data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Xian-He Bu' _publ_contact_author_address ; Department of Chemistry Nankai University Tianjin 300071 CHINA ; _publ_contact_author_email BUXH@NANKAI.EDU.CN loop_ _publ_author_name 'Xian-He Bu.' 'Qiang Chen.' 'Tong-Liang Hu.' 'Qinhe Pan.' 'Wei-Chao Song.' #----end----- data_Zn-1 _database_code_depnum_ccdc_archive 'CCDC 764683' #TrackingRef 'Zn-1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H34 Co N6 O19 Zn2' _chemical_formula_weight 768.13 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9116(18) _cell_length_b 9.2445(18) _cell_length_c 18.724(4) _cell_angle_alpha 103.92(3) _cell_angle_beta 92.14(3) _cell_angle_gamma 109.46(3) _cell_volume 1400.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11268 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.3 _exptl_crystal_description plate-shaped _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 786 _exptl_absorpt_coefficient_mu 2.377 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 SCX-MINI _diffrn_measurement_method multi-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14301 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 27.37 _reflns_number_total 6251 _reflns_number_gt 3833 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution DirectMethod _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ? _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^)+(0.0381P)^2^+3.1723P] 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 6251 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1445 _refine_ls_R_factor_gt 0.0811 _refine_ls_wR_factor_ref 0.1491 _refine_ls_wR_factor_gt 0.1298 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn -0.51378(12) -0.21685(10) -0.42054(5) 0.0552(3) Uani 1 1 d . . . Zn2 Zn -0.41462(9) -0.15923(8) -0.12418(4) 0.0310(2) Uani 1 1 d . . . Co1 Co -0.09870(10) -0.31274(10) 0.22581(5) 0.0337(2) Uani 1 1 d . . . O1 O -0.6286(7) -0.6392(6) -0.5777(3) 0.0672(16) Uani 1 1 d . . . O2 O -0.6464(7) -0.4125(6) -0.5077(3) 0.0687(17) Uani 1 1 d . . . O3 O -0.6437(6) -0.0798(6) -0.4443(3) 0.0568(14) Uani 1 1 d . . . O4 O -0.6383(7) 0.0941(6) -0.5109(3) 0.0616(15) Uani 1 1 d . . . O5 O -0.6495(6) -0.2844(5) -0.3359(3) 0.0526(13) Uani 1 1 d . . . O6 O -0.6198(5) -0.2333(5) -0.2119(2) 0.0385(11) Uani 1 1 d . . . O7 O -0.3554(6) -0.0593(5) -0.3260(3) 0.0534(14) Uani 1 1 d . . . O8 O -0.3046(5) -0.0633(5) -0.2088(2) 0.0411(11) Uani 1 1 d . . . O9 O -0.4381(5) -0.3987(5) -0.1725(2) 0.0409(11) Uani 1 1 d . . . O10 O -0.2901(6) -0.5555(6) -0.1870(3) 0.0727(18) Uani 1 1 d . . . O11 O -0.1978(5) -0.1611(5) -0.0803(3) 0.0483(13) Uani 1 1 d . . . O12 O -0.0292(6) -0.2953(6) -0.1089(3) 0.0614(15) Uani 1 1 d . . . O13 O -0.3816(5) 0.0760(5) -0.0647(2) 0.0370(11) Uani 1 1 d . . . O14 O -0.4411(5) 0.2059(5) 0.0419(2) 0.0367(11) Uani 1 1 d . . . N1 N -0.2893(7) -0.3632(7) 0.2801(3) 0.0527(16) Uani 1 1 d . . . H1A H -0.3710 -0.4458 0.2510 0.080 Uiso 1 1 calc . . . H1B H -0.2654 -0.3900 0.3210 0.080 Uiso 1 1 calc . . . N2 N -0.1428(7) -0.1189(7) 0.2226(4) 0.0565(17) Uani 1 1 d . . . H2A H -0.0683 -0.0333 0.2540 0.080 Uiso 1 1 calc . . . H2B H -0.1375 -0.1060 0.1765 0.080 Uiso 1 1 calc . . . N3 N -0.2307(7) -0.4358(7) 0.1297(3) 0.0486(16) Uani 1 1 d . . . H3A H -0.2871 -0.5352 0.1319 0.080 Uiso 1 1 calc . . . H3B H -0.3007 -0.3898 0.1199 0.080 Uiso 1 1 calc . . . N4 N 0.0813(6) -0.2631(6) 0.1676(3) 0.0427(14) Uani 1 1 d . . . H4A H 0.1449 -0.1603 0.1856 0.080 Uiso 1 1 calc . . . H4B H 0.1402 -0.3241 0.1710 0.080 Uiso 1 1 calc . . . N5 N 0.0480(6) -0.2033(6) 0.3205(3) 0.0442(14) Uani 1 1 d . . . H5A H 0.1166 -0.1087 0.3177 0.080 Uiso 1 1 calc . . . H5B H -0.0092 -0.1856 0.3581 0.080 Uiso 1 1 calc . . . N6 N -0.0600(6) -0.5057(6) 0.2374(3) 0.0437(15) Uani 1 1 d . . . H6A H -0.1543 -0.5866 0.2310 0.080 Uiso 1 1 calc . . . H6B H -0.0008 -0.5346 0.2026 0.080 Uiso 1 1 calc . . . C1 C -0.3369(10) -0.2179(12) 0.3013(5) 0.077(3) Uani 1 1 d . . . H1C H -0.4497 -0.2500 0.3077 0.080 Uiso 1 1 calc . . . H1D H -0.2755 -0.1482 0.3481 0.080 Uiso 1 1 calc . . . C2 C -0.3079(13) -0.1321(13) 0.2442(7) 0.098(4) Uani 1 1 d . . . H2C H -0.3131 -0.0268 0.2631 0.080 Uiso 1 1 calc . . . H2D H -0.3886 -0.1891 0.2013 0.080 Uiso 1 1 calc . . . C3 C -0.1271(9) -0.4435(9) 0.0688(4) 0.052(2) Uani 1 1 d . . . H3C H -0.0939 -0.5350 0.0635 0.080 Uiso 1 1 calc . . . H3D H -0.1868 -0.4548 0.0221 0.080 Uiso 1 1 calc . . . C4 C 0.0172(9) -0.2939(9) 0.0873(4) 0.0507(19) Uani 1 1 d . . . H4C H -0.0121 -0.2056 0.0805 0.080 Uiso 1 1 calc . . . H4D H 0.0979 -0.3064 0.0555 0.080 Uiso 1 1 calc . . . C5 C 0.1387(9) -0.3035(9) 0.3347(4) 0.0517(19) Uani 1 1 d . . . H5C H 0.1815 -0.2712 0.3867 0.080 Uiso 1 1 calc . . . H5D H 0.2276 -0.2920 0.3055 0.080 Uiso 1 1 calc . . . C6 C 0.0268(10) -0.4727(9) 0.3136(4) 0.060(2) Uani 1 1 d . . . H6C H -0.0494 -0.4893 0.3491 0.080 Uiso 1 1 calc . . . H6D H 0.0864 -0.5436 0.3129 0.080 Uiso 1 1 calc . . . C7 C -0.5807(11) -0.5150(9) -0.5239(4) 0.061(2) Uani 1 1 d . . . C8 C -0.5810(9) 0.0043(8) -0.4871(4) 0.0491(19) Uani 1 1 d . . . C9 C -0.5717(8) -0.2201(7) -0.2727(4) 0.0348(15) Uani 1 1 d . . . C10 C -0.3937(8) -0.1036(7) -0.2685(4) 0.0357(16) Uani 1 1 d . . . C11 C -0.3096(8) -0.4273(7) -0.1619(4) 0.0386(16) Uani 1 1 d . . . C12 C -0.1653(8) -0.2827(8) -0.1130(4) 0.0425(17) Uani 1 1 d . . . C13 C -0.4488(7) 0.0815(7) -0.0071(4) 0.0317(15) Uani 1 1 d . . . O1W O -0.9677(12) -0.3535(15) -0.4751(6) 0.190(5) Uani 1 1 d . . . O2W O -0.4904(11) -0.3736(14) 0.0588(6) 0.188(5) Uani 