX 0 C24 1 0.348379 0.426463 0.551332 11.00000 0.03718 0.03096 = 0.03078 0.00039 -0.00386 -0.00098 C32 1 0.420497 0.508078 0.411482 11.00000 0.02646 0.03538 = 0.03204 -0.00222 0.00289 -0.00314 C60 1 0.078155 0.501256 0.586675 11.00000 0.02787 0.03465 = 0.03224 0.00213 0.00343 0.00196 C33 1 0.315976 0.671106 0.576826 11.00000 0.03332 0.03425 = 0.02973 -0.00236 0.00085 0.00208 C36 1 0.373011 0.710617 0.512696 11.00000 0.03922 0.02768 = 0.02992 -0.00113 -0.00181 0.00242 C54 1 0.131582 0.416310 0.333985 11.00000 0.04499 0.03641 = 0.03534 -0.00179 0.00484 -0.00287 AFIX 23 H54A 2 0.130285 0.369790 0.316059 11.00000 -1.20000 H54B 2 0.069082 0.427878 0.341549 11.00000 -1.20000 AFIX 0 C1 1 0.196404 0.668688 0.424578 11.00000 0.02949 0.04339 = 0.03122 0.00347 0.00133 -0.00444 C53 1 0.110654 0.502071 0.275066 11.00000 0.04045 0.04312 = 0.02893 -0.00239 0.00268 -0.00408 AFIX 23 H53A 2 0.080534 0.455125 0.263682 11.00000 -1.20000 H53B 2 0.148421 0.523464 0.253194 11.00000 -1.20000 AFIX 0 C46 1 0.084857 0.768265 0.308179 11.00000 0.05105 0.04402 = 0.02618 0.00442 -0.00298 0.01468 C26 1 0.423848 0.369187 0.428704 11.00000 0.03193 0.03567 = 0.03434 -0.00753 0.00203 -0.00315 C58 1 0.065314 0.363975 0.566371 11.00000 0.02938 0.03493 = 0.03620 0.00535 0.00073 -0.00182 C20 1 0.461807 0.543855 0.715346 11.00000 0.03188 0.03688 = 0.03263 -0.00058 -0.00179 0.00111 AFIX 23 H20A 2 0.501960 0.550910 0.740601 11.00000 -1.20000 H20B 2 0.498461 0.525457 0.692319 11.00000 -1.20000 AFIX 0 C56 1 0.142784 0.425620 0.444891 11.00000 0.03720 0.03667 = 0.03038 -0.00187 -0.00118 0.00059 C19 1 0.472037 0.681072 0.699814 11.00000 0.04390 0.03792 = 0.02418 -0.00559 -0.00103 -0.01268 C59 1 0.056777 0.420210 0.596079 11.00000 0.03582 0.03632 = 0.03367 0.00497 0.00535 0.00057 AFIX 43 H59 2 0.036974 0.406830 0.622861 11.00000 -1.20000 AFIX 0 C14 1 0.425652 0.752820 0.694797 11.00000 0.05329 0.03905 = 0.02471 -0.00524 -0.00269 -0.01136 C51 1 0.035356 0.697857 0.303996 11.00000 0.04500 0.04458 = 0.02461 0.00631 -0.00176 0.01155 C31 1 0.435890 0.427022 0.400193 11.00000 0.03863 0.03809 = 0.03230 -0.00706 0.00692 -0.00452 AFIX 43 H31 2 0.454260 0.414611 0.373033 11.00000 -1.20000 AFIX 0 C41 1 0.438588 0.748450 0.445190 11.00000 0.04599 0.03199 = 0.03411 0.00382 0.00183 -0.00186 C42 1 0.499507 0.767929 0.375527 11.00000 0.04219 0.04273 = 0.03918 0.00510 0.00750 -0.00898 PART 1 AFIX 23 H42A 2 0.532451 0.734616 0.356315 21.00000 -1.20000 H42B 2 0.543658 0.803407 0.389481 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H42C 2 0.565186 0.757704 0.375920 -21.00000 -1.20000 H42D 2 0.490834 0.822965 0.382526 -21.00000 -1.20000 AFIX 0 PART 0 C9 1 0.084472 0.744690 0.558524 11.00000 0.04434 0.03523 = 0.03577 -0.00379 0.00178 0.00418 C10 1 0.018961 0.763306 0.626922 11.00000 0.04116 0.04278 = 0.04298 -0.00614 0.01008 0.00790 PART 1 AFIX 23 H10A 2 -0.016784 0.730127 0.645083 61.00000 -1.20000 H10B 2 -0.023237 0.799578 0.612286 61.00000 -1.20000 AFIX 23 PART 0 PART 2 H10C 2 0.031478 0.818119 0.620759 -61.00000 -1.20000 H10D 2 -0.047237 0.755827 0.624680 -61.00000 -1.20000 AFIX 0 PART 0 C52 1 0.039296 0.561193 0.285750 11.00000 0.03474 0.04419 = 0.03346 0.00114 -0.00209 -0.00425 AFIX 23 H52A 2 -0.001145 0.571940 0.260990 11.00000 -1.20000 H52B 2 0.002453 0.541607 0.308431 11.00000 -1.20000 AFIX 0 C61 1 0.053880 0.277480 0.572911 11.00000 0.04059 0.03310 = 0.04855 0.00450 0.00058 -0.00296 AFIX 23 H61A 2 0.016766 0.255870 0.549243 11.00000 -1.20000 H61B 2 0.021313 0.268685 0.598744 11.00000 -1.20000 AFIX 0 C18 1 0.567513 0.679501 0.700727 11.00000 0.04377 0.05485 = 0.03193 -0.01005 -0.00031 -0.01384 AFIX 43 H18 2 0.598762 0.632042 0.704423 11.00000 -1.20000 AFIX 0 C23 1 0.298096 0.401114 0.622185 11.00000 0.04700 0.03614 = 0.03111 0.00060 0.00172 -0.01015 AFIX 23 H23A 2 0.301302 0.347603 0.611579 11.00000 -1.20000 H23B 2 0.235031 0.410856 0.629523 11.00000 -1.20000 AFIX 0 C34 1 0.306644 0.752763 0.588360 11.00000 0.04703 0.03685 = 0.03448 -0.00684 0.00410 0.00292 AFIX 43 H34 2 0.282794 0.766088 0.614360 11.00000 -1.20000 AFIX 0 C50 1 -0.059938 0.699118 0.304283 11.00000 0.04354 0.06336 = 0.03342 0.01014 -0.00007 0.01329 AFIX 43 H50 2 -0.093058 0.652426 0.301444 11.00000 -1.20000 AFIX 0 C27 1 0.433520 0.282770 0.419882 11.00000 0.05295 0.03370 = 0.04215 -0.00947 0.00175 -0.00043 PART 1 AFIX 23 H27A 2 0.470771 0.259624 0.443061 41.00000 -1.20000 H27B 2 0.467162 0.276785 0.394130 41.00000 -1.20000 AFIX 23 PART 0 PART 2 H27C 2 0.481554 0.259512 0.438312 -41.00000 -1.20000 H27D 2 0.447588 0.273587 0.390409 -41.00000 -1.20000 AFIX 0 PART 0 C15 1 0.475267 0.821581 0.689548 11.00000 0.07824 0.03848 = 0.03188 -0.00348 -0.00314 -0.01913 AFIX 43 H15 2 0.444629 0.869276 0.685620 11.00000 -1.20000 AFIX 0 C55 1 0.190924 0.401739 0.373451 11.00000 0.05323 0.04385 = 0.03389 -0.00149 0.00487 0.01123 AFIX 23 H55A 2 0.181647 0.347962 0.382705 11.00000 -1.20000 H55B 2 0.254959 0.407037 0.366534 11.00000 -1.20000 AFIX 0 C47 1 0.038295 0.838409 0.313331 11.00000 0.07384 0.04357 = 0.03303 0.00236 -0.00384 0.01864 AFIX 43 H47 2 0.070983 0.885253 0.316573 11.00000 -1.20000 AFIX 0 C35 1 0.332275 0.809675 0.561687 11.00000 0.06151 0.03290 = 0.03986 -0.00599 0.00356 0.00284 C2 1 0.215108 0.749749 0.415081 11.00000 0.04834 0.04682 = 0.03727 0.00863 0.00536 -0.01101 AFIX 43 H2 2 0.239259 0.763114 0.389153 11.00000 -1.20000 AFIX 0 C45 1 0.230238 0.832478 0.301502 11.00000 0.06964 0.03312 = 0.04793 0.01225 -0.01366 -0.00180 AFIX 23 H45A 2 0.229591 0.863744 0.327328 11.00000 -1.20000 H45B 2 0.203682 0.863480 0.278082 11.00000 -1.20000 AFIX 0 C13 1 0.282708 0.820246 0.703446 11.00000 0.07685 0.03139 = 0.04478 -0.01451 -0.01408 0.00486 AFIX 23 H13A 2 0.280709 0.852799 0.678048 11.00000 -1.20000 H13B 2 0.312853 0.849619 0.726619 11.00000 -1.20000 AFIX 0 C16 1 0.570849 0.819067 0.690169 11.00000 0.07863 0.05975 = 0.03403 -0.00783 0.00429 -0.03957 AFIX 43 H16 2 0.604097 0.865160 0.686537 11.00000 -1.20000 AFIX 0 C49 1 -0.106071 0.770085 0.308810 11.00000 0.05073 0.08031 = 0.03770 0.01139 0.00281 0.02818 AFIX 43 H49 2 -0.170059 0.770943 0.308550 11.00000 -1.20000 AFIX 0 C17 1 0.616308 0.749086 0.696099 11.00000 0.05375 0.06613 = 0.03995 -0.01186 0.00174 -0.02775 AFIX 43 H17 2 0.680333 0.748091 0.697039 11.00000 -1.20000 AFIX 0 C3 1 0.197865 0.806078 0.443452 11.00000 0.06206 0.03965 = 0.04467 0.00717 0.00302 -0.01376 C12 1 0.188187 0.797611 0.714519 11.00000 0.07488 0.04843 = 0.05322 -0.02552 -0.00387 0.01962 AFIX 23 H12A 2 0.191740 0.763620 0.739357 11.00000 -1.20000 H12B 2 0.154378 0.844544 0.721853 11.00000 -1.20000 AFIX 0 C48 1 -0.057168 0.838940 0.313665 11.00000 0.07517 0.06592 = 0.03565 0.00414 0.00294 0.03792 AFIX 43 H48 2 -0.088188 0.886200 