# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1945 data_ifn52 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H33 Br3 Cu2 N4 O' _chemical_formula_weight 700.30 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.282(3) _cell_length_b 11.3423(19) _cell_length_c 28.242(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4895.4(14) _cell_formula_units_Z 8 _cell_measurement_temperature 423(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 6.653 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4352 _exptl_absorpt_correction_T_max 0.5559 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30453 _diffrn_reflns_av_R_equivalents 0.3510 _diffrn_reflns_av_sigmaI/netI 0.1653 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 28.33 _reflns_number_total 5961 _reflns_number_gt 3871 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0741P)^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 5961 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1770 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.02133(5) 0.23994(8) 0.36343(3) 0.0228(2) Uani 1 1 d . . . Cu2 Cu 0.03382(5) -0.03231(8) 0.37603(3) 0.0237(2) Uani 1 1 d . . . Br1 Br 0.07912(5) 0.27292(8) 0.42896(2) 0.0337(2) Uani 1 1 d . . . Br2 Br 0.08327(4) 0.09864(7) 0.31272(2) 0.0294(2) Uani 1 1 d . . . Br3 Br -0.06155(5) -0.18490(7) 0.32895(3) 0.0330(2) Uani 1 1 d . . . O1 O -0.0559(3) 0.0874(5) 0.39013(15) 0.0244(10) Uani 1 1 d . . . N1 N -0.1432(4) 0.2445(6) 0.3332(2) 0.0296(14) Uani 1 1 d . . . N2 N 0.0013(4) 0.3961(6) 0.3300(2) 0.0277(13) Uani 1 1 d . . . N3 N 0.1489(4) -0.1255(6) 0.3809(2) 0.0303(14) Uani 1 1 d . . . N4 N 0.0115(4) -0.1016(6) 0.4389(2) 0.0280(13) Uani 1 1 d . . . C1 C -0.1320(4) 0.0648(7) 0.4128(2) 0.0235(14) Uani 1 1 d . . . C2 C -0.1378(4) -0.0293(7) 0.4450(2) 0.0257(15) Uani 1 1 d . . . C3 C -0.2186(5) -0.0536(8) 0.4679(2) 0.0332(17) Uani 1 1 d . . . H3 H -0.2215 -0.1149 0.4897 0.040 Uiso 1 1 calc R . . C4 C -0.2924(5) 0.0113(7) 0.4585(2) 0.0303(16) Uani 1 1 d . . . C5 C -0.2852(5) 0.1037(7) 0.4268(3) 0.0319(17) Uani 1 1 d . . . H5 H -0.3346 0.1491 0.4206 0.038 Uiso 1 1 calc R . . C6 C -0.2069(4) 0.1319(7) 0.4035(2) 0.0250(15) Uani 1 1 d . . . C7 C -0.2071(4) 0.2399(7) 0.3735(2) 0.0291(17) Uani 1 1 d . . . H7A H -0.1960 0.3071 0.3939 0.035 Uiso 1 1 calc R . . H7B H -0.2655 0.2495 0.3606 0.035 Uiso 1 1 calc R . . C8 C -0.1510(5) 0.3595(9) 0.3084(3) 0.040(2) Uani 1 1 d . . . H8A H -0.1739 0.4184 0.3299 0.048 Uiso 1 1 calc R . . H8B H -0.1913 0.3521 0.2820 0.048 Uiso 1 1 calc R . . C9 C -0.0631(5) 0.3975(9) 0.2905(3) 0.042(2) Uani 1 1 d . . . H9A H -0.0439 0.3447 0.2656 0.051 Uiso 1 1 calc R . . H9B H -0.0670 0.4764 0.2774 0.051 Uiso 1 1 calc R . . C10 C 0.1304(6) -0.2218(8) 0.4151(3) 0.041(2) Uani 1 1 d . . . H10A H 0.1850 -0.2571 0.4254 0.049 Uiso 1 1 calc R . . H10B H 0.0958 -0.2824 0.3997 0.049 Uiso 1 1 calc R . . C11 C 0.0814(5) -0.1752(8) 0.4577(3) 0.0384(19) Uani 1 1 d . . . H11A H 0.0574 -0.2397 0.4761 0.046 Uiso 1 1 calc R . . H11B H 0.1200 -0.1293 0.4777 0.046 Uiso 1 1 calc R . . C12 C -0.0643(5) -0.1005(7) 0.4596(2) 0.0300(16) Uani 1 1 d . . . H12 H -0.0718 -0.1491 0.4858 0.036 Uiso 1 1 calc R . . C13 C 0.0890(5) 0.4090(9) 0.3109(3) 0.042(2) Uani 1 1 d . . . H13A H 0.0931 0.4822 0.2940 0.064 Uiso 1 1 calc R . . H13B H 0.1012 0.3448 0.2898 0.064 Uiso 1 1 calc R . . H13C H 0.1306 0.4085 0.3364 0.064 Uiso 1 1 calc R . . C14 C -0.0169(6) 0.4953(8) 0.3628(3) 0.046(2) Uani 1 1 d . . . H14A H 0.0304 0.5027 0.3850 0.068 Uiso 1 1 calc R . . H14B H -0.0704 0.4803 0.3796 0.068 Uiso 1 1 calc R . . H14C H -0.0224 0.5671 0.3451 0.068 Uiso 1 1 calc R . . C15 C 0.2155(5) -0.0433(8) 0.4010(3) 0.0379(19) Uani 1 1 d . . . H15A H 0.2660 -0.0873 0.4109 0.057 Uiso 1 1 calc R . . H15B H 0.1910 -0.0029 0.4278 0.057 Uiso 1 1 calc R . . H15C H 0.2322 0.0132 0.3774 0.057 Uiso 1 1 calc R . . C16 C 0.1809(5) -0.1765(7) 0.3360(3) 0.0349(18) Uani 1 1 d . . . H16A H 0.1929 -0.1142 0.3139 0.052 Uiso 1 1 calc R . . H16B H 0.1370 -0.2278 0.3231 0.052 Uiso 1 1 calc R . . H16C H 0.2334 -0.2205 0.3418 0.052 Uiso 1 1 calc R . . C17 C -0.1548(5) 0.1413(8) 0.3000(2) 0.0328(18) Uani 1 1 d . . . H17A H -0.1443 0.0694 0.3177 0.039 Uiso 1 1 calc R . . H17B H -0.1103 0.1464 0.2757 0.039 Uiso 1 1 calc R . . C18 C -0.2433(5) 0.1311(9) 0.2761(3) 0.044(2) Uani 1 1 d . . . H18A H -0.2876 0.1178 0.2995 0.065 Uiso 1 1 calc R . . H18B H -0.2424 0.0663 0.2542 0.065 Uiso 1 1 calc R . . H18C H -0.2558 0.2027 0.2593 0.065 Uiso 1 1 calc R . . C19 C -0.3780(5) -0.0169(9) 0.4833(3) 0.047(2) Uani 1 1 d . . . H19A H -0.4182 0.0472 0.4789 0.071 Uiso 1 1 calc R . . H19B H -0.3674 -0.0283 0.5165 0.071 Uiso 1 1 calc R . . H19C H -0.4025 -0.0876 0.4700 0.071 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 Cu1 0.0226(4) 0.0241(5) 0.0216(4) 0.0036(3) -0.0006(3) -0.0012(3) Cu2 0.0214(4) 0.0262(5) 0.0236(4) 0.0018(3) 0.0007(3) 0.0019(3) Br1 0.0362(4) 0.0405(5) 0.0243(3) 0.0040(3) -0.0062(3) -0.0095(3) Br2 0.0292(4) 0.0333(5) 0.0258(3) 0.0005(3) 0.0068(3) -0.0005(3) Br3 0.0306(4) 0.0326(5) 0.0358(4) -0.0041(3) -0.0008(3) -0.0066(3) O1 0.020(2) 0.030(3) 0.024(2) 0.004(2) 0.0040(18) 0.003(2) N1 0.031(3) 0.027(4) 0.030(3) 0.002(3) -0.001(3) 0.002(3) N2 0.028(3) 0.028(4) 0.028(3) 0.006(3) -0.003(2) -0.004(3) N3 0.025(3) 0.035(4) 0.031(3) 0.000(3) -0.002(2) 0.009(3) N4 0.032(3) 0.030(4) 0.022(3) 0.006(2) -0.003(2) 0.000(3) C1 0.021(3) 0.028(4) 0.021(3) -0.004(3) 0.008(3) -0.001(3) C2 0.030(3) 0.027(4) 0.020(3) -0.004(3) 0.001(3) -0.003(3) C3 0.037(4) 0.040(5) 0.023(3) -0.002(3) 0.007(3) -0.003(3) C4 0.031(4) 0.036(5) 0.024(3) -0.005(3) 0.007(3) -0.007(3) C5 0.026(3) 0.036(5) 0.033(4) -0.014(3) 0.009(3) -0.005(3) C6 0.023(3) 0.029(4) 0.023(3) -0.001(3) 0.002(3) -0.003(3) C7 0.020(3) 0.035(5) 0.032(3) -0.006(3) 0.002(3) 0.002(3) C8 0.035(4) 0.045(6) 0.041(4) 0.011(4) -0.009(3) -0.003(4) C9 0.045(4) 0.043(6) 0.039(4) 0.019(4) -0.005(4) -0.004(4) C10 0.040(4) 0.038(5) 0.045(4) 0.003(4) -0.010(4) 0.011(4) C11 0.039(4) 0.036(5) 0.040(4) 0.012(4) -0.002(3) 0.007(4) C12 0.040(4) 0.030(4) 0.019(3) 0.007(3) 0.001(3) 0.005(3) C13 0.036(4) 0.043(6) 0.048(5) 0.020(4) -0.001(4) -0.005(4) C14 0.058(5) 0.029(5) 0.049(5) -0.001(4) -0.004(4) 0.002(4) C15 0.024(3) 0.046(6) 0.044(4) -0.008(4) -0.005(3) 0.006(3) C16 0.034(4) 0.029(5) 0.042(4) -0.007(3) 0.001(3) 0.003(3) C17 0.026(3) 0.046(5) 0.026(3) -0.013(3) -0.005(3) -0.001(3) C18 0.039(4) 0.053(6) 0.039(4) 0.003(4) -0.017(4) -0.011(4) C19 0.030(4) 0.060(7) 0.051(5) -0.006(5) 0.014(4) -0.008(4) _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 Cu1 O1 1.960(5) . ? Cu1 N2 2.036(6) . ? Cu1 N1 2.049(6) . ? Cu1 Br1 2.4334(11) . ? Cu1 Br2 2.6786(11) . ? Cu2 O1 1.971(5) . ? Cu2 N4 1.972(6) . ? Cu2 N3 2.057(6) . ? Cu2 Br2 2.4441(11) . ? Cu2 Br3 2.6245(12) . ? O1 C1 1.352(7) . ? N1 C8 1.486(11) . ? N1 C7 1.501(9) . ? N1 C17 1.509(10) . ? N2 C13 1.453(9) . ? N2 C14 1.484(11) . ? N2 C9 1.488(10) . ? N3 C16 1.476(9) . ? N3 C10 1.485(10) . ? N3 C15 1.493(10) . ? N4 C12 1.297(9) . ? N4 C11 1.456(9) . ? C1 C6 1.399(9) . ? C1 C2 1.405(10) . ? C2 C3 1.419(9) . ? C2 C12 1.444(10) . ? C3 C4 1.373(11) . ? C4 C5 1.384(11) . ? C4 C19 1.516(10) . ? C5 C6 1.403(9) . ? C6 C7 1.489(10) . ? C8 C9 1.499(11) . ? C10 C11 1.512(12) . ? C17 C18 1.517(10) . ? 