Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 1350 _publ_contact_author_name 'Ning-Hai Hu' _publ_contact_author_address ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P.R.China ; _publ_contact_author_fax 86-431-85685653 _publ_contact_author_email hunh@ciac.jl.cn _publ_requested_journal CrystEngComm _publ_section_title ; Constructing porous frameworks from one-dimensional cobalt oxygen clusters and pyridinedicarboxylate ligands adopting two rare coordination modes ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Li, Zhi-Gang' ? ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P. R. China ; 'Wang, Guan-Hua' ? ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P. R. China ; 'Jia, Heng-Qing' ? ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P. R. China ; 'Hu, Ning-Hai' ? ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P. R. China ; 'Xu, Jing-Wei' ? ; Changchun Institute of Applied Chemistry Chinese Academy of Sciences Changchun 130022 P. R. China ; data_l070 _database_code_depnum_ccdc_archive 'CCDC 664033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14.50 H20 Co3 N2 O15.50' _chemical_formula_weight 647.11 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 11.1193(12) _cell_length_b 11.2473(12) _cell_length_c 11.3620(12) _cell_angle_alpha 75.651(2) _cell_angle_beta 66.119(1) _cell_angle_gamma 76.991(2) _cell_volume 1246.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 165(2) _cell_measurement_reflns_used 2742 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 25.49 _exptl_crystal_description block _exptl_crystal_colour dark-pink _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 2.047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6172 _exptl_absorpt_correction_T_max 0.8683 _exptl_absorpt_process_details 'SADABS (Sheldrick,1996)' _diffrn_ambient_temperature 165(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6742 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0430 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.52 _reflns_number_total 4548 _reflns_number_gt 3831 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0651P)^2^+3.7978P] 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 4548 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.10894(6) 0.38861(5) 0.49877(5) 0.01111(17) Uani 1 1 d . . . Co2 Co -0.02891(6) 0.43127(5) 0.28995(5) 0.01110(17) Uani 1 1 d . . . Co3 Co -0.00083(6) 0.64226(5) -0.00891(5) 0.01231(17) Uani 1 1 d . . . O1 O 0.0489(3) 0.3755(3) 0.7003(3) 0.0151(7) Uani 1 1 d . . . O2 O -0.0353(3) 0.2540(3) 0.8957(3) 0.0200(7) Uani 1 1 d . . . O3 O 0.0365(3) -0.2440(3) 0.6776(3) 0.0197(7) Uani 1 1 d . . . O4 O -0.0393(3) -0.1916(3) 0.8764(3) 0.0211(7) Uani 1 1 d . . . O5 O 0.1616(3) 0.4056(3) 0.3004(3) 0.0158(7) Uani 1 1 d . . . O6 O 0.3232(3) 0.4352(4) 0.1038(3) 0.0294(9) Uani 1 1 d . . . O7 O 0.7981(3) 0.3589(3) 0.1375(3) 0.0183(7) Uani 1 1 d . . . O8 O 0.7748(3) 