#------------------------------------------------------------------------------ #$Date: 2019-04-28 01:11:52 +0300 (Sun, 28 Apr 2019) $ #$Revision: 214820 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/33/7123343.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_7123343 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_sum 'C256 H106 N8 Ni2 S4 Y2' _chemical_formula_weight 3716.96 _chemical_name_common Y@C2v(9)-C82-Ni(OEP) _chemical_name_systematic Y@C2v(9)-C82-Ni(OEP) _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 107.076(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 26.7012(15) _cell_length_b 17.2044(10) _cell_length_c 17.8379(10) _cell_measurement_reflns_used 9882 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 24.88 _cell_measurement_theta_min 2.45 _cell_volume 7833.1(8) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 quest' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0586 _diffrn_reflns_av_unetI/netI 0.0385 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _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 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 58599 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.681 _diffrn_reflns_theta_min 2.652 _diffrn_source 'Bruker D8 quest' _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6969 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.576 _exptl_crystal_description block _exptl_crystal_F_000 3792 _exptl_crystal_size_max 0.040 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _refine_diff_density_max 1.304 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.111 _refine_ls_extinction_coef 0.0015(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2016/6 (Sheldrick 2016)' _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 999 _refine_ls_number_reflns 7691 _refine_ls_number_restraints 3934 _refine_ls_restrained_S_all 1.399 _refine_ls_R_factor_all 0.1823 _refine_ls_R_factor_gt 0.1346 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1923P)^2^+53.5859P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3585 _refine_ls_wR_factor_ref 0.3993 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4881 _reflns_number_total 7691 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc02095k2.cif _cod_data_source_block sad _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 7123343 _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 0.957 _shelx_estimated_absorpt_t_max 0.978 _exptl_absorpt_special_details SADABS _shelx_res_file ; TITL sad.res in C2/m sad.res created by SHELXL-2016/6 at 02:16:35 on 01-Jan-2019 CELL 0.71073 26.7012 17.2044 17.8379 90.000 107.076 90.000 ZERR 2.000 0.0015 0.0010 0.0010 0.000 0.002 0.000 LATT 7 SYMM -X, Y, -Z SFAC C H N S NI Y UNIT 512 212 16 8 4 4 TEMP -100 SIZE 0.04 0.04 0.02 !black block L.S. 20 BOND $H LIST 6 ACTA FMAP 2 PLAN 10 DFIX 1.40 0.01 C107 C108 C108 C109 SIMU 0.025 C1 > C82 EADP C10 C2 C53 EADP C24 C20 C8 OMIT 8 2 3 OMIT -1 1 1 OMIT 2 0 1 OMIT -2 0 1 OMIT 2 0 0 OMIT 0 2 0 OMIT -2 0 2 OMIT 1 1 0 OMIT 0 0 2 OMIT 4 8 2 OMIT -1 1 2 OMIT 8 0 6 OMIT 1 1 1 OMIT -6 2 2 OMIT 0 0 1 rem pentagon SADI 0.03 C1 C2 C2 C12 C12 C11 C11 C10 C10 C1 SADI 0.06 C1 C12 C1 C11 C2 C11 C2 C10 C12 C10 SADI 0.03 C7 C8 C8 C24 C24 C23 C23 C22 C22 C7 SADI 0.06 C7 C24 C7 C23 C8 C23 C8 C22 C24 C22 SADI 0.03 C14 C15 C15 C16 C16 C35 C35 C34 C34 C14 SADI 0.06 C14 C16 C14 C35 C15 C35 C15 C34 C16 C34 SADI 0.03 C4 C5 C5 C20 C20 C19 C19 C18 C18 C4 SADI 0.06 C4 C20 C4 C19 C5 C19 C5 C18 C20 C18 SADI 0.03 C26 C27 C27 C28 C28 C50 C50 C49 C49 C26 SADI 0.06 C26 C28 C26 C50 C27 C50 C27 C49 C28 C49 SADI 0.03 C30 C31 C31 C32 C32 C53 C53 C52 C52 C30 SADI 0.06 C30 C32 C30 C53 C31 C53 C31 C52 C32 C52 SADI 0.03 C37 C38 C38 C39 C39 C61 C61 C60 C60 C37 SADI 0.06 C37 C39 C37 C61 C38 C61 C38 C60 C39 C60 SADI 0.03 C41 C42 C42 C43 C43 C64 C64 C63 C63 C41 SADI 0.06 C41 C43 C41 C64 C42 C64 C42 C63 C43 C63 SADI 0.03 C47 C48 C48 C70 C70 C69 C69 C68 C68 C47 SADI 0.06 C47 C70 C47 C69 C48 C69 C48 C68 C70 C68 SADI 0.03 C54 C55 C55 C74 C74 C73 C73 C72 C72 C54 SADI 0.06 C54 C74 C54 C73 C55 C73 C55 C72 C74 C72 SADI 0.03 C58 C59 C59 C77 C77 C76 C76 C75 C75 C58 SADI 0.06 C58 C77 C58 C76 C59 C76 C59 C75 C77 C75 SADI 0.03 C65 C66 C66 C67 C67 C80 C80 C79 C79 C65 SADI 0.06 C65 C67 C65 C80 C66 C80 C66 C79 C67 C79 SADI 0.02 C42 C41 C41 C63 C63 C64 C64 C43 C43 C42 SADI 0.04 C42 C63 C42 C64 C41 C64 C41 C43 C63 C43 rem hex SADI 0.03 C48 C70 C70 C71 C71 C51 C51 C50 C50 C49 C49 C48 SADI 0.06 C48 C71 C48 C50 C70 C51 C70 C49 C51 C49 C71 C50 SADI 0.03 C48 C47 C47 C46 C46 C25 C25 C26 C26 C49 C49 C48 SADI 0.06 C48 C46 C48 C26 C47 C25 C47 C49 C25 C49 C46 C26 SADI 0.03 C10 C9 C9 C27 C27 C28 C28 C29 C29 C11 C11 C10 SADI 0.06 C10 C27 C10 C29 C9 C28 C9 C11 C28 C11 C27 C29 SADI 0.03 C67 C80 C80 C81 C81 C82 C82 C69 C69 C68 C68 C67 SADI 0.06 C67 C81 C67 C69 C80 C82 C80 C68 C82 C68 C81 C69 SADI 0.03 C41 C40 C40 C39 C39 C61 C61 C62 C62 C63 C63 C41 SADI 0.06 C41 C39 C41 C62 C40 C61 C40 C63 C61 C63 C39 C62 SADI 0.03 C75 C74 C74 C73 C73 C82 C82 C81 C81 C76 C76 C75 SADI 0.06 C75 C73 C75 C81 C74 C82 C74 C76 C82 C76 C73 C81 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 0.03 C56 C75 C58 C55 C57 C74 sadi 0.03 c36 c17 c16 c37 c35 c38 SADI 0.03 C36 C35 C35 C34 C34 C33 C33 C56 C56 C57 C57 C36 SADI 0.06 C36 C34 C36 C56 C35 C33 C35 C57 C33 C57 C34 C56 SADI 0.03 C45 C46 C46 C25 C25 C24 C24 C23 C23 C44 C44 C45 SADI 0.06 C45 C25 C45 C23 C46 C24 C46 C44 C24 C44 C25 C23 SADI 0.03 C21 C20 C20 C5 C5 C6 C6 C7 C7 C22 C22 C21 SADI 0.06 C21 C5 C21 C7 C20 C6 C20 C22 C6 C22 C5 C7 sadi 0.03 c33 C54 C53 C56 C55 C32 SADI 0.03 c79 c78 C78 C77 C78 C62 C62 C63 C62 C61 SADI 0.03 C9 C27 C9 C8 C9 C10 SADI 0.03 C29 C51 C29 C13 C29 C9 SADI 0.03 C56 C33 C56 C57 C56 C55 SADI 0.03 C13 C31 C13 C12 C13 C14 SADI 0.06 c11 c31 C11 C27 SADI 0.06 c51 C29 C51 C54 C51 C48 SADI 0.03 c29 c30 C29 C28 C29 C11 SUMP 0.5 0.0001 1 2 1 3 1 4 1 5 WGHT 0.192300 53.585941 EXTI 0.001503 FVAR 0.19312 PART 2 Y1 6 0.238245 1.000000 0.280292 10.08284 0.17356 PART -4 Y3 6 0.271593 1.032051 0.143204 10.11631 0.11178 0.12088 = 0.25876 0.00043 0.11725 -0.02197 PART -2 Y4 6 0.266638 0.936438 0.151945 10.07156 0.04070 0.03620 = 0.03200 