# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author 'Shu Hua Zhang ' _publ_contact_author_email zsh720108@163.com _publ_contact_author_name 'Shu Hua Zhang' loop_ _publ_author_name 'Ning Li' 'Shu Hua Zhang' 'Ning Li' 'Cheng Min Ge' 'Chao Feng' ; Lu-Fang Ma ; data_771961 _database_code_depnum_ccdc_archive 'CCDC 771961' #TrackingRef 'content .cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H42 N8 Na2 Ni2 O14 ' _chemical_formula_sum 'C38 H42 N8 Na2 Ni2 O14' _chemical_formula_weight 998.20 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' Na Na 0.0362 0.0249 '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 ' _symmetry_space_group_name_Hall '-P 2yn' 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 10.867(2) _cell_length_b 10.846(2) _cell_length_c 19.070(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.15(3) _cell_angle_gamma 90.00 _cell_volume 2188.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3787 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 25.10 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.955 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11326 _diffrn_reflns_av_R_equivalents 0.0937 _diffrn_reflns_av_sigmaI/netI 0.0996 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.10 _reflns_number_total 3877 _reflns_number_gt 2184 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART(Bruker 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _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^)+(0.0012P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3877 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.55245(5) 0.56751(4) 0.93700(2) 0.04596(16) Uani 1 1 d . . . Na1 Na 0.33904(14) 0.32847(13) 0.88685(7) 0.0572(4) Uani 1 1 d . . . C1 C 0.5671(4) 0.4037(3) 0.8162(2) 0.0447(10) Uani 1 1 d . . . C2 C 0.6750(4) 0.4625(4) 0.8033(2) 0.0547(11) Uani 1 1 d . . . C3 C 0.7182(5) 0.4391(4) 0.7407(3) 0.0783(14) Uani 1 1 d . . . H3 H 0.7911 0.4779 0.7342 0.094 Uiso 1 1 calc R . . C4 C 0.6558(5) 0.3616(5) 0.6899(3) 0.0811(15) Uani 1 1 d . . . H4 H 0.6840 0.3483 0.6480 0.097 Uiso 1 1 calc R . . C5 C 0.5489(5) 0.3017(4) 0.7006(2) 0.0688(13) Uani 1 1 d . . . H5 H 0.5058 0.2475 0.6658 0.083 Uiso 1 1 calc R . . C6 C 0.5068(4) 0.3213(4) 0.7610(2) 0.0516(10) Uani 1 1 d . . . C7 C 0.3340(4) 0.1810(4) 0.7244(2) 0.0887(15) Uani 1 1 d . . . H7A H 0.2996 0.2246 0.6805 0.133 Uiso 1 1 calc R . . H7B H 0.2665 0.1442 0.7420 0.133 Uiso 1 1 calc R . . H7C H 0.3901 0.1176 0.7153 0.133 Uiso 1 1 calc R . . C8 C 0.7469(4) 0.5441(4) 0.8538(2) 0.0705(13) Uani 1 1 d . . . H8 H 0.8215 0.5720 0.8431 0.085 Uiso 1 1 calc R . . C9 C 0.6003(4) 0.8317(4) 0.9689(2) 0.0483(10) Uani 1 1 d . . . C10 C 0.5416(4) 0.8668(4) 0.8985(2) 0.0541(11) Uani 1 1 d . . . C11 C 0.5455(4) 0.9915(5) 0.8768(3) 0.0764(15) Uani 1 1 d . . . H11 H 0.5053 1.0141 0.8302 0.092 Uiso 1 1 calc R . . C12 C 0.6059(5) 1.0771(4) 0.9221(3) 0.0815(16) Uani 1 1 d . . . H12 H 0.6059 1.1588 0.9072 0.098 Uiso 1 1 calc R . . C13 C 0.6686(4) 1.0447(4) 0.9916(3) 0.0773(14) Uani 1 1 d . . . H13 H 0.7124 1.1044 1.0225 0.093 Uiso 1 1 calc R . . C14 C 0.6665(4) 0.9256(4) 1.0147(2) 0.0570(11) Uani 1 1 d . . . C15 C 0.8042(4) 0.9711(4) 1.1290(2) 0.0942(16) Uani 1 1 d . . . H15A H 0.8659 1.0040 1.1051 0.141 Uiso 1 1 calc R . . H15B H 0.8463 0.9302 1.1724 0.141 Uiso 1 1 calc R . . H15C H 0.7533 1.0370 1.1405 0.141 Uiso 1 1 calc R . . C16 C 0.4780(4) 0.7832(4) 0.8473(2) 0.0670(13) Uani 1 1 d . . . H16 H 0.4365 0.8183 0.8038 0.080 Uiso 1 1 calc R . . C17 C 0.0283(6) 0.3043(5) 0.8367(3) 0.1017(18) Uani 1 1 d . . . H17 H -0.0221 0.2768 0.7934 0.122 Uiso 1 1 calc R . . C18 C 0.0574(5) 0.3273(6) 0.9627(3) 0.148(3) Uani 1 1 d . . . H18A H 0.0795 0.2600 0.9958 0.221 Uiso 1 1 calc R . . H18B H 0.0062 0.3853 0.9814 0.221 Uiso 1 1 calc R . . H18C H 0.1330 0.3674 0.9565 0.221 Uiso 1 1 calc R . . C19 C -0.1233(5) 0.2105(5) 0.8917(3) 0.132(2) Uani 1 1 d . . . H19A H -0.1516 0.1767 0.8442 0.198 Uiso 1 1 calc R . . H19B H -0.1882 0.2622 0.9026 0.198 Uiso 1 1 calc R . . H19C H -0.1053 0.1446 0.9262 0.198 Uiso 1 1 calc R . . N1 N 0.3812(3) 0.5317(3) 0.96782(16) 0.0462(8) Uani 1 1 d . . . N2 N 0.2961(4) 0.6022(3) 0.96148(17) 0.0513(9) Uani 1 1 d . . . N3 N 0.2125(4) 0.6709(3) 0.9551(2) 0.0794(12) Uani 1 1 d . . . N4 N -0.0116(4) 0.2817(4) 0.8949(2) 0.0820(12) Uani 1 1 d . . . O1 O 0.5226(2) 0.4185(2) 0.87256(12) 0.0517(7) Uani 1 1 d . . . O2 O 0.4016(3) 0.2643(2) 0.77655(14) 0.0648(8) Uani 1 1 d . . . O3 O 0.7252(3) 0.5840(2) 0.91025(16) 0.0675(8) Uani 1 1 d . . . O4 O 