# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'M. Fatima C. Guedes da Silva' _publ_contact_author_email fatima.guedes@ist.utl.pt _publ_author_name A.J.L.Pombeiro data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 840090' #TrackingRef '2Cifs_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H18 Co N6 O6 S' _chemical_formula_sum 'C12 H18 Co N6 O6 S' _chemical_formula_weight 433.31 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' S S 0.1246 0.1234 '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 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' 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 7.8225(6) _cell_length_b 12.4161(10) _cell_length_c 17.4883(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.384(5) _cell_angle_gamma 90.00 _cell_volume 1695.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7959 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 30.77 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.697 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 1.180 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.820 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21091 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3107 _reflns_number_gt 2649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+2.2937P] 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 3107 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5023(5) 0.4339(3) 0.6480(2) 0.0246(8) Uani 1 1 d . . . H1 H 0.4508 0.4525 0.5992 0.029 Uiso 1 1 calc R . . C2 C 0.4817(5) 0.4920(3) 0.7149(2) 0.0290(9) Uani 1 1 d . . . H2 H 0.4166 0.5558 0.7203 0.035 Uiso 1 1 calc R . . C3 C 0.5749(5) 0.4378(3) 0.7713(2) 0.0235(8) Uani 1 1 d . . . H3 H 0.5862 0.4560 0.8241 0.028 Uiso 1 1 calc R . . C4 C 1.0810(4) 0.2299(3) 0.6478(2) 0.0193(7) Uani 1 1 d . . . H4 H 1.1243 0.2146 0.5993 0.023 Uiso 1 1 calc R . . C5 C 1.1830(5) 0.2516(3) 0.7148(2) 0.0203(7) Uani 1 1 d . . . H5 H 1.3045 0.2537 0.7203 0.024 Uiso 1 1 calc R . . C6 C 1.0709(4) 0.2688(3) 0.7704(2) 0.0175(7) Uani 1 1 d . . . H6 H 1.0992 0.2856 0.8226 0.021 Uiso 1 1 calc R . . C7 C 0.5127(4) 0.0403(3) 0.7140(2) 0.0179(7) Uani 1 1 d . . . H7 H 0.4593 -0.0058 0.6764 0.022 Uiso 1 1 calc R . . C8 C 0.5028(5) 0.0266(3) 0.7927(2) 0.0216(8) Uani 1 1 d . . . H8 H 0.4445 -0.0288 0.8181 0.026 Uiso 1 1 calc R . . C9 C 0.5953(4) 0.1103(3) 0.8256(2) 0.0188(7) Uani 1 1 d . . . H9 H 0.6131 0.1251 0.8788 0.023 Uiso 1 1 calc R . . C10 C 0.7498(4) 0.2671(3) 0.7723(2) 0.0154(7) Uani 1 1 d . . . H10 H 0.7735 0.2853 0.8276 0.019 Uiso 1 1 calc R . . C11 C 0.8126(5) 0.0669(3) 0.4685(2) 0.0269(8) Uani 1 1 d . . . H11A H 0.7138 0.0861 0.4341 0.040 Uiso 1 1 calc R . . H11B H 0.8513 -0.0058 0.4563 0.040 Uiso 1 1 calc R . . H11C H 0.9056 0.1183 0.4619 0.040 Uiso 1 1 calc R . . C12 C 0.8405(5) 0.4016(3) 0.5070(2) 0.0283(9) Uani 1 1 d . . . H12A H 0.7860 0.4522 0.5410 0.042 Uiso 1 1 calc R . . H12B H 0.8411 0.4324 0.4554 0.042 Uiso 1 1 calc R . . H12C H 0.9585 0.3880 0.5266 0.042 Uiso 1 1 calc R . . N1 N 0.6027(4) 0.3494(2) 0.66103(16) 0.0181(6) Uani 1 1 d . . . N2 N 0.6481(4) 0.3529(2) 0.73685(16) 0.0162(6) Uani 1 1 d . . . N3 N 0.9153(4) 0.2339(2) 