# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Enrique Colacio' _publ_contact_author_email ECOLACIO@UGR.ES _publ_section_title ; Enhanced Ferromagnetic interaction in Metallacyclic Complexes Incorporating m-phenylenediamidato bridges. Design, Magneto-Structural Characterisation and Theoretical study ; loop_ _publ_author_name 'Enrique Colacio' 'Joan Cano' 'Juan Herrera' 'Antonio J. Mota' 'M Angeles Palacios' ; A.Rodriguez-Dieguez ; 'A Sironi' # Attachment 'Colacio1234.cif' data_compound1 _database_code_depnum_ccdc_archive 'CCDC 721057' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 Cu2 N8 O4, 2(H2 O)' _chemical_formula_sum 'C36 H28 Cu2 N8 O6' _chemical_formula_weight 795.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6561(17) _cell_length_b 10.239(2) _cell_length_c 11.330(2) _cell_angle_alpha 88.28(3) _cell_angle_beta 70.29(3) _cell_angle_gamma 71.76(3) _cell_volume 894.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1030 _cell_measurement_theta_min 2.508 _cell_measurement_theta_max 25.235 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 406 _exptl_absorpt_coefficient_mu 1.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.945 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3721 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.1730 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2780 _reflns_number_gt 1353 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker APEXII' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1104P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2780 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1567 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2373 _refine_ls_wR_factor_gt 0.2116 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 Cu1 Cu 0.88301(18) 0.09761(13) 0.28915(13) 0.0409(5) Uani 1 1 d . . . O1W O 0.3404(11) 0.4436(8) 0.8561(9) 0.074(3) Uani 1 1 d . . . H1A H 0.4262 0.4187 0.7877 0.089 Uiso 1 1 d R . . H1B H 0.2966 0.3787 0.8669 0.089 Uiso 1 1 d R . . N1 N 1.0971(11) -0.0337(8) 0.1553(8) 0.036(2) Uani 1 1 d . . . C2 C 1.2654(15) -0.0452(11) 0.1278(10) 0.045(3) Uani 1 1 d . . . H2 H 1.2907 0.0239 0.1618 0.055 Uiso 1 1 calc R . . C3 C 1.4063(14) -0.1559(11) 0.0504(11) 0.046(3) Uani 1 1 d . . . H3 H 1.5204 -0.1600 0.0348 0.055 Uiso 1 1 calc R . . C4 C 1.3664(15) -0.2615(10) -0.0029(11) 0.046(3) Uani 1 1 d . . . H4 H 1.4550 -0.3366 -0.0529 0.056 Uiso 1 1 calc R . . C5 C 1.1933(14) -0.2500(10) 0.0212(10) 0.038(3) Uani 1 1 d . . . H5 H 1.1657 -0.3143 -0.0172 0.046 Uiso 1 1 calc R . . C6 C 1.0583(13) -0.1387(10) 0.1056(10) 0.033(3) Uani 1 1 d . . . C7 C 0.8626(14) -0.1252(10) 0.1530(10) 0.038(3) Uani 1 1 d . . . O8 O 0.8176(10) -0.2124(7) 0.1038(7) 0.051(2) Uani 1 1 d . . . N9 N 0.7614(11) -0.0207(8) 0.2441(8) 0.037(2) Uani 1 1 d . . . C10 C 0.5765(14) 0.0040(10) 0.3068(10) 0.037(3) Uani 1 1 d . . . C11 C 0.5073(13) -0.1028(9) 0.3708(9) 0.031(3) Uani 1 1 d . . . H11 H 0.5798 -0.1935 0.3615 0.037 Uiso 1 1 calc R . . C12 C 0.4597(13) 0.1413(10) 0.3165(10) 0.034(3) Uani 1 1 d . . . H12 H 0.5022 0.2090 0.2744 0.041 Uiso 1 1 calc R . . C13 C 0.2830(14) 0.1760(11) 0.3880(10) 0.041(3) Uani 1 1 d . . . H13 H 0.2088 0.2653 0.3927 0.050 Uiso 1 1 calc R . . C14 C 0.7824(14) -0.0708(10) 0.5454(10) 0.041(3) Uani 1 1 d . . . H14 H 0.8994 -0.0935 0.4970 0.049 Uiso 1 1 calc R . . C15 C 0.6701(14) 0.0676(10) 0.5529(10) 0.037(3) Uani 1 1 d . . . N16 N 0.7453(11) 0.1594(8) 0.4689(8) 0.040(2) Uani 1 1 d . . . O17 O 0.6390(13) 0.3552(9) 0.6178(8) 0.087(3) Uani 1 1 d . . . C18 C 0.7229(13) 0.2908(11) 0.5089(10) 0.043(3) Uani 1 1 d . . . C19 C 0.8298(13) 0.3605(10) 0.4021(11) 0.038(3) Uani 1 1 d . . . C20 C 0.8345(15) 0.4965(11) 0.4209(12) 0.051(3) Uani 1 1 d . . . H20 H 0.7636 0.5504 0.4958 0.061 Uiso 1 1 calc R . . C21 C 0.9475(16) 0.5484(11) 0.3253(12) 0.056(4) Uani 1 1 d . . . H21 H 0.9544 0.6355 0.3375 0.067 Uiso 1 1 calc R . . C22 C 1.0498(16) 0.4669(12) 0.2106(11) 0.053(3) Uani 1 1 d . . . H22 H 1.1250 0.4993 0.1464 0.064 Uiso 1 1 calc R . . C23 C 1.0357(14) 0.3328(11) 0.1952(10) 0.040(3) Uani 1 1 d . . . H23 H 1.1011 0.2788 0.1197 0.048 Uiso 1 1 calc R . . N24 N 0.9281(11) 0.2839(8) 0.2893(8) 0.039(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0491(9) 0.0315(8) 0.0463(10) -0.0013(6) -0.0115(7) -0.0239(6) O1W 0.075(6) 0.052(5) 0.090(7) -0.018(5) -0.016(5) -0.024(5) N1 0.039(6) 0.030(5) 0.044(6) 0.006(4) -0.011(5) -0.020(4) C2 0.049(8) 0.038(6) 0.053(8) 0.002(6) -0.019(7) -0.017(6) C3 0.035(7) 0.045(7) 0.058(8) 0.003(6) -0.014(6) -0.014(6) C4 0.046(8) 0.025(6) 0.049(8) -0.002(5) 0.000(6) -0.002(5) C5 0.045(7) 0.031(6) 0.047(7) 0.005(5) -0.020(6) -0.019(5) C6 0.046(7) 0.027(5) 0.037(7) 0.008(5) -0.020(6) -0.021(5) C7 0.046(7) 0.032(6) 0.038(7) 0.007(5) -0.015(6) -0.015(5) O8 0.061(5) 0.047(5) 0.048(5) -0.014(4) -0.007(4) -0.033(4) N9 0.040(6) 0.035(5) 0.033(5) -0.005(4) -0.003(5) -0.019(4) C10 0.044(7) 0.030(6) 0.038(7) -0.004(5) -0.013(6) -0.015(5) C11 0.035(6) 0.017(5) 0.039(6) -0.004(5) -0.011(6) -0.008(5) C12 0.034(7) 0.025(6) 0.042(7) 0.000(5) -0.015(6) -0.006(5) C13 0.047(7) 0.030(6) 0.054(8) 0.000(6) -0.027(7) -0.011(5) C14 0.037(7) 0.034(6) 0.051(8) -0.003(6) -0.012(6) -0.012(5) C15 0.043(7) 0.035(6) 0.037(7) -0.011(5) -0.013(6) -0.018(5) N16 0.046(6) 0.030(5) 0.043(6) 0.006(4) -0.006(5) -0.023(4) O17 0.120(8) 0.062(6) 0.061(6) -0.027(5) 0.024(6) -0.063(6) C18 0.037(7) 0.037(6) 0.043(8) -0.015(6) 0.008(6) -0.018(5) C19 0.033(6) 0.030(6) 0.048(7) 0.002(5) -0.006(6) -0.013(5) C20 0.064(8) 0.033(6) 0.058(8) 0.004(6) -0.021(7) -0.019(6) C21 0.073(9) 0.028(6) 0.077(10) 0.012(7) -0.029(8) -0.027(6) C22 0.082(9) 0.044(7) 0.049(8) 0.017(6) -0.028(7) -0.037(7) C23 0.040(7) 0.046(7) 0.039(7) 0.006(6) -0.011(6) -0.025(6) N24 0.048(6) 0.032(5) 0.037(6) 0.004(5) -0.011(5) -0.017(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N16 1.984(8) . ? Cu1 N9 2.008(8) . ? Cu1 N1 2.051(8) . ? Cu1 N24 2.063(8) . ? O1W H1A 0.8500 . ? O1W H1B 0.8500 . ? N1 C2 1.350(12) . ? N1 C6 1.406(11) . ? C2 C3 1.419(14) . ? C2 H2 0.9300 . ? C3 C4 1.437(14) . ? C3 H3 0.9300 . ? C4 C5 1.397(14) . ? C4 H4 0.9300 . ? C5 C6 1.434(13) . ? C5 H5 0.9300 . ? C6 C7 1.556(14) . ? C7 O8 1.286(11) . ? C7 N9 1.359(12) . ? N9 C10 1.456(12) . ? C10 C12 1.434(14) . ? C10 C11 1.466(13) . ? C11 C15 1.419(13) 2_656 ? C11 H11 0.9300 . ? C12 C13 1.401(13) . ? C12 H12 0.9300 . ? C13 C14 1.446(14) 2_656 ? C13 H13 0.9300 . ? C14 C15 1.432(14) . ? C14 C13 1.446(14) 2_656 ? C14 H14 0.9300 . ? C15 C11 1.419(13) 2_656 ? C15 N16 1.457(13) . ? N16 C18 1.366(12) . ? O17 C18 1.276(12) . ? C18 C19 1.561(15) . ? C19 N24 1.371(12) . ? C19 C20 1.431(13) . ? C20 C21 1.410(15) . ? C20 H20 0.9300 . ? C21 C22 1.412(15) . ? C21 H21 0.9300 . ? C22 C23 1.436(14) . ? C22 H22 0.9300 . ? C23 N24 1.358(13) . ? C23 H23 0.9300 . ? 