#------------------------------------------------------------------------------ #$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $ #$Revision: 176729 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/51/27/1512757.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1512757 loop_ _publ_author_name 'Maxim P. Yutkin' 'Marina S. Zavakhina' 'Denis G. Samsonenko' 'Danil N. Dybtsev' 'Vladimir P. Fedin' _publ_section_title ; Synthesis and characterization of expected and unexpected topologies of homochiral porous metal(II) malate frameworks ; _journal_name_full ; Inorganica Chimica Acta ; _journal_page_first 367 _journal_page_last 372 _journal_paper_doi 10.1016/j.ica.2012.08.012 _journal_volume 394 _journal_year 2013 _chemical_formula_structural '(Co2 (C10 H8 N2) (C4 H4 O5)2) . 2(H2 O)' _chemical_formula_sum 'C18 H20 Co2 N2 O12' _chemical_formula_weight 574.22 _space_group_IT_number 18 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2 2ab' _symmetry_space_group_name_H-M 'P 21 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 22.334(1) _cell_length_b 6.746(1) _cell_length_c 7.597(1) _cell_measurement_reflns_used 3250 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 32.0 _cell_measurement_theta_min 3.2 _cell_volume 1144.6(2) _computing_cell_refinement 'DENZO (Z. Otwinowski & W. Minor, 1997)' _computing_data_collection 'ADSC Quantum software' _computing_data_reduction 'HKL2000 (Z. Otwinowski & W. Minor, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker-AXS, 2004)' _computing_publication_material 'CIFTAB-97 (Sheldrick, 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1998)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 19.5 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measurement_device_type 'ADSC Quantum 210' _diffrn_measurement_method '\f scans' _diffrn_radiation_monochromator 'Double Crystal Monochromator' _diffrn_radiation_probe x-ray _diffrn_radiation_source synchrotron _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.85000 _diffrn_reflns_av_R_equivalents 0.0796 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 7050 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 32.08 _diffrn_reflns_theta_min 3.21 _diffrn_source synchrotron _diffrn_source_type 'PAL 4A MXW Beamline' _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.454 _exptl_absorpt_correction_T_max 0.9526 _exptl_absorpt_correction_T_min 0.8871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SCALEPACK (Z. Otwinowski & W. Minor, 1997)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 584 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.961 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.174 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(2) _refine_ls_extinction_coef 0.044(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 161 _refine_ls_number_reflns 2288 _refine_ls_number_restraints 36 _refine_ls_restrained_S_all 1.109 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0492 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+1.5595P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1389 _refine_ls_wR_factor_ref 0.1413 _reflns_number_gt 2162 _reflns_number_total 2288 _reflns_threshold_expression >2\s(I) _cod_data_source_file ICA-2013-394-367-372-1.cif _cod_data_source_block compound1 _cod_database_code 1512757 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' 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 Co1 Co 0.71090(2) -1.46466(8) 0.75151(7) 0.0148(3) Uani 1 1 d . O1 O 0.75403(13) -1.2533(5) 0.5998(4) 0.0216(7) Uani 1 1 d . O2 O 0.82852(13) -1.1078(5) 0.4554(4) 0.0218(7) Uani 1 1 d . C1 C 0.80861(19) -1.2141(7) 0.5773(6) 0.0187(9) Uani 1 1 d . C2 C 0.85638(19) -1.2943(8) 0.7018(6) 0.0207(10) Uani 1 1 d . H2A H 0.8852 -1.3725 0.6313 0.025 Uiso 1 1 calc R H2B H 0.8785 -1.1800 0.7513 0.025 Uiso 1 1 calc R C3 C 0.83552(19) -1.4223(6) 0.8537(5) 0.0179(9) Uani 1 1 d . H3 H 0.8714 -1.4770 0.9157 0.022 Uiso 1 1 calc R O3 O 0.80121(13) -1.5842(5) 0.7831(4) 0.0180(6) Uani 1 1 d . H3A H 0.8148 -1.7142 0.7562 0.022 Uiso 1 1 calc R C4 C 0.79878(19) -1.3004(7) 0.9846(5) 0.0171(9) Uani 1 1 d . O4 O 0.74233(14) -1.3245(5) 0.9815(4) 0.0201(7) Uani 1 1 d . O5 O 0.82626(13) -1.1824(5) 1.0816(4) 0.0202(7) Uani 1 1 d . N1 N 0.63252(16) -1.2870(6) 0.7750(5) 0.0203(8) Uani 1 1 d U C5 C 0.6314(2) -1.0991(8) 0.7141(7) 0.0266(10) Uani 1 1 d U H5 H 0.6668 -1.0457 0.6637 0.032 Uiso 1 1 calc R C6 C 0.5805(2) -0.9803(7) 0.7222(7) 0.0264(10) Uani 1 1 d U H6 H 0.5818 -0.8474 0.6810 0.032 Uiso 1 1 calc R C7 C 0.5278(2) -1.0585(7) 0.7912(6) 0.0232(10) Uani 1 1 d U C8 C 0.5304(3) -1.2469(9) 0.8591(10) 0.0469(16) Uani 1 1 d U H8 H 0.4956 -1.3048 0.9093 0.056 Uiso 1 1 calc R C9 C 0.5835(3) -1.3532(9) 0.8547(11) 0.0499(16) Uani 1 1 d U H9 H 0.5849 -1.4788 0.9111 0.060 Uiso 1 1 calc R O1W O 1.0000 -2.0000 0.7817(12) 0.059(2) Uani 0.80 2 d SP O2W O 0.8979(3) -1.8214(11) 0.6416(9) 0.0453(17) Uani 0.60 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 0.0182(3) 0.0124(4) 0.0138(3) -0.0006(3) -0.0003(2) 0.00024(18) O1 0.0200(15) 0.0188(18) 0.0260(17) 0.0025(13) 0.0002(13) 0.0021(13) O2 0.0222(15) 0.0245(17) 0.0187(14) 0.0061(13) 0.0022(12) -0.0004(15) C1 0.025(2) 0.013(2) 0.018(2) 0.0015(18) 0.0013(16) -0.0003(17) C2 0.0211(19) 0.022(2) 0.019(2) 0.0003(17) 0.0032(15) -0.0020(18) C3 0.022(2) 0.014(2) 0.0181(19) -0.0023(17) -0.0022(16) -0.0011(18) O3 0.0252(14) 0.0079(14) 0.0209(14) -0.0023(12) 0.0004(12) -0.0016(12) C4 0.023(2) 0.010(2) 0.0182(19) 0.0071(16) 0.0011(16) 0.0008(17) O4 0.0204(15) 0.0197(18) 0.0202(15) -0.0040(13) -0.0006(12) -0.0003(14) O5 0.0240(15) 0.0158(16) 0.0208(15) -0.0020(13) -0.0025(12) -0.0011(14) N1 0.0229(16) 0.0194(19) 0.0186(18) -0.0007(15) 0.0001(14) 0.0010(14) C5 0.027(2) 0.019(2) 0.034(2) 