#------------------------------------------------------------------------------ #$Date: 2021-06-05 20:56:44 +0300 (Sat, 05 Jun 2021) $ #$Revision: 265922 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/06/1560621.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_1560621 loop_ _publ_author_name 'Miyagawa, Kazuya' 'Hisaki, Ichiro' 'Fukui, Norihito' 'Shinokubo, Hiroshi' _publ_section_title ; Redox-induced reversible [2 + 2] cycloaddition of an etheno-fused diporphyrin ; _journal_issue 14 _journal_name_full 'Chemical Science' _journal_page_first 5224 _journal_page_last 5229 _journal_paper_doi 10.1039/D1SC00438G _journal_volume 12 _journal_year 2021 _chemical_formula_sum 'C56.08 H50 Cl12.16 N4 Ni Sb' _chemical_formula_weight 1391.33 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-01-13 deposited with the CCDC. 2021-02-24 downloaded from the CCDC. ; _cell_angle_alpha 114.680(3) _cell_angle_beta 94.469(2) _cell_angle_gamma 98.787(2) _cell_formula_units_Z 2 _cell_length_a 9.2156(2) _cell_length_b 20.0257(6) _cell_length_c 21.5606(6) _cell_measurement_reflns_used 9568 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 29.1480 _cell_measurement_theta_min 2.1140 _cell_volume 3528.32(19) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'RIGAKU CrystalClear' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Yadokari-XG 2009(Wakita Nemoto et al.)' _computing_publication_material 'Yadokari-XG 2009(Wakita,Nemoto et al.)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 93(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Rigaku VariMax Saturn' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator Confocal _diffrn_radiation_source 'rotating-anode X-ray tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_unetI/netI 0.0431 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 32830 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.000 _diffrn_reflns_theta_min 1.861 _exptl_absorpt_coefficient_mu 1.144 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.85358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.310 _exptl_crystal_description prism _exptl_crystal_F_000 1400 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _refine_diff_density_max 3.098 _refine_diff_density_min -1.877 _refine_diff_density_rms 0.291 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 811 _refine_ls_number_reflns 13791 _refine_ls_number_restraints 1253 _refine_ls_restrained_S_all 1.119 _refine_ls_R_factor_all 0.2397 _refine_ls_R_factor_gt 0.1965 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.5000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.5232 _refine_ls_wR_factor_ref 0.5915 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8266 _reflns_number_total 13791 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc00438g2.cif _cod_data_source_block KM201214 _cod_depositor_comments 'Adding full bibliography for 1560621--1560622.cif.' _cod_original_cell_volume 3528.31(18) _cod_database_code 1560621 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; TITL --- KM201214.res created by SHELXL-2018/3 at 18:30:19 on 19-Dec-2020 REM Yadorkari-X generated CELL 0.71073 9.2156 20.0257 21.5606 114.6800 94.4690 98.7870 ZERR 2.0 0.0002 0.0006 0.0006 0.0030 0.0020 0.0020 LATT 1 REM SPGR P-1 triclinic SFAC C H N Sb Cl Ni UNIT 112.1634 100 8 1.9982 24.316 2 L.S. 50 FMAP 2 PLAN -50 ACTA CONF LIST 4 MERG 2 OMIT -10.000000 52.000000 SADI 0.01 C37 C53 C37 C38 C37 C39 SADI 0.01 C38 C53 C53 C39 C39 C38 SADI 0.01 C56 C55 C56 C57 C56 C58 SADI 0.01 C55 C58 C58 C57 C57 C55 DFIX 1.54 0.01 C37 C53 C37 C38 C37 C39 DFIX 1.54 0.01 C56 C55 C56 C57 C56 C58 DFIX 1.56 0.01 C63 C64 DFIX 1.78 0.01 C63 Cl18 C63 Cl21 C64 Cl19 C64 Cl20 DANG 3.08 0.01 Cl18 Cl21 Cl19 Cl20 DFIX 2.32 0.01 Sb3 Cl22 Sb3 Cl23 Sb3 Cl24 Sb3 Cl25 Sb3 Cl26 Sb3 Cl27 SADI 0.01 Cl22 Cl23 Cl22 Cl25 Cl22 Cl26 Cl22 Cl27 SADI 0.01 Cl24 Cl23 Cl24 Cl25 Cl24 Cl26 Cl24 Cl27 SADI 0.01 Cl23 Cl22 Cl23 Cl25 Cl23 Cl27 Cl23 Cl24 SADI 0.01 Cl26 Cl27 Cl26 Cl22 Cl26 Cl25 Cl26 Cl24 DFIX 4.64 0.01 Cl25 Cl27 DFIX 1.56 0.01 C65 C66 DFIX 1.78 0.01 C65 Cl28 C65 Cl30 C66 Cl29 C66 Cl31 DANG 3.08 0.01 Cl28 Cl30 Cl29 Cl31 DFIX 4.21 0.01 Cl28 Cl29 Cl30 Cl31 DFIX 3.1 0.01 Cl28 Cl31 Cl29 Cl30 SIMU 0.01 ISOR 0.01 SADI 0.03 Sb1 Cl1 Sb1 Cl2 Sb1 Cl3 Sb1 Cl4 Sb1 Cl5 Sb1 Cl6 SUMP 1 0.001 1 2 0.5 3 1 4 WGHT 0.500000 FVAR 1.88257 0.50083 0.51275 0.24194 C1 1 0.456510 0.393185 0.415360 11.00000 0.06012 0.04114 = 0.03853 0.01076 0.00791 0.01338 C2 1 0.481062 0.461891 0.408261 11.00000 0.06892 0.04518 = 0.04001 0.01398 0.00059 0.01202 C3 1 0.474049 0.440759 0.339720 11.00000 0.06684 0.04829 = 0.03825 0.01414 0.00873 0.01249 AFIX 43 H2 2 0.487696 0.472571 0.318309 11.00000 -1.20000 AFIX 0 C4 1 0.442724 0.362822 0.307029 11.00000 0.07160 0.05178 = 0.04020 0.01795 0.00225 0.01504 C5 1 0.434096 0.317303 0.238142 11.00000 0.08618 0.05507 = 0.04664 0.01971 0.00252 0.01645 C6 1 0.410515 0.240853 0.212847 11.00000 0.09319 0.05535 = 0.05124 0.01485 0.00267 0.01691 C7 1 0.405611 0.193691 0.140625 11.00000 0.10191 0.06497 = 0.05284 0.01659 0.00973 0.01557 AFIX 43 H3 2 0.410329 0.209285 0.105669 11.00000 -1.20000 AFIX 0 C8 1 0.393017 0.123312 0.133122 11.00000 0.10183 0.06012 = 0.05661 0.01173 0.00894 0.01957 AFIX 43 H4 2 0.393634 0.080834 0.092764 11.00000 -1.20000 AFIX 0 C9 1 0.377913 0.126711 0.201990 11.00000 0.09310 0.05367 = 0.05551 0.01205 0.00307 0.01717 C10 1 0.359363 0.063609 0.214764 11.00000 0.08984 0.05396 = 0.05572 0.01785 0.00478 0.01188 C11 1 0.341976 0.067135 0.278406 11.00000 0.08944 0.04234 = 0.05813 0.01412 0.00342 0.01480 C12 1 0.300922 0.001869 0.291124 11.00000 0.09283 0.04858 = 0.06456 0.01680 0.00998 0.01463 AFIX 43 H5 2 0.279844 -0.048168 0.258700 11.00000 -1.20000 AFIX 0 C13 1 0.299543 0.028201 0.358785 11.00000 0.09480 0.05139 = 0.06251 0.02433 0.00348 0.00708 AFIX 43 H6 2 0.280503 -0.000731 0.382702 11.00000 -1.20000 AFIX 0 C14 1 0.332527 0.109162 0.388883 11.00000 0.08160 0.04548 = 0.05936 0.01965 0.00373 0.01364 C15 1 0.342675 0.152560 0.457740 11.00000 0.08419 0.04972 = 0.05859 0.02465 0.00508 0.01413 C16 1 0.378585 0.228953 0.486479 11.00000 0.08665 0.04745 = 0.05278 0.02015 0.00357 0.01334 C17 1 0.394558 0.277223 0.558261 11.00000 0.09287 0.05613 = 0.05135 0.02628 0.00784 0.01431 AFIX 43 H7 2 0.379849 0.262078 0.593015 11.00000 -1.20000 AFIX 0 C18 1 0.433808 0.347150 0.567092 11.00000 0.08863 0.04770 = 0.05055 0.01273 0.00664 0.01346 AFIX 43 H8 2 0.455979 0.390160 0.608882 11.00000 -1.20000 AFIX 0 C19 1 0.435409 0.343576 0.500111 11.00000 0.07129 0.04451 = 0.04156 0.01295 0.00728 0.01074 C20 1 0.461037 0.404110 0.483459 11.00000 0.06745 0.04451 = 0.04334 0.01314 0.00331 0.01507 C21 1 0.493309 0.481444 0.523039 11.00000 0.06569 0.04680 = 0.04029 0.01551 0.00423 0.01296 N1 3 0.430250 0.332775 0.356117 11.00000 0.06566 0.04293 = 0.03740 0.01357 0.00328 0.00981 N2 3 0.390014 0.197949 0.248902 11.00000 0.08677 0.04662 = 0.04271 0.01328 0.00077 0.01584 N3 3 0.357796 0.131733 0.338786 11.00000 0.08680 0.04348 = 0.04954 0.01405 0.00427 0.01556 N4 3 0.404792 0.272554 0.449248 11.00000 0.07179 0.04168 = 0.04481 0.01597 0.00135 0.01105 NI1 6 0.395029 0.232901 0.347826 11.00000 0.08018 0.03481 = 0.03676 0.00636 0.00053 0.01296 AFIX 66 C22 1 0.451392 0.351568 0.189483 11.00000 0.10292 0.06570 = 0.05591 0.02559 0.00426 0.01862 C23 1 0.592332 0.367394 0.173876 11.00000 0.11641 0.07379 = 0.06737 0.02933 0.02059 0.01858 C24 1 0.611108 0.394645 0.124749 11.00000 0.13167 0.09323 = 0.08587 0.03637 0.02539 0.01244 AFIX 43 H9 2 0.705407 