# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Jie Zhang' _publ_contact_author_address ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; _publ_contact_author_email zhangjie@fjirsm.ac.cn _publ_contact_author_phone 86-591-83792871 _publ_contact_author_fax 86-591-83710051 _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; This CIF will be submitted for publication as a communication in 'Chem. Commun.' ; # 2.AUTHOR LIST loop_ _publ_author_name _publ_author_address 'Hong-Peng Jia' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Wei Li' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Zhan-Feng Ju' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Jie Zhang' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; # Attachment 'Mn-hpdc-jhp_.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 661336' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H14 Mn3 N4 O16, 2(H2 O)' _chemical_formula_sum 'C12 H18 Mn3 N4 O18' _chemical_formula_weight 671.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 7.499(4) _cell_length_b 9.246(5) _cell_length_c 9.374(5) _cell_angle_alpha 112.158(2) _cell_angle_beta 107.435(4) _cell_angle_gamma 100.623(4) _cell_volume 540.8(5) _cell_formula_units_Z 1 _cell_measurement_temperature 294 _cell_measurement_reflns_used 1664 _cell_measurement_theta_min 2.5257 _cell_measurement_theta_max 27.4410 _exptl_crystal_description Prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 337 _exptl_absorpt_coefficient_mu 1.826 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5757 _exptl_absorpt_correction_T_max 0.8244 _exptl_absorpt_process_details 'CrystalClear (Rigaku/MSC Inc., 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_measurement_device_type 'Saturn70 (4x4 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4202 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.45 _reflns_number_total 2410 _reflns_number_gt 2149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+0.2844P] 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 2410 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.10955(5) 0.74916(4) -0.22562(4) 0.02055(13) Uani 1 1 d . . . Mn2 Mn 0.0000 0.5000 -1.0000 0.01929(14) Uani 1 2 d S . . O1 O 0.1945(3) 1.0119(2) -0.15382(19) 0.0295(4) Uani 1 1 d . . . O2 O 0.3279(3) 1.2099(2) -0.2072(2) 0.0386(5) Uani 1 1 d . . . O3 O 0.3315(3) 1.0092(2) -0.8018(2) 0.0315(4) Uani 1 1 d . . . O4 O 0.1409(3) 0.74630(19) -0.98359(19) 0.0261(4) Uani 1 1 d . . . O5 O -0.0471(3) 0.50871(19) -0.6605(2) 