Comparison of H-H versus Si-H σ-Bond Coordination and Activation on 16e Metal Fragments. Organosilane, N2, and Ethylene Addition to the Agostic Complex W(CO)3(PR3)2 and Dynamic NMR Behavior of the Latter
Matthew D. Butts; Jeffrey C. Bryan; Xiao-Liang Luo; Gregory J. Kubas; Inorganic Chemistry 36 (1997) 3341–3353; doi:10.1021/ic960870a

data_4323498
_publ_section_title
;
 Comparison of H-H versus Si-H \s-Bond Coordination and Activation on 16e
 Metal Fragments. Organosilane, N2, and Ethylene Addition to the Agostic
 Complex W(CO)3(PR3)2 and Dynamic NMR Behavior of the Latter
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3341
_journal_page_last               3353
_journal_paper_doi               10.1021/ic960870a
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         'W, 3(C O), (C9 H21 P), H, (C12 H10 Si)'
_chemical_formula_sum            'C48 H64 O6 P2 Si2 W2'
_chemical_formula_weight         1222.81
_chemical_name_common
;
tri-isopropylphosphinetricarbonylhydridetungsten dimer \m-diphenylsilane
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.390(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.760(2)
_cell_length_b                   17.427(2)
_cell_length_c                   17.957(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      42.4
_cell_measurement_theta_min      7.6
_cell_volume                     4931.8(10)
_computing_cell_refinement       XSCANS
_computing_data_collection       XSCANS
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       omega
_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  0.0885
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5382
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.58
_diffrn_standards_interval_count 147
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.820
_exptl_absorpt_correction_T_max  0.511
_exptl_absorpt_correction_T_min  0.178
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.691
_refine_diff_density_min         -3.228
_refine_diff_density_rms         0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.088
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.088
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_obs          0.0607
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+6.5801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1661
_refine_ls_wR_factor_obs         0.1462
_reflns_number_observed          3383
_reflns_number_total             4539
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960870a_3.cif
_cod_data_source_block           wsil1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+6.5801P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+6.5801P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323498