Synthesis of (tBu3SiNH)2ClW\τbWCl(NHSitBu3)2 and Its Degradation via NH Bond Activation
Stephen M. Holmes; Daniel F. Schafer; Peter T. Wolczanski; Emil B. Lobkovsky; Journal of the American Chemical Society 123 (2001) 10571–10583; doi:10.1021/ja010957h

data_4115741
_publ_section_title
;
 Synthesis of (tBu3SiNH)2ClW\\tbWCl(NHSitBu3)2 and Its Degradation via NH
 Bond Activation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10571
_journal_page_last               10583
_journal_paper_doi               10.1021/ja010957h
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C38 H65 Cl N2 Si2 W'
_chemical_formula_weight         825.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 110.903(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.393(2)
_cell_length_b                   17.903(3)
_cell_length_c                   17.057(2)
_cell_measurement_temperature    173(2)
_cell_volume                     4105.9(10)
_computing_cell_refinement       SAINT+
_computing_data_collection       SMART
_computing_data_reduction        SAINT+
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker 1K CCD'
_diffrn_measurement_method       '0.3 deg. omega & phi scans'
_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  0.0720
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44227
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    2.963
_exptl_absorpt_correction_T_max  0.7560
_exptl_absorpt_correction_T_min  0.557664
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       rod
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.550
_refine_diff_density_min         -1.897
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         10173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+3.2520P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0927
_reflns_number_gt                7927
_reflns_number_total             10173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010957h_6.cif
_cod_data_source_block           (tBu3SiHN)(tBu3SiN)ClW(PhCCPh)_12.cif_file
_cod_original_cell_volume        4105.8(10)
_cod_database_code               4115741