0.4580(3) 0.2972(3) 0.0173(7) Uani 1 1 d . . . O9 O 0.0506(3) 0.4711(3) 0.0941(3) 0.0122(6) Uani 1 1 d . . . H7 H 0.1268 0.4761 0.0781 0.015 Uiso 1 1 d . . . O10 O -0.0817(3) 0.4257(3) 0.4903(3) 0.0126(6) Uani 1 1 d . . . O11 O -0.2062(3) 0.6777(3) 0.1172(3) 0.0262(8) Uani 1 1 d . . . N1 N 0.1048(4) 0.1967(3) 0.5707(4) 0.0142(8) Uani 1 1 d . . . N2 N 0.3191(4) 0.3674(3) 0.4272(4) 0.0147(8) Uani 1 1 d . . . C1 C 0.0150(5) 0.2735(4) 0.7734(4) 0.0143(9) Uani 1 1 d . . . C2 C 0.0450(4) 0.1677(4) 0.7013(4) 0.0147(9) Uani 1 1 d . . . C3 C 0.0147(5) 0.0502(4) 0.7649(4) 0.0171(10) Uani 1 1 d . . . H3 H -0.0278 0.0325 0.8573 0.021 Uiso 1 1 calc R . . C4 C 0.0481(5) -0.0416(4) 0.6900(4) 0.0158(10) Uani 1 1 d . . . C5 C 0.1145(5) -0.0126(4) 0.5558(5) 0.0189(10) Uani 1 1 d . . . H5 H 0.1418 -0.0745 0.5030 0.023 Uiso 1 1 calc R . . C6 C 0.1403(5) 0.1072(4) 0.5000(4) 0.0180(10) Uani 1 1 d . . . H6 H 0.1850 0.1267 0.4080 0.022 Uiso 1 1 calc R . . C7 C 0.0122(5) -0.1707(4) 0.7537(4) 0.0156(10) Uani 1 1 d . . . C8 C 0.2818(5) 0.4138(4) 0.2244(5) 0.0183(10) Uani 1 1 d . . . C9 C 0.3768(4) 0.3932(4) 0.2955(4) 0.0150(9) Uani 1 1 d . . . C10 C 0.5103(5) 0.4026(4) 0.2311(5) 0.0176(10) Uani 1 1 d . . . H10 H 0.5481 0.4196 0.1383 0.021 Uiso 1 1 calc R . . C11 C 0.5883(5) 0.3867(4) 0.3050(5) 0.0170(10) Uani 1 1 d . . . C12 C 0.5297(5) 0.3596(5) 0.4407(5) 0.0223(11) Uani 1 1 d . . . H12 H 0.5808 0.3489 0.4933 0.027 Uiso 1 1 calc R . . C13 C 0.3952(5) 0.3484(5) 0.4978(5) 0.0199(10) Uani 1 1 d . . . H13 H 0.3560 0.3265 0.5902 0.024 Uiso 1 1 calc R . . C14 C 0.7330(5) 0.4022(4) 0.2404(4) 0.0162(10) Uani 1 1 d . . . O1W O -0.2672(7) 0.1543(7) 1.0731(7) 0.097(2) Uani 1 1 d . . . O2W O -0.3152(9) -0.1037(8) 1.2053(9) 0.091(3) Uani 0.80 1 d P . . O3W O 0.5232(9) 0.2598(10) -0.0360(10) 0.100(3) Uani 0.75 1 d P . . O3W' O 0.431(3) 0.286(3) -0.081(3) 0.090(8) Uiso 0.25 1 d P . . O4W O 0.3091(9) 0.1072(12) 0.1397(14) 0.124(5) Uani 0.70 1 d P . . C15 C -0.1827(10) 0.3494(9) 0.5836(9) 0.018(2) Uani 0.50 1 d P . . O5W O -0.2934(13) 0.2949(12) 0.6782(12) 0.087(4) Uani 0.50 1 d P . . O6W O 0.5798(14) 0.1255(16) -0.2468(14) 0.102(5) Uani 0.50 1 d P . . 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 0.0146(3) 0.0115(3) 0.0075(3) -0.0023(2) -0.0031(2) -0.0035(2) Co2 0.0152(3) 0.0115(3) 0.0074(3) -0.0024(2) -0.0036(2) -0.0036(2) Co3 0.0187(3) 0.0111(3) 0.0073(3) -0.0020(2) -0.0037(2) -0.0044(2) O1 0.0231(17) 0.0124(16) 0.0106(16) -0.0027(12) -0.0053(13) -0.0048(13) O2 0.0310(19) 0.0192(17) 0.0106(17) -0.0039(13) -0.0044(14) -0.0101(14) O3 0.036(2) 0.0122(16) 0.0128(16) -0.0023(13) -0.0095(15) -0.0062(14) O4 0.033(2) 0.0138(16) 0.0136(17) -0.0012(13) -0.0052(15) -0.0055(14) O5 0.0125(16) 0.0260(18) 0.0100(16) -0.0069(13) -0.0028(13) -0.0029(13) O6 0.0214(19) 0.056(3) 0.0100(18) -0.0014(16) -0.0060(15) -0.0089(17) O7 0.0170(16) 0.0263(18) 0.0110(16) -0.0051(13) -0.0013(13) -0.0074(14) O8 0.0144(16) 0.0225(17) 