0.5958(2) 0.7215(2) 0.99502(12) 0.0523(7) Uani 1 1 d . . . O5 O 0.4680(3) 0.6703(3) 0.85037(13) 0.0638(8) Uani 1 1 d . . . O6 O 0.7256(3) 0.8851(2) 1.08260(17) 0.0672(8) Uani 1 1 d . . . O7 O 0.1265(3) 0.3585(3) 0.83362(18) 0.0926(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0482(3) 0.0448(3) 0.0437(3) 0.0008(3) 0.0080(2) -0.0059(3) Na1 0.0550(10) 0.0612(10) 0.0540(9) -0.0038(8) 0.0095(8) -0.0130(8) C1 0.047(3) 0.042(2) 0.046(2) 0.004(2) 0.013(2) 0.006(2) C2 0.059(3) 0.056(3) 0.052(3) -0.007(2) 0.018(2) -0.003(2) C3 0.075(4) 0.086(4) 0.085(4) 0.005(3) 0.041(3) 0.001(3) C4 0.097(4) 0.092(4) 0.065(3) -0.007(3) 0.041(3) 0.004(3) C5 0.078(4) 0.070(3) 0.059(3) -0.015(2) 0.015(3) 0.010(3) C6 0.050(3) 0.055(3) 0.050(3) -0.001(2) 0.010(2) 0.004(2) C7 0.092(4) 0.094(4) 0.070(3) -0.018(3) -0.001(3) -0.019(3) C8 0.069(3) 0.074(3) 0.078(3) 0.013(3) 0.034(3) -0.003(3) C9 0.042(3) 0.046(3) 0.063(3) 0.002(2) 0.024(2) 0.001(2) C10 0.054(3) 0.052(3) 0.061(3) 0.011(2) 0.022(3) 0.002(2) C11 0.069(4) 0.069(3) 0.102(4) 0.025(3) 0.043(3) 0.009(3) C12 0.072(4) 0.048(3) 0.138(5) 0.031(3) 0.054(4) 0.008(3) C13 0.066(3) 0.047(3) 0.127(5) -0.005(3) 0.039(4) -0.011(2) C14 0.050(3) 0.042(3) 0.083(3) 0.001(3) 0.024(3) -0.004(2) C15 0.086(4) 0.071(3) 0.118(4) -0.034(3) 0.008(3) -0.020(3) C16 0.067(3) 0.079(3) 0.059(3) 0.020(3) 0.021(3) 0.012(3) C17 0.086(5) 0.131(5) 0.079(4) -0.005(4) 0.002(4) 0.009(4) C18 0.101(5) 0.247(8) 0.089(4) -0.054(5) 0.010(4) -0.013(5) C19 0.105(5) 0.129(5) 0.170(6) -0.029(5) 0.045(5) -0.056(4) N1 0.046(2) 0.0440(19) 0.049(2) -0.0017(16) 0.0129(18) 0.0049(16) N2 0.067(3) 0.047(2) 0.042(2) 0.0022(18) 0.016(2) -0.0080(19) N3 0.092(3) 0.068(3) 0.082(3) 0.009(2) 0.026(3) 0.024(2) N4 0.070(3) 0.115(3) 0.066(3) -0.017(3) 0.025(3) -0.011(3) O1 0.0594(18) 0.0582(17) 0.0403(15) -0.0083(13) 0.0171(14) -0.0112(14) O2 0.068(2) 0.067(2) 0.0561(18) -0.0175(15) 0.0060(17) -0.0042(16) O3 0.065(2) 0.069(2) 0.0707(19) -0.0051(17) 0.0206(18) -0.0202(16) O4 0.0642(19) 0.0383(15) 0.0529(16) 0.0026(13) 0.0104(15) -0.0080(14) O5 0.076(2) 0.0630(19) 0.0496(17) 0.0063(16) 0.0078(16) -0.0009(17) O6 0.065(2) 0.0506(18) 0.083(2) -0.0147(17) 0.0101(19) -0.0137(15) O7 0.054(2) 0.119(3) 0.099(3) 0.010(2) 0.006(2) -0.019(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 O4 2.000(2) . ? Ni1 O1 2.011(2) . ? Ni1 O5 2.031(3) . ? Ni1 O3 2.062(3) . ? Ni1 N1 2.092(3) 3_667 ? Ni1 N1 2.112(3) . ? Ni1 Na1 3.4848(17) 3_667 ? Na1 O4 2.268(3) 3_667 ? Na1 O1 2.292(3) . ? Na1 O7 2.325(4) . ? Na1 O2 2.454(3) . ? Na1 O6 2.527(3) 3_667 ? Na1 Ni1 3.4848(17) 3_667 ? C1 O1 1.286(4) . ? C1 C2 1.405(5) . ? C1 C6 1.422(5) . ? C2 C3 1.402(5) . ? C2 C8 1.407(6) . ? C3 C4 1.344(6) . ? C3 H3 0.9300 . ? C4 C5 1.386(6) . ? C4 H4 0.9300 . ? C5 C6 1.349(5) . ? C5 H5 0.9300 . ? C6 O2 1.389(4) . ? C7 O2 1.419(4) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 O3 1.231(4) . ? C8 H8 0.9300 . ? C9 O4 1.301(4) . ? C9 C10 1.402(5) . ? C9 C14 1.425(5) . ? C10 C16 1.395(5) . ? C10 C11 1.417(5) . ? C11 C12 1.334(6) . ? C11 H11 0.9300 . ? C12 C13 1.390(6) . ? C12 H12 0.9300 . ? C13 C14 1.367(5) . ? C13 H13 0.9300 . ? C14 O6 1.379(5) . ? C15 O6 1.427(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 O5 1.232(4) . ? C16 H16 0.9300 . ? C17 O7 1.231(6) . ? C17 N4 1.305(6) . ? C17 H17 0.9300 . ? C18 N4 1.427(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N4 1.429(5) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? N1 N2 1.184(4) . ? N1 Ni1 2.092(3) 3_667 ? N2 N3 1.160(4) . ? O4 Na1 2.268(3) 3_667 ? O6 Na1 2.527(3) 3_667 ? 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 O4 Ni1 O1 173.78(9) . . ? O4 Ni1 O5 89.86(11) . . ? O1 Ni1 O5 87.93(11) . . ? O4 Ni1 O3 87.23(10) . . ? O1 Ni1 O3 87.01(10) . . ? O5 Ni1 O3 91.13(11) . . ? O4 Ni1 N1 87.60(11) . 3_667 ? O1 Ni1 N1 95.32(11) . 3_667 ? O5 Ni1 N1 172.25(11) . 3_667 ? O3 Ni1 N1 96.06(12) . 3_667 ? O4 Ni1 N1 96.38(10) . . ? O1 Ni1 N1 89.56(11) . . ? O5 Ni1 N1 93.64(12) . . ? O3 Ni1 N1 174.02(12) . . ? N1 Ni1 N1 79.37(14) 3_667 . ? O4 Ni1 Na1 37.89(7) . 3_667 ? O1 Ni1 Na1 145.21(7) . 3_667 ? O5 Ni1 Na1 126.69(8) . 3_667 ? O3 Ni1 Na1 94.76(9) . 3_667 ? N1 Ni1 Na1 49.90(9) 3_667 3_667 ? N1 Ni1 Na1 85.28(9) . 3_667 ? O4 Na1 O1 97.84(11) 3_667 . ? O4 Na1 O7 121.46(12) 3_667 . ? O1 Na1 O7 133.91(12) . . ? O4 Na1 O2 134.33(11) 3_667 . ? O1 Na1 O2 66.46(10) . . ? O7 Na1 O2 96.14(12) . . ? O4 Na1 O6 65.94(10) 3_667 3_667 ? O1 Na1 O6 135.49(11) . 3_667 ? O7 Na1 O6 85.88(12) . 3_667 ? O2 Na1 O6 94.78(10) . 3_667 ? O4 Na1 Ni1 32.79(6) 3_667 3_667 ? O1 Na1 Ni1 82.18(7) . 