# 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 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Papaefstathiou, Giannis' _publ_contact_author_email gspapaef@chem.uoa.gr loop_ _publ_author_name A.Katsenis V.Kessler G.Papaefstathiou data_tdk473t _database_code_depnum_ccdc_archive 'CCDC 803774' #TrackingRef '- complex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H68 Cl4 N8 Ni4 O12' _chemical_formula_weight 1421.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.098(4) _cell_length_b 17.364(5) _cell_length_c 11.925(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.253(5) _cell_angle_gamma 90.00 _cell_volume 2872.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 998 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.00 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 1.547 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5427 _exptl_absorpt_correction_T_max 0.8011 _exptl_absorpt_process_details 'Bruker SADABS' _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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17328 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.35 _reflns_number_total 6827 _reflns_number_gt 4346 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0704P)^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 6827 _refine_ls_number_parameters 359 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.069 _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 0.86994(3) 1.01181(3) 0.65480(4) 0.03205(14) Uani 1 1 d . . . Ni2 Ni 1.09105(3) 1.02872(3) 0.58615(4) 0.02987(14) Uani 1 1 d . . . Cl1 Cl 0.99924(6) 1.10304(5) 0.70219(8) 0.0392(2) Uani 1 1 d . . . Cl2 Cl 0.59500(12) 1.03317(16) 0.80386(15) 0.1381(9) Uani 1 1 d . . . O1 O 0.97523(15) 0.95100(12) 0.57644(19) 0.0284(5) Uani 1 1 d . . . O2 O 1.06110(16) 0.83637(14) 0.5947(2) 0.0381(6) Uani 1 1 d . . . H2A H 1.0892 0.8628 0.5540 0.057 Uiso 1 1 calc R . . O3 O 0.83456(15) 1.05488(14) 0.49558(19) 0.0326(5) Uani 1 1 d . . . O4 O 0.68403(17) 1.11542(16) 0.4726(2) 0.0498(7) Uani 1 1 d . . . O5 O 0.78866(18) 1.07348(16) 0.7602(2) 0.0495(7) Uani 1 1 d . . . N1 N 0.8473(2) 0.86668(17) 0.4502(3) 0.0362(7) Uani 1 1 d . . . N2 N 0.9262(2) 0.93308(16) 0.7793(2) 0.0345(7) Uani 1 1 d . . . N3 N 0.7401(2) 0.95481(18) 0.5961(3) 0.0400(7) Uani 1 1 d . . . N4 N 0.8060(2) 1.00861(19) 0.2826(3) 0.0410(7) Uani 1 1 d . . . C1 C 0.7745(3) 0.8295(3) 0.3838(4) 0.0506(10) Uani 1 1 d . . . H1 H 0.7444 0.8527 0.3166 0.061 Uiso 1 1 calc R . . C2 C 0.7435(3) 0.7592(3) 0.4116(5) 0.0605(12) Uani 1 1 d . . . H2 H 0.6936 0.7345 0.3634 0.073 Uiso 1 1 calc R . . C3 C 0.7861(3) 0.7251(3) 0.5107(5) 0.0649(13) Uani 1 1 d . . . H3 H 0.7635 0.6780 0.5323 0.078 Uiso 1 1 calc R . . C4 C 0.8626(3) 0.7606(2) 0.5786(4) 0.0504(10) Uani 1 1 d . . . H4 H 0.8945 0.7370 0.6448 0.060 Uiso 1 1 calc R . . C5 C 0.8910(2) 0.8326(2) 0.5460(3) 0.0356(8) Uani 1 1 d . . . C6 C 0.9775(2) 0.8754(2) 0.6138(3) 0.0314(8) Uani 1 1 d . . . C7 C 0.9764(2) 0.8752(2) 0.7419(3) 0.0356(8) Uani 1 1 d . . . C8 C 1.0247(3) 0.8215(2) 0.8163(3) 0.0493(10) Uani 1 1 d . . . H8 H 1.0580 0.7813 0.7895 0.059 Uiso 1 1 calc R . . C9 C 1.0227(3) 0.8286(3) 0.9308(4) 0.0562(11) Uani 1 1 d . . . H9 H 1.0546 0.7929 0.9822 0.067 Uiso 1 1 calc R . . C10 C 0.9738(3) 0.8879(2) 0.9686(3) 0.0517(10) Uani 1 1 d . . . H10 H 0.9728 0.8937 1.0459 0.062 Uiso 1 1 calc R . . C11 C 0.9254(3) 0.9396(2) 0.8903(3) 0.0448(9) Uani 1 1 d . . . H11 H 0.8914 0.9798 0.9159 0.054 Uiso 1 1 calc R . . C12 C 0.6993(3) 0.8996(3) 0.6479(4) 0.0554(11) Uani 1 1 d . . . H12 H 0.7332 0.8801 0.7159 0.066 Uiso 1 1 calc R . . C13 C 0.6095(3) 0.8696(3) 0.6065(5) 0.0710(15) Uani 1 1 d . . . H13 H 0.5848 0.8296 0.6444 0.085 Uiso 1 1 calc R . . C14 C 0.5586(3) 0.8990(3) 0.5106(5) 0.0719(15) Uani 1 1 d . . . H14 H 0.4971 0.8804 0.4823 0.086 Uiso 1 1 calc R . . C15 C 0.5976(3) 0.9579(3) 0.4532(4) 0.0551(11) Uani 1 1 d . . . H15 H 0.5633 0.9787 0.3862 0.066 Uiso 1 1 calc R . . C16 C 0.6894(3) 0.9845(2) 0.4989(3) 0.0407(9) Uani 1 1 d . . . C17 C 0.7374(2) 1.0504(2) 0.4473(3) 0.0394(9) Uani 1 1 d . . . C18 C 0.7307(3) 1.0424(2) 0.3168(3) 0.0473(10) Uani 1 1 d . . . C19 C 0.6532(3) 1.0692(4) 0.2388(4) 0.0847(18) Uani 1 1 d . . . H19 H 0.6007 1.0923 0.2629 0.102 Uiso 1 1 calc R . . C20 C 0.6557(4) 1.0609(5) 0.1251(5) 0.113(3) Uani 1 1 d . . . H20 H 0.6038 1.0778 0.0714 0.136 Uiso 1 1 calc R . . C21 C 0.7339(4) 1.0279(4) 0.0890(4) 0.095(2) Uani 1 1 d . . . H21 H 0.7369 1.0238 0.0119 0.114 Uiso 1 1 calc R . . C22 C 0.8073(3) 1.0011(3) 0.1714(4) 0.0600(12) Uani 1 1 d . . . H22 H 0.8598 0.9770 0.1489 0.072 Uiso 1 1 calc R . . C23 C 0.7238(3) 1.1896(3) 0.4543(5) 0.0790(16) Uani 1 1 d . . . H23A H 0.6822 1.2292 0.4740 0.118 Uiso 1 1 calc R . . H23B H 0.7294 1.1947 0.3756 0.118 Uiso 1 1 calc R . . H23C H 0.7864 1.1944 0.5011 0.118 Uiso 1 1 calc R . . C24 C 0.7903(4) 1.1484(4) 0.7838(6) 0.104(2) Uani 1 1 d . . . H24A H 0.7460 1.1591 0.8343 0.156 Uiso 1 1 calc R . . H24B H 0.7720 1.1771 0.7145 0.156 Uiso 1 1 calc R . . H24C H 0.8542 1.1630 0.8196 0.156 Uiso 1 1 calc R . . C53 C 0.5251(15) 0.8139(13) 1.2141(17) 0.324(10) Uiso 1 1 d D . . C54 C 0.4821(14) 0.7508(10) 1.2818(15) 0.324(9) Uiso 1 1 d D . . O50 O 0.517(3) 0.819(3) 1.087(2) 0.73(3) Uiso 0.66(3) 1 d PD . . C52 C 0.5898(8) 0.8766(7) 0.9067(10) 0.180(4) Uiso 1 1 d D . . C51 C 0.576(2) 0.870(2) 1.029(2) 0.57(2) Uiso 1 1 d D . . O50A O 0.5670(17) 0.8602(14) 1.152(2) 0.197(17) Uiso 0.34(3) 1 d P . . 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 0.0308(2) 0.0351(3) 0.0320(2) 0.00077(19) 0.01027(18) 0.00216(18) Ni2 0.0269(2) 0.0345(3) 0.0282(2) -0.00169(19) 0.00475(17) -0.00041(18) Cl1 0.0403(5) 0.0411(5) 0.0377(5) -0.0080(4) 0.0111(4) -0.0018(4) Cl2 0.0621(9) 0.277(3) 0.0784(11) -0.0456(14) 0.0224(8) -0.0303(13) O1 0.0281(12) 0.0290(13) 0.0288(12) 0.0030(10) 0.0071(9) 0.0010(9) O2 0.0380(13) 0.0336(14) 0.0463(15) 0.0034(11) 0.0175(11) 0.0079(11) O3 0.0229(11) 0.0420(15) 0.0330(13) 0.0012(11) 0.0051(9) 0.0031(10) O4 0.0367(14) 0.0483(17) 0.0669(19) 0.0067(14) 0.0157(13) 0.0132(12) O5 0.0428(15) 0.0468(18) 0.0627(19) -0.0030(14) 0.0199(13) 0.0088(13) N1 0.0342(16) 0.0365(18) 0.0394(18) -0.0069(14) 0.0110(13) -0.0038(13) N2 0.0385(16) 0.0333(17) 0.0338(16) 0.0010(13) 0.0123(13) 0.0030(13) N3 0.0322(16) 0.0397(18) 0.051(2) -0.0035(15) 0.0163(14) 0.0010(13) N4 0.0334(16) 0.054(2) 0.0339(16) -0.0002(15) 0.0011(13) 0.0040(14) C1 0.044(2) 0.056(3) 0.051(2) -0.010(2) 0.0071(18) -0.006(2) C2 0.045(2) 0.048(3) 0.086(4) -0.018(3) 0.007(2) -0.014(2) C3 0.057(3) 0.036(3) 0.102(4) -0.006(3) 0.018(3) -0.015(2) C4 0.047(2) 0.035(2) 0.070(3) 0.003(2) 0.015(2) -0.0064(18) C5 0.0342(19) 0.0306(19) 0.045(2) -0.0066(16) 0.0155(16) -0.0011(15) C6 0.0317(18) 0.0272(19) 0.0380(19) 0.0011(15) 0.0134(15) 0.0016(14) C7 0.0374(19) 0.036(2) 0.0347(19) 0.0037(16) 0.0098(15) -0.0036(16) C8 0.066(3) 0.038(2) 0.045(2) 0.0108(19) 0.015(2) 0.0113(19) C9 0.068(3) 0.056(3) 0.045(2) 0.018(2) 0.009(2) 0.007(2) C10 0.075(3) 0.053(3) 0.029(2) 0.0069(19) 0.0148(19) 0.001(2) C11 0.053(2) 0.051(3) 0.033(2) -0.0017(18) 0.0143(17) -0.0040(19) C12 0.049(2) 0.054(3) 0.069(3) 0.007(2) 0.027(2) -0.004(2) C13 0.046(3) 0.069(3) 0.104(4) 0.002(3) 0.032(3) -0.014(2) C14 0.033(2) 0.071(3) 0.114(5) -0.020(3) 0.021(3) -0.013(2) C15 0.029(2) 0.059(3) 0.076(3) -0.008(2) 0.005(2) 0.0028(19) C16 0.0294(19) 0.046(2) 0.048(2) -0.0091(18) 0.0103(16) 0.0003(16) C17 0.0245(18) 0.047(2) 0.046(2) 0.0029(18) 0.0066(15) 0.0074(15) C18 0.034(2) 0.064(3) 0.042(2) 0.004(2) -0.0008(17) 0.0041(18) C19 0.051(3) 0.149(6) 0.049(3) 0.009(3) -0.005(2) 0.035(3) C20 0.073(4) 0.199(8) 0.057(4) 0.010(4) -0.017(3) 0.050(5) C21 0.066(3) 0.180(7) 0.036(3) 0.000(3) -0.001(2) 0.027(4) C22 0.050(3) 0.088(4) 0.039(2) -0.003(2) -0.0015(19) 0.006(2) C23 0.071(3) 0.055(3) 0.119(5) 0.021(3) 0.039(3) 0.021(3) C24 0.094(4) 0.096(5) 0.135(6) -0.028(4) 0.054(4) 0.016(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 O3 2.019(2) . ? Ni1 N2 2.070(3) . ? Ni1 N3 2.089(3) . ? Ni1 O5 2.134(3) . ? Ni1 O1 2.165(2) . ? Ni1 Cl1 2.4051(11) . ? Ni2 O1 2.028(2) 3_776 ? Ni2 N4 2.042(3) 3_776 ? Ni2 N1 2.092(3) 3_776 ? Ni2 O1 2.106(2) . ? Ni2 O3 2.126(2) 3_776 ? Ni2 Cl1 2.4275(10) . ? O1 C6 1.386(4) . ? O1 Ni2 2.028(2) 3_776 ? O2 C6 1.413(4) . ? O3 C17 1.391(4) . ? O3 Ni2 2.126(2) 3_776 ? O4 C17 1.419(4) . ? O4 C23 1.436(5) . ? O5 C24 1.330(6) . ? N1 C5 1.336(5) . ? N1 C1 1.345(5) . ? N1 Ni2 2.092(3) 3_776 ? N2 C11 1.330(5) . ? N2 C7 1.350(4) . ? N3 C12 1.326(5) . ? N3 C16 1.351(5) . ? N4 C22 1.335(5) . ? N4 C18 1.339(5) . ? N4 Ni2 2.042(3) 3_776 ? C1 C2 1.358(6) . ? C2 C3 1.361(7) . ? C3 C4 1.374(6) . ? C4 C5 1.389(5) . ? C5 C6 1.530(5) . ? C6 C7 1.530(5) . ? C7 C8 1.380(5) . ? C8 C9 1.377(6) . ? C9 C10 1.360(6) . ? C10 C11 1.384(5) . ? C12 C13 1.376(6) . ? C13 C14 1.339(7) . ? C14 C15 1.397(7) . ? C15 C16 1.390(5) . ? C16 C17 1.516(5) . ? C17 C18 1.548(5) . ? C18 C19 1.384(6) . ? C19 C20 1.370(7) . ? C20 C21 1.378(8) . ? C21 C22 1.375(6) . ? C53 O50A 1.30(3) . ? C53 O50 1.500(19) . ? C53 C54 1.547(16) . ? O50 O50A 1.19(5) . ? O50 C51 1.471(19) . ? C52 C51 1.509(18) . ? C51 O50A 1.51(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ni1 N2 156.68(11) . . ? O3 Ni1 N3 78.77(11) . . ? N2 Ni1 N3 97.39(12) . . ? O3 Ni1 O5 107.43(10) . . ? N2 Ni1 O5 94.95(11) . . ? N3 Ni1 O5 84.54(11) . . ? O3 Ni1 O1 81.27(9) . . ? N2 Ni1 O1 77.45(10) . . ? N3 Ni1 O1 104.56(10) . . ? O5 Ni1 O1 168.70(10) . . ? O3 Ni1 Cl1 91.55(7) . . ? N2 Ni1 Cl1 95.09(9) . . ? N3 Ni1 Cl1 166.66(9) . . ? O5 Ni1 Cl1 89.72(8) . . ? O1 Ni1 Cl1 82.73(7) . . ? O1 Ni2 N4 158.76(11) 3_776 3_776 ? O1 Ni2 N1 77.80(10) 3_776 3_776 ? N4 Ni2 N1 99.79(12) 3_776 3_776 ? O1 Ni2 O1 80.67(9) 3_776 . ? N4 Ni2 O1 106.08(11) 3_776 . ? N1 Ni2 O1 153.09(10) 3_776 . ? O1 Ni2 O3 82.02(9) 3_776 3_776 ? N4 Ni2 O3 78.09(11) 3_776 3_776 ? N1 Ni2 O3 103.94(10) 3_776 3_776 ? O1 Ni2 O3 88.75(9) . 3_776 ? O1 Ni2 Cl1 104.54(7) 3_776 . ? N4 Ni2 Cl1 96.31(9) 3_776 . ? N1 Ni2 Cl1 86.55(8) 3_776 . ? O1 Ni2 Cl1 83.41(7) . . ? O3 Ni2 Cl1 168.74(7) 3_776 . ? Ni1 Cl1 Ni2 88.55(4) . . ? C6 O1 Ni2 116.9(2) . 3_776 ? C6 O1 Ni2 128.09(19) . . ? Ni2 O1 Ni2 99.33(9) 3_776 . ? C6 O1 Ni1 107.55(18) . . ? Ni2 O1 Ni1 95.36(9) 3_776 . ? Ni2 O1 Ni1 104.37(10) . . ? C17 O3 Ni1 115.4(2) . . ? C17 O3 Ni2 107.6(2) . 3_776 ? Ni1 O3 Ni2 96.82(10) . 3_776 ? C17 O4 C23 116.4(3) . . ? C24 O5 Ni1 128.6(3) . . ? C5 N1 C1 118.6(3) . . ? C5 N1 Ni2 114.7(2) . 3_776 ? C1 N1 Ni2 126.6(3) . 3_776 ? C11 N2 C7 119.3(3) . . ? C11 N2 Ni1 126.0(3) . . ? C7 N2 Ni1 114.3(2) . . ? C12 N3 C16 117.9(3) . . ? C12 N3 Ni1 127.9(3) . . ? C16 N3 Ni1 113.9(2) . . ? C22 N4 C18 119.8(3) . . ? C22 N4 Ni2 126.7(3) . 3_776 ? C18 N4 Ni2 113.5(2) . 