# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Xiao-Ming Chen' _publ_contact_author_email CXM@MAIL.SYSU.EDU.CN _publ_section_title ; Two Temperature-induced Metal-Carboxylate Framework Isomers Based on Different Linear Trinuclear Co3(OOCR)8 Clusters ; loop_ _publ_author_name 'Xiao-Ming Chen.' 'Xiao-Lin Qi.' 'Xiao-Feng Wang.' 'Wei Xue.' ; Yue-Biao Zhang ; data_1 _database_code_depnum_ccdc_archive 'CCDC 766294' #TrackingRef 'C003032E.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Me2NH2)2(Co3(1,4-bdc)4)4DMF _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H60 Co3 N6 O20' _chemical_formula_weight 1217.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.225(4) _cell_length_b 9.8510(10) _cell_length_c 17.7341(19) _cell_angle_alpha 90.00 _cell_angle_beta 99.335(2) _cell_angle_gamma 90.00 _cell_volume 5727.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2524 _exptl_absorpt_coefficient_mu 0.935 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8257 _exptl_absorpt_correction_T_max 0.9115 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_reflns_number 13764 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4994 _reflns_number_gt 4099 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _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^)+(0.1454P)^2^+111.3205P] 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 4994 _refine_ls_number_parameters 290 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0950 _refine_ls_wR_factor_ref 0.2685 _refine_ls_wR_factor_gt 0.2537 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.069 _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 Co1 Co 0.2500 -0.2500 1.0000 0.0116(4) Uani 1 2 d S . . Co2 Co 0.14935(3) -0.17912(10) 0.96560(5) 0.0156(3) Uani 1 1 d . . . O1 O 0.15820(15) -0.2926(6) 0.8775(3) 0.0236(12) Uani 1 1 d . . . O2 O 0.22649(15) -0.2890(5) 0.8886(3) 0.0207(11) Uani 1 1 d . . . O3 O 0.15000(15) -0.6878(6) 0.5519(3) 0.0236(12) Uani 1 1 d . . . O4 O 0.21220(14) -0.6138(5) 0.5392(3) 0.0189(11) Uani 1 1 d . . . O5 O 0.16910(17) 0.0182(6) 0.9115(3) 0.0324(14) Uani 1 1 d . . . O6 O 0.20507(14) -0.0894(5) 1.0081(3) 0.0183(10) Uani 1 1 d . . . O7 O 0.11152(16) -0.0403(6) 1.0328(3) 0.0346(14) Uani 1 1 d . . . O8 O 0.08743(17) -0.1588(7) 0.9317(3) 0.0357(15) Uani 1 1 d . . . C1 C 0.1888(2) -0.3967(8) 0.7817(4) 0.0189(15) Uani 1 1 d . . . C2 C 0.2231(2) -0.4127(8) 0.7474(4) 0.0235(17) Uani 1 1 d . . . H2C H 0.2480 -0.3772 0.7704 0.028 Uiso 1 1 calc R . . C3 C 0.2201(2) -0.4817(8) 0.6789(4) 0.0232(17) Uani 1 1 d . . . H3A H 0.2430 -0.4901 0.6555 0.028 Uiso 1 1 calc R . . C4 C 0.1839(2) -0.5380(7) 0.6449(4) 0.0181(15) Uani 1 1 d . . . C5 C 0.1496(2) -0.5225(9) 0.6795(4) 0.0272(18) Uani 1 1 d . . . H5A H 0.1248 -0.5594 0.6568 0.033 Uiso 1 1 calc R . . C6 C 0.1522(2) -0.4525(9) 0.7473(4) 0.0292(19) Uani 1 1 d . . . H6A H 0.1291 -0.4426 0.7701 0.035 Uiso 1 1 calc R . . C7 C 0.1916(2) -0.3206(7) 0.8551(4) 0.0190(15) Uani 1 1 d . . . C8 C 0.1817(2) -0.6193(7) 0.5728(4) 0.0167(14) Uani 1 1 d . . . C9 C 0.2205(2) 0.2504(8) 0.9351(4) 0.0250(17) Uani 1 1 d . . . H9A H 0.2008 0.2501 0.8913 0.030 Uiso 1 1 calc R . . C10 C 0.2255(2) 0.1364(7) 0.9822(4) 0.0208(15) Uani 1 1 d . . . C11 C 0.2556(2) 0.1369(8) 1.0472(4) 0.0231(16) Uani 1 1 d . . . H11A H 