3_667 ? O7 Na1 Ni1 117.40(10) . 3_667 ? O2 Na1 Ni1 144.99(9) . 3_667 ? O6 Na1 Ni1 97.21(8) 3_667 3_667 ? O1 C1 C2 125.3(4) . . ? O1 C1 C6 120.0(4) . . ? C2 C1 C6 114.8(3) . . ? C3 C2 C1 121.4(4) . . ? C3 C2 C8 117.2(4) . . ? C1 C2 C8 121.4(4) . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 O2 124.6(4) . . ? C5 C6 C1 122.8(4) . . ? O2 C6 C1 112.6(3) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C2 129.2(4) . . ? O3 C8 H8 115.4 . . ? C2 C8 H8 115.4 . . ? O4 C9 C10 124.6(4) . . ? O4 C9 C14 118.6(4) . . ? C10 C9 C14 116.7(4) . . ? C16 C10 C9 122.6(4) . . ? C16 C10 C11 117.4(4) . . ? C9 C10 C11 120.0(4) . . ? C12 C11 C10 121.3(5) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 120.2(5) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 120.4(5) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 O6 124.4(4) . . ? C13 C14 C9 121.3(4) . . ? O6 C14 C9 114.2(4) . . ? O6 C15 H15A 109.5 . . ? O6 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O6 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O5 C16 C10 130.4(4) . . ? O5 C16 H16 114.8 . . ? C10 C16 H16 114.8 . . ? O7 C17 N4 126.1(6) . . ? O7 C17 H17 116.9 . . ? N4 C17 H17 116.9 . . ? N4 C18 H18A 109.5 . . ? N4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N4 C19 H19A 109.5 . . ? N4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 N1 Ni1 121.9(3) . 3_667 ? N2 N1 Ni1 124.7(3) . . ? Ni1 N1 Ni1 100.63(14) 3_667 . ? N3 N2 N1 179.7(5) . . ? C17 N4 C18 119.9(5) . . ? C17 N4 C19 120.6(5) . . ? C18 N4 C19 119.5(4) . . ? C1 O1 Ni1 124.9(2) . . ? C1 O1 Na1 123.3(2) . . ? Ni1 O1 Na1 107.07(11) . . ? C6 O2 C7 116.9(3) . . ? C6 O2 Na1 117.3(2) . . ? C7 O2 Na1 125.6(2) . . ? C8 O3 Ni1 123.5(3) . . ? C9 O4 Ni1 125.5(2) . . ? C9 O4 Na1 124.7(2) . 3_667 ? Ni1 O4 Na1 109.32(11) . 3_667 ? C16 O5 Ni1 123.8(3) . . ? C14 O6 C15 117.3(3) . . ? C14 O6 Na1 114.4(2) . 3_667 ? C15 O6 Na1 127.9(3) . 3_667 ? C17 O7 Na1 134.3(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.410 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.057 #=============================================================== data_771963 _database_code_depnum_ccdc_archive 'CCDC 771963' #TrackingRef 'content .cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41.05 H58.10 Ni4 O20' _chemical_formula_sum 'C41.05 H58.10 Ni4 O20' _chemical_formula_weight 1106.36 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' O O 0.0106 0.0060 '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 Tetragonal _symmetry_space_group_name_H-M P4/ncc _symmetry_space_group_name_Hall '-P 4a 2ac ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 16.780(3) _cell_length_b 16.780(3) _cell_length_c 18.814(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5297(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1934 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 23.35 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2305.7 _exptl_absorpt_coefficient_mu 1.468 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area apex II detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean no _diffrn_standards_number no _diffrn_standards_interval_count no _diffrn_standards_interval_time no _diffrn_standards_decay_% no _diffrn_reflns_number 30187 _diffrn_reflns_av_R_equivalents 0.1102 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 23.35 _reflns_number_total 1930 _reflns_number_gt 1315 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART(Bruker 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _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^)+(0.1143P)^2^+15.8091P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1930 _refine_ls_number_parameters 160 _refine_ls_number_restraints 64 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.2134 _refine_ls_wR_factor_gt 0.1627 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.21805(6) 0.66247(6) 0.05590(5) 0.0444(4) Uani 1 1 d U . . C1 C 0.2878(5) 0.5092(5) 0.1052(4) 0.0508(19) Uani 1 1 d . . . C2 C 0.2656(5) 0.5242(5) 0.1772(4) 0.056(2) Uani 1 1 d U A . C3 C 0.2841(6) 0.4677(6) 0.2308(5) 0.075(3) Uani 1 1 d U . . H3 H 0.2711 0.4786 0.2779 0.090 Uiso 1 1 calc R A . C4 C 0.3205(6) 0.3980(6) 0.2141(5) 0.081(3) Uani 1 1 d U A . H4 H 0.3296 0.3602 0.2493 0.097 Uiso 1 1 calc R . . C5 C 0.3442(6) 0.3828(6) 0.1447(5) 0.071(3) Uani 1 1 d U . . H5 H 0.3711 0.3358 0.1344 0.085 Uiso 1 1 calc R A . C6 C 0.3288(5) 0.4355(5) 0.0913(5) 0.055(2) Uani 1 1 d U A . C7 C 0.3824(7) 0.3513(6) 0.0008(6) 0.089(3) Uani 1 1 d . A . H7A H 0.3497 