0.0337(4) Uani 1 1 d . . . N1 N 0.1121(3) 0.7760(2) -0.4586(2) 0.0186(4) Uani 1 1 d . . . N2 N 0.1016(3) 0.6860(2) -0.7361(2) 0.0177(4) Uani 1 1 d . . . C1 C 0.2455(3) 1.0623(3) -0.2469(3) 0.0216(4) Uani 1 1 d . . . C2 C 0.2011(3) 0.9319(2) -0.4241(2) 0.0170(4) Uani 1 1 d . . . C3 C 0.2458(3) 0.9732(2) -0.5392(3) 0.0195(4) Uani 1 1 d . . . H3 H 0.3093 1.0847 -0.5121 0.023 Uiso 1 1 calc R . . C4 C 0.1929(3) 0.8431(2) -0.6963(2) 0.0166(4) Uani 1 1 d . . . C5 C 0.2266(3) 0.8706(3) -0.8373(3) 0.0204(4) Uani 1 1 d . . . C6 C 0.0556(3) 0.6531(3) -0.6190(2) 0.0193(4) Uani 1 1 d . . . O1W O 0.4266(3) 0.7697(2) -0.1442(2) 0.0322(4) Uani 1 1 d . . . H1 H 0.5039 0.8463 -0.1484 0.039 Uiso 1 1 d R . . H2 H 0.4756 0.7740 -0.0478 0.039 Uiso 1 1 d R . . O2W O -0.2041(3) 0.7163(3) -0.2850(3) 0.0459(5) Uani 1 1 d . . . H4 H -0.2264 0.8052 -0.2369 0.055 Uiso 1 1 d R . . H5 H -0.2421 0.6843 -0.3903 0.055 Uiso 1 1 d R . . O3W O 0.2836(3) 0.4605(3) -0.9562(3) 0.0506(6) Uani 1 1 d . . . H6 H 0.3879 0.5004 -0.8662 0.061 Uiso 1 1 d R . . H7 H 0.2861 0.3783 -1.0360 0.061 Uiso 1 1 d R . . O4W O 0.4072(4) 1.4207(3) -0.3689(4) 0.0817(10) Uani 1 1 d . . . H9 H 0.3286 1.4548 -0.3261 0.098 Uiso 1 1 d R . . H8 H 0.4895 1.4913 -0.3764 0.098 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0304(2) 0.01667(18) 0.01426(18) 0.00781(13) 0.00973(14) 0.00459(14) Mn2 0.0299(3) 0.0149(2) 0.0117(2) 0.00440(17) 0.00989(18) 0.00598(18) O1 0.0532(11) 0.0199(7) 0.0150(7) 0.0071(6) 0.0165(7) 0.0086(7) O2 0.0661(13) 0.0159(8) 0.0280(9) 0.0037(7) 0.0266(9) 0.0025(8) O3 0.0467(10) 0.0222(8) 0.0265(9) 0.0121(7) 0.0206(8) 0.0018(7) O4 0.0443(9) 0.0202(7) 0.0138(7) 0.0077(6) 0.0149(7) 0.0059(7) O5 0.0605(12) 0.0148(7) 0.0196(8) 0.0059(6) 0.0182(8) 0.0004(7) N1 0.0284(9) 0.0152(8) 0.0111(8) 0.0057(6) 0.0084(7) 0.0054(7) N2 0.0260(9) 0.0153(8) 0.0106(8) 0.0054(6) 0.0075(7) 0.0055(7) C1 0.0294(11) 0.0173(9) 0.0147(9) 0.0051(8) 0.0076(8) 0.0078(8) C2 0.0219(9) 0.0153(9) 0.0116(9) 0.0054(7) 0.0058(7) 0.0054(7) C3 0.0278(10) 0.0141(9) 0.0138(9) 0.0062(8) 0.0081(8) 0.0025(8) C4 0.0222(9) 0.0170(9) 0.0125(9) 0.0079(8) 0.0084(8) 0.0061(8) C5 0.0283(11) 0.0204(10) 0.0170(10) 0.0103(8) 0.0127(8) 0.0084(8) C6 0.0296(11) 0.0154(9) 0.0117(9) 0.0065(8) 0.0076(8) 0.0055(8) O1W 0.0284(8) 0.0345(9) 0.0312(9) 0.0157(8) 0.0110(7) 0.0057(7) O2W 0.0409(11) 0.0391(11) 0.0604(14) 0.0207(10) 0.0264(10) 0.0146(9) O3W 0.0412(11) 0.0570(13) 0.0281(10) -0.0036(9) 0.0042(8) 0.0294(10) O4W 0.0540(15) 0.0611(16) 0.079(2) -0.0015(15) 