# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Dr Duk-Young Jung' _publ_contact_author_email dyjung@skku.edu loop_ _publ_author_name 'YooJin Kim' 'Duk-Young Jung' # Attachment '- 2.cif' data_co3mi _database_code_depnum_ccdc_archive 'CCDC 795499' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co3(obc)3(bpy)2)(H2O) _chemical_melting_point ? _chemical_formula_moiety 'C62 H40 Co3 N4 O15, O' _chemical_formula_sum 'C62 H42 Co3 N4 O16' _chemical_formula_weight 1275.79 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.213(3) _cell_length_b 16.590(2) _cell_length_c 23.677(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.497(16) _cell_angle_gamma 90.00 _cell_volume 5924.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2596 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6611 _exptl_absorpt_correction_T_max 0.8401 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5391 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5187 _reflns_number_gt 3734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1141P)^2^+29.4738P] 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 5187 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.2036 _refine_ls_wR_factor_gt 0.1810 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.035 _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 Co1 Co 0.31210(5) 0.05022(4) 0.50294(3) 0.0258(2) Uani 1 1 d . . . Co2 Co 0.2500 0.2500 0.5000 0.0235(3) Uani 1 2 d S . . O1 O 0.4277(2) 0.1079(2) 0.52627(17) 0.0327(9) Uani 1 1 d . . . O4 O 0.2689(3) 0.0781(3) 0.57865(18) 0.0399(10) Uani 1 1 d . . . O5 O 0.3755(3) 0.2298(2) 0.54583(17) 0.0328(9) Uani 1 1 d . . . O6 O 0.1831(3) 0.1860(3) 0.55786(16) 0.0341(9) Uani 1 1 d . . . O8 O 0.0000 0.0142(5) 0.7500 0.121(5) Uani 1 2 d S . . N1 N 0.1977(3) -0.0230(3) 0.4839(2) 0.0405(13) Uani 1 1 d . . . N2 N 0.3553(3) -0.0615(3) 0.5381(2) 0.0300(11) Uani 1 1 d . . . C1 C 0.4336(4) 0.1762(3) 0.5504(2) 0.0268(12) Uani 1 1 d . . . C2 C 0.5189(4) 0.1928(3) 0.5880(2) 0.0272(12) Uani 1 1 d . . . C3 C 0.5873(4) 0.1382(4) 0.5917(3) 0.0344(13) Uani 1 1 d . . . H3 H 0.5810 0.0916 0.5697 0.041 Uiso 1 1 calc R . . C4 C 0.6656(4) 0.1512(4) 0.6278(3) 0.0389(15) Uani 1 1 d . . . H4 H 0.7111 0.1134 0.6305 0.047 Uiso 1 1 calc R . . C6 C 0.6068(4) 0.2763(4) 0.6566(3) 0.0443(16) Uani 1 1 d . . . H6 H 0.6128 0.3229 0.6787 0.053 Uiso 1 1 calc R . . C7 C 0.5290(4) 0.2618(4) 0.6203(3) 0.0373(14) Uani 1 1 d . . . H7 H 0.4833 0.2993 0.6179 0.045 Uiso 1 1 calc R . . C15 C 0.2071(4) 0.1257(3) 0.5866(2) 0.0280(12) Uani 1 1 d . . . C16 C 0.1570(4) 0.1038(4) 0.6351(2) 0.0328(13) Uani 1 1 d . . . C17 C 0.1769(5) 0.0322(4) 0.6647(3) 0.0515(19) Uani 1 1 d . . . H17 H 0.2255 0.0017 0.6574 0.062 Uiso 1 1 calc R . . C18 C 0.1255(6) 0.0065(4) 0.7045(4) 0.072(3) Uani 1 1 d . . . H18 H 0.1390 -0.0416 0.7240 0.086 Uiso 1 1 calc R . . C19 C 0.0539(6) 0.0515(4) 0.7159(3) 0.062(2) Uani 1 1 d . . . C20 C 0.0344(5) 0.1248(4) 0.6896(3) 0.0482(17) Uani 1 1 d . . . H20 H -0.0131 0.1558 0.6980 0.058 Uiso 1 1 calc R . . C21 C 0.0886(4) 0.1508(4) 0.6499(3) 0.0388(14) Uani 1 1 d . . . H21 H 0.0783 0.2011 0.6330 0.047 Uiso 1 1 calc R . . C22 C 0.1205(5) -0.0008(5) 0.4550(3) 0.0541(19) Uani 1 1 d . . . H22 H 0.1175 0.0486 0.4363 0.065 Uiso 1 1 calc R . . C23 C 0.0455(5) -0.0468(5) 0.4514(4) 0.060(2) Uani 1 1 d . . . H23 H -0.0067 -0.0293 0.4301 0.073 Uiso 1 1 calc R . . C24 C 0.0482(5) -0.1197(5) 0.4799(4) 0.062(2) Uani 1 1 d . . . H24 H -0.0023 -0.1515 0.4792 0.075 Uiso 1 1 calc R . . C25 C 0.1277(5) -0.1440(4) 0.5094(3) 0.0527(18) Uani 1 1 d . . . H25 H 0.1315 -0.1930 0.5286 0.063 Uiso 1 1 calc R . . C26 C 0.2024(4) -0.0954(4) 0.5107(3) 0.0378(14) Uani 1 1 d . . . C27 C 0.2900(4) -0.1171(4) 0.5398(3) 0.0359(14) Uani 1 1 d . . . C28 C 0.3082(5) -0.1893(4) 0.5688(3) 0.0509(18) Uani 1 1 d . . . H28 H 0.2634 -0.2269 0.5706 0.061 Uiso 1 1 calc R . . C29 C 0.3923(5) -0.2048(5) 0.5945(3) 0.060(2) Uani 1 1 d . . . H29 H 0.4045 -0.2527 0.6144 0.072 Uiso 1 1 calc R . . C30 C 0.4591(5) -0.1494(4) 0.5910(3) 0.0521(18) Uani 1 1 d . . . H30 H 0.5171 -0.1599 0.6071 0.063 Uiso 1 1 calc R . . C31 C 0.4373(4) -0.0780(4) 0.5628(3) 0.0395(15) Uani 1 1 d . . . H31 H 0.4815 -0.0397 0.5609 0.047 Uiso 1 1 calc R . . C5 C 0.6750(4) 0.2209(4) 0.6597(3) 0.0397(15) Uani 1 1 d . . . O2 O 0.7557(2) 0.3558(2) 0.94722(15) 0.0289(9) Uani 1 1 d . . . O3 O 0.8355(3) 0.4500(2) 0.91416(16) 0.0372(10) Uani 1 1 d . . . O7 O 0.7563(3) 0.2345(3) 0.69170(18) 0.0535(14) Uani 1 1 d . . . C8 C 0.7586(4) 0.2741(4) 0.7435(3) 0.0415(16) Uani 1 1 d . . . C9 C 0.8173(4) 0.3369(5) 0.7544(3) 0.0489(18) Uani 1 1 d . . . H9 H 0.8504 0.3543 0.7264 0.059 Uiso 1 1 calc R . . C10 C 0.8270(4) 0.3742(4) 0.8067(3) 0.0435(16) Uani 1 1 d . . . H10 H 0.8667 0.4167 0.8141 0.052 Uiso 1 1 calc R . . C11 C 0.7778(4) 0.3483(3) 0.8484(2) 0.0312(13) Uani 1 1 d . . . C12 C 0.7171(4) 0.2856(4) 0.8370(2) 0.0360(14) Uani 1 1 d . . . H12 H 0.6833 0.2684 0.8648 0.043 Uiso 1 1 calc R . . C13 C 0.7075(4) 0.2492(4) 0.7841(3) 0.0439(16) Uani 1 1 d . . . H13 H 0.6666 0.2078 0.7759 0.053 Uiso 1 1 calc R . . C14 C 0.7907(4) 0.3870(3) 0.9062(2) 0.0280(12) Uani 1 1 d . . . OW O 0.5000 0.0517(6) 0.7500 0.080 Uiso 1 2 d S . . 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 Co1 0.0241(4) 0.0259(4) 0.0270(4) 0.0010(3) 0.0019(3) 0.0007(3) Co2 0.0234(5) 0.0247(5) 0.0219(5) 0.0008(4) 0.0020(4) 0.0040(4) O1 0.024(2) 0.034(2) 0.039(2) -0.0116(18) 0.0007(17) -0.0023(17) O4 0.046(3) 0.041(2) 0.036(2) 0.0072(19) 0.020(2) 0.012(2) O5 0.027(2) 0.032(2) 0.038(2) -0.0016(17) -0.0018(17) 0.0064(18) O6 0.031(2) 0.041(2) 0.031(2) 0.0082(19) 0.0079(17) 0.0028(19) O8 0.202(12) 0.041(4) 0.157(10) 0.000 0.156(10) 0.000 N1 0.032(3) 0.039(3) 0.048(3) 0.002(2) -0.005(2) -0.008(2) N2 0.029(3) 0.029(3) 0.033(3) 0.000(2) 0.009(2) 0.002(2) C1 0.025(3) 0.032(3) 0.023(3) 0.002(2) 0.004(2) 0.000(2) C2 0.028(3) 0.029(3) 0.024(3) -0.002(2) 0.002(2) 0.002(2) C3 0.033(3) 0.034(3) 0.036(3) -0.009(3) 0.001(3) 0.002(3) C4 0.026(3) 0.053(4) 0.035(3) -0.010(3) -0.004(2) 0.007(3) C6 0.044(4) 0.044(4) 0.042(4) -0.017(3) -0.005(3) -0.001(3) C7 0.030(3) 0.036(3) 0.045(4) -0.009(3) -0.004(3) 0.007(3) C15 0.025(3) 0.034(3) 0.025(3) -0.001(2) 0.002(2) -0.001(2) C16 0.034(3) 0.034(3) 0.032(3) 0.001(2) 0.012(3) 0.000(3) C17 0.069(5) 0.041(4) 0.053(4) 0.013(3) 0.038(4) 0.018(3) C18 0.118(8) 0.035(4) 0.077(6) 0.014(4) 0.062(6) 0.012(4) C19 0.089(6) 0.039(4) 0.069(5) 0.000(4) 0.058(5) 0.001(4) C20 0.051(4) 0.044(4) 0.056(4) -0.002(3) 0.032(3) 0.004(3) C21 0.041(3) 0.036(3) 0.041(4) 0.001(3) 0.012(3) 0.003(3) C22 0.038(4) 0.056(4) 0.065(5) 0.006(4) -0.008(3) -0.001(3) C23 0.033(4) 0.073(6) 0.072(5) -0.002(4) -0.006(3) -0.004(4) C24 0.042(4) 0.064(5) 0.080(6) -0.017(4) 0.004(4) -0.020(4) C25 0.049(4) 0.046(4) 0.064(5) 0.000(3) 0.010(4) -0.017(3) C26 0.037(3) 0.037(3) 0.041(3) -0.005(3) 0.009(3) -0.003(3) C27 0.042(4) 0.030(3) 0.037(3) -0.003(3) 0.011(3) -0.003(3) C28 0.057(5) 0.035(4) 0.063(5) 0.011(3) 0.014(4) -0.008(3) C29 0.065(5) 0.045(4) 0.070(5) 0.023(4) 0.006(4) 0.016(4) C30 0.048(4) 0.050(4) 0.056(4) 0.012(3) -0.001(3) 0.013(4) C31 0.034(3) 0.039(3) 0.044(4) 0.006(3) 0.000(3) 0.005(3) C5 0.026(3) 0.062(4) 0.029(3) -0.010(3) -0.003(2) 0.003(3) O2 0.032(2) 0.032(2) 0.0237(19) 0.0001(16) 0.0069(16) -0.0067(18) O3 0.049(3) 0.034(2) 0.028(2) -0.0004(18) 0.0033(18) -0.015(2) O7 0.027(2) 0.097(4) 0.035(2) -0.029(3) -0.0048(19) -0.001(2) C8 0.030(3) 0.061(4) 0.032(3) -0.012(3) -0.005(3) 0.000(3) C9 0.044(4) 0.073(5) 0.030(3) -0.007(3) 0.006(3) -0.016(4) C10 0.044(4) 0.057(4) 0.030(3) -0.001(3) 0.005(3) -0.019(3) C11 0.030(3) 0.034(3) 0.028(3) 0.003(2) -0.003(2) -0.004(3) C12 0.032(3) 0.046(4) 0.028(3) -0.002(3) -0.003(2) -0.006(3) C13 0.035(3) 0.056(4) 0.039(4) -0.008(3) -0.004(3) -0.013(3) C14 0.026(3) 0.026(3) 0.030(3) 0.005(2) -0.002(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O1 2.015(4) . ? Co1 O4 2.041(4) . ? Co1 N2 2.102(5) . ? Co1 N1 2.122(5) . ? Co1 O2 2.148(4) 8_455 ? Co1 O3 2.177(4) 8_455 ? Co1 C14 2.499(6) 8_455 ? Co2 O5 