# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Christopher Levy' _publ_contact_author_email clevy@ksu.edu loop_ _publ_author_name C.Levy D.Prema K.Oshin J.Desper data_(R,R)-1 _database_code_depnum_ccdc_archive 'CCDC 846322' #TrackingRef '- output.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; KO0802 Ni-benzoquinoline imine I ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C34 H28 N4) Ni I2 (C H2 Cl2) ; _chemical_formula_sum 'C35 H30 Cl2 I2 N4 Ni' _chemical_formula_weight 890.04 _chemical_absolute_configuration ad 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' I I -0.4742 1.8119 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.3765(12) _cell_length_b 24.333(3) _cell_length_c 13.5813(15) _cell_angle_alpha 90.00 _cell_angle_beta 104.936(5) _cell_angle_gamma 90.00 _cell_volume 3313.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9828 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 33.03 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 2.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6201 _exptl_absorpt_correction_T_max 0.7781 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 50478 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 33.14 _reflns_number_total 22909 _reflns_number_gt 20081 _reflns_threshold_expression >2sigma(I) _reflns_Friedel_coverage 0.798 _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^)+(0.0350P)^2^+0.0300P] 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 0.017(9) _refine_ls_number_reflns 22909 _refine_ls_number_parameters 793 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Cl1_1 Cl 0.19696(16) 0.51869(6) 0.76542(12) 0.0746(4) Uani 1 1 d . . . Cl2_1 Cl 0.34005(11) 0.41423(6) 0.79061(10) 0.0603(3) Uani 1 1 d . . . C1S_1 C 0.2294(4) 0.45755(19) 0.8339(3) 0.0504(10) Uani 1 1 d . . . H1A_1 H 0.1443 0.4378 0.8281 0.060 Uiso 1 1 calc R . . H1B_1 H 0.2682 0.4661 0.9067 0.060 Uiso 1 1 calc R . . Ni1_1 Ni 0.84672(4) 0.315596(16) 0.75059(3) 0.02285(7) Uani 1 1 d . . . I1_1 I 0.60289(2) 0.311041(8) 0.629813(17) 0.03056(5) Uani 1 1 d . . . I2_1 I 1.01887(2) 0.346828(8) 0.922012(16) 0.03297(5) Uani 1 1 d . . . N11_1 N 0.8228(3) 0.23283(10) 0.8101(2) 0.0240(5) Uani 1 1 d . . . C12_1 C 0.8845(3) 0.19803(13) 0.7596(3) 0.0282(6) Uani 1 1 d . . . C13_1 C 0.8894(4) 0.14102(12) 0.7745(3) 0.0325(7) Uani 1 1 d . . . H13_1 H 0.9313 0.1179 0.7357 0.039 Uiso 1 1 calc R . . C14_1 C 0.8326(4) 0.11957(13) 0.8459(3) 0.0345(7) Uani 1 1 d . . . H14_1 H 0.8356 0.0811 0.8583 0.041 Uiso 1 1 calc R . . C15_1 C 0.7697(4) 0.15465(13) 0.9011(3) 0.0326(7) Uani 1 1 d . . . C16_1 C 0.7137(4) 0.13327(15) 0.9799(3) 0.0467(10) Uani 1 1 d . . . H16_1 H 0.7190 0.0950 0.9938 0.056 Uiso 1 1 calc R . . C17_1 C 0.6545(5) 0.16599(16) 1.0336(4) 0.0531(12) Uani 1 1 d . . . H17_1 H 0.6197 0.1507 1.0857 0.064 Uiso 1 1 calc R . . C18_1 C 0.6426(4) 0.22392(14) 1.0140(3) 0.0364(8) Uani 1 1 d . . . C19_1 C 0.5730(4) 0.25697(16) 1.0684(3) 0.0413(9) Uani 1 1 d . . . H19_1 H 0.5393 0.2410 1.1206 0.050 Uiso 1 1 calc R . . C20_1 C 0.5534(4) 0.31194(16) 1.0468(3) 0.0365(7) Uani 1 1 d . . . H20_1 H 0.5060 0.3339 1.0835 0.044 Uiso 1 1 calc R . . C21_1 C 0.6035(3) 0.33529(13) 0.9704(3) 0.0321(7) Uani 1 1 d . . . H21_1 H 0.5898 0.3733 0.9551 0.039 Uiso 1 1 calc R . . C22_1 C 0.6727(3) 0.30372(11) 0.9170(3) 0.0277(6) Uani 1 1 d . . . H22_1 H 0.7062 0.3203 0.8653 0.033 Uiso 1 1 calc R . . C23_1 C 0.6945(3) 0.24767(12) 0.9374(2) 0.0253(6) Uani 1 1 d . . . C24_1 C 0.7654(3) 0.21223(12) 0.8811(2) 0.0272(6) Uani 1 1 d . . . C25_1 C 0.9443(3) 0.22103(13) 0.6826(2) 0.0282(6) Uani 1 1 d . . . H25_1 H 0.9892 0.1982 0.6454 0.034 Uiso 1 1 calc R . . N25_1 N 0.9345(2) 0.27244(10) 0.66656(18) 0.0238(5) Uani 1 1 d . . . N31_1 N 0.7742(3) 0.51446(10) 0.6664(2) 0.0248(5) Uani 1 1 d . . . C32_1 C 0.7887(3) 0.46375(12) 0.7034(2) 0.0257(6) Uani 1 1 d . . . C33_1 C 0.7315(3) 0.44538(13) 0.7817(3) 0.0281(6) Uani 1 1 d . . . H33_1 H 0.7443 0.4087 0.8062 0.034 Uiso 1 1 calc R . . C34_1 C 0.6574(3) 0.48172(13) 0.8212(2) 0.0282(6) Uani 1 1 d . . . H34_1 H 0.6191 0.4706 0.8744 0.034 Uiso 1 1 calc R . . C35_1 C 0.6383(3) 0.53555(13) 0.7825(3) 0.0291(6) Uani 1 1 d . . . C36_1 C 0.5590(4) 0.57503(16) 0.8175(3) 0.0448(9) Uani 1 1 d . . . H36_1 H 0.5198 0.5659 0.8713 0.054 Uiso 1 1 calc R . . C37_1 C 0.5394(5) 0.62534(16) 0.7743(4) 0.0563(12) Uani 1 1 d . . . H37_1 H 0.4850 0.6509 0.7981 0.068 Uiso 1 1 calc R . . C38_1 C 0.5974(4) 0.64156(14) 0.6943(3) 0.0403(8) Uani 1 1 d . . . C39_1 C 0.5724(4) 0.69351(16) 0.6473(4) 0.0503(11) Uani 1 1 d . . . H39_1 H 0.5196 0.7194 0.6719 0.060 Uiso 1 1 calc R . . C40_1 C 0.6223(4) 0.70727(16) 0.5678(4) 0.0505(11) Uani 1 1 d . . . H40_1 H 0.6041 0.7425 0.5372 0.061 Uiso 1 1 calc R . . C41_1 C 0.7001(4) 0.66994(15) 0.5307(3) 0.0412(8) Uani 1 1 d . . . H41_1 H 0.7340 0.6797 0.4745 0.049 Uiso 1 1 calc R . . C42_1 C 0.7281(3) 0.61877(14) 0.5752(3) 0.0336(7) Uani 1 1 d . . . H42_1 H 0.7815 0.5935 0.5498 0.040 Uiso 1 1 calc R . . C43_1 C 0.6774(3) 0.60419(13) 0.6585(3) 0.0297(6) Uani 1 1 d . . . C44_1 C 0.6983(3) 0.55008(13) 0.7036(2) 0.0254(6) Uani 1 1 d . . . C45_1 C 0.8799(3) 0.43150(12) 0.6587(2) 0.0253(6) Uani 1 1 d . . . H45_1 H 0.9201 0.4507 0.6135 0.030 Uiso 1 1 calc R . . N45_1 N 0.9113(2) 0.38107(10) 0.67342(19) 0.0240(5) Uani 1 1 d . . . C51_1 C 0.9782(3) 0.30199(11) 0.5866(2) 0.0268(6) Uani 1 1 d . . . H51_1 H 0.8988 0.3066 0.5271 0.032 Uiso 1 1 calc R . . C52_1 C 1.0867(3) 0.27342(13) 0.5489(2) 0.0304(6) Uani 1 1 d . . . H52A_1 H 1.0532 0.2377 0.5175 0.036 Uiso 1 1 calc R . . H52B_1 H 1.1648 0.2662 0.6070 0.036 Uiso 1 1 calc R . . C53_1 C 1.1285(3) 0.31005(14) 0.4698(2) 0.0352(6) Uani 1 1 d . . . H53A_1 H 1.2022 0.2922 0.4478 0.042 Uiso 1 1 calc R . . H53B_1 H 1.0522 0.3145 0.4092 0.042 Uiso 1 1 calc R . . C54_1 C 1.1734(3) 0.36585(14) 0.5147(2) 0.0346(6) Uani 1 1 d . . . H54A_1 H 1.1984 0.3889 0.4625 0.042 Uiso 1 1 calc R . . H54B_1 H 1.2533 0.3615 0.5725 0.042 Uiso 1 1 calc R . . C55_1 C 1.0630(3) 0.39481(12) 0.5519(2) 0.0292(6) Uani 1 1 d . . . H55A_1 H 1.0963 0.4306 0.5829 0.035 Uiso 1 1 calc R . . H55B_1 H 0.9854 0.4019 0.4934 0.035 Uiso 1 1 calc R . . C56_1 C 1.0200(3) 0.35907(11) 0.6304(2) 0.0245(5) Uani 1 1 d . . . H56_1 H 1.1003 0.3540 0.6890 0.029 Uiso 1 1 calc R . . Cl3_2 Cl 0.16763(14) 0.42958(7) 0.23308(12) 0.0796(4) Uani 1 1 d . . . Cl4_2 Cl 0.32021(18) 0.32793(8) 0.25265(13) 0.0933(5) Uani 1 1 d . . . C2S_2 C 0.2732(6) 0.3871(3) 0.1811(4) 0.0725(16) Uani 1 1 d . . . H2A_2 H 0.2259 0.3768 0.1105 0.087 Uiso 1 1 calc R . . H2B_2 H 0.3540 0.4081 0.1784 0.087 Uiso 1 1 calc R . . Ni2_2 Ni 0.65834(4) 0.526687(15) 0.25226(3) 0.02247(8) Uani 1 1 d . . . I3_2 I 0.49078(2) 0.489804(8) 0.082846(16) 0.03123(5) Uani 1 1 d . . . I4_2 I 0.89958(2) 0.539094(8) 0.373911(17) 0.03204(5) Uani 1 1 d . . . N11_2 N 0.6688(3) 0.60829(10) 0.1884(2) 0.0259(5) Uani 1 1 d . . . C12_2 C 0.6010(3) 0.64261(13) 0.2341(3) 0.0300(7) Uani 1 1 d . . . C13_2 C 0.5967(4) 0.69978(14) 0.2227(3) 0.0358(7) Uani 1 1 d . . . H13_2 H 0.5502 0.7222 0.2593 0.043 Uiso 1 1 calc R . . C14_2 C 0.6622(4) 0.72212(14) 0.1565(3) 0.0417(9) Uani 1 1 d . . . H14_2 H 0.6626 0.7608 0.1474 0.050 Uiso 1 1 calc R . . C15_2 C 0.7275(4) 0.68865(14) 0.1032(3) 0.0363(8) Uani 1 1 d . . . C16_2 C 0.7875(5) 0.71138(16) 0.0291(4) 0.0559(12) Uani 1 1 d . . . H16_2 H 0.7825 0.7498 0.0165 0.067 Uiso 1 1 calc R . . C17_2 C 0.8500(6) 0.67964(19) -0.0223(5) 0.0695(16) Uani 1 1 d . . . H17_2 H 0.8877 0.6961 -0.0718 0.083 Uiso 1 1 calc R . . C18_2 C 0.8637(4) 0.62117(16) -0.0069(3) 0.0421(9) Uani 1 1 d . . . C19_2 C 0.9339(4) 0.58819(18) -0.0604(3) 0.0500(10) Uani 1 1 d . . . H19_2 H 0.9692 0.6047 -0.1112 0.060 Uiso 1 1 calc R . . C20_2 C 0.9532(4) 0.53373(16) -0.0422(3) 0.0397(8) Uani 1 1 d . . . H20_2 H 1.0007 0.5124 -0.0798 0.048 Uiso 1 1 calc R . . C21_2 C 0.9016(4) 0.50940(15) 0.0333(3) 0.0356(7) Uani 1 1 d . . . H21_2 H 0.9160 0.4714 0.0483 0.043 Uiso 1 1 calc R . . C22_2 C 0.8307(3) 0.54028(14) 0.0853(3) 0.0325(7) Uani 1 1 d . . . H22_2 H 0.7955 0.5227 0.1352 0.039 Uiso 1 1 calc R . . C23_2 C 0.8079(3) 0.59639(13) 0.0682(3) 0.0296(6) Uani 1 1 d . . . C24_2 C 0.7346(3) 0.63071(13) 0.1218(2) 0.0266(6) Uani 1 1 d . . . C25_2 C 0.5203(3) 0.61675(13) 0.2967(2) 0.0310(6) Uani 1 1 d . . . H25_2 H 0.4642 0.6380 0.3274 0.037 Uiso 1 1 calc R . . N25_2 N 0.5290(2) 0.56525(10) 0.30763(19) 0.0259(5) Uani 1 1 d . . . N31_2 N 0.7345(3) 0.32706(10) 0.3314(2) 0.0254(5) Uani 1 1 d . . . C32_2 C 0.7216(3) 0.37915(12) 0.2982(2) 0.0247(6) Uani 1 1 d . . . C33_2 C 0.7812(3) 0.39871(13) 0.2233(3) 0.0285(6) Uani 1 1 d . . . H33_2 H 0.7702 0.4359 0.2016 0.034 Uiso 1 1 calc R . . C34_2 C 0.8556(3) 0.36322(13) 0.1817(3) 0.0303(6) Uani 1 1 d . . . H34_2 H 0.8954 0.3756 0.1301 0.036 Uiso 1 1 calc R . . C35_2 C 0.8727(3) 0.30863(13) 0.2156(2) 0.0275(6) Uani 1 1 d . . . C36_2 C 0.9577(5) 0.27070(16) 0.1817(3) 0.0457(9) Uani 1 1 d . . . H36_2 H 1.0004 0.2813 0.1306 0.055 Uiso 1 1 calc R . . C37_2 C 0.9769(5) 0.22001(16) 0.2223(3) 0.0524(11) Uani 1 1 d . . . H37_2 H 1.0367 0.1959 0.2014 0.063 Uiso 1 1 calc R . . C38_2 C 0.9103(4) 0.20111(13) 0.2961(3) 0.0379(8) Uani 1 1 d . . . C39_2 C 0.9330(4) 0.14782(14) 0.3369(3) 0.0439(9) Uani 1 1 d . . . H39_2 H 0.9903 0.1235 0.3135 0.053 Uiso 1 1 calc R . . C40_2 C 0.8724(4) 0.13077(15) 0.4108(3) 0.0415(8) Uani 1 1 d . . . H40_2 H 0.8880 0.0947 0.4382 0.050 Uiso 1 1 calc R . . C41_2 C 0.7880(4) 0.16650(15) 0.4452(3) 0.0387(8) Uani 1 1 d . . . H41_2 H 0.7464 0.1545 0.4961 0.046 Uiso 1 1 calc R . . C42_2 C 0.7644(3) 0.21890(14) 0.4065(3) 0.0319(7) Uani 1 1 d . . . H42_2 H 0.7067 0.2428 0.4306 0.038 Uiso 1 1 calc R . . C43_2 C 0.8257(3) 0.23696(12) 0.3315(3) 0.0269(6) Uani 1 1 d . . . C44_2 C 0.8076(3) 0.29223(12) 0.2908(2) 0.0247(6) Uani 1 1 d . . . C45_2 C 0.6468(3) 0.41212(13) 0.3559(2) 0.0266(6) Uani 1 1 d . . . H45_2 H 0.6158 0.3932 0.4064 0.032 Uiso 1 1 calc R . . N45_2 N 0.6189(2) 0.46317(10) 0.34565(19) 0.0244(5) Uani 1 1 d . . . C51_2 C 0.4527(3) 0.53118(11) 0.3608(2) 0.0261(5) Uani 1 1 d . . . H51_2 H 0.3833 0.5112 0.3082 0.031 Uiso 1 1 calc R . . C52_2 C 0.3819(3) 0.56194(14) 0.4299(3) 0.0334(7) Uani 1 1 d . . . H52A_2 H 0.4475 0.5840 0.4803 0.040 Uiso 1 1 calc R . . H52B_2 H 0.3149 0.5874 0.3885 0.040 Uiso 1 1 calc R . . C53_2 C 0.3131(3) 0.52137(15) 0.4854(3) 0.0381(7) Uani 1 1 d . . . H53A_2 H 0.2717 0.5416 0.5326 0.046 Uiso 1 1 calc R . . H53B_2 H 0.2415 0.5019 0.4352 0.046 Uiso 1 1 calc R . . C54_2 C 0.4123(3) 0.47984(14) 0.5450(2) 0.0336(6) Uani 1 1 d . . . H54A_2 H 0.3646 0.4531 0.5778 0.040 Uiso 1 1 calc R . . H54B_2 H 0.4786 0.4992 0.5996 0.040 Uiso 1 1 calc R . . C55_2 C 0.4848(3) 0.44900(13) 0.4781(2) 0.0289(6) Uani 1 1 d . . . H55A_2 H 0.4204 0.4257 0.4292 0.035 Uiso 1 1 calc R . . H55B_2 H 0.5530 0.4246 0.5211 0.035 Uiso 1 1 calc R . . C56_2 C 0.5520(3) 0.48844(12) 0.4196(2) 0.0250(5) Uani 1 1 d . . . H56_2 H 0.6219 0.5089 0.4710 0.030 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 Cl1_1 0.0825(9) 0.0710(8) 0.0695(8) 0.0192(7) 0.0182(7) -0.0123(7) Cl2_1 0.0400(5) 0.0828(8) 0.0526(6) 0.0001(6) 0.0022(4) -0.0112(5) C1S_1 0.050(2) 0.062(2) 0.0350(19) 0.0038(18) 0.0028(17) -0.0139(19) Ni1_1 0.02646(17) 0.02254(16) 0.02109(17) -0.00114(15) 0.00892(14) -0.00062(15) I1_1 0.02916(10) 0.03171(9) 0.02892(10) 0.00249(8) 0.00406(8) -0.00341(8) I2_1 0.03676(11) 0.03729(10) 0.02279(9) 0.00053(8) 0.00394(8) -0.00682(8) N11_1 0.0249(12) 0.0233(11) 0.0233(12) 0.0001(10) 0.0051(9) -0.0001(9) C12_1 0.0320(15) 0.0264(13) 0.0259(15) -0.0046(12) 0.0069(12) 0.0012(12) C13_1 0.0390(17) 0.0212(13) 0.0354(18) -0.0030(13) 0.0061(14) 0.0038(12) C14_1 0.0410(18) 0.0211(13) 0.0398(19) 0.0002(13) 0.0078(15) 0.0016(13) C15_1 0.0380(17) 0.0243(14) 0.0358(18) 0.0024(13) 0.0098(14) -0.0023(13) C16_1 0.064(3) 0.0241(15) 0.061(3) 0.0082(17) 0.034(2) -0.0015(16) C17_1 0.082(3) 0.0313(17) 0.063(3) 0.0156(18) 0.049(3) 0.0032(19) C18_1 0.0426(19) 0.0309(16) 0.0389(19) 0.0060(14) 0.0162(16) -0.0033(14) C19_1 0.050(2) 0.0449(19) 0.039(2) 0.0020(16) 0.0290(18) -0.0075(17) C20_1 0.0400(18) 0.0371(16) 0.0371(18) -0.0031(16) 0.0188(15) 0.0005(16) C21_1 0.0361(16) 0.0283(15) 0.0345(17) 0.0009(13) 0.0136(14) 0.0018(13) C22_1 0.0336(16) 0.0239(15) 0.0273(16) 0.0000(11) 0.0113(13) -0.0007(11) C23_1 0.0276(14) 0.0224(12) 0.0274(15) -0.0005(11) 0.0099(12) -0.0039(11) C24_1 0.0301(15) 0.0224(13) 0.0267(15) -0.0002(12) 0.0030(12) -0.0051(11) C25_1 0.0294(14) 0.0301(14) 0.0252(14) -0.0033(12) 0.0070(11) 0.0027(11) N25_1 0.0242(11) 0.0257(11) 0.0215(11) -0.0021(9) 0.0059(9) -0.0015(9) N31_1 0.0261(12) 0.0230(11) 0.0274(13) 0.0001(10) 0.0107(10) -0.0018(10) C32_1 0.0307(15) 0.0224(13) 0.0251(15) -0.0020(11) 0.0095(12) -0.0024(11) C33_1 0.0349(16) 0.0224(13) 0.0287(16) 0.0018(12) 0.0112(13) 0.0006(12) C34_1 0.0342(15) 0.0310(14) 0.0224(13) 0.0004(12) 0.0130(12) -0.0050(13) C35_1 0.0311(15) 0.0283(15) 0.0292(16) -0.0021(12) 0.0099(12) 0.0004(12) C36_1 0.058(2) 0.0371(17) 0.053(2) 0.0017(16) 0.039(2) 0.0052(16) C37_1 0.067(3) 0.0327(17) 0.084(3) 0.001(2) 0.047(3) 0.0124(19) C38_1 0.0357(18) 0.0315(16) 0.056(2) 0.0055(16) 0.0155(17) 0.0031(14) C39_1 0.0396(19) 0.0318(17) 0.080(3) 0.013(2) 0.017(2) 0.0044(15) C40_1 0.0376(19) 0.0337(18) 0.073(3) 0.0174(19) 0.0003(19) -0.0032(15) C41_1 0.0415(18) 0.0346(17) 0.044(2) 0.0121(15) 0.0044(15) -0.0105(15) C42_1 0.0361(16) 0.0290(15) 0.0347(17) 0.0036(13) 0.0072(13) -0.0053(13) C43_1 0.0288(15) 0.0242(13) 0.0333(16) 0.0006(12) 0.0031(13) -0.0003(12) C44_1 0.0261(13) 0.0264(14) 0.0235(14) 0.0009(11) 0.0058(11) -0.0023(11) C45_1 0.0279(13) 0.0259(13) 0.0246(14) -0.0017(11) 0.0115(11) -0.0030(11) N45_1 0.0270(11) 0.0258(11) 0.0205(11) -0.0022(9) 0.0081(9) -0.0008(9) C51_1 0.0306(13) 0.0294(14) 0.0223(13) -0.0026(10) 0.0100(11) 0.0008(10) C52_1 0.0318(14) 0.0329(14) 0.0296(15) -0.0050(12) 0.0137(12) 0.0008(12) C53_1 0.0342(15) 0.0446(17) 0.0325(15) -0.0035(14) 0.0190(13) 0.0001(14) C54_1 0.0341(15) 0.0418(16) 0.0324(15) -0.0019(14) 0.0166(12) -0.0035(13) C55_1 0.0333(15) 0.0290(14) 0.0291(14) -0.0008(12) 0.0150(12) -0.0012(12) C56_1 0.0230(11) 0.0278(13) 0.0241(12) -0.0035(10) 0.0087(10) -0.0017(10) Cl3_2 0.0526(7) 0.1086(11) 0.0676(8) 0.0011(8) -0.0027(6) -0.0260(7) Cl4_2 0.0997(11) 0.1061(12) 0.0800(10) 0.0281(9) 0.0341(9) -0.0034(10) C2S_2 0.078(3) 0.102(4) 0.038(2) -0.009(3) 0.016(2) -0.038(3) Ni2_2 0.02460(18) 0.02308(16) 0.02059(18) -0.00049(14) 0.00740(15) 0.00066(13) I3_2 0.03446(10) 0.03283(9) 0.02418(10) -0.00396(8) 0.00354(8) -0.00109(8) I4_2 0.02606(9) 0.04157(11) 0.02763(10) 0.00182(8) 0.00537(8) -0.00414(8) N11_2 0.0291(13) 0.0229(11) 0.0242(13) 0.0001(10) 0.0043(10) -0.0011(10) C12_2 0.0350(16) 0.0247(13) 0.0287(16) -0.0006(12) 0.0051(13) 0.0018(12) C13_2 0.0395(18) 0.0270(15) 0.0389(19) -0.0028(14) 0.0066(15) 0.0037(13) C14_2 0.048(2) 0.0215(14) 0.051(2) 0.0021(15) 0.0046(18) -0.0032(14) C15_2 0.0370(18) 0.0271(15) 0.044(2) 0.0050(15) 0.0101(15) -0.0088(13) C16_2 0.074(3) 0.0313(17) 0.075(3) 0.016(2) 0.041(3) -0.0027(19) C17_2 0.091(4) 0.050(2) 0.089(4) 0.027(3) 0.062(3) -0.001(3) C18_2 0.046(2) 0.0430(19) 0.046(2) 0.0064(17) 0.0272(18) -0.0065(16) C19_2 0.056(3) 0.055(2) 0.049(2) 0.011(2) 0.031(2) -0.005(2) C20_2 0.0365(17) 0.052(2) 0.0350(18) -0.0057(16) 0.0174(15) -0.0070(16) C21_2 0.0441(19) 0.0335(16) 0.0328(18) -0.0017(14) 0.0162(16) -0.0015(15) C22_2 0.0370(17) 0.0343(15) 0.0295(17) 0.0025(14) 0.0145(14) -0.0023(14) C23_2 0.0306(16) 0.0324(15) 0.0254(15) 0.0025(12) 0.0066(12) -0.0073(13) C24_2 0.0263(14) 0.0250(13) 0.0272(15) 0.0027(12) 0.0047(12) -0.0040(11) C25_2 0.0332(15) 0.0320(15) 0.0274(14) -0.0031(12) 0.0070(12) 0.0061(12) N25_2 0.0261(11) 0.0295(12) 0.0217(11) -0.0024(9) 0.0053(9) 0.0022(9) N31_2 0.0284(12) 0.0253(11) 0.0230(12) 0.0010(10) 0.0076(10) -0.0022(10) C32_2 0.0249(13) 0.0241(13) 0.0262(15) 0.0018(11) 0.0085(11) 0.0009(11) C33_2 0.0361(16) 0.0232(13) 0.0293(15) 0.0061(12) 0.0138(13) 0.0007(12) C34_2 0.0366(16) 0.0291(14) 0.0284(15) 0.0028(13) 0.0139(13) 0.0013(13) C35_2 0.0351(15) 0.0248(13) 0.0252(14) 0.0020(12) 0.0124(12) 0.0014(12) C36_2 0.070(3) 0.0359(17) 0.043(2) 0.0033(16) 0.035(2) 0.0098(18) C37_2 0.082(3) 0.0375(19) 0.051(2) 0.0073(18) 0.042(2) 0.020(2) C38_2 0.052(2) 0.0242(14) 0.0417(19) 0.0030(14) 0.0201(17) 0.0067(14) C39_2 0.055(2) 0.0271(15) 0.051(2) 0.0043(15) 0.0173(19) 0.0084(16) C40_2 0.047(2) 0.0255(15) 0.048(2) 0.0114(15) 0.0052(16) 0.0004(14) C41_2 0.0443(19) 0.0324(15) 0.0396(19) 0.0106(14) 0.0109(15) -0.0078(14) C42_2 0.0353(16) 0.0286(14) 0.0314(16) -0.0002(12) 0.0077(13) -0.0073(13) C43_2 0.0307(15) 0.0245(13) 0.0265(14) 0.0007(11) 0.0091(12) -0.0040(12) C44_2 0.0294(14) 0.0223(12) 0.0223(13) -0.0007(11) 0.0068(12) -0.0005(12) C45_2 0.0263(13) 0.0278(13) 0.0268(14) 0.0026(11) 0.0092(11) 0.0003(11) N45_2 0.0239(11) 0.0281(11) 0.0226(11) -0.0015(9) 0.0083(9) -0.0001(9) C51_2 0.0260(12) 0.0318(14) 0.0219(12) -0.0009(10) 0.0085(10) 0.0013(10) C52_2 0.0345(15) 0.0377(16) 0.0305(15) -0.0048(13) 0.0126(13) 0.0063(13) C53_2 0.0335(15) 0.0482(18) 0.0398(18) -0.0048(15) 0.0222(14) 0.0030(14) C54_2 0.0341(14) 0.0421(17) 0.0275(13) -0.0045(13) 0.0132(12) -0.0082(13) C55_2 0.0301(14) 0.0323(14) 0.0279(14) 0.0021(12) 0.0139(12) -0.0008(12) C56_2 0.0262(12) 0.0284(12) 0.0220(12) -0.0007(11) 0.0089(10) 0.0007(11) _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 Cl1_1 C1S_1 1.740(5) . ? Cl2_1 C1S_1 1.767(5) . ? C1S_1 H1A_1 0.9900 . ? C1S_1 H1B_1 0.9900 . ? Ni1_1 N25_1 1.942(2) . ? Ni1_1 N45_1 2.109(3) . ? Ni1_1 N11_1 2.208(3) . ? Ni1_1 I1_1 2.6391(5) . ? Ni1_1 I2_1 2.6543(5) . ? N11_1 C12_1 1.350(4) . ? N11_1 C24_1 1.353(4) . ? C12_1 C13_1 1.401(4) . ? C12_1 C25_1 1.459(5) . ? C13_1 C14_1 1.361(5) . ? C13_1 H13_1 0.9500 . ? C14_1 C15_1 1.404(5) . ? C14_1 H14_1 0.9500 . ? C15_1 C24_1 1.426(4) . ? C15_1 C16_1 1.440(5) . ? C16_1 C17_1 1.332(6) . ? C16_1 H16_1 0.9500 . ? C17_1 C18_1 1.434(5) . ? C17_1 H17_1 0.9500 . ? C18_1 C19_1 1.411(5) . ? C18_1 C23_1 1.412(5) . ? C19_1 C20_1 1.373(5) . ? C19_1 H19_1 0.9500 . ? C20_1 C21_1 1.395(5) . ? C20_1 H20_1 0.9500 . ? C21_1 C22_1 1.378(5) . ? C21_1 H21_1 0.9500 . ? C22_1 C23_1 1.398(4) . ? C22_1 H22_1 0.9500 . ? C23_1 C24_1 1.470(5) . ? C25_1 N25_1 1.269(4) . ? C25_1 H25_1 0.9500 . ? N25_1 C51_1 1.468(4) . ? N31_1 C32_1 1.326(4) . ? N31_1 C44_1 1.354(4) . ? C32_1 C33_1 1.417(5) . ? C32_1 C45_1 1.474(4) . ? C33_1 C34_1 1.369(5) . ? C33_1 H33_1 0.9500 . ? C34_1 C35_1 1.406(4) . ? C34_1 H34_1 0.9500 . ? C35_1 C44_1 1.415(5) . ? C35_1 C36_1 1.424(5) . ? C36_1 C37_1 1.350(6) . ? C36_1 H36_1 0.9500 . ? C37_1 C38_1 1.427(6) . ? C37_1 H37_1 0.9500 . ? C38_1 C43_1 1.400(5) . ? C38_1 C39_1 1.410(5) . ? C39_1 C40_1 1.354(7) . ? C39_1 H39_1 0.9500 . ? C40_1 C41_1 1.393(6) . ? C40_1 H40_1 0.9500 . ? C41_1 C42_1 1.382(5) . ? C41_1 H41_1 0.9500 . ? C42_1 C43_1 1.411(5) . ? C42_1 H42_1 0.9500 . ? C43_1 C44_1 1.445(4) . ? C45_1 N45_1 1.272(4) . ? C45_1 H45_1 0.9500 . ? N45_1 C56_1 1.496(4) . ? C51_1 C52_1 1.521(4) . ? C51_1 C56_1 1.529(4) . ? C51_1 H51_1 1.0000 . ? C52_1 C53_1 1.541(4) . ? C52_1 H52A_1 0.9900 . ? C52_1 H52B_1 0.9900 . ? C53_1 C54_1 1.512(5) . ? C53_1 H53A_1 0.9900 . ? C53_1 H53B_1 0.9900 . ? C54_1 C55_1 1.537(4) . ? C54_1 H54A_1 0.9900 . ? C54_1 H54B_1 0.9900 . ? C55_1 C56_1 1.529(4) . ? C55_1 H55A_1 0.9900 . ? C55_1 H55B_1 0.9900 . ? C56_1 H56_1 1.0000 . ? Cl3_2 C2S_2 1.779(7) . ? Cl4_2 C2S_2 1.735(6) . ? C2S_2 H2A_2 0.9900 . ? C2S_2 H2B_2 0.9900 . ? Ni2_2 N25_2 1.941(2) . ? Ni2_2 N45_2 2.105(3) . ? Ni2_2 N11_2 2.181(3) . ? Ni2_2 I4_2 2.6373(5) . ? Ni2_2 I3_2 2.6571(5) . ? N11_2 C12_2 1.344(4) . ? N11_2 C24_2 1.378(4) . ? C12_2 C13_2 1.399(4) . ? C12_2 C25_2 1.479(5) . ? C13_2 C14_2 1.371(6) . ? C13_2 H13_2 0.9500 . ? C14_2 C15_2 1.378(6) . ? C14_2 H14_2 0.9500 . ? C15_2 C16_2 1.425(5) . ? C15_2 C24_2 1.431(5) . ? C16_2 C17_2 1.318(7) . ? C16_2 H16_2 0.9500 . ? C17_2 C18_2 1.440(6) . ? C17_2 H17_2 0.9500 . ? C18_2 C19_2 1.406(6) . ? C18_2 C23_2 1.429(5) . ? C19_2 C20_2 1.353(6) . ? C19_2 H19_2 0.9500 . ? C20_2 C21_2 1.404(5) . ? C20_2 H20_2 0.9500 . ? C21_2 C22_2 1.369(5) . ? C21_2 H21_2 0.9500 . ? C22_2 C23_2 1.395(5) . ? C22_2 H22_2 0.9500 . ? C23_2 C24_2 1.445(5) . ? C25_2 N25_2 1.262(4) . ? C25_2 H25_2 0.9500 . ? N25_2 C51_2 1.460(4) . ? N31_2 C32_2 1.340(4) . ? N31_2 C44_2 1.346(4) . ? C32_2 C33_2 1.403(4) . ? C32_2 C45_2 1.474(4) . ? C33_2 C34_2 1.373(5) . ? C33_2 H33_2 0.9500 . ? C34_2 C35_2 1.402(4) . ? C34_2 H34_2 0.9500 . ? C35_2 C44_2 1.420(4) . ? C35_2 C36_2 1.432(5) . ? C36_2 C37_2 1.345(5) . ? C36_2 H36_2 0.9500 . ? C37_2 C38_2 1.432(6) . ? C37_2 H37_2 0.9500 . ? C38_2 C39_2 1.406(5) . ? C38_2 C43_2 1.407(5) . ? C39_2 C40_2 1.378(6) . ? C39_2 H39_2 0.9500 . ? C40_2 C41_2 1.398(6) . ? C40_2 H40_2 0.9500 . ? C41_2 C42_2 1.377(5) . ? C41_2 H41_2 0.9500 . ? C42_2 C43_2 1.404(5) . ? C42_2 H42_2 0.9500 . ? C43_2 C44_2 1.448(4) . ? C45_2 N45_2 1.275(4) . ? C45_2 H45_2 0.9500 . ? N45_2 C56_2 1.492(4) . ? C51_2 C52_2 1.528(4) . ? C51_2 C56_2 1.535(4) . ? C51_2 H51_2 1.0000 . ? C52_2 C53_2 1.526(5) . ? C52_2 H52A_2 0.9900 . ? C52_2 H52B_2 0.9900 . ? C53_2 C54_2 1.519(5) . ? C53_2 H53A_2 0.9900 . ? C53_2 H53B_2 0.9900 . ? C54_2 C55_2 1.520(4) . ? C54_2 H54A_2 0.9900 . ? C54_2 H54B_2 0.9900 . ? C55_2 C56_2 1.524(4) . ? C55_2 H55A_2 0.9900 . ? C55_2 H55B_2 0.9900 . ? C56_2 H56_2 1.0000 . ? 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 Cl1_1 C1S_1 Cl2_1 112.7(3) . . ? Cl1_1 C1S_1 H1A_1 109.1 . . ? Cl2_1 C1S_1 H1A_1 109.1 . . ? Cl1_1 C1S_1 H1B_1 109.1 . . ? Cl2_1 C1S_1 H1B_1 109.1 . . ? H1A_1 C1S_1 H1B_1 107.8 . . ? N25_1 Ni1_1 N45_1 81.90(10) . . ? N25_1 Ni1_1 N11_1 80.55(10) . . ? N45_1 Ni1_1 N11_1 162.01(10) . . ? N25_1 Ni1_1 I1_1 97.58(7) . . ? N45_1 Ni1_1 I1_1 95.71(7) . . ? N11_1 Ni1_1 I1_1 90.51(7) . . ? N25_1 Ni1_1 I2_1 111.02(7) . . ? N45_1 Ni1_1 I2_1 89.50(7) . . ? N11_1 Ni1_1 I2_1 93.09(7) . . ? I1_1 Ni1_1 I2_1 151.385(18) . . ? C12_1 N11_1 C24_1 118.9(3) . . ? C12_1 N11_1 Ni1_1 105.9(2) . . ? C24_1 N11_1 Ni1_1 135.2(2) . . ? N11_1 C12_1 C13_1 123.5(3) . . ? N11_1 C12_1 C25_1 117.9(3) . . ? C13_1 C12_1 C25_1 118.5(3) . . ? C14_1 C13_1 C12_1 118.4(3) . . ? C14_1 C13_1 H13_1 120.8 . . ? C12_1 C13_1 H13_1 120.8 . . ? C13_1 C14_1 C15_1 119.6(3) . . ? C13_1 C14_1 H14_1 120.2 . . ? C15_1 C14_1 H14_1 120.2 . . ? C14_1 C15_1 C24_1 119.4(3) . . ? C14_1 C15_1 C16_1 120.6(3) . . ? C24_1 C15_1 C16_1 119.9(3) . . ? C17_1 C16_1 C15_1 121.5(3) . . ? C17_1 C16_1 H16_1 119.3 . . ? C15_1 C16_1 H16_1 119.3 . . ? C16_1 C17_1 C18_1 121.0(4) . . ? C16_1 C17_1 H17_1 119.5 . . ? C18_1 C17_1 H17_1 119.5 . . ? C19_1 C18_1 C23_1 119.8(3) . . ? C19_1 C18_1 C17_1 119.6(3) . . ? C23_1 C18_1 C17_1 120.5(3) . . ? C20_1 C19_1 C18_1 120.7(3) . . ? C20_1 C19_1 H19_1 119.7 . . ? C18_1 C19_1 H19_1 119.7 . . ? C19_1 C20_1 C21_1 119.5(3) . . ? C19_1 C20_1 H20_1 120.2 . . ? C21_1 C20_1 H20_1 120.2 . . ? C22_1 C21_1 C20_1 120.6(3) . . ? C22_1 C21_1 H21_1 119.7 . . ? C20_1 C21_1 H21_1 119.7 . . ? C21_1 C22_1 C23_1 121.3(3) . . ? C21_1 C22_1 H22_1 119.4 . . ? C23_1 C22_1 H22_1 119.4 . . ? C22_1 C23_1 C18_1 118.2(3) . . ? C22_1 C23_1 C24_1 123.1(3) . . ? C18_1 C23_1 C24_1 118.7(3) . . ? N11_1 C24_1 C15_1 120.1(3) . . ? N11_1 C24_1 C23_1 121.7(3) . . ? C15_1 C24_1 C23_1 118.2(3) . . ? N25_1 C25_1 C12_1 118.1(3) . . ? N25_1 C25_1 H25_1 120.9 . . ? C12_1 C25_1 H25_1 120.9 . . ? C25_1 N25_1 C51_1 125.7(3) . . ? C25_1 N25_1 Ni1_1 117.5(2) . . ? C51_1 N25_1 Ni1_1 116.79(18) . . ? C32_1 N31_1 C44_1 118.3(3) . . ? N31_1 C32_1 C33_1 123.3(3) . . ? N31_1 C32_1 C45_1 111.2(3) . . ? C33_1 C32_1 C45_1 125.3(3) . . ? C34_1 C33_1 C32_1 118.5(3) . . ? C34_1 C33_1 H33_1 120.8 . . ? C32_1 C33_1 H33_1 120.8 . . ? C33_1 C34_1 C35_1 119.6(3) . . ? C33_1 C34_1 H34_1 120.2 . . ? C35_1 C34_1 H34_1 120.2 . . ? C34_1 C35_1 C44_1 117.9(3) . . ? C34_1 C35_1 C36_1 122.8(3) . . ? C44_1 C35_1 C36_1 119.3(3) . . ? C37_1 C36_1 C35_1 120.1(4) . . ? C37_1 C36_1 H36_1 119.9 . . ? C35_1 C36_1 H36_1 119.9 . . ? C36_1 C37_1 C38_1 122.4(4) . . ? C36_1 C37_1 H37_1 118.8 . . ? C38_1 C37_1 H37_1 118.8 . . ? C43_1 C38_1 C39_1 118.8(4) . . ? C43_1 C38_1 C37_1 119.2(3) . . ? C39_1 C38_1 C37_1 121.9(4) . . ? C40_1 C39_1 C38_1 121.3(4) . . ? C40_1 C39_1 H39_1 119.4 . . ? C38_1 C39_1 H39_1 119.4 . . ? C39_1 C40_1 C41_1 120.2(4) . . ? C39_1 C40_1 H40_1 119.9 . . ? C41_1 C40_1 H40_1 119.9 . . ? C42_1 C41_1 C40_1 120.4(4) . . ? C42_1 C41_1 H41_1 119.8 . . ? C40_1 C41_1 H41_1 119.8 . . ? C41_1 C42_1 C43_1 119.8(3) . . ? C41_1 C42_1 H42_1 120.1 . . ? C43_1 C42_1 H42_1 120.1 . . ? C38_1 C43_1 C42_1 119.5(3) . . ? C38_1 C43_1 C44_1 118.9(3) . . ? C42_1 C43_1 C44_1 121.5(3) . . ? N31_1 C44_1 C35_1 122.3(3) . . ? N31_1 C44_1 C43_1 117.6(3) . . ? C35_1 C44_1 C43_1 120.1(3) . . ? N45_1 C45_1 C32_1 127.9(3) . . ? N45_1 C45_1 H45_1 116.0 . . ? C32_1 C45_1 H45_1 116.0 . . ? C45_1 N45_1 C56_1 118.2(2) . . ? C45_1 N45_1 Ni1_1 134.8(2) . . ? C56_1 N45_1 Ni1_1 106.95(17) . . ? N25_1 C51_1 C52_1 114.9(2) . . ? N25_1 C51_1 C56_1 105.5(2) . . ? C52_1 C51_1 C56_1 112.7(2) . . ? N25_1 C51_1 H51_1 107.8 . . ? C52_1 C51_1 H51_1 107.8 . . ? C56_1 C51_1 H51_1 107.8 . . ? C51_1 C52_1 C53_1 109.6(3) . . ? C51_1 C52_1 H52A_1 109.7 . . ? C53_1 C52_1 H52A_1 109.7 . . ? C51_1 C52_1 H52B_1 109.7 . . ? C53_1 C52_1 H52B_1 109.7 . . ? H52A_1 C52_1 H52B_1 108.2 . . ? C54_1 C53_1 C52_1 110.6(3) . . ? C54_1 C53_1 H53A_1 109.5 . . ? C52_1 C53_1 H53A_1 109.5 . . ? C54_1 C53_1 H53B_1 109.5 . . ? C52_1 C53_1 H53B_1 109.5 . . ? H53A_1 C53_1 H53B_1 108.1 . . ? C53_1 C54_1 C55_1 111.5(3) . . ? C53_1 C54_1 H54A_1 109.3 . . ? C55_1 C54_1 H54A_1 109.3 . . ? C53_1 C54_1 H54B_1 109.3 . . ? C55_1 C54_1 H54B_1 109.3 . . ? H54A_1 C54_1 H54B_1 108.0 . . ? C56_1 C55_1 C54_1 110.2(2) . . ? C56_1 C55_1 H55A_1 109.6 . . ? C54_1 C55_1 H55A_1 109.6 . . ? C56_1 C55_1 H55B_1 109.6 . . ? C54_1 C55_1 H55B_1 109.6 . . ? H55A_1 C55_1 H55B_1 108.1 . . ? N45_1 C56_1 C55_1 117.0(2) . . ? N45_1 C56_1 C51_1 108.1(2) . . ? C55_1 C56_1 C51_1 110.5(2) . . ? N45_1 C56_1 H56_1 107.0 . . ? C55_1 C56_1 H56_1 107.0 . . ? C51_1 C56_1 H56_1 107.0 . . ? Cl4_2 C2S_2 Cl3_2 111.9(3) . . ? Cl4_2 C2S_2 H2A_2 109.2 . . ? Cl3_2 C2S_2 H2A_2 109.2 . . ? Cl4_2 C2S_2 H2B_2 109.2 . . ? Cl3_2 C2S_2 H2B_2 109.2 . . ? H2A_2 C2S_2 H2B_2 107.9 . . ? N25_2 Ni2_2 N45_2 81.97(10) . . ? N25_2 Ni2_2 N11_2 79.89(11) . . ? N45_2 Ni2_2 N11_2 161.00(10) . . ? N25_2 Ni2_2 I4_2 109.96(7) . . ? N45_2 Ni2_2 I4_2 90.41(7) . . ? N11_2 Ni2_2 I4_2 90.48(7) . . ? N25_2 Ni2_2 I3_2 97.77(7) . . ? N45_2 Ni2_2 I3_2 95.07(7) . . ? N11_2 Ni2_2 I3_2 92.96(7) . . ? I4_2 Ni2_2 I3_2 152.221(18) . . ? C12_2 N11_2 C24_2 117.7(3) . . ? C12_2 N11_2 Ni2_2 107.2(2) . . ? C24_2 N11_2 Ni2_2 134.9(2) . . ? N11_2 C12_2 C13_2 124.9(3) . . ? N11_2 C12_2 C25_2 116.3(3) . . ? C13_2 C12_2 C25_2 118.7(3) . . ? C14_2 C13_2 C12_2 117.4(3) . . ? C14_2 C13_2 H13_2 121.3 . . ? C12_2 C13_2 H13_2 121.3 . . ? C13_2 C14_2 C15_2 120.3(3) . . ? C13_2 C14_2 H14_2 119.9 . . ? C15_2 C14_2 H14_2 119.9 . . ? C14_2 C15_2 C16_2 120.4(3) . . ? C14_2 C15_2 C24_2 120.0(3) . . ? C16_2 C15_2 C24_2 119.7(4) . . ? C17_2 C16_2 C15_2 120.7(4) . . ? C17_2 C16_2 H16_2 119.6 . . ? C15_2 C16_2 H16_2 119.6 . . ? C16_2 C17_2 C18_2 123.1(4) . . ? C16_2 C17_2 H17_2 118.5 . . ? C18_2 C17_2 H17_2 118.5 . . ? C19_2 C18_2 C23_2 119.2(4) . . ? C19_2 C18_2 C17_2 122.3(4) . . ? C23_2 C18_2 C17_2 118.5(4) . . ? C20_2 C19_2 C18_2 122.5(4) . . ? C20_2 C19_2 H19_2 118.8 . . ? C18_2 C19_2 H19_2 118.8 . . ? C19_2 C20_2 C21_2 118.7(4) . . ? C19_2 C20_2 H20_2 120.7 . . ? C21_2 C20_2 H20_2 120.7 . . ? C22_2 C21_2 C20_2 120.2(3) . . ? C22_2 C21_2 H21_2 119.9 . . ? C20_2 C21_2 H21_2 119.9 . . ? C21_2 C22_2 C23_2 122.8(3) . . ? C21_2 C22_2 H22_2 118.6 . . ? C23_2 C22_2 H22_2 118.6 . . ? C22_2 C23_2 C18_2 116.7(3) . . ? C22_2 C23_2 C24_2 124.8(3) . . ? C18_2 C23_2 C24_2 118.5(3) . . ? N11_2 C24_2 C15_2 119.6(3) . . ? N11_2 C24_2 C23_2 121.0(3) . . ? C15_2 C24_2 C23_2 119.4(3) . . ? N25_2 C25_2 C12_2 117.1(3) . . ? N25_2 C25_2 H25_2 121.4 . . ? C12_2 C25_2 H25_2 121.4 . . ? C25_2 N25_2 C51_2 126.2(3) . . ? C25_2 N25_2 Ni2_2 118.1(2) . . ? C51_2 N25_2 Ni2_2 115.76(18) . . ? C32_2 N31_2 C44_2 118.4(3) . . ? N31_2 C32_2 C33_2 122.7(3) . . ? N31_2 C32_2 C45_2 110.9(3) . . ? C33_2 C32_2 C45_2 126.3(3) . . ? C34_2 C33_2 C32_2 119.0(3) . . ? C34_2 C33_2 H33_2 120.5 . . ? C32_2 C33_2 H33_2 120.5 . . ? C33_2 C34_2 C35_2 119.9(3) . . ? C33_2 C34_2 H34_2 120.1 . . ? C35_2 C34_2 H34_2 120.1 . . ? C34_2 C35_2 C44_2 117.3(3) . . ? C34_2 C35_2 C36_2 122.8(3) . . ? C44_2 C35_2 C36_2 119.8(3) . . ? C37_2 C36_2 C35_2 119.8(4) . . ? C37_2 C36_2 H36_2 120.1 . . ? C35_2 C36_2 H36_2 120.1 . . ? C36_2 C37_2 C38_2 122.3(4) . . ? C36_2 C37_2 H37_2 118.8 . . ? C38_2 C37_2 H37_2 118.8 . . ? C39_2 C38_2 C43_2 119.6(4) . . ? C39_2 C38_2 C37_2 120.6(3) . . ? C43_2 C38_2 C37_2 119.7(3) . . ? C40_2 C39_2 C38_2 120.2(4) . . ? C40_2 C39_2 H39_2 119.9 . . ? C38_2 C39_2 H39_2 119.9 . . ? C39_2 C40_2 C41_2 120.0(3) . . ? C39_2 C40_2 H40_2 120.0 . . ? C41_2 C40_2 H40_2 120.0 . . ? C42_2 C41_2 C40_2 120.9(3) . . ? C42_2 C41_2 H41_2 119.6 . . ? C40_2 C41_2 H41_2 119.6 . . ? C41_2 C42_2 C43_2 119.8(3) . . ? C41_2 C42_2 H42_2 120.1 . . ? C43_2 C42_2 H42_2 120.1 . . ? C42_2 C43_2 C38_2 119.5(3) . . ? C42_2 C43_2 C44_2 122.0(3) . . ? C38_2 C43_2 C44_2 118.5(3) . . ? N31_2 C44_2 C35_2 122.7(3) . . ? N31_2 C44_2 C43_2 117.4(3) . . ? C35_2 C44_2 C43_2 119.8(3) . . ? N45_2 C45_2 C32_2 127.5(3) . . ? N45_2 C45_2 H45_2 116.3 . . ? C32_2 C45_2 H45_2 116.3 . . ? C45_2 N45_2 C56_2 117.4(3) . . ? C45_2 N45_2 Ni2_2 135.0(2) . . ? C56_2 N45_2 Ni2_2 107.41(17) . . ? N25_2 C51_2 C52_2 115.7(3) . . ? N25_2 C51_2 C56_2 105.4(2) . . ? C52_2 C51_2 C56_2 112.2(2) . . ? N25_2 C51_2 H51_2 107.8 . . ? C52_2 C51_2 H51_2 107.8 . . ? C56_2 C51_2 H51_2 107.8 . . ? C53_2 C52_2 C51_2 110.3(3) . . ? C53_2 C52_2 H52A_2 109.6 . . ? C51_2 C52_2 H52A_2 109.6 . . ? C53_2 C52_2 H52B_2 109.6 . . ? C51_2 C52_2 H52B_2 109.6 . . ? H52A_2 C52_2 H52B_2 108.1 . . ? C54_2 C53_2 C52_2 110.7(3) . . ? C54_2 C53_2 H53A_2 109.5 . . ? C52_2 C53_2 H53A_2 109.5 . . ? C54_2 C53_2 H53B_2 109.5 . . ? C52_2 C53_2 H53B_2 109.5 . . ? H53A_2 C53_2 H53B_2 108.1 . . ? C53_2 C54_2 C55_2 112.4(2) . . ? C53_2 C54_2 H54A_2 109.1 . . ? C55_2 C54_2 H54A_2 109.1 . . ? C53_2 C54_2 H54B_2 109.1 . . ? C55_2 C54_2 H54B_2 109.1 . . ? H54A_2 C54_2 H54B_2 107.8 . . ? C54_2 C55_2 C56_2 111.4(3) . . ? C54_2 C55_2 H55A_2 109.4 . . ? C56_2 C55_2 H55A_2 109.4 . . ? C54_2 C55_2 H55B_2 109.4 . . ? C56_2 C55_2 H55B_2 109.4 . . ? H55A_2 C55_2 H55B_2 108.0 . . ? N45_2 C56_2 C55_2 116.5(2) . . ? N45_2 C56_2 C51_2 107.2(2) . . ? C55_2 C56_2 C51_2 111.2(2) . . ? N45_2 C56_2 H56_2 107.2 . . ? C55_2 C56_2 H56_2 107.2 . . ? C51_2 C56_2 H56_2 107.2 . . ? 