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 Cu1 N2 172.7(2) . . ? O1 Cu1 N1 86.4(2) . . ? N2 Cu1 N1 86.5(2) . . ? O1 Cu1 Br1 90.75(14) . . ? N2 Cu1 Br1 96.40(16) . . ? N1 Cu1 Br1 152.39(18) . . ? O1 Cu1 Br2 80.70(14) . . ? N2 Cu1 Br2 99.88(18) . . ? N1 Cu1 Br2 109.57(18) . . ? Br1 Cu1 Br2 97.01(4) . . ? O1 Cu2 N4 88.4(2) . . ? O1 Cu2 N3 159.4(2) . . ? N4 Cu2 N3 83.3(2) . . ? O1 Cu2 Br2 86.80(14) . . ? N4 Cu2 Br2 162.66(19) . . ? N3 Cu2 Br2 95.56(18) . . ? O1 Cu2 Br3 99.82(15) . . ? N4 Cu2 Br3 95.58(18) . . ? N3 Cu2 Br3 99.77(19) . . ? Br2 Cu2 Br3 101.65(4) . . ? Cu2 Br2 Cu1 77.76(3) . . ? C1 O1 Cu1 125.6(4) . . ? C1 O1 Cu2 124.3(5) . . ? Cu1 O1 Cu2 110.1(2) . . ? C8 N1 C7 109.7(6) . . ? C8 N1 C17 112.2(6) . . ? C7 N1 C17 111.6(6) . . ? C8 N1 Cu1 106.9(4) . . ? C7 N1 Cu1 105.9(4) . . ? C17 N1 Cu1 110.2(4) . . ? C13 N2 C14 109.1(7) . . ? C13 N2 C9 109.3(6) . . ? C14 N2 C9 109.6(7) . . ? C13 N2 Cu1 114.6(5) . . ? C14 N2 Cu1 109.8(5) . . ? C9 N2 Cu1 104.2(5) . . ? C16 N3 C10 109.5(6) . . ? C16 N3 C15 110.3(6) . . ? C10 N3 C15 109.9(6) . . ? C16 N3 Cu2 115.3(4) . . ? C10 N3 Cu2 105.0(4) . . ? C15 N3 Cu2 106.7(5) . . ? C12 N4 C11 119.8(6) . . ? C12 N4 Cu2 123.8(5) . . ? C11 N4 Cu2 115.4(5) . . ? O1 C1 C6 120.8(6) . . ? O1 C1 C2 120.4(6) . . ? C6 C1 C2 118.8(6) . . ? C1 C2 C3 119.8(7) . . ? C1 C2 C12 124.1(6) . . ? C3 C2 C12 115.9(7) . . ? C4 C3 C2 121.5(7) . . ? C3 C4 C5 117.7(6) . . ? C3 C4 C19 120.5(7) . . ? C5 C4 C19 121.8(7) . . ? C4 C5 C6 122.9(7) . . ? C1 C6 C5 119.1(7) . . ? C1 C6 C7 123.8(6) . . ? C5 C6 C7 116.8(6) . . ? C6 C7 N1 117.3(6) . . ? N1 C8 C9 109.9(7) . . ? N2 C9 C8 109.7(6) . . ? N3 C10 C11 110.8(7) . . ? N4 C11 C10 106.0(6) . . ? N4 C12 C2 124.8(6) . . ? N1 C17 C18 116.2(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu2 Br2 Cu1 13.81(14) . . . . ? N4 Cu2 Br2 Cu1 -60.3(6) . . . . ? N3 Cu2 Br2 Cu1 -145.63(18) . . . . ? Br3 Cu2 Br2 Cu1 113.18(4) . . . . ? O1 Cu1 Br2 Cu2 -14.06(14) . . . . ? N2 Cu1 Br2 Cu2 173.34(16) . . . . ? N1 Cu1 Br2 Cu2 -96.84(19) . . . . ? Br1 Cu1 Br2 Cu2 75.56(4) . . . . ? N2 Cu1 O1 C1 -63.3(19) . . . . ? N1 Cu1 O1 C1 -48.0(5) . . . . ? Br1 Cu1 O1 C1 104.5(5) . . . . ? Br2 Cu1 O1 C1 -158.5(5) . . . . ? N2 Cu1 O1 Cu2 113.5(17) . . . . ? N1 Cu1 O1 Cu2 128.8(3) . . . . ? Br1 Cu1 O1 Cu2 -78.7(2) . . . . ? Br2 Cu1 O1 Cu2 18.26(18) . . . . ? N4 Cu2 O1 C1 -39.7(5) . . . . ? N3 Cu2 O1 C1 -105.7(8) . . . . ? Br2 Cu2 O1 C1 157.0(5) . . . . ? Br3 Cu2 O1 C1 55.7(5) . . . . ? N4 Cu2 O1 Cu1 143.5(3) . . . . ? N3 Cu2 O1 Cu1 77.4(7) . . . . ? Br2 Cu2 O1 Cu1 -19.84(19) . . . . ? Br3 Cu2 O1 Cu1 -121.12(19) . . . . ? O1 Cu1 N1 C8 176.9(5) . . . . ? N2 Cu1 N1 C8 -5.1(5) . . . . ? Br1 Cu1 N1 C8 92.1(6) . . . . ? Br2 Cu1 N1 C8 -104.3(5) . . . . ? O1 Cu1 N1 C7 59.9(5) . . . . ? N2 Cu1 N1 C7 -122.0(5) . . . . ? Br1 Cu1 N1 C7 -24.8(7) . . . . ? Br2 Cu1 N1 C7 138.7(4) . . . . ? O1 Cu1 N1 C17 -60.9(5) . . . . ? N2 Cu1 N1 C17 117.2(5) . . . . ? Br1 Cu1 N1 C17 -145.6(4) . . . . ? Br2 Cu1 N1 C17 17.9(5) . . . . ? O1 Cu1 N2 C13 -125.8(17) . . . . ? N1 Cu1 N2 C13 -141.2(6) . . . . ? Br1 Cu1 N2 C13 66.4(5) . . . . ? Br2 Cu1 N2 C13 -31.9(5) . . . . ? O1 Cu1 N2 C14 110.9(18) . . . . ? N1 Cu1 N2 C14 95.6(5) . . . . ? Br1 Cu1 N2 C14 -56.9(5) . . . . ? Br2 Cu1 N2 C14 -155.2(5) . . . . ? O1 Cu1 N2 C9 -6(2) . . . . ? N1 Cu1 N2 C9 -21.8(5) . . . . ? Br1 Cu1 N2 C9 -174.2(5) . . . . ? Br2 Cu1 N2 C9 87.5(5) . . . . ? O1 Cu2 N3 C16 -149.3(6) . . . . ? N4 Cu2 N3 C16 143.8(6) . . . . ? Br2 Cu2 N3 C16 -53.6(5) . . . . ? Br3 Cu2 N3 C16 49.3(6) . . . . ? O1 Cu2 N3 C10 90.1(8) . . . . ? N4 Cu2 N3 C10 23.2(5) . . . . ? Br2 Cu2 N3 C10 -174.2(4) . . . . ? Br3 Cu2 N3 C10 -71.3(5) . . . . ? O1 Cu2 N3 C15 -26.5(9) . . . . ? N4 Cu2 N3 C15 -93.4(5) . . . . ? Br2 Cu2 N3 C15 69.2(5) . . . . ? Br3 Cu2 N3 C15 172.0(4) . . . . ? O1 Cu2 N4 C12 32.1(6) . . . . ? N3 Cu2 N4 C12 -166.8(7) . . . . ? Br2 Cu2 N4 C12 106.0(7) . . . . ? Br3 Cu2 N4 C12 -67.6(6) . . . . ? O1 Cu2 N4 C11 -159.3(6) . . . . ? N3 Cu2 N4 C11 1.8(6) . . . . ? Br2 Cu2 N4 C11 -85.4(8) . . . . ? Br3 Cu2 N4 C11 101.0(5) . . . . ? Cu1 O1 C1 C6 25.9(9) . . . . ? Cu2 O1 C1 C6 -150.5(5) . . . . ? Cu1 O1 C1 C2 -156.4(5) . . . . ? Cu2 O1 C1 C2 27.3(8) . . . . ? O1 C1 C2 C3 -178.7(6) . . . . ? C6 C1 C2 C3 -0.9(10) . . . . ? O1 C1 C2 C12 6.0(10) . . . . ? C6 C1 C2 C12 -176.2(7) . . . . ? C1 C2 C3 C4 1.5(11) . . . . ? C12 C2 C3 C4 177.2(7) . . . . ? C2 C3 C4 C5 -1.5(11) . . . . ? C2 C3 C4 C19 179.7(7) . . . . ? C3 C4 C5 C6 1.0(11) . . . . ? C19 C4 C5 C6 179.8(7) . . . . ? O1 C1 C6 C5 178.2(6) . . . . ? C2 C1 C6 C5 0.4(10) . . . . ? O1 C1 C6 C7 -7.8(10) . . . . ? C2 C1 C6 C7 174.4(6) . . . . ? C4 C5 C6 C1 -0.5(11) . . . . ? C4 C5 C6 C7 -174.9(6) . . . . ? C1 C6 C7 N1 32.1(9) . . . . ? C5 C6 C7 N1 -153.8(6) . . . . ? C8 N1 C7 C6 -178.3(6) . . . . ? C17 N1 C7 C6 56.8(8) . . . . ? Cu1 N1 C7 C6 -63.2(7) . . . . ? C7 N1 C8 C9 146.0(7) . . . . ? C17 N1 C8 C9 -89.4(8) . . . . ? Cu1 N1 C8 C9 31.5(8) . . . . ? C13 N2 C9 C8 168.3(8) . . . . ? C14 N2 C9 C8 -72.1(9) . . . . ? Cu1 N2 C9 C8 45.4(8) . . . . ? N1 C8 C9 N2 -53.1(10) . . . . ? C16 N3 C10 C11 -169.0(6) . . . . ? C15 N3 C10 C11 69.7(8) . . . . ? Cu2 N3 C10 C11 -44.7(7) . . . . ? C12 N4 C11 C10 143.1(7) . . . . ? Cu2 N4 C11 C10 -26.0(8) . . . . ? N3 C10 C11 N4 46.7(9) . . . . ? C11 N4 C12 C2 178.5(7) . . . . ? Cu2 N4 C12 C2 -13.3(11) . . . . ? C1 C2 C12 N4 -13.5(12) . . . . ? C3 C2 C12 N4 171.0(7) . . . . ? C8 N1 C17 C18 -62.7(8) . . . . ? C7 N1 C17 C18 60.9(9) . . . . ? Cu1 N1 C17 C18 178.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.087 _refine_diff_density_min -2.235 _refine_diff_density_rms 0.407 data_ifn76s _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H36 Cl2 Cu2 N4 O10' _chemical_formula_weight 690.51 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.138(3) _cell_length_b 12.800(4) _cell_length_c 18.132(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.870(10) _cell_angle_gamma 90.00 _cell_volume 2902.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4277 _exptl_absorpt_correction_T_max 0.5487 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6404 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5118 _reflns_number_gt 3456 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1116P)^2^+3.1782P] 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 5118 _refine_ls_number_parameters 399 _refine_ls_number_restraints 104 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.1988 _refine_ls_wR_factor_gt 0.1724 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.72762(6) 0.96798(6) 0.12430(5) 0.0472(3) Uani 1 1 d . . . Cu2 Cu 0.79390(6) 0.75337(6) 0.09902(5) 0.0490(3) Uani 1 1 d . . . Cl1 Cl 0.3757(2) 0.72018(18) 0.08844(15) 0.0808(6) Uani 1 1 d D . . Cl2 Cl 0.8913(2) 0.86050(15) 0.29937(11) 0.0767(6) Uani 1 1 d D . . O1 O 0.8377(4) 0.8989(3) 0.0878(2) 0.0487(10) Uani 1 1 d . . . O2 O 0.6686(4) 0.8309(3) 0.1025(3) 0.0628(13) Uani 1 1 d . . . H2 H 0.5992 0.8078 0.0955 0.094 Uiso 1 1 calc R . . O3A O 0.3600(19) 0.8195(8) 0.0534(10) 0.127(7) Uani 0.470(12) 1 d PDU A 1 O3B O 0.4414(11) 0.7858(14) 0.0604(10) 0.127(6) Uani 0.530(12) 1 d PDU A 2 O4A O 0.4745(8) 0.7250(18) 0.1474(8) 0.130(7) Uani 0.470(12) 1 d PDU A 1 O4B O 0.4263(14) 0.6243(9) 0.1146(12) 0.139(7) Uani 0.530(12) 1 d PDU A 2 O5A O 0.2866(11) 0.694(2) 0.1121(15) 0.158(10) Uani 0.470(12) 1 d PDU A 1 O5B O 0.3568(17) 0.7740(12) 0.1507(7) 0.130(6) Uani 0.530(12) 1 d PDU A 2 O6A O 0.3802(18) 0.6644(14) 0.0226(8) 0.151(9) Uani 0.470(12) 1 d PDU A 1 O6B O 0.2740(8) 0.7031(15) 0.0348(9) 0.143(7) Uani 0.530(12) 1 d PDU A 2 O7 O 0.8457(5) 0.9541(4) 0.2637(3) 0.091(2) Uani 1 1 d D B . O8 O 0.8709(6) 0.7771(4) 0.2475(3) 0.093(2) Uani 1 1 d . B . O9A O 0.9887(8) 0.8587(12) 0.3601(7) 0.113(3) Uani 0.544(8) 1 d PDU B 1 O9B O 0.9946(7) 0.8780(12) 0.2935(9) 0.113(3) Uani 0.456(8) 