0.66140(16) 0.0180(6) Uani 1 1 d . . . N4 N 0.9121(4) 0.2572(2) 0.73699(16) 0.0158(6) Uani 1 1 d . . . N5 N 0.6059(4) 0.1256(2) 0.69804(16) 0.0160(6) Uani 1 1 d . . . N6 N 0.6556(4) 0.1672(2) 0.76755(15) 0.0154(6) Uani 1 1 d . . . O1 O 0.7644(3) 0.0699(2) 0.54610(14) 0.0212(6) Uani 1 1 d . . . O2 O 0.7473(4) 0.3027(2) 0.50408(16) 0.0215(6) Uani 1 1 d . . . O3 O 0.4330(3) 0.1946(2) 0.55039(14) 0.0197(6) Uani 1 1 d . . . O4 O 0.4453(4) 0.3043(2) 0.43567(15) 0.0247(6) Uani 1 1 d . . . O5 O 0.3874(4) 0.1161(2) 0.42397(14) 0.0268(6) Uani 1 1 d . . . H5A H 0.3394 0.0627 0.4429 0.040 Uiso 1 1 calc R . . O6 O 0.1761(3) 0.2336(2) 0.47278(16) 0.0296(7) Uani 1 1 d . . . S1 S 0.35836(11) 0.21247(7) 0.47110(5) 0.0161(2) Uani 1 1 d . . . Co1 Co 0.67676(6) 0.20946(4) 0.59800(2) 0.0147(2) Uani 1 1 d . . . H2O H 0.673(6) 0.313(4) 0.476(2) 0.022 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 C1 0.0192(19) 0.0170(18) 0.037(2) 0.0052(15) -0.0034(15) 0.0006(15) C2 0.019(2) 0.0136(18) 0.055(2) -0.0032(17) 0.0037(17) 0.0001(16) C3 0.0132(18) 0.0170(18) 0.041(2) -0.0085(15) 0.0058(15) -0.0022(15) C4 0.0111(18) 0.0162(17) 0.0312(19) 0.0014(14) 0.0067(14) 0.0011(14) C5 0.0112(17) 0.0144(18) 0.035(2) 0.0016(15) 0.0013(14) -0.0001(14) C6 0.0104(17) 0.0112(16) 0.0306(18) 0.0028(13) -0.0017(13) -0.0004(13) C7 0.0104(17) 0.0132(17) 0.0301(18) -0.0020(14) 0.0006(13) -0.0020(13) C8 0.0179(19) 0.0153(18) 0.0316(19) 0.0021(14) 0.0032(14) -0.0040(14) C9 0.0142(17) 0.0203(18) 0.0222(17) 0.0020(14) 0.0033(13) -0.0014(14) C10 0.0068(16) 0.0127(16) 0.0268(17) -0.0016(13) 0.0007(13) -0.0015(13) C11 0.025(2) 0.026(2) 0.030(2) -0.0045(16) 0.0030(15) 0.0042(17) C12 0.024(2) 0.025(2) 0.036(2) 0.0046(16) 0.0018(16) -0.0113(17) N1 0.0147(15) 0.0119(14) 0.0276(15) 0.0012(11) 0.0015(11) -0.0017(12) N2 0.0100(14) 0.0126(14) 0.0263(15) -0.0025(11) 0.0029(11) -0.0010(12) N3 0.0129(15) 0.0159(15) 0.0252(15) -0.0020(12) 0.0021(12) -0.0001(12) N4 0.0116(15) 0.0140(14) 0.0216(14) -0.0006(11) 0.0002(11) -0.0011(12) N5 0.0111(14) 0.0145(14) 0.0223(14) -0.0010(11) -0.0004(11) 0.0021(12) N6 0.0115(14) 0.0129(14) 0.0217(14) -0.0005(11) 0.0001(11) 0.0012(12) O1 0.0203(14) 0.0157(12) 0.0276(13) -0.0041(10) 0.0014(10) 0.0025(11) O2 0.0169(14) 0.0187(13) 0.0285(14) 0.0034(10) -0.0002(11) -0.0056(11) O3 0.0143(13) 0.0221(13) 0.0226(13) 0.0016(10) -0.0009(10) -0.0029(10) O4 0.0238(15) 0.0212(14) 0.0285(14) 0.0061(10) -0.0045(11) -0.0057(11) O5 0.0333(16) 0.0186(13) 0.0290(14) -0.0043(11) 0.0055(11) -0.0050(12) O6 0.0141(14) 0.0416(17) 0.0330(15) 0.0069(12) -0.0002(11) 0.0067(12) S1 0.0127(5) 0.0159(5) 0.0196(5) 0.0002(3) -0.0008(3) -0.0011(3) Co1 0.0118(3) 0.0122(3) 0.0201(3) -0.00014(16) -0.00034(19) -0.00045(17) _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 C1 N1 1.323(5) . ? C1 C2 1.393(6) . ? C1 H1 0.9500 . ? C2 C3 1.368(6) . ? C2 H2 0.9500 . ? C3 N2 1.357(5) . ? C3 H3 0.9500 . ? C4 N3 1.332(5) . ? C4 C5 1.405(5) . ? C4 H4 0.9500 . ? C5 C6 1.364(5) . ? C5 H5 0.9500 . ? C6 N4 1.349(5) . ? C6 H6 0.9500 . ? C7 N5 1.324(5) . ? C7 C8 1.394(5) . ? C7 H7 0.9500 . ? C8 C9 1.374(5) . ? C8 H8 0.9500 . ? C9 N6 1.345(4) . ? C9 H9 0.9500 . ? C10 N6 