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_4313986
_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_formula_moiety         ' C33 H44 N4 Si2 W1 '
_chemical_formula_sum            'C33 H44 N4 Si2 W'
_chemical_formula_weight         736.76
_chemical_name_systematic
;                                                 
  [W{(2-C5NH4)C(Me)(CH2NSiMe3)2}(NPh)Ph2]   
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 108.1435(28)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6367(5)
_cell_length_b                   17.1252(11)
_cell_length_c                   10.4777(5)
_cell_measurement_reflns_used    5881
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1643.17(16)
_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       \w/2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.07
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11744
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.910
_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    3.62
_exptl_absorpt_correction_T_max  0.696
_exptl_absorpt_correction_T_min  0.337
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.49
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             741.54
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.97
_refine_ls_abs_structure_Flack   0.20(3)
_refine_ls_extinction_coef       'none required'
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9146
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         3096
_refine_ls_number_restraints     382
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.0019
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979,
0.640    -.336E-010.307  
;
_refine_ls_weighting_scheme      'Chebychev polynomial'
_refine_ls_wR_factor_ref         0.0683
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              22
_reflns_limit_k_min              -21
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                3096
_reflns_number_total             6948
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ic034377ssi20030415_021439_1.cif
_cod_data_source_block           compound_6
_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_cell_volume        1643.2(6)
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        ' C33 H44 N4 Si2 W1 '
_cod_database_code               4313986