#------------------------------------------------------------------------------ #$Date: 2019-04-28 01:11:52 +0300 (Sun, 28 Apr 2019) $ #$Revision: 214820 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/33/7123342.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_7123342 loop_ _publ_author_name 'Lu, Xing' 'Bao, Lipiao' 'Wang, Bingzhe' 'Yu, Pengyuan' 'Huang, Chenli' 'Pan, Changwang' 'Fang, Hongyun' 'Akasaka, Takeshi' 'Guldi, Dirk M.' _publ_section_title ; Intermolecular packing and charge transfer in metallofullerene/porphyrin cocrystals ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC02095K _journal_year 2019 _chemical_formula_moiety 'Y C82, C36 H44 N4 Ni, 2(C6 H6)' _chemical_formula_sum 'C130 H56 N4 Ni Y' _chemical_formula_weight 1821.40 _chemical_name_common 'Y@C2v(9)-C82 Ni(OEP) 2(C6H6)' _chemical_name_systematic 'Y@C2v(9)-C82 Ni(OEP) 2(C6H6)' _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_Hall '-C 2y' _space_group_name_H-M_alt 'C 1 2/m 1' _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 1 2/m 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2018-12-31 deposited with the CCDC. 2019-04-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.0350(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 25.3135(5) _cell_length_b 15.1618(4) _cell_length_c 19.8648(5) _cell_measurement_reflns_used 9259 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.476 _cell_measurement_theta_min 2.323 _cell_volume 7594.7(3) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.947 _diffrn_measured_fraction_theta_max 0.939 _diffrn_measurement_device_type 'CCD MX-300' _diffrn_measurement_method 'phi scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.6525 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_unetI/netI 0.0313 _diffrn_reflns_Laue_measured_fraction_full 0.947 _diffrn_reflns_Laue_measured_fraction_max 0.939 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 68528 _diffrn_reflns_point_group_measured_fraction_full 0.947 _diffrn_reflns_point_group_measured_fraction_max 0.939 _diffrn_reflns_theta_full 23.048 _diffrn_reflns_theta_max 25.783 _diffrn_reflns_theta_min 0.945 _diffrn_source 'SSRF, Beamline B17B1' _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6707 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.593 _exptl_crystal_description block _exptl_crystal_F_000 3724 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _refine_diff_density_max 1.295 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1022 _refine_ls_number_reflns 9190 _refine_ls_number_restraints 1377 _refine_ls_restrained_S_all 1.192 _refine_ls_R_factor_all 0.0761 _refine_ls_R_factor_gt 0.0691 _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^)+(0.1278P)^2^+15.6868P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1955 _refine_ls_wR_factor_ref 0.2022 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8046 _reflns_number_total 9190 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc02095k2.cif _cod_data_source_block lb230 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas ; _cod_database_code 7123342 _shelx_shelxl_version_number 2016/6 _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_min 0.782 _shelx_estimated_absorpt_t_max 0.847 _exptl_absorpt_special_details SADABS _shelx_res_file ; TITL lb230.res in C2/m lb230.res created by SHELXL-2016/6 at 14:39:47 on 01-Nov-2018 CELL 0.65250 25.3135 15.1618 19.8648 90.000 95.035 90.000 ZERR 4.000 0.0005 0.0004 0.0005 0.000 0.001 0.000 LATT 7 SYMM -X, Y, -Z SFAC C H N NI Y DISP $C 0.00267 0.00139 9.59013!source kissel DISP $H -0.00002 0.00000 0.66485!source kissel DISP $N 0.00529 0.00282 15.94814!source kissel DISP $Ni 0.34362 0.96224 3601.26400!source kissel DISP $Y -1.16938 3.09218 11411.95543!source kissel UNIT 520 224 16 4 4 TEMP -173 size 0.30 0.30 0.20 L.S. 10 BOND $H LIST 6 FMAP 2 PLAN 10 ACTA OMIT 8 0 2 OMIT 10 4 2 OMIT 12 4 3 OMIT 10 2 6 OMIT 8 0 5 SADI 0.02 C1 C2 C2 C3 C3 C4 C4 C5 C5 C1 SADI 0.04 C1 C3 C1 C4 C2 C4 C2 C5 C3 C5 SADI 0.02 C7 C8 C8 C25 C25 C24 C24 C23 C23 C7 SADI 0.04 C7 C25 C7 C24 C8 C24 C8 C23 C25 C23 SADI 0.02 C10 C11 C11 C29 C29 C28 C28 C27 C27 C10 SADI 0.04 C10 C29 C10 C28 C11 C28 C11 C27 C29 C27 SADI 0.02 C14 C15 C15 C16 C16 C35 C35 C34 C34 C14 SADI 0.04 C14 C16 C14 C35 C15 C35 C15 C34 C16 C34 SADI 0.02 C19 C20 C20 C21 C21 C41 C41 C40 C40 C19 SADI 0.04 C19 C21 C19 C41 C20 C41 C20 C40 C21 C40 SADI 0.02 C30 C31 C31 C32 C32 C53 C53 C52 C52 C30 SADI 0.04 C30 C32 C30 C53 C31 C53 C31 C52 C32 C52 SADI 0.02 C36 C37 C37 C59 C59 C58 C58 C57 C57 C36 SADI 0.04 C36 C59 C36 C58 C37 C58 C37 C57 C59 C57 SADI 0.02 C43 C44 C44 C45 C45 C66 C66 C65 C65 C43 SADI 0.04 C43 C45 C43 C66 C44 C66 C44 C65 C45 C65 SADI 0.02 C47 C48 C48 C49 C49 C69 C69 C68 C68 C47 SADI 0.04 C47 C49 C47 C69 C48 C69 C48 C68 C49 C68 SADI 0.02 C54 C55 C55 C74 C74 C73 C73 C72 C72 C54 SADI 0.04 C54 C74 C54 C73 C55 C73 C55 C72 C74 C72 SADI 0.02 C60 C61 C61 C62 C62 C63 C63 C77 C77 C60 SADI 0.04 C60 C62 C60 C63 C61 C63 C61 C77 C62 C77 SADI 0.02 C78 C79 C79 C80 C80 C81 C81 C82 C82 C78 SADI 0.04 C78 C80 C78 C81 C79 C81 C79 C82 C80 C82 SADI 0.03 C33 C56 C56 C57 C57 C36 C36 C35 C35 C34 C34 C33 SADI 0.06 C33 C57 C33 C35 C56 C36 C56 C34 C36 C34 C57 C35 SADI 0.03 C15 C3 C3 C4 C4 C18 C18 C17 C17 C16 C16 C15 SADI 0.06 C15 C4 C15 C17 C3 C18 C3 C16 C18 C16 C4 C17 SADI 0.03 C3 C15 C15 C14 C14 C13 C13 C12 C12 C2 C2 C3 SADI 0.06 C3 C14 C3 C12 C15 C13 C15 C2 C13 C2 C14 C12 SADI 0.03 C17 C16 C16 C15 C15 C3 C3 C4 C4 C18 C18 C17 SADI 0.04 C17 C15 C17 C4 C16 C3 C16 C18 C3 C18 C15 C4 SADI 0.03 C53 C54 C54 C72 C72 C71 C71 C51 C51 C52 C52 C53 SADI 0.06 C53 C72 C53 C51 C54 C71 C54 C52 C71 C52 C72 C51 SADI 0.04 C3 C13 C3 C17 C15 C12 C15 C18 C2 C14 C4 C16 SADI 0.03 C19 C18 C18 C17 C17 C38 C38 C39 C39 C40 C40 C19 SADI 0.06 C19 C17 C19 C39 C18 C38 C18 C40 C38 C40 C17 C39 SADI 0.03 C33 C56 C56 C55 C55 C54 C54 C53 C53 C32 C32 C33 SADI 0.06 C33 C55 C33 C53 C56 C54 C56 C32 C54 C32 C55 C53 SADI 0.02 C81 C70 C70 C69 C70 C71 C81 C80 C81 C82 SADI 0.02 C46 C45 C46 C24 C46 C47 WGHT 0.127800 15.686800 FVAR 0.29823 0.22214 0.14473 0.13309 0.02673 0.40000 0.66600 PART 2 Y1 5 0.658766 0.594319 0.233701 10.22214 0.12498 0.04609 = 0.19529 -0.03686 0.12230 0.00186 Y2 5 0.642460 0.583021 0.198831 10.14473 0.26722 0.50779 = 0.27827 0.11834 0.10082 0.32507 Y3 5 0.658725 0.614038 0.217192 10.13313 0.04198 0.01474 = 0.03836 -0.00626 0.00658 0.00903 PART 3 NI 4 0.518901 0.500000 0.418590 10.50000 0.02066 0.01342 = 0.01749 0.00000 0.00150 0.00000 N1 3 0.463705 0.500000 0.343447 10.50000 0.02456 0.01645 = 0.02072 0.00000 0.00122 0.00000 N2 3 0.519950 0.370510 0.417179 11.00000 0.02392 0.01571 = 0.02087 -0.00025 0.00249 -0.00017 N3 3 0.576490 0.500000 0.491017 10.50000 0.02253 0.01711 = 0.02008 0.00000 0.00299 0.00000 C106 1 0.728355 1.000000 0.233043 10.50000 0.06564 0.05361 = 0.04219 0.00000 0.00596 0.00000 AFIX 43 H106 2 0.765148 1.000000 0.247443 10.50000 -1.20000 AFIX 0 C105 1 0.691849 1.000000 0.281785 10.50000 0.06377 0.04953 = 0.03627 0.00000 -0.00001 0.00000 AFIX 43 H105 2 0.703748 1.000000 0.328492 10.50000 -1.20000 AFIX 0 C104 1 0.640071 1.000000 0.262120 10.50000 0.06147 0.05589 = 0.05440 0.00000 0.01708 0.00000 AFIX 43 H104 2 0.615192 1.000000 0.295251 10.50000 -1.20000 AFIX 0 C103 1 0.622008 1.000000 0.194495 10.50000 0.06445 0.12226 = 0.06608 0.00000 -0.01146 0.00000 AFIX 43 H103 2 0.585109 1.000000 0.180708 10.50000 -1.20000 AFIX 0 C102 1 0.660254 1.000000 0.145922 10.50000 0.10207 0.10322 = 0.03817 0.00000 -0.01209 0.00000 AFIX 43 H102 2 0.648707 1.000000 0.099109 10.50000 -1.20000 AFIX 0 C101 1 0.713134 1.000000 0.165776 10.50000 0.08793 0.04059 = 0.03772 0.00000 0.01491 0.00000 AFIX 43 H101 2 0.738662 1.000000 0.133460 10.50000 -1.20000 AFIX 0 C100 1 0.727136 0.364071 0.563342 11.00000 0.03466 0.05354 = 0.04061 0.01532 0.00783 0.01897 AFIX 137 H10A 2 0.752134 0.325768 0.590059 11.00000 -1.50000 H10B 2 0.745948 0.415944 0.548241 11.00000 -1.50000 H10C 2 0.711372 0.331591 0.523911 11.00000 -1.50000 AFIX 0 C99 1 0.683439 0.393532 0.606677 11.00000 0.02860 0.03132 = 0.02358 0.00374 -0.00049 0.00400 AFIX 23 H99A 2 0.664026 0.341046 0.620991 11.00000 -1.20000 H99B 2 0.699690 0.423104 0.647848 11.00000 -1.20000 AFIX 0 C98 1 0.645186 0.455283 0.569442 11.00000 0.02209 0.02698 = 0.01909 0.00074 0.00168 0.00100 C97 1 0.602440 0.428322 0.520746 11.00000 0.02076 0.02294 = 0.01870 0.00145 0.00201 0.00163 C96 1 0.590584 0.341619 0.505867 11.00000 0.02591 0.01941 = 0.02239 0.00382 0.00297 0.00434 AFIX 43 H96 2 0.610116 0.297398 0.531141 11.00000 -1.20000 AFIX 0 C95 1 0.552311 0.314769 0.456806 11.00000 0.02512 0.01708 = 0.02311 0.00143 0.00449 0.00172 C94 1 0.626758 0.133512 0.446320 11.00000 0.04345 0.03185 = 0.07045 -0.00055 0.00729 0.01510 AFIX 137 H94A 2 0.622564 0.120406 0.397836 11.00000 -1.50000 H94B 2 0.644721 0.084138 0.470548 11.00000 -1.50000 H94C 2 0.647971 0.187213 0.454063 11.00000 -1.50000 AFIX 0 C93 1 0.572340 0.147172 0.472005 11.00000 0.03553 0.01696 = 0.04809 0.00439 -0.00049 0.00203 AFIX 23 H93A 2 0.551112 0.092811 0.463621 11.00000 -1.20000 H93B 2 0.576842 0.156892 0.521458 11.00000 -1.20000 AFIX 0 C92 1 0.542379 0.223542 0.439383 11.00000 0.02956 0.01711 = 0.03168 0.00075 0.00392 0.00059 C91 1 0.501470 0.135425 0.280002 11.00000 0.05821 0.03469 = 0.05674 -0.02164 0.00124 -0.00075 AFIX 137 H91A 2 0.484814 0.084241 0.256677 11.00000 -1.50000 H91B 2 0.539887 0.126229 0.286834 11.00000 -1.50000 H91C 2 0.494042 0.188453 0.252587 11.00000 -1.50000 AFIX 0 C90 1 0.479149 0.146871 0.348378 11.00000 0.04158 0.01765 = 0.04922 -0.00490 -0.00418 -0.00351 AFIX 23 H90A 2 0.440322 0.155760 0.341110 11.00000 -1.20000 H90B 2 0.485546 0.092196 0.375099 11.00000 -1.20000 AFIX 0 C89 1 0.503433 0.223501 0.388008 11.00000 0.03027 0.01542 = 0.03313 -0.00118 0.00277 -0.00003 C88 1 0.489512 0.314924 0.375033 11.00000 0.02611 0.01638 = 0.02515 -0.00105 0.00375 -0.00227 C87 1 0.451782 0.341794 0.325390 11.00000 0.02763 0.01981 = 0.02346 -0.00310 0.00043 -0.00394 AFIX 43 H87 2 0.432151 0.297631 0.300174 11.00000 -1.20000 AFIX 0 C86 1 0.440626 0.428396 0.309886 11.00000 0.02173 0.02252 = 0.02197 -0.00066 0.00063 -0.00178 C85 1 0.404128 0.455347 0.253747 11.00000 0.02543 0.02778 = 0.02485 -0.00119 -0.00234 -0.00095 C84 1 0.375602 0.393454 0.204415 11.00000 0.03274 0.03045 = 0.03404 -0.00257 -0.00795 -0.00575 AFIX 23 H84A 2 0.346149 0.425494 0.179032 11.00000 -1.20000 H84B 2 0.359978 0.345083 0.229638 11.00000 -1.20000 AFIX 0 C83 1 0.411185 0.354019 0.154579 11.00000 0.05100 0.03906 = 0.02844 -0.00727 -0.00478 -0.00431 AFIX 137 H83A 2 0.390150 0.315677 0.122826 11.00000 -1.50000 H83B 2 0.439345 0.319419 0.179144 11.00000 -1.50000 H83C 2 0.427027 0.401510 0.129601 11.00000 -1.50000 AFIX 66 PART 0 PART -2 10.5000 PART 0 SIMU 0.03 C1z > C6z PART -3 10.500 C1Z 1 0.478758 0.139123 0.073065 10.50000 0.10520 0.13207 = 0.08067 0.01788 0.03340 -0.00664 AFIX 43 H1Z 2 0.460118 0.139452 0.112539 10.50000 -1.20000 AFIX 65 C2Z 1 0.454107 0.169226 0.012092 10.50000 0.23832 0.23592 = 0.16049 0.07712 0.06169 0.18396 AFIX 43 H2Z 2 0.418618 0.190130 0.009894 10.50000 -1.20000 AFIX 65 C3Z 1 0.481381 0.168745 -0.045664 10.50000 0.25901 0.27586 = 0.18188 0.07431 0.05634 0.16813 AFIX 43 H3Z 2 0.464532 0.189319 -0.087336 10.50000 -1.20000 AFIX 65 C4Z 1 0.533306 0.138159 -0.042448 10.50000 0.10544 0.20155 = 0.14003 -0.07630 0.04320 0.02651 AFIX 43 H4Z 2 0.551946 0.137830 -0.081923 10.50000 -1.20000 AFIX 65 C5Z 1 0.557958 0.108055 0.018524 10.50000 0.07836 0.13742 = 0.20839 -0.06972 0.00760 -0.00182 AFIX 43 H5Z 2 0.593447 0.087152 0.020721 10.50000 -1.20000 AFIX 65 C6Z 1 0.530685 0.108537 0.076281 10.50000 0.10576 0.12401 = 0.17416 -0.01439 0.01187 0.00142 AFIX 43 H6Z 2 0.547534 0.087962 0.117953 10.50000 -1.20000 PART 0 AFIX 0 SIMU 0.023 C61 > C82 SIMU 0.01 C4 C15 C16 C17 C18 EADP C3 C2 PART 0 C61 1 0.864947 0.500000 0.233568 10.50000 0.03737 0.11107 = 0.22254 0.00000 0.01243 0.00000 C52 1 0.566979 0.340637 0.176253 11.00000 0.06903 0.08108 = 0.15580 -0.02274 0.00860 -0.03982 C11 1 0.571628 0.500000 0.043331 10.50000 0.17064 0.12316 = 0.11141 0.00000 -0.09833 0.00000 PART -1 10.500 C1 1 0.649355 0.619207 0.009827 10.50000 0.23502 0.09739 = 0.03589 0.02899 -0.03384 -0.06228 C2 1 0.646179 0.531577 -0.013137 10.50000 0.31439 0.13021 = 0.02542 0.01634 0.02831 -0.02959 C3 1 0.697294 0.513795 -0.018693 10.50000 0.31439 0.13021 = 0.02542 0.01634 0.02831 -0.02959 C4 1 0.733092 0.583723 -0.002062 10.50000 0.28053 0.14506 = 0.08544 0.03553 0.11261 -0.02909 C5 1 0.700031 0.651096 0.018453 10.50000 0.26029 0.09414 = 0.05100 0.02892 0.05138 -0.03027 C6 1 0.715919 0.718955 0.072981 10.50000 0.20316 0.06330 = 0.05764 0.02380 0.05223 -0.04212 C7 1 0.683610 0.750832 0.110734 10.50000 0.21545 0.02554 = 0.09091 0.01331 -0.01219 -0.01252 C8 1 0.630756 0.718167 0.095278 10.50000 0.16242 0.05497 = 0.09576 0.02429 -0.04634 0.02177 C9 1 0.617430 0.652893 0.047477 10.50000 0.14287 0.05853 = 0.06536 0.03628 -0.05292 -0.02469 C10 1 0.573968 0.589376 0.062151 10.50000 0.10376 0.05811 = 0.12044 0.04127 -0.08598 -0.02320 C12 1 0.608093 0.475871 0.007613 