#------------------------------------------------------------------------------ #$Date: 2009-11-18 16:56:34 +0200 (Wed, 18 Nov 2009) $ #$Revision: 858 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4000500.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_4000500 loop_ _publ_author_name 'Josefina Perles' 'Carlos Fortes-Revilla' 'Enrique Guti\'errez-Puebla' 'Marta Iglesias' 'M. \'Angeles Monge' 'Caridad Ruiz-Valero' 'Natalia Snejko' _publ_section_title ; Synthesis, Structure, and Catalytic Properties of Rare-Earth Ternary Sulfates ; _journal_issue 10 _journal_name_full 'Chemistry of Materials' _journal_page_first 2701 _journal_page_last 2706 _journal_volume 17 _journal_year 2005 _chemical_formula_sum 'Gd H2 Na O9 S2' _[local]_cod_chemical_formula_sum_orig 'H2 Gd Na O9 S2' _chemical_formula_weight 390.38 _chemical_name_systematic ; ? ; _symmetry_cell_setting Trigonal _symmetry_space_group_name_Hall 'P 32 2"' _symmetry_space_group_name_H-M 'P 32 2 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 3 _cell_length_a 6.8816(6) _cell_length_b 6.8816(6) _cell_length_c 12.7702(17) _cell_measurement_reflns_used 3792 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 31.17 _cell_measurement_theta_min 3.77 _cell_volume 523.73(10) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.955 _diffrn_measured_fraction_theta_max 0.955 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega 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 0.0954 _diffrn_reflns_av_sigmaI/netI 0.1050 _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 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 3759 _diffrn_reflns_theta_full 31.17 _diffrn_reflns_theta_max 31.17 _diffrn_reflns_theta_min 3.77 _exptl_absorpt_coefficient_mu 10.181 _exptl_absorpt_correction_T_max 0.8223 _exptl_absorpt_correction_T_min 0.1851 _exptl_absorpt_correction_type multiscan _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 3.713 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description hexagonal _exptl_crystal_F_000 543 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.413 _refine_diff_density_min -1.523 _refine_diff_density_rms 0.317 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(5) _refine_ls_extinction_coef 0.0020(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 66 _refine_ls_number_reflns 1068 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.994 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0519 _refine_ls_shift/su_max 2.835 _refine_ls_shift/su_mean 0.305 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0868 _refine_ls_wR_factor_ref 0.0908 _reflns_number_gt 874 _reflns_number_total 1068 _reflns_threshold_expression >2sigma(I) _space_group_IT_number 154 _[local]_cod_data_source_file cm049451zsi20041006_054353.cif _[local]_cod_cif_authors_sg_H-M P3(2)21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Gd1 Gd 0.56458(12) 0.56458(12) 0.0000 0.0098(2) Uani 1 2 d S S1 S 0.5454(4) 0.5579(5) -0.24222(15) 0.0109(4) Uani 1 1 d . O1 O 0.4859(13) 0.3523(13) 0.1688(5) 0.018(2) Uani 1 1 d . O2 O 0.7422(11) 0.6117(11) -0.1748(5) 0.0167(18) Uani 1 1 d . O3 O 0.1696(11) 0.4128(11) 0.0298(6) 0.0152(18) Uani 1 1 d . O4 O 0.8722(14) 0.4959(13) 0.0169(6) 0.0133(19) Uani 1 1 d . O5 O 0.922(2) 0.922(2) 0.0000 0.047(6) Uani 1 2 d S Na1 Na 0.4688(9) 1.0000 0.1667 0.0165(12) Uani 1 2 d S H1 H 0.91(3) 1.03(2) 0.041(10) 0.08(5) Uiso 1 1 d . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Gd1 0.0101(3) 0.0101(3) 0.0098(3) 0.0000(2) 0.0000(2) 0.0055(5) S1 0.0143(12) 0.0108(12) 0.0099(9) 0.0015(10) -0.0005(9) 0.0081(12) O1 0.020(5) 0.018(4) 0.016(4) -0.002(3) -0.003(3) 0.010(4) O2 0.011(4) 0.022(5) 0.016(3) 0.000(3) -0.005(3) 0.007(4) O3 0.007(3) 0.015(4) 0.022(4) 0.006(3) 0.006(3) 0.004(3) O4 0.011(4) 0.015(5) 0.011(3) -0.002(3) -0.003(3) 0.005(4) O5 0.015(6) 0.015(6) 0.103(14) -0.016(5) 0.016(5) 0.001(7) Na1 0.015(2) 0.014(4) 0.020(3) 0.003(3) 0.0013(15) 0.007(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Gd1 O4 2.398(8) 4 Gd1 O4 2.398(8) . Gd1 O3 2.405(7) 4 Gd1 O3 2.405(7) . Gd1 O5 2.465(15) . Gd1 O2 2.488(7) 4 Gd1 O2 2.488(7) . Gd1 O1 2.506(7) 4 Gd1 O1 2.506(7) . Gd1 S1 3.0954(19) 4 Gd1 S1 3.0954(19) . Gd1 Na1 3.990(3) 2_764 S1 O4 1.479(8) 2_654 S1 O3 1.475(7) 2_664 S1 O2 1.487(7) . S1 O1 1.494(7) 4 S1 Na1 3.296(2) 3_564 O1 S1 1.494(7) 4 O1 Na1 2.368(9) 1_545 O2 Na1 2.423(9) 2_764 O3 S1 1.475(7) 3_565 O3 Na1 2.874(8) 2_664 O4 S1 1.479(8) 3_665 O4 Na1 2.543(7) 2_764 Na1 O1 2.368(9) 5_565 Na1 O1 2.368(9) 1_565 Na1 O2 2.423(9) 3_675 Na1 O2 2.423(9) 4 Na1 O4 2.543(7) 3_675 Na1 O4 2.543(7) 4 Na1 O3 2.874(8) 3_565 Na1 O3 2.874(8) 4_565 Na1 S1 3.296(2) 2_665 Na1 S1 3.296(2) 6_664 Na1 Gd1 3.990(3) 3_675 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_3 O4 Gd1 O4 139.9(4) 4 . O4 Gd1 O3 144.8(3) 4 4 O4 Gd1 O3 73.7(2) . 4 O4 Gd1 O3 73.7(2) 4 . O4 Gd1 O3 144.8(3) . . O3 Gd1 O3 77.1(3) 4 . O4 Gd1 O5 69.64(19) 4 . O4 Gd1 O5 70.25(19) . . O3 Gd1 O5 141.75(16) 4 . O3 Gd1 O5 141.16(16) . . O4 Gd1 O2 71.4(2) 4 4 O4 Gd1 O2 96.0(2) . 4 O3 Gd1 O2 125.0(2) 4 4 O3 Gd1 O2 85.0(2) . 4 O5 Gd1 O2 71.78(15) . 4 O4 Gd1 O2 96.0(2) 4 . O4 Gd1 O2 71.4(2) . . O3 Gd1 O2 85.0(2) 4 . O3 Gd1 O2 125.0(2) . . O5 Gd1 O2 71.98(15) . . O2 Gd1 O2 143.8(3) 4 . O4 Gd1 O1 76.3(3) 4 4 O4 Gd1 O1 120.7(3) . 4 O3 Gd1 O1 75.1(3) 4 4 O3 Gd1 O1 68.4(2) . 4 O5 Gd1 O1 113.43(17) . 4 O2 Gd1 O1 142.8(2) 4 4 O2 Gd1 O1 56.7(2) . 4 O4 Gd1 O1 120.7(3) 4 . O4 Gd1 O1 76.3(3) . . O3 Gd1 O1 68.4(2) 4 . O3 Gd1 O1 75.1(3) . . O5 Gd1 O1 113.64(17) . . O2 Gd1 O1 56.7(2) 4 . O2 Gd1 O1 142.8(2) . . O1 Gd1 O1 132.9(3) 4 . O4 Gd1 S1 97.01(18) 4 4 O4 Gd1 S1 84.12(18) . 4 O3 Gd1 S1 96.97(19) 4 4 O3 Gd1 S1 80.43(19) . 4 O5 Gd1 S1 91.65(5) . 4 O2 Gd1 S1 28.31(16) 4 4 O2 Gd1 S1 153.94(16) . 4 O1 Gd1 S1 148.82(18) 4 4 O1 Gd1 S1 28.53(18) . 4 O4 Gd1 S1 84.12(18) 4 . O4 Gd1 S1 97.02(18) . . O3 Gd1 S1 80.43(19) 4 . O3 Gd1 S1 96.97(19) . . O5 Gd1 S1 91.64(5) . . O2 Gd1 S1 153.93(16) 4 . O2 Gd1 S1 28.31(16) . . O1 Gd1 S1 28.53(18) 4 . O1 Gd1 S1 148.83(18) . . S1 Gd1 S1 176.71(10) 4 . O4 Gd1 Na1 126.4(2) 4 2_764 O4 Gd1 Na1 37.39(17) . 