#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:47:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179263 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/83/4318331.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_4318331
loop_
_publ_author_name
'Christian Lorber'
'Robert Choukroun'
'Bruno Donnadieu'
_publ_contact_author             'Dr Christian Lorber'
_publ_contact_author_address
;
Laboratoire de Chimie de Coordination
UPR-CNRS 8241
205, route de Narbonne
31077 Toulouse cedex, France
;
_publ_contact_author_email       ' lorber@lcc-toulouse.fr'
_publ_section_title
;
 Synthesis and Structure of a Series of New d1-Aryl Imido-Vanadium(IV)
 Complexes Stabilized by N-Donor Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4217
_journal_page_last               4226
_journal_paper_doi               10.1021/ic020312y
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C19 H22 Cl4 N4 V'
_chemical_formula_weight         499.15
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.152(5)
_cell_angle_beta                 112.847(5)
_cell_angle_gamma                96.685(5)
_cell_formula_units_Z            2
_cell_length_a                   9.916(5)
_cell_length_b                   11.723(5)
_cell_length_c                   12.082(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_volume                     1163.1(9)
_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    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.893
_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  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11148
_diffrn_reflns_theta_full        26.12
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.520
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0509P)²+0.5512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                3832
_reflns_number_total             4130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020312y_6.cif
_cod_data_source_block           (7c)
_cod_database_code               4318331
#BEGIN Tags that were not found in dictionaries:
_cell_measurement_2theta_min     4.3
_cell_measurement_2theta_max     52.1
_computing_corr_abs              DIFABS
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
V1 V 0.75475(3) 0.23589(3) 0.56936(3) 0.02704(11) Uani 1 1 d . . .
Cl1 Cl 0.52133(5) 0.20021(5) 0.58363(5) 0.03870(14) Uani 1 1 d . . .
Cl2 Cl 0.85376(5) 0.45182(4) 0.73578(5) 0.03490(13) Uani 1 1 d . . .
N1 N 0.85604(17) 0.17574(15) 0.67058(16) 0.0318(3) Uani 1 1 d . . .
N2 N 0.65902(16) 0.32548(15) 0.43117(15) 0.0297(3) Uani 1 1 d . . .
N3 N 0.92134(16) 0.27403(15) 0.50714(16) 0.0295(3) Uani 1 1 d . . .
N4 N 0.64505(18) 0.05199(16) 0.39489(17) 0.0353(4) Uani 1 1 d . . .
C1 C 0.9548(2) 0.14304(19) 0.76297(19) 0.0345(4) Uani 1 1 d . . .
C2 C 0.9184(3) 0.0222(2) 0.7577(2) 0.0434(5) Uani 1 1 d . . .
H2 H 0.8242 -0.0386 0.6894 0.052 Uiso 1 1 calc R . .
C3 C 1.0183(4) -0.0096(3) 0.8510(3) 0.0622(7) Uani 1 1 d . . .
H3 H 0.9922 -0.0918 0.8473 0.075 Uiso 1 1 calc R . .
C4 C 1.1549(4) 0.0768(4) 0.9488(3) 0.0782(9) Uani 1 1 d . . .
H4 H 1.2235 0.0543 1.0127 0.094 Uiso 1 1 calc R . .
C5 C 1.1930(4) 0.1955(4) 0.9548(3) 0.0791(9) Uani 1 1 d . . .
H5 H 1.2886 0.2546 1.0225 0.095 Uiso 1 1 calc R . .
C6 C 1.0935(3) 0.2308(3) 0.8630(2) 0.0560(6) Uani 1 1 d . . .
H6 H 1.1200 0.3138 0.8685 0.067 Uiso 1 1 calc R . .
C7 C 0.5276(2) 0.3564(2) 0.4025(2) 0.0375(4) Uani 1 1 d . . .
H7 H 0.4670 0.3376 0.4420 0.045 Uiso 1 1 calc R . .
C8 C 0.4759(2) 0.4140(2) 0.3183(2) 0.0432(5) Uani 1 1 d . . .
H8 H 0.3829 0.4359 0.3016 0.052 Uiso 1 1 calc R . .
C9 C 0.5623(3) 0.4390(2) 0.2593(2) 0.0451(5) Uani 1 1 d . . .
H9 H 0.5287 0.4770 0.1994 0.054 Uiso 1 1 calc R . .
C10 C 0.6983(2) 0.4085(2) 0.2878(2) 0.0402(5) Uani 1 1 d . . .
H10 H 0.7593 0.4250 0.2477 0.048 Uiso 1 1 calc R . .
C11 C 0.7447(2) 0.35338(17) 0.37556(18) 0.0290(4) Uani 1 1 d . . .
C12 C 0.8919(2) 0.32414(17) 0.41792(18) 0.0288(4) Uani 1 1 d . . .
C13 C 0.9964(2) 0.3493(2) 0.3734(2) 0.0376(4) Uani 1 1 d . . .
H13 H 0.9734 0.3842 0.3103 0.045 Uiso 1 1 calc R . .
C14 C 1.1337(2) 0.3231(2) 0.4216(2) 0.0441(5) Uani 1 1 d . . .
H14 H 1.2065 0.3397 0.3919 0.053 Uiso 1 1 calc R . .
C15 C 1.1647(2) 0.2729(2) 0.5128(2) 0.0430(5) Uani 1 1 d . . .
H15 H 1.2592 0.2547 0.5477 0.052 Uiso 1 1 calc R . .
C16 C 1.0558(2) 0.24951(19) 0.5528(2) 0.0361(4) Uani 1 1 d . . .
H16 H 1.0772 0.2144 0.6157 0.043 Uiso 1 1 calc R . .
C17 C 0.5200(3) 0.0401(3) 0.2714(3) 0.0601(7) Uani 1 1 d . . .