1 1 d . . . O3W O -0.1226(11) -0.2059(12) -0.5465(4) 0.151(4) Uani 1 1 d . . . O4W O -0.0406(11) -0.1623(9) -0.3507(4) 0.137(3) Uani 1 1 d . . . O5W O 0.1942(6) 0.0243(6) -0.0759(3) 0.0572(14) 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 Zn1 0.0911(7) 0.0319(5) 0.0333(5) 0.0073(4) 0.0036(5) 0.0114(5) Zn2 0.0304(4) 0.0278(4) 0.0340(4) 0.0051(3) 0.0091(3) 0.0107(3) Co1 0.0256(5) 0.0291(5) 0.0403(5) 0.0003(4) 0.0071(4) 0.0080(4) O1 0.113(5) 0.037(3) 0.039(3) -0.001(3) -0.018(3) 0.022(3) O2 0.108(5) 0.037(3) 0.050(3) -0.002(3) -0.017(3) 0.023(3) O3 0.084(4) 0.046(3) 0.050(3) 0.024(3) 0.024(3) 0.027(3) O4 0.096(4) 0.056(3) 0.052(3) 0.028(3) 0.032(3) 0.040(3) O5 0.056(3) 0.042(3) 0.040(3) 0.014(2) -0.005(3) -0.007(2) O6 0.028(2) 0.045(3) 0.039(3) 0.014(2) 0.008(2) 0.007(2) O7 0.067(3) 0.036(3) 0.036(3) 0.009(2) 0.011(2) -0.009(2) O8 0.041(3) 0.035(3) 0.032(3) 0.006(2) 0.008(2) -0.004(2) O9 0.036(3) 0.030(2) 0.052(3) 0.001(2) 0.000(2) 0.014(2) O10 0.048(3) 0.037(3) 0.124(5) -0.007(3) 0.004(3) 0.025(3) O11 0.040(3) 0.047(3) 0.051(3) -0.007(2) -0.002(2) 0.022(2) O12 0.036(3) 0.064(4) 0.078(4) -0.006(3) -0.005(3) 0.028(3) O13 0.040(3) 0.032(2) 0.041(3) 0.013(2) 0.018(2) 0.013(2) O14 0.042(3) 0.024(2) 0.041(3) 0.002(2) 0.013(2) 0.012(2) N1 0.041(4) 0.059(4) 0.047(4) 0.001(3) 0.014(3) 0.012(3) N2 0.057(4) 0.046(4) 0.069(4) 0.006(3) 0.006(3) 0.029(3) N3 0.039(3) 0.043(3) 0.050(4) -0.001(3) 0.004(3) 0.008(3) N4 0.034(3) 0.032(3) 0.053(4) 0.009(3) 0.006(3) 0.002(3) N5 0.037(3) 0.040(3) 0.053(4) 0.010(3) 0.010(3) 0.011(3) N6 0.034(3) 0.032(3) 0.063(4) 0.012(3) 0.014(3) 0.008(3) C1 0.052(5) 0.081(7) 0.088(7) -0.012(6) 0.024(5) 0.032(5) C2 0.094(8) 0.092(8) 0.147(11) 0.041(8) 0.042(8) 0.073(7) C3 0.046(5) 0.058(5) 0.040(4) -0.002(4) 0.007(4) 0.013(4) C4 0.050(5) 0.051(5) 0.040(4) 0.006(4) 0.010(4) 0.009(4) C5 0.043(4) 0.052(5) 0.059(5) 0.020(4) 0.000(4) 0.014(4) C6 0.069(6) 0.049(5) 0.061(5) 0.026(4) 0.000(4) 0.014(4) C7 0.105(7) 0.033(4) 0.029(4) 0.007(4) -0.006(4) 0.009(5) C8 0.082(6) 0.031(4) 0.031(4) 0.000(3) 0.013(4) 0.021(4) C9 0.042(4) 0.023(3) 0.035(4) 0.010(3) -0.002(3) 0.006(3) C10 0.045(4) 0.024(3) 0.028(4) 0.005(3) 0.009(3) 0.000(3) C11 0.039(4) 0.029(4) 0.048(4) 0.008(3) 0.012(3) 0.013(3) C12 0.038(4) 0.042(4) 0.045(4) 0.002(3) 0.006(3) 0.017(3) C13 0.026(3) 0.030(3) 0.041(4) 0.010(3) 0.004(3) 0.011(3) O1W 0.135(8) 0.334(15) 0.183(10) 0.139(11) 0.067(7) 0.131(10) O2W 0.134(7) 0.299(14) 0.237(11) 0.206(11) 0.048(8) 0.113(9) O3W 0.179(9) 0.239(11) 0.123(7) 0.109(7) 0.099(6) 0.136(8) O4W 0.170(8) 0.090(5) 0.127(7) -0.036(5) -0.049(6) 0.069(5) O5W 0.058(3) 0.053(3) 0.059(3) 0.016(3) 0.001(3) 0.018(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 Zn1 O2 2.084(5) . ? Zn1 O3 2.087(5) . ? Zn1 O7 2.110(5) . ? Zn1 O5 2.116(5) . ? Zn1 O1 2.119(6) 2_444 ? Zn1 O4 2.140(5) 2_454 ? Zn2 O14 2.076(4) 2_455 ? Zn2 O11 2.078(4) . ? Zn2 O13 2.107(4) . ? Zn2 O8 2.115(4) . ? Zn2 O9 2.116(4) . ? Zn2 O6 2.215(4) . ? Co1 N4 1.963(5) . ? Co1 N3 1.971(6) . ? Co1 N2 1.972(6) . ? Co1 N6 1.984(6) . ? Co1 N5 1.990(6) . ? Co1 N1 1.991(6) . ? O1 C7 1.264(8) . ? O1 Zn1 2.119(6) 2_444 ? O2 C7 1.256(9) . ? O3 C8 1.266(8) . ? O4 C8 1.262(9) . ? O4 Zn1 2.140(5) 2_454 ? O5 C9 1.250(7) . ? O6 C9 1.251(7) . ? O7 C10 1.261(7) . ? O8 C10 1.246(7) . ? O9 C11 1.277(7) . ? O10 C11 1.237(7) . ? O11 C12 1.274(7) . ? O12 C12 1.257(8) . ? O13 C13 1.252(7) . ? O14 C13 1.267(7) . ? O14 Zn2 2.076(4) 2_455 ? N1 C1 1.509(10) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.514(11) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C3 1.497(9) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C4 1.512(9) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C5 1.477(9) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 C6 1.510(9) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? C1 C2 1.460(13) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.495(10) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 C6 1.493(10) . ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 C7 1.570(17) 2_444 ? C8 C8 1.560(15) 2_454 ? C9 C10 1.579(9) . ? C11 C12 1.567(9) . ? C13 C13 1.571(12) 2_455 ? 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 O2 Zn1 O3 92.4(2) . . ? O2 Zn1 O7 165.7(2) . . ? O3 Zn1 O7 101.7(2) . . ? O2 Zn1 O5 97.3(2) . . ? O3 Zn1 O5 94.2(2) . . ? O7 Zn1 O5 79.98(18) . . ? O2 Zn1 O1 80.3(2) . 2_444 ? O3 Zn1 O1 166.67(19) . 2_444 ? O7 Zn1 O1 86.1(2) . 2_444 ? O5 Zn1 O1 97.7(2) . 2_444 ? O2 Zn1 O4 94.9(2) . 2_454 ? O3 Zn1 O4 79.9(2) . 2_454 ? O7 Zn1 O4 89.4(2) . 2_454 ? O5 Zn1 O4 166.64(19) . 2_454 ? O1 Zn1 O4 89.6(2) 2_444 2_454 ? O14 Zn2 O11 102.32(19) 2_455 . ? O14 Zn2 O13 80.56(16) 2_455 . ? O11 Zn2 O13 96.11(18) . . ? O14 Zn2 O8 162.60(17) 2_455 . ? O11 Zn2 O8 91.12(19) . . ? O13 Zn2 O8 87.13(16) . . ? O14 Zn2 O9 95.92(17) 2_455 . ? O11 Zn2 O9 79.26(18) . . ? O13 Zn2 O9 173.53(18) . . ? O8 Zn2 O9 97.43(17) . . ? O14 Zn2 O6 94.11(16) 2_455 . ? O11 Zn2 O6 153.96(17) . . ? O13 Zn2 O6 106.51(17) . . ? O8 Zn2 O6 77.58(16) . . ? O9 Zn2 O6 79.06(17) . . ? N4 Co1 N3 85.5(2) . . ? N4 Co1 N2 92.6(2) . . ? N3 Co1 N2 92.7(3) . . ? N4 Co1 N6 91.4(2) . . ? N3 Co1 N6 90.2(2) . . ? N2 Co1 N6 175.3(3) . . ? N4 Co1 N5 91.4(2) . . ? N3 Co1 N5 174.0(2) . . ? N2 Co1 N5 92.6(2) . . ? N6 Co1 N5 84.7(2) . . ? N4 Co1 N1 176.8(3) . . ? N3 Co1 N1 91.8(2) . . ? N2 Co1 N1 85.8(3) . . ? N6 Co1 N1 90.4(2) . . ? N5 Co1 N1 91.5(2) . . ? C7 O1 Zn1 112.6(5) . 2_444 ? C7 O2 Zn1 112.8(5) . . ? C8 O3 Zn1 113.7(5) . . ? C8 O4 Zn1 112.1(5) . 