#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100777.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_1100777 _publ_requested_journal 'Inorganic Chemistry' _publ_section_title ; The Reaction between ZnO and Molten Na~2~S~2~O~7~ or K~2~S~2~O~7~ forming Na~2~Zn(SO~4 ~)~2~ or K~2~Zn(SO~4~)~2~, studied by Raman Spectroscopy and X-ray Diffraction ; _chemical_formula_moiety 'Na2 O8 S2 Zn' _chemical_formula_sum 'Na2 O8 S2 Zn' _chemical_formula_weight 303.47 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' '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 2/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 8.648(3) _cell_length_b 10.323(3) _cell_length_c 15.103(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.879(6) _cell_angle_gamma 90.00 _cell_volume 1348.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 923 _cell_measurement_theta_min 3.342 _cell_measurement_theta_max 28.627 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.991 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 4.401 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3519 _exptl_absorpt_correction_T_max 0.9573 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2000)' _diffrn_ambient_temperature 295(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 'Siemens/Bruker SMART 1K' _diffrn_measurement_method 'omega scan, frame data integration' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13993 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.36 _reflns_number_total 2748 _reflns_number_gt 1741 _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^)+(0.0399P)^2^+0.3988P] 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_number_reflns 2748 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0758 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Zn1 Zn 0.58357(6) 0.61983(5) 0.12303(3) 0.01704(16) Uani 1 1 d . . . Zn2 Zn 1.07368(6) 0.87539(5) 0.12374(3) 0.01721(17) Uani 1 1 d . . . S1 S 0.92734(13) 0.60864(11) 0.15714(7) 0.0139(3) Uani 1 1 d . . . S2 S 0.92296(13) 1.12960(11) 0.09012(7) 0.0160(3) Uani 1 1 d . . . S3 S 0.43586(13) 0.88941(11) 0.15759(7) 0.0141(3) Uani 1 1 d . . . S4 S 0.43670(13) 0.37216(11) 0.09497(7) 0.0156(3) Uani 1 1 d . . . Na1 Na 0.2500 0.1589(3) 0.2500 0.0301(7) Uani 1 2 d S . . Na2 Na 0.8023(2) 0.39753(18) -0.01361(12) 0.0252(5) Uani 1 1 d . . . Na3 Na 1.2500 0.5798(3) 0.2500 0.0286(7) Uani 1 2 d S . . Na4 Na 0.3021(2) 0.10596(19) 0.01832(13) 0.0306(5) Uani 1 1 d . . . Na5 Na 0.7500 1.0048(3) 0.2500 0.0357(8) Uani 1 2 d S . . Na6 Na 0.7500 0.3458(3) 0.2500 0.0491(10) Uani 1 2 d S . . O1 O 0.7947(4) 0.6968(3) 0.1471(2) 0.0216(8) Uani 1 1 d . . . O2 O 0.5726(4) 0.5452(3) 0.2555(2) 0.0201(8) Uani 1 1 d . . . O3 O 0.9287(4) 0.5127(3) 0.0885(2) 