Dehydration of microporous vanadosilicates: the case of VSH-13Na
Danisi, Rosa Micaela; Armbruster, Thomas; Acta Crystallographica Section B 74 (2018) 483–491; doi:10.1107/S2052520618011423

data_2108332
_publ_section_title
;
 Dehydration of microporous vanadosilicates: the case of VSH-13Na
;
_journal_coeditor_code           LO5030SUP1
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              483
_journal_page_last               491
_journal_paper_doi               10.1107/S2052520618011423
_journal_volume                  74
_journal_year                    2018
_chemical_formula_sum            'H0 Na2 O14 Si4 V'
_chemical_formula_weight         433.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90.007(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3328(7)
_cell_length_b                   9.1209(4)
_cell_length_c                   10.3732(5)
_cell_measurement_reflns_used    29173
_cell_measurement_temperature    304(2)
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      1.6
_cell_volume                     1356.07(11)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      304(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29173
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.233
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.6152
_refine_diff_density_max         2.183
_refine_diff_density_min         -2.627
_refine_diff_density_rms         0.306
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.030(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         5549
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1282
_refine_ls_R_factor_gt           0.1095
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1155P)^2^+43.7061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2699
_refine_ls_wR_factor_ref         0.2867
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4686
_reflns_number_total             5549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5030sup1.cif
_cod_data_source_block           I
_cod_database_code               2108332
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              4231
_shelx_hkl_checksum              45432
_cod_database_fobs_code 2108332