2_454 ? C9 O5 Zn1 112.5(4) . . ? C9 O6 Zn2 110.8(4) . . ? C10 O7 Zn1 110.9(4) . . ? C10 O8 Zn2 114.8(4) . . ? C11 O9 Zn2 113.5(4) . . ? C12 O11 Zn2 113.5(4) . . ? C13 O13 Zn2 112.3(4) . . ? C13 O14 Zn2 113.3(4) . 2_455 ? C1 N1 Co1 108.4(5) . . ? C1 N1 H1A 110.0 . . ? Co1 N1 H1A 110.0 . . ? C1 N1 H1B 110.0 . . ? Co1 N1 H1B 110.0 . . ? H1A N1 H1B 108.4 . . ? C2 N2 Co1 110.1(5) . . ? C2 N2 H2A 109.6 . . ? Co1 N2 H2A 109.6 . . ? C2 N2 H2B 109.6 . . ? Co1 N2 H2B 109.6 . . ? H2A N2 H2B 108.2 . . ? C3 N3 Co1 110.6(4) . . ? C3 N3 H3A 109.5 . . ? Co1 N3 H3A 109.5 . . ? C3 N3 H3B 109.5 . . ? Co1 N3 H3B 109.5 . . ? H3A N3 H3B 108.1 . . ? C4 N4 Co1 109.4(4) . . ? C4 N4 H4A 109.8 . . ? Co1 N4 H4A 109.8 . . ? C4 N4 H4B 109.8 . . ? Co1 N4 H4B 109.8 . . ? H4A N4 H4B 108.2 . . ? C5 N5 Co1 109.6(4) . . ? C5 N5 H5A 109.8 . . ? Co1 N5 H5A 109.8 . . ? C5 N5 H5B 109.8 . . ? Co1 N5 H5B 109.8 . . ? H5A N5 H5B 108.2 . . ? C6 N6 Co1 110.1(4) . . ? C6 N6 H6A 109.6 . . ? Co1 N6 H6A 109.6 . . ? C6 N6 H6B 109.6 . . ? Co1 N6 H6B 109.6 . . ? H6A N6 H6B 108.2 . . ? C2 C1 N1 110.6(7) . . ? C2 C1 H1C 109.5 . . ? N1 C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? N1 C1 H1D 109.5 . . ? H1C C1 H1D 108.1 . . ? C1 C2 N2 108.0(7) . . ? C1 C2 H2C 110.1 . . ? N2 C2 H2C 110.1 . . ? C1 C2 H2D 110.1 . . ? N2 C2 H2D 110.1 . . ? H2C C2 H2D 108.4 . . ? C4 C3 N3 108.9(6) . . ? C4 C3 H3C 109.9 . . ? N3 C3 H3C 109.9 . . ? C4 C3 H3D 109.9 . . ? N3 C3 H3D 109.9 . . ? H3C C3 H3D 108.3 . . ? C3 C4 N4 107.0(6) . . ? C3 C4 H4C 110.3 . . ? N4 C4 H4C 110.3 . . ? C3 C4 H4D 110.3 . . ? N4 C4 H4D 110.3 . . ? H4C C4 H4D 108.6 . . ? N5 C5 C6 108.1(6) . . ? N5 C5 H5C 110.1 . . ? C6 C5 H5C 110.1 . . ? N5 C5 H5D 110.1 . . ? C6 C5 H5D 110.1 . . ? H5C C5 H5D 108.4 . . ? C5 C6 N6 107.4(6) . . ? C5 C6 H6C 110.2 . . ? N6 C6 H6C 110.2 . . ? C5 C6 H6D 110.2 . . ? N6 C6 H6D 110.2 . . ? H6C C6 H6D 108.5 . . ? O2 C7 O1 126.1(8) . . ? O2 C7 C7 118.1(8) . 2_444 ? O1 C7 C7 115.7(10) . 2_444 ? O4 C8 O3 125.7(7) . . ? O4 C8 C8 117.2(8) . 2_454 ? O3 C8 C8 117.1(9) . 2_454 ? O5 C9 O6 127.6(6) . . ? O5 C9 C10 116.5(6) . . ? O6 C9 C10 115.9(6) . . ? O8 C10 O7 126.1(6) . . ? O8 C10 C9 117.3(5) . . ? O7 C10 C9 116.6(6) . . ? O10 C11 O9 126.1(6) . . ? O10 C11 C12 118.7(6) . . ? O9 C11 C12 115.2(5) . . ? O12 C12 O11 125.6(6) . . ? O12 C12 C11 118.5(6) . . ? O11 C12 C11 115.9(6) . . ? O13 C13 O14 126.6(6) . . ? O13 C13 C13 117.3(7) . 2_455 ? O14 C13 C13 116.2(7) . 2_455 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O9 0.90 2.07 2.956(7) 168.0 2_445 N1 H1B O3W 0.90 2.64 3.285(11) 129.6 1_556 N2 H2A O4W 0.90 2.15 3.010(9) 160.1 2 N2 H2B O5W 0.90 2.29 3.137(8) 157.1 2 N3 H3A O14 0.90 2.48 3.193(7) 136.5 1_545 N3 H3A O9 0.90 2.51 3.075(7) 121.0 2_445 N3 H3B O2W 0.90 2.07 2.911(10) 154.5 . N4 H4A O8 0.90 2.01 2.902(7) 169.7 2 N4 H4B O10 0.90 2.06 2.955(7) 174.2 2_545 N5 H5A O7 0.90 2.15 2.973(7) 151.6 2 N5 H5B O3W 0.90 2.10 2.966(9) 160.9 1_556 N6 H6A O6 0.90 2.09 2.992(7) 176.1 2_445 N6 H6B O12 0.90 2.15 2.965(7) 150.7 2_545 N6 H6B O10 0.90 2.50 3.201(7) 135.4 2_545 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.495 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.107 # Attachment 'Mn-2.cif' data_Mn-2 _database_code_depnum_ccdc_archive 'CCDC 764684' #TrackingRef 'Mn-2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H38 Co Mn2 N6 O20' _chemical_formula_weight 791.32 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.133(3) _cell_length_b 22.410(5) _cell_length_c 10.267(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.96(3) _cell_angle_gamma 90.00 _cell_volume 2984.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22759 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.9 _exptl_crystal_description rod-shaped _exptl_crystal_colour 'Salmon pink' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.761 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1628 _exptl_absorpt_coefficient_mu 1.476 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 SCX-MINI _diffrn_measurement_method multi-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25026 _diffrn_reflns_av_R_equivalents 0.1078 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5258 _reflns_number_gt 3653 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution DirectMethod _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ? _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^)+(0.0486P)^2^+9.0336P] 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 5258 _refine_ls_number_parameters 406 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1283 _refine_ls_R_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.1635 _refine_ls_wR_factor_gt 0.1454 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn -0.75783(8) 0.70020(5) 1.15349(10) 0.0335(3) Uani 1 1 d . . . Mn2 Mn -0.68982(8) 0.47256(5) 1.33933(11) 0.0353(3) Uani 1 1 d . . . Co1 Co -0.24648(7) 0.62879(4) 1.15810(9) 0.0301(3) Uani 1 1 d . . . O1 O -0.7798(5) 0.3132(2) 1.4786(5) 0.0609(16) Uani 1 1 d . . . O2 O -0.6214(4) 0.5299(2) 1.5005(5) 0.0548(15) Uani 1 1 d . . . O3 O -0.7718(4) 0.3031(2) 1.2161(5) 0.0536(15) Uani 1 1 d . . . O4 O -0.6542(4) 0.5266(2) 1.1791(5) 0.0512(14) Uani 1 1 d . . . O5 O -0.5284(4) 0.4437(2) 1.3830(5) 0.0469(13) Uani 1 1 d . . . O6 O -0.7322(4) 0.3990(2) 1.2127(5) 0.0440(13) Uani 1 1 d . . . O7 O -0.8132(4) 0.5364(2) 1.3104(5) 0.0482(14) Uani 1 1 d . . . O8 O -0.7434(4) 0.4093(2) 1.4664(5) 0.0435(13) Uani 1 1 d . . . O9 O -0.8472(4) 0.7032(2) 0.9587(5) 0.0438(13) Uani 1 1 d . . . O10 O -0.6740(4) 0.6208(2) 1.1143(5) 