#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:33:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179116 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/78/4307898.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4307898
loop_
_publ_author_name
'Christian Lorber'
'Robert Choukroun'
'Laure Vendier'
_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         'C15 H15 Cl3 N3 V1'
_chemical_formula_sum            'C15 H15 Cl3 N3 V'
_chemical_formula_weight         394.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.878(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2975(10)
_cell_length_b                   8.5345(8)
_cell_length_c                   15.5771(14)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_measurement_wavelength     0.71073
_cell_volume                     1746.6(3)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       φ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13232
_diffrn_reflns_theta_full        26.13
_diffrn_reflns_theta_max         26.13
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  4
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    1.025
_exptl_absorpt_correction_T_max  0.853
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0450P)²+0.4673P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                3011
_reflns_number_total             3406
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic062404jsi20061215_111655_8.cif
_cod_data_source_block           (7)
_cod_database_code               4307898
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.56025(13) 0.1145(2) 1.16873(11) 0.0370(4) Uani 1 1 d . . .
H1 H 0.5431 0.0151 1.1862 0.044 Uiso 1 1 calc R . .
C2 C 0.49339(15) 0.2352(3) 1.17404(12) 0.0472(5) Uani 1 1 d . . .
H2 H 0.4325 0.2178 1.195 0.057 Uiso 1 1 calc R . .
C3 C 0.51780(18) 0.3820(3) 1.14791(14) 0.0561(6) Uani 1 1 d . . .
H3 H 0.473 0.4652 1.1495 0.067 Uiso 1 1 calc R . .
C4 C 0.60933(19) 0.4043(2) 1.11940(14) 0.0548(5) Uani 1 1 d . . .
H4 H 0.6279 0.5033 1.1024 0.066 Uiso 1 1 calc R . .
C5 C 0.67364(15) 0.2782(2) 1.11624(12) 0.0407(4) Uani 1 1 d . . .
H5 H 0.7358 0.2943 1.0973 0.049 Uiso 1 1 calc R . .
C6 C 0.67689(13) 0.0906(2) 0.94017(11) 0.0363(4) Uani 1 1 d . . .
H6 H 0.6134 0.0895 0.9582 0.044 Uiso 1 1 calc R . .
C7 C 0.68741(16) 0.1673(3) 0.86404(12) 0.0490(5) Uani 1 1 d . . .
H7 H 0.6322 0.2191 0.8325 0.059 Uiso 1 1 calc R . .
C8 C 0.78048(18) 0.1666(3) 0.83511(13) 0.0539(5) Uani 1 1 d . . .
H8 H 0.7895 0.2199 0.7848 0.065 Uiso 1 1 calc R . .
C9 C 0.85983(16) 0.0851(3) 0.88265(12) 0.0469(5) Uani 1 1 d . . .
H9 H 0.9225 0.0782 0.8635 0.056 Uiso 1 1 calc R . .
C10 C 0.84454(13) 0.0140(2) 0.95909(11) 0.0372(4) Uani 1 1 d . . .
H10 H 0.8988 -0.0388 0.9914 0.045 Uiso 1 1 calc R . .
C11 C 0.89452(13) -0.3442(2) 1.14919(11) 0.0360(4) Uani 1 1 d . . .
H11 H 0.9135 -0.2944 1.2023 0.043 Uiso 1 1 calc R . .
C12 C 0.94098(14) -0.4845(2) 1.13405(13) 0.0426(4) Uani 1 1 d . . .
H12 H 0.9896 -0.5283 1.1766 0.051 Uiso 1 1 calc R . .
C13 C 0.91454(14) -0.5584(2) 1.05551(13) 0.0413(4) Uani 1 1 d . . .
H13 H 0.9444 -0.6533 1.0443 0.05 Uiso 1 1 calc R . .
C14 C 0.84286(14) -0.4893(2) 0.99332(12) 0.0407(4) Uani 1 1 d . . .
H14 H 0.8246 -0.5358 0.9392 0.049 Uiso 1 1 calc R . .
C15 C 0.79896(13) -0.3504(2) 1.01284(11) 0.0366(4) Uani 1 1 d . . .
H15 H 0.7505 -0.3047 0.9709 0.044 Uiso 1 1 calc R . .
N1 N 0.64968(10) 0.13324(16) 1.13941(9) 0.0318(3) Uani 1 1 d . . .
