Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Meyer, Franc' 'Pritzkow, Hans' 'Roder, Jens C.' _publ_contact_author_name 'Dr Franc Meyer' _publ_contact_author_address ; Anorganisch-Chemisches Institut der Universitaet Heidelberg Im Neunheimer Feld 270 Heidelberg D-69120 GERMANY ; _publ_contact_author_email 'FRANC.MEYER@URZ.UNI-HEIDELBERG.DE' _publ_section_title ; An Unusual Hexanickel Cage Complex with u2- and u3- Chloro Bridges and an Interstitial u6-Chloride ; data_jaa _database_code_CSD 171005 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C87 H111 Cl9 N12 Ni6, 5(C H2 Cl2)' _chemical_formula_sum 'C92 H121 Cl19 N12 Ni6' _chemical_formula_weight 2420.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.699(10) _cell_length_b 34.114(15) _cell_length_c 22.346(17) _cell_angle_alpha 90.00 _cell_angle_beta 107.01(4) _cell_angle_gamma 90.00 _cell_volume 10715(12) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4992 _exptl_absorpt_coefficient_mu 1.556 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4456 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; All crystals investigated were non-merohedrally twinned. A crystal was chosen, for which one component was relatively predominant. ; _diffrn_ambient_temperature 190(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 omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63802 _diffrn_reflns_av_R_equivalents 0.0797 _diffrn_reflns_av_sigmaI/netI 0.0626 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 24.78 _reflns_number_total 18308 _reflns_number_gt 12524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1458P)^2^+77.8664P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18308 _refine_ls_number_parameters 1192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.2547 _refine_ls_wR_factor_gt 0.2140 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Ni 0.09052(7) 0.19192(3) 0.63176(5) 0.0187(2) Uani 1 1 d . . . Ni2 Ni 0.16079(7) 0.30995(3) 0.61090(5) 0.0186(2) Uani 1 1 d . . . Ni3 Ni 0.07397(7) 0.17990(3) 0.48893(5) 0.0188(2) Uani 1 1 d . . . Ni4 Ni 0.10557(7) 0.29975(3) 0.46283(5) 0.0195(2) Uani 1 1 d . . . Ni5 Ni -0.11007(7) 0.20199(3) 0.52771(5) 0.0189(2) Uani 1 1 d . . . Ni6 Ni -0.05099(7) 0.32144(3) 0.52701(5) 0.0181(2) Uani 1 1 d . . . Cl1 Cl -0.00463(13) 0.14584(5) 0.55389(9) 0.0207(4) Uani 1 1 d . . . Cl2 Cl 0.20785(13) 0.17824(5) 0.57994(9) 0.0228(4) Uani 1 1 d . . . Cl3 Cl -0.08922(14) 0.19281(6) 0.42647(9) 0.0235(4) Uani 1 1 d . . . Cl4 Cl -0.06066(13) 0.20951(6) 0.63992(9) 0.0225(4) Uani 1 1 d . . . Cl5 Cl 0.25513(13) 0.29333(6) 0.54512(9) 0.0237(4) Uani 1 1 d . . . Cl6 Cl -0.06175(13) 0.30897(6) 0.41734(9) 0.0237(4) Uani 1 1 d . . . Cl7 Cl 0.01855(13) 0.32414(5) 0.63803(9) 0.0220(4) Uani 1 1 d . . . Cl8 Cl 0.09020(13) 0.35629(5) 0.52519(9) 0.0212(4) Uani 1 1 d . . . Cl9 Cl 0.04492(14) 0.25214(6) 0.54042(9) 0.0279(5) Uani 1 1 d . . . Cl10 Cl -0.5268(2) 0.20426(17) 0.5558(2) 0.1073(18) Uani 1 1 d . . . Cl11 Cl -0.57627(18) 0.25849(8) 0.45336(15) 0.0551(7) Uani 1 1 d . . . Cl12 Cl 0.3311(4) 0.19572(16) 0.24317(18) 0.120(2) Uani 1 1 d . . . Cl13 Cl 0.2133(2) 0.25817(8) 0.17681(15) 0.0550(7) Uani 1 1 d . . . Cl14 Cl 0.2979(4) 0.56763(15) 0.1954(2) 0.1164(17) Uani 1 1 d . . . Cl15 Cl 0.3094(3) 0.49248(13) 0.2547(2) 0.0963(13) Uani 1 1 d . . . Cl16 Cl -0.4262(4) 0.43031(17) 0.4792(3) 0.149(3) Uani 1 1 d . . . Cl17 Cl -0.3915(4) 0.48932(16) 0.5759(3) 0.1226(17) Uani 1 1 d . . . Cl18 Cl -0.5720(4) -0.01095(15) 0.4057(3) 0.1246(19) Uani 1 1 d . . . Cl19 Cl -0.4668(3) 0.00187(11) 0.31693(18) 0.0770(10) Uani 1 1 d . . . N1 N 0.1710(4) 0.23258(18) 0.6844(3) 0.0198(14) Uani 1 1 d . . . N2 N 0.1998(4) 0.26888(18) 0.6758(3) 0.0208(14) Uani 1 1 d . . . N3 N 0.1354(4) 0.16156(17) 0.7174(3) 0.0183(13) Uani 1 1 d . . . N4 N 0.2705(4) 0.33998(17) 0.6775(3) 0.0196(14) Uani 1 1 d . . . N5 N 0.1273(5) 0.21266(19) 0.4349(3) 0.0232(15) Uani 1 1 d . . . N6 N 0.1305(4) 0.25053(18) 0.4233(3) 0.0186(13) Uani 1 1 d . . . N7 N 0.1296(5) 0.13587(19) 0.4427(3) 0.0217(14) Uani 1 1 d . . . N8 N 0.1532(5) 0.32260(19) 0.3890(3) 0.0220(14) Uani 1 1 d . . . N9 N -0.1843(5) 0.25116(19) 0.5182(3) 0.0220(14) Uani 1 1 d . . . N10 N -0.1636(5) 0.28920(18) 0.5223(3) 0.0215(14) Uani 1 1 d . . . N11 N -0.2484(5) 0.17938(18) 0.5100(3) 0.0214(14) Uani 1 1 d . . . N12 N -0.1515(5) 0.36556(19) 0.5268(3) 0.0215(14) Uani 1 1 d . . . C1 C 0.2650(5) 0.2802(2) 0.7297(4) 0.0205(16) Uani 1 1 d . . . C2 C 0.2804(6) 0.2506(2) 0.7736(4) 0.0245(18) Uani 1 1 d . . . H2 H 0.3230 0.2504 0.8148 0.033(14) Uiso 1 1 calc R . . C3 C 0.2187(5) 0.2211(2) 0.7432(4) 0.0200(16) Uani 1 1 d . . . C4 C 0.1935(5) 0.1821(2) 0.7587(4) 0.0234(17) Uani 1 1 d . . . H4 H 0.2205 0.1719 0.7996 0.037(11) Uiso 1 1 calc R . . C5 C 0.3038(6) 0.3188(2) 0.7270(4) 0.0209(17) Uani 1 1 d . . . H5 H 0.3534 0.3285 0.7613 0.037(11) Uiso 1 1 calc R . . C6 C 0.0979(5) 0.1269(2) 0.7392(3) 0.0195(16) Uani 1 1 d . . . C7 C 0.0408(6) 0.1320(2) 0.7800(4) 0.0246(18) Uani 1 1 d . . . C8 C 0.0098(6) 0.0988(3) 0.8033(4) 0.033(2) Uani 1 1 d . . . H8 H -0.0273 0.1015 0.8314 0.038(6) Uiso 1 1 calc R . . C9 C 0.0314(7) 0.0614(3) 0.7866(5) 0.037(2) Uani 1 1 d . . . H9 H 0.0111 0.0389 0.8043 0.038(6) Uiso 1 1 calc R . . C10 C 0.0826(6) 0.0573(2) 0.7443(4) 0.030(2) Uani 1 1 d . . . H10 H 0.0944 0.0317 0.7314 0.038(6) Uiso 1 1 calc R . . C11 C 0.1174(6) 0.0893(2) 0.7201(4) 0.0245(18) Uani 1 1 d . . . C12 C 0.0131(6) 0.1724(3) 0.7993(4) 0.0289(19) Uani 1 1 d . . . H12 H 0.0343 0.1927 0.7738 0.029(7) Uiso 1 1 calc R . . C13 C 0.0646(7) 0.1804(3) 0.8690(4) 0.041(2) Uani 1 1 d . . . H13A H 0.0424 0.1618 0.8950 0.054(4) Uiso 1 1 calc R . . H13B H 0.0507 0.2072 0.8796 0.054(4) Uiso 1 1 calc R . . H13C H 0.1333 0.1774 0.8766 0.054(4) Uiso 1 1 calc R . . C14 C -0.0933(7) 0.1762(3) 0.7861(5) 0.042(2) Uani 1 1 d . . . H14A H -0.1245 0.1711 0.7416 0.054(4) Uiso 1 1 calc R . . H14B H -0.1089 0.2027 0.7966 0.054(4) Uiso 1 1 calc R . . H14C H -0.1156 0.1571 0.8114 0.054(4) Uiso 1 1 calc R . . C15 C 0.1773(6) 0.0828(2) 0.6754(4) 0.031(2) Uani 1 1 d . . . H15 H 0.1938 0.1089 0.6611 0.029(7) Uiso 1 1 calc R . . C16 C 0.2702(7) 0.0612(3) 0.7091(5) 0.041(2) Uani 1 1 d . . . H16A H 0.3051 0.0762 0.7461 0.054(4) Uiso 1 1 calc R . . H16B H 0.3094 0.0585 0.6806 0.054(4) Uiso 1 1 calc R . . H16C H 0.2551 0.0351 0.7221 0.054(4) Uiso 1 1 calc R . . C17 C 0.1229(8) 0.0590(3) 0.6180(5) 0.044(2) Uani 1 1 d . . . H17A H 0.1087 0.0329 0.6312 0.054(4) Uiso 1 1 calc R . . H17B H 0.1620 0.0565 0.5893 0.054(4) Uiso 1 1 calc R . . H17C H 0.0634 0.0725 0.5966 0.054(4) Uiso 1 1 calc R . . C18 C 0.3241(5) 0.3749(2) 0.6719(4) 0.0206(16) Uani 1 1 d . . . C19 C 0.2838(6) 0.4118(2) 0.6707(4) 0.0253(18) Uani 1 1 d . . . C20 C 0.3397(6) 0.4440(2) 0.6669(4) 0.030(2) Uani 1 1 d . . . H20 H 0.3138 0.4696 0.6665 0.038(6) Uiso 1 1 calc R . . C21 C 0.4321(6) 0.4401(3) 0.6638(4) 0.034(2) Uani 1 1 d . . . H21 H 0.4688 0.4627 0.6616 0.038(6) Uiso 1 1 calc R . . C22 C 0.4702(6) 0.4032(3) 0.6640(4) 0.033(2) Uani 1 1 d . . . H22 H 0.5334 0.4005 0.6617 0.038(6) Uiso 1 1 calc R . . C23 C 0.4184(5) 0.3700(2) 0.6676(4) 0.0237(17) Uani 1 1 d . . . C24 C 0.1838(6) 0.4183(2) 0.6758(4) 0.0279(19) Uani 1 1 d . . . H24 H 0.1526 0.3922 0.6751 0.029(7) Uiso 1 1 calc R . . C25 C 0.1864(7) 0.4392(3) 0.7372(5) 0.039(2) Uani 1 1 d . . . H25A H 0.2227 0.4233 0.7728 0.054(4) Uiso 1 1 calc R . . H25B H 0.1213 0.4427 0.7395 0.054(4) Uiso 1 1 calc R . . H25C H 0.2169 0.4648 0.7385 0.054(4) Uiso 1 1 calc R . . C26 C 0.1241(7) 0.4426(3) 0.6211(5) 0.039(2) Uani 1 1 d . . . H26A H 0.1493 