0.405234 0.114307 11.00000 -1.20000 AFIX 65 C25 1 0.488945 0.406069 0.091229 11.00000 0.13736 0.09470 = 0.09159 0.04357 0.01060 0.01703 C26 1 0.348004 0.390243 0.106835 11.00000 0.12847 0.08625 = 0.08345 0.04379 0.00050 0.02468 AFIX 43 H10 2 0.266269 0.397886 0.084407 11.00000 -1.20000 AFIX 65 C27 1 0.329225 0.362992 0.155962 11.00000 0.11694 0.07599 = 0.07848 0.03517 -0.00088 0.01838 AFIX 0 C28 1 0.727322 0.361150 0.208881 11.00000 0.12043 0.10737 = 0.09821 0.02105 0.05511 0.02584 AFIX 33 H16 2 0.811164 0.374793 0.189728 11.00000 -1.50000 H17 2 0.740002 0.394172 0.257298 11.00000 -1.50000 H18 2 0.719954 0.310360 0.202735 11.00000 -1.50000 AFIX 0 C29 1 0.513475 0.427896 0.034413 11.00000 0.16866 0.10483 = 0.11020 0.05996 0.01478 0.01051 AFIX 33 H19 2 0.617819 0.436393 0.031990 11.00000 -1.50000 H20 2 0.460888 0.388362 -0.008614 11.00000 -1.50000 H21 2 0.477585 0.473049 0.043112 11.00000 -1.50000 AFIX 0 C30 1 0.179419 0.350043 0.176281 11.00000 0.12989 0.10390 = 0.10195 0.05366 -0.02202 0.01642 AFIX 33 H22 2 0.186530 0.331292 0.210517 11.00000 -1.50000 H23 2 0.145398 0.396490 0.194971 11.00000 -1.50000 H24 2 0.110341 0.314051 0.136376 11.00000 -1.50000 AFIX 66 C31 1 0.356062 -0.009721 0.156492 11.00000 0.09874 0.05950 = 0.07020 0.01746 0.00859 0.01799 C32 1 0.249562 -0.040046 0.097403 11.00000 0.10111 0.07087 = 0.07367 0.01798 0.00851 0.02022 AFIX 43 H11 2 0.171457 -0.016250 0.095310 11.00000 -1.20000 AFIX 65 C33 1 0.259799 -0.105938 0.041441 11.00000 0.11076 0.08952 = 0.09295 0.01992 0.01348 0.02178 C34 1 0.376535 -0.141505 0.044568 11.00000 0.11787 0.08178 = 0.09131 0.01954 0.01433 0.03089 AFIX 43 H12 2 0.383384 -0.185591 0.007125 11.00000 -1.20000 AFIX 65 C35 1 0.483036 -0.111180 0.103657 11.00000 0.11995 0.08126 = 0.07965 0.03751 0.01774 0.03493 C36 1 0.472801 -0.045288 0.159620 11.00000 0.10399 0.06714 = 0.06531 0.02921 0.02105 0.02822 AFIX 43 H13 2 0.544057 -0.024999 0.199154 11.00000 -1.20000 AFIX 0 C37 1 0.163162 -0.127501 -0.031063 11.00000 0.12611 0.10980 = 0.10550 0.02895 0.01450 0.03280 C38 1 0.008086 -0.135755 -0.011267 11.00000 0.14470 0.14014 = 0.11744 0.04867 0.01182 0.01859 AFIX 33 H25 2 -0.000430 -0.089663 0.026285 11.00000 -1.50000 H26 2 -0.065265 -0.147126 -0.050310 11.00000 -1.50000 H27 2 -0.007501 -0.175661 0.002663 11.00000 -1.50000 AFIX 0 C39 1 0.175576 -0.201174 -0.090884 11.00000 0.15168 0.14549 = 0.12361 0.02457 0.00724 0.04494 AFIX 33 H28 2 0.272843 -0.196353 -0.103579 11.00000 -1.50000 H29 2 0.159720 -0.240976 -0.076826 11.00000 -1.50000 H30 2 0.101957 -0.212441 -0.129799 11.00000 -1.50000 AFIX 66 C44 1 0.325446 0.118072 0.505526 11.00000 0.09736 0.05669 = 0.06380 0.03405 0.00459 0.01396 C45 1 0.445615 0.101428 0.535362 11.00000 0.10194 0.06605 = 0.07330 0.03897 0.00570 0.01166 C46 1 0.425040 0.070038 0.581432 11.00000 0.11363 0.07798 = 0.08312 0.03871 -0.00665 0.01867 AFIX 43 H14 2 0.505441 0.058903 0.601394 11.00000 -1.20000 AFIX 65 C47 1 0.284296 0.055292 0.597667 11.00000 0.12111 0.08497 = 0.07913 0.04746 0.00053 0.01925 C48 1 0.164126 0.071936 0.567832 11.00000 0.11151 0.08937 = 0.08519 0.04441 0.01351 0.01334 AFIX 43 H15 2 0.069959 0.062070 0.578695 11.00000 -1.20000 AFIX 65 C49 1 0.184699 0.103325 0.521762 11.00000 0.10467 0.07276 = 0.07418 0.04115 0.01076 0.01381 AFIX 0 C50 1 0.596759 0.118739 0.519546 11.00000 0.11953 0.09775 = 0.10510 0.06238 0.00553 0.03324 AFIX 33 H31 2 0.666176 0.103769 0.544249 11.00000 -1.50000 H32 2 0.596628 0.091940 0.470788 11.00000 -1.50000 H33 2 0.625259 0.171706 0.533368 11.00000 -1.50000 AFIX 0 C51 1 0.270982 0.024555 0.649202 11.00000 0.15729 0.11278 = 0.09256 0.06330 0.00669 0.01789 AFIX 33 H34 2 0.169175 0.016799 0.655986 11.00000 -1.50000 H35 2 0.303218 -0.022404 0.632744 11.00000 -1.50000 H36 2 0.331930 0.059365 0.692246 11.00000 -1.50000 AFIX 0 C52 1 0.051606 0.121332 0.489619 11.00000 0.12372 0.08748 = 0.11008 0.05620 0.02383 0.01762 AFIX 33 H37 2 0.083314 0.142552 0.459177 11.00000 -1.50000 H38 2 -0.021962 0.076106 0.463941 11.00000 -1.50000 H39 2 0.009689 0.156674 0.525506 11.00000 -1.50000 AFIX 0 C58 1 0.634674 -0.207331 0.038267 11.00000 0.14748 0.13133 = 0.11531 0.02472 0.02916 0.06786 AFIX 33 H40 2 0.651240 -0.185365 0.006809 11.00000 -1.50000 H41 2 0.716359 -0.230286 0.043025 11.00000 -1.50000 H42 2 0.544200 -0.244673 0.020676 11.00000 -1.50000 AFIX 0 C55 1 0.767945 -0.086791 0.137601 11.00000 0.15109 0.12292 = 0.09148 0.03664 0.01481 0.03903 AFIX 33 H43 2 0.760223 -0.048444 0.181894 11.00000 -1.50000 H44 2 0.848849 -0.110181 0.142444 11.00000 -1.50000 H45 2 0.785715 -0.064740 0.106291 11.00000 -1.50000 AFIX 0 C56 1 0.622245 -0.146073 0.109047 11.00000 0.14090 0.10947 = 0.09984 0.03680 0.01497 0.04209 C57 1 0.595717 -0.181100 0.159513 11.00000 0.15837 0.13653 = 0.12338 0.05075 0.00784 0.04292 AFIX 33 H46 2 0.587966 -0.142702 0.203772 11.00000 -1.50000 H47 2 0.505228 -0.218431 0.141970 11.00000 -1.50000 H48 2 0.677387 -0.204045 0.164319 11.00000 -1.50000 AFIX 0 C53 1 0.184451 -0.065481 -0.055526 11.00000 0.16355 0.13963 = 0.11482 0.05144 0.01276 0.02282 AFIX 33 H49 2 0.281702 -0.059893 -0.068088 11.00000 -1.50000 H50 2 0.110584 -0.078669 -0.094900 11.00000 -1.50000 H51 2 0.174403 -0.019024 -0.018916 11.00000 -1.50000 PART 1 AFIX 0 SB1 4 0.887409 0.221097 0.339274 21.00000 0.08823 0.13026 = 0.11809 0.07953 0.01229 0.02516 CL1 5 0.777886 0.327099 0.373761 21.00000 0.12272 0.16752 = 0.12421 0.08108 0.01972 0.06599 CL2 5 1.054261 0.265244 0.283250 21.00000 0.07720 0.16457 = 0.11455 0.10166 0.01655 0.00097 CL3 5 1.061147 0.281626 0.441674 21.00000 0.09637 0.13160 = 0.14408 0.07642 -0.01147 0.03065 CL4 5 0.985288 0.110745 0.300787 21.00000 0.10151 0.11804 = 0.12615 0.08081 0.02712 0.04384 CL5 5 0.728197 0.165673 0.235437 21.00000 0.08701 0.11909 = 0.08636 0.04888 -0.00019 0.02605 CL6 5 0.731541 0.173896 0.390857 21.00000 0.12441 0.13518 = 0.11265 0.07788 0.01131 0.02857 PART 2 SB2 4 0.000000 0.500000 0.000000 30.50000 0.17809 0.14229 = 0.07823 0.04299 -0.04633 -0.00410 CL11 5 0.222856 0.562472 0.076317 31.00000 0.17953 0.18574 = 0.14803 0.03711 -0.04459 0.01289 CL12 5 -0.034812 0.402108 0.026011 31.00000 0.21789 0.24953 = 0.23900 0.11744 0.01251 0.07335 CL13 5 -0.134784 0.589209 0.060097 31.00000 0.24925 0.28923 = 0.27321 0.07079 -0.01119 0.02407 PART 1 CL7 5 1.635372 0.739819 0.279517 21.00000 0.15092 0.05428 = 0.04498 0.02349 0.01251 0.00365 CL8 5 1.671611 0.577727 0.263409 21.00000 0.15517 0.06039 = 0.05623 0.02174 0.03195 0.02894 CL9 5 1.372732 0.598448 0.263465 21.00000 0.10389 0.13001 = 0.05146 0.03320 -0.00965 -0.00643 CL10 5 1.691952 0.640839 0.147353 21.00000 0.18023 0.10150 = 0.06828 0.03807 0.02857 0.02041 C59 1 1.513996 0.592631 0.215286 21.00000 0.10229 0.08025 = 0.06538 0.03489 0.01207 0.00858 C60 1 1.547255 0.656907 0.205875 21.00000 0.10799 0.08195 = 0.06410 0.03369 0.01119 0.01527 CL18 5 0.311736 -0.197706 0.272424 31.00000 0.13114 0.12159 = 0.17961 0.07528 0.02862 0.03648 CL19 5 0.000548 -0.141706 0.282550 31.00000 0.13935 0.13689 = 0.16950 0.04513 0.04546 0.03962 CL20 5 0.119858 -0.198230 0.145361 31.00000 0.20733 0.12974 = 0.12800 0.04855 0.00696 0.01943 CL21 5 0.039642 -0.299518 0.282304 31.00000 0.18560 0.17851 = 0.18868 0.09446 0.03163 0.00625 C63 1 0.139396 -0.262304 0.232205 31.00000 0.16404 0.15431 = 0.17014 0.06753 0.02339 0.02952 C64 1 0.038027 -0.218266 0.209358 31.00000 0.16329 0.15065 = 0.16433 0.06078 0.02147 0.03189 PART 3 SB3 4 0.980495 0.457966 0.545056 41.00000 0.09830 0.21399 = 0.17349 0.08140 0.01390 0.04743 CL22 5 1.138152 0.444925 0.627327 