1 d PDU B 2 O10A O 0.8218(9) 0.8331(10) 0.3422(7) 0.111(3) Uani 0.544(8) 1 d PDU B 1 O10B O 0.9291(18) 0.8534(15) 0.3807(3) 0.112(3) Uani 0.456(8) 1 d PDU B 2 N1 N 0.7985(5) 1.1012(4) 0.1315(3) 0.0506(13) Uani 1 1 d . . . N2 N 0.6166(5) 1.0450(4) 0.1613(3) 0.0545(14) Uani 1 1 d . . . N3 N 0.7326(5) 0.6066(4) 0.0889(4) 0.0583(15) Uani 1 1 d . . . N4 N 0.9299(4) 0.6937(4) 0.0885(3) 0.0515(13) Uani 1 1 d . . . C1 C 0.9347(5) 0.9349(5) 0.0939(4) 0.0491(15) Uani 1 1 d . . . C2 C 1.0081(6) 0.8697(5) 0.0742(4) 0.0556(17) Uani 1 1 d . . . C3 C 1.1104(6) 0.9042(6) 0.0830(4) 0.0638(19) Uani 1 1 d . . . H3A H 1.1583 0.8589 0.0710 0.077 Uiso 1 1 calc R . . C4 C 1.1451(6) 1.0049(6) 0.1092(4) 0.0620(18) Uani 1 1 d . . . C5 C 1.0700(6) 1.0697(5) 0.1249(4) 0.0562(17) Uani 1 1 d . . . H5A H 1.0900 1.1377 0.1409 0.067 Uiso 1 1 calc R . . C6 C 0.9657(5) 1.0379(5) 0.1177(4) 0.0494(15) Uani 1 1 d . . . C7 C 0.8933(6) 1.1153(5) 0.1317(4) 0.0528(16) Uani 1 1 d . . . H7B H 0.9199 1.1829 0.1420 0.063 Uiso 1 1 calc R . . C8 C 0.7355(6) 1.1872(5) 0.1496(5) 0.065(2) Uani 1 1 d . . . H8B H 0.6879 1.2167 0.1023 0.078 Uiso 1 1 calc R . . H8C H 0.7824 1.2419 0.1780 0.078 Uiso 1 1 calc R . . C9 C 0.6719(6) 1.1404(5) 0.1986(4) 0.0621(19) Uani 1 1 d . . . H9A H 0.7195 1.1235 0.2497 0.075 Uiso 1 1 calc R . . H9B H 0.6198 1.1908 0.2046 0.075 Uiso 1 1 calc R . . C10 C 0.8206(7) 0.5352(5) 0.0800(5) 0.070(2) Uani 1 1 d . . . H10A H 0.8604 0.5072 0.1303 0.084 Uiso 1 1 calc R . . H10B H 0.7889 0.4771 0.0465 0.084 Uiso 1 1 calc R . . C11 C 0.8951(7) 0.5920(6) 0.0468(5) 0.073(2) Uani 1 1 d . . . H11A H 0.8599 0.6055 -0.0077 0.087 Uiso 1 1 calc R . . H11B H 0.9574 0.5489 0.0511 0.087 Uiso 1 1 calc R . . C12 C 0.9706(6) 0.7623(6) 0.0377(4) 0.0621(19) Uani 1 1 d . . . H12A H 0.9145 0.7724 -0.0110 0.075 Uiso 1 1 calc R . . H12B H 1.0299 0.7278 0.0265 0.075 Uiso 1 1 calc R . . C13 C 0.5218(6) 1.0698(7) 0.0937(5) 0.076(2) Uani 1 1 d . . . H13A H 0.4695 1.1058 0.1113 0.114 Uiso 1 1 calc R . . H13B H 0.4916 1.0061 0.0683 0.114 Uiso 1 1 calc R . . H13C H 0.5434 1.1133 0.0581 0.114 Uiso 1 1 calc R . . C14 C 0.5798(8) 0.9845(7) 0.2187(5) 0.079(2) Uani 1 1 d . . . H14A H 0.5278 1.0246 0.2339 0.119 Uiso 1 1 calc R . . H14B H 0.6398 0.9699 0.2634 0.119 Uiso 1 1 calc R . . H14C H 0.5482 0.9200 0.1957 0.119 Uiso 1 1 calc R . . C15 C 0.6330(7) 0.6006(6) 0.0217(5) 0.078(2) Uani 1 1 d . . . H15A H 0.5760 0.6359 0.0355 0.094 Uiso 1 1 calc R . . H15B H 0.6127 0.5278 0.0121 0.094 Uiso 1 1 calc R . . C16 C 0.6422(8) 0.6481(8) -0.0520(6) 0.105(3) Uani 1 1 d . . . H16A H 0.5752 0.6411 -0.0923 0.158 Uiso 1 1 calc R . . H16B H 0.6971 0.6126 -0.0671 0.158 Uiso 1 1 calc R . . H16C H 0.6601 0.7207 -0.0437 0.158 Uiso 1 1 calc R . . C17 C 0.7089(7) 0.5799(6) 0.1626(5) 0.077(2) Uani 1 1 d . . . H17A H 0.6571 0.6297 0.1699 0.092 Uiso 1 1 calc R . . H17B H 0.7740 0.5882 0.2055 0.092 Uiso 1 1 calc R . . C18 C 0.6656(9) 0.4697(7) 0.1658(6) 0.100(3) Uani 1 1 d . . . H18A H 0.6529 0.4594 0.2147 0.150 Uiso 1 1 calc R . . H18B H 0.7170 0.4194 0.1602 0.150 Uiso 1 1 calc R . . H18C H 0.5999 0.4610 0.1246 0.150 Uiso 1 1 calc R . . C19 C 1.0140(6) 0.6741(7) 0.1631(5) 0.077(2) Uani 1 1 d . . . H19A H 1.0762 0.6457 0.1532 0.116 Uiso 1 1 calc R . . H19B H 0.9878 0.6254 0.1932 0.116 Uiso 1 1 calc R . . H19C H 1.0324 0.7386 0.1910 0.116 Uiso 1 1 calc R . . C20 C 1.2552(7) 1.0418(7) 0.1146(5) 0.082(2) Uani 1 1 d . . . H20A H 1.2950 0.9853 0.1020 0.123 Uiso 1 1 calc R . . H20B H 1.2907 1.0654 0.1664 0.123 Uiso 1 1 calc R . . H20C H 1.2505 1.0983 0.0789 0.123 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 Cu1 0.0582(5) 0.0321(4) 0.0518(5) -0.0052(3) 0.0175(4) 0.0041(3) Cu2 0.0590(5) 0.0323(4) 0.0558(5) -0.0069(3) 0.0181(4) 0.0024(4) Cl1 0.0857(15) 0.0673(13) 0.0981(17) 0.0014(12) 0.0412(14) -0.0003(11) Cl2 0.1087(16) 0.0494(10) 0.0543(10) -0.0006(8) -0.0014(11) 0.0173(11) O1 0.058(3) 0.034(2) 0.058(3) -0.0069(19) 0.023(2) 0.002(2) O2 0.053(3) 0.037(2) 0.099(4) -0.019(2) 0.025(3) -0.001(2) O3A 0.153(18) 0.110(13) 0.126(14) 0.029(11) 0.054(13) 0.002(12) O3B 0.083(9) 0.142(14) 0.166(15) 0.057(12) 0.052(10) -0.009(10) O4A 0.112(13) 0.149(17) 0.127(14) -0.012(12) 0.030(11) 0.008(12) O4B 0.169(15) 0.095(11) 0.180(17) 0.051(11) 0.092(13) 0.050(11) O5A 0.122(14) 0.21(2) 0.160(19) 0.104(18) 0.070(14) 0.002(14) O5B 0.179(17) 0.098(11) 0.117(12) 0.020(9) 0.051(11) 0.035(11) O6A 0.19(2) 0.098(12) 0.153(17) -0.065(12) 0.034(14) -0.003(13) O6B 0.111(12) 0.146(15) 0.182(17) -0.057(14) 0.057(12) -0.038(11) O7 0.133(5) 0.048(3) 0.070(3) 0.002(3) -0.001(4) 0.016(3) O8 0.160(6) 0.048(3) 0.064(3) -0.007(3) 0.024(4) 0.003(4) O9A 0.149(7) 0.090(5) 0.084(5) 0.002(5) 0.013(5) 0.020(6) O9B 0.147(8) 0.089(5) 0.087(5) -0.003(5) 0.011(6) 0.018(6) O10A 0.152(8) 0.096(5) 0.082(5) 0.011(5) 0.030(5) 0.023(6) O10B 0.152(7) 0.094(5) 0.081(5) 0.007(4) 0.021(5) 0.021(6) N1 0.060(3) 0.036(3) 0.055(3) -0.001(2) 0.016(3) 0.008(3) N2 0.069(4) 0.043(3) 0.053(3) -0.007(3) 0.022(3) 0.005(3) N3 0.064(4) 0.037(3) 0.074(4) -0.011(3) 0.021(3) -0.002(3) N4 0.065(3) 0.038(3) 0.051(3) -0.006(2) 0.017(3) 0.011(3) C1 0.061(4) 0.044(3) 0.043(3) 0.002(3) 0.017(3) -0.001(3) C2 0.066(4) 0.048(4) 0.054(4) -0.006(3) 0.021(3) 0.002(3) C3 0.063(5) 0.062(5) 0.071(5) 0.004(4) 0.029(4) 0.012(4) C4 0.063(4) 0.063(4) 0.060(4) 0.002(4) 0.019(4) -0.009(4) C5 0.075(5) 0.044(4) 0.050(4) -0.001(3) 0.020(4) -0.011(4) C6 0.061(4) 0.043(3) 0.042(3) 0.002(3) 0.012(3) -0.002(3) C7 0.076(5) 0.033(3) 0.046(4) 0.002(3) 0.013(3) 0.001(3) C8 0.081(5) 0.036(4) 0.075(5) -0.014(3) 0.017(4) 0.009(4) C9 0.076(5) 0.050(4) 0.060(4) -0.013(3) 0.020(4) 0.013(4) C10 0.099(6) 0.031(3) 0.087(5) -0.011(4) 0.039(5) 0.008(4) C11 0.096(6) 0.048(4) 0.081(5) -0.018(4) 0.037(5) 0.004(4) C12 0.069(5) 0.056(4) 0.067(5) -0.009(4) 0.030(4) 0.010(4) C13 0.067(5) 0.082(6) 0.072(5) -0.010(4) 0.010(4) 0.013(4) C14 0.108(6) 0.070(5) 0.077(5) 0.005(4) 0.055(5) 0.009(5) C15 0.079(5) 0.053(4) 0.098(6) -0.026(4) 0.022(5) -0.016(4) C16 0.113(8) 0.094(7) 0.084(7) -0.002(6) -0.004(6) -0.028(6) C17 0.097(6) 0.048(4) 0.092(6) -0.011(4) 0.039(5) -0.015(4) C18 0.147(9) 0.056(5) 0.112(8) -0.007(5) 0.063(7) -0.007(6) C19 0.079(5) 0.078(5) 0.065(5) 0.003(4) 0.009(4) 0.025(5) C20 0.082(5) 0.082(6) 0.088(6) 0.005(5) 0.035(5) -0.015(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 Cu1 O2 1.910(4) . ? Cu1 N1 1.928(6) . ? Cu1 O1 1.974(4) . ? Cu1 N2 2.037(6) . ? Cu1 Cu2 2.9596(13) . ? Cu2 O2 1.940(4) . ? Cu2 O1 1.979(4) . ? Cu2 N4 2.005(5) . ? Cu2 N3 2.030(5) . ? Cl1 O5A 1.406(5) . ? Cl1 O3B 1.406(5) . ? Cl1 O4A 1.407(5) . ? Cl1 O6B 1.407(5) . ? Cl1 O4B 1.407(5) . ? Cl1 O6A 1.408(5) . ? Cl1 O5B 1.408(5) . ? Cl1 O3A 1.408(5) . ? Cl2 O8 1.394(6) . ? Cl2 O7 1.406(4) . ? Cl2 O10B 1.407(5) . ? Cl2 O9A 1.408(5) . ? Cl2 O9B 1.412(5) . ? Cl2 O10A 1.412(5) . ? O1 C1 1.328(8) . ? N1 C7 1.257(9) . ? N1 C8 1.473(8) . ? N2 C9 1.475(9) . ? N2 C13 1.488(9) . ? N2 C14 1.492(10) . ? N3 C15 1.491(10) . ? N3 C17 1.502(10) . ? N3 C10 1.520(9) . ? N4 C19 1.482(9) . ? N4 C12 1.486(9) . ? N4 C11 1.504(9) . ? C1 C2 1.402(9) . ? C1 C6 1.407(9) . ? C2 C3 1.377(10) . ? C2 C12 1.540(10) . ? C3 C4 1.400(11) . ? C4 C5 1.383(10) . ? C4 C20 1.496(11) . ? C5 C6 1.398(9) . ? C6 C7 1.449(9) . ? C8 C9 1.517(10) . ? C10 C11 1.487(11) . ? C15 C16 1.508(13) . ? C17 C18 1.529(11) . ? 