Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Pasini, Alessandro' 'Chiari, Brunetto' 'Cinti, Antonio' 'Crispu, Ornella' 'Demartin, Francesco' 'Piovesana, Olivo' _publ_contact_author_name 'Dr Alessandro Pasini' _publ_contact_author_address ; Dipartimento di Chimica Inorganica Metallorganica e Analitia and CNR centre via Venezian 21 Milano 20133 ITALY ; _publ_contact_author_email 'ALESSANDRO.PASINI@UNIMI.IT' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; New pentanuclear miced valence Co(II)-Co(III) complexes of "short" salen homologues ; data_H2salNO2ben _database_code_CSD 188686 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H17 N3 O4' _chemical_formula_weight 375.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pna21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 9.2106(18) _cell_length_b 15.578(3) _cell_length_c 13.018(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1867.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD DIFFRACTOMETER' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2112 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 26.95 _reflns_number_total 2112 _reflns_number_gt 1522 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0549P)^2^+0.0844P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.015(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.5(16) _refine_ls_number_reflns 2112 _refine_ls_number_parameters 322 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.1067(3) 0.55548(16) 0.56588(18) 0.0727(7) Uani 1 1 d . . . O25 O 0.4472(3) 0.64659(15) 0.9191(2) 0.0813(7) Uani 1 1 d . . . O27 O 0.6604(4) 0.5326(2) 0.3382(3) 0.1260(13) Uani 1 1 d . . . O28 O 0.6795(5) 0.6646(3) 0.2996(3) 0.1486(17) Uani 1 1 d . . . N9 N 0.1056(3) 0.63244(15) 0.66287(17) 0.0518(6) Uani 1 1 d . . . N17 N 0.2916(3) 0.70322(15) 0.76442(19) 0.0537(6) Uani 1 1 d . . . N26 N 0.6298(4) 0.6075(3) 0.3510(2) 0.0855(9) Uani 1 1 d . . . C2 C -0.1268(3) 0.50940(19) 0.6531(2) 0.0562(7) Uani 1 1 d . . . C3 C -0.2315(4) 0.4466(2) 0.6550(3) 0.0687(9) Uani 1 1 d . . . C4 C -0.2525(4) 0.3986(2) 0.7422(3) 0.0732(9) Uani 1 1 d . . . C5 C -0.1708(4) 0.4121(2) 0.8278(3) 0.0701(9) Uani 1 1 d . . . C6 C -0.0659(4) 0.4740(2) 0.8273(3) 0.0622(8) Uani 1 1 d . . . C7 C -0.0413(3) 0.52408(17) 0.7403(2) 0.0489(6) Uani 1 1 d . . . C8 C 0.0730(3) 0.58904(18) 0.7416(2) 0.0506(6) Uani 1 1 d . . . C10 C 0.2213(3) 0.69655(18) 0.6645(2) 0.0514(7) Uani 1 1 d . . . C18 C 0.2717(3) 0.7721(2) 0.8161(2) 0.0537(7) Uani 1 1 d . . . C19 C 0.3324(3) 0.78487(19) 0.9167(2) 0.0539(7) Uani 1 1 d . . . C20 C 0.3012(4) 0.8607(2) 0.9700(3) 0.0686(9) Uani 1 1 d . . . C21 C 0.3524(5) 0.8740(3) 1.0674(3) 0.0804(10) Uani 1 1 d . . . C22 C 0.4372(5) 0.8128(3) 1.1124(3) 0.0808(12) Uani 1 1 d . . . C23 C 0.4709(5) 0.7373(3) 1.0630(3) 0.0742(10) Uani 1 1 d . . . C24 C 0.4163(3) 0.7228(2) 0.9645(2) 0.0597(8) Uani 1 1 d . . . C11 C 0.3319(3) 0.67339(17) 0.5836(2) 0.0495(7) Uani 1 1 d . . . C12 C 0.3919(4) 0.5916(2) 0.5799(2) 0.0628(8) Uani 1 1 d . . . C13 C 0.4902(4) 0.5698(2) 0.5042(3) 0.0692(9) Uani 1 1 d . . . C14 C 0.5288(3) 0.6307(2) 0.4336(2) 0.0612(8) Uani 1 1 d . . . C15 C 0.4733(4) 0.7127(2) 0.4353(3) 0.0649(8) Uani 1 1 d . . . C16 C 0.3727(4) 0.73299(19) 0.5107(3) 0.0566(7) Uani 1 1 d . . . H1 H -0.036(4) 0.589(2) 0.574(3) 0.068(11) Uiso 1 1 d . . . H3 H -0.272(4) 0.435(2) 0.599(3) 0.071(11) Uiso 1 1 d . . . H4 H -0.321(4) 0.354(2) 0.739(3) 0.070(10) Uiso 1 1 d . . . H5 H -0.185(4) 0.376(3) 0.885(3) 0.087(12) Uiso 1 1 d . . . H6 H -0.008(4) 0.488(2) 0.883(3) 0.061(9) Uiso 1 1 d . . . H8 H 0.131(3) 0.594(2) 0.807(3) 0.060(8) Uiso 1 1 d . . . H10 H 0.182(3) 0.7507(17) 0.645(2) 0.035(6) Uiso 1 1 d . . . H18 H 0.212(3) 0.820(2) 0.789(3) 0.056(8) Uiso 1 1 d . . . H20 H 0.241(4) 0.901(2) 0.934(3) 0.065(9) Uiso 1 1 d . . . H21 H 0.303(6) 0.927(3) 1.107(4) 0.142(19) Uiso 1 1 d . . . H22 H 0.470(5) 0.825(3) 1.180(4) 0.102(13) Uiso 1 1 d . . . H23 H 0.531(4) 0.693(2) 1.086(3) 0.082(12) Uiso 1 1 d . . . H25 H 0.376(6) 0.646(4) 0.858(5) 0.141(19) Uiso 1 1 d . . . H12 H 0.342(4) 0.551(2) 0.630(3) 0.072(10) Uiso 1 1 d . . . H13 H 0.537(5) 0.512(3) 0.500(3) 0.094(12) Uiso 1 1 d . . . H15 H 0.515(5) 0.758(3) 0.379(4) 0.120(15) Uiso 1 1 d . . . H16 H 0.322(4) 0.788(2) 0.511(3) 0.068(10) 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 O1 0.0856(16) 0.0748(15) 0.0577(13) 0.0165(12) -0.0213(12) -0.0194(13) O25 0.0979(17) 0.0719(15) 0.0742(16) -0.0139(13) -0.0268(14) 0.0131(13) O27 0.137(3) 0.119(3) 0.122(3) -0.010(2) 0.056(2) 0.026(2) O28 0.179(4) 0.142(3) 0.125(3) 0.006(3) 0.091(3) -0.014(3) N9 0.0556(13) 0.0555(13) 0.0442(12) -0.0021(11) -0.0023(11) -0.0033(11) N17 0.0624(14) 0.0526(13) 0.0461(13) -0.0036(12) -0.0052(11) -0.0036(11) N26 0.080(2) 0.110(3) 0.067(2) -0.006(2) 0.0164(16) -0.006(2) C2 0.0570(16) 0.0584(16) 0.0532(17) 0.0046(15) -0.0017(14) 0.0059(14) C3 0.0627(19) 0.072(2) 0.072(2) 0.0010(19) -0.0128(19) -0.0061(17) C4 0.0643(19) 0.072(2) 0.084(3) 0.004(2) 0.0113(19) -0.0129(18) C5 0.073(2) 0.073(2) 0.064(2) 0.007(2) 0.0181(19) -0.0022(18) C6 0.0674(18) 0.072(2) 0.0474(16) 0.0014(15) 0.0073(16) -0.0024(17) C7 0.0531(15) 0.0518(15) 0.0417(14) -0.0019(12) 0.0046(12) 0.0070(13) C8 0.0549(15) 0.0559(16) 0.0410(14) -0.0041(13) 0.0016(13) 0.0047(13) C10 0.0582(16) 0.0509(16) 0.0450(15) 0.0001(13) -0.0054(13) 0.0023(14) C18 0.0578(16) 0.0532(16) 0.0501(15) -0.0038(14) 0.0032(14) -0.0057(15) C19 0.0574(15) 0.0548(16) 0.0494(16) -0.0065(14) 0.0056(14) -0.0142(14) C20 0.078(2) 0.065(2) 0.0632(19) -0.0132(17) 0.0040(18) -0.0109(18) C21 0.091(3) 0.081(2) 0.069(2) -0.026(2) 0.003(2) -0.018(2) C22 0.088(2) 0.102(3) 0.052(2) -0.023(2) 0.0022(19) -0.033(2) C23 0.077(2) 0.085(3) 0.061(2) -0.001(2) -0.0104(18) -0.011(2) C24 0.0636(18) 0.0667(19) 0.0489(16) -0.0081(15) -0.0007(14) -0.0110(15) C11 0.0544(15) 0.0492(15) 0.0448(15) -0.0009(12) -0.0094(12) -0.0038(13) C12 0.0698(18) 0.0627(18) 0.0559(18) 0.0113(16) 0.0036(15) 0.0047(16) C13 0.075(2) 0.069(2) 0.063(2) 0.0032(18) 0.0049(18) 0.0129(18) C14 0.0561(16) 0.079(2) 0.0482(15) -0.0067(16) -0.0013(13) -0.0053(15) C15 0.0732(19) 0.0659(19) 0.0555(18) 0.0036(16) 0.0013(16) -0.0202(17) C16 0.0683(18) 0.0469(17) 0.0547(16) 0.0005(13) -0.0063(15) -0.0097(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 O1 C2 1.356(4) . ? O25 C24 1.356(4) . ? O27 N26 1.211(4) . ? O28 N26 1.204(5) . ? N9 C8 1.264(3) . ? N9 C10 1.461(4) . ? N17 C18 1.279(4) . ? N17 C10 1.456(4) . ? N26 C14 1.468(4) . ? C2 C3 1.374(5) . ? C2 C7 1.400(4) . ? C3 C4 1.373(5) . ? C4 C5 1.361(6) . ? C5 C6 1.365(5) . ? C6 C7 1.394(4) . ? C7 C8 1.460(4) . ? C10 C11 1.510(4) . ? C18 C19 1.438(4) . ? C19 C24 1.386(4) . ? C19 C20 1.400(5) . ? C20 C21 1.369(6) . ? C21 C22 1.364(6) . ? C22 C23 1.377(6) . ? C23 C24 1.395(5) . ? C11 C16 1.379(4) . ? C11 C12 1.390(4) . ? C12 C13 1.381(5) . ? C13 C14 1.367(5) . ? C14 C15 1.376(5) . ? C15 C16 1.387(5) . ? 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 C8 N9 C10 121.8(2) . . ? C18 N17 C10 117.8(3) . . ? O28 N26 O27 123.1(4) . . ? O28 N26 C14 117.8(4) . . ? O27 N26 C14 119.1(4) . . ? O1 C2 C3 119.2(3) . . ? O1 C2 C7 121.0(3) . . ? C3 C2 C7 119.8(3) . . ? C4 C3 C2 120.1(4) . . ? C5 C4 C3 121.0(3) . . ? C4 C5 C6 119.8(3) . . ? C5 C6 C7 120.9(3) . . ? C6 C7 C2 118.4(3) . . ? C6 C7 C8 119.7(3) . . ? C2 C7 C8 121.9(2) . . ? N9 C8 C7 122.2(3) . . ? N17 C10 N9 112.7(2) . . ? N17 C10 C11 109.9(2) . . ? N9 C10 C11 108.6(2) . . ? N17 C18 C19 122.7(3) . . ? C24 C19 C20 118.7(3) . . ? C24 C19 C18 121.9(3) . . ? C20 C19 C18 119.3(3) . . ? C21 C20 C19 121.1(4) . . ? C22 C21 C20 119.3(4) . . ? C21 C22 C23 121.7(4) . . ? C22 C23 C24 119.1(4) . . ? O25 C24 C19 122.1(3) . . ? O25 C24 C23 117.8(3) . . ? C19 C24 C23 120.0(3) . . ? C16 C11 C12 119.1(3) . . ? C16 C11 C10 120.2(3) . . ? C12 C11 C10 120.7(2) . . ? C13 C12 C11 120.6(3) . . ? C14 C13 C12 118.7(3) . . ? C13 C14 C15 122.5(3) . . ? C13 C14 N26 119.1(3) . . ? C15 C14 N26 118.4(3) . . ? C14 C15 C16 118.1(3) . . ? C11 C16 C15 121.0(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.95 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.136 _refine_diff_density_min -0.119 _refine_diff_density_rms 0.027 #===END data_[Co5(OH)2(salNO2ben)4]I.2(CH3)2CO _database_code_CSD 188687 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Co5(OH)2(salNO2ben)4]I.2(CH3)2CO _chemical_formula_sum 'C90 H74 Co5 I N12 O20' _chemical_formula_weight 2065.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'I' 'I' -0.4742 1.8119 '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' 'O' 'O' 0.0106 0.0060 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic unique axis b' _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 15.7710(10) _cell_length_b 25.007(2) _cell_length_c 23.185(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.880(10) _cell_angle_gamma 90.00 _cell_volume 9008.