#------------------------------------------------------------------------------ #$Date: 2016-03-22 22:43:47 +0000 (Tue, 22 Mar 2016) $ #$Revision: 179125 $ #$URL: svn://www.crystallography.net/cod/cif/4/30/87/4308778.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_4308778 loop_ _publ_author_name 'Zheming Wang' 'Bin Zhang' 'Mohamedally Kurmoo' 'Mark A. Green' 'Hideki Fujiwara' 'Takeo Otsuka' 'Hayao Kobayashi' _publ_section_title ; Synthesis and Characterization of a Porous Magnetic Diamond Framework, Co3(HCOO)6, and Its N2 Sorption Characteristic ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 1230 _journal_page_last 1237 _journal_paper_doi 10.1021/ic048986r _journal_volume 44 _journal_year 2005 _chemical_formula_sum 'C6 H6 Co3 O12' _chemical_formula_weight 446.90 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 127.193(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.2858(4) _cell_length_b 9.8690(4) _cell_length_c 18.1797(6) _cell_measurement_reflns_used 28990 _cell_measurement_temperature 180.0(1) _cell_measurement_theta_max 27.47 _cell_measurement_theta_min 3.49 _cell_volume 1613.00(11) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_collection 'KappaCCD (Nonius B. V., 1998)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 180.0(1) _diffrn_detector_area_resol_mean 0.76 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method CCD _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1137 _diffrn_reflns_av_sigmaI/netI 0.0718 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 28990 _diffrn_reflns_theta_full 27.47 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_min 3.49 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 3.098 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995, 1997) ; _exptl_crystal_colour 'violet red' _exptl_crystal_density_diffrn 1.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'thin plate' _exptl_crystal_F_000 876 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.455 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.110 _refine_ls_extinction_coef 0.0030(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 0.981 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 218 _refine_ls_number_reflns 3688 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.981 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0356 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.0807 _reflns_number_gt 2583 _reflns_number_total 3688 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic048986rsi20041026_094359_4.cif _cod_data_source_block 2-at-180K _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_original_cell_volume 