# 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_email stliu@ntu.edu.tw _publ_contact_author_name 'Shiuh-Tzung Liu' loop_ _publ_author_name 'Ting-Peng Cheng' 'Yi-Hung Liu' 'Shiuh-Tzung Liu' data_ic14048 _database_code_depnum_ccdc_archive 'CCDC 835817' #TrackingRef '- ic14048-complex 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 Cl8 N6 Ni2 O2' _chemical_formula_weight 755.44 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 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 10.9327(6) _cell_length_b 16.7419(6) _cell_length_c 16.6176(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.925(5) _cell_angle_gamma 90.00 _cell_volume 3034.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7494 _cell_measurement_theta_min 3.0624 _cell_measurement_theta_max 30.0034 _exptl_crystal_description ? _exptl_crystal_colour ? _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 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 1.973 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84986 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22170 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6957 _reflns_number_gt 4379 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6957 _refine_ls_number_parameters 359 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1878 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.33584(7) 0.09939(4) 0.67818(5) 0.0182(2) Uani 1 1 d . . . Ni2 Ni 0.20817(7) -0.07380(4) 0.69607(4) 0.0183(2) Uani 1 1 d . . . Cl3 Cl 0.41185(13) -0.02461(8) 0.72912(9) 0.0219(3) Uani 1 1 d . . . Cl1 Cl 0.24801(14) 0.21727(8) 0.61749(9) 0.0256(3) Uani 1 1 d . . . Cl2 Cl 0.14046(13) 0.05860(7) 0.72382(9) 0.0217(3) Uani 1 1 d . . . Cl4 Cl 0.28938(14) -0.20088(8) 0.66062(9) 0.0250(3) Uani 1 1 d . . . O1 O 0.3778(4) 0.1632(2) 0.7829(3) 0.0240(9) Uani 1 1 d D . . H1 H 0.331(5) 0.199(3) 0.788(5) 0.036 Uiso 1 1 d D . . O2 O 0.1907(4) -0.1137(2) 0.8122(3) 0.0260(10) Uani 1 1 d D . . H2 H 0.206(7) -0.1581(19) 0.825(4) 0.039 Uiso 1 1 d D . . N1 N 0.4991(4) 0.1337(3) 0.6365(3) 0.0225(11) Uani 1 1 d . . . N2 N 0.4997(4) 0.1297(3) 0.5550(3) 0.0202(10) Uani 1 1 d . . . N3 N 0.3322(4) 0.0472(2) 0.5586(3) 0.0191(10) Uani 1 1 d . . . N4 N 0.1770(4) -0.0458(2) 0.5692(3) 0.0170(10) Uani 1 1 d . . . N5 N 0.0129(4) -0.1283(3) 0.5857(3) 0.0206(10) Uani 1 1 d . . . N6 N 0.0376(5) -0.1185(3) 0.6668(3) 0.0217(11) Uani 1 1 d . . . C1 C 0.5941(6) 0.1790(3) 0.6603(4) 0.0294(15) Uani 1 1 d . . . H1A H 0.6165 0.1926 0.7148 0.035 Uiso 1 1 calc R . . C2 C 0.6568(6) 0.2042(4) 0.5943(5) 0.0332(16) Uani 1 1 d . . . H2A H 0.7275 0.2373 0.5956 0.040 Uiso 1 1 calc R . . C3 C 0.5967(6) 0.1720(3) 0.5280(4) 0.0310(15) Uani 1 1 d . . . H3A H 0.6174 0.1776 0.4737 0.037 Uiso 1 1 calc R . . C4 C 0.4097(5) 0.0834(3) 0.5121(4) 0.0191(12) Uani 1 1 d . . . C5 C 0.4098(6) 0.0783(3) 0.4287(4) 0.0224(13) Uani 1 1 d . . . H5A H 0.4705 0.1039 0.3996 0.027 Uiso 1 1 calc R . . C6 C 0.3166(6) 0.0341(3) 0.3904(4) 0.0247(13) Uani 1 1 d . . . H6A H 0.3092 0.0312 0.3332 0.030 Uiso 1 1 calc R . . C7 C 0.2329(5) -0.0066(3) 0.4353(4) 0.0220(13) Uani 1 1 d . . . C8 C 0.2465(5) -0.0019(3) 0.5196(4) 0.0174(11) Uani 1 1 d . . . C9 C 0.1334(6) -0.0519(3) 0.4009(4) 0.0245(13) Uani 1 1 d . . . H9A H 0.1190 -0.0550 0.3440 0.029 Uiso 1 1 calc R . . C10 C 0.0576(6) -0.0914(3) 0.4502(4) 0.0236(13) Uani 1 1 d . . . H10A H -0.0119 -0.1204 0.4287 0.028 Uiso 1 1 calc R . . C11 C 0.0868(5) -0.0873(3) 0.5328(4) 0.0200(12) Uani 1 1 d . . . C12 C -0.0857(6) -0.1770(3) 0.5696(4) 0.0282(15) Uani 1 1 d . . . H12A H -0.1193 -0.1931 0.5179 0.034 Uiso 1 1 calc R . . C13 C -0.1266(6) -0.1983(4) 0.6428(4) 0.0281(14) Uani 1 1 d . . . H13A H -0.1946 -0.2315 0.6523 0.034 Uiso 1 1 calc R . . C14 C -0.0476(5) -0.1609(3) 0.7003(4) 0.0251(13) Uani 1 1 d . . . H14A H -0.0540 -0.1653 0.7568 0.030 Uiso 1 1 calc R . . C15 C 0.4022(9) 0.1296(4) 0.8613(5) 0.051(2) Uani 1 1 d . . . H15A H 0.4190 0.1725 0.9006 0.077 Uiso 1 1 calc R . . H15B H 0.4737 0.0942 0.8611 0.077 Uiso 1 1 calc R . . H15C H 0.3308 0.0989 0.8761 0.077 Uiso 1 1 calc R . . C16 C 0.2185(8) -0.0708(4) 0.8831(5) 0.046(2) Uani 1 1 d . . . H16A H 0.2023 -0.1041 0.9297 0.069 Uiso 1 1 calc R . . H16B H 0.1676 -0.0226 0.8832 0.069 Uiso 1 1 calc R . . H16C H 0.3053 -0.0555 0.8862 0.069 Uiso 1 1 calc R . . C17 C -0.4901(7) -0.2053(5) 0.8192(5) 0.050(2) Uani 1 1 d . . . H17A H -0.5218 -0.2607 0.8147 0.060 Uiso 1 1 calc R . . H17B H -0.5556 -0.1688 0.7977 0.060 Uiso 1 1 calc R . . Cl5 Cl -0.3639(3) -0.1959(2) 0.76304(18) 0.0883(9) Uani 1 1 d . . . Cl6 Cl -0.4512(2) -0.18237(14) 0.92321(15) 0.0621(6) Uani 1 1 d . . . C18 C 0.5209(16) 0.3653(11) 0.4207(11) 0.106(5) Uani 0.580(5) 1 d PDU A 1 H18A H 0.4892 0.4104 0.3869 0.128 Uiso 0.580(5) 1 calc PR A 1 H18B H 0.5717 0.3316 0.3872 0.128 Uiso 0.580(5) 1 calc PR A 1 Cl7 Cl 0.4024(3) 0.31118(15) 0.44816(18) 0.0321(8) Uani 0.580(5) 1 d PDU A 1 Cl8 Cl 0.6150(7) 0.4038(4) 0.5024(6) 0.130(3) Uani 0.580(5) 1 d PDU A 1 C18' C 0.780(3) 0.4988(17) 0.607(2) 0.110(7) Uani 0.420(5) 1 d PU A 2 H18C H 0.8104 0.5287 0.5608 0.132 Uiso 0.420(5) 1 calc PR A 2 H18D H 0.8476 0.4658 0.6321 0.132 Uiso 0.420(5) 1 calc PR A 2 Cl7' Cl 0.6505(10) 0.4399(5) 0.5770(8) 0.134(4) Uani 0.420(5) 1 d PU A 2 Cl8' Cl 0.7149(9) 0.5679(4) 0.6825(3) 0.103(3) Uani 0.420(5) 1 d PU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0206(4) 0.0162(3) 0.0176(4) -0.0009(3) 0.0005(3) 0.0003(3) Ni2 0.0208(4) 0.0170(3) 0.0169(4) 0.0007(3) 0.0002(3) 0.0000(3) Cl3 0.0220(7) 0.0189(6) 0.0245(8) 0.0014(5) 0.0003(6) 0.0018(5) Cl1 0.0350(9) 0.0182(6) 0.0227(8) -0.0008(5) -0.0036(6) 0.0020(6) Cl2 0.0226(7) 0.0204(6) 0.0222(8) -0.0010(5) 0.0025(6) 0.0023(5) Cl4 0.0335(8) 0.0187(6) 0.0234(8) 0.0003(5) 0.0059(7) 0.0019(6) O1 0.025(2) 0.025(2) 0.021(2) -0.0047(17) -0.0031(19) 0.0020(17) O2 0.038(3) 0.021(2) 0.020(2) 0.0025(17) 0.005(2) 0.0018(19) N1 0.025(3) 0.017(2) 0.026(3) -0.0009(19) 0.000(2) -0.0007(19) N2 0.025(3) 0.018(2) 0.018(3) 0.0004(18) 0.005(2) 0.0004(19) N3 0.019(2) 0.015(2) 0.023(3) -0.0003(18) 0.000(2) 0.0050(18) N4 0.018(2) 0.017(2) 0.015(3) -0.0007(18) 0.000(2) 0.0036(18) N5 0.022(3) 0.017(2) 0.022(3) 0.0022(19) -0.003(2) 0.0011(19) N6 0.025(3) 0.022(2) 0.018(3) -0.0009(19) -0.001(2) -0.001(2) C1 0.026(3) 0.024(3) 0.037(4) -0.007(3) -0.003(3) 0.001(2) C2 0.026(4) 0.028(3) 0.046(5) -0.002(3) 0.004(3) -0.007(3) C3 0.031(4) 0.029(3) 0.034(4) 0.003(3) 0.010(3) -0.003(3) C4 0.019(3) 0.017(3) 0.022(3) 0.002(2) 0.005(2) 0.006(2) C5 0.028(3) 0.020(3) 0.020(3) 0.005(2) 0.008(3) 0.006(2) C6 0.033(4) 0.026(3) 0.015(3) 0.001(2) 0.001(3) 0.007(3) C7 0.027(3) 0.021(3) 0.018(3) -0.005(2) 0.002(3) 0.007(2) C8 0.019(3) 0.015(2) 0.018(3) 0.000(2) -0.004(2) 0.006(2) C9 0.031(3) 0.026(3) 0.016(3) -0.004(2) -0.002(3) 0.006(2) C10 0.023(3) 0.020(3) 0.027(4) -0.002(2) -0.002(3) 0.004(2) C11 0.018(3) 0.017(3) 0.024(3) -0.001(2) 0.000(2) 0.008(2) C12 0.028(3) 0.021(3) 0.034(4) -0.002(3) -0.013(3) -0.001(2) C13 0.021(3) 0.031(3) 