0.3072 0.0168 0.107 Uiso 1 1 calc R . . H7B H 0.4349 0.3461 0.0220 0.107 Uiso 1 1 calc R . . C8 C 0.3886(8) 0.3510(8) -0.0781(7) 0.116(4) Uani 1 1 d U . . H8A H 0.3361 0.3518 -0.0984 0.174 Uiso 1 1 calc R . . H8B H 0.4160 0.3038 -0.0933 0.174 Uiso 1 1 calc R . . H8C H 0.4176 0.3972 -0.0935 0.174 Uiso 1 1 calc R . . C9 C 0.2273(5) 0.5954(5) 0.1991(4) 0.060(2) Uani 1 1 d U . . H9 H 0.2148 0.5984 0.2472 0.072 Uiso 1 1 calc R A . C10 C 0.1122(5) 0.8005(5) 0.0980(4) 0.062(2) Uani 1 1 d . . . H10A H 0.0681 0.7645 0.0926 0.093 Uiso 1 1 calc R A . H10B H 0.0956 0.8535 0.0858 0.093 Uiso 1 1 calc R . . H10C H 0.1302 0.7996 0.1465 0.093 Uiso 1 1 calc R . . O1 O 0.2720(3) 0.5554(3) 0.0522(2) 0.0506(13) Uani 1 1 d . A . O2 O 0.2081(3) 0.6544(3) 0.1628(3) 0.0570(15) Uani 1 1 d U A . O3 O 0.3471(4) 0.4254(3) 0.0210(3) 0.0644(16) Uani 1 1 d . . . O4 O 0.1754(3) 0.7766(3) 0.0525(2) 0.0448(13) Uani 1 1 d U . . O5 O 0.092(2) 0.630(2) 0.056(2) 0.0448(13) Uani 0.263(17) 1 d PU A 2 H5A H 0.0731 0.6636 0.0269 0.067 Uiso 0.263(17) 1 d PR A 2 C11 C 0.0605(17) 0.5666(17) 0.0864(16) 0.051(6) Uani 0.263(17) 1 d PU A 2 H11A H 0.0957 0.5295 0.1093 0.076 Uiso 0.263(17) 1 d PR A 2 H11B H 0.0245 0.5382 0.0559 0.076 Uiso 0.263(17) 1 d PR A 2 H11C H 0.0308 0.5952 0.1217 0.076 Uiso 0.263(17) 1 d PR A 2 O5' O 0.1038(7) 0.6120(7) 0.0441(6) 0.052(3) Uani 0.737(17) 1 d PD A 1 H5A' H 0.0848 0.6454 0.0147 0.078 Uiso 0.737(17) 1 d PRD A 1 H5B H 0.1518 0.5958 0.0464 0.078 Uiso 0.737(17) 1 d PRD A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0497(7) 0.0411(6) 0.0424(7) 0.0014(4) 0.0028(4) 0.0025(4) C1 0.053(5) 0.048(4) 0.051(5) 0.003(4) -0.005(4) -0.003(3) C2 0.068(5) 0.047(4) 0.053(4) 0.001(4) -0.006(4) 0.003(4) C3 0.089(5) 0.072(4) 0.064(4) 0.005(4) -0.007(4) 0.009(4) C4 0.093(6) 0.076(6) 0.073(6) 0.014(5) -0.013(5) 0.017(5) C5 0.079(6) 0.064(5) 0.071(5) 0.003(4) -0.009(4) 0.014(4) C6 0.056(5) 0.050(4) 0.061(5) -0.001(4) -0.004(4) 0.002(4) C7 0.091(8) 0.083(7) 0.095(7) -0.005(6) 0.009(6) 0.039(6) C8 0.123(8) 0.116(8) 0.109(7) -0.013(6) 0.025(7) 0.035(7) C9 0.068(4) 0.062(4) 0.050(4) -0.001(3) -0.001(3) 0.000(3) C10 0.069(6) 0.061(5) 0.056(5) 0.005(4) 0.024(5) 0.015(4) O1 0.057(3) 0.046(3) 0.050(3) 0.001(2) 0.001(2) 0.007(2) O2 0.077(4) 0.049(3) 0.046(3) 0.001(2) 0.003(3) 0.013(3) O3 0.075(4) 0.055(3) 0.063(4) -0.002(3) 0.010(3) 0.018(3) O4 0.047(3) 0.044(3) 0.044(3) -0.001(2) 0.005(2) 0.004(2) O5 0.047(3) 0.044(3) 0.044(3) -0.001(2) 0.005(2) 0.004(2) C11 0.049(8) 0.050(8) 0.053(8) 0.010(7) 0.001(7) -0.004(7) O5' 0.045(5) 0.051(7) 0.061(7) 0.001(5) 0.012(4) 0.007(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 Ni1 O1 2.013(5) . ? Ni1 O2 2.022(6) . ? Ni1 O4 2.045(5) . ? Ni1 O4 2.052(5) 12_665 ? Ni1 O4 2.061(5) 2_565 ? Ni1 O5' 2.107(12) . ? Ni1 O5 2.18(4) . ? C1 O1 1.290(8) . ? C1 C2 1.427(11) . ? C1 C6 1.439(11) . ? C2 C9 1.417(11) . ? C2 C3 1.419(11) . ? C3 C4 1.357(12) . ? C3 H3 0.9300 . ? C4 C5 1.388(13) . ? C4 H4 0.9300 . ? C5 C6 1.363(12) . ? C5 H5 0.9300 . ? C6 O3 1.368(10) . ? C7 O3 1.428(10) . ? C7 C8 1.488(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O2 1.246(9) . ? C9 H9 0.9300 . ? C10 O4 1.422(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? O4 Ni1 2.052(5) 11_565 ? O4 Ni1 2.061(5) 2_565 ? O5 C11 1.32(5) . ? O5 H5A 0.8503 . ? O5 H5A' 0.8334 . ? O5 H5B 1.1701 . ? C11 H11A 0.9600 . ? C11 H11B 0.9601 . ? C11 H11C 0.9599 . ? O5' H5A 1.0587 . ? O5' H5A' 0.8502 . ? O5' H5B 0.8503 . ? 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 O2 90.7(2) . . ? O1 Ni1 O4 172.7(2) . . ? O2 Ni1 O4 93.72(19) . . ? O1 Ni1 O4 92.28(19) . 12_665 ? O2 Ni1 O4 176.9(2) . 12_665 ? O4 Ni1 O4 83.4(2) . 12_665 ? O1 Ni1 O4 93.0(2) . 2_565 ? O2 Ni1 O4 97.8(2) . 2_565 ? O4 Ni1 O4 80.7(2) . 2_565 ? O4 Ni1 O4 83.0(2) 12_665 2_565 ? O1 Ni1 O5' 92.7(3) . . ? O2 Ni1 O5' 90.2(4) . . ? O4 Ni1 O5' 93.1(3) . . ? O4 Ni1 O5' 88.7(4) 12_665 . ? O4 Ni1 O5' 170.2(4) 2_565 . ? O1 Ni1 O5 102.4(10) . . ? O2 Ni1 O5 84.2(10) . . ? O4 Ni1 O5 83.9(10) . . ? O4 Ni1 O5 94.2(10) 12_665 . ? O4 Ni1 O5 164.5(10) 2_565 . ? O1 Ni1 H5B 71.5 . . ? O2 Ni1 H5B 90.4 . . ? O4 Ni1 H5B 114.3 . . ? O4 Ni1 H5B 89.6 12_665 . ? O4 Ni1 H5B 162.5 2_565 . ? O5' Ni1 H5B 21.2 . . ? O5 Ni1 H5B 31.5 . . ? O1 C1 C2 125.0(7) . . ? O1 C1 C6 118.3(7) . . ? C2 C1 C6 116.7(7) . . ? C9 C2 C3 117.1(8) . . ? C9 C2 C1 122.9(7) . . ? C3 C2 C1 120.0(8) . . ? C4 C3 C2 120.6(9) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.4(9) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 121.3(9) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 O3 126.1(8) . . ? C5 C6 C1 121.0(8) . . ? O3 C6 C1 112.9(7) . . ? O3 C7 C8 107.3(8) . . ? O3 C7 H7A 110.3 . . ? C8 C7 H7A 110.3 . . ? O3 C7 H7B 110.3 . . ? C8 C7 H7B 110.3 . . ? H7A C7 H7B 108.