# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_120911a _database_code_depnum_ccdc_archive 'CCDC 928786' #TrackingRef 'web_deposit_cif_file_0_HiroshiShinokubo_1363047956.120911a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H70 Cl6 N8 Ni2' _chemical_formula_weight 1545.62 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 34.583(5) _cell_length_b 29.038(4) _cell_length_c 14.934(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.398(3) _cell_angle_gamma 90.00 _cell_volume 14952(3) _cell_formula_units_Z 8 _cell_measurement_temperature 153 _cell_measurement_reflns_used 5179 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.85 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6400 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 106511 _diffrn_reflns_av_R_equivalents 0.0650 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 0.59 _diffrn_reflns_theta_max 28.37 _reflns_number_total 37217 _reflns_number_gt 21482 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+12.2738P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 37217 _refine_ls_number_parameters 1933 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1357 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2023 _refine_ls_wR_factor_gt 0.1706 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C30A C 0.40894(14) 0.43423(16) 0.0525(4) 0.0603(15) Uani 1 1 d . . . C1A C 0.29429(10) 0.64375(12) 0.1048(2) 0.0275(8) Uani 1 1 d . . . C2A C 0.26379(10) 0.67864(11) 0.1038(2) 0.0243(7) Uani 1 1 d . . . C3A C 0.27904(10) 0.71560(11) 0.0645(2) 0.0265(8) Uani 1 1 d . . . H3A H 0.2664 0.7435 0.0528 0.032 Uiso 1 1 calc R . . C4A C 0.31756(10) 0.70498(12) 0.0440(2) 0.0263(8) Uani 1 1 d . . . C5A C 0.34234(11) 0.73520(12) 0.0034(2) 0.0294(8) Uani 1 1 d . . . C6A C 0.37970(12) 0.72346(13) -0.0122(3) 0.0336(9) Uani 1 1 d . . . C7A C 0.40686(13) 0.75412(15) -0.0496(3) 0.0467(11) Uani 1 1 d . . . H7A H 0.4024 0.7846 -0.0666 0.056 Uiso 1 1 calc R . . C8A C 0.43991(14) 0.73050(15) -0.0551(3) 0.0533(13) Uani 1 1 d . . . H8A H 0.4626 0.7416 -0.0769 0.064 Uiso 1 1 calc R . . C9A C 0.43381(12) 0.68526(14) -0.0215(3) 0.0398(10) Uani 1 1 d . . . C10A C 0.45472(12) 0.61136(14) 0.0094(3) 0.0411(10) Uani 1 1 d . . . C11A C 0.48440(13) 0.57647(16) 0.0114(3) 0.0513(12) Uani 1 1 d . . . H11A H 0.5092 0.5798 -0.0077 0.062 Uiso 1 1 calc R . . C12A C 0.46939(12) 0.53821(16) 0.0461(3) 0.0526(13) Uani 1 1 d . . . H12A H 0.4819 0.5101 0.0561 0.063 Uiso 1 1 calc R . . C13A C 0.43034(12) 0.54915(14) 0.0648(3) 0.0437(11) Uani 1 1 d . . . C14A C 0.40498(12) 0.51759(14) 0.0976(3) 0.0464(11) Uani 1 1 d . . . C15A C 0.36743(12) 0.52963(14) 0.1136(3) 0.0439(11) Uani 1 1 d . . . C16A C 0.33953(13) 0.49835(15) 0.1470(4) 0.0586(15) Uani 1 1 d . . . H16A H 0.3431 0.4671 0.1585 0.070 Uiso 1 1 calc R . . C17A C 0.30751(13) 0.52284(14) 0.1582(4) 0.0592(15) Uani 1 1 d . . . H17A H 0.2847 0.5120 0.1798 0.071 Uiso 1 1 calc R . . C18A C 0.31513(11) 0.56934(13) 0.1302(3) 0.0405(10) Uani 1 1 d . . . C19A C 0.22474(10) 0.67371(12) 0.1349(2) 0.0243(7) Uani 1 1 d . . . C20A C 0.20914(11) 0.63176(13) 0.1591(3) 0.0352(9) Uani 1 1 d . . . H20A H 0.2242 0.6053 0.1581 0.042 Uiso 1 1 calc R . . C21A C 0.17136(11) 0.62884(13) 0.1848(3) 0.0343(9) Uani 1 1 d . . . H21A H 0.1614 0.6004 0.2001 0.041 Uiso 1 1 calc R . . C22A C 0.14856(12) 0.66768(13) 0.1876(3) 0.0336(9) Uani 1 1 d . . . H22A H 0.1233 0.6658 0.2047 0.040 Uiso 1 1 calc R . . C23A C 0.16397(13) 0.70942(14) 0.1646(3) 0.0456(11) Uani 1 1 d . . . H23A H 0.1489 0.7359 0.1662 0.055 Uiso 1 1 calc R . . C24A C 0.20108(12) 0.71251(13) 0.1396(3) 0.0387(10) Uani 1 1 d . . . H24A H 0.2108 0.7412 0.1252 0.046 Uiso 1 1 calc R . . C25A C 0.41795(13) 0.46834(16) 0.1159(4) 0.0521(13) Uani 1 1 d . . . C26A C 0.43831(13) 0.45785(19) 0.1974(4) 0.0625(16) Uani 1 1 d . . . C27A C 0.44923(15) 0.4111(2) 0.2134(5) 0.077(2) Uani 1 1 d . . . H27A H 0.4627 0.4033 0.2675 0.092 Uiso 1 1 calc R . . C28A C 0.44018(17) 0.3768(2) 0.1496(6) 0.087(2) Uani 1 1 d . . . C29A C 0.42020(15) 0.38906(17) 0.0706(5) 0.076(2) Uani 1 1 d . . . H29A H 0.4140 0.3665 0.0277 0.091 Uiso 1 1 calc R . . C42A C 0.44786(16) 0.4936(2) 0.2670(4) 0.083(2) Uani 1 1 d . . . H42A H 0.4680 0.5132 0.2480 0.124 Uiso 1 1 calc R . . H42B H 0.4565 0.4789 0.3226 0.124 Uiso 1 1 calc R . . H42C H 0.4252 0.5117 0.2754 0.124 Uiso 1 1 calc R . . C31A C 0.4529(2) 0.3275(2) 0.1697(6) 0.137(4) Uani 1 1 d . . . H31A H 0.4320 0.3069 0.1513 0.206 Uiso 1 1 calc R . . H31B H 0.4594 0.3241 0.2330 0.206 Uiso 1 1 calc R . . H31C H 0.4751 0.3204 0.1374 0.206 Uiso 1 1 calc R . . C32A C 0.38728(16) 0.44520(16) -0.0354(4) 0.0692(16) Uani 1 1 d . . . H32A H 0.3847 0.4178 -0.0714 0.104 Uiso 1 1 calc R . . H32B H 0.4012 0.4681 -0.0663 0.104 Uiso 1 1 calc R . . H32C H 0.3620 0.4567 -0.0250 0.104 Uiso 1 1 calc R . . C33A C 0.32721(12) 0.78245(12) -0.0233(3) 0.0322(9) Uani 1 1 d . . . C34A C 0.31071(12) 0.78948(13) -0.1106(3) 0.0348(9) Uani 1 1 d . . . C35A C 0.29605(13) 0.83253(14) -0.1338(3) 0.0434(11) Uani 1 1 d . . . H35A H 0.2849 0.8371 -0.1918 0.052 Uiso 1 1 calc R . . C36A C 0.29729(14) 0.86887(14) -0.0743(4) 0.0500(13) Uani 1 1 d . . . C37A C 0.31331(15) 0.86154(14) 0.0111(3) 0.0529(13) Uani 1 1 d . . . H37A H 0.3142 0.8857 0.0520 0.064 Uiso 1 1 calc R . . C38A C 0.32852(14) 0.81847(13) 0.0388(3) 0.0434(11) Uani 1 1 d . . . C39A C 0.30937(14) 0.75165(14) -0.1789(3) 0.0456(11) Uani 1 1 d . . . H39A H 0.2943 0.7614 -0.2321 0.068 Uiso 1 1 calc R . . H39B H 0.2978 0.7248 -0.1548 0.068 Uiso 1 1 calc R . . H39C H 0.3352 0.7445 -0.1935 0.068 Uiso 1 1 calc R . . C40A C 0.28141(17) 0.91553(15) -0.1051(4) 0.0780(19) Uani 1 1 d . . . H40A H 0.2552 0.9120 -0.1306 0.117 Uiso 1 1 calc R . . H40B H 0.2972 0.9280 -0.1495 0.117 Uiso 1 1 calc R . . H40C H 0.2818 0.9361 -0.0547 0.117 Uiso 1 1 calc R . . C41A C 0.34527(18) 0.81242(16) 0.1342(3) 0.0677(17) Uani 1 1 d . . . H41A H 0.3262 0.7986 0.1692 0.102 Uiso 1 1 calc R . . H41B H 0.3526 0.8419 0.1591 0.102 Uiso 1 1 calc R . . H41C H 0.3677 0.7929 0.1351 0.102 Uiso 1 1 calc R . . C1B C 0.28992(11) 0.35777(13) 0.5886(3) 0.0303(8) Uani 1 1 d . . . C2B C 0.25872(11) 0.32337(12) 0.5845(3) 0.0296(8) Uani 1 1 d . . . C3B C 0.27467(11) 0.28595(13) 0.5472(3) 0.0348(9) Uani 1 1 d . . . H3B H 0.2622 0.2580 0.5351 0.042 Uiso 1 1 calc R . . C4B C 0.31357(12) 0.29640(13) 0.5295(3) 0.0330(9) Uani 1 1 d . . . C5B C 0.33858(12) 0.26570(13) 0.4909(3) 0.0377(10) Uani 1 1 d . . . C6B C 0.37596(13) 0.27756(14) 0.4758(3) 0.0423(10) Uani 1 1 d . . . C7B C 0.40309(14) 0.24694(17) 0.4376(3) 0.0549(13) Uani 1 1 d . . . H7B H 0.3985 0.2165 0.4206 0.066 Uiso 1 1 calc R . . C8B C 0.43608(15) 0.27038(16) 0.4311(4) 0.0588(14) Uani 1 1 d . . . H8B H 0.4586 0.2594 0.4081 0.071 Uiso 1 1 calc R . . C9B C 0.43023(13) 0.31572(16) 0.4664(3) 0.0459(11) Uani 1 1 d . . . C10B C 0.45185(12) 0.38849(16) 0.5010(3) 0.0454(11) Uani 1 1 d . . . C11B C 0.48190(14) 0.42283(18) 0.5048(4) 0.0599(14) Uani 1 1 d . . . H11B H 0.5065 0.4196 0.4847 0.072 Uiso 1 1 calc R . . C12B C 0.46760(13) 0.46059(18) 0.5430(3) 0.0580(14) Uani 1 1 d . . . H12B H 0.4806 0.4881 0.5555 0.070 Uiso 1 1 calc R . . C13B C 0.42809(12) 0.44994(16) 0.5607(3) 0.0474(12) Uani 1 1 d . . . C14B C 0.40313(13) 0.48121(16) 0.5954(3) 0.0497(12) Uani 1 1 d . . . C15B C 0.36511(12) 0.46976(15) 0.6082(3) 0.0434(11) Uani 1 1 d . . . C16B C 0.33744(13) 0.50163(15) 0.6413(3) 0.0510(13) Uani 1 1 d . . . H16B H 0.3417 0.5325 0.6557 0.061 Uiso 1 1 calc R . . C17B C 0.30442(12) 0.47785(14) 0.6469(3) 0.0482(12) Uani 1 1 d . . . H17B H 0.2813 0.4892 0.6661 0.058 Uiso 1 1 calc R . . C18B C 0.31140(11) 0.43163(13) 0.6177(3) 0.0345(9) Uani 1 1 d . . . C19B C 0.21943(11) 0.32931(12) 0.6129(3) 0.0293(8) Uani 1 1 d . . . C20B C 0.21029(13) 0.36247(15) 0.6747(3) 0.0496(12) Uani 1 1 d . . . H20B H 0.2297 0.3813 0.7011 0.060 Uiso 1 1 calc R . . C21B C 0.17208(14) 0.36779(15) 0.6976(4) 0.0565(14) Uani 1 1 d . . . H21B H 0.1662 0.3907 0.7379 0.068 Uiso 1 1 calc R . . C22B C 0.14312(12) 0.33939(14) 0.6608(3) 0.0419(10) Uani 1 1 d . . . H22B H 0.1176 0.3434 0.6752 0.050 Uiso 1 1 calc R . . C23B C 0.15220(13) 0.30578(16) 0.6038(3) 0.0478(11) Uani 1 1 d . . . H23B H 0.1329 0.2860 0.5798 0.057 Uiso 1 1 calc R . . C24B C 0.18998(12) 0.30029(14) 0.5804(3) 0.0401(10) Uani 1 1 d . . . H24B H 0.1956 0.2765 0.5419 0.048 Uiso 1 1 calc R . . C25B C 0.32389(13) 0.21841(14) 0.4671(3) 0.0446(11) Uani 1 1 d . . . C26B C 0.30729(13) 0.20982(14) 0.3813(3) 0.0462(11) Uani 1 1 d . . . C27B C 0.29239(14) 0.16590(15) 0.3609(4) 0.0571(13) Uani 1 1 d . . . H27B H 0.2810 0.1600 0.3036 0.068 Uiso 1 1 calc R . . C28B C 0.29426(16) 0.13115(15) 0.4245(4) 0.0609(15) Uani 1 1 d . . . C29B C 0.31100(19) 0.13996(17) 0.5083(4) 0.0728(18) Uani 1 1 d . . . H29B H 0.3124 0.1166 0.5510 0.087 Uiso 1 1 calc R . . C30B C 0.32612(17) 0.18321(16) 0.5316(4) 0.0619(15) Uani 1 1 d . . . C31B C 0.30486(17) 0.24641(17) 0.3102(3) 0.0668(16) Uani 1 1 d . . . H31D H 0.2924 0.2732 0.3323 0.100 Uiso 1 1 calc R . . H31E H 0.2901 0.2351 0.2577 0.100 Uiso 1 1 calc R . . H31F H 0.3305 0.2543 0.2951 0.100 Uiso 1 1 calc R . . C32B C 0.27690(19) 0.08398(17) 0.4002(5) 0.097(2) Uani 1 1 d . . . H32D H 0.2825 0.0630 0.4492 0.145 Uiso 1 1 calc R . . H32E H 0.2879 0.0725 0.3476 0.145 Uiso 1 1 calc R . . H32F H 0.2493 0.0868 0.3885 0.145 Uiso 1 1 calc R . . C33B C 0.3431(2) 0.1911(2) 0.6257(4) 0.105(3) Uani 1 1 d . . . H33A H 0.3238 0.2044 0.6608 0.157 Uiso 1 1 calc R . . H33B H 0.3648 0.2118 0.6249 0.157 Uiso 1 1 calc R . . H33C H 0.3517 0.1623 0.6518 0.157 Uiso 1 1 calc R . . C34B C 0.41716(13) 0.52942(18) 0.6189(4) 0.0611(16) Uani 1 1 d . . . C35B C 0.43582(15) 0.5375(2) 0.7047(5) 0.083(2) Uani 1 1 d . . . C36B C 0.44720(18) 0.5832(3) 0.7257(5) 0.101(3) Uani 1 1 d . . . H36B H 0.4589 0.5896 0.7825 0.121 Uiso 1 1 calc R . . C37B C 0.44143(19) 0.6186(3) 0.6643(7) 0.118(4) Uani 1 1 d . . . C38B C 0.42274(16) 0.60945(19) 0.5806(5) 0.091(2) Uani 1 1 d . . . H38B H 0.4182 0.6333 0.5395 0.110 Uiso 1 1 calc R . . C39B C 0.41075(14) 0.56462(18) 0.5574(4) 0.0660(17) Uani 1 1 d . . . C40B C 0.44210(18) 0.5011(3) 0.7718(4) 0.102(3) Uani 1 1 d . . . H40D H 0.4181 0.4853 0.7786 0.153 Uiso 1 1 calc R . . H40E H 0.4514 0.5143 0.8283 0.153 Uiso 1 1 calc R . . H40F H 0.4609 0.4796 0.7527 0.153 Uiso 1 1 calc R . . C41B C 0.4547(2) 0.6671(2) 0.6906(7) 0.176(5) Uani 1 1 d . . . H41D H 0.4586 0.6692 0.7548 0.264 Uiso 1 1 calc R . . H41E H 0.4353 0.6889 0.6690 0.264 Uiso 1 1 calc R . . H41F H 0.4786 0.6737 0.6645 0.264 Uiso 1 1 calc R . . C42B C 0.39128(16) 0.55640(17) 0.4654(4) 0.0740(18) Uani 1 1 d . . . H42D H 0.4064 0.5351 0.4334 0.111 Uiso 1 1 calc R . . H42E H 0.3891 0.5850 0.4332 0.111 Uiso 1 1 calc R . . H42F H 0.3659 0.5438 0.4707 0.111 Uiso 1 1 calc R . . C1C C 0.20980(10) 0.39413(12) 0.3973(2) 0.0247(7) Uani 1 1 d . . . C2C C 0.24242(10) 0.42640(11) 0.4085(2) 0.0250(7) Uani 1 1 d . . . C3C C 0.22850(10) 0.46229(11) 0.4542(2) 0.0266(8) Uani 1 1 d . . . H3C H 0.2423 0.4887 0.4717 0.032 Uiso 1 1 calc R . . C4C C 0.18931(10) 0.45312(12) 0.4709(2) 0.0259(8) Uani 1 1 d . . . C5C C 0.16607(10) 0.48289(11) 0.5161(2) 0.0260(8) Uani 1 1 d . . . C6C C 0.12793(10) 0.47284(11) 0.5294(2) 0.0266(8) Uani 1 1 d . . . C7C C 0.10218(11) 0.50284(12) 0.5739(3) 0.0339(9) Uani 1 1 d . . . H7C H 0.1084 0.5314 0.5991 0.041 Uiso 1 1 calc R . . C8C C 0.06761(12) 0.48193(13) 0.5721(3) 0.0400(10) Uani 1 1 d . . . H8C H 0.0453 0.4932 0.5953 0.048 Uiso 1 1 calc R . . C9C C 0.07184(11) 0.43835(12) 0.5268(3) 0.0296(8) Uani 1 1 d . . . C10C C 0.04638(10) 0.36910(12) 0.4766(2) 0.0268(8) Uani 1 1 d . . . C11C C 0.01466(11) 0.33690(12) 0.4662(3) 0.0315(9) Uani 1 1 d . . . H11C H -0.0103 0.3413 0.4840 0.038 Uiso 1 1 calc R . . C12C C 0.02795(10) 0.29943(12) 0.4258(3) 0.0301(8) Uani 1 1 d . . . H12C H 0.0140 0.2728 0.4105 0.036 Uiso 1 1 calc R . . C13C C 0.06767(10) 0.30817(11) 0.4108(2) 0.0248(7) Uani 1 1 d . . . C14C C 0.09191(10) 0.27694(11) 0.3725(2) 0.0250(7) Uani 1 1 d . . . C15C C 0.12976(10) 0.28752(12) 0.3577(2) 0.0274(8) Uani 1 1 d . . . C16C C 0.15563(11) 0.25683(13) 0.3160(3) 0.0398(10) Uani 1 1 d . . . H16C H 0.1503 0.2268 0.2970 0.048 Uiso 1 1 calc R . . C17C C 0.18899(12) 0.27981(13) 0.3096(3) 0.0422(11) Uani 1 1 d . . . H17C H 0.2110 0.2691 0.2843 0.051 Uiso 1 1 calc R . . C18C C 0.18405(11) 0.32436(12) 0.3496(3) 0.0286(8) Uani 1 1 d . . . C19C C 0.28149(11) 0.42010(11) 0.3785(2) 0.0261(8) Uani 1 1 d . . . C20C C 0.30625(13) 0.45723(14) 0.3786(3) 0.0521(13) Uani 1 1 d . . . H20C H 0.2974 0.4861 0.3949 0.063 Uiso 1 1 calc R . . C21C C 0.34385(14) 0.45261(16) 0.3552(4) 0.0601(15) Uani 1 1 d . . . H21C H 0.3599 0.4783 0.3566 0.072 Uiso 1 1 calc R . . C22C C 0.35787(12) 0.41129(14) 0.3302(3) 0.0395(10) Uani 1 