0.0456(13) Uani 1 1 d . . . O11 O -0.6592(4) 0.7103(2) 1.3447(5) 0.0441(13) Uani 1 1 d . . . O12 O -0.6689(4) 0.7581(2) 1.0470(5) 0.0438(13) Uani 1 1 d . . . O13 O -0.8408(4) 0.6290(2) 1.2348(5) 0.0460(13) Uani 1 1 d . . . O14 O -0.8388(4) 0.7646(2) 1.2560(5) 0.0411(12) Uani 1 1 d . . . C1 C -0.4227(7) 0.5618(4) 1.1804(9) 0.065(3) Uani 1 1 d . . . H1C H -0.4647 0.5902 1.2199 0.080 Uiso 1 1 calc . . . H1D H -0.4485 0.5220 1.1927 0.080 Uiso 1 1 calc . . . C2 C -0.4283(7) 0.5749(4) 1.0345(9) 0.062(2) Uani 1 1 d . . . H2A H -0.4048 0.5404 0.9904 0.080 Uiso 1 1 calc . . . H2B H -0.4992 0.5830 0.9958 0.080 Uiso 1 1 calc . . . C3 C -0.4141(6) 0.6868(4) 1.0132(8) 0.058(2) Uani 1 1 d . . . H3C H -0.4826 0.6845 0.9618 0.080 Uiso 1 1 calc . . . H3D H -0.3746 0.7158 0.9720 0.080 Uiso 1 1 calc . . . C4 C -0.4217(6) 0.7061(4) 1.1507(9) 0.058(2) Uani 1 1 d . . . H4C H -0.4312 0.7490 1.1535 0.080 Uiso 1 1 calc . . . H4D H -0.4803 0.6870 1.1804 0.080 Uiso 1 1 calc . . . C5 C -0.0679(6) 0.6981(4) 1.1446(9) 0.055(2) Uani 1 1 d . . . H5A H -0.0437 0.7384 1.1334 0.080 Uiso 1 1 calc . . . H5B H -0.0233 0.6706 1.1073 0.080 Uiso 1 1 calc . . . C6 C -0.0662(6) 0.6849(4) 1.2883(8) 0.051(2) Uani 1 1 d . . . H6C H 0.0042 0.6780 1.3306 0.080 Uiso 1 1 calc . . . H6D H -0.0933 0.7187 1.3310 0.080 Uiso 1 1 calc . . . C7 C -0.0751(7) 0.5738(4) 1.3024(9) 0.064(2) Uani 1 1 d . . . H7A H -0.1111 0.5434 1.3449 0.080 Uiso 1 1 calc . . . H7B H -0.0063 0.5780 1.3518 0.080 Uiso 1 1 calc . . . C8 C -0.0685(7) 0.5548(4) 1.1600(10) 0.069(3) Uani 1 1 d . . . H8A H -0.0125 0.5759 1.1285 0.080 Uiso 1 1 calc . . . H8B H -0.0550 0.5124 1.1568 0.080 Uiso 1 1 calc . . . C9 C -0.4733(6) 0.4754(3) 1.4663(7) 0.0380(17) Uani 1 1 d . . . C10 C -0.7926(5) 0.5817(3) 1.2470(7) 0.0349(17) Uani 1 1 d . . . C11 C -0.7024(5) 0.7621(3) 0.9260(7) 0.0327(16) Uani 1 1 d . . . C12 C -0.8057(5) 0.7691(3) 1.3753(7) 0.0353(17) Uani 1 1 d . . . C13 C -0.7584(6) 0.3580(3) 1.4183(7) 0.0386(18) Uani 1 1 d . . . C14 C -0.7546(5) 0.3513(3) 1.2702(7) 0.0379(18) Uani 1 1 d . . . C15 C -0.6986(6) 0.5755(3) 1.1738(7) 0.0357(17) Uani 1 1 d . . . N1 N -0.3168(5) 0.5665(3) 1.2415(6) 0.0533(18) Uani 1 1 d . . . H1A H -0.2848 0.5314 1.2347 0.080 Uiso 1 1 calc . . . H1B H -0.3139 0.5748 1.3278 0.080 Uiso 1 1 calc . . . N2 N -0.3631(5) 0.6272(3) 1.0157(6) 0.0520(18) Uani 1 1 d . . . H2 H -0.3383 0.6224 0.9383 0.080 Uiso 1 1 calc . . . N3 N -0.3264(5) 0.6890(3) 1.2362(6) 0.0462(16) Uani 1 1 d . . . H3A H -0.3421 0.6748 1.3126 0.080 Uiso 1 1 calc . . . H3B H -0.2871 0.7217 1.2550 0.080 Uiso 1 1 calc . . . N4 N -0.1731(5) 0.6917(3) 1.0787(6) 0.0520(17) Uani 1 1 d . . . H4A H -0.1728 0.6832 0.9931 0.080 Uiso 1 1 calc . . . H4B H -0.2065 0.7266 1.0829 0.080 Uiso 1 1 calc . . . N5 N -0.1304(5) 0.6307(3) 1.3016(6) 0.0490(17) Uani 1 1 d . . . H5 H -0.1559 0.6337 1.3788 0.080 Uiso 1 1 calc . . . N6 N -0.1677(5) 0.5692(3) 1.0753(6) 0.0510(17) Uani 1 1 d . . . H6A H -0.2055 0.5357 1.0600 0.080 Uiso 1 1 calc . . . H6B H -0.1551 0.5833 0.9972 0.080 Uiso 1 1 calc . . . O1W O 0.1684(12) 0.5693(8) 1.5777(12) 0.259(8) Uani 1 1 d . . . O2W O 0.0239(11) 0.6422(6) 1.6281(15) 0.125(5) Uani 0.60 1 d P . . O2W' O -0.032(2) 0.5683(13) 1.647(3) 0.164(10) Uani 0.40 1 d P . . O3W O 0.3987(9) 0.6410(4) 0.7274(9) 0.155(4) Uani 1 1 d U . . O4W O -0.0073(8) 0.6142(5) 0.8890(9) 0.158(4) Uani 1 1 d . . . O5W O 0.2581(8) 0.5553(3) 1.8546(8) 0.142(4) Uani 1 1 d . . . O6W O 0.5337(5) 0.6604(3) 1.4349(6) 0.079(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0379(6) 0.0315(6) 0.0311(6) 0.0018(5) 0.0056(5) 0.0006(5) Mn2 0.0402(6) 0.0268(6) 0.0383(6) 0.0016(5) 0.0046(5) -0.0017(5) Co1 0.0300(5) 0.0333(5) 0.0280(5) -0.0017(4) 0.0072(4) -0.0009(4) O1 0.103(5) 0.044(3) 0.035(3) 0.005(3) 0.008(3) -0.020(3) O2 0.036(3) 0.053(3) 0.072(4) -0.020(3) 0.000(3) 0.006(3) O3 0.087(4) 0.034(3) 0.040(3) -0.008(3) 0.009(3) -0.006(3) O4 0.065(4) 0.033(3) 0.063(4) 0.010(3) 0.035(3) 0.008(3) O5 0.044(3) 0.040(3) 0.055(3) -0.014(3) 0.002(3) -0.002(3) O6 0.060(3) 0.044(3) 0.029(3) -0.002(2) 0.009(2) -0.007(3) O7 0.037(3) 0.047(3) 0.064(4) 0.021(3) 0.018(3) 0.002(3) O8 0.063(3) 0.035(3) 0.033(3) -0.005(2) 0.010(2) -0.006(3) O9 0.039(3) 0.052(3) 0.038(3) 0.007(3) -0.001(2) -0.013(3) O10 0.061(4) 0.033(3) 0.049(3) 0.008(3) 0.029(3) 0.006(3) O11 0.041(3) 0.053(3) 0.038(3) -0.005(3) 0.003(2) 0.011(3) O12 0.046(3) 0.048(3) 0.035(3) 0.005(2) -0.001(2) -0.014(3) O13 0.037(3) 0.038(3) 0.067(4) 0.016(3) 0.020(3) 0.007(2) O14 0.047(3) 0.041(3) 0.032(3) 0.000(2) -0.005(2) 0.012(2) C1 0.058(6) 0.066(6) 0.075(7) -0.004(5) 0.020(5) -0.026(5) C2 0.059(6) 0.063(6) 0.062(6) -0.020(5) 0.008(5) -0.015(5) C3 0.047(5) 0.065(6) 0.057(6) 0.010(5) -0.003(4) 0.018(4) C4 0.049(5) 0.057(6) 0.069(6) -0.003(5) 0.015(5) 0.019(4) C5 0.040(5) 0.049(5) 0.076(6) 0.008(5) 0.017(4) 0.001(4) C6 0.042(5) 0.050(5) 0.057(5) -0.010(4) -0.004(4) -0.006(4) C7 0.065(6) 0.064(6) 0.063(6) 0.018(5) 0.011(5) 0.011(5) C8 0.061(6) 0.058(6) 0.091(8) -0.005(5) 0.023(6) 0.008(5) C9 0.044(5) 0.031(4) 0.041(4) -0.002(4) 0.012(4) -0.001(4) C10 0.024(4) 0.038(4) 0.041(4) 0.000(4) 0.000(3) -0.002(3) C11 0.033(4) 0.028(4) 0.036(5) -0.002(3) 0.002(3) 0.002(3) C12 0.034(4) 0.037(4) 0.034(4) 0.003(4) 0.000(4) 0.002(3) C13 0.043(5) 0.043(5) 0.027(4) 0.006(4) -0.002(3) -0.004(4) C14 0.036(4) 0.041(5) 0.036(4) 0.006(4) 0.004(3) -0.008(4) C15 0.050(5) 0.024(4) 0.034(4) -0.003(3) 0.007(3) 0.004(4) N1 0.063(5) 0.052(4) 0.047(4) 0.003(3) 0.015(4) -0.007(4) N2 0.052(4) 0.071(5) 0.035(4) -0.001(4) 