#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:33:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179116 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/78/4307893.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_4307893
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         'C22 H38 N6 O4 S2 V2'
_chemical_formula_sum            'C22 H38 N6 O4 S2 V2'
_chemical_formula_weight         616.60
_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                 94.020(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0142(5)
_cell_length_b                   8.8093(8)
_cell_length_c                   20.0954(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                     1415.23(19)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12049
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         3.08
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  4
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  0.8950
_exptl_absorpt_correction_T_min  0.8211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.375
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0272
_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)+(0.0462P)²+0.3629P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                2314
_reflns_number_total             2749
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic062404jsi20061215_111655_3.cif
_cod_data_source_block           (2)
_cod_original_cell_volume        1415.23(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4307893
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 0.9467(2) 0.35924(19) -0.17868(8) 0.0230(4) Uani 1 1 d . . .
C2 C 0.8557(2) 0.2255(2) -0.18420(9) 0.0285(4) Uani 1 1 d . . .
H2 H 0.8905 0.1404 -0.1596 0.034 Uiso 1 1 calc R . .
C3 C 0.7128(2) 0.2199(2) -0.22669(10) 0.0330(4) Uani 1 1 d . . .
H3 H 0.6523 0.13 -0.2308 0.04 Uiso 1 1 calc R . .
C4 C 0.6578(2) 0.3460(2) -0.26345(9) 0.0312(4) Uani 1 1 d . . .
C5 C 0.7506(2) 0.4785(2) -0.25719(9) 0.0303(4) Uani 1 1 d . . .
H5 H 0.7157 0.5638 -0.2816 0.036 Uiso 1 1 calc R . .
C6 C 0.8945(2) 0.4857(2) -0.21516(9) 0.0268(4) Uani 1 1 d . . .
H6 H 0.9559 0.5752 -0.2114 0.032 Uiso 1 1 calc R . .
C7 C 0.5016(3) 0.3362(3) -0.30978(12) 0.0473(6) Uani 1 1 d . . .
H7A H 0.5028 0.2433 -0.3348 0.071 Uiso 1 1 calc R . .
H7B H 0.4977 0.4209 -0.3399 0.071 Uiso 1 1 calc R . .
H7C H 0.4049 0.338 -0.2841 0.071 Uiso 1 1 calc R . .
C8 C 0.8899(3) 0.1729(2) 0.10203(10) 0.0368(5) Uani 1 1 d . . .
H8A H 0.8454 0.0722 0.0963 0.055 Uiso 1 1 calc R . .
H8B H 0.7995 0.2445 0.1022 0.055 Uiso 1 1 calc R . .
H8C H 0.9564 0.1788 0.1436 0.055 Uiso 1 1 calc R . .
C9 C 1.1484(2) 0.1227(2) 0.04834(10) 0.0340(4) Uani 1 1 d . . .
H9A H 1.2147 0.1441 0.0889 0.051 Uiso 1 1 calc R . .
H9B H 1.2094 0.1513 0.0108 0.051 Uiso 1 1 calc R . .
H9C H 1.1236 0.0162 0.046 0.051 Uiso 1 1 calc R . .
C10 C 0.6286(2) 0.4773(2) -0.07628(9) 0.0321(4) Uani 1 1 d . . .
H10A H 0.6081 0.4392 -0.1209 0.048 Uiso 1 1 calc R . .
H10B H 0.7061 0.5604 -0.0764 0.048 Uiso 1 1 calc R . .
H10C H 0.5254 0.5116 -0.06 0.048 Uiso 1 1 calc R . .
C11 C 0.5884(2) 0.2262(2) -0.03228(12) 0.0389(5) Uani 1 1 d . . .
H11A H 0.4804 0.2581 -0.0197 0.058 Uiso 1 1 calc R . .
H11B H 0.6343 0.1531 -0.0006 0.058 Uiso 1 1 calc R . .
H11C H 0.5773 0.1811 -0.0759 0.058 Uiso 1 1 calc R . .
N1 N 1.06042(17) 0.43469(16) -0.05584(7) 0.0204(3) Uani 1 1 d . . .
N2 N 0.99374(19) 0.20826(16) 0.04722(7) 0.0256(3) Uani 1 1 d . . .
N3 N 0.69897(18) 0.35667(16) -0.03318(7) 0.0251(3) Uani 1 1 d . . .
O1 O 1.18849(17) 0.21632(15) -0.11312(7) 0.0349(3) Uani 1 1 d . . .
O2 O 1.24001(16) 0.47664(16) -0.15001(6) 0.0340(3) Uani 1 1 d . . .
S1 S 1.12760(5) 0.36906(5) -0.12323(2) 0.02273(12) Uani 1 1 d . . .
V1 V 0.91015(3) 0.37881(3) 0.007149(13) 0.01832(10) 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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C6 C1 C2 120.31(17) . . ?
C6 C1 S1 119.95(14) . . ?
C2 C1 S1 119.73(14) . . ?
C3 C2 C1 119.25(17) . . ?
C2 C3 C4 121.30(18) . . ?
C5 C4 C3 118.49(17) . . ?
C5 C4 C7 121.45(19) . . ?
C3 C4 C7 120.06(19) . . ?
C6 C5 C4 120.94(18) . . ?
C1 C6 C5 119.70(17) . . ?
S1 N1 V1 138.37(9) . . ?
S1 N1 V1 134.79(9) . 3_765 ?
V1 N1 V1 86.69(6) . 3_765 ?
C9 N2 C8 114.19(15) . . ?
C9 N2 V1 136.68(12) . . ?
C8 N2 V1 107.44(12) . . ?
C11 N3 C10 111.90(16) . . ?
C11 N3 V1 128.56(13) . . ?
C10 N3 V1 119.41(12) . . ?
O2 S1 O1 116.96(8) . . ?
O2 S1 N1 109.60(8) . . ?
O1 S1 N1 110.42(8) . . ?
O2 S1 C1 107.70(8) . . ?
O1 S1 C1 107.33(8) . . ?
N1 S1 C1 103.97(7) . . ?
N2 V1 N3 114.16(7) . . ?
N2 V1 N1 106.45(6) . . ?
N3 V1 N1 110.26(6) . . ?
N2 V1 N1 117.09(6) . 3_765 ?
N3 V1 N1 113.14(6) . 3_765 ?
N1 V1 N1 93.31(6) . 3_765 ?
N2 V1 V1 122.65(5) . 3_765 ?
N3 V1 V1 122.60(5) . 3_765 ?
N1 V1 V1 47.38(4) . 3_765 ?
N1 V1 V1 45.93(4) 3_765 3_765 ?
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 C6 1.382(3) . ?
C1 C2 1.386(2) . ?
C1 S1 1.7678(18) . ?
C2 C3 1.380(3) . ?
C3 C4 1.389(3) . ?
C4 C5 1.385(3) . ?
C4 C7 1.509(3) . ?
C5 C6 1.382(3) . ?
C8 N2 1.460(2) . ?
C9 N2 1.449(2) . ?
C10 N3 1.459(2) . ?
C11 N3 1.453(2) . ?
N1 S1 1.6000(14) . ?
N1 V1 1.8731(14) . ?
N1 V1 1.9183(14) 3_765 ?
N2 V1 1.8107(15) . ?
N3 V1 1.8349(15) . ?
O1 S1 1.4409(13) . ?
O2 S1 1.4379(13) . ?
V1 N1 1.9183(14) 3_765 ?
V1 V1 2.6027(6) 3_765 ?