10.50000 0.22101 0.11058 = 0.03723 -0.00427 -0.07187 -0.01562 C13 1 0.620605 0.383823 0.020732 10.50000 0.18726 0.11522 = 0.06701 -0.00752 -0.05962 -0.07942 C14 1 0.675644 0.358631 0.011747 10.50000 0.14536 0.09322 = 0.04944 -0.04426 0.01565 -0.03602 C15 1 0.710060 0.426209 -0.006547 10.50000 0.27466 0.10850 = 0.06368 -0.03489 0.09203 -0.01309 C16 1 0.763755 0.412755 0.015607 10.50000 0.24460 0.13075 = 0.08581 -0.04138 0.11226 0.01069 C17 1 0.801109 0.480081 0.046141 10.50000 0.25582 0.13154 = 0.11548 -0.00820 0.14402 0.01396 C18 1 0.782178 0.566699 0.033713 10.50000 0.26940 0.14349 = 0.11075 0.03890 0.13192 -0.00565 C19 1 0.805192 0.631636 0.080849 10.50000 0.19174 0.13158 = 0.11824 0.02438 0.08831 -0.06830 C20 1 0.770653 0.704922 0.094513 10.50000 0.16415 0.07969 = 0.08241 0.02381 0.02889 -0.07287 C21 1 0.785941 0.732017 0.164117 10.50000 0.10176 0.07022 = 0.10752 0.01171 -0.00051 -0.07015 C22 1 0.747566 0.760338 0.206785 10.50000 0.11397 0.02543 = 0.11291 -0.00351 0.00241 -0.03289 C23 1 0.690544 0.772452 0.181318 10.50000 0.15038 0.03413 = 0.08610 0.00750 0.04680 0.00070 C24 1 0.639689 0.757705 0.204368 10.50000 0.16375 0.04383 = 0.15183 0.00631 -0.04088 0.04352 C25 1 0.606082 0.709669 0.157054 10.50000 0.18448 0.07771 = 0.17432 0.00958 -0.01639 0.09601 C27 1 0.552595 0.594051 0.128869 10.50000 0.05159 0.08847 = 0.14462 0.04707 -0.03789 0.00972 C28 1 0.538045 0.508518 0.149420 10.50000 0.03554 0.11516 = 0.14728 -0.00450 -0.01853 0.01619 C29 1 0.548455 0.450368 0.095544 10.50000 0.08592 0.10131 = 0.10256 -0.00036 -0.04496 -0.03274 C30 1 0.561335 0.372444 0.109474 10.50000 0.09633 0.11134 = 0.11448 -0.04328 -0.01003 -0.05630 C31 1 0.598265 0.337781 0.067789 10.50000 0.12940 0.10599 = 0.09563 -0.04847 -0.01533 -0.04731 C32 1 0.626810 0.275097 0.106898 10.50000 0.09946 0.04751 = 0.06012 -0.02419 0.00246 -0.02077 C33 1 0.682074 0.259019 0.098519 10.50000 0.15316 0.04346 = 0.09697 -0.04236 -0.04595 0.03065 C34 1 0.710680 0.300611 0.049318 10.50000 0.14831 0.07359 = 0.06634 -0.04239 0.01422 0.01993 C35 1 0.762727 0.336052 0.051037 10.50000 0.13399 0.08737 = 0.05858 -0.02779 0.02503 0.05805 C36 1 0.796429 0.315155 0.108472 10.50000 0.13466 0.10978 = 0.10534 -0.03799 0.02454 0.07452 C37 1 0.833954 0.377837 0.141888 10.50000 0.11011 0.14296 = 0.15917 -0.00134 0.08279 0.05567 C38 1 0.839948 0.457491 0.102198 10.50000 0.11391 0.15272 = 0.20062 -0.03957 0.12475 0.00622 C39 1 0.855998 0.524764 0.160699 10.50000 0.09643 0.16356 = 0.19072 -0.02935 0.10658 -0.02177 C40 1 0.842671 0.612142 0.139104 10.50000 0.09264 0.15195 = 0.17078 -0.03206 0.09249 -0.07439 C41 1 0.827856 0.670614 0.191780 10.50000 0.08118 0.07849 = 0.14073 -0.00873 0.02662 -0.05702 C42 1 0.830377 0.650584 0.260753 10.50000 0.05445 0.07663 = 0.13268 -0.02796 -0.01789 -0.02953 C43 1 0.792165 0.687636 0.299726 10.50000 0.08971 0.06764 = 0.10257 -0.04203 -0.02480 -0.03185 C44 1 0.748352 0.739871 0.275212 10.50000 0.11775 0.03734 = 0.08927 -0.03016 -0.00484 -0.02342 C45 1 0.702329 0.719125 0.312444 10.50000 0.10642 0.05986 = 0.07436 -0.05147 0.01207 -0.00502 C46 1 0.647229 0.728332 0.276018 10.50000 0.19703 0.09472 = 0.14118 -0.02310 0.04674 0.05060 C47 1 0.619711 0.659669 0.312865 10.50000 0.17285 0.12183 = 0.12394 -0.04608 0.11068 -0.02153 C48 1 0.580006 0.638836 0.255288 10.50000 0.14649 0.14988 = 0.15573 -0.00376 0.05049 0.07422 C49 1 0.562420 0.549454 0.266019 10.50000 0.05557 0.12733 = 0.10156 -0.01880 0.05373 0.01424 C50 1 0.545512 0.476501 0.214270 10.50000 0.03648 0.12891 = 0.09347 -0.01052 0.02858 -0.02177 C51 1 0.560603 0.388888 0.233215 10.50000 0.03614 0.10749 = 0.09299 -0.03705 0.03355 -0.04169 C53 1 0.601522 0.270390 0.167786 10.50000 0.11099 0.03801 = 0.12838 -0.00218 0.00273 -0.05253 C54 1 0.634628 0.255936 0.223620 10.50000 0.20502 0.08391 = 0.06288 0.00718 -0.00692 -0.10714 C55 1 0.688447 0.230494 0.218265 10.50000 0.16166 0.02327 = 0.12020 0.01454 -0.03406 -0.03033 C56 1 0.717632 0.233244 0.157018 10.50000 0.15621 0.02171 = 0.11303 -0.02369 -0.06131 0.03811 C57 1 0.771180 0.262793 0.158181 10.50000 0.14191 0.05997 = 0.08798 -0.01814 -0.01232 0.07509 C58 1 0.800560 0.284513 0.223071 10.50000 0.10635 0.05906 = 0.09387 0.00123 -0.00124 0.05822 C59 1 0.840398 0.351555 0.212035 10.50000 0.05418 0.09640 = 0.14615 -0.00195 0.01607 0.04470 C60 1 0.851809 0.410646 0.259607 10.50000 0.04567 0.09406 = 0.18836 0.00938 -0.01213 0.03253 C62 1 0.848204 0.563413 0.286410 10.50000 0.04569 0.10827 = 0.15085 0.00264 -0.04298 -0.02495 C63 1 0.824576 0.512869 0.341818 10.50000 0.09426 0.11963 = 0.16878 0.00374 -0.09789 -0.01113 C64 1 0.785418 0.535639 0.374733 10.50000 0.12780 0.11679 = 0.06018 -0.03333 -0.06575 0.01796 C65 1 0.775458 0.631612 0.353737 10.50000 0.11713 0.09286 = 0.06998 -0.04057 -0.04146 -0.01548 C66 1 0.721209 0.652653 0.361865 10.50000 0.13351 0.08547 = 0.05575 -0.04659 0.02346 -0.03677 C67 1 0.680213 0.584042 0.377574 10.50000 0.20622 0.09041 = 0.06126 -0.04812 0.05990 -0.02097 C68 1 0.630784 0.578208 0.350015 10.50000 0.13468 0.20224 = 0.06770 -0.04769 0.06582 -0.01655 C69 1 0.593168 0.512262 0.322353 10.50000 0.07377 0.18973 = 0.07333 -0.04547 0.05615 -0.02549 C70 1 0.614025 0.427775 0.337895 10.50000 0.11299 0.19439 = 0.06862 -0.02664 0.06550 -0.07274 C71 1 0.595329 0.364571 0.290181 10.50000 0.10021 0.19176 = 0.06458 -0.00351 0.03226 -0.08289 C72 1 0.629973 0.294620 0.285810 10.50000 0.14484 0.09964 = 0.07375 0.00530 0.04618 -0.08048 C73 1 0.683095 0.293471 0.318985 10.50000 0.12743 0.07394 = 0.07730 0.03025 0.02366 -0.03302 C74 1 0.716861 0.254146 0.276904 10.50000 0.10735 0.03295 = 0.09241 0.02596 0.00495 0.00865 C75 1 0.774107 0.281796 0.278386 10.50000 0.08086 0.04248 = 0.07674 0.01799 -0.00801 0.02734 C76 1 0.791894 0.353736 0.332402 10.50000 0.10134 0.08122 = 0.07043 0.00996 -0.01742 0.05072 C77 1 0.826646 0.414775 0.325933 10.50000 0.07170 0.07969 = 0.13819 0.02020 -0.06825 0.01548 C78 1 0.751253 0.385676 0.372883 10.50000 0.12858 0.05892 = 0.03088 0.02274 -0.01310 -0.00014 C79 1 0.745078 0.475552 0.393590 10.50000 0.15381 0.09219 = 0.01446 0.00429 -0.00357 0.02872 C80 1 0.691226 0.496976 0.393715 10.50000 0.21416 0.08060 = 0.04076 0.01031 0.04902 -0.04236 C81 1 0.663309 0.420024 0.376663 10.50000 0.13740 0.12160 = 0.03008 -0.00794 0.04281 -0.05162 C82 1 0.700287 0.351553 0.363590 10.50000 0.13940 0.06663 = 0.05223 0.02454 0.03047 0.00022 PART 0 HKLF 4 REM lb230.res in C2/m REM R1 = 0.0691 for 8046 Fo > 4sig(Fo) and 0.0761 for all 9190 data REM 1022 parameters refined using 1377 restraints END WGHT 0.1279 15.6629 