#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/2/21/44/2214419.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_2214419 loop_ _publ_author_name 'Abdelhedi, Mohamed' 'Ktari, Lilia' 'Dammak, Mohamed' 'Cousson, Alain' 'Kolsi, Abdelwaheb' _publ_section_title ; K~2~(SO~4~)~0.63~(SeO~4~)~0.37~·Te(OH)~6~ ; _journal_coeditor_code WM2119 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i153 _journal_page_last i154 _journal_paper_doi 10.1107/S1600536807027705 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac 'K2 (S O4)0.63 (Se O4)0.37 Te (O H)6' _chemical_formula_moiety 'H6 O6 Te, O4 S0.63 Se0.37, 2(K)' _chemical_formula_sum 'H6 K2 O10 S0.63 Se0.37 Te' _chemical_formula_weight 421.16 _chemical_name_systematic 'Dipotassium sulfate/selenate tellurate' _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method CRYSTALS_ver_12.51 _cell_angle_alpha 102.138(2) _cell_angle_beta 90.073(2) _cell_angle_gamma 116.9430(10) _cell_formula_units_Z 2 _cell_length_a 6.2463(2) _cell_length_b 6.6470(2) _cell_length_c 13.1326(4) _cell_measurement_reflns_used 7138 _cell_measurement_temperature 298 _cell_measurement_theta_max 30.1 _cell_measurement_theta_min 2.7 _cell_volume 472.28(3) _computing_cell_refinement DENZO/SCALEPACK _computing_data_collection 'COLLECT (Nonius, 2001)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg & Berndt, 1999)' _computing_publication_material CRYSTALS _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f rotation scans with 2\% width' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 69116 _diffrn_reflns_theta_full 29.571 _diffrn_reflns_theta_max 30.174 _diffrn_reflns_theta_min 1.596 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.63 _exptl_absorpt_correction_T_max 0.569 _exptl_absorpt_correction_T_min 0.447 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(MULABS in PLATON; Spek, 2003)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.961 _exptl_crystal_description prism _exptl_crystal_F_000 397.250 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _refine_diff_density_max 2.40 _refine_diff_density_min -2.99 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0914 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 114 _refine_ls_number_reflns 1719 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0448 _refine_ls_shift/su_max 0.0019 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, [Watkin (1994). Acta Cryst. A50, 411--437; Prince, (1982). Mathematical Techniques in Crystallography and Materials Science. Springer-Verlag: New York.] [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 4.11 -3.38 2.64 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0508 _refine_ls_wR_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0508 _reflns_number_gt 1719 _reflns_number_total 2787 _reflns_threshold_expression I>3\s(I) _cod_data_source_file wm2119.