Oxovanadium(IV) Silsesquioxane Complexes
Christian Ohde; Christian Limberg; Reinhard Stösser; Serhiy Demeshko; Inorganic Chemistry 49 (2010) 2479–2485; doi:10.1021/ic902392y

data_4315080
_publ_section_title
;
 Oxovanadium(IV) Silsesquioxane Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2479
_journal_page_last               2485
_journal_paper_doi               10.1021/ic902392y
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C78 H142 O29 Si14 V3'
_chemical_formula_sum            'C78 H142 O29 Si14 V3'
_chemical_formula_weight         2090.00
_chemical_name_systematic
; 
 Tetradecacyclopentyl-bis(silsesquioxane)-tri(oxovanadium)
bis(tetrahydrofuran)-adduct 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   25.9729(5)
_cell_length_b                   19.5740(4)
_cell_length_c                   20.5865(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     10466.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0611
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21820
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.492
_exptl_absorpt_correction_T_max  0.8911
_exptl_absorpt_correction_T_min  0.8585
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    none
_exptl_crystal_description       cube
_exptl_crystal_F_000             4428
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_platon_squeeze_details
;
;
_refine_diff_density_max         0.590
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.266
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         9455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.266
_refine_ls_R_factor_all          0.1173
_refine_ls_R_factor_gt           0.1052
_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^)+132.2490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2268
_refine_ls_wR_factor_ref         0.2309
_reflns_number_gt                8133
_reflns_number_total             9455
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic902392y_si_001_1.cif
_cod_data_source_block           chris102
_cod_database_code               4315080