2_764 O3 Gd1 Na1 70.51(18) 4 2_764 O3 Gd1 Na1 142.36(18) . 2_764 O5 Gd1 Na1 73.22(6) . 2_764 O2 Gd1 Na1 129.48(16) 4 2_764 O2 Gd1 Na1 35.12(17) . 2_764 O1 Gd1 Na1 84.85(18) 4 2_764 O1 Gd1 Na1 108.9(2) . 2_764 S1 Gd1 Na1 121.49(7) 4 2_764 S1 Gd1 Na1 59.63(6) . 2_764 O4 S1 O3 108.1(4) 2_654 2_664 O4 S1 O2 110.4(5) 2_654 . O3 S1 O2 110.2(4) 2_664 . O4 S1 O1 111.0(4) 2_654 4 O3 S1 O1 111.7(5) 2_664 4 O2 S1 O1 105.5(4) . 4 O4 S1 Gd1 129.9(3) 2_654 . O3 S1 Gd1 122.0(3) 2_664 . O2 S1 Gd1 52.5(3) . . O1 S1 Gd1 53.3(3) 4 . O4 S1 Na1 47.5(3) 2_654 3_564 O3 S1 Na1 60.5(3) 2_664 3_564 O2 S1 Na1 126.1(3) . 3_564 O1 S1 Na1 127.7(3) 4 3_564 Gd1 S1 Na1 177.20(12) . 3_564 S1 O1 Na1 137.9(4) 4 1_545 S1 O1 Gd1 98.2(4) 4 . Na1 O1 Gd1 118.2(3) 1_545 . S1 O2 Na1 133.2(4) . 2_764 S1 O2 Gd1 99.2(3) . . Na1 O2 Gd1 108.7(3) 2_764 . S1 O3 Gd1 141.2(4) 3_565 . S1 O3 Na1 92.9(3) 3_565 2_664 Gd1 O3 Na1 104.5(2) . 2_664 S1 O4 Gd1 145.2(4) 3_665 . S1 O4 Na1 107.1(4) 3_665 2_764 Gd1 O4 Na1 107.7(3) . 2_764 O1 Na1 O1 125.0(5) 5_565 1_565 O1 Na1 O2 156.7(4) 5_565 3_675 O1 Na1 O2 78.2(2) 1_565 3_675 O1 Na1 O2 78.2(2) 5_565 4 O1 Na1 O2 156.7(4) 1_565 4 O2 Na1 O2 78.9(4) 3_675 4 O1 Na1 O4 113.0(2) 5_565 3_675 O1 Na1 O4 80.7(2) 1_565 3_675 O2 Na1 O4 70.1(3) 3_675 3_675 O2 Na1 O4 87.7(3) 4 3_675 O1 Na1 O4 80.7(2) 5_565 4 O1 Na1 O4 113.0(2) 1_565 4 O2 Na1 O4 87.7(3) 3_675 4 O2 Na1 O4 70.1(3) 4 4 O4 Na1 O4 151.5(4) 3_675 4 O1 Na1 O3 62.8(2) 5_565 3_565 O1 Na1 O3 98.4(3) 1_565 3_565 O2 Na1 O3 121.4(2) 3_675 3_565 O2 Na1 O3 90.0(2) 4 3_565 O4 Na1 O3 51.9(2) 3_675 3_565 O4 Na1 O3 141.5(2) 4 3_565 O1 Na1 O3 98.4(3) 5_565 4_565 O1 Na1 O3 62.8(2) 1_565 4_565 O2 Na1 O3 90.0(2) 3_675 4_565 O2 Na1 O3 121.4(2) 4 4_565 O4 Na1 O3 141.5(2) 3_675 4_565 O4 Na1 O3 51.9(2) 4 4_565 O3 Na1 O3 140.6(4) 3_565 4_565 O1 Na1 S1 88.37(16) 5_565 2_665 O1 Na1 S1 89.37(17) 1_565 2_665 O2 Na1 S1 95.18(19) 3_675 2_665 O2 Na1 S1 88.60(18) 4 2_665 O4 Na1 S1 25.4(2) 3_675 2_665 O4 Na1 S1 157.6(2) 4 2_665 O3 Na1 S1 26.54(15) 3_565 2_665 O3 Na1 S1 150.0(2) 4_565 2_665 O1 Na1 S1 89.37(17) 5_565 6_664 O1 Na1 S1 88.37(16) 1_565 6_664 O2 Na1 S1 88.60(18) 3_675 6_664 O2 Na1 S1 95.18(19) 4 6_664 O4 Na1 S1 157.6(2) 3_675 6_664 O4 Na1 S1 25.40(19) 4 6_664 O3 Na1 S1 150.0(2) 3_565 6_664 O3 Na1 S1 26.54(14) 4_565 6_664 S1 Na1 S1 175.1(2) 2_665 6_664 O1 Na1 Gd1 146.38(16) 5_565 3_675 O1 Na1 Gd1 70.55(19) 1_565 3_675 O2 Na1 Gd1 36.20(16) 3_675 3_675 O2 Na1 Gd1 88.4(2) 4 3_675 O4 Na1 Gd1 34.9(2) 3_675 3_675 O4 Na1 Gd1 123.6(2) 4 3_675 O3 Na1 Gd1 86.86(14) 3_565 3_675 O3 Na1 Gd1 114.79(15) 4_565 3_675 S1 Na1 Gd1 60.33(6) 2_665 3_675 S1 Na1 Gd1 122.76(10) 6_664 3_675 O1 Na1 Gd1 70.55(19) 5_565 . O1 Na1 Gd1 146.38(16) 1_565 . O2 Na1 Gd1 88.4(2) 3_675 . O2 Na1 Gd1 36.20(16) 4 . O4 Na1 Gd1 123.6(2) 3_675 . O4 Na1 Gd1 34.9(2) 4 . O3 Na1 Gd1 114.79(14) 3_565 . O3 Na1 Gd1 86.86(14) 4_565 . S1 Na1 Gd1 122.76(10) 2_665 . S1 Na1 Gd1 60.33(6) 6_664 . Gd1 Na1 Gd1 114.53(15) 3_675 .