41.00000 0.17294 0.20560 = 0.20156 0.07861 0.02576 0.03740 CL23 5 0.868109 0.535601 0.632259 41.00000 0.16132 0.23652 = 0.21106 0.05293 0.00269 0.08690 CL24 5 0.826065 0.471617 0.463270 41.00000 0.16414 0.18197 = 0.17942 0.07294 0.02319 0.04453 CL25 5 0.811139 0.354202 0.533809 41.00000 0.16217 0.21402 = 0.19308 0.07694 0.02126 0.00016 CL26 5 1.096133 0.380925 0.458644 41.00000 0.13756 0.16979 = 0.17300 0.03806 0.01974 0.01253 CL27 5 1.152909 0.562271 0.556934 41.00000 0.13576 0.15929 = 0.15998 0.06258 0.01721 0.04122 PART 2 CL28 5 1.179556 0.481461 0.587857 31.00000 0.15140 0.17996 = 0.18316 0.07143 0.02767 0.04054 CL29 5 0.763734 0.358317 0.581159 31.00000 0.16092 0.23095 = 0.18074 0.07499 0.02344 -0.02426 CL30 5 0.866623 0.514378 0.581970 31.00000 0.15775 0.23971 = 0.22119 0.04964 0.00551 0.06938 C65 1 0.983279 0.447068 0.563374 31.00000 0.15294 0.20448 = 0.18665 0.07873 0.02158 0.03891 CL31 5 1.069296 0.392768 0.669266 31.00000 0.25704 0.25934 = 0.24520 0.09113 0.02936 0.03300 C66 1 0.960087 0.390844 0.596342 31.00000 0.17509 0.20467 = 0.19287 0.08217 0.02427 0.02825 PART 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM --- REM wR2 = 0.5915, GooF = S = 1.104, Restrained GooF = 1.119 for all data REM R1 = 0.1965 for 8266 Fo > 4sig(Fo) and 0.2397 for all 13791 data REM 811 parameters refined using 1253 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 3.098, deepest hole -1.877, 1-sigma level 0.291 Q1 1 0.9836 0.4601 0.7024 11.00000 0.05 2.81 Q2 1 -0.0401 0.4900 0.0994 11.00000 0.05 1.85 Q3 1 1.5336 0.7386 0.2783 11.00000 0.05 1.77 Q4 1 0.4132 0.6233 0.1430 11.00000 0.05 1.54 Q5 1 0.9008 0.2775 0.3864 11.00000 0.05 1.53 Q6 1 0.8365 0.4861 0.6335 11.00000 0.05 1.46 Q7 1 0.9571 0.4084 0.5123 11.00000 0.05 1.43 Q8 1 0.8367 0.3220 0.5882 11.00000 0.05 1.36 Q9 1 0.4250 0.3939 0.1011 11.00000 0.05 1.27 Q10 1 1.1144 0.3653 0.5858 11.00000 0.05 1.27 Q11 1 0.2210 0.0702 0.5990 11.00000 0.05 1.27 Q12 1 0.2665 0.1150 0.5109 11.00000 0.05 1.24 Q13 1 0.5147 0.3522 0.1847 11.00000 0.05 1.22 Q14 1 1.0078 0.1729 0.3457 11.00000 0.05 1.20 Q15 1 0.7406 0.2106 0.2710 11.00000 0.05 1.15 Q16 1 0.0299 -0.2359 0.2466 11.00000 0.05 1.15 Q17 1 0.7991 0.3819 0.4238 11.00000 0.05 1.11 Q18 1 0.0512 -0.2332 0.3560 11.00000 0.05 1.11 Q19 1 0.2594 -0.2117 0.1766 11.00000 0.05 1.11 Q20 1 1.0846 0.3354 0.4901 11.00000 0.05 1.09 Q21 1 0.0181 -0.1601 0.2525 11.00000 0.05 1.04 Q22 1 -0.1386 0.5542 0.0870 11.00000 0.05 1.03 Q23 1 0.3508 0.0754 0.5913 11.00000 0.05 1.02 Q24 1 1.1326 0.4712 0.4620 11.00000 0.05 1.01 Q25 1 0.1478 -0.2424 0.2692 11.00000 0.05 1.00 Q26 1 0.2300 -0.2330 0.2627 11.00000 0.05 0.99 Q27 1 0.5467 0.3927 0.1089 11.00000 0.05 0.99 Q28 1 0.2680 0.3615 0.1666 11.00000 0.05 0.97 Q29 1 0.3878 -0.1418 0.0902 11.00000 0.05 0.90 Q30 1 0.3868 0.1060 0.5374 11.00000 0.05 0.89 Q31 1 -0.0490 0.6100 0.0310 11.00000 0.05 0.88 Q32 1 0.1942 -0.1848 0.3161 11.00000 0.05 0.87 Q33 1 0.5306 -0.1788 0.0962 11.00000 0.05 0.87 Q34 1 0.4363 -0.2572 0.0911 11.00000 0.05 0.82 Q35 1 0.1316 -0.2433 0.2032 11.00000 0.05 0.80 Q36 1 0.2905 -0.1482 0.0514 11.00000 0.05 0.79 Q37 1 0.1144 -0.1619 -0.0046 11.00000 0.05 0.77 Q38 1 0.5078 0.1144 0.5398 11.00000 0.05 0.76 Q39 1 0.0274 -0.2098 0.1673 11.00000 0.05 0.75 Q40 1 0.0444 -0.2068 0.0198 11.00000 0.05 0.75 Q41 1 0.1142 0.1055 0.5212 11.00000 0.05 0.75 Q42 1 0.8776 0.1627 0.2885 11.00000 0.05 0.73 Q43 1 0.0499 -0.1807 0.3115 11.00000 0.05 0.71 Q44 1 -0.0775 -0.2753 0.2707 11.00000 0.05 0.71 Q45 1 -0.0125 -0.2677 0.2874 11.00000 0.05 0.68 Q46 1 0.4656 0.1885 0.1436 11.00000 0.05 0.66 Q47 1 0.2435 0.0216 0.3660 11.00000 0.05 0.66 Q48 1 0.3207 0.2768 0.5619 11.00000 0.05 0.64 Q49 1 0.0108 -0.0766 -0.0103 11.00000 0.05 0.63 Q50 1 1.0059 0.5075 0.4913 11.00000 0.05 0.62 ; _shelx_res_checksum 79686 _shelx_hkl_file ; 0 0 -2-12.1594 10.3641 0 0 -2-7.63997 7.39918 0 0 -3 12443.2 151.552 0 0 3 12389.3 169.736 0 0 3 12920.0 157.249 0 0 -3 12485.6 154.308 0 0 -3 12305.2 168.882 0 0 3 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1813.78 187.335 2 -19 -1 1675.85 152.756 -2 19 0 1141.12 141.257 2 -19 0 1073.89 122.455 2 -19 0 1431.63 170.882 2 -19 1 90.8825 61.0373 -2 19 -1-6.40969 65.5391 2 -19 1 58.6909 75.0642 2 -19 2-55.5668 60.8762 -2 19 -2 54.2915 70.0742 2 -19 2 60.6358 72.8354 -2 19 -3 535.120 106.462 2 -19 3 612.381 125.162 2 -19 3 495.148 92.7982 2 -19 4 140.298 85.3826 2 -19 4 202.020 74.9630 -2 19 -4 17.1245 67.0508 2 -19 5 39.6348 74.0057 -2 19 -5 31.8275 72.9205 2 -19 5 1.54149 56.8150 2 -19 6 895.189 134.384 -2 19 -6 816.640 119.513 2 -19 6 1047.08 130.368 2 -19 7 1417.68 143.887 -2 19 -7 1463.63 151.177 2 -19 7 1634.22 178.641 2 -19 8 26.2124 62.3511 -2 19 -8-60.7093 68.9900 2 -19 9 922.621 128.084 2 -19 9 712.834 113.212 -2 19 -9 887.291 124.581 2 -19 10 650.456 114.644 2 -19 10 598.491 105.805 -2 19 -10 563.495 108.476 2 -19 11-46.8500 71.6822 2 -19 11 91.2455 66.3158 -2 19 -11 56.3374 68.3389 -2 19 -12 1341.85 148.574 2 -19 12 1559.94 156.594 -2 19 -12 1546.81 152.863 -2 19 -13 650.600 114.486 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173.564 2 -18 15 1169.30 146.994 -2 18 -15 1016.78 132.035 -2 18 -15 1129.25 131.701 2 -18 16 57.1715 73.6638 -2 18 -16 42.0966 69.3658 -2 18 -16-118.642 74.6062 2 -18 17 555.701 121.029 -2 18 -17 582.960 100.281 -2 18 -17 422.960 106.542 -2 18 -18 353.767 91.5065 -2 18 -18 294.417 96.7224 2 -18 18 228.459 94.6853 -2 18 -19 197.342 83.6668 -2 18 -19 115.232 75.8789 2 -18 19 122.766 78.0770 -2 18 -20 110.871 69.8146 -2 18 -20 6.37858 80.1576 2 -18 20 62.1625 74.8908 -2 18 -21 60.7232 67.0232 2 -18 21 128.455 85.4053 -2 18 -21 1.88290 75.1461 -2 18 -22-1.92221 68.9307 -2 18 -22 128.037 90.7383 2 -18 22 266.004 112.549 -2 18 -23 173.783 85.9089 -2 18 -23 96.4368 95.6064 2 -18 23 65.2136 94.5956 -2 18 -24 243.583 82.3680 -2 18 -24 261.229 120.594 2 -18 24 162.629 102.605 2 -18 25 19.0083 91.0958 -2 18 -25 64.8398 77.3856 -2 18 -25-89.7996 110.600 2 -18 26 52.6011 92.5425 -2 18 -26 13.6079 74.0051 -2 18 -26 16.0298 91.9656 -2 18 -27 137.081 119.244 2 -18 27 74.7439 108.731 -2 18 -27 157.577 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95.9163 -11 2 13-136.996 106.081 -11 2 12-44.9676 97.1031 -11 2 11-110.884 86.5409 -11 2 10-41.6236 92.5967 -11 2 9 86.0861 89.9653 -11 2 0-35.8477 74.2994 -11 2 -1 63.7555 85.3875 -11 2 -2-3.39547 81.3834 -11 2 -3 25.8444 81.7880 -11 2 -4-60.9740 88.3517 11 -1 -17-142.559 137.874 11 -1 -16 53.3223 121.120 11 -1 -15-29.9587 134.974 11 -1 -14-89.9089 124.668 -11 1 9 36.9201 85.9873 -11 1 1 76.6897 76.7725 -11 1 0-42.2662 80.2902 -11 1 -1 60.1872 75.7154 -11 1 -2 63.4219 87.6283 -11 1 -3-52.5936 87.4502 -11 1 -4-87.4545 93.1117 -11 1 -5 65.3895 92.7561 -11 1 -6-120.793 109.995 -11 1 -7 65.9523 99.6436 -11 1 -8 45.3310 102.057 -11 1 -9-67.6185 98.6441 11 0 -17-85.5229 123.869 11 0 -16 168.305 140.699 11 0 -15 6.87115 110.957 11 0 -14 153.517 122.431 11 0 -13-127.771 113.219 11 0 -12-84.1008 120.107 11 0 -11 17.8003 102.067 11 0 -10 35.0950 100.466 -11 0 2-4.09087 74.7798 -11 0 1 111.015 77.4584 -11 0 0-16.6305 71.5462 -11 0 -1 47.2190 76.4433 -11 0 -2-163.269 93.7565 -11 0 -3 82.8043 92.7690 -11 0 -4 58.9354 83.4434 -11 0 -5 104.444 92.4048 -11 0 -6-9.52786 89.8774 -11 0 -7 202.134 114.712 -11 0 -8 116.004 105.875 -11 0 -9 90.6907 114.522 11 1 -17 79.9236 134.678 11 1 -16 58.8298 110.799 11 1 -15 156.304 137.354 11 1 -14-3.70835 119.528 11 1 -13-280.110 129.006 11 1 -12 144.531 104.998 11 1 -11-72.4165 103.425 11 1 -10 94.8181 109.725 -11 -1 2 49.4571 