N2 N 0.82305(10) -0.27727(16) 1.09015(9) 0.0318(3) Uani 1 1 d . . .
N3 N 0.75502(10) 0.01732(16) 0.98925(8) 0.0304(3) Uani 1 1 d . . .
Cl3 Cl 0.73817(3) -0.15153(6) 1.26103(3) 0.04340(13) Uani 1 1 d . . .
Cl1 Cl 0.89177(3) 0.07181(5) 1.16276(3) 0.03581(11) Uani 1 1 d . . .
Cl2 Cl 0.59130(3) -0.19175(5) 1.05810(3) 0.03667(12) Uani 1 1 d . . .
V1 V 0.740960(19) -0.06975(3) 1.119818(16) 0.02692(9) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 C2 123.03(18) . . ?
N1 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
C3 C2 C1 118.89(19) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 119.02(18) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 119.3(2) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C4 122.39(19) . . ?
N1 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
N3 C6 C7 122.47(17) . . ?
N3 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C6 C7 C8 119.54(18) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C9 C8 C7 118.46(18) . . ?
C9 C8 H8 120.8 . . ?
C7 C8 H8 120.8 . . ?
C10 C9 C8 118.87(18) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
N3 C10 C9 123.26(16) . . ?
N3 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N2 C11 C12 122.57(17) . . ?
N2 C11 H11 118.7 . . ?
C12 C11 H11 118.7 . . ?
C13 C12 C11 119.31(17) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 118.85(16) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C15 C14 C13 118.89(17) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
N2 C15 C14 123.02(16) . . ?
N2 C15 H15 118.5 . . ?
C14 C15 H15 118.5 . . ?
C5 N1 C1 117.37(15) . . ?
C5 N1 V1 122.61(12) . . ?
C1 N1 V1 119.74(12) . . ?
C11 N2 C15 117.34(14) . . ?
C11 N2 V1 121.86(11) . . ?
C15 N2 V1 120.65(11) . . ?
C6 N3 C10 117.29(14) . . ?
C6 N3 V1 120.92(11) . . ?
C10 N3 V1 121.44(11) . . ?
N1 V1 N2 175.04(5) . . ?
N1 V1 N3 89.40(5) . . ?
N2 V1 N3 87.79(5) . . ?
N1 V1 Cl3 90.90(4) . . ?
N2 V1 Cl3 92.22(4) . . ?
N3 V1 Cl3 175.49(4) . . ?
N1 V1 Cl2 87.35(4) . . ?
N2 V1 Cl2 88.45(4) . . ?
N3 V1 Cl2 87.61(4) . . ?
Cl3 V1 Cl2 96.89(2) . . ?
N1 V1 Cl1 91.20(4) . . ?
N2 V1 Cl1 92.58(4) . . ?
N3 V1 Cl1 84.19(4) . . ?
Cl3 V1 Cl1 91.30(2) . . ?
Cl2 V1 Cl1 171.696(19) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.348(2) . ?
C1 C2 1.372(3) . ?
C1 H1 0.93 . ?
C2 C3 1.372(3) . ?
C2 H2 0.93 . ?
C3 C4 1.372(3) . ?
C3 H3 0.93 . ?
C4 C5 1.380(3) . ?
C4 H4 0.93 . ?
C5 N1 1.341(2) . ?
C5 H5 0.93 . ?
C6 N3 1.345(2) . ?
C6 C7 1.381(3) . ?
C6 H6 0.93 . ?
C7 C8 1.381(3) . ?
C7 H7 0.93 . ?
C8 C9 1.380(3) . ?
C8 H8 0.93 . ?
C9 C10 1.379(3) . ?
C9 H9 0.93 . ?
C10 N3 1.346(2) . ?
C10 H10 0.93 . ?
C11 N2 1.344(2) . ?
C11 C12 1.384(3) . ?
C11 H11 0.93 . ?
C12 C13 1.373(3) . ?
C12 H12 0.93 . ?
C13 C14 1.382(3) . ?
C13 H13 0.93 . ?
C14 C15 1.376(2) . ?
C14 H14 0.93 . ?
C15 N2 1.350(2) . ?
C15 H15 0.93 . ?
N1 V1 2.1639(14) . ?
N2 V1 2.1674(14) . ?
N3 V1 2.2003(13) . ?
Cl3 V1 2.3135(5) . ?
Cl1 V1 2.3483(5) . ?
Cl2 V1 2.3191(5) . ?