0.317198 11.00000 -1.20000 AFIX 0 C44 1 0.326185 0.809261 0.292708 11.00000 0.06932 0.04249 = 0.05996 0.02634 -0.00166 -0.01147 AFIX 23 H44A 2 0.325788 0.776257 0.267499 11.00000 -1.20000 H44B 2 0.362230 0.855933 0.287257 11.00000 -1.20000 AFIX 0 C62 1 0.146771 0.234132 0.576390 11.00000 0.05265 0.03825 = 0.07929 -0.00335 -0.00815 0.00276 PART 1 AFIX 23 H62A 2 0.185466 0.253755 0.554404 31.00000 -1.20000 H62B 2 0.177077 0.246330 0.603766 31.00000 -1.20000 AFIX 23 PART 0 PART 2 H62C 2 0.186572 0.266630 0.594753 -31.00000 -1.20000 H62D 2 0.135517 0.186537 0.592395 -31.00000 -1.20000 AFIX 0 PART 0 PART 1 C11 1 0.086970 0.809888 0.654503 61.00000 0.04166 0.03308 = 0.04187 -0.00710 0.00707 0.00949 AFIX 23 H11A 2 0.127064 0.839835 0.636725 61.00000 -1.20000 H11B 2 0.054440 0.846514 0.672103 61.00000 -1.20000 AFIX 0 C28 1 0.344607 0.235746 0.414524 41.00000 0.04993 0.02665 = 0.05826 -0.00784 -0.00018 0.00407 AFIX 23 H28A 2 0.302620 0.264242 0.395190 41.00000 -1.20000 H28B 2 0.358403 0.186003 0.401066 41.00000 -1.20000 AFIX 0 PART 0 C37 1 0.324564 0.897289 0.568852 11.00000 0.11427 0.03518 = 0.06231 -0.01014 0.01721 0.00048 PART 1 AFIX 23 H37A 2 0.269133 0.915140 0.553376 51.00000 -1.20000 H37B 2 0.315126 0.905356 0.598907 51.00000 -1.20000 AFIX 23 PART 0 PART 2 H37C 2 0.284347 0.908974 0.591813 -51.00000 -1.20000 H37D 2 0.301966 0.924130 0.543186 -51.00000 -1.20000 AFIX 0 PART 0 C5 1 0.217977 0.891999 0.438726 11.00000 0.13673 0.03726 = 0.08243 0.01229 0.01606 -0.01919 PART 1 AFIX 23 H5AA 2 0.234900 0.901364 0.409651 71.00000 -1.20000 H5AB 2 0.271123 0.904786 0.457263 71.00000 -1.20000 AFIX 23 PART 0 PART 2 H5BC 2 0.230407 0.914953 0.466683 -71.00000 -1.20000 H5BD 2 0.272583 0.898469 0.422473 -71.00000 -1.20000 AFIX 0 PART 0 PART 1 C29 1 0.296151 0.218848 0.454437 41.00000 0.06209 0.04851 = 0.06485 -0.01036 0.00701 -0.01417 AFIX 23 H29A 2 0.278040 0.268183 0.467146 41.00000 -1.20000 H29B 2 0.338363 0.192479 0.474574 41.00000 -1.20000 AFIX 0 C63 1 0.139049 0.148070 0.572171 31.00000 0.07021 0.03570 = 0.04708 -0.00007 0.00356 0.00513 AFIX 23 H63A 2 0.108565 0.135513 0.544883 31.00000 -1.20000 H63B 2 0.101201 0.128005 0.594365 31.00000 -1.20000 AFIX 0 C39 1 0.479597 0.934117 0.587268 51.00000 0.11059 0.04685 = 0.09542 0.01483 0.01029 0.00186 AFIX 23 H39A 2 0.494536 0.878492 0.586613 51.00000 -1.20000 H39B 2 0.462431 0.946889 0.615930 51.00000 -1.20000 AFIX 0 C38 1 0.399924 0.949308 0.557196 51.00000 0.10704 0.02650 = 0.08032 -0.00160 0.01801 0.01045 AFIX 23 H38A 2 0.381007 1.003917 0.559008 51.00000 -1.20000 H38B 2 0.416546 0.938705 0.528201 51.00000 -1.20000 AFIX 0 C30 1 0.211475 0.167865 0.446527 41.00000 0.07310 0.07634 = 0.09513 -0.01258 0.00947 -0.03259 AFIX 137 H30A 2 0.166188 0.196391 0.429489 41.00000 -1.50000 H30B 2 0.186495 0.154094 0.473284 41.00000 -1.50000 H30C 2 0.228124 0.120827 0.431798 41.00000 -1.50000 AFIX 0 C43 1 0.425875 0.816898 0.349356 21.00000 0.04974 0.03047 = 0.03943 0.00593 0.01097 -0.00733 AFIX 23 H43A 2 0.392157 0.849999 0.368378 21.00000 -1.20000 H43B 2 0.455884 0.850623 0.329307 21.00000 -1.20000 AFIX 0 C64 1 0.233754 0.106903 0.575409 31.00000 0.09848 0.05741 = 0.10103 0.00260 -0.00085 0.03470 AFIX 137 H64A 2 0.268855 0.121925 0.551579 31.00000 -1.50000 H64B 2 0.225151 0.050871 0.575248 31.00000 -1.50000 H64C 2 0.266167 0.122304 0.601415 31.00000 -1.50000 AFIX 0 C6 1 0.140416 0.948424 0.448661 71.00000 0.15183 0.04877 = 0.08609 0.02047 0.02545 -0.00613 AFIX 23 H6A 2 0.113059 0.932250 0.474848 71.00000 -1.20000 H6B 2 0.165297 1.000972 0.452901 71.00000 -1.20000 AFIX 0 C40 1 0.566004 0.982185 0.576860 51.00000 0.11363 0.06552 = 0.13585 0.03168 0.00437 -0.00716 AFIX 137 H40A 2 0.584890 0.968305 0.548958 51.00000 -1.50000 H40B 2 0.614909 0.970744 0.597534 51.00000 -1.50000 H40C 2 0.551868 1.037355 0.577624 51.00000 -1.50000 AFIX 0 C8 1 -0.016185 1.003198 0.415981 71.00000 0.20625 0.15246 = 0.13353 -0.05404 -0.01288 0.08317 AFIX 133 H8A 2 -0.065231 0.974457 0.428270 71.00000 -1.50000 H8B 2 -0.035017 1.019278 0.387595 71.00000 -1.50000 H8C 2 -0.001782 1.048857 0.433027 71.00000 -1.50000 AFIX 0 C7 1 0.070348 0.949801 0.414443 71.00000 0.17187 0.08898 = 0.10192 -0.01910 0.00761 0.03684 AFIX 23 H7A 2 0.048406 0.896195 0.410765 71.00000 -1.20000 H7B 2 0.100940 0.963491 0.388672 71.00000 -1.20000 AFIX 0 PART 0 PART 2 C43A 1 0.458356 0.752137 0.331745 -21.00000 0.04049 0.04739 = 0.03704 0.00628 0.01125 -0.00516 AFIX 23 H43C 2 0.489704 0.784202 0.311379 -21.00000 -1.20000 H43D 2 0.468514 0.697360 0.324618 -21.00000 -1.20000 AFIX 0 C63A 1 0.196142 0.212817 0.545880 -31.00000 0.05982 0.04830 = 0.06693 0.00169 0.00245 0.00605 AFIX 23 H63C 2 0.220392 0.259905 0.533010 -31.00000 -1.20000 H63D 2 0.156128 0.187417 0.524450 -31.00000 -1.20000 AFIX 0 C64A 1 0.277807 0.156892 0.556583 -31.00000 0.07262 0.06854 = 0.10563 0.00760 0.00423 0.02583 AFIX 137 H64D 2 0.313075 0.149926 0.531774 -31.00000 -1.50000 H64E 2 0.254807 0.106833 0.565468 -31.00000 -1.50000 H64F 2 0.316278 0.179173 0.579158 -31.00000 -1.50000 AFIX 0 C28A 1 0.335247 0.247903 0.429832 -41.00000 0.06664 0.06894 = 0.07151 -0.03617 0.01847 -0.02326 AFIX 23 H28C 2 0.331778 0.245583 0.460571 -41.00000 -1.20000 H28D 2 0.289276 0.285589 0.419529 -41.00000 -1.20000 AFIX 0 C29A 1 0.308700 0.172709 0.413334 -41.00000 0.13088 0.11886 = 0.21014 -0.11988 0.11989 -0.08224 AFIX 23 H29C 2 0.359974 0.137678 0.420176 -41.00000 -1.20000 H29D 2 0.305370 0.178138 0.382558 -41.00000 -1.20000 AFIX 0 C30A 1 0.226300 0.130246 0.424149 -41.00000 0.09080 0.09179 = 0.12944 -0.06227 0.05903 -0.04780 AFIX 137 H30D 2 0.224105 0.080626 0.409509 -41.00000 -1.50000 H30E 2 0.172880 0.160717 0.415739 -41.00000 -1.50000 H30F 2 0.227444 0.121323 0.454350 -41.00000 -1.50000 AFIX 0 C38A 1 0.426126 0.920508 0.580963 -51.00000 0.12131 0.04903 = 0.10800 0.00883 0.00046 -0.00901 AFIX 23 H38C 2 0.442337 0.887374 0.605323 -51.00000 -1.20000 H38D 2 0.460417 0.899524 0.557758 -51.00000 -1.20000 AFIX 0 C39A 1 0.474284 0.998651 0.591680 -51.00000 0.10184 0.04909 = 0.07066 0.00117 0.03035 -0.00571 AFIX 23 H39C 2 0.465622 1.030279 0.566093 -51.00000 -1.20000 H39D 2 0.436939 1.023183 0.612769 -51.00000 -1.20000 AFIX 0 C40A 1 0.572925 1.013790 0.607273 -51.00000 0.10468 0.05943 = 0.09692 -0.00191 0.02267 -0.00736 AFIX 137 H40D 2 0.613651 1.000846 0.585122 -51.00000 -1.50000 H40E 2 0.587473 0.981787 0.631864 -51.00000 -1.50000 H40F 2 0.580139 1.068329 0.614709 -51.00000 -1.50000 AFIX 0 C11A 1 0.052155 0.745788 0.670143 -61.00000 0.06595 0.05011 = 0.03456 -0.00137 0.01640 0.01268 AFIX 23 H11C 2 0.016304 0.776797 0.689307 -61.00000 -1.20000 H11D 2 0.038886 0.690866 0.675667 -61.00000 -1.20000 AFIX 0 C6A 1 0.139671 0.934062 0.416887 -71.00000 0.15573 