0.012(3) -0.005(4) N3 0.043(4) 0.045(4) 0.048(4) -0.010(3) -0.001(3) 0.006(3) N4 0.058(4) 0.048(4) 0.052(4) 0.000(3) 0.013(4) -0.004(3) N5 0.049(4) 0.058(4) 0.041(4) 0.001(3) 0.010(3) 0.004(4) N6 0.052(4) 0.053(4) 0.049(4) -0.011(3) 0.010(3) 0.005(3) O1W 0.263(15) 0.40(2) 0.127(10) 0.028(12) 0.075(10) 0.092(15) O2W 0.115(11) 0.096(10) 0.150(13) -0.024(9) -0.024(10) -0.005(9) O2W' 0.14(2) 0.19(3) 0.15(2) -0.03(2) 0.013(17) 0.04(2) O3W 0.207(8) 0.132(6) 0.130(6) 0.000(5) 0.040(6) 0.059(6) O4W 0.191(10) 0.172(10) 0.111(7) -0.014(7) 0.024(7) -0.072(8) O5W 0.229(11) 0.080(6) 0.109(7) -0.013(5) -0.004(7) 0.026(6) O6W 0.059(4) 0.087(5) 0.095(5) 0.025(4) 0.025(4) 0.016(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 Mn1 O12 2.154(5) . ? Mn1 O9 2.156(5) . ? Mn1 O14 2.161(5) . ? Mn1 O10 2.162(5) . ? Mn1 O13 2.170(5) . ? Mn1 O11 2.189(5) . ? Mn2 O8 2.120(5) . ? Mn2 O6 2.120(5) . ? Mn2 O7 2.148(5) . ? Mn2 O4 2.153(5) . ? Mn2 O2 2.175(5) . ? Mn2 O5 2.194(5) . ? Co1 N1 1.945(6) . ? Co1 N2 1.946(6) . ? Co1 N5 1.949(6) . ? Co1 N3 1.956(6) . ? Co1 N4 1.957(6) . ? Co1 N6 1.961(6) . ? O1 C13 1.234(8) . ? O2 C9 1.244(8) 3_468 ? O3 C14 1.219(8) . ? O4 C15 1.237(8) . ? O5 C9 1.251(8) . ? O6 C14 1.276(8) . ? O7 C10 1.257(8) . ? O8 C13 1.256(8) . ? O9 C12 1.251(8) 4_575 ? O10 C15 1.254(8) . ? O11 C11 1.245(8) 4_576 ? O12 C11 1.255(8) . ? O13 C10 1.231(8) . ? O14 C12 1.238(8) . ? C1 N1 1.439(10) . ? C1 C2 1.517(12) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 N2 1.482(10) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 N2 1.493(10) . ? C3 C4 1.494(12) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 N3 1.464(10) . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 N4 1.447(10) . ? C5 C6 1.502(11) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 N5 1.497(10) . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 N5 1.467(10) . ? C7 C8 1.538(12) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 N6 1.485(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O2 1.244(8) 3_468 ? C9 C9 1.527(13) 3_468 ? C10 C15 1.549(10) . ? C11 O11 1.245(8) 4_575 ? C11 C12 1.542(9) 4_575 ? C12 O9 1.251(8) 4_576 ? C12 C11 1.542(9) 4_576 ? C13 C14 1.537(10) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 H2 0.9100 . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 H5 0.9100 . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? 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 O12 Mn1 O9 76.76(18) . . ? O12 Mn1 O14 101.08(19) . . ? O9 Mn1 O14 101.12(19) . . ? O12 Mn1 O10 93.94(19) . . ? O9 Mn1 O10 94.1(2) . . ? O14 Mn1 O10 160.62(18) . . ? O12 Mn1 O13 169.1(2) . . ? O9 Mn1 O13 98.4(2) . . ? O14 Mn1 O13 89.35(19) . . ? O10 Mn1 O13 76.56(18) . . ? O12 Mn1 O11 95.78(19) . . ? O9 Mn1 O11 171.55(19) . . ? O14 Mn1 O11 76.18(18) . . ? O10 Mn1 O11 90.29(19) . . ? O13 Mn1 O11 89.6(2) . . ? O8 Mn2 O6 77.10(18) . . ? O8 Mn2 O7 102.41(19) . . ? O6 Mn2 O7 108.3(2) . . ? O8 Mn2 O4 168.4(2) . . ? O6 Mn2 O4 92.1(2) . . ? O7 Mn2 O4 76.58(19) . . ? O8 Mn2 O2 93.6(2) . . ? O6 Mn2 O2 164.5(2) . . ? O7 Mn2 O2 85.7(2) . . ? O4 Mn2 O2 97.8(2) . . ? O8 Mn2 O5 94.6(2) . . ? O6 Mn2 O5 92.84(19) . . ? O7 Mn2 O5 155.28(19) . . ? O4 Mn2 O5 90.2(2) . . ? O2 Mn2 O5 75.34(19) . . ? N1 Co1 N2 86.9(3) . . ? N1 Co1 N5 93.0(3) . . ? N2 Co1 N5 179.6(3) . . ? N1 Co1 N3 89.6(3) . . ? N2 Co1 N3 84.9(3) . . ? N5 Co1 N3 94.7(3) . . ? N1 Co1 N4 178.4(3) . . ? N2 Co1 N4 94.7(3) . . ? N5 Co1 N4 85.5(3) . . ? N3 Co1 N4 90.2(3) . . ? N1 Co1 N6 91.2(3) . . ? N2 Co1 N6 93.9(3) . . ? N5 Co1 N6 86.5(3) . . ? N3 Co1 N6 178.5(3) . . ? N4 Co1 N6 89.0(3) . . ? C9 O2 Mn2 115.4(5) 3_468 . ? C15 O4 Mn2 112.0(4) . . ? C9 O5 Mn2 114.2(4) . . ? C14 O6 Mn2 115.1(4) . . ? C10 O7 Mn2 113.0(4) . . ? C13 O8 Mn2 114.7(4) . . ? C12 O9 Mn1 114.7(4) 4_575 . ? C15 O10 Mn1 113.5(4) . . ? C11 O11 Mn1 112.6(4) 4_576 . ? C11 O12 Mn1 114.3(4) . . ? C10 O13 Mn1 113.1(4) . . ? C12 O14 Mn1 114.3(4) . . ? N1 C1 C2 108.2(7) . . ? N1 C1 H1C 110.1 . . ? C2 C1 H1C 110.1 . . ? N1 C1 H1D 110.1 . . ? C2 C1 H1D 110.1 . . ? H1C C1 H1D 108.4 . . ? N2 C2 C1 110.0(7) . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 109.8(6) . . ? N2 C3 H3C 109.7 . . ? C4 C3 H3C 109.7 . . ? N2 C3 H3D 109.7 . . ? C4 C3 H3D 109.7 . . ? H3C C3 H3D 108.2 . . ? N3 C4 C3 108.3(6) . . ? N3 C4 H4C 110.0 . . ? C3 C4 H4C 110.0 . . ? N3 C4 H4D 110.0 . . ? C3 C4 H4D 110.0 . . ? H4C C4 H4D 108.4 . . ? N4 C5 C6 107.9(6) . . ? N4 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? N4 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? N5 C6 C5 109.1(6) . . ? N5 C6 H6C 109.9 . . ? C5 C6 H6C 109.9 . . ? N5 C6 H6D 109.9 . . ? C5 C6 H6D 109.9 . . ? H6C C6 H6D 108.3 . . ? N5 C7 C8 109.6(7) . . ? N5 C7 H7A 109.7 . . ? C8 C7 H7A 109.7 . . ? N5 C7 H7B 109.7 . . ? C8 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N6 C8 C7 108.8(7) . . ? N6 C8 H8A 109.9 . . ? C7 C8 H8A 109.9 . . ? N6 C8 H8B 109.9 . . ? C7 C8 H8B 109.9 . . ? H8A C8 H8B 108.3 . . ? O2 C9 O5 125.5(6) 3_468 . ? O2 C9 C9 117.0(8) 3_468 3_468 ? O5 C9 C9 117.5(8) . 3_468 ? O13 C10 O7 126.9(6) . . ? O13 C10 C15 117.6(6) . . ? O7 C10 C15 115.5(6) . . ? O11 C11 O12 125.0(6) 4_575 . ? O11 C11 C12 117.9(6) 4_575 4_575 ? O12 C11 C12 117.2(6) . 4_575 ? O14 C12 O9 126.5(6) . 4_576 ? O14 C12 C11 116.9(6) . 