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_4115737
_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            'C36 H83 N3 Si3 W'
_chemical_formula_weight         826.18
_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   'diff. map for H1, geom. for the rest'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.477(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4342(2)
_cell_length_b                   16.2068(1)
_cell_length_c                   20.8307(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4535.22(10)
_computing_cell_refinement       SMART
_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       \w-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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25801
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.59
_diffrn_standards_decay_%        3.4
_exptl_absorpt_coefficient_mu    2.651
_exptl_absorpt_correction_T_max  0.4918
_exptl_absorpt_correction_T_min  0.8621
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.722
_refine_diff_density_min         -1.566
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.088
_refine_ls_goodness_of_fit_obs   1.039
_refine_ls_hydrogen_treatment    'isotropic H1, riding for the rest'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         9075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.039
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_obs          0.0319
_refine_ls_shift/esd_max         1.271
_refine_ls_shift/esd_mean        0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+3.2776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0943
_refine_ls_wR_factor_obs         0.0789
_reflns_number_observed          7392
_reflns_number_total             9840
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja010957h_2.cif
_cod_data_source_block           (tBu3SiN)2(tBu3SiHN)WH_2.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^)+(0.0433P)^2^+3.2776P] 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^)+(0.0433P)^2^+3.2776P] 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_original_cell_volume        4535.2(1)
_cod_database_code               4115737