0.06393 = 0.08560 0.00196 0.00809 0.00373 AFIX 23 H6AA 2 0.161131 0.979422 0.401433 -71.00000 -1.20000 H6AB 2 0.106163 0.899478 0.397085 -71.00000 -1.20000 AFIX 0 C7A 1 0.080866 0.958726 0.451801 -71.00000 0.13742 0.04518 = 0.08752 -0.00488 0.00429 -0.01504 AFIX 23 H7AA 2 0.118814 0.979739 0.475357 -71.00000 -1.20000 H7AB 2 0.047133 0.913816 0.462046 -71.00000 -1.20000 AFIX 0 C8A 1 0.014959 1.020403 0.435102 -71.00000 0.13414 0.04304 = 0.10281 0.00104 0.00733 -0.01735 AFIX 133 H8AA 2 0.016106 1.064436 0.454277 -71.00000 -1.50000 H8AB 2 -0.046106 0.998829 0.432808 -71.00000 -1.50000 H8AC 2 0.032638 1.037472 0.407520 -71.00000 -1.50000 AFIX 0 HKLF 4 REM yww-czu-1a_a.res in P2(1)/n REM wR2 = 0.1666, GooF = S = 1.071, Restrained GooF = 1.089 for all data REM R1 = 0.0523 for 12945 Fo > 4sig(Fo) and 0.0799 for all 18989 data REM 1138 parameters refined using 121 restraints END WGHT 0.0819 2.6554 REM Highest difference peak 0.692, deepest hole -0.532, 1-sigma level 0.056 Q1 1 0.3838 0.5622 0.2598 11.00000 0.05 0.69 Q2 1 0.3184 0.5164 0.2170 11.00000 0.05 0.60 Q3 1 0.4612 0.9056 0.5804 11.00000 0.05 0.54 Q4 1 0.0191 1.0184 0.4163 11.00000 0.05 0.47 Q5 1 0.1183 0.5557 0.7392 11.00000 0.05 0.45 Q6 1 0.1779 0.5003 0.7809 11.00000 0.05 0.44 Q7 1 0.4864 0.9421 0.5505 11.00000 0.05 0.44 Q8 1 0.4128 0.6757 0.2186 11.00000 0.05 0.42 Q9 1 0.3007 0.5969 0.1652 11.00000 0.05 0.41 Q10 1 -0.0624 0.9861 0.4375 11.00000 0.05 0.34 Q11 1 0.1381 0.6792 0.8003 11.00000 0.05 0.31 Q12 1 0.1602 0.9410 0.4173 11.00000 0.05 0.30 Q13 1 -0.0052 1.0166 0.4624 11.00000 0.05 0.30 Q14 1 0.3637 0.7985 0.3418 11.00000 0.05 0.30 Q15 1 0.0900 1.0063 0.4193 11.00000 0.05 0.29 Q16 1 0.2030 0.5748 0.8319 11.00000 0.05 0.27 Q17 1 0.0878 0.6619 0.7775 11.00000 0.05 0.27 Q18 1 0.4810 0.9397 0.5976 11.00000 0.05 0.27 Q19 1 0.1521 0.7823 0.6591 11.00000 0.05 0.26 Q20 1 0.3978 0.5581 0.4607 11.00000 0.05 0.25 Q21 1 0.4047 0.7605 0.3195 11.00000 0.05 0.25 Q22 1 0.2338 0.8762 0.4406 11.00000 0.05 0.25 Q23 1 0.3728 0.8916 0.5795 11.00000 0.05 0.25 Q24 1 0.3753 0.7465 0.5207 11.00000 0.05 0.25 Q25 1 0.1363 0.7471 0.4795 11.00000 0.05 0.24 Q26 1 0.5641 0.9898 0.5507 11.00000 0.05 0.24 Q27 1 0.3415 0.4041 0.6401 11.00000 0.05 0.24 Q28 1 0.2137 0.4178 0.3371 11.00000 0.05 0.23 Q29 1 0.1062 0.5537 0.5401 11.00000 0.05 0.23 Q30 1 0.3741 0.4608 0.5353 11.00000 0.05 0.23 Q31 1 0.2633 0.5305 0.1823 11.00000 0.05 0.22 Q32 1 0.1241 0.4612 0.4645 11.00000 0.05 0.22 Q33 1 0.4179 0.4612 0.4031 11.00000 0.05 0.22 Q34 1 0.2161 0.5003 0.3187 11.00000 0.05 0.21 Q35 1 0.1130 1.0633 0.4610 11.00000 0.05 0.21 Q36 1 0.0739 0.5632 0.8234 11.00000 0.05 0.21 Q37 1 0.1586 0.6766 0.4774 11.00000 0.05 0.21 Q38 1 0.0534 0.5820 0.8025 11.00000 0.05 0.20 Q39 1 0.4086 1.0191 0.5818 11.00000 0.05 0.20 Q40 1 0.0758 0.3847 0.5788 11.00000 0.05 0.20 Q41 1 0.4513 0.6221 0.2371 11.00000 0.05 0.20 Q42 1 0.1693 0.3742 0.4635 11.00000 0.05 0.20 Q43 1 0.2751 0.8749 0.5590 11.00000 0.05 0.20 Q44 1 0.4169 0.5246 0.7188 11.00000 0.05 0.20 Q45 1 0.2132 0.5781 0.4006 11.00000 0.05 0.19 Q46 1 -0.0739 0.8009 0.3132 11.00000 0.05 0.19 Q47 1 0.1866 0.6428 0.7618 11.00000 0.05 0.19 Q48 1 0.3109 0.2396 0.4240 11.00000 0.05 0.19 Q49 1 0.3716 0.6263 0.5393 11.00000 0.05 0.19 Q50 1 0.3998 0.5090 0.4596 11.00000 0.05 0.19 ; _shelx_res_checksum 84239 _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 1.338 _oxdiff_exptl_absorpt_empirical_full_min 0.738 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 K2 K 0.22304(3) 0.60906(2) 0.67831(2) 0.03372(11) Uani 1 1 d . . . . . K1 K 0.27911(3) 0.61652(2) 0.32167(2) 0.03520(11) Uani 1 1 d . . . . . P1 P 0.35357(4) 0.58712(3) 0.21339(2) 0.03962(14) Uani 1 1 d . . . . . P2 P 0.14743(4) 0.57039(3) 0.78587(2) 0.03941(14) Uani 1 1 d . . . . . O12 O 0.32904(9) 0.47198(7) 0.68665(4) 0.0318(3) Uani 1 1 d . . . . . O4 O 0.16829(10) 0.48130(8) 0.31152(4) 0.0355(3) Uani 1 1 d . . . . . F6 F 0.27026(9) 0.63260(8) 0.23403(4) 0.0557(4) Uani 1 1 d . . . . . F9 F 0.23347(10) 0.61478(8) 0.76706(4) 0.0575(4) Uani 1 1 d . . . . . O5 O 0.42523(10) 0.56204(8) 0.38475(4) 0.0390(3) Uani 1 1 d . . . . . O14 O 0.33138(11) 0.74871(8) 0.69613(4) 0.0412(3) Uani 1 1 d . . . . . O13 O 0.41708(10) 0.61647(8) 0.70385(4) 0.0363(3) Uani 1 1 d . . . . . O3 O 0.08743(10) 0.63139(8) 0.29916(4) 0.0383(3) Uani 1 1 d . . . . . O11 O 0.29490(11) 0.61673(8) 0.60118(4) 0.0387(3) Uani 1 1 d . . . . . O10 O 0.07820(10) 0.55342(8) 0.61455(4) 0.0386(3) Uani 1 1 d . . . . . O2 O 0.17876(11) 0.76160(8) 0.30635(5) 0.0416(3) Uani 1 1 d . . . . . O16 O 0.21005(11) 0.61500(8) 0.39861(4) 0.0419(3) Uani 1 1 d . . . . . O9 O 0.35779(12) 0.35539(8) 0.54414(4) 0.0448(4) Uani 1 1 d . . . . . O7 O 0.12596(12) 0.35497(8) 0.45030(5) 0.0475(4) Uani 1 1 d . . . . . F3 F 0.43727(11) 0.54063(10) 0.19470(5) 0.0691(4) Uani 1 1 d . . . . . N8 N 0.10044(11) 0.52031(9) 0.54556(5) 0.0300(3) Uani 1 1 d . . . . . O6 O 0.44782(13) 0.81863(8) 0.45502(5) 0.0514(4) Uani 1 1 d . . . . . F11 F 0.14203(12) 0.63372(10) 0.82182(5) 0.0757(5) Uani 1 1 d . . . . . F8 F 0.15437(11) 0.50591(10) 0.74872(5) 0.0741(5) Uani 1 1 d . . . . . N2 N 0.40019(11) 0.52532(9) 0.45293(5) 0.0304(3) Uani 1 1 d . . . . . N3 N 0.36538(11) 0.48345(9) 0.52022(5) 0.0316(3) Uani 1 1 d . . . . . H3 H 0.360408 0.532171 0.527188 0.038 Uiso 1 1 calc R . . . . O8 O 0.08170(13) 0.81548(9) 0.55021(5) 0.0539(4) Uani 1 1 d . . . . . N15 N 0.16290(11) 0.64971(9) 0.46363(5) 0.0311(3) Uani 1 1 d . . . . . N12 N 0.34914(11) 0.65252(9) 0.53754(5) 0.0305(3) Uani 1 1 d . . . . . F10 F 0.06069(11) 0.52512(11) 0.80263(5) 0.0746(5) Uani 1 1 d . . . . . N6 N 0.13208(11) 0.48122(9) 0.47731(5) 0.0327(3) Uani 1 1 d . . . . . H6 H 0.141899 0.529879 0.471485 0.039 Uiso 1 1 calc R . . . . O15 O 0.13937(12) 0.75783(9) 0.68041(5) 0.0535(4) Uani 1 1 d D . . . . O1 O 0.36716(12) 0.76750(9) 0.32809(6) 0.0572(5) Uani 1 1 d D . . . . N14 N 0.11236(12) 0.68923(9) 0.52867(5) 0.0348(4) Uani 1 1 d . . . . . H14 H 0.107856 0.640241 0.535150 0.042 Uiso 1 1 calc R . . . . N7 N 0.09130(12) 0.38691(9) 0.52678(5) 0.0342(4) Uani 1 1 d . . . . . H7 H 0.097721 0.351925 0.507357 0.041 Uiso 1 1 calc R . . . . N10 N 0.40622(12) 0.69295(9) 0.47394(5) 0.0349(4) Uani 1 1 d . . . . . H10 H 0.407397 0.644200 0.466606 0.042 Uiso 1 1 calc R . . . . N1 N 0.39978(12) 0.39052(9) 0.46883(5) 0.0336(4) Uani 1 1 d . . . . . H1 H 0.391189 0.354573 0.487506 0.040 Uiso 1 1 calc R . . . . F7 F 0.08064(12) 0.61910(10) 0.75490(6) 0.0809(5) Uani 1 1 d . . . . . N0AA N 0.32136(12) 0.45515(9) 0.58811(5) 0.0350(4) Uani 1 1 d . . . . . H0AA H 0.317591 0.505186 0.591815 0.042 Uiso 1 1 calc R . . . . N9 N 0.45774(13) 0.71895(10) 0.40759(5) 0.0382(4) Uani 1 1 d . . . . . H9 H 0.445435 0.670420 0.402000 