#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100930.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_1100930 _chemical_formula_sum 'C4.50 H15 F2 Ge6.44 N1.50 O17 Si0.56' _chemical_formula_weight 883.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' 'C' 'C' 0.0033 0.0016 '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' 'F' 'F' 0.0171 0.0103 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M 'I4/mmm ?' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x, y, -z' 'x, -y, -z' '-y, -x, z' 'y, x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 27.646(2) _cell_length_b 27.646(2) _cell_length_c 17.0885(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 13060.8(18) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _exptl_crystal_density_diffrn 1.797 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6726 _exptl_absorpt_coefficient_mu 5.933 _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 47555 _diffrn_reflns_av_R_equivalents 0.1026 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5977 _reflns_number_gt 5471 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0975P)^2^+100.2118P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 5977 _refine_ls_number_parameters 327 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0570 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1430 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.171 _refine_ls_shift/su_mean 0.001 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 _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.35377(4) 0.19211(4) 0.25829(6) 0.0166(3) Uani 1 1 d . . . Ge2 Ge 0.36200(4) 0.05832(4) 0.28091(6) 0.0163(3) Uani 1 1 d . . . Ge3 Ge 0.29027(4) 0.09192(4) 0.17012(6) 0.0192(3) Uani 1 1 d . . . Ge4 Ge 0.32048(4) 0.13247(4) 0.39945(6) 0.0170(5) Uani 0.864(7) 1 d P . . Si4 Si 0.32048(4) 0.13247(4) 0.39945(6) 0.0170(5) Uani 0.14 1 d P . . Ge5 Ge 0.43849(4) 0.12649(4) 0.20203(6) 0.0166(4) Uani 0.892(7) 1 d P . . Si5 Si 0.43849(4) 0.12649(4) 0.20203(6) 0.0166(4) Uani 0.11 1 d P . . Ge6 Ge 0.36095(4) 0.15980(5) 0.08770(6) 0.0183(5) Uani 0.841(7) 1 d P . . Si6 Si 0.36095(4) 0.15980(5) 0.08770(6) 0.0183(5) Uani 0.16 1 d P . . Ge7 Ge 0.24548(4) 0.16457(4) 0.28281(7) 0.0193(5) Uani 0.841(6) 1 d P . . Si7 Si 0.24548(4) 0.16457(4) 0.28281(7) 0.0193(5) Uani 0.16 1 d P . . F1 F 0.3693(3) 0.2552(2) 0.2766(4) 0.0349(17) Uani 1 1 d . . . F2 F 0.2502(3) 0.0530(3) 0.1124(4) 0.0404(18) Uani 1 1 d . . . O1 O 0.4206(3) 0.1767(3) 0.2551(4) 0.0204(15) Uani 1 1 d . . . O2 O 0.3371(3) 0.1242(2) 0.2372(4) 0.0180(15) Uani 1 1 d . . . O3 O 0.2876(3) 0.2098(3) 0.2627(4) 0.0228(16) Uani 1 1 d . . . O4 O 0.3512(3) 0.2061(3) 0.1512(4) 0.0218(16) Uani 1 1 d . . . O5 O 0.3545(3) 0.1805(3) 0.3662(4) 0.0241(17) Uani 1 1 d . . . O6 O 0.3464(3) 0.0767(3) 0.3775(4) 0.0230(16) Uani 1 1 d . . . O7 O 0.3157(3) 0.0393(3) 0.2145(4) 0.0233(16) Uani 1 1 d . . . O8 O 0.4212(3) 0.0722(3) 0.2454(4) 0.0237(16) Uani 1 1 d . . . O9 O 0.3790(3) -0.0015(3) 0.3146(5) 0.035(2) Uani 1 1 d . . . O10 O 0.2390(3) 0.1215(3) 0.2098(4) 0.0261(17) Uani 1 1 d . . . O11 O 0.3138(3) 0.1169(3) 0.0845(4) 0.0227(16) Uani 1 1 d . . . O12 O 0.2604(3) 0.1343(3) 0.3687(4) 0.0234(16) Uani 1 1 d . . . O13 O 0.3136(3) 0.1339(3) 0.4992(4) 0.034(2) Uani 1 1 d . . . O14 O 0.4151(3) 0.1286(3) 0.1070(4) 0.0218(16) Uani 1 1 d . . . O15 O 0.1876(3) 0.1876(3) 0.2960(6) 0.030(3) Uani 1 2 d S . . OW1 O 0.5000 0.0000 -0.2500 0.18(2) Uani 1 4 d S . . OW2 O 0.4224(5) 0.2859(5) 0.2433(13) 0.115(7) Uani 1 1 d . . . OW3 O 0.4686(6) 0.2664(8) 0.286(2) 0.211(17) Uani 1 1 d . . . OW4 O 0.4454(10) 0.5002(9) 0.4095(16) 0.018(10) Uani 0.25(3) 1 d P . . N1 N 0.3432(5) 0.0000 0.5000 0.033(3) Uani 1 2 d S . . H1A H 0.3539 -0.0109 0.4542 0.050 Uiso 0.50 1 calc PR . . H1B H 0.3539 -0.0191 0.5382 0.050 Uiso 0.50 1 calc PR . . H1C H 0.3539 0.0300 0.5076 0.050 Uiso 0.50 1 calc PR . . C1 C 0.2917(7) 0.0000 0.5000 0.070(8) Uani 1 2 d SD . . H1D H 0.2827 0.0188 0.4543 0.084 Uiso 0.50 1 calc PR . . H1E H 0.2827 -0.0331 0.4881 0.084 Uiso 0.50 1 calc PR . . C2 C 0.2599(8) 0.0141(13) 0.5569(17) 0.053(8) Uani 0.50 1 d PD . . H2A H 0.2629 0.0488 0.5639 0.064 Uiso 0.50 1 calc PR . . H2B H 0.2693 -0.0011 0.6058 0.064 Uiso 0.50 1 calc PR . . C3 C 0.2084(7) 0.002(2) 0.541(3) 0.12(2) Uani 0.50 1 d PD . . H3D H 0.1890 0.0128 0.5849 0.187 Uiso 0.50 1 calc PR . . H3E H 0.2049 -0.0318 0.5343 0.187 Uiso 0.50 1 calc PR . . H3F H 0.1980 0.0189 0.4949 0.187 Uiso 0.50 1 calc PR . . N2 N 0.2216(8) 0.2216(8) 0.6267(19) 0.32(5) Uani 1 2 d SD . . H2C H 0.2338 0.2371 0.6679 0.475 Uiso 0.50 1 calc PR . . H2D H 0.2073 0.2427 0.5949 0.475 Uiso 0.50 1 calc PR . . H2E H 0.2453 0.2066 0.6012 0.475 Uiso 0.50 1 calc PR . . C4 C 0.1924(10) 0.1924(10) 0.6485(16) 0.20(4) Uani 1 2 d SD . . H4A H 0.1702 0.2099 0.6821 0.245 Uiso 0.50 1 calc PR . . H4B H 0.2099 0.1702 0.6821 0.245 Uiso 0.50 1 calc PR . . C5 C 0.1652(8) 0.1652(8) 0.603(3) 0.82(18) Uani 1 2 d SD . . H5A H 0.1313 0.1715 0.6130 0.985 Uiso 0.50 1 calc PR . . H5B H 0.1715 0.1313 0.6130 0.985 Uiso 0.50 1 calc PR . . C6 C 0.1773(16) 0.1773(16) 0.513(2) 0.41(8) Uani 1 2 d SD . . H6A H 0.1568 0.1585 0.4790 0.616 Uiso 1 2 calc SR . . H6B H 0.2106 0.1697 0.5020 0.616 Uiso 0.50 1 calc PR . . H6C H 0.1718 0.2111 0.5029 0.616 Uiso 0.50 1 calc PR . . N3 N 0.2902(7) 0.2902(7) 0.3762(13) 0.107(12) Uani 1 2 d SD . . H3A H 0.2954 0.2674 0.3405 0.161 Uiso 0.50 1 calc PR . . H3B H 0.3182 0.3040 0.3889 0.161 Uiso 0.50 1 calc PR . . H3C H 0.2703 0.3125 0.3568 0.161 Uiso 0.50 1 calc PR . . C7 C 0.2689(10) 0.2689(10) 0.4447(16) 0.24(4) Uani 1 2 d SD . . H7A H 0.2396 0.2527 0.4279 0.287 Uiso 0.50 1 calc PR . . H7B H 0.2909 0.2439 0.4625 0.287 Uiso 0.50 1 calc PR . . C8 C 0.2569(18) 0.2966(16) 0.5102(14) 0.44(12) Uani 0.50 1 d PD . . H8A H 0.2223 0.2940 0.5190 0.526 Uiso 0.50 1 calc PR . . H8B H 0.2639 0.3303 0.4988 0.526 Uiso 0.50 1 calc PR . . C9 C 0.2828(19) 0.2828(19) 0.585(2) 0.26(5) Uani 1 2 d SD . . H9A H 0.2735 0.3045 0.6260 0.385 Uiso 0.50 1 calc PR . . H9B H 0.3171 0.2847 0.5768 0.385 Uiso 0.50 1 calc PR . . H9C H 0.2742 0.2503 0.5991 0.385 Uiso 0.50 1 calc PR . . 