# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Li, Yan' 'Zou, Wen-Qiang' 'Wu, Mei-Feng' 'Lin, Jian-Di' 'Zheng, Fakun' 'Liu, Zhi-Fa' 'Wang, Shuai-Hua' 'Guo, Guo-Cong' 'Huang, Jin-Shun' _publ_contact_author_name 'Zheng, Fakun' _publ_contact_author_email zfk@fjirsm.ac.cn _publ_section_title ; Hydrothermal syntheses, crystal structures and magnetic properties of four Mn(II) and Co(II) coordination polymers generated from new carboxylate-introduced 1,2,3-triazole ligands ; _publ_contact_author_address ; State Key Laboratory of Structural Chemistry, Fujian Institute on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; _publ_contact_author_fax '+86 591 8371 4946' _publ_contact_author_phone '+86 591 8370 4827' # Attachment '- Polymer 1.cif' ## cif for 'Mn(C10H9.50N3O6.25)' data_15 _database_code_depnum_ccdc_archive 'CCDC 813387' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; Mn(C10H9.50N3O6.25) ; _chemical_name_common Mn(C10H9.50N3O6.25) _chemical_melting_point 'not measured' _chemical_formula_moiety Mn(C10H9.50N3O6.25) _chemical_formula_sum 'C10 H9.50 Mn N3 O6.25' _chemical_formula_weight 326.65 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 monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.666(3) _cell_length_b 10.4447(15) _cell_length_c 13.887(7) _cell_angle_alpha 90.00 _cell_angle_beta 122.89(2) _cell_angle_gamma 90.00 _cell_volume 2395.3(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 77 _cell_measurement_theta_min 3.2751 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.812 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8791 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _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 7942 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0140 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2201 _reflns_number_gt 2070 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2002)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2002)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2002)' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0336P)^2^+2.3510P] 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 2201 _refine_ls_number_parameters 206 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0267 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0627 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.303501(14) 0.36686(2) 0.18605(2) 0.02274(10) Uani 1 1 d . . . C10 C 0.57941(9) 0.97432(15) 0.46305(13) 0.0188(3) Uani 1 1 d . . . C11 C 0.51502(9) 1.05409(15) 0.39074(13) 0.0193(3) Uani 1 1 d . . . H11A H 0.5221 1.1424 0.3966 0.023 Uiso 1 1 calc R . . C12 C 0.43981(9) 1.00257(15) 0.30949(13) 0.0192(3) Uani 1 1 d . . . C13 C 0.43000(9) 0.87124(15) 0.30035(14) 0.0204(3) Uani 1 1 d . . . H13A H 0.3806 0.8359 0.2444 0.024 Uiso 1 1 calc R . . C14 C 0.49400(9) 0.79251(14) 0.37468(13) 0.0193(3) Uani 1 1 d . . . C15 C 0.56897(9) 0.84234(15) 0.45637(14) 0.0215(3) Uani 1 1 d . . . H15A H 0.6116 0.7885 0.5059 0.026 Uiso 1 1 calc R . . C16 C 0.66121(9) 1.03011(16) 0.54896(14) 0.0224(3) Uani 1 1 d . . . C17 C 0.36814(9) 1.08651(15) 0.23086(14) 0.0219(3) Uani 1 1 d . . . C18 C 0.53561(11) 0.56073(17) 0.40539(19) 0.0410(5) Uani 1 1 d . . . H18A H 0.5917 0.5671 0.4519 0.049 Uiso 1 1 calc R . . C19 C 0.49045(11) 0.45262(18) 0.36480(19) 0.0419(5) Uani 1 1 d . . . H19A H 0.5104 0.3694 0.3789 0.050 Uiso 1 1 calc R . . N11 N 0.48140(8) 0.65680(13) 0.36360(12) 0.0233(3) Uani 1 1 d . . . N12 N 0.40585(8) 0.61110(13) 0.29978(14) 0.0296(3) Uani 1 1 d . . . N13 N 0.41173(8) 0.48611(13) 0.30059(13) 0.0294(3) Uani 1 1 d . . . O1W O 0.27827(9) 0.32870(18) 0.32042(13) 0.0397(3) Uani 1 1 d D . . H1B H 0.2544(18) 0.386(3) 0.326(3) 0.073(10) Uiso 1 1 d D . . H1A H 0.266(2) 0.258(4) 0.327(3) 0.098(13) Uiso 1 1 d D . . O2W O 0.32024(8) 0.37425(13) 0.04276(11) 0.0286(3) Uani 1 1 d D . . H2B H 0.2825(15) 0.401(2) -0.017(2) 0.046(7) Uiso 1 1 d D . . H2A H 0.3311(14) 0.306(2) 0.026(2) 0.046(7) Uiso 1 1 d D . . O3W O 0.7248(7) 0.7257(13) 0.4779(15) 0.113(4) Uani 0.25 1 d P . . O11 O 0.71944(7) 0.95688(12) 0.61399(11) 0.0317(3) Uani 1 1 d . . . O12 O 0.66995(7) 1.14978(11) 0.55398(11) 0.0293(3) Uani 1 1 d . . . O21 O 0.37936(7) 1.20530(11) 0.24340(11) 0.0335(3) Uani 1 1 d . . . O22 O 0.30264(7) 1.03334(12) 0.15875(11) 0.0329(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.01504(14) 0.01541(15) 0.02564(16) 0.00014(10) 0.00317(12) 0.00213(9) C10 0.0154(7) 0.0187(8) 0.0182(7) -0.0009(6) 0.0065(6) -0.0024(6) C11 0.0206(8) 0.0144(7) 0.0215(8) -0.0001(6) 0.0106(7) -0.0019(6) C12 0.0175(8) 0.0184(8) 0.0197(8) 0.0019(6) 0.0088(7) 0.0024(6) C13 0.0136(7) 0.0186(8) 0.0217(8) -0.0010(6) 0.0049(6) -0.0010(6) C14 0.0171(7) 0.0144(7) 