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 O2 Cu1 N1 169.5(2) . . ? O2 Cu1 O1 79.16(19) . . ? N1 Cu1 O1 91.7(2) . . ? O2 Cu1 N2 103.1(2) . . ? N1 Cu1 N2 86.0(2) . . ? O1 Cu1 N2 177.6(2) . . ? O2 Cu1 Cu2 40.12(14) . . ? N1 Cu1 Cu2 132.24(17) . . ? O1 Cu1 Cu2 41.58(13) . . ? N2 Cu1 Cu2 140.77(17) . . ? O2 Cu2 O1 78.33(19) . . ? O2 Cu2 N4 171.0(2) . . ? O1 Cu2 N4 93.1(2) . . ? O2 Cu2 N3 99.2(2) . . ? O1 Cu2 N3 169.1(2) . . ? N4 Cu2 N3 88.8(2) . . ? O2 Cu2 Cu1 39.38(13) . . ? O1 Cu2 Cu1 41.46(12) . . ? N4 Cu2 Cu1 132.96(16) . . ? N3 Cu2 Cu1 138.20(17) . . ? O5A Cl1 O3B 156.2(13) . . ? O5A Cl1 O4A 116.1(13) . . ? O3B Cl1 O4A 73.9(11) . . ? O5A Cl1 O6B 58.0(11) . . ? O3B Cl1 O6B 113.6(11) . . ? O4A Cl1 O6B 172.1(13) . . ? O5A Cl1 O4B 92.1(12) . . ? O3B Cl1 O4B 111.4(10) . . ? O4A Cl1 O4B 63.4(11) . . ? O6B Cl1 O4B 110.3(12) . . ? O5A Cl1 O6A 113.0(17) . . ? O3B Cl1 O6A 78.9(11) . . ? O4A Cl1 O6A 113.4(12) . . ? O6B Cl1 O6A 67.3(10) . . ? O4B Cl1 O6A 72.9(11) . . ? O5A Cl1 O5B 60.3(13) . . ? O3B Cl1 O5B 106.0(12) . . ? O4A Cl1 O5B 73.6(11) . . ? O6B Cl1 O5B 105.4(11) . . ? O4B Cl1 O5B 109.7(10) . . ? O6A Cl1 O5B 172.6(13) . . ? O5A Cl1 O3A 109.6(13) . . ? O3B Cl1 O3A 47.0(9) . . ? O4A Cl1 O3A 106.0(13) . . ? O6B Cl1 O3A 81.5(12) . . ? O4B Cl1 O3A 158.3(11) . . ? O6A Cl1 O3A 96.6(12) . . ? O5B Cl1 O3A 83.2(10) . . ? O8 Cl2 O7 112.0(4) . . ? O8 Cl2 O10B 126.3(8) . . ? O7 Cl2 O10B 120.1(8) . . ? O8 Cl2 O9A 117.1(7) . . ? O7 Cl2 O9A 122.0(7) . . ? O10B Cl2 O9A 40.2(9) . . ? O8 Cl2 O9B 93.5(7) . . ? O7 Cl2 O9B 96.5(7) . . ? O10B Cl2 O9B 93.0(11) . . ? O9A Cl2 O9B 53.0(9) . . ? O8 Cl2 O10A 99.1(7) . . ? O7 Cl2 O10A 102.0(6) . . ? O10B Cl2 O10A 59.2(10) . . ? O9A Cl2 O10A 98.7(9) . . ? O9B Cl2 O10A 151.7(8) . . ? C1 O1 Cu1 126.9(4) . . ? C1 O1 Cu2 128.3(4) . . ? Cu1 O1 Cu2 96.96(19) . . ? Cu1 O2 Cu2 100.5(2) . . ? C7 N1 C8 121.0(6) . . ? C7 N1 Cu1 125.8(5) . . ? C8 N1 Cu1 112.5(5) . . ? C9 N2 C13 111.8(6) . . ? C9 N2 C14 109.2(6) . . ? C13 N2 C14 108.5(6) . . ? C9 N2 Cu1 104.5(4) . . ? C13 N2 Cu1 109.6(4) . . ? C14 N2 Cu1 113.3(5) . . ? C15 N3 C17 110.2(6) . . ? C15 N3 C10 112.9(6) . . ? C17 N3 C10 109.2(6) . . ? C15 N3 Cu2 110.2(5) . . ? C17 N3 Cu2 108.3(4) . . ? C10 N3 Cu2 105.8(4) . . ? C19 N4 C12 110.9(6) . . ? C19 N4 C11 109.8(6) . . ? C12 N4 C11 108.2(5) . . ? C19 N4 Cu2 114.4(5) . . ? C12 N4 Cu2 109.6(4) . . ? C11 N4 Cu2 103.6(5) . . ? O1 C1 C2 119.3(6) . . ? O1 C1 C6 122.0(6) . . ? C2 C1 C6 118.7(6) . . ? C3 C2 C1 120.2(6) . . ? C3 C2 C12 120.5(6) . . ? C1 C2 C12 119.2(6) . . ? C2 C3 C4 122.6(7) . . ? C5 C4 C3 116.3(7) . . ? C5 C4 C20 122.2(7) . . ? C3 C4 C20 121.4(8) . . ? C4 C5 C6 123.2(6) . . ? C5 C6 C1 118.9(6) . . ? C5 C6 C7 117.5(6) . . ? C1 C6 C7 123.5(6) . . ? N1 C7 C6 127.1(6) . . ? N1 C8 C9 106.5(6) . . ? N2 C9 C8 109.9(5) . . ? C11 C10 N3 111.5(6) . . ? C10 C11 N4 110.8(6) . . ? N4 C12 C2 112.9(6) . . ? N3 C15 C16 114.5(7) . . ? N3 C17 C18 115.1(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 Cu2 O2 -169.7(3) . . . . ? O1 Cu1 Cu2 O2 -153.9(3) . . . . ? N2 Cu1 Cu2 O2 26.1(4) . . . . ? O2 Cu1 Cu2 O1 153.9(3) . . . . ? N1 Cu1 Cu2 O1 -15.8(3) . . . . ? N2 Cu1 Cu2 O1 180.0(3) . . . . ? O2 Cu1 Cu2 N4 173.2(3) . . . . ? N1 Cu1 Cu2 N4 3.5(3) . . . . ? O1 Cu1 Cu2 N4 19.3(3) . . . . ? N2 Cu1 Cu2 N4 -160.7(3) . . . . ? O2 Cu1 Cu2 N3 -9.7(4) . . . . ? N1 Cu1 Cu2 N3 -179.3(3) . . . . ? O1 Cu1 Cu2 N3 -163.5(3) . . . . ? N2 Cu1 Cu2 N3 16.5(4) . . . . ? O2 Cu1 O1 C1 -167.5(5) . . . . ? N1 Cu1 O1 C1 17.6(5) . . . . ? N2 Cu1 O1 C1 29(5) . . . . ? Cu2 Cu1 O1 C1 -150.8(6) . . . . ? O2 Cu1 O1 Cu2 -16.8(2) . . . . ? N1 Cu1 O1 Cu2 168.4(2) . . . . ? N2 Cu1 O1 Cu2 180(100) . . . . ? O2 Cu2 O1 C1 166.7(5) . . . . ? N4 Cu2 O1 C1 -15.9(5) . . . . ? N3 Cu2 O1 C1 -115.5(11) . . . . ? Cu1 Cu2 O1 C1 150.1(6) . . . . ? O2 Cu2 O1 Cu1 16.6(2) . . . . ? N4 Cu2 O1 Cu1 -166.0(2) . . . . ? N3 Cu2 O1 Cu1 94.4(11) . . . . ? N1 Cu1 O2 Cu2 46.9(13) . . . . ? O1 Cu1 O2 Cu2 17.3(2) . . . . ? N2 Cu1 O2 Cu2 -163.4(2) . . . . ? O1 Cu2 O2 Cu1 -17.3(2) . . . . ? N4 Cu2 O2 Cu1 -33.9(15) . . . . ? N3 Cu2 O2 Cu1 173.5(2) . . . . ? O2 Cu1 N1 C7 -45.2(15) . . . . ? O1 Cu1 N1 C7 -16.1(6) . . . . ? N2 Cu1 N1 C7 164.4(6) . . . . ? Cu2 Cu1 N1 C7 -5.7(7) . . . . ? O2 Cu1 N1 C8 144.1(11) . . . . ? O1 Cu1 N1 C8 173.2(5) . . . . ? N2 Cu1 N1 C8 -6.3(5) . . . . ? Cu2 Cu1 N1 C8 -176.4(4) . . . . ? O2 Cu1 N2 C9 164.9(4) . . . . ? N1 Cu1 N2 C9 -20.4(4) . . . . ? O1 Cu1 N2 C9 -32(5) . . . . ? Cu2 Cu1 N2 C9 147.9(3) . . . . ? O2 Cu1 N2 C13 -75.2(5) . . . . ? N1 Cu1 N2 C13 99.5(5) . . . . ? O1 Cu1 N2 C13 88(5) . . . . ? Cu2 Cu1 N2 C13 -92.1(5) . . . . ? O2 Cu1 N2 C14 46.1(6) . . . . ? N1 Cu1 N2 C14 -139.2(6) . . . . ? O1 Cu1 N2 C14 -151(5) . . . . ? Cu2 Cu1 N2 C14 29.2(6) . . . . ? O2 Cu2 N3 C15 54.1(5) . . . . ? O1 Cu2 N3 C15 -21.8(14) . . . . ? N4 Cu2 N3 C15 -121.8(5) . . . . ? Cu1 Cu2 N3 C15 60.3(6) . . . . ? O2 Cu2 N3 C17 -66.6(5) . . . . ? O1 Cu2 N3 C17 -142.4(10) . . . . ? N4 Cu2 N3 C17 117.5(5) . . . . ? Cu1 Cu2 N3 C17 -60.4(6) . . . . ? O2 Cu2 N3 C10 176.4(5) . . . . ? O1 Cu2 N3 C10 100.6(11) . . . . ? N4 Cu2 N3 C10 0.5(5) . . . . ? Cu1 Cu2 N3 C10 -177.4(4) . . . . ? O2 Cu2 N4 C19 110.8(14) . . . . ? O1 Cu2 N4 C19 94.5(5) . . . . ? N3 Cu2 N4 C19 -96.2(5) . . . . ? Cu1 Cu2 N4 C19 81.9(5) . . . . ? O2 Cu2 N4 C12 -14.4(16) . . . . ? O1 Cu2 N4 C12 -30.7(4) . . . . ? N3 Cu2 N4 C12 138.5(5) . . . . ? Cu1 Cu2 N4 C12 -43.3(5) . . . . ? O2 Cu2 N4 C11 -129.7(13) . . . . ? O1 Cu2 N4 C11 -145.9(4) . . . . ? N3 Cu2 N4 C11 23.3(5) . . . . ? Cu1 Cu2 N4 C11 -158.6(4) . . . . ? Cu1 O1 C1 C2 171.5(4) . . . . ? Cu2 O1 C1 C2 29.7(8) . . . . ? Cu1 O1 C1 C6 -10.1(9) . . . . ? Cu2 O1 C1 C6 -152.0(5) . . . . ? O1 C1 C2 C3 -177.5(6) . . . . ? C6 C1 C2 C3 4.1(10) . . . . ? O1 C1 C2 C12 6.6(9) . . . . ? C6 C1 C2 C12 -171.8(6) . . . . ? C1 C2 C3 C4 -1.8(11) . . . . ? C12 C2 C3 C4 173.9(7) . . . . ? C2 C3 C4 C5 -1.1(11) . . . . ? C2 C3 C4 C20 -177.2(7) . . . . ? C3 C4 C5 C6 1.8(10) . . . . ? C20 C4 C5 C6 177.9(7) . . . . ? C4 C5 C6 C1 0.4(10) . . . . ? C4 C5 C6 C7 -176.6(6) . . . . ? O1 C1 C6 C5 178.3(6) . . . . ? C2 C1 C6 C5 -3.3(9) . . . . ? O1 C1 C6 C7 -5.0(10) . . . . ? C2 C1 C6 C7 173.4(6) . . . . ? C8 N1 C7 C6 177.8(6) . . . . ? Cu1 N1 C7 C6 7.8(10) . . . . ? C5 C6 C7 N1 -176.7(7) . . . . ? C1 C6 C7 N1 6.5(11) . . . . ? C7 N1 C8 C9 -140.2(7) . . . . ? Cu1 N1 C8 C9 31.0(7) . . . . ? C13 N2 C9 C8 -75.4(7) . . . . ? C14 N2 C9 C8 164.6(6) . . . . ? Cu1 N2 C9 C8 43.0(6) . . . . ? N1 C8 C9 N2 -49.5(7) . . . . ? C15 N3 C10 C11 94.9(8) . . . . ? C17 N3 C10 C11 -142.1(7) . . . . ? Cu2 N3 C10 C11 -25.7(8) . . . . ? N3 C10 C11 N4 48.3(9) . . . . ? C19 N4 C11 C10 78.6(8) . . . . ? C12 N4 C11 C10 -160.3(6) . . . . ? Cu2 N4 C11 C10 -44.1(7) . . . . ? C19 N4 C12 C2 -60.0(7) . . . . ? C11 N4 C12 C2 179.6(6) . . . . ? Cu2 N4 C12 C2 67.3(7) . . . . ? C3 C2 C12 N4 124.1(7) . . . . ? C1 C2 C12 N4 -60.0(8) . . . . ? C17 N3 C15 C16 167.4(7) . . . . ? C10 N3 C15 C16 -70.2(9) . . . . ? Cu2 N3 C15 C16 47.8(8) . . . . ? C15 N3 C17 C18 61.5(10) . . . . ? C10 N3 C17 C18 -63.1(10) . . . . ? Cu2 N3 C17 C18 -177.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.734 _refine_diff_density_min -1.076 _refine_diff_density_rms 0.109 data_ifn6mons _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H58 Cl2 N4 Ni2 O18' _chemical_formula_weight 951.12 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.938(6) _cell_length_b 10.148(2) _cell_length_c 17.916(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.963(4) _cell_angle_gamma 90.00 _cell_volume 3867.