2.096(4) . ? Co2 O5 2.096(4) 7_556 ? Co2 O6 2.098(4) . ? Co2 O6 2.098(4) 7_556 ? Co2 O2 2.163(4) 8_455 ? Co2 O2 2.163(4) 2_656 ? O1 C1 1.267(7) . ? O4 C15 1.260(7) . ? O5 C1 1.249(7) . ? O6 C15 1.237(7) . ? O8 C19 1.372(7) 2_556 ? O8 C19 1.372(7) . ? N1 C22 1.332(8) . ? N1 C26 1.355(8) . ? N2 C31 1.334(8) . ? N2 C27 1.361(7) . ? C1 C2 1.500(8) . ? C2 C3 1.373(8) . ? C2 C7 1.375(8) . ? C3 C4 1.390(8) . ? C4 C5 1.378(9) . ? C6 C5 1.381(9) . ? C6 C7 1.389(8) . ? C15 C16 1.505(8) . ? C16 C21 1.383(8) . ? C16 C17 1.391(9) . ? C17 C18 1.371(9) . ? C18 C19 1.374(11) . ? C19 C20 1.382(10) . ? C20 C21 1.395(9) . ? C22 C23 1.367(10) . ? C23 C24 1.383(12) . ? C24 C25 1.374(11) . ? C25 C26 1.390(9) . ? C26 C27 1.464(9) . ? C27 C28 1.389(9) . ? C28 C29 1.368(11) . ? C29 C30 1.381(10) . ? C30 C31 1.379(9) . ? C5 O7 1.383(7) . ? O2 C14 1.277(7) . ? O2 Co1 2.148(4) 8_556 ? O2 Co2 2.163(4) 2_656 ? O3 C14 1.249(7) . ? O3 Co1 2.177(4) 8_556 ? O7 C8 1.388(7) . ? C8 C9 1.375(9) . ? C8 C13 1.376(9) . ? C9 C10 1.375(9) . ? C10 C11 1.383(8) . ? C11 C12 1.394(8) . ? C11 C14 1.500(8) . ? C12 C13 1.381(8) . ? C14 Co1 2.499(6) 8_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 O1 Co1 O4 91.22(17) . . ? O1 Co1 N2 95.36(18) . . ? O4 Co1 N2 88.42(17) . . ? O1 Co1 N1 172.91(19) . . ? O4 Co1 N1 88.1(2) . . ? N2 Co1 N1 77.6(2) . . ? O1 Co1 O2 95.04(16) . 8_455 ? O4 Co1 O2 103.09(15) . 8_455 ? N2 Co1 O2 164.30(17) . 8_455 ? N1 Co1 O2 91.98(18) . 8_455 ? O1 Co1 O3 91.08(17) . 8_455 ? O4 Co1 O3 163.79(16) . 8_455 ? N2 Co1 O3 107.34(16) . 8_455 ? N1 Co1 O3 91.50(19) . 8_455 ? O2 Co1 O3 60.72(14) 8_455 8_455 ? O1 Co1 C14 93.34(17) . 8_455 ? O4 Co1 C14 133.82(17) . 8_455 ? N2 Co1 C14 136.62(18) . 8_455 ? N1 Co1 C14 92.20(19) . 8_455 ? O2 Co1 C14 30.74(16) 8_455 8_455 ? O3 Co1 C14 29.98(16) 8_455 8_455 ? O5 Co2 O5 180 . 7_556 ? O5 Co2 O6 93.89(16) . . ? O5 Co2 O6 86.11(16) 7_556 . ? O5 Co2 O6 86.11(16) . 7_556 ? O5 Co2 O6 93.89(16) 7_556 7_556 ? O6 Co2 O6 180 . 7_556 ? O5 Co2 O2 93.85(14) . 8_455 ? O5 Co2 O2 86.15(14) 7_556 8_455 ? O6 Co2 O2 91.50(15) . 8_455 ? O6 Co2 O2 88.50(15) 7_556 8_455 ? O5 Co2 O2 86.15(14) . 2_656 ? O5 Co2 O2 93.85(14) 7_556 2_656 ? O6 Co2 O2 88.50(15) . 2_656 ? O6 Co2 O2 91.50(15) 7_556 2_656 ? O2 Co2 O2 180 8_455 2_656 ? C1 O1 Co1 123.8(4) . . ? C15 O4 Co1 127.2(4) . . ? C1 O5 Co2 138.2(4) . . ? C15 O6 Co2 129.4(4) . . ? C19 O8 C19 126.4(8) 2_556 . ? C22 N1 C26 118.3(6) . . ? C22 N1 Co1 126.5(5) . . ? C26 N1 Co1 114.6(4) . . ? C31 N2 C27 119.5(5) . . ? C31 N2 Co1 125.5(4) . . ? C27 N2 Co1 114.7(4) . . ? O5 C1 O1 126.2(5) . . ? O5 C1 C2 117.9(5) . . ? O1 C1 C2 115.9(5) . . ? C3 C2 C7 119.0(5) . . ? C3 C2 C1 120.4(5) . . ? C7 C2 C1 120.5(5) . . ? C2 C3 C4 121.2(6) . . ? C5 C4 C3 119.1(6) . . ? C5 C6 C7 119.4(6) . . ? C2 C7 C6 120.8(6) . . ? O6 C15 O4 126.7(5) . . ? O6 C15 C16 118.2(5) . . ? O4 C15 C16 115.0(5) . . ? C21 C16 C17 118.4(6) . . ? C21 C16 C15 122.0(5) . . ? C17 C16 C15 119.5(5) . . ? C18 C17 C16 120.4(7) . . ? C17 C18 C19 120.2(7) . . ? O8 C19 C18 114.8(7) . . ? O8 C19 C20 123.6(7) . . ? C18 C19 C20 121.3(6) . . ? C19 C20 C21 117.7(6) . . ? C16 C21 C20 121.7(6) . . ? N1 C22 C23 123.4(7) . . ? C22 C23 C24 119.1(7) . . ? C25 C24 C23 118.2(7) . . ? C24 C25 C26 120.2(7) . . ? N1 C26 C25 120.7(6) . . ? N1 C26 C27 115.3(5) . . ? C25 C26 C27 124.0(6) . . ? N2 C27 C28 120.0(6) . . ? N2 C27 C26 116.2(5) . . ? C28 C27 C26 123.8(6) . . ? C29 C28 C27 119.8(7) . . ? C28 C29 C30 120.0(7) . . ? C31 C30 C29 117.9(7) . . ? N2 C31 C30 122.7(6) . . ? C4 C5 C6 120.5(6) . . ? C4 C5 O7 117.3(6) . . ? C6 C5 O7 122.2(6) . . ? C14 O2 Co1 90.0(3) . 8_556 ? C14 O2 Co2 145.2(4) . 2_656 ? Co1 O2 Co2 106.09(15) 8_556 2_656 ? C14 O3 Co1 89.4(3) . 8_556 ? C5 O7 C8 118.6(5) . . ? C9 C8 C13 120.6(6) . . ? C9 C8 O7 117.8(6) . . ? C13 C8 O7 121.6(6) . . ? C8 C9 C10 120.0(6) . . ? C9 C10 C11 119.9(6) . . ? C10 C11 C12 120.0(6) . . ? C10 C11 C14 119.9(5) . . ? C12 C11 C14 120.1(5) . . ? C13 C12 C11 119.4(6) . . ? C8 C13 C12 120.0(6) . . ? O3 C14 O2 119.9(5) . . ? O3 C14 C11 120.0(5) . . ? O2 C14 C11 120.1(5) . . ? O3 C14 Co1 60.6(3) . 8_556 ? O2 C14 Co1 59.3(3) . 8_556 ? C11 C14 Co1 179.2(4) . 8_556 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.206 _refine_diff_density_min -4.518 _refine_diff_density_rms 0.118 # Attachment '- 5.cif' data_cophen _database_code_depnum_ccdc_archive 'CCDC 795500' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Co3(obc)3(phen)2 _chemical_melting_point ? _chemical_formula_moiety 'C66 H40 Co3 N4 O15' _chemical_formula_sum 'C66 H40 Co3 N4 O15' _chemical_formula_weight 1305.81 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.138(2) _cell_length_b 16.501(2) _cell_length_c 25.844(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.021(2) _cell_angle_gamma 90.00 _cell_volume 6454.8(15) _cell_formula_units_Z 4 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 3794 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 26.52 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2660 _exptl_absorpt_coefficient_mu 0.829 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8195 _exptl_absorpt_correction_T_max 0.8999 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 253(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19222 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.0998 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.46 _reflns_number_total 7542 _reflns_number_gt 4036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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^)+(0.0810P)^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 7542 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1270 _refine_ls_R_factor_gt 0.0599 _refine_ls_wR_factor_ref 0.1692 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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 Co1 Co 0.47004(4) 0.17747(3) 0.50601(2) 0.03410(18) Uani 1 1 d . . . Co2 Co 0.2500 0.2500 0.5000 0.0280(2) Uani 1 2 d S . . N1 N 0.5493(3) 0.2538(2) 0.55529(14) 0.0466(9) Uani 1 1 d . . . N2 N 0.5982(2) 0.1276(2) 0.49834(13) 0.0392(8) Uani 1 1 d . . . O2 O 0.35406(18) 0.21325(17) 0.55437(9) 0.0359(6) Uani 1 1 d . . . O3 O 0.44044(19) 0.11003(17) 0.57425(10) 0.0439(7) Uani 1 1 d . . . O4 O 0.4646(2) 0.2667(2) 0.45459(12) 0.0547(9) Uani 1 1 d . . . O7 O 0.2401(2) 0.13490(19) 0.78742(11) 0.0561(9) Uani 1 1 d . . . O8 O 0.5000 0.4675(2) 0.2500 0.0497(11) Uani 1 2 d S . . C2 C 0.3105(3) -0.0428(2) 0.89551(14) 0.0341(9) Uani 1 1 d . . . C3 C 0.3703(3) 0.0173(3) 0.88252(15) 0.0406(10) Uani 1 1 d . . . H3 H 0.4255 0.0187 0.8989 0.049 Uiso 1 1 calc R . . C4 C 0.3492(3) 0.0754(3) 0.84549(16) 0.0454(11) Uani 1 1 d . . . H4 H 0.3899 0.1152 0.8370 0.055 Uiso 1 1 calc R . . C5 C 0.2673(3) 0.0733(3) 0.82153(15) 0.0447(11) Uani 1 1 d . . . C6 C 0.2066(3) 0.0136(3) 0.83295(16) 0.0513(12) Uani 1 1 d . . . H6 H 0.1519 0.0121 0.8161 0.062 Uiso 1 1 calc R . . C7 C 0.2290(3) -0.0443(3) 0.87009(16) 0.0454(11) Uani 1 1 d . . . H7 H 0.1885 -0.0847 0.8780 0.054 Uiso 1 1 calc R . . C8 C 0.2766(3) 0.1374(3) 0.73855(15) 0.0415(11) Uani 1 1 d . . . C9 C 0.3309(3) 0.0773(3) 0.71928(16) 0.0497(12) Uani 1 1 d . . . H9 H 0.3460 0.0325 0.7394 0.060 Uiso 1 1 calc R . . C10 C 0.3623(3) 0.0850(3) 0.66936(16) 0.0484(12) Uani 1 1 d . . . H10 H 0.3989 0.0449 0.6563 0.058 Uiso 1 1 calc R . . C11 C 0.3401(3) 0.1513(2) 0.63845(14) 0.0335(9) Uani 1 1 d . . . C12 C 0.2855(3) 0.2105(2) 0.65841(15) 0.0374(10) Uani 1 1 d . . . H12 H 0.2697 0.2549 0.6381 0.045 Uiso 1 1 calc R . . C13 C 0.2539(3) 0.2043(3) 0.70822(15) 0.0415(10) Uani 1 1 d . . . H13 H 0.2178 0.2447 0.7214 0.050 Uiso 1 1 calc R . . C14 C 0.3784(3) 0.1581(2) 0.58593(15) 0.0352(9) Uani 1 1 d . . . C15 C 0.4041(3) 0.3130(3) 0.43690(15) 0.0364(10) Uani 1 1 d . . . C16 C 0.4258(3) 0.3534(2) 0.38588(14) 0.0330(9) Uani 1 1 d . . . C17 C 0.3816(3) 0.4202(2) 0.36747(15) 0.0398(10) Uani 1 1 d . . . H17 H 0.3356 0.4419 0.3865 0.048 Uiso 1 1 calc R . . C18 C 0.4041(3) 0.4561(3) 0.32096(15) 0.0402(10) Uani 1 1 d . . . H18 H 0.3731 0.5009 0.3086 0.048 Uiso 1 1 calc