0.033(4) 0.001(3) 0.003(3) -0.002(3) C14 0.025(3) 0.028(3) 0.022(3) 0.005(2) 0.003(3) -0.001(2) C15 0.082(6) 0.038(4) 0.031(5) -0.001(3) -0.008(4) 0.001(4) C16 0.076(6) 0.034(4) 0.029(4) -0.002(3) 0.006(4) 0.005(4) C17 0.036(4) 0.066(5) 0.048(5) 0.021(4) 0.010(4) 0.013(4) Cl5 0.0599(16) 0.143(3) 0.0648(18) 0.0341(17) 0.0234(14) 0.0322(16) Cl6 0.0534(13) 0.0780(14) 0.0548(15) -0.0033(11) 0.0037(11) 0.0041(11) C18 0.123(12) 0.071(9) 0.131(12) -0.001(9) 0.054(10) 0.000(9) Cl7 0.0309(16) 0.0295(14) 0.0361(18) -0.0019(11) 0.0035(12) 0.0034(11) Cl8 0.142(6) 0.100(4) 0.151(7) 0.040(4) 0.021(5) -0.019(4) C18' 0.154(14) 0.093(12) 0.081(13) 0.011(11) 0.002(12) -0.031(12) Cl7' 0.154(8) 0.097(6) 0.141(8) -0.005(5) -0.051(7) 0.002(5) Cl8' 0.185(8) 0.106(5) 0.021(3) -0.002(3) 0.034(4) -0.070(5) _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 2.041(5) . ? Ni1 O1 2.067(4) . ? Ni1 N3 2.168(5) . ? Ni1 Cl3 2.3708(15) . ? Ni1 Cl1 2.3878(15) . ? Ni1 Cl2 2.4136(16) . ? Ni2 N6 2.037(5) . ? Ni2 O2 2.063(4) . ? Ni2 N4 2.163(5) . ? Ni2 Cl2 2.3918(14) . ? Ni2 Cl4 2.3944(15) . ? Ni2 Cl3 2.4024(16) . ? O1 C15 1.428(9) . ? O2 C16 1.396(8) . ? N1 C1 1.325(8) . ? N1 N2 1.356(7) . ? N2 C3 1.376(8) . ? N2 C4 1.407(8) . ? N3 C4 1.331(7) . ? N3 C8 1.375(7) . ? N4 C11 1.318(7) . ? N4 C8 1.373(7) . ? N5 C12 1.364(8) . ? N5 N6 1.366(7) . ? N5 C11 1.412(7) . ? N6 C14 1.324(7) . ? C1 C2 1.399(10) . ? C2 C3 1.355(10) . ? C4 C5 1.390(8) . ? C5 C6 1.379(9) . ? C6 C7 1.397(8) . ? C7 C8 1.401(8) . ? C7 C9 1.414(9) . ? C9 C10 1.374(9) . ? C10 C11 1.389(9) . ? C12 C13 1.373(9) . ? C13 C14 1.392(9) . ? C17 Cl5 1.725(8) . ? C17 Cl6 1.793(9) . ? C18 Cl7 1.670(14) . ? C18 Cl8 1.768(16) . ? C18' Cl7' 1.77(3) . ? C18' Cl8' 1.88(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 O1 89.54(18) . . ? N1 Ni1 N3 76.33(19) . . ? O1 Ni1 N3 165.70(17) . . ? N1 Ni1 Cl3 94.26(13) . . ? O1 Ni1 Cl3 95.72(12) . . ? N3 Ni1 Cl3 87.62(12) . . ? N1 Ni1 Cl1 87.69(14) . . ? O1 Ni1 Cl1 89.32(12) . . ? N3 Ni1 Cl1 87.95(12) . . ? Cl3 Ni1 Cl1 174.60(6) . . ? N1 Ni1 Cl2 178.45(16) . . ? O1 Ni1 Cl2 91.82(12) . . ? N3 Ni1 Cl2 102.28(13) . . ? Cl3 Ni1 Cl2 86.34(5) . . ? Cl1 Ni1 Cl2 91.58(6) . . ? N6 Ni2 O2 87.85(19) . . ? N6 Ni2 N4 76.47(19) . . ? O2 Ni2 N4 164.33(18) . . ? N6 Ni2 Cl2 95.54(13) . . ? O2 Ni2 Cl2 94.01(12) . . ? N4 Ni2 Cl2 87.54(12) . . ? N6 Ni2 Cl4 87.90(13) . . ? O2 Ni2 Cl4 90.12(12) . . ? N4 Ni2 Cl4 89.37(12) . . ? Cl2 Ni2 Cl4 174.72(6) . . ? N6 Ni2 Cl3 178.30(14) . . ? O2 Ni2 Cl3 92.35(13) . . ? N4 Ni2 Cl3 103.31(13) . . ? Cl2 Ni2 Cl3 86.13(5) . . ? Cl4 Ni2 Cl3 90.42(5) . . ? Ni1 Cl3 Ni2 85.51(5) . . ? Ni2 Cl2 Ni1 84.80(5) . . ? C15 O1 Ni1 125.6(4) . . ? C16 O2 Ni2 126.5(4) . . ? C1 N1 N2 105.6(5) . . ? C1 N1 Ni1 138.2(5) . . ? N2 N1 Ni1 112.9(4) . . ? N1 N2 C3 110.9(5) . . ? N1 N2 C4 118.8(4) . . ? C3 N2 C4 130.2(5) . . ? C4 N3 C8 116.0(5) . . ? C4 N3 Ni1 112.1(4) . . ? C8 N3 Ni1 130.0(4) . . ? C11 N4 C8 115.7(5) . . ? C11 N4 Ni2 113.4(4) . . ? C8 N4 Ni2 130.1(4) . . ? C12 N5 N6 111.4(5) . . ? C12 N5 C11 130.3(6) . . ? N6 N5 C11 118.2(5) . . ? C14 N6 N5 104.7(5) . . ? C14 N6 Ni2 139.1(4) . . ? N5 N6 Ni2 113.3(4) . . ? N1 C1 C2 110.8(6) . . ? C3 C2 C1 106.3(6) . . ? C2 C3 N2 106.3(6) . . ? N3 C4 C5 126.5(6) . . ? N3 C4 N2 114.1(5) . . ? C5 C4 N2 119.4(5) . . ? C6 C5 C4 116.2(5) . . ? C5 C6 C7 120.4(6) . . ? C6 C7 C8 118.5(5) . . ? C6 C7 C9 124.0(6) . . ? C8 C7 C9 117.4(5) . . ? N4 C8 N3 115.1(5) . . ? N4 C8 C7 123.0(5) . . ? N3 C8 C7 121.9(5) . . ? C10 C9 