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 57 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 28.20 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6098 _exptl_absorpt_correction_T_max 0.8900 _exptl_absorpt_process_details ? _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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12499 _diffrn_reflns_av_R_equivalents 0.1299 _diffrn_reflns_av_sigmaI/netI 0.1316 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.20 _reflns_number_total 4584 _reflns_number_gt 1688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL-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^)+(0.2000P)^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 4584 _refine_ls_number_parameters 383 _refine_ls_number_restraints 144 _refine_ls_R_factor_all 0.2391 _refine_ls_R_factor_gt 0.1264 _refine_ls_wR_factor_ref 0.3780 _refine_ls_wR_factor_gt 0.3124 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.008 _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 -0.04457(6) 0.58267(12) -0.07067(7) 0.0899(7) Uani 1 1 d . . . O1 O 0.0418(3) 0.4981(6) -0.0335(3) 0.0868(18) Uani 1 1 d . . . C1 C 0.0905(6) 0.5319(10) -0.0517(5) 0.081(3) Uani 1 1 d . . . C2 C 0.0941(7) 0.6391(11) -0.0958(6) 0.104(4) Uani 1 1 d . A . C3 C 0.1471(8) 0.6820(11) -0.1105(7) 0.108(4) Uani 1 1 d . . . H3 H 0.1452 0.7583 -0.1400 0.129 Uiso 1 1 calc R A . C4 C 0.1989(6) 0.6135(12) -0.0824(7) 0.105(4) Uani 1 1 d D A . C5 C 0.1984(6) 0.4970(10) -0.0355(6) 0.100(3) Uani 1 1 d . . . H5 H 0.2350 0.4478 -0.0127 0.120 Uiso 1 1 calc R A . C6 C 0.1447(6) 0.4580(11) -0.0241(6) 0.095(3) Uani 1 1 d . A . C7A C 0.264(2) 0.655(14) -0.082(4) 0.127(13) Uani 0.557(9) 1 d PDU A 1 H7A1 H 0.2960 0.6235 -0.0336 0.190 Uiso 0.557(9) 1 calc PR A 1 H7A2 H 0.2657 0.7496 -0.0836 0.190 Uiso 0.557(9) 1 calc PR A 1 H7A3 H 0.2695 0.6186 -0.1278 0.190 Uiso 0.557(9) 1 calc PR A 1 C7B C 0.255(4) 0.656(19) -0.105(6) 0.133(16) Uani 0.443(9) 1 d PDU A 2 H7B1 H 0.2931 0.6215 -0.0656 0.200 Uiso 0.443(9) 1 calc PR A 2 H7B2 H 0.2571 0.7504 -0.1050 0.200 Uiso 0.443(9) 1 calc PR A 2 H7B3 H 0.2493 0.6225 -0.1569 0.200 Uiso 0.443(9) 1 calc PR A 2 C8 C 0.1475(5) 0.3310(12) 0.0206(6) 0.106(3) Uani 1 1 d . . . H8A H 0.1896 0.2949 0.0384 0.127 Uiso 0.557(9) 1 calc PR A 1 H8B H 0.1188 0.2674 -0.0148 0.127 Uiso 0.557(9) 1 calc PR A 1 H8C H 0.1168 0.2737 -0.0175 0.127 Uiso 0.443(9) 1 calc PR A 2 H8D H 0.1883 0.2934 0.0288 0.127 Uiso 0.443(9) 1 calc PR A 2 C9A C 0.1405(9) 0.229(2) 0.1434(11) 0.092(4) Uani 0.557(9) 1 d PU A 1 H9A1 H 0.1303 0.2388 0.1911 0.110 Uiso 0.557(9) 1 calc PR A 1 H9A2 H 0.1115 0.1654 0.1089 0.110 Uiso 0.557(9) 1 calc PR A 1 N1A N 0.1278(10) 0.359(2) 0.1003(12) 0.081(4) Uani 0.557(9) 1 d PU . 1 C10A C 0.2025(12) 0.175(2) 0.1681(16) 0.141(10) Uani 0.557(9) 1 d P A 1 H10A H 0.2046 0.0954 0.1978 0.211 Uiso 0.557(9) 1 calc PR A 1 H10B H 0.2323 0.2375 0.2015 0.211 Uiso 0.557(9) 1 calc PR A 1 H10C H 0.2120 0.1562 0.1214 0.211 Uiso 0.557(9) 1 calc PR A 1 C11A C 0.1703(8) 0.468(2) 0.1515(9) 0.078(4) Uani 0.557(9) 1 d PU A 1 H11A H 0.2088 0.4297 0.1894 0.093 Uiso 0.557(9) 1 calc PR A 1 H11B H 0.1812 0.5293 0.1174 0.093 Uiso 0.557(9) 1 calc PR A 1 N2A N -0.0751(7) 0.4165(16) -0.1450(10) 0.085(4) Uani 0.557(9) 1 d PU . 1 C12A C 0.1351(9) 0.538(2) 0.1964(14) 0.083(5) Uani 0.557(9) 1 d PU . 1 H12A H 0.1302 0.4791 0.2360 0.099 Uiso 0.557(9) 1 calc PR A 1 H12B H 0.1599 0.6131 0.2249 0.099 Uiso 0.557(9) 1 calc PR A 1 C13A C -0.0795(11) 0.2914(19) -0.1069(12) 0.109(5) Uani 0.557(9) 1 d PU A 1 H13A H -0.0383 0.2641 -0.0718 0.163 Uiso 0.557(9) 1 calc PR A 1 H13B H -0.0974 0.2256 -0.1475 0.163 Uiso 0.557(9) 1 calc PR A 1 H13C H -0.1057 0.3023 -0.0762 0.163 Uiso 0.557(9) 1 calc PR A 1 C14A C -0.0448(13) 0.395(2) -0.2067(14) 0.100(7) Uani 0.557(9) 1 d PU A 1 H14A H -0.0029 0.3616 -0.1802 0.150 Uiso 0.557(9) 1 calc PR A 1 H14B H -0.0431 0.4773 -0.2324 0.150 Uiso 0.557(9) 1 calc PR A 1 H14C H -0.0692 0.3329 -0.2465 0.150 Uiso 0.557(9) 1 calc PR A 1 C9B C 0.1364(14) 0.159(3) 0.1110(17) 0.102(5) Uani 0.443(9) 1 d PU A 2 H9B1 H 0.1767 0.1206 0.1167 0.122 Uiso 0.443(9) 1 calc PR A 2 H9B2 H 0.1332 0.1529 0.1634 0.122 Uiso 0.443(9) 1 calc PR A 2 N1B N 0.1397(14) 0.313(3) 0.0916(17) 0.088(4) Uani 0.443(9) 1 d PU . 2 C10B C 0.0937(13) 0.083(2) 0.063(2) 0.116(10) Uani 0.443(9) 1 d P A 2 H10D H 0.0965 -0.0026 0.0876 0.174 Uiso 0.443(9) 1 calc PR A 2 H10E H 0.0996 0.0743 0.0133 0.174 Uiso 0.443(9) 1 calc PR A 2 H10F H 0.0530 0.1198 0.0537 0.174 Uiso 0.443(9) 1 calc PR A 2 C11B C 0.1899(11) 0.378(3) 0.1566(13) 0.089(4) Uani 0.443(9) 1 d PU A 2 H11C H 0.2086 0.4462 0.1349 0.107 Uiso 0.443(9) 1 calc PR A 2 H11D H 0.2224 0.3144 0.1845 0.107 Uiso 0.443(9) 1 calc PR A 2 N2B N -0.1082(12) 0.483(3) -0.1709(14) 0.090(5) Uani 0.443(9) 1 d PU . 2 C12B C 0.1642(10) 0.436(2) 0.2128(15) 0.088(5) Uani 0.443(9) 1 d PU . 2 H12C H 0.1961 0.4901 0.2516 0.106 Uiso 0.443(9) 1 calc PR A 2 H12D H 0.1532 0.3659 0.2420 0.106 Uiso 0.443(9) 1 calc PR A 2 C13B C -0.1316(10) 0.364(2) -0.1442(11) 0.089(5) Uani 0.443(9) 1 d PU A 2 H13D H -0.1536 0.3881 -0.1100 0.133 Uiso 0.443(9) 1 calc PR A 2 H13E H -0.0967 0.3077 -0.1149 0.133 Uiso 0.443(9) 1 calc PR A 2 H13F H -0.1596 0.3170 -0.1903 0.133 Uiso 0.443(9) 1 calc PR A 2 C14B C -0.0791(14) 0.456(3) -0.2244(17) 0.094(8) Uani 0.443(9) 1 d PU A 2 H14D H -0.0643 0.5372 -0.2390 0.142 Uiso 0.443(9) 1 calc PR A 2 H14E H -0.1086 0.4155 -0.2717 0.142 Uiso 0.443(9) 1 calc PR A 2 H14F H -0.0442 0.3982 -0.1995 0.142 Uiso 0.443(9) 1 calc PR A 2 C15 C 0.0468(5) 0.7044(13) -0.1356(7) 0.147(7) Uani 1 1 d D . . H15A H 0.0552 0.7791 -0.1600 0.176 Uiso 0.557(9) 1 calc PR A 1 H15B H 0.0524 0.7474 -0.1783 0.176 Uiso 0.443(9) 1 calc PR A 2 O2A O -0.0233(4) 0.6830(14) -0.1515(9) 0.089(4) Uani 0.557(9) 1 d PDU A 1 O2B O -0.0186(5) 0.7339(18) -0.1339(12) 0.108(5) Uani 0.443(9) 1 d PDU A 2 O3 O 0.0018(7) 0.7544(15) 0.0012(9) 0.217(6) Uani 1 1 d . A . Cl1 Cl -0.35817(16) 0.5649(4) -0.1730(2) 0.1283(14) Uani 1 1 d . . . O4A O -0.3376(12) 0.604(2) -0.2496(16) 0.190(10) Uani 0.522(14) 1 d P B 1 O5A O -0.4111(9) 0.499(2) -0.2280(12) 0.140(7) Uani 0.522(14) 1 d PU B 1 O7A O -0.3104(12) 0.488(2) -0.1324(14) 0.152(7) Uani 0.522(14) 1 d PU B 1 O4B O -0.3179(12) 0.462(2) -0.1865(15) 0.126(6) Uani 0.478(14) 1 d PU B 2 O5B O -0.4178(12) 0.604(3) -0.197(2) 0.183(9) Uani 0.478(14) 1 d PU B 2 O7B O -0.3575(9) 0.5127(16) -0.0914(9) 0.123(6) Uani 0.478(14) 1 d PU B 2 O6 O -0.3334(7) 0.6845(12) -0.1511(8) 0.203(5) Uani 1 1 d . B . O1S O 0.0085(8) 0.140(2) -0.1340(12) 0.283(9) Uani 1 1 d . . . O2SA O -0.0538(18) 0.042(4) 0.018(3) 0.283(14) Uani 0.39(2) 1 d PU C 1 O2SB O 0.0028(12) 0.035(3) 0.105(2) 0.282(14) Uani 0.61(2) 1 d PU C 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 0.1374(12) 0.0839(9) 0.0489(7) 0.0046(5) 0.0354(7) -0.0310(7) O1 0.131(5) 0.088(4) 0.047(3) 0.001(3) 0.041(3) -0.038(4) C1 0.127(8) 0.076(6) 0.045(4) -0.009(4) 0.039(5) -0.024(6) C2 0.178(11) 0.085(7) 0.041(5) 0.008(5) 0.031(7) -0.006(8) C3 0.195(12) 0.080(7) 0.088(7) -0.014(6) 0.099(9) -0.048(8) C4 0.159(10) 0.094(8) 0.092(8) -0.029(6) 0.084(8) -0.029(8) C5 0.153(9) 0.094(7) 0.074(6) -0.028(5) 0.067(7) -0.047(7) C6 0.147(9) 0.095(7) 0.057(5) -0.013(5) 0.056(6) -0.046(7) C7A 0.22(2) 0.101(12) 0.13(4) -0.02(3) 0.14(3) -0.05(2) C7B 0.22(2) 0.108(14) 0.13(4) -0.02(4) 0.13(2) -0.05(2) C8 0.114(7) 0.127(9) 0.070(6) 0.016(6) 0.026(6) -0.017(7) C9A 0.105(7) 0.104(9) 0.059(7) 0.018(6) 0.021(6) 0.000(7) N1A 0.092(7) 0.101(9) 0.046(5) 0.012(5) 0.020(5) 0.001(6) C10A 0.18(2) 0.133(18) 0.14(2) 0.092(16) 0.100(19) 0.082(17) C11A 0.090(7) 0.101(9) 0.044(6) 0.005(6) 0.027(5) 0.004(7) N2A 0.087(8) 0.096(9) 0.068(8) -0.006(6) 0.025(7) -0.031(7) C12A 0.078(11) 0.081(11) 0.092(12) 0.003(10) 0.035(9) -0.034(9) C13A 