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_4065160
_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            'C36 H82 K N3 Si3 W'
_chemical_formula_weight         864.27
_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   'all but H1 geom'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                70.85(4)
_cell_angle_beta                 71.47(4)
_cell_angle_gamma                62.55(3)
_cell_formula_units_Z            2
_cell_length_a                   12.941(1)
_cell_length_b                   13.103(1)
_cell_length_c                   16.293(1)
_cell_measurement_temperature    295(2)
_cell_volume                     2269.8(8)
_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      295(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       \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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0653
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13041
_diffrn_reflns_theta_max         28.07
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    2.741
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.609
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_meas      ?
_exptl_crystal_description       bulk
_exptl_crystal_F_000             908
_exptl_crystal_size_max          0.60
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_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.660
_refine_diff_density_min         -4.880
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.037
_refine_ls_hydrogen_treatment    'all but h1 riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8500
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.037
_refine_ls_R_factor_all          0.0671
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+5.9010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1661
_refine_ls_wR_factor_obs         0.1500
_reflns_number_observed          7838
_reflns_number_total             9148
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om200597z_si_001.cif
_cod_data_source_block           522
_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^)+(0.1034P)^2^+5.9010P] 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^)+(0.1034P)^2^+5.9010P] 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        2269.9(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065160