0.0174(17) -0.0073(13) -0.0046(13) -0.0052(13) O9 0.0130(15) 0.0147(16) 0.0093(15) -0.0017(12) -0.0031(12) -0.0049(12) O10 0.0153(16) 0.0124(15) 0.0095(15) -0.0025(12) -0.0035(13) -0.0025(12) O11 0.0220(18) 0.0213(18) 0.026(2) -0.0042(15) -0.0009(15) -0.0008(14) N1 0.020(2) 0.0125(19) 0.0105(19) -0.0030(15) -0.0050(16) -0.0039(15) N2 0.0151(19) 0.0157(19) 0.0119(19) -0.0022(15) -0.0031(16) -0.0033(15) C1 0.019(2) 0.016(2) 0.011(2) -0.0041(17) -0.0057(18) -0.0061(18) C2 0.016(2) 0.014(2) 0.014(2) -0.0029(18) -0.0052(18) -0.0029(18) C3 0.023(2) 0.019(2) 0.010(2) -0.0017(18) -0.0063(19) -0.0044(19) C4 0.023(2) 0.012(2) 0.014(2) -0.0012(17) -0.0071(19) -0.0057(18) C5 0.026(3) 0.017(2) 0.016(2) -0.0072(18) -0.007(2) -0.0025(19) C6 0.027(3) 0.017(2) 0.011(2) -0.0046(18) -0.006(2) -0.0037(19) C7 0.021(2) 0.013(2) 0.014(2) -0.0011(18) -0.0078(19) -0.0037(18) C8 0.020(2) 0.019(2) 0.016(2) -0.0050(19) -0.005(2) -0.0048(19) C9 0.014(2) 0.017(2) 0.012(2) -0.0027(17) -0.0037(18) -0.0020(18) C10 0.019(2) 0.020(2) 0.015(2) -0.0044(18) -0.0045(19) -0.0056(19) C11 0.020(2) 0.016(2) 0.015(2) -0.0048(18) -0.0047(19) -0.0055(19) C12 0.023(3) 0.032(3) 0.016(2) -0.006(2) -0.009(2) -0.006(2) C13 0.019(2) 0.029(3) 0.011(2) -0.0019(19) -0.0042(19) -0.008(2) C14 0.018(2) 0.018(2) 0.013(2) 0.0007(18) -0.0060(19) -0.0056(19) O1W 0.089(5) 0.094(5) 0.094(5) -0.033(4) 0.003(4) -0.039(4) O2W 0.084(6) 0.088(6) 0.095(6) -0.029(5) -0.017(5) -0.015(5) O3W 0.078(6) 0.124(8) 0.104(7) -0.068(7) -0.021(6) -0.001(6) O4W 0.050(6) 0.164(12) 0.172(12) -0.074(10) -0.044(7) 0.015(6) C15 0.023(5) 0.017(5) 0.014(5) 0.002(4) -0.006(4) -0.007(4) O5W 0.083(9) 0.077(8) 0.073(8) -0.019(7) 0.015(7) -0.031(7) O6W 0.077(9) 0.147(14) 0.096(11) -0.040(10) -0.011(8) -0.063(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.056(3) . ? Co1 O10 2.069(3) 2_566 ? Co1 O1 2.085(3) . ? Co1 O10 2.103(3) . ? Co1 N1 2.114(4) . ? Co1 N2 2.118(4) . ? Co2 O9 2.007(3) . ? Co2 O3 2.061(3) 2_556 ? Co2 O10 2.096(3) . ? Co2 O8 2.106(3) 1_455 ? Co2 O5 2.121(3) . ? Co2 O1 2.161(3) 2_566 ? Co3 O9 2.057(3) 2_565 ? Co3 O4 2.063(3) 1_564 ? Co3 O9 2.081(3) . ? Co3 O2 2.133(3) 2_566 ? Co3 O7 2.133(3) 2_665 ? Co3 O11 2.157(3) . ? O1 C1 1.272(5) . ? O1 Co2 2.161(3) 2_566 ? O2 C1 1.251(5) . ? O2 Co3 2.133(3) 2_566 ? O3 C7 1.251(6) . ? O3 Co2 2.061(3) 2_556 ? O4 C7 1.256(6) . ? O4 Co3 2.063(3) 1_546 ? O5 C8 1.274(6) . ? O6 C8 1.234(6) . ? O7 C14 1.252(6) . ? O7 Co3 2.133(3) 2_665 ? O8 C14 1.265(6) . ? O8 Co2 2.106(3) 1_655 ? O9 Co3 2.057(3) 2_565 ? O9 H7 0.8034 . ? O10 C15 1.463(9) . ? O10 Co1 2.069(3) 2_566 ? N1 C6 1.334(6) . ? N1 C2 1.345(6) . ? N2 C13 1.338(6) . ? N2 C9 1.350(6) . ? C1 C2 1.510(6) . ? C2 C3 1.384(6) . ? C3 C4 1.391(6) . ? C3 H3 0.9500 . ? C4 C5 1.388(7) . ? C4 C7 1.516(6) . ? C5 C6 1.380(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.520(7) . ? C9 C10 1.379(6) . ? C10 C11 1.391(7) . ? C10 H10 0.9500 . ? C11 C12 1.392(7) . ? C11 C14 1.505(6) . ? C12 C13 1.390(7) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? O3W O3W' 1.27(3) . ? C15 O5W 1.410(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O10 98.79(12) . 