0.4694 0.6242 0.054(4) Uiso 1 1 calc R . . H26B H 0.0580 0.4433 0.6222 0.054(4) Uiso 1 1 calc R . . H26C H 0.1267 0.4308 0.5816 0.054(4) Uiso 1 1 calc R . . C27 C 0.4656(6) 0.3298(3) 0.6669(4) 0.031(2) Uani 1 1 d . . . H27 H 0.4156 0.3093 0.6633 0.029(7) Uiso 1 1 calc R . . C28 C 0.5427(7) 0.3226(3) 0.7269(5) 0.047(3) Uani 1 1 d . . . H28A H 0.5680 0.2960 0.7265 0.054(4) Uiso 1 1 calc R . . H28B H 0.5164 0.3252 0.7623 0.054(4) Uiso 1 1 calc R . . H28C H 0.5938 0.3417 0.7311 0.054(4) Uiso 1 1 calc R . . C29 C 0.5032(7) 0.3255(3) 0.6105(5) 0.039(2) Uani 1 1 d . . . H29A H 0.5550 0.3443 0.6141 0.054(4) Uiso 1 1 calc R . . H29B H 0.4518 0.3308 0.5721 0.054(4) Uiso 1 1 calc R . . H29C H 0.5270 0.2988 0.6092 0.054(4) Uiso 1 1 calc R . . C30 C 0.1741(5) 0.2555(2) 0.3779(4) 0.0204(16) Uani 1 1 d . . . C31 C 0.1986(6) 0.2194(2) 0.3582(4) 0.0253(18) Uani 1 1 d . . . H31 H 0.2291 0.2139 0.3271 0.033(14) Uiso 1 1 calc R . . C32 C 0.1667(6) 0.1931(2) 0.3959(4) 0.0220(17) Uani 1 1 d . . . C33 C 0.1690(5) 0.1507(2) 0.4036(4) 0.0216(17) Uani 1 1 d . . . H33 H 0.1988 0.1345 0.3804 0.037(11) Uiso 1 1 calc R . . C34 C 0.1823(6) 0.2952(2) 0.3599(4) 0.0248(18) Uani 1 1 d . . . H34 H 0.2088 0.3012 0.3270 0.037(11) Uiso 1 1 calc R . . C35 C 0.1436(6) 0.0946(2) 0.4552(4) 0.0232(17) Uani 1 1 d . . . C36 C 0.0624(6) 0.0705(2) 0.4390(4) 0.0237(17) Uani 1 1 d . . . C37 C 0.0745(6) 0.0301(2) 0.4486(4) 0.0285(19) Uani 1 1 d . . . H37 H 0.0209 0.0131 0.4380 0.038(6) Uiso 1 1 calc R . . C38 C 0.1665(7) 0.0148(3) 0.4742(4) 0.035(2) Uani 1 1 d . . . H38 H 0.1750 -0.0127 0.4799 0.038(6) Uiso 1 1 calc R . . C39 C 0.2444(7) 0.0393(3) 0.4909(4) 0.034(2) Uani 1 1 d . . . H39 H 0.3057 0.0282 0.5089 0.038(6) Uiso 1 1 calc R . . C40 C 0.2359(6) 0.0800(2) 0.4823(4) 0.0267(18) Uani 1 1 d . . . C41 C -0.0361(6) 0.0875(3) 0.4070(4) 0.0285(19) Uani 1 1 d . . . H41 H -0.0345 0.1157 0.4193 0.029(7) Uiso 1 1 calc R . . C42 C -0.1151(7) 0.0684(3) 0.4271(5) 0.040(2) Uani 1 1 d . . . H42A H -0.1202 0.0407 0.4147 0.054(4) Uiso 1 1 calc R . . H42B H -0.1754 0.0817 0.4070 0.054(4) Uiso 1 1 calc R . . H42C H -0.1010 0.0702 0.4727 0.054(4) Uiso 1 1 calc R . . C43 C -0.0542(7) 0.0863(3) 0.3363(5) 0.047(3) Uani 1 1 d . . . H43A H -0.0022 0.0997 0.3254 0.054(4) Uiso 1 1 calc R . . H43B H -0.1145 0.0995 0.3158 0.054(4) Uiso 1 1 calc R . . H43C H -0.0575 0.0590 0.3223 0.054(4) Uiso 1 1 calc R . . C44 C 0.3238(6) 0.1056(3) 0.5048(4) 0.033(2) Uani 1 1 d . . . H44 H 0.3031 0.1336 0.4993 0.029(7) Uiso 1 1 calc R . . C45 C 0.3762(7) 0.0989(3) 0.5739(5) 0.045(3) Uani 1 1 d . . . H45A H 0.3346 0.1062 0.5993 0.054(4) Uiso 1 1 calc R . . H45B H 0.4338 0.1151 0.5860 0.054(4) Uiso 1 1 calc R . . H45C H 0.3937 0.0712 0.5808 0.054(4) Uiso 1 1 calc R . . C46 C 0.3929(7) 0.0984(4) 0.4654(6) 0.054(3) Uani 1 1 d . . . H46A H 0.4155 0.0712 0.4710 0.054(4) Uiso 1 1 calc R . . H46B H 0.4472 0.1163 0.4792 0.054(4) Uiso 1 1 calc R . . H46C H 0.3597 0.1031 0.4212 0.054(4) Uiso 1 1 calc R . . C47 C 0.1434(6) 0.3611(2) 0.3621(4) 0.0223(17) Uani 1 1 d . . . C48 C 0.2037(6) 0.3910(2) 0.3932(4) 0.0276(18) Uani 1 1 d . . . C49 C 0.1948(6) 0.4281(2) 0.3632(4) 0.031(2) Uani 1 1 d . . . H49 H 0.2344 0.4492 0.3831 0.038(6) Uiso 1 1 calc R . . C50 C 0.1302(7) 0.4337(3) 0.3066(5) 0.038(2) Uani 1 1 d . . . H50 H 0.1264 0.4586 0.2869 0.038(6) Uiso 1 1 calc R . . C51 C 0.0695(7) 0.4040(3) 0.2766(4) 0.036(2) Uani 1 1 d . . . H51 H 0.0240 0.4090 0.2374 0.038(6) Uiso 1 1 calc R . . C52 C 0.0743(6) 0.3670(3) 0.3033(4) 0.0293(19) Uani 1 1 d . . . C53 C 0.2775(6) 0.3838(3) 0.4540(4) 0.0273(18) Uani 1 1 d . . . H53 H 0.2571 0.3603 0.4736 0.029(7) Uiso 1 1 calc R . . C54 C 0.3724(7) 0.3735(4) 0.4416(5) 0.049(3) Uani 1 1 d . . . H54A H 0.3640 0.3500 0.4153 0.054(4) Uiso 1 1 calc R . . H54B H 0.4211 0.3685 0.4814 0.054(4) Uiso 1 1 calc R . . H54C H 0.3926 0.3954 0.4200 0.054(4) Uiso 1 1 calc R . . C55 C 0.2916(8) 0.4174(3) 0.5009(5) 0.047(3) Uani 1 1 d . . . H55A H 0.3187 0.4400 0.4852 0.054(4) Uiso 1 1 calc R . . H55B H 0.3351 0.4090 0.5411 0.054(4) Uiso 1 1 calc R . . H55C H 0.2302 0.4246 0.5066 0.054(4) Uiso 1 1 calc R . . C56 C 0.0065(6) 0.3349(3) 0.2697(4) 0.032(2) Uani 1 1 d . . . H56 H 0.0109 0.3127 0.2995 0.029(7) Uiso 1 1 calc R . . C57 C -0.0953(7) 0.3484(3) 0.2480(5) 0.042(2) Uani 1 1 d . . . H57A H -0.1152 0.3567 0.2843 0.054(4) Uiso 1 1 calc R . . H57B H -0.1359 0.3268 0.2267 0.054(4) Uiso 1 1 calc R . . H57C H -0.1010 0.3705 0.2191 0.054(4) Uiso 1 1 calc R . . C58 C 0.0355(8) 0.3195(3) 0.2129(5) 0.046(3) Uani 1 1 d . . . H58A H 0.0372 0.3414 0.1848 0.054(4) Uiso 1 1 calc R . . H58B H -0.0110 0.3000 0.1905 0.054(4) Uiso 1 1 calc R . . H58C H 0.0986 0.3074 0.2274 0.054(4) Uiso 1 1 calc R . . C59 C -0.2447(5) 0.3095(2) 0.5198(4) 0.0235(17) Uani 1 1 d . . . C60 C -0.3194(6) 0.2832(2) 0.5144(4) 0.0251(18) Uani 1 1 d . . . H60 H -0.3836 0.2889 0.5120 0.033(14) Uiso 1 1 calc R . . C61 C -0.2780(5) 0.2471(2) 0.5134(4) 0.0202(16) Uani 1 1 d . . . C62 C -0.3098(5) 0.2068(2) 0.5077(4) 0.0225(17) Uani 1 1 d . . . H62 H -0.3747 0.2006 0.5022 0.037(11) Uiso 1 1 calc R . . C63 C -0.2341(5) 0.3513(2) 0.5233(4) 0.0218(17) Uani 1 1 d . . . H63 H -0.2861 0.3679 0.5231 0.037(11) Uiso 1 1 calc R . . C64 C -0.2857(5) 0.1408(2) 0.4914(4) 0.0216(17) Uani 1 1 d . . . C65 C -0.3358(6) 0.1341(2) 0.4280(4) 0.0269(18) Uani 1 1 d . . . C66 C -0.3705(6) 0.0966(3) 0.4116(4) 0.033(2) Uani 1 1 d . . . H66 H -0.4047 0.0910 0.3694 0.038(6) Uiso 1 1 calc R . . C67 C -0.3562(6) 0.0671(2) 0.4559(5) 0.033(2) Uani 1 1 d . . . H67 H -0.3806 0.0416 0.4437 0.038(6) Uiso 1 1 calc R . . C68 C -0.3072(6) 0.0743(2) 0.5171(4) 0.031(2) Uani 1 1 d . . . H68 H -0.2985 0.0537 0.5468 0.038(6) Uiso 1 1 calc R . . C69 C -0.2696(6) 0.1115(2) 0.5368(4) 0.0262(18) Uani 1 1 d . . . C70 C -0.3538(7) 0.1660(3) 0.3786(4) 0.035(2) Uani 1 1 d . . . H70 H -0.3118 0.1887 0.3966 0.029(7) Uiso 1 1 calc R . . C71 C -0.3314(8) 0.1532(3) 0.3194(5) 0.047(3) Uani 1 1 d . . . H71A H -0.2642 0.1457 0.3296 0.054(4) Uiso 1 1 calc R . . H71B H -0.3440 0.1750 0.2894 0.054(4) Uiso 1 1 calc R . . H71C H -0.3714 0.1308 0.3010 0.054(4) Uiso 1 1 calc R . . C72 C -0.4576(7) 0.1802(3) 0.3618(5) 0.048(3) Uani 1 1 d . . . H72A H -0.4695 0.1990 0.3273 0.054(4) Uiso 1 1 calc R . . H72B H -0.4690 0.1928 0.3984 0.054(4) Uiso 1 1 calc R . . H72C H -0.5006 0.1577 0.3491 0.054(4) Uiso 1 1 calc R . . C73 C -0.2212(6) 0.1195(2) 0.6051(4) 0.0275(18) Uani 1 1 d . . . H73 H -0.1831 0.1441 0.6079 0.029(7) Uiso 1 1 calc R . . C74 C -0.2983(8) 0.1272(3) 0.6381(5) 0.047(3) Uani 1 1 d . . . H74A H -0.3372 0.1497 0.6185 0.054(4) Uiso 1 1 calc R . . H74B H -0.2678 0.1328 0.6825 0.054(4) Uiso 1 1 calc R . . H74C H -0.3389 0.1040 0.6343 0.054(4) Uiso 1 1 calc R . . C75 C -0.1528(8) 0.0867(3) 0.6375(5) 0.047(3) Uani 1 1 d . . . H75A H -0.1894 0.0635 0.6422 0.054(4) Uiso 1 1 calc R . . H75B H -0.1145 0.0956 0.6789 0.054(4) Uiso 1 1 calc R . . H75C H -0.1107 0.0800 0.6122 0.054(4) Uiso 1 1 calc R . . C76 C -0.1392(5) 0.4071(2) 0.5382(4) 0.0216(17) Uani 1 1 d . . . C77 C -0.1443(6) 0.4224(2) 0.5961(4) 0.0292(19) Uani 1 1 d . . . C78 C -0.1356(6) 0.4630(2) 0.6039(5) 0.033(2) Uani 1 1 d . . . H78 H -0.1404 0.4744 0.6416 0.038(6) Uiso 1 1 calc R . . C79 C -0.1202(6) 0.4870(3) 0.5580(5) 0.039(2) Uani 1 1 d . . . H79 H -0.1148 0.5145 0.5646 0.038(6) Uiso 1 1 calc R . . C80 C -0.1125(6) 0.4714(2) 0.5028(5) 0.033(2) Uani 1 1 d . . . H80 H -0.1007 0.4881 0.4719 0.038(6) Uiso 1 1 calc R . . C81 C -0.1219(5) 0.4309(2) 0.4920(4) 0.0253(18) Uani 1 1 d . . . C82 C -0.1595(6) 0.3970(3) 0.6484(4) 