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 N25_1 Ni1_1 N11_1 C12_1 2.0(2) . . . . ? N45_1 Ni1_1 N11_1 C12_1 -10.9(4) . . . . ? I1_1 Ni1_1 N11_1 C12_1 99.6(2) . . . . ? I2_1 Ni1_1 N11_1 C12_1 -108.8(2) . . . . ? N25_1 Ni1_1 N11_1 C24_1 -178.9(3) . . . . ? N45_1 Ni1_1 N11_1 C24_1 168.2(3) . . . . ? I1_1 Ni1_1 N11_1 C24_1 -81.3(3) . . . . ? I2_1 Ni1_1 N11_1 C24_1 70.3(3) . . . . ? C24_1 N11_1 C12_1 C13_1 1.9(5) . . . . ? Ni1_1 N11_1 C12_1 C13_1 -178.8(3) . . . . ? C24_1 N11_1 C12_1 C25_1 179.3(3) . . . . ? Ni1_1 N11_1 C12_1 C25_1 -1.4(3) . . . . ? N11_1 C12_1 C13_1 C14_1 -2.2(6) . . . . ? C25_1 C12_1 C13_1 C14_1 -179.5(3) . . . . ? C12_1 C13_1 C14_1 C15_1 0.9(5) . . . . ? C13_1 C14_1 C15_1 C24_1 0.4(5) . . . . ? C13_1 C14_1 C15_1 C16_1 -177.5(4) . . . . ? C14_1 C15_1 C16_1 C17_1 179.4(4) . . . . ? C24_1 C15_1 C16_1 C17_1 1.6(7) . . . . ? C15_1 C16_1 C17_1 C18_1 0.9(8) . . . . ? C16_1 C17_1 C18_1 C19_1 176.5(5) . . . . ? C16_1 C17_1 C18_1 C23_1 -0.5(7) . . . . ? C23_1 C18_1 C19_1 C20_1 1.0(6) . . . . ? C17_1 C18_1 C19_1 C20_1 -176.1(4) . . . . ? C18_1 C19_1 C20_1 C21_1 -0.3(6) . . . . ? C19_1 C20_1 C21_1 C22_1 -0.2(6) . . . . ? C20_1 C21_1 C22_1 C23_1 0.1(5) . . . . ? C21_1 C22_1 C23_1 C18_1 0.6(5) . . . . ? C21_1 C22_1 C23_1 C24_1 178.8(3) . . . . ? C19_1 C18_1 C23_1 C22_1 -1.1(5) . . . . ? C17_1 C18_1 C23_1 C22_1 176.0(4) . . . . ? C19_1 C18_1 C23_1 C24_1 -179.4(3) . . . . ? C17_1 C18_1 C23_1 C24_1 -2.3(6) . . . . ? C12_1 N11_1 C24_1 C15_1 -0.5(5) . . . . ? Ni1_1 N11_1 C24_1 C15_1 -179.5(2) . . . . ? C12_1 N11_1 C24_1 C23_1 -178.9(3) . . . . ? Ni1_1 N11_1 C24_1 C23_1 2.1(5) . . . . ? C14_1 C15_1 C24_1 N11_1 -0.6(5) . . . . ? C16_1 C15_1 C24_1 N11_1 177.3(3) . . . . ? C14_1 C15_1 C24_1 C23_1 177.8(3) . . . . ? C16_1 C15_1 C24_1 C23_1 -4.3(5) . . . . ? C22_1 C23_1 C24_1 N11_1 4.9(5) . . . . ? C18_1 C23_1 C24_1 N11_1 -177.0(3) . . . . ? C22_1 C23_1 C24_1 C15_1 -173.5(3) . . . . ? C18_1 C23_1 C24_1 C15_1 4.7(5) . . . . ? N11_1 C12_1 C25_1 N25_1 -0.4(4) . . . . ? C13_1 C12_1 C25_1 N25_1 177.1(3) . . . . ? C12_1 C25_1 N25_1 C51_1 -174.5(3) . . . . ? C12_1 C25_1 N25_1 Ni1_1 2.4(4) . . . . ? N45_1 Ni1_1 N25_1 C25_1 173.6(2) . . . . ? N11_1 Ni1_1 N25_1 C25_1 -2.4(2) . . . . ? I1_1 Ni1_1 N25_1 C25_1 -91.7(2) . . . . ? I2_1 Ni1_1 N25_1 C25_1 87.3(2) . . . . ? N45_1 Ni1_1 N25_1 C51_1 -9.23(19) . . . . ? N11_1 Ni1_1 N25_1 C51_1 174.7(2) . . . . ? I1_1 Ni1_1 N25_1 C51_1 85.49(19) . . . . ? I2_1 Ni1_1 N25_1 C51_1 -95.56(19) . . . . ? C44_1 N31_1 C32_1 C33_1 -1.6(5) . . . . ? C44_1 N31_1 C32_1 C45_1 -176.9(3) . . . . ? N31_1 C32_1 C33_1 C34_1 0.0(5) . . . . ? C45_1 C32_1 C33_1 C34_1 174.7(3) . . . . ? C32_1 C33_1 C34_1 C35_1 1.0(5) . . . . ? C33_1 C34_1 C35_1 C44_1 -0.4(5) . . . . ? C33_1 C34_1 C35_1 C36_1 178.0(4) . . . . ? C34_1 C35_1 C36_1 C37_1 -177.1(4) . . . . ? C44_1 C35_1 C36_1 C37_1 1.3(6) . . . . ? C35_1 C36_1 C37_1 C38_1 -1.0(8) . . . . ? C36_1 C37_1 C38_1 C43_1 0.1(7) . . . . ? C36_1 C37_1 C38_1 C39_1 177.7(5) . . . . ? C43_1 C38_1 C39_1 C40_1 1.1(7) . . . . ? C37_1 C38_1 C39_1 C40_1 -176.4(4) . . . . ? C38_1 C39_1 C40_1 C41_1 -0.1(7) . . . . ? C39_1 C40_1 C41_1 C42_1 -0.6(6) . . . . ? C40_1 C41_1 C42_1 C43_1 0.2(5) . . . . ? C39_1 C38_1 C43_1 C42_1 -1.5(6) . . . . ? C37_1 C38_1 C43_1 C42_1 176.1(4) . . . . ? C39_1 C38_1 C43_1 C44_1 -177.3(4) . . . . ? C37_1 C38_1 C43_1 C44_1 0.3(6) . . . . ? C41_1 C42_1 C43_1 C38_1 0.9(5) . . . . ? C41_1 C42_1 C43_1 C44_1 176.6(3) . . . . ? C32_1 N31_1 C44_1 C35_1 2.1(5) . . . . ? C32_1 N31_1 C44_1 C43_1 -176.6(3) . . . . ? C34_1 C35_1 C44_1 N31_1 -1.2(5) . . . . ? C36_1 C35_1 C44_1 N31_1 -179.6(3) . . . . ? C34_1 C35_1 C44_1 C43_1 177.6(3) . . . . ? C36_1 C35_1 C44_1 C43_1 -0.9(5) . . . . ? C38_1 C43_1 C44_1 N31_1 178.9(3) . . . . ? C42_1 C43_1 C44_1 N31_1 3.2(5) . . . . ? C38_1 C43_1 C44_1 C35_1 0.1(5) . . . . ? C42_1 C43_1 C44_1 C35_1 -175.6(3) . . . . ? N31_1 C32_1 C45_1 N45_1 -176.5(3) . . . . ? C33_1 C32_1 C45_1 N45_1 8.3(6) . . . . ? C32_1 C45_1 N45_1 C56_1 -172.0(3) . . . . ? C32_1 C45_1 N45_1 Ni1_1 6.8(5) . . . . ? N25_1 Ni1_1 N45_1 C45_1 162.3(3) . . . . ? N11_1 Ni1_1 N45_1 C45_1 175.2(3) . . . . ? I1_1 Ni1_1 N45_1 C45_1 65.5(3) . . . . ? I2_1 Ni1_1 N45_1 C45_1 -86.3(3) . . . . ? N25_1 Ni1_1 N45_1 C56_1 -18.76(17) . . . . ? N11_1 Ni1_1 N45_1 C56_1 -5.9(4) . . . . ? I1_1 Ni1_1 N45_1 C56_1 -115.63(16) . . . . ? I2_1 Ni1_1 N45_1 C56_1 92.55(16) . . . . ? C25_1 N25_1 C51_1 C52_1 -24.1(4) . . . . ? Ni1_1 N25_1 C51_1 C52_1 159.0(2) . . . . ? C25_1 N25_1 C51_1 C56_1 -148.9(3) . . . . ? Ni1_1 N25_1 C51_1 C56_1 34.2(3) . . . . ? N25_1 C51_1 C52_1 C53_1 -176.9(2) . . . . ? C56_1 C51_1 C52_1 C53_1 -56.0(3) . . . . ? C51_1 C52_1 C53_1 C54_1 56.5(3) . . . . ? C52_1 C53_1 C54_1 C55_1 -58.1(4) . . . . ? C53_1 C54_1 C55_1 C56_1 57.4(3) . . . . ? C45_1 N45_1 C56_1 C55_1 -13.7(4) . . . . ? Ni1_1 N45_1 C56_1 C55_1 167.2(2) . . . . ? C45_1 N45_1 C56_1 C51_1 -139.1(3) . . . . ? Ni1_1 N45_1 C56_1 C51_1 41.8(2) . . . . ? C54_1 C55_1 C56_1 N45_1 -179.1(2) . . . . ? C54_1 C55_1 C56_1 C51_1 -55.0(3) . . . . ? N25_1 C51_1 C56_1 N45_1 -48.8(3) . . . . ? C52_1 C51_1 C56_1 N45_1 -175.0(2) . . . . ? N25_1 C51_1 C56_1 C55_1 -177.9(2) . . . . ? C52_1 C51_1 C56_1 C55_1 55.9(3) . . . . ? N25_2 Ni2_2 N11_2 C12_2 10.4(2) . . . . ? N45_2 Ni2_2 N11_2 C12_2 -7.1(4) . . . . ? I4_2 Ni2_2 N11_2 C12_2 -99.8(2) . . . . ? I3_2 Ni2_2 N11_2 C12_2 107.8(2) . . . . ? N25_2 Ni2_2 N11_2 C24_2 -175.4(3) . . . . ? N45_2 Ni2_2 N11_2 C24_2 167.0(3) . . . . ? I4_2 Ni2_2 N11_2 C24_2 74.4(3) . . . . ? I3_2 Ni2_2 N11_2 C24_2 -78.0(3) . . . . ? C24_2 N11_2 C12_2 C13_2 -2.9(5) . . . . ? Ni2_2 N11_2 C12_2 C13_2 172.5(3) . . . . ? C24_2 N11_2 C12_2 C25_2 173.9(3) . . . . ? Ni2_2 N11_2 C12_2 C25_2 -10.8(3) . . . . ? N11_2 C12_2 C13_2 C14_2 2.8(6) . . . . ? C25_2 C12_2 C13_2 C14_2 -173.9(3) . . . . ? C12_2 C13_2 C14_2 C15_2 0.9(6) . . . . ? C13_2 C14_2 C15_2 C16_2 175.5(4) . . . . ? C13_2 C14_2 C15_2 C24_2 -4.1(6) . . . . ? C14_2 C15_2 C16_2 C17_2 -179.9(5) . . . . ? C24_2 C15_2 C16_2 C17_2 -0.3(8) . . . . ? C15_2 C16_2 C17_2 C18_2 -0.9(9) . . . . ? C16_2 C17_2 C18_2 C19_2 -178.1(5) . . . . ? C16_2 C17_2 C18_2 C23_2 -0.5(9) . . . . ? C23_2 C18_2 C19_2 C20_2 -1.3(7) . . . . ? C17_2 C18_2 C19_2 C20_2 176.3(5) . . . . ? C18_2 C19_2 C20_2 C21_2 -0.3(7) . . . . ? C19_2 C20_2 C21_2 C22_2 1.5(6) . . . . ? C20_2 C21_2 C22_2 C23_2 -1.1(6) . . . . ? C21_2 C22_2 C23_2 C18_2 -0.5(5) . . . . ? C21_2 C22_2 C23_2 C24_2 -179.5(3) . . . . ? C19_2 C18_2 C23_2 C22_2 1.7(6) . . . . ? C17_2 C18_2 C23_2 C22_2 -176.0(4) . . . . ? C19_2 C18_2 C23_2 C24_2 -179.3(4) . . . . ? C17_2 C18_2 C23_2 C24_2 3.0(6) . . . . ? C12_2 N11_2 C24_2 C15_2 -0.6(5) . . . . ? Ni2_2 N11_2 C24_2 C15_2 -174.3(2) . . . . ? C12_2 N11_2 C24_2 C23_2 -178.9(3) . . . . ? Ni2_2 N11_2 C24_2 C23_2 7.3(5) . . . . ? C14_2 C15_2 C24_2 N11_2 4.1(5) . . . . ? C16_2 C15_2 C24_2 N11_2 -175.6(4) . . . . ? C14_2 C15_2 C24_2 C23_2 -177.6(3) . . . . ? C16_2 C15_2 C24_2 C23_2 2.8(6) . . . . ? C22_2 C23_2 C24_2 N11_2 -6.8(5) . . . . ? C18_2 C23_2 C24_2 N11_2 174.3(3) . . . . ? C22_2 C23_2 C24_2 C15_2 174.8(3) . . . . ? C18_2 C23_2 C24_2 C15_2 -4.1(5) . . . . ? N11_2 C12_2 C25_2 N25_2 4.8(5) . . . . ? C13_2 C12_2 C25_2 N25_2 -178.3(3) . . . . ? C12_2 C25_2 N25_2 C51_2 -176.1(3) . . . . ? C12_2 C25_2 N25_2 Ni2_2 5.5(4) . . . . ? N45_2 Ni2_2 N25_2 C25_2 165.5(2) . . . . ? N11_2 Ni2_2 N25_2 C25_2 -8.8(2) . . . . ? I4_2 Ni2_2 N25_2 C25_2 78.0(2) . . . . ? I3_2 Ni2_2 N25_2 C25_2 -100.5(2) . . . . ? N45_2 Ni2_2 N25_2 C51_2 -13.0(2) . . . . ? N11_2 Ni2_2 N25_2 C51_2 172.7(2) . . . . ? I4_2 Ni2_2 N25_2 C51_2 -100.54(19) . . . . ? I3_2 Ni2_2 N25_2 C51_2 81.02(19) . . . . ? C44_2 N31_2 C32_2 C33_2 -0.1(5) . . . . ? C44_2 N31_2 C32_2 C45_2 -176.0(3) . . . . ? N31_2 C32_2 C33_2 C34_2 0.2(5) . . . . ? C45_2 C32_2 C33_2 C34_2 175.4(3) . . . . ? C32_2 C33_2 C34_2 C35_2 -1.0(5) . . . . ? C33_2 C34_2 C35_2 C44_2 1.7(5) . . . . ? C33_2 C34_2 C35_2 C36_2 -174.8(4) . . . . ? C34_2 C35_2 C36_2 C37_2 175.5(4) . . . . ? C44_2 C35_2 C36_2 C37_2 -1.0(6) . . . . ? C35_2 C36_2 C37_2 C38_2 2.9(8) . . . . ? C36_2 C37_2 C38_2 C39_2 -180.0(5) . . . . ? C36_2 C37_2 C38_2 C43_2 -2.7(7) . . . . ? C43_2 C38_2 C39_2 C40_2 0.2(7) . . . . ? C37_2 C38_2 C39_2 C40_2 177.5(4) . . . . ? C38_2 C39_2 C40_2 C41_2 0.0(7) . . . . ? C39_2 C40_2 C41_2 C42_2 -0.1(6) . . . . ? C40_2 C41_2 C42_2 C43_2 -0.1(5) . . . . ? C41_2 C42_2 C43_2 C38_2 0.4(5) . . . . ? C41_2 C42_2 C43_2 C44_2 -177.9(3) . . . . ? C39_2 C38_2 C43_2 C42_2 -0.4(6) . . . . ? C37_2 C38_2 C43_2 C42_2 -177.7(4) . . . . ? C39_2 C38_2 C43_2 C44_2 177.9(4) . . . . ? C37_2 C38_2 C43_2 C44_2 0.6(6) . . . . ? C32_2 N31_2 C44_2 C35_2 0.9(5) . . . . ? C32_2 N31_2 C44_2 C43_2 177.0(3) . . . . ? C34_2 C35_2 C44_2 N31_2 -1.7(5) . . . . ? C36_2 C35_2 C44_2 N31_2 174.9(3) . . . . ? C34_2 C35_2 C44_2 C43_2 -177.7(3) . . . . ? C36_2 C35_2 C44_2 C43_2 -1.0(5) . . . . ? C42_2 C43_2 C44_2 N31_2 3.3(5) . . . . ? C38_2 C43_2 C44_2 N31_2 -175.0(3) . . . . ? C42_2 C43_2 C44_2 C35_2 179.5(3) . . . . ? C38_2 C43_2 C44_2 C35_2 1.2(5) . . . . ? N31_2 C32_2 C45_2 N45_2 178.5(3) . . . . ? C33_2 C32_2 C45_2 N45_2 2.8(6) . . . . ? C32_2 C45_2 N45_2 C56_2 -174.7(3) . . . . ? C32_2 C45_2 N45_2 Ni2_2 -0.8(5) . . . . ? N25_2 Ni2_2 N45_2 C45_2 169.1(3) . . . . ? N11_2 Ni2_2 N45_2 C45_2 -173.4(3) . . . . ? I4_2 Ni2_2 N45_2 C45_2 -80.7(3) . . . . ? I3_2 Ni2_2 N45_2 C45_2 72.0(3) . . . . ? N25_2 Ni2_2 N45_2 C56_2 -16.49(18) . . . . ? N11_2 Ni2_2 N45_2 C56_2 1.0(4) . . . . ? I4_2 Ni2_2 N45_2 C56_2 93.62(17) . . . . ? I3_2 Ni2_2 N45_2 C56_2 -113.65(16) . . . . ? C25_2 N25_2 C51_2 C52_2 -15.4(4) . . . . ? Ni2_2 N25_2 C51_2 C52_2 163.0(2) . . . . ? C25_2 N25_2 C51_2 C56_2 -139.9(3) . . . . ? Ni2_2 N25_2 C51_2 C56_2 38.5(3) . . . . ? N25_2 C51_2 C52_2 C53_2 -176.7(3) . . . . ? C56_2 C51_2 C52_2 C53_2 -55.8(4) . . . . ? C51_2 C52_2 C53_2 C54_2 56.2(4) . . . . ? C52_2 C53_2 C54_2 C55_2 -56.4(4) . . . . ? C53_2 C54_2 C55_2 C56_2 54.7(3) . . . . ? C45_2 N45_2 C56_2 C55_2 -18.5(4) . . . . ? Ni2_2 N45_2 C56_2 C55_2 166.0(2) . . . . ? C45_2 N45_2 C56_2 C51_2 -143.7(3) . . . . ? Ni2_2 N45_2 C56_2 C51_2 40.8(2) . . . . ? C54_2 C55_2 C56_2 N45_2 -176.0(2) . . . . ? C54_2 C55_2 C56_2 C51_2 -52.8(3) . . . . ? N25_2 C51_2 C56_2 N45_2 -50.7(3) . . . . ? C52_2 C51_2 C56_2 N45_2 -177.4(2) . . . . ? N25_2 C51_2 C56_2 C55_2 -179.1(2) . . . . ? C52_2 C51_2 C56_2 C55_2 54.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.521 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.091 data_(R,R)-2 _database_code_depnum_ccdc_archive 'CCDC 846323' #TrackingRef '- output.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; DP-2-74-1 quinoline cyclohexane imine Ni2 I4 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 I2 N4 Ni' _chemical_formula_sum 'C32 H36 I2 N4 Ni' _chemical_formula_weight 789.16 _chemical_absolute_configuration syn 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' I I -0.4742 1.8119 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.9311(17) _cell_length_b 8.6427(9) _cell_length_c 25.050(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.466(8) _cell_angle_gamma 90.00 _cell_volume 3143.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3707 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 27.05 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 2.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.344 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_reflns_number 21125 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.1154 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.41 _reflns_number_total 12469 _reflns_number_gt 10092 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0800P)^2^+200.0000P] 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 0.05(9) _refine_ls_number_reflns 12469 _refine_ls_number_parameters 703 _refine_ls_number_restraints 486 _refine_ls_R_factor_all 0.1301 _refine_ls_R_factor_gt 0.1131 _refine_ls_wR_factor_ref 0.3052 _refine_ls_wR_factor_gt 0.2956 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.000 _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 Ni1_1 Ni 0.79046(18) 0.5577(3) 0.30401(11) 0.0182(6) Uani 1 1 d . . . I1_1 I 0.95037(9) 0.41793(19) 0.31330(6) 0.0279(3) Uani 1 1 d . . . I2_1 I 0.65782(10) 0.76643(17) 0.29533(7) 0.0278(3) Uani 1 1 d . . . N11_1 N 0.7987(12) 0.5278(18) 0.3903(6) 0.020(4) Uani 1 1 d DU . . C12_1 C 0.7463(15) 0.402(3) 0.3955(8) 0.029(5) Uani 1 1 d DU . . C13_1 C 0.735(2) 0.348(3) 0.4457(9) 0.044(7) Uani 1 1 d DU . . H13_1 H 0.6967 0.2610 0.4472 0.052 Uiso 1 1 calc R . . C14_1 C 0.7800(19) 0.419(3) 0.4925(9) 0.044(6) Uani 1 1 d DU . . H14_1 H 0.7736 0.3816 0.5270 0.052 Uiso 1 1 calc R . . C15_1 C 0.8364(16) 0.550(3) 0.4901(8) 0.031(5) Uani 1 1 d DU . . C16_1 C 0.879(2) 0.629(3) 0.5373(9) 0.048(7) Uani 1 1 d DU . . H16_1 H 0.8679 0.5995 0.5717 0.058 Uiso 1 1 calc R . . C17_1 C 0.9393(18) 0.754(3) 0.5342(9) 0.043(6) Uani 1 1 d DU . . H17_1 H 0.9761 0.8012 0.5662 0.052 Uiso 1 1 calc R . . C18_1 C 0.9410(18) 0.803(3) 0.4835(9) 0.040(6) Uani 1 1 d DU . . H18_1 H 0.9788 0.8898 0.4813 0.048 Uiso 1 1 calc R . . C19_1 C 0.8942(16) 0.740(2) 0.4342(8) 0.030(5) Uani 1 1 d DU . . C20_1 C 0.8390(17) 0.608(3) 0.4372(8) 0.039(6) Uani 1 1 d DU . . C21_1 C 0.6957(15) 0.333(3) 0.3443(8) 0.029(5) Uani 1 1 d DU . . H21_1 H 0.6543 0.2496 0.3446 0.035 Uiso 1 1 calc R . . N21_1 N 0.7083(11) 0.386(2) 0.2991(6) 0.020(4) Uani 1 1 d DU . . C22_1 C 0.9080(16) 0.813(3) 0.3811(8) 0.031(6) Uani 1 1 d DU . . H22_1 H 0.8710 0.7530 0.3495 0.037 Uiso 1 1 calc R . . C23_1 C 1.0079(19) 0.804(4) 0.3788(14) 0.059(10) Uani 1 1 d DU . . H23A_1 H 1.0279 0.6954 0.3822 0.089 Uiso 1 1 calc R . . H23B_1 H 1.0453 0.8641 0.4091 0.089 Uiso 1 1 calc R . . H23C_1 H 1.0154 0.8454 0.3438 0.089 Uiso 1 1 calc R . . C24_1 C 0.8714(19) 0.979(3) 0.3768(12) 0.042(7) Uani 1 1 d DU . . H24A_1 H 0.8068 0.9783 0.3792 0.062 Uiso 1 1 calc R . . H24B_1 H 0.8760 1.0234 0.3416 0.062 Uiso 1 1 calc R . . H24C_1 H 0.9078 1.0408 0.4069 0.062 Uiso 1 1 calc R . . N31_1 N 0.8262(14) 0.799(2) 0.1308(7) 0.031(5) Uani 1 1 d DU . . C32_1 C 0.8254(15) 0.755(2) 0.1791(7) 0.026(5) Uani 1 1 d DU . . C33_1 C 0.8617(19) 0.838(3) 0.2284(9) 0.037(6) Uani 1 1 d DU . . H33_1 H 0.8623 0.7959 0.2636 0.044 Uiso 1 1 calc R . . C34_1 C 0.8964(19) 0.984(3) 0.2217(8) 0.036(6) Uani 1 1 d DU . . H34_1 H 0.9155 1.0503 0.2525 0.043 Uiso 1 1 calc R . . C35_1 C 0.9029(19) 1.033(2) 0.1701(8) 0.034(6) Uani 1 1 d DU . . C36_1 C 0.9328(19) 1.185(3) 0.1611(10) 0.039(6) Uani 1 1 d DU . . H36_1 H 0.9618 1.2484 0.1910 0.047 Uiso 1 1 calc R . . C37_1 C 0.9190(19) 1.237(3) 0.1085(10) 0.044(7) Uani 1 1 d DU . . H37_1 H 0.9204 1.3443 0.1008 0.053 Uiso 1 1 calc R . . C38_1 C 0.9030(19) 1.128(3) 0.0669(10) 0.044(7) Uani 1 1 d DU . . H38_1 H 0.9223 1.1521 0.0343 0.053 Uiso 1 1 calc R . . C39_1 C 0.8604(19) 0.987(3) 0.0697(9) 0.041(6) Uani 1 1 d DU . . C40_1 C 0.8617(18) 0.941(2) 0.1242(8) 0.034(6) Uani 1 1 d DU . . C41_1 C 0.7830(14) 0.600(2) 0.1793(8) 0.027(5) Uani 1 1 d DU . . H41_1 H 0.7639 0.5500 0.1448 0.032 Uiso 1 1 calc R . . N41_1 N 0.7692(11) 0.527(2) 0.2208(7) 0.017(3) Uani 1 1 d DU . . C42_1 C 0.827(3) 0.883(4) 0.0218(10) 0.090(15) Uani 1 1 d DU . . H42_1 H 0.7978 0.7892 0.0339 0.108 Uiso 1 1 calc R . . C43_1 C 0.906(3) 0.832(6) -0.0075(13) 0.12(2) Uani 1 1 d DU . . H43A_1 H 0.8798 0.7641 -0.0384 0.175 Uiso 1 1 calc R . . H43B_1 H 0.9541 0.7775 0.0189 0.175 Uiso 1 1 calc R . . H43C_1 H 0.9320 0.9244 -0.0209 0.175 Uiso 1 1 calc R . . C44_1 C 0.757(3) 0.965(5) -0.0229(17) 0.089(14) Uani 1 1 d DU . . H44A_1 H 0.7032 0.9944 -0.0087 0.133 Uiso 1 1 calc R . . H44B_1 H 0.7372 0.8959 -0.0544 0.133 Uiso 1 1 calc R . . H44C_1 H 0.7847 1.0584 -0.0343 0.133 Uiso 1 1 calc R . . C51_1 C 0.6579(14) 0.337(2) 0.2441(9) 0.019(4) Uani 1 1 d U . . H51_1 H 0.6046 0.4087 0.2312 0.023 Uiso 1 1 calc R . . C52_1 C 0.7267(15) 0.362(3) 0.2082(9) 0.024(5) Uani 1 1 d U . . H52_1 H 0.7782 0.2875 0.2222 0.028 Uiso 1 1 calc R . . C53_1 C 0.6873(16) 0.317(3) 0.1492(10) 0.029(5) Uani 1 1 d U . . H53A_1 H 0.7363 0.3202 0.1286 0.035 Uiso 1 1 calc R . . H53B_1 H 0.6386 0.3913 0.1321 0.035 Uiso 1 1 calc R . . C54_1 C 0.646(2) 0.149(3) 0.1466(12) 0.043(7) Uani 1 1 d U . . H54A_1 H 0.6146 0.1253 0.1081 0.051 Uiso 1 1 calc R . . H54B_1 H 0.6966 0.0741 0.1583 0.051 Uiso 1 1 calc R . . C55_1 C 0.5787(18) 0.129(3) 0.1818(10) 0.037(6) Uani 1 1 d U . . H55A_1 H 0.5592 0.0193 0.1811 0.044 Uiso 1 1 calc R . . H55B_1 H 0.5234 0.1931 0.1675 0.044 Uiso 1 1 calc R . . C56_1 C 0.6233(19) 0.177(3) 0.2401(11) 0.035(6) Uani 1 1 d U . . H56A_1 H 0.5778 0.1658 0.2629 0.042 Uiso 1 1 calc R . . H56B_1 H 0.6752 0.1057 0.2550 0.042 Uiso 1 1 calc R . . Ni2_2 Ni 0.2846(2) 0.3001(3) 0.30960(12) 0.0234(6) Uani 1 1 d . . . I3_2 I 0.15367(10) 0.10112(17) 0.31183(7) 0.0277(3) Uani 1 1 d . . . I4_2 I 0.44521(10) 0.4201(2) 0.30531(7) 0.0317(4) Uani 1 1 d . . . N11_2 N 0.3008(12) 0.336(2) 0.3974(6) 0.025(4) Uani 1 1 d DU . . C12_2 C 0.2505(15) 0.463(2) 0.4015(7) 0.026(5) Uani 1 1 d DU . . C13_2 C 0.2341(17) 0.515(3) 0.4510(8) 0.032(6) Uani 1 1 d DU . . H13_2 H 0.1946 0.6008 0.4516 0.039 Uiso 1 1 calc R . . C14_2 C 0.2748(18) 0.442(3) 0.4985(9) 0.038(6) Uani 1 1 d DU . . H14_2 H 0.2670 0.4807 0.5326 0.046 Uiso 1 1 calc R . . C15_2 C 0.329(2) 0.308(3) 0.4971(9) 0.043(7) Uani 1 1 d DU . . C16_2 C 0.3733(18) 0.231(3) 0.5443(9) 0.041(6) Uani 1 1 d DU . . H16_2 H 0.3637 0.2634 0.5788 0.049 Uiso 1 1 calc R . . C17_2 C 0.4332(18) 0.105(3) 0.5418(9) 0.044(6) Uani 1 1 d DU . . H17_2 H 0.4709 0.0597 0.5739 0.053 Uiso 1 1 calc R . . C18_2 C 0.433(2) 0.054(3) 0.4913(9) 0.049(8) Uani 1 1 d DU . . H18_2 H 0.4630 -0.0426 0.4893 0.059 Uiso 1 1 calc R . . C19_2 C 0.3945(15) 0.123(2) 0.4418(8) 0.029(5) Uani 1 1 d DU . . C20_2 C 0.3430(14) 0.259(2) 0.4450(7) 0.022(4) Uani 1 1 d DU . . C21_2 C 0.2150(15) 0.551(2) 0.3513(8) 0.027(5) Uani 1 1 d DU . . H21_2 H 0.1836 0.6464 0.3523 0.032 Uiso 1 1 calc R . . N21_2 N 0.2267(11) 0.498(2) 0.3063(6) 0.019(4) Uani 1 1 d DU . . C22_2 C 0.4114(15) 0.051(3) 0.3891(9) 0.033(6) Uani 1 1 d DU . . H22_2 H 0.3742 0.1109 0.3573 0.040 Uiso 1 1 calc R . . C23_2 C 0.378(2) -0.114(3) 0.3834(13) 0.052(8) Uani 1 1 d DU . . H23A_2 H 0.3128 -0.1180 0.3832 0.078 Uiso 1 1 calc R . . H23B_2 H 0.4134 -0.1753 0.4143 0.078 Uiso 1 1 calc R . . H23C_2 H 0.3879 -0.1574 0.3489 0.078 Uiso 1 1 calc R . . C24_2 C 0.5125(16) 0.066(4) 0.3876(12) 0.045(8) Uani 1 1 d DU . . H24A_2 H 0.5220 0.0216 0.3534 0.068 Uiso 1 1 calc R . . H24B_2 H 0.5507 0.0115 0.4190 0.068 Uiso 1 1 calc R . . H24C_2 H 0.5298 0.1761 0.3894 0.068 Uiso 1 1 calc R . . N31_2 N 0.3209(16) 0.064(2) 0.1365(7) 0.037(5) Uani 1 1 d DU . . C32_2 C 0.3121(15) 0.101(2) 0.1844(7) 0.026(5) Uani 1 1 d DU . . C33_2 C 0.3458(17) 0.010(2) 0.2324(8) 0.031(5) Uani 1 1 d DU . . H33A_2 H 0.3367 0.0406 0.2673 0.037 Uiso 1 1 calc R . . C34_2 C 0.3928(15) -0.125(2) 0.2257(8) 0.026(5) Uani 1 1 d DU . . H34_2 H 0.4213 -0.1851 0.2568 0.031 Uiso 1 1 calc R . . C35_2 C 0.3979(17) -0.171(2) 0.1738(8) 0.030(5) Uani 1 1 d DU . . C36_2 C 0.448(2) -0.305(3) 0.1660(10) 0.042(7) Uani 1 1 d DU . . H36_2 H 0.4785 -0.3654 0.1965 0.051 Uiso 1 1 calc R . . C37_2 C 0.451(2) -0.346(3) 0.1144(11) 0.052(8) Uani 1 1 d DU . . H37_2 H 0.4818 -0.4371 0.1072 0.062 Uiso 1 1 calc R . . C38_2 C 0.4084(16) -0.248(3) 0.0725(9) 0.036(6) Uani 1 1 d DU . . H38_2 H 0.3962 -0.2891 0.0364 0.044 Uiso 1 1 calc R . . C39_2 C 0.381(2) -0.095(3) 0.0772(10) 0.052(7) Uani 1 1 d DU . . C40_2 C 0.3646(17) -0.070(2) 0.1299(8) 0.034(5) Uani 1 1 d DU . . C41_2 C 0.2524(15) 0.238(2) 0.1835(8) 0.026(5) Uani 1 1 d DU . . H41_2 H 0.2205 0.2731 0.1483 0.031 Uiso 1 1 calc R . . N41_2 N 0.2387(13) 0.314(2) 0.2244(8) 0.026(4) Uani 1 1 d DU . . C42_2 C 0.344(3) 0.010(4) 0.0305(11) 0.074(13) Uani 1 1 d DU . . H42_2 H 0.3308 0.1129 0.0453 0.088 Uiso 1 1 calc R . . C43_2 C 0.411(3) 0.033(6) -0.0091(16) 0.104(17) Uani 1 1 d DU . . H43A_2 H 0.4696 0.0761 0.0118 0.155 Uiso 1 1 calc R . . H43B_2 H 0.3832 0.1045 -0.0387 0.155 Uiso 1 1 calc R . . H43C_2 H 0.4224 -0.0668 -0.0248 0.155 Uiso 1 1 calc R . . C44_2 C 0.255(3) -0.052(5) -0.0058(16) 0.12(2) Uani 1 1 d DU . . H44A_2 H 0.2322 0.0204 -0.0359 0.182 Uiso 1 1 calc R . . H44B_2 H 0.2088 -0.0643 0.0160 0.182 Uiso 1 1 calc R . . H44C_2 H 0.2670 -0.1528 -0.0208 0.182 Uiso 1 1 calc R . . C51_2 C 0.1989(18) 0.569(3) 0.2536(10) 0.032(5) Uani 1 1 d U . . H51_2 H 0.2558 0.6160 0.2457 0.038 Uiso 1 1 calc R . . C52_2 C 0.1702(16) 0.441(3) 0.2123(9) 0.027(5) Uani 1 1 d U . . H52_2 H 0.1110 0.3989 0.2184 0.033 Uiso 1 1 calc R . . C53_2 C 0.149(2) 0.503(4) 0.1527(12) 0.045(7) Uani 1 1 d U . . H53A_2 H 0.1264 0.4173 0.1269 0.054 Uiso 1 1 calc R . . H53B_2 H 0.2067 0.5433 0.1444 0.054 Uiso 1 1 calc R . . C54_2 C 0.076(2) 0.634(4) 0.1449(12) 0.046(7) Uani 1 1 d U . . H54A_2 H 0.0683 0.6803 0.1080 0.055 Uiso 1 1 calc R . . H54B_2 H 0.0160 0.5902 0.1478 0.055 Uiso 1 1 calc R . . C55_2 C 0.107(2) 0.760(4) 0.1894(12) 0.044(6) Uani 1 1 d U . . H55A_2 H 0.1614 0.8135 0.1825 0.053 Uiso 1 1 calc R . . H55B_2 H 0.0567 0.8374 0.1858 0.053 Uiso 1 1 calc R . . C56_2 C 0.130(2) 0.698(3) 0.2477(12) 0.040(6) Uani 1 1 d U . . H56A_2 H 0.1546 0.7825 0.2735 0.047 Uiso 1 1 calc R . . H56B_2 H 0.0728 0.6590 0.2571 0.047 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_1 0.0107(12) 0.0135(13) 0.0298(14) 0.0052(11) 0.0036(10) -0.0024(10) I1_1 0.0150(6) 0.0258(8) 0.0421(8) 0.0020(7) 0.0053(5) 0.0052(6) I2_1 0.0215(7) 0.0160(7) 0.0464(9) 0.0045(7) 0.0086(6) 0.0026(6) N11_1 0.017(6) 0.017(6) 0.027(6) 0.001(5) 0.004(5) 0.005(5) C12_1 0.031(7) 0.025(7) 0.032(7) 0.007(6) 0.008(6) 0.010(6) C13_1 0.045(9) 0.042(9) 0.045(9) 0.009(7) 0.015(7) -0.002(7) C14_1 0.045(9) 0.047(9) 0.040(8) 0.007(7) 0.012(7) 0.007(7) C15_1 0.033(8) 0.028(8) 0.031(8) 0.005(6) 0.006(6) 0.009(6) C16_1 0.049(9) 0.053(10) 0.043(9) 0.000(7) 0.011(7) 0.015(7) C17_1 0.037(9) 0.049(9) 0.043(9) -0.003(7) 0.006(7) 0.009(7) C18_1 0.037(8) 0.039(9) 0.042(9) -0.001(7) 0.005(7) 0.004(7) C19_1 0.030(8) 0.027(8) 0.029(7) 0.002(6) 0.002(6) 0.002(6) C20_1 0.041(8) 0.036(8) 0.040(8) -0.002(7) 0.011(6) 0.009(7) C21_1 0.024(7) 0.029(8) 0.036(8) 0.010(6) 0.010(6) -0.002(6) N21_1 0.012(6) 0.019(7) 0.031(7) 0.006(5) 0.013(5) 0.010(5) C22_1 0.030(12) 0.038(15) 0.024(11) -0.013(10) 0.004(9) -0.007(11) C23_1 0.043(17) 0.06(2) 0.09(2) -0.041(19) 0.036(17) -0.023(16) C24_1 0.036(15) 0.023(13) 0.063(18) -0.014(13) 0.007(13) -0.009(12) N31_1 0.035(7) 0.027(7) 0.035(7) -0.002(6) 0.015(6) -0.005(6) C32_1 0.028(7) 0.020(7) 0.028(7) 0.001(6) 0.003(6) -0.003(6) C33_1 0.038(9) 0.038(9) 0.035(8) 0.002(7) 0.010(7) -0.010(7) C34_1 0.039(9) 0.033(8) 0.034(8) -0.001(6) 0.006(6) -0.004(7) C35_1 0.036(8) 0.031(8) 0.036(8) 0.001(6) 0.009(6) -0.004(7) C36_1 0.039(9) 0.036(9) 0.043(9) 0.001(7) 0.010(7) -0.003(7) C37_1 0.040(9) 0.047(10) 0.050(9) 0.002(7) 0.021(7) -0.009(7) C38_1 0.039(9) 0.052(10) 0.047(9) 0.010(7) 0.021(7) -0.010(7) C39_1 0.040(9) 0.038(9) 0.046(9) -0.002(7) 0.014(7) 0.002(7) C40_1 0.037(8) 0.033(9) 0.034(8) 0.003(6) 0.010(6) -0.007(6) C41_1 0.023(7) 0.028(8) 0.026(7) -0.001(6) -0.002(6) 0.002(6) N41_1 0.008(6) 0.019(6) 0.022(6) 0.009(5) -0.001(5) 0.003(5) C42_1 0.20(4) 0.05(2) 0.031(16) 0.007(14) 0.04(2) -0.04(3) C43_1 0.22(6) 0.10(4) 0.026(18) -0.012(19) 0.02(3) 0.04(4) C44_1 0.06(2) 0.10(3) 0.11(3) -0.03(3) 0.04(2) -0.04(2) C51_1 0.014(6) 0.018(7) 0.025(7) 0.001(6) 0.003(5) 0.000(6) C52_1 0.020(7) 0.023(7) 0.025(7) -0.003(6) -0.002(6) 0.001(6) C53_1 0.024(7) 0.030(8) 0.034(8) 0.001(6) 0.011(6) 0.002(6) C54_1 0.045(9) 0.036(9) 0.046(9) -0.006(7) 0.006(7) -0.003(7) C55_1 0.034(8) 0.035(9) 0.039(8) -0.002(7) 0.003(6) -0.010(7) C56_1 0.030(8) 0.035(9) 0.039(8) 0.005(7) 0.008(6) -0.004(7) Ni2_2 0.0222(14) 0.0138(15) 0.0361(16) -0.0022(11) 0.0108(12) -0.0011(11) I3_2 0.0243(7) 0.0176(7) 0.0440(8) -0.0093(6) 0.0140(6) -0.0059(6) I4_2 0.0178(7) 0.0276(8) 0.0508(9) 0.0034(8) 0.0100(6) -0.0034(7) N11_2 0.021(7) 0.028(7) 0.025(7) -0.003(6) 0.006(5) -0.006(6) C12_2 0.025(7) 0.027(8) 0.029(7) -0.006(6) 0.010(6) -0.008(6) C13_2 0.032(8) 0.032(8) 0.034(8) -0.007(6) 0.007(6) -0.003(6) C14_2 0.040(8) 0.039(9) 0.036(8) -0.003(7) 0.012(6) -0.007(7) C15_2 0.048(9) 0.040(9) 0.043(9) -0.002(7) 0.013(7) -0.010(7) C16_2 0.043(9) 0.044(9) 0.036(8) -0.002(7) 0.010(7) -0.013(7) C17_2 0.039(9) 0.048(9) 0.043(9) 0.003(7) 0.007(7) -0.009(7) C18_2 0.046(10) 0.047(10) 0.052(10) 0.006(7) 0.006(7) -0.003(7) C19_2 0.029(7) 0.028(8) 0.029(7) 0.002(6) 0.007(6) -0.006(6) C20_2 0.020(7) 0.020(7) 0.028(7) 0.002(6) 0.010(6) 0.001(6) C21_2 0.027(7) 0.025(8) 0.030(7) -0.004(6) 0.011(6) 0.000(6) N21_2 0.011(6) 0.018(6) 0.027(6) -0.008(5) 0.000(5) -0.008(5) C22_2 0.020(11) 0.027(13) 0.060(15) 0.018(11) 0.024(11) 0.000(10) C23_2 0.058(19) 0.039(18) 0.07(2) 0.009(15) 0.037(16) 0.027(16) C24_2 0.030(13) 0.047(18) 0.062(17) 0.032(15) 0.019(12) 0.011(13) N31_2 0.039(8) 0.037(8) 0.038(7) -0.001(6) 0.013(6) 0.007(6) C32_2 0.023(7) 0.026(8) 0.032(7) -0.002(6) 0.011(6) 0.002(6) C33_2 0.031(8) 0.030(8) 0.031(8) -0.001(6) 0.007(6) 0.004(6) C34_2 0.021(7) 0.028(8) 0.030(7) 0.005(6) 0.008(6) 0.001(6) C35_2 0.029(8) 0.030(8) 0.030(8) -0.004(6) 0.006(6) 0.003(6) C36_2 0.043(9) 0.040(9) 0.043(9) 0.000(7) 0.006(7) 0.009(7) C37_2 0.055(10) 0.049(10) 0.053(10) -0.003(7) 0.015(7) 0.008(7) C38_2 0.018(7) 0.044(9) 0.044(8) -0.007(7) 0.001(6) -0.006(7) C39_2 0.053(10) 0.052(10) 0.053(9) 0.004(7) 0.014(7) 0.011(7) C40_2 0.037(8) 0.031(8) 0.032(8) -0.003(7) 0.007(6) 0.001(7) C41_2 0.024(7) 0.023(8) 0.027(7) -0.002(6) 0.000(6) 0.001(6) N41_2 0.021(7) 0.023(7) 0.036(7) 0.001(6) 0.012(6) -0.004(6) C42_2 0.15(4) 0.05(2) 0.030(15) 0.002(14) 0.034(19) 0.05(2) C43_2 0.12(4) 0.11(4) 0.09(3) -0.02(3) 0.04(3) -0.05(3) C44_2 0.24(6) 0.07(3) 0.08(3) 0.04(2) 0.08(3) 0.07(3) C51_2 0.032(8) 0.030(8) 0.035(8) -0.003(6) 0.007(6) 0.004(6) C52_2 0.026(7) 0.025(8) 0.029(7) -0.005(6) 0.001(6) 0.004(6) C53_2 0.043(9) 0.043(9) 0.047(9) 0.001(7) 0.008(7) 0.004(7) C54_2 0.044(9) 0.042(9) 0.048(9) 0.000(7) 0.005(7) 0.008(7) C55_2 0.045(9) 0.035(9) 0.050(9) -0.001(7) 0.005(7) 0.002(7) C56_2 0.043(9) 0.034(9) 0.044(9) 0.005(7) 0.014(7) 0.002(7) _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_1 N21_1 1.910(18) . ? Ni1_1 N41_1 2.050(17) . ? Ni1_1 N11_1 2.151(16) . ? Ni1_1 I1_1 2.637(3) . ? Ni1_1 I2_1 2.650(3) . ? N11_1 C12_1 1.36(2) . ? N11_1 C20_1 1.38(2) . ? C12_1 C13_1 1.39(2) . ? C12_1 C21_1 1.46(2) . ? C13_1 C14_1 1.36(3) . ? C13_1 H13_1 0.9500 . ? C14_1 C15_1 1.42(3) . ? C14_1 H14_1 0.9500 . ? C15_1 C16_1 1.39(3) . ? C15_1 C20_1 1.43(2) . ? C16_1 C17_1 1.42(3) . ? C16_1 H16_1 0.9500 . ? C17_1 C18_1 1.34(3) . ? C17_1 H17_1 0.9500 . ? C18_1 C19_1 1.38(2) . ? C18_1 H18_1 0.9500 . ? C19_1 C20_1 1.42(2) . ? C19_1 C22_1 1.53(2) . ? C21_1 N21_1 1.28(2) . ? C21_1 H21_1 0.9500 . ? N21_1 C51_1 1.47(3) . ? C22_1 C23_1 1.51(3) . ? C22_1 C24_1 1.53(3) . ? C22_1 H22_1 1.0000 . ? C23_1 H23A_1 0.9800 . ? C23_1 H23B_1 0.9800 . ? C23_1 H23C_1 0.9800 . ? C24_1 H24A_1 0.9800 . ? C24_1 H24B_1 0.9800 . ? C24_1 H24C_1 0.9800 . ? N31_1 C32_1 1.27(2) . ? N31_1 C40_1 1.36(2) . ? C32_1 C33_1 1.42(2) . ? C32_1 C41_1 1.48(2) . ? C33_1 C34_1 1.39(2) . ? C33_1 H33_1 0.9500 . ? C34_1 C35_1 1.38(2) . ? C34_1 H34_1 0.9500 . ? C35_1 C40_1 1.41(2) . ? C35_1 C36_1 1.42(2) . ? C36_1 C37_1 1.36(3) . ? C36_1 H36_1 0.9500 . ? C37_1 C38_1 1.38(3) . ? C37_1 H37_1 0.9500 . ? C38_1 C39_1 1.39(3) . ? C38_1 H38_1 0.9500 . ? C39_1 C40_1 1.42(3) . ? C39_1 C42_1 1.49(3) . ? C41_1 N41_1 1.27(2) . ? C41_1 H41_1 0.9500 . ? N41_1 C52_1 1.57(3) . ? C42_1 C44_1 1.52(5) . ? C42_1 C43_1 1.59(4) . ? C42_1 H42_1 1.0000 . ? C43_1 H43A_1 0.9800 . ? C43_1 H43B_1 0.9800 . ? C43_1 H43C_1 0.9800 . ? C44_1 H44A_1 0.9800 . ? C44_1 H44B_1 0.9800 . ? C44_1 H44C_1 0.9800 . ? C51_1 C56_1 1.48(3) . ? C51_1 C52_1 1.53(3) . ? C51_1 H51_1 1.0000 . ? C52_1 C53_1 1.51(3) . ? C52_1 H52_1 1.0000 . ? C53_1 C54_1 1.57(4) . ? C53_1 H53A_1 0.9900 . ? C53_1 H53B_1 0.9900 . ? C54_1 C55_1 1.49(4) . ? C54_1 H54A_1 0.9900 . ? C54_1 H54B_1 0.9900 . ? C55_1 C56_1 1.51(4) . ? C55_1 H55A_1 0.9900 . ? C55_1 H55B_1 0.9900 . ? C56_1 H56A_1 0.9900 . ? C56_1 H56B_1 0.9900 . ? Ni2_2 N21_2 1.907(18) . ? Ni2_2 N41_2 2.087(19) . ? Ni2_2 N11_2 2.178(16) . ? Ni2_2 I3_2 2.614(3) . ? Ni2_2 I4_2 2.638(3) . ? N11_2 C12_2 1.35(2) . ? N11_2 C20_2 1.38(2) . ? C12_2 C13_2 1.39(2) . ? C12_2 C21_2 1.46(2) . ? C13_2 C14_2 1.36(3) . ? C13_2 H13_2 0.9500 . ? C14_2 C15_2 1.42(3) . ? C14_2 H14_2 0.9500 . ? C15_2 C16_2 1.38(3) . ? C15_2 C20_2 1.43(2) . ? C16_2 C17_2 1.42(3) . ? C16_2 H16_2 0.9500 . ? C17_2 C18_2 1.34(3) . ? C17_2 H17_2 0.9500 . ? C18_2 C19_2 1.38(3) . ? C18_2 H18_2 0.9500 . ? C19_2 C20_2 1.42(2) . ? C19_2 C22_2 1.53(2) . ? C21_2 N21_2 1.27(2) . ? C21_2 H21_2 0.9500 . ? N21_2 C51_2 1.43(3) . ? C22_2 C23_2 1.51(3) . ? C22_2 C24_2 1.53(3) . ? C22_2 H22_2 1.0000 . ? C23_2 H23A_2 0.9800 . ? C23_2 H23B_2 0.9800 . ? C23_2 H23C_2 0.9800 . ? C24_2 H24A_2 0.9800 . ? C24_2 H24B_2 0.9800 . ? C24_2 H24C_2 0.9800 . ? N31_2 C32_2 1.28(2) . ? N31_2 C40_2 1.36(2) . ? C32_2 C33_2 1.42(2) . ? C32_2 C41_2 1.48(2) . ? C33_2 C34_2 1.39(2) . ? C33_2 H33A_2 0.9500 . ? C34_2 C35_2 1.38(2) . ? C34_2 H34_2 0.9500 . ? C35_2 C40_2 1.41(2) . ? C35_2 C36_2 1.41(2) . ? C36_2 C37_2 1.35(3) . ? C36_2 H36_2 0.9500 . ? C37_2 C38_2 1.38(3) . ? C37_2 H37_2 0.9500 . ? C38_2 C39_2 1.39(3) . ? C38_2 H38_2 0.9500 . ? C39_2 C40_2 1.42(3) . ? C39_2 C42_2 1.49(3) . ? C41_2 N41_2 1.27(2) . ? C41_2 H41_2 0.9500 . ? N41_2 C52_2 1.49(3) . ? C42_2 C44_2 1.52(5) . ? C42_2 C43_2 1.58(4) . ? C42_2 H42_2 1.0000 . ? C43_2 H43A_2 0.9800 . ? C43_2 H43B_2 0.9800 . ? C43_2 H43C_2 0.9800 . ? C44_2 H44A_2 0.9800 . ? C44_2 H44B_2 0.9800 . ? C44_2 H44C_2 0.9800 . ? C51_2 C56_2 1.50(4) . ? C51_2 C52_2 1.51(3) . ? C51_2 H51_2 1.0000 . ? C52_2 C53_2 1.55(4) . ? C52_2 H52_2 1.0000 . ? C53_2 C54_2 1.56(4) . ? C53_2 H53A_2 0.9900 . ? C53_2 H53B_2 0.9900 . ? C54_2 C55_2 1.55(4) . ? C54_2 H54A_2 0.9900 . ? C54_2 H54B_2 0.9900 . ? C55_2 C56_2 1.52(4) . ? C55_2 H55A_2 0.9900 . ? C55_2 H55B_2 0.9900 . ? C56_2 H56A_2 0.9900 . ? C56_2 H56B_2 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 N21_1 Ni1_1 N41_1 83.7(6) . . ? N21_1 Ni1_1 N11_1 81.8(6) . . ? N41_1 Ni1_1 N11_1 164.7(6) . . ? N21_1 Ni1_1 I1_1 101.8(5) . . ? N41_1 Ni1_1 I1_1 87.3(5) . . ? N11_1 Ni1_1 I1_1 91.0(5) . . ? N21_1 Ni1_1 I2_1 93.8(5) . . ? N41_1 Ni1_1 I2_1 93.9(5) . . ? N11_1 Ni1_1 I2_1 91.8(5) . . ? I1_1 Ni1_1 I2_1 164.35(12) . . ? C12_1 N11_1 C20_1 117.8(16) . . ? C12_1 N11_1 Ni1_1 107.0(11) . . ? C20_1 N11_1 Ni1_1 135.1(12) . . ? N11_1 C12_1 C13_1 123.4(18) . . ? N11_1 C12_1 C21_1 115.8(16) . . ? C13_1 C12_1 C21_1 120.6(18) . . ? C14_1 C13_1 C12_1 119(2) . . ? C14_1 C13_1 H13_1 120.4 . . ? C12_1 C13_1 H13_1 120.4 . . ? C13_1 C14_1 C15_1 120.4(19) . . ? C13_1 C14_1 H14_1 119.8 . . ? C15_1 C14_1 H14_1 119.8 . . ? C16_1 C15_1 C14_1 121.1(19) . . ? C16_1 C15_1 C20_1 120.8(19) . . ? C14_1 C15_1 C20_1 117.7(18) . . ? C15_1 C16_1 C17_1 120(2) . . ? C15_1 C16_1 H16_1 120.0 . . ? C17_1 C16_1 H16_1 120.0 . . ? C18_1 C17_1 C16_1 116(2) . . ? C18_1 C17_1 H17_1 121.9 . . ? C16_1 C17_1 H17_1 121.9 . . ? C17_1 C18_1 C19_1 127(2) . . ? C17_1 C18_1 H18_1 116.3 . . ? C19_1 C18_1 H18_1 116.3 . . ? C18_1 C19_1 C20_1 116.6(17) . . ? C18_1 C19_1 C22_1 118.1(17) . . ? C20_1 C19_1 C22_1 125.3(16) . . ? N11_1 C20_1 C19_1 120.2(17) . . ? N11_1 C20_1 C15_1 121.0(17) . . ? C19_1 C20_1 C15_1 118.3(17) . . ? N21_1 C21_1 C12_1 118.6(17) . . ? N21_1 C21_1 H21_1 120.7 . . ? C12_1 C21_1 H21_1 120.7 . . ? C21_1 N21_1 C51_1 125.4(17) . . ? C21_1 N21_1 Ni1_1 116.6(14) . . ? C51_1 N21_1 Ni1_1 117.6(12) . . ? C23_1 C22_1 C24_1 113.0(19) . . ? C23_1 C22_1 C19_1 110(2) . . ? C24_1 C22_1 C19_1 109.3(19) . . ? C23_1 C22_1 H22_1 108.1 . . ? C24_1 C22_1 H22_1 108.1 . . ? C19_1 C22_1 H22_1 108.1 . . ? C22_1 C23_1 H23A_1 109.5 . . ? C22_1 C23_1 H23B_1 109.5 . . ? H23A_1 C23_1 H23B_1 109.5 . . ? C22_1 C23_1 H23C_1 109.5 . . ? H23A_1 C23_1 H23C_1 109.5 . . ? H23B_1 C23_1 H23C_1 109.5 . . ? C22_1 C24_1 H24A_1 109.5 . . ? C22_1 C24_1 H24B_1 109.5 . . ? H24A_1 C24_1 H24B_1 109.5 . . ? C22_1 C24_1 H24C_1 109.5 . . ? H24A_1 C24_1 H24C_1 109.5 . . ? H24B_1 C24_1 H24C_1 109.5 . . ? C32_1 N31_1 C40_1 118.4(17) . . ? N31_1 C32_1 C33_1 126.0(17) . . ? N31_1 C32_1 C41_1 112.0(16) . . ? C33_1 C32_1 C41_1 122.0(16) . . ? C34_1 C33_1 C32_1 115.5(18) . . ? C34_1 C33_1 H33_1 122.3 . . ? C32_1 C33_1 H33_1 122.3 . . ? C35_1 C34_1 C33_1 120.1(19) . . ? C35_1 C34_1 H34_1 120.0 . . ? C33_1 C34_1 H34_1 120.0 . . ? C34_1 C35_1 C40_1 118.3(17) . . ? C34_1 C35_1 C36_1 121.7(19) . . ? C40_1 C35_1 C36_1 118.8(18) . . ? C37_1 C36_1 C35_1 119(2) . . ? C37_1 C36_1 H36_1 120.7 . . ? C35_1 C36_1 H36_1 120.7 . . ? C36_1 C37_1 C38_1 118(2) . . ? C36_1 C37_1 H37_1 121.1 . . ? C38_1 C37_1 H37_1 121.1 . . ? C37_1 C38_1 C39_1 124(2) . . ? C37_1 C38_1 H38_1 117.9 . . ? C39_1 C38_1 H38_1 117.9 . . ? C38_1 C39_1 C40_1 112.9(19) . . ? C38_1 C39_1 C42_1 124(2) . . ? C40_1 C39_1 C42_1 123(2) . . ? N31_1 C40_1 C35_1 121.1(17) . . ? N31_1 C40_1 C39_1 116.5(17) . . ? C35_1 C40_1 C39_1 122.3(18) . . ? N41_1 C41_1 C32_1 127.0(18) . . ? N41_1 C41_1 H41_1 116.5 . . ? C32_1 C41_1 H41_1 116.5 . . ? C41_1 N41_1 C52_1 115.0(17) . . ? C41_1 N41_1 Ni1_1 138.6(15) . . ? C52_1 N41_1 Ni1_1 106.5(11) . . ? C39_1 C42_1 C44_1 111(3) . . ? C39_1 C42_1 C43_1 113(3) . . ? C44_1 C42_1 C43_1 104(2) . . ? C39_1 C42_1 H42_1 109.4 . . ? C44_1 C42_1 H42_1 109.4 . . ? C43_1 C42_1 H42_1 109.4 . . ? C42_1 C43_1 H43A_1 109.5 . . ? C42_1 C43_1 H43B_1 109.5 . . ? H43A_1 C43_1 H43B_1 109.5 . . ? C42_1 C43_1 H43C_1 109.5 . . ? H43A_1 C43_1 H43C_1 109.5 . . ? H43B_1 C43_1 H43C_1 109.5 . . ? C42_1 C44_1 H44A_1 109.5 . . ? C42_1 C44_1 H44B_1 109.5 . . ? H44A_1 C44_1 H44B_1 109.5 . . ? C42_1 C44_1 H44C_1 109.5 . . ? H44A_1 C44_1 H44C_1 109.5 . . ? H44B_1 C44_1 H44C_1 109.5 . . ? N21_1 C51_1 C56_1 115.4(19) . . ? N21_1 C51_1 C52_1 104.2(16) . . ? C56_1 C51_1 C52_1 111(2) . . ? N21_1 C51_1 H51_1 108.6 . . ? C56_1 C51_1 H51_1 108.6 . . ? C52_1 C51_1 H51_1 108.6 . . ? C53_1 C52_1 C51_1 112.3(18) . . ? C53_1 C52_1 N41_1 118.7(18) . . ? C51_1 C52_1 N41_1 107.7(17) . . ? C53_1 C52_1 H52_1 105.8 . . ? C51_1 C52_1 H52_1 105.8 . . ? N41_1 C52_1 H52_1 105.8 . . ? C52_1 C53_1 C54_1 110(2) . . ? C52_1 C53_1 H53A_1 109.7 . . ? C54_1 C53_1 H53A_1 109.7 . . ? C52_1 C53_1 H53B_1 109.7 . . ? C54_1 