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_4115736
_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            'C54 H124 Cl2 N4 Si4 W2'
_chemical_formula_weight         1380.53
_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
_cell_angle_alpha                90.0000(15)
_cell_angle_beta                 100.117(2)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            4
_cell_length_a                   13.7997(4)
_cell_length_b                   23.8392(2)
_cell_length_c                   21.7517(7)
_cell_measurement_temperature    293(2)
_cell_volume                     7044.5(3)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       '0.5 deg. \w-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  0.1404
_diffrn_reflns_av_sigmaI/netI    0.1571
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23390
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         1.28
_exptl_absorpt_coefficient_mu    3.439
_exptl_absorpt_correction_T_max  0.962155
_exptl_absorpt_correction_T_min  0.496917
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         6.354
_refine_diff_density_min         -1.034
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.010
_refine_ls_goodness_of_fit_obs   1.111
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5498
_refine_ls_number_restraints     1392
_refine_ls_restrained_S_all      0.936
_refine_ls_restrained_S_obs      0.984
_refine_ls_R_factor_all          0.1726
_refine_ls_R_factor_obs          0.0970
_refine_ls_shift/esd_max         8.580
_refine_ls_shift/esd_mean        0.118
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1844P)^2^+49.8403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3030
_refine_ls_wR_factor_obs         0.2486
_reflns_number_observed          3463
_reflns_number_total             7281
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja010957h_1.cif
_cod_data_source_block           '[(tBu3SiHN)2ClW]2_1.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^)+(0.1844P)^2^+49.8403P] 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^)+(0.1844P)^2^+49.8403P] 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               4115736