0.2594 0.0607 1.0785 0.028 Uiso 1 1 calc R . . C12 C 0.1987(2) 0.0166(7) 0.9642(4) 0.0223(16) Uani 1 1 d . . . C13 C 0.0333(3) 0.0632(12) 1.0439(6) 0.051(3) Uani 1 1 d . . . H13A H 0.0555 0.1057 1.0733 0.061 Uiso 1 1 calc R . . C14 C 0.0394(3) -0.0385(11) 0.9926(5) 0.040(2) Uani 1 1 d . . . C15 C 0.0067(3) -0.1014(12) 0.9488(6) 0.048(3) Uani 1 1 d . . . H15A H 0.0110 -0.1692 0.9145 0.058 Uiso 1 1 calc R . . C16 C 0.0820(2) -0.0799(10) 0.9855(5) 0.033(2) Uani 1 1 d . . . O9 O -0.0859(4) -0.1227(13) 0.7436(7) 0.117(2) Uiso 1 1 d D . . N1 N -0.1358(4) -0.0122(15) 0.8134(8) 0.117(2) Uiso 1 1 d D . . C17 C -0.1106(5) -0.1013(18) 0.7841(11) 0.117(2) Uiso 1 1 d D . . H17A H -0.1148 -0.1846 0.8063 0.140 Uiso 1 1 calc R . . C18 C -0.1411(5) 0.1143(14) 0.7747(11) 0.117(2) Uiso 1 1 d D . . H18A H -0.1150 0.1493 0.7678 0.175 Uiso 1 1 calc R . . H18B H -0.1541 0.1772 0.8044 0.175 Uiso 1 1 calc R . . H18C H -0.1578 0.1018 0.7257 0.175 Uiso 1 1 calc R . . C19 C -0.1761(5) -0.0807(18) 0.8192(11) 0.117(2) Uiso 1 1 d D . . H19A H -0.1712 -0.1720 0.8371 0.175 Uiso 1 1 calc R . . H19B H -0.1930 -0.0820 0.7697 0.175 Uiso 1 1 calc R . . H19C H -0.1898 -0.0313 0.8543 0.175 Uiso 1 1 calc R . . N2 N 0.0407(13) -0.490(4) 0.6767(19) 0.157(7) Uiso 0.50 1 d PD A 1 H2A H 0.0183 -0.5057 0.6975 0.188 Uiso 0.50 1 d PR A 1 H2B H 0.0623 -0.5211 0.7093 0.188 Uiso 0.50 1 d PR A 1 C20 C 0.0438(16) -0.343(4) 0.675(3) 0.157(7) Uiso 0.50 1 d PD A 1 H20A H 0.0456 -0.3001 0.7236 0.235 Uiso 0.50 1 d PR A 1 H20B H 0.0681 -0.3244 0.6536 0.235 Uiso 0.50 1 d PR A 1 H20C H 0.0205 -0.3077 0.6409 0.235 Uiso 0.50 1 d PR A 1 C21 C 0.0383(15) -0.560(4) 0.601(2) 0.157(7) Uiso 0.50 1 d PD A 1 H21A H 0.0354 -0.6548 0.6108 0.235 Uiso 0.50 1 d PR A 1 H21B H 0.0150 -0.5287 0.5662 0.235 Uiso 0.50 1 d PR A 1 H21C H 0.0625 -0.5454 0.5789 0.235 Uiso 0.50 1 d PR A 1 N2' N 0.0308(10) -0.846(4) 0.7635(19) 0.157(7) Uiso 0.50 1 d PD B 2 H2'A H 0.0561 -0.8813 0.7700 0.188 Uiso 0.50 1 d PR B 2 H2'B H 0.0276 -0.8044 0.8074 0.188 Uiso 0.50 1 d PR B 2 C20' C 0.0000 -0.957(3) 0.7500 0.157(7) Uiso 1 2 d SD . 2 H20D H 0.0038 -1.0202 0.7917 0.235 Uiso 0.50 1 d PR . 2 H20E H -0.0270 -0.9198 0.7442 0.235 Uiso 0.50 1 d PR . 2 H20F H 0.0037 -1.0027 0.7038 0.235 Uiso 0.50 1 d PR . 2 C21' C 0.0284(15) -0.745(4) 0.699(3) 0.157(7) Uiso 0.50 1 d PD B 2 H21D H 0.0485 -0.6752 0.7118 0.235 Uiso 0.50 1 d PR B 2 H21E H 0.0324 -0.7879 0.6521 0.235 Uiso 0.50 1 d PR B 2 H21F H 0.0017 -0.7049 0.6924 0.235 Uiso 0.50 1 d PR B 2 N3 N 0.0973(7) -0.348(4) 0.425(2) 0.225(8) Uiso 0.50 1 d PD C 3 O10 O 0.0729(13) -0.272(5) 0.311(3) 0.225(8) Uiso 0.50 1 d PD C 3 C22 C 0.0890(12) -0.242(5) 0.378(3) 0.225(8) Uiso 0.50 1 d PD C 3 H22A H 0.0947 -0.1529 0.3934 0.270 Uiso 0.50 1 calc PR C 3 C23 C 0.0885(9) -0.486(4) 0.4019(16) 0.225(8) Uiso 0.50 1 d PD C 3 H23A H 0.0772 -0.4894 0.3486 0.338 Uiso 0.50 1 d PR C 3 H23B H 0.0672 -0.4978 0.4319 0.338 Uiso 0.50 1 d PR C 3 H23C H 0.1084 -0.5567 0.4137 0.338 Uiso 0.50 1 d PR C 3 C24 C 0.1155(9) -0.322(3) 0.5018(18) 0.225(8) Uiso 0.50 1 d PD C 3 H24A H 0.1267 -0.2324 0.5035 0.338 Uiso 0.50 1 d PR C 3 H24B H 0.1370 -0.3866 0.5175 0.338 Uiso 0.50 1 d PR C 3 H24C H 0.0958 -0.3277 0.5357 0.338 Uiso 0.50 1 d PR C 3 N3' N 0.0857(7) -0.425(3) 0.4742(16) 0.225(8) Uiso 0.50 1 d PD D 4 