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_4065161
_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            'C111 H245 Ar3 I3 N9 Si9 W3'
_chemical_formula_weight         3011.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                67.569(5)
_cell_angle_beta                 66.668(7)
_cell_angle_gamma                63.299(6)
_cell_formula_units_Z            2
_cell_length_a                   19.065(4)
_cell_length_b                   20.937(4)
_cell_length_c                   23.744(5)
_cell_measurement_temperature    293(2)
_cell_volume                     7531(3)
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_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       '0.3deg. oscillations'
_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  0.0797
_diffrn_reflns_av_sigmaI/netI    0.1955
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22563
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    3.079
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             3070
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.534
_refine_diff_density_min         -3.143
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.088
_refine_ls_goodness_of_fit_obs   1.418
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1243
_refine_ls_number_reflns         17251
_refine_ls_number_restraints     10187
_refine_ls_restrained_S_all      1.298
_refine_ls_restrained_S_obs      1.506
_refine_ls_R_factor_all          0.1771
_refine_ls_R_factor_obs          0.1055
_refine_ls_shift/esd_max         3.150
_refine_ls_shift/esd_mean        0.242
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2705
_refine_ls_wR_factor_obs         0.2398
_reflns_number_observed          8486
_reflns_number_total             17257
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om200597z_si_001.cif
_cod_data_source_block           el8s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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        7531.3(26)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065161