#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/49/2204928.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_2204928 loop_ _publ_author_name 'Gao, Shan' 'Liu, Ji-Wei' 'Huo, Li-Hua' 'Zhao, Hui' _publ_section_title ; Poly[aquamanganese(II)-\m~3~-1H-imidazole-4,5-dicarboxylato] ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m155 _journal_page_last m157 _journal_paper_doi 10.1107/S1600536804033306 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Mn (C5 H2 N2 O4) (H2 O1)]' _chemical_formula_moiety 'C5 H4 Mn N2 O5' _chemical_formula_sum 'C5 H4 Mn N2 O5' _chemical_formula_weight 227.04 _chemical_name_systematic ; Poly[aquamanganese(II)-\m~3~-1H-imidazole-4,5-dicarboxylato] ; _space_group_IT_number 4 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 117.36(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 7.0561(14) _cell_length_b 7.5531(15) _cell_length_c 7.6261(15) _cell_measurement_reflns_used 3428 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 3.01 _cell_volume 360.97(16) _computing_cell_refinement RAPID-AUTO _computing_data_collection 'RAPID-AUTO (Rigaku, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2002' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'Please provide missing information' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \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 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 3525 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 3.01 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.818 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_correction_T_min 0.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_meas ? _exptl_crystal_density_method . _exptl_crystal_description Prism _exptl_crystal_F_000 226 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.255 _refine_diff_density_min -0.216 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack 0.013(17) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 124 _refine_ls_number_reflns 1534 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0219 _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^)+(0.0256P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.0487 _reflns_number_gt 1456 _reflns_number_total 1534 _reflns_threshold_expression I>2\s(I) _cod_data_source_file nc6009.cif _cod_data_source_block I _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 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 2204928 _cod_database_fobs_code 2204928 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, 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_type_symbol Mn1 0.28813(4) 0.74557(3) 0.16233(4) 0.01539(9) Uani d . 1 Mn N1 0.1831(3) 0.6125(3) 0.3638(3) 0.0191(4) Uani d . 1 N N2 0.0594(3) 0.5519(3) 0.5732(3) 0.0215(4) Uani d . 1 N O1 0.5815(3) 0.6474(2) 0.4159(3) 0.0231(4) Uani d . 1 O O2 0.7245(2) 0.5010(2) 0.6994(2) 0.0193(3) Uani d . 1 O O3 0.5465(3) 0.3925(2) 0.9622(2) 0.0297(4) Uani d . 1 O O4 0.2724(3) 0.5204(2) 0.9794(2) 0.0204(3) Uani d . 1 O O1W -0.0375(3) 0.7794(2) -0.0537(3) 0.0305(5) Uani d D 1 O C1 0.0107(4) 0.5991(3) 0.3880(4) 0.0226(5) Uani d . 1 C C2 0.5667(3) 0.5713(3) 0.5535(3) 0.0160(4) Uani d . 1 C C3 0.3512(3) 0.5645(3) 0.5426(3) 0.0154(4) Uani d . 1 C C4 0.2763(3) 0.5269(3) 0.6752(3) 0.0176(5) Uani d . 1 C C5 0.3747(4) 0.4762(3) 0.8882(3) 0.0179(5) Uani d . 1 C H1 -0.1272 0.6196 0.2892 0.027 Uiso calc R 1 H H2 -0.0297 0.5394 0.6202 0.026 Uiso calc R 1 H H3 -0.133(4) 0.839(4) -0.042(5) 0.046 Uiso d D 1 H H4 -0.098(4) 0.688(3) -0.122(4) 0.046 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 0.01473(13) 0.01772(14) 0.01484(13) -0.00036(16) 0.00778(10) -0.00005(17) N1 0.0140(9) 0.0256(10) 0.0175(9) 0.0000(8) 0.0071(8) 0.0016(8) N2 0.0143(9) 0.0292(10) 0.0245(10) 0.0027(8) 0.0119(8) 0.0040(9) O1 0.0155(8) 0.0320(9) 0.0245(8) 0.0004(7) 0.0115(7) 0.0065(7) O2 0.0125(7) 0.0224(8) 0.0206(8) 0.0022(6) 0.0057(6) 0.0063(7) O3 0.0310(9) 0.0408(10) 0.0200(9) 0.0167(8) 0.0142(8) 0.0043(8) O4 0.0240(8) 0.0212(8) 0.0242(8) -0.0009(7) 0.0181(7) -0.0026(7) O1W 0.0209(8) 0.0260(12) 0.0340(9) 0.0064(8) 0.0037(7) -0.0092(8) C1 0.0141(10) 0.0291(13) 0.0239(12) 0.0027(10) 0.0081(9) 0.0052(10) C2 0.0156(10) 0.0159(10) 0.0176(10) -0.0007(9) 0.0085(9) -0.0021(9) C3 0.0133(10) 0.0164(10) 0.0158(10) 0.0013(9) 0.0060(8) -0.0002(9) C4 0.0149(10) 0.0189(11) 0.0211(11) 0.0017(9) 0.0101(9) 0.0003(9) C5 0.0201(10) 0.0165(11) 0.0191(10) -0.0015(9) 0.0108(9) -0.0022(9) 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 O1 Mn1 N1 . . 