0.0223(8) -0.0012(6) 0.0079(6) -0.0013(6) C15 0.0152(7) 0.0186(8) 0.0217(8) 0.0023(6) 0.0042(6) 0.0022(6) C16 0.0196(8) 0.0228(9) 0.0210(8) -0.0023(7) 0.0086(7) -0.0051(6) C17 0.0200(8) 0.0204(8) 0.0237(8) 0.0050(7) 0.0107(7) 0.0043(6) C18 0.0188(8) 0.0187(9) 0.0569(13) -0.0016(9) 0.0021(9) 0.0028(7) C19 0.0267(9) 0.0154(9) 0.0577(13) -0.0022(9) 0.0062(9) 0.0024(7) N11 0.0163(6) 0.0147(7) 0.0280(7) -0.0014(6) 0.0049(6) -0.0008(5) N12 0.0173(7) 0.0174(7) 0.0380(8) -0.0031(6) 0.0047(6) -0.0028(5) N13 0.0246(7) 0.0157(7) 0.0362(8) -0.0032(6) 0.0090(7) -0.0020(6) O1W 0.0296(7) 0.0443(9) 0.0417(8) 0.0068(7) 0.0172(6) 0.0081(7) O2W 0.0226(6) 0.0256(7) 0.0260(7) -0.0001(6) 0.0057(6) 0.0036(5) O3W 0.114(12) 0.099(11) 0.160(14) -0.006(8) 0.096(12) 0.009(8) O11 0.0171(6) 0.0264(6) 0.0324(7) 0.0013(5) 0.0010(5) -0.0022(5) O12 0.0226(6) 0.0225(6) 0.0315(7) -0.0025(5) 0.0073(5) -0.0079(5) O21 0.0281(6) 0.0178(6) 0.0422(7) 0.0054(5) 0.0110(6) 0.0084(5) O22 0.0186(6) 0.0311(7) 0.0322(7) 0.0087(5) 0.0028(5) 0.0025(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 Mn1 O21 2.1018(12) 1_545 ? Mn1 O2W 2.1875(17) . ? Mn1 O1W 2.2118(18) . ? Mn1 N13 2.2215(15) . ? Mn1 O12 2.2496(14) 8_465 ? Mn1 O11 2.3080(12) 8_465 ? Mn1 C16 2.6129(17) 8_465 ? C10 C11 1.388(2) . ? C10 C15 1.389(2) . ? C10 C16 1.506(2) . ? C11 C12 1.392(2) . ? C11 H11A 0.9300 . ? C12 C13 1.381(2) . ? C12 C17 1.509(2) . ? C13 C14 1.384(2) . ? C13 H13A 0.9300 . ? C14 C15 1.384(2) . ? C14 N11 1.433(2) . ? C15 H15A 0.9300 . ? C16 O12 1.258(2) . ? C16 O11 1.261(2) . ? C16 Mn1 2.6129(17) 8_566 ? C17 O22 1.253(2) . ? C17 O21 1.256(2) . ? C18 N11 1.345(2) . ? C18 C19 1.356(3) . ? C18 H18A 0.9300 . ? C19 N13 1.347(2) . ? C19 H19A 0.9300 . ? N11 N12 1.3383(19) . ? N12 N13 1.310(2) . ? O1W H1B 0.79(3) . ? O1W H1A 0.79(4) . ? O2W H2B 0.80(2) . ? O2W H2A 0.81(2) . ? O3W O3W 0.98(2) 7_666 ? O11 Mn1 2.3080(12) 8_566 ? O12 Mn1 2.2496(14) 8_566 ? O21 Mn1 2.1018(12) 1_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 O21 Mn1 O2W 86.94(6) 1_545 . ? O21 Mn1 O1W 88.50(6) 1_545 . ? O2W Mn1 O1W 170.83(6) . . ? O21 Mn1 N13 88.39(5) 1_545 . ? O2W Mn1 N13 94.17(6) . . ? O1W Mn1 N13 93.64(7) . . ? O21 Mn1 O12 121.41(5) 1_545 8_465 ? O2W Mn1 O12 86.95(6) . 8_465 ? O1W Mn1 O12 88.65(6) . 8_465 ? N13 Mn1 O12 150.18(5) . 8_465 ? O21 Mn1 O11 177.04(5) 1_545 8_465 ? O2W Mn1 O11 90.21(5) . 8_465 ? O1W Mn1 O11 94.22(6) . 8_465 ? N13 Mn1 O11 92.61(5) . 8_465 ? O12 Mn1 O11 57.58(4) 8_465 8_465 ? O21 Mn1 C16 149.97(5) 1_545 8_465 ? O2W Mn1 C16 87.32(6) . 8_465 ? O1W Mn1 C16 92.68(6) . 8_465 ? N13 Mn1 C16 121.43(6) . 8_465 ? O12 Mn1 C16 28.77(5) 8_465 8_465 ? O11 Mn1 C16 28.84(5) 8_465 8_465 ? C11 C10 C15 120.24(14) . . ? C11 C10 C16 120.25(14) . . ? C15 C10 C16 119.51(14) . . ? C10 C11 C12 120.33(14) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 119.48(14) . . ? C13 C12 C17 118.78(14) . . ? C11 C12 C17 121.73(14) . . ? C12 C13 C14 119.77(14) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C15 C14 C13 121.37(14) . . ? C15 C14 N11 120.35(14) . . ? C13 C14 N11 118.27(14) . . ? C14 C15 C10 118.75(14) . . ? C14 C15 H15A 120.6 . . ? C10 C15 H15A 120.6 . . ? O12 C16 O11 121.29(15) . . ? O12 C16 C10 118.91(14) . . ? O11 C16 C10 119.80(15) . . ? O12 C16 Mn1 59.37(8) . 8_566 ? O11 C16 Mn1 62.03(8) . 8_566 ? C10 C16 Mn1 176.00(11) . 8_566 ? O22 C17 O21 125.16(14) . . ? O22 C17 C12 118.16(15) . . ? O21 C17 C12 116.68(14) . . ? N11 C18 C19 104.78(16) . . ? N11 C18 H18A 127.6 . . ? C19 C18 H18A 127.6 . . ? N13 C19 C18 108.48(16) . . ? N13 C19 H19A 125.8 . . ? C18 C19 H19A 125.8 . . ? N12 N11 C18 110.77(14) . . ? N12 N11 C14 119.28(13) . . ? C18 N11 C14 129.91(14) . . ? N13 N12 N11 106.78(13) . . ? N12 N13 C19 109.19(14) . . ? N12 N13 Mn1 120.45(11) . . ? C19 N13 Mn1 129.66(12) . . ? Mn1 O1W H1B 111(2) . . ? Mn1 O1W H1A 119(3) . . ? H1B O1W H1A 117(3) . . ? Mn1 O2W H2B 115.8(16) . . ? Mn1 O2W H2A 115.3(17) . . ? H2B O2W H2A 104(2) . . ? C16 O11 Mn1 89.13(10) . 8_566 ? C16 O12 Mn1 91.85(10) . 8_566 ? C17 O21 Mn1 134.88(11) . 1_565 ? 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 O1W H1B O22 0.79(3) 1.98(3) 2.772(2) 178(3) 4_545 O1W H1A O11 0.79(4) 2.36(4) 3.112(2) 160(3) 5_666 O2W H2B O22 0.80(2) 1.89(3) 2.694(2) 177(2) 7_565 O2W H2A O12 0.81(2) 1.97(3) 2.7604(18) 165(2) 2_645 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.315 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.046 # Attachment '- Polymer 2.CIF' ## cif for 'Mn(H2O)(C10H5N3O4)' data_16 _database_code_depnum_ccdc_archive 'CCDC 813388' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; Mn(H2O)(C10H5N3O4) ; _chemical_name_common Mn(H2O)(C10H5N3O4) _chemical_melting_point 'not measured' _chemical_formula_moiety Mn(H2O)(C10H5N3O4) _chemical_formula_sum 'C10 H7 Mn N3 O5' _chemical_formula_weight 304.