0.02706 0.03055 0.02723 PART -3 Y2 6 0.260078 0.916106 0.188950 10.22929 0.07111 0.05968 = 0.17029 -0.00418 -0.00627 0.03608 PART 1 C1 1 0.119239 1.000000 -0.067990 10.50000 0.14780 0.27343 = 0.07639 0.00000 -0.02054 0.00000 PART -1 10.5000 C43 1 0.340031 0.980753 0.094863 10.50000 0.08746 0.10196 = 0.16286 0.03354 0.10069 0.03006 C2 1 0.089195 0.944873 -0.036961 10.50000 0.10689 0.18215 = 0.11675 0.03879 0.01779 -0.00398 C3 1 0.103579 0.861631 -0.008542 10.50000 0.07436 0.13985 = 0.06913 -0.02756 0.00460 -0.05960 C4 1 0.144090 0.847547 -0.022500 10.50000 0.11342 0.16491 = 0.06716 -0.05778 0.00438 -0.07720 C5 1 0.170513 0.905610 -0.058713 10.50000 0.14040 0.18632 = 0.05233 -0.04661 0.05418 -0.06884 C6 1 0.163653 0.987036 -0.075652 10.50000 0.19280 0.27190 = 0.05773 -0.00270 0.02836 -0.03459 C7 1 0.205766 1.044506 -0.064876 10.50000 0.18552 0.20900 = 0.04002 0.00582 0.05225 -0.06861 C8 1 0.203464 1.123548 -0.030195 10.50000 0.16884 0.17109 = 0.11809 0.00806 0.08994 -0.03633 C9 1 0.153789 1.147982 -0.020099 10.50000 0.18116 0.15603 = 0.13124 0.04766 0.01838 0.00104 C10 1 0.115857 1.086633 -0.046203 10.50000 0.10689 0.18215 = 0.11675 0.03879 0.01779 -0.00398 C11 1 0.078634 1.077045 0.002019 10.50000 0.08948 0.15677 = 0.14522 0.03941 -0.06214 0.02593 C12 1 0.066648 0.996222 0.009024 10.50000 0.07504 0.16915 = 0.14624 0.02954 -0.03414 0.00818 C13 1 0.052358 0.961029 0.073668 10.50000 0.05645 0.16322 = 0.17731 0.02858 -0.02251 -0.02261 C14 1 0.062454 0.881529 0.100858 10.50000 0.06305 0.14165 = 0.15542 -0.01503 0.03041 -0.05887 C15 1 0.086760 0.842446 0.048842 10.50000 0.09198 0.14673 = 0.11968 -0.04899 0.00243 -0.06095 C16 1 0.121988 0.788060 0.099246 10.50000 0.10566 0.07571 = 0.12769 -0.05525 0.03640 -0.05559 C17 1 0.175941 0.763179 0.097453 10.50000 0.13160 0.09981 = 0.11901 -0.03740 0.04319 -0.02514 C18 1 0.187322 0.799792 0.025133 10.50000 0.12076 0.14424 = 0.10374 -0.08500 0.03146 0.00805 C19 1 0.234510 0.828696 0.017510 10.50000 0.16439 0.16678 = 0.10786 -0.06930 0.07025 -0.00242 C20 1 0.225664 0.887671 -0.042238 10.50000 0.16884 0.17109 = 0.11809 0.00806 0.08994 -0.03633 C21 1 0.269705 0.937298 -0.008477 10.50000 0.17856 0.20596 = 0.11650 -0.01077 0.09934 0.00197 C22 1 0.259907 1.017427 -0.030973 10.50000 0.20570 0.18061 = 0.09140 0.01599 0.10779 -0.01072 C23 1 0.292149 1.079857 0.019317 10.50000 0.14928 0.20756 = 0.10802 0.03302 0.10212 -0.03097 C24 1 0.257749 1.144194 0.012685 10.50000 0.16884 0.17109 = 0.11809 0.00806 0.08994 -0.03633 C25 1 0.253339 1.191480 0.079031 10.50000 0.18073 0.11275 = 0.18997 0.04907 0.06164 -0.07373 C26 1 0.204659 1.221210 0.088588 10.50000 0.13590 0.04394 = 0.17509 0.05436 0.08119 0.02130 C27 1 0.151267 1.198707 0.042838 10.50000 0.15470 0.05573 = 0.12520 0.05947 0.04762 0.02425 C28 1 0.115556 1.187380 0.086973 10.50000 0.13031 0.06188 = 0.19255 0.05160 0.02338 0.03799 C29 1 0.077259 1.124709 0.067337 10.50000 0.07835 0.11634 = 0.17683 0.08272 -0.00424 0.04288 C30 1 0.064607 1.096221 0.137217 10.50000 0.04898 0.12592 = 0.17813 0.04701 0.00547 0.04116 C31 1 0.051084 1.015307 0.138854 10.50000 0.04501 0.15384 = 0.19116 0.04843 0.02515 0.00590 C32 1 0.066008 0.988651 0.219249 10.50000 0.06336 0.14700 = 0.20070 0.04899 0.07903 0.00943 C33 1 0.089525 0.906699 0.247964 10.50000 0.13175 0.12938 = 0.17694 0.01156 0.12067 -0.05634 C34 1 0.084269 0.858060 0.179360 10.50000 0.11388 0.07999 = 0.11438 -0.01628 0.07818 -0.06212 C35 1 0.124404 0.799968 0.179972 10.50000 0.13233 0.06336 = 0.11392 -0.04015 0.06495 -0.05829 C36 1 0.167962 0.792462 0.249792 10.50000 0.15725 0.06896 = 0.13247 0.01281 0.05517 -0.02801 C37 1 0.206018 0.765189 0.230214 10.50000 0.12423 0.03979 = 0.12884 0.01102 0.08177 -0.00830 C38 1 0.219941 0.758742 0.158788 10.50000 0.08276 0.03824 = 0.13363 -0.01520 0.02493 0.01569 C39 1 0.270554 0.774668 0.168462 10.50000 0.09082 0.04305 = 0.11827 -0.01321 0.04997 0.02518 C40 1 0.283410 0.802871 0.103979 10.50000 0.10375 0.12204 = 0.12103 -0.05397 0.04352 0.05434 C41 1 0.320026 0.856330 0.114836 10.50000 0.10896 0.11564 = 0.13222 -0.01724 0.08736 0.04204 C42 1 0.313497 0.912929 0.056251 10.50000 0.11855 0.17287 = 0.13214 0.00208 0.10230 0.04175 C44 1 0.331620 1.070902 0.095673 10.50000 0.13301 0.17269 = 0.17191 0.04747 0.09558 -0.02298 C45 1 0.331810 1.122964 0.157707 10.50000 0.13193 0.14259 = 0.18342 0.05014 0.06576 -0.06412 C46 1 0.296368 1.188143 0.151976 10.50000 0.16840 0.09982 = 0.20543 0.05697 0.06167 -0.07735 C47 1 0.283165 1.206319 0.224137 10.50000 0.16297 0.08552 = 0.20803 -0.00629 0.04832 -0.06093 C48 1 0.233396 1.231781 0.231780 10.50000 0.19540 0.08631 = 0.23415 -0.01360 0.03444 -0.00369 C49 1 0.192998 1.232328 0.162865 10.50000 0.17449 0.05549 = 0.22772 0.02449 0.01412 0.02385 C50 1 0.140444 1.215625 0.164599 10.50000 0.13450 0.04543 = 0.20959 0.01635 0.07635 0.03312 C51 1 0.124887 1.181719 0.228813 10.50000 0.14251 0.09533 = 0.20904 -0.04215 0.07857 0.05400 C52 1 0.084905 1.122265 0.215971 10.50000 0.10718 0.13005 = 0.19226 0.01302 0.07089 0.04551 C53 1 0.087794 1.053437 0.267707 10.50000 0.10689 0.18215 = 0.11675 0.03879 0.01779 -0.00398 C54 1 0.130267 1.049090 0.330352 10.50000 0.19009 0.17946 = 0.13744 0.00891 0.13559 -0.02362 C55 1 0.147366 0.975294 0.360960 10.50000 0.18903 0.15725 = 0.10808 -0.02217 0.11859 -0.00508 C56 1 0.130169 0.901817 0.315213 10.50000 0.15575 0.11540 = 0.13735 0.01716 0.10524 -0.04606 C57 1 0.170331 0.843762 0.319993 10.50000 0.18975 0.08619 = 0.08101 0.00069 0.10318 -0.01930 C58 1 0.221141 0.863265 0.367755 10.50000 0.16461 0.12936 = 0.09639 0.04255 0.08755 0.03770 C59 1 0.265319 0.835007 0.350031 10.50000 0.15346 0.10994 = 0.09009 0.06490 0.05494 0.03905 C60 1 0.255450 0.791388 0.284312 10.50000 0.14988 0.03964 = 0.08482 0.00768 0.04742 0.03790 C61 1 0.293333 0.797617 0.244897 10.50000 0.08870 0.03714 = 0.12005 0.01623 0.01461 0.03091 C62 1 0.329699 0.858193 0.255512 10.50000 0.05771 0.06179 = 0.12098 0.02572 -0.00460 0.02830 C63 1 0.344255 0.888818 0.190420 10.50000 0.04149 0.10234 = 0.13820 -0.00684 0.03989 0.01634 C64 1 0.357547 0.965327 0.176664 10.50000 0.05401 0.08895 = 0.11811 -0.00452 0.05333 0.00099 C65 1 0.360814 1.021363 0.237084 10.50000 0.03760 0.07886 = 0.12173 -0.01161 0.01668 -0.01224 C66 1 0.348203 1.100375 0.231568 10.50000 0.07279 0.09386 = 0.13749 0.01457 0.00956 -0.04055 C67 1 0.338224 1.113369 0.305169 10.50000 0.12623 0.12992 = 0.15555 -0.02563 -0.01202 -0.07119 C68 1 0.301253 1.170738 0.299082 10.50000 0.16443 0.12929 = 0.17738 -0.04606 0.02056 -0.07859 C69 1 0.261687 1.155838 0.333179 10.50000 0.19834 0.11210 = 0.15755 -0.09960 0.02228 -0.04532 C70 1 0.218574 1.200019 0.296432 10.50000 0.19567 0.09159 = 0.18385 -0.08112 0.05606 0.02018 C71 1 0.168859 1.173285 0.298562 10.50000 0.22131 0.10862 = 0.17971 -0.06324 0.08597 0.03169 C72 1 0.170817 1.107265 0.345522 10.50000 0.22382 0.16640 = 0.15174 -0.05633 0.11358 -0.00798 C73 1 0.213309 1.071864 0.397113 10.50000 0.21343 0.15076 = 0.08859 -0.05281 0.10869 -0.02458 C74 1 0.199474 0.992355 0.390452 10.50000 0.24433 0.19714 = 0.10263 -0.00106 0.09915 0.00365 C75 1 0.236242 0.939734 0.394719 10.50000 0.15502 0.20061 = 0.06933 0.07316 0.05965 0.05040 C76 1 0.285616 0.962391 0.387718 10.50000 0.12984 0.16653 = 0.06187 0.06547 -0.03690 0.00353 C77 1 0.303044 0.893696 0.358903 10.50000 0.08138 0.09016 = 0.09760 0.05669 -0.02869 0.02126 C78 1 0.334058 0.914640 0.312662 10.50000 0.07957 0.09379 = 0.12747 0.02469 -0.03868 0.04743 C79 1 0.351117 0.987842 0.304495 10.50000 0.04306 0.08280 = 0.09341 0.01305 -0.00649 -0.02366 C80 1 0.330335 1.043132 0.343298 10.50000 0.11025 0.14344 = 0.11576 -0.01990 -0.03267 -0.02448 C81 1 0.299910 1.039613 0.394708 10.50000 0.14273 0.16473 = 0.08821 -0.01381 -0.04179 -0.00553 C82 1 0.261363 1.100008 0.387260 10.50000 0.19999 0.11013 = 0.09391 -0.05847 0.00587 -0.02438 PART 4 NI1 5 0.450503 1.000000 0.412720 10.50000 0.03583 0.12743 = 0.02276 0.00000 0.01311 0.00000 S1 4 0.294119 0.587896 0.262304 11.00000 0.20900 0.11613 = 0.23172 -0.03059 0.10086 -0.03579 N2 3 0.468338 0.919103 0.347150 11.00000 0.04077 0.14193 = 0.02669 0.01033 0.01305 0.02541 C83 1 0.401038 1.000000 0.566971 10.50000 0.03976 0.12082 = 0.02597 0.00000 0.01731 0.00000 AFIX 43 H83 2 0.388275 0.999999 0.611389 10.50000 -1.20000 AFIX 0 C84 1 0.409401 0.929183 0.537872 11.00000 0.04063 0.12098 = 0.02793 0.01247 0.01577 0.02347 C85 1 0.397562 0.856099 0.566183 11.00000 0.05961 0.12024 = 0.03268 0.02519 0.02164 0.03339 C86 1 0.372457 0.848064 0.631975 11.00000 0.06990 0.10351 = 0.04235 0.01606 0.02992 0.02671 AFIX 23 H86A 2 0.388387 0.886371 0.673554 11.00000 -1.20000 H86B 2 0.379760 0.795476 0.655148 11.00000 -1.20000 AFIX 0 C87 1 0.313266 0.860852 0.603502 11.00000 0.06628 0.11166 = 0.05583 0.01551 0.03525 0.01192 AFIX 137 H87A 2 0.305800 0.912233 0.579046 11.00000 -1.50000 H87B 2 0.298996 0.857796 0.648148 11.00000 -1.50000 H87C 2 0.297024 0.820732 0.565044 11.00000 -1.50000 AFIX 0 C88 1 0.410879 0.800002 0.523204 11.00000 0.07748 0.11136 = 0.04516 0.02883 0.03056 0.04913 C89 1 0.404683 0.713974 0.527780 11.00000 0.15689 0.12839 = 0.06179 0.05086 0.06860 0.08497 AFIX 23 H89A 2 0.405830 0.699832 0.582057 11.00000 -1.20000 H89B 2 0.434549 0.688085 0.515799 11.00000 -1.20000 AFIX 0 C90 1 0.354166 0.684059 0.472061 11.00000 0.20550 0.10444 = 0.08966 0.03995 0.07316 0.06240 AFIX 137 H90A 2 0.353323 0.696084 0.418003 11.00000 -1.50000 H90B 2 0.324372 0.709043 0.483869 11.00000 -1.50000 H90C 2 0.352051 0.627656 0.478188 11.00000 -1.50000 AFIX 0 C91 1 0.431533 0.839673 0.466595 11.00000 0.06480 0.12426 = 0.03791 0.02889 0.02478 0.05079 C92 1 0.448238 0.802213 0.411078 11.00000 0.08140 0.12370 = 0.04349 0.02405 0.03417 0.05369 AFIX 43 H92 2 0.448277 0.746995 0.411345 11.00000 -1.20000 AFIX 0 C93 1 0.465131 0.839647 0.354389 11.00000 0.05436 0.14199 = 0.03506 0.02132 0.01671 0.04487 C94 1 0.480547 0.799361 0.293593 11.00000 0.06718 0.14876 = 0.04127 0.01659 0.02622 0.06223 C95 1 0.479590 0.712498 0.283835 11.00000 0.14061 0.16682 = 0.07354 0.04498 0.06615 0.11156 AFIX 23 H95A 2 0.493564 0.688047 0.336067 11.00000 -1.20000 H95B 2 0.502959 0.698003 0.252075 11.00000 -1.20000 AFIX 0 C96 1 0.424846 0.680356 0.244445 11.00000 0.17108 0.09267 = 0.08964 0.00327 0.03600 0.05730 AFIX 137 H96A 2 0.408053 0.711118 0.197558 11.00000 -1.50000 H96B 2 0.403810 0.683253 0.281073 11.00000 -1.50000 H96C 2 0.427551 0.626076 0.229430 11.00000 -1.50000 AFIX 0 C97 1 0.493680 0.855154 0.249827 11.00000 0.05018 0.15963 = 0.03531 0.01599 0.02181 0.04655 C98 1 0.511493 0.843315 0.177291 11.00000 0.07339 0.17823 = 0.04094 0.01660 0.03178 0.05773 AFIX 23 H98A 2 0.531633 0.794260 0.182783 11.00000 -1.20000 H98B 2 0.535135 0.886420 0.173282 11.00000 -1.20000 AFIX 0 C99 1 0.465766 0.840063 0.102244 11.00000 0.10408 0.18732 = 0.03739 0.00231 0.03041 0.03114 AFIX 137 H99A 2 0.478305 0.821821 0.058900 11.00000 -1.50000 H99B 2 0.450565 0.892063 0.090106 11.00000 -1.50000 H99C 2 0.439047 0.804215 0.109504 11.00000 -1.50000 AFIX 0 C100 1 0.486231 0.929580 0.282629 11.00000 0.03767 0.14072 = 0.03007 0.00644 0.01665 0.02062 C101 1 0.495183 1.000000 0.253486 10.50000 0.03979 0.15476 = 0.02770 0.00000 0.01822 0.00000 AFIX 43 H101 2 0.508624 1.000000 0.209731 10.50000 -1.20000 AFIX 0 C102 1 0.294494 0.500000 0.261335 10.50000 0.16239 0.06491 = 0.11453 0.00000 0.04128 0.00000 C103 1 0.157368 0.500000 0.205601 10.50000 0.09421 0.08052 = 0.07628 0.00000 -0.00366 0.00000 AFIX 43 H103 2 0.177463 0.500000 0.259262 10.50000 -1.20000 AFIX 0 C104 1 0.142981 0.431898 0.167180 11.00000 0.10993 0.05271 = 0.08899 0.00939 0.01411 0.00574 AFIX 43 H104 2 0.155754 0.384260 0.192576 11.00000 -1.20000 AFIX 0 C105 1 0.110489 0.431200 0.092750 11.00000 0.12996 0.07562 = 0.06086 -0.00294 0.03666 -0.02822 AFIX 43 H105 2 0.099706 0.383424 0.066215 11.00000 -1.20000 AFIX 0 C106 1 0.093625 0.500000 0.056785 10.50000 0.10144 0.09683 = 0.04662 0.00000 0.01674 0.00000 AFIX 43 H106 2 0.069598 0.500001 0.005550 10.50000 -1.20000 AFIX 0 C107 1 0.006753 1.000000 0.581673 10.50000 0.24031 0.13722 = 0.15174 0.00000 0.09712 0.00000 AFIX 43 H107 2 0.011421 1.000000 0.636562 10.50000 -1.20000 AFIX 0 C108 1 0.048935 1.000000 0.550841 10.50000 0.12041 0.17669 = 0.18301 0.00000 0.01690 0.00000 AFIX 43 H108 2 0.083757 1.000000 0.584954 10.50000 -1.20000 AFIX 0 C109 1 0.040071 1.000000 0.469972 10.50000 0.23289 0.09871 = 0.22033 0.00000 