73.76(7) yes O1 Mn1 O2 . 2_656 95.83(7) yes O2 Mn1 N1 2_656 . 88.03(7) yes O3 Mn1 N1 2_656 . 165.64(7) yes O3 Mn1 O1 2_656 . 94.61(7) yes O3 Mn1 O2 2_656 2_656 84.76(7) yes O3 Mn1 O4 2_656 1_554 89.90(7) yes O3 Mn1 O1W 2_656 . 102.08(8) yes O4 Mn1 N1 1_554 . 98.91(7) yes O4 Mn1 O1 1_554 . 92.88(7) yes O4 Mn1 O2 1_554 2_656 170.11(6) yes O1W Mn1 N1 . . 90.29(8) yes O1W Mn1 O1 . . 162.79(7) yes O1W Mn1 O2 . 2_656 89.92(6) yes O1W Mn1 O4 . 1_554 83.05(7) yes Mn1 O1W H3 . . 127(2) no Mn1 O1W H4 . . 116(2) no N1 C1 N2 . . 111.3(2) no N1 C1 H1 . . 124.4 no N1 C3 C2 . . 116.03(19) no N2 C1 H1 . . 124.4 no N2 C4 C5 . . 119.4(2) no O1 C2 O2 . . 123.5(2) no O1 C2 C3 . . 116.72(19) no O2 C2 C3 . . 119.75(19) no O3 C5 O4 . . 124.7(2) no O3 C5 C4 . . 119.4(2) no O4 C5 C4 . . 115.8(2) no C1 N1 Mn1 . . 138.91(16) no C1 N1 C3 . . 105.7(2) no C1 N2 C4 . . 108.3(2) no C1 N2 H2 . . 125.9 no C2 O1 Mn1 . . 119.05(14) no C2 O2 Mn1 . 2_646 124.61(14) no C3 N1 Mn1 . . 113.05(15) no C3 C4 N2 . . 105.10(19) no C3 C4 C5 . . 135.41(19) no C4 N2 H2 . . 125.9 no C4 C3 N1 . . 109.61(19) no C4 C3 C2 . . 134.31(19) no C5 O3 Mn1 . 2_646 132.91(16) no C5 O4 Mn1 . 1_556 133.77(14) no H3 O1W H4 . . 107(2) 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 N1 . 2.228(2) yes Mn1 O1 . 2.2125(18) yes Mn1 O2 2_656 2.2197(16) yes Mn1 O3 2_656 2.1246(18) yes Mn1 O4 1_554 2.1700(16) yes Mn1 O1W . 2.1399(18) yes O1 C2 . 1.242(3) yes O2 C2 . 1.273(3) yes O3 C5 . 1.248(3) yes O4 C5 . 1.256(3) yes N1 C1 . 1.315(3) no N1 C3 . 1.382(3) no N2 C1 . 1.340(3) no N2 C4 . 1.374(3) no N2 H2 . 0.8600 no O2 Mn1 2_646 2.2197(16) no O3 Mn1 2_646 2.1246(18) no O4 Mn1 1_556 2.1700(16) no O1W H3 . 0.85(3) no O1W H4 . 0.85(3) no C1 H1 . 0.9300 no C2 C3 . 1.485(3) no C3 C4 . 1.370(3) no C4 C5 . 1.493(3) 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 N2 H2 O1 1_455 0.86 2.59 3.101(3) 119 yes N2 H2 O2 1_455 0.86 2.10 2.958(3) 173 yes O1W H4 O2 1_454 0.85(3) 1.96(3) 2.808(2) 171(3) yes O1W H3 O4 2_556 0.85(3) 1.87(3) 2.692(2) 162(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_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag Mn1 N1 C1 N2 . -158.03(19) no Mn1 N1 C3 C2 . -13.2(2) no Mn1 N1 C3 C4 . 164.48(15) no Mn1 O1 C2 O2 . 175.53(16) no Mn1 O1 C2 C3 . -4.5(3) no Mn1 O2 C2 O1 2_646 -140.18(18) no Mn1 O2 C2 C3 2_646 39.8(3) no Mn1 O3 C5 O4 2_646 161.83(17) no Mn1 O3 C5 C4 2_646 -16.9(3) no Mn1 O4 C5 O3 1_556 86.1(3) no Mn1 O4 C5 C4 1_556 -95.1(2) no N1 Mn1 O1 C2 . -1.90(16) no N1 C3 C4 N2 . 0.4(3) no N1 C3 C4 C5 . -177.0(2) no N2 C4 C5 O3 . 153.9(2) no N2 C4 C5 O4 . -24.9(3) no O1 Mn1 N1 C1 . 167.5(3) no O1 Mn1 N1 C3 . 8.13(15) no O1 C2 C3 N1 . 12.1(3) no O1 C2 C3 C4 . -164.8(3) no O2 Mn1 N1 C1 2_656 70.9(2) no O2 Mn1 N1 C3 2_656 -88.53(16) no O2 Mn1 O1 C2 2_656 84.34(18) no O2 C2 C3 N1 . -167.9(2) no O2 C2 C3 C4 . 15.2(4) no O3 Mn1 N1 C1 2_656 130.7(3) no O3 Mn1 N1 C3 2_656 -28.7(4) no O3 Mn1 O1 C2 2_656 169.52(17) no O4 Mn1 N1 C1 1_554 -102.0(3) no O4 Mn1 N1 C3 1_554 98.55(16) no O4 Mn1 O1 C2 1_554 -100.34(18) no O1W Mn1 N1 C1 . -19.0(3) no O1W Mn1 N1 C3 . -178.44(16) no O1W Mn1 O1 C2 . -24.6(4) no C1 N1 C3 C2 . -179.26(19) no C1 N1 C3 C4 . -1.6(3) no C1 N2 C4 C3 . 1.1(3) no C1 N2 C4 C5 . 178.9(2) no C2 C3 C4 N2 . 177.4(2) no C2 C3 C4 C5 . 0.0(5) no C3 N1 C1 N2 . 2.3(3) no C3 C4 C5 O3 . -29.0(4) no C3 C4 C5 O4 . 152.2(3) no C4 N2 C1 N1 . -2.2(3) no