3_776 ? N1 C1 C2 122.2(4) . . ? C1 C2 C3 119.4(4) . . ? C2 C3 C4 119.7(4) . . ? C3 C4 C5 118.3(4) . . ? N1 C5 C4 121.7(3) . . ? N1 C5 C6 116.0(3) . . ? C4 C5 C6 122.1(3) . . ? O1 C6 O2 112.0(3) . . ? O1 C6 C5 108.7(3) . . ? O2 C6 C5 106.9(3) . . ? O1 C6 C7 108.6(3) . . ? O2 C6 C7 108.5(3) . . ? C5 C6 C7 112.3(3) . . ? N2 C7 C8 121.2(3) . . ? N2 C7 C6 115.3(3) . . ? C8 C7 C6 123.5(3) . . ? C7 C8 C9 118.9(4) . . ? C10 C9 C8 119.8(4) . . ? C9 C10 C11 119.1(4) . . ? N2 C11 C10 121.7(4) . . ? N3 C12 C13 123.7(5) . . ? C14 C13 C12 118.7(5) . . ? C13 C14 C15 120.0(4) . . ? C16 C15 C14 118.1(4) . . ? N3 C16 C15 121.6(4) . . ? N3 C16 C17 115.5(3) . . ? C15 C16 C17 122.9(4) . . ? O3 C17 O4 112.8(3) . . ? O3 C17 C16 110.6(3) . . ? O4 C17 C16 102.9(3) . . ? O3 C17 C18 107.5(3) . . ? O4 C17 C18 110.2(3) . . ? C16 C17 C18 112.9(3) . . ? N4 C18 C19 121.1(4) . . ? N4 C18 C17 115.8(3) . . ? C19 C18 C17 123.0(4) . . ? C20 C19 C18 118.2(5) . . ? C19 C20 C21 121.1(5) . . ? C22 C21 C20 117.3(5) . . ? N4 C22 C21 122.4(4) . . ? O50A C53 O50 49(2) . . ? O50A C53 C54 173(2) . . ? O50 C53 C54 127.1(19) . . ? O50A O50 C53 56.6(18) . . ? O50A O50 C51 68(2) . . ? C53 O50 C51 124(3) . . ? O50 C51 C52 133(2) . . ? O50 C51 O50A 47(2) . . ? C52 C51 O50A 177(3) . . ? O50 O50A C53 73.9(17) . . ? O50 O50A C51 64.9(15) . . ? C53 O50A C51 139(2) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.671 _refine_diff_density_min -0.947 _refine_diff_density_rms 0.084 # Attachment '- complex2.cif' data_nibr2nw_0m _database_code_depnum_ccdc_archive 'CCDC 803775' #TrackingRef '- complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H68 Br4 N8 Ni4 O12' _chemical_formula_weight 1599.66 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' Ni Ni 0.3393 1.1124 '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 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 13.6786(3) _cell_length_b 17.2699(4) _cell_length_c 11.9272(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.519(2) _cell_angle_gamma 90.00 _cell_volume 2770.19(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20957 _cell_measurement_theta_min 3.8274 _cell_measurement_theta_max 32.2348 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 4.297 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2921 _exptl_absorpt_correction_T_max 0.5845 _exptl_absorpt_process_details 'CrysAlis RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Excalibur Cappa CCD' _diffrn_measurement_method CrysAlis _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34362 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5408 _reflns_number_gt 4430 _reflns_threshold_expression >2\s(I) _computing_data_collection CrysAlis171.NET _computing_cell_refinement CrysAlis171.NET _computing_data_reduction CrysAlis171.NET _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL-6.31' _computing_publication_material 'Bruker SHELXTL-6.31' _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^ > 2\s(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^)+(0.0720P)^2^+12.4812P] 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 5408 _refine_ls_number_parameters 355 _refine_ls_number_restraints 328 _refine_ls_R_factor_all 0.0603 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1338 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.048 _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 -0.13850(5) 0.51147(4) 0.65107(5) 0.01772(17) Uani 1 1 d U . . Ni2 Ni 0.09456(5) 0.52685(4) 0.58824(5) 0.01799(17) Uani 1 1 d U . . Br1 Br -0.00112(4) 0.60937(3) 0.71068(4) 0.02347(15) Uani 1 1 d U . . Br2 Br 0.46515(5) 0.65284(4) 0.85991(6) 0.0454(2) Uani 1 1 d . . . N1 N -0.1613(3) 0.3689(3) 0.4445(3) 0.0202(9) Uani 1 1 d U . . N2 N -0.0827(3) 0.4321(2) 0.7742(3) 0.0194(8) Uani 1 1 d U . . N3 N -0.2724(3) 0.4568(3) 0.5830(4) 0.0213(9) Uani 1 1 d U . . N4 N -0.1969(3) 0.5171(3) 0.2799(4) 0.0282(10) Uani 1 1 d U . . O1 O -0.0276(2) 0.45123(19) 0.5754(3) 0.0163(7) Uani 1 1 d U . . O2 O 0.0583(3) 0.3340(2) 0.5938(3) 0.0206(7) Uani 1 1 d U . . H2A H 0.0964 0.3643 0.5674 0.031 Uiso 1 1 calc R . . O3 O -0.1684(2) 0.5575(2) 0.4937(3) 0.0203(7) Uani 1 1 d U . . O4 O -0.3213(3) 0.6227(2) 0.4719(3) 0.0301(9) Uani 1 1 d U . . O5 O -0.2253(3) 0.5686(2) 0.7548(3) 0.0269(8) Uani 1 1 d U . . C1 C -0.2372(4) 0.3329(3) 0.3757(5) 0.0260(11) Uani 1 1 d U . . H1 H -0.2663 0.3571 0.3061 0.031 Uiso 1 1 calc R . . C2 C -0.2740(4) 0.2624(3) 0.4029(5) 0.0332(13) Uani 1 1 d U . . H2 H -0.3281 0.2388 0.3534 0.040 Uiso 1 1 calc R . . C3 C -0.2307(4) 0.2267(3) 0.5034(5) 0.0300(12) Uani 1 1 d U . . H3 H -0.2554 0.1784 0.5244 0.036 Uiso 1 1 calc R . . C4 C -0.1505(4) 0.2619(3) 0.5738(5) 0.0242(11) Uani 1 1 d U . . H4 H -0.1191 0.2379 0.6427 0.029 Uiso 1 1 calc R . . C5 C -0.1179(4) 0.3326(3) 0.5409(4) 0.0186(10) Uani 1 1 d U . . C6 C -0.0277(4) 0.3747(3) 0.6108(4) 0.0177(9) Uani 1 1 d U . . C7 C -0.0301(4) 0.3744(3) 0.7395(4) 0.0173(9) Uani 1 1 d U . . C8 C 0.0205(4) 0.3206(3) 0.8138(4) 0.0237(11) Uani 1 1 d U . . H8 H 0.0563 0.2797 0.7865 0.028 Uiso 1 1 calc R . . C9 C 0.0179(4) 0.3274(3) 0.9287(5) 0.0278(12) Uani 1 1 d U . . H9 H 0.0511 0.2906 0.9815 0.033 Uiso 1 1 calc R . . C10 C -0.0337(5) 0.3881(3) 0.9657(4) 0.0288(12) Uani 1 1 d U . . H10 H -0.0346 0.3948 1.0446 0.035 Uiso 1 1 calc R . . C11 C -0.0841(4) 0.4391(3) 0.8855(4) 0.0225(11) Uani 1 1 d U . . H11 H -0.1207 0.4804 0.9104 0.027 Uiso 1 1 calc R . . C12 C -0.3161(4) 0.3973(3) 0.6274(5) 0.0259(11) Uani 1 1 d U . . H12 H -0.2830 0.3752 0.6970 0.031 Uiso 1 1 calc R . . C13 C -0.4063(4) 0.3669(4) 0.5770(6) 0.0334(13) Uani 1 1 d U . . H13 H -0.4346 0.3243 0.6102 0.040 Uiso 1 1 calc R . . C14 C -0.4552(4) 0.4003(4) 0.4757(6) 0.0359(14) Uani 1 1 d U . . H14 H -0.5176 0.3805 0.4387 0.043 Uiso 1 1 calc R . . C15 C -0.4128(4) 0.4620(4) 0.4297(5) 0.0315(12) Uani 1 1 d U . . H15 H -0.4455 0.4858 0.3612 0.038 Uiso 1 1 calc R . . C16 C -0.3206(4) 0.4890(3) 0.4860(4) 0.0248(11) Uani 1 1 d U . . C17 C -0.2676(4) 0.5570(3) 0.4431(4) 0.0253(11) Uani 1 1 d U . . C18 C -0.2712(4) 0.5547(4) 0.3130(5) 0.0337(13) Uani 1 1 d U . . C19 C -0.3458(5) 0.5919(6) 0.2352(6) 0.061(2) Uani 1 1 d U . . H19 H -0.3992 0.6171 0.2611 0.073 Uiso 1 1 calc R . . C20 C -0.3409(5) 0.5914(7) 0.1212(6) 0.072(3) Uani 1 1 d U . . H20 H -0.3903 0.6168 0.0672 0.086 Uiso 1 1 calc R . . C21 C -0.2627(5) 0.5534(6) 0.0869(6) 0.061(2) Uani 1 1 d U . . H21 H -0.2569 0.5530 0.0087 0.074 Uiso 1 1 calc R . . C22 C -0.1922(5) 0.5155(4) 0.1676(5) 0.0382(15) Uani 1 1 d U . . H22 H -0.1398 0.4879 0.1432 0.046 Uiso 1 1 calc R . . C23 C -0.2764(5) 0.6966(4) 0.4600(7) 0.0487(18) Uani 1 1 d U . . H23A H -0.3188 0.7376 0.4817 0.073 Uiso 1 1 calc R . . H23B H -0.2689 0.7039 0.3805 0.073 Uiso 1 1 calc R . . H23C H -0.2109 0.6986 0.5096 0.073 Uiso 1 1 calc R . . C24 C -0.2338(6) 0.6493(4) 0.7747(7) 0.0469(18) Uani 1 1 d U . . H24A H -0.2801 0.6576 0.8273 0.070 Uiso 1 1 calc R . . H24B H -0.2588 0.6756 0.7024 0.070 Uiso 1 1 calc R . . H24C H -0.1684 0.6702 0.8083 0.070 Uiso 1 1 calc R . . O50 O -0.581(2) 0.6176(10) 0.101(2) 0.387(14) Uiso 1 1 d DU . . C51 C -0.6031(6) 0.5458(4) 0.1268(7) 0.0556(19) Uiso 1 1 d DU . . C53 C -0.569(3) 0.6895(16) 0.168(5) 0.57(3) Uiso 1 1 d DU . . C52 C -0.6047(3) 0.4834(3) 0.2009(4) 0.0133(9) Uiso 1 1 d DU . . C54 C -0.4705(18) 0.7311(13) 0.150(2) 0.220(11) Uiso 1 1 d DU . . 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 0.0210(3) 0.0253(3) 0.0078(3) -0.0001(2) 0.0051(2) -0.0003(3) Ni2 0.0196(3) 0.0294(4) 0.0047(3) -0.0003(2) 0.0015(2) -0.0018(3) Br1 0.0294(3) 0.0325(3) 0.0096(2) -0.0047(2) 0.00654(19) -0.0054(2) Br2 0.0452(4) 0.0552(4) 0.0316(4) -0.0046(3) -0.0039(3) 0.0216(3) N1 0.023(2) 0.030(2) 0.0081(19) -0.0042(16) 0.0039(16) -0.0007(18) N2 0.023(2) 0.027(2) 0.0096(19) -0.0001(16) 0.0053(16) -0.0025(17) N3 0.019(2) 0.030(2) 0.015(2) -0.0035(17) 0.0063(16) -0.0001(17) N4 0.021(2) 0.050(3) 0.012(2) 0.003(2) -0.0010(17) -0.007(2) O1 0.0177(16) 0.0260(17) 0.0051(15) 0.0021(13) 0.0020(12) 0.0012(13) O2 0.0209(18) 0.0303(19) 0.0116(17) 0.0019(14) 0.0060(14) 0.0000(15) O3 0.0173(17) 0.0318(19) 0.0115(16) 0.0031(14) 0.0018(13) 0.0026(14) O4 0.0212(19) 0.039(2) 0.032(2) 0.0136(18) 0.0114(17) 0.0060(16) O5 0.029(2) 0.031(2) 0.024(2) -0.0022(16) 0.0123(16) 0.0004(16) C1 0.026(3) 0.038(3) 0.014(3) -0.008(2) 0.003(2) 0.001(2) C2 0.032(3) 0.033(3) 0.033(3) -0.014(2) 0.000(2) -0.005(2) C3 0.034(3) 0.029(3) 0.027(3) -0.008(2) 0.004(2) -0.001(2) C4 0.029(3) 0.024(2) 0.020(3) -0.003(2) 0.005(2) 0.003(2) C5 0.024(2) 0.026(2) 0.007(2) -0.0045(18) 0.0060(18) 0.0018(19) C6 0.022(2) 0.025(2) 0.008(2) 0.0001(18) 0.0060(18) 0.0011(19) C7 0.018(2) 0.028(2) 0.007(2) -0.0014(18) 0.0056(18) -0.0037(19) C8 0.032(3) 0.028(3) 0.012(2) 0.002(2) 0.006(2) -0.001(2) C9 0.037(3) 0.033(3) 0.013(2) 0.007(2) 0.003(2) -0.005(2) C10 0.046(3) 0.032(3) 0.009(2) 0.001(2) 0.006(2) -0.008(2) C11 0.032(3) 0.027(3) 0.010(2) -0.0019(19) 0.010(2) -0.005(2) C12 0.031(3) 0.027(3) 0.023(3) -0.004(2) 0.015(2) -0.001(2) C13 0.029(3) 0.034(3) 0.043(3) -0.006(3) 0.020(3) -0.004(2) C14 0.018(3) 0.044(3) 0.048(4) -0.015(3) 0.013(2) -0.001(2) C15 0.021(3) 0.045(3) 0.028(3) -0.005(2) 0.005(2) 0.004(2) C16 0.024(3) 0.040(3) 0.012(2) -0.002(2) 0.007(2) 0.002(2) C17 0.017(2) 0.042(3) 0.017(2) 0.006(2) 0.0037(19) 0.004(2) C18 0.018(3) 0.067(4) 0.014(2) 0.010(3) 0.000(2) -0.003(3) C19 0.028(3) 0.128(7) 0.026(3) 0.024(4) 0.001(3) 0.016(4) C20 0.032(4) 0.154(9) 0.025(3) 0.028(5) -0.006(3) 0.010(4) C21 0.039(4) 0.128(7) 0.013(3) 0.010(4) -0.006(3) 0.000(4) C22 0.034(3) 0.072(5) 0.008(2) 0.002(3) 0.002(2) -0.006(3) C23 0.039(4) 0.039(3) 0.074(5) 0.023(3) 0.025(4) 0.011(3) C24 0.057(4) 0.033(3) 0.060(5) -0.011(3) 0.034(4) -0.003(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O3 2.011(3) . ? Ni1 N2 2.052(4) . ? Ni1 N3 2.089(4) . ? Ni1 O5 2.110(4) . ? Ni1 O1 2.168(3) . ? Ni1 Br1 2.5312(8) . ? Ni2 O1 2.035(3) 3_566 ? Ni2 N4 2.051(5) 3_566 ? Ni2 N1 2.088(4) 3_566 ? Ni2 O1 2.104(3) . ? Ni2 O3 2.112(4) 3_566 ? Ni2 Br1 2.5641(8) . ? N1 C5 1.348(7) . ? N1 C1 1.352(7) . ? N1 Ni2 2.088(4) 3_566 ? N2 C11 1.336(6) . ? N2 C7 1.339(7) . ? N3 C16 1.342(7) . ? N3 C12 1.345(7) . ? N4 C18 1.326(8) . ? N4 C22 1.352(7) . ? N4 Ni2 2.051(5) 3_566 ? O1 C6 1.388(6) . ? O1 Ni2 2.035(3) 3_566 ? O2 C6 1.415(6) . ? O3 C17 1.380(6) . ? O3 Ni2 2.112(4) 3_566 ? O4 C17 1.428(7) . ? O4 C23 1.433(8) . ? O5 C24 1.421(7) . ? C1 C2 1.379(8) . ? C2 C3 1.382(9) . ? C3 C4 1.393(8) . ? C4 C5 1.381(7) . ? C5 C6 1.540(7) . ? C6 C7 1.541(6) . ? C7 C8 1.379(7) . ? C8 C9 1.382(7) . ? C9 C10 1.381(8) . ? C10 C11 1.389(8) . ? C12 C13 1.375(8) . ? C13 C14 1.394(9) . ? C14 C15 1.375(9) . ? C15 C16 1.397(8) . ? C16 C17 1.517(8) . ? C17 C18 1.544(7) . ? C18 C19 1.403(9) . ? C19 C20 1.374(10) . ? C20 C21 1.380(12) . ? C21 C22 1.395(10) . ? O50 C51 1.329(13) . ? O50 C53 1.471(19) . ? C51 C52 1.395(8) . ? C53 C54 1.57(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 O3 Ni1 N2 156.68(16) . . ? O3 Ni1 N3 78.54(16) . . ? N2 Ni1 N3 99.28(17) . . ? O3 Ni1 O5 108.76(15) . . ? N2 Ni1 O5 93.93(16) . . ? N3 Ni1 O5 83.80(16) . . ? O3 Ni1 O1 80.80(13) . . ? N2 Ni1 O1 77.29(14) . . ? N3 Ni1 O1 104.59(14) . . ? O5 Ni1 O1 168.61(14) . . ? O3 Ni1 Br1 90.70(10) . . ? N2 Ni1 Br1 94.88(12) . . ? N3 Ni1 Br1 164.70(13) . . ? O5 Ni1 Br1 89.51(11) . . ? O1 Ni1 Br1 84.10(9) . . ? O1 Ni2 N4 158.36(17) 3_566 3_566 ? O1 Ni2 N1 78.21(15) 3_566 3_566 ? N4 Ni2 N1 101.65(18) 3_566 3_566 ? O1 Ni2 O1 80.40(14) 3_566 . ? N4 Ni2 O1 104.36(16) 3_566 . ? N1 Ni2 O1 152.91(15) 3_566 . ? O1 Ni2 O3 81.63(13) 3_566 3_566 ? N4 Ni2 O3 77.43(17) 3_566 3_566 ? N1 Ni2 O3 104.25(15) 3_566 3_566 ? O1 Ni2 O3 88.78(13) . 3_566 ? O1 Ni2 Br1 104.81(10) 3_566 . ? N4 Ni2 Br1 96.70(14) 3_566 . ? N1 Ni2 Br1 85.03(11) 3_566 . ? O1 Ni2 Br1 84.57(9) . . ? O3 Ni2 Br1 169.78(10) 3_566 . ? Ni1 Br1 Ni2 84.19(2) . . ? C5 N1 C1 118.3(5) . . ? C5 N1 Ni2 114.9(3) . 3_566 ? C1 N1 Ni2 126.6(4) . 