#------------------------------------------------------------------------------ #$Date: 2020-02-07 10:23:31 +0200 (Fri, 07 Feb 2020) $ #$Revision: 247949 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557266.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_1557266 loop_ _publ_author_name 'Simonsen, Ole' _publ_section_title ; Crystal Structures of Hexaaquamagnesium Diliturate Dihydrate, Mg(H2O)6(2+)(C4H2N3O5-)2.2H2O and the Isomorphous Calcium Salt ; _journal_name_full 'Acta Chemica Scandinavica' _journal_page_first 861 _journal_page_last 864 _journal_paper_doi 10.3891/acta.chem.scand.51-0861 _journal_volume 51 _journal_year 1997 _chemical_formula_moiety '2(C4 H2 N3 O5), Ca (H2 O)6, 2(H2 O)' _chemical_formula_sum 'C8 H20 Ca N6 O18' _chemical_formula_weight 528.356 _chemical_name_common ; Hexaaquacalcium Diliturate Dihydrate ; _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90. _cell_angle_beta 97.08(1) _cell_angle_gamma 90. _cell_formula_units_Z 2 _cell_length_a 12.349(1) _cell_length_b 12.167(1) _cell_length_c 6.818(1) _cell_volume 1016.60(19) _diffrn_ambient_temperature 293 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu 0.3978 _exptl_crystal_density_diffrn 1.726 _refine_ls_number_parameters 181 _refine_ls_number_reflns 2186 _refine_ls_R_factor_gt 0.044 _refine_ls_wR_factor_gt 0.037 _cod_data_source_file Acta-Chem-Scand-1997-51-861-2.cif _cod_data_source_block 2 _cod_original_cell_volume 1016.6(3) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1557266 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ca Ca Uiso 0.50000 0.50000 0.50000 1.000 0.0362(2) . . . . O2 O Uiso -0.17390(10) 0.82420(10) 0.1164(3) 1.000 0.0418(7) . . . . O4 O Uiso 0.12400(10) 1.02160(10) 0.3440(3) 1.000 0.0440(7) . . . . O6 O Uiso 0.12450(10) 0.62900(10) 0.3473(3) 1.000 0.0365(6) . . . . O51 O Uiso 0.30320(10) 0.7393(2) 0.4724(4) 1.000 0.0675(9) . . . . O52 O Uiso 0.30190(10) 0.91270(10) 0.4703(4) 1.000 0.0574(8) . . . . N1 N Uiso -0.02100(10) 0.73060(10) 0.2337(3) 1.000 0.0280(7) . . . . N3 N Uiso -0.02110(10) 0.91940(10) 0.2321(4) 1.000 0.0318(7) . . . . N5 N Uiso 0.25420(10) 0.8254(2) 0.4349(4) 1.000 0.0328(7) . . . . C2 C Uiso -0.0777(2) 0.8250(2) 0.1896(4) 1.000 0.0301(8) . . . . C4 C Uiso 0.0875(2) 0.9281(2) 0.3140(4) 1.000 0.0291(8) . . . . C5 C Uiso 0.1425(2) 0.8257(2) 0.3548(4) 1.000 0.0266(7) . . . . C6 C Uiso 0.0883(2) 0.7225(2) 0.3159(4) 1.000 0.0263(7) . . . . O10 O Uiso 0.31230(10) 0.50640(10) 0.4691(4) 1.000 0.0521(7) . . . . O20 O Uiso 0.47040(10) 0.34940(10) 0.2935(4) 1.000 0.0624(9) . . . . O30 O Uiso 0.49860(10) 0.61130(10) 0.2190(3) 1.000 0.0463(7) . . . . O40 O Uiso 0.31700(10) 0.35700(10) -0.0361(4) 1.000 0.0486(7) . . . . 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' Ca Ca 0.2262 0.3064 ' 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' 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N1 C6 126.37(17) . . . yes C2 N3 C4 126.55(18) . . . yes O51 N5 O52 119.29(17) . . . yes O51 N5 C5 121.1(2) . . . yes O52 N5 C5 119.7(2) . . . yes O2 C2 N1 121.9(2) . . . yes O2 C2 N3 122.6(2) . . . yes N1 C2 N3 115.5(2) . . . yes O4 C4 N3 116.9(2) . . . yes O4 C4 C5 128.1(2) . . . yes N3 C4 C5 115.0(2) . . . yes N5 C5 C4 119.5(2) . . . yes N5 C5 C6 118.6(2) . . . yes C4 C5 C6 121.9(2) . . . no O6 C6 N1 116.5(2) . . . yes O6 C6 C5 128.8(2) . . . yes N1 C6 C5 114.7(2) . . . yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 C2 1.231(3) . . yes O4 C4 1.231(3) . . yes O6 C6 1.231(3) . . yes O51 N5 1.221(3) . . yes O52 N5 1.224(3) . . yes N1 C2 1.359(3) . . yes N1 C6 1.400(3) . . yes N3 C2 1.357(3) . . yes N3 C4 1.392(3) . . yes N5 C5 1.420(3) . . yes C4 C5 1.430(3) . . no C5 C6 1.432(3) . . no 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 O2 179.7(2) . . . . no C6 N1 C2 N3 -0.5(4) . . . . no C2 N1 C6 O6 179.1(2) . . . . no C2 N1 C6 C5 0.0(4) . . . . no C4 N3 C2 O2 -179.8(3) . . . . no C4 N3 C2 N1 0.4(4) . . . . no C2 N3 C4 O4 -179.1(3) . . . . no C2 N3 C4 C5 0.3(4) . . . . no O51 N5 C5 C4 179.6(3) . . . . no O51 N5 C5 C6 -0.9(4) . . . . no O52 N5 C5 C4 0.8(4) . . . . no O52 N5 C5 C6 -179.6(3) . . . . no O4 C4 C5 N5 -2.0(4) . . . . no O4 C4 C5 C6 178.5(3) . . . . no N3 C4 C5 N5 178.8(2) . . . . no N3 C4 C5 C6 -0.8(4) . . . . no N5 C5 C6 O6 2.2(4) . . . . no N5 C5 C6 N1 -178.9(2) . . . . no C4 C5 C6 O6 -178.3(3) . . . . no C4 C5 C6 N1 0.7(4) . . . . no