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_2108333
_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                 90.056(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.364(4)
_cell_length_b                   9.134(3)
_cell_length_c                   10.373(3)
_cell_measurement_reflns_used    5566
_cell_measurement_temperature    304(2)
_cell_measurement_theta_max      21.03
_cell_measurement_theta_min      1.6
_cell_volume                     1360.9(7)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      304(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5566
_diffrn_reflns_point_group_measured_fraction_full 0.680
_diffrn_reflns_point_group_measured_fraction_max 0.680
_diffrn_reflns_theta_full        21.033
_diffrn_reflns_theta_max         21.033
_diffrn_reflns_theta_min         2.230
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.115
_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   0.7452
_exptl_transmission_factor_min   0.5870
_refine_diff_density_max         1.338
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.230
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.029(5)
_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   1.046
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1997
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.088
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1458P)^2^+32.8662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2457
_refine_ls_wR_factor_ref         0.2629
_reflns_Friedel_coverage         0.284
_reflns_Friedel_fraction_full    0.328
_reflns_Friedel_fraction_max     0.328
_reflns_number_gt                1679
_reflns_number_total             1997
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5030sup1.cif
_cod_data_source_block           II
_cod_database_code               2108333
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              33377
_shelx_hkl_checksum              71342