# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Susan A. Bourne' _publ_contact_author_address ; Chemistry Department, University of Cape Town, Rondebosch, 7701, Cape Town, South Africa ; _publ_contact_author_email susan.bourne@uct.ac.za _publ_contact_author_phone '+27 21 650 2563' _publ_contact_author_fax '+27 21 650 5195' loop_ _publ_author_name S.Bourne G.Mehlana G.Ramon data_1 _database_code_depnum_ccdc_archive 'CCDC 850071' #TrackingRef '- DT-ART-10-2011-012016 CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H9 N O2' _chemical_formula_weight 199.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.7482(12) _cell_length_b 11.7997(13) _cell_length_c 14.7279(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1867.9(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9874 _exptl_absorpt_correction_T_max 0.9971 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6844 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 27.17 _reflns_number_total 4121 _reflns_number_gt 2564 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 3.0(17) _refine_ls_number_reflns 4121 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1068 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _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 N1A N 0.1147(3) 1.1848(2) 0.02214(17) 0.0353(7) Uani 1 1 d . . . C2A C 0.2146(3) 1.1193(2) 0.02923(18) 0.0306(7) Uani 1 1 d . . . H2A H 0.2928 1.1548 0.0389 0.037 Uiso 1 1 calc R . . C3A C 0.2113(3) 1.0031(2) 0.02336(19) 0.0300(7) Uani 1 1 d . . . H3A H 0.2857 0.9603 0.0296 0.036 Uiso 1 1 calc R . . C4A C 0.0984(3) 0.9483(2) 0.00820(18) 0.0245(7) Uani 1 1 d . . . C5A C -0.0073(3) 1.0164(3) -0.0012(2) 0.0313(8) Uani 1 1 d . . . H5A H -0.0863 0.9836 -0.0131 0.038 Uiso 1 1 calc R . . C6A C 0.0053(3) 1.1325(3) 0.0073(2) 0.0352(8) Uani 1 1 d . . . H6A H -0.0674 1.1779 0.0023 0.042 Uiso 1 1 calc R . . C7A C 0.0920(3) 0.8229(2) 0.00276(19) 0.0245(7) Uani 1 1 d . . . C8A C 0.1641(3) 0.7567(2) 0.06099(19) 0.0275(7) Uani 1 1 d . . . H8A H 0.2160 0.7922 0.1048 0.033 Uiso 1 1 calc R . . C9A C 0.1606(3) 0.6390(3) 0.05539(19) 0.0286(7) Uani 1 1 d . . . H9A H 0.2095 0.5947 0.0957 0.034 Uiso 1 1 calc R . . C10A C 0.0860(3) 0.5857(3) -0.00875(18) 0.0251(7) Uani 1 1 d . . . C11A C 0.0154(3) 0.6519(3) -0.0674(2) 0.0285(7) Uani 1 1 d . . . H11A H -0.0345 0.6161 -0.1122 0.034 Uiso 1 1 calc R . . C12A C 0.0164(3) 0.7693(3) -0.0617(2) 0.0265(7) Uani 1 1 d . . . H12A H -0.0341 0.8132 -0.1013 0.032 Uiso 1 1 calc R . . C13A C 0.0765(3) 0.4596(3) -0.0157(2) 0.0286(7) Uani 1 1 d . . . O14A O 0.0046(2) 0.41260(19) -0.06730(15) 0.0431(6) Uani 1 1 d . . . O15A O 0.1514(2) 0.40315(19) 0.03915(15) 0.0391(6) Uani 1 1 d . . . H15A H 0.125(4) 0.317(3) 0.029(2) 0.074(13) Uiso 1 1 d . . . N1B N 0.7959(3) 0.2563(2) 0.19595(17) 0.0321(6) Uani 1 1 d . . . C2B C 0.8956(3) 0.3240(3) 0.1932(2) 0.0338(8) Uani 1 1 d . . . H2B H 0.9754 0.2903 0.1869 0.041 Uiso 1 1 calc R . . C3B C 0.8881(3) 0.4400(3) 0.1991(2) 0.0307(7) Uani 1 1 d . . . H3B H 0.9616 0.4845 0.1964 0.037 Uiso 1 1 calc R . . C4B C 0.7730(3) 0.4923(2) 0.20917(18) 0.0254(7) Uani 1 1 d . . . C5B C 0.6689(3) 0.4214(3) 0.21227(18) 0.0276(7) Uani 1 1 d . . . H5B H 0.5879 0.4527 0.2186 0.033 Uiso 1 1 calc R . . C6B C 0.6848(3) 0.3059(3) 0.2061(2) 0.0326(8) Uani 1 1 d . . . H6B H 0.6132 0.2589 0.2092 0.039 Uiso 1 1 calc R . . C7B C 0.7612(3) 0.6174(2) 0.21445(19) 0.0266(7) Uani 1 1 d . . . C8B C 0.8411(3) 0.6891(3) 0.1665(2) 0.0311(8) Uani 1 1 d . . . H8B H 0.9036 0.6570 0.1288 0.037 Uiso 1 1 calc R . . C9B C 0.8314(3) 0.8053(3) 0.1727(2) 0.0314(8) Uani 1 1 d . . . H9B H 0.8860 0.8525 0.1388 0.038 Uiso 1 1 calc R . . C10B C 0.7421(3) 0.8529(3) 0.22836(19) 0.0246(7) Uani 1 1 d . . . C11B C 0.6613(3) 0.7837(3) 0.27590(19) 0.0293(7) Uani 1 1 d . . . H11B H 0.5999 0.8167 0.3140 0.035 Uiso 1 1 calc R . . C12B C 0.6686(3) 0.6673(3) 0.2687(2) 0.0304(8) Uani 1 1 d . . . H12B H 0.6110 0.6208 0.3004 0.036 Uiso 1 1 calc R . . C13B C 0.7275(3) 0.9792(3) 0.2354(2) 0.0303(7) Uani 1 1 d . . . O14B O 0.6441(2) 1.02512(18) 0.27678(15) 0.0372(6) Uani 1 1 d . . . O15B O 0.8164(2) 1.03584(19) 0.19240(17) 0.0429(6) Uani 1 1 d . . . H15B H 0.801(3) 1.125(3) 0.194(2) 0.069(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1A 0.048(2) 0.0209(15) 0.0370(15) 0.0009(12) -0.0051(14) -0.0025(14) C2A 0.0357(19) 0.0277(17) 0.0282(16) -0.0009(14) -0.0038(15) -0.0023(16) C3A 0.0282(17) 0.0298(17) 0.0319(15) 0.0012(14) -0.0046(15) -0.0012(15) C4A 0.0272(17) 0.0269(17) 0.0193(13) 0.0025(13) 0.0008(14) -0.0010(14) C5A 0.0317(19) 0.0315(18) 0.0308(17) 0.0040(15) 0.0009(16) -0.0019(15) C6A 0.039(2) 0.0308(19) 0.0354(18) 0.0015(16) -0.0016(17) 0.0067(16) C7A 0.0245(17) 0.0243(16) 0.0245(14) 0.0003(13) 0.0040(14) 0.0001(13) C8A 0.0247(17) 0.0322(18) 0.0257(14) 0.0007(14) -0.0026(14) -0.0032(14) C9A 0.0259(17) 0.0315(17) 0.0286(15) 0.0068(14) 0.0005(14) 0.0020(15) C10A 0.0215(16) 0.0283(16) 0.0253(15) 0.0002(14) 0.0047(14) 0.0006(14) C11A 0.0279(19) 0.0319(17) 0.0258(15) 0.0005(14) -0.0012(15) -0.0049(15) C12A 0.0236(17) 0.0319(18) 0.0241(14) 0.0037(14) -0.0017(14) -0.0002(14) C13A 0.0286(18) 0.0280(18) 0.0293(16) 0.0039(14) 0.0030(15) 0.0006(15) O14A 0.0453(14) 0.0309(12) 0.0529(14) -0.0065(12) -0.0170(13) -0.0023(12) O15A 0.0442(14) 0.0246(13) 0.0484(13) 0.0035(11) -0.0169(11) -0.0006(11) N1B 0.0352(15) 0.0265(14) 0.0346(13) 0.0000(12) -0.0032(14) 0.0007(13) C2B 0.0317(19) 0.0345(19) 0.0352(17) 0.0009(15) -0.0028(16) -0.0019(16) C3B 0.0248(17) 0.0295(18) 0.0378(17) 0.0021(15) -0.0026(16) -0.0029(15) C4B 0.0284(18) 0.0267(16) 0.0211(15) 0.0027(13) 0.0019(14) 0.0004(14) C5B 0.0257(17) 0.0281(16) 0.0290(15) -0.0008(14) 0.0023(13) -0.0002(14) C6B 0.0269(19) 0.0345(18) 0.0364(17) 0.0039(15) 0.0005(16) -0.0054(15) C7B 0.0266(17) 0.0295(17) 0.0235(15) 0.0012(13) -0.0025(14) 0.0001(14) C8B 0.0290(19) 0.0345(18) 0.0298(16) -0.0026(14) 0.0062(15) -0.0019(15) C9B 0.030(2) 0.0242(16) 0.0395(18) 0.0009(14) 0.0057(15) -0.0024(15) C10B 0.0219(17) 0.0261(15) 0.0258(15) 0.0006(14) -0.0028(13) 0.0003(13) C11B 0.0281(18) 0.0340(18) 0.0256(15) 0.0003(14) 0.0026(14) 0.0026(15) C12B 0.0289(19) 0.0346(18) 0.0276(16) 0.0029(14) 0.0042(14) -0.0042(15) C13B 0.0332(19) 0.0291(17) 0.0287(16) -0.0019(15) -0.0068(16) 0.0009(16) O14B 0.0347(13) 0.0311(12) 0.0460(13) -0.0042(11) 0.0049(12) 0.0055(11) O15B 0.0381(15) 0.0271(12) 0.0637(15) 0.0027(12) 0.0169(13) -0.0018(11) _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 N1A C2A 1.327(4) . ? N1A C6A 1.346(4) . ? C2A C3A 1.374(4) . ? C2A H2A 0.9500 . ? C3A C4A 1.394(4) . ? C3A H3A 0.9500 . ? C4A C5A 1.398(4) . ? C4A C7A 1.483(4) . ? C5A C6A 1.381(4) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7A C8A 1.395(4) . ? C7A C12A 1.400(4) . ? C8A C9A 1.392(4) . ? C8A H8A 0.9500 . ? C9A C10A 1.389(4) . ? C9A H9A 0.9500 . ? C10A C11A 1.390(4) . ? C10A C13A 1.495(4) . ? C11A C12A 1.388(4) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A O14A 1.217(3) . ? C13A O15A 1.321(3) . ? O15A H15A 1.07(4) . ? N1B C2B 1.337(4) . ? N1B C6B 1.338(4) . ? C2B C3B 1.374(4) . ? C2B H2B 0.9500 . ? C3B C4B 1.390(4) . ? C3B H3B 0.9500 . ? C4B C5B 1.398(4) . ? C4B C7B 1.484(4) . ? C5B C6B 1.377(4) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C7B C8B 1.398(4) . ? C7B C12B 1.406(4) . ? C8B C9B 1.378(4) . ? C8B H8B 0.9500 . ? C9B C10B 1.382(4) . ? C9B H9B 0.9500 . ? C10B C11B 1.383(4) . ? C10B C13B 1.502(4) . ? C11B C12B 1.380(4) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B O14B 1.212(4) . ? C13B O15B 1.326(4) . ? O15B H15B 1.07(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 C2A N1A C6A 116.9(3) . . ? N1A C2A C3A 123.7(3) . . ? N1A C2A H2A 118.1 . . ? C3A C2A H2A 118.1 . . ? C2A C3A C4A 119.7(3) . . ? C2A C3A H3A 120.1 . . ? C4A C3A H3A 120.1 . . ? C3A C4A C5A 117.1(3) . . ? C3A C4A C7A 120.8(3) . . ? C5A C4A C7A 122.1(3) . . ? C6A C5A C4A 118.8(3) . . ? C6A C5A H5A 120.6 . . ? C4A C5A H5A 120.6 . . ? N1A C6A C5A 123.7(3) . . ? N1A C6A H6A 118.2 . . ? C5A C6A H6A 118.2 . . ? C8A C7A C12A 119.1(3) . . ? C8A C7A C4A 120.0(3) . . ? C12A C7A C4A 120.9(3) . . ? C9A C8A C7A 120.5(3) . . ? C9A C8A H8A 119.7 . . ? C7A C8A H8A 119.7 . . ? C8A C9A C10A 120.5(3) . . ? C8A C9A H9A 119.7 . . ? C10A C9A H9A 119.7 . . ? C11A C10A C9A 118.9(3) . . ? C11A C10A C13A 118.6(3) . . ? C9A C10A C13A 122.5(3) . . ? C10A C11A C12A 121.3(3) . . ? C10A C11A H11A 119.3 . . ? C12A C11A H11A 119.3 . . ? C11A C12A C7A 119.7(3) . . ? C11A C12A H12A 120.1 . . ? C7A C12A H12A 120.1 . . ? O14A C13A O15A 122.6(3) . . ? O14A C13A C10A 122.7(3) . . ? O15A C13A C10A 114.7(3) . . ? C13A O15A H15A 104(2) . . ? C2B N1B C6B 117.2(3) . . ? N1B C2B C3B 123.1(3) . . ? N1B C2B H2B 118.4 . . ? C3B C2B H2B 118.4 . . ? C2B C3B C4B 120.1(3) . . ? C2B C3B H3B 120.0 . . ? C4B C3B H3B 120.0 . . ? C3B C4B C5B 116.8(3) . . ? C3B C4B C7B 121.6(3) . . ? C5B C4B C7B 121.6(3) . . ? C6B C5B C4B 119.3(3) . . ? C6B C5B H5B 120.3 . . ? C4B C5B H5B 120.3 . . ? N1B C6B C5B 123.5(3) . . ? N1B C6B H6B 118.3 . . ? C5B C6B H6B 118.3 . . ? C8B C7B C12B 118.0(3) . . ? C8B C7B C4B 121.6(3) . . ? C12B C7B C4B 120.5(3) . . ? C9B C8B C7B 121.5(3) . . ? C9B C8B H8B 119.3 . . ? C7B C8B H8B 119.3 . . ? C8B C9B C10B 119.8(3) . . ? C8B C9B H9B 120.1 . . ? C10B C9B H9B 120.1 . . ? C11B C10B C9B 119.7(3) . . ? C11B C10B C13B 119.1(3) . . ? C9B C10B C13B 121.1(3) . . ? C12B C11B C10B 120.9(3) . . ? C12B C11B H11B 119.5 . . ? C10B C11B H11B 119.5 . . ? C11B C12B C7B 120.1(3) . . ? C11B C12B H12B 120.0 . . ? C7B C12B H12B 120.0 . . ? O14B C13B O15B 123.2(3) . . ? O14B C13B C10B 123.7(3) . . ? O15B C13B C10B 113.1(3) . . ? C13B O15B H15B 112(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6A N1A C2A C3A -0.8(5) . . . . ? N1A C2A C3A C4A 0.7(5) . . . . ? C2A C3A C4A C5A 0.6(4) . . . . ? C2A C3A C4A C7A -179.2(3) . . . . ? C3A C4A C5A C6A -1.6(4) . . . . ? C7A C4A C5A C6A 178.2(3) . . . . ? C2A N1A C6A C5A -0.3(5) . . . . ? C4A C5A C6A N1A 1.5(5) . . . . ? C3A C4A C7A C8A 39.0(4) . . . . ? C5A C4A C7A C8A -140.8(3) . . . . ? C3A C4A C7A C12A -139.5(3) . . . . ? C5A C4A C7A C12A 40.7(4) . . . . ? C12A C7A C8A C9A -0.3(4) . . . . ? C4A C7A C8A C9A -178.8(3) . . . . ? C7A C8A C9A C10A 0.6(4) . . . . ? C8A C9A C10A C11A 0.2(4) . . . . ? C8A C9A C10A C13A -178.3(3) . . . . ? C9A C10A C11A C12A -1.3(4) . . . . ? C13A C10A C11A C12A 177.3(3) . . . . ? C10A C11A C12A C7A 1.6(5) . . . . ? C8A C7A C12A C11A -0.8(4) . . . . ? C4A C7A C12A C11A 177.8(3) . . . . ? C11A C10A C13A O14A -4.0(5) . . . . ? C9A C10A C13A O14A 174.5(3) . . . . ? C11A C10A C13A O15A 176.6(3) . . . . ? C9A C10A C13A O15A -4.8(4) . . . . ? C6B N1B C2B C3B -0.9(5) . . . . ? N1B C2B C3B C4B 0.5(5) . . . . ? C2B C3B C4B C5B -0.3(4) . . . . ? C2B C3B C4B C7B -179.1(3) . . . . ? C3B C4B C5B C6B 0.5(4) . . . . ? C7B C4B C5B C6B 179.3(3) . . . . ? C2B N1B C6B C5B 1.1(5) . . . . ? C4B C5B C6B N1B -0.9(5) . . . . ? C3B C4B C7B C8B 33.4(4) . . . . ? C5B C4B C7B C8B -145.3(3) . . . . ? C3B C4B C7B C12B -146.3(3) . . . . ? C5B C4B C7B C12B 35.0(4) . . . . ? C12B C7B C8B C9B 0.9(4) . . . . ? C4B C7B C8B C9B -178.9(3) . . . . ? C7B C8B C9B C10B 0.9(5) . . . . ? C8B C9B C10B C11B -1.4(5) . . . . ? C8B C9B C10B C13B -178.9(3) . . . . ? C9B C10B C11B C12B 0.1(5) . . . . ? C13B C10B C11B C12B 177.6(3) . . . . ? C10B C11B C12B C7B 1.8(5) . . . . ? C8B C7B C12B C11B -2.2(4) . . . . ? C4B C7B C12B C11B 177.5(3) . . . . ? C11B C10B C13B O14B -4.2(5) . . . . ? C9B C10B C13B O14B 173.3(3) . . . . ? C11B C10B C13B O15B 175.1(3) . . . . ? C9B C10B C13B O15B -7.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.17 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.197 _refine_diff_density_min -0.204 _refine_diff_density_rms 0.047 data_2 _database_code_depnum_ccdc_archive 'CCDC 850072' #TrackingRef '- DT-ART-10-2011-012016 CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C106.25 H96.75 Co4 N11.25 O23.75' _chemical_formula_weight 2146.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 31.9819(12) _cell_length_b 31.9819(12) _cell_length_c 25.3323(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25910.9(18) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 47724 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 27.34 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8888 _exptl_absorpt_coefficient_mu 0.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8669 _exptl_absorpt_correction_T_max 0.8716 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type diffractometer _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47723 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0729 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.34 _reflns_number_total 21373 _reflns_number_gt 11369 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Pseudosymmetry is present in the form of a non-crystallographic inversion centre. ADDSYM was used to establish that the space group is correct. Guest atoms are refined isotropically, except for nitrogen and oxygen atoms on DMF and Ethanol. The low site occupancies of the solvent molecules prevented anisotropic refinement. Further solvent accessible voids are present, but analytical data matches the solvent model presented. Further disorder may be present. 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^)+(0.1649P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(3) _refine_ls_number_reflns 21373 _refine_ls_number_parameters 1319 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1514 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.2718 _refine_ls_wR_factor_gt 0.2142 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.158 _refine_ls_shift/su_mean 0.077 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 Co2 Co 0.98396(5) 0.24451(6) 0.41547(8) 0.0366(4) Uani 1 1 d . . . Co4 Co 1.48165(5) 0.74845(6) 0.41472(8) 0.0355(4) Uani 1 1 d . . . Co1 Co 0.74626(6) -0.01673(6) 0.16632(7) 0.0357(5) Uani 1 1 d . . . Co3 Co 1.24585(6) 0.48308(5) 0.17014(7) 0.0341(5) Uani 1 1 d . . . O14D O 0.8140(4) 0.4762(3) 0.6693(4) 0.064(3) Uani 1 1 d . . . O15F O 1.3191(4) 0.9836(4) 0.6694(4) 0.064(3) Uani 1 1 d . . . O15B O 1.0178(3) 0.1838(2) 0.4159(4) 0.0350(19) Uani 1 1 d . . . O14H O 1.5164(3) 0.6865(2) 0.4128(4) 0.042(2) Uani 1 1 d . . . O14A O 1.2326(3) 0.4414(3) 0.2306(4) 0.041(2) Uani 1 1 d . . . O14E O 1.4439(2) 0.7346(3) 0.3545(4) 0.042(2) Uani 1 1 d . . . O14B O 1.0164(3) 0.2287(4) 0.4838(4) 0.063(3) Uani 1 1 d . . . O14F O 1.2731(3) 0.9821(3) 0.6060(4) 0.035(2) Uani 1 1 d . . . O15C O 0.9452(3) 0.2310(3) 0.3543(4) 0.045(2) Uani 1 1 d . . . O15H O 1.5134(3) 0.7305(3) 0.4803(4) 0.053(3) Uani 1 1 d . . . C10D C 0.8333(4) 0.4412(4) 0.5906(5) 0.042(3) Uani 1 1 d . . . O15D O 0.7722(3) 0.4809(2) 0.6030(4) 0.0324(19) Uani 1 1 d . . . O15A O 1.2097(3) 0.4228(3) 0.1551(5) 0.050(3) Uani 1 1 d . . . C13D C 0.8022(5) 0.4682(4) 0.6228(5) 0.046(4) Uani 1 1 d . . . C13H C 1.5279(4) 0.6930(3) 0.4600(5) 0.035(3) Uani 1 1 d . . . C10C C 0.8908(5) 0.1817(4) 0.3536(6) 0.045(3) Uani 1 1 d . . . C10B C 1.0545(4) 0.1646(4) 0.4964(6) 0.043(3) Uani 1 1 d . . . C3C C 0.8155(5) 0.0503(6) 0.2853(7) 0.065(5) Uani 1 1 d . . . H3C H 0.8296 0.0428 0.3169 0.078 Uiso 1 1 calc R . . C13F C 1.3037(7) 0.9750(4) 0.6212(6) 0.061(5) Uani 1 1 d . . . N1E N 1.2723(3) 0.5327(3) 0.2112(4) 0.029(2) Uani 1 1 d . . . N1D N 0.9574(3) 0.2926(4) 0.4486(5) 0.049(3) Uani 1 1 d . . . O14C O 0.9270(3) 0.2031(3) 0.4309(4) 0.051(3) Uani 1 1 d . . . C9A C 1.1863(4) 0.3823(5) 0.2849(6) 0.045(4) Uani 1 1 d . . . H9A H 1.2052 0.3997 0.3036 0.054 Uiso 1 1 calc R . . C4F C 1.4134(4) 0.8666(4) 0.5030(6) 0.040(3) Uani 1 1 d . . . C13B C 1.0284(4) 0.1911(3) 0.4622(5) 0.033(3) Uani 1 1 d . . . N1C N 0.7759(3) 0.0307(3) 0.2081(4) 0.040(3) Uani 1 1 d . . . C4B C 1.1399(4) 0.0854(5) 0.5825(6) 0.048(4) Uani 1 1 d . . . N1F N 1.4588(3) 0.7991(4) 0.4488(5) 0.051(3) Uani 1 1 d . . . O15E O 1.4215(4) 0.7090(3) 0.4331(5) 0.066(3) Uani 1 1 d . . . C10F C 1.3372(5) 0.9471(5) 0.5908(5) 0.048(4) Uani 1 1 d . . . C11C C 0.8834(4) 0.1877(4) 0.2995(6) 0.046(3) Uani 1 1 d . . . H11C H 0.8944 0.2110 0.2809 0.055 Uiso 1 1 calc R . . C10E C 1.3872(4) 0.6872(4) 0.3537(6) 0.041(3) Uani 1 1 d . . . C10H C 1.5539(4) 0.6677(4) 0.4901(6) 0.045(3) Uani 1 1 d . . . C3E C 1.2959(5) 0.6022(6) 0.2202(6) 0.063(5) Uani 1 1 d . . . H3E H 1.2971 0.6294 0.2054 0.076 Uiso 1 1 calc R . . C10A C 1.1853(4) 0.3857(4) 0.2306(5) 0.040(3) Uani 1 1 d . . . C2E C 1.2784(5) 0.5712(5) 0.1936(6) 0.062(5) Uani 1 1 d . . . H2E H 1.2693 0.5771 0.1586 0.075 Uiso 1 1 calc R . . C4A C 1.0978(4) 0.3108(4) 0.3153(6) 0.043(3) Uani 1 1 d . . . C8E C 1.3559(4) 0.6598(4) 0.2720(6) 0.042(3) Uani 1 1 d . . . H8E H 1.3540 0.6607 0.2346 0.050 Uiso 1 1 calc R . . C13A C 1.2107(4) 0.4198(4) 0.2033(7) 0.042(3) Uani 1 1 d . . . C7E C 1.3341(4) 0.6296(4) 0.2983(6) 0.045(4) Uani 1 1 d . . . C6F C 1.4591(5) 0.8033(4) 0.5025(5) 0.046(4) Uani 1 1 d . . . H6F H 1.4745 0.7832 0.5221 0.056 Uiso 1 1 calc R . . C5A C 1.0558(4) 0.3058(4) 0.2933(5) 0.040(3) Uani 1 1 d . . . H5A H 1.0494 0.3164 0.2592 0.048 Uiso 1 1 calc R . . C9E C 1.3813(4) 0.6900(4) 0.2979(6) 0.038(3) Uani 1 1 d . . . H9E H 1.3943 0.7118 0.2783 0.046 Uiso 1 1 calc R . . C4H C 1.6430(5) 0.5925(5) 0.5772(6) 0.053(4) Uani 1 1 d . . . C4E C 1.3126(5) 0.5948(5) 0.2699(5) 0.044(3) Uani 1 1 d . . . C5C C 0.7973(5) 0.0991(6) 0.2217(7) 0.063(4) Uani 1 1 d . . . H5C H 0.7969 0.1272 0.2095 0.076 Uiso 1 1 calc R . . C3G C 1.5490(5) 0.8151(5) 0.2947(6) 0.050(4) Uani 1 1 d . . . H3G H 1.5408 0.8277 0.2624 0.060 Uiso 1 1 calc R . . C5F C 1.4385(4) 0.8351(4) 0.5313(6) 0.037(3) Uani 1 1 d . . . H5F H 1.4408 0.8361 0.5687 0.045 Uiso 1 1 calc R . . C12C C 0.8583(5) 0.1564(4) 0.2737(6) 0.049(4) Uani 1 1 d . . . H12C H 0.8549 0.1575 0.2365 0.058 Uiso 1 1 calc R . . C7G C 1.6232(4) 0.8422(4) 0.2844(5) 0.037(3) Uani 1 1 d . . . C11D C 0.8197(5) 0.4288(6) 0.5413(6) 0.068(6) Uani 1 1 d . . . H11D H 0.7944 0.4393 0.5267 0.082 Uiso 1 1 calc R . . C13C C 0.9209(5) 0.2061(5) 0.3814(6) 0.047(4) Uani 1 1 d . . . C6G C 1.5674(3) 0.7758(3) 0.3860(5) 