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_4065158
_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            'C48 H111 K N3 O3 Si3 W'
_chemical_formula_weight         1085.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_atom_sites_solution_hydrogens   'H1 from diff. map, rest geom.'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 95.6070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2546(2)
_cell_length_b                   22.01670(10)
_cell_length_c                   20.8776(3)
_cell_measurement_temperature    165(1)
_cell_volume                     6063.40(13)
_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      165(1)
_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
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_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       368
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
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_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  0.927985
_exptl_absorpt_correction_T_min  0.655568
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.40
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_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.999
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.062
_refine_ls_hydrogen_treatment    'H1 isotropic, rest riding'
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         10322
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.062
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_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         0.1685
_refine_ls_wR_factor_obs         0.1331
_reflns_number_observed          8560
_reflns_number_total             13553
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om200597z_si_001.cif
_cod_data_source_block           dfs502
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_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_sg_symbol_H-M      P2(1)/n
_cod_database_code               4065158