0.146(11) 0.086(10) 0.080(10) -0.012(7) 0.026(10) -0.037(10) C14A 0.16(2) 0.092(16) 0.076(13) -0.042(12) 0.076(15) -0.041(12) C9B 0.114(8) 0.109(10) 0.073(8) 0.029(7) 0.024(7) -0.002(8) N1B 0.097(7) 0.106(10) 0.059(6) 0.020(7) 0.026(6) -0.006(7) C10B 0.13(2) 0.052(11) 0.19(3) 0.020(15) 0.08(2) -0.007(13) C11B 0.096(7) 0.112(10) 0.053(6) 0.016(7) 0.020(6) 0.005(7) N2B 0.084(11) 0.112(11) 0.065(10) 0.005(8) 0.016(9) -0.035(9) C12B 0.079(11) 0.098(12) 0.086(12) 0.012(11) 0.028(10) -0.022(9) C13B 0.098(10) 0.129(12) 0.032(8) -0.001(8) 0.016(8) -0.049(9) C14B 0.11(2) 0.12(2) 0.061(12) -0.012(15) 0.044(15) -0.022(14) C15 0.238(17) 0.152(13) 0.088(9) -0.049(9) 0.104(11) -0.144(13) O2A 0.151(7) 0.054(10) 0.030(6) -0.008(5) 0.000(5) -0.063(6) O2B 0.173(9) 0.068(12) 0.035(9) 0.012(8) -0.019(7) -0.073(8) O3 0.243(12) 0.252(14) 0.165(11) -0.070(11) 0.086(10) -0.050(12) Cl1 0.115(2) 0.104(3) 0.130(3) 0.038(2) 0.005(2) -0.0151(19) O4A 0.23(2) 0.20(2) 0.15(2) 0.063(17) 0.085(19) 0.044(17) O5A 0.134(11) 0.131(15) 0.110(14) 0.028(12) -0.006(10) -0.014(13) O7A 0.168(12) 0.138(12) 0.115(13) 0.033(12) 0.014(13) -0.009(11) O4B 0.152(12) 0.117(11) 0.113(14) -0.023(12) 0.056(13) 0.008(10) O5B 0.124(12) 0.20(2) 0.183(19) 0.042(17) 0.010(13) -0.004(16) O7B 0.185(14) 0.107(11) 0.076(9) 0.030(8) 0.049(10) -0.006(10) O6 0.305(15) 0.117(8) 0.169(12) 0.002(8) 0.067(11) -0.002(9) O1S 0.296(18) 0.36(3) 0.242(18) -0.111(18) 0.162(16) -0.007(18) O2SA 0.197(18) 0.22(2) 0.36(4) 0.14(2) 0.024(18) 0.009(17) O2SB 0.197(17) 0.219(19) 0.36(4) 0.14(2) 0.024(17) 0.002(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1A 1.88(2) 5_565 ? Ni1 O2A 1.975(15) . ? Ni1 O1 2.017(5) 5_565 ? Ni1 O1 2.029(7) . ? Ni1 N2A 2.100(15) . ? Ni1 N2B 2.10(2) . ? Ni1 O2B 2.12(2) . ? Ni1 O3 2.192(13) . ? Ni1 N1B 2.32(3) 5_565 ? O1 C1 1.321(11) . ? O1 Ni1 2.017(5) 5_565 ? C1 C2 1.366(14) . ? C1 C6 1.376(14) . ? C2 C15 1.245(15) . ? C2 C3 1.404(17) . ? C3 C4 1.304(16) . ? C4 C5 1.453(16) . ? C4 C7A 1.5400(11) . ? C4 C7B 1.5400(11) . ? C5 C6 1.380(14) . ? C6 C8 1.506(15) . ? C8 N1B 1.36(3) . ? C8 N1A 1.67(2) . ? C9A C10A 1.43(3) . ? C9A N1A 1.50(3) . ? N1A C11A 1.53(3) . ? N1A Ni1 1.88(2) 5_565 ? C11A C12A 1.52(3) . ? N2A C12A 1.41(3) 5_565 ? N2A C13A 1.46(2) . ? N2A C14A 1.53(3) . ? C12A N2A 1.41(3) 5_565 ? C9B C10B 1.29(4) . ? C9B N1B 1.61(4) . ? N1B C11B 1.45(3) . ? N1B Ni1 2.32(3) 5_565 ? C11B C12B 1.47(3) . ? N2B C14B 1.38(4) . ? N2B C12B 1.47(4) 5_565 ? N2B C13B 1.48(3) . ? C12B N2B 1.47(4) 5_565 ? C15 O2A 1.5394(11) . ? C15 O2B 1.5397(11) . ? Cl1 O7A 1.32(2) . ? Cl1 O5B 1.33(3) . ? Cl1 O6 1.336(13) . ? Cl1 O5A 1.416(18) . ? Cl1 O4B 1.47(2) . ? Cl1 O7B 1.549(15) . ? Cl1 O4A 1.66(2) . ? 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 N1A Ni1 O2A 97.7(8) 5_565 . ? N1A Ni1 O1 93.8(7) 5_565 5_565 ? O2A Ni1 O1 163.1(3) . 5_565 ? N1A Ni1 O1 172.6(7) 5_565 . ? O2A Ni1 O1 88.9(4) . . ? O1 Ni1 O1 80.5(3) 5_565 . ? N1A Ni1 N2A 90.7(8) 5_565 . ? O2A Ni1 N2A 93.7(5) . . ? O1 Ni1 N2A 98.5(5) 5_565 . ? O1 Ni1 N2A 85.5(5) . . ? N1A Ni1 N2B 66.5(11) 5_565 . ? O2A Ni1 N2B 84.5(7) . . ? O1 Ni1 N2B 111.5(7) 5_565 . ? O1 Ni1 N2B 111.0(9) . . ? N2A Ni1 N2B 27.4(8) . . ? N1A Ni1 O2B 94.6(8) 5_565 . ? O2A Ni1 O2B 16.2(5) . . ? O1 Ni1 O2B 150.5(5) 5_565 . ? O1 Ni1 O2B 92.7(4) . . ? N2A Ni1 O2B 109.6(6) . . ? N2B Ni1 O2B 97.8(8) . . ? N1A Ni1 O3 97.7(7) 5_565 . ? O2A Ni1 O3 79.8(5) . . ? O1 Ni1 O3 86.5(4) 5_565 . ? O1 Ni1 O3 86.8(4) . . ? N2A Ni1 O3 170.0(6) . . ? N2B Ni1 O3 156.0(9) . . ? O2B Ni1 O3 64.3(6) . . ? N1A Ni1 N1B 10.4(11) 5_565 5_565 ? O2A Ni1 N1B 97.0(8) . 5_565 ? O1 Ni1 N1B 92.2(8) 5_565 5_565 ? O1 Ni1 N1B 170.8(7) . 5_565 ? N2A Ni1 N1B 101.1(8) . 5_565 ? N2B Ni1 N1B 76.7(11) . 5_565 ? O2B Ni1 N1B 91.1(8) . 5_565 ? O3 Ni1 N1B 87.3(8) . 5_565 ? C1 O1 Ni1 126.7(6) . 5_565 ? C1 O1 Ni1 128.4(6) . . ? Ni1 O1 Ni1 99.5(3) 5_565 . ? O1 C1 C2 126.2(12) . . ? O1 C1 C6 120.2(8) . . ? C2 C1 C6 113.6(11) . . ? C15 C2 C1 121.8(14) . . ? C15 C2 C3 111.0(11) . . ? C1 C2 C3 126.9(13) . . ? C4 C3 C2 119.3(11) . . ? C3 C4 C5 117.0(9) . . ? C3 C4 C7A 126(5) . . ? C5 C4 C7A 116(5) . . ? C3 C4 C7B 119(7) . . ? C5 C4 C7B 124(7) . . ? C7A C4 C7B 14(6) . . ? C6 C5 C4 121.3(12) . . ? C1 C6 C5 121.8(10) . . ? C1 C6 C8 120.7(9) . . ? C5 C6 C8 117.5(12) . . ? N1B C8 C6 128.1(15) . . ? N1B C8 N1A 19.0(14) . . ? C6 C8 N1A 109.7(11) . . ? C10A C9A N1A 118.4(17) . . ? C9A N1A C11A 111.4(16) . . ? C9A N1A C8 103.3(13) . . ? C11A N1A C8 108.6(16) . . ? C9A N1A Ni1 113.8(15) . 5_565 ? C11A N1A Ni1 107.2(12) . 5_565 ? C8 N1A Ni1 112.5(11) . 5_565 ? C12A C11A N1A 108.2(14) . . ? C12A N2A C13A 111.4(14) 5_565 . ? C12A N2A C14A 99.8(16) 5_565 . ? C13A N2A C14A 110.1(17) . . ? C12A N2A Ni1 99.5(14) 5_565 . ? C13A N2A Ni1 117.7(12) . . ? C14A N2A Ni1 116.1(11) . . ? N2A C12A C11A 112.9(18) 5_565 . ? C10B C9B N1B 122(2) . . ? C8 N1B C11B 110(2) . . ? C8 N1B C9B 111(2) . . ? C11B N1B C9B 111(2) . . ? C8 N1B Ni1 103.4(15) . 5_565 ? C11B N1B Ni1 109.9(17) . 5_565 ? C9B N1B Ni1 111.2(19) . 5_565 ? N1B C11B C12B 109.1(19) . . ? C14B N2B C12B 108(2) . 5_565 ? C14B N2B C13B 113(3) . . ? C12B N2B C13B 106(2) 5_565 . ? C14B N2B Ni1 109.0(17) . . ? C12B N2B Ni1 111.3(19) 5_565 . ? C13B N2B Ni1 109.8(15) . . ? C11B C12B N2B 112(2) . 5_565 ? C2 C15 O2A 131.1(13) . . ? C2 C15 O2B 137.7(14) . . ? O2A C15 O2B 22.2(6) . . ? C15 O2A Ni1 117.7(10) . . ? C15 O2B Ni1 109.9(11) . . ? O7A Cl1 O5B 153.6(17) . . ? O7A Cl1 O6 101.4(13) . . ? O5B Cl1 O6 95.4(15) . . ? O7A Cl1 O5A 115.1(13) . . ? O5B Cl1 O5A 53.8(14) . . ? O6 Cl1 O5A 142.8(10) . . ? O7A Cl1 O4B 39.6(11) . . ? O5B Cl1 O4B 142.4(18) . . ? O6 Cl1 O4B 117.9(12) . . ? O5A Cl1 O4B 88.7(13) . . ? O7A Cl1 O7B 64.2(13) . . ? O5B Cl1 O7B 93.0(16) . . ? O6 Cl1 O7B 100.3(9) . . ? O5A Cl1 O7B 101.4(10) . . ? O4B Cl1 O7B 97.3(12) . . ? O7A Cl1 O4A 99.4(15) . . ? O5B Cl1 O4A 103.8(17) . . ? O6 Cl1 O4A 78.7(11) . . ? O5A Cl1 O4A 88.5(13) . . ? O4B Cl1 O4A 69.1(12) . . ? O7B Cl1 O4A 163.2(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A Ni1 O1 C1 165(5) 5_565 . . . ? O2A Ni1 O1 C1 12.0(7) . . . . ? O1 Ni1 O1 C1 -154.8(8) 5_565 . . . ? N2A Ni1 O1 C1 105.8(8) . . . . ? N2B Ni1 O1 C1 95.6(9) . . . . ? O2B Ni1 O1 C1 -3.7(8) . . . . ? O3 Ni1 O1 C1 -67.8(7) . . . . ? N1B Ni1 O1 C1 -118(5) 5_565 . . . ? N1A Ni1 O1 Ni1 -40(5) 5_565 . . 5_565 ? O2A Ni1 O1 Ni1 166.8(4) . . . 5_565 ? O1 Ni1 O1 Ni1 0.0 5_565 . . 5_565 ? N2A Ni1 O1 Ni1 -99.4(5) . . . 5_565 ? N2B Ni1 O1 Ni1 -109.5(7) . . . 5_565 ? O2B Ni1 O1 Ni1 151.1(5) . . . 5_565 ? O3 Ni1 O1 Ni1 87.0(4) . . . 5_565 ? N1B Ni1 O1 Ni1 37(5) 5_565 . . 5_565 ? Ni1 O1 C1 C2 -143.3(8) 5_565 . . . ? Ni1 O1 C1 C2 5.2(13) . . . . ? Ni1 O1 C1 C6 35.1(11) 5_565 . . . ? Ni1 O1 C1 C6 -176.5(6) . . . . ? O1 C1 C2 C15 -13.0(17) . . . . ? C6 C1 C2 C15 168.6(11) . . . . ? O1 C1 C2 C3 174.7(9) . . . . ? C6 C1 C2 C3 -3.7(15) . . . . ? C15 C2 C3 C4 -170.9(11) . . . . ? C1 C2 C3 C4 2.2(17) . . . . ? C2 C3 C4 C5 -1.3(15) . . . . ? C2 C3 C4 C7A -170(4) . . . . ? C2 C3 C4 C7B 175(6) . . . . ? C3 C4 C5 C6 2.5(15) . . . . ? C7A C4 C5 C6 173(5) . . . . ? C7B C4 C5 C6 -174(6) . . . . ? O1 C1 C6 C5 -173.8(8) . . . . ? C2 C1 C6 C5 4.7(13) . . . . ? O1 C1 C6 C8 5.8(13) . . . . ? C2 C1 C6 C8 -175.7(9) . . . . ? C4 C5 C6 C1 -4.5(14) . . . . ? C4 C5 C6 C8 175.9(9) . . . . ? C1 C6 C8 N1B -62(2) . . . . ? C5 C6 C8 N1B 118(2) . . . . ? C1 C6 C8 N1A -56.0(14) . . . . ? C5 C6 C8 N1A 123.6(11) . . . . ? C10A C9A N1A C11A -59(2) . . . . ? C10A C9A N1A C8 57(2) . . . . ? C10A C9A N1A Ni1 179.4(18) . . . 