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 N16 Cu1 N9 103.2(3) . . ? N16 Cu1 N1 149.5(4) . . ? N9 Cu1 N1 83.2(3) . . ? N16 Cu1 N24 83.1(3) . . ? N9 Cu1 N24 150.2(4) . . ? N1 Cu1 N24 106.3(3) . . ? H1A O1W H1B 105.0 . . ? C2 N1 C6 118.1(8) . . ? C2 N1 Cu1 128.6(7) . . ? C6 N1 Cu1 112.1(6) . . ? N1 C2 C3 124.2(10) . . ? N1 C2 H2 117.9 . . ? C3 C2 H2 117.9 . . ? C2 C3 C4 117.7(10) . . ? C2 C3 H3 121.2 . . ? C4 C3 H3 121.2 . . ? C5 C4 C3 119.3(9) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 119.6(9) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? N1 C6 C5 120.9(9) . . ? N1 C6 C7 114.7(8) . . ? C5 C6 C7 124.4(8) . . ? O8 C7 N9 128.7(10) . . ? O8 C7 C6 117.5(9) . . ? N9 C7 C6 113.8(9) . . ? C7 N9 C10 122.5(8) . . ? C7 N9 Cu1 115.9(7) . . ? C10 N9 Cu1 121.6(6) . . ? C12 C10 N9 118.5(9) . . ? C12 C10 C11 118.8(9) . . ? N9 C10 C11 122.4(9) . . ? C15 C11 C10 120.0(9) 2_656 . ? C15 C11 H11 120.0 2_656 . ? C10 C11 H11 120.0 . . ? C13 C12 C10 121.6(10) . . ? C13 C12 H12 119.2 . . ? C10 C12 H12 119.2 . . ? C12 C13 C14 119.1(10) . 2_656 ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 2_656 . ? C15 C14 C13 121.1(10) . 2_656 ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 2_656 . ? C11 C15 C14 119.4(10) 2_656 . ? C11 C15 N16 124.3(9) 2_656 . ? C14 C15 N16 116.0(9) . . ? C18 N16 C15 122.1(9) . . ? C18 N16 Cu1 117.2(7) . . ? C15 N16 Cu1 120.6(6) . . ? O17 C18 N16 129.5(10) . . ? O17 C18 C19 119.5(9) . . ? N16 C18 C19 110.9(8) . . ? N24 C19 C20 120.1(10) . . ? N24 C19 C18 117.6(8) . . ? C20 C19 C18 122.2(9) . . ? C21 C20 C19 119.6(10) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 119.3(10) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C21 C22 C23 118.8(10) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? N24 C23 C22 121.0(10) . . ? N24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 N24 C19 121.2(9) . . ? C23 N24 Cu1 128.2(7) . . ? C19 N24 Cu1 110.6(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1A O17 0.85 2.11 2.961(12) 179.5 . O1W H1B O8 0.85 2.19 3.037(10) 179.5 2_656 _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.741 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.125 data_compound2 _database_code_depnum_ccdc_archive 'CCDC 721058' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H36 F6 N12 Ni2 O6 P' _chemical_formula_weight 1211.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 13.790(2) _cell_length_b 13.790(2) _cell_length_c 21.995(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3622.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5120 _cell_measurement_theta_min 2.518 _cell_measurement_theta_max 21.776 _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.111 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1234 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.975 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33082 _diffrn_reflns_av_R_equivalents 0.0739 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 23.62 _reflns_number_total 1869 _reflns_number_gt 1436 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker APEXII' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+0.4652P] 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 SHELXL _refine_ls_extinction_coef 0.0018(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1869 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.6667 0.3333 0.59242(3) 0.0519(3) Uani 1 3 d S . . N1 N 0.5357(2) 0.2076(2) 0.54004(11) 0.0614(7) Uani 1 1 d . . . C2 C 0.5440(3) 0.1607(3) 0.48818(16) 0.0750(10) Uani 1 1 d . . . H2 H 0.6147 0.1822 0.4727 0.090 Uiso 1 1 calc R . . C3 C 0.4513(4) 0.0821(4) 0.4573(2) 0.0963(14) Uani 1 1 d . . . H3 H 0.4590 0.0512 0.4213 0.116 Uiso 1 1 calc R . . C4 C 0.3479(4) 0.0501(4) 0.4803(2) 0.1000(14) Uani 1 1 d . . . H4 H 0.2841 -0.0022 0.4597 0.120 Uiso 1 1 calc R . . C5 C 0.3385(4) 0.0955(3) 0.53403(18) 0.0820(11) Uani 1 1 d . . . H5 H 0.2685 0.0731 0.5508 0.098 Uiso 1 1 calc R . . C6 C 0.4336(3) 0.1742(3) 0.56238(16) 0.0597(9) Uani 1 1 d . . . C7 C 0.4291(3) 0.2312(3) 0.61990(15) 0.0572(8) Uani 1 1 d . . . O8 O 0.33308(19) 0.1970(2) 0.64310(12) 0.0848(8) Uani 1 1 d . . . N9 N 0.5255(2) 0.3102(2) 0.63918(10) 0.0515(6) Uani 1 1 d . . . C10 C 0.5261(2) 0.3645(3) 0.69527(13) 0.0503(8) Uani 1 1 d . . . C11 C 0.5141(3) 0.3089(4) 0.7500 0.0506(10) Uani 1 2 d S . . H11 H 0.4982 0.2349 0.7500 0.061 Uiso 1 2 calc SR . . C12 C 0.5445(3) 0.4712(3) 0.69522(14) 0.0571(8) Uani 1 1 d . . . H12 H 0.5521 0.5083 0.6587 0.069 Uiso 1 1 calc R . . C13 C 0.5516(4) 0.5241(4) 0.7500 0.0644(13) Uani 1 2 d S . . H13 H 0.5614 0.5958 0.7500 0.077 Uiso 1 2 calc SR . . P1 P 0.0000 0.0000 0.5000 0.1307(14) Uani 1 6 d S . . F1 F 0.1001(4) 0.0330(5) 0.4590(3) 0.236(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0594(4) 0.0594(4) 0.0371(4) 0.000 0.000 0.02968(18) N1 0.0772(19) 0.0699(17) 0.0408(15) -0.0022(12) -0.0035(13) 0.0396(15) C2 0.081(2) 0.087(3) 0.059(2) -0.018(2) -0.0106(19) 0.044(2) C3 0.112(4) 0.095(3) 0.079(3) -0.041(2) -0.024(3) 0.051(3) C4 0.093(3) 0.086(3) 0.105(3) -0.043(3) -0.035(3) 0.033(3) C5 0.077(3) 0.077(3) 0.078(3) -0.016(2) -0.013(2) 0.028(2) C6 0.065(2) 0.0572(19) 0.0519(19) -0.0012(15) -0.0105(16) 0.0272(17) C7 0.057(2) 0.064(2) 0.0490(18) 0.0009(16) -0.0041(16) 0.0291(17) O8 0.0549(15) 0.110(2) 0.0709(17) -0.0108(15) 0.0013(12) 0.0276(14) N9 0.0600(16) 0.0612(15) 0.0379(13) -0.0042(11) -0.0056(11) 0.0337(13) C10 0.0486(17) 0.063(2) 0.0434(17) -0.0003(14) -0.0021(13) 0.0314(15) C11 0.048(2) 0.061(3) 0.044(2) 0.000 0.000 0.028(2) C12 0.069(2) 0.073(2) 0.0443(17) 0.0065(15) 0.0001(14) 0.0461(18) C13 0.082(3) 0.064(3) 0.062(3) 0.000 0.000 0.048(3) P1 0.0986(15) 0.0986(15) 0.195(4) 0.000 0.000 0.0493(8) F1 0.156(4) 0.218(5) 0.335(7) 0.031(6) 0.069(4) 0.095(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N9 2.080(2) . ? Ni1 N9 2.080(2) 2_655 ? Ni1 N9 2.080(2) 3_665 ? Ni1 N1 2.112(3) 2_655 ? Ni1 N1 2.112(3) 3_665 ? Ni1 N1 2.112(3) . ? N1 C6 1.337(4) . ? N1 C2 1.344(4) . ? C2 C3 1.372(5) . ? C2 H2 0.9300 . ? C3 C4 1.361(6) . ? C3 H3 0.9300 . ? C4 C5 1.374(6) . ? C4 H4 0.9300 . ? C5 C6 1.365(5) . ? C5 H5 0.9300 . ? C6 C7 1.507(5) . ? C7 O8 1.269(4) . ? C7 N9 1.298(4) . ? N9 C10 1.441(4) . ? C10 C12 1.362(4) . ? C10 C11 1.392(4) . ? C11 C10 1.392(4) 10_557 ? C11 H11 0.9300 . ? C12 C13 1.386(4) . ? C12 H12 0.9300 . ? C13 C12 1.386(4) 10_557 ? C13 H13 0.9300 . ? P1 F1 1.516(5) . ? P1 F1 1.516(5) 9_556 ? P1 F1 1.516(5) 3 ? P1 F1 1.516(5) 2 ? P1 F1 1.516(5) 8_556 ? P1 F1 1.516(5) 7_556 ? 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 N9 Ni1 N9 97.65(8) . 2_655 ? N9 Ni1 N9 97.65(8) . 3_665 ? N9 Ni1 N9 97.65(8) 2_655 3_665 ? N9 Ni1 N1 170.15(10) . 2_655 ? N9 Ni1 N1 78.08(10) 2_655 2_655 ? N9 Ni1 N1 91.74(10) 3_665 2_655 ? N9 Ni1 N1 91.74(10) . 