C53_1 H53B_1 109.7 . . ? H53A_1 C53_1 H53B_1 108.2 . . ? C55_1 C54_1 C53_1 113(2) . . ? C55_1 C54_1 H54A_1 108.9 . . ? C53_1 C54_1 H54A_1 108.9 . . ? C55_1 C54_1 H54B_1 108.9 . . ? C53_1 C54_1 H54B_1 108.9 . . ? H54A_1 C54_1 H54B_1 107.7 . . ? C54_1 C55_1 C56_1 109(2) . . ? C54_1 C55_1 H55A_1 109.8 . . ? C56_1 C55_1 H55A_1 109.8 . . ? C54_1 C55_1 H55B_1 109.8 . . ? C56_1 C55_1 H55B_1 109.8 . . ? H55A_1 C55_1 H55B_1 108.2 . . ? C51_1 C56_1 C55_1 113(2) . . ? C51_1 C56_1 H56A_1 109.0 . . ? C55_1 C56_1 H56A_1 109.0 . . ? C51_1 C56_1 H56B_1 109.0 . . ? C55_1 C56_1 H56B_1 109.0 . . ? H56A_1 C56_1 H56B_1 107.8 . . ? N21_2 Ni2_2 N41_2 82.3(7) . . ? N21_2 Ni2_2 N11_2 82.0(6) . . ? N41_2 Ni2_2 N11_2 163.2(7) . . ? N21_2 Ni2_2 I3_2 104.9(5) . . ? N41_2 Ni2_2 I3_2 89.5(5) . . ? N11_2 Ni2_2 I3_2 88.8(5) . . ? N21_2 Ni2_2 I4_2 93.0(5) . . ? N41_2 Ni2_2 I4_2 91.2(5) . . ? N11_2 Ni2_2 I4_2 95.6(5) . . ? I3_2 Ni2_2 I4_2 161.97(13) . . ? C12_2 N11_2 C20_2 118.4(15) . . ? C12_2 N11_2 Ni2_2 105.0(11) . . ? C20_2 N11_2 Ni2_2 136.5(12) . . ? N11_2 C12_2 C13_2 122.9(17) . . ? N11_2 C12_2 C21_2 117.2(16) . . ? C13_2 C12_2 C21_2 119.9(17) . . ? C14_2 C13_2 C12_2 119.7(19) . . ? C14_2 C13_2 H13_2 120.1 . . ? C12_2 C13_2 H13_2 120.1 . . ? C13_2 C14_2 C15_2 120.0(19) . . ? C13_2 C14_2 H14_2 120.0 . . ? C15_2 C14_2 H14_2 120.0 . . ? C16_2 C15_2 C14_2 122.4(19) . . ? C16_2 C15_2 C20_2 119.7(19) . . ? C14_2 C15_2 C20_2 117.8(18) . . ? C15_2 C16_2 C17_2 121(2) . . ? C15_2 C16_2 H16_2 119.6 . . ? C17_2 C16_2 H16_2 119.6 . . ? C18_2 C17_2 C16_2 116(2) . . ? C18_2 C17_2 H17_2 122.2 . . ? C16_2 C17_2 H17_2 122.2 . . ? C17_2 C18_2 C19_2 128(2) . . ? C17_2 C18_2 H18_2 116.1 . . ? C19_2 C18_2 H18_2 116.1 . . ? C18_2 C19_2 C20_2 115.5(17) . . ? C18_2 C19_2 C22_2 118.6(18) . . ? C20_2 C19_2 C22_2 125.9(16) . . ? N11_2 C20_2 C19_2 119.5(16) . . ? N11_2 C20_2 C15_2 120.8(16) . . ? C19_2 C20_2 C15_2 119.5(16) . . ? N21_2 C21_2 C12_2 118.7(17) . . ? N21_2 C21_2 H21_2 120.7 . . ? C12_2 C21_2 H21_2 120.7 . . ? C21_2 N21_2 C51_2 126.4(19) . . ? C21_2 N21_2 Ni2_2 116.2(14) . . ? C51_2 N21_2 Ni2_2 117.4(14) . . ? C23_2 C22_2 C24_2 112.4(18) . . ? C23_2 C22_2 C19_2 110.6(18) . . ? C24_2 C22_2 C19_2 110(2) . . ? C23_2 C22_2 H22_2 107.7 . . ? C24_2 C22_2 H22_2 107.7 . . ? C19_2 C22_2 H22_2 107.7 . . ? C22_2 C23_2 H23A_2 109.5 . . ? C22_2 C23_2 H23B_2 109.5 . . ? H23A_2 C23_2 H23B_2 109.5 . . ? C22_2 C23_2 H23C_2 109.5 . . ? H23A_2 C23_2 H23C_2 109.5 . . ? H23B_2 C23_2 H23C_2 109.5 . . ? C22_2 C24_2 H24A_2 109.5 . . ? C22_2 C24_2 H24B_2 109.5 . . ? H24A_2 C24_2 H24B_2 109.5 . . ? C22_2 C24_2 H24C_2 109.5 . . ? H24A_2 C24_2 H24C_2 109.5 . . ? H24B_2 C24_2 H24C_2 109.5 . . ? C32_2 N31_2 C40_2 118.9(17) . . ? N31_2 C32_2 C33_2 124.3(17) . . ? N31_2 C32_2 C41_2 112.2(16) . . ? C33_2 C32_2 C41_2 123.1(16) . . ? C34_2 C33_2 C32_2 116.6(17) . . ? C34_2 C33_2 H33A_2 121.7 . . ? C32_2 C33_2 H33A_2 121.7 . . ? C35_2 C34_2 C33_2 119.9(18) . . ? C35_2 C34_2 H34_2 120.1 . . ? C33_2 C34_2 H34_2 120.1 . . ? C34_2 C35_2 C40_2 118.0(17) . . ? C34_2 C35_2 C36_2 121.0(18) . . ? C40_2 C35_2 C36_2 120.3(18) . . ? C37_2 C36_2 C35_2 119(2) . . ? C37_2 C36_2 H36_2 120.6 . . ? C35_2 C36_2 H36_2 120.6 . . ? C36_2 C37_2 C38_2 117(2) . . ? C36_2 C37_2 H37_2 121.5 . . ? C38_2 C37_2 H37_2 121.5 . . ? C37_2 C38_2 C39_2 127(2) . . ? C37_2 C38_2 H38_2 116.3 . . ? C39_2 C38_2 H38_2 116.3 . . ? C38_2 C39_2 C40_2 110(2) . . ? C38_2 C39_2 C42_2 125(2) . . ? C40_2 C39_2 C42_2 121(2) . . ? N31_2 C40_2 C35_2 122.0(17) . . ? N31_2 C40_2 C39_2 116.2(18) . . ? C35_2 C40_2 C39_2 121.7(18) . . ? N41_2 C41_2 C32_2 127.6(18) . . ? N41_2 C41_2 H41_2 116.2 . . ? C32_2 C41_2 H41_2 116.2 . . ? C41_2 N41_2 C52_2 116.8(18) . . ? C41_2 N41_2 Ni2_2 135.8(16) . . ? C52_2 N41_2 Ni2_2 107.3(13) . . ? C39_2 C42_2 C44_2 112(3) . . ? C39_2 C42_2 C43_2 113(3) . . ? C44_2 C42_2 C43_2 105(2) . . ? C39_2 C42_2 H42_2 108.9 . . ? C44_2 C42_2 H42_2 108.9 . . ? C43_2 C42_2 H42_2 108.9 . . ? C42_2 C43_2 H43A_2 109.5 . . ? C42_2 C43_2 H43B_2 109.5 . . ? H43A_2 C43_2 H43B_2 109.5 . . ? C42_2 C43_2 H43C_2 109.5 . . ? H43A_2 C43_2 H43C_2 109.5 . . ? H43B_2 C43_2 H43C_2 109.5 . . ? C42_2 C44_2 H44A_2 109.5 . . ? C42_2 C44_2 H44B_2 109.5 . . ? H44A_2 C44_2 H44B_2 109.5 . . ? C42_2 C44_2 H44C_2 109.5 . . ? H44A_2 C44_2 H44C_2 109.5 . . ? H44B_2 C44_2 H44C_2 109.5 . . ? N21_2 C51_2 C56_2 117(2) . . ? N21_2 C51_2 C52_2 107(2) . . ? C56_2 C51_2 C52_2 113(2) . . ? N21_2 C51_2 H51_2 106.3 . . ? C56_2 C51_2 H51_2 106.3 . . ? C52_2 C51_2 H51_2 106.3 . . ? N41_2 C52_2 C51_2 109.4(18) . . ? N41_2 C52_2 C53_2 115(2) . . ? C51_2 C52_2 C53_2 112(2) . . ? N41_2 C52_2 H52_2 106.7 . . ? C51_2 C52_2 H52_2 106.7 . . ? C53_2 C52_2 H52_2 106.7 . . ? C52_2 C53_2 C54_2 110(2) . . ? C52_2 C53_2 H53A_2 109.6 . . ? C54_2 C53_2 H53A_2 109.6 . . ? C52_2 C53_2 H53B_2 109.6 . . ? C54_2 C53_2 H53B_2 109.6 . . ? H53A_2 C53_2 H53B_2 108.1 . . ? C55_2 C54_2 C53_2 110(2) . . ? C55_2 C54_2 H54A_2 109.7 . . ? C53_2 C54_2 H54A_2 109.7 . . ? C55_2 C54_2 H54B_2 109.7 . . ? C53_2 C54_2 H54B_2 109.7 . . ? H54A_2 C54_2 H54B_2 108.2 . . ? C56_2 C55_2 C54_2 114(3) . . ? C56_2 C55_2 H55A_2 108.8 . . ? C54_2 C55_2 H55A_2 108.8 . . ? C56_2 C55_2 H55B_2 108.8 . . ? C54_2 C55_2 H55B_2 108.8 . . ? H55A_2 C55_2 H55B_2 107.7 . . ? C51_2 C56_2 C55_2 111(2) . . ? C51_2 C56_2 H56A_2 109.5 . . ? C55_2 C56_2 H56A_2 109.5 . . ? C51_2 C56_2 H56B_2 109.5 . . ? C55_2 C56_2 H56B_2 109.5 . . ? H56A_2 C56_2 H56B_2 108.1 . . ? 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 N21_1 Ni1_1 N11_1 C12_1 2.8(14) . . . . ? N41_1 Ni1_1 N11_1 C12_1 -15(3) . . . . ? I1_1 Ni1_1 N11_1 C12_1 -99.0(14) . . . . ? I2_1 Ni1_1 N11_1 C12_1 96.4(14) . . . . ? N21_1 Ni1_1 N11_1 C20_1 -173(2) . . . . ? N41_1 Ni1_1 N11_1 C20_1 168(2) . . . . ? I1_1 Ni1_1 N11_1 C20_1 85(2) . . . . ? I2_1 Ni1_1 N11_1 C20_1 -80(2) . . . . ? C20_1 N11_1 C12_1 C13_1 -3(4) . . . . ? Ni1_1 N11_1 C12_1 C13_1 180(2) . . . . ? C20_1 N11_1 C12_1 C21_1 173(2) . . . . ? Ni1_1 N11_1 C12_1 C21_1 -4(2) . . . . ? N11_1 C12_1 C13_1 C14_1 -2(4) . . . . ? C21_1 C12_1 C13_1 C14_1 -177(3) . . . . ? C12_1 C13_1 C14_1 C15_1 1(5) . . . . ? C13_1 C14_1 C15_1 C16_1 177(3) . . . . ? C13_1 C14_1 C15_1 C20_1 4(4) . . . . ? C14_1 C15_1 C16_1 C17_1 177(3) . . . . ? C20_1 C15_1 C16_1 C17_1 -11(4) . . . . ? C15_1 C16_1 C17_1 C18_1 9(4) . . . . ? C16_1 C17_1 C18_1 C19_1 -3(5) . . . . ? C17_1 C18_1 C19_1 C20_1 -1(4) . . . . ? C17_1 C18_1 C19_1 C22_1 -179(3) . . . . ? C12_1 N11_1 C20_1 C19_1 -180(2) . . . . ? Ni1_1 N11_1 C20_1 C19_1 -4(4) . . . . ? C12_1 N11_1 C20_1 C15_1 8(3) . . . . ? Ni1_1 N11_1 C20_1 C15_1 -175.8(17) . . . . ? C18_1 C19_1 C20_1 N11_1 -172(2) . . . . ? C22_1 C19_1 C20_1 N11_1 5(4) . . . . ? C18_1 C19_1 C20_1 C15_1 0(4) . . . . ? C22_1 C19_1 C20_1 C15_1 177(2) . . . . ? C16_1 C15_1 C20_1 N11_1 178(2) . . . . ? C14_1 C15_1 C20_1 N11_1 -9(4) . . . . ? C16_1 C15_1 C20_1 C19_1 6(4) . . . . ? C14_1 C15_1 C20_1 C19_1 179(2) . . . . ? N11_1 C12_1 C21_1 N21_1 5(3) . . . . ? C13_1 C12_1 C21_1 N21_1 -180(2) . . . . ? C12_1 C21_1 N21_1 C51_1 -175(2) . . . . ? C12_1 C21_1 N21_1 Ni1_1 -2(3) . . . . ? N41_1 Ni1_1 N21_1 C21_1 174.7(17) . . . . ? N11_1 Ni1_1 N21_1 C21_1 -0.6(16) . . . . ? I1_1 Ni1_1 N21_1 C21_1 88.8(16) . . . . ? I2_1 Ni1_1 N21_1 C21_1 -91.8(16) . . . . ? N41_1 Ni1_1 N21_1 C51_1 -11.4(14) . . . . ? N11_1 Ni1_1 N21_1 C51_1 173.4(15) . . . . ? I1_1 Ni1_1 N21_1 C51_1 -97.3(13) . . . . ? I2_1 Ni1_1 N21_1 C51_1 82.1(13) . . . . ? C18_1 C19_1 C22_1 C23_1 61(3) . . . . ? C20_1 C19_1 C22_1 C23_1 -117(3) . . . . ? C18_1 C19_1 C22_1 C24_1 -64(3) . . . . ? C20_1 C19_1 C22_1 C24_1 118(3) . . . . ? C40_1 N31_1 C32_1 C33_1 -3(4) . . . . ? C40_1 N31_1 C32_1 C41_1 179(2) . . . . ? N31_1 C32_1 C33_1 C34_1 4(4) . . . . ? C41_1 C32_1 C33_1 C34_1 -178(2) . . . . ? C32_1 C33_1 C34_1 C35_1 -7(4) . . . . ? C33_1 C34_1 C35_1 C40_1 9(4) . . . . ? C33_1 C34_1 C35_1 C36_1 176(3) . . . . ? C34_1 C35_1 C36_1 C37_1 -166(3) . . . . ? C40_1 C35_1 C36_1 C37_1 1(4) . . . . ? C35_1 C36_1 C37_1 C38_1 -19(4) . . . . ? C36_1 C37_1 C38_1 C39_1 30(4) . . . . ? C37_1 C38_1 C39_1 C40_1 -19(4) . . . . ? C37_1 C38_1 C39_1 C42_1 168(3) . . . . ? C32_1 N31_1 C40_1 C35_1 5(4) . . . . ? C32_1 N31_1 C40_1 C39_1 -179(2) . . . . ? C34_1 C35_1 C40_1 N31_1 -8(4) . . . . ? C36_1 C35_1 C40_1 N31_1 -176(3) . . . . ? C34_1 C35_1 C40_1 C39_1 176(3) . . . . ? C36_1 C35_1 C40_1 C39_1 9(4) . . . . ? C38_1 C39_1 C40_1 N31_1 -176(2) . . . . ? C42_1 C39_1 C40_1 N31_1 -3(4) . . . . ? C38_1 C39_1 C40_1 C35_1 0(4) . . . . ? C42_1 C39_1 C40_1 C35_1 173(3) . . . . ? N31_1 C32_1 C41_1 N41_1 -177(2) . . . . ? C33_1 C32_1 C41_1 N41_1 4(4) . . . . ? C32_1 C41_1 N41_1 C52_1 -177(2) . . . . ? C32_1 C41_1 N41_1 Ni1_1 0(4) . . . . ? N21_1 Ni1_1 N41_1 C41_1 166(2) . . . . ? N11_1 Ni1_1 N41_1 C41_1 -176(2) . . . . ? I1_1 Ni1_1 N41_1 C41_1 -92(2) . . . . ? I2_1 Ni1_1 N41_1 C41_1 73(2) . . . . ? N21_1 Ni1_1 N41_1 C52_1 -16.5(12) . . . . ? N11_1 Ni1_1 N41_1 C52_1 2(3) . . . . ? I1_1 Ni1_1 N41_1 C52_1 85.8(11) . . . . ? I2_1 Ni1_1 N41_1 C52_1 -109.8(11) . . . . ? C38_1 C39_1 C42_1 C44_1 -58(4) . . . . ? C40_1 C39_1 C42_1 C44_1 129(3) . . . . ? C38_1 C39_1 C42_1 C43_1 59(4) . . . . ? C40_1 C39_1 C42_1 C43_1 -114(3) . . . . ? C21_1 N21_1 C51_1 C56_1 -28(3) . . . . ? Ni1_1 N21_1 C51_1 C56_1 158.5(16) . . . . ? C21_1 N21_1 C51_1 C52_1 -150(2) . . . . ? Ni1_1 N21_1 C51_1 C52_1 36(2) . . . . ? N21_1 C51_1 C52_1 C53_1 179.8(18) . . . . ? C56_1 C51_1 C52_1 C53_1 55(3) . . . . ? N21_1 C51_1 C52_1 N41_1 -48(2) . . . . ? C56_1 C51_1 C52_1 N41_1 -172.6(18) . . . . ? C41_1 N41_1 C52_1 C53_1 -13(3) . . . . ? Ni1_1 N41_1 C52_1 C53_1 168.9(16) . . . . ? C41_1 N41_1 C52_1 C51_1 -141.8(19) . . . . ? Ni1_1 N41_1 C52_1 C51_1 40.0(17) . . . . ? C51_1 C52_1 C53_1 C54_1 -51(3) . . . . ? N41_1 C52_1 C53_1 C54_1 -178.1(19) . . . . ? C52_1 C53_1 C54_1 C55_1 53(3) . . . . ? C53_1 C54_1 C55_1 C56_1 -54(3) . . . . ? N21_1 C51_1 C56_1 C55_1 -175(2) . . . . ? C52_1 C51_1 C56_1 C55_1 -57(3) . . . . ? C54_1 C55_1 C56_1 C51_1 57(3) . . . . ? N21_2 Ni2_2 N11_2 C12_2 8.7(14) . . . . ? N41_2 Ni2_2 N11_2 C12_2 -12(3) . . . . ? I3_2 Ni2_2 N11_2 C12_2 -96.5(14) . . . . ? I4_2 Ni2_2 N11_2 C12_2 101.0(14) . . . . ? N21_2 Ni2_2 N11_2 C20_2 -175(2) . . . . ? N41_2 Ni2_2 N11_2 C20_2 164(2) . . . . ? I3_2 Ni2_2 N11_2 C20_2 80(2) . . . . ? I4_2 Ni2_2 N11_2 C20_2 -83(2) . . . . ? C20_2 N11_2 C12_2 C13_2 -5(3) . . . . ? Ni2_2 N11_2 C12_2 C13_2 172(2) . . . . ? C20_2 N11_2 C12_2 C21_2 174(2) . . . . ? Ni2_2 N11_2 C12_2 C21_2 -10(2) . . . . ? N11_2 C12_2 C13_2 C14_2 5(4) . . . . ? C21_2 C12_2 C13_2 C14_2 -173(2) . . . . ? C12_2 C13_2 C14_2 C15_2 -4(4) . . . . ? C13_2 C14_2 C15_2 C16_2 179(3) . . . . ? C13_2 C14_2 C15_2 C20_2 4(4) . . . . ? C14_2 C15_2 C16_2 C17_2 -175(3) . . . . ? C20_2 C15_2 C16_2 C17_2 0(4) . . . . ? C15_2 C16_2 C17_2 C18_2 -9(4) . . . . ? C16_2 C17_2 C18_2 C19_2 12(5) . . . . ? C17_2 C18_2 C19_2 C20_2 -5(5) . . . . ? C17_2 C18_2 C19_2 C22_2 174(3) . . . . ? C12_2 N11_2 C20_2 C19_2 179(2) . . . . ? Ni2_2 N11_2 C20_2 C19_2 3(3) . . . . ? C12_2 N11_2 C20_2 C15_2 4(3) . . . . ? Ni2_2 N11_2 C20_2 C15_2 -171.6(19) . . . . ? C18_2 C19_2 C20_2 N11_2 -179(2) . . . . ? C22_2 C19_2 C20_2 N11_2 2(3) . . . . ? C18_2 C19_2 C20_2 C15_2 -4(3) . . . . ? C22_2 C19_2 C20_2 C15_2 176(2) . . . . ? C16_2 C15_2 C20_2 N11_2 -179(2) . . . . ? C14_2 C15_2 C20_2 N11_2 -4(4) . . . . ? C16_2 C15_2 C20_2 C19_2 7(4) . . . . ? C14_2 C15_2 C20_2 C19_2 -178(2) . . . . ? N11_2 C12_2 C21_2 N21_2 5(3) . . . . ? C13_2 C12_2 C21_2 N21_2 -176(2) . . . . ? C12_2 C21_2 N21_2 C51_2 -178(2) . . . . ? C12_2 C21_2 N21_2 Ni2_2 3(3) . . . . ? N41_2 Ni2_2 N21_2 C21_2 167.2(17) . . . . ? N11_2 Ni2_2 N21_2 C21_2 -6.8(16) . . . . ? I3_2 Ni2_2 N21_2 C21_2 79.9(16) . . . . ? I4_2 Ni2_2 N21_2 C21_2 -102.0(16) . . . . ? N41_2 Ni2_2 N21_2 C51_2 -11.2(16) . . . . ? N11_2 Ni2_2 N21_2 C51_2 174.8(17) . . . . ? I3_2 Ni2_2 N21_2 C51_2 -98.6(16) . . . . ? I4_2 Ni2_2 N21_2 C51_2 79.6(16) . . . . ? C18_2 C19_2 C22_2 C23_2 58(3) . . . . ? C20_2 C19_2 C22_2 C23_2 -123(3) . . . . ? C18_2 C19_2 C22_2 C24_2 -68(3) . . . . ? C20_2 C19_2 C22_2 C24_2 112(3) . . . . ? C40_2 N31_2 C32_2 C33_2 0(4) . . . . ? C40_2 N31_2 C32_2 C41_2 -172(2) . . . . ? N31_2 C32_2 C33_2 C34_2 1(4) . . . . ? C41_2 C32_2 C33_2 C34_2 173(2) . . . . ? C32_2 C33_2 C34_2 C35_2 -5(4) . . . . ? C33_2 C34_2 C35_2 C40_2 8(4) . . . . ? C33_2 C34_2 C35_2 C36_2 178(3) . . . . ? C34_2 C35_2 C36_2 C37_2 -180(3) . . . . ? C40_2 C35_2 C36_2 C37_2 -10(4) . . . . ? C35_2 C36_2 C37_2 C38_2 3(5) . . . . ? C36_2 C37_2 C38_2 C39_2 17(5) . . . . ? C37_2 C38_2 C39_2 C40_2 -26(4) . . . . ? C37_2 C38_2 C39_2 C42_2 174(3) . . . . ? C32_2 N31_2 C40_2 C35_2 2(4) . . . . ? C32_2 N31_2 C40_2 C39_2 -173(3) . . . . ? C34_2 C35_2 C40_2 N31_2 -6(4) . . . . ? C36_2 C35_2 C40_2 N31_2 -176(3) . . . . ? C34_2 C35_2 C40_2 C39_2 169(3) . . . . ? C36_2 C35_2 C40_2 C39_2 -1(4) . . . . ? C38_2 C39_2 C40_2 N31_2 -168(2) . . . . ? C42_2 C39_2 C40_2 N31_2 -6(4) . . . . ? C38_2 C39_2 C40_2 C35_2 17(4) . . . . ? C42_2 C39_2 C40_2 C35_2 178(3) . . . . ? N31_2 C32_2 C41_2 N41_2 -171(2) . . . . ? C33_2 C32_2 C41_2 N41_2 16(4) . . . . ? C32_2 C41_2 N41_2 C52_2 -176(2) . . . . ? C32_2 C41_2 N41_2 Ni2_2 0(4) . . . . ? N21_2 Ni2_2 N41_2 C41_2 169(2) . . . . ? N11_2 Ni2_2 N41_2 C41_2 -170(2) . . . . ? I3_2 Ni2_2 N41_2 C41_2 -85(2) . . . . ? I4_2 Ni2_2 N41_2 C41_2 77(2) . . . . ? N21_2 Ni2_2 N41_2 C52_2 -14.4(14) . . . . ? N11_2 Ni2_2 N41_2 C52_2 7(3) . . . . ? I3_2 Ni2_2 N41_2 C52_2 90.7(13) . . . . ? I4_2 Ni2_2 N41_2 C52_2 -107.3(13) . . . . ? C38_2 C39_2 C42_2 C44_2 61(4) . . . . ? C40_2 C39_2 C42_2 C44_2 -98(4) . . . . ? C38_2 C39_2 C42_2 C43_2 -58(5) . . . . ? C40_2 C39_2 C42_2 C43_2 144(3) . . . . ? C21_2 N21_2 C51_2 C56_2 -16(4) . . . . ? Ni2_2 N21_2 C51_2 C56_2 162.0(18) . . . . ? C21_2 N21_2 C51_2 C52_2 -145(2) . . . . ? Ni2_2 N21_2 C51_2 C52_2 34(2) . . . . ? C41_2 N41_2 C52_2 C51_2 -147(2) . . . . ? Ni2_2 N41_2 C52_2 C51_2 36(2) . . . . ? C41_2 N41_2 C52_2 C53_2 -20(3) . . . . ? Ni2_2 N41_2 C52_2 C53_2 162.6(18) . . . . ? N21_2 C51_2 C52_2 N41_2 -44(2) . . . . ? C56_2 C51_2 C52_2 N41_2 -175(2) . . . . ? N21_2 C51_2 C52_2 C53_2 -173(2) . . . . ? C56_2 C51_2 C52_2 C53_2 56(3) . . . . ? N41_2 C52_2 C53_2 C54_2 179(2) . . . . ? C51_2 C52_2 C53_2 C54_2 -55(3) . . . . ? C52_2 C53_2 C54_2 C55_2 53(3) . . . . ? C53_2 C54_2 C55_2 C56_2 -54(3) . . . . ? N21_2 C51_2 C56_2 C55_2 -179(2) . . . . ? C52_2 C51_2 C56_2 C55_2 -54(3) . . . . ? C54_2 C55_2 C56_2 C51_2 53(3) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.307 _refine_diff_density_min -5.033 _refine_diff_density_rms 0.381 data_(R,R)-2a _database_code_depnum_ccdc_archive 'CCDC 846324' #TrackingRef '- output.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; DP-2-96-1 cyclohexyl Ni quinoline imine Ni(OTf) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H72 I3.20 N8 Ni2 O0.80' _chemical_formula_sum 'C64 H72 I3.20 N8 Ni2 O0.80' _chemical_formula_weight 1489.60 _chemical_absolute_configuration ad 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 43.3113(17) _cell_length_b 43.3113(17) _cell_length_c 10.1110(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 16425.8(16) _cell_formula_units_Z 9 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6603 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 20.95 _exptl_crystal_description prism _exptl_crystal_colour browm _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6696 _exptl_absorpt_coefficient_mu 1.909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 40885 _diffrn_reflns_av_R_equivalents 0.1204 _diffrn_reflns_av_sigmaI/netI 0.1352 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_h_max 57 _diffrn_reflns_limit_k_min -56 _diffrn_reflns_limit_k_max 57 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.38 _reflns_number_total 13549 _reflns_number_gt 6745 _reflns_threshold_expression >2sigma(I) _reflns_Friedel_coverage 0.570 _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1700P)^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 0.01(5) _refine_ls_number_reflns 13549 _refine_ls_number_parameters 713 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1615 _refine_ls_R_factor_gt 0.0883 _refine_ls_wR_factor_ref 0.2763 _refine_ls_wR_factor_gt 0.2337 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _refine_ls_shift/su_max 0.001 _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 Ni1_1 Ni 0.58718(6) 0.48954(6) 0.2047(2) 0.0485(6) Uani 1 1 d . . . I1_1 I 0.58880(3) 0.54528(3) 0.09453(10) 0.0608(4) Uani 1 1 d . A . I2_1 I 0.56548(9) 0.41912(8) 0.3073(2) 0.0817(10) Uani 0.50 1 d P A 1 O1_1 O 0.5671(5) 0.4397(5) 0.2224(18) 0.029(4) Uiso 0.50 1 d P A 2 N11_1 N 0.6191(5) 0.4824(4) 0.0614(16) 0.063(4) Uani 1 1 d . A . C12_1 C 0.6526(6) 0.4965(6) 0.109(2) 0.071(6) Uani 1 1 d . . . C13_1 C 0.6800(7) 0.4964(7) 0.049(2) 0.087(7) Uani 1 1 d . A . H13_1 H 0.7032 0.5085 0.0857 0.105 Uiso 1 1 calc R . . C14_1 C 0.6731(7) 0.4778(7) -0.071(2) 0.086(8) Uani 1 1 d . . . H14_1 H 0.6909 0.4748 -0.1147 0.103 Uiso 1 1 calc R A . C15_1 C 0.6415(6) 0.4650(5) -0.1204(19) 0.069(6) Uani 1 1 d . A . C16_1 C 0.6315(7) 0.4485(6) -0.262(2) 0.072(6) Uani 1 1 d . . . H16_1 H 0.6504 0.4490 -0.3123 0.086 Uiso 1 1 calc R A . C17_1 C 0.6028(7) 0.4352(6) -0.316(2) 0.082(7) Uani 1 1 d . A . H17_1 H 0.5994 0.4238 -0.3997 0.098 Uiso 1 1 calc R . . C18_1 C 0.5743(7) 0.4367(5) -0.255(2) 0.075(6) Uani 1 1 d . . . H18_1 H 0.5522 0.4282 -0.2995 0.090 Uiso 1 1 calc R A . C19_1 C 0.5791(5) 0.4513(5) -0.1246(16) 0.063(6) Uani 1 1 d . A . C20_1 C 0.6132(5) 0.4668(5) -0.0625(14) 0.046(4) Uani 1 1 d . . . C21_1 C 0.6594(5) 0.5167(5) 0.2330(17) 0.056(5) Uani 1 1 d . A . H21_1 H 0.6827 0.5289 0.2698 0.067 Uiso 1 1 calc R . . C22_1 C 0.5439(5) 0.4487(5) -0.0537(19) 0.060(5) Uani 1 1 d . . . H22_1 H 0.5511 0.4618 0.0326 0.072 Uiso 1 1 calc R A . C23_1 C 0.5260(6) 0.4650(6) -0.1418(16) 0.075(6) Uani 1 1 d . A . H23A_1 H 0.5051 0.4629 -0.0959 0.112 Uiso 1 1 calc R . . H23B_1 H 0.5185 0.4521 -0.2259 0.112 Uiso 1 1 calc R . . H23C_1 H 0.5431 0.4902 -0.1588 0.112 Uiso 1 1 calc R . . C24_1 C 0.5176(5) 0.4098(5) -0.0280(15) 0.059(5) Uani 1 1 d . A . H24A_1 H 0.4969 0.4077 0.0197 0.089 Uiso 1 1 calc R . . H24B_1 H 0.5290 0.3994 0.0253 0.089 Uiso 1 1 calc R . . H24C_1 H 0.5097 0.3971 -0.1125 0.089 Uiso 1 1 calc R . . N31_1 N 0.4811(3) 0.4353(3) 0.4533(13) 0.038(3) Uani 1 1 d . . . C32_1 C 0.5048(5) 0.4590(5) 0.3767(17) 0.050(4) Uani 1 1 d . A . C33_1 C 0.5010(5) 0.4631(5) 0.2395(18) 0.056(5) Uani 1 1 d . . . H33_1 H 0.5199 0.4807 0.1878 0.067 Uiso 1 1 calc R . . C34_1 C 0.4685(5) 0.4404(4) 0.1866(16) 0.048(4) Uani 1 1 d . . . H34_1 H 0.4643 0.4438 0.0971 0.058 Uiso 1 1 calc R . . C35_1 C 0.4414(4) 0.4126(5) 0.2553(16) 0.045(4) Uani 1 1 d . . . C36_1 C 0.4099(5) 0.3894(6) 0.2050(19) 0.063(5) Uani 1 1 d . . . H36_1 H 0.4044 0.3912 0.1153 0.075 Uiso 1 1 calc R . . C37_1 C 0.3837(5) 0.3609(5) 0.290(2) 0.062(5) Uani 1 1 d . . . H37_1 H 0.3619 0.3430 0.2534 0.074 Uiso 1 1 calc R . . C38_1 C 0.3899(5) 0.3596(5) 0.4173(17) 0.060(5) Uani 1 1 d . . . H38_1 H 0.3717 0.3409 0.4681 0.072 Uiso 1 1 calc R . . C39_1 C 0.4215(4) 0.3839(4) 0.4831(17) 0.044(4) Uani 1 1 d . . . C40_1 C 0.4493(4) 0.4113(5) 0.3983(15) 0.042(4) Uani 1 1 d . . . C41_1 C 0.5400(5) 0.4813(5) 0.4471(17) 0.061(5) Uani 1 1 d . . . H41_1 H 0.5391 0.4842 0.5400 0.074 Uiso 1 1 calc R A . C42_1 C 0.4302(6) 0.3844(5) 0.6192(18) 0.067(6) Uani 1 1 d . . . H42_1 H 0.4441 0.4099 0.6475 0.080 Uiso 1 1 calc R . . C43_1 C 0.4553(5) 0.3673(5) 0.6364(19) 0.055(5) Uani 1 1 d . . . H43A_1 H 0.4762 0.3797 0.5787 0.082 Uiso 1 1 calc R . . H43B_1 H 0.4420 0.3420 0.6123 0.082 Uiso 1 1 calc R . . H43C_1 H 0.4632 0.3697 0.7286 0.082 Uiso 1 1 calc R . . C44_1 C 0.3951(5) 0.3645(6) 0.7143(17) 0.066(6) Uani 1 1 d . . . H44A_1 H 0.4026 0.3644 0.8056 0.099 Uiso 1 1 calc R . . H44B_1 H 0.3798 0.3400 0.6840 0.099 Uiso 1 1 calc R . . H44C_1 H 0.3818 0.3774 0.7104 0.099 Uiso 1 1 calc R . . C51_1 C 0.6338(3) 0.5366(4) 0.4039(14) 0.042(3) Uani 1 1 d . . . H51A_1 H 0.6313 0.5572 0.3732 0.051 Uiso 1 1 calc R A . N51_1 N 0.6332(4) 0.5174(4) 0.2907(12) 0.045(3) Uani 1 1 d . A . C52_1 C 0.6010(4) 0.5128(4) 0.4875(13) 0.042(4) Uani 1 1 d . A . H52A_1 H 0.6043 0.4930 0.5224 0.051 Uiso 1 1 calc R . . N52_1 N 0.5696(3) 0.4962(4) 0.3951(12) 0.044(3) Uani 1 1 d . A . C53_1 C 0.6006(5) 0.5336(6) 0.6031(17) 0.064(6) Uani 1 1 d . . . H53A_1 H 0.5990 0.5543 0.5710 0.076 Uiso 1 1 calc R A . H53B_1 H 0.5790 0.5185 0.6561 0.076 Uiso 1 1 calc R . . C54_1 C 0.6306(4) 0.5459(5) 0.6855(14) 0.052(4) Uani 1 1 d . A . H54A_1 H 0.6325 0.5254 0.7182 0.063 Uiso 1 1 calc R . . H54B_1 H 0.6277 0.5582 0.7629 0.063 Uiso 1 1 calc R . . C55_1 C 0.6668(6) 0.5732(5) 0.6064(17) 0.070(6) Uani 1 1 d . . . H55A_1 H 0.6660 0.5946 0.5774 0.084 Uiso 1 1 calc R A . H55B_1 H 0.6880 0.5807 0.6633 0.084 Uiso 1 1 calc R . . C56_1 C 0.6680(5) 0.5518(5) 0.4852(17) 0.057(5) Uani 1 1 d . A . H56A_1 H 0.6886 0.5676 0.4286 0.068 Uiso 1 1 calc R . . H56B_1 H 0.6715 0.5320 0.5162 0.068 Uiso 1 1 calc R . . Ni2_2 Ni 0.82289(6) 0.57278(7) 0.4573(2) 0.0527(6) Uani 1 1 d . . . I3_2 I 0.88121(3) 0.62328(4) 0.57205(10) 0.0620(4) Uani 1 1 d . B . I4_2 I 0.75401(5) 0.53367(7) 0.36369(18) 0.0798(7) Uani 0.70 1 d P B 1 O2_2 O 0.7719(10) 0.5426(10) 0.439(4) 0.043(9) Uiso 0.30 1 d P B 2 N11_2 N 0.8146(4) 0.5338(4) 0.6069(14) 0.056(4) Uani 1 1 d . B . C12_2 C 0.8239(5) 0.5119(5) 0.5549(17) 0.053(5) Uani 1 1 d . . . C13_2 C 0.8244(6) 0.4821(6) 0.632(2) 0.079(7) Uani 1 1 d . B . H13_2 H 0.8335 0.4684 0.5919 0.095 Uiso 1 1 calc R . . C14_2 C 0.8126(6) 0.4755(6) 0.751(2) 0.073(6) Uani 1 1 d . . . H14_2 H 0.8121 0.4565 0.7991 0.088 Uiso 1 1 calc R B . C15_2 C 0.7992(5) 0.4990(6) 0.8129(17) 0.060(5) Uani 1 1 d . B . C16_2 C 0.7859(7) 0.4939(9) 0.934(2) 0.106(9) Uani 1 1 d . . . H16_2 H 0.7849 0.4747 0.9827 0.127 Uiso 1 1 calc R B . C17_2 C 0.7742(6) 0.5128(7) 0.9914(19) 0.082(7) Uani 1 1 d . B . H17_2 H 0.7656 0.5083 1.0799 0.098 Uiso 1 1 calc R . . C18_2 C 0.7749(5) 0.5398(7) 0.916(2) 0.075(7) Uani 1 1 d . . . H18_2 H 0.7651 0.5529 0.9551 0.090 Uiso 1 1 calc R B . C19_2 C 0.7881(5) 0.5492(6) 0.7931(19) 0.057(5) Uani 1 1 d . B . C20_2 C 0.8003(5) 0.5279(7) 0.746(2) 0.075(6) Uani 1 1 d . . . C21_2 C 0.8385(6) 0.5200(6) 0.4254(19) 0.067(6) Uani 1 1 d . B . H21_2 H 0.8466 0.5055 0.3849 0.081 Uiso 1 1 calc R . . C22_2 C 0.7848(5) 0.5780(6) 0.7254(16) 0.068(6) Uani 1 1 d . . . H22_2 H 0.7953 0.5802 0.6355 0.081 Uiso 1 1 calc R B . C23_2 C 0.8077(6) 0.6160(6) 0.792(2) 0.084(7) Uani 1 1 d . B . H23A_2 H 0.8049 0.6337 0.7411 0.126 Uiso 1 1 calc R . . H23B_2 H 0.8329 0.6226 0.7927 0.126 Uiso 1 1 calc R . . H23C_2 H 0.7995 0.6152 0.8828 0.126 Uiso 1 1 calc R . . C24_2 C 0.7483(6) 0.5725(9) 0.702(2) 0.140(15) Uani 1 1 d . B . H24A_2 H 0.7501 0.5930 0.6544 0.210 Uiso 1 1 calc R . . H24B_2 H 0.7365 0.5700 0.7873 0.210 Uiso 1 1 calc R . . H24C_2 H 0.7344 0.5508 0.6497 0.210 Uiso 1 1 calc R . . N31_2 N 0.7743(4) 0.6287(4) 0.2018(13) 0.056(4) Uani 1 1 d . . . C32_2 C 0.7977(5) 0.6265(6) 0.2831(18) 0.062(5) Uani 1 1 d . B . C33_2 C 0.8009(6) 0.6357(5) 0.4198(19) 0.063(6) Uani 1 1 d . . . H33_2 H 0.8189 0.6354 0.4723 0.076 Uiso 1 1 calc R . . C34_2 C 0.7784(6) 0.6447(6) 0.473(2) 0.066(6) Uani 1 1 d . . . H34_2 H 0.7800 0.6509 0.5643 0.079 Uiso 1 1 calc R . . C35_2 C 0.7515(5) 0.6447(4) 0.3885(15) 0.045(4) Uani 1 1 d . . . C36_2 C 0.7263(5) 0.6526(5) 0.4423(17) 0.055(5) Uani 1 1 d . . . H36_2 H 0.7271 0.6581 0.5336 0.065 Uiso 1 1 calc R . . C37_2 C 0.7015(5) 0.6522(6) 0.3657(15) 0.062(5) Uani 1 1 d . . . H37_2 H 0.6848 0.6582 0.4005 0.074 Uiso 1 1 calc R . . C38_2 C 0.7001(5) 0.6426(5) 0.2270(15) 0.055(5) Uani 1 1 d . . . H38_2 H 0.6817 0.6416 0.1727 0.066 Uiso 1 1 calc R . . C39_2 C 0.7240(5) 0.6352(5) 0.1735(16) 0.050(4) Uani 1 1 d . . . C40_2 C 0.7503(5) 0.6352(5) 0.2549(18) 0.050(4) Uani 1 1 d . . . C41_2 C 0.8207(6) 0.6164(5) 0.221(2) 0.063(5) Uani 1 1 d . . . H41_2 H 0.8260 0.6223 0.1306 0.076 Uiso 1 1 calc R B . C42_2 C 0.7188(4) 0.6221(5) 0.0257(14) 0.038(4) Uani 1 1 d . . . H42_2 H 0.7431 0.6325 -0.0141 0.046 Uiso 1 1 calc R . . C43_2 C 0.7033(5) 0.5862(6) 0.0158(16) 0.067(6) Uani 1 1 d . . . H43A_2 H 0.7154 0.5777 0.0749 0.101 Uiso 1 1 calc R . . H43B_2 H 0.7051 0.5797 -0.0756 0.101 Uiso 1 1 calc R . . H43C_2 H 0.6781 0.5751 0.0408 0.101 Uiso 1 1 calc R . . C44_2 C 0.6990(6) 0.6350(6) -0.054(2) 0.085(7) Uani 1 1 d . . . H44A_2 H 0.6981 0.6276 -0.1466 0.127 Uiso 1 1 calc R . . H44B_2 H 0.7110 0.6610 -0.0497 0.127 Uiso 1 1 calc R . . H44C_2 H 0.6746 0.6248 -0.0201 0.127 Uiso 1 1 calc R . . C51_2 C 0.8505(4) 0.5555(4) 0.2228(14) 0.047(4) Uani 1 1 d . . . H51_2 H 0.8288 0.5414 0.1673 0.056 Uiso 1 1 calc R B . N51_2 N 0.8406(4) 0.5457(4) 0.3659(15) 0.054(4) Uani 1 1 d . B . C52_2 C 0.8621(4) 0.5943(5) 0.2100(14) 0.050(4) Uani 1 1 d . B . H52_2 H 0.8851 0.6082 0.2587 0.060 Uiso 1 1 calc R . . N52_2 N 0.8352(4) 0.5998(4) 0.2783(14) 0.054(4) Uani 1 1 d . B . C53_2 C 0.8687(5) 0.6062(5) 0.0659(19) 0.056(5) Uani 1 1 d . . . H53A_2 H 0.8768 0.6320 0.0583 0.067 Uiso 1 1 calc R B . H53B_2 H 0.8468 0.5926 0.0125 0.067 Uiso 1 1 calc R . . C54_2 C 0.9004(5) 0.5978(5) 0.0165(17) 0.056(4) Uani 1 1 d . B . H54A_2 H 0.9054 0.6037 -0.0785 0.067 Uiso 1 1 calc R . . H54B_2 H 0.9226 0.6132 0.0663 0.067 Uiso 1 1 calc R . . C55_2 C 0.8901(5) 0.5608(5) 0.0369(17) 0.060(5) Uani 1 1 d . . . H55A_2 H 0.9104 0.5574 0.0123 0.072 Uiso 1 1 calc R B . H55B_2 H 0.8700 0.5458 -0.0229 0.072 Uiso 1 1 calc R . . C56_2 C 0.8794(5) 0.5482(5) 0.1747(18) 0.052(4) Uani 1 1 d . B . H56A_2 H 0.9004 0.5605 0.2334 0.062 Uiso 1 1 calc R . . H56B_2 H 0.8706 0.5223 0.1792 0.062 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_1 0.0436(13) 0.0524(15) 0.0408(11) -0.0053(10) -0.0043(10) 0.0175(11) I1_1 0.0626(8) 0.0576(8) 0.0501(6) 0.0099(6) -0.0056(6) 0.0209(7) I2_1 0.100(2) 0.0645(17) 0.0356(11) 0.0049(11) 0.0111(12) 0.0077(15) N11_1 0.077(12) 0.058(10) 0.052(9) -0.014(8) 0.002(8) 0.033(9) C12_1 0.057(13) 0.061(13) 0.078(14) 0.003(11) -0.002(11) 0.015(11) C13_1 0.094(17) 0.13(2) 0.062(12) -0.031(12) 0.012(11) 0.072(17) C14_1 0.082(17) 0.104(19) 0.068(14) -0.041(13) -0.001(12) 0.044(15) C15_1 0.086(16) 0.058(12) 0.050(10) -0.015(9) 0.002(10) 0.027(12) C16_1 0.106(18) 0.074(14) 0.050(11) -0.010(10) 0.025(12) 0.055(14) C17_1 0.095(17) 0.081(16) 0.062(13) -0.041(11) 0.000(12) 0.039(14) C18_1 0.104(18) 0.062(13) 0.053(11) -0.016(10) -0.009(11) 0.037(13) C19_1 0.063(12) 0.066(13) 0.029(8) -0.004(8) -0.004(8) 0.009(10) C20_1 0.056(10) 0.046(10) 0.025(6) -0.004(6) -0.005(7) 0.016(8) C21_1 0.037(9) 0.077(13) 0.044(9) -0.026(8) -0.004(7) 0.021(9) C22_1 0.053(12) 0.065(13) 0.057(11) -0.017(9) -0.025(9) 0.027(11) C23_1 0.119(18) 0.085(15) 0.027(7) 0.005(8) 0.000(9) 0.056(14) C24_1 0.063(11) 0.068(12) 0.026(7) 0.008(7) -0.009(7) 0.017(10) N31_1 0.033(7) 0.041(7) 0.042(7) -0.004(6) -0.006(6) 0.020(6) C32_1 0.045(11) 0.054(11) 0.049(9) 0.002(8) 0.001(8) 0.023(9) C33_1 0.043(10) 0.052(11) 0.057(10) 0.016(9) -0.013(8) 0.012(9) C34_1 0.053(11) 0.041(9) 0.040(9) 0.015(7) -0.007(8) 0.015(8) C35_1 0.039(9) 0.049(10) 0.044(8) -0.004(7) 0.004(7) 0.020(8) C36_1 0.071(14) 0.084(15) 0.050(10) -0.015(9) -0.019(9) 0.052(13) C37_1 0.041(11) 0.045(11) 0.093(14) -0.012(10) -0.012(10) 0.017(9) C38_1 0.059(12) 0.042(10) 0.047(9) 0.009(8) 0.009(8) 0.002(9) C39_1 0.045(10) 0.032(8) 0.053(9) 0.001(7) 0.016(8) 0.018(8) C40_1 0.037(9) 0.047(9) 0.036(7) 0.004(7) 0.004(6) 0.017(8) C41_1 0.044(11) 0.072(13) 0.037(8) 0.001(8) -0.004(8) 0.006(10) C42_1 0.079(15) 0.050(12) 0.046(9) 0.008(8) 0.001(9) 0.013(11) C43_1 0.048(10) 0.067(12) 0.064(11) -0.009(9) -0.006(9) 0.040(10) C44_1 0.051(12) 0.088(15) 0.042(9) 0.001(9) 0.019(8) 0.021(11) C51_1 0.022(7) 0.043(9) 0.049(8) 0.002(7) 0.002(6) 0.006(7) N51_1 0.055(9) 0.049(8) 0.031(6) 0.002(5) -0.005(6) 0.025(7) C52_1 0.027(7) 0.041(9) 0.038(7) 0.012(6) 0.001(6) 0.002(7) N52_1 0.031(7) 0.049(8) 0.036(6) 0.001(6) -0.001(6) 0.009(6) C53_1 0.050(11) 0.099(16) 0.035(9) 0.000(9) 0.010(8) 0.031(11) C54_1 0.048(10) 0.057(11) 0.042(7) -0.007(7) -0.005(7) 0.020(9) C55_1 0.094(15) 0.082(14) 0.046(9) -0.018(9) 0.011(9) 0.053(13) C56_1 0.062(12) 0.067(12) 0.047(9) -0.030(9) -0.009(8) 0.036(10) Ni2_2 0.0470(14) 0.0605(16) 0.0527(13) -0.0093(11) 0.0061(11) 0.0285(13) I3_2 0.0593(8) 0.0716(9) 0.0597(7) -0.0170(7) -0.0107(6) 0.0362(7) I4_2 0.0524(11) 0.142(2) 0.0417(8) -0.0127(10) -0.0043(8) 0.0465(13) N11_2 0.063(10) 0.071(10) 0.042(8) -0.009(7) 0.009(7) 0.039(9) C12_2 0.060(11) 0.043(10) 0.054(10) 0.010(8) 0.023(8) 0.024(9) C13_2 0.076(15) 0.060(14) 0.105(17) 0.022(12) 0.046(13) 0.036(12) C14_2 0.064(13) 0.102(17) 0.060(12) 0.023(11) -0.009(10) 0.046(13) C15_2 0.070(13) 0.066(12) 0.038(8) 0.003(8) 0.002(8) 0.031(10) C16_2 0.078(17) 0.15(3) 0.066(15) 0.003(15) 0.019(13) 0.036(17) C17_2 0.089(16) 0.106(18) 0.031(8) -0.001(10) -0.005(9) 0.035(14) C18_2 0.045(11) 0.114(19) 0.057(11) -0.019(12) 0.001(9) 0.033(12) C19_2 0.045(11) 0.068(12) 0.052(10) -0.011(9) -0.003(8) 0.023(10) C20_2 0.035(10) 0.096(17) 0.075(13) -0.010(12) 0.007(9) 0.019(11) C21_2 0.082(15) 0.068(13) 0.047(9) -0.027(9) -0.004(9) 0.033(12) C22_2 0.038(10) 0.132(19) 0.029(8) -0.011(10) 0.000(7) 0.040(12) C23_2 0.072(14) 0.105(18) 0.085(15) -0.030(13) -0.008(12) 0.052(14) C24_2 0.068(16) 0.26(4) 0.067(14) -0.069(19) 0.003(12) 0.06(2) N31_2 0.085(11) 0.074(11) 0.038(7) -0.005(7) -0.017(7) 0.061(10) C32_2 0.072(13) 0.086(15) 0.055(10) -0.026(10) -0.011(9) 0.060(12) C33_2 0.085(15) 0.058(12) 0.060(11) -0.012(9) -0.033(11) 0.045(12) C34_2 0.090(16) 0.080(14) 0.056(11) -0.018(10) -0.017(10) 0.065(13) C35_2 0.057(11) 0.042(9) 0.039(8) -0.009(7) -0.002(7) 0.027(8) C36_2 0.072(13) 0.070(12) 0.050(9) -0.009(8) -0.008(9) 0.057(11) C37_2 0.055(11) 0.102(16) 0.034(8) -0.013(9) 0.004(7) 0.044(11) C38_2 0.052(11) 0.090(14) 0.032(7) -0.007(8) 0.005(7) 0.042(10) C39_2 0.051(11) 0.053(11) 0.041(8) -0.007(7) -0.004(8) 0.022(9) C40_2 0.047(10) 0.061(11) 0.060(10) 0.006(8) 0.001(8) 0.040(9) C41_2 0.079(14) 0.071(13) 0.054(10) -0.021(9) -0.030(10) 0.048(12) C42_2 0.046(9) 0.054(11) 0.029(6) 0.006(7) 0.004(6) 0.035(9) C43_2 0.070(13) 0.108(18) 0.026(7) -0.010(9) -0.014(8) 0.047(13) C44_2 0.091(18) 0.101(19) 0.082(16) -0.036(14) -0.014(13) 0.062(16) C51_2 0.055(10) 0.041(9) 0.046(8) -0.012(7) 0.008(7) 0.026(8) N51_2 0.032(7) 0.059(9) 0.063(9) 0.010(8) 0.008(6) 0.016(7) C52_2 0.040(9) 0.081(13) 0.040(8) -0.017(8) -0.005(7) 0.037(9) N52_2 0.049(9) 0.068(10) 0.053(8) -0.020(7) -0.009(7) 0.034(8) C53_2 0.065(12) 0.050(10) 0.055(11) -0.003(8) 0.001(9) 0.030(9) C54_2 0.053(10) 0.052(11) 0.063(10) 0.003(8) 0.011(8) 0.027(9) C55_2 0.059(12) 0.072(13) 0.056(9) -0.003(9) 0.017(8) 0.039(11) C56_2 0.062(12) 0.030(9) 0.064(11) 0.002(8) 0.014(9) 0.024(8) _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_1 O1_1 1.892(18) . ? Ni1_1 N51_1 1.944(14) . ? Ni1_1 N11_1 2.129(16) . ? Ni1_1 N52_1 2.142(13) . ? Ni1_1 I1_1 2.628(3) . ? Ni1_1 I2_1 2.897(4) . ? N11_1 C12_1 1.35(3) . ? N11_1 C20_1 1.38(2) . ? C12_1 C13_1 1.34(3) . ? C12_1 C21_1 1.47(3) . ? C13_1 C14_1 1.41(3) . ? C13_1 H13_1 0.9500 . ? C14_1 C15_1 1.29(3) . ? C14_1 H14_1 0.9500 . ? C15_1 C20_1 1.39(3) . ? C15_1 C16_1 1.57(3) . ? C16_1 C17_1 1.21(3) . ? C16_1 H16_1 0.9500 . ? C17_1 C18_1 1.41(3) . ? C17_1 H17_1 0.9500 . ? C18_1 C19_1 1.43(3) . ? C18_1 H18_1 0.9500 . ? C19_1 C20_1 1.43(2) . ? C19_1 C22_1 1.64(3) . ? C21_1 N51_1 1.29(2) . ? C21_1 H21_1 0.9500 . ? C22_1 C24_1 1.51(3) . ? C22_1 C23_1 1.56(3) . ? C22_1 H22_1 1.0000 . ? C23_1 H23A_1 0.9800 . ? C23_1 H23B_1 0.9800 . ? C23_1 H23C_1 0.9800 . ? C24_1 H24A_1 0.9800 . ? C24_1 H24B_1 0.9800 . ? C24_1 H24C_1 0.9800 . ? N31_1 C32_1 1.29(2) . ? N31_1 C40_1 1.36(2) . ? C32_1 C33_1 1.42(2) . ? C32_1 C41_1 1.51(3) . ? C33_1 C34_1 1.36(2) . ? C33_1 H33_1 0.9500 . ? C34_1 C35_1 1.38(2) . ? C34_1 H34_1 0.9500 . ? C35_1 C36_1 1.32(3) . ? C35_1 C40_1 1.49(2) . ? C36_1 C37_1 1.47(3) . ? C36_1 H36_1 0.9500 . ? C37_1 C38_1 1.32(3) . ? C37_1 H37_1 0.9500 . ? C38_1 C39_1 1.41(2) . ? C38_1 H38_1 0.9500 . ? C39_1 C42_1 1.42(2) . ? C39_1 C40_1 1.47(2) . ? C41_1 N52_1 1.23(2) . ? C41_1 H41_1 0.9500 . ? C42_1 C43_1 1.61(3) . ? C42_1 C44_1 1.63(3) . ? C42_1 H42_1 1.0000 . ? C43_1 H43A_1 0.9800 . ? C43_1 H43B_1 0.9800 . ? C43_1 H43C_1 0.9800 . ? C44_1 H44A_1 0.9800 . ? C44_1 H44B_1 0.9800 . ? C44_1 H44C_1 0.9800 . ? C51_1 N51_1 1.410(19) . ? C51_1 C52_1 1.526(18) . ? C51_1 C56_1 1.53(2) . ? C51_1 H51A_1 1.0000 . ? C52_1 C53_1 1.48(2) . ? C52_1 N52_1 