3_566 ? C11 N2 C7 118.8(4) . . ? C11 N2 Ni1 125.4(4) . . ? C7 N2 Ni1 115.2(3) . . ? C16 N3 C12 118.2(5) . . ? C16 N3 Ni1 113.9(4) . . ? C12 N3 Ni1 127.8(4) . . ? C18 N4 C22 118.8(5) . . ? C18 N4 Ni2 113.9(4) . 3_566 ? C22 N4 Ni2 127.1(4) . 3_566 ? C6 O1 Ni2 116.3(3) . 3_566 ? C6 O1 Ni2 127.9(3) . . ? Ni2 O1 Ni2 99.60(14) 3_566 . ? C6 O1 Ni1 106.9(3) . . ? Ni2 O1 Ni1 94.76(13) 3_566 . ? Ni2 O1 Ni1 106.19(14) . . ? C17 O3 Ni1 114.9(3) . . ? C17 O3 Ni2 108.0(3) . 3_566 ? Ni1 O3 Ni2 97.23(15) . 3_566 ? C17 O4 C23 115.8(4) . . ? C24 O5 Ni1 129.0(4) . . ? N1 C1 C2 122.5(5) . . ? C3 C2 C1 118.7(5) . . ? C2 C3 C4 119.6(5) . . ? C5 C4 C3 118.3(5) . . ? N1 C5 C4 122.6(5) . . ? N1 C5 C6 115.3(4) . . ? C4 C5 C6 122.2(5) . . ? O1 C6 O2 112.5(4) . . ? O1 C6 C7 107.9(4) . . ? O2 C6 C7 108.1(4) . . ? O1 C6 C5 109.3(4) . . ? O2 C6 C5 107.0(4) . . ? C7 C6 C5 112.1(4) . . ? N2 C7 C8 122.5(4) . . ? N2 C7 C6 114.6(4) . . ? C8 C7 C6 122.9(5) . . ? C7 C8 C9 118.6(5) . . ? C10 C9 C8 119.3(5) . . ? C9 C10 C11 118.7(5) . . ? N2 C11 C10 122.1(5) . . ? N3 C12 C13 123.2(6) . . ? C12 C13 C14 118.1(6) . . ? C15 C14 C13 119.8(6) . . ? C14 C15 C16 118.4(6) . . ? N3 C16 C15 122.3(5) . . ? N3 C16 C17 115.0(5) . . ? C15 C16 C17 122.7(5) . . ? O3 C17 O4 113.4(5) . . ? O3 C17 C16 110.5(4) . . ? O4 C17 C16 103.7(4) . . ? O3 C17 C18 106.7(4) . . ? O4 C17 C18 109.8(4) . . ? C16 C17 C18 113.0(5) . . ? N4 C18 C19 122.1(6) . . ? N4 C18 C17 115.2(5) . . ? C19 C18 C17 122.6(6) . . ? C20 C19 C18 119.5(7) . . ? C19 C20 C21 118.4(7) . . ? C20 C21 C22 119.6(6) . . ? N4 C22 C21 121.5(6) . . ? C51 O50 C53 132(2) . . ? O50 C51 C52 154.1(13) . . ? O50 C53 C54 108.9(19) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.586 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.139 # Attachment '- complex3.cif' data_tdk672_0ma _database_code_depnum_ccdc_archive 'CCDC 803776' #TrackingRef '- complex3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50.50 H51.75 I2 N8 Ni3 O10.50' _chemical_formula_weight 1368.68 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 24.004(2) _cell_length_b 15.6042(14) _cell_length_c 15.6950(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.9160(10) _cell_angle_gamma 90.00 _cell_volume 5790.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9990 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 25.93 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2739 _exptl_absorpt_coefficient_mu 2.092 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5280 _exptl_absorpt_correction_T_max 0.7874 _exptl_absorpt_process_details 'Bruker SADABS' _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 'Bruker APEX-II CCD' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34516 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11340 _reflns_number_gt 8610 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0954P)^2^+9.9589P] 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 none _refine_ls_number_reflns 11340 _refine_ls_number_parameters 659 _refine_ls_number_restraints 687 _refine_ls_R_factor_all 0.0756 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1804 _refine_ls_wR_factor_gt 0.1700 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.004 _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 0.19072(2) 0.48241(4) 0.23880(3) 0.03318(15) Uani 1 1 d U . . Ni2 Ni 0.25529(3) 0.40737(5) 0.38636(4) 0.0518(2) Uani 1 1 d U . . Ni3 Ni 0.31043(2) 0.55194(4) 0.33297(4) 0.03543(15) Uani 1 1 d U . . I1 I 0.389360(19) 0.93821(3) 0.36931(3) 0.07659(17) Uani 1 1 d . . . I2A I 0.10348(8) -0.03859(10) 0.2659(3) 0.1696(13) Uani 0.607(6) 1 d P . . I2B I 0.0848(4) 0.5575(3) -0.1552(9) 0.347(9) Uani 0.393(6) 1 d P . . N1 N 0.15265(16) 0.3815(3) 0.1664(2) 0.0394(8) Uani 1 1 d U . . N2 N 0.25084(18) 0.2801(3) 0.3769(3) 0.0476(9) Uani 1 1 d U . . N3 N 0.12548(16) 0.5622(3) 0.2529(3) 0.0398(8) Uani 1 1 d U . . N4 N 0.28119(16) 0.6648(2) 0.2707(2) 0.0389(8) Uani 1 1 d U . . N5 N 0.21523(17) 0.5472(2) 0.1362(2) 0.0388(8) Uani 1 1 d U . . N6 N 0.37446(17) 0.5283(3) 0.2662(3) 0.0451(9) Uani 1 1 d U . . N7 N 0.25891(18) 0.4202(3) 0.5136(3) 0.0473(9) Uani 1 1 d U . . N8 N 0.35218(16) 0.6130(3) 0.4429(2) 0.0415(8) Uani 1 1 d U . . O1 O 0.17620(13) 0.39885(19) 0.33329(19) 0.0366(6) Uani 1 1 d U . . O2 O 0.10822(14) 0.2967(2) 0.3486(2) 0.0474(8) Uani 1 1 d U . . O3 O 0.22805(13) 0.55317(19) 0.34843(19) 0.0344(6) Uani 1 1 d U . . O4 O 0.21062(15) 0.6729(2) 0.4286(2) 0.0464(8) Uani 1 1 d U . . O5 O 0.27410(13) 0.44957(19) 0.25187(19) 0.0360(6) Uani 1 1 d U . . O6 O 0.28838(16) 0.3780(2) 0.1266(2) 0.0506(8) Uani 1 1 d U . . O7 O 0.33205(14) 0.4501(2) 0.41487(19) 0.0408(7) Uani 1 1 d U . . O8 O 0.39814(16) 0.4135(3) 0.5344(2) 0.0597(10) Uani 1 1 d U . . C1 C 0.1397(2) 0.3782(4) 0.0803(3) 0.0557(13) Uani 1 1 d U . . H1 H 0.1495 0.4244 0.0485 0.067 Uiso 1 1 calc R . . C2 C 0.1124(3) 0.3098(4) 0.0364(3) 0.0612(14) Uani 1 1 d U . . H2 H 0.1039 0.3100 -0.0236 0.073 Uiso 1 1 calc R . . C3 C 0.0980(3) 0.2417(4) 0.0823(4) 0.0614(14) Uani 1 1 d U . . H3 H 0.0791 0.1950 0.0541 0.074 Uiso 1 1 calc R . . C4 C 0.1118(2) 0.2433(3) 0.1706(3) 0.0522(12) Uani 1 1 d U . . H4 H 0.1027 0.1971 0.2030 0.063 Uiso 1 1 calc R . . C5 C 0.13961(19) 0.3141(3) 0.2114(3) 0.0375(9) Uani 1 1 d U . . C6 C 0.15634(19) 0.3195(3) 0.3104(3) 0.0367(9) Uani 1 1 d U . . C7 C 0.1994(2) 0.2504(3) 0.3457(3) 0.0390(9) Uani 1 1 d U . . C8 C 0.1871(3) 0.1642(3) 0.3507(3) 0.0511(12) Uani 1 1 d U . . H8 H 0.1509 0.1443 0.3294 0.061 Uiso 1 1 calc R . . C9 C 0.2279(3) 0.1089(4) 0.3865(4) 0.0638(15) Uani 1 1 d U . . H9 H 0.2196 0.0510 0.3912 0.077 Uiso 1 1 calc R . . C10 C 0.2813(3) 0.1387(4) 0.4159(4) 0.0680(16) Uani 1 1 d U . . H10 H 0.3102 0.1014 0.4391 0.082 Uiso 1 1 calc R . . C11 C 0.2912(3) 0.2244(4) 0.4105(4) 0.0640(15) Uani 1 1 d U . . H11 H 0.3274 0.2450 0.4310 0.077 Uiso 1 1 calc R . . C12 C 0.0633(2) 0.3568(4) 0.3319(5) 0.0703(17) Uani 1 1 d U . . H12A H 0.0325 0.3380 0.3591 0.105 Uiso 1 1 calc R . . H12B H 0.0506 0.3614 0.2706 0.105 Uiso 1 1 calc R . . H12C H 0.0763 0.4118 0.3546 0.105 Uiso 1 1 calc R . . C13 C 0.0715(2) 0.5540(4) 0.2162(4) 0.0541(13) Uani 1 1 d U . . H13 H 0.0611 0.5095 0.1773 0.065 Uiso 1 1 calc R . . C14 C 0.0302(3) 0.6099(5) 0.2345(5) 0.0738(18) Uani 1 1 d U . . H14 H -0.0074 0.6029 0.2085 0.089 Uiso 1 1 calc R . . C15 C 0.0457(3) 0.6760(5) 0.2916(5) 0.0776(19) Uani 1 1 d U . . H15 H 0.0188 0.7150 0.3036 0.093 Uiso 1 1 calc R . . C16 C 0.1011(2) 0.6838(4) 0.3308(4) 0.0591(14) Uani 1 1 d U . . H16 H 0.1122 0.7269 0.3710 0.071 Uiso 1 1 calc R . . C17 C 0.14036(19) 0.6258(3) 0.3090(3) 0.0407(10) Uani 1 1 d U . . C18 C 0.20365(18) 0.6323(3) 0.3465(3) 0.0361(9) Uani 1 1 d U . . C20 C 0.23310(19) 0.6943(3) 0.2924(3) 0.0378(9) Uani 1 1 d U . . C21 C 0.2129(2) 0.7752(3) 0.2688(3) 0.0510(12) Uani 1 1 d U . . H21 H 0.1796 0.7947 0.2851 0.061 Uiso 1 1 calc R . . C22 C 0.2418(3) 0.8256(4) 0.2222(4) 0.0598(14) Uani 1 1 d U . . H22 H 0.2287 0.8804 0.2062 0.072 Uiso 1 1 calc R . . C23 C 0.2905(3) 0.7961(4) 0.1984(4) 0.0601(14) Uani 1 1 d U . . H23 H 0.3105 0.8298 0.1651 0.072 Uiso 1 1 calc R . . C25 C 0.3093(2) 0.7159(3) 0.2244(3) 0.0510(12) Uani 1 1 d U . . H25 H 0.3429 0.6962 0.2094 0.061 Uiso 1 1 calc R . . C26 C 0.1937(3) 0.6214(4) 0.4946(4) 0.0691(17) Uani 1 1 d U . . H26A H 0.1995 0.6525 0.5481 0.104 Uiso 1 1 calc R . . H26B H 0.2157 0.5697 0.5014 0.104 Uiso 1 1 calc R . . H26C H 0.1543 0.6072 0.4787 0.104 Uiso 1 1 calc R . . C27 C 0.1859(2) 0.6054(3) 0.0860(3) 0.0502(12) Uani 1 1 d U . . H27 H 0.1512 0.6227 0.0986 0.060 Uiso 1 1 calc R . . C28 C 0.2043(3) 0.6415(4) 0.0165(4) 0.0609(14) Uani 1 1 d U . . H28 H 0.1824 0.6823 -0.0172 0.073 Uiso 1 1 calc R . . C29 C 0.2551(3) 0.6168(4) -0.0028(4) 0.0607(14) Uani 1 1 d U . . H29 H 0.2682 0.6408 -0.0499 0.073 Uiso 1 1 calc R . . C30 C 0.2866(3) 0.5567(3) 0.0472(3) 0.0516(12) Uani 1 1 d U . . H30 H 0.3214 0.5392 0.0350 0.062 Uiso 1 1 calc R . . C31 C 0.2654(2) 0.5222(3) 0.1171(3) 0.0395(10) Uani 1 1 d U . . C32 C 0.2967(2) 0.4538(3) 0.1771(3) 0.0402(10) Uani 1 1 d U . . C33 C 0.3593(2) 0.4758(3) 0.1979(3) 0.0461(11) Uani 1 1 d U . . C34 C 0.3981(3) 0.4493(5) 0.1482(5) 0.0716(17) Uani 1 1 d U . . H34 H 0.3870 0.4135 0.1010 0.086 Uiso 1 1 calc R . . C35 C 0.4532(3) 0.4760(5) 0.1687(6) 0.087(2) Uani 1 1 d U . . H35 H 0.4798 0.4584 0.1356 0.104 Uiso 1 1 calc R . . C36 C 0.4685(3) 0.5278(5) 0.2372(5) 0.0810(19) Uani 1 1 d U . . H36 H 0.5058 0.5459 0.2524 0.097 Uiso 1 1 calc R . . C37 C 0.4279(2) 0.5541(4) 0.2850(4) 0.0609(14) Uani 1 1 d U . . H37 H 0.4385 0.5908 0.3317 0.073 Uiso 1 1 calc R . . C38 C 0.3048(3) 0.3008(4) 0.1731(4) 0.0754(19) Uani 1 1 d U . . H38A H 0.2978 0.2528 0.1345 0.113 Uiso 1 1 calc R . . H38B H 0.2833 0.2944 0.2189 0.113 Uiso 1 1 calc R . . H38C H 0.3443 0.3033 0.1971 0.113 Uiso 1 1 calc R . . C39 C 0.2167(3) 0.4033(4) 0.5580(4) 0.0655(16) Uani 1 1 d U . . H39 H 0.1824 0.3827 0.5282 0.079 Uiso 1 1 calc R . . C40 C 0.2227(3) 0.4153(4) 0.6449(4) 0.0719(17) Uani 1 1 d U . . H40 H 0.1929 0.4034 0.6740 0.086 Uiso 1 1 calc R . . C41 C 0.2721(4) 0.4443(4) 0.6877(4) 0.0752(19) Uani 1 1 d U . . H41 H 0.2764 0.4542 0.7470 0.090 Uiso 1 1 calc R . . C42 C 0.3170(3) 0.4600(4) 0.6447(4) 0.0608(15) Uani 1 1 d U . . H42 H 0.3520 0.4775 0.6745 0.073 Uiso 1 1 calc R . . C43 C 0.3077(2) 0.4487(3) 0.5564(3) 0.0436(10) Uani 1 1 d U . . C44 C 0.3522(2) 0.4683(3) 0.4994(3) 0.0428(10) Uani 1 1 d U . . C45 C 0.3716(2) 0.5613(3) 0.5090(3) 0.0437(10) Uani 1 1 d U . . C46 C 0.4060(2) 0.5915(4) 0.5820(4) 0.0606(14) Uani 1 1 d U . . H46 H 0.4199 0.5541 0.6267 0.073 Uiso 1 1 calc R . . C47 C 0.4200(3) 0.6775(5) 0.5888(4) 0.0717(17) Uani 1 1 d U . . H47 H 0.4433 0.6986 0.6377 0.086 Uiso 1 1 calc R . . C48 C 0.3984(3) 0.7313(4) 0.5211(4) 0.0670(16) Uani 1 1 d U . . H48 H 0.4062 0.7897 0.5243 0.080 Uiso 1 1 calc R . . C49 C 0.3656(2) 0.6971(4) 0.4495(4) 0.0541(12) Uani 1 1 d U . . H49 H 0.3519 0.7331 0.4035 0.065 Uiso 1 1 calc R . . C50 C 0.4410(3) 0.4085(5) 0.4823(5) 0.083(2) Uani 1 1 d U . . H50A H 0.4706 0.3710 0.5092 0.124 Uiso 1 1 calc R . . H50B H 0.4563 0.4646 0.4763 0.124 Uiso 1 1 calc R . . H50C H 0.4251 0.3866 0.4262 0.124 Uiso 1 1 calc R . . O60 O 0.4608(5) 0.7432(8) 0.8039(8) 0.204(4) Uiso 1 1 d DU . . C60 C 0.5194(7) 0.7465(12) 0.8283(11) 0.209(7) Uiso 1 1 d DU . . H60A H 0.5294 0.7938 0.8670 0.314 Uiso 1 1 calc R . . H60B H 0.5365 0.7539 0.7778 0.314 Uiso 1 1 calc R . . H60C H 0.5326 0.6941 0.8568 0.314 Uiso 1 1 calc R . . O61 O 0.4421(9) 0.1467(14) 0.4548(14) 0.344(10) Uiso 1 1 d DU . . C61 C 0.4396(10) 0.1720(16) 0.3731(15) 0.281(11) Uiso 1 1 d DU . . H61A H 0.4107 0.1404 0.3363 0.422 Uiso 1 1 calc R . . H61B H 0.4754 0.1618 0.3555 0.422 Uiso 1 1 calc R . . H61C H 0.4309 0.2321 0.3685 0.422 Uiso 1 1 calc R . . C62 C 0.0418(9) 0.6755(14) 0.0055(14) 0.150(7) Uiso 0.607(6) 1 d PDU . . H62A H 0.0067 0.6981 0.0170 0.225 Uiso 0.607(6) 1 calc PR . . H62B H 0.0588 0.7158 -0.0284 0.225 Uiso 0.607(6) 1 calc PR . . H62C H 0.0668 0.6653 0.0592 0.225 Uiso 0.607(6) 1 calc PR . . O62 O 0.0321(10) 0.6011(15) -0.0384(15) 0.242(9) Uiso 0.607(6) 1 d PDU . . 