1613.00(10) _cod_database_code 4308778 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' 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 0.37780(5) 0.07788(4) 0.13315(3) 0.01832(13) Uani 1 1 d . . . Co2 Co 0.56982(5) -0.11228(4) 0.31021(3) 0.01953(14) Uani 1 1 d . . . Co3 Co 0.5000 0.0000 0.0000 0.02065(17) Uani 1 2 d S . . Co4 Co 0.0000 0.0000 0.0000 0.02096(17) Uani 1 2 d S . . O1 O 0.4371(2) 0.19830(19) 0.24532(13) 0.0209(5) Uani 1 1 d . . . O2 O 0.5507(3) 0.0577(2) 0.36741(14) 0.0271(5) Uani 1 1 d . . . O3 O 0.5892(3) -0.0068(2) 0.21842(14) 0.0210(5) Uani 1 1 d . . . O4 O 0.6813(3) 0.0047(2) 0.13954(15) 0.0295(6) Uani 1 1 d . . . O5 O 0.4551(3) 0.25505(19) 0.10878(14) 0.0222(5) Uani 1 1 d . . . O6 O 0.4794(3) 0.2082(2) -0.00224(15) 0.0279(6) Uani 1 1 d . . . O7 O 0.3451(3) -0.0845(2) 0.19484(14) 0.0223(5) Uani 1 1 d . . . O8 O 0.1007(3) -0.1057(2) 0.12313(16) 0.0299(6) Uani 1 1 d . . . O9 O 0.3390(3) -0.0275(2) 0.02360(14) 0.0221(5) Uani 1 1 d . . . O10 O 0.1152(3) -0.1147(2) -0.03321(15) 0.0265(5) Uani 1 1 d . . . O11 O 0.1642(2) 0.1533(2) 0.06063(13) 0.0215(5) Uani 1 1 d . . . O12 O 0.2052(3) 0.3761(2) 0.09180(15) 0.0253(5) Uani 1 1 d . . . C1 C 0.4993(4) 0.1707(3) 0.3299(2) 0.0266(8) Uani 1 1 d . . . C2 C 0.6931(4) -0.0145(3) 0.2111(2) 0.0266(8) Uani 1 1 d . . . C3 C 0.4693(4) 0.2873(3) 0.0471(2) 0.0279(8) Uani 1 1 d . . . C4 C 0.2310(4) -0.1303(3) 0.1858(2) 0.0264(8) Uani 1 1 d . . . C5 C 0.2254(4) -0.1061(3) -0.0298(2) 0.0253(8) Uani 1 1 d . . . C6 C 0.1218(4) 0.2775(3) 0.0504(2) 0.0245(8) Uani 1 1 d . . . H1 H 0.511(3) 0.255(3) 0.3701(17) 0.009(7) Uiso 1 1 d . . . H2 H 0.784(4) -0.038(3) 0.264(2) 0.032(10) Uiso 1 1 d . . . H3 H 0.475(4) 0.386(3) 0.038(2) 0.024(9) Uiso 1 1 d . . . H4 H 0.256(4) -0.200(3) 0.235(2) 0.034(9) Uiso 1 1 d . . . H5 H 0.234(4) -0.156(3) -0.068(2) 0.028(9) Uiso 1 1 d . . . H6 H 0.013(4) 0.299(3) 0.005(2) 0.020(8) Uiso 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 0.0218(3) 0.0154(2) 0.0191(2) -0.00062(16) 0.0130(2) -0.00029(18) Co2 0.0240(3) 0.0151(2) 0.0205(2) 0.00152(16) 0.0139(2) 0.00124(18) Co3 0.0246(4) 0.0201(3) 0.0225(3) -0.0020(2) 0.0170(3) -0.0014(3) Co4 0.0202(4) 0.0195(3) 0.0227(3) -0.0019(2) 0.0128(3) -0.0026(3) O1 0.0284(14) 0.0153(11) 0.0178(11) -0.0014(8) 0.0134(10) -0.0021(10) O2 0.0390(16) 0.0192(12) 0.0239(12) 0.0044(9) 0.0195(12) 0.0058(11) O3 0.0217(13) 0.0208(12) 0.0234(11) 0.0018(9) 0.0152(11) 0.0022(9) O4 0.0285(15) 0.0403(14) 0.0255(13) 0.0010(10) 0.0195(12) -0.0008(11) O5 0.0317(15) 0.0173(11) 0.0241(11) -0.0007(9) 0.0203(11) -0.0019(10) O6 0.0416(16) 0.0230(12) 0.0318(13) -0.0020(10) 