0.030(3) Uani 1 1 d . . . H6G H 1.5737 0.7596 0.4163 0.036 Uiso 1 1 calc R . . C3A C 1.1039(3) 0.2947(4) 0.3649(5) 0.033(3) Uani 1 1 d . . . H3A H 1.1307 0.2968 0.3808 0.040 Uiso 1 1 calc R . . C4D C 0.9073(4) 0.3553(5) 0.5025(6) 0.056(4) Uani 1 1 d . . . C7H C 1.6102(5) 0.6186(5) 0.5466(6) 0.057(4) Uani 1 1 d . . . C5B C 1.1649(7) 0.0627(5) 0.5571(7) 0.072(6) Uani 1 1 d . . . H5B H 1.1612 0.0585 0.5203 0.086 Uiso 1 1 calc R . . C7B C 1.1053(7) 0.1114(6) 0.5527(6) 0.075(5) Uani 1 1 d . . . C7C C 0.8389(5) 0.1249(5) 0.3018(7) 0.058(4) Uani 1 1 d . . . C8A C 1.1626(4) 0.3562(4) 0.3127(6) 0.041(3) Uani 1 1 d . . . H8A H 1.1674 0.3516 0.3492 0.049 Uiso 1 1 calc R . . C2D C 0.9627(5) 0.3030(5) 0.5021(6) 0.062(5) Uani 1 1 d . . . H2D H 0.9841 0.2890 0.5211 0.075 Uiso 1 1 calc R . . C9D C 0.8691(4) 0.4237(4) 0.6124(6) 0.054(4) Uani 1 1 d . . . H9D H 0.8761 0.4307 0.6478 0.065 Uiso 1 1 calc R . . C12G C 1.6588(4) 0.8573(4) 0.3075(6) 0.041(3) Uani 1 1 d . . . H12G H 1.6662 0.8490 0.3422 0.049 Uiso 1 1 calc R . . C11G C 1.6830(4) 0.8838(5) 0.2808(5) 0.049(4) Uani 1 1 d . . . H11G H 1.7043 0.8984 0.2993 0.059 Uiso 1 1 calc R . . C11H C 1.5726(7) 0.6791(6) 0.5389(9) 0.093(8) Uani 1 1 d . . . H11H H 1.5655 0.7060 0.5520 0.112 Uiso 1 1 calc R . . C2F C 1.4378(4) 0.8305(4) 0.4241(5) 0.046(3) Uani 1 1 d . . . H2F H 1.4363 0.8289 0.3867 0.055 Uiso 1 1 calc R . . C13E C 1.4157(4) 0.7120(4) 0.3826(5) 0.031(3) Uani 1 1 d . . . C8B C 1.0929(5) 0.1504(5) 0.5735(6) 0.059(4) Uani 1 1 d . . . H8B H 1.1033 0.1600 0.6064 0.071 Uiso 1 1 calc R . . C9G C 1.6456(4) 0.8736(4) 0.2010(5) 0.035(3) Uani 1 1 d . . . H9G H 1.6407 0.8803 0.1651 0.043 Uiso 1 1 calc R . . N1G N 1.5259(4) 0.7783(3) 0.3701(5) 0.049(3) Uani 1 1 d . . . C2C C 0.7952(4) 0.0183(5) 0.2548(6) 0.049(4) Uani 1 1 d . . . H2C H 0.7950 -0.0100 0.2661 0.059 Uiso 1 1 calc R . . C6E C 1.2912(5) 0.5236(6) 0.2592(6) 0.063(5) Uani 1 1 d . . . H6E H 1.2906 0.4957 0.2723 0.076 Uiso 1 1 calc R . . C6C C 0.7811(5) 0.0698(5) 0.1921(6) 0.051(4) Uani 1 1 d . . . H6C H 0.7726 0.0769 0.1573 0.061 Uiso 1 1 calc R . . C7A C 1.1303(5) 0.3362(5) 0.2860(6) 0.056(4) Uani 1 1 d . . . C5G C 1.6010(4) 0.7961(4) 0.3596(5) 0.036(3) Uani 1 1 d . . . H5G H 1.6286 0.7952 0.3734 0.043 Uiso 1 1 calc R . . C2A C 1.0706(3) 0.2747(4) 0.3932(5) 0.035(3) Uani 1 1 d . . . H2A H 1.0761 0.2618 0.4262 0.042 Uiso 1 1 calc R . . C4G C 1.5924(4) 0.8177(5) 0.3125(8) 0.054(4) Uani 1 1 d . . . C8G C 1.6210(5) 0.8476(5) 0.2262(6) 0.057(4) Uani 1 1 d . . . H8G H 1.6013 0.8317 0.2066 0.069 Uiso 1 1 calc R . . C7F C 1.3884(4) 0.8962(4) 0.5308(6) 0.042(3) Uani 1 1 d . . . C11E C 1.3639(4) 0.6582(4) 0.3814(5) 0.050(4) Uani 1 1 d . . . H11E H 1.3637 0.6582 0.4189 0.060 Uiso 1 1 calc R . . C9C C 0.8699(5) 0.1513(5) 0.3805(6) 0.060(4) Uani 1 1 d . . . H9C H 0.8715 0.1503 0.4180 0.073 Uiso 1 1 calc R . . C8D C 0.8958(5) 0.3961(6) 0.5847(6) 0.066(5) Uani 1 1 d . . . H8D H 0.9204 0.3847 0.5999 0.080 Uiso 1 1 calc R . . C9H C 1.5648(5) 0.6278(4) 0.4730(6) 0.053(4) Uani 1 1 d . . . H9H H 1.5521 0.6158 0.4426 0.064 Uiso 1 1 calc R . . C11A C 1.1567(4) 0.3609(5) 0.2039(6) 0.052(4) Uani 1 1 d . . . H11A H 1.1559 0.3623 0.1664 0.063 Uiso 1 1 calc R . . C12E C 1.3391(5) 0.6270(5) 0.3514(6) 0.071(6) Uani 1 1 d . . . H12E H 1.3264 0.6046 0.3699 0.086 Uiso 1 1 calc R . . C3B C 1.1425(5) 0.0874(4) 0.6368(6) 0.052(4) Uani 1 1 d . . . H3B H 1.1230 0.1040 0.6557 0.062 Uiso 1 1 calc R . . C9F C 1.3204(6) 0.9311(5) 0.5442(6) 0.068(6) Uani 1 1 d . . . H9F H 1.2924 0.9361 0.5331 0.081 Uiso 1 1 calc R . . C12B C 1.0925(4) 0.1004(5) 0.5051(6) 0.052(4) Uani 1 1 d . . . H12B H 1.1028 0.0751 0.4904 0.063 Uiso 1 1 calc R . . C8C C 0.8452(5) 0.1205(5) 0.3524(6) 0.058(5) Uani 1 1 d . . . H8C H 0.8338 0.0972 0.3706 0.070 Uiso 1 1 calc R . . N1A N 1.0296(4) 0.2741(3) 0.3722(4) 0.048(3) Uani 1 1 d . . . C8H C 1.5948(5) 0.6060(4) 0.5015(6) 0.054(4) Uani 1 1 d . . . H8H H 1.6048 0.5804 0.4873 0.064 Uiso 1 1 calc R . . C12D C 0.8458(5) 0.3989(7) 0.5127(6) 0.085(7) Uani 1 1 d . . . H12D H 0.8364 0.3880 0.4799 0.102 Uiso 1 1 calc R . . C4C C 0.8150(4) 0.0905(5) 0.2702(5) 0.040(3) Uani 1 1 d . . . C3F C 1.4182(5) 0.8650(5) 0.4475(6) 0.060(4) Uani 1 1 d . . . H3F H 1.4082 0.8872 0.4261 0.073 Uiso 1 1 calc R . . C2G C 1.5214(4) 0.7949(5) 0.3240(6) 0.047(4) Uani 1 1 d . . . H2G H 1.4943 0.7923 0.3090 0.057 Uiso 1 1 calc R . . C11B C 1.0644(4) 0.1244(4) 0.4752(6) 0.043(3) Uani 1 1 d . . . H11B H 1.0527 0.1145 0.4431 0.052 Uiso 1 1 calc R . . C12H C 1.5990(6) 0.6565(5) 0.5690(8) 0.089(8) Uani 1 1 d . . . H12H H 1.6090 0.6657 0.6023 0.107 Uiso 1 1 calc R . . C2H C 1.6957(5) 0.5430(5) 0.5812(7) 0.059(4) Uani 1 1 d . . . H2H H 1.7128 0.5234 0.5631 0.071 Uiso 1 1 calc R . . H6H H 1.6824 0.5770 0.6962 0.071 Uiso 1 1 d R . . N1H N 1.7012(3) 0.5472(3) 0.6314(4) 0.032(2) Uani 1 1 d . . . C8F C 1.3498(4) 0.9062(5) 0.5146(6) 0.056(4) Uani 1 1 d . . . H8F H 1.3411 0.8960 0.4810 0.067 Uiso 1 1 calc R . . C6D C 0.9234(8) 0.3164(7) 0.4284(6) 0.146(13) Uani 1 1 d . . . H6D H 0.9179 0.3133 0.3917 0.175 Uiso 1 1 calc R . . C3H C 1.6665(7) 0.5651(7) 0.5519(8) 0.089(7) Uani 1 1 d . . . H3H H 1.6636 0.5608 0.5149 0.107 Uiso 1 1 calc R . . C5H C 1.6491(6) 0.5978(6) 0.6296(7) 0.094(7) Uani 1 1 d . . . H5H H 1.6326 0.6176 0.6482 0.112 Uiso 1 1 calc R . . C5D C 0.8973(7) 0.3435(7) 0.4551(8) 0.128(11) Uani 1 1 d . . . H5D H 0.8724 0.3534 0.4391 0.153 Uiso 1 1 calc R . . N1B N 1.2002(3) 0.0450(3) 0.6359(4) 0.032(2) Uani 1 1 d . . . C6B C 1.1993(5) 0.0430(4) 0.5845(7) 0.057(4) Uani 1 1 d . . . H6B H 1.2207 0.0289 0.5655 0.068 Uiso 1 1 calc R . . C2B C 1.1718(5) 0.0663(5) 0.6635(7) 0.059(4) Uani 1 1 d . . . H2B H 1.1724 0.0666 0.7009 0.070 Uiso 1 1 calc R . . C11F C 1.3778(7) 0.9364(6) 0.6060(7) 0.080(6) Uani 1 1 d . . . H11F H 1.3882 0.9469 0.6385 0.096 Uiso 1 1 calc R . . CM5 C 1.2527(6) 0.1378(5) 0.5422(7) 0.107(6) Uiso 1 1 d D . . HM5A H 1.2664 0.1235 0.5718 0.161 Uiso 1 1 calc R . . HM5B H 1.2734 0.1547 0.5231 0.161 Uiso 1 1 calc R . . HM5C H 1.2406 0.1170 0.5183 0.161 Uiso 1 1 calc R . . CK5 C 1.3635(5) 0.7517(6) 0.5492(7) 0.105(6) Uiso 1 1 d D . . HK5A H 1.3694 0.7297 0.5233 0.157 Uiso 1 1 calc R . . HK5B H 1.3499 0.7395 0.5802 0.157 Uiso 1 1 calc R . . HK5C H 1.3897 0.7651 0.5599 0.157 Uiso 1 1 calc R . . NK3 N 1.3361(4) 0.7826(3) 0.5256(4) 0.079(4) Uani 1 1 d D . . OL1 O 1.6937(5) 0.8111(6) 0.4205(8) 0.108(9) Uani 0.50 1 d PDU . . NM3 N 1.2199(4) 0.1649(4) 0.5623(4) 0.100(6) Uani 1 1 d D . . CK2 C 1.3379(4) 0.7904(5) 0.4744(4) 0.088(5) Uiso 1 1 d D . . HK2 H 1.3568 0.7745 0.4536 0.105 Uiso 1 1 calc R . . CM2 C 1.2139(5) 0.1685(5) 0.6136(4) 0.104(6) Uiso 1 1 d D . . HM2 H 1.2326 0.1539 0.6362 0.125 Uiso 1 1 calc R . . CM4 C 1.1937(6) 0.1872(7) 0.5252(6) 0.141(9) Uiso 1 1 d D . . HM4A H 1.1907 0.2163 0.5367 0.211 Uiso 1 1 calc R . . HM4B H 1.1661 0.1739 0.5236 0.211 Uiso 1 1 calc R . . HM4C H 1.2067 0.1865 0.4901 0.211 Uiso 1 1 calc R . . CK4 C 1.3127(6) 0.8097(5) 0.5605(5) 0.109(7) Uiso 1 1 d D . . HK4A H 1.3018 0.8335 0.5404 0.164 Uiso 1 1 calc R . . HK4B H 1.3310 0.8199 0.5886 0.164 Uiso 1 1 calc R . . HK4C H 1.2894 0.7940 0.5760 0.164 Uiso 1 1 calc R . . C7D C 0.8828(5) 0.3868(4) 0.5320(6) 0.044(3) Uani 1 1 d . . . C9B C 1.0653(6) 0.1738(6) 0.5449(6) 0.069(5) Uani 1 1 d . . . H9B H 1.0535 0.1979 0.5609 0.083 Uiso 1 1 calc R . . CL2 C 1.7283(6) 0.8074(5) 0.4003(10) 0.055(7) Uiso 0.50 1 d PDU . . HL2 H 1.7448 0.8319 0.3967 0.066 Uiso 0.50 1 calc PR . . C5E C 1.3113(6) 0.5554(5) 0.2890(6) 0.060(5) Uani 1 1 d . . . H5E H 1.3237 0.5490 0.3221 0.072 Uiso 1 1 calc R . . OM1 O 1.1861(4) 0.1893(4) 0.6346(5) 0.125(6) Uani 1 1 d D . . C12A C 1.1302(5) 0.3352(5) 0.2285(6) 0.057(4) Uani 1 1 d . . . H12A H 1.1121 0.3171 0.2094 0.069 Uiso 1 1 calc R . . C12F C 1.4015(5) 0.9130(7) 0.5781(7) 0.085(6) Uani 1 1 d . . . H12F H 1.4290 0.9070 0.5903 0.102 Uiso 1 1 calc R . . C6A C 1.0268(4) 0.2865(4) 0.3214(6) 0.038(3) Uani 1 1 d . . . H6A H 1.0012 0.2807 0.3040 0.046 Uiso 1 1 calc R . . CL4 C 1.7195(9) 0.7339(5) 0.3839(16) 0.094(12) Uiso 0.50 1 d PDU . . HL4A H 1.7100 0.7284 0.4200 0.141 Uiso 0.50 1 calc PR . . HL4B H 1.7365 0.7104 0.3715 0.141 Uiso 0.50 1 calc PR . . HL4C H 1.6952 0.7374 0.3607 0.141 Uiso 0.50 1 calc PR . . C3D C 0.9392(4) 0.3318(4) 0.5287(6) 0.049(4) Uani 1 1 d . . . H3D H 0.9441 0.3363 0.5652 0.059 Uiso 1 1 calc R . . C10G C 1.6782(4) 0.8907(4) 0.2274(6) 0.044(3) Uani 1 1 d . . . CL5 C 1.7881(5) 0.7690(7) 0.3699(10) 0.052(6) Uiso 0.50 1 d PDU . . HL5A H 1.8020 0.7954 0.3788 0.077 Uiso 0.50 1 calc PR . . HL5B H 1.7911 0.7636 0.3320 0.077 Uiso 0.50 1 calc PR . . HL5C H 1.8011 0.7462 0.3899 0.077 Uiso 0.50 1 calc PR . . OK1 O 1.3164(4) 0.8171(3) 0.4520(4) 0.097(4) Uani 1 1 d D . . C13G C 1.7088(5) 0.9237(4) 0.2006(7) 0.045(4) Uani 1 1 d . . . O15G O 1.7329(3) 0.9422(3) 0.2264(4) 0.038(2) Uani 1 1 d . . . O14G O 1.7062(3) 0.9287(3) 0.1526(4) 0.045(2) Uani 1 1 d . . . ON1 O 0.9716(11) 0.3776(11) 0.2817(15) 0.059(10) Uiso 0.25 1 d P A 2 O5W O 0.9733(13) 0.0996(13) 0.3897(17) 0.067(11) Uiso 0.25 1 d P . . CN3 C 0.9821(15) 0.4069(14) 0.2003(17) 0.040(10) Uiso 0.25 1 d P A 2 HN3A H 1.0117 0.3996 0.1970 0.060 Uiso 0.25 1 calc PR A 2 HN3B H 0.9762 0.4320 0.1794 0.060 Uiso 0.25 1 calc PR A 2 HN3C H 0.9649 0.3837 0.1874 0.060 Uiso 0.25 1 calc PR A 2 CN2 C 0.9733(12) 0.4141(12) 0.2495(15) 0.030(8) Uiso 0.25 1 d P A 2 HN2A H 0.9459 0.4285 0.2514 0.036 Uiso 0.25 1 calc PR A 2 HN2B H 0.9946 0.4333 0.2642 0.036 Uiso 0.25 1 calc PR A 2 O6W O 0.9671(7) 0.1157(8) 0.2703(10) 0.089(7) Uiso 0.50 1 d P . . O12W O 1.0368(10) 0.4823(10) 0.1463(14) 0.056(9) Uiso 0.25 1 d P . . O7W O 1.5677(9) 0.5020(10) 0.5654(12) 0.046(7) Uiso 0.25 1 d P . . O8W O 1.5505(16) 0.9745(16) 0.540(2) 0.108(16) Uiso 0.25 1 d P . . O11W O 1.0539(15) 0.4141(14) 0.3487(19) 0.089(13) Uiso 0.25 1 d P B 2 O9W O 0.9671(9) 0.3894(9) 0.7040(11) 0.031(7) Uiso 0.25 1 d P . . O15W O 1.6690(9) 0.7483(13) 0.5381(16) 0.056(7) Uiso 0.25 1 d P . . NJ3 N 0.7689(4) 0.2487(4) 0.2043(7) 0.085(5) Uani 0.75 1 d PDU . . CJ2 C 0.8045(4) 0.2313(6) 0.1886(10) 0.098(8) Uiso 0.75 1 d PDU . . HJ2 H 0.8296 0.2464 0.1947 0.118 Uiso 0.75 1 calc PR . . OJ1 O 0.8072(5) 0.1972(5) 0.1668(6) 0.094(5) Uani 0.75 1 d PDU . . CJ4 C 0.7695(7) 0.2893(6) 0.2296(12) 0.125(11) Uiso 0.75 1 d PDU . . HJ4A H 0.7986 0.2979 0.2355 0.188 Uiso 0.75 1 calc PR . . HJ4B H 0.7549 0.2877 0.2635 0.188 Uiso 0.75 1 calc PR . . HJ4C H 0.7555 0.3098 0.2069 0.188 Uiso 0.75 1 calc PR . . CJ5 C 0.7299(4) 0.2265(8) 0.1965(14) 0.162(14) Uiso 0.75 1 d PDU . . HJ5A H 0.7259 0.2209 0.1588 0.242 Uiso 0.75 1 calc PR . . HJ5B H 0.7067 0.2436 0.2096 0.242 Uiso 0.75 1 calc PR . . HJ5C H 0.7307 0.2000 0.2158 0.242 Uiso 0.75 1 calc PR . . NL3 N 1.7443(5) 0.7717(5) 0.3832(10) 0.101(9) Uani 0.50 1 d PDU . . O2W O 0.8843(7) -0.0327(6) 0.7725(9) 0.072(6) Uiso 0.50 1 d P . . C6H C 1.6789(7) 0.5747(6) 0.6567(7) 0.092(7) Uani 1 1 d . . . O3W O 1.0000(14) 0.0609(13) 0.5578(17) 0.079(12) Uiso 0.25 1 d P . . O4W O 1.040(2) 0.0734(19) 0.319(3) 0.13(2) Uiso 0.25 1 d P . . O10W O 1.015(3) 0.364(3) 0.400(4) 0.20(4) Uiso 0.25 1 d P C 1 O1W O 0.8914(13) -0.0363(13) 0.8851(17) 0.066(11) Uiso 0.25 1 d P . . O14W O 0.9107(15) 0.4732(15) 0.429(2) 0.104(16) Uiso 0.25 1 d P . . O13W O 0.9339(18) 0.450(2) 0.283(2) 0.13(2) Uiso 0.25 1 d P D 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co2 0.0308(8) 0.0467(10) 0.0322(9) -0.0010(10) 0.0153(7) -0.0036(7) Co4 0.0302(8) 0.0455(10) 0.0308(9) 0.0007(9) 0.0152(7) -0.0018(7) Co1 0.0380(10) 0.0355(10) 0.0336(11) 0.0171(6) 0.0022(8) 0.0014(8) Co3 0.0368(10) 0.0332(10) 0.0324(12) 0.0147(6) -0.0013(8) 0.0011(8) O14D 0.089(8) 0.060(6) 0.045(6) -0.026(5) 0.012(5) 0.023(6) O15F 0.073(8) 0.085(8) 0.035(6) -0.028(5) -0.003(5) 0.033(6) O15B 0.050(5) 0.022(4) 0.033(5) -0.009(4) 0.012(4) -0.002(3) O14H 0.044(5) 0.030(4) 0.052(6) -0.004(4) 0.016(5) 0.012(4) O14A 0.038(5) 0.036(5) 0.050(6) 0.014(4) -0.004(4) -0.015(4) O14E 0.027(4) 0.053(6) 0.046(6) 0.000(5) 0.012(4) -0.008(4) O14B 0.063(7) 0.094(8) 0.031(5) 0.003(5) 0.009(4) 0.024(6) O14F 0.031(5) 0.039(5) 0.035(5) 0.001(4) -0.009(4) 0.019(4) O15C 0.034(5) 0.066(6) 0.034(5) 0.011(5) 0.008(4) -0.016(4) O15H 0.057(6) 0.065(6) 0.037(5) -0.008(5) -0.003(4) 0.043(5) C10D 0.054(8) 0.048(8) 0.026(6) -0.005(6) 0.015(6) 0.009(6) O15D 0.026(4) 0.026(4) 0.045(5) 0.004(3) 0.004(4) 0.012(3) O15A 0.047(6) 0.062(6) 0.040(6) 0.004(5) 0.006(5) -0.017(5) C13D 0.055(9) 0.050(8) 0.032(7) -0.018(6) 0.020(6) 0.000(7) C13H 0.041(7) 0.021(5) 0.043(7) -0.004(5) 0.036(6) 0.005(5) C10C 0.057(9) 0.034(7) 0.043(8) -0.010(6) 0.009(7) -0.014(6) C10B 0.039(7) 0.026(6) 0.065(10) -0.011(6) 0.009(6) -0.003(5) C3C 0.056(10) 0.081(13) 0.059(10) 0.019(9) 0.017(8) -0.026(8) C13F 0.116(15) 0.037(8) 0.030(7) -0.014(6) 0.021(9) 0.012(9) N1E 0.045(6) 0.014(4) 0.029(5) -0.004(4) -0.020(4) -0.002(4) N1D 0.034(6) 0.063(8) 0.051(7) -0.011(6) -0.004(5) 0.023(5) O14C 0.068(7) 0.051(6) 0.035(6) 0.015(5) -0.007(5) -0.016(5) C9A 0.037(7) 0.065(10) 0.034(7) -0.002(6) 0.006(6) -0.021(7) C4F 0.033(6) 0.043(7) 0.045(7) -0.010(6) -0.006(6) 0.014(5) C13B 0.028(6) 0.017(5) 0.055(8) -0.007(5) 0.023(6) -0.005(4) N1C 0.061(7) 0.014(4) 0.044(6) -0.001(4) -0.024(5) -0.011(5) C4B 0.040(7) 0.074(10) 0.031(7) -0.002(7) -0.002(6) 0.016(7) N1F 0.035(6) 0.084(9) 0.033(6) 0.006(6) -0.003(5) 0.022(6) O15E 0.081(8) 0.057(7) 0.062(8) 0.005(6) 0.006(6) -0.020(6) C10F 0.050(8) 0.070(10) 0.023(6) -0.009(6) 0.009(6) 0.026(7) C11C 0.046(8) 0.052(8) 0.041(8) -0.004(7) -0.004(6) 0.013(6) C10E 0.052(8) 0.029(6) 0.042(8) 0.000(5) 0.015(6) -0.015(6) C10H 0.033(7) 0.050(8) 0.051(9) -0.015(7) 0.012(6) 0.016(6) C3E 0.078(11) 0.074(11) 0.038(8) -0.009(8) -0.023(8) -0.002(9) C10A 0.058(9) 0.028(6) 0.033(7) 0.006(5) 0.005(6) -0.005(6) C2E 0.044(8) 0.100(13) 0.043(8) 0.043(8) -0.004(6) -0.025(8) C4A 0.043(7) 0.041(7) 0.045(8) -0.013(6) -0.002(6) -0.006(6) C8E 0.058(9) 0.033(7) 0.034(7) 0.001(6) 0.007(6) 0.009(6) C13A 0.038(7) 0.027(6) 0.059(10) -0.001(6) -0.008(7) 0.010(6) C7E 0.027(6) 0.045(8) 0.062(9) -0.021(7) 0.016(6) -0.008(5) C6F 0.070(10) 0.039(7) 0.030(7) 0.000(6) -0.002(6) 0.021(7) C5A 0.051(8) 0.044(7) 0.025(6) -0.006(6) 0.003(6) -0.027(6) C9E 0.042(7) 0.025(6) 0.047(8) 0.014(5) 0.011(6) 0.010(5) C4H 0.053(9) 0.065(10) 0.041(8) -0.010(7) 0.009(7) 0.024(7) C4E 0.052(8) 0.054(9) 0.026(6) -0.007(6) -0.003(6) -0.017(7) C5C 0.058(10) 0.082(11) 0.050(10) 0.008(8) -0.015(8) 0.010(8) C3G 0.056(9) 0.063(10) 0.030(7) 0.012(7) -0.015(6) -0.014(7) C5F 0.033(6) 0.043(7) 0.036(7) 0.007(6) -0.004(6) 0.005(5) C12C 0.064(10) 0.045(8) 0.037(7) 0.002(6) 0.010(7) -0.002(7) C7G 0.042(7) 0.037(7) 0.031(7) 0.018(5) -0.006(5) -0.006(5) C11D 0.069(11) 0.086(13) 0.050(10) -0.023(8) -0.043(8) 0.037(10) C13C 0.062(9) 0.048(8) 0.030(7) 0.010(6) 0.006(7) -0.013(7) C6G 0.016(5) 0.026(6) 0.048(7) 0.001(5) 0.007(5) 0.005(4) C3A 0.011(5) 0.045(7) 0.043(7) 0.002(6) 0.004(5) -0.015(5) C4D 0.030(7) 0.093(12) 0.046(9) -0.023(8) -0.010(6) 0.035(7) C7H 0.067(10) 0.057(9) 0.046(9) -0.018(7) 0.023(8) 0.013(8) C5B 0.120(16) 0.063(11) 0.033(8) -0.014(8) -0.019(9) 0.030(10) C7B 0.116(16) 0.077(13) 0.033(8) 0.000(8) -0.009(9) 0.020(11) C7C 0.072(10) 0.046(8) 0.058(10) -0.017(7) 0.045(8) -0.023(7) C8A 0.045(8) 0.038(7) 0.040(8) 0.021(6) -0.006(6) -0.016(6) C2D 0.082(11) 0.055(9) 0.050(9) -0.025(7) -0.038(8) 0.030(8) C9D 0.057(9) 0.057(9) 0.049(8) -0.010(7) -0.018(7) 0.000(7) C12G 0.047(8) 0.042(7) 0.034(7) 0.014(6) 0.009(6) -0.016(6) C11G 0.054(8) 0.063(9) 0.029(7) 0.003(6) -0.012(6) -0.043(7) C11H 0.130(19) 0.069(13) 0.082(15) 0.012(11) -0.028(13) 0.042(13) C2F 0.068(9) 0.044(7) 0.026(6) -0.018(5) 0.003(6) 0.006(6) C13E 0.040(7) 0.021(6) 0.032(6) 0.002(5) 0.015(5) -0.008(5) C8B 0.065(10) 0.072(11) 0.040(8) -0.031(8) -0.013(7) 0.026(8) C9G 0.032(6) 0.049(7) 0.024(6) 0.010(5) -0.001(5) -0.010(5) N1G 0.067(8) 0.036(6) 0.042(7) -0.006(5) -0.008(5) 0.013(5) C2C 0.056(8) 0.051(8) 0.041(7) 0.003(6) 0.004(6) 0.003(7) C6E 0.070(10) 0.093(12) 0.027(7) 0.031(7) 0.009(7) 0.016(9) C6C 0.051(8) 0.062(9) 0.040(8) 0.020(7) -0.012(6) -0.019(7) C7A 0.058(9) 0.075(10) 0.035(8) 0.032(7) -0.016(6) -0.037(8) C5G 0.026(6) 0.039(7) 0.043(8) 0.001(6) -0.001(5) -0.016(5) C2A 0.021(5) 0.051(7) 0.033(6) 0.001(5) 0.016(4) 0.003(5) C4G 0.038(8) 0.042(8) 0.082(12) -0.012(8) 0.008(8) -0.014(6) C8G 0.065(10) 0.080(11) 0.027(7) -0.012(7) -0.014(6) -0.010(8) C7F 0.049(8) 0.045(7) 0.032(7) -0.010(6) 0.004(6) 0.015(6) C11E 0.069(9) 0.052(8) 0.030(6) -0.001(6) 0.014(6) -0.029(7) C9C 0.067(10) 0.067(10) 0.047(8) -0.018(7) 0.023(7) -0.036(8) C8D 0.050(9) 0.101(13) 0.048(9) -0.031(9) -0.002(7) 0.009(8) C9H 0.066(9) 0.041(7) 0.053(9) -0.020(6) -0.027(7) 0.033(7) C11A 0.060(9) 0.063(10) 0.034(8) 0.007(6) -0.012(6) -0.022(8) C12E 0.083(11) 0.080(11) 0.052(10) -0.016(8) 0.009(8) -0.075(9) C3B 0.080(10) 0.041(7) 0.033(7) -0.007(6) -0.009(6) 0.022(7) C9F 0.094(13) 0.058(10) 0.051(10) -0.032(8) -0.044(9) 0.030(9) C12B 0.051(8) 0.063(9) 0.043(8) -0.014(7) -0.013(6) 0.034(7) C8C 0.067(9) 0.064(9) 0.043(8) -0.011(7) 0.005(7) -0.061(8) N1A 0.076(8) 0.037(6) 0.033(6) -0.026(5) -0.008(5) -0.001(5) C8H 0.080(10) 0.037(7) 0.044(7) -0.013(6) -0.011(7) 0.042(7) C12D 0.045(9) 0.171(19) 0.039(9) -0.036(10) -0.016(7) 0.054(11) C4C 0.035(7) 0.052(8) 0.032(6) -0.003(6) 0.003(6) -0.017(6) C3F 0.084(11) 0.047(8) 0.051(9) 0.012(7) -0.010(8) 0.009(7) C2G 0.016(5) 0.081(10) 0.046(8) 0.011(7) 0.007(5) -0.018(6) C11B 0.046(7) 0.031(6) 0.052(8) -0.007(6) -0.007(6) 0.021(6) C12H 0.091(13) 0.075(12) 0.102(15) -0.059(11) -0.062(12) 0.054(10) C2H 0.078(11) 0.044(8) 0.057(10) -0.010(7) -0.019(8) 0.026(8) N1H 0.029(5) 0.029(5) 0.039(6) 0.001(4) -0.006(4) 0.010(4) C8F 0.044(8) 0.085(12) 0.039(8) -0.015(7) 0.003(6) 0.030(8) C6D 0.25(3) 0.148(19) 0.038(10) -0.048(11) -0.059(13) 0.18(2) C3H 0.098(15) 0.120(17) 0.048(10) -0.019(10) -0.031(10) 0.057(13) C5H 0.090(13) 0.125(17) 0.066(11) -0.043(11) -0.025(10) 0.077(12) C5D 0.15(2) 0.17(2) 0.065(13) -0.053(14) -0.061(14) 0.105(18) N1B 0.029(5) 0.030(5) 0.037(6) 0.007(4) -0.001(4) 0.008(4) C6B 0.087(12) 