REM Highest difference peak 1.295, deepest hole -0.889, 1-sigma level 0.085 Q1 1 0.7403 0.5000 -0.0019 10.50000 0.05 1.29 Q2 1 0.6602 0.5000 -0.0184 10.50000 0.05 0.94 Q3 1 0.8269 0.5000 0.0635 10.50000 0.05 0.94 Q4 1 0.6851 0.5432 0.2819 11.00000 0.05 0.92 Q5 1 0.4868 0.2142 0.0261 11.00000 0.05 0.90 Q6 1 0.6075 0.2846 0.2204 11.00000 0.05 0.79 Q7 1 0.6293 0.5000 0.1812 10.50000 0.05 0.56 Q8 1 0.5905 0.5751 0.0384 11.00000 0.05 0.56 Q9 1 0.8619 0.5672 0.1811 11.00000 0.05 0.56 Q10 1 0.8342 0.4234 0.0887 11.00000 0.05 0.54 ; _shelx_res_checksum 54892 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, 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 Y1 Y 0.65877(18) 0.5943(2) 0.2337(3) 0.1157(19) Uani 0.2221 1 d . . P A 2 Y2 Y 0.6425(6) 0.5830(13) 0.1988(8) 0.347(12) Uani 0.1447 1 d . . P A 2 Y3 Y 0.65873(14) 0.6140(2) 0.21719(14) 0.0315(6) Uani 0.1331 1 d . . P A 2 Ni Ni 0.51890(2) 0.500000 0.41859(2) 0.01720(13) Uani 1 2 d S T P B 3 N1 N 0.46371(11) 0.500000 0.34345(13) 0.0206(5) Uani 1 2 d S T P B 3 N2 N 0.51995(7) 0.37051(12) 0.41718(8) 0.0201(4) Uani 1 1 d . . . B 3 N3 N 0.57649(10) 0.500000 0.49102(12) 0.0198(5) Uani 1 2 d S T P B 3 C106 C 0.7284(2) 1.000000 0.2330(2) 0.0537(11) Uani 1 2 d S T P C 3 H106 H 0.765148 1.000000 0.247443 0.064 Uiso 1 2 calc R U P C 3 C105 C 0.6918(2) 1.000000 0.2818(2) 0.0501(11) Uani 1 2 d S T P C 3 H105 H 0.703748 1.000000 0.328492 0.060 Uiso 1 2 calc R U P C 3 C104 C 0.6401(2) 1.000000 0.2621(3) 0.0565(12) Uani 1 2 d S T P C 3 H104 H 0.615192 1.000000 0.295251 0.068 Uiso 1 2 calc R U P C 3 C103 C 0.6220(3) 1.000000 0.1945(4) 0.085(2) Uani 1 2 d S T P C 3 H103 H 0.585109 1.000000 0.180708 0.102 Uiso 1 2 calc R U P C 3 C102 C 0.6603(3) 1.000000 0.1459(3) 0.082(2) Uani 1 2 d S T P C 3 H102 H 0.648707 1.000000 0.099109 0.099 Uiso 1 2 calc R U P C 3 C101 C 0.7131(3) 1.000000 0.1658(2) 0.0549(12) Uani 1 2 d S T P C 3 H101 H 0.738662 1.000000 0.133460 0.066 Uiso 1 2 calc R U P C 3 C100 C 0.72714(12) 0.3641(2) 0.56334(15) 0.0427(7) Uani 1 1 d . . . B 3 H10A H 0.752134 0.325768 0.590059 0.064 Uiso 1 1 calc R U . B 3 H10B H 0.745948 0.415944 0.548241 0.064 Uiso 1 1 calc R U . B 3 H10C H 0.711372 0.331591 0.523911 0.064 Uiso 1 1 calc R U . B 3 C99 C 0.68344(10) 0.39353(16) 0.60668(11) 0.0280(5) Uani 1 1 d . . . B 3 H99A H 0.664026 0.341046 0.620991 0.034 Uiso 1 1 calc R U . B 3 H99B H 0.699690 0.423104 0.647848 0.034 Uiso 1 1 calc R U . B 3 C98 C 0.64519(9) 0.45528(15) 0.56944(10) 0.0227(4) Uani 1 1 d . . . B 3 C97 C 0.60244(9) 0.42832(14) 0.52075(10) 0.0208(4) Uani 1 1 d . . . B 3 C96 C 0.59058(9) 0.34162(14) 0.50587(11) 0.0225(4) Uani 1 1 d . . . B 3 H96 H 0.610116 0.297398 0.531141 0.027 Uiso 1 1 calc R U . B 3 C95 C 0.55231(9) 0.31477(14) 0.45681(10) 0.0216(4) Uani 1 1 d . . . B 3 C94 C 0.62676(13) 0.1335(2) 0.44632(19) 0.0484(7) Uani 1 1 d . . . B 3 H94A H 0.622564 0.120406 0.397836 0.073 Uiso 1 1 calc R U . B 3 H94B H 0.644721 0.084138 0.470548 0.073 Uiso 1 1 calc R U . B 3 H94C H 0.647971 0.187213 0.454063 0.073 Uiso 1 1 calc R U . B 3 C93 C 0.57234(11) 0.14717(15) 0.47201(14) 0.0338(5) Uani 1 1 d . . . B 3 H93A H 0.551112 0.092811 0.463621 0.041 Uiso 1 1 calc R U . B 3 H93B H 0.576842 0.156892 0.521458 0.041 Uiso 1 1 calc R U . B 3 C92 C 0.54238(10) 0.22354(14) 0.43938(12) 0.0260(4) Uani 1 1 d . . . B 3 C91 C 0.50147(15) 0.1354(2) 0.28000(17) 0.0501(8) Uani 1 1 d . . . B 3 H91A H 0.484814 0.084241 0.256677 0.075 Uiso 1 1 calc R U . B 3 H91B H 0.539887 0.126229 0.286834 0.075 Uiso 1 1 calc R U . B 3 H91C H 0.494042 0.188453 0.252587 0.075 Uiso 1 1 calc R U . B 3 C90 C 0.47915(12) 0.14687(16) 0.34838(15) 0.0366(6) Uani 1 1 d . . . B 3 H90A H 0.440322 0.155760 0.341110 0.044 Uiso 1 1 calc R U . B 3 H90B H 0.485546 0.092196 0.375099 0.044 Uiso 1 1 calc R U . B 3 C89 C 0.50343(10) 0.22350(14) 0.38801(12) 0.0263(5) Uani 1 1 d . . . B 3 C88 C 0.48951(9) 0.31492(14) 0.37503(11) 0.0225(4) Uani 1 1 d . . . B 3 C87 C 0.45178(9) 0.34179(14) 0.32539(11) 0.0237(4) Uani 1 1 d . . . B 3 H87 H 0.432151 0.297631 0.300174 0.028 Uiso 1 1 calc R U . B 3 C86 C 0.44063(9) 0.42840(14) 0.30989(11) 0.0222(4) Uani 1 1 d . . . B 3 C85 C 0.40413(10) 0.45535(16) 0.25375(11) 0.0263(5) Uani 1 1 d . . . B 3 C84 C 0.37560(11) 0.39345(17) 0.20442(13) 0.0331(5) Uani 1 1 d . . . B 3 H84A H 0.346149 0.425494 0.179032 0.040 Uiso 1 1 calc R U . B 3 H84B H 0.359978 0.345083 0.229638 0.040 Uiso 1 1 calc R U . B 3 C83 C 0.41119(13) 0.3540(2) 0.15458(13) 0.0400(6) Uani 1 1 d . . . B 3 H83A H 0.390150 0.315677 0.122826 0.060 Uiso 1 1 calc R U . B 3 H83B H 0.439345 0.319419 0.179144 0.060 Uiso 1 1 calc R U . B 3 H83C H 0.427027 0.401510 0.129601 0.060 Uiso 1 1 calc R U . B 3 C1Z C 0.4788(5) 0.1391(10) 0.0731(5) 0.104(5) Uani 0.5 1 d G U P D -3 H1Z H 0.460118 0.139452 0.112539 0.125 Uiso 0.5 1 calc R U P D -3 C2Z C 0.4541(5) 0.1692(10) 0.0121(6) 0.209(9) Uani 0.5 1 d G U P D -3 H2Z H 0.418618 0.190130 0.009894 0.251 Uiso 0.5 1 calc R U P D -3 C3Z C 0.4814(7) 0.1687(11) -0.0457(5) 0.237(9) Uani 0.5 1 d G U P D -3 H3Z H 0.464532 0.189319 -0.087336 0.284 Uiso 0.5 1 calc R U P D -3 C4Z C 0.5333(6) 0.1382(12) -0.0424(6) 0.147(7) Uani 0.5 1 d G U P D -3 H4Z H 0.551946 0.137830 -0.081923 0.177 Uiso 0.5 1 calc R U P D -3 C5Z C 0.5580(4) 0.1081(8) 0.0185(8) 0.142(6) Uani 0.5 1 d G U P D -3 H5Z H 0.593447 0.087152 0.020721 0.170 Uiso 0.5 1 calc R U P D -3 C6Z C 0.5307(5) 0.1085(8) 0.0763(6) 0.135(5) Uani 0.5 1 d G U P D -3 H6Z H 0.547534 0.087962 0.117953 0.162 Uiso 0.5 1 calc R U P D -3 C61 C 0.8649(3) 0.500000 0.2336(7) 0.124(3) Uani 1 2 d DS TU P . . C52 C 0.5670(2) 0.3406(4) 0.1763(4) 0.1020(19) Uani 1 1 d D U . . . C11 C 0.5716(5) 0.500000 0.0433(6) 0.142(4) Uani 1 2 d DS TU P . . C1 C 0.6494(8) 0.6192(9) 0.0098(8) 0.125(6) Uani 0.5 1 d D U P E -1 C2 C 0.6462(7) 0.5316(8) -0.0131(5) 0.156(4) Uani 0.5 1 d D U P E -1 C3 C 0.6973(6) 0.5138(9) -0.0187(4) 0.156(4) Uani 0.5 1 d D U P E -1 C4 C 0.7331(7) 0.5837(10) -0.0021(11) 0.165(5) Uani 0.5 1 d D U P E -1 C5 C 0.7000(8) 0.6511(11) 0.0185(9) 0.133(6) Uani 0.5 1 d D U P E -1 C6 C 0.7159(10) 0.7190(12) 0.0730(7) 0.106(5) Uani 0.5 1 d . U P E -1 C7 C 0.6836(9) 0.7508(17) 0.1107(9) 0.112(5) Uani 0.5 1 d D U P E -1 C8 C 0.6308(10) 0.718(2) 0.0953(11) 0.108(6) Uani 0.5 1 d D U P E -1 C9 C 0.6174(8) 0.6529(10) 0.0475(8) 0.093(5) Uani 0.5 1 d . U P E -1 C10 C 0.5740(5) 0.5894(6) 0.0622(6) 0.100(4) Uani 0.5 1 d D U P E -1 C12 C 0.6081(6) 0.4759(8) 0.0076(5) 0.128(5) Uani 0.5 1 d D U P E -1 C13 C 0.6206(7) 0.3838(10) 0.0207(9) 0.127(6) Uani 0.5 1 d D U P E -1 C14 C 