Reaction of p-Toluenesulfonylamide and M(NMe2)4 (M = Ti, V): Generation of Electron-Deficient Imido Complexes of Early Transition Metals
Christian Lorber; Robert Choukroun; Laure Vendier; Inorganic Chemistry 46 (2007) 3192–3202; doi:10.1021/ic062404j

data_4307891
_publ_contact_author
;
Christian Lorber
;
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
205 Route de Narbonne
31077 Toulouse Cedex 04
;
_publ_contact_author_email       lorber@lcc-toulouse.fr
_publ_section_title
;
Reaction of p-Toluenesulfonylamide and M(NMe2)4 (M = Ti, V): Generation of
Electron-Deficient Imido Complexes of Early Transition Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3192
_journal_page_last               3202
_journal_paper_doi               10.1021/ic062404j
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H30 Cl4 N6 O V2'
_chemical_formula_sum            'C30 H30 Cl4 N6 O V2'
_chemical_formula_weight         734.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.44(3)
_cell_angle_beta                 96.79(3)
_cell_angle_gamma                98.97(3)
_cell_formula_units_Z            4
_cell_length_a                   15.306(3)
_cell_length_b                   15.806(3)
_cell_length_c                   16.916(3)
_cell_measurement_reflns_used    4000
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_measurement_wavelength     0.71073
_cell_volume                     3956.7(14)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_unetI/netI     0.7025
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15915
_diffrn_reflns_theta_full        26.22
_diffrn_reflns_theta_max         26.22
_diffrn_reflns_theta_min         1.96
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  4
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            'yellow orange'
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.195
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.679
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         15915
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.679
_refine_ls_R_factor_all          0.3463
_refine_ls_R_factor_gt           0.1096
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1953
_refine_ls_wR_factor_ref         0.2596
_reflns_number_gt                7033
_reflns_number_total             15915
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic062404jsi20061215_111655_1.cif
_cod_data_source_block           (8)
_cod_original_cell_volume        3956.8(14)
_cod_database_code               4307891