0.032(2) Uani 1 1 d . . . H82 H -0.1552 0.3689 0.6367 0.029(7) Uiso 1 1 calc R . . C83 C -0.2581(8) 0.4038(4) 0.6567(6) 0.056(3) Uani 1 1 d . . . H83A H -0.2618 0.4305 0.6719 0.054(4) Uiso 1 1 calc R . . H83B H -0.2687 0.3850 0.6871 0.054(4) Uiso 1 1 calc R . . H83C H -0.3068 0.4003 0.6164 0.054(4) Uiso 1 1 calc R . . C84 C -0.0811(8) 0.4048(3) 0.7104(5) 0.048(3) Uani 1 1 d . . . H84A H -0.0185 0.4004 0.7043 0.054(4) Uiso 1 1 calc R . . H84B H -0.0895 0.3870 0.7428 0.054(4) Uiso 1 1 calc R . . H84C H -0.0855 0.4320 0.7235 0.054(4) Uiso 1 1 calc R . . C85 C -0.1229(6) 0.4130(3) 0.4294(4) 0.0301(19) Uani 1 1 d . . . H85 H -0.1068 0.3846 0.4367 0.029(7) Uiso 1 1 calc R . . C86 C -0.2209(7) 0.4156(4) 0.3841(5) 0.054(3) Uani 1 1 d . . . H86A H -0.2665 0.4030 0.4024 0.054(4) Uiso 1 1 calc R . . H86B H -0.2218 0.4021 0.3452 0.054(4) Uiso 1 1 calc R . . H86C H -0.2382 0.4431 0.3752 0.054(4) Uiso 1 1 calc R . . C87 C -0.0473(7) 0.4318(3) 0.4022(5) 0.040(2) Uani 1 1 d . . . H87A H -0.0624 0.4595 0.3932 0.054(4) Uiso 1 1 calc R . . H87B H -0.0474 0.4182 0.3636 0.054(4) Uiso 1 1 calc R . . H87C H 0.0158 0.4295 0.4328 0.054(4) Uiso 1 1 calc R . . C88 C -0.6144(7) 0.2232(3) 0.4974(7) 0.058(3) Uani 1 1 d . . . H88A H -0.6622 0.2352 0.5151 0.20(3) Uiso 1 1 calc R . . H88B H -0.6462 0.2017 0.4692 0.20(3) Uiso 1 1 calc R . . C89 C 0.2933(10) 0.2209(4) 0.1759(7) 0.070(4) Uani 1 1 d . . . H89A H 0.2629 0.2025 0.1417 0.20(3) Uiso 1 1 calc R . . H89B H 0.3492 0.2325 0.1663 0.20(3) Uiso 1 1 calc R . . C90 C 0.3466(12) 0.5214(5) 0.2041(9) 0.098(5) Uani 1 1 d . . . H90A H 0.3299 0.5084 0.1626 0.20(3) Uiso 1 1 calc R . . H90B H 0.4167 0.5237 0.2193 0.20(3) Uiso 1 1 calc R . . C91 C -0.3737(16) 0.4732(6) 0.5025(12) 0.134(8) Uani 1 1 d . . . H91A H -0.3998 0.4932 0.4698 0.20(3) Uiso 1 1 calc R . . H91B H -0.3047 0.4708 0.5078 0.20(3) Uiso 1 1 calc R . . C92 C -0.5625(11) 0.0170(5) 0.3445(7) 0.085(4) Uani 1 1 d . . . H92A H -0.5530 0.0447 0.3580 0.20(3) Uiso 1 1 calc R . . H92B H -0.6225 0.0153 0.3100 0.20(3) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0197(5) 0.0152(5) 0.0210(5) -0.0011(4) 0.0054(4) -0.0006(4) Ni2 0.0183(5) 0.0145(5) 0.0225(5) 0.0014(4) 0.0054(4) 0.0006(4) Ni3 0.0200(5) 0.0140(5) 0.0230(5) 0.0001(4) 0.0073(4) -0.0001(4) Ni4 0.0215(5) 0.0157(5) 0.0221(5) -0.0003(4) 0.0076(4) 0.0003(4) Ni5 0.0184(5) 0.0136(5) 0.0243(5) 0.0001(4) 0.0055(4) 0.0010(4) Ni6 0.0184(5) 0.0125(5) 0.0237(5) -0.0003(4) 0.0066(4) -0.0009(4) Cl1 0.0242(9) 0.0113(9) 0.0280(10) -0.0008(7) 0.0098(8) -0.0007(7) Cl2 0.0199(9) 0.0219(10) 0.0257(10) -0.0009(8) 0.0054(8) 0.0031(7) Cl3 0.0242(10) 0.0207(10) 0.0254(10) 0.0004(8) 0.0069(8) 0.0001(8) Cl4 0.0223(9) 0.0209(10) 0.0251(10) -0.0018(8) 0.0080(8) 0.0002(7) Cl5 0.0204(9) 0.0228(10) 0.0285(10) -0.0005(8) 0.0080(8) 0.0020(7) Cl6 0.0233(10) 0.0217(10) 0.0252(10) -0.0011(8) 0.0058(8) -0.0004(8) Cl7 0.0210(9) 0.0209(10) 0.0239(10) -0.0010(8) 0.0064(8) 0.0013(7) Cl8 0.0219(9) 0.0137(9) 0.0284(10) 0.0004(7) 0.0080(8) 0.0003(7) Cl9 0.0209(9) 0.0399(12) 0.0235(10) -0.0014(9) 0.0076(8) 0.0046(9) Cl10 0.0464(18) 0.181(5) 0.092(3) 0.079(3) 0.0147(18) 0.009(2) Cl11 0.0367(13) 0.0502(16) 0.078(2) 0.0120(14) 0.0163(13) -0.0049(12) Cl12 0.135(4) 0.181(5) 0.061(2) 0.050(3) 0.055(2) 0.113(4) Cl13 0.0550(16) 0.0398(15) 0.076(2) -0.0036(13) 0.0279(15) 0.0045(12) Cl14 0.158(5) 0.095(3) 0.108(4) 0.031(3) 0.059(3) -0.009(3) Cl15 0.091(3) 0.084(3) 0.117(3) 0.017(2) 0.035(2) 0.019(2) Cl16 0.114(4) 0.101(4) 0.191(6) -0.034(4) -0.019(4) 0.025(3) Cl17 0.114(4) 0.100(4) 0.161(5) 0.008(3) 0.052(4) 0.004(3) Cl18 0.155(5) 0.090(3) 0.167(5) 0.021(3) 0.109(4) 0.001(3) Cl19 0.084(2) 0.072(2) 0.078(2) -0.0084(18) 0.0290(19) -0.0026(18) N1 0.025(3) 0.014(3) 0.022(3) 0.001(3) 0.008(3) -0.001(3) N2 0.019(3) 0.014(3) 0.030(4) 0.004(3) 0.008(3) -0.002(3) N3 0.023(3) 0.010(3) 0.024(3) 0.001(3) 0.009(3) 0.003(3) N4 0.023(3) 0.008(3) 0.029(4) -0.002(3) 0.009(3) -0.001(3) N5 0.032(4) 0.014(3) 0.026(4) 0.000(3) 0.013(3) 0.000(3) N6 0.017(3) 0.016(3) 0.024(3) 0.001(3) 0.009(3) 0.000(3) N7 0.023(3) 0.018(3) 0.025(4) -0.001(3) 0.009(3) -0.004(3) N8 0.025(3) 0.017(3) 0.026(4) 0.005(3) 0.010(3) -0.001(3) N9 0.025(3) 0.018(3) 0.025(4) 0.002(3) 0.010(3) -0.001(3) N10 0.024(3) 0.010(3) 0.031(4) -0.005(3) 0.009(3) -0.002(3) N11 0.023(3) 0.010(3) 0.030(4) -0.005(3) 0.006(3) -0.005(3) N12 0.022(3) 0.017(3) 0.024(4) -0.001(3) 0.005(3) -0.001(3) C1 0.023(4) 0.017(4) 0.019(4) -0.004(3) 0.002(3) -0.002(3) C2 0.022(4) 0.025(4) 0.021(4) -0.002(3) -0.001(3) 0.003(3) C3 0.021(4) 0.015(4) 0.021(4) -0.006(3) 0.002(3) 0.003(3) C4 0.019(4) 0.023(4) 0.030(4) -0.006(3) 0.009(3) 0.003(3) C5 0.023(4) 0.014(4) 0.024(4) 0.002(3) 0.005(3) 0.001(3) C6 0.025(4) 0.015(4) 0.016(4) 0.002(3) 0.003(3) -0.001(3) C7 0.028(4) 0.022(4) 0.022(4) 0.004(3) 0.003(3) 0.002(3) C8 0.032(5) 0.040(6) 0.027(5) 0.006(4) 0.009(4) -0.003(4) C9 0.037(5) 0.023(5) 0.045(6) 0.009(4) 0.005(4) -0.009(4) C10 0.036(5) 0.013(4) 0.035(5) 0.004(4) 0.001(4) -0.005(3) C11 0.031(4) 0.015(4) 0.026(4) -0.002(3) 0.006(4) -0.004(3) C12 0.033(5) 0.034(5) 0.023(4) -0.002(4) 0.013(4) 0.004(4) C13 0.043(6) 0.050(6) 0.031(5) -0.005(4) 0.013(4) 0.005(5) C14 0.042(6) 0.051(6) 0.036(5) 0.009(5) 0.018(5) 0.011(5) C15 0.042(5) 0.016(4) 0.037(5) -0.001(4) 0.017(4) 0.000(4) C16 0.039(5) 0.038(6) 0.047(6) 0.007(5) 0.014(5) 0.005(4) C17 0.059(7) 0.034(5) 0.036(5) -0.008(4) 0.011(5) -0.002(5) C18 0.020(4) 0.016(4) 0.023(4) -0.001(3) 0.002(3) -0.008(3) C19 0.027(4) 0.019(4) 0.027(4) 0.003(3) 0.003(4) -0.002(3) C20 0.036(5) 0.012(4) 0.043(5) -0.004(4) 0.012(4) -0.007(3) C21 0.033(5) 0.024(5) 0.048(6) -0.002(4) 0.014(4) -0.011(4) C22 0.022(4) 0.027(5) 0.050(6) -0.002(4) 0.009(4) -0.004(4) C23 0.020(4) 0.019(4) 0.028(4) -0.005(3) 0.001(3) -0.003(3) C24 0.028(4) 0.013(4) 0.040(5) -0.001(4) 0.006(4) -0.003(3) C25 0.030(5) 0.041(6) 0.047(6) -0.003(5) 0.014(4) 0.000(4) C26 0.036(5) 0.027(5) 0.048(6) -0.002(4) 0.004(4) 0.007(4) C27 0.023(4) 0.027(5) 0.041(5) -0.001(4) 0.007(4) 0.002(4) C28 0.039(6) 0.051(7) 0.049(6) 0.000(5) 0.011(5) 0.014(5) C29 0.037(5) 0.039(6) 0.045(6) -0.007(4) 0.017(5) 0.003(4) C30 0.019(4) 0.021(4) 0.023(4) 0.000(3) 0.010(3) -0.004(3) C31 0.031(4) 0.019(4) 0.028(4) -0.009(3) 0.013(4) -0.001(3) C32 0.030(4) 0.015(4) 0.026(4) -0.005(3) 0.016(4) -0.006(3) C33 0.024(4) 0.016(4) 0.027(4) -0.007(3) 0.011(3) -0.003(3) C34 0.026(4) 0.023(4) 0.028(4) 0.003(3) 0.011(4) -0.006(3) C35 0.035(5) 0.016(4) 0.019(4) -0.007(3) 0.008(3) 0.003(3) C36 0.036(5) 0.017(4) 0.023(4) -0.001(3) 0.015(4) 0.004(3) C37 0.039(5) 0.016(4) 0.033(5) -0.003(4) 0.014(4) -0.001(4) C38 0.052(6) 0.018(4) 0.040(5) 0.002(4) 0.022(5) 0.011(4) C39 0.038(5) 0.026(5) 0.037(5) 0.002(4) 0.010(4) 0.015(4) C40 0.027(4) 0.025(4) 0.028(4) 0.002(4) 0.007(4) 0.006(3) C41 0.024(4) 0.024(4) 0.037(5) -0.001(4) 0.007(4) 0.004(3) C42 0.039(5) 0.029(5) 0.053(6) 0.003(4) 0.016(5) -0.010(4) C43 0.030(5) 0.063(7) 0.043(6) 0.002(5) 0.005(4) -0.004(5) C44 0.024(4) 0.038(5) 0.038(5) -0.003(4) 0.012(4) 0.002(4) C45 0.032(5) 0.052(7) 0.046(6) -0.006(5) 0.004(5) 0.008(5) C46 0.033(5) 0.071(8) 0.063(7) -0.007(6) 0.019(5) 0.003(5) C47 0.028(4) 0.018(4) 0.025(4) 0.002(3) 0.014(4) 0.004(3) C48 0.034(5) 0.018(4) 0.034(5) -0.001(4) 0.015(4) -0.002(3) C49 0.037(5) 0.017(4) 0.042(5) 0.005(4) 0.016(4) -0.003(4) C50 0.053(6) 0.019(5) 0.045(6) 0.016(4) 0.018(5) 0.008(4) C51 0.042(5) 0.027(5) 0.034(5) 0.013(4) 0.006(4) 0.007(4) C52 0.033(5) 0.027(5) 0.033(5) 0.008(4) 0.018(4) 0.003(4) C53 0.030(4) 0.028(5) 0.026(4) 0.000(4) 0.011(4) -0.003(4) C54 0.035(5) 0.073(8) 