1.443(4) . ? C10 N2 1.447(4) . ? C10 N4 1.449(4) . ? C10 H10 1.0000 . ? C11 O1 1.430(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 O2 1.427(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? N1 N2 1.353(4) . ? N1 Co1 2.155(3) . ? N3 N4 1.355(4) . ? N3 Co1 2.135(3) . ? N5 N6 1.356(4) . ? N5 Co1 2.137(3) . ? O1 Co1 2.090(2) . ? O2 Co1 2.110(3) . ? O2 H2O 0.75(5) . ? O3 S1 1.489(2) . ? O3 Co1 2.044(2) . ? O4 S1 1.482(3) . ? O5 S1 1.478(3) . ? O5 H5A 0.8400 . ? O6 S1 1.452(3) . ? 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 N1 C1 C2 111.3(3) . . ? N1 C1 H1 124.4 . . ? C2 C1 H1 124.4 . . ? C3 C2 C1 105.6(3) . . ? C3 C2 H2 127.2 . . ? C1 C2 H2 127.2 . . ? N2 C3 C2 106.4(3) . . ? N2 C3 H3 126.8 . . ? C2 C3 H3 126.8 . . ? N3 C4 C5 110.7(3) . . ? N3 C4 H4 124.6 . . ? C5 C4 H4 124.6 . . ? C6 C5 C4 105.5(3) . . ? C6 C5 H5 127.2 . . ? C4 C5 H5 127.2 . . ? N4 C6 C5 106.8(3) . . ? N4 C6 H6 126.6 . . ? C5 C6 H6 126.6 . . ? N5 C7 C8 111.7(3) . . ? N5 C7 H7 124.2 . . ? C8 C7 H7 124.2 . . ? C9 C8 C7 105.2(3) . . ? C9 C8 H8 127.4 . . ? C7 C8 H8 127.4 . . ? N6 C9 C8 106.3(3) . . ? N6 C9 H9 126.9 . . ? C8 C9 H9 126.9 . . ? N6 C10 N2 110.1(3) . . ? N6 C10 N4 111.1(3) . . ? N2 C10 N4 110.7(3) . . ? N6 C10 H10 108.3 . . ? N2 C10 H10 108.3 . . ? N4 C10 H10 108.3 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? O2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C1 N1 N2 105.2(3) . . ? C1 N1 Co1 136.6(3) . . ? N2 N1 Co1 117.7(2) . . ? N1 N2 C3 111.6(3) . . ? N1 N2 C10 120.1(3) . . ? C3 N2 C10 128.1(3) . . ? C4 N3 N4 104.9(3) . . ? C4 N3 Co1 137.0(2) . . ? N4 N3 Co1 118.1(2) . . ? C6 N4 N3 112.1(3) . . ? C6 N4 C10 127.9(3) . . ? N3 N4 C10 120.0(3) . . ? C7 N5 N6 104.3(3) . . ? C7 N5 Co1 137.3(2) . . ? N6 N5 Co1 118.3(2) . . ? C9 N6 N5 112.5(3) . . ? C9 N6 C10 127.5(3) . . ? N5 N6 C10 119.8(3) . . ? C11 O1 Co1 123.1(2) . . ? C12 O2 Co1 126.9(2) . . ? C12 O2 H2O 105(4) . . ? Co1 O2 H2O 112(4) . . ? S1 O3 Co1 132.16(16) . . ? S1 O5 H5A 109.5 . . ? O6 S1 O5 109.93(17) . . ? O6 S1 O4 110.17(17) . . ? O5 S1 O4 107.48(16) . . ? O6 S1 O3 109.85(16) . . ? O5 S1 O3 109.55(15) . . ? O4 S1 O3 109.83(15) . . ? O3 Co1 O1 94.04(10) . . ? O3 Co1 O2 90.74(11) . . ? O1 Co1 O2 90.54(10) . . ? O3 Co1 N3 172.00(11) . . ? O1 Co1 N3 92.54(11) . . ? O2 Co1 N3 93.75(11) . . ? O3 Co1 N5 90.49(10) . . ? O1 Co1 N5 93.39(10) . . ? O2 Co1 N5 175.79(11) . . ? N3 Co1 N5 84.56(11) . . ? O3 Co1 N1 90.48(11) . . ? O1 Co1 N1 174.43(10) . . ? O2 Co1 N1 92.65(11) . . ? N3 Co1 N1 82.70(11) . . ? N5 Co1 N1 83.31(11) . . ? 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 O5 H5A O1 0.84 1.85 2.663(4) 162.4 3_656 O2 H2O O4 0.75(5) 1.88(5) 2.584(4) 157(5) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.067 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.136 #==END===================================================== data_Compound3 _database_code_depnum_ccdc_archive 'CCDC 840091' #TrackingRef '2Cifs_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 Co N12 O2, 2(C11 H18 Co N6 O4), 6(H2 O), 6(Cl)' _chemical_formula_sum 'C44 H72 Cl6 Co3 N24 O16' _chemical_formula_weight 1582.75 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' Cl Cl 0.1484 0.1585 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.590(3) _cell_length_b 11.736(2) _cell_length_c 13.908(5) _cell_angle_alpha 108.336(13) _cell_angle_beta 105.474(13) _cell_angle_gamma 102.185(9) _cell_volume 1638.