Refinement of the layered titanosilicate AM-1 from single-crystal X-ray diffraction data
Ferdov, Stanislav; Kolitsch, Uwe; Lengauer, Christian; Tillmanns, Ekkehart; Lin, Zhi; Sá Ferreira, Rute A.; Acta Crystallographica Section E 63 (2007) i186–i186; doi:10.1107/S160053680704812X

data_2215786
_publ_section_title
;
 Refinement of the layered titanosilicate AM-1 from single-crystal
 X-ray diffraction data
;
_journal_coeditor_code           BR2055
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i186
_journal_page_last               i186
_journal_paper_doi               10.1107/S160053680704812X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'Na4 Ti2 Si8 O22, 4H2 O'
_chemical_formula_sum            'H4 Na2 O13 Si4 Ti'
_chemical_formula_weight         418.27
_chemical_name_common            'sodium titanium silicate'
_chemical_name_systematic
;
disodium titanium tetrasilicate dihydrate
;
_space_group_IT_number           90
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4ab 2ab'
_symmetry_space_group_name_H-M   'P 4 21 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     isomor
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.3740(10)
_cell_length_b                   7.3740(10)
_cell_length_c                   10.709(2)
_cell_measurement_reflns_used    901
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.037
_cell_volume                     582.31(16)
_computing_cell_refinement       'SCALEPACK (Otwinowski <i>et al.</i>,  2003)'
_computing_data_collection       'COLLECT (Nonius, 2003)'
_computing_data_reduction
'SCALEPACK and DENZO (Otwinowski <i>et al.</i>,  2003)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            1399
_diffrn_reflns_theta_full        27.84
_diffrn_reflns_theta_max         27.84
_diffrn_reflns_theta_min         3.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.290
_exptl_absorpt_correction_T_max  0.9872
_exptl_absorpt_correction_T_min  0.9151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(SCALEPACK; Otwinowski <i>et al.</i>,  2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.351
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_coef       0.006(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     54
_refine_ls_number_reflns         706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0245
_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^)+(0.03P)^2^+0.065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0606
_reflns_number_gt                631
_reflns_number_total             706
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br2055.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P4 21 2'
_cod_database_code               2215786
_cod_database_fobs_code          2215786