C7 119.7(6) . . ? C9 C10 C11 117.2(6) . . ? N4 C11 C10 126.5(5) . . ? N4 C11 N5 114.3(5) . . ? C10 C11 N5 119.2(5) . . ? N5 C12 C13 106.4(6) . . ? C12 C13 C14 105.5(5) . . ? N6 C14 C13 112.0(6) . . ? Cl5 C17 Cl6 110.9(5) . . ? Cl7 C18 Cl8 114.2(11) . . ? Cl7' C18' Cl8' 101.3(18) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.075 _refine_diff_density_min -1.279 _refine_diff_density_rms 0.164 # Attachment '- ic14842-complex 4.cif' data_ic14842 _database_code_depnum_ccdc_archive 'CCDC 835818' #TrackingRef '- ic14842-complex 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H106 Cl16 N18 Ni6 O12' _chemical_formula_weight 2287.17 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 Trigonal _symmetry_space_group_name_H-M P3(2)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 14.76480(10) _cell_length_b 14.76480(10) _cell_length_c 36.4182(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6875.50(13) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 20802 _cell_measurement_theta_min 2.9714 _cell_measurement_theta_max 28.9176 _exptl_crystal_description ? _exptl_crystal_colour ? _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 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 1.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94230 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Oxford Diffraction Gemini A' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42248 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10505 _reflns_number_gt 9569 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0837P)^2^+16.7407P] 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(17) _refine_ls_number_reflns 10505 _refine_ls_number_parameters 523 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1587 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.48439(5) 0.66593(5) 0.150899(19) 0.02269(15) Uani 1 1 d . . . Ni2 Ni 0.69654(5) 0.80490(5) 0.104815(19) 0.02217(15) Uani 1 1 d . . . Cl1 Cl 0.45214(11) 0.55614(11) 0.20212(4) 0.0314(3) Uani 1 1 d . . . Cl2 Cl 0.66543(10) 0.77643(10) 0.16818(3) 0.0239(3) Uani 1 1 d . . . Cl3 Cl 0.52377(11) 0.77153(10) 0.09595(4) 0.0268(3) Uani 1 1 d . . . O1 O 0.4498(3) 0.7676(3) 0.17674(13) 0.0311(9) Uani 1 1 d . . . H51A H 0.4433 0.8155 0.1670 0.037 Uiso 1 1 calc R . . O2 O 0.7390(3) 0.9582(3) 0.11397(11) 0.0288(9) Uani 1 1 d . . . H52A H 0.7530 0.9880 0.1345 0.035 Uiso 1 1 calc R . . O3 O 0.7205(4) 0.8211(3) 0.04620(11) 0.0328(9) Uani 1 1 d . . . H53A H 0.7661 0.8097 0.0370 0.039 Uiso 1 1 calc R . . N1 N 0.3308(4) 0.5680(4) 0.13560(13) 0.0259(10) Uani 1 1 d . . . N2 N 0.3175(4) 0.4705(4) 0.12893(13) 0.0271(10) Uani 1 1 d . . . N3 N 0.4958(4) 0.5553(3) 0.11694(12) 0.0232(9) Uani 1 1 d . . . N4 N 0.6727(4) 0.6504(3) 0.10180(12) 0.0229(9) Uani 1 1 d . . . N5 N 0.8525(4) 0.7450(4) 0.09677(14) 0.0270(10) Uani 1 1 d . . . N6 N 0.8447(4) 0.8308(4) 0.10545(13) 0.0267(10) Uani 1 1 d . . . C1 C 0.4326(7) 0.7667(6) 0.2165(2) 0.0488(19) Uani 1 1 d . . . H1A H 0.4174 0.8223 0.2228 0.073 Uiso 1 1 calc R . . H1B H 0.4955 0.7783 0.2296 0.073 Uiso 1 1 calc R . . H1C H 0.3733 0.6989 0.2237 0.073 Uiso 1 1 calc R . . C2 C 0.7493(7) 1.0302(6) 0.0864(2) 0.0477(18) Uani 1 1 d . . . H2A H 0.7707 1.0983 0.0977 0.072 Uiso 1 1 calc R . . H2B H 0.6822 1.0047 0.0739 0.072 Uiso 1 1 calc R . . H2C H 0.8024 1.0376 0.0686 0.072 Uiso 1 1 calc R . . C3 C 0.6729(6) 0.8482(6) 0.0182(2) 0.0467(17) Uani 1 1 d . . . H3A H 0.7041 0.8478 -0.0055 0.070 Uiso 1 1 calc R . . H3B H 0.6836 