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.895(4) _cell_length_b 8.0248(16) _cell_length_c 17.604(4) _cell_angle_alpha 90.00 _cell_angle_beta 120.80(3) _cell_angle_gamma 90.00 _cell_volume 2292.9(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 63 _cell_measurement_theta_min 3.4010 _cell_measurement_theta_max 27.4835 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.173 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7100 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _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 7018 _diffrn_reflns_av_R_equivalents 0.0480 _diffrn_reflns_av_sigmaI/netI 0.1012 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1963 _reflns_number_gt 1525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2002)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2002)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2002)' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0972P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1963 _refine_ls_number_parameters 178 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1735 _refine_ls_wR_factor_gt 0.1697 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.990 _refine_ls_shift/su_max 0.099 _refine_ls_shift/su_mean 0.003 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 0.037471(19) 0.72078(5) 0.46493(2) 0.02151(12) Uani 1 1 d . . . O1W O 0.07751(12) 0.8069(3) 0.60078(14) 0.0536(8) Uani 1 1 d D . . H1WA H 0.0697(7) 0.7394(11) 0.6335(6) 0.080 Uiso 1 1 d D . . H1WB H 0.0477(6) 0.8905(10) 0.5976(12) 0.080 Uiso 1 1 d D . . O1 O 0.08885(11) 0.4867(2) 0.50698(14) 0.0444(7) Uani 1 1 d . . . O2 O 0.08455(10) 0.2378(2) 0.55857(12) 0.0320(6) Uani 1 1 d . . . O3 O 0.34974(10) 0.6686(2) 0.52485(12) 0.0336(5) Uani 1 1 d . . . O4 O 0.46477(9) 0.5259(2) 0.60406(12) 0.0305(5) Uani 1 1 d . . . N1 N 0.37300(12) 0.0150(2) 0.71034(13) 0.0243(6) Uani 1 1 d . . . N2 N 0.44100(12) 0.0214(3) 0.79190(13) 0.0257(6) Uani 1 1 d . . . N3 N 0.45984(12) -0.1353(3) 0.81865(13) 0.0272(6) Uani 1 1 d . . . C1 C 0.33490(14) 0.1657(3) 0.66230(15) 0.0233(7) Uani 1 1 d . . . C2 C 0.25212(14) 0.1884(3) 0.63086(16) 0.0253(7) Uani 1 1 d . . . H2A H 0.2226 0.1094 0.6421 0.030 Uiso 1 1 calc R . . C3 C 0.21290(13) 0.3313(3) 0.58182(15) 0.0217(7) Uani 1 1 d . . . C4 C 0.25829(13) 0.4477(3) 0.56553(15) 0.0215(7) Uani 1 1 d . . . H4A H 0.2326 0.5437 0.5337 0.026 Uiso 1 1 calc R . . C5 C 0.34224(13) 0.4220(3) 0.59650(15) 0.0218(7) Uani 1 1 d . . . C6 C 0.38089(14) 0.2801(3) 0.64563(16) 0.0230(7) Uani 1 1 d . . . H6A H 0.4366 0.2617 0.6671 0.028 Uiso 1 1 calc R . . C7 C 0.12210(14) 0.3540(3) 0.54684(15) 0.0251(7) Uani 1 1 d . . . C8 C 0.38847(14) 0.5465(3) 0.57359(16) 0.0252(7) Uani 1 1 d . . . C9 C 0.40336(18) -0.2375(4) 0.75482(19) 0.0347(9) Uani 1 1 d . . . H9A H 0.4026 -0.3530 0.7582 0.042 Uiso 1 1 calc R . . C10 C 0.34828(16) -0.1442(3) 0.68538(17) 0.0327(9) Uani 1 1 d . . . H10A H 0.3035 -0.1812 0.6324 0.039 Uiso 1 1 calc 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 0.01520(16) 0.0187(2) 0.02967(18) 0.00193(14) 0.01076(13) -0.00035(14) O1W 0.0386(10) 0.0740(16) 0.0409(11) -0.0063(10) 0.0150(8) 0.0199(11) O1 0.0242(9) 0.0255(10) 0.0726(13) 0.0163(9) 0.0170(8) 0.0108(8) O2 0.0173(7) 0.0330(10) 0.0464(10) 0.0073(8) 0.0168(6) -0.0003(7) O3 0.0279(7) 0.0259(10) 0.0496(9) 0.0105(8) 0.0217(6) 0.0011(8) O4 0.0201(7) 0.0263(10) 0.0463(9) -0.0047(8) 0.0179(6) -0.0070(7) N1 0.0223(9) 0.0201(11) 0.0250(9) 0.0048(8) 0.0080(7) 0.0030(8) N2 0.0209(9) 0.0198(11) 0.0285(10) 0.0041(9) 0.0070(7) 0.0021(8) N3 0.0261(9) 0.0227(11) 0.0291(10) 0.0052(9) 0.0115(7) 0.0034(9) C1 0.0221(10) 0.0203(13) 0.0232(10) 0.0019(10) 0.0086(8) 0.0027(10) C2 0.0228(10) 0.0213(13) 0.0309(12) 0.0035(10) 0.0132(8) -0.0016(10) C3 0.0189(9) 0.0193(12) 0.0281(11) 0.0035(10) 0.0128(8) 0.0039(10) C4 0.0211(10) 0.0158(12) 0.0250(11) 0.0027(9) 0.0098(8) 0.0001(9) C5 0.0201(9) 0.0196(13) 0.0255(10) -0.0029(10) 0.0116(7) -0.0038(10) C6 0.0158(10) 0.0249(14) 0.0270(11) 0.0006(10) 0.0099(8) -0.0011(10) C7 0.0183(9) 0.0299(15) 0.0253(11) -0.0041(10) 0.0099(8) 0.0014(11) C8 0.0246(10) 0.0200(13) 0.0341(11) -0.0070(10) 0.0173(8) -0.0078(10) C9 0.0346(14) 0.0241(14) 0.0345(14) 0.0017(11) 0.0098(11) 0.0014(12) C10 0.0366(13) 0.0200(14) 0.0278(13) -0.0001(11) 0.0066(10) -0.0006(12) _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 O1 2.0694(19) . ? Mn1 O2 2.150(2) 5_566 ? Mn1 O1W 2.217(2) . ? Mn1 O3 2.229(2) 7_566 ? Mn1 N3 2.321(2) 8_455 ? Mn1 O4 2.3573(19) 7_566 ? Mn1 C8 2.622(3) 7_566 ? O1W H1WA 0.857(8) . ? O1W H1WB 0.859(8) . ? O1 C7 1.253(3) . ? O2 C7 1.251(3) . ? O2 Mn1 2.150(2) 5_566 ? O3 C8 1.260(3) . ? O3 Mn1 2.229(2) 7_566 ? O4 C8 1.266(3) . ? O4 Mn1 2.3573(19) 7_566 ? N1 N2 1.351(2) . ? N1 C10 1.354(3) . ? N1 C1 1.440(3) . ? N2 N3 1.326(3) . ? N3 C9 1.359(3) . ? N3 Mn1 2.321(2) 8_556 ? C1 C2 1.378(3) . ? C1 C6 1.395(4) . ? C2 C3 1.398(3) . ? C2 H2A 0.9300 . ? C3 C4 1.393(4) . ? C3 C7 1.508(3) . ? C4 C5 1.404(3) . ? C4 H4A 0.9300 . ? C5 C6 1.390(3) . ? C5 C8 1.512(4) . ? C6 H6A 0.9300 . ? C8 Mn1 2.622(3) 7_566 ? C9 C10 1.354(4) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? 