2_566 ? O5 Co1 O1 177.89(13) . . ? O10 Co1 O1 80.13(12) 2_566 . ? O5 Co1 O10 80.79(12) . . ? O10 Co1 O10 85.45(12) 2_566 . ? O1 Co1 O10 97.29(12) . . ? O5 Co1 N1 104.50(14) . . ? O10 Co1 N1 156.54(13) 2_566 . ? O1 Co1 N1 76.50(13) . . ? O10 Co1 N1 95.42(13) . . ? O5 Co1 N2 76.78(13) . . ? O10 Co1 N2 95.29(13) 2_566 . ? O1 Co1 N2 105.09(14) . . ? O10 Co1 N2 157.41(13) . . ? N1 Co1 N2 92.74(15) . . ? O9 Co2 O3 101.95(12) . 2_556 ? O9 Co2 O10 164.52(12) . . ? O3 Co2 O10 90.78(12) 2_556 . ? O9 Co2 O8 94.07(12) . 1_455 ? O3 Co2 O8 86.49(13) 2_556 1_455 ? O10 Co2 O8 95.49(12) . 1_455 ? O9 Co2 O5 90.79(12) . . ? O3 Co2 O5 93.96(13) 2_556 . ? O10 Co2 O5 79.45(12) . . ? O8 Co2 O5 174.93(12) 1_455 . ? O9 Co2 O1 90.08(12) . 2_566 ? O3 Co2 O1 167.63(12) 2_556 2_566 ? O10 Co2 O1 77.81(12) . 2_566 ? O8 Co2 O1 89.85(12) 1_455 2_566 ? O5 Co2 O1 88.66(12) . 2_566 ? O9 Co3 O4 97.75(13) 2_565 1_564 ? O9 Co3 O9 80.76(13) 2_565 . ? O4 Co3 O9 175.54(12) 1_564 . ? O9 Co3 O2 172.16(12) 2_565 2_566 ? O4 Co3 O2 87.76(13) 1_564 2_566 ? O9 Co3 O2 94.15(12) . 2_566 ? O9 Co3 O7 97.26(12) 2_565 2_665 ? O4 Co3 O7 86.66(13) 1_564 2_665 ? O9 Co3 O7 89.35(12) . 2_665 ? O2 Co3 O7 88.59(13) 2_566 2_665 ? O9 Co3 O11 90.00(13) 2_565 . ? O4 Co3 O11 85.53(13) 1_564 . ? O9 Co3 O11 98.65(12) . . ? O2 Co3 O11 84.85(14) 2_566 . ? O7 Co3 O11 169.99(13) 2_665 . ? C1 O1 Co1 118.2(3) . . ? C1 O1 Co2 140.5(3) . 2_566 ? Co1 O1 Co2 99.65(12) . 2_566 ? C1 O2 Co3 121.8(3) . 2_566 ? C7 O3 Co2 132.1(3) . 2_556 ? C7 O4 Co3 123.9(3) . 1_546 ? C8 O5 Co1 119.7(3) . . ? C8 O5 Co2 139.3(3) . . ? Co1 O5 Co2 100.14(13) . . ? C14 O7 Co3 131.9(3) . 2_665 ? C14 O8 Co2 125.4(3) . 1_655 ? Co2 O9 Co3 111.76(13) . 2_565 ? Co2 O9 Co3 121.65(15) . . ? Co3 O9 Co3 99.24(13) 2_565 . ? Co2 O9 H7 104.2 . . ? Co3 O9 H7 121.4 2_565 . ? Co3 O9 H7 99.2 . . ? C15 O10 Co1 118.7(4) . 2_566 ? C15 O10 Co2 118.6(4) . . ? Co1 O10 Co2 102.31(13) 2_566 . ? C15 O10 Co1 119.0(4) . . ? Co1 O10 Co1 94.55(12) 2_566 . ? Co2 O10 Co1 99.40(12) . . ? C6 N1 C2 118.5(4) . . ? C6 N1 Co1 126.8(3) . . ? C2 N1 Co1 114.2(3) . . ? C13 N2 C9 118.5(4) . . ? C13 N2 Co1 126.7(3) . . ? C9 N2 Co1 114.1(3) . . ? O2 C1 O1 126.2(4) . . ? O2 C1 C2 119.3(4) . . ? O1 C1 C2 114.5(4) . . ? N1 C2 C3 122.8(4) . . ? N1 C2 C1 114.7(4) . . ? C3 C2 C1 122.5(4) . . ? C2 C3 C4 118.3(4) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C5 C4 C3 118.8(4) . . ? C5 C4 C7 120.6(4) . . ? C3 C4 C7 120.6(4) . . ? C6 C5 C4 119.2(4) . . ? C6 C5 H5 120.4 . . ? C4 C5 H5 120.4 . . ? N1 C6 C5 122.3(4) . . ? N1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? O3 C7 O4 127.5(4) . . ? O3 C7 C4 116.0(4) . . ? O4 C7 C4 116.5(4) . . ? O6 C8 O5 125.7(4) . . ? O6 C8 C9 120.5(4) . . ? O5 C8 C9 