0.9182 0.0230 0.070 Uiso 1 1 calc R . . H3C H 0.5978 0.7975 0.0177 0.070 Uiso 1 1 calc R . . C4 C 0.2166(6) 0.6382(5) 0.1541(2) 0.0383(14) Uani 1 1 d . . . H4A H 0.2811 0.7055 0.1511 0.057 Uiso 1 1 calc R . . H4B H 0.1913 0.6319 0.1794 0.057 Uiso 1 1 calc R . . H4C H 0.1634 0.6341 0.1371 0.057 Uiso 1 1 calc R . . C5 C 0.2378(5) 0.5520(5) 0.14632(16) 0.0303(12) Uani 1 1 d . . . C6 C 0.1656(5) 0.4449(5) 0.14781(16) 0.0340(14) Uani 1 1 d . . . H6A H 0.0941 0.4139 0.1546 0.041 Uiso 1 1 calc R . . C7 C 0.2167(5) 0.3928(5) 0.13763(16) 0.0327(13) Uani 1 1 d . . . C8 C 0.1752(6) 0.2780(5) 0.13584(19) 0.0455(18) Uani 1 1 d . . . H8A H 0.1016 0.2410 0.1433 0.068 Uiso 1 1 calc R . . H8B H 0.2156 0.2592 0.1524 0.068 Uiso 1 1 calc R . . H8C H 0.1812 0.2582 0.1106 0.068 Uiso 1 1 calc R . . C9 C 0.4027(4) 0.4660(4) 0.11472(15) 0.0243(11) Uani 1 1 d . . . C10 C 0.3899(5) 0.3762(4) 0.09728(17) 0.0290(12) Uani 1 1 d . . . H10A H 0.3222 0.3166 0.0946 0.035 Uiso 1 1 calc R . . C11 C 0.4764(5) 0.3751(4) 0.08401(16) 0.0312(13) Uani 1 1 d . . . H11A H 0.4698 0.3137 0.0730 0.037 Uiso 1 1 calc R . . C12 C 0.5753(5) 0.4663(4) 0.08699(16) 0.0306(13) Uani 1 1 d . . . C13 C 0.5809(4) 0.5565(4) 0.10170(14) 0.0223(10) Uani 1 1 d . . . C14 C 0.6672(6) 0.4727(5) 0.07490(17) 0.0337(13) Uani 1 1 d . . . H14A H 0.6651 0.4139 0.0634 0.040 Uiso 1 1 calc R . . C15 C 0.7589(6) 0.5607(5) 0.07918(18) 0.0361(14) Uani 1 1 d . . . H15A H 0.8227 0.5631 0.0731 0.043 Uiso 1 1 calc R . . C16 C 0.7584(5) 0.6488(4) 0.09282(15) 0.0259(11) Uani 1 1 d . . . C17 C 0.9961(6) 0.6958(6) 0.0907(3) 0.0497(19) Uani 1 1 d . . . H17A H 1.0724 0.7330 0.0933 0.075 Uiso 1 1 calc R . . H17B H 0.9770 0.6675 0.0658 0.075 Uiso 1 1 calc R . . H17C H 0.9648 0.6384 0.1085 0.075 Uiso 1 1 calc R . . C18 C 0.9566(5) 0.7702(5) 0.09766(18) 0.0328(13) Uani 1 1 d . . . C19 C 1.0119(5) 0.8716(5) 0.10649(18) 0.0315(13) Uani 1 1 d . . . H19A H 1.0857 0.9108 0.1095 0.038 Uiso 1 1 calc RD . . C20 C 0.9434(4) 0.9101(5) 0.11064(15) 0.0274(12) Uani 1 1 d . . . C21 C 0.9681(6) 1.0179(5) 0.1183(2) 0.0403(15) Uani 1 1 d . . . H21A H 0.9031 1.0205 0.1197 0.060 Uiso 1 1 calc R . . H21B H 1.0122 1.0641 0.0986 0.060 Uiso 1 1 calc R . . H21C H 1.0054 1.0410 0.1417 0.060 Uiso 1 1 calc R . . Ni3 Ni 0.87442(6) 0.72972(6) 0.32983(2) 0.02627(17) Uani 1 1 d . . . Cl4 Cl 0.99007(12) 0.82644(12) 0.37879(4) 0.0295(3) Uani 1 1 d . . . Cl5 Cl 0.74440(13) 0.61747(14) 0.37363(4) 0.0397(3) Uani 1 1 d . . . O4 O 0.8291(4) 0.8421(4) 0.32867(12) 0.0375(10) Uani 1 1 d . . . H54A H 0.8503 0.8927 0.3141 0.045 Uiso 1 1 calc R . . N7 N 0.7708(4) 0.6368(4) 0.29010(13) 0.0287(10) Uani 1 1 d . . . N8 N 0.7547(4) 0.5372(4) 0.29287(13) 0.0278(10) Uani 1 1 d . . . N9 N 0.9143(4) 0.6119(4) 0.32171(12) 0.0262(10) Uani 1 1 d . . . C22 C 0.7549(7) 0.8438(8) 0.3535(2) 0.053(2) Uani 1 1 d . . . H22A H 0.7457 0.9035 0.3478 0.080 Uiso 1 1 calc R . . H22B H 0.7805 0.8501 0.3788 0.080 Uiso 1 1 calc R . . H22C H 0.6878 0.7788 0.3510 0.080 Uiso 1 1 calc R . . C23 C 0.6744(6) 0.7191(5) 0.26516(19) 0.0386(15) Uani 1 1 d . . . H23A H 0.7373 0.7839 0.2726 0.058 Uiso 1 1 calc R . . H23B H 0.6134 0.7135 0.2780 0.058 Uiso 1 1 calc R . . H23C H 0.6645 0.7200 0.2386 0.058 Uiso 1 1 calc R . . C24 C 0.6868(5) 0.6281(5) 0.27486(15) 0.0290(12) Uani 1 1 d . . . C25 C 0.6127(5) 0.5216(5) 0.26827(16) 0.0326(13) Uani 1 1 d . . . H25A H 0.5451 0.4948 0.2578 0.039 Uiso 1 1 calc R . . C26 C 0.6567(5) 0.4659(5) 0.27968(15) 0.0287(12) Uani 1 1 d . . . C27 C 