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 Mn1 O2 118.02(8) . 5_566 ? O1 Mn1 O1W 93.36(9) . . ? O2 Mn1 O1W 84.22(9) 5_566 . ? O1 Mn1 O3 94.50(8) . 7_566 ? O2 Mn1 O3 147.22(7) 5_566 7_566 ? O1W Mn1 O3 90.26(9) . 7_566 ? O1 Mn1 N3 92.46(8) . 8_455 ? O2 Mn1 N3 79.97(8) 5_566 8_455 ? O1W Mn1 N3 164.09(8) . 8_455 ? O3 Mn1 N3 104.02(8) 7_566 8_455 ? O1 Mn1 O4 148.04(9) . 7_566 ? O2 Mn1 O4 91.88(7) 5_566 7_566 ? O1W Mn1 O4 101.13(8) . 7_566 ? O3 Mn1 O4 57.48(6) 7_566 7_566 ? N3 Mn1 O4 81.30(7) 8_455 7_566 ? O1 Mn1 C8 121.61(9) . 7_566 ? O2 Mn1 C8 120.12(8) 5_566 7_566 ? O1W Mn1 C8 97.14(9) . 7_566 ? O3 Mn1 C8 28.68(7) 7_566 7_566 ? N3 Mn1 C8 92.37(8) 8_455 7_566 ? O4 Mn1 C8 28.82(7) 7_566 7_566 ? Mn1 O1W H1WA 116.6(7) . . ? Mn1 O1W H1WB 108.8(12) . . ? H1WA O1W H1WB 101.8(14) . . ? C7 O1 Mn1 168.7(2) . . ? C7 O2 Mn1 119.73(16) . 5_566 ? C8 O3 Mn1 93.25(16) . 7_566 ? C8 O4 Mn1 87.30(15) . 7_566 ? N2 N1 C10 111.29(19) . . ? N2 N1 C1 120.64(19) . . ? C10 N1 C1 128.05(18) . . ? N3 N2 N1 106.12(18) . . ? N2 N3 C9 108.91(19) . . ? N2 N3 Mn1 125.21(15) . 8_556 ? C9 N3 Mn1 121.48(18) . 8_556 ? C2 C1 C6 122.0(2) . . ? C2 C1 N1 118.0(2) . . ? C6 C1 N1 119.9(2) . . ? C1 C2 C3 119.3(2) . . ? C1 C2 H2A 120.3 . . ? C3 C2 H2A 120.3 . . ? C4 C3 C2 119.3(2) . . ? C4 C3 C7 121.8(2) . . ? C2 C3 C7 118.9(2) . . ? C3 C4 C5 120.9(2) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 119.4(2) . . ? C6 C5 C8 121.1(2) . . ? C4 C5 C8 119.5(2) . . ? C5 C6 C1 119.0(2) . . ? C5 C6 H6A 120.5 . . ? C1 C6 H6A 120.5 . . ? O2 C7 O1 124.2(2) . . ? O2 C7 C3 117.7(2) . . ? O1 C7 C3 118.1(2) . . ? O3 C8 O4 121.9(3) . . ? O3 C8 C5 118.8(2) . . ? O4 C8 C5 119.3(2) . . ? O3 C8 Mn1 58.07(14) . 7_566 ? O4 C8 Mn1 63.88(14) . 7_566 ? C5 C8 Mn1 175.94(19) . 7_566 ? C10 C9 N3 109.2(2) . . ? C10 C9 H9A 125.4 . . ? N3 C9 H9A 125.4 . . ? N1 C10 C9 104.5(2) . . ? N1 C10 H10A 127.7 . . ? C9 C10 H10A 127.7 . . ? 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 O1W H1WA N2 0.857(8) 2.257(8) 3.101(3) 168.1(12) 4_556 O1W H1WB O4 0.859(8) 1.957(11) 2.785(3) 161.4(15) 3_455 _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.842 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.137 # Attachment '- Polymer 3.CIF' ## cif for 'Co(C10H11N3O7)' data_14 _database_code_depnum_ccdc_archive 'CCDC 813389' #===================================================================== # start Validation Reply Form _vrf_PLAT430_14 ; PROBLEM: "Short Inter D...A Contact O3W .. O4W .. 1.98 Ang." RESPONSE: It is caused by the disorder of water molecules. ; # end Validation Reply Form #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Co(C10H11N3O7)' ; _chemical_name_common Co(C10H11N3O7) _chemical_melting_point 'not measured' _chemical_formula_moiety Co(C10H11N3O7) _chemical_formula_sum 'C10 H11 Co N3 O7' _chemical_formula_weight 344.15 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)/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 10.446(3) _cell_length_b 16.862(2) _cell_length_c 7.3912(15) _cell_angle_alpha 90.00 _cell_angle_beta 96.063(19) _cell_angle_gamma 90.00 _cell_volume 1294.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 6 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 1.365 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.8659 _exptl_absorpt_correction_T_max 0.9922 _exptl_absorpt_process_details 'Psi (Rigaku WinAFC)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 3 _diffrn_standards_interval_time 200 _diffrn_standards_decay_% 1.6063 _diffrn_reflns_number 2590 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0961 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -2 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.35 _reflns_number_total 2358 _reflns_number_gt 1524 _reflns_threshold_expression >2sigma(I) _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction 'CrystalStructure Version 3.10' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.1273P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2358 _refine_ls_number_parameters 211 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1204 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.2214 _refine_ls_wR_factor_gt 