O10' O 0.0522(11) -0.416(4) 0.574(2) 0.225(8) Uiso 0.50 1 d PD D 4 C22' C 0.0552(10) -0.468(4) 0.5120(19) 0.225(8) Uiso 0.50 1 d PD D 4 H22B H 0.0369 -0.5341 0.4909 0.270 Uiso 0.50 1 calc PR D 4 C23' C 0.0885(9) -0.486(4) 0.4019(16) 0.225(8) Uiso 0.50 1 d PD D 4 H23D H 0.0711 -0.5640 0.3944 0.338 Uiso 0.50 1 calc PR D 4 H23E H 0.1162 -0.5128 0.4010 0.338 Uiso 0.50 1 calc PR D 4 H23F H 0.0802 -0.4213 0.3619 0.338 Uiso 0.50 1 calc PR D 4 C24' C 0.1155(9) -0.322(3) 0.5018(18) 0.225(8) Uiso 0.50 1 d PD D 4 H24D H 0.1079 -0.2788 0.5459 0.338 Uiso 0.50 1 calc PR D 4 H24E H 0.1165 -0.2561 0.4625 0.338 Uiso 0.50 1 calc PR D 4 H24F H 0.1418 -0.3637 0.5154 0.338 Uiso 0.50 1 calc PR D 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0136(6) 0.0105(7) 0.0115(6) 0.0005(5) 0.0043(5) -0.0003(5) Co2 0.0144(5) 0.0186(6) 0.0143(5) 0.0001(4) 0.0041(4) 0.0024(4) O1 0.020(3) 0.032(3) 0.019(3) -0.008(2) 0.005(2) 0.006(2) O2 0.020(3) 0.027(3) 0.016(2) 0.001(2) 0.006(2) 0.000(2) O3 0.019(3) 0.032(3) 0.021(3) -0.010(2) 0.007(2) -0.006(2) O4 0.024(3) 0.013(3) 0.022(3) -0.002(2) 0.011(2) 0.001(2) O5 0.030(3) 0.017(3) 0.045(3) 0.008(3) -0.011(3) 0.000(2) O6 0.019(2) 0.012(2) 0.026(3) 0.002(2) 0.007(2) 0.003(2) O7 0.021(3) 0.045(4) 0.037(3) -0.007(3) 0.003(2) 0.009(3) O8 0.023(3) 0.052(4) 0.032(3) 0.000(3) 0.003(2) 0.018(3) C1 0.016(3) 0.027(4) 0.013(3) 0.001(3) 0.004(3) 0.003(3) C2 0.020(4) 0.035(5) 0.016(3) -0.006(3) 0.004(3) -0.004(3) C3 0.020(4) 0.026(4) 0.028(4) -0.007(3) 0.014(3) -0.005(3) C4 0.014(3) 0.021(4) 0.020(3) -0.001(3) 0.005(3) 0.002(3) C5 0.018(4) 0.034(5) 0.031(4) -0.015(4) 0.008(3) -0.007(3) C6 0.018(4) 0.044(5) 0.027(4) -0.010(4) 0.009(3) 0.003(4) C7 0.020(4) 0.020(4) 0.018(4) 0.002(3) 0.006(3) 0.003(3) C8 0.019(3) 0.016(4) 0.016(3) 0.000(3) 0.005(3) 0.004(3) C9 0.025(4) 0.022(4) 0.026(4) -0.001(3) -0.002(3) 0.002(3) C10 0.026(4) 0.012(4) 0.026(4) 0.001(3) 0.008(3) 0.003(3) C11 0.029(4) 0.012(4) 0.030(4) 0.004(3) 0.009(3) 0.002(3) C12 0.023(4) 0.014(4) 0.032(4) -0.004(3) 0.013(3) 0.001(3) C13 0.021(4) 0.074(8) 0.054(6) -0.029(6) -0.002(4) 0.014(5) C14 0.022(4) 0.053(6) 0.045(5) -0.007(5) 0.005(4) 0.019(4) C15 0.028(5) 0.061(7) 0.054(6) -0.027(5) 0.001(4) 0.016(5) C16 0.025(4) 0.043(5) 0.028(4) 0.004(4) 0.003(3) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O4 2.035(5) 6_546 ? Co1 O4 2.035(5) 4_556 ? Co1 O2 2.040(5) . ? Co1 O2 2.040(5) 7_547 ? Co1 O6 2.196(5) . ? Co1 O6 2.196(5) 7_547 ? Co2 O1 1.982(5) . ? Co2 O3 2.013(5) 6_546 ? Co2 O8 2.057(5) . ? Co2 O6 2.079(5) . ? Co2 O5 2.309(6) . ? Co2 O7 2.314(6) . ? Co2 C16 2.518(8) . ? O1 C7 1.267(8) . ? O2 C7 1.253(9) . ? O3 C8 1.255(9) . ? O3 Co2 2.013(5) 6_545 ? O4 C8 1.257(8) . ? O4 Co1 2.035(5) 4_546 ? O5 C12 1.242(9) . ? O6 C12 1.299(9) . ? O7 C16 1.245(10) . ? O8 C16 1.266(10) . ? C1 C6 1.383(11) . ? C1 C2 1.384(9) . ? C1 C7 1.492(10) . ? C2 C3 1.382(10) . ? C3 C4 1.372(10) . ? C4 C5 1.388(10) . ? C4 C8 1.501(10) . ? C5 C6 1.376(11) . ? C9 C11 1.371(11) 7_557 ? C9 C10 1.394(11) . ? C10 C11 1.399(11) . ? C10 C12 1.481(10) . ? C11 C9 1.371(11) 7_557 ? C13 C14 1.392(13) . ? C13 C15 1.407(12) 5_557 ? C14 C15 1.376(13) . ? C14 C16 1.497(11) . ? C15 C13 1.407(12) 5_557 ? O9 C17 1.195(13) . ? N1 C17 1.371(13) . ? N1 C18 1.419(14) . ? N1 C19 1.520(14) . ? N2 C20 1.45(2) . ? N2 C21 1.500(19) . ? N2' C20' 1.492(19) . ? N2' C21' 1.511(19) . ? C20' N2' 1.492(19) 2_556 ? N3 C22 1.34(2) . ? N3 C24 1.42(2) . ? N3 C23 1.43(2) . ? O10 C22 1.25(2) . ? N3' C22' 1.37(2) . ? O10' C22' 1.23(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Co1 O4 180.0(2) 6_546 4_556 ? O4 Co1 O2 92.6(2) 6_546 . ? O4 Co1 O2 87.4(2) 4_556 . ? O4 Co1 O2 87.4(2) 6_546 7_547 ? O4 Co1 O2 92.6(2) 4_556 7_547 ? O2 Co1 O2 180.000(1) . 