R . . C19 C 0.4734(3) 0.4244(3) 0.29329(14) 0.0375(10) Uani 1 1 d . . . C20 C 0.5169(3) 0.3560(3) 0.31011(15) 0.0427(10) Uani 1 1 d . . . H20 H 0.5620 0.3337 0.2907 0.051 Uiso 1 1 calc R . . C21 C 0.4927(3) 0.3207(3) 0.35640(15) 0.0405(10) Uani 1 1 d . . . H21 H 0.5218 0.2742 0.3679 0.049 Uiso 1 1 calc R . . C22 C 0.5226(4) 0.3156(3) 0.5830(2) 0.0771(18) Uani 1 1 d . . . H22 H 0.4639 0.3317 0.5797 0.092 Uiso 1 1 calc R . . C23 C 0.5775(5) 0.3582(4) 0.6168(3) 0.107(3) Uani 1 1 d . . . H23 H 0.5555 0.4010 0.6362 0.129 Uiso 1 1 calc R . . C24 C 0.6646(5) 0.3363(4) 0.6214(3) 0.095(2) Uani 1 1 d . . . H24 H 0.7023 0.3641 0.6439 0.113 Uiso 1 1 calc R . . C25 C 0.6967(4) 0.2721(3) 0.59197(19) 0.0570(13) Uani 1 1 d . . . C26 C 0.6347(3) 0.2326(3) 0.55909(16) 0.0427(11) Uani 1 1 d . . . C27 C 0.6626(3) 0.1645(3) 0.52831(15) 0.0390(10) Uani 1 1 d . . . C28 C 0.7504(3) 0.1387(3) 0.52990(18) 0.0504(12) Uani 1 1 d . . . C29 C 0.7723(3) 0.0709(3) 0.5009(2) 0.0646(15) Uani 1 1 d . . . H29 H 0.8301 0.0517 0.5011 0.078 Uiso 1 1 calc R . . C30 C 0.7078(3) 0.0323(3) 0.47175(19) 0.0605(14) Uani 1 1 d . . . H30 H 0.7217 -0.0135 0.4525 0.073 Uiso 1 1 calc R . . C31 C 0.6215(3) 0.0623(3) 0.47127(17) 0.0483(11) Uani 1 1 d . . . H31 H 0.5787 0.0357 0.4514 0.058 Uiso 1 1 calc R . . C32 C 0.7862(4) 0.2448(3) 0.5928(2) 0.0666(15) Uani 1 1 d . . . H32 H 0.8275 0.2706 0.6141 0.080 Uiso 1 1 calc R . . C33 C 0.8119(3) 0.1820(4) 0.5630(2) 0.0649(15) Uani 1 1 d . . . H33 H 0.8709 0.1663 0.5639 0.078 Uiso 1 1 calc R . . O1 O 0.4107(2) -0.09914(19) 0.95683(11) 0.0487(8) Uani 1 1 d . . . O5 O 0.27546(19) -0.15532(17) 0.94875(10) 0.0406(7) Uani 1 1 d . . . C1 C 0.3338(3) -0.1045(2) 0.93716(14) 0.0332(9) Uani 1 1 d . . . O6 O 0.33140(19) 0.32746(17) 0.45705(11) 0.0425(7) 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 Co1 0.0327(3) 0.0431(3) 0.0265(3) -0.0012(2) 0.0007(2) 0.0014(3) Co2 0.0299(4) 0.0339(4) 0.0205(4) 0.0005(3) 0.0048(3) 0.0014(3) N1 0.046(2) 0.045(2) 0.049(2) -0.0075(18) -0.0014(18) 0.0010(19) N2 0.037(2) 0.046(2) 0.0350(19) -0.0002(16) 0.0053(16) 0.0002(17) O2 0.0375(16) 0.0447(16) 0.0255(14) 0.0057(12) 0.0021(12) 0.0040(14) O3 0.0424(17) 0.0531(18) 0.0365(16) 0.0032(14) 0.0074(13) 0.0140(15) O4 0.0414(19) 0.076(2) 0.0471(18) 0.0276(17) 0.0070(15) 0.0009(17) O7 0.070(2) 0.065(2) 0.0340(17) 0.0232(15) 0.0182(15) 0.0273(18) O8 0.077(3) 0.045(2) 0.028(2) 0.000 0.022(2) 0.000 C2 0.037(2) 0.042(2) 0.0240(19) 0.0036(17) 0.0034(17) -0.0021(19) C3 0.036(2) 0.054(3) 0.032(2) 0.008(2) -0.0003(18) -0.005(2) C4 0.046(3) 0.051(3) 0.040(2) 0.011(2) 0.008(2) -0.004(2) C5 0.056(3) 0.055(3) 0.024(2) 0.012(2) 0.011(2) 0.011(2) C6 0.048(3) 0.070(3) 0.036(2) 0.009(2) -0.007(2) 0.004(3) C7 0.038(3) 0.056(3) 0.043(2) 0.012(2) -0.002(2) -0.012(2) C8 0.051(3) 0.048(3) 0.026(2) 0.0086(19) 0.0060(19) 0.009(2) C9 0.067(3) 0.048(3) 0.034(2) 0.016(2) 0.006(2) 0.020(2) C10 0.061(3) 0.050(3) 0.035(2) 0.008(2) 0.010(2) 0.017(2) C11 0.039(2) 0.040(2) 0.0221(19) 0.0051(17) 0.0007(17) 0.0059(19) C12 0.045(3) 0.039(2) 0.028(2) 0.0064(18) 0.0007(18) 0.007(2) C13 0.048(3) 0.046(3) 0.030(2) 0.0065(19) 0.0036(19) 0.015(2) C14 0.034(2) 0.043(2) 0.029(2) 0.0009(18) -0.0020(17) -0.001(2) C15 0.035(2) 0.044(2) 0.030(2) 0.0037(18) 0.0039(18) -0.008(2) C16 0.029(2) 0.043(2) 0.027(2) 0.0028(17) 0.0038(16) -0.0056(19) C17 0.044(3) 0.040(2) 0.036(2) -0.0024(19) 0.0133(19) 0.001(2) C18 0.045(3) 0.044(2) 0.031(2) 0.0012(19) 0.0072(19) 0.001(2) C19 0.042(2) 0.046(2) 0.025(2) -0.0031(18) 0.0070(18) -0.005(2) C20 0.042(3) 0.056(3) 0.031(2) 0.003(2) 0.0110(19) 0.008(2) C21 0.031(2) 0.054(3) 0.037(2) 0.008(2) -0.0010(18) 0.006(2) C22 0.066(4) 0.065(4) 0.101(5) -0.036(3) 0.003(3) -0.004(3) C23 0.081(5) 0.094(5) 0.147(7) -0.075(5) -0.001(5) -0.016(4) C24 0.078(5) 0.102(5) 0.103(5) -0.055(4) -0.014(4) -0.027(4) C25 0.054(3) 0.067(3) 0.050(3) -0.002(3) -0.006(2) -0.023(3) C26 0.042(3) 0.047(3) 0.039(2) 0.004(2) -0.003(2) -0.006(2) C27 0.032(2) 0.051(3) 0.033(2) 0.006(2) -0.0009(18) -0.008(2) C28 0.038(3) 0.063(3) 0.051(3) 0.009(2) 0.003(2) -0.001(2) C29 0.034(3) 0.081(4) 0.080(4) 0.004(3) 0.014(3) 0.007(3) C30 0.052(3) 0.061(3) 0.070(4) -0.010(3) 0.022(3) 0.008(3) C31 0.041(3) 0.056(3) 0.049(3) -0.011(2) 0.009(2) 0.002(2) C32 0.050(3) 0.089(4) 0.060(3) -0.001(3) -0.013(3) -0.025(3) C33 0.035(3) 0.098(4) 0.061(3) 0.014(3) -0.008(2) -0.006(3) O1 0.0401(18) 0.064(2) 0.0415(17) 0.0184(15) -0.0075(14) -0.0065(16) O5 0.0431(18) 0.0444(17) 0.0343(16) 0.0101(13) -0.0001(13) -0.0063(14) C1 0.039(2) 0.039(2) 0.0214(19) 0.0024(17) 0.0050(17) 0.003(2) O6 0.0428(18) 0.0469(17) 0.0381(16) 0.0037(13) 0.0149(14) -0.0014(14) _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 Co1 O4 1.984(3) . ? Co1 O1 2.013(3) 6 ? Co1 N2 2.120(3) . ? Co1 O3 2.140(3) . ? Co1 N1 2.143(4) . ? Co1 O2 2.252(3) . ? Co2 O5 2.088(3) 4_556 ? Co2 O5 2.088(3) 6 ? Co2 O6 2.106(3) . ? Co2 O6 2.106(3) 7_556 ? Co2 O2 2.178(3) . ? Co2 O2 2.178(3) 7_556 ? N1 C22 1.314(6) . ? N1 C26 1.342(6) . ? N2 C31 1.336(5) . ? N2 C27 1.376(5) . ? O2 C14 1.272(4) . ? O3 C14 1.270(5) . ? O4 C15 1.271(5) . ? O7 C8 1.388(5) . ? O7 C5 1.402(5) . ? O8 C19 1.391(4) . ? O8 C19 1.391(4) 2_655 ? C2 C3 1.388(5) . ? C2 C7 1.389(5) . ? C2 C1 1.518(5) . ? C3 C4 1.388(5) . ? C4 C5 1.376(6) . ? C5 C6 1.384(6) . ? C6 C7 1.391(6) . ? C8 C9 1.386(6) . ? C8 C13 1.393(5) . ? C9 C10 1.389(6) . ? C10 C11 1.392(5) . ? C11 C12 1.386(5) . ? C11 C14 1.490(5) . ? C12 C13 1.384(5) . ? C15 O6 1.249(5) . ? C15 C16 1.519(5) . ? C16 C17 1.371(5) . ? C16 C21 1.388(6) . ? C17 C18 1.388(5) . ? C18 C19 1.382(5) . ? C19 C20 1.374(6) . ? C20 C21 1.386(5) . ? C22 C23 1.386(8) . ? C23 C24 1.371(9) . ? C24 C25 1.395(8) . ? C25 C26 1.414(6) . ? C25 C32 1.428(7) . ? C26 C27 1.443(6) . ? C27 C28 1.396(6) . ? C28 C29 1.391(7) . ? C28 C33 1.444(7) . ? C29 C30 1.378(7) . ? C30 C31 1.397(6) . ? C32 C33 1.351(7) . ? O1 C1 1.265(5) . ? O1 Co1 2.013(3) 6_556 ? O5 C1 1.258(5) . ? O5 Co2 2.088(3) 4_546 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Co1 O1 92.33(14) . 6 ? O4 Co1 N2 104.63(13) . . ? O1 Co1 N2 95.20(13) 6 . ? O4 Co1 O3 158.64(13) . . ? O1 Co1 O3 95.10(12) 6 . ? N2 Co1 O3 94.62(12) . . ? O4 Co1 N1 88.75(14) . . ? O1 Co1 N1 172.45(14) 6 . ? N2 Co1 N1 77.31(14) . . ? O3 Co1 N1 86.51(13) . . ? O4 Co1 O2 98.84(12) . . ? O1 Co1 O2 100.10(11) 6 . ? N2 Co1 O2 151.34(11) . . ? O3 Co1 O2 60.14(10) . . ? N1 Co1 O2 87.11(13) . . ? O5 Co2 O5 180 4_556 6 ? O5 Co2 O6 89.81(11) 4_556 . ? O5 Co2 O6 90.19(11) 6 . ? O5 Co2 O6 90.19(11) 4_556 7_556 ? O5 Co2 O6 89.81(11) 6 7_556 ? O6 Co2 O6 180 . 7_556 ? O5 Co2 O2 86.48(10) 4_556 . ? O5 Co2 O2 93.52(10) 6 . ? O6 Co2 O2 94.92(11) . . ? O6 Co2 O2 85.08(11) 7_556 . ? O5 Co2 O2 93.52(10) 4_556 7_556 ? O5 Co2 O2 86.48(10) 6 7_556 ? O6 Co2 O2 85.08(11) . 7_556 ? O6 Co2 O2 94.92(11) 7_556 7_556 ? O2 Co2 O2 180 . 7_556 ? C22 N1 C26 117.9(4) . . ? C22 N1 Co1 127.3(4) . . ? C26 N1 Co1 114.7(3) . . ? C31 N2 C27 117.5(4) . . ? C31 N2 Co1 127.8(3) . . ? C27 N2 Co1 114.6(3) . . ? C14 O2 Co2 144.1(3) . . ? C14 O2 Co1 87.0(2) . . ? Co2 O2 Co1 106.08(10) . . ? C14 O3 Co1 92.2(2) . . ? C15 O4 Co1 135.1(3) . . ? C8 O7 C5 118.4(3) . . ? C19 O8 C19 118.5(4) . 2_655 ? C3 C2 C7 118.4(4) . . ? C3 C2 C1 120.5(4) . . ? C7 C2 C1 121.1(4) . . ? C2 C3 C4 121.2(4) . . ? C5 C4 C3 119.2(4) . . ? C4 C5 C6 121.2(4) . . ? C4 C5 O7 121.2(4) . . ? C6 C5 O7 117.5(4) . . ? C5 C6 C7 118.8(4) . . ? C2 C7 C6 121.2(4) . . ? C9 C8 O7 123.6(4) . . ? C9 C8 C13 120.4(4) . . ? O7 C8 C13 115.9(4) . . ? C8 C9 C10 118.9(4) . . ? C9 C10 C11 121.5(4) . . ? C12 C11 C10 118.7(4) . . ? C12 C11 C14 122.0(3) . . ? C10 C11 C14 119.3(4) . . ? C13 C12 C11 120.8(4) . . ? C12 C13 C8 119.7(4) . . ? O3 C14 O2 120.1(4) . . ? O3 C14 C11 118.1(3) . . ? O2 C14 C11 121.7(4) . . ? O6 C15 O4 126.8(4) . . ? O6 C15 C16 118.9(4) . . ? O4 C15 C16 114.3(4) . . ? C17 C16 C21 118.7(4) . . ? C17 C16 C15 122.9(4) . . ? C21 C16 C15 118.5(4) . . ? C16 C17 C18 121.1(4) . . ? C19 C18 C17 119.2(4) . . ? C20 C19 C18 120.7(4) . . ? C20 C19 O8 122.0(4) . . ? C18 C19 O8 117.1(4) . . ? C19 C20 C21 119.1(4) . . ? C20 C21 C16 121.1(4) . . ? N1 C22 C23 123.4(6) . . ? C24 C23 C22 119.0(6) . . ? C23 C24 C25 119.8(5) . . ? C24 C25 C26 116.3(5) . . ? C24 C25 C32 124.8(5) . . ? C26 C25 C32 118.8(5) . . ? N1 C26 C25 123.5(4) . . ? N1 C26 C27 117.0(4) . . ? C25 C26 C27 119.5(4) . . ? N2 C27 C28 123.1(4) . . ? N2 C27 C26 116.3(4) . . ? C28 C27 C26 120.6(4) . . ? C29 C28 C27 117.8(4) . . ? C29 C28 C33 124.1(5) . . ? C27 C28 C33 118.1(5) . . ? C30 C29 C28 119.5(5) . . ? C29 C30 C31 119.7(5) . . ? N2 C31 C30 122.5(4) . . ? C33 C32 C25 121.1(5) . . ? C32 C33 C28 121.8(5) . . ? C1 O1 Co1 127.3(3) . 