0.024(6) 0.059(10) 0.004(6) 0.026(9) 0.004(7) C2B 0.077(11) 0.048(8) 0.051(9) 0.001(7) 0.016(8) 0.012(8) C11F 0.122(16) 0.080(12) 0.038(9) -0.019(9) -0.013(10) 0.019(11) NK3 0.089(10) 0.084(9) 0.065(9) 0.017(7) -0.006(8) -0.004(8) OL1 0.071(14) 0.099(16) 0.15(2) 0.096(16) -0.076(14) -0.031(11) NM3 0.179(17) 0.047(8) 0.075(10) 0.007(7) 0.026(11) 0.012(9) C7D 0.054(8) 0.038(7) 0.042(8) -0.013(6) 0.012(7) 0.021(6) C9B 0.103(15) 0.076(11) 0.027(8) 0.009(7) -0.005(8) 0.035(10) C5E 0.097(13) 0.047(9) 0.035(8) 0.012(7) -0.008(8) -0.035(8) OM1 0.093(10) 0.112(11) 0.172(15) -0.008(11) 0.060(10) 0.026(8) C12A 0.070(10) 0.062(10) 0.040(8) -0.003(7) -0.008(7) -0.008(8) C12F 0.051(10) 0.143(18) 0.061(11) -0.039(11) -0.003(8) -0.016(10) C6A 0.025(6) 0.043(7) 0.047(8) -0.008(6) 0.000(5) -0.010(5) C3D 0.042(7) 0.050(8) 0.056(9) -0.018(7) -0.022(7) 0.035(6) C10G 0.053(8) 0.045(8) 0.035(7) 0.010(6) -0.008(6) -0.017(6) OK1 0.152(11) 0.077(8) 0.063(7) 0.017(6) -0.025(8) -0.012(7) C13G 0.048(8) 0.039(7) 0.049(9) 0.007(6) -0.009(7) 0.007(6) O15G 0.033(5) 0.042(5) 0.041(5) 0.011(4) -0.005(4) -0.006(4) O14G 0.055(6) 0.046(5) 0.036(6) -0.002(4) 0.004(4) -0.009(4) NJ3 0.063(11) 0.093(14) 0.099(16) 0.022(10) -0.034(10) -0.013(9) OJ1 0.115(14) 0.078(11) 0.088(12) 0.030(8) -0.015(10) -0.013(9) NL3 0.082(17) 0.12(2) 0.10(2) 0.069(17) -0.057(15) -0.060(13) C6H 0.136(17) 0.085(13) 0.055(10) -0.041(10) -0.018(11) 0.080(13) _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 Co2 N1D 1.949(11) . ? Co2 O15C 2.030(9) . ? Co2 N1A 2.057(12) . ? Co2 O14B 2.080(11) . ? Co2 O15B 2.223(8) . ? Co2 O14C 2.285(10) . ? Co2 C13C 2.515(15) . ? Co2 C13B 2.517(13) . ? Co4 N1F 1.976(12) . ? Co4 O14E 1.995(10) . ? Co4 O15H 2.029(10) . ? Co4 N1G 2.048(13) . ? Co4 O14H 2.272(8) . ? Co4 O15E 2.347(11) . ? Co1 O15G 2.053(9) 1_445 ? Co1 O15D 2.057(9) 7_654 ? Co1 N1C 2.078(9) . ? Co1 N1H 2.134(9) 7_754 ? Co1 O14G 2.193(9) 1_445 ? Co1 O14D 2.322(11) 7_654 ? Co1 C13G 2.414(15) 1_445 ? Co1 C13D 2.454(13) 7_654 ? Co3 O14F 2.061(9) 7_764 ? Co3 O14A 2.075(9) . ? Co3 N1E 2.078(8) . ? Co3 N1B 2.131(9) 7_754 ? Co3 O15A 2.282(9) . ? Co3 O15F 2.334(10) 7_764 ? Co3 C13F 2.417(15) 7_764 ? Co3 C13A 2.461(14) . ? O14D C13D 1.263(17) . ? O14D Co1 2.322(11) 7_655 ? O15F C13F 1.345(19) . ? O15F Co3 2.334(10) 7_765 ? O15B C13B 1.242(16) . ? O14H C13H 1.269(17) . ? O14A C13A 1.203(16) . ? O14E C13E 1.357(13) . ? O14B C13B 1.376(15) . ? O14F C13F 1.07(2) . ? O14F Co3 2.061(9) 7_765 ? O15C C13C 1.308(15) . ? O15H C13H 1.383(14) . ? C10D C9D 1.390(19) . ? C10D C11D 1.378(19) . ? C10D C13D 1.551(17) . ? O15D C13D 1.157(17) . ? O15D Co1 2.057(9) 7_655 ? O15A C13A 1.224(18) . ? C13D Co1 2.454(13) 7_655 ? C13H C10H 1.390(19) . ? C10C C9C 1.364(19) . ? C10C C11C 1.40(2) . ? C10C C13C 1.426(19) . ? C10B C9B 1.31(2) . ? C10B C11B 1.430(16) . ? C10B C13B 1.47(2) . ? C3C C4C 1.34(2) . ? C3C C2C 1.43(2) . ? C3C H3C 0.9500 . ? C13F C10F 1.593(19) . ? C13F Co3 2.417(15) 7_765 ? N1E C2E 1.323(16) . ? N1E C6E 1.390(16) . ? N1D C2D 1.405(18) . ? N1D C6D 1.423(18) . ? O14C C13C 1.272(17) . ? C9A C8A 1.328(17) . ? C9A C10A 1.380(19) . ? C9A H9A 0.9500 . ? C4F C3F 1.42(2) . ? C4F C7F 1.427(17) . ? C4F C5F 1.474(17) . ? N1C C6C 1.325(16) . ? N1C C2C 1.393(17) . ? C4B C5B 1.26(2) . ? C4B C3B 1.38(2) . ? C4B C7B 1.58(2) . ? N1F C2F 1.360(17) . ? N1F C6F 1.367(17) . ? O15E C13E 1.294(17) . ? C10F C11F 1.40(2) . ? C10F C9F 1.396(19) . ? C11C C12C 1.44(2) . ? C11C H11C 0.9500 . ? C10E C11E 1.382(17) . ? C10E C13E 1.415(18) . ? C10E C9E 1.43(2) . ? C10H C9H 1.393(16) . ? C10H C11H 1.42(2) . ? C3E C2E 1.32(2) . ? C3E C4E 1.39(2) . ? C3E H3E 0.9500 . ? C10A C11A 1.387(19) . ? C10A C13A 1.527(18) . ? C2E H2E 0.9500 . ? C4A C3A 1.37(2) . ? C4A C5A 1.463(18) . ? C4A C7A 1.512(19) . ? C8E C7E 1.364(19) . ? C8E C9E 1.424(19) . ? C8E H8E 0.9500 . ? C7E C12E 1.36(2) . ? C7E C4E 1.495(18) . ? C6F C5F 1.414(19) . ? C6F H6F 0.9500 . ? C5A C6A 1.324(17) . ? C5A H5A 0.9500 . ? C9E H9E 0.9500 . ? C4H C3H 1.32(2) . ? C4H C5H 1.35(2) . ? C4H C7H 1.55(2) . ? C4E C5E 1.35(2) . ? C5C C6C 1.31(2) . ? C5C C4C 1.38(2) . ? C5C H5C 0.9500 . ? C3G C2G 1.322(18) . ? C3G C4G 1.46(2) . ? C3G H3G 0.9500 . ? C5F H5F 0.9500 . ? C12C C7C 1.38(2) . ? C12C H12C 0.9500 . ? C7G C12G 1.368(18) . ? C7G C4G 1.448(19) . ? C7G C8G 1.487(18) . ? C11D C12D 1.46(2) . ? C11D H11D 0.9500 . ? C6G N1G 1.390(15) . ? C6G C5G 1.422(15) . ? C6G H6G 0.9500 . ? C3A C2A 1.433(14) . ? C3A H3A 0.9500 . ? C4D C5D 1.30(2) . ? C4D C3D 1.429(18) . ? C4D C7D 1.479(18) . ? C7H C8H 1.31(2) . ? C7H C12H 1.39(2) . ? C5B C6B 1.44(2) . ? C5B H5B 0.9500 . ? C7B C12B 1.32(2) . ? C7B C8B 1.41(2) . ? C7C C8C 1.30(2) . ? C7C C4C 1.560(19) . ? C8A C7A 1.391(18) . ? C8A H8A 0.9500 . ? C2D C3D 1.368(19) . ? C2D H2D 0.9500 . ? C9D C8D 1.41(2) . ? C9D H9D 0.9500 . ? C12G C11G 1.330(17) . ? C12G H12G 0.9500 . ? C11G C10G 1.381(19) . ? C11G H11G 0.9500 . ? C11H C12H 1.35(2) . ? C11H H11H 0.9500 . ? C2F C3F 1.397(18) . ? C2F H2F 0.9500 . ? C8B C9B 1.36(2) . ? C8B H8B 0.9500 . ? C9G C8G 1.311(18) . ? C9G C10G 1.352(17) . ? C9G H9G 0.9500 . ? N1G C2G 1.290(18) . ? C2C H2C 0.9500 . ? C6E C5E 1.42(2) . ? C6E H6E 0.9500 . ? C6C H6C 0.9500 . ? C7A C12A 1.46(2) . ? C5G C4G 1.40(2) . ? C5G H5G 0.9500 . ? C2A N1A 1.413(15) . ? C2A H2A 0.9500 . ? C8G H8G 0.9500 . ? C7F C8F 1.339(19) . ? C7F C12F 1.38(2) . ? C11E C12E 1.481(17) . ? C11E H11E 0.9500 . ? C9C C8C 1.451(17) . ? C9C H9C 0.9500 . ? C8D C7D 1.43(2) . ? C8D H8D 0.9500 . ? C9H C8H 1.387(18) . ? C9H H9H 0.9500 . ? C11A C12A 1.34(2) . ? C11A H11A 0.9500 . ? C12E H12E 0.9500 . ? C3B C2B 1.34(2) . ? C3B H3B 0.9500 . ? C9F C8F 1.44(2) . ? C9F H9F 0.9500 . ? C12B C11B 1.404(18) . ? C12B H12B 0.9500 . ? C8C H8C 0.9500 . ? N1A C6A 1.349(17) . ? C8H H8H 0.9500 . ? C12D C7D 1.34(2) . ? C12D H12D 0.9500 . ? C3F H3F 0.9500 . ? C2G H2G 0.9500 . ? C11B H11B 0.9500 . ? C12H H12H 0.9500 . ? C2H N1H 1.292(19) . ? C2H C3H 1.39(2) . ? C2H H2H 0.9500 . ? N1H C6H 1.300(17) . ? N1H Co1 2.134(9) 7_755 ? C8F H8F 0.9500 . ? C6D C5D 1.38(2) . ? C6D H6D 0.9500 . ? C3H H3H 0.9500 . ? C5H C6H 1.39(2) . ? C5H H5H 0.9500 . ? C5D H5D 0.9500 . ? N1B C6B 1.304(19) . ? N1B C2B 1.333(18) . ? N1B Co3 2.131(9) 7_755 ? C6B H6B 0.9500 . ? C2B H2B 0.9500 . ? C11F C12F 1.28(2) . ? C11F H11F 0.9500 . ? CM5 NM3 1.453(5) . ? CM5 HM5A 0.9800 . ? CM5 HM5B 0.9800 . ? CM5 HM5C 0.9800 . ? CK5 NK3 1.448(5) . ? CK5 HK5A 0.9800 . ? CK5 HK5B 0.9800 . ? CK5 HK5C 0.9800 . ? NK3 CK2 1.322(5) . ? NK3 CK4 1.445(5) . ? OL1 CL2 1.223(5) . ? NM3 CM2 1.318(5) . ? NM3 CM4 1.446(5) . ? CK2 OK1 1.235(5) . ? CK2 HK2 0.9500 . ? CM2 OM1 1.230(5) . ? CM2 HM2 0.9500 . ? CM4 HM4A 0.9823 . ? CM4 HM4B 0.9823 . ? CM4 HM4C 0.9823 . ? CK4 HK4A 0.9851 . ? CK4 HK4B 0.9851 . ? CK4 HK4C 0.9853 . ? C9B H9B 0.9500 . ? CL2 NL3 1.324(5) . ? CL2 HL2 0.9500 . ? C5E H5E 0.9500 . ? C12A H12A 0.9500 . ? C12F H12F 0.9500 . ? C6A H6A 0.9500 . ? CL4 NL3 1.447(5) . ? CL4 HL4A 0.9928 . ? CL4 HL4B 0.9911 . ? CL4 HL4C 0.9911 . ? C3D H3D 0.9500 . ? C10G C13G 1.589(19) . ? CL5 NL3 1.444(5) . ? CL5 HL5A 0.9800 . ? CL5 HL5B 0.9800 . ? CL5 HL5C 0.9800 . ? C13G O15G 1.172(16) . ? C13G O14G 1.230(18) . ? C13G Co1 2.414(15) 1_665 ? O15G Co1 2.053(9) 1_665 ? O14G Co1 2.193(9) 1_665 ? ON1 CN2 1.43(5) . ? CN3 CN2 1.30(5) . ? CN3 HN3A 0.9804 . ? CN3 HN3B 0.9804 . ? CN3 HN3C 0.9804 . ? CN2 HN2A 0.9900 . ? CN2 HN2B 0.9900 . ? NJ3 CJ2 1.326(5) . ? NJ3 CJ5 1.449(5) . ? NJ3 CJ4 1.449(5) . ? CJ2 OJ1 1.228(5) . ? CJ2 HJ2 0.9500 . ? CJ4 HJ4A 0.9801 . ? CJ4 HJ4B 0.9801 . ? CJ4 HJ4C 0.9802 . ? CJ5 HJ5A 0.9807 . ? CJ5 HJ5B 0.9807 . ? CJ5 HJ5C 0.9807 . ? C6H H6H 1.0094 . ? 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 N1D Co2 O15C 103.4(5) . . ? N1D Co2 N1A 100.1(5) . . ? O15C Co2 N1A 97.2(4) . . ? N1D Co2 O14B 92.9(5) . . ? O15C Co2 O14B 152.6(5) . . ? N1A Co2 O14B 101.6(5) . . ? N1D Co2 O15B 154.2(5) . . ? O15C Co2 O15B 96.6(4) . . ? N1A Co2 O15B 93.4(4) . . ? O14B Co2 O15B 62.7(4) . . ? N1D Co2 O14C 92.1(5) . . ? O15C Co2 O14C 61.4(3) . . ? N1A Co2 O14C 157.5(4) . . ? O14B Co2 O14C 96.6(4) . . ? O15B Co2 O14C 83.2(3) . . ? N1D Co2 C13C 100.6(5) . . ? O15C Co2 C13C 31.2(4) . . ? N1A Co2 C13C 127.7(4) . . ? O14B Co2 C13C 124.6(5) . . ? O15B Co2 C13C 88.1(4) . . ? O14C Co2 C13C 30.3(4) . . ? N1D Co2 C13B 125.4(5) . . ? O15C Co2 C13B 123.9(4) . . ? N1A Co2 C13B 99.3(4) . . ? O14B Co2 C13B 33.1(4) . . ? O15B Co2 C13B 29.6(3) . . ? O14C Co2 C13B 88.6(4) . . ? C13C Co2 C13B 106.5(4) . . ? N1F Co4 O14E 107.0(4) . . ? N1F Co4 O15H 93.5(4) . . ? O14E Co4 O15H 149.9(5) . . ? N1F Co4 N1G 96.6(5) . . ? O14E Co4 N1G 95.7(4) . . ? O15H Co4 N1G 103.8(5) . . ? N1F Co4 O14H 154.9(4) . . ? O14E Co4 O14H 94.9(4) . . ? O15H Co4 O14H 61.7(4) . . ? N1G Co4 O14H 93.3(4) . . ? N1F Co4 O15E 92.9(5) . . ? O14E Co4 O15E 62.3(4) . . ? O15H Co4 O15E 95.5(5) . . ? N1G Co4 O15E 157.9(5) . . ? O14H Co4 O15E 86.3(4) . . ? O15G Co1 O15D 150.9(4) 1_445 7_654 ? O15G Co1 N1C 100.6(4) 1_445 . ? O15D Co1 N1C 97.0(4) 7_654 . ? O15G Co1 N1H 100.3(4) 1_445 7_754 ? O15D Co1 N1H 99.0(4) 7_654 7_754 ? N1C Co1 N1H 100.7(4) . 7_754 ? O15G Co1 O14G 59.2(4) 1_445 1_445 ? O15D Co1 O14G 98.8(4) 7_654 1_445 ? N1C Co1 O14G 158.2(4) . 1_445 ? N1H Co1 O14G 91.7(4) 7_754 1_445 ? O15G Co1 O14D 99.2(4) 1_445 7_654 ? O15D Co1 O14D 58.5(3) 7_654 7_654 ? N1C Co1 O14D 87.4(4) . 7_654 ? N1H Co1 O14D 157.1(4) 7_754 7_654 ? O14G Co1 O14D 88.0(4) 1_445 7_654 ? O15G Co1 C13G 29.0(4) 1_445 1_445 ? O15D Co1 C13G 125.3(4) 7_654 1_445 ? N1C Co1 C13G 128.3(5) . 1_445 ? N1H Co1 C13G 100.3(4) 7_754 1_445 ? O14G Co1 C13G 30.5(4) 1_445 1_445 ? O14D Co1 C13G 91.0(4) 7_654 1_445 ? O15G Co1 C13D 127.3(4) 1_445 7_654 ? O15D Co1 C13D 28.0(4) 7_654 7_654 ? N1C Co1 C13D 93.2(4) . 7_654 ? N1H Co1 C13D 126.8(5) 7_754 7_654 ? O14G Co1 C13D 93.6(4) 1_445 7_654 ? O14D Co1 C13D 30.5(4) 7_654 7_654 ? C13G Co1 C13D 110.3(5) 1_445 7_654 ? O14F Co3 O14A 150.4(4) 7_764 . ? O14F Co3 N1E 95.8(4) 7_764 . ? O14A Co3 N1E 101.8(4) . . ? O14F Co3 N1B 98.3(4) 7_764 7_754 ? O14A Co3 N1B 101.3(4) . 7_754 ? N1E Co3 N1B 101.3(4) . 7_754 ? O14F Co3 O15A 100.1(4) 7_764 . ? O14A Co3 O15A 58.4(4) . . ? N1E Co3 O15A 159.4(4) . . ? N1B Co3 O15A 89.3(4) 7_754 . ? O14F Co3 O15F 59.0(3) 7_764 7_764 ? O14A Co3 O15F 96.8(4) . 7_764 ? N1E Co3 O15F 91.0(4) . 7_764 ? N1B Co3 O15F 155.5(4) 7_754 7_764 ? O15A Co3 O15F 86.2(4) . 7_764 ? O14F Co3 C13F 26.3(5) 7_764 7_764 ? O14A Co3 C13F 127.0(6) . 7_764 ? N1E Co3 C13F 95.7(4) . 7_764 ? N1B Co3 C13F 123.8(5) 7_754 7_764 ? O15A Co3 C13F 92.9(5) . 7_764 ? O15F Co3 C13F 32.8(5) 7_764 7_764 ? O14F Co3 C13A 125.3(4) 7_764 . ? O14A Co3 C13A 29.2(4) . . ? N1E Co3 C13A 130.0(5) . . ? N1B Co3 C13A 99.4(4) 7_754 . ? O15A Co3 C13A 29.6(4) . . ? O15F Co3 C13A 88.4(4) 7_764 . ? C13F Co3 C13A 109.4(6) 7_764 . ? C13D O14D Co1 80.5(9) . 7_655 ? C13F O15F Co3 77.0(9) . 7_765 ? C13B O15B Co2 88.4(7) . . ? C13H O14H Co4 88.7(7) . . ? C13A O14A Co3 93.5(9) . . ? C13E O14E Co4 96.9(8) . . ? C13B O14B Co2 91.1(8) . . ? C13F O14F Co3 95.7(9) . 7_765 ? C13C O15C Co2 95.3(8) . . ? C13H O15H Co4 96.2(8) . . ? C9D C10D C11D 120.3(13) . . ? C9D C10D C13D 122.9(13) . . ? C11D C10D C13D 115.7(13) . . ? C13D O15D Co1 95.5(8) . 7_655 ? C13A O15A Co3 83.3(8) . . ? O15D C13D O14D 125.5(13) . . ? O15D C13D C10D 120.0(12) . . ? O14D C13D C10D 114.4(14) . . ? O15D C13D Co1 56.5(7) . 7_655 ? O14D C13D Co1 69.0(8) . 7_655 ? C10D C13D Co1 173.8(10) . 7_655 ? O14H C13H O15H 113.3(11) . . ? O14H C13H C10H 126.5(11) . . ? O15H C13H C10H 120.1(12) . . ? C9C C10C C11C 120.3(14) . . ? C9C C10C C13C 118.2(14) . . ? C11C C10C C13C 121.5(13) . . ? C9B C10B C11B 119.6(15) . . ? C9B C10B C13B 125.1(13) . . ? C11B C10B C13B 115.0(13) . . ? C4C C3C C2C 121.6(17) . . ? C4C C3C H3C 119.1 . . ? C2C C3C H3C 119.2 . . ? O14F C13F O15F 128.0(14) . . ? O14F C13F C10F 123.8(14) . . ? O15F C13F C10F 107.9(15) . . ? O14F C13F Co3 58.1(8) . 7_765 ? O15F C13F Co3 70.2(7) . 7_765 ? C10F C13F Co3 178.0(13) . 7_765 ? C2E N1E C6E 115.3(12) . . ? C2E N1E Co3 127.0(9) . . ? C6E N1E Co3 117.0(10) . . ? C2D N1D C6D 108.3(11) . . ? C2D N1D Co2 123.3(9) . . ? C6D N1D Co2 126.9(10) . . ? C13C O14C Co2 84.9(8) . . ? C8A C9A C10A 124.5(14) . . ? C8A C9A H9A 117.7 . . ? C10A C9A H9A 117.8 . . ? C3F C4F C7F 125.1(13) . . ? C3F C4F C5F 113.5(12) . . ? C7F C4F C5F 121.4(13) . . ? O15B C13B O14B 117.7(11) . . ? O15B C13B C10B 127.0(11) . . ? O14B C13B C10B 115.2(12) . . ? O15B C13B Co2 62.0(7) . . ? O14B C13B Co2 55.7(6) . . ? C10B C13B Co2 171.0(9) . . ? C6C N1C C2C 118.2(11) . . ? C6C N1C Co1 126.2(9) . . ? C2C N1C Co1 115.3(8) . . ? C5B C4B C3B 119.9(14) . . ? C5B C4B C7B 120.4(14) . . ? C3B C4B C7B 119.6(13) . . ? C2F N1F C6F 112.8(12) . . ? C2F N1F Co4 126.0(9) . . ? C6F N1F Co4 120.9(9) . . ? C13E O15E Co4 83.2(8) . . ? C11F C10F C9F 120.1(13) . . ? C11F C10F C13F 129.1(14) . . ? C9F C10F C13F 110.8(14) . . ? C10C C11C C12C 116.3(14) . . ? C10C C11C H11C 121.8 . . ? C12C C11C H11C 121.9 . . ? C11E C10E C13E 117.5(13) . . ? C11E C10E C9E 118.4(12) . . ? C13E C10E C9E 124.1(12) . . ? C13H C10H C9H 120.9(14) . . ? C13H C10H C11H 125.5(13) . . ? C9H C10H C11H 113.6(14) . . ? C2E C3E C4E 119.8(16) . . ? C2E C3E H3E 120.1 . . ? C4E C3E H3E 120.1 . . ? C9A C10A C11A 117.1(12) . . ? C9A C10A C13A 119.8(13) . . ? C11A C10A C13A 122.6(12) . . ? N1E C2E C3E 125.9(14) . . ? N1E C2E H2E 117.0 . . ? C3E C2E H2E 117.1 . . ? C3A C4A C5A 115.9(12) . . ? C3A C4A C7A 123.7(12) . . ? C5A C4A C7A 120.2(13) . . ? C7E C8E C9E 123.2(14) . . ? C7E C8E H8E 118.5 . . ? C9E C8E H8E 118.3 . . ? O14A C13A O15A 123.2(14) . . ? O14A C13A C10A 117.3(14) . . ? O15A C13A C10A 119.5(12) . . ? O14A C13A Co3 57.3(7) . . ? O15A C13A Co3 67.1(8) . . ? C10A C13A Co3 170.0(10) . . ? C8E C7E C12E 117.8(13) . . ? C8E C7E C4E 121.8(13) . . ? C12E C7E C4E 119.1(13) . . ? N1F C6F C5F 125.6(12) . . ? N1F C6F H6F 117.2 . . ? C5F C6F H6F 117.2 . . ? C6A C5A C4A 119.4(13) . . ? C6A C5A H5A 120.3 . . ? C4A C5A H5A 120.4 . . ? C8E C9E C10E 119.2(12) . . ? C8E C9E H9E 120.5 . . ? C10E C9E H9E 120.4 . . ? C3H C4H C5H 118.5(15) . . ? C3H C4H C7H 120.0(14) . . ? C5H C4H C7H 121.5(12) . . ? C5E C4E C3E 118.3(14) . . ? C5E C4E C7E 122.4(14) . . ? C3E C4E C7E 119.1(14) . . ? C6C C5C C4C 121.9(16) . . ? C6C C5C H5C 118.9 . . ? C4C C5C H5C 119.1 . . ? C2G C3G C4G 119.3(14) . . ? C2G C3G H3G 120.4 . . ? C4G C3G H3G 120.4 . . ? C6F C5F C4F 119.6(12) . . ? C6F C5F H5F 120.2 . . ? C4F C5F H5F 120.2 . . ? C7C C12C C11C 121.6(15) . . ? C7C C12C H12C 119.2 . . ? C11C C12C H12C 119.2 . . ? C12G C7G C4G 123.3(12) . . ? C12G C7G C8G 114.9(12) . . ? C4G C7G C8G 121.3(13) . . ? C10D C11D C12D 117.1(13) . . ? C10D C11D H11D 121.4 . . ? C12D C11D H11D 121.5 . . ? O14C C13C O15C 118.1(13) . . ? O14C C13C C10C 123.4(13) . . ? O15C C13C C10C 118.4(12) . . ? O14C C13C Co2 64.8(8) . . ? O15C C13C Co2 53.5(7) . . ? C10C C13C Co2 168.1(11) . . ? N1G C6G C5G 124.0(12) . . ? N1G C6G H6G 118.0 . . ? C5G C6G H6G 118.0 . . ? C4A C3A C2A 121.4(11) . . ? C4A C3A H3A 119.3 . . ? C2A C3A H3A 119.3 . . ? C5D C4D C3D 116.9(14) . . ? C5D C4D C7D 122.2(14) . . ? C3D C4D C7D 120.2(13) . . ? C8H C7H C12H 121.9(16) . . ? C8H C7H C4H 121.8(13) . . ? C12H C7H C4H 116.2(14) . . ? C4B C5B C6B 119.4(15) . . ? C4B C5B H5B 120.3 . . ? C6B C5B H5B 120.3 . . ? C12B C7B C8B 119.1(16) . . ? C12B C7B C4B 120.9(15) . . ? C8B C7B C4B 119.2(14) . . ? C8C C7C C12C 120.9(15) . . ? C8C C7C C4C 120.3(12) . . ? C12C C7C C4C 118.0(14) . . ? C9A C8A C7A 117.1(14) . . ? C9A C8A H8A 121.5 . . ? C7A C8A H8A 121.5 . . ? C3D C2D N1D 124.5(13) . . ? C3D C2D H2D 117.7 . . ? N1D C2D H2D 117.7 . . ? C10D C9D C8D 123.4(14) . . ? C10D C9D H9D 118.4 . . ? C8D C9D H9D 118.2 . . ? C11G C12G C7G 119.5(13) . . ? C11G C12G H12G 120.3 . . ? C7G C12G H12G 120.2 . . ? C12G C11G C10G 122.3(13) . . ? C12G C11G H11G 118.8 . . ? C10G C11G H11G 118.8 . . ? C12H C11H C10H 128.2(19) . . ? C12H C11H H11H 115.9 . . ? C10H C11H H11H 116.0 . . ? N1F C2F C3F 127.5(13) . . ? N1F C2F H2F 116.1 . . ? C3F C2F H2F 116.3 . . ? O15E C13E O14E 117.5(12) . . ? O15E C13E C10E 124.2(11) . . ? O14E C13E C10E 117.1(11) . . ? C9B C8B C7B 118.1(14) . . ? C9B C8B H8B 120.9 . . ? C7B C8B H8B 121.0 . . ? C8G C9G C10G 118.7(12) . . ? C8G C9G H9G 120.7 . . ? C10G C9G H9G 120.6 . . ? C2G N1G C6G 113.2(12) . . ? C2G N1G Co4 127.9(10) . . ? C6G N1G Co4 118.3(9) . . ? N1C C2C C3C 117.1(13) . . ? N1C C2C H2C 121.5 . . ? C3C C2C H2C 121.4 . . ? N1E C6E C5E 120.7(14) . . ? N1E C6E H6E 119.6 . . ? C5E C6E H6E 119.7 . . ? N1C C6C C5C 123.5(14) . . ? N1C C6C H6C 118.2 . . ? C5C C6C H6C 118.3 . . ? C8A C7A C12A 119.8(13) . . ? C8A C7A C4A 121.2(12) . . ? C12A C7A C4A 118.6(13) . . ? C6G C5G C4G 118.3(11) . . ? C6G C5G H5G 121.0 . . ? C4G C5G H5G 120.8 . . ? C3A C2A N1A 120.5(11) . . ? C3A C2A H2A 119.8 . . ? N1A C2A H2A 119.8 . . ? C5G C4G C7G 123.3(13) . . ? C5G C4G C3G 114.9(13) . . ? C7G C4G C3G 121.7(15) . . ? C9G C8G C7G 121.8(12) . . ? C9G C8G H8G 119.1 . . ? C7G C8G H8G 119.1 . . ? C8F C7F C12F 117.2(14) . . ? C8F C7F C4F 121.5(13) . . ? C12F C7F C4F 121.0(14) . . ? C10E C11E C12E 118.5(12) . . ? C10E C11E H11E 120.7 . . ? C12E C11E H11E 120.8 . . ? C10C C9C C8C 120.3(14) . . ? C10C C9C H9C 119.9 . . ? C8C C9C H9C 119.9 . . ? C9D C8D C7D 114.8(14) . . ? C9D C8D H8D 122.6 . . ? C7D C8D H8D 122.6 . . ? C10H C9H C8H 118.2(13) . . ? C10H C9H H9H 120.9 . . ? C8H C9H H9H 120.9 . . ? C12A C11A C10A 122.8(13) . . ? C12A C11A H11A 118.5 . . ? C10A C11A H11A 118.7 . . ? C7E C12E C11E 122.1(13) . . ? C7E C12E H12E 119.0 . . ? C11E C12E H12E 118.9 . . ? C2B C3B C4B 121.5(13) . . ? C2B C3B H3B 119.3 . . ? C4B C3B H3B 119.2 . . ? C10F C9F C8F 113.0(14) . . ? C10F C9F H9F 123.5 . . ? C8F C9F H9F 123.5 . . ? C7B C12B C11B 123.1(14) . . ? C7B C12B H12B 118.4 . . ? C11B C12B H12B 118.5 . . ? C7C C8C C9C 119.6(13) . . ? C7C C8C H8C 120.2 . . ? C9C C8C H8C 120.1 . . ? C6A N1A C2A 114.6(11) . . ? C6A N1A Co2 126.5(9) . . ? C2A N1A Co2 117.7(9) . . ? C7H C8H C9H 124.1(13) . . ? C7H C8H H8H 118.0 . . ? C9H C8H H8H 117.9 . . ? C7D C12D C11D 120.9(14) . . ? C7D C12D H12D 119.5 . . ? C11D C12D H12D 119.6 . . ? C3C C4C C5C 116.7(15) . . ? C3C C4C C7C 121.6(14) . . ? C5C C4C C7C 121.1(15) . . ? C2F C3F C4F 119.9(13) . . ? C2F C3F H3F 120.0 . . ? C4F C3F H3F 120.1 . . ? N1G C2G C3G 129.3(13) . . ? N1G C2G H2G 115.3 . . ? C3G C2G H2G 115.4 . . ? C12B C11B C10B 115.5(13) . . ? C12B C11B H11B 122.2 . . ? C10B C11B H11B 122.2 . . ? C11H C12H C7H 113.6(17) . . ? C11H C12H H12H 123.3 . . ? C7H C12H H12H 123.2 . . ? N1H C2H C3H 124.5(15) . . ? N1H C2H H2H 117.7 . . ? C3H C2H H2H 117.8 . . ? C2H N1H C6H 118.8(13) . . ? C2H N1H Co1 118.0(9) . 