V2O5/SiO2 surface inspired, silsesquioxane-derived oxovanadium complexes and their properties
Ohde, Christian; Brandt, Marcus; Limberg, Christian; Döbler, Jens; Ziemer, Burckhard; Sauer, Joachim; Dalton Transactions  (2008) 326–; doi:10.1039/b714933f

data_7003255
_publ_section_title
;
 V2O5/SiO2 surface inspired, silsesquioxane-derived oxovanadium
 complexes and their properties
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              326
_journal_paper_doi               10.1039/b714933f
_journal_year                    2008
_chemical_formula_moiety         'C35 H64 O14 Si7 V, C24 H20 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C61 H88 Cl4 O14 P Si7 V'
_chemical_formula_weight         1465.65
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.33(3)
_cell_angle_beta                 88.66(3)
_cell_angle_gamma                85.85(3)
_cell_formula_units_Z            2
_cell_length_a                   10.292(3)
_cell_length_b                   14.543(4)
_cell_length_c                   24.244(6)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      5.0
_cell_volume                     3614.6(17)
_computing_cell_refinement       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_collection       'IPDS2.87 (Stoe & Cie, 1997)'
_computing_data_reduction        'IPDS2.87 (Stoe & Cie, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.667
_diffrn_measured_fraction_theta_full 0.934
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device       'Stoe IPDS diffractometer'
_diffrn_measurement_method       '\f-oscill.,\f-incr.=1.2\%,200 exposures'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0947
_diffrn_reflns_av_sigmaI/netI    0.1718
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21258
_diffrn_reflns_theta_full        24.16
_diffrn_reflns_theta_max         24.16
_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    0.482
_exptl_absorpt_correction_T_max  0.9625
_exptl_absorpt_correction_T_min  0.7948
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
The correction was carried out by ABSCOR (Stoe, 1997), a modification of
DIFABS (Walker, N. & Stuart, D. (1983). Acta Cryst. A39, 158-166.
In contrary to DIFABS, ABSCOR loads F^2^ values instead of F ones.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             1540
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         10790
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.2055
_refine_ls_R_factor_gt           0.1085
_refine_ls_shift/su_max          0.095
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1618P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2673
_refine_ls_wR_factor_ref         0.3183
_reflns_number_gt                3992
_reflns_number_total             10790
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b714933f.txt
_cod_data_source_block           c:\ziemer\co-20\ohde9
_cod_database_code               7003255