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 0.0367(3) 0.0310(3) 0.0319(3) 0.0014(2) 0.0061(2) -0.0010(2) Ni2 0.0570(4) 0.0504(4) 0.0426(4) 0.0117(3) -0.0063(3) -0.0166(3) Ni3 0.0336(3) 0.0368(3) 0.0360(3) 0.0022(2) 0.0063(2) -0.0008(2) I1 0.0611(3) 0.0794(3) 0.0912(3) 0.0152(2) 0.0185(2) 0.0002(2) I2A 0.0810(8) 0.0675(8) 0.369(4) -0.0307(12) 0.0634(14) 0.0016(6) I2B 0.227(7) 0.139(3) 0.568(17) 0.088(6) -0.233(9) -0.107(4) N1 0.045(2) 0.042(2) 0.0325(17) -0.0026(16) 0.0087(15) -0.0038(17) N2 0.052(2) 0.047(2) 0.043(2) 0.0115(18) 0.0084(18) 0.0027(18) N3 0.0362(19) 0.040(2) 0.043(2) -0.0001(16) 0.0062(16) -0.0008(16) N4 0.039(2) 0.038(2) 0.0388(19) 0.0046(16) 0.0060(15) -0.0036(16) N5 0.046(2) 0.034(2) 0.0369(18) 0.0049(15) 0.0069(16) -0.0023(16) N6 0.0370(19) 0.049(2) 0.051(2) 0.0063(18) 0.0123(17) -0.0002(17) N7 0.048(2) 0.050(2) 0.044(2) 0.0110(18) 0.0068(17) -0.0011(19) N8 0.039(2) 0.043(2) 0.042(2) -0.0023(16) 0.0055(16) -0.0027(17) O1 0.0449(16) 0.0319(15) 0.0348(15) -0.0014(12) 0.0116(13) -0.0052(13) O2 0.0482(18) 0.0436(19) 0.0558(19) 0.0021(16) 0.0244(16) -0.0054(15) O3 0.0369(15) 0.0306(15) 0.0358(15) -0.0021(12) 0.0070(12) -0.0003(12) O4 0.060(2) 0.0415(19) 0.0388(16) -0.0104(14) 0.0114(15) -0.0008(16) O5 0.0387(15) 0.0363(16) 0.0342(14) 0.0005(12) 0.0100(12) 0.0026(13) O6 0.072(2) 0.0380(18) 0.0458(18) -0.0061(15) 0.0222(17) 0.0017(17) O7 0.0462(17) 0.0393(17) 0.0356(15) 0.0017(13) 0.0036(13) 0.0007(14) O8 0.054(2) 0.065(2) 0.056(2) 0.0093(19) -0.0051(17) 0.0148(19) C1 0.070(4) 0.064(3) 0.034(2) -0.004(2) 0.010(2) -0.016(3) C2 0.074(4) 0.069(4) 0.039(3) -0.014(2) 0.006(3) -0.008(3) C3 0.070(4) 0.057(3) 0.055(3) -0.020(3) 0.004(3) -0.010(3) C4 0.058(3) 0.041(3) 0.054(3) -0.006(2) 0.001(2) -0.008(2) C5 0.038(2) 0.034(2) 0.041(2) -0.0035(18) 0.0092(18) 0.0008(18) C6 0.041(2) 0.033(2) 0.038(2) -0.0008(18) 0.0125(18) -0.0045(18) C7 0.051(2) 0.037(2) 0.032(2) 0.0028(18) 0.0126(18) 0.0013(19) C8 0.067(3) 0.043(3) 0.046(3) 0.004(2) 0.017(2) 0.003(2) C9 0.098(4) 0.044(3) 0.051(3) 0.006(2) 0.019(3) 0.012(3) C10 0.089(4) 0.064(4) 0.051(3) 0.019(3) 0.014(3) 0.032(3) C11 0.056(3) 0.077(4) 0.058(3) 0.019(3) 0.007(3) 0.010(3) C12 0.050(3) 0.072(4) 0.097(5) 0.007(4) 0.033(3) 0.005(3) C13 0.043(3) 0.053(3) 0.063(3) -0.001(3) 0.002(2) -0.003(2) C14 0.038(3) 0.080(4) 0.100(5) -0.001(4) 0.001(3) 0.006(3) C15 0.049(3) 0.072(4) 0.113(5) -0.010(4) 0.016(3) 0.015(3) C16 0.050(3) 0.049(3) 0.080(4) -0.012(3) 0.018(3) 0.007(2) C17 0.039(2) 0.039(2) 0.046(2) 0.000(2) 0.0113(19) 0.0025(19) C18 0.037(2) 0.033(2) 0.038(2) -0.0040(18) 0.0058(17) 0.0005(18) C20 0.041(2) 0.035(2) 0.036(2) -0.0023(18) 0.0021(18) -0.0021(18) C21 0.055(3) 0.042(3) 0.056(3) 0.005(2) 0.008(2) 0.005(2) C22 0.074(4) 0.038(3) 0.066(3) 0.010(3) 0.008(3) -0.002(3) C23 0.073(4) 0.046(3) 0.062(3) 0.015(3) 0.014(3) -0.010(3) C25 0.055(3) 0.047(3) 0.052(3) 0.007(2) 0.011(2) -0.007(2) C26 0.097(5) 0.070(4) 0.044(3) 0.000(3) 0.026(3) 0.014(4) C27 0.057(3) 0.042(3) 0.049(3) 0.010(2) 0.002(2) 0.001(2) C28 0.080(4) 0.050(3) 0.049(3) 0.019(2) 0.002(3) -0.005(3) C29 0.088(4) 0.052(3) 0.045(3) 0.012(2) 0.018(3) -0.009(3) C30 0.070(3) 0.048(3) 0.042(3) -0.001(2) 0.025(2) -0.010(2) C31 0.051(3) 0.037(2) 0.031(2) -0.0024(18) 0.0102(18) -0.007(2) C32 0.050(2) 0.039(2) 0.034(2) -0.0035(18) 0.0147(19) 0.0032(19) C33 0.046(2) 0.047(3) 0.049(3) 0.005(2) 0.018(2) 0.006(2) C34 0.064(3) 0.082(5) 0.077(4) -0.009(3) 0.036(3) 0.005(3) C35 0.061(4) 0.101(6) 0.109(5) -0.006(4) 0.047(4) 0.006(4) C36 0.039(3) 0.102(6) 0.107(5) 0.010(4) 0.025(3) -0.002(3) C37 0.043(3) 0.069(4) 0.072(4) 0.007(3) 0.011(2) -0.005(3) C38 0.108(5) 0.046(3) 0.078(4) -0.003(3) 0.032(4) 0.017(3) C39 0.059(3) 0.074(4) 0.065(3) 0.019(3) 0.015(3) -0.015(3) C40 0.085(4) 0.069(4) 0.072(4) 0.010(3) 0.040(3) -0.014(3) C41 0.114(5) 0.068(4) 0.048(3) 0.002(3) 0.027(3) -0.021(4) C42 0.078(4) 0.060(4) 0.044(3) 0.000(3) 0.008(3) -0.016(3) C43 0.052(3) 0.037(2) 0.041(2) 0.005(2) 0.005(2) 0.000(2) C44 0.040(2) 0.047(3) 0.039(2) 0.004(2) 0.0004(18) 0.004(2) C45 0.037(2) 0.051(3) 0.042(2) -0.001(2) 0.0052(19) -0.004(2) C46 0.057(3) 0.068(3) 0.051(3) 0.003(3) -0.007(2) -0.013(3) C47 0.071(4) 0.082(4) 0.057(3) -0.010(3) -0.006(3) -0.028(3) C48 0.074(4) 0.057(3) 0.068(4) -0.010(3) 0.006(3) -0.026(3) C49 0.053(3) 0.047(3) 0.060(3) -0.002(2) 0.003(2) -0.007(2) C50 0.054(4) 0.094(5) 0.100(5) 0.003(4) 0.012(3) 0.021(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N3 2.042(4) . ? Ni1 O5 2.042(3) . ? Ni1 O1 2.049(3) . ? Ni1 N1 2.061(4) . ? Ni1 N5 2.070(4) . ? Ni1 O3 2.110(3) . ? Ni1 Ni2 2.8109(9) . ? Ni2 O7 1.938(3) . ? Ni2 O1 1.942(3) . ? Ni2 N2 1.993(5) . ? Ni2 N7 1.994(4) . ? Ni2 O5 2.328(3) . ? Ni2 Ni3 2.8151(9) . ? Ni3 O3 2.033(3) . ? Ni3 N6 2.038(4) . ? Ni3 O7 2.054(3) . ? Ni3 N8 2.072(4) . ? Ni3 N4 2.076(4) . ? Ni3 O5 2.133(3) . ? I2A I2B 1.418(15) 4_566 ? I2B I2A 1.418(15) 4_565 ? N1 C5 1.333(6) . ? N1 C1 1.335(6) . ? N2 C7 1.330(6) . ? N2 C11 1.340(7) . ? N3 C13 1.331(7) . ? N3 C17 1.335(6) . ? N4 C25 1.338(6) . ? N4 C20 1.340(6) . ? N5 C27 1.324(6) . ? N5 C31 1.347(6) . ? N6 C37 1.328(7) . ? N6 C33 1.348(7) . ? N7 C43 1.322(7) . ? N7 C39 1.351(7) . ? N8 C45 1.334(6) . ? N8 C49 1.351(7) . ? O1 C6 1.354(5) . ? O2 C12 1.420(7) . ? O2 C6 1.435(5) . ? O3 C18 1.365(5) . ? O4 C18 1.419(5) . ? O4 C26 1.424(7) . ? O5 C32 1.377(5) . ? O6 C32 1.418(6) . ? O6 C38 1.429(7) . ? O7 C44 1.361(5) . ? O8 C50 1.423(8) . ? O8 C44 1.429(6) . ? C1 C2 1.373(8) . ? C2 C3 1.360(9) . ? C3 C4 1.368(8) . ? C4 C5 1.389(7) . ? C5 C6 1.538(6) . ? C6 C7 1.531(6) . ? C7 C8 1.381(7) . ? C8 C9 1.352(8) . ? C9 C10 1.367(10) . ? C10 C11 1.363(9) . ? C13 C14 1.387(9) . ? C14 C15 1.374(10) . ? C15 C16 1.372(9) . ? C16 C17 1.390(7) . ? C17 C18 1.535(6) . ? C18 C20 1.538(6) . ? C20 C21 1.380(7) . ? C21 C22 1.346(8) . ? C22 C23 1.368(9) . ? C23 C25 1.369(8) . ? C27 C28 1.366(7) . ? C28 C29 1.362(9) . ? C29 C30 1.366(8) . ? C30 C31 1.395(6) . ? C31 C32 1.532(7) . ? C32 C33 1.522(7) . ? C33 C34 1.378(7) . ? C34 C35 1.371(10) . ? C35 C36 1.345(11) . ? C36 C37 1.390(9) . ? C39 C40 1.359(9) . ? C40 C41 1.338(10) . ? C41 C42 1.389(9) . ? C42 C43 1.378(7) . ? C43 C44 1.536(7) . ? C44 C45 1.524(7) . ? C45 C46 1.375(7) . ? C46 C47 1.382(9) . ? C47 C48 1.383(9) . ? C48 C49 1.365(8) . ? O60 C60 1.392(13) . ? O61 C61 1.334(16) . ? C62 O62 1.349(16) . ? 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 N3 Ni1 O5 154.01(14) . . ? N3 Ni1 O1 94.61(14) . . ? O5 Ni1 O1 93.07(12) . . ? N3 Ni1 N1 104.47(16) . . ? O5 Ni1 N1 101.39(14) . . ? O1 Ni1 N1 78.35(13) . . ? N3 Ni1 N5 96.47(16) . . ? O5 Ni1 N5 78.21(14) . . ? O1 Ni1 N5 168.52(14) . . ? N1 Ni1 N5 95.90(15) . . ? N3 Ni1 O3 79.56(14) . . ? O5 Ni1 O3 77.18(12) . . ? O1 Ni1 O3 81.03(12) . . ? N1 Ni1 O3 159.23(13) . . ? N5 Ni1 O3 103.95(14) . . ? N3 Ni1 Ni2 119.28(11) . . ? O5 Ni1 Ni2 54.60(8) . . ? O1 Ni1 Ni2 43.70(9) . . ? N1 Ni1 Ni2 105.37(11) . . ? N5 Ni1 Ni2 130.83(11) . . ? O3 Ni1 Ni2 56.60(8) . . ? O7 Ni2 O1 160.56(13) . . ? O7 Ni2 N2 113.37(16) . . ? O1 Ni2 N2 82.17(15) . . ? O7 Ni2 N7 81.87(15) . . ? O1 Ni2 N7 107.88(15) . . ? N2 Ni2 N7 99.64(17) . . ? O7 Ni2 O5 77.70(12) . . ? O1 Ni2 O5 87.62(11) . . ? N2 Ni2 O5 103.32(14) . . ? N7 Ni2 O5 153.87(15) . . ? O7 Ni2 Ni1 114.48(9) . . ? O1 Ni2 Ni1 46.80(9) . . ? N2 Ni2 Ni1 109.79(12) . . ? N7 Ni2 Ni1 134.91(13) . . ? O5 Ni2 Ni1 45.63(8) . . ? O7 Ni2 Ni3 46.84(9) . . ? O1 Ni2 Ni3 113.72(9) . . ? N2 Ni2 Ni3 142.95(12) . . ? N7 Ni2 Ni3 106.03(13) . . ? O5 Ni2 Ni3 47.86(8) . . ? Ni1 Ni2 Ni3 69.01(2) . . ? O3 Ni3 N6 153.93(15) . . ? O3 Ni3 O7 94.52(13) . . ? N6 Ni3 O7 92.90(15) . . ? O3 Ni3 N8 103.72(14) . . ? N6 Ni3 N8 102.24(16) . . ? O7 Ni3 N8 78.51(14) . . ? O3 Ni3 N4 77.95(13) . . ? N6 Ni3 N4 97.76(16) . . ? O7 Ni3 N4 168.30(14) . . ? N8 Ni3 N4 94.45(15) . . ? O3 Ni3 O5 76.83(11) . . ? N6 Ni3 O5 79.90(15) . . ? O7 Ni3 O5 80.05(12) . . ? N8 Ni3 O5 158.54(14) . . ? N4 Ni3 O5 106.50(14) . . ? O3 Ni3 Ni2 57.00(9) . . ? N6 Ni3 Ni2 116.31(12) . . ? O7 Ni3 Ni2 43.50(9) . . ? N8 Ni3 Ni2 107.78(11) . . ? N4 Ni3 Ni2 132.96(11) . . ? O5 Ni3 Ni2 54.04(8) . . ? C5 N1 C1 118.1(4) . . ? C5 N1 Ni1 115.7(3) . . ? C1 N1 Ni1 126.3(4) . . ? C7 N2 C11 118.7(5) . . ? C7 N2 Ni2 114.2(3) . . ? C11 N2 Ni2 126.2(4) . . ? C13 N3 C17 119.1(4) . . ? C13 N3 Ni1 127.1(4) . . ? C17 N3 Ni1 113.7(3) . . ? C25 N4 C20 118.1(4) . . ? C25 N4 Ni3 126.8(3) . . ? C20 N4 Ni3 114.1(3) . . ? C27 N5 C31 118.0(4) . . ? C27 N5 Ni1 127.3(4) . . ? C31 N5 Ni1 114.6(3) . . ? C37 N6 C33 118.6(5) . . ? C37 N6 Ni3 128.0(4) . . ? C33 N6 Ni3 113.2(3) . . ? C43 N7 C39 118.8(5) . . ? C43 N7 Ni2 115.1(3) . . ? C39 N7 Ni2 126.1(4) . . ? C45 N8 C49 118.7(4) . . ? C45 N8 Ni3 115.1(3) . . ? C49 N8 Ni3 125.8(4) . . ? C6 O1 Ni2 116.8(3) . . ? C6 O1 Ni1 119.1(3) . . ? Ni2 O1 Ni1 89.50(12) . . ? C12 O2 C6 113.6(4) . . ? C18 O3 Ni3 115.4(3) . . ? C18 O3 Ni1 109.6(2) . . ? Ni3 O3 Ni1 100.54(12) . . ? C18 O4 C26 113.9(4) . . ? C32 O5 Ni1 115.2(3) . . ? C32 O5 Ni3 107.0(3) . . ? Ni1 O5 Ni3 99.50(12) . . ? C32 O5 Ni2 162.3(3) . . ? Ni1 O5 Ni2 79.76(10) . . ? Ni3 O5 Ni2 78.11(10) . . ? C32 O6 C38 114.8(4) . . ? C44 O7 Ni2 117.4(3) . . ? C44 O7 Ni3 117.2(3) . . ? Ni2 O7 Ni3 89.66(13) . . ? C50 O8 C44 113.5(4) . . ? N1 C1 C2 123.1(5) . . ? C3 C2 C1 118.9(5) . . ? C2 C3 C4 118.9(5) . . ? C3 C4 C5 119.6(5) . . ? N1 C5 C4 121.4(4) . . ? N1 C5 C6 116.6(4) . . ? C4 C5 C6 122.0(4) . . ? O1 C6 O2 112.8(3) . . ? O1 C6 C7 111.3(4) . . ? O2 C6 C7 102.5(3) . . ? O1 C6 C5 109.7(4) . . ? O2 C6 C5 108.7(4) . . ? C7 C6 C5 111.7(4) . . ? N2 C7 C8 120.8(5) . . ? N2 C7 C6 114.4(4) . . ? C8 C7 C6 124.6(5) . . ? C9 C8 C7 119.9(6) . . ? C8 C9 C10 119.5(6) . . ? C11 C10 C9 118.4(6) . . ? N2 C11 C10 122.6(6) . . ? N3 C13 C14 121.9(6) . . ? C15 C14 C13 118.9(6) . . ? C16 C15 C14 119.4(6) . . ? C15 C16 C17 118.6(6) . . ? N3 C17 C16 122.1(5) . . ? N3 C17 C18 115.9(4) . . ? C16 C17 C18 122.0(5) . . ? O3 C18 O4 113.6(4) . . ? O3 C18 C17 109.9(4) . . ? O4 C18 C17 109.4(4) . . ? O3 C18 C20 110.2(4) . . ? O4 C18 C20 103.2(3) . . ? C17 C18 C20 110.4(4) . . ? N4 C20 C21 121.7(4) . . ? N4 C20 C18 114.9(4) . . ? C21 C20 C18 123.3(4) . . ? C22 C21 C20 119.3(5) . . ? C21 C22 C23 119.8(5) . . ? C22 C23 C25 118.7(5) . . ? N4 C25 C23 122.4(5) . . ? N5 C27 C28 123.2(5) . . ? C29 C28 C27 119.0(5) . . ? C28 C29 C30 119.7(5) . . ? C29 C30 C31 118.4(5) . . ? N5 C31 C30 121.7(5) . . ? N5 C31 C32 115.3(4) . . ? C30 C31 C32 123.0(5) . . ? O5 C32 O6 113.4(4) . . ? O5 C32 C33 110.3(4) . . ? O6 C32 C33 110.3(4) . . ? O5 C32 C31 109.5(4) . . ? O6 C32 C31 103.3(4) . . ? C33 C32 C31 109.7(4) . . ? N6 C33 C34 121.1(5) . . ? N6 C33 C32 115.4(4) . . ? C34 C33 C32 123.4(5) . . ? C35 C34 C33 119.7(7) . . ? C36 C35 C34 119.3(6) . . ? C35 C36 C37 119.3(6) . . ? N6 C37 C36 122.0(6) . . ? N7 C39 C40 122.1(6) . . ? C41 C40 C39 118.9(6) . . ? C40 C41 C42 120.7(6) . . ? C43 C42 C41 117.5(6) . . ? N7 C43 C42 121.9(5) . . ? N7 C43 C44 114.5(4) . . ? C42 C43 C44 123.5(5) . . ? O7 C44 O8 111.7(4) . . ? O7 C44 C45 110.3(4) . . ? O8 C44 C45 109.2(4) . . ? O7 C44 C43 111.1(4) . . ? O8 C44 C43 103.0(4) . . ? C45 C44 C43 111.4(4) . . ? N8 C45 C46 121.3(5) . . ? N8 C45 C44 116.0(4) . . ? C46 C45 C44 122.6(5) . . ? C45 C46 C47 120.0(6) . . ? C46 C47 C48 118.5(5) . . ? C49 C48 C47 118.7(6) . . ? N8 C49 C48 122.7(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.386 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.111 # Attachment '- complex4.cif' data_tdk647ma _database_code_depnum_ccdc_archive 'CCDC 803777' #TrackingRef '- complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H50.50 I1.50 N8.50 Ni3 O11.50' _chemical_formula_weight 1320.97 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 24.0128(12) _cell_length_b 15.6980(7) _cell_length_c 15.7309(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.010(2) _cell_angle_gamma 90.00 _cell_volume 5820.