1 d . . . H22C H 0.3832 0.4084 0.3140 0.047 Uiso 1 1 calc R . . C23C C 0.33375(13) 0.37432(15) 0.3296(3) 0.0530(13) Uani 1 1 d . . . H23C H 0.3428 0.3456 0.3133 0.064 Uiso 1 1 calc R . . C24C C 0.29606(12) 0.37867(14) 0.3528(3) 0.0500(12) Uani 1 1 d . . . H24C H 0.2801 0.3528 0.3509 0.060 Uiso 1 1 calc R . . C25C C 0.18283(10) 0.52811(11) 0.5508(3) 0.0273(8) Uani 1 1 d . . . C26C C 0.19789(11) 0.53152(13) 0.6406(3) 0.0317(8) Uani 1 1 d . . . C27C C 0.21289(12) 0.57351(13) 0.6717(3) 0.0384(10) Uani 1 1 d . . . H27C H 0.2228 0.5760 0.7312 0.046 Uiso 1 1 calc R . . C28C C 0.21352(13) 0.61180(14) 0.6165(3) 0.0416(10) Uani 1 1 d . . . C29C C 0.19850(13) 0.60749(13) 0.5281(3) 0.0414(10) Uani 1 1 d . . . H29C H 0.1986 0.6331 0.4906 0.050 Uiso 1 1 calc R . . C30C C 0.18335(11) 0.56621(12) 0.4937(3) 0.0311(8) Uani 1 1 d . . . C31C C 0.19748(13) 0.49070(14) 0.7030(3) 0.0436(11) Uani 1 1 d . . . H31G H 0.2104 0.4987 0.7602 0.065 Uiso 1 1 calc R . . H31H H 0.2107 0.4653 0.6777 0.065 Uiso 1 1 calc R . . H31I H 0.1711 0.4821 0.7109 0.065 Uiso 1 1 calc R . . C32C C 0.22943(15) 0.65751(15) 0.6518(4) 0.0616(15) Uani 1 1 d . . . H32G H 0.2106 0.6722 0.6862 0.092 Uiso 1 1 calc R . . H32H H 0.2349 0.6769 0.6023 0.092 Uiso 1 1 calc R . . H32I H 0.2528 0.6523 0.6893 0.092 Uiso 1 1 calc R . . C33C C 0.16797(13) 0.56310(13) 0.3963(3) 0.0409(10) Uani 1 1 d . . . H33D H 0.1602 0.5931 0.3750 0.061 Uiso 1 1 calc R . . H33E H 0.1460 0.5428 0.3910 0.061 Uiso 1 1 calc R . . H33F H 0.1879 0.5514 0.3611 0.061 Uiso 1 1 calc R . . C34C C 0.07672(10) 0.22993(11) 0.3457(3) 0.0265(8) Uani 1 1 d . . . C35C C 0.05670(11) 0.22286(13) 0.2623(3) 0.0321(9) Uani 1 1 d . . . C36C C 0.04390(11) 0.17883(13) 0.2386(3) 0.0369(10) Uani 1 1 d . . . H36C H 0.0304 0.1742 0.1830 0.044 Uiso 1 1 calc R . . C37C C 0.05079(11) 0.14149(13) 0.2958(3) 0.0401(10) Uani 1 1 d . . . C38C C 0.07051(11) 0.14916(12) 0.3788(3) 0.0351(9) Uani 1 1 d . . . H38C H 0.0751 0.1245 0.4179 0.042 Uiso 1 1 calc R . . C39C C 0.08356(11) 0.19268(12) 0.4054(3) 0.0295(8) Uani 1 1 d . . . C40C C 0.04925(13) 0.26226(15) 0.1973(3) 0.0484(11) Uani 1 1 d . . . H40G H 0.0410 0.2503 0.1390 0.073 Uiso 1 1 calc R . . H40H H 0.0727 0.2797 0.1936 0.073 Uiso 1 1 calc R . . H40I H 0.0294 0.2818 0.2179 0.073 Uiso 1 1 calc R . . C41C C 0.03712(14) 0.09360(14) 0.2695(4) 0.0591(14) Uani 1 1 d . . . H41G H 0.0586 0.0726 0.2762 0.089 Uiso 1 1 calc R . . H41H H 0.0266 0.0937 0.2081 0.089 Uiso 1 1 calc R . . H41I H 0.0175 0.0841 0.3076 0.089 Uiso 1 1 calc R . . C42C C 0.10496(13) 0.19962(13) 0.4952(3) 0.0407(10) Uani 1 1 d . . . H42G H 0.1060 0.1710 0.5276 0.061 Uiso 1 1 calc R . . H42H H 0.0917 0.2223 0.5284 0.061 Uiso 1 1 calc R . . H42I H 0.1308 0.2100 0.4873 0.061 Uiso 1 1 calc R . . C1CS C 0.06469(16) 0.39730(14) 0.2218(3) 0.0510(12) Uani 1 1 d . . . C1D C 0.20821(10) 0.61450(11) 0.9286(2) 0.0211(7) Uani 1 1 d . . . C2D C 0.23759(10) 0.57821(11) 0.9279(2) 0.0230(7) Uani 1 1 d . . . C3D C 0.22059(10) 0.54069(11) 0.9635(2) 0.0258(8) Uani 1 1 d . . . H3D H 0.2319 0.5119 0.9728 0.031 Uiso 1 1 calc R . . C4D C 0.18244(10) 0.55332(11) 0.9839(2) 0.0249(7) Uani 1 1 d . . . C5D C 0.15648(11) 0.52333(11) 1.0209(2) 0.0268(8) Uani 1 1 d . . . C6D C 0.11977(11) 0.53684(11) 1.0385(2) 0.0286(8) Uani 1 1 d . . . C7D C 0.09164(12) 0.50675(13) 1.0752(3) 0.0371(10) Uani 1 1 d . . . H7D H 0.0954 0.4760 1.0914 0.044 Uiso 1 1 calc R . . C8D C 0.05883(12) 0.53164(13) 1.0817(3) 0.0418(11) Uani 1 1 d . . . H8D H 0.0357 0.5214 1.1028 0.050 Uiso 1 1 calc R . . C9D C 0.06692(11) 0.57718(12) 1.0492(3) 0.0310(8) Uani 1 1 d . . . C10D C 0.04795(10) 0.65147(11) 1.0184(2) 0.0268(8) Uani 1 1 d . . . C11D C 0.01881(11) 0.68707(12) 1.0157(3) 0.0320(9) Uani 1 1 d . . . H11D H -0.0063 0.6844 1.0336 0.038 Uiso 1 1 calc R . . C12D C 0.03499(10) 0.72477(12) 0.9824(2) 0.0279(8) Uani 1 1 d . . . H12D H 0.0231 0.7533 0.9727 0.033 Uiso 1 1 calc R . . C13D C 0.07387(10) 0.71300(11) 0.9644(2) 0.0243(7) Uani 1 1 d . . . C14D C 0.10017(10) 0.74370(11) 0.9325(2) 0.0243(7) Uani 1 1 d . . . C15D C 0.13747(10) 0.73064(11) 0.9176(2) 0.0226(7) Uani 1 1 d . . . C16D C 0.16619(11) 0.76090(12) 0.8860(3) 0.0315(9) Uani 1 1 d . . . H16D H 0.1632 0.7922 0.8741 0.038 Uiso 1 1 calc R . . C17D C 0.19842(11) 0.73572(12) 0.8768(3) 0.0339(9) Uani 1 1 d . . . H17D H 0.2218 0.7461 0.8571 0.041 Uiso 1 1 calc R . . C18D C 0.18933(10) 0.68953(11) 0.9037(2) 0.0239(7) Uani 1 1 d . . . C19D C 0.27673(10) 0.58130(11) 0.8959(2) 0.0250(8) Uani 1 1 d . . . C20D C 0.29706(13) 0.54094(13) 0.8829(3) 0.0454(11) Uani 1 1 d . . . H20D H 0.2855 0.5128 0.8935 0.054 Uiso 1 1 calc R . . C21D C 0.33397(13) 0.54181(15) 0.8547(3) 0.0538(13) Uani 1 1 d . . . H21D H 0.3470 0.5143 0.8467 0.065 Uiso 1 1 calc R . . C22D C 0.35183(12) 0.58294(14) 0.8381(3) 0.0387(10) Uani 1 1 d . . . H22D H 0.3770 0.5835 0.8201 0.046 Uiso 1 1 calc R . . C23D C 0.33196(12) 0.62305(13) 0.8486(3) 0.0403(10) Uani 1 1 d . . . H23D H 0.3435 0.6511 0.8366 0.048 Uiso 1 1 calc R . . C24D C 0.29484(11) 0.62228(13) 0.8769(3) 0.0362(9) Uani 1 1 d . . . H24D H 0.2817 0.6499 0.8832 0.043 Uiso 1 1 calc R . . C25D C 0.16922(11) 0.47423(11) 1.0385(3) 0.0280(8) Uani 1 1 d . . . C26D C 0.19035(11) 0.46232(13) 1.1193(3) 0.0354(9) Uani 1 1 d . . . C27D C 0.20383(12) 0.41732(13) 1.1296(3) 0.0422(10) Uani 1 1 d . . . H27D H 0.2182 0.4092 1.1825 0.051 Uiso 1 1 calc R . . C28D C 0.19660(13) 0.38412(13) 1.0636(3) 0.0450(11) Uani 1 1 d . . . C29D C 0.17484(12) 0.39632(13) 0.9857(3) 0.0398(10) Uani 1 1 d . . . H29D H 0.1695 0.3743 0.9413 0.048 Uiso 1 1 calc R . . C30D C 0.16076(11) 0.44102(12) 0.9722(3) 0.0318(9) Uani 1 1 d . . . C31D C 0.19730(14) 0.49660(15) 1.1941(3) 0.0485(12) Uani 1 1 d . . . H31J H 0.2134 0.4829 1.2422 0.073 Uiso 1 1 calc R . . H31K H 0.1729 0.5055 1.2155 0.073 Uiso 1 1 calc R . . H31L H 0.2101 0.5232 1.1722 0.073 Uiso 1 1 calc R . . C32D C 0.21176(15) 0.33546(14) 1.0783(4) 0.0615(15) Uani 1 1 d . . . H32J H 0.1922 0.3169 1.1030 0.092 Uiso 1 1 calc R . . H32K H 0.2346 0.3361 1.1192 0.092 Uiso 1 1 calc R . . H32L H 0.2181 0.3227 1.0220 0.092 Uiso 1 1 calc R . . C33D C 0.13623(14) 0.45307(14) 0.8883(3) 0.0450(11) Uani 1 1 d . . . H33G H 0.1367 0.4281 0.8463 0.068 Uiso 1 1 calc R . . H33H H 0.1463 0.4804 0.8622 0.068 Uiso 1 1 calc R . . H33I H 0.1100 0.4585 0.9028 0.068 Uiso 1 1 calc R . . C34D C 0.08755(10) 0.79235(11) 0.9131(3) 0.0262(8) Uani 1 1 d . . . C35D C 0.09557(11) 0.82678(12) 0.9781(3) 0.0298(8) Uani 1 1 d . . . C36D C 0.08456(11) 0.87175(12) 0.9578(3) 0.0329(9) Uani 1 1 d . . . H36D H 0.0897 0.8945 1.0010 0.040 Uiso 1 1 calc R . . C37D C 0.06639(11) 0.88400(12) 0.8761(3) 0.0343(9) Uani 1 1 d . . . C38D C 0.05859(11) 0.84956(12) 0.8125(3) 0.0331(9) Uani 1 1 d . . . H38D H 0.0463 0.8573 0.7569 0.040 Uiso 1 1 calc R . . C39D C 0.06866(10) 0.80401(12) 0.8301(3) 0.0269(8) Uani 1 1 d . . . C40D C 0.11556(13) 0.81530(13) 1.0684(3) 0.0401(10) Uani 1 1 d . . . H40J H 0.1199 0.8431 1.1026 0.060 Uiso 1 1 calc R . . H40K H 0.1400 0.8007 1.0603 0.060 Uiso 1 1 calc R . . H40L H 0.0996 0.7948 1.0998 0.060 Uiso 1 1 calc R . . C41D C 0.05512(13) 0.93384(13) 0.8569(4) 0.0529(13) Uani 1 1 d . . . H41J H 0.0307 0.9402 0.8807 0.079 Uiso 1 1 calc R . . H41K H 0.0529 0.9389 0.7932 0.079 Uiso 1 1 calc R . . H41L H 0.0746 0.9539 0.8846 0.079 Uiso 1 1 calc R . . C42D C 0.05993(12) 0.76771(13) 0.7582(3) 0.0386(10) Uani 1 1 d . . . H42J H 0.0400 0.7475 0.7764 0.058 Uiso 1 1 calc R . . H42K H 0.0830 0.7503 0.7500 0.058 Uiso 1 1 calc R . . H42L H 0.0512 0.7824 0.7027 0.058 Uiso 1 1 calc R . . C1SA C 0.43456(19) 0.6568(2) 0.2516(4) 0.0790(18) Uani 1 1 d . . . C1SB C 0.43102(18) 0.34570(18) 0.7444(4) 0.0723(16) Uani 1 1 d . . . C1SD C 0.07114(16) 0.59052(17) 0.7886(3) 0.0576(13) Uani 1 1 d . . . Cl10 Cl 0.04121(5) 0.61703(7) 0.70155(12) 0.0979(6) Uani 1 1 d . . . Cl11 Cl 0.11922(4) 0.58918(5) 0.75898(9) 0.0672(4) Uani 1 1 d . . . Cl12 Cl 0.05376(5) 0.53507(5) 0.80757(11) 0.0796(4) Uani 1 1 d . . . Cl1S Cl 0.44459(6) 0.71258(6) 0.21732(11) 0.0904(5) Uani 1 1 d . . . Cl2S Cl 0.38606(5) 0.65259(6) 0.28137(12) 0.0906(5) Uani 1 1 d . . . Cl3S Cl 0.46588(5) 0.64199(7) 0.34467(15) 0.1167(7) Uani 1 1 d . . . Cl4S Cl 0.43989(5) 0.29026(5) 0.70654(10) 0.0839(5) Uani 1 1 d . . . Cl5S Cl 0.46249(6) 0.35780(7) 0.83929(14) 0.1144(7) Uani 1 1 d . . . Cl6S Cl 0.38241(5) 0.35071(6) 0.77436(12) 0.0880(5) Uani 1 1 d . . . Cl7S Cl 0.11344(4) 0.39267(4) 0.19493(8) 0.0580(3) Uani 1 1 d . . . Cl8S Cl 0.03356(4) 0.39444(5) 0.12351(9) 0.0633(4) Uani 1 1 d . . . Cl9S Cl 0.05772(4) 0.44889(4) 0.27927(8) 0.0594(3) Uani 1 1 d . . . N1A N 0.32695(9) 0.66042(9) 0.0695(2) 0.0272(7) Uani 1 1 d . . . N2A N 0.39681(9) 0.68084(10) 0.0052(2) 0.0318(7) Uani 1 1 d . . . N3A N 0.42146(9) 0.59440(11) 0.0428(2) 0.0366(8) Uani 1 1 d . . . N4A N 0.35155(9) 0.57310(10) 0.1017(2) 0.0346(8) Uani 1 1 d . . . N5A N 0.28837(9) 0.60152(10) 0.1348(2) 0.0347(8) Uani 1 1 d . . . N6A N 0.46125(10) 0.65325(12) -0.0203(3) 0.0445(9) Uani 1 1 d . . . N1C N 0.17776(8) 0.41108(9) 0.43583(19) 0.0244(6) Uani 1 1 d . . . N2C N 0.10867(8) 0.43299(9) 0.50081(19) 0.0248(6) Uani 1 1 d . . . N3C N 0.07871(8) 0.35165(9) 0.44170(19) 0.0243(6) Uani 1 1 d . . . N4C N 0.14797(8) 0.32899(9) 0.37897(19) 0.0237(6) Uani 1 1 d . . . N5C N 0.21324(9) 0.35450(10) 0.3562(2) 0.0289(7) Uani 1 1 d . . . N6C N 0.04209(9) 0.40963(10) 0.5163(2) 0.0338(8) Uani 1 1 d . . . N1D N 0.32309(9) 0.34071(10) 0.5556(2) 0.0315(7) Uani 1 1 d . . . N2D N 0.34845(9) 0.42706(11) 0.5928(2) 0.0351(8) Uani 1 1 d . . . N3D N 0.41871(9) 0.40544(12) 0.5357(2) 0.0403(8) Uani 1 1 d . . . N4D N 0.39328(10) 0.31986(11) 0.4939(2) 0.0367(8) Uani 1 1 d . . . N5D N 0.28402(9) 0.39995(10) 0.6180(2) 0.0329(7) Uani 1 1 d . . . N6D N 0.45762(11) 0.34674(14) 0.4684(3) 0.0500(10) Uani 1 1 d . . . N7D N 0.17480(8) 0.59862(9) 0.96242(18) 0.0210(6) Uani 1 1 d . . . N8D N 0.10405(8) 0.58035(9) 1.0225(2) 0.0254(6) Uani 1 1 d . . . N9D N 0.08144(8) 0.66744(9) 0.98638(19) 0.0224(6) Uani 1 1 d . . . N10D N 0.15240(8) 0.68683(9) 0.92968(19) 0.0213(6) Uani 1 1 d . . . N11D N 0.04040(9) 0.60982(10) 1.0485(2) 0.0325(7) Uani 1 1 d . . . N12D N 0.21565(8) 0.65652(9) 0.9001(2) 0.0253(6) Uani 1 1 d . . . Ni1A Ni 0.374030(13) 0.627224(16) 0.05467(3) 0.02997(12) Uani 1 1 d . . . Ni1B Ni 0.370775(14) 0.373247(17) 0.54423(3) 0.03201(13) Uani 1 1 d . . . Ni3C Ni 0.128299(13) 0.381206(14) 0.43947(3) 0.02170(11) Uani 1 1 d . . . Ni4D Ni 0.128500(12) 0.633385(14) 0.97621(3) 0.02023(11) Uani 1 1 d . . . 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 C30A 0.043(3) 0.040(3) 0.102(4) 0.030(3) 0.035(3) 0.015(2) C1A 0.025(2) 0.0254(18) 0.032(2) 0.0080(15) 0.0021(15) 0.0023(14) C2A 0.0229(19) 0.0210(17) 0.0282(19) 0.0024(14) -0.0028(14) 0.0028(13) C3A 0.028(2) 0.0209(17) 0.030(2) 0.0036(14) -0.0010(15) 0.0026(14) C4A 0.027(2) 0.0237(18) 0.0276(19) 0.0066(14) -0.0026(15) 0.0012(14) C5A 0.033(2) 0.0241(18) 0.031(2) 0.0091(15) 0.0016(16) -0.0004(15) C6A 0.032(2) 0.029(2) 0.040(2) 0.0104(16) 0.0041(17) -0.0010(16) C7A 0.042(3) 0.035(2) 0.066(3) 0.018(2) 0.015(2) -0.0047(19) C8A 0.043(3) 0.041(3) 0.078(4) 0.023(2) 0.021(2) -0.003(2) C9A 0.029(2) 0.036(2) 0.056(3) 0.0149(19) 0.0091(19) -0.0007(17) C10A 0.029(2) 0.038(2) 0.057(3) 0.019(2) 0.0101(19) 0.0044(17) C11A 0.025(2) 0.056(3) 0.075(3) 0.017(2) 0.019(2) 0.009(2) C12A 0.029(2) 0.049(3) 0.082(4) 0.023(2) 0.019(2) 0.015(2) C13A 0.025(2) 0.042(2) 0.065(3) 0.023(2) 0.010(2) 0.0119(17) C14A 0.028(2) 0.041(2) 0.072(3) 0.024(2) 0.017(2) 0.0139(18) C15A 0.028(2) 0.034(2) 0.071(3) 0.023(2) 0.013(2) 0.0094(17) C16A 0.036(3) 0.038(2) 0.105(4) 0.033(3) 0.030(3) 0.0144(19) C17A 0.034(3) 0.036(2) 0.111(4) 0.035(3) 0.030(3) 0.0118(19) C18A 0.026(2) 0.026(2) 0.070(3) 0.0210(19) 0.010(2) 0.0048(16) C19A 0.0243(19) 0.0260(18) 0.0217(18) 0.0011(14) -0.0037(14) 0.0034(14) C20A 0.029(2) 0.026(2) 0.051(3) 0.0049(17) 0.0068(18) 0.0036(15) C21A 0.031(2) 0.031(2) 0.041(2) 0.0032(17) 0.0063(17) 0.0023(16) C22A 0.028(2) 0.041(2) 0.032(2) 0.0053(17) 0.0064(16) 0.0073(17) C23A 0.046(3) 0.036(2) 0.057(3) 0.011(2) 0.020(2) 0.0185(19) C24A 0.041(3) 0.0233(19) 0.054(3) 0.0090(17) 0.013(2) 0.0080(16) C25A 0.033(3) 0.048(3) 0.080(4) 0.034(3) 0.027(2) 0.018(2) C26A 0.028(3) 0.076(4) 0.086(4) 0.041(3) 0.026(3) 0.019(2) C27A 0.036(3) 0.088(4) 0.111(5) 0.071(4) 0.032(3) 0.027(3) C28A 0.048(4) 0.061(4) 0.158(7) 0.058(4) 0.056(4) 0.029(3) C29A 0.052(3) 0.041(3) 0.141(6) 0.041(3) 0.046(4) 0.021(2) C42A 0.045(4) 0.119(6) 0.085(5) 0.048(4) 0.009(3) 0.021(3) C31A 0.093(5) 0.074(5) 0.253(10) 0.101(6) 0.065(6) 0.053(4) C32A 0.070(4) 0.042(3) 0.099(5) 0.020(3) 0.028(3) 0.009(3) C33A 0.038(2) 0.0206(18) 0.040(2) 0.0073(15) 0.0133(18) 0.0025(15) C34A 0.037(2) 0.027(2) 0.040(2) 0.0051(17) 0.0077(18) 0.0062(16) C35A 