#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/43/2014330.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2014330 loop_ _publ_author_name 'Michel Fleck' 'Ladislav Bohat\'y' _publ_section_title ; Compounds of glycine with metal sulfates and thiosulfates: glycine cobalt sulfate pentahydrate, glycine sodium thiosulfate dihydrate and glycine potassium thiosulfate ; _journal_coeditor_code FG3001 _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m22 _journal_page_last m26 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Co (H2 O)6] [Co (C2 H5 N O2)2 (H2 O)4] (S O4)2' _chemical_formula_moiety 'H12 Co1 O6 2+, C4 H18 Co1 N2 O8 2+, 2O4 S 2-' _chemical_formula_sum 'C4 H30 Co2 N2 O22 S2' _chemical_formula_weight 640.28 _chemical_name_common 'glycin cobalt sulphate pentahydrate' _chemical_name_systematic ; hexaaquacobalt(II) tetraaquadiglycinatocobalt(II) sulfate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 85.23(3) _cell_angle_beta 83.31(3) _cell_angle_gamma 83.22(3) _cell_formula_units_Z 1 _cell_length_a 5.9700(10) _cell_length_b 6.7750(10) _cell_length_c 13.335(3) _cell_measurement_reflns_used 2894 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.766 _cell_measurement_theta_min 4.876 _cell_volume 530.62(17) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection 'Collect (Nonius, 2003)' _computing_data_reduction 'HKL Denzo (Otwinowski & Minor 1997) and Scalepack' _computing_molecular_graphics 'DIAMOND (Version 2.1; Bergerhoff et al., 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997; Farrugia 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\w scans' _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 0.0139 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 5847 _diffrn_reflns_theta_full 30.47 _diffrn_reflns_theta_max 30.47 _diffrn_reflns_theta_min 4.17 _exptl_absorpt_coefficient_mu 1.866 _exptl_absorpt_correction_T_max 0.5710 _exptl_absorpt_correction_T_min 0.4788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Otwinowski & Minor, 1997)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.004 _exptl_crystal_density_method 'not measured' _exptl_crystal_description fragment _exptl_crystal_F_000 330 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _refine_diff_density_max 0.458 _refine_diff_density_min -0.431 _refine_ls_extinction_coef 0.076(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 209 _refine_ls_number_reflns 3191 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0202 _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^)+(0.0202P)^2^+0.2124P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0511 _refine_ls_wR_factor_ref 0.0519 _reflns_number_gt 3036 _reflns_number_total 3191 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file fg3001.cif _[local]_cod_data_source_block I _cod_database_code 2014330 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Co1 0.5000 0.0000 0.0000 0.01566(6) Uani d S 1 . . Co O1W 0.54763(15) 0.23385(14) 0.08030(9) 0.0351(2) Uani d . 