H17A H 0.4461 0.0804 0.2917 0.090 Uiso 1 1 calc R . .
H17B H 0.4690 -0.0499 0.2110 0.090 Uiso 1 1 calc R . .
H17C H 0.5616 0.0820 0.2291 0.090 Uiso 1 1 calc R . .
C18 C 0.7503(3) -0.0176(2) 0.3639(3) 0.0492(5) Uani 1 1 d . . .
H18A H 0.8272 -0.0170 0.4453 0.074 Uiso 1 1 calc R . .
H18B H 0.8012 0.0235 0.3266 0.074 Uiso 1 1 calc R . .
H18C H 0.6923 -0.1055 0.2992 0.074 Uiso 1 1 calc R . .
C1S C 0.7850(3) 0.3487(3) 0.9545(3) 0.0543(6) Uani 1 1 d . . .
H1S1 H 0.8828 0.4168 1.0019 0.065 Uiso 1 1 calc R . .
H1S2 H 0.7585 0.3100 0.8591 0.065 Uiso 1 1 calc R . .
Cl1S Cl 0.64177(10) 0.41453(10) 0.97437(8) 0.0802(3) Uani 1 1 d . . .
Cl2S Cl 0.80816(8) 0.23284(6) 1.01567(6) 0.05862(18) Uani 1 1 d . . .
H4N H 0.607(3) 0.012(2) 0.430(2) 0.041(6) Uiso 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 0.0000 0.0000 '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 V1 N3 95.71(7) . . ?
N1 V1 N4 93.94(8) . . ?
N3 V1 N4 88.82(7) . . ?
N1 V1 N2 169.40(7) . . ?
N3 V1 N2 73.79(6) . . ?
N4 V1 N2 87.39(7) . . ?
N1 V1 Cl1 100.23(6) . . ?
N3 V1 Cl1 163.35(5) . . ?
N4 V1 Cl1 85.35(5) . . ?
N2 V1 Cl1 90.35(5) . . ?
N1 V1 Cl2 95.46(7) . . ?
N3 V1 Cl2 89.47(5) . . ?
N4 V1 Cl2 170.57(5) . . ?
N2 V1 Cl2 83.22(6) . . ?
Cl1 V1 Cl2 93.73(3) . . ?
C1 N1 V1 171.74(14) . . ?
C7 N2 C11 117.94(16) . . ?
C7 N2 V1 125.90(13) . . ?
C11 N2 V1 116.13(12) . . ?
C16 N3 C12 118.11(16) . . ?
C16 N3 V1 122.32(13) . . ?
C12 N3 V1 119.57(12) . . ?
C17 N4 C18 109.8(2) . . ?
C17 N4 V1 119.93(15) . . ?
C18 N4 V1 115.50(13) . . ?
C17 N4 H4N 108.5(15) . . ?
C18 N4 H4N 104.7(16) . . ?
V1 N4 H4N 96.3(16) . . ?
N1 C1 C6 119.97(19) . . ?
N1 C1 C2 120.82(18) . . ?
C6 C1 C2 119.21(19) . . ?
C3 C2 C1 120.3(2) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 120.3(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.1(2) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C6 120.9(3) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C1 C6 C5 119.2(2) . . ?
C1 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
N2 C7 C8 123.25(19) . . ?
N2 C7 H7 118.4 . . ?
C8 C7 H7 118.4 . . ?
C9 C8 C7 118.34(19) . . ?
C9 C8 H8 120.8 . . ?
C7 C8 H8 120.8 . . ?
C8 C9 C10 119.37(19) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
C9 C10 C11 119.11(19) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
N2 C11 C10 121.94(17) . . ?
N2 C11 C12 115.00(15) . . ?
C10 C11 C12 123.03(17) . . ?
N3 C12 C13 121.56(17) . . ?
N3 C12 C11 115.41(15) . . ?
C13 C12 C11 123.00(17) . . ?
C14 C13 C12 119.32(19) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C15 C14 C13 119.40(18) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 118.56(19) . . ?
C14 C15 H15 120.7 . . ?
C16 C15 H15 120.7 . . ?
N3 C16 C15 123.05(19) . . ?
N3 C16 H16 118.5 . . ?
C15 C16 H16 118.5 . . ?
N4 C17 H17A 109.5 . . ?
N4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Cl1S C1S Cl2S 111.84(14) . . ?
Cl1S C1S H1S1 109.2 . . ?
Cl2S C1S H1S1 109.2 . . ?
Cl1S C1S H1S2 109.2 . . ?
Cl2S C1S H1S2 109.2 . . ?
H1S1 C1S H1S2 107.9 . . ?
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
V1 N1 1.6754(16) . ?
V1 N3 2.1255(17) . ?
V1 N4 2.1947(19) . ?
V1 N2 2.2363(16) . ?
V1 Cl1 2.3866(12) . ?
V1 Cl2 2.4075(10) . ?
N1 C1 1.373(2) . ?
N2 C7 1.340(2) . ?
N2 C11 1.346(2) . ?
N3 C16 1.339(2) . ?
N3 C12 1.351(2) . ?
N4 C17 1.471(3) . ?
N4 C18 1.479(3) . ?
N4 H4N 0.88(3) . ?
C1 C6 1.390(3) . ?
C1 C2 1.394(3) . ?
C2 C3 1.378(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.367(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.368(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.379(3) . ?
C7 H7 0.9500 . ?
C8 C9 1.375(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.379(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.472(3) . ?
C12 C13 1.386(3) . ?
C13 C14 1.375(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.372(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.379(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C1S Cl1S 1.750(3) . ?
C1S Cl2S 1.753(3) . ?
C1S H1S1 0.9900 . ?
C1S H1S2 0.9900 . ?