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 23.0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4184 _exptl_absorpt_coefficient_mu 1.321 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD DIFFRACTOMETER' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12972 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 23.28 _reflns_number_total 12972 _reflns_number_gt 9829 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0737P)^2^+1.6600P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12972 _refine_ls_number_parameters 1167 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1283 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.264 _refine_ls_shift/su_mean 0.018 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 C201 C 0.1982(10) 0.9905(6) 0.4193(6) 0.220(7) Uani 1 1 d . . . C203 C 0.0380(10) 0.9979(7) 0.3795(8) 0.237(8) Uani 1 1 d . . . I1 I 0.17500(3) 0.041733(15) 0.24836(2) 0.08901(18) Uani 1 1 d . . . Co1 Co 0.03094(3) 0.77026(2) 0.37562(2) 0.02844(14) Uani 1 1 d . . . Co2 Co -0.13028(4) 0.74611(2) 0.49286(3) 0.04173(17) Uani 1 1 d . . . Co3 Co 0.23059(4) 0.73830(2) 0.39762(2) 0.03566(15) Uani 1 1 d . . . Co4 Co 0.16171(3) 0.78535(2) 0.28448(2) 0.02999(14) Uani 1 1 d . . . Co5 Co -0.01438(4) 0.82315(2) 0.24927(2) 0.03790(16) Uani 1 1 d . . . O25A O 0.12736(16) 0.78550(11) 0.43443(11) 0.0319(6) Uani 1 1 d . . . O1 O 0.06303(17) 0.82578(10) 0.32655(11) 0.0326(6) Uani 1 1 d . . . O1C O 0.2695(2) 0.70547(14) 0.47170(13) 0.0551(9) Uani 1 1 d . . . O1B O 0.25405(17) 0.80381(11) 0.35441(11) 0.0370(7) Uani 1 1 d . . . O25C O 0.06065(17) 0.76853(11) 0.22017(12) 0.0373(7) Uani 1 1 d . . . O25B O -0.12730(19) 0.85110(15) 0.22871(16) 0.0632(10) Uani 1 1 d . . . O1A O -0.1935(2) 0.68150(13) 0.48711(15) 0.0561(9) Uani 1 1 d . . . O25D O -0.1339(2) 0.79585(14) 0.55472(15) 0.0593(9) Uani 1 1 d . . . O1D O -0.05275(17) 0.75843(11) 0.30819(12) 0.0348(7) Uani 1 1 d . . . O2 O 0.11639(16) 0.72961(10) 0.34543(11) 0.0301(6) Uani 1 1 d . . . O27D O 0.1422(4) 0.45699(18) 0.5523(3) 0.1125(18) Uani 1 1 d . . . O28D O 0.0483(4) 0.47194(17) 0.6077(2) 0.1029(16) Uani 1 1 d . . . O27A O -0.3421(4) 1.0390(2) 0.3631(3) 0.138(3) Uani 1 1 d . . . O28A O -0.3791(4) 1.0113(3) 0.4435(4) 0.164(3) Uani 1 1 d . . . O27B O 0.0378(3) 0.7483(2) -0.0392(2) 0.1059(17) Uani 1 1 d . . . O28B O 0.1620(3) 0.7173(2) -0.00846(19) 0.0922(14) Uani 1 1 d . . . O27C O 0.5491(4) 0.8793(4) 0.2087(3) 0.203(4) Uani 1 1 d . . . O28C O 0.6217(5) 0.8645(4) 0.2927(3) 0.232(5) Uani 1 1 d . . . N26D N 0.0892(4) 0.4848(2) 0.5702(2) 0.0740(15) Uani 1 1 d . . . N9A N -0.1753(2) 0.77063(14) 0.41179(15) 0.0375(8) Uani 1 1 d . . . N17D N -0.0036(2) 0.73260(14) 0.51337(15) 0.0377(8) Uani 1 1 d . . . N9C N 0.3036(2) 0.69118(14) 0.35324(15) 0.0384(8) Uani 1 1 d . . . N9D N 0.0003(2) 0.70634(13) 0.41579(14) 0.0304(8) Uani 1 1 d . . . N17A N -0.0460(2) 0.81871(13) 0.40850(14) 0.0327(8) Uani 1 1 d . . . N17B N 0.0403(2) 0.88553(14) 0.21187(14) 0.0346(8) Uani 1 1 d . . . N9B N 0.1862(2) 0.86006(13) 0.24786(14) 0.0336(8) Uani 1 1 d . . . N17C N 0.2264(2) 0.71723(13) 0.25921(14) 0.0348(8) Uani 1 1 d . . . N26A N -0.3413(4) 1.0068(2) 0.4035(4) 0.104(2) Uani 1 1 d . . . N26B N 0.1038(3) 0.7470(2) -0.00443(19) 0.0666(13) Uani 1 1 d . . . N26C N 0.5603(5) 0.8580(4) 0.2559(3) 0.149(3) Uani 1 1 d . . . C102 C 0.0888(6) 0.5743(3) 0.3062(4) 0.109(3) Uani 1 1 d . . . C202 C 0.1165(10) 0.9648(3) 0.3881(4) 0.145(5) Uani 1 1 d . . . O204 O 0.1080(8) 0.9238(3) 0.3700(3) 0.242(6) Uani 1 1 d . . . O104 O 0.1058(3) 0.61901(18) 0.3284(2) 0.1039(16) Uani 1 1 d . . . C101 C 0.1350(6) 0.5265(3) 0.3384(4) 0.129(3) Uani 1 1 d . . . C103 C 0.0298(7) 0.5653(4) 0.2497(4) 0.146(4) Uani 1 1 d . . . C10D C 0.0416(3) 0.69784(16) 0.47740(17) 0.0334(9) Uani 1 1 d . . . H10D H 0.1008 0.7112 0.4812 0.023(9) Uiso 1 1 calc R . . C24D C -0.0699(3) 0.8082(2) 0.5968(2) 0.0493(12) Uani 1 1 d . . . C2D C -0.0989(3) 0.71493(16) 0.29343(18) 0.0336(10) Uani 1 1 d . . . C2A C -0.2596(3) 0.66982(18) 0.4465(2) 0.0465(12) Uani 1 1 d . . . C11D C 0.0471(3) 0.64010(17) 0.49900(18) 0.0372(10) Uani 1 1 d . . . C24C C 0.0497(3) 0.72961(19) 0.18014(18) 0.0412(11) Uani 1 1 d . . . C2C C 0.3073(3) 0.6585(2) 0.4793(2) 0.0504(12) Uani 1 1 d . . . C24B C -0.1482(3) 0.9012(2) 0.2123(2) 0.0535(13) Uani 1 1 d . . . C24A C 0.1351(3) 0.82414(16) 0.47374(17) 0.0332(10) Uani 1 1 d . . . C2B C 0.3100(3) 0.84333(18) 0.36335(19) 0.0393(10) Uani 1 1 d . . . C3D C -0.1514(3) 0.71246(19) 0.23895(19) 0.0458(12) Uani 1 1 d . . . H3D H -0.1546 0.7418 0.2141 0.055 Uiso 1 1 calc R . . C3B C 0.3726(3) 0.8439(2) 0.4142(2) 0.0591(14) Uani 1 1 d . . . H3B H 0.3736 0.8164 0.4414 0.071 Uiso 1 1 calc R . . C3C C 0.3130(3) 0.6351(2) 0.5349(2) 0.0681(16) Uani 1 1 d . . . H3C H 0.2935 0.6537 0.5647 0.082 Uiso 1 1 calc R . . C23C C -0.0241(3) 0.7292(2) 0.1373(2) 0.0589(14) Uani 1 1 d . . . H23C H -0.0649 0.7562 0.1367 0.071 Uiso 1 1 calc R . . C12D C 0.1049(3) 0.60649(19) 0.4788(2) 0.0516(12) Uani 1 1 d . . . H12D H 0.1342 0.6181 0.4496 0.062 Uiso 1 1 calc R . . C3A C -0.3105(4) 0.6245(2) 0.4547(3) 0.0648(15) Uani 1 1 d . . . H3A H -0.2968 0.6037 0.4883 0.078 Uiso 1 1 calc R . . C23B C -0.2356(3) 0.9146(3) 0.2037(2) 0.0748(18) Uani 1 1 d . . . H23B H -0.2763 0.8885 0.2072 0.090 Uiso 1 1 calc R . . C23A C 0.2148(3) 0.83140(19) 0.5106(2) 0.0491(12) Uani 1 1 d . . . H23A H 0.2606 0.8091 0.5066 0.059 Uiso 1 1 calc R . . C23D C -0.0852(4) 0.8461(2) 0.6396(2) 0.0611(14) Uani 1 1 d . . . H23D H -0.1393 0.8617 0.6365 0.073 Uiso 1 1 calc R . . C22D C -0.0229(4) 0.8598(2) 0.6845(2) 0.0743(17) Uani 1 1 d . . . H22D H -0.0348 0.8846 0.7120 0.089 Uiso 1 1 calc R . . C22A C 0.2264(4) 0.8706(2) 0.5522(2) 0.0654(15) Uani 1 1 d . . . H22A H 0.2798 0.8745 0.5760 0.078 Uiso 1 1 calc R . . C4C C 0.3471(4) 0.5850(3) 0.5455(3) 0.082(2) Uani 1 1 d . . . H4C H 0.3493 0.5699 0.5824 0.099 Uiso 1 1 calc R . . C4B C 0.4323(4) 0.8841(3) 0.4245(3) 0.090(2) Uani 1 1 d . . . H4B H 0.4733 0.8834 0.4585 0.108 Uiso 1 1 calc R . . C22B C -0.2612(4) 0.9658(3) 0.1902(3) 0.084(2) Uani 1 1 d . . . H22B H -0.3192 0.9743 0.1866 0.100 Uiso 1 1 calc R . . C22C C -0.0372(4) 0.6893(3) 0.0957(3) 0.087(2) Uani 1 1 d . . . H22C H -0.0860 0.6902 0.0668 0.105 Uiso 1 1 calc R . . C4D C -0.1984(3) 0.6679(2) 0.2212(2) 0.0594(14) Uani 1 1 d . . . H4D H -0.2317 0.6669 0.1840 0.071 Uiso 1 1 calc R . . C4A C -0.3804(4) 0.6115(3) 0.4126(3) 0.0783(19) Uani 1 1 d . . . H4A H -0.4134 0.5819 0.4191 0.094 Uiso 1 1 calc R . . C13D C 0.1193(3) 0.5553(2) 0.5020(3) 0.0625(15) Uani 1 1 d . . . H13D H 0.1583 0.5324 0.4888 0.075 Uiso 1 1 calc R . . C5A C -0.4035(4) 0.6397(3) 0.3620(3) 0.0730(17) Uani 1 1 d . . . H5A H -0.4509 0.6298 0.3345 0.088 Uiso 1 1 calc R . . C5C C 0.3778(5) 0.5567(3) 0.5034(3) 0.092(2) Uani 1 1 d . . . H5C H 0.4004 0.5226 0.5116 0.110 Uiso 1 1 calc R . . C5B C 0.4325(5) 0.9258(3) 0.3850(3) 0.117(3) Uani 1 1 d . . . H5B H 0.4733 0.9529 0.3922 0.140 Uiso 1 1 calc R . . C21B C -0.2045(4) 1.0048(3) 0.1818(3) 0.081(2) Uani 1 1 d . . . H21B H -0.2232 1.0395 0.1721 0.097 Uiso 1 1 calc R . . C21C C 0.0209(5) 0.6482(3) 0.0963(3) 0.090(2) Uani 1 1 d . . . H21C H 0.0103 0.6204 0.0693 0.108 Uiso 1 1 calc R . . C21D C 0.0580(4) 0.8377(3) 0.6905(2) 0.0778(18) Uani 1 1 d . . . H21D H 0.0998 0.8470 0.7223 0.093 Uiso 1 1 calc R . . C14D C 0.0745(3) 0.53956(19) 0.5448(2) 0.0546(13) Uani 1 1 d . . . C5D C -0.1970(3) 0.6239(2) 0.2579(2) 0.0642(15) Uani 1 1 d . . . H5D H -0.2286 0.5934 0.2454 0.077 Uiso 1 1 calc R . . C21A C 0.1596(4) 0.9048(2) 0.5595(2) 0.0705(16) Uani 1 1 d . . . H21A H 0.1684 0.9321 0.5871 0.085 Uiso 1 1 calc R . . C20A C 0.0806(4) 0.8975(2) 0.5253(2) 0.0586(14) Uani 1 1 d . . . H20A H 0.0348 0.9192 0.5309 0.070 Uiso 1 1 calc R . . C6B C 0.3714(4) 0.9262(3) 0.3351(3) 0.086(2) Uani 1 1 d . . . H6B H 0.3711 0.9542 0.3086 0.103 Uiso 1 1 calc R . . C20B C -0.1183(4) 0.9917(2) 0.1880(2) 0.0607(14) Uani 1 1 d . . . H20B H -0.0789 1.0180 0.1821 0.073 Uiso 1 1 calc R . . C20C C 0.0937(4) 0.6487(2) 0.1366(2) 0.0733(17) Uani 1 1 d . . . H20C H 0.1339 0.6216 0.1359 0.088 Uiso 1 1 calc R . . C6C C 0.3755(4) 0.5785(2) 0.4486(3) 0.0759(17) Uani 1 1 d . . . H6C H 0.3974 0.5594 0.4200 0.091 Uiso 1 1 calc R . . C6A C -0.3548(3) 0.6830(2) 0.3530(3) 0.0603(14) Uani 1 1 d . . . H6A H -0.3695 0.7022 0.3185 0.072 Uiso 1 1 calc R . . C15D C 0.0151(4) 0.5719(2) 0.5640(2) 0.0708(17) Uani 1 1 d . . . H15D H -0.0160 0.5599 0.5921 0.085 Uiso 1 1 calc R . . C20D C 0.0769(4) 0.8027(2) 0.6502(2) 0.0658(15) Uani 1 1 d . . . H20D H 0.1323 0.7888 0.6541 0.079 Uiso 1 1 calc R . . C6D C -0.1491(3) 0.62614(18) 0.3122(2) 0.0496(12) Uani 1 1 d . . . H6D H -0.1501 0.5973 0.3374 0.060 Uiso 1 1 calc R . . C7B C 0.3089(3) 0.88519(18) 0.3228(2) 0.0464(12) Uani 1 1 d . . . C7C C 0.3395(3) 0.6302(2) 0.4360(2) 0.0531(13) Uani 1 1 d . . . C19C C 0.1109(3) 0.68863(19) 0.17968(19) 0.0461(11) Uani 1 1 d . . . C19B C -0.0887(3) 0.9401(2) 0.20273(19) 0.0456(12) Uani 1 1 d . . . C19A C 0.0675(3) 0.85745(17) 0.48143(18) 0.0382(10) Uani 1 1 d . . . C16D C 0.0023(4) 0.62247(19) 0.5411(2) 0.0604(14) Uani 1 1 d . . . H16D H -0.0372 0.6450 0.5542 0.073 Uiso 1 1 calc R . . C7D C -0.0978(3) 0.67084(16) 0.33148(18) 0.0341(10) Uani 1 1 d . . . C7A C -0.2838(3) 0.69959(18) 0.3937(2) 0.0439(11) Uani 1 1 d . . . C19D C 0.0138(3) 0.78653(19) 0.60183(19) 0.0464(11) Uani 1 1 d . . . C8C C 0.3384(3) 0.64808(19) 0.3768(2) 0.0490(12) Uani 1 1 d . . . H8C H 0.3657 0.6262 0.3531 0.055(14) Uiso 1 1 calc R . . C8D C -0.0505(3) 0.67011(16) 0.39000(18) 0.0339(10) Uani 1 1 d . . . H8D H -0.0573 0.6398 0.4120 0.041(12) Uiso 1 1 calc R . . C18C C 0.1915(3) 0.68408(18) 0.21926(19) 0.0440(11) Uani 1 1 d . . . H18C H 0.2228 0.6531 0.2156 0.052(14) Uiso 1 1 calc R . . C10A C -0.1408(3) 0.81747(17) 0.38528(19) 0.0372(10) Uani 1 1 d . . . H10A H -0.1482 0.8112 0.3430 0.020(9) Uiso 1 1 calc R . . C18B C 0.0004(3) 0.93027(18) 0.20082(18) 0.0409(11) Uani 1 1 d . . . H18B H 0.0324 0.9590 0.1906 0.041(12) Uiso 1 1 calc R . . C8A C -0.2390(3) 0.74591(18) 0.3794(2) 0.0432(11) Uani 1 1 d . . . H8A H -0.2575 0.7602 0.3423 0.030(11) Uiso 1 1 calc R . . C18A C -0.0183(3) 0.85165(17) 0.44978(18) 0.0385(10) Uani 1 1 d . . . H18A H -0.0592 0.8747 0.4605 0.040(12) Uiso 1 1 calc R . . C18D C 0.0422(3) 0.75210(17) 0.56019(18) 0.0406(11) Uani 1 1 d . . . H18D H 0.1001 0.7426 0.5675 0.043(12) Uiso 1 1 calc R . . C8B C 0.2460(3) 0.89210(17) 0.2713(2) 0.0418(11) Uani 1 1 d . . . H8B H 0.2486 0.9245 0.2519 0.031(11) Uiso 1 1 calc R . . C11A C -0.1886(3) 0.86861(18) 0.3947(2) 0.0443(11) Uani 1 1 d . . . C12A C -0.1869(4) 0.9102(2) 0.3563(2) 0.0660(15) Uani 1 1 d . . . H12A H -0.1518 0.9076 0.3281 0.079 Uiso 1 1 calc R . . C13A C -0.2355(5) 0.9553(2) 0.3584(3) 0.085(2) Uani 1 1 d . . . H13A H -0.2348 0.9826 0.3313 0.102 Uiso 1 1 calc R . . C14A C -0.2849(4) 0.9592(2) 0.4008(3) 0.0693(17) Uani 1 1 d . . . C15A C -0.2860(4) 0.9209(2) 0.4409(4) 0.091(2) Uani 1 1 d . . . H15A H -0.3184 0.9249 0.4705 0.109 Uiso 1 1 calc R . . C16A C -0.2371(4) 0.8743(2) 0.4372(3) 0.0785(19) Uani 1 1 d . . . H16A H -0.2381 0.8470 0.4643 0.094 Uiso 1 1 calc R . . C10B C 0.1276(3) 0.88194(17) 0.19669(18) 0.0361(10) Uani 1 1 d . . . H10B H 0.1468 0.9181 0.1890 0.048(13) Uiso 1 1 calc R . . C11B C 0.1246(3) 0.84883(18) 0.14184(18) 0.0397(11) Uani 1 1 d . . . C12B C 0.0542(3) 0.8519(2) 0.0976(2) 0.0574(14) Uani 1 1 d . . . H12B H 0.0099 0.8757 0.1007 0.069 Uiso 1 1 calc R . . C13B C 0.0491(3) 0.8195(2) 0.0481(2) 0.0650(16) Uani 1 1 d . . . H13B H 0.0023 0.8219 0.0178 0.078 Uiso 1 1 calc R . . C14B C 0.1132(3) 0.7846(2) 0.04501(19) 0.0508(13) Uani 1 1 d . . . C15B C 0.1854(3) 0.7814(2) 0.0870(2) 0.0512(12) Uani 1 1 d . . . H15B H 0.2294 0.7575 0.0833 0.061 Uiso 1 1 calc R . . C16B C 0.1913(3) 0.81455(19) 0.13497(19) 0.0454(11) Uani 1 1 d . . . H16B H 0.2408 0.8139 0.1633 0.054 Uiso 1 1 calc R . . C10C C 0.3110(3) 0.69973(17) 0.29175(18) 0.0403(11) Uani 1 1 d . . . H10C H 0.3263 0.6657 0.2753 0.039(11) Uiso 1 1 calc R . . C11C C 0.3789(3) 0.74126(18) 0.2838(2) 0.0426(11) Uani 1 1 d . . . C12C C 0.3790(3) 0.7619(2) 0.2275(2) 0.0520(13) Uani 1 1 d . . . H12C H 0.3380 0.7500 0.1964 0.062 Uiso 1 1 calc R . . C13C C 0.4383(3) 0.7991(3) 0.2174(2) 0.0703(17) Uani 1 1 d . . . H13C H 0.4378 0.8131 0.1802 0.084 Uiso 1 1 calc R . . C14C C 0.4991(3) 0.8152(3) 0.2647(3) 0.083(2) Uani 1 1 d . . . C15C C 0.5028(3) 0.7942(3) 0.3192(2) 0.0765(19) Uani 1 1 d . . . H15C H 0.5452 0.8052 0.3499 0.092 Uiso 1 1 calc R . . C16C C 0.4430(3) 0.7566(2) 0.3283(2) 0.0551(14) Uani 1 1 d . . . H16C H 0.4460 0.7413 0.3652 0.066 Uiso 1 1 calc R . . H2 H 0.0993 0.6943 0.3367 0.064(16) Uiso 1 1 d R . . H1 H 0.0790 0.8622 0.3442 0.15(3) Uiso 1 1 d 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 C201 0.289(18) 0.219(14) 0.154(11) -0.034(10) 0.039(11) -0.111(14) C203 0.241(16) 0.202(14) 0.31(2) 0.078(14) 0.165(15) 0.055(13) I1 0.1114(4) 0.0424(2) 0.1245(4) 0.0014(2) 0.0520(3) -0.0030(2) Co1 0.0291(3) 0.0268(3) 0.0296(3) 0.0028(2) 0.0055(2) -0.0017(2) Co2 0.0402(3) 0.0457(4) 0.0398(4) 0.0009(3) 0.0084(3) -0.0020(3) Co3 0.0342(3) 0.0401(3) 0.0316(3) 0.0061(3) 0.0023(2) 0.0012(3) Co4 0.0298(3) 0.0291(3) 0.0305(3) 0.0028(2) 0.0034(2) 0.0002(2) Co5 0.0306(3) 0.0442(4) 0.0386(3) 0.0125(3) 0.0053(2) 0.0046(3) O25A 0.0296(15) 0.0337(16) 0.0320(15) -0.0024(13) 0.0046(12) -0.0004(12) O1 0.0335(15) 0.0293(16) 0.0361(15) 0.0062(12) 0.0094(12) -0.0008(12) O1C 0.063(2) 0.066(2) 0.0349(18) 0.0127(16) 0.0045(15) 0.0109(19) O1B 0.0357(16) 0.0400(17) 0.0333(16) 0.0056(13) 0.0004(12) -0.0060(14) O25C 0.0355(16) 0.0413(17) 0.0331(16) 0.0011(14) 0.0004(12) -0.0009(13) O25B 0.0335(18) 0.075(3) 0.081(3) 0.036(2) 0.0089(17) 0.0069(17) O1A 0.051(2) 0.050(2) 0.066(2) 0.0119(17) 0.0065(18) -0.0062(17) O25D 0.053(2) 0.068(2) 0.056(2) -0.0151(18) 0.0087(17) 0.0085(18) O1D 0.0331(15) 0.0366(16) 0.0335(16) 0.0073(13) 0.0021(12) -0.0058(13) O2 0.0325(15) 0.0275(15) 0.0297(14) -0.0001(12) 0.0035(11) -0.0019(12) O27D 0.137(5) 0.055(3) 0.138(5) 0.018(3) 0.000(4) 0.033(3) O28D 0.132(4) 0.062(3) 0.109(4) 0.045(3) 0.004(3) -0.010(3) O27A 0.145(5) 0.074(4) 0.169(6) -0.021(4) -0.049(4) 0.052(4) O28A 0.115(5) 0.109(5) 0.281(10) -0.050(6) 0.066(6) 0.044(4) O27B 0.095(4) 0.154(5) 0.061(3) -0.030(3) -0.007(3) 0.006(3) O28B 0.092(3) 0.108(4) 0.080(3) -0.029(3) 0.023(3) 0.021(3) O27C 0.134(5) 0.298(10) 0.162(6) 0.115(7) -0.017(5) -0.127(6) O28C 0.149(6) 0.416(14) 0.116(5) 0.065(7) -0.020(5) -0.190(8) N26D 0.086(4) 0.048(3) 0.073(4) 0.015(3) -0.025(3) -0.006(3) N9A 0.032(2) 0.036(2) 0.045(2) -0.0033(17) 0.0100(17) 0.0002(16) N17D 0.044(2) 0.038(2) 0.033(2) 0.0045(16) 0.0103(17) -0.0050(17) N9C 0.041(2) 0.037(2) 0.037(2) 0.0084(17) 0.0030(16) 0.0062(17) N9D 0.0303(18) 0.0319(19) 0.0296(18) 0.0022(15) 0.0070(14) -0.0014(15) N17A 0.0324(19) 0.0292(19) 0.037(2) 0.0053(16) 0.0087(15) -0.0007(15) N17B 0.0306(19) 0.038(2) 0.0361(19) 0.0087(16) 0.0072(15) 0.0057(16) N9B 0.0301(19) 0.034(2) 0.0373(19) 0.0044(16) 0.0080(15) 0.0011(16) N17C 0.039(2) 0.034(2) 0.0311(19) -0.0006(16) 0.0054(15) 0.0011(16) N26A 0.080(4) 0.047(3) 0.169(7) -0.017(4) -0.021(4) 0.019(3) N26B 0.062(3) 0.092(4) 0.045(3) -0.004(3) 0.007(2) -0.002(3) N26C 0.098(5) 0.245(10) 0.098(5) 0.051(6) 0.004(4) -0.092(6) C102 0.123(6) 0.077(5) 0.155(8) -0.016(5) 0.107(6) -0.018(5) C202 0.332(16) 0.043(4) 0.093(6) -0.022(4) 0.127(8) -0.051(6) O204 0.548(18) 0.068(4) 0.154(6) -0.040(4) 0.184(9) -0.097(7) O104 0.126(4) 0.057(3) 0.143(4) -0.027(3) 0.065(3) -0.014(3) C101 0.171(9) 0.065(5) 0.177(9) 0.021(5) 0.107(7) 0.022(5) C103 0.161(9) 0.159(9) 0.123(8) -0.055(7) 0.036(7) -0.023(7) C10D 0.035(2) 0.034(2) 0.031(2) 0.0025(18) 0.0067(18) -0.0012(19) C24D 0.059(3) 0.054(3) 0.036(3) 0.000(2) 0.011(2) -0.002(3) C2D 0.031(2) 0.032(2) 0.039(2) -0.0010(19) 0.0108(18) 0.0000(19) C2A 0.039(3) 0.041(3) 0.062(3) -0.007(2) 0.017(2) -0.001(2) C11D 0.037(2) 0.035(2) 0.037(2) 0.006(2) -0.0009(19) 0.000(2) C24C 0.044(3) 0.050(3) 0.028(2) 0.003(2) 0.001(2) -0.016(2) C2C 0.039(3) 0.066(3) 0.042(3) 0.015(3) -0.005(2) -0.006(2) C24B 0.043(3) 0.073(4) 0.046(3) 0.020(3) 0.013(2) 0.022(3) C24A 0.042(2) 0.031(2) 0.028(2) -0.0010(18) 0.0096(19) -0.0063(19) C2B 0.032(2) 0.043(3) 0.042(3) -0.005(2) 0.005(2) -0.006(2) C3D 0.043(3) 0.052(3) 0.038(3) 0.012(2) -0.004(2) -0.010(2) C3B 0.053(3) 0.073(4) 0.047(3) 0.009(3) -0.005(2) -0.014(3) C3C 0.056(3) 0.085(4) 0.057(3) 0.034(3) -0.008(3) -0.006(3) C23C 0.043(3) 0.090(4) 0.041(3) -0.004(3) 0.000(2) -0.017(3) C12D 0.047(3) 0.045(3) 0.064(3) 0.007(2) 0.013(2) 0.003(2) C3A 0.064(4) 0.055(3) 0.079(4) 0.001(3) 0.024(3) -0.012(3) C23B 0.046(3) 0.112(5) 0.068(4) 0.039(4) 0.011(3) 0.031(3) C23A 0.046(3) 0.051(3) 0.048(3) -0.012(2) 0.002(2) 0.000(2) C23D 0.076(4) 0.057(3) 0.054(3) -0.009(3) 0.021(3) 0.012(3) C22D 0.106(5) 0.071(4) 0.050(3) -0.020(3) 0.021(3) 0.005(4) C22A 0.062(3) 0.076(4) 0.053(3) -0.024(3) -0.004(3) -0.008(3) C4C 0.080(4) 0.093(5) 0.066(4) 0.037(4) -0.012(3) -0.016(4) C4B 0.083(5) 0.108(5) 0.065(4) 0.004(4) -0.024(3) -0.045(4) C22B 0.052(4) 0.134(6) 0.067(4) 0.028(4) 0.017(3) 0.047(4) C22C 0.071(4) 0.134(6) 0.050(4) -0.016(4) -0.012(3) -0.032(4) C4D 0.062(3) 0.062(4) 0.047(3) 0.000(3) -0.008(2) -0.015(3) C4A 0.065(4) 0.063(4) 0.113(5) -0.022(4) 0.034(4) -0.029(3) C13D 0.055(3) 0.039(3) 0.090(4) 0.003(3) 0.004(3) 0.006(2) C5A 0.054(3) 0.073(4) 0.089(5) -0.013(4) 0.005(3) -0.016(3) C5C 0.105(5) 0.062(4) 0.097(5) 0.042(4) -0.019(4) 0.003(4) C5B 0.104(6) 0.122(6) 0.107(6) 0.019(5) -0.029(5) -0.078(5) C21B 0.084(5) 0.090(5) 0.069(4) 0.011(4) 0.013(3) 0.053(4) C21C 0.098(5) 0.097(5) 0.068(4) -0.041(4) -0.007(4) -0.021(4) C21D 0.092(5) 0.087(4) 0.048(3) -0.024(3) -0.004(3) 0.001(4) C14D 0.064(3) 0.034(3) 0.059(3) 0.017(2) -0.010(3) -0.005(2) C5D 0.068(4) 0.054(3) 0.061(3) 0.000(3) -0.018(3) -0.023(3) C21A 0.074(4) 0.068(4) 0.065(4) -0.036(3) 0.002(3) -0.004(3) C20A 0.068(4) 0.052(3) 0.059(3) -0.022(3) 0.018(3) 0.000(3) C6B 0.088(5) 0.080(4) 0.078(4) 0.023(3) -0.016(4) -0.047(4) C20B 0.066(4) 0.055(3) 0.061(3) 0.005(3) 0.010(3) 0.027(3) C20C 0.093(5) 0.059(4) 0.065(4) -0.025(3) 0.006(3) -0.009(3) C6C 0.090(4) 0.053(3) 0.078(4) 0.021(3) -0.005(3) 0.013(3) C6A 0.049(3) 0.054(3) 0.076(4) -0.010(3) 0.003(3) -0.003(3) C15D 0.112(5) 0.046(3) 0.058(3) 0.018(3) 0.027(3) -0.002(3) C20D 0.071(4) 0.080(4) 0.042(3) -0.015(3) -0.003(3) 0.000(3) C6D 0.056(3) 0.036(3) 0.053(3) 0.009(2) -0.003(2) -0.008(2) C7B 0.042(3) 0.043(3) 0.050(3) 0.002(2) -0.001(2) -0.014(2) C7C 0.053(3) 0.052(3) 0.049(3) 0.021(2) -0.005(2) 0.001(2) C19C 0.053(3) 0.047(3) 0.038(3) -0.006(2) 0.006(2) -0.010(2) C19B 0.047(3) 0.056(3) 0.034(2) 0.004(2) 0.009(2) 0.019(2) C19A 0.043(3) 0.034(2) 0.038(2) -0.003(2) 0.007(2) -0.006(2) C16D 0.089(4) 0.040(3) 0.059(3) 0.017(2) 0.033(3) 0.012(3) C7D 0.032(2) 0.032(2) 0.039(2) 0.0018(19) 0.0047(18) -0.0030(18) C7A 0.037(3) 0.042(3) 0.055(3) -0.011(2) 0.012(2) 0.000(2) C19D 0.055(3) 0.048(3) 0.036(3) -0.001(2) 0.008(2) -0.003(2) C8C 0.049(3) 0.043(3) 0.054(3) 0.006(2) 0.005(2) 0.012(2) C8D 0.036(2) 0.029(2) 