#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/21/2202189.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_2202189 loop_ _publ_author_name 'Deng, Yuan-Fu' 'Zhou, Zhao-Hui' 'Wan, Hui-Lin' 'Ng, Seik Weng' _publ_section_title ; \D-Aqua-S-citrato(2--)manganese(II) ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m310 _journal_page_last m312 _journal_paper_doi 10.1107/S1600536803009383 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Mn (C6 H6 O7) (H2 O)]' _chemical_formula_moiety '(C6 H6 O7), (H2 O), Mn' _chemical_formula_sum 'C6 H8 Mn O8' _chemical_formula_weight 263.06 _chemical_name_systematic ; \D-Aqua-S-citrato(2-)manganese(II) ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.0300(10) _cell_length_b 10.4670(10) _cell_length_c 13.5680(10) _cell_measurement_reflns_used 2130 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 28.2 _cell_measurement_theta_min 2.5 _cell_volume 856.36(18) _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_collection 'SMART (Bruker, 1998)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.95 _diffrn_measured_fraction_theta_max 0.95 _diffrn_measurement_device_type 'Bruker APEX area-detector' _diffrn_measurement_method '\f and \w' _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 0.037 _diffrn_reflns_av_sigmaI/netI 0.047 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5277 _diffrn_reflns_theta_full 28.2 _diffrn_reflns_theta_max 28.2 _diffrn_reflns_theta_min 2.5 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.567 _exptl_absorpt_correction_T_max 0.889 _exptl_absorpt_correction_T_min 0.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 2.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 532 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.50 _refine_diff_density_min -0.46 _refine_ls_abs_structure_details 'ad (Flack & Schwarzenbach, 1988)' _refine_ls_abs_structure_Flack 0.05(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.21 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 160 _refine_ls_number_reflns 1936 _refine_ls_number_restraints 11 _refine_ls_restrained_S_all 1.20 _refine_ls_R_factor_gt 0.048 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0243P)^2^+1.1167P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.094 _refine_ls_wR_factor_ref 0.094 _reflns_number_gt 1914 _reflns_number_total 1936 _reflns_threshold_expression I>2\s(I) _cod_data_source_file tk6102.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' 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 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 856.4(2) _cod_database_code 2202189 _cod_database_fobs_code 2202189 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -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 Mn1 0.59460(10) 0.33199(5) 0.44853(4) 0.0132(2) Uani d . 1 . . Mn O1 0.4604(5) 0.4990(3) 0.3799(2) 0.0156(6) Uani d D 1 . . O O2 0.2213(5) 0.3352(3) 0.4800(2) 0.0176(6) Uani d . 