σ-Silane, Disilanyl, and [W(μ-H)Si(μ-H)W] Bridging Silylene Complexes via the Reactions of W(PMe3)4(η(2)-CH2PMe2)H with Phenylsilanes.
Zuzek, Ashley A.; Neary, Michelle C.; Parkin, Gerard; Journal of the American Chemical Society  (2014) 141217070549000–; doi:10.1021/ja510703s

data_4123153
_publ_section_title
;
 \s-Silane, Disilanyl, and [W(\m-H)Si(\m-H)W] Bridging Silylene Complexes
 via the Reactions of W(PMe3)4(\h(2)-CH2PMe2)H with Phenylsilanes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141217070549000
_journal_paper_doi               10.1021/ja510703s
_journal_year                    2014
_chemical_formula_sum            'C24 H52 P4 Si2 W'
_chemical_formula_weight         704.56
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.0754(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7561(9)
_cell_length_b                   16.1203(15)
_cell_length_c                   10.2677(10)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.82
_cell_measurement_theta_min      2.35
_cell_volume                     1612.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0400
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28352
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.920
_diffrn_reflns_theta_min         1.986
_exptl_absorpt_coefficient_mu    3.866
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5573
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       plate
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.461
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   -0.023(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         11341
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.961
_reflns_number_gt                10479
_reflns_number_total             11341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja510703s_si_004.cif
_cod_data_source_block           wpsi2s10
_cod_database_code               4123153
_shelx_estimated_absorpt_t_min   0.411
_shelx_estimated_absorpt_t_max   0.893
_shelxl_version_number           2013-4
_shelx_res_checksum              5378
_shelx_hkl_checksum              70434