Salt-Templated Mesoporous Solids Comprised of Interlinked Polyoxovanadate Clusters
Wendy L. Queen; Shiou-Jyh Hwu; Shane Reighard; Inorganic Chemistry 49 (2010) 1316–1318; doi:10.1021/ic902283g

data_4314897
_publ_contact_author_address
;Department of Chemistry

Clemson University

Clemson, SC  29634-0973 

USA

;
_publ_contact_author_email       shwu@clemson.edu
_publ_contact_author_name        'Shiou-Jyh Hwu'
_publ_contact_author_phone       864-656-5031
_publ_section_title
;
 Salt-Templated Mesoporous Solids Comprised of Interlinked Polyoxovanadate
 Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1316
_journal_page_last               1318
_journal_paper_doi               10.1021/ic902283g
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'As2 Cl0.99 Cs3.88 Na0.12 O16.6 V4.6'
_chemical_formula_weight         1203.46
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           227
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_atom_sites_solution_hydrogens   none
_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            48
_cell_length_a                   32.957(4)
_cell_length_b                   32.957(4)
_cell_length_c                   32.957(4)
_cell_measurement_reflns_used    1540
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.14
_cell_volume                     35797(8)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;

scan:

    Number of images: 360

               Slice: -90.0000 - 90.0000

         Image width: 0.5000

            Exp time: 200.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 45.0000

                 Phi: 0.0000

                 XTD: 27.5840

              2theta: -0.2029

scan:

    Number of images: 120

               Slice: -30.0000 - 30.0000

         Image width: 0.5000

            Exp time: 200.0000

       Rotation axis: Omega

               Omega: 0.0000

                 Chi: 45.0000

                 Phi: 90.0000

                 XTD: 27.5840

              2theta: -0.2029

;
_diffrn_measurement_device_type  'Rigaku AFC8S'
_diffrn_measurement_method       '\w scans'
_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  0.0980
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            14654
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.398
_exptl_absorpt_correction_T_max  0.7300
_exptl_absorpt_correction_T_min  0.6788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB, CrystalClear'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.680
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             25739
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.703
_refine_diff_density_min         -2.149
_refine_diff_density_rms         0.378
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.1055
_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^)+(0.1990P)^2^+3585.0071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2604
_refine_ls_wR_factor_ref         0.3310
_reflns_number_gt                955
_reflns_number_total             1540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902283g_si_002_2.cif
_cod_data_source_block           Cs3.88Na0.12(V4.6O8.6)(AsO4)2Cl0.99
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi scan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        35797(7)
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_original_formula_sum        'As2 Cl0.99 Cs3.88 Na0.12 O16.60 V4.60'
_cod_database_code               4314897