0.041(3) 0.037(2) 0.053(3) 0.014(2) 0.010(2) 0.0117(19) C36A 0.055(3) 0.024(2) 0.075(4) 0.019(2) 0.033(3) 0.0106(19) C37A 0.076(4) 0.023(2) 0.064(3) -0.001(2) 0.036(3) -0.008(2) C38A 0.063(3) 0.029(2) 0.040(2) 0.0029(18) 0.018(2) -0.0118(19) C39A 0.058(3) 0.042(2) 0.037(2) 0.0021(19) -0.001(2) 0.013(2) C40A 0.080(4) 0.029(3) 0.130(5) 0.031(3) 0.040(4) 0.023(2) C41A 0.116(5) 0.041(3) 0.046(3) 0.000(2) 0.006(3) -0.026(3) C1B 0.025(2) 0.031(2) 0.035(2) -0.0108(16) 0.0004(16) 0.0009(15) C2B 0.027(2) 0.0224(18) 0.039(2) -0.0041(15) -0.0017(16) -0.0012(14) C3B 0.033(2) 0.0256(19) 0.045(2) -0.0088(17) -0.0029(18) -0.0009(16) C4B 0.033(2) 0.030(2) 0.035(2) -0.0091(16) -0.0043(17) 0.0016(16) C5B 0.037(2) 0.034(2) 0.043(2) -0.0128(18) 0.0050(19) 0.0030(17) C6B 0.044(3) 0.037(2) 0.046(3) -0.0139(19) 0.006(2) 0.0083(19) C7B 0.049(3) 0.047(3) 0.071(3) -0.019(2) 0.017(3) 0.011(2) C8B 0.050(3) 0.055(3) 0.074(4) -0.018(3) 0.024(3) 0.017(2) C9B 0.032(3) 0.054(3) 0.053(3) -0.018(2) 0.009(2) 0.006(2) C10B 0.027(2) 0.056(3) 0.054(3) -0.021(2) 0.007(2) 0.0008(19) C11B 0.029(3) 0.078(4) 0.074(4) -0.031(3) 0.016(2) -0.011(2) C12B 0.028(3) 0.070(3) 0.078(4) -0.032(3) 0.018(2) -0.017(2) C13B 0.026(2) 0.060(3) 0.057(3) -0.025(2) 0.010(2) -0.013(2) C14B 0.032(3) 0.056(3) 0.063(3) -0.028(2) 0.015(2) -0.019(2) C15B 0.029(2) 0.046(3) 0.057(3) -0.025(2) 0.015(2) -0.0122(18) C16B 0.035(3) 0.041(2) 0.079(4) -0.030(2) 0.022(2) -0.0147(19) C17B 0.031(2) 0.035(2) 0.081(3) -0.028(2) 0.021(2) -0.0085(18) C18B 0.024(2) 0.029(2) 0.052(3) -0.0170(17) 0.0073(17) -0.0051(15) C19B 0.026(2) 0.0246(18) 0.036(2) 0.0008(15) -0.0014(16) -0.0014(14) C20B 0.034(3) 0.039(2) 0.077(3) -0.017(2) 0.013(2) -0.0100(19) C21B 0.042(3) 0.035(2) 0.096(4) -0.012(2) 0.027(3) -0.002(2) C22B 0.027(2) 0.043(2) 0.056(3) 0.018(2) 0.0079(19) -0.0024(18) C23B 0.037(3) 0.054(3) 0.052(3) -0.006(2) 0.001(2) -0.019(2) C24B 0.036(2) 0.036(2) 0.048(3) -0.0122(19) 0.0034(19) -0.0113(18) C25B 0.052(3) 0.027(2) 0.058(3) -0.0120(19) 0.020(2) 0.0048(18) C26B 0.048(3) 0.032(2) 0.059(3) -0.011(2) 0.010(2) -0.0078(19) C27B 0.053(3) 0.039(3) 0.080(4) -0.020(2) 0.009(3) -0.007(2) C28B 0.067(4) 0.028(2) 0.093(4) -0.005(3) 0.037(3) -0.001(2) C29B 0.109(5) 0.036(3) 0.079(4) 0.006(3) 0.045(4) 0.024(3) C30B 0.091(4) 0.035(3) 0.064(3) -0.004(2) 0.025(3) 0.022(3) C31B 0.090(4) 0.056(3) 0.052(3) -0.011(2) -0.008(3) -0.020(3) C32B 0.103(5) 0.033(3) 0.160(7) -0.016(3) 0.046(5) -0.016(3) C33B 0.187(8) 0.064(4) 0.061(4) -0.003(3) 0.002(4) 0.059(4) C34B 0.029(3) 0.065(3) 0.093(4) -0.044(3) 0.032(3) -0.022(2) C35B 0.032(3) 0.124(6) 0.095(5) -0.073(4) 0.027(3) -0.034(3) C36B 0.047(4) 0.133(6) 0.128(6) -0.102(5) 0.045(4) -0.046(4) C37B 0.046(4) 0.103(6) 0.215(10) -0.111(6) 0.066(5) -0.046(4) C38B 0.050(4) 0.053(3) 0.179(7) -0.059(4) 0.059(4) -0.024(3) C39B 0.039(3) 0.052(3) 0.113(5) -0.044(3) 0.042(3) -0.020(2) C40B 0.055(4) 0.180(8) 0.072(5) -0.056(5) 0.011(3) -0.036(4) C41B 0.088(6) 0.107(6) 0.341(14) -0.156(8) 0.065(7) -0.055(5) C42B 0.067(4) 0.046(3) 0.113(5) -0.024(3) 0.033(4) -0.011(3) C1C 0.0219(19) 0.0233(17) 0.0289(19) -0.0015(14) 0.0031(14) -0.0027(14) C2C 0.0227(19) 0.0214(17) 0.031(2) -0.0014(14) 0.0004(15) -0.0033(13) C3C 0.0234(19) 0.0180(16) 0.038(2) -0.0041(14) 0.0017(15) -0.0073(13) C4C 0.0237(19) 0.0247(18) 0.0289(19) -0.0047(14) -0.0001(15) -0.0026(14) C5C 0.027(2) 0.0218(17) 0.0289(19) -0.0048(14) 0.0018(15) -0.0027(14) C6C 0.027(2) 0.0230(18) 0.030(2) -0.0069(14) 0.0010(15) -0.0025(14) C7C 0.030(2) 0.0257(19) 0.047(2) -0.0146(17) 0.0092(18) -0.0025(15) C8C 0.034(2) 0.033(2) 0.055(3) -0.0140(19) 0.014(2) -0.0007(17) C9C 0.028(2) 0.0237(18) 0.038(2) -0.0033(15) 0.0079(16) -0.0017(15) C10C 0.0222(19) 0.0237(18) 0.035(2) -0.0015(15) 0.0037(15) -0.0014(14) C11C 0.019(2) 0.030(2) 0.046(2) -0.0024(17) 0.0100(16) -0.0050(15) C12C 0.022(2) 0.0259(19) 0.043(2) 0.0010(16) 0.0042(16) -0.0075(14) C13C 0.0236(19) 0.0210(17) 0.0297(19) 0.0028(14) 0.0019(15) -0.0047(13) C14C 0.0224(19) 0.0213(17) 0.032(2) -0.0009(14) 0.0024(15) -0.0048(13) C15C 0.023(2) 0.0227(18) 0.037(2) -0.0048(15) 0.0023(15) -0.0053(14) C16C 0.031(2) 0.027(2) 0.063(3) -0.0185(19) 0.014(2) -0.0062(16) C17C 0.033(2) 0.029(2) 0.066(3) -0.0236(19) 0.018(2) -0.0066(17) C18C 0.025(2) 0.0221(18) 0.040(2) -0.0092(15) 0.0086(16) -0.0044(14) C19C 0.027(2) 0.0216(17) 0.030(2) -0.0039(14) 0.0052(15) -0.0039(14) C20C 0.046(3) 0.030(2) 0.084(4) -0.024(2) 0.029(2) -0.0159(19) C21C 0.046(3) 0.048(3) 0.091(4) -0.025(3) 0.031(3) -0.025(2) C22C 0.033(2) 0.041(2) 0.046(3) -0.0024(19) 0.0147(19) -0.0050(18) C23C 0.034(3) 0.040(3) 0.088(4) -0.024(2) 0.023(2) -0.0057(19) C24C 0.028(2) 0.034(2) 0.090(4) -0.025(2) 0.018(2) -0.0102(17) C25C 0.024(2) 0.0199(17) 0.038(2) -0.0090(15) 0.0059(16) -0.0014(13) C26C 0.029(2) 0.031(2) 0.035(2) -0.0104(16) 0.0052(16) -0.0045(15) C27C 0.038(2) 0.037(2) 0.040(2) -0.0152(18) 0.0055(18) -0.0074(18) C28C 0.040(3) 0.031(2) 0.055(3) -0.0201(19) 0.008(2) -0.0067(17) C29C 0.046(3) 0.0213(19) 0.058(3) -0.0066(18) 0.016(2) 0.0008(17) C30C 0.028(2) 0.0217(18) 0.044(2) -0.0078(16) 0.0056(17) 0.0022(14) C31C 0.050(3) 0.045(3) 0.036(2) -0.0007(19) 0.002(2) -0.007(2) C32C 0.073(4) 0.035(3) 0.077(4) -0.024(2) 0.010(3) -0.018(2) C33C 0.046(3) 0.031(2) 0.046(3) 0.0006(18) 0.002(2) 0.0020(18) C34C 0.0179(18) 0.0220(17) 0.040(2) -0.0060(15) 0.0028(15) -0.0054(13) C35C 0.023(2) 0.030(2) 0.044(2) -0.0040(17) 0.0045(17) -0.0063(15) C36C 0.022(2) 0.037(2) 0.052(3) -0.0191(19) 0.0002(18) -0.0050(16) C37C 0.023(2) 0.026(2) 0.072(3) -0.021(2) 0.007(2) -0.0075(15) C38C 0.026(2) 0.0208(18) 0.060(3) -0.0095(17) 0.0145(19) -0.0017(15) C39C 0.026(2) 0.0211(18) 0.042(2) -0.0040(15) 0.0079(16) -0.0045(14) C40C 0.047(3) 0.048(3) 0.048(3) 0.001(2) -0.006(2) -0.011(2) C41C 0.043(3) 0.031(2) 0.102(4) -0.026(2) -0.004(3) -0.0035(19) C42C 0.050(3) 0.029(2) 0.043(2) -0.0016(18) 0.001(2) -0.0027(18) C1CS 0.083(4) 0.033(2) 0.038(3) 0.0023(19) 0.012(2) -0.006(2) C1D 0.0216(18) 0.0175(16) 0.0244(18) -0.0014(13) 0.0021(14) 0.0029(13) C2D 0.0233(19) 0.0193(16) 0.0265(18) -0.0012(13) 0.0022(14) 0.0063(13) C3D 0.025(2) 0.0208(17) 0.032(2) 0.0026(14) 0.0029(15) 0.0042(14) C4D 0.027(2) 0.0189(16) 0.0283(19) 0.0031(14) 0.0016(15) 0.0027(13) C5D 0.032(2) 0.0176(16) 0.031(2) 0.0029(14) 0.0056(16) 0.0028(14) C6D 0.036(2) 0.0189(17) 0.032(2) 0.0060(14) 0.0071(16) 0.0015(15) C7D 0.034(2) 0.0231(19) 0.056(3) 0.0152(17) 0.0186(19) 0.0033(16) C8D 0.035(2) 0.028(2) 0.065(3) 0.0154(19) 0.021(2) 0.0034(17) C9D 0.027(2) 0.0234(18) 0.044(2) 0.0066(16) 0.0116(17) 0.0011(15) C10D 0.0198(19) 0.0224(18) 0.039(2) 0.0030(15) 0.0064(15) 0.0013(13) C11D 0.0183(19) 0.029(2) 0.049(2) 0.0010(17) 0.0098(17) 0.0027(14) C12D 0.023(2) 0.0228(18) 0.038(2) 0.0019(15) 0.0074(16) 0.0085(14) C13D 0.0208(19) 0.0228(17) 0.0295(19) -0.0007(14) 0.0030(14) 0.0030(13) C14D 0.0224(19) 0.0187(16) 0.032(2) 0.0010(14) 0.0028(15) 0.0056(13) C15D 0.0236(19) 0.0196(16) 0.0246(18) 0.0033(13) 0.0024(14) 0.0037(13) C16D 0.029(2) 0.0193(17) 0.047(2) 0.0095(16) 0.0107(17) 0.0040(14) C17D 0.026(2) 0.0197(18) 0.057(3) 0.0099(17) 0.0130(18) 0.0034(14) C18D 0.0212(19) 0.0181(16) 0.033(2) 0.0052(14) 0.0040(15) 0.0029(13) C19D 0.026(2) 0.0217(17) 0.0276(19) -0.0010(14) 0.0014(15) 0.0046(14) C20D 0.042(3) 0.025(2) 0.072(3) 0.008(2) 0.023(2) 0.0091(17) C21D 0.040(3) 0.036(2) 0.088(4) 0.010(2) 0.024(2) 0.020(2) C22D 0.031(2) 0.042(2) 0.045(2) 0.0009(19) 0.0127(18) 0.0068(18) C23D 0.032(2) 0.030(2) 0.061(3) 0.0039(19) 0.015(2) 0.0001(16) C24D 0.029(2) 0.0261(19) 0.055(3) 0.0028(17) 0.0135(18) 0.0056(15) C25D 0.027(2) 0.0193(17) 0.039(2) 0.0069(15) 0.0109(16) 0.0025(14) C26D 0.033(2) 0.0256(19) 0.048(3) 0.0103(17) 0.0050(18) 0.0045(16) C27D 0.037(3) 0.030(2) 0.060(3) 0.017(2) 0.004(2) 0.0086(17) C28D 0.040(3) 0.021(2) 0.076(3) 0.011(2) 0.018(2) 0.0079(17) C29D 0.042(3) 0.0235(19) 0.056(3) -0.0015(18) 0.017(2) -0.0039(17) C30D 0.032(2) 0.0256(19) 0.039(2) 0.0048(16) 0.0120(17) -0.0002(15) C31D 0.055(3) 0.042(3) 0.047(3) 0.009(2) -0.008(2) 0.006(2) C32D 0.058(3) 0.025(2) 0.102(4) 0.013(2) 0.011(3) 0.014(2) C33D 0.064(3) 0.033(2) 0.039(2) 0.0030(18) 0.008(2) -0.008(2) C34D 0.0189(19) 0.0182(17) 0.042(2) 0.0023(15) 0.0060(15) 0.0052(13) C35D 0.026(2) 0.0260(19) 0.038(2) 0.0023(16) 0.0041(16) 0.0018(15) C36D 0.024(2) 0.0247(19) 0.050(2) -0.0023(17) 0.0015(17) 0.0036(14) C37D 0.020(2) 0.0212(18) 0.061(3) 0.0063(17) 0.0000(18) 0.0012(14) C38D 0.024(2) 0.028(2) 0.047(2) 0.0112(17) -0.0009(17) 0.0032(15) C39D 0.0171(18) 0.0233(18) 0.041(2) 0.0036(15) 0.0054(15) 0.0009(13) C40D 0.046(3) 0.033(2) 0.041(2) 0.0006(18) 0.000(2) 0.0038(18) C41D 0.045(3) 0.027(2) 0.084(4) 0.007(2) -0.015(3) 0.0039(19) C42D 0.043(3) 0.033(2) 0.039(2) -0.0009(17) 0.0015(19) 0.0019(18) C1SA 0.079(5) 0.074(4) 0.085(4) -0.018(3) 0.009(3) 0.006(3) C1SB 0.083(5) 0.050(3) 0.084(4) 0.011(3) 0.007(3) -0.003(3) C1SD 0.073(4) 0.057(3) 0.042(3) 0.006(2) -0.003(2) 0.016(3) Cl10 0.0680(11) 0.1303(15) 0.0961(12) 0.0650(11) 0.0106(9) 0.0249(10) Cl11 0.0661(9) 0.0777(9) 0.0549(8) -0.0133(7) -0.0141(7) 0.0064(7) Cl12 0.0915(12) 0.0565(8) 0.0912(11) 0.0130(7) 0.0098(9) 0.0132(8) Cl1S 0.1166(15) 0.0842(11) 0.0697(10) 0.0009(8) 0.0021(10) 0.0075(10) Cl2S 0.0762(11) 0.0960(12) 0.0982(12) -0.0414(10) -0.0020(9) -0.0053(9) Cl3S 0.0712(12) 0.1328(17) 0.1487(19) 0.0631(14) 0.0244(12) 0.0293(11) Cl4S 0.1175(15) 0.0643(9) 0.0686(10) -0.0056(7) -0.0016(9) -0.0054(9) Cl5S 0.0809(13) 0.1303(16) 0.1349(17) -0.0691(14) 0.0257(11) -0.0350(11) Cl6S 0.0852(12) 0.0785(11) 0.0991(12) 0.0285(9) -0.0009(9) 0.0108(9) Cl7S 0.0668(9) 0.0521(7) 0.0543(7) 0.0097(6) -0.0012(6) 0.0121(6) Cl8S 0.0616(9) 0.0736(9) 0.0546(8) -0.0144(6) 0.0038(6) -0.0144(7) Cl9S 0.0874(10) 0.0433(7) 0.0480(7) -0.0051(5) 0.0074(6) -0.0015(6) N1A 0.0236(17) 0.0226(15) 0.0350(18) 0.0097(12) -0.0012(13) 0.0004(12) N2A 0.0237(18) 0.0315(17) 0.0405(19) 0.0084(14) 0.0038(14) -0.0007(13) N3A 0.0229(18) 0.0378(19) 0.050(2) 0.0151(15) 0.0078(15) 0.0047(14) N4A 0.0240(18) 0.0258(16) 0.055(2) 0.0138(15) 0.0089(15) 0.0059(13) N5A 0.0236(18) 0.0251(16) 0.056(2) 0.0155(15) 0.0095(15) 0.0044(13) N6A 0.028(2) 0.045(2) 0.062(2) 0.0163(18) 0.0127(17) 0.0005(15) N1C 0.0214(16) 0.0199(14) 0.0320(17) -0.0024(12) 0.0037(12) -0.0029(11) N2C 0.0240(17) 0.0209(15) 0.0300(16) -0.0029(12) 0.0054(12) -0.0024(11) N3C 0.0220(16) 0.0194(14) 0.0317(17) -0.0010(12) 0.0026(12) -0.0002(11) N4C 0.0221(16) 0.0192(14) 0.0301(16) -0.0009(12) 0.0043(12) -0.0044(11) N5C 0.0252(17) 0.0224(15) 0.0400(19) -0.0061(13) 0.0086(13) -0.0061(12) N6C 0.0275(18) 0.0262(16) 0.049(2) -0.0050(14) 0.0110(15) -0.0050(13) N1D 0.0246(18) 0.0308(17) 0.0386(19) -0.0098(14) -0.0004(14) 0.0032(13) N2D 0.0246(18) 0.0347(18) 0.047(2) -0.0168(15) 0.0057(15) -0.0049(13) N3D 0.0246(19) 0.049(2) 0.049(2) -0.0201(17) 0.0086(15) -0.0047(15) N4D 0.0302(19) 0.0385(19) 0.042(2) -0.0111(15) 0.0047(15) 0.0059(14) N5D 0.0251(18) 0.0287(17) 0.045(2) -0.0131(14) 0.0033(14) -0.0028(13) N6D 0.029(2) 0.064(3) 0.058(3) -0.018(2) 0.0095(17) 0.0052(18) N7D 0.0221(16) 0.0165(14) 0.0244(15) 0.0031(11) 0.0008(12) 0.0030(11) N8D 0.0242(17) 0.0170(14) 0.0355(17) 0.0027(12) 0.0058(13) 0.0020(11) N9D 0.0201(16) 0.0183(14) 0.0291(16) 0.0024(11) 0.0031(12) 0.0015(11) N10D 0.0200(15) 0.0158(13) 0.0284(16) 0.0003(11) 0.0039(12) 0.0039(11) N11D 0.0255(18) 0.0254(16) 0.048(2) 0.0034(14) 0.0113(14) 0.0018(13) N12D 0.0213(16) 0.0207(14) 0.0345(17) 0.0037(12) 0.0055(13) 0.0021(11) Ni1A 0.0192(3) 0.0278(2) 0.0432(3) 0.0140(2) 0.0043(2) 0.00270(18) Ni1B 0.0201(3) 0.0370(3) 0.0389(3) -0.0160(2) 0.0021(2) 0.0002(2) Ni3C 0.0198(2) 0.0171(2) 0.0284(2) -0.00190(17) 0.00359(18) -0.00248(16) Ni4D 0.0183(2) 0.0160(2) 0.0267(2) 0.00334(17) 0.00367(17) 0.00217(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C30A C29A 1.389(6) . ? C30A C25A 1.389(7) . ? C30A C32A 1.495(8) . ? C1A N5A 1.327(4) . ? C1A N1A 1.371(4) . ? C1A C2A 1.462(5) . ? C2A C3A 1.349(5) . ? C2A C19A 1.469(5) . ? C3A C4A 1.423(5) . ? C4A N1A 1.381(4) . ? C4A C5A 1.397(5) . ? C5A C6A 1.373(5) . ? C5A C33A 1.511(5) . ? C6A N2A 1.388(5) . ? C6A C7A 1.438(5) . ? C7A C8A 1.341(6) . ? C8A C9A 1.428(5) . ? C9A N6A 1.327(5) . ? C9A N2A 1.375(5) . ? C10A N6A 1.320(5) . ? C10A N3A 1.380(5) . ? C10A C11A 1.441(6) . ? C11A C12A 1.347(6) . ? C12A C13A 1.435(6) . ? C13A N3A 1.383(5) . ? C13A C14A 1.384(6) . ? C14A C15A 1.383(5) . ? C14A C25A 1.517(6) . ? C15A N4A 1.383(5) . ? C15A C16A 1.441(6) . ? C16A C17A 1.337(6) . ? C17A C18A 1.444(5) . ? C18A N5A 1.321(5) . ? C18A N4A 1.364(5) . ? C19A C20A 1.391(5) . ? C19A C24A 1.397(5) . ? C20A C21A 1.392(5) . ? C21A C22A 1.379(5) . ? C22A C23A 1.378(6) . ? C23A C24A 1.367(6) . ? C25A C26A 1.393(7) . ? C26A C27A 1.423(7) . ? C26A C42A 1.488(8) . ? C27A C28A 