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_4307897
_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
;
?
;
_chemical_formula_moiety         ' C20 H35 Cl4 N5 O4 S2 Ti2 '
_chemical_formula_sum            'C20 H35 Cl4 N5 O4 S2 Ti2'
_chemical_formula_weight         711.27
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 128.659(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6523(17)
_cell_length_b                   11.4504(8)
_cell_length_c                   15.3571(11)
_cell_measurement_reflns_used    4360
_cell_measurement_temperature    180
_cell_measurement_theta_max      32
_cell_measurement_theta_min      3
_cell_volume                     3110.5(4)
_computing_cell_refinement
; 
 CrysAlis RED, (Oxford Diffraction, 2002) 
;
_computing_data_collection
; 
 Xcalibur, (Oxford Diffraction, 2002) 
;
_computing_data_reduction
; 
 CrysAlis RED, (Oxford Diffraction, 2002) 
;
_computing_structure_solution
; 
 SIR92 (Altomare et al, 1994) 
;
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
; 
Oxford Diffraction XCALIBUR 
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31117
_diffrn_reflns_theta_full        32.096
_diffrn_reflns_theta_max         32.096
_diffrn_reflns_theta_min         3.258
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  0.78
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       ' stick '
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.57
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0804
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2640
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000282
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 6.35 -3.08 5.13 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0455
_refine_ls_wR_factor_gt          0.0380
_refine_ls_wR_factor_ref         0.0380
_reflns_limit_h_max              25
_reflns_limit_h_min              -33
_reflns_limit_k_max              16
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2640
_reflns_number_total             5123
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            ic062404jsi20061215_111655_7.cif
_cod_data_source_block           (6)
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        ' C20 H35 Cl4 N5 O4 S2 Ti2 '
_cod_database_code               4307897