0.6756(6) 0.3586(9) 0.0117(9) 0.096(4) Uani 0.5 1 d D U P E -1 C15 C 0.7101(5) 0.4262(8) -0.0065(8) 0.144(5) Uani 0.5 1 d D U P E -1 C16 C 0.7638(6) 0.4128(9) 0.0156(8) 0.148(4) Uani 0.5 1 d D U P E -1 C17 C 0.8011(6) 0.4801(10) 0.0461(6) 0.160(4) Uani 0.5 1 d D U P E -1 C18 C 0.7822(7) 0.5667(10) 0.0337(8) 0.168(5) Uani 0.5 1 d D U P E -1 C19 C 0.8052(7) 0.6316(10) 0.0808(7) 0.143(5) Uani 0.5 1 d D U P E -1 C20 C 0.7707(7) 0.7049(9) 0.0945(7) 0.108(4) Uani 0.5 1 d D U P E -1 C21 C 0.7859(7) 0.7320(15) 0.1641(9) 0.094(5) Uani 0.5 1 d D U P E -1 C22 C 0.7476(5) 0.7603(5) 0.2068(7) 0.085(3) Uani 0.5 1 d . U P E -1 C23 C 0.6905(7) 0.7725(8) 0.1813(6) 0.088(4) Uani 0.5 1 d D U P E -1 C24 C 0.6397(8) 0.7577(12) 0.2044(10) 0.123(5) Uani 0.5 1 d D U P E -1 C25 C 0.6061(8) 0.7097(12) 0.1571(13) 0.147(8) Uani 0.5 1 d D U P E -1 C27 C 0.5526(5) 0.5941(9) 0.1289(7) 0.098(4) Uani 0.5 1 d D U P E -1 C28 C 0.5380(3) 0.5085(12) 0.1494(6) 0.101(3) Uani 0.5 1 d D U P E -1 C29 C 0.5485(5) 0.4504(9) 0.0955(7) 0.100(4) Uani 0.5 1 d D U P E -1 C30 C 0.5613(6) 0.3724(9) 0.1095(7) 0.109(5) Uani 0.5 1 d D U P E -1 C31 C 0.5983(7) 0.3378(12) 0.0678(8) 0.112(6) Uani 0.5 1 d D U P E -1 C32 C 0.6268(7) 0.2751(16) 0.1069(8) 0.069(4) Uani 0.5 1 d D U P E -1 C33 C 0.6821(6) 0.2590(15) 0.0985(8) 0.101(5) Uani 0.5 1 d D U P E -1 C34 C 0.7107(6) 0.3006(10) 0.0493(7) 0.096(5) Uani 0.5 1 d D U P E -1 C35 C 0.7627(5) 0.3361(7) 0.0510(5) 0.092(3) Uani 0.5 1 d D U P E -1 C36 C 0.7964(6) 0.3152(12) 0.1085(7) 0.116(5) Uani 0.5 1 d D U P E -1 C37 C 0.8340(11) 0.3778(16) 0.1419(10) 0.133(6) Uani 0.5 1 d D U P E -1 C38 C 0.8399(5) 0.4575(11) 0.1022(9) 0.149(5) Uani 0.5 1 d D U P E -1 C39 C 0.8560(5) 0.5248(11) 0.1607(9) 0.145(6) Uani 0.5 1 d D U P E -1 C40 C 0.8427(9) 0.6121(14) 0.1391(10) 0.134(6) Uani 0.5 1 d D U P E -1 C41 C 0.8279(8) 0.6706(11) 0.1918(9) 0.099(5) Uani 0.5 1 d D U P E -1 C42 C 0.8304(5) 0.6506(8) 0.2608(8) 0.089(3) Uani 0.5 1 d . U P E -1 C43 C 0.7922(5) 0.6876(11) 0.2997(9) 0.089(4) Uani 0.5 1 d D U P E -1 C44 C 0.7484(8) 0.7399(8) 0.2752(8) 0.082(4) Uani 0.5 1 d D U P E -1 C45 C 0.7023(6) 0.7191(11) 0.3124(9) 0.080(4) Uani 0.5 1 d D U P E -1 C46 C 0.6472(7) 0.7283(14) 0.2760(10) 0.142(6) Uani 0.5 1 d D U P E -1 C47 C 0.6197(8) 0.6597(11) 0.3129(9) 0.134(5) Uani 0.5 1 d D U P E -1 C48 C 0.5800(9) 0.6388(12) 0.2553(11) 0.149(7) Uani 0.5 1 d D U P E -1 C49 C 0.5624(4) 0.5495(9) 0.2660(6) 0.092(3) Uani 0.5 1 d D U P E -1 C50 C 0.5455(4) 0.4765(9) 0.2143(6) 0.085(4) Uani 0.5 1 d . U P E -1 C51 C 0.5606(4) 0.3889(9) 0.2332(6) 0.077(3) Uani 0.5 1 d D U P E -1 C53 C 0.6015(5) 0.2704(8) 0.1678(7) 0.093(4) Uani 0.5 1 d D U P E -1 C54 C 0.6346(6) 0.2559(10) 0.2236(6) 0.118(5) Uani 0.5 1 d D U P E -1 C55 C 0.6884(6) 0.2305(6) 0.2183(6) 0.104(4) Uani 0.5 1 d D U P E -1 C56 C 0.7176(5) 0.2332(5) 0.1570(6) 0.101(4) Uani 0.5 1 d D U P E -1 C57 C 0.7712(7) 0.2628(13) 0.1582(8) 0.098(5) Uani 0.5 1 d D U P E -1 C58 C 0.8006(5) 0.2845(6) 0.2231(6) 0.087(3) Uani 0.5 1 d D U P E -1 C59 C 0.8404(7) 0.3516(12) 0.2120(10) 0.098(5) Uani 0.5 1 d D U P E -1 C60 C 0.8518(7) 0.4106(8) 0.2596(9) 0.111(5) Uani 0.5 1 d D U P E -1 C62 C 0.8482(6) 0.5634(9) 0.2864(8) 0.105(5) Uani 0.5 1 d D U P E -1 C63 C 0.8246(5) 0.5129(11) 0.3418(7) 0.134(5) Uani 0.5 1 d D U P E -1 C64 C 0.7854(7) 0.5356(9) 0.3747(6) 0.106(4) Uani 0.5 1 d . U P E -1 C65 C 0.7755(7) 0.6316(12) 0.3537(8) 0.096(5) Uani 0.5 1 d D U P E -1 C66 C 0.7212(7) 0.6527(13) 0.3619(10) 0.091(5) Uani 0.5 1 d D U P E -1 C67 C 0.6802(10) 0.5840(13) 0.3776(10) 0.116(5) Uani 0.5 1 d . U P E -1 C68 C 0.6308(9) 0.5782(15) 0.3500(10) 0.132(6) Uani 0.5 1 d D U P E -1 C69 C 0.5932(4) 0.5123(13) 0.3224(5) 0.109(4) Uani 0.5 1 d D U P E -1 C70 C 0.6140(6) 0.4278(12) 0.3379(9) 0.122(5) Uani 0.5 1 d D U P E -1 C71 C 0.5953(6) 0.3646(12) 0.2902(6) 0.117(5) Uani 0.5 1 d D U P E -1 C72 C 0.6300(6) 0.2946(11) 0.2858(6) 0.104(5) Uani 0.5 1 d D U P E -1 C73 C 0.6831(6) 0.2935(13) 0.3190(9) 0.092(5) Uani 0.5 1 d D U P E -1 C74 C 0.7169(6) 0.2541(7) 0.2769(7) 0.078(3) Uani 0.5 1 d D U P E -1 C75 C 0.7741(7) 0.2818(9) 0.2784(8) 0.068(3) Uani 0.5 1 d . U P E -1 C76 C 0.7919(7) 0.3537(13) 0.3324(9) 0.086(4) Uani 0.5 1 d . U P E -1 C77 C 0.8266(5) 0.4148(8) 0.3259(7) 0.101(4) Uani 0.5 1 d D U P E -1 C78 C 0.7513(6) 0.3857(7) 0.3729(5) 0.074(3) Uani 0.5 1 d D U P E -1 C79 C 0.7451(5) 0.4756(6) 0.3936(3) 0.087(4) Uani 0.5 1 d D U P E -1 C80 C 0.6912(5) 0.4970(12) 0.3937(3) 0.110(3) Uani 0.5 1 d D U P E -1 C81 C 0.6633(5) 0.4200(11) 0.3767(8) 0.094(5) Uani 0.5 1 d D U P E -1 C82 C 0.7003(6) 0.3516(11) 0.3636(10) 0.085(4) Uani 0.5 1 d D U P E -1 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 Y1 0.125(3) 0.0461(16) 0.195(4) -0.037(2) 0.122(3) 0.0019(15) Y2 0.267(13) 0.51(2) 0.278(14) 0.118(14) 0.101(11) 0.325(17) Y3 0.0420(13) 0.0147(11) 0.0384(10) -0.0063(8) 0.0066(9) 0.0090(9) Ni 0.0207(2) 0.01342(19) 0.01749(19) 0.000 0.00150(13) 0.000 N1 0.0246(13) 0.0165(11) 0.0207(11) 0.000 0.0012(9) 0.000 N2 0.0239(10) 0.0157(8) 0.0209(8) -0.0002(6) 0.0025(7) -0.0002(6) N3 0.0225(13) 0.0171(11) 0.0201(11) 0.000 0.0030(9) 0.000 C106 0.066(3) 0.054(3) 0.042(2) 0.000 0.006(2) 0.000 C105 0.064(3) 0.050(3) 0.036(2) 0.000 0.0000(19) 0.000 C104 0.061(3) 0.056(3) 0.054(3) 0.000 0.017(2) 0.000 C103 0.064(4) 0.122(6) 0.066(4) 0.000 -0.011(3) 0.000 C102 0.102(6) 0.103(5) 0.038(3) 0.000 -0.012(3) 0.000 C101 0.088(4) 0.041(2) 0.038(2) 0.000 0.015(2) 0.000 C100 0.0347(15) 0.0535(17) 0.0406(14) 0.0153(13) 0.0078(11) 0.0190(12) C99 0.0286(12) 0.0313(12) 0.0236(10) 0.0037(9) -0.0005(8) 0.0040(9) C98 0.0221(11) 0.0270(11) 0.0191(9) 0.0007(8) 0.0017(7) 0.0010(8) C97 0.0208(10) 0.0229(10) 0.0187(9) 0.0015(7) 0.0020(7) 0.0016(7) C96 0.0259(11) 0.0194(9) 0.0224(9) 0.0038(7) 0.0030(8) 0.0043(8) C95 0.0251(11) 0.0171(9) 0.0231(9) 0.0014(7) 0.0045(8) 0.0017(7) C94 0.0434(17) 0.0319(14) 0.070(2) -0.0006(13) 0.0073(14) 0.0151(12) C93 0.0355(14) 0.0170(10) 0.0481(14) 0.0044(9) -0.0005(10) 0.0020(9) C92 0.0296(12) 0.0171(10) 0.0317(11) 0.0008(8) 0.0039(9) 0.0006(8) C91 0.058(2) 0.0347(15) 0.0567(18) -0.0216(13) 0.0012(14) -0.0008(13) C90 0.0416(15) 0.0176(11) 0.0492(15) -0.0049(10) -0.0042(11) -0.0035(9) C89 0.0303(12) 0.0154(9) 0.0331(11) -0.0012(8) 0.0028(9) 0.0000(8) C88 0.0261(11) 0.0164(9) 0.0251(10) -0.0011(7) 0.0038(8) -0.0023(7) C87 0.0276(11) 0.0198(9) 0.0235(9) -0.0031(8) 0.0004(8) -0.0039(8) C86 0.0217(11) 0.0225(10) 0.0220(9) -0.0007(8) 0.0006(7) -0.0018(7) C85 0.0254(12) 0.0278(12) 0.0248(10) -0.0012(8) -0.0023(8) -0.0010(8) C84 0.0327(13) 0.0305(12) 