7_547 ? O4 Co1 O6 89.37(18) 6_546 . ? O4 Co1 O6 90.63(18) 4_556 . ? O2 Co1 O6 92.38(19) . . ? O2 Co1 O6 87.62(19) 7_547 . ? O4 Co1 O6 90.63(18) 6_546 7_547 ? O4 Co1 O6 89.37(18) 4_556 7_547 ? O2 Co1 O6 87.62(19) . 7_547 ? O2 Co1 O6 92.38(19) 7_547 7_547 ? O6 Co1 O6 180.000(1) . 7_547 ? O1 Co2 O3 104.3(2) . 6_546 ? O1 Co2 O8 95.4(2) . . ? O3 Co2 O8 99.9(2) 6_546 . ? O1 Co2 O6 106.8(2) . . ? O3 Co2 O6 95.9(2) 6_546 . ? O8 Co2 O6 148.6(2) . . ? O1 Co2 O5 93.4(2) . . ? O3 Co2 O5 153.6(2) 6_546 . ? O8 Co2 O5 97.7(2) . . ? O6 Co2 O5 59.78(19) . . ? O1 Co2 O7 154.4(2) . . ? O3 Co2 O7 86.1(2) 6_546 . ? O8 Co2 O7 59.5(2) . . ? O6 Co2 O7 95.1(2) . . ? O5 Co2 O7 86.1(2) . . ? O1 Co2 C16 125.3(3) . . ? O3 Co2 C16 92.7(2) 6_546 . ? O8 Co2 C16 30.0(3) . . ? O6 Co2 C16 122.9(3) . . ? O5 Co2 C16 92.9(3) . . ? O7 Co2 C16 29.5(2) . . ? C7 O1 Co2 128.2(5) . . ? C7 O2 Co1 133.2(4) . . ? C8 O3 Co2 118.6(4) . 6_545 ? C8 O4 Co1 136.3(5) . 4_546 ? C12 O5 Co2 85.4(4) . . ? C12 O6 Co2 94.3(4) . . ? C12 O6 Co1 125.9(4) . . ? Co2 O6 Co1 104.2(2) . . ? C16 O7 Co2 84.4(5) . . ? C16 O8 Co2 95.6(5) . . ? C6 C1 C2 119.2(7) . . ? C6 C1 C7 120.7(6) . . ? C2 C1 C7 120.1(6) . . ? C3 C2 C1 119.7(7) . . ? C4 C3 C2 121.3(6) . . ? C3 C4 C5 119.0(7) . . ? C3 C4 C8 120.6(6) . . ? C5 C4 C8 120.4(6) . . ? C6 C5 C4 120.1(7) . . ? C5 C6 C1 120.8(7) . . ? O2 C7 O1 126.0(7) . . ? O2 C7 C1 117.3(6) . . ? O1 C7 C1 116.7(6) . . ? O3 C8 O4 125.9(6) . . ? O3 C8 C4 117.4(6) . . ? O4 C8 C4 116.7(6) . . ? C11 C9 C10 120.5(7) 7_557 . ? C9 C10 C11 119.3(7) . . ? C9 C10 C12 120.3(7) . . ? C11 C10 C12 120.3(7) . . ? C9 C11 C10 120.2(7) 7_557 . ? O5 C12 O6 119.6(7) . . ? O5 C12 C10 121.8(7) . . ? O6 C12 C10 118.5(7) . . ? C14 C13 C15 119.6(9) . 5_557 ? C15 C14 C13 120.4(8) . . ? C15 C14 C16 120.1(8) . . ? C13 C14 C16 119.5(8) . . ? C14 C15 C13 120.0(9) . 5_557 ? O7 C16 O8 120.5(7) . . ? O7 C16 C14 120.6(8) . . ? O8 C16 C14 118.8(8) . . ? O7 C16 Co2 66.1(4) . . ? O8 C16 Co2 54.4(4) . . ? C14 C16 Co2 172.1(7) . . ? C17 N1 C18 114.5(12) . . ? C17 N1 C19 109.9(13) . . ? C18 N1 C19 112.4(12) . . ? O9 C17 N1 149.4(17) . . ? C20 N2 C21 115(2) . . ? C20' N2' C21' 114.2(19) . . ? N2' C20' N2' 86(3) 2_556 . ? C22 N3 C24 118(4) . . ? C22 N3 C23 123(4) . . ? C24 N3 C23 118(2) . . ? O10 C22 N3 115(5) . . ? O10' C22' N3' 119(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.641 _refine_diff_density_min -2.499 _refine_diff_density_rms 0.177 #===============================END data_2 _database_code_depnum_ccdc_archive 'CCDC 766295' #TrackingRef 'C003032E.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Me2NH2)2(Co3(1,4-bdc)4)4DMF _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H60 Co3 N6 O20' _chemical_formula_weight 1217.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.232(4) _cell_length_b 9.7670(12) _cell_length_c 18.311(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.609(2) _cell_angle_gamma 90.00 _cell_volume 5937.