0.044(6) 0.010(6) 0.019(5) 0.007(5) C55 0.065(7) 0.032(6) 0.045(6) -0.011(5) 0.016(5) -0.008(5) C56 0.029(5) 0.030(5) 0.037(5) 0.006(4) 0.008(4) -0.003(4) C57 0.034(5) 0.043(6) 0.048(6) 0.013(5) 0.007(5) 0.003(4) C58 0.046(6) 0.045(6) 0.046(6) -0.007(5) 0.012(5) -0.002(5) C59 0.018(4) 0.016(4) 0.035(5) 0.001(3) 0.005(3) 0.004(3) C60 0.018(4) 0.021(4) 0.036(5) 0.001(4) 0.008(4) 0.000(3) C61 0.017(4) 0.016(4) 0.027(4) 0.000(3) 0.006(3) -0.002(3) C62 0.015(4) 0.020(4) 0.032(5) 0.002(3) 0.006(3) -0.004(3) C63 0.016(4) 0.016(4) 0.033(5) 0.003(3) 0.006(3) 0.001(3) C64 0.018(4) 0.017(4) 0.030(4) -0.004(3) 0.008(3) 0.000(3) C65 0.029(4) 0.017(4) 0.035(5) -0.002(4) 0.011(4) -0.001(3) C66 0.029(5) 0.029(5) 0.039(5) -0.011(4) 0.007(4) -0.003(4) C67 0.029(5) 0.015(4) 0.054(6) -0.007(4) 0.011(4) -0.011(3) C68 0.035(5) 0.018(4) 0.041(5) 0.002(4) 0.012(4) -0.001(4) C69 0.023(4) 0.022(4) 0.036(5) 0.005(4) 0.011(4) 0.002(3) C70 0.039(5) 0.033(5) 0.031(5) 0.004(4) 0.008(4) -0.010(4) C71 0.059(7) 0.047(6) 0.034(5) -0.003(5) 0.014(5) -0.015(5) C72 0.046(6) 0.033(6) 0.054(7) 0.007(5) -0.004(5) 0.008(5) C73 0.028(4) 0.020(4) 0.033(5) 0.003(4) 0.005(4) -0.006(3) C74 0.054(6) 0.050(6) 0.040(6) -0.010(5) 0.020(5) -0.011(5) C75 0.055(7) 0.033(6) 0.043(6) 0.010(5) -0.002(5) -0.002(5) C76 0.018(4) 0.009(4) 0.032(4) 0.000(3) -0.001(3) 0.006(3) C77 0.024(4) 0.022(4) 0.043(5) -0.011(4) 0.011(4) -0.002(3) C78 0.036(5) 0.019(4) 0.046(6) -0.007(4) 0.017(4) 0.000(4) C79 0.035(5) 0.016(4) 0.064(7) -0.008(4) 0.012(5) -0.007(4) C80 0.033(5) 0.014(4) 0.052(6) 0.005(4) 0.012(4) -0.001(4) C81 0.016(4) 0.016(4) 0.041(5) -0.001(4) 0.004(4) -0.002(3) C82 0.030(5) 0.038(5) 0.030(5) -0.006(4) 0.011(4) -0.001(4) C83 0.044(6) 0.071(8) 0.061(7) -0.002(6) 0.025(6) 0.002(6) C84 0.049(6) 0.052(7) 0.042(6) -0.011(5) 0.014(5) -0.011(5) C85 0.031(5) 0.024(5) 0.033(5) 0.006(4) 0.006(4) -0.001(4) C86 0.041(6) 0.075(8) 0.039(6) -0.001(6) 0.002(5) -0.009(6) C87 0.049(6) 0.027(5) 0.048(6) -0.001(4) 0.023(5) -0.001(4) C88 0.033(5) 0.039(6) 0.107(10) 0.023(6) 0.030(6) 0.012(5) C89 0.092(10) 0.046(7) 0.099(10) 0.029(7) 0.070(9) 0.028(7) C90 0.094(12) 0.077(11) 0.137(16) -0.012(11) 0.055(11) -0.020(9) C91 0.126(17) 0.091(14) 0.18(2) -0.018(15) 0.030(16) -0.018(13) C92 0.077(10) 0.096(12) 0.082(10) 0.000(9) 0.024(8) -0.007(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 Ni1 N1 1.973(6) . ? Ni1 N3 2.104(6) . ? Ni1 Cl4 2.360(3) . ? Ni1 Cl2 2.388(2) . ? Ni1 Cl1 2.456(2) . ? Ni1 Cl9 2.835(3) . ? Ni1 Ni3 3.156(3) . ? Ni1 Ni5 3.195(3) . ? Ni1 Ni2 4.216(2) . ? Ni2 N2 1.977(6) . ? Ni2 N4 2.112(6) . ? Ni2 Cl5 2.366(2) . ? Ni2 Cl7 2.391(2) . ? Ni2 Cl8 2.466(2) . ? Ni2 Cl9 2.775(3) . ? Ni2 Ni6 3.153(3) . ? Ni2 Ni4 3.187(3) . ? Ni3 N5 1.969(7) . ? Ni3 N7 2.118(7) . ? Ni3 Cl2 2.381(3) . ? Ni3 Cl1 2.403(2) . ? Ni3 Cl3 2.437(3) . ? Ni3 Cl9 2.805(3) . ? Ni3 Ni5 3.164(2) . ? Ni3 Ni4 4.175(2) . ? Ni4 N6 1.980(6) . ? Ni4 N8 2.120(7) . ? Ni4 Cl6 2.391(3) . ? Ni4 Cl8 2.428(2) . ? Ni4 Cl5 2.429(3) . ? Ni4 Cl9 2.710(3) . ? Ni4 Ni6 3.136(2) . ? Ni5 N9 1.978(7) . ? Ni5 N11 2.102(7) . ? Ni5 Cl3 2.391(3) . ? Ni5 Cl4 2.411(3) . ? Ni5 Cl1 2.426(2) . ? Ni5 Cl9 2.796(3) . ? Ni5 Ni6 4.167(2) . ? Ni6 N10 1.965(6) . ? Ni6 N12 2.108(7) . ? Ni6 Cl7 2.392(3) . ? Ni6 Cl8 2.402(2) . ? Ni6 Cl6 2.446(3) . ? Ni6 Cl9 2.724(2) . ? Cl10 C88 1.671(12) . ? Cl11 C88 1.748(11) . ? Cl12 C89 1.679(13) . ? Cl13 C89 1.735(11) . ? Cl14 C90 1.720(18) . ? Cl15 C90 1.706(17) . ? Cl16 C91 1.66(2) . ? Cl17 C91 1.82(2) . ? Cl18 C92 1.705(16) . ? Cl19 C92 1.771(16) . ? N1 N2 1.341(9) . ? N1 C3 1.354(10) . ? N2 C1 1.357(10) . ? N3 C4 1.269(10) . ? N3 C6 1.449(10) . ? N4 C5 1.291(10) . ? N4 C18 1.454(9) . ? N5 N6 1.321(9) . ? N5 C32 1.355(10) . ? N6 C30 1.360(10) . ? N7 C33 1.285(10) . ? N7 C35 1.439(10) . ? N8 C34 1.282(11) . ? N8 C47 1.434(10) . ? N9 N10 1.330(9) . ? N9 C61 1.357(10) . ? N10 C59 1.365(10) . ? N11 C62 1.289(10) . ? N11 C64 1.439(10) . ? N12 C63 1.290(10) . ? N12 C76 1.441(10) . ? C1 C2 1.381(11) . ? C1 C5 1.441(11) . ? C2 C3 1.392(11) . ? C3 C4 1.450(11) . ? C6 C11 1.406(11) . ? C6 C7 1.419(11) . ? C7 C8 1.378(12) . ? C7 C12 1.535(12) . ? C8 C9 1.391(13) . ? C9 C10 1.377(14) . ? C10 C11 1.382(12) . ? C11 C15 1.529(12) . ? C12 C14 1.509(13) . ? C12 C13 1.545(12) . ? C15 C17 1.531(13) . ? C15 C16 1.541(13) . ? C18 C19 1.388(11) . ? C18 C23 1.427(11) . ? C19 C20 1.391(11) . ? C19 C24 1.523(12) . ? C20 C21 1.386(12) . ? C21 C22 1.379(13) . ? C22 C23 1.379(12) . ? C23 C27 1.539(11) . ? C24 C26 1.526(12) . ? C24 C25 1.537(13) . ? C27 C28 1.501(13) . ? C27 C29 1.523(13) . ? C30 C31 1.393(11) . ? C30 C34 1.428(11) . ? C31 C32 1.401(11) . ? C32 C33 1.456(11) . ? C35 C36 1.405(12) . ? C35 C40 1.405(12) . ? C36 C37 1.400(11) . ? C36 C41 1.529(11) . ? C37 C38 1.405(13) . ? C38 C39 1.377(13) . ? C39 C40 1.403(12) . ? C40 C44 1.518(12) . ? C41 C42 1.511(12) . ? C41 C43 1.523(13) . ? C44 C45 1.528(13) . ? C44 C46 1.544(13) . ? C47 C48 1.397(12) . ? C47 C52 1.421(12) . ? C48 C49 1.420(12) . ? C48 C53 1.490(12) . ? C49 C50 1.356(13) . ? C50 C51 1.385(14) . ? C51 C52 1.389(12) . ? C52 C56 1.523(12) . ? C53 C55 1.524(12) . ? C53 C54 1.541(13) . ? C56 C57 1.504(12) . ? C56 C58 1.542(14) . ? C59 C60 1.395(11) . ? C59 C63 1.434(11) . ? C60 C61 1.378(11) . ? C61 C62 1.445(11) . ? C64 C69 1.394(11) . ? C64 C65 1.412(12) . ? C65 C66 1.386(12) . ? C65 C70 1.517(12) . ? C66 C67 1.383(13) . ? C67 C68 1.367(13) . ? C68 C69 1.404(12) . ? C69 C73 1.509(12) . ? C70 C71 1.517(13) . ? C70 C72 1.539(14) . ? C73 C75 1.538(12) . ? C73 C74 1.544(13) . ? C76 C81 1.395(12) . ? C76 C77 1.418(12) . ? C77 C78 1.398(12) . ? C77 C82 1.521(13) . ? C78 C79 1.380(14) . ? C79 C80 1.379(14) . ? C80 C81 1.402(11) . ? C81 C85 1.521(12) . ? C82 C83 1.532(13) . ? C82 C84 1.545(13) . ? C85 C86 1.500(13) . ? C85 C87 1.552(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N3 80.2(3) . . ? N1 Ni1 Cl4 100.89(19) . . ? N3 Ni1 Cl4 96.15(18) . . ? N1 Ni1 Cl2 92.0(2) . . ? N3 Ni1 Cl2 105.39(18) . . ? Cl4 Ni1 Cl2 156.53(8) . . ? N1 Ni1 Cl1 172.02(19) . . ? N3 Ni1 Cl1 106.93(18) . . ? Cl4 Ni1 Cl1 82.16(8) . . ? Cl2 Ni1 Cl1 82.74(8) . . ? N1 Ni1 Cl9 83.93(19) . . ? N3 Ni1 Cl9 163.02(18) . . ? Cl4 Ni1 Cl9 80.89(7) . . ? Cl2 Ni1 Cl9 81.06(8) . . ? Cl1 Ni1 Cl9 89.31(8) . . ? N1 Ni1 Ni3 123.36(19) . . ? N3 Ni1 Ni3 140.01(17) . . ? Cl4 Ni1 Ni3 108.39(7) . . ? Cl2 Ni1 Ni3 48.48(6) . . ? Cl1 Ni1 Ni3 48.76(6) . . ? Cl9 Ni1 Ni3 55.52(6) . . ? N1 Ni1 Ni5 128.54(19) . . ? N3 Ni1 Ni5 133.77(18) . . ? Cl4 Ni1 Ni5 48.65(7) . . ? Cl2 Ni1 Ni5 108.17(8) . . ? Cl1 Ni1 Ni5 48.71(6) . . ? Cl9 Ni1 Ni5 54.87(5) . . ? Ni3 Ni1 Ni5 59.76(5) . . ? N1 Ni1 Ni2 43.21(18) . . ? N3 Ni1 Ni2 123.28(17) . . ? Cl4 Ni1 Ni2 91.85(6) . . ? Cl2 Ni1 Ni2 84.15(6) . . ? Cl1 Ni1 Ni2 129.80(6) . . ? Cl9 Ni1 Ni2 40.74(5) . . ? Ni3 Ni1 Ni2 87.77(3) . . ? Ni5 Ni1 Ni2 91.18(4) . . ? N2 Ni2 N4 80.1(3) . . ? N2 Ni2 Cl5 100.9(2) . . ? N4 Ni2 Cl5 95.10(19) . . ? N2 Ni2 Cl7 92.59(19) . . ? N4 Ni2 Cl7 105.47(19) . . ? Cl5 Ni2 Cl7 157.10(8) . . ? N2 Ni2 Cl8 171.87(19) . . ? N4 Ni2 Cl8 107.31(18) . . ? Cl5 Ni2 Cl8 82.01(8) . . ? Cl7 Ni2 Cl8 82.34(8) . . ? N2 Ni2 Cl9 84.9(2) . . ? N4 Ni2 Cl9 163.73(18) . . ? Cl5 Ni2 Cl9 81.44(8) . . ? Cl7 Ni2 Cl9 81.41(8) . . ? Cl8 Ni2 Cl9 88.05(8) . . ? N2 Ni2 Ni6 123.27(18) . . ? N4 Ni2 Ni6 140.89(17) . . ? Cl5 Ni2 Ni6 108.46(8) . . ? Cl7 Ni2 Ni6 48.78(7) . . ? Cl8 Ni2 Ni6 48.75(5) . . ? Cl9 Ni2 Ni6 54.25(6) . . ? N2 Ni2 Ni4 128.0(2) . . ? N4 Ni2 Ni4 134.02(18) . . ? Cl5 Ni2 Ni4 49.19(7) . . ? Cl7 Ni2 Ni4 108.02(7) . . ? Cl8 Ni2 Ni4 48.86(6) . . ? Cl9 Ni2 Ni4 