0.0340(12) -0.0026(9) -0.0079(9) -0.0058(9) C83 0.0510(17) 0.0391(14) 0.0284(12) -0.0073(10) -0.0048(11) -0.0043(12) C1Z 0.105(10) 0.132(11) 0.081(8) 0.018(8) 0.033(7) -0.007(8) C2Z 0.238(17) 0.236(17) 0.160(16) 0.077(14) 0.062(14) 0.184(14) C3Z 0.26(2) 0.28(2) 0.182(17) 0.074(16) 0.056(16) 0.168(16) C4Z 0.105(12) 0.202(17) 0.140(15) -0.076(13) 0.043(11) 0.027(12) C5Z 0.078(9) 0.137(13) 0.208(17) -0.070(12) 0.008(10) -0.002(9) C6Z 0.106(11) 0.124(11) 0.174(15) -0.014(11) 0.012(10) 0.001(9) C61 0.037(4) 0.111(7) 0.223(10) 0.000 0.012(5) 0.000 C52 0.069(4) 0.081(4) 0.156(6) -0.023(4) 0.009(3) -0.040(3) C11 0.171(10) 0.123(8) 0.111(7) 0.000 -0.098(7) 0.000 C1 0.235(14) 0.097(8) 0.036(5) 0.029(6) -0.034(9) -0.062(10) C2 0.314(11) 0.130(8) 0.025(2) 0.016(4) 0.028(5) -0.030(9) C3 0.314(11) 0.130(8) 0.025(2) 0.016(4) 0.028(5) -0.030(9) C4 0.281(12) 0.145(9) 0.085(8) 0.036(7) 0.113(9) -0.029(10) C5 0.260(14) 0.094(9) 0.051(7) 0.029(7) 0.051(10) -0.030(11) C6 0.203(12) 0.063(7) 0.058(8) 0.024(6) 0.052(8) -0.042(8) C7 0.215(14) 0.026(5) 0.091(9) 0.013(6) -0.012(10) -0.013(8) C8 0.162(14) 0.055(8) 0.096(10) 0.024(9) -0.046(9) 0.022(10) C9 0.143(11) 0.059(6) 0.065(7) 0.036(5) -0.053(7) -0.025(8) C10 0.104(8) 0.058(5) 0.120(8) 0.041(6) -0.086(6) -0.023(5) C12 0.221(12) 0.111(10) 0.037(4) -0.004(5) -0.072(6) -0.016(8) C13 0.187(12) 0.115(9) 0.067(8) -0.008(7) -0.060(9) -0.079(10) C14 0.145(10) 0.093(9) 0.049(6) -0.044(7) 0.016(8) -0.036(9) C15 0.275(11) 0.108(8) 0.064(6) -0.035(6) 0.092(8) -0.013(9) C16 0.245(10) 0.131(8) 0.086(7) -0.041(6) 0.112(7) 0.011(8) C17 0.256(10) 0.132(9) 0.115(6) -0.008(6) 0.144(6) 0.014(8) C18 0.269(11) 0.143(9) 0.111(8) 0.039(7) 0.132(7) -0.006(9) C19 0.192(12) 0.132(10) 0.118(9) 0.024(8) 0.088(9) -0.068(10) C20 0.164(12) 0.080(7) 0.082(8) 0.024(6) 0.029(8) -0.073(8) C21 0.102(9) 0.070(8) 0.108(10) 0.012(7) -0.001(7) -0.070(6) C22 0.114(8) 0.025(3) 0.113(7) -0.004(4) 0.002(6) -0.033(4) C23 0.150(10) 0.034(4) 0.086(7) 0.007(5) 0.047(7) 0.001(6) C24 0.164(12) 0.044(5) 0.152(12) 0.006(8) -0.041(10) 0.044(7) C25 0.184(14) 0.078(10) 0.174(15) 0.010(10) -0.016(12) 0.096(10) C27 0.052(6) 0.088(9) 0.145(10) 0.047(8) -0.038(6) 0.010(6) C28 0.036(4) 0.115(8) 0.147(8) -0.004(11) -0.019(4) 0.016(8) C29 0.086(8) 0.101(8) 0.103(8) 0.000(7) -0.045(6) -0.033(6) C30 0.096(8) 0.111(9) 0.114(9) -0.043(8) -0.010(7) -0.056(7) C31 0.129(10) 0.106(9) 0.096(10) -0.048(8) -0.015(7) -0.047(8) C32 0.099(8) 0.048(7) 0.060(6) -0.024(5) 0.002(6) -0.021(6) C33 0.153(10) 0.043(9) 0.097(9) -0.042(7) -0.046(8) 0.031(8) C34 0.148(10) 0.074(9) 0.066(9) -0.042(7) 0.014(8) 0.020(7) C35 0.134(9) 0.087(6) 0.059(5) -0.028(5) 0.025(5) 0.058(6) C36 0.135(11) 0.110(10) 0.105(10) -0.038(8) 0.025(8) 0.075(8) C37 0.110(12) 0.143(12) 0.159(11) -0.001(11) 0.083(9) 0.056(9) C38 0.114(9) 0.153(11) 0.201(11) -0.040(9) 0.125(9) 0.006(7) C39 0.096(7) 0.164(13) 0.191(10) -0.029(10) 0.107(8) -0.022(8) C40 0.093(9) 0.152(11) 0.171(11) -0.032(10) 0.092(8) -0.074(8) C41 0.081(10) 0.078(8) 0.141(10) -0.009(8) 0.027(8) -0.057(6) C42 0.054(6) 0.077(6) 0.133(8) -0.028(7) -0.018(6) -0.030(5) C43 0.090(8) 0.068(8) 0.103(9) -0.042(7) -0.025(7) -0.032(6) C44 0.118(11) 0.037(6) 0.089(7) -0.030(5) -0.005(10) -0.023(8) C45 0.106(9) 0.060(7) 0.074(7) -0.051(6) 0.012(7) -0.005(7) C46 0.197(13) 0.095(10) 0.141(12) -0.023(9) 0.047(11) 0.051(10) C47 0.173(12) 0.122(10) 0.124(11) -0.046(8) 0.111(9) -0.022(9) C48 0.146(15) 0.150(13) 0.156(14) -0.004(12) 0.050(12) 0.074(11) C49 0.056(6) 0.127(8) 0.102(7) -0.019(7) 0.054(5) 0.014(5) C50 0.036(4) 0.129(11) 0.093(6) -0.011(6) 0.029(4) -0.022(5) C51 0.036(5) 0.107(8) 0.093(6) -0.037(6) 0.034(4) -0.042(4) C53 0.111(8) 0.038(5) 0.128(9) -0.002(6) 0.003(7) -0.053(6) C54 0.205(11) 0.084(9) 0.063(6) 0.007(6) -0.007(7) -0.107(8) C55 0.162(10) 0.023(4) 0.120(9) 0.015(6) -0.034(9) -0.030(5) C56 0.156(10) 0.022(4) 0.113(8) -0.024(5) -0.061(8) 0.038(5) C57 0.142(12) 0.060(7) 0.088(8) -0.018(6) -0.012(8) 0.075(8) C58 0.106(8) 0.059(5) 0.094(6) 0.001(5) -0.001(6) 0.058(5) C59 0.054(7) 0.096(10) 0.146(11) -0.002(9) 0.016(8) 0.045(6) C60 0.046(6) 0.094(9) 0.188(12) 0.009(9) -0.012(8) 0.033(7) C62 0.046(7) 0.108(9) 0.151(11) 0.003(8) -0.043(7) -0.025(7) C63 0.094(7) 0.120(11) 0.169(9) 0.004(10) -0.098(7) -0.011(9) C64 0.128(10) 0.117(8) 0.060(6) -0.033(5) -0.066(6) 0.018(7) C65 0.117(11) 0.093(10) 0.070(10) -0.041(8) -0.041(8) -0.015(9) C66 0.134(11) 0.085(8) 0.056(6) -0.047(6) 0.023(8) -0.037(8) C67 0.206(13) 0.090(9) 0.061(7) -0.048(6) 0.060(8) -0.021(9) C68 0.135(13) 0.202(12) 0.068(9) -0.048(9) 0.066(8) -0.017(11) C69 0.074(6) 0.190(12) 0.073(5) -0.045(9) 0.056(5) -0.025(10) C70 0.113(10) 0.194(13) 0.069(8) -0.027(9) 0.066(7) -0.073(9) C71 0.100(10) 0.192(12) 0.065(6) -0.004(8) 0.032(6) -0.083(9) C72 0.145(10) 0.100(10) 0.074(6) 0.005(6) 0.046(7) -0.080(8) C73 0.127(11) 0.074(8) 0.077(7) 0.030(6) 0.024(8) -0.033(8) C74 0.107(9) 0.033(4) 0.092(7) 0.026(4) 0.005(8) 0.009(6) C75 0.081(8) 0.042(7) 0.077(6) 0.018(5) -0.008(7) 0.027(6) C76 0.101(8) 0.081(8) 0.070(8) 0.010(6) -0.017(6) 0.051(7) C77 0.072(8) 0.080(6) 0.138(9) 0.020(7) -0.068(6) 0.015(5) C78 0.129(10) 0.059(5) 0.031(4) 0.023(4) -0.013(5) 0.000(6) C79 0.154(9) 0.092(8) 0.014(2) 0.004(3) -0.004(4) 0.029(6) C80 0.214(10) 0.081(6) 0.041(3) 0.010(8) 0.049(5) -0.042(12) C81 0.137(11) 0.122(10) 0.030(5) -0.008(6) 0.043(6) -0.052(8) C82 0.139(11) 0.067(7) 0.052(5) 0.025(5) 0.030(8) 0.000(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0027 0.0014 '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 0.0053 0.0028 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3436 0.9622 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -1.1694 3.0922 '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 Y2 Y1 C52 49.0(8) . 6_565 C52 Y1 Y2 98.3(5) 6_565 6_565 C52 Y1 Y1 111.55(18) 6_565 6_565 C52 Y1 Y3 109.2(2) 6_565 6_565 Y3 Y2 Y1 33.8(10) . . Y3 Y2 C52 102.0(11) . 6_565 Y1 Y2 C52 115.6(11) . 6_565 C52 Y2 Y2 121.0(6) 6_565 6_565 C52 Y2 Y1 130.5(10) 6_565 6_565 C52 Y2 Y3 129.5(9) 6_565 6_565 Y2 Y3 C52 61.9(8) . 