# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shourong Zhu' _publ_contact_author_email SHOURONGZHU@SHU.EDU.CN _publ_section_title ; Coordination Polymer Based on Cu(II), Co(II) and 4,4 -Bipyridine-2,6,2 ,6 -tetracarboxylate: Synthesis, Structure and adsorption properties ; loop_ _publ_author_name 'Shourong Zhu' 'Xiang He' 'Min Shao' 'Zhao Zhao' 'Yongmei Zhou' # Attachment 'ligand_ren.CIF' data_b _database_code_depnum_ccdc_archive 'CCDC 696646' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H14 N2 O11' _chemical_formula_weight 386.27 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.012(6) _cell_length_b 9.438(9) _cell_length_c 13.165(12) _cell_angle_alpha 97.952(11) _cell_angle_beta 103.674(13) _cell_angle_gamma 110.541(12) _cell_volume 768.9(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 516 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 20.56 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 400 _exptl_absorpt_coefficient_mu 0.147 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9532 _exptl_absorpt_correction_T_max 0.9762 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4593 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.1103 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 27.28 _reflns_number_total 3233 _reflns_number_gt 1543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart apex (Bruker, 2000)' _computing_cell_refinement 'Saint (Bruker, 2000)' _computing_data_reduction 'Saint (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _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^)+(0.0927P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.030(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3233 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1515 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.2094 _refine_ls_wR_factor_gt 0.1652 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.947 _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 C16 C 0.6397(7) 0.2929(4) 1.4780(3) 0.0344(10) Uani 1 1 d . . . H16A H 0.5598 0.1863 1.4507 0.041 Uiso 1 1 calc R . . N2 N 0.8708(5) 0.5034(4) 1.6320(2) 0.0339(8) Uani 1 1 d . . . C12 C 0.7465(6) 0.5532(4) 1.4605(3) 0.0318(9) Uani 1 1 d . . . H12A H 0.7486 0.6263 1.4197 0.038 Uiso 1 1 calc R . . N1 N 0.3139(5) 0.2337(3) 1.0705(2) 0.0319(8) Uani 1 1 d . . . C10 C 0.4666(6) 0.1868(4) 1.2392(3) 0.0325(9) Uani 1 1 d . . . H10A H 0.4980 0.1165 1.2761 0.039 Uiso 1 1 calc R . . C8 C 0.4665(7) 0.4359(4) 1.2341(3) 0.0342(10) Uani 1 1 d . . . H8A H 0.4985 0.5387 1.2672 0.041 Uiso 1 1 calc R . . C17 C 0.6335(6) 0.3945(4) 1.4116(3) 0.0304(9) Uani 1 1 d . . . C15 C 0.7643(7) 0.3506(4) 1.5842(3) 0.0326(10) Uani 1 1 d . . . C13 C 0.8547(7) 0.6016(4) 1.5691(3) 0.0324(9) Uani 1 1 d . . . C4 C 0.7951(7) 0.2394(5) 1.6506(3) 0.0358(10) Uani 1 1 d . . . C9 C 0.5206(6) 0.3385(4) 1.2946(3) 0.0305(9) Uani 1 1 d . . . C3 C 0.9715(7) 0.7706(4) 1.6256(3) 0.0360(10) Uani 1 1 d . . . C2 C 0.3061(7) 0.4878(4) 1.0632(3) 0.0349(10) Uani 1 1 d . . . C5 C 0.3666(6) 0.1405(4) 1.1296(3) 0.0321(9) Uani 1 1 d . . . C7 C 0.3655(6) 0.3796(4) 1.1250(3) 0.0312(9) Uani 1 1 d . . . C1 C 0.3120(7) -0.0225(4) 1.0689(3) 0.0359(10) Uani 1 1 d . . . O4 O 0.2077(5) 0.4290(3) 0.9622(2) 0.0553(10) Uani 1 1 d . . . H4A H 0.1701 0.4922 0.9358 