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 C2 128.9(8) . . ? O2 C9 H9 115.5 . . ? C2 C9 H9 115.5 . . ? O4 C10 H10A 109.5 . . ? O4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C1 O1 Ni1 127.0(5) . . ? C9 O2 Ni1 125.2(5) . . ? C6 O3 C7 117.3(7) . . ? C10 O4 Ni1 120.4(4) . . ? C10 O4 Ni1 120.5(5) . 11_565 ? Ni1 O4 Ni1 96.3(2) . 11_565 ? C10 O4 Ni1 119.2(5) . 2_565 ? Ni1 O4 Ni1 99.2(2) . 2_565 ? Ni1 O4 Ni1 95.8(2) 11_565 2_565 ? C11 O5 Ni1 126(3) . . ? C11 O5 H5A 131.3 . . ? Ni1 O5 H5A 101.5 . . ? C11 O5 H5A' 126.1 . . ? Ni1 O5 H5A' 93.8 . . ? C11 O5 H5B 90.7 . . ? Ni1 O5 H5B 45.1 . . ? H5A O5 H5B 122.9 . . ? H5A' O5 H5B 97.4 . . ? O5 C11 H11A 118.0 . . ? O5 C11 H11B 113.6 . . ? H11A C11 H11B 109.5 . . ? O5 C11 H11C 95.8 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Ni1 O5' H5A 98.4 . . ? Ni1 O5' H5A' 98.4 . . ? H5A O5' H5B 137.6 . . ? H5A' O5' H5B 126.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O1 0.85 1.86 2.69(4) 164.3 11_565 O5' H5A' O1 0.85 1.94 2.781(13) 172.3 11_565 O5' H5B O1 0.85 2.13 2.981(12) 179.8 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.056 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.124 #========================================================== data_771964 _database_code_depnum_ccdc_archive 'CCDC 771964' #TrackingRef 'content .cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H48 Ni7 O24, 3(Cl O4) ' _chemical_formula_sum 'C48 H48 Cl3 Ni7 O36' _chemical_formula_weight 1718.18 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' 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 ' _symmetry_space_group_name_Hall '-C 2yc ' 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 21.751(2) _cell_length_b 13.7046(14) _cell_length_c 22.953(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.2590(10) _cell_angle_gamma 90.00 _cell_volume 6497.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3299 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 25.10 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.360 _exptl_crystal_size_min 0.355 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3484 _exptl_absorpt_coefficient_mu 2.202 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19058 _diffrn_reflns_av_R_equivalents 0.0845 _diffrn_reflns_av_sigmaI/netI 0.0776 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5664 _reflns_number_gt 3290 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART(Bruker 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _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^)+(0.1159P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5664 _refine_ls_number_parameters 444 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.2046 _refine_ls_wR_factor_gt 0.1929 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.004 _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 0.2500 0.7500 0.0000 0.0571(4) Uani 1 2 d S . . Ni2 Ni 0.16333(4) 0.89045(7) 0.04525(4) 0.0578(3) Uani 1 1 d . . . Ni3 Ni 0.30624(5) 0.85543(7) 0.12556(4) 0.0580(3) Uani 1 1 d . . . Ni4 Ni 0.38971(4) 0.70421(7) 0.08338(4) 0.0569(3) Uani 1 1 d . . . Cl1 Cl 0.18831(13) 0.5230(2) 0.09811(15) 0.0938(8) Uani 1 1 d U . . Cl2 Cl 0.5000 0.2807(4) 0.2500 0.1142(13) Uani 1 2 d SU . . C1 C 0.2500(4) 1.0510(6) 0.0937(3) 0.0584(19) Uani 1 1 d . . . C2 C 0.3086(4) 1.0969(6) 0.1237(4) 0.073(2) Uani 1 1 d . . . C3 C 0.3099(5) 1.2048(8) 0.1179(5) 0.102(3) Uani 1 1 d U . . H3 H 0.3469 1.2406 0.1376 0.123 Uiso 1 1 calc R . . C4 C 0.2562(5) 1.2479(9) 0.0836(5) 0.110(3) Uani 1 1 d U . . H4 H 0.2578 1.3155 0.0810 0.132 Uiso 1 1 calc R . . C5 C 0.2005(5) 1.2062(8) 0.0526(5) 0.102(3) Uani 1 1 d U . . H5 H 0.1650 1.2418 0.0290 0.123 Uiso 1 1 calc R . . C6 C 0.1990(5) 1.1056(7) 0.0580(4) 0.080(3) Uani 1 1 d U . . C7 C 0.0871(7) 1.0843(12) -0.0107(6) 0.158(5) Uani 1 1 d U . . H7A H 0.0786 1.1459 0.0051 0.237 Uiso 1 1 calc R . . H7B H 0.0516 1.0407 -0.0142 0.237 Uiso 1 1 calc R . . H7C H 0.0922 1.0938 -0.0504 0.237 Uiso 1 1 calc R . . C8 C 0.3622(6) 1.0485(10) 0.1557(5) 0.111(3) Uani 1 1 d U . . H8 H 0.3972 1.0883 0.1755 0.133 Uiso 1 1 calc R . . C9 C 0.4532(3) 0.7364(6) -0.0053(4) 0.0589(19) Uani 1 1 d . . . C10 C 0.4580(4) 0.7421(7) -0.0632(4) 0.069(2) Uani 1 1 d . . . C11 C 0.5006(5) 0.8100(8) -0.0744(5) 0.094(3) Uani 1 1 d . . . H11 H 0.5058 0.8133 -0.1131 