113.8(4) . . ? N2 C9 C10 122.8(4) . . ? N2 C9 C8 114.4(4) . . ? C10 C9 C8 122.8(4) . . ? C9 C10 C11 118.5(4) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C10 C11 C12 119.0(4) . . ? C10 C11 C14 121.0(4) . . ? C12 C11 C14 120.0(4) . . ? C13 C12 C11 118.8(5) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? N2 C13 C12 122.3(4) . . ? N2 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? O7 C14 O8 127.5(4) . . ? O7 C14 C11 116.8(4) . . ? O8 C14 C11 115.7(4) . . ? O5W C15 O10 170.4(10) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.52 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.926 _refine_diff_density_min -0.612 _refine_diff_density_rms 0.139 # start Validation Reply Form _vrf_PLAT220_l070 ; PROBLEM: Large Non-Solvent O Ueq(max)/Ueq(min) ... 7.21 Ratio RESPONSE: The disordered solvent water molecules resulted in larger Ueq for O atoms. ; _vrf_PLAT306_l070 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W RESPONSE: The hydrogen atoms on the lattice water molecule were not located in difference Fourier maps. ; _vrf_PLAT430_l070 ; PROBLEM: Short Inter D...A Contact O5W .. O6W .. 2.40 Ang. RESPONSE: Both O5W and O6W are half-occupied, so this short contact is meaningless. Some short contacts should be hydrogen-bonding interactions with H atoms not located. ; data_l079 _database_code_depnum_ccdc_archive 'CCDC 664034' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H10 Co3 N2 O11' _chemical_formula_weight 559.03 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 11.1575(8) _cell_length_b 11.2606(8) _cell_length_c 11.4240(9) _cell_angle_alpha 76.7620(10) _cell_angle_beta 65.8140(10) _cell_angle_gamma 80.6800(10) _cell_volume 1270.77(16) _cell_formula_units_Z 2 _cell_measurement_temperature 187(2) _cell_measurement_reflns_used 4871 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 26.01 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 554 _exptl_absorpt_coefficient_mu 1.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 187(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7808 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0255 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.02 _reflns_number_total 4869 _reflns_number_gt 4395 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0419P)^2^+0.1556P] 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 4869 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0696 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.10282(2) 0.39292(2) 0.49932(2) 0.01223(8) Uani 1 1 d . . . Co2 Co -0.02916(2) 0.42820(2) 0.28977(2) 0.01232(8) Uani 1 1 d . . . Co3 Co 0.00718(2) 0.64072(2) -0.00867(2) 0.01375(8) Uani 1 1 d . . . O1 O 0.03904(14) 0.38043(11) 0.70146(12) 0.0171(3) Uani 1 1 d . . . O2 O -0.04994(14) 0.25945(12) 0.89608(12) 0.0204(3) Uani 1 1 d . . . O3 O 0.03856(15) -0.24233(12) 0.68297(13) 0.0227(3) Uani 1 1 d . . . O4 O -0.02686(15) -0.19396(12) 0.88146(13) 0.0241(3) Uani 