#------------------------------------------------------------------------------ #$Date: 2011-01-02 20:00:31 +0000 (Sun, 02 Jan 2011) $ #$Revision: 5310 $ #$URL: svn://www.crystallography.net/cod/cif/2/2204971.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_2204971 loop_ _publ_author_name 'Zhu-Yan Zhang' 'Shan Gao' 'Li-Hua Huo' 'Hui Zhao' 'Jing-Gui Zhao' _publ_section_title ; Hexaaquamanganese(II) tris[(4-oxo-4H-pyridin-1-yl)acetate] dihydrate ; _journal_issue 1 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m85 _journal_page_last m86 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Mn (H2 O1)6] (C7 H6 N O3)2, 2H2 O' _chemical_formula_moiety 'H12 Mn O6 2+, 2C7 H6 N O3 -, 2H2 O' _chemical_formula_sum 'C14 H28 Mn N2 O14' _chemical_formula_weight 503.32 _chemical_name_systematic ; Hexaaquamanganese(II) bis[(4-oxo-4H-pyridin-1-yl)acetate] dihydrate ; _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 _cell_angle_alpha 90.00 _cell_angle_beta 98.68(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 12.561(3) _cell_length_b 12.949(3) _cell_length_c 6.8550(10) _cell_measurement_reflns_used 10242 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.52 _cell_measurement_theta_min 3.00 _cell_volume 1102.2(4) _computing_cell_refinement RAPID-AUTO _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2002)' _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_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _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 0.024 _diffrn_reflns_av_sigmaI/netI 0.015 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 10259 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 3.2 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.67 _exptl_absorpt_correction_T_max 0.883 _exptl_absorpt_correction_T_min 0.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 526 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _refine_diff_density_max 0.29 _refine_diff_density_min -0.34 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 166 _refine_ls_number_reflns 2509 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.041 _refine_ls_R_factor_all 0.036 _refine_ls_R_factor_gt 0.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.3365P] where P(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.083 _refine_ls_wR_factor_ref 0.085 _reflns_number_gt 2273 _reflns_number_total 2509 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sj6038.cif _[local]_cod_cif_authors_sg_H-M 'P 21/c' _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. '_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_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2204971 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_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_type_symbol Mn1 0.0000 0.5000 0.0000 0.03130(10) Uani d S 1 Mn O1W -0.02960(10) 0.42600(10) 0.2719(2) 0.0498(3) Uani d D 1 O H1W1 -0.0906(9) 0.4004(2) 0.284(3) 0.075 Uiso d D 1 H H1W2 0.0190(10) 0.392(2) 0.345(3) 0.075 Uiso d D 1 H O2W 0.17244(9) 0.48079(9) 0.0791(2) 0.0475(3) Uani d D 1 O H2W1 0.201(2) 0.4217(9) 0.089(3) 0.071 Uiso d D 1 H H2W2 0.211(2) 0.5250(10) 0.148(3) 0.071 Uiso d D 1 H O3W 0.01204(9) 0.64785(8) 0.1499(2) 0.0407(3) Uani d D 1 O H3W1 -0.023(2) 0.6940(10) 0.077(2) 0.061 Uiso d D 1 H H3W2 -0.012(2) 0.648(2) 0.261(2) 0.061 Uiso d D 1 H O4W 0.21890(10) 0.83300(10) 0.1817(3) 0.0697(4) Uani d D 1 O H4W1 0.219(2) 0.7675(9) 0.199(4) 0.105 Uiso d D 1 H H4W2 0.223(2) 0.843(2) 0.058(2) 0.105 Uiso d D 1 H O1 -0.10557(8) 0.80018(8) -0.0420(2) 0.0389(3) Uani d . 1 O O2 -0.25982(8) 0.70991(8) -0.0938(2) 0.0412(3) Uani d . 1 O O3 -0.71104(9) 0.87990(10) -0.1775(2) 0.0498(3) Uani d . 1 O N1 -0.38310(10) 0.88615(9) -0.1402(2) 0.0354(3) Uani d . 1 N C1 -0.44640(10) 0.89550(10) -0.3168(2) 0.0417(4) Uani d . 1 C H1 -0.4143 0.9046 -0.4293 0.050 Uiso calc R 1 H C2 -0.55570(10) 0.89200(10) -0.3353(3) 0.0436(4) Uani d . 1 C H2 -0.5966 0.8983 -0.4596 0.052 Uiso calc R 1 H C3 -0.60840(10) 0.87880(10) -0.1665(2) 0.0372(3) Uani d . 1 C C4 -0.53830(10) 0.86420(10) 0.0143(2) 0.0402(3) Uani d . 1 C H4 -0.5673 0.8515 0.1291 0.048 Uiso calc R 1 H C5 -0.42980(10) 0.86830(10) 0.0227(2) 0.0397(3) Uani d . 1 C H5 -0.3862 0.8587 0.1435 0.048 Uiso calc R 1 H C6 -0.26520(10) 0.89420(10) -0.1207(3) 0.0387(3) Uani d . 1 C H6A -0.2400 0.9410 -0.0131 0.046 Uiso calc R 1 H H6B -0.2464 0.9240 -0.2408 0.046 Uiso calc R 1 H C7 -0.20680(10) 0.79110(10) -0.0822(2) 0.0315(3) Uani d . 1 C 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 0.0289(2) 0.0276(2) 0.0359(2) 0.00240(10) 0.00060(10) 0.00030(10) O1W 0.0412(6) 0.0581(8) 0.0488(7) -0.0004(5) 0.0032(5) 0.0203(6) O2W 0.0328(6) 0.0345(6) 0.0698(9) 0.0051(4) -0.0100(5) -0.0081(5) O3W 0.0458(6) 0.0338(6) 0.0420(6) 0.0051(4) 0.0051(5) -0.0029(5) O4W 0.0714(9) 0.0580(9) 0.0874(12) 0.0149(7) 0.0364(9) 0.0105(8) O1 0.0295(5) 0.0393(6) 0.0468(6) 0.0027(4) 0.0016(4) 0.0004(5) O2 0.0359(5) 0.0300(5) 0.0555(7) 0.0016(4) -0.0001(5) -0.0020(5) O3 0.0313(6) 0.0546(7) 0.0621(8) 0.0045(5) 0.0019(5) 0.0112(6) N1 0.0322(6) 0.0312(6) 0.0422(7) 0.0066(5) 0.0036(5) 0.0034(5) C1 0.0443(8) 0.0449(8) 0.0366(8) 0.0079(7) 0.0078(6) 0.0035(6) C2 0.0424(8) 0.0490(9) 0.0370(8) 0.0065(7) -0.0024(6) 0.0015(7) C3 0.0354(7) 0.0278(7) 0.0474(9) 0.0044(5) 0.0025(6) 0.0037(6) C4 0.0394(8) 0.0408(8) 0.0410(8) 0.0048(6) 0.0080(6) 0.0078(7) C5 0.0393(8) 0.0411(8) 0.0372(8) 0.0060(6) 0.0006(6) 0.0075(6) C6 0.0315(7) 0.0322(7) 0.0523(9) 0.0034(6) 0.0059(6) 0.0026(6) C7 0.0325(7) 0.0323(7) 0.0290(7) 0.0037(5) 0.0027(5) -0.0013(5) 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' 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 O2W Mn1 O1W . . 91.64(6) yes O2W Mn1 O1W . 3_565 88.36(6) yes O2W Mn1 O3W . . 89.27(5) yes O2W Mn1 O3W . 3_565 90.73(5) yes O3W Mn1 O1W . . 