0.046 Uiso 1 1 calc R . . . . F1 F 0.36108(13) 0.65299(12) 0.17955(6) 0.0965(7) Uani 1 1 d . . . . . N13 N 0.06152(12) 0.71396(10) 0.59536(5) 0.0385(4) Uani 1 1 d . . . . . H13 H 0.071731 0.664977 0.600620 0.046 Uiso 1 1 calc R . . . . N5 N 0.17284(12) 0.45487(10) 0.40879(5) 0.0381(4) Uani 1 1 d . . . . . H5 H 0.181600 0.504679 0.406232 0.046 Uiso 1 1 calc R . . . . F4 F 0.34270(12) 0.51846(10) 0.24777(6) 0.0880(6) Uani 1 1 d . . . . . F12 F 0.21533(13) 0.51867(11) 0.81499(6) 0.0879(6) Uani 1 1 d . . . . . N11 N 0.36647(14) 0.78774(9) 0.52351(5) 0.0420(4) Uani 1 1 d . . . . . H11 H 0.384017 0.823313 0.506171 0.050 Uiso 1 1 calc R . . . . F5 F 0.42285(12) 0.62851(12) 0.24580(7) 0.0965(7) Uani 1 1 d . . . . . N4 N 0.16064(13) 0.78418(10) 0.48117(5) 0.0423(4) Uani 1 1 d . . . . . H4 H 0.146469 0.819691 0.499239 0.051 Uiso 1 1 calc R . . . . C25 C 0.38936(13) 0.46663(10) 0.47951(6) 0.0291(4) Uani 1 1 d . . . . . F2 F 0.28189(14) 0.54151(14) 0.18331(7) 0.1049(7) Uani 1 1 d . . . . . C57 C 0.10692(13) 0.46298(11) 0.51777(6) 0.0295(4) Uani 1 1 d . . . . . C01F C 0.14609(13) 0.70741(11) 0.49011(6) 0.0324(4) Uani 1 1 d . . . . . C22 C 0.35969(14) 0.40793(11) 0.66204(6) 0.0330(4) Uani 1 1 d . . . . . H22A H 0.357418 0.359598 0.678400 0.040 Uiso 1 1 calc R . . . . H22B H 0.422837 0.416637 0.654505 0.040 Uiso 1 1 calc R . . . . C21 C 0.38753(14) 0.48607(11) 0.72381(6) 0.0327(4) Uani 1 1 d . . . . . H21A H 0.415189 0.436801 0.733365 0.039 Uiso 1 1 calc R . . . . H21B H 0.350789 0.505935 0.746459 0.039 Uiso 1 1 calc R . . . . C24 C 0.34838(14) 0.42646(11) 0.55133(6) 0.0331(4) Uani 1 1 d . . . . . C32 C 0.42050(13) 0.50808(11) 0.41148(6) 0.0312(4) Uani 1 1 d . . . . . C60 C 0.07816(13) 0.50126(11) 0.58668(6) 0.0315(4) Uani 1 1 d . . . . . C33 C 0.31598(13) 0.67111(11) 0.57683(6) 0.0325(4) Uani 1 1 d . . . . . C36 C 0.37301(14) 0.71062(10) 0.51270(6) 0.0324(4) Uani 1 1 d . . . . . C54 C 0.13158(15) 0.41631(12) 0.33399(6) 0.0388(5) Uani 1 1 d . . . . . H54A H 0.130285 0.369790 0.316059 0.047 Uiso 1 1 calc R . . . . H54B H 0.069082 0.427878 0.341549 0.047 Uiso 1 1 calc R . . . . C1 C 0.19640(14) 0.66869(12) 0.42458(6) 0.0347(4) Uani 1 1 d . . . . . C53 C 0.11065(15) 0.50207(12) 0.27507(6) 0.0375(4) Uani 1 1 d . . . . . H53A H 0.080534 0.455125 0.263682 0.045 Uiso 1 1 calc R . . . . H53B H 0.148421 0.523464 0.253194 0.045 Uiso 1 1 calc R . . . . C46 C 0.08486(16) 0.76827(12) 0.30818(6) 0.0406(5) Uani 1 1 d . . . . . C26 C 0.42385(14) 0.36919(11) 0.42870(6) 0.0340(4) Uani 1 1 d . . . . . C58 C 0.06531(13) 0.36398(11) 0.56637(6) 0.0335(4) Uani 1 1 d . . . . . C20 C 0.46181(14) 0.54386(11) 0.71535(6) 0.0339(4) Uani 1 1 d . . . . . H20A H 0.501960 0.550910 0.740601 0.041 Uiso 1 1 calc R . . . . H20B H 0.498461 0.525457 0.692319 0.041 Uiso 1 1 calc R . . . . C56 C 0.14278(14) 0.42562(11) 0.44489(6) 0.0348(4) Uani 1 1 d . . . . . C19 C 0.47204(15) 0.68107(11) 0.69981(6) 0.0354(4) Uani 1 1 d . . . . . C59 C 0.05678(14) 0.42021(11) 0.59608(6) 0.0352(4) Uani 1 1 d . . . . . H59 H 0.036974 0.406830 0.622861 0.042 Uiso 1 1 calc R . . . . C14 C 0.42565(16) 0.75282(12) 0.69480(6) 0.0392(5) Uani 1 1 d . . . . . C51 C 0.03536(15) 0.69786(12) 0.30400(6) 0.0382(5) Uani 1 1 d . . . . . C31 C 0.43589(14) 0.42702(11) 0.40019(6) 0.0362(4) Uani 1 1 d . . . . . H31 H 0.454260 0.414611 0.373033 0.043 Uiso 1 1 calc R . . . . C41 C 0.43859(15) 0.74845(11) 0.44519(6) 0.0374(4) Uani 1 1 d . . . . . C42 C 0.49951(15) 0.76793(13) 0.37553(7) 0.0412(5) Uani 1 1 d D . . . . H42A H 0.532451 0.734616 0.356315 0.049 Uiso 0.416(5) 1 calc R . P A 1 H42B H 0.543658 0.803407 0.389481 0.049 Uiso 0.416(5) 1 calc R . P A 1 H42C H 0.565186 0.757704 0.375920 0.049 Uiso 0.584(5) 1 calc R . P A 2 H42D H 0.490834 0.822965 0.382526 0.049 Uiso 0.584(5) 1 calc R . P A 2 C9 C 0.08447(15) 0.74469(12) 0.55852(6) 0.0384(5) Uani 1 1 d . . . . . C10 C 0.01896(15) 0.76331(13) 0.62692(7) 0.0421(5) Uani 1 1 d D . . . . H10A H -0.016784 0.730127 0.645083 0.050 Uiso 0.804(6) 1 calc R . P B 1 H10B H -0.023237 0.799578 0.612286 0.050 Uiso 0.804(6) 1 calc R . P B 1 H10C H 0.031478 0.818119 0.620759 0.050 Uiso 0.196(6) 1 calc R . P B 2 H10D H -0.047237 0.755827 0.624680 0.050 Uiso 0.196(6) 1 calc R . P B 2 C52 C 0.03930(14) 0.56119(12) 0.28575(6) 0.0376(4) Uani 1 1 d . . . . . H52A H -0.001145 0.571940 0.260990 0.045 Uiso 1 1 calc R . . . . H52B H 0.002453 0.541607 0.308431 0.045 Uiso 1 1 calc R . . . . C61 C 0.05388(15) 0.27748(11) 0.57291(7) 0.0408(5) Uani 1 1 d . . . . . H61A H 0.016766 0.255870 0.549243 0.049 Uiso 1 1 calc R . . . . H61B H 0.021313 0.268685 0.598744 0.049 Uiso 1 1 calc R . . . . C18 C 0.56751(16) 0.67950(14) 0.70073(6) 0.0436(5) Uani 1 1 d . . . . . H18 H 0.598762 0.632042 0.704423 0.052 Uiso 1 1 calc R . . . . C23 C 0.29810(16) 0.40111(12) 0.62218(6) 0.0381(5) Uani 1 1 d . . . . . H23A H 0.301302 0.347603 0.611579 0.046 Uiso 1 1 calc R . . . . H23B H 0.235031 0.410856 0.629523 0.046 Uiso 1 1 calc R . . . . C34 C 0.30664(15) 0.75276(12) 0.58836(6) 0.0394(5) Uani 1 1 d . . . . . H34 H 0.282794 0.766088 0.614360 0.047 Uiso 1 1 calc R . . . . C50 C -0.05994(16) 0.69912(15) 0.30428(7) 0.0468(5) Uani 1 1 d . . . . . H50 H -0.093058 0.652426 0.301444 0.056 Uiso 1 1 calc R . . . . C27 C 0.43352(16) 0.28277(12) 0.41988(7) 0.0429(4) Uani 1 1 d D U . . . H27A H 0.470771 0.259624 0.443061 0.052 Uiso 0.797(5) 1 calc R . P C 1 H27B H 0.467162 0.276785 0.394130 0.052 Uiso 0.797(5) 1 calc R . P C 1 H27C H 0.481554 0.259512 0.438312 0.052 Uiso 0.203(5) 1 calc R . P C 2 H27D H 0.447588 0.273587 0.390409 0.052 Uiso 0.203(5) 1 calc R . P C 2 C15 C 0.47527(19) 0.82158(13) 0.68955(7) 0.0497(6) Uani 1 1 d . . . . . H15 H 0.444629 0.869276 0.685620 0.060 Uiso 1 1 calc R . . . . C55 C 0.19092(17) 0.40174(13) 0.37345(6) 0.0436(5) Uani 1 1 d . . . . . H55A H 0.181647 0.347962 0.382705 0.052 Uiso 1 1 calc R . . . . H55B H 0.254959 0.407037 0.366534 0.052 Uiso 1 1 calc R . . . . C47 C 0.03829(19) 0.83841(13) 0.31333(7) 0.0503(6) Uani 1 1 d . . . . . H47 H 0.070983 0.885253 0.316573 0.060 Uiso 1 1 calc R . . . . C35 C 0.33228(17) 0.80968(12) 0.56169(7) 0.0447(5) Uani 1 1 d D . . . . C2 C 0.21511(16) 0.74975(13) 0.41508(7) 0.0440(5) Uani 1 1 d . . . . . H2 H 0.239259 0.763114 0.389153 0.053 Uiso 1 1 calc R . . . . C45 C 0.23024(18) 0.83248(12) 0.30150(8) 0.0507(6) Uani 1 1 d . . . . . H45A H 0.229591 0.863744 0.327328 0.061 Uiso 1 1 calc R . . . . H45B H 0.203682 0.863480 0.278082 0.061 Uiso 1 1 calc R . . . . C13 C 0.28271(19) 0.82025(12) 0.70345(8) 0.0515(6) Uani 1 1 d . . . . . H13A H 0.280709 0.852799 0.678048 0.062 Uiso 1 1 calc R . . . . H13B H 0.312853 0.849619 0.726619 0.062 Uiso 1 1 calc R . . . . C16 C 0.5708(2) 0.81907(15) 0.69017(7) 