6_565 C52 Y3 Y2 96.9(4) 6_565 6_565 C52 Y3 Y1 107.5(2) 6_565 6_565 C52 Y3 Y3 106.02(18) 6_565 6_565 N1 Ni N3 177.52(10) . . N1 Ni N2 89.93(5) . . N3 Ni N2 90.02(5) . . N2 Ni N2 177.65(10) 6_565 . C86 N1 C86 104.1(3) 6_565 . C86 N1 Ni 127.93(13) 6_565 . C86 N1 Ni 127.93(13) . . C88 N2 C95 104.21(18) . . C88 N2 Ni 127.86(14) . . C95 N2 Ni 127.90(14) . . C97 N3 C97 104.3(3) 6_565 . C97 N3 Ni 127.77(12) 6_565 . C97 N3 Ni 127.77(13) . . C101 C106 C105 122.3(6) . . C101 C106 H106 118.8 . . C105 C106 H106 118.8 . . C104 C105 C106 119.3(5) . . C104 C105 H105 120.3 . . C106 C105 H105 120.3 . . C105 C104 C103 121.2(6) . . C105 C104 H104 119.4 . . C103 C104 H104 119.4 . . C104 C103 C102 118.2(6) . . C104 C103 H103 120.9 . . C102 C103 H103 120.9 . . C101 C102 C103 120.8(5) . . C101 C102 H102 119.6 . . C103 C102 H102 119.6 . . C106 C101 C102 118.2(5) . . C106 C101 H101 120.9 . . C102 C101 H101 120.9 . . C99 C100 H10A 109.5 . . C99 C100 H10B 109.5 . . H10A C100 H10B 109.5 . . C99 C100 H10C 109.5 . . H10A C100 H10C 109.5 . . H10B C100 H10C 109.5 . . C98 C99 C100 111.97(19) . . C98 C99 H99A 109.2 . . C100 C99 H99A 109.2 . . C98 C99 H99B 109.2 . . C100 C99 H99B 109.2 . . H99A C99 H99B 107.9 . . C98 C98 C97 106.43(12) 6_565 . C98 C98 C99 128.77(13) 6_565 . C97 C98 C99 124.6(2) . . C96 C97 N3 125.2(2) . . C96 C97 C98 123.4(2) . . N3 C97 C98 111.4(2) . . C95 C96 C97 124.2(2) . . C95 C96 H96 117.9 . . C97 C96 H96 117.9 . . C96 C95 N2 124.84(19) . . C96 C95 C92 123.5(2) . . N2 C95 C92 111.68(19) . . C93 C94 H94A 109.5 . . C93 C94 H94B 109.5 . . H94A C94 H94B 109.5 . . C93 C94 H94C 109.5 . . H94A C94 H94C 109.5 . . H94B C94 H94C 109.5 . . C92 C93 C94 113.4(2) . . C92 C93 H93A 108.9 . . C94 C93 H93A 108.9 . . C92 C93 H93B 108.9 . . C94 C93 H93B 108.9 . . H93A C93 H93B 107.7 . . C89 C92 C95 106.32(19) . . C89 C92 C93 129.2(2) . . C95 C92 C93 124.5(2) . . C90 C91 H91A 109.5 . . C90 C91 H91B 109.5 . . H91A C91 H91B 109.5 . . C90 C91 H91C 109.5 . . H91A C91 H91C 109.5 . . H91B C91 H91C 109.5 . . C89 C90 C91 112.8(2) . . C89 C90 H90A 109.0 . . C91 C90 H90A 109.0 . . C89 C90 H90B 109.0 . . C91 C90 H90B 109.0 . . H90A C90 H90B 107.8 . . C92 C89 C88 106.45(19) . . C92 C89 C90 129.1(2) . . C88 C89 C90 124.4(2) . . C87 C88 N2 124.93(19) . . C87 C88 C89 123.7(2) . . N2 C88 C89 111.33(19) . . C86 C87 C88 124.2(2) . . C86 C87 H87 117.9 . . C88 C87 H87 117.9 . . C87 C86 N1 125.1(2) . . C87 C86 C85 123.3(2) . . N1 C86 C85 111.5(2) . . C85 C85 C86 106.45(13) 6_565 . C85 C85 C84 128.85(13) 6_565 . C86 C85 C84 124.6(2) . . C85 C84 C83 113.2(2) . . C85 C84 H84A 108.9 . . C83 C84 H84A 108.9 . . C85 C84 H84B 108.9 . . C83 C84 H84B 108.9 . . H84A C84 H84B 107.7 . . C84 C83 H83A 109.5 . . C84 C83 H83B 109.5 . . H83A C83 H83B 109.5 . . C84 C83 H83C 109.5 . . H83A C83 H83C 109.5 . . H83B C83 H83C 109.5 . . C2Z C1Z C6Z 120.0 . . C2Z C1Z H1Z 120.0 . . C6Z C1Z H1Z 120.0 . . C1Z C2Z C3Z 120.0 . . C1Z C2Z H2Z 120.0 . . C3Z C2Z H2Z 120.0 . . C4Z C3Z C2Z 120.0 . . C4Z C3Z H3Z 120.0 . . C2Z C3Z H3Z 120.0 . . C3Z C4Z C5Z 120.0 . . C3Z C4Z H4Z 120.0 . . C5Z C4Z H4Z 120.0 . . C4Z C5Z C6Z 120.0 . . C4Z C5Z H5Z 120.0 . . C6Z C5Z H5Z 120.0 . . C5Z C6Z C1Z 120.0 . . C5Z C6Z H6Z 120.0 . . C1Z C6Z H6Z 120.0 . . C39 C61 C60 122.9(11) . . C39 C61 C62 119.0(9) . . C60 C61 C62 104.6(10) . . C51 C52 C53 128.8(10) . . C51 C52 C30 125.9(10) . . C53 C52 C30 99.2(9) . . C51 C52 Y2 73.7(6) . 6_565 C53 C52 Y2 83.5(9) . 6_565 C30 C52 Y2 91.5(7) . 6_565 C51 C52 Y3 75.9(4) . 6_565 C53 C52 Y3 71.0(6) . 6_565 C30 C52 Y3 103.2(6) . 6_565 C51 C52 Y1 67.2(4) . 6_565 C53 C52 Y1 78.7(6) . 6_565 C30 C52 Y1 106.7(6) . 6_565 C12 C11 C10 114.3(12) . . C12 C11 C29 127.8(8) . . C10 C11 C29 108.7(10) . . C9 C1 C5 115.3(14) . . C9 C1 C2 123.8(14) . . C5 C1 C2 113.7(13) . . C3 C2 C12 127.7(12) . . C3 C2 C1 100.9(11) . . C12 C2 C1 120.4(11) . . C2 C3 C15 113.1(11) . . C2 C3 C4 115.8(10) . . C15 C3 C4 122.9(10) . . C18 C4 C5 120.8(18) . . C18 C4 C3 120.1(11) . . C5 C4 C3 103.1(10) . . C1 C5 C4 106.4(12) . . C1 C5 C6 121.0(17) . . C4 C5 C6 125(2) . . C7 C6 C20 123.0(17) . . C7 C6 C5 123(2) . . C20 C6 C5 107.5(18) . . C6 C7 C8 113(2) . . C6 C7 C23 130(2) . . C8 C7 C23 108.6(12) . . C9 C8 C25 115(2) . . C9 C8 C7 124(2) . . C25 C8 C7 108.5(12) . . C1 C9 C8 124.4(18) . . C1 C9 C10 111.9(14) . . C8 C9 C10 117.3(19) . . C11 C10 C27 106.0(9) . . C11 C10 C9 125.3(14) . . C27 C10 C9 118.3(11) . . C11 C12 C2 123.8(10) . . C11 C12 C13 109.6(11) . . C2 C12 C13 119.9(12) . . C31 C13 C12 122.1(16) . . C31 C13 C14 114.5(15) . . C12 C13 C14 115.0(12) . . C15 C14 C34 102.4(10) . . C15 C14 C13 117.1(11) . . C34 C14 C13 130.9(14) . . C3 C15 C16 113.5(10) . . C3 C15 C14 127.0(11) . . C16 C15 C14 114.5(10) . . C35 C16 C15 102.9(10) . . C35 C16 C17 114.6(13) . . C15 C16 C17 126.3(11) . . C18 C17 C38 123.2(13) . . C18 C17 C16 112.0(10) . . C38 C17 C16 120.8(13) . . C4 C18 C17 122.2(12) . . C4 C18 C19 119.5(16) . . C17 C18 C19 114.1(13) . . C18 C19 C20 115.3(15) . . C18 C19 C40 124.9(14) . . C20 C19 C40 111.5(11) . . C6 C20 C19 129.8(15) . . C6 C20 C21 114.2(15) . . C19 C20 C21 106.1(11) . . C22 C21 C20 121.0(15) . . C22 C21 C41 118.5(17) . . C20 C21 C41 107.2(11) . . C44 C22 C21 124.5(14) . . C44 C22 C23 106.7(13) . . C21 C22 C23 121.9(12) . . C24 C23 C7 104.0(12) . . C24 C23 C22 138.1(13) . . C7 C23 C22 109.5(14) . . C25 C24 C23 112.1(12) . . C25 C24 C46 120.1(17) . . C23 C24 C46 108.2(14) . . C24 C25 C8 104.0(12) . . C28 C27 C10 109.8(10) . . C50 C28 C27 125.1(13) . . C50 C28 C29 117.7(14) . . C27 C28 C29 106.2(10) . . C30 C29 C28 118.6(15) . . C30 C29 C11 122.4(13) . . C28 C29 C11 109.2(10) . . C29 C30 C31 113.4(15) . . C29 C30 C52 122.4(14) . . C31 C30 C52 114.2(11) . . C13 C31 C32 121.3(17) . . C13 C31 C30 124.3(17) . . C32 C31 C30 105.5(11) . . C31 C32 C53 105.0(10) . . C31 C32 C33 120.8(16) . . C53 C32 C33 127.1(13) . . C34 C33 C32 124.3(15) . . C34 C33 C56 110.6(13) . . C32 C33 C56 119.3(13) . . C14 C34 C33 107.8(13) . . C14 C34 C35 108.3(10) . . C33 C34 C35 133.0(12) . . C16 C35 C36 125.2(13) . . C16 C35 C34 111.8(10) . . C36 C35 C34 115.6(12) . . C35 C36 C57 113.8(13) . . C35 C36 C37 123.3(17) . . C57 C36 C37 110.7(11) . . C59 C37 C38 137.9(18) . . C59 C37 C36 105.8(12) . . C38 C37 C36 112.8(17) . . C37 C38 C17 120.8(15) . . C37 C38 C39 99.8(14) . . C17 C38 C39 121.6(13) . . C40 C39 C61 122.5(14) . . C40 C39 C38 110.0(14) . . C61 C39 C38 124.1(13) . . C39 C40 C41 115.0(18) . . C39 C40 C19 123.2(16) . . C41 C40 C19 104.9(11) . . C42 C41 C40 125.7(16) . . C42 C41 C21 118.0(16) . . C40 C41 C21 109.9(11) . . C41 C42 C43 118.5(15) . . C41 C42 C62 121.3(14) . . C43 C42 C62 111.8(15) . . C42 C43 C44 126.2(17) . . C42 C43 C65 115.4(17) . . C44 C43 C65 108.1(10) . . C22 C44 C43 113.9(16) . . C22 C44 C45 126.6(16) . . C43 C44 C45 109.9(10) . . C66 C45 C44 105.0(10) . . C66 C45 C46 128.1(15) . . C44 C45 C46 118.4(16) . . C47 C46 C24 131.1(18) . . C47 C46 C45 98.7(15) . . C24 C46 C45 121.2(16) . . C68 C47 C46 140.4(18) . . C68 C47 C48 107.3(11) . . C46 C47 C48 94.8(16) . . C49 