0.0288(13) -0.0007(11) O7 0.0247(14) 0.0190(11) 0.0239(11) 0.0002(9) 0.0150(11) -0.0008(10) O8 0.0224(14) 0.0361(14) 0.0281(12) 0.0033(10) 0.0136(12) -0.0045(11) O9 0.0239(14) 0.0208(12) 0.0236(11) -0.0053(9) 0.0154(11) -0.0035(10) O10 0.0228(14) 0.0284(13) 0.0335(13) -0.0066(10) 0.0198(12) -0.0048(10) O11 0.0236(13) 0.0166(11) 0.0254(11) -0.0023(9) 0.0153(11) -0.0018(10) O12 0.0246(14) 0.0188(11) 0.0260(12) -0.0047(9) 0.0117(11) -0.0025(10) C1 0.033(2) 0.0182(17) 0.0297(19) -0.0002(14) 0.0193(17) 0.0008(15) C2 0.022(2) 0.0253(19) 0.0277(19) 0.0008(14) 0.0129(17) 0.0001(15) C3 0.039(2) 0.0166(17) 0.0341(18) 0.0014(14) 0.0252(18) 0.0005(15) C4 0.029(2) 0.0263(19) 0.0244(18) 0.0008(14) 0.0163(17) -0.0023(16) C5 0.034(2) 0.0202(18) 0.0261(18) -0.0036(14) 0.0200(17) -0.0006(16) C6 0.023(2) 0.0244(19) 0.0242(17) 0.0004(14) 0.0133(17) 0.0009(16) 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' 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' 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 O9 Co1 O11 94.67(8) . . ? O9 Co1 O3 89.75(8) . . ? O11 Co1 O3 172.71(8) . . ? O9 Co1 O1 173.05(9) . . ? O11 Co1 O1 88.84(8) . . ? O3 Co1 O1 87.39(8) . . ? O9 Co1 O7 97.35(8) . . ? O11 Co1 O7 95.83(8) . . ? O3 Co1 O7 77.83(8) . . ? O1 Co1 O7 88.24(8) . . ? O9 Co1 O5 95.10(8) . . ? O11 Co1 O5 92.19(8) . . ? O3 Co1 O5 93.19(8) . . ? O1 Co1 O5 78.75(8) . . ? O7 Co1 O5 164.58(8) . . ? O12 Co2 O2 93.43(9) 2_645 . ? O12 Co2 O3 92.86(9) 2_645 . ? O2 Co2 O3 95.21(8) . . ? O12 Co2 O1 91.99(9) 2_645 2_645 ? O2 Co2 O1 169.97(9) . 2_645 ? O3 Co2 O1 92.94(8) . 2_645 ? O12 Co2 O5 88.63(9) 2_645 2_645 ? O2 Co2 O5 93.13(8) . 2_645 ? O3 Co2 O5 171.42(8) . 2_645 ? O1 Co2 O5 78.56(8) 2_645 2_645 ? O12 Co2 O7 170.41(8) 2_645 . ? O2 Co2 O7 88.07(8) . . ? O3 Co2 O7 77.57(8) . . ? O1 Co2 O7 87.98(8) 2_645 . ? O5 Co2 O7 100.75(9) 2_645 . ? O6 Co3 O6 180.0 3_655 . ? O6 Co3 O4 88.99(9) 3_655 . ? O6 Co3 O4 91.01(9) . . ? O6 Co3 O4 91.01(9) 3_655 3_655 ? O6 Co3 O4 88.99(9) . 3_655 ? O4 Co3 O4 180.00(12) . 3_655 ? O6 Co3 O9 88.21(8) 3_655 . ? O6 Co3 O9 91.79(8) . . ? O4 Co3 O9 95.01(8) . . ? O4 Co3 O9 84.99(8) 3_655 . ? O6 Co3 O9 91.79(8) 3_655 3_655 ? O6 Co3 O9 88.21(8) . 3_655 ? O4 Co3 O9 84.99(8) . 3_655 ? O4 Co3 O9 95.01(8) 3_655 3_655 ? O9 Co3 O9 180.00(9) . 3_655 ? O10 Co4 O10 180.00(9) 3 . ? O10 Co4 O8 89.50(9) 3 . ? O10 Co4 O8 90.50(9) . . ? O10 Co4 O8 90.50(9) 3 3 ? O10 Co4 O8 89.50(9) . 3 ? O8 Co4 O8 180.00(17) . 3 ? O10 Co4 O11 92.07(8) 3 3 ? O10 Co4 O11 87.93(8) . 3 ? O8 Co4 O11 86.48(8) . 3 ? O8 Co4 O11 93.52(8) 3 3 ? O10 Co4 O11 87.93(8) 3 . ? O10 Co4 O11 92.07(8) . . ? O8 Co4 O11 93.52(8) . . ? O8 Co4 O11 86.48(8) 3 . ? O11 Co4 O11 180.0 3 . ? C1 O1 Co1 132.31(19) . . ? C1 O1 Co2 127.04(19) . 