0.1881 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 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 0.358064(14) 0.926502(9) 0.23007(3) 0.02330(4) Uani 1 1 d . . . O1W O 0.36875(8) 0.93390(5) -0.04911(13) 0.0376(3) Uani 1 1 d D . . H1WA H 0.4133(2) 0.9061(2) -0.1172(4) 0.056 Uiso 1 1 d D . . H1WB H 0.29755(18) 0.9083(2) -0.0528(10) 0.056 Uiso 1 1 d D . . O2W O 0.37046(8) 0.93006(5) 0.51221(12) 0.0354(3) Uani 1 1 d D . . H2WA H 0.45296(17) 0.9268(8) 0.5301(8) 0.053 Uiso 1 1 d D . . H2WB H 0.3518(3) 0.9311(9) 0.6228(3) 0.053 Uiso 1 1 d D . . O3W O 1.0947(3) 0.52063(15) 0.1103(5) 0.1117(14) Uani 0.50 1 d P . . O4W O 1.0583(3) 0.5056(2) 0.3651(10) 0.270(3) Uani 0.50 1 d P . . O11 O 0.58643(8) 0.56089(5) 0.26031(14) 0.0352(3) Uani 1 1 d . . . O12 O 0.78319(8) 0.51582(5) 0.27989(15) 0.0375(3) Uani 1 1 d . . . O13 O 0.67938(10) 0.93509(6) 0.2683(2) 0.0775(5) Uani 1 1 d . . . O14 O 0.51375(8) 0.85201(6) 0.24991(15) 0.0404(3) Uani 1 1 d . . . N11 N 1.06588(9) 0.75910(6) 0.21499(15) 0.0233(3) Uani 1 1 d . . . N12 N 1.11354(9) 0.83221(6) 0.23133(17) 0.0297(3) Uani 1 1 d . . . N13 N 1.23655(9) 0.82721(6) 0.20780(15) 0.0253(3) Uani 1 1 d . . . C10 C 0.71925(11) 0.79677(7) 0.25470(18) 0.0237(3) Uani 1 1 d . . . C11 C 0.67470(11) 0.71977(8) 0.26317(18) 0.0279(4) Uani 1 1 d . . . H11A H 0.5876 0.7107 0.2705 0.033 Uiso 1 1 calc R . . C12 C 0.75721(11) 0.65646(7) 0.26092(18) 0.0247(3) Uani 1 1 d . . . C13 C 0.88780(11) 0.66804(7) 0.24384(18) 0.0241(3) Uani 1 1 d . . . H13A H 0.9438 0.6253 0.2395 0.029 Uiso 1 1 calc R . . C14 C 0.93128(10) 0.74616(7) 0.23344(18) 0.0231(3) Uani 1 1 d . . . C15 C 0.85000(11) 0.80973(7) 0.23636(19) 0.0266(4) Uani 1 1 d . . . H15A H 0.8811 0.8610 0.2263 0.032 Uiso 1 1 calc R . . C16 C 0.63186(12) 0.86716(7) 0.2566(2) 0.0336(4) Uani 1 1 d . . . C17 C 0.70655(11) 0.57349(7) 0.26610(19) 0.0272(4) Uani 1 1 d . . . C19 C 1.15822(12) 0.70713(8) 0.1788(2) 0.0431(5) Uani 1 1 d . . . H19A H 1.1492 0.6528 0.1604 0.052 Uiso 1 1 calc R . . C20 C 1.26488(12) 0.75012(8) 0.1748(2) 0.0409(5) Uani 1 1 d . . . H20A H 1.3452 0.7307 0.1532 0.049 Uiso 1 1 calc 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 0.01321(6) 0.01353(7) 0.04391(9) -0.00126(8) 0.00650(6) -0.00001(6) O1W 0.0335(5) 0.0293(5) 0.0523(6) 0.0026(5) 0.0151(4) 0.0039(4) O2W 0.0314(5) 0.0309(5) 0.0444(5) -0.0011(5) 0.0066(4) 0.0076(4) O3W 0.142(2) 0.0180(11) 0.184(3) -0.0034(16) 0.061(2) 0.0106(14) O4W 0.0673(16) 0.093(2) 0.611(9) -0.103(4) -0.143(3) 0.0524(17) O11 0.0219(4) 0.0270(5) 0.0570(6) 0.0019(4) 0.0059(4) -0.0049(4) O12 0.0273(4) 0.0169(4) 0.0688(7) 0.0031(5) 0.0071(5) 0.0008(4) O13 0.0294(5) 0.0186(5) 0.1872(15) 0.0033(7) 0.0248(7) 0.0036(4) O14 0.0164(4) 0.0273(5) 0.0777(7) 0.0008(5) 0.0065(4) 0.0030(4) N11 0.0134(4) 0.0152(4) 0.0413(6) -0.0067(5) 0.0024(4) -0.0033(4) N12 0.0130(4) 0.0145(5) 0.0617(7) 0.0015(5) 0.0040(5) -0.0025(4) N13 0.0164(4) 0.0181(5) 0.0427(6) -0.0001(5) 0.0086(4) -0.0049(4) C10 0.0149(5) 0.0194(5) 0.0378(7) -0.0016(5) 0.0071(5) 0.0015(5) C11 0.0151(5) 0.0269(6) 0.0421(7) 0.0056(6) 0.0053(5) -0.0039(5) C12 0.0186(5) 0.0209(6) 0.0352(7) 0.0027(6) 0.0059(5) -0.0020(5) C13 0.0185(5) 0.0152(5) 0.0391(7) -0.0034(5) 0.0057(5) 0.0029(5) C14 0.0098(5) 0.0156(5) 0.0444(7) -0.0001(5) 0.0047(5) -0.0011(4) C15 0.0222(6) 0.0107(5) 0.0474(8) -0.0044(6) 0.0055(6) -0.0020(5) C16 0.0217(6) 0.0143(5) 0.0652(9) -0.0001(6) 0.0069(6) 0.0029(5) C17 0.0167(5) 0.0207(6) 0.0447(7) 0.0003(6) 0.0054(5) -0.0015(5) C19 0.0264(6) 0.0128(6) 0.0912(11) -0.0016(7) 0.0115(7) 0.0032(5) C20 0.0150(5) 0.0236(6) 0.0854(11) -0.0068(7) 0.0109(7) -0.0008(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 Co1 O14 2.0478(10) . ? Co1 O2W 2.0766(10) . ? Co1 O1W 2.0820(11) . ? Co1 N13 2.0970(10) 1_455 ? Co1 O12 2.1043(9) 2_655 ? Co1 O11 2.3382(9) 2_655 ? O1W H1WA 0.860(3) . ? O1W H1WB 0.858(3) . ? O2W H2WA 0.860(2) . ? O2W H2WB 0.861(2) . ? O11 C17 1.2689(15) . ? O11 Co1 2.3382(9) 2_645 ? O12 C17 1.2568(15) . ? O12 Co1 2.1043(9) 2_645 ? O13 C16 1.2477(16) . ? O14 C16 1.2558(15) . ? N11 N12 1.3303(14) . ? N11 C19 1.3508(17) . ? N11 C14 1.4435(15) . ? N12 N13 1.3175(14) . ? N13 C20 1.3607(17) . ? N13 Co1 2.0970(10) 1_655 ? C10 C11 1.3829(17) . ? C10 C15 1.4038(17) . ? C10 C16 1.4984(17) . ? C11 C12 1.3731(17) . ? C11 H11A 0.9300 . ? C12 C13 1.3969(17) . ? C12 C17 1.4977(17) . ? C13 C14 1.3981(16) . ? C13 H13A 0.9300 . ? C14 C15 1.3691(16) . ? C15 H15A 0.9300 . ? C19 C20 1.3321(19) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? 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 O14 Co1 O2W 88.91(4) . . ? O14 Co1 O1W 88.99(4) . . ? O2W Co1 O1W 171.65(3) . . ? O14 Co1 N13 89.17(4) . 1_455 ? O2W Co1 N13 94.29(4) . 