0.0574(7) Uani 1 1 d . . . . . H16 H 0.604097 0.865160 0.686537 0.069 Uiso 1 1 calc R . . . . C49 C -0.10607(18) 0.77008(17) 0.30881(7) 0.0562(7) Uani 1 1 d . . . . . H49 H -0.170059 0.770943 0.308550 0.067 Uiso 1 1 calc R . . . . C17 C 0.61631(18) 0.74909(15) 0.69610(7) 0.0533(6) Uani 1 1 d . . . . . H17 H 0.680333 0.748091 0.697039 0.064 Uiso 1 1 calc R . . . . C3 C 0.19787(18) 0.80608(13) 0.44345(7) 0.0488(6) Uani 1 1 d D . . . . C12 C 0.1882(2) 0.79761(15) 0.71452(8) 0.0591(7) Uani 1 1 d . . . . . H12A H 0.191740 0.763620 0.739357 0.071 Uiso 1 1 calc R . . . . H12B H 0.154378 0.844544 0.721853 0.071 Uiso 1 1 calc R . . . . C48 C -0.0572(2) 0.83894(16) 0.31367(7) 0.0589(7) Uani 1 1 d . . . . . H48 H -0.088188 0.886200 0.317198 0.071 Uiso 1 1 calc R . . . . C44 C 0.32619(19) 0.80926(14) 0.29271(8) 0.0574(7) Uani 1 1 d . . . . . H44A H 0.325788 0.776257 0.267499 0.069 Uiso 1 1 calc R . . . . H44B H 0.362230 0.855933 0.287257 0.069 Uiso 1 1 calc R . . . . C62 C 0.14677(18) 0.23413(14) 0.57639(10) 0.0571(6) Uani 1 1 d D . . . . H62A H 0.185466 0.253755 0.554404 0.068 Uiso 0.673(5) 1 calc R . P D 1 H62B H 0.177077 0.246330 0.603766 0.068 Uiso 0.673(5) 1 calc R . P D 1 H62C H 0.186572 0.266630 0.594753 0.068 Uiso 0.327(5) 1 calc R . P D 2 H62D H 0.135517 0.186537 0.592395 0.068 Uiso 0.327(5) 1 calc R . P D 2 C11 C 0.08697(18) 0.80989(14) 0.65450(8) 0.0387(8) Uani 0.804(6) 1 d D . P B 1 H11A H 0.127064 0.839835 0.636725 0.046 Uiso 0.804(6) 1 calc R . P B 1 H11B H 0.054440 0.846514 0.672103 0.046 Uiso 0.804(6) 1 calc R . P B 1 C28 C 0.3446(2) 0.23575(16) 0.41452(12) 0.0450(6) Uani 0.797(5) 1 d D U P C 1 H28A H 0.302620 0.264242 0.395190 0.054 Uiso 0.797(5) 1 calc R . P C 1 H28B H 0.358403 0.186003 0.401066 0.054 Uiso 0.797(5) 1 calc R . P C 1 C37 C 0.3246(2) 0.89729(14) 0.56885(9) 0.0702(6) Uani 1 1 d D U . . . H37A H 0.269133 0.915140 0.553376 0.084 Uiso 0.718(5) 1 calc R . P E 1 H37B H 0.315126 0.905356 0.598907 0.084 Uiso 0.718(5) 1 calc R . P E 1 H37C H 0.284347 0.908974 0.591813 0.084 Uiso 0.282(5) 1 calc R . P E 2 H37D H 0.301966 0.924130 0.543186 0.084 Uiso 0.282(5) 1 calc R . P E 2 C5 C 0.2180(3) 0.89200(15) 0.43873(11) 0.0851(8) Uani 1 1 d D U . . . H5AA H 0.234900 0.901364 0.409651 0.102 Uiso 0.680(5) 1 calc R . P F 1 H5AB H 0.271123 0.904786 0.457263 0.102 Uiso 0.680(5) 1 calc R . P F 1 H5BC H 0.230407 0.914953 0.466683 0.102 Uiso 0.320(5) 1 calc R . P F 2 H5BD H 0.272583 0.898469 0.422473 0.102 Uiso 0.320(5) 1 calc R . P F 2 C29 C 0.2962(2) 0.21885(19) 0.45444(11) 0.0584(8) Uani 0.797(5) 1 d D U P C 1 H29A H 0.278040 0.268183 0.467146 0.070 Uiso 0.797(5) 1 calc R . P C 1 H29B H 0.338363 0.192479 0.474574 0.070 Uiso 0.797(5) 1 calc R . P C 1 C63 C 0.1390(3) 0.14807(18) 0.57217(11) 0.0510(10) Uani 0.673(5) 1 d D . P D 1 H63A H 0.108565 0.135513 0.544883 0.061 Uiso 0.673(5) 1 calc R . P D 1 H63B H 0.101201 0.128005 0.594365 0.061 Uiso 0.673(5) 1 calc R . P D 1 C39 C 0.4796(4) 0.9341(3) 0.58727(17) 0.0841(12) Uani 0.718(5) 1 d D U P E 1 H39A H 0.494536 0.878492 0.586613 0.101 Uiso 0.718(5) 1 calc R . P E 1 H39B H 0.462431 0.946889 0.615930 0.101 Uiso 0.718(5) 1 calc R . P E 1 C38 C 0.3999(3) 0.9493(2) 0.55720(14) 0.0709(8) Uani 0.718(5) 1 d D U P E 1 H38A H 0.381007 1.003917 0.559008 0.085 Uiso 0.718(5) 1 calc R . P E 1 H38B H 0.416546 0.938705 0.528201 0.085 Uiso 0.718(5) 1 calc R . P E 1 C30 C 0.2115(3) 0.1679(3) 0.44653(16) 0.0814(12) Uani 0.797(5) 1 d D U P C 1 H30A H 0.166188 0.196391 0.429489 0.122 Uiso 0.797(5) 1 calc GR . P C 1 H30B H 0.186495 0.154094 0.473284 0.122 Uiso 0.797(5) 1 calc GR . P C 1 H30C H 0.228124 0.120827 0.431798 0.122 Uiso 0.797(5) 1 calc GR . P C 1 C43 C 0.4259(4) 0.8169(3) 0.34936(15) 0.0396(14) Uani 0.416(5) 1 d D . P A 1 H43A H 0.392157 0.849999 0.368378 0.048 Uiso 0.416(5) 1 calc R . P A 1 H43B H 0.455884 0.850623 0.329307 0.048 Uiso 0.416(5) 1 calc R . P A 1 C64 C 0.2338(4) 0.1069(3) 0.57541(19) 0.0858(17) Uani 0.673(5) 1 d D . P D 1 H64A H 0.268855 0.121925 0.551579 0.129 Uiso 0.673(5) 1 calc GR . P D 1 H64B H 0.225151 0.050871 0.575248 0.129 Uiso 0.673(5) 1 calc GR . P D 1 H64C H 0.266167 0.122304 0.601415 0.129 Uiso 0.673(5) 1 calc GR . P D 1 C6 C 0.1404(4) 0.9484(3) 0.44866(18) 0.0949(13) Uani 0.680(5) 1 d D U P F 1 H6A H 0.113059 0.932250 0.474848 0.114 Uiso 0.680(5) 1 calc R . P F 1 H6B H 0.165297 1.000972 0.452901 0.114 Uiso 0.680(5) 1 calc R . P F 1 C40 C 0.5660(4) 0.9822(3) 0.5769(2) 0.1050(17) Uani 0.718(5) 1 d D U P E 1 H40A H 0.584890 0.968305 0.548958 0.158 Uiso 0.718(5) 1 calc GR . P E 1 H40B H 0.614909 0.970744 0.597534 0.158 Uiso 0.718(5) 1 calc GR . P E 1 H40C H 0.551868 1.037355 0.577624 0.158 Uiso 0.718(5) 1 calc GR . P E 1 C8 C -0.0162(7) 1.0032(5) 0.4160(3) 0.165(3) Uani 0.680(5) 1 d D U P F 1 H8A H -0.065231 0.974457 0.428270 0.247 Uiso 0.680(5) 1 calc R . P F 1 H8B H -0.035017 1.019278 0.387595 0.247 Uiso 0.680(5) 1 calc R . P F 1 H8C H -0.001782 1.048857 0.433027 0.247 Uiso 0.680(5) 1 calc R . P F 1 C7 C 0.0703(5) 0.9498(4) 0.4144(2) 0.121(2) Uani 0.680(5) 1 d D U P F 1 H7A H 0.048406 0.896195 0.410765 0.145 Uiso 0.680(5) 1 calc R . P F 1 H7B H 0.100940 0.963491 0.388672 0.145 Uiso 0.680(5) 1 calc R . P F 1 C43A C 0.4584(3) 0.7521(2) 0.33174(11) 0.0413(11) Uani 0.584(5) 1 d D . P A 2 H43C H 0.489704 0.784202 0.311379 0.050 Uiso 0.584(5) 1 calc R . P A 2 H43D H 0.468514 0.697360 0.324618 0.050 Uiso 0.584(5) 1 calc R . P A 2 C63A C 0.1961(6) 0.2128(5) 0.5459(3) 0.058(2) Uani 0.327(5) 1 d D . P D 2 H63C H 0.220392 0.259905 0.533010 0.070 Uiso 0.327(5) 1 calc R . P D 2 H63D H 0.156128 0.187417 0.524450 0.070 Uiso 0.327(5) 1 calc R . P D 2 C64A C 0.2778(7) 0.1569(6) 0.5566(4) 0.082(3) Uani 0.327(5) 1 d D . P D 2 H64D H 0.313075 0.149926 0.531774 0.123 Uiso 0.327(5) 1 calc GR . P D 2 H64E H 0.254807 0.106833 0.565468 0.123 Uiso 0.327(5) 1 calc GR . P D 2 H64F H 0.316278 0.179173 0.579158 0.123 Uiso 0.327(5) 1 calc GR . P D 2 C28A C 0.3352(10) 0.2479(9) 0.4298(6) 0.069(4) Uani 0.203(5) 1 d D U P C 2 H28C H 0.331778 0.245583 0.460571 0.082 Uiso 0.203(5) 1 calc R . P C 2 H28D H 0.289276 0.285589 0.419529 0.082 Uiso 0.203(5) 1 calc R . P C 2 C29A C 0.3087(14) 0.1727(11) 0.4133(8) 0.150(5) Uani 0.203(5) 1 d D U P C 2 H29C H 0.359974 0.137678 0.420176 0.180 Uiso 0.203(5) 1 calc R . P C 2 H29D H 0.305370 0.178138 0.382558 0.180 Uiso 0.203(5) 1 calc R . P C 2 C30A C 0.2263(12) 0.1302(10) 0.4241(7) 0.102(6) Uani 0.203(5) 1 d D U P C 2 H30D H 0.224105 0.080626 0.409509 0.153 Uiso 0.203(5) 1 calc GR . P C 2 H30E H 0.172880 0.160717 0.415739 0.153 Uiso 0.203(5) 1 calc GR . P C 2 H30F H 0.227444 0.121323 0.454350 0.153 Uiso 0.203(5) 1 calc GR . P C 2 C38A C 0.4261(7) 0.9205(6) 0.5810(5) 0.093(3) Uani 0.282(5) 1 d D U P E 