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4019 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 25.58 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 815 _exptl_absorpt_coefficient_mu 1.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7044 _exptl_absorpt_correction_T_max 0.7898 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14754 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5842 _reflns_number_gt 4331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+4.6891P] 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 5842 _refine_ls_number_parameters 430 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1614 _refine_ls_wR_factor_gt 0.1466 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 C1 C 0.6969(5) 0.2307(5) 0.5666(5) 0.0320(12) Uani 1 1 d . . . H1A H 0.6338 0.1672 0.4986 0.038 Uiso 1 1 calc R . . H1B H 0.7375 0.1875 0.6075 0.038 Uiso 1 1 calc R . . C2 C 0.3299(5) -0.0041(5) 0.2287(4) 0.0310(12) Uani 1 1 d . . . H2A H 0.2504 -0.0265 0.2398 0.037 Uiso 1 1 calc R . . H2B H 0.3426 -0.0820 0.1895 0.037 Uiso 1 1 calc R . . C10 C 0.7944(5) 0.3176(5) 0.5445(4) 0.0244(11) Uani 1 1 d . . . C11 C 0.7254(5) 0.5028(5) 0.3938(4) 0.0317(12) Uani 1 1 d . . . H11 H 0.7486 0.5620 0.3651 0.038 Uiso 1 1 calc R . . C12 C 0.6098(5) 0.3638(6) 0.4336(5) 0.0395(14) Uani 1 1 d . . . H12 H 0.5425 0.3098 0.4388 0.047 Uiso 1 1 calc R . . C13 C 0.6013(6) 0.4402(6) 0.3779(5) 0.0454(16) Uani 1 1 d . . . H13 H 0.5279 0.4488 0.3376 0.054 Uiso 1 1 calc R . . C14 C 0.9854(7) 0.2106(5) 0.4018(5) 0.0446(16) Uani 1 1 d . . . H14 H 1.0464 0.2228 0.3707 0.054 Uiso 1 1 calc R . . C15 C 0.8443(7) 0.1189(5) 0.4541(5) 0.0480(17) Uani 1 1 d . . . H15 H 0.7900 0.0599 0.4673 0.058 Uiso 1 1 calc R . . C16 C 0.9253(8) 0.0955(6) 0.4008(6) 0.057(2) Uani 1 1 d . . . H16 H 0.9373 0.0183 0.3702 0.069 Uiso 1 1 calc R . . C17 C 1.0584(5) 0.5650(5) 0.7496(4) 0.0265(11) Uani 1 1 d . . . H17 H 1.1324 0.6325 0.7742 0.032 Uiso 1 1 calc R . . C18 C 0.9008(5) 0.4237(5) 0.7492(4) 0.0241(11) Uani 1 1 d . . . H18 H 0.8458 0.3743 0.7695 0.029 Uiso 1 1 calc R . . C19 C 1.0090(5) 0.5215(5) 0.8169(4) 0.0276(11) Uani 1 1 d . . . H19 H 1.0426 0.5526 0.8923 0.033 Uiso 1 1 calc R . . C20 C 0.3229(4) 0.0767(4) 0.1609(4) 0.0215(10) Uani 1 1 d . . . C21 C 0.2722(5) 0.3717(5) 0.2384(4) 0.0296(12) Uani 1 1 d . . . H21 H 0.2661 0.4454 0.2288 0.036 Uiso 1 1 calc R . . C22 C 0.2704(5) 0.2276(6) 0.3064(4) 0.0320(13) Uani 1 1 d . . . H22 H 0.2631 0.1820 0.3496 0.038 Uiso 1 1 calc R . . C23 C 0.2548(5) 0.3427(5) 0.3224(5) 0.0366(14) Uani 1 1 d . . . H23 H 0.2361 0.3920 0.3793 0.044 Uiso 1 1 calc R . . C24 C 0.5688(5) 0.1857(5) 0.0740(4) 0.0262(11) Uani 1 1 d . . . H24 H 0.6042 0.2273 0.0367 0.031 Uiso 1 1 calc R . . C25 C 0.5467(5) 0.0770(5) 0.1746(4) 0.0277(12) Uani 1 1 d . . . H25 H 0.5597 0.0310 0.2178 0.033 Uiso 1 1 calc R . . C26 C 0.6290(5) 0.1255(5) 0.1326(4) 0.0288(12) Uani 1 1 