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9968 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 24.18 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2662 _exptl_absorpt_coefficient_mu 1.818 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5687 _exptl_absorpt_correction_T_max 0.7356 _exptl_absorpt_process_details 'Bruker SADABS' _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 'Bruker SMART Apex2 CCD' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33783 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0357 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 24.28 _reflns_number_total 9334 _reflns_number_gt 7202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+54.4382P] 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 none _refine_ls_number_reflns 9334 _refine_ls_number_parameters 674 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0991 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.2183 _refine_ls_wR_factor_gt 0.2088 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.013 _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 0.18957(4) 0.98339(6) -0.26451(6) 0.0311(2) Uani 1 1 d . . . Ni2 Ni 0.30990(4) 1.05406(6) -0.16618(6) 0.0341(3) Uani 1 1 d . . . Ni3 Ni 0.25491(5) 0.90937(8) -0.11457(7) 0.0504(3) Uani 1 1 d . . . I1 I 0.39025(4) 0.05967(6) 0.37334(7) 0.0919(3) Uani 1 1 d . . . I2A I 0.0984(6) 0.4532(8) -0.1873(16) 0.342(19) Uani 0.327(6) 1 d P . . I2B I 0.1033(2) 0.4617(3) -0.2304(7) 0.121(3) Uani 0.327(6) 1 d P . . N1 N 0.2147(3) 1.0473(4) -0.3669(4) 0.0370(15) Uani 1 1 d . . . N2 N 0.3750(3) 1.0321(5) -0.2305(5) 0.0446(17) Uani 1 1 d . . . N3 N 0.1515(3) 0.8818(4) -0.3383(4) 0.0382(15) Uani 1 1 d . . . N4 N 0.2513(3) 0.7825(5) -0.1245(4) 0.0456(17) Uani 1 1 d . . . N5 N 0.1238(3) 1.0617(4) -0.2528(4) 0.0391(15) Uani 1 1 d . . . N6 N 0.2801(3) 1.1666(4) -0.2291(4) 0.0411(16) Uani 1 1 d . . . N7 N 0.3519(3) 1.1151(4) -0.0551(4) 0.0427(16) Uani 1 1 d . . . N8 N 0.2582(3) 0.9226(5) 0.0137(4) 0.0462(17) Uani 1 1 d . . . O1 O 0.2733(2) 0.9509(3) -0.2480(3) 0.0347(12) Uani 1 1 d . . . O2 O 0.2879(3) 0.8798(4) -0.3731(4) 0.0520(16) Uani 1 1 d . . . O3 O 0.1751(2) 0.9005(3) -0.1704(3) 0.0345(12) Uani 1 1 d . . . O4 O 0.1071(2) 0.7980(4) -0.1565(4) 0.0449(14) Uani 1 1 d . . . O5 O 0.2272(2) 1.0546(3) -0.1533(3) 0.0310(11) Uani 1 1 d . . . O6 O 0.2093(3) 1.1728(3) -0.0738(3) 0.0466(14) Uani 1 1 d . . . O7 O 0.3321(2) 0.9526(3) -0.0834(3) 0.0389(12) Uani 1 1 d . . . O8 O 0.3987(3) 0.9157(4) 0.0382(4) 0.0616(18) Uani 1 1 d . . . C1 C 0.1843(4) 1.1050(6) -0.4194(6) 0.052(2) Uani 1 1 d . . . H1 H 0.1488 1.1207 -0.4091 0.062 Uiso 1 1 calc R . . C2 C 0.2035(5) 1.1416(6) -0.4876(6) 0.062(3) Uani 1 1 d . . . H2 H 0.1820 1.1829 -0.5215 0.074 Uiso 1 1 calc R . . C3 C 0.2544(5) 1.1167(6) -0.5048(6) 0.063(3) Uani 1 1 d . . . H3 H 0.2674 1.1399 -0.5517 0.076 Uiso 1 1 calc R . . C4 C 0.2865(4) 1.0575(5) -0.4533(5) 0.048(2) Uani 1 1 d . . . H4 H 0.3217 1.0408 -0.4638 0.058 Uiso 1 1 calc R . . C5 C 0.2647(4) 1.0228(5) -0.3845(5) 0.0406(19) Uani 1 1 d . . . C6 C 0.2957(4) 0.9551(5) -0.3230(5) 0.0408(19) Uani 1 1 d . . . C7 C 0.3596(4) 0.9779(6) -0.2992(6) 0.047(2) Uani 1 1 d . . . C8 C 0.3987(5) 0.9505(8) -0.3477(8) 0.073(3) Uani 1 1 d . . . H8 H 0.3877 0.9139 -0.3944 0.088 Uiso 1 1 calc R . . C9 C 0.4542(6) 0.9783(11) -0.3259(10) 0.099(5) Uani 1 1 d . . . H9 H 0.4812 0.9606 -0.3573 0.119 Uiso 1 1 calc R . . C10 C 0.4686(5) 1.0325(10) -0.2567(10) 0.090(4) Uani 1 1 d . . . H10 H 0.5056 1.0525 -0.2411 0.108 Uiso 1 1 calc R . . C11 C 0.4280(4) 1.0573(7) -0.2104(7) 0.062(3) Uani 1 1 d . . . H11 H 0.4386 1.0932 -0.1631 0.074 Uiso 1 1 calc R . . C12 C 0.3050(6) 0.8033(6) -0.3242(7) 0.076(3) Uani 1 1 d . . . H12A H 0.2983 0.7548 -0.3620 0.114 Uiso 1 1 calc R . . H12B H 0.2835 0.7975 -0.2790 0.114 Uiso 1 1 calc R . . H12C H 0.3447 0.8066 -0.2991 0.114 Uiso 1 1 calc R . . C13 C 0.1381(4) 0.8801(6) -0.4242(5) 0.054(2) Uani 1 1 d . . . H13 H 0.1472 0.9270 -0.4551 0.065 Uiso 1 1 calc R . . C14 C 0.1111(5) 0.8110(7) -0.4698(6) 0.062(3) Uani 1 1 d . . . H14 H 0.1029 0.8110 -0.5300 0.075 Uiso 1 1 calc R . . C15 C 0.0969(4) 0.7428(6) -0.4239(6) 0.060(3) Uani 1 1 d . . . H15 H 0.0779 0.6964 -0.4525 0.072 Uiso 1 1 calc R . . C16 C 0.1112(4) 0.7439(6) -0.3344(6) 0.046(2) Uani 1 1 d . . . H16 H 0.1022 0.6979 -0.3023 0.056 Uiso 1 1 calc R . . C17 C 0.1391(3) 0.8145(5) -0.2929(5) 0.0365(17) Uani 1 1 d . . . C18 C 0.1554(3) 0.8202(5) -0.1944(5) 0.0354(17) Uani 1 1 d . . . C19 C 0.1993(4) 0.7525(5) -0.1558(5) 0.0374(18) Uani 1 1 d . . . C20 C 0.1869(4) 0.6664(5) -0.1510(6) 0.050(2) Uani 1 1 d . . . H20 H 0.1507 0.6456 -0.1724 0.060 Uiso 1 1 calc R . . C21 C 0.2304(6) 0.6126(6) -0.1131(6) 0.065(3) Uani 1 1 d . . . H21 H 0.2230 0.5548 -0.1084 0.077 Uiso 1 1 calc R . . C22 C 0.2827(5) 0.6416(7) -0.0833(7) 0.064(3) Uani 1 1 d . . . H22 H 0.3119 0.6051 -0.0590 0.077 Uiso 1 1 calc R . . C23 C 0.2914(4) 0.7258(7) -0.0899(6) 0.063(3) Uani 1 1 d . . . H23 H 0.3278 0.7464 -0.0690 0.075 Uiso 1 1 calc R . . C24 C 0.0618(4) 0.8579(7) -0.1739(8) 0.065(3) Uani 1 1 d . . . H24A H 0.0312 0.8392 -0.1471 0.098 Uiso 1 1 calc R . . H24B H 0.0487 0.8625 -0.2353 0.098 Uiso 1 1 calc R . . H24C H 0.0750 0.9125 -0.1509 0.098 Uiso 1 1 calc R . . C25 C 0.0697(4) 1.0536(6) -0.2911(6) 0.055(2) Uani 1 1 d . . . H25 H 0.0600 1.0099 -0.3311 0.066 Uiso 1 1 calc R . . C26 C 0.0270(4) 1.1074(8) -0.2741(8) 0.076(3) Uani 1 1 d . . . H26 H -0.0107 1.0988 -0.3003 0.091 Uiso 1 1 calc R . . C27 C 0.0426(4) 1.1741(8) -0.2169(9) 0.080(4) Uani 1 1 d . . . H27 H 0.0156 1.2134 -0.2070 0.096 Uiso 1 1 calc R . . C28 C 0.0990(4) 1.1823(6) -0.1742(7) 0.062(3) Uani 1 1 d . . . H28 H 0.1097 1.2245 -0.1327 0.074 Uiso 1 1 calc R . . C29 C 0.1381(3) 1.1261(5) -0.1955(5) 0.0392(18) Uani 1 1 d . . . C30 C 0.2024(3) 1.1332(5) -0.1562(5) 0.0369(18) Uani 1 1 d . . . C31 C 0.2317(3) 1.1953(5) -0.2089(5) 0.0381(18) Uani 1 1 d . . . C32 C 0.2110(4) 1.2751(5) -0.2335(6) 0.050(2) Uani 1 1 d . . . H32 H 0.1769 1.2933 -0.2198 0.060 Uiso 1 1 calc R . . C33 C 0.2404(5) 1.3272(6) -0.2777(7) 0.065(3) Uani 1 1 d . . . H33 H 0.2273 1.3820 -0.2927 0.077 Uiso 1 1 calc R . . C34 C 0.2894(5) 1.2984(7) -0.3000(7) 0.063(3) Uani 1 1 d . . . H34 H 0.3095 1.3324 -0.3320 0.076 Uiso 1 1 calc R . . C35 C 0.3083(4) 1.2181(6) -0.2741(6) 0.051(2) Uani 1 1 d . . . H35 H 0.3420 1.1987 -0.2884 0.061 Uiso 1 1 calc R . . C36 C 0.1922(5) 1.1214(7) -0.0079(6) 0.068(3) Uani 1 1 d . . . H36A H 0.1981 1.1526 0.0456 0.103 Uiso 1 1 calc R . . H36B H 0.2143 1.0701 -0.0003 0.103 Uiso 1 1 calc R . . H36C H 0.1527 1.1072 -0.0248 0.103 Uiso 1 1 calc R . . C37 C 0.3655(4) 1.1984(6) -0.0472(6) 0.056(2) Uani 1 1 d . . . H37 H 0.3517 1.2346 -0.0932 0.067 Uiso 1 1 calc R . . C38 C 0.3989(5) 1.2323(8) 0.0257(7) 0.073(3) Uani 1 1 d . . . H38 H 0.4070 1.2902 0.0291 0.088 Uiso 1 1 calc R . . C39 C 0.4196(5) 1.1798(8) 0.0927(7) 0.074(3) Uani 1 1 d . . . H39 H 0.4424 1.2014 0.1425 0.088 Uiso 1 1 calc R . . C40 C 0.4067(4) 1.0944(7) 0.0866(6) 0.060(3) Uani 1 1 d . . . H40 H 0.4214 1.0576 0.1316 0.072 Uiso 1 1 calc R . . C41 C 0.3715(3) 1.0635(6) 0.0123(5) 0.0425(19) Uani 1 1 d . . . C42 C 0.3527(3) 0.9704(6) 0.0015(5) 0.043(2) Uani 1 1 d . . . C43 C 0.3080(4) 0.9507(5) 0.0569(5) 0.0402(19) Uani 1 1 d . . . C44 C 0.3164(5) 0.9604(6) 0.1468(6) 0.057(2) Uani 1 1 d . . . H44 H 0.3515 0.9777 0.1776 0.068 Uiso 1 1 calc R . . C45 C 0.2728(6) 0.9443(7) 0.1891(7) 0.068(3) Uani 1 1 d . . . H45 H 0.2775 0.9525 0.2486 0.082 Uiso 1 1 calc R . . C46 C 0.2230(5) 0.9164(7) 0.1435(7) 0.069(3) Uani 1 1 d . . . H46 H 0.1928 0.9052 0.1710 0.083 Uiso 1 1 calc R . . C47 C 0.2174(4) 0.9046(7) 0.0557(7) 0.063(3) Uani 1 1 d . . . H47 H 0.1835 0.8829 0.0248 0.075 Uiso 1 1 calc R . . C48 C 0.4416(5) 0.9095(10) -0.0108(10) 0.099(4) Uani 1 1 d . . . H48A H 0.4709 0.8723 0.0179 0.149 Uiso 1 1 calc R . . H48B H 0.4572 0.9650 -0.0168 0.149 Uiso 1 1 calc R . . H48C H 0.4259 0.8871 -0.0671 0.149 Uiso 1 1 calc R . . N10 N 0.0565(13) 0.4210(18) -0.0957(19) 0.144(11) Uiso 0.68(3) 1 d PD . . O10 O 0.087(9) 0.363(6) -0.110(15) 0.9(3) Uiso 0.327(6) 1 d PD . . O11 O 0.071(5) 0.493(3) -0.109(6) 0.70(9) Uiso 0.68(3) 1 d PD . . O12 O 0.0302(16) 0.410(3) -0.038(2) 0.27(2) Uiso 0.68(3) 1 d PD . . C60 C 0.5238(19) 0.254(3) 0.835(3) 0.278(17) Uiso 1 1 d . . . C61 C 0.4669(17) 0.838(3) 0.428(4) 0.283(18) Uiso 1 1 d D . . O60 O 0.4635(10) 0.2577(14) 0.8140(13) 0.230(8) Uiso 1 1 d . . . O61A O 0.433(2) 0.824(3) 0.354(3) 0.27(3) Uiso 0.52(5) 1 d PD . . O61B O 0.427(2) 0.859(3) 0.469(3) 0.21(2) Uiso 0.48(5) 1 d PD . . O10A O 0.0984(14) 0.483(2) -0.280(2) 0.172(17) Uiso 0.673(6) 1 d P . . 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 0.0366(5) 0.0282(5) 0.0293(5) 0.0014(4) 0.0081(4) -0.0005(4) Ni2 0.0322(5) 0.0363(6) 0.0344(5) 0.0029(4) 0.0078(4) -0.0010(4) Ni3 0.0579(7) 0.0492(7) 0.0389(6) 0.0106(5) -0.0035(5) -0.0166(6) I1 0.0750(6) 0.0981(7) 0.1061(7) -0.0197(5) 0.0265(5) -0.0021(5) I2A 0.200(14) 0.205(12) 0.54(4) -0.008(12) -0.142(16) 0.083(9) I2B 0.064(2) 0.0498(18) 0.254(9) -0.017(3) 0.045(4) 0.0030(16) N1 0.045(4) 0.032(3) 0.033(3) 0.004(3) 0.006(3) -0.001(3) N2 0.033(4) 0.056(4) 0.049(4) 0.013(4) 0.018(3) 0.005(3) N3 0.045(4) 0.038(4) 0.033(3) -0.004(3) 0.011(3) -0.002(3) N4 0.053(4) 0.045(4) 0.039(4) 0.011(3) 0.009(3) 0.006(3) N5 0.036(4) 0.038(4) 0.044(4) 0.004(3) 0.008(3) 0.000(3) N6 0.042(4) 0.040(4) 0.040(4) 0.004(3) 0.006(3) -0.009(3) N7 0.037(4) 0.046(4) 0.043(4) -0.002(3) 0.002(3) -0.007(3) N8 0.048(4) 0.050(4) 0.039(4) 0.006(3) 0.003(3) -0.005(3) O1 0.040(3) 0.036(3) 0.031(3) 0.000(2) 0.014(2) 0.004(2) O2 0.080(5) 0.038(3) 0.044(3) -0.004(3) 0.025(3) 0.004(3) O3 0.047(3) 0.029(3) 0.031(3) -0.002(2) 0.014(2) -0.005(2) O4 0.047(3) 0.040(3) 0.055(3) 0.006(3) 0.028(3) -0.004(3) O5 0.035(3) 0.028(3) 0.029(3) -0.001(2) 0.007(2) 0.001(2) O6 0.064(4) 0.037(3) 0.039(3) -0.010(3) 0.011(3) 0.004(3) O7 0.046(3) 0.035(3) 0.034(3) -0.001(2) 0.003(2) 0.004(2) O8 0.052(4) 0.069(4) 0.059(4) 0.014(3) -0.002(3) 0.015(3) C1 0.058(6) 0.046(5) 0.050(5) 0.007(4) 0.007(4) -0.001(4) C2 0.095(8) 0.044(5) 0.045(5) 0.020(4) 0.010(5) -0.004(5) C3 0.090(8) 0.056(6) 0.049(5) 0.017(5) 0.025(5) -0.018(6) C4 0.062(6) 0.043(5) 0.042(5) 0.005(4) 0.018(4) -0.010(4) C5 0.050(5) 0.038(4) 0.034(4) 0.000(3) 0.008(4) -0.008(4) C6 0.043(5) 0.039(5) 0.043(4) -0.007(4) 0.015(4) 0.003(4) C7 0.046(5) 0.046(5) 0.057(5) 0.011(4) 0.030(4) 0.007(4) C8 0.056(7) 0.095(9) 0.078(7) -0.015(6) 0.031(6) 0.008(6) C9 0.064(8) 0.134(13) 0.113(11) -0.015(10) 0.049(8) 0.012(8) C10 0.036(6) 0.116(11) 0.122(11) 0.022(9) 0.026(7) 0.003(6) C11 0.059(7) 0.062(6) 0.063(6) 0.004(5) 0.010(5) -0.011(5) C12 0.113(10) 0.040(5) 0.078(7) -0.005(5) 0.027(7) 0.015(6) C13 0.065(6) 0.062(6) 0.035(5) -0.003(4) 0.010(4) -0.017(5) C14 0.077(7) 0.069(7) 0.039(5) -0.015(5) 0.005(5) -0.008(6) C15 0.065(6) 0.048(6) 0.063(6) -0.021(5) 0.000(5) -0.007(5) C16 0.052(5) 0.039(5) 0.048(5) -0.004(4) 0.009(4) -0.007(4) C17 0.034(4) 0.038(4) 0.039(4) -0.005(3) 0.008(3) 0.004(3) C18 