2 H38C H 0.442337 0.887374 0.605323 0.112 Uiso 0.282(5) 1 calc R . P E 2 H38D H 0.460417 0.899524 0.557758 0.112 Uiso 0.282(5) 1 calc R . P E 2 C39A C 0.4743(7) 0.9987(5) 0.5917(3) 0.073(2) Uani 0.282(5) 1 d D U P E 2 H39C H 0.465622 1.030279 0.566093 0.088 Uiso 0.282(5) 1 calc R . P E 2 H39D H 0.436939 1.023183 0.612769 0.088 Uiso 0.282(5) 1 calc R . P E 2 C40A C 0.5729(8) 1.0138(7) 0.6073(4) 0.086(3) Uani 0.282(5) 1 d D U P E 2 H40D H 0.613651 1.000846 0.585122 0.130 Uiso 0.282(5) 1 calc GR . P E 2 H40E H 0.587473 0.981787 0.631864 0.130 Uiso 0.282(5) 1 calc GR . P E 2 H40F H 0.580139 1.068329 0.614709 0.130 Uiso 0.282(5) 1 calc GR . P E 2 C11A C 0.0522(8) 0.7458(7) 0.6701(3) 0.050(4) Uani 0.196(6) 1 d D . P B 2 H11C H 0.016304 0.776797 0.689307 0.060 Uiso 0.196(6) 1 calc R . P B 2 H11D H 0.038886 0.690866 0.675667 0.060 Uiso 0.196(6) 1 calc R . P B 2 C6A C 0.1397(7) 0.9341(6) 0.4169(3) 0.102(2) Uani 0.320(5) 1 d D U P F 2 H6AA H 0.161131 0.979422 0.401433 0.122 Uiso 0.320(5) 1 calc R . P F 2 H6AB H 0.106163 0.899478 0.397085 0.122 Uiso 0.320(5) 1 calc R . P F 2 C7A C 0.0809(8) 0.9587(6) 0.4518(3) 0.0901(19) Uani 0.320(5) 1 d D U P F 2 H7AA H 0.118814 0.979739 0.475357 0.108 Uiso 0.320(5) 1 calc R . P F 2 H7AB H 0.047133 0.913816 0.462046 0.108 Uiso 0.320(5) 1 calc R . P F 2 C8A C 0.0150(8) 1.0204(5) 0.4351(4) 0.093(2) Uani 0.320(5) 1 d D U P F 2 H8AA H 0.016106 1.064436 0.454277 0.140 Uiso 0.320(5) 1 calc R . P F 2 H8AB H -0.046106 0.998829 0.432808 0.140 Uiso 0.320(5) 1 calc R . P F 2 H8AC H 0.032638 1.037472 0.407520 0.140 Uiso 0.320(5) 1 calc R . P F 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 K2 0.0375(2) 0.0330(2) 0.0309(2) -0.00387(15) 0.00331(17) 0.00326(17) K1 0.0385(3) 0.0364(2) 0.0309(2) 0.00445(16) 0.00362(17) -0.00135(17) P1 0.0346(3) 0.0474(3) 0.0377(3) 0.0054(2) 0.0099(2) 0.0051(2) P2 0.0354(3) 0.0467(3) 0.0367(3) -0.0042(2) 0.0079(2) -0.0022(2) O12 0.0305(7) 0.0326(7) 0.0323(7) -0.0037(5) 0.0007(5) 0.0020(5) O4 0.0357(8) 0.0382(7) 0.0325(7) 0.0009(5) 0.0020(6) -0.0021(6) F6 0.0478(8) 0.0701(9) 0.0501(8) 0.0135(6) 0.0129(6) 0.0267(7) F9 0.0474(8) 0.0706(9) 0.0555(8) -0.0157(7) 0.0131(6) -0.0231(7) O5 0.0453(9) 0.0374(7) 0.0349(7) 0.0013(6) 0.0088(6) -0.0028(6) O14 0.0521(10) 0.0302(7) 0.0406(8) -0.0066(6) -0.0041(7) -0.0017(6) O13 0.0354(8) 0.0325(7) 0.0404(8) -0.0009(5) -0.0038(6) -0.0058(6) O3 0.0365(8) 0.0375(7) 0.0403(8) 0.0005(6) -0.0044(6) 0.0052(6) O11 0.0496(9) 0.0339(7) 0.0331(7) -0.0001(5) 0.0093(6) -0.0002(6) O10 0.0458(9) 0.0367(7) 0.0338(7) -0.0023(6) 0.0086(6) 0.0013(6) O2 0.0487(9) 0.0320(7) 0.0433(8) 0.0051(6) -0.0053(7) 0.0037(6) O16 0.0497(9) 0.0444(8) 0.0323(7) 0.0007(6) 0.0099(6) -0.0017(7) O9 0.0699(11) 0.0290(7) 0.0358(8) -0.0010(6) 0.0066(7) 0.0002(7) O7 0.0705(11) 0.0353(8) 0.0371(8) -0.0041(6) 0.0073(7) -0.0046(7) F3 0.0623(10) 0.0796(11) 0.0682(10) 0.0007(8) 0.0332(8) 0.0206(8) N8 0.0283(9) 0.0321(8) 0.0298(8) 0.0016(6) 0.0021(6) -0.0003(6) O6 0.0811(13) 0.0309(7) 0.0430(9) 0.0007(6) 0.0119(8) -0.0085(7) F11 0.0682(11) 0.0885(12) 0.0719(11) -0.0407(9) 0.0184(8) 0.0012(9) F8 0.0666(10) 0.0781(11) 0.0799(11) -0.0417(9) 0.0262(8) -0.0268(8) N2 0.0293(9) 0.0312(8) 0.0306(8) -0.0023(6) 0.0018(6) -0.0001(6) N3 0.0401(10) 0.0269(7) 0.0277(8) -0.0014(6) 0.0006(7) 0.0016(7) O8 0.0829(13) 0.0315(8) 0.0483(9) 0.0001(6) 0.0123(8) 0.0072(8) N15 0.0317(9) 0.0331(8) 0.0284(8) 0.0017(6) 0.0011(6) -0.0031(6) N12 0.0352(9) 0.0286(8) 0.0275(8) -0.0001(6) 0.0004(6) 0.0010(6) F10 0.0666(11) 0.0940(12) 0.0657(10) -0.0004(8) 0.0304(8) -0.0261(9) N6 0.0375(9) 0.0312(8) 0.0293(8) 0.0003(6) 0.0004(7) -0.0031(7) O15 0.0589(11) 0.0401(8) 0.0599(10) -0.0155(7) -0.0127(8) 0.0151(7) O1 0.0522(11) 0.0472(9) 0.0707(11) 0.0224(8) -0.0146(9) -0.0108(8) N14 0.0446(10) 0.0278(8) 0.0320(8) -0.0009(6) 0.0031(7) -0.0018(7) N7 0.0390(10) 0.0306(8) 0.0329(9) -0.0011(6) 0.0018(7) -0.0021(7) N10 0.0495(11) 0.0261(8) 0.0293(8) 0.0012(6) 0.0035(7) -0.0004(7) N1 0.0396(10) 0.0286(8) 0.0324(8) -0.0017(6) 0.0015(7) -0.0001(7) F7 0.0625(11) 0.0836(12) 0.0940(13) 0.0244(10) -0.0236(9) -0.0027(9) N0AA 0.0462(10) 0.0301(8) 0.0287(8) -0.0003(6) 0.0011(7) -0.0020(7) N9 0.0495(11) 0.0324(8) 0.0331(9) 0.0036(6) 0.0047(8) -0.0035(7) F1 0.0794(13) 0.1086(14) 0.1054(14) 0.0673(12) 0.0455(11) 0.0280(11) N13 0.0466(11) 0.0327(8) 0.0366(9) -0.0042(7) 0.0052(8) 0.0045(7) N5 0.0474(11) 0.0368(9) 0.0301(8) -0.0007(7) 0.0030(7) 0.0012(7) F4 0.0743(11) 0.0814(11) 0.1120(14) 0.0501(10) 0.0450(10) 0.0339(9) F12 0.0863(13) 0.0835(12) 0.0918(13) 0.0173(10) -0.0191(10) 0.0187(10) N11 0.0654(13) 0.0269(8) 0.0341(9) -0.0001(6) 0.0063(8) 0.0006(8) F5 0.0593(11) 0.1031(14) 0.1238(16) -0.0513(12) -0.0330(11) 0.0200(10) N4 0.0577(12) 0.0319(9) 0.0376(9) -0.0003(7) 0.0043(8) -0.0090(8) C25 0.0267(10) 0.0314(9) 0.0291(9) -0.0023(7) -0.0009(7) 0.0001(7) F2 0.0758(13) 0.1254(17) 0.1121(16) -0.0445(13) -0.0116(11) -0.0096(12) C57 0.0250(10) 0.0327(9) 0.0305(9) 0.0021(7) -0.0007(7) -0.0007(7) C01F 0.0335(11) 0.0319(9) 0.0314(10) 0.0011(7) -0.0009(8) -0.0042(8) C22 0.0390(11) 0.0306(9) 0.0298(10) 0.0007(7) 0.0058(8) 0.0024(8) C21 0.0357(11) 0.0359(10) 0.0266(9) 0.0009(7) 0.0024(8) 0.0012(8) C24 0.0372(11) 0.0310(9) 0.0308(10) 0.0004(7) -0.0039(8) -0.0010(8) C32 0.0265(10) 0.0354(10) 0.0320(10) -0.0022(7) 0.0029(7) -0.0031(7) C60 0.0279(10) 0.0346(10) 0.0322(10) 0.0021(7) 0.0034(8) 0.0020(7) C33 0.0333(11) 0.0343(10) 0.0297(10) -0.0024(7) 0.0009(8) 0.0021(8) C36 0.0392(11) 0.0277(9) 0.0299(9) -0.0011(7) -0.0018(8) 0.0024(8) C54 0.0450(13) 0.0364(10) 0.0353(11) -0.0018(8) 0.0048(9) -0.0029(9) C1 0.0295(10) 0.0434(11) 0.0312(10) 0.0035(8) 0.0013(8) -0.0044(8) C53 0.0404(12) 0.0431(11) 0.0289(10) -0.0024(8) 0.0027(8) -0.0041(9) C46 0.0511(14) 0.0440(11) 0.0262(10) 0.0044(8) -0.0030(9) 0.0147(10) C26 0.0319(11) 0.0357(10) 0.0343(10) -0.0075(7) 0.0020(8) -0.0032(8) C58 0.0294(10) 0.0349(10) 0.0362(10) 0.0054(8) 0.0007(8) -0.0018(8) C20 0.0319(11) 0.0369(10) 0.0326(10) -0.0006(7) -0.0018(8) 0.0011(8) C56 0.0372(11) 0.0367(10) 0.0304(10) -0.0019(7) -0.0012(8) 0.0006(8) C19 0.0439(12) 0.0379(10) 0.0242(9) -0.0056(7) -0.0010(8) -0.0127(9) C59 0.0358(11) 0.0363(10) 0.0337(10) 0.0050(8) 0.0054(8) 0.0006(8) C14 0.0533(14) 0.0391(11) 0.0247(9) -0.0052(7) -0.0027(9) -0.0114(9) C51 0.0450(13) 0.0446(11) 0.0246(9) 0.0063(8) -0.0018(8) 0.0116(9) C31 0.0386(12) 0.0381(10) 0.0323(10) -0.0071(8) 0.0069(8) -0.0045(8) C41 0.0460(13) 0.0320(10) 0.0341(10) 0.0038(8) 0.0018(9) -0.0019(9) C42 0.0422(13) 0.0427(11) 0.0392(11) 0.0051(8) 0.0075(9) -0.0090(9) C9 0.0443(13) 0.0352(10) 0.0358(11) -0.0038(8) 0.0018(9) 0.0042(9) C10 0.0412(12) 0.0428(11) 0.0430(12) -0.0061(9) 0.0101(9) 0.0079(9) C52 0.0347(11) 0.0442(11) 