Group 6 Imido Complexes Supported by Diamido-Donor Ligands
Benjamin D. Ward; Stuart R. Dubberley; Lutz H. Gade; Philip Mountford; Inorganic Chemistry 42 (2003) 4961–4969; doi:10.1021/ic034377s

data_4313987
_publ_contact_author
;
  Dr P. Mountford         
  Inorganic Chemistry Laboratory
  South Parks Road
  Oxford
  OX1 3QR
  UK
;
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk
_publ_contact_author_fax         '+44 1865 272690'
_publ_contact_author_phone       '+44 1865 272679'
_publ_section_title
;
 Group 6 Imido Complexes Supported by Diamido-Donor Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4961
_journal_page_last               4969
_journal_paper_doi               10.1021/ic034377s
_journal_volume                  42
_journal_year                    2003
_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            ic034377ssi20030415_021439_2.cif
_cod_data_source_block           compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z 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:

'_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               4313987