1 . . O H1W1 0.4630 0.3239 0.0902 0.042 Uiso d R 1 . . H H2W1 0.6680 0.2499 0.0923 0.042 Uiso d R 1 . . H O2W 0.20748(14) 0.15817(13) -0.05029(7) 0.02450(17) Uani d . 1 . . O H1W2 0.2180 0.2500 -0.0908 0.029 Uiso d R 1 . . H H2W2 0.1190 0.1960 -0.0007 0.029 Uiso d R 1 . . H O3W 0.29385(15) -0.10454(13) 0.13058(7) 0.02451(17) Uani d . 1 . . O H1W3 0.2561 -0.2200 0.1317 0.029 Uiso d R 1 . . H H2W3 0.1791 -0.0280 0.1437 0.029 Uiso d R 1 . . H Co2 0.5000 0.5000 0.5000 0.01567(6) Uani d S 1 . . Co O1 0.97249(16) 0.82634(18) 0.38482(9) 0.0405(3) Uani d . 1 . . O O2 0.64348(15) 0.77729(13) 0.47608(6) 0.02304(17) Uani d . 1 . . O O4W 0.19176(14) 0.65457(15) 0.53687(7) 0.02818(19) Uani d . 1 . . O H1W4 0.1141 0.6960 0.4921 0.034 Uiso d R 1 . . H H2W4 0.1071 0.6390 0.5888 0.034 Uiso d R 1 . . H O5W 0.43859(14) 0.53851(14) 0.34563(6) 0.02478(18) Uani d . 1 . . O H1W5 0.5420 0.5300 0.3010 0.030 Uiso d R 1 . . H H2W5 0.3350 0.4940 0.3282 0.030 Uiso d R 1 . . H N1 0.39389(18) 0.99860(17) 0.34518(8) 0.0264(2) Uani d . 1 . . N H1N 0.3660 1.0420 0.4093 0.032 Uiso d R 1 . . H H2N 0.3390 0.8900 0.3421 0.032 Uiso d R 1 . . H H3N 0.3250 1.0830 0.3057 0.032 Uiso d R 1 . . H C1 0.76362(19) 0.84857(17) 0.39963(9) 0.0206(2) Uani d . 1 . . C C2 0.6424(2) 0.97830(19) 0.31948(9) 0.0244(2) Uani d . 1 . . C H1C 0.6950 1.1093 0.3129 0.029 Uiso calc R 1 . . H H2C 0.6799 0.9200 0.2548 0.029 Uiso calc R 1 . . H S1 0.01339(4) 0.41135(4) 0.187221(19) 0.01505(6) Uani d . 1 . . S O1S 0.09684(15) 0.34647(14) 0.28635(7) 0.02613(18) Uani d . 1 . . O O2S 0.18447(15) 0.51719(13) 0.12291(7) 0.02591(18) Uani d . 1 . . O O3S -0.02773(14) 0.23353(13) 0.13789(7) 0.02426(17) Uani d . 1 . . O O4S -0.20125(14) 0.54266(13) 0.20217(7) 0.02488(18) Uani d . 1 . . O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.01402(9) 0.01463(10) 0.01847(10) -0.00038(7) -0.00293(7) -0.00207(7) O1W 0.0186(4) 0.0282(5) 0.0628(7) 0.0016(3) -0.0108(4) -0.0249(5) O2W 0.0217(4) 0.0266(4) 0.0226(4) 0.0065(3) -0.0023(3) 0.0010(3) O3W 0.0236(4) 0.0209(4) 0.0279(4) -0.0032(3) 0.0012(3) -0.0002(3) Co2 0.01228(9) 0.01925(10) 0.01489(10) -0.00075(7) -0.00090(7) 0.00010(7) O1 0.0175(4) 0.0558(7) 0.0442(6) -0.0010(4) -0.0030(4) 0.0159(5) O2 0.0257(4) 0.0229(4) 0.0206(4) -0.0060(3) -0.0016(3) 0.0017(3) O4W 0.0168(4) 0.0392(5) 0.0248(4) 0.0060(3) 0.0014(3) 0.0016(4) O5W 0.0186(4) 0.0398(5) 0.0170(4) -0.0077(3) -0.0014(3) -0.0027(3) N1 0.0225(5) 0.0293(5) 0.0268(5) 0.0026(4) -0.0076(4) 0.0012(4) C1 0.0195(5) 0.0202(5) 0.0222(5) -0.0029(4) -0.0034(4) 0.0006(4) C2 0.0222(5) 0.0272(6) 0.0229(5) -0.0029(4) -0.0030(4) 0.0044(4) S1 0.01277(11) 0.01520(11) 0.01667(12) -0.00067(8) -0.00031(8) -0.00108(9) O1S 0.0259(4) 0.0316(5) 0.0207(4) 0.0007(3) -0.0070(3) 0.0001(3) O2S 0.0213(4) 0.0195(4) 0.0343(5) -0.0044(3) 0.0083(3) 0.0004(3) O3S 0.0220(4) 0.0224(4) 0.0300(4) -0.0045(3) -0.0024(3) -0.0089(3) O4S 0.0183(4) 0.0264(4) 0.0260(4) 0.0066(3) 0.0036(3) 0.0005(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 O1W . 2.0487(10) ? Co1 O1W 2_655 2.0487(10) ? Co1 O2W 2_655 2.0879(10) ? Co1 O2W . 2.0879(10) ? Co1 O3W . 2.1330(11) ? Co1 O3W 2_655 2.1330(11) ? O1W H1W1 . 0.7552 ? O1W H2W1 . 