0.043(4) 0.030(4) 0.035(4) -0.003(3) 0.013(3) -0.006(3) C19 0.053(5) 0.033(4) 0.030(4) -0.002(3) 0.016(4) 0.003(4) C20 0.066(6) 0.035(5) 0.050(5) 0.001(4) 0.018(4) 0.003(4) C21 0.112(10) 0.041(5) 0.045(5) 0.012(4) 0.025(6) 0.013(6) C22 0.077(8) 0.061(7) 0.056(6) 0.018(5) 0.016(5) 0.028(6) C23 0.058(6) 0.079(8) 0.050(5) 0.012(5) 0.010(5) 0.013(5) C24 0.054(6) 0.059(6) 0.092(8) 0.012(6) 0.039(6) 0.000(5) C25 0.050(6) 0.048(5) 0.062(6) 0.001(4) -0.001(5) -0.005(4) C26 0.037(5) 0.082(8) 0.104(9) 0.006(7) 0.003(6) 0.010(5) C27 0.040(6) 0.082(8) 0.118(10) -0.016(7) 0.016(6) 0.014(6) C28 0.048(6) 0.049(6) 0.090(8) -0.010(5) 0.019(5) 0.007(5) C29 0.041(5) 0.035(4) 0.040(4) 0.001(4) 0.005(3) 0.001(4) C30 0.037(4) 0.035(4) 0.036(4) -0.004(3) 0.002(3) 0.003(3) C31 0.044(5) 0.032(4) 0.036(4) -0.002(3) 0.003(3) -0.003(4) C32 0.058(6) 0.038(5) 0.054(5) -0.002(4) 0.009(4) 0.003(4) C33 0.094(8) 0.035(5) 0.063(6) 0.008(5) 0.011(6) -0.001(5) C34 0.074(7) 0.055(6) 0.060(6) 0.013(5) 0.012(5) -0.016(5) C35 0.050(5) 0.052(6) 0.053(5) 0.010(4) 0.013(4) -0.011(4) C36 0.110(9) 0.058(6) 0.045(5) 0.002(5) 0.034(6) 0.020(6) C37 0.054(6) 0.053(6) 0.060(6) 0.004(5) 0.007(5) -0.012(5) C38 0.069(7) 0.074(7) 0.075(7) -0.011(6) 0.008(6) -0.030(6) C39 0.060(7) 0.099(9) 0.053(6) -0.003(6) -0.008(5) -0.028(6) C40 0.054(6) 0.072(7) 0.049(5) 0.005(5) -0.001(4) -0.023(5) C41 0.033(4) 0.057(5) 0.038(4) -0.003(4) 0.007(3) -0.003(4) C42 0.037(4) 0.055(5) 0.036(4) 0.004(4) 0.002(3) 0.010(4) C43 0.047(5) 0.040(4) 0.035(4) 0.009(3) 0.011(4) 0.003(4) C44 0.069(6) 0.065(6) 0.036(5) -0.008(4) 0.008(4) -0.010(5) C45 0.101(9) 0.067(7) 0.042(5) -0.005(5) 0.025(6) -0.008(6) C46 0.085(8) 0.067(7) 0.068(7) 0.010(6) 0.046(6) -0.009(6) C47 0.056(6) 0.065(6) 0.068(7) 0.023(5) 0.013(5) -0.014(5) C48 0.057(8) 0.121(12) 0.112(11) 0.011(9) -0.001(7) 0.029(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N5 2.038(7) . ? Ni1 O1 2.042(5) . ? Ni1 O3 2.049(5) . ? Ni1 N3 2.078(6) . ? Ni1 N1 2.083(6) . ? Ni1 O5 2.126(5) . ? Ni1 Ni3 2.8216(14) . ? Ni2 O5 2.034(5) . ? Ni2 N2 2.047(7) . ? Ni2 O7 2.062(5) . ? Ni2 N7 2.077(7) . ? Ni2 N6 2.084(7) . ? Ni2 O1 2.149(5) . ? Ni2 Ni3 2.8234(14) . ? Ni3 O7 1.946(6) . ? Ni3 O3 1.954(5) . ? Ni3 N4 1.998(7) . ? Ni3 N8 2.014(7) . ? Ni3 O1 2.319(5) . ? I2A I2B 0.72(3) . ? I2A O10A 1.53(4) . ? I2A O11 1.63(7) . ? I2A N10 1.97(3) . ? I2A O10 1.92(9) . ? I2B O10A 0.84(3) . ? I2B O11 2.25(8) . ? N1 C5 1.339(11) . ? N1 C1 1.344(11) . ? N2 C11 1.312(12) . ? N2 C7 1.369(12) . ? N3 C13 1.329(10) . ? N3 C17 1.340(10) . ? N4 C19 1.337(11) . ? N4 C23 1.348(12) . ? N5 C25 1.328(11) . ? N5 C29 1.354(10) . ? N6 C31 1.341(11) . ? N6 C35 1.340(11) . ? N7 C41 1.346(11) . ? N7 C37 1.348(12) . ? N8 C47 1.313(12) . ? N8 C43 1.331(11) . ? O1 C6 1.390(9) . ? O2 C6 1.413(10) . ? O2 C12 1.442(12) . ? O3 C18 1.374(9) . ? O4 C24 1.424(11) . ? O4 C18 1.444(9) . ? O5 C30 1.368(9) . ? O6 C30 1.419(9) . ? O6 C36 1.433(11) . ? O7 C42 1.361(9) . ? O8 C48 1.401(15) . ? O8 C42 1.432(10) . ? C1 C2 1.373(13) . ? C2 C3 1.357(15) . ? C3 C4 1.370(14) . ? C4 C5 1.399(11) . ? C5 C6 1.531(12) . ? C6 C7 1.551(12) . ? C7 C8 1.387(13) . ? C8 C9 1.380(18) . ? C9 C10 1.373(19) . ? C10 C11 1.380(16) . ? C13 C14 1.391(13) . ? C14 C15 1.370(14) . ? C15 C16 1.383(13) . ? C16 C17 1.392(11) . ? C17 C18 1.526(10) . ? C18 C19 1.539(11) . ? C19 C20 1.389(12) . ? C20 C21 1.387(14) . ? C21 C22 1.333(16) . ? C22 C23 1.346(15) . ? C25 C26 1.393(15) . ? C26 C27 1.385(16) . ? C27 C28 1.397(15) . ? C28 C29 1.378(12) . ? C29 C30 1.553(11) . ? C30 C31 1.534(11) . ? C31 C32 1.376(12) . ? C32 C33 1.355(14) . ? C33 C34 1.368(15) . ? C34 C35 1.376(14) . ? C37 C38 1.375(14) . ? C38 C39 1.355(16) . ? C39 C40 1.375(15) . ? C40 C41 1.392(12) . ? C41 C42 1.529(12) . ? C42 C43 1.539(11) . ? C43 C44 1.398(12) . ? C44 C45 1.367(14) . ? C45 C46 1.344(16) . ? C46 C47 1.375(15) . ? N10 O11 1.213(15) . ? N10 O10 1.212(15) . ? N10 O12 1.218(14) . ? O10 O10A 3.33(13) . ? C60 O60 1.42(4) . ? C61 O61B 1.293(19) . ? C61 O61A 1.311(19) . ? 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 N5 Ni1 O1 154.3(2) . . ? N5 Ni1 O3 94.4(2) . . ? O1 Ni1 O3 92.7(2) . . ? N5 Ni1 N3 104.3(3) . . ? O1 Ni1 N3 101.4(2) . . ? O3 Ni1 N3 78.4(2) . . ? N5 Ni1 N1 97.1(3) . . ? O1 Ni1 N1 78.2(2) . . ? O3 Ni1 N1 168.1(2) . . ? N3 Ni1 N1 95.7(3) . . ? N5 Ni1 O5 79.9(2) . . ? O1 Ni1 O5 76.87(19) . . ? O3 Ni1 O5 81.00(19) . . ? N3 Ni1 O5 159.2(2) . . ? N1 Ni1 O5 104.0(2) . . ? N5 Ni1 Ni3 119.35(19) . . ? O1 Ni1 Ni3 54.11(14) . . ? O3 Ni1 Ni3 43.83(15) . . ? N3 Ni1 Ni3 105.43(19) . . ? N1 Ni1 Ni3 130.38(19) . . ? O5 Ni1 Ni3 56.48(13) . . ? O5 Ni2 N2 154.4(3) . . ? O5 Ni2 O7 94.6(2) . . ? N2 Ni2 O7 93.0(2) . . ? O5 Ni2 N7 103.9(2) . . ? N2 Ni2 N7 101.5(3) . . ? O7 Ni2 N7 78.4(2) . . ? O5 Ni2 N6 77.9(2) . . ? N2 Ni2 N6 97.7(3) . . ? O7 Ni2 N6 168.2(2) . . ? N7 Ni2 N6 94.4(3) . . ? O5 Ni2 O1 76.51(19) . . ? N2 Ni2 O1 80.9(3) . . ? O7 Ni2 O1 79.8(2) . . ? N7 Ni2 O1 158.2(2) . . ? N6 Ni2 O1 106.9(2) . . ? O5 Ni2 Ni3 57.02(14) . . ? N2 Ni2 Ni3 116.7(2) . . ? O7 Ni2 Ni3 43.58(16) . . ? N7 Ni2 Ni3 107.90(19) . . ? N6 Ni2 Ni3 132.96(19) . . ? O1 Ni2 Ni3 53.52(13) . . ? O7 Ni3 O3 160.5(2) . . ? O7 Ni3 N4 113.1(3) . . ? O3 Ni3 N4 82.5(3) . . ? O7 Ni3 N8 81.8(3) . . ? O3 Ni3 N8 107.8(3) . . ? N4 Ni3 N8 100.0(3) . . ? O7 Ni3 O1 78.1(2) . . ? O3 Ni3 O1 87.29(19) . . ? N4 Ni3 O1 102.8(2) . . ? N8 Ni3 O1 154.1(2) . . ? O7 Ni3 Ni1 114.68(16) . . ? O3 Ni3 Ni1 46.58(14) . . ? N4 Ni3 Ni1 109.6(2) . . ? N8 Ni3 Ni1 134.8(2) . . ? O1 Ni3 Ni1 45.51(13) . . ? O7 Ni3 Ni2 46.90(15) . . ? O3 Ni3 Ni2 113.59(15) . . ? N4 Ni3 Ni2 142.7(2) . . ? N8 Ni3 Ni2 105.9(2) . . ? O1 Ni3 Ni2 48.20(13) . . ? Ni1 Ni3 Ni2 69.16(4) . . ? I2B I2A O10A 11.7(15) . . ? I2B I2A O11 143(3) . . ? O10A I2A O11 132(3) . . ? I2B I2A N10 158.3(17) . . ? O10A I2A N10 149.9(17) . . ? O11 I2A N10 37.8(9) . . ? I2B I2A O10 143(6) . . ? O10A I2A O10 149(7) . . ? O11 I2A O10 71(4) . . ? N10 I2A O10 36.2(10) . . ? I2A I2B O10A 158(3) . . ? I2A I2B O11 26(2) . . ? O10A I2B O11 134(3) . . ? C5 N1 C1 118.1(7) . . ? C5 N1 Ni1 115.2(5) . . ? C1 N1 Ni1 126.6(6) . . ? C11 N2 C7 118.7(8) . . ? C11 N2 Ni2 128.8(7) . . ? C7 N2 Ni2 112.2(5) . . ? C13 N3 C17 119.4(7) . . ? C13 N3 Ni1 125.3(6) . . ? C17 N3 Ni1 115.2(5) . . ? C19 N4 C23 117.5(8) . . ? C19 N4 Ni3 113.8(5) . . ? C23 N4 Ni3 127.6(7) . . ? C25 N5 C29 118.4(7) . . ? C25 N5 Ni1 127.5(6) . . ? C29 N5 Ni1 114.0(5) . . ? C31 N6 C35 118.1(7) . . ? C31 N6 Ni2 114.0(5) . . ? C35 N6 Ni2 126.8(6) . . ? C41 N7 C37 117.9(7) . . ? C41 N7 Ni2 115.2(5) . . ? C37 N7 Ni2 126.5(6) . . ? C47 N8 C43 119.8(8) . . ? C47 N8 Ni3 126.2(7) . . ? C43 N8 Ni3 113.9(6) . . ? C6 O1 Ni1 114.3(5) . . ? C6 O1 Ni2 107.0(4) . . ? Ni1 O1 Ni2 99.7(2) . . ? C6 O1 Ni3 162.5(5) . . ? Ni1 O1 Ni3 80.38(17) . . ? Ni2 O1 Ni3 78.28(16) . . ? C6 O2 C12 113.9(7) . . ? C18 O3 Ni3 116.5(5) . . ? C18 O3 Ni1 118.7(4) . . ? Ni3 O3 Ni1 89.6(2) . . ? C24 O4 C18 113.9(6) . . ? C30 O5 Ni2 115.4(4) . . ? C30 O5 Ni1 109.4(4) . . ? Ni2 O5 Ni1 100.7(2) . . ? C30 O6 C36 114.5(7) . . ? C42 O7 Ni3 118.0(5) . . ? C42 O7 Ni2 117.5(5) . . ? Ni3 O7 Ni2 89.5(2) . . ? C48 O8 C42 114.2(8) . . ? N1 C1 C2 122.5(9) . . ? C3 C2 C1 119.0(9) . . ? C2 C3 C4 120.3(8) . . ? C3 C4 C5 118.0(9) . . ? N1 C5 C4 122.0(8) . . ? N1 C5 C6 114.6(7) . . ? C4 C5 C6 123.4(8) . . ? O1 C6 O2 113.7(7) . . ? O1 C6 C5 110.4(6) . . ? O2 C6 C5 103.5(6) . . ? O1 C6 C7 109.4(7) . . ? O2 C6 C7 110.3(7) . . ? C5 C6 C7 109.4(7) . . ? N2 C7 C8 121.2(9) . . ? N2 C7 C6 116.0(7) . . ? C8 C7 C6 122.6(9) . . ? C9 C8 C7 119.1(11) . . ? C10 C9 C8 118.6(11) . . ? C9 C10 C11 119.7(11) . . ? N2 C11 C10 122.6(11) . . ? N3 C13 C14 122.5(9) . . ? C15 C14 C13 118.4(9) . . ? C14 C15 C16 119.3(9) . . ? C15 C16 C17 119.4(8) . . ? N3 C17 C16 120.9(7) . . ? N3 C17 C18 117.0(7) . . ? C16 C17 C18 122.0(7) . . ? O3 C18 O4 111.8(6) . . ? O3 C18 C17 109.9(6) . . ? O4 C18 C17 109.5(6) . . ? O3 C18 C19 110.5(6) . . ? O4 C18 C19 102.4(6) . . ? C17 C18 C19 112.5(6) . . ? N4 C19 C20 121.2(8) . . ? N4 C19 C18 115.0(7) . . ? C20 C19 C18 123.7(8) . . ? C21 C20 C19 117.7(10) . . ? C22 C21 C20 121.7(10) . . ? C21 C22 C23 117.3(10) . . ? C22 C23 N4 124.8(11) . . ? N5 C25 C26 123.1(9) . . ? C27 C26 C25 117.7(10) . . ? C26 C27 C28 120.0(10) . . ? C29 C28 C27 117.8(10) . . ? N5 C29 C28 122.8(8) . . ? N5 C29 C30 115.2(7) . . ? C28 C29 C30 122.0(8) . . ? O5 C30 O6 113.0(6) . . ? O5 C30 C31 110.4(6) . . ? O6 C30 C31 103.3(6) . . ? O5 C30 C29 110.0(6) . . ? O6 C30 C29 109.2(6) . . ? C31 C30 C29 110.7(6) . . ? N6 C31 C32 121.4(8) . . ? N6 C31 C30 115.0(7) . . ? C32 C31 C30 123.6(8) . . ? C33 C32 C31 120.0(9) . . ? C32 C33 C34 119.3(9) . . ? C33 C34 C35 118.6(9) . . ? N6 C35 C34 122.5(9) . . ? N7 C37 C38 123.0(10) . . ? C39 C38 C37 118.9(11) . . ? C38 C39 C40 119.6(10) . . ? C39 C40 C41 119.4(10) . . ? N7 C41 C40 121.1(8) . . ? N7 C41 C42 115.8(7) . . ? C40 C41 C42 123.1(8) . . ? O7 C42 O8 112.4(7) . . ? O7 C42 C41 110.5(7) . . ? O8 C42 C41 109.8(7) . . ? O7 C42 C43 110.6(7) . . ? O8 C42 C43 102.6(7) . . ? C41 C42 C43 110.7(7) . . ? N8 C43 C44 119.7(8) . . ? N8 C43 C42 115.6(7) . . ? C44 C43 C42 124.7(8) . . ? C45 C44 C43 119.7(9) . . ? C46 C45 C44 119.1(9) . . ? C45 C46 C47 119.1(10) . . ? N8 C47 C46 122.5(10) . . ? O11 N10 O10 118(3) . . ? O11 N10 O12 117(3) . . ? O10 N10 O12 117(3) . . ? O11 N10 I2A 56(4) . . ? O10 N10 I2A 69(4) . . ? O12 N10 I2A 173(3) . . ? N10 O10 O10A 82(5) . . ? N10 O10 I2A 74(3) . . ? O10A O10 I2A 14(3) . . ? N10 O11 I2A 87(4) . . ? N10 O11 I2B 95(4) . . ? I2A O11 I2B 11.1(10) . . ? O61B C61 O61A 95(4) . . ? I2A O10A O10 17(4) . . ? I2A O10A I2B 10.0(13) . . ? O10 O10A I2B 16(5) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 24.28 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.874 _refine_diff_density_min -1.947 _refine_diff_density_rms 0.129 # Attachment '- complex5.cif' data_tki157c_0m _database_code_depnum_ccdc_archive 'CCDC 803778' #TrackingRef '- complex5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101 H108 F10.40 N16 Ni6 O21 Si1.60' _chemical_formula_weight 2476.