0.17421 0.00000 AFIX 43 H109 2 0.069701 1.000000 0.450765 10.50000 -1.20000 AFIX 0 N1 3 0.430102 0.919327 0.475507 11.00000 0.03877 0.13087 = 0.02465 0.01250 0.01558 0.02319 PART 0 HKLF 4 REM sad.res in C2/m REM R1 = 0.1346 for 4881 Fo > 4sig(Fo) and 0.1823 for all 7691 data REM 999 parameters refined using 3934 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.304, deepest hole -0.947, 1-sigma level 0.111 Q1 1 0.2428 1.0582 0.2726 11.00000 0.05 1.30 Q2 1 0.2523 1.0000 0.4154 10.50000 0.05 1.15 Q3 1 0.2927 0.5000 0.3810 10.50000 0.05 1.13 Q4 1 0.2312 1.0000 -0.0666 10.50000 0.05 1.04 Q5 1 0.1303 1.0536 -0.0778 11.00000 0.05 1.01 Q6 1 0.2484 0.7839 0.0273 11.00000 0.05 0.92 Q7 1 0.3167 0.9901 0.0329 11.00000 0.05 0.92 Q8 1 0.0763 1.0000 0.2648 10.50000 0.05 0.85 Q9 1 0.2913 0.8494 0.0661 11.00000 0.05 0.81 Q10 1 0.3044 0.5593 0.3419 11.00000 0.05 0.74 ; _shelx_res_checksum 12327 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 0.2382(8) 1.000000 0.2803(11) 0.174(6) Uiso 0.1657 2 d S . P A 2 Y3 Y 0.2716(7) 1.0321(10) 0.1432(15) 0.150(9) Uani 0.1163 1 d . . P B -4 Y4 Y 0.2666(5) 0.9364(8) 0.1519(6) 0.032(3) Uani 0.0716 1 d . . P A -2 Y2 Y 0.2601(2) 0.9161(3) 0.1890(5) 0.109(2) Uani 0.2293 1 d . . P C -3 C1 C 0.1192(12) 1.000000 -0.0680(13) 0.177(8) Uani 1 2 d S TU P D 1 C43 C 0.3400(7) 0.9808(11) 0.0949(12) 0.104(7) Uani 0.5 1 d D U P D -1 C2 C 0.0892(13) 0.945(2) -0.0370(19) 0.138(5) Uani 0.5 1 d D U P D -1 C3 C 0.1036(9) 0.8616(16) -0.0085(12) 0.098(6) Uani 0.5 1 d . U P D -1 C4 C 0.1441(9) 0.8475(17) -0.0225(15) 0.120(7) Uani 0.5 1 d D U P D -1 C5 C 0.1705(8) 0.9056(13) -0.0587(11) 0.121(6) Uani 0.5 1 d D U P D -1 C6 C 0.1637(11) 0.9870(16) -0.0757(13) 0.176(8) Uani 0.5 1 d D U P D -1 C7 C 0.2058(10) 1.0445(13) -0.0649(10) 0.141(7) Uani 0.5 1 d D U P D -1 C8 C 0.2035(10) 1.1235(16) -0.0302(17) 0.142(5) Uani 0.5 1 d D U P D -1 C9 C 0.1538(12) 1.148(2) -0.020(2) 0.162(9) Uani 0.5 1 d D U P D -1 C10 C 0.1159(11) 1.0866(17) -0.0462(15) 0.138(5) Uani 0.5 1 d D U P D -1 C11 C 0.0786(8) 1.0770(14) 0.0020(14) 0.151(9) Uani 0.5 1 d D U P D -1 C12 C 0.0666(7) 0.9962(19) 0.0090(14) 0.144(7) Uani 0.5 1 d D U P D -1 C13 C 0.0524(8) 0.9610(13) 0.0737(16) 0.145(8) Uani 0.5 1 d D U P D -1 C14 C 0.0625(10) 0.8815(16) 0.1009(15) 0.120(7) Uani 0.5 1 d D U P D -1 C15 C 0.0868(11) 0.8424(16) 0.0488(14) 0.126(8) Uani 0.5 1 d D U P D -1 C16 C 0.1220(10) 0.7881(16) 0.0992(12) 0.103(7) Uani 0.5 1 d D U P D -1 C17 C 0.1759(13) 0.7632(18) 0.0975(16) 0.115(7) Uani 0.5 1 d D U P D -1 C18 C 0.1873(10) 0.7998(13) 0.0251(13) 0.123(7) Uani 0.5 1 d D U P D -1 C19 C 0.2345(10) 0.8287(16) 0.0175(14) 0.140(7) Uani 0.5 1 d D U P D -1 C20 C 0.2257(10) 0.8877(15) -0.0422(17) 0.142(5) Uani 0.5 1 d D U P D -1 C21 C 0.2697(11) 0.9373(17) -0.008(2) 0.155(8) Uani 0.5 1 d D U P D -1 C22 C 0.2599(10) 1.0174(13) -0.0310(14) 0.145(7) Uani 0.5 1 d D U P D -1 C23 C 0.2921(10) 1.0799(17) 0.0193(14) 0.141(7) Uani 0.5 1 d D U P D -1 C24 C 0.2577(10) 1.1442(15) 0.0127(15) 0.142(5) Uani 0.5 1 d D U P D -1 C25 C 0.2533(10) 1.1915(14) 0.0790(15) 0.160(8) Uani 0.5 1 d D U P D -1 C26 C 0.2047(8) 1.2212(12) 0.0886(14) 0.111(6) Uani 0.5 1 d D U P D -1 C27 C 0.1513(9) 1.1987(11) 0.0428(12) 0.110(6) Uani 0.5 1 d D U P D -1 C28 C 0.1156(10) 1.1874(16) 0.0870(16) 0.133(9) Uani 0.5 1 d D U P D -1 C29 C 0.0773(9) 1.1247(12) 0.0673(12) 0.133(9) Uani 0.5 1 d D U P D -1 C30 C 0.0646(10) 1.0962(15) 0.1372(14) 0.124(8) Uani 0.5 1 d D U P D -1 C31 C 0.0511(7) 1.0153(16) 0.1389(14) 0.132(7) Uani 0.5 1 d D U P D -1 C32 C 0.0660(6) 0.9887(16) 0.2192(13) 0.128(6) Uani 0.5 1 d D U P D -1 C33 C 0.0895(9) 0.9067(14) 0.2480(13) 0.130(7) Uani 0.5 1 d D U P D -1 C34 C 0.0843(8) 0.8581(11) 0.1794(11) 0.093(5) Uani 0.5 1 d D U P D -1 C35 C 0.1244(8) 0.8000(13) 0.1800(10) 0.097(6) Uani 0.5 1 d D U P D -1 C36 C 0.1680(10) 0.7925(13) 0.2498(11) 0.117(6) Uani 0.5 1 d D U P D -1 C37 C 0.2060(8) 0.7652(12) 0.2302(11) 0.088(5) Uani 0.5 1 d D U P D -1 C38 C 0.2199(7) 0.7587(12) 0.1588(12) 0.086(5) Uani 0.5 1 d D U P D -1 C39 C 0.2706(7) 0.7747(10) 0.1685(11) 0.080(5) Uani 0.5 1 d D U P D -1 C40 C 0.2834(9) 0.8029(13) 0.1040(13) 0.113(7) Uani 0.5 1 d D U P D -1 C41 C 0.3200(9) 0.8563(10) 0.1148(12) 0.108(6) Uani 0.5 1 d D U P D -1 C42 C 0.3135(11) 0.9129(14) 0.0563(12) 0.127(7) Uani 0.5 1 d D U P D -1 C44 C 0.3316(13) 1.0709(19) 0.0957(17) 0.148(8) Uani 0.5 1 d D U P D -1 C45 C 0.3318(12) 1.1230(18) 0.1577(19) 0.148(9) Uani 0.5 1 d D U P D -1 C46 C 0.2964(10) 1.1881(15) 0.1520(16) 0.156(9) Uani 0.5 1 d D U P D -1 C47 C 0.2832(11) 1.206(3) 0.2241(16) 0.153(10) Uani 0.5 1 d D U P D -1 C48 C 0.2334(9) 1.2318(19) 0.2318(15) 0.178(10) Uani 0.5 1 d D U P D -1 C49 C 0.1930(9) 1.2323(17) 0.1629(14) 0.162(9) Uani 0.5 1 d D U P D -1 C50 C 0.1404(10) 1.2156(16) 0.1646(14) 0.124(8) Uani 0.5 1 d D U P D -1 C51 C 0.1249(9) 1.1817(12) 0.2288(13) 0.143(8) Uani 0.5 1 d D U P D -1 C52 C 0.0849(12) 1.1223(14) 0.2160(16) 0.137(8) Uani 0.5 1 d D U P D -1 C53 C 0.0878(10) 1.0534(14) 0.2677(13) 0.138(5) Uani 0.5 1 d D U P D -1 C54 C 0.1303(9) 1.0491(12) 0.3304(14) 0.150(7) Uani 0.5 1 d D U P D -1 C55 C 0.1474(8) 0.9753(11) 0.3610(13) 0.135(7) Uani 0.5 1 d D U P D -1 C56 C 0.1302(8) 0.9018(11) 0.3152(13) 0.123(7) Uani 0.5 1 d D U P D -1 C57 C 0.1703(11) 0.8438(13) 0.3200(12) 0.105(6) Uani 0.5 1 d D U P D -1 C58 C 0.2211(9) 0.8633(13) 0.3678(14) 0.120(6) Uani 0.5 1 d D U P D -1 C59 C 0.2653(10) 0.8350(14) 0.3500(16) 0.114(7) Uani 0.5 1 d D U P D -1 C60 C 0.2555(8) 0.7914(10) 0.2843(11) 0.089(5) Uani 0.5 1 d D U P D -1 C61 C 0.2933(8) 0.7976(14) 0.2449(11) 0.085(6) Uani 0.5 1 d D U P D -1 C62 C 0.3297(7) 0.8582(10) 0.2555(11) 0.087(5) Uani 0.5 1 d D U P D -1 C63 C 0.3443(8) 0.8888(11) 0.1904(11) 0.091(6) Uani 0.5 1 d D U P D -1 C64 C 0.3575(6) 0.9653(9) 0.1767(11) 0.081(5) Uani 0.5 1 d D U P D -1 C65 C 0.3608(6) 1.0214(9) 0.2371(12) 0.081(5) Uani 0.5 1 d D U P D -1 C66 C 0.3482(11) 1.1004(12) 0.2316(16) 0.106(7) Uani 0.5 1 d D U P D -1 C67 C 0.3382(13) 1.1134(14) 0.305(2) 0.149(9) Uani 0.5 1 d D U P D -1 C68 C 0.3013(10) 1.1707(16) 0.2991(18) 0.163(9) Uani 0.5 1 d D U P D -1 C69 C 0.2617(12) 1.1558(17) 0.3332(17) 0.162(10) Uani 0.5 1 d D U P D -1 C70 