72.0493 -11 -1 1 26.3864 76.3044 -11 -1 0 113.046 86.5115 -11 -1 -1-47.4505 82.7595 -11 -1 -2 64.9517 84.6343 -11 -1 -3 94.3775 88.4035 -11 -1 -4 23.6669 87.0615 -11 -1 -5-85.2120 99.3163 -11 -1 -6-40.2829 100.337 -11 -1 -7 155.992 113.715 -11 -1 -8 19.1864 99.3746 11 2 -17 197.035 140.432 11 2 -16 261.042 143.402 11 2 -15-51.8508 120.653 11 2 -14-109.258 118.081 11 2 -13-71.5080 99.2180 11 2 -12-18.4043 98.8444 11 2 -11 7.84335 96.8201 -11 -2 3-47.9666 69.8148 -11 -2 2 22.6509 72.4991 -11 -2 1-144.864 97.9032 -11 -2 0-99.0476 96.7604 -11 -2 -1 27.7227 89.1747 -11 -2 -2-5.80504 81.8856 -11 -2 -3 0.07924 83.5259 -11 -2 -4-149.492 100.352 -11 -2 -5 190.531 110.762 -11 -2 -6 157.526 101.294 -11 -2 -7-129.994 98.1221 11 3 -18-40.7141 126.210 11 3 -17 169.062 139.319 11 3 -16-77.6877 117.989 11 3 -15 129.645 120.900 11 3 -14-98.2695 122.451 11 3 -13 10.3191 104.536 11 3 -12 33.1189 102.343 11 3 -11 113.401 105.469 -11 -3 3 105.193 78.2078 -11 -3 2 38.0249 82.3960 -11 -3 1-45.0048 76.2829 -11 -3 0-33.0596 90.6679 -11 -3 -1-26.0790 86.0084 -11 -3 -2-37.2136 88.8356 -11 -3 -3-80.1059 99.8663 -11 -3 -4-20.4985 94.7339 -11 -3 -5 133.378 106.025 -11 -3 -6-84.5776 93.6366 11 4 -18-389.850 158.254 11 4 -17-99.6045 127.898 11 4 -16-159.993 127.761 11 4 -15 70.1037 128.809 11 4 -14 71.2516 105.101 11 4 -13-128.945 120.991 11 4 -12-142.259 109.496 -11 -4 4 14.0617 71.9162 -11 -4 3 18.4774 75.6066 -11 -4 2 20.7838 79.3868 -11 -4 1 18.7189 83.7605 -11 -4 0 38.5219 90.9123 -11 -4 -1 87.6329 91.5507 -11 -4 -2 6.37581 91.6313 -11 -4 -3-49.5669 93.5662 -11 -4 -4 232.006 120.838 -11 -4 -5 135.398 102.184 11 5 -18-162.113 131.439 11 5 -17-91.3385 138.653 11 5 -16 20.2882 111.249 11 5 -15-242.202 138.853 11 5 -14 214.448 127.515 11 5 -13 96.9646 105.831 -11 -5 4 136.291 79.4750 -11 -5 3 66.5520 77.5639 -11 -5 2-70.8281 80.4440 -11 -5 1-11.6560 81.6089 -11 -5 0 81.5930 92.3668 -11 -5 -1-13.9010 86.1256 -11 -5 -2 212.328 106.828 -11 -5 -3-24.0854 88.2661 -11 -5 -4-220.739 111.404 11 6 -18 156.732 146.172 11 6 -17 18.9483 113.812 11 6 -16-43.1097 125.509 11 6 -15-187.891 124.111 11 6 -14 149.446 120.990 -11 -6 5-28.4268 78.3138 -11 -6 4 101.671 73.9471 -11 -6 3 6.54269 76.3534 -11 -6 2-16.0564 86.1359 -11 -6 1-58.5117 105.443 -11 -6 0 123.817 98.2185 -11 -6 -1-87.9191 98.9729 -11 -6 -2 265.332 115.716 -11 -6 -3 30.9917 91.2067 11 7 -18-113.753 137.832 11 7 -17-159.170 124.664 11 7 -16 5.27448 113.982 11 7 -15-74.9278 111.459 -11 -7 5 28.7642 79.0257 -11 -7 4 12.8008 75.4672 -11 -7 3 134.392 92.3104 -11 -7 2 250.353 113.145 -11 -7 1 66.0274 97.0292 -11 -7 0 162.807 104.847 -11 -7 -1-134.252 101.945 -11 -7 -2-40.0641 92.2961 11 8 -18 1.25057 119.025 11 8 -17 88.6483 129.561 11 8 -16 235.821 129.268 -11 -8 5 113.929 90.2787 -11 -8 4-179.989 98.9571 -11 -8 3-31.0679 79.8619 -11 -8 2 35.4646 82.2992 -11 -8 1 137.686 101.881 -11 -8 0-40.1186 96.8735 -11 -9 6-39.0330 80.7609 -11 -9 5-149.678 92.8667 -11 -9 4-50.9782 85.7446 -11 -9 3-74.5549 97.7563 -11 -9 2-18.8182 80.7600 -11 -9 1-23.0504 96.4423 -11 -10 6-226.715 106.819 -11 -10 5 48.1631 91.1501 -11 -10 4-122.086 105.734 -11 -10 3-202.760 110.685 -11 -11 7-126.185 98.1167 -11 -11 6-31.1851 82.6339 -11 -11 5-0.31328 84.9508 12 -14 -1 90.4582 115.730 -12 14 -1 14.0086 102.130 -12 14 -2 70.2158 106.899 -12 14 -3 83.9288 110.300 -12 14 -4 2.80662 102.300 12 -13 -4 15.4777 122.071 12 -13 -3-96.0353 108.887 12 -13 -2 214.800 124.898 -12 13 0-58.6987 111.499 -12 13 -1-49.0505 100.077 -12 13 -2-46.6106 101.826 -12 13 -3-98.1520 110.644 -12 13 -4 9.45166 94.5351 -12 13 -5 110.530 108.963 -12 13 -6 74.2112 109.812 -12 13 -7-60.0684 104.677 12 -13 8-26.4915 102.059 12 -13 9-6.15454 105.364 12 -12 -7-86.6440 115.822 12 -12 -6-120.785 116.488 -12 12 6 33.2507 97.7730 12 -12 -5 152.379 126.935 12 -12 -4-289.516 145.287 12 -12 -3-51.5985 114.919 12 -12 -2-34.7458 105.145 -12 12 0-49.4009 92.7048 -12 12 -1 27.9757 103.796 -12 12 -2 68.9160 105.630 -12 12 -3 111.193 104.236 -12 12 -4 169.005 116.533 -12 12 -5 30.2626 105.240 -12 12 -6-196.789 116.703 12 -12 7-15.6752 101.614 -12 12 -7 112.231 103.372 12 -12 8-20.8367 100.781 -12 12 -8 88.0575 104.551 12 -12 9-196.839 115.314 12 -11 -8-72.9652 112.263 -12 11 8-91.4331 118.705 12 -11 -7 65.7417 120.540 -12 11 7 48.3787 105.295 12 -11 -6 37.4258 120.553 -12 11 6-31.4983 98.0139 12 -11 -5 158.593 131.076 12 -11 -4 9.73351 108.403 12 -11 -3-59.7770 99.0300 -12 11 1 90.7119 98.1875 -12 11 0 187.491 114.886 -12 11 -1 252.315 115.511 -12 11 -2-133.408 95.9027 -12 11 -3-41.1739 93.1094 -12 11 -4 286.914 121.159 -12 11 -5 8.43278 96.9497 -12 11 -6-116.088 104.281 12 -11 6 8.45788 97.6319 -12 11 -7 128.448 102.832 12 -11 7-219.234 131.277 12 -11 8-9.44307 105.243 -12 11 -8-14.2718 97.1427 12 -11 9 68.6916 117.606 -12 11 -9 108.177 101.905 -12 10 9 81.6852 103.502 12 -10 -8-77.2031 117.973 -12 10 8 10.9164 101.332 12 -10 -7 175.109 118.962 -12 10 7 45.4395 103.407 12 -10 -6 97.5826 107.966 12 -10 -5 54.6795 101.317 12 -10 -4 103.738 106.825 -12 10 2-187.185 109.232 -12 10 1-106.841 95.4661 -12 10 0-60.3012 91.0016 -12 10 -1-54.4883 94.7187 -12 10 -2 26.1132 87.8970 -12 10 -3 217.340 108.916 -12 10 -4 56.8897 88.2656 -12 10 -5 254.669 125.446 -12 10 -6 159.537 105.647 12 -10 6 220.495 125.140 -12 10 -7-5.35397 91.1837 12 -10 7 58.7039 99.0328 -12 10 -8 37.2169 88.6391 12 -10 8 4.27647 103.731 -12 10 -9-89.7331 101.594 12 -10 9-174.971 125.727 -12 9 9 70.8675 98.8057 -12 9 8 104.666 108.010 12 -9 -6-18.5501 101.045 12 -9 -5 22.7868 99.8846 -12 9 2-80.5349 95.9217 -12 9 1 40.8878 91.6909 -12 9 0 80.7899 88.1658 -12 9 -1 26.6863 94.6765 -12 9 -2-34.4485 89.0726 -12 9 -3 151.677 97.9864 -12 9 -4 76.6034 102.828 -12 9 -5 3.01684 85.8675 12 -9 5-97.3173 109.161 -12 9 -6 64.7500 95.1127 12 -9 6-26.1070 102.427 -12 9 -7 81.3260 90.4084 12 -9 7-12.8935 106.071 -12 9 -8-95.1144 89.3204 12 -9 8 230.269 131.664 -12 9 -9 30.3129 87.9830 12 -9 9 7.76384 108.027 -12 9 -10 126.161 100.003 -12 8 10 159.220 123.232 -12 8 9-214.578 124.850 -12 8 8-140.184 104.400 -12 8 -1 51.9349 88.8910 -12 8 -2-67.3116 91.4564 -12 8 -3 73.8199 91.9041 12 -8 4 75.5559 100.268 -12 8 -4-67.4481 89.5834 12 -8 5-89.6659 104.531 -12 8 -5-53.4276 93.1010 12 -8 6 32.6023 113.264 -12 8 -6 45.9483 82.6781 12 -8 7-142.702 118.946 -12 8 -7 165.917 105.004 12 -8 8 376.543 137.486 -12 8 -8-67.5892 83.2263 12 -8 9-222.271 138.045 -12 8 -9-65.5981 95.5156 -12 8 -10 187.144 107.348 -12 7 11 82.8306 108.435 -12 7 10-133.849 110.585 -12 7 9 120.163 115.160 12 -7 4-188.513 113.478 12 -7 5 80.8901 101.684 -12 7 -6-183.489 97.3593 12 -7 6-148.654 111.908 -12 7 -7-48.5982 88.9100 12 -7 7 37.6759 108.768 -12 7 -8-3.58882 85.2066 12 -7 8-132.953 116.610 -12 7 -9-206.403 102.741 12 -7 9 24.6856 104.196 -12 6 12 32.1594 113.912 -12 6 11 36.3845 100.594 -12 6 10-79.7148 115.683 12 -6 3-160.206 107.503 12 -6 4 33.0414 91.9611 12 -6 5 119.509 109.713 12 -6 6-6.11487 97.7661 12 -6 7-207.525 126.389 12 -6 8 188.642 125.045 -12 5 12-201.500 125.561 -12 5 11 122.842 107.528 -12 5 10 130.698 113.224 12 -5 4 209.728 121.367 12 -5 5-185.359 117.073 12 -5 6-115.424 104.159 12 -5 7-254.024 120.277 12 -5 8 192.722 120.439 -12 4 13-47.9459 104.260 -12 4 12 75.0260 104.724 -12 4 11 94.2063 105.619 -12 4 -3 4.64409 88.0315 12 -4 7 87.8589 109.786 12 -4 8-42.1077 99.9721 -12 3 14-43.7332 111.497 -12 3 13-29.7488 108.372 -12 3 12 227.772 120.424 -12 3 -2 6.79808 89.5163 -12 3 -3 100.240 105.140 -12 3 -4 18.2906 86.1404 -12 3 -5-86.1724 92.9127 -12 3 -6 104.529 98.5246 -12 3 -7 55.0371 