0.0054(14) 0.0208(13) _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 O5 2.1006(19) 2_564 ? Mn1 O1 2.167(2) . ? Mn1 O2W 2.182(2) . ? Mn1 O1W 2.215(2) . ? Mn1 O4 2.2208(19) 1_556 ? Mn1 N1 2.294(2) . ? Mn2 O3W 2.168(2) . ? Mn2 O3W 2.168(2) 2_563 ? Mn2 N2 2.1992(19) 2_563 ? Mn2 N2 2.1992(19) . ? Mn2 O4 2.2532(19) . ? Mn2 O4 2.2532(19) 2_563 ? O1 C1 1.252(3) . ? O2 C1 1.245(3) . ? O3 C5 1.233(3) . ? O4 C5 1.275(3) . ? O4 Mn1 2.2208(19) 1_554 ? O5 C6 1.256(3) . ? O5 Mn1 2.1006(19) 2_564 ? N1 C2 1.339(3) . ? N1 C6 1.372(3) . ? N2 C4 1.338(3) . ? N2 C6 1.362(3) . ? C1 C2 1.527(3) . ? C2 C3 1.379(3) . ? C3 C4 1.383(3) . ? C3 H3 0.9500 . ? C4 C5 1.518(3) . ? O1W H1 0.8500 . ? O1W H2 0.8499 . ? O2W H4 0.8500 . ? O2W H5 0.8500 . ? O3W H6 0.8500 . ? O3W H7 0.8499 . ? O4W H9 0.8500 . ? O4W H8 0.8500 . ? 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 O5 Mn1 O1 167.04(7) 2_564 . ? O5 Mn1 O2W 91.18(8) 2_564 . ? O1 Mn1 O2W 94.29(8) . . ? O5 Mn1 O1W 86.17(7) 2_564 . ? O1 Mn1 O1W 89.64(7) . . ? O2W Mn1 O1W 173.08(8) . . ? O5 Mn1 O4 89.32(6) 2_564 1_556 ? O1 Mn1 O4 102.50(6) . 1_556 ? O2W Mn1 O4 88.98(8) . 1_556 ? O1W Mn1 O4 84.60(7) . 1_556 ? O5 Mn1 N1 94.81(7) 2_564 . ? O1 Mn1 N1 72.95(6) . . ? O2W Mn1 N1 96.06(8) . . ? O1W Mn1 N1 90.54(7) . . ? O4 Mn1 N1 173.41(6) 1_556 . ? O3W Mn2 O3W 180.000(1) . 2_563 ? O3W Mn2 N2 87.47(7) . 2_563 ? O3W Mn2 N2 92.53(7) 2_563 2_563 ? O3W Mn2 N2 92.53(7) . . ? O3W Mn2 N2 87.47(7) 2_563 . ? N2 Mn2 N2 180.000(1) 2_563 . ? O3W Mn2 O4 88.87(9) . . ? O3W Mn2 O4 91.13(9) 2_563 . ? N2 Mn2 O4 106.46(7) 2_563 . ? N2 Mn2 O4 73.54(7) . . ? O3W Mn2 O4 91.13(9) . 2_563 ? O3W Mn2 O4 88.87(9) 2_563 2_563 ? N2 Mn2 O4 73.54(7) 2_563 2_563 ? N2 Mn2 O4 106.46(7) . 2_563 ? O4 Mn2 O4 180.00(9) . 2_563 ? C1 O1 Mn1 119.45(14) . . ? C5 O4 Mn1 126.44(14) . 1_554 ? C5 O4 Mn2 117.04(14) . . ? Mn1 O4 Mn2 116.50(7) 1_554 . ? C6 O5 Mn1 151.48(17) . 2_564 ? C2 N1 C6 117.78(18) . . ? C2 N1 Mn1 113.40(13) . . ? C6 N1 Mn1 128.37(14) . . ? C4 N2 C6 118.98(18) . . ? C4 N2 Mn2 116.89(14) . . ? C6 N2 Mn2 123.63(14) . . ? O2 C1 O1 125.3(2) . . ? O2 C1 C2 117.5(2) . . ? O1 C1 C2 117.12(19) . . ? N1 C2 C3 123.23(19) . . ? N1 C2 C1 114.46(18) . . ? C3 C2 C1 122.30(18) . . ? C2 C3 C4 116.22(19) . . ? C2 C3 H3 121.9 . . ? C4 C3 H3 121.9 . . ? N2 C4 C3 122.25(19) . . ? N2 C4 C5 115.71(18) . . ? C3 C4 C5 121.98(18) . . ? O3 C5 O4 125.9(2) . . ? O3 C5 C4 118.07(19) . . ? O4 C5 C4 116.01(19) . . ? O5 C6 N2 119.31(18) . . ? O5 C6 N1 119.2(2) . . ? N2 C6 N1 