53.53(5) . . ? Ni6 Ni2 Ni4 59.28(5) . . ? N2 Ni2 Ni1 43.13(19) . . ? N4 Ni2 Ni1 123.12(17) . . ? Cl5 Ni2 Ni1 92.69(6) . . ? Cl7 Ni2 Ni1 84.53(6) . . ? Cl8 Ni2 Ni1 129.57(6) . . ? Cl9 Ni2 Ni1 41.81(5) . . ? Ni6 Ni2 Ni1 87.33(4) . . ? Ni4 Ni2 Ni1 90.82(3) . . ? N5 Ni3 N7 79.8(3) . . ? N5 Ni3 Cl2 99.2(2) . . ? N7 Ni3 Cl2 93.41(19) . . ? N5 Ni3 Cl1 173.3(2) . . ? N7 Ni3 Cl1 105.92(18) . . ? Cl2 Ni3 Cl1 84.02(9) . . ? N5 Ni3 Cl3 92.7(2) . . ? N7 Ni3 Cl3 107.73(19) . . ? Cl2 Ni3 Cl3 157.31(8) . . ? Cl1 Ni3 Cl3 82.34(8) . . ? N5 Ni3 Cl9 83.6(2) . . ? N7 Ni3 Cl9 161.81(18) . . ? Cl2 Ni3 Cl9 81.81(7) . . ? Cl1 Ni3 Cl9 91.10(8) . . ? Cl3 Ni3 Cl9 80.42(7) . . ? N5 Ni3 Ni1 128.3(2) . . ? N7 Ni3 Ni1 131.23(18) . . ? Cl2 Ni3 Ni1 48.66(7) . . ? Cl1 Ni3 Ni1 50.23(6) . . ? Cl3 Ni3 Ni1 109.12(7) . . ? Cl9 Ni3 Ni1 56.42(5) . . ? N5 Ni3 Ni5 124.0(2) . . ? N7 Ni3 Ni5 141.77(18) . . ? Cl2 Ni3 Ni5 109.33(8) . . ? Cl1 Ni3 Ni5 49.37(6) . . ? Cl3 Ni3 Ni5 48.43(7) . . ? Cl9 Ni3 Ni5 55.48(5) . . ? Ni1 Ni3 Ni5 60.73(5) . . ? N5 Ni3 Ni4 43.77(19) . . ? N7 Ni3 Ni4 123.48(18) . . ? Cl2 Ni3 Ni4 92.56(6) . . ? Cl1 Ni3 Ni4 130.60(6) . . ? Cl3 Ni3 Ni4 82.76(5) . . ? Cl9 Ni3 Ni4 39.95(5) . . ? Ni1 Ni3 Ni4 92.02(3) . . ? Ni5 Ni3 Ni4 86.79(3) . . ? N6 Ni4 N8 79.6(3) . . ? N6 Ni4 Cl6 102.90(19) . . ? N8 Ni4 Cl6 98.86(19) . . ? N6 Ni4 Cl8 171.71(19) . . ? N8 Ni4 Cl8 105.18(19) . . ? Cl6 Ni4 Cl8 83.27(8) . . ? N6 Ni4 Cl5 90.95(19) . . ? N8 Ni4 Cl5 101.0(2) . . ? Cl6 Ni4 Cl5 157.57(8) . . ? Cl8 Ni4 Cl5 81.53(8) . . ? N6 Ni4 Cl9 85.13(19) . . ? N8 Ni4 Cl9 164.49(19) . . ? Cl6 Ni4 Cl9 82.00(8) . . ? Cl8 Ni4 Cl9 90.32(8) . . ? Cl5 Ni4 Cl9 81.71(8) . . ? N6 Ni4 Ni6 131.29(18) . . ? N8 Ni4 Ni6 136.29(18) . . ? Cl6 Ni4 Ni6 50.37(7) . . ? Cl8 Ni4 Ni6 49.17(5) . . ? Cl5 Ni4 Ni6 107.33(8) . . ? Cl9 Ni4 Ni6 54.96(6) . . ? N6 Ni4 Ni2 122.07(19) . . ? N8 Ni4 Ni2 136.53(19) . . ? Cl6 Ni4 Ni2 110.17(7) . . ? Cl8 Ni4 Ni2 49.89(5) . . ? Cl5 Ni4 Ni2 47.50(6) . . ? Cl9 Ni4 Ni2 55.43(6) . . ? Ni6 Ni4 Ni2 59.83(5) . . ? N6 Ni4 Ni3 43.48(18) . . ? N8 Ni4 Ni3 122.98(18) . . ? Cl6 Ni4 Ni3 92.61(6) . . ? Cl8 Ni4 Ni3 131.66(6) . . ? Cl5 Ni4 Ni3 85.35(6) . . ? Cl9 Ni4 Ni3 41.65(5) . . ? Ni6 Ni4 Ni3 92.33(4) . . ? Ni2 Ni4 Ni3 88.09(3) . . ? N9 Ni5 N11 79.5(3) . . ? N9 Ni5 Cl3 103.3(2) . . ? N11 Ni5 Cl3 99.13(19) . . ? N9 Ni5 Cl4 90.6(2) . . ? N11 Ni5 Cl4 102.4(2) . . ? Cl3 Ni5 Cl4 156.19(8) . . ? N9 Ni5 Cl1 171.5(2) . . ? N11 Ni5 Cl1 105.68(18) . . ? Cl3 Ni5 Cl1 82.82(8) . . ? Cl4 Ni5 Cl1 81.75(7) . . ? N9 Ni5 Cl9 84.3(2) . . ? N11 Ni5 Cl9 163.44(18) . . ? Cl3 Ni5 Cl9 81.37(7) . . ? Cl4 Ni5 Cl9 80.84(7) . . ? Cl1 Ni5 Cl9 90.83(8) . . ? N9 Ni5 Ni3 131.45(19) . . ? N11 Ni5 Ni3 135.95(18) . . ? Cl3 Ni5 Ni3 49.68(6) . . ? Cl4 Ni5 Ni3 106.78(7) . . ? Cl1 Ni5 Ni3 48.75(5) . . ? Cl9 Ni5 Ni3 55.74(6) . . ? N9 Ni5 Ni1 122.14(19) . . ? N11 Ni5 Ni1 137.20(19) . . ? Cl3 Ni5 Ni1 109.15(8) . . ? Cl4 Ni5 Ni1 47.28(6) . . ? Cl1 Ni5 Ni1 49.53(5) . . ? Cl9 Ni5 Ni1 56.00(6) . . ? Ni3 Ni5 Ni1 59.51(6) . . ? N9 Ni5 Ni6 43.93(19) . . ? N11 Ni5 Ni6 123.34(17) . . ? Cl3 Ni5 Ni6 92.29(6) . . ? Cl4 Ni5 Ni6 84.27(5) . . ? Cl1 Ni5 Ni6 130.84(6) . . ? Cl9 Ni5 Ni6 40.33(5) . . ? Ni3 Ni5 Ni6 92.07(4) . . ? Ni1 Ni5 Ni6 87.65(3) . . ? N10 Ni6 N12 79.7(3) . . ? N10 Ni6 Cl7 100.1(2) . . ? N12 Ni6 Cl7 93.54(19) . . ? N10 Ni6 Cl8 174.1(2) . . ? N12 Ni6 Cl8 104.77(19) . . ? Cl7 Ni6 Cl8 83.65(8) . . ? N10 Ni6 Cl6 92.4(2) . . ? N12 Ni6 Cl6 106.37(19) . . ? Cl7 Ni6 Cl6 158.15(8) . . ? Cl8 Ni6 Cl6 82.65(8) . . ? N10 Ni6 Cl9 85.46(19) . . ? N12 Ni6 Cl9 163.71(19) . . ? Cl7 Ni6 Cl9 82.47(7) . . ? Cl8 Ni6 Cl9 90.54(8) . . ? Cl6 Ni6 Cl9 80.73(7) . . ? N10 Ni6 Ni4 124.26(19) . . ? N12 Ni6 Ni4 140.80(18) . . ? Cl7 Ni6 Ni4 109.59(8) . . ? Cl8 Ni6 Ni4 49.89(6) . . ? Cl6 Ni6 Ni4 48.83(6) . . ? Cl9 Ni6 Ni4 54.55(5) . . ? N10 Ni6 Ni2 129.2(2) . . ? N12 Ni6 Ni2 131.27(18) . . ? Cl7 Ni6 Ni2 48.73(6) . . ? Cl8 Ni6 Ni2 50.51(6) . . ? Cl6 Ni6 Ni2 109.70(7) . . ? Cl9 Ni6 Ni2 55.77(5) . . ? Ni4 Ni6 Ni2 60.89(6) . . ? N10 Ni6 Ni5 43.90(18) . . ? N12 Ni6 Ni5 123.48(18) . . ? Cl7 Ni6 Ni5 93.44(5) . . ? Cl8 Ni6 Ni5 131.75(6) . . ? Cl6 Ni6 Ni5 83.18(5) . . ? Cl9 Ni6 Ni5 41.64(6) . . ? Ni4 Ni6 Ni5 87.28(4) . . ? Ni2 Ni6 Ni5 92.68(3) . . ? Ni3 Cl1 Ni5 81.87(7) . . ? Ni3 Cl1 Ni1 81.01(8) . . ? Ni5 Cl1 Ni1 81.76(8) . . ? Ni3 Cl2 Ni1 82.87(9) . . ? Ni5 Cl3 Ni3 81.89(8) . . ? Ni1 Cl4 Ni5 84.06(8) . . ? Ni2 Cl5 Ni4 83.31(9) . . ? Ni4 Cl6 Ni6 80.80(8) . . ? Ni2 Cl7 Ni6 82.49(8) . . ? Ni6 Cl8 Ni4 80.95(7) . . ? Ni6 Cl8 Ni2 80.73(8) . . ? Ni4 Cl8 Ni2 81.26(8) . . ? Ni4 Cl9 Ni6 70.49(7) . . ? Ni4 Cl9 Ni2 71.04(7) . . ? Ni6 Cl9 Ni2 69.98(7) . . ? Ni4 Cl9 Ni5 135.44(9) . . ? Ni6 Cl9 Ni5 98.03(8) . . ? Ni2 Cl9 Ni5 147.03(8) . . ? Ni4 Cl9 Ni3 98.40(8) . . ? Ni6 Cl9 Ni3 148.59(9) . . ? Ni2 Cl9 Ni3 135.68(8) . . ? Ni5 Cl9 Ni3 68.78(7) . . ? Ni4 Cl9 Ni1 147.39(8) . . ? Ni6 Cl9 Ni1 135.56(8) . . ? Ni2 Cl9 Ni1 97.46(8) . . ? Ni5 Cl9 Ni1 69.13(7) . . ? Ni3 Cl9 Ni1 68.06(7) . . ? N2 N1 C3 108.1(6) . . ? N2 N1 Ni1 136.3(5) . . ? C3 N1 Ni1 115.2(5) . . ? N1 N2 C1 107.9(6) . . ? N1 N2 Ni2 136.4(5) . . ? C1 N2 Ni2 115.2(5) . . ? C4 N3 C6 116.5(7) . . ? C4 N3 Ni1 110.8(5) . . ? C6 N3 Ni1 131.2(5) . . ? C5 N4 C18 116.9(6) . . ? C5 N4 Ni2 110.6(5) . . ? C18 N4 Ni2 131.1(5) . . ? N6 N5 C32 108.0(6) . . ? N6 N5 Ni3 135.9(5) . . ? C32 N5 Ni3 115.9(5) . . ? N5 N6 C30 108.6(6) . . ? N5 N6 Ni4 136.1(5) . . ? C30 N6 Ni4 114.5(5) . . ? C33 N7 C35 116.8(7) . . ? C33 N7 Ni3 111.5(5) . . ? C35 N7 Ni3 130.8(5) . . ? C34 N8 C47 117.5(7) . . ? C34 N8 Ni4 111.3(5) . . ? C47 N8 Ni4 130.3(5) . . ? N10 N9 C61 108.2(6) . . ? N10 N9 Ni5 135.4(5) . . ? C61 N9 Ni5 115.9(5) . . ? N9 N10 C59 108.2(6) . . ? N9 N10 Ni6 136.3(5) . . ? C59 N10 Ni6 115.5(5) . . ? C62 N11 C64 116.6(6) . . ? C62 N11 Ni5 111.6(5) . . ? C64 N11 Ni5 131.0(5) . . ? C63 N12 C76 116.7(7) . . ? C63 N12 Ni6 112.2(5) . . ? C76 N12 Ni6 130.5(5) . . ? N2 C1 C2 110.4(7) . . ? N2 C1 C5 114.1(7) . . ? C2 C1 C5 135.4(7) . . ? C1 C2 C3 103.6(7) . . ? N1 C3 C2 110.0(7) . . ? N1 C3 C4 113.6(7) . . ? C2 C3 C4 136.4(7) . . ? N3 C4 C3 119.8(8) . . ? N4 C5 C1 119.4(7) . . ? C11 C6 C7 121.2(7) . . ? C11 C6 N3 120.7(7) . . ? C7 C6 N3 118.2(7) . . ? C8 C7 C6 117.7(8) . . ? C8 C7 C12 119.3(8) . . ? C6 C7 C12 123.0(7) . . ? C7 C8 C9 121.7(9) . . ? C10 C9 C8 119.4(8) . . ? C9 C10 C11 121.8(8) . . ? C10 C11 C6 118.1(8) . . ? C10 C11 C15 119.3(7) . . ? C6 C11 C15 122.6(7) . . ? C14 C12 C7 111.5(8) . . ? C14 C12 C13 110.9(7) . . ? C7 C12 C13 110.4(7) . . ? C11 C15 C17 111.5(8) . . ? C11 C15 C16 110.4(7) . . ? C17 C15 C16 109.1(8) . . ? C19 C18 C23 121.5(7) . . ? C19 C18 N4 120.3(7) . . ? C23 C18 N4 118.2(7) . . ? C18 C19 C20 117.5(8) . . ? C18 C19 C24 123.1(7) . . ? C20 C19 C24 119.4(7) . . ? C21 C20 C19 122.1(8) . . ? C22 C21 C20 119.4(8) . . ? C21 C22 C23 121.3(8) . . ? C22 C23 C18 118.1(7) . . ? C22 C23 C27 118.2(7) . . ? C18 C23 C27 123.6(7) . . ? C19 C24 C26 111.1(7) . . ? C19 C24 C25 111.2(7) . . ? C26 C24 C25 108.7(7) . . ? C28 C27 C29 111.2(8) . . ? C28 C27 C23 111.2(8) . . ? C29 C27 C23 111.5(8) . . ? N6 C30 C31 110.4(7) . . ? N6 C30 C34 115.3(7) . . ? C31 C30 C34 134.3(7) . . ? C30 C31 C32 102.3(7) . . ? N5 C32 C31 110.7(7) . . ? N5 C32 C33 114.3(7) . . ? C31 C32 C33 135.0(7) . . ? N7 C33 C32 118.3(7) . . ? N8 C34 C30 118.6(7) . . ? C36 C35 C40 123.0(7) . . ? C36 C35 N7 117.3(7) . . ? C40 C35 N7 119.7(7) . . ? C37 C36 C35 118.4(8) . . ? C37 C36 C41 120.3(8) . . ? C35 C36 C41 121.1(7) . . ? C36 C37 C38 119.5(8) . . ? C39 C38 C37 120.7(8) . . ? C38 C39 C40 121.9(8) . . ? C39 C40 C35 116.5(8) . . ? C39 C40 C44 