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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 'Triclinic' changed to 'triclinic' 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_formula_sum 'H6 K2 O10 S0.63 Se0.37 Te1' _cod_database_code 2214419 _cod_database_fobs_code 2214419 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_site_type_symbol _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_occupancy Te Te1 0.0000 0.0000 0.0000 0.0150 Uani 1.0000 Te Te2 0.5000 0.0000 0.5000 0.0144 Uani 1.0000 Se Se1 -0.24991(17) 0.46625(17) 0.24814(17) 0.0439 Uani 0.368(7) S S1 -0.24991(17) 0.46625(17) 0.24814(17) 0.0439 Uani 0.632(7) K K1 0.1921(4) 0.2576(3) 0.35079(18) 0.0274 Uani 1.0000 K K2 0.4207(4) -0.2342(3) 0.14873(17) 0.0254 Uani 1.0000 O O1 -0.0604(11) -0.0373(10) 0.1399(5) 0.0232 Uani 1.0000 O O2 -0.1770(12) 0.1704(11) 0.0061(5) 0.0251 Uani 1.0000 O O3 0.2905(11) 0.2817(10) 0.0548(6) 0.0269 Uani 1.0000 O O4 0.7680(10) -0.0037(10) 0.4321(5) 0.0250 Uani 1.0000 O O5 0.6055(11) 0.3137(9) 0.4891(5) 0.0215 Uani 1.0000 O O6 0.3083(10) -0.1107(10) 0.3668(5) 0.0233 Uani 1.0000 O O7 -0.1044(11) 0.4714(11) 0.3412(5) 0.0260 Uani 1.0000 O O8 -0.3641(13) 0.6150(12) 0.2807(6) 0.0281 Uani 1.0000 O O9 -0.0842(12) 0.5509(12) 0.1687(6) 0.0312 Uani 1.0000 O O10 -0.4411(12) 0.2270(10) 0.2057(6) 0.0301 Uani 1.0000 H H1 -0.0693 -0.1671 0.1452 0.0436 Uiso 1.0000 H H2 -0.1419 0.2746 0.0589 0.0436 Uiso 1.0000 H H3 0.3657 0.2491 0.0937 0.0436 Uiso 1.0000 H H4 0.7229 -0.1343 0.3896 0.0436 Uiso 1.0000 H H5 0.6985 0.3395 0.4404 0.0436 Uiso 1.0000 H H6 0.1875 -0.2315 0.3702 0.0436 Uiso 1.0000 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 Te1 0.01489(9) 0.01533(9) 0.01406(9) 0.00653(9) 0.00131(9) 0.00335(9) Te2 0.01472(9) 0.01349(9) 0.01512(9) 0.00649(9) 0.00155(9) 0.00350(9) Se1 0.03752(17) 0.04897(17) 0.03836(17) 0.01470(17) 0.00249(17) 0.00931(17) S1 0.03752(17) 0.04897(17) 0.03836(17) 0.01470(17) 0.00249(17) 0.00931(17) K1 0.0242(8) 0.0260(8) 0.0370(11) 0.0156(7) 0.0043(7) 0.0079(7) K2 0.0244(8) 0.0227(8) 0.0346(10) 0.0146(7) 0.0013(7) 0.0093(7) O1 0.033(3) 0.025(3) 0.016(3) 0.015(2) 0.007(2) 0.009(2) O2 0.031(3) 0.028(3) 0.024(3) 0.022(3) 0.000(2) 0.003(2) O3 0.025(3) 0.016(2) 0.035(4) 0.004(2) -0.007(2) 0.008(2) O4 0.019(3) 0.020(3) 0.032(3) 0.008(2) 0.008(2) 0.001(2) O5 0.026(3) 0.013(2) 0.026(3) 0.009(2) 0.006(2) 0.006(2) O6 0.024(3) 0.019(3) 0.020(3) 0.004(2) -0.004(2) 0.006(2) O7 0.023(3) 0.031(3) 0.028(3) 0.011(2) 0.000(2) 0.017(3) O8 0.036(4) 0.032(3) 0.029(4) 0.029(3) 0.006(3) 0.001(3) O9 0.032(3) 0.030(3) 0.033(4) 0.013(3) 0.006(3) 0.012(3) O10 0.031(3) 0.016(3) 0.038(4) 0.007(2) -0.005(3) 