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_4114910
_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            'H3.2 K2 O18.6 Si6 V2'
_chemical_formula_weight         649.45
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   IGNORE
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4936(17)
_cell_length_b                   8.2673(9)
_cell_length_c                   13.1465(15)
_cell_measurement_temperature    293(2)
_cell_volume                     1683.9(3)
_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 0.942
_diffrn_measured_fraction_theta_max 0.942
_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  0.0912
_diffrn_reflns_av_sigmaI/netI    0.1443
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9952
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    2.130
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8290
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            'SKY BLUE'
_exptl_crystal_density_diffrn    2.562
_exptl_crystal_description       POLYHEDRA
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.58(6)
_refine_ls_extinction_coef       0.00042(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_hydrogen_treatment    NA
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         3006
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.858
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0329P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0768
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                1700
_reflns_number_total             3006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja020354l_01.cif
_cod_data_source_block           VSH-3K
_cod_original_formula_sum        'H3.20 K2 O18.60 Si6 V2'
_cod_database_code               4114910