1.397(9) . ? C28A C29A 1.368(9) . ? C28A C31A 1.521(7) . ? C33A C38A 1.396(5) . ? C33A C34A 1.398(5) . ? C34A C35A 1.383(5) . ? C34A C39A 1.497(6) . ? C35A C36A 1.378(6) . ? C36A C37A 1.368(7) . ? C36A C40A 1.520(6) . ? C37A C38A 1.406(6) . ? C38A C41A 1.507(6) . ? C1B N5D 1.322(4) . ? C1B N1D 1.376(5) . ? C1B C2B 1.468(5) . ? C2B C3B 1.357(5) . ? C2B C19B 1.464(5) . ? C3B C4B 1.423(6) . ? C4B N1D 1.377(4) . ? C4B C5B 1.396(5) . ? C5B C6B 1.373(6) . ? C5B C25B 1.498(5) . ? C6B N4D 1.384(5) . ? C6B C7B 1.441(6) . ? C7B C8B 1.338(7) . ? C8B C9B 1.438(6) . ? C9B N6D 1.306(6) . ? C9B N4D 1.377(5) . ? C10B N6D 1.328(5) . ? C10B N3D 1.383(5) . ? C10B C11B 1.438(6) . ? C11B C12B 1.348(6) . ? C12B C13B 1.445(6) . ? C13B N3D 1.377(5) . ? C13B C14B 1.381(6) . ? C14B C15B 1.383(6) . ? C14B C34B 1.514(6) . ? C15B N2D 1.379(5) . ? C15B C16B 1.445(6) . ? C16B C17B 1.343(5) . ? C17B C18B 1.437(5) . ? C18B N5D 1.320(5) . ? C18B N2D 1.368(5) . ? C19B C24B 1.381(5) . ? C19B C20B 1.387(6) . ? C20B C21B 1.398(6) . ? C21B C22B 1.378(6) . ? C22B C23B 1.348(6) . ? C23B C24B 1.387(6) . ? C25B C26B 1.385(6) . ? C25B C30B 1.403(6) . ? C26B C27B 1.400(6) . ? C26B C31B 1.500(7) . ? C27B C28B 1.383(7) . ? C28B C29B 1.362(8) . ? C28B C32B 1.528(7) . ? C29B C30B 1.394(7) . ? C30B C33B 1.499(8) . ? C34B C39B 1.381(8) . ? C34B C35B 1.409(8) . ? C35B C36B 1.412(8) . ? C35B C40B 1.463(9) . ? C36B C37B 1.382(12) . ? C37B C38B 1.388(11) . ? C37B C41B 1.522(8) . ? C38B C39B 1.402(6) . ? C39B C42B 1.502(8) . ? C1C N5C 1.314(4) . ? C1C N1C 1.378(4) . ? C1C C2C 1.466(5) . ? C2C C3C 1.354(5) . ? C2C C19C 1.467(5) . ? C3C C4C 1.422(5) . ? C4C N1C 1.376(4) . ? C4C C5C 1.390(5) . ? C5C C6C 1.380(5) . ? C5C C25C 1.511(5) . ? C6C N2C 1.386(4) . ? C6C C7C 1.443(5) . ? C7C C8C 1.339(5) . ? C8C C9C 1.447(5) . ? C9C N6C 1.324(5) . ? C9C N2C 1.368(5) . ? C10C N6C 1.331(4) . ? C10C N3C 1.367(4) . ? C10C C11C 1.441(5) . ? C11C C12C 1.342(5) . ? C12C C13C 1.431(5) . ? C13C N3C 1.388(4) . ? C13C C14C 1.388(5) . ? C14C C15C 1.379(5) . ? C14C C34C 1.506(4) . ? C15C N4C 1.385(4) . ? C15C C16C 1.438(5) . ? C16C C17C 1.343(5) . ? C17C C18C 1.440(5) . ? C18C N5C 1.334(4) . ? C18C N4C 1.361(4) . ? C19C C24C 1.371(5) . ? C19C C20C 1.377(5) . ? C20C C21C 1.379(6) . ? C21C C22C 1.357(6) . ? C22C C23C 1.359(6) . ? C23C C24C 1.380(6) . ? C25C C30C 1.398(5) . ? C25C C26C 1.405(5) . ? C26C C27C 1.391(5) . ? C26C C31C 1.509(5) . ? C27C C28C 1.385(6) . ? C28C C29C 1.386(6) . ? C28C C32C 1.516(5) . ? C29C C30C 1.391(5) . ? C30C C33C 1.512(5) . ? C34C C35C 1.393(5) . ? C34C C39C 1.410(5) . ? C35C C36C 1.390(5) . ? C35C C40C 1.510(6) . ? C36C C37C 1.389(6) . ? C37C C38C 1.387(6) . ? C37C C41C 1.511(5) . ? C38C C39C 1.389(5) . ? C39C C42C 1.495(5) . ? C1CS Cl9S 1.753(4) . ? C1CS Cl8S 1.754(5) . ? C1CS Cl7S 1.768(5) . ? C1D N12D 1.324(4) . ? C1D N7D 1.375(4) . ? C1D C2D 1.464(4) . ? C2D C3D 1.365(5) . ? C2D C19D 1.473(5) . ? C3D C4D 1.425(5) . ? C4D N7D 1.375(4) . ? C4D C5D 1.395(5) . ? C5D C6D 1.374(5) . ? C5D C25D 1.510(5) . ? C6D N8D 1.389(4) . ? C6D C7D 1.446(5) . ? C7D C8D 1.355(5) . ? C8D C9D 1.444(5) . ? C9D N11D 1.318(5) . ? C9D N8D 1.376(5) . ? C10D N11D 1.323(4) . ? C10D N9D 1.367(4) . ? C10D C11D 1.442(5) . ? C11D C12D 1.343(5) . ? C12D C13D 1.432(5) . ? C13D N9D 1.383(4) . ? C13D C14D 1.384(5) . ? C14D C15D 1.378(5) . ? C14D C34D 1.500(4) . ? C15D N10D 1.380(4) . ? C15D C16D 1.433(5) . ? C16D C17D 1.349(5) . ? C17D C18D 1.442(5) . ? C18D N12D 1.326(4) . ? C18D N10D 1.366(4) . ? C19D C24D 1.384(5) . ? C19D C20D 1.388(5) . ? C20D C21D 1.375(6) . ? C21D C22D 1.376(6) . ? C22D C23D 1.367(5) . ? C23D C24D 1.382(5) . ? C25D C30D 1.397(5) . ? C25D C26D 1.405(5) . ? C26D C27D 1.392(5) . ? C26D C31D 1.501(6) . ? C27D C28D 1.388(6) . ? C28D C29D 1.383(6) . ? C28D C32D 1.517(5) . ? C29D C30D 1.395(5) . ? C30D C33D 1.499(6) . ? C34D C39D 1.398(5) . ? C34D C35D 1.407(5) . ? C35D C36D 1.388(5) . ? C35D C40D 1.504(5) . ? C36D C37D 1.375(5) . ? C37D C38D 1.391(6) . ? C37D C41D 1.520(5) . ? C38D C39D 1.388(5) . ? C39D C42D 1.518(5) . ? C1SA Cl1S 1.743(6) . ? C1SA Cl3S 1.749(7) . ? C1SA Cl2S 1.772(7) . ? C1SB Cl4S 1.741(6) . ? C1SB Cl5S 1.755(6) . ? C1SB Cl6S 1.779(6) . ? C1SD Cl12 1.749(5) . ? C1SD Cl11 1.754(6) . ? C1SD Cl10 1.774(5) . ? N1A Ni1A 1.919(3) . ? N2A Ni1A 1.918(3) . ? N3A Ni1A 1.917(3) . ? N4A Ni1A 1.911(3) . ? N1C Ni3C 1.922(3) . ? N2C Ni3C 1.912(3) . ? N3C Ni3C 1.920(3) . ? N4C Ni3C 1.916(3) . ? N1D Ni1B 1.919(3) . ? N2D Ni1B 1.910(3) . ? N3D Ni1B 1.916(3) . ? N4D Ni1B 1.914(3) . ? N7D Ni4D 1.917(3) . ? N8D Ni4D 1.912(3) . ? N9D Ni4D 1.920(3) . ? N10D Ni4D 1.914(3) . ? 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 C29A C30A C25A 119.7(6) . . ? C29A C30A C32A 119.1(6) . . ? C25A C30A C32A 121.2(4) . . ? N5A C1A N1A 127.5(3) . . ? N5A C1A C2A 120.9(3) . . ? N1A C1A C2A 111.5(3) . . ? C3A C2A C1A 104.5(3) . . ? C3A C2A C19A 127.9(3) . . ? C1A C2A C19A 127.6(3) . . ? C2A C3A C4A 109.0(3) . . ? N1A C4A C5A 124.7(3) . . ? N1A C4A C3A 110.3(3) . . ? C5A C4A C3A 124.9(3) . . ? C6A C5A C4A 122.3(3) . . ? C6A C5A C33A 119.5(3) . . ? C4A C5A C33A 118.3(3) . . ? C5A C6A N2A 125.6(3) . . ? C5A C6A C7A 124.3(4) . . ? N2A C6A C7A 110.1(4) . . ? C8A C7A C6A 107.0(4) . . ? C7A C8A C9A 107.4(4) . . ? N6A C9A N2A 127.7(4) . . ? N6A C9A C8A 121.6(4) . . ? N2A C9A C8A 110.7(4) . . ? N6A C10A N3A 128.3(4) . . ? N6A C10A C11A 121.0(4) . . ? N3A C10A C11A 110.7(3) . . ? C12A C11A C10A 107.0(4) . . ? C11A C12A C13A 106.8(4) . . ? N3A C13A C14A 125.3(4) . . ? N3A C13A C12A 111.1(4) . . ? C14A C13A C12A 123.6(4) . . ? C15A C14A C13A 121.5(4) . . ? C15A C14A C25A 118.4(4) . . ? C13A C14A C25A 120.1(4) . . ? N4A C15A C14A 125.3(4) . . ? N4A C15A C16A 110.5(3) . . ? C14A C15A C16A 124.3(4) . . ? C17A C16A C15A 106.9(4) . . ? C16A C17A C18A 106.9(4) . . ? N5A C18A N4A 128.8(3) . . ? N5A C18A C17A 120.2(4) . . ? N4A C18A C17A 111.0(3) . . ? C20A C19A C24A 116.9(4) . . ? C20A C19A C2A 123.5(3) . . ? C24A C19A C2A 119.6(3) . . ? C19A C20A C21A 121.1(3) . . ? C22A C21A C20A 120.7(4) . . ? C23A C22A C21A 118.6(4) . . ? C24A C23A C22A 121.0(4) . . ? C23A C24A C19A 121.8(4) . . ? C30A C25A C26A 120.8(5) . . ? C30A C25A C14A 120.1(4) . . ? C26A C25A C14A 119.1(5) . . ? C25A C26A C27A 117.7(6) . . ? C25A C26A C42A 121.9(5) . . ? C27A C26A C42A 120.4(5) . . ? C28A C27A C26A 121.5(6) . . ? C29A C28A C27A 118.4(5) . . ? C29A C28A C31A 122.2(8) . . ? C27A C28A C31A 119.4(7) . . ? C28A C29A C30A 121.9(7) . . ? C38A C33A C34A 120.0(3) . . ? C38A C33A C5A 120.8(4) . . ? C34A C33A C5A 119.2(3) . . ? C35A C34A C33A 118.8(4) . . ? C35A C34A C39A 120.0(4) . . ? C33A C34A C39A 121.2(3) . . ? C36A C35A C34A 122.5(4) . . ? C37A C36A C35A 118.2(4) . . ? C37A C36A C40A 122.1(5) . . ? C35A C36A C40A 119.7(5) . . ? C36A C37A C38A 121.9(4) . . ? C33A C38A C37A 118.6(4) . . ? C33A C38A C41A 122.1(4) . . ? C37A C38A C41A 119.3(4) . . ? N5D C1B N1D 127.4(3) . . ? N5D C1B C2B 120.9(3) . . ? N1D C1B C2B 111.7(3) . . ? C3B C2B C19B 128.9(3) . . ? C3B C2B C1B 104.0(3) . . ? C19B C2B C1B 127.1(3) . . ? C2B C3B C4B 109.0(3) . . ? N1D C4B C5B 124.8(4) . . ? N1D C4B C3B 110.8(3) . . ? C5B C4B C3B 124.4(4) . . ? C6B C5B C4B 121.9(4) . . ? C6B C5B C25B 119.8(4) . . ? C4B C5B C25B 118.3(4) . . ? C5B C6B N4D 126.1(4) . . ? C5B C6B C7B 124.1(4) . . ? N4D C6B C7B 109.9(4) . . ? C8B C7B C6B 107.4(4) . . ? C7B C8B C9B 107.1(4) . . ? N6D C9B N4D 128.4(4) . . ? N6D C9B C8B 121.2(4) . . ? N4D C9B C8B 110.4(4) . . ? N6D C10B N3D 127.9(4) . . ? N6D C10B C11B 121.3(4) . . ? N3D C10B C11B 110.8(4) . . ? C12B C11B C10B 107.0(4) . . ? C11B C12B C13B 106.6(4) . . ? N3D C13B C14B 125.3(4) . . ? N3D C13B C12B 110.9(4) . . ? C14B C13B C12B 123.7(4) . . ? C13B C14B C15B 121.5(4) . . ? C13B C14B C34B 119.7(4) . . ? C15B C14B C34B 118.8(4) . . ? N2D C15B C14B 125.6(4) . . ? N2D C15B C16B 110.7(3) . . ? C14B C15B C16B 123.7(4) . . ? C17B C16B C15B 106.3(4) . . ? C16B C17B C18B 107.3(4) . . ? N5D C18B N2D 128.3(3) . . ? N5D C18B C17B 120.8(4) . . ? N2D C18B C17B 110.8(3) . . ? C24B C19B C20B 117.2(4) . . ? C24B C19B C2B 120.1(3) . . ? C20B C19B C2B 122.6(3) . . ? C19B C20B C21B 120.5(4) . . ? C22B C21B C20B 120.5(4) . . ? C23B C22B C21B 119.2(4) . . ? C22B C23B C24B 120.8(4) . . ? C19B C24B C23B 121.7(4) . . ? C26B C25B C30B 120.1(4) . . ? C26B C25B C5B 119.6(4) . . ? C30B C25B C5B 120.3(4) . . ? C25B C26B C27B 119.0(4) . . ? C25B C26B C31B 121.6(4) . . ? C27B C26B C31B 119.5(4) . . ? C28B C27B C26B 121.2(5) . . ? C29B C28B C27B 119.2(5) . . ? C29B C28B C32B 121.2(5) . . ? C27B C28B C32B 119.6(6) . . ? C28B C29B C30B 121.5(5) . . ? C29B C30B C25B 119.0(5) . . ? C29B C30B C33B 119.0(5) . . ? C25B C30B C33B 122.0(5) . . ? C39B C34B C35B 121.4(5) . . ? C39B C34B C14B 119.9(5) . . ? C35B C34B C14B 118.7(6) . . ? C34B C35B C36B 117.3(7) . . ? C34B C35B C40B 122.4(6) . . ? C36B C35B C40B 120.2(6) . . ? C37B C36B C35B 121.9(7) . . ? C36B C37B C38B 119.3(6) . . ? C36B C37B C41B 119.4(9) . . ? C38B C37B C41B 121.3(10) . . ? C37B C38B C39B 120.6(8) . . ? C34B C39B C38B 119.6(6) . . ? C34B C39B C42B 121.9(4) . . ? C38B C39B C42B 118.5(6) . . ? N5C C1C N1C 127.8(3) . . ? N5C C1C C2C 121.1(3) . . ? N1C C1C C2C 111.1(3) . . ? C3C C2C C1C 104.4(3) . . ? C3C C2C C19C 128.4(3) . . ? C1C C2C C19C 127.2(3) . . ? C2C C3C C4C 109.0(3) . . ? N1C C4C C5C 125.1(3) . . ? N1C C4C C3C 110.6(3) . . ? C5C C4C C3C 124.3(3) . . ? C6C C5C C4C 122.2(3) . . ? C6C C5C C25C 118.7(3) . . ? C4C C5C C25C 119.1(3) . . ? C5C C6C N2C 125.0(3) . . ? C5C C6C C7C 124.7(3) . . ? N2C C6C C7C 110.3(3) . . ? C8C C7C C6C 107.3(3) . . ? C7C C8C C9C 106.5(3) . . ? N6C C9C N2C 128.8(3) . . ? N6C C9C C8C 120.0(4) . . ? N2C C9C C8C 111.2(3) . . ? N6C C10C N3C 128.3(3) . . ? N6C C10C C11C 120.8(3) . . ? N3C C10C C11C 110.9(3) . . ? C12C C11C C10C 106.9(3) . . ? C11C C12C C13C 107.0(3) . . ? N3C C13C C14C 124.9(3) . . ? N3C C13C C12C 110.6(3) . . ? C14C C13C C12C 124.5(3) . . ? C15C C14C C13C 122.1(3) . . ? C15C C14C C34C 118.4(3) . . ? C13C C14C C34C 119.5(3) . . ? C14C C15C N4C 125.3(3) . . ? C14C C15C C16C 124.1(3) . . ? N4C C15C C16C 110.6(3) . . ? C17C C16C C15C 106.8(3) . . ? C16C C17C C18C 106.7(3) . . ? N5C C18C N4C 128.2(3) . . ? N5C C18C C17C 120.5(3) . . ? N4C C18C C17C 111.3(3) . . ? C24C C19C C20C 116.5(4) . . ? C24C C19C C2C 124.2(3) . . ? C20C C19C C2C 119.3(3) . . ? C19C C20C C21C 121.5(4) . . ? C22C C21C C20C 121.3(4) . . ? C21C C22C C23C 117.9(4) . . ? C22C C23C C24C 121.1(4) . . ? C19C C24C C23C 121.7(4) . . ? C30C C25C C26C 120.4(3) . . ? C30C C25C C5C 120.1(3) . . ? C26C C25C C5C 119.5(3) . . ? C27C C26C C25C 118.8(4) . . ? C27C C26C C31C 120.2(4) . . ? C25C C26C C31C 121.0(3) . . ? C28C C27C C26C 121.8(4) . . ? C27C C28C C29C 118.2(4) . . ? C27C C28C C32C 121.1(4) . . ? C29C C28C C32C 120.7(4) . . ? C28C C29C C30C 122.2(4) . . ? C29C C30C C25C 118.6(4) . . ? C29C C30C C33C 120.1(4) . . ? C25C C30C C33C 121.3(3) . . ? C35C C34C C39C 120.0(3) . . ? C35C C34C C14C 120.7(3) . . ? C39C C34C C14C 119.3(3) . . ? C36C C35C C34C 119.4(4) . . ? C36C C35C C40C 119.8(4) . . ? C34C C35C C40C 120.8(3) . . ? C37C C36C C35C 121.6(4) . . ? C38C C37C C36C 118.3(3) . . ? C38C C37C C41C 120.2(4) . . ? C36C C37C C41C 121.5(4) . . ? C37C C38C C39C 121.9(4) . . ? C38C C39C C34C 118.8(4) . . ? C38C C39C C42C 120.4(3) . . ? C34C C39C C42C 120.7(3) . . ? Cl9S C1CS Cl8S 110.6(3) . . ? Cl9S C1CS Cl7S 110.2(3) . . ? Cl8S C1CS Cl7S 110.0(2) . . ? N12D C1D N7D 128.1(3) . . ? N12D C1D C2D 120.6(3) . . ? N7D C1D C2D 111.4(3) . . ? C3D C2D C1D 104.6(3) . . ? C3D C2D C19D 127.5(3) . . ? C1D C2D C19D 127.9(3) . . ? C2D C3D C4D 108.1(3) . . ? N7D C4D C5D 124.9(3) . . ? N7D C4D C3D 111.2(3) . . ? C5D C4D C3D 124.0(3) . . ? C6D C5D C4D 122.0(3) . . ? C6D C5D C25D 119.9(3) . . ? C4D C5D C25D 118.1(3) . . ? C5D C6D N8D 125.6(3) . . ? C5D C6D C7D 124.0(3) . . ? N8D C6D C7D 110.4(3) . . ? C8D C7D C6D 107.2(3) . . ? C7D C8D C9D 106.2(3) . . ? N11D C9D N8D 127.9(3) . . ? N11D C9D C8D 120.6(3) . . ? N8D C9D C8D 111.6(3) . . ? N11D C10D N9D 128.6(3) . . ? N11D C10D C11D 120.6(3) . . ? N9D C10D C11D 110.9(3) . . ? C12D C11D C10D 106.5(3) . . ? C11D C12D C13D 107.4(3) . . ? N9D C13D C14D 125.5(3) . . ? N9D C13D C12D 110.3(3) . . ? C14D C13D C12D 124.2(3) . . ? C15D C14D C13D 121.7(3) . . ? C15D C14D C34D 119.3(3) . . ? C13D C14D C34D 118.9(3) . . ? C14D C15D N10D 125.3(3) . . ? C14D C15D C16D 124.4(3) . . ? N10D C15D C16D 110.3(3) . . ? C17D C16D C15D 107.5(3) . . ? C16D C17D C18D 106.0(3) . . ? N12D C18D N10D 129.0(3) . . ? N12D C18D C17D 119.8(3) . . ? N10D C18D C17D 111.2(3) . . ? C24D C19D C20D 117.1(4) . . ? C24D C19D C2D 124.1(3) . . ? C20D C19D C2D 118.8(3) . . ? C21D C20D C19D 121.3(4) . . ? C20D C21D C22D 120.7(4) . . ? C23D C22D C21D 118.8(4) . . ? C22D C23D