d . . . H26 H 0.7096 0.1195 0.1415 0.035 Uiso 1 1 calc R . . C27 C 0.0874(5) -0.0257(4) -0.0965(4) 0.0235(11) Uani 1 1 d . . . H27 H 0.0457 -0.0138 -0.1578 0.028 Uiso 1 1 calc R . . C28 C 0.1360(5) -0.1146(5) 0.0195(4) 0.0266(11) Uani 1 1 d . . . H28 H 0.1369 -0.1707 0.0541 0.032 Uiso 1 1 calc R . . C29 C 0.0514(5) -0.1353(5) -0.0785(4) 0.0278(12) Uani 1 1 d . . . H29 H -0.0168 -0.2082 -0.1241 0.033 Uiso 1 1 calc R . . N11 N 0.8053(4) 0.4668(4) 0.4550(3) 0.0253(9) Uani 1 1 d . . . N12 N 0.7339(4) 0.3805(4) 0.4800(3) 0.0234(9) Uani 1 1 d . . . N14 N 0.9458(4) 0.3020(4) 0.4525(4) 0.0280(10) Uani 1 1 d . . . N15 N 0.8575(4) 0.2432(4) 0.4841(4) 0.0274(10) Uani 1 1 d . . . N17 N 0.9871(4) 0.4986(4) 0.6460(3) 0.0238(9) Uani 1 1 d . . . N18 N 0.8888(4) 0.4122(4) 0.6468(3) 0.0208(9) Uani 1 1 d . . . N21 N 0.2985(4) 0.2813(4) 0.1730(3) 0.0233(9) Uani 1 1 d . . . N22 N 0.2984(4) 0.1922(4) 0.2158(3) 0.0224(9) Uani 1 1 d . . . N24 N 0.4541(4) 0.1764(4) 0.0777(3) 0.0228(9) Uani 1 1 d . . . N25 N 0.4412(4) 0.1091(4) 0.1405(3) 0.0208(9) Uani 1 1 d . . . N27 N 0.1888(4) 0.0596(4) -0.0149(3) 0.0200(9) Uani 1 1 d . . . N28 N 0.2186(4) 0.0038(4) 0.0567(3) 0.0208(9) Uani 1 1 d . . . O1 O 0.6388(4) 0.3045(4) 0.6263(3) 0.0408(10) Uani 1 1 d . . . H1 H 0.5861 0.2587 0.6389 0.061 Uiso 1 1 calc R . . O2 O 0.4299(4) 0.0617(4) 0.3308(3) 0.0376(9) Uani 1 1 d . . . H2 H 0.4187 0.1271 0.3644 0.056 Uiso 1 1 calc R . . O10 O 0.4851(4) 0.1851(4) 0.7841(3) 0.0412(10) Uani 1 1 d D . . O20 O 0.1845(4) 0.2631(4) 0.6923(4) 0.0500(11) Uani 1 1 d D . . O21 O 0.2996(4) 0.1840(4) -0.1407(3) 0.0416(10) Uani 1 1 d . . . O22 O 0.1481(3) 0.3062(3) -0.0297(3) 0.0338(9) Uani 1 1 d . . . O23 O 0.4220(4) 0.4234(4) 0.0669(4) 0.0437(11) Uani 1 1 d . . . O30 O 0.3286(4) 0.5049(4) 0.8519(3) 0.0402(10) Uani 1 1 d . . . Co1 Co 1.0000 0.5000 0.5000 0.0198(2) Uani 1 2 d S . . Co2 Co 0.30604(6) 0.24218(6) 0.01719(5) 0.02201(19) Uani 1 1 d . . . Cl1 Cl 0.35139(13) 0.15470(14) 0.53883(11) 0.0389(4) Uani 1 1 d . . . Cl2 Cl 0.25831(11) 0.60930(11) 0.06349(9) 0.0244(3) Uani 1 1 d . . . Cl3 Cl 0.95068(12) 0.13970(11) 0.73642(10) 0.0256(3) Uani 1 1 d . . . H21A H 0.2583 0.2311 -0.1756 0.038 Uiso 1 1 d . . . H21C H 0.3847 0.2008 -0.1407 0.038 Uiso 1 1 d . . . H22B H 0.0944 0.2516 -0.1037 0.038 Uiso 1 1 d . . . H22C H 0.1783 0.3913 -0.0254 0.038 Uiso 1 1 d . . . H10A H 0.456(5) 0.178(6) 0.718(2) 0.038 Uiso 1 1 d D . . H10B H 0.538(5) 0.260(3) 0.825(4) 0.038 Uiso 1 1 d D . . H20A H 0.200(6) 0.221(5) 0.638(3) 0.038 Uiso 1 1 d D . . H20B H 0.1077 0.2266 0.6937 0.038 Uiso 1 1 d . . . H23A H 0.3922 0.4846 0.0538 0.038 Uiso 1 1 d . . . H23B H 0.5109 0.4565 0.1048 0.038 Uiso 1 1 d . . . H30A H 0.2988 0.5256 0.9022 0.038 Uiso 1 1 d . . . H30B H 0.2967 0.4256 0.8236 0.038 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 C1 0.031(3) 0.029(3) 0.034(3) 0.009(2) 0.016(3) 0.003(2) C2 0.028(3) 0.032(3) 0.029(3) 0.015(2) 0.006(2) 0.005(2) C10 0.025(3) 0.022(2) 0.027(3) 0.008(2) 0.011(2) 0.008(2) C11 0.031(3) 0.031(3) 0.030(3) 0.015(2) 0.004(2) 0.007(2) C12 0.022(3) 0.041(3) 0.039(3) 0.016(3) -0.004(2) -0.003(2) C13 0.024(3) 0.057(4) 0.044(4) 0.023(3) -0.003(3) 0.004(3) C14 