0.066 Uiso 1 1 calc R . . O2 O 0.2247(5) -0.0706(3) 0.9740(2) 0.0524(9) Uani 1 1 d . . . O8 O 1.0051(6) 0.8609(3) 1.5596(2) 0.0577(10) Uani 1 1 d . . . H8B H 1.0717 0.9519 1.5941 0.069 Uiso 1 1 calc R . . O7 O 1.0271(6) 0.8157(3) 1.7219(2) 0.0592(10) Uani 1 1 d . . . O6 O 0.6639(5) 0.1054(3) 1.6294(2) 0.0572(10) Uani 1 1 d . . . O5 O 0.9729(5) 0.2986(3) 1.7291(2) 0.0504(9) Uani 1 1 d . . . H5A H 0.9862 0.2309 1.7595 0.061 Uiso 1 1 calc R . . O3 O 0.3564(6) 0.6217(3) 1.1093(2) 0.0564(10) Uani 1 1 d . . . O1 O 0.3743(6) -0.1018(3) 1.1331(2) 0.0579(10) Uani 1 1 d . . . H1A H 0.3733 -0.1805 1.0974 0.069 Uiso 1 1 calc R . . O1W O 1.2865(5) 1.1402(3) 1.6649(2) 0.0530(9) Uani 1 1 d . . . H1WA H 1.3175 1.1756 1.7323 0.080 Uiso 1 1 d R . . H1WB H 1.3963 1.1298 1.6542 0.080 Uiso 1 1 d R . . O2W O 0.1077(5) 0.6186(3) 0.8656(2) 0.0592(10) Uani 1 1 d . . . H2WA H 0.1618 0.7169 0.8906 0.089 Uiso 1 1 d R . . H2WB H 0.0688 0.6144 0.7987 0.089 Uiso 1 1 d R . . O3W O 1.1035(5) 0.1224(3) 1.8358(2) 0.0562(10) Uani 1 1 d . . . H3WA H 1.0952 0.0296 1.8197 0.084 Uiso 1 1 d R . . H3WB H 1.1640 0.1547 1.9035 0.084 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 C16 0.043(3) 0.024(2) 0.031(2) 0.0055(16) 0.0037(19) 0.0127(19) N2 0.042(2) 0.0292(18) 0.0303(17) 0.0090(14) 0.0081(16) 0.0151(16) C12 0.041(2) 0.028(2) 0.030(2) 0.0091(17) 0.0103(18) 0.0176(19) N1 0.041(2) 0.0244(17) 0.0322(17) 0.0083(14) 0.0074(15) 0.0173(15) C10 0.043(2) 0.0223(19) 0.029(2) 0.0064(16) 0.0031(18) 0.0152(18) C8 0.046(3) 0.024(2) 0.031(2) 0.0036(16) 0.0088(19) 0.0146(19) C17 0.039(2) 0.026(2) 0.026(2) 0.0068(16) 0.0066(18) 0.0142(18) C15 0.043(3) 0.024(2) 0.030(2) 0.0057(16) 0.0096(19) 0.0134(19) C13 0.043(3) 0.026(2) 0.029(2) 0.0072(16) 0.0107(19) 0.0146(19) C4 0.046(3) 0.035(2) 0.026(2) 0.0074(17) 0.007(2) 0.019(2) C9 0.036(2) 0.028(2) 0.027(2) 0.0067(16) 0.0073(18) 0.0137(18) C3 0.042(3) 0.030(2) 0.031(2) 0.0096(18) 0.0031(19) 0.0139(19) C2 0.048(3) 0.027(2) 0.031(2) 0.0080(17) 0.006(2) 0.021(2) C5 0.044(3) 0.026(2) 0.028(2) 0.0090(16) 0.0084(19) 0.0166(19) C7 0.042(3) 0.0223(19) 0.030(2) 0.0066(16) 0.0076(19) 0.0167(18) C1 0.052(3) 0.025(2) 0.031(2) 0.0084(17) 0.010(2) 0.018(2) O4 0.093(3) 0.0385(17) 0.0349(16) 0.0123(14) 0.0004(17) 0.0382(18) O2 0.087(3) 0.0309(16) 0.0302(16) 0.0029(13) -0.0010(16) 0.0264(16) O8 0.088(3) 0.0245(16) 0.0387(17) 0.0066(13) 0.0058(17) 0.0063(16) O7 0.093(3) 0.0300(17) 0.0361(18) 0.0006(14) 0.0047(18) 0.0158(17) O6 0.070(2) 0.0307(17) 0.0525(19) 0.0179(14) 0.0022(17) 0.0071(16) O5 0.062(2) 0.0345(17) 0.0436(17) 0.0153(14) -0.0030(16) 0.0172(16) O3 0.084(3) 0.0255(16) 0.0485(18) 0.0037(14) -0.0033(17) 0.0266(16) O1 0.103(3) 0.0315(17) 0.0414(18) 0.0074(14) 0.0070(18) 0.0392(18) O1W 0.058(2) 0.0378(17) 0.0502(19) 0.0060(15) 0.0068(17) 0.0124(16) O2W 0.089(3) 0.0395(18) 0.0353(17) 0.0094(14) -0.0031(17) 0.0240(18) O3W 0.088(3) 0.0342(17) 0.0376(16) 0.0058(13) -0.0041(16) 0.0302(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 C16 C15 1.376(5) . ? C16 C17 1.388(5) . ? C16 H16A 0.9300 . ? N2 C13 1.342(4) . ? N2 C15 1.343(5) . ? C12 C13 1.375(5) . ? C12 C17 1.395(5) . ? C12 H12A 0.9300 . ? N1 C7 1.340(4) . ? N1 C5 1.340(4) . ? C10 C5 1.377(5) . ? C10 C9 1.388(5) . ? C10 H10A 0.9300 . ? C8 C7 1.375(5) . ? C8 C9 1.388(5) . ? C8 H8A 