1.505(18) . ? C52_1 H52A_1 1.0000 . ? C53_1 C54_1 1.40(2) . ? C53_1 H53A_1 0.9900 . ? C53_1 H53B_1 0.9900 . ? C54_1 C55_1 1.63(2) . ? C54_1 H54A_1 0.9900 . ? C54_1 H54B_1 0.9900 . ? C55_1 C56_1 1.55(2) . ? C55_1 H55A_1 0.9900 . ? C55_1 H55B_1 0.9900 . ? C56_1 H56A_1 0.9900 . ? C56_1 H56B_1 0.9900 . ? Ni2_2 N51_2 1.929(16) . ? Ni2_2 O2_2 1.93(4) . ? Ni2_2 N52_2 2.075(16) . ? Ni2_2 N11_2 2.160(16) . ? Ni2_2 I3_2 2.643(3) . ? Ni2_2 I4_2 2.759(3) . ? N11_2 C12_2 1.31(2) . ? N11_2 C20_2 1.51(2) . ? C12_2 C21_2 1.42(3) . ? C12_2 C13_2 1.52(3) . ? C13_2 C14_2 1.28(3) . ? C13_2 H13_2 0.9500 . ? C14_2 C15_2 1.54(3) . ? C14_2 H14_2 0.9500 . ? C15_2 C16_2 1.32(3) . ? C15_2 C20_2 1.40(3) . ? C16_2 C17_2 1.30(4) . ? C16_2 H16_2 0.9500 . ? C17_2 C18_2 1.38(3) . ? C17_2 H17_2 0.9500 . ? C18_2 C19_2 1.34(3) . ? C18_2 H18_2 0.9500 . ? C19_2 C20_2 1.36(3) . ? C19_2 C22_2 1.49(3) . ? C21_2 N51_2 1.23(2) . ? C21_2 H21_2 0.9500 . ? C22_2 C24_2 1.50(3) . ? C22_2 C23_2 1.59(3) . ? C22_2 H22_2 1.0000 . ? C23_2 H23A_2 0.9800 . ? C23_2 H23B_2 0.9800 . ? C23_2 H23C_2 0.9800 . ? C24_2 H24A_2 0.9800 . ? C24_2 H24B_2 0.9800 . ? C24_2 H24C_2 0.9800 . ? N31_2 C40_2 1.32(2) . ? N31_2 C32_2 1.34(2) . ? C32_2 C41_2 1.42(3) . ? C32_2 C33_2 1.43(3) . ? C33_2 C34_2 1.33(3) . ? C33_2 H33_2 0.9500 . ? C34_2 C35_2 1.45(3) . ? C34_2 H34_2 0.9500 . ? C35_2 C36_2 1.40(2) . ? C35_2 C40_2 1.41(2) . ? C36_2 C37_2 1.32(2) . ? C36_2 H36_2 0.9500 . ? C37_2 C38_2 1.45(2) . ? C37_2 H37_2 0.9500 . ? C38_2 C39_2 1.34(2) . ? C38_2 H38_2 0.9500 . ? C39_2 C40_2 1.40(2) . ? C39_2 C42_2 1.57(2) . ? C41_2 N52_2 1.30(2) . ? C41_2 H41_2 0.9500 . ? C42_2 C43_2 1.36(3) . ? C42_2 C44_2 1.48(3) . ? C42_2 H42_2 1.0000 . ? C43_2 H43A_2 0.9800 . ? C43_2 H43B_2 0.9800 . ? C43_2 H43C_2 0.9800 . ? C44_2 H44A_2 0.9800 . ? C44_2 H44B_2 0.9800 . ? C44_2 H44C_2 0.9800 . ? C51_2 C52_2 1.50(2) . ? C51_2 N51_2 1.51(2) . ? C51_2 C56_2 1.51(2) . ? C51_2 H51_2 1.0000 . ? C52_2 N52_2 1.47(2) . ? C52_2 C53_2 1.52(2) . ? C52_2 H52_2 1.0000 . ? C53_2 C54_2 1.66(2) . ? C53_2 H53A_2 0.9900 . ? C53_2 H53B_2 0.9900 . ? C54_2 C55_2 1.45(2) . ? C54_2 H54A_2 0.9900 . ? C54_2 H54B_2 0.9900 . ? C55_2 C56_2 1.48(2) . ? C55_2 H55A_2 0.9900 . ? C55_2 H55B_2 0.9900 . ? C56_2 H56A_2 0.9900 . ? C56_2 H56B_2 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 O1_1 Ni1_1 N51_1 114.1(7) . . ? O1_1 Ni1_1 N11_1 81.9(7) . . ? N51_1 Ni1_1 N11_1 81.7(6) . . ? O1_1 Ni1_1 N52_1 94.4(7) . . ? N51_1 Ni1_1 N52_1 80.7(5) . . ? N11_1 Ni1_1 N52_1 158.7(6) . . ? O1_1 Ni1_1 I1_1 151.1(6) . . ? N51_1 Ni1_1 I1_1 94.1(4) . . ? N11_1 Ni1_1 I1_1 97.1(5) . . ? N52_1 Ni1_1 I1_1 96.1(4) . . ? O1_1 Ni1_1 I2_1 16.6(6) . . ? N51_1 Ni1_1 I2_1 100.7(4) . . ? N11_1 Ni1_1 I2_1 89.1(5) . . ? N52_1 Ni1_1 I2_1 82.5(4) . . ? I1_1 Ni1_1 I2_1 164.69(12) . . ? C12_1 N11_1 C20_1 116.0(18) . . ? C12_1 N11_1 Ni1_1 108.5(14) . . ? C20_1 N11_1 Ni1_1 135.5(14) . . ? C13_1 C12_1 N11_1 126(2) . . ? C13_1 C12_1 C21_1 118(2) . . ? N11_1 C12_1 C21_1 115(2) . . ? C12_1 C13_1 C14_1 118(2) . . ? C12_1 C13_1 H13_1 121.2 . . ? C14_1 C13_1 H13_1 121.2 . . ? C15_1 C14_1 C13_1 117(2) . . ? C15_1 C14_1 H14_1 121.5 . . ? C13_1 C14_1 H14_1 121.5 . . ? C14_1 C15_1 C20_1 125.9(18) . . ? C14_1 C15_1 C16_1 123(2) . . ? C20_1 C15_1 C16_1 111.2(19) . . ? C17_1 C16_1 C15_1 128(2) . . ? C17_1 C16_1 H16_1 116.0 . . ? C15_1 C16_1 H16_1 116.0 . . ? C16_1 C17_1 C18_1 120(2) . . ? C16_1 C17_1 H17_1 120.2 . . ? C18_1 C17_1 H17_1 120.2 . . ? C17_1 C18_1 C19_1 119(2) . . ? C17_1 C18_1 H18_1 120.3 . . ? C19_1 C18_1 H18_1 120.3 . . ? C20_1 C19_1 C18_1 120.0(19) . . ? C20_1 C19_1 C22_1 123.3(15) . . ? C18_1 C19_1 C22_1 116.7(17) . . ? N11_1 C20_1 C15_1 117.1(16) . . ? N11_1 C20_1 C19_1 121.4(17) . . ? C15_1 C20_1 C19_1 121.4(16) . . ? N51_1 C21_1 C12_1 118.7(17) . . ? N51_1 C21_1 H21_1 120.7 . . ? C12_1 C21_1 H21_1 120.7 . . ? C24_1 C22_1 C23_1 109.4(16) . . ? C24_1 C22_1 C19_1 108.0(16) . . ? C23_1 C22_1 C19_1 112.0(16) . . ? C24_1 C22_1 H22_1 109.1 . . ? C23_1 C22_1 H22_1 109.1 . . ? C19_1 C22_1 H22_1 109.1 . . ? C22_1 C23_1 H23A_1 109.5 . . ? C22_1 C23_1 H23B_1 109.5 . . ? H23A_1 C23_1 H23B_1 109.5 . . ? C22_1 C23_1 H23C_1 109.5 . . ? H23A_1 C23_1 H23C_1 109.5 . . ? H23B_1 C23_1 H23C_1 109.5 . . ? C22_1 C24_1 H24A_1 109.5 . . ? C22_1 C24_1 H24B_1 109.5 . . ? H24A_1 C24_1 H24B_1 109.5 . . ? C22_1 C24_1 H24C_1 109.5 . . ? H24A_1 C24_1 H24C_1 109.5 . . ? H24B_1 C24_1 H24C_1 109.5 . . ? C32_1 N31_1 C40_1 117.5(14) . . ? N31_1 C32_1 C33_1 126.3(17) . . ? N31_1 C32_1 C41_1 112.0(15) . . ? C33_1 C32_1 C41_1 121.5(17) . . ? C34_1 C33_1 C32_1 115.9(17) . . ? C34_1 C33_1 H33_1 122.0 . . ? C32_1 C33_1 H33_1 122.0 . . ? C33_1 C34_1 C35_1 123.8(16) . . ? C33_1 C34_1 H34_1 118.1 . . ? C35_1 C34_1 H34_1 118.1 . . ? C36_1 C35_1 C34_1 125.0(18) . . ? C36_1 C35_1 C40_1 120.7(17) . . ? C34_1 C35_1 C40_1 114.2(15) . . ? C35_1 C36_1 C37_1 118.8(17) . . ? C35_1 C36_1 H36_1 120.6 . . ? C37_1 C36_1 H36_1 120.6 . . ? C38_1 C37_1 C36_1 121.3(18) . . ? C38_1 C37_1 H37_1 119.3 . . ? C36_1 C37_1 H37_1 119.3 . . ? C37_1 C38_1 C39_1 124.8(18) . . ? C37_1 C38_1 H38_1 117.6 . . ? C39_1 C38_1 H38_1 117.6 . . ? C38_1 C39_1 C42_1 128.2(16) . . ? C38_1 C39_1 C40_1 115.2(16) . . ? C42_1 C39_1 C40_1 116.5(16) . . ? N31_1 C40_1 C39_1 119.0(14) . . ? N31_1 C40_1 C35_1 122.0(15) . . ? C39_1 C40_1 C35_1 118.9(15) . . ? N52_1 C41_1 C32_1 125.9(17) . . ? N52_1 C41_1 H41_1 117.1 . . ? C32_1 C41_1 H41_1 117.1 . . ? C39_1 C42_1 C43_1 109.5(16) . . ? C39_1 C42_1 C44_1 113.0(16) . . ? C43_1 C42_1 C44_1 111.2(15) . . ? C39_1 C42_1 H42_1 107.6 . . ? C43_1 C42_1 H42_1 107.6 . . ? C44_1 C42_1 H42_1 107.6 . . ? C42_1 C43_1 H43A_1 109.5 . . ? C42_1 C43_1 H43B_1 109.5 . . ? H43A_1 C43_1 H43B_1 109.5 . . ? C42_1 C43_1 H43C_1 109.5 . . ? H43A_1 C43_1 H43C_1 109.5 . . ? H43B_1 C43_1 H43C_1 109.5 . . ? C42_1 C44_1 H44A_1 109.5 . . ? C42_1 C44_1 H44B_1 109.5 . . ? H44A_1 C44_1 H44B_1 109.5 . . ? C42_1 C44_1 H44C_1 109.5 . . ? H44A_1 C44_1 H44C_1 109.5 . . ? H44B_1 C44_1 H44C_1 109.5 . . ? N51_1 C51_1 C52_1 108.3(12) . . ? N51_1 C51_1 C56_1 114.6(13) . . ? C52_1 C51_1 C56_1 111.6(13) . . ? N51_1 C51_1 H51A_1 107.3 . . ? C52_1 C51_1 H51A_1 107.3 . . ? C56_1 C51_1 H51A_1 107.3 . . ? C21_1 N51_1 C51_1 128.8(14) . . ? C21_1 N51_1 Ni1_1 115.2(11) . . ? C51_1 N51_1 Ni1_1 116.0(10) . . ? C53_1 C52_1 N52_1 119.9(14) . . ? C53_1 C52_1 C51_1 108.3(13) . . ? N52_1 C52_1 C51_1 107.0(11) . . ? C53_1 C52_1 H52A_1 107.0 . . ? N52_1 C52_1 H52A_1 107.0 . . ? C51_1 C52_1 H52A_1 107.0 . . ? C41_1 N52_1 C52_1 116.2(14) . . ? C41_1 N52_1 Ni1_1 131.6(13) . . ? C52_1 N52_1 Ni1_1 108.9(9) . . ? C54_1 C53_1 C52_1 114.2(16) . . ? C54_1 C53_1 H53A_1 108.7 . . ? C52_1 C53_1 H53A_1 108.7 . . ? C54_1 C53_1 H53B_1 108.7 . . ? C52_1 C53_1 H53B_1 108.7 . . ? H53A_1 C53_1 H53B_1 107.6 . . ? C53_1 C54_1 C55_1 111.0(15) . . ? C53_1 C54_1 H54A_1 109.4 . . ? C55_1 C54_1 H54A_1 109.4 . . ? C53_1 C54_1 H54B_1 109.4 . . ? C55_1 C54_1 H54B_1 109.4 . . ? H54A_1 C54_1 H54B_1 108.0 . . ? C56_1 C55_1 C54_1 105.3(15) . . ? C56_1 C55_1 H55A_1 110.7 . . ? C54_1 C55_1 H55A_1 110.7 . . ? C56_1 C55_1 H55B_1 110.7 . . ? C54_1 C55_1 H55B_1 110.7 . . ? H55A_1 C55_1 H55B_1 108.8 . . ? C51_1 C56_1 C55_1 111.4(15) . . ? C51_1 C56_1 H56A_1 109.3 . . ? C55_1 C56_1 H56A_1 109.3 . . ? C51_1 C56_1 H56B_1 109.3 . . ? C55_1 C56_1 H56B_1 109.3 . . ? H56A_1 C56_1 H56B_1 108.0 . . ? N51_2 Ni2_2 O2_2 102.2(12) . . ? N51_2 Ni2_2 N52_2 81.8(6) . . ? O2_2 Ni2_2 N52_2 100.6(12) . . ? N51_2 Ni2_2 N11_2 79.7(6) . . ? O2_2 Ni2_2 N11_2 81.3(12) . . ? N52_2 Ni2_2 N11_2 161.4(6) . . ? N51_2 Ni2_2 I3_2 102.0(4) . . ? O2_2 Ni2_2 I3_2 153.8(11) . . ? N52_2 Ni2_2 I3_2 92.7(4) . . ? N11_2 Ni2_2 I3_2 93.2(4) . . ? N51_2 Ni2_2 I4_2 95.7(4) . . ? O2_2 Ni2_2 I4_2 14.8(11) . . ? N52_2 Ni2_2 I4_2 86.6(4) . . ? N11_2 Ni2_2 I4_2 93.1(4) . . ? I3_2 Ni2_2 I4_2 162.04(11) . . ? C12_2 N11_2 C20_2 120.1(18) . . ? C12_2 N11_2 Ni2_2 107.0(11) . . ? C20_2 N11_2 Ni2_2 132.9(14) . . ? N11_2 C12_2 C21_2 117.0(17) . . ? N11_2 C12_2 C13_2 123.3(17) . . ? C21_2 C12_2 C13_2 119.1(18) . . ? C14_2 C13_2 C12_2 120(2) . . ? C14_2 C13_2 H13_2 120.1 . . ? C12_2 C13_2 H13_2 120.1 . . ? C13_2 C14_2 C15_2 119(2) . . ? C13_2 C14_2 H14_2 120.7 . . ? C15_2 C14_2 H14_2 120.7 . . ? C16_2 C15_2 C20_2 114(2) . . ? C16_2 C15_2 C14_2 123(2) . . ? C20_2 C15_2 C14_2 122.5(17) . . ? C17_2 C16_2 C15_2 126(3) . . ? C17_2 C16_2 H16_2 117.0 . . ? C15_2 C16_2 H16_2 117.0 . . ? C16_2 C17_2 C18_2 116(2) . . ? C16_2 C17_2 H17_2 122.1 . . ? C18_2 C17_2 H17_2 122.1 . . ? C19_2 C18_2 C17_2 126(2) . . ? C19_2 C18_2 H18_2 116.8 . . ? C17_2 C18_2 H18_2 116.8 . . ? C18_2 C19_2 C20_2 112(2) . . ? C18_2 C19_2 C22_2 118.4(19) . . ? C20_2 C19_2 C22_2 129.7(19) . . ? C19_2 C20_2 C15_2 126(2) . . ? C19_2 C20_2 N11_2 119(2) . . ? C15_2 C20_2 N11_2 115.4(19) . . ? N51_2 C21_2 C12_2 119.7(19) . . ? N51_2 C21_2 H21_2 120.1 . . ? C12_2 C21_2 H21_2 120.1 . . ? C19_2 C22_2 C24_2 118(2) . . ? C19_2 C22_2 C23_2 113.8(16) . . ? C24_2 C22_2 C23_2 107.1(19) . . ? C19_2 C22_2 H22_2 105.5 . . ? C24_2 C22_2 H22_2 105.5 . . ? C23_2 C22_2 H22_2 105.5 . . ? C22_2 C23_2 H23A_2 109.5 . . ? C22_2 C23_2 H23B_2 109.5 . . ? H23A_2 C23_2 H23B_2 109.5 . . ? C22_2 C23_2 H23C_2 109.5 . . ? H23A_2 C23_2 H23C_2 109.5 . . ? H23B_2 C23_2 H23C_2 109.5 . . ? C22_2 C24_2 H24A_2 109.5 . . ? C22_2 C24_2 H24B_2 109.5 . . ? H24A_2 C24_2 H24B_2 109.5 . . ? C22_2 C24_2 H24C_2 109.5 . . ? H24A_2 C24_2 H24C_2 109.5 . . ? H24B_2 C24_2 H24C_2 109.5 . . ? C40_2 N31_2 C32_2 117.9(15) . . ? N31_2 C32_2 C41_2 115.0(17) . . ? N31_2 C32_2 C33_2 123.0(17) . . ? C41_2 C32_2 C33_2 121.9(19) . . ? C34_2 C33_2 C32_2 119.6(18) . . ? C34_2 C33_2 H33_2 120.2 . . ? C32_2 C33_2 H33_2 120.2 . . ? C33_2 C34_2 C35_2 117.7(18) . . ? C33_2 C34_2 H34_2 121.1 . . ? C35_2 C34_2 H34_2 121.1 . . ? C36_2 C35_2 C40_2 121.7(16) . . ? C36_2 C35_2 C34_2 119.6(16) . . ? C40_2 C35_2 C34_2 118.6(16) . . ? C37_2 C36_2 C35_2 119.8(17) . . ? C37_2 C36_2 H36_2 120.1 . . ? C35_2 C36_2 H36_2 120.1 . . ? C36_2 C37_2 C38_2 119.1(17) . . ? C36_2 C37_2 H37_2 120.4 . . ? C38_2 C37_2 H37_2 120.4 . . ? C39_2 C38_2 C37_2 122.0(17) . . ? C39_2 C38_2 H38_2 119.0 . . ? C37_2 C38_2 H38_2 119.0 . . ? C38_2 C39_2 C40_2 119.1(16) . . ? C38_2 C39_2 C42_2 118.7(15) . . ? C40_2 C39_2 C42_2 121.8(16) . . ? N31_2 C40_2 C39_2 119.1(17) . . ? N31_2 C40_2 C35_2 122.5(16) . . ? C39_2 C40_2 C35_2 118.2(16) . . ? N52_2 C41_2 C32_2 126(2) . . ? N52_2 C41_2 H41_2 117.2 . . ? C32_2 C41_2 H41_2 117.2 . . ? C43_2 C42_2 C44_2 110.1(16) . . ? C43_2 C42_2 C39_2 112.5(13) . . ? C44_2 C42_2 C39_2 113.0(14) . . ? C43_2 C42_2 H42_2 106.9 . . ? C44_2 C42_2 H42_2 106.9 . . ? C39_2 C42_2 H42_2 106.9 . . ? C42_2 C43_2 H43A_2 109.5 . . ? C42_2 C43_2 H43B_2 109.5 . . ? H43A_2 C43_2 H43B_2 109.5 . . ? C42_2 C43_2 H43C_2 109.5 . . ? H43A_2 C43_2 H43C_2 109.5 . . ? H43B_2 C43_2 H43C_2 109.5 . . ? C42_2 C44_2 H44A_2 109.5 . . ? C42_2 C44_2 H44B_2 109.5 . . ? H44A_2 C44_2 H44B_2 109.5 . . ? C42_2 C44_2 H44C_2 109.5 . . ? H44A_2 C44_2 H44C_2 109.5 . . ? H44B_2 C44_2 H44C_2 109.5 . . ? C52_2 C51_2 N51_2 106.6(11) . . ? C52_2 C51_2 C56_2 110.9(13) . . ? N51_2 C51_2 C56_2 113.5(14) . . ? C52_2 C51_2 H51_2 108.6 . . ? N51_2 C51_2 H51_2 108.6 . . ? C56_2 C51_2 H51_2 108.6 . . ? C21_2 N51_2 C51_2 127.3(16) . . ? C21_2 N51_2 Ni2_2 116.5(14) . . ? C51_2 N51_2 Ni2_2 115.6(11) . . ? N52_2 C52_2 C51_2 107.1(14) . . ? N52_2 C52_2 C53_2 115.0(14) . . ? C51_2 C52_2 C53_2 111.3(13) . . ? N52_2 C52_2 H52_2 107.7 . . ? C51_2 C52_2 H52_2 107.7 . . ? C53_2 C52_2 H52_2 107.7 . . ? C41_2 N52_2 C52_2 121.4(17) . . ? C41_2 N52_2 Ni2_2 129.8(14) . . ? C52_2 N52_2 Ni2_2 108.5(11) . . ? C52_2 C53_2 C54_2 104.4(14) . . ? C52_2 C53_2 H53A_2 110.9 . . ? C54_2 C53_2 H53A_2 110.9 . . ? C52_2 C53_2 H53B_2 110.9 . . ? C54_2 C53_2 H53B_2 110.9 . . ? H53A_2 C53_2 H53B_2 108.9 . . ? C55_2 C54_2 C53_2 111.7(14) . . ? C55_2 C54_2 H54A_2 109.3 . . ? C53_2 C54_2 H54A_2 109.3 . . ? C55_2 C54_2 H54B_2 109.3 . . ? C53_2 C54_2 H54B_2 109.3 . . ? H54A_2 C54_2 H54B_2 107.9 . . ? C54_2 C55_2 C56_2 113.9(14) . . ? C54_2 C55_2 H55A_2 108.8 . . ? C56_2 C55_2 H55A_2 108.8 . . ? C54_2 C55_2 H55B_2 108.8 . . ? C56_2 C55_2 H55B_2 108.8 . . ? H55A_2 C55_2 H55B_2 107.7 . . ? C55_2 C56_2 C51_2 111.6(15) . . ? C55_2 C56_2 H56A_2 109.3 . . ? C51_2 C56_2 H56A_2 109.3 . . ? C55_2 C56_2 H56B_2 109.3 . . ? C51_2 C56_2 H56B_2 109.3 . . ? H56A_2 C56_2 H56B_2 108.0 . . ? 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 O1_1 Ni1_1 N11_1 C12_1 -108.8(15) . . . . ? N51_1 Ni1_1 N11_1 C12_1 7.2(14) . . . . ? N52_1 Ni1_1 N11_1 C12_1 -27(2) . . . . ? I1_1 Ni1_1 N11_1 C12_1 100.4(14) . . . . ? I2_1 Ni1_1 N11_1 C12_1 -93.7(14) . . . . ? O1_1 Ni1_1 N11_1 C20_1 69.9(19) . . . . ? N51_1 Ni1_1 N11_1 C20_1 -174.2(19) . . . . ? N52_1 Ni1_1 N11_1 C20_1 151.3(16) . . . . ? I1_1 Ni1_1 N11_1 C20_1 -81.0(18) . . . . ? I2_1 Ni1_1 N11_1 C20_1 84.9(18) . . . . ? C20_1 N11_1 C12_1 C13_1 0(3) . . . . ? Ni1_1 N11_1 C12_1 C13_1 178(2) . . . . ? C20_1 N11_1 C12_1 C21_1 172.9(17) . . . . ? Ni1_1 N11_1 C12_1 C21_1 -8(2) . . . . ? N11_1 C12_1 C13_1 C14_1 -5(4) . . . . ? C21_1 C12_1 C13_1 C14_1 -178(2) . . . . ? C12_1 C13_1 C14_1 C15_1 6(4) . . . . ? C13_1 C14_1 C15_1 C20_1 -3(4) . . . . ? C13_1 C14_1 C15_1 C16_1 171(2) . . . . ? C14_1 C15_1 C16_1 C17_1 178(3) . . . . ? C20_1 C15_1 C16_1 C17_1 -7(4) . . . . ? C15_1 C16_1 C17_1 C18_1 7(4) . . . . ? C16_1 C17_1 C18_1 C19_1 -5(4) . . . . ? C17_1 C18_1 C19_1 C20_1 5(3) . . . . ? C17_1 C18_1 C19_1 C22_1 -174.2(19) . . . . ? C12_1 N11_1 C20_1 C15_1 4(3) . . . . ? Ni1_1 N11_1 C20_1 C15_1 -174.2(15) . . . . ? C12_1 N11_1 C20_1 C19_1 -179.4(18) . . . . ? Ni1_1 N11_1 C20_1 C19_1 2(3) . . . . ? C14_1 C15_1 C20_1 N11_1 -3(3) . . . . ? C16_1 C15_1 C20_1 N11_1 -177.2(16) . . . . ? C14_1 C15_1 C20_1 C19_1 -179(2) . . . . ? C16_1 C15_1 C20_1 C19_1 7(3) . . . . ? C18_1 C19_1 C20_1 N11_1 177.4(18) . . . . ? C22_1 C19_1 C20_1 N11_1 -3(3) . . . . ? C18_1 C19_1 C20_1 C15_1 -6(3) . . . . ? C22_1 C19_1 C20_1 C15_1 172.9(18) . . . . ? C13_1 C12_1 C21_1 N51_1 179(2) . . . . ? N11_1 C12_1 C21_1 N51_1 5(3) . . . . ? C20_1 C19_1 C22_1 C24_1 -112.6(19) . . . . ? C18_1 C19_1 C22_1 C24_1 67(2) . . . . ? C20_1 C19_1 C22_1 C23_1 127(2) . . . . ? C18_1 C19_1 C22_1 C23_1 -54(2) . . . . ? C40_1 N31_1 C32_1 C33_1 1(3) . . . . ? C40_1 N31_1 C32_1 C41_1 -174.0(16) . . . . ? N31_1 C32_1 C33_1 C34_1 2(3) . . . . ? C41_1 C32_1 C33_1 C34_1 177.2(19) . . . . ? C32_1 C33_1 C34_1 C35_1 -6(3) . . . . ? C33_1 C34_1 C35_1 C36_1 -178(2) . . . . ? C33_1 C34_1 C35_1 C40_1 5(3) . . . . ? C34_1 C35_1 C36_1 C37_1 179.2(17) . . . . ? C40_1 C35_1 C36_1 C37_1 -4(3) . . . . ? C35_1 C36_1 C37_1 C38_1 5(3) . . . . ? C36_1 C37_1 C38_1 C39_1 -2(3) . . . . ? C37_1 C38_1 C39_1 C42_1 -180(2) . . . . ? C37_1 C38_1 C39_1 C40_1 -3(3) . . . . ? C32_1 N31_1 C40_1 C39_1 -179.5(16) . . . . ? C32_1 N31_1 C40_1 C35_1 -2(2) . . . . ? C38_1 C39_1 C40_1 N31_1 -178.3(16) . . . . ? C42_1 C39_1 C40_1 N31_1 -1(2) . . . . ? C38_1 C39_1 C40_1 C35_1 4(2) . . . . ? C42_1 C39_1 C40_1 C35_1 -178.5(16) . . . . ? C36_1 C35_1 C40_1 N31_1 -178.5(17) . . . . ? C34_1 C35_1 C40_1 N31_1 -1(2) . . . . ? C36_1 C35_1 C40_1 C39_1 -1(3) . . . . ? C34_1 C35_1 C40_1 C39_1 176.6(15) . . . . ? N31_1 C32_1 C41_1 N52_1 152(2) . . . . ? C33_1 C32_1 C41_1 N52_1 -23(3) . . . . ? C38_1 C39_1 C42_1 C43_1 100(2) . . . . ? C40_1 C39_1 C42_1 C43_1 -77(2) . . . . ? C38_1 C39_1 C42_1 C44_1 -25(3) . . . . ? C40_1 C39_1 C42_1 C44_1 158.3(16) . . . . ? C12_1 C21_1 N51_1 C51_1 -175.4(17) . . . . ? C12_1 C21_1 N51_1 Ni1_1 2(2) . . . . ? C52_1 C51_1 N51_1 C21_1 -140.2(18) . . . . ? C56_1 C51_1 N51_1 C21_1 -15(3) . . . . ? C52_1 C51_1 N51_1 Ni1_1 42.6(15) . . . . ? C56_1 C51_1 N51_1 Ni1_1 167.9(12) . . . . ? O1_1 Ni1_1 N51_1 C21_1 72.3(15) . . . . ? N11_1 Ni1_1 N51_1 C21_1 -4.9(13) . . . . ? N52_1 Ni1_1 N51_1 C21_1 163.0(14) . . . . ? I1_1 Ni1_1 N51_1 C21_1 -101.5(13) . . . . ? I2_1 Ni1_1 N51_1 C21_1 82.5(13) . . . . ? O1_1 Ni1_1 N51_1 C51_1 -110.1(12) . . . . ? N11_1 Ni1_1 N51_1 C51_1 172.7(12) . . . . ? N52_1 Ni1_1 N51_1 C51_1 -19.4(11) . . . . ? I1_1 Ni1_1 N51_1 C51_1 76.1(10) . . . . ? I2_1 Ni1_1 N51_1 C51_1 -99.9(10) . . . . ? N51_1 C51_1 C52_1 C53_1 -177.2(14) . . . . ? C56_1 C51_1 C52_1 C53_1 55.7(18) . . . . ? N51_1 C51_1 C52_1 N52_1 -46.7(17) . . . . ? C56_1 C51_1 C52_1 N52_1 -173.8(13) . . . . ? C32_1 C41_1 N52_1 C52_1 -171.8(18) . . . . ? C32_1 C41_1 N52_1 Ni1_1 -15(3) . . . . ? C53_1 C52_1 N52_1 C41_1 -43(2) . . . . ? C51_1 C52_1 N52_1 C41_1 -167.0(17) . . . . ? C53_1 C52_1 N52_1 Ni1_1 154.8(13) . . . . ? C51_1 C52_1 N52_1 Ni1_1 31.1(14) . . . . ? O1_1 Ni1_1 N52_1 C41_1 -52.7(19) . . . . ? N51_1 Ni1_1 N52_1 C41_1 -166(2) . . . . ? N11_1 Ni1_1 N52_1 C41_1 -132(2) . . . . ? I1_1 Ni1_1 N52_1 C41_1 100.3(19) . . . . ? I2_1 Ni1_1 N52_1 C41_1 -64.3(18) . . . . ? O1_1 Ni1_1 N52_1 C52_1 105.4(11) . . . . ? N51_1 Ni1_1 N52_1 C52_1 -8.3(10) . . . . ? N11_1 Ni1_1 N52_1 C52_1 26(2) . . . . ? I1_1 Ni1_1 N52_1 C52_1 -101.5(9) . . . . ? I2_1 Ni1_1 N52_1 C52_1 93.8(10) . . . . ? N52_1 C52_1 C53_1 C54_1 176.6(15) . . . . ? C51_1 C52_1 C53_1 C54_1 -60(2) . . . . ? C52_1 C53_1 C54_1 C55_1 63(2) . . . . ? C53_1 C54_1 C55_1 C56_1 -57(2) . . . . ? N51_1 C51_1 C56_1 C55_1 178.9(14) . . . . ? C52_1 C51_1 C56_1 C55_1 -58(2) . . . . ? C54_1 C55_1 C56_1 C51_1 55(2) . . . . ? N51_2 Ni2_2 N11_2 C12_2 -3.3(13) . . . . ? O2_2 Ni2_2 N11_2 C12_2 100.9(17) . . . . ? N52_2 Ni2_2 N11_2 C12_2 3(3) . . . . ? I3_2 Ni2_2 N11_2 C12_2 -104.9(13) . . . . ? I4_2 Ni2_2 N11_2 C12_2 92.0(13) . . . . ? N51_2 Ni2_2 N11_2 C20_2 178.5(17) . . . . ? O2_2 Ni2_2 N11_2 C20_2 -77(2) . . . . ? N52_2 Ni2_2 N11_2 C20_2 -174.7(17) . . . . ? I3_2 Ni2_2 N11_2 C20_2 76.9(16) . . . . ? I4_2 Ni2_2 N11_2 C20_2 -86.3(16) . . . . ? C20_2 N11_2 C12_2 C21_2 -177.6(17) . . . . ? Ni2_2 N11_2 C12_2 C21_2 4(2) . . . . ? C20_2 N11_2 C12_2 C13_2 -6(3) . . . . ? Ni2_2 N11_2 C12_2 C13_2 175.6(17) . . . . ? N11_2 C12_2 C13_2 C14_2 6(4) . . . . ? C21_2 C12_2 C13_2 C14_2 177(2) . . . . ? C12_2 C13_2 C14_2 C15_2 -2(3) . . . . ? C13_2 C14_2 C15_2 C16_2 179(2) . . . . ? C13_2 C14_2 C15_2 C20_2 -2(3) . . . . ? C20_2 C15_2 C16_2 C17_2 1(4) . . . . ? C14_2 C15_2 C16_2 C17_2 -180(2) . . . . ? C15_2 C16_2 C17_2 C18_2 2(4) . . . . ? C16_2 C17_2 C18_2 C19_2 -4(4) . . . . ? C17_2 C18_2 C19_2 C20_2 2(3) . . . . ? C17_2 C18_2 C19_2 C22_2 177(2) . . . . ? C18_2 C19_2 C20_2 C15_2 1(3) . . . . ? C22_2 C19_2 C20_2 C15_2 -173(2) . . . . ? C18_2 C19_2 C20_2 N11_2 177.5(17) . . . . ? C22_2 C19_2 C20_2 N11_2 3(3) . . . . ? C16_2 C15_2 C20_2 C19_2 -2(3) . . . . ? C14_2 C15_2 C20_2 C19_2 178.2(19) . . . . ? C16_2 C15_2 C20_2 N11_2 -178.8(19) . . . . ? C14_2 C15_2 C20_2 N11_2 2(3) . . . . ? C12_2 N11_2 C20_2 C19_2 -174.6(19) . . . . ? Ni2_2 N11_2 C20_2 C19_2 3(3) . . . . ? C12_2 N11_2 C20_2 C15_2 2(3) . . . . ? Ni2_2 N11_2 C20_2 C15_2 -179.8(14) . . . . ? N11_2 C12_2 C21_2 N51_2 -3(3) . . . . ? C13_2 C12_2 C21_2 N51_2 -174.7(19) . . . . ? C18_2 C19_2 C22_2 C24_2 -60(3) . . . . ? C20_2 C19_2 C22_2 C24_2 114(2) . . . . ? C18_2 C19_2 C22_2 C23_2 67(2) . . . . ? C20_2 C19_2 C22_2 C23_2 -119(2) . . . . ? C40_2 N31_2 C32_2 C41_2 174.9(18) . . . . ? C40_2 N31_2 C32_2 C33_2 -9(3) . . . . ? N31_2 C32_2 C33_2 C34_2 5(3) . . . . ? C41_2 C32_2 C33_2 C34_2 -179(2) . . . . ? C32_2 C33_2 C34_2 C35_2 0(3) . . . . ? C33_2 C34_2 C35_2 C36_2 177.3(19) . . . . ? C33_2 C34_2 C35_2 C40_2 0(3) . . . . ? C40_2 C35_2 C36_2 C37_2 -2(3) . . . . ? C34_2 C35_2 C36_2 C37_2 -179.3(19) . . . . ? C35_2 C36_2 C37_2 C38_2 2(3) . . . . ? C36_2 C37_2 C38_2 C39_2 -2(3) . . . . ? C37_2 C38_2 C39_2 C40_2 3(3) . . . . ? C37_2 C38_2 C39_2 C42_2 175.3(17) . . . . ? C32_2 N31_2 C40_2 C39_2 -175.6(18) . . . . ? C32_2 N31_2 C40_2 C35_2 9(3) . . . . ? C38_2 C39_2 C40_2 N31_2 -178.5(18) . . . . ? C42_2 C39_2 C40_2 N31_2 9(3) . . . . ? C38_2 C39_2 C40_2 C35_2 -3(3) . . . . ? C42_2 C39_2 C40_2 C35_2 -175.3(16) . . . . ? C36_2 C35_2 C40_2 N31_2 178.2(18) . . . . ? C34_2 C35_2 C40_2 N31_2 -5(3) . . . . ? C36_2 C35_2 C40_2 C39_2 3(3) . . . . ? C34_2 C35_2 C40_2 C39_2 179.7(17) . . . . ? N31_2 C32_2 C41_2 N52_2 -152(2) . . . . ? C33_2 C32_2 C41_2 N52_2 32(3) . . . . ? C38_2 C39_2 C42_2 C43_2 -99(2) . . . . ? C40_2 C39_2 C42_2 C43_2 74(2) . . . . ? C38_2 C39_2 C42_2 C44_2 27(2) . . . . ? C40_2 C39_2 C42_2 C44_2 -160.8(19) . . . . ? C12_2 C21_2 N51_2 C51_2 -171.0(16) . . . . ? C12_2 C21_2 N51_2 Ni2_2 -1(3) . . . . ? C52_2 C51_2 N51_2 C21_2 -160.1(18) . . . . ? C56_2 C51_2 N51_2 C21_2 -38(2) . . . . ? C52_2 C51_2 N51_2 Ni2_2 29.4(15) . . . . ? C56_2 C51_2 N51_2 Ni2_2 151.8(11) . . . . ? O2_2 Ni2_2 N51_2 C21_2 -76.5(19) . . . . ? N52_2 Ni2_2 N51_2 C21_2 -175.7(16) . . . . ? N11_2 Ni2_2 N51_2 C21_2 2.1(15) . . . . ? I3_2 Ni2_2 N51_2 C21_2 93.3(14) . . . . ? I4_2 Ni2_2 N51_2 C21_2 -90.0(15) . . . . ? O2_2 Ni2_2 N51_2 C51_2 95.0(15) . . . . ? N52_2 Ni2_2 N51_2 C51_2 -4.1(11) . . . . ? N11_2 Ni2_2 N51_2 C51_2 173.7(12) . . . . ? I3_2 Ni2_2 N51_2 C51_2 -95.2(11) . . . . ? I4_2 Ni2_2 N51_2 C51_2 81.6(11) . . . . ? N51_2 C51_2 C52_2 N52_2 -47.0(16) . . . . ? C56_2 C51_2 C52_2 N52_2 -171.0(13) . . . . ? N51_2 C51_2 C52_2 C53_2 -173.5(13) . . . . ? C56_2 C51_2 C52_2 C53_2 62.5(18) . . . . ? C32_2 C41_2 N52_2 C52_2 -172.6(18) . . . . ? C32_2 C41_2 N52_2 Ni2_2 15(3) . . . . ? C51_2 C52_2 N52_2 C41_2 -129.8(17) . . . . ? C53_2 C52_2 N52_2 C41_2 -6(2) . . . . ? C51_2 C52_2 N52_2 Ni2_2 44.3(14) . . . . ? C53_2 C52_2 N52_2 Ni2_2 168.6(12) . . . . ? N51_2 Ni2_2 N52_2 C41_2 150.7(17) . . . . ? O2_2 Ni2_2 N52_2 C41_2 50(2) . . . . ? N11_2 Ni2_2 N52_2 C41_2 144.0(19) . . . . ? I3_2 Ni2_2 N52_2 C41_2 -107.5(16) . . . . ? I4_2 Ni2_2 N52_2 C41_2 54.5(16) . . . . ? N51_2 Ni2_2 N52_2 C52_2 -22.7(11) . . . . ? O2_2 Ni2_2 N52_2 C52_2 -123.7(15) . . . . ? N11_2 Ni2_2 N52_2 C52_2 -29(2) . . . . ? I3_2 Ni2_2 N52_2 C52_2 79.0(10) . . . . ? I4_2 Ni2_2 N52_2 C52_2 -119.0(11) . . . . ? N52_2 C52_2 C53_2 C54_2 178.7(14) . . . . ? C51_2 C52_2 C53_2 C54_2 -59.3(18) . . . . ? C52_2 C53_2 C54_2 C55_2 55.9(19) . . . . ? C53_2 C54_2 C55_2 C56_2 -54(2) . . . . ? C54_2 C55_2 C56_2 C51_2 54(2) . . . . ? C52_2 C51_2 C56_2 C55_2 -55.7(19) . . . . ? N51_2 C51_2 C56_2 C55_2 -175.7(14) . . . . ? _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 2.237 _refine_diff_density_min -1.528 _refine_diff_density_rms 0.193 data_(R,R)-3a _database_code_depnum_ccdc_archive 'CCDC 846325' #TrackingRef '- output.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,2-bis(benzoquinoline imine) cyclohexane Ni I2, dichloromethane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C34 H28 N4) (Ni2 Cl1.85 I2.15) (C H2 Cl2)2.65 ; _chemical_formula_sum 'C36.65 H33.30 Cl7.15 I2.15 N4 Ni2' _chemical_formula_weight 1173.50 _chemical_absolute_configuration syn 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' I I -0.4742 1.8119 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.8504(14) _cell_length_b 14.2408(15) _cell_length_c 23.225(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4580.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2061 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 26.85 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2291 _exptl_absorpt_coefficient_mu 2.718 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.665 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_reflns_number 32516 _diffrn_reflns_av_R_equivalents 0.1255 _diffrn_reflns_av_sigmaI/netI 0.1684 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.91 _reflns_number_total 10504 _reflns_number_gt 4217 _reflns_threshold_expression >2sigma(I) _reflns_Friedel_coverage 0.809 _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1000P)^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 0.04(5) _refine_ls_number_reflns 10504 _refine_ls_number_parameters 476 _refine_ls_number_restraints 109 _refine_ls_R_factor_all 0.1935 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2287 _refine_ls_wR_factor_gt 0.1883 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.000 _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 C1S C -0.1974(17) 0.821(3) -0.2446(13) 0.171(15) Uiso 0.65 1 d PD A 1 H1A H -0.1696 0.7950 -0.2804 0.205 Uiso 0.65 1 calc PR A 1 H1B H -0.2049 0.8898 -0.2499 0.205 Uiso 0.65 1 calc PR A 1 Cl3 Cl -0.3122(9) 0.7705(6) -0.2326(5) 0.176(5) Uani 0.65 1 d PD A 1 Cl4 Cl -0.1174(12) 0.8001(18) -0.1872(8) 0.367(16) Uani 0.65 1 d PD A 1 C2S C -0.177(3) 0.709(5) -0.255(3) 0.189(3) Uiso 0.35 1 d PD B 2 H2A H -0.2254 0.6616 -0.2666 0.227 Uiso 0.35 1 calc PR B 2 H2B H -0.2027 0.7433 -0.2210 0.227 Uiso 0.35 1 calc PR B 2 Cl5 Cl -0.1574(17) 0.7894(17) -0.3123(10) 0.189(3) Uiso 0.35 1 d PD B 2 Cl6 Cl -0.0661(17) 0.6538(17) -0.2371(10) 0.189(3) Uiso 0.35 1 d PD B 2 C3S C 0.035(8) 0.520(3) -0.242(3) 0.189(3) Uiso 0.25 1 d PD C 3 H3A H 0.0052 0.5219 -0.2031 0.227 Uiso 0.25 1 calc PR C 3 H3B H 0.1021 0.5445 -0.2381 0.227 Uiso 0.25 1 calc PR C 3 Cl7 Cl 0.039(2) 0.401(2) -0.2674(15) 0.189(3) Uiso 0.25 1 d PD C 3 Cl8 Cl -0.032(3) 0.594(2) -0.2900(18) 0.189(3) Uiso 0.25 1 d PD C 3 C4S C 0.007(6) 0.476(3) -0.2541(13) 0.189(3) Uiso 0.40 1 d PD D 1 H4A H -0.0244 0.4137 -0.2545 0.227 Uiso 0.40 1 calc PR D 1 H4B H 0.0778 0.4666 -0.2592 0.227 Uiso 0.40 1 calc PR D 1 Cl9 Cl -0.0163(17) 0.5352(15) -0.1870(9) 0.189(3) Uiso 0.40 1 d PD D 1 Cl10 Cl -0.0400(19) 0.5491(17) -0.3116(9) 0.189(3) Uiso 0.40 1 d PD D 1 C5S C -0.213(8) 0.506(4) -0.054(3) 0.189(3) Uiso 0.25 1 d PD E 1 H5A H -0.2437 0.4551 -0.0766 0.227 Uiso 0.25 1 calc PR E 1 H5B H -0.1479 0.4834 -0.0420 0.227 Uiso 0.25 1 calc PR E 1 Cl11 Cl -0.284(3) 0.530(3) 0.0087(14) 0.189(3) Uiso 0.25 1 d PD E 1 Cl12 Cl -0.201(2) 0.610(2) -0.0974(14) 0.189(3) Uiso 0.25 1 d PD E 1 C6S C -0.278(5) 0.5663(19) -0.036(2) 0.189(3) Uiso 0.45 1 d PD F 2 H6A H -0.2585 0.5846 -0.0756 0.227 Uiso 0.45 1 calc PR F 2 H6B H -0.3495 0.5725 -0.0337 0.227 Uiso 0.45 1 calc PR F 2 Cl13 Cl -0.2237(15) 0.6424(12) 0.0143(8) 0.189(3) Uiso 0.45 1 d PD F 2 Cl14 Cl -0.2451(16) 0.4478(12) -0.0233(9) 0.189(3) Uiso 0.45 1 d PD F 2 C7S C -0.267(5) 0.435(3) 0.052(3) 0.189(3) Uiso 0.30 1 d PD G 3 H7A H -0.2631 0.4095 0.0910 0.227 Uiso 0.30 1 calc PR G 3 H7B H -0.3357 0.4478 0.0424 0.227 Uiso 0.30 1 calc PR G 3 Cl15 Cl -0.197(2) 0.5431(18) 0.0464(13) 0.189(3) Uiso 0.30 1 d PD G 3 Cl16 Cl -0.217(2) 0.3544(18) 0.0010(12) 0.189(3) Uiso 0.30 1 d PD G 3 Ni1 Ni 0.34810(15) 0.62166(10) -0.32269(7) 0.0592(6) Uani 1 1 d . . . Ni2 Ni 0.36886(14) 0.60800(10) -0.18123(8) 0.0531(5) Uani 1 1 d . . . Cl1 Cl 0.2385(3) 0.56122(17) -0.24769(14) 0.0862(16) Uani 0.875(6) 1 d P H 1 I1 I 0.2385(3) 0.56122(17) -0.24769(14) 0.0862(16) Uani 0.125(6) 1 d P H 2 Cl2 Cl 0.4103(3) 0.71997(16) -0.24989(14) 0.0611(14) Uani 0.970(5) 1 d P H 1 I2 I 0.4103(3) 0.71997(16) -0.24989(14) 0.0611(14) Uani 0.030(5) 1 d P H 2 I3 I 0.43329(12) 0.71701(8) -0.40565(4) 0.1067(6) Uani 1 1 d . H . I4 I 0.47566(10) 0.69413(7) -0.10209(5) 0.0907(5) Uani 1 1 d . H . N11 N 0.2759(11) 0.5352(8) -0.3772(5) 0.076(3) Uani 1 1 d U H . C12 C 0.3203(17) 0.4554(10) -0.3811(6) 0.085(4) Uani 1 1 d U . . C13 C 0.2896(16) 0.3807(12) -0.4186(8) 0.098(5) Uani 1 1 d U H . H13A H 0.3265 0.3246 -0.4215 0.117 Uiso 1 1 calc R . . C14 C 0.2127(18) 0.3906(14) -0.4477(8) 0.108(6) Uani 1 1 d U . . H14A H 0.1913 0.3414 -0.4722 0.129 Uiso 1 1 calc R H . C15 C 0.1552(16) 0.4802(13) -0.4434(7) 0.098(5) Uani 1 1 d U H . C16 C 0.0735(17) 0.4905(15) -0.4773(6) 0.104(5) Uani 1 1 d U . . H16A H 0.0501 0.4439 -0.5030 0.125 Uiso 1 1 calc R H . C17 C 0.031(2) 0.5762(18) -0.4692(9) 0.140(8) Uani 1 1 d U H . H17A H -0.0280 0.5869 -0.4893 0.168 Uiso 1 1 calc R . . C18 C 0.0601(17) 0.6409(14) -0.4386(7) 0.100(5) Uani 1 1 d U . . C19 C -0.004(2) 0.7256(18) -0.4280(9) 0.152(9) Uani 1 1 d U H . H19A H -0.0664 0.7312 -0.4450 0.182 Uiso 1 1 calc R . . C20 C 0.0301(17) 0.7884(16) -0.3953(8) 0.125(7) Uani 1 1 d U . . H20A H -0.0040 0.8463 -0.3953 0.150 Uiso 1 1 calc R H . C21 C 0.1092(16) 0.7852(13) -0.3598(8) 0.109(7) Uani 1 1 d U H . H21A H 0.1244 0.8339 -0.3333 0.130 Uiso 1 1 calc R . . C22 C 0.1649(15) 0.7055(11) -0.3658(6) 0.085(5) Uani 1 1 d U . . H22A H 0.2220 0.7001 -0.3434 0.103 Uiso 1 1 calc R H . C23 C 0.1418(15) 0.6341(11) -0.4024(7) 0.086(4) Uani 1 1 d U H . C24 C 0.1891(14) 0.5486(11) -0.4089(6) 0.077(4) Uani 1 1 d U . . C25 C 0.4140(15) 0.4463(10) -0.3498(8) 0.079(5) Uani 1 1 d . H . H25A H 0.4530 0.3917 -0.3529 0.094 Uiso 1 1 calc R . . N25 N 0.4386(10) 0.5161(7) -0.3188(6) 0.076(4) Uani 1 1 d . H . N31 N 0.2925(9) 0.5286(7) -0.1236(4) 0.057(3) Uani 1 1 d U H . C32 C 0.3378(14) 0.4428(10) -0.1213(7) 0.073(4) Uani 1 1 d U . . C33 C 0.2996(16) 0.3753(12) -0.0848(9) 0.107(6) Uani 1 1 d U H . H33A H 0.3291 0.3151 -0.0854 0.128 Uiso 1 1 calc R . . C34 C 0.2248(16) 0.3870(13) -0.0487(8) 0.101(5) Uani 1 1 d U . . H34A H 0.2049 0.3397 -0.0225 0.121 Uiso 1 1 calc R H . C35 C 0.1771(14) 0.4764(12) -0.0528(7) 0.081(4) Uani 1 1 d U H . C36 C 0.0956(16) 0.4941(14) -0.0210(7) 0.100(5) Uani 1 1 d U . . H36A H 0.0708 0.4442 0.0018 0.120 Uiso 1 1 calc R H . C37 C 0.0464(16) 0.5788(15) -0.0193(7) 0.107(5) Uani 1 1 d U H . H37A H -0.0076 0.5872 0.0054 0.128 Uiso 1 1 calc R . . C38 C 0.0819(14) 0.6602(12) -0.0591(6) 0.078(4) Uani 1 1 d U . . C39 C 0.0370(17) 0.7411(14) -0.0649(8) 0.108(6) Uani 1 1 d U H . H39A H -0.0196 0.7514 -0.0427 0.130 Uiso 1 1 calc R . . C40 C 0.0670(13) 0.8115(11) -0.1011(7) 0.083(4) Uani 1 1 d U . . H40A H 0.0334 0.8694 -0.1042 0.100 Uiso 1 1 calc R H . C41 C 0.1470(14) 0.7931(13) -0.1318(7) 0.099(6) Uani 1 1 d U H . H41A H 0.1698 0.8415 -0.1564 0.118 Uiso 1 1 calc R . . C42 C 0.1992(13) 0.7102(11) -0.1307(6) 0.083(5) Uani 1 1 d U . . H42A H 0.2547 0.7026 -0.1542 0.100 Uiso 1 1 calc R H . C43 C 0.1695(12) 0.6407(9) -0.0956(6) 0.071(4) Uani 1 1 d U H . C44 C 0.2146(13) 0.5465(9) -0.0886(6) 0.061(3) Uani 1 1 d U . . C45 C 0.4172(14) 0.4245(11) -0.1599(7) 0.079(5) Uani 1 1 d . H . H45A H 0.4476 0.3648 -0.1613 0.095 Uiso 1 1 calc R . . N45 N 0.4451(9) 0.4929(7) -0.1924(6) 0.063(4) Uani 1 1 d . H . C51 C 0.5326(12) 0.5170(9) -0.2861(9) 0.083(4) Uani 1 1 d U . . H51A H 0.5430 0.5834 -0.2736 0.100 Uiso 1 1 calc R H . C52 C 0.5286(12) 0.4616(10) -0.2339(9) 0.092(5) Uani 1 1 d U H . H52A H 0.5211 0.3936 -0.2437 0.110 Uiso 1 1 calc R . . C53 C 0.6242(14) 0.4769(11) -0.1986(9) 0.103(5) Uani 1 1 d U . . H53A H 0.6305 0.4294 -0.1677 0.124 Uiso 1 1 calc R H . H53B H 0.6255 0.5403 -0.1811 0.124 Uiso 1 1 calc R . . C54 C 0.7100(14) 0.4653(12) -0.2460(12) 0.131(7) Uani 1 1 d U H . H54A H 0.7707 0.4845 -0.2268 0.157 Uiso 1 1 calc R . . H54B H 0.7159 0.3973 -0.2541 0.157 Uiso 1 1 calc R . . C55 C 0.7082(15) 0.5110(14) -0.2998(12) 0.135(8) Uani 1 1 d U . . H55A H 0.7628 0.4886 -0.3236 0.161 Uiso 1 1 calc R H . H55B H 0.7161 0.5795 -0.2940 0.161 Uiso 1 1 calc R . . C56 C 0.6183(14) 0.4932(10) -0.3296(10) 0.113(5) Uani 1 1 d U H . H56A H 0.6148 0.4266 -0.3416 0.135 Uiso 1 1 calc R . . H56B H 0.6136 0.5331 -0.3644 0.135 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 Cl3 0.237(13) 0.081(5) 0.210(12) -0.024(6) 0.024(10) 0.022(7) Cl4 0.30(2) 0.53(4) 0.27(2) 0.18(2) 0.110(19) 0.20(3) Ni1 0.0978(16) 0.0367(8) 0.0430(10) -0.0111(8) 0.0170(11) -0.0146(9) Ni2 0.0804(13) 0.0325(7) 0.0464(10) 0.0059(7) -0.0058(10) -0.0017(8) Cl1 0.157(4) 0.0600(16) 0.0420(16) 0.0028(14) 0.010(2) 0.0167(17) I1 0.157(4) 0.0600(16) 0.0420(16) 0.0028(14) 0.010(2) 0.0167(17) Cl2 0.100(3) 0.0340(14) 0.0487(17) 0.0010(16) 0.007(2) -0.0059(14) I2 0.100(3) 0.0340(14) 0.0487(17) 0.0010(16) 0.007(2) -0.0059(14) I3 0.1901(15) 0.0844(7) 0.0457(6) -0.0223(6) 0.0331(8) -0.0798(8) I4 0.1422(11) 0.0654(6) 0.0645(7) 0.0155(5) -0.0344(7) -0.0338(7) N11 0.118(10) 0.054(5) 0.057(8) -0.008(6) 0.023(6) -0.035(6) C12 0.166(15) 0.049(6) 0.039(9) -0.017(6) 0.030(9) -0.027(7) C13 0.148(16) 0.062(8) 0.083(14) -0.029(9) 0.037(10) -0.052(9) C14 0.170(18) 0.083(9) 0.070(13) -0.022(10) 0.029(10) -0.057(10) C15 0.150(14) 0.092(9) 0.052(10) -0.021(8) 0.016(9) -0.054(8) C16 0.172(16) 0.119(10) 0.022(7) -0.006(8) -0.002(9) -0.071(10) C17 0.19(2) 0.145(15) 0.079(15) -0.019(13) -0.047(14) -0.030(12) C18 0.158(15) 0.103(9) 0.038(9) 0.021(7) -0.016(9) -0.043(8) C19 0.23(2) 0.141(16) 0.090(15) -0.001(12) -0.079(17) 0.015(14) C20 0.156(18) 0.135(14) 0.083(15) -0.003(11) -0.043(12) 0.012(13) C21 0.161(19) 0.077(9) 0.088(13) 0.015(8) -0.050(12) 0.016(10) C22 0.147(14) 0.071(8) 0.039(8) 0.000(6) -0.014(8) -0.005(9) C23 0.148(12) 0.067(6) 0.044(8) 0.014(6) -0.013(9) -0.044(7) C24 0.124(11) 0.087(7) 0.020(7) -0.019(6) 0.022(7) -0.043(7) C25 0.096(14) 0.048(8) 0.092(13) -0.023(8) 