#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:47:51 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179263 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/83/4318328.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_4318328
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            'C10 H17 Cl4 N3 V'
_chemical_formula_weight         372.01
_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                109.261(5)
_cell_angle_beta                 100.005(5)
_cell_angle_gamma                117.271(5)
_cell_formula_units_Z            2
_cell_length_a                   9.879(5)
_cell_length_b                   10.247(5)
_cell_length_c                   10.334(5)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_volume                     809.3(7)
_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 0.936
_diffrn_measured_fraction_theta_max 0.936
_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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5927
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    1.259
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.25
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             378
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.832
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2175
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1191P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1587
_reflns_number_gt                1791
_reflns_number_total             2175
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020312y_3.cif
_cod_data_source_block           (3d)
_cod_database_code               4318328
#BEGIN Tags that were not found in dictionaries:
_cell_measurement_2theta_min     4.9
_cell_measurement_2theta_max     52.0
_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
C1 C -0.0656(6) 0.1807(5) 0.2464(5) 0.0278(10) Uani 1 1 d . . .
C2 C -0.0387(6) 0.0871(5) 0.3089(5) 0.0292(10) Uani 1 1 d . . .
C3 C -0.1656(7) -0.0388(6) 0.3181(6) 0.0388(12) Uani 1 1 d . . .
H3 H -0.1459 -0.1036 0.3566 0.047 Uiso 1 1 calc R . .
C4 C -0.3231(7) -0.0706(6) 0.2707(6) 0.0429(13) Uani 1 1 d . . .
H4 H -0.4104 -0.1550 0.2801 0.052 Uiso 1 1 calc R . .
C5 C -0.3532(6) 0.0188(6) 0.2105(5) 0.0386(12) Uani 1 1 d . . .
H5 H -0.4608 -0.0028 0.1788 0.046 Uiso 1 1 calc R . .
C6 C -0.2256(6) 0.1408(5) 0.1961(5) 0.0299(10) Uani 1 1 d . . .
C21 C 0.3008(7) 0.2113(6) 0.1045(6) 0.0410(12) Uani 1 1 d . . .
H21A H 0.1975 0.1344 0.1081 0.062 Uiso 1 1 calc R . .
H21B H 0.3757 0.1741 0.1139 0.062 Uiso 1 1 calc R . .
H21C H 0.2774 0.2139 0.0096 0.062 Uiso 1 1 calc R . .
C22 C 0.5413(7) 0.4944(7) 0.2307(6) 0.0420(12) Uani 1 1 d . . .
H22A H 0.5967 0.6034 0.3175 0.063 Uiso 1 1 calc R . .
H22B H 0.5249 0.5059 0.1398 0.063 Uiso 1 1 calc R . .
H22C H 0.6097 0.4494 0.2361 0.063 Uiso 1 1 calc R . .
C31 C 0.2341(8) 0.7858(6) 0.2736(7) 0.0468(13) Uani 1 1 d . . .
H31A H 0.2767 0.7706 0.1948 0.070 Uiso 1 1 calc R . .
H31B H 0.3266 0.8593 0.3707 0.070 Uiso 1 1 calc R . .
H31C H 0.1716 0.8354 0.2608 0.070 Uiso 1 1 calc R . .
C32 C 0.0585(7) 0.6456(7) 0.3829(6) 0.0414(13) Uani 1 1 d . . .
H32A H -0.0179 0.5372 0.3750 0.062 Uiso 1 1 calc R . .
H32B H -0.0002 0.6990 0.3711 0.062 Uiso 1 1 calc R . .
H32C H 0.1498 0.7158 0.4806 0.062 Uiso 1 1 calc R . .
N1 N 0.0639(5) 0.3102(4) 0.2405(4) 0.0275(9) Uani 1 1 d . . .
N2 N 0.3794(5) 0.3802(5) 0.2286(5) 0.0296(9) Uani 1 1 d D . .
N3 N 0.1244(5) 0.6226(5) 0.2654(5) 0.0325(10) Uani 1 1 d D . .
Cl1 Cl 0.19886(16) 0.45104(16) 0.01138(13) 0.0394(4) Uani 1 1 d . . .
Cl2 Cl 0.41466(15) 0.66518(14) 0.48693(13) 0.0394(4) Uani 1 1 d . . .
Cl3 Cl 0.16064(16) 0.13616(15) 0.37776(15) 0.0397(4) Uani 1 1 d . . .
Cl4 Cl -0.26681(15) 0.24546(15) 0.11033(14) 0.0393(4) Uani 1 1 d . . .
V1 V 0.22301(9) 0.47219(8) 0.24605(8) 0.0250(3) Uani 1 1 d . . .
HN2 H 0.397(7) 0.369(7) 0.291(5) 0.030 Uiso 1 1 d D . .
HN3 H 0.052(6) 0.579(7) 0.204(6) 0.030 Uiso 1 1 d 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
C6 C1 N1 121.9(4) . . ?
C6 C1 C2 116.9(4) . . ?
N1 C1 C2 121.2(4) . . ?
C3 C2 C1 121.5(4) . . ?
C3 C2 Cl3 119.9(4) . . ?
C1 C2 Cl3 118.6(3) . . ?
C2 C3 C4 119.4(5) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 120.5(5) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 119.5(5) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C1 122.0(5) . . ?
C5 C6 Cl4 119.3(4) . . ?
C1 C6 Cl4 118.6(4) . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C1 N1 V1 176.0(3) . . ?
C22 N2 C21 109.8(4) . . ?
C22 N2 V1 115.1(3) . . ?
C21 N2 V1 115.5(3) . . ?
C22 N2 HN2 106(5) . . ?
C21 N2 HN2 103(5) . . ?
V1 N2 HN2 107(5) . . ?
C32 N3 C31 109.3(4) . . ?
C32 N3 V1 116.2(3) . . ?
C31 N3 V1 115.0(3) . . ?
C32 N3 HN3 99(5) . . ?
C31 N3 HN3 108(5) . . ?
V1 N3 HN3 108(5) . . ?
N1 V1 N3 97.86(18) . . ?
N1 V1 N2 98.18(17) . . ?
N3 V1 N2 163.96(17) . . ?
N1 V1 Cl2 111.99(14) . . ?
N3 V1 Cl2 87.61(12) . . ?
N2 V1 Cl2 86.40(12) . . ?
N1 V1 Cl1 112.31(13) . . ?
N3 V1 Cl1 86.21(13) . . ?
N2 V1 Cl1 87.71(12) . . ?
Cl2 V1 Cl1 135.69(6) . . ?
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 1.385(7) . ?
C1 N1 1.388(6) . ?
C1 C2 1.411(7) . ?
C2 C3 1.373(7) . ?
C2 Cl3 1.734(5) . ?
C3 C4 1.390(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.370(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(7) . ?
C5 H5 0.9500 . ?
C6 Cl4 1.733(5) . ?
C21 N2 1.484(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 N2 1.478(7) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C31 N3 1.480(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 N3 1.476(7) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
N1 V1 1.656(4) . ?
N2 V1 2.151(4) . ?
N2 HN2 0.69(5) . ?
N3 V1 2.146(4) . ?
N3 HN3 0.69(5) . ?
Cl1 V1 2.3216(18) . ?
Cl2 V1 2.3185(16) . ?