3_665 ? N9 Ni1 N1 170.15(10) 2_655 3_665 ? N9 Ni1 N1 78.08(10) 3_665 3_665 ? N1 Ni1 N1 93.09(10) 2_655 3_665 ? N9 Ni1 N1 78.08(10) . . ? N9 Ni1 N1 91.74(10) 2_655 . ? N9 Ni1 N1 170.15(10) 3_665 . ? N1 Ni1 N1 93.09(10) 2_655 . ? N1 Ni1 N1 93.09(10) 3_665 . ? C6 N1 C2 118.3(3) . . ? C6 N1 Ni1 113.8(2) . . ? C2 N1 Ni1 127.9(3) . . ? N1 C2 C3 122.0(4) . . ? N1 C2 H2 119.0 . . ? C3 C2 H2 119.0 . . ? C4 C3 C2 118.9(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 118.9(4) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? N1 C6 C5 122.3(3) . . ? N1 C6 C7 116.1(3) . . ? C5 C6 C7 121.6(3) . . ? O8 C7 N9 128.4(3) . . ? O8 C7 C6 116.8(3) . . ? N9 C7 C6 114.8(3) . . ? C7 N9 C10 116.9(3) . . ? C7 N9 Ni1 117.1(2) . . ? C10 N9 Ni1 125.59(19) . . ? C12 C10 C11 120.1(3) . . ? C12 C10 N9 120.7(3) . . ? C11 C10 N9 119.0(3) . . ? C10 C11 C10 119.7(4) . 10_557 ? C10 C11 H11 120.1 . . ? C10 C11 H11 120.1 10_557 . ? C10 C12 C13 119.5(3) . . ? C10 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C12 C13 C12 120.8(4) . 10_557 ? C12 C13 H13 119.6 . . ? C12 C13 H13 119.6 10_557 . ? F1 P1 F1 91.8(4) . 9_556 ? F1 P1 F1 88.2(4) . 3 ? F1 P1 F1 180.0(3) 9_556 3 ? F1 P1 F1 88.2(4) . 2 ? F1 P1 F1 91.8(4) 9_556 2 ? F1 P1 F1 88.2(4) 3 2 ? F1 P1 F1 91.8(4) . 8_556 ? F1 P1 F1 88.2(4) 9_556 8_556 ? F1 P1 F1 91.8(4) 3 8_556 ? F1 P1 F1 180.0(4) 2 8_556 ? F1 P1 F1 179.998(1) . 7_556 ? F1 P1 F1 88.2(4) 9_556 7_556 ? F1 P1 F1 91.8(4) 3 7_556 ? F1 P1 F1 91.8(4) 2 7_556 ? F1 P1 F1 88.2(4) 8_556 7_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.62 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.304 _refine_diff_density_min -0.587 _refine_diff_density_rms 0.063 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.015 -0.009 0.250 715 229 ' ' 2 -0.013 -0.008 0.750 715 231 ' ' _platon_squeeze_details ; ; data_compound4 _database_code_depnum_ccdc_archive 'CCDC 721060' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H36 Ag2 N12 Ni2 O7, 11(H2O)' _chemical_formula_sum 'C54 H60 Ag2 N12 Ni2 O18' _chemical_formula_weight 1498.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Orthorrhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 18.279(4) _cell_length_b 20.892(4) _cell_length_c 14.844(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5669(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3928 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 19.35 _exptl_crystal_description prismatic _exptl_crystal_colour green _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2952.0 _exptl_absorpt_coefficient_mu 1.421 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32613 _diffrn_reflns_av_R_equivalents 0.0753 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 22.90 _reflns_number_total 4011 _reflns_number_gt 3005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker APEXII' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+14.3863P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4011 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Ag1 Ag 0.03593(3) 0.2500 0.20109(4) 0.0541(2) Uani 1 2 d S . . Ag2 Ag 0.10664(3) 0.2500 0.38692(4) 0.0482(2) Uani 1 2 d S . . Ni1 Ni 0.30021(3) 0.08349(3) 0.20672(4) 0.02693(17) Uani 1 1 d . . . N1A N 0.2024(2) 0.02877(18) 0.1968(3) 0.0323(10) Uani 1 1 d . . . C2A C 0.1930(3) -0.0299(3) 0.1629(4) 0.0413(14) Uani 1 1 d . . . H2A H 0.2327 -0.0503 0.1363 0.050 Uiso 1 1 calc R . . C3A C 0.1269(3) -0.0614(3) 0.1658(4) 0.0487(15) Uani 1 1 d . . . H3A H 0.1229 -0.1031 0.1443 0.058 Uiso 1 1 calc R . . C4A C 0.0671(3) -0.0308(3) 0.2004(4) 0.0469(15) Uani 1 1 d . . . H4A H 0.0217 -0.0509 0.2015 0.056 Uiso 1 1 calc R . . C5A C 0.0754(3) 0.0309(3) 0.2340(3) 0.0388(13) Uani 1 1 d . . . H5A H 0.0354 0.0532 0.2566 0.047 Uiso 1 1 calc R . . C6A C 0.1436(3) 0.0582(2) 0.2331(3) 0.0293(12) Uani 1 1 d . . . C7A C 0.1576(3) 0.1214(2) 0.2775(3) 0.0331(12) Uani 1 1 d . . . O8A O 0.10253(17) 0.15299(17) 0.3034(2) 0.0445(9) Uani 1 1 d . . . N9A N 0.2278(2) 0.13436(18) 0.2870(2) 0.0283(9) Uani 1 1 d . . . C10A C 0.2452(2) 0.1924(2) 0.3321(3) 0.0244(11) Uani 1 1 d . . . C11A C 0.2267(3) 0.2500 0.2927(4) 0.0273(16) Uani 1 2 d S . . H11A H 0.2012 0.2500 0.2385 0.033 Uiso 1 2 calc SR . . C12A C 0.2825(2) 0.1924(2) 0.4123(3) 0.0296(12) Uani 1 1 d . . . H12A H 0.2951 0.1540 0.4400 0.036 Uiso 1 1 calc R . . C13A C 0.3012(4) 0.2500 0.4516(4) 0.0328(18) Uani 1 2 d S . . H13A H 0.3268 0.2500 0.5057 0.039 Uiso 1 2 calc SR . . N1B N 0.3555(2) 0.02734(18) 0.1126(3) 0.0312(10) Uani 1 1 d . . . C2B C 0.3899(3) -0.0282(2) 0.1268(4) 0.0408(14) Uani 1 1 d . . . H2B H 0.3942 -0.0432 0.1856 0.049 Uiso 1 1 calc R . . C3B C 0.4191(3) -0.0637(3) 0.0585(4) 0.0536(16) Uani 1 1 d . . . H3B H 0.4409 -0.1030 0.0703 0.064 Uiso 1 1 calc R . . C4B C 0.4157(3) -0.0408(3) -0.0272(4) 0.0611(18) Uani 1 1 d . . . H4B H 0.4353 -0.0641 -0.0747 0.073 Uiso 1 1 calc R . . C5B C 0.3827(3) 0.0175(3) -0.0424(4) 0.0460(15) Uani 1 1 d . . . H5B H 0.3808 0.0345 -0.1002 0.055 Uiso 1 1 calc R . . C6B C 0.3527(2) 0.0500(2) 0.0287(3) 0.0299(12) Uani 1 1 d . . . C7B C 0.3134(2) 0.1127(2) 0.0151(3) 0.0308(12) Uani 1 1 d . . . O8B O 0.31503(18) 0.13699(16) -0.0629(2) 0.0400(9) Uani 1 1 d . . . N9B N 0.27831(19) 0.13325(17) 0.0865(2) 0.0239(9) Uani 1 1 d . . . C10B C 0.2388(2) 0.1917(2) 0.0775(3) 0.0240(11) Uani 1 1 d . . . C11B C 0.2756(4) 0.2500 0.0779(4) 0.0272(16) Uani 1 2 d S . . H11B H 0.3265 0.2500 0.0784 0.033 Uiso 1 2 calc SR . . C12B C 0.1629(2) 0.1924(2) 0.0711(3) 0.0256(11) Uani 1 1 d . . . H12B H 0.1369 0.1541 0.0701 0.031 Uiso 1 1 calc R . . C13B C 0.1263(3) 0.2500 0.0664(4) 0.0247(16) Uani 1 2 d S . . H13B H 0.0758 0.2500 0.0597 0.030 Uiso 1 2 calc SR . . N1C N 0.3389(2) 0.03305(19) 0.3192(3) 0.0305(10) Uani 1 1 d . . . C2C C 0.3115(3) -0.0205(2) 0.3536(3) 0.0377(13) Uani 1 1 d . . . H2C H 0.2722 -0.0397 0.3245 0.045 Uiso 1 1 calc R . . C3C C 0.3382(3) -0.0485(3) 0.4298(3) 0.0416(14) Uani 1 1 d . . . H3C H 0.3188 -0.0869 0.4507 0.050 Uiso 1 1 calc R . . C4C C 0.3940(3) -0.0192(3) 0.4745(4) 0.0443(14) Uani 1 1 d . . . H4C H 0.4126 -0.0367 0.5273 0.053 Uiso 1 1 calc R . . C5C C 0.4225(3) 0.0366(2) 0.4405(3) 0.0391(14) Uani 1 1 d . . . H5C H 0.4603 0.0576 0.4703 0.047 Uiso 1 1 calc R . . C6C C 0.3943(3) 0.0612(2) 0.3617(3) 0.0300(12) Uani 1 1 d . . . C7C C -0.0757(3) 0.1217(2) 0.1791(3) 0.0297(12) Uani 1 1 d . . . O8C O -0.02775(18) 0.15213(16) 0.1354(2) 0.0399(9) Uani 1 1 d . . . N9C N 0.3971(2) 0.13423(17) 0.2408(2) 0.0258(9) Uani 1 1 d . . . C10C C 0.4194(2) 0.1921(2) 0.1991(3) 0.0259(11) Uani 1 1 d . . . C11C C 0.4055(3) 0.2500 0.2415(4) 0.0256(16) Uani 1 2 d S . . H11C H 0.3864 0.2500 0.2996 0.031 Uiso 1 2 calc SR . . C12C C 0.4505(2) 0.1922(2) 0.1139(3) 0.0289(11) Uani 1 1 d . . . H12C H 0.4608 0.1538 0.0848 0.035 Uiso 1 1 calc R . . C13C C 0.4660(3) 0.2500 0.0725(5) 0.0317(17) Uani 1 2 d S . . H13C H 0.4873 0.2500 0.0156 0.038 Uiso 1 2 calc SR . . O1W O 0.1285(3) 0.2500 0.5463(3) 0.0652(17) Uani 1 2 d S . . O2W O 0.8504(4) 0.2500 0.8184(4) 0.093(2) Uani 1 2 d S . . O3W O 0.2939(2) 0.8158(2) 0.3263(3) 0.0710(13) Uani 