0.005(2) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H 0.0000 0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4' K 0.2009 0.2494 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Se -0.0929 2.2259 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Te -0.5308 1.6751 'International Tables Vol C 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 Te1 O3 2_555 2_555 89.9(3) ? O1 Te1 O2 2_555 2_555 91.2(3) ? O3 Te1 O2 2_555 2_555 90.4(3) ? O1 Te1 O1 2_555 . 179.994 no O3 Te1 O1 2_555 . 90.1(3) ? O2 Te1 O1 2_555 . 88.8(3) ? O1 Te1 O2 2_555 . 88.8(3) ? O3 Te1 O2 2_555 . 89.6(3) ? O2 Te1 O2 2_555 . 179.994 no O1 Te1 O2 . . 91.2(3) ? O1 Te1 O3 2_555 . 90.1(3) ? O3 Te1 O3 2_555 . 179.994 no O2 Te1 O3 2_555 . 89.6(3) ? O1 Te1 O3 . . 89.9(3) ? O2 Te1 O3 . . 90.4(3) ? O6 Te2 O5 2_656 2_656 89.6(3) ? O6 Te2 O4 2_656 2_656 90.4(3) ? O5 Te2 O4 2_656 2_656 90.0(3) ? O6 Te2 O4 2_656 . 89.6(3) ? O5 Te2 O4 2_656 . 90.0(3) ? O4 Te2 O4 2_656 . 179.994 no O6 Te2 O5 2_656 . 90.4(3) ? O5 Te2 O5 2_656 . 179.994 no O4 Te2 O5 2_656 . 90.0(3) ? O4 Te2 O5 . . 90.0(3) ? O6 Te2 O6 2_656 . 179.994 no O5 Te2 O6 2_656 . 90.4(3) ? O4 Te2 O6 2_656 . 89.6(3) ? O4 Te2 O6 . . 90.4(3) ? O5 Te2 O6 . . 89.6(3) ? O7 X1 O8 . . 109.8(4) ? O7 X1 O9 . . 108.3(4) ? O8 X1 O9 . . 110.1(4) ? O7 X1 O10 . . 109.3(4) ? O8 X1 O10 . . 108.4(4) ? O9 X1 O10 . . 111.0(4) ? Te1 O1 H1 . . 109.426 no Te1 O2 H2 . . 114.986 no Te1 O3 H3 . . 105.734 no Te2 O4 H4 . . 109.438 no Te2 O5 H5 . . 108.396 no Te2 O6 H6 . . 106.016 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 Te1 O1 2_555 1.920(6) yes Te1 O3 2_555 1.915(6) yes Te1 O2 2_555 1.900(6) yes Te1 O1 . 1.920(6) yes Te1 O2 . 1.900(6) yes Te1 O3 . 1.915(6) yes Te2 O6 2_656 1.921(6) yes Te2 O5 2_656 1.919(5) yes Te2 O4 2_656 1.905(6) yes Te2 O4 . 1.905(6) yes Te2 O5 . 1.919(5) yes Te2 O6 . 1.921(6) yes X1 O7 . 1.508(6) yes X1 O8 . 1.460(7) yes X1 O9 . 1.482(7) yes X1 O10 . 1.473(6) yes O1 H1 . 0.857 no O2 H2 . 0.817 no O3 H3 . 0.817 no O4 H4 . 0.848 no O5 H5 . 0.856 no O6 H6 . 0.826 no K1 O4 1_455 2.792(6) yes K1 O7 . 2.815(6) yes K1 O5 2_666 2.889(6) yes K1 O6 . 2.897(6) yes K1 O1 . 2.984(7) yes K1 O5 . 2.990(6) yes K1 O8 1_655 3.022(8) yes K1 O10 1_655 3.032(8) yes K2 O10 1_655 2.709(6) yes K2 O2 2_555 2.751(6) yes K2 O8 1_645 2.786(8) yes K2 O9 1_545 2.852(7) yes K2 O1 1_655 2.908(7) yes K2 O3 1_545 2.915(6) yes K2 O6 . 2.984(7) yes K2 O3 2_655 3.267(8) yes 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 O1 H1 O9 1_545 0.857(6) 1.924(7) 2.780(9) 175.6(5) yes O2 H2 O9 . 0.817(6) 1.967(7) 2.773(10) 168.7(5) yes O3 H3 O10 1_655 0.817(6) 1.972(7) 2.778(9) 169.1(5) yes O4 H4 O8 1_645 0.848(6) 1.815(7) 2.654(9) 169.7(5) yes O5 H5 O7 1_655 0.856(6) 1.868(6) 2.701(9) 164.3(4) yes O6 H6 O7 1_545 0.826(6) 1.946(6) 2.755(8) 166.0(5) yes