1_455 ? O1W Co1 N13 93.75(4) . 1_455 ? O14 Co1 O12 171.94(4) . 2_655 ? O2W Co1 O12 89.06(4) . 2_655 ? O1W Co1 O12 91.91(4) . 2_655 ? N13 Co1 O12 98.76(4) 1_455 2_655 ? O14 Co1 O11 113.56(4) . 2_655 ? O2W Co1 O11 87.28(4) . 2_655 ? O1W Co1 O11 86.16(4) . 2_655 ? N13 Co1 O11 157.26(3) 1_455 2_655 ? O12 Co1 O11 58.54(3) 2_655 2_655 ? Co1 O1W H1WA 129.5(2) . . ? Co1 O1W H1WB 82.2(5) . . ? H1WA O1W H1WB 103.2(4) . . ? Co1 O2W H2WA 96.2(4) . . ? Co1 O2W H2WB 163.4(2) . . ? H2WA O2W H2WB 100.3(5) . . ? C17 O11 Co1 85.42(7) . 2_645 ? C17 O12 Co1 96.47(7) . 2_645 ? C16 O14 Co1 130.36(8) . . ? N12 N11 C19 110.55(10) . . ? N12 N11 C14 119.36(9) . . ? C19 N11 C14 130.08(10) . . ? N13 N12 N11 106.83(9) . . ? N12 N13 C20 108.57(10) . . ? N12 N13 Co1 121.95(8) . 1_655 ? C20 N13 Co1 129.45(8) . 1_655 ? C11 C10 C15 119.08(11) . . ? C11 C10 C16 122.35(11) . . ? C15 C10 C16 118.52(10) . . ? C12 C11 C10 120.98(11) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 120.84(11) . . ? C11 C12 C17 120.13(11) . . ? C13 C12 C17 118.94(10) . . ? C12 C13 C14 117.56(10) . . ? C12 C13 H13A 121.2 . . ? C14 C13 H13A 121.2 . . ? C15 C14 C13 122.09(11) . . ? C15 C14 N11 119.68(10) . . ? C13 C14 N11 118.22(10) . . ? C14 C15 C10 119.40(11) . . ? C14 C15 H15A 120.3 . . ? C10 C15 H15A 120.3 . . ? O13 C16 O14 124.86(12) . . ? O13 C16 C10 119.31(11) . . ? O14 C16 C10 115.82(11) . . ? O12 C17 O11 119.49(11) . . ? O12 C17 C12 120.07(10) . . ? O11 C17 C12 120.42(10) . . ? C20 C19 N11 105.52(12) . . ? C20 C19 H19A 127.2 . . ? N11 C19 H19A 127.2 . . ? C19 C20 N13 108.53(12) . . ? C19 C20 H20A 125.7 . . ? N13 C20 H20A 125.7 . . ? 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 O1W H1WA O11 0.860(3) 2.178(3) 2.7998(15) 129.0(3) 4_575 O1W H1WB N13 0.858(3) 2.499(6) 3.0501(15) 122.8(5) 1_455 O2W H2WA O11 0.860(2) 2.093(5) 2.7571(14) 133.6(5) 4_576 O2W H2WB O1W 0.861(2) 2.413(2) 3.2449(15) 162.8(3) 1_556 O2W H2WB O13 0.861(2) 2.429(13) 2.8726(16) 112.7(11) 3_676 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.769 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.166 # Attachment '- Polymer 4.cif' ## cif for 'Co3(C22H36N6O26)' data_2 _database_code_depnum_ccdc_archive 'CCDC 813390' #===================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'Co3(C22H36N6O26)' ; _chemical_name_common Co3(C22H36N6O26) _chemical_melting_point 'not measured' _chemical_formula_moiety Co3(C22H36N6O26) _chemical_formula_sum 'C22 H36 Co3 N6 O26' _chemical_formula_weight 977.36 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.994(3) _cell_length_b 10.990(4) _cell_length_c 12.008(5) _cell_angle_alpha 82.639(10) _cell_angle_beta 82.527(10) _cell_angle_gamma 71.827(9) _cell_volume 865.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2075 _cell_measurement_theta_min 3.0817 _cell_measurement_theta_max 27.4835 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 499 _exptl_absorpt_coefficient_mu 1.533 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8856 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating-anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury CCD' _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 6913 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3914 _reflns_number_gt 3120 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2002)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2002)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2002)' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0456P)^2^+0.5559P] 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 3914 _refine_ls_number_parameters 304 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.029 _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 0.0000 0.5000 0.5000 0.02015(14) Uani 1 2 d S . . Co2 Co 0.0000 0.0000 0.0000 0.02033(14) Uani 1 2 d S . . Co3 Co 0.5000 1.0000 0.5000 0.02669(15) Uani 1 2 d S . . O1W O 0.4180(4) 1.1304(3) 0.3595(2) 0.0468(7) Uani 1 1 d D . . H1WA H 0.472(5) 1.188(3) 0.330(3) 0.070 Uiso 1 1 d D . . H1WB H 0.293(2) 1.163(4) 0.347(4) 0.070 Uiso 1 1 d D . . O2W O 0.2293(4) 0.9596(3) 0.5190(2) 0.0459(6) Uani 1 1 d D . . H2WA H 0.136(5) 0.975(4) 0.574(2) 0.069 Uiso 1 1 d D . . H2WB H 0.183(6) 0.924(4) 0.474(3) 0.069 Uiso 1 1 d D . . O3W O 0.1732(4) -0.0641(2) 0.14076(19) 0.0355(5) Uani 1 1 d D . . H3WA H 0.146(5) -0.089(4) 0.2097(13) 0.053 Uiso 1 1 d D . . H3WB H 0.3015(18) -0.077(4) 0.134(3) 0.053 Uiso 1 1 d D . . O4W O 0.2581(4) -0.1029(2) -0.0965(2) 0.0402(6) Uani 1 1 d D . . H4WA H 0.279(6) -0.160(3) -0.142(3) 0.060 Uiso 1 1 d D . . H4WB H 0.315(6) -0.047(3) -0.128(3) 0.060 Uiso 1 1 d D . . O5W O 0.3121(3) 0.4075(2) 0.52764(16) 0.0244(4) Uani 1 1 d D . . H5WA H 0.386(4) 0.414(3) 0.4661(15) 0.037 Uiso 