0.9300 . ? C17 C9 1.478(5) . ? C15 C4 1.496(5) . ? C13 C3 1.495(5) . ? C4 O6 1.220(5) . ? C4 O5 1.294(5) . ? C3 O7 1.201(4) . ? C3 O8 1.304(4) . ? C2 O3 1.210(4) . ? C2 O4 1.282(4) . ? C2 C7 1.499(5) . ? C5 C1 1.502(5) . ? C1 O2 1.195(4) . ? C1 O1 1.302(4) . ? O4 H4A 0.8200 . ? O8 H8B 0.8200 . ? O5 H5A 0.8200 . ? O1 H1A 0.8200 . ? O1W H1WA 0.8500 . ? O1W H1WB 0.8500 . ? O2W H2WA 0.8501 . ? O2W H2WB 0.8501 . ? O3W H3WA 0.8502 . ? O3W H3WB 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 C15 C16 C17 119.8(3) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C13 N2 C15 116.1(3) . . ? C13 C12 C17 120.0(3) . . ? C13 C12 H12A 120.0 . . ? C17 C12 H12A 120.0 . . ? C7 N1 C5 115.6(3) . . ? C5 C10 C9 119.9(3) . . ? C5 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C7 C8 C9 119.6(3) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C16 C17 C12 116.4(3) . . ? C16 C17 C9 122.2(3) . . ? C12 C17 C9 121.3(3) . . ? N2 C15 C16 123.9(3) . . ? N2 C15 C4 116.8(3) . . ? C16 C15 C4 119.3(3) . . ? N2 C13 C12 123.5(3) . . ? N2 C13 C3 114.6(3) . . ? C12 C13 C3 121.9(3) . . ? O6 C4 O5 124.7(4) . . ? O6 C4 C15 121.7(4) . . ? O5 C4 C15 113.6(4) . . ? C10 C9 C8 116.6(3) . . ? C10 C9 C17 121.7(3) . . ? C8 C9 C17 121.7(3) . . ? O7 C3 O8 124.6(4) . . ? O7 C3 C13 122.5(3) . . ? O8 C3 C13 112.9(3) . . ? O3 C2 O4 124.9(4) . . ? O3 C2 C7 119.4(3) . . ? O4 C2 C7 115.6(3) . . ? N1 C5 C10 123.9(3) . . ? N1 C5 C1 115.9(3) . . ? C10 C5 C1 120.2(3) . . ? N1 C7 C8 124.3(3) . . ? N1 C7 C2 117.8(3) . . ? C8 C7 C2 117.9(3) . . ? O2 C1 O1 125.4(4) . . ? O2 C1 C5 123.7(3) . . ? O1 C1 C5 110.9(3) . . ? C2 O4 H4A 109.5 . . ? C3 O8 H8B 109.5 . . ? C4 O5 H5A 109.5 . . ? C1 O1 H1A 109.5 . . ? H1WA O1W H1WB 106.8 . . ? H2WA O2W H2WB 99.6 . . ? H3WA O3W H3WB 105.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C16 C17 C12 -4.1(6) . . . . ? C15 C16 C17 C9 173.6(4) . . . . ? C13 C12 C17 C16 -0.5(6) . . . . ? C13 C12 C17 C9 -178.3(4) . . . . ? C13 N2 C15 C16 -1.7(6) . . . . ? C13 N2 C15 C4 175.0(4) . . . . ? C17 C16 C15 N2 5.5(7) . . . . ? C17 C16 C15 C4 -171.1(4) . . . . ? C15 N2 C13 C12 -3.3(6) . . . . ? C15 N2 C13 C3 178.8(4) . . . . ? C17 C12 C13 N2 4.4(6) . . . . ? C17 C12 C13 C3 -177.8(4) . . . . ? N2 C15 C4 O6 157.4(4) . . . . ? C16 C15 C4 O6 -25.7(6) . . . . ? N2 C15 C4 O5 -23.9(5) . . . . ? C16 C15 C4 O5 153.0(4) . . . . ? C5 C10 C9 C8 0.6(6) . . . . ? C5 C10 C9 C17 -178.2(4) . . . . ? C7 C8 C9 C10 -0.2(6) . . . . ? C7 C8 C9 C17 178.6(4) . . . . ? C16 C17 C9 C10 -18.4(6) . . . . ? C12 C17 C9 C10 159.3(4) . . . . ? C16 C17 C9 C8 162.8(4) . . . . ? C12 C17 C9 C8 -19.5(6) . . . . ? N2 C13 C3 O7 -18.3(6) . . . . ? C12 C13 C3 O7 163.7(4) . . . . ? N2 C13 C3 O8 161.6(4) . . . . ? C12 C13 C3 O8 -16.3(6) . . . . ? C7 N1 C5 C10 0.1(6) . . . . ? C7 N1 C5 C1 -179.2(4) . . . . ? C9 C10 C5 N1 -0.6(6) . . . . ? C9 C10 C5 C1 178.7(4) . . . . ? C5 N1 C7 C8 0.3(6) . . . . ? C5 N1 C7 C2 -178.8(4) . . . . ? C9 C8 C7 N1 -0.3(6) . . . . ? C9 C8 C7 C2 178.8(4) . . . . ? O3 C2 C7 N1 -177.7(4) . . . . ? O4 C2 C7 N1 0.8(6) . . . . ? O3 C2 C7 C8 3.2(6) . . . . ? O4 C2 C7 C8 -178.4(4) . . . . ? N1 C5 C1 O2 -0.9(6) . . . . ? C10 C5 C1 O2 179.7(4) . . . . ? N1 C5 C1 O1 178.5(4) . . . . ? C10 C5 C1 O1 -0.9(6) . . . . ? 