1 1 d . . . O4W O 0.5333(2) 0.8166(2) 0.4526(3) 0.0744(13) Uani 1 1 d . . . O5W O 0.4422(2) 0.8459(2) 0.3064(3) 0.0702(13) Uani 1 1 d . . . O6W O 0.8753(3) 0.2500 0.6310(3) 0.0521(15) Uani 1 2 d S . . O7W O 0.4784(3) 0.7500 0.1779(4) 0.0748(19) Uani 1 2 d S . . O8W O 0.2705(3) 0.8307(2) 0.1420(3) 0.0927(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0374(4) 0.0814(5) 0.0435(4) 0.000 0.0087(3) 0.000 Ag2 0.0372(4) 0.0643(5) 0.0431(4) 0.000 0.0103(3) 0.000 Ni1 0.0264(3) 0.0287(3) 0.0257(3) 0.0007(3) -0.0011(3) 0.0024(3) N1A 0.035(3) 0.028(2) 0.034(2) 0.000(2) -0.005(2) 0.000(2) C2A 0.042(3) 0.036(3) 0.046(3) -0.002(3) -0.007(3) 0.006(3) C3A 0.055(4) 0.032(3) 0.059(4) -0.005(3) -0.010(3) -0.008(3) C4A 0.045(4) 0.045(4) 0.051(4) 0.008(3) -0.009(3) -0.014(3) C5A 0.034(3) 0.048(4) 0.035(3) 0.003(3) -0.004(2) -0.003(3) C6A 0.029(3) 0.032(3) 0.027(3) 0.000(2) -0.003(2) 0.001(2) C7A 0.034(3) 0.038(3) 0.027(3) 0.000(2) 0.000(2) 0.001(3) O8A 0.023(2) 0.052(2) 0.058(2) -0.016(2) 0.0061(18) -0.0003(18) N9A 0.026(2) 0.031(2) 0.028(2) -0.0013(19) -0.0020(18) 0.0002(18) C10A 0.017(2) 0.031(3) 0.025(3) 0.001(2) 0.004(2) -0.001(2) C11A 0.025(4) 0.039(4) 0.018(4) 0.000 0.005(3) 0.000 C12A 0.027(3) 0.038(3) 0.024(3) 0.004(2) 0.001(2) 0.005(2) C13A 0.030(4) 0.051(5) 0.017(4) 0.000 -0.003(3) 0.000 N1B 0.029(2) 0.029(2) 0.035(3) 0.000(2) -0.0031(19) 0.0064(19) C2B 0.047(3) 0.034(3) 0.041(3) 0.005(3) -0.003(3) 0.009(3) C3B 0.066(4) 0.041(4) 0.054(4) -0.005(3) -0.001(3) 0.026(3) C4B 0.077(5) 0.054(4) 0.052(4) -0.019(3) 0.005(3) 0.030(4) C5B 0.054(4) 0.050(4) 0.034(3) -0.004(3) 0.002(3) 0.024(3) C6B 0.027(3) 0.032(3) 0.031(3) -0.008(2) 0.000(2) 0.001(2) C7B 0.024(3) 0.033(3) 0.035(3) -0.002(3) -0.003(2) -0.001(2) O8B 0.048(2) 0.044(2) 0.028(2) 0.0021(17) 0.0046(17) 0.0105(18) N9B 0.023(2) 0.022(2) 0.027(2) -0.0005(18) -0.0009(18) 0.0040(17) C10B 0.023(3) 0.032(3) 0.017(2) -0.005(2) -0.001(2) -0.002(2) C11B 0.021(4) 0.038(4) 0.022(4) 0.000 0.001(3) 0.000 C12B 0.030(3) 0.025(3) 0.022(3) -0.003(2) 0.000(2) -0.006(2) C13B 0.019(4) 0.033(4) 0.022(4) 0.000 -0.005(3) 0.000 N1C 0.030(2) 0.032(2) 0.030(2) 0.0036(19) -0.0001(19) 0.005(2) C2C 0.035(3) 0.037(3) 0.041(3) 0.008(3) -0.004(3) -0.001(3) C3C 0.043(3) 0.041(3) 0.041(3) 0.013(3) 0.000(3) 0.000(3) C4C 0.055(4) 0.045(4) 0.033(3) 0.011(3) -0.006(3) 0.006(3) C5C 0.040(3) 0.040(3) 0.038(3) 0.005(3) -0.010(3) -0.002(3) C6C 0.028(3) 0.033(3) 0.029(3) 0.001(2) -0.001(2) 0.004(2) C7C 0.027(3) 0.033(3) 0.029(3) 0.002(2) -0.001(2) 0.007(2) O8C 0.035(2) 0.048(2) 0.037(2) -0.0033(18) 0.0105(17) -0.0089(18) N9C 0.027(2) 0.027(2) 0.023(2) -0.0010(18) -0.0007(18) 0.0016(18) C10C 0.018(2) 0.036(3) 0.023(3) 0.003(2) -0.005(2) 0.004(2) C11C 0.025(4) 0.031(4) 0.021(4) 0.000 0.004(3) 0.000 C12C 0.023(3) 0.034(3) 0.030(3) -0.004(2) -0.003(2) 0.006(2) C13C 0.017(4) 0.054(5) 0.024(4) 0.000 0.000(3) 0.000 O1W 0.050(4) 0.108(5) 0.038(3) 0.000 -0.001(3) 0.000 O2W 0.060(4) 0.164(7) 0.055(4) 0.000 0.007(3) 0.000 O3W 0.067(3) 0.070(3) 0.076(3) -0.022(2) 0.017(2) -0.013(2) O4W 0.084(3) 0.085(3) 0.055(3) 0.013(2) -0.005(2) -0.029(3) O5W 0.065(3) 0.070(3) 0.076(3) -0.002(3) 0.005(2) -0.007(2) O6W 0.042(3) 0.068(4) 0.045(3) 0.000 0.000(3) 0.000 O7W 0.056(4) 0.111(5) 0.058(4) 0.000 -0.004(3) 0.000 O8W 0.107(4) 0.087(4) 0.084(4) -0.005(3) 0.000(3) 0.014(3) _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 Ag1 C11C 2.532(6) 6_556 ? Ag1 O8C 2.547(3) . ? Ag1 O8C 2.547(3) 8_565 ? Ag1 C13B 2.594(6) . ? Ag1 Ag2 3.0462(10) . ? Ag2 O8A 2.377(3) 8_565 ? Ag2 O8A 2.377(3) . ? Ag2 O1W 2.399(5) . ? Ag2 C11A 2.602(6) . ? Ag2 C13C 2.640(6) 6_556 ? Ni1 N9A 2.075(4) . ? Ni1 N1B 2.085(4) . ? Ni1 N1C 2.097(4) . ? Ni1 N9B 2.104(4) . ? Ni1 N9C 2.125(4) . ? Ni1 N1A 2.127(4) . ? N1A C2A 1.336(6) . ? N1A C6A 1.351(6) . ? C2A C3A 1.377(7) . ? C2A H2A 0.9300 . ? C3A C4A 1.365(7) . ? C3A H3A 0.9300 . ? C4A C5A 1.390(7) . ? C4A H4A 0.9300 . ? C5A C6A 1.371(7) . ? C5A H5A 0.9300 . ? C6A C7A 1.497(7) . ? C7A O8A 1.263(6) . ? C7A N9A 1.318(6) . ? N9A C10A 1.421(6) . ? C10A C12A 1.373(6) . ? C10A C11A 1.380(5) . ? C11A C10A 1.380(5) 8_565 ? C11A H11A 0.9300 . ? C12A C13A 1.379(6) . ? C12A H12A 0.9300 . ? C13A C12A 1.379(6) 8_565 ? C13A H13A 0.9300 . ? N1B C6B 1.333(6) . ? N1B C2B 1.336(6) . ? C2B C3B 1.365(7) . ? C2B H2B 0.9300 . ? C3B C4B 1.360(8) . ? C3B H3B 0.9300 . ? C4B C5B 1.377(7) . ? C4B H4B 0.9300 . ? C5B C6B 1.369(7) . ? C5B H5B 0.9300 . ? C6B C7B 1.508(7) . ? C7B O8B 1.265(5) . ? C7B N9B 1.310(6) . ? N9B C10B 1.425(6) . ? C10B C12B 1.390(6) . ? C10B C11B 1.393(5) . ? C11B C10B 1.393(5) 8_565 ? C11B H11B 0.9300 . ? C12B C13B 1.379(5) . ? C12B H12B 0.9300 . ? C13B C12B 1.379(5) 8_565 ? C13B H13B 0.9300 . ? N1C C2C 1.327(6) . ? N1C C6C 1.330(6) . ? C2C C3C 1.364(7) . ? C2C H2C 0.9300 . ? C3C C4C 1.362(7) . ? C3C H3C 0.9300 . ? C4C C5C 1.373(7) . ? C4C H4C 0.9300 . ? C5C C6C 1.378(6) . ? C5C H5C 0.9300 . ? C6C C7C 1.505(7) 6_656 ? C7C O8C 1.262(5) . ? C7C N9C 1.315(6) 6_556 ? C7C C6C 1.505(7) 6_556 ? N9C C7C 1.315(6) 6_656 ? N9C C10C 1.419(6) . ? C10C C12C 1.386(6) . ? C10C C11C 1.387(6) . ? C11C C10C 1.387(6) 8_565 ? C11C Ag1 2.532(6) 6_656 ? C11C H11C 0.9300 . ? C12C C13C 1.384(6) . ? C12C H12C 0.9300 . ? C13C C12C 1.384(6) 8_565 ? C13C Ag2 2.640(6) 6_656 ? C13C H13C 0.9300 . ? 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 C11C Ag1 O8C 72.45(11) 6_556 . ? C11C Ag1 O8C 72.45(11) 6_556 8_565 ? O8C Ag1 O8C 106.80(16) . 8_565 ? C11C Ag1 C13B 149.2(2) 6_556 . ? O8C Ag1 C13B 89.77(11) . . ? O8C Ag1 C13B 89.77(11) 8_565 . ? C11C Ag1 Ag2 95.44(15) 6_556 . ? O8C Ag1 Ag2 122.73(8) . . ? O8C Ag1 Ag2 122.73(8) 8_565 . ? C13B Ag1 Ag2 115.32(14) . . ? O8A Ag2 O8A 116.98(18) 8_565 . ? O8A Ag2 O1W 121.31(9) 8_565 . ? O8A Ag2 O1W 121.31(9) . . ? O8A Ag2 C11A 75.30(11) 8_565 . ? O8A Ag2 C11A 75.30(11) . . ? O1W Ag2 C11A 112.9(2) . . ? O8A Ag2 C13C 95.07(11) 8_565 6_556 ? O8A Ag2 C13C 95.06(11) . 6_556 ? O1W Ag2 C13C 86.4(2) . 6_556 ? C11A Ag2 C13C 160.7(2) . 6_556 ? O8A Ag2 Ag1 60.93(9) 8_565 . ? O8A Ag2 Ag1 60.93(9) . . ? O1W Ag2 Ag1 164.46(13) . . ? C11A Ag2 Ag1 82.60(15) . . ? C13C Ag2 Ag1 78.08(15) 6_556 . ? N9A Ni1 N1B 169.23(15) . . ? N9A Ni1 N1C 90.89(15) . . ? N1B Ni1 N1C 94.99(15) . . ? N9A Ni1 N9B 96.49(14) . . ? N1B Ni1 N9B 78.57(15) . . ? N1C Ni1 N9B 171.02(15) . . ? N9A Ni1 N9C 98.02(14) . . ? N1B Ni1 N9C 92.08(14) . . ? N1C Ni1 N9C 77.29(15) . . ? N9B Ni1 N9C 96.54(14) . . ? N9A Ni1 N1A 77.20(15) . . ? N1B Ni1 N1A 93.37(15) . . ? N1C Ni1 N1A 93.94(15) . . ? N9B Ni1 N1A 92.69(14) . . ? N9C Ni1 N1A 170.06(15) . . ? C2A N1A C6A 117.7(4) . . ? C2A N1A Ni1 128.9(4) . . ? C6A N1A Ni1 113.4(3) . . ? N1A C2A C3A 122.7(5) . . ? N1A C2A H2A 118.6 . . ? C3A C2A H2A 118.6 . . ? C4A C3A C2A 119.3(5) . . ? C4A C3A H3A 120.4 . . ? C2A C3A H3A 120.4 . . ? C3A C4A C5A 118.8(5) . . ? C3A C4A H4A 120.6 . . ? C5A C4A H4A 120.6 . . ? C6A C5A C4A 118.8(5) . . ? C6A C5A H5A 120.6 . . ? C4A C5A H5A 120.6 . . ? N1A C6A C5A 122.5(5) . . ? N1A C6A C7A 116.2(4) . . ? C5A C6A C7A 121.3(5) . . ? O8A C7A N9A 129.5(5) . . ? O8A C7A C6A 117.2(4) . . ? N9A C7A C6A 113.2(4) . . ? C7A O8A Ag2 125.3(3) . . ? C7A N9A C10A 116.4(4) . . ? C7A N9A Ni1 117.0(3) . . ? C10A N9A Ni1 124.3(3) . . ? C12A C10A C11A 119.3(5) . . ? C12A C10A N9A 121.4(4) . . ? C11A C10A N9A 119.3(4) . . ? C10A C11A C10A 121.4(6) 8_565 . ? C10A C11A Ag2 88.8(3) 8_565 . ? C10A C11A Ag2 88.8(3) . . ? C10A C11A H11A 119.3 8_565 . ? C10A C11A H11A 119.3 . . ? Ag2 C11A H11A 92.4 . . ? C13A C12A C10A 119.3(5) . . ? C13A C12A H12A 120.3 . . ? C10A C12A H12A 120.3 . . ? C12A C13A C12A 121.4(6) . 