121.38(19) . . ? Mn1 O1W H1 116.7 . . ? Mn1 O1W H2 113.0 . . ? H1 O1W H2 109.4 . . ? Mn1 O2W H4 114.0 . . ? Mn1 O2W H5 97.6 . . ? H4 O2W H5 111.2 . . ? Mn2 O3W H6 131.0 . . ? Mn2 O3W H7 115.7 . . ? H6 O3W H7 112.1 . . ? H9 O4W H8 117.0 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.431 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.081 data_2: _database_code_depnum_ccdc_archive 'CCDC 661337' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H14 Co3 N4 O16, 2(H2 O)' _chemical_formula_sum 'C12 H18 Co3 N4 O18' _chemical_formula_weight 683.1 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 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 7.3879(19) _cell_length_b 9.073(2) _cell_length_c 9.1324(18) _cell_angle_alpha 112.463(5) _cell_angle_beta 106.946(6) _cell_angle_gamma 99.518(5) _cell_volume 513.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293 _cell_measurement_reflns_used 1379 _cell_measurement_theta_min 4.8534 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 343 _exptl_absorpt_coefficient_mu 2.499 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6349 _exptl_absorpt_correction_T_max 0.7882 _exptl_absorpt_process_details 'CrystalClear (Rigaku/MSC Inc., 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 3973 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.93 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2312 _reflns_number_gt 1975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2000)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0701P)^2^+0.1051P] 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 2312 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.11529(6) 0.24776(4) -0.22632(4) 0.01823(15) Uani 1 1 d . . . Co2 Co 0.0000 0.0000 -1.0000 0.01605(16) Uani 1 2 d S . . O1 O 0.1884(3) 0.5061(3) -0.1439(3) 0.0254(5) Uani 1 1 d . . . O2 O 0.3236(4) 0.7060(3) -0.1990(3) 0.0325(6) Uani 1 1 d . . . O3 O 0.3325(4) 0.4969(3) -0.8069(3) 0.0300(5) Uani 1 1 d . . . O4 O 0.1404(3) 0.2323(3) -0.9923(2) 0.0231(5) Uani 1 1 d . . . O5 O -0.0706(3) 0.0029(2) -0.6606(3) 0.0251(5) Uani 1 1 d . . . N1 N 0.1034(3) 0.2696(3) -0.4552(3) 0.0166(5) Uani 1 1 d . . . N2 N 0.0911(3) 0.1750(3) -0.7405(3) 0.0162(5) Uani 1 1 d . . . C1 C 0.2414(4) 0.5579(3) -0.2397(3) 0.0191(6) Uani 1 1 d . . . C2 C 0.1971(4) 0.4249(3) -0.4205(3) 0.0162(5) Uani 1 1 d . . . C3 C 0.2438(4) 0.4647(3) -0.5389(3) 0.0187(6) Uani 1 1 d . . . H3 H 0.3097 0.5764 -0.5121 0.022 Uiso 1 1 calc R . . C4 C 0.1887(4) 0.3313(3) -0.6997(3) 