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_4115740
_publ_section_title
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 Synthesis of (tBu3SiNH)2ClW\\tbWCl(NHSitBu3)2 and Its Degradation via NH
 Bond Activation
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_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         825.42
_chemical_name_systematic
; 
 ? 
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_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
_cell_angle_alpha                90.00
_cell_angle_beta                 101.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.081(2)
_cell_length_b                   12.080(2)
_cell_length_c                   29.080(6)
_cell_measurement_temperature    173(2)
_cell_volume                     4163.1(14)
_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_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_wavelength     0.94300
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            5625
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    2.925
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_description       prism
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         .837
_refine_diff_density_min         -1.454
_refine_diff_density_rms         .109
_refine_ls_extinction_coef       0.0031(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.151
_refine_ls_goodness_of_fit_obs   1.176
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         3393
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.151
_refine_ls_restrained_S_obs      1.175
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_obs          0.0626
_refine_ls_shift/esd_max         0.568
_refine_ls_shift/esd_mean        0.045
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1137P)^2^+12.7268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1890
_refine_ls_wR_factor_obs         0.1846
_reflns_number_observed          3131
_reflns_number_total             3393
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja010957h_5.cif
_cod_data_source_block           (tBu3SiN)2ClW(trans-PhCCHPh)_11.cif
_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^)+(0.1137P)^2^+12.7268P] 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^)+(0.1137P)^2^+12.7268P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4115740