0.065(4) 0.026(3) 0.059(4) 0.014(3) 0.045(4) 0.020(3) C15 0.076(5) 0.016(3) 0.058(4) 0.011(3) 0.041(4) 0.010(3) C16 0.096(6) 0.021(3) 0.073(5) 0.012(3) 0.061(5) 0.024(3) C17 0.025(3) 0.021(2) 0.026(3) 0.003(2) 0.005(2) 0.007(2) C18 0.030(3) 0.026(3) 0.028(3) 0.015(2) 0.016(2) 0.017(2) C19 0.030(3) 0.032(3) 0.022(3) 0.010(2) 0.006(2) 0.016(2) C20 0.015(2) 0.019(2) 0.023(3) 0.004(2) 0.004(2) 0.0016(19) C21 0.023(3) 0.022(3) 0.035(3) 0.000(2) 0.009(2) 0.010(2) C22 0.023(3) 0.045(3) 0.022(3) 0.008(2) 0.009(2) 0.007(2) C23 0.029(3) 0.039(3) 0.032(3) -0.001(3) 0.012(3) 0.012(3) C24 0.018(3) 0.024(3) 0.036(3) 0.009(2) 0.014(2) 0.006(2) C25 0.025(3) 0.023(3) 0.031(3) 0.009(2) 0.003(2) 0.010(2) C26 0.017(3) 0.025(3) 0.039(3) 0.008(2) 0.008(2) 0.008(2) C27 0.023(3) 0.023(2) 0.026(3) 0.007(2) 0.010(2) 0.014(2) C28 0.027(3) 0.019(2) 0.032(3) 0.009(2) 0.009(2) 0.006(2) C29 0.024(3) 0.020(2) 0.030(3) 0.003(2) 0.007(2) 0.004(2) N11 0.027(2) 0.024(2) 0.026(2) 0.0092(19) 0.0131(19) 0.0063(18) N12 0.023(2) 0.021(2) 0.022(2) 0.0052(18) 0.0079(18) 0.0039(17) N14 0.035(3) 0.018(2) 0.034(2) 0.0065(19) 0.021(2) 0.0079(18) N15 0.035(3) 0.017(2) 0.034(2) 0.0076(19) 0.022(2) 0.0067(18) N17 0.023(2) 0.019(2) 0.027(2) 0.0057(18) 0.0098(19) 0.0044(17) N18 0.023(2) 0.020(2) 0.019(2) 0.0065(17) 0.0078(18) 0.0066(17) N21 0.020(2) 0.019(2) 0.029(2) 0.0070(18) 0.0088(18) 0.0060(17) N22 0.018(2) 0.024(2) 0.021(2) 0.0053(18) 0.0079(18) 0.0047(17) N24 0.024(2) 0.020(2) 0.027(2) 0.0105(18) 0.0119(19) 0.0084(17) N25 0.020(2) 0.0180(19) 0.026(2) 0.0084(17) 0.0092(18) 0.0086(16) N27 0.022(2) 0.0165(19) 0.022(2) 0.0067(17) 0.0064(18) 0.0090(17) N28 0.020(2) 0.0169(19) 0.021(2) 0.0056(17) 0.0058(17) 0.0038(16) O1 0.034(2) 0.044(2) 0.043(2) 0.013(2) 0.0223(19) 0.0043(18) O2 0.033(2) 0.037(2) 0.032(2) 0.0111(18) 0.0021(18) 0.0081(18) O10 0.049(3) 0.039(2) 0.031(2) 0.016(2) 0.011(2) 0.008(2) O20 0.050(3) 0.036(2) 0.051(3) 0.012(2) 0.014(2) 0.003(2) O21 0.051(3) 0.052(3) 0.035(2) 0.024(2) 0.016(2) 0.030(2) O22 0.028(2) 0.0225(18) 0.045(2) 0.0117(17) 0.0062(18) 0.0092(16) O23 0.023(2) 0.029(2) 0.077(3) 0.032(2) 0.004(2) 0.0054(16) O30 0.031(2) 0.042(2) 0.039(2) 0.0094(19) 0.0124(18) 0.0056(18) Co1 0.0219(5) 0.0144(4) 0.0228(5) 0.0052(4) 0.0107(4) 0.0054(4) Co2 0.0200(4) 0.0192(3) 0.0271(4) 0.0096(3) 0.0077(3) 0.0070(3) Cl1 0.0313(7) 0.0477(8) 0.0284(7) 0.0166(6) 0.0078(6) -0.0038(6) Cl2 0.0265(6) 0.0231(6) 0.0203(6) 0.0064(5) 0.0056(5) 0.0084(5) Cl3 0.0304(7) 0.0263(6) 0.0299(7) 0.0159(5) 0.0139(5) 0.0169(5) _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 C1 O1 1.409(7) . ? C1 C10 1.520(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 O2 1.418(6) . ? C2 C20 1.533(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C10 N18 1.454(6) . ? C10 N15 1.462(6) . ? C10 N12 1.462(7) . ? C11 N11 1.316(7) . ? C11 C13 1.392(8) . ? C11 H11 0.9300 . ? C12 N12 1.353(7) . ? C12 C13 1.359(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 N14 1.329(7) . ? C14 C16 1.377(8) . ? C14 H14 0.9300 . ? C15 N15 1.348(7) . ? C15 C16 1.363(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 N17 1.324(6) . ? C17 C19 1.389(7) . ? C17 H17 0.9300 . ? C18 