0.0048(18) 0.0028(19) 0.0019(19) C6 0.030(2) 0.017(2) 0.032(2) 0.0043(19) -0.0016(19) 0.0040(18) C7 0.025(2) 0.021(2) 0.024(2) 0.0002(17) -0.0014(17) 0.0068(19) C8 0.032(3) 0.030(3) 0.079(4) 0.026(3) 0.023(3) 0.006(2) C9 0.036(3) 0.028(3) 0.086(4) 0.026(3) 0.020(3) 0.011(2) O1W 0.060(5) 0.077(7) 0.039(4) 0.000 0.000 0.019(5) O2W 0.070(4) 0.030(4) 0.036(3) -0.005(3) -0.006(3) 0.002(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C -0.0020 0.0024 '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 -0.0031 0.0049 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O -0.0042 0.0090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.1291 1.3427 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 Co1 O3 83.44(12) . . yes O1 Co1 O4 89.85(13) . . yes O1 Co1 O5 175.14(12) . 4_647 yes O1 Co1 N1 92.38(13) . . yes O2 Co1 O1 95.60(13) 4_646 . yes O2 Co1 O3 107.93(12) 4_646 . yes O2 Co1 O4 173.29(12) 4_646 . yes O2 Co1 O5 87.92(13) 4_646 4_647 yes O2 Co1 N1 88.63(13) 4_646 . yes O4 Co1 O3 76.53(12) . . yes O4 Co1 O5 86.87(13) . 4_647 yes O4 Co1 N1 87.24(13) . . yes O5 Co1 O3 92.30(11) 4_647 . yes O5 Co1 N1 91.04(13) 4_647 . yes N1 Co1 O3 163.21(13) . . yes C1 O1 Co1 132.1(3) . . ? C1 O2 Co1 133.3(3) . 4_656 ? O1 C1 C2 121.3(4) . . ? O2 C1 O1 124.3(4) . . ? O2 C1 C2 114.4(4) . . ? C1 C2 H2A 108.0 . . ? C1 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? C3 C2 C1 117.4(4) . . ? C3 C2 H2A 108.0 . . ? C3 C2 H2B 108.0 . . ? C2 C3 H3 108.8 . . ? C2 C3 C4 110.7(4) . . ? O3 C3 C2 108.2(3) . . ? O3 C3 H3 108.8 . . ? O3 C3 C4 111.4(3) . . ? C4 C3 H3 108.8 . . ? Co1 O3 H3A 127.7 . . ? C3 O3 Co1 104.6(2) . . ? C3 O3 H3A 127.7 . . ? O4 C4 C3 116.8(4) . . ? O5 C4 C3 117.6(4) . . ? O5 C4 O4 125.5(4) . . ? C4 O4 Co1 113.8(3) . . ? C4 O5 Co1 127.3(3) . 4_657 ? C5 N1 Co1 121.0(3) . . ? C9 N1 Co1 121.8(4) . . ? C9 N1 C5 117.2(4) . . ? N1 C5 H5 118.6 . . ? N1 C5 C6 122.8(4) . . ? C6 C5 H5 118.6 . . ? C5 C6 H6 120.4 . . ? C5 C6 C7 119.2(4) . . ? C7 C6 H6 120.4 . . ? C6 C7 C7 120.7(5) . 2_635 ? C8 C7 C6 117.2(5) . . ? C8 C7 C7 122.1(6) . 2_635 ? C7 C8 H8 119.8 . . ? C7 C8 C9 120.3(5) . . ? C9 C8 H8 119.8 . . ? N1 C9 C8 122.8(5) . . ? N1 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? 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 O1 2.071(3) . yes Co1 O2 2.044(3) 4_646 yes Co1 O3 2.185(3) . yes Co1 O4 2.107(3) . yes Co1 O5 2.110(3) 4_647 yes Co1 N1 2.129(4) . yes O1 C1 1.259(5) . ? O2 Co1 2.044(3) 4_656 ? O2 C1 1.253(6) . ? C1 C2 1.525(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.515(6) . ? C3 H3 1.0000 . ? C3 O3 1.438(5) . ? C3 C4 1.529(6) . ? O3 H3A 0.9500 . ? C4 O4 1.271(5) . ? C4 O5 1.247(6) . ? O5 Co1 2.110(3) 4_657 ? N1 C5 1.350(7) . ? N1 C9 1.328(7) . ? C5 H5 0.9500 . ? C5 C6 1.391(7) . ? C6 H6 0.9500 . ? C6 C7 1.393(7) . ? C7 C7 1.473(9) 2_635 ? C7 C8 1.373(8) . ? C8 H8 0.9500 . ? C8 C9 1.387(8) . ? C9 H9 0.9500 . ?