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 23.105(5) _cell_length_b 22.054(5) _cell_length_c 23.008(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11723(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9996 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 26.14 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5112 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6796 _exptl_absorpt_correction_T_max 0.8024 _exptl_absorpt_process_details 'Bruker SADABS' _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 'Bruker SMART Apex2 CCD' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90131 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.00 _reflns_number_total 11494 _reflns_number_gt 8490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+9.8425P] 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 none _refine_ls_number_reflns 11494 _refine_ls_number_parameters 774 _refine_ls_number_restraints 771 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1612 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.044 _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 0.534616(19) 0.612739(19) 0.30962(2) 0.03640(14) Uani 1 1 d U . . Ni2 Ni 0.5000 0.50548(3) 0.2500 0.0648(3) Uani 1 2 d SU . . Ni3 Ni 0.945412(18) 0.607552(19) 0.29180(2) 0.03457(13) Uani 1 1 d U . . Ni4 Ni 1.0000 0.50051(3) 0.2500 0.0534(2) Uani 1 2 d SU . . O1 O 0.52869(10) 0.52106(11) 0.32742(12) 0.0442(6) Uani 1 1 d U . . O2 O 0.56688(12) 0.44805(13) 0.38945(13) 0.0551(7) Uani 1 1 d U . . O3 O 0.45037(10) 0.59871(10) 0.27720(11) 0.0355(5) Uani 1 1 d U . . O4 O 0.35404(11) 0.61848(12) 0.30143(13) 0.0533(7) Uani 1 1 d U . . O5 O 0.92656(11) 0.51614(11) 0.28817(10) 0.0398(5) Uani 1 1 d U . . O6 O 0.87118(11) 0.44318(12) 0.33520(12) 0.0493(6) Uani 1 1 d U . . O7 O 0.96767(10) 0.59323(11) 0.20279(10) 0.0353(5) Uani 1 1 d U . . O8 O 0.93449(12) 0.61654(13) 0.10924(12) 0.0508(7) Uani 1 1 d U . . N1 N 0.61442(13) 0.59541(14) 0.34930(14) 0.0437(7) Uani 1 1 d U . . N2 N 0.56903(16) 0.45079(14) 0.24605(16) 0.0534(8) Uani 1 1 d U . . N3 N 0.48670(14) 0.64192(15) 0.37910(14) 0.0464(7) Uani 1 1 d U . . N4 N 0.44093(14) 0.69908(14) 0.21912(14) 0.0465(8) Uani 1 1 d U . . N5 N 0.91601(13) 0.59115(14) 0.37588(13) 0.0412(7) Uani 1 1 d U . . N6 N 1.01222(14) 0.44675(14) 0.31877(15) 0.0479(8) Uani 1 1 d U . . N7 N 0.87124(12) 0.63453(14) 0.25208(14) 0.0440(7) Uani 1 1 d U . . N8 N 1.02380(13) 0.69412(13) 0.18823(14) 0.0441(7) Uani 1 1 d U . . C1 C 0.65324(18) 0.6377(2) 0.36664(19) 0.0580(11) Uani 1 1 d U . . H1 H 0.6473 0.6778 0.3555 0.070 Uiso 1 1 calc R . . C2 C 0.70073(19) 0.6244(2) 0.3997(2) 0.0674(12) Uani 1 1 d U . . H2 H 0.7270 0.6544 0.4101 0.081 Uiso 1 1 calc R . . C3 C 0.7086(2) 0.5646(3) 0.4173(2) 0.0726(13) Uani 1 1 d U . . H3 H 0.7396 0.5542 0.4411 0.087 Uiso 1 1 calc R . . C4 C 0.67002(19) 0.5208(2) 0.3990(2) 0.0631(12) Uani 1 1 d U . . H4 H 0.6753 0.4804 0.4095 0.076 Uiso 1 1 calc R . . C5 C 0.62338(15) 0.53766(18) 0.36501(17) 0.0441(8) Uani 1 1 d U . . C6 C 0.57792(15) 0.49116(16) 0.34405(17) 0.0414(8) Uani 1 1 d U . . C7 C 0.60148(16) 0.45128(17) 0.29505(17) 0.0453(8) Uani 1 1 d U . . C8 C 0.65023(19) 0.4160(2) 0.2985(2) 0.0694(13) Uani 1 1 d U . . H8 H 0.6719 0.4152 0.3325 0.083 Uiso 1 1 calc R . . C9 C 0.6671(2) 0.3814(3) 0.2507(3) 0.0836(16) Uani 1 1 d U . . H9 H 0.7007 0.3582 0.2523 0.100 Uiso 1 1 calc R . . C10 C 0.6350(3) 0.3815(2) 0.2027(3) 0.0788(15) Uani 1 1 d U . . H10 H 0.6456 0.3582 0.1708 0.095 Uiso 1 1 calc R . . C11 C 0.5856(3) 0.4167(2) 0.2008(2) 0.0750(14) Uani 1 1 d U . . H11 H 0.5632 0.4168 0.1672 0.090 Uiso 1 1 calc R . . C12 C 0.5370(2) 0.4729(3) 0.4387(2) 0.0787(15) Uani 1 1 d U . . H12A H 0.5313 0.4417 0.4672 0.118 Uiso 1 1 calc R . . H12B H 0.5001 0.4884 0.4265 0.118 Uiso 1 1 calc R . . H12C H 0.5596 0.5051 0.4552 0.118 Uiso 1 1 calc R . . C13 C 0.5055(2) 0.6539(2) 0.43267(18) 0.0637(12) Uani 1 1 d U . . H13 H 0.5444 0.6470 0.4410 0.076 Uiso 1 1 calc R . . C14 C 0.4710(3) 0.6757(3) 0.4757(2) 0.0830(16) Uani 1 1 d U . . H14 H 0.4858 0.6845 0.5123 0.100 Uiso 1 1 calc R . . C15 C 0.4128(3) 0.6844(3) 0.4630(2) 0.0895(18) Uani 1 1 d U . . H15 H 0.3877 0.6990 0.4915 0.107 Uiso 1 1 calc R . . C16 C 0.3921(2) 0.6712(2) 0.4077(2) 0.0698(13) Uani 1 1 d U . . H16 H 0.3531 0.6763 0.3988 0.084 Uiso 1 1 calc R . . C17 C 0.43033(17) 0.65063(18) 0.36652(17) 0.0488(9) Uani 1 1 d U . . C18 C 0.41215(15) 0.63820(16) 0.30330(16) 0.0403(8) Uani 1 1 d U . . C19 C 0.40976(15) 0.69807(16) 0.26874(17) 0.0406(8) Uani 1 1 d U . . C20 C 0.37612(19) 0.74723(18) 0.2850(2) 0.0540(10) Uani 1 1 d U . . H20 H 0.3547 0.7460 0.3191 0.065 Uiso 1 1 calc R . . C21 C 0.3747(2) 0.79802(19) 0.2501(2) 0.0680(13) Uani 1 1 d U . . H21 H 0.3514 0.8309 0.2600 0.082 Uiso 1 1 calc R . . C22 C 0.4078(2) 0.7998(2) 0.2008(2) 0.0716(13) Uani 1 1 d U . . H22 H 0.4084 0.8342 0.1774 0.086 Uiso 1 1 calc R . . C23 C 0.4400(2) 0.74988(19) 0.1866(2) 0.0634(12) Uani 1 1 d U . . H23 H 0.4623 0.7511 0.1529 0.076 Uiso 1 1 calc R . . C24 C 0.3441(2) 0.5606(2) 0.3258(3) 0.0841(17) Uani 1 1 d U . . H24A H 0.3037 0.5508 0.3230 0.126 Uiso 1 1 calc R . . H24B H 0.3555 0.5607 0.3659 0.126 Uiso 1 1 calc R . . H24C H 0.3663 0.5308 0.3051 0.126 Uiso 1 1 calc R . . C25 C 0.90298(18) 0.6334(2) 0.41620(18) 0.0547(10) Uani 1 1 d U . . H25 H 0.9131 0.6735 0.4087 0.066 Uiso 1 1 calc R . . C26 C 0.87569(19) 0.6204(2) 0.46746(19) 0.0612(11) Uani 1 1 d U . . H26 H 0.8678 0.6510 0.4941 0.073 Uiso 1 1 calc R . . C27 C 0.8601(2) 0.5617(2) 0.47902(19) 0.0635(12) Uani 1 1 d U . . H27 H 0.8414 0.5517 0.5135 0.076 Uiso 1 1 calc R . . C28 C 0.87289(18) 0.5174(2) 0.43815(19) 0.0561(10) Uani 1 1 d U . . H28 H 0.8625 0.4773 0.4448 0.067 Uiso 1 1 calc R . . C29 C 0.90142(15) 0.53353(17) 0.38719(15) 0.0414(8) Uani 1 1 d U . . C30 C 0.91658(15) 0.48682(16) 0.33963(15) 0.0388(7) Uani 1 1 d U . . C31 C 0.96871(16) 0.44711(17) 0.35695(17) 0.0444(8) Uani 1 1 d U . . C32 C 0.9708(2) 0.4122(2) 0.4073(2) 0.0682(13) Uani 1 1 d U . . H32 H 0.9404 0.4135 0.4338 0.082 Uiso 1 1 calc R . . C33 C 1.0185(3) 0.3755(3) 0.4176(2) 0.0830(16) Uani 1 1 d U . . H33 H 1.0198 0.3504 0.4501 0.100 Uiso 1 1 calc R . . C34 C 1.0647(2) 0.3770(2) 0.3781(2) 0.0763(14) Uani 1 1 d U . . H34 H 1.0981 0.3545 0.3846 0.092 Uiso 1 1 calc R . . C35 C 1.05946(19) 0.4124(2) 0.3299(2) 0.0632(12) Uani 1 1 d U . . H35 H 1.0898 0.4130 0.3034 0.076 Uiso 1 1 calc R . . C36 C 0.8178(2) 0.4676(2) 0.3136(2) 0.0705(13) Uani 1 1 d U . . H36A H 0.7893 0.4360 0.3116 0.106 Uiso 1 1 calc R . . H36B H 0.8239 0.4843 0.2756 0.106 Uiso 1 1 calc R . . H36C H 0.8044 0.4989 0.3394 0.106 Uiso 1 1 calc R . . C37 C 0.81941(17) 0.6428(2) 0.2777(2) 0.0603(11) Uani 1 1 d U . . H37 H 0.8158 0.6366 0.3175 0.072 Uiso 1 1 calc R . . C38 C 0.7711(2) 0.6605(3) 0.2458(2) 0.0801(16) Uani 1 1 d U . . H38 H 0.7355 0.6657 0.2640 0.096 Uiso 1 1 calc R . . C39 C 0.77656(19) 0.6699(3) 0.1879(2) 0.0855(18) Uani 1 1 d U . . H39 H 0.7448 0.6825 0.1662 0.103 Uiso 1 1 calc R . . C40 C 0.82957(17) 0.6607(2) 0.1610(2) 0.0651(12) Uani 1 1 d U . . H40 H 0.8335 0.6661 0.1211 0.078 Uiso 1 1 calc R . . C41 C 0.87678(15) 0.64330(18) 0.19455(17) 0.0444(9) Uani 1 1 d U . . C42 C 0.93806(15) 0.63380(16) 0.16889(16) 0.0397(8) Uani 1 1 d U . . C43 C 0.97037(15) 0.69452(16) 0.16544(16) 0.0406(8) Uani 1 1 d U . . C44 C 0.9483(2) 0.74559(19) 0.13806(19) 0.0549(10) Uani 1 1 d U . . H44 H 0.9112 0.7448 0.1223 0.066 Uiso 1 1 calc R . . C45 C 0.9815(2) 0.79750(19) 0.1343(2) 0.0622(11) Uani 1 1 d U . . H45 H 0.9672 0.8319 0.1157 0.075 Uiso 1 1 calc R . . C46 C 1.0355(2) 0.79760(19) 0.1582(2) 0.0678(12) Uani 1 1 d U . . H46 H 1.0585 0.8321 0.1563 0.081 Uiso 1 1 calc R . . C47 C 1.0556(2) 0.74536(18) 0.1853(2) 0.0580(11) Uani 1 1 d U . . H47 H 1.0922 0.7458 0.2021 0.070 Uiso 1 1 calc R . . C48 C 0.9115(3) 0.5576(2) 0.0986(2) 0.0774(15) Uani 1 1 d U . . H48A H 0.9108 0.5501 0.0575 0.116 Uiso 1 1 calc R . . H48B H 0.8729 0.5552 0.1138 0.116 Uiso 1 1 calc R . . H48C H 0.9355 0.5278 0.1172 0.116 Uiso 1 1 calc R . . C60 C 0.1349(7) 0.9372(6) 0.4506(6) 0.212(6) Uani 1 1 d DU . . C70 C 0.2819(5) 0.9512(5) 0.3488(5) 0.160(4) Uani 1 1 d DU . . C50A C 0.1509(12) 0.3315(16) 0.0128(16) 0.172(13) Uiso 0.30 1 d PDU A 1 C50B C 0.1241(15) 0.2598(14) 0.0464(14) 0.108(10) Uiso 0.20 1 d PDU A 2 O50 O 0.0969(6) 0.3018(6) 0.0087(6) 0.162(5) Uiso 0.50 1 d PDU . . O60 O 0.1070(2) 0.8791(3) 0.4559(3) 0.1361(19) Uani 1 1 d DU . . O70 O 0.2938(2) 0.8941(3) 0.3250(3) 0.140(2) Uani 1 1 d DU . . Si1 Si 0.25151(6) 0.21254(9) 0.94471(9) 0.0712(5) Uani 0.80 1 d PU . . F1 F 0.2501(6) 0.4221(6) 0.9905(9) 0.198(8) Uani 0.40 1 d PU . . O80 O 0.3084(8) 0.2680(10) 0.1060(8) 0.503(14) Uani 1 1 d U . . C80 C 0.2477(14) 0.2837(18) 0.132(2) 0.48(2) Uiso 1 1 d U . . F3 F 0.25453(16) 0.28689(17) 0.93509(18) 0.0835(11) Uani 0.80 1 d PU B . F6 F 0.24932(17) 0.1381(2) 0.9581(3) 0.1140(17) Uani 0.80 1 d PU B . F4 F 0.2623(5) 0.2152(6) 1.0101(4) 0.103(3) Uani 0.45 1 d PU B 3 F5 F 0.3233(4) 0.2014(5) 0.9290(4) 0.068(2) Uani 0.45 1 d PU B 3 F7 F 0.2427(5) 0.1998(5) 0.8682(5) 0.114(3) Uani 0.45 1 d PU B 3 F8 F 0.1815(3) 0.2147(6) 0.9449(10) 0.147(5) Uani 0.45 1 d PU B 3 F8A F 0.1934(6) 0.2263(7) 0.9991(7) 0.130(5) Uani 0.35 1 d PU B 4 F7A F 0.2026(8) 0.2079(6) 0.9002(8) 0.120(5) Uani 0.35 1 d PU B 4 F4A F 0.2929(6) 0.2309(6) 1.0094(5) 0.092(4) Uani 0.35 1 d PU B 4 F5A F 0.3068(7) 0.2122(7) 0.9086(7) 0.107(5) Uani 0.35 1 d PU B 4 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 0.0353(3) 0.0354(2) 0.0385(3) -0.00227(18) -0.00058(18) 0.00006(18) Ni2 0.0702(5) 0.0367(4) 0.0877(6) 0.000 -0.0497(5) 0.000 Ni3 0.0302(2) 0.0352(2) 0.0383(3) 0.00099(18) -0.00165(17) 0.00260(17) Ni4 0.0686(5) 0.0376(4) 0.0539(5) 0.000 0.0303(4) 0.000 O1 0.0322(12) 0.0408(13) 0.0597(16) 0.0081(11) -0.0085(11) 0.0000(10) O2 0.0596(17) 0.0530(16) 0.0527(17) 0.0134(13) -0.0031(13) 0.0045(13) O3 0.0324(12) 0.0339(12) 0.0402(13) 0.0009(10) 0.0008(10) 0.0047(9) O4 0.0354(14) 0.0486(15) 0.076(2) -0.0014(13) 0.0106(13) -0.0001(11) O5 0.0450(13) 0.0393(13) 0.0351(13) -0.0008(10) 0.0031(10) -0.0036(10) O6 0.0412(14) 0.0473(15) 0.0594(17) 0.0030(12) 0.0035(12) -0.0106(11) O7 0.0307(12) 0.0388(12) 0.0364(13) 0.0063(10) -0.0042(9) -0.0017(9) O8 0.0586(17) 0.0550(16) 0.0389(14) 0.0040(12) -0.0108(12) -0.0007(13) N1 0.0367(16) 0.0469(17) 0.0476(18) -0.0077(14) -0.0010(13) -0.0065(13) N2 0.065(2) 0.0368(17) 0.059(2) -0.0032(14) -0.0201(17) -0.0032(14) N3 0.0460(17) 0.0498(18) 0.0433(17) -0.0020(14) -0.0010(14) 0.0045(14) N4 0.055(2) 0.0327(15) 0.052(2) 0.0050(14) -0.0011(15) 0.0026(14) N5 0.0381(16) 0.0474(17) 0.0381(16) -0.0032(13) -0.0013(12) 0.0069(13) N6 0.0465(18) 0.0385(16) 0.059(2) -0.0016(14) 0.0096(15) 0.0029(13) N7 0.0312(15) 0.0494(18) 0.0514(19) 0.0084(14) -0.0015(13) 0.0049(13) N8 0.0413(17) 0.0348(15) 0.056(2) 0.0018(14) 0.0032(14) -0.0035(13) C1 0.047(2) 0.064(3) 0.063(3) -0.011(2) -0.0063(19) -0.0125(19) C2 0.047(2) 0.085(3) 0.069(3) -0.021(3) -0.011(2) -0.018(2) C3 0.046(2) 0.104(4) 0.068(3) -0.014(3) -0.023(2) -0.001(2) C4 0.053(2) 0.066(3) 0.071(3) -0.003(2) -0.020(2) 0.005(2) C5 0.0344(18) 0.055(2) 0.043(2) -0.0055(17) -0.0060(15) -0.0004(15) C6 0.0356(17) 0.0414(18) 0.047(2) 0.0079(15) -0.0076(15) 0.0025(14) C7 0.0395(19) 0.042(2) 0.054(2) 0.0040(16) -0.0068(16) -0.0050(15) C8 0.042(2) 0.085(3) 0.081(3) -0.020(3) -0.013(2) 0.012(2) C9 0.055(3) 0.094(4) 0.102(4) -0.033(3) -0.002(3) 0.011(3) C10 0.085(4) 0.073(3) 0.079(3) -0.025(3) 0.011(3) -0.007(3) C11 0.101(4) 0.056(3) 0.069(3) -0.017(2) -0.022(3) -0.001(3) C12 0.090(4) 0.086(4) 0.060(3) 0.017(3) 0.014(3) -0.001(3) C13 0.074(3) 0.076(3) 0.041(2) -0.007(2) -0.005(2) 0.013(2) C14 0.108(4) 0.098(4) 0.044(3) -0.012(3) -0.004(3) 0.029(3) C15 0.105(4) 0.113(5) 0.050(3) -0.011(3) 0.020(3) 0.037(4) C16 0.065(3) 0.090(3) 0.054(3) -0.005(2) 0.013(2) 0.029(3) C17 0.050(2) 0.049(2) 0.047(2) -0.0013(17) 0.0097(16) 0.0101(17) C18 0.0325(17) 0.0419(19) 0.046(2) -0.0016(15) 0.0032(14) 0.0065(14) C19 0.0350(18) 0.0358(17) 0.051(2) -0.0045(15) -0.0064(15) 0.0037(14) C20 0.052(2) 0.045(2) 0.065(3) -0.0121(18) -0.0074(19) 0.0084(18) C21 0.071(3) 0.036(2) 0.097(4) -0.008(2) -0.015(3) 0.012(2) C22 0.088(4) 0.036(2) 0.091(4) 0.012(2) -0.004(3) 0.006(2) C23 0.085(3) 0.039(2) 0.066(3) 0.0113(19) 0.002(2) -0.002(2) C24 0.067(3) 0.056(3) 0.129(5) 0.008(3) 0.037(3) -0.006(2) C25 0.056(2) 0.056(2) 0.052(2) -0.0114(18) 0.0025(19) 0.0113(19) C26 0.060(3) 0.074(3) 0.050(2) -0.022(2) 0.004(2) 0.014(2) C27 0.061(3) 0.088(3) 0.041(2) -0.001(2) 0.014(2) 0.007(2) C28 0.054(2) 0.067(3) 0.048(2) 