6_556 ? C1 O5 Co2 142.0(3) . 4_546 ? O5 C1 O1 126.6(4) . . ? O5 C1 C2 117.5(4) . . ? O1 C1 C2 116.0(4) . . ? C15 O6 Co2 129.2(3) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 28.46 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.869 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.089 data_mn3mi _database_code_depnum_ccdc_archive 'CCDC 795501' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Mn3(obc)3(bpy)2 _chemical_melting_point ? _chemical_formula_moiety 'C62 H40 Mn3 N4 O15' _chemical_formula_sum 'C62 H40 Mn3 N4 O15' _chemical_formula_weight 1245.80 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.271(4) _cell_length_b 17.077(4) _cell_length_c 25.897(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.986(11) _cell_angle_gamma 90.00 _cell_volume 6303(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 6.2 _cell_measurement_theta_max 16.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2540 _exptl_absorpt_coefficient_mu 0.658 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7788 _exptl_absorpt_correction_T_max 0.8581 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5627 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5399 _reflns_number_gt 4286 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+18.0622P] 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 0.00031(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5399 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1343 _refine_ls_wR_factor_gt 0.1140 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 Mn1 Mn 0.00772(3) 0.17698(3) 0.491873(18) 0.03387(17) Uani 1 1 d . . . Mn2 Mn 0.2500 0.2500 0.5000 0.02921(18) Uani 1 2 d S . . O1 O 0.06953(18) 0.10420(18) 0.54870(10) 0.0556(7) Uani 1 1 d . . . O4 O 0.48331(18) 0.22536(18) 0.46027(10) 0.0535(7) Uani 1 1 d . . . O5 O 0.21321(18) 0.15741(15) 0.55329(9) 0.0464(6) Uani 1 1 d . . . O6 O 0.34091(18) 0.16958(15) 0.46020(9) 0.0455(6) Uani 1 1 d . . . O8 O 0.5000 0.0408(2) 0.2500 0.0441(8) Uani 1 2 d S . . N1 N -0.0998(3) 0.24288(19) 0.44055(13) 0.0532(8) Uani 1 1 d . . . N2 N -0.13337(19) 0.11664(17) 0.49677(11) 0.0397(7) Uani 1 1 d . . . C1 C 0.1538(2) 0.1094(2) 0.56676(12) 0.0379(8) Uani 1 1 d . . . C2 C 0.1818(2) 0.0500(2) 0.60824(12) 0.0374(8) Uani 1 1 d . . . C3 C 0.1215(3) -0.0110(2) 0.61916(13) 0.0456(9) Uani 1 1 d . . . H3 H 0.0627 -0.0136 0.6020 0.055 Uiso 1 1 calc R . . C4 C 0.1474(3) -0.0681(2) 0.65523(14) 0.0517(10) Uani 1 1 d . . . H4 H 0.1070 -0.1093 0.6618 0.062 Uiso 1 1 calc R . . C6 C 0.2949(3) -0.0020(3) 0.67183(15) 0.0528(10) Uani 1 1 d . . . H6 H 0.3526 0.0015 0.6901 0.063 Uiso 1 1 calc R . . C7 C 0.2691(3) 0.0540(2) 0.63484(14) 0.0491(9) Uani 1 1 d . . . H7 H 0.3103 0.0943 0.6278 0.059 Uiso 1 1 calc R . . C15 C 0.4181(2) 0.1825(2) 0.44080(12) 0.0365(7) Uani 1 1 d . . . C16 C 0.4376(2) 0.1460(2) 0.38932(12) 0.0345(7) Uani 1 1 d . . . C17 C 0.4998(2) 0.1823(2) 0.35758(13) 0.0407(8) Uani 1 1 d . . . H17 H 0.5290 0.2286 0.3686 0.049 Uiso 1 1 calc R . . C18 C 0.5196(2) 0.1514(2) 0.31006(13) 0.0419(8) Uani 1 1 d . . . H18 H 0.5605 0.1770 0.2889 0.050 Uiso 1 1 calc R . . C19 C 0.4772(2) 0.0812(2) 0.29448(11) 0.0352(7) Uani 1 1 d . . . C20 C 0.4138(3) 0.0455(2) 0.32490(13) 0.0431(8) Uani 1 1 d . . . H20 H 0.3842 -0.0005 0.3137 0.052 Uiso 1 1 calc R . . C21 C 0.3940(3) 0.0777(2) 0.37217(13) 0.0438(8) Uani 1 1 d . . . H21 H 0.3509 0.0533 0.3926 0.053 Uiso 1 1 calc R . . C22 C -0.0783(4) 0.3069(3) 0.4138(2) 0.0832(16) Uani 1 1 d . . . H22 H -0.0165 0.3244 0.4147 0.100 Uiso 1 1 calc R . . C23 C -0.1466(7) 0.3474(4) 0.3848(3) 0.120(3) Uani 1 1 d . . . H23 H -0.1305 0.3916 0.3662 0.144 Uiso 1 1 calc R . . C24 C -0.2365(7) 0.3229(5) 0.3834(3) 0.134(3) Uani 1 1 d . . . H24 H -0.2822 0.3494 0.3634 0.160 Uiso 1 1 calc R . . C25 C -0.2602(5) 0.2587(4) 0.4117(3) 0.099(2) Uani 1 1 d . . . H25 H -0.3223 0.2424 0.4121 0.119 Uiso 1 1 calc R . . C26 C -0.1899(3) 0.2184(2) 0.43972(15) 0.0526(10) Uani 1 1 d . . . C27 C -0.2079(2) 0.1465(2) 0.46907(15) 0.0458(9) Uani 1 1 d . . . C28 C -0.2954(3) 0.1094(3) 0.46851(19) 0.0698(13) Uani 1 1 d . . . H28 H -0.3470 0.1312 0.4503 0.084 Uiso 1 1 calc R . . C29 C -0.3043(3) 0.0401(4) 0.4953(2) 0.0791(15) Uani 1 1 d . . . H29 H -0.3619 0.0146 0.4949 0.095 Uiso 1 1 calc R . . C30 C -0.2284(3) 0.0091(3) 0.52239(19) 0.0653(12) Uani 1 1 d . . . H30 H -0.2333 -0.0378 0.5403 0.078 Uiso 1 1 calc R . . C31 C -0.1447(3) 0.0488(2) 0.52260(15) 0.0503(9) Uani 1 1 d . . . H31 H -0.0932 0.0280 0.5414 0.060 Uiso 1 1 calc R . . C5 C 0.2341(3) -0.0630(2) 0.68130(13) 0.0489(9) Uani 1 1 d . . . O7 O 0.2646(2) -0.12203(19) 0.71584(10) 0.0642(9) Uani 1 1 d . . . O2 O 0.13516(16) -0.21836(15) 0.94065(8) 0.0402(6) Uani 1 1 d . . . O3 O 0.05323(18) -0.11041(16) 0.92541(9) 0.0501(7) Uani 1 1 d . . . C8 C 0.2236(3) -0.1296(2) 0.76275(13) 0.0460(9) Uani 1 1 d . . . C9 C 0.1660(3) -0.0718(2) 0.78256(14) 0.0523(10) Uani 1 1 d . . . H9 H 0.1512 -0.0268 0.7637 0.063 Uiso 1 1 calc R . . C10 C 0.1314(3) -0.0834(2) 0.83127(14) 0.0485(9) Uani 1 1 d . . . H10 H 0.0922 -0.0459 0.8447 0.058 Uiso 1 1 calc R . . C11 C 0.1541(2) -0.1496(2) 0.86019(12) 0.0376(8) Uani 1 1 d . . . C12 C 0.2122(3) -0.2059(2) 0.84006(13) 0.0421(8) Uani 1 1 d . . . H12 H 0.2282 -0.2504 0.8593 0.051 Uiso 1 1 calc R . . C13 C 0.2466(3) -0.1957(2) 0.79116(13) 0.0468(9) Uani 1 1 d . . . H13 H 0.2851 -0.2337 0.7776 0.056 Uiso 1 1 calc R . . C14 C 0.1129(2) -0.1600(2) 0.91184(12) 0.0358(7) 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 Mn1 0.0301(3) 0.0448(3) 0.0266(3) 0.0013(2) 0.00098(19) -0.0026(2) Mn2 0.0287(3) 0.0376(4) 0.0219(3) -0.0022(3) 0.0060(2) -0.0059(3) O1 0.0409(14) 0.0743(19) 0.0501(15) 0.0226(14) -0.0107(12) -0.0054(13) O4 0.0461(15) 0.0705(18) 0.0441(14) -0.0225(13) 0.0036(12) -0.0050(13) O5 0.0472(14) 0.0508(15) 0.0415(13) 0.0162(12) 0.0052(11) -0.0095(12) O6 0.0482(15) 0.0503(15) 0.0397(13) -0.0073(11) 0.0187(11) -0.0010(12) O8 0.060(2) 0.049(2) 0.0241(16) 0.000 0.0127(15) 0.000 N1 0.061(2) 0.0473(19) 0.0501(19) 0.0087(15) -0.0076(16) 0.0032(16) N2 0.0330(15) 0.0422(16) 0.0437(16) 0.0015(13) 0.0014(12) -0.0002(13) C1 0.0366(18) 0.050(2) 0.0276(16) 0.0041(15) 0.0034(13) -0.0035(16) C2 0.0351(17) 0.051(2) 0.0262(15) 0.0063(15) 0.0005(13) -0.0045(15) C3 0.0381(19) 0.061(2) 0.0375(18) 0.0142(17) -0.0012(15) -0.0072(17) C4 0.051(2) 0.057(2) 0.048(2) 0.0175(19) 0.0081(17) -0.0076(19) C6 0.042(2) 0.070(3) 0.046(2) 0.0142(19) -0.0076(17) 0.0008(19) C7 0.0386(19) 0.063(2) 0.045(2) 0.0101(18) -0.0039(16) -0.0063(18) C15 0.0385(18) 0.0393(18) 0.0321(17) -0.0025(14) 0.0060(14) 0.0047(15) C16 0.0335(17) 0.0431(19) 0.0272(16) -0.0017(14) 0.0035(13) 0.0026(14) C17 0.0350(18) 0.052(2) 0.0357(17) -0.0061(16) 0.0020(14) -0.0061(16) C18 0.0365(18) 0.058(2) 0.0319(17) 0.0006(16) 0.0101(14) -0.0083(16) C19 0.0384(17) 0.0458(19) 0.0219(15) 0.0012(14) 0.0043(13) 0.0041(15) C20 0.055(2) 0.042(2) 0.0330(17) -0.0037(15) 0.0108(16) -0.0091(17) C21 0.053(2) 0.046(2) 0.0339(17) -0.0019(15) 0.0165(15) -0.0078(17) C22 0.102(4) 0.057(3) 0.091(4) 0.032(3) 0.001(3) -0.004(3) C23 0.158(7) 0.075(4) 0.123(6) 0.055(4) -0.021(5) 0.007(5) C24 0.145(7) 0.107(6) 0.141(7) 0.046(5) -0.067(6) 0.031(5) C25 0.087(4) 0.089(4) 0.115(5) 0.010(4) -0.047(4) 0.025(3) C26 0.050(2) 0.056(2) 0.050(2) -0.0090(19) -0.0162(18) 0.0122(19) C27 0.0323(18) 0.056(2) 0.049(2) -0.0091(18) -0.0025(15) 0.0051(16) C28 0.035(2) 0.094(4) 0.080(3) -0.013(3) -0.005(2) 