5_565 ? N1B C8 N1A C9A -7(5) . . . . ? C6 C8 N1A C9A -173.2(13) . . . . ? N1B C8 N1A C11A 112(6) . . . . ? C6 C8 N1A C11A -54.8(16) . . . . ? N1B C8 N1A Ni1 -130(7) . . . 5_565 ? C6 C8 N1A Ni1 63.6(15) . . . 5_565 ? C9A N1A C11A C12A -94.3(19) . . . . ? C8 N1A C11A C12A 152.6(14) . . . . ? Ni1 N1A C11A C12A 30.8(18) 5_565 . . . ? N1A Ni1 N2A C12A 19.9(13) 5_565 . . 5_565 ? O2A Ni1 N2A C12A -77.9(11) . . . 5_565 ? O1 Ni1 N2A C12A 113.9(11) 5_565 . . 5_565 ? O1 Ni1 N2A C12A -166.4(11) . . . 5_565 ? N2B Ni1 N2A C12A -7(2) . . . 5_565 ? O2B Ni1 N2A C12A -75.2(11) . . . 5_565 ? O3 Ni1 N2A C12A -127(3) . . . 5_565 ? N1B Ni1 N2A C12A 20.0(13) 5_565 . . 5_565 ? N1A Ni1 N2A C13A -100.5(16) 5_565 . . . ? O2A Ni1 N2A C13A 161.7(15) . . . . ? O1 Ni1 N2A C13A -6.5(16) 5_565 . . . ? O1 Ni1 N2A C13A 73.2(15) . . . . ? N2B Ni1 N2A C13A -128(3) . . . . ? O2B Ni1 N2A C13A 164.4(14) . . . . ? O3 Ni1 N2A C13A 113(3) . . . . ? N1B Ni1 N2A C13A -100.4(17) 5_565 . . . ? N1A Ni1 N2A C14A 125.9(17) 5_565 . . . ? O2A Ni1 N2A C14A 28.1(16) . . . . ? O1 Ni1 N2A C14A -140.1(15) 5_565 . . . ? O1 Ni1 N2A C14A -60.5(15) . . . . ? N2B Ni1 N2A C14A 99(3) . . . . ? O2B Ni1 N2A C14A 30.8(17) . . . . ? O3 Ni1 N2A C14A -21(5) . . . . ? N1B Ni1 N2A C14A 126.0(17) 5_565 . . . ? N1A C11A C12A N2A -53(2) . . . 5_565 ? C6 C8 N1B C11B -65(3) . . . . ? N1A C8 N1B C11B -81(6) . . . . ? C6 C8 N1B C9B 171.7(16) . . . . ? N1A C8 N1B C9B 155(7) . . . . ? C6 C8 N1B Ni1 52(2) . . . 5_565 ? N1A C8 N1B Ni1 36(5) . . . 5_565 ? C10B C9B N1B C8 -60(4) . . . . ? C10B C9B N1B C11B 177(3) . . . . ? C10B C9B N1B Ni1 55(3) . . . 5_565 ? C8 N1B C11B C12B 142(2) . . . . ? C9B N1B C11B C12B -94(3) . . . . ? Ni1 N1B C11B C12B 29(3) 5_565 . . . ? N1A Ni1 N2B C14B 144(2) 5_565 . . . ? O2A Ni1 N2B C14B 43(2) . . . . ? O1 Ni1 N2B C14B -132(2) 5_565 . . . ? O1 Ni1 N2B C14B -44(2) . . . . ? N2A Ni1 N2B C14B -66(3) . . . . ? O2B Ni1 N2B C14B 52(2) . . . . ? O3 Ni1 N2B C14B 92(3) . . . . ? N1B Ni1 N2B C14B 141(2) 5_565 . . . ? N1A Ni1 N2B C12B 24.6(16) 5_565 . . 5_565 ? O2A Ni1 N2B C12B -76.3(16) . . . 5_565 ? O1 Ni1 N2B C12B 109.2(15) 5_565 . . 5_565 ? O1 Ni1 N2B C12B -163.0(14) . . . 5_565 ? N2A Ni1 N2B C12B 175(3) . . . 5_565 ? O2B Ni1 N2B C12B -67.1(16) . . . 5_565 ? O3 Ni1 N2B C12B -27(3) . . . 5_565 ? N1B Ni1 N2B C12B 22.2(17) 5_565 . . 5_565 ? N1A Ni1 N2B C13B -92(2) 5_565 . . . ? O2A Ni1 N2B C13B 167(2) . . . . ? O1 Ni1 N2B C13B -7(2) 5_565 . . . ? O1 Ni1 N2B C13B 80(2) . . . . ? N2A Ni1 N2B C13B 58(2) . . . . ? O2B Ni1 N2B C13B 176.2(19) . . . . ? O3 Ni1 N2B C13B -144.0(17) . . . . ? N1B Ni1 N2B C13B -95(2) 5_565 . . . ? N1B C11B C12B N2B -50(3) . . . 5_565 ? C1 C2 C15 O2A -5(2) . . . . ? C3 C2 C15 O2A 168.8(11) . . . . ? C1 C2 C15 O2B 25(2) . . . . ? C3 C2 C15 O2B -161.2(14) . . . . ? C2 C15 O2A Ni1 26.2(18) . . . . ? O2B C15 O2A Ni1 -91(3) . . . . ? N1A Ni1 O2A C15 160.4(10) 5_565 . . . ? O1 Ni1 O2A C15 28(2) 5_565 . . . ? O1 Ni1 O2A C15 -22.9(9) . . . . ? N2A Ni1 O2A C15 -108.4(10) . . . . ? N2B Ni1 O2A C15 -134.2(13) . . . . ? O2B Ni1 O2A C15 80.7(17) . . . . ? O3 Ni1 O2A C15 64.0(9) . . . . ? N1B Ni1 O2A C15 150.0(11) 5_565 . . . ? C2 C15 O2B Ni1 -23(2) . . . . ? O2A C15 O2B Ni1 61(3) . . . . ? N1A Ni1 O2B C15 -170.2(11) 5_565 . . . ? O2A Ni1 O2B C15 -68.3(13) . . . . ? O1 Ni1 O2B C15 83.6(12) 5_565 . . . ? O1 Ni1 O2B C15 8.3(10) . . . . ? N2A Ni1 O2B C15 -77.9(11) . . . . ? N2B Ni1 O2B C15 -103.3(13) . . . . ? O3 Ni1 O2B C15 93.5(11) . . . . ? N1B Ni1 O2B C15 180.0(12) 5_565 . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.164 _refine_diff_density_min -0.881 _refine_diff_density_rms 0.157 data_ifn3t _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H58 Cl2 N4 Ni2 O17' _chemical_formula_weight 947.13 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 10.3948(15) _cell_length_b 10.6991(15) _cell_length_c 10.8277(14) _cell_angle_alpha 73.874(3) _cell_angle_beta 85.768(3) _cell_angle_gamma 62.618(2) _cell_volume 1025.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 102 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 23.38 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 498 _exptl_absorpt_coefficient_mu 1.124 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8770 _exptl_absorpt_correction_T_max 0.9779 _exptl_absorpt_process_details ? _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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '/w scans with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4539 _diffrn_reflns_av_R_equivalents 0.0953 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 23.38 _reflns_number_total 2938 _reflns_number_gt 2235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXTL-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^)+(0.2000P)^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 2938 _refine_ls_number_parameters 273 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0892 _refine_ls_wR_factor_ref 0.2946 _refine_ls_wR_factor_gt 0.2436 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_restrained_S_all 1.200 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.4584(5) 0.1063(5) 0.5553(5) 0.0491(13) Uani 1 1 d . . . Ni1 Ni 0.35103(8) -0.00101(9) 0.52184(9) 0.0487(5) Uani 1 1 d . . . C1 C 0.4172(7) 0.2127(7) 0.6091(7) 0.0466(18) Uani 1 1 d . . . C2 C 0.5038(7) 0.2891(7) 0.6045(7) 0.0446(17) Uani 1 1 d . . . C3 C 0.4530(8) 0.4084(8) 0.6582(8) 0.0512(19) Uani 1 1 d . . . H3 H 0.5079 0.4579 0.6524 0.061 Uiso 1 1 calc R . . C4 C 0.3246(8) 0.4537(8) 0.7188(8) 0.053(2) Uani 1 1 d . . . C5 C 0.2774(8) 0.5780(8) 0.7823(9) 0.065(2) Uani 1 1 d . . . H5A H 0.2284 0.6704 0.7186 0.098 Uiso 1 1 calc R . . H5B H 0.3613 0.5727 0.8197 0.098 Uiso 1 1 calc R . . H5C H 0.2128 0.5690 0.8483 0.098 Uiso 1 1 calc R . . C6 C 0.2495(8) 0.3747(8) 0.7287(8) 0.054(2) Uani 1 1 d . . . H6 H 0.1653 0.4018 0.7732 0.065 Uiso 1 1 calc R . . C7 C 0.2893(7) 0.2563(8) 0.6771(8) 0.0484(18) Uani 1 1 d . . . C8 C 0.2059(8) 0.1699(8) 0.7092(8) 0.054(2) Uani 1 1 d . . . H8A H 0.2630 0.0798 0.7747 0.065 Uiso 1 1 calc R . . H8B H 0.1174 0.2251 0.7469 0.065 Uiso 1 1 calc R . . N1 N 0.1656(7) 0.1310(7) 0.6009(7) 0.0563(17) Uani 1 1 d . . . C9 C 0.0767(8) 0.0545(10) 0.6534(10) 0.068(2) Uani 1 1 d . . . H9A H -0.0096 0.1190 0.6857 0.101 Uiso 1 1 calc R . . H9B H 0.1318 -0.0311 0.7220 0.101 Uiso 1 1 calc R . . H9C H 0.0504 0.0261 0.5863 0.101 Uiso 1 1 calc R . . C10 C 0.0814(8) 0.2659(8) 0.4957(8) 0.058(2) Uani 1 1 d . . . H10A H 0.1198 0.3347 0.4880 0.070 Uiso 1 1 calc R . . H10B H -0.0192 0.3117 0.5168 0.070 Uiso 1 1 calc R . . C11 C 0.0892(8) 0.2306(8) 0.3695(9) 0.062(2) Uani 1 1 d . . . H11A H 0.0432 0.1687 0.3733 0.075 Uiso 1 1 calc R . . H11B H 0.0401 0.3198 0.3005 0.075 Uiso 1 1 calc R . . N2 N 0.2470(6) 0.1524(7) 0.3464(6) 0.0545(17) Uani 1 1 d . . . H2 H 0.2812 0.2196 0.3296 0.065 Uiso 1 1 calc R . . C12 C 0.2687(9) 0.0978(9) 0.2313(8) 0.065(2) Uani 1 1 d . . . H12A H 0.2291 0.0290 0.2454 0.078 Uiso 1 1 calc R . . H12B H 0.3722 0.0443 0.2231 0.078 Uiso 1 1 calc R . . C13 C 0.1996(12) 0.2163(12) 0.1017(10) 0.090(3) Uani 1 1 d . . . H13A H 0.0972 0.2717 0.1085 0.135 Uiso 1 1 calc R . . H13B H 0.2153 0.1698 0.0340 0.135 Uiso 1 1 calc R . . H13C H 0.2435 0.2807 0.0824 0.135 Uiso 1 1 calc R . . C14 C 0.6441(8) 0.2451(8) 0.5527(8) 0.054(2) Uani 1 1 d . . . H14 H 0.6860 0.3056 0.5522 0.065 Uiso 1 1 calc R . . O2 O 0.7181(5) 0.1412(5) 0.5089(5) 0.0515(13) Uani 1 1 d . . . O3 O 0.4463(6) -0.1622(6) 0.7016(6) 0.0605(15) Uani 1 1 d . . . Cl1 Cl -0.2342(2) 0.4534(2) 0.7912(2) 0.0624(7) Uani 1 1 d . . . O4 O -0.3376(9) 0.4755(9) 0.8907(8) 0.111(3) Uani 1 1 d . A . O5 O -0.3074(9) 0.5681(8) 0.6809(7) 0.095(2) Uani 1 1 d . A . O6A O -0.1110(14) 0.4505(15) 0.839(3) 0.093(5) Uani 0.82(7) 1 d PU A 1 O6B O -0.105(6) 0.454(7) 0.770(13) 0.080(15) Uani 0.18(7) 1 d PU A 2 O7 O -0.2035(6) 0.3166(6) 0.7672(7) 0.0755(18) Uani 1 1 d . A . C1S C 0.4227(17) -0.185(2) 1.0260(13) 0.134(6) Uani 1 1 d . . . H1S1 H 0.3699 -0.0956 1.0504 0.200 Uiso 1 1 calc R . . H1S2 H 0.5121 -0.1899 0.9914 0.200 Uiso 1 1 calc R . . H1S3 H 0.4433 -0.2669 1.1002 0.200 Uiso 1 1 calc R . . O1S O 0.3429(10) -0.1886(11) 0.9368(8) 0.125(4) Uani 1 1 d . . . H1S H 0.3701 -0.1643 0.8652 0.188 Uiso 1 1 calc R . . C2S C 0.0000 0.0000 1.0000 0.195(14) Uani 1 2 d SU . . O2S O 0.106(4) -0.157(3) 0.945(6) 0.33(3) Uani 0.50 1 d PU . . 