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_7003254
_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         'C102 H166 O32 Si18 V2'
_chemical_formula_sum            'C102 H166 O32 Si18 V2'
_chemical_formula_weight         1255.92
_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                77.43(3)
_cell_angle_beta                 77.90(3)
_cell_angle_gamma                67.34(3)
_cell_formula_units_Z            1
_cell_length_a                   13.076(4)
_cell_length_b                   14.748(3)
_cell_length_c                   18.540(5)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      22.0
_cell_measurement_theta_min      5.0
_cell_volume                     3188.7(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_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  0.1061
_diffrn_reflns_av_sigmaI/netI    0.1512
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20620
_diffrn_reflns_theta_full        23.21
_diffrn_reflns_theta_max         23.21
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  0.9338
_exptl_absorpt_correction_T_min  0.8610
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         8447
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1740
_refine_ls_R_factor_gt           0.0948
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1434P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2591
_reflns_number_gt                3804
_reflns_number_total             8447
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b714933f.txt
_cod_data_source_block           MAN?
_cod_original_cell_volume        3188.7(15)
_cod_database_code               7003254