1 1 d . . . O5 O 0.15894(13) 0.40662(13) 0.30093(12) 0.0178(3) Uani 1 1 d . . . O6 O 0.32358(15) 0.43219(17) 0.10489(13) 0.0361(4) Uani 1 1 d . . . O7 O 0.79104(13) 0.35872(13) 0.13605(13) 0.0218(3) Uani 1 1 d . . . O8 O 0.77736(13) 0.44887(13) 0.29853(13) 0.0205(3) Uani 1 1 d . . . O9 O 0.04948(12) 0.47010(11) 0.09374(12) 0.0140(3) Uani 1 1 d . . . H7 H 0.1268 0.4761 0.0781 0.017 Uiso 1 1 d . . . O10 O -0.08278(12) 0.42420(11) 0.48836(11) 0.0127(3) Uani 1 1 d . . . H10A H -0.1466 0.3725 0.5390 0.015 Uiso 1 1 d . . . O11 O -0.19388(15) 0.67085(14) 0.12803(14) 0.0294(4) Uani 1 1 d . . . N1 N 0.09289(16) 0.20295(14) 0.57214(15) 0.0154(3) Uani 1 1 d . . . N2 N 0.31226(16) 0.37644(14) 0.42741(15) 0.0169(3) Uani 1 1 d . . . C1 C 0.00346(19) 0.27884(17) 0.77458(18) 0.0155(4) Uani 1 1 d . . . C2 C 0.03406(19) 0.17282(17) 0.70372(18) 0.0155(4) Uani 1 1 d . . . C3 C 0.0090(2) 0.05381(17) 0.76818(18) 0.0174(4) Uani 1 1 d . . . H3 H -0.0319 0.0356 0.8607 0.021 Uiso 1 1 calc R . . C4 C 0.04506(19) -0.03848(17) 0.69473(18) 0.0174(4) Uani 1 1 d . . . C5 C 0.1071(2) -0.00831(18) 0.56071(19) 0.0209(4) Uani 1 1 d . . . H5 H 0.1341 -0.0700 0.5086 0.025 Uiso 1 1 calc R . . C6 C 0.1297(2) 0.11353(18) 0.50273(18) 0.0201(4) Uani 1 1 d . . . H6 H 0.1729 0.1335 0.4105 0.024 Uiso 1 1 calc R . . C7 C 0.01670(19) -0.16916(17) 0.75850(18) 0.0175(4) Uani 1 1 d . . . C8 C 0.2804(2) 0.41387(19) 0.22474(19) 0.0203(4) Uani 1 1 d . . . C9 C 0.37248(19) 0.39606(18) 0.29585(18) 0.0183(4) Uani 1 1 d . . . C10 C 0.5068(2) 0.40140(19) 0.23157(19) 0.0203(4) Uani 1 1 d . . . H10 H 0.5465 0.4142 0.1390 0.024 Uiso 1 1 calc R . . C11 C 0.58373(19) 0.38769(18) 0.30505(19) 0.0189(4) Uani 1 1 d . . . C12 C 0.5218(2) 0.36624(19) 0.44043(19) 0.0215(4) Uani 1 1 d . . . H12 H 0.5716 0.3558 0.4929 0.026 Uiso 1 1 calc R . . C13 C 0.3867(2) 0.36027(19) 0.49749(19) 0.0212(4) Uani 1 1 d . . . H13 H 0.3451 0.3441 0.5900 0.025 Uiso 1 1 calc R . . C14 C 0.73019(19) 0.39787(17) 0.24035(18) 0.0167(4) 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 0.01392(14) 0.01257(13) 0.01097(13) -0.00340(9) -0.00501(10) -0.00082(10) Co2 0.01484(15) 0.01284(14) 0.01103(13) -0.00365(9) -0.00561(10) -0.00204(10) Co3 0.01846(15) 0.01248(14) 0.01106(13) -0.00331(10) -0.00547(11) -0.00220(10) O1 0.0266(8) 0.0130(7) 0.0133(6) -0.0031(5) -0.0085(6) -0.0029(6) O2 0.0304(8) 0.0189(7) 0.0112(6) -0.0041(5) -0.0046(6) -0.0070(6) O3 0.0406(9) 0.0132(7) 0.0178(7) -0.0031(5) -0.0135(6) -0.0048(6) O4 0.0421(9) 0.0135(7) 0.0157(7) -0.0025(5) -0.0111(6) 0.0000(6) O5 0.0131(7) 0.0286(8) 0.0128(6) -0.0062(6) -0.0050(5) -0.0008(6) O6 0.0179(8) 0.0759(13) 0.0130(7) -0.0060(7) -0.0051(6) -0.0050(8) O7 0.0166(7) 0.0320(8) 0.0167(7) -0.0085(6) -0.0030(6) -0.0050(6) O8 0.0156(7) 0.0258(7) 0.0236(7) -0.0091(6) -0.0080(6) -0.0030(6) O9 0.0143(7) 0.0163(7) 0.0120(6) -0.0021(5) -0.0052(5) -0.0027(5) O10 0.0132(7) 0.0135(6) 0.0116(6) -0.0031(5) -0.0041(5) -0.0028(5) O11 