Experimental and Theoretical Study of a Tungsten Dihydride Silyl Complex: New Insight into Its Bonding Nature and Fluxional Behavior
Ray, Mausumi; Nakao, Yoshihide; Sato, Hirofumi; Sakaki, Shigeyoshi; Watanabe, Takahito; Hashimoto, Hisako; Tobita, Hiromi; Organometallics 29 (2010) 6267–; doi:10.1021/om100653v

data_4066813
_publ_section_title
;
 Experimental and Theoretical Study of a Tungsten Dihydride Silyl Complex:
 New Insight into Its Bonding Nature and Fluxional Behavior
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6267
_journal_paper_doi               10.1021/om100653v
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C23 H48 O3 Si4 W'
_chemical_formula_weight         668.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 94.745(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7384(17)
_cell_length_b                   8.9528(15)
_cell_length_c                   20.893(2)
_cell_measurement_temperature    150(2)
_cell_volume                     2933.8(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12367
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    4.122
_exptl_absorpt_correction_T_max  0.8525
_exptl_absorpt_correction_T_min  0.4255
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.04
_refine_diff_density_max         6.798
_refine_diff_density_min         -7.077
_refine_diff_density_rms         0.456
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         6372
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.1243
_refine_ls_shift/su_max          2.181
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+523.6761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2919
_refine_ls_wR_factor_ref         0.3036
_reflns_number_gt                5649
_reflns_number_total             6372
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100653v_si_001.cif
_cod_data_source_block           tak
_cod_original_cell_volume        2933.7(7)
_cod_database_code               4066813