7_755 ? C6H N1H Co1 122.4(11) . 7_755 ? C7F C8F C9F 124.9(14) . . ? C7F C8F H8F 117.6 . . ? C9F C8F H8F 117.5 . . ? N1D C6D C5D 128.3(14) . . ? N1D C6D H6D 115.9 . . ? C5D C6D H6D 115.8 . . ? C4H C3H C2H 117.5(17) . . ? C4H C3H H3H 121.3 . . ? C2H C3H H3H 121.3 . . ? C6H C5H C4H 121.2(14) . . ? C6H C5H H5H 119.4 . . ? C4H C5H H5H 119.3 . . ? C4D C5D C6D 119.2(16) . . ? C4D C5D H5D 120.4 . . ? C6D C5D H5D 120.4 . . ? C6B N1B C2B 122.3(13) . . ? C6B N1B Co3 113.8(10) . 7_755 ? C2B N1B Co3 123.6(10) . 7_755 ? N1B C6B C5B 118.3(14) . . ? N1B C6B H6B 120.9 . . ? C5B C6B H6B 120.8 . . ? N1B C2B C3B 118.1(15) . . ? N1B C2B H2B 121.1 . . ? C3B C2B H2B 120.8 . . ? C12F C11F C10F 123.0(16) . . ? C12F C11F H11F 118.6 . . ? C10F C11F H11F 118.5 . . ? NM3 CM5 HM5A 109.5 . . ? NM3 CM5 HM5B 109.4 . . ? HM5A CM5 HM5B 109.5 . . ? NM3 CM5 HM5C 109.5 . . ? HM5A CM5 HM5C 109.5 . . ? HM5B CM5 HM5C 109.5 . . ? NK3 CK5 HK5A 109.4 . . ? NK3 CK5 HK5B 109.6 . . ? HK5A CK5 HK5B 109.5 . . ? NK3 CK5 HK5C 109.4 . . ? HK5A CK5 HK5C 109.5 . . ? HK5B CK5 HK5C 109.5 . . ? CK2 NK3 CK4 120.5(5) . . ? CK2 NK3 CK5 120.5(6) . . ? CK4 NK3 CK5 118.1(9) . . ? CM2 NM3 CM4 120.9(6) . . ? CM2 NM3 CM5 120.1(6) . . ? CM4 NM3 CM5 119.0(9) . . ? OK1 CK2 NK3 124.0(6) . . ? OK1 CK2 HK2 117.9 . . ? NK3 CK2 HK2 118.1 . . ? OM1 CM2 NM3 125.3(7) . . ? OM1 CM2 HM2 117.4 . . ? NM3 CM2 HM2 117.3 . . ? NM3 CM4 HM4A 109.6 . . ? NM3 CM4 HM4B 109.8 . . ? HM4A CM4 HM4B 109.2 . . ? NM3 CM4 HM4C 109.7 . . ? HM4A CM4 HM4C 109.2 . . ? HM4B CM4 HM4C 109.2 . . ? NK3 CK4 HK4A 109.9 . . ? NK3 CK4 HK4B 109.8 . . ? HK4A CK4 HK4B 108.9 . . ? NK3 CK4 HK4C 110.3 . . ? HK4A CK4 HK4C 108.9 . . ? HK4B CK4 HK4C 108.9 . . ? C12D C7D C8D 122.5(13) . . ? C12D C7D C4D 118.9(14) . . ? C8D C7D C4D 117.3(14) . . ? C10B C9B C8B 123.2(16) . . ? C10B C9B H9B 118.4 . . ? C8B C9B H9B 118.4 . . ? OL1 CL2 NL3 124.9(7) . . ? OL1 CL2 HL2 117.6 . . ? NL3 CL2 HL2 117.6 . . ? C4E C5E C6E 119.4(14) . . ? C4E C5E H5E 120.2 . . ? C6E C5E H5E 120.3 . . ? C11A C12A C7A 117.0(14) . . ? C11A C12A H12A 121.5 . . ? C7A C12A H12A 121.5 . . ? C11F C12F C7F 121.7(17) . . ? C11F C12F H12F 119.1 . . ? C7F C12F H12F 119.2 . . ? C5A C6A N1A 127.1(12) . . ? C5A C6A H6A 116.4 . . ? N1A C6A H6A 116.5 . . ? NL3 CL4 HL4A 111.5 . . ? NL3 CL4 HL4B 110.2 . . ? HL4A CL4 HL4B 108.4 . . ? NL3 CL4 HL4C 110.4 . . ? HL4A CL4 HL4C 108.0 . . ? HL4B CL4 HL4C 108.3 . . ? C2D C3D C4D 121.2(14) . . ? C2D C3D H3D 119.4 . . ? C4D C3D H3D 119.3 . . ? C9G C10G C11G 120.3(12) . . ? C9G C10G C13G 122.1(12) . . ? C11G C10G C13G 117.1(12) . . ? NL3 CL5 HL5A 109.5 . . ? NL3 CL5 HL5B 109.6 . . ? HL5A CL5 HL5B 109.5 . . ? NL3 CL5 HL5C 109.4 . . ? HL5A CL5 HL5C 109.5 . . ? HL5B CL5 HL5C 109.5 . . ? O15G C13G O14G 121.8(14) . . ? O15G C13G C10G 120.3(14) . . ? O14G C13G C10G 117.9(13) . . ? O15G C13G Co1 58.2(8) . 1_665 ? O14G C13G Co1 64.8(8) . 1_665 ? C10G C13G Co1 169.3(10) . 1_665 ? C13G O15G Co1 92.8(9) . 1_665 ? C13G O14G Co1 84.7(9) . 1_665 ? CN2 CN3 HN3A 109.8 . . ? CN2 CN3 HN3B 109.1 . . ? HN3A CN3 HN3B 109.4 . . ? CN2 CN3 HN3C 109.7 . . ? HN3A CN3 HN3C 109.4 . . ? HN3B CN3 HN3C 109.4 . . ? CN3 CN2 ON1 114(4) . . ? CN3 CN2 HN2A 108.9 . . ? ON1 CN2 HN2A 108.6 . . ? CN3 CN2 HN2B 108.6 . . ? ON1 CN2 HN2B 108.6 . . ? HN2A CN2 HN2B 107.5 . . ? CJ2 NJ3 CJ5 119.5(6) . . ? CJ2 NJ3 CJ4 119.7(6) . . ? CJ5 NJ3 CJ4 120.8(10) . . ? OJ1 CJ2 NJ3 124.5(7) . . ? OJ1 CJ2 HJ2 117.7 . . ? NJ3 CJ2 HJ2 117.8 . . ? NJ3 CJ4 HJ4A 109.4 . . ? NJ3 CJ4 HJ4B 109.2 . . ? HJ4A CJ4 HJ4B 109.5 . . ? NJ3 CJ4 HJ4C 109.8 . . ? HJ4A CJ4 HJ4C 109.5 . . ? HJ4B CJ4 HJ4C 109.4 . . ? NJ3 CJ5 HJ5A 109.7 . . ? NJ3 CJ5 HJ5B 109.5 . . ? HJ5A CJ5 HJ5B 109.4 . . ? NJ3 CJ5 HJ5C 109.4 . . ? HJ5A CJ5 HJ5C 109.4 . . ? HJ5B CJ5 HJ5C 109.4 . . ? CL2 NL3 CL5 120.3(6) . . ? CL2 NL3 CL4 120.2(6) . . ? CL5 NL3 CL4 119.0(10) . . ? N1H C6H C5H 119.4(15) . . ? N1H C6H H6H 118.7 . . ? C5H C6H H6H 121.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1D Co2 O15B C13B -18.7(13) . . . . ? O15C Co2 O15B C13B -159.4(7) . . . . ? N1A Co2 O15B C13B 103.0(7) . . . . ? O14B Co2 O15B C13B 1.7(7) . . . . ? O14C Co2 O15B C13B -99.4(7) . . . . ? C13C Co2 O15B C13B -129.3(7) . . . . ? N1F Co4 O14H C13H -9.0(13) . . . . ? O14E Co4 O14H C13H -159.8(7) . . . . ? O15H Co4 O14H C13H 0.2(7) . . . . ? N1G Co4 O14H C13H 104.1(7) . . . . ? O15E Co4 O14H C13H -98.0(7) . . . . ? O14F Co3 O14A C13A 41.5(13) 7_764 . . . ? N1E Co3 O14A C13A 166.7(8) . . . . ? N1B Co3 O14A C13A -89.1(9) 7_754 . . . ? O15A Co3 O14A C13A -7.0(8) . . . . ? O15F Co3 O14A C13A 74.3(9) 7_764 . . . ? C13F Co3 O14A C13A 60.2(10) 7_764 . . . ? N1F Co4 O14E C13E -85.5(8) . . . . ? O15H Co4 O14E C13E 45.2(11) . . . . ? N1G Co4 O14E C13E 175.8(7) . . . . ? O14H Co4 O14E C13E 82.0(7) . . . . ? O15E Co4 O14E C13E -1.3(7) . . . . ? N1D Co2 O14B C13B 169.7(8) . . . . ? O15C Co2 O14B C13B 42.8(12) . . . . ? N1A Co2 O14B C13B -89.3(7) . . . . ? O15B Co2 O14B C13B -1.5(6) . . . . ? O14C Co2 O14B C13B 77.2(7) . . . . ? C13C Co2 O14B C13B 64.8(8) . . . . ? N1D Co2 O15C C13C -88.3(10) . . . . ? N1A Co2 O15C C13C 169.4(9) . . . . ? O14B Co2 O15C C13C 36.5(14) . . . . ? O15B Co2 O15C C13C 75.2(9) . . . . ? O14C Co2 O15C C13C -3.3(9) . . . . ? C13B Co2 O15C C13C 63.1(10) . . . . ? N1F Co4 O15H C13H 175.9(8) . . . . ? O14E Co4 O15H C13H 42.5(12) . . . . ? N1G Co4 O15H C13H -86.5(8) . . . . ? O14H Co4 O15H C13H -0.2(6) . . . . ? O15E Co4 O15H C13H 82.6(8) . . . . ? O14F Co3 O15A C13A -151.1(8) 7_764 . . . ? O14A Co3 O15A C13A 6.9(8) . . . . ? N1E Co3 O15A C13A -10.8(16) . . . . ? N1B Co3 O15A C13A 110.6(9) 7_754 . . . ? O15F Co3 O15A C13A -93.5(8) 7_764 . . . ? C13F Co3 O15A C13A -125.6(9) 7_764 . . . ? Co1 O15D C13D O14D 2.0(17) 7_655 . . . ? Co1 O15D C13D C10D -174.0(11) 7_655 . . . ? Co1 O14D C13D O15D -1.8(15) 7_655 . . . ? Co1 O14D C13D C10D 174.4(11) 7_655 . . . ? C9D C10D C13D O15D -177.6(14) . . . . ? C11D C10D C13D O15D -9(2) . . . . ? C9D C10D C13D O14D 6(2) . . . . ? C11D C10D C13D O14D 174.5(15) . . . . ? C9D C10D C13D Co1 128(10) . . . 7_655 ? C11D C10D C13D Co1 -63(11) . . . 7_655 ? Co4 O14H C13H O15H -0.3(10) . . . . ? Co4 O14H C13H C10H -177.6(12) . . . . ? Co4 O15H C13H O14H 0.3(11) . . . . ? Co4 O15H C13H C10H 177.8(10) . . . . ? Co3 O14F C13F O15F 6(2) 7_765 . . . ? Co3 O14F C13F C10F 179.3(14) 7_765 . . . ? Co3 O15F C13F O14F -5.8(18) 7_765 . . . ? Co3 O15F C13F C10F -179.6(12) 7_765 . . . ? O14F Co3 N1E C2E -8.4(12) 7_764 . . . ? O14A Co3 N1E C2E -164.5(11) . . . . ? N1B Co3 N1E C2E 91.3(12) 7_754 . . . ? O15A Co3 N1E C2E -149.2(12) . . . . ? O15F Co3 N1E C2E -67.4(12) 7_764 . . . ? C13F Co3 N1E C2E -34.8(13) 7_764 . . . ? C13A Co3 N1E C2E -156.1(11) . . . . ? O14F Co3 N1E C6E -178.3(10) 7_764 . . . ? O14A Co3 N1E C6E 25.6(10) . . . . ? N1B Co3 N1E C6E -78.6(10) 7_754 . . . ? O15A Co3 N1E C6E 40.9(16) . . . . ? O15F Co3 N1E C6E 122.7(10) 7_764 . . . ? C13F Co3 N1E C6E 155.3(10) 7_764 . . . ? C13A Co3 N1E C6E 34.0(12) . . . . ? O15C Co2 N1D C2D 154.3(13) . . . . ? N1A Co2 N1D C2D -105.7(13) . . . . ? O14B Co2 N1D C2D -3.4(14) . . . . ? O15B Co2 N1D C2D 15(2) . . . . ? O14C Co2 N1D C2D 93.3(13) . . . . ? C13C Co2 N1D C2D 122.6(13) . . . . ? C13B Co2 N1D C2D 3.5(16) . . . . ? O15C Co2 N1D C6D -10.0(18) . . . . ? N1A Co2 N1D C6D 89.9(18) . . . . ? O14B Co2 N1D C6D -167.8(18) . . . . ? O15B Co2 N1D C6D -149.7(16) . . . . ? O14C Co2 N1D C6D -71.1(18) . . . . ? C13C Co2 N1D C6D -41.8(18) . . . . ? C13B Co2 N1D C6D -160.9(17) . . . . ? N1D Co2 O14C C13C 107.5(9) . . . . ? O15C Co2 O14C C13C 3.4(9) . . . . ? N1A Co2 O14C C13C -15.7(16) . . . . ? O14B Co2 O14C C13C -159.3(9) . . . . ? O15B Co2 O14C C13C -98.0(9) . . . . ? C13B Co2 O14C C13C -127.1(9) . . . . ? Co2 O15B C13B O14B -2.6(10) . . . . ? Co2 O15B C13B C10B -179.3(11) . . . . ? Co2 O14B C13B O15B 2.8(11) . . . . ? Co2 O14B C13B C10B 179.9(9) . . . . ? C9B C10B C13B O15B 179.1(15) . . . . ? C11B C10B C13B O15B -7.5(19) . . . . ? C9B C10B C13B O14B 2(2) . . . . ? C11B C10B C13B O14B 175.8(11) . . . . ? C9B C10B C13B Co2 3(6) . . . . ? C11B C10B C13B Co2 176(5) . . . . ? N1D Co2 C13B O15B 170.1(7) . . . . ? O15C Co2 C13B O15B 24.9(8) . . . . ? N1A Co2 C13B O15B -80.3(7) . . . . ? O14B Co2 C13B O15B -177.2(11) . . . . ? O14C Co2 C13B O15B 78.5(7) . . . . ? C13C Co2 C13B O15B 53.7(7) . . . . ? N1D Co2 C13B O14B -12.6(9) . . . . ? O15C Co2 C13B O14B -157.8(7) . . . . ? N1A Co2 C13B O14B 96.9(7) . . . . ? O15B Co2 C13B O14B 177.2(11) . . . . ? O14C Co2 C13B O14B -104.3(7) . . . . ? C13C Co2 C13B O14B -129.0(7) . . . . ? N1D Co2 C13B C10B -13(6) . . . . ? O15C Co2 C13B C10B -159(5) . . . . ? N1A Co2 C13B C10B 96(5) . . . . ? O14B Co2 C13B C10B -1(5) . . . . ? O15B Co2 C13B C10B 177(6) . . . . ? O14C Co2 C13B C10B -105(5) . . . . ? C13C Co2 C13B C10B -130(5) . . . . ? O15G Co1 N1C C6C -160.3(12) 1_445 . . . ? O15D Co1 N1C C6C -3.6(13) 7_654 . . . ? N1H Co1 N1C C6C 97.0(12) 7_754 . . . ? O14G Co1 N1C C6C -139.4(13) 1_445 . . . ? O14D Co1 N1C C6C -61.4(12) 7_654 . . . ? C13G Co1 N1C C6C -150.6(12) 1_445 . . . ? C13D Co1 N1C C6C -31.4(13) 7_654 . . . ? O15G Co1 N1C C2C 26.1(10) 1_445 . . . ? O15D Co1 N1C C2C -177.2(10) 7_654 . . . ? N1H Co1 N1C C2C -76.6(10) 7_754 . . . ? O14G Co1 N1C C2C 46.9(17) 1_445 . . . ? O14D Co1 N1C C2C 125.0(10) 7_654 . . . ? C13G Co1 N1C C2C 35.8(12) 1_445 . . . ? C13D Co1 N1C C2C 154.9(10) 7_654 . . . ? O14E Co4 N1F C2F -31.9(13) . . . . ? O15H Co4 N1F C2F 170.4(12) . . . . ? N1G Co4 N1F C2F 66.1(13) . . . . ? O14H Co4 N1F C2F 178.6(9) . . . . ? O15E Co4 N1F C2F -93.9(12) . . . . ? O14E Co4 N1F C6F 140.9(11) . . . . ? O15H Co4 N1F C6F -16.7(12) . . . . ? N1G Co4 N1F C6F -121.0(12) . . . . ? O14H Co4 N1F C6F -8.5(19) . . . . ? O15E Co4 N1F C6F 79.0(12) . . . . ? N1F Co4 O15E C13E 109.0(9) . . . . ? O14E Co4 O15E C13E 1.3(8) . . . . ? O15H Co4 O15E C13E -157.3(8) . . . . ? N1G Co4 O15E C13E -6.5(16) . . . . ? O14H Co4 O15E C13E -96.2(8) . . . . ? O14F C13F C10F C11F 178.9(19) . . . . ? O15F C13F C10F C11F -7(2) . . . . ? Co3 C13F C10F C11F -18(38) 7_765 . . . ? O14F C13F C10F C9F -4(2) . . . . ? O15F C13F C10F C9F 169.9(15) . . . . ? Co3 C13F C10F C9F 159(36) 7_765 . . . ? C9C C10C C11C C12C -9(2) . . . . ? C13C C10C C11C C12C 168.9(14) . . . . ? O14H C13H C10H C9H -11(2) . . . . ? O15H C13H C10H C9H 172.4(13) . . . . ? O14H C13H C10H C11H 167.7(16) . . . . ? O15H C13H C10H C11H -9(2) . . . . ? C8A C9A C10A C11A 2(2) . . . . ? C8A C9A C10A C13A 173.7(14) . . . . ? C6E N1E C2E C3E -9(2) . . . . ? Co3 N1E C2E C3E -178.9(13) . . . . ? C4E C3E C2E N1E 5(3) . . . . ? Co3 O14A C13A O15A 13.3(15) . . . . ? Co3 O14A C13A C10A -170.4(10) . . . . ? Co3 O15A C13A O14A -12.2(14) . . . . ? Co3 O15A C13A C10A 171.6(12) . . . . ? C9A C10A C13A O14A 4(2) . . . . ? C11A C10A C13A O14A 175.2(14) . . . . ? C9A C10A C13A O15A -179.9(14) . . . . ? C11A C10A C13A O15A -8(2) . . . . ? C9A C10A C13A Co3 -51(6) . . . . ? C11A C10A C13A Co3 121(6) . . . . ? O14F Co3 C13A O14A -156.4(8) 7_764 . . . ? N1E Co3 C13A O14A -17.0(11) . . . . ? N1B Co3 C13A O14A 96.4(9) 7_754 . . . ? O15A Co3 C13A O14A 167.9(14) . . . . ? O15F Co3 C13A O14A -107.0(9) 7_764 . . . ? C13F Co3 C13A O14A -132.7(9) 7_764 . . . ? O14F Co3 C13A O15A 35.7(10) 7_764 . . . ? O14A Co3 C13A O15A -167.9(14) . . . . ? N1E Co3 C13A O15A 175.1(7) . . . . ? N1B Co3 C13A O15A -71.5(9) 7_754 . . . ? O15F Co3 C13A O15A 85.1(8) 7_764 . . . ? C13F Co3 C13A O15A 59.4(9) 7_764 . . . ? O14F Co3 C13A C10A -97(6) 7_764 . . . ? O14A Co3 C13A C10A 59(6) . . . . ? N1E Co3 C13A C10A 42(6) . . . . ? N1B Co3 C13A C10A 156(6) 7_754 . . . ? O15A Co3 C13A C10A -133(6) . . . . ? O15F Co3 C13A C10A -48(6) 7_764 . . . ? C13F Co3 C13A C10A -73(6) 7_764 . . . ? C9E C8E C7E C12E -4(2) . . . . ? C9E C8E C7E C4E -171.2(13) . . . . ? C2F N1F C6F C5F 3(2) . . . . ? Co4 N1F C6F C5F -170.4(11) . . . . ? C3A C4A C5A C6A -0.3(19) . . . . ? C7A C4A C5A C6A -174.5(13) . . . . ? C7E C8E C9E C10E 4.8(19) . . . . ? C11E C10E C9E C8E -7.6(19) . . . . ? C13E C10E C9E C8E 171.8(13) . . . . ? C2E C3E C4E C5E 2(3) . . . . ? C2E C3E C4E C7E 177.0(15) . . . . ? C8E C7E C4E C5E 142.5(16) . . . . ? C12E C7E C4E C5E -25(2) . . . . ? C8E C7E C4E C3E -33(2) . . . . ? C12E C7E C4E C3E 160.2(17) . . . . ? N1F C6F C5F C4F 1(2) . . . . ? C3F C4F C5F C6F -9.4(19) . . . . ? C7F C4F C5F C6F 173.0(13) . . . . ? C10C C11C C12C C7C 7(2) . . . . ? C9D C10D C11D C12D -4(3) . . . . ? C13D C10D C11D C12D -172.3(16) . . . . ? Co2 O14C C13C O15C -5.2(14) . . . . ? Co2 O14C C13C C10C 170.2(15) . . . . ? Co2 O15C C13C O14C 5.9(16) . . . . ? Co2 O15C C13C C10C -169.8(12) . . . . ? C9C C10C C13C O14C -5(2) . . . . ? C11C C10C C13C O14C 176.6(14) . . . . ? C9C C10C C13C O15C 170.1(14) . . . . ? C11C C10C C13C O15C -8(2) . . . . ? C9C C10C C13C Co2 126(5) . . . . ? C11C C10C C13C Co2 -52(6) . . . . ? N1D Co2 C13C O14C -75.8(9) . . . . ? O15C Co2 C13C O14C -174.2(15) . . . . ? N1A Co2 C13C O14C 172.5(8) . . . . ? O14B Co2 C13C O14C 25.2(11) . . . . ? O15B Co2 C13C O14C 79.7(9) . . . . ? C13B Co2 C13C O14C 56.2(9) . . . . ? N1D Co2 C13C O15C 98.4(9) . . . . ? N1A Co2 C13C O15C -13.3(11) . . . . ? O14B Co2 C13C O15C -160.6(8) . . . . ? O15B Co2 C13C O15C -106.1(9) . . . . ? O14C Co2 C13C O15C 174.2(15) . . . . ? C13B Co2 C13C O15C -129.5(8) . . . . ? N1D Co2 C13C C10C 148(5) . . . . ? O15C Co2 C13C C10C 50(5) . . . . ? N1A Co2 C13C C10C 36(6) . . . . ? O14B Co2 C13C C10C -111(5) . . . . ? O15B Co2 C13C C10C -56(5) . . . . ? O14C Co2 C13C C10C -136(6) . . . . ? C13B Co2 C13C C10C -80(5) . . . . ? C5A C4A C3A C2A -0.7(19) . . . . ? C7A C4A C3A C2A 173.3(14) . . . . ? C3H C4H C7H C8H 23(3) . . . . ? C5H C4H C7H C8H -159(2) . . . . ? C3H C4H C7H C12H -155(2) . . . . ? C5H C4H C7H C12H 23(3) . . . . ? C3B C4B C5B C6B -8(3) . . . . ? C7B C4B C5B C6B 173.0(16) . . . . ? C5B C4B C7B C12B 22(3) . . . . ? C3B C4B C7B C12B -157.0(18) . . . . ? C5B C4B C7B C8B -147.4(19) . . . . ? C3B C4B C7B C8B 33(2) . . . . ? C11C C12C C7C C8C -5(2) . . . . ? C11C C12C C7C C4C -175.5(13) . . . . ? C10A C9A C8A C7A -11(2) . . . . ? C6D N1D C2D C3D -1(3) . . . . ? Co2 N1D C2D C3D -168.1(13) . . . . ? C11D C10D C9D C8D 6(2) . . . . ? C13D C10D C9D C8D 174.4(15) . . . . ? C4G C7G C12G C11G -171.8(15) . . . . ? C8G C7G C12G C11G 16(2) . . . . ? C7G C12G C11G C10G -12(2) . . . . ? C13H C10H C11H C12H -178(2) . . . . ? C9H C10H C11H C12H 1(3) . . . . ? C6F N1F C2F C3F 1(2) . . . . ? Co4 N1F C2F C3F 174.2(12) . . . . ? Co4 O15E C13E O14E -1.9(11) . . . . ? Co4 O15E C13E C10E 165.2(13) . . . . ? Co4 O14E C13E O15E 2.3(13) . . . . ? Co4 O14E C13E C10E -165.8(10) . . . . ? C11E C10E C13E O15E 1(2) . . . . ? C9E C10E C13E O15E -178.8(13) . . . . ? C11E C10E C13E O14E 167.8(12) . . . . ? C9E C10E C13E O14E -11.6(19) . . . . ? C12B C7B C8B C9B 5(3) . . . . ? C4B C7B C8B C9B 174.9(17) . . . . ? C5G C6G N1G C2G 11.1(18) . . . . ? C5G C6G N1G Co4 -178.0(9) . . . . ? N1F Co4 N1G C2G -86.0(12) . . . . ? O14E Co4 N1G C2G 21.9(13) . . . . ? O15H Co4 N1G C2G 178.8(12) . . . . ? O14H Co4 N1G C2G 117.1(12) . . . . ? O15E Co4 N1G C2G 28.8(19) . . . . ? N1F Co4 N1G C6G 104.5(9) . . . . ? O14E Co4 N1G C6G -147.6(9) . . . . ? O15H Co4 N1G C6G 9.3(9) . . . . ? O14H Co4 N1G C6G -52.3(9) . . . . ? O15E Co4 N1G C6G -140.7(11) . . . . ? C6C N1C C2C C3C 7(2) . . . . ? Co1 N1C C2C C3C -179.1(10) . . . . ? C4C C3C C2C N1C 2(2) . . . . ? C2E N1E C6E C5E 7(2) . . . . ? Co3 N1E C6E C5E 177.9(12) . . . . ? C2C N1C C6C C5C -12(2) . . . . ? Co1 N1C C6C C5C 174.8(13) . . . . ? C4C C5C C6C N1C 8(3) . . . . ? C9A C8A C7A C12A 16(2) . . . . ? C9A C8A C7A C4A -171.2(15) . . . . ? C3A C4A C7A C8A -21(2) . . . . ? C5A C4A C7A C8A 152.6(14) . . . . ? C3A C4A C7A C12A 151.6(14) . . . . ? C5A C4A C7A C12A -35(2) . . . . ? N1G C6G C5G C4G -4.6(19) . . . . ? C4A C3A C2A N1A -5.1(19) . . . . ? C6G C5G C4G C7G 175.0(12) . . . . ? C6G C5G C4G C3G -3(2) . . . . ? C12G C7G C4G C5G -21(2) . . . . ? C8G C7G C4G C5G 150.8(14) . . . . ? C12G C7G C4G C3G 156.8(15) . . . . ? C8G C7G C4G C3G -32(2) . . . . ? C2G C3G C4G C5G 3(2) . . . . ? C2G C3G C4G C7G -174.7(14) . . . . ? C10G C9G C8G C7G 11(2) . . . . ? C12G C7G C8G C9G -16(2) . . . . ? C4G C7G C8G C9G 171.7(15) . . . . ? C3F C4F C7F C8F 45(2) . . . . ? C5F C4F C7F C8F -138.0(15) . . . . ? C3F C4F C7F C12F -141.3(17) . . . . ? C5F C4F C7F C12F 36(2) . . . . ? C13E C10E C11E C12E -169.9(14) . . . . ? C9E C10E C11E C12E 10(2) . . . . ? C11C C10C C9C C8C 10(2) . . . . ? C13C C10C C9C C8C -167.9(15) . . . . ? C10D C9D C8D C7D -1(2) . . . . ? C13H C10H C9H C8H 172.3(14) . . . . ? C11H C10H C9H C8H -6(2) . . . . ? C9A C10A C11A C12A 1(2) . . . . ? C13A C10A C11A C12A -170.3(14) . . . . ? C8E C7E C12E C11E 6(3) . . . . ? C4E C7E C12E C11E 173.7(15) . . . . ? C10E C11E C12E C7E -9(3) . . . . ? C5B C4B C3B C2B 2(3) . . . . ? C7B C4B C3B C2B -178.9(16) . . . . ? C11F C10F C9F C8F -4(3) . . . . ? C13F C10F C9F C8F 179.0(14) . . . . ? C8B C7B C12B C11B -5(3) . . . . ? C4B C7B C12B C11B -174.6(15) . . . . ? C12C C7C C8C C9C 6(3) . . . . ? C4C C7C C8C C9C 175.9(14) . . . . ? C10C C9C C8C C7C -8(3) . . . . ? C3A C2A N1A C6A 11.4(17) . . . . ? C3A C2A N1A Co2 179.7(9) . . . . ? N1D Co2 N1A C6A -93.3(11) . . . . ? O15C Co2 N1A C6A 11.7(11) . . . . ? O14B Co2 N1A C6A 171.6(10) . . . . ? O15B Co2 N1A C6A 108.8(10) . . . . ? O14C Co2 N1A C6A 28.6(18) . . . . ? C13C Co2 N1A C6A 18.6(13) . . . . ? C13B Co2 N1A C6A 138.0(11) . . . . ? N1D Co2 N1A C2A 99.9(9) . . . . ? O15C Co2 N1A C2A -155.1(8) . . . . ? O14B Co2 N1A C2A 4.8(9) . . . . ? O15B Co2 N1A C2A -58.0(9) . . . . ? O14C Co2 N1A C2A -138.2(10) . . . . ? C13C Co2 N1A C2A -148.2(8) . . . . ? C13B Co2 N1A C2A -28.9(9) . . . . ? C12H C7H C8H C9H -3(3) . . . . ? C4H C7H C8H C9H 178.7(16) . . . . ? C10H C9H C8H C7H 8(3) . . . . ? C10D C11D C12D C7D -5(3) . . . . ? C2C C3C C4C C5C -6(2) . . . . ? C2C C3C C4C C7C -177.0(13) . . . . ? C6C C5C C4C C3C 1(2) . . . . ? C6C C5C C4C C7C 172.7(15) . . . . ? C8C C7C C4C C3C -28(2) . . . . ? C12C C7C C4C C3C 142.4(16) . . . . ? C8C C7C C4C C5C 160.9(17) . . . . ? C12C C7C C4C C5C -29(2) . . . . ? N1F C2F C3F C4F -10(2) . . . . ? C7F C4F C3F C2F -169.4(14) . . . . ? C5F C4F C3F C2F 13(2) . . . . ? C6G N1G C2G C3G -12(2) . . . . ? Co4 N1G C2G C3G 178.6(13) . . . . ? C4G C3G C2G N1G 5(3) . . . . ? C7B C12B C11B C10B 8(2) . . . . ? C9B C10B C11B C12B -12(2) . . . . ? C13B C10B C11B C12B 174.0(12) . . . . ? C10H C11H C12H C7H 4(4) . . . . ? C8H C7H C12H C11H -2(3) . . . . ? C4H C7H C12H C11H 175.8(19) . . . . ? C3H C2H N1H C6H -2(3) . . . . ? C3H C2H N1H Co1 -171.2(16) . . . 