1 1 d D . . H5WB H 0.348(5) 0.448(3) 0.573(2) 0.037 Uiso 1 1 d D . . O6W O 0.3839(4) 1.1434(2) 0.61141(19) 0.0406(6) Uani 1 1 d D . . H6WA H 0.397(6) 1.134(3) 0.6821(11) 0.061 Uiso 1 1 d D . . H6WB H 0.358(6) 1.2237(13) 0.592(3) 0.061 Uiso 1 1 d D . . O7W O 0.0303(6) 1.1706(4) 0.3233(4) 0.0883(12) Uani 1 1 d D . . H7WA H -0.090(4) 1.224(5) 0.319(5) 0.132 Uiso 1 1 d D . . H7WB H 0.054(9) 1.141(6) 0.258(3) 0.132 Uiso 1 1 d D . . O11 O 0.3954(3) 0.1055(2) -0.14783(18) 0.0326(5) Uani 1 1 d . . . O12 O 0.1189(3) 0.15167(19) -0.02432(17) 0.0256(4) Uani 1 1 d . . . O13 O 0.3798(4) 0.70599(19) -0.23970(17) 0.0338(5) Uani 1 1 d . . . O14 O 0.4479(3) 0.5437(2) -0.34588(15) 0.0272(5) Uani 1 1 d . . . O15 O 0.1175(4) 0.8338(2) 0.35972(18) 0.0398(6) Uani 1 1 d . . . O16 O 0.0477(3) 0.68036(19) 0.48465(16) 0.0275(5) Uani 1 1 d . . . N11 N 0.1724(3) 0.5303(2) 0.15255(17) 0.0163(4) Uani 1 1 d . . . N12 N 0.1145(4) 0.4566(2) 0.24137(18) 0.0210(5) Uani 1 1 d . . . N13 N 0.0764(4) 0.5253(2) 0.32725(18) 0.0202(5) Uani 1 1 d . . . C11 C 0.3344(4) 0.5091(3) -0.1527(2) 0.0167(5) Uani 1 1 d . . . C12 C 0.3433(4) 0.3826(3) -0.1627(2) 0.0185(5) Uani 1 1 d . . . H20A H 0.3880 0.3481 -0.2316 0.022 Uiso 1 1 calc R . . C13 C 0.2854(4) 0.3075(3) -0.0700(2) 0.0186(5) Uani 1 1 d . . . C14 C 0.2280(4) 0.3564(3) 0.0347(2) 0.0186(5) Uani 1 1 d . . . H16A H 0.1906 0.3064 0.0971 0.022 Uiso 1 1 calc R . . C15 C 0.2277(4) 0.4805(2) 0.0443(2) 0.0149(5) Uani 1 1 d . . . C16 C 0.2765(4) 0.5580(2) -0.0483(2) 0.0182(5) Uani 1 1 d . . . H13A H 0.2705 0.6423 -0.0406 0.022 Uiso 1 1 calc R . . C17 C 0.3902(4) 0.5934(3) -0.2537(2) 0.0195(5) Uani 1 1 d . . . C18 C 0.2677(4) 0.1766(3) -0.0820(2) 0.0195(6) Uani 1 1 d . . . C19 C 0.1709(4) 0.6448(3) 0.1821(2) 0.0188(5) Uani 1 1 d . . . H19A H 0.2040 0.7115 0.1362 0.023 Uiso 1 1 calc R . . C20 C 0.1093(4) 0.6406(3) 0.2953(2) 0.0187(5) Uani 1 1 d . . . C21 C 0.0893(5) 0.7266(3) 0.3857(2) 0.0251(6) 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 Co1 0.0311(3) 0.0194(3) 0.0120(2) -0.00134(19) 0.0027(2) -0.0124(2) Co2 0.0278(3) 0.0141(3) 0.0208(3) -0.00259(19) 0.0039(2) -0.0109(2) Co3 0.0356(3) 0.0230(3) 0.0230(3) -0.0017(2) -0.0017(2) -0.0116(3) O1W 0.0488(16) 0.0461(16) 0.0466(15) 0.0216(12) -0.0138(13) -0.0221(14) O2W 0.0391(15) 0.0592(18) 0.0477(16) -0.0135(13) 0.0000(12) -0.0247(14) O3W 0.0390(14) 0.0419(14) 0.0289(12) 0.0078(10) -0.0045(10) -0.0206(12) O4W 0.0495(15) 0.0265(12) 0.0478(14) -0.0179(10) 0.0226(11) -0.0211(12) O5W 0.0320(12) 0.0263(11) 0.0171(10) -0.0036(8) 0.0024(8) -0.0132(9) O6W 0.0658(17) 0.0246(12) 0.0279(12) -0.0049(9) -0.0035(12) -0.0078(12) O7W 0.073(3) 0.064(2) 0.130(4) -0.003(2) -0.044(2) -0.013(2) O11 0.0409(13) 0.0229(11) 0.0357(12) -0.0131(9) 0.0146(10) -0.0153(10) O12 0.0316(12) 0.0184(10) 0.0299(11) -0.0042(8) 0.0067(9) -0.0152(9) O13 0.0621(16) 0.0187(11) 0.0227(11) -0.0033(8) 0.0097(10) -0.0199(11) O14 0.0422(13) 0.0295(11) 0.0148(9) -0.0047(8) 0.0059(8) -0.0203(10) O15 0.0728(18) 0.0303(12) 0.0264(11) -0.0044(9) 0.0021(11) -0.0321(13) O16 0.0447(13) 0.0242(11) 0.0176(10) -0.0038(8) 0.0014(9) -0.0173(10) N11 0.0206(12) 0.0169(11) 0.0115(10) -0.0014(8) 0.0006(8) -0.0069(9) N12 0.0307(13) 0.0218(12) 0.0121(10) -0.0010(8) 0.0031(9) -0.0126(11) N13 0.0288(13) 0.0213(12) 0.0128(10) -0.0021(9) 0.0009(9) -0.0116(10) C11 0.0196(13) 0.0184(13) 0.0141(12) -0.0003(9) -0.0010(10) -0.0091(11) C12 0.0222(14) 0.0188(13) 0.0164(12) -0.0041(10) -0.0004(10) -0.0083(11) C13 0.0206(14) 0.0169(13) 0.0205(13) -0.0027(10) -0.0007(10) -0.0090(11) C14 0.0222(14) 0.0178(13) 0.0166(12) 0.0009(10) 0.0019(10) -0.0094(11) C15 0.0161(13) 0.0166(13) 0.0127(12) -0.0011(9) -0.0023(9) -0.0057(10) C16 0.0251(14) 0.0137(12) 0.0176(13) -0.0019(10) 0.0021(10) -0.0101(11) C17 0.0226(14) 0.0237(14) 0.0149(12) -0.0011(10) -0.0016(10) -0.0110(12) C18 0.0289(15) 0.0161(13) 0.0148(12) 0.0007(10) -0.0023(11) -0.0094(12) C19 0.0254(14) 0.0175(13) 0.0148(12) -0.0001(10) 0.0006(10) -0.0098(11) C20 0.0236(14) 0.0170(13) 0.0158(12) -0.0026(10) 0.0013(10) -0.0074(11) C21 0.0359(17) 0.0221(15) 0.0189(14) -0.0019(11) 0.0005(12) -0.0121(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 Co1 N13 2.079(2) 2_566 ? Co1 N13 2.079(2) . ? Co1 O16 2.092(2) . ? Co1 O16 2.092(2) 2_566 ? Co1 O5W 2.151(2) 2_566 ? Co1 O5W 2.151(2) . ? Co2 O12 2.0573(19) . ? Co2 O12 2.0573(19) 2 ? Co2 O4W 2.097(2) 2 ? Co2 O4W 2.097(2) . ? Co2 O3W 2.125(2) 2 ? Co2 O3W 2.125(2) . ? Co3 O2W 2.054(2) 2_676 ? Co3 O2W 2.054(2) . ? Co3 O1W 2.085(2) . ? Co3 O1W 2.085(2) 2_676 ? Co3 O6W 2.096(2) . ? Co3 O6W 2.096(2) 2_676 ? O1W H1WA 0.859(10) . ? O1W H1WB 0.861(10) . ? O2W H2WA 0.854(10) . ? O2W H2WB 0.859(10) . ? O3W H3WA 0.854(10) . ? O3W H3WB 