101.872 -12 2 14 59.8748 100.944 -12 2 13-76.7478 118.181 -12 2 -2-31.0505 87.3662 -12 2 -3-21.0765 87.0832 -12 2 -4-0.17079 87.4613 -12 2 -5 10.9711 92.2147 -12 2 -6 118.532 111.908 -12 1 14 266.497 128.488 -12 1 -1 278.344 109.207 -12 1 -2 80.2757 91.7607 -12 1 -3 147.266 98.3551 -12 1 -5 64.4746 102.021 -12 1 -6 86.4310 104.099 -12 0 -1 156.768 98.7592 -12 0 -2-108.260 92.6488 -12 0 -3 108.341 99.4895 -12 0 -4 7.39910 93.3078 -12 0 -5-90.1259 96.5606 12 1 -15-12.8396 117.789 12 1 -14-198.339 142.614 -12 -1 0 179.755 99.0322 -12 -1 -1 21.9832 83.9638 -12 -1 -2 23.6120 88.2492 -12 -1 -3 114.750 100.126 -12 -1 -4 5.67065 92.6316 -12 -2 0 80.8050 97.5987 -12 -2 -1-96.8609 96.8179 -12 -2 -2-165.742 102.149 -12 -2 -3-40.5345 88.5776 -12 -3 1-99.4490 92.2990 -12 -3 0-20.5279 97.9470 -12 -3 -1-201.039 107.041 -12 -3 -2-113.959 102.455 -12 -4 1 78.9892 87.1484 -12 -4 0-26.2037 97.2017 -12 -4 -1 14.6228 91.9420 -12 -5 2-132.783 96.6881 -12 -5 1 34.0393 96.7995 -12 -5 0 110.114 101.752 -12 -6 2-26.5320 84.6975 -12 -6 1-8.68032 88.7117 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 93644 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4565(9) 0.3932(4) 0.4154(4) 0.0485(16) Uani 1 1 d . U . . . C2 C 0.4811(10) 0.4619(4) 0.4083(4) 0.0534(17) Uani 1 1 d . U . . . C3 C 0.4740(9) 0.4408(4) 0.3397(4) 0.0527(17) Uani 1 1 d . U . . . H2 H 0.487696 0.472571 0.318309 0.063 Uiso 1 1 calc R U . . . C4 C 0.4427(10) 0.3628(5) 0.3070(4) 0.0554(17) Uani 1 1 d . U . . . C5 C 0.4341(11) 0.3173(5) 0.2381(5) 0.0637(19) Uani 1 1 d . U . . . C6 C 0.4105(12) 0.2409(5) 0.2128(5) 0.070(2) Uani 1 1 d . U . . . C7 C 0.4056(13) 0.1937(6) 0.1406(5) 0.077(2) Uani 1 1 d . U . . . H3 H 0.410329 0.209285 0.105669 0.092 Uiso 1 1 calc R U . . . C8 C 0.3930(13) 0.1233(6) 0.1331(5) 0.077(2) Uani 1 1 d . U . . . H4 H 0.393634 0.080834 0.092764 0.093 Uiso 1 1 calc R U . . . C9 C 0.3779(12) 0.1267(5) 0.2020(5) 0.072(2) Uani 1 1 d . U . . . C10 C 0.3594(12) 0.0636(5) 0.2148(5) 0.069(2) Uani 1 1 d . U . . . C11 C 0.3420(12) 0.0671(5) 0.2784(5) 0.066(2) Uani 1 1 d . U . . . C12 C 0.3009(12) 0.0019(5) 0.2911(5) 0.072(2) Uani 1 1 d . U . . . H5 H 0.279844 -0.048168 0.258700 0.086 Uiso 1 1 calc R U . . . C13 C 0.2995(12) 0.0282(5) 0.3588(5) 0.071(2) Uani 1 1 d . U . . . H6 H 0.280503 -0.000731 0.382702 0.085 Uiso 1 1 calc R U . . . C14 C 0.3325(11) 0.1092(5) 0.3889(5) 0.0636(19) Uani 1 1 d . U . . . C15 C 0.3427(11) 0.1526(5) 0.4577(5) 0.0641(19) Uani 1 1 d . U . . . C16 C 0.3786(11) 0.2290(5) 0.4865(5) 0.0634(19) Uani 1 1 d . U . . . C17 C 0.3946(12) 0.2772(5) 0.5583(5) 0.066(2) Uani 1 1 d . U . . . H7 H 0.379849 0.262078 0.593015 0.079 Uiso 1 1 calc R U . . . C18 C 0.4338(12) 0.3472(5) 0.5671(5) 0.066(2) Uani 1 1 d . U . . . H8 H 0.455979 0.390160 0.608882 0.079 Uiso 1 1 calc R U . . . C19 C 0.4354(10) 0.3436(4) 0.5001(4) 0.0547(17) Uani 1 1 d . U . . . C20 C 0.4610(10) 0.4041(4) 0.4835(4) 0.0538(17) Uani 1 1 d . U . . . C21 C 0.4933(9) 0.4814(4) 0.5230(4) 0.0522(17) Uani 1 1 d . U . . . N1 N 0.4303(8) 0.3328(3) 0.3561(3) 0.0505(14) Uani 1 1 d . U . . . N2 N 0.3900(9) 0.1979(4) 0.2489(4) 0.0612(16) Uani 1 1 d . U . . . N3 N 0.3578(9) 0.1317(4) 0.3388(4) 0.0622(16) Uani 1 1 d . U . . . N4 N 0.4048(8) 0.2726(4) 0.4492(3) 0.0543(15) Uani 1 1 d . U . . . Ni1 Ni 0.39503(12) 0.23290(5) 0.34783(5) 0.0542(5) Uani 1 1 d . U . . . C22 C 0.4514(8) 0.3516(4) 0.1895(4) 0.075(2) Uani 1 1 d G U . . . C23 C 0.5923(7) 0.3674(5) 0.1739(4) 0.086(3) Uani 1 1 d G U . . . C24 C 0.6111(8) 0.3946(5) 0.1247(4) 0.105(3) Uani 1 1 d G U . . . H9 H 0.705407 0.405234 0.114307 0.126 Uiso 1 1 calc R U . . . C25 C 0.4889(11) 0.4061(5) 0.0912(4) 0.108(3) Uani 1 1 d G U . . . C26 C 0.3480(9) 0.3902(5) 0.1068(4) 0.098(3) Uani 1 1 d G U . . . H10 H 0.266269 0.397886 0.084407 0.117 Uiso 1 1 calc R U . . . C27 C 0.3292(7) 0.3630(5) 0.1560(4) 0.091(3) Uani 1 1 d G U . . . C28 C 0.7273(18) 0.3611(9) 0.2089(8) 0.114(5) Uani 1 1 d . U . . . H16 H 0.811164 0.374793 0.189728 0.172 Uiso 1 1 calc R U . . . H17 H 0.740002 0.394172 0.257298 0.172 Uiso 1 1 calc R U . . . H18 H 0.719954 0.310360 0.202735 0.172 Uiso 1 1 calc R U . . . C29 C 0.513(2) 0.4279(10) 0.0344(9) 0.126(5) Uani 1 1 d . U . . . H19 H 0.617819 0.436393 0.031990 0.189 Uiso 1 1 calc R U . . . H20 H 0.460888 0.388362 -0.008614 0.189 Uiso 1 1 calc R U . . . H21 H 0.477585 0.473049 0.043112 0.189 Uiso 1 1 calc R U . . . C30 C 0.1794(17) 0.3500(9) 0.1763(8) 0.112(4) Uani 1 1 d . U . . . H22 H 0.186530 0.331292 0.210517 0.168 Uiso 1 1 calc R U . . . H23 H 0.145398 0.396490 0.194971 0.168 Uiso 1 1 calc R U . . . H24 H 0.110341 0.314051 0.136376 0.168 Uiso 1 1 calc R U . . . C31 C 0.3561(8) -0.0097(3) 0.1565(3) 0.080(2) Uani 1 1 d G U . . . C32 C 0.2496(8) -0.0400(4) 0.0974(4) 0.087(3) Uani 1 1 d G U . . . H11 H 0.171457 -0.016250 0.095310 0.104 Uiso 1 1 calc R U . . . C33 C 0.2598(9) -0.1059(4) 0.0414(3) 0.105(3) Uani 1 1 d G U . . . C34 C 0.3765(10) -0.1415(4) 0.0446(3) 0.102(3) Uani 1 1 d G U . . . H12 H 0.383384 -0.185591 0.007125 0.123 Uiso 1 1 calc R U . . . C35 C 0.4830(8) -0.1112(4) 0.1037(4) 0.091(3) Uani 1 1 d G U . . . C36 C 0.4728(8) -0.0453(4) 0.1596(3) 0.077(2) Uani 1 1 d G U . . . H13 H 0.544057 -0.024999 0.199154 0.092 Uiso 1 1 calc R U . . . C37 C 0.1632(16) -0.1275(7) -0.0311(7) 0.119(4) Uani 1 1 d D U . . . C38 C 0.0081(16) -0.1358(9) -0.0113(10) 0.138(5) Uani 1 1 d D U . . . H25 H -0.000430 -0.089663 0.026285 0.208 Uiso 1 1 calc R U . . . H26 H -0.065265 -0.147126 -0.050310 0.208 Uiso 1 1 calc R U . . . H27 H -0.007501 -0.175661 0.002663 0.208 Uiso 1 1 calc R U . . . C39 C 0.176(2) -0.2012(8) -0.0909(9) 0.151(6) Uani 1 1 d D U . . . H28 H 0.272843 -0.196353 -0.103579 0.227 Uiso 1 1 calc R U . . . H29 H 0.159720 -0.240976 -0.076826 0.227 Uiso 1 1 calc R U . . . H30 H 0.101957 -0.212441 -0.129799 0.227 Uiso 1 1 calc R U . . . C44 C 0.3254(8) 0.1181(4) 0.5055(3) 0.071(2) Uani 1 1 d G U . . . C45 C 0.4456(6) 0.1014(4) 0.5354(4) 0.079(2) Uani 1 1 d G U . . . C46 C 0.4250(8) 0.0700(5) 0.5814(4) 0.092(3) Uani 1 1 d G U . . . H14 H 0.505441 0.058903 0.601394 0.110 Uiso 1 1 calc R U . . . C47 C 0.2843(9) 0.0553(5) 0.5977(4) 0.092(3) Uani 1 1 d G U . . . C48 C 0.1641(7) 0.0719(5) 0.5678(4) 0.094(3) Uani 1 1 d G U . . . H15 H 0.069959 0.062070 0.578695 0.113 Uiso 1 1 calc R U . . . C49 C 0.1847(7) 0.1033(4) 0.5218(4) 0.081(2) Uani 1 1 d G U . . . C50 C 0.5968(16) 0.1187(8) 0.5195(8) 0.101(4) Uani 1 1 d . U . . . H31 H 0.666176 0.103769 0.544249 0.151 Uiso 1 1 calc R U . . . H32 H 0.596628 0.091940 0.470788 0.151 Uiso 1 1 calc R U . . . H33 H 0.625259 0.171706 0.533368 0.151 Uiso 1 1 calc R U . . . C51 C 0.271(2) 0.0246(10) 0.6492(8) 0.116(4) Uani 1 1 d . U . . . H34 H 0.169175 0.016799 0.655986 0.174 Uiso 1 1 calc R U . . . H35 H 0.303218 -0.022404 0.632744 0.174 Uiso 1 1 calc R U . . . H36 H 0.331930 0.059365 0.692246 0.174 Uiso 1 1 calc R U . . . C52 C 0.0516(17) 0.1213(8) 0.4896(8) 0.103(4) Uani 1 1 d . U . . . H37 H 0.083314 0.142552 0.459177 0.154 Uiso 1 1 calc R U . . . H38 H -0.021962 0.076106 0.463941 0.154 Uiso 1 1 calc R U . . . H39 H 0.009689 0.156674 0.525506 0.154 Uiso 1 1 calc R U . . . C58 C 0.635(2) -0.2073(8) 0.0383(7) 0.136(5) Uani 1 1 d D U . . . H40 H 0.651240 -0.185365 0.006809 0.205 Uiso 1 1 calc R U . . . H41 H 0.716359 -0.230286 0.043025 0.205 Uiso 1 1 calc R U . . . H42 H 0.544200 -0.244673 0.020676 0.205 Uiso 1 1 calc R U . . . C55 C 0.7679(16) -0.0868(8) 0.1376(7) 0.124(5) Uani 1 1 d D U . . . H43 H 0.760223 -0.048444 0.181894 0.186 Uiso 1 1 calc