0.0168(5) Uani 1 1 d . . . C5 C 0.2263(4) 0.3581(3) -0.8435(3) 0.0187(6) Uani 1 1 d . . . C6 C 0.0399(4) 0.1440(3) -0.6205(3) 0.0171(6) Uani 1 1 d . . . O1W O 0.4227(3) 0.2713(3) -0.1521(3) 0.0275(5) Uani 1 1 d . . . H2 H 0.4665 0.2633 -0.0647 0.033 Uiso 1 1 d R . . H1 H 0.4954 0.3502 -0.1487 0.033 Uiso 1 1 d R . . O2W O -0.1831(4) 0.2238(3) -0.2696(4) 0.0407(6) Uani 1 1 d . . . H4 H -0.1998 0.3139 -0.2535 0.049 Uiso 1 1 d R . . H5 H -0.2546 0.1848 -0.2323 0.049 Uiso 1 1 d R . . O3W O 0.2693(4) -0.0472(3) -0.9481(3) 0.0421(7) Uani 1 1 d . . . H7 H 0.2895 -0.1254 -1.0145 0.051 Uiso 1 1 d R . . H6 H 0.3544 -0.0061 -0.8523 0.051 Uiso 1 1 d R . . O4W O 0.4218(5) 0.9105(5) -0.3683(5) 0.0919(15) Uani 1 1 d . . . H8 H 0.4578 0.9273 -0.4382 0.110 Uiso 1 1 d R . . H9 H 0.3592 0.9728 -0.3340 0.110 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0265(2) 0.0150(2) 0.0126(2) 0.00641(16) 0.00859(16) 0.00296(16) Co2 0.0237(3) 0.0130(3) 0.0103(3) 0.0043(2) 0.0076(2) 0.0034(2) O1 0.0417(13) 0.0190(10) 0.0139(9) 0.0057(8) 0.0131(9) 0.0062(9) O2 0.0534(15) 0.0156(10) 0.0243(11) 0.0040(9) 0.0207(11) 0.0032(10) O3 0.0436(13) 0.0205(10) 0.0221(11) 0.0093(9) 0.0156(10) -0.0030(9) O4 0.0371(12) 0.0191(10) 0.0120(9) 0.0072(8) 0.0112(8) 0.0033(8) O5 0.0408(13) 0.0133(9) 0.0175(10) 0.0058(8) 0.0128(9) -0.0004(8) N1 0.0251(12) 0.0156(11) 0.0106(10) 0.0058(9) 0.0094(9) 0.0056(9) N2 0.0236(12) 0.0133(11) 0.0115(10) 0.0047(8) 0.0083(9) 0.0045(9) C1 0.0281(15) 0.0144(12) 0.0136(12) 0.0045(10) 0.0096(11) 0.0058(11) C2 0.0206(13) 0.0154(12) 0.0123(12) 0.0056(10) 0.0070(10) 0.0051(10) C3 0.0238(14) 0.0141(12) 0.0161(13) 0.0067(10) 0.0076(11) 0.0014(10) C4 0.0206(13) 0.0184(13) 0.0119(12) 0.0073(10) 0.0073(10) 0.0048(10) C5 0.0241(14) 0.0165(13) 0.0145(13) 0.0067(11) 0.0086(10) 0.0025(10) C6 0.0248(14) 0.0155(13) 0.0101(12) 0.0072(10) 0.0056(10) 0.0027(11) O1W 0.0250(11) 0.0277(11) 0.0273(11) 0.0138(9) 0.0088(9) 0.0015(9) O2W 0.0366(14) 0.0407(15) 0.0625(18) 0.0325(14) 0.0284(13) 0.0161(11) O3W 0.0323(13) 0.0513(16) 0.0215(12) -0.0038(11) 0.0039(10) 0.0235(12) O4W 0.056(2) 0.081(3) 0.074(3) -0.015(2) 0.0070(19) 0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.027(2) 2_554 ? Co1 O2W 2.081(3) . ? Co1 O1 2.085(2) . ? Co1 O1W 2.120(2) . ? Co1 O4 2.151(2) 1_556 ? Co1 N1 2.152(2) . ? Co2 O3W 2.062(2) . ? Co2 O3W 2.062(2) 2_553 ? Co2 N2 2.106(2) . ? Co2 N2 2.106(2) 2_553 ? Co2 O4 2.155(2) . ? Co2 O4 2.155(2) 2_553 ? O1 C1 1.262(3) . ? O2 C1 1.237(3) . ? O3 C5 1.230(3) . ? O4 C5 