0.113 Uiso 1 1 calc R . . C12 C 0.5343(5) 0.8710(8) -0.0298(5) 0.100(3) Uani 1 1 d . . . H12 H 0.5618 0.9168 -0.0385 0.120 Uiso 1 1 calc R . . C13 C 0.5289(4) 0.8668(7) 0.0284(4) 0.087(3) Uani 1 1 d . . . H13 H 0.5525 0.9089 0.0590 0.105 Uiso 1 1 calc R . . C14 C 0.4879(3) 0.7992(6) 0.0401(4) 0.064(2) Uani 1 1 d . . . C15 C 0.5144(5) 0.8404(8) 0.1477(5) 0.112(3) Uani 1 1 d U . . H15A H 0.5596 0.8283 0.1545 0.168 Uiso 1 1 calc R . . H15B H 0.5031 0.8201 0.1831 0.168 Uiso 1 1 calc R . . H15C H 0.5058 0.9089 0.1409 0.168 Uiso 1 1 calc R . . C16 C 0.4207(5) 0.6805(8) -0.1133(4) 0.088(3) Uani 1 1 d . . . H16 H 0.4296 0.6868 -0.1501 0.105 Uiso 1 1 calc R . . C17 C 0.3636(3) 0.6953(6) 0.2029(3) 0.060(2) Uani 1 1 d . . . C18 C 0.3936(4) 0.6061(6) 0.2187(4) 0.072(2) Uani 1 1 d . . . C19 C 0.3889(5) 0.5584(8) 0.2717(4) 0.095(3) Uani 1 1 d . . . H19 H 0.4098 0.4990 0.2836 0.114 Uiso 1 1 calc R . . C20 C 0.3541(6) 0.5986(9) 0.3055(5) 0.102(3) Uani 1 1 d . . . H20 H 0.3527 0.5677 0.3411 0.122 Uiso 1 1 calc R . . C21 C 0.3219(5) 0.6816(8) 0.2882(4) 0.088(3) Uani 1 1 d . . . H21 H 0.2963 0.7055 0.3107 0.106 Uiso 1 1 calc R . . C22 C 0.3256(4) 0.7340(7) 0.2370(4) 0.067(2) Uani 1 1 d . . . C23 C 0.2494(5) 0.8594(8) 0.2403(5) 0.114(4) Uani 1 1 d U . . H23A H 0.2210 0.8088 0.2455 0.172 Uiso 1 1 calc R . . H23B H 0.2245 0.9089 0.2135 0.172 Uiso 1 1 calc R . . H23C H 0.2718 0.8878 0.2795 0.172 Uiso 1 1 calc R . . C24 C 0.4271(4) 0.5593(7) 0.1810(5) 0.085(3) Uani 1 1 d . . . H24 H 0.4462 0.4998 0.1956 0.102 Uiso 1 1 calc R . . O1 O 0.2413(2) 0.9565(4) 0.0976(2) 0.0662(14) Uani 1 1 d . . . O2 O 0.1422(3) 1.0454(5) 0.0279(3) 0.094(2) Uani 1 1 d . . . O3 O 0.3726(3) 0.9649(6) 0.1631(3) 0.102(2) Uani 1 1 d U . . O4 O 0.4152(2) 0.6706(4) 0.0103(2) 0.0599(13) Uani 1 1 d . . . O5 O 0.4769(3) 0.7869(4) 0.0953(2) 0.0736(15) Uani 1 1 d U . . O6 O 0.3789(3) 0.6216(5) -0.1126(3) 0.0832(18) Uani 1 1 d . . . O7 O 0.3680(2) 0.7489(4) 0.1556(2) 0.0614(13) Uani 1 1 d . . . O8 O 0.2952(3) 0.8192(5) 0.2143(2) 0.0768(16) Uani 1 1 d . . . O9 O 0.4339(3) 0.5862(5) 0.1329(3) 0.0861(19) Uani 1 1 d . . . O10 O 0.2253(2) 0.7727(3) 0.07567(19) 0.0514(12) Uani 1 1 d . . . H10A H 0.2039 0.7207 0.0751 0.077 Uiso 1 1 d R . . O11 O 0.3300(2) 0.8257(3) 0.04620(19) 0.0519(11) Uani 1 1 d . . . H11B H 0.3413 0.8670 0.0239 0.078 Uiso 1 1 d R . . O12 O 0.3060(2) 0.6331(3) 0.0314(2) 0.0511(11) Uani 1 1 d . . . H12B H 0.2944 0.5888 0.0517 0.077 Uiso 1 1 d R . . O13 O 0.1461(4) 0.5430(7) 0.0381(4) 0.160(4) Uani 1 1 d . A . O14 O 0.1644(3) 0.4439(6) 0.1260(3) 0.110(2) Uani 1 1 d U A . O16 O 0.1897(4) 0.6105(7) 0.1346(4) 0.149(3) Uani 1 1 d U A . O17 O 0.4339(9) 0.272(2) 0.2500(8) 0.215(12) Uani 0.50 1 d P . . O18 O 0.4744(5) 0.3246(8) 0.1945(5) 0.186(4) Uani 1 1 d U . . O19 O 0.5000 0.1829(18) 0.2500 0.245(8) Uani 1 2 d SU . . O15 O 0.196(3) 0.502(4) 0.065(3) 0.03(2) Uani 0.086(17) 1 d PU A 2 O15' O 0.2511(4) 0.5034(6) 0.0979(6) 0.170(6) Uani 0.914(17) 1 d P A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0564(8) 0.0498(9) 0.0621(8) -0.0047(6) 0.0142(6) 0.0006(6) Ni2 0.0574(6) 0.0476(6) 0.0694(7) -0.0084(5) 0.0210(5) 0.0011(4) Ni3 0.0675(6) 0.0456(6) 0.0547(6) -0.0072(4) 0.0101(5) -0.0006(4) Ni4 0.0481(5) 0.0635(7) 0.0550(6) 0.0065(5) 0.0103(4) 0.0058(4) Cl1 0.0912(11) 0.0875(11) 0.0992(11) 0.0165(9) 0.0247(9) -0.0095(8) Cl2 0.1191(16) 0.1139(16) 0.1128(15) 0.000 0.0410(10) 0.000 C1 0.074(5) 0.043(5) 0.065(5) -0.007(4) 0.033(4) 0.000(4) C2 0.078(6) 0.058(6) 0.083(6) -0.004(4) 0.029(5) -0.004(4) C3 0.102(3) 0.102(3) 0.103(3) -0.0009(11) 0.0326(14) -0.0016(11) C4 0.111(3) 0.109(4) 0.110(3) 0.0000(11) 0.0348(15) -0.0003(11) C5 0.103(3) 0.102(3) 0.102(3) 0.0006(11) 0.0325(14) 0.0008(11) C6 0.080(3) 0.080(3) 0.080(3) -0.0005(11) 0.0255(13) 0.0005(11) C7 0.158(5) 0.158(5) 0.158(5) -0.0003(11) 0.0491(19) 0.0008(11) C8 0.111(4) 0.111(4) 0.111(4) -0.0006(11) 0.0348(15) 0.0003(11) C9 0.041(4) 0.065(5) 0.069(5) 0.010(4) 0.015(4) 0.007(4) C10 0.060(5) 0.074(6) 0.081(6) -0.006(5) 0.033(4) -0.003(4) C11 0.087(7) 0.110(9) 0.092(7) -0.010(6) 0.037(6) -0.016(6) C12 0.092(7) 0.103(9) 0.111(8) -0.003(6) 0.043(6) -0.040(6) C13 0.070(6) 0.099(8) 0.089(7) -0.020(6) 0.020(5) -0.018(5) C14 0.050(4) 0.072(6) 0.072(5) -0.002(4) 0.019(4) 0.001(4) C15 0.112(4) 0.112(4) 0.112(4) -0.0009(11) 0.0349(15) -0.0005(11) C16 0.097(7) 0.103(8) 0.081(6) -0.022(6) 0.054(6) -0.011(6) C17 0.051(4) 0.069(6) 0.050(4) 0.006(4) 0.002(3) -0.009(4) C18 0.064(5) 0.068(6) 0.078(6) 0.016(5) 0.015(4) 0.006(4) C19 0.097(7) 0.089(8) 