0.0335(10) 0.0011(8) -0.0021(8) -0.0043(9) C61 0.0406(12) 0.0331(10) 0.0485(12) 0.0045(8) 0.0006(9) -0.0030(9) C18 0.0438(13) 0.0548(13) 0.0319(11) -0.0100(9) -0.0003(9) -0.0138(10) C23 0.0470(13) 0.0361(10) 0.0311(10) 0.0006(8) 0.0017(9) -0.0102(9) C34 0.0470(13) 0.0369(10) 0.0345(10) -0.0068(8) 0.0041(9) 0.0029(9) C50 0.0435(13) 0.0634(14) 0.0334(11) 0.0101(10) -0.0001(9) 0.0133(11) C27 0.0530(9) 0.0337(9) 0.0421(11) -0.0095(8) 0.0018(8) -0.0004(7) C15 0.0782(18) 0.0385(11) 0.0319(11) -0.0035(8) -0.0031(11) -0.0191(11) C55 0.0532(14) 0.0439(12) 0.0339(11) -0.0015(8) 0.0049(10) 0.0112(10) C47 0.0738(18) 0.0436(12) 0.0330(11) 0.0024(9) -0.0038(11) 0.0186(11) C35 0.0615(15) 0.0329(10) 0.0399(12) -0.0060(8) 0.0036(10) 0.0028(10) C2 0.0483(14) 0.0468(12) 0.0373(11) 0.0086(9) 0.0054(10) -0.0110(10) C45 0.0696(17) 0.0331(11) 0.0479(13) 0.0122(9) -0.0137(11) -0.0018(10) C13 0.0769(18) 0.0314(11) 0.0448(13) -0.0145(9) -0.0141(12) 0.0049(11) C16 0.0786(19) 0.0597(15) 0.0340(12) -0.0078(10) 0.0043(11) -0.0396(14) C49 0.0507(15) 0.0803(19) 0.0377(12) 0.0114(11) 0.0028(11) 0.0282(13) C17 0.0537(15) 0.0661(16) 0.0399(12) -0.0119(11) 0.0017(10) -0.0277(12) C3 0.0621(16) 0.0397(12) 0.0447(13) 0.0072(9) 0.0030(11) -0.0138(11) C12 0.0749(19) 0.0484(13) 0.0532(15) -0.0255(11) -0.0039(13) 0.0196(13) C48 0.0752(19) 0.0659(16) 0.0356(12) 0.0041(11) 0.0029(12) 0.0379(15) C44 0.0693(18) 0.0425(12) 0.0600(15) 0.0263(11) -0.0017(13) -0.0115(12) C62 0.0526(16) 0.0383(12) 0.0793(18) -0.0033(11) -0.0081(13) 0.0028(10) C11 0.0417(16) 0.0331(13) 0.0419(15) -0.0071(10) 0.0071(11) 0.0095(11) C28 0.0499(10) 0.0266(11) 0.0583(13) -0.0078(9) -0.0002(8) 0.0041(8) C37 0.1143(16) 0.0352(11) 0.0623(15) -0.0101(10) 0.0172(12) 0.0005(10) C5 0.137(2) 0.0373(12) 0.0824(18) 0.0123(12) 0.0161(16) -0.0192(12) C29 0.0621(13) 0.0485(15) 0.0649(14) -0.0104(10) 0.0070(10) -0.0142(11) C63 0.070(3) 0.0357(17) 0.047(2) -0.0001(13) 0.0036(17) 0.0051(16) C39 0.1106(17) 0.047(2) 0.095(2) 0.0148(16) 0.0103(16) 0.0019(13) C38 0.1070(17) 0.0265(13) 0.080(2) -0.0016(12) 0.0180(13) 0.0105(11) C30 0.0731(15) 0.076(2) 0.095(2) -0.0126(17) 0.0095(15) -0.0326(16) C43 0.050(3) 0.030(2) 0.039(3) 0.0059(19) 0.011(2) -0.007(2) C64 0.098(4) 0.057(3) 0.101(4) 0.003(3) -0.001(3) 0.035(3) C6 0.152(3) 0.0488(18) 0.086(2) 0.0205(17) 0.0255(17) -0.0061(16) C40 0.1136(19) 0.066(3) 0.136(5) 0.032(3) 0.004(2) -0.0072(18) C8 0.206(3) 0.152(6) 0.134(5) -0.054(5) -0.013(4) 0.083(4) C7 0.172(3) 0.089(4) 0.102(3) -0.019(3) 0.008(2) 0.037(2) C43A 0.040(2) 0.047(2) 0.037(2) 0.0063(15) 0.0113(16) -0.0052(16) C63A 0.060(5) 0.048(4) 0.067(5) 0.002(4) 0.002(4) 0.006(4) C64A 0.073(7) 0.069(6) 0.106(8) 0.008(6) 0.004(6) 0.026(5) C28A 0.0666(19) 0.069(3) 0.072(9) -0.036(5) 0.018(4) -0.023(2) C29A 0.131(4) 0.119(4) 0.210(12) -0.120(6) 0.120(6) -0.082(4) C30A 0.091(5) 0.092(5) 0.129(14) -0.062(7) 0.059(7) -0.048(5) C38A 0.1213(19) 0.049(3) 0.108(9) 0.009(4) 0.000(2) -0.0090(16) C39A 0.102(3) 0.049(3) 0.071(6) 0.001(3) 0.030(3) -0.0057(19) C40A 0.105(3) 0.059(4) 0.097(8) -0.002(5) 0.023(4) -0.007(2) C11A 0.066(9) 0.050(7) 0.035(6) -0.001(5) 0.016(6) 0.013(6) C6A 0.156(3) 0.064(5) 0.086(3) 0.002(2) 0.0081(19) 0.004(3) C7A 0.137(3) 0.045(4) 0.088(3) -0.005(3) 0.004(3) -0.015(3) C8A 0.134(4) 0.043(3) 0.103(4) 0.001(4) 0.007(4) -0.017(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 K2 O14 111.87(4) . . ? O12 K2 O13 59.05(4) . . ? O12 K2 O10 99.62(4) . . ? O12 K2 F8 69.45(4) . . ? O12 K2 O15 169.92(5) . . ? O12 K2 F7 109.96(4) . . ? F9 K2 O12 86.07(4) . . ? F9 K2 O14 76.93(4) . . ? F9 K2 O13 73.44(4) . . ? F9 K2 O10 133.21(4) . . ? F9 K2 F8 45.06(4) . . ? F9 K2 O15 87.04(5) . . ? F9 K2 F7 42.65(4) . . ? O14 K2 O13 52.84(4) . . ? O14 K2 O10 138.59(4) . . ? O14 K2 F8 121.96(4) . . ? O14 K2 F7 100.01(5) . . ? O13 K2 O10 147.62(4) . . ? O13 K2 F8 99.95(5) . . ? O13 K2 F7 115.97(4) . . ? O11 K2 O12 83.63(4) . . ? O11 K2 F9 153.56(5) . . ? O11 K2 O14 84.44(4) . . ? O11 K2 O13 80.38(4) . . ? O11 K2 O10 72.71(4) . . ? O11 K2 F8 147.41(4) . . ? O11 K2 O15 99.48(5) . . ? O11 K2 F7 162.36(5) . . ? O10 K2 F8 93.46(4) . . ? O10 K2 F7 93.41(4) . . ? F8 K2 F7 41.11(4) . . ? O15 K2 O14 59.25(5) . . ? O15 K2 O13 111.81(5) . . ? O15 K2 O10 90.46(4) . . ? O15 K2 F8 110.24(5) . . ? O15 K2 F7 69.13(5) . . ? O4 K1 O5 102.00(4) . . ? O4 K1 O3 59.81(4) . . ? O4 K1 O2 113.26(4) . . ? O4 K1 F4 70.05(5) . . ? O4 K1 F5 110.63(4) . . ? F6 K1 O4 88.17(4) . . ? F6 K1 O5 133.69(4) . . ? F6 K1 O3 75.24(4) . . ? F6 K1 O2 75.56(4) . . ? F6 K1 F4 45.11(4) . . ? F6 K1 F5 42.65(4) . . ? O5 K1 F4 96.01(5) . . ? O5 K1 F5 92.53(4) . . ? O3 K1 O5 148.06(4) . . ? O3 K1 O2 53.45(4) . . ? O3 K1 F4 100.83(5) . . ? O3 K1 F5 117.84(4) . . ? O2 K1 O5 135.45(4) . . ? O2 K1 F4 120.63(4) . . ? O2 K1 F5 99.28(5) . . ? O16 K1 O4 81.75(4) . . ? O16 K1 F6 154.69(5) . . ? O16 K1 O5 71.39(4) . . ? O16 K1 O3 79.64(5) . . ? O16 K1 O2 87.16(4) . . ? O16 K1 F4 146.16(5) . . ? O16 K1 F5 161.83(5) . . ? F4 K1 F5 40.91(5) . . ? F6 P1 F4 88.73(8) . . ? F3 P1 F6 177.75(9) . . ? F3 P1 F4 89.35(9) . . ? F1 P1 F6 90.48(9) . . ? F1 P1 F3 91.48(9) . . ? F1 P1 F4 178.25(12) . . ? F1 P1 F5 93.32(13) . . ? F1 P1 F2 90.56(13) . . ? F5 P1 F6 89.75(9) . . ? F5 P1 F3 89.03(10) . . ? F5 P1 F4 88.24(13) . . ? F5 P1 F2 176.03(14) . . ? F2 P1 F6 89.34(10) . . ? F2 P1 F3 91.75(11) . . ? F2 P1 F4 87.87(13) . . ? F9 P2 F8 88.64(8) . . ? F11 P2 F9 90.51(8) . . ? F11 P2 F8 179.14(10) . . ? F11 P2 F10 91.51(9) . . ? F11 P2 F7 91.96(11) . . ? F11 P2 F12 90.91(11) . . ? F10 P2 F9 177.63(9) . . ? F10 P2 F8 89.34(9) . . ? F7 P2 F9 89.67(9) . . ? F7 P2 F8 88.14(11) . . ? F7 P2 F10 89.03(10) . . ? F7 P2 F12 177.11(12) . . ? F12 P2 F9 89.87(10) . . ? F12 P2 F8 88.99(11) . . ? F12 P2 F10 91.33(11) . . ? C22 O12 K2 140.63(11) . . ? C22 O12 C21 112.51(14) . . ? C21 O12 K2 103.92(10) . . ? C54 O4 K1 143.17(11) . . ? C54 O4 C53 111.59(15) . . ? C53 O4 K1 101.53(10) . . ? P1 F6 K1 110.82(6) . . ? P2 F9 K2 110.29(7) . . ? C32 O5 K1 127.96(12) . . ? C14 O14 K2 124.84(11) . . ? C14 O14 C13 117.59(17) . . ? C13 O14 K2 117.37(13) . . ? C20 O13 K2 117.17(10) . . ? C19 O13 K2 125.07(12) . . ? C19 O13 C20 117.02(16) . . ? C51 O3 K1 125.65(12) . . ? C51 O3 C52 116.88(16) . . ? C52 O3 K1 117.13(11) . . ? C33 O11 K2 134.96(12) . . ? C60 O10 K2 132.28(13) . . ? C46 O2 K1 123.90(12) . . ? C46 O2 C45 117.47(17) . . ? C45 O2 K1 118.21(13) . . ? C1 O16 K1 131.78(13) . . ? C57 N8 C60 118.26(16) . . ? P2 F8 K2 99.79(8) . . ? C25 N2 C32 118.39(16) . . ? C25 N3 C24 124.44(15) . . ? C01F N15 C1 118.16(16) . . ? C36 N12 C33 118.11(16) . . ? C57 N6 C56 124.26(16) . . ? C12 O15 K2 104.08(13) . . ? C11 O15 K2 141.12(13) . . ? C11 O15 C12 111.99(18) . . ? C11A O15 K2 105.6(5) . . ? C11A