Synthesis and reactivity of the imidotungsten methyl cation [W(N2Npy)(NPh)Me]+: CO2 adds to the W???NPh bond and does not insert into the W???Me bondElectronic supplementary information (ESI) available: crystal data for 2, DFT/computational notes, supporting characterising data and selected experimental details for the new compounds. See http://www.rsc.org/suppdata/cc/b2/b208327b/
Ward, Benjamin D.; Clot, Eric; Dubberley, Stuart R.; Gade, Lutz H.; Mountford, Philip; Chemical Communications  (2002) 2618–; doi:10.1039/b208327b

data_7114056
_publ_section_title
;
 Synthesis and reactivity of the imidotungsten methyl cation
 [W(N2Npy)(NPh)Me]+: CO2 adds to the W???NPh bond and does not insert into
 the W???Me bondElectronic supplementary information (ESI) available:
 crystal data for 2, DFT/computational notes, supporting characterising
 data and selected experimental details for the new compounds. See
 http://www.rsc.org/suppdata/cc/b2/b208327b/
;
_journal_issue                   22
_journal_name_full               'Chemical Communications'
_journal_page_first              2618
_journal_paper_doi               10.1039/b208327b
_journal_year                    2002
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C23 H40 N4 Si2 W1 '
_chemical_formula_sum            'C23 H40 N4 Si2 W'
_chemical_formula_weight         612.62
_chemical_name_systematic
;                                                                               
 [W{(2-C5NH4)C(Me)(CH2NSiMe3)2}(NPh)Me2]                                                                              
;
_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   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90.00
_cell_angle_beta                 91.659(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.6452(2)
_cell_length_b                   16.4633(3)
_cell_length_c                   15.2794(2)
_cell_measurement_reflns_used    6261
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2676.67(8)
_computing_cell_refinement
;                                                                               
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)                            
;
_computing_data_collection
;                                                                               
KappaCCD software 'Collect' (Nonius, 2000)                                      
;
_computing_data_reduction
;                                                                               
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)                            
;
_computing_molecular_graphics    'CAMERON (Watkin, Prout and Pearce, 1996)'
_computing_publication_material
;                                                                               
CRYSTALS Issue 10 (Watkin et al., 1996)                                         
;
_computing_structure_refinement
;                                                                               
CRYSTALS Issue 10 (Watkin et al., 1996)                                         
;
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.01
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12044
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.91
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    4.42
_exptl_absorpt_correction_T_max  0.643
_exptl_absorpt_correction_T_min  0.413
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.52
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       'block '
_exptl_crystal_F_000             1227.09
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.19
_refine_diff_density_min         -0.60
_refine_ls_abs_structure_Flack   none
_refine_ls_extinction_coef       71.1(39)
_refine_ls_extinction_method
'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   1.2430
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4338
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 2 parameters, Carruthers & Watkin , 1979, 
0.828E-01-.519    
;
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_ref         0.0106
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                4338
_reflns_number_total             6111
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            b208327b.txt
_cod_data_source_block           COMPOUND_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

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:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C23 H40 N4 Si2 W1 '
_cod_database_code               7114056