0.6081(5) 0.3501(5) 0.2795(2) 0.0355(14) Uani 1 1 d . . . H27A H 0.5381 0.3187 0.2687 0.053 Uiso 1 1 calc R . . H27B H 0.6029 0.3248 0.3047 0.053 Uiso 1 1 calc R . . H27C H 0.6514 0.3304 0.2649 0.053 Uiso 1 1 calc R . . C28 C 0.8374(5) 0.5262(5) 0.30664(15) 0.0265(12) Uani 1 1 d . . . C29 C 0.8365(5) 0.4317(5) 0.30237(18) 0.0323(13) Uani 1 1 d . . . H29A H 0.7811 0.3748 0.2896 0.039 Uiso 1 1 calc R . . C30 C 0.9158(5) 0.4229(5) 0.31675(17) 0.0333(13) Uani 1 1 d . . . H30A H 0.9149 0.3582 0.3157 0.040 Uiso 1 1 calc R . . C31 C 1.0000 0.5105(5) 0.3333 0.0267(15) Uani 1 2 d S . . C32 C 1.0000 0.6083(5) 0.3333 0.0215(14) Uani 1 2 d S . . Cl6 Cl 0.60038(16) 0.0000 0.1667 0.0369(5) Uani 1 2 d S . . Cl7 Cl 1.0000 1.07917(18) 0.3333 0.0566(7) Uani 1 2 d S . . C33 C 0.9592(15) 0.4825(17) -0.0233(5) 0.137(7) Uani 1 1 d . . . H33A H 0.9251 0.4828 -0.0467 0.165 Uiso 1 1 calc R . . H33B H 0.9861 0.4333 -0.0256 0.165 Uiso 1 1 calc R . . Cl8 Cl 0.8730(3) 0.4469(3) 0.01220(11) 0.1005(10) Uani 1 1 d . . . Cl9 Cl 1.0728(3) 0.6230(3) -0.01159(11) 0.1083(12) Uani 1 1 d . . . O5 O 0.4026(10) 0.1086(11) 0.2325(4) 0.154(5) Uiso 1 1 d D . . H5 H 0.3733 0.1095 0.2129 0.185 Uiso 1 1 calc RD . . O6 O 0.3249(13) 0.1158(13) 0.1476(4) 0.181(6) Uiso 1 1 d D . . H6 H 0.3026 0.0715 0.1646 0.217 Uiso 1 1 calc R . . C34 C 0.4616(16) 0.0743(16) 0.2265(5) 0.143(7) Uiso 1 1 d D . . H34A H 0.5267 0.1153 0.2403 0.214 Uiso 1 1 calc R . . H34B H 0.4772 0.0793 0.2002 0.214 Uiso 1 1 calc R . . H34C H 0.4280 0.0010 0.2342 0.214 Uiso 1 1 calc R . . C35 C 0.2664(11) 0.0789(12) 0.1203(5) 0.134(6) Uiso 1 1 d D . . H35A H 0.2135 0.1004 0.1207 0.201 Uiso 1 1 calc R . . H35B H 0.2319 0.0024 0.1208 0.201 Uiso 1 1 calc R . . H35C H 0.3081 0.1050 0.0978 0.201 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 0.0194(3) 0.0149(3) 0.0276(3) 0.0006(3) -0.0016(3) 0.0040(3) Ni2 0.0208(3) 0.0145(3) 0.0261(3) 0.0005(2) -0.0001(3) 0.0050(3) Cl1 0.0295(7) 0.0252(7) 0.0304(7) 0.0054(5) -0.0022(5) 0.0068(6) Cl2 0.0210(6) 0.0195(6) 0.0264(6) -0.0012(4) -0.0022(5) 0.0066(5) Cl3 0.0228(6) 0.0184(6) 0.0330(7) 0.0021(5) -0.0046(5) 0.0057(5) O1 0.023(2) 0.0189(19) 0.047(3) 0.0033(17) 0.0039(18) 0.0077(16) O2 0.029(2) 0.0172(18) 0.033(2) -0.0020(16) -0.0007(17) 0.0064(16) O3 0.037(2) 0.028(2) 0.031(2) -0.0016(17) -0.0037(17) 0.0149(19) N1 0.024(2) 0.022(2) 0.027(2) 0.0046(18) -0.0008(18) 0.0085(19) N2 0.023(2) 0.017(2) 0.029(2) 0.0005(18) -0.0032(19) 0.0011(18) N3 0.025(2) 0.016(2) 0.024(2) 0.0004(16) -0.0015(17) 0.0068(18) N4 0.023(2) 0.014(2) 0.026(2) -0.0001(16) 0.0008(18) 0.0055(18) N5 0.023(2) 0.019(2) 0.038(3) 0.0032(19) 0.003(2) 0.0103(19) N6 0.027(2) 0.023(2) 0.028(2) 0.0009(18) 0.0063(19) 0.011(2) C1 0.053(5) 0.041(4) 0.054(4) -0.002(3) 0.018(4) 0.024(4) C2 0.058(5) 0.027(3) 0.051(4) 0.007(3) -0.003(4) 0.016(3) C3 0.048(4) 0.043(4) 0.043(4) 0.000(3) -0.004(3) 0.018(3) C4 0.035(3) 0.033(3) 0.043(4) 0.004(3) 0.007(3) 0.015(3) C5 0.029(3) 0.030(3) 0.028(3) 0.003(2) -0.006(2) 0.012(3) C6 0.025(3) 0.028(3) 0.029(3) -0.001(2) -0.004(2) -0.002(2) C7 0.025(3) 0.031(3) 0.026(3) -0.002(2) -0.004(2) 0.002(3) C8 0.046(4) 0.027(3) 0.034(3) -0.004(3) 0.009(3) -0.004(3) C9 0.025(3) 0.016(2) 0.023(2) 0.0019(19) -0.004(2) 0.004(2) C10 0.023(3) 0.014(2) 0.036(3) -0.002(2) -0.006(2) -0.001(2) C11 0.041(3) 0.013(2) 0.031(3) -0.003(2) -0.002(3) 0.007(2) C12 0.038(3) 0.019(3) 0.026(3) -0.002(2) -0.005(2) 0.008(2) C13 0.024(3) 0.018(2) 0.019(2) 0.0045(18) -0.0034(19) 0.007(2) C14 0.047(4) 