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 Ge1 0.0240(6) 0.0155(5) 0.0102(5) -0.0004(4) 0.0016(4) 0.0021(4) Ge2 0.0202(6) 0.0148(5) 0.0139(5) -0.0009(4) -0.0008(4) 0.0020(4) Ge3 0.0204(6) 0.0237(6) 0.0135(5) -0.0003(4) -0.0016(4) 0.0017(4) Ge4 0.0252(7) 0.0186(7) 0.0072(6) -0.0002(4) -0.0008(4) 0.0048(5) Si4 0.0252(7) 0.0186(7) 0.0072(6) -0.0002(4) -0.0008(4) 0.0048(5) Ge5 0.0137(7) 0.0229(7) 0.0133(6) 0.0000(4) -0.0007(4) 0.0000(4) Si5 0.0137(7) 0.0229(7) 0.0133(6) 0.0000(4) -0.0007(4) 0.0000(4) Ge6 0.0214(7) 0.0253(8) 0.0082(6) 0.0012(5) -0.0002(4) 0.0032(5) Si6 0.0214(7) 0.0253(8) 0.0082(6) 0.0012(5) -0.0002(4) 0.0032(5) Ge7 0.0214(7) 0.0236(8) 0.0129(6) 0.0035(5) 0.0023(5) 0.0093(5) Si7 0.0214(7) 0.0236(8) 0.0129(6) 0.0035(5) 0.0023(5) 0.0093(5) F1 0.061(5) 0.017(3) 0.027(3) 0.003(3) 0.006(3) -0.002(3) F2 0.040(4) 0.046(5) 0.035(4) -0.003(3) -0.015(3) -0.008(4) O1 0.025(4) 0.023(4) 0.013(3) -0.004(3) 0.001(3) -0.008(3) O2 0.022(4) 0.019(4) 0.013(3) 0.002(3) -0.003(3) 0.003(3) O3 0.032(4) 0.018(4) 0.018(4) 0.002(3) 0.006(3) 0.009(3) O4 0.034(4) 0.022(4) 0.010(3) 0.001(3) 0.005(3) 0.002(3) O5 0.033(4) 0.029(4) 0.010(3) -0.007(3) 0.002(3) -0.001(3) O6 0.035(5) 0.022(4) 0.012(3) 0.002(3) 0.001(3) 0.006(3) O7 0.033(4) 0.016(4) 0.020(3) -0.004(3) -0.004(3) -0.002(3) O8 0.020(4) 0.030(4) 0.022(4) 0.007(3) 0.000(3) 0.011(3) O9 0.048(5) 0.011(4) 0.045(5) 0.002(3) -0.020(4) 0.000(3) O10 0.021(4) 0.039(5) 0.019(4) -0.002(3) 0.006(3) 0.005(3) O11 0.027(4) 0.027(4) 0.015(3) -0.009(3) -0.006(3) 0.002(3) O12 0.030(4) 0.024(4) 0.015(3) 0.004(3) 0.000(3) 0.002(3) O13 0.048(5) 0.047(5) 0.008(3) -0.006(3) -0.009(3) -0.002(4) O14 0.023(4) 0.028(4) 0.015(3) 0.001(3) 0.001(3) 0.004(3) O15 0.030(4) 0.030(4) 0.030(6) 0.007(4) 0.007(4) 0.016(5) OW1 0.022(7) 0.022(7) 0.49(8) 0.000 0.000 0.000 OW2 0.063(9) 0.052(8) 0.23(2) -0.010(10) 0.070(11) -0.024(6) OW3 0.070(11) 0.131(17) 0.43(5) -0.15(2) -0.105(19) 0.052(11) OW4 0.021(17) 0.000(14) 0.032(18) -0.007(11) -0.024(13) 0.002(10) N1 0.039(9) 0.032(8) 0.028(7) 0.006(6) 0.000 0.000 C1 0.052(15) 0.069(17) 0.088(18) 0.051(15) 0.000 0.000 C2 0.026(15) 0.09(3) 0.047(16) -0.021(16) 0.003(12) 0.011(15) C3 0.04(2) 0.15(5) 0.19(6) -0.08(5) 0.03(3) 0.01(3) N2 0.36(6) 0.36(6) 0.24(6) -0.24(6) -0.24(6) 0.23(7) C4 0.21(4) 0.21(4) 0.19(4) 0.17(4) 0.17(4) 0.19(5) C5 1.0(2) 1.0(2) 0.4(2) -0.27(14) -0.27(14) -0.524 C6 0.43(11) 0.43(11) 0.38(12) 0.22(10) 0.22(10) 0.40(11) N3 0.096(13) 0.096(13) 0.13(2) -0.071(15) -0.071(15) 0.057(16) C7 0.35(7) 0.35(7) 0.026(16) 0.00(3) 0.00(3) 0.20(8) C8 0.9(3) 0.21(8) 0.25(10) 0.18(8) 0.34(15) 0.41(14) C9 0.16(4) 0.16(4) 0.44(13) -0.10(6) -0.10(6) 0.13(5) _data_global _publ_section_title ; Synthesis, structure and catalytic properties of rare-earth ternary sulfates ; loop_ _publ_author_name 'Josefina Perles' 'Carlos Fortes-Revilla' 'Enrique Gutierrez-Puebla' 'Marta Iglesias' 'M. Angeles Monge' 'Caridad Ruiz-Valero' 'Natalia Snejko' _chemical_formula_sum 'H2 La Na O9 S2' _chemical_formula_weight 372.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' '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' 'La' 'La' -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(1)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 7.0538(5) _cell_length_b 7.0538(5) _cell_length_c 12.9625(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 558.55(8) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4245 _cell_measurement_theta_min 4.59 _cell_measurement_theta_max 31.13 _exptl_crystal_description polyhedron _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 3.