C 0.2186(10) 1.2000(15) 0.2964(15) 0.157(9) Uani 0.5 1 d D U P D -1 C71 C 0.1689(11) 1.1733(17) 0.2986(16) 0.164(9) Uani 0.5 1 d D U P D -1 C72 C 0.1708(11) 1.1073(14) 0.3455(16) 0.168(8) Uani 0.5 1 d D U P D -1 C73 C 0.2133(9) 1.0719(13) 0.3971(15) 0.137(7) Uani 0.5 1 d D U P D -1 C74 C 0.1995(8) 0.9924(12) 0.3905(13) 0.171(7) Uani 0.5 1 d D U P D -1 C75 C 0.2362(8) 0.9397(13) 0.3947(14) 0.136(7) Uani 0.5 1 d D U P D -1 C76 C 0.2856(9) 0.9624(13) 0.3877(15) 0.133(8) Uani 0.5 1 d D U P D -1 C77 C 0.3030(7) 0.8937(12) 0.3589(12) 0.101(6) Uani 0.5 1 d D U P D -1 C78 C 0.3341(9) 0.9146(12) 0.3127(14) 0.115(7) Uani 0.5 1 d D U P D -1 C79 C 0.3511(5) 0.9878(12) 0.3045(10) 0.079(5) Uani 0.5 1 d D U P D -1 C80 C 0.3303(10) 1.0431(15) 0.3433(14) 0.137(9) Uani 0.5 1 d D U P D -1 C81 C 0.2999(10) 1.0396(14) 0.3947(19) 0.148(9) Uani 0.5 1 d D U P D -1 C82 C 0.2614(10) 1.1000(13) 0.3873(15) 0.143(8) Uani 0.5 1 d D U P D -1 Ni1 Ni 0.45050(4) 1.000000 0.41272(6) 0.0610(6) Uani 1 2 d S T P E 4 S1 S 0.2941(2) 0.5879(3) 0.2623(4) 0.178(2) Uani 1 1 d . . . F 4 N2 N 0.4683(2) 0.9191(5) 0.3472(3) 0.069(2) Uani 1 1 d . . . E 4 C83 C 0.4010(4) 1.000000 0.5670(5) 0.061(3) Uani 1 2 d S T P E 4 H83 H 0.388275 0.999999 0.611389 0.073 Uiso 1 2 calc R U P E 4 C84 C 0.4094(3) 0.9292(6) 0.5379(4) 0.062(2) Uani 1 1 d . . . E 4 C85 C 0.3976(3) 0.8561(6) 0.5662(4) 0.069(2) Uani 1 1 d . . . E 4 C86 C 0.3725(3) 0.8481(6) 0.6320(4) 0.069(2) Uani 1 1 d . . . E 4 H86A H 0.388387 0.886371 0.673554 0.083 Uiso 1 1 calc R U . E 4 H86B H 0.379760 0.795476 0.655148 0.083 Uiso 1 1 calc R U . E 4 C87 C 0.3133(3) 0.8609(6) 0.6035(5) 0.074(2) Uani 1 1 d . . . E 4 H87A H 0.305800 0.912233 0.579046 0.111 Uiso 1 1 calc R U . E 4 H87B H 0.298996 0.857796 0.648148 0.111 Uiso 1 1 calc R U . E 4 H87C H 0.297024 0.820732 0.565044 0.111 Uiso 1 1 calc R U . E 4 C88 C 0.4109(3) 0.8000(6) 0.5232(4) 0.075(3) Uani 1 1 d . . . E 4 C89 C 0.4047(5) 0.7140(7) 0.5278(6) 0.108(4) Uani 1 1 d . . . E 4 H89A H 0.405830 0.699832 0.582057 0.129 Uiso 1 1 calc R U . E 4 H89B H 0.434549 0.688085 0.515799 0.129 Uiso 1 1 calc R U . E 4 C90 C 0.3542(7) 0.6841(7) 0.4721(7) 0.127(5) Uani 1 1 d . . . E 4 H90A H 0.353323 0.696084 0.418003 0.190 Uiso 1 1 calc R U . E 4 H90B H 0.324372 0.709043 0.483869 0.190 Uiso 1 1 calc R U . E 4 H90C H 0.352051 0.627656 0.478188 0.190 Uiso 1 1 calc R U . E 4 C91 C 0.4315(3) 0.8397(6) 0.4666(4) 0.074(3) Uani 1 1 d . . . E 4 C92 C 0.4482(3) 0.8022(6) 0.4111(4) 0.079(3) Uani 1 1 d . . . E 4 H92 H 0.448277 0.746995 0.411345 0.095 Uiso 1 1 calc R U . E 4 C93 C 0.4651(3) 0.8396(7) 0.3544(4) 0.076(3) Uani 1 1 d . . . E 4 C94 C 0.4805(3) 0.7994(7) 0.2936(4) 0.084(3) Uani 1 1 d . . . E 4 C95 C 0.4796(5) 0.7125(8) 0.2838(6) 0.120(5) Uani 1 1 d . . . E 4 H95A H 0.493564 0.688047 0.336067 0.143 Uiso 1 1 calc R U . E 4 H95B H 0.502959 0.698003 0.252075 0.143 Uiso 1 1 calc R U . E 4 C96 C 0.4248(6) 0.6804(7) 0.2444(7) 0.118(4) Uani 1 1 d . . . E 4 H96A H 0.408053 0.711118 0.197558 0.177 Uiso 1 1 calc R U . E 4 H96B H 0.403810 0.683253 0.281073 0.177 Uiso 1 1 calc R U . E 4 H96C H 0.427551 0.626076 0.229430 0.177 Uiso 1 1 calc R U . E 4 C97 C 0.4937(3) 0.8552(7) 0.2498(4) 0.080(3) Uani 1 1 d . . . E 4 C98 C 0.5115(3) 0.8433(7) 0.1773(4) 0.094(4) Uani 1 1 d . . . E 4 H98A H 0.531633 0.794260 0.182783 0.113 Uiso 1 1 calc R U . E 4 H98B H 0.535135 0.886420 0.173282 0.113 Uiso 1 1 calc R U . E 4 C99 C 0.4658(4) 0.8401(8) 0.1022(5) 0.108(4) Uani 1 1 d . . . E 4 H99A H 0.478305 0.821821 0.058900 0.161 Uiso 1 1 calc R U . E 4 H99B H 0.450565 0.892063 0.090106 0.161 Uiso 1 1 calc R U . E 4 H99C H 0.439047 0.804215 0.109504 0.161 Uiso 1 1 calc R U . E 4 C100 C 0.4862(3) 0.9296(6) 0.2826(4) 0.068(2) Uani 1 1 d . . . E 4 C101 C 0.4952(4) 1.000000 0.2535(5) 0.072(4) Uani 1 2 d S T P E 4 H101 H 0.508624 1.000000 0.209731 0.087 Uiso 1 2 calc R U P E 4 C102 C 0.2945(8) 0.500000 0.2613(11) 0.114(6) Uani 1 2 d S T P F 4 C103 C 0.1574(6) 0.500000 0.2056(9) 0.090(4) Uani 1 2 d S T P G 4 H103 H 0.177463 0.500000 0.259262 0.108 Uiso 1 2 calc R U P G 4 C104 C 0.1430(4) 0.4319(5) 0.1672(6) 0.087(3) Uani 1 1 d . . . G 4 H104 H 0.155754 0.384260 0.192576 0.105 Uiso 1 1 calc R U . G 4 C105 C 0.1105(5) 0.4312(6) 0.0927(5) 0.087(3) Uani 1 1 d . . . G 4 H105 H 0.099706 0.383424 0.066215 0.104 Uiso 1 1 calc R U . G 4 C106 C 0.0936(6) 0.500000 0.0568(7) 0.083(4) Uani 1 2 d S T P G 4 H106 H 0.069598 0.500001 0.005550 0.099 Uiso 1 2 calc R U P G 4 C107 C 0.0068(19) 1.000000 0.5817(19) 0.168(12) Uani 1 2 d DS T P H 4 H107 H 0.011421 1.000000 0.636562 0.202 Uiso 1 2 calc R U P H 4 C108 C 0.0489(10) 1.000000 0.551(2) 0.166(10) Uani 1 2 d DS T P H 4 H108 H 0.083757 1.000000 0.584954 0.199 Uiso 1 2 calc R U P H 4 C109 C 0.0401(17) 1.000000 0.470(2) 0.161(12) Uani 1 2 d DS T P H 4 H109 H 0.069701 1.000000 0.450765 0.193 Uiso 1 2 calc R U P H 4 N1 N 0.4301(2) 0.9193(5) 0.4755(3) 0.0634(19) Uani 1 1 d . . . E 4 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 Y3 0.112(9) 0.121(19) 0.26(2) 0.000(10) 0.117(12) -0.022(8) Y4 0.041(5) 0.036(7) 0.032(4) 0.027(4) 0.031(4) 0.027(5) Y2 0.071(3) 0.060(3) 0.170(6) -0.004(4) -0.006(4) 0.036(2) C1 0.148(14) 0.273(16) 0.076(10) 0.000 -0.021(11) 0.000 C43 0.087(9) 0.102(17) 0.163(12) 0.034(11) 0.101(9) 0.030(9) C2 0.107(9) 0.182(10) 0.117(8) 0.039(8) 0.018(7) -0.004(8) C3 0.074(10) 0.140(13) 0.069(10) -0.028(10) 0.005(8) -0.060(10) C4 0.113(13) 0.165(15) 0.067(10) -0.058(11) 0.004(10) -0.077(12) C5 0.140(13) 0.186(15) 0.052(9) -0.047(10) 0.054(9) -0.069(12) C6 0.193(16) 0.272(17) 0.058(8) -0.003(16) 0.028(12) -0.035(16) C7 0.186(15) 0.209(17) 0.040(8) 0.006(10) 0.052(11) -0.069(14) C8 0.169(10) 0.171(10) 0.118(9) 0.008(8) 0.090(8) -0.036(8) C9 0.181(16) 0.156(15) 0.131(15) 0.048(14) 0.018(15) 0.001(15) C10 0.107(9) 0.182(10) 0.117(8) 0.039(8) 0.018(7) -0.004(8) C11 0.089(12) 0.157(16) 0.145(15) 0.039(13) -0.062(12) 0.026(13) C12 0.075(9) 0.169(15) 0.146(13) 0.030(17) -0.034(10) 0.008(16) C13 0.056(9) 0.163(16) 0.177(16) 0.029(14) -0.023(13) -0.023(11) C14 0.063(11) 0.142(15) 0.155(15) -0.015(14) 0.030(12) -0.059(11) C15 0.092(12) 0.147(15) 0.120(14) -0.049(13) 0.002(11) -0.061(13) C16 0.106(12) 0.076(13) 