C24D 120.5(4) . . ? C23D C24D C19D 121.5(4) . . ? C30D C25D C26D 120.4(3) . . ? C30D C25D C5D 119.1(3) . . ? C26D C25D C5D 120.5(3) . . ? C27D C26D C25D 118.3(4) . . ? C27D C26D C31D 120.5(4) . . ? C25D C26D C31D 121.2(3) . . ? C28D C27D C26D 122.2(4) . . ? C29D C28D C27D 118.5(4) . . ? C29D C28D C32D 121.3(4) . . ? C27D C28D C32D 120.2(4) . . ? C28D C29D C30D 121.4(4) . . ? C29D C30D C25D 119.2(4) . . ? C29D C30D C33D 120.4(4) . . ? C25D C30D C33D 120.4(3) . . ? C39D C34D C35D 119.6(3) . . ? C39D C34D C14D 120.6(3) . . ? C35D C34D C14D 119.8(3) . . ? C36D C35D C34D 118.8(3) . . ? C36D C35D C40D 120.3(3) . . ? C34D C35D C40D 120.9(3) . . ? C37D C36D C35D 122.5(4) . . ? C36D C37D C38D 118.1(3) . . ? C36D C37D C41D 120.4(4) . . ? C38D C37D C41D 121.5(4) . . ? C39D C38D C37D 121.6(4) . . ? C38D C39D C34D 119.5(3) . . ? C38D C39D C42D 119.7(3) . . ? C34D C39D C42D 120.9(3) . . ? Cl1S C1SA Cl3S 109.7(3) . . ? Cl1S C1SA Cl2S 110.5(3) . . ? Cl3S C1SA Cl2S 108.9(4) . . ? Cl4S C1SB Cl5S 109.5(3) . . ? Cl4S C1SB Cl6S 110.5(3) . . ? Cl5S C1SB Cl6S 108.7(3) . . ? Cl12 C1SD Cl11 111.4(3) . . ? Cl12 C1SD Cl10 109.2(3) . . ? Cl11 C1SD Cl10 109.6(3) . . ? C1A N1A C4A 104.7(3) . . ? C1A N1A Ni1A 126.8(2) . . ? C4A N1A Ni1A 128.5(2) . . ? C9A N2A C6A 104.8(3) . . ? C9A N2A Ni1A 127.3(3) . . ? C6A N2A Ni1A 127.9(3) . . ? C10A N3A C13A 104.4(3) . . ? C10A N3A Ni1A 126.8(3) . . ? C13A N3A Ni1A 128.8(3) . . ? C18A N4A C15A 104.7(3) . . ? C18A N4A Ni1A 126.3(2) . . ? C15A N4A Ni1A 129.0(3) . . ? C18A N5A C1A 120.6(3) . . ? C10A N6A C9A 120.6(4) . . ? C4C N1C C1C 104.9(3) . . ? C4C N1C Ni3C 128.5(2) . . ? C1C N1C Ni3C 126.6(2) . . ? C9C N2C C6C 104.7(3) . . ? C9C N2C Ni3C 126.7(2) . . ? C6C N2C Ni3C 128.6(2) . . ? C10C N3C C13C 104.6(3) . . ? C10C N3C Ni3C 126.8(2) . . ? C13C N3C Ni3C 128.6(2) . . ? C18C N4C C15C 104.6(3) . . ? C18C N4C Ni3C 126.7(2) . . ? C15C N4C Ni3C 128.7(2) . . ? C1C N5C C18C 120.9(3) . . ? C9C N6C C10C 119.8(3) . . ? C1B N1D C4B 104.5(3) . . ? C1B N1D Ni1B 126.9(2) . . ? C4B N1D Ni1B 128.6(3) . . ? C18B N2D C15B 104.8(3) . . ? C18B N2D Ni1B 126.7(2) . . ? C15B N2D Ni1B 128.5(3) . . ? C13B N3D C10B 104.5(3) . . ? C13B N3D Ni1B 128.8(3) . . ? C10B N3D Ni1B 126.6(3) . . ? C9B N4D C6B 105.2(3) . . ? C9B N4D Ni1B 127.0(3) . . ? C6B N4D Ni1B 127.8(3) . . ? C18B N5D C1B 121.0(3) . . ? C9B N6D C10B 120.6(4) . . ? C4D N7D C1D 104.8(3) . . ? C4D N7D Ni4D 128.7(2) . . ? C1D N7D Ni4D 126.5(2) . . ? C9D N8D C6D 104.6(3) . . ? C9D N8D Ni4D 127.4(2) . . ? C6D N8D Ni4D 128.1(2) . . ? C10D N9D C13D 104.9(3) . . ? C10D N9D Ni4D 126.8(2) . . ? C13D N9D Ni4D 128.3(2) . . ? C18D N10D C15D 105.0(3) . . ? C18D N10D Ni4D 126.1(2) . . ? C15D N10D Ni4D 128.9(2) . . ? C9D N11D C10D 120.3(3) . . ? C1D N12D C18D 120.2(3) . . ? N4A Ni1A N3A 90.00(13) . . ? N4A Ni1A N2A 178.79(15) . . ? N3A Ni1A N2A 89.34(13) . . ? N4A Ni1A N1A 89.88(12) . . ? N3A Ni1A N1A 178.60(14) . . ? N2A Ni1A N1A 90.79(13) . . ? N2D Ni1B N4D 179.10(16) . . ? N2D Ni1B N3D 90.18(14) . . ? N4D Ni1B N3D 89.38(14) . . ? N2D Ni1B N1D 89.67(13) . . ? N4D Ni1B N1D 90.80(14) . . ? N3D Ni1B N1D 178.71(15) . . ? N2C Ni3C N4C 179.49(12) . . ? N2C Ni3C N3C 89.59(12) . . ? N4C Ni3C N3C 90.25(12) . . ? N2C Ni3C N1C 90.46(12) . . ? N4C Ni3C N1C 89.70(12) . . ? N3C Ni3C N1C 179.31(13) . . ? N8D Ni4D N10D 179.32(12) . . ? N8D Ni4D N7D 90.63(12) . . ? N10D Ni4D N7D 90.03(11) . . ? N8D Ni4D N9D 89.14(12) . . ? N10D Ni4D N9D 90.19(11) . . ? N7D Ni4D N9D 178.15(12) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.423 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.106 data_120912y1 _database_code_depnum_ccdc_archive 'CCDC 928787' #TrackingRef 'web_deposit_cif_file_1_HiroshiShinokubo_1363047956.120912y1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H80 N12 Ni2' _chemical_formula_weight 1326.98 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.455(5) _cell_length_b 13.354(5) _cell_length_c 16.134(5) _cell_angle_alpha 110.622(5) _cell_angle_beta 90.985(5) _cell_angle_gamma 96.490(5) _cell_volume 1690.8(13) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour dark _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8144 _exptl_absorpt_correction_T_max 0.9701 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11929 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.50 _reflns_number_total 9952 _reflns_number_gt 8846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.27(2) _refine_ls_number_reflns 9952 _refine_ls_number_parameters 862 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1419 _refine_ls_wR_factor_gt 0.1369 _refine_ls_goodness_of_fit_ref 1.210 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.066 _refine_ls_shift/su_mean 0.004 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.95631(9) 0.91429(6) 0.46157(5) 0.03441(15) Uani 1 1 d . . . Ni2 Ni 0.96509(7) 0.92513(5) 0.96689(4) 0.02496(12) Uani 1 1 d . . . N1 N 0.9342(5) 0.8924(3) 0.5732(3) 0.0364(9) Uani 1 1 d . . . N2 N 0.8839(7) 0.7677(5) 0.3990(4) 0.0366(13) Uani 1 1 d . . . N3 N 0.9765(5) 0.9339(3) 0.3487(3) 0.0373(9) Uani 1 1 d . . . N4 N 1.0296(8) 1.0634(5) 0.5236(4) 0.0394(14) Uani 1 1 d . . . C75 C 1.2654(10) 1.5010(5) 0.3022(5) 0.072(2) Uani 1 1 d . . . H75A H 1.3750 1.5014 0.2834 0.108 Uiso 1 1 calc R . . H75B H 1.2572 1.5672 0.3528 0.108 Uiso 1 1 calc R . . H75C H 1.1925 1.4971 0.2530 0.108 Uiso 1 1 calc R . . N9 N 0.8923(6) 0.7790(4) 0.9057(4) 0.0264(11) Uani 1 1 d . . . N12 N 0.6310(5) 0.7850(3) 0.8474(3) 0.0361(9) Uani 1 1 d . . . N10 N 0.7700(5) 0.9619(3) 0.9311(3) 0.0289(8) Uani 1 1 d . . . N11 N 1.0393(7) 1.0754(4) 1.0273(4) 0.0295(12) Uani 1 1 d . . . N8 N 1.1622(5) 0.8882(3) 1.0043(3) 0.0307(8) Uani 1 1 d . . . C1 C 0.8779(6) 0.7990(4) 0.5876(3) 0.0377(11) Uani 1 1 d . . . C2 C 0.8325(6) 0.7015(4) 0.5228(4) 0.0402(11) Uani 1 1 d . . . C3 C 0.8368(6) 0.6861(4) 0.4324(3) 0.0373(11) Uani 1 1 d . . . C4 C 0.8699(7) 0.7135(4) 0.3080(4) 0.0464(12) Uani 1 1 d . . . N5 N 0.8938(6) 0.7541(4) 0.2452(3) 0.0547(13) Uani 1 1 d . . . C6 C 0.9420(7) 0.8573(4) 0.2669(4) 0.0472(13) Uani 1 1 d . . . C7 C 1.0274(6) 1.0278(4) 0.3342(4) 0.0429(12) Uani 1 1 d . . . C8 C 1.0742(6) 1.1269(4) 0.3995(3) 0.0369(11) Uani 1 1 d . . . C9 C 1.0773(6) 1.1419(4) 0.4883(4) 0.0388(11) Uani 1 1 d . . . C10 C 1.0518(7) 1.1130(4) 0.6129(4) 0.0477(13) Uani 1 1 d . . . N6 N 1.0245(6) 1.0710(4) 0.6768(3) 0.0498(12) Uani 1 1 d . . . C12 C 0.9737(7) 0.9691(4) 0.6559(4) 0.0475(13) Uani 1 1 d . . . C13 C 0.9569(10) 0.9261(6) 0.7293(4) 0.0483(15) Uani 1 1 d . . . H1 H 0.8940 0.9702 0.7777 0.058 Uiso 1 1 calc R . . C14 C 0.8743(8) 0.8163(5) 0.6830(4) 0.0553(15) Uani 1 1 d . . . H2 H 0.9300 0.7624 0.6972 0.066 Uiso 1 1 calc R . . H3 H 0.7630 0.8105 0.7006 0.066 Uiso 1 1 calc R . . C15 C 1.1257(8) 0.9185(7) 0.7640(5) 0.085(2) Uani 1 1 d . . . H4 H 1.1165 0.8927 0.8138 0.127 Uiso 1 1 calc R . . H5 H 1.1887 0.9899 0.7840 0.127 Uiso 1 1 calc R . . H6 H 1.1785 0.8681 0.7163 0.127 Uiso 1 1 calc R . . C16 C 1.1083(9) 1.2240(4) 0.6364(4) 0.0536(15) Uani 1 1 d . . . H9 H 1.1299 1.2760 0.6945 0.064 Uiso 1 1 calc R . . C17 C 1.1253(7) 1.2405(4) 0.5587(4) 0.0477(14) Uani 1 1 d . . . H8 H 1.1631 1.3071 0.5526 0.057 Uiso 1 1 calc R . . C18 C 1.1257(6) 1.2208(4) 0.3730(4) 0.0402(11) Uani 1 1 d . . . C19 C 1.0133(6) 1.2802(4) 0.3561(3) 0.0424(12) Uani 1 1 d . . . C20 C 1.0605(7) 1.3695(4) 0.3331(4) 0.0491(13) Uani 1 1 d . . . H14 H 0.9826 1.4084 0.3197 0.059 Uiso 1 1 calc R . . C21 C 1.2205(9) 1.4019(5) 0.3297(5) 0.0610(18) Uani 1 1 d . . . C22 C 1.3310(7) 1.3426(5) 0.3463(4) 0.0558(16) Uani 1 1 d . . . H13 H 1.4409 1.3644 0.3430 0.067 Uiso 1 1 calc R . . C23 C 1.2874(8) 1.2515(6) 0.3678(5) 0.0517(17) Uani 1 1 d . . . C24 C 1.4101(8) 1.1887(7) 0.3826(6) 0.080(2) Uani 1 1 d . . . H10 H 1.5143 1.2176 0.3692 0.120 Uiso 1 1 calc R . . H11 H 1.3842 1.1131 0.3439 0.120 Uiso 1 1 calc R . . H12 H 1.4136 1.1938 0.4447 0.120 Uiso 1 1 calc R . . C25 C 0.8371(9) 1.2509(7) 0.3633(6) 0.057(2) Uani 1 1 d . . . H17 H 0.7990 1.1820 0.3161 0.086 Uiso 1 1 calc R . . H16 H 0.7782 1.3074 0.3573 0.086 Uiso 1 1 calc R . . H15 H 0.8199 1.2443 0.4212 0.086 Uiso 1 1 calc R . . C26 C 1.0266(8) 1.0086(5) 0.2396(4) 0.0546(15) Uani 1 1 d . . . H18 H 1.0618 1.0592 0.2126 0.065 Uiso 1 1 calc R . . C27 C 0.9654(12) 0.9038(7) 0.1977(4) 0.061(2) Uani 1 1 d . . . H19 H 0.9423 0.8678 0.1357 0.074 Uiso 1 1 calc R . . C28 C 0.8149(8) 0.6004(5) 0.2857(4) 0.0511(14) Uani 1 1 d . . . H22 H 0.7970 0.5472 0.2278 0.061 Uiso 1 1 calc R . . C29 C 0.7940(8) 0.5852(5) 0.3631(4) 0.0458(14) Uani 1 1 d . . . H21 H 0.7573 0.5189 0.3700 0.055 Uiso 1 1 calc R . . C30 C 0.7829(6) 0.6049(4) 0.5483(3) 0.0383(11) Uani 1 1 d . . . C31 C 0.8975(6) 0.5449(4) 0.5630(4) 0.0426(12) Uani 1 1 d . . . C32 C 0.8475(8) 0.4568(5) 0.5859(4) 0.0535(14) Uani 1 1 d . . . H28 H 0.9257 0.4163 0.5967 0.064 Uiso 1 1 calc R . . C33 C 0.6905(8) 0.4248(4) 0.5937(4) 0.0492(14) Uani 1 1 d . . . C34 C 0.5804(8) 0.4842(4) 0.5774(4) 0.0489(14) Uani 1 1 d . . . H26 H 0.4707 0.4620 0.5808 0.059 Uiso 1 1 calc R . . C35 C 0.6208(7) 0.5740(5) 0.5563(5) 0.0444(14) Uani 1 1 d . . . C36 C 0.4940(7) 0.6409(6) 0.5429(5) 0.0663(19) Uani 1 1 d . . . H24 H 0.3958 0.5931 0.5157 0.099 Uiso 1 1 calc R . . H25 H 0.5327 0.6793 0.5039 0.099 Uiso 1 1 calc R . . H23 H 0.4724 0.6932 0.6004 0.099 Uiso 1 1 calc R . . C37 C 1.0714(9) 0.5768(7) 0.5542(6) 0.0539(19) Uani 1 1 d . . . H30 H 1.1133 0.6390 0.6067 0.081 Uiso 1 1 calc R . . H29 H 1.0831 0.5960 0.5011 0.081 Uiso 1 1 calc R . . H31 H 1.1309 0.5162 0.5490 0.081 Uiso 1 1 calc R . . C38 C 0.7474(6) 0.7336(3) 0.8585(3) 0.0334(10) Uani 1 1 d . . . C39 C 0.6411(6) 0.8911(4) 0.8818(4) 0.0360(10) Uani 1 1 d . . . C40 C 0.7214(6) 1.0620(3) 0.9496(3) 0.0324(10) Uani 1 1 d . . . C41 C 0.8137(5) 1.1583(3) 0.9963(3) 0.0301(9) Uani 1 1 d . . . C42 C 0.7497(6) 1.2628(4) 1.0074(3) 0.0376(11) Uani 1 1 d . . . C43 C 0.6702(7) 1.3121(4) 1.0833(4) 0.0413(13) Uani 1 1 d . . . C44 C 0.6148(7) 1.4115(4) 1.0932(4) 0.0489(14) Uani 1 1 d . . . H39 H 0.5569 1.4452 1.1432 0.059 Uiso 1 1 calc R . . C45 C 0.6432(7) 1.4610(4) 1.0312(5) 0.0528(16) Uani 1 1 d . . . C46 C 0.7203(7) 1.4085(4) 0.9557(4) 0.0469(13) Uani 1 1 d . . . H35 H 0.7363 1.4407 0.9120 0.056 Uiso 1 1 calc R . . C47 C 0.7744(6) 1.3103(4) 0.9428(4) 0.0406(12) Uani 1 1 d . . . C48 C 0.8518(10) 1.2570(6) 0.8593(5) 0.0501(18) Uani 1 1 d . . . H32 H 0.8449 1.2984 0.8201 0.075 Uiso 1 1 calc R . . H33 H 0.7974 1.1837 0.8296 0.075 Uiso 1 1 calc R . . H34 H 0.9641 1.2539 0.8731 0.075 Uiso 1 1 calc R . . C49 C 0.5939(10) 1.5715(5) 1.0474(7) 0.070(2) Uani 1 1 d . . . H37 H 0.5935 1.6109 1.1114 0.105 Uiso 1 1 calc R . . H36 H 0.4868 1.5637 1.0199 0.105 Uiso 1 1 calc R . . H38 H 0.6695 1.6116 1.0214 0.105 Uiso 1 1 calc R . . C50 C 0.6461(8) 1.2624(5) 1.1535(4) 0.0586(15) Uani 1 1 d . . . H40 H 0.5702 1.1964 1.1300 0.088 Uiso 1 1 calc R . . H42 H 0.6041 1.3136 1.2056 0.088 Uiso 1 1 calc R . . H41 H 0.7483 1.2448 1.1705 0.088 Uiso 1 1 calc R . . C51 C 0.9633(6) 1.1618(3) 1.0328(3) 0.0310(9) Uani 1 1 d . . . C52 C 1.1798(6) 1.1159(4) 1.0734(3) 0.0318(10) Uani 1 1 d . . . C53 C 1.1950(7) 1.2310(4) 1.1089(4) 0.0423(13) Uani 1 1 d . . . H43 H 1.2835 1.2786 1.1434 0.051 Uiso 1 1 calc R . . C54 C 1.0587(7) 1.2587(4) 1.0837(4) 0.0469(15) Uani 1 1 d . . . H44 H 1.0320 1.3298 1.0975 0.056 Uiso 1 1 calc R . . N7 N 1.2952(5) 1.0632(3) 1.0898(3) 0.0399(10) Uani 1 1 d . . . C56 C 1.2808(6) 0.9594(4) 1.0572(4) 0.0429(12) Uani 1 1 d . . . C57 C 1.2095(6) 0.7875(4) 0.9849(3) 0.0331(10) Uani 1 1 d . . . C58 C 1.1236(6) 0.6926(3) 0.9335(3) 0.0322(10) Uani 1 1 d . . . C59 C 1.1873(6) 0.5874(4) 0.9167(3) 0.0362(11) Uani 1 1 d . . . C60 C 1.2662(7) 0.5414(5) 0.8389(4) 0.0443(14) Uani 1 1 d . . . C61 C 1.3183(7) 0.4419(4) 0.8227(4) 0.0540(15) Uani 1 1 d . . . H53 H 1.3716 0.4104 0.7702 0.065 Uiso 1 1 calc R . . C62 C 1.2947(8) 0.3875(4) 0.8811(5) 0.0605(19) Uani 1 1 d . . . C63 C 1.2203(7) 0.4356(4) 0.9575(4) 0.0505(15) Uani 1 1 d . . . H49 H 1.2066 0.3992 0.9985 0.061 Uiso 1 1 calc R . . C64 C 1.1636(6) 0.5355(4) 0.9780(4) 0.0430(12) Uani 1 1 d . . . C65 C 1.0771(10) 0.5846(6) 1.0620(6) 0.0519(19) Uani 1 1 d . . . H48 H 1.1543 0.6310 1.1098 0.078 Uiso 1 1 calc R . . H47 H 1.0230 0.5268 1.0794 0.078 Uiso 1 1 calc R . . H46 H 0.9983 0.6275 1.0508 0.078 Uiso 1 1 calc R . . C66 C 1.3486(10) 0.2771(6) 0.8622(7) 0.087(3) Uani 1 1 d . . . H50 H 1.2614 0.2208 0.8306 0.130 Uiso 1 1 calc R . . H51 H 1.3782 0.2691 0.9183 0.130 Uiso 1 1 calc R . . H52 H 1.4409 0.2702 0.8256 0.130 Uiso 1 1 calc R . . C67 C 1.2892(7) 0.5958(5) 0.7726(4) 0.0561(15) Uani 1 1 d . . . H56 H 1.3407 0.5499 0.7215 0.084 Uiso 1 1 calc R . . H55 H 1.3566 0.6651 0.7999 0.084 Uiso 1 1 calc R . . H54 H 1.1853 0.6081 0.7527 0.084 Uiso 1 1 calc R . . C68 C 