#------------------------------------------------------------------------------ #$Date: 2016-02-16 20:30:59 +0000 (Tue, 16 Feb 2016) $ #$Revision: 176467 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/00/4000093.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_4000093 _journal_name_full 'Chemistry of Materials' _journal_year 2001 _chemical_formula_sum 'H17 Na8 O47.5 Si12 Ti5' _chemical_formula_weight 1537.64 _space_group_IT_number 65 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-C 2 2' _symmetry_space_group_name_H-M 'C m m m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 1 _cell_length_a 23.2272(4) _cell_length_b 7.1751(11) _cell_length_c 6.9727(6) _cell_measurement_reflns_used ? _cell_measurement_temperature 293(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 1162.1(2) _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _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 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 981 _diffrn_reflns_theta_max 24.93 _diffrn_reflns_theta_min 4.85 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 1.334 _exptl_absorpt_correction_T_max 0.9868 _exptl_absorpt_correction_T_min 0.9008 _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 2.197 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 763 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 83 _refine_ls_number_reflns 582 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.119 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_gt 0.0677 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1593 _refine_ls_wR_factor_ref 0.1795 _reflns_number_gt 413 _reflns_number_total 582 _reflns_threshold_expression >2sigma(I) _cod_original_sg_symbol_H-M Cmmm _cod_original_formula_sum 'H17 Na8 O47.50 Si12 Ti5' _cod_database_code 4000093 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 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 Ti1 Ti 0.2500 0.2500 0.5000 0.0172(8) Uani 1 4 d S . . Ti2 Ti 0.0000 0.0000 0.4417(14) 0.016(3) Uani 0.25 4 d SP . . Si1 Si 0.16178(11) 0.5000 0.2304(4) 0.0111(8) Uani 1 2 d S . . Si2 Si 0.0642(2) 0.4050(8) 0.5000 0.0127(12) Uani 0.50 2 d SP . . O1 O 0.1537(4) 0.5000 0.0000 0.019(2) Uani 1 4 d S . . O2 O 0.0955(3) 0.5000 0.3108(11) 0.0236(19) Uani 1 2 d S . . O3 O 0.1934(2) 0.3122(7) 0.2971(7) 0.0199(13) Uani 1 1 d . . . O4 O 0.2199(4) 0.0000 0.5000 0.018(2) Uani 1 4 d S . . O5 O 0.0000 0.5000 0.5000 0.019(3) Uani 1 8 d S . . O6 O 0.0612(7) 0.179(2) 0.5000 0.026(4) Uani 0.50 2 d SP . . O7 O 0.0000 0.0000 0.198(9) 0.039(13) Uani 0.25 4 d SP . . Na1 Na 0.2500 0.2500 0.0000 0.030(3) Uani 0.50 4 d SP . . Na2 Na 0.1400(4) 0.0000 0.2757(14) 0.063(3) Uani 0.75 2 d SP . . O1W O 0.2084(10) 0.058(3) 0.0000 0.056(7) Uani 0.50 2 d SP . . O2W O 0.0812(17) 0.094(7) 0.0000 0.057(13) Uani 0.25 2 d SP . . O5W O 0.473(2) 0.148(10) 0.0000 0.10(2) Uiso 0.25 2 d SP . . O6W O 0.5000 0.0000 0.0000 0.08(3) Uiso 0.25 8 d SP . . 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 Ti1 0.0173(15) 0.0219(17) 0.0124(14) 0.000 0.000 0.0057(11) Ti2 0.017(5) 0.014(5) 0.016(7) 0.000 0.000 0.000 Si1 0.0135(14) 0.0147(15) 0.0052(14) 0.000 -0.0008(10) 0.000 Si2 0.010(3) 0.014(3) 0.015(3) 0.000 0.000 0.001(2) O1 0.023(6) 0.031(6) 0.003(5) 0.000 0.000 0.000 O2 0.013(4) 0.037(5) 0.021(4) 0.000 0.005(3) 0.000 O3 0.024(3) 0.018(3) 0.017(3) 0.001(2) -0.010(2) 0.002(2) O4 0.009(5) 0.015(5) 0.029(6) 0.000 0.000 0.000 O5 0.018(8) 0.025(9) 0.014(8) 0.000 0.000 0.000 O6 0.037(10) 0.020(9) 0.022(9) 0.000 0.000 -0.014(7) O7 0.05(3) 0.01(2) 0.06(4) 0.000 0.000 0.000 Na1 0.042(8) 0.030(8) 0.018(6) 0.000 0.000 0.017(6) Na2 0.089(7) 0.040(5) 0.060(5) 0.000 -0.038(5) 0.000 O1W 0.090(15) 0.037(16) 0.040(11) 0.000 0.000 0.022(10) O2W 0.04(2) 0.09(3) 0.04(2) 0.000 0.000 0.03(2)