0.039(2) 0.0074(19) 0.0129(19) -0.0019(19) C18C 0.059(3) 0.034(3) 0.040(3) 0.000(2) 0.012(2) 0.004(2) C10A 0.035(2) 0.038(2) 0.039(3) 0.006(2) 0.0055(19) 0.0011(19) C18B 0.045(3) 0.038(3) 0.041(3) 0.004(2) 0.010(2) 0.005(2) C8A 0.038(3) 0.048(3) 0.043(3) 0.000(2) 0.007(2) 0.007(2) C18A 0.047(3) 0.031(2) 0.040(3) 0.001(2) 0.014(2) 0.003(2) C18D 0.040(3) 0.044(3) 0.037(3) 0.003(2) 0.004(2) -0.001(2) C8B 0.046(3) 0.030(2) 0.051(3) 0.005(2) 0.012(2) -0.008(2) C11A 0.035(2) 0.040(3) 0.056(3) 0.003(2) 0.005(2) 0.004(2) C12A 0.089(4) 0.049(3) 0.061(3) 0.005(3) 0.014(3) 0.019(3) C13A 0.128(6) 0.043(3) 0.077(4) 0.007(3) -0.006(4) 0.022(4) C14A 0.050(3) 0.040(3) 0.109(5) -0.010(3) -0.011(3) 0.010(3) C15A 0.072(4) 0.053(4) 0.162(7) -0.009(4) 0.065(5) 0.004(3) C16A 0.070(4) 0.048(3) 0.131(6) 0.012(3) 0.054(4) 0.009(3) C10B 0.033(2) 0.036(2) 0.041(2) 0.011(2) 0.0093(19) 0.0028(19) C11B 0.036(2) 0.048(3) 0.037(2) 0.013(2) 0.011(2) 0.007(2) C12B 0.047(3) 0.082(4) 0.042(3) 0.006(3) 0.004(2) 0.026(3) C13B 0.044(3) 0.105(5) 0.043(3) 0.005(3) -0.001(2) 0.015(3) C14B 0.050(3) 0.073(4) 0.031(3) 0.000(2) 0.012(2) 0.005(3) C15B 0.043(3) 0.071(3) 0.042(3) 0.005(3) 0.015(2) 0.013(2) C16B 0.035(2) 0.062(3) 0.038(3) 0.005(2) 0.006(2) 0.007(2) C10C 0.046(3) 0.035(2) 0.040(3) 0.001(2) 0.009(2) 0.016(2) C11C 0.033(2) 0.051(3) 0.046(3) 0.008(2) 0.010(2) 0.017(2) C12C 0.043(3) 0.073(4) 0.041(3) 0.010(2) 0.008(2) 0.006(3) C13C 0.049(3) 0.112(5) 0.052(3) 0.028(3) 0.015(3) 0.000(3) C14C 0.042(3) 0.134(6) 0.074(4) 0.027(4) 0.014(3) -0.022(3) C15C 0.044(3) 0.135(6) 0.049(3) 0.010(4) 0.001(3) -0.011(4) C16C 0.041(3) 0.087(4) 0.037(3) 0.015(3) 0.005(2) 0.006(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 C201 C202 1.510(16) . ? C203 C202 1.473(17) . ? Co1 O1D 1.888(3) . ? Co1 O25A 1.899(3) . ? Co1 O2 1.914(3) . ? Co1 O1 1.917(3) . ? Co1 N9D 1.952(3) . ? Co1 N17A 1.959(3) . ? Co2 O1A 1.891(3) . ? Co2 O25D 1.907(3) . ? Co2 N9A 1.989(4) . ? Co2 N17D 2.002(4) . ? Co3 O1C 1.908(3) . ? Co3 O1B 1.988(3) . ? Co3 O2 2.002(3) . ? Co3 N9C 2.044(4) . ? Co3 O25A 2.291(3) . ? Co3 Co4 2.9098(8) . ? Co4 O25C 2.031(3) . ? Co4 O1B 2.038(3) . ? Co4 N9B 2.115(3) . ? Co4 N17C 2.119(3) . ? Co4 O2 2.190(3) . ? Co4 O1 2.217(3) . ? Co4 Co5 2.9145(8) . ? Co5 O25B 1.896(3) . ? Co5 O1 1.989(3) . ? Co5 O25C 1.999(3) . ? Co5 N17B 2.046(3) . ? Co5 O1D 2.266(3) . ? O25A C24A 1.319(5) . ? O1C C2C 1.315(6) . ? O1B C2B 1.317(5) . ? O25C C24C 1.335(5) . ? O25B C24B 1.335(6) . ? O1A C2A 1.312(6) . ? O25D C24D 1.315(6) . ? O1D C2D 1.321(5) . ? O27D N26D 1.214(7) . ? O28D N26D 1.212(7) . ? O27A N26A 1.233(9) . ? O28A N26A 1.189(10) . ? O27B N26B 1.203(6) . ? O28B N26B 1.197(6) . ? O27C N26C 1.203(8) . ? O28C N26C 1.187(8) . ? N26D C14D 1.492(6) . ? N9A C8A 1.303(6) . ? N9A C10A 1.470(5) . ? N17D C18D 1.292(5) . ? N17D C10D 1.471(5) . ? N9C C8C 1.288(5) . ? N9C C10C 1.466(5) . ? N9D C8D 1.287(5) . ? N9D C10D 1.480(5) . ? N17A C18A 1.281(5) . ? N17A C10A 1.501(5) . ? N17B C18B 1.288(5) . ? N17B C10B 1.480(5) . ? N9B C8B 1.285(5) . ? N9B C10B 1.478(5) . ? N17C C18C 1.293(5) . ? N17C C10C 1.482(5) . ? N26A C14A 1.495(8) . ? N26B C14B 1.469(7) . ? N26C C14C 1.480(9) . ? C102 O104 1.242(8) . ? C102 C103 1.488(13) . ? C102 C101 1.526(12) . ? C202 O204 1.107(8) . ? C10D C11D 1.526(6) . ? C24D C19D 1.412(7) . ? C24D C23D 1.423(7) . ? C2D C3D 1.388(6) . ? C2D C7D 1.410(6) . ? C2A C3A 1.420(7) . ? C2A C7A 1.427(7) . ? C11D C16D 1.372(6) . ? C11D C12D 1.378(6) . ? C24C C23C 1.396(6) . ? C24C C19C 1.409(7) . ? C2C C7C 1.395(7) . ? C2C C3C 1.403(7) . ? C24B C19B 1.394(7) . ? C24B C23B 1.398(7) . ? C24A C19A 1.389(6) . ? C24A C23A 1.405(6) . ? C2B C3B 1.401(6) . ? C2B C7B 1.405(6) . ? C3D C4D 1.363(7) . ? C3B C4B 1.370(7) . ? C3C C4C 1.369(9) . ? C23C C22C 1.379(8) . ? C12D C13D 1.392(7) . ? C3A C4A 1.381(8) . ? C23B C22B 1.362(9) . ? C23A C22A 1.366(7) . ? C23D C22D 1.348(8) . ? C22D C21D 1.374(8) . ? C22A C21A 1.389(8) . ? C4C C5C 1.360(9) . ? C4B C5B 1.388(9) . ? C22B C21B 1.361(9) . ? C22C C21C 1.377(9) . ? C4D C5D 1.389(7) . ? C4A C5A 1.365(9) . ? C13D C14D 1.372(8) . ? C5A C6A 1.362(8) . ? C5C C6C 1.377(9) . ? C5B C6B 1.373(9) . ? C21B C20B 1.382(8) . ? C21C C20C 1.350(8) . ? C21D C20D 1.351(7) . ? C14D C15D 1.369(8) . ? C5D C6D 1.353(6) . ? C21A C20A 1.369(7) . ? C20A C19A 1.417(6) . ? C6B C7B 1.418(7) . ? C20B C19B 1.395(7) . ? C20C C19C 1.406(7) . ? C6C C7C 1.423(7) . ? C6A C7A 1.398(7) . ? C15D C16D 1.374(7) . ? C20D C19D 1.424(7) . ? C6D C7D 1.407(6) . ? C7B C8B 1.426(6) . ? C7C C8C 1.442(7) . ? C19C C18C 1.439(6) . ? C19B C18B 1.436(6) . ? C19A C18A 1.432(6) . ? C7D C8D 1.432(6) . ? C7A C8A 1.425(6) . ? C19D C18D 1.422(6) . ? C10A C11A 1.519(6) . ? C11A C16A 1.354(7) . ? C11A C12A 1.371(7) . ? C12A C13A 1.369(8) . ? C13A C14A 1.358(9) . ? C14A C15A 1.338(9) . ? C15A C16A 1.408(8) . ? C10B C11B 1.512(6) . ? C11B C12B 1.379(6) . ? C11B C16B 1.386(6) . ? C12B C13B 1.396(7) . ? C13B C14B 1.346(7) . ? C14B C15B 1.368(7) . ? C15B C16B 1.377(7) . ? C10C C11C 1.526(6) . ? C11C C16C 1.368(7) . ? C11C C12C 1.405(6) . ? C12C C13C 1.366(7) . ? C13C C14C 1.387(8) . ? C14C C15C 1.359(8) . ? C15C C16C 1.375(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 Co1 O25A 170.37(12) . . ? O1D Co1 O2 92.87(12) . . ? O25A Co1 O2 80.90(11) . . ? O1D Co1 O1 80.81(11) . . ? O25A Co1 O1 91.17(11) . . ? O2 Co1 O1 83.88(11) . . ? O1D Co1 N9D 94.11(12) . . ? O25A Co1 N9D 93.15(12) . . ? O2 Co1 N9D 89.26(12) . . ? O1 Co1 N9D 171.22(13) . . ? O1D Co1 N17A 91.58(13) . . ? O25A Co1 N17A 93.98(13) . . ? O2 Co1 N17A 173.05(13) . . ? O1 Co1 N17A 91.57(12) . . ? N9D Co1 N17A 95.75(13) . . ? O1A Co2 O25D 121.79(15) . . ? O1A Co2 N9A 95.64(14) . . ? O25D Co2 N9A 117.24(15) . . ? O1A Co2 N17D 111.43(14) . . ? O25D Co2 N17D 95.11(14) . . ? N9A Co2 N17D 117.16(14) . . ? O1C Co3 O1B 138.56(14) . . ? O1C Co3 O2 127.91(13) . . ? O1B Co3 O2 90.62(11) . . ? O1C Co3 N9C 94.78(14) . . ? O1B Co3 N9C 92.97(13) . . ? O2 Co3 N9C 99.16(12) . . ? O1C Co3 O25A 91.46(12) . . ? O1B Co3 O25A 88.21(11) . . ? O2 Co3 O25A 70.00(10) . . ? N9C Co3 O25A 169.12(12) . . ? O1C Co3 Co4 176.68(11) . . ? O1B Co3 Co4 44.39(8) . . ? O2 Co3 Co4 48.78(7) . . ? N9C Co3 Co4 86.25(9) . . ? O25A Co3 Co4 87.04(7) . . ? O25C Co4 O1B 174.11(12) . . ? O25C Co4 N9B 93.60(12) . . ? O1B Co4 N9B 87.96(12) . . ? O25C Co4 N17C 89.13(12) . . ? O1B Co4 N17C 95.16(12) . . ? N9B Co4 N17C 118.00(13) . . ? O25C Co4 O2 92.30(10) . . ? O1B Co4 O2 84.18(10) . . ? N9B Co4 O2 157.44(11) . . ? N17C Co4 O2 83.83(11) . . ? O25C Co4 O1 84.01(11) . . ? O1B Co4 O1 90.37(11) . . ? N9B Co4 O1 87.95(11) . . ? N17C Co4 O1 153.58(12) . . ? O2 Co4 O1 71.03(10) . . ? O25C Co4 Co3 134.64(8) . . ? O1B Co4 Co3 43.03(8) . . ? N9B Co4 Co3 130.79(9) . . ? N17C Co4 Co3 78.54(9) . . ? O2 Co4 Co3 43.42(7) . . ? O1 Co4 Co3 88.25(7) . . ? O25C Co4 Co5 43.24(8) . . ? O1B Co4 Co5 131.75(8) . . ? N9B Co4 Co5 80.33(9) . . ? N17C Co4 Co5 131.60(9) . . ? O2 Co4 Co5 89.22(7) . . ? O1 Co4 Co5 42.97(7) . . ? Co3 Co4 Co5 125.03(3) . . ? O25B Co5 O1 128.26(14) . . ? O25B Co5 O25C 138.75(15) . . ? O1 Co5 O25C 91.10(11) . . ? O25B Co5 N17B 93.36(14) . . ? O1 Co5 N17B 96.79(12) . . ? O25C Co5 N17B 93.48(12) . . ? O25B Co5 O1D 94.49(12) . . ? O1 Co5 O1D 70.52(10) . . ? O25C Co5 O1D 87.15(11) . . ? N17B Co5 O1D 167.31(12) . . ? O25B Co5 Co4 176.95(13) . . ? O1 Co5 Co4 49.47(8) . . ? O25C Co5 Co4 44.11(8) . . ? N17B Co5 Co4 85.13(9) . . ? O1D Co5 Co4 86.54(7) . . ? C24A O25A Co1 127.7(3) . . ? C24A O25A Co3 130.3(2) . . ? Co1 O25A Co3 99.31(11) . . ? Co1 O1 Co5 109.09(13) . . ? Co1 O1 Co4 101.98(11) . . ? Co5 O1 Co4 87.55(10) . . ? C2C O1C Co3 125.0(3) . . ? C2B O1B Co3 135.8(3) . . ? C2B O1B Co4 131.5(3) . . ? Co3 O1B Co4 92.57(11) . . ? C24C O25C Co5 136.0(3) . . ? C24C O25C Co4 130.7(3) . . ? Co5 O25C Co4 92.65(12) . . ? C24B O25B Co5 126.4(3) . . ? C2A O1A Co2 125.8(3) . . ? C24D O25D Co2 126.3(3) . . ? C2D O1D Co1 128.3(3) . . ? C2D O1D Co5 128.6(2) . . ? Co1 O1D Co5 99.57(11) . . ? Co1 O2 Co3 109.77(12) . . ? Co1 O2 Co4 103.07(12) . . ? Co3 O2 Co4 87.80(10) . . ? O28D N26D O27D 125.1(5) . . ? O28D N26D C14D 117.4(6) . . ? O27D N26D C14D 117.5(6) . . ? C8A N9A C10A 116.2(4) . . ? C8A N9A Co2 120.9(3) . . ? C10A N9A Co2 122.9(3) . . ? C18D N17D C10D 116.3(4) . . ? C18D N17D Co2 121.8(3) . . ? C10D N17D Co2 121.8(3) . . ? C8C N9C C10C 115.7(4) . . ? C8C N9C Co3 120.4(3) . . ? C10C N9C Co3 123.5(3) . . ? C8D N9D C10D 118.9(3) . . ? C8D N9D Co1 122.7(3) . . ? C10D N9D Co1 118.3(2) . . ? C18A N17A C10A 118.1(4) . . ? C18A N17A Co1 122.3(3) . . ? C10A N17A Co1 119.6(3) . . ? C18B N17B C10B 116.6(4) . . ? C18B N17B Co5 121.3(3) . . ? C10B N17B Co5 122.1(3) . . ? C8B N9B C10B 114.9(4) . . ? C8B N9B Co4 123.5(3) . . ? C10B N9B Co4 121.1(3) . . ? C18C N17C C10C 114.2(4) . . ? C18C N17C Co4 123.2(3) . . ? C10C N17C Co4 122.1(3) . . ? O28A N26A O27A 126.2(7) . . ? O28A N26A C14A 119.3(8) . . ? O27A N26A C14A 114.5(8) . . ? O28B N26B O27B 123.4(5) . . ? O28B N26B C14B 118.8(5) . . ? O27B N26B C14B 117.8(5) . . ? O28C N26C O27C 124.6(7) . . ? O28C N26C C14C 118.1(7) . . ? O27C N26C C14C 116.7(7) . . ? O104 C102 C103 124.1(9) . . ? O104 C102 C101 116.8(9) . . ? C103 C102 C101 119.1(8) . . ? O204 C202 C203 115.1(16) . . ? O204 C202 C201 127.9(16) . . ? C203 C202 C201 117.0(11) . . ? N17D C10D