0.9733(6) 0.6881(4) 0.8948(3) 0.0331(10) Uani 1 1 d . . . C69 C 0.8767(7) 0.5908(4) 0.8398(4) 0.0420(12) Uani 1 1 d . . . H58 H 0.9048 0.5197 0.8226 0.050 Uiso 1 1 calc R . . C70 C 0.7396(7) 0.6191(4) 0.8172(4) 0.0428(13) Uani 1 1 d . . . H57 H 0.6531 0.5718 0.7804 0.051 Uiso 1 1 calc R . . C71 C 1.3689(7) 0.7920(4) 1.0259(4) 0.0444(13) Uani 1 1 d . . . H60 H 1.4310 0.7344 1.0168 0.053 Uiso 1 1 calc R . . C72 C 1.4095(10) 0.9035(5) 1.0828(7) 0.110(4) Uani 1 1 d . . . C73 C 0.5626(6) 1.0543(4) 0.9111(4) 0.0431(12) Uani 1 1 d . . . H61 H 0.5044 1.1118 0.9130 0.052 Uiso 1 1 calc R . . C74 C 0.5156(7) 0.9483(4) 0.8722(4) 0.0462(12) Uani 1 1 d . . . H62 H 0.4141 0.9166 0.8429 0.055 Uiso 1 1 calc R . . C76 C 0.6387(12) 0.3266(6) 0.6174(6) 0.084(3) Uani 1 1 d . . . H76A H 0.6532 0.3455 0.6817 0.126 Uiso 1 1 calc R . . H76B H 0.7032 0.2693 0.5873 0.126 Uiso 1 1 calc R . . H76C H 0.5260 0.3013 0.5984 0.126 Uiso 1 1 calc R . . C77 C 1.5248(15) 0.9518(8) 1.1418(9) 0.185(7) Uani 1 1 d . . . H77A H 1.4838 0.9711 1.2011 0.277 Uiso 1 1 calc R . . H77B H 1.5719 1.0173 1.1326 0.277 Uiso 1 1 calc R . . H77C H 1.6064 0.9036 1.1364 0.277 Uiso 1 1 calc R . . C3S C 0.5119(19) 0.9648(14) 0.5040(8) 0.294(17) Uani 1 1 d D . . H3S1 H 0.6162 0.9366 0.4970 0.353 Uiso 1 1 calc R . . H3S2 H 0.5287 1.0376 0.5002 0.353 Uiso 1 1 calc R . . C1S C 0.5394(19) 1.0643(12) 0.6682(9) 0.178(6) Uani 1 1 d D . . H1S1 H 0.4826 1.0686 0.7215 0.268 Uiso 1 1 calc R . . H1S2 H 0.5389 1.1320 0.6573 0.268 Uiso 1 1 calc R . . H1S3 H 0.6498 1.0523 0.6768 0.268 Uiso 1 1 calc R . . C2S C 0.461(2) 0.9756(15) 0.5927(9) 0.257(12) Uani 1 1 d D . . H2S1 H 0.3455 0.9817 0.5929 0.309 Uiso 1 1 calc R . . H2S2 H 0.4748 0.9077 0.6022 0.309 Uiso 1 1 calc R . . C6S C 0.365(2) 0.7567(11) 0.2763(10) 0.236(12) Uani 1 1 d D . . H6S1 H 0.4271 0.7131 0.2293 0.354 Uiso 1 1 calc R . . H6S2 H 0.3075 0.8026 0.2540 0.354 Uiso 1 1 calc R . . H6S3 H 0.2886 0.7090 0.2948 0.354 Uiso 1 1 calc R . . C4S C 0.4024(17) 0.8949(17) 0.4293(10) 0.36(2) Uani 1 1 d D . . H4S1 H 0.3268 0.8493 0.4516 0.430 Uiso 1 1 calc R . . H4S2 H 0.3393 0.9413 0.4095 0.430 Uiso 1 1 calc R . . C5S C 0.4730(15) 0.8244(16) 0.3524(13) 0.39(3) Uani 1 1 d D . . H5S1 H 0.5331 0.7765 0.3721 0.463 Uiso 1 1 calc R . . H5S2 H 0.5513 0.8699 0.3316 0.463 Uiso 1 1 calc R . . 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 Ni1 0.0357(3) 0.0388(4) 0.0296(3) 0.0140(2) 0.00330(19) 0.0018(2) Ni2 0.0282(2) 0.0201(2) 0.0297(2) 0.01100(18) 0.00492(16) 0.00828(17) N1 0.044(2) 0.040(2) 0.024(2) 0.0110(15) 0.0055(16) 0.0008(17) N2 0.029(3) 0.048(3) 0.034(3) 0.017(2) 0.000(2) 0.000(2) N3 0.039(2) 0.038(2) 0.036(2) 0.0147(16) 0.0018(17) 0.0020(16) N4 0.046(3) 0.044(3) 0.032(3) 0.018(2) 0.002(2) 0.006(2) C75 0.097(6) 0.050(4) 0.070(5) 0.027(3) 0.031(4) -0.007(4) N9 0.023(2) 0.021(2) 0.036(3) 0.0115(19) 0.0015(19) 0.0050(18) N12 0.034(2) 0.0234(18) 0.048(2) 0.0099(16) -0.0060(18) 0.0040(16) N10 0.031(2) 0.0215(17) 0.034(2) 0.0108(14) 0.0019(15) 0.0034(15) N11 0.040(3) 0.020(2) 0.029(3) 0.0067(18) 0.005(2) 0.0087(19) N8 0.036(2) 0.0245(18) 0.034(2) 0.0104(15) 0.0033(16) 0.0137(15) C1 0.040(3) 0.043(3) 0.034(3) 0.019(2) 0.008(2) 0.006(2) C2 0.026(2) 0.042(3) 0.053(3) 0.019(2) 0.001(2) 0.0002(19) C3 0.036(2) 0.039(2) 0.038(3) 0.017(2) -0.003(2) -0.0031(19) C4 0.051(3) 0.049(3) 0.037(3) 0.014(2) 0.005(2) 0.000(2) N5 0.066(3) 0.052(3) 0.041(3) 0.015(2) -0.002(2) -0.007(2) C6 0.059(3) 0.054(3) 0.031(3) 0.018(2) 0.007(2) 0.007(3) C7 0.036(2) 0.049(3) 0.048(3) 0.022(2) 0.010(2) 0.006(2) C8 0.036(2) 0.047(3) 0.039(3) 0.027(2) 0.012(2) 0.009(2) C9 0.029(2) 0.037(2) 0.050(3) 0.014(2) 0.005(2) 0.0041(18) C10 0.055(3) 0.041(3) 0.046(3) 0.016(2) -0.007(2) -0.001(2) N6 0.072(3) 0.046(2) 0.029(2) 0.0136(18) 0.001(2) 0.001(2) C12 0.055(3) 0.047(3) 0.038(3) 0.015(2) 0.002(2) -0.004(2) C13 0.058(3) 0.058(3) 0.030(4) 0.019(3) 0.007(3) 0.002(2) C14 0.079(4) 0.052(3) 0.034(3) 0.016(2) 0.006(3) 0.001(3) C15 0.065(4) 0.138(7) 0.075(5) 0.073(5) -0.012(3) -0.008(4) C16 0.077(4) 0.032(3) 0.045(3) 0.007(2) -0.002(3) 0.001(3) C17 0.049(3) 0.039(3) 0.056(4) 0.020(2) 0.001(3) -0.001(2) C18 0.037(3) 0.040(3) 0.049(3) 0.023(2) 0.011(2) 0.006(2) C19 0.047(3) 0.046(3) 0.040(3) 0.022(2) 0.007(2) 0.007(2) C20 0.055(3) 0.048(3) 0.055(3) 0.029(3) 0.012(3) 0.013(2) C21 0.083(5) 0.042(3) 0.055(4) 0.018(3) 0.022(3) -0.009(3) C22 0.040(3) 0.061(4) 0.059(4) 0.017(3) 0.015(3) -0.009(3) C23 0.046(3) 0.057(4) 0.060(4) 0.029(3) 0.018(3) 0.004(3) C24 0.040(3) 0.100(6) 0.113(7) 0.052(5) 0.023(4) 0.011(4) C25 0.041(4) 0.079(5) 0.066(5) 0.041(4) 0.013(3) 0.014(3) C26 0.077(4) 0.054(3) 0.036(3) 0.022(2) 0.011(3) 0.002(3) C27 0.083(4) 0.073(5) 0.030(4) 0.025(4) 0.004(4) 0.001(4) C28 0.057(4) 0.048(3) 0.041(3) 0.010(2) -0.005(3) -0.001(3) C29 0.054(4) 0.038(3) 0.042(3) 0.013(2) -0.006(3) -0.002(2) C30 0.038(3) 0.038(2) 0.040(3) 0.016(2) 0.010(2) 0.0035(19) C31 0.037(3) 0.044(3) 0.048(3) 0.018(2) 0.013(2) 0.007(2) C32 0.067(4) 0.046(3) 0.054(4) 0.023(3) 0.013(3) 0.017(3) C33 0.064(4) 0.041(3) 0.049(3) 0.022(2) 0.019(3) 0.008(3) C34 0.052(3) 0.041(3) 0.051(3) 0.017(2) 0.012(3) -0.006(2) C35 0.038(3) 0.044(3) 0.052(3) 0.020(2) 0.003(2) -0.001(2) C36 0.035(3) 0.082(5) 0.100(6) 0.051(4) 0.012(3) 0.018(3) C37 0.038(3) 0.071(5) 0.063(4) 0.036(4) -0.002(3) 0.008(3) C38 0.035(2) 0.025(2) 0.042(3) 0.0126(19) 0.001(2) 0.0041(19) C39 0.031(2) 0.030(2) 0.048(3) 0.014(2) 0.002(2) 0.0087(18) C40 0.036(3) 0.026(2) 0.038(3) 0.0127(18) 0.003(2) 0.0105(19) C41 0.033(2) 0.0210(19) 0.035(2) 0.0074(17) 0.0040(18) 0.0067(17) C42 0.042(3) 0.025(2) 0.044(3) 0.0074(19) 0.001(2) 0.0150(19) C43 0.041(3) 0.031(2) 0.045(3) 0.003(2) -0.012(2) 0.012(2) C44 0.041(3) 0.029(2) 0.062(3) -0.004(2) -0.006(2) 0.015(2) C45 0.038(3) 0.029(2) 0.083(4) 0.010(3) -0.026(3) 0.005(2) C46 0.045(3) 0.029(2) 0.066(3) 0.016(2) -0.012(2) 0.011(2) C47 0.046(3) 0.022(2) 0.050(3) 0.0081(19) -0.013(2) 0.0069(19) C48 0.068(5) 0.039(3) 0.050(4) 0.023(3) 0.001(3) 0.009(3) C49 0.060(4) 0.022(3) 0.118(6) 0.011(3) -0.016(4) 0.016(3) C50 0.055(3) 0.066(4) 0.051(4) 0.012(3) 0.014(3) 0.022(3) C51 0.033(2) 0.024(2) 0.038(2) 0.0115(17) 0.0001(19) 0.0098(17) C52 0.032(2) 0.029(2) 0.035(2) 0.0105(18) -0.0003(19) 0.0084(18) C53 0.039(3) 0.022(2) 0.059(4) 0.007(2) -0.009(2) 0.002(2) C54 0.049(3) 0.026(2) 0.058(4) 0.004(2) -0.007(3) 0.011(2) N7 0.029(2) 0.032(2) 0.053(3) 0.0086(18) -0.0042(18) 0.0060(17) C56 0.037(3) 0.030(2) 0.060(3) 0.014(2) -0.009(2) 0.012(2) C57 0.036(2) 0.031(2) 0.036(3) 0.0139(19) 0.001(2) 0.0133(19) C58 0.037(2) 0.025(2) 0.039(3) 0.0140(18) 0.0031(19) 0.0117(18) C59 0.032(2) 0.028(2) 0.046(3) 0.0079(19) -0.006(2) 0.0113(18) C60 0.030(2) 0.037(3) 0.057(3) 0.005(2) -0.002(2) 0.006(2) C61 0.035(3) 0.037(3) 0.067(4) -0.010(2) -0.012(2) 0.010(2) C62 0.054(4) 0.020(2) 0.092(5) -0.001(3) -0.017(3) 0.016(2) C63 0.053(3) 0.024(2) 0.072(4) 0.016(2) -0.022(3) 0.001(2) C64 0.040(3) 0.033(2) 0.056(3) 0.015(2) -0.004(2) 0.011(2) C65 0.059(4) 0.040(3) 0.060(4) 0.025(3) -0.004(3) -0.001(3) C66 0.076(5) 0.035(3) 0.125(7) -0.005(4) -0.037(5) 0.027(3) C67 0.045(3) 0.062(4) 0.050(3) 0.005(3) 0.003(3) 0.010(3) C68 0.036(2) 0.025(2) 0.036(2) 0.0076(17) 0.0042(19) 0.0048(18) C69 0.047(3) 0.023(2) 0.052(3) 0.010(2) -0.007(2) 0.007(2) C70 0.041(3) 0.029(3) 0.051(3) 0.007(2) -0.007(2) 0.004(2) C71 0.044(3) 0.027(2) 0.061(3) 0.012(2) -0.009(2) 0.012(2) C72 0.088(5) 0.033(3) 0.177(9) -0.007(4) -0.086(6) 0.028(3) C73 0.032(3) 0.036(2) 0.060(3) 0.014(2) -0.003(2) 0.011(2) C74 0.043(3) 0.037(3) 0.059(3) 0.018(2) -0.007(2) 0.007(2) C76 0.114(7) 0.054(4) 0.094(6) 0.039(4) 0.027(5) 0.005(4) C77 0.214(12) 0.082(6) 0.222(13) 0.001(7) -0.146(11) 0.069(7) C3S 0.132(14) 0.45(4) 0.49(4) 0.37(4) 0.05(2) 0.130(19) C1S 0.229(18) 0.195(15) 0.111(11) 0.064(11) 0.018(10) -0.004(13) C2S 0.36(3) 0.29(2) 0.081(10) -0.009(13) 0.032(14) 0.08(2) C6S 0.42(3) 0.119(11) 0.164(15) 0.071(10) -0.115(18) -0.019(15) C4S 0.091(11) 0.54(4) 0.67(6) 0.48(5) 0.14(2) 0.08(2) C5S 0.065(8) 0.63(6) 0.66(7) 0.50(6) -0.04(2) -0.022(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ni1 N2 1.882(6) . ? Ni1 N4 1.909(6) . ? Ni1 N1 1.932(4) . ? Ni1 N3 1.936(4) . ? Ni2 N9 1.874(5) . ? Ni2 N10 1.909(4) . ? Ni2 N11 1.920(5) . ? Ni2 N8 1.936(4) . ? N1 C12 1.373(7) . ? N1 C1 1.383(6) . ? N2 C4 1.385(8) . ? N2 C3 1.399(8) . ? N3 C6 1.358(6) . ? N3 C7 1.380(6) . ? N4 C10 1.357(9) . ? N4 C9 1.387(8) . ? C75 C21 1.549(8) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? N9 C38 1.387(7) . ? N9 C68 1.419(7) . ? N12 C38 1.306(6) . ? N12 C39 1.320(6) . ? N10 C40 1.376(6) . ? N10 C39 1.386(6) . ? N11 C52 1.341(8) . ? N11 C51 1.360(7) . ? N8 C56 1.349(6) . ? N8 C57 1.376(6) . ? C1 C2 1.360(7) . ? C1 C14 1.475(7) . ? C2 C3 1.400(7) . ? C2 C30 1.507(7) . ? C3 C29 1.419(7) . ? C4 N5 1.316(7) . ? C4 C28 1.442(7) . ? N5 C6 1.310(7) . ? C6 C27 1.463(9) . ? C7 C8 1.379(7) . ? C7 C26 1.456(8) . ? C8 C9 1.374(7) . ? C8 C18 1.485(6) . ? C9 C17 1.414(8) . ? C10 N6 1.347(7) . ? C10 C16 1.417(7) . ? N6 C12 1.300(6) . ? C12 C13 1.490(9) . ? C13 C14 1.474(9) . ? C13 C15 1.551(11) . ? C13 H1 1.0000 . ? C14 H2 0.9900 . ? C14 H3 0.9900 . ? C15 H4 0.9800 . ? C15 H5 0.9800 . ? C15 H6 0.9800 . ? C16 C17 1.354(9) . ? C16 H9 0.9500 . ? C17 H8 0.9500 . ? C18 C19 1.385(7) . ? C18 C23 1.395(8) . ? C19 C20 1.389(7) . ? C19 C25 1.514(9) . ? C20 C21 1.381(9) . ? C20 H14 0.9500 . ? C21 C22 1.371(10) . ? C22 C23 1.391(8) . ? C22 H13 0.9500 . ? C23 C24 1.472(10) . ? C24 H10 0.9800 . ? C24 H11 0.9800 . ? C24 H12 0.9800 . ? C25 H17 0.9800 . ? C25 H16 0.9800 . ? C25 H15 0.9800 . ? C26 C27 1.356(9) . ? C26 H18 0.9500 . ? C27 H19 0.9500 . ? C28 C29 1.345(9) . ? C28 H22 0.9500 . ? C29 H21 0.9500 . ? C30 C31 1.391(7) . ? C30 C35 1.407(8) . ? C31 C32 1.378(7) . ? C31 C37 1.508(9) . ? C32 C33 1.370(9) . ? C32 H28 0.9500 . ? C33 C34 1.368(9) . ? C33 C76 1.511(8) . ? C34 C35 1.367(8) . ? C34 H26 0.9500 . ? C35 C36 1.530(9) . ? C36 H24 0.9800 . ? C36 H25 0.9800 . ? C36 H23 0.9800 . ? C37 H30 0.9800 . ? C37 H29 0.9800 . ? C37 H31 0.9800 . ? C38 C70 1.429(7) . ? C39 C74 1.412(7) . ? C40 C41 1.378(6) . ? C40 C73 1.447(7) . ? C41 C51 1.375(6) . ? C41 C42 1.507(6) . ? C42 C43 1.395(8) . ? C42 C47 1.405(7) . ? C43 C44 1.414(8) . ? C43 C50 1.508(9) . ? C44 C45 1.390(9) . ? C44 H39 0.9500 . ? C45 C46 1.388(9) . ? C45 C49 1.514(9) . ? C46 C47 1.386(7) . ? C46 H35 0.9500 . ? C47 C48 1.487(10) . ? C48 H32 0.9800 . ? C48 H33 0.9800 . ? C48 H34 0.9800 . ? C49 H37 0.9800 . ? C49 H36 0.9800 . ? C49 H38 0.9800 . ? C50 H40 0.9800 . ? C50 H42 0.9800 . ? C50 H41 0.9800 . ? C51 C54 1.411(7) . ? C52 N7 1.340(6) . ? C52 C53 1.429(6) . ? C53 C54 1.348(9) . ? C53 H43 0.9500 . ? C54 H44 0.9500 . ? N7 C56 1.289(6) . ? C56 C72 1.515(8) . ? C57 C58 1.361(6) . ? C57 C71 1.477(7) . ? C58 C68 1.392(7) . ? C58 C59 1.498(6) . ? C59 C64 1.399(7) . ? C59 C60 1.406(8) . ? C60 C61 1.385(8) . ? C60 C67 1.494(9) . ? C61 C62 1.383(10) . ? C61 H53 0.9500 . ? C62 C63 1.375(10) . ? C62 C66 1.522(9) . ? C63 C64 1.399(7) . ? C63 H49 0.9500 . ? C64 C65 1.523(11) . ? C65 H48 0.9800 . ? C65 H47 0.9800 . ? C65 H46 0.9800 . ? C66 H50 0.9800 . ? C66 H51 0.9800 . ? C66 H52 0.9800 . ? C67 H56 0.9800 . ? C67 H55 0.9800 . ? C67 H54 0.9800 . ? C68 C69 1.437(6) . ? C69 C70 1.343(8) . ? C69 H58 0.9500 . ? C70 H57 0.9500 . ? C71 C72 1.446(8) . ? C71 H60 0.9500 . ? C72 C77 1.290(12) . ? C73 C74 1.339(7) . ? C73 H61 0.9500 . ? C74 H62 0.9500 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C3S C2S 1.464(10) . ? C3S C4S 1.468(9) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C1S C2S 1.451(9) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C6S C5S 1.467(9) . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? C4S C5S 1.453(10) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S H5S1 0.9900 . ? C5S H5S2 0.9900 . ? 