0.0240(8) 0.0304(8) 0.0288(8) -0.0086(7) -0.0055(7) 0.0032(7) N1 0.0190(9) 0.0151(8) 0.0134(7) -0.0035(6) -0.0072(7) -0.0007(6) N2 0.0154(9) 0.0184(8) 0.0169(8) -0.0064(6) -0.0049(7) -0.0002(6) C1 0.0169(10) 0.0165(9) 0.0162(9) -0.0056(7) -0.0085(8) -0.0005(7) C2 0.0171(10) 0.0165(9) 0.0153(9) -0.0049(7) -0.0076(8) -0.0010(7) C3 0.0224(11) 0.0170(10) 0.0133(9) -0.0032(7) -0.0072(8) -0.0018(8) C4 0.0216(11) 0.0156(9) 0.0182(9) -0.0035(7) -0.0105(8) -0.0018(8) C5 0.0306(12) 0.0173(10) 0.0182(9) -0.0085(8) -0.0105(9) -0.0001(8) C6 0.0274(12) 0.0188(10) 0.0135(9) -0.0047(8) -0.0063(8) -0.0021(8) C7 0.0207(11) 0.0147(9) 0.0189(10) -0.0033(8) -0.0098(8) 0.0000(8) C8 0.0176(11) 0.0271(11) 0.0192(10) -0.0051(8) -0.0093(8) -0.0027(8) C9 0.0178(10) 0.0214(10) 0.0166(9) -0.0050(8) -0.0071(8) -0.0011(8) C10 0.0195(11) 0.0267(11) 0.0158(9) -0.0061(8) -0.0064(8) -0.0031(8) C11 0.0163(10) 0.0211(10) 0.0209(10) -0.0060(8) -0.0074(8) -0.0022(8) C12 0.0212(11) 0.0280(11) 0.0194(10) -0.0073(8) -0.0109(8) -0.0005(9) C13 0.0198(11) 0.0302(11) 0.0144(9) -0.0062(8) -0.0062(8) -0.0023(9) C14 0.0175(10) 0.0158(9) 0.0175(9) -0.0007(7) -0.0086(8) -0.0010(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O5 2.0641(13) . ? Co1 O10 2.0661(13) 2_566 ? Co1 O10 2.0938(13) . ? Co1 O1 2.0967(13) . ? Co1 N1 2.1135(16) . ? Co1 N2 2.1276(16) . ? Co2 O9 2.0119(12) . ? Co2 O3 2.0577(13) 2_556 ? Co2 O10 2.0872(12) . ? Co2 O8 2.0965(14) 1_455 ? Co2 O5 2.1260(13) . ? Co2 O1 2.1631(13) 2_566 ? Co3 O9 2.0532(13) 2_565 ? Co3 O4 2.0681(14) 1_564 ? Co3 O9 2.1005(13) . ? Co3 O2 2.1178(13) 2_566 ? Co3 O7 2.1217(14) 2_665 ? Co3 O11 2.1707(15) . ? O1 C1 1.266(2) . ? O1 Co2 2.1631(13) 2_566 ? O2 C1 1.247(2) . ? O2 Co3 2.1178(13) 2_566 ? O3 C7 1.253(2) . ? O3 Co2 2.0578(13) 2_556 ? O4 C7 1.262(2) . ? O4 Co3 2.0680(14) 1_546 ? O5 C8 1.280(2) . ? O6 C8 1.229(2) . ? O7 C14 1.247(2) . ? O7 Co3 2.1217(14) 2_665 ? O8 C14 1.268(2) . ? O8 Co2 2.0964(14) 1_655 ? O9 Co3 2.0531(13) 2_565 ? O9 H7 0.8172 . ? O10 Co1 2.0660(13) 2_566 ? O10 H10A 0.9072 . ? N1 C6 1.333(2) . ? N1 C2 1.355(2) . ? N2 C13 1.339(3) . ? N2 C9 1.352(2) . ? C1 C2 1.510(2) . ? C2 C3 1.385(3) . ? C3 C4 1.391(3) . ? C3 H3 0.9500 . ? C4 C5 1.381(3) . ? C4 C7 1.506(3) . ? C5 C6 1.394(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C9 1.516(3) . ? C9 C10 1.377(3) . ? C10 C11 1.397(3) . ? C10 H10 0.9500 . ? C11 C12 1.391(3) . ? C11 C14 1.504(3) . ? C12 C13 1.381(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Co1 O10 100.25(5) . 2_566 ? O5 Co1 O10 80.29(5) . . ? O10 Co1 O10 85.87(5) 2_566 . ? O5 Co1 O1 178.02(5) . . ? O10 Co1 O1 79.43(5) 2_566 . ? O10 Co1 O1 97.74(5) . . ? O5 Co1 N1 103.91(6) . . ? O10 Co1 N1 155.78(5) 2_566 . ? O10 Co1 N1 96.34(6) . . ? O1 Co1 N1 76.37(5) . . ? O5 Co1 N2 76.53(6) . . ? O10 Co1 N2 95.45(6) 2_566 . ? O10 Co1 N2 156.66(6) . . ? O1 Co1 N2 105.43(6) . . ? N1 Co1 N2 91.92(6) . . ? O9 Co2 O3 100.68(5) . 