7_755 ? C12F C7F C8F C9F -4(3) . . . . ? C4F C7F C8F C9F 170.8(16) . . . . ? C10F C9F C8F C7F 5(3) . . . . ? C2D N1D C6D C5D -4(4) . . . . ? Co2 N1D C6D C5D 163(2) . . . . ? C5H C4H C3H C2H 1(3) . . . . ? C7H C4H C3H C2H 179.2(17) . . . . ? N1H C2H C3H C4H 0(3) . . . . ? C3H C4H C5H C6H -1(3) . . . . ? C7H C4H C5H C6H -179(2) . . . . ? C3D C4D C5D C6D -15(4) . . . . ? C7D C4D C5D C6D 175(2) . . . . ? N1D C6D C5D C4D 12(5) . . . . ? C2B N1B C6B C5B -4(2) . . . . ? Co3 N1B C6B C5B -177.3(12) 7_755 . . . ? C4B C5B C6B N1B 9(3) . . . . ? C6B N1B C2B C3B -2(2) . . . . ? Co3 N1B C2B C3B 170.8(11) 7_755 . . . ? C4B C3B C2B N1B 3(2) . . . . ? C9F C10F C11F C12F 2(3) . . . . ? C13F C10F C11F C12F 178.8(18) . . . . ? CK4 NK3 CK2 OK1 -9(3) . . . . ? CK5 NK3 CK2 OK1 -177.9(17) . . . . ? CM4 NM3 CM2 OM1 2(3) . . . . ? CM5 NM3 CM2 OM1 -177.3(19) . . . . ? C11D C12D C7D C8D 11(3) . . . . ? C11D C12D C7D C4D 177.7(17) . . . . ? C9D C8D C7D C12D -8(3) . . . . ? C9D C8D C7D C4D -174.8(15) . . . . ? C5D C4D C7D C12D 10(3) . . . . ? C3D C4D C7D C12D -159.6(17) . . . . ? C5D C4D C7D C8D 178(2) . . . . ? C3D C4D C7D C8D 8(2) . . . . ? C11B C10B C9B C8B 13(3) . . . . ? C13B C10B C9B C8B -173.4(16) . . . . ? C7B C8B C9B C10B -10(3) . . . . ? C3E C4E C5E C6E -3(3) . . . . ? C7E C4E C5E C6E -178.4(14) . . . . ? N1E C6E C5E C4E -1(2) . . . . ? C10A C11A C12A C7A 4(2) . . . . ? C8A C7A C12A C11A -13(2) . . . . ? C4A C7A C12A C11A 173.9(15) . . . . ? C10F C11F C12F C7F -1(3) . . . . ? C8F C7F C12F C11F 1(3) . . . . ? C4F C7F C12F C11F -173.0(19) . . . . ? C4A C5A C6A N1A 8(2) . . . . ? C2A N1A C6A C5A -13.4(19) . . . . ? Co2 N1A C6A C5A 179.4(11) . . . . ? N1D C2D C3D C4D -2(3) . . . . ? C5D C4D C3D C2D 11(3) . . . . ? C7D C4D C3D C2D -178.9(16) . . . . ? C8G C9G C10G C11G -6(2) . . . . ? C8G C9G C10G C13G -178.1(14) . . . . ? C12G C11G C10G C9G 7(3) . . . . ? C12G C11G C10G C13G 179.1(15) . . . . ? C9G C10G C13G O15G 169.2(14) . . . . ? C11G C10G C13G O15G -3(2) . . . . ? C9G C10G C13G O14G -11(2) . . . . ? C11G C10G C13G O14G 176.6(14) . . . . ? C9G C10G C13G Co1 91(6) . . . 1_665 ? C11G C10G C13G Co1 -82(6) . . . 1_665 ? O14G C13G O15G Co1 12.6(15) . . . 1_665 ? C10G C13G O15G Co1 -167.7(12) . . . 1_665 ? O15G C13G O14G Co1 -11.8(14) . . . 1_665 ? C10G C13G O14G Co1 168.4(12) . . . 1_665 ? CJ5 NJ3 CJ2 OJ1 1(4) . . . . ? CJ4 NJ3 CJ2 OJ1 -180(3) . . . . ? OL1 CL2 NL3 CL5 -167(3) . . . . ? OL1 CL2 NL3 CL4 5(5) . . . . ? C2H N1H C6H C5H 2(3) . . . . ? Co1 N1H C6H C5H 170.7(17) 7_755 . . . ? C4H C5H C6H N1H -1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.34 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.756 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.103 data_3 _database_code_depnum_ccdc_archive 'CCDC 850073' #TrackingRef '- DT-ART-10-2011-012016 CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108.80 H98.70 N11.60 Ni4 O22.35' _chemical_formula_weight 2161.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 31.8199(19) _cell_length_b 31.8199(19) _cell_length_c 25.1149(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 25429(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 31528 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 28.29 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8988 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8297 _exptl_absorpt_correction_T_max 0.8551 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type diffractometer _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90225 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.29 _reflns_number_total 31528 _reflns_number_gt 17450 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Pseudosymmetry is present in the form of a non-crystallographic inversion centre. ADDSYM was used to establish that the space group is correct. Guest atoms are refined isotropically, except for nitrogen and oxygen atoms on DMF and Ethanol. The low site occupancies of the solvent molecules prevented anisotropic refinement. Further solvent accessible voids are present, but analytical data matches the solvent model presented. Further disorder may be present. 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^)+(0.1848P)^2^+492.4306P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(3) _refine_ls_number_reflns 31528 _refine_ls_number_parameters 1268 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.2020 _refine_ls_R_factor_gt 0.1397 _refine_ls_wR_factor_ref 0.4313 _refine_ls_wR_factor_gt 0.3935 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.019 _refine_ls_shift/su_mean 0.009 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 0.98670(4) 0.24245(4) 0.14040(12) 0.0260(3) Uani 1 1 d . . . Ni2 Ni 1.24329(5) 0.48525(4) -0.10703(11) 0.0268(3) Uani 1 1 d . . . Ni3 Ni 1.48493(4) 0.74418(4) 0.14029(12) 0.0268(3) Uani 1 1 d . . . Ni4 Ni 1.74338(5) 0.98623(4) -0.10882(12) 0.0270(3) Uani 1 1 d . . . N1A N 1.5295(3) 0.7748(3) 0.0986(4) 0.029(2) Uani 1 1 d . . . C2A C 1.5704(3) 0.7770(4) 0.1155(5) 0.031(2) Uani 1 1 d . . . H2A H 1.5770 0.7647 0.1489 0.037 Uiso 1 1 calc R . . C3A C 1.6033(4) 0.7963(5) 0.0871(5) 0.047(3) Uani 1 1 d . . . H3A H 1.6314 0.7963 0.0997 0.056 Uiso 1 1 calc R . . C4A C 1.5915(4) 0.8162(4) 0.0372(5) 0.030(2) Uani 1 1 d . . . C5A C 1.5510(4) 0.8146(4) 0.0202(5) 0.036(3) Uani 1 1 d . . . H5A H 1.5428 0.8276 -0.0122 0.043 Uiso 1 1 calc R . . C6A C 1.5217(4) 0.7933(4) 0.0516(4) 0.032(3) Uani 1 1 d . . . H6A H 1.4937 0.7917 0.0385 0.038 Uiso 1 1 calc R . . C7A C 1.6234(4) 0.8407(4) 0.0069(4) 0.032(3) Uani 1 1 d . . . C8A C 1.6591(4) 0.8575(4) 0.0326(5) 0.039(3) Uani 1 1 d . . . H8A H 1.6645 0.8500 0.0685 0.047 Uiso 1 1 calc R . . C9A C 1.6866(4) 0.8847(4) 0.0067(5) 0.030(2) Uani 1 1 d . . . H9A H 1.7088 0.8982 0.0255 0.036 Uiso 1 1 calc R . . C10A C 1.6806(4) 0.8917(4) -0.0476(5) 0.031(2) Uani 1 1 d . . . C11A C 1.6485(4) 0.8743(4) -0.0744(5) 0.041(3) Uani 1 1 d . . . H11A H 1.6451 0.8797 -0.1114 0.050 Uiso 1 1 calc R . . C12A C 1.6190(4) 0.8472(5) -0.0470(5) 0.046(4) Uani 1 1 d . . . H12A H 1.5968 0.8341 -0.0660 0.055 Uiso 1 1 calc R . . C13A C 1.7078(4) 0.9246(4) -0.0738(4) 0.030(2) Uani 1 1 d . . . O14A O 1.7330(2) 0.9456(2) -0.0469(3) 0.0270(16) Uani 1 1 d . . . O15A O 1.7034(3) 0.9311(3) -0.1237(3) 0.034(2) Uani 1 1 d . . . N1B N 1.5412(3) 1.2048(3) -0.3275(4) 0.026(2) Uani 1 1 d . . . C2B C 1.5350(4) 1.1991(4) -0.2741(5) 0.038(3) Uani 1 1 d . . . H2B H 1.5149 1.2152 -0.2551 0.045 Uiso 1 1 calc R . . C3B C 1.5597(4) 1.1683(4) -0.2484(5) 0.037(3) Uani 1 1 d . . . H3B H 1.5566 1.1648 -0.2110 0.044 Uiso 1 1 calc R . . C4B C 1.5877(4) 1.1435(4) -0.2743(5) 0.039(3) Uani 1 1 d . . . C5B C 1.5910(5) 1.1490(6) -0.3280(6) 0.066(5) Uani 1 1 d . . . H5B H 1.6096 1.1317 -0.3479 0.079 Uiso 1 1 calc R . . C6B C 1.5675(5) 1.1796(4) -0.3539(7) 0.058(4) Uani 1 1 d . . . H6B H 1.5702 1.1827 -0.3913 0.069 Uiso 1 1 calc R . . C7B C 1.6108(4) 1.1123(5) -0.2441(5) 0.043(3) Uani 1 1 d . . . C8B C 1.6002(4) 1.0959(5) -0.1962(6) 0.048(4) Uani 1 1 d . . . H8B H 1.5733 1.1024 -0.1821 0.058 Uiso 1 1 calc R . . C9B C 1.6258(4) 1.0707(5) -0.1674(6) 0.050(4) Uani 1 1 d . . . H9B H 1.6164 1.0607 -0.1337 0.060 Uiso 1 1 calc R . . C10B C 1.6653(4) 1.0591(4) -0.1857(5) 0.036(3) Uani 1 1 d . . . C11B C 1.6782(4) 1.0742(4) -0.2350(5) 0.038(3) Uani 1 1 d . . . H11B H 1.7043 1.0656 -0.2498 0.046 Uiso 1 1 calc R . . C12B C 1.6523(5) 1.1024(5) -0.2627(5) 0.055(5) Uani 1 1 d . . . H12B H 1.6624 1.1151 -0.2945 0.066 Uiso 1 1 calc R . . C13B C 1.6938(4) 1.0317(3) -0.1531(4) 0.031(3) Uani 1 1 d . . . O14B O 1.6854(3) 1.0217(2) -0.1052(3) 0.0331(18) Uani 1 1 d . . . O15B O 1.7293(2) 1.0219(2) -0.1731(3) 0.0298(17) Uani 1 1 d . . . N1C N 1.7747(3) 1.0311(3) -0.0670(4) 0.033(2) Uani 1 1 d . . . C2C C 1.7926(5) 1.0225(4) -0.0202(5) 0.043(3) Uani 1 1 d . . . H2C H 1.7915 0.9944 -0.0078 0.052 Uiso 1 1 calc R . . C3C C 1.8132(5) 1.0526(4) 0.0122(6) 0.045(3) Uani 1 1 d . . . H3C H 1.8246 1.0450 0.0458 0.053 Uiso 1 1 calc R . . C4C C 1.8160(4) 1.0928(4) -0.0061(5) 0.032(3) Uani 1 1 d . . . C5C C 1.7973(4) 1.1042(4) -0.0549(5) 0.035(3) Uani 1 1 d . . . H5C H 1.7979 1.1322 -0.0678 0.042 Uiso 1 1 calc R . . C6C C 1.7772(4) 1.0707(4) -0.0837(5) 0.032(3) Uani 1 1 d . . . H6C H 1.7648 1.0773 -0.1171 0.038 Uiso 1 1 calc R . . C7C C 1.8403(5) 1.1243(4) 0.0251(5) 0.043(3) Uani 1 1 d . . . C8C C 1.8458(6) 1.1197(5) 0.0791(6) 0.066(5) Uani 1 1 d . . . H8C H 1.8316 1.0982 0.0983 0.079 Uiso 1 1 calc R . . C9C C 1.8736(5) 1.1481(5) 0.1056(5) 0.049(4) Uani 1 1 d . . . H9C H 1.8798 1.1442 0.1422 0.059 Uiso 1 1 calc R . . C10C C 1.8910(4) 1.1808(4) 0.0789(5) 0.035(3) Uani 1 1 d . . . C11C C 1.8836(4) 1.1872(4) 0.0260(5) 0.036(3) Uani 1 1 d . . . H11C H 1.8965 1.2099 0.0077 0.043 Uiso 1 1 calc R . . C12C C 1.8562(4) 1.1591(4) -0.0012(5) 0.035(3) Uani 1 1 d . . . H12C H 1.8489 1.1642 -0.0373 0.042 Uiso 1 1 calc R . . C13C C 1.9244(4) 1.2072(4) 0.1053(5) 0.033(3) Uani 1 1 d . . . O14C O 1.9314(3) 1.2036(3) 0.1555(3) 0.043(2) Uani 1 1 d . . . O15C O 1.9458(2) 1.2324(2) 0.0786(3) 0.0260(16) Uani 1 1 d . . . N1D N 1.7959(3) 0.9582(3) -0.1420(4) 0.030(2) Uani 1 1 d . . . C2D C 1.8184(5) 0.9300(5) -0.1170(5) 0.057(5) Uani 1 1 d . . . H2D H 1.8131 0.9250 -0.0803 0.068 Uiso 1 1 calc R . . C3D C 1.8486(5) 0.9080(4) -0.1414(6) 0.054(4) Uani 1 1 d . . . H3D H 1.8651 0.8890 -0.1210 0.064 Uiso 1 1 calc R . . C4D C 1.8567(4) 0.9119(4) -0.1953(5) 0.039(3) Uani 1 1 d . . . C5D C 1.8328(4) 0.9394(4) -0.2216(4) 0.030(3) Uani 1 1 d . . . H5D H 1.8363 0.9431 -0.2589 0.036 Uiso 1 1 calc R . . C6D C 1.8015(4) 0.9637(4) -0.1933(5) 0.038(3) Uani 1 1 d . . . H6D H 1.7850 0.9838 -0.2119 0.046 Uiso 1 1 calc R . . C7D C 1.8883(4) 0.8877(4) -0.2254(5) 0.039(3) Uani 1 1 d . . . C8D C 1.9060(4) 0.9009(4) -0.2708(5) 0.042(3) Uani 1 1 d . . . H8D H 1.8992 0.9279 -0.2846 0.051 Uiso 1 1 calc R . . C9D C 1.9348(4) 0.8745(4) -0.2982(6) 0.044(3) Uani 1 1 d . . . H9D H 1.9498 0.8856 -0.3277 0.053 Uiso 1 1 calc R . . C10D C 1.9414(4) 0.8344(4) -0.2836(5) 0.033(3) Uani 1 1 d . . . C11D C 1.9230(4) 0.8202(5) -0.2351(6) 0.042(3) Uiso 1 1 d . . . H11D H 1.9302 0.7933 -0.2214 0.050 Uiso 1 1 calc R . . C12D C 1.8952(5) 0.8447(4) -0.2083(6) 0.048(4) Uani 1 1 d . . . H12D H 1.8805 0.8338 -0.1785 0.058 Uiso 1 1 calc R . . C13D C 1.9691(4) 0.8052(4) -0.3159(5) 0.037(3) Uani 1 1 d . . . O14D O 1.9806(2) 0.8153(3) -0.3611(4) 0.0385(19) Uani 1 1 d . . . O15D O 1.9792(2) 0.7704(3) -0.2960(3) 0.0307(17) Uani 1 1 d . . . N1E N 1.2728(3) 0.5312(3) -0.0651(4) 0.030(2) Uani 1 1 d . . . C2E C 1.2761(4) 0.5710(4) -0.0840(5) 0.036(3) Uani 1 1 d . . . H2E H 1.2639 0.5769 -0.1177 0.043 Uiso 1 1 calc R . . C3E C 1.2960(4) 0.6039(4) -0.0571(5) 0.038(3) Uani 1 1 d . . . H3E H 1.2981 0.6310 -0.0728 0.046 Uiso 1 1 calc R . . C4E C 1.3129(4) 0.5960(4) -0.0064(4) 0.028(2) Uani 1 1 d . . . C5E C 1.3076(4) 0.5538(4) 0.0128(5) 0.035(3) Uani 1 1 d . . . H5E H 1.3174 0.5466 0.0473 0.042 Uiso 1 1 calc R . . C6E C 1.2889(4) 0.5245(4) -0.0172(5) 0.037(3) Uani 1 1 d . . . H6E H 1.2870 0.4968 -0.0031 0.045 Uiso 1 1 calc R . . C7E C 1.3363(4) 0.6281(4) 0.0236(4) 0.034(3) Uani 1 1 d . . . C8E C 1.3413(4) 0.6251(5) 0.0778(5) 0.044(3) Uani 1 1 d . . . H8E H 1.3263 0.6043 0.0972 0.053 Uiso 1 1 calc R . . C9E C 1.3690(5) 0.6531(5) 0.1053(5) 0.054(4) Uani 1 1 d . . . H9E H 1.3735 0.6498 0.1425 0.065 Uiso 1 1 calc R . . C10E C 1.3891(4) 0.6844(4) 0.0785(4) 0.030(3) Uani 1 1 d . . . C11E C 1.3824(3) 0.6885(4) 0.0243(4) 0.029(2) Uani 1 1 d . . . H11E H 1.3968 0.7098 0.0051 0.035 Uiso 1 1 calc R . . C12E C 1.3547(4) 0.6618(4) -0.0030(4) 0.031(2) Uani 1 1 d . . . H12E H 1.3485 0.6668 -0.0395 0.037 Uiso 1 1 calc R . . C13E C 1.4218(3) 0.7098(4) 0.1070(5) 0.028(2) Uani 1 1 d . . . O14E O 1.4443(2) 0.7345(2) 0.0793(3) 0.0268(16) Uani 1 1 d . . . O15E O 1.4286(3) 0.7057(3) 0.1549(3) 0.044(2) Uani 1 1 d . . . N1F N 1.0410(3) 0.7031(3) -0.3266(4) 0.028(2) Uani 1 1 d . . . C2F C 1.0639(4) 0.6746(4) -0.3533(6) 0.049(3) Uani 1 1 d . . . H2F H 1.0654 0.6771 -0.3910 0.059 Uiso 1 1 calc R . . C3F C 1.0856(4) 0.6420(5) -0.3297(5) 0.047(4) Uani 1 1 d . . . H3F H 1.1005 0.6220 -0.3506 0.057 Uiso 1 1 calc R . . C4F C 1.0848(4) 0.6390(4) -0.2731(6) 0.044(3) Uani 1 1 d . . . C5F C 1.0597(4) 0.6655(4) -0.2485(5) 0.036(3) Uani 1 1 d . . . H5F H 1.0563 0.6629 -0.2110 0.043 Uiso 1 1 calc R . . C6F C 1.0381(4) 0.6967(4) -0.2748(5) 0.035(3) Uani 1 1 d . . . H6F H 1.0203 0.7146 -0.2546 0.042 Uiso 1 1 calc R . . C7F C 1.1100(4) 0.6069(4) -0.2451(5) 0.041(3) Uani 1 1 d . . . C8F C 1.1501(5) 0.5982(5) -0.2631(6) 0.056(4) Uani 1 1 d . . . H8F H 1.1594 0.6094 -0.2962 0.068 Uiso 1 1 calc R . . C9F C 1.1774(5) 0.5726(4) -0.2326(6) 0.048(4) Uani 1 1 d . . . H9F H 1.2053 0.5672 -0.2442 0.058 Uiso 1 1 calc R . . C10F C 1.1629(4) 0.5559(4) -0.1862(5) 0.040(3) Uani 1 1 d . . . C11F C 1.1213(4) 0.5618(4) -0.1699(5) 0.038(3) Uani 1 1 d . . . H11F H 1.1108 0.5480 -0.1391 0.045 Uiso 1 1 calc R . . C12F C 1.0957(4) 0.5882(4) -0.1994(5) 0.034(3) Uani 1 1 d . . . H12F H 1.0678 0.5933 -0.1879 0.041 Uiso 1 1 calc R . . C13F C 1.1924(4) 0.5298(3) -0.1529(4) 0.029(2) Uani 1 1 d . . . O14F O 1.2278(3) 0.5203(2) -0.1719(3) 0.0320(18) Uani 1 1 d . . . O15F O 1.1821(3) 0.5175(3) -0.1060(3) 0.0353(19) Uani 1 1 d . . . N1G N 1.0314(3) 0.2734(3) 0.0996(4) 0.027(2) Uani 1 1 d . . . C2G C 1.0245(4) 0.2891(5) 0.0511(5) 0.040(3) Uani 1 1 d . . . H2G H 0.9968 0.2870 0.0373 0.048 Uiso 1 1 calc R . . C3G C 1.0547(4) 0.3085(4) 0.0188(5) 0.037(3) Uani 1 1 d . . . H3G H 1.0480 0.3186 -0.0158 0.044 Uiso 1 1 calc R . . C4G C 1.0964(4) 0.3124(3) 0.0406(4) 0.028(2) Uani 1 1 d . . . C5G C 1.1047(4) 0.2965(4) 0.0899(5) 0.037(3) Uani 1 1 d . . . H5G H 1.1320 0.2988 0.1050 0.045 Uiso 1 1 calc R . . C6G C 1.0717(4) 0.2764(4) 0.1183(5) 0.035(3) Uani 1 1 d . . . H6G H 1.0780 0.2645 0.1521 0.043 Uiso 1 1 calc R . . C7G C 1.1288(4) 0.3358(4) 0.0097(5) 0.037(3) Uani 1 1 d . . . C8G C 1.1253(5) 0.3396(4) -0.0453(5) 0.046(3) Uani 1 1 d . . . H8G H 1.1044 0.3246 -0.0645 0.056 Uiso 1 1 calc R . . C9G C 1.1538(5) 0.3663(5) -0.0716(5) 0.056(4) Uani 1 1 d . . . H9G H 1.1522 0.3686 -0.1092 0.067 Uiso 1 1 calc R . . C10G C 1.1840(4) 0.3892(4) -0.0449(4) 0.029(2) Uani 1 1 d . . . C11G C 1.1884(4) 0.3830(4) 0.0086(4) 0.029(2) Uani 1 1 d . . . H11G H 1.2096 0.3978 0.0275 0.035 Uiso 1 1 calc R . . C12G C 1.1615(3) 0.3546(4) 0.0365(4) 0.027(2) Uani 1 1 d . . . H12G H 1.1661 0.3489 0.0732 0.033 Uiso 1 1 calc R . . C13G C 1.2101(4) 0.4225(4) -0.0727(4) 0.030(2) Uani 1 1 d . . . O14G O 1.2057(3) 0.4278(3) -0.1221(3) 0.040(2) Uani 1 1 d . . . O15G O 1.2338(2) 0.4442(2) -0.0446(3) 0.0255(16) Uani 1 1 d . . . N1H N 1.2040(3) 0.0405(3) 0.3614(4) 0.029(2) Uani 1 1 d . . . C2H C 1.1995(4) 0.0370(4) 0.3077(5) 0.041(3) Uani 1 1 d . . . H2H H 1.2180 0.0196 0.2879 0.049 Uiso 1 1 calc R . . C3H C 1.1670(4) 0.0596(4) 0.2814(5) 0.034(3) Uani 1 1 d . . . H3H H 1.1642 0.0573 0.2439 0.041 Uiso 1 1 calc R . . C4H C 1.1406(4) 0.0838(4) 0.3080(5) 0.037(3) Uani 1 1 d . . . C5H C 1.1417(5) 0.0853(4) 0.3638(5) 0.046(4) Uani 1 1 d . . . H5H H 1.1217 0.1006 0.3841 0.055 Uiso 1 1 calc R . . C6H C 1.1759(4) 0.0619(4) 0.3880(6) 0.046(3) Uani 1 1 d . . . H6H H 1.1779 0.0621 0.4257 0.056 Uiso 1 1 calc R . . C7H C 1.1071(4) 0.1088(4) 0.2804(5) 0.039(3) Uani 1 1 d . . . C8H C 1.0897(5) 0.0968(4) 0.2320(5) 0.044(3) Uani 1 1 d . . . H8H H 1.0949 0.0692 0.2194 0.052 Uiso 1 1 calc R . . C9H C 1.0661(5) 0.1221(4) 0.2024(5) 0.049(4) Uani 1 1 d . . . H9H H 1.0560 0.1123 0.1690 0.058 Uiso 1 1 calc R . . C11H C 1.0707(4) 0.1758(4) 0.2701(5) 0.031(3) Uani 1 1 d . . . H11H H 1.0622 0.2021 0.2846 0.037 Uiso 1 1 calc R . . C12H C 1.0980(4) 0.1496(4) 0.2992(5) 0.041(3) Uani 1 1 d . . . H12H H 1.1102 0.1594 0.3314 0.049 Uiso 1 1 calc R . . C13H C 1.0314(3) 0.1922(4) 0.1863(4) 0.027(2) Uani 1 1 d . . . O14H O 1.0217(2) 0.2280(3) 0.2070(3) 0.0286(17) Uani 1 1 d . . . O15H O 1.0209(2) 0.1819(2) 0.1402(4) 0.0345(17) Uani 1 1 d . . . O1J O 1.1876(4) 0.1842(5) 0.3615(5) 0.095(5) Uiso 1 1 d D . . C2J C 1.2134(5) 0.1616(6) 0.3386(4) 0.088(6) Uiso 1 1 d D . . H2J H 1.2305 0.1439 0.3599 0.105 Uiso 1 1 calc R . . N3J N 1.2187(4) 0.1603(4) 0.2864(4) 0.074(4) Uiso 1 1 d D . . C4J C 1.2507(5) 0.1330(5) 0.2639(6) 0.072(5) Uiso 1 1 d D . . H4J1 H 1.2720 0.1269 0.2910 0.109 Uiso 1 1 calc R . . H4J2 H 1.2640 0.1470 0.2335 0.109 Uiso 1 1 calc R . . H4J3 H 1.2378 0.1067 0.2520 0.109 Uiso 1 1 calc R . . C5J C 1.1968(7) 0.1897(7) 0.2523(6) 0.111(8) Uiso 1 1 d D . . H5J1 H 1.1734 0.2024 0.2720 0.167 Uiso 1 1 calc R . . H5J2 H 1.1858 0.1749 0.2211 0.167 Uiso 1 1 calc R . . H5J3 H 1.2162 0.2118 0.2407 0.167 Uiso 1 1 calc R . . O1K O 1.6954(6) 0.8084(5) 0.1472(8) 0.110(6) Uiso 0.85 1 d PD . . C2K C 1.7299(6) 0.8056(5) 0.1255(11) 0.098(8) Uiso 0.85 1 d PD . . H2K H 1.7460 0.8306 0.1225 0.118 Uiso 0.85 1 calc PR . . N3K N 1.7463(6) 0.7709(6) 0.1061(11) 0.128(9) Uiso 0.85 1 d PD . . C4K C 1.7238(9) 0.7315(5) 0.1084(12) 0.109(10) Uiso 0.85 1 d PD . . H4K1 H 1.7077 0.7301 0.1416 0.164 Uiso 0.85 1 calc PR . . H4K2 H 1.7438 0.7081 0.1071 0.164 Uiso 0.85 1 calc PR . . H4K3 H 1.7045 0.7296 0.0781 0.164 Uiso 0.85 1 calc PR . . O1L O 1.6880(4) 0.8157(4) -0.3269(5) 0.091(4) Uiso 1 1 d D . . C2L C 1.7141(5) 0.8383(6) -0.3049(4) 0.089(6) Uiso 1 1 d D . . H2L H 1.7302 0.8567 -0.3268 0.107 Uiso 1 1 calc R . . N3L N 1.7214(4) 0.8390(4) -0.2531(4) 0.066(4) Uiso 1 1 d D . . C4L C 1.7008(9) 0.8093(8) -0.2182(6) 0.141(11) Uiso 1 1 d D . . H4L1 H 1.6817 0.8243 -0.1943 0.211 Uiso 1 1 calc R . . H4L2 H 1.7220 0.7943 -0.1972 0.211 Uiso 1 1 calc R . . H4L3 H 1.6848 0.7891 -0.2396 0.211 Uiso 1 1 calc R . . C5L C 1.7543(5) 0.8656(6) -0.2318(6) 0.079(6) Uiso 1 1 d D . . H5L1 H 1.7683 0.8804 -0.2610 0.119 Uiso 1 1 calc R . . H5L2 H 1.7748 0.8483 -0.2128 0.119 Uiso 1 1 calc R . . H5L3 H 1.7420 0.8861 -0.2072 0.119 Uiso 1 1 calc R . . O1M O 1.8075(5) 1.1990(6) -0.1116(8) 0.100(6) Uiso 0.75 1 d PD . . C2M C 1.8037(5) 1.2333(6) -0.0896(10) 0.073(7) Uiso 0.75 1 d PD . . H2M H 1.8275 1.2515 -0.0896 0.087 Uiso 0.75 1 calc PR . . N3M N 1.7692(5) 1.2468(6) -0.0662(10) 0.103(8) Uiso 0.75 1 d PD . . C4M C 1.7306(5) 1.2232(8) -0.0697(11) 0.094(9) Uiso 0.75 1 d PD . . H4M1 H 1.7362 1.1956 -0.0854 0.141 Uiso 0.75 1 calc PR . . H4M2 H 1.7105 1.2385 -0.0921 0.141 Uiso 0.75 1 calc PR . . H4M3 H 1.7187 1.2196 -0.0339 0.141 Uiso 0.75 1 calc PR . . C5M C 1.7670(8) 1.2887(6) -0.0442(13) 0.108(11) Uiso 0.75 1 d PD . . H5M1 H 1.7933 1.2952 -0.0257 0.161 Uiso 0.75 1 calc PR . . H5M2 H 1.7435 1.2904 -0.0190 0.161 Uiso 0.75 1 calc PR . . H5M3 H 1.7626 1.3090 -0.0730 0.161 Uiso 0.75 1 calc PR . . O1N O 1.034(2) 0.601(2) -0.0068(17) 0.10(2) Uiso 0.25 1 d PD . . C2N C 1.0204(18) 0.5975(16) -0.0609(16) 0.046(13) Uiso 0.25 1 d PD . . H2N1 H 1.0301 0.6245 -0.0762 0.055 Uiso 0.25 1 calc PR . . H2N2 H 0.9896 0.6006 -0.0575 0.055 Uiso 0.25 1 calc PR . . C3N C 1.0245(19) 0.5674(17) -0.1087(19) 0.053(13) Uiso 0.25 1 d PD . . H3N1 H 1.0499 0.5744 -0.1290 0.079 Uiso 0.25 1 calc PR . . H3N2 H 0.9998 0.5703 -0.1317 0.079 Uiso 0.25 1 calc PR . . H3N3 H 1.0265 0.5384 -0.0958 0.079 Uiso 0.25 1 calc PR . . C2O C 1.674(2) 0.7688(16) 0.3033(16) 0.08(2) Uiso 0.25 1 d PD . . H2O1 H 1.7017 0.7740 0.3190 0.096 Uiso 0.25 1 calc PR . . H2O2 H 1.6610 0.7971 0.2995 0.096 Uiso 0.25 1 calc PR . . C3O C 1.685(2) 0.758(2) 0.2452(15) 0.072(19) Uiso 0.25 1 d PD . . H3O1 H 1.6618 0.7417 0.2293 0.107 Uiso 0.25 1 calc PR . . H3O2 H 1.7107 0.7412 0.2445 0.107 Uiso 0.25 1 calc PR . . H3O3 H 1.6890 0.7839 0.2249 0.107 Uiso 0.25 1 calc PR . . O1W O 1.961(2) 1.084(2) 0.041(3) 0.11(2) Uiso 0.25 1 d P . . O3W O 1.9826(16) 0.8978(16) -0.136(2) 0.071(13) Uiso 0.25 1 d P . . C2Q C 0.9098(18) 0.527(3) -0.0252(13) 0.09(2) Uiso 0.25 1 d PD . . H2Q1 H 0.9388 0.5379 -0.0246 0.104 Uiso 0.25 1 calc PR . . H2Q2 H 0.9132 0.4958 -0.0230 0.104 Uiso 0.25 1 calc PR . . O4W O 1.6430(18) 0.7486(18) -0.310(2) 0.085(16) Uiso 0.25 1 d P . . O6W O 1.054(2) 0.472(2) -0.375(3) 0.13(3) Uiso 0.25 1 d P . . C5K C 1.7835(9) 0.7627(9) 0.0858(14) 0.128(12) Uiso 0.85 1 d PD . . H5K1 H 1.7914 0.7851 0.0609 0.193 Uiso 0.85 1 calc PR . . H5K2 H 1.7826 0.7358 0.0669 0.193 Uiso 0.85 1 calc PR . . H5K3 H 1.8044 0.7612 0.1145 0.193 Uiso 0.85 1 calc PR . . C10H C 1.0557(4) 0.1632(4) 0.2192(5) 0.032(3) Uani 1 1 d . . . O1Q O 0.8985(13) 0.5322(13) -0.0799(12) 0.052(10) Uiso 0.25 1 d PD . . O1O O 1.6510(10) 0.7522(11) 0.3478(12) 0.037(7) Uiso 0.25 1 d PD . . O5W O 1.0929(16) 0.5638(16) -0.422(2) 0.073(13) Uiso 0.25 1 d P . . C3Q C 0.894(2) 0.537(2) 0.0313(13) 0.061(16) Uiso 0.25 1 d PD . . H3Q1 H 0.8755 0.5617 0.0297 0.091 Uiso 0.25 1 calc PR . . H3Q2 H 0.9185 0.5440 0.0540 0.091 Uiso 0.25 1 calc PR . . H3Q3 H 0.8792 0.5132 0.0461 0.091 Uiso 0.25 1 calc PR . . O2W O 1.986(7) 0.986(13) -0.264(3) 0.21(6) Uiso 0.25 1 d P . . O7W O 1.026(3) 0.061(3) 0.353(3) 0.14(3) Uiso 0.25 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 0.0267(7) 0.0314(7) 0.0198(6) 0.0001(7) -0.0102(6) 0.0001(5) Ni2 0.0338(8) 0.0268(7) 0.0198(8) -0.0121(6) 0.0003(6) -0.0016(6) Ni3 0.0250(7) 0.0353(7) 0.0200(6) -0.0012(7) -0.0085(6) -0.0002(6) Ni4 0.0343(8) 0.0265(7) 0.0201(8) -0.0090(6) 0.0012(7) -0.0013(6) N1A 0.026(5) 0.032(5) 0.030(5) 0.001(4) -0.009(4) -0.004(4) C2A 0.017(5) 0.037(6) 0.038(6) 0.002(5) 0.000(4) 0.003(5) C3A 0.030(7) 0.073(10) 0.036(7) 0.007(7) -0.003(5) -0.005(7) C4A 0.033(6) 0.025(6) 0.033(6) 0.001(5) 0.001(5) -0.016(5) C5A 0.020(5) 0.057(8) 0.031(6) 0.003(6) -0.006(5) -0.001(5) C6A 0.029(6) 0.046(7) 0.021(5) -0.004(5) 0.006(4) 0.002(5) C7A 0.037(6) 0.036(6) 0.023(5) 0.009(5) -0.012(5) -0.008(5) C8A 0.036(7) 0.056(8) 0.025(6) 0.003(5) 0.009(5) -0.025(6) C9A 0.028(6) 0.029(6) 0.034(6) -0.001(5) -0.003(5) -0.007(5) C10A 0.030(6) 0.036(6) 0.028(6) 0.000(5) -0.003(5) -0.012(5) C11A 0.054(8) 0.045(7) 0.026(6) 0.003(5) -0.010(5) -0.020(6) C12A 0.038(7) 0.085(11) 0.016(5) 0.003(6) 0.003(5) -0.009(7) C13A 0.039(6) 0.030(6) 0.021(5) 0.001(5) -0.002(5) 0.010(5) O14A 0.030(4) 0.024(4) 0.027(4) -0.003(3) -0.007(3) -0.010(3) O15A 0.047(5) 0.038(5) 0.018(4) -0.010(3) -0.007(3) -0.016(4) N1B 0.015(4) 0.040(5) 0.024(4) 0.012(4) 0.003(3) 0.006(4) C2B 0.045(7) 0.043(7) 0.026(6) 0.012(5) 0.013(5) 0.009(6) C3B 0.048(8) 0.036(7) 0.026(6) 0.009(5) 0.008(5) 0.010(6) C4B 0.043(7) 0.039(7) 0.034(6) 0.008(5) 0.012(5) 0.020(6) C5B 0.042(8) 0.100(14) 0.056(9) 0.036(9) 0.027(7) 0.047(9) C6B 0.064(9) 0.045(8) 0.063(10) -0.004(8) 0.026(8) 0.033(7) C7B 0.035(7) 0.054(9) 0.040(7) 0.016(6) -0.008(6) 0.010(6) C8B 0.027(6) 0.059(9) 0.058(9) 0.006(7) 0.017(6) 0.019(6) C9B 0.044(8) 0.062(9) 0.044(8) 0.025(7) 0.021(6) 0.024(7) C10B 0.025(6) 0.040(7) 0.042(7) -0.006(5) -0.006(5) 0.002(5) C11B 0.022(6) 0.049(8) 0.044(7) 0.022(6) -0.001(5) -0.001(5) C12B 0.053(8) 0.079(11) 0.032(7) 0.038(7) 0.022(6) 0.043(8) C13B 0.049(7) 0.022(5) 0.022(5) -0.001(4) -0.008(5) 0.004(5) O14B 0.053(5) 0.023(4) 0.024(4) 0.005(3) 0.007(4) 0.013(4) O15B 0.032(4) 0.030(4) 0.027(4) -0.013(3) 0.008(3) 0.002(3) N1C 0.038(6) 0.038(6) 0.023(5) 0.005(4) 0.001(4) -0.004(5) C2C 0.073(10) 0.034(7) 0.022(5) -0.009(5) 0.001(6) -0.015(7) C3C 0.053(8) 0.041(7) 0.040(7) 0.013(6) 0.022(6) -0.024(6) C4C 0.023(6) 0.034(6) 0.040(6) -0.002(5) -0.006(5) -0.014(5) C5C 0.037(7) 0.030(6) 0.038(6) -0.001(5) -0.006(5) 0.003(5) C6C 0.030(6) 0.032(6) 0.034(6) 0.004(5) -0.014(5) -0.002(5) C7C 0.054(8) 0.034(7) 0.041(7) 0.009(6) -0.026(6) -0.015(6) C8C 0.099(14) 0.058(10) 0.041(8) -0.001(7) -0.015(9) -0.042(10) C9C 0.064(9) 0.057(9) 0.027(6) 0.000(6) -0.007(6) -0.036(8) C10C 0.030(6) 0.028(6) 0.047(7) -0.006(5) 0.004(5) -0.008(5) C11C 0.027(6) 0.038(7) 0.042(7) -0.014(6) -0.012(5) -0.004(5) C12C 0.038(7) 0.041(7) 0.026(5) 0.009(5) -0.005(5) -0.020(6) C13C 0.039(7) 0.031(6) 0.030(6) -0.005(5) 0.000(5) 0.001(5) O14C 0.032(5) 0.064(6) 0.034(5) 0.008(4) 0.009(4) 0.013(4) O15C 0.021(4) 0.033(4) 0.024(4) 0.000(3) -0.005(3) -0.008(3) N1D 0.047(6) 0.015(4) 0.027(5) 0.003(4) 0.002(4) 0.004(4) C2D 0.083(11) 0.059(9) 0.029(7) 0.016(6) 0.021(7) 0.050(9) C3D 0.080(11) 0.034(7) 0.047(8) 0.024(6) 0.017(7) 0.032(7) C4D 0.044(7) 0.037(7) 0.035(6) 0.016(5) 0.014(5) 0.020(6) C5D 0.026(6) 0.043(7) 0.022(5) 0.004(5) 0.004(4) 0.008(5) C6D 0.043(7) 0.040(7) 0.032(6) 0.010(5) -0.010(5) 0.005(6) C7D 0.035(7) 0.034(7) 0.049(8) -0.017(6) 0.016(5) 0.019(5) C8D 0.056(8) 0.021(6) 0.051(8) 0.013(5) 0.027(6) 0.015(5) C9D 0.053(8) 0.032(7) 0.047(7) 0.003(6) 0.021(6) 0.021(6) C10D 0.033(6) 0.034(6) 0.031(6) -0.004(5) 0.012(5) 0.009(5) C12D 0.054(9) 0.040(8) 0.051(8) 0.006(6) 0.019(7) 0.012(7) C13D 0.025(6) 0.054(8) 0.033(6) -0.015(6) -0.010(5) -0.008(6) O14D 0.030(4) 0.049(5) 0.036(4) 0.003(5) 0.002(4) 0.020(4) O15D 0.028(4) 0.038(5) 0.027(4) -0.002(3) 0.004(3) 0.010(4) N1E 0.035(5) 0.032(5) 0.022(5) 0.003(4) 0.016(4) 0.002(4) C2E 0.037(7) 0.039(7) 0.032(6) -0.008(5) 0.014(5) -0.011(5) C3E 0.061(9) 0.026(6) 0.028(6) -0.003(5) -0.015(6) -0.014(6) C4E 0.027(6) 0.034(6) 0.024(5) 0.002(4) -0.003(4) -0.010(5) C5E 0.044(7) 0.036(6) 0.024(5) 0.015(5) -0.011(5) -0.013(5) C6E 0.051(8) 0.032(6) 0.029(6) -0.001(5) 0.005(5) -0.005(6) C7E 0.035(6) 0.046(7) 0.021(5) 0.015(5) -0.003(5) -0.018(5) C8E 0.051(8) 0.062(9) 0.019(5) -0.005(5) 0.000(5) -0.033(7) C9E 0.079(11) 0.054(9) 0.030(6) 0.006(6) 0.003(7) -0.053(8) C10E 0.036(6) 0.033(6) 0.020(5) -0.012(4) -0.002(4) -0.020(5) C11E 0.029(6) 0.033(6) 0.024(5) 0.000(5) 0.001(4) -0.007(5) C12E 0.044(7) 0.027(6) 0.022(5) -0.003(4) -0.003(5) -0.006(5) C13E 0.018(5) 0.035(6) 0.031(6) 0.004(5) -0.002(4) 0.003(5) O14E 0.020(4) 0.039(4) 0.022(4) -0.002(3) -0.012(3) -0.007(3) O15E 0.037(5) 0.066(6) 0.029(5) 0.004(4) 0.009(4) 0.002(4) N1F 0.020(5) 0.033(5) 0.032(5) 0.002(4) -0.002(4) 0.009(4) C2F 0.057(8) 0.052(8) 0.039(7) 0.002(7) 0.015(7) 0.023(7) C3F 0.039(7) 0.070(10) 0.034(7) 0.020(6) 0.013(5) 0.025(7) C4F 0.038(7) 0.039(7) 0.055(8) 0.018(6) -0.012(6) 0.010(6) C5F 0.038(7) 0.039(7) 0.030(6) 0.012(5) -0.007(5) 0.006(5) C6F 0.035(6) 0.032(6) 0.038(6) 0.004(5) 0.007(5) 0.006(5) C7F 0.043(8) 0.043(7) 0.038(7) 0.014(6) 0.002(6) 0.002(6) C8F 0.046(8) 0.065(10) 0.058(9) 0.028(8) 0.016(7) 0.029(8) C9F 0.056(9) 0.032(7) 0.057(9) 0.011(6) -0.021(7) -0.003(6) C10F 0.038(7) 0.052(8) 0.030(6) 0.001(6) -0.007(5) 0.017(6) C11F 0.037(7) 0.048(7) 0.028(6) 0.007(5) 0.002(5) 0.013(6) C12F 0.035(6) 0.038(7) 0.030(6) 0.004(5) -0.005(5) 0.015(5) C13F 0.044(7) 0.024(5) 0.020(5) 0.008(4) -0.009(5) 0.003(5) O14F 0.040(5) 0.024(4) 0.032(4) -0.007(3) 0.004(4) 0.002(4) O15F 0.039(4) 0.038(5) 0.030(4) 0.009(4) 0.018(4) 0.005(4) N1G 0.017(4) 0.041(6) 0.023(4) -0.006(4) -0.016(3) -0.004(4) C2G 0.030(6) 0.063(9) 0.028(6) 0.013(6) -0.001(5) -0.013(6) C3G 0.028(6) 0.052(8) 0.030(6) 0.012(6) -0.007(5) -0.012(6) C4G 0.044(7) 0.024(5) 0.018(5) 0.002(4) 0.001(5) -0.013(5) C5G 0.032(6) 0.048(8) 0.032(6) 0.007(5) -0.004(5) -0.006(5) C6G 0.020(5) 0.060(8) 0.027(5) 0.002(5) -0.007(4) -0.002(5) C7G 0.047(7) 0.037(7) 0.026(6) 0.001(5) -0.012(5) 0.000(6) C8G 0.077(10) 0.030(6) 0.032(6) 0.005(5) -0.007(7) -0.013(7) C9G 0.074(10) 0.061(9) 0.032(7) 0.001(6) -0.014(7) -0.053(8) C10G 0.033(6) 0.029(6) 0.023(5) 0.001(4) 0.005(4) -0.014(5) C11G 0.026(5) 0.038(6) 0.023(5) -0.007(4) 0.003(4) -0.005(5) C12G 0.023(5) 0.033(6) 0.026(5) 0.006(4) 0.002(4) 0.005(4) C13G 0.043(7) 0.023(5) 0.023(5) 0.000(4) 0.000(5) 0.005(5) O14G 0.057(6) 0.041(5) 0.021(4) -0.001(4) -0.009(4) -0.010(4) O15G 0.033(4) 0.020(4) 0.024(4) -0.006(3) -0.001(3) -0.011(3) N1H 0.043(6) 0.011(4) 0.031(5) 0.003(3) -0.004(4) 0.000(4) C2H 0.053(8) 0.032(6) 0.039(7) -0.017(5) -0.007(6) 0.017(6) C3H 0.035(6) 0.039(7) 0.029(6) -0.003(5) -0.018(5) 0.008(5) C4H 0.044(7) 0.042(7) 0.026(6) -0.001(5) -0.015(5) 0.013(6) C5H 0.084(11) 0.031(6) 0.024(6) -0.004(5) -0.008(6) 0.028(7) C6H 0.040(7) 0.058(8) 0.041(7) 0.014(7) -0.028(6) 0.022(6) C7H 0.057(8) 0.037(7) 0.023(5) -0.002(5) -0.024(5) 0.021(6) C8H 0.066(9) 0.023(6) 0.041(7) 0.000(5) -0.020(6) 0.017(6) C9H 0.072(10) 0.039(7) 0.035(7) -0.001(6) -0.028(7) 0.028(7) C11H 0.033(6) 0.023(6) 0.036(6) 0.011(4) -0.010(5) 0.004(5) C12H 0.055(8) 0.034(7) 0.033(6) -0.004(5) -0.021(6) 0.021(6) C13H 0.026(6) 0.029(6) 0.026(5) 0.011(4) -0.007(4) 0.006(5) O14H 0.021(4) 0.040(5) 0.025(4) 0.006(3) -0.002(3) 0.002(3) O15H 0.037(4) 0.042(4) 0.025(4) 0.003(4) 0.000(4) 0.012(3) C10H 0.046(7) 0.024(6) 0.027(6) 0.005(4) -0.007(5) 0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1G 2.009(10) . ? Ni1 O15C 2.052(7) 1_445 ? Ni1 O14H 2.061(7) . ? Ni1 N1B 2.062(9) 7_765 ? Ni1 O14C 2.183(10) 1_445 ? Ni1 O15H 2.211(8) . ? Ni1 C13H 2.430(10) . ? Ni1 C13C 2.442(13) 1_445 ? Ni2 N1H 2.027(10) 7_754 ? Ni2 N1E 2.033(10) . ? Ni2 O14F 2.033(8) . ? Ni2 O15G 2.064(7) . ? Ni2 O15F 2.201(8) . ? Ni2 O14G 2.217(9) . ? Ni2 C13G 2.416(12) . ? Ni2 C13F 2.441(11) . ? Ni3 N1A 2.014(10) . ? Ni3 O15D 2.019(8) 7_865 ? Ni3 O14E 2.028(7) . ? Ni3 N1F 2.047(9) 7_765 ? Ni3 O14D 2.186(8) 7_865 ? Ni3 O15E 2.202(10) . ? Ni3 C13D 2.411(13) 7_865 ? Ni3 C13E 2.436(11) . ? Ni4 O15B 2.024(8) . ? Ni4 N1C 2.034(10) . ? Ni4 O14A 2.050(8) . ? Ni4 N1D 2.068(10) . ? Ni4 O14B 2.165(8) . ? Ni4 O15A 2.199(8) . ? Ni4 C13B 2.411(11) . ? Ni4 C13A 2.429(12) . ? N1A C6A 1.341(14) . ? N1A C2A 1.371(14) . ? C2A C3A 1.408(17) . ? C2A H2A 0.9500 . ? C3A C4A 1.451(18) . ? C3A H3A 0.9500 . ? C4A C5A 1.360(16) . ? C4A C7A 1.490(15) . ? C5A C6A 1.396(17) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C7A C12A 1.378(15) . ? C7A C8A 1.409(16) . ? C8A C9A 1.393(15) . ? C8A H8A 0.9500 . ? C9A C10A 1.396(16) . ? C9A H9A 0.9500 . ? C10A C11A 1.344(16) . ? C10A C13A 1.508(16) . ? C11A C12A 1.447(18) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? C13A O14A 1.243(14) . ? C13A O15A 1.278(13) . ? N1B C6B 1.334(15) . ? N1B C2B 1.367(14) . ? N1B Ni1 2.062(9) 7_764 ? C2B C3B 1.414(17) . ? C2B H2B 0.9500 . ? C3B C4B 1.355(16) . ? C3B H3B 0.9500 . ? C4B C5B 1.365(19) . ? C4B C7B 1.448(16) . ? C5B C6B 1.390(19) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C7B C8B 1.354(19) . ? C7B C12B 1.438(18) . ? C8B C9B 1.352(18) . ? C8B H8B 0.9500 . ? C9B C10B 1.389(17) . ? C9B H9B 0.9500 . ? C10B C11B 1.392(18) . ? C10B C13B 1.503(16) . ? C11B C12B 1.401(16) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? C13B O15B 1.273(14) . ? C13B O14B 1.273(14) . ? N1C C2C 1.333(16) . ? N1C C6C 1.329(15) . ? C2C C3C 1.417(18) . ? C2C H2C 0.9500 . ? C3C C4C 1.363(17) . ? C3C H3C 0.9500 . ? C4C C5C 1.408(16) . ? C4C C7C 1.488(16) . ? C5C C6C 1.438(16) . ? C5C H5C 0.9500 . ? C6C H6C 0.9500 . ? C7C C8C 1.375(19) . ? C7C C12C 1.387(16) . ? C8C C9C 1.429(18) . ? C8C H8C 0.9500 . ? C9C C10C 1.355(17) . ? C9C H9C 0.9500 . ? C10C C11C 1.364(18) . ? C10C C13C 1.510(17) . ? C11C C12C 1.423(15) . ? C11C H11C 0.9500 . ? C12C H12C 0.9500 . ? C13C O15C 1.247(14) . ? C13C O14C 1.286(14) . ? C13C Ni1 2.442(13) 1_665 ? O14C Ni1 2.183(10) 1_665 ? O15C Ni1 2.052(7) 1_665 ? N1D C2D 1.309(15) . ? N1D C6D 1.311(15) . ? C2D C3D 1.340(18) . ? C2D H2D 0.9500 . ? C3D C4D 1.384(18) . ? C3D H3D 0.9500 . ? C4D C5D 1.335(16) . ? C4D C7D 1.474(15) . ? C5D C6D 1.447(17) . ? C5D H5D 0.9500 . ? C6D H6D 0.9500 . ? C7D C8D 1.340(17) . ? C7D C12D 1.450(18) . ? C8D C9D 1.420(16) . ? C8D H8D 0.9500 . ? C9D C10D 1.346(17) . ? C9D H9D 0.9500 . ? C10D C11D 1.426(18) . ? C10D C13D 1.517(16) . ? C11D C12D 1.356(19) . ? C11D H11D 0.9500 . ? C12D H12D 0.9500 . ? C13D O14D 1.235(16) . ? C13D O15D 1.255(16) . ? C13D Ni3 2.411(13) 7_864 ? O14D Ni3 2.186(8) 7_864 ? O15D Ni3 2.019(8) 7_864 ? N1E C6E 1.324(15) . ? N1E C2E 1.356(15) . ? C2E C3E 1.399(16) . ? C2E H2E 0.9500 . ? C3E C4E 1.405(15) . ? C3E H3E 0.9500 . ? C4E C5E 1.437(16) . ? C4E C7E 1.470(16) . ? C5E C6E 1.339(17) . ? C5E H5E 0.9500 . ? C6E H6E 0.9500 . ? C7E C8E 1.374(15) . ? C7E C12E 1.393(15) . ? C8E C9E 1.431(16) . ? C8E H8E 0.9500 . ? C9E C10E 1.361(15) . ? C9E H9E 0.9500 . ? C10E C11E 1.384(14) . ? C10E C13E 1.500(15) . ? C11E C12E 1.401(15) . ? C11E H11E 0.9500 . ? C12E H12E 0.9500 . ? C13E O15E 1.230(14) . ? C13E O14E 1.271(14) . ? N1F C6F 1.320(15) . ? N1F C2F 1.342(15) . ? N1F Ni3 2.047(9) 7_764 ? C2F C3F 1.380(18) . ? C2F H2F 0.9500 . ? C3F C4F 1.425(19) . ? C3F H3F 0.9500 . ? C4F C5F 1.315(19) . ? C4F C7F 1.479(17) . ? C5F C6F 1.378(16) . ? C5F H5F 0.9500 . ? C6F H6F 0.9500 . ? C7F C12F 1.371(17) . ? C7F C8F 1.381(18) . ? C8F C9F 1.417(19) . ? C8F H8F 0.9500 . ? C9F C10F 1.36(2) . ? C9F H9F 0.9500 . ? C10F C11F 1.397(17) . ? C10F C13F 1.507(15) . ? C11F C12F 1.385(15) . ? C11F H11F 0.9500 . ? C12F H12F 0.9500 . ? C13F O14F 1.261(14) . ? C13F O15F 1.284(13) . ? N1G C2G 1.335(14) . ? N1G C6G 1.372(13) . ? C2G C3G 1.400(16) . ? C2G H2G 0.9500 . ? C3G C4G 1.440(16) . ? C3G H3G 0.9500 . ? C4G C5G 1.365(15) . ? C4G C7G 1.491(17) . ? C5G C6G 1.419(17) . ? C5G H5G 0.9500 . ? C6G H6G 0.9500 . ? C7G C12G 1.377(16) . ? C7G C8G 1.390(16) . ? C8G C9G 1.406(19) . ? C8G H8G 0.9500 . ? C9G C10G 1.379(16) . ? C9G H9G 0.9500 . ? C10G C11G 1.364(15) . ? C10G C13G 1.519(15) . ? C11G C12G 1.428(15) . ? C11G H11G 0.9500 . ? C12G H12G 0.9500 . ? C13G O15G 1.242(14) . ? C13G O14G 1.260(13) . ? N1H C6H 1.307(17) . ? N1H C2H 1.361(16) . ? N1H Ni2 2.027(10) 7_755 ? C2H C3H 1.423(16) . ? C2H H2H 0.9500 . ? C3H C4H 1.320(17) . ? C3H H3H 0.9500 . ? C4H C5H 1.401(16) . ? C4H C7H 1.500(15) . ? C5H C6H 1.451(16) . ? C5H H5H 0.9500 . ? C6H H6H 0.9500 . ? C7H C8H 1.391(16) . ? C7H C12H 1.411(16) . ? C8H C9H 1.326(16) . ? C8H H8H 0.9500 . ? C9H C10H 1.414(17) . ? C9H H9H 0.9500 . ? C11H C12H 1.408(15) . ? C11H C10H 1.422(16) . ? C11H H11H 0.9500 . ? C12H H12H 0.9500 . ? C13H O15H 1.249(14) . ? C13H O14H 1.288(14) . ? C13H C10H 1.461(14) . ? O1J C2J 1.231(5) . ? C2J N3J 1.323(5) . ? C2J H2J 0.9500 . ? N3J C5J 1.448(5) . ? N3J C4J 1.453(5) . ? C4J H4J1 0.9800 . ? C4J H4J2 0.9800 . ? C4J H4J3 0.9800 . ? C5J H5J1 0.9800 . ? C5J H5J2 0.9800 . ? C5J H5J3 0.9800 . ? O1K C2K 1.228(5) . ? C2K N3K 1.318(5) . ? C2K H2K 0.9500 . ? N3K C5K 1.31(2) . ? N3K C4K 1.445(5) . ? C4K H4K1 0.9800 . ? C4K H4K2 0.9800 . ? C4K H4K3 0.9800 . ? O1L C2L 1.230(5) . ? C2L N3L 1.322(5) . ? C2L H2L 0.9500 . ? N3L C4L 1.446(5) . ? N3L C5L 1.449(5) . ? C4L H4L1 0.9800 . ? C4L H4L2 0.9800 . ? C4L H4L3 0.9800 . ? C5L H5L1 0.9800 . ? C5L H5L2 0.9800 . ? C5L H5L3 0.9800 . ? O1M C2M 1.230(5) . ? C2M N3M 1.319(5) . ? C2M H2M 0.9500 . ? N3M C4M 1.444(5) . ? N3M C5M 1.444(5) . ? C4M H4M1 0.9800 . ? C4M H4M2 0.9800 . ? C4M H4M3 0.9800 . ? C5M H5M1 0.9800 . ? C5M H5M2 0.9800 . ? C5M H5M3 0.9800 . ? O1N C2N 1.431(5) . ? C2N C3N 1.540(5) . ? C2N H2N1 0.9900 . ? C2N H2N2 0.9900 . ? C3N H3N1 0.9800 . ? C3N H3N2 0.9800 . ? C3N H3N3 0.9800 . ? C2O O1O 1.432(5) . ? C2O C3O 1.541(5) . ? C2O H2O1 0.9900 . ? C2O H2O2 0.9900 . ? C3O H3O1 0.9801 . ? C3O H3O2 0.9801 . ? C3O H3O3 0.9801 . ? C2Q O1Q 1.430(5) . ? C2Q C3Q 1.540(5) . ? C2Q H2Q1 0.9900 . ? C2Q H2Q2 0.9900 . ? C5K H5K1 0.9800 . ? C5K H5K2 0.9800 . ? C5K H5K3 0.9800 . ? C3Q H3Q1 0.9800 . ? C3Q H3Q2 0.9800 . ? C3Q H3Q3 0.9800 . ? O2W O2W 0.9(3) 2_845 ? O2W O2W 0.9(3) 4_685 ? O2W O2W 1.3(4) 3_975 ? 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 N1G Ni1 O15C 98.0(3) . 