N9D 106.6(3) . . ? N17D C10D C11D 112.3(3) . . ? N9D C10D C11D 116.3(3) . . ? O25D C24D C19D 124.0(4) . . ? O25D C24D C23D 118.2(5) . . ? C19D C24D C23D 117.8(5) . . ? O1D C2D C3D 119.2(4) . . ? O1D C2D C7D 122.3(4) . . ? C3D C2D C7D 118.4(4) . . ? O1A C2A C3A 118.6(5) . . ? O1A C2A C7A 124.2(4) . . ? C3A C2A C7A 117.3(5) . . ? C16D C11D C12D 119.8(4) . . ? C16D C11D C10D 122.0(4) . . ? C12D C11D C10D 118.0(4) . . ? O25C C24C C23C 119.5(5) . . ? O25C C24C C19C 121.9(4) . . ? C23C C24C C19C 118.6(4) . . ? O1C C2C C7C 124.7(4) . . ? O1C C2C C3C 116.9(5) . . ? C7C C2C C3C 118.4(5) . . ? O25B C24B C19B 124.0(4) . . ? O25B C24B C23B 117.1(5) . . ? C19B C24B C23B 118.9(5) . . ? O25A C24A C19A 123.1(4) . . ? O25A C24A C23A 118.8(4) . . ? C19A C24A C23A 118.1(4) . . ? O1B C2B C3B 119.7(4) . . ? O1B C2B C7B 121.5(4) . . ? C3B C2B C7B 118.8(4) . . ? C4D C3D C2D 121.3(4) . . ? C4B C3B C2B 121.2(5) . . ? C4C C3C C2C 120.6(6) . . ? C22C C23C C24C 120.6(6) . . ? C11D C12D C13D 120.3(5) . . ? C4A C3A C2A 119.6(6) . . ? C22B C23B C24B 120.3(6) . . ? C22A C23A C24A 121.3(5) . . ? C22D C23D C24D 121.3(5) . . ? C23D C22D C21D 121.1(5) . . ? C23A C22A C21A 121.0(5) . . ? C5C C4C C3C 121.7(6) . . ? C3B C4B C5B 121.0(5) . . ? C21B C22B C23B 122.1(6) . . ? C21C C22C C23C 121.0(6) . . ? C3D C4D C5D 120.8(5) . . ? C5A C4A C3A 123.3(5) . . ? C14D C13D C12D 118.2(5) . . ? C6A C5A C4A 117.9(5) . . ? C4C C5C C6C 119.9(6) . . ? C6B C5B C4B 118.8(6) . . ? C22B C21B C20B 118.3(6) . . ? C20C C21C C22C 119.0(6) . . ? C20D C21D C22D 120.1(5) . . ? C15D C14D C13D 122.2(4) . . ? C15D C14D N26D 118.9(5) . . ? C13D C14D N26D 118.9(6) . . ? C6D C5D C4D 119.1(5) . . ? C20A C21A C22A 118.8(5) . . ? C21A C20A C19A 121.0(5) . . ? C5B C6B C7B 121.7(6) . . ? C21B C20B C19B 121.8(6) . . ? C21C C20C C19C 122.5(6) . . ? C5C C6C C7C 119.8(6) . . ? C5A C6A C7A 122.7(6) . . ? C14D C15D C16D 118.7(5) . . ? C21D C20D C19D 121.4(6) . . ? C5D C6D C7D 121.8(4) . . ? C2B C7B C6B 118.5(4) . . ? C2B C7B C8B 125.2(4) . . ? C6B C7B C8B 116.1(4) . . ? C2C C7C C6C 119.7(5) . . ? C2C C7C C8C 125.6(4) . . ? C6C C7C C8C 114.7(5) . . ? C20C C19C C24C 118.2(5) . . ? C20C C19C C18C 116.1(5) . . ? C24C C19C C18C 125.7(4) . . ? C24B C19B C20B 118.6(4) . . ? C24B C19B C18B 125.1(4) . . ? C20B C19B C18B 115.9(5) . . ? C24A C19A C20A 119.7(4) . . ? C24A C19A C18A 123.6(4) . . ? C20A C19A C18A 116.6(4) . . ? C11D C16D C15D 120.8(5) . . ? C6D C7D C2D 118.5(4) . . ? C6D C7D C8D 117.9(4) . . ? C2D C7D C8D 123.5(4) . . ? C6A C7A C8A 117.1(5) . . ? C6A C7A C2A 119.2(4) . . ? C8A C7A C2A 123.6(4) . . ? C24D C19D C18D 125.1(4) . . ? C24D C19D C20D 118.3(4) . . ? C18D C19D C20D 116.5(5) . . ? N9C C8C C7C 126.7(5) . . ? N9D C8D C7D 127.8(4) . . ? N17C C18C C19C 128.8(4) . . ? N9A C10A N17A 106.5(3) . . ? N9A C10A C11A 112.5(3) . . ? N17A C10A C11A 114.8(3) . . ? N17B C18B C19B 126.1(4) . . ? N9A C8A C7A 127.9(4) . . ? N17A C18A C19A 128.2(4) . . ? N17D C18D C19D 127.1(4) . . ? N9B C8B C7B 129.3(4) . . ? C16A C11A C12A 118.0(5) . . ? C16A C11A C10A 123.2(4) . . ? C12A C11A C10A 118.7(4) . . ? C13A C12A C11A 121.9(6) . . ? C14A C13A C12A 118.6(6) . . ? C15A C14A C13A 121.9(5) . . ? C15A C14A N26A 117.5(7) . . ? C13A C14A N26A 120.5(7) . . ? C14A C15A C16A 118.6(6) . . ? C11A C16A C15A 120.9(6) . . ? N9B C10B N17B 108.1(3) . . ? N9B C10B C11B 113.4(3) . . ? N17B C10B C11B 109.7(3) . . ? C12B C11B C16B 118.6(4) . . ? C12B C11B C10B 120.0(4) . . ? C16B C11B C10B 121.4(4) . . ? C11B C12B C13B 120.3(5) . . ? C14B C13B C12B 118.8(5) . . ? C13B C14B C15B 122.7(5) . . ? C13B C14B N26B 118.6(5) . . ? C15B C14B N26B 118.6(5) . . ? C14B C15B C16B 118.2(4) . . ? C15B C16B C11B 121.2(4) . . ? N9C C10C N17C 108.8(3) . . ? N9C C10C C11C 113.0(4) . . ? N17C C10C C11C 109.1(3) . . ? C16C C11C C12C 118.7(4) . . ? C16C C11C C10C 122.8(4) . . ? C12C C11C C10C 118.4(4) . . ? C13C C12C C11C 121.2(5) . . ? C12C C13C C14C 117.5(5) . . ? C15C C14C C13C 122.5(6) . . ? C15C C14C N26C 118.8(6) . . ? C13C C14C N26C 118.6(6) . . ? C14C C15C C16C 119.0(5) . . ? C11C C16C C15C 120.9(5) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.469 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.071 #===END data_[Co5(OH)2(salClben)4]I.2dmf.CH2Cl2 _database_code_CSD 188688 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H78 Cl6 Co5 I N10 O12' _chemical_formula_weight 2137.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'I' 'I' -0.4742 1.8119 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic unique axis b' _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 15.495(2) _cell_length_b 25.344(4) _cell_length_c 23.663(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.640(10) _cell_angle_gamma 90.00 _cell_volume 9101(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.0 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4320 _exptl_absorpt_coefficient_mu 1.474 _exptl_absorpt_correction_type 'SADABS' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD DIFFRACTOMETER' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23202 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2259 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 29.46 _reflns_number_total 23202 _reflns_number_gt 13363 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23202 _refine_ls_number_parameters 1191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1062 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _refine_ls_shift/su_max 0.426 _refine_ls_shift/su_mean 0.031 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 I1 I 0.83806(3) 0.538306(12) 0.755353(19) 0.09422(14) Uani 1 1 d . . . Co1 Co 0.96845(3) 0.260455(16) 0.627407(18) 0.02894(10) Uani 1 1 d . . . Co2 Co 1.13635(3) 0.231386(19) 0.52042(2) 0.04260(12) Uani 1 1 d . . . Co3 Co 0.76334(3) 0.232012(17) 0.597987(19) 0.03642(11) Uani 1 1 d . . . Co4 Co 0.83224(3) 0.277200(16) 0.711501(19) 0.03209(11) Uani 1 1 d . . . Co5 Co 1.01518(3) 0.309483(18) 0.75352(2) 0.03705(11) Uani 1 1 d . . . ClD Cl 0.86708(10) -0.03226(5) 0.44326(7) 0.0994(5) Uani 1 1 d . . . ClB Cl 0.88457(9) 0.24098(6) 1.01392(5) 0.0862(4) Uani 1 1 d . . . ClA Cl 1.34342(9) 0.50427(5) 0.58581(9) 0.1123(6) Uani 1 1 d . . . ClC Cl 0.40805(10) 0.36480(7) 0.72119(7) 0.1181(6) Uani 1 1 d . . . Cl1S Cl 0.6272(3) 0.38276(16) 0.86191(18) 0.1288(12) Uani 1 1 d P . . Cl2S Cl 0.7694(3) 0.45371(14) 0.9047(2) 0.1326(13) Uani 1 1 d P . . O1B O 0.74053(14) 0.29717(8) 0.64030(9) 0.0385(5) Uani 1 1 d . . . O1A O 1.20348(18) 0.16839(11) 0.53027(12) 0.0596(7) Uani 1 1 d . . . O1 O 0.93762(14) 0.31447(9) 0.67543(10) 0.0330(5) Uani 1 1 d . . . O1D O 1.05340(14) 0.24687(8) 0.69548(9) 0.0344(5) Uani 1 1 d . . . O1S O 0.9376(3) 0.41399(13) 0.64328(16) 0.1003(13) Uani 1 1 d . . . O1C O 0.72570(18) 0.20011(11) 0.52430(11) 0.0564(7) Uani 1 1 d . . . O2 O 0.87759(13) 0.22190(8) 0.65327(9) 0.0318(5) Uani 1 1 d . . . H2 H 0.8919 0.1861 0.6677 0.064(9) Uiso 1 1 calc R . . O6S O 0.9003(2) 0.11966(12) 0.68318(16) 0.0816(10) Uani 1 1 d . . . O25C O 0.93310(14) 0.25733(9) 0.77744(9) 0.0375(5) Uani 1 1 d . . . O25B O 1.13222(16) 0.33478(12) 0.77799(14) 0.0672(8) Uani 1 1 d . . . O25D O 1.14610(17) 0.28118(11) 0.46169(12) 0.0567(7) Uani 1 1 d . . . O25A O 0.87121(13) 0.27745(8) 0.56704(9) 0.0339(5) Uani 1 1 d . . . N3S N 0.8960(4) 0.48985(19) 0.5995(2) 0.1103(18) Uani 1 1 d . . . N8S N 0.9563(4) 0.0469(2) 0.7324(3) 0.121(2) Uani 1 1 d . . . N9A N 1.18099(17) 0.25859(11) 0.60020(12) 0.0375(6) Uani 1 1 d . . . N9D N 0.99725(16) 0.19711(10) 0.58871(11) 0.0310(6) Uani 1 1 d . . . N9B N 0.81170(17) 0.35149(11) 0.74755(12) 0.0364(6) Uani 1 1 d . . . N9C N 0.68461(17) 0.18632(11) 0.63781(12) 0.0394(7) Uani 1 1 d . . . N17B N 0.96171(18) 0.37258(11) 0.78728(12) 0.0376(6) Uani 1 1 d . . . N17D N 1.00653(18) 0.22075(11) 0.49379(11) 0.0369(6) Uani 1 1 d . . . N17C N 0.75993(17) 0.21178(10) 0.73254(11) 0.0348(6) Uani 1 1 d . . . N17A N 1.04950(16) 0.30750(10) 0.59751(11) 0.0325(6) Uani 1 1 d . . . C1S C 0.6921(8) 0.3986(4) 0.9212(4) 0.202(5) Uani 1 1 d . . . C2S C 0.8785(5) 0.4412(2) 0.6149(3) 0.0939(18) Uani 1 1 d . . . C2D C 1.1002(2) 0.20349(12) 0.71016(14) 0.0332(7) Uani 1 1 d . . . C2A C 1.2722(2) 0.15889(15) 0.57271(18) 0.0511(10) Uani 1 1 d . . . C2C C 0.6878(2) 0.15317(17) 0.51525(17) 0.0540(10) Uani 1 1 d . . . C2B C 0.6888(2) 0.33913(14) 0.62854(15) 0.0414(8) Uani 1 1 d . . . C3D C 1.1546(2) 0.20100(15) 0.76516(15) 0.0458(9) Uani 1 1 d . . . H3D H 1.1572 0.2295 0.7901 0.053(11) Uiso 1 1 calc R . . C3C C 0.6841(3) 0.1294(2) 0.4610(2) 0.0698(13) Uani 1 1 d . . . H3C H 0.7056 0.1477 0.4326 0.084(17) Uiso 1 1 calc R . . C3A C 1.3260(3) 0.11475(17) 0.5684(2) 0.0672(12) Uani 1 1 d . . . H3A H 1.3135 0.0936 0.5357 0.088(16) Uiso 1 1 calc R . . C3B C 0.6263(3) 0.34162(18) 0.57670(17) 0.0610(11) Uani 1 1 d . . . H3B H 0.6211 0.3134 0.5511 0.073(14) Uiso 1 1 calc R . . C4A C 1.3959(3) 0.1025(2) 0.6113(3) 0.0768(14) Uani 1 1 d . . . H4A H 1.4300 0.0731 0.6070 0.088(15) Uiso 1 1 calc R . . C4C C 0.6496(3) 0.0798(2) 0.4490(2) 0.0815(16) Uani 1 1 d . . . H4C H 0.6483 0.0651 0.4128 0.17(3) Uiso 1 1 calc R . . C4B C 0.5727(4) 0.3846(2) 0.5630(2) 0.0961(19) Uani 1 1 d . . . H4B H 0.5317 0.3854 0.5285 0.12(2) Uiso 1 1 calc R . . C4S C 0.9868(6) 0.5131(3) 0.6216(5) 0.166(4) Uani 1 1 d . . . C4D C 1.2044(3) 0.15641(17) 0.78253(17) 