0.128(13) -0.055(10) 0.036(11) -0.056(10) C17 0.132(13) 0.100(13) 0.119(13) -0.037(12) 0.043(12) -0.025(12) C18 0.121(13) 0.144(14) 0.104(12) -0.085(11) 0.031(11) 0.008(12) C19 0.164(15) 0.167(15) 0.108(12) -0.069(12) 0.070(12) -0.002(13) C20 0.169(10) 0.171(10) 0.118(9) 0.008(8) 0.090(8) -0.036(8) C21 0.179(15) 0.206(17) 0.116(14) -0.011(14) 0.099(13) 0.002(15) C22 0.206(15) 0.181(19) 0.091(11) 0.016(13) 0.108(11) -0.011(15) C23 0.149(16) 0.208(16) 0.108(14) 0.033(13) 0.102(12) -0.031(14) C24 0.169(10) 0.171(10) 0.118(9) 0.008(8) 0.090(8) -0.036(8) C25 0.181(15) 0.113(13) 0.190(16) 0.049(13) 0.062(15) -0.074(13) C26 0.136(14) 0.044(10) 0.175(16) 0.054(11) 0.081(13) 0.021(10) C27 0.155(14) 0.056(10) 0.125(14) 0.059(10) 0.048(12) 0.024(11) C28 0.130(15) 0.062(13) 0.193(17) 0.052(13) 0.023(14) 0.038(12) C29 0.078(12) 0.116(14) 0.177(17) 0.083(13) -0.004(14) 0.043(12) C30 0.049(9) 0.126(15) 0.178(16) 0.047(14) 0.005(12) 0.041(11) C31 0.045(7) 0.154(16) 0.191(15) 0.048(14) 0.025(11) 0.006(12) C32 0.063(8) 0.147(14) 0.201(14) 0.049(14) 0.079(9) 0.009(13) C33 0.132(13) 0.129(14) 0.177(14) 0.012(13) 0.121(11) -0.056(12) C34 0.114(12) 0.080(11) 0.114(12) -0.016(10) 0.078(10) -0.062(10) C35 0.132(13) 0.063(12) 0.114(12) -0.040(10) 0.065(11) -0.058(10) C36 0.157(15) 0.069(11) 0.132(13) 0.013(11) 0.055(12) -0.028(12) C37 0.124(12) 0.040(9) 0.129(12) 0.011(9) 0.082(10) -0.008(9) C38 0.083(10) 0.038(9) 0.134(13) -0.015(9) 0.025(10) 0.016(8) C39 0.091(10) 0.043(9) 0.118(12) -0.013(9) 0.050(9) 0.025(8) C40 0.104(12) 0.122(14) 0.121(12) -0.054(12) 0.044(11) 0.054(11) C41 0.109(12) 0.116(14) 0.132(13) -0.017(12) 0.087(11) 0.042(11) C42 0.119(14) 0.173(16) 0.132(15) 0.002(13) 0.102(12) 0.042(12) C44 0.133(14) 0.173(17) 0.172(15) 0.047(14) 0.096(13) -0.023(14) C45 0.132(15) 0.143(16) 0.183(17) 0.050(15) 0.066(15) -0.064(13) C46 0.168(16) 0.100(14) 0.205(17) 0.057(15) 0.062(15) -0.077(12) C47 0.163(17) 0.086(15) 0.208(18) -0.006(17) 0.048(17) -0.061(15) C48 0.195(18) 0.086(14) 0.234(19) -0.014(16) 0.034(18) -0.004(16) C49 0.174(17) 0.055(12) 0.228(18) 0.024(15) 0.014(17) 0.024(14) C50 0.134(14) 0.045(11) 0.210(17) 0.016(13) 0.076(15) 0.033(12) C51 0.143(15) 0.095(14) 0.209(17) -0.042(14) 0.079(14) 0.054(12) C52 0.107(13) 0.130(16) 0.192(17) 0.013(15) 0.071(14) 0.046(12) C53 0.107(9) 0.182(10) 0.117(8) 0.039(8) 0.018(7) -0.004(8) C54 0.190(15) 0.179(16) 0.137(14) 0.009(13) 0.136(11) -0.024(14) C55 0.189(14) 0.157(17) 0.108(12) -0.022(11) 0.119(11) -0.005(13) C56 0.156(14) 0.115(13) 0.137(14) 0.017(12) 0.105(12) -0.046(12) C57 0.190(15) 0.086(13) 0.081(10) 0.001(10) 0.103(10) -0.019(12) C58 0.165(14) 0.129(14) 0.096(12) 0.043(11) 0.088(11) 0.038(13) C59 0.153(14) 0.110(14) 0.090(11) 0.065(11) 0.055(11) 0.039(12) C60 0.150(13) 0.040(9) 0.085(10) 0.008(8) 0.047(10) 0.038(9) C61 0.089(11) 0.037(9) 0.120(12) 0.016(10) 0.015(10) 0.031(9) C62 0.058(9) 0.062(10) 0.121(13) 0.026(10) -0.005(9) 0.028(8) C63 0.041(9) 0.102(13) 0.138(14) -0.007(13) 0.040(11) 0.016(9) C64 0.054(8) 0.089(10) 0.118(12) -0.005(9) 0.053(9) 0.001(7) C65 0.038(6) 0.079(13) 0.122(11) -0.012(9) 0.017(8) -0.012(7) C66 0.073(11) 0.094(13) 0.137(14) 0.015(13) 0.010(13) -0.041(10) C67 0.126(15) 0.130(16) 0.156(16) -0.026(15) -0.012(15) -0.071(14) C68 0.164(17) 0.129(16) 0.177(17) -0.046(15) 0.021(16) -0.079(14) C69 0.198(18) 0.112(15) 0.158(18) -0.100(13) 0.022(15) -0.045(14) C70 0.196(17) 0.092(14) 0.184(17) -0.081(13) 0.056(16) 0.020(14) C71 0.221(18) 0.109(16) 0.180(18) -0.063(15) 0.086(16) 0.032(16) C72 0.224(17) 0.166(17) 0.152(16) -0.056(14) 0.114(14) -0.008(16) C73 0.213(17) 0.151(16) 0.089(11) -0.053(11) 0.109(12) -0.025(14) C74 0.244(16) 0.197(17) 0.103(11) -0.001(16) 0.099(12) 0.004(18) C75 0.155(15) 0.201(16) 0.069(10) 0.073(12) 0.060(12) 0.050(14) C76 0.130(14) 0.167(14) 0.062(10) 0.065(11) -0.037(11) 0.004(13) C77 0.081(11) 0.090(11) 0.098(11) 0.057(10) -0.029(9) 0.021(10) C78 0.080(11) 0.094(13) 0.127(14) 0.025(12) -0.039(11) 0.047(11) C79 0.043(6) 0.083(13) 0.093(9) 0.013(10) -0.006(6) -0.024(9) C80 0.110(14) 0.143(15) 0.116(15) -0.020(13) -0.033(12) -0.024(13) C81 0.143(15) 0.165(15) 0.088(13) -0.014(15) -0.042(13) -0.006(14) C82 0.200(17) 0.110(15) 0.094(13) -0.058(12) 0.006(14) -0.024(14) Ni1 0.0358(7) 0.1274(14) 0.0228(6) 0.000 0.0131(4) 0.000 S1 0.209(5) 0.116(3) 0.232(6) -0.031(3) 0.101(5) -0.036(3) N2 0.041(3) 0.142(7) 0.027(3) 0.010(3) 0.013(2) 0.025(4) C83 0.040(5) 0.121(10) 0.026(4) 0.000 0.017(4) 0.000 C84 0.041(3) 0.121(7) 0.028(3) 0.012(4) 0.016(3) 0.023(4) C85 0.060(4) 0.120(7) 0.033(3) 0.025(4) 0.022(3) 0.033(5) C86 0.070(5) 0.104(7) 0.042(4) 0.016(4) 0.030(3) 0.027(5) C87 0.066(5) 0.112(7) 0.056(4) 0.016(4) 0.035(4) 0.012(5) C88 0.077(5) 0.111(7) 0.045(4) 0.029(4) 0.031(4) 0.049(5) C89 0.157(11) 0.128(10) 0.062(5) 0.051(6) 0.069(7) 0.085(8) C90 0.206(15) 0.104(9) 0.090(8) 0.040(7) 0.073(10) 0.062(10) C91 0.065(5) 0.124(8) 0.038(4) 0.029(4) 0.025(3) 0.051(5) C92 0.081(5) 0.124(8) 0.043(4) 0.024(4) 0.034(4) 0.054(5) C93 0.054(4) 0.142(9) 0.035(4) 0.021(5) 0.017(3) 0.045(5) C94 0.067(5) 0.149(9) 0.041(4) 0.017(5) 0.026(4) 0.062(6) C95 0.141(10) 0.167(12) 0.074(6) 0.045(7) 0.066(7) 0.112(10) C96 0.171(13) 0.093(8) 0.090(7) 0.003(6) 0.036(8) 0.057(8) C97 0.050(4) 0.160(9) 0.035(3) 0.016(5) 0.022(3) 0.047(5) C98 0.073(5) 0.178(11) 0.041(4) 0.017(5) 0.032(4) 0.058(6) C99 0.104(7) 0.187(12) 0.037(4) 0.002(6) 0.030(4) 0.031(8) C100 0.038(3) 0.141(8) 0.030(3) 0.006(4) 0.017(3) 0.021(4) C101 0.040(5) 0.155(13) 0.028(4) 0.000 0.018(4) 0.000 C102 0.162(17) 0.065(10) 0.115(13) 0.000 0.041(12) 0.000 C103 0.094(10) 0.081(10) 0.076(8) 0.000 -0.004(7) 0.000 C104 0.110(7) 0.053(5) 0.089(7) 0.009(5) 0.014(6) 0.006(5) C105 0.130(8) 0.076(6) 0.061(5) -0.003(5) 0.037(5) -0.028(6) C106 0.101(10) 0.097(11) 0.047(6) 0.000 0.017(6) 0.000 C107 0.24(3) 0.14(2) 0.15(2) 0.000 0.10(3) 0.000 C108 0.120(18) 0.18(2) 0.18(3) 0.000 0.017(18) 0.000 C109 0.23(3) 0.099(15) 0.22(3) 0.000 0.17(3) 0.000 N1 0.039(3) 0.131(6) 0.025(2) 0.012(3) 0.016(2) 0.023(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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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 