8_565 ? C12A C13A H13A 119.3 . . ? C12A C13A H13A 119.3 8_565 . ? C6B N1B C2B 118.3(4) . . ? C6B N1B Ni1 114.1(3) . . ? C2B N1B Ni1 127.6(3) . . ? N1B C2B C3B 122.6(5) . . ? N1B C2B H2B 118.7 . . ? C3B C2B H2B 118.7 . . ? C4B C3B C2B 119.0(5) . . ? C4B C3B H3B 120.5 . . ? C2B C3B H3B 120.5 . . ? C3B C4B C5B 119.0(5) . . ? C3B C4B H4B 120.5 . . ? C5B C4B H4B 120.5 . . ? C4B C5B C6B 119.2(5) . . ? C4B C5B H5B 120.4 . . ? C6B C5B H5B 120.4 . . ? N1B C6B C5B 121.9(5) . . ? N1B C6B C7B 116.8(4) . . ? C5B C6B C7B 121.3(5) . . ? O8B C7B N9B 128.3(4) . . ? O8B C7B C6B 117.4(4) . . ? N9B C7B C6B 114.2(4) . . ? C7B N9B C10B 117.0(4) . . ? C7B N9B Ni1 115.5(3) . . ? C10B N9B Ni1 126.8(3) . . ? C12B C10B C11B 118.3(5) . . ? C12B C10B N9B 121.4(4) . . ? C11B C10B N9B 120.2(4) . . ? C10B C11B C10B 122.1(6) . 8_565 ? C10B C11B H11B 119.0 . . ? C10B C11B H11B 119.0 8_565 . ? C13B C12B C10B 119.7(5) . . ? C13B C12B H12B 120.1 . . ? C10B C12B H12B 120.1 . . ? C12B C13B C12B 121.7(6) . 8_565 ? C12B C13B Ag1 105.6(3) . . ? C12B C13B Ag1 105.6(3) 8_565 . ? C12B C13B H13B 119.1 . . ? C12B C13B H13B 119.1 8_565 . ? Ag1 C13B H13B 56.5 . . ? C2C N1C C6C 118.5(4) . . ? C2C N1C Ni1 127.1(3) . . ? C6C N1C Ni1 114.3(3) . . ? N1C C2C C3C 123.1(5) . . ? N1C C2C H2C 118.4 . . ? C3C C2C H2C 118.4 . . ? C4C C3C C2C 118.5(5) . . ? C4C C3C H3C 120.7 . . ? C2C C3C H3C 120.7 . . ? C3C C4C C5C 119.1(5) . . ? C3C C4C H4C 120.4 . . ? C5C C4C H4C 120.4 . . ? C4C C5C C6C 119.2(5) . . ? C4C C5C H5C 120.4 . . ? C6C C5C H5C 120.4 . . ? N1C C6C C5C 121.5(5) . . ? N1C C6C C7C 117.3(4) . 6_656 ? C5C C6C C7C 121.2(5) . 6_656 ? O8C C7C N9C 128.9(5) . 6_556 ? O8C C7C C6C 118.0(4) . 6_556 ? N9C C7C C6C 113.1(4) 6_556 6_556 ? C7C O8C Ag1 121.6(3) . . ? C7C N9C C10C 117.1(4) 6_656 . ? C7C N9C Ni1 115.6(3) 6_656 . ? C10C N9C Ni1 124.2(3) . . ? C12C C10C C11C 119.2(5) . . ? C12C C10C N9C 121.2(4) . . ? C11C C10C N9C 119.5(4) . . ? C10C C11C C10C 121.3(6) . 8_565 ? C10C C11C Ag1 88.8(3) . 6_656 ? C10C C11C Ag1 88.8(3) 8_565 6_656 ? C10C C11C H11C 119.3 . . ? C10C C11C H11C 119.3 8_565 . ? Ag1 C11C H11C 92.4 6_656 . ? C10C C12C C13C 119.4(5) . . ? C10C C12C H12C 120.3 . . ? C13C C12C H12C 120.3 . . ? C12C C13C C12C 121.4(6) 8_565 . ? C12C C13C Ag2 95.6(3) 8_565 6_656 ? C12C C13C Ag2 95.6(3) . 6_656 ? C12C C13C H13C 119.3 8_565 . ? C12C C13C H13C 119.3 . . ? Ag2 C13C H13C 78.4 6_656 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.90 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.517 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.077 data_compound3 _database_code_depnum_ccdc_archive 'CCDC 721868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H76 Co N12 Ni2 O23' _chemical_formula_weight 1485.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.330(5) _cell_length_b 13.521(5) _cell_length_c 21.544(8) _cell_angle_alpha 91.506(7) _cell_angle_beta 102.991(6) _cell_angle_gamma 113.280(6) _cell_volume 3447(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7368 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.22 _exptl_crystal_description prismatic _exptl_crystal_colour brown _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1550 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.528 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _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 18577 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11875 _reflns_number_gt 9842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker APEXII' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1246P)^2^+2.9926P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11875 _refine_ls_number_parameters 843 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1933 _refine_ls_wR_factor_gt 0.1836 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.003 _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 O7W O 0.5227(3) 0.4721(3) 0.32215(18) 0.0636(10) Uani 1 1 d . . . O8W O 0.3797(4) 0.1844(3) -0.10954(19) 0.0766(12) Uani 1 1 d . . . O9W O 0.4974(4) 0.6576(4) 0.1791(2) 0.0848(13) Uani 1 1 d . . . O10W O 1.2583(3) 0.5371(4) 0.3558(2) 0.0812(13) Uani 1 1 d . . . O11W O 0.7449(5) 0.7342(4) 0.3974(3) 0.1151(19) Uani 1 1 d . . . O12W O 1.2667(7) 0.3166(7) 0.3371(4) 0.174(3) Uani 1 1 d . . . O15W O 0.2981(7) 0.5244(8) 0.2014(5) 0.204(4) Uani 1 1 d . . . O13W O 1.3624(11) 0.1740(13) 0.5172(8) 0.340(10) Uani 1 1 d . . . O17W O 0.3265(13) 0.3493(15) 0.2272(8) 0.336(9) Uani 1 1 d . . . O18W O 0.2643(18) 0.0277(14) 0.0854(16) 0.62(3) Uani 1 1 d . . . C5D C 0.2558(15) 0.1039(16) 0.2512(9) 0.227(7) Uiso 1 1 d . . . H5D1 H 0.1829 0.1076 0.2439 0.273 Uiso 1 1 calc R . . H5D2 H 0.3070 0.1631 0.2341 0.273 Uiso 1 1 calc R . . O1D O 0.2471(14) 0.0000(16) 0.2276(9) 0.302(7) Uiso 1 1 d . . . C2D C 0.2495(18) -0.0630(18) 0.2811(11) 0.254(9) Uiso 1 1 d . . . H2D1 H 0.2797 -0.1154 0.2735 0.305 Uiso 1 1 calc R . . H2D2 H 0.1738 -0.1018 0.2862 0.305 Uiso 1 1 calc R . . C3D C 0.324(2) 0.016(3) 0.3405(14) 0.339(14) Uiso 1 1 d . . . H3D1 H 0.2997 -0.0107 0.3785 0.407 Uiso 1 1 calc R . . H3D2 H 0.4021 0.0275 0.3463 0.407 Uiso 1 1 calc R . . C4D C 0.311(2) 0.098(2) 0.3297(11) 0.274(10) Uiso 1 1 d . . . H4D1 H 0.3832 0.1596 0.3448 0.329 Uiso 1 1 calc R . . H4D2 H 0.2611 0.1056 0.3546 0.329 Uiso 1 1 calc R . . Ni1 Ni 0.79651(4) 0.18254(4) 0.35844(2) 0.03059(16) Uani 1 1 d . . . Ni2 Ni 0.86722(4) 0.58283(4) 0.15754(2) 0.03147(16) Uani 1 1 d . . . Co1 Co 0.5000 0.0000 0.0000 0.0392(2) Uani 1 2 d S . . Co2 Co 1.5000 0.5000 0.5000 0.0391(2) Uani 1 2 d S . . N9B N 0.6873(3) 0.2616(3) 0.34551(15) 0.0322(7) Uani 1 1 d . . . O17A O 0.6975(2) 0.2874(2) 0.03941(14) 0.0436(7) Uani 1 1 d . . . N9A N 0.7790(3) 0.1421(2) 0.26109(15) 0.0308(7) Uani 1 1 d . . . N9C N 0.9482(3) 0.3209(3) 0.37857(15) 0.0333(7) Uani 1 1 d . . . N16A N 0.8279(3) 0.4235(2) 0.11931(15) 0.0310(7) Uani 1 1 d . . . N1C N 0.9167(3) 0.1166(3) 0.38922(16) 0.0390(8) Uani 1 1 d . . . O5W O 1.4679(3) 0.5661(3) 0.41584(16) 0.0548(8) Uani 1 1 d . . . O8A O 0.6560(3) 0.0187(2) 0.17275(13) 0.0468(7) Uani 1 1 d . . . N16C N 0.9991(3) 0.6010(2) 0.23590(15) 0.0340(7) Uani 1 1 d . . . C11A C 0.8015(3) 0.2739(3) 0.18448(17) 0.0307(8) Uani 1 1 d . . . H11A H 0.7275 0.2650 0.1809 0.037 Uiso 1 1 calc R . . N24C N 1.0059(3) 0.6431(3) 0.11766(17) 0.0403(8) Uani 1 1 d . . . C11C C 0.9845(3) 0.4677(3) 0.31210(18) 0.0322(8) Uani 1 1 d . . . H11C H 1.0003 0.4262 0.2838 0.039 Uiso 1 1 calc R . . O8B O 0.6163(3) 0.3543(3) 0.40236(14) 0.0474(7) Uani 1 1 d . . . N16B N 0.7410(3) 0.5458(2) 0.20627(15) 0.0320(7) Uani 1 1 d . . . N24A N 0.7489(3) 0.5652(3) 0.07036(17) 0.0396(8) Uani 1 1 d . . . N24B N 0.8790(3) 0.7387(3) 0.18555(17) 0.0393(8) Uani 1 1 d . . . O2W O 0.4805(3) 0.1466(3) 0.00448(16) 0.0536(8) Uani 1 1 d . . . O3W O 0.6716(3) 0.0819(2) 0.05403(14) 0.0460(7) Uani 1 1 d . . . N1B N 0.7806(3) 0.2045(3) 0.45214(15) 0.0364(7) Uani 1 1 d . . . C15B C 0.6736(3) 0.4387(3) 0.21789(18) 0.0309(8) Uani 1 1 d . . . C10B C 0.6475(3) 0.2974(3) 0.28714(17) 0.0305(8) Uani 1 1 d . . . C13C C 0.9415(4) 0.5924(3) 0.39729(19) 0.0402(9) Uani 1 1 d . . . H13C H 0.9284 0.6350 0.4264 0.048 Uiso 1 1 calc R . . C18A C 0.7459(3) 0.3841(3) 0.06750(18) 0.0327(8) Uani 1 1 d . . . O17B O 0.6658(3) 0.6254(3) 0.26874(16) 0.0514(8) Uani 1 1 d . . . O4W O 1.4402(3) 0.3467(3) 0.44628(17) 0.0570(8) Uani 1 1 d . . . N1A N 0.6587(3) 0.0298(3) 0.33753(17) 0.0403(8) Uani 1 1 d . . . O8C O 1.1413(3) 0.3809(3) 0.4181(2) 0.0653(10) Uani 1 1 d . . . O6W O 1.6659(2) 0.5374(3) 0.48585(15) 0.0478(7) Uani 1 1 d . . . C11B C 0.7042(3) 0.4041(3) 0.27639(18) 0.0323(8) Uani 1 1 d . . . H11B H 0.7634 0.4529 0.3089 0.039 Uiso 1 1 calc R . . O1W O 0.4515(3) -0.0312(3) 0.08678(16) 0.0603(9) Uani 1 1 d . . . C6C C 1.0232(4) 0.1922(3) 0.4078(2) 0.0425(10) Uani 1 1 d . . . C19B C 0.8087(3) 0.7371(3) 0.22173(19) 0.0375(9) Uani 1 1 d . . . C10A C 0.8447(3) 0.2109(3) 0.22234(18) 0.0311(8) Uani 1 1 d . . . C19A C 0.7075(3) 0.4665(3) 0.03681(19) 0.0375(9) Uani 1 1 d . . . C13A C 1.0194(3) 0.2957(3) 0.1916(2) 0.0420(10) Uani 1 1 d . . . H13A H 1.0917 0.3012 0.1929 0.050 Uiso 1 1 calc R . . O17C O 1.1914(3) 0.6442(3) 0.26430(17) 0.0626(10) Uani 1 1 d . . . C13B C 0.5237(3) 0.2609(3) 0.1816(2) 0.0404(9) Uani 1 1 d . . . H13B H 0.4619 0.2133 0.1499 0.048 Uiso 1 1 calc R . . C6B C 0.7178(3) 0.2590(3) 0.45814(19) 0.0379(9) Uani 1 1 d . . . C12B C 0.5561(3) 0.2257(3) 0.23890(19) 0.0365(9) Uani 1 1 d . . . H12B H 0.5172 0.1543 0.2455 0.044 Uiso 1 1 calc R . . C10C C 0.9598(3) 0.4295(3) 0.36869(18) 0.0338(8) Uani 1 1 d . . . C18B C 0.7322(3) 0.6271(3) 0.23399(19) 0.0359(9) Uani 1 1 d . . . C7B C 0.6704(3) 0.2960(3) 0.39782(19) 0.0354(9) Uani 1 1 d . . . C15C C 0.9855(3) 0.5682(3) 0.29757(18) 0.0324(8) Uani 1 1 d . . . C12C C 0.9389(3) 0.4925(3) 0.41147(19) 0.0379(9) Uani 1 1 d . . . H12C H 0.9233 0.4677 0.4496 0.045 Uiso 1 1 calc R . . C12A C 0.9543(3) 0.2226(3) 0.2263(2) 0.0376(9) Uani 1 1 d . . . H12A H 0.9842 0.1818 0.2521 0.045 Uiso 1 1 calc R . . C19C C 1.1053(4) 0.6625(3) 0.1594(2) 0.0415(9) Uani 1 1 d . . . C7C C 1.0411(3) 0.3088(3) 0.4018(2) 0.0420(10) Uani 1 1 d . . . C14C C 0.9631(3) 0.6300(3) 0.3405(2) 0.0385(9) Uani 1 1 d . . . H14C H 0.9627 0.6966 0.3311 0.046 Uiso 1 1 calc R . . C15A C 0.8688(3) 0.3509(3) 0.15168(17) 0.0308(8) Uani 1 1 d . . . C14A C 0.9769(3) 0.3605(3) 0.15472(19) 0.0369(9) Uani 1 1 d . . . H14A H 1.0213 0.4101 0.1323 0.044 Uiso 1 1 calc R . . C7A C 0.6903(3) 0.0553(3) 0.23182(19) 0.0342(8) Uani 1 1 d . . . C14B C 0.5822(3) 0.3669(3) 0.17042(19) 0.0361(9) Uani 1 1 d . . . H14B H 0.5601 0.3895 0.1313 0.043 Uiso 1 1 calc R . . C18C C 1.1001(3) 0.6336(3) 0.2264(2) 0.0391(9) Uani 1 1 d . . . C2C C 0.8990(4) 0.0121(4) 0.3934(2) 0.0464(10) Uani 1 1 d . . . H2C H 0.8251 -0.0405 0.3809 0.056 Uiso 1 1 calc R . . C6A C 0.6238(3) -0.0120(3) 0.2755(2) 0.0386(9) Uani 1 1 d . . . C3B C 0.8067(4) 0.1848(4) 0.5632(2) 0.0507(11) Uani 1 1 d . . . H3B H 0.8364 0.1569 0.5982 0.061 Uiso 1 1 calc R . . C2B C 0.8232(4) 0.1684(4) 0.5041(2) 0.0443(10) Uani 1 1 d . . . H2B H 0.8663 0.1300 0.4999 0.053 Uiso 1 1 calc R . . C5B C 0.7002(4) 0.2814(4) 0.5164(2) 0.0538(12) Uani 1 1 d . . . H5B H 0.6585 0.3216 0.5199 0.065 Uiso 1 1 calc R . . C5A C 0.5330(4) -0.1116(4) 0.2526(3) 0.0612(14) Uani 1 1 d . . . H5A H 0.5104 -0.1381 0.2092 0.073 Uiso 1 1 calc R . . C20B C 0.8060(4) 0.8308(4) 0.2460(2) 0.0498(11) Uani 1 1 d . . . H20B H 0.7573 0.8276 0.2716 0.060 Uiso 1 1 calc R . . C20A C 0.6333(5) 0.4411(4) -0.0238(2) 0.0620(14) Uani 1 1 d . . . H20A H 0.6058 0.3724 -0.0467 0.074 Uiso 1 1 calc R . . C3C C 0.9840(5) -0.0205(5) 0.4151(3) 0.0649(14) Uani 1 1 d . . . H3C H 0.9686 -0.0936 0.4167 0.078 Uiso 1 1 calc R . . C23C C 1.0069(4) 0.6616(4) 0.0571(2) 0.0560(12) Uani 1 1 d . . . H23C H 0.9388 0.6464 0.0272 0.067 Uiso 1 1 calc R . . C23B C 0.9471(4) 0.8350(4) 0.1727(3) 0.0539(12) Uani 1 1 d . . . H23B H 0.9962 0.8368 0.1477 0.065 Uiso 1 1 calc R . . C20C C 1.2053(4) 0.7040(5) 0.1420(3) 0.0624(14) Uani 1 1 d . . . H20C H 1.2729 0.7171 0.1719 0.075 Uiso 1 1 calc R . . C21B C 0.8759(5) 0.9298(4) 0.2321(3) 0.0611(14) Uani 1 1 d . . . H21B H 0.8744 0.9939 0.2476 0.073 Uiso 1 1 calc R . . C4B C 0.7453(5) 0.2434(5) 0.5696(2) 0.0588(13) Uani 1 1 d . . . H4B H 0.7341 0.2575 0.6093 0.071 Uiso 1 1 calc R . . C23A C 0.7142(4) 0.6392(4) 0.0453(2) 0.0534(12) Uani 1 1 d . . . H23A H 0.7397 0.7063 0.0696 0.064 Uiso 1 1 calc R . . C22B C 0.9472(5) 0.9312(4) 0.1952(3) 0.0642(14) Uani 1 1 d . . . H22B H 0.9955 0.9967 0.1853 0.077 Uiso 1 1 calc R . . C2A C 0.6037(5) -0.0286(4) 0.3785(3) 0.0676(16) Uani 1 1 d . . . H2A H 0.6269 -0.0006 0.4217 0.081 Uiso 1 1 calc R . . C22A C 0.6431(6) 0.6206(5) -0.0142(3) 0.0754(18) Uani 1 1 d . . . H22A H 0.6232 0.6749 -0.0309 0.090 Uiso 1 1 calc R . . C3A C 0.5142(6) -0.1287(6) 0.3587(3) 0.099(3) Uani 1 1 d . . . H3A H 0.4792 -0.1679 0.3884 0.119 Uiso 1 1 calc R . . C22C C 1.1062(5) 0.7026(5) 0.0373(3) 0.0692(15) Uani 1 1 d . . . H22C H 1.1045 0.7137 -0.0052 0.083 Uiso 1 1 calc R . . C5C C 1.1143(4) 0.1661(4) 0.4311(3) 0.0640(14) Uani 1 1 d . . . H5C H 1.1875 0.2199 0.4442 0.077 Uiso 1 1 calc R . . C4A C 0.4768(6) -0.1704(5) 0.2946(3) 0.090(2) Uani 1 1 d . . . H4A H 0.4150 -0.2366 0.2801 0.108 Uiso 1 1 calc R . . C21C C 1.2054(5) 0.7260(5) 0.0809(3) 0.0732(17) Uani 1 1 d . . . H21C H 1.2732 0.7569 0.0692 0.088 Uiso 1 1 calc R . . C21A C 0.6012(6) 0.5192(5) -0.0493(3) 0.082(2) Uani 1 1 d . . . H21A H 0.5517 0.5041 -0.0898 0.099 Uiso 1 1 calc R . . C4C C 1.0934(5) 0.0576(5) 0.4345(3) 0.0764(18) Uani 1 1 d . . . H4C H 1.1528 0.0377 0.4498 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O7W 0.069(2) 0.084(3) 0.062(2) 0.0270(19) 0.0354(19) 0.046(2) O8W 0.096(3) 0.070(3) 0.055(2) -0.0029(19) -0.008(2) 0.040(2) O9W 0.091(3) 0.074(3) 0.078(3) 0.008(2) 0.004(2) 0.032(2) O10W 0.046(2) 0.114(3) 0.090(3) 0.040(3) 0.013(2) 0.040(2) O11W 0.140(5) 0.090(4) 0.087(4) -0.012(3) 0.029(3) 0.020(3) O12W 0.140(6) 0.184(8) 0.184(8) -0.056(6) -0.016(5) 0.087(6) O15W 0.116(5) 0.209(9) 0.264(11) -0.026(8) 0.104(7) 0.016(6) O13W 0.226(12) 