0.0589(11) Uani 1 1 d . . . H4D H 1.2403 0.1553 0.8191 0.061(12) Uiso 1 1 calc R . . C5B C 0.5796(4) 0.4277(2) 0.6011(3) 0.116(2) Uani 1 1 d . . . H5B H 0.5435 0.4570 0.5919 0.109(18) Uiso 1 1 calc R . . C5C C 0.6166(4) 0.0515(2) 0.4896(3) 0.0914(18) Uani 1 1 d . . . H5C H 0.5941 0.0178 0.4812 0.095(17) Uiso 1 1 calc R . . C5A C 1.4176(3) 0.13222(18) 0.6609(2) 0.0687(13) Uani 1 1 d . . . H5A H 1.4655 0.1232 0.6898 0.093(17) Uiso 1 1 calc R . . C5S C 0.8249(8) 0.5225(4) 0.5660(5) 0.232(6) Uani 1 1 d . . . C5D C 1.2011(3) 0.11355(16) 0.74611(18) 0.0619(11) Uani 1 1 d . . . H5D H 1.2333 0.0832 0.7585 0.086(15) Uiso 1 1 calc R . . C6A C 1.3674(3) 0.17498(17) 0.6667(2) 0.0567(10) Uani 1 1 d . . . H6A H 1.3814 0.1952 0.7001 0.072(14) Uiso 1 1 calc R . . C6D C 1.1502(3) 0.11601(15) 0.69168(17) 0.0543(10) Uani 1 1 d . . . H6D H 1.1498 0.0874 0.6670 0.061(12) Uiso 1 1 calc R . . C6C C 0.6175(3) 0.07396(18) 0.5437(2) 0.0723(13) Uani 1 1 d . . . H6C H 0.5941 0.0555 0.5710 0.064(14) Uiso 1 1 calc R . . C6B C 0.6397(4) 0.4258(2) 0.6516(2) 0.0952(19) Uani 1 1 d . . . H6B H 0.6443 0.4544 0.6767 0.098(17) Uiso 1 1 calc R . . C7A C 1.2943(2) 0.18974(14) 0.62323(16) 0.0439(8) Uani 1 1 d . . . C7S C 0.9496(4) 0.0992(2) 0.7251(3) 0.105(2) Uani 1 1 d . . . C7B C 0.6953(3) 0.38192(15) 0.66717(17) 0.0529(10) Uani 1 1 d . . . C7C C 0.6539(2) 0.12480(15) 0.55687(17) 0.0497(9) Uani 1 1 d . . . C7D C 1.0986(2) 0.16059(13) 0.67202(14) 0.0363(7) Uani 1 1 d . . . C8D C 1.0492(2) 0.16043(12) 0.61395(14) 0.0357(7) Uani 1 1 d . . . H8D H 1.0551 0.1307 0.5920 0.037(9) Uiso 1 1 calc R . . C8A C 1.2474(2) 0.23567(13) 0.63458(15) 0.0406(8) Uani 1 1 d . . . H8A H 1.2660 0.2512 0.6706 0.024(8) Uiso 1 1 calc R . . C8C C 0.6515(2) 0.14280(14) 0.61435(16) 0.0461(9) Uani 1 1 d . . . H8C H 0.6234 0.1211 0.6367 0.062(12) Uiso 1 1 calc R . . C8B C 0.7569(2) 0.38609(15) 0.72126(16) 0.0489(9) Uani 1 1 d . . . H8B H 0.7573 0.4184 0.7400 0.053(11) Uiso 1 1 calc R . . C9S C 1.0173(6) 0.0256(4) 0.7817(4) 0.180(4) Uani 1 1 d . . . C10B C 0.8718(2) 0.37193(13) 0.79934(14) 0.0388(8) Uani 1 1 d . . . H10B H 0.8546 0.4082 0.8063 0.033(8) Uiso 1 1 calc R . . C10C C 0.6733(2) 0.19634(13) 0.69721(14) 0.0396(8) Uani 1 1 d . . . H10C H 0.6545 0.1634 0.7128 0.035(8) Uiso 1 1 calc R . . C10S C 0.9004(7) 0.0131(3) 0.6909(4) 0.161(4) Uani 1 1 d . . . C10D C 0.9551(2) 0.18924(12) 0.52697(13) 0.0352(7) Uani 1 1 d . . . H10D H 0.8964 0.2052 0.5212 0.022(7) Uiso 1 1 calc R . . C10A C 1.1460(2) 0.30640(12) 0.62324(14) 0.0356(7) Uani 1 1 d . . . H10A H 1.1531 0.3023 0.6651 0.032(8) Uiso 1 1 calc R . . C11C C 0.6048(2) 0.23894(14) 0.70129(15) 0.0410(8) Uani 1 1 d . . . C11D C 0.9425(2) 0.13198(13) 0.50767(15) 0.0402(8) Uani 1 1 d . . . C11B C 0.8727(2) 0.33934(14) 0.85366(15) 0.0432(8) Uani 1 1 d . . . C11A C 1.1957(2) 0.35587(13) 0.61168(16) 0.0417(8) Uani 1 1 d . . . C12A C 1.2476(2) 0.35784(15) 0.57073(18) 0.0538(10) Uani 1 1 d . . . H12A H 1.2519 0.3284 0.5481 0.046(10) Uiso 1 1 calc R . . C12D C 0.8918(3) 0.09984(15) 0.53526(18) 0.0535(10) Uani 1 1 d . . . H12D H 0.8722 0.1126 0.5673 0.061(12) Uiso 1 1 calc R . . C12C C 0.5448(2) 0.25699(17) 0.65402(17) 0.0533(10) Uani 1 1 d . . . H12C H 0.5452 0.2432 0.6176 0.040(9) Uiso 1 1 calc R . . C12B C 0.8051(2) 0.30516(17) 0.85851(17) 0.0544(10) Uani 1 1 d . . . H12B H 0.7570 0.3023 0.8280 0.051(11) Uiso 1 1 calc R . . C13A C 1.2934(3) 0.40352(18) 0.5630(2) 0.0675(12) Uani 1 1 d . . . H13A H 1.3292 0.4045 0.5359 0.077(14) Uiso 1 1 calc R . . C13B C 0.8072(3) 0.27507(19) 0.90756(18) 0.0639(12) Uani 1 1 d . . . H13B H 0.7618 0.2516 0.9099 0.69(19) Uiso 1 1 calc R . . C13C C 0.4841(3) 0.29546(18) 0.6604(2) 0.0636(12) Uani 1 1 d . . . H13C H 0.4441 0.3078 0.6284 0.12(2) Uiso 1 1 calc R . . C13D C 0.8697(3) 0.04899(15) 0.5162(2) 0.0602(11) Uani 1 1 d . . . H13D H 0.8362 0.0276 0.5354 0.064(13) Uiso 1 1 calc R . . C14D C 0.8979(3) 0.03117(16) 0.4691(2) 0.0636(12) Uani 1 1 d . . . C14A C 1.2855(3) 0.44707(16) 0.5958(2) 0.0659(13) Uani 1 1 d . . . C14C C 0.4834(3) 0.31485(19) 0.7135(2) 0.0676(12) Uani 1 1 d . . . C14B C 0.8778(3) 0.28061(18) 0.95278(16) 0.0580(11) Uani 1 1 d . . . C15C C 0.5392(3) 0.2960(2) 0.7616(2) 0.0762(14) Uani 1 1 d . . . H15C H 0.5356 0.3087 0.7980 0.106(18) Uiso 1 1 calc R . . C15B C 0.9436(3) 0.3156(2) 0.95020(18) 0.0720(14) Uani 1 1 d . . . H15B H 0.9900 0.3199 0.9816 0.13(2) Uiso 1 1 calc R . . C15A C 1.2340(3) 0.44679(17) 0.6364(2) 0.0676(12) Uani 1 1 d . . . H15A H 1.2293 0.4769 0.6581 0.066(13) Uiso 1 1 calc R . . C15D C 0.9496(3) 0.06075(18) 0.44129(19) 0.0700(13) Uani 1 1 d . . . H15D H 0.9697 0.0471 0.4098 0.084(15) Uiso 1 1 calc R . . C16D C 0.9726(3) 0.11287(16) 0.46114(18) 0.0589(11) Uani 1 1 d . . . H16D H 1.0077 0.1338 0.4426 0.042(10) Uiso 1 1 calc R . . C16B C 0.9410(3) 0.34459(19) 0.90062(17) 0.0630(12) Uani 1 1 d . . . H16B H 0.9863 0.3682 0.8988 0.066(12) Uiso 1 1 calc R . . C16C C 0.6011(3) 0.25776(18) 0.75596(18) 0.0578(11) Uani 1 1 d . . . H16C H 0.6396 0.2449 0.7883 2.0(8) Uiso 1 1 calc R . . C16A C 1.1883(3) 0.40068(15) 0.64519(18) 0.0542(10) Uani 1 1 d . . . H16A H 1.1534 0.3998 0.6729 2.0(8) Uiso 1 1 calc R . . C18D C 0.9628(2) 0.24378(14) 0.44804(15) 0.0434(8) Uani 1 1 d . . . H18D H 0.9026 0.2371 0.4391 0.065(13) Uiso 1 1 calc R . . C18C C 0.7915(2) 0.17774(13) 0.77235(15) 0.0410(8) Uani 1 1 d . . . H18C H 0.7568 0.1482 0.7742 0.043(10) Uiso 1 1 calc R . . C18B C 1.0022(2) 0.41731(14) 0.79409(15) 0.0445(9) Uani 1 1 d . . . H18B H 0.9698 0.4468 0.8005 0.070(13) Uiso 1 1 calc R . . C18A C 1.0228(2) 0.34125(13) 0.55725(14) 0.0387(8) Uani 1 1 d . . . H18A H 1.0657 0.3637 0.5485 0.030(8) Uiso 1 1 calc R . . C19C C 0.8735(2) 0.17969(14) 0.81404(15) 0.0439(8) Uani 1 1 d . . . C19A C 0.9357(2) 0.34878(13) 0.52416(15) 0.0389(8) Uani 1 1 d . . . C19B C 1.0936(3) 0.42513(15) 0.79254(15) 0.0481(9) Uani 1 1 d . . . C19D C 0.9961(3) 0.27830(15) 0.40957(15) 0.0487(9) Uani 1 1 d . . . C20A C 0.9229(3) 0.38968(15) 0.48323(17) 0.0553(10) Uani 1 1 d . . . H20A H 0.9703 0.4111 0.4798 0.057(11) Uiso 1 1 calc R . . C20D C 0.9339(3) 0.29869(18) 0.36206(18) 0.0641(12) Uani 1 1 d . . . H20D H 0.8757 0.2873 0.3565 0.052(11) Uiso 1 1 calc R . . C20C C 0.8863(3) 0.13908(18) 0.85513(19) 0.0662(12) Uani 1 1 d . . . H20C H 0.8439 0.1127 0.8528 0.13(2) Uiso 1 1 calc R . . C20B C 1.1236(4) 0.4781(2) 0.80060(18) 0.0731(14) Uani 1 1 d . . . H20B H 1.0826 0.5049 0.8005 0.20(4) Uiso 1 1 calc R . . C21C C 0.9593(3) 0.1372(2) 0.8986(2) 0.0854(16) Uani 1 1 d . . . H21C H 0.9664 0.1098 0.9253 0.116(19) Uiso 1 1 calc R . . C21D C 0.9565(4) 0.3341(2) 0.3247(2) 0.0768(14) Uani 1 1 d . . . H21D H 0.9147 0.3468 0.2940 0.077(14) Uiso 1 1 calc R . . C21A C 0.8425(3) 0.39881(18) 0.4483(2) 0.0688(13) Uani 1 1 d . . . H21A H 0.8344 0.4270 0.4227 0.090(15) Uiso 1 1 calc R . . C21B C 1.2105(4) 0.4907(2) 0.8085(2) 0.0850(16) Uani 1 1 d . . . H21B H 1.2291 0.5255 0.8140 2.0(7) Uiso 1 1 calc R . . C22A C 0.7736(3) 0.36529(18) 0.45200(19) 0.0658(12) Uani 1 1 d . . . H22A H 0.7193 0.3702 0.4274 0.064(12) Uiso 1 1 calc R . . C22D C 1.0441(4) 0.35096(19) 0.3334(2) 0.0774(14) Uani 1 1 d . . . H22D H 1.0609 0.3747 0.3077 0.092(16) Uiso 1 1 calc R . . C22B C 1.2699(4) 0.4509(3) 0.8081(2) 0.0924(19) Uani 1 1 d . . . H22B H 1.3295 0.4592 0.8138 0.103(18) Uiso 1 1 calc R . . C22C C 1.0214(3) 0.1756(2) 0.90242(19) 0.0727(13) Uani 1 1 d . . . H22C H 1.0701 0.1750 0.9327 0.096(16) Uiso 1 1 calc R . . C23B C 1.2439(3) 0.3979(2) 0.7994(2) 0.0788(15) Uani 1 1 d . . . H23B H 1.2861 0.3717 0.8001 0.070(15) Uiso 1 1 calc R . . C23C C 1.0130(3) 0.21584(17) 0.86145(16) 0.0547(10) Uani 1 1 d . . . H23C H 1.0571 0.2411 0.8642 0.063(13) Uiso 1 1 calc R . . C23A C 0.7841(2) 0.32486(15) 0.49141(16) 0.0484(9) Uani 1 1 d . . . H23A H 0.7368 0.3027 0.4929 0.032(8) Uiso 1 1 calc R . . C23D C 1.1048(3) 0.33311(17) 0.37879(19) 0.0653(12) Uani 1 1 d . . . H23D H 1.1622 0.3458 0.3840 0.054(12) Uiso 1 1 calc R . . C24B C 1.1540(3) 0.38453(18) 0.78969(17) 0.0563(11) Uani 1 1 d . . . C24A C 0.8641(2) 0.31634(12) 0.52910(13) 0.0339(7) Uani 1 1 d . . . C24C C 0.9401(2) 0.21881(14) 0.81686(14) 0.0396(8) Uani 1 1 d . . . C24D C 1.0839(3) 0.29574(15) 0.41856(16) 0.0497(9) Uani 1 1 d . . . H1 H 0.936(3) 0.3427(16) 0.6651(17) 0.057(14) 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 I1 0.1183(3) 0.04537(18) 0.1264(3) 0.00114(18) 0.0425(3) 0.00947(18) Co1 0.0280(2) 0.0267(2) 0.0316(2) -0.00016(17) 0.00465(17) 0.00292(17) Co2 0.0370(3) 0.0506(3) 0.0396(3) -0.0026(2) 0.0063(2) 0.0046(2) Co3 0.0333(2) 0.0387(3) 0.0353(2) -0.00219(19) 0.00220(19) 0.00045(19) Co4 0.0292(2) 0.0303(2) 0.0356(2) -0.00062(18) 0.00388(18) -0.00061(18) Co5 0.0301(2) 0.0397(3) 0.0407(3) -0.0082(2) 0.00558(19) -0.00498(19) ClD 0.1209(11) 0.0467(6) 0.1105(11) -0.0300(7) -0.0246(9) -0.0011(7) ClB 0.0836(9) 0.1231(11) 0.0538(7) 0.0230(7) 0.0182(6) -0.0024(8) ClA 0.0734(9) 0.0577(7) 0.2006(18) 0.0322(9) 0.0157(10) -0.0197(6) ClC 0.0793(10) 0.1529(15) 0.1196(13) -0.0291(11) 0.0145(9) 0.0600(10) Cl1S 0.150(3) 0.151(3) 0.162(3) -0.036(2) 0.028(2) 0.000(2) Cl2S 0.150(3) 0.112(2) 0.227(4) -0.021(2) 0.068(3) -0.007(2) O1B 0.0372(13) 0.0356(12) 0.0406(13) -0.0017(10) 0.0030(10) 0.0043(10) O1A 0.0537(17) 0.0541(16) 0.0673(19) -0.0158(14) 0.0033(14) 0.0128(13) O1 0.0332(12) 0.0281(12) 