119.4(8) . . ? C35 C40 C44 124.1(8) . . ? C42 C41 C43 112.4(8) . . ? C42 C41 C36 113.7(7) . . ? C43 C41 C36 109.2(7) . . ? C40 C44 C45 112.2(8) . . ? C40 C44 C46 111.0(8) . . ? C45 C44 C46 109.4(8) . . ? C48 C47 C52 122.3(7) . . ? C48 C47 N8 119.3(7) . . ? C52 C47 N8 118.4(7) . . ? C47 C48 C49 117.3(8) . . ? C47 C48 C53 121.4(7) . . ? C49 C48 C53 121.3(8) . . ? C50 C49 C48 120.6(8) . . ? C49 C50 C51 121.6(8) . . ? C50 C51 C52 120.9(9) . . ? C51 C52 C47 117.3(8) . . ? C51 C52 C56 119.9(8) . . ? C47 C52 C56 122.8(7) . . ? C48 C53 C55 114.9(8) . . ? C48 C53 C54 109.2(7) . . ? C55 C53 C54 110.3(8) . . ? C57 C56 C52 112.6(8) . . ? C57 C56 C58 109.2(8) . . ? C52 C56 C58 110.6(7) . . ? N10 C59 C60 109.5(7) . . ? N10 C59 C63 115.0(7) . . ? C60 C59 C63 135.6(7) . . ? C61 C60 C59 103.7(7) . . ? N9 C61 C60 110.4(7) . . ? N9 C61 C62 113.5(7) . . ? C60 C61 C62 136.1(7) . . ? N11 C62 C61 118.8(7) . . ? N12 C63 C59 117.6(7) . . ? C69 C64 C65 122.8(7) . . ? C69 C64 N11 118.4(7) . . ? C65 C64 N11 118.8(7) . . ? C66 C65 C64 117.3(8) . . ? C66 C65 C70 119.9(8) . . ? C64 C65 C70 122.9(7) . . ? C67 C66 C65 121.0(8) . . ? C68 C67 C66 120.7(8) . . ? C67 C68 C69 121.2(8) . . ? C64 C69 C68 117.0(8) . . ? C64 C69 C73 122.4(7) . . ? C68 C69 C73 120.4(7) . . ? C65 C70 C71 113.1(8) . . ? C65 C70 C72 110.6(8) . . ? C71 C70 C72 109.3(8) . . ? C69 C73 C75 113.2(7) . . ? C69 C73 C74 108.7(7) . . ? C75 C73 C74 111.7(8) . . ? C81 C76 C77 122.0(7) . . ? C81 C76 N12 118.8(7) . . ? C77 C76 N12 119.2(7) . . ? C78 C77 C76 116.8(8) . . ? C78 C77 C82 119.9(8) . . ? C76 C77 C82 123.3(7) . . ? C79 C78 C77 121.7(9) . . ? C80 C79 C78 120.6(8) . . ? C79 C80 C81 120.4(9) . . ? C76 C81 C80 118.5(8) . . ? C76 C81 C85 119.5(7) . . ? C80 C81 C85 121.8(8) . . ? C77 C82 C83 111.3(8) . . ? C77 C82 C84 110.7(8) . . ? C83 C82 C84 110.4(8) . . ? C86 C85 C81 110.3(8) . . ? C86 C85 C87 111.6(8) . . ? C81 C85 C87 112.3(7) . . ? Cl10 C88 Cl11 113.9(6) . . ? Cl12 C89 Cl13 114.3(7) . . ? Cl15 C90 Cl14 113.7(10) . . ? Cl16 C91 Cl17 111.8(14) . . ? Cl18 C92 Cl19 112.1(9) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.78 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 3.111 _refine_diff_density_min -1.608 _refine_diff_density_rms 0.189 #========================================================== data_fm46 _database_code_CSD 171006 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H98 Cl6 N8 Ni4 O4, 4 (C H Cl3)' _chemical_formula_sum 'C70 H102 Cl18 N8 Ni4 O4' _chemical_formula_weight 1992.54 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5542(2) _cell_length_b 13.6937(2) _cell_length_c 16.0974(3) _cell_angle_alpha 97.3680(10) _cell_angle_beta 110.2490(10) _cell_angle_gamma 102.4780(10) _cell_volume 2275.05(7) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 1.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8138 _exptl_absorpt_correction_T_max 1.0000 _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 omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30353 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0259 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.30 _reflns_number_total 11068 _reflns_number_gt 8851 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0477P)^2^+2.6433P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11068 _refine_ls_number_parameters 656 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Ni 0.58284(3) 0.41943(2) 0.325632(19) 0.01898(8) Uani 1 1 d . . . Ni2 Ni 0.43259(3) 0.37323(2) 0.513295(19) 0.01891(8) Uani 1 1 d . . . Cl1 Cl 0.40705(6) 0.27945(5) 0.22574(4) 0.02840(13) Uani 1 1 d . . . Cl2 Cl 0.28214(5) 0.41969(4) 0.56736(4) 0.02252(12) Uani 1 1 d . . . Cl3 Cl 0.58456(5) 0.52233(4) 0.61642(4) 0.02181(11) Uani 1 1 d . . . Cl4 Cl 0.97783(10) -0.15780(9) -0.03665(8) 0.0694(3) Uani 1 1 d . . . Cl5 Cl 0.84440(13) -0.30226(8) 0.03741(9) 0.0776(3) Uani 1 1 d . . . Cl6 Cl 0.84376(10) -0.09166(7) 0.07042(8) 0.0636(3) Uani 1 1 d . . . Cl7 Cl 0.22744(15) -0.01152(10) 0.16337(11) 0.1120(6) Uani 1 1 d . . . Cl8 Cl 0.33378(16) 0.01480(10) 0.35950(11) 0.0968(4) Uani 1 1 d . . . Cl9 Cl 0.48351(13) -0.02248(10) 0.25820(10) 0.0854(4) Uani 1 1 d . . . O1 O 0.5836(2) 0.49912(15) 0.22749(12) 0.0299(4) Uani 1 1 d . . . O2 O 0.29348(17) 0.26007(14) 0.40079(13) 0.0280(4) Uani 1 1 d . . . N1 N 0.61379(18) 0.33777(14) 0.41869(12) 0.0187(4) Uani 1 1 d . . . N2 N 0.56297(18) 0.32150(14) 0.47914(13) 0.0189(4) Uani 1 1 d . . . N3 N 0.73117(18) 0.34863(15) 0.30439(13) 0.0203(4) Uani 1 1 d . . . N4 N 0.48466(18) 0.27271(14) 0.60625(13) 0.0209(4) Uani 1 1 d . . . C1 C 0.6094(2) 0.25056(17) 0.52169(16) 0.0210(4) Uani 1 1 d . . . C2 C 0.6943(2) 0.22056(18) 0.48682(16) 0.0227(5) Uani 1 1 d . . . C3 C 0.6943(2) 0.27792(17) 0.42149(15) 0.0201(4) Uani 1 1 d . . . C4 C 0.7562(2) 0.28721(18) 0.35759(16) 0.0217(4) Uani 1 1 d . . . C5 C 0.7888(2) 0.35127(19) 0.23773(16) 0.0234(5) Uani 1 1 d . . . C6 C 0.7421(2) 0.2692(2) 0.16189(17) 0.0277(5) Uani 1 1 d . . . C7 C 0.7984(3) 0.2771(2) 0.09785(19) 0.0372(6) Uani 1 1 d . . . C8 C 0.8982(3) 0.3600(3) 0.1095(2) 0.0437(7) Uani 1 1 d . . . C9 C 0.9438(3) 0.4392(2) 0.1854(2) 0.0375(6) Uani 1 1 d . . . C10 C 0.8898(2) 0.4374(2) 0.25055(17) 0.0266(5) Uani 1 1 d . . . C11 C 0.6364(3) 0.1723(2) 0.14707(19) 0.0312(6) Uani 1 1 d . . . C12 C 0.5245(3) 0.1508(3) 0.0553(2) 0.0446(7) Uani 1 1 d . . . C13 C 0.6913(4) 0.0804(3) 0.1555(3) 0.0474(8) Uani 1 1 d . . . C14 C 0.9440(2) 0.5237(2) 0.33479(18) 0.0290(5) Uani 1 1 d . . . C15 C 1.0568(3) 0.5035(3) 0.4070(3) 0.0499(8) Uani 1 1 d . . . C16 C 0.9838(4) 0.6292(3) 0.3160(3) 0.0508(8) Uani 1 1 d . . . C17 C 0.5652(2) 0.22812(18) 0.59226(16) 0.0226(5) Uani 1 1 d . . . C18 C 0.4556(2) 0.25983(17) 0.68445(16) 0.0229(5) Uani 1 1 d . . . C19 C 0.5507(2) 0.30298(18) 0.77167(17) 0.0250(5) Uani 1 1 d . . . C20 C 0.5165(3) 0.2877(2) 0.84574(19) 0.0324(6) Uani 1 1 d . . . C21 C 0.3936(3) 0.2328(2) 0.8324(2) 0.0390(7) Uani 1 1 d . . . C22 C 0.3021(3) 0.1916(2) 0.7460(2) 0.0356(6) Uani 1 1 d . . . C23 C 0.3296(2) 0.20371(19) 0.66971(18) 0.0280(5) Uani 1 1 d . . . C24 C 0.6891(2) 0.3614(2) 0.79011(17) 0.0271(5) Uani 1 1 d . . . C25 C 0.7804(3) 0.2967(3) 0.8278(2) 0.0388(6) Uani 1 1 d . . . C26 C 0.7334(3) 0.4665(2) 0.8544(2) 0.0353(6) Uani 1 1 d . . . C27 C 0.2345(3) 0.1508(2) 0.5743(2) 0.0337(6) Uani 1 1 d . . . C28 C 0.2424(4) 0.0408(3) 0.5507(3) 0.0486(8) Uani 1 1 d . . . C29 C 0.0965(3) 0.1514(3) 0.5577(3) 0.0518(9) Uani 1 1 d . . . C30 C 0.5440(3) 0.4550(2) 0.13205(18) 0.0344(6) Uani 1 1 d . . . C31 C 0.6365(3) 0.5068(3) 0.0940(2) 0.0430(7) Uani 1 1 d . . . C32 C 0.1632(3) 0.2655(3) 0.3552(2) 0.0418(7) Uani 1 1 d . . . H32A H 0.1658 0.3244 0.3254 0.079(10) Uiso 1 1 calc R . . H32B H 0.1259 0.2781 0.4010 0.079(10) Uiso 1 1 calc R . . C33 C 0.0802(4) 0.1723(4) 0.2872(3) 0.0765(14) Uani 1 1 d . . . H33A H 0.1166 0.1593 0.2416 0.149(15) Uiso 1 1 calc R . . H33B H -0.0056 0.1809 0.2576 0.149(15) Uiso 1 1 calc R . . H33C H 0.0738 0.1142 0.3167 0.149(15) Uiso 1 1 calc R . . C34 C 0.8453(3) -0.1925(3) -0.0077(2) 0.0413(7) Uani 1 1 d . . . C35 C 0.3639(4) 0.0347(3) 0.2625(3) 0.0676(11) Uani 1 1 d . . . H1O H 0.588(3) 0.553(3) 0.237(2) 0.031(9) Uiso 1 1 d . . . H2O H 0.325(3) 0.262(3) 0.368(2) 0.042(10) Uiso 1 1 d . . . H2 H 0.737(3) 0.176(3) 0.499(2) 0.041(9) Uiso 1 1 d . . . H4 H 0.811(3) 0.248(2) 0.3556(18) 0.021(7) Uiso 1 1 d . . . H7 H 0.763(3) 0.222(3) 0.044(2) 0.046(9) Uiso 1 1 d . . . H8 H 0.935(3) 0.361(3) 0.067(2) 0.042(9) Uiso 1 1 d . . . H9 H 1.011(3) 0.495(3) 0.194(2) 0.041(9) Uiso 1 1 d . . . H11 H 0.606(3) 0.182(2) 0.193(2) 0.034(8) Uiso 1 1 