Mixed crystals containing the dioxo complex [[Ph3SiO]2VO2]- and novel pentacoordinated oxoperoxo complex [[Ph3SiO]2VO(O2)]-: X-ray crystal structure and assessment as oxidation catalysts.
Vennat, Maxence; Bregeault, Jean-Marie; Herson, Patrick; Dalton transactions (Cambridge, England : 2003)  (2004) 908–913; doi:10.1039/b400657g

data_7014058
_publ_section_title
;
 Mixed crystals containing the dioxo complex [[Ph3SiO]2VO2]- and novel
 pentacoordinated oxoperoxo complex [[Ph3SiO]2VO(O2)]-: X-ray crystal
 structure and assessment as oxidation catalysts.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              908
_journal_page_last               913
_journal_paper_doi               10.1039/b400657g
_journal_year                    2004
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' (C36 H30 O4.43 Si2 V1)-, (C24 H30 P1)+ '
_chemical_formula_sum            'C60 H50 O4.43 P Si2 V'
_chemical_formula_weight         980.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             03-14-10
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 119.00(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.362(8)
_cell_length_b                   11.270(6)
_cell_length_c                   23.069(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      13.2
_cell_measurement_theta_min      13
_cell_volume                     5085(4)
_computing_cell_refinement
;
Cad4 Express, (Enraf-Nonius, 1989)
;
_computing_data_collection
;
Cad4 Express, (Enraf-Nonius, 1989)
;
_computing_data_reduction
;
RC93 (Watkin, Prout & Lilley, 1994)
;
_computing_molecular_graphics
;
CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
SHELXS 86 (Sheldrick, 1986)
;
_diffrn_ambient_pressure         1
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Enraf-Nonius CAD4
;
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.06
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9714
_diffrn_reflns_theta_full        24.972
_diffrn_reflns_theta_max         24.972
_diffrn_reflns_theta_min         1.041
_diffrn_standards_decay_%        6.46
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
Azimutal absorption correction (North et al, 1968)
;
_exptl_crystal_colour            ' dark violet '
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       ' stick '
_exptl_crystal_F_000             2045.732
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.93
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         5459
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.000463
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2

11.0 3.50 8.99
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0657
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0636
_reflns_limit_h_max              23
_reflns_limit_h_min              -26
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                5459
_reflns_number_total             8949
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b400657g.txt
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C60 H50 O4.43 P1 Si2 V1 '
_cod_database_code               7014058