4_576 ? O9 C12 C11 116.6(6) 4_576 4_576 ? O1 C13 O8 125.6(7) . . ? O1 C13 C14 117.6(7) . . ? O8 C13 C14 116.8(6) . . ? O3 C14 O6 124.8(7) . . ? O3 C14 C13 120.3(7) . . ? O6 C14 C13 115.0(7) . . ? O4 C15 O10 125.7(7) . . ? O4 C15 C10 117.6(6) . . ? O10 C15 C10 116.7(6) . . ? C1 N1 Co1 110.7(5) . . ? C1 N1 H1A 109.5 . . ? Co1 N1 H1A 109.5 . . ? C1 N1 H1B 109.5 . . ? Co1 N1 H1B 109.5 . . ? H1A N1 H1B 108.1 . . ? C2 N2 C3 116.2(6) . . ? C2 N2 Co1 108.7(5) . . ? C3 N2 Co1 107.2(5) . . ? C2 N2 H2 108.2 . . ? C3 N2 H2 108.2 . . ? Co1 N2 H2 108.2 . . ? C4 N3 Co1 113.5(5) . . ? C4 N3 H3A 108.9 . . ? Co1 N3 H3A 108.9 . . ? C4 N3 H3B 108.9 . . ? Co1 N3 H3B 108.9 . . ? H3A N3 H3B 107.7 . . ? C5 N4 Co1 111.9(5) . . ? C5 N4 H4A 109.2 . . ? Co1 N4 H4A 109.2 . . ? C5 N4 H4B 109.2 . . ? Co1 N4 H4B 109.2 . . ? H4A N4 H4B 107.9 . . ? C7 N5 C6 114.9(6) . . ? C7 N5 Co1 108.3(5) . . ? C6 N5 Co1 109.5(5) . . ? C7 N5 H5 108.0 . . ? C6 N5 H5 108.0 . . ? Co1 N5 H5 108.0 . . ? C8 N6 Co1 111.6(5) . . ? C8 N6 H6A 109.3 . . ? Co1 N6 H6A 109.3 . . ? C8 N6 H6B 109.3 . . ? Co1 N6 H6B 109.3 . . ? H6A N6 H6B 108.0 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A O3 0.90 2.18 3.003(8) 151.8 3_467 N4 H4B O1 0.90 2.04 2.833(8) 146.2 2_457 N3 H3A O6W 0.90 2.23 3.019(9) 146.0 1_455 N3 H3A O1 0.90 2.48 3.041(8) 120.6 3_468 N3 H3B O3 0.90 1.99 2.872(8) 167.8 2_457 N1 H1A O5W 0.90 2.20 3.042(10) 155.7 3_568 N1 H1B O8 0.90 2.16 3.028(8) 162.1 3_468 N6 H6A O5W 0.90 2.37 3.159(11) 147.0 3_568 N6 H6B O6 0.90 2.45 3.125(8) 132.1 3_467 N6 H6B O4W 0.90 2.48 3.220(12) 139.6 . N5 H5 O1 0.91 2.16 2.982(8) 150.3 3_468 N5 H5 O8 0.91 2.42 3.233(8) 148.8 3_468 N2 H2 O6 0.91 1.99 2.885(8) 169.7 3_467 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.599 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.092 # Attachment 'Cd-3.cif' data_Cd-3 _database_code_depnum_ccdc_archive 'CCDC 764685' #TrackingRef 'Cd-3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H35 Cd2 Co N6 O19.50' _chemical_formula_weight 895.22 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.955(3) _cell_length_b 9.5430(19) _cell_length_c 18.549(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.01(3) _cell_angle_gamma 90.00 _cell_volume 3001.2(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22091 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.9 _exptl_crystal_description rod-shaped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.981 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 2.041 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 SCX-MINI _diffrn_measurement_method multi-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24586 _diffrn_reflns_av_R_equivalents 0.1289 _diffrn_reflns_av_sigmaI/netI 0.1017 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5288 _reflns_number_gt 3582 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_structure_solution DirectMethod _computing_structure_refinement SHELXL _computing_publication_material 'CrystalStructure 3.7.0' _computing_molecular_graphics ? _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^)+(0.0429P)^2^+9.7260P] 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 5288 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1363 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.1295 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.145 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.41415(4) 0.91346(8) -0.36861(4) 0.0332(2) Uani 1 1 d . . . Cd2 Cd 0.08065(4) 0.75183(8) -0.43168(5) 0.0444(3) Uani 1 1 d . . . Co1 Co 0.28391(7) 1.14867(13) -0.11745(7) 0.0319(4) Uani 1 1 d . . . O1 O 0.4921(4) 0.7578(8) -0.3069(4) 0.053(2) Uani 1 1 d . . . O2 O 0.3804(4) 0.7662(7) -0.2428(4) 0.0465(19) Uani 1 1 d . . . O3 O 0.4449(4) 1.0790(7) -0.2863(4) 0.0442(18) Uani 1 1 d . . . O4 O 0.5557(4) 1.0822(8) -0.3518(4) 0.059(2) Uani 1 1 d . . . O5 O 0.4112(4) 1.0666(7) -0.4651(4) 0.0443(19) Uani 1 1 d . . . O6 O 0.4901(4) 1.1585(7) -0.5467(4) 0.0432(19) Uani 1 1 d . . . O7 O 0.2819(4) 0.9777(7) -0.3431(4) 0.0445(19) Uani 1 1 d . . . O8 O 0.1582(4) 0.9227(8) -0.3700(4) 0.054(2) Uani 1 1 d . . . O9 O 0.3337(4) 0.7667(7) -0.4295(4) 0.0461(19) Uani 1 1 d . . . O10 O 0.2110(4) 0.7187(9) -0.4579(5) 0.065(3) Uani 1 1 d . . . O11 O 0.0673(4) 0.8803(8) -0.5367(4) 0.056(2) Uani 1 1 d . . . O12 O 0.0130(4) 1.0686(8) -0.5868(4) 0.053(2) Uani 1 1 d . . . O13 O -0.0402(4) 0.6395(8) -0.4508(4) 0.056(2) Uani 1 1 d . . . O14 O -0.0997(4) 0.4652(8) -0.5100(5) 0.070(3) Uani 1 1 d . . . O15 O 0.0779(5) 0.6628(11) -0.3155(5) 0.090(3) Uani 1 1 d . . . N1 N 0.3368(5) 1.3186(9) -0.1551(5) 0.044(2) Uani 1 1 d . . . H1A H 0.3213 1.3942 -0.1297 0.080 Uiso 1 1 calc . . . H1B H 0.3894 1.3099 -0.1506 0.080 Uiso 1 1 calc . . . N2 N 0.2341(5) 1.1408(9) -0.2118(5) 0.047(2) Uani 1 1 d . . . H2 H 0.2653 1.0855 -0.2397 0.080 Uiso 1 1 calc . . . N3 N 0.2233(5) 0.9782(8) -0.0948(5) 0.043(2) Uani 1 1 d . . . H3A H 0.2565 0.9076 -0.0842 0.080 Uiso 1 1 calc . . . H3B H 0.1923 0.9936 -0.0562 0.080 Uiso 1 1 calc . . . N4 N 0.2012(4) 1.2656(8) -0.0714(4) 0.037(2) Uani 1 1 d . . . H4A H 0.1940 1.3445 -0.0972 0.080 Uiso 1 1 calc . . . H4B H 0.1553 1.2183 -0.0704 0.080 Uiso 1 1 calc . . . N5 N 0.3367(5) 1.1610(9) -0.0243(5) 0.041(2) Uani 1 1 d . . . H5 H 0.3694 1.2366 -0.0259 0.080 Uiso 1 1 calc . . . N6 N 0.3727(5) 1.0291(8) -0.1467(5) 0.041(2) Uani 1 1 d . . . H6A H 0.3548 0.9437 -0.1590 0.080 Uiso 1 1 calc . . . H6B H 0.3968 1.0667 -0.1854 0.080 Uiso 1 1 calc . . . C1 C 0.3156(7) 1.3365(13) -0.2320(7) 0.061(4) Uani 1 1 d . . . H1C H 0.3178 1.4350 -0.2447 0.080 Uiso 1 1 calc . . . H1D H 0.3531 1.2865 -0.2620 0.080 Uiso 1 1 calc . . . C2 C 0.2353(8) 1.2819(13) -0.2450(7) 0.063(4) Uani 1 1 d . . . H2A H 0.2246 1.2761 -0.2963 0.080 Uiso 1 1 calc . . . H2B H 0.1962 1.3422 -0.2228 0.080 Uiso 1 1 calc . . . C3 C 0.1577(8) 1.0661(14) -0.2042(6) 0.066(4) Uani 1 1 d . . . H3C H 0.1377 1.0389 -0.2512 0.080 Uiso 1 1 calc . . . H3D H 0.1190 1.1261 -0.1811 0.080 Uiso 1 1 calc . . . C4 C 0.1730(7) 0.9388(12) -0.1589(7) 0.059(3) Uani 1 1 d . . . H4C H 0.1999 0.8683 -0.1874 0.080 Uiso 1 1 calc . . . H4D H 0.1234 0.8997 -0.1424 0.080 Uiso 1 1 calc . . . C5 C 0.2259(7) 1.3020(13) 0.0037(6) 0.057(3) Uani 1 1 d . . . H5A H 0.2543 1.3902 0.0037 0.080 Uiso 1 1 calc . . . H5B H 0.1797 1.3122 0.0342 0.080 Uiso 1 1 calc . . . C6 C 0.2776(7) 1.1881(14) 0.0321(6) 0.057(3) Uani 1 1 d . . . H6C H 0.3030 1.2174 0.0765 0.080 Uiso 1 1 calc . . . H6D H 0.2469 1.1043 0.0417 0.080 Uiso 1 1 calc . . . C7 C 0.3869(6) 1.0345(11) -0.0160(6) 0.049(3) Uani 1 1 d . . . H7A H 0.3547 0.9529 -0.0057 0.080 Uiso 1 1 calc . . . H7B H 0.4243 1.0472 0.0231 0.080 Uiso 1 1 calc . . . C8 C 0.4296(6) 1.0163(11) -0.0867(6) 0.047(3) Uani 1 1 d . . . H8A H 0.4703 1.0871 -0.0914 0.080 Uiso 1 1 calc . . . H8B H 0.4547 0.9249 -0.0882 0.080 Uiso 1 1 calc . . . C9 C 0.4497(6) 0.7228(11) -0.2547(6) 0.041(3) Uani 1 1 d . . . C10 C 0.5141(6) 1.1193(10) -0.3002(6) 0.042(3) Uani 1 1 d . . . C11 C 0.4720(6) 1.0666(10) -0.5042(5) 0.034(2) Uani 1 1 d . . . C12 C 0.2304(6) 0.9056(11) -0.3748(6) 0.037(3) Uani 1 1 d . . . C13 C 0.2602(6) 0.7861(10) -0.4246(5) 0.034(3) Uani 1 1 d . . . C14 C 0.0228(6) 0.9876(12) -0.5358(6) 0.041(3) Uani 1 1 d . . . C15 C -0.0412(6) 0.5318(13) -0.4882(6) 0.044(3) Uani 1 1 d . . . O1W O 0.2006(4) 0.9369(7) -0.6186(4) 0.056(2) Uani 1 1 d . . . O2W O 0.3294(4) 0.7195(8) -0.0825(4) 0.053(2) Uani 1 1 d . . . O3W O -0.0291(7) 0.5828(14) 0.2468(7) 0.144(5) Uani 1 1 d . . . O4W O 0.2267(5) 0.6481(9) -0.2623(5) 0.073(3) Uani 1 1 d . . . O5W O -0.0621(18) 0.784(3) 0.3565(15) 0.204(15) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0290(4) 0.0347(4) 0.0359(5) -0.0028(4) 0.0040(3) 0.0034(4) Cd2 0.0297(4) 0.0439(5) 0.0595(6) -0.0093(4) 0.0053(4) 0.0008(4) Co1 0.0257(7) 0.0293(8) 0.0408(9) 0.0008(7) 0.0039(6) -0.0017(6) O1 0.055(5) 0.063(5) 0.042(5) 0.026(4) 0.013(4) 0.009(4) O2 0.037(4) 0.053(5) 0.050(5) 0.008(4) 0.002(4) 0.014(4) O3 0.031(4) 0.055(5) 0.046(5) -0.011(4) 0.007(3) -0.018(4) O4 0.061(5) 0.063(5) 0.052(5) -0.027(4) 0.026(4) -0.017(5) O5 0.040(4) 0.049(5) 0.044(4) 0.016(4) 0.020(4) 0.021(4) O6 0.050(5) 0.036(4) 0.044(5) 0.016(4) 0.022(4) 0.015(4) O7 0.035(4) 0.035(4) 0.063(5) -0.018(4) 0.012(4) -0.002(4) O8 0.035(4) 0.049(5) 0.077(6) -0.011(4) 0.013(4) 0.005(4) O9 0.033(4) 0.048(5) 0.057(5) -0.023(4) 0.001(4) 0.001(4) O10 0.033(4) 0.082(6) 0.081(6) -0.045(5) 0.011(4) -0.012(4) O11 0.055(5) 0.047(5) 0.065(6) 0.001(4) 0.016(4) 0.018(4) O12 0.045(5) 0.052(5) 0.063(6) 0.002(4) 0.014(4) 0.011(4) O13 0.028(4) 0.051(5) 0.087(6) -0.031(5) 0.009(4) 0.003(4) O14 0.027(4) 0.061(5) 0.122(8) -0.044(5) 0.009(5) 0.000(4) O15 0.065(6) 0.123(8) 0.081(7) 0.047(6) -0.004(5) -0.021(6) N1 0.035(5) 0.041(5) 0.055(6) -0.005(5) 0.002(4) 0.002(4) N2 0.045(6) 0.048(6) 0.047(6) -0.005(5) -0.001(5) 0.014(5) N3 0.037(5) 0.034(5) 0.057(6) -0.006(5) 0.000(5) -0.002(4) N4 0.029(5) 0.028(5) 0.054(6) -0.002(4) 0.006(4) -0.006(4) N5 0.028(5) 0.041(5) 0.053(6) 0.003(5) -0.003(4) -0.013(4) N6 0.035(5) 0.039(5) 0.049(6) 0.002(4) 0.007(4) 0.001(4) C1 0.061(8) 0.053(8) 0.069(9) 0.026(7) 0.021(7) 0.017(7) C2 0.075(9) 0.053(8) 0.060(9) 0.011(7) -0.004(7) -0.001(7) C3 0.079(10) 0.077(10) 0.043(8) -0.004(7) -0.021(7) -0.012(8) C4 0.064(8) 0.043(7) 0.070(9) -0.013(7) -0.004(7) -0.011(6) C5 0.059(8) 0.063(8) 0.048(8) -0.031(7) 0.008(6) -0.014(7) C6 0.045(7) 0.072(9) 0.054(8) -0.013(7) 0.008(6) -0.007(7) C7 0.044(7) 0.038(7) 0.065(9) 0.016(6) -0.029(6) -0.002(6) C8 0.043(7) 0.036(6) 0.063(9) 0.008(6) -0.010(6) -0.002(6) C9 0.038(7) 0.039(7) 0.046(7) 0.005(6) -0.008(6) 0.003(6) C10 0.041(7) 0.028(6) 0.057(8) 0.004(5) 0.004(6) -0.002(5) C11 0.042(6) 0.035(6) 0.026(6) 0.001(5) 0.001(5) 0.009(5) C12 0.030(6) 0.034(6) 0.048(7) -0.002(6) 0.006(5) -0.001(6) C13 0.034(6) 0.038(7) 0.030(6) -0.004(5) 0.009(5) 0.003(5) C14 0.031(6) 0.039(7) 0.053(8) 0.000(6) 0.004(5) 0.003(6) C15 0.021(6) 0.055(8) 0.055(8) -0.006(6) 0.005(5) -0.001(6) O1W 0.064(5) 0.038(4) 0.066(5) -0.003(4) 0.017(4) -0.002(4) O2W 0.039(4) 0.058(5) 0.064(5) 0.007(4) 0.004(4) 0.009(4) O3W 0.119(10) 0.157(12) 0.157(12) 0.018(9) 0.007(9) 0.004(9) O4W 0.079(6) 0.064(6) 0.076(6) 0.005(5) -0.011(5) 0.002(5) O5W 0.21(3) 0.25(4) 0.15(2) -0.03(2) -0.14(2) -0.06(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 Cd1 O3 2.258(7) . ? Cd1 O9 2.258(7) . ? Cd1 O1 2.294(7) . ? Cd1 O5 2.311(6) . ? Cd1 O6 2.362(6) 3_674 ? Cd1 O7 2.373(6) . ? Cd2 O10 2.286(7) . ? Cd2 O11 2.313(8) . ? Cd2 O15 2.317(8) . ? Cd2 O13 2.340(7) . ? Cd2 O14 2.358(7) 3_564 ? Cd2 O12 2.361(7) 3_574 ? Cd2 O8 2.387(7) . ? Co1 N2 1.944(9) . ? Co1 N5 1.949(8) . ? Co1 N6 1.966(8) . ? Co1 N3 1.970(8) . ? Co1 N1 1.980(9) . ? Co1 N4 1.985(8) . ? O1 C9 1.250(12) . ? O2 C9 1.266(11) . ? O3 C10 1.262(11) . ? O4 C10 1.240(12) . ? O5 C11 1.261(11) . ? O6 C11 1.218(11) . ? O6 Cd1 2.362(6) 3_674 ? O7 C12 1.258(11) . ? O8 C12 1.239(11) . ? O9 C13 1.263(11) . ? O10 C13 1.221(11) . ? O11 C14 1.273(12) . ? O12 C14 1.233(12) . ? O12 Cd2 2.361(7) 3_574 ? O13 C15 1.240(12) . ? O14 C15 1.246(12) . ? O14 Cd2 2.358(7) 3_564 ? N1 C1 1.481(14) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C2 1.481(14) . ? N2 C3 1.485(14) . ? N2 H2 0.9100 . ? N3 C4 1.509(14) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C5 1.496(13) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C6 1.473(13) . ? N5 C7 1.485(13) . ? N5 H5 0.9100 . ? N6 C8 1.478(13) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? C1 C2 1.477(16) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.500(16) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 C6 1.492(17) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 C8 1.508(15) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.546(14) 2_644 ? C10 C9 1.546(14) 2_654 ? C11 C11 1.594(18) 3_674 ? C12 C13 1.551(13) . ? C14 C14 1.55(2) 3_574 ? C15 C15 1.586(19) 3_564 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Cd1 O9 155.8(2) . . ? O3 Cd1 O1 89.0(3) . . ? O9 Cd1 O1 101.3(3) . . ? O3 Cd1 O5 94.9(3) . . ? O9 Cd1 O5 89.5(3) . . ? O1 Cd1 O5 143.9(2) . . ? O3 Cd1 O6 119.6(2) . 