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 O4 H4A O2W 0.82 1.72 2.530(4) 171.4 . O5 H5A O3W 0.82 1.79 2.586(4) 161.7 . O8 H8B O1W 0.82 1.82 2.610(4) 162.7 . O1 H1A O3 0.82 1.86 2.540(4) 139.6 1_545 C10 H10A O1 0.93 2.33 2.659(5) 100.2 . C16 H16A O6 0.93 2.59 2.857(5) 96.8 . _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 27.28 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.318 _refine_diff_density_min -0.310 _refine_diff_density_rms 0.089 # Attachment 'Dcopper_ren.CIF' data_d _database_code_depnum_ccdc_archive 'CCDC 696647' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H8 Cu2 N2 O12' _chemical_formula_weight 523.30 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.1533(14) _cell_length_b 18.168(3) _cell_length_c 6.3974(12) _cell_angle_alpha 90.00 _cell_angle_beta 107.124(2) _cell_angle_gamma 90.00 _cell_volume 794.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 527 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 20.62 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 2.758 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9260 _exptl_absorpt_correction_T_max 0.9498 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4945 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.1027 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.57 _reflns_number_total 1831 _reflns_number_gt 1164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart apex (Bruker, 2000)' _computing_cell_refinement 'Saint (Bruker, 2000)' _computing_data_reduction 'Saint (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1831 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1859 _refine_ls_wR_factor_gt 0.1540 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 Cu1 Cu 0.09740(11) 0.30787(4) 0.21700(13) 0.0224(3) Uani 1 1 d . . . N2 N -0.1215(7) 0.3714(3) 0.1285(8) 0.0177(11) Uani 1 1 d . . . O4 O -0.3255(7) 0.3003(2) 0.5213(7) 0.0290(12) Uani 1 1 d . . . O3 O -0.0398(7) 0.2808(3) 0.4495(7) 0.0251(10) Uani 1 1 d . . . O2 O 0.1605(7) 0.3626(3) -0.0373(7) 0.0249(10) Uani 1 1 d . . . C9 C -0.2064(9) 0.3131(3) 0.4226(10) 0.0208(13) Uani 1 1 d . . . O1 O 0.0180(7) 0.4386(3) -0.3124(7) 0.0305(11) Uani 1 1 d . . . O1w O 0.3252(7) 0.2435(2) 0.2964(7) 0.0255(10) Uani 1 1 d . . . H2WA H 0.3373 0.2250 0.1789 0.031 Uiso 1 1 d R . . H2WB H 0.3002 0.2082 0.3713 0.031 Uiso 1 1 d R . . C6 C -0.4024(9) 0.4215(3) 0.1959(10) 0.0205(13) Uani 1 1 d . . . H6A H -0.4898 0.4226 0.2784 0.025 Uiso 1 1 calc R . . C3 C -0.1390(10) 0.4163(3) -0.0399(10) 0.0203(13) Uani 1 1 d . . . C2 C -0.2914(9) 0.4667(4) -0.1009(10) 0.0217(14) Uani 1 1 d . . . H2A H -0.3055 0.4970 -0.2216 0.026 Uiso 1 1 calc R . . C5 C -0.2511(9) 0.3712(3) 0.2431(10) 0.0205(14) Uani 1 1 d . . . C8 C 0.0237(9) 0.4059(4) -0.1439(10) 0.0222(14) Uani 1 1 d . . . C1 C -0.4229(9) 0.4709(4) 0.0221(10) 0.0230(14) Uani 1 1 d . . . O2w O 0.2904(7) 0.3984(3) 0.4821(8) 0.0340(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0193(5) 0.0243(5) 0.0250(5) 0.0038(3) 0.0084(3) 0.0031(3) N2 0.012(3) 0.021(3) 0.020(3) 0.001(2) 0.005(2) 0.003(2) O4 0.025(3) 0.038(3) 0.027(3) 0.012(2) 0.011(2) 0.001(2) O3 0.028(3) 0.023(2) 0.025(2) 0.006(2) 0.0073(19) 0.002(2) O2 0.022(2) 0.025(2) 0.029(3) 0.002(2) 0.0104(19) 0.0006(19) C9 0.018(3) 0.027(4) 0.019(3) -0.002(3) 0.007(2) -0.001(3) O1 0.039(3) 0.033(3) 0.022(2) 0.003(2) 