O15 C12 134.5(5) . . ? C43 O1 C44 107.9(2) . . ? C43A O1 C44 122.4(2) . . ? C01F N14 C9 124.69(16) . . ? C57 N7 C58 121.32(17) . . ? C36 N10 C41 124.79(16) . . ? C25 N1 C26 121.27(17) . . ? P2 F7 K2 91.95(8) . . ? C24 N0AA C23 119.59(16) . . ? C41 N9 C42 120.73(17) . . ? C9 N13 C10 119.94(17) . . ? C56 N5 C55 119.59(17) . . ? P1 F4 K1 99.15(8) . . ? C36 N11 C35 120.89(17) . . ? P1 F5 K1 91.87(9) . . ? C01F N4 C3 120.73(18) . . ? N2 C25 N3 118.51(16) . . ? N2 C25 N1 123.51(17) . . ? N1 C25 N3 117.98(16) . . ? N8 C57 N6 118.53(16) . . ? N8 C57 N7 123.67(17) . . ? N7 C57 N6 117.79(17) . . ? N15 C01F N14 118.56(16) . . ? N15 C01F N4 123.45(18) . . ? N4 C01F N14 117.98(17) . . ? O12 C22 C23 108.75(16) . . ? O12 C21 C20 111.83(15) . . ? O9 C24 N3 121.37(17) . . ? O9 C24 N0AA 123.78(18) . . ? N0AA C24 N3 114.85(16) . . ? O5 C32 N2 120.01(17) . . ? O5 C32 C31 121.48(17) . . ? N2 C32 C31 118.51(17) . . ? O10 C60 N8 119.79(17) . . ? O10 C60 C59 121.81(17) . . ? N8 C60 C59 118.39(17) . . ? O11 C33 N12 118.99(16) . . ? O11 C33 C34 122.00(17) . . ? N12 C33 C34 119.01(17) . . ? N12 C36 N10 118.61(16) . . ? N12 C36 N11 123.53(17) . . ? N11 C36 N10 117.86(17) . . ? O4 C54 C55 108.84(18) . . ? O16 C1 N15 119.01(17) . . ? O16 C1 C2 121.87(18) . . ? N15 C1 C2 119.12(18) . . ? O4 C53 C52 111.90(16) . . ? O2 C46 C51 115.69(18) . . ? O2 C46 C47 124.6(2) . . ? C47 C46 C51 119.7(2) . . ? N1 C26 C27 117.24(18) . . ? C31 C26 N1 117.70(17) . . ? C31 C26 C27 125.06(18) . . ? N7 C58 C61 116.16(18) . . ? C59 C58 N7 117.71(17) . . ? C59 C58 C61 126.06(18) . . ? O13 C20 C21 106.71(16) . . ? O7 C56 N6 121.58(18) . . ? O7 C56 N5 123.63(18) . . ? N5 C56 N6 114.79(17) . . ? O13 C19 C14 115.43(19) . . ? O13 C19 C18 124.84(19) . . ? C18 C19 C14 119.73(19) . . ? C58 C59 C60 120.47(18) . . ? O14 C14 C19 115.37(17) . . ? O14 C14 C15 124.8(2) . . ? C15 C14 C19 119.8(2) . . ? O3 C51 C46 115.47(19) . . ? O3 C51 C50 124.8(2) . . ? C50 C51 C46 119.7(2) . . ? C26 C31 C32 120.45(18) . . ? O6 C41 N10 121.52(18) . . ? O6 C41 N9 124.22(18) . . ? N9 C41 N10 114.26(17) . . ? N9 C42 C43 111.7(2) . . ? N9 C42 C43A 111.7(2) . . ? O8 C9 N14 121.46(19) . . ? O8 C9 N13 124.24(19) . . ? N13 C9 N14 114.29(17) . . ? N13 C10 C11 113.87(19) . . ? C11A C10 N13 112.7(5) . . ? O3 C52 C53 106.88(16) . . ? C58 C61 C62 112.20(18) . . ? C19 C18 C17 119.8(2) . . ? N0AA C23 C22 114.24(16) . . ? C35 C34 C33 120.24(19) . . ? C51 C50 C49 120.1(2) . . ? C26 C27 C28 116.6(2) . . ? C26 C27 C28A 103.6(6) . . ? C14 C15 C16 119.9(2) . . ? N5 C55 C54 114.13(17) . . ? C46 C47 C48 120.1(2) . . ? N11 C35 C37 115.5(2) . . ? C34 C35 N11 118.20(18) . . ? C34 C35 C37 126.3(2) . . ? C3 C2 C1 120.21(19) . . ? O2 C45 C44 107.25(18) . . ? O14 C13 C12 106.74(18) . . ? C17 C16 C15 120.3(2) . . ? C48 C49 C50 120.0(2) . . ? C16 C17 C18 120.5(2) . . ? N4 C3 C5 115.8(2) . . ? C2 C3 N4 118.23(19) . . ? C2 C3 C5 125.9(2) . . ? O15 C12 C13 112.3(2) . . ? C49 C48 C47 120.4(2) . . ? O1 C44 C45 110.4(2) . . ? C63 C62 C61 114.0(2) . . ? C63A C62 C61 127.3(4) . . ? O15 C11 C10 109.03(19) . . ? C29 C28 C27 116.1(3) . . ? C35 C37 C38A 102.1(5) . . ? C38 C37 C35 119.7(3) . . ? C3 C5 C6 116.3(3) . . ? C6A C5 C3 111.5(6) . . ? C28 C29 C30 112.5(3) . . ? C62 C63 C64 112.3(3) . . ? C38 C39 C40 113.1(4) . . ? C37 C38 C39 107.8(4) . . ? O1 C43 C42 109.4(3) . . ? C7 C6 C5 111.1(5) . . ? C6 C7 C8 122.0(6) . . ? O1 C43A C42 113.1(3) . . ? C62 C63A C64A 117.7(7) . . ? C29A C28A C27 119.5(11) . . ? C28A C29A C30A 124.9(13) . . ? C39A C38A C37 133.8(10) . . ? C40A C39A C38A 129.4(10) . . ? O15 C11A C10 118.3(8) . . ? C7A C6A C5 104.5(8) . . ? C6A C7A C8A 108.7(9) . . ? 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 K2 O12 2.7979(13) . ? K2 F9 2.7865(15) . ? K2 O14 2.8879(15) . ? K2 O13 2.8992(15) . ? K2 O11 2.6859(14) . ? K2 O10 2.9902(15) . ? K2 F8 3.0274(18) . ? K2 O15 2.8069(15) . ? K2 F7 3.251(2) . ? K1 O4 2.8154(14) . ? K1 F6 2.7633(14) . ? K1 O5 2.9833(15) . ? K1 O3 2.8537(15) . ? K1 O2 2.8927(14) . ? K1 O16 2.6601(14) . ? K1 F4 3.036(2) . ? K1 F5 3.249(2) . ? P1 F6 1.5993(13) . ? P1 F3 1.5862(15) . ? P1 F1 1.5506(16) . ? P1 F4 1.6025(16) . ? P1 F5 1.5650(18) . ? P1 F2 1.5769(19) . ? P2 F9 1.5973(14) . ? P2 F11 1.5641(15) . ? P2 F8 1.6071(15) . ? P2 F10 1.5876(15) . ? P2 F7 1.5763(17) . ? P2 F12 1.5806(17) . ? O12 C22 1.419(2) . ? O12 C21 1.432(2) . ? O4 C54 1.427(2) . ? O4 C53 1.431(2) . ? O5 C32 1.247(2) . ? O14 C14 1.375(3) . ? O14 C13 1.430(3) . ? O13 C20 1.433(2) . ? O13 C19 1.367(2) . ? O3 C51 1.372(2) . ? O3 C52 1.436(2) . ? O11 C33 1.247(2) . ? O10 C60 1.246(2) . ? O2 C46 1.374(3) . ? O2 C45 1.430(3) . ? O16 C1 1.246(2) . ? O9 C24 1.237(2) . ? O7 C56 1.238(2) . ? N8 C57 1.314(2) . ? N8 C60 1.384(2) . ? O6 C41 1.237(2) . ? N2 C25 1.314(2) . ? N2 C32 1.380(2) . ? N3 C25 1.371(2) . ? N3 C24 1.406(2) . ? O8 C9 1.231(2) . ? N15 C01F 1.316(2) . ? N15 C1 1.379(2) . ? N12 C33 1.382(2) . ? N12 C36 1.315(2) . ? N6 C57 1.374(2) . ? N6 C56 1.403(2) . ? O15 C12 1.427(3) . ? O15 C11 1.402(3) . ? O15 C11A 1.310(11) . ? O1 C44 1.425(3) . ? O1 C43 1.351(5) . ? O1 C43A 1.351(4) . ? N14 C01F 1.363(2) . ? N14 C9 1.403(2) . ? N7 C57 1.344(2) . ? N7 C58 1.373(2) . ? N10 C36 1.364(2) . ? N10 C41 1.402(2) . ? N1 C25 1.346(2) . ? N1 C26 1.372(2) . ? N0AA C24 1.330(2) . ? N0AA C23 1.462(2) . ? N9 C41 1.324(3) . ? N9 C42 1.460(2) . ? N13 C9 1.326(3) . ? N13 C10 1.458(2) . ? N5 C56 1.330(3) . ? N5 C55 1.464(2) . ? N11 C36 1.358(2) . ? N11 C35 1.371(3) . ? N4 C01F 1.353(2) . ? N4 C3 1.376(3) . ? C22 C23 1.509(3) . ? C21 C20 1.492(3) . ? C32 C31 1.442(3) . ? C60 C59 1.445(3) . ? C33 C34 1.442(3) . ? C54 C55 1.497(3) . ? C1 C2 1.438(3) . ? C53 C52 1.493(3) . ? C46 C51 1.399(3) . ? C46 C47 1.384(3) . ? C26 C31 1.346(3) . ? C26 C27 1.502(3) . ? C58 C59 1.345(3) . ? C58 C61 1.494(3) . ? C19 C14 1.398(3) . ? C19 C18 1.387(3) . ? C14 C15 1.387(3) . ? C51 C50 1.386(3) . ? C42 C43 1.559(5) . ? C42 C43A 1.498(4) . ? C10 C11 1.508(3) . ? C10 C11A 1.450(10) . ? C61 C62 1.538(3) . ? C18 C17 1.390(3) . ? C34 C35 1.343(3) . ? C50 C49 1.390(3) . ? C27 C28 1.522(4) . ? C27 C28A 1.591(12) . ? C15 C16 1.389(4) . ? C47 C48 1.388(4) . ? C35 C37 1.510(3) . ? C2 C3 1.339(3) . ? C45 C44 1.488(4) . ? C13 C12 1.484(4) . ? C16 C17 1.369(4) . ? C49 C48 1.374(4) . ? C3 C5 1.497(3) . ? C62 C63 1.472(4) . ? C62 C63A 1.276(8) . ? C28 C29 1.494(5) . ? C37 C38 1.467(5) . ? C37 C38A 1.558(7) . ? C5 C6 1.523(6) . ? C5 C6A 1.485(7) . ? C29 C30 1.516(5) . ? C63 C64 1.543(5) . ? C39 C38 1.482(7) . ? C39 C40 1.546(7) . ? C6 C7 1.446(8) . ? C8 C7 1.554(8) . ? C63A C64A 1.545(10) . ? C28A C29A 1.425(14) . ? C29A C30A 1.452(14) . ? C38A C39A 1.531(7) . ? C39A C40A 1.515(13) . ? C6A C7A 1.482(7) . ? C7A C8A 1.498(8) . ?