0.001(2) C29 0.045(3) 0.094(4) 0.100(4) -0.005(3) 0.018(3) -0.027(3) C30 0.054(3) 0.065(3) 0.080(3) 0.003(2) 0.025(2) -0.012(2) C31 0.043(2) 0.053(2) 0.056(2) 0.0033(19) 0.0114(17) -0.0026(18) C5 0.052(2) 0.065(3) 0.0297(17) 0.0155(17) 0.0101(16) 0.0172(19) O7 0.0697(19) 0.084(2) 0.0406(14) 0.0335(14) 0.0237(13) 0.0363(16) O2 0.0384(13) 0.0536(15) 0.0287(11) 0.0099(11) 0.0023(9) 0.0063(11) O3 0.0515(15) 0.0597(16) 0.0402(13) 0.0107(12) 0.0143(11) 0.0194(13) C8 0.0419(19) 0.066(2) 0.0310(17) 0.0128(17) 0.0065(14) 0.0134(18) C9 0.059(2) 0.057(2) 0.042(2) 0.0235(18) 0.0102(17) 0.0202(19) C10 0.051(2) 0.055(2) 0.0406(19) 0.0144(17) 0.0119(16) 0.0208(18) C11 0.0344(17) 0.050(2) 0.0279(16) 0.0080(15) 0.0024(13) 0.0066(15) C12 0.045(2) 0.048(2) 0.0338(18) 0.0099(15) 0.0030(15) 0.0120(16) C13 0.049(2) 0.057(2) 0.0352(18) 0.0116(17) 0.0107(16) 0.0175(18) C14 0.0304(16) 0.050(2) 0.0269(16) 0.0048(14) -0.0004(13) 0.0036(15) _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 Mn1 O4 2.078(3) 7_556 ? Mn1 O1 2.086(3) . ? Mn1 O3 2.189(3) 6 ? Mn1 N2 2.271(3) . ? Mn1 N1 2.275(3) . ? Mn1 O2 2.412(2) 6 ? Mn1 C14 2.637(3) 6 ? Mn2 O5 2.181(2) 7_556 ? Mn2 O5 2.181(2) . ? Mn2 O6 2.184(2) 7_556 ? Mn2 O6 2.184(2) . ? Mn2 O2 2.253(2) 6 ? Mn2 O2 2.253(2) 4_556 ? O1 C1 1.270(4) . ? O4 C15 1.268(4) . ? O4 Mn1 2.078(3) 7_556 ? O5 C1 1.243(4) . ? O6 C15 1.254(4) . ? O8 C19 1.395(4) . ? O8 C19 1.395(4) 2_655 ? N1 C22 1.339(6) . ? N1 C26 1.351(5) . ? N2 C31 1.351(5) . ? N2 C27 1.352(4) . ? C1 C2 1.515(5) . ? C2 C3 1.390(5) . ? C2 C7 1.393(5) . ? C3 C4 1.388(5) . ? C4 C5 1.381(5) . ? C6 C5 1.386(6) . ? C6 C7 1.389(5) . ? C15 C16 1.510(4) . ? C16 C21 1.385(5) . ? C16 C17 1.387(5) . ? C17 C18 1.382(5) . ? C18 C19 1.393(5) . ? C19 C20 1.373(5) . ? C20 C21 1.385(5) . ? C22 C23 1.385(8) . ? C23 C24 1.348(11) . ? C24 C25 1.371(10) . ? C25 C26 1.390(6) . ? C26 C27 1.473(6) . ? C27 C28 1.400(6) . ? C28 C29 1.381(7) . ? C29 C30 1.367(7) . ? C30 C31 1.374(6) . ? C5 O7 1.402(4) . ? O7 C8 1.381(4) . ? O2 C14 1.275(4) . ? O2 Mn2 2.253(2) 4_546 ? O2 Mn1 2.412(2) 6_556 ? O3 C14 1.263(4) . ? O3 Mn1 2.189(3) 6_556 ? C8 C13 1.378(5) . ? C8 C9 1.399(5) . ? C9 C10 1.393(5) . ? C10 C11 1.385(5) . ? C11 C12 1.389(5) . ? C11 C14 1.500(4) . ? C12 C13 1.392(5) . ? C14 Mn1 2.637(3) 6_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 O4 Mn1 O1 92.68(12) 7_556 . ? O4 Mn1 O3 150.95(10) 7_556 6 ? O1 Mn1 O3 96.50(12) . 6 ? O4 Mn1 N2 110.98(11) 7_556 . ? O1 Mn1 N2 91.93(10) . . ? O3 Mn1 N2 96.23(10) 6 . ? O4 Mn1 N1 88.29(12) 7_556 . ? O1 Mn1 N1 162.61(12) . . ? O3 Mn1 N1 90.93(12) 6 . ? N2 Mn1 N1 71.59(12) . . ? O4 Mn1 O2 93.91(10) 7_556 6 ? O1 Mn1 O2 105.02(10) . 6 ? O3 Mn1 O2 57.09(9) 6 6 ? N2 Mn1 O2 149.28(9) . 6 ? N1 Mn1 O2 92.22(11) . 6 ? O4 Mn1 C14 122.49(11) 7_556 6 ? O1 Mn1 C14 104.58(11) . 6 ? O3 Mn1 C14 28.46(10) 6 6 ? N2 Mn1 C14 122.44(10) . 6 ? N1 Mn1 C14 89.39(12) . 6 ? O2 Mn1 C14 28.82(9) 6 6 ? O5 Mn2 O5 180 7_556 . ? O5 Mn2 O6 90.65(10) 7_556 7_556 ? O5 Mn2 O6 89.35(10) . 7_556 ? O5 Mn2 O6 89.35(10) 7_556 . ? O5 Mn2 O6 90.65(10) . . ? O6 Mn2 O6 180 7_556 . ? O5 Mn2 O2 86.14(9) 7_556 6 ? O5 Mn2 O2 93.86(9) . 6 ? O6 Mn2 O2 92.51(9) 7_556 6 ? O6 Mn2 O2 87.49(9) . 6 ? O5 Mn2 O2 93.86(9) 7_556 4_556 ? O5 Mn2 O2 86.14(9) . 4_556 ? O6 Mn2 O2 87.49(9) 7_556 4_556 ? O6 Mn2 O2 92.51(9) . 4_556 ? O2 Mn2 O2 180 6 4_556 ? C1 O1 Mn1 125.1(2) . . ? C15 O4 Mn1 136.2(2) . 7_556 ? C1 O5 Mn2 147.8(2) . . ? C15 O6 Mn2 129.4(2) . . ? C19 O8 C19 120.8(4) . 2_655 ? C22 N1 C26 119.3(4) . . ? C22 N1 Mn1 122.7(3) . . ? C26 N1 Mn1 117.9(3) . . ? C31 N2 C27 118.4(3) . . ? C31 N2 Mn1 123.1(2) . . ? C27 N2 Mn1 118.3(2) . . ? O5 C1 O1 126.1(3) . . ? O5 C1 C2 118.8(3) . . ? O1 C1 C2 115.1(3) . . ? C3 C2 C7 118.9(3) . . ? C3 C2 C1 120.1(3) . . ? C7 C2 C1 121.0(3) . . ? C4 C3 C2 121.2(3) . . ? C5 C4 C3 119.0(4) . . ? C5 C6 C7 119.6(4) . . ? C6 C7 C2 120.4(4) . . ? O6 C15 O4 125.8(3) . . ? O6 C15 C16 119.2(3) . . ? O4 C15 C16 115.1(3) . . ? C21 C16 C17 118.5(3) . . ? C21 C16 C15 122.0(3) . . ? C17 C16 C15 119.5(3) . . ? C18 C17 C16 121.6(3) . . ? C17 C18 C19 118.8(3) . . ? C20 C19 C18 120.4(3) . . ? C20 C19 O8 116.3(3) . . ? C18 C19 O8 123.2(3) . . ? C19 C20 C21 120.1(3) . . ? C16 C21 C20 120.6(3) . . ? N1 C22 C23 121.0(6) . . ? C24 C23 C22 120.1(6) . . ? C23 C24 C25 119.7(6) . . ? C24 C25 C26 118.9(6) . . ? N1 C26 C25 121.0(5) . . ? N1 C26 C27 116.2(3) . . ? C25 C26 C27 122.8(5) . . ? N2 C27 C28 120.8(4) . . ? N2 C27 C26 115.7(3) . . ? C28 C27 C26 123.5(4) . . ? C29 C28 C27 119.2(4) . . ? C30 C29 C28 120.0(4) . . ? C29 C30 C31 118.5(5) . . ? N2 C31 C30 123.2(4) . . ? C4 C5 C6 120.9(3) . . ? C4 C5 O7 120.5(4) . . ? C6 C5 O7 118.5(3) . . ? C8 O7 C5 119.8(3) . . ? C14 O2 Mn2 137.5(2) . 4_546 ? C14 O2 Mn1 85.45(18) . 6_556 ? Mn2 O2 Mn1 103.75(9) 4_546 6_556 ? C14 O3 Mn1 95.9(2) . 6_556 ? C13 C8 O7 116.5(3) . . ? C13 C8 C9 120.7(3) . . ? O7 C8 C9 122.7(3) . . ? C10 C9 C8 118.3(3) . . ? C11 C10 C9 121.5(3) . . ? C10 C11 C12 119.3(3) . . ? C10 C11 C14 119.2(3) . . ? C12 C11 C14 121.5(3) . . ? C11 C12 C13 120.0(3) . . ? C8 C13 C12 120.2(3) . . ? O3 C14 O2 120.8(3) . . ? O3 C14 C11 118.0(3) . . ? O2 C14 C11 121.1(3) . . ? O3 C14 Mn1 55.67(17) . 6_556 ? O2 C14 Mn1 65.74(16) . 6_556 ? C11 C14 Mn1 168.4(2) . 6_556 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.460 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.068 # Attachment '- 4.cif' data_24 _database_code_depnum_ccdc_archive 'CCDC 795502' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Mn3(obc)3(phen)2)(2H2O) _chemical_melting_point ? _chemical_formula_moiety 'C66 H40 Mn3 N4 O15, 2(O H2)' _chemical_formula_sum 'C66 H44 Mn3 N4 O17' _chemical_formula_weight 1345.88 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2/c ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.2012(11) _cell_length_b 16.7136(12) _cell_length_c 25.8544(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.2600(10) _cell_angle_gamma 90.00 _cell_volume 6568.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 5.30 _cell_measurement_theta_max 12.49 _exptl_crystal_description BLOCK _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2708 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7844 _exptl_absorpt_correction_T_max 0.9104 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19575 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7617 _reflns_number_gt 5368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^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 7617 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Mn1 Mn 0.47472(2) 0.17864(2) 0.498993(12) 0.03391(11) Uani 1 1 d . . . Mn2 Mn 0.2500 0.2500 0.5000 0.02911(12) Uani 1 2 d S . . O1 O 0.42429(12) 0.09956(11) 0.55391(7) 0.0559(5) Uani 1 1 d . . . O2 O 0.35735(10) -0.22090(10) 0.94361(6) 0.0414(4) Uani 1 1 d . . . O3 O 0.43711(12) -0.11370(10) 0.92893(6) 0.0489(4) Uani 1 1 d . . . O4 O 0.45812(11) 0.27650(12) 0.54704(7) 0.0545(5) Uani 1 1 d . . . O5 O 0.29028(11) 0.15298(10) 0.55293(6) 0.0459(4) Uani 1 1 d . . . O6 O 0.32664(11) 0.33436(10) 0.54481(6) 0.0441(4) Uani 1 1 d . . . O7 O 0.23855(13) -0.13077(12) 0.71348(6) 0.0620(5) Uani 1 1 d . . . O8 O 0.5000 0.47645(14) 0.7500 0.0572(7) Uani 1 2 d S . . N1 N 0.61001(12) 0.12134(12) 0.50270(7) 0.0398(4) Uani 1 1 d . . . N2 N 0.56479(14) 0.25448(12) 0.45016(8) 0.0487(5) Uani 1 1 d . . . C1 C 0.34572(15) 0.10364(13) 0.56855(8) 0.0367(5) Uani 1 1 d . . . C2 C 0.31864(14) 0.04295(13) 0.60843(8) 0.0364(5) Uani 1 1 d . . . C3 C 0.23762(16) 0.04797(16) 0.63200(9) 0.0469(6) Uani 1 1 d . . . H3 H 0.1997 0.0897 0.6236 0.056 Uiso 1 1 calc R . . C4 C 0.21213(17) -0.00906(17) 0.66839(10) 0.0530(6) Uani 1 1 d . . . H4 H 0.1579 -0.0051 0.6846 0.064 Uiso 1 1 calc R . . C5 C 0.26782(17) -0.07082(16) 0.67988(8) 0.0482(6) Uani 1 1 d . . . C6 C 0.34853(17) -0.07763(16) 0.65667(9) 0.0490(6) Uani 1 1 d . . . H6 H 0.3854 -0.1202 0.6647 0.059 Uiso 1 1 calc R . . C7 C 0.37455(15) -0.02015(15) 0.62094(9) 0.0440(5) Uani 1 1 d . . . H7 H 0.4294 -0.0239 0.6054 0.053 Uiso 1 1 calc R . . C8 