3_674 ? O9 Cd1 O6 84.4(2) . 3_674 ? O1 Cd1 O6 75.4(2) . 3_674 ? O5 Cd1 O6 71.6(2) . 3_674 ? O3 Cd1 O7 84.4(2) . . ? O9 Cd1 O7 71.9(2) . . ? O1 Cd1 O7 127.7(3) . . ? O5 Cd1 O7 88.3(2) . . ? O6 Cd1 O7 149.1(3) 3_674 . ? O10 Cd2 O11 89.3(3) . . ? O10 Cd2 O15 99.6(3) . . ? O11 Cd2 O15 167.4(3) . . ? O10 Cd2 O13 138.7(3) . . ? O11 Cd2 O13 91.7(3) . . ? O15 Cd2 O13 87.4(3) . . ? O10 Cd2 O14 69.4(3) . 3_564 ? O11 Cd2 O14 95.3(3) . 3_564 ? O15 Cd2 O14 96.1(3) . 3_564 ? O13 Cd2 O14 69.4(2) . 3_564 ? O10 Cd2 O12 141.4(3) . 3_574 ? O11 Cd2 O12 70.9(3) . 3_574 ? O15 Cd2 O12 96.7(3) . 3_574 ? O13 Cd2 O12 76.4(3) . 3_574 ? O14 Cd2 O12 142.8(3) 3_564 3_574 ? O10 Cd2 O8 70.4(3) . . ? O11 Cd2 O8 95.5(3) . . ? O15 Cd2 O8 79.4(3) . . ? O13 Cd2 O8 150.2(2) . . ? O14 Cd2 O8 138.1(2) 3_564 . ? O12 Cd2 O8 78.7(2) 3_574 . ? N2 Co1 N5 177.9(4) . . ? N2 Co1 N6 93.6(4) . . ? N5 Co1 N6 85.9(4) . . ? N2 Co1 N3 86.2(4) . . ? N5 Co1 N3 95.8(3) . . ? N6 Co1 N3 88.8(3) . . ? N2 Co1 N1 84.9(4) . . ? N5 Co1 N1 93.2(3) . . ? N6 Co1 N1 91.8(3) . . ? N3 Co1 N1 171.0(4) . . ? N2 Co1 N4 95.8(3) . . ? N5 Co1 N4 84.8(4) . . ? N6 Co1 N4 170.5(4) . . ? N3 Co1 N4 90.2(3) . . ? N1 Co1 N4 90.6(3) . . ? C9 O1 Cd1 103.2(6) . . ? C10 O3 Cd1 106.8(6) . . ? C11 O5 Cd1 115.3(6) . . ? C11 O6 Cd1 113.2(6) . 3_674 ? C12 O7 Cd1 114.9(6) . . ? C12 O8 Cd2 114.8(7) . . ? C13 O9 Cd1 117.9(6) . . ? C13 O10 Cd2 118.6(6) . . ? C14 O11 Cd2 118.2(7) . . ? C14 O12 Cd2 115.7(7) . 3_574 ? C15 O13 Cd2 118.5(6) . . ? C15 O14 Cd2 119.2(7) . 3_564 ? C1 N1 Co1 108.9(7) . . ? C1 N1 H1A 109.9 . . ? Co1 N1 H1A 109.9 . . ? C1 N1 H1B 109.9 . . ? Co1 N1 H1B 109.9 . . ? H1A N1 H1B 108.3 . . ? C2 N2 C3 119.3(9) . . ? C2 N2 Co1 109.4(7) . . ? C3 N2 Co1 108.2(7) . . ? C2 N2 H2 106.4 . . ? C3 N2 H2 106.4 . . ? Co1 N2 H2 106.4 . . ? C4 N3 Co1 109.4(7) . . ? C4 N3 H3A 109.8 . . ? Co1 N3 H3A 109.8 . . ? C4 N3 H3B 109.8 . . ? Co1 N3 H3B 109.8 . . ? H3A N3 H3B 108.2 . . ? C5 N4 Co1 109.5(6) . . ? C5 N4 H4A 109.8 . . ? Co1 N4 H4A 109.8 . . ? C5 N4 H4B 109.8 . . ? Co1 N4 H4B 109.8 . . ? H4A N4 H4B 108.2 . . ? C6 N5 C7 117.3(9) . . ? C6 N5 Co1 109.1(6) . . ? C7 N5 Co1 107.8(6) . . ? C6 N5 H5 107.4 . . ? C7 N5 H5 107.4 . . ? Co1 N5 H5 107.4 . . ? C8 N6 Co1 109.9(6) . . ? C8 N6 H6A 109.7 . . ? Co1 N6 H6A 109.7 . . ? C8 N6 H6B 109.7 . . ? Co1 N6 H6B 109.7 . . ? H6A N6 H6B 108.2 . . ? C2 C1 N1 109.8(9) . . ? C2 C1 H1C 109.7 . . ? N1 C1 H1C 109.7 . . ? C2 C1 H1D 109.7 . . ? N1 C1 H1D 109.7 . . ? H1C C1 H1D 108.2 . . ? C1 C2 N2 105.5(10) . . ? C1 C2 H2A 110.6 . . ? N2 C2 H2A 110.6 . . ? C1 C2 H2B 110.6 . . ? N2 C2 H2B 110.6 . . ? H2A C2 H2B 108.8 . . ? N2 C3 C4 106.9(10) . . ? N2 C3 H3C 110.3 . . ? C4 C3 H3C 110.3 . . ? N2 C3 H3D 110.3 . . ? C4 C3 H3D 110.3 . . ? H3C C3 H3D 108.6 . . ? C3 C4 N3 109.7(9) . . ? C3 C4 H4C 109.7 . . ? N3 C4 H4C 109.7 . . ? C3 C4 H4D 109.7 . . ? N3 C4 H4D 109.7 . . ? H4C C4 H4D 108.2 . . ? C6 C5 N4 108.9(9) . . ? C6 C5 H5A 109.9 . . ? N4 C5 H5A 109.9 . . ? C6 C5 H5B 109.9 . . ? N4 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? N5 C6 C5 106.0(10) . . ? N5 C6 H6C 110.5 . . ? C5 C6 H6C 110.5 . . ? N5 C6 H6D 110.5 . . ? C5 C6 H6D 110.5 . . ? H6C C6 H6D 108.7 . . ? N5 C7 C8 106.2(8) . . ? N5 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? N5 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? N6 C8 C7 109.4(8) . . ? N6 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? N6 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? O1 C9 O2 125.6(10) . . ? O1 C9 C10 117.0(9) . 2_644 ? O2 C9 C10 117.4(10) . 2_644 ? O4 C10 O3 126.9(10) . . ? O4 C10 C9 117.8(9) . 2_654 ? O3 C10 C9 115.3(10) . 2_654 ? O6 C11 O5 125.3(9) . . ? O6 C11 C11 119.2(11) . 3_674 ? O5 C11 C11 115.5(11) . 3_674 ? O8 C12 O7 125.4(10) . . ? O8 C12 C13 117.5(9) . . ? O7 C12 C13 117.1(9) . . ? O10 C13 O9 124.0(9) . . ? O10 C13 C12 117.8(9) . . ? O9 C13 C12 118.2(9) . . ? O12 C14 O11 125.0(10) . . ? O12 C14 C14 119.6(12) . 3_574 ? O11 C14 C14 115.4(13) . 3_574 ? O13 C15 O14 128.0(9) . . ? O13 C15 C15 117.4(12) . 3_564 ? O14 C15 C15 114.6(13) . 3_564 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A O1W 0.90 2.61 3.352(11) 139.8 4_586 N1 H1B O1 0.90 2.22 3.042(11) 152.5 2_654 N1 H1B O6 0.90 2.59 3.293(11) 135.3 4_586 N2 H2 O7 0.91 2.19 3.002(11) 147.7 . N3 H3A O2W 0.90 2.18 3.064(11) 167.1 . N3 H3B O14 0.90 2.01 2.861(11) 156.7 2_554 N4 H4A O1W 0.90 2.13 2.971(10) 155.8 4_586 N4 H4B O13 0.90 2.13 3.012(10) 167.0 2_554 N5 H5 O5 0.91 2.30 3.092(10) 144.8 4_586 N5 H5 O6 0.91 2.31 3.146(10) 152.7 4_586 N6 H6A O2 0.90 2.34 3.080(11) 139.7 . N6 H6A O2W 0.90 2.60 3.269(11) 131.4 . N6 H6B O3 0.90 2.05 2.904(10) 159.0 . N6 H6B O1 0.90 2.63 3.280(11) 130.2 2_654 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.773 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.134