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2524 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7863 _exptl_absorpt_correction_T_max 0.9120 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _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 'Bruker Apex CCD' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15378 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0715 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5808 _reflns_number_gt 3788 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, 1998.' _computing_cell_refinement 'SAINT-PLUS, Ver. 6.0, 1997' _computing_data_reduction 'SAINT-PLUS, Ver. 6.0, 1997' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, Ver. 6.10, Bruker AXS Inc., 2000.' _computing_publication_material 'SHELXTL-Bruker AXS Inc., 1998.' _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^)+(0.1383P)^2^+5.0947P] 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 5808 _refine_ls_number_parameters 296 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1158 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2298 _refine_ls_wR_factor_gt 0.1986 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.2500 -0.2500 1.0000 0.0271(3) Uani 1 2 d S . . Co2 Co 0.34740(2) -0.30171(8) 1.01300(4) 0.0335(3) Uani 1 1 d . . . O1 O 0.34626(12) -0.1927(5) 0.9209(2) 0.0504(11) Uani 1 1 d . A . O2 O 0.28465(12) -0.1196(4) 0.94209(19) 0.0418(9) Uani 1 1 d . A . O3 O 0.34066(12) 0.1844(4) 0.5992(2) 0.0490(10) Uani 1 1 d . . . O4 O 0.27352(12) 0.1853(4) 0.59962(19) 0.0433(10) Uani 1 1 d . . . O5 O 0.32185(17) -0.5156(5) 1.0915(3) 0.0815(17) Uani 1 1 d . A . O6 O 0.29643(10) -0.4093(4) 0.9936(2) 0.0383(9) Uani 1 1 d . A . C1 C 0.31300(17) -0.0546(6) 0.8316(3) 0.0418(14) Uani 1 1 d . A . C2 C 0.27712(18) 0.0007(7) 0.8046(3) 0.0532(16) Uani 1 1 d . . . H2C H 0.2540 -0.0073 0.8310 0.064 Uiso 1 1 calc R . . C3 C 0.27565(19) 0.0684(7) 0.7376(3) 0.0552(17) Uani 1 1 d . . . H3A H 0.2513 0.1040 0.7190 0.066 Uiso 1 1 calc R . . C4 C 0.30989(17) 0.0831(6) 0.6987(3) 0.0414(13) Uani 1 1 d . . . C5 C 0.34539(19) 0.0293(8) 0.7259(3) 0.0572(18) Uani 1 1 d . . . H5A H 0.3686 0.0383 0.6997 0.069 Uiso 1 1 calc R . . C6 C 0.3470(2) -0.0389(8) 0.7926(3) 0.0600(19) Uani 1 1 d . . . H6A H 0.3714 -0.0744 0.8109 0.072 Uiso 1 1 calc R . . C7 C 0.31503(17) -0.1281(6) 0.9038(3) 0.0393(13) Uani 1 1 d . . . C8 C 0.30763(18) 0.1577(6) 0.6266(3) 0.0387(13) Uani 1 1 d . . . C9 C 0.2721(2) -0.7469(6) 1.0655(3) 0.0510(16) Uani 1 1 d . . . H9A H 0.2873 -0.7444 1.1095 0.061 Uiso 1 1 calc R . . C10 C 0.27259(17) -0.6351(6) 1.0179(3) 0.0386(13) Uani 1 1 d . A . C11 C 0.25060(19) -0.6394(6) 0.9525(3) 0.0457(14) Uani 1 1 d . . . H11A H 0.2511 -0.5655 0.9205 0.055 Uiso 1 1 calc R . . C12 C 0.29851(18) -0.5135(6) 1.0376(3) 0.0452(14) Uani 1 1 d . . . C13 C 0.4678(3) -0.5800(14) 0.9780(9) 0.150(6) Uani 1 1 d . . . H13A H 0.4463 -0.6358 0.9629 0.180 Uiso 1 1 calc R . . C14 C 0.4611(2) -0.4499(11) 1.0013(5) 0.086(3) Uani 1 1 d . . . C15 C 0.4927(4) -0.3715(14) 1.0229(6) 0.117(4) Uani 1 1 d U . . H15A H 0.4882 -0.2827 1.0389 0.140 Uiso 1 1 calc R . . C16 C 0.4157(7) -0.419(2) 0.9922(12) 0.077(5) Uiso 0.510(15) 1 d P A 1 O7 O 