0.044(12) -0.008(9) N25 0.083(10) 0.039(5) 0.106(10) -0.020(7) 0.012(9) -0.013(6) N31 0.088(8) 0.044(5) 0.038(6) 0.014(5) -0.028(5) -0.024(5) C32 0.091(12) 0.053(6) 0.073(11) 0.014(7) -0.039(8) -0.024(6) C33 0.133(16) 0.061(8) 0.126(18) 0.049(9) -0.053(9) -0.045(8) C34 0.149(16) 0.084(8) 0.070(12) 0.040(9) -0.056(8) -0.075(9) C35 0.110(12) 0.087(7) 0.047(9) 0.025(7) -0.049(6) -0.072(7) C36 0.121(15) 0.120(10) 0.061(11) 0.051(11) -0.032(8) -0.080(9) C37 0.145(16) 0.148(12) 0.028(8) 0.025(9) 0.003(9) -0.052(10) C38 0.103(12) 0.092(8) 0.038(8) 0.000(7) 0.011(7) -0.033(7) C39 0.146(17) 0.103(10) 0.076(12) -0.012(9) 0.048(11) -0.006(9) C40 0.105(13) 0.077(8) 0.068(11) -0.017(7) 0.024(9) -0.003(8) C41 0.130(16) 0.077(9) 0.089(13) 0.012(9) 0.048(11) 0.024(10) C42 0.107(13) 0.082(9) 0.061(10) 0.034(8) 0.022(8) 0.019(8) C43 0.114(11) 0.060(6) 0.040(8) -0.008(6) 0.015(7) -0.027(6) C44 0.103(10) 0.054(5) 0.025(7) -0.003(5) -0.024(6) -0.035(5) C45 0.088(14) 0.069(10) 0.080(12) -0.012(9) -0.038(12) 0.003(10) N45 0.062(9) 0.033(5) 0.094(9) 0.023(6) -0.023(7) -0.001(6) C51 0.067(10) 0.032(6) 0.151(13) -0.029(7) 0.002(9) 0.007(8) C52 0.067(9) 0.045(7) 0.164(15) -0.019(8) 0.001(9) 0.001(8) C53 0.105(12) 0.053(8) 0.153(15) -0.018(10) -0.017(9) -0.015(10) C54 0.064(10) 0.068(10) 0.26(2) -0.010(14) 0.011(11) 0.006(10) C55 0.076(10) 0.077(12) 0.25(2) -0.013(13) 0.066(13) -0.037(11) C56 0.106(13) 0.040(7) 0.192(15) -0.043(10) 0.042(11) -0.006(9) _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 C1S Cl4 1.760(18) . ? C1S Cl3 1.768(18) . ? C1S H1A 0.9900 . ? C1S H1B 0.9900 . ? C2S Cl5 1.77(2) . ? C2S Cl6 1.78(2) . ? C2S H2A 0.9900 . ? C2S H2B 0.9900 . ? C3S Cl8 1.80(2) . ? C3S Cl7 1.80(2) . ? C3S H3A 0.9900 . ? C3S H3B 0.9900 . ? C4S Cl9 1.80(2) . ? C4S Cl10 1.82(2) . ? C4S H4A 0.9900 . ? C4S H4B 0.9900 . ? C5S Cl11 1.79(2) . ? C5S Cl12 1.81(2) . ? C5S H5A 0.9900 . ? C5S H5B 0.9900 . ? C6S Cl13 1.77(2) . ? C6S Cl14 1.78(2) . ? C6S H6A 0.9900 . ? C6S H6B 0.9900 . ? C7S Cl16 1.78(2) . ? C7S Cl15 1.82(2) . ? C7S H7A 0.9900 . ? C7S H7B 0.9900 . ? Ni1 N25 1.959(13) . ? Ni1 N11 2.030(13) . ? Ni1 Cl2 2.358(3) . ? Ni1 Cl1 2.465(4) . ? Ni1 I3 2.636(2) . ? Ni2 N45 1.967(11) . ? Ni2 N31 2.047(11) . ? Ni2 Cl2 2.327(3) . ? Ni2 Cl1 2.467(4) . ? Ni2 I4 2.659(2) . ? N11 C12 1.30(2) . ? N11 C24 1.42(2) . ? C12 C13 1.44(2) . ? C12 C25 1.49(3) . ? C13 C14 1.27(3) . ? C13 H13A 0.9500 . ? C14 C15 1.51(3) . ? C14 H14A 0.9500 . ? C15 C24 1.35(2) . ? C15 C16 1.39(3) . ? C16 C17 1.37(3) . ? C16 H16A 0.9500 . ? C17 C18 1.23(3) . ? C17 H17A 0.9500 . ? C18 C23 1.41(2) . ? C18 C19 1.52(3) . ? C19 C20 1.27(3) . ? C19 H19A 0.9500 . ? C20 C21 1.37(2) . ? C20 H20A 0.9500 . ? C21 C22 1.38(2) . ? C21 H21A 0.9500 . ? C22 C23 1.36(2) . ? C22 H22A 0.9500 . ? C23 C24 1.39(2) . ? C25 N25 1.275(18) . ? C25 H25A 0.9500 . ? N25 C51 1.51(2) . ? N31 C32 1.374(19) . ? N31 C44 1.375(19) . ? C32 C33 1.39(2) . ? C32 C45 1.44(2) . ? C33 C34 1.34(3) . ? C33 H33A 0.9500 . ? C34 C35 1.44(3) . ? C34 H34A 0.9500 . ? C35 C36 1.37(3) . ? C35 C44 1.399(19) . ? C36 C37 1.39(3) . ? C36 H36A 0.9500 . ? C37 C38 1.56(2) . ? C37 H37A 0.9500 . ? C38 C39 1.32(2) . ? C38 C43 1.51(2) . ? C39 C40 1.37(2) . ? C39 H39A 0.9500 . ? C40 C41 1.34(2) . ? C40 H40A 0.9500 . ? C41 C42 1.39(2) . ? C41 H41A 0.9500 . ? C42 C43 1.346(19) . ? C42 H42A 0.9500 . ? C43 C44 1.49(2) . ? C45 N45 1.291(19) . ? C45 H45A 0.9500 . ? N45 C52 1.57(2) . ? C51 C52 1.45(3) . ? C51 C56 1.60(2) . ? C51 H51A 1.0000 . ? C52 C53 1.57(2) . ? C52 H52A 1.0000 . ? C53 C54 1.63(3) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.41(3) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.45(3) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9900 . ? C56 H56B 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 Cl4 C1S Cl3 112.2(15) . . ? Cl4 C1S H1A 109.2 . . ? Cl3 C1S H1A 109.2 . . ? Cl4 C1S H1B 109.2 . . ? Cl3 C1S H1B 109.2 . . ? H1A C1S H1B 107.9 . . ? Cl5 C2S Cl6 109.0(16) . . ? Cl5 C2S H2A 109.9 . . ? Cl6 C2S H2A 109.9 . . ? Cl5 C2S H2B 109.9 . . ? Cl6 C2S H2B 109.9 . . ? H2A C2S H2B 108.3 . . ? Cl8 C3S Cl7 111.0(17) . . ? Cl8 C3S H3A 109.4 . . ? Cl7 C3S H3A 109.4 . . ? Cl8 C3S H3B 109.4 . . ? Cl7 C3S H3B 109.4 . . ? H3A C3S H3B 108.0 . . ? Cl9 C4S Cl10 107.5(15) . . ? Cl9 C4S H4A 110.2 . . ? Cl10 C4S H4A 110.2 . . ? Cl9 C4S H4B 110.2 . . ? Cl10 C4S H4B 110.2 . . ? H4A C4S H4B 108.5 . . ? Cl11 C5S Cl12 110.1(17) . . ? Cl11 C5S H5A 109.6 . . ? Cl12 C5S H5A 109.6 . . ? Cl11 C5S H5B 109.6 . . ? Cl12 C5S H5B 109.6 . . ? H5A C5S H5B 108.1 . . ? Cl13 C6S Cl14 111.0(16) . . ? Cl13 C6S H6A 109.4 . . ? Cl14 C6S H6A 109.4 . . ? Cl13 C6S H6B 109.4 . . ? Cl14 C6S H6B 109.4 . . ? H6A C6S H6B 108.0 . . ? Cl16 C7S Cl15 107.3(16) . . ? Cl16 C7S H7A 110.3 . . ? Cl15 C7S H7A 110.3 . . ? Cl16 C7S H7B 110.3 . . ? Cl15 C7S H7B 110.3 . . ? H7A C7S H7B 108.5 . . ? N25 Ni1 N11 83.0(6) . . ? N25 Ni1 Cl2 100.9(4) . . ? N11 Ni1 Cl2 170.9(4) . . ? N25 Ni1 Cl1 95.3(4) . . ? N11 Ni1 Cl1 85.7(3) . . ? Cl2 Ni1 Cl1 85.73(12) . . ? N25 Ni1 I3 98.2(4) . . ? N11 Ni1 I3 94.4(3) . . ? Cl2 Ni1 I3 93.14(9) . . ? Cl1 Ni1 I3 166.37(12) . . ? N45 Ni2 N31 84.4(5) . . ? N45 Ni2 Cl2 110.4(4) . . ? N31 Ni2 Cl2 162.6(4) . . ? N45 Ni2 Cl1 94.9(3) . . ? N31 Ni2 Cl1 83.2(3) . . ? Cl2 Ni2 Cl1 86.37(12) . . ? N45 Ni2 I4 100.2(3) . . ? N31 Ni2 I4 95.2(3) . . ? Cl2 Ni2 I4 91.17(10) . . ? Cl1 Ni2 I4 164.61(11) . . ? Ni1 Cl1 Ni2 84.10(13) . . ? Ni2 Cl2 Ni1 89.69(10) . . ? C12 N11 C24 118.9(15) . . ? C12 N11 Ni1 110.0(14) . . ? C24 N11 Ni1 131.1(11) . . ? N11 C12 C13 123(2) . . ? N11 C12 C25 117.0(15) . . ? C13 C12 C25 119.2(18) . . ? C14 C13 C12 119(2) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C15 120.2(19) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C24 C15 C16 123(2) . . ? C24 C15 C14 118(2) . . ? C16 C15 C14 119.0(18) . . ? C17 C16 C15 111.7(18) . . ? C17 C16 H16A 124.2 . . ? C15 C16 H16A 124.2 . . ? C18 C17 C16 127(3) . . ? C18 C17 H17A 116.5 . . ? C16 C17 H17A 116.5 . . ? C17 C18 C23 124(2) . . ? C17 C18 C19 119(2) . . ? C23 C18 C19 115.4(18) . . ? C20 C19 C18 116(2) . . ? C20 C19 H19A 122.1 . . ? C18 C19 H19A 122.1 . . ? C19 C20 C21 130(2) . . ? C19 C20 H20A 115.2 . . ? C21 C20 H20A 115.2 . . ? C20 C21 C22 114.4(19) . . ? C20 C21 H21A 122.8 . . ? C22 C21 H21A 122.8 . . ? C23 C22 C21 123.1(18) . . ? C23 C22 H22A 118.5 . . ? C21 C22 H22A 118.5 . . ? C22 C23 C24 127.6(18) . . ? C22 C23 C18 120.5(18) . . ? C24 C23 C18 111.9(16) . . ? C15 C24 C23 122(2) . . ? C15 C24 N11 120.3(19) . . ? C23 C24 N11 117.4(14) . . ? N25 C25 C12 116.2(16) . . ? N25 C25 H25A 121.9 . . ? C12 C25 H25A 121.9 . . ? C25 N25 C51 121.5(14) . . ? C25 N25 Ni1 113.6(13) . . ? C51 N25 Ni1 124.8(8) . . ? C32 N31 C44 120.1(12) . . ? C32 N31 Ni2 106.3(11) . . ? C44 N31 Ni2 133.6(9) . . ? N31 C32 C33 117.7(19) . . ? N31 C32 C45 119.0(14) . . ? C33 C32 C45 123.1(18) . . ? C34 C33 C32 126(2) . . ? C34 C33 H33A 116.9 . . ? C32 C33 H33A 116.9 . . ? C33 C34 C35 115.1(16) . . ? C33 C34 H34A 122.5 . . ? C35 C34 H34A 122.5 . . ? C36 C35 C44 119.6(19) . . ? C36 C35 C34 120.4(16) . . ? C44 C35 C34 120(2) . . ? C35 C36 C37 125.4(16) . . ? C35 C36 H36A 117.3 . . ? C37 C36 H36A 117.3 . . ? C36 C37 C38 118.3(18) . . ? C36 C37 H37A 120.8 . . ? C38 C37 H37A 120.8 . . ? C39 C38 C43 119.0(15) . . ? C39 C38 C37 124.1(19) . . ? C43 C38 C37 116.8(17) . . ? C38 C39 C40 123.9(19) . . ? C38 C39 H39A 118.0 . . ? C40 C39 H39A 118.0 . . ? C41 C40 C39 115.7(17) . . ? C41 C40 H40A 122.2 . . ? C39 C40 H40A 122.2 . . ? C40 C41 C42 126.0(17) . . ? C40 C41 H41A 117.0 . . ? C42 C41 H41A 117.0 . . ? C43 C42 C41 118.6(16) . . ? C43 C42 H42A 120.7 . . ? C41 C42 H42A 120.7 . . ? C42 C43 C44 126.9(15) . . ? C42 C43 C38 116.8(15) . . ? C44 C43 C38 116.3(13) . . ? N31 C44 C35 120.6(15) . . ? N31 C44 C43 115.6(12) . . ? C35 C44 C43 123.5(17) . . ? N45 C45 C32 117.1(15) . . ? N45 C45 H45A 121.4 . . ? C32 C45 H45A 121.4 . . ? C45 N45 C52 111.5(13) . . ? C45 N45 Ni2 113.0(12) . . ? C52 N45 Ni2 135.5(9) . . ? C52 C51 N25 112.6(14) . . ? C52 C51 C56 116.3(14) . . ? N25 C51 C56 108.8(15) . . ? C52 C51 H51A 106.1 . . ? N25 C51 H51A 106.1 . . ? C56 C51 H51A 106.1 . . ? C51 C52 N45 112.8(13) . . ? C51 C52 C53 109.2(15) . . ? N45 C52 C53 105.1(14) . . ? C51 C52 H52A 109.9 . . ? N45 C52 H52A 109.9 . . ? C53 C52 H52A 109.9 . . ? C52 C53 C54 104.4(16) . . ? C52 C53 H53A 110.9 . . ? C54 C53 H53A 110.9 . . ? C52 C53 H53B 110.9 . . ? C54 C53 H53B 110.9 . . ? H53A C53 H53B 108.9 . . ? C55 C54 C53 122.6(18) . . ? C55 C54 H54A 106.7 . . ? C53 C54 H54A 106.7 . . ? C55 C54 H54B 106.7 . . ? C53 C54 H54B 106.7 . . ? H54A C54 H54B 106.6 . . ? C54 C55 C56 111.0(17) . . ? C54 C55 H55A 109.4 . . ? C56 C55 H55A 109.4 . . ? C54 C55 H55B 109.4 . . ? C56 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? C55 C56 C51 107.4(17) . . ? C55 C56 H56A 110.2 . . ? C51 C56 H56A 110.2 . . ? C55 C56 H56B 110.2 . . ? C51 C56 H56B 110.2 . . ? H56A C56 H56B 108.5 . . ? 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 N25 Ni1 Cl1 Ni2 73.5(4) . . . . ? N11 Ni1 Cl1 Ni2 156.1(4) . . . . ? Cl2 Ni1 Cl1 Ni2 -26.99(11) . . . . ? I3 Ni1 Cl1 Ni2 -112.7(5) . . . . ? N45 Ni2 Cl1 Ni1 -82.8(4) . . . . ? N31 Ni2 Cl1 Ni1 -166.6(4) . . . . ? Cl2 Ni2 Cl1 Ni1 27.36(11) . . . . ? I4 Ni2 Cl1 Ni1 108.5(4) . . . . ? N45 Ni2 Cl2 Ni1 65.3(4) . . . . ? N31 Ni2 Cl2 Ni1 -81.8(10) . . . . ? Cl1 Ni2 Cl2 Ni1 -28.55(12) . . . . ? I4 Ni2 Cl2 Ni1 166.65(11) . . . . ? N25 Ni1 Cl2 Ni2 -66.0(4) . . . . ? N11 Ni1 Cl2 Ni2 49(3) . . . . ? Cl1 Ni1 Cl2 Ni2 28.60(12) . . . . ? I3 Ni1 Cl2 Ni2 -165.02(11) . . . . ? N25 Ni1 N11 C12 2.2(11) . . . . ? Cl2 Ni1 N11 C12 -114(3) . . . . ? Cl1 Ni1 N11 C12 -93.7(10) . . . . ? I3 Ni1 N11 C12 99.9(10) . . . . ? N25 Ni1 N11 C24 -178.6(13) . . . . ? Cl2 Ni1 N11 C24 65(3) . . . . ? Cl1 Ni1 N11 C24 85.5(12) . . . . ? I3 Ni1 N11 C24 -80.8(12) . . . . ? C24 N11 C12 C13 4(2) . . . . ? Ni1 N11 C12 C13 -177.0(13) . . . . ? C24 N11 C12 C25 176.6(13) . . . . ? Ni1 N11 C12 C25 -4.1(17) . . . . ? N11 C12 C13 C14 -3(3) . . . . ? C25 C12 C13 C14 -176.1(18) . . . . ? C12 C13 C14 C15 1(3) . . . . ? C13 C14 C15 C24 1(3) . . . . ? C13 C14 C15 C16 177.6(19) . . . . ? C24 C15 C16 C17 -3(3) . . . . ? C14 C15 C16 C17 -178.8(19) . . . . ? C15 C16 C17 C18 4(4) . . . . ? C16 C17 C18 C23 -5(4) . . . . ? C16 C17 C18 C19 -171(2) . . . . ? C17 C18 C19 C20 179(2) . . . . ? C23 C18 C19 C20 11(3) . . . . ? C18 C19 C20 C21 -13(4) . . . . ? C19 C20 C21 C22 8(4) . . . . ? C20 C21 C22 C23 -2(3) . . . . ? C21 C22 C23 C24 -175.4(18) . . . . ? C21 C22 C23 C18 3(3) . . . . ? C17 C18 C23 C22 -174(2) . . . . ? C19 C18 C23 C22 -7(2) . . . . ? C17 C18 C23 C24 5(3) . . . . ? C19 C18 C23 C24 171.4(17) . . . . ? C16 C15 C24 C23 3(3) . . . . ? C14 C15 C24 C23 179.5(16) . . . . ? C16 C15 C24 N11 -177.0(15) . . . . ? C14 C15 C24 N11 -1(2) . . . . ? C22 C23 C24 C15 174.7(17) . . . . ? C18 C23 C24 C15 -4(2) . . . . ? C22 C23 C24 N11 -5(3) . . . . ? C18 C23 C24 N11 176.4(13) . . . . ? C12 N11 C24 C15 -2(2) . . . . ? Ni1 N11 C24 C15 179.2(12) . . . . ? C12 N11 C24 C23 178.2(14) . . . . ? Ni1 N11 C24 C23 -1(2) . . . . ? N11 C12 C25 N25 5(2) . . . . ? C13 C12 C25 N25 177.9(14) . . . . ? C12 C25 N25 C51 -178.5(14) . . . . ? C12 C25 N25 Ni1 -2.5(19) . . . . ? N11 Ni1 N25 C25 0.3(12) . . . . ? Cl2 Ni1 N25 C25 172.0(11) . . . . ? Cl1 Ni1 N25 C25 85.4(12) . . . . ? I3 Ni1 N25 C25 -93.2(11) . . . . ? N11 Ni1 N25 C51 176.1(14) . . . . ? Cl2 Ni1 N25 C51 -12.2(13) . . . . ? Cl1 Ni1 N25 C51 -98.9(13) . . . . ? I3 Ni1 N25 C51 82.6(13) . . . . ? N45 Ni2 N31 C32 3.5(9) . . . . ? Cl2 Ni2 N31 C32 152.8(9) . . . . ? Cl1 Ni2 N31 C32 99.1(8) . . . . ? I4 Ni2 N31 C32 -96.3(8) . . . . ? N45 Ni2 N31 C44 -179.9(12) . . . . ? Cl2 Ni2 N31 C44 -30.6(18) . . . . ? Cl1 Ni2 N31 C44 -84.2(11) . . . . ? I4 Ni2 N31 C44 80.4(11) . . . . ? C44 N31 C32 C33 3(2) . . . . ? Ni2 N31 C32 C33 180.0(12) . . . . ? C44 N31 C32 C45 177.9(12) . . . . ? Ni2 N31 C32 C45 -4.9(15) . . . . ? N31 C32 C33 C34 -4(3) . . . . ? C45 C32 C33 C34 -178.7(17) . . . . ? C32 C33 C34 C35 5(3) . . . . ? C33 C34 C35 C36 175.4(16) . . . . ? C33 C34 C35 C44 -6(2) . . . . ? C44 C35 C36 C37 -2(3) . . . . ? C34 C35 C36 C37 176.7(17) . . . . ? C35 C36 C37 C38 4(3) . . . . ? C36 C37 C38 C39 174(2) . . . . ? C36 C37 C38 C43 -1(2) . . . . ? C43 C38 C39 C40 -2(3) . . . . ? C37 C38 C39 C40 -178.2(17) . . . . ? C38 C39 C40 C41 0(3) . . . . ? C39 C40 C41 C42 1(3) . . . . ? C40 C41 C42 C43 -1(3) . . . . ? C41 C42 C43 C44 179.4(16) . . . . ? C41 C42 C43 C38 -1(2) . . . . ? C39 C38 C43 C42 3(2) . . . . ? C37 C38 C43 C42 178.9(15) . . . . ? C39 C38 C43 C44 -177.7(16) . . . . ? C37 C38 C43 C44 -2(2) . . . . ? C32 N31 C44 C35 -3.8(18) . . . . ? Ni2 N31 C44 C35 180.0(9) . . . . ? C32 N31 C44 C43 -178.5(12) . . . . ? Ni2 N31 C44 C43 5.2(17) . . . . ? C36 C35 C44 N31 -175.8(13) . . . . ? C34 C35 C44 N31 5(2) . . . . ? C36 C35 C44 C43 -2(2) . . . . ? C34 C35 C44 C43 179.6(14) . . . . ? C42 C43 C44 N31 -3(2) . . . . ? C38 C43 C44 N31 177.8(12) . . . . ? C42 C43 C44 C35 -177.3(15) . . . . ? C38 C43 C44 C35 3(2) . . . . ? N31 C32 C45 N45 4(2) . . . . ? C33 C32 C45 N45 178.9(16) . . . . ? C32 C45 N45 C52 -177.4(13) . . . . ? C32 C45 N45 Ni2 -0.6(17) . . . . ? N31 Ni2 N45 C45 -1.6(11) . . . . ? Cl2 Ni2 N45 C45 -172.3(10) . . . . ? Cl1 Ni2 N45 C45 -84.3(11) . . . . ? I4 Ni2 N45 C45 92.6(10) . . . . ? N31 Ni2 N45 C52 174.0(13) . . . . ? Cl2 Ni2 N45 C52 3.4(14) . . . . ? Cl1 Ni2 N45 C52 91.3(13) . . . . ? I4 Ni2 N45 C52 -91.7(13) . . . . ? C25 N25 C51 C52 -78.2(19) . . . . ? Ni1 N25 C51 C52 106.4(13) . . . . ? C25 N25 C51 C56 52.3(19) . . . . ? Ni1 N25 C51 C56 -123.2(11) . . . . ? N25 C51 C52 N45 -56.2(16) . . . . ? C56 C51 C52 N45 177.3(12) . . . . ? N25 C51 C52 C53 -172.6(12) . . . . ? C56 C51 C52 C53 60.8(17) . . . . ? C45 N45 C52 C51 153.9(14) . . . . ? Ni2 N45 C52 C51 -22(2) . . . . ? C45 N45 C52 C53 -87.3(15) . . . . ? Ni2 N45 C52 C53 97.0(16) . . . . ? C51 C52 C53 C54 -47.3(16) . . . . ? N45 C52 C53 C54 -168.6(12) . . . . ? C52 C53 C54 C55 48(2) . . . . ? C53 C54 C55 C56 -52(3) . . . . ? C54 C55 C56 C51 51(2) . . . . ? C52 C51 C56 C55 -61.8(18) . . . . ? N25 C51 C56 C55 169.9(14) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.066 _refine_diff_density_min -1.215 _refine_diff_density_rms 0.153 data_(R,R,R,R)-4 _database_code_depnum_ccdc_archive 'CCDC 846326' #TrackingRef '- output.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; DP-3-1-1 [1-(benzoquinoline imine)-2-amino-cyclohexane]2 Ni (OTf)2 (MeOH) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C20 H19 N3)2 Ni (C F3 O3 S)2 (C2 H6 O) ; _chemical_formula_sum 'C44 H44 F6 N6 Ni O7 S2' _chemical_formula_weight 1005.68 _chemical_absolute_configuration ad 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 12.3347(12) _cell_length_b 12.8896(13) _cell_length_c 17.0469(17) _cell_angle_alpha 86.5080(10) _cell_angle_beta 73.8200(10) _cell_angle_gamma 62.9640(10) _cell_volume 2311.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7001 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.20 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_max 0.46 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.862 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_reflns_number 20473 _diffrn_reflns_av_R_equivalents 0.0097 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.29 _reflns_number_total 17704 _reflns_number_gt 16127 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1500P)^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 0.056(15) _refine_ls_number_reflns 17704 _refine_ls_number_parameters 1172 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0895 _refine_ls_wR_factor_ref 0.2594 _refine_ls_wR_factor_gt 0.2530 _refine_ls_goodness_of_fit_ref 1.501 _refine_ls_restrained_S_all 1.538 _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 O71_1 O 0.9276(9) 0.3641(10) 0.2344(6) 0.022(3) Uiso 0.334(12) 1 d PD A 1 H71A_1 H 0.9709 0.3074 0.2577 0.033 Uiso 0.334(12) 1 calc PR A 1 C71_1 C 1.0051(17) 0.416(2) 0.189(2) 0.096(11) Uiso 0.334(12) 1 d PD A 1 H71B_1 H 1.0731 0.3591 0.1435 0.115 Uiso 0.334(12) 1 calc PR A 1 H71C_1 H 1.0456 0.4336 0.2249 0.115 Uiso 0.334(12) 1 calc PR A 1 C72_1 C 0.9265(15) 0.5271(12) 0.1535(9) 0.030(4) Uiso 0.334(12) 1 d PD A 1 H72A_1 H 0.9762 0.5323 0.0988 0.046 Uiso 0.334(12) 1 calc PR A 1 H72B_1 H 0.9034 0.5949 0.1894 0.046 Uiso 0.334(12) 1 calc PR A 1 H72C_1 H 0.8493 0.5259 0.1497 0.046 Uiso 0.334(12) 1 calc PR A 1 O81_1 O 0.8824(10) 0.1788(10) 0.2485(7) 0.0278(12) Uiso 0.304(7) 1 d PD B 2 H81A_1 H 0.8064 0.2039 0.2767 0.042 Uiso 0.304(7) 1 calc PR B 2 C81_1 C 0.9108(12) 0.2790(11) 0.2258(10) 0.0278(12) Uiso 0.304(7) 1 d PD B 2 H81B_1 H 0.8903 0.3279 0.2755 0.033 Uiso 0.304(7) 1 calc PR B 2 H81C_1 H 0.8597 0.3282 0.1898 0.033 Uiso 0.304(7) 1 calc PR B 2 C82_1 C 1.0543(11) 0.2275(14) 0.1802(9) 0.0278(12) Uiso 0.304(7) 1 d PD B 2 H82A_1 H 1.0659 0.2650 0.1289 0.042 Uiso 0.304(7) 1 calc PR B 2 H82B_1 H 1.0894 0.1432 0.1682 0.042 Uiso 0.304(7) 1 calc PR B 2 H82C_1 H 1.0984 0.2419 0.2148 0.042 Uiso 0.304(7) 1 calc PR B 2 O91_1 O 0.9093(10) 0.3163(9) 0.2257(6) 0.0278(12) Uiso 0.363(10) 1 d PD C 3 H91A_1 H 0.9155 0.2730 0.2648 0.042 Uiso 0.363(10) 1 calc PR C 3 C91_1 C 0.9509(13) 0.3958(11) 0.2352(7) 0.0278(12) Uiso 0.363(10) 1 d PD C 3 H91B_1 H 1.0351 0.3503 0.2449 0.033 Uiso 0.363(10) 1 calc PR C 3 H91C_1 H 0.8933 0.4438 0.2868 0.033 Uiso 0.363(10) 1 calc PR C 3 C92_1 C 0.9648(13) 0.4798(11) 0.1729(8) 0.0278(12) Uiso 0.363(10) 1 d PD C 3 H92A_1 H 1.0279 0.4360 0.1220 0.042 Uiso 0.363(10) 1 calc PR C 3 H92B_1 H 0.9926 0.5298 0.1940 0.042 Uiso 0.363(10) 1 calc PR C 3 H92C_1 H 0.8830 0.5283 0.1619 0.042 Uiso 0.363(10) 1 calc PR C 3 O71_2 O 0.1239(6) 0.7508(5) 0.7554(4) 0.0288(16) Uiso 0.594(11) 1 d PD D 1 H71A_2 H 0.0886 0.8211 0.7734 0.043 Uiso 0.594(11) 1 calc PR D 1 C71_2 C 0.0454(14) 0.6973(11) 0.7946(11) 0.083(5) Uiso 0.594(11) 1 d PD D 1 H71B_2 H -0.0355 0.7401 0.7802 0.099 Uiso 0.594(11) 1 calc PR D 1 H71C_2 H 0.0253 0.7137 0.8543 0.099 Uiso 0.594(11) 1 calc PR D 1 C72_2 C 0.0845(15) 0.5721(10) 0.7812(10) 0.058(4) Uiso 0.594(11) 1 d PD D 1 H72A_2 H 0.0958 0.5536 0.7236 0.087 Uiso 0.594(11) 1 calc PR D 1 H72B_2 H 0.0191 0.5532 0.8163 0.087 Uiso 0.594(11) 1 calc PR D 1 H72C_2 H 0.1648 0.5260 0.7947 0.087 Uiso 0.594(11) 1 calc PR D 1 O81_2 O 0.184(2) 0.849(2) 0.7629(15) 0.0278(12) Uiso 0.138(7) 1 d PD E 2 H81A_2 H 0.1612 0.8770 0.7209 0.042 Uiso 0.138(7) 1 calc PR E 2 C81_2 C 0.094(3) 0.812(3) 0.8128(14) 0.0278(12) Uiso 0.138(7) 1 d PD E 2 H81B_2 H 0.0096 0.8797 0.8318 0.033 Uiso 0.138(7) 1 calc PR E 2 H81C_2 H 0.1217 0.7766 0.8615 0.033 Uiso 0.138(7) 1 calc PR E 2 C82_2 C 0.086(3) 0.720(3) 0.762(2) 0.0278(12) Uiso 0.138(7) 1 d PD E 2 H82A_2 H 0.1691 0.6738 0.7234 0.042 Uiso 0.138(7) 1 calc PR E 2 H82B_2 H 0.0229 0.7607 0.7325 0.042 Uiso 0.138(7) 1 calc PR E 2 H82C_2 H 0.0614 0.6688 0.7995 0.042 Uiso 0.138(7) 1 calc PR E 2 O91_2 O 0.0724(13) 0.5457(13) 0.7964(7) 0.0278(12) Uiso 0.269(8) 1 d PD F 3 H91A_2 H 0.0276 0.5625 0.7640 0.042 Uiso 0.269(8) 1 calc PR F 3 C91_2 C 0.0214(14) 0.4982(16) 0.8661(9) 0.0278(12) Uiso 0.269(8) 1 d PD F 3 H91B_2 H 0.0106 0.4331 0.8473 0.033 Uiso 0.269(8) 1 calc PR F 3 H91C_2 H -0.0635 0.5590 0.8964 0.033 Uiso 0.269(8) 1 calc PR F 3 C92_2 C 0.1051(16) 0.4531(16) 0.9240(9) 0.0278(12) Uiso 0.269(8) 1 d PD F 3 H92A_2 H 0.1858 0.4550 0.8985 0.042 Uiso 0.269(8) 1 calc PR F 3 H92B_2 H 0.1213 0.3727 0.9353 0.042 Uiso 0.269(8) 1 calc PR F 3 H92C_2 H 0.0619 0.5027 0.9755 0.042 Uiso 0.269(8) 1 calc PR F 3 S1 S 0.2849(2) 0.9089(2) 0.54166(13) 0.0589(5) Uani 1 1 d D . . O1 O 0.4140(6) 0.8246(7) 0.5137(5) 0.079(2) Uani 1 1 d . G . O2 O 0.2432(10) 1.0125(10) 0.4977(8) 0.132(4) Uani 1 1 d . G . O3 O 0.2336(10) 0.9352(15) 0.6257(5) 0.160(6) Uani 1 1 d . G . C1A C 0.1964(7) 0.8436(6) 0.5201(4) 0.0595(19) Uiso 0.506(17) 1 d PD G 1 F1A F 0.2411(9) 0.7321(6) 0.5320(7) 0.074(4) Uiso 0.506(17) 1 d PD G 1 F2A F 0.2116(11) 0.8381(11) 0.4408(4) 0.081(4) Uiso 0.506(17) 1 d PD G 1 F3A F 0.0786(6) 0.8921(10) 0.5574(7) 0.085(6) Uiso 0.506(17) 1 d PD G 1 C1B C 0.1964(7) 0.8436(6) 0.5201(4) 0.0595(19) Uiso 0.494(17) 1 d PD G 2 F1B F 0.2033(11) 0.7617(9) 0.5801(7) 0.073(4) Uiso 0.494(17) 1 d PD G 2 F2B F 0.2447(12) 0.7678(12) 0.4621(8) 0.103(5) Uiso 0.494(17) 1 d PD G 2 F3B F 0.0746(5) 0.9071(7) 0.5410(6) 0.039(2) Uiso 0.494(17) 1 d PD G 2 S2 S 0.27963(18) 0.71432(17) 0.99776(12) 0.0568(5) Uani 1 1 d . . . C2 C 0.1216(9) 0.8276(9) 1.0157(6) 0.076(3) Uani 1 1 d . . . O4 O 0.3040(9) 0.6454(8) 0.9287(5) 0.094(2) Uiso 1 1 d . . . O5 O 0.2932(12) 0.6813(11) 1.0756(7) 0.125(3) Uiso 1 1 d . . . O6 O 0.3442(10) 0.7885(9) 0.9753(6) 0.108(3) Uiso 1 1 d . . . F4 F 0.0433(7) 0.7825(14) 1.0293(6) 0.175(6) Uani 1 1 d . . . F5 F 0.0863(7) 0.8888(8) 1.0868(6) 0.132(4) Uani 1 1 d . . . F6 F 0.0942(12) 0.8685(10) 0.9530(9) 0.174(5) Uani 1 1 d . . . S3A S 0.7076(4) 0.0790(4) 0.4668(2) 0.0392(5) Uiso 0.602(7) 1 d P H 1 C3A C 0.8530(11) 0.1026(11) 0.3995(7) 0.049(3) Uiso 0.602(7) 1 d P H 1 O7A O 0.6112(8) 0.1553(7) 0.4448(5) 0.0472(19) Uiso 0.602(7) 1 d P H 1 O8A O 0.7557(9) -0.0366(9) 0.4561(7) 0.058(2) Uiso 0.602(7) 1 d P H 1 O9A O 0.7169(9) 0.1157(8) 0.5488(6) 0.057(2) Uiso 0.602(7) 1 d P H 1 F7A F 0.8161(8) 0.2170(7) 0.3978(5) 0.063(2) Uiso 0.602(7) 1 d P H 1 F8A F 0.8741(7) 0.0584(7) 0.3274(5) 0.0597(19) Uiso 0.602(7) 1 d P H 1 F9A F 0.9514(8) 0.0543(7) 0.4229(5) 0.0530(17) Uiso 0.602(7) 1 d P H 1 S3B S 0.7201(6) 0.0810(5) 0.4736(4) 0.0392(5) Uiso 0.398(7) 1 d PD H 2 C3B C 0.7961(9) 0.1442(9) 0.4907(6) 0.036(3) Uiso 0.398(7) 1 d PD H 2 O7B O 0.7532(9) -0.0334(7) 0.4989(6) 0.037(2) Uiso 0.398(7) 1 d PD H 2 O8B O 0.5819(9) 0.1532(10) 0.5081(7) 0.060(4) Uiso 0.398(7) 1 d PD H 2 O9B O 0.7341(11) 0.0717(10) 0.3848(5) 0.052(3) Uiso 0.398(7) 1 d PD H 2 F7B F 0.7848(8) 0.1481(8) 0.5680(4) 0.045(2) Uiso 0.398(7) 1 d PD H 2 F8B F 0.7580(9) 0.2491(7) 0.4687(6) 0.051(3) Uiso 0.398(7) 1 d PD H 2 F9B F 0.9153(7) 0.0881(8) 0.4532(6) 0.044(2) Uiso 0.398(7) 1 d PD H 2 S4 S 0.74649(19) 0.26505(16) 0.00359(12) 0.0527(5) Uani 1 1 d . . . C4 C 0.9188(10) 0.1940(9) -0.0290(6) 0.073(3) Uani 1 1 d . . . O10 O 0.7120(6) 0.3409(5) 0.0738(4) 0.0654(16) Uani 1 1 d . . . O11 O 0.7150(6) 0.3222(6) -0.0681(4) 0.0749(19) Uani 1 1 d . . . O12 O 0.7200(7) 0.1670(5) 0.0226(3) 0.0691(17) Uani 1 1 d . . . F10 F 0.9614(6) 0.2745(6) -0.0510(5) 0.094(2) Uani 1 1 d . . . F11 F 0.9650(7) 0.1180(6) -0.0901(4) 0.105(2) Uani 1 1 d . . . F12 F 0.9655(7) 0.1466(7) 0.0329(5) 0.107(2) Uani 1 1 d . . . Ni1_1 Ni 0.56074(6) 0.71757(6) 0.72447(6) 0.0446(2) Uani 1 1 d . . . N11_1 N 0.6642(5) 0.7013(5) 0.8351(4) 0.0481(14) Uani 1 1 d . . . C12_1 C 0.6436(7) 0.6223(6) 0.8820(5) 0.0531(18) Uani 1 1 d . . . C13_1 C 0.6556(9) 0.6029(7) 0.9614(5) 0.065(2) Uani 1 1 d . . . H13_1 H 0.6364 0.5458 0.9913 0.078 Uiso 1 1 calc R . . C14_1 C 0.6970(14) 0.6702(9) 0.9962(6) 0.094(4) Uani 1 1 d . . . H14_1 H 0.7125 0.6562 1.0483 0.112 Uiso 1 1 calc R . . C15_1 C 0.7143(10) 0.7590(8) 0.9501(5) 0.073(3) Uani 1 1 d . . . C16_1 C 0.7455(14) 0.8355(10) 0.9846(6) 0.086(3) Uani 1 1 d . . . H16_1 H 0.7539 0.8264 1.0386 0.103 Uiso 1 1 calc R . . C17_1 C 0.7636(14) 0.9213(9) 0.9421(6) 0.091(4) Uani 1 1 d . . . H17_1 H 0.7774 0.9761 0.9675 0.109 Uiso 1 1 calc R . . C18_1 C 0.7615(10) 0.9286(8) 0.8563(5) 0.064(2) Uani 1 1 d . . . C19_1 C 0.7921(9) 1.0102(8) 0.8071(6) 0.068(2) Uani 1 1 d . . . H19_1 H 0.8069 1.0641 0.8326 0.081 Uiso 1 1 calc R . . C20_1 C 0.8010(8) 1.0152(7) 0.7283(6) 0.062(2) Uani 1 1 d . . . H20_1 H 0.8167 1.0742 0.6988 0.075 Uiso 1 1 calc R . . C21_1 C 0.7866(6) 0.9307(6) 0.6883(6) 0.0532(19) Uani 1 1 d . . . H21_1 H 0.7984 0.9301 0.6308 0.064 Uiso 1 1 calc R . . C22_1 C 0.7556(6) 0.8489(6) 0.7322(5) 0.0455(15) Uani 1 1 d . . . H22_1 H 0.7452 0.7932 0.7051 0.055 Uiso 1 1 calc R . . C23_1 C 0.7393(7) 0.8493(6) 0.8192(5) 0.0512(17) Uani 1 1 d . . . C24_1 C 0.7046(7) 0.7681(6) 0.8692(5) 0.0542(18) Uani 1 1 d . . . C25_1 C 0.5940(7) 0.5533(6) 0.8467(6) 0.057(2) Uani 1 1 d . . . H25_1 H 0.5848 0.4907 0.8751 0.068 Uiso 1 1 calc R . . C31_1 C 0.5080(6) 0.5149(6) 0.7507(5) 0.0517(18) Uani 1 1 d . . . H31_1 H 0.4178 0.5449 0.7847 0.062 Uiso 1 1 calc R . . N31_1 N 0.5651(5) 0.5770(5) 0.7813(4) 0.0457(14) Uani 1 1 d . . . C32_1 C 0.5082(7) 0.5470(6) 0.6604(7) 0.062(2) Uani 1 1 d . . . H32_1 H 0.5974 0.5077 0.6243 0.074 Uiso 1 1 calc R . . N32_1 N 0.4605(7) 0.6772(6) 0.6607(6) 0.069(2) Uani 1 1 d . . . C33_1 C 0.4309(8) 0.5023(8) 0.6331(8) 0.073(3) Uani 1 1 d . . . H33A_1 H 0.4274 0.5240 0.5768 0.087 Uiso 1 1 calc R . . H33B_1 H 0.3432 0.5374 0.6698 0.087 Uiso 1 1 calc R . . C34_1 C 0.4933(9) 0.3673(8) 0.6351(8) 0.077(3) Uani 1 1 d . . . H34A_1 H 0.4422 0.3366 0.6181 0.093 Uiso 1 1 calc R . . H34B_1 H 0.5793 0.3325 0.5961 0.093 Uiso 1 1 calc R . . C35_1 C 0.5021(9) 0.3327(8) 0.7216(8) 0.078(3) Uani 1 1 d . . . H35A_1 H 0.5447 0.2464 0.7208 0.094 Uiso 1 1 calc R . . H35B_1 H 0.4152 0.3614 0.7590 0.094 Uiso 1 1 calc R . . C36_1 C 0.5758(9) 0.3815(6) 0.7560(7) 0.071(3) Uani 1 1 d . . . H36A_1 H 0.5727 0.3624 0.8135 0.085 Uiso 1 1 calc R . . H36B_1 H 0.6657 0.3481 0.7228 0.085 Uiso 1 1 calc R . . N41_1 N 0.7286(5) 0.6476(5) 0.6080(4) 0.0425(12) Uani 1 1 d . . . C42_1 C 0.7021(6) 0.7309(6) 0.5542(4) 0.0414(14) Uani 1 1 d . . . C43_1 C 0.7480(7) 0.7115(6) 0.4701(5) 0.0499(18) Uani 1 1 d . . . H43_1 H 0.7284 0.7753 0.4365 0.060 Uiso 1 1 calc R . . C44_1 C 0.8225(6) 0.5989(7) 0.4351(5) 0.0499(16) Uani 1 1 d . . . H44_1 H 0.8511 0.5833 0.3772 0.060 Uiso 1 1 calc R . . C45_1 C 0.8555(7) 0.5063(6) 0.4878(5) 0.0484(16) Uani 1 1 d . . . C46_1 C 0.9275(7) 0.3850(7) 0.4571(5) 0.0497(16) Uani 1 1 d . . . H46_1 H 0.9546 0.3649 0.3998 0.060 Uiso 1 1 calc R . . C47_1 C 0.9556(6) 0.3026(6) 0.5078(5) 0.0533(18) Uani 1 1 d . . . H47_1 H 0.9944 0.2234 0.4869 0.064 Uiso 1 1 calc R . . C48_1 C 0.9297(6) 0.3280(6) 0.5935(5) 0.0448(15) Uani 1 1 d . . . C49_1 C 0.9714(6) 0.2380(7) 0.6446(5) 0.0545(19) Uani 1 1 d . . . H49_1 H 1.0079 0.1591 0.6237 0.065 Uiso 1 1 calc R . . C50_1 C 0.9603(6) 0.2620(6) 0.7245(5) 0.0496(17) Uani 1 1 d . . . H50_1 H 0.9895 0.1998 0.7584 0.060 Uiso 1 1 calc R . . C51_1 C 0.9060(6) 0.3781(6) 0.7564(5) 0.0499(17) Uani 1 1 d . . . H51_1 H 0.9032 0.3946 0.8107 0.060 Uiso 1 1 calc R . . C52_1 C 0.8562(5) 0.4686(6) 0.7082(4) 0.0395(13) Uani 1 1 d . . . H52_1 H 0.8171 0.5472 0.7303 0.047 Uiso 1 1 calc R . . C53_1 C 0.8633(6) 0.4446(6) 0.6260(5) 0.0431(15) Uani 1 1 d . . . C54_1 C 0.8137(6) 0.5346(6) 0.5745(4) 0.0403(14) Uani 1 1 d . . . C55_1 C 0.6046(7) 0.8487(6) 0.5886(5) 0.0485(18) Uani 1 1 d . . . H55_1 H 0.5890 0.9139 0.5563 0.058 Uiso 1 1 calc R . . C61_1 C 0.4285(6) 0.9677(6) 0.7031(6) 0.0525(19) Uani 1 1 d . . . H61_1 H 0.3567 0.9705 0.6852 0.063 Uiso 1 1 calc R . . N61_1 N 0.5404(5) 0.8603(5) 0.6652(4) 0.0462(14) Uani 1 1 d . . . C62_1 C 0.3991(6) 0.9549(6) 0.7948(7) 0.064(2) Uani 1 1 d . . . H62_1 H 0.4681 0.9547 0.8148 0.077 Uiso 1 1 calc R . . N62_1 N 0.3979(6) 0.8402(5) 0.8079(6) 0.073(3) Uani 1 1 d . . . C63_1 C 0.2718(7) 1.0557(6) 0.8412(8) 0.074(3) Uani 1 1 d . . . H63A_1 H 0.2576 1.0496 0.9010 0.089 Uiso 1 1 calc R . . H63B_1 H 0.2014 1.0528 0.8260 0.089 Uiso 1 1 calc R . . C64_1 C 0.2775(7) 1.1747(7) 0.8168(7) 0.067(2) Uani 1 1 d . . . H64A_1 H 0.1944 1.2412 0.8435 0.081 Uiso 1 1 calc R . . H64B_1 H 0.3423 1.1798 0.8376 0.081 Uiso 1 1 calc R . . C65_1 C 0.3083(7) 1.1849(7) 0.7269(6) 0.060(2) Uani 1 1 d . . . H65A_1 H 0.3116 1.2598 0.7153 0.072 Uiso 1 1 calc R . . H65B_1 H 0.2403 1.1857 0.7065 0.072 Uiso 1 1 calc R . . C66_1 C 0.4372(7) 1.0827(6) 0.6805(7) 0.059(2) Uani 1 1 d . . . H66A_1 H 0.5073 1.0841 0.6972 0.071 Uiso 1 1 calc R . . H66B_1 H 0.4532 1.0894 0.6207 0.071 Uiso 1 1 calc R . . Ni2_2 Ni 0.43402(5) 1.28978(5) 0.27577(4) 0.03183(18) Uani 1 1 d . . . N11_2 N 0.3655(5) 1.2885(5) 0.1608(3) 0.0380(11) Uani 1 1 d . . . C12_2 C 0.3964(6) 1.3632(6) 0.1124(4) 0.0411(14) Uani 1 1 d . . . C13_2 C 0.4218(9) 1.3550(8) 0.0276(5) 0.060(2) Uani 1 1 d . . . H13_2 H 0.4305 1.4158 -0.0035 0.072 Uiso 1 1 calc R . . C14_2 C 0.4341(14) 1.2571(11) -0.0107(5) 0.086(4) Uani 1 1 d . . . H14_2 H 0.4652 1.2422 -0.0685 0.103 Uiso 1 1 calc R . . C15_2 C 0.3997(13) 1.1827(10) 0.0381(5) 0.081(3) Uani 1 1 d . . . C16_2 C 0.4184(14) 1.0740(12) 0.0011(6) 0.092(4) Uani 1 1 d . . . H16_2 H 0.4592 1.0537 -0.0558 0.110 Uiso 1 1 calc R . . C17_2 C 0.3787(13) 1.0034(9) 0.0466(6) 0.082(3) Uani 1 1 d . . . H17_2 H 0.3880 0.9354 0.0208 0.098 Uiso 1 1 calc R . . C18_2 C 0.3212(8) 1.0277(6) 0.1350(5) 0.0500(16) Uani 1 1 d . . . C19_2 C 0.2741(8) 0.9585(6) 0.1815(5) 0.0488(16) Uani 1 1 d . . . H19_2 H 0.2818 0.8911 0.1558 0.059 Uiso 1 1 calc R . . C20_2 C 0.2167(8) 0.9842(7) 0.2636(5) 0.0509(17) Uani 1 1 d . . . H20_2 H 0.1903 0.9320 0.2949 0.061 Uiso 1 1 calc R . . C21_2 C 0.1970(8) 1.0844(9) 0.3010(5) 0.062(2) Uani 1 1 d . . . H21_2 H 0.1538 1.1040 0.3577 0.074 Uiso 1 1 calc R . . C22_2 C 0.2414(6) 1.1579(6) 0.2547(4) 0.0386(13) Uani 1 1 d . . . H22_2 H 0.2261 1.2286 0.2804 0.046 Uiso 1 1 calc R . . C23_2 C 0.3073(6) 1.1298(6) 0.1724(4) 0.0404(13) Uani 1 1 d . . . C24_2 C 0.3569(6) 1.2020(6) 0.1243(4) 0.0411(13) Uani 1 1 d . . . C25_2 C 0.4136(6) 1.4498(5) 0.1536(4) 0.0392(13) Uani 1 1 d . . . H25_2 H 0.4184 1.5144 0.1259 0.047 Uiso 1 1 calc R . . C31_2 C 0.4429(5) 1.5138(6) 0.2706(4) 0.0366(12) Uani 1 1 d . . . H31_2 H 0.3618 1.5591 0.3141 0.044 Uiso 1 1 calc R . . N31_2 N 0.4218(4) 1.4370(5) 0.2252(3) 0.0329(10) Uani 1 1 d . . . C32_2 C 0.5413(6) 1.4367(6) 0.3143(4) 0.0374(12) Uani 1 1 d . . . H32_2 H 0.6246 1.3946 0.2719 0.045 Uiso 1 1 calc R . . N32_2 N 0.5042(6) 1.3493(6) 0.3549(3) 0.0491(15) Uani 1 1 d . . . C33_2 C 0.5567(8) 1.5111(7) 0.3727(5) 0.0482(16) Uani 1 1 d . . . H33A_2 H 0.6250 1.4606 0.3976 0.058 Uiso 1 1 calc R . . H33B_2 H 0.4769 1.5501 0.4174 0.058 Uiso 1 1 calc R . . C34_2 C 0.5899(7) 1.6046(6) 0.3255(5) 0.0511(16) Uani 1 1 d . . . H34A_2 H 0.5938 1.6556 0.3647 0.061 Uiso 1 1 calc R . . H34B_2 H 0.6749 1.5650 0.2856 0.061 Uiso 1 1 calc R . . C35_2 C 0.4969(8) 1.6773(7) 0.2817(5) 0.0527(17) Uani 1 1 d . . . H35A_2 H 0.5257 1.7313 0.2495 0.063 Uiso 1 1 calc R . . H35B_2 H 0.4143 1.7250 0.3220 0.063 Uiso 1 1 calc R . . C36_2 C 0.4792(6) 1.6022(6) 0.2233(5) 0.0433(14) Uani 1 1 d . . . H36A_2 H 0.4120 1.6533 0.1978 0.052 Uiso 1 1 calc R . . H36B_2 H 0.5591 1.5610 0.1791 0.052 Uiso 1 1 calc R . . N41_2 N 0.2582(5) 1.3428(6) 0.3934(3) 0.0413(12) Uani 1 1 d . . . C42_2 C 0.2965(7) 1.2474(7) 0.4370(4) 0.0451(16) Uani 1 1 d . . . C43_2 C 0.2527(7) 1.2557(8) 0.5230(4) 0.0498(18) Uani 1 1 d . . . H43_2 H 0.2744 1.1882 0.5531 0.060 Uiso 1 1 calc R . . C44_2 C 0.1768(8) 1.3666(10) 0.5617(5) 0.068(3) Uani 1 1 d . . . H44_2 H 0.1500 1.3749 0.6199 0.082 Uiso 1 1 calc R . . C45_2 C 0.1379(7) 1.4666(8) 0.5190(4) 0.0514(18) Uani 1 1 d . . . C46_2 C 0.0620(7) 1.5829(9) 0.5573(5) 0.061(2) Uani 1 1 d . . . H46_2 H 0.0343 1.5950 0.6153 0.074 Uiso 1 1 calc R . . C47_2 C 0.0293(9) 1.6762(9) 0.5110(6) 0.068(3) Uani 1 1 d . . . H47_2 H -0.0194 1.7524 0.5380 0.081 Uiso 1 1 calc R . . C48_2 C 0.0642(8) 1.6646(8) 0.4253(6) 0.059(2) Uani 1 1 d . . . C49_2 C 0.0339(9) 1.7581(9) 0.3777(7) 0.067(2) Uani 1 1 d . . . H49_2 H -0.0081 1.8348 0.4038 0.081 Uiso 1 1 calc R . . C50_2 C 0.0606(8) 1.7457(8) 0.2977(8) 0.074(3) Uani 1 1 d . . . H50_2 H 0.0448 1.8129 0.2674 0.089 Uiso 1 1 calc R . . C51_2 C 0.1129(7) 1.6337(8) 0.2546(6) 0.0580(19) Uani 1 1 d . . . H51_2 H 0.1259 1.6248 0.1973 0.070 Uiso 1 1 calc R . . C52_2 C 0.1432(6) 1.5391(7) 0.3026(5) 0.0511(17) Uani 1 1 d . . . H52_2 H 0.1760 1.4634 0.2769 0.061 Uiso 1 1 calc R . . C53_2 C 0.1286(7) 1.5487(7) 0.3848(5) 0.0508(17) Uani 1 1 d . . . C54_2 C 0.1755(6) 1.4493(7) 0.4324(4) 0.0465(16) Uani 1 1 d . . . C55_2 C 0.3923(6) 1.1349(6) 0.3938(4) 0.0397(13) Uani 1 1 d . . . H55_2 H 0.4087 1.0634 0.4188 0.048 Uiso 1 1 calc R . . C61_2 C 0.5529(5) 1.0365(5) 0.2671(4) 0.0332(11) Uani 1 1 d . . . H61_2 H 0.5223 1.0295 0.2202 0.040 Uiso 1 1 calc R . . N61_2 N 0.4527(5) 1.1386(5) 0.3202(3) 0.0344(10) Uani 1 1 d . . . C62_2 C 0.6651(6) 1.0644(6) 0.2326(5) 0.0467(15) Uani 1 1 d . . . H62_2 H 0.6955 1.0704 0.2800 0.056 Uiso 1 1 calc R . . N62_2 N 0.6160(5) 1.1837(5) 0.2001(4) 0.0410(12) Uani 1 1 d . . . C63_2 C 0.7724(7) 0.9709(7) 0.1745(8) 0.079(3) Uani 1 1 d . . . H63A_2 H 0.8459 0.9878 0.1609 0.095 Uiso 1 1 calc R . . H63B_2 H 0.7495 0.9706 0.1233 0.095 Uiso 1 1 calc R . . C64_2 C 0.8109(8) 0.8516(8) 0.2064(10) 0.104(5) Uani 1 1 d . . . H64A_2 H 0.8533 0.8458 0.2491 0.125 Uiso 1 1 calc R . . H64B_2 H 0.8733 0.7921 0.1611 0.125 Uiso 1 