0.0293(9) Uani 1 1 d . . . O4 O 1.0698(3) 0.6873(3) 0.1523(2) 0.0162(7) Uani 1 1 d . . . O5 O 0.8991(4) 0.9850(3) 0.0856(2) 0.0198(7) Uani 1 1 d . . . O6 O 0.8280(4) 1.1802(3) 0.1595(2) 0.0230(8) Uani 1 1 d . . . O7 O 1.0851(4) 1.1552(3) 0.1054(2) 0.0261(8) Uani 1 1 d . . . O8 O 1.1289(4) 0.8177(3) -0.0035(2) 0.0274(9) Uani 1 1 d . . . O9 O 0.4154(4) 0.7475(3) 0.1486(2) 0.0206(8) Uani 1 1 d . . . O10 O 1.2830(4) 0.9494(3) 0.1473(2) 0.0291(9) Uani 1 1 d . . . O11 O 0.5382(4) 0.9405(3) 0.0933(2) 0.0327(9) Uani 1 1 d . . . O12 O 1.0037(4) 0.9209(3) 0.2541(2) 0.0296(9) Uani 1 1 d . . . O13 O 0.6010(4) 0.6799(3) -0.0067(2) 0.0248(8) Uani 1 1 d . . . O14 O 0.5967(4) 0.4268(3) 0.0929(2) 0.0230(8) Uani 1 1 d . . . O15 O 0.3350(4) 0.4800(3) 0.1158(2) 0.0269(9) Uani 1 1 d . . . O16 O 0.4268(4) 0.2705(3) 0.1591(2) 0.0284(9) Uani 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 Zn1 0.0170(3) 0.0164(3) 0.0177(3) -0.0030(2) 0.0006(2) 0.0012(2) Zn2 0.0181(3) 0.0156(3) 0.0179(3) 0.0009(2) -0.0006(2) 0.0021(2) S1 0.0136(6) 0.0163(7) 0.0117(6) 0.0002(5) 0.0009(5) -0.0026(5) S2 0.0189(7) 0.0159(7) 0.0134(6) 0.0004(5) 0.0029(5) 0.0047(5) S3 0.0138(6) 0.0148(6) 0.0140(6) 0.0012(5) 0.0033(5) 0.0007(5) S4 0.0211(7) 0.0130(6) 0.0126(6) 0.0004(5) 0.0006(5) -0.0011(5) Na1 0.0393(18) 0.0290(17) 0.0223(16) 0.000 0.0126(14) 0.000 Na2 0.0317(12) 0.0243(12) 0.0196(10) -0.0032(8) 0.0000(9) 0.0086(9) Na3 0.0258(16) 0.0406(19) 0.0194(15) 0.000 -0.0008(13) 0.000 Na4 0.0348(12) 0.0275(12) 0.0299(11) -0.0057(9) 0.0168(10) -0.0067(9) Na5 0.0245(17) 0.0322(19) 0.051(2) 0.000 0.0145(15) 0.000 Na6 0.091(3) 0.0189(18) 0.0379(19) 0.000 0.0305(19) 0.000 O1 0.0161(18) 0.025(2) 0.0241(19) 0.0063(15) -0.0013(15) 0.0028(14) O2 0.026(2) 0.0184(19) 0.0159(17) -0.0048(13) 0.0057(15) -0.0014(14) O3 0.037(2) 0.029(2) 0.0213(19) -0.0110(15) 0.0019(17) -0.0044(17) O4 0.0128(17) 0.0137(18) 0.0221(17) 0.0027(14) 0.0038(14) -0.0018(13) O5 0.0235(18) 0.0153(18) 0.0206(18) 0.0009(14) 0.0011(15) 0.0035(14) O6 0.028(2) 0.025(2) 0.0170(17) -0.0036(15) 0.0071(15) 0.0076(15) O7 0.0203(19) 0.028(2) 0.030(2) 0.0000(16) 0.0040(16) -0.0011(15) O8 0.041(2) 0.027(2) 0.0143(18) 0.0022(15) 0.0019(17) 0.0164(16) O9 0.021(2) 0.0147(19) 0.0256(18) 0.0023(14) 0.0035(15) 0.0000(14) O10 0.024(2) 0.021(2) 0.043(2) -0.0004(16) -0.0070(17) 0.0043(15) O11 0.038(2) 0.026(2) 0.035(2) -0.0019(17) 0.0239(18) -0.0072(17) O12 0.040(2) 0.033(2) 0.0162(18) 0.0001(16) -0.0068(17) 0.0135(18) O13 0.038(2) 0.022(2) 0.0144(18) -0.0046(14) -0.0003(16) -0.0075(16) O14 0.0214(19) 0.0220(19) 0.0256(19) -0.0070(15) 0.0061(15) -0.0060(15) O15 0.029(2) 0.026(2) 0.025(2) -0.0054(15) -0.0033(16) 0.0099(16) O16 0.038(2) 0.023(2) 0.025(2) 0.0093(16) 0.0065(18) -0.0008(17) _cod_database_code 1100777