0.4040(4) -0.3386(14) 1.0329(7) 0.078(4) Uiso 0.510(15) 1 d P A 1 O8 O 0.3914(4) -0.4745(13) 0.9447(7) 0.093(5) Uiso 0.510(15) 1 d P A 1 C16' C 0.4236(7) -0.368(3) 1.0130(12) 0.078(5) Uiso 0.490(15) 1 d P A 2 O7' O 0.3923(4) -0.4383(12) 1.0033(7) 0.071(4) Uiso 0.490(15) 1 d P A 2 O8' O 0.4199(4) -0.2519(17) 1.0303(7) 0.097(5) Uiso 0.490(15) 1 d P A 2 O9 O 0.4211(9) -0.670(4) 0.7131(15) 0.564(14) Uiso 0.50 1 d PD B 3 N1 N 0.3739(8) -0.502(3) 0.7613(13) 0.564(14) Uiso 0.50 1 d PD B 3 C17 C 0.4118(10) -0.536(3) 0.727(2) 0.564(14) Uiso 0.50 1 d PD B 3 H17A H 0.4293 -0.4661 0.7141 0.677 Uiso 0.50 1 calc PR B 3 C18 C 0.3487(14) -0.617(4) 0.779(4) 0.564(14) Uiso 0.50 1 d PD B 3 H18A H 0.3251 -0.5841 0.8017 0.677 Uiso 0.50 1 calc PR B 3 H18B H 0.3633 -0.6776 0.8114 0.677 Uiso 0.50 1 calc PR B 3 H18C H 0.3408 -0.6649 0.7347 0.677 Uiso 0.50 1 calc PR B 3 C19 C 0.3635(16) -0.364(4) 0.776(3) 0.564(14) Uiso 0.50 1 d PD B 3 H19A H 0.3857 -0.3053 0.7652 0.677 Uiso 0.50 1 calc PR B 3 H19B H 0.3575 -0.3546 0.8264 0.677 Uiso 0.50 1 calc PR B 3 H19C H 0.3403 -0.3386 0.7457 0.677 Uiso 0.50 1 calc PR B 3 O9' O 0.4211(9) -0.670(4) 0.7131(15) 0.564(14) Uiso 0.50 1 d PD C 4 N1' N 0.3739(8) -0.502(3) 0.7613(13) 0.564(14) Uiso 0.50 1 d PD C 4 C17' C 0.3844(9) -0.644(3) 0.741(2) 0.564(14) Uiso 0.50 1 d PD C 4 H17B H 0.3662 -0.7146 0.7477 0.677 Uiso 0.50 1 calc PR C 4 C18' C 0.4042(16) -0.400(3) 0.749(5) 0.564(14) Uiso 0.50 1 d PD C 4 H18D H 0.3951 -0.3128 0.7664 0.677 Uiso 0.50 1 calc PR C 4 H18E H 0.4087 -0.3940 0.6979 0.677 Uiso 0.50 1 calc PR C 4 H18F H 0.4288 -0.4247 0.7752 0.677 Uiso 0.50 1 calc PR C 4 C19' C 0.3361(10) -0.473(5) 0.791(3) 0.564(14) Uiso 0.50 1 d PD C 4 H19D H 0.3349 -0.3776 0.8031 0.677 Uiso 0.50 1 calc PR C 4 H19E H 0.3330 -0.5271 0.8339 0.677 Uiso 0.50 1 calc PR C 4 H19F H 0.3149 -0.4945 0.7552 0.677 Uiso 0.50 1 calc PR C 4 N2 N 0.4361(10) -1.287(5) 0.817(3) 0.47(2) Uiso 0.50 1 d PRD C 5 H2A H 0.4417 -1.2539 0.8620 0.570 Uiso 0.50 1 calc PR C 5 H2B H 0.4185 -1.2301 0.7938 0.570 Uiso 0.50 1 calc PR C 5 C20 C 0.417(2) -1.425(6) 0.823(4) 0.47(2) Uiso 0.50 1 d PD C 5 H20A H 0.3972 -1.4229 0.8583 0.570 Uiso 0.50 1 calc PR C 5 H20B H 0.4378 -1.4909 0.8374 0.570 Uiso 0.50 1 calc PR C 5 H20C H 0.4054 -1.4513 0.7761 0.570 Uiso 0.50 1 calc PR C 5 C21 C 0.4744(19) -1.293(8) 0.775(5) 0.47(2) Uiso 0.50 1 d PD . 5 H21A H 0.4932 -1.2266 0.7954 0.570 Uiso 0.50 1 calc PR . 5 H21B H 0.4684 -1.2727 0.7248 0.570 Uiso 0.50 1 calc PR . 5 H21C H 0.4860 -1.3827 0.7798 0.570 Uiso 0.50 1 calc PR . 5 N2' N 0.5351(18) -1.001(5) 0.751(4) 0.47(2) Uiso 0.50 1 d PD D 6 H2'A H 0.5120 -0.9525 0.7476 0.570 Uiso 0.50 1 calc PR D 6 H2'B H 0.5554 -0.9451 0.7397 0.570 Uiso 0.50 1 calc PR D 6 C20' C 0.533(3) -1.119(9) 0.698(3) 0.47(2) Uiso 0.50 1 d PD D 6 H20D H 0.5292 -1.0852 0.6490 0.570 Uiso 0.50 1 calc PR D 6 H20E H 0.5101 -1.1765 0.7088 0.570 Uiso 0.50 1 calc PR D 6 H20F H 0.5569 -1.1722 0.7027 0.570 Uiso 0.50 1 calc PR D 6 C21' C 0.542(2) -1.054(8) 0.829(3) 0.47(2) Uiso 0.50 1 d PD D 6 H21D H 0.5420 -0.9787 0.8629 0.570 Uiso 0.50 1 calc PR D 6 H21E H 0.5677 -1.0999 0.8338 0.570 Uiso 0.50 1 calc PR D 6 H21F H 0.5211 -1.1172 0.8404 0.570 Uiso 0.50 1 calc PR D 6 N3 N 0.6073(8) -0.828(3) 0.4576(17) 0.357(8) Uiso 0.50 1 d PD E 7 O10 O 0.5885(12) -0.716(5) 