1 calc R . . C65_2 C 0.6990(7) 0.8238(7) 0.2427(7) 0.064(2) Uani 1 1 d . . . H65A_2 H 0.6656 0.8154 0.1983 0.077 Uiso 1 1 calc R . . H65B_2 H 0.7288 0.7487 0.2685 0.077 Uiso 1 1 calc R . . C66_2 C 0.5940(7) 0.9198(6) 0.3060(4) 0.0442(15) Uani 1 1 d . . . H66A_2 H 0.6247 0.9237 0.3531 0.053 Uiso 1 1 calc R . . H66B_2 H 0.5208 0.9027 0.3265 0.053 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 S1 0.0712(12) 0.0724(13) 0.0622(11) 0.0054(10) -0.0146(9) -0.0595(11) O1 0.053(3) 0.099(5) 0.101(5) -0.005(4) -0.026(3) -0.045(3) O2 0.111(7) 0.137(9) 0.178(10) 0.086(8) -0.036(7) -0.095(7) O3 0.121(8) 0.349(19) 0.062(4) -0.046(7) 0.005(4) -0.161(11) S2 0.0447(9) 0.0479(10) 0.0487(9) 0.0088(8) -0.0051(7) -0.0021(7) C2 0.053(5) 0.062(5) 0.073(6) 0.007(5) -0.001(4) -0.002(4) F4 0.058(4) 0.343(16) 0.112(6) -0.110(9) 0.022(4) -0.093(7) F5 0.066(4) 0.139(7) 0.153(7) -0.094(6) 0.029(4) -0.036(4) F6 0.147(9) 0.127(8) 0.206(12) 0.019(8) -0.117(10) 0.010(6) S4 0.0658(11) 0.0352(8) 0.0487(9) 0.0061(7) 0.0062(8) -0.0290(8) C4 0.072(6) 0.054(5) 0.072(6) 0.000(4) 0.012(5) -0.028(4) O10 0.076(4) 0.044(3) 0.068(3) -0.020(3) 0.016(3) -0.038(3) O11 0.065(3) 0.077(4) 0.073(4) 0.036(3) -0.013(3) -0.031(3) O12 0.105(5) 0.052(3) 0.055(3) 0.001(3) 0.008(3) -0.056(3) F10 0.074(4) 0.095(5) 0.111(5) 0.014(4) 0.002(3) -0.053(3) F11 0.088(4) 0.072(4) 0.094(4) -0.010(3) 0.022(4) -0.012(3) F12 0.081(4) 0.083(4) 0.117(6) 0.016(4) -0.025(4) -0.007(3) Ni1_1 0.0307(4) 0.0280(4) 0.0772(6) 0.0110(4) -0.0088(4) -0.0197(3) N11_1 0.046(3) 0.027(2) 0.060(3) 0.005(2) 0.008(2) -0.020(2) C12_1 0.043(3) 0.033(3) 0.071(5) 0.009(3) 0.004(3) -0.020(3) C13_1 0.084(6) 0.038(4) 0.058(5) -0.001(3) 0.018(4) -0.035(4) C14_1 0.145(10) 0.058(5) 0.054(5) -0.004(4) 0.024(6) -0.055(6) C15_1 0.099(7) 0.045(4) 0.056(5) -0.011(4) 0.026(4) -0.042(4) C16_1 0.144(10) 0.072(6) 0.055(5) -0.001(4) -0.009(6) -0.071(7) C17_1 0.151(11) 0.061(5) 0.064(5) -0.015(5) 0.015(6) -0.074(7) C18_1 0.086(6) 0.047(4) 0.054(4) -0.001(3) 0.004(4) -0.040(4) C19_1 0.074(5) 0.048(4) 0.082(6) 0.000(4) 0.003(4) -0.042(4) C20_1 0.059(4) 0.048(4) 0.092(6) 0.028(4) -0.012(4) -0.042(4) C21_1 0.037(3) 0.043(4) 0.091(6) 0.028(4) -0.023(3) -0.028(3) C22_1 0.043(3) 0.035(3) 0.063(4) 0.016(3) -0.017(3) -0.022(3) C23_1 0.054(4) 0.037(3) 0.061(4) 0.008(3) 0.000(3) -0.029(3) C24_1 0.050(4) 0.033(3) 0.067(5) 0.003(3) 0.007(3) -0.021(3) C25_1 0.039(3) 0.029(3) 0.086(6) -0.002(4) 0.016(4) -0.020(3) C31_1 0.036(3) 0.031(3) 0.087(5) 0.005(3) -0.001(3) -0.025(3) N31_1 0.037(3) 0.027(3) 0.069(4) 0.010(3) -0.002(3) -0.019(2) C32_1 0.045(4) 0.033(3) 0.114(7) 0.019(4) -0.020(4) -0.026(3) N32_1 0.054(3) 0.037(3) 0.136(7) 0.020(4) -0.038(4) -0.032(3) C33_1 0.054(4) 0.050(5) 0.128(9) 0.017(5) -0.024(5) -0.037(4) C34_1 0.063(5) 0.048(4) 0.138(9) 0.007(5) -0.023(5) -0.042(4) C35_1 0.057(5) 0.038(4) 0.144(10) 0.004(5) -0.017(5) -0.030(4) C36_1 0.062(5) 0.026(3) 0.101(7) -0.005(4) 0.012(4) -0.018(3) N41_1 0.036(2) 0.041(3) 0.063(3) 0.010(2) -0.017(2) -0.026(2) C42_1 0.039(3) 0.039(3) 0.061(4) 0.005(3) -0.020(3) -0.027(3) C43_1 0.049(3) 0.045(4) 0.079(5) 0.027(4) -0.040(4) -0.032(3) C44_1 0.043(3) 0.065(5) 0.058(4) 0.003(3) -0.025(3) -0.032(3) C45_1 0.045(3) 0.043(3) 0.077(5) 0.014(3) -0.027(3) -0.032(3) C46_1 0.046(3) 0.058(4) 0.053(4) 0.003(3) -0.009(3) -0.033(3) C47_1 0.038(3) 0.039(3) 0.084(5) -0.007(4) -0.001(3) -0.028(3) C48_1 0.037(3) 0.035(3) 0.055(4) -0.003(3) 0.007(3) -0.021(3) C49_1 0.032(3) 0.039(3) 0.077(5) 0.003(3) 0.007(3) -0.015(3) C50_1 0.031(3) 0.038(3) 0.064(4) 0.022(3) 0.000(3) -0.013(2) C51_1 0.041(3) 0.044(4) 0.053(4) 0.020(3) 0.001(3) -0.019(3) C52_1 0.031(3) 0.036(3) 0.044(3) 0.005(3) 0.004(2) -0.017(2) C53_1 0.029(3) 0.040(3) 0.062(4) 0.011(3) -0.002(3) -0.024(2) C54_1 0.038(3) 0.036(3) 0.058(4) 0.013(3) -0.013(3) -0.027(2) C55_1 0.048(3) 0.040(3) 0.079(5) 0.026(3) -0.031(4) -0.034(3) C61_1 0.034(3) 0.034(3) 0.106(6) 0.017(4) -0.027(3) -0.026(3) N61_1 0.034(3) 0.036(3) 0.081(4) 0.013(3) -0.025(3) -0.023(2) C62_1 0.031(3) 0.027(3) 0.127(8) 0.020(4) -0.008(4) -0.016(2) N62_1 0.035(3) 0.027(3) 0.138(7) 0.006(4) 0.012(3) -0.018(2) C63_1 0.036(3) 0.028(3) 0.136(9) 0.002(4) -0.001(4) -0.009(3) C64_1 0.043(4) 0.032(3) 0.119(8) 0.010(4) -0.015(4) -0.015(3) C65_1 0.048(4) 0.034(3) 0.103(7) 0.014(4) -0.030(4) -0.019(3) C66_1 0.037(3) 0.035(3) 0.117(7) 0.023(4) -0.030(4) -0.023(3) Ni2_2 0.0337(3) 0.0371(4) 0.0339(3) 0.0053(3) -0.0085(3) -0.0247(3) N11_2 0.043(3) 0.039(3) 0.041(3) 0.012(2) -0.023(2) -0.021(2) C12_2 0.051(3) 0.043(3) 0.046(3) 0.017(3) -0.027(3) -0.029(3) C13_2 0.097(6) 0.071(5) 0.055(4) 0.031(4) -0.045(4) -0.064(5) C14_2 0.169(11) 0.117(9) 0.043(4) 0.024(5) -0.041(6) -0.120(9) C15_2 0.150(10) 0.101(8) 0.050(4) 0.011(5) -0.038(5) -0.101(8) C16_2 0.150(11) 0.115(9) 0.049(4) -0.018(5) 0.001(5) -0.106(9) C17_2 0.149(10) 0.071(6) 0.057(5) 0.002(4) -0.024(6) -0.080(7) C18_2 0.069(4) 0.044(4) 0.058(4) 0.007(3) -0.028(4) -0.038(3) C19_2 0.068(4) 0.044(4) 0.054(4) 0.010(3) -0.030(3) -0.036(3) C20_2 0.065(4) 0.048(4) 0.066(4) 0.011(3) -0.025(4) -0.044(4) C21_2 0.068(5) 0.090(6) 0.052(4) 0.003(4) -0.004(4) -0.064(5) C22_2 0.039(3) 0.042(3) 0.047(3) 0.008(3) -0.013(2) -0.029(3) C23_2 0.047(3) 0.036(3) 0.052(4) 0.011(3) -0.027(3) -0.024(3) C24_2 0.052(3) 0.044(3) 0.043(3) 0.009(3) -0.027(3) -0.028(3) C25_2 0.041(3) 0.031(3) 0.056(4) 0.012(3) -0.021(3) -0.022(2) C31_2 0.033(3) 0.040(3) 0.040(3) -0.003(2) -0.003(2) -0.023(2) N31_2 0.029(2) 0.038(3) 0.039(3) 0.009(2) -0.0091(19) -0.023(2) C32_2 0.049(3) 0.046(3) 0.038(3) 0.011(3) -0.016(2) -0.037(3) N32_2 0.078(4) 0.070(4) 0.036(3) 0.018(3) -0.019(3) -0.064(4) C33_2 0.063(4) 0.055(4) 0.051(4) 0.005(3) -0.023(3) -0.044(4) C34_2 0.056(4) 0.043(4) 0.076(5) 0.004(3) -0.021(3) -0.039(3) C35_2 0.063(4) 0.037(3) 0.074(5) 0.003(3) -0.029(4) -0.030(3) C36_2 0.044(3) 0.033(3) 0.062(4) 0.004(3) -0.022(3) -0.020(3) N41_2 0.049(3) 0.058(3) 0.037(3) 0.006(2) -0.008(2) -0.044(3) C42_2 0.057(4) 0.066(5) 0.037(3) 0.003(3) -0.007(3) -0.051(4) C43_2 0.061(4) 0.078(5) 0.031(3) 0.004(3) 0.000(3) -0.056(4) C44_2 0.064(5) 0.124(9) 0.040(4) -0.015(5) 0.006(3) -0.072(6) C45_2 0.050(4) 0.072(5) 0.045(4) -0.008(4) 0.005(3) -0.047(4) C46_2 0.052(4) 0.084(6) 0.054(4) -0.025(4) 0.011(3) -0.047(4) C47_2 0.072(5) 0.069(6) 0.078(6) -0.022(5) 0.012(4) -0.061(5) C48_2 0.049(4) 0.067(5) 0.076(5) -0.008(4) -0.003(4) -0.046(4) C49_2 0.059(5) 0.061(5) 0.095(7) -0.012(5) -0.007(4) -0.043(4) C50_2 0.052(4) 0.046(4) 0.139(10) 0.002(5) -0.036(5) -0.030(4) C51_2 0.040(3) 0.057(4) 0.076(5) 0.008(4) -0.014(3) -0.023(3) C52_2 0.035(3) 0.044(4) 0.072(5) -0.004(3) -0.009(3) -0.019(3) C53_2 0.042(3) 0.052(4) 0.068(5) -0.005(3) 0.002(3) -0.038(3) C54_2 0.042(3) 0.062(4) 0.050(4) -0.014(3) 0.005(3) -0.044(3) C55_2 0.055(4) 0.049(4) 0.036(3) 0.009(3) -0.015(3) -0.040(3) C61_2 0.033(3) 0.036(3) 0.044(3) 0.016(2) -0.019(2) -0.024(2) N61_2 0.042(3) 0.041(3) 0.036(2) 0.006(2) -0.011(2) -0.033(2) C62_2 0.037(3) 0.043(3) 0.071(4) 0.026(3) -0.021(3) -0.027(3) N62_2 0.034(2) 0.033(3) 0.061(3) 0.013(2) -0.011(2) -0.021(2) C63_2 0.036(3) 0.041(4) 0.137(9) 0.024(5) 0.008(4) -0.018(3) C64_2 0.037(4) 0.040(4) 0.214(15) 0.045(6) -0.010(6) -0.018(3) C65_2 0.048(4) 0.044(4) 0.105(7) 0.031(4) -0.023(4) -0.027(3) C66_2 0.065(4) 0.048(4) 0.047(3) 0.025(3) -0.031(3) -0.041(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 O71_1 C71_1 1.435(10) . ? O71_1 H71A_1 0.8400 . ? C71_1 C72_1 1.522(10) . ? C71_1 H71B_1 0.9900 . ? C71_1 H71C_1 0.9900 . ? C72_1 H72A_1 0.9800 . ? C72_1 H72B_1 0.9800 . ? C72_1 H72C_1 0.9800 . ? O81_1 C81_1 1.489(10) . ? O81_1 H81A_1 0.8400 . ? C81_1 C82_1 1.551(9) . ? C81_1 H81B_1 0.9900 . ? C81_1 H81C_1 0.9900 . ? C82_1 H82A_1 0.9800 . ? C82_1 H82B_1 0.9800 . ? C82_1 H82C_1 0.9800 . ? O91_1 C91_1 1.372(9) . ? O91_1 H91A_1 0.8400 . ? C91_1 C92_1 1.503(9) . ? C91_1 H91B_1 0.9900 . ? C91_1 H91C_1 0.9900 . ? C92_1 H92A_1 0.9800 . ? C92_1 H92B_1 0.9800 . ? C92_1 H92C_1 0.9800 . ? O71_2 C71_2 1.432(9) . ? O71_2 H71A_2 0.8400 . ? C71_2 C72_2 1.472(9) . ? C71_2 H71B_2 0.9900 . ? C71_2 H71C_2 0.9900 . ? C72_2 H72A_2 0.9800 . ? C72_2 H72B_2 0.9800 . ? C72_2 H72C_2 0.9800 . ? O81_2 C81_2 1.443(10) . ? O81_2 H81A_2 0.8400 . ? C81_2 C82_2 1.552(10) . ? C81_2 H81B_2 0.9900 . ? C81_2 H81C_2 0.9900 . ? C82_2 H82A_2 0.9800 . ? C82_2 H82B_2 0.9800 . ? C82_2 H82C_2 0.9800 . ? O91_2 C91_2 1.423(10) . ? O91_2 H91A_2 0.8400 . ? C91_2 C92_2 1.528(9) . ? C91_2 H91B_2 0.9900 . ? C91_2 H91C_2 0.9900 . ? C92_2 H92A_2 0.9800 . ? C92_2 H92B_2 0.9800 . ? C92_2 H92C_2 0.9800 . ? S1 O3 1.388(8) . ? S1 O1 1.418(7) . ? S1 O2 1.441(10) . ? S1 C1A 1.771(8) . ? C1A F3A 1.270(7) . ? C1A F1A 1.310(7) . ? C1A F2A 1.313(7) . ? S2 O4 1.397(9) . ? S2 O5 1.400(12) . ? S2 O6 1.475(11) . ? S2 C2 1.778(9) . ? C2 F6 1.227(15) . ? C2 F4 1.302(16) . ? C2 F5 1.339(13) . ? S3A O7A 1.290(9) . ? S3A O8A 1.333(11) . ? S3A O9A 1.553(10) . ? S3A C3A 1.983(13) . ? C3A F9A 1.254(14) . ? C3A F8A 1.294(14) . ? C3A F7A 1.332(15) . ? S3B O7B 1.414(8) . ? S3B O8B 1.478(8) . ? S3B O9B 1.481(8) . ? S3B C3B 1.582(13) . ? C3B F8B 1.284(9) . ? C3B F7B 1.287(9) . ? C3B F9B 1.288(9) . ? S4 O10 1.432(6) . ? S4 O12 1.441(5) . ? S4 O11 1.443(7) . ? S4 C4 1.816(11) . ? C4 F11 1.287(12) . ? C4 F12 1.326(13) . ? C4 F10 1.354(12) . ? Ni1_1 N31_1 1.988(6) . ? Ni1_1 N61_1 1.991(6) . ? Ni1_1 N62_1 2.086(7) . ? Ni1_1 N32_1 2.093(8) . ? Ni1_1 N41_1 2.296(6) . ? Ni1_1 N11_1 2.505(7) . ? N11_1 C12_1 1.328(9) . ? N11_1 C24_1 1.394(11) . ? C12_1 C13_1 1.398(13) . ? C12_1 C25_1 1.514(12) . ? C13_1 C14_1 1.414(17) . ? C13_1 H13_1 0.9500 . ? C14_1 C15_1 1.412(12) . ? C14_1 H14_1 0.9500 . ? C15_1 C24_1 1.410(14) . ? C15_1 C16_1 1.416(14) . ? C16_1 C17_1 1.355(13) . ? C16_1 H16_1 0.9500 . ? C17_1 C18_1 1.466(14) . ? C17_1 H17_1 0.9500 . ? C18_1 C23_1 1.396(12) . ? C18_1 C19_1 1.424(11) . ? C19_1 C20_1 1.317(14) . ? C19_1 H19_1 0.9500 . ? C20_1 C21_1 1.420(13) . ? C20_1 H20_1 0.9500 . ? C21_1 C22_1 1.389(9) . ? C21_1 H21_1 0.9500 . ? C22_1 C23_1 1.440(11) . ? C22_1 H22_1 0.9500 . ? C23_1 C24_1 1.449(9) . ? C25_1 N31_1 1.243(12) . ? C25_1 H25_1 0.9500 . ? C31_1 N31_1 1.476(10) . ? C31_1 C36_1 1.543(10) . ? C31_1 C32_1 1.568(13) . ? C31_1 H31_1 1.0000 . ? C32_1 C33_1 1.496(12) . ? C32_1 N32_1 1.505(9) . ? C32_1 H32_1 1.0000 . ? C33_1 C34_1 1.553(12) . ? C33_1 H33A_1 0.9900 . ? C33_1 H33B_1 0.9900 . ? C34_1 C35_1 1.532(17) . ? C34_1 H34A_1 0.9900 . ? C34_1 H34B_1 0.9900 . ? C35_1 C36_1 1.558(14) . ? C35_1 H35A_1 0.9900 . ? C35_1 H35B_1 0.9900 . ? C36_1 H36A_1 0.9900 . ? C36_1 H36B_1 0.9900 . ? N41_1 C42_1 1.352(9) . ? N41_1 C54_1 1.388(9) . ? C42_1 C43_1 1.379(11) . ? C42_1 C55_1 1.466(10) . ? C43_1 C44_1 1.376(11) . ? C43_1 H43_1 0.9500 . ? C44_1 C45_1 1.425(10) . ? C44_1 H44_1 0.9500 . ? C45_1 C54_1 1.433(11) . ? C45_1 C46_1 1.444(11) . ? C46_1 C47_1 1.310(12) . ? C46_1 H46_1 0.9500 . ? C47_1 C48_1 1.431(12) . ? C47_1 H47_1 0.9500 . ? C48_1 C49_1 1.398(11) . ? C48_1 C53_1 1.402(10) . ? C49_1 C50_1 1.370(12) . ? C49_1 H49_1 0.9500 . ? C50_1 C51_1 1.403(11) . ? C50_1 H50_1 0.9500 . ? C51_1 C52_1 1.387(9) . ? C51_1 H51_1 0.9500 . ? C52_1 C53_1 1.423(10) . ? C52_1 H52_1 0.9500 . ? C53_1 C54_1 1.423(9) . ? C55_1 N61_1 1.302(11) . ? C55_1 H55_1 0.9500 . ? C61_1 N61_1 1.453(9) . ? C61_1 C62_1 1.520(14) . ? C61_1 C66_1 1.553(9) . ? C61_1 H61_1 1.0000 . ? C62_1 N62_1 1.488(9) . ? C62_1 C63_1 1.536(10) . ? C62_1 H62_1 1.0000 . ? C63_1 C64_1 1.592(11) . ? C63_1 H63A_1 0.9900 . ? C63_1 H63B_1 0.9900 . ? C64_1 C65_1 1.485(15) . ? C64_1 H64A_1 0.9900 . ? C64_1 H64B_1 0.9900 . ? C65_1 C66_1 1.552(11) . ? C65_1 H65A_1 0.9900 . ? C65_1 H65B_1 0.9900 . ? C66_1 H66A_1 0.9900 . ? C66_1 H66B_1 0.9900 . ? Ni2_2 N61_2 1.983(5) . ? Ni2_2 N31_2 1.995(5) . ? Ni2_2 N62_2 2.094(6) . ? Ni2_2 N32_2 2.130(5) . ? Ni2_2 N11_2 2.345(5) . ? Ni2_2 N41_2 2.363(6) . ? N11_2 C12_2 1.347(8) . ? N11_2 C24_2 1.367(8) . ? C12_2 C13_2 1.391(10) . ? C12_2 C25_2 1.475(9) . ? C13_2 C14_2 1.383(13) . ? C13_2 H13_2 0.9500 . ? C14_2 C15_2 1.367(13) . ? C14_2 H14_2 0.9500 . ? C15_2 C24_2 1.411(11) . ? C15_2 C16_2 1.466(13) . ? C16_2 C17_2 1.333(14) . ? C16_2 H16_2 0.9500 . ? C17_2 C18_2 1.461(12) . ? C17_2 H17_2 0.9500 . ? C18_2 C19_2 1.374(10) . ? C18_2 C23_2 1.415(9) . ? C19_2 C20_2 1.364(11) . ? C19_2 H19_2 0.9500 . ? C20_2 C21_2 1.365(12) . ? C20_2 H20_2 0.9500 . ? C21_2 C22_2 1.400(10) . ? C21_2 H21_2 0.9500 . ? C22_2 C23_2 1.386(10) . ? C22_2 H22_2 0.9500 . ? C23_2 C24_2 1.435(9) . ? C25_2 N31_2 1.248(8) . ? C25_2 H25_2 0.9500 . ? C31_2 N31_2 1.444(8) . ? C31_2 C36_2 1.517(9) . ? C31_2 C32_2 1.526(9) . ? C31_2 H31_2 1.0000 . ? C32_2 N32_2 1.468(7) . ? C32_2 C33_2 1.528(8) . ? C32_2 H32_2 1.0000 . ? C33_2 C34_2 1.555(10) . ? C33_2 H33A_2 0.9900 . ? C33_2 H33B_2 0.9900 . ? C34_2 C35_2 1.472(10) . ? C34_2 H34A_2 0.9900 . ? C34_2 H34B_2 0.9900 . ? C35_2 C36_2 1.552(9) . ? C35_2 H35A_2 0.9900 . ? C35_2 H35B_2 0.9900 . ? C36_2 H36A_2 0.9900 . ? C36_2 H36B_2 0.9900 . ? N41_2 C54_2 1.353(10) . ? N41_2 C42_2 1.358(10) . ? C42_2 C43_2 1.406(9) . ? C42_2 C55_2 1.459(11) . ? C43_2 C44_2 1.382(13) . ? C43_2 H43_2 0.9500 . ? C44_2 C45_2 1.393(14) . ? C44_2 H44_2 0.9500 . ? C45_2 C54_2 1.417(10) . ? C45_2 C46_2 1.433(12) . ? C46_2 C47_2 1.360(15) . ? C46_2 H46_2 0.9500 . ? C47_2 C48_2 1.400(13) . ? C47_2 H47_2 0.9500 . ? C48_2 C49_2 1.375(15) . ? C48_2 C53_2 1.443(12) . ? C49_2 C50_2 1.313(16) . ? C49_2 H49_2 0.9500 . ? C50_2 C51_2 1.435(13) . ? C50_2 H50_2 0.9500 . ? C51_2 C52_2 1.390(12) . ? C51_2 H51_2 0.9500 . ? C52_2 C53_2 1.367(12) . ? C52_2 H52_2 0.9500 . ? C53_2 C54_2 1.448(12) . ? C55_2 N61_2 1.279(8) . ? C55_2 H55_2 0.9500 . ? C61_2 N61_2 1.457(8) . ? C61_2 C66_2 1.527(8) . ? C61_2 C62_2 1.538(8) . ? C61_2 H61_2 1.0000 . ? C62_2 C63_2 1.466(12) . ? C62_2 N62_2 1.508(8) . ? C62_2 H62_2 1.0000 . ? C63_2 C64_2 1.505(11) . ? C63_2 H63A_2 0.9900 . ? C63_2 H63B_2 0.9900 . ? C64_2 C65_2 1.537(11) . ? C64_2 H64A_2 0.9900 . ? C64_2 H64B_2 0.9900 . ? C65_2 C66_2 1.517(13) . ? C65_2 H65A_2 0.9900 . ? C65_2 H65B_2 0.9900 . ? C66_2 H66A_2 0.9900 . ? C66_2 H66B_2 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 C71_1 O71_1 H71A_1 109.5 . . ? O71_1 C71_1 C72_1 111.0(10) . . ? O71_1 C71_1 H71B_1 109.4 . . ? C72_1 C71_1 H71B_1 109.4 . . ? O71_1 C71_1 H71C_1 109.4 . . ? C72_1 C71_1 H71C_1 109.4 . . ? H71B_1 C71_1 H71C_1 108.0 . . ? C71_1 C72_1 H72A_1 109.5 . . ? C71_1 C72_1 H72B_1 109.5 . . ? H72A_1 C72_1 H72B_1 109.5 . . ? C71_1 C72_1 H72C_1 109.5 . . ? H72A_1 C72_1 H72C_1 109.5 . . ? H72B_1 C72_1 H72C_1 109.5 . . ? C81_1 O81_1 H81A_1 109.5 . . ? O81_1 C81_1 C82_1 107.3(8) . . ? O81_1 C81_1 H81B_1 110.3 . . ? C82_1 C81_1 H81B_1 110.3 . . ? O81_1 C81_1 H81C_1 110.3 . . ? C82_1 C81_1 H81C_1 110.3 . . ? H81B_1 C81_1 H81C_1 108.5 . . ? C81_1 C82_1 H82A_1 109.5 . . ? C81_1 C82_1 H82B_1 109.5 . . ? H82A_1 C82_1 H82B_1 109.5 . . ? C81_1 C82_1 H82C_1 109.5 . . ? H82A_1 C82_1 H82C_1 109.5 . . ? H82B_1 C82_1 H82C_1 109.5 . . ? C91_1 O91_1 H91A_1 109.5 . . ? O91_1 C91_1 C92_1 124.2(10) . . ? O91_1 C91_1 H91B_1 106.3 . . ? C92_1 C91_1 H91B_1 106.3 . . ? O91_1 C91_1 H91C_1 106.3 . . ? C92_1 C91_1 H91C_1 106.3 . . ? H91B_1 C91_1 H91C_1 106.4 . . ? C91_1 C92_1 H92A_1 109.5 . . ? C91_1 C92_1 H92B_1 109.5 . . ? H92A_1 C92_1 H92B_1 109.5 . . ? C91_1 C92_1 H92C_1 109.5 . . ? H92A_1 C92_1 H92C_1 109.5 . . ? H92B_1 C92_1 H92C_1 109.5 . . ? C71_2 O71_2 H71A_2 109.5 . . ? O71_2 C71_2 C72_2 123.0(10) . . ? O71_2 C71_2 H71B_2 106.6 . . ? C72_2 C71_2 H71B_2 106.6 . . ? O71_2 C71_2 H71C_2 106.6 . . ? C72_2 C71_2 H71C_2 106.6 . . ? H71B_2 C71_2 H71C_2 106.5 . . ? C71_2 C72_2 H72A_2 109.5 . . ? C71_2 C72_2 H72B_2 109.5 . . ? H72A_2 C72_2 H72B_2 109.5 . . ? C71_2 C72_2 H72C_2 109.5 . . ? H72A_2 C72_2 H72C_2 109.5 . . ? H72B_2 C72_2 H72C_2 109.5 . . ? C81_2 O81_2 H81A_2 109.5 . . ? O81_2 C81_2 C82_2 110.0(10) . . ? O81_2 C81_2 H81B_2 109.7 . . ? C82_2 C81_2 H81B_2 109.7 . . ? O81_2 C81_2 H81C_2 109.7 . . ? C82_2 C81_2 H81C_2 109.7 . . ? H81B_2 C81_2 H81C_2 108.2 . . ? C81_2 C82_2 H82A_2 109.5 . . ? C81_2 C82_2 H82B_2 109.5 . . ? H82A_2 C82_2 H82B_2 109.5 . . ? C81_2 C82_2 H82C_2 109.5 . . ? H82A_2 C82_2 H82C_2 109.5 . . ? H82B_2 C82_2 H82C_2 109.5 . . ? C91_2 O91_2 H91A_2 109.5 . . ? O91_2 C91_2 C92_2 112.9(9) . . ? O91_2 C91_2 H91B_2 109.0 . . ? C92_2 C91_2 H91B_2 109.0 . . ? O91_2 C91_2 H91C_2 109.0 . . ? C92_2 C91_2 H91C_2 109.0 . . ? H91B_2 C91_2 H91C_2 107.8 . . ? C91_2 C92_2 H92A_2 109.5 . . ? C91_2 C92_2 H92B_2 109.5 . . ? H92A_2 C92_2 H92B_2 109.5 . . ? C91_2 C92_2 H92C_2 109.5 . . ? H92A_2 C92_2 H92C_2 109.5 . . ? H92B_2 C92_2 H92C_2 109.5 . . ? O3 S1 O1 116.7(7) . . ? O3 S1 O2 111.5(9) . . ? O1 S1 O2 117.5(5) . . ? O3 S1 C1A 101.7(5) . . ? O1 S1 C1A 105.9(4) . . ? O2 S1 C1A 100.5(5) . . ? F3A C1A F1A 107.4(7) . . ? F3A C1A F2A 109.3(7) . . ? F1A C1A F2A 99.6(7) . . ? F3A C1A S1 115.8(7) . . ? F1A C1A S1 113.9(6) . . ? F2A C1A S1 109.5(6) . . ? O4 S2 O5 129.5(7) . . ? O4 S2 O6 109.6(6) . . ? O5 S2 O6 104.0(7) . . ? O4 S2 C2 106.7(6) . . ? O5 S2 C2 105.2(6) . . ? O6 S2 C2 97.3(6) . . ? F6 C2 F4 92.1(12) . . ? F6 C2 F5 125.6(11) . . ? F4 C2 F5 102.4(8) . . ? F6 C2 S2 113.7(9) . . ? F4 C2 S2 109.7(9) . . ? F5 C2 S2 109.9(8) . . ? O7A S3A O8A 126.1(6) . . ? O7A S3A O9A 113.6(6) . . ? O8A S3A O9A 111.2(6) . . ? O7A S3A C3A 104.7(6) . . ? O8A S3A C3A 100.8(6) . . ? O9A S3A C3A 93.7(5) . . ? F9A C3A F8A 110.3(11) . . ? F9A C3A F7A 109.7(10) . . ? F8A C3A F7A 109.9(10) . . ? F9A C3A S3A 115.0(9) . . ? F8A C3A S3A 103.4(8) . . ? F7A C3A S3A 108.3(8) . . ? O7B S3B O8B 108.6(7) . . ? O7B S3B O9B 105.6(6) . . ? O8B S3B O9B 102.5(6) . . ? O7B S3B C3B 117.4(7) . . ? O8B S3B C3B 111.1(8) . . ? O9B S3B C3B 110.6(7) . . ? F8B C3B F7B 107.9(8) . . ? F8B C3B F9B 106.8(9) . . ? F7B C3B F9B 107.6(8) . . ? F8B C3B S3B 113.9(8) . . ? F7B C3B S3B 109.0(8) . . ? F9B C3B S3B 111.5(9) . . ? O10 S4 O12 113.7(3) . . ? O10 S4 O11 115.7(4) . . ? O12 S4 O11 115.8(5) . . ? O10 S4 C4 104.9(5) . . ? O12 S4 C4 101.8(4) . . ? O11 S4 C4 102.5(4) . . ? F11 C4 F12 111.0(9) . . ? F11 C4 F10 108.3(8) . . ? F12 C4 F10 103.7(10) . . ? F11 C4 S4 112.4(9) . . ? F12 C4 S4 111.1(7) . . ? F10 C4 S4 110.0(7) . . ? N31_1 Ni1_1 N61_1 174.2(2) . . ? N31_1 Ni1_1 N62_1 96.7(2) . . ? N61_1 Ni1_1 N62_1 81.1(3) . . ? N31_1 Ni1_1 N32_1 82.2(3) . . ? N61_1 Ni1_1 N32_1 92.6(3) . . ? N62_1 Ni1_1 N32_1 94.3(3) . . ? N31_1 Ni1_1 N41_1 105.4(2) . . ? N61_1 Ni1_1 N41_1 76.7(2) . . ? N62_1 Ni1_1 N41_1 157.8(2) . . ? N32_1 Ni1_1 N41_1 86.9(3) . . ? N31_1 Ni1_1 N11_1 74.0(2) . . ? N61_1 Ni1_1 N11_1 111.0(2) . . ? N62_1 Ni1_1 N11_1 84.4(3) . . ? N32_1 Ni1_1 N11_1 155.8(2) . . ? N41_1 Ni1_1 N11_1 103.37(19) . . ? C12_1 N11_1 C24_1 115.3(7) . . ? C12_1 N11_1 Ni1_1 104.9(5) . . ? C24_1 N11_1 Ni1_1 137.3(5) . . ? N11_1 C12_1 C13_1 126.4(8) . . ? N11_1 C12_1 C25_1 115.6(8) . . ? C13_1 C12_1 C25_1 117.9(7) . . ? C12_1 C13_1 C14_1 118.4(7) . . ? C12_1 C13_1 H13_1 120.8 . . ? C14_1 C13_1 H13_1 120.8 . . ? C15_1 C14_1 C13_1 117.1(11) . . ? C15_1 C14_1 H14_1 121.4 . . ? C13_1 C14_1 H14_1 121.4 . . ? C24_1 C15_1 C14_1 119.6(9) . . ? C24_1 C15_1 C16_1 120.8(8) . . ? C14_1 C15_1 C16_1 119.6(10) . . ? C17_1 C16_1 C15_1 121.4(10) . . ? C17_1 C16_1 H16_1 119.3 . . ? C15_1 C16_1 H16_1 119.3 . . ? C16_1 C17_1 C18_1 119.1(9) . . ? C16_1 C17_1 H17_1 120.5 . . ? C18_1 C17_1 H17_1 120.5 . . ? C23_1 C18_1 C19_1 118.4(8) . . ? C23_1 C18_1 C17_1 120.5(7) . . ? C19_1 C18_1 C17_1 120.9(8) . . ? C20_1 C19_1 C18_1 123.7(9) . . ? C20_1 C19_1 H19_1 118.1 . . ? C18_1 C19_1 H19_1 118.1 . . ? C19_1 C20_1 C21_1 118.8(7) . . ? C19_1 C20_1 H20_1 120.6 . . ? C21_1 C20_1 H20_1 120.6 . . ? C22_1 C21_1 C20_1 120.8(8) . . ? C22_1 C21_1 H21_1 119.6 . . ? C20_1 C21_1 H21_1 119.6 . . ? C21_1 C22_1 C23_1 119.4(7) . . ? C21_1 C22_1 H22_1 120.3 . . ? C23_1 C22_1 H22_1 120.3 . . ? C18_1 C23_1 C22_1 118.7(6) . . ? C18_1 C23_1 C24_1 118.8(8) . . ? C22_1 C23_1 C24_1 122.5(7) . . ? N11_1 C24_1 C15_1 122.7(7) . . ? N11_1 C24_1 C23_1 118.6(8) . . ? C15_1 C24_1 C23_1 118.7(8) . . ? N31_1 C25_1 C12_1 121.2(7) . . ? N31_1 C25_1 H25_1 119.4 . . ? C12_1 C25_1 H25_1 119.4 . . ? N31_1 C31_1 C36_1 113.2(7) . . ? N31_1 C31_1 C32_1 107.6(5) . . ? C36_1 C31_1 C32_1 111.6(7) . . ? N31_1 C31_1 H31_1 108.1 . . ? C36_1 C31_1 H31_1 108.1 . . ? C32_1 C31_1 H31_1 108.1 . . ? C25_1 N31_1 C31_1 120.7(6) . . ? C25_1 N31_1 Ni1_1 122.4(5) . . ? C31_1 N31_1 Ni1_1 115.9(5) . . ? C33_1 C32_1 N32_1 115.1(7) . . ? C33_1 C32_1 C31_1 108.6(7) . . ? N32_1 C32_1 C31_1 106.6(8) . . ? C33_1 C32_1 H32_1 108.8 . . ? N32_1 C32_1 H32_1 108.8 . . ? C31_1 C32_1 H32_1 108.8 . . ? C32_1 N32_1 Ni1_1 106.4(5) . . ? C32_1 C33_1 C34_1 108.7(7) . . ? C32_1 C33_1 H33A_1 110.0 . . ? C34_1 C33_1 H33A_1 110.0 . . ? C32_1 C33_1 H33B_1 110.0 . . ? C34_1 C33_1 H33B_1 110.0 . . ? H33A_1 C33_1 H33B_1 108.3 . . ? C35_1 C34_1 C33_1 110.4(9) . . ? C35_1 C34_1 H34A_1 109.6 . . ? C33_1 C34_1 H34A_1 109.6 . . ? C35_1 C34_1 H34B_1 109.6 . . ? C33_1 C34_1 H34B_1 109.6 . . ? H34A_1 C34_1 H34B_1 108.1 . . ? C34_1 C35_1 C36_1 113.8(8) . . ? C34_1 C35_1 H35A_1 108.8 . . ? C36_1 C35_1 H35A_1 108.8 . . ? C34_1 C35_1 H35B_1 108.8 . . ? C36_1 C35_1 H35B_1 108.8 . . ? H35A_1 C35_1 H35B_1 107.7 . . ? C31_1 C36_1 C35_1 105.4(8) . . ? C31_1 C36_1 H36A_1 110.7 . . ? C35_1 C36_1 H36A_1 110.7 . . ? C31_1 C36_1 H36B_1 110.7 . . ? C35_1 C36_1 H36B_1 110.7 . . ? H36A_1 C36_1 H36B_1 108.8 . . ? C42_1 N41_1 C54_1 116.1(6) . . ? C42_1 N41_1 Ni1_1 106.7(4) . . ? C54_1 N41_1 Ni1_1 131.6(4) . . ? N41_1 C42_1 C43_1 125.4(7) . . ? N41_1 C42_1 C55_1 116.3(7) . . ? C43_1 C42_1 C55_1 117.8(6) . . ? C44_1 C43_1 C42_1 119.6(6) . . ? C44_1 C43_1 H43_1 120.2 . . ? C42_1 C43_1 H43_1 120.2 . . ? C43_1 C44_1 C45_1 118.3(7) . . ? C43_1 C44_1 H44_1 120.9 . . ? C45_1 C44_1 H44_1 120.9 . . ? C44_1 C45_1 C54_1 118.7(7) . . ? C44_1 C45_1 C46_1 122.3(8) . . ? C54_1 C45_1 C46_1 118.9(6) . . ? C47_1 C46_1 C45_1 120.3(8) . . ? C47_1 C46_1 H46_1 119.8 . . ? C45_1 C46_1 H46_1 119.8 . . ? C46_1 C47_1 C48_1 122.1(7) . . ? C46_1 C47_1 H47_1 118.9 . . ? C48_1 C47_1 H47_1 118.9 . . ? C49_1 C48_1 C53_1 119.9(7) . . ? C49_1 C48_1 C47_1 120.7(7) . . ? C53_1 C48_1 C47_1 119.4(7) . . ? C50_1 C49_1 C48_1 121.0(7) . . ? C50_1 C49_1 H49_1 119.5 . . ? C48_1 C49_1 H49_1 119.5 . . ? C49_1 C50_1 C51_1 120.1(7) . . ? C49_1 C50_1 H50_1 119.9 . . ? C51_1 C50_1 H50_1 119.9 . . ? C52_1 C51_1 C50_1 119.7(8) . . ? C52_1 C51_1 H51_1 120.2 . . ? C50_1 C51_1 H51_1 120.2 . . ? C51_1 C52_1 C53_1 120.5(7) . . ? C51_1 C52_1 H52_1 119.7 . . ? C53_1 C52_1 H52_1 119.7 . . ? C48_1 C53_1 C54_1 119.2(7) . . ? C48_1 C53_1 C52_1 118.3(6) . . ? C54_1 C53_1 C52_1 122.4(6) . . ? N41_1 C54_1 C53_1 120.2(7) . . ? N41_1 C54_1 C45_1 121.2(6) . . ? C53_1 C54_1 C45_1 118.5(6) . . ? N61_1 C55_1 C42_1 117.3(6) . . ? N61_1 C55_1 H55_1 121.3 . . ? C42_1 C55_1 H55_1 121.3 . . ? N61_1 C61_1 C62_1 106.2(6) . . ? N61_1 C61_1 C66_1 115.9(6) . . ? C62_1 C61_1 C66_1 112.6(7) . . ? N61_1 C61_1 H61_1 107.3 . . ? C62_1 C61_1 H61_1 107.3 . . ? C66_1 C61_1 H61_1 107.3 . . ? C55_1 N61_1 C61_1 122.7(6) . . ? C55_1 N61_1 Ni1_1 119.0(5) . . ? C61_1 N61_1 Ni1_1 115.8(5) . . ? N62_1 C62_1 C61_1 107.2(8) . . ? N62_1 C62_1 C63_1 111.3(6) . . ? C61_1 C62_1 C63_1 111.3(7) . . ? N62_1 C62_1 H62_1 109.0 . . ? C61_1 C62_1 H62_1 109.0 . . ? C63_1 C62_1 H62_1 109.0 . . ? C62_1 N62_1 Ni1_1 106.6(5) . . ? C62_1 C63_1 C64_1 107.6(7) . . ? C62_1 C63_1 H63A_1 110.2 . . ? C64_1 C63_1 H63A_1 110.2 . . ? C62_1 C63_1 H63B_1 110.2 . . ? C64_1 C63_1 H63B_1 110.2 . . ? H63A_1 C63_1 H63B_1 108.5 . . ? C65_1 C64_1 C63_1 112.8(8) . . ? C65_1 C64_1 H64A_1 109.0 . . ? C63_1 C64_1 H64A_1 109.0 . . ? C65_1 C64_1 H64B_1 109.0 . . ? C63_1 C64_1 H64B_1 109.0 . . ? H64A_1 C64_1 H64B_1 107.8 . . ? C64_1 C65_1 C66_1 112.0(7) . . ? C64_1 C65_1 H65A_1 109.2 . . ? C66_1 C65_1 H65A_1 109.2 . . ? C64_1 C65_1 H65B_1 109.2 . . ? C66_1 C65_1 H65B_1 109.2 . . ? H65A_1 C65_1 H65B_1 107.9 . . ? C65_1 C66_1 C61_1 107.0(6) . . ? C65_1 C66_1 H66A_1 110.3 . . ? C61_1 C66_1 H66A_1 110.3 . . ? C65_1 C66_1 H66B_1 110.3 . . ? C61_1 C66_1 H66B_1 110.3 . . ? H66A_1 C66_1 H66B_1 108.6 . . ? N61_2 Ni2_2 N31_2 176.9(2) . . ? N61_2 Ni2_2 N62_2 82.3(2) . . ? N31_2 Ni2_2 N62_2 94.9(2) . . ? N61_2 Ni2_2 N32_2 101.1(2) . . ? N31_2 Ni2_2 N32_2 80.4(2) . . ? N62_2 Ni2_2 N32_2 93.1(3) . . ? N61_2 Ni2_2 N11_2 102.1(2) . . ? N31_2 Ni2_2 N11_2 76.2(2) . . ? N62_2 Ni2_2 N11_2 85.3(2) . . ? N32_2 Ni2_2 N11_2 156.3(2) . . ? N61_2 Ni2_2 N41_2 75.9(2) . . ? N31_2 Ni2_2 N41_2 107.1(2) . . ? N62_2 Ni2_2 N41_2 156.3(2) . . ? N32_2 Ni2_2 N41_2 82.2(2) . . ? N11_2 Ni2_2 N41_2 108.15(19) . . ? C12_2 N11_2 C24_2 118.0(5) . . ? C12_2 N11_2 Ni2_2 104.2(4) . . ? C24_2 N11_2 Ni2_2 130.8(4) . . ? N11_2 C12_2 C13_2 123.1(6) . . ? N11_2 C12_2 C25_2 116.1(6) . . ? C13_2 C12_2 C25_2 120.6(6) . . ? C14_2 C13_2 C12_2 119.1(7) . . ? C14_2 C13_2 H13_2 120.5 . . ? C12_2 C13_2 H13_2 120.5 . . ? C15_2 C14_2 C13_2 117.3(8) . . ? C15_2 C14_2 H14_2 121.4 . . ? C13_2 C14_2 H14_2 121.4 . . ? C14_2 C15_2 C24_2 121.9(8) . . ? C14_2 C15_2 C16_2 119.5(9) . . ? C24_2 C15_2 C16_2 118.4(8) . . ? C17_2 C16_2 C15_2 120.6(8) . . ? C17_2 C16_2 H16_2 119.7 . . ? C15_2 C16_2 H16_2 119.7 . . ? C16_2 C17_2 C18_2 121.8(8) . . ? C16_2 C17_2 H17_2 119.1 . . ? C18_2 C17_2 H17_2 119.1 . . ? C19_2 C18_2 C23_2 119.6(7) . . ? C19_2 C18_2 C17_2 122.0(7) . . ? C23_2 C18_2 C17_2 118.3(7) . . ? C20_2 C19_2 C18_2 121.5(7) . . ? C20_2 C19_2 H19_2 119.2 . . ? C18_2 C19_2 H19_2 119.2 . . ? C19_2 C20_2 C21_2 120.4(7) . . ? C19_2 C20_2 H20_2 119.8 . . ? C21_2 C20_2 H20_2 119.8 . . ? C20_2 C21_2 C22_2 119.1(7) . . ? C20_2 C21_2 H21_2 120.4 . . ? C22_2 C21_2 H21_2 120.4 . . ? C23_2 C22_2 C21_2 121.4(7) . . ? C23_2 C22_2 H22_2 119.3 . . ? C21_2 C22_2 H22_2 119.3 . . ? C22_2 C23_2 C18_2 117.7(6) . . ? C22_2 C23_2 C24_2 122.5(6) . . ? C18_2 C23_2 C24_2 119.8(6) . . ? N11_2 C24_2 C15_2 119.2(6) . . ? N11_2 C24_2 C23_2 121.0(6) . . ? C15_2 C24_2 C23_2 119.8(6) . . ? N31_2 C25_2 C12_2 119.2(6) . . ? N31_2 C25_2 H25_2 120.4 . . ? C12_2 C25_2 H25_2 120.4 . . ? N31_2 C31_2 C36_2 117.1(5) . . ? N31_2 C31_2 C32_2 107.2(5) . . ? C36_2 C31_2 C32_2 111.4(5) . . ? N31_2 C31_2 H31_2 106.9 . . ? C36_2 C31_2 H31_2 106.9 . . ? C32_2 C31_2 H31_2 106.9 . . ? C25_2 N31_2 C31_2 124.1(5) . . ? C25_2 N31_2 Ni2_2 119.0(5) . . ? C31_2 N31_2 Ni2_2 116.2(4) . . ? N32_2 C32_2 C31_2 108.5(5) . . ? N32_2 C32_2 C33_2 113.5(5) . . ? C31_2 C32_2 C33_2 110.6(6) . . ? N32_2 C32_2 H32_2 108.0 . . ? C31_2 C32_2 H32_2 108.0 . . ? C33_2 C32_2 H32_2 108.0 . . ? C32_2 N32_2 Ni2_2 108.6(4) . . ? C32_2 C33_2 C34_2 110.0(6) . . ? C32_2 C33_2 H33A_2 109.7 . . ? C34_2 C33_2 H33A_2 109.7 . . ? C32_2 C33_2 H33B_2 109.7 . . ? C34_2 C33_2 H33B_2 109.7 . . ? H33A_2 C33_2 H33B_2 108.2 . . ? C35_2 C34_2 C33_2 112.6(6) . . ? C35_2 C34_2 H34A_2 109.1 . . ? C33_2 C34_2 H34A_2 109.1 . . ? C35_2 C34_2 H34B_2 109.1 . . ? C33_2 C34_2 H34B_2 109.1 . . ? H34A_2 C34_2 H34B_2 107.8 . . ? C34_2 C35_2 C36_2 111.8(6) . . ? C34_2 C35_2 H35A_2 109.3 . . ? C36_2 C35_2 H35A_2 109.3 . . ? C34_2 C35_2 H35B_2 109.3 . . ? C36_2 C35_2 H35B_2 109.3 . . ? H35A_2 C35_2 H35B_2 107.9 . . ? C31_2 C36_2 C35_2 110.0(6) . . ? C31_2 C36_2 H36A_2 109.7 . . ? C35_2 C36_2 H36A_2 109.7 . . ? C31_2 C36_2 H36B_2 109.7 . . ? C35_2 C36_2 H36B_2 109.7 . . ? H36A_2 C36_2 H36B_2 108.2 . . ? C54_2 N41_2 C42_2 120.1(6) . . ? C54_2 N41_2 Ni2_2 129.6(4) . . ? C42_2 N41_2 Ni2_2 102.3(5) . . ? N41_2 C42_2 C43_2 121.8(7) . . ? N41_2 C42_2 C55_2 118.9(6) . . ? C43_2 C42_2 C55_2 119.1(7) . . ? C44_2 C43_2 C42_2 116.9(8) . . ? C44_2 C43_2 H43_2 121.5 . . ? C42_2 C43_2 H43_2 121.5 . . ? C43_2 C44_2 C45_2 122.7(7) . . ? C43_2 C44_2 H44_2 118.6 . . ? C45_2 C44_2 H44_2 118.6 . . ? C44_2 C45_2 C54_2 116.6(7) . . ? C44_2 C45_2 C46_2 124.1(7) . . ? C54_2 C45_2 C46_2 119.3(8) . . ? C47_2 C46_2 C45_2 120.4(7) . . ? C47_2 C46_2 H46_2 119.8 . . ? C45_2 C46_2 H46_2 119.8 . . ? C46_2 C47_2 C48_2 122.8(9) . . ? C46_2 C47_2 H47_2 118.6 . . ? C48_2 C47_2 H47_2 118.6 . . ? C49_2 C48_2 C47_2 123.5(9) . . ? C49_2 C48_2 C53_2 118.0(9) . . ? C47_2 C48_2 C53_2 118.4(9) . . ? C50_2 C49_2 C48_2 122.6(9) . . ? C50_2 C49_2 H49_2 118.7 . . ? C48_2 C49_2 H49_2 118.7 . . ? C49_2 C50_2 C51_2 122.0(10) . . ? C49_2 C50_2 H50_2 119.0 . . ? C51_2 C50_2 H50_2 119.0 . . ? C52_2 C51_2 C50_2 115.2(9) . . ? C52_2 C51_2 H51_2 122.4 . . ? C50_2 C51_2 H51_2 122.4 . . ? C53_2 C52_2 C51_2 123.8(8) . . ? C53_2 C52_2 H52_2 118.1 . . ? C51_2 C52_2 H52_2 118.1 . . ? C52_2 C53_2 C48_2 117.7(8) . . ? C52_2 C53_2 C54_2 123.5(7) . . ? C48_2 C53_2 C54_2 118.7(8) . . ? N41_2 C54_2 C45_2 121.3(8) . . ? N41_2 C54_2 C53_2 119.4(6) . . ? C45_2 C54_2 C53_2 119.3(7) . . ? N61_2 C55_2 C42_2 115.8(6) . . ? N61_2 C55_2 H55_2 122.1 . . ? C42_2 C55_2 H55_2 122.1 . . ? N61_2 C61_2 C66_2 116.4(5) . . ? N61_2 C61_2 C62_2 106.0(5) . . ? C66_2 C61_2 C62_2 111.3(5) . . ? N61_2 C61_2 H61_2 107.6 . . ? C66_2 C61_2 H61_2 107.6 . . ? C62_2 C61_2 H61_2 107.6 . . ? C55_2 N61_2 C61_2 124.4(5) . . ? C55_2 N61_2 Ni2_2 120.8(5) . . ? C61_2 N61_2 Ni2_2 114.1(4) . . ? C63_2 C62_2 N62_2 115.1(6) . . ? C63_2 C62_2 C61_2 112.4(6) . . ? N62_2 C62_2 C61_2 108.3(5) . . ? C63_2 C62_2 H62_2 106.9 . . ? N62_2 C62_2 H62_2 106.9 . . ? C61_2 C62_2 H62_2 106.9 . . ? C62_2 N62_2 Ni2_2 108.6(4) . . ? C62_2 C63_2 C64_2 113.5(9) . . ? C62_2 C63_2 H63A_2 108.9 . . ? C64_2 C63_2 H63A_2 108.9 . . ? C62_2 C63_2 H63B_2 108.9 . . ? C64_2 C63_2 H63B_2 108.9 . . ? H63A_2 C63_2 H63B_2 107.7 . . ? C63_2 C64_2 C65_2 113.5(7) . . ? C63_2 C64_2 H64A_2 108.9 . . ? C65_2 C64_2 H64A_2 108.9 . . ? C63_2 C64_2 H64B_2 108.9 . . ? C65_2 C64_2 H64B_2 108.9 . . ? H64A_2 C64_2 H64B_2 107.7 . . ? C66_2 C65_2 C64_2 110.9(8) . . ? C66_2 C65_2 H65A_2 109.5 . . ? C64_2 C65_2 H65A_2 109.5 . . ? C66_2 C65_2 H65B_2 109.5 . . ? C64_2 C65_2 H65B_2 109.5 . . ? H65A_2 C65_2 H65B_2 108.0 . . ? C65_2 C66_2 C61_2 109.3(6) . . ? C65_2 C66_2 H66A_2 109.8 . . ? C61_2 C66_2 H66A_2 109.8 . . ? C65_2 C66_2 H66B_2 109.8 . . ? C61_2 C66_2 H66B_2 109.8 . . ? H66A_2 C66_2 H66B_2 108.3 . . ? 