β-Agostic Silylamido and Silyl-Hydrido Compounds of Molybdenum and Tungsten
Stanislav K. Ignatov; Andrey Y. Khalimon; Nicholas H. Rees; Alexei G. Razuvaev; Philip Mountford; Georgii I. Nikonov; Inorganic Chemistry 48 (2009) 9605–9622; doi:10.1021/ic900591e

data_4303365
_publ_contact_author
; Dr Georgii I. Nikonov
  Department of Chemistry, Brock University
  500 Glenridge Ave., St. Catharines, L2S 3A1, ON, Canada
;
_publ_contact_author_email       gnikonov@brocku.ca
_publ_section_title
;
\b-Agostic Silylamido and Silyl-Hydrido Compounds of Molybdenum and
Tungsten
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9605
_journal_page_last               9622
_journal_paper_doi               10.1021/ic900591e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C28 H47 Cl2 N2 P Si W'
_chemical_formula_weight         725.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 107.7540(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0467(2)
_cell_length_b                   32.2846(3)
_cell_length_c                   10.5529(2)
_cell_measurement_temperature    150(2)
_cell_volume                     3259.86(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14107
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         5.14
_exptl_absorpt_coefficient_mu    3.812
_exptl_absorpt_correction_T_max  0.583
_exptl_absorpt_correction_T_min  0.466
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.567
_refine_diff_density_min         -0.865
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         7401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0199P)^2^+5.2815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                6229
_reflns_number_total             7401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900591e_si_001.cif
_cod_data_source_block           gin17
_cod_original_cell_volume        3259.86(9)
_cod_database_code               4303365