Symmetry and Geometry Considerations of Atom Transfer: Deoxygenation of (silox)3WNO and R3PO (R = Me, Ph,tBu) by (silox)3M (M = V, NbL (L = PMe3, 4-Picoline), Ta; silox =tBu3SiO)
Adam S. Veige; LeGrande M. Slaughter; Emil B. Lobkovsky; Peter T. Wolczanski; Nikita Matsunaga; Stephen A. Decker; Thomas R. Cundari; Inorganic Chemistry 42 (2003) 6204–6224; doi:10.1021/ic0300114

data_4314298
_publ_section_title
;
 Symmetry and Geometry Considerations of Atom Transfer: Deoxygenation of
 (silox)3WNO and R3PO (R = Me, Ph,tBu) by (silox)3M (M = V, NbL (L = PMe3,
 4-Picoline), Ta; silox =tBu3SiO)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6204
_journal_page_last               6224
_journal_paper_doi               10.1021/ic0300114
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C39 H90 O4 P Si3 V'
_chemical_formula_weight         789.29
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.294(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2336(12)
_cell_length_b                   17.4681(17)
_cell_length_c                   21.070(2)
_cell_measurement_temperature    193(2)
_cell_volume                     4870.6(8)
_computing_cell_refinement       SAINT+
_computing_data_collection       SMART
_computing_data_reduction        SAINT+
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.874
_diffrn_measured_fraction_theta_max 0.874
_diffrn_measurement_device_type  'Bruker 1K CCD'
_diffrn_measurement_method       '0.3 deg. omega & phi scans'
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23139
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  0.9346
_exptl_absorpt_correction_T_min  0.7795
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    RIDING
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0654P)^2^+1.3395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                6363
_reflns_number_total             7278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0300114_1.cif
_cod_data_source_block           asv355
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4870.7(8)
_cod_database_code               4314298