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 O3 S1 C1A F3A 41.1(11) . . . . ? O1 S1 C1A F3A 163.6(8) . . . . ? O2 S1 C1A F3A -73.6(10) . . . . ? O3 S1 C1A F1A -84.1(10) . . . . ? O1 S1 C1A F1A 38.3(8) . . . . ? O2 S1 C1A F1A 161.1(8) . . . . ? O3 S1 C1A F2A 165.3(10) . . . . ? O1 S1 C1A F2A -72.3(8) . . . . ? O2 S1 C1A F2A 50.5(9) . . . . ? O4 S2 C2 F6 -40.9(13) . . . . ? O5 S2 C2 F6 178.8(12) . . . . ? O6 S2 C2 F6 72.1(12) . . . . ? O4 S2 C2 F4 60.6(9) . . . . ? O5 S2 C2 F4 -79.6(10) . . . . ? O6 S2 C2 F4 173.7(9) . . . . ? O4 S2 C2 F5 172.4(9) . . . . ? O5 S2 C2 F5 32.2(11) . . . . ? O6 S2 C2 F5 -74.5(9) . . . . ? O7A S3A C3A F9A 165.8(10) . . . . ? O8A S3A C3A F9A -62.2(11) . . . . ? O9A S3A C3A F9A 50.2(10) . . . . ? O7A S3A C3A F8A -74.0(9) . . . . ? O8A S3A C3A F8A 58.0(9) . . . . ? O9A S3A C3A F8A 170.4(8) . . . . ? O7A S3A C3A F7A 42.6(9) . . . . ? O8A S3A C3A F7A 174.6(8) . . . . ? O9A S3A C3A F7A -73.0(8) . . . . ? O7B S3B C3B F8B -177.7(8) . . . . ? O8B S3B C3B F8B -51.9(10) . . . . ? O9B S3B C3B F8B 61.1(10) . . . . ? O7B S3B C3B F7B -57.2(10) . . . . ? O8B S3B C3B F7B 68.6(9) . . . . ? O9B S3B C3B F7B -178.3(7) . . . . ? O7B S3B C3B F9B 61.4(10) . . . . ? O8B S3B C3B F9B -172.8(8) . . . . ? O9B S3B C3B F9B -59.8(9) . . . . ? O10 S4 C4 F11 177.0(7) . . . . ? O12 S4 C4 F11 58.3(8) . . . . ? O11 S4 C4 F11 -61.8(8) . . . . ? O10 S4 C4 F12 52.0(9) . . . . ? O12 S4 C4 F12 -66.7(8) . . . . ? O11 S4 C4 F12 173.2(8) . . . . ? O10 S4 C4 F10 -62.3(8) . . . . ? O12 S4 C4 F10 179.0(7) . . . . ? O11 S4 C4 F10 59.0(9) . . . . ? N31_1 Ni1_1 N11_1 C12_1 -12.0(4) . . . . ? N61_1 Ni1_1 N11_1 C12_1 164.8(4) . . . . ? N62_1 Ni1_1 N11_1 C12_1 86.6(5) . . . . ? N32_1 Ni1_1 N11_1 C12_1 -1.5(9) . . . . ? N41_1 Ni1_1 N11_1 C12_1 -114.5(4) . . . . ? N31_1 Ni1_1 N11_1 C24_1 -172.2(7) . . . . ? N61_1 Ni1_1 N11_1 C24_1 4.6(7) . . . . ? N62_1 Ni1_1 N11_1 C24_1 -73.6(7) . . . . ? N32_1 Ni1_1 N11_1 C24_1 -161.7(7) . . . . ? N41_1 Ni1_1 N11_1 C24_1 85.3(7) . . . . ? C24_1 N11_1 C12_1 C13_1 1.6(11) . . . . ? Ni1_1 N11_1 C12_1 C13_1 -163.6(7) . . . . ? C24_1 N11_1 C12_1 C25_1 177.3(6) . . . . ? Ni1_1 N11_1 C12_1 C25_1 12.1(7) . . . . ? N11_1 C12_1 C13_1 C14_1 -1.9(13) . . . . ? C25_1 C12_1 C13_1 C14_1 -177.5(9) . . . . ? C12_1 C13_1 C14_1 C15_1 4.6(15) . . . . ? C13_1 C14_1 C15_1 C24_1 -7.3(16) . . . . ? C13_1 C14_1 C15_1 C16_1 174.8(11) . . . . ? C24_1 C15_1 C16_1 C17_1 1.7(19) . . . . ? C14_1 C15_1 C16_1 C17_1 179.6(12) . . . . ? C15_1 C16_1 C17_1 C18_1 -5(2) . . . . ? C16_1 C17_1 C18_1 C23_1 1.0(18) . . . . ? C16_1 C17_1 C18_1 C19_1 -173.9(12) . . . . ? C23_1 C18_1 C19_1 C20_1 -0.2(15) . . . . ? C17_1 C18_1 C19_1 C20_1 174.8(10) . . . . ? C18_1 C19_1 C20_1 C21_1 -3.7(15) . . . . ? C19_1 C20_1 C21_1 C22_1 4.2(12) . . . . ? C20_1 C21_1 C22_1 C23_1 -0.7(10) . . . . ? C19_1 C18_1 C23_1 C22_1 3.6(13) . . . . ? C17_1 C18_1 C23_1 C22_1 -171.4(9) . . . . ? C19_1 C18_1 C23_1 C24_1 -178.3(8) . . . . ? C17_1 C18_1 C23_1 C24_1 6.7(14) . . . . ? C21_1 C22_1 C23_1 C18_1 -3.2(11) . . . . ? C21_1 C22_1 C23_1 C24_1 178.8(7) . . . . ? C12_1 N11_1 C24_1 C15_1 -4.4(11) . . . . ? Ni1_1 N11_1 C24_1 C15_1 154.4(7) . . . . ? C12_1 N11_1 C24_1 C23_1 174.9(6) . . . . ? Ni1_1 N11_1 C24_1 C23_1 -26.3(10) . . . . ? C14_1 C15_1 C24_1 N11_1 7.5(14) . . . . ? C16_1 C15_1 C24_1 N11_1 -174.6(9) . . . . ? C14_1 C15_1 C24_1 C23_1 -171.8(9) . . . . ? C16_1 C15_1 C24_1 C23_1 6.1(14) . . . . ? C18_1 C23_1 C24_1 N11_1 170.6(7) . . . . ? C22_1 C23_1 C24_1 N11_1 -11.4(11) . . . . ? C18_1 C23_1 C24_1 C15_1 -10.1(12) . . . . ? C22_1 C23_1 C24_1 C15_1 167.9(8) . . . . ? N11_1 C12_1 C25_1 N31_1 -5.7(10) . . . . ? C13_1 C12_1 C25_1 N31_1 170.3(7) . . . . ? C12_1 C25_1 N31_1 C31_1 -175.4(6) . . . . ? C12_1 C25_1 N31_1 Ni1_1 -7.6(9) . . . . ? C36_1 C31_1 N31_1 C25_1 -45.3(9) . . . . ? C32_1 C31_1 N31_1 C25_1 -169.1(6) . . . . ? C36_1 C31_1 N31_1 Ni1_1 146.1(6) . . . . ? C32_1 C31_1 N31_1 Ni1_1 22.4(7) . . . . ? N62_1 Ni1_1 N31_1 C25_1 -71.7(6) . . . . ? N32_1 Ni1_1 N31_1 C25_1 -165.2(6) . . . . ? N41_1 Ni1_1 N31_1 C25_1 110.3(6) . . . . ? N11_1 Ni1_1 N31_1 C25_1 10.5(5) . . . . ? N62_1 Ni1_1 N31_1 C31_1 96.7(5) . . . . ? N32_1 Ni1_1 N31_1 C31_1 3.2(5) . . . . ? N41_1 Ni1_1 N31_1 C31_1 -81.3(5) . . . . ? N11_1 Ni1_1 N31_1 C31_1 178.8(5) . . . . ? N31_1 C31_1 C32_1 C33_1 -170.3(6) . . . . ? C36_1 C31_1 C32_1 C33_1 65.0(8) . . . . ? N31_1 C31_1 C32_1 N32_1 -45.8(7) . . . . ? C36_1 C31_1 C32_1 N32_1 -170.5(6) . . . . ? C33_1 C32_1 N32_1 Ni1_1 168.0(7) . . . . ? C31_1 C32_1 N32_1 Ni1_1 47.6(7) . . . . ? N31_1 Ni1_1 N32_1 C32_1 -29.0(6) . . . . ? N61_1 Ni1_1 N32_1 C32_1 153.6(6) . . . . ? N62_1 Ni1_1 N32_1 C32_1 -125.2(6) . . . . ? N41_1 Ni1_1 N32_1 C32_1 77.1(6) . . . . ? N11_1 Ni1_1 N32_1 C32_1 -39.2(10) . . . . ? N32_1 C32_1 C33_1 C34_1 179.3(9) . . . . ? C31_1 C32_1 C33_1 C34_1 -61.5(10) . . . . ? C32_1 C33_1 C34_1 C35_1 58.3(11) . . . . ? C33_1 C34_1 C35_1 C36_1 -56.7(10) . . . . ? N31_1 C31_1 C36_1 C35_1 179.8(7) . . . . ? C32_1 C31_1 C36_1 C35_1 -58.7(8) . . . . ? C34_1 C35_1 C36_1 C31_1 55.6(10) . . . . ? N31_1 Ni1_1 N41_1 C42_1 157.2(4) . . . . ? N61_1 Ni1_1 N41_1 C42_1 -17.2(4) . . . . ? N62_1 Ni1_1 N41_1 C42_1 -17.6(9) . . . . ? N32_1 Ni1_1 N41_1 C42_1 76.2(4) . . . . ? N11_1 Ni1_1 N41_1 C42_1 -126.0(4) . . . . ? N31_1 Ni1_1 N41_1 C54_1 5.3(6) . . . . ? N61_1 Ni1_1 N41_1 C54_1 -169.1(6) . . . . ? N62_1 Ni1_1 N41_1 C54_1 -169.5(8) . . . . ? N32_1 Ni1_1 N41_1 C54_1 -75.7(6) . . . . ? N11_1 Ni1_1 N41_1 C54_1 82.1(6) . . . . ? C54_1 N41_1 C42_1 C43_1 3.0(9) . . . . ? Ni1_1 N41_1 C42_1 C43_1 -153.9(5) . . . . ? C54_1 N41_1 C42_1 C55_1 175.3(5) . . . . ? Ni1_1 N41_1 C42_1 C55_1 18.4(6) . . . . ? N41_1 C42_1 C43_1 C44_1 3.3(9) . . . . ? C55_1 C42_1 C43_1 C44_1 -168.8(6) . . . . ? C42_1 C43_1 C44_1 C45_1 -3.5(9) . . . . ? C43_1 C44_1 C45_1 C54_1 -2.2(9) . . . . ? C43_1 C44_1 C45_1 C46_1 176.6(6) . . . . ? C44_1 C45_1 C46_1 C47_1 -179.9(6) . . . . ? C54_1 C45_1 C46_1 C47_1 -1.0(10) . . . . ? C45_1 C46_1 C47_1 C48_1 -7.2(10) . . . . ? C46_1 C47_1 C48_1 C49_1 -174.0(7) . . . . ? C46_1 C47_1 C48_1 C53_1 5.1(10) . . . . ? C53_1 C48_1 C49_1 C50_1 -6.9(10) . . . . ? C47_1 C48_1 C49_1 C50_1 172.2(6) . . . . ? C48_1 C49_1 C50_1 C51_1 0.3(10) . . . . ? C49_1 C50_1 C51_1 C52_1 4.1(10) . . . . ? C50_1 C51_1 C52_1 C53_1 -1.9(9) . . . . ? C49_1 C48_1 C53_1 C54_1 -175.6(6) . . . . ? C47_1 C48_1 C53_1 C54_1 5.3(9) . . . . ? C49_1 C48_1 C53_1 C52_1 8.9(9) . . . . ? C47_1 C48_1 C53_1 C52_1 -170.2(6) . . . . ? C51_1 C52_1 C53_1 C48_1 -4.5(8) . . . . ? C51_1 C52_1 C53_1 C54_1 -180.0(6) . . . . ? C42_1 N41_1 C54_1 C53_1 169.8(5) . . . . ? Ni1_1 N41_1 C54_1 C53_1 -40.4(8) . . . . ? C42_1 N41_1 C54_1 C45_1 -9.0(8) . . . . ? Ni1_1 N41_1 C54_1 C45_1 140.8(5) . . . . ? C48_1 C53_1 C54_1 N41_1 168.1(5) . . . . ? C52_1 C53_1 C54_1 N41_1 -16.5(8) . . . . ? C48_1 C53_1 C54_1 C45_1 -13.1(8) . . . . ? C52_1 C53_1 C54_1 C45_1 162.3(5) . . . . ? C44_1 C45_1 C54_1 N41_1 8.8(9) . . . . ? C46_1 C45_1 C54_1 N41_1 -170.1(6) . . . . ? C44_1 C45_1 C54_1 C53_1 -170.0(5) . . . . ? C46_1 C45_1 C54_1 C53_1 11.1(9) . . . . ? N41_1 C42_1 C55_1 N61_1 -8.8(8) . . . . ? C43_1 C42_1 C55_1 N61_1 164.0(6) . . . . ? C42_1 C55_1 N61_1 C61_1 -169.9(5) . . . . ? C42_1 C55_1 N61_1 Ni1_1 -8.8(7) . . . . ? C62_1 C61_1 N61_1 C55_1 -168.2(6) . . . . ? C66_1 C61_1 N61_1 C55_1 -42.4(10) . . . . ? C62_1 C61_1 N61_1 Ni1_1 30.1(6) . . . . ? C66_1 C61_1 N61_1 Ni1_1 155.9(6) . . . . ? N62_1 Ni1_1 N61_1 C55_1 -165.9(5) . . . . ? N32_1 Ni1_1 N61_1 C55_1 -72.0(5) . . . . ? N41_1 Ni1_1 N61_1 C55_1 14.2(5) . . . . ? N11_1 Ni1_1 N61_1 C55_1 113.6(5) . . . . ? N62_1 Ni1_1 N61_1 C61_1 -3.6(5) . . . . ? N32_1 Ni1_1 N61_1 C61_1 90.4(5) . . . . ? N41_1 Ni1_1 N61_1 C61_1 176.6(5) . . . . ? N11_1 Ni1_1 N61_1 C61_1 -84.0(5) . . . . ? N61_1 C61_1 C62_1 N62_1 -50.2(6) . . . . ? C66_1 C61_1 C62_1 N62_1 -178.0(5) . . . . ? N61_1 C61_1 C62_1 C63_1 -172.1(6) . . . . ? C66_1 C61_1 C62_1 C63_1 60.0(8) . . . . ? C61_1 C62_1 N62_1 Ni1_1 47.3(7) . . . . ? C63_1 C62_1 N62_1 Ni1_1 169.2(8) . . . . ? N31_1 Ni1_1 N62_1 C62_1 160.9(7) . . . . ? N61_1 Ni1_1 N62_1 C62_1 -24.5(6) . . . . ? N32_1 Ni1_1 N62_1 C62_1 -116.5(7) . . . . ? N41_1 Ni1_1 N62_1 C62_1 -24.2(12) . . . . ? N11_1 Ni1_1 N62_1 C62_1 87.7(7) . . . . ? N62_1 C62_1 C63_1 C64_1 -174.7(9) . . . . ? C61_1 C62_1 C63_1 C64_1 -55.1(10) . . . . ? C62_1 C63_1 C64_1 C65_1 55.5(11) . . . . ? C63_1 C64_1 C65_1 C66_1 -58.2(9) . . . . ? C64_1 C65_1 C66_1 C61_1 57.0(9) . . . . ? N61_1 C61_1 C66_1 C65_1 179.6(7) . . . . ? C62_1 C61_1 C66_1 C65_1 -57.9(8) . . . . ? N61_2 Ni2_2 N11_2 C12_2 -157.7(4) . . . . ? N31_2 Ni2_2 N11_2 C12_2 19.6(4) . . . . ? N62_2 Ni2_2 N11_2 C12_2 -76.6(4) . . . . ? N32_2 Ni2_2 N11_2 C12_2 10.3(8) . . . . ? N41_2 Ni2_2 N11_2 C12_2 123.4(4) . . . . ? N61_2 Ni2_2 N11_2 C24_2 -8.7(6) . . . . ? N31_2 Ni2_2 N11_2 C24_2 168.6(6) . . . . ? N62_2 Ni2_2 N11_2 C24_2 72.4(6) . . . . ? N32_2 Ni2_2 N11_2 C24_2 159.4(6) . . . . ? N41_2 Ni2_2 N11_2 C24_2 -87.6(6) . . . . ? C24_2 N11_2 C12_2 C13_2 -1.1(10) . . . . ? Ni2_2 N11_2 C12_2 C13_2 152.7(6) . . . . ? C24_2 N11_2 C12_2 C25_2 -175.7(5) . . . . ? Ni2_2 N11_2 C12_2 C25_2 -21.9(6) . . . . ? N11_2 C12_2 C13_2 C14_2 -9.6(13) . . . . ? C25_2 C12_2 C13_2 C14_2 164.8(9) . . . . ? C12_2 C13_2 C14_2 C15_2 10.7(17) . . . . ? C13_2 C14_2 C15_2 C24_2 -1.9(19) . . . . ? C13_2 C14_2 C15_2 C16_2 -176.2(12) . . . . ? C14_2 C15_2 C16_2 C17_2 -175.9(14) . . . . ? C24_2 C15_2 C16_2 C17_2 10(2) . . . . ? C15_2 C16_2 C17_2 C18_2 -3(2) . . . . ? C16_2 C17_2 C18_2 C19_2 176.5(11) . . . . ? C16_2 C17_2 C18_2 C23_2 0.5(17) . . . . ? C23_2 C18_2 C19_2 C20_2 -1.7(11) . . . . ? C17_2 C18_2 C19_2 C20_2 -177.7(9) . . . . ? C18_2 C19_2 C20_2 C21_2 4.3(12) . . . . ? C19_2 C20_2 C21_2 C22_2 -2.7(13) . . . . ? C20_2 C21_2 C22_2 C23_2 -1.5(12) . . . . ? C21_2 C22_2 C23_2 C18_2 4.0(10) . . . . ? C21_2 C22_2 C23_2 C24_2 -178.1(7) . . . . ? C19_2 C18_2 C23_2 C22_2 -2.4(10) . . . . ? C17_2 C18_2 C23_2 C22_2 173.8(8) . . . . ? C19_2 C18_2 C23_2 C24_2 179.6(6) . . . . ? C17_2 C18_2 C23_2 C24_2 -4.2(11) . . . . ? C12_2 N11_2 C24_2 C15_2 10.0(10) . . . . ? Ni2_2 N11_2 C24_2 C15_2 -135.6(8) . . . . ? C12_2 N11_2 C24_2 C23_2 -171.1(6) . . . . ? Ni2_2 N11_2 C24_2 C23_2 43.3(9) . . . . ? C14_2 C15_2 C24_2 N11_2 -8.7(16) . . . . ? C16_2 C15_2 C24_2 N11_2 165.7(10) . . . . ? C14_2 C15_2 C24_2 C23_2 172.4(11) . . . . ? C16_2 C15_2 C24_2 C23_2 -13.2(15) . . . . ? C22_2 C23_2 C24_2 N11_2 14.1(9) . . . . ? C18_2 C23_2 C24_2 N11_2 -168.1(6) . . . . ? C22_2 C23_2 C24_2 C15_2 -167.0(8) . . . . ? C18_2 C23_2 C24_2 C15_2 10.8(11) . . . . ? N11_2 C12_2 C25_2 N31_2 12.8(9) . . . . ? C13_2 C12_2 C25_2 N31_2 -162.0(7) . . . . ? C12_2 C25_2 N31_2 C31_2 177.9(6) . . . . ? C12_2 C25_2 N31_2 Ni2_2 7.9(8) . . . . ? C36_2 C31_2 N31_2 C25_2 -10.7(9) . . . . ? C32_2 C31_2 N31_2 C25_2 -136.6(6) . . . . ? C36_2 C31_2 N31_2 Ni2_2 159.5(4) . . . . ? C32_2 C31_2 N31_2 Ni2_2 33.5(6) . . . . ? N62_2 Ni2_2 N31_2 C25_2 68.8(5) . . . . ? N32_2 Ni2_2 N31_2 C25_2 161.1(5) . . . . ? N11_2 Ni2_2 N31_2 C25_2 -15.1(5) . . . . ? N41_2 Ni2_2 N31_2 C25_2 -120.2(5) . . . . ? N62_2 Ni2_2 N31_2 C31_2 -101.9(4) . . . . ? N32_2 Ni2_2 N31_2 C31_2 -9.6(4) . . . . ? N11_2 Ni2_2 N31_2 C31_2 174.2(4) . . . . ? N41_2 Ni2_2 N31_2 C31_2 69.1(4) . . . . ? N31_2 C31_2 C32_2 N32_2 -47.5(6) . . . . ? C36_2 C31_2 C32_2 N32_2 -176.8(5) . . . . ? N31_2 C31_2 C32_2 C33_2 -172.6(5) . . . . ? C36_2 C31_2 C32_2 C33_2 58.1(7) . . . . ? C31_2 C32_2 N32_2 Ni2_2 39.9(6) . . . . ? C33_2 C32_2 N32_2 Ni2_2 163.3(5) . . . . ? N61_2 Ni2_2 N32_2 C32_2 159.5(5) . . . . ? N31_2 Ni2_2 N32_2 C32_2 -17.7(5) . . . . ? N62_2 Ni2_2 N32_2 C32_2 76.7(5) . . . . ? N11_2 Ni2_2 N32_2 C32_2 -8.6(9) . . . . ? N41_2 Ni2_2 N32_2 C32_2 -126.6(5) . . . . ? N32_2 C32_2 C33_2 C34_2 -177.5(6) . . . . ? C31_2 C32_2 C33_2 C34_2 -55.3(7) . . . . ? C32_2 C33_2 C34_2 C35_2 54.9(9) . . . . ? C33_2 C34_2 C35_2 C36_2 -54.9(9) . . . . ? N31_2 C31_2 C36_2 C35_2 179.5(5) . . . . ? C32_2 C31_2 C36_2 C35_2 -56.6(7) . . . . ? C34_2 C35_2 C36_2 C31_2 55.5(8) . . . . ? N61_2 Ni2_2 N41_2 C54_2 168.7(6) . . . . ? N31_2 Ni2_2 N41_2 C54_2 -12.2(6) . . . . ? N62_2 Ni2_2 N41_2 C54_2 145.0(6) . . . . ? N32_2 Ni2_2 N41_2 C54_2 65.2(6) . . . . ? N11_2 Ni2_2 N41_2 C54_2 -92.9(6) . . . . ? N61_2 Ni2_2 N41_2 C42_2 20.9(4) . . . . ? N31_2 Ni2_2 N41_2 C42_2 -160.0(4) . . . . ? N62_2 Ni2_2 N41_2 C42_2 -2.8(7) . . . . ? N32_2 Ni2_2 N41_2 C42_2 -82.6(4) . . . . ? N11_2 Ni2_2 N41_2 C42_2 119.3(4) . . . . ? C54_2 N41_2 C42_2 C43_2 -0.2(9) . . . . ? Ni2_2 N41_2 C42_2 C43_2 151.4(5) . . . . ? C54_2 N41_2 C42_2 C55_2 -175.9(5) . . . . ? Ni2_2 N41_2 C42_2 C55_2 -24.2(6) . . . . ? N41_2 C42_2 C43_2 C44_2 -5.1(9) . . . . ? C55_2 C42_2 C43_2 C44_2 170.6(6) . . . . ? C42_2 C43_2 C44_2 C45_2 3.6(10) . . . . ? C43_2 C44_2 C45_2 C54_2 2.8(10) . . . . ? C43_2 C44_2 C45_2 C46_2 -178.3(7) . . . . ? C44_2 C45_2 C46_2 C47_2 179.2(7) . . . . ? C54_2 C45_2 C46_2 C47_2 -1.9(10) . . . . ? C45_2 C46_2 C47_2 C48_2 1.5(12) . . . . ? C46_2 C47_2 C48_2 C49_2 -178.7(8) . . . . ? C46_2 C47_2 C48_2 C53_2 5.3(11) . . . . ? C47_2 C48_2 C49_2 C50_2 -175.7(8) . . . . ? C53_2 C48_2 C49_2 C50_2 0.3(12) . . . . ? C48_2 C49_2 C50_2 C51_2 6.0(13) . . . . ? C49_2 C50_2 C51_2 C52_2 -5.3(12) . . . . ? C50_2 C51_2 C52_2 C53_2 -1.7(11) . . . . ? C51_2 C52_2 C53_2 C48_2 7.6(10) . . . . ? C51_2 C52_2 C53_2 C54_2 -171.6(6) . . . . ? C49_2 C48_2 C53_2 C52_2 -6.9(10) . . . . ? C47_2 C48_2 C53_2 C52_2 169.3(7) . . . . ? C49_2 C48_2 C53_2 C54_2 172.3(6) . . . . ? C47_2 C48_2 C53_2 C54_2 -11.5(10) . . . . ? C42_2 N41_2 C54_2 C45_2 7.2(8) . . . . ? Ni2_2 N41_2 C54_2 C45_2 -135.8(5) . . . . ? C42_2 N41_2 C54_2 C53_2 -175.6(5) . . . . ? Ni2_2 N41_2 C54_2 C53_2 41.4(8) . . . . ? C44_2 C45_2 C54_2 N41_2 -8.3(9) . . . . ? C46_2 C45_2 C54_2 N41_2 172.7(6) . . . . ? C44_2 C45_2 C54_2 C53_2 174.4(6) . . . . ? C46_2 C45_2 C54_2 C53_2 -4.6(9) . . . . ? C52_2 C53_2 C54_2 N41_2 13.0(9) . . . . ? C48_2 C53_2 C54_2 N41_2 -166.1(6) . . . . ? C52_2 C53_2 C54_2 C45_2 -169.7(6) . . . . ? C48_2 C53_2 C54_2 C45_2 11.2(9) . . . . ? N41_2 C42_2 C55_2 N61_2 14.2(8) . . . . ? C43_2 C42_2 C55_2 N61_2 -161.6(6) . . . . ? C42_2 C55_2 N61_2 C61_2 179.2(5) . . . . ? C42_2 C55_2 N61_2 Ni2_2 9.0(7) . . . . ? C66_2 C61_2 N61_2 C55_2 -5.4(8) . . . . ? C62_2 C61_2 N61_2 C55_2 -129.7(6) . . . . ? C66_2 C61_2 N61_2 Ni2_2 165.3(4) . . . . ? C62_2 C61_2 N61_2 Ni2_2 41.0(5) . . . . ? N62_2 Ni2_2 N61_2 C55_2 153.7(5) . . . . ? N32_2 Ni2_2 N61_2 C55_2 62.0(5) . . . . ? N11_2 Ni2_2 N61_2 C55_2 -122.9(5) . . . . ? N41_2 Ni2_2 N61_2 C55_2 -16.9(5) . . . . ? N62_2 Ni2_2 N61_2 C61_2 -17.4(4) . . . . ? N32_2 Ni2_2 N61_2 C61_2 -109.1(4) . . . . ? N11_2 Ni2_2 N61_2 C61_2 66.1(4) . . . . ? N41_2 Ni2_2 N61_2 C61_2 172.0(4) . . . . ? N61_2 C61_2 C62_2 C63_2 -177.4(7) . . . . ? C66_2 C61_2 C62_2 C63_2 55.2(9) . . . . ? N61_2 C61_2 C62_2 N62_2 -49.1(7) . . . . ? C66_2 C61_2 C62_2 N62_2 -176.5(6) . . . . ? C63_2 C62_2 N62_2 Ni2_2 162.3(6) . . . . ? C61_2 C62_2 N62_2 Ni2_2 35.6(7) . . . . ? N61_2 Ni2_2 N62_2 C62_2 -11.1(4) . . . . ? N31_2 Ni2_2 N62_2 C62_2 170.3(4) . . . . ? N32_2 Ni2_2 N62_2 C62_2 89.7(4) . . . . ? N11_2 Ni2_2 N62_2 C62_2 -114.0(4) . . . . ? N41_2 Ni2_2 N62_2 C62_2 12.1(8) . . . . ? N62_2 C62_2 C63_2 C64_2 -174.7(8) . . . . ? C61_2 C62_2 C63_2 C64_2 -50.1(12) . . . . ? C62_2 C63_2 C64_2 C65_2 49.1(16) . . . . ? C63_2 C64_2 C65_2 C66_2 -52.3(15) . . . . ? C64_2 C65_2 C66_2 C61_2 56.3(9) . . . . ? N61_2 C61_2 C66_2 C65_2 -179.6(5) . . . . ? C62_2 C61_2 C66_2 C65_2 -58.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.666 _refine_diff_density_min -1.201 _refine_diff_density_rms 0.142 data_(R)-5 _database_code_depnum_ccdc_archive 'CCDC 846327' #TrackingRef '- output.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; DP-2-70-2 3,3'-bis(naphthoquinoline imine) binaphthyl Ni2 I4 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C48 H30 I4 N4 Ni2) (C H Cl3)3 ; _chemical_formula_sum 'C51 H33 Cl9 I4 N4 Ni2' _chemical_formula_weight 1645.88 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' I I -0.4742 1.8119 '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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6896(8) _cell_length_b 22.8266(16) _cell_length_c 11.9341(9) _cell_angle_alpha 90.00 _cell_angle_beta 118.9240(10) _cell_angle_gamma 90.00 _cell_volume 2787.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9457 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.25 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 3.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.752 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 24886 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.26 _reflns_number_total 12862 _reflns_number_gt 12403 _reflns_threshold_expression >2sigma(I) _reflns_Friedel_coverage 0.884 _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0300P)^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 0.007(10) _refine_ls_number_reflns 12862 _refine_ls_number_parameters 631 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0284 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0606 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 C1S C 0.2470(5) 0.3568(2) 0.6466(5) 0.0336(11) Uani 1 1 d . . . H1S H 0.2921 0.3896 0.6282 0.040 Uiso 1 1 calc R . . Cl1 Cl 0.08116(17) 0.36225(9) 0.5417(2) 0.0892(7) Uani 1 1 d . . . Cl2 Cl 0.2789(2) 0.36336(7) 0.80421(14) 0.0633(5) Uani 1 1 d . . . Cl3 Cl 0.30841(14) 0.28989(6) 0.62194(14) 0.0438(3) Uani 1 1 d . . . C2S C 0.2814(5) 0.3019(2) 0.1530(5) 0.0308(11) Uani 1 1 d . . . H2S H 0.3403 0.2711 0.1493 0.037 Uiso 1 1 calc R . . Cl4 Cl 0.32910(16) 0.37004(6) 0.12211(15) 0.0491(4) Uani 1 1 d . . . Cl5 Cl 0.11903(14) 0.28582(6) 0.03611(12) 0.0417(3) Uani 1 1 d . . . Cl6 Cl 0.29492(13) 0.30083(6) 0.30591(12) 0.0374(3) Uani 1 1 d . . . C3S C 0.7072(5) 0.3948(2) 0.1995(5) 0.0369(12) Uani 1 1 d . . . H3S H 0.6669 0.3570 0.2050 0.044 Uiso 1 1 calc R . . Cl7 Cl 0.59759(13) 0.43027(6) 0.05754(13) 0.0404(3) Uani 1 1 d . . . Cl8 Cl 0.73860(19) 0.43711(7) 0.33309(15) 0.0591(4) Uani 1 1 d . . . Cl9 Cl 0.85506(14) 0.37865(6) 0.19779(13) 0.0438(3) Uani 1 1 d . . . Ni1 Ni 0.45749(5) 0.54929(2) 0.59811(4) 0.01299(10) Uani 1 1 d . . . Ni2 Ni 0.33221(4) 0.65338(2) 0.76425(4) 0.01231(10) Uani 1 1 d . . . I1 I 0.42297(2) 0.443588(10) 0.49944(2) 0.01779(6) Uani 1 1 d . . . I2 I 0.42200(2) 0.745561(10) 0.91960(2) 0.01564(5) Uani 1 1 d . . . I3 I 0.55388(2) 0.646780(11) 0.75078(2) 0.01796(6) Uani 1 1 d . . . I4 I 0.30423(2) 0.537565(11) 0.70330(2) 0.01820(6) Uani 1 1 d . . . C11 C -0.0089(4) 0.64887(17) 0.2802(3) 0.0131(7) Uani 1 1 d . . . C12 C 0.1315(4) 0.64952(17) 0.3507(3) 0.0139(7) Uani 1 1 d . . . C13 C 0.1964(4) 0.59660(17) 0.3796(4) 0.0134(8) Uani 1 1 d . . . N13 N 0.3370(3) 0.59261(13) 0.4394(3) 0.0119(6) Uani 1 1 d . . . C14 C 0.1294(4) 0.54310(18) 0.3534(4) 0.0158(7) Uani 1 1 d . . . H14 H 0.1771 0.5075 0.3827 0.019 Uiso 1 1 calc R . . C15 C -0.0038(3) 0.54180(17) 0.2862(3) 0.0148(7) Uani 1 1 d . . . H15 H -0.0485 0.5053 0.2682 0.018 Uiso 1 1 calc R . . C16 C -0.0756(4) 0.59443(18) 0.2433(4) 0.0154(8) Uani 1 1 d . . . C17 C -0.2133(4) 0.59392(18) 0.1633(4) 0.0170(8) Uani 1 1 d . . . H17 H -0.2582 0.5576 0.1359 0.020 Uiso 1 1 calc R . . C18 C -0.2816(4) 0.6453(2) 0.1256(4) 0.0211(8) Uani 1 1 d . . . H18 H -0.3736 0.6446 0.0714 0.025 Uiso 1 1 calc R . . C19 C -0.2163(4) 0.69898(18) 0.1664(4) 0.0195(9) Uani 1 1 d . . . H19 H -0.2650 0.7344 0.1418 0.023 Uiso 1 1 calc R . . C20 C -0.0827(4) 0.70112(17) 0.2417(4) 0.0169(8) Uani 1 1 d . . . H20 H -0.0399 0.7379 0.2680 0.020 Uiso 1 1 calc R . . C21 C 0.2300(4) 0.73914(16) 0.3034(3) 0.0134(7) Uani 1 1 d . . . C22 C 0.2042(4) 0.70583(16) 0.3913(4) 0.0123(7) Uani 1 1 d . . . C23 C 0.2503(4) 0.72694(16) 0.5132(4) 0.0136(7) Uani 1 1 d . . . N23 N 0.2187(3) 0.69843(13) 0.6033(3) 0.0135(6) Uani 1 1 d . . . C24 C 0.3258(4) 0.77824(17) 0.5562(4) 0.0178(8) Uani 1 1 d . . . H24 H 0.3581 0.7909 0.6421 0.021 Uiso 1 1 calc R . . C25 C 0.3523(4) 0.80954(18) 0.4754(4) 0.0201(9) Uani 1 1 d . . . H25 H 0.4032 0.8442 0.5052 0.024 Uiso 1 1 calc R . . C26 C 0.3052(4) 0.79141(16) 0.3461(4) 0.0148(8) Uani 1 1 d . . . C27 C 0.3341(4) 0.82251(17) 0.2601(4) 0.0200(9) Uani 1 1 d . . . H27 H 0.3863 0.8569 0.2886 0.024 Uiso 1 1 calc R . . C28 C 0.2886(4) 0.80413(18) 0.1377(4) 0.0198(8) Uani 1 1 d . . . H28 H 0.3078 0.8259 0.0810 0.024 Uiso 1 1 calc R . . C29 C 0.2127(4) 0.75260(17) 0.0946(4) 0.0183(8) Uani 1 1 d . . . H29 H 0.1820 0.7396 0.0092 0.022 Uiso 1 1 calc R . . C30 C 0.1830(4) 0.72132(17) 0.1745(4) 0.0166(8) Uani 1 1 d . . . H30 H 0.1303 0.6872 0.1436 0.020 Uiso 1 1 calc R . . N31 N 0.5923(3) 0.56895(14) 0.5401(3) 0.0149(7) Uani 1 1 d . . . C32 C 0.5379(4) 0.60447(17) 0.4396(4) 0.0151(8) Uani 1 1 d . . . C33 C 0.6073(4) 0.62786(18) 0.3807(4) 0.0196(8) Uani 1 1 d . . . H33 H 0.5674 0.6551 0.3123 0.024 Uiso 1 1 calc R . . C34 C 0.7333(4) 0.61017(19) 0.4246(4) 0.0212(9) Uani 1 1 d . . . H34 H 0.7827 0.6255 0.3873 0.025 Uiso 1 1 calc R . . C35 C 0.7900(4) 0.56946(18) 0.5248(4) 0.0177(8) Uani 1 1 d . . . C36 C 0.9176(4) 0.54509(19) 0.5656(4) 0.0226(9) Uani 1 1 d . . . H36 H 0.9665 0.5579 0.5257 0.027 Uiso 1 1 calc R . . C37 C 0.9689(4) 0.50493(19) 0.6579(4) 0.0238(9) Uani 1 1 d . . . H37 H 1.0507 0.4877 0.6786 0.029 Uiso 1 1 calc R . . C38 C 0.9026(4) 0.48757(18) 0.7260(4) 0.0198(9) Uani 1 1 d . . . C39 C 0.9625(4) 0.4475(2) 0.8296(4) 0.0277(10) Uani 1 1 d . . . H39 H 1.0442 0.4305 0.8491 0.033 Uiso 1 1 calc R . . C40 C 0.9045(4) 0.4328(2) 0.9022(4) 0.0278(10) Uani 1 1 d . . . H40 H 0.9444 0.4050 0.9694 0.033 Uiso 1 1 calc R . . C41 C 0.7861(4) 0.45924(19) 0.8761(4) 0.0250(10) Uani 1 1 d . . . H41 H 0.7477 0.4507 0.9285 0.030 Uiso 1 1 calc R . . C42 C 0.7248(4) 0.49761(19) 0.7747(4) 0.0209(9) Uani 1 1 d . . . H42 H 0.6439 0.5147 0.7578 0.025 Uiso 1 1 calc R . . C43 C 0.7790(4) 0.51208(17) 0.6956(4) 0.0163(8) Uani 1 1 d . . . C44 C 0.7177(4) 0.55104(17) 0.5869(4) 0.0151(8) Uani 1 1 d . . . C45 C 0.3974(4) 0.61551(17) 0.3853(4) 0.0165(8) Uani 1 1 d . . . H45 H 0.3522 0.6392 0.3111 0.020 Uiso 1 1 calc R . . N51 N 0.1618(3) 0.65359(13) 0.7805(3) 0.0121(6) Uani 1 1 d . . . C52 C 0.0711(4) 0.68694(17) 0.6856(4) 0.0153(8) Uani 1 1 d . . . C53 C -0.0528(4) 0.69938(18) 0.6703(4) 0.0184(8) Uani 1 1 d . . . H53 H -0.1116 0.7244 0.6037 0.022 Uiso 1 1 calc R . . C54 C -0.0867(4) 0.67419(17) 0.7547(4) 0.0176(8) Uani 1 1 d . . . H54 H -0.1697 0.6820 0.7478 0.021 Uiso 1 1 calc R . . C55 C 0.0016(4) 0.63696(16) 0.8508(4) 0.0144(7) Uani 1 1 d . . . C56 C -0.0357(4) 0.60645(17) 0.9331(4) 0.0172(8) Uani 1 1 d . . . H56 H -0.1194 0.6132 0.9253 0.021 Uiso 1 1 calc R . . C57 C 0.0465(4) 0.56830(18) 1.0212(4) 0.0191(8) Uani 1 1 d . . . H57 H 0.0174 0.5460 1.0698 0.023 Uiso 1 1 calc R . . C58 C 0.1768(4) 0.56086(17) 1.0426(4) 0.0156(8) Uani 1 1 d . . . C59 C 0.2638(4) 0.52213(18) 1.1401(4) 0.0206(9) Uani 1 1 d . . . H59 H 0.2327 0.4987 1.1855 0.025 Uiso 1 1 calc R . . C60 C 0.3919(4) 0.51834(18) 1.1688(4) 0.0202(9) Uani 1 1 d . . . H60 H 0.4493 0.4923 1.2338 0.024 Uiso 1 1 calc R . . C61 C 0.4384(4) 0.55283(17) 1.1025(4) 0.0185(8) Uani 1 1 d . . . H61 H 0.5280 0.5510 1.1243 0.022 Uiso 1 1 calc R . . C62 C 0.3558(4) 0.58903(18) 1.0068(4) 0.0171(8) Uani 1 1 d . . . H62 H 0.3894 0.6121 0.9630 0.020 Uiso 1 1 calc R . . C63 C 0.2231(4) 0.59346(16) 0.9708(4) 0.0141(8) Uani 1 1 d . . . C64 C 0.1301(4) 0.62901(17) 0.8663(4) 0.0138(8) Uani 1 1 d . . . C65 C 0.1066(4) 0.70983(17) 0.5925(4) 0.0143(8) Uani 1 1 d . . . H65 H 0.0462 0.7333 0.5234 0.017 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 C1S 0.044(3) 0.026(2) 0.029(2) -0.0002(19) 0.015(2) -0.007(2) Cl1 0.0466(10) 0.0633(12) 0.1044(15) -0.0207(11) -0.0057(10) 0.0048(9) Cl2 0.1198(15) 0.0354(8) 0.0410(8) -0.0020(6) 0.0438(9) -0.0062(9) Cl3 0.0490(8) 0.0407(7) 0.0467(8) -0.0035(6) 0.0271(7) -0.0056(6) C2S 0.038(3) 0.016(2) 0.043(3) -0.006(2) 0.024(2) -0.0032(19) Cl4 0.0732(10) 0.0258(7) 0.0670(10) -0.0022(6) 0.0487(9) -0.0105(6) Cl5 0.0403(7) 0.0463(8) 0.0318(6) -0.0060(5) 0.0121(6) -0.0038(6) Cl6 0.0449(7) 0.0330(6) 0.0324(6) -0.0082(5) 0.0172(6) -0.0124(6) C3S 0.054(3) 0.028(3) 0.036(3) -0.011(2) 0.028(3) -0.018(2) Cl7 0.0447(7) 0.0376(7) 0.0472(7) -0.0055(6) 0.0289(6) -0.0047(6) Cl8 0.0896(12) 0.0490(9) 0.0487(8) -0.0239(7) 0.0414(8) -0.0204(8) Cl9 0.0446(8) 0.0390(7) 0.0432(7) -0.0080(6) 0.0176(6) -0.0067(6) Ni1 0.0123(2) 0.0125(2) 0.0164(2) 0.00078(18) 0.00866(19) 0.00024(18) Ni2 0.0115(2) 0.0120(2) 0.0149(2) 0.00094(18) 0.00753(18) 0.00081(18) I1 0.01922(12) 0.01178(11) 0.02221(12) 0.00007(10) 0.00990(10) 0.00266(10) I2 0.01626(12) 0.01336(12) 0.01661(11) -0.00120(9) 0.00740(9) 0.00027(10) I3 0.01615(12) 0.01836(12) 0.02200(12) -0.00361(10) 0.01130(10) -0.00128(10) I4 0.02036(13) 0.01529(12) 0.02590(13) -0.00162(10) 0.01668(11) -0.00177(10) C11 0.0161(17) 0.0168(18) 0.0087(16) -0.0014(14) 0.0079(14) -0.0008(16) C12 0.0177(18) 0.0136(18) 0.0134(17) -0.0010(15) 0.0099(15) -0.0016(15) C13 0.0129(18) 0.0162(19) 0.0146(18) 0.0044(14) 0.0093(15) 0.0017(15) N13 0.0118(15) 0.0122(15) 0.0118(15) -0.0015(12) 0.0057(13) -0.0013(12) C14 0.0197(19) 0.0123(18) 0.0177(18) -0.0003(15) 0.0108(15) -0.0009(15) C15 0.0141(17) 0.0133(18) 0.0183(18) -0.0013(15) 0.0089(15) -0.0061(15) C16 0.0138(18) 0.0183(19) 0.0162(19) -0.0005(15) 0.0089(16) -0.0019(15) C17 0.0170(19) 0.020(2) 0.018(2) -0.0020(15) 0.0110(16) -0.0032(16) C18 0.0091(17) 0.034(2) 0.0165(18) 0.0014(18) 0.0030(15) 0.0017(17) C19 0.017(2) 0.021(2) 0.022(2) 0.0065(16) 0.0101(17) 0.0044(16) C20 0.0172(19) 0.0148(19) 0.0167(19) 0.0022(14) 0.0066(16) -0.0007(15) C21 0.0153(18) 0.0102(18) 0.0164(17) 0.0029(14) 0.0091(14) 0.0028(14) C22 0.0102(17) 0.0110(18) 0.0170(18) 0.0009(14) 0.0078(15) 0.0014(14) C23 0.0152(18) 0.0121(18) 0.0140(18) 0.0031(13) 0.0076(15) 0.0024(14) N23 0.0164(16) 0.0107(15) 0.0145(15) -0.0023(12) 0.0084(13) -0.0020(12) C24 0.022(2) 0.0161(19) 0.0146(18) -0.0009(15) 0.0085(16) -0.0038(16) C25 0.025(2) 0.017(2) 0.022(2) -0.0021(16) 0.0138(18) -0.0085(17) C26 0.0153(18) 0.0124(18) 0.0164(18) 0.0011(14) 0.0075(15) -0.0024(15) C27 0.026(2) 0.0127(19) 0.022(2) -0.0018(15) 0.0122(17) -0.0059(16) C28 0.025(2) 0.018(2) 0.021(2) 0.0001(16) 0.0150(17) -0.0012(17) C29 0.022(2) 0.017(2) 0.0143(17) 0.0010(15) 0.0077(16) 0.0012(16) C30 0.019(2) 0.0121(18) 0.0168(19) -0.0014(14) 0.0077(16) -0.0014(15) N31 0.0168(16) 0.0137(16) 0.0175(16) -0.0022(13) 0.0108(14) -0.0025(13) C32 0.0139(18) 0.0175(19) 0.0145(18) -0.0012(14) 0.0073(15) -0.0004(15) C33 0.019(2) 0.025(2) 0.0176(19) -0.0022(16) 0.0103(16) -0.0058(16) C34 0.019(2) 0.027(2) 0.020(2) -0.0058(17) 0.0115(17) -0.0099(17) C35 0.0148(19) 0.023(2) 0.0153(18) -0.0073(15) 0.0076(16) -0.0047(16) C36 0.018(2) 0.028(2) 0.031(2) -0.0089(18) 0.0189(18) -0.0055(17) C37 0.014(2) 0.028(2) 0.027(2) -0.0108(18) 0.0086(17) -0.0020(17) C38 0.0138(19) 0.018(2) 0.025(2) -0.0077(16) 0.0068(17) -0.0041(15) C39 0.019(2) 0.023(2) 0.035(2) 0.0011(19) 0.0089(18) 0.0059(18) C40 0.025(2) 0.021(2) 0.030(2) 0.0071(18) 0.0079(19) 0.0046(18) C41 0.020(2) 0.022(2) 0.029(2) 0.0036(17) 0.0092(18) -0.0010(17) C42 0.0146(19) 0.022(2) 0.025(2) -0.0026(17) 0.0086(17) 0.0005(16) C43 0.0136(18) 0.0147(19) 0.0196(19) -0.0045(15) 0.0071(15) -0.0019(15) C44 0.0129(18) 0.0159(19) 0.0161(18) -0.0061(14) 0.0069(15) -0.0022(15) C45 0.019(2) 0.0134(19) 0.0160(18) 0.0017(15) 0.0072(16) 0.0008(15) N51 0.0095(14) 0.0125(15) 0.0140(14) -0.0011(12) 0.0055(12) -0.0028(12) C52 0.0138(18) 0.0162(19) 0.0164(19) 0.0002(15) 0.0077(15) 0.0028(15) C53 0.0149(19) 0.021(2) 0.0181(19) 0.0024(15) 0.0072(16) 0.0046(16) C54 0.0139(18) 0.0168(19) 0.026(2) -0.0002(16) 0.0123(17) 0.0010(15) C55 0.0144(18) 0.0128(18) 0.0174(18) -0.0013(14) 0.0088(15) -0.0024(15) C56 0.0111(18) 0.021(2) 0.023(2) -0.0041(16) 0.0108(16) -0.0036(15) C57 0.021(2) 0.023(2) 0.020(2) -0.0034(16) 0.0145(17) -0.0078(17) C58 0.020(2) 0.0131(18) 0.0151(18) -0.0030(14) 0.0098(16) -0.0016(15) C59 0.030(2) 0.022(2) 0.0132(18) 0.0016(15) 0.0131(17) -0.0018(17) C60 0.021(2) 0.017(2) 0.0179(19) 0.0036(15) 0.0056(17) 0.0016(16) C61 0.0179(19) 0.017(2) 0.0163(18) -0.0002(15) 0.0050(16) -0.0008(15) C62 0.017(2) 0.017(2) 0.0173(19) 0.0006(15) 0.0084(16) -0.0022(15) C63 0.0192(19) 0.0113(17) 0.0156(18) -0.0019(14) 0.0114(16) 0.0001(15) C64 0.0145(18) 0.0127(18) 0.0180(18) -0.0040(14) 0.0108(15) -0.0028(14) C65 0.0105(17) 0.0148(19) 0.0160(18) 0.0021(14) 0.0052(15) 0.0021(14) _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 C1S Cl1 1.730(5) . ? C1S Cl2 1.738(5) . ? C1S Cl3 1.771(5) . ? C1S H1S 1.0000 . ? C2S Cl4 1.751(5) . ? C2S Cl6 1.754(5) . ? C2S Cl5 1.767(5) . ? C2S H2S 1.0000 . ? C3S Cl8 1.745(5) . ? C3S Cl7 1.751(6) . ? C3S Cl9 1.776(6) . ? C3S H3S 1.0000 . ? Ni1 N13 1.992(3) . ? Ni1 N31 2.054(3) . ? Ni1 I1 2.6290(5) . ? Ni1 I4 2.6519(5) . ? Ni1 I3 2.7487(5) . ? Ni2 N23 2.011(3) . ? Ni2 N51 2.093(3) . ? Ni2 I2 2.6615(5) . ? Ni2 I3 2.6770(6) . ? Ni2 I4 2.7195(6) . ? C11 C20 1.412(5) . ? C11 C16 1.419(5) . ? C11 C12 1.437(5) . ? C12 C13 1.379(5) . ? C12 C22 1.487(5) . ? C13 C14 1.402(5) . ? C13 N13 1.444(5) . ? N13 C45 1.278(5) . ? C14 C15 1.365(5) . ? C14 H14 0.9500 . ? C15 C16 1.412(6) . ? C15 H15 0.9500 . ? C16 C17 1.420(5) . ? C17 C18 1.367(6) . ? C17 H17 0.9500 . ? C18 C19 1.401(6) . ? C18 H18 0.9500 . ? C19 C20 1.375(6) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C30 1.419(5) . ? C21 C26 1.423(5) . ? C21 C22 1.441(5) . ? C22 C23 1.371(5) . ? C23 C24 1.405(5) . ? C23 N23 1.449(5) . ? N23 C65 1.280(5) . ? C24 C25 1.351(5) . ? C24 H24 0.9500 . ? C25 C26 1.426(5) . ? C25 H25 0.9500 . ? C26 C27 1.417(5) . ? C27 C28 1.357(6) . ? C27 H27 0.9500 . ? C28 C29 1.412(6) . ? C28 H28 0.9500 . ? C29 C30 1.364(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? N31 C32 1.327(5) . ? N31 C44 1.356(5) . ? C32 C33 1.411(5) . ? C32 C45 1.466(5) . ? C33 C34 1.364(6) . ? C33 H33 0.9500 . ? C34 C35 1.402(6) . ? C34 H34 0.9500 . ? C35 C44 1.431(5) . ? C35 C36 1.438(6) . ? C36 C37 1.332(6) . ? C36 H36 0.9500 . ? C37 C38 1.424(6) . ? C37 H37 0.9500 . ? C38 C39 1.421(6) . ? C38 C43 1.423(5) . ? C39 C40 1.374(7) . ? C39 H39 0.9500 . ? C40 C41 1.400(6) . ? C40 H40 0.9500 . ? C41 C42 1.381(6) . ? C41 H41 0.9500 . ? C42 C43 1.407(6) . ? C42 H42 0.9500 . ? C43 C44 1.445(5) . ? C45 H45 0.9500 . ? N51 C52 1.351(5) . ? N51 C64 1.366(5) . ? C52 C53 1.398(5) . ? C52 C65 1.458(5) . ? C53 C54 1.374(6) . ? C53 H53 0.9500 . ? C54 C55 1.399(5) . ? C54 H54 0.9500 . ? C55 C56 1.433(5) . ? C55 C64 1.434(5) . ? C56 C57 1.345(6) . ? C56 H56 0.9500 . ? C57 C58 1.426(6) . ? C57 H57 0.9500 . ? C58 C59 1.423(5) . ? C58 C63 1.425(5) . ? C59 C60 1.368(6) . ? C59 H59 0.9500 . ? C60 C61 1.399(6) . ? C60 H60 0.9500 . ? C61 C62 1.361(5) . ? C61 H61 0.9500 . ? C62 C63 1.399(5) . ? C62 H62 0.9500 . ? C63 C64 1.444(5) . ? C65 H65 0.9500 . ? 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 Cl1 C1S Cl2 110.8(3) . . ? Cl1 C1S Cl3 110.2(3) . . ? Cl2 C1S Cl3 111.2(3) . . ? Cl1 C1S H1S 108.2 . . ? Cl2 C1S H1S 108.2 . . ? Cl3 C1S H1S 108.2 . . ? Cl4 C2S Cl6 110.7(3) . . ? Cl4 C2S Cl5 110.4(3) . . ? Cl6 C2S Cl5 109.9(3) . . ? Cl4 C2S H2S 108.6 . . ? Cl6 C2S H2S 108.6 . . ? Cl5 C2S H2S 108.6 . . ? Cl8 C3S Cl7 111.1(3) . . ? Cl8 C3S Cl9 110.5(3) . . ? Cl7 C3S Cl9 110.2(3) . . ? Cl8 C3S H3S 108.3 . . ? Cl7 C3S H3S 108.3 . . ? Cl9 C3S H3S 108.3 . . ? N13 Ni1 N31 82.88(13) . . ? N13 Ni1 I1 98.34(9) . . ? N31 Ni1 I1 91.50(9) . . ? N13 Ni1 I4 99.85(9) . . ? N31 Ni1 I4 170.28(9) . . ? I1 Ni1 I4 97.289(17) . . ? N13 Ni1 I3 95.91(9) . . ? N31 Ni1 I3 84.90(9) . . ? I1 Ni1 I3 164.76(2) . . ? I4 Ni1 I3 85.537(16) . . ? N23 Ni2 N51 82.50(13) . . ? N23 Ni2 I2 96.71(9) . . ? N51 Ni2 I2 90.35(8) . . ? N23 Ni2 I3 100.48(10) . . ? N51 Ni2 I3 176.50(9) . . ? I2 Ni2 I3 91.105(16) . . ? N23 Ni2 I4 107.65(9) . . ? N51 Ni2 I4 91.73(8) . . ? I2 Ni2 I4 155.61(2) . . ? I3 Ni2 I4 85.634(15) . . ? Ni2 I3 Ni1 89.255(16) . . ? Ni1 I4 Ni2 90.407(16) . . ? C20 C11 C16 118.7(3) . . ? C20 C11 C12 121.8(3) . . ? C16 C11 C12 119.4(3) . . ? C13 C12 C11 118.2(3) . . ? C13 C12 C22 121.1(3) . . ? C11 C12 C22 120.7(3) . . ? C12 C13 C14 121.8(3) . . ? C12 C13 N13 122.4(3) . . ? C14 C13 N13 115.8(3) . . ? C45 N13 C13 120.0(3) . . ? C45 N13 Ni1 112.0(3) . . ? C13 N13 Ni1 127.9(2) . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 119.5(3) . . ? C15 C16 C17 121.2(4) . . ? C11 C16 C17 119.3(4) . . ? C18 C17 C16 120.4(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.2(3) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 120.9(4) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C11 120.3(4) . . ? C19 C20 H20 119.8 . . ? C11 C20 H20 119.8 . . ? C30 C21 C26 118.5(3) . . ? C30 C21 C22 122.0(3) . . ? C26 C21 C22 119.5(3) . . ? C23 C22 C21 118.3(3) . . ? C23 C22 C12 121.3(3) . . ? C21 C22 C12 120.4(3) . . ? C22 C23 C24 122.4(4) . . ? C22 C23 N23 121.3(3) . . ? C24 C23 N23 116.3(3) . . ? C65 N23 C23 116.7(3) . . ? C65 N23 Ni2 111.7(3) . . ? C23 N23 Ni2 130.7(2) . . ? C25 C24 C23 120.0(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 121.1(4) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C21 118.9(3) . . ? C27 C26 C25 122.4(3) . . ? C21 C26 C25 118.7(3) . . ? C28 C27 C26 121.2(4) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 120.0(4) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.6(4) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C21 120.8(4) . . ? C29 C30 H30 119.6 . . ? C21 C30 H30 119.6 . . ? C32 N31 C44 120.4(3) . . ? C32 N31 Ni1 109.1(3) . . ? C44 N31 Ni1 130.5(3) . . ? N31 C32 C33 122.8(4) . . ? N31 C32 C45 116.7(3) . . ? C33 C32 C45 120.3(4) . . ? C34 C33 C32 118.1(4) . . ? C34 C33 H33 121.0 . . ? C32 C33 H33 121.0 . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C44 118.8(4) . . ? C34 C35 C36 122.0(4) . . ? C44 C35 C36 119.1(4) . . ? C37 C36 C35 121.6(4) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 C38 120.9(4) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C39 C38 C43 119.2(4) . . ? C39 C38 C37 120.1(4) . . ? C43 C38 C37 120.7(4) . . ? C40 C39 C38 121.3(4) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 119.4(4) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C42 C41 C40 120.4(4) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 121.7(4) . . ? C41 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C42 C43 C38 117.9(4) . . ? C42 C43 C44 123.9(4) . . ? C38 C43 C44 118.2(4) . . ? N31 C44 C35 119.4(4) . . ? N31 C44 C43 121.5(4) . . ? C35 C44 C43 119.1(3) . . ? N13 C45 C32 118.7(3) . . ? N13 C45 H45 120.6 . . ? C32 C45 H45 120.6 . . ? C52 N51 C64 118.2(3) . . ? C52 N51 Ni2 108.7(2) . . ? C64 N51 Ni2 133.1(2) . . ? N51 C52 C53 124.6(4) . . ? N51 C52 C65 116.3(3) . . ? C53 C52 C65 119.1(3) . . ? C54 C53 C52 117.8(4) . . ? C54 C53 H53 121.1 . . ? C52 C53 H53 121.1 . . ? C53 C54 C55 119.7(4) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C54 C55 C56 120.5(4) . . ? C54 C55 C64 119.6(3) . . ? C56 C55 C64 119.8(3) . . ? C57 C56 C55 120.7(4) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C56 C57 C58 121.0(4) . . ? C56 C57 H57 119.5 . . ? C58 C57 H57 119.5 . . ? C59 C58 C63 119.1(4) . . ? C59 C58 C57 120.0(4) . . ? C63 C58 C57 120.9(4) . . ? C60 C59 C58 120.5(4) . . ? C60 C59 H59 119.7 . . ? C58 C59 H59 119.7 . . ? C59 C60 C61 120.0(4) . . ? C59 C60 H60 120.0 . . ? C61 C60 H60 120.0 . . ? C62 C61 C60 120.3(4) . . ? C62 C61 H61 119.9 . . ? C60 C61 H61 119.9 . . ? C61 C62 C63 122.2(4) . . ? C61 C62 H62 118.9 . . ? C63 C62 H62 118.9 . . ? C62 C63 C58 117.7(4) . . ? C62 C63 C64 124.4(4) . . ? C58 C63 C64 117.8(3) . . ? N51 C64 C55 119.9(3) . . ? N51 C64 C63 121.0(3) . . ? C55 C64 C63 119.1(3) . . ? N23 C65 C52 120.4(3) . . ? N23 C65 H65 119.8 . . ? C52 C65 H65 119.8 . . ? 