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 O1 0.025(2) 0.042(3) 0.086(3) -0.035(3) -0.005(2) -0.009(2) Ni1 0.0230(6) 0.0330(7) 0.0937(9) -0.0310(5) -0.0091(5) -0.0064(5) C1 0.023(3) 0.031(4) 0.082(5) -0.029(3) -0.014(3) 0.000(3) C2 0.029(4) 0.034(4) 0.076(5) -0.024(3) -0.013(3) -0.012(3) C3 0.036(4) 0.035(4) 0.087(5) -0.024(3) -0.018(4) -0.013(3) C4 0.029(4) 0.038(4) 0.094(6) -0.033(4) -0.013(4) -0.005(3) C5 0.035(4) 0.041(4) 0.122(7) -0.044(4) -0.014(4) -0.004(4) C6 0.029(4) 0.049(4) 0.083(5) -0.031(4) -0.007(3) -0.007(3) C7 0.020(3) 0.036(4) 0.093(5) -0.029(3) -0.012(3) -0.007(3) C8 0.028(4) 0.039(4) 0.099(6) -0.034(4) -0.008(4) -0.008(3) N1 0.031(3) 0.037(3) 0.104(5) -0.034(3) -0.006(3) -0.009(3) C9 0.033(4) 0.062(5) 0.132(7) -0.067(5) 0.006(4) -0.020(4) C10 0.030(4) 0.045(4) 0.099(6) -0.036(4) -0.010(4) -0.005(3) C11 0.036(4) 0.035(4) 0.107(6) -0.021(4) -0.022(4) -0.004(3) N2 0.027(3) 0.043(3) 0.091(5) -0.023(3) -0.016(3) -0.010(3) C12 0.048(5) 0.052(5) 0.091(6) -0.028(4) -0.020(4) -0.010(4) C13 0.085(8) 0.070(7) 0.100(7) -0.027(5) -0.021(6) -0.017(6) C14 0.032(4) 0.039(4) 0.095(6) -0.022(4) -0.014(4) -0.014(3) O2 0.030(3) 0.038(3) 0.094(4) -0.034(3) -0.004(2) -0.012(2) O3 0.038(3) 0.039(3) 0.101(4) -0.021(3) -0.014(3) -0.010(2) Cl1 0.0377(11) 0.0426(11) 0.1035(16) -0.0334(10) -0.0131(10) -0.0058(9) O4 0.088(6) 0.108(6) 0.147(7) -0.084(6) 0.031(5) -0.032(5) O5 0.090(5) 0.062(4) 0.120(6) -0.028(4) -0.026(4) -0.018(4) O6A 0.034(5) 0.096(7) 0.156(16) -0.080(8) -0.025(7) -0.006(4) O6B 0.044(19) 0.07(2) 0.17(4) -0.09(3) 0.00(3) -0.028(16) O7 0.052(4) 0.043(3) 0.130(5) -0.043(3) -0.011(3) -0.007(3) C1S 0.122(12) 0.170(15) 0.106(9) -0.005(9) -0.039(8) -0.076(11) O1S 0.095(6) 0.144(8) 0.095(5) -0.055(5) 0.000(5) -0.008(6) C2S 0.13(2) 0.21(3) 0.138(18) -0.030(18) -0.006(15) 0.00(2) O2S 0.15(3) 0.12(2) 0.71(9) -0.18(3) -0.19(4) 0.018(18) _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 O1 C1 1.305(8) . ? O1 Ni1 2.028(5) 2_656 ? O1 Ni1 2.041(5) . ? Ni1 O1 2.028(5) 2_656 ? Ni1 O2 2.045(5) 2_656 ? Ni1 N1 2.090(6) . ? Ni1 N2 2.100(6) . ? Ni1 O3 2.143(5) . ? C1 C7 1.416(11) . ? C1 C2 1.458(10) . ? C2 C3 1.411(10) . ? C2 C14 1.434(11) . ? C3 C4 1.379(11) . ? C4 C6 1.371(11) . ? C4 C5 1.530(11) . ? C6 C7 1.401(11) . ? C7 C8 1.497(11) . ? C8 N1 1.492(10) . ? N1 C9 1.486(11) . ? N1 C10 1.489(11) . ? C10 C11 1.503(12) . ? C11 N2 1.499(10) . ? N2 C12 1.479(11) . ? C12 C13 1.554(13) . ? C14 O2 1.227(9) . ? O2 Ni1 2.045(5) 2_656 ? Cl1 O6B 1.35(6) . ? Cl1 O6A 1.401(14) . ? Cl1 O5 1.404(7) . ? Cl1 O7 1.443(6) . ? Cl1 O4 1.452(8) . ? C1S O1S 1.338(15) . ? C2S O2S 1.77(3) . ? C2S O2S 1.77(3) 2_557 ? 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 C1 O1 Ni1 129.8(5) . 2_656 ? C1 O1 Ni1 130.7(5) . . ? Ni1 O1 Ni1 99.6(2) 2_656 . ? O1 Ni1 O1 80.4(2) 2_656 . ? O1 Ni1 O2 90.0(2) 2_656 2_656 ? O1 Ni1 O2 169.12(19) . 2_656 ? O1 Ni1 N1 171.2(2) 2_656 . ? O1 Ni1 N1 91.0(2) . . ? O2 Ni1 N1 98.6(2) 2_656 . ? O1 Ni1 N2 94.6(2) 2_656 . ? O1 Ni1 N2 94.9(2) . . ? O2 Ni1 N2 91.1(2) 2_656 . ? N1 Ni1 N2 83.9(3) . . ? O1 Ni1 O3 87.2(2) 2_656 . ? O1 Ni1 O3 88.7(2) . . ? O2 Ni1 O3 85.6(2) 2_656 . ? N1 Ni1 O3 94.7(2) . . ? N2 Ni1 O3 176.2(2) . . ? O1 C1 C7 121.6(6) . . ? O1 C1 C2 121.1(6) . . ? C7 C1 C2 117.2(6) . . ? C3 C2 C14 116.9(6) . . ? C3 C2 C1 119.8(6) . . ? C14 C2 C1 123.2(6) . . ? C4 C3 C2 122.0(7) . . ? C6 C4 C3 117.0(7) . . ? C6 C4 C5 122.3(7) . . ? C3 C4 C5 120.5(7) . . ? C4 C6 C7 125.3(7) . . ? C6 C7 C1 118.4(7) . . ? C6 C7 C8 118.9(7) . . ? C1 C7 C8 122.3(6) . . ? N1 C8 C7 116.8(7) . . ? C9 N1 C10 110.5(6) . . ? C9 N1 C8 107.3(7) . . ? C10 N1 C8 110.1(6) . . ? C9 N1 Ni1 111.2(5) . . ? C10 N1 Ni1 106.9(5) . . ? C8 N1 Ni1 110.8(4) . . ? N1 C10 C11 111.0(6) . . ? N2 C11 C10 106.8(6) . . ? C12 N2 C11 111.6(6) . . ? C12 N2 Ni1 117.5(5) . . ? C11 N2 Ni1 106.6(5) . . ? N2 C12 C13 115.9(7) . . ? O2 C14 C2 130.9(7) . . ? C14 O2 Ni1 124.3(5) . 2_656 ? O6B Cl1 O6A 31(5) . . ? O6B Cl1 O5 95(5) . . ? O6A Cl1 O5 115.7(10) . . ? O6B Cl1 O7 101(2) . . ? O6A Cl1 O7 112.3(7) . . ? O5 Cl1 O7 108.8(4) . . ? O6B Cl1 O4 137(5) . . ? O6A Cl1 O4 106.7(14) . . ? O5 Cl1 O4 105.5(5) . . ? O7 Cl1 O4 107.2(5) . . ? O2S C2S O2S 180(3) . 2_557 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 O1 Ni1 O1 179.3(8) . . . 2_656 ? Ni1 O1 Ni1 O1 0.0 2_656 . . 2_656 ? C1 O1 Ni1 O2 -151.5(10) . . . 2_656 ? Ni1 O1 Ni1 O2 29.2(12) 2_656 . . 2_656 ? C1 O1 Ni1 N1 1.4(7) . . . . ? Ni1 O1 Ni1 N1 -177.9(2) 2_656 . . . ? C1 O1 Ni1 N2 85.4(6) . . . . ? Ni1 O1 Ni1 N2 -93.9(3) 2_656 . . . ? C1 O1 Ni1 O3 -93.3(6) . . . . ? Ni1 O1 Ni1 O3 87.4(2) 2_656 . . . ? Ni1 O1 C1 C7 -169.2(5) 2_656 . . . ? Ni1 O1 C1 C7 11.7(11) . . . . ? Ni1 O1 C1 C2 9.1(10) 2_656 . . . ? Ni1 O1 C1 C2 -170.0(5) . . . . ? O1 C1 C2 C3 177.0(6) . . . . ? C7 C1 C2 C3 -4.7(10) . . . . ? O1 C1 C2 C14 -6.0(11) . . . . ? C7 C1 C2 C14 172.3(7) . . . . ? C14 C2 C3 C4 -175.3(7) . . . . ? C1 C2 C3 C4 1.9(11) . . . . ? C2 C3 C4 C6 2.0(11) . . . . ? C2 C3 C4 C5 176.6(7) . . . . ? C3 C4 C6 C7 -3.1(12) . . . . ? C5 C4 C6 C7 -177.6(7) . . . . ? C4 C6 C7 C1 0.2(12) . . . . ? C4 C6 C7 C8 172.8(7) . . . . ? O1 C1 C7 C6 -178.0(7) . . . . ? C2 C1 C7 C6 3.7(10) . . . . ? O1 C1 C7 C8 9.6(11) . . . . ? C2 C1 C7 C8 -168.7(7) . . . . ? C6 C7 C8 N1 136.0(7) . . . . ? C1 C7 C8 N1 -51.6(9) . . . . ? C7 C8 N1 C9 -176.5(6) . . . . ? C7 C8 N1 C10 -56.2(8) . . . . ? C7 C8 N1 Ni1 61.9(7) . . . . ? O1 Ni1 N1 C9 -167.5(13) 2_656 . . . ? O1 Ni1 N1 C9 -153.7(6) . . . . ? O2 Ni1 N1 C9 21.3(6) 2_656 . . . ? N2 Ni1 N1 C9 111.5(6) . . . . ? O3 Ni1 N1 C9 -65.0(6) . . . . ? O1 Ni1 N1 C10 71.8(16) 2_656 . . . ? O1 Ni1 N1 C10 85.6(5) . . . . ? O2 Ni1 N1 C10 -99.4(5) 2_656 . . . ? N2 Ni1 N1 C10 -9.2(5) . . . . ? O3 Ni1 N1 C10 174.3(5) . . . . ? O1 Ni1 N1 C8 -48.2(17) 2_656 . . . ? O1 Ni1 N1 C8 -34.5(5) . . . . ? O2 Ni1 N1 C8 140.5(5) 2_656 . . . ? N2 Ni1 N1 C8 -129.3(5) . . . . ? O3 Ni1 N1 C8 54.3(5) . . . . ? C9 N1 C10 C11 -83.7(8) . . . . ? C8 N1 C10 C11 157.9(7) . . . . ? Ni1 N1 C10 C11 37.5(7) . . . . ? N1 C10 C11 N2 -55.8(8) . . . . ? C10 C11 N2 C12 173.8(7) . . . . ? C10 C11 N2 Ni1 44.3(7) . . . . ? O1 Ni1 N2 C12 43.1(6) 2_656 . . . ? O1 Ni1 N2 C12 123.8(6) . . . . ? O2 Ni1 N2 C12 -47.1(6) 2_656 . . . ? N1 Ni1 N2 C12 -145.6(6) . . . . ? O3 Ni1 N2 C12 -76(3) . . . . ? O1 Ni1 N2 C11 169.2(5) 2_656 . . . ? O1 Ni1 N2 C11 -110.1(5) . . . . ? O2 Ni1 N2 C11 79.0(5) 2_656 . . . ? N1 Ni1 N2 C11 -19.5(5) . . . . ? O3 Ni1 N2 C11 50(3) . . . . ? C11 N2 C12 C13 60.8(10) . . . . ? Ni1 N2 C12 C13 -175.6(7) . . . . ? C3 C2 C14 O2 174.5(8) . . . . ? C1 C2 C14 O2 -2.6(13) . . . . ? C2 C14 O2 Ni1 6.9(12) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 23.38 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.916 _refine_diff_density_min -0.991 _refine_diff_density_rms 0.188