1 . . O O3 -0.0829(6) 0.3704(3) 0.3897(2) 0.0236(7) Uani d . 1 . . O O4 0.4665(5) 0.2358(3) 0.3166(2) 0.0182(7) Uani d . 1 . . O O5 0.3837(6) 0.2248(2) 0.1576(2) 0.0210(7) Uani d . 1 . . O O6 0.1039(8) 0.6292(3) 0.4979(2) 0.0329(8) Uani d D 1 . . O O7 0.1345(6) 0.8052(3) 0.4082(3) 0.0310(9) Uani d . 1 . . O O1w 0.6686(6) 0.4344(3) 0.5833(2) 0.0297(8) Uani d D 1 . . O C1 0.2454(7) 0.4781(3) 0.3398(3) 0.0122(8) Uani d . 1 . . C C2 0.1170(8) 0.3889(3) 0.4098(3) 0.0134(8) Uani d . 1 . . C C3 0.2694(8) 0.4114(4) 0.2395(3) 0.0168(9) Uani d D 1 . . C C4 0.3823(7) 0.2829(3) 0.2382(3) 0.0147(8) Uani d . 1 . . C C5 0.1214(8) 0.6039(4) 0.3255(3) 0.0147(8) Uani d D 1 . . C C6 0.1219(8) 0.6909(3) 0.4142(3) 0.0183(9) Uani d . 1 . . C H1o 0.511(7) 0.572(2) 0.366(3) 0.019 Uiso d D 1 . . H H6o 0.118(9) 0.678(4) 0.547(2) 0.039 Uiso d D 1 . . H H1w1 0.668(7) 0.5150(10) 0.590(4) 0.036 Uiso d D 1 . . H H1w2 0.789(5) 0.403(4) 0.605(4) 0.036 Uiso d D 1 . . H H3a 0.142(3) 0.397(4) 0.215(3) 0.020 Uiso d D 1 . . H H3b 0.346(5) 0.457(4) 0.200(2) 0.020 Uiso d D 1 . . H H5a -0.017(2) 0.595(4) 0.316(3) 0.018 Uiso d D 1 . . H H5b 0.179(5) 0.646(4) 0.278(2) 0.018 Uiso d D 1 . . H 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 Mn1 0.0111(3) 0.0133(2) 0.0153(3) 0.0006(3) -0.0022(3) 0.0035(2) O1 0.008(2) 0.0130(10) 0.026(2) -0.0020(10) -0.00460(10) 0.0070(10) O2 0.019(2) 0.0210(10) 0.0130(10) 0.0010(10) 0.0010(10) 0.0060(10) O3 0.013(2) 0.030(2) 0.028(2) -0.0050(10) -0.001(2) 0.0050(10) O4 0.023(2) 0.0150(10) 0.0170(10) 0.0040(10) -0.0050(10) 0.0010(10) O5 0.029(2) 0.0180(10) 0.0170(10) 0.0100(10) -0.002(2) -0.0040(10) O6 0.061(2) 0.0210(10) 0.017(2) 0.003(2) 0.004(2) -0.0050(10) O7 0.042(3) 0.0140(10) 0.037(2) 0.0000(10) -0.007(2) -0.0030(10) O1w 0.040(2) 0.0180(10) 0.031(2) 0.0060(10) -0.010(2) -0.0040(10) C1 0.009(2) 0.011(2) 0.017(2) -0.001(2) 0.000(2) 0.0000(10) C2 0.017(2) 0.0090(10) 0.014(2) 0.002(2) 0.005(2) -0.0010(10) C3 0.017(2) 0.017(2) 0.017(2) 0.002(2) 0.000(2) 0.001(2) C4 0.012(2) 0.016(2) 0.016(2) -0.004(2) 0.007(2) -0.002(2) C5 0.013(2) 0.016(2) 0.015(2) 0.002(2) 0.001(2) -0.0010(10) C6 0.012(2) 0.018(2) 0.025(2) 0.002(2) -0.001(2) -0.004(2) 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' Mn Mn 0.3368 0.7283 '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 _geom_angle_publ_flag O1 Mn1 O2 . . 72.40(10) yes O1 Mn1 O2 . 4_556 178.40(10) yes O1 Mn1 O3 . 1_655 91.60(10) yes O1 Mn1 O4 . . 83.50(10) yes O1 Mn1 O1w . . 92.40(10) yes O2 Mn1 O2 4_556 . 106.15(9) yes O2 Mn1 O1w 4_556 . 87.10(10) yes O2 Mn1 O4 4_556 . 96.90(10) yes O3 Mn1 O2 1_655 . 163.60(10) yes O3 Mn1 O2 1_655 4_556 89.90(10) yes O3 Mn1 O4 1_655 . 95.90(10) yes O3 Mn1 O1w 1_655 . 92.00(10) yes O4 Mn1 O2 . . 79.20(10) yes O1w Mn1 O2 . . 92.20(10) yes O1w Mn1 O4 . . 171.20(10) yes C1 O1 Mn1 . . 112.7(2) no C2 O2 Mn1 . 