d . . . H12A H 0.461(4) 0.095(3) 0.051(2) 0.045(9) Uiso 1 1 d . . . H12B H 0.489(3) 0.210(3) 0.047(2) 0.050(10) Uiso 1 1 d . . . H12C H 0.548(3) 0.135(3) 0.008(3) 0.048(10) Uiso 1 1 d . . . H13A H 0.629(4) 0.020(3) 0.143(3) 0.062(12) Uiso 1 1 d . . . H13B H 0.729(4) 0.070(3) 0.117(3) 0.060(12) Uiso 1 1 d . . . H13C H 0.754(4) 0.090(3) 0.213(3) 0.058(11) Uiso 1 1 d . . . H14 H 0.882(3) 0.521(2) 0.357(2) 0.032(8) Uiso 1 1 d . . . H15A H 1.080(4) 0.553(3) 0.457(3) 0.065(12) Uiso 1 1 d . . . H15B H 1.127(4) 0.506(3) 0.387(3) 0.059(11) Uiso 1 1 d . . . H15C H 1.031(4) 0.434(3) 0.424(3) 0.066(12) Uiso 1 1 d . . . H16A H 1.010(3) 0.684(3) 0.369(3) 0.048(10) Uiso 1 1 d . . . H16B H 0.920(4) 0.645(3) 0.276(3) 0.052(11) Uiso 1 1 d . . . H16C H 1.060(5) 0.642(4) 0.294(3) 0.086(15) Uiso 1 1 d . . . H17 H 0.598(3) 0.185(2) 0.627(2) 0.029(7) Uiso 1 1 d . . . H20 H 0.579(3) 0.312(2) 0.902(2) 0.030(8) Uiso 1 1 d . . . H21 H 0.374(4) 0.230(3) 0.876(3) 0.056(11) Uiso 1 1 d . . . H22 H 0.222(3) 0.155(2) 0.739(2) 0.038(8) Uiso 1 1 d . . . H24 H 0.691(3) 0.370(2) 0.7359(19) 0.022(7) Uiso 1 1 d . . . H25A H 0.754(3) 0.233(3) 0.786(2) 0.043(9) Uiso 1 1 d . . . H25B H 0.861(4) 0.330(3) 0.841(2) 0.049(10) Uiso 1 1 d . . . H25C H 0.773(3) 0.280(2) 0.880(2) 0.039(9) Uiso 1 1 d . . . H26A H 0.728(3) 0.460(3) 0.914(2) 0.045(9) Uiso 1 1 d . . . H26B H 0.823(3) 0.501(3) 0.865(2) 0.041(9) Uiso 1 1 d . . . H26C H 0.685(3) 0.511(3) 0.831(2) 0.040(9) Uiso 1 1 d . . . H27 H 0.258(3) 0.185(2) 0.535(2) 0.035(8) Uiso 1 1 d . . . H28A H 0.187(3) 0.006(3) 0.486(2) 0.039(9) Uiso 1 1 d . . . H28B H 0.334(4) 0.043(3) 0.564(3) 0.058(11) Uiso 1 1 d . . . H28C H 0.229(4) 0.004(3) 0.590(3) 0.059(12) Uiso 1 1 d . . . H29A H 0.089(4) 0.223(3) 0.573(3) 0.056(11) Uiso 1 1 d . . . H29B H 0.069(4) 0.115(3) 0.596(2) 0.049(10) Uiso 1 1 d . . . H29C H 0.039(3) 0.117(3) 0.495(3) 0.047(9) Uiso 1 1 d . . . H30A H 0.540(3) 0.382(2) 0.129(2) 0.034(8) Uiso 1 1 d . . . H30B H 0.457(4) 0.459(3) 0.100(2) 0.049(10) Uiso 1 1 d . . . H31A H 0.602(4) 0.475(3) 0.025(3) 0.062(11) Uiso 1 1 d . . . H31B H 0.727(5) 0.506(3) 0.125(3) 0.082(14) Uiso 1 1 d . . . H31C H 0.626(4) 0.575(3) 0.091(3) 0.063(12) Uiso 1 1 d . . . H34 H 0.771(4) -0.212(3) -0.060(3) 0.062(11) Uiso 1 1 d . . . H35 H 0.367(3) 0.116(3) 0.299(2) 0.053(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02126(14) 0.01916(15) 0.01681(14) 0.00431(11) 0.00701(11) 0.00662(11) Ni2 0.01919(14) 0.01874(14) 0.01975(15) 0.00260(11) 0.00805(11) 0.00729(11) Cl1 0.0258(3) 0.0242(3) 0.0282(3) -0.0005(2) 0.0051(2) 0.0056(2) Cl2 0.0205(2) 0.0234(3) 0.0240(3) 0.0012(2) 0.0100(2) 0.0069(2) Cl3 0.0219(3) 0.0202(3) 0.0218(3) 0.0033(2) 0.0061(2) 0.0076(2) Cl4 0.0621(6) 0.0893(8) 0.0763(7) 0.0206(6) 0.0477(5) 0.0237(5) Cl5 0.1002(9) 0.0443(5) 0.0883(8) 0.0210(5) 0.0395(7) 0.0110(5) Cl6 0.0684(6) 0.0532(5) 0.0819(7) 0.0055(5) 0.0449(5) 0.0211(5) Cl7 0.1035(10) 0.0690(8) 0.1123(11) 0.0181(7) -0.0214(9) 0.0285(7) Cl8 0.1362(12) 0.0687(7) 0.1167(11) 0.0277(7) 0.0663(10) 0.0569(8) Cl9 0.0894(8) 0.0749(7) 0.1218(11) 0.0558(7) 0.0561(8) 0.0372(6) O1 0.0470(11) 0.0235(10) 0.0214(9) 0.0067(7) 0.0140(8) 0.0120(8) O2 0.0240(9) 0.0284(9) 0.0275(9) -0.0004(7) 0.0063(8) 0.0088(7) N1 0.0197(9) 0.0212(9) 0.0170(9) 0.0036(7) 0.0079(7) 0.0084(7) N2 0.0204(9) 0.0181(9) 0.0193(9) 0.0038(7) 0.0079(7) 0.0073(7) N3 0.0178(9) 0.0210(9) 0.0198(9) -0.0012(7) 0.0078(7) 0.0035(7) N4 0.0227(9) 0.0180(9) 0.0225(9) 0.0048(7) 0.0100(8) 0.0042(7) C1 0.0237(11) 0.0166(10) 0.0225(11) 0.0048(8) 0.0079(9) 0.0068(9) C2 0.0259(11) 0.0211(11) 0.0253(12) 0.0069(9) 0.0105(10) 0.0129(9) C3 0.0209(10) 0.0186(10) 0.0213(11) 0.0016(8) 0.0079(9) 0.0083(9) C4 0.0202(10) 0.0218(11) 0.0241(11) 0.0021(9) 0.0086(9) 0.0092(9) C5 0.0216(11) 0.0289(12) 0.0224(11) 0.0032(9) 0.0108(9) 0.0098(9) C6 0.0264(12) 0.0313(13) 0.0246(12) -0.0014(10) 0.0116(10) 0.0082(10) C7 0.0399(15) 0.0421(16) 0.0281(13) -0.0056(12) 0.0185(12) 0.0074(13) C8 0.0479(18) 0.0522(19) 0.0385(16) 0.0014(14) 0.0322(15) 0.0079(14) C9 0.0358(15) 0.0371(15) 0.0430(16) 0.0033(13) 0.0260(13) 0.0023(12) C10 0.0250(12) 0.0295(13) 0.0276(12) 0.0029(10) 0.0142(10) 0.0074(10) C11 0.0286(13) 0.0301(13) 0.0308(13) -0.0063(11) 0.0135(11) 0.0042(10) C12 0.0351(16) 0.0464(19) 0.0364(17) -0.0090(14) 0.0057(13) 0.0041(14) C13 0.0461(19) 0.0327(17) 0.061(2) 0.0000(15) 0.0212(18) 0.0129(15) C14 0.0231(12) 0.0282(13) 0.0352(14) -0.0025(10) 0.0155(11) 0.0043(10) C15 0.0421(18) 0.046(2) 0.0424(18) -0.0079(16) 0.0004(15) 0.0123(15) C16 0.063(2) 0.0318(16) 0.054(2) 0.0041(15) 0.0250(19) 0.0063(16) C17 0.0263(11) 0.0178(11) 0.0258(12) 0.0073(9) 0.0107(10) 0.0080(9) C18 0.0290(12) 0.0181(11) 0.0282(12) 0.0088(9) 0.0163(10) 0.0086(9) C19 0.0300(12) 0.0239(12) 0.0278(12) 0.0093(10) 0.0168(10) 0.0093(10) C20 0.0378(15) 0.0359(14) 0.0289(14) 0.0100(11) 0.0179(12) 0.0108(12) C21 0.0505(18) 0.0409(16) 0.0404(16) 0.0158(13) 0.0331(15) 0.0121(14) C22 0.0337(14) 0.0320(14) 0.0479(17) 0.0127(12) 0.0259(13) 0.0034(12) C23 0.0291(12) 0.0211(11) 0.0374(14) 0.0076(10) 0.0177(11) 0.0053(10) C24 0.0283(12) 0.0337(13) 0.0235(12) 0.0086(10) 0.0136(10) 0.0097(10) C25 0.0335(15) 0.0470(18) 0.0407(17) 0.0144(15) 0.0153(13) 0.0161(14) C26 0.0293(14) 0.0394(16) 0.0350(15) 0.0016(12) 0.0148(12) 0.0052(12) C27 0.0285(13) 0.0266(13) 0.0441(16) 0.0055(12) 0.0156(12) 0.0027(10) C28 0.048(2) 0.0306(16) 0.058(2) -0.0031(15) 0.0167(17) 0.0053(14) C29 0.0296(15) 0.052(2) 0.063(2) -0.0026(18) 0.0166(16) 0.0023(14) C30 0.0414(16) 0.0438(17) 0.0227(13) 0.0093(11) 0.0145(12) 0.0163(13) C31 0.0470(18) 0.062(2) 0.0357(16) 0.0230(15) 0.0243(14) 0.0255(16) C32 0.0249(13) 0.0497(18) 0.0410(16) -0.0004(14) 0.0036(12) 0.0120(12) C33 0.0383(19) 0.091(3) 0.066(3) -0.025(2) -0.0007(18) 0.008(2) C34 0.0329(15) 0.0496(18) 0.0378(16) 0.0074(14) 0.0114(13) 0.0093(13) C35 0.077(3) 0.0379(19) 0.081(3) 0.0211(19) 0.014(2) 0.0244(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.9631(19) . ? Ni1 O1 2.0334(18) . ? Ni1 N3 2.2433(19) . ? Ni1 Cl1 2.3773(6) . ? Ni1 Cl2 2.4363(6) 2_666 ? Ni1 Cl3 2.6405(6) 2_666 ? Ni1 Ni2 3.6697(4) 2_666 ? Ni1 Ni2 4.0232(4) . ? Ni1 Ni1 6.7923(6) 2_666 ? Ni2 N2 2.0021(18) . ? Ni2 O2 2.1103(18) . ? Ni2 N4 2.1815(19) . ? Ni2 Cl2 2.3594(6) . ? Ni2 Cl3 2.3604(6) . ? Ni2 Cl3 2.6546(6) 2_666 ? Ni2 Ni2 3.6291(6) 2_666 ? Cl1 O2 3.512(2) . ? Cl2 Ni1 2.4363(6) 2_666 ? Cl3 Ni1 2.6405(6) 2_666 ? Cl3 Ni2 2.6546(6) 2_666 ? Cl4 C34 1.739(3) . ? Cl5 C34 1.750(4) . ? Cl6 C34 1.752(3) . ? Cl7 C35 1.732(5) . ? Cl8 C35 1.754(5) . ? Cl9 C35 1.746(5) . ? O1 C30 1.446(3) . ? O1 H1O 0.72(3) . ? O2 C32 1.451(3) . ? O2 H2O 0.73(4) . ? N1 N2 1.318(3) . ? N1 C3 1.360(3) . ? N2 C1 1.357(3) . ? N3 C4 1.282(3) . ? N3 C5 1.446(3) . ? N4 C17 1.283(3) . ? N4 C18 1.433(3) . ? C1 C2 1.393(3) . ? C1 C17 1.438(3) . ? C2 C3 1.391(3) . ? C2 H2 0.87(3) . ? C3 C4 1.445(3) . ? C4 H4 0.92(3) . ? C5 C10 1.404(3) . ? C5 C6 1.405(3) . ? C6 C7 1.400(4) . ? C6 C11 1.526(4) . ? C7 C8 1.373(4) . ? C7 H7 0.96(3) . ? C8 C9 1.384(4) . ? C8 H8 0.93(3) . ? C9 C10 1.394(4) . ? C9 H9 0.92(3) . ? C10 C14 1.520(3) . ? C11 C13 1.527(4) . ? C11 C12 1.531(4) . ? C11 H11 0.92(3) . ? C12 H12A 0.91(4) . ? C12 H12B 0.99(4) . ? C12 H12C 0.90(4) . ? C13 H13A 0.91(4) . ? C13 H13B 0.89(4) . ? C13 H13C 0.93(4) . ? C14 C16 1.520(4) . ? C14 C15 1.522(4) . ? C14 H14 0.90(3) . ? C15 H15A 0.91(4) . ? C15 H15B 0.97(4) . ? C15 H15C 1.04(4) . ? C16 H16A 0.97(4) . ? C16 H16B 0.89(4) . ? C16 H16C 1.04(5) . ? C17 H17 0.91(3) . ? C18 C19 1.402(4) . ? C18 C23 1.413(3) . ? C19 C20 1.406(3) . ? C19 C24 1.531(3) . ? C20 C21 1.383(4) . ? C20 H20 0.91(3) . ? C21 C22 1.377(5) . ? C21 H21 0.82(4) . ? C22 C23 1.391(4) . ? C22 H22 0.92(3) . ? C23 C27 1.515(4) . ? C24 C26 1.528(4) . ? C24 C25 1.538(4) . ? C24 H24 0.90(3) . ? C25 H25A 0.95(4) . ? C25 H25B 0.89(4) . ? C25 H25C 0.93(3) . ? C26 H26A 0.99(4) . ? C26 H26B 0.99(3) . ? C26 H26C 0.94(3) . ? C27 C29 1.525(4) . ? C27 C28 1.535(4) . ? C27 H27 0.92(3) . ? C28 H28A 1.00(3) . ? C28 H28B 1.00(4) . ? C28 H28C 0.90(4) . ? C29 H29A 1.01(4) . ? C29 H29B 0.94(4) . ? C29 H29C 0.98(4) . ? C30 C31 1.503(4) . ? C30 H30A 0.99(3) . ? C30 H30B 0.98(4) . ? C31 H31A 1.03(4) . ? C31 H31B 0.99(5) . ? C31 H31C 0.97(4) . ? C32 C33 1.461(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34 0.92(4) . ? C35 H35 1.18(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 O1 168.46(8) . . ? N1 Ni1 N3 77.34(7) . . ? O1 Ni1 N3 91.45(8) . . ? N1 Ni1 Cl1 89.32(6) . . ? O1 Ni1 Cl1 94.22(6) . . ? N3 Ni1 Cl1 93.86(5) . . ? N1 Ni1 Cl2 93.80(6) . 