0.014(2) -0.005(2) O1w 0.031(3) 0.027(3) 0.023(2) 0.002(2) 0.0136(19) 0.004(2) C6 0.019(3) 0.019(3) 0.027(3) 0.003(3) 0.011(3) 0.003(3) C3 0.034(4) 0.012(3) 0.016(3) -0.003(2) 0.010(3) -0.006(3) C2 0.021(3) 0.023(3) 0.021(3) 0.001(3) 0.006(2) 0.005(3) C5 0.021(3) 0.022(4) 0.019(3) 0.000(3) 0.007(2) -0.005(3) C8 0.020(3) 0.021(3) 0.026(4) -0.004(3) 0.008(3) -0.005(3) C1 0.020(3) 0.025(4) 0.026(3) -0.002(3) 0.009(3) 0.001(3) O2w 0.031(3) 0.042(3) 0.030(3) 0.000(2) 0.011(2) 0.000(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 Cu1 N2 1.893(5) . ? Cu1 O1w 1.948(4) . ? Cu1 O2w 2.472(5) . ? Cu1 O2 2.067(4) . ? Cu1 O3 2.068(5) . ? Cu1 O3 2.344(4) 4_565 ? N2 C3 1.327(8) . ? N2 C5 1.341(7) . ? O4 C9 1.223(8) . ? O3 C9 1.295(8) . ? O3 Cu1 2.344(4) 4_566 ? O2 C8 1.283(8) . ? C9 C5 1.522(9) . ? O1 C8 1.221(7) . ? C6 C5 1.380(8) . ? C6 C1 1.403(9) . ? C3 C2 1.389(9) . ? C3 C8 1.513(9) . ? C2 C1 1.395(9) . ? C1 C1 1.492(12) 3_465 ? 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 N2 Cu1 O1w 177.5(2) . . ? N2 Cu1 O2 79.9(2) . . ? O1w Cu1 O2 97.71(18) . . ? N2 Cu1 O3 80.5(2) . . ? O1w Cu1 O3 101.95(18) . . ? O2 Cu1 O3 160.15(18) . . ? N2 Cu1 O3 93.97(19) . 4_565 ? O1w Cu1 O3 85.17(18) . 4_565 ? O2 Cu1 O3 84.10(17) . 4_565 ? O3 Cu1 O3 100.15(14) . 4_565 ? C3 N2 C5 122.1(5) . . ? C3 N2 Cu1 119.3(4) . . ? C5 N2 Cu1 118.6(4) . . ? C9 O3 Cu1 114.2(4) . . ? C9 O3 Cu1 125.5(4) . 4_566 ? Cu1 O3 Cu1 120.2(2) . 4_566 ? C8 O2 Cu1 113.8(4) . . ? O4 C9 O3 126.8(6) . . ? O4 C9 C5 119.9(6) . . ? O3 C9 C5 113.3(5) . . ? C5 C6 C1 119.3(6) . . ? N2 C3 C2 120.8(6) . . ? N2 C3 C8 112.3(5) . . ? C2 C3 C8 126.9(6) . . ? C1 C2 C3 118.8(6) . . ? N2 C5 C6 120.1(6) . . ? N2 C5 C9 113.0(5) . . ? C6 C5 C9 126.9(5) . . ? O1 C8 O2 126.1(6) . . ? O1 C8 C3 119.8(6) . . ? O2 C8 C3 114.1(5) . . ? C2 C1 C6 118.7(6) . . ? C2 C1 C1 121.1(7) . 3_465 ? C6 C1 C1 120.1(7) . 3_465 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1w Cu1 N2 C3 -12(5) . . . . ? O2 Cu1 N2 C3 1.5(4) . . . . ? O3 Cu1 N2 C3 178.6(5) . . . . ? O3 Cu1 N2 C3 -81.8(5) 4_565 . . . ? O1w Cu1 N2 C5 170(5) . . . . ? O2 Cu1 N2 C5 -176.5(5) . . . . ? O3 Cu1 N2 C5 0.6(5) . . . . ? O3 Cu1 N2 C5 100.2(5) 4_565 . . . ? N2 Cu1 O3 C9 4.2(4) . . . . ? O1w Cu1 O3 C9 -175.4(4) . . . . ? O2 Cu1 O3 C9 12.7(8) . . . . ? O3 Cu1 O3 C9 -88.2(4) 4_565 . . . ? N2 Cu1 O3 Cu1 -179.8(3) . . . 4_566 ? O1w Cu1 O3 Cu1 0.6(3) . . . 4_566 ? O2 Cu1 O3 Cu1 -171.3(4) . . . 4_566 ? O3 Cu1 O3 Cu1 87.8(3) 4_565 . . 4_566 ? N2 Cu1 O2 C8 -6.1(4) . . . . ? O1w Cu1 O2 C8 173.3(4) . . . . ? O3 Cu1 O2 C8 -14.6(8) . . . . ? O3 Cu1 O2 C8 89.0(4) 4_565 . . . ? Cu1 O3 C9 O4 171.0(5) . . . . ? Cu1 O3 C9 O4 -4.8(9) 4_566 . . . ? Cu1 O3 C9 C5 -7.4(6) . . . . ? Cu1 O3 C9 C5 176.9(4) 4_566 . . . ? C5 N2 C3 C2 1.8(9) . . . . ? Cu1 N2 C3 C2 -176.1(4) . . . . ? C5 N2 C3 C8 -179.5(5) . . . . ? Cu1 N2 C3 C8 2.6(7) . . . . ? N2 C3 C2 C1 1.9(9) . . . . ? C8 C3 C2 C1 -176.7(6) . . . . ? C3 N2 C5 C6 -3.9(9) . . . . ? Cu1 N2 C5 C6 174.0(4) . . . . ? C3 N2 C5 C9 177.6(5) . . . . ? Cu1 N2 C5 C9 -4.5(7) . . . . ? C1 C6 C5 N2 2.3(9) . . . . ? C1 C6 C5 C9 -179.4(6) . . . . ? O4 C9 C5 N2 -170.6(6) . . . . ? O3 C9 C5 N2 7.9(8) . . . . ? O4 C9 C5 C6 11.0(10) . . . . ? O3 C9 C5 C6 -170.5(6) . . . . ? Cu1 O2 C8 O1 -172.5(5) . . . . ? Cu1 O2 C8 C3 8.9(6) . . . . ? N2 C3 C8 O1 173.5(6) . . . . ? C2 C3 C8 O1 -7.8(10) . . . . ? N2 C3 C8 O2 -7.8(8) . . . . ? C2 C3 C8 O2 170.9(6) . . . . ? C3 C2 C1 C6 -3.3(9) . . . . ? C3 C2 C1 C1 173.8(7) . . . 