0.341(18) 0.356(18) 0.223(15) -0.022(12) 0.058(12) O17W 0.243(14) 0.37(2) 0.324(18) 0.097(15) -0.024(13) 0.100(14) O18W 0.46(3) 0.251(17) 1.13(6) -0.24(3) 0.56(4) -0.040(17) Ni1 0.0322(3) 0.0297(3) 0.0274(3) 0.00332(19) 0.0049(2) 0.0116(2) Ni2 0.0340(3) 0.0283(3) 0.0294(3) 0.0034(2) 0.0061(2) 0.0113(2) Co1 0.0416(4) 0.0337(4) 0.0316(4) -0.0002(3) 0.0018(3) 0.0089(3) Co2 0.0332(4) 0.0495(5) 0.0367(4) 0.0006(3) 0.0066(3) 0.0208(4) N9B 0.0337(17) 0.0338(17) 0.0301(17) 0.0065(13) 0.0090(14) 0.0142(14) O17A 0.0496(17) 0.0318(15) 0.0392(16) -0.0007(12) 0.0010(13) 0.0122(13) N9A 0.0339(16) 0.0265(15) 0.0293(16) 0.0024(13) 0.0053(13) 0.0111(13) N9C 0.0327(17) 0.0335(17) 0.0301(17) 0.0061(13) 0.0036(14) 0.0123(14) N16A 0.0337(17) 0.0297(16) 0.0280(16) 0.0039(13) 0.0068(14) 0.0119(13) N1C 0.045(2) 0.0392(19) 0.0341(18) 0.0067(14) 0.0077(15) 0.0199(16) O5W 0.0458(18) 0.076(2) 0.0470(19) 0.0152(16) 0.0095(15) 0.0301(17) O8A 0.0542(18) 0.0389(16) 0.0306(16) -0.0009(12) 0.0023(13) 0.0070(14) N16C 0.0343(17) 0.0295(16) 0.0327(17) 0.0054(13) 0.0059(14) 0.0088(13) C11A 0.0304(19) 0.0310(19) 0.0286(19) -0.0018(15) 0.0050(15) 0.0121(15) N24C 0.046(2) 0.0346(18) 0.0368(19) 0.0052(14) 0.0133(16) 0.0112(15) C11C 0.0275(18) 0.035(2) 0.0299(19) -0.0003(16) 0.0030(15) 0.0110(15) O8B 0.0582(19) 0.062(2) 0.0400(17) 0.0078(14) 0.0186(15) 0.0392(16) N16B 0.0334(17) 0.0309(17) 0.0312(17) 0.0034(13) 0.0068(14) 0.0137(13) N24A 0.0428(19) 0.0370(18) 0.0386(19) 0.0072(15) 0.0079(15) 0.0172(15) N24B 0.0395(19) 0.0330(18) 0.0396(19) 0.0050(14) 0.0053(15) 0.0116(14) O2W 0.057(2) 0.0416(17) 0.053(2) 0.0009(14) 0.0027(16) 0.0172(15) O3W 0.0449(17) 0.0405(16) 0.0409(17) -0.0015(13) 0.0012(13) 0.0113(13) N1B 0.0396(18) 0.0371(18) 0.0297(17) 0.0048(14) 0.0069(14) 0.0141(15) C15B 0.0287(18) 0.0317(19) 0.035(2) 0.0046(15) 0.0092(16) 0.0151(15) C10B 0.0284(18) 0.037(2) 0.0271(19) 0.0039(15) 0.0067(15) 0.0147(16) C13C 0.046(2) 0.037(2) 0.032(2) -0.0057(17) 0.0052(18) 0.0150(18) C18A 0.034(2) 0.032(2) 0.0281(19) 0.0027(16) 0.0077(16) 0.0107(16) O17B 0.062(2) 0.0453(18) 0.060(2) 0.0082(15) 0.0314(17) 0.0263(15) O4W 0.0540(19) 0.053(2) 0.062(2) -0.0024(16) 0.0207(17) 0.0180(16) N1A 0.0388(18) 0.0359(18) 0.0376(19) 0.0064(15) 0.0094(15) 0.0067(14) O8C 0.0330(17) 0.056(2) 0.090(3) 0.0251(19) -0.0057(17) 0.0109(15) O6W 0.0364(16) 0.063(2) 0.0468(18) -0.0003(15) 0.0076(13) 0.0250(15) C11B 0.0290(19) 0.035(2) 0.031(2) 0.0013(16) 0.0060(16) 0.0121(16) O1W 0.059(2) 0.069(2) 0.0407(18) 0.0101(16) 0.0114(16) 0.0146(17) C6C 0.043(2) 0.045(2) 0.043(2) 0.0135(19) 0.0071(19) 0.022(2) C19B 0.042(2) 0.036(2) 0.035(2) 0.0038(17) 0.0038(18) 0.0200(18) C10A 0.034(2) 0.0279(18) 0.0296(19) 0.0004(15) 0.0080(16) 0.0115(15) C19A 0.040(2) 0.036(2) 0.030(2) 0.0002(16) 0.0003(17) 0.0136(17) C13A 0.033(2) 0.043(2) 0.056(3) 0.007(2) 0.0148(19) 0.0194(18) O17C 0.0315(16) 0.090(3) 0.057(2) 0.0278(19) 0.0068(15) 0.0168(16) C13B 0.029(2) 0.038(2) 0.040(2) -0.0007(17) -0.0030(17) 0.0063(17) C6B 0.040(2) 0.039(2) 0.033(2) 0.0051(17) 0.0108(17) 0.0147(18) C12B 0.033(2) 0.034(2) 0.039(2) 0.0073(17) 0.0088(17) 0.0098(16) C10C 0.0287(19) 0.0314(19) 0.032(2) 0.0028(16) -0.0009(16) 0.0080(15) C18B 0.039(2) 0.037(2) 0.034(2) 0.0050(16) 0.0061(17) 0.0202(17) C7B 0.038(2) 0.039(2) 0.032(2) 0.0056(16) 0.0107(17) 0.0173(17) C15C 0.0286(19) 0.0312(19) 0.0289(19) 0.0022(15) 0.0027(15) 0.0063(15) C12C 0.039(2) 0.041(2) 0.0262(19) 0.0003(16) 0.0025(17) 0.0117(18) C12A 0.039(2) 0.034(2) 0.043(2) 0.0056(17) 0.0084(18) 0.0196(17) C19C 0.041(2) 0.037(2) 0.040(2) 0.0024(18) 0.0094(19) 0.0100(18) C7C 0.036(2) 0.040(2) 0.044(2) 0.0098(19) 0.0012(18) 0.0135(18) C14C 0.043(2) 0.030(2) 0.037(2) -0.0004(16) 0.0034(18) 0.0134(17) C15A 0.035(2) 0.0267(18) 0.0274(19) -0.0015(14) 0.0042(15) 0.0116(15) C14A 0.037(2) 0.037(2) 0.037(2) 0.0053(17) 0.0133(18) 0.0133(17) C7A 0.039(2) 0.030(2) 0.032(2) 0.0042(16) 0.0056(17) 0.0143(17) C14B 0.035(2) 0.041(2) 0.030(2) 0.0065(17) 0.0035(16) 0.0167(17) C18C 0.038(2) 0.038(2) 0.037(2) 0.0050(17) 0.0080(18) 0.0118(17) C2C 0.057(3) 0.039(2) 0.044(2) 0.0057(19) 0.009(2) 0.023(2) C6A 0.039(2) 0.031(2) 0.038(2) 0.0019(17) 0.0068(18) 0.0077(17) C3B 0.055(3) 0.055(3) 0.033(2) 0.010(2) 0.005(2) 0.016(2) C2B 0.050(3) 0.046(2) 0.037(2) 0.0093(19) 0.0063(19) 0.023(2) C5B 0.063(3) 0.072(3) 0.038(2) 0.012(2) 0.021(2) 0.035(3) C5A 0.060(3) 0.047(3) 0.049(3) -0.003(2) 0.012(2) -0.005(2) C20B 0.056(3) 0.039(2) 0.059(3) 0.001(2) 0.017(2) 0.023(2) C20A 0.078(4) 0.050(3) 0.045(3) -0.005(2) -0.017(3) 0.031(3) C3C 0.082(4) 0.053(3) 0.069(4) 0.015(3) 0.013(3) 0.041(3) C23C 0.058(3) 0.064(3) 0.038(3) 0.011(2) 0.014(2) 0.017(2) C23B 0.062(3) 0.038(2) 0.061(3) 0.010(2) 0.024(2) 0.016(2) C20C 0.040(3) 0.080(4) 0.055(3) 0.009(3) 0.018(2) 0.010(2) C21B 0.074(3) 0.033(2) 0.079(4) 0.000(2) 0.019(3) 0.024(2) C4B 0.073(3) 0.072(3) 0.032(2) 0.009(2) 0.016(2) 0.029(3) C23A 0.067(3) 0.042(3) 0.050(3) 0.006(2) 0.002(2) 0.028(2) C22B 0.071(3) 0.030(2) 0.084(4) 0.011(2) 0.022(3) 0.011(2) C2A 0.070(3) 0.060(3) 0.046(3) 0.004(2) 0.024(3) -0.005(3) C22A 0.097(4) 0.062(3) 0.063(3) 0.005(3) -0.019(3) 0.049(3) C3A 0.098(5) 0.079(4) 0.068(4) 0.003(3) 0.040(4) -0.026(4) C22C 0.072(4) 0.085(4) 0.051(3) 0.017(3) 0.033(3) 0.022(3) C5C 0.047(3) 0.060(3) 0.086(4) 0.025(3) 0.007(3) 0.027(2) C4A 0.083(4) 0.069(4) 0.064(4) 0.002(3) 0.023(3) -0.026(3) C21C 0.050(3) 0.098(4) 0.059(3) 0.008(3) 0.027(3) 0.011(3) C21A 0.107(5) 0.075(4) 0.055(3) -0.007(3) -0.031(3) 0.055(4) C4C 0.069(4) 0.073(4) 0.099(5) 0.031(3) 0.010(3) 0.047(3) _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 C5D O1D 1.43(2) . ? C5D C4D 1.70(2) . ? O1D C2D 1.45(2) . ? C2D C3D 1.51(3) . ? C3D C4D 1.22(3) . ? Ni1 N9C 2.085(3) . ? Ni1 N9A 2.091(3) . ? Ni1 N9B 2.099(3) . ? Ni1 N1B 2.102(3) . ? Ni1 N1A 2.103(3) . ? Ni1 N1C 2.118(3) . ? Ni2 N16C 2.074(3) . ? Ni2 N16B 2.083(3) . ? Ni2 N24C 2.093(4) . ? Ni2 N16A 2.101(3) . ? Ni2 N24A 2.103(4) . ? Ni2 N24B 2.112(4) . ? Co1 O2W 2.101(3) . ? Co1 O2W 2.101(3) 2_655 ? Co1 O1W 2.112(3) . ? Co1 O1W 2.112(3) 2_655 ? Co1 O3W 2.132(3) 2_655 ? Co1 O3W 2.132(3) . ? Co2 O5W 2.075(3) 2_866 ? Co2 O5W 2.075(3) . ? Co2 O4W 2.104(3) 2_866 ? Co2 O4W 2.104(3) . ? Co2 O6W 2.160(3) 2_866 ? Co2 O6W 2.160(3) . ? N9B C7B 1.305(5) . ? N9B C10B 1.425(5) . ? O17A C18A 1.268(5) . ? N9A C7A 1.305(5) . ? N9A C10A 1.434(5) . ? N9C C7C 1.303(5) . ? N9C C10C 1.441(5) . ? N16A C18A 1.298(5) . ? N16A C15A 1.427(5) . ? N1C C6C 1.340(6) . ? N1C C2C 1.346(6) . ? O8A C7A 1.265(5) . ? N16C C18C 1.308(5) . ? N16C C15C 1.439(5) . ? C11A C10A 1.391(5) . ? C11A C15A 1.404(5) . ? N24C C23C 1.337(6) . ? N24C C19C 1.346(6) . ? C11C C10C 1.393(5) . ? C11C C15C 1.397(5) . ? O8B C7B 1.277(5) . ? N16B C18B 1.296(5) . ? N16B C15B 1.435(5) . ? N24A C23A 1.336(6) . ? N24A C19A 1.341(5) . ? N24B C23B 1.339(6) . ? N24B C19B 1.342(5) . ? N1B C2B 1.332(5) . ? N1B C6B 1.339(5) . ? C15B