0.0386(13) -0.0021(10) 0.0092(10) 0.0023(10) O1D 0.0332(12) 0.0332(12) 0.0353(12) -0.0034(9) 0.0029(10) 0.0049(9) O1S 0.169(4) 0.0449(19) 0.091(3) 0.0083(18) 0.038(3) 0.010(2) O1C 0.0600(17) 0.0666(18) 0.0398(15) -0.0102(13) 0.0038(12) -0.0090(14) O2 0.0305(11) 0.0285(11) 0.0356(12) 0.0031(9) 0.0047(9) 0.0010(9) O6S 0.098(3) 0.0520(18) 0.101(3) 0.0195(18) 0.034(2) 0.0169(17) O25C 0.0331(12) 0.0397(13) 0.0372(13) 0.0030(10) 0.0010(10) -0.0040(10) O25B 0.0343(14) 0.0673(19) 0.098(2) -0.0337(17) 0.0090(14) -0.0127(13) O25D 0.0480(16) 0.0715(19) 0.0518(16) 0.0088(14) 0.0128(13) -0.0045(13) O25A 0.0295(11) 0.0340(12) 0.0360(12) 0.0032(10) 0.0015(9) 0.0021(9) N3S 0.183(6) 0.066(3) 0.085(3) 0.017(2) 0.035(3) 0.045(3) N8S 0.161(5) 0.081(4) 0.143(5) 0.052(4) 0.080(4) 0.036(4) N9A 0.0318(15) 0.0383(15) 0.0423(16) 0.0001(13) 0.0072(12) -0.0006(12) N9D 0.0319(14) 0.0309(14) 0.0291(14) -0.0005(11) 0.0035(11) 0.0020(11) N9B 0.0333(15) 0.0379(15) 0.0387(16) -0.0020(12) 0.0091(12) 0.0010(12) N9C 0.0342(15) 0.0390(16) 0.0430(17) -0.0017(13) 0.0029(13) -0.0041(12) N17B 0.0380(16) 0.0377(15) 0.0369(15) -0.0065(12) 0.0075(12) -0.0051(12) N17D 0.0397(16) 0.0404(15) 0.0295(14) -0.0025(12) 0.0047(12) 0.0034(12) N17C 0.0326(15) 0.0339(14) 0.0367(15) -0.0003(12) 0.0043(12) -0.0016(12) N17A 0.0312(14) 0.0312(14) 0.0354(15) -0.0017(12) 0.0075(11) 0.0020(11) C1S 0.307(13) 0.200(10) 0.098(6) 0.009(6) 0.035(8) 0.030(10) C2S 0.150(6) 0.056(3) 0.088(4) 0.006(3) 0.054(4) 0.017(3) C2D 0.0296(17) 0.0340(17) 0.0358(18) 0.0021(14) 0.0056(14) 0.0025(13) C2A 0.042(2) 0.045(2) 0.068(3) 0.0060(19) 0.016(2) 0.0072(17) C2C 0.041(2) 0.063(3) 0.050(2) -0.013(2) -0.0099(18) 0.0063(19) C2B 0.0351(19) 0.047(2) 0.041(2) 0.0031(16) 0.0066(15) 0.0108(16) C3D 0.046(2) 0.048(2) 0.039(2) -0.0063(17) -0.0015(16) 0.0096(17) C3C 0.058(3) 0.095(4) 0.049(3) -0.025(3) -0.006(2) 0.006(3) C3A 0.060(3) 0.051(2) 0.092(4) -0.007(2) 0.021(3) 0.008(2) C3B 0.060(3) 0.075(3) 0.045(2) 0.000(2) 0.004(2) 0.021(2) C4A 0.053(3) 0.065(3) 0.114(4) 0.019(3) 0.022(3) 0.024(2) C4C 0.077(3) 0.095(4) 0.060(3) -0.035(3) -0.015(3) 0.015(3) C4B 0.093(4) 0.118(5) 0.065(3) -0.001(3) -0.016(3) 0.064(4) C4S 0.154(7) 0.101(6) 0.241(11) 0.039(6) 0.037(7) -0.030(5) C4D 0.059(3) 0.068(3) 0.041(2) -0.001(2) -0.0102(19) 0.022(2) C5B 0.135(5) 0.108(5) 0.085(4) -0.008(3) -0.027(4) 0.085(4) C5C 0.099(4) 0.062(3) 0.096(4) -0.041(3) -0.021(3) 0.005(3) C5A 0.052(3) 0.065(3) 0.086(4) 0.020(3) 0.008(3) 0.017(2) C5S 0.291(13) 0.130(7) 0.226(11) 0.038(7) -0.062(10) 0.104(8) C5D 0.071(3) 0.051(2) 0.058(3) 0.005(2) -0.003(2) 0.027(2) C6A 0.044(2) 0.058(2) 0.066(3) 0.013(2) 0.006(2) 0.0090(19) C6D 0.064(3) 0.039(2) 0.055(2) -0.0053(18) -0.002(2) 0.0216(18) C6C 0.079(3) 0.055(3) 0.077(3) -0.020(2) 0.004(3) -0.014(2) C6B 0.112(4) 0.076(3) 0.083(4) -0.017(3) -0.015(3) 0.054(3) C7A 0.0353(19) 0.045(2) 0.052(2) 0.0054(17) 0.0095(16) 0.0024(16) C7S 0.119(5) 0.094(4) 0.120(5) 0.038(4) 0.068(4) 0.034(4) C7B 0.050(2) 0.052(2) 0.052(2) 0.0013(18) -0.0011(19) 0.0221(18) C7C 0.044(2) 0.050(2) 0.052(2) -0.0158(18) 0.0007(18) -0.0015(17) C7D 0.0356(18) 0.0346(17) 0.0369(18) 0.0005(14) 0.0029(14) 0.0081(14) C8D 0.0399(19) 0.0307(17) 0.0361(18) -0.0046(14) 0.0067(15) 0.0047(14) C8A 0.0336(18) 0.045(2) 0.042(2) 0.0043(16) 0.0050(15) 0.0015(15) C8C 0.039(2) 0.045(2) 0.053(2) -0.0052(18) 0.0056(17) -0.0085(16) C8B 0.054(2) 0.041(2) 0.052(2) -0.0070(18) 0.0117(19) 0.0113(18) C9S 0.158(8) 0.177(8) 0.205(9) 0.122(7) 0.034(7) 0.051(6) C10B 0.0369(19) 0.0369(18) 0.043(2) -0.0093(15) 0.0096(15) -0.0007(15) C10C 0.0359(18) 0.0418(19) 0.0393(19) 0.0000(15) 0.0036(15) -0.0134(15) C10S 0.232(10) 0.089(5) 0.183(9) -0.015(6) 0.089(8) -0.009(6) C10D 0.0357(18) 0.0346(17) 0.0340(18) -0.0024(14) 0.0036(14) 0.0046(14) C10A 0.0291(17) 0.0400(18) 0.0377(19) 0.0017(14) 0.0068(14) 0.0017(14) C11C 0.0282(17) 0.050(2) 0.044(2) -0.0017(16) 0.0067(15) -0.0127(15) C11D 0.0383(19) 0.0384(19) 0.041(2) -0.0077(15) -0.0001(15) 0.0049(15) C11B 0.039(2) 0.052(2) 0.040(2) -0.0119(17) 0.0120(16) -0.0008(16) C11A 0.0303(18) 0.0412(19) 0.051(2) 0.0028(16) 0.0019(16) -0.0004(15) C12A 0.043(2) 0.047(2) 0.075(3) -0.002(2) 0.021(2) -0.0053(17) C12D 0.051(2) 0.047(2) 0.060(3) -0.0092(19) 0.006(2) 0.0008(18) C12C 0.040(2) 0.074(3) 0.044(2) -0.006(2) 0.0034(17) 0.0006(19) C12B 0.038(2) 0.083(3) 0.042(2) -0.004(2) 0.0058(17) -0.013(2) C13A 0.049(3) 0.066(3) 0.093(4) 0.019(3) 0.028(2) -0.003(2) C13B 0.052(3) 0.090(3) 0.051(2) -0.002(2) 0.015(2) -0.017(2) C13C 0.041(2) 0.086(3) 0.060(3) -0.004(2) 0.002(2) 0.012(2) C13D 0.058(3) 0.040(2) 0.078(3) -0.007(2) 0.005(2) -0.0032(19) C14D 0.067(3) 0.045(2) 0.067(3) -0.014(2) -0.016(2) 0.000(2) C14A 0.041(2) 0.046(2) 0.105(4) 0.020(2) 0.001(2) -0.0070(18) C14C 0.039(2) 0.090(3) 0.073(3) -0.007(3) 0.012(2) 0.015(2) C14B 0.052(2) 0.086(3) 0.039(2) 0.003(2) 0.0151(19) -0.005(2) C15C 0.054(3) 0.118(4) 0.060(3) -0.024(3) 0.018(2) 0.014(3) C15B 0.055(3) 0.117(4) 0.039(2) 0.002(2) -0.002(2) -0.017(3) C15A 0.065(3) 0.042(2) 0.089(3) -0.007(2) 0.000(3) -0.001(2) C15D 0.089(3) 0.064(3) 0.053(3) -0.027(2) 0.006(2) 0.012(3) C16D 0.072(3) 0.052(2) 0.053(2) -0.008(2) 0.015(2) 0.000(2) C16B 0.049(2) 0.088(3) 0.050(3) -0.006(2) 0.0050(19) -0.028(2) C16C 0.041(2) 0.082(3) 0.051(2) -0.006(2) 0.0113(18) 0.002(2) C16A 0.055(2) 0.043(2) 0.062(3) -0.0048(19) 0.005(2) -0.0020(18) C18D 0.041(2) 0.049(2) 0.0379(19) -0.0064(16) 0.0029(16) 0.0018(16) C18C 0.045(2) 0.0348(18) 0.043(2) 0.0025(15) 0.0080(16) -0.0068(16) C18B 0.051(2) 0.0356(19) 0.047(2) -0.0033(16) 0.0105(17) -0.0057(17) C18A 0.0406(19) 0.0361(18) 0.041(2) 0.0016(15) 0.0115(16) -0.0008(15) C19C 0.048(2) 0.044(2) 0.038(2) 0.0081(16) 0.0055(16) 0.0044(16) C19A 0.0390(19) 0.0364(18) 0.041(2) 0.0075(15) 0.0073(15) 0.0045(15) C19B 0.054(2) 0.049(2) 0.040(2) -0.0079(17) 0.0067(17) -0.0196(19) C19D 0.062(3) 0.050(2) 0.0340(19) 0.0028(17) 0.0101(18) 0.0056(19) C20A 0.048(2) 0.055(2) 0.062(3) 0.023(2) 0.007(2) -0.0068(19) C20D 0.064(3) 0.073(3) 0.050(3) 0.009(2) -0.001(2) 0.005(2) C20C 0.065(3) 0.068(3) 0.060(3) 0.026(2) 0.001(2) -0.006(2) C20B 0.094(4) 0.064(3) 0.056(3) -0.001(2) 0.004(2) -0.045(3) C21C 0.081(4) 0.095(4) 0.071(3) 0.043(3) -0.006(3) 0.007(3) C21D 0.098(4) 0.077(3) 0.049(3) 0.019(2) 0.002(3) 0.009(3) C21A 0.064(3) 0.067(3) 0.072(3) 0.040(2) 0.003(2) 0.002(2) C21B 0.079(4) 0.096(4) 0.079(4) -0.002(3) 0.013(3) -0.047(3) C22A 0.052(3) 0.078(3) 0.060(3) 0.030(2) -0.006(2) 0.008(2) C22D 0.115(5) 0.069(3) 0.054(3) 0.018(2) 0.029(3) 0.007(3) C22B 0.063(3) 0.138(5) 0.076(4) -0.019(3) 0.014(3) -0.066(4) C22C 0.058(3) 0.103(4) 0.046(3) 0.017(2) -0.014(2) 0.007(3) C23B 0.044(3) 0.112(4) 0.081(3) -0.031(3) 0.012(2) -0.031(3) C23C 0.040(2) 0.078(3) 0.043(2) 0.003(2) -0.0002(17) 0.003(2) C23A 0.037(2) 0.052(2) 0.052(2) 0.0131(18) 0.0012(17) -0.0017(17) C23D 0.077(3) 0.063(3) 0.062(3) 0.004(2) 0.026(2) -0.008(2) C24B 0.043(2) 0.075(3) 0.052(2) -0.022(2) 0.0138(18) -0.022(2) C24A 0.0382(18) 0.0326(17) 0.0315(17) 0.0017(14) 0.0086(14) 0.0055(14) C24C 0.0383(19) 0.044(2) 0.0365(19) -0.0026(15) 0.0070(15) 0.0054(15) C24D 0.060(3) 0.051(2) 0.041(2) -0.0013(17) 0.0189(19) 0.0024(19) _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 O1D 1.895(2) . ? Co1 O1 1.901(2) . ? Co1 O25A 1.905(2) . ? Co1 O2 1.913(2) . ? Co1 N9D 1.944(2) . ? Co1 N17A 1.964(3) . ? Co2 O1A 1.894(3) . ? Co2 O25D 1.906(3) . ? Co2 N9A 1.998(3) . ? Co2 N17D 2.001(3) . ? Co3 O1C 1.904(2) . ? Co3 O2 1.994(2) . ? Co3 O1B 1.999(2) . ? Co3 N9C 2.045(3) . ? Co3 O25A 2.269(2) . ? Co3 Co4 2.9170(7) . ? Co4 O25C 2.036(2) . ? Co4 O1B 2.037(2) . ? Co4 N17C 2.116(3) . ? Co4 N9B 2.117(3) . ? Co4 O2 2.179(2) . ? Co4 O1 2.202(2) . ? Co4 Co5 2.9251(7) . ? Co5 O25B 1.900(3) . ? Co5 O25C 1.994(2) . ? Co5 O1 1.995(2) . ? Co5 N17B 2.037(3) . ? Co5 O1D 2.255(2) . ? ClD C14D 1.751(4) . ? ClB C14B 1.747(4) . ? ClA C14A 1.746(4) . ? ClC C14C 1.756(4) . ? Cl1S C1S 1.605(10) . ? Cl2S C1S 1.930(12) . ? O1B C2B 1.327(4) . ? O1A C2A 1.330(5) . ? O1D C2D 1.324(4) . ? O1S C2S 1.232(7) . ? O1C C2C 1.325(5) . ? O6S C7S 1.238(7) . ? O25C C24C 1.340(4) . ? O25B C24B 1.320(5) . ? O25D C24D 1.307(5) . ? O25A C24A 1.323(4) . ? N3S C2S 1.329(7) . ? N3S C5S 1.474(9) . ? N3S C4S 1.517(9) . ? N8S C7S 1.338(7) . ? N8S C9S 1.450(9) . ? N8S C10S 1.451(10) . ? N9A C8A 1.311(4) . ? N9A C10A 1.476(4) . ? N9D C8D 1.294(4) . ? N9D C10D 1.489(4) . ? N9B C8B 1.290(4) . ? N9B C10B 1.476(4) . ? N9C C8C 1.294(4) . ? N9C C10C 1.473(4) . ? N17B C18B 1.290(4) . ? N17B C10B 1.477(4) . ? N17D C18D 1.294(4) . ? N17D C10D 1.463(4) . ? N17C C18C 1.298(4) . ? N17C C10C 1.484(4) . ? N17A C18A 1.285(4) . ? N17A C10A 1.497(4) . ? C2D C3D 1.402(4) . ? C2D C7D 1.410(4) . ? C2A C3A 1.411(5) . ? C2A C7A 1.412(5) . ? C2C C7C 1.404(6) . ? C2C C3C 1.410(5) . ? C2B C3B 1.403(5) . ? C2B C7B 1.409(5) . ? C3D C4D 1.383(5) . ? C3C C4C 1.372(7) . ? C3A C4A 1.363(6) . ? C3B C4B 1.369(6) . ? C4A C5A 1.378(7) . ? C4C C5C 1.378(8) . ? C4B C5B 1.404(7) . ? C4D C5D 1.381(6) . ? C5B C6B 1.360(7) . ? C5C C6C 1.397(7) . ? C5A C6A 1.356(6) . ? C5D C6D 1.369(5) . ? C6A C7A 1.418(5) . ? C6D C7D 1.408(4) . ? C6C C7C 1.416(5) . ? C6B C7B 1.410(5) . ? C7A C8A 1.426(5) . ? C7B C8B 1.438(5) . ? C7C C8C 1.442(5) . ? C7D C8D 1.432(4) . ? C10B C11B 1.526(5) . ? C10C C11C 1.530(5) . ? C10D C11D 1.522(4) . ? C10A C11A 1.524(5) . ? C11C C12C 1.380(5) . ? C11C C16C 1.391(5) . ? C11D C16D 1.368(5) . ? C11D C12D 1.383(5) . ? C11B C16B 1.378(5) . ? C11B C12B 1.382(5) . ? C11A C12A 1.379(5) . ? C11A C16A 1.403(5) . ? C12A C13A 1.389(5) . ? C12D C13D 1.385(5) . ? C12C C13C 1.385(6) . ? C12B C13B 1.384(6) . ? C13A C14A 1.368(6) . ? C13B C14B 1.374(6) . ? C13C C14C 1.351(6) . ? C13D C14D 1.355(6) . ? C14D C15D 1.360(7) . ? C14A C15A 1.368(7) . ? C14C C15C 1.370(6) . ? C14B C15B 1.363(6) . ? C15C C16C 1.389(6) . ? C15B C16B 1.378(6) . ? C15A C16A 1.404(6) . ? C15D C16D 1.423(6) . ? C18D C19D 1.432(5) . ? C18C C19C 1.443(5) . ? C18B C19B 1.437(5) . ? C18A C19A 1.429(5) . ? C19C C20C 1.402(5) . ? C19C C24C 1.423(5) . ? C19A C24A 1.405(5) . ? C19A C20A 1.405(5) . ? C19B C24B 1.402(6) . ? C19B C20B 1.421(5) . ? C19D C24D 1.405(5) . ? C19D C20D 1.423(5) . ? C20A C21A 1.369(5) . ? C20D C21D 1.353(6) . ? C20C C21C 1.367(6) . ? C20B C21B 1.360(7) . ? C21C C22C 1.360(7) . ? C21D C22D 1.398(7) . ? C21A C22A 1.380(6) . ? C21B C22B 1.365(8) . ? C22A C23A 1.373(5) . ? C22D C23D 1.355(6) . ? C22B C23B 1.405(7) . ? C22C C23C 1.395(6) . ? C23B C24B 1.407(5) . ? C23C C24C 1.383(5) . ? C23A C24A 1.390(5) . ? C23D C24D 1.418(5) . ? 