1_445 ? N1G Ni1 O14H 98.1(3) . . ? O15C Ni1 O14H 157.3(3) 1_445 . ? N1G Ni1 N1B 96.1(4) . 7_765 ? O15C Ni1 N1B 98.6(3) 1_445 7_765 ? O14H Ni1 N1B 95.6(3) . 7_765 ? N1G Ni1 O14C 159.3(3) . 1_445 ? O15C Ni1 O14C 62.1(3) 1_445 1_445 ? O14H Ni1 O14C 99.7(3) . 1_445 ? N1B Ni1 O14C 92.6(4) 7_765 1_445 ? N1G Ni1 O15H 94.5(4) . . ? O15C Ni1 O15H 100.0(3) 1_445 . ? O14H Ni1 O15H 62.7(3) . . ? N1B Ni1 O15H 157.1(4) 7_765 . ? O14C Ni1 O15H 84.4(3) 1_445 . ? N1G Ni1 C13H 98.6(4) . . ? O15C Ni1 C13H 128.9(4) 1_445 . ? O14H Ni1 C13H 32.0(3) . . ? N1B Ni1 C13H 127.0(4) 7_765 . ? O14C Ni1 C13H 90.9(4) 1_445 . ? O15H Ni1 C13H 30.8(3) . . ? N1G Ni1 C13C 127.9(4) . 1_445 ? O15C Ni1 C13C 30.7(3) 1_445 1_445 ? O14H Ni1 C13C 129.0(4) . 1_445 ? N1B Ni1 C13C 99.4(4) 7_765 1_445 ? O14C Ni1 C13C 31.7(4) 1_445 1_445 ? O15H Ni1 C13C 89.9(4) . 1_445 ? C13H Ni1 C13C 110.2(4) . 1_445 ? N1H Ni2 N1E 96.3(4) 7_754 . ? N1H Ni2 O14F 96.2(4) 7_754 . ? N1E Ni2 O14F 97.6(3) . . ? N1H Ni2 O15G 99.3(3) 7_754 . ? N1E Ni2 O15G 97.4(3) . . ? O14F Ni2 O15G 157.0(3) . . ? N1H Ni2 O15F 157.6(4) 7_754 . ? N1E Ni2 O15F 93.9(4) . . ? O14F Ni2 O15F 62.6(3) . . ? O15G Ni2 O15F 99.1(3) . . ? N1H Ni2 O14G 92.7(4) 7_754 . ? N1E Ni2 O14G 158.6(3) . . ? O14F Ni2 O14G 100.6(3) . . ? O15G Ni2 O14G 61.9(3) . . ? O15F Ni2 O14G 84.8(3) . . ? N1H Ni2 C13G 99.6(4) 7_754 . ? N1E Ni2 C13G 127.7(4) . . ? O14F Ni2 C13G 129.2(4) . . ? O15G Ni2 C13G 30.9(3) . . ? O15F Ni2 C13G 89.7(4) . . ? O14G Ni2 C13G 31.2(3) . . ? N1H Ni2 C13F 126.8(4) 7_754 . ? N1E Ni2 C13F 97.7(4) . . ? O14F Ni2 C13F 31.1(3) . . ? O15G Ni2 C13F 129.0(4) . . ? O15F Ni2 C13F 31.6(3) . . ? O14G Ni2 C13F 92.3(4) . . ? C13G Ni2 C13F 111.0(4) . . ? N1A Ni3 O15D 97.2(3) . 7_865 ? N1A Ni3 O14E 97.4(3) . . ? O15D Ni3 O14E 157.5(3) 7_865 . ? N1A Ni3 N1F 95.6(4) . 7_765 ? O15D Ni3 N1F 95.4(4) 7_865 7_765 ? O14E Ni3 N1F 100.0(4) . 7_765 ? N1A Ni3 O14D 93.3(4) . 7_865 ? O15D Ni3 O14D 62.0(3) 7_865 7_865 ? O14E Ni3 O14D 100.2(3) . 7_865 ? N1F Ni3 O14D 156.6(4) 7_765 7_865 ? N1A Ni3 O15E 158.3(3) . . ? O15D Ni3 O15E 101.6(3) 7_865 . ? O14E Ni3 O15E 61.5(3) . . ? N1F Ni3 O15E 93.4(4) 7_765 . ? O14D Ni3 O15E 86.0(3) 7_865 . ? N1A Ni3 C13D 97.2(4) . 7_865 ? O15D Ni3 C13D 31.4(4) 7_865 7_865 ? O14E Ni3 C13D 129.2(4) . 7_865 ? N1F Ni3 C13D 126.4(4) 7_765 7_865 ? O14D Ni3 C13D 30.7(4) 7_865 7_865 ? O15E Ni3 C13D 93.2(4) . 7_865 ? N1A Ni3 C13E 128.3(4) . . ? O15D Ni3 C13E 129.4(4) 7_865 . ? O14E Ni3 C13E 31.4(3) . . ? N1F Ni3 C13E 100.1(4) 7_765 . ? O14D Ni3 C13E 91.1(4) 7_865 . ? O15E Ni3 C13E 30.2(3) . . ? C13D Ni3 C13E 111.4(4) 7_865 . ? O15B Ni4 N1C 97.3(3) . . ? O15B Ni4 O14A 157.5(3) . . ? N1C Ni4 O14A 97.4(3) . . ? O15B Ni4 N1D 95.7(3) . . ? N1C Ni4 N1D 96.6(4) . . ? O14A Ni4 N1D 99.4(3) . . ? O15B Ni4 O14B 63.4(3) . . ? N1C Ni4 O14B 91.7(4) . . ? O14A Ni4 O14B 99.2(3) . . ? N1D Ni4 O14B 158.4(3) . . ? O15B Ni4 O15A 100.6(3) . . ? N1C Ni4 O15A 158.6(3) . . ? O14A Ni4 O15A 62.1(3) . . ? N1D Ni4 O15A 93.2(4) . . ? O14B Ni4 O15A 86.0(3) . . ? O15B Ni4 C13B 31.9(3) . . ? N1C Ni4 C13B 97.9(4) . . ? O14A Ni4 C13B 128.6(4) . . ? N1D Ni4 C13B 126.9(4) . . ? O14B Ni4 C13B 31.7(4) . . ? O15A Ni4 C13B 91.3(4) . . ? O15B Ni4 C13A 129.7(4) . . ? N1C Ni4 C13A 127.4(4) . . ? O14A Ni4 C13A 30.8(3) . . ? N1D Ni4 C13A 100.1(4) . . ? O14B Ni4 C13A 90.4(3) . . ? O15A Ni4 C13A 31.6(3) . . ? C13B Ni4 C13A 110.3(4) . . ? C6A N1A C2A 115.2(10) . . ? C6A N1A Ni3 122.7(8) . . ? C2A N1A Ni3 122.1(8) . . ? N1A C2A C3A 124.8(11) . . ? N1A C2A H2A 117.6 . . ? C3A C2A H2A 117.6 . . ? C2A C3A C4A 115.9(11) . . ? C2A C3A H3A 122.1 . . ? C4A C3A H3A 122.1 . . ? C5A C4A C3A 119.9(11) . . ? C5A C4A C7A 120.4(11) . . ? C3A C4A C7A 119.6(11) . . ? C4A C5A C6A 118.3(11) . . ? C4A C5A H5A 120.8 . . ? C6A C5A H5A 120.9 . . ? N1A C6A C5A 125.9(11) . . ? N1A C6A H6A 117.0 . . ? C5A C6A H6A 117.0 . . ? C12A C7A C8A 118.3(11) . . ? C12A C7A C4A 120.8(11) . . ? C8A C7A C4A 120.9(10) . . ? C9A C8A C7A 121.9(11) . . ? C9A C8A H8A 119.0 . . ? C7A C8A H8A 119.0 . . ? C8A C9A C10A 117.9(11) . . ? C8A C9A H9A 121.0 . . ? C10A C9A H9A 121.0 . . ? C11A C10A C9A 121.9(11) . . ? C11A C10A C13A 120.3(11) . . ? C9A C10A C13A 117.2(10) . . ? C10A C11A C12A 120.0(11) . . ? C10A C11A H11A 120.0 . . ? C12A C11A H11A 120.0 . . ? C7A C12A C11A 119.4(12) . . ? C7A C12A H12A 120.3 . . ? C11A C12A H12A 120.3 . . ? O14A C13A O15A 121.1(11) . . ? O14A C13A C10A 120.4(10) . . ? O15A C13A C10A 118.4(11) . . ? O14A C13A Ni4 57.5(6) . . ? O15A C13A Ni4 64.2(6) . . ? C10A C13A Ni4 170.1(9) . . ? C13A O14A Ni4 91.7(7) . . ? C13A O15A Ni4 84.2(7) . . ? C6B N1B C2B 119.8(11) . . ? C6B N1B Ni1 124.4(9) . 7_764 ? C2B N1B Ni1 115.4(8) . 7_764 ? N1B C2B C3B 117.4(11) . . ? N1B C2B H2B 121.3 . . ? C3B C2B H2B 121.3 . . ? C4B C3B C2B 123.3(11) . . ? C4B C3B H3B 118.3 . . ? C2B C3B H3B 118.3 . . ? C3B C4B C5B 116.8(12) . . ? C3B C4B C7B 118.8(11) . . ? C5B C4B C7B 124.4(12) . . ? C4B C5B C6B 120.7(14) . . ? C4B C5B H5B 119.7 . . ? C6B C5B H5B 119.7 . . ? N1B C6B C5B 121.8(15) . . ? N1B C6B H6B 119.1 . . ? C5B C6B H6B 119.1 . . ? C8B C7B C12B 115.5(11) . . ? C8B C7B C4B 127.1(12) . . ? C12B C7B C4B 116.7(12) . . ? C7B C8B C9B 123.9(12) . . ? C7B C8B H8B 118.1 . . ? C9B C8B H8B 118.1 . . ? C8B C9B C10B 121.6(12) . . ? C8B C9B H9B 119.2 . . ? C10B C9B H9B 119.2 . . ? C9B C10B C11B 118.1(12) . . ? C9B C10B C13B 121.4(12) . . ? C11B C10B C13B 120.5(11) . . ? C10B C11B C12B 119.3(12) . . ? C10B C11B H11B 120.4 . . ? C12B C11B H11B 120.4 . . ? C11B C12B C7B 121.4(11) . . ? C11B C12B H12B 119.3 . . ? C7B C12B H12B 119.3 . . ? O15B C13B O14B 119.9(10) . . ? O15B C13B C10B 117.5(10) . . ? O14B C13B C10B 122.2(11) . . ? O15B C13B Ni4 57.1(6) . . ? O14B C13B Ni4 63.4(6) . . ? C10B C13B Ni4 174.3(9) . . ? C13B O14B Ni4 84.9(7) . . ? C13B O15B Ni4 91.1(6) . . ? C2C N1C C6C 116.5(11) . . ? C2C N1C Ni4 121.4(8) . . ? C6C N1C Ni4 122.1(8) . . ? N1C C2C C3C 124.4(12) . . ? N1C C2C H2C 117.8 . . ? C3C C2C H2C 117.8 . . ? C4C C3C C2C 118.1(13) . . ? C4C C3C H3C 121.0 . . ? C2C C3C H3C 121.0 . . ? C3C C4C C5C 120.4(12) . . ? C3C C4C C7C 119.2(12) . . ? C5C C4C C7C 120.4(11) . . ? C4C C5C C6C 115.9(11) . . ? C4C C5C H5C 122.1 . . ? C6C C5C H5C 122.1 . . ? N1C C6C C5C 124.7(11) . . ? N1C C6C H6C 117.7 . . ? C5C C6C H6C 117.7 . . ? C8C C7C C12C 120.5(12) . . ? C8C C7C C4C 121.0(12) . . ? C12C C7C C4C 118.4(11) . . ? C7C C8C C9C 118.1(13) . . ? C7C C8C H8C 121.0 . . ? C9C C8C H8C 121.0 . . ? C10C C9C C8C 120.5(12) . . ? C10C C9C H9C 119.7 . . ? C8C C9C H9C 119.7 . . ? C9C C10C C11C 121.8(11) . . ? C9C C10C C13C 119.8(12) . . ? C11C C10C C13C 117.7(11) . . ? C10C C11C C12C 118.5(12) . . ? C10C C11C H11C 120.7 . . ? C12C C11C H11C 120.7 . . ? C7C C12C C11C 119.9(11) . . ? C7C C12C H12C 120.1 . . ? C11C C12C H12C 120.1 . . ? O15C C13C O14C 119.4(12) . . ? O15C C13C C10C 120.4(11) . . ? O14C C13C C10C 120.2(12) . . ? O15C C13C Ni1 57.1(6) . 1_665 ? O14C C13C Ni1 63.0(7) . 1_665 ? C10C C13C Ni1 170.5(9) . 1_665 ? C13C O14C Ni1 85.3(8) . 1_665 ? C13C O15C Ni1 92.2(7) . 1_665 ? C2D N1D C6D 119.2(11) . . ? C2D N1D Ni4 123.0(8) . . ? C6D N1D Ni4 116.7(8) . . ? N1D C2D C3D 122.2(12) . . ? N1D C2D H2D 118.9 . . ? C3D C2D H2D 118.9 . . ? C2D C3D C4D 122.2(12) . . ? C2D C3D H3D 118.9 . . ? C4D C3D H3D 118.9 . . ? C5D C4D C3D 116.0(11) . . ? C5D C4D C7D 118.6(11) . . ? C3D C4D C7D 125.4(11) . . ? C4D C5D C6D 120.0(11) . . ? C4D C5D H5D 120.0 . . ? C6D C5D H5D 120.0 . . ? N1D C6D C5D 120.3(11) . . ? N1D C6D H6D 119.8 . . ? C5D C6D H6D 119.8 . . ? C8D C7D C12D 118.9(11) . . ? C8D C7D C4D 123.9(12) . . ? C12D C7D C4D 116.5(11) . . ? C7D C8D C9D 119.9(11) . . ? C7D C8D H8D 120.1 . . ? C9D C8D H8D 120.1 . . ? C10D C9D C8D 122.0(12) . . ? C10D C9D H9D 119.0 . . ? C8D C9D H9D 119.0 . . ? C9D C10D C11D 117.9(11) . . ? C9D C10D C13D 121.9(11) . . ? C11D C10D C13D 120.1(11) . . ? C12D C11D C10D 120.6(13) . . ? C12D C11D H11D 119.7 . . ? C10D C11D H11D 119.7 . . ? C11D C12D C7D 119.7(13) . . ? C11D C12D H12D 120.1 . . ? C7D C12D H12D 120.1 . . ? O14D C13D O15D 121.3(12) . . ? O14D C13D C10D 120.2(12) . . ? O15D C13D C10D 118.5(11) . . ? O14D C13D Ni3 64.5(6) . 7_864 ? O15D C13D Ni3 56.8(6) . 7_864 ? C10D C13D Ni3 174.8(10) . 7_864 ? C13D O14D Ni3 84.8(8) . 7_864 ? C13D O15D Ni3 91.8(7) . 7_864 ? C6E N1E C2E 116.1(11) . . ? C6E N1E Ni2 122.2(8) . . ? C2E N1E Ni2 121.7(8) . . ? N1E C2E C3E 124.4(12) . . ? N1E C2E H2E 117.8 . . ? C3E C2E H2E 117.8 . . ? C2E C3E C4E 118.5(11) . . ? C2E C3E H3E 120.8 . . ? C4E C3E H3E 120.8 . . ? C3E C4E C5E 115.2(10) . . ? C3E C4E C7E 122.3(10) . . ? C5E C4E C7E 122.4(10) . . ? C6E C5E C4E 121.0(11) . . ? C6E C5E H5E 119.5 . . ? C4E C5E H5E 119.5 . . ? N1E C6E C5E 124.7(12) . . ? N1E C6E H6E 117.6 . . ? C5E C6E H6E 117.6 . . ? C8E C7E C12E 118.6(11) . . ? C8E C7E C4E 121.3(10) . . ? C12E C7E C4E 120.1(10) . . ? C7E C8E C9E 120.5(11) . . ? C7E C8E H8E 119.8 . . ? C9E C8E H8E 119.8 . . ? C10E C9E C8E 120.3(11) . . ? C10E C9E H9E 119.8 . . ? C8E C9E H9E 119.8 . . ? C9E C10E C11E 118.9(10) . . ? C9E C10E C13E 118.9(10) . . ? C11E C10E C13E 121.7(10) . . ? C10E C11E C12E 121.4(10) . . ? C10E C11E H11E 119.3 . . ? C12E C11E H11E 119.3 . . ? C7E C12E C11E 119.8(10) . . ? C7E C12E H12E 120.1 . . ? C11E C12E H12E 120.1 . . ? O15E C13E O14E 120.1(11) . . ? O15E C13E C10E 122.2(11) . . ? O14E C13E C10E 117.6(10) . . ? O15E C13E Ni3 64.3(7) . . ? O14E C13E Ni3 56.3(5) . . ? C10E C13E Ni3 168.0(8) . . ? C13E O14E Ni3 92.3(6) . . ? C13E O15E Ni3 85.5(7) . . ? C6F N1F C2F 115.3(11) . . ? C6F N1F Ni3 119.8(8) . 7_764 ? C2F N1F Ni3 124.7(9) . 7_764 ? N1F C2F C3F 124.4(13) . . ? N1F C2F H2F 117.8 . . ? C3F C2F H2F 117.8 . . ? C2F C3F C4F 117.9(13) . . ? C2F C3F H3F 121.0 . . ? C4F C3F H3F 121.0 . . ? C5F C4F C3F 116.0(11) . . ? C5F C4F C7F 123.2(13) . . ? C3F C4F C7F 120.7(13) . . ? C4F C5F C6F 122.6(12) . . ? C4F C5F H5F 118.7 . . ? C6F C5F H5F 118.7 . . ? N1F C6F C5F 123.3(11) . . ? N1F C6F H6F 118.4 . . ? C5F C6F H6F 118.4 . . ? C12F C7F C8F 119.6(12) . . ? C12F C7F C4F 121.2(12) . . ? C8F C7F C4F 118.9(12) . . ? C7F C8F C9F 120.2(14) . . ? C7F C8F H8F 119.9 . . ? C9F C8F H8F 119.9 . . ? C10F C9F C8F 118.7(15) . . ? C10F C9F H9F 120.7 . . ? C8F C9F H9F 120.7 . . ? C9F C10F C11F 121.3(12) . . ? C9F C10F C13F 118.5(12) . . ? C11F C10F C13F 120.1(11) . . ? C12F C11F C10F 118.8(12) . . ? C12F C11F H11F 120.6 . . ? C10F C11F H11F 120.6 . . ? C7F C12F C11F 121.1(12) . . ? C7F C12F H12F 119.5 . . ? C11F C12F H12F 119.5 . . ? O14F C13F O15F 120.1(10) . . ? O14F C13F C10F 118.7(10) . . ? O15F C13F C10F 121.2(11) . . ? O14F C13F Ni2 56.3(6) . . ? O15F C13F Ni2 63.8(6) . . ? C10F C13F Ni2 174.5(9) . . ? C13F O14F Ni2 92.6(6) . . ? C13F O15F Ni2 84.6(7) . . ? C2G N1G C6G 116.0(10) . . ? C2G N1G Ni1 122.3(8) . . ? C6G N1G Ni1 121.5(8) . . ? N1G C2G C3G 125.6(12) . . ? N1G C2G H2G 117.2 . . ? C3G C2G H2G 117.2 . . ? C2G C3G C4G 116.7(11) . . ? C2G C3G H3G 121.6 . . ? C4G C3G H3G 121.7 . . ? C5G C4G C3G 119.5(11) . . ? C5G C4G C7G 121.6(11) . . ? C3G C4G C7G 118.9(10) . . ? C4G C5G C6G 118.7(11) . . ? C4G C5G H5G 120.7 . . ? C6G C5G H5G 120.7 . . ? N1G C6G C5G 123.5(11) . . ? N1G C6G H6G 118.3 . . ? C5G C6G H6G 118.3 . . ? C12G C7G C8G 120.6(12) . . ? C12G C7G C4G 119.0(10) . . ? C8G C7G C4G 120.3(11) . . ? C7G C8G C9G 117.9(13) . . ? C7G C8G H8G 121.1 . . ? C9G C8G H8G 121.1 . . ? C10G C9G C8G 122.6(12) . . ? C10G C9G H9G 118.7 . . ? C8G C9G H9G 118.7 . . ? C11G C10G C9G 118.3(11) . . ? C11G C10G C13G 119.8(10) . . ? C9G C10G C13G 121.8(10) . . ? C10G C11G C12G 120.9(10) . . ? C10G C11G H11G 119.6 . . ? C12G C11G H11G 119.6 . . ? C7G C12G C11G 119.1(10) . . ? C7G C12G H12G 120.4 . . ? C11G C12G H12G 120.4 . . ? O15G C13G O14G 123.7(11) . . ? O15G C13G C10G 117.2(10) . . ? O14G C13G C10G 119.0(11) . . ? O15G C13G Ni2 58.7(6) . . ? O14G C13G Ni2 65.6(6) . . ? C10G C13G Ni2 168.6(8) . . ? C13G O14G Ni2 83.2(7) . . ? C13G O15G Ni2 90.4(7) . . ? C6H N1H C2H 118.4(10) . . ? C6H N1H Ni2 125.3(8) . 7_755 ? C2H N1H Ni2 116.2(8) . 7_755 ? N1H C2H C3H 119.7(11) . . ? N1H C2H H2H 120.1 . . ? C3H C2H H2H 120.1 . . ? C4H C3H C2H 121.5(11) . . ? C4H C3H H3H 119.3 . . ? C2H C3H H3H 119.3 . . ? C3H C4H C5H 120.7(11) . . ? C3H C4H C7H 121.8(11) . . ? C5H C4H C7H 117.5(11) . . ? C4H C5H C6H 114.8(12) . . ? C4H C5H H5H 122.6 . . ? C6H C5H H5H 122.6 . . ? N1H C6H C5H 124.5(12) . . ? N1H C6H H6H 117.7 . . ? C5H C6H H6H 117.7 . . ? C8H C7H C12H 117.4(10) . . ? C8H C7H C4H 122.9(11) . . ? C12H C7H C4H 118.7(10) . . ? C9H C8H C7H 123.4(12) . . ? C9H C8H H8H 118.3 . . ? C7H C8H H8H 118.3 . . ? C8H C9H C10H 121.7(12) . . ? C8H C9H H9H 119.2 . . ? C10H C9H H9H 119.1 . . ? C12H C11H C10H 120.4(11) . . ? C12H C11H H11H 119.8 . . ? C10H C11H H11H 119.8 . . ? C11H C12H C7H 120.0(11) . . ? C11H C12H H12H 120.0 . . ? C7H C12H H12H 120.0 . . ? O15H C13H O14H 122.8(9) . . ? O15H C13H C10H 120.0(10) . . ? O14H C13H C10H 117.2(10) . . ? O15H C13H Ni1 64.9(5) . . ? O14H C13H Ni1 58.0(5) . . ? C10H C13H Ni1 173.7(9) . . ? C13H O14H Ni1 90.0(6) . . ? C13H O15H Ni1 84.3(6) . . ? O1J C2J N3J 124.5(7) . . ? O1J C2J H2J 117.7 . . ? N3J C2J H2J 117.7 . . ? C2J N3J C5J 120.2(6) . . ? C2J N3J C4J 119.6(6) . . ? C5J N3J C4J 119.7(9) . . ? N3J C4J H4J1 109.5 . . ? N3J C4J H4J2 109.5 . . ? H4J1 C4J H4J2 109.5 . . ? N3J C4J H4J3 109.5 . . ? H4J1 C4J H4J3 109.5 . . ? H4J2 C4J H4J3 109.5 . . ? N3J C5J H5J1 109.5 . . ? N3J C5J H5J2 109.5 . . ? H5J1 C5J H5J2 109.5 . . ? N3J C5J H5J3 109.5 . . ? H5J1 C5J H5J3 109.5 . . ? H5J2 C5J H5J3 109.5 . . ? O1K C2K N3K 125.4(7) . . ? O1K C2K H2K 117.3 . . ? N3K C2K H2K 117.3 . . ? C2K N3K C5K 131.8(19) . . ? C2K N3K C4K 121.0(6) . . ? C5K N3K C4K 107.1(19) . . ? N3K C4K H4K1 109.4 . . ? N3K C4K H4K2 109.5 . . ? H4K1 C4K H4K2 109.5 . . ? N3K C4K H4K3 109.5 . . ? H4K1 C4K H4K3 109.5 . . ? H4K2 C4K H4K3 109.5 . . ? O1L C2L N3L 124.7(7) . . ? O1L C2L H2L 117.7 . . ? N3L C2L H2L 117.6 . . ? C2L N3L C4L 120.4(6) . . ? C2L N3L C5L 120.0(6) . . ? C4L N3L C5L 119.0(10) . . ? N3L C4L H4L1 109.5 . . ? N3L C4L H4L2 109.5 . . ? H4L1 C4L H4L2 109.5 . . ? N3L C4L H4L3 109.5 . . ? H4L1 C4L H4L3 109.5 . . ? H4L2 C4L H4L3 109.5 . . ? N3L C5L H5L1 109.5 . . ? N3L C5L H5L2 109.5 . . ? H5L1 C5L H5L2 109.5 . . ? N3L C5L H5L3 109.5 . . ? H5L1 C5L H5L3 109.5 . . ? H5L2 C5L H5L3 109.5 . . ? O1M C2M N3M 124.8(7) . . ? O1M C2M H2M 117.6 . . ? N3M C2M H2M 117.6 . . ? C2M N3M C4M 120.9(6) . . ? C2M N3M C5M 120.9(6) . . ? C4M N3M C5M 117.4(12) . . ? N3M C4M H4M1 109.5 . . ? N3M C4M H4M2 109.5 . . ? H4M1 C4M H4M2 109.5 . . ? N3M C4M H4M3 109.5 . . ? H4M1 C4M H4M3 109.5 . . ? H4M2 C4M H4M3 109.5 . . ? N3M C5M H5M1 109.5 . . ? N3M C5M H5M2 109.5 . . ? H5M1 C5M H5M2 109.5 . . ? N3M C5M H5M3 109.5 . . ? H5M1 C5M H5M3 109.5 . . ? H5M2 C5M H5M3 109.5 . . ? O1N C2N C3N 139(5) . . ? O1N C2N H2N1 102.2 . . ? C3N C2N H2N1 102.3 . . ? O1N C2N H2N2 102.2 . . ? C3N C2N H2N2 102.2 . . ? H2N1 C2N H2N2 104.8 . . ? C2N C3N H3N1 109.4 . . ? C2N C3N H3N2 109.5 . . ? H3N1 C3N H3N2 109.5 . . ? C2N C3N H3N3 109.5 . . ? H3N1 C3N H3N3 109.5 . . ? H3N2 C3N H3N3 109.5 . . ? O1O C2O C3O 140.5(10) . . ? O1O C2O H2O1 101.9 . . ? C3O C2O H2O1 101.8 . . ? O1O C2O H2O2 102.0 . . ? C3O C2O H2O2 102.0 . . ? H2O1 C2O H2O2 104.7 . . ? C2O C3O H3O1 109.4 . . ? C2O C3O H3O2 109.6 . . ? H3O1 C3O H3O2 109.5 . . ? C2O C3O H3O3 109.4 . . ? H3O1 C3O H3O3 109.5 . . ? H3O2 C3O H3O3 109.5 . . ? O1Q C2Q C3Q 141.0(10) . . ? O1Q C2Q H2Q1 101.7 . . ? C3Q C2Q H2Q1 101.7 . . ? O1Q C2Q H2Q2 101.8 . . ? C3Q C2Q H2Q2 101.8 . . ? H2Q1 C2Q H2Q2 104.7 . . ? N3K C5K H5K1 109.5 . . ? N3K C5K H5K2 109.5 . . ? H5K1 C5K H5K2 109.5 . . ? N3K C5K H5K3 109.4 . . ? H5K1 C5K H5K3 109.5 . . ? H5K2 C5K H5K3 109.5 . . ? C9H C10H C11H 116.8(10) . . ? C9H C10H C13H 122.7(10) . . ? C11H C10H C13H 120.5(10) . . ? C2Q C3Q H3Q1 109.5 . . ? C2Q C3Q H3Q2 109.5 . . ? H3Q1 C3Q H3Q2 109.5 . . ? C2Q C3Q H3Q3 109.4 . . ? H3Q1 C3Q H3Q3 109.5 . . ? H3Q2 C3Q H3Q3 109.5 . . ? O2W O2W O2W 90.00(11) 2_845 4_685 ? O2W O2W O2W 45.00(8) 2_845 3_975 ? O2W O2W O2W 45.00(2) 4_685 3_975 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O15D Ni3 N1A C6A -177.4(9) 7_865 . . . ? O14E Ni3 N1A C6A 19.7(10) . . . . ? N1F Ni3 N1A C6A -81.1(10) 7_765 . . . ? O14D Ni3 N1A C6A 120.5(9) 7_865 . . . ? O15E Ni3 N1A C6A 32.9(17) . . . . ? C13D Ni3 N1A C6A 151.0(10) 7_865 . . . ? C13E Ni3 N1A C6A 26.4(11) . . . . ? O15D Ni3 N1A C2A 4.9(10) 7_865 . . . ? O14E Ni3 N1A C2A -158.0(9) . . . . ? N1F Ni3 N1A C2A 101.1(9) 7_765 . . . ? O14D Ni3 N1A C2A -57.3(9) 7_865 . . . ? O15E Ni3 N1A C2A -144.8(10) . . . . ? C13D Ni3 N1A C2A -26.7(10) 7_865 . . . ? C13E Ni3 N1A C2A -151.3(8) . . . . ? C6A N1A C2A C3A -0.9(18) . . . . ? Ni3 N1A C2A C3A 177.0(11) . . . . ? N1A C2A C3A C4A 2(2) . . . . ? C2A C3A C4A C5A -1(2) . . . . ? C2A C3A C4A C7A 174.3(12) . . . . ? C3A C4A C5A C6A -0.4(19) . . . . ? C7A C4A C5A C6A -176.2(11) . . . . ? C2A N1A C6A C5A -1.3(18) . . . . ? Ni3 N1A C6A C5A -179.2(10) . . . . ? C4A C5A C6A N1A 2(2) . . . . ? C5A C4A C7A C12A -27.3(19) . . . . ? C3A C4A C7A C12A 156.9(14) . . . . ? C5A C4A C7A C8A 153.4(13) . . . . ? C3A C4A C7A C8A -22.4(19) . . . . ? C12A C7A C8A C9A 9(2) . . . . ? C4A C7A C8A C9A -172.1(12) . . . . ? C7A C8A C9A C10A -7(2) . . . . ? C8A C9A C10A C11A 3(2) . . . . ? C8A C9A C10A C13A 173.8(12) . . . . ? C9A C10A C11A C12A 0(2) . . . . ? C13A C10A C11A C12A -171.3(13) . . . . ? C8A C7A C12A C11A -6(2) . . . . ? C4A C7A C12A C11A 174.6(13) . . . . ? C10A C11A C12A C7A 2(2) . . . . ? C11A C10A C13A O14A 168.3(12) . . . . ? C9A C10A C13A O14A -3.0(17) . . . . ? C11A C10A C13A O15A -9.8(19) . . . . ? C9A C10A C13A O15A 178.9(11) . . . . ? C11A C10A C13A Ni4 93(5) . . . . ? C9A C10A C13A Ni4 -78(5) . . . . ? O15B Ni4 C13A O14A -162.2(6) . . . . ? N1C Ni4 C13A O14A -14.9(9) . . . . ? N1D Ni4 C13A O14A 91.6(7) . . . . ? O14B Ni4 C13A O14A -107.4(7) . . . . ? O15A Ni4 C13A O14A 171.1(11) . . . . ? C13B Ni4 C13A O14A -132.7(7) . . . . ? O15B Ni4 C13A O15A 26.7(9) . . . . ? N1C Ni4 C13A O15A 174.0(7) . . . . ? O14A Ni4 C13A O15A -171.1(11) . . . . ? N1D Ni4 C13A O15A -79.5(7) . . . . ? O14B Ni4 