3_465 ? C5 C6 C1 C2 1.3(9) . . . . ? C5 C6 C1 C1 -175.8(7) . . . 3_465 ? 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 C2 H2A O2w 0.93 2.55 3.459(8) 165.8 3_565 C6 H6A O2w 0.93 2.36 3.275(8) 168.0 1_455 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.708 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.166 # Attachment 'DCo_ren.CIF' data_c _database_code_depnum_ccdc_archive 'CCDC 696648' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H40 Co4 N4 O26' _chemical_formula_weight 1084.36 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.170(7) _cell_length_b 10.833(5) _cell_length_c 14.400(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.519(6) _cell_angle_gamma 90.00 _cell_volume 2173.2(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2840 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.82 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 1.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9532 _exptl_absorpt_correction_T_max 0.9762 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12926 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.1333 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.65 _reflns_number_total 4932 _reflns_number_gt 2905 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart apex (Bruker, 2000)' _computing_cell_refinement 'Saint (Bruker, 2000)' _computing_data_reduction 'Saint (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL (Sheldrick, 2000)' _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. There are solvent accessible voids in the structure. SQUEEZE was used in the structure. ; _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^)+(0.1200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4932 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.2276 _refine_ls_wR_factor_gt 0.2163 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _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 Co2 Co 0.17939(6) 0.28856(9) 0.30066(6) 0.0249(3) Uani 1 1 d . . . Co3 Co 1.0000 0.5000 1.0000 0.0269(3) Uani 1 2 d S . . N1 N 0.0916(4) 0.2770(5) 0.3952(4) 0.0246(12) Uani 1 1 d . . . N2 N -0.2291(3) 0.2203(5) 0.7090(4) 0.0215(11) Uani 1 1 d . . . O5w O 0.8948(6) 0.7274(7) 1.1734(5) 0.083(2) Uani 1 1 d . . . O1 O -0.1961(3) 0.1122(5) 0.8681(3) 0.0374(12) Uani 1 1 d . . . O2 O -0.0396(3) 0.0872(4) 0.8655(3) 0.0291(10) Uani 1 1 d . . . O3 O -0.4023(3) 0.3045(5) 0.6786(3) 0.0370(12) Uani 1 1 d . . . O4 O -0.3912(3) 0.3744(4) 0.5362(3) 0.0295(11) Uani 1 1 d . . . O5 O 0.2056(4) 0.0172(6) 0.5044(4) 0.0588(17) Uani 1 1 d . . . O6 O 0.2298(3) 0.1279(5) 0.3838(4) 0.0443(14) Uani 1 1 d . . . O7 O -0.0379(4) 0.5416(5) 0.3133(4) 0.0443(13) Uani 1 1 d . . . O8 O 0.0880(3) 0.4492(5) 0.2730(3) 0.0382(12) Uani 1 1 d . . . O2w O 0.8785(3) 0.5957(5) 1.0118(4) 0.0415(13) Uani 1 1 d . . . O3w O 0.9530(3) 0.3608(4) 1.0864(3) 0.0366(12) Uani 1 1 d . . . O4w O 1.0802(3) 0.5903(5) 1.1187(3) 0.0379(12) Uani 1 1 d . . . C1 C -0.2560(5) 0.2781(6) 0.6253(5) 0.0243(13) Uani 1 1 d . . . C2 C -0.1948(4) 0.2906(6) 0.5632(4) 0.0238(13) Uani 1 1 d . . . H2B H -0.2145 0.3334 0.5054 0.029 