2_666 ? O1 Ni1 Cl2 85.63(6) . 2_666 ? N3 Ni1 Cl2 101.25(5) . 2_666 ? Cl1 Ni1 Cl2 164.89(2) . 2_666 ? N1 Ni1 Cl3 88.31(5) . 2_666 ? O1 Ni1 Cl3 102.87(6) . 2_666 ? N3 Ni1 Cl3 165.65(5) . 2_666 ? Cl1 Ni1 Cl3 86.15(2) . 2_666 ? Cl2 Ni1 Cl3 79.175(19) 2_666 2_666 ? N1 Ni1 Ni2 90.15(5) . 2_666 ? O1 Ni1 Ni2 96.59(6) . 2_666 ? N3 Ni1 Ni2 138.29(5) . 2_666 ? Cl1 Ni1 Ni2 126.028(18) . 2_666 ? Cl2 Ni1 Ni2 39.308(14) 2_666 2_666 ? Cl3 Ni1 Ni2 39.899(13) 2_666 2_666 ? N1 Ni1 Ni2 47.63(5) . . ? O1 Ni1 Ni2 143.52(6) . . ? N3 Ni1 Ni2 124.98(5) . . ? Cl1 Ni1 Ni2 86.079(18) . . ? Cl2 Ni1 Ni2 85.134(15) 2_666 . ? Cl3 Ni1 Ni2 40.685(13) 2_666 . ? Ni2 Ni1 Ni2 56.069(9) 2_666 . ? N1 Ni1 Ni1 66.57(5) . 2_666 ? O1 Ni1 Ni1 122.56(6) . 2_666 ? N3 Ni1 Ni1 137.98(5) . 2_666 ? Cl1 Ni1 Ni1 106.098(18) . 2_666 ? Cl2 Ni1 Ni1 62.077(14) 2_666 2_666 ? Cl3 Ni1 Ni1 30.272(12) 2_666 2_666 ? Ni2 Ni1 Ni1 29.436(5) 2_666 2_666 ? Ni2 Ni1 Ni1 26.633(5) . 2_666 ? N2 Ni2 O2 86.00(8) . . ? N2 Ni2 N4 77.14(7) . . ? O2 Ni2 N4 97.91(7) . . ? N2 Ni2 Cl2 172.36(6) . . ? O2 Ni2 Cl2 94.77(6) . . ? N4 Ni2 Cl2 95.22(5) . . ? N2 Ni2 Cl3 94.20(6) . . ? O2 Ni2 Cl3 167.73(6) . . ? N4 Ni2 Cl3 94.09(5) . . ? Cl2 Ni2 Cl3 86.67(2) . . ? N2 Ni2 Cl3 86.73(6) . 2_666 ? O2 Ni2 Cl3 80.28(6) . 2_666 ? N4 Ni2 Cl3 163.87(5) . 2_666 ? Cl2 Ni2 Cl3 100.90(2) . 2_666 ? Cl3 Ni2 Cl3 87.48(2) . 2_666 ? N2 Ni2 Ni2 90.34(5) . 2_666 ? O2 Ni2 Ni2 120.80(6) . 2_666 ? N4 Ni2 Ni2 138.51(5) . 2_666 ? Cl2 Ni2 Ni2 95.769(18) . 2_666 ? Cl3 Ni2 Ni2 46.951(15) . 2_666 ? Cl3 Ni2 Ni2 40.525(13) 2_666 2_666 ? N2 Ni2 Ni1 46.31(5) . . ? O2 Ni2 Ni1 80.13(6) . . ? N4 Ni2 Ni1 123.45(5) . . ? Cl2 Ni2 Ni1 141.316(18) . . ? Cl3 Ni2 Ni1 91.120(16) . . ? Cl3 Ni2 Ni1 40.423(13) 2_666 . ? Ni2 Ni2 Ni1 57.034(9) 2_666 . ? Ni1 Cl1 O2 89.12(3) . . ? Ni2 Cl2 Ni1 99.84(2) . 2_666 ? Ni2 Cl3 Ni1 94.25(2) . 2_666 ? Ni2 Cl3 Ni2 92.52(2) . 2_666 ? Ni1 Cl3 Ni2 98.892(19) 2_666 2_666 ? C30 O1 Ni1 125.82(17) . . ? C30 O1 H1O 114(3) . . ? Ni1 O1 H1O 119(3) . . ? C32 O2 Ni2 123.14(16) . . ? C32 O2 Cl1 100.21(16) . . ? Ni2 O2 Cl1 104.62(7) . . ? C32 O2 H2O 108(3) . . ? Ni2 O2 H2O 101(3) . . ? Cl1 O2 H2O 8(3) . . ? N2 N1 C3 108.87(18) . . ? N2 N1 Ni1 132.23(14) . . ? C3 N1 Ni1 118.68(15) . . ? N1 N2 C1 108.57(18) . . ? N1 N2 Ni2 133.80(15) . . ? C1 N2 Ni2 117.55(15) . . ? C4 N3 C5 117.25(19) . . ? C4 N3 Ni1 110.04(15) . . ? C5 N3 Ni1 132.29(15) . . ? C17 N4 C18 117.1(2) . . ? C17 N4 Ni2 112.30(16) . . ? C18 N4 Ni2 130.14(15) . . ? N2 C1 C2 109.5(2) . . ? N2 C1 C17 114.5(2) . . ? C2 C1 C17 135.9(2) . . ? C3 C2 C1 103.7(2) . . ? C3 C2 H2 125(2) . . ? C1 C2 H2 131(2) . . ? N1 C3 C2 109.3(2) . . ? N1 C3 C4 114.9(2) . . ? C2 C3 C4 135.8(2) . . ? N3 C4 C3 118.8(2) . . ? N3 C4 H4 122.1(17) . . ? C3 C4 H4 119.0(17) . . ? C10 C5 C6 121.8(2) . . ? C10 C5 N3 118.4(2) . . ? C6 C5 N3 119.8(2) . . ? C7 C6 C5 117.5(2) . . ? C7 C6 C11 118.9(2) . . ? C5 C6 C11 123.6(2) . . ? C8 C7 C6 121.7(3) . . ? C8 C7 H7 121(2) . . ? C6 C7 H7 117(2) . . ? C7 C8 C9 119.7(3) . . ? C7 C8 H8 119(2) . . ? C9 C8 H8 121(2) . . ? C8 C9 C10 121.4(3) . . ? C8 C9 H9 120(2) . . ? C10 C9 H9 118(2) . . ? C9 C10 C5 117.8(2) . . ? C9 C10 C14 120.5(2) . . ? C5 C10 C14 121.6(2) . . ? C6 C11 C13 110.3(2) . . ? C6 C11 C12 112.2(3) . . ? C13 C11 C12 110.3(3) . . ? C6 C11 H11 107.4(19) . . ? C13 C11 H11 107.8(19) . . ? C12 C11 H11 108.8(19) . . ? C11 C12 H12A 109(2) . . ? C11 C12 H12B 112(2) . . ? H12A C12 H12B 109(3) . . ? C11 C12 H12C 112(2) . . ? H12A C12 H12C 106(3) . . ? H12B C12 H12C 107(3) . . ? C11 C13 H13A 113(3) . . ? C11 C13 H13B 113(3) . . ? H13A C13 H13B 105(3) . . ? C11 C13 H13C 111(2) . . ? H13A C13 H13C 110(3) . . ? H13B C13 H13C 106(3) . . ? C10 C14 C16 113.4(3) . . ? C10 C14 C15 109.6(2) . . ? C16 C14 C15 110.4(3) . . ? C10 C14 H14 106.6(19) . . ? C16 C14 H14 109.9(19) . . ? C15 C14 H14 106.7(19) . . ? C14 C15 H15A 106(3) . . ? C14 C15 H15B 110(2) . . ? H15A C15 H15B 111(3) . . ? C14 C15 H15C 112(2) . . ? H15A C15 H15C 108(3) . . ? H15B C15 H15C 110(3) . . ? C14 C16 H16A 112(2) . . ? C14 C16 H16B 113(3) . . ? H16A C16 H16B 103(3) . . ? C14 C16 H16C 116(3) . . ? H16A C16 H16C 105(3) . . ? H16B C16 H16C 107(4) . . ? N4 C17 C1 118.3(2) . . ? N4 C17 H17 122.8(18) . . ? C1 C17 H17 118.8(18) . . ? C19 C18 C23 122.5(2) . . ? C19 C18 N4 119.8(2) . . ? C23 C18 N4 117.7(2) . . ? C18 C19 C20 117.2(2) . . ? C18 C19 C24 123.9(2) . . ? C20 C19 C24 118.9(2) . . ? C21 C20 C19 121.0(3) . . ? C21 C20 H20 121.9(19) . . ? C19 C20 H20 117.1(19) . . ? C22 C21 C20 120.5(3) . . ? C22 C21 H21 120(3) . . ? C20 C21 H21 119(3) . . ? C21 C22 C23 121.5(3) . . ? C21 C22 H22 119(2) . . ? C23 C22 H22 120(2) . . ? C22 C23 C18 117.3(2) . . ? C22 C23 C27 122.3(2) . . ? C18 C23 C27 120.1(2) . . ? C26 C24 C19 112.8(2) . . ? C26 C24 C25 110.3(2) . . ? C19 C24 C25 110.1(2) . . ? C26 C24 H24 108.9(18) . . ? C19 C24 H24 106.7(18) . . ? C25 C24 H24 107.9(17) . . ? C24 C25 H25A 110(2) . . ? C24 C25 H25B 111(2) . . ? H25A C25 H25B 112(3) . . ? C24 C25 H25C 110(2) . . ? H25A C25 H25C 106(3) . . ? H25B C25 H25C 109(3) . . ? C24 C26 H26A 111(2) . . ? C24 C26 H26B 109.9(19) . . ? H26A C26 H26B 109(3) . . ? C24 C26 H26C 113(2) . . ? H26A C26 H26C 109(3) . . ? H26B C26 H26C 106(3) . . ? C23 C27 C29 113.9(3) . . ? C23 C27 C28 110.2(3) . . ? C29 C27 C28 110.7(3) . . ? C23 C27 H27 108(2) . . ? C29 C27 H27 107(2) . . ? C28 C27 H27 107(2) . . ? C27 C28 H28A 112.2(19) . . ? C27 C28 H28B 109(2) . . ? H28A C28 H28B 110(3) . . ? C27 C28 H28C 113(3) . . ? H28A C28 H28C 113(3) . . ? H28B C28 H28C 99(3) . . ? C27 C29 H29A 112(2) . . ? C27 C29 H29B 109(2) . . ? H29A C29 H29B 107(3) . . ? C27 C29 H29C 111(2) . . ? H29A C29 H29C 111(3) . . ? H29B C29 H29C 108(3) . . ? O1 C30 C31 111.5(3) . . ? O1 C30 H30A 104.9(18) . . ? C31 C30 H30A 111.8(18) . . ? O1 C30 H30B 108(2) . . ? C31 C30 H30B 112(2) . . ? H30A C30 H30B 108(3) . . ? C30 C31 H31A 109(2) . . ? C30 C31 H31B 115(3) . . ? H31A C31 H31B 112(3) . . ? C30 C31 H31C 107(2) . . ? H31A C31 H31C 99(3) . . ? H31B C31 H31C 114(4) . . ? O2 C32 C33 113.0(3) . . ? O2 C32 H32A 109.0 . . ? C33 C32 H32A 109.0 . . ? O2 C32 H32B 109.0 . . ? C33 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Cl4 C34 Cl5 111.03(18) . . ? Cl4 C34 Cl6 110.68(18) . . ? Cl5 C34 Cl6 109.85(18) . . ? Cl4 C34 H34 109(2) . . ? Cl5 C34 H34 104(2) . . ? Cl6 C34 H34 112(3) . . ? Cl7 C35 Cl9 111.1(3) . . ? Cl7 C35 Cl8 112.9(3) . . ? Cl9 C35 Cl8 108.1(2) . . ? Cl7 C35 H35 110.0(18) . . ? Cl9 C35 H35 132.7(18) . . ? Cl8 C35 H35 75.5(17) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.686 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.083 #====END