0.018(3) 0.034(3) -0.002(2) -0.002(3) 0.014(3) C15 0.042(4) 0.031(3) 0.040(3) 0.001(3) 0.008(3) 0.022(3) C16 0.026(3) 0.022(3) 0.029(3) 0.005(2) 0.001(2) 0.011(2) C17 0.034(4) 0.032(3) 0.090(6) 0.000(4) -0.002(4) 0.021(3) C18 0.025(3) 0.033(3) 0.037(3) 0.012(3) 0.006(2) 0.013(3) C19 0.019(3) 0.027(3) 0.040(3) 0.008(2) 0.003(2) 0.005(2) C20 0.023(3) 0.023(3) 0.025(3) 0.002(2) 0.000(2) 0.003(2) C21 0.033(3) 0.031(3) 0.042(3) -0.009(3) 0.002(3) 0.005(3) Ni3 0.0338(4) 0.0251(4) 0.0251(3) -0.0040(3) -0.0063(3) 0.0186(3) Cl4 0.0379(7) 0.0329(7) 0.0257(6) -0.0067(5) -0.0077(5) 0.0236(6) Cl5 0.0371(8) 0.0521(9) 0.0367(8) 0.0038(7) 0.0006(6) 0.0273(8) O4 0.045(3) 0.040(3) 0.038(2) -0.0086(19) -0.013(2) 0.030(2) N7 0.039(3) 0.020(2) 0.028(2) -0.0003(18) -0.002(2) 0.015(2) N8 0.037(3) 0.023(2) 0.024(2) -0.0015(18) -0.002(2) 0.016(2) N9 0.036(3) 0.025(2) 0.023(2) -0.0004(18) -0.001(2) 0.019(2) C22 0.068(5) 0.066(5) 0.048(4) -0.008(4) -0.006(4) 0.050(5) C23 0.047(4) 0.036(3) 0.041(3) -0.003(3) -0.014(3) 0.027(3) C24 0.034(3) 0.033(3) 0.023(3) -0.003(2) -0.007(2) 0.019(3) C25 0.034(3) 0.032(3) 0.030(3) -0.002(2) -0.003(2) 0.015(3) C26 0.036(3) 0.026(3) 0.025(3) 0.001(2) 0.003(2) 0.016(3) C27 0.030(3) 0.022(3) 0.052(4) -0.005(3) 0.006(3) 0.011(2) C28 0.028(3) 0.030(3) 0.022(3) 0.000(2) 0.001(2) 0.015(2) C29 0.036(3) 0.021(3) 0.040(3) -0.003(2) -0.002(3) 0.014(3) C30 0.041(3) 0.027(3) 0.035(3) -0.003(2) -0.003(3) 0.020(3) C31 0.029(4) 0.024(3) 0.029(4) 0.0012(16) 0.002(3) 0.014(2) C32 0.024(4) 0.018(2) 0.024(3) -0.0003(14) -0.001(3) 0.0122(19) Cl6 0.0323(8) 0.0177(9) 0.0558(13) -0.0025(9) -0.0013(4) 0.0089(4) Cl7 0.079(2) 0.0427(9) 0.0600(16) -0.0141(7) -0.0282(15) 0.0397(10) C33 0.159(17) 0.21(2) 0.110(11) -0.024(12) 0.001(11) 0.139(17) Cl8 0.086(2) 0.108(3) 0.121(3) -0.016(2) -0.0174(19) 0.059(2) Cl9 0.101(3) 0.115(3) 0.116(3) 0.021(2) -0.027(2) 0.060(2) _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 O1 2.041(4) . ? Ni1 N1 2.065(5) . ? Ni1 N3 2.122(5) . ? Ni1 Cl1 2.3583(15) . ? Ni1 Cl2 2.4170(14) . ? Ni1 Cl3 2.4222(15) . ? Ni2 N6 2.024(5) . ? Ni2 O2 2.052(4) . ? Ni2 N4 2.130(4) . ? Ni2 O3 2.157(4) . ? Ni2 Cl2 2.3493(14) . ? Ni2 Cl3 2.3659(15) . ? O1 C1 1.469(9) . ? O2 C2 1.413(8) . ? O3 C3 1.405(9) . ? N1 C5 1.330(8) . ? N1 N2 1.373(7) . ? N2 C7 1.388(7) . ? N2 C9 1.392(8) . ? N3 C9 1.350(7) . ? N3 C13 1.365(7) . ? N4 C16 1.318(7) . ? N4 C13 1.371(7) . ? N5 N6 1.365(7) . ? N5 C18 1.389(8) . ? N5 C16 1.412(7) . ? N6 C20 1.350(7) . ? C4 C5 1.482(9) . ? C5 C6 1.397(8) . ? C6 C7 1.370(10) . ? C7 C8 1.489(10) . ? C9 C10 1.395(8) . ? C10 C11 1.374(9) . ? C11 C12 1.411(8) . ? C12 C14 1.385(10) . ? C12 C13 1.400(8) . ? C14 C15 1.336(10) . ? C15 C16 1.397(8) . ? C17 C18 1.501(9) . ? C18 C19 1.338(9) . ? C19 C20 1.395(9) . ? C20 C21 1.471(9) . ? Ni3 N7 2.054(5) . ? Ni3 O4 2.077(5) . ? Ni3 N9 2.117(5) . ? Ni3 Cl4 2.3804(17) 6_765 ? Ni3 Cl4 2.3866(16) . ? Ni3 Cl5 2.4071(18) . ? Cl4 Ni3 2.3804(17) 6_765 ? O4 C22 1.431(9) . ? N7 C24 1.304(8) . ? N7 N8 1.371(7) . ? N8 C26 1.383(8) . ? N8 C28 1.402(8) . ? N9 C28 1.324(8) . ? N9 C32 1.360(6) . ? C23 C24 1.487(8) . ? C24 C25 1.417(9) . ? C25 C26 1.343(9) . ? C26 C27 1.488(8) . ? C28 C29 1.398(8) . ? C29 C30 1.347(9) . ? C30 C31 1.405(7) . ? C31 C30 1.405(7) 6_765 ? C31 C32 1.444(11) . ? C32 N9 1.360(6) 6_765 ? C33 Cl8 1.702(17) . ? C33 Cl9 1.95(2) . ? O5 C34 1.225(15) . ? O6 C35 1.250(14) . ? 