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 522 _exptl_absorpt_coefficient_mu 6.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1427 _exptl_absorpt_correction_T_max 0.5680 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4198 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.59 _diffrn_reflns_theta_max 31.13 _reflns_number_total 1136 _reflns_number_gt 972 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0002(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 1136 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 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 _atom_site_disorder_assembly _atom_site_disorder_group La1 La 0.56735(8) 0.56735(8) 1.0000 0.01057(14) Uani 1 2 d S . . O1 O 0.4956(9) 0.3630(9) 0.8257(3) 0.0210(12) Uani 1 1 d . . . O2 O 0.6109(7) 0.7406(7) 0.8184(3) 0.0180(11) Uani 1 1 d . . . O3 O 0.4090(8) 0.1637(8) 1.0262(4) 0.0206(12) Uani 1 1 d . . . O4 O 0.4975(9) 0.8821(9) 1.0137(3) 0.0195(12) Uani 1 1 d . . . S1 S 0.5600(3) 0.5474(3) 0.75332(9) 0.0119(3) Uani 1 1 d . . . O5 O 0.9302(14) 0.9302(14) 1.0000 0.058(4) Uani 1 2 d S . . Na1 Na 1.0000 0.4700(6) 0.1667 0.0228(8) Uani 1 2 d S . . H1 H 1.049(17) 0.93(2) 1.056(7) 0.08(4) 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 La1 0.0109(2) 0.0109(2) 0.0107(2) -0.00002(12) 0.00002(12) 0.0060(3) O1 0.032(3) 0.023(3) 0.015(2) -0.0001(17) 0.001(2) 0.018(3) O2 0.024(3) 0.016(3) 0.0156(19) -0.0037(18) -0.0003(16) 0.011(2) O3 0.025(3) 0.020(2) 0.023(2) 0.0063(19) -0.0002(18) 0.015(2) O4 0.029(4) 0.016(3) 0.017(2) 0.001(2) 0.004(2) 0.014(3) S1 0.0113(7) 0.0145(7) 0.0109(5) -0.0006(5) 0.0002(6) 0.0071(7) O5 0.023(4) 0.023(4) 0.116(9) 0.013(3) -0.013(3) 0.003(4) Na1 0.018(3) 0.0268(17) 0.0209(16) -0.0006(9) -0.0011(17) 0.0088(13) _data_global _publ_section_title ; Synthesis, structure and catalytic properties of rare-earth ternary sulfates ; loop_ _publ_author_name 'Josefina Perles' 'Carlos Fortes-Revilla' 'Enrique Gutierrez-Puebla' 'Marta Iglesias' 'M. \'Angeles Monge' 'Caridad Ruiz-Valero' 'Natalia Snejko' _chemical_formula_sum 'H2 Gd Na O9 S2' _chemical_formula_weight 390.38 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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P3(2)21 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' _cell_length_a 6.8816(6) _cell_length_b 6.8816(6) _cell_length_c 12.7702(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 523.73(10) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3792 _cell_measurement_theta_min 3.77 _cell_measurement_theta_max 31.17 _exptl_crystal_description hexagonal _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 3.