C 0.27624(16) -0.13610(15) 0.76226(8) 0.0440(5) Uani 1 1 d . . . C9 C 0.33219(18) -0.07899(17) 0.78234(9) 0.0540(7) Uani 1 1 d . . . H9 H 0.3478 -0.0346 0.7628 0.065 Uiso 1 1 calc R . . C10 C 0.36483(17) -0.08854(16) 0.83202(9) 0.0494(6) Uani 1 1 d . . . H10 H 0.4028 -0.0504 0.8457 0.059 Uiso 1 1 calc R . . C11 C 0.34153(14) -0.15437(14) 0.86158(8) 0.0381(5) Uani 1 1 d . . . C12 C 0.28455(15) -0.21067(14) 0.84105(8) 0.0413(5) Uani 1 1 d . . . H12 H 0.2680 -0.2547 0.8608 0.050 Uiso 1 1 calc R . . C13 C 0.25199(16) -0.20176(15) 0.79117(9) 0.0464(6) Uani 1 1 d . . . H13 H 0.2140 -0.2399 0.7773 0.056 Uiso 1 1 calc R . . C14 C 0.37974(14) -0.16290(14) 0.91441(8) 0.0372(5) Uani 1 1 d . . . C15 C 0.39945(15) 0.32080(13) 0.56495(8) 0.0370(5) Uani 1 1 d . . . C16 C 0.42226(13) 0.36134(13) 0.61547(7) 0.0328(4) Uani 1 1 d . . . C17 C 0.49172(14) 0.33111(15) 0.64449(9) 0.0419(5) Uani 1 1 d . . . H17 H 0.5216 0.2860 0.6329 0.050 Uiso 1 1 calc R . . C18 C 0.51721(16) 0.36677(16) 0.69024(9) 0.0456(6) Uani 1 1 d . . . H18 H 0.5638 0.3461 0.7095 0.055 Uiso 1 1 calc R . . C19 C 0.47242(16) 0.43355(14) 0.70693(8) 0.0404(5) Uani 1 1 d . . . C20 C 0.40051(16) 0.46287(14) 0.67993(8) 0.0425(5) Uani 1 1 d . . . H20 H 0.3689 0.5063 0.6925 0.051 Uiso 1 1 calc R . . C21 C 0.37652(15) 0.42634(14) 0.63381(8) 0.0394(5) Uani 1 1 d . . . H21 H 0.3289 0.4461 0.6150 0.047 Uiso 1 1 calc R . . C22 C 0.63100(17) 0.05427(15) 0.52692(10) 0.0488(6) Uani 1 1 d . . . H22 H 0.5882 0.0292 0.5467 0.059 Uiso 1 1 calc R . . C23 C 0.71417(18) 0.01924(18) 0.52420(11) 0.0599(7) Uani 1 1 d . . . H23 H 0.7264 -0.0279 0.5419 0.072 Uiso 1 1 calc R . . C24 C 0.77726(18) 0.0556(2) 0.49493(12) 0.0658(8) Uani 1 1 d . . . H24 H 0.8329 0.0329 0.4925 0.079 Uiso 1 1 calc R . . C25 C 0.75851(16) 0.12705(18) 0.46850(10) 0.0537(7) Uani 1 1 d . . . C26 C 0.67224(15) 0.15737(15) 0.47322(9) 0.0416(5) Uani 1 1 d . . . C27 C 0.64817(16) 0.22783(15) 0.44548(9) 0.0445(6) Uani 1 1 d . . . C28 C 0.7104(2) 0.26716(19) 0.41370(12) 0.0629(8) Uani 1 1 d . . . C29 C 0.82041(19) 0.1694(2) 0.43740(13) 0.0693(9) Uani 1 1 d . . . H29 H 0.8779 0.1507 0.4353 0.083 Uiso 1 1 calc R . . C30 C 0.7978(2) 0.2352(2) 0.41119(14) 0.0746(10) Uani 1 1 d . . . H30 H 0.8395 0.2608 0.3909 0.089 Uiso 1 1 calc R . . C31 C 0.6825(3) 0.3344(2) 0.38786(15) 0.0859(11) Uani 1 1 d . . . H31 H 0.7214 0.3618 0.3665 0.103 Uiso 1 1 calc R . . C32 C 0.5988(3) 0.3612(2) 0.39322(17) 0.0963(13) Uani 1 1 d . . . H32 H 0.5802 0.4070 0.3759 0.116 Uiso 1 1 calc R . . C33 C 0.5406(2) 0.31933(18) 0.42514(13) 0.0716(9) Uani 1 1 d . . . H33 H 0.4833 0.3379 0.4287 0.086 Uiso 1 1 calc R . . O9 O 0.9497(5) 0.3819(4) 0.3550(3) 0.238(3) 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 Mn1 0.03387(18) 0.0404(2) 0.02746(17) 0.00183(13) 0.00204(12) 0.00199(14) Mn2 0.0312(2) 0.0334(2) 0.0228(2) -0.00179(17) -0.00357(16) 0.00290(18) O1 0.0527(10) 0.0630(11) 0.0522(10) 0.0229(9) 0.0170(8) 0.0081(9) O2 0.0416(8) 0.0527(9) 0.0300(8) 0.0098(7) 0.0026(6) -0.0016(7) O3 0.0608(10) 0.0481(10) 0.0378(8) 0.0013(7) -0.0105(7) -0.0125(8) O4 0.0431(9) 0.0717(12) 0.0487(10) -0.0279(9) -0.0017(7) -0.0006(9) O5 0.0512(9) 0.0452(9) 0.0413(9) 0.0148(7) -0.0050(7) 0.0055(8) O6 0.0474(9) 0.0458(9) 0.0390(8) -0.0048(7) -0.0143(7) -0.0020(7) O7 0.0774(12) 0.0719(13) 0.0367(9) 0.0235(9) -0.0179(8) -0.0334(10) O8 0.103(2) 0.0369(12) 0.0318(12) 0.000 -0.0292(12) 0.000 N1 0.0369(9) 0.0431(11) 0.0393(10) 0.0001(8) 0.0005(8) -0.0007(8) N2 0.0548(13) 0.0403(11) 0.0509(12) 0.0096(9) 0.0061(9) -0.0013(9) C1 0.0436(12) 0.0392(12) 0.0274(10) 0.0035(9) 0.0001(9) -0.0004(10) C2 0.0436(12) 0.0404(12) 0.0251(10) 0.0061(9) -0.0019(8) -0.0001(10) C3 0.0437(13) 0.0525(15) 0.0444(13) 0.0096(11) 0.0032(10) 0.0019(11) C4 0.0487(14) 0.0648(17) 0.0455(14) 0.0103(12) 0.0072(11) -0.0063(13) C5 0.0604(15) 0.0556(15) 0.0285(11) 0.0113(10) -0.0082(10) -0.0157(12) C6 0.0559(15) 0.0484(14) 0.0427(13) 0.0155(11) -0.0101(11) 0.0020(12) C7 0.0443(12) 0.0499(14) 0.0378(12) 0.0092(10) -0.0016(9) 0.0042(11) C8 0.0516(13) 0.0511(14) 0.0292(11) 0.0102(10) -0.0061(9) -0.0127(11) C9 0.0691(17) 0.0547(16) 0.0381(12) 0.0197(11) -0.0077(11) -0.0244(13) C10 0.0588(15) 0.0535(15) 0.0360(12) 0.0086(11) -0.0080(10) -0.0218(12) C11 0.0418(12) 0.0437(12) 0.0287(10) 0.0050(9) 0.0013(9) -0.0033(10) C12 0.0519(13) 0.0407(12) 0.0314(11) 0.0118(9) -0.0013(9) -0.0078(11) C13 0.0544(14) 0.0494(14) 0.0351(12) 0.0065(10) -0.0053(10) -0.0192(11) C14 0.0405(12) 0.0429(12) 0.0283(10) 0.0003(9) 0.0028(9) 0.0009(10) C15 0.0414(12) 0.0396(12) 0.0301(10) -0.0033(9) 0.0004(9) -0.0074(10) C16 0.0344(10) 0.0363(11) 0.0278(10) -0.0001(8) -0.0003(8) -0.0057(9) C17 0.0375(12) 0.0496(14) 0.0385(12) -0.0058(10) -0.0010(9) 0.0049(10) C18 0.0429(12) 0.0582(15) 0.0358(12) 0.0001(11) -0.0096(9) 0.0051(11) C19 0.0605(14) 0.0356(12) 0.0249(10) 0.0014(9) -0.0074(9) -0.0064(10) C20 0.0621(15) 0.0340(12) 0.0313(11) -0.0003(9) -0.0052(10) 0.0054(11) C21 0.0464(12) 0.0400(12) 0.0316(11) 0.0013(9) -0.0098(9) 0.0039(10) C22 0.0495(14) 0.0454(14) 0.0513(14) 0.0037(11) -0.0064(11) 0.0033(11) C23 0.0568(16) 0.0568(17) 0.0658(18) 0.0007(14) -0.0199(14) 0.0103(14) C24 0.0418(14) 0.078(2) 0.077(2) -0.0174(17) -0.0111(14) 0.0158(14) C25 0.0372(13) 0.0711(19) 0.0528(15) -0.0192(14) 0.0016(11) -0.0013(12) C26 0.0370(11) 0.0488(13) 0.0391(12) -0.0108(10) 0.0027(9) -0.0049(10) C27 0.0475(13) 0.0466(14) 0.0396(12) -0.0058(10) 0.0086(10) -0.0113(11) C28 0.0636(17) 0.0691(19) 0.0562(16) -0.0029(14) 0.0142(13) -0.0251(15) C29 0.0394(14) 0.097(3) 0.072(2) -0.0205(19) 0.0110(13) -0.0081(15) C30 0.0541(17) 0.097(3) 0.073(2) -0.0140(19) 0.0281(15) -0.0270(18) C31 0.097(3) 0.075(2) 0.086(2) 0.0254(19) 0.020(2) -0.032(2) C32 0.108(3) 0.072(2) 0.109(3) 0.046(2) 0.008(2) -0.016(2) C33 0.083(2) 0.0510(17) 0.081(2) 0.0242(15) 0.0083(17) 0.0013(15) _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 Mn1 O4 2.0700(17) . ? Mn1 O1 2.0881(17) . ? Mn1 O3 2.1856(16) 6 ? Mn1 N2 2.256(2) . ? Mn1 N1 2.2702(19) . ? Mn1 O2 2.3894(16) 6 ? Mn1 C14 2.628(2) 6 ? Mn2 O6 2.1622(15) 7_556 ? Mn2 O6 2.1622(15) . ? Mn2 O5 2.2067(15) . ? Mn2 O5 2.2067(15) 7_556 ? Mn2 O2 2.2465(14) 4_556 ? Mn2 O2 2.2465(14) 6 ? O1 C1 1.256(3) . ? O2 C14 1.276(3) . ? O2 Mn2 2.2465(14) 4_546 ? O2 Mn1 2.3894(16) 6_556 ? O3 C14 1.255(3) . ? O3 Mn1 2.1856(16) 6_556 ? O4 C15 1.250(3) . ? O5 C1 1.245(3) . ? O6 C15 1.242(3) . ? O7 C8 1.386(3) . ? O7 C5 1.400(3) . ? O8 C19 1.388(2) . ? O8 C19 1.388(2) 2_656 ? N1 C22 1.322(3) . ? N1 C26 1.358(3) . ? N2 C33 1.314(4) . ? N2 C27 1.349(3) . ? C1 C2 1.505(3) . ? C2 C3 1.379(3) . ? C2 C7 1.392(3) . ? C3 C4 1.395(4) . ? C3 H3 0.9300 . ? C4 C5 1.367(4) . ? C4 H4 0.9300 . ? C5 C6 1.373(4) . ? C6 C7 1.391(3) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.378(3) . ? C8 C13 1.379(3) . ? C9 C10 1.384(3) . ? C9 H9 0.9300 . ? C10 C11 1.386(3) . ? C10 H10 0.9300 . ? C11 C12 1.383(3) . ? C11 C14 1.489(3) . ? C12 C13 1.387(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 Mn1 2.628(2) 6_556 ? C15 C16 1.511(3) . ? C16 C21 1.375(3) . ? C16 C17 1.388(3) . ? C17 C18 1.378(3) . ? C17 H17 0.9300 . ? C18 C19 1.378(3) . ? C18 H18 0.9300 . ? C19 C20 1.384(3) . ? C20 C21 1.387(3) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.395(4) . ? C22 H22 0.9300 . ? C23 C24 1.367(4) . ? C23 H23 0.9300 . ? C24 C25 1.404(4) . ? C24 H24 0.9300 . ? C25 C26 1.412(3) . ? C25 C29 1.428(4) . ? C26 C27 1.426(4) . ? C27 C28 1.417(3) . ? C28 C31 1.373(5) . ? C28 C30 1.434(5) . ? C29 C30 1.336(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.357(5) . ? C31 H31 0.9300 . ? C32 C33 1.399(5) . ? C32 H32 0.9300 . ? C33 H33 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 O4 Mn1 O1 92.63(8) . . ? O4 Mn1 O3 149.05(7) . 6 ? O1 Mn1 O3 98.84(8) . 6 ? O4 Mn1 N2 88.16(8) . . ? O1 Mn1 N2 164.08(8) . . ? O3 Mn1 N2 88.41(8) 6 . ? O4 Mn1 N1 114.89(7) . . ? O1 Mn1 N1 92.26(7) . . ? O3 Mn1 N1 93.38(7) 6 . ? N2 Mn1 N1 73.07(7) . . ? O4 Mn1 O2 91.91(6) . 6 ? O1 Mn1 O2 108.61(7) . 6 ? O3 Mn1 O2 57.20(6) 6 6 ? N2 Mn1 O2 87.25(7) . 