C13A O15A 81.5(7) . . . . ? C13B Ni4 C13A O15A 56.2(8) . . . . ? O15B Ni4 C13A C10A -81(5) . . . . ? N1C Ni4 C13A C10A 66(5) . . . . ? O14A Ni4 C13A C10A 81(5) . . . . ? N1D Ni4 C13A C10A 172(5) . . . . ? O14B Ni4 C13A C10A -26(5) . . . . ? O15A Ni4 C13A C10A -108(5) . . . . ? C13B Ni4 C13A C10A -52(5) . . . . ? O15A C13A O14A Ni4 9.4(12) . . . . ? C10A C13A O14A Ni4 -168.7(10) . . . . ? O15B Ni4 O14A C13A 37.8(12) . . . . ? N1C Ni4 O14A C13A 168.1(7) . . . . ? N1D Ni4 O14A C13A -93.8(7) . . . . ? O14B Ni4 O14A C13A 75.2(7) . . . . ? O15A Ni4 O14A C13A -5.3(7) . . . . ? C13B Ni4 O14A C13A 61.8(8) . . . . ? O14A C13A O15A Ni4 -8.8(11) . . . . ? C10A C13A O15A Ni4 169.3(10) . . . . ? O15B Ni4 O15A C13A -159.4(7) . . . . ? N1C Ni4 O15A C13A -13.1(14) . . . . ? O14A Ni4 O15A C13A 5.1(7) . . . . ? N1D Ni4 O15A C13A 104.1(7) . . . . ? O14B Ni4 O15A C13A -97.5(7) . . . . ? C13B Ni4 O15A C13A -128.8(7) . . . . ? C6B N1B C2B C3B 5.0(19) . . . . ? Ni1 N1B C2B C3B -168.3(10) 7_764 . . . ? N1B C2B C3B C4B -3(2) . . . . ? C2B C3B C4B C5B -1(2) . . . . ? C2B C3B C4B C7B -178.8(13) . . . . ? C3B C4B C5B C6B 2(3) . . . . ? C7B C4B C5B C6B 179.8(16) . . . . ? C2B N1B C6B C5B -4(2) . . . . ? Ni1 N1B C6B C5B 168.6(13) 7_764 . . . ? C4B C5B C6B N1B 1(3) . . . . ? C3B C4B C7B C8B 21(2) . . . . ? C5B C4B C7B C8B -157.1(18) . . . . ? C3B C4B C7B C12B -149.0(15) . . . . ? C5B C4B C7B C12B 33(2) . . . . ? C12B C7B C8B C9B -2(3) . . . . ? C4B C7B C8B C9B -171.7(16) . . . . ? C7B C8B C9B C10B -1(3) . . . . ? C8B C9B C10B C11B 0(2) . . . . ? C8B C9B C10B C13B 178.9(14) . . . . ? C9B C10B C11B C12B 4(2) . . . . ? C13B C10B C11B C12B -175.1(13) . . . . ? C10B C11B C12B C7B -7(2) . . . . ? C8B C7B C12B C11B 6(2) . . . . ? C4B C7B C12B C11B 176.7(15) . . . . ? C9B C10B C13B O15B 178.9(13) . . . . ? C11B C10B C13B O15B -2.3(17) . . . . ? C9B C10B C13B O14B -7.9(19) . . . . ? C11B C10B C13B O14B 170.9(12) . . . . ? C9B C10B C13B Ni4 161(8) . . . . ? C11B C10B C13B Ni4 -20(10) . . . . ? N1C Ni4 C13B O15B 91.1(7) . . . . ? O14A Ni4 C13B O15B -162.8(6) . . . . ? N1D Ni4 C13B O15B -13.3(8) . . . . ? O14B Ni4 C13B O15B 171.6(11) . . . . ? O15A Ni4 C13B O15B -108.3(6) . . . . ? C13A Ni4 C13B O15B -134.0(6) . . . . ? O15B Ni4 C13B O14B -171.6(11) . . . . ? N1C Ni4 C13B O14B -80.4(7) . . . . ? O14A Ni4 C13B O14B 25.7(8) . . . . ? N1D Ni4 C13B O14B 175.1(6) . . . . ? O15A Ni4 C13B O14B 80.2(7) . . . . ? C13A Ni4 C13B O14B 54.4(7) . . . . ? O15B Ni4 C13B C10B 19(9) . . . . ? N1C Ni4 C13B C10B 110(9) . . . . ? O14A Ni4 C13B C10B -144(9) . . . . ? N1D Ni4 C13B C10B 6(9) . . . . ? O14B Ni4 C13B C10B -169(9) . . . . ? O15A Ni4 C13B C10B -89(9) . . . . ? C13A Ni4 C13B C10B -115(9) . . . . ? O15B C13B O14B Ni4 -8.2(10) . . . . ? C10B C13B O14B Ni4 178.7(10) . . . . ? O15B Ni4 O14B C13B 5.0(6) . . . . ? N1C Ni4 O14B C13B 102.2(7) . . . . ? O14A Ni4 O14B C13B -159.9(6) . . . . ? N1D Ni4 O14B C13B -10.7(13) . . . . ? O15A Ni4 O14B C13B -99.0(7) . . . . ? C13A Ni4 O14B C13B -130.3(7) . . . . ? O14B C13B O15B Ni4 8.7(11) . . . . ? C10B C13B O15B Ni4 -177.9(9) . . . . ? N1C Ni4 O15B C13B -93.2(7) . . . . ? O14A Ni4 O15B C13B 37.2(11) . . . . ? N1D Ni4 O15B C13B 169.3(7) . . . . ? O14B Ni4 O15B C13B -5.0(6) . . . . ? O15A Ni4 O15B C13B 75.0(7) . . . . ? C13A Ni4 O15B C13B 61.2(8) . . . . ? O15B Ni4 N1C C2C -177.3(10) . . . . ? O14A Ni4 N1C C2C 19.8(11) . . . . ? N1D Ni4 N1C C2C -80.6(11) . . . . ? O14B Ni4 N1C C2C 119.3(10) . . . . ? O15A Ni4 N1C C2C 36.1(18) . . . . ? C13B Ni4 N1C C2C 150.6(10) . . . . ? C13A Ni4 N1C C2C 27.5(12) . . . . ? O15B Ni4 N1C C6C 5.1(10) . . . . ? O14A Ni4 N1C C6C -157.8(10) . . . . ? N1D Ni4 N1C C6C 101.7(10) . . . . ? O14B Ni4 N1C C6C -58.3(10) . . . . ? O15A Ni4 N1C C6C -141.6(11) . . . . ? C13B Ni4 N1C C6C -27.1(10) . . . . ? C13A Ni4 N1C C6C -150.2(9) . . . . ? C6C N1C C2C C3C 1(2) . . . . ? Ni4 N1C C2C C3C -176.9(11) . . . . ? N1C C2C C3C C4C -2(2) . . . . ? C2C C3C C4C C5C 3(2) . . . . ? C2C C3C C4C C7C -175.4(13) . . . . ? C3C C4C C5C C6C -2.6(18) . . . . ? C7C C4C C5C C6C 175.8(12) . . . . ? C2C N1C C6C C5C -0.5(19) . . . . ? Ni4 N1C C6C C5C 177.3(9) . . . . ? C4C C5C C6C N1C 1.3(19) . . . . ? C3C C4C C7C C8C -25(2) . . . . ? C5C C4C C7C C8C 156.4(16) . . . . ? C3C C4C C7C C12C 156.5(13) . . . . ? C5C C4C C7C C12C -22(2) . . . . ? C12C C7C C8C C9C -9(3) . . . . ? C4C C7C C8C C9C 172.6(15) . . . . ? C7C C8C C9C C10C 5(3) . . . . ? C8C C9C C10C C11C -1(2) . . . . ? C8C C9C C10C C13C -172.2(15) . . . . ? C9C C10C C11C C12C 1(2) . . . . ? C13C C10C C11C C12C 172.1(11) . . . . ? C8C C7C C12C C11C 9(2) . . . . ? C4C C7C C12C C11C -172.6(12) . . . . ? C10C C11C C12C C7C -5(2) . . . . ? C9C C10C C13C O15C 167.4(13) . . . . ? C11C C10C C13C O15C -3.7(18) . . . . ? C9C C10C C13C O14C -11.6(19) . . . . ? C11C C10C C13C O14C 177.3(12) . . . . ? C9C C10C C13C Ni1 96(6) . . . 1_665 ? C11C C10C C13C Ni1 -75(6) . . . 1_665 ? O15C C13C O14C Ni1 -9.2(11) . . . 1_665 ? C10C C13C O14C Ni1 169.8(11) . . . 1_665 ? O14C C13C O15C Ni1 9.8(12) . . . 1_665 ? C10C C13C O15C Ni1 -169.2(10) . . . 1_665 ? O15B Ni4 N1D C2D -178.7(12) . . . . ? N1C Ni4 N1D C2D 83.3(13) . . . . ? O14A Ni4 N1D C2D -15.4(13) . . . . ? O14B Ni4 N1D C2D -164.6(12) . . . . ? O15A Ni4 N1D C2D -77.7(12) . . . . ? C13B Ni4 N1D C2D -171.6(12) . . . . ? C13A Ni4 N1D C2D -46.6(13) . . . . ? O15B Ni4 N1D C6D -11.4(9) . . . . ? N1C Ni4 N1D C6D -109.4(9) . . . . ? O14A Ni4 N1D C6D 151.9(9) . . . . ? O14B Ni4 N1D C6D 2.7(16) . . . . ? O15A Ni4 N1D C6D 89.6(9) . . . . ? C13B Ni4 N1D C6D -4.3(11) . . . . ? C13A Ni4 N1D C6D 120.7(9) . . . . ? C6D N1D C2D C3D 4(3) . . . . ? Ni4 N1D C2D C3D 170.6(14) . . . . ? N1D C2D C3D C4D -3(3) . . . . ? C2D C3D C4D C5D 1(3) . . . . ? C2D C3D C4D C7D -177.6(16) . . . . ? C3D C4D C5D C6D 2(2) . . . . ? C7D C4D C5D C6D -180.0(12) . . . . ? C2D N1D C6D C5D -1(2) . . . . ? Ni4 N1D C6D C5D -168.9(9) . . . . ? C4D C5D C6D N1D -1(2) . . . . ? C5D C4D C7D C8D 26(2) . . . . ? C3D C4D C7D C8D -155.6(17) . . . . ? C5D C4D C7D C12D -144.3(14) . . . . ? C3D C4D C7D C12D 34(2) . . . . ? C12D C7D C8D C9D -7(2) . . . . ? C4D C7D C8D C9D -177.2(14) . . . . ? C7D C8D C9D C10D 8(2) . . . . ? C8D C9D C10D C11D -8(2) . . . . ? C8D C9D C10D C13D 174.3(13) . . . . ? C9D C10D C11D C12D 8(2) . . . . ? C13D C10D C11D C12D -174.2(13) . . . . ? C10D C11D C12D C7D -8(2) . . . . ? C8D C7D C12D C11D 7(2) . . . . ? C4D C7D C12D C11D 178.1(14) . . . . ? C9D C10D C13D O14D -12.2(19) . . . . ? C11D C10D C13D O14D 170.5(12) . . . . ? C9D C10D C13D O15D 169.2(13) . . . . ? C11D C10D C13D O15D -8.0(17) . . . . ? C9D C10D C13D Ni3 145(10) . . . 7_864 ? C11D C10D C13D Ni3 -32(11) . . . 7_864 ? O15D C13D O14D Ni3 -3.6(11) . . . 7_864 ? C10D C13D O14D Ni3 177.8(10) . . . 7_864 ? O14D C13D O15D Ni3 3.9(11) . . . 7_864 ? C10D C13D O15D Ni3 -177.5(9) . . . 7_864 ? N1H Ni2 N1E C6E -83.9(10) 7_754 . . . ? O14F Ni2 N1E C6E 178.9(9) . . . . ? O15G Ni2 N1E C6E 16.3(10) . . . . ? O15F Ni2 N1E C6E 116.0(9) . . . . ? O14G Ni2 N1E C6E 30.4(16) . . . . ? C13G Ni2 N1E C6E 23.4(11) . . . . ? C13F Ni2 N1E C6E 147.5(9) . . . . ? N1H Ni2 N1E C2E 98.2(9) 7_754 . . . ? O14F Ni2 N1E C2E 1.0(9) . . . . ? O15G Ni2 N1E C2E -161.6(8) . . . . ? O15F Ni2 N1E C2E -61.9(9) . . . . ? O14G Ni2 N1E C2E -147.5(10) . . . . ? C13G Ni2 N1E C2E -154.5(8) . . . . ? C13F Ni2 N1E C2E -30.4(9) . . . . ? C6E N1E C2E C3E 2.1(18) . . . . ? Ni2 N1E C2E C3E -179.9(10) . . . . ? N1E C2E C3E C4E -2(2) . . . . ? C2E C3E C4E C5E -0.1(18) . . . . ? C2E C3E C4E C7E 176.8(12) . . . . ? C3E C4E C5E C6E 2.1(19) . . . . ? C7E C4E C5E C6E -174.8(12) . . . . ? C2E N1E C6E C5E 0.1(19) . . . . ? Ni2 N1E C6E C5E -177.9(11) . . . . ? C4E C5E C6E N1E -2(2) . . . . ? C3E C4E C7E C8E 159.7(14) . . . . ? C5E C4E C7E C8E -24(2) . . . . ? C3E C4E C7E C12E -21.7(19) . . . . ? C5E C4E C7E C12E 155.0(13) . . . . ? C12E C7E C8E C9E -8(2) . . . . ? C4E C7E C8E C9E 171.0(14) . . . . ? C7E C8E C9E C10E 3(3) . . . . ? C8E C9E C10E C11E 0(2) . . . . ? C8E C9E C10E C13E -172.7(14) . . . . ? C9E C10E C11E C12E 2(2) . . . . ? C13E C10E C11E C12E 173.8(11) . . . . ? C8E C7E C12E C11E 9(2) . . . . ? C4E C7E C12E C11E -169.9(11) . . . . ? C10E C11E C12E C7E -5.9(19) . . . . ? C9E C10E C13E O15E -6(2) . . . . ? C11E C10E C13E O15E -178.4(12) . . . . ? C9E C10E C13E O14E 169.9(13) . . . . ? C11E C10E C13E O14E -2.2(17) . . . . ? C9E C10E C13E Ni3 114(4) . . . . ? C11E C10E C13E Ni3 -59(5) . . . . ? N1A Ni3 C13E O15E 175.2(7) . . . . ? O15D Ni3 C13E O15E 26.4(9) 7_865 . . . ? O14E Ni3 C13E O15E -172.1(12) . . . . ? N1F Ni3 C13E O15E -79.3(8) 7_765 . . . ? O14D Ni3 C13E O15E 80.1(8) 7_865 . . . ? C13D Ni3 C13E O15E 56.5(8) 7_865 . . . ? N1A Ni3 C13E O14E -12.7(9) . . . . ? O15D Ni3 C13E O14E -161.5(6) 7_865 . . . ? N1F Ni3 C13E O14E 92.7(7) 7_765 . . . ? O14D Ni3 C13E O14E -107.9(7) 7_865 . . . ? O15E Ni3 C13E O14E 172.1(12) . . . . ? C13D Ni3 C13E O14E -131.5(7) 7_865 . . . ? N1A Ni3 C13E C10E 50(4) . . . . ? O15D Ni3 C13E C10E -99(4) 7_865 . . . ? O14E Ni3 C13E C10E 62(4) . . . . ? N1F Ni3 C13E C10E 155(4) 7_765 . . . ? O14D Ni3 C13E C10E -45(4) 7_865 . . . ? O15E Ni3 C13E C10E -126(4) . . . . ? C13D Ni3 C13E C10E -69(4) 7_865 . . . ? O15E C13E O14E Ni3 8.3(12) . . . . ? C10E C13E O14E Ni3 -168.0(9) . . . . ? N1A Ni3 O14E C13E 169.9(7) . . . . ? O15D Ni3 O14E C13E 39.7(12) 7_865 . . . ? N1F Ni3 O14E C13E -93.0(7) 7_765 . . . ? O14D Ni3 O14E C13E 75.2(7) 7_865 . . . ? O15E Ni3 O14E C13E -4.5(7) . . . . ? C13D Ni3 O14E C13E 64.3(8) 7_865 . . . ? O14E C13E O15E Ni3 -7.6(11) . . . . ? C10E C13E O15E Ni3 168.5(11) . . . . ? N1A Ni3 O15E C13E -10.2(15) . . . . ? O15D Ni3 O15E C13E -159.5(7) 7_865 . . . ? O14E Ni3 O15E C13E 4.7(7) . . . . ? N1F Ni3 O15E C13E 104.3(8) 7_765 . . . ? O14D Ni3 O15E C13E -99.2(8) 7_865 . . . ? C13D Ni3 O15E C13E -129.0(8) 7_865 . . . ? C6F N1F C2F C3F -4(2) . . . . ? Ni3 N1F C2F C3F 171.7(12) 7_764 . . . ? N1F C2F C3F C4F -2(2) . . . . ? C2F C3F C4F C5F 7(2) . . . . ? C2F C3F C4F C7F -175.0(14) . . . . ? C3F C4F C5F C6F -6(2) . . . . ? C7F C4F C5F C6F 176.3(13) . . . . ? C2F N1F C6F C5F 5.3(19) . . . . ? Ni3 N1F C6F C5F -170.4(10) 7_764 . . . ? C4F C5F C6F N1F -1(2) . . . . ? C5F C4F C7F C12F 33(2) . . . . ? C3F C4F C7F C12F -145.3(15) . . . . ? C5F C4F C7F C8F -142.2(16) . . . . ? C3F C4F C7F C8F 40(2) . . . . ? C12F C7F C8F C9F -5(2) . . . . ? C4F C7F C8F C9F 170.2(14) . . . . ? C7F C8F C9F C10F 2(2) . . . . ? C8F C9F C10F C11F 3(2) . . . . ? C8F C9F C10F C13F -178.1(13) . . . . ? C9F C10F C11F C12F -5(2) . . . . ? C13F C10F C11F C12F 175.8(12) . . . . ? C8F C7F C12F C11F 2(2) . . . . ? C4F C7F C12F C11F -172.4(13) . . . . ? C10F C11F C12F C7F 3(2) . . . . ? C9F C10F C13F O14F -8.1(18) . . . . ? C11F C10F C13F O14F 170.7(12) . . . . ? C9F C10F C13F O15F 171.5(12) . . . . ? C11F C10F C13F O15F -9.7(19) . . . . ? C9F C10F C13F Ni2 -34(10) . . . . ? C11F C10F C13F Ni2 145(9) . . . . ? N1H Ni2 C13F O14F -11.9(8) 7_754 . . . ? N1E Ni2 C13F O14F 92.0(7) . . . . ? O15G Ni2 C13F O14F -161.9(6) . . . . ? O15F Ni2 C13F O14F 176.9(11) . . . . ? O14G Ni2 C13F O14F -106.9(7) . . . . ? C13G Ni2 C13F O14F -132.6(6) . . . . ? N1H Ni2 C13F O15F 171.2(6) 7_754 . . . ? N1E Ni2 C13F O15F -84.9(7) . . . . ? O14F Ni2 C13F O15F -176.9(11) . . . . ? O15G Ni2 C13F O15F 21.2(8) . . . . ? O14G Ni2 C13F O15F 76.2(7) . . . . ? C13G Ni2 C13F O15F 50.6(7) . . . . ? N1H Ni2 C13F C10F 15(10) 7_754 . . . ? N1E Ni2 C13F C10F 119(10) . . . . ? O14F Ni2 C13F C10F 27(9) . . . . ? O15G Ni2 C13F C10F -135(10) . . . . ? O15F Ni2 C13F C10F -156(10) . . . . ? O14G Ni2 C13F C10F -80(10) . . . . ? C13G Ni2 C13F C10F -105(10) . . . . ? O15F C13F O14F Ni2 3.2(11) . . . . ? C10F C13F O14F Ni2 -177.1(10) . . . . ? N1H Ni2 O14F C13F 170.4(7) 7_754 . . . ? N1E Ni2 O14F C13F -92.3(7) . . . . ? O15G Ni2 O14F C13F 38.1(11) . . . . ? O15F Ni2 O14F C13F -1.8(6) . . . . ? O14G Ni2 O14F C13F 76.5(7) . . . . ? C13G Ni2 O14F C13F 62.6(8) . . . . ? O14F C13F O15F Ni2 -3.0(10) . . . . ? C10F C13F O15F Ni2 177.4(11) . . . . ? N1H Ni2 O15F C13F -18.7(13) 7_754 . . . ? N1E Ni2 O15F C13F 98.4(7) . . . . ? O14F Ni2 O15F C13F 1.8(6) . . . . ? O15G Ni2 O15F C13F -163.5(6) . . . . ? O14G Ni2 O15F C13F -103.0(7) . . . . ? C13G Ni2 O15F C13F -133.9(7) . . . . ? O15C Ni1 N1G C2G 14.8(11) 1_445 . . . ? O14H Ni1 N1G C2G 178.7(10) . . . . ? N1B Ni1 N1G C2G -84.8(11) 7_765 . . . ? O14C Ni1 N1G C2G 29.6(17) 1_445 . . . ? O15H Ni1 N1G C2G 115.6(10) . . . . ? C13H Ni1 N1G C2G 146.3(10) . . . . ? C13C Ni1 N1G C2G 22.2(12) 1_445 . . . ? O15C Ni1 N1G C6G -159.8(9) 1_445 . . . ? O14H Ni1 N1G C6G 4.1(10) . . . . ? N1B Ni1 N1G C6G 100.6(10) 7_765 . . . ? O14C Ni1 N1G C6G -145.0(10) 1_445 . . . ? O15H Ni1 N1G C6G -59.0(10) . . . . ? C13H Ni1 N1G C6G -28.3(10) . . . . ? C13C Ni1 N1G C6G -152.4(9) 1_445 . . . ? C6G N1G C2G C3G -1(2) . . . . ? Ni1 N1G C2G C3G -175.5(11) . . . . ? N1G C2G C3G C4G -1(2) . . . . ? C2G C3G C4G C5G 1.6(19) . . . . ? C2G C3G C4G C7G -175.2(12) . . . . ? C3G C4G C5G C6G 0.1(19) . . . . ? C7G C4G C5G C6G 176.8(12) . . . . ? C2G N1G C6G C5G 2.5(19) . . . . ? Ni1 N1G C6G C5G 177.4(10) . . . . ? C4G C5G C6G N1G -2(2) . . . . ? C5G C4G C7G C12G -23.3(18) . . . . ? C3G C4G C7G C12G 153.4(12) . . . . ? C5G C4G C7G C8G 158.7(13) . . . . ? C3G C4G C7G C8G -24.6(18) . . . . ? C12G C7G C8G C9G -6(2) . . . . ? C4G C7G C8G C9G 172.2(14) . . . . ? C7G C8G C9G C10G -1(3) . . . . ? C8G C9G C10G C11G 5(2) . . . . ? C8G C9G C10G C13G -170.8(14) . . . . ? C9G C10G C11G C12G -2.1(19) . . . . ? C13G C10G C11G C12G 174.1(11) . . . . ? C8G C7G C12G C11G 8.8(19) . . . . ? C4G C7G C12G C11G -169.2(11) . . . . ? C10G C11G C12G C7G -4.9(17) . . . . ? C11G C10G C13G O15G -2.4(17) . . . . ? C9G C10G C13G O15G 173.7(13) . . . . ? C11G C10G C13G O14G 180.0(12) . . . . ? C9G C10G C13G O14G -4(2) . . . . ? C11G C10G C13G Ni2 -69(5) . . . . ? C9G C10G C13G Ni2 108(4) . . . . ? N1H Ni2 C13G O15G 92.1(7) 7_754 . . . ? N1E Ni2 C13G O15G -13.7(9) . . . . ? O14F Ni2 C13G O15G -161.6(6) . . . . ? O15F Ni2 C13G O15G -108.4(7) . . . . ? O14G Ni2 C13G O15G 171.2(12) . . . . ? C13F Ni2 C13G O15G -132.3(7) . . . . ? N1H Ni2 C13G O14G -79.1(8) 7_754 . . . ? N1E Ni2 C13G O14G 175.1(7) . . . . ? O14F Ni2 C13G O14G 27.2(9) . . . . ? O15G Ni2 C13G O14G -171.2(12) . . . . ? O15F Ni2 C13G O14G 80.4(7) . . . . ? C13F Ni2 C13G O14G 56.6(8) . . . . ? N1H Ni2 C13G C10G 164(4) 7_754 . . . ? N1E Ni2 C13G C10G 58(4) . . . . ? O14F Ni2 C13G C10G -90(4) . . . . ? O15G Ni2 C13G C10G 72(4) . . . . ? O15F Ni2 C13G C10G -36(4) . . . . ? O14G Ni2 C13G C10G -117(5) . . . . ? C13F Ni2 C13G C10G -60(4) . . . . ? O15G C13G O14G Ni2 -9.1(12) . . . . ? C10G C13G O14G Ni2 168.4(10) . . . . ? N1H Ni2 O14G C13G 104.2(8) 7_754 . . . ? N1E Ni2 O14G C13G -10.7(15) . . . . ? O14F Ni2 O14G C13G -158.9(7) . . . . ? O15G Ni2 O14G C13G 5.1(7) . . . . ? O15F Ni2 O14G C13G -98.1(7) . . . . ? C13F Ni2 O14G C13G -128.8(8) . . . . ? O14G C13G O15G Ni2 9.7(13) . . . . ? C10G C13G O15G Ni2 -167.8(9) . . . . ? N1H Ni2 O15G C13G -93.2(7) 7_754 . . . ? N1E Ni2 O15G C13G 169.1(7) . . . . ? O14F Ni2 O15G C13G 38.6(11) . . . . ? O15F Ni2 O15G C13G 73.9(7) . . . . ? O14G Ni2 O15G C13G -5.2(7) . . . . ? C13F Ni2 O15G C13G 62.8(8) . . . . ? C6H N1H C2H C3H 5.6(19) . . . . ? Ni2 N1H C2H C3H -170.4(10) 7_755 . . . ? N1H C2H C3H C4H -1(2) . . . . ? C2H C3H C4H C5H -5(2) . . . . ? C2H C3H C4H C7H 178.0(13) . . . . ? C3H C4H C5H C6H 5(2) . . . . ? C7H C4H C5H C6H -177.6(13) . . . . ? C2H N1H C6H C5H -5(2) . . . . ? Ni2 N1H C6H C5H 170.4(11) 7_755 . . . ? C4H C5H C6H N1H 0(2) . . . . ? C3H C4H C7H C8H 27(2) . . . . ? C5H C4H C7H C8H -149.8(15) . . . . ? C3H C4H C7H C12H -141.3(15) . . . . ? C5H C4H C7H C12H 42(2) . . . . ? C12H C7H C8H C9H 2(2) . . . . ? C4H C7H C8H C9H -167.0(15) . . . . ? C7H C8H C9H C10H -2(3) . . . . ? C10H C11H C12H C7H -7(2) . . . . ? C8H C7H C12H C11H 3(2) . . . . ? C4H C7H C12H C11H 171.9(13) . . . . ? N1G Ni1 C13H O15H -84.2(7) . . . . ? O15C Ni1 C13H O15H 23.5(8) 1_445 . . . ? O14H Ni1 C13H O15H -175.6(10) . . . . ? N1B Ni1 C13H O15H 171.4(6) 7_765 . . . ? O14C Ni1 C13H O15H 77.4(7) 1_445 . . . ? C13C Ni1 C13H O15H 51.7(7) 1_445 . . . ? N1G Ni1 C13H O14H 91.5(6) . . . . ? O15C Ni1 C13H O14H -160.9(5) 1_445 . . . ? N1B Ni1 C13H O14H -13.0(8) 7_765 . . . ? O14C Ni1 C13H O14H -106.9(6) 1_445 . . . ? O15H Ni1 C13H O14H 175.6(10) . . . . ? C13C Ni1 C13H O14H -132.6(6) 1_445 . . . ? N1G Ni1 C13H C10H 134(8) . . . . ? O15C Ni1 C13H C10H -119(8) 1_445 . . . ? O14H Ni1 C13H C10H 42(8) . . . . ? N1B Ni1 C13H C10H 29(8) 7_765 . . . ? O14C Ni1 C13H C10H -65(8) 1_445 . . . ? O15H Ni1 C13H C10H -142(8) . . . . ? C13C Ni1 C13H C10H -90(8) 1_445 . . . ? O15H C13H O14H Ni1 4.7(11) . . . . ? C10H C13H O14H Ni1 -175.3(9) . . . . ? N1G Ni1 O14H C13H -93.4(7) . . . . ? O15C Ni1 O14H C13H 41.3(11) 1_445 . . . ? N1B Ni1 O14H C13H 169.6(6) 7_765 . . . ? O14C Ni1 O14H C13H 76.0(7) 1_445 . . . ? O15H Ni1 O14H C13H -2.5(6) . . . . ? C13C Ni1 O14H C13H 62.7(8) 1_445 . . . ? O14H C13H O15H Ni1 -4.4(11) . . . . ? C10H C13H O15H Ni1 175.5(10) . . . . ? N1G Ni1 O15H C13H 99.4(7) . . . . ? O15C Ni1 O15H C13H -161.6(6) 1_445 . . . ? O14H Ni1 O15H C13H 2.6(6) . . . . ? N1B Ni1 O15H C13H -17.8(12) 7_765 . . . ? O14C Ni1 O15H C13H -101.3(7) 1_445 . . . ? C13C Ni1 O15H C13H -132.5(7) 1_445 . . . ? O1J C2J N3J C5J 7(4) . . . . ? O1J C2J N3J C4J 179(2) . . . . ? O1K C2K N3K C5K -174(4) . . . . ? O1K C2K N3K C4K 1(5) . . . . ? O1L C2L N3L C4L 6(4) . . . . ? O1L C2L N3L C5L 177(2) . . . . ? O1M C2M N3M C4M -7(5) . . . . ? O1M C2M N3M C5M -176(3) . . . . ? C8H C9H C10H C11H -2(2) . . . . ? C8H C9H C10H C13H 177.2(14) . . . . ? C12H C11H C10H C9H 6.1(19) . . . . ? C12H C11H C10H C13H -172.9(12) . . . . ? O15H C13H C10H C9H -3.8(19) . . . . ? O14H C13H C10H C9H 176.1(12) . . . . ? Ni1 C13H C10H C9H 136(8) . . . . ? O15H C13H C10H C11H 175.0(11) . . . . ? O14H C13H C10H C11H -5.0(17) . . . . ? Ni1 C13H C10H C11H -45(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.067 _refine_diff_density_min -1.942 _refine_diff_density_rms 0.197