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 543 _exptl_absorpt_coefficient_mu 10.181 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.1851 _exptl_absorpt_correction_T_max 0.8223 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3759 _diffrn_reflns_av_R_equivalents 0.0954 _diffrn_reflns_av_sigmaI/netI 0.1050 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 31.17 _reflns_number_total 1068 _reflns_number_gt 874 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(5) _refine_ls_number_reflns 1068 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 2.835 _refine_ls_shift/su_mean 0.305 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 _atom_site_disorder_assembly _atom_site_disorder_group 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) _data_global _publ_section_title ; Synthesis, structure and catalytic properties of rare-earth ternary sulfates ; loop_ _publ_author_name 'Josefina Perles' 'Carlos Fortes-Revilla' 'Enrique Gutierrez-Puebla' 'Marta Iglesias' 'M. \'Angeles Monge' 'Caridad Ruiz-Valero' 'Natalia Snejko' _chemical_formula_sum 'H2 Na Nd O9 S2' _chemical_formula_weight 377.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Nd' 'Nd' -0.1943 3.0179 '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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'y, x, -z' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' _cell_length_a 6.968(2) _cell_length_b 6.968(2) _cell_length_c 12.856(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 540.6(4) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4128 _cell_measurement_theta_min 3.73 _cell_measurement_theta_max 31.01 _exptl_crystal_description octahedron _exptl_crystal_colour mauve _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 531 _exptl_absorpt_coefficient_mu 7.866 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.8585 _exptl_absorpt_correction_T_max 0.8585 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4056 _diffrn_reflns_av_R_equivalents 0.0612 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.73 _diffrn_reflns_theta_max 31.01 _reflns_number_total 1099 _reflns_number_gt 999 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0132P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0046(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 1099 _refine_ls_number_parameters 66 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.650 _refine_ls_shift/su_mean 0.051 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 _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.56586(7) 0.56586(7) 1.0000 0.00792(12) Uani 1 2 d S . . O1 O 0.4922(7) 0.3592(7) 0.8280(2) 0.0142(9) Uani 1 1 d . . . O2 O 0.6120(6) 0.7397(6) 0.8222(3) 0.0168(9) Uani 1 1 d . . . O3 O 0.4111(6) 0.1660(6) 1.0284(3) 0.0145(9) Uani 1 1 d . . . O4 O 0.4954(7) 0.8772(8) 1.0156(3) 0.0146(10) Uani 1 1 d . . . S1 S 0.5585(2) 0.5458(2) 0.75580(7) 0.0089(2) Uani 1 1 d . . . O5 O 0.9234(12) 0.9234(12) 1.0000 0.049(3) Uani 1 2 d S . . Na1 Na 1.0000 0.4691(5) 0.1667 0.0203(7) Uani 1 2 d S . . H1 H 1.019(11) 0.924(15) 1.046(5) 0.04(2) 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 Nd1 0.00920(18) 0.00920(18) 0.00588(14) 0.00018(10) -0.00018(10) 0.0050(3) O1 0.022(3) 0.0106(19) 0.0094(15) -0.0004(13) 0.0003(16) 0.0074(19) O2 0.024(2) 0.016(2) 0.0133(14) -0.0069(15) -0.0020(14) 0.012(2) O3 0.019(2) 0.014(2) 0.0152(16) 0.0054(14) -0.0022(14) 0.0122(17) O4 0.020(3) 0.014(3) 0.0122(14) -0.0013(17) 0.0062(17) 0.010(2) S1 0.0100(6) 0.0118(6) 0.0064(4) 0.0001(4) 0.0005(5) 0.0064(6) O5 0.015(3) 0.015(3) 0.111(8) 0.013(3) -0.013(3) 0.002(4) Na1 0.015(2) 0.0254(15) 0.0169(12) 0.0002(7) 0.0004(15) 0.0077(11)