1.275(3) . ? O4 Co1 2.151(2) 1_554 ? O5 C6 1.250(3) . ? O5 Co1 2.027(2) 2_554 ? N1 C2 1.332(3) . ? N1 C6 1.376(3) . ? N2 C4 1.331(4) . ? N2 C6 1.365(3) . ? C1 C2 1.524(4) . ? C2 C3 1.375(4) . ? C3 C4 1.384(4) . ? C3 H3 0.9500 . ? C4 C5 1.515(4) . ? O1W H2 0.8051 . ? O1W H1 0.8050 . ? O2W H4 0.8107 . ? O2W H5 0.8089 . ? O3W H7 0.8077 . ? O3W H6 0.8077 . ? O4W H8 0.8131 . ? O4W H9 0.8167 . ? 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 O5 Co1 O2W 94.65(10) 2_554 . ? O5 Co1 O1 168.53(8) 2_554 . ? O2W Co1 O1 92.14(10) . . ? O5 Co1 O1W 85.29(9) 2_554 . ? O2W Co1 O1W 172.63(9) . . ? O1 Co1 O1W 89.15(9) . . ? O5 Co1 O4 87.68(8) 2_554 1_556 ? O2W Co1 O4 86.37(10) . 1_556 ? O1 Co1 O4 101.98(8) . 1_556 ? O1W Co1 O4 86.26(9) . 1_556 ? O5 Co1 N1 93.31(8) 2_554 . ? O2W Co1 N1 95.78(10) . . ? O1 Co1 N1 76.80(8) . . ? O1W Co1 N1 91.58(9) . . ? O4 Co1 N1 177.54(8) 1_556 . ? O3W Co2 O3W 180.000(1) . 2_553 ? O3W Co2 N2 90.79(9) . . ? O3W Co2 N2 89.21(9) 2_553 . ? O3W Co2 N2 89.21(9) . 2_553 ? O3W Co2 N2 90.79(9) 2_553 2_553 ? N2 Co2 N2 180.000(1) . 2_553 ? O3W Co2 O4 89.73(11) . . ? O3W Co2 O4 90.27(11) 2_553 . ? N2 Co2 O4 76.97(8) . . ? N2 Co2 O4 103.03(8) 2_553 . ? O3W Co2 O4 90.27(11) . 2_553 ? O3W Co2 O4 89.73(11) 2_553 2_553 ? N2 Co2 O4 103.03(8) . 2_553 ? N2 Co2 O4 76.97(8) 2_553 2_553 ? O4 Co2 O4 180.0 . 2_553 ? C1 O1 Co1 116.21(18) . . ? C5 O4 Co1 123.51(18) . 1_554 ? C5 O4 Co2 115.74(17) . . ? Co1 O4 Co2 120.61(9) 1_554 . ? C6 O5 Co1 145.1(2) . 2_554 ? C2 N1 C6 118.3(2) . . ? C2 N1 Co1 112.27(17) . . ? C6 N1 Co1 128.65(18) . . ? C4 N2 C6 119.1(2) . . ? C4 N2 Co2 115.16(18) . . ? C6 N2 Co2 125.34(17) . . ? O2 C1 O1 125.5(3) . . ? O2 C1 C2 118.3(2) . . ? O1 C1 C2 116.3(2) . . ? N1 C2 C3 123.4(2) . . ? N1 C2 C1 114.3(2) . . ? C3 C2 C1 122.2(2) . . ? C2 C3 C4 115.7(2) . . ? C2 C3 H3 122.2 . . ? C4 C3 H3 122.2 . . ? N2 C4 C3 122.7(2) . . ? N2 C4 C5 116.0(2) . . ? C3 C4 C5 121.1(2) . . ? O3 C5 O4 126.7(3) . . ? O3 C5 C4 117.8(2) . . ? O4 C5 C4 115.5(2) . . ? O5 C6 N2 120.5(2) . . ? O5 C6 N1 119.0(2) . . ? N2 C6 N1 120.4(2) . . ? Co1 O1W H2 111.9 . . ? Co1 O1W H1 117.6 . . ? H2 O1W H1 110.9 . . ? Co1 O2W H4 108.8 . . ? Co1 O2W H5 130.4 . . ? H4 O2W H5 104.3 . . ? Co2 O3W H7 123.4 . . ? Co2 O3W H6 123.1 . . ? H7 O3W H6 111.6 . . ? H8 O4W H9 111.2 . . ? _diffrn_measured_fraction_theta_max 27.4835 _diffrn_reflns_theta_full 27.4835 _diffrn_measured_fraction_theta_full 98.1000 _refine_diff_density_max 1.419 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.113