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 Co1 O1 80.67(9) . . ? O1D Co1 O25A 170.89(9) . . ? O1 Co1 O25A 91.68(10) . . ? O1D Co1 O2 93.73(9) . . ? O1 Co1 O2 83.49(10) . . ? O25A Co1 O2 80.41(9) . . ? O1D Co1 N9D 93.69(10) . . ? O1 Co1 N9D 170.26(11) . . ? O25A Co1 N9D 93.18(10) . . ? O2 Co1 N9D 89.00(10) . . ? O1D Co1 N17A 91.80(10) . . ? O1 Co1 N17A 91.96(10) . . ? O25A Co1 N17A 93.40(10) . . ? O2 Co1 N17A 172.17(10) . . ? N9D Co1 N17A 96.17(10) . . ? O1A Co2 O25D 121.71(12) . . ? O1A Co2 N9A 95.61(11) . . ? O25D Co2 N9A 113.41(12) . . ? O1A Co2 N17D 114.67(12) . . ? O25D Co2 N17D 94.72(11) . . ? N9A Co2 N17D 118.58(11) . . ? O1C Co3 O2 127.86(11) . . ? O1C Co3 O1B 139.21(11) . . ? O2 Co3 O1B 90.04(9) . . ? O1C Co3 N9C 94.62(12) . . ? O2 Co3 N9C 99.10(10) . . ? O1B Co3 N9C 93.14(10) . . ? O1C Co3 O25A 91.69(10) . . ? O2 Co3 O25A 70.29(8) . . ? O1B Co3 O25A 87.63(9) . . ? N9C Co3 O25A 169.37(9) . . ? O1C Co3 Co4 176.16(9) . . ? O2 Co3 Co4 48.30(6) . . ? O1B Co3 Co4 44.22(6) . . ? N9C Co3 Co4 86.53(8) . . ? O25A Co3 Co4 86.64(6) . . ? O25C Co4 O1B 174.18(9) . . ? O25C Co4 N17C 89.25(9) . . ? O1B Co4 N17C 94.31(10) . . ? O25C Co4 N9B 93.77(10) . . ? O1B Co4 N9B 88.61(10) . . ? N17C Co4 N9B 118.18(10) . . ? O25C Co4 O2 91.71(8) . . ? O1B Co4 O2 84.08(8) . . ? N17C Co4 O2 84.17(9) . . ? N9B Co4 O2 157.01(9) . . ? O25C Co4 O1 83.60(9) . . ? O1B Co4 O1 91.20(9) . . ? N17C Co4 O1 153.71(9) . . ? N9B Co4 O1 87.60(9) . . ? O2 Co4 O1 70.84(8) . . ? O25C Co4 Co3 133.64(7) . . ? O1B Co4 Co3 43.21(6) . . ? N17C Co4 Co3 78.25(7) . . ? N9B Co4 Co3 131.55(8) . . ? O2 Co4 Co3 43.11(5) . . ? O1 Co4 Co3 88.49(6) . . ? O25C Co4 Co5 42.90(6) . . ? O1B Co4 Co5 132.71(7) . . ? N17C Co4 Co5 131.45(7) . . ? N9B Co4 Co5 80.12(7) . . ? O2 Co4 Co5 88.90(6) . . ? O1 Co4 Co5 42.97(6) . . ? Co3 Co4 Co5 124.91(2) . . ? O25B Co5 O25C 139.58(12) . . ? O25B Co5 O1 128.35(12) . . ? O25C Co5 O1 90.31(9) . . ? O25B Co5 N17B 93.11(11) . . ? O25C Co5 N17B 94.35(10) . . ? O1 Co5 N17B 95.56(10) . . ? O25B Co5 O1D 94.08(10) . . ? O25C Co5 O1D 88.13(9) . . ? O1 Co5 O1D 70.34(8) . . ? N17B Co5 O1D 165.72(10) . . ? O25B Co5 Co4 176.12(10) . . ? O25C Co5 Co4 44.04(6) . . ? O1 Co5 Co4 48.81(7) . . ? N17B Co5 Co4 84.83(8) . . ? O1D Co5 Co4 87.24(6) . . ? C2B O1B Co3 135.8(2) . . ? C2B O1B Co4 131.6(2) . . ? Co3 O1B Co4 92.56(9) . . ? C2A O1A Co2 125.6(2) . . ? Co1 O1 Co5 109.34(11) . . ? Co1 O1 Co4 102.61(11) . . ? Co5 O1 Co4 88.23(9) . . ? C2D O1D Co1 128.6(2) . . ? C2D O1D Co5 128.45(19) . . ? Co1 O1D Co5 99.62(9) . . ? C2C O1C Co3 125.0(2) . . ? Co1 O2 Co3 109.74(10) . . ? Co1 O2 Co4 103.06(9) . . ? Co3 O2 Co4 88.59(8) . . ? C24C O25C Co5 135.6(2) . . ? C24C O25C Co4 131.0(2) . . ? Co5 O25C Co4 93.06(9) . . ? C24B O25B Co5 125.0(3) . . ? C24D O25D Co2 127.0(2) . . ? C24A O25A Co1 128.5(2) . . ? C24A O25A Co3 129.17(19) . . ? Co1 O25A Co3 99.56(9) . . ? C2S N3S C5S 119.7(8) . . ? C2S N3S C4S 119.5(6) . . ? C5S N3S C4S 120.5(7) . . ? C7S N8S C9S 119.5(8) . . ? C7S N8S C10S 118.5(7) . . ? C9S N8S C10S 122.0(7) . . ? C8A N9A C10A 115.8(3) . . ? C8A N9A Co2 120.8(2) . . ? C10A N9A Co2 123.3(2) . . ? C8D N9D C10D 117.7(3) . . ? C8D N9D Co1 123.8(2) . . ? C10D N9D Co1 118.43(19) . . ? C8B N9B C10B 113.9(3) . . ? C8B N9B Co4 123.2(2) . . ? C10B N9B Co4 121.7(2) . . ? C8C N9C C10C 116.3(3) . . ? C8C N9C Co3 120.5(3) . . ? C10C N9C Co3 122.6(2) . . ? C18B N17B C10B 116.1(3) . . ? C18B N17B Co5 120.8(2) . . ? C10B N17B Co5 122.8(2) . . ? C18D N17D C10D 116.4(3) . . ? C18D N17D Co2 121.7(2) . . ? C10D N17D Co2 121.8(2) . . ? C18C N17C C10C 113.6(3) . . ? C18C N17C Co4 123.4(2) . . ? C10C N17C Co4 122.4(2) . . ? C18A N17A C10A 117.4(3) . . ? C18A N17A Co1 122.5(2) . . ? C10A N17A Co1 120.1(2) . . ? Cl1S C1S Cl2S 108.0(5) . . ? O1S C2S N3S 119.8(6) . . ? O1D C2D C3D 118.4(3) . . ? O1D C2D C7D 122.3(3) . . ? C3D C2D C7D 119.3(3) . . ? O1A C2A C3A 118.9(4) . . ? O1A C2A C7A 124.0(3) . . ? C3A C2A C7A 117.0(4) . . ? O1C C2C C7C 124.2(3) . . ? O1C C2C C3C 117.8(4) . . ? C7C C2C C3C 117.9(4) . . ? O1B C2B C3B 120.1(3) . . ? O1B C2B C7B 121.3(3) . . ? C3B C2B C7B 118.6(3) . . ? C4D C3D C2D 120.5(3) . . ? C4C C3C C2C 121.5(5) . . ? C4A C3A C2A 121.3(5) . . ? C4B C3B C2B 121.4(4) . . ? C3A C4A C5A 122.0(4) . . ? C3C C4C C5C 121.1(5) . . ? C3B C4B C5B 120.2(5) . . ? C5D C4D C3D 120.6(4) . . ? C6B C5B C4B 119.1(5) . . ? C4C C5C C6C 119.4(5) . . ? C6A C5A C4A 118.4(4) . . ? C6D C5D C4D 119.5(4) . . ? C5A C6A C7A 121.9(5) . . ? C5D C6D C7D 121.9(3) . . ? C5C C6C C7C 120.1(5) . . ? C5B C6B C7B 122.1(5) . . ? C2A C7A C6A 119.3(4) . . ? C2A C7A C8A 124.4(3) . . ? C6A C7A C8A 116.2(4) . . ? O6S C7S N8S 122.5(7) . . ? C2B C7B C6B 118.6(4) . . ? C2B C7B C8B 125.6(3) . . ? C6B C7B C8B 115.8(4) . . ? C2C C7C C6C 120.0(4) . . ? C2C C7C C8C 125.7(3) . . ? C6C C7C C8C 114.3(4) . . ? C6D C7D C2D 118.1(3) . . ? C6D C7D C8D 118.2(3) . . ? C2D C7D C8D 123.6(3) . . ? N9D C8D C7D 127.1(3) . . ? N9A C8A C7A 127.6(3) . . ? N9C C8C C7C 126.2(4) . . ? N9B C8B C7B 129.3(3) . . ? N9B C10B N17B 107.8(2) . . ? N9B C10B C11B 114.0(3) . . ? N17B C10B C11B 108.7(3) . . ? N9C C10C N17C 108.3(3) . . ? N9C C10C C11C 113.5(3) . . ? N17C C10C C11C 109.8(3) . . ? N17D C10D N9D 106.0(2) . . ? N17D C10D C11D 114.2(3) . . ? N9D C10D C11D 115.2(3) . . ? N9A C10A N17A 106.0(2) . . ? N9A C10A C11A 111.9(3) . . ? N17A C10A C11A 114.2(3) . . ? C12C C11C C16C 119.5(4) . . ? C12C C11C C10C 123.0(3) . . ? C16C C11C C10C 117.4(3) . . ? C16D C11D C12D 119.3(4) . . ? C16D C11D C10D 122.4(3) . . ? C12D C11D C10D 118.1(3) . . ? C16B C11B C12B 117.7(4) . . ? C16B C11B C10B 120.1(3) . . ? C12B C11B C10B 122.1(3) . . ? C12A C11A C16A 119.6(3) . . ? C12A C11A C10A 122.9(3) . . ? C16A C11A C10A 117.6(3) . . ? C11A C12A C13A 120.6(4) . . ? C11D C12D C13D 121.4(4) . . ? C11C C12C C13C 120.5(4) . . ? C11B C12B C13B 121.7(4) . . ? C14A C13A C12A 119.4(4) . . ? C14B C13B C12B 118.5(4) . . ? C14C C13C C12C 119.3(4) . . ? C14D C13D C12D 118.5(4) . . ? C13D C14D C15D 122.3(4) . . ? C13D C14D ClD 118.9(4) . . ? C15D C14D ClD 118.9(4) . . ? C15A C14A C13A 121.7(4) . . ? C15A C14A ClA 119.2(4) . . ? C13A C14A ClA 119.1(4) . . ? C13C C14C C15C 121.6(4) . . ? C13C C14C ClC 119.3(4) . . ? C15C C14C ClC 119.1(4) . . ? C15B C14B C13B 121.1(4) . . ? C15B C14B ClB 119.4(3) . . ? C13B C14B ClB 119.4(3) . . ? C14C C15C C16C 119.7(4) . . ? C14B C15B C16B 119.4(4) . . ? C14A C15A C16A 119.5(4) . . ? C14D C15D C16D 119.0(4) . . ? C11D C16D C15D 119.4(4) . . ? C11B C16B C15B 121.4(4) . . ? C15C C16C C11C 119.2(4) . . ? C11A C16A C15A 119.3(4) . . ? N17D C18D C19D 127.8(3) . . ? N17C C18C C19C 128.7(3) . . ? N17B C18B C19B 125.1(3) . . ? N17A C18A C19A 128.5(3) . . ? C20C C19C C24C 118.6(3) . . ? C20C C19C C18C 115.5(3) . . ? C24C C19C C18C 125.9(3) . . ? C24A C19A C20A 119.0(3) . . ? C24A C19A C18A 123.4(3) . . ? C20A C19A C18A 117.6(3) . . ? C24B C19B C20B 119.7(4) . . ? C24B C19B C18B 124.8(3) . . ? C20B C19B C18B 115.1(4) . . ? C24D C19D C20D 119.1(4) . . ? C24D C19D C18D 123.9(3) . . ? C20D C19D C18D 116.8(4) . . ? C21A C20A C19A 121.7(4) . . ? C21D C20D C19D 122.2(5) . . ? C21C C20C C19C 121.8(4) . . ? C21B C20B C19B 121.9(6) . . ? C22C C21C C20C 119.5(4) . . ? C20D C21D C22D 118.6(5) . . ? C20A C21A C22A 118.6(4) . . ? C20B C21B C22B 118.4(5) . . ? C23A C22A C21A 121.0(4) . . ? C23D C22D C21D 120.8(4) . . ? C21B C22B C23B 122.2(5) . . ? C21C C22C C23C 120.7(4) . . ? C22B C23B C24B 119.9(5) . . ? C24C C23C C22C 121.2(4) . . ? C22A C23A C24A 121.3(4) . . ? C22D C23D C24D 122.3(5) . . ? O25B C24B C19B 124.5(3) . . ? O25B C24B C23B 117.9(4) . . ? C19B C24B C23B 117.7(4) . . ? O25A C24A C23A 119.5(3) . . ? O25A C24A C19A 122.3(3) . . ? C23A C24A C19A 118.2(3) . . ? O25C C24C C23C 120.7(3) . . ? O25C C24C C19C 121.2(3) . . ? C23C C24C C19C 118.1(3) . . ? O25D C24D C19D 124.6(3) . . ? O25D C24D C23D 118.4(4) . . ? C19D C24D C23D 116.9(4) . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 29.46 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 1.091 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.072