R U . . . H44 H 0.848849 -0.110181 0.142444 0.186 Uiso 1 1 calc R U . . . H45 H 0.785715 -0.064740 0.106291 0.186 Uiso 1 1 calc R U . . . C56 C 0.6222(16) -0.1461(7) 0.1090(5) 0.118(4) Uani 1 1 d D U . . . C57 C 0.596(2) -0.1811(9) 0.1595(7) 0.141(6) Uani 1 1 d D U . . . H46 H 0.587966 -0.142702 0.203772 0.211 Uiso 1 1 calc R U . . . H47 H 0.505228 -0.218431 0.141970 0.211 Uiso 1 1 calc R U . . . H48 H 0.677387 -0.204045 0.164319 0.211 Uiso 1 1 calc R U . . . C53 C 0.184(2) -0.0655(9) -0.0555(9) 0.142(6) Uani 1 1 d D U . . . H49 H 0.281702 -0.059893 -0.068088 0.213 Uiso 1 1 calc R U . . . H50 H 0.110584 -0.078669 -0.094900 0.213 Uiso 1 1 calc R U . . . H51 H 0.174403 -0.019024 -0.018916 0.213 Uiso 1 1 calc R U . . . Sb1 Sb 0.88741(19) 0.22110(12) 0.33927(11) 0.1032(9) Uani 0.501(3) 1 d D U P A 1 Cl1 Cl 0.7779(10) 0.3271(6) 0.3738(5) 0.128(3) Uani 0.501(3) 1 d D U P A 1 Cl2 Cl 1.0543(7) 0.2652(5) 0.2832(4) 0.107(2) Uani 0.501(3) 1 d D U P A 1 Cl3 Cl 1.0611(8) 0.2816(5) 0.4417(5) 0.119(2) Uani 0.501(3) 1 d D U P A 1 Cl4 Cl 0.9853(8) 0.1107(4) 0.3008(4) 0.103(2) Uani 0.501(3) 1 d D U P A 1 Cl5 Cl 0.7282(7) 0.1657(4) 0.2354(3) 0.0963(18) Uani 0.501(3) 1 d D U P A 1 Cl6 Cl 0.7315(9) 0.1739(5) 0.3909(4) 0.116(2) Uani 0.501(3) 1 d D U P A 1 Sb2 Sb 0.000000 0.500000 0.000000 0.1429(17) Uani 0.513(5) 2 d S U P B 2 Cl11 Cl 0.2229(16) 0.5625(8) 0.0763(7) 0.191(5) Uani 0.513(5) 1 d . U P B 2 Cl12 Cl -0.035(2) 0.4021(11) 0.0260(11) 0.230(7) Uani 0.513(5) 1 d . U P B 2 Cl13 Cl -0.135(3) 0.5892(15) 0.0601(13) 0.295(11) Uani 0.513(5) 1 d . U P B 2 Cl7 Cl 1.6354(8) 0.7398(3) 0.2795(2) 0.0850(17) Uani 0.501(3) 1 d . U P A 1 Cl8 Cl 1.6716(8) 0.5777(3) 0.2634(3) 0.0902(17) Uani 0.501(3) 1 d . U P A 1 Cl9 Cl 1.3727(7) 0.5984(4) 0.2635(3) 0.102(2) Uani 0.501(3) 1 d . U P A 1 Cl10 Cl 1.6920(11) 0.6408(4) 0.1474(3) 0.117(2) Uani 0.501(3) 1 d . U P A 1 C59 C 1.514(3) 0.5926(13) 0.2153(12) 0.083(4) Uani 0.501(3) 1 d . U P A 1 C60 C 1.547(3) 0.6569(13) 0.2059(11) 0.085(4) Uani 0.501(3) 1 d . U P A 1 Cl18 Cl 0.3117(9) -0.1977(5) 0.2724(6) 0.139(3) Uani 0.513(5) 1 d D U P B 1 Cl19 Cl 0.0005(12) -0.1417(6) 0.2826(6) 0.154(4) Uani 0.513(5) 1 d D U P B 1 Cl20 Cl 0.1199(14) -0.1982(6) 0.1454(5) 0.161(4) Uani 0.513(5) 1 d D U P B 1 Cl21 Cl 0.0396(13) -0.2995(8) 0.2823(8) 0.183(5) Uani 0.513(5) 1 d D U P B 1 C63 C 0.139(2) -0.2623(17) 0.2322(11) 0.164(6) Uani 0.513(5) 1 d D U P B 1 C64 C 0.038(4) -0.2183(9) 0.2094(11) 0.162(6) Uani 0.513(5) 1 d D U P B 1 Sb3 Sb 0.9805(6) 0.4580(4) 0.5451(4) 0.162(3) Uani 0.242(3) 1 d D U P C 3 Cl22 Cl 1.1382(17) 0.4449(11) 0.6273(8) 0.197(7) Uani 0.242(3) 1 d D U P C 3 Cl23 Cl 0.8681(19) 0.5356(10) 0.6323(8) 0.215(10) Uani 0.242(3) 1 d D U P C 3 Cl24 Cl 0.8261(17) 0.4716(11) 0.4633(8) 0.176(11) Uani 0.242(3) 1 d D U P C 3 Cl25 Cl 0.8111(17) 0.3542(8) 0.5338(10) 0.199(8) Uani 0.242(3) 1 d D U P C 3 Cl26 Cl 1.0961(17) 0.3809(8) 0.4586(8) 0.175(8) Uani 0.242(3) 1 d D U P C 3 Cl27 Cl 1.1529(17) 0.5623(7) 0.5569(9) 0.153(8) Uani 0.242(3) 1 d D U P C 3 Cl28 Cl 1.1796(10) 0.4815(7) 0.5879(7) 0.173(4) Uani 0.513(5) 1 d D U P B 2 Cl29 Cl 0.7637(12) 0.3583(8) 0.5812(8) 0.204(5) Uani 0.513(5) 1 d D U P B 2 Cl30 Cl 0.8666(13) 0.5144(8) 0.5820(9) 0.222(6) Uani 0.513(5) 1 d D U P B 2 C65 C 0.9833(15) 0.4471(10) 0.563(2) 0.184(5) Uani 0.513(5) 1 d D U P B 2 Cl31 Cl 1.0693(16) 0.3928(10) 0.6693(9) 0.263(7) Uani 0.513(5) 1 d D U P B 2 C66 C 0.9601(17) 0.391(3) 0.5963(19) 0.194(6) Uani 0.513(5) 1 d D U P B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.060(3) 0.041(3) 0.039(3) 0.011(2) 0.008(3) 0.013(3) C2 0.069(4) 0.045(3) 0.040(3) 0.014(3) 0.001(3) 0.012(3) C3 0.067(4) 0.048(3) 0.038(3) 0.014(3) 0.009(3) 0.012(3) C4 0.072(4) 0.052(3) 0.040(3) 0.018(3) 0.002(3) 0.015(3) C5 0.086(4) 0.055(3) 0.047(3) 0.020(3) 0.003(3) 0.016(3) C6 0.093(4) 0.055(4) 0.051(4) 0.015(3) 0.003(3) 0.017(3) C7 0.102(5) 0.065(4) 0.053(4) 0.017(3) 0.010(4) 0.016(4) C8 0.102(5) 0.060(4) 0.057(4) 0.012(3) 0.009(4) 0.020(4) C9 0.093(4) 0.054(4) 0.056(4) 0.012(3) 0.003(3) 0.017(3) C10 0.090(4) 0.054(4) 0.056(4) 0.018(3) 0.005(3) 0.012(3) C11 0.089(4) 0.042(3) 0.058(4) 0.014(3) 0.003(3) 0.015(3) C12 0.093(5) 0.049(4) 0.065(4) 0.017(3) 0.010(4) 0.015(3) C13 0.095(5) 0.051(4) 0.063(4) 0.024(3) 0.003(4) 0.007(4) C14 0.082(4) 0.045(3) 0.059(4) 0.020(3) 0.004(3) 0.014(3) C15 0.084(4) 0.050(3) 0.059(4) 0.025(3) 0.005(3) 0.014(3) C16 0.087(4) 0.047(3) 0.053(3) 0.020(3) 0.004(3) 0.013(3) C17 0.093(5) 0.056(4) 0.051(4) 0.026(3) 0.008(3) 0.014(3) C18 0.089(5) 0.048(3) 0.051(4) 0.013(3) 0.007(3) 0.013(3) C19 0.071(4) 0.045(3) 0.042(3) 0.013(3) 0.007(3) 0.011(3) C20 0.067(4) 0.045(3) 0.043(3) 0.013(3) 0.003(3) 0.015(3) C21 0.066(4) 0.047(3) 0.040(3) 0.016(3) 0.004(3) 0.013(3) N1 0.066(3) 0.043(3) 0.037(3) 0.014(2) 0.003(2) 0.010(2) N2 0.087(4) 0.047(3) 0.043(3) 0.013(2) 0.001(3) 0.016(3) N3 0.087(4) 0.043(3) 0.050(3) 0.014(2) 0.004(3) 0.016(3) N4 0.072(3) 0.042(3) 0.045(3) 0.016(2) 0.001(3) 0.011(2) Ni1 0.0802(9) 0.0348(6) 0.0368(6) 0.0064(4) 0.0005(5) 0.0130(5) C22 0.103(5) 0.066(4) 0.056(4) 0.026(3) 0.004(4) 0.019(4) C23 0.116(5) 0.074(4) 0.067(4) 0.029(4) 0.021(4) 0.019(4) C24 0.132(6) 0.093(5) 0.086(5) 0.036(4) 0.025(5) 0.012(5) C25 0.137(6) 0.095(5) 0.092(5) 0.044(4) 0.011(5) 0.017(5) C26 0.128(6) 0.086(5) 0.083(5) 0.044(4) 0.000(5) 0.025(5) C27 0.117(5) 0.076(4) 0.078(5) 0.035(4) -0.001(4) 0.018(4) C28 0.120(9) 0.107(8) 0.098(8) 0.021(7) 0.055(7) 0.026(7) C29 0.169(11) 0.105(8) 0.110(9) 0.060(7) 0.015(8) 0.011(8) C30 0.130(9) 0.104(8) 0.102(8) 0.054(7) -0.022(7) 0.016(7) C31 0.099(5) 0.059(4) 0.070(4) 0.017(3) 0.009(4) 0.018(4) C32 0.101(5) 0.071(4) 0.074(5) 0.018(4) 0.009(4) 0.020(4) C33 0.111(5) 0.090(5) 0.093(5) 0.020(4) 0.013(4) 0.022(4) C34 0.118(5) 0.082(5) 0.091(5) 0.020(4) 0.014(5) 0.031(4) C35 0.120(5) 0.081(4) 0.080(4) 0.038(4) 0.018(4) 0.035(4) C36 0.104(5) 0.067(4) 0.065(4) 0.029(3) 0.021(4) 0.028(4) C37 0.126(6) 0.110(6) 0.106(6) 0.029(5) 0.015(5) 0.033(5) C38 0.145(10) 0.140(10) 0.117(10) 0.049(8) 0.012(8) 0.019(9) C39 0.152(11) 0.145(11) 0.124(10) 0.025(9) 0.007(9) 0.045(9) C44 0.097(4) 0.057(4) 0.064(4) 0.034(3) 0.005(4) 0.014(3) C45 0.102(5) 0.066(4) 0.073(4) 0.039(4) 0.006(4) 0.012(4) C46 0.114(5) 0.078(5) 0.083(5) 0.039(4) -0.007(4) 0.019(4) C47 0.121(5) 0.085(5) 0.079(5) 0.047(4) 0.001(4) 0.019(4) C48 0.112(5) 0.089(5) 0.085(5) 0.044(4) 0.014(4) 0.013(4) C49 0.105(5) 0.073(4) 0.074(4) 0.041(4) 0.011(4) 0.014(4) C50 0.120(8) 0.098(7) 0.105(8) 0.062(6) 0.006(7) 0.033(6) C51 0.157(10) 0.113(8) 0.093(8) 0.063(7) 0.007(7) 0.018(8) C52 0.124(9) 0.087(7) 0.110(8) 0.056(6) 0.024(7) 0.018(6) C58 0.147(10) 0.131(10) 0.115(10) 0.025(8) 0.029(8) 0.068(8) C55 0.151(10) 0.123(9) 0.091(8) 0.037(7) 0.015(8) 0.039(8) C56 0.141(6) 0.109(6) 0.100(6) 0.037(5) 0.015(5) 0.042(5) C57 0.158(11) 0.137(10) 0.123(10) 0.051(8) 0.008(9) 0.043(9) C53 0.164(11) 0.140(11) 0.115(10) 0.051(8) 0.013(9) 0.023(9) Sb1 0.0882(13) 0.1303(17) 0.1181(16) 0.0795(14) 0.0123(10) 0.0252(10) Cl1 0.123(5) 0.168(8) 0.124(6) 0.081(6) 0.020(4) 0.066(5) Cl2 0.077(3) 0.165(6) 0.115(5) 0.102(5) 0.017(3) 0.001(4) Cl3 0.096(4) 0.132(6) 0.144(6) 0.076(5) -0.011(4) 0.031(4) Cl4 0.102(4) 0.118(5) 0.126(5) 0.081(4) 0.027(4) 0.044(4) Cl5 0.087(4) 0.119(5) 0.086(4) 0.049(4) 0.000(3) 0.026(3) Cl6 0.124(5) 0.135(6) 0.113(5) 0.078(5) 0.011(4) 0.029(4) Sb2 0.178(3) 0.142(3) 0.0782(18) 0.0430(18) -0.0463(18) -0.004(2) Cl11 0.180(9) 0.186(10) 0.148(9) 0.037(7) -0.045(7) 0.013(8) Cl12 0.218(13) 0.250(14) 0.239(14) 0.117(11) 0.013(10) 0.073(11) Cl13 