0.7762 ? O2W H1W2 . 0.7925 ? O2W H2W2 . 0.8350 ? O3W H1W3 . 0.8377 ? O3W H2W3 . 0.8199 ? Co2 O4W 2_666 2.0358(11) ? Co2 O4W . 2.0358(11) ? Co2 O5W . 2.1222(10) ? Co2 O5W 2_666 2.1222(10) ? Co2 O2 2_666 2.1404(10) ? Co2 O2 . 2.1404(10) ? O1 C1 . 1.2328(15) ? O2 C1 . 1.2714(14) ? O4W H1W4 . 0.8103 ? O4W H2W4 . 0.8155 ? O5W H1W5 . 0.8064 ? O5W H2W5 . 0.7851 ? N1 C2 . 1.4758(16) ? N1 H1N . 0.9178 ? N1 H2N . 0.8460 ? N1 H3N . 0.8474 ? C1 C2 . 1.5207(17) ? C2 H1C . 0.9700 ? C2 H2C . 0.9700 ? S1 O2S . 1.4695(10) ? S1 O4S . 1.4744(10) ? S1 O3S . 1.4776(9) ? S1 O1S . 1.4812(10) ? 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' S S 0.1246 0.1234 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O1W Co1 O1W . 2_655 180.00(5) O1W Co1 O2W . 2_655 89.46(4) O1W Co1 O2W 2_655 2_655 90.54(4) O1W Co1 O2W . . 90.54(4) O1W Co1 O2W 2_655 . 89.46(4) O2W Co1 O2W 2_655 . 180.00(6) O1W Co1 O3W . . 87.26(5) O1W Co1 O3W 2_655 . 92.74(5) O2W Co1 O3W 2_655 . 91.92(4) O2W Co1 O3W . . 88.08(4) O1W Co1 O3W . 2_655 92.74(5) O1W Co1 O3W 2_655 2_655 87.26(5) O2W Co1 O3W 2_655 2_655 88.08(4) O2W Co1 O3W . 2_655 91.92(4) O3W Co1 O3W . 2_655 180.00(3) Co1 O1W H1W1 . . 125.8 Co1 O1W H2W1 . . 120.7 H1W1 O1W H2W1 . . 111.9 Co1 O2W H1W2 . . 119.8 Co1 O2W H2W2 . . 109.6 H1W2 O2W H2W2 . . 108.2 Co1 O3W H1W3 . . 117.6 Co1 O3W H2W3 . . 112.3 H1W3 O3W H2W3 . . 108.3 O4W Co2 O4W 2_666 . 180.0000(10) O4W Co2 O5W 2_666 . 91.13(5) O4W Co2 O5W . . 88.87(5) O4W Co2 O5W 2_666 2_666 88.87(5) O4W Co2 O5W . 2_666 91.13(5) O5W Co2 O5W . 2_666 180.0 O4W Co2 O2 2_666 2_666 88.70(4) O4W Co2 O2 . 2_666 91.30(4) O5W Co2 O2 . 2_666 93.25(4) O5W Co2 O2 2_666 2_666 86.75(4) O4W Co2 O2 2_666 . 91.30(4) O4W Co2 O2 . . 88.70(4) O5W Co2 O2 . . 86.75(4) O5W Co2 O2 2_666 . 93.25(4) O2 Co2 O2 2_666 . 180.0 C1 O2 Co2 . . 130.14(8) Co2 O4W H1W4 . . 118.9 Co2 O4W H2W4 . . 127.0 H1W4 O4W H2W4 . . 107.6 Co2 O5W H1W5 . . 120.9 Co2 O5W H2W5 . . 119.7 H1W5 O5W H2W5 . . 108.6 C2 N1 H1N . . 106.7 C2 N1 H2N . . 112.0 H1N N1 H2N . . 111.1 C2 N1 H3N . . 112.9 H1N N1 H3N . . 108.1 H2N N1 H3N . . 106.1 O1 C1 O2 . . 126.01(11) O1 C1 C2 . . 115.98(11) O2 C1 C2 . . 117.98(10) N1 C2 C1 . . 111.74(10) N1 C2 H1C . . 109.3 C1 C2 H1C . . 109.3 N1 C2 H2C . . 109.3 C1 C2 H2C . . 109.3 H1C C2 H2C . . 107.9 O2S S1 O4S . . 110.05(6) O2S S1 O3S . . 109.46(6) O4S S1 O3S . . 108.97(6) O2S S1 O1S . . 109.69(6) O4S S1 O1S . . 109.87(6) O3S S1 O1S . . 108.79(6) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1W H1W1 O2S . 0.76 2.02 2.7605(16) 166.6 O1W H2W1 O3S 1_655 0.78 1.97 2.7329(14) 167.7 O2W H1W2 O4S 2_565 0.79 1.96 2.7438(15) 169.6 O2W H2W2 O3S . 0.84 1.97 2.7843(15) 163.5 O3W H1W3 O2S 1_545 0.84 1.90 2.7311(13) 175.0 O3W H2W3 O3S . 0.82 2.04 2.8101(15) 156.8 O4W H1W4 O1 1_455 0.81 1.85 2.6543(16) 169.5 O4W H2W4 O1S 2_566 0.82 1.95 2.7531(16) 169.7 O5W H1W5 O4S 1_655 0.81 1.91 2.7075(15) 172.0 O5W H2W5 O1S . 0.79 1.99 2.7666(14) 172.4 N1 H1N O2 2_676 0.92 2.03 2.9042(16) 159.1 N1 H2N O1 1_455 0.85 2.28 2.8725(17) 127.5 N1 H2N O5W . 0.85 2.38 3.0966(15) 142.4 N1 H3N O1S 1_565 0.85 2.13 2.8887(16) 148.8