0.858(10) . ? O4W H4WA 0.848(10) . ? O4W H4WB 0.852(10) . ? O5W H5WA 0.854(10) . ? O5W H5WB 0.853(10) . ? O6W H6WA 0.855(10) . ? O6W H6WB 0.852(10) . ? O7W H7WA 0.865(10) . ? O7W H7WB 0.866(10) . ? O11 C18 1.254(3) . ? O12 C18 1.257(3) . ? O13 C17 1.249(3) . ? O14 C17 1.260(3) . ? O15 C21 1.249(3) . ? O16 C21 1.266(3) . ? N11 C19 1.347(3) . ? N11 N12 1.352(3) . ? N11 C15 1.435(3) . ? N12 N13 1.307(3) . ? N13 C20 1.356(3) . ? C11 C16 1.389(3) . ? C11 C12 1.393(4) . ? C11 C17 1.515(4) . ? C12 C13 1.393(4) . ? C12 H20A 0.9300 . ? C13 C14 1.392(4) . ? C13 C18 1.508(4) . ? C14 C15 1.383(4) . ? C14 H16A 0.9300 . ? C15 C16 1.385(3) . ? C16 H13A 0.9300 . ? C19 C20 1.371(3) . ? C19 H19A 0.9300 . ? C20 C21 1.494(4) . ? 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 N13 Co1 N13 180.000(1) 2_566 . ? N13 Co1 O16 101.08(8) 2_566 . ? N13 Co1 O16 78.92(8) . . ? N13 Co1 O16 78.92(8) 2_566 2_566 ? N13 Co1 O16 101.08(8) . 2_566 ? O16 Co1 O16 180.0 . 2_566 ? N13 Co1 O5W 90.89(9) 2_566 2_566 ? N13 Co1 O5W 89.11(9) . 2_566 ? O16 Co1 O5W 89.55(8) . 2_566 ? O16 Co1 O5W 90.45(8) 2_566 2_566 ? N13 Co1 O5W 89.11(9) 2_566 . ? N13 Co1 O5W 90.89(9) . . ? O16 Co1 O5W 90.45(8) . . ? O16 Co1 O5W 89.55(8) 2_566 . ? O5W Co1 O5W 180.00(10) 2_566 . ? O12 Co2 O12 180.00(14) . 2 ? O12 Co2 O4W 92.66(8) . 2 ? O12 Co2 O4W 87.34(8) 2 2 ? O12 Co2 O4W 87.34(8) . . ? O12 Co2 O4W 92.66(8) 2 . ? O4W Co2 O4W 180.0(2) 2 . ? O12 Co2 O3W 94.07(9) . 2 ? O12 Co2 O3W 85.93(9) 2 2 ? O4W Co2 O3W 86.46(11) 2 2 ? O4W Co2 O3W 93.54(11) . 2 ? O12 Co2 O3W 85.93(9) . . ? O12 Co2 O3W 94.07(9) 2 . ? O4W Co2 O3W 93.54(11) 2 . ? O4W Co2 O3W 86.46(11) . . ? O3W Co2 O3W 180.00(7) 2 . ? O2W Co3 O2W 180.000(1) 2_676 . ? O2W Co3 O1W 87.80(11) 2_676 . ? O2W Co3 O1W 92.20(11) . . ? O2W Co3 O1W 92.20(11) 2_676 2_676 ? O2W Co3 O1W 87.80(11) . 2_676 ? O1W Co3 O1W 180.00(10) . 2_676 ? O2W Co3 O6W 89.20(11) 2_676 . ? O2W Co3 O6W 90.80(11) . . ? O1W Co3 O6W 92.55(11) . . ? O1W Co3 O6W 87.45(11) 2_676 . ? O2W Co3 O6W 90.80(11) 2_676 2_676 ? O2W Co3 O6W 89.20(11) . 2_676 ? O1W Co3 O6W 87.45(11) . 2_676 ? O1W Co3 O6W 92.55(11) 2_676 2_676 ? O6W Co3 O6W 180.000(1) . 2_676 ? Co3 O1W H1WA 128(3) . . ? Co3 O1W H1WB 121(3) . . ? H1WA O1W H1WB 104(2) . . ? Co3 O2W H2WA 128(3) . . ? Co3 O2W H2WB 128(2) . . ? H2WA O2W H2WB 104(2) . . ? Co2 O3W H3WA 134(2) . . ? Co2 O3W H3WB 122(2) . . ? H3WA O3W H3WB 104(2) . . ? Co2 O4W H4WA 134(3) . . ? Co2 O4W H4WB 106(3) . . ? H4WA O4W H4WB 107(2) . . ? Co1 O5W H5WA 109(2) . . ? Co1 O5W H5WB 110(2) . . ? H5WA O5W H5WB 105(2) . . ? Co3 O6W H6WA 126(3) . . ? Co3 O6W H6WB 124(2) . . ? H6WA O6W H6WB 106(2) . . ? H7WA O7W H7WB 101(2) . . ? C18 O12 Co2 136.13(18) . . ? C21 O16 Co1 116.54(17) . . ? C19 N11 N12 111.8(2) . . ? C19 N11 C15 129.0(2) . . ? N12 N11 C15 119.2(2) . . ? N13 N12 N11 105.5(2) . . ? N12 N13 C20 110.6(2) . . ? N12 N13 Co1 137.06(18) . . ? C20 N13 Co1 112.16(16) . . ? C16 C11 C12 119.5(2) . . ? C16 C11 C17 119.6(2) . . ? C12 C11 C17 120.9(2) . . ? C13 C12 C11 120.3(2) . . ? C13 C12 H20A 119.9 . . ? C11 C12 H20A 119.9 . . ? C14 C13 C12 120.1(2) . . ? C14 C13 C18 118.4(2) . . ? C12 C13 C18 121.3(2) . . ? C15 C14 C13 118.9(2) . . ? C15 C14 H16A 120.6 . . ? C13 C14 H16A 120.6 . . ? C14 C15 C16 121.5(2) . . ? C14 C15 N11 119.0(2) . . ? C16 C15 N11 119.5(2) . . ? C15 C16 C11 119.6(2) . . ? C15 C16 H13A 120.2 . . ? C11 C16 H13A 120.2 . . ? O13 C17 O14 124.5(2) . . ? O13 C17 C11 118.1(2) . . ? O14 C17 C11 117.4(2) . . ? O11 C18 O12 126.6(2) . . ? O11 C18 C13 118.9(2) . . ? O12 C18 C13 114.5(2) . . ? N11 C19 C20 104.3(2) . . ? N11 C19 H19A 127.8 . . ? C20 C19 H19A 127.8 . . ? N13 C20 C19 107.8(2) . . ? N13 C20 C21 117.3(2) . . ? C19 C20 C21 134.7(2) . . ? O15 C21 O16 125.7(3) . . ? O15 C21 C20 119.3(2) . . ? O16 C21 C20 114.9(2) . . ? 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 O1W H1WA O13 0.859(10) 1.929(14) 2.775(3) 168(4) 2_675 O1W H1WB O7W 0.861(10) 1.870(17) 2.691(5) 159(4) . O2W H2WA O15 0.854(10) 2.44(3) 3.107(4) 136(4) 2_576 O2W H2WA O7W 0.854(10) 2.39(4) 2.993(5) 128(4) 2_576 O2W H2WB O15 0.859(10) 1.962(11) 2.815(3) 172(4) . O3W H3WA O15 0.854(10) 1.904(12) 2.752(3) 172(4) 1_545 O3W H3WB O11 0.858(10) 2.071(13) 2.919(3) 170(3) 2_655 O4W H4WA O13 0.848(10) 1.905(13) 2.743(3) 169(4) 1_545 O4W H4WB O11 0.852(10) 1.909(15) 2.721(3) 159(3) . O5W H5WA O14 0.854(10) 1.838(12) 2.679(3) 168(3) 2_665 O5W H5WB O14 0.853(10) 1.854(11) 2.701(3) 172(3) 1_556 O6W H6WA O11 0.855(10) 2.026(12) 2.876(3) 173(4) 1_566 O6W H6WB O5W 0.852(10) 2.008(11) 2.856(3) 174(4) 1_565 O7W H7WA O13 0.865(10) 2.23(3) 3.008(4) 150(5) 2_575 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.695 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.082