0.336(2) 0.357(8) Uiso 0.50 1 d PD E 7 C22 C 0.6016(14) -0.748(6) 0.397(2) 0.357(8) Uiso 0.50 1 d PD E 7 H22B H 0.6164 -0.6704 0.4107 0.429 Uiso 0.50 1 calc PR E 7 C23 C 0.5830(9) -0.948(3) 0.4384(16) 0.357(8) Uiso 0.50 1 d PD E 7 H23A H 0.5695 -0.9344 0.3916 0.429 Uiso 0.50 1 calc PR E 7 H23B H 0.5634 -0.9623 0.4747 0.429 Uiso 0.50 1 calc PR E 7 H23C H 0.6001 -1.0271 0.4364 0.429 Uiso 0.50 1 calc PR E 7 C24 C 0.6270(7) -0.831(3) 0.5300(16) 0.357(8) Uiso 0.50 1 d PD E 7 H24A H 0.6428 -0.7496 0.5374 0.429 Uiso 0.50 1 calc PR E 7 H24B H 0.6441 -0.9099 0.5343 0.429 Uiso 0.50 1 calc PR E 7 H24C H 0.6070 -0.8355 0.5662 0.429 Uiso 0.50 1 calc PR E 7 N3' N 0.5911(9) -0.902(2) 0.5130(15) 0.357(8) Uiso 0.50 1 d PD F 8 O10' O 0.5653(10) -0.895(4) 0.6221(19) 0.357(8) Uiso 0.50 1 d PD F 8 C22' C 0.5609(10) -0.932(3) 0.557(2) 0.357(8) Uiso 0.50 1 d PD F 8 H22A H 0.5379 -0.9781 0.5403 0.429 Uiso 0.50 1 calc PR F 8 C23' C 0.5830(9) -0.948(3) 0.4384(16) 0.357(8) Uiso 0.50 1 d PD F 8 H23D H 0.6060 -0.9300 0.4100 0.429 Uiso 0.50 1 calc PR F 8 H23E H 0.5600 -0.9006 0.4175 0.429 Uiso 0.50 1 calc PR F 8 H23F H 0.5777 -1.0448 0.4385 0.429 Uiso 0.50 1 calc PR F 8 C24' C 0.6270(7) -0.831(3) 0.5300(16) 0.357(8) Uiso 0.50 1 d PD F 8 H24D H 0.6311 -0.8248 0.5822 0.429 Uiso 0.50 1 calc PR F 8 H24E H 0.6253 -0.7406 0.5096 0.429 Uiso 0.50 1 calc PR F 8 H24F H 0.6491 -0.8791 0.5100 0.429 Uiso 0.50 1 calc PR F 8 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0385(6) 0.0233(5) 0.0198(5) 0.0009(4) 0.0051(4) -0.0004(4) Co2 0.0399(5) 0.0350(5) 0.0259(4) -0.0006(3) 0.0049(3) 0.0032(3) O1 0.051(3) 0.065(3) 0.035(2) 0.0177(19) 0.0079(18) 0.007(2) O2 0.057(2) 0.034(2) 0.036(2) 0.0068(16) 0.0155(18) 0.0021(18) O3 0.055(3) 0.059(3) 0.033(2) 0.0135(18) 0.0048(18) -0.004(2) O4 0.056(3) 0.045(3) 0.0283(19) 0.0081(16) 0.0039(17) 0.0012(19) O5 0.095(4) 0.043(3) 0.102(4) 0.005(3) -0.047(3) -0.011(3) O6 0.046(2) 0.023(2) 0.047(2) -0.0022(16) 0.0125(17) 0.0001(16) C1 0.047(3) 0.051(4) 0.028(3) 0.009(2) 0.010(2) -0.002(3) C2 0.048(4) 0.076(5) 0.037(3) 0.017(3) 0.012(3) 0.005(3) C3 0.048(4) 0.074(5) 0.044(3) 0.024(3) 0.008(3) 0.008(3) C4 0.050(3) 0.044(3) 0.030(3) 0.009(2) 0.007(2) 0.000(3) C5 0.053(4) 0.083(5) 0.037(3) 0.027(3) 0.016(3) 0.013(3) C6 0.053(4) 0.079(5) 0.049(4) 0.034(3) 0.010(3) 0.012(3) C7 0.049(3) 0.040(3) 0.030(3) 0.006(2) 0.009(2) 0.001(3) C8 0.050(3) 0.040(3) 0.027(3) 0.000(2) 0.005(2) -0.006(3) C9 0.068(4) 0.035(3) 0.048(3) -0.002(3) -0.014(3) 0.003(3) C10 0.050(3) 0.024(3) 0.041(3) -0.001(2) 0.000(2) 0.002(2) C11 0.073(4) 0.026(3) 0.038(3) 0.008(2) 0.000(3) 0.002(3) C12 0.053(4) 0.027(3) 0.055(4) -0.003(3) -0.004(3) 0.002(3) C13 0.081(7) 0.110(10) 0.254(16) -0.011(10) -0.060(9) 0.042(7) C14 0.056(5) 0.097(7) 0.106(7) 0.023(5) 0.007(4) 0.037(5) C15 0.107(5) 0.114(5) 0.129(5) -0.005(4) -0.007(4) 0.022(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 2.046(4) . ? Co1 O2 2.046(4) 7_547 ? Co1 O4 2.051(4) 6_556 ? Co1 O4 2.051(4) 4_546 ? Co1 O6 2.198(4) . ? Co1 O6 2.198(4) 7_547 ? Co2 O7 1.933(13) . ? Co2 O3 1.972(4) 6_556 ? Co2 O1 1.993(4) . ? Co2 O6 2.011(4) . ? Co2 O7' 2.015(12) . ? O1 C7 1.242(7) . ? O2 C7 1.258(6) . ? O3 C8 1.254(6) . ? O3 Co2 1.972(4) 6 ? O4 C8 1.245(7) . ? O4 Co1 2.051(4) 4_556 ? O5 C12 1.227(7) . ? O6 C12 1.297(7) . ? C1 