2_655 ? Co1 O1 Co2 98.06(8) . 2_655 ? C1 O2 Co2 127.5(2) . . ? C2 O3 Co1 131.9(2) . . ? C2 O3 Co2 127.4(2) . . ? Co1 O3 Co2 99.75(9) . . ? C2 O4 Co3 132.6(2) . . ? C3 O5 Co2 127.12(19) . 2_655 ? C3 O5 Co1 133.0(2) . . ? Co2 O5 Co1 96.92(8) 2_655 . ? C3 O6 Co3 131.9(2) . . ? C4 O7 Co1 133.3(2) . . ? C4 O7 Co2 126.3(2) . . ? Co1 O7 Co2 97.78(9) . . ? C4 O8 Co4 132.1(2) . . ? C5 O9 Co1 124.5(2) . . ? C5 O9 Co3 120.3(2) . . ? Co1 O9 Co3 115.23(10) . . ? C5 O10 Co4 139.0(2) . . ? C6 O11 Co1 128.6(2) . . ? C6 O11 Co4 118.3(2) . . ? Co1 O11 Co4 113.07(9) . . ? C6 O12 Co2 131.3(2) . 2_655 ? O2 C1 O1 125.7(3) . . ? O2 C1 H1 120.0(14) . . ? O1 C1 H1 114.3(14) . . ? O4 C2 O3 125.8(4) . . ? O4 C2 H2 118(2) . . ? O3 C2 H2 116(2) . . ? O6 C3 O5 126.6(3) . . ? O6 C3 H3 117.3(18) . . ? O5 C3 H3 116.1(18) . . ? O8 C4 O7 126.9(3) . . ? O8 C4 H4 119(2) . . ? O7 C4 H4 113(2) . . ? O10 C5 O9 126.8(3) . . ? O10 C5 H5 121(2) . . ? O9 C5 H5 113(2) . . ? O12 C6 O11 125.4(3) . . ? O12 C6 H6 115.9(17) . . ? O11 C6 H6 118.8(17) . . ? 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 O9 2.046(2) . ? Co1 O11 2.064(2) . ? Co1 O3 2.078(2) . ? Co1 O1 2.0899(19) . ? Co1 O7 2.112(2) . ? Co1 O5 2.117(2) . ? Co2 O12 2.041(2) 2_645 ? Co2 O2 2.053(2) . ? Co2 O3 2.087(2) . ? Co2 O1 2.1033(19) 2_645 ? Co2 O5 2.113(2) 2_645 ? Co2 O7 2.115(2) . ? Co3 O6 2.065(2) 3_655 ? Co3 O6 2.065(2) . ? Co3 O4 2.085(2) . ? Co3 O4 2.085(2) 3_655 ? Co3 O9 2.122(2) . ? Co3 O9 2.122(2) 3_655 ? Co4 O10 2.070(2) 3 ? Co4 O10 2.070(2) . ? Co4 O8 2.077(2) . ? Co4 O8 2.077(2) 3 ? Co4 O11 2.114(2) 3 ? Co4 O11 2.114(2) . ? O1 C1 1.276(4) . ? O1 Co2 2.1033(19) 2_655 ? O2 C1 1.251(4) . ? O3 C2 1.260(4) . ? O4 C2 1.240(4) . ? O5 C3 1.265(4) . ? O5 Co2 2.113(2) 2_655 ? O6 C3 1.246(4) . ? O7 C4 1.278(4) . ? O8 C4 1.222(4) . ? O9 C5 1.297(4) . ? O10 C5 1.211(4) . ? O11 C6 1.288(4) . ? O12 C6 1.241(4) . ? O12 Co2 2.041(2) 2_655 ? C1 H1 1.06(3) . ? C2 H2 0.91(4) . ? C3 H3 0.99(3) . ? C4 H4 1.02(3) . ? C5 H5 0.91(3) . ? C6 H6 1.01(3) . ? 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 C1 H1 O3 1.06(3) 2.68(3) 3.293(4) 116.3(17) 2_655 C1 H1 O6 1.06(3) 2.58(3) 3.409(4) 134.5(19) 4_566 C1 H1 O9 1.06(3) 2.69(3) 3.663(4) 152(2) 2_655 C2 H2 O12 0.91(4) 2.70(3) 3.217(4) 117(3) 2_645 C3 H3 O2 0.99(3) 2.55(3) 3.165(4) 120(2) 2_655 C4 H4 O5 1.02(3) 2.77(4) 3.432(4) 123(2) 2_645 C5 H5 O4 0.91(3) 2.51(3) 2.937(4) 109(2) 3_655 C5 H5 O6 0.91(3) 2.71(3) 3.178(4) 113(3) 3_655 C6 H6 O8 1.01(3) 2.66(3) 3.092(4) 106(2) 3 C6 H6 O10 1.01(3) 2.56(3) 2.971(4) 104(2) 3