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 N2 Ni1 N4 179.2(3) . . ? N2 Ni1 N1 90.6(2) . . ? N4 Ni1 N1 90.1(2) . . ? N2 Ni1 N3 88.4(2) . . ? N4 Ni1 N3 90.8(2) . . ? N1 Ni1 N3 179.05(19) . . ? N9 Ni2 N10 89.39(19) . . ? N9 Ni2 N11 178.8(3) . . ? N10 Ni2 N11 90.0(2) . . ? N9 Ni2 N8 90.8(2) . . ? N10 Ni2 N8 179.4(2) . . ? N11 Ni2 N8 89.9(2) . . ? C12 N1 C1 105.7(4) . . ? C12 N1 Ni1 125.9(3) . . ? C1 N1 Ni1 128.5(3) . . ? C4 N2 C3 103.1(5) . . ? C4 N2 Ni1 128.1(4) . . ? C3 N2 Ni1 128.8(4) . . ? C6 N3 C7 105.5(4) . . ? C6 N3 Ni1 126.9(3) . . ? C7 N3 Ni1 127.7(4) . . ? C10 N4 C9 105.8(5) . . ? C10 N4 Ni1 126.1(4) . . ? C9 N4 Ni1 128.1(5) . . ? C21 C75 H75A 109.5 . . ? C21 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C21 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C38 N9 C68 103.2(4) . . ? C38 N9 Ni2 128.4(4) . . ? C68 N9 Ni2 128.4(4) . . ? C38 N12 C39 121.7(4) . . ? C40 N10 C39 103.9(4) . . ? C40 N10 Ni2 129.2(3) . . ? C39 N10 Ni2 126.9(3) . . ? C52 N11 C51 105.9(5) . . ? C52 N11 Ni2 125.9(4) . . ? C51 N11 Ni2 128.2(4) . . ? C56 N8 C57 106.5(4) . . ? C56 N8 Ni2 125.2(3) . . ? C57 N8 Ni2 128.3(3) . . ? C2 C1 N1 125.0(5) . . ? C2 C1 C14 123.1(4) . . ? N1 C1 C14 111.9(4) . . ? C1 C2 C3 122.5(4) . . ? C1 C2 C30 119.2(5) . . ? C3 C2 C30 118.3(4) . . ? N2 C3 C2 124.6(5) . . ? N2 C3 C29 111.4(5) . . ? C2 C3 C29 124.0(5) . . ? N5 C4 N2 127.9(5) . . ? N5 C4 C28 120.5(5) . . ? N2 C4 C28 111.6(5) . . ? C6 N5 C4 119.6(5) . . ? N5 C6 N3 129.0(5) . . ? N5 C6 C27 120.0(5) . . ? N3 C6 C27 111.0(5) . . ? C8 C7 N3 125.3(5) . . ? C8 C7 C26 123.9(4) . . ? N3 C7 C26 110.7(5) . . ? C9 C8 C7 122.5(4) . . ? C9 C8 C18 118.6(5) . . ? C7 C8 C18 118.9(4) . . ? C8 C9 N4 125.5(5) . . ? C8 C9 C17 125.7(5) . . ? N4 C9 C17 108.7(5) . . ? N6 C10 N4 128.8(5) . . ? N6 C10 C16 120.0(5) . . ? N4 C10 C16 111.2(5) . . ? C12 N6 C10 120.4(5) . . ? N6 C12 N1 128.6(5) . . ? N6 C12 C13 117.7(5) . . ? N1 C12 C13 113.7(5) . . ? C14 C13 C12 102.1(5) . . ? C14 C13 C15 109.1(7) . . ? C12 C13 C15 108.6(6) . . ? C14 C13 H1 112.1 . . ? C12 C13 H1 112.1 . . ? C15 C13 H1 112.1 . . ? C1 C14 C13 105.5(4) . . ? C1 C14 H2 110.6 . . ? C13 C14 H2 110.6 . . ? C1 C14 H3 110.6 . . ? C13 C14 H3 110.6 . . ? H2 C14 H3 108.8 . . ? C13 C15 H4 109.5 . . ? C13 C15 H5 109.5 . . ? H4 C15 H5 109.5 . . ? C13 C15 H6 109.5 . . ? H4 C15 H6 109.5 . . ? H5 C15 H6 109.5 . . ? C17 C16 C10 105.7(5) . . ? C17 C16 H9 127.1 . . ? C10 C16 H9 127.1 . . ? C16 C17 C9 108.5(5) . . ? C16 C17 H8 125.7 . . ? C9 C17 H8 125.7 . . ? C19 C18 C23 119.9(5) . . ? C19 C18 C8 120.0(4) . . ? C23 C18 C8 120.1(5) . . ? C18 C19 C20 120.4(5) . . ? C18 C19 C25 121.3(5) . . ? C20 C19 C25 118.3(6) . . ? C21 C20 C19 120.1(6) . . ? C21 C20 H14 119.9 . . ? C19 C20 H14 119.9 . . ? C22 C21 C20 119.1(5) . . ? C22 C21 C75 123.1(6) . . ? C20 C21 C75 117.7(7) . . ? C21 C22 C23 122.1(6) . . ? C21 C22 H13 118.9 . . ? C23 C22 H13 118.9 . . ? C22 C23 C18 118.4(7) . . ? C22 C23 C24 120.1(6) . . ? C18 C23 C24 121.5(5) . . ? C23 C24 H10 109.5 . . ? C23 C24 H11 109.5 . . ? H10 C24 H11 109.5 . . ? C23 C24 H12 109.5 . . ? H10 C24 H12 109.5 . . ? H11 C24 H12 109.5 . . ? C19 C25 H17 109.5 . . ? C19 C25 H16 109.5 . . ? H17 C25 H16 109.5 . . ? C19 C25 H15 109.5 . . ? H17 C25 H15 109.5 . . ? H16 C25 H15 109.5 . . ? C27 C26 C7 106.3(5) . . ? C27 C26 H18 126.9 . . ? C7 C26 H18 126.9 . . ? C26 C27 C6 106.3(5) . . ? C26 C27 H19 126.8 . . ? C6 C27 H19 126.8 . . ? C29 C28 C4 106.3(5) . . ? C29 C28 H22 126.8 . . ? C4 C28 H22 126.8 . . ? C28 C29 C3 107.6(5) . . ? C28 C29 H21 126.2 . . ? C3 C29 H21 126.2 . . ? C31 C30 C35 119.8(5) . . ? C31 C30 C2 120.0(4) . . ? C35 C30 C2 120.3(5) . . ? C32 C31 C30 118.3(5) . . ? C32 C31 C37 121.4(6) . . ? C30 C31 C37 120.3(5) . . ? C33 C32 C31 123.1(6) . . ? C33 C32 H28 118.5 . . ? C31 C32 H28 118.5 . . ? C34 C33 C32 117.3(5) . . ? C34 C33 C76 120.7(6) . . ? C32 C33 C76 122.0(6) . . ? C35 C34 C33 123.1(6) . . ? C35 C34 H26 118.5 . . ? C33 C34 H26 118.5 . . ? C34 C35 C30 118.5(6) . . ? C34 C35 C36 121.2(6) . . ? C30 C35 C36 120.3(5) . . ? C35 C36 H24 109.5 . . ? C35 C36 H25 109.5 . . ? H24 C36 H25 109.5 . . ? C35 C36 H23 109.5 . . ? H24 C36 H23 109.5 . . ? H25 C36 H23 109.5 . . ? C31 C37 H30 109.5 . . ? C31 C37 H29 109.5 . . ? H30 C37 H29 109.5 . . ? C31 C37 H31 109.5 . . ? H30 C37 H31 109.5 . . ? H29 C37 H31 109.5 . . ? N12 C38 N9 126.7(4) . . ? N12 C38 C70 121.5(4) . . ? N9 C38 C70 111.7(5) . . ? N12 C39 N10 126.9(4) . . ? N12 C39 C74 122.7(5) . . ? N10 C39 C74 110.5(4) . . ? N10 C40 C41 124.6(4) . . ? N10 C40 C73 111.6(4) . . ? C41 C40 C73 123.8(4) . . ? C51 C41 C40 121.9(4) . . ? C51 C41 C42 118.9(4) . . ? C40 C41 C42 119.3(4) . . ? C43 C42 C47 121.2(5) . . ? C43 C42 C41 118.9(5) . . ? C47 C42 C41 119.9(5) . . ? C42 C43 C44 117.9(6) . . ? C42 C43 C50 121.3(5) . . ? C44 C43 C50 120.8(6) . . ? C45 C44 C43 121.4(6) . . ? C45 C44 H39 119.3 . . ? C43 C44 H39 119.3 . . ? C46 C45 C44 119.0(5) . . ? C46 C45 C49 120.9(7) . . ? C44 C45 C49 120.1(7) . . ? C47 C46 C45 121.4(5) . . ? C47 C46 H35 119.3 . . ? C45 C46 H35 119.3 . . ? C46 C47 C42 119.1(5) . . ? C46 C47 C48 118.6(5) . . ? C42 C47 C48 122.3(5) . . ? C47 C48 H32 109.5 . . ? C47 C48 H33 109.5 . . ? H32 C48 H33 109.5 . . ? C47 C48 H34 109.5 . . ? H32 C48 H34 109.5 . . ? H33 C48 H34 109.5 . . ? C45 C49 H37 109.5 . . ? C45 C49 H36 109.5 . . ? H37 C49 H36 109.5 . . ? C45 C49 H38 109.5 . . ? H37 C49 H38 109.5 . . ? H36 C49 H38 109.5 . . ? C43 C50 H40 109.5 . . ? C43 C50 H42 109.5 . . ? H40 C50 H42 109.5 . . ? C43 C50 H41 109.5 . . ? H40 C50 H41 109.5 . . ? H42 C50 H41 109.5 . . ? N11 C51 C41 126.1(4) . . ? N11 C51 C54 110.5(5) . . ? C41 C51 C54 123.4(5) . . ? N7 C52 N11 128.8(4) . . ? N7 C52 C53 120.6(4) . . ? N11 C52 C53 110.5(5) . . ? C54 C53 C52 106.3(4) . . ? C54 C53 H43 126.9 . . ? C52 C53 H43 126.8 . . ? C53 C54 C51 106.8(5) . . ? C53 C54 H44 126.6 . . ? C51 C54 H44 126.6 . . ? C56 N7 C52 120.2(4) . . ? N7 C56 N8 129.9(5) . . ? N7 C56 C72 118.1(5) . . ? N8 C56 C72 112.0(4) . . ? C58 C57 N8 125.6(4) . . ? C58 C57 C71 122.0(4) . . ? N8 C57 C71 112.4(4) . . ? C57 C58 C68 122.1(4) . . ? C57 C58 C59 121.0(4) . . ? C68 C58 C59 116.9(4) . . ? C64 C59 C60 121.2(5) . . ? C64 C59 C58 119.1(5) . . ? C60 C59 C58 119.6(5) . . ? C61 C60 C59 118.8(6) . . ? C61 C60 C67 119.9(6) . . ? C59 C60 C67 121.3(5) . . ? C62 C61 C60 121.6(6) . . ? C62 C61 H53 119.2 . . ? C60 C61 H53 119.2 . . ? C63 C62 C61 118.3(5) . . ? C63 C62 C66 120.1(7) . . ? C61 C62 C66 121.5(7) . . ? C62 C63 C64 123.2(6) . . ? C62 C63 H49 118.4 . . ? C64 C63 H49 118.4 . . ? C63 C64 C59 116.9(5) . . ? C63 C64 C65 121.7(5) . . ? C59 C64 C65 121.4(5) . . ? C64 C65 H48 109.5 . . ? C64 C65 H47 109.5 . . ? H48 C65 H47 109.5 . . ? C64 C65 H46 109.5 . . ? H48 C65 H46 109.5 . . ? H47 C65 H46 109.5 . . ? C62 C66 H50 109.5 . . ? C62 C66 H51 109.5 . . ? H50 C66 H51 109.5 . . ? C62 C66 H52 109.5 . . ? H50 C66 H52 109.5 . . ? H51 C66 H52 109.5 . . ? C60 C67 H56 109.5 . . ? C60 C67 H55 109.5 . . ? H56 C67 H55 109.5 . . ? C60 C67 H54 109.5 . . ? H56 C67 H54 109.5 . . ? H55 C67 H54 109.5 . . ? C58 C68 N9 124.7(4) . . ? C58 C68 C69 124.9(5) . . ? N9 C68 C69 110.4(5) . . ? C70 C69 C68 107.3(5) . . ? C70 C69 H58 126.4 . . ? C68 C69 H58 126.4 . . ? C69 C70 C38 107.5(5) . . ? C69 C70 H57 126.3 . . ? C38 C70 H57 126.3 . . ? C72 C71 C57 104.6(5) . . ? C72 C71 H60 127.7 . . ? C57 C71 H60 127.7 . . ? C77 C72 C71 132.1(7) . . ? C77 C72 C56 124.5(7) . . ? C71 C72 C56 103.4(5) . . ? C74 C73 C40 104.9(5) . . ? C74 C73 H61 127.5 . . ? C40 C73 H61 127.5 . . ? C73 C74 C39 109.1(5) . . ? C73 C74 H62 125.5 . . ? C39 C74 H62 125.5 . . ? C33 C76 H76A 109.5 . . ? C33 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C33 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C72 C77 H77A 109.5 . . ? C72 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C72 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C2S C3S C4S 116.0(13) . . ? C2S C3S H3S1 108.3 . . ? C4S C3S H3S1 108.3 . . ? C2S C3S H3S2 108.3 . . ? C4S C3S H3S2 108.3 . . ? H3S1 C3S H3S2 107.4 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C1S C2S C3S 118.4(13) . . ? C1S C2S H2S1 107.7 . . ? C3S C2S H2S1 107.7 . . ? C1S C2S H2S2 107.7 . . ? C3S C2S H2S2 107.7 . . ? H2S1 C2S H2S2 107.1 . . ? C5S C6S H6S1 109.5 . . ? C5S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? C5S C4S C3S 117.0(10) . . ? C5S C4S H4S1 108.0 . . ? C3S C4S H4S1 108.0 . . ? C5S C4S H4S2 108.1 . . ? C3S C4S H4S2 108.0 . . ? H4S1 C4S H4S2 107.3 . . ? C4S C5S C6S 117.5(11) . . ? C4S C5S H5S1 107.9 . . ? C6S C5S H5S1 107.9 . . ? C4S C5S H5S2 107.9 . . ? C6S C5S H5S2 107.9 . . ? H5S1 C5S H5S2 107.2 . . ? 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 N2 Ni1 N1 C12 177.3(5) . . . . ? N4 Ni1 N1 C12 -2.8(5) . . . . ? N3 Ni1 N1 C12 -171(15) . . . . ? N2 Ni1 N1 C1 -2.2(5) . . . . ? N4 Ni1 N1 C1 177.7(5) . . . . ? N3 Ni1 N1 C1 10(16) . . . . ? N4 Ni1 N2 C4 12(29) . . . . ? N1 Ni1 N2 C4 -177.2(6) . . . . ? N3 Ni1 N2 C4 3.0(6) . . . . ? N4 Ni1 N2 C3 -171(28) . . . . ? N1 Ni1 N2 C3 0.2(6) . . . . ? N3 Ni1 N2 C3 -179.6(6) . . . . ? N2 Ni1 N3 C6 0.4(5) . . . . ? N4 Ni1 N3 C6 -179.5(5) . . . . ? N1 Ni1 N3 C6 -12(16) . . . . ? N2 Ni1 N3 C7 179.9(5) . . . . ? N4 Ni1 N3 C7 0.0(5) . . . . ? N1 Ni1 N3 C7 168(15) . . . . ? N2 Ni1 N4 C10 173(100) . . . . ? N1 Ni1 N4 C10 1.8(6) . . . . ? N3 Ni1 N4 C10 -178.4(6) . . . . ? N2 Ni1 N4 C9 -10(29) . . . . ? N1 Ni1 N4 C9 178.8(6) . . . . ? N3 Ni1 N4 C9 -1.4(6) . . . . ? N10 Ni2 N9 C38 -0.9(5) . . . . ? N11 Ni2 N9 C38 -61(16) . . . . ? N8 Ni2 N9 C38 178.6(5) . . . . ? N10 Ni2 N9 C68 177.6(5) . . . . ? N11 Ni2 N9 C68 118(16) . . . . ? N8 Ni2 N9 C68 -2.9(5) . . . . ? N9 Ni2 N10 C40 179.9(4) . . . . ? N11 Ni2 N10 C40 -1.2(4) . . . . ? N8 Ni2 N10 C40 75(18) . . . . ? N9 Ni2 N10 C39 2.1(4) . . . . ? N11 Ni2 N10 C39 -179.0(4) . . . . ? N8 Ni2 N10 C39 -103(18) . . . . ? N9 Ni2 N11 C52 -121(16) . . . . ? N10 Ni2 N11 C52 179.0(5) . . . . ? N8 Ni2 N11 C52 -0.5(5) . . . . ? N9 Ni2 N11 C51 59(16) . . . . ? N10 Ni2 N11 C51 -0.9(5) . . . . ? N8 Ni2 N11 C51 179.7(5) . . . . ? N9 Ni2 N8 C56 -178.0(4) . . . . ? N10 Ni2 N8 C56 -73(18) . . . . ? N11 Ni2 N8 C56 3.1(4) . . . . ? N9 Ni2 N8 C57 0.9(4) . . . . ? N10 Ni2 N8 C57 106(18) . . . . ? N11 Ni2 N8 C57 -178.0(4) . . . . ? C12 N1 C1 C2 -176.8(5) . . . . ? Ni1 N1 C1 C2 2.8(8) . . . . ? C12 N1 C1 C14 2.4(6) . . . . ? Ni1 N1 C1 C14 -178.0(4) . . . . ? N1 C1 C2 C3 -0.7(8) . . . . ? C14 C1 C2 C3 -179.8(5) . . . . ? N1 C1 C2 C30 176.3(5) . . . . ? C14 C1 C2 C30 -2.9(8) . . . . ? C4 N2 C3 C2 179.4(5) . . . . ? Ni1 N2 C3 C2 1.5(9) . . . . ? C4 N2 C3 C29 -0.5(7) . . . . ? Ni1 N2 C3 C29 -178.4(5) . . . . ? C1 C2 C3 N2 -1.5(9) . . . . ? C30 C2 C3 N2 -178.4(5) . . . . ? C1 C2 C3 C29 178.4(5) . . . . ? C30 C2 C3 C29 1.4(8) . . . . ? C3 N2 C4 N5 176.9(6) . . . . ? Ni1 N2 C4 N5 -5.1(10) . . . . ? C3 N2 C4 C28 0.1(7) . . . . ? Ni1 N2 C4 C28 178.0(5) . . . . ? N2 C4 N5 C6 2.6(10) . . . . ? C28 C4 N5 C6 179.2(6) . . . . ? C4 N5 C6 N3 1.4(10) . . . . ? C4 N5 C6 C27 -178.6(7) . . . . ? C7 N3 C6 N5 177.8(6) . . . . ? Ni1 N3 C6 N5 -2.6(9) . . . . ? C7 N3 C6 C27 -2.2(7) . . . . ? Ni1 N3 C6 C27 177.3(5) . . . . ? C6 N3 C7 C8 179.7(5) . . . . ? Ni1 N3 C7 C8 0.1(8) . . . . ? C6 N3 C7 C26 -0.8(6) . . . . ? Ni1 N3 C7 C26 179.6(4) . . . . ? N3 C7 C8 C9 1.1(8) . . . . ? C26 C7 C8 C9 -178.4(5) . . . . ? N3 C7 C8 C18 -179.9(5) . . . . ? C26 C7 C8 C18 0.7(8) . . . . ? C7 C8 C9 N4 -2.6(9) . . . . ? C18 C8 C9 N4 178.3(6) . . . . ? C7 C8 C9 C17 179.3(5) . . . . ? C18 C8 C9 C17 0.3(8) . . . . ? C10 N4 C9 C8 -179.7(5) . . . . ? Ni1 N4 C9 C8 2.9(9) . . . . ? C10 N4 C9 C17 -1.3(7) . . . . ? Ni1 N4 C9 C17 -178.8(5) . . . . ? C9 N4 C10 N6 -179.3(6) . . . . ? Ni1 N4 C10 N6 -1.8(11) . . . . ? C9 N4 C10 C16 2.0(8) . . . . ? Ni1 N4 C10 C16 179.5(5) . . . . ? N4 C10 N6 C12 1.9(10) . . . . ? C16 C10 N6 C12 -179.5(6) . . . . ? C10 N6 C12 N1 -3.1(10) . . . . ? C10 N6 C12 C13 175.8(6) . . . . ? C1 N1 C12 N6 -176.3(6) . . . . ? Ni1 N1 C12 N6 4.1(9) . . . . ? C1 N1 C12 C13 4.7(7) . . . . ? Ni1 N1 C12 C13 -174.9(5) . . . . ? N6 C12 C13 C14 171.3(6) . . . . ? N1 C12 C13 C14 -9.7(8) . . . . ? N6 C12 C13 C15 -73.5(8) . . . . ? N1 C12 C13 C15 105.6(6) . . . . ? C2 C1 C14 C13 170.8(6) . . . . ? N1 C1 C14 C13 -8.5(7) . . . . ? C12 C13 C14 C1 10.1(8) . . . . ? C15 C13 C14 C1 -104.7(6) . . . . ? N6 C10 C16 C17 179.3(6) . . . . ? N4 C10 C16 C17 -2.0(8) . . . . ? C10 C16 C17 C9 1.1(8) . . . . ? C8 C9 C17 C16 178.5(6) . . . . ? N4 C9 C17 C16 0.1(8) . . . . ? C9 C8 C18 C19 -95.6(6) . . . . ? C7 C8 C18 C19 85.3(6) . . . . ? C9 C8 C18 C23 82.5(7) . . . . ? C7 C8 C18 C23 -96.6(7) . . . . ? C23 C18 C19 C20 0.6(9) . . . . ? C8 C18 C19 C20 178.6(5) . . . . ? C23 C18 C19 C25 -178.5(7) . . . . ? C8 C18 C19 C25 -0.5(8) . . . . ? C18 C19 C20 C21 -2.1(9) . . . . ? C25 C19 C20 C21 177.1(6) . . . . ? C19 C20 C21 C22 2.2(9) . . . . ? C19 C20 C21 C75 179.1(6) . . . . ? C20 C21 C22 C23 -1.0(10) . . . . ? C75 C21 C22 C23 -177.6(7) . . . . ? C21 C22 C23 C18 -0.5(11) . . . . ? C21 C22 C23 C24 178.3(7) . . . . ? C19 C18 C23 C22 0.6(10) . . . . ? C8 C18 C23 C22 -177.4(6) . . . . ? C19 C18 C23 C24 -178.1(7) . . . . ? C8 C18 C23 C24 3.9(10) . . . . ? C8 C7 C26 C27 -176.8(6) . . . . ? N3 C7 C26 C27 3.7(8) . . . . ? C7 C26 C27 C6 -4.8(9) . . . . ? N5 C6 C27 C26 -175.4(6) . . . . ? N3 C6 C27 C26 4.6(9) . . . . ? N5 C4 C28 C29 -176.7(6) . . . . ? N2 C4 C28 C29 0.4(8) . . . . ? C4 C28 C29 C3 -0.7(8) . . . . ? N2 C3 C29 C28 0.8(8) . . . . ? C2 C3 C29 C28 -179.1(6) . . . . ? C1 C2 C30 C31 -86.0(6) . . . . ? C3 C2 C30 C31 91.1(6) . . . . ? C1 C2 C30 C35 94.9(7) . . . . ? C3 C2 C30 C35 -88.1(7) . . . . ? C35 C30 C31 C32 -0.6(8) . . . . ? C2 C30 C31 C32 -179.7(5) . . . . ? C35 