C6 C1 C2 124.9(19) . . C6 C1 C10 109(2) . . C2 C1 C10 117(3) . . C64 C43 C42 108.0(10) . . C64 C43 C44 100.4(18) . . C42 C43 C44 139(2) . . C12 C2 C1 101(2) . . C12 C2 C3 119(3) . . C1 C2 C3 129(3) . . C4 C3 C15 132(3) . . C4 C3 C2 106(2) . . C15 C3 C2 113(3) . . C3 C4 C18 126(2) . . C3 C4 C5 122(3) . . C18 C4 C5 103.7(16) . . C6 C5 C20 108.1(17) . . C6 C5 C4 135(2) . . C20 C5 C4 110.8(16) . . C1 C6 C5 102.6(19) . . C1 C6 C7 125(2) . . C5 C6 C7 126(2) . . C6 C7 C22 117.6(19) . . C6 C7 C8 123(2) . . C22 C7 C8 105.8(15) . . C9 C8 C24 131(3) . . C9 C8 C7 118(2) . . C24 C8 C7 106.2(16) . . C27 C9 C10 120.4(17) . . C27 C9 C8 122(3) . . C10 C9 C8 109(2) . . C9 C10 C11 114.5(19) . . C9 C10 C1 134(3) . . C11 C10 C1 98(2) . . C29 C11 C12 115(2) . . C29 C11 C10 125.6(18) . . C12 C11 C10 110.9(18) . . C11 C12 C13 126(3) . . C11 C12 C2 114(2) . . C13 C12 C2 116(3) . . C12 C13 C14 126(3) . . C12 C13 C31 115(2) . . C14 C13 C31 112(2) . . C34 C14 C15 111.9(17) . . C34 C14 C13 126(2) . . C15 C14 C13 107(2) . . C3 C15 C16 110(3) . . C3 C15 C14 136(3) . . C16 C15 C14 103.6(17) . . C35 C16 C15 111.2(17) . . C35 C16 C17 107.4(18) . . C15 C16 C17 129(2) . . C38 C17 C16 127.3(19) . . C38 C17 C18 111(2) . . C16 C17 C18 109(3) . . C19 C18 C4 108.8(18) . . C19 C18 C17 129(2) . . C4 C18 C17 113(2) . . C18 C19 C20 111.5(18) . . C18 C19 C40 106.4(19) . . C20 C19 C40 138(2) . . C21 C20 C19 100(2) . . C21 C20 C5 128(2) . . C19 C20 C5 103.7(16) . . C20 C21 C22 113(2) . . C20 C21 C42 122(2) . . C22 C21 C42 123(3) . . C21 C22 C7 120(2) . . C21 C22 C23 120(2) . . C7 C22 C23 110.0(16) . . C24 C23 C44 115(2) . . C24 C23 C22 105.4(16) . . C44 C23 C22 128(3) . . C23 C24 C25 125(2) . . C23 C24 C8 111.7(18) . . C25 C24 C8 105(2) . . C26 C25 C46 113.9(18) . . C26 C25 C24 125(2) . . C46 C25 C24 117.9(18) . . C25 C26 C49 126.1(19) . . C25 C26 C27 127(2) . . C49 C26 C27 96.2(15) . . C28 C27 C9 122.9(17) . . C28 C27 C26 115.4(17) . . C9 C27 C26 109(2) . . C27 C28 C50 107.1(16) . . C27 C28 C29 120.5(18) . . C50 C28 C29 125(2) . . C11 C29 C28 115.8(16) . . C11 C29 C30 124(2) . . C28 C29 C30 111.3(19) . . C52 C30 C31 108.0(16) . . C52 C30 C29 128(2) . . C31 C30 C29 117(2) . . C30 C31 C32 109.2(17) . . C30 C31 C13 122(2) . . C32 C31 C13 121(2) . . C53 C32 C31 107.3(17) . . C53 C32 C33 116.9(18) . . C31 C32 C33 125(2) . . C56 C33 C34 124(2) . . C56 C33 C32 118.8(19) . . C34 C33 C32 108(2) . . C14 C34 C33 126(2) . . C14 C34 C35 106.9(15) . . C33 C34 C35 119.8(18) . . C16 C35 C36 129.9(17) . . C16 C35 C34 105.8(15) . . C36 C35 C34 118.2(15) . . C37 C36 C35 107.9(17) . . C37 C36 C57 127(2) . . C35 C36 C57 119.3(18) . . C36 C37 C38 135.8(19) . . C36 C37 C60 110.4(18) . . C38 C37 C60 101.0(13) . . C39 C38 C17 134(2) . . C39 C38 C37 112.6(15) . . C17 C38 C37 108.9(17) . . C38 C39 C61 108.8(14) . . C38 C39 C40 116.9(19) . . C61 C39 C40 125.3(16) . . C41 C40 C39 118.6(18) . . C41 C40 C19 106(2) . . C39 C40 C19 121.1(18) . . C40 C41 C42 117(2) . . C40 C41 C63 121.6(16) . . C42 C41 C63 110.8(11) . . C41 C42 C43 105.8(11) . . C41 C42 C21 134(2) . . C43 C42 C21 109(2) . . C45 C44 C23 120(2) . . C45 C44 C43 131(3) . . C23 C44 C43 99(2) . . C66 C45 C44 121(3) . . C66 C45 C46 108(3) . . C44 C45 C46 125(2) . . C45 C46 C25 114.7(19) . . C45 C46 C47 115(3) . . C25 C46 C47 116(2) . . C68 C47 C48 96.3(16) . . C68 C47 C46 129(3) . . C48 C47 C46 128(2) . . C49 C48 C70 113.1(19) . . C49 C48 C47 115(2) . . C70 C48 C47 116.1(19) . . C48 C49 C50 119.5(19) . . C48 C49 C26 119.3(18) . . C50 C49 C26 117.5(16) . . C28 C50 C49 103.0(16) . . C28 C50 C51 118(2) . . C49 C50 C51 127(2) . . C71 C51 C52 116.1(17) . . C71 C51 C50 111.8(17) . . C52 C51 C50 122(2) . . C30 C52 C51 115(2) . . C30 C52 C53 107.3(16) . . C51 C52 C53 124.2(19) . . C54 C53 C32 124(2) . . C54 C53 C52 116.0(19) . . C32 C53 C52 108.0(16) . . C53 C54 C55 118(2) . . C53 C54 C72 121.5(18) . . C55 C54 C72 114.5(17) . . C74 C55 C54 97.7(17) . . C74 C55 C56 120.3(18) . . C54 C55 C56 122(2) . . C33 C56 C57 118.6(18) . . C33 C56 C55 117.6(19) . . C57 C56 C55 116.4(17) . . C58 C57 C56 115.7(18) . . C58 C57 C36 116(2) . . C56 C57 C36 120.1(18) . . C59 C58 C57 120(2) . . C59 C58 C75 103.0(17) . . C57 C58 C75 123(2) . . C60 C59 C58 115(2) . . C60 C59 C77 117(2) . . C58 C59 C77 110.5(17) . . C59 C60 C61 114(2) . . C59 C60 C37 130.8(19) . . C61 C60 C37 109.8(14) . . C39 C61 C60 107.6(14) . . C39 C61 C62 115.8(16) . . C60 C61 C62 124(2) . . C78 C62 C61 121.7(19) . . C78 C62 C63 110.8(18) . . C61 C62 C63 120.6(15) . . C64 C63 C41 105.7(10) . . C64 C63 C62 129.1(18) . . C41 C63 C62 117.9(14) . . C63 C64 C43 109.3(10) . . C63 C64 C65 117.6(15) . . C43 C64 C65 125.3(16) . . C66 C65 C79 110.7(15) . . C66 C65 C64 130.0(19) . . C79 C65 C64 112.2(14) . . C45 C66 C65 111(2) . . C45 C66 C67 141(3) . . C65 C66 C67 101.1(16) . . C68 C67 C66 111(3) . . C68 C67 C80 116(2) . . C66 C67 C80 113.4(18) . . C67 C68 C69 117(2) . . C67 C68 C47 115(3) . . C69 C68 C47 113.6(19) . . C82 C69 C70 123(3) . . C82 C69 C68 127(2) . . C70 C69 C68 109.1(18) . . C69 C70 C71 118(3) . . C69 C70 C48 101.8(17) . . C71 C70 C48 129(2) . . C72 C71 C70 114(3) . . C72 C71 C51 118.3(19) . . C70 C71 C51 118.4(19) . . C73 C72 C71 130(2) . . C73 C72 C54 104.2(16) . . C71 C72 C54 124(2) . . C72 C73 C74 103.2(18) . . C72 C73 C82 111(2) . . C74 C73 C82 122.6(18) . . C75 C74 C55 122.0(19) . . C75 C74 C73 119.2(19) . . C55 C74 C73 116.9(17) . . C74 C75 C76 120.1(18) . . C74 C75 C58 118.9(19) . . C76 C75 C58 113.9(17) . . C81 C76 C75 119.9(19) . . C81 C76 C77 136(2) . . C75 C76 C77 102.4(16) . . C78 C77 C59 131(2) . . C78 C77 C76 108.5(19) . . C59 C77 C76 109.8(16) . . C79 C78 C77 126(2) . . C79 C78 C62 122(2) . . C77 C78 C62 109(2) . . C78 C79 C80 113(2) . . C78 C79 C65 127.9(19) . . C80 C79 C65 110.0(16) . . C79 C80 C81 134(2) . . C79 C80 C67 101.9(17) . . C81 C80 C67 123.0(19) . . C76 C81 C80 100(3) . . C76 C81 C82 121(2) . . C80 C81 C82 117(2) . . C69 C82 C73 121(3) . . C69 C82 C81 114.9(19) . . C73 C82 C81 112.8(18) . . N1 Ni1 N1 90.3(4) . 