C6 1.374(8) . ? C1 C2 1.380(8) . ? C1 C7 1.503(7) . ? C2 C3 1.391(8) . ? C3 C4 1.377(8) . ? C4 C5 1.364(8) . ? C4 C8 1.508(7) . ? C5 C6 1.390(8) . ? C9 C11 1.375(9) 7_537 ? C9 C10 1.397(8) . ? C10 C11 1.375(7) . ? C10 C12 1.501(8) . ? C11 C9 1.375(9) 7_537 ? C13 C14 1.362(16) . ? C13 C15 1.396(14) 5_647 ? C14 C15 1.346(14) . ? C14 C16' 1.51(3) . ? C14 C16 1.54(2) . ? C15 C13 1.396(14) 5_647 ? C16 O7 1.16(3) . ? C16 O8 1.28(2) . ? C16' O8' 1.18(3) . ? C16' O7' 1.25(3) . ? O9 C17 1.371(8) . ? N1 C19 1.422(8) . ? N1 C18 1.443(9) . ? N1 C17 1.471(8) . ? N2 C20 1.49(2) . ? N2 C21 1.51(2) . ? C21 C21 1.97(8) 2_656 ? N2' C20' 1.51(2) . ? N2' C21' 1.53(2) . ? N3 C22 1.36(2) . ? N3 C24 1.453(19) . ? N3 C23 1.459(19) . ? O10 C22 1.230(19) . ? N3' C22' 1.35(2) . ? O10' C22' 1.24(2) . ? 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 Co1 O2 180.00(17) . 7_547 ? O2 Co1 O4 93.92(15) . 6_556 ? O2 Co1 O4 86.08(15) 7_547 6_556 ? O2 Co1 O4 86.08(15) . 4_546 ? O2 Co1 O4 93.92(15) 7_547 4_546 ? O4 Co1 O4 180.000(1) 6_556 4_546 ? O2 Co1 O6 90.01(14) . . ? O2 Co1 O6 89.99(14) 7_547 . ? O4 Co1 O6 91.46(14) 6_556 . ? O4 Co1 O6 88.54(14) 4_546 . ? O2 Co1 O6 89.99(14) . 7_547 ? O2 Co1 O6 90.01(14) 7_547 7_547 ? O4 Co1 O6 88.54(14) 6_556 7_547 ? O4 Co1 O6 91.46(14) 4_546 7_547 ? O6 Co1 O6 180.000(1) . 7_547 ? O7 Co2 O3 95.9(4) . 6_556 ? O7 Co2 O1 103.9(4) . . ? O3 Co2 O1 111.62(19) 6_556 . ? O7 Co2 O6 137.7(4) . . ? O3 Co2 O6 108.64(16) 6_556 . ? O1 Co2 O6 98.42(17) . . ? O7 Co2 O7' 34.5(5) . . ? O3 Co2 O7' 124.5(4) 6_556 . ? O1 Co2 O7' 105.3(4) . . ? O6 Co2 O7' 105.0(4) . . ? C7 O1 Co2 117.9(3) . . ? C7 O2 Co1 137.1(4) . . ? C8 O3 Co2 125.0(4) . 6 ? C8 O4 Co1 136.2(3) . 4_556 ? C12 O6 Co2 106.2(3) . . ? C12 O6 Co1 122.6(3) . . ? Co2 O6 Co1 102.02(15) . . ? C6 C1 C2 119.2(5) . . ? C6 C1 C7 120.4(5) . . ? C2 C1 C7 120.4(5) . . ? C1 C2 C3 119.8(5) . . ? C4 C3 C2 120.6(6) . . ? C5 C4 C3 119.5(5) . . ? C5 C4 C8 120.9(5) . . ? C3 C4 C8 119.6(5) . . ? C4 C5 C6 120.2(6) . . ? C1 C6 C5 120.7(6) . . ? O1 C7 O2 125.1(5) . . ? O1 C7 C1 117.9(5) . . ? O2 C7 C1 116.9(5) . . ? O4 C8 O3 126.5(5) . . ? O4 C8 C4 117.4(5) . . ? O3 C8 C4 116.1(5) . . ? C11 C9 C10 120.2(5) 7_537 . ? C11 C10 C9 119.9(5) . . ? C11 C10 C12 120.6(5) . . ? C9 C10 C12 119.4(5) . . ? C10 C11 C9 119.8(5) . 7_537 ? O5 C12 O6 121.8(5) . . ? O5 C12 C10 120.9(5) . . ? O6 C12 C10 117.3(5) . . ? C14 C13 C15 119.1(11) . 5_647 ? C15 C14 C13 119.2(9) . . ? C15 C14 C16' 107.2(14) . . ? C13 C14 C16' 133.5(13) . . ? C15 C14 C16 132.0(13) . . ? C13 C14 C16 108.7(12) . . ? C16' C14 C16 25.6(9) . . ? C14 C15 C13 121.7(11) . 5_647 ? O7 C16 O8 120(2) . . ? O7 C16 C14 115(2) . . ? O8 C16 C14 125.3(18) . . ? C16 O7 Co2 111.0(15) . . ? O8' C16' O7' 118(2) . . ? O8' C16' C14 130(2) . . ? O7' C16' C14 112(2) . . ? C16' O7' Co2 103.7(14) . . ? C19 N1 C18 123.1(8) . . ? C19 N1 C17 120.7(9) . . ? C18 N1 C17 116.2(6) . . ? O9 C17 N1 119.6(7) . . ? C20 N2 C21 111(2) . . ? N2 C21 C21 177(7) . 2_656 ? C20' N2' C21' 110(2) . . ? C22 N3 C24 143(4) . . ? C22 N3 C23 102(4) . . ? C24 N3 C23 115.1(19) . . ? O10 C22 N3 157(8) . . ? O10' C22' N3' 117(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.630 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.137 #End of Crystallographic Information File