Reactivity Studies of (tBu3SiNH)(tBu3SiN═)2WH Including Anionic Derivatives Featuring the Tris-tri-tert-butylsilylimide Tungsten Core
Schafer, Daniel F.; Wolczanski, Peter T.; Lobkovsky, Emil B.; Organometallics 30 (2011) 6539–; doi:10.1021/om200597z

data_4065159
_publ_section_title
;
 Reactivity Studies of (tBu3SiNH)(tBu3SiN&#x2550;)2WH Including Anionic
 Derivatives Featuring the Tris-tri-tert-butylsilylimide Tungsten Core
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              6539
_journal_paper_doi               10.1021/om200597z
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C56 H128 K N5 O6.5 Si3 W'
_chemical_formula_weight         1282.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                88.37(3)
_cell_angle_beta                 88.41(3)
_cell_angle_gamma                69.99(3)
_cell_formula_units_Z            2
_cell_length_a                   12.168(2)
_cell_length_b                   17.080(3)
_cell_length_c                   18.459(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3602.6(14)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0676
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21561
_diffrn_reflns_theta_max         28.08
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    1.755
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_F_000             1372
_refine_diff_density_max         3.294
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.079
_refine_ls_goodness_of_fit_obs   1.095
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         10151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.240
_refine_ls_restrained_S_obs      1.095
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_obs          0.0519
_refine_ls_shift/esd_max         9.680
_refine_ls_shift/esd_mean        0.207
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+6.0095P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1820
_refine_ls_wR_factor_obs         0.1285
_reflns_number_observed          8807
_reflns_number_total             14926
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om200597z_si_001.cif
_cod_data_source_block           518
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+6.0095P] 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^)+(0.0668P)^2^+6.0095P] 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        3602.4(12)
_cod_original_formula_sum        'C56 H128 K N5 O6.50 Si3 W'
_cod_database_code               4065159