Coordinatively Unsaturated W(IV)-Bis(pyridine) Complexes, a Reactive Source of W(IV)
R. C. Mills; S. Y. S. Wang; K. A. Abboud; J. M. Boncella; Inorganic Chemistry 40 (2001) 5077–5082; doi:10.1021/ic010195r

data_4320290
_publ_section_title
;
 Coordinatively Unsaturated W(IV)-Bis(pyridine) Complexes, a Reactive
 Source of W(IV)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5077
_journal_page_last               5082
_journal_paper_doi               10.1021/ic010195r
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C31 H42 N5 O1.5 Si2 W'
_chemical_formula_weight         748.73
_chemical_name_systematic
;
?
;
_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                69.341(1)
_cell_angle_beta                 78.022(1)
_cell_angle_gamma                76.008(1)
_cell_formula_units_Z            2
_cell_length_a                   10.0740(7)
_cell_length_b                   12.0912(9)
_cell_length_c                   15.336(1)
_cell_measurement_temperature    173(2)
_cell_volume                     1680.6(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11730
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    3.540
_exptl_absorpt_correction_T_max  0.9287
_exptl_absorpt_correction_T_min  0.3380
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plates
_exptl_crystal_F_000             754
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7565
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+3.5875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0801
_reflns_number_gt                6907
_reflns_number_total             7565
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010195r_2.cif
_cod_data_source_block           8a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_formula_sum        'C31 H42 N5 O1.50 Si2 W'
_cod_database_code               4320290