C30 C31 C37 179.6(7) . . . . ? C2 C30 C31 C37 0.5(8) . . . . ? C30 C31 C32 C33 0.8(9) . . . . ? C37 C31 C32 C33 -179.4(7) . . . . ? C31 C32 C33 C34 0.3(9) . . . . ? C31 C32 C33 C76 178.9(7) . . . . ? C32 C33 C34 C35 -1.8(10) . . . . ? C76 C33 C34 C35 179.6(7) . . . . ? C33 C34 C35 C30 2.0(10) . . . . ? C33 C34 C35 C36 -177.1(6) . . . . ? C31 C30 C35 C34 -0.8(9) . . . . ? C2 C30 C35 C34 178.3(6) . . . . ? C31 C30 C35 C36 178.3(6) . . . . ? C2 C30 C35 C36 -2.6(9) . . . . ? C39 N12 C38 N9 0.2(8) . . . . ? C39 N12 C38 C70 -176.5(5) . . . . ? C68 N9 C38 N12 -178.9(5) . . . . ? Ni2 N9 C38 N12 -0.1(9) . . . . ? C68 N9 C38 C70 -1.8(6) . . . . ? Ni2 N9 C38 C70 177.0(4) . . . . ? C38 N12 C39 N10 1.2(8) . . . . ? C38 N12 C39 C74 -178.6(5) . . . . ? C40 N10 C39 N12 179.1(5) . . . . ? Ni2 N10 C39 N12 -2.7(7) . . . . ? C40 N10 C39 C74 -1.1(5) . . . . ? Ni2 N10 C39 C74 177.2(4) . . . . ? C39 N10 C40 C41 -178.5(5) . . . . ? Ni2 N10 C40 C41 3.3(7) . . . . ? C39 N10 C40 C73 -0.6(5) . . . . ? Ni2 N10 C40 C73 -178.8(4) . . . . ? N10 C40 C41 C51 -3.2(7) . . . . ? C73 C40 C41 C51 179.1(5) . . . . ? N10 C40 C41 C42 176.4(4) . . . . ? C73 C40 C41 C42 -1.3(7) . . . . ? C51 C41 C42 C43 -86.8(6) . . . . ? C40 C41 C42 C43 93.7(6) . . . . ? C51 C41 C42 C47 91.6(6) . . . . ? C40 C41 C42 C47 -88.0(6) . . . . ? C47 C42 C43 C44 0.1(8) . . . . ? C41 C42 C43 C44 178.5(5) . . . . ? C47 C42 C43 C50 -178.9(5) . . . . ? C41 C42 C43 C50 -0.6(8) . . . . ? C42 C43 C44 C45 -2.3(8) . . . . ? C50 C43 C44 C45 176.7(5) . . . . ? C43 C44 C45 C46 3.5(8) . . . . ? C43 C44 C45 C49 -175.1(5) . . . . ? C44 C45 C46 C47 -2.4(8) . . . . ? C49 C45 C46 C47 176.1(5) . . . . ? C45 C46 C47 C42 0.3(7) . . . . ? C45 C46 C47 C48 178.3(6) . . . . ? C43 C42 C47 C46 0.8(7) . . . . ? C41 C42 C47 C46 -177.5(4) . . . . ? C43 C42 C47 C48 -177.0(6) . . . . ? C41 C42 C47 C48 4.7(8) . . . . ? C52 N11 C51 C41 -178.9(5) . . . . ? Ni2 N11 C51 C41 1.0(8) . . . . ? C52 N11 C51 C54 0.0(6) . . . . ? Ni2 N11 C51 C54 179.9(5) . . . . ? C40 C41 C51 N11 1.0(8) . . . . ? C42 C41 C51 N11 -178.5(5) . . . . ? C40 C41 C51 C54 -177.7(5) . . . . ? C42 C41 C51 C54 2.7(7) . . . . ? C51 N11 C52 N7 177.9(5) . . . . ? Ni2 N11 C52 N7 -2.0(9) . . . . ? C51 N11 C52 C53 -0.5(6) . . . . ? Ni2 N11 C52 C53 179.7(4) . . . . ? N7 C52 C53 C54 -177.8(5) . . . . ? N11 C52 C53 C54 0.7(7) . . . . ? C52 C53 C54 C51 -0.7(7) . . . . ? N11 C51 C54 C53 0.4(7) . . . . ? C41 C51 C54 C53 179.3(5) . . . . ? N11 C52 N7 C56 2.1(9) . . . . ? C53 C52 N7 C56 -179.7(5) . . . . ? C52 N7 C56 N8 1.1(9) . . . . ? C52 N7 C56 C72 -175.9(7) . . . . ? C57 N8 C56 N7 176.9(6) . . . . ? Ni2 N8 C56 N7 -4.0(9) . . . . ? C57 N8 C56 C72 -6.0(7) . . . . ? Ni2 N8 C56 C72 173.2(6) . . . . ? C56 N8 C57 C58 179.6(5) . . . . ? Ni2 N8 C57 C58 0.5(7) . . . . ? C56 N8 C57 C71 -0.9(6) . . . . ? Ni2 N8 C57 C71 -180.0(4) . . . . ? N8 C57 C58 C68 -0.5(8) . . . . ? C71 C57 C58 C68 180.0(5) . . . . ? N8 C57 C58 C59 179.9(5) . . . . ? C71 C57 C58 C59 0.4(7) . . . . ? C57 C58 C59 C64 85.6(6) . . . . ? C68 C58 C59 C64 -94.0(6) . . . . ? C57 C58 C59 C60 -95.9(6) . . . . ? C68 C58 C59 C60 84.5(6) . . . . ? C64 C59 C60 C61 1.1(8) . . . . ? C58 C59 C60 C61 -177.3(5) . . . . ? C64 C59 C60 C67 179.0(5) . . . . ? C58 C59 C60 C67 0.5(7) . . . . ? C59 C60 C61 C62 0.0(8) . . . . ? C67 C60 C61 C62 -177.9(5) . . . . ? C60 C61 C62 C63 -1.3(9) . . . . ? C60 C61 C62 C66 178.6(6) . . . . ? C61 C62 C63 C64 1.7(9) . . . . ? C66 C62 C63 C64 -178.2(6) . . . . ? C62 C63 C64 C59 -0.7(8) . . . . ? C62 C63 C64 C65 178.0(6) . . . . ? C60 C59 C64 C63 -0.7(7) . . . . ? C58 C59 C64 C63 177.7(4) . . . . ? C60 C59 C64 C65 -179.5(5) . . . . ? C58 C59 C64 C65 -1.1(7) . . . . ? C57 C58 C68 N9 -1.6(8) . . . . ? C59 C58 C68 N9 178.0(5) . . . . ? C57 C58 C68 C69 179.8(5) . . . . ? C59 C58 C68 C69 -0.6(7) . . . . ? C38 N9 C68 C58 -177.5(5) . . . . ? Ni2 N9 C68 C58 3.7(8) . . . . ? C38 N9 C68 C69 1.3(6) . . . . ? Ni2 N9 C68 C69 -177.5(4) . . . . ? C58 C68 C69 C70 178.5(5) . . . . ? N9 C68 C69 C70 -0.3(7) . . . . ? C68 C69 C70 C38 -0.8(7) . . . . ? N12 C38 C70 C69 179.0(5) . . . . ? N9 C38 C70 C69 1.7(7) . . . . ? C58 C57 C71 C72 -173.0(6) . . . . ? N8 C57 C71 C72 7.4(7) . . . . ? C57 C71 C72 C77 171.0(15) . . . . ? C57 C71 C72 C56 -9.9(8) . . . . ? N7 C56 C72 C77 7.1(17) . . . . ? N8 C56 C72 C77 -170.4(13) . . . . ? N7 C56 C72 C71 -172.1(6) . . . . ? N8 C56 C72 C71 10.4(9) . . . . ? N10 C40 C73 C74 2.1(6) . . . . ? C41 C40 C73 C74 -180.0(5) . . . . ? C40 C73 C74 C39 -2.6(6) . . . . ? N12 C39 C74 C73 -177.7(5) . . . . ? N10 C39 C74 C73 2.4(6) . . . . ? C4S C3S C2S C1S -163.4(18) . . . . ? C2S C3S C4S C5S -139(2) . . . . ? C3S C4S C5S C6S -178.1(15) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.645 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.076 data_12606ay _database_code_depnum_ccdc_archive 'CCDC 928788' #TrackingRef 'web_deposit_cif_file_2_HiroshiShinokubo_1363047956.12606ay.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H32 N6 Ni' _chemical_formula_weight 619.40 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.477(5) _cell_length_b 24.012(15) _cell_length_c 7.890(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.629(10) _cell_angle_gamma 90.00 _cell_volume 1503.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4077 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.86 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6464 _exptl_absorpt_correction_T_max 0.8755 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8091 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 4 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2947 _reflns_number_gt 2339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+0.3976P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2947 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1359 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0468(3) 0.44486(10) 0.6530(4) 0.0528(6) Uani 1 1 d . B . C2 C 0.0204(4) 0.40083(12) 0.5746(5) 0.0604(7) Uani 1 1 d . . . H10 H -0.0203 0.3894 0.4514 0.072 Uiso 0.50 1 calc P A 2 C3 C 0.1500(4) 0.37915(11) 0.7073(5) 0.0614(7) Uani 1 1 d . B . H3 H 0.2206 0.3497 0.6961 0.074 Uiso 1 1 calc R . . C4 C 0.1640(3) 0.40824(9) 0.8702(4) 0.0524(6) Uani 1 1 d . . . C5 C 0.2826(3) 0.39667(10) 1.0384(4) 0.0543(7) Uani 1 1 d . B . C6 C 0.2892(3) 0.42527(10) 1.1931(4) 0.0530(6) Uani 1 1 d . . . C7 C 0.4058(3) 0.41390(12) 1.3705(5) 0.0642(8) Uani 1 1 d . B . H7 H 0.4905 0.3859 1.4021 0.077 Uiso 1 1 calc R . . C8 C 0.3742(3) 0.44971(12) 1.4843(5) 0.0645(8) Uani 1 1 d . . . H8 H 0.4316 0.4522 1.6114 0.077 Uiso 1 1 calc R B . C9 C 0.2346(3) 0.48412(11) 1.3745(4) 0.0558(7) Uani 1 1 d . . . C11 C 0.4074(3) 0.35043(10) 1.0549(4) 0.0560(7) Uani 1 1 d . . . C12 C 0.5670(4) 0.36214(11) 1.0465(5) 0.0618(7) Uani 1 1 d . B . C13 C 0.6769(3) 0.31819(12) 1.0593(4) 0.0626(7) Uani 1 1 d . . . H13 H 0.7843 0.3258 1.0520 0.075 Uiso 1 1 calc R B . C14 C 0.6358(3) 0.26352(11) 1.0825(4) 0.0573(7) Uani 1 1 d . B . C15 C 0.4786(3) 0.25315(10) 1.0931(4) 0.0575(7) Uani 1 1 d . . . H15 H 0.4487 0.2160 1.1098 0.069 Uiso 1 1 calc R B . C16 C 0.3639(3) 0.29553(10) 1.0801(4) 0.0546(7) Uani 1 1 d . B . C17 C 0.6197(4) 0.42152(13) 1.0278(7) 0.0913(12) Uani 1 1 d . . . H17A H 0.5263 0.4412 0.9376 0.137 Uiso 1 1 calc R B . H17B H 0.7175 0.4212 0.9889 0.137 Uiso 1 1 calc R . . H17C H 0.6495 0.4405 1.1448 0.137 Uiso 1 1 calc R . . C18 C 0.7577(4) 0.21628(13) 1.0954(5) 0.0750(9) Uani 1 1 d . . . H18A H 0.7347 0.1857 1.1654 0.112 Uiso 1 1 calc R B . H18B H 0.8734 0.2295 1.1556 0.112 Uiso 1 1 calc R . . H18C H 0.7439 0.2031 0.9734 0.112 Uiso 1 1 calc R . . C19 C 0.1935(4) 0.28203(12) 1.0921(5) 0.0723(9) Uani 1 1 d . . . H19A H 0.1819 0.2416 1.0994 0.108 Uiso 1 1 calc R B . H19B H 0.1041 0.2962 0.9842 0.108 Uiso 1 1 calc R . . H19C H 0.1843 0.2995 1.2004 0.108 Uiso 1 1 calc R . . N1 N 0.0408(2) 0.44894(7) 0.8345(3) 0.0476(5) Uani 1 1 d . B . N2 N 0.1823(2) 0.46877(8) 1.1963(3) 0.0485(5) Uani 1 1 d . B . N3 N -0.1757(3) 0.47555(10) 0.5511(3) 0.0591(6) Uani 1 1 d . . . Ni1 Ni 0.0000 0.5000 1.0000 0.04433(19) Uani 1 2 d S . . C10 C -0.0365(9) 0.3861(3) 0.4027(9) 0.0736(17) Uani 0.50 1 d P B 1 H10A H 0.0216 0.3523 0.3872 0.110 Uiso 0.50 1 calc PR B 1 H10B H -0.0155 0.4162 0.3294 0.110 Uiso 0.50 1 calc PR B 1 H10C H -0.1579 0.3789 0.3637 0.110 Uiso 0.50 1 calc PR B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0483(13) 0.0362(12) 0.0787(19) 0.0025(12) 0.0283(13) -0.0038(10) C2 0.0653(17) 0.0427(14) 0.0798(19) -0.0090(14) 0.0339(14) -0.0081(12) C3 0.0613(16) 0.0372(13) 0.094(2) -0.0044(13) 0.0381(16) 0.0006(11) C4 0.0490(13) 0.0305(11) 0.0853(19) 0.0048(11) 0.0331(13) -0.0008(9) C5 0.0469(13) 0.0321(12) 0.090(2) 0.0103(12) 0.0310(14) 0.0033(10) C6 0.0447(13) 0.0357(12) 0.0830(19) 0.0124(12) 0.0282(13) 0.0044(10) C7 0.0521(15) 0.0483(15) 0.090(2) 0.0149(14) 0.0231(15) 0.0081(12) C8 0.0524(15) 0.0574(17) 0.080(2) 0.0130(15) 0.0191(14) 0.0065(13) C9 0.0486(14) 0.0433(13) 0.0765(19) 0.0083(13) 0.0232(14) -0.0011(11) C11 0.0504(14) 0.0373(12) 0.086(2) 0.0088(12) 0.0308(13) 0.0063(10) C12 0.0522(14) 0.0445(14) 0.096(2) 0.0063(14) 0.0344(14) 0.0005(12) C13 0.0460(14) 0.0589(17) 0.089(2) -0.0013(15) 0.0309(14) 0.0018(12) C14 0.0519(15) 0.0501(15) 0.0686(18) -0.0035(12) 0.0195(13) 0.0119(11) C15 0.0538(15) 0.0355(13) 0.0808(19) 0.0046(12) 0.0210(14) 0.0074(10) C16 0.0472(13) 0.0361(12) 0.0844(19) 0.0080(12) 0.0281(13) 0.0050(10) C17 0.071(2) 0.0546(18) 0.162(4) 0.018(2) 0.059(2) -0.0060(15) C18 0.0626(18) 0.0638(18) 0.098(2) -0.0039(17) 0.0276(17) 0.0228(14) C19 0.0555(16) 0.0452(15) 0.125(3) 0.0209(16) 0.0420(17) 0.0051(12) N1 0.0436(10) 0.0290(9) 0.0749(15) 0.0054(9) 0.0267(10) 0.0002(8) N2 0.0441(10) 0.0314(9) 0.0746(15) 0.0084(9) 0.0269(10) 0.0007(8) N3 0.0537(13) 0.0491(13) 0.0757(16) 0.0013(12) 0.0243(12) -0.0009(10) Ni1 0.0404(3) 0.0263(2) 0.0709(3) 0.00746(17) 0.0253(2) 0.00023(14) C10 0.083(4) 0.074(4) 0.065(4) -0.012(3) 0.028(3) -0.016(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N3 1.328(3) . ? C1 N1 1.365(4) . ? C1 C2 1.440(4) . ? C2 C10 1.318(7) . ? C2 C3 1.329(4) . ? C2 H10 0.9500 . ? C3 C4 1.430(4) . ? C3 H3 0.9500 . ? C4 C5 1.382(4) . ? C4 N1 1.385(3) . ? C5 C6 1.384(4) . ? C5 C11 1.508(3) . ? C6 N2 1.389(3) . ? C6 C7 1.427(4) . ? C7 C8 1.336(5) . ? C7 H7 0.9500 . ? C8 C9 1.453(4) . ? C8 H8 0.9500 . ? C9 N3 1.318(4) 3_567 ? C9 N2 1.368(4) . ? C11 C16 1.402(4) . ? C11 C12 1.406(4) . ? C12 C13 1.388(4) . ? C12 C17 1.517(4) . ? C13 C14 1.387(4) . ? C13 H13 0.9500 . ? C14 C15 1.387(4) . ? C14 C18 1.514(4) . ? C15 C16 1.386(3) . ? C15 H15 0.9500 . ? C16 C19 1.515(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N1 Ni1 1.909(2) . ? N2 Ni1 1.914(2) . ? N3 C9 1.318(4) 3_567 ? Ni1 N1 1.909(2) 3_567 ? Ni1 N2 1.914(2) 3_567 ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 N3 C1 N1 128.5(2) . . ? N3 C1 C2 120.9(3) . . ? N1 C1 C2 110.6(2) . . ? C10 C2 C3 127.4(4) . . ? C10 C2 C1 125.6(4) . . ? C3 C2 C1 107.0(3) . . ? C10 C2 H10 1.2 . . ? C3 C2 H10 126.5 . . ? C1 C2 H10 126.5 . . ? C2 C3 C4 107.5(2) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? C5 C4 N1 125.3(3) . . ? C5 C4 C3 124.5(2) . . ? N1 C4 C3 110.1(3) . . ? C4 C5 C6 122.5(2) . . ? C4 C5 C11 118.8(3) . . ? C6 C5 C11 118.7(3) . . ? C5 C6 N2 124.4(2) . . ? C5 C6 C7 124.7(2) . . ? N2 C6 C7 110.9(3) . . ? C8 C7 C6 107.6(2) . . ? C8 C7 H7 126.2 . . ? C6 C7 H7 126.2 . . ? C7 C8 C9 106.3(3) . . ? C7 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? N3 C9 N2 128.3(3) 3_567 . ? N3 C9 C8 120.6(3) 3_567 . ? N2 C9 C8 111.1(3) . . ? C16 C11 C12 120.0(2) . . ? C16 C11 C5 119.5(2) . . ? C12 C11 C5 120.4(2) . . ? C13 C12 C11 118.5(2) . . ? C13 C12 C17 120.5(3) . . ? C11 C12 C17 120.9(3) . . ? C14 C13 C12 122.4(3) . . ? C14 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C13 C14 C15 118.0(2) . . ? C13 C14 C18 121.4(3) . . ? C15 C14 C18 120.6(3) . . ? C16 C15 C14 121.8(2) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C11 119.2(2) . . ? C15 C16 C19 119.8(2) . . ? C11 C16 C19 121.0(2) . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 H18A 109.5 . . ? C14 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C14 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C1 N1 C4 104.8(2) . . ? C1 N1 Ni1 126.94(17) . . ? C4 N1 Ni1 128.3(2) . . ? C9 N2 C6 104.2(2) . . ? C9 N2 Ni1 127.09(18) . . ? C6 N2 Ni1 128.7(2) . . ? C9 N3 C1 119.9(3) 3_567 . ? N1 Ni1 N1 180.00(11) . 3_567 ? N1 Ni1 N2 89.28(10) . 3_567 ? N1 Ni1 N2 90.72(10) 3_567 3_567 ? N1 Ni1 N2 90.72(10) . . ? N1 Ni1 N2 89.28(10) 3_567 . ? N2 Ni1 N2 180.000(1) 3_567 . ? C2 C10 H10A 109.5 . . ? C2 C10 H10B 109.5 . . ? C2 C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.596 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.067