The First Framework Solid Composed of Vanadosilicate Clusters
Akhilesh Tripathi; Timothy Hughbanks; Abraham Clearfield; Journal of the American Chemical Society 125 (2003) 10528–10529; doi:10.1021/ja0365173

data_4114115
_publ_contact_author_address
;
Department of Chemistry
Texas A & M University
College Station
Texas 77842-3012
;
_publ_contact_author_email       Clearfield@mail.chem.tamu.edu
_publ_contact_author_fax         '979 845 2370'
_publ_contact_author_name        'Professor Abraham Clearfield'
_publ_contact_author_phone       '979 845 2936'
_publ_section_title
;
 The First Framework Solid Composed of Vanadosilicate Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10528
_journal_page_last               10529
_journal_paper_doi               10.1021/ja0365173
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C8 H16 Ge0 N6.5 O27.5 Si4 V9'
_chemical_formula_weight         1214.09
_chemical_name_common            vanadosilicate
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_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                   16.169(2)
_cell_length_b                   16.169(2)
_cell_length_c                   18.199(4)
_cell_measurement_reflns_used    22345
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.81
_cell_measurement_theta_min      1.26
_cell_volume                     4757.9(13)
_computing_data_reduction        'SHELXTL V5.0 (Sheldrick, 1994)'
_computing_molecular_graphics    'SHELXTL V5.0 (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL V5.0 (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXTL V5.0 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL V5.0 (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 81.92
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Model CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0667
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16354
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    1.863
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.34
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(XPREP in SHELXTL; Bruker, 1997)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2370
_exptl_crystal_size_max          0.058
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.058
_refine_diff_density_max         2.044
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.178
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(3)
_refine_ls_extinction_coef       0.0000(2)
_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   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         2486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.065
_refine_ls_R_factor_gt           0.072
_refine_ls_shift/su_max          1.806
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1164P)^2^+57.0998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1537
_refine_ls_wR_factor_ref         0.1455
_reflns_number_gt                2112
_reflns_number_total             2486
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0365173si20030717_070009.cif
_cod_data_source_block           AT_VGePIP
_cod_original_cell_volume        4758.0(13)
_cod_original_formula_sum        'C8 H16 Ge0 N6.50 O27.50 Si4 V9'
_cod_database_code               4114115