6_575 N1 Ni1 N2 89.7(3) . . N1 Ni1 N2 177.9(2) 6_575 . C93 N2 C100 104.7(7) . . C93 N2 Ni1 127.9(5) . . C100 N2 Ni1 127.4(7) . . C84 C83 H83 117.1 . . C84 C83 H83 117.1 6_575 . C83 C84 N1 124.0(8) . . C83 C84 C85 125.0(6) . . N1 C84 C85 111.0(8) . . C88 C85 C84 108.0(6) . . C88 C85 C86 128.8(9) . . C84 C85 C86 123.3(8) . . C85 C86 C87 112.2(6) . . C85 C86 H86A 109.2 . . C87 C86 H86A 109.2 . . C85 C86 H86B 109.2 . . C87 C86 H86B 109.2 . . H86A C86 H86B 107.9 . . C86 C87 H87A 109.5 . . C86 C87 H87B 109.5 . . H87A C87 H87B 109.5 . . C86 C87 H87C 109.5 . . H87A C87 H87C 109.5 . . H87B C87 H87C 109.5 . . C85 C88 C91 106.1(9) . . C85 C88 C89 128.9(8) . . C91 C88 C89 125.0(8) . . C88 C89 C90 113.1(8) . . C88 C89 H89A 108.9 . . C90 C89 H89A 108.9 . . C88 C89 H89B 108.9 . . C90 C89 H89B 108.9 . . H89A C89 H89B 107.8 . . C89 C90 H90A 109.5 . . C89 C90 H90B 109.5 . . H90A C90 H90B 109.5 . . C89 C90 H90C 109.5 . . H90A C90 H90C 109.5 . . H90B C90 H90C 109.5 . . C92 C91 N1 125.4(8) . . C92 C91 C88 123.7(10) . . N1 C91 C88 110.9(7) . . C91 C92 C93 124.0(10) . . C91 C92 H92 118.0 . . C93 C92 H92 118.0 . . N2 C93 C92 125.0(8) . . N2 C93 C94 111.5(8) . . C92 C93 C94 123.5(11) . . C97 C94 C93 105.9(10) . . C97 C94 C95 129.8(7) . . C93 C94 C95 124.4(9) . . C94 C95 C96 113.2(8) . . C94 C95 H95A 108.9 . . C96 C95 H95A 108.9 . . C94 C95 H95B 108.9 . . C96 C95 H95B 108.9 . . H95A C95 H95B 107.7 . . C95 C96 H96A 109.5 . . C95 C96 H96B 109.5 . . H96A C96 H96B 109.5 . . C95 C96 H96C 109.5 . . H96A C96 H96C 109.5 . . H96B C96 H96C 109.5 . . C94 C97 C100 107.8(6) . . C94 C97 C98 126.8(10) . . C100 C97 C98 125.4(9) . . C97 C98 C99 112.5(7) . . C97 C98 H98A 109.1 . . C99 C98 H98A 109.1 . . C97 C98 H98B 109.1 . . C99 C98 H98B 109.1 . . H98A C98 H98B 107.8 . . C98 C99 H99A 109.5 . . C98 C99 H99B 109.5 . . H99A C99 H99B 109.5 . . C98 C99 H99C 109.5 . . H99A C99 H99C 109.5 . . H99B C99 H99C 109.5 . . C101 C100 N2 125.1(9) . . C101 C100 C97 124.8(6) . . N2 C100 C97 110.1(8) . . C100 C101 C100 124.8(9) 6_575 . C100 C101 H101 117.6 6_575 . C100 C101 H101 117.6 . . S1 C102 S1 178.3(16) 6_565 . C104 C103 C104 119.7(13) 6_565 . C104 C103 H103 120.1 6_565 . C104 C103 H103 120.1 . . C103 C104 C105 120.5(10) . . C103 C104 H104 119.7 . . C105 C104 H104 119.7 . . C104 C105 C106 118.9(10) . . C104 C105 H105 120.6 . . C106 C105 H105 120.6 . . C105 C106 H106 119.4 . . C105 C106 H106 119.4 6_565 . C109 C107 C108 116(3) 5_576 . C109 C107 H107 122.1 5_576 . C108 C107 H107 122.1 . . C107 C108 C109 120(2) . . C107 C108 H108 120.0 . . C109 C108 H108 120.0 . . C107 C109 C108 124(2) 5_576 . C107 C109 H109 117.9 5_576 . C108 C109 H109 117.9 . . C91 N1 C84 104.1(7) . . C91 N1 Ni1 128.0(4) . . C84 N1 Ni1 127.9(7) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Y1 Y4 2.83(2) . C1 C6 1.25(4) . C1 C2 1.45(3) . C1 C10 1.55(3) . C43 C64 1.420(13) . C43 C42 1.432(14) . C43 C44 1.57(4) . C2 C12 1.45(2) . C2 C3 1.53(4) . C3 C4 1.20(3) . C3 C15 1.28(3) . C4 C18 1.47(2) . C4 C5 1.477(19) . C5 C6 1.43(2) . C5 C20 1.448(19) . C6 C7 1.467(19) . C7 C22 1.469(19) . C7 C8 1.50(2) . C8 C9 1.45(2) . C8 C24 1.47(2) . C9 C27 1.439(19) . C9 C10 1.44(2) . C10 C11 1.50(2) . C11 C29 1.434(19) . C11 C12 1.44(2) . C12 C13 1.45(2) . C13 C14 1.45(2) . C13 C31 1.50(2) . C14 C34 1.41(2) . C14 C15 1.44(2) . C15 C16 1.44(2) . C16 C35 1.44(2) . C16 C17 1.51(4) . C17 C38 1.35(4) . C17 C18 1.54(3) . C18 C19 1.40(2) . C19 C20 1.44(2) . C19 C40 1.76(3) . C20 C21 1.43(2) . C21 C22 1.44(2) . C21 C42 1.44(4) . C22 C23 1.499(19) . C23 C24 1.42(2) . C23 C44 1.47(2) . C24 C25 1.469(19) . C25 C26 1.453(18) . C25 C46 1.46(2) . C26 C49 1.460(19) . C26 C27 1.471(19) . C27 C28 1.417(19) . C28 C50 1.43(2) . C28 C29 1.456(19) . C29 C30 1.468(19) . C30 C52 1.42(2) . C30 C31 1.44(2) . C31 C32 1.446(19) . C32 C53 1.43(2) . C32 C33 1.57(4) . C33 C56 1.36(2) . C33 C34 1.455(19) . C34 C35 1.463(19) . C35 C36 1.439(19) . C36 C37 1.26(3) . C36 C57 1.518(19) . C37 C38 1.432(19) . C37 C60 1.459(19) . C38 C39 1.340(18) . C39 C61 1.378(18) . C39 C40 1.381(18) . C40 C41 1.315(19) . C41 C42 1.401(14) . C41 C63 1.427(13) . C44 C45 1.42(2) . C45 C66 1.32(4) . C45 C46 1.45(2) . C46 C47 1.46(2) . C47 C68 1.42(2) . C47 C48 1.44(2) . C48 C49 1.377(19) . C48 C70 1.43(2) . C49 C50 1.442(19) . C50 C51 1.451(18) . C51 C71 1.446(19) . C51 C52 1.447(19) . C52 C53 1.489(19) . C53 C54 1.340(19) . C54 C55 1.404(19) . C54 C72 1.441(19) . C55 C74 1.367(19) . C55 C56 1.50(2) . C56 C57 1.450(19) . C57 C58 1.41(3) . C58 C59 1.395(19) . C58 C75 1.42(2) . C59 C60 1.35(3) . C59 C77 1.40(2) . C60 C61 1.395(18) . C61 C62 1.399(18) . C62 C78 1.388(19) . C62 C63 1.429(18) . C63 C64 1.404(13) . C64 C65 1.43(2) . C65 C66 1.397(19) . C65 C79 1.424(17) . C66 C67 1.43(2) . C67 C68 1.38(2) . C67 C80 1.43(2) . C68 C69 1.39(2) . C69 C82 1.363(19) . C69 C70 1.37(2) . C70 C71 1.42(2) . C71 C72 1.403(19) . C72 C73 1.38(2) . C73 C74 1.413(19) . C73 C82 1.430(19) . C74 C75 1.321(19) . C75 C76 1.415(19) . C76 C81 1.378(19) . C76 C77 1.421(19) . C77 C78 1.38(2) . C78 C79 1.362(19) . C79 C80 1.385(19) . C80 C81 1.39(2) . C81 C82 1.441(19) . Ni1 N1 1.959(7) . Ni1 N1 1.959(7) 6_575 Ni1 N2 1.964(7) . Ni1 N2 1.964(7) 6_575 S1 C102 1.512(5) . N2 C93 1.378(13) . N2 C100 1.381(8) . C83 C84 1.368(9) . C83 C84 1.368(9) 6_575 C83 H83 0.9500 . C84 N1 1.390(7) . C84 C85 1.425(13) . C85 C88 1.344(12) . C85 C86 1.519(9) . C86 C87 1.527(11) . C86 H86A 0.9900 . C86 H86B 0.9900 . C87 H87A 0.9800 . C87 H87B 0.9800 . C87 H87C 0.9800 . C88 C91 1.455(11) . C88 C89 1.494(16) . C89 C90 1.512(19) . C89 H89A 0.9900 . C89 H89B 0.9900 . C90 H90A 0.9800 . C90 H90B 0.9800 . C90 H90C 0.9800 . C91 C92 1.362(11) . C91 N1 1.381(12) . C92 C93 1.382(12) . C92 H92 0.9500 . C93 C94 1.445(11) . C94 C97 1.347(14) . C94 C95 1.504(18) . C95 C96 1.527(19) . C95 H95A 0.9900 . C95 H95B 0.9900 . C96 H96A 0.9800 . C96 H96B 0.9800 . C96 H96C 0.9800 . C97 C100 1.446(14) . C97 C98 1.518(9) . C98 C99 1.525(12) . C98 H98A 0.9900 . C98 H98B 0.9900 . C99 H99A 0.9800 . C99 H99B 0.9800 . C99 H99C 0.9800 . C100 C101 1.367(10) . C101 H101 0.9500 . C103 C104 1.355(12) 6_565 C103 C104 1.355(12) . C103 H103 0.9500 . C104 C105 1.356(13) . C104 H104 0.9500 . C105 C106 1.359(12) . C105 H105 0.9500 . C106 H106 0.9500 . C107 C109 1.32(3) 5_576 C107 C108 1.391(10) . C107 H107 0.9500 . C108 C109 1.392(10) . C108 H108 0.9500 . C109 H109 0.9500 .