Open-Framework and Microporous Vanadium Silicates
Xiqu Wang; Lumei Liu; Allan J. Jacobson; Journal of the American Chemical Society 124 (2002) 7812–7820; doi:10.1021/ja020354l

data_4114914
_publ_contact_author_address
;
Department of Chemistry    
University of Houston,
Houston, TX 77204-5003
;
_publ_contact_author_email       ' ajjcob@uh.edu '
_publ_contact_author_fax         ' 713 743 2787 '
_publ_contact_author_name
;
Prof. Allan J. Jacobson
;
_publ_contact_author_phone       ' 713 743 2785 '
_publ_section_title
;
 Open-Framework and Microporous Vanadium Silicates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7812
_journal_page_last               7820
_journal_paper_doi               10.1021/ja020354l
_journal_volume                  124
_journal_year                    2002
_chemical_formula_sum            'Cs1.33 H4.8 K0.67 O13.4 Si4 V'
_chemical_formula_weight         585.82
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   IGNORED
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.110(15)
_cell_length_b                   13.110(15)
_cell_length_c                   14.35(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2136(5)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SIEMENS SMART/CCD'
_diffrn_measurement_method       'NARROW FRAME, 0.3w'
_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  0.1074
_diffrn_reflns_av_sigmaI/netI    0.0765
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5222
_diffrn_reflns_theta_full        22.47
_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    4.650
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5778
_exptl_absorpt_correction_type   'multi-scan  (SADABS)'
_exptl_crystal_colour            BLUE-GREEN
_exptl_crystal_density_diffrn    2.733
_exptl_crystal_description       POLYHEDRON
_exptl_crystal_F_000             1662
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.839
_refine_diff_density_min         -1.560
_refine_diff_density_rms         0.471
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.16(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   2.424
_refine_ls_hydrogen_treatment    NA
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1260
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      2.421
_refine_ls_R_factor_all          0.1788
_refine_ls_R_factor_gt           0.1420
_refine_ls_shift/su_max          2.051
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3276
_refine_ls_wR_factor_ref         0.3474
_reflns_number_gt                926
_reflns_number_total             1260
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja020354l_05.cif
_cod_data_source_block           VSH-6CsK
_cod_original_formula_sum        'H4.80 Cs1.33 K0.67 O13.40 Si4 V'
_cod_database_code               4114914