2_556 ? O9 Co2 O10 164.48(5) . . ? O3 Co2 O10 92.63(5) 2_556 . ? O9 Co2 O8 93.16(5) . 1_455 ? O3 Co2 O8 87.51(6) 2_556 1_455 ? O10 Co2 O8 95.37(5) . 1_455 ? O9 Co2 O5 92.34(5) . . ? O3 Co2 O5 92.56(6) 2_556 . ? O10 Co2 O5 79.03(5) . . ? O8 Co2 O5 174.40(5) 1_455 . ? O9 Co2 O1 89.52(5) . 2_566 ? O3 Co2 O1 169.70(5) 2_556 2_566 ? O10 Co2 O1 77.47(5) . 2_566 ? O8 Co2 O1 90.59(5) 1_455 2_566 ? O5 Co2 O1 88.35(5) . 2_566 ? O9 Co3 O4 97.53(5) 2_565 1_564 ? O9 Co3 O9 81.12(5) 2_565 . ? O4 Co3 O9 176.94(5) 1_564 . ? O9 Co3 O2 172.10(5) 2_565 2_566 ? O4 Co3 O2 88.01(5) 1_564 2_566 ? O9 Co3 O2 93.61(5) . 2_566 ? O9 Co3 O7 97.62(5) 2_565 2_665 ? O4 Co3 O7 88.59(6) 1_564 2_665 ? O9 Co3 O7 88.88(5) . 2_665 ? O2 Co3 O7 88.10(5) 2_566 2_665 ? O9 Co3 O11 91.76(5) 2_565 . ? O4 Co3 O11 86.10(6) 1_564 . ? O9 Co3 O11 96.67(5) . . ? O2 Co3 O11 82.97(6) 2_566 . ? O7 Co3 O11 169.75(6) 2_665 . ? C1 O1 Co1 118.41(11) . . ? C1 O1 Co2 140.88(12) . 2_566 ? Co1 O1 Co2 99.69(5) . 2_566 ? C1 O2 Co3 121.52(12) . 2_566 ? C7 O3 Co2 133.78(12) . 2_556 ? C7 O4 Co3 125.55(13) . 1_546 ? C8 O5 Co1 120.02(12) . . ? C8 O5 Co2 139.24(12) . . ? Co1 O5 Co2 100.10(5) . . ? C14 O7 Co3 131.13(13) . 2_665 ? C14 O8 Co2 127.95(13) . 1_655 ? Co2 O9 Co3 112.38(6) . 2_565 ? Co2 O9 Co3 122.17(6) . . ? Co3 O9 Co3 98.88(5) 2_565 . ? Co2 O9 H7 102.5 . . ? Co3 O9 H7 122.4 2_565 . ? Co3 O9 H7 99.4 . . ? Co1 O10 Co2 103.25(5) 2_566 . ? Co1 O10 Co1 94.13(5) 2_566 . ? Co2 O10 Co1 100.41(5) . . ? Co1 O10 H10A 122.8 2_566 . ? Co2 O10 H10A 112.2 . . ? Co1 O10 H10A 120.4 . . ? C6 N1 C2 118.24(16) . . ? C6 N1 Co1 127.05(13) . . ? C2 N1 Co1 114.54(12) . . ? C13 N2 C9 118.49(17) . . ? C13 N2 Co1 126.90(13) . . ? C9 N2 Co1 114.31(13) . . ? O2 C1 O1 126.34(17) . . ? O2 C1 C2 118.91(16) . . ? O1 C1 C2 114.73(16) . . ? N1 C2 C3 122.73(17) . . ? N1 C2 C1 114.48(16) . . ? C3 C2 C1 122.74(16) . . ? C2 C3 C4 118.61(17) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 118.77(17) . . ? C5 C4 C7 119.98(17) . . ? C3 C4 C7 121.25(17) . . ? C4 C5 C6 119.35(18) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? N1 C6 C5 122.28(17) . . ? N1 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? O3 C7 O4 126.66(18) . . ? O3 C7 C4 116.04(16) . . ? O4 C7 C4 117.29(17) . . ? O6 C8 O5 125.55(18) . . ? O6 C8 C9 120.80(18) . . ? O5 C8 C9 113.65(16) . . ? N2 C9 C10 122.52(18) . . ? N2 C9 C8 114.78(17) . . ? C10 C9 C8 122.69(17) . . ? C9 C10 C11 118.77(18) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 118.62(19) . . ? C12 C11 C14 120.16(18) . . ? C10 C11 C14 121.22(17) . . ? C13 C12 C11 119.06(19) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? N2 C13 C12 122.51(18) . . ? N2 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? O7 C14 O8 127.28(18) . . ? O7 C14 C11 117.82(17) . . ? O8 C14 C11 114.88(17) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.552 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.071 #End of the file