0.0040(19) 0.0109(18) -0.002(2) C29 0.0365(18) 0.053(2) 0.0348(18) 0.0003(15) 0.0006(14) 0.0032(15) C30 0.0403(18) 0.0409(18) 0.0351(18) 0.0036(14) 0.0038(14) -0.0066(14) C31 0.044(2) 0.048(2) 0.041(2) 0.0000(16) 0.0040(16) -0.0023(16) C32 0.069(3) 0.085(3) 0.050(3) 0.018(2) 0.006(2) 0.015(2) C33 0.090(4) 0.093(4) 0.066(3) 0.021(3) -0.009(3) 0.027(3) C34 0.071(3) 0.074(3) 0.084(4) -0.002(3) -0.013(3) 0.025(3) C35 0.052(2) 0.055(3) 0.083(3) -0.004(2) 0.011(2) 0.012(2) C36 0.047(2) 0.075(3) 0.089(4) -0.011(3) -0.003(2) -0.014(2) C37 0.038(2) 0.082(3) 0.061(3) 0.019(2) 0.0069(18) 0.009(2) C38 0.035(2) 0.120(5) 0.086(3) 0.036(3) 0.005(2) 0.014(3) C39 0.034(2) 0.135(5) 0.088(4) 0.045(3) -0.009(2) 0.009(3) C40 0.043(2) 0.093(3) 0.060(3) 0.033(2) -0.0078(18) 0.004(2) C41 0.0334(18) 0.052(2) 0.048(2) 0.0124(17) -0.0057(15) -0.0005(15) C42 0.0356(18) 0.0438(19) 0.0396(19) 0.0068(15) -0.0049(14) 0.0005(14) C43 0.0431(19) 0.0391(18) 0.040(2) 0.0051(15) 0.0062(15) 0.0034(15) C44 0.058(2) 0.050(2) 0.057(3) 0.0110(19) 0.0075(19) 0.0115(18) C45 0.081(3) 0.039(2) 0.067(3) 0.013(2) 0.016(2) 0.013(2) C46 0.084(3) 0.037(2) 0.083(3) 0.004(2) 0.015(3) -0.007(2) C47 0.058(3) 0.039(2) 0.076(3) -0.003(2) 0.006(2) -0.0108(18) C48 0.099(4) 0.065(3) 0.068(3) -0.003(2) -0.035(3) -0.005(3) C60 0.257(15) 0.192(10) 0.186(12) -0.044(10) 0.013(11) -0.007(9) C70 0.159(8) 0.161(8) 0.159(9) -0.036(7) 0.029(7) 0.030(7) O60 0.083(3) 0.176(5) 0.149(5) 0.000(4) -0.001(3) 0.017(3) O70 0.114(4) 0.162(5) 0.144(5) -0.017(4) 0.014(4) 0.034(4) Si1 0.0456(8) 0.0704(11) 0.0976(13) 0.0495(10) -0.0127(8) -0.0093(7) F1 0.177(12) 0.081(8) 0.34(2) -0.050(10) -0.088(12) 0.017(7) O80 0.43(2) 0.71(3) 0.37(2) -0.07(2) -0.091(18) -0.34(2) F3 0.097(3) 0.065(2) 0.089(3) 0.0309(19) -0.033(2) -0.0119(17) F6 0.102(3) 0.074(3) 0.166(5) 0.065(3) 0.002(3) -0.009(2) F4 0.139(9) 0.115(7) 0.056(4) 0.041(4) 0.036(5) 0.024(6) F5 0.050(3) 0.074(5) 0.081(6) 0.027(4) 0.015(3) 0.012(3) F7 0.163(9) 0.079(5) 0.099(5) 0.007(4) -0.064(5) 0.008(6) F8 0.031(3) 0.123(7) 0.289(14) 0.037(14) 0.001(6) -0.001(3) F8A 0.095(7) 0.149(10) 0.146(10) 0.055(9) 0.054(7) 0.026(8) F7A 0.144(11) 0.086(8) 0.131(10) 0.035(10) -0.097(8) -0.047(11) F4A 0.110(8) 0.095(8) 0.072(6) 0.005(5) -0.034(6) 0.036(7) F5A 0.120(10) 0.092(8) 0.109(10) -0.017(8) 0.071(8) -0.045(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 2.048(3) . ? Ni1 O3 2.051(2) 3_655 ? Ni1 O1 2.067(2) . ? Ni1 N1 2.093(3) . ? Ni1 N4 2.093(3) 3_655 ? Ni1 O3 2.107(2) . ? Ni1 Ni2 2.8491(9) . ? Ni2 O1 1.931(3) 3_655 ? Ni2 O1 1.931(3) . ? Ni2 N2 2.002(4) . ? Ni2 N2 2.002(4) 3_655 ? Ni2 Ni1 2.8491(9) 3_655 ? Ni3 N7 2.031(3) . ? Ni3 O7 2.037(2) 3_755 ? Ni3 O5 2.064(2) . ? Ni3 N5 2.082(3) . ? Ni3 N8 2.089(3) 3_755 ? Ni3 O7 2.135(2) . ? Ni3 Ni4 2.8441(9) . ? Ni4 O5 1.942(2) 3_755 ? Ni4 O5 1.942(2) . ? Ni4 N6 1.997(3) 3_755 ? Ni4 N6 1.997(3) . ? Ni4 Ni3 2.8441(9) 3_755 ? O1 C6 1.369(4) . ? O2 C12 1.435(6) . ? O2 C6 1.435(4) . ? O3 C18 1.378(4) . ? O3 Ni1 2.051(2) 3_655 ? O4 C24 1.414(5) . ? O4 C18 1.412(4) . ? O5 C30 1.369(4) . ? O6 C30 1.427(4) . ? O6 C36 1.434(5) . ? O7 C42 1.370(4) . ? O7 Ni3 2.037(2) 3_755 ? O8 C48 1.425(5) . ? O8 C42 1.427(5) . ? N1 C5 1.340(5) . ? N1 C1 1.354(5) . ? N2 C11 1.339(6) . ? N2 C7 1.354(5) . ? N3 C13 1.333(5) . ? N3 C17 1.348(5) . ? N4 C19 1.350(5) . ? N4 C23 1.348(5) . ? N4 Ni1 2.093(3) 3_655 ? N5 C29 1.340(5) . ? N5 C25 1.349(5) . ? N6 C31 1.335(5) . ? N6 C35 1.353(5) . ? N7 C41 1.344(5) . ? N7 C37 1.347(5) . ? N8 C43 1.341(5) . ? N8 C47 1.349(5) . ? N8 Ni3 2.089(3) 3_755 ? C1 C2 1.367(6) . ? C2 C3 1.392(7) . ? C3 C4 1.380(6) . ? C4 C5 1.383(5) . ? C5 C6 1.545(5) . ? C6 C7 1.530(6) . ? C7 C8 1.371(6) . ? C8 C9 1.395(7) . ? C9 C10 1.329(8) . ? C10 C11 1.381(8) . ? C13 C14 1.359(6) . ? C14 C15 1.390(8) . ? C15 C16 1.390(7) . ? C16 C17 1.373(5) . ? C17 C18 1.539(5) . ? C18 C19 1.542(5) . ? C19 C20 1.385(5) . ? C20 C21 1.379(7) . ? C21 C22 1.368(7) . ? C22 C23 1.369(7) . ? C25 C26 1.368(6) . ? C26 C27 1.371(7) . ? C27 C28 1.387(6) . ? C28 C29 1.391(5) . ? C29 C30 1.543(5) . ? C30 C31 1.541(5) . ? C31 C32 1.391(6) . ? C32 C33 1.389(7) . ? C33 C34 1.402(8) . ? C34 C35 1.360(7) . ? C37 C38 1.392(6) . ? C38 C39 1.354(7) . ? C39 C40 1.387(7) . ? C40 C41 1.390(5) . ? C41 C42 1.548(5) . ? C42 C43 1.535(5) . ? C43 C44 1.388(5) . ? C44 C45 1.381(6) . ? C45 C46 1.363(7) . ? C46 C47 1.391(6) . ? C60 O60 1.439(11) . ? C70 O70 1.399(9) . ? C50A O50 1.411(18) . ? C50B O50 1.415(18) . ? Si1 F5A 1.524(14) . ? Si1 F7A 1.528(10) . ? Si1 F4 1.526(11) . ? Si1 F8 1.618(7) . ? Si1 F3 1.656(4) . ? Si1 F6 1.671(4) . ? Si1 F5 1.715(9) . ? Si1 F7 1.793(10) . ? Si1 F4A 1.814(11) . ? Si1 F8A 1.862(12) . ? O80 C80 1.56(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ni1 O3 154.03(11) . 3_655 ? N3 Ni1 O1 96.71(12) . . ? O3 Ni1 O1 93.24(10) 3_655 . ? N3 Ni1 N1 101.13(12) . . ? O3 Ni1 N1 104.38(11) 3_655 . ? O1 Ni1 N1 78.08(11) . . ? N3 Ni1 N4 96.12(13) . 3_655 ? O3 Ni1 N4 77.52(11) 3_655 3_655 ? O1 Ni1 N4 165.93(12) . 3_655 ? N1 Ni1 N4 93.79(12) . 3_655 ? N3 Ni1 O3 79.82(11) . . ? O3 Ni1 O3 77.84(10) 3_655 . ? O1 Ni1 O3 82.26(9) . . ? N1 Ni1 O3 160.30(11) . . ? N4 Ni1 O3 105.73(11) 3_655 . ? N3 Ni1 Ni2 119.01(9) . . ? O3 Ni1 Ni2 56.86(6) 3_655 . ? O1 Ni1 Ni2 42.67(8) . . ? N1 Ni1 Ni2 107.80(8) . . ? N4 Ni1 Ni2 132.76(9) 3_655 . ? O3 Ni1 Ni2 56.52(6) . . ? O1 Ni2 O1 159.49(15) 3_655 . ? O1 Ni2 N2 109.81(13) 3_655 . ? O1 Ni2 N2 82.86(12) . . ? O1 Ni2 N2 82.86(12) 3_655 3_655 ? O1 Ni2 N2 109.81(13) . 3_655 ? N2 Ni2 N2 105.90(19) . 3_655 ? O1 Ni2 Ni1 46.52(7) 3_655 3_655 ? O1 Ni2 Ni1 113.11(8) . 3_655 ? N2 Ni2 Ni1 134.59(11) . 3_655 ? N2 Ni2 Ni1 107.36(9) 3_655 3_655 ? O1 Ni2 Ni1 113.12(8) 3_655 . ? O1 Ni2 Ni1 46.52(7) . . ? N2 Ni2 Ni1 107.36(9) . . ? N2 Ni2 Ni1 134.59(11) 3_655 . ? Ni1 Ni2 Ni1 67.74(3) 3_655 . ? N7 Ni3 O7 154.80(11) . 3_755 ? N7 Ni3 O5 95.16(11) . . ? O7 Ni3 O5 93.39(10) 3_755 . ? N7 Ni3 N5 101.17(12) . . ? O7 Ni3 N5 103.76(11) 3_755 . ? O5 Ni3 N5 78.40(11) . . ? N7 Ni3 N8 96.81(13) . 3_755 ? O7 Ni3 N8 78.03(11) 3_755 3_755 ? O5 Ni3 N8 166.79(11) . 3_755 ? N5 Ni3 N8 93.76(12) . 3_755 ? N7 Ni3 O7 79.34(11) . . ? O7 Ni3 O7 78.36(10) 3_755 . ? O5 Ni3 O7 82.39(9) . . ? N5 Ni3 O7 160.76(11) . . ? N8 Ni3 O7 105.32(11) 3_755 . ? N7 Ni3 Ni4 117.72(9) . . ? O7 Ni3 Ni4 56.95(7) 3_755 . ? O5 Ni3 Ni4 43.05(7) . . ? N5 Ni3 Ni4 108.34(8) . . ? N8 Ni3 Ni4 133.01(9) 3_755 . ? O7 Ni3 Ni4 56.36(6) . . ? O5 Ni4 O5 159.54(15) 3_755 . ? O5 Ni4 N6 82.56(12) 3_755 3_755 ? O5 Ni4 N6 109.89(12) . 3_755 ? O5 Ni4 N6 109.89(12) 3_755 . ? O5 Ni4 N6 82.56(12) . . ? N6 Ni4 N6 107.18(19) 3_755 . ? O5 Ni4 Ni3 46.53(7) 3_755 3_755 ? O5 Ni4 Ni3 113.15(8) . 3_755 ? N6 Ni4 Ni3 106.71(9) 3_755 3_755 ? N6 Ni4 Ni3 134.26(10) . 3_755 ? O5 Ni4 Ni3 113.15(8) 3_755 . ? O5 Ni4 Ni3 46.53(7) . . ? N6 Ni4 Ni3 134.26(10) 3_755 . ? N6 Ni4 Ni3 106.71(9) . . ? Ni3 Ni4 Ni3 67.79(3) 3_755 . ? C6 O1 Ni2 117.2(2) . . ? C6 O1 Ni1 118.1(2) . . ? Ni2 O1 Ni1 90.81(11) . . ? C12 O2 C6 114.0(3) . . ? C18 O3 Ni1 115.9(2) . 3_655 ? C18 O3 Ni1 110.2(2) . . ? Ni1 O3 Ni1 99.58(10) 3_655 . ? C24 O4 C18 114.9(3) . . ? C30 O5 Ni4 117.0(2) . . ? C30 O5 Ni3 117.5(2) . . ? Ni4 O5 Ni3 90.42(10) . . ? C30 O6 C36 113.8(3) . . ? C42 O7 Ni3 115.2(2) . 3_755 ? C42 O7 Ni3 109.2(2) . . ? Ni3 O7 Ni3 98.97(10) 3_755 . ? C48 O8 C42 115.5(3) . . ? C5 N1 C1 118.2(3) . . ? C5 N1 Ni1 115.3(2) . . ? C1 N1 Ni1 125.9(3) . . ? C11 N2 C7 119.6(4) . . ? C11 N2 Ni2 126.9(3) . . ? C7 N2 Ni2 113.5(3) . . ? C13 N3 C17 119.0(4) . . ? C13 N3 Ni1 127.4(3) . . ? C17 N3 Ni1 113.5(3) . . ? C19 N4 C23 118.4(4) . . ? C19 N4 Ni1 113.3(2) . 3_655 ? C23 N4 Ni1 125.8(3) . 3_655 ? C29 N5 C25 117.8(3) . . ? C29 N5 Ni3 115.3(2) . . ? C25 N5 Ni3 126.3(3) . . ? C31 N6 C35 119.1(4) . . ? C31 N6 Ni4 114.3(3) . . ? C35 N6 Ni4 126.6(3) . . ? C41 N7 C37 119.7(3) . . ? C41 N7 Ni3 113.9(2) . . ? C37 N7 Ni3 126.4(3) . . ? C43 N8 C47 118.4(3) . . ? C43 N8 Ni3 113.9(2) . 3_755 ? C47 N8 Ni3 126.2(3) . 3_755 ? N1 C1 C2 123.2(4) . . ? C3 C2 C1 118.1(4) . . ? C2 C3 C4 119.3(4) . . ? C3 C4 C5 119.2(4) . . ? N1 C5 C4 121.9(4) . . ? N1 C5 C6 116.2(3) . . ? C4 C5 C6 121.9(4) . . ? O1 C6 O2 112.0(3) . . ? O1 C6 C7 111.5(3) . . ? O2 C6 C7 102.6(3) . . ? O1 C6 C5 109.4(3) . . ? O2 C6 C5 109.5(3) . . ? C7 C6 C5 111.7(3) . . ? N2 C7 C8 119.9(4) . . ? N2 C7 C6 114.9(3) . . ? C8 C7 C6 125.2(4) . . ? C7 C8 C9 119.7(5) . . ? C10 C9 C8 119.8(5) . . ? C9 C10 C11 119.3(5) . . ? N2 C11 C10 121.8(5) . . ? N3 C13 C14 123.5(5) . . ? C13 C14 C15 117.7(5) . . ? C16 C15 C14 119.7(4) . . ? C17 C16 C15 118.7(5) . . ? N3 C17 C16 121.4(4) . . ? N3 C17 C18 116.2(3) . . ? C16 C17 C18 122.4(4) . . ? O3 C18 O4 113.7(3) . . ? O3 C18 C17 110.5(3) . . ? O4 C18 C17 110.1(3) . . ? O3 C18 C19 109.8(3) . . ? O4 C18 C19 102.4(3) . . ? C17 C18 C19 110.2(3) . . ? N4 C19 C20 121.0(4) . . ? N4 C19 C18 115.5(3) . . ? C20 C19 C18 123.4(4) . . ? C21 C20 C19 119.5(4) . . ? C22 C21 C20 119.5(4) . . ? C21 C22 C23 118.6(4) . . ? N4 C23 C22 123.0(5) . . ? N5 C25 C26 123.4(4) . . ? C27 C26 C25 119.1(4) . . ? C26 C27 C28 118.5(4) . . ? C27 C28 C29 119.5(4) . . ? N5 C29 C28 121.7(4) . . ? N5 C29 C30 116.0(3) . . ? C28 C29 C30 122.3(4) . . ? O5 C30 O6 112.4(3) . . ? O5 C30 C31 111.1(3) . . ? O6 C30 C31 102.1(3) . . ? O5 C30 C29 109.6(3) . . ? O6 C30 C29 109.5(3) . . ? C31 C30 C29 111.9(3) . . ? N6 C31 C32 121.2(4) . . ? N6 C31 C30 114.9(3) . . ? C32 C31 C30 123.8(4) . . ? C33 C32 C31 119.5(5) . . ? C32 C33 C34 118.6(5) . . ? C35 C34 C33 118.3(5) . . ? N6 C35 C34 123.2(5) . . ? N7 C37 C38 121.4(4) . . ? C39 C38 C37 119.1(4) . . ? C38 C39 C40 119.9(4) . . ? C39 C40 C41 119.1(4) . . ? N7 C41 C40 120.8(4) . . ? N7 C41 C42 116.3(3) . . ? C40 C41 C42 122.9(3) . . ? O7 C42 O8 113.7(3) . . ? O7 C42 C43 110.9(3) . . ? O8 C42 C43 102.2(3) . . ? O7 C42 C41 109.1(3) . . ? O8 C42 C41 110.5(3) . . ? C43 C42 C41 110.3(3) . . ? N8 C43 C44 121.4(4) . . ? N8 C43 C42 114.9(3) . . ? C44 C43 C42 123.6(3) . . ? C43 C44 C45 119.9(4) . . ? C46 C45 C44 118.9(4) . . ? C45 C46 C47 119.1(4) . . ? N8 C47 C46 122.2(4) . . ? C50B O50 C50A 83(2) . . ? F5A Si1 F7A 104.8(11) . . ? F5A Si1 F4 113.6(8) . . ? F7A Si1 F4 141.6(10) . . ? F5A Si1 F8 147.1(10) . . ? F7A Si1 F8 42.7(7) . . ? F4 Si1 F8 99.2(8) . . ? F5A Si1 F3 84.1(6) . . ? F7A Si1 F3 90.5(5) . . ? F4 Si1 F3 95.0(5) . . ? F8 Si1 F3 90.8(5) . . ? F5A Si1 F6 96.9(6) . . ? F7A Si1 F6 92.0(5) . . ? F4 Si1 F6 82.0(5) . . ? F8 Si1 F6 89.9(5) . . ? F3 Si1 F6 177.0(3) . . ? F5A Si1 F5 22.1(7) . . ? F7A Si1 F5 124.4(10) . . ? F4 Si1 F5 93.2(5) . . ? F8 Si1 F5 166.3(9) . . ? F3 Si1 F5 94.2(4) . . ? F6 Si1 F5 85.8(4) . . ? F5A Si1 F7 63.9(8) . . ? F7A Si1 F7 41.3(8) . . ? F4 Si1 F7 172.6(6) . . ? F8 Si1 F7 83.9(7) . . ? F3 Si1 F7 91.7(4) . . ? F6 Si1 F7 91.3(4) . . ? F5 Si1 F7 83.1(5) . . ? F5A Si1 F4A 90.3(8) . . ? F7A Si1 F4A 162.6(10) . . ? F4 Si1 F4A 25.5(5) . . ? F8 Si1 F4A 121.2(9) . . ? F3 Si1 F4A 82.3(5) . . ? F6 Si1 F4A 94.8(5) . . ? F5 Si1 F4A 72.2(6) . . ? F7 Si1 F4A 154.0(6) . . ? F5A Si1 F8A 166.5(9) . . ? F7A Si1 F8A 85.9(9) . . ? F4 Si1 F8A 56.5(6) . . ? F8 Si1 F8A 43.3(7) . . ? F3 Si1 F8A 87.6(5) . . ? F6 Si1 F8A 90.9(5) . . ? F5 Si1 F8A 149.6(7) . . ? F7 Si1 F8A 127.1(6) . . ? F4A Si1 F8A 78.0(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.911 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.087