C11B 1.387(5) . ? C15B C14B 1.387(5) . ? C10B C11B 1.393(5) . ? C10B C12B 1.396(5) . ? C13C C14C 1.384(6) . ? C13C C12C 1.382(6) . ? C18A C19A 1.509(6) . ? O17B C18B 1.275(5) . ? N1A C6A 1.339(5) . ? N1A C2A 1.346(6) . ? O8C C7C 1.265(5) . ? C6C C5C 1.389(6) . ? C6C C7C 1.511(6) . ? C19B C20B 1.375(6) . ? C19B C18B 1.504(6) . ? C10A C12A 1.388(6) . ? C19A C20A 1.390(6) . ? C13A C14A 1.395(6) . ? C13A C12A 1.394(6) . ? O17C C18C 1.256(5) . ? C13B C12B 1.374(6) . ? C13B C14B 1.393(6) . ? C6B C5B 1.376(6) . ? C6B C7B 1.500(6) . ? C10C C12C 1.383(6) . ? C15C C14C 1.387(6) . ? C19C C20C 1.370(6) . ? C19C C18C 1.513(6) . ? C15A C14A 1.381(6) . ? C7A C6A 1.510(6) . ? C2C C3C 1.366(7) . ? C6A C5A 1.389(6) . ? C3B C2B 1.368(6) . ? C3B C4B 1.369(7) . ? C5B C4B 1.379(7) . ? C5A C4A 1.372(7) . ? C20B C21B 1.382(7) . ? C20A C21A 1.372(7) . ? C3C C4C 1.378(8) . ? C23C C22C 1.387(7) . ? C23B C22B 1.376(7) . ? C20C C21C 1.356(8) . ? C21B C22B 1.365(8) . ? C23A C22A 1.361(7) . ? C2A C3A 1.379(8) . ? C22A C21A 1.383(8) . ? C3A C4A 1.379(9) . ? C22C C21C 1.352(8) . ? C5C C4C 1.388(8) . ? 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 O1D C5D C4D 95.7(16) . . ? C5D O1D C2D 108.2(18) . . ? O1D C2D C3D 107(2) . . ? C4D C3D C2D 103(3) . . ? C3D C4D C5D 115(3) . . ? N9C Ni1 N9A 99.36(12) . . ? N9C Ni1 N9B 97.51(13) . . ? N9A Ni1 N9B 96.84(12) . . ? N9C Ni1 N1B 91.01(13) . . ? N9A Ni1 N1B 168.99(13) . . ? N9B Ni1 N1B 78.00(13) . . ? N9C Ni1 N1A 171.26(14) . . ? N9A Ni1 N1A 78.12(13) . . ? N9B Ni1 N1A 91.12(14) . . ? N1B Ni1 N1A 92.16(13) . . ? N9C Ni1 N1C 78.15(13) . . ? N9A Ni1 N1C 93.40(13) . . ? N9B Ni1 N1C 169.43(13) . . ? N1B Ni1 N1C 92.35(13) . . ? N1A Ni1 N1C 93.58(14) . . ? N16C Ni2 N16B 97.42(13) . . ? N16C Ni2 N24C 78.56(13) . . ? N16B Ni2 N24C 171.17(13) . . ? N16C Ni2 N16A 98.82(12) . . ? N16B Ni2 N16A 97.60(12) . . ? N24C Ni2 N16A 90.82(13) . . ? N16C Ni2 N24A 172.12(13) . . ? N16B Ni2 N24A 90.33(13) . . ? N24C Ni2 N24A 93.96(14) . . ? N16A Ni2 N24A 78.65(13) . . ? N16C Ni2 N24B 90.82(13) . . ? N16B Ni2 N24B 78.38(13) . . ? N24C Ni2 N24B 93.73(14) . . ? N16A Ni2 N24B 170.00(13) . . ? N24A Ni2 N24B 92.14(13) . . ? O2W Co1 O2W 180.00(18) . 2_655 ? O2W Co1 O1W 90.00(14) . . ? O2W Co1 O1W 90.00(14) 2_655 . ? O2W Co1 O1W 90.00(14) . 2_655 ? O2W Co1 O1W 89.99(14) 2_655 2_655 ? O1W Co1 O1W 180.0(3) . 2_655 ? O2W Co1 O3W 89.89(12) . 2_655 ? O2W Co1 O3W 90.11(12) 2_655 2_655 ? O1W Co1 O3W 90.78(13) . 2_655 ? O1W Co1 O3W 89.22(13) 2_655 2_655 ? O2W Co1 O3W 90.11(12) . . ? O2W Co1 O3W 89.89(12) 2_655 . ? O1W Co1 O3W 89.22(13) . . ? O1W Co1 O3W 90.78(13) 2_655 . ? O3W Co1 O3W 180.0(2) 2_655 . ? O5W Co2 O5W 180.00(10) 2_866 . ? O5W Co2 O4W 89.87(15) 2_866 2_866 ? O5W Co2 O4W 90.13(15) . 2_866 ? O5W Co2 O4W 90.13(15) 2_866 . ? O5W Co2 O4W 89.87(15) . . ? O4W Co2 O4W 180.000(1) 2_866 . ? O5W Co2 O6W 86.61(12) 2_866 2_866 ? O5W Co2 O6W 93.39(12) . 2_866 ? O4W Co2 O6W 89.59(12) 2_866 2_866 ? O4W Co2 O6W 90.41(13) . 2_866 ? O5W Co2 O6W 93.39(12) 2_866 . ? O5W Co2 O6W 86.61(12) . . ? O4W Co2 O6W 90.41(13) 2_866 . ? O4W Co2 O6W 89.59(12) . . ? O6W Co2 O6W 180.000(1) 2_866 . ? C7B N9B C10B 117.6(3) . . ? C7B N9B Ni1 115.9(3) . . ? C10B N9B Ni1 125.5(2) . . ? C7A N9A C10A 117.7(3) . . ? C7A N9A Ni1 116.4(3) . . ? C10A N9A Ni1 125.1(2) . . ? C7C N9C C10C 116.7(3) . . ? C7C N9C Ni1 117.6(3) . . ? C10C N9C Ni1 125.7(2) . . ? C18A N16A C15A 118.1(3) . . ? C18A N16A Ni2 115.9(3) . . ? C15A N16A Ni2 125.0(2) . . ? C6C N1C C2C 118.2(4) . . ? C6C N1C Ni1 113.1(3) . . ? C2C N1C Ni1 128.7(3) . . ? C18C N16C C15C 117.6(3) . . ? C18C N16C Ni2 117.3(3) . . ? C15C N16C Ni2 124.6(2) . . ? C10A C11A C15A 120.5(3) . . ? C23C N24C C19C 117.6(4) . . ? C23C N24C Ni2 128.5(3) . . ? C19C N24C Ni2 113.9(3) . . ? C10C C11C C15C 120.4(4) . . ? C18B N16B C15B 118.0(3) . . ? C18B N16B Ni2 116.7(3) . . ? C15B N16B Ni2 124.9(2) . . ? C23A N24A C19A 118.6(4) . . ? C23A N24A Ni2 128.4(3) . . ? C19A N24A Ni2 113.0(3) . . ? C23B N24B C19B 118.2(4) . . ? C23B N24B Ni2 128.6(3) . . ? C19B N24B Ni2 113.2(3) . . ? C2B N1B C6B 118.2(4) . . ? C2B N1B Ni1 127.4(3) . . ? C6B N1B Ni1 114.4(3) . . ? C11B C15B C14B 119.3(3) . . ? C11B C15B N16B 119.4(3) . . ? C14B C15B N16B 121.2(3) . . ? C11B C10B C12B 119.2(3) . . ? C11B C10B N9B 119.7(3) . . ? C12B C10B N9B 121.1(3) . . ? C14C C13C C12C 121.1(4) . . ? O17A C18A N16A 128.3(4) . . ? O17A C18A C19A 117.3(3) . . ? N16A C18A C19A 114.4(3) . . ? C6A N1A C2A 118.0(4) . . ? C6A N1A Ni1 114.2(3) . . ? C2A N1A Ni1 127.8(3) . . ? C15B C11B C10B 121.0(3) . . ? N1C C6C C5C 122.2(4) . . ? N1C C6C C7C 117.2(4) . . ? C5C C6C C7C 120.6(4) . . ? N24B C19B C20B 121.9(4) . . ? N24B C19B C18B 116.5(3) . . ? C20B C19B C18B 121.7(4) . . ? C12A C10A C11A 119.5(3) . . ? C12A C10A N9A 120.9(3) . . ? C11A C10A N9A 119.3(3) . . ? N24A C19A C20A 121.6(4) . . ? N24A C19A C18A 117.1(3) . . ? C20A C19A C18A 121.3(4) . . ? C14A C13A C12A 120.5(4) . . ? C12B C13B C14B 120.9(4) . . ? N1B C6B C5B 121.7(4) . . ? N1B C6B C7B 115.8(3) . . ? C5B C6B C7B 122.4(4) . . ? C13B C12B C10B 119.8(4) . . ? C12C C10C C11C 119.8(4) . . ? C12C C10C N9C 121.6(4) . . ? C11C C10C N9C 118.4(3) . . ? O17B C18B N16B 128.3(4) . . ? O17B C18B C19B 116.6(3) . . ? N16B C18B C19B 115.0(4) . . ? O8B C7B N9B 127.0(4) . . ? O8B C7B C6B 117.7(3) . . ? N9B C7B C6B 115.2(3) . . ? C14C C15C C11C 119.2(4) . . ? C14C C15C N16C 121.0(3) . . ? C11C C15C N16C 119.5(3) . . ? C13C C12C C10C 119.6(4) . . ? C10A C12A C13A 120.0(4) . . ? N24C C19C C20C 121.9(4) . . ? N24C C19C C18C 116.2(4) . . ? C20C C19C C18C 121.9(4) . . ? O8C C7C N9C 128.3(4) . . ? O8C C7C C6C 117.9(4) . . ? N9C C7C C6C 113.8(4) . . ? C13C C14C C15C 119.9(4) . . ? C14A C15A C11A 119.6(3) . . ? C14A C15A N16A 120.5(3) . . ? C11A C15A N16A 119.7(3) . . ? C15A C14A C13A 119.8(4) . . ? O8A C7A N9A 128.6(4) . . ? O8A C7A C6A 116.6(3) . . ? N9A C7A C6A 114.7(3) . . ? C15B C14B C13B 119.7(4) . . ? O17C C18C N16C 129.5(4) . . ? O17C C18C C19C 116.6(4) . . ? N16C C18C C19C 113.8(4) . . ? N1C C2C C3C 123.3(5) . . ? N1A C6A C5A 122.3(4) . . ? N1A C6A C7A 115.9(3) . . ? C5A C6A C7A 121.8(4) . . ? C2B C3B C4B 118.1(4) . . ? N1B C2B C3B 123.4(4) . . ? C6B C5B C4B 119.0(5) . . ? C4A C5A C6A 119.4(5) . . ? C19B C20B C21B 119.6(5) . . ? C21A C20A C19A 118.8(5) . . ? C2C C3C C4C 118.4(5) . . ? N24C C23C C22C 122.2(5) . . ? N24B C23B C22B 122.4(5) . . ? C21C C20C C19C 119.8(5) . . ? C22B C21B C20B 118.5(4) . . ? C3B C4B C5B 119.5(5) . . ? N24A C23A C22A 122.9(5) . . ? C21B C22B C23B 119.5(5) . . ? N1A C2A C3A 122.2(5) . . ? C23A C22A C21A 118.7(5) . . ? C4A C3A C2A 119.7(5) . . ? C21C C22C C23C 119.0(5) . . ? C4C C5C C6C 118.3(5) . . ? C5A C4A C3A 118.3(5) . . ? C22C C21C C20C 119.4(5) . . ? C20A C21A C22A 119.4(5) . . ? C3C C4C C5C 119.7(5) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.063 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.111