Uiso 1 1 calc R . . C3 C -0.1034(4) 0.2404(6) 0.5850(5) 0.0241(14) Uani 1 1 d . . . C4 C -0.0764(4) 0.1828(6) 0.6723(5) 0.0278(15) Uani 1 1 d . . . H4A H -0.0131 0.1512 0.6903 0.033 Uiso 1 1 calc R . . C5 C -0.1406(4) 0.1714(6) 0.7319(4) 0.0244(14) Uani 1 1 d . . . C6 C -0.1220(4) 0.1189(6) 0.8291(5) 0.0275(14) Uani 1 1 d . . . C7 C -0.3591(4) 0.3225(6) 0.6122(5) 0.0244(14) Uani 1 1 d . . . C8 C 0.0218(4) 0.3618(6) 0.3939(5) 0.0272(14) Uani 1 1 d . . . C9 C -0.0422(4) 0.3513(7) 0.4551(5) 0.0300(15) Uani 1 1 d . . . H2A H -0.0915 0.4111 0.4539 0.036 Uiso 1 1 calc R . . C10 C -0.0348(4) 0.2529(6) 0.5188(5) 0.0244(14) Uani 1 1 d . . . C11 C 0.0379(4) 0.1654(7) 0.5187(5) 0.0298(15) Uani 1 1 d . . . H5A H 0.0445 0.0970 0.5606 0.036 Uiso 1 1 calc R . . C12 C 0.0998(4) 0.1815(6) 0.4559(5) 0.0270(14) Uani 1 1 d . . . C13 C 0.1852(5) 0.1013(7) 0.4479(5) 0.0339(16) Uani 1 1 d . . . C14 C 0.0226(5) 0.4599(7) 0.3203(5) 0.0294(15) Uani 1 1 d . . . Co1 Co -0.5000 0.5000 0.5000 0.0194(3) Uani 1 2 d S . . O1w O -0.6062(3) 0.3924(5) 0.5505(4) 0.0393(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co2 0.0193(4) 0.0355(5) 0.0236(5) -0.0019(4) 0.0140(3) -0.0005(4) Co3 0.0242(6) 0.0238(7) 0.0340(7) 0.0050(5) 0.0090(5) -0.0034(5) N1 0.024(3) 0.026(3) 0.028(3) 0.003(2) 0.016(2) 0.002(2) N2 0.020(2) 0.028(3) 0.020(3) 0.008(2) 0.012(2) 0.002(2) O5w 0.093(6) 0.083(6) 0.065(5) -0.008(4) -0.005(4) -0.001(4) O1 0.029(2) 0.059(3) 0.026(2) 0.016(2) 0.008(2) 0.006(2) O2 0.022(2) 0.039(3) 0.025(2) 0.008(2) 0.0016(19) 0.0031(19) O3 0.025(2) 0.061(4) 0.028(3) 0.007(2) 0.011(2) 0.013(2) O4 0.023(2) 0.038(3) 0.027(2) 0.005(2) 0.0018(19) 0.0082(19) O5 0.047(3) 0.071(4) 0.064(4) 0.032(3) 0.025(3) 0.027(3) O6 0.033(3) 0.057(4) 0.048(3) 0.007(3) 0.020(2) 0.021(2) O7 0.046(3) 0.047(3) 0.045(3) 0.016(3) 0.023(3) 0.013(3) O8 0.038(3) 0.048(3) 0.033(3) 0.014(2) 0.020(2) 0.007(2) O2w 0.030(2) 0.026(3) 0.067(4) 0.006(2) 0.004(2) -0.002(2) O3w 0.035(3) 0.032(3) 0.045(3) 0.011(2) 0.012(2) -0.006(2) O4w 0.032(3) 0.047(3) 0.032(3) 0.010(2) 0.001(2) -0.015(2) C1 0.027(3) 0.015(3) 0.030(3) 0.000(3) 0.005(3) 0.005(2) C2 0.022(3) 0.030(3) 0.021(3) 0.007(3) 0.007(2) 0.007(3) C3 0.022(3) 0.026(3) 0.027(3) 0.007(3) 0.012(3) 0.002(2) C4 0.019(3) 0.036(4) 0.030(4) 0.011(3) 0.008(3) 0.005(3) C5 0.020(3) 0.033(4) 0.020(3) 0.000(3) 0.002(2) -0.001(3) C6 0.025(3) 0.032(4) 0.025(3) 0.008(3) 0.004(3) -0.001(3) C7 0.018(3) 0.027(4) 0.028(3) 0.001(3) 0.004(3) 0.000(2) C8 0.025(3) 0.033(4) 0.026(3) 0.000(3) 0.012(3) 0.003(3) C9 0.020(3) 0.036(4) 0.036(4) 0.003(3) 0.011(3) 0.005(3) C10 0.022(3) 0.030(4) 0.025(3) 0.001(3) 0.013(3) 0.001(2) C11 0.024(3) 0.035(4) 0.033(4) 0.005(3) 0.012(3) 0.010(3) C12 0.023(3) 0.032(4) 0.029(4) 0.003(3) 0.013(3) 0.006(3) C13 0.030(4) 0.039(4) 0.035(4) 0.000(3) 0.015(3) 0.012(3) C14 0.028(3) 0.039(4) 0.024(3) 0.001(3) 0.011(3) 0.005(3) Co1 0.0177(5) 0.0198(6) 0.0212(6) -0.0010(5) 0.0051(5) 0.0020(4) O1w 0.033(3) 0.043(3) 0.043(3) 0.009(2) 0.011(2) -0.005(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 Co2 N1 2.009(5) . ? Co2 N2 2.015(5) 4_665 ? Co2 O1 2.141(5) 4_665 ? Co2 O6 2.159(5) . ? Co2 O8 2.162(5) . ? Co2 O3 2.168(5) 4_665 ? Co3 O2w 2.043(5) . ? Co3 O2w 2.043(5) 3_767 ? Co3 O4w 2.112(5) 3_767 ? Co3 O4w 2.112(5) . ? Co3 O3w 2.137(5) . ? Co3 