6 ? N1 Mn1 O2 145.47(6) . 6 ? O4 Mn1 C14 120.69(7) . 6 ? O1 Mn1 C14 107.48(7) . 6 ? O3 Mn1 C14 28.36(6) 6 6 ? N2 Mn1 C14 85.59(8) . 6 ? N1 Mn1 C14 119.14(7) . 6 ? O2 Mn1 C14 28.96(6) 6 6 ? O6 Mn2 O6 180 7_556 . ? O6 Mn2 O5 90.02(6) 7_556 . ? O6 Mn2 O5 89.98(6) . . ? O6 Mn2 O5 89.98(6) 7_556 7_556 ? O6 Mn2 O5 90.02(6) . 7_556 ? O5 Mn2 O5 180 . 7_556 ? O6 Mn2 O2 95.61(6) 7_556 4_556 ? O6 Mn2 O2 84.39(6) . 4_556 ? O5 Mn2 O2 87.53(6) . 4_556 ? O5 Mn2 O2 92.47(6) 7_556 4_556 ? O6 Mn2 O2 84.39(6) 7_556 6 ? O6 Mn2 O2 95.61(6) . 6 ? O5 Mn2 O2 92.47(6) . 6 ? O5 Mn2 O2 87.53(6) 7_556 6 ? O2 Mn2 O2 180 4_556 6 ? C1 O1 Mn1 121.53(15) . . ? C14 O2 Mn2 138.17(15) . 4_546 ? C14 O2 Mn1 85.96(13) . 6_556 ? Mn2 O2 Mn1 102.57(6) 4_546 6_556 ? C14 O3 Mn1 95.81(13) . 6_556 ? C15 O4 Mn1 141.23(15) . . ? C1 O5 Mn2 150.84(15) . . ? C15 O6 Mn2 125.64(15) . . ? C8 O7 C5 118.66(18) . . ? C19 O8 C19 117.8(2) . 2_656 ? C22 N1 C26 118.3(2) . . ? C22 N1 Mn1 126.46(16) . . ? C26 N1 Mn1 114.98(15) . . ? C33 N2 C27 119.3(2) . . ? C33 N2 Mn1 124.8(2) . . ? C27 N2 Mn1 115.93(16) . . ? O5 C1 O1 125.5(2) . . ? O5 C1 C2 118.8(2) . . ? O1 C1 C2 115.7(2) . . ? C3 C2 C7 119.3(2) . . ? C3 C2 C1 120.6(2) . . ? C7 C2 C1 120.09(19) . . ? C2 C3 C4 120.5(2) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.3(2) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.4(2) . . ? C4 C5 O7 118.5(2) . . ? C6 C5 O7 119.9(2) . . ? C5 C6 C7 119.4(2) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C6 C7 C2 120.2(2) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? C9 C8 C13 120.9(2) . . ? C9 C8 O7 123.4(2) . . ? C13 C8 O7 115.7(2) . . ? C8 C9 C10 119.2(2) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C9 C10 C11 120.8(2) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 119.3(2) . . ? C12 C11 C14 121.9(2) . . ? C10 C11 C14 118.8(2) . . ? C11 C12 C13 120.3(2) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C8 C13 C12 119.6(2) . . ? C8 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? O3 C14 O2 120.52(19) . . ? O3 C14 C11 118.64(19) . . ? O2 C14 C11 120.8(2) . . ? O3 C14 Mn1 55.83(11) . 6_556 ? O2 C14 Mn1 65.08(11) . 6_556 ? C11 C14 Mn1 169.61(15) . 6_556 ? O6 C15 O4 126.1(2) . . ? O6 C15 C16 118.8(2) . . ? O4 C15 C16 115.13(19) . . ? C21 C16 C17 119.07(19) . . ? C21 C16 C15 122.55(19) . . ? C17 C16 C15 118.4(2) . . ? C18 C17 C16 121.1(2) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C19 C18 C17 118.8(2) . . ? C19 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C18 C19 C20 121.3(2) . . ? C18 C19 O8 121.5(2) . . ? C20 C19 O8 117.2(2) . . ? C19 C20 C21 118.8(2) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C16 C21 C20 120.8(2) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? N1 C22 C23 123.3(2) . . ? N1 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? C24 C23 C22 118.6(3) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 120.4(2) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 116.7(2) . . ? C24 C25 C29 124.2(3) . . ? C26 C25 C29 119.0(3) . . ? N1 C26 C25 122.6(2) . . ? N1 C26 C27 118.1(2) . . ? C25 C26 C27 119.3(2) . . ? N2 C27 C28 121.9(3) . . ? N2 C27 C26 117.8(2) . . ? C28 C27 C26 120.3(2) . . ? C31 C28 C27 117.2(3) . . ? C31 C28 C30 124.5(3) . . ? C27 C28 C30 118.3(3) . . ? C30 C29 C25 121.7(3) . . ? C30 C29 H29 119.2 . . ? C25 C29 H29 119.2 . . ? C29 C30 C28 121.3(3) . . ? C29 C30 H30 119.3 . . ? C28 C30 H30 119.3 . . ? C32 C31 C28 120.5(3) . . ? C32 C31 H31 119.7 . . ? C28 C31 H31 119.7 . . ? C31 C32 C33 119.4(3) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? N2 C33 C32 121.8(3) . . ? N2 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.701 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.066 # Attachment '- 3.cif' data_ni3mi _database_code_depnum_ccdc_archive 'CCDC 795503' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ni3(obc)3(bpy)2)(H2O) _chemical_melting_point ? _chemical_formula_moiety 'C62 H40 N4 Ni3 O15, O' _chemical_formula_sum 'C62 H42 N4 Ni3 O16' _chemical_formula_weight 1275.07 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.163(5) _cell_length_b 16.373(4) _cell_length_c 23.383(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.486(18) _cell_angle_gamma 90.00 _cell_volume 5756(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 33 _cell_measurement_theta_min 5.45 _cell_measurement_theta_max 17.81 _exptl_crystal_description 'BLOCK ' _exptl_crystal_colour 'GREEN ' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 1.046 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1881 _exptl_absorpt_correction_T_max 0.2150 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5218 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0717 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5020 _reflns_number_gt 3358 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1175P)^2^+41.7070P] 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 0.00023(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5020 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2221 _refine_ls_wR_factor_gt 0.1867 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.010 _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 0.30999(5) 0.05113(5) 0.50287(3) 0.0285(3) Uani 1 1 d . . . Ni2 Ni 0.2500 0.2500 0.5000 0.0269(3) Uani 1 2 d S . . O1 O 0.4248(3) 0.1082(3) 0.5254(2) 0.0332(11) Uani 1 1 d . . . O4 O 0.2707(3) 0.0790(3) 0.5790(2) 0.0392(12) Uani 1 1 d . . . O5 O 0.3729(3) 0.2313(3) 0.54575(19) 0.0331(11) Uani 1 1 d . . . O6 O 0.1834(3) 0.1867(3) 0.5566(2) 0.0353(11) Uani 1 1 d . . . O8 O 0.0000 0.0139(6) 0.7500 0.124(6) Uani 1 2 d S . . N1 N 0.1969(4) -0.0194(4) 0.4847(3) 0.0362(14) Uani 1 1 d . . . N2 N 0.3545(4) -0.0580(3) 0.5376(2) 0.0332(13) Uani 1 1 d . . . C1 C 0.4311(4) 0.1768(4) 0.5499(3) 0.0301(15) Uani 1 1 d . . . C2 C 0.5164(4) 0.1939(4) 0.5867(3) 0.0306(15) Uani 1 1 d . . . C3 C 0.5853(5) 0.1385(5) 0.5902(3) 0.0384(17) Uani 1 1 d . . . H3 H 0.5788 0.0911 0.5681 0.046 Uiso 1 1 calc R . . C4 C 0.6639(5) 0.1523(5) 0.6262(3) 0.0408(18) Uani 1 1 d . . . H4 H 0.7099 0.1143 0.6282 0.049 Uiso 1 1 calc R . . C5 C 0.6736(5) 0.2219(5) 0.6585(3) 0.0400(18) Uani 1 1 d . . . C6 C 0.6059(5) 0.2777(5) 0.6561(3) 0.049(2) Uani 1 1 d . . . H6 H 0.6124 0.3245 0.6788 0.059 Uiso 1 1 calc R . . C7 C 0.5276(5) 0.2641(4) 0.6195(3) 0.0400(17) Uani 1 1 d . . . H7 H 0.4823 0.3027 0.6171 0.048 Uiso 1 1 calc R . . C15 C 0.2088(4) 0.1259(4) 0.5863(3) 0.0323(15) Uani 1 1 d . . . C16 C 0.1578(5) 0.1040(4) 0.6356(3) 0.0348(16) Uani 1 1 d . . . C17 C 0.1776(6) 0.0321(5) 0.6655(4) 0.055(2) Uani 1 1 d . . . H17 H 0.2260 0.0008 0.6582 0.066 Uiso 1 1 calc R . . C18 C 0.1260(7) 0.0072(6) 0.7058(4) 0.070(3) Uani 1 1 d . . . H18 H 0.1401 -0.0407 0.7265 0.083 Uiso 1 1 calc R . . C19 C 0.0547(7) 0.0515(5) 0.7159(4) 0.062(3) Uani 1 1 d . . . C20 C 0.0357(6) 0.1247(5) 0.6890(4) 0.052(2) Uani 1 1 d . . . H20 H -0.0122 0.1560 0.6973 0.062 Uiso 1 1 calc R . . C21 C 0.0888(5) 0.1512(5) 0.6493(3) 0.0406(17) Uani 1 1 d . . . H21 H 0.0778 0.2017 0.6316 0.049 Uiso 1 1 calc R . . C22 C 0.1209(5) 0.0045(6) 0.4552(4) 0.053(2) Uani 1 1 d . . . H22 H 0.1185 0.0552 0.4372 0.063 Uiso 1 1 calc R . . C23 C 0.0450(6) -0.0428(6) 0.4500(4) 0.060(2) Uani 1 1 d . . . H23 H -0.0075 -0.0255 0.4284 0.072 Uiso 1 1 calc R . . C24 C 0.0502(6) -0.1168(6) 0.4783(4) 0.064(3) Uani 1 1 d . . . H24 H 0.0001 -0.1499 0.4767 0.076 Uiso 1 1 calc R . . C25 C 0.1277(5) -0.1418(5) 0.5085(4) 0.055(2) Uani 1 1 d . . . H25 H 0.1311 -0.1916 0.5278 0.066 Uiso 1 1 calc R . . C26 C 0.2019(5) -0.0921(4) 0.5104(3) 0.0363(16) Uani 1 1 d . . . C27 C 0.2892(5) -0.1142(4) 0.5397(3) 0.0371(16) Uani 1 1 d . . . C28 C 0.3083(6) -0.1878(5) 0.5676(4) 0.053(2) Uani 1 1 d . . . H28 H 0.2636 -0.2264 0.5689 0.064 Uiso 1 1 calc R . . C29 C 0.3932(6) -0.2039(5) 0.5934(4) 0.061(2) Uani 1 1 d . . . H29 H 0.4062 -0.2529 0.6129 0.073 Uiso 1 1 calc R . . C30 C 0.4586(6) -0.1470(5) 0.5899(4) 0.056(2) Uani 1 1 d . . . H30 H 0.5168 -0.1573 0.6062 0.067 Uiso 1 1 calc R . . C31 C 0.4369(5) -0.0746(5) 0.5621(3) 0.0423(18) Uani 1 1 d . . . H31 H 0.4813 -0.0358 0.5603 0.051 Uiso 1 1 calc R . . O7 O 0.7557(3) 0.2364(4) 0.6901(2) 0.0536(16) Uani 1 1 d . . . C8 C 0.7580(5) 0.2747(5) 0.7429(3) 0.0433(19) Uani 1 1 d . . . C9 C 0.8176(5) 0.3381(5) 0.7539(3) 0.050(2) Uani 1 1 d . . . H9 H 0.8504 0.3562 0.7254 0.060 Uiso 1 1 calc R . . C10 C 0.8280(5) 0.3740(5) 0.8071(3) 0.0448(19) Uani 1 1 d . . . H10 H 0.8687 0.4162 0.8150 0.054 Uiso 1 1 calc R . . C11 C 0.7783(5) 0.3480(4) 0.8491(3) 0.0354(16) Uani 1 1 d . . . C12 C 0.7170(5) 0.2857(5) 0.8368(3) 0.0401(17) Uani 1 1 d . . . H12 H 0.6829 0.2679 0.8647 0.048 Uiso 1 1 calc R . . C13 C 0.7070(5) 0.2501(5) 0.7829(3) 0.0431(18) Uani 1 1 d . . . H13 H 0.6650 0.2091 0.7740 0.052 Uiso 1 1 calc R . . C14 C 0.7918(4) 0.3864(4) 0.9071(3) 0.0307(15) Uani 1 1 d . . . O2 O 0.7571(3) 0.3554(3) 0.94904(18) 0.0300(10) Uani 1 1 d . . . O3 O 0.8356(3) 0.4511(3) 0.91548(19) 0.0361(11) Uani 1 1 d . . . OW O 0.5000 0.0523(6) 0.7500 0.080 Uiso 1 2 d S . . 