0.097(7) 0.039(6) 0.027(6) 0.009(6) C20 0.129(9) 0.103(9) 0.086(7) 0.028(6) 0.051(7) 0.008(7) C21 0.096(7) 0.096(8) 0.083(6) 0.011(6) 0.041(5) 0.003(6) C22 0.065(5) 0.074(6) 0.057(5) -0.007(4) 0.011(4) -0.003(4) C23 0.115(4) 0.115(4) 0.114(4) -0.0008(11) 0.0362(15) 0.0014(11) C24 0.073(6) 0.081(7) 0.094(7) 0.025(6) 0.016(5) 0.021(5) O1 0.072(3) 0.040(3) 0.082(4) -0.012(3) 0.017(3) 0.003(2) O2 0.086(4) 0.092(5) 0.103(5) 0.005(4) 0.027(4) 0.040(4) O3 0.102(2) 0.101(2) 0.102(2) -0.0003(10) 0.0303(12) -0.0016(10) O4 0.047(3) 0.067(4) 0.063(3) -0.004(3) 0.013(2) 0.000(2) O5 0.0717(17) 0.0748(18) 0.0735(17) -0.0010(10) 0.0216(11) -0.0018(10) O6 0.080(4) 0.093(5) 0.085(4) -0.033(3) 0.039(3) -0.013(4) O7 0.065(3) 0.058(3) 0.057(3) 0.006(3) 0.014(2) 0.006(3) O8 0.088(4) 0.082(4) 0.064(3) -0.001(3) 0.029(3) 0.015(3) O9 0.081(4) 0.098(5) 0.080(4) 0.032(4) 0.026(3) 0.037(3) O10 0.062(3) 0.041(3) 0.052(3) -0.008(2) 0.019(2) -0.003(2) O11 0.054(3) 0.046(3) 0.052(3) -0.001(2) 0.013(2) -0.002(2) O12 0.049(3) 0.038(3) 0.064(3) 0.006(2) 0.015(2) 0.002(2) O13 0.124(6) 0.179(9) 0.127(6) 0.080(6) -0.033(5) -0.072(6) O14 0.109(2) 0.109(2) 0.111(2) 0.0050(11) 0.0327(12) -0.0037(11) O16 0.150(3) 0.148(3) 0.148(3) 0.0006(11) 0.0472(14) -0.0007(11) O17 0.121(14) 0.39(4) 0.129(14) -0.105(19) 0.037(11) -0.087(18) O18 0.186(4) 0.185(4) 0.185(4) 0.0000(11) 0.0577(16) 0.0017(11) O19 0.245(8) 0.244(8) 0.245(8) 0.000 0.076(3) 0.000 O15 0.03(2) 0.03(2) 0.03(2) 0.0000(11) 0.010(6) -0.0001(11) O15' 0.080(7) 0.108(7) 0.329(15) 0.100(8) 0.073(8) 0.011(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 O10 1.997(4) . ? Ni1 O10 1.997(4) 7_565 ? Ni1 O12 2.005(4) 7_565 ? Ni1 O12 2.005(4) . ? Ni1 O11 2.018(4) 7_565 ? Ni1 O11 2.018(4) . ? Ni2 O1 1.965(5) . ? Ni2 O4 1.970(5) 7_565 ? Ni2 O6 2.039(6) 7_565 ? Ni2 O10 2.078(5) . ? Ni2 O12 2.093(5) 7_565 ? Ni2 O2 2.183(6) . ? Ni3 O1 1.938(5) . ? Ni3 O7 1.957(5) . ? Ni3 O3 2.073(7) . ? Ni3 O11 2.084(4) . ? Ni3 O10 2.105(5) . ? Ni3 O8 2.181(5) . ? Ni4 O7 1.959(5) . ? Ni4 O4 1.979(5) . ? Ni4 O9 2.037(6) . ? Ni4 O12 2.080(4) . ? Ni4 O11 2.119(5) . ? Ni4 O5 2.151(5) . ? Cl1 O15 0.87(6) . ? Cl1 O15' 1.394(9) . ? Cl1 O13 1.422(7) . ? Cl1 O14 1.437(7) . ? Cl1 O16 1.457(9) . ? Cl2 O19 1.34(2) . ? Cl2 O18 1.361(11) 2_655 ? Cl2 O18 1.361(11) . ? Cl2 O17 1.441(19) . ? Cl2 O17 1.441(19) 2_655 ? C1 O1 1.316(9) . ? C1 C6 1.375(11) . ? C1 C2 1.395(11) . ? C2 C8 1.343(13) . ? C2 C3 1.485(13) . ? C3 C4 1.325(13) . ? C3 H3 0.9300 . ? C4 C5 1.328(13) . ? C4 H4 0.9300 . ? C5 C6 1.386(13) . ? C5 H5 0.9300 . ? C6 O2 1.467(11) . ? C7 O2 1.355(14) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 O3 1.169(12) . ? C8 H8 0.9300 . ? C9 O4 1.345(9) . ? C9 C10 1.369(10) . ? C9 C14 1.380(10) . ? C10 C11 1.393(12) . ? C10 C16 1.452(12) . ? C11 C12 1.346(12) . ? C11 H11 0.9300 . ? C12 C13 1.379(12) . ? C12 H12 0.9300 . ? C13 C14 1.370(11) . ? C13 H13 0.9300 . ? C14 O5 1.372(9) . ? C15 O5 1.427(11) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 O6 1.218(10) . ? C16 H16 0.9300 . ? C17 O7 1.339(8) . ? C17 C18 1.379(11) . ? C17 C22 1.409(11) . ? C18 C19 1.413(12) . ? C18 C24 1.444(12) . ? C19 C20 1.360(13) . ? C19 H19 0.9300 . ? C20 C21 1.329(13) . ? C20 H20 0.9300 . ? C21 C22 1.401(12) . ? C21 H21 0.9300 . ? C22 O8 1.362(10) . ? C23 O8 1.423(11) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O9 1.215(10) . ? C24 H24 0.9300 . ? O4 Ni2 1.970(5) 7_565 ? O6 Ni2 2.039(6) 7_565 ? O10 H10A 0.8499 . ? O11 H11B 0.8498 . ? O12 Ni2 2.093(5) 7_565 ? O12 H12B 0.8499 . ? O13 O15 1.21(6) . ? 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 O10 Ni1 O10 180.0 . 7_565 ? O10 Ni1 O12 83.67(19) . 7_565 ? O10 Ni1 O12 96.33(19) 7_565 7_565 ? O10 Ni1 O12 96.33(19) . . ? O10 Ni1 O12 83.67(19) 7_565 . ? O12 Ni1 O12 180.000(1) 7_565 . ? O10 Ni1 O11 96.56(18) . 7_565 ? O10 Ni1 O11 83.44(18) 7_565 7_565 ? O12 Ni1 O11 83.97(18) 7_565 7_565 ? O12 Ni1 O11 96.03(18) . 7_565 ? O10 Ni1 O11 83.44(18) . . ? O10 Ni1 O11 96.56(18) 7_565 . ? O12 Ni1 O11 96.03(18) 7_565 . ? O12 Ni1 O11 83.97(18) . . ? O11 Ni1 O11 180.0 7_565 . ? O1 Ni2 O4 177.1(2) . 7_565 ? O1 Ni2 O6 94.7(2) . 7_565 ? O4 Ni2 O6 87.2(2) 7_565 7_565 ? O1 Ni2 O10 78.88(19) . . ? O4 Ni2 O10 103.17(19) 7_565 . ? O6 Ni2 O10 94.7(2) 7_565 . ? O1 Ni2 O12 98.23(19) . 7_565 ? O4 Ni2 O12 80.23(18) 7_565 7_565 ? O6 Ni2 O12 164.5(2) 7_565 7_565 ? O10 Ni2 O12 79.56(17) . 