O3w 2.137(5) 3_767 ? N1 C12 1.345(8) . ? N1 C8 1.347(8) . ? N2 C5 1.345(8) . ? N2 C1 1.349(8) . ? N2 Co2 2.015(5) 4_566 ? O1 C6 1.280(8) . ? O1 Co2 2.141(5) 4_566 ? O2 C6 1.239(7) . ? O2 Co1 2.136(4) 2_446 ? O3 C7 1.240(8) . ? O3 Co2 2.168(5) 4_566 ? O4 C7 1.241(7) . ? O4 Co1 2.051(4) . ? O5 C13 1.221(9) . ? O6 C13 1.243(8) . ? O7 C14 1.223(8) . ? O8 C14 1.252(8) . ? C1 C2 1.361(9) . ? C1 C7 1.517(8) . ? C2 C3 1.386(8) . ? C3 C4 1.393(9) . ? C3 C10 1.487(8) . ? C4 C5 1.366(9) . ? C5 C6 1.489(9) . ? C8 C9 1.380(9) . ? C8 C14 1.502(9) . ? C9 C10 1.398(9) . ? C10 C11 1.401(9) . ? C11 C12 1.381(9) . ? C12 C13 1.511(9) . ? Co1 O4 2.051(4) 3_466 ? Co1 O1w 2.133(5) . ? Co1 O1w 2.133(5) 3_466 ? Co1 O2 2.136(4) 2_456 ? Co1 O2 2.136(4) 4_565 ? 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 Co2 N2 173.5(2) . 4_665 ? N1 Co2 O1 106.5(2) . 4_665 ? N2 Co2 O1 75.25(19) 4_665 4_665 ? N1 Co2 O6 75.9(2) . . ? N2 Co2 O6 97.9(2) 4_665 . ? O1 Co2 O6 89.5(2) 4_665 . ? N1 Co2 O8 75.56(19) . . ? N2 Co2 O8 110.7(2) 4_665 . ? O1 Co2 O8 95.5(2) 4_665 . ? O6 Co2 O8 151.31(18) . . ? N1 Co2 O3 102.5(2) . 4_665 ? N2 Co2 O3 76.04(19) 4_665 4_665 ? O1 Co2 O3 150.98(18) 4_665 4_665 ? O6 Co2 O3 98.6(2) . 4_665 ? O8 Co2 O3 90.7(2) . 4_665 ? O2w Co3 O4w 88.0(2) . 3_767 ? O2w Co3 O4w 92.0(2) 3_767 3_767 ? O2w Co3 O4w 92.0(2) . . ? O2w Co3 O4w 88.0(2) 3_767 . ? O2w Co3 O3w 87.3(2) . . ? O2w Co3 O3w 92.7(2) 3_767 . ? O4w Co3 O3w 88.02(19) 3_767 . ? O4w Co3 O3w 91.98(19) . . ? O2w Co3 O3w 92.7(2) . 3_767 ? O2w Co3 O3w 87.3(2) 3_767 3_767 ? O4w Co3 O3w 91.98(19) 3_767 3_767 ? O4w Co3 O3w 88.02(19) . 3_767 ? C12 N1 C8 120.7(5) . . ? C12 N1 Co2 119.8(4) . . ? C8 N1 Co2 119.5(4) . . ? C5 N2 C1 120.0(5) . . ? C5 N2 Co2 120.2(4) . 4_566 ? C1 N2 Co2 119.8(4) . 4_566 ? C6 O1 Co2 116.5(4) . 4_566 ? C6 O2 Co1 125.3(4) . 2_446 ? C7 O3 Co2 115.6(4) . 4_566 ? C7 O4 Co1 131.5(4) . . ? C13 O6 Co2 115.9(4) . . ? C14 O8 Co2 116.9(4) . . ? N2 C1 C2 121.5(6) . . ? N2 C1 C7 111.5(6) . . ? C2 C1 C7 127.0(6) . . ? C1 C2 C3 119.5(6) . . ? C2 C3 C4 118.2(6) . . ? C2 C3 C10 120.8(6) . . ? C4 C3 C10 121.0(5) . . ? C5 C4 C3 120.1(6) . . ? N2 C5 C4 120.6(6) . . ? N2 C5 C6 112.2(5) . . ? C4 C5 C6 127.0(6) . . ? O2 C6 O1 125.7(6) . . ? O2 C6 C5 119.7(6) . . ? O1 C6 C5 114.6(5) . . ? O4 C7 O3 126.7(6) . . ? O4 C7 C1 116.3(6) . . ? O3 C7 C1 117.0(6) . . ? N1 C8 C9 120.1(6) . . ? N1 C8 C14 113.1(6) . . ? C9 C8 C14 126.8(6) . . ? C8 C9 C10 120.2(6) . . ? C11 C10 C9 118.8(6) . . ? C11 C10 C3 120.4(6) . . ? C9 C10 C3 120.7(6) . . ? C12 C11 C10 118.1(6) . . ? N1 C12 C11 122.1(6) . . ? N1 C12 C13 111.6(6) . . ? C11 C12 C13 126.2(6) . . ? O5 C13 O6 125.2(6) . . ? O5 C13 C12 118.3(6) . . ? O6 C13 C12 116.5(6) . . ? O7 C14 O8 126.8(7) . . ? O7 C14 C8 118.3(6) . . ? O8 C14 C8 114.8(6) . . ? O4 Co1 O1w 84.53(19) 3_466 . ? O4 Co1 O1w 95.47(19) . . ? O4 Co1 O1w 95.47(19) 3_466 3_466 ? O4 Co1 O1w 84.53(19) . 3_466 ? O4 Co1 O2 89.88(17) 3_466 2_456 ? O4 Co1 O2 90.12(17) . 2_456 ? O1w Co1 O2 91.01(19) . 2_456 ? O1w Co1 O2 88.99(19) 3_466 2_456 ? O4 Co1 O2 90.12(17) 3_466 4_565 ? O4 Co1 O2 89.88(17) . 4_565 ? O1w Co1 O2 88.99(19) . 4_565 ? O1w Co1 O2 91.01(19) 3_466 4_565 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 2.700 _refine_diff_density_min -0.878 _refine_diff_density_rms 0.179