89.51(5) yes O3W Mn1 O1W . 3_565 90.49(5) yes N1 C6 C7 . . 113.90(10) yes O1W Mn1 O1W . 3_565 180.00(6) no O2W Mn1 O1W 3_565 . 88.36(6) no O2W Mn1 O1W 3_565 3_565 91.64(6) no O2W Mn1 O2W 3_565 . 180.00(6) no O2W Mn1 O3W 3_565 3_565 89.27(5) no O2W Mn1 O3W 3_565 . 90.73(5) no O3W Mn1 O1W 3_565 . 90.49(5) no O3W Mn1 O1W 3_565 3_565 89.51(5) no O3W Mn1 O3W 3_565 . 180.00(6) no Mn1 O1W H1W1 . . 122(2) no Mn1 O1W H1W2 . . 122(2) no Mn1 O2W H2W1 . . 122.0(10) no Mn1 O2W H2W2 . . 122(2) no Mn1 O3W H3W1 . . 110.3(9) no Mn1 O3W H3W2 . . 114(2) no H1W1 O1W H1W2 . . 109.0(10) no H2W1 O2W H2W2 . . 111.0(10) no H3W1 O3W H3W2 . . 107.0(10) no H4W1 O4W H4W2 . . 106(2) no O1 C7 C6 . . 113.40(10) no O2 C7 O1 . . 127.20(10) no O2 C7 C6 . . 119.40(10) no O3 C3 C2 . . 122.5(2) no O3 C3 C4 . . 122.6(2) no N1 C1 H1 . . 119.0 no N1 C1 C2 . . 122.0(2) no N1 C5 H5 . . 119.1 no N1 C6 H6A . . 108.8 no N1 C6 H6B . . 108.8 no C1 N1 C5 . . 118.90(10) no C1 N1 C6 . . 121.60(10) no C1 C2 H2 . . 119.5 no C1 C2 C3 . . 120.9(2) no C2 C1 H1 . . 119.0 no C3 C2 H2 . . 119.5 no C3 C4 H4 . . 119.4 no C4 C3 C2 . . 114.90(10) no C4 C5 N1 . . 121.9(2) no C4 C5 H5 . . 119.1 no C5 N1 C6 . . 119.50(10) no C5 C4 C3 . . 121.2(2) no C5 C4 H4 . . 119.4 no C7 C6 H6A . . 108.8 no C7 C6 H6B . . 108.8 no H6A C6 H6B . . 107.7 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 O1W . 2.1770(10) yes Mn1 O2W . 2.1660(10) yes Mn1 O3W . 2.1670(10) yes O1 C7 . 1.265(2) yes O2 C7 . 1.241(2) yes O3 C3 . 1.280(2) yes C1 C2 . 1.360(2) yes C4 C5 . 1.356(2) yes Mn1 O1W 3_565 2.1770(10) no Mn1 O2W 3_565 2.1660(10) no Mn1 O3W 3_565 2.1670(10) no O1W H1W1 . 0.85(2) no O1W H1W2 . 0.85(2) no O2W H2W1 . 0.84(2) no O2W H2W2 . 0.85(2) no O3W H3W1 . 0.86(2) no O3W H3W2 . 0.86(2) no O4W H4W1 . 0.86(2) no O4W H4W2 . 0.86(2) no N1 C1 . 1.350(2) no N1 C5 . 1.358(2) no N1 C6 . 1.471(2) no C1 H1 . 0.9300 no C2 C3 . 1.427(2) no C2 H2 . 0.9300 no C3 C4 . 1.421(2) no C4 H4 . 0.9300 no C5 H5 . 0.9300 no C6 C7 . 1.527(2) no C6 H6A . 0.9700 no C6 H6B . 0.9700 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 O1W H1W1 O4W 2_545 0.85(2) 1.878(11) 2.727(2) 175(2) yes O1W H1W2 O1 2_545 0.85(2) 1.99(2) 2.831(2) 167(2) yes O2W H2W1 O2 3_565 0.84(2) 1.85(2) 2.698(2) 176(2) yes O2W H2W2 O3 4_676 0.85(2) 1.89(2) 2.728(2) 174(3) yes O3W H3W1 O1 . 0.86(2) 1.84(2) 2.687(2) 171(2) yes O3W H3W2 O1 4_576 0.86(2) 2.03(2) 2.835(2) 155(2) yes O4W H4W1 O3 4_676 0.86(2) 2.22(3) 3.007(2) 154(3) yes O4W H4W2 O3 1_655 0.86(2) 1.99(3) 2.804(2) 158(3) 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 _geom_torsion_publ_flag O3 C3 C4 C5 -176.9(2) no N1 C1 C2 C3 0.4(3) no N1 C6 C7 O2 8.5(2) no N1 C6 C7 O1 -171.90(10) no C1 N1 C5 C4 -2.9(2) no C1 N1 C6 C7 -106.7(2) no C1 C2 C3 O3 176.8(2) no C1 C2 C3 C4 -3.4(2) no C2 C3 C4 C5 3.3(2) no C3 C4 C5 N1 -0.3(2) no C5 N1 C1 C2 2.9(2) no C5 N1 C6 C7 72.9(2) no C6 N1 C1 C2 -177.5(2) no C6 N1 C5 C4 177.40(10) no