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_4314301
_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 Nb O3 P Si3'
_chemical_formula_weight         815.26
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 92.718(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   46.322(7)
_cell_length_b                   12.8527(14)
_cell_length_c                   18.580(3)
_cell_measurement_temperature    243(2)
_cell_volume                     11049(3)
_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      243(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       61
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63777
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  0.8766
_exptl_absorpt_correction_T_min  0.705289
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.914
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         13712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          5.071
_refine_ls_shift/su_mean         0.283
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+18.0027P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1302
_reflns_number_gt                10887
_reflns_number_total             13712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0300114_4.cif
_cod_data_source_block           asv366b
_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        11050(3)
_cod_database_code               4314301