7_565 ? O1 Ni2 O2 75.9(2) . . ? O4 Ni2 O2 101.8(2) 7_565 . ? O6 Ni2 O2 95.6(2) 7_565 . ? O10 Ni2 O2 153.4(2) . . ? O12 Ni2 O2 95.8(2) 7_565 . ? O1 Ni3 O7 176.5(2) . . ? O1 Ni3 O3 87.7(3) . . ? O7 Ni3 O3 94.7(3) . . ? O1 Ni3 O11 101.8(2) . . ? O7 Ni3 O11 80.27(19) . . ? O3 Ni3 O11 100.0(2) . . ? O1 Ni3 O10 78.8(2) . . ? O7 Ni3 O10 98.9(2) . . ? O3 Ni3 O10 166.0(2) . . ? O11 Ni3 O10 79.25(17) . . ? O1 Ni3 O8 101.0(2) . . ? O7 Ni3 O8 76.4(2) . . ? O3 Ni3 O8 92.4(2) . . ? O11 Ni3 O8 154.4(2) . . ? O10 Ni3 O8 93.9(2) . . ? O7 Ni4 O4 174.9(2) . . ? O7 Ni4 O9 88.4(2) . . ? O4 Ni4 O9 94.5(2) . . ? O7 Ni4 O12 103.42(19) . . ? O4 Ni4 O12 80.35(19) . . ? O9 Ni4 O12 97.1(2) . . ? O7 Ni4 O11 79.38(18) . . ? O4 Ni4 O11 98.09(19) . . ? O9 Ni4 O11 166.2(2) . . ? O12 Ni4 O11 79.73(17) . . ? O7 Ni4 O5 99.4(2) . . ? O4 Ni4 O5 76.2(2) . . ? O9 Ni4 O5 96.0(2) . . ? O12 Ni4 O5 153.9(2) . . ? O11 Ni4 O5 92.39(19) . . ? O15 Cl1 O15' 58(4) . . ? O15 Cl1 O13 58(4) . . ? O15' Cl1 O13 111.7(7) . . ? O15 Cl1 O14 109(4) . . ? O15' Cl1 O14 110.4(5) . . ? O13 Cl1 O14 111.2(4) . . ? O15 Cl1 O16 143(4) . . ? O15' Cl1 O16 108.5(7) . . ? O13 Cl1 O16 106.8(6) . . ? O14 Cl1 O16 108.0(5) . . ? O19 Cl2 O18 116.3(5) . 2_655 ? O19 Cl2 O18 116.3(5) . . ? O18 Cl2 O18 127.5(11) 2_655 . ? O19 Cl2 O17 85.5(12) . . ? O18 Cl2 O17 98.6(8) 2_655 . ? O18 Cl2 O17 85.4(11) . . ? O19 Cl2 O17 85.5(12) . 2_655 ? O18 Cl2 O17 85.4(11) 2_655 2_655 ? O18 Cl2 O17 98.6(8) . 2_655 ? O17 Cl2 O17 171(2) . 2_655 ? O1 C1 C6 118.0(8) . . ? O1 C1 C2 122.6(7) . . ? C6 C1 C2 119.4(8) . . ? C8 C2 C1 123.3(10) . . ? C8 C2 C3 120.3(10) . . ? C1 C2 C3 116.4(8) . . ? C4 C3 C2 117.4(11) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C5 C4 C3 127.8(13) . . ? C5 C4 H4 116.1 . . ? C3 C4 H4 116.1 . . ? C4 C5 C6 115.0(11) . . ? C4 C5 H5 122.5 . . ? C6 C5 H5 122.5 . . ? C1 C6 C5 123.9(9) . . ? C1 C6 O2 112.3(8) . . ? C5 C6 O2 123.8(9) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C2 131.2(12) . . ? O3 C8 H8 114.4 . . ? C2 C8 H8 114.4 . . ? O4 C9 C10 122.5(7) . . ? O4 C9 C14 117.0(7) . . ? C10 C9 C14 120.5(7) . . ? C9 C10 C11 118.4(8) . . ? C9 C10 C16 122.8(8) . . ? C11 C10 C16 118.8(8) . . ? C12 C11 C10 120.6(9) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 121.3(9) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C14 C13 C12 118.5(8) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 O5 125.3(8) . . ? C13 C14 C9 120.6(8) . . ? O5 C14 C9 114.1(7) . . ? O5 C15 H15A 109.5 . . ? O5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O6 C16 C10 127.6(8) . . ? O6 C16 H16 116.2 . . ? C10 C16 H16 116.2 . . ? O7 C17 C18 123.5(7) . . ? O7 C17 C22 116.5(7) . . ? C18 C17 C22 120.0(8) . . ? C17 C18 C19 118.7(9) . . ? C17 C18 C24 121.4(8) . . ? C19 C18 C24 119.8(9) . . ? C20 C19 C18 120.4(10) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 120.8(9) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 121.8(9) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? O8 C22 C21 127.8(8) . . ? O8 C22 C17 114.2(7) . . ? C21 C22 C17 118.0(9) . . ? O8 C23 H23A 109.5 . . ? O8 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O8 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O9 C24 C18 129.6(9) . . ? O9 C24 H24 115.2 . . ? C18 C24 H24 115.2 . . ? C1 O1 Ni3 128.3(5) . . ? C1 O1 Ni2 121.8(5) . . ? Ni3 O1 Ni2 105.9(2) . . ? C7 O2 C6 121.9(9) . . ? C7 O2 Ni2 126.4(8) . . ? C6 O2 Ni2 111.2(5) . . ? C8 O3 Ni3 124.9(8) . . ? C9 O4 Ni2 126.3(4) . 7_565 ? C9 O4 Ni4 115.3(5) . . ? Ni2 O4 Ni4 103.4(2) 7_565 . ? C14 O5 C15 119.7(7) . . ? C14 O5 Ni4 110.4(5) . . ? C15 O5 Ni4 128.8(6) . . ? C16 O6 Ni2 125.3(6) . 7_565 ? C17 O7 Ni3 118.7(5) . . ? C17 O7 Ni4 127.7(5) . . ? Ni3 O7 Ni4 104.8(2) . . ? C22 O8 C23 119.4(7) . . ? C22 O8 Ni3 111.7(5) . . ? C23 O8 Ni3 126.9(6) . . ? C24 O9 Ni4 125.2(6) . . ? Ni1 O10 Ni2 98.73(18) . . ? Ni1 O10 Ni3 98.64(19) . . ? Ni2 O10 Ni3 96.23(19) . . ? Ni1 O10 H10A 98.7 . . ? Ni2 O10 H10A 110.6 . . ? Ni3 O10 H10A 145.3 . . ? Ni1 O11 Ni3 98.63(19) . . ? Ni1 O11 Ni4 97.27(19) . . ? Ni3 O11 Ni4 95.17(18) . . ? Ni1 O11 H11B 113.0 . . ? Ni3 O11 H11B 126.4 . . ? Ni4 O11 H11B 120.7 . . ? Ni1 O12 Ni4 98.95(19) . . ? Ni1 O12 Ni2 97.95(19) . 7_565 ? Ni4 O12 Ni2 95.85(18) . 7_565 ? Ni1 O12 H12B 121.1 . . ? Ni4 O12 H12B 112.2 . . ? Ni2 O12 H12B 125.3 7_565 . ? Cl1 O13 O15 38(3) . . ? Cl1 O15 O13 84(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O10 H10A O16 0.85 2.12 2.835(10) 140.9 . O11 H11B O13 0.85 1.97 2.808(8) 170.5 7_565 O12 H12B O15 0.85 2.55 3.27(6) 143.6 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.073 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.109 #===================================================================