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 N23 Ni2 I3 Ni1 -84.96(9) . . . . ? I2 Ni2 I3 Ni1 178.006(16) . . . . ? I4 Ni2 I3 Ni1 22.207(15) . . . . ? N13 Ni1 I3 Ni2 76.66(9) . . . . ? N31 Ni1 I3 Ni2 158.95(9) . . . . ? I1 Ni1 I3 Ni2 -124.21(8) . . . . ? I4 Ni1 I3 Ni2 -22.807(15) . . . . ? N13 Ni1 I4 Ni2 -72.81(9) . . . . ? I1 Ni1 I4 Ni2 -172.627(16) . . . . ? I3 Ni1 I4 Ni2 22.430(15) . . . . ? N23 Ni2 I4 Ni1 76.56(10) . . . . ? N51 Ni2 I4 Ni1 159.25(8) . . . . ? I2 Ni2 I4 Ni1 -106.08(5) . . . . ? I3 Ni2 I4 Ni1 -23.062(16) . . . . ? C20 C11 C12 C13 -177.1(4) . . . . ? C16 C11 C12 C13 0.2(5) . . . . ? C20 C11 C12 C22 3.0(5) . . . . ? C16 C11 C12 C22 -179.7(3) . . . . ? C11 C12 C13 C14 -6.4(5) . . . . ? C22 C12 C13 C14 173.5(4) . . . . ? C11 C12 C13 N13 174.1(3) . . . . ? C22 C12 C13 N13 -6.0(5) . . . . ? C12 C13 N13 C45 -58.6(5) . . . . ? C14 C13 N13 C45 121.9(4) . . . . ? C12 C13 N13 Ni1 126.3(3) . . . . ? C14 C13 N13 Ni1 -53.2(5) . . . . ? N31 Ni1 N13 C45 -5.6(3) . . . . ? I1 Ni1 N13 C45 -96.1(3) . . . . ? I4 Ni1 N13 C45 165.0(2) . . . . ? I3 Ni1 N13 C45 78.5(3) . . . . ? N31 Ni1 N13 C13 169.9(3) . . . . ? I1 Ni1 N13 C13 79.4(3) . . . . ? I4 Ni1 N13 C13 -19.6(3) . . . . ? I3 Ni1 N13 C13 -106.1(3) . . . . ? C12 C13 C14 C15 6.7(6) . . . . ? N13 C13 C14 C15 -173.7(3) . . . . ? C13 C14 C15 C16 -0.5(6) . . . . ? C14 C15 C16 C11 -5.5(5) . . . . ? C14 C15 C16 C17 174.2(4) . . . . ? C20 C11 C16 C15 -176.9(4) . . . . ? C12 C11 C16 C15 5.7(5) . . . . ? C20 C11 C16 C17 3.4(5) . . . . ? C12 C11 C16 C17 -174.1(3) . . . . ? C15 C16 C17 C18 178.2(4) . . . . ? C11 C16 C17 C18 -2.1(6) . . . . ? C16 C17 C18 C19 -0.6(6) . . . . ? C17 C18 C19 C20 1.9(6) . . . . ? C18 C19 C20 C11 -0.6(6) . . . . ? C16 C11 C20 C19 -2.1(6) . . . . ? C12 C11 C20 C19 175.3(4) . . . . ? C30 C21 C22 C23 -178.3(4) . . . . ? C26 C21 C22 C23 2.0(5) . . . . ? C30 C21 C22 C12 2.7(5) . . . . ? C26 C21 C22 C12 -176.9(3) . . . . ? C13 C12 C22 C23 -81.2(5) . . . . ? C11 C12 C22 C23 98.7(4) . . . . ? C13 C12 C22 C21 97.7(4) . . . . ? C11 C12 C22 C21 -82.4(4) . . . . ? C21 C22 C23 C24 -2.7(6) . . . . ? C12 C22 C23 C24 176.2(4) . . . . ? C21 C22 C23 N23 174.7(3) . . . . ? C12 C22 C23 N23 -6.4(5) . . . . ? C22 C23 N23 C65 -80.4(5) . . . . ? C24 C23 N23 C65 97.1(4) . . . . ? C22 C23 N23 Ni2 111.2(4) . . . . ? C24 C23 N23 Ni2 -71.2(4) . . . . ? N51 Ni2 N23 C65 5.3(3) . . . . ? I2 Ni2 N23 C65 -84.1(3) . . . . ? I3 Ni2 N23 C65 -176.5(2) . . . . ? I4 Ni2 N23 C65 94.8(3) . . . . ? N51 Ni2 N23 C23 174.1(3) . . . . ? I2 Ni2 N23 C23 84.6(3) . . . . ? I3 Ni2 N23 C23 -7.7(3) . . . . ? I4 Ni2 N23 C23 -96.5(3) . . . . ? C22 C23 C24 C25 1.8(6) . . . . ? N23 C23 C24 C25 -175.7(4) . . . . ? C23 C24 C25 C26 -0.2(6) . . . . ? C30 C21 C26 C27 -2.1(6) . . . . ? C22 C21 C26 C27 177.6(4) . . . . ? C30 C21 C26 C25 179.8(4) . . . . ? C22 C21 C26 C25 -0.5(5) . . . . ? C24 C25 C26 C27 -178.4(4) . . . . ? C24 C25 C26 C21 -0.4(6) . . . . ? C21 C26 C27 C28 1.7(6) . . . . ? C25 C26 C27 C28 179.7(4) . . . . ? C26 C27 C28 C29 -1.0(6) . . . . ? C27 C28 C29 C30 0.8(6) . . . . ? C28 C29 C30 C21 -1.3(6) . . . . ? C26 C21 C30 C29 2.0(6) . . . . ? C22 C21 C30 C29 -177.7(4) . . . . ? N13 Ni1 N31 C32 6.8(3) . . . . ? I1 Ni1 N31 C32 105.0(2) . . . . ? I3 Ni1 N31 C32 -89.8(2) . . . . ? N13 Ni1 N31 C44 -172.3(3) . . . . ? I1 Ni1 N31 C44 -74.1(3) . . . . ? I3 Ni1 N31 C44 91.0(3) . . . . ? C44 N31 C32 C33 -3.4(6) . . . . ? Ni1 N31 C32 C33 177.3(3) . . . . ? C44 N31 C32 C45 172.3(3) . . . . ? Ni1 N31 C32 C45 -6.9(4) . . . . ? N31 C32 C33 C34 4.1(6) . . . . ? C45 C32 C33 C34 -171.5(4) . . . . ? C32 C33 C34 C35 0.6(6) . . . . ? C33 C34 C35 C44 -5.5(6) . . . . ? C33 C34 C35 C36 173.6(4) . . . . ? C34 C35 C36 C37 -177.7(4) . . . . ? C44 C35 C36 C37 1.4(6) . . . . ? C35 C36 C37 C38 -4.4(6) . . . . ? C36 C37 C38 C39 -176.0(4) . . . . ? C36 C37 C38 C43 1.0(6) . . . . ? C43 C38 C39 C40 -1.2(6) . . . . ? C37 C38 C39 C40 175.8(4) . . . . ? C38 C39 C40 C41 -2.0(7) . . . . ? C39 C40 C41 C42 3.0(7) . . . . ? C40 C41 C42 C43 -0.8(6) . . . . ? C41 C42 C43 C38 -2.3(6) . . . . ? C41 C42 C43 C44 178.8(4) . . . . ? C39 C38 C43 C42 3.3(6) . . . . ? C37 C38 C43 C42 -173.7(4) . . . . ? C39 C38 C43 C44 -177.7(4) . . . . ? C37 C38 C43 C44 5.3(6) . . . . ? C32 N31 C44 C35 -1.7(5) . . . . ? Ni1 N31 C44 C35 177.3(3) . . . . ? C32 N31 C44 C43 -179.6(3) . . . . ? Ni1 N31 C44 C43 -0.5(5) . . . . ? C34 C35 C44 N31 6.1(5) . . . . ? C36 C35 C44 N31 -173.0(3) . . . . ? C34 C35 C44 C43 -176.0(3) . . . . ? C36 C35 C44 C43 4.9(5) . . . . ? C42 C43 C44 N31 -11.3(6) . . . . ? C38 C43 C44 N31 169.8(3) . . . . ? C42 C43 C44 C35 170.8(4) . . . . ? C38 C43 C44 C35 -8.1(5) . . . . ? C13 N13 C45 C32 -172.4(3) . . . . ? Ni1 N13 C45 C32 3.5(4) . . . . ? N31 C32 C45 N13 2.6(5) . . . . ? C33 C32 C45 N13 178.5(4) . . . . ? N23 Ni2 N51 C52 -5.4(2) . . . . ? I2 Ni2 N51 C52 91.3(2) . . . . ? I4 Ni2 N51 C52 -113.0(2) . . . . ? N23 Ni2 N51 C64 176.7(3) . . . . ? I2 Ni2 N51 C64 -86.6(3) . . . . ? I4 Ni2 N51 C64 69.1(3) . . . . ? C64 N51 C52 C53 1.6(6) . . . . ? Ni2 N51 C52 C53 -176.7(3) . . . . ? C64 N51 C52 C65 -177.0(3) . . . . ? Ni2 N51 C52 C65 4.7(4) . . . . ? N51 C52 C53 C54 -2.6(6) . . . . ? C65 C52 C53 C54 176.0(4) . . . . ? C52 C53 C54 C55 -0.7(6) . . . . ? C53 C54 C55 C56 -174.8(4) . . . . ? C53 C54 C55 C64 4.7(6) . . . . ? C54 C55 C56 C57 176.5(4) . . . . ? C64 C55 C56 C57 -3.0(6) . . . . ? C55 C56 C57 C58 5.4(6) . . . . ? C56 C57 C58 C59 177.3(4) . . . . ? C56 C57 C58 C63 -0.3(6) . . . . ? C63 C58 C59 C60 3.2(6) . . . . ? C57 C58 C59 C60 -174.5(4) . . . . ? C58 C59 C60 C61 0.2(6) . . . . ? C59 C60 C61 C62 -1.8(6) . . . . ? C60 C61 C62 C63 0.0(6) . . . . ? C61 C62 C63 C58 3.3(6) . . . . ? C61 C62 C63 C64 -177.0(4) . . . . ? C59 C58 C63 C62 -4.9(5) . . . . ? C57 C58 C63 C62 172.8(4) . . . . ? C59 C58 C63 C64 175.4(3) . . . . ? C57 C58 C63 C64 -7.0(5) . . . . ? C52 N51 C64 C55 2.6(5) . . . . ? Ni2 N51 C64 C55 -179.6(3) . . . . ? C52 N51 C64 C63 -179.3(3) . . . . ? Ni2 N51 C64 C63 -1.5(5) . . . . ? C54 C55 C64 N51 -5.7(5) . . . . ? C56 C55 C64 N51 173.8(3) . . . . ? C54 C55 C64 C63 176.1(3) . . . . ? C56 C55 C64 C63 -4.4(5) . . . . ? C62 C63 C64 N51 11.2(6) . . . . ? C58 C63 C64 N51 -169.0(3) . . . . ? C62 C63 C64 C55 -170.6(4) . . . . ? C58 C63 C64 C55 9.1(5) . . . . ? C23 N23 C65 C52 -174.9(3) . . . . ? Ni2 N23 C65 C52 -4.4(4) . . . . ? N51 C52 C65 N23 -0.4(5) . . . . ? C53 C52 C65 N23 -179.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.018 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.103 data_(R)-6 _database_code_depnum_ccdc_archive 'CCDC 846328' #TrackingRef '- output.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; DP-2-68-1 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; (C46 H38 I4 N4 Ni2) (C H2 Cl2)1.6 (O)1 ; _chemical_formula_sum 'C47.60 H41.20 Cl3.20 I4 N4 Ni2 O' _chemical_formula_weight 1423.71 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' I I -0.4742 1.8119 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.1481(14) _cell_length_b 22.485(3) _cell_length_c 19.246(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5257.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8060 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 27.85 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2741 _exptl_absorpt_coefficient_mu 3.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.393 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 36142 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_sigmaI/netI 0.0624 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.30 _reflns_number_total 12468 _reflns_number_gt 10178 _reflns_threshold_expression >2sigma(I) _reflns_Friedel_coverage 0.791 _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0800P)^2^+10.0000P] 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 0.03(3) _refine_ls_number_reflns 12468 _refine_ls_number_parameters 582 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.001 _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 C1S C 0.5515(15) 0.7878(9) 0.8073(11) 0.074(6) Uiso 0.60 1 d PD A 1 H1A H 0.5032 0.7523 0.8075 0.088 Uiso 0.60 1 calc PR A 1 H1B H 0.5707 0.7979 0.8559 0.088 Uiso 0.60 1 calc PR A 1 Cl1 Cl 0.6667(6) 0.7744(3) 0.7604(5) 0.121(3) Uani 0.60 1 d PD A 1 Cl2 Cl 0.4881(6) 0.8452(3) 0.7688(6) 0.121(3) Uani 0.60 1 d PD A 1 C2S C 0.4171(16) 0.7846(10) 0.9018(12) 0.050(6) Uiso 0.40 1 d PD B 2 H2A H 0.3915 0.7668 0.8576 0.060 Uiso 0.40 1 calc PR B 2 H2B H 0.3646 0.8164 0.9147 0.060 Uiso 0.40 1 calc PR B 2 Cl3 Cl 0.5466(6) 0.8158(5) 0.8890(5) 0.104(4) Uani 0.40 1 d PD B 2 Cl4 Cl 0.4169(8) 0.7289(4) 0.9677(5) 0.094(3) Uani 0.40 1 d PD B 2 C3S C 0.2317(14) 0.8290(8) 0.8789(7) 0.054(4) Uiso 0.60 1 d PD C 1 H3A H 0.1942 0.8657 0.8630 0.064 Uiso 0.60 1 calc PR C 1 H3B H 0.3052 0.8408 0.8964 0.064 Uiso 0.60 1 calc PR C 1 Cl5 Cl 0.2501(5) 0.7824(3) 0.8073(3) 0.0765(16) Uani 0.60 1 d PD C 1 Cl6 Cl 0.1565(5) 0.79937(18) 0.9482(3) 0.0667(14) Uani 0.60 1 d PD C 1 O1S O 0.1529(7) 0.2959(5) 0.5883(8) 0.144(7) Uani 1 1 d . . . Ni1 Ni 0.51429(8) 0.57817(5) 0.66266(7) 0.0397(3) Uani 1 1 d . . . Ni2 Ni 0.80307(8) 0.55146(5) 0.58621(7) 0.0390(3) Uani 1 1 d . . . I1 I 0.38490(5) 0.66913(3) 0.69906(4) 0.05160(19) Uani 1 1 d . . . I2 I 0.96107(5) 0.46940(3) 0.57261(4) 0.05240(19) Uani 1 1 d . . . I3 I 0.66712(4) 0.48633(2) 0.66174(4) 0.04311(16) Uani 1 1 d . . . I4 I 0.67709(4) 0.64789(2) 0.62376(3) 0.04080(15) Uani 1 1 d . . . C11 C 0.4755(8) 0.4562(4) 0.4356(5) 0.047(2) Uani 1 1 d . . . C12 C 0.5421(8) 0.5040(4) 0.4561(5) 0.043(2) Uani 1 1 d . . . C13 C 0.6497(7) 0.4929(4) 0.4778(5) 0.039(2) Uani 1 1 d . . . N13 N 0.7273(6) 0.5375(3) 0.4950(4) 0.0418(18) Uani 1 1 d . . . C14 C 0.6881(9) 0.4327(4) 0.4828(5) 0.048(2) Uani 1 1 d . . . H14 H 0.7614 0.4248 0.4974 0.057 Uiso 1 1 calc R . . C15 C 0.6205(8) 0.3877(4) 0.4669(5) 0.043(2) Uani 1 1 d . . . H15 H 0.6447 0.3479 0.4733 0.052 Uiso 1 1 calc R . . C16 C 0.5126(8) 0.3986(4) 0.4404(5) 0.047(2) Uani 1 1 d . . . C17 C 0.4436(10) 0.3503(5) 0.4214(7) 0.061(3) Uani 1 1 d . . . H17 H 0.4684 0.3106 0.4271 0.073 Uiso 1 1 calc R . . C18 C 0.3390(12) 0.3617(5) 0.3941(8) 0.073(4) Uani 1 1 d . . . H18 H 0.2933 0.3301 0.3785 0.088 Uiso 1 1 calc R . . C19 C 0.3035(12) 0.4203(6) 0.3904(8) 0.084(5) Uani 1 1 d . . . H19 H 0.2317 0.4282 0.3732 0.100 Uiso 1 1 calc R . . C20 C 0.3661(9) 0.4656(4) 0.4101(7) 0.063(3) Uani 1 1 d . . . H20 H 0.3380 0.5050 0.4071 0.075 Uiso 1 1 calc R . . C21 C 0.5011(9) 0.5974(4) 0.3870(6) 0.050(3) Uani 1 1 d . . . C22 C 0.4976(8) 0.5674(4) 0.4515(7) 0.054(3) Uani 1 1 d . . . C23 C 0.4463(8) 0.5920(4) 0.5063(6) 0.051(3) Uani 1 1 d . . . N23 N 0.4352(5) 0.5621(3) 0.5739(5) 0.0444(19) Uani 1 1 d . . . C24 C 0.3971(10) 0.6493(4) 0.5008(7) 0.059(3) Uani 1 1 d . . . H24 H 0.3624 0.6668 0.5400 0.071 Uiso 1 1 calc R . . C25 C 0.4002(10) 0.6788(4) 0.4393(7) 0.063(4) Uani 1 1 d . . . H25 H 0.3655 0.7166 0.4359 0.076 Uiso 1 1 calc R . . C26 C 0.4522(10) 0.6554(4) 0.3813(7) 0.061(3) Uani 1 1 d . . . C27 C 0.4561(11) 0.6845(5) 0.3164(8) 0.078(5) Uani 1 1 d . . . H27 H 0.4250 0.7231 0.3127 0.093 Uiso 1 1 calc R . . C28 C 0.5016(12) 0.6600(5) 0.2599(8) 0.073(4) Uani 1 1 d . . . H28 H 0.5006 0.6811 0.2172 0.088 Uiso 1 1 calc R . . C29 C 0.5514(10) 0.6030(5) 0.2630(7) 0.065(3) Uani 1 1 d . . . H29 H 0.5861 0.5861 0.2235 0.078 Uiso 1 1 calc R . . C30 C 0.5476(10) 0.5728(5) 0.3263(7) 0.064(3) Uani 1 1 d . . . H30 H 0.5778 0.5339 0.3286 0.076 Uiso 1 1 calc R . . N31 N 0.8892(6) 0.6132(3) 0.5315(4) 0.0422(19) Uani 1 1 d . . . C32 C 0.8511(7) 0.6166(4) 0.4682(5) 0.041(2) Uani 1 1 d . . . C33 C 0.8904(8) 0.6568(4) 0.4161(5) 0.043(2) Uani 1 1 d . . . H33 H 0.8614 0.6570 0.3702 0.052 Uiso 1 1 calc R . . C34 C 0.9711(8) 0.6945(5) 0.4358(6) 0.051(3) Uani 1 1 d . . . H34 H 0.9969 0.7233 0.4036 0.061 Uiso 1 1 calc R . . C35 C 1.0171(7) 0.6927(4) 0.5006(5) 0.043(2) Uani 1 1 d . . . C36 C 1.1044(7) 0.7297(4) 0.5213(6) 0.051(3) Uani 1 1 d . . . H36 H 1.1365 0.7555 0.4878 0.061 Uiso 1 1 calc R . . C37 C 1.1444(7) 0.7302(4) 0.5863(7) 0.052(3) Uani 1 1 d . . . H37 H 1.2030 0.7561 0.5990 0.062 Uiso 1 1 calc R . . C38 C 1.0963(7) 0.6909(4) 0.6355(6) 0.050(3) Uani 1 1 d . . . H38 H 1.1218 0.6929 0.6821 0.059 Uiso 1 1 calc R . . C39 C 1.0160(6) 0.6504(4) 0.6204(6) 0.041(2) Uani 1 1 d . . . C40 C 0.9735(7) 0.6515(4) 0.5510(6) 0.044(2) Uani 1 1 d . . . C41 C 0.7633(7) 0.5749(4) 0.4487(6) 0.046(2) Uani 1 1 d . . . H41 H 0.7332 0.5753 0.4032 0.056 Uiso 1 1 calc R . . C42 C 0.9784(6) 0.6122(4) 0.6798(5) 0.042(2) Uani 1 1 d . . . H42 H 0.9186 0.5859 0.6617 0.050 Uiso 1 1 calc R . . C43 C 0.9288(8) 0.6488(5) 0.7406(5) 0.050(2) Uani 1 1 d . . . H43A H 0.8703 0.6746 0.7228 0.075 Uiso 1 1 calc R . . H43B H 0.9865 0.6731 0.7620 0.075 Uiso 1 1 calc R . . H43C H 0.8981 0.6216 0.7754 0.075 Uiso 1 1 calc R . . C44 C 1.0710(8) 0.5718(5) 0.7049(7) 0.057(3) Uani 1 1 d . . . H44A H 1.1013 0.5497 0.6654 0.085 Uiso 1 1 calc R . . H44B H 1.0420 0.5437 0.7393 0.085 Uiso 1 1 calc R . . H44C H 1.1292 0.5959 0.7261 0.085 Uiso 1 1 calc R . . N51 N 0.4060(5) 0.5175(3) 0.7004(5) 0.0433(19) Uani 1 1 d . . . C52 C 0.3447(7) 0.4977(4) 0.6508(7) 0.056(3) Uani 1 1 d . . . C53 C 0.2626(8) 0.4520(5) 0.6597(8) 0.065(3) Uani 1 1 d . . . H53 H 0.2171 0.4398 0.6222 0.078 Uiso 1 1 calc R . . C54 C 0.2533(7) 0.4280(4) 0.7212(9) 0.073(4) Uani 1 1 d . . . H54 H 0.2005 0.3974 0.7282 0.088 Uiso 1 1 calc R . . C55 C 0.3185(7) 0.4461(4) 0.7768(7) 0.057(3) Uani 1 1 d . . . C56 C 0.3123(10) 0.4203(5) 0.8436(10) 0.081(5) Uani 1 1 d . . . H56 H 0.2608 0.3892 0.8516 0.097 Uiso 1 1 calc R . . C57 C 0.3788(12) 0.4388(5) 0.8978(8) 0.071(4) Uani 1 1 d . . . H57 H 0.3749 0.4207 0.9423 0.086 Uiso 1 1 calc R . . C58 C 0.4526(9) 0.4857(5) 0.8841(7) 0.063(3) Uani 1 1 d . . . H58 H 0.4968 0.4999 0.9213 0.075 Uiso 1 1 calc R . . C59 C 0.4647(9) 0.5123(4) 0.8200(6) 0.049(2) Uani 1 1 d . . . C60 C 0.3979(7) 0.4938(4) 0.7647(6) 0.050(3) Uani 1 1 d . . . C61 C 0.3588(7) 0.5236(4) 0.5823(7) 0.055(3) Uani 1 1 d . . . H61 H 0.3127 0.5123 0.5447 0.065 Uiso 1 1 calc R . . C62 C 0.5446(9) 0.5632(5) 0.8191(7) 0.058(3) Uani 1 1 d . . . H62 H 0.5481 0.5787 0.7705 0.069 Uiso 1 1 calc R . . C63 C 0.6611(10) 0.5418(7) 0.8392(7) 0.079(4) Uani 1 1 d . . . H63A H 0.6837 0.5095 0.8082 0.118 Uiso 1 1 calc R . . H63B H 0.6606 0.5274 0.8873 0.118 Uiso 1 1 calc R . . H63C H 0.7131 0.5750 0.8350 0.118 Uiso 1 1 calc R . . C64 C 0.5072(14) 0.6151(6) 0.8670(8) 0.081(4) Uani 1 1 d . . . H64A H 0.4343 0.6289 0.8523 0.122 Uiso 1 1 calc R . . H64B H 0.5600 0.6478 0.8636 0.122 Uiso 1 1 calc R . . H64C H 0.5035 0.6011 0.9151 0.122 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 Cl1 0.085(4) 0.075(4) 0.202(8) -0.076(5) 0.059(5) -0.026(3) Cl2 0.089(4) 0.061(4) 0.213(9) 0.022(5) -0.004(5) -0.030(3) Cl3 0.041(3) 0.159(10) 0.112(7) -0.098(7) 0.019(4) -0.020(5) Cl4 0.076(5) 0.084(6) 0.120(8) -0.054(6) -0.035(5) 0.027(5) Cl5 0.076(3) 0.076(4) 0.077(3) -0.034(3) -0.012(3) 0.028(3) Cl6 0.081(3) 0.028(2) 0.091(4) -0.005(2) 0.021(3) -0.024(2) O1S 0.040(4) 0.145(10) 0.247(14) -0.170(11) 0.040(7) -0.027(5) Ni1 0.0205(4) 0.0281(5) 0.0703(8) 0.0023(6) -0.0123(5) 0.0009(4) Ni2 0.0251(5) 0.0307(6) 0.0612(8) 0.0133(5) -0.0053(5) 0.0044(4) I1 0.0283(3) 0.0334(3) 0.0930(5) -0.0082(3) -0.0121(3) 0.0045(2) I2 0.0348(3) 0.0439(4) 0.0786(5) 0.0126(3) -0.0085(3) 0.0146(3) I3 0.0263(2) 0.0304(3) 0.0726(4) 0.0140(3) -0.0013(3) 0.0068(2) I4 0.0255(2) 0.0290(3) 0.0679(4) 0.0101(3) -0.0077(3) 0.0021(2) C11 0.054(5) 0.024(4) 0.062(6) 0.010(4) -0.023(5) -0.002(4) C12 0.043(5) 0.028(4) 0.058(6) 0.012(4) -0.013(4) 0.000(4) C13 0.040(5) 0.024(4) 0.052(5) 0.008(4) 0.002(4) 0.007(3) N13 0.031(3) 0.033(4) 0.062(5) -0.001(4) -0.003(3) 0.010(3) C14 0.045(5) 0.038(5) 0.060(6) 0.011(4) -0.001(5) 0.006(4) C15 0.048(5) 0.021(4) 0.060(6) 0.001(4) -0.006(5) 0.006(4) C16 0.046(5) 0.039(5) 0.056(6) 0.000(4) -0.002(4) 0.000(4) C17 0.062(6) 0.031(5) 0.090(9) 0.011(5) -0.003(6) -0.003(5) C18 0.083(9) 0.036(6) 0.100(10) 0.010(6) -0.021(8) -0.002(6) C19 0.076(9) 0.055(7) 0.120(12) 0.012(7) -0.056(8) -0.014(6) C20 0.064(7) 0.027(5) 0.097(9) 0.010(5) -0.048(6) 0.000(4) C21 0.055(6) 0.028(5) 0.068(7) 0.000(5) -0.033(5) -0.003(4) C22 0.037(4) 0.024(4) 0.099(9) 0.003(5) -0.032(5) 0.007(4) C23 0.047(5) 0.021(4) 0.083(8) -0.004(5) -0.034(5) -0.002(4) N23 0.023(3) 0.034(4) 0.076(6) 0.002(4) -0.013(4) 0.012(3) C24 0.064(6) 0.028(5) 0.085(8) -0.014(5) -0.039(6) 0.011(5) C25 0.067(7) 0.011(4) 0.112(10) 0.001(5) -0.048(7) 0.003(4) C26 0.077(7) 0.030(5) 0.077(8) -0.003(5) -0.051(7) 0.002(5) C27 0.085(9) 0.025(5) 0.123(12) 0.005(6) -0.069(9) 0.000(5) C28 0.083(9) 0.042(7) 0.094(10) 0.018(7) -0.048(8) -0.013(6) C29 0.064(7) 0.058(7) 0.073(8) 0.015(6) -0.036(6) -0.021(6) C30 0.063(6) 0.039(6) 0.089(9) 0.018(6) -0.038(7) -0.006(5) N31 0.021(3) 0.033(4) 0.073(6) 0.022(4) -0.001(3) 0.006(3) C32 0.037(4) 0.032(5) 0.053(6) 0.012(4) 0.000(4) 0.008(4) C33 0.044(5) 0.042(5) 0.044(5) 0.011(4) 0.012(4) 0.009(4) C34 0.038(5) 0.046(5) 0.069(7) 0.034(5) 0.015(5) 0.016(4) C35 0.028(4) 0.034(5) 0.066(6) 0.017(4) 0.008(4) 0.004(4) C36 0.028(4) 0.038(5) 0.088(8) 0.024(5) 0.013(5) 0.009(4) C37 0.024(4) 0.028(5) 0.102(9) 0.005(5) 0.016(5) 0.001(3) C38 0.027(4) 0.043(5) 0.079(7) 0.023(5) -0.007(4) -0.001(4) C39 0.014(3) 0.029(4) 0.079(7) 0.009(4) 0.008(4) 0.007(3) C40 0.028(4) 0.031(4) 0.073(7) 0.012(4) 0.013(4) 0.007(3) C41 0.035(4) 0.046(6) 0.058(6) 0.013(5) -0.009(4) 0.012(4) C42 0.022(4) 0.038(5) 0.065(6) 0.011(4) -0.009(4) -0.001(3) C43 0.037(5) 0.055(6) 0.057(6) 0.013(5) -0.003(4) -0.010(4) C44 0.045(5) 0.041(6) 0.084(8) 0.027(5) -0.019(5) 0.003(4) N51 0.023(3) 0.028(4) 0.080(6) -0.004(4) -0.006(4) -0.001(3) C52 0.026(4) 0.028(5) 0.113(9) 0.000(5) -0.010(5) 0.006(3) C53 0.033(5) 0.033(5) 0.128(11) -0.001(7) 0.002(6) -0.001(4) C54 0.021(4) 0.024(5) 0.175(15) 0.011(7) -0.010(6) -0.005(4) C55 0.025(4) 0.029(5) 0.118(10) 0.004(5) 0.012(5) 0.005(4) C56 0.041(6) 0.030(5) 0.173(15) 0.011(8) 0.038(8) 0.007(4) C57 0.074(8) 0.030(5) 0.109(11) 0.018(6) 0.037(8) 0.017(6) C58 0.054(6) 0.046(6) 0.089(9) 0.014(6) 0.017(6) 0.018(5) C59 0.050(5) 0.037(5) 0.062(7) 0.007(5) 0.000(5) 0.002(4) C60 0.024(4) 0.024(4) 0.101(8) -0.004(5) 0.012(5) 0.002(3) C61 0.034(4) 0.022(4) 0.108(9) -0.012(5) -0.025(5) 0.006(3) C62 0.043(5) 0.043(6) 0.087(9) 0.007(5) -0.003(5) 0.001(4) C63 0.057(7) 0.099(10) 0.080(8) 0.022(8) -0.030(7) -0.017(7) C64 0.100(11) 0.052(7) 0.091(10) 0.004(7) 0.016(9) -0.016(7) _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 C1S Cl2 1.677(17) . ? C1S Cl1 1.692(16) . ? C1S H1A 0.9900 . ? C1S H1B 0.9900 . ? C2S Cl3 1.740(17) . ? C2S Cl4 1.783(18) . ? C2S H2A 0.9900 . ? C2S H2B 0.9900 . ? C3S Cl5 1.747(14) . ? C3S Cl6 1.749(14) . ? C3S H3A 0.9900 . ? C3S H3B 0.9900 . ? Ni1 N23 1.993(8) . ? Ni1 N51 2.030(8) . ? Ni1 I4 2.6325(12) . ? Ni1 I1 2.6730(13) . ? Ni1 I3 2.7770(12) . ? Ni2 N13 2.007(8) . ? Ni2 N31 2.033(7) . ? Ni2 I3 2.6429(13) . ? Ni2 I2 2.6753(12) . ? Ni2 I4 2.7507(13) . ? C11 C16 1.375(13) . ? C11 C12 1.401(13) . ? C11 C20 1.432(13) . ? C12 C13 1.395(12) . ? C12 C22 1.527(12) . ? C13 N13 1.415(12) . ? C13 C14 1.434(12) . ? N13 C41 1.301(12) . ? C14 C15 1.340(14) . ? C14 H14 0.9500 . ? C15 C16 1.427(14) . ? C15 H15 0.9500 . ? C16 C17 1.419(14) . ? C17 C18 1.398(17) . ? C17 H17 0.9500 . ? C18 C19 1.387(17) . ? C18 H18 0.9500 . ? C19 C20 1.328(15) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C30 1.411(18) . ? C21 C22 1.413(16) . ? C21 C26 1.438(14) . ? C22 C23 1.344(17) . ? C23 C24 1.424(13) . ? C23 N23 1.472(14) . ? N23 C61 1.279(12) . ? C24 C25 1.356(17) . ? C24 H24 0.9500 . ? C25 C26 1.387(18) . ? C25 H25 0.9500 . ? C26 C27 1.410(19) . ? C27 C28 1.34(2) . ? C27 H27 0.9500 . ? C28 C29 1.419(18) . ? C28 H28 0.9500 . ? C29 C30 1.395(16) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? N31 C32 1.305(12) . ? N31 C40 1.389(12) . ? C32 C33 1.434(13) . ? C32 C41 1.468(14) . ? C33 C34 1.351(15) . ? C33 H33 0.9500 . ? C34 C35 1.367(15) . ? C34 H34 0.9500 . ? C35 C36 1.407(14) . ? C35 C40 1.442(12) . ? C36 C37 1.342(17) . ? C36 H36 0.9500 . ? C37 C38 1.421(14) . ? C37 H37 0.9500 . ? C38 C39 1.366(13) . ? C38 H38 0.9500 . ? C39 C40 1.432(15) . ? C39 C42 1.501(13) . ? C41 H41 0.9500 . ? C42 C44 1.525(12) . ? C42 C43 1.551(14) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? N51 C52 1.291(13) . ? N51 C60 1.351(14) . ? C52 C53 1.442(14) . ? C52 C61 1.452(18) . ? C53 C54 1.305(19) . ? C53 H53 0.9500 . ? C54 C55 1.392(18) . ? C54 H54 0.9500 . ? C55 C56 1.41(2) . ? C55 C60 1.463(13) . ? C56 C57 1.38(2) . ? C56 H56 0.9500 . ? C57 C58 1.409(17) . ? C57 H57 0.9500 . ? C58 C59 1.378(16) . ? C58 H58 0.9500 . ? C59 C60 1.400(15) . ? C59 C62 1.502(15) . ? C61 H61 0.9500 . ? C62 C63 1.544(16) . ? C62 C64 1.555(18) . ? C62 H62 1.0000 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 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 Cl2 C1S Cl1 106.3(12) . . ? Cl2 C1S H1A 110.5 . . ? Cl1 C1S H1A 110.5 . . ? Cl2 C1S H1B 110.5 . . ? Cl1 C1S H1B 110.5 . . ? H1A C1S H1B 108.7 . . ? Cl3 C2S Cl4 112.7(13) . . ? Cl3 C2S H2A 109.1 . . ? Cl4 C2S H2A 109.1 . . ? Cl3 C2S H2B 109.1 . . ? Cl4 C2S H2B 109.1 . . ? H2A C2S H2B 107.8 . . ? Cl5 C3S Cl6 116.1(10) . . ? Cl5 C3S H3A 108.3 . . ? Cl6 C3S H3A 108.3 . . ? Cl5 C3S H3B 108.3 . . ? Cl6 C3S H3B 108.3 . . ? H3A C3S H3B 107.4 . . ? N23 Ni1 N51 82.7(4) . . ? N23 Ni1 I4 103.1(2) . . ? N51 Ni1 I4 171.5(2) . . ? N23 Ni1 I1 94.6(2) . . ? N51 Ni1 I1 92.2(2) . . ? I4 Ni1 I1 93.48(4) . . ? N23 Ni1 I3 100.5(2) . . ? N51 Ni1 I3 86.3(2) . . ? I4 Ni1 I3 86.49(4) . . ? I1 Ni1 I3 164.55(6) . . ? N13 Ni2 N31 83.7(3) . . ? N13 Ni2 I3 96.2(2) . . ? N31 Ni2 I3 170.1(2) . . ? N13 Ni2 I2 97.8(2) . . ? N31 Ni2 I2 92.9(2) . . ? I3 Ni2 I2 96.89(4) . . ? N13 Ni2 I4 95.6(2) . . ? N31 Ni2 I4 83.3(2) . . ? I3 Ni2 I4 86.83(4) . . ? I2 Ni2 I4 165.60(5) . . ? Ni2 I3 Ni1 90.53(4) . . ? Ni1 I4 Ni2 91.33(4) . . ? C16 C11 C12 120.9(9) . . ? C16 C11 C20 117.8(9) . . ? C12 C11 C20 121.3(8) . . ? C13 C12 C11 119.2(8) . . ? C13 C12 C22 121.0(8) . . ? C11 C12 C22 119.7(8) . . ? C12 C13 N13 124.6(8) . . ? C12 C13 C14 119.5(9) . . ? N13 C13 C14 115.9(8) . . ? C41 N13 C13 121.5(9) . . ? C41 N13 Ni2 110.1(7) . . ? C13 N13 Ni2 128.4(6) . . ? C15 C14 C13 119.9(9) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 121.0(9) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C11 C16 C17 120.6(9) . . ? C11 C16 C15 119.2(9) . . ? C17 C16 C15 120.2(9) . . ? C18 C17 C16 119.6(10) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C19 C18 C17 118.4(12) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C20 C19 C18 122.5(12) . . ? C20 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? C19 C20 C11 121.0(10) . . ? C19 C20 H20 119.5 . . ? C11 C20 H20 119.5 . . ? C30 C21 C22 123.6(9) . . ? C30 C21 C26 117.2(10) . . ? C22 C21 C26 119.2(11) . . ? C23 C22 C21 120.4(9) . . ? C23 C22 C12 120.2(10) . . ? C21 C22 C12 119.0(11) . . ? C22 C23 C24 120.6(11) . . ? C22 C23 N23 123.2(8) . . ? C24 C23 N23 116.1(11) . . ? C61 N23 C23 119.2(9) . . ? C61 N23 Ni1 111.4(8) . . ? C23 N23 Ni1 129.1(6) . . ? C25 C24 C23 119.6(12) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 122.0(9) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C27 123.6(10) . . ? C25 C26 C21 118.1(10) . . ? C27 C26 C21 118.3(12) . . ? C28 C27 C26 122.9(11) . . ? C28 C27 H27 118.5 . . ? C26 C27 H27 118.5 . . ? C27 C28 C29 120.9(12) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 117.5(14) . . ? C30 C29 H29 121.2 . . ? C28 C29 H29 121.2 . . ? C29 C30 C21 123.1(11) . . ? C29 C30 H30 118.4 . . ? C21 C30 H30 118.4 . . ? C32 N31 C40 118.5(8) . . ? C32 N31 Ni2 109.9(6) . . ? C40 N31 Ni2 131.5(7) . . ? N31 C32 C33 124.9(9) . . ? N31 C32 C41 117.3(8) . . ? C33 C32 C41 117.7(9) . . ? C34 C33 C32 116.2(9) . . ? C34 C33 H33 121.9 . . ? C32 C33 H33 121.9 . . ? C33 C34 C35 122.3(9) . . ? C33 C34 H34 118.9 . . ? C35 C34 H34 118.9 . . ? C34 C35 C36 123.2(9) . . ? C34 C35 C40 118.9(9) . . ? C36 C35 C40 117.9(9) . . ? C37 C36 C35 122.8(9) . . ? C37 C36 H36 118.6 . . ? C35 C36 H36 118.6 . . ? C36 C37 C38 117.8(9) . . ? C36 C37 H37 121.1 . . ? C38 C37 H37 121.1 . . ? C39 C38 C37 124.5(11) . . ? C39 C38 H38 117.8 . . ? C37 C38 H38 117.8 . . ? C38 C39 C40 116.5(9) . . ? C38 C39 C42 115.8(9) . . ? C40 C39 C42 127.6(8) . . ? N31 C40 C39 120.5(8) . . ? N31 C40 C35 119.1(9) . . ? C39 C40 C35 120.3(9) . . ? N13 C41 C32 118.8(9) . . ? N13 C41 H41 120.6 . . ? C32 C41 H41 120.6 . . ? C39 C42 C44 111.0(8) . . ? C39 C42 C43 113.0(8) . . ? C44 C42 C43 111.4(9) . . ? C39 C42 H42 107.1 . . ? C44 C42 H42 107.1 . . ? C43 C42 H42 107.1 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C52 N51 C60 120.0(9) . . ? C52 N51 Ni1 109.9(8) . . ? C60 N51 Ni1 129.8(6) . . ? N51 C52 C53 123.8(12) . . ? N51 C52 C61 117.7(9) . . ? C53 C52 C61 118.5(11) . . ? C54 C53 C52 117.6(12) . . ? C54 C53 H53 121.2 . . ? C52 C53 H53 121.2 . . ? C53 C54 C55 121.8(10) . . ? C53 C54 H54 119.1 . . ? C55 C54 H54 119.1 . . ? C54 C55 C56 123.4(11) . . ? C54 C55 C60 117.9(12) . . ? C56 C55 C60 118.7(12) . . ? C57 C56 C55 122.1(11) . . ? C57 C56 H56 118.9 . . ? C55 C56 H56 118.9 . . ? C56 C57 C58 117.1(13) . . ? C56 C57 H57 121.5 . . ? C58 C57 H57 121.5 . . ? C59 C58 C57 124.0(13) . . ? C59 C58 H58 118.0 . . ? C57 C58 H58 118.0 . . ? C58 C59 C60 119.4(10) . . ? C58 C59 C62 114.2(10) . . ? C60 C59 C62 126.2(10) . . ? N51 C60 C59 122.5(8) . . ? N51 C60 C55 118.8(10) . . ? C59 C60 C55 118.6(11) . . ? N23 C61 C52 118.1(10) . . ? N23 C61 H61 120.9 . . ? C52 C61 H61 120.9 . . ? C59 C62 C63 110.7(9) . . ? C59 C62 C64 112.1(10) . . ? C63 C62 C64 110.7(12) . . ? C59 C62 H62 107.8 . . ? C63 C62 H62 107.8 . . ? C64 C62 H62 107.8 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? 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 N13 Ni2 I3 Ni1 -79.2(2) . . . . ? I2 Ni2 I3 Ni1 -177.89(4) . . . . ? I4 Ni2 I3 Ni1 16.08(4) . . . . ? N23 Ni1 I3 Ni2 85.9(2) . . . . ? N51 Ni1 I3 Ni2 167.7(3) . . . . ? I4 Ni1 I3 Ni2 -16.83(4) . . . . ? I1 Ni1 I3 Ni2 -107.17(19) . . . . ? N23 Ni1 I4 Ni2 -83.8(2) . . . . ? I1 Ni1 I4 Ni2 -179.33(4) . . . . ? I3 Ni1 I4 Ni2 16.15(4) . . . . ? N13 Ni2 I4 Ni1 78.9(2) . . . . ? N31 Ni2 I4 Ni1 161.9(2) . . . . ? I3 Ni2 I4 Ni1 -16.99(4) . . . . ? I2 Ni2 I4 Ni1 -122.5(2) . . . . ? C16 C11 C12 C13 3.7(16) . . . . ? C20 C11 C12 C13 -177.2(11) . . . . ? C16 C11 C12 C22 -178.7(11) . . . . ? C20 C11 C12 C22 0.3(17) . . . . ? C11 C12 C13 N13 175.4(9) . . . . ? C22 C12 C13 N13 -2.1(16) . . . . ? C11 C12 C13 C14 -3.8(15) . . . . ? C22 C12 C13 C14 178.7(10) . . . . ? C12 C13 N13 C41 -64.6(13) . . . . ? C14 C13 N13 C41 114.6(10) . . . . ? C12 C13 N13 Ni2 118.8(9) . . . . ? C14 C13 N13 Ni2 -62.0(11) . . . . ? N31 Ni2 N13 C41 -3.6(6) . . . . ? I3 Ni2 N13 C41 166.5(6) . . . . ? I2 Ni2 N13 C41 -95.7(6) . . . . ? I4 Ni2 N13 C41 79.1(6) . . . . ? N31 Ni2 N13 C13 173.4(7) . . . . ? I3 Ni2 N13 C13 -16.6(7) . . . . ? I2 Ni2 N13 C13 81.3(7) . . . . ? I4 Ni2 N13 C13 -104.0(7) . . . . ? C12 C13 C14 C15 -0.2(15) . . . . ? N13 C13 C14 C15 -179.4(9) . . . . ? C13 C14 C15 C16 4.3(16) . . . . ? C12 C11 C16 C17 178.3(11) . . . . ? C20 C11 C16 C17 -0.8(17) . . . . ? C12 C11 C16 C15 0.2(17) . . . . ? C20 C11 C16 C15 -178.9(10) . . . . ? C14 C15 C16 C11 -4.3(17) . . . . ? C14 C15 C16 C17 177.6(11) . . . . ? C11 C16 C17 C18 3.3(18) . . . . ? C15 C16 C17 C18 -178.6(12) . . . . ? C16 C17 C18 C19 -4(2) . . . . ? C17 C18 C19 C20 2(2) . . . . ? C18 C19 C20 C11 1(2) . . . . ? C16 C11 C20 C19 -1(2) . . . . ? C12 C11 C20 C19 179.6(13) . . . . ? C30 C21 C22 C23 -176.1(10) . . . . ? C26 C21 C22 C23 2.1(15) . . . . ? C30 C21 C22 C12 -2.6(15) . . . . ? C26 C21 C22 C12 175.6(9) . . . . ? C13 C12 C22 C23 -91.1(12) . . . . ? C11 C12 C22 C23 91.4(12) . . . . ? C13 C12 C22 C21 95.4(12) . . . . ? C11 C12 C22 C21 -82.1(13) . . . . ? C21 C22 C23 C24 -1.7(15) . . . . ? C12 C22 C23 C24 -175.1(8) . . . . ? C21 C22 C23 N23 177.1(8) . . . . ? C12 C22 C23 N23 3.6(14) . . . . ? C22 C23 N23 C61 -81.3(12) . . . . ? C24 C23 N23 C61 97.5(10) . . . . ? C22 C23 N23 Ni1 105.9(9) . . . . ? C24 C23 N23 Ni1 -75.3(10) . . . . ? N51 Ni1 N23 C61 -0.1(6) . . . . ? I4 Ni1 N23 C61 173.6(6) . . . . ? I1 Ni1 N23 C61 -91.8(6) . . . . ? I3 Ni1 N23 C61 84.8(6) . . . . ? N51 Ni1 N23 C23 173.1(8) . . . . ? I4 Ni1 N23 C23 -13.2(8) . . . . ? I1 Ni1 N23 C23 81.4(8) . . . . ? I3 Ni1 N23 C23 -102.0(7) . . . . ? C22 C23 C24 C25 1.4(15) . . . . ? N23 C23 C24 C25 -177.4(9) . . . . ? C23 C24 C25 C26 -1.5(16) . . . . ? C24 C25 C26 C27 179.3(10) . . . . ? C24 C25 C26 C21 1.9(16) . . . . ? C30 C21 C26 C25 176.2(10) . . . . ? C22 C21 C26 C25 -2.1(15) . . . . ? C30 C21 C26 C27 -1.4(15) . . . . ? C22 C21 C26 C27 -179.7(10) . . . . ? C25 C26 C27 C28 -176.4(11) . . . . ? C21 C26 C27 C28 1.0(17) . . . . ? C26 C27 C28 C29 -1.4(19) . . . . ? C27 C28 C29 C30 2.2(17) . . . . ? C28 C29 C30 C21 -2.7(16) . . . . ? C22 C21 C30 C29 -179.4(10) . . . . ? C26 C21 C30 C29 2.4(16) . . . . ? N13 Ni2 N31 C32 3.9(6) . . . . ? I2 Ni2 N31 C32 101.4(6) . . . . ? I4 Ni2 N31 C32 -92.6(6) . . . . ? N13 Ni2 N31 C40 -179.1(8) . . . . ? I2 Ni2 N31 C40 -81.6(7) . . . . ? I4 Ni2 N31 C40 84.4(7) . . . . ? C40 N31 C32 C33 0.6(13) . . . . ? Ni2 N31 C32 C33 178.0(7) . . . . ? C40 N31 C32 C41 179.1(8) . . . . ? Ni2 N31 C32 C41 -3.5(10) . . . . ? N31 C32 C33 C34 -1.6(14) . . . . ? C41 C32 C33 C34 179.9(8) . . . . ? C32 C33 C34 C35 3.2(14) . . . . ? C33 C34 C35 C36 177.1(9) . . . . ? C33 C34 C35 C40 -3.8(14) . . . . ? C34 C35 C36 C37 175.7(9) . . . . ? C40 C35 C36 C37 -3.5(14) . . . . ? C35 C36 C37 C38 0.7(14) . . . . ? C36 C37 C38 C39 3.5(14) . . . . ? C37 C38 C39 C40 -4.5(13) . . . . ? C37 C38 C39 C42 178.7(8) . . . . ? C32 N31 C40 C39 178.4(8) . . . . ? Ni2 N31 C40 C39 1.7(12) . . . . ? C32 N31 C40 C35 -1.0(12) . . . . ? Ni2 N31 C40 C35 -177.8(6) . . . . ? C38 C39 C40 N31 -178.0(8) . . . . ? C42 C39 C40 N31 -1.6(13) . . . . ? C38 C39 C40 C35 1.5(12) . . . . ? C42 C39 C40 C35 177.9(8) . . . . ? C34 C35 C40 N31 2.6(13) . . . . ? C36 C35 C40 N31 -178.3(8) . . . . ? C34 C35 C40 C39 -176.9(8) . . . . ? C36 C35 C40 C39 2.3(13) . . . . ? C13 N13 C41 C32 -174.4(8) . . . . ? Ni2 N13 C41 C32 2.8(10) . . . . ? N31 C32 C41 N13 0.6(13) . . . . ? C33 C32 C41 N13 179.2(8) . . . . ? C38 C39 C42 C44 -65.2(11) . . . . ? C40 C39 C42 C44 118.4(10) . . . . ? C38 C39 C42 C43 60.7(10) . . . . ? C40 C39 C42 C43 -115.7(10) . . . . ? N23 Ni1 N51 C52 2.1(6) . . . . ? I1 Ni1 N51 C52 96.5(6) . . . . ? I3 Ni1 N51 C52 -98.9(6) . . . . ? N23 Ni1 N51 C60 176.1(8) . . . . ? I1 Ni1 N51 C60 -89.5(8) . . . . ? I3 Ni1 N51 C60 75.0(8) . . . . ? C60 N51 C52 C53 2.4(14) . . . . ? Ni1 N51 C52 C53 177.0(8) . . . . ? C60 N51 C52 C61 -178.3(8) . . . . ? Ni1 N51 C52 C61 -3.7(10) . . . . ? N51 C52 C53 C54 -2.6(15) . . . . ? C61 C52 C53 C54 178.1(9) . . . . ? C52 C53 C54 C55 0.9(16) . . . . ? C53 C54 C55 C56 -178.6(10) . . . . ? C53 C54 C55 C60 0.9(15) . . . . ? C54 C55 C56 C57 179.5(10) . . . . ? C60 C55 C56 C57 0.0(15) . . . . ? C55 C56 C57 C58 1.1(16) . . . . ? C56 C57 C58 C59 -2.4(16) . . . . ? C57 C58 C59 C60 2.3(16) . . . . ? C57 C58 C59 C62 177.3(10) . . . . ? C52 N51 C60 C59 177.9(9) . . . . ? Ni1 N51 C60 C59 4.5(13) . . . . ? C52 N51 C60 C55 -0.4(12) . . . . ? Ni1 N51 C60 C55 -173.9(6) . . . . ? C58 C59 C60 N51 -179.4(9) . . . . ? C62 C59 C60 N51 6.3(16) . . . . ? C58 C59 C60 C55 -1.0(14) . . . . ? C62 C59 C60 C55 -175.3(9) . . . . ? C54 C55 C60 N51 -1.2(13) . . . . ? C56 C55 C60 N51 178.3(8) . . . . ? C54 C55 C60 C59 -179.6(9) . . . . ? C56 C55 C60 C59 -0.1(13) . . . . ? C23 N23 C61 C52 -175.8(8) . . . . ? Ni1 N23 C61 C52 -1.8(10) . . . . ? N51 C52 C61 N23 3.9(13) . . . . ? C53 C52 C61 N23 -176.7(8) . . . . ? C58 C59 C62 C63 61.6(14) . . . . ? C60 C59 C62 C63 -123.9(12) . . . . ? C58 C59 C62 C64 -62.5(13) . . . . ? C60 C59 C62 C64 112.1(13) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.233 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.176