4_456 121.6(3) no C2 O2 Mn1 . . 110.7(3) no Mn1 O2 Mn1 4_456 . 115.00(10) no C2 O3 Mn1 . 1_455 145.5(3) no C4 O4 Mn1 . . 129.9(2) no O1 C1 C5 . . 111.3(3) no O1 C1 C3 . . 108.8(3) no C5 C1 C3 . . 109.0(3) no O1 C1 C2 . . 108.3(3) no C5 C1 C2 . . 110.8(3) no C3 C1 C2 . . 108.5(3) no O3 C2 O2 . . 124.8(4) no O3 C2 C1 . . 116.4(3) no O2 C2 C1 . . 118.8(4) no C4 C3 C1 . . 117.3(3) no O5 C4 O4 . . 122.5(4) no O5 C4 C3 . . 116.6(4) no O4 C4 C3 . . 120.9(3) no C6 C5 C1 . . 114.7(3) no O7 C6 O6 . . 123.6(4) no O7 C6 C5 . . 123.2(4) no O6 C6 C5 . . 113.2(3) no 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 Mn1 O1 . 2.139(3) yes Mn1 O2 . 2.292(3) yes Mn1 O2 4_556 2.142(3) yes Mn1 O3 1_655 2.140(4) yes Mn1 O4 . 2.195(3) yes Mn1 O1w . 2.166(3) yes O1 C1 . 1.423(5) no O2 C2 . 1.272(5) no O3 C2 . 1.251(6) no O4 C4 . 1.278(5) no O5 C4 . 1.251(4) no O6 C6 . 1.311(5) no O7 C6 . 1.201(5) no C1 C2 . 1.540(5) no C1 C3 . 1.536(5) no C1 C5 . 1.526(5) no C3 C4 . 1.508(6) no C5 C6 . 1.509(5) no O1 H1o . 0.850(10) no O6 H6o . 0.850(10) no O1w H1w1 . 0.850(10) no O1w H1w2 . 0.850(10) no C3 H3a . 0.850(10) no C3 H3b . 0.850(10) no C5 H5a . 0.850(10) no C5 H5b . 0.850(10) no 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 _geom_hbond_publ_flag O1 H1o O5 3_655 0.85 1.75 2.594(4) 178 yes O6 H6o O5 2_565 0.85 1.81 2.652(4) 173 yes O1w H1w2 O4 4_556 0.85 2.10 2.871(4) 152 yes O1w H1w1 O7 4_566 0.85 1.90 2.737(4) 172 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O3 Mn1 O1 C1 1_655 . 139.7(2) no O2 Mn1 O1 C1 4_556 . -60(4) no O1w Mn1 O1 C1 . . -128.3(3) no O4 Mn1 O1 C1 . . 44.0(2) no O2 Mn1 O1 C1 . . -36.7(2) no O1 Mn1 O2 C2 . . 30.7(2) no O3 Mn1 O2 C2 1_655 . 17.9(5) no O2 Mn1 O2 C2 4_556 . -150.0(3) no O1w Mn1 O2 C2 . . 122.5(2) no O4 Mn1 O2 C2 . . -55.9(2) no O1 Mn1 O2 Mn1 . 4_456 173.17(16) no O3 Mn1 O2 Mn1 1_655 4_456 160.4(3) no O2 Mn1 O2 Mn1 4_556 4_456 -7.48(7) no O1w Mn1 O2 Mn1 . 4_456 -95.05(14) no O4 Mn1 O2 Mn1 . 4_456 86.63(13) no O1 Mn1 O4 C4 . . 7.5(4) no O3 Mn1 O4 C4 1_655 . -83.5(4) no O2 Mn1 O4 C4 4_556 . -174.1(4) no O1w Mn1 O4 C4 . . 69.7(9) no O2 Mn1 O4 C4 . . 80.7(4) no Mn1 O1 C1 C5 . . 159.5(3) no Mn1 O1 C1 C3 . . -80.3(3) no Mn1 O1 C1 C2 . . 37.5(3) no Mn1 O3 C2 O2 1_455 . 34.7(7) no Mn1 O3 C2 C1 1_455 . -148.8(3) no Mn1 O2 C2 O3 4_456 . 16.5(5) no Mn1 O2 C2 O3 . . 156.1(3) no Mn1 O2 C2 C1 4_456 . -160.0(2) no Mn1 O2 C2 C1 . . -20.4(4) no O1 C1 C2 O3 . . 173.7(3) no C5 C1 C2 O3 . . 51.4(4) no C3 C1 C2 O3 . . -68.3(4) no O1 C1 C2 O2 . . -9.6(4) no C5 C1 C2 O2 . . -131.9(4) no C3 C1 C2 O2 . . 108.4(4) no O1 C1 C3 C4 . . 60.2(5) no C5 C1 C3 C4 . . -178.3(4) no C2 C1 C3 C4 . . -57.5(5) no Mn1 O4 C4 O5 . . 155.5(3) no Mn1 O4 C4 C3 . . -26.2(6) no C1 C3 C4 O5 . . 174.1(4) no C1 C3 C4 O4 . . -4.3(6) no O1 C1 C5 C6 . . -49.4(5) no C3 C1 C5 C6 . . -169.4(4) no C2 C1 C5 C6 . . 71.2(4) no C1 C5 C6 O7 . . 143.1(5) no C1 C5 C6 O6 . . -37.9(6) no