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 Ni1 N1 92.78(19) . . ? O1 Ni1 N3 168.62(19) . . ? N1 Ni1 N3 77.61(19) . . ? O1 Ni1 Cl1 95.85(13) . . ? N1 Ni1 Cl1 87.61(14) . . ? N3 Ni1 Cl1 89.89(13) . . ? O1 Ni1 Cl2 89.00(13) . . ? N1 Ni1 Cl2 178.19(15) . . ? N3 Ni1 Cl2 100.65(14) . . ? Cl1 Ni1 Cl2 91.90(5) . . ? O1 Ni1 Cl3 88.60(13) . . ? N1 Ni1 Cl3 93.10(14) . . ? N3 Ni1 Cl3 85.88(13) . . ? Cl1 Ni1 Cl3 175.46(6) . . ? Cl2 Ni1 Cl3 87.25(5) . . ? N6 Ni2 O2 94.84(18) . . ? N6 Ni2 N4 77.70(18) . . ? O2 Ni2 N4 170.30(18) . . ? N6 Ni2 O3 83.59(18) . . ? O2 Ni2 O3 95.49(16) . . ? N4 Ni2 O3 89.88(17) . . ? N6 Ni2 Cl2 96.82(14) . . ? O2 Ni2 Cl2 87.84(12) . . ? N4 Ni2 Cl2 86.92(13) . . ? O3 Ni2 Cl2 176.60(12) . . ? N6 Ni2 Cl3 172.73(14) . . ? O2 Ni2 Cl3 87.41(13) . . ? N4 Ni2 Cl3 100.75(13) . . ? O3 Ni2 Cl3 89.32(13) . . ? Cl2 Ni2 Cl3 90.16(5) . . ? Ni2 Cl2 Ni1 85.20(5) . . ? Ni2 Cl3 Ni1 84.73(5) . . ? C1 O1 Ni1 123.6(4) . . ? C2 O2 Ni2 125.0(4) . . ? C3 O3 Ni2 132.2(4) . . ? C5 N1 N2 105.8(5) . . ? C5 N1 Ni1 136.0(4) . . ? N2 N1 Ni1 108.2(4) . . ? N1 N2 C7 110.9(5) . . ? N1 N2 C9 117.2(5) . . ? C7 N2 C9 131.8(5) . . ? C9 N3 C13 118.0(5) . . ? C9 N3 Ni1 110.7(4) . . ? C13 N3 Ni1 130.8(4) . . ? C16 N4 C13 117.0(5) . . ? C16 N4 Ni2 112.7(4) . . ? C13 N4 Ni2 129.3(4) . . ? N6 N5 C18 110.0(5) . . ? N6 N5 C16 117.4(5) . . ? C18 N5 C16 132.2(5) . . ? C20 N6 N5 106.4(5) . . ? C20 N6 Ni2 139.6(4) . . ? N5 N6 Ni2 114.0(4) . . ? N1 C5 C6 110.4(6) . . ? N1 C5 C4 123.1(6) . . ? C6 C5 C4 126.4(6) . . ? C7 C6 C5 107.5(6) . . ? C6 C7 N2 105.2(5) . . ? C6 C7 C8 128.5(6) . . ? N2 C7 C8 126.3(6) . . ? N3 C9 N2 115.7(5) . . ? N3 C9 C10 122.9(5) . . ? N2 C9 C10 121.2(5) . . ? C11 C10 C9 119.1(5) . . ? C10 C11 C12 119.1(5) . . ? C14 C12 C13 117.8(5) . . ? C14 C12 C11 123.5(6) . . ? C13 C12 C11 118.6(6) . . ? N3 C13 N4 116.8(5) . . ? N3 C13 C12 121.7(5) . . ? N4 C13 C12 121.4(5) . . ? C15 C14 C12 120.8(6) . . ? C14 C15 C16 118.2(6) . . ? N4 C16 C15 123.8(6) . . ? N4 C16 N5 115.3(5) . . ? C15 C16 N5 120.8(6) . . ? C19 C18 N5 106.3(6) . . ? C19 C18 C17 128.0(6) . . ? N5 C18 C17 125.7(6) . . ? C18 C19 C20 108.7(5) . . ? N6 C20 C19 108.6(5) . . ? N6 C20 C21 122.8(6) . . ? C19 C20 C21 128.6(6) . . ? N7 Ni3 O4 95.13(18) . . ? N7 Ni3 N9 76.89(19) . . ? O4 Ni3 N9 170.57(18) . . ? N7 Ni3 Cl4 95.10(15) . 6_765 ? O4 Ni3 Cl4 87.61(15) . 6_765 ? N9 Ni3 Cl4 88.10(14) . 6_765 ? N7 Ni3 Cl4 175.75(14) . . ? O4 Ni3 Cl4 87.53(13) . . ? N9 Ni3 Cl4 100.74(14) . . ? Cl4 Ni3 Cl4 88.31(6) 6_765 . ? N7 Ni3 Cl5 86.30(15) . . ? O4 Ni3 Cl5 95.69(15) . . ? N9 Ni3 Cl5 88.88(14) . . ? Cl4 Ni3 Cl5 176.30(6) 6_765 . ? Cl4 Ni3 Cl5 90.15(6) . . ? Ni3 Cl4 Ni3 85.04(5) 6_765 . ? C22 O4 Ni3 123.8(5) . . ? C24 N7 N8 106.2(5) . . ? C24 N7 Ni3 136.0(4) . . ? N8 N7 Ni3 109.6(4) . . ? N7 N8 C26 110.2(5) . . ? N7 N8 C28 117.2(5) . . ? C26 N8 C28 132.6(5) . . ? C28 N9 C32 117.5(5) . . ? C28 N9 Ni3 112.7(4) . . ? C32 N9 Ni3 129.4(4) . . ? N7 C24 C25 110.5(5) . . ? N7 C24 C23 123.5(6) . . ? C25 C24 C23 126.0(6) . . ? C26 C25 C24 106.6(6) . . ? C25 C26 N8 106.5(5) . . ? C25 C26 C27 126.8(6) . . ? N8 C26 C27 126.6(6) . . ? N9 C28 C29 125.2(6) . . ? N9 C28 N8 114.7(5) . . ? C29 C28 N8 120.1(5) . . ? C30 C29 C28 118.5(6) . . ? C29 C30 C31 119.3(6) . . ? C30 C31 C30 122.9(8) . 6_765 ? C30 C31 C32 118.6(4) . . ? C30 C31 C32 118.6(4) 6_765 . ? N9 C32 N9 119.5(7) . 6_765 ? N9 C32 C31 120.3(3) . . ? N9 C32 C31 120.3(3) 6_765 . ? Cl8 C33 Cl9 106.0(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.727 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.128