0.249(16) 0.289(17) 0.273(17) 0.071(14) -0.011(13) 0.024(13) Cl7 0.151(5) 0.054(2) 0.045(2) 0.0235(19) 0.013(3) 0.004(3) Cl8 0.155(5) 0.060(3) 0.056(3) 0.022(2) 0.032(3) 0.029(3) Cl9 0.104(4) 0.130(5) 0.051(3) 0.033(3) -0.010(3) -0.006(4) Cl10 0.180(7) 0.101(4) 0.068(3) 0.038(3) 0.029(4) 0.020(4) C59 0.102(7) 0.080(6) 0.065(6) 0.035(5) 0.012(6) 0.009(6) C60 0.108(7) 0.082(6) 0.064(6) 0.034(5) 0.011(6) 0.015(6) Cl18 0.131(6) 0.122(6) 0.180(8) 0.075(5) 0.029(5) 0.036(4) Cl19 0.139(6) 0.137(7) 0.170(8) 0.045(6) 0.045(6) 0.040(5) Cl20 0.207(9) 0.130(6) 0.128(7) 0.049(5) 0.007(6) 0.019(6) Cl21 0.186(9) 0.179(9) 0.189(9) 0.094(8) 0.032(7) 0.006(7) C63 0.164(8) 0.154(8) 0.170(8) 0.068(6) 0.023(7) 0.030(7) C64 0.163(8) 0.151(8) 0.164(8) 0.061(6) 0.021(7) 0.032(7) Sb3 0.098(3) 0.214(5) 0.173(5) 0.081(4) 0.014(3) 0.047(3) Cl22 0.173(9) 0.206(10) 0.202(10) 0.079(8) 0.026(9) 0.037(9) Cl23 0.161(12) 0.237(15) 0.211(16) 0.053(12) 0.003(12) 0.087(11) Cl24 0.164(13) 0.182(13) 0.179(13) 0.073(9) 0.023(9) 0.045(9) Cl25 0.162(11) 0.214(12) 0.193(12) 0.077(10) 0.021(10) 0.000(10) Cl26 0.138(11) 0.170(12) 0.173(13) 0.038(10) 0.020(10) 0.013(10) Cl27 0.136(10) 0.159(11) 0.160(11) 0.063(8) 0.017(8) 0.041(8) Cl28 0.151(7) 0.180(8) 0.183(8) 0.071(6) 0.028(6) 0.041(6) Cl29 0.161(8) 0.231(10) 0.181(9) 0.075(8) 0.023(7) -0.024(7) Cl30 0.158(7) 0.240(9) 0.221(10) 0.050(8) 0.006(8) 0.069(7) C65 0.153(6) 0.204(7) 0.187(7) 0.079(5) 0.022(6) 0.039(6) Cl31 0.257(11) 0.259(11) 0.245(11) 0.091(9) 0.029(10) 0.033(9) C66 0.175(7) 0.205(8) 0.193(8) 0.082(6) 0.024(6) 0.028(6) 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C20 133.1(7) . . ? N1 C1 C2 113.6(7) . . ? C20 C1 C2 113.3(7) . . ? C3 C2 C21 150.6(8) . 2_666 ? C3 C2 C1 105.1(7) . . ? C21 C2 C1 104.2(7) 2_666 . ? C2 C3 C4 107.5(7) . . ? C5 C4 C3 127.6(8) . . ? C5 C4 N1 121.4(8) . . ? C3 C4 N1 110.8(7) . . ? C4 C5 C6 121.9(9) . . ? C4 C5 C22 119.2(8) . . ? C6 C5 C22 118.9(8) . . ? C5 C6 N2 128.1(9) . . ? C5 C6 C7 121.4(9) . . ? N2 C6 C7 110.5(8) . . ? C8 C7 C6 107.2(10) . . ? C7 C8 C9 105.9(9) . . ? N2 C9 C10 126.3(9) . . ? N2 C9 C8 110.6(9) . . ? C10 C9 C8 123.1(9) . . ? C11 C10 C9 122.6(9) . . ? C11 C10 C31 119.5(8) . . ? C9 C10 C31 117.9(9) . . ? C10 C11 N3 126.0(8) . . ? C10 C11 C12 123.8(8) . . ? N3 C11 C12 110.2(8) . . ? C13 C12 C11 105.8(8) . . ? C12 C13 C14 108.6(9) . . ? N3 C14 C15 128.0(8) . . ? N3 C14 C13 109.3(8) . . ? C15 C14 C13 122.6(9) . . ? C16 C15 C14 122.7(9) . . ? C16 C15 C44 116.7(8) . . ? C14 C15 C44 120.5(8) . . ? C15 C16 N4 125.2(8) . . ? C15 C16 C17 125.2(9) . . ? N4 C16 C17 109.6(7) . . ? C18 C17 C16 108.3(8) . . ? C17 C18 C19 106.2(8) . . ? N4 C19 C20 119.9(7) . . ? N4 C19 C18 113.4(7) . . ? C20 C19 C18 126.8(7) . . ? C1 C20 C21 105.7(7) . . ? C1 C20 C19 121.3(7) . . ? C21 C20 C19 133.1(8) . . ? C20 C21 C2 143.2(8) . 2_666 ? C20 C21 C21 109.1(8) . 2_666 ? C2 C21 C21 107.7(8) 2_666 2_666 ? C1 N1 C4 102.9(6) . . ? C1 N1 Ni1 124.0(5) . . ? C4 N1 Ni1 133.0(5) . . ? C9 N2 C6 105.5(8) . . ? C9 N2 Ni1 126.5(7) . . ? C6 N2 Ni1 127.7(6) . . ? C14 N3 C11 106.1(7) . . ? C14 N3 Ni1 127.5(6) . . ? C11 N3 Ni1 126.3(6) . . ? C19 N4 C16 102.4(7) . . ? C19 N4 Ni1 131.7(6) . . ? C16 N4 Ni1 125.9(5) . . ? N1 Ni1 N3 179.4(3) . . ? N1 Ni1 N2 87.8(3) . . ? N3 Ni1 N2 91.8(3) . . ? N1 Ni1 N4 90.0(3) . . ? N3 Ni1 N4 90.3(3) . . ? N2 Ni1 N4 177.7(3) . . ? C23 C22 C27 120.0 . . ? C23 C22 C5 118.4(6) . . ? C27 C22 C5 121.4(6) . . ? C22 C23 C24 120.0 . . ? C22 C23 C28 123.9(8) . . ? C24 C23 C28 116.1(8) . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 C29 122.2(10) . . ? C24 C25 C29 117.5(10) . . ? C27 C26 C25 120.0 . . ? C26 C27 C22 120.0 . . ? C26 C27 C30 120.5(7) . . ? C22 C27 C30 119.4(7) . . ? C32 C31 C36 120.0 . . ? C32 C31 C10 122.5(6) . . ? C36 C31 C10 117.3(6) . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C32 C33 C37 118.3(6) . . ? C34 C33 C37 119.8(6) . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 C56 122.6(6) . . ? C36 C35 C56 117.4(6) . . ? C35 C36 C31 120.0 . . ? C38 C37 C39 109.1(9) . . ? C38 C37 C53 108.9(9) . . ? C39 C37 C53 108.4(9) . . ? C38 C37 C33 99.1(11) . . ? C39 C37 C33 116.6(12) . . ? C53 C37 C33 114.2(12) . . ? C45 C44 C49 120.0 . . ? C45 C44 C15 121.8(6) . . ? C49 C44 C15 118.2(6) . . ? C44 C45 C46 120.0 . . ? C44 C45 C50 120.2(6) . . ? C46 C45 C50 119.7(6) . . ? C47 C46 C45 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 C51 117.3(9) . . ? C48 C47 C51 122.7(9) . . ? C49 C48 C47 120.0 . . ? C48 C49 C44 120.0 . . ? C48 C49 C52 119.3(7) . . ? C44 C49 C52 120.7(7) . . ? C58 C56 C57 109.6(8) . . ? C58 C56 C55 109.4(8) . . ? C57 C56 C55 108.9(8) . . ? C58 C56 C35 110.5(11) . . ? C57 C56 C35 105.9(12) . . ? C55 C56 C35 112.5(11) . . ? Cl6 Sb1 Cl5 93.1(3) . . ? Cl6 Sb1 Cl2 177.3(3) . . ? Cl5 Sb1 Cl2 86.5(3) . . ? Cl6 Sb1 Cl1 89.2(3) . . ? Cl5 Sb1 Cl1 90.0(3) . . ? Cl2 Sb1 Cl1 93.4(3) . . ? Cl6 Sb1 Cl3 90.8(3) . . ? Cl5 Sb1 Cl3 176.0(3) . . ? Cl2 Sb1 Cl3 89.5(3) . . ? Cl1 Sb1 Cl3 89.9(3) . . ? Cl6 Sb1 Cl4 89.5(3) . . ? Cl5 Sb1 Cl4 87.3(3) . . ? Cl2 Sb1 Cl4 87.8(3) . . ? Cl1 Sb1 Cl4 176.9(3) . . ? Cl3 Sb1 Cl4 93.0(3) . . ? Cl12 Sb2 Cl12 180.0(3) 2_565 . ? Cl12 Sb2 Cl13 68.2(9) 2_565 . ? Cl12 Sb2 Cl13 111.8(9) . . ? Cl13 Sb2 Cl13 180.0 2_565 . ? Cl12 Sb2 Cl11 84.4(6) 2_565 . ? Cl12 Sb2 Cl11 95.6(6) . . ? Cl13 Sb2 Cl11 85.2(7) 2_565 . ? Cl13 Sb2 Cl11 94.9(7) . . ? C60 C59 Cl9 109.9(19) . . ? C60 C59 Cl8 113.2(18) . . ? Cl9 C59 Cl8 105.8(12) . . ? C59 C60 Cl7 116.6(17) . . ? C59 C60 Cl10 105.8(18) . . ? Cl7 C60 Cl10 103.1(13) . . ? C64 C63 Cl18 105(2) . . ? C64 C63 Cl21 107.1(14) . . ? Cl18 C63 Cl21 118.4(9) . . ? C63 C64 Cl20 106.8(13) . . ? C63 C64 Cl19 111(2) . . ? Cl20 C64 Cl19 118.0(9) . . ? Cl24 Sb3 Cl27 95.1(6) 2_766 2_766 ? Cl24 Sb3 Cl25 162.2(7) 2_766 . ? Cl27 Sb3 Cl25 83.8(6) 2_766 . ? Cl24 Sb3 Cl24 93.7(6) 2_766 . ? Cl27 Sb3 Cl24 17.6(7) 2_766 . ? Cl25 Sb3 Cl24 90.5(3) . . ? Cl24 Sb3 Cl23 106.9(7) 2_766 . ? Cl27 Sb3 Cl23 106.7(7) 2_766 . ? Cl25 Sb3 Cl23 90.3(3) . . ? Cl24 Sb3 Cl23 90.4(3) . . ? Cl24 Sb3 Cl26 72.6(7) 2_766 . ? Cl27 Sb3 Cl26 74.0(7) 2_766 . ? Cl25 Sb3 Cl26 90.2(3) . . ? Cl24 Sb3 Cl26 90.2(3) . . ? Cl23 Sb3 Cl26 179.2(4) . . ? Cl24 Sb3 Cl22 85.8(6) 2_766 . ? Cl27 Sb3 Cl22 162.4(7) 2_766 . ? Cl25 Sb3 Cl22 90.0(3) . . ? Cl24 Sb3 Cl22 179.4(4) . . ? Cl23 Sb3 Cl22 89.8(3) . . ? Cl26 Sb3 Cl22 89.6(3) . . ? Cl24 Sb3 Cl27 17.5(7) 2_766 . ? Cl27 Sb3 Cl27 96.6(5) 2_766 . ? Cl25 Sb3 Cl27 179.5(4) . . ? Cl24 Sb3 Cl27 90.0(3) . . ? Cl23 Sb3 Cl27 89.8(3) . . ? Cl26 Sb3 Cl27 89.7(3) . . ? Cl22 Sb3 Cl27 89.5(3) . . ? Cl27 Cl24 Sb3 78.6(19) 2_766 . ? Sb3 Cl24 Sb3 86.3(6) 2_766 . ? Cl24 Cl27 Sb3 68(2) 2_766 . ? Sb3 Cl27 Sb3 83.4(5) 2_766 . ? C66 C65 Cl28 100.3(14) . . ? C66 C65 Cl30 118(3) . . ? Cl28 C65 Cl30 117.8(9) . . ? C65 C66 Cl29 104.3(13) . . ? C65 C66 Cl31 128(3) . . ? Cl29 C66 Cl31 119.6(10) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.314(9) . ? C1 C20 1.387(11) . ? C1 C2 1.433(11) . ? C2 C3 1.350(11) . ? C2 C21 1.413(11) 2_666 ? C3 C4 1.389(11) . ? C4 C5 1.368(12) . ? C4 N1 1.423(10) . ? C5 C6 1.368(13) . ? C5 C22 1.480(11) . ? C6 N2 1.382(13) . ? C6 C7 1.438(13) . ? C7 C8 1.335(15) . ? C8 C9 1.476(15) . ? C9 N2 1.341(11) . ? C9 C10 1.391(14) . ? C10 C11 1.368(14) . ? C10 C31 1.475(10) . ? C11 N3 1.377(11) . ? C11 C12 1.446(13) . ? C12 C13 1.330(14) . ? C13 C14 1.443(12) . ? C14 N3 1.356(12) . ? C14 C15 1.358(13) . ? C15 C16 1.362(12) . ? C15 C44 1.466(10) . ? C16 N4 1.420(11) . ? C16 C17 1.422(13) . ? C17 C18 1.319(13) . ? C18 C19 1.417(13) . ? C19 N4 1.353(10) . ? C19 C20 1.394(12) . ? C20 C21 1.390(11) . ? C21 C21 1.470(16) 2_666 ? N1 Ni1 1.906(6) . ? N2 Ni1 1.941(7) . ? N3 Ni1 1.926(7) . ? N4 Ni1 1.979(7) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C23 C28 1.454(19) . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C25 C29 1.484(16) . ? C26 C27 1.3900 . ? C27 C30 1.498(18) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C33 C37 1.589(17) . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C35 C56 1.570(16) . ? C37 C38 1.528(7) . ? C37 C39 1.529(7) . ? C37 C53 1.532(7) . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C45 C46 1.3900 . ? C45 C50 1.484(16) . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C47 C51 1.483(14) . ? C48 C49 1.3900 . ? C49 C52 1.525(16) . ? C58 C56 1.534(7) . ? C55 C56 1.538(7) . ? C56 C57 1.537(7) . ? Sb1 Cl6 2.215(8) . ? Sb1 Cl5 2.305(6) . ? Sb1 Cl2 2.318(5) . ? Sb1 Cl1 2.352(8) . ? Sb1 Cl3 2.351(8) . ? Sb1 Cl4 2.362(7) . ? Sb2 Cl12 2.24(2) 2_565 ? Sb2 Cl12 2.24(2) . ? Sb2 Cl13 2.33(3) 2_565 ? Sb2 Cl13 2.33(3) . ? Sb2 Cl11 2.337(11) . ? Sb2 Cl11 2.337(11) 2_565 ? Cl7 C60 1.77(2) . ? Cl8 C59 1.85(3) . ? Cl9 C59 1.72(2) . ? Cl10 C60 1.88(3) . ? C59 C60 1.38(3) . ? Cl18 C63 1.780(10) . ? Cl19 C64 1.785(10) . ? Cl20 C64 1.779(10) . ? Cl21 C63 1.785(10) . ? C63 C64 1.561(10) . ? Sb3 Cl24 2.17(2) 2_766 ? Sb3 Cl27 2.28(2) 2_766 ? Sb3 Cl25 2.311(8) . ? Sb3 Cl24 2.311(8) . ? Sb3 Cl23 2.319(8) . ? Sb3 Cl26 2.323(8) . ? Sb3 Cl22 2.330(8) . ? Sb3 Cl27 2.330(8) . ? Sb3 Sb3 3.065(15) 2_766 ? Cl24 Cl27 0.70(3) 2_766 ? Cl28 C65 1.787(10) . ? Cl29 C66 1.782(10) . ? Cl30 C65 1.787(10) . ? C65 C66 1.561(10) . ? Cl31 C66 1.783(10) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -2.3(10) . . . . ? C20 C1 C2 C3 179.5(8) . . . . ? N1 C1 C2 C21 -180.0(7) . . . 2_666 ? C20 C1 C2 C21 1.8(10) . . . 2_666 ? C21 C2 C3 C4 177.0(15) 2_666 . . . ? C1 C2 C3 C4 1.5(9) . . . . ? C2 C3 C4 C5 -175.9(9) . . . . ? C2 C3 C4 N1 -0.4(10) . . . . ? C3 C4 C5 C6 176.2(10) . . . . ? N1 C4 C5 C6 1.2(15) . . . . ? C3 C4 C5 C22 -3.5(15) . . . . ? N1 C4 C5 C22 -178.5(8) . . . . ? C4 C5 C6 N2 1.1(17) . . . . ? C22 C5 C6 N2 -179.2(9) . . . . ? C4 C5 C6 C7 -178.3(10) . . . . ? C22 C5 C6 C7 1.4(15) . . . . ? C5 C6 C7 C8 175.2(11) . . . . ? N2 C6 C7 C8 -4.3(13) . . . . ? C6 C7 C8 C9 4.5(12) . . . . ? C7 C8 C9 N2 -3.4(12) . . . . ? C7 C8 C9 C10 178.8(11) . . . . ? N2 C9 C10 C11 4.1(18) . . . . ? C8 C9 C10 C11 -178.4(10) . . . . ? N2 C9 C10 C31 -176.9(9) . . . . ? C8 C9 C10 C31 0.5(15) . . . . ? C9 C10 C11 N3 -8.2(17) . . . . ? C31 C10 C11 N3 172.8(9) . . . . ? C9 C10 C11 C12 170.6(10) . . . . ? C31 C10 C11 C12 -8.4(15) . . . . ? C10 C11 C12 C13 178.3(10) . . . . ? N3 C11 C12 C13 -2.7(12) . . . . ? C11 C12 C13 C14 2.5(12) . . . . ? C12 C13 C14 N3 -1.6(12) . . . . ? C12 C13 C14 C15 -178.4(10) . . . . ? N3 C14 C15 C16 1.6(17) . . . . ? C13 C14 C15 C16 177.8(10) . . . . ? N3 C14 C15 C44 -174.0(9) . . . . ? C13 C14 C15 C44 2.3(15) . . . . ? C14 C15 C16 N4 2.1(16) . . . . ? C44 C15 C16 N4 177.8(8) . . . . ? C14 C15 C16 C17 -178.3(10) . . . . ? C44 C15 C16 C17 -2.6(15) . . . . ? C15 C16 C17 C18 178.2(10) . . . . ? N4 C16 C17 C18 -2.1(12) . . . . ? C16 C17 C18 C19 2.9(11) . . . . ? C17 C18 C19 N4 -2.9(11) . . . . ? C17 C18 C19 C20 175.5(9) . . . . ? N1 C1 C20 C21 -179.4(9) . . . . ? C2 C1 C20 C21 -1.7(10) . . . . ? N1 C1 C20 C19 0.4(15) . . . . ? C2 C1 C20 C19 178.2(8) . . . . ? N4 C19 C20 C1 -0.3(13) . . . . ? C18 C19 C20 C1 -178.6(9) . . . . ? N4 C19 C20 C21 179.5(9) . . . . ? C18 C19 C20 C21 1.2(16) . . . . ? C1 C20 C21 C2 -178.8(12) . . . 2_666 ? C19 C20 C21 C2 1(2) . . . 2_666 ? C1 C20 C21 C21 0.8(12) . . . 2_666 ? C19 C20 C21 C21 -179.0(10) . . . 2_666 ? C20 C1 N1 C4 179.7(9) . . . . ? C2 C1 N1 C4 1.9(9) . . . . ? C20 C1 N1 Ni1 -2.8(13) . . . . ? C2 C1 N1 Ni1 179.4(6) . . . . ? C5 C4 N1 C1 174.9(9) . . . . ? C3 C4 N1 C1 -0.9(9) . . . . ? C5 C4 N1 Ni1 -2.3(13) . . . . ? C3 C4 N1 Ni1 -178.1(6) . . . . ? C10 C9 N2 C6 178.5(11) . . . . ? C8 C9 N2 C6 0.7(12) . . . . ? C10 C9 N2 Ni1 3.3(16) . . . . ? C8 C9 N2 Ni1 -174.4(7) . . . . ? C5 C6 N2 C9 -177.4(11) . . . . ? C7 C6 N2 C9 2.1(12) . . . . ? C5 C6 N2 Ni1 -2.3(16) . . . . ? C7 C6 N2 Ni1 177.1(7) . . . . ? C15 C14 N3 C11 176.4(10) . . . . ? C13 C14 N3 C11 -0.2(11) . . . . ? C15 C14 N3 Ni1 -7.4(16) . . . . ? C13 C14 N3 Ni1 176.0(7) . . . . ? C10 C11 N3 C14 -179.3(10) . . . . ? C12 C11 N3 C14 1.8(11) . . . . ? C10 C11 N3 Ni1 4.5(15) . . . . ? C12 C11 N3 Ni1 -174.5(7) . . . . ? C20 C19 N4 C16 -177.0(8) . . . . ? C18 C19 N4 C16 1.5(10) . . . . ? C20 C19 N4 Ni1 2.8(13) . . . . ? C18 C19 N4 Ni1 -178.7(7) . . . . ? C15 C16 N4 C19 179.9(9) . . . . ? C17 C16 N4 C19 0.3(10) . . . . ? C15 C16 N4 Ni1 0.1(14) . . . . ? C17 C16 N4 Ni1 -179.5(6) . . . . ? C4 C5 C22 C23 92.6(10) . . . . ? C6 C5 C22 C23 -87.1(10) . . . . ? C4 C5 C22 C27 -92.0(10) . . . . ? C6 C5 C22 C27 88.3(10) . . . . ? C27 C22 C23 C24 0.0 . . . . ? C5 C22 C23 C24 175.5(8) . . . . ? C27 C22 C23 C28 176.5(10) . . . . ? C5 C22 C23 C28 -8.0(11) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C28 C23 C24 C25 -176.8(9) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C23 C24 C25 C29 -174.0(11) . . . . ? C24 C25 C26 C27 0.0 . . . . ? C29 C25 C26 C27 173.7(12) . . . . ? C25 C26 C27 C22 0.0 . . . . ? C25 C26 C27 C30 176.4(10) . . . . ? C23 C22 C27 C26 0.0 . . . . ? C5 C22 C27 C26 -175.3(8) . . . . ? C23 C22 C27 C30 -176.4(9) . . . . ? C5 C22 C27 C30 8.3(10) . . . . ? C11 C10 C31 C32 118.3(9) . . . . ? C9 C10 C31 C32 -60.7(11) . . . . ? C11 C10 C31 C36 -67.6(11) . . . . ? C9 C10 C31 C36 113.5(9) . . . . ? C36 C31 C32 C33 0.0 . . . . ? C10 C31 C32 C33 174.0(8) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C31 C32 C33 C37 -164.5(9) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C37 C33 C34 C35 164.2(9) . . . . ? C33 C34 C35 C36 0.0 . . . . ? C33 C34 C35 C56 -176.6(9) . . . . ? C34 C35 C36 C31 0.0 . . . . ? C56 C35 C36 C31 176.8(8) . . . . ? C32 C31 C36 C35 0.0 . . . . ? C10 C31 C36 C35 -174.3(8) . . . . ? C32 C33 C37 C38 -62.1(9) . . . . ? C34 C33 C37 C38 133.4(7) . . . . ? C32 C33 C37 C39 -178.9(7) . . . . ? C34 C33 C37 C39 16.6(11) . . . . ? C32 C33 C37 C53 53.4(10) . . . . ? C34 C33 C37 C53 -111.1(9) . . . . ? C16 C15 C44 C45 -87.3(10) . . . . ? C14 C15 C44 C45 88.4(10) . . . . ? C16 C15 C44 C49 91.5(9) . . . . ? C14 C15 C44 C49 -92.8(10) . . . . ? C49 C44 C45 C46 0.0 . . . . ? C15 C44 C45 C46 178.8(8) . . . . ? C49 C44 C45 C50 -178.5(9) . . . . ? C15 C44 C45 C50 0.3(10) . . . . ? C44 C45 C46 C47 0.0 . . . . ? C50 C45 C46 C47 178.5(9) . . . . ? C45 C46 C47 C48 0.0 . . . . ? C45 C46 C47 C51 -177.7(10) . . . . ? C46 C47 C48 C49 0.0 . . . . ? C51 C47 C48 C49 177.6(11) . . . . ? C47 C48 C49 C44 0.0 . . . . ? C47 C48 C49 C52 -179.9(9) . . . . ? C45 C44 C49 C48 0.0 . . . . ? C15 C44 C49 C48 -178.8(7) . . . . ? C45 C44 C49 C52 179.9(9) . . . . ? C15 C44 C49 C52 1.1(10) . . . . ? C34 C35 C56 C58 9.3(10) . . . . ? C36 C35 C56 C58 -167.4(7) . . . . ? C34 C35 C56 C57 -109.3(8) . . . . ? C36 C35 C56 C57 74.0(8) . . . . ? C34 C35 C56 C55 131.9(7) . . . . ? C36 C35 C56 C55 -44.7(9) . . . . ? Cl9 C59 C60 Cl7 70(2) . . . . ? Cl8 C59 C60 Cl7 -48(2) . . . . ? Cl9 C59 C60 Cl10 -175.9(12) . . . . ? Cl8 C59 C60 Cl10 66.1(18) . . . . ? Cl18 C63 C64 Cl20 65(2) . . . . ? Cl21 C63 C64 Cl20 -168.1(10) . . . . ? Cl18 C63 C64 Cl19 -64.8(14) . . . . ? Cl21 C63 C64 Cl19 62(2) . . . . ? Cl28 C65 C66 Cl29 175.4(16) . . . . ? Cl30 C65 C66 Cl29 46(4) . . . . ? Cl28 C65 C66 Cl31 27(5) . . . . ? Cl30 C65 C66 Cl31 -102(3) . . . . ?