N18 1.353(6) . ? C18 C19 1.364(7) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 N22 1.459(6) . ? C20 N28 1.464(6) . ? C20 N25 1.470(6) . ? C21 N21 1.313(6) . ? C21 C23 1.368(8) . ? C21 H21 0.9300 . ? C22 N22 1.346(7) . ? C22 C23 1.357(8) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 N24 1.327(6) . ? C24 C26 1.384(7) . ? C24 H24 0.9300 . ? C25 C26 1.361(7) . ? C25 N25 1.363(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 N27 1.322(6) . ? C27 C29 1.387(7) . ? C27 H27 0.9300 . ? C28 N28 1.356(6) . ? C28 C29 1.362(7) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? N11 N12 1.362(5) . ? N11 Co1 2.088(4) . ? N14 N15 1.360(6) . ? N14 Co1 2.104(4) . ? N17 N18 1.361(5) . ? N17 Co1 2.080(4) . ? N21 N22 1.357(6) . ? N21 Co2 2.099(4) . ? N24 N25 1.365(5) . ? N24 Co2 2.109(4) . ? N27 N28 1.365(5) . ? N27 Co2 2.117(4) . ? O1 H1 0.8200 . ? O2 H2 0.8200 . ? O10 H10A 0.87(5) . ? O10 H10B 0.86(5) . ? O20 H20A 0.85(5) . ? O20 H20B 0.910 . ? O21 Co2 2.059(4) . ? O21 H21A 0.964 . ? O21 H21C 0.964 . ? O22 Co2 2.143(4) . ? O22 H22B 0.965 . ? O22 H22C 0.964 . ? O23 Co2 2.044(4) . ? O23 H23A 0.907 . ? O23 H23B 0.950 . ? O30 H30A 0.852 . ? O30 H30B 0.839 . ? Co1 N17 2.080(4) 2_766 ? Co1 N11 2.088(4) 2_766 ? Co1 N14 2.104(4) 2_766 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C10 108.5(4) . . ? O1 C1 H1A 110.0 . . ? C10 C1 H1A 110.0 . . ? O1 C1 H1B 110.0 . . ? C10 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? O2 C2 C20 111.4(4) . . ? O2 C2 H2A 109.4 . . ? C20 C2 H2A 109.4 . . ? O2 C2 H2B 109.4 . . ? C20 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? N18 C10 N15 108.7(4) . . ? N18 C10 N12 109.8(4) . . ? N15 C10 N12 108.6(4) . . ? N18 C10 C1 109.6(4) . . ? N15 C10 C1 109.5(4) . . ? N12 C10 C1 110.6(4) . . ? N11 C11 C13 110.6(5) . . ? N11 C11 H11 124.7 . . ? C13 C11 H11 124.7 . . ? N12 C12 C13 107.6(5) . . ? N12 C12 H12 126.2 . . ? C13 C12 H12 126.2 . . ? C12 C13 C11 105.6(5) . . ? C12 C13 H13 127.2 . . ? C11 C13 H13 127.2 . . ? N14 C14 C16 111.7(5) . . ? N14 C14 H14 124.1 . . ? C16 C14 H14 124.1 . . ? N15 C15 C16 107.2(5) . . ? N15 C15 H15 126.4 . . ? C16 C15 H15 126.4 . . ? C15 C16 C14 105.4(5) . . ? C15 C16 H16 127.3 . . ? C14 C16 H16 127.3 . . ? N17 C17 C19 111.6(5) . . ? N17 C17 H17 124.2 . . ? C19 C17 H17 124.2 . . ? N18 C18 C19 106.9(4) . . ? N18 C18 H18 126.6 . . ? C19 C18 H18 126.6 . . ? C18 C19 C17 105.4(5) . . ? C18 C19 H19 127.3 . . ? C17 C19 H19 127.3 . . ? N22 C20 N28 108.2(4) . . ? N22 C20 N25 109.9(4) . . ? N28 C20 N25 108.8(4) . . ? N22 C20 C2 110.6(4) . . ? N28 C20 C2 108.8(4) . . ? N25 C20 C2 110.4(4) . . ? N21 C21 C23 110.8(5) . . ? N21 C21 H21 124.6 . . ? C23 C21 H21 124.6 . . ? N22 C22 C23 106.7(5) . . ? N22 C22 H22 126.6 . . ? C23 C22 H22 126.6 . . ? C22 C23 C21 106.4(5) . . ? C22 C23 H23 126.8 . . ? C21 C23 H23 126.8 . . ? N24 C24 C26 111.4(5) . . ? N24 C24 H24 124.3 . . ? C26 C24 H24 124.3 . . ? C26 C25 N25 106.2(4) . . ? C26 C25 H25 126.9 . . ? N25 C25 H25 126.9 . . ? C25 C26 C24 106.3(5) . . ? C25 C26 H26 126.8 . . ? C24 C26 H26 126.8 . . ? N27 C27 C29 111.1(5) . . ? N27 C27 H27 124.4 . . ? C29 C27 H27 124.4 . . ? N28 C28 C29 106.6(4) . . ? N28 C28 