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 0.0283(5) 0.0285(5) 0.0280(5) 0.0009(4) 0.0015(3) 0.0009(4) Ni2 0.0282(6) 0.0283(6) 0.0237(6) 0.0008(5) 0.0022(5) 0.0031(5) O1 0.027(2) 0.037(3) 0.036(3) -0.006(2) 0.005(2) -0.001(2) O4 0.041(3) 0.044(3) 0.034(3) 0.007(2) 0.013(2) 0.008(2) O5 0.033(3) 0.034(3) 0.031(2) 0.001(2) 0.001(2) 0.003(2) O6 0.034(3) 0.038(3) 0.035(3) 0.005(2) 0.006(2) 0.005(2) O8 0.200(13) 0.046(6) 0.161(11) 0.000 0.163(11) 0.000 N1 0.029(3) 0.035(3) 0.043(3) 0.003(3) -0.003(3) -0.004(3) N2 0.033(3) 0.032(3) 0.036(3) 0.002(2) 0.006(2) 0.003(3) C1 0.030(4) 0.030(4) 0.031(3) 0.001(3) 0.008(3) -0.003(3) C2 0.030(4) 0.033(4) 0.027(3) 0.000(3) -0.003(3) 0.003(3) C3 0.037(4) 0.041(4) 0.037(4) -0.009(3) 0.005(3) 0.002(3) C4 0.027(3) 0.054(5) 0.038(4) -0.004(3) -0.007(3) 0.004(3) C5 0.034(4) 0.057(5) 0.028(4) -0.012(3) 0.000(3) -0.003(4) C6 0.044(4) 0.049(5) 0.053(5) -0.027(4) -0.003(4) -0.001(4) C7 0.036(4) 0.036(4) 0.046(4) -0.011(3) -0.003(3) 0.003(3) C15 0.031(4) 0.038(4) 0.027(3) -0.004(3) 0.001(3) -0.003(3) C16 0.035(4) 0.037(4) 0.035(4) 0.000(3) 0.012(3) -0.002(3) C17 0.072(6) 0.048(5) 0.052(5) 0.006(4) 0.031(4) 0.013(4) C18 0.101(8) 0.045(5) 0.072(6) 0.016(5) 0.051(6) 0.011(5) C19 0.093(7) 0.036(4) 0.069(6) -0.005(4) 0.059(6) -0.002(5) C20 0.054(5) 0.047(5) 0.060(5) -0.003(4) 0.030(4) 0.004(4) C21 0.043(4) 0.039(4) 0.041(4) 0.002(3) 0.013(3) -0.001(3) C22 0.041(5) 0.053(5) 0.061(5) 0.006(4) -0.005(4) -0.001(4) C23 0.040(5) 0.062(6) 0.073(6) -0.004(5) -0.011(4) -0.005(4) C24 0.045(5) 0.064(6) 0.081(7) -0.012(5) 0.002(5) -0.022(5) C25 0.045(5) 0.047(5) 0.073(6) 0.005(4) 0.007(4) -0.010(4) C26 0.033(4) 0.030(4) 0.046(4) -0.006(3) 0.009(3) -0.002(3) C27 0.038(4) 0.037(4) 0.036(4) 0.000(3) 0.005(3) -0.006(3) C28 0.054(5) 0.042(5) 0.064(6) 0.014(4) 0.008(4) -0.004(4) C29 0.072(6) 0.040(5) 0.069(6) 0.019(4) -0.001(5) 0.009(5) C30 0.052(5) 0.044(5) 0.068(6) 0.011(4) -0.004(4) 0.011(4) C31 0.036(4) 0.038(4) 0.053(5) 0.007(3) 0.004(3) 0.006(3) O7 0.031(3) 0.093(5) 0.034(3) -0.028(3) -0.006(2) -0.002(3) C8 0.035(4) 0.060(5) 0.032(4) -0.012(4) -0.005(3) 0.001(4) C9 0.047(4) 0.073(6) 0.031(4) -0.010(4) 0.011(3) -0.015(4) C10 0.042(4) 0.058(5) 0.033(4) -0.004(4) 0.000(3) -0.016(4) C11 0.035(4) 0.035(4) 0.033(4) 0.000(3) -0.006(3) -0.002(3) C12 0.036(4) 0.051(5) 0.031(4) -0.002(3) -0.002(3) -0.006(4) C13 0.039(4) 0.049(5) 0.039(4) -0.005(4) 0.000(3) -0.016(4) C14 0.027(3) 0.036(4) 0.028(3) 0.004(3) 0.002(3) 0.005(3) O2 0.034(2) 0.031(2) 0.025(2) -0.0001(19) 0.0042(19) -0.003(2) O3 0.042(3) 0.035(3) 0.031(2) -0.001(2) 0.002(2) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.985(5) . ? Ni1 O4 2.002(5) . ? Ni1 N2 2.040(6) . ? Ni1 N1 2.064(6) . ? Ni1 O2 2.075(4) 8_455 ? Ni1 O3 2.129(5) 8_455 ? Ni1 C14 2.444(7) 8_455 ? Ni2 O5 2.048(5) . ? Ni2 O5 2.048(5) 7_556 ? Ni2 O6 2.048(5) . ? Ni2 O6 2.048(5) 7_556 ? Ni2 O2 2.108(4) 8_455 ? Ni2 O2 2.108(4) 2_656 ? O1 C1 1.259(8) . ? O4 C15 1.243(8) . ? O5 C1 1.250(8) . ? O6 C15 1.245(8) . ? O8 C19 1.370(9) . ? O8 C19 1.370(9) 2_556 ? N1 C22 1.323(10) . ? N1 C26 1.330(9) . ? N2 C31 1.334(9) . ? N2 C27 1.359(9) . ? C1 C2 1.485(9) . ? C2 C3 1.377(10) . ? C2 C7 1.381(10) . ? C3 C4 1.385(10) . ? C4 C5 1.366(10) . ? C5 C6 1.370(11) . ? C5 O7 1.383(8) . ? C6 C7 1.387(10) . ? C15 C16 1.513(9) . ? C16 C21 1.371(10) . ? C16 C17 1.383(11) . ? C17 C18 1.363(11) . ? C18 C19 1.348(12) . ? C19 C20 1.367(12) . ? C20 C21 1.375(10) . ? C22 C23 1.380(12) . ? C23 C24 1.378(13) . ? C24 C25 1.352(12) . ? C25 C26 1.385(10) . ? C26 C27 1.455(10) . ? C27 C28 1.382(11) . ? C28 C29 1.375(12) . ? C29 C30 1.371(12) . ? C30 C31 1.371(11) . ? O7 C8 1.381(8) . ? C8 C13 1.351(11) . ? C8 C9 1.378(11) . ? C9 C10 1.366(10) . ? C10 C11 1.381(10) . ? C11 C12 1.385(10) . ? C11 C14 1.485(9) . ? C12 C13 1.380(10) . ? C14 O3 1.251(8) . ? C14 O2 1.277(8) . ? C14 Ni1 2.444(7) 8_556 ? O2 Ni1 2.075(4) 8_556 ? O2 Ni2 2.108(4) 2_656 ? O3 Ni1 2.129(5) 8_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 O1 Ni1 O4 90.5(2) . . ? O1 Ni1 N2 94.2(2) . . ? O4 Ni1 N2 88.1(2) . . ? O1 Ni1 N1 173.5(2) . . ? O4 Ni1 N1 88.6(2) . . ? N2 Ni1 N1 79.3(2) . . ? O1 Ni1 O2 94.02(19) . 8_455 ? O4 Ni1 O2 103.62(18) . 8_455 ? N2 Ni1 O2 165.6(2) . 8_455 ? N1 Ni1 O2 92.5(2) . 8_455 ? O1 Ni1 O3 89.98(19) . 8_455 ? O4 Ni1 O3 165.89(19) . 8_455 ? N2 Ni1 O3 105.9(2) . 8_455 ? N1 Ni1 O3 92.5(2) . 8_455 ? O2 Ni1 O3 62.28(17) 8_455 8_455 ? O1 Ni1 C14 92.1(2) . 8_455 ? O4 Ni1 C14 135.1(2) . 8_455 ? N2 Ni1 C14 136.3(2) . 8_455 ? N1 Ni1 C14 93.1(2) . 8_455 ? O2 Ni1 C14 31.5(2) 8_455 8_455 ? O3 Ni1 C14 30.79(19) 8_455 8_455 ? O5 Ni2 O5 180 . 7_556 ? O5 Ni2 O6 94.51(18) . . ? O5 Ni2 O6 85.49(18) 7_556 . ? O5 Ni2 O6 85.49(18) . 7_556 ? O5 Ni2 O6 94.51(18) 7_556 7_556 ? O6 Ni2 O6 180 . 7_556 ? O5 Ni2 O2 93.62(17) . 8_455 ? O5 Ni2 O2 86.38(17) 7_556 8_455 ? O6 Ni2 O2 90.97(18) . 8_455 ? O6 Ni2 O2 89.03(18) 7_556 8_455 ? O5 Ni2 O2 86.38(17) . 2_656 ? O5 Ni2 O2 93.62(17) 7_556 2_656 ? O6 Ni2 O2 89.03(18) . 2_656 ? O6 Ni2 O2 90.97(18) 7_556 2_656 ? O2 Ni2 O2 180 8_455 2_656 ? C1 O1 Ni1 123.5(4) . . ? C15 O4 Ni1 125.5(4) . . ? C1 O5 Ni2 137.0(4) . . ? C15 O6 Ni2 128.5(4) . . ? C19 O8 C19 126.5(10) . 2_556 ? C22 N1 C26 119.6(7) . . ? C22 N1 Ni1 125.8(6) . . ? C26 N1 Ni1 114.3(5) . . ? C31 N2 C27 119.5(6) . . ? C31 N2 Ni1 126.4(5) . . ? C27 N2 Ni1 113.8(5) . . ? O5 C1 O1 126.3(6) . . ? O5 C1 C2 117.6(6) . . ? O1 C1 C2 116.1(6) . . ? C3 C2 C7 118.5(6) . . ? C3 C2 C1 120.5(6) . . ? C7 C2 C1 120.9(6) . . ? C2 C3 C4 121.0(7) . . ? C5 C4 C3 119.6(7) . . ? C4 C5 C6 120.6(7) . . ? C4 C5 O7 117.6(7) . . ? C6 C5 O7 121.7(7) . . ? C5 C6 C7 119.6(7) . . ? C2 C7 C6 120.7(7) . . ? O4 C15 O6 127.0(6) . . ? O4 C15 C16 115.4(6) . . ? O6 C15 C16 117.5(6) . . ? C21 C16 C17 118.9(7) . . ? C21 C16 C15 121.8(6) . . ? C17 C16 C15 119.2(6) . . ? C18 C17 C16 119.9(8) . . ? C19 C18 C17 120.3(9) . . ? C18 C19 C20 121.1(7) . . ? C18 C19 O8 114.8(8) . . ? C20 C19 O8 123.7(8) . . ? C19 C20 C21 118.7(8) . . ? C16 C21 C20 120.7(7) . . ? N1 C22 C23 122.7(8) . . ? C24 C23 C22 117.2(8) . . ? C25 C24 C23 120.5(8) . . ? C24 C25 C26 119.1(8) . . ? N1 C26 C25 120.9(7) . . ? N1 C26 C27 115.5(6) . . ? C25 C26 C27 123.6(7) . . ? N2 C27 C28 120.0(7) . . ? N2 C27 C26 115.9(6) . . ? C28 C27 C26 124.2(7) . . ? C29 C28 C27 120.1(8) . . ? C30 C29 C28 119.1(8) . . ? C31 C30 C29 119.1(8) . . ? N2 C31 C30 122.2(8) . . ? C8 O7 C5 118.1(6) . . ? C13 C8 C9 121.1(7) . . ? C13 C8 O7 122.2(7) . . ? C9 C8 O7 116.7(7) . . ? C10 C9 C8 119.3(7) . . ? C9 C10 C11 120.5(7) . . ? C10 C11 C12 119.5(7) . . ? C10 C11 C14 119.8(6) . . ? C12 C11 C14 120.7(6) . . ? C13 C12 C11 119.5(7) . . ? C8 C13 C12 120.1(7) . . ? O3 C14 O2 118.7(6) . . ? O3 C14 C11 120.5(6) . . ? O2 C14 C11 120.7(6) . . ? O3 C14 Ni1 60.6(3) . 8_556 ? O2 C14 Ni1 58.1(3) . 8_556 ? C11 C14 Ni1 178.5(5) . 8_556 ? C14 O2 Ni1 90.4(4) . 8_556 ? C14 O2 Ni2 144.7(4) . 2_656 ? Ni1 O2 Ni2 107.76(19) 8_556 2_656 ? C14 O3 Ni1 88.6(4) . 8_556 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.096 _refine_diff_density_min -4.560 _refine_diff_density_rms 0.130