C48 C47 106.3(11) . . C69 C49 C48 109.4(11) . . C69 C49 C50 109.9(11) . . C48 C49 C50 130.0(12) . . C28 C50 C51 126.1(12) . . C28 C50 C49 112.2(12) . . C51 C50 C49 116.1(10) . . C52 C51 C71 114.2(10) . . C52 C51 C50 109.2(10) . . C71 C51 C50 125.9(11) . . C54 C53 C52 112.0(12) . . C54 C53 C32 114.5(12) . . C52 C53 C32 113.5(10) . . C53 C54 C72 124.8(13) . . C53 C54 C55 120.7(10) . . C72 C54 C55 109.7(10) . . C74 C55 C54 107.5(10) . . C74 C55 C56 115.6(11) . . C54 C55 C56 127.0(10) . . C57 C56 C33 116.6(12) . . C57 C56 C55 122.6(11) . . C33 C56 C55 110.2(11) . . C56 C57 C36 129.3(13) . . C56 C57 C58 119.5(13) . . C36 C57 C58 104.7(10) . . C75 C58 C59 123.1(14) . . C75 C58 C57 117.6(14) . . C59 C58 C57 109.1(10) . . C60 C59 C37 120.3(17) . . C60 C59 C58 118.5(16) . . C37 C59 C58 108.4(11) . . C59 C60 C61 114.2(14) . . C59 C60 C77 124.8(14) . . C61 C60 C77 112.7(10) . . C42 C62 C63 125.4(13) . . C42 C62 C61 115.2(12) . . C63 C62 C61 109.7(10) . . C64 C63 C62 127.6(14) . . C64 C63 C77 114.3(13) . . C62 C63 C77 108.8(10) . . C63 C64 C79 124.0(12) . . C63 C64 C65 103.5(16) . . C79 C64 C65 124.7(13) . . C66 C65 C43 107.2(10) . . C66 C65 C64 108.5(17) . . C43 C65 C64 134.7(16) . . C65 C66 C45 109.8(11) . . C65 C66 C67 123.3(18) . . C45 C66 C67 114.9(17) . . C68 C67 C80 101.3(18) . . C68 C67 C66 127(2) . . C80 C67 C66 125(2) . . C67 C68 C47 106.6(19) . . C67 C68 C69 140.0(19) . . C47 C68 C69 107.6(11) . . C70 C69 C49 134.5(12) . . C70 C69 C68 108.8(12) . . C49 C69 C68 108.6(11) . . C71 C70 C69 112.1(15) . . C71 C70 C81 122.8(15) . . C69 C70 C81 119.4(13) . . C72 C71 C70 112.9(14) . . C72 C71 C51 120.0(11) . . C70 C71 C51 120.7(15) . . C54 C72 C71 119.1(12) . . C54 C72 C73 104.7(10) . . C71 C72 C73 123.4(12) . . C82 C73 C74 121.2(14) . . C82 C73 C72 123.1(15) . . C74 C73 C72 109.2(10) . . C55 C74 C73 108.8(11) . . C55 C74 C75 121.7(14) . . C73 C74 C75 120.9(13) . . C58 C75 C74 122.9(16) . . C58 C75 C76 114.0(16) . . C74 C75 C76 115.1(13) . . C77 C76 C78 109.9(17) . . C77 C76 C75 126.0(17) . . C78 C76 C75 116.0(16) . . C76 C77 C60 113.5(13) . . C76 C77 C63 130.1(13) . . C60 C77 C63 104.2(9) . . C82 C78 C79 105.6(10) . . C82 C78 C76 120.0(14) . . C79 C78 C76 125.4(14) . . C80 C79 C78 110.5(11) . . C80 C79 C64 124.4(10) . . C78 C79 C64 115.3(9) . . C67 C80 C81 131.1(15) . . C67 C80 C79 113.4(14) . . C81 C80 C79 106.2(12) . . C80 C81 C70 118.0(14) . . C80 C81 C82 109.0(11) . . C70 C81 C82 121.3(14) . . C73 C82 C78 126.6(14) . . C73 C82 C81 115.4(16) . . C78 C82 C81 108.6(10) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Y1 Y2 0.79(2) . Y1 C52 2.685(8) 6_565 Y1 Y2 2.798(17) 6_565 Y1 Y1 2.860(7) 6_565 Y1 Y3 3.176(4) 6_565 Y2 Y3 0.71(2) . Y2 C52 2.245(10) 6_565 Y2 Y2 2.52(4) 6_565 Y2 Y3 3.034(17) 6_565 Y3 C52 2.489(7) 6_565 Y3 Y3 3.458(6) 6_565 Ni N1 1.953(3) . Ni N3 1.956(3) . Ni N2 1.9637(18) 6_565 Ni N2 1.9637(18) . N1 C86 1.377(3) 6_565 N1 C86 1.377(3) . N2 C88 1.375(3) . N2 C95 1.375(3) . N3 C97 1.376(3) 6_565 N3 C97 1.376(3) . C106 C101 1.358(7) . C106 C105 1.396(7) . C106 H106 0.9500 . C105 C104 1.334(8) . C105 H105 0.9500 . C104 C103 1.381(8) . C104 H104 0.9500 . C103 C102 1.426(11) . C103 H103 0.9500 . C102 C101 1.362(10) . C102 H102 0.9500 . C101 H101 0.9500 . C100 C99 1.527(4) . C100 H10A 0.9800 . C100 H10B 0.9800 . C100 H10C 0.9800 . C99 C98 1.495(3) . C99 H99A 0.9900 . C99 H99B 0.9900 . C98 C98 1.356(5) 6_565 C98 C97 1.446(3) . C97 C96 1.375(3) . C96 C95 1.374(3) . C96 H96 0.9500 . C95 C92 1.443(3) . C94 C93 1.525(4) . C94 H94A 0.9800 . C94 H94B 0.9800 . C94 H94C 0.9800 . C93 C92 1.500(3) . C93 H93A 0.9900 . C93 H93B 0.9900 . C92 C89 1.355(4) . C91 C90 1.526(4) . C91 H91A 0.9800 . C91 H91B 0.9800 . C91 H91C 0.9800 . C90 C89 1.504(3) . C90 H90A 0.9900 . C90 H90B 0.9900 . C89 C88 1.448(3) . C88 C87 1.373(3) . C87 C86 1.372(3) . C87 H87 0.9500 . C86 C85 1.443(3) . C85 C85 1.354(5) 6_565 C85 C84 1.496(3) . C84 C83 1.518(4) . C84 H84A 0.9900 . C84 H84B 0.9900 . C83 H83A 0.9800 . C83 H83B 0.9800 . C83 H83C 0.9800 . C1Z C2Z 1.3900 . C1Z C6Z 1.3900 . C1Z H1Z 0.9500 . C2Z C3Z 1.3900 . C2Z H2Z 0.9500 . C3Z C4Z 1.3900 . C3Z H3Z 0.9500 . C4Z C5Z 1.3900 . C4Z H4Z 0.9500 . C5Z C6Z 1.3900 . C5Z H5Z 0.9500 . C6Z H6Z 0.9500 . C61 C39 1.49(2) . C61 C60 1.498(13) . C61 C62 1.511(14) . C52 C51 1.369(11) . C52 C53 1.398(11) . C52 C30 1.407(13) . C11 C12 1.267(19) . C11 C10 1.406(10) . C11 C29 1.447(13) . C1 C9 1.26(3) . C1 C5 1.368(16) . C1 C2 1.405(14) . C2 C3 1.336(12) . C2 C12 1.372(14) . C3 C15 1.383(15) . C3 C4 1.415(12) . C4 C18 1.400(16) . C4 C5 1.403(15) . C5 C6 1.52(2) . C6 C7 1.25(3) . C6 C20 1.43(3) . C7 C8 1.434(17) . C7 C23 1.436(16) . C8 C9 1.39(2) . C8 C25 1.431(17) . C9 C10 1.510(19) . C10 C27 1.477(15) . C12 C13 1.450(16) . C13 C31 1.33(2) . C13 C14 1.471(17) . C14 C15 1.413(11) . C14 C34 1.415(14) . C15 C16 1.406(12) . C16 C35 1.361(13) . C16 C17 1.484(16) . C17 C18 1.412(16) . C17 C38 1.460(16) . C18 C19 1.446(16) . C19 C20 1.454(15) . C19 C40 1.461(13) . C20 C21 1.462(15) . C21 C22 1.41(2) . C21 C41 1.481(16) . C22 C44 1.393(19) . C22 C23 1.50(2) . C23 C24 1.421(16) . C24 C25 1.413(17) . C24 C46 1.488(15) . C27 C28 1.418(15) . C28 C50 1.374(17) . C28 C29 1.429(13) . C29 C30 1.25(2) . C30 C31 1.404(15) . C31 C32 1.389(15) . C32 C53 1.419(11) . C32 C33 1.444(16) . C33 C34 1.415(17) . C33 C56 1.459(14) . C34 C35 1.420(12) . C35 C36 1.400(15) . C36 C57 1.458(12) . C36 C37 1.461(16) . C37 C59 1.445(16) . C37 C38 1.46(3) . C38 C39 1.573(16) . C39 C40 1.424(19) . C40 C41 1.446(15) . C41 C42 1.40(2) . C42 C43 1.408(19) . C42 C62 1.47(2) . C43 C44 1.414(14) . C43 C65 1.460(15) . C44 C45 1.468(15) . C45 C66 1.458(16) . C45 C46 1.520(16) . C46 C47 1.481(15) . C47 C68 1.453(17) . C47 C48 1.489(16) . C48 C49 1.448(16) . C49 C69 1.422(15) . C49 C50 1.545(16) . C50 C51 1.424(19) . C51 C71 1.419(16) . C53 C54 1.348(15) . C54 C72 1.382(11) . C54 C55 1.429(12) . C55 C74 1.362(13) . C55 C56 1.478(15) . C56 C57 1.426(16) . C57 C58 1.468(14) . C58 C75 1.34(2) . C58 C59 1.462(15) . C59 C60 1.32(2) . C60 C77 1.514(15) . C62 C63 1.507(14) . C63 C64 1.282(19) . C63 C77 1.522(15) . C64 C79 1.442(17) . C64 C65 1.53(2) . C65 C66 1.433(15) . C66 C67 1.52(3) . C67 C68 1.32(3) . C67 C80 1.38(2) . C68 C69 1.455(16) . C69 C70 1.409(14) . C70 C71 1.401(14) . C70 C81 1.412(13) . C71 C72 1.384(17) . C72 C73 1.445(15) . C73 C82 1.30(2) . C73 C74 1.382(14) . C74 C75 1.51(2) . C75 C76 1.57(2) . C76 C77 1.29(2) . C76 C78 1.44(2) . C78 C82 1.387(14) . C78 C79 1.436(12) . C79 C80 1.402(13) . C80 C81 1.390(14) . C81 C82 1.437(14) .