H28 126.7 . . ? C29 C28 H28 126.7 . . ? C28 C29 C27 106.1(4) . . ? C28 C29 H29 126.9 . . ? C27 C29 H29 126.9 . . ? C11 N11 N12 106.3(4) . . ? C11 N11 Co1 133.6(4) . . ? N12 N11 Co1 119.7(3) . . ? C12 N12 N11 109.9(4) . . ? C12 N12 C10 129.9(4) . . ? N11 N12 C10 120.1(4) . . ? C14 N14 N15 104.6(4) . . ? C14 N14 Co1 135.0(4) . . ? N15 N14 Co1 120.1(3) . . ? C15 N15 N14 111.0(4) . . ? C15 N15 C10 129.6(4) . . ? N14 N15 C10 119.3(4) . . ? C17 N17 N18 104.8(4) . . ? C17 N17 Co1 134.7(3) . . ? N18 N17 Co1 120.6(3) . . ? C18 N18 N17 111.3(4) . . ? C18 N18 C10 129.0(4) . . ? N17 N18 C10 119.5(4) . . ? C21 N21 N22 105.8(4) . . ? C21 N21 Co2 132.9(4) . . ? N22 N21 Co2 120.2(3) . . ? C22 N22 N21 110.3(4) . . ? C22 N22 C20 129.9(4) . . ? N21 N22 C20 119.8(4) . . ? C24 N24 N25 104.7(4) . . ? C24 N24 Co2 136.0(3) . . ? N25 N24 Co2 119.2(3) . . ? C25 N25 N24 111.3(4) . . ? C25 N25 C20 128.2(4) . . ? N24 N25 C20 120.5(4) . . ? C27 N27 N28 105.2(4) . . ? C27 N27 Co2 134.9(3) . . ? N28 N27 Co2 119.9(3) . . ? C28 N28 N27 111.0(4) . . ? C28 N28 C20 129.4(4) . . ? N27 N28 C20 119.4(4) . . ? C1 O1 H1 109.5 . . ? C2 O2 H2 109.5 . . ? H10A O10 H10B 110(6) . . ? H20A O20 H20B 114 . . ? Co2 O21 H21A 109.2 . . ? Co2 O21 H21C 109.2 . . ? H21A O21 H21C 108.8 . . ? Co2 O22 H22B 109.3 . . ? Co2 O22 H22C 109.3 . . ? H22B O22 H22C 108.7 . . ? Co2 O23 H23A 122.0 . . ? Co2 O23 H23B 127.7 . . ? H23A O23 H23B 110.3 . . ? H30A O30 H30B 102.6 . . ? N17 Co1 N17 179.999(1) 2_766 . ? N17 Co1 N11 83.43(16) 2_766 2_766 ? N17 Co1 N11 96.57(16) . 2_766 ? N17 Co1 N11 96.57(16) 2_766 . ? N17 Co1 N11 83.43(16) . . ? N11 Co1 N11 180.0(2) 2_766 . ? N17 Co1 N14 83.31(16) 2_766 2_766 ? N17 Co1 N14 96.69(16) . 2_766 ? N11 Co1 N14 82.99(17) 2_766 2_766 ? N11 Co1 N14 97.01(17) . 2_766 ? N17 Co1 N14 96.69(16) 2_766 . ? N17 Co1 N14 83.30(16) . . ? N11 Co1 N14 97.01(17) 2_766 . ? N11 Co1 N14 82.99(17) . . ? N14 Co1 N14 180.0 2_766 . ? O23 Co2 O21 95.80(18) . . ? O23 Co2 N21 90.57(17) . . ? O21 Co2 N21 173.62(16) . . ? O23 Co2 N24 94.23(15) . . ? O21 Co2 N24 97.18(16) . . ? N21 Co2 N24 82.59(16) . . ? O23 Co2 N27 173.28(17) . . ? O21 Co2 N27 90.85(16) . . ? N21 Co2 N27 82.78(15) . . ? N24 Co2 N27 83.95(15) . . ? O23 Co2 O22 88.19(14) . . ? O21 Co2 O22 88.76(16) . . ? N21 Co2 O22 91.17(16) . . ? N24 Co2 O22 173.32(15) . . ? N27 Co2 O22 92.93(14) . . ? 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 O1 H1 Cl1 0.82 2.52 3.112(4) 131.0 . O2 H2 Cl1 0.82 2.69 3.198(4) 122.0 . O21 H21A O20 0.964 1.995 2.875(6) 150.9(3) 1_554 O21 H21C O10 0.964 1.762 2.630(6) 148.1(3) 1_554 O22 H22B Cl3 0.965 2.1698 3.127(4) 171.1(2) 1_454 O22 H22C Cl2 0.964 2.3086 3.204(4) 154.0 . O10 H10A Cl1 0.87(2) 2.36(2) 3.216(4) 172(6) . O10 H10B Cl2 0.86(5) 2.31(4) 3.090(5) 150(6) 2_666 O20 H20A Cl1 0.85(5) 2.60(7) 3.384(5) 153(6) . O20 H20B Cl3 0.910 2.2092 3.099(5) 165.6(3) 1_455 O23 H23A Cl2 0.907 2.3483 3.183(4) 153.0 . O23 H23B O30 0.950 1.704 2.640(5) 167.9(3) 2_666 O30 H30A Cl2 0.852 2.3630 3.202(4) 168.5(3) 1_556 O30 H30B O20 0.839 2.039 2.798(6) 150.0 . _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 2.113 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.111