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_4115739
_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            'C14.5 H29.5 Cl N1.5 Si W0.5'
_chemical_formula_weight         380.36
_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                 93.97(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.999(2)
_cell_length_b                   12.801(3)
_cell_length_c                   23.170(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3550.4(13)
_computing_cell_refinement       SAINT+
_computing_data_collection       SMART
_computing_data_reduction        SAINT+
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Bruker 1K  CCD'
_diffrn_measurement_method       '0.3 deg. omega scan'
_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  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0838
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11393
_diffrn_reflns_theta_max         28.57
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    3.493
_exptl_absorpt_correction_T_max  0.962333
_exptl_absorpt_correction_T_min  0.794497
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.575
_refine_diff_density_min         -1.826
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.984
_refine_ls_goodness_of_fit_obs   1.020
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         3020
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.020
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_obs          0.0418
_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^)+(0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1203
_refine_ls_wR_factor_obs         0.0956
_reflns_number_observed          2583
_reflns_number_total             4120
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja010957h_4.cif
_cod_data_source_block           W(NSitBu3)2Cl2py.6-py.cif_file
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+0.0000P] 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^)+(0.0621P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3550.4(12)
_cod_original_formula_sum        'C14.50 H29.50 Cl N1.50 Si W0.50'
_cod_database_code               4115739