#------------------------------------------------------------------------------
#$Date: 2017-10-13 14:42:48 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/83/4318327.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_4318327
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_moiety         'C24 H42 N6 V2'
_chemical_formula_sum            'C24 H42 N6 V2'
_chemical_formula_weight         516.52
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.638(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2676(8)
_cell_length_b                   14.6499(11)
_cell_length_c                   18.1559(14)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    180(2)
_cell_volume                     2706.8(4)
_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 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  '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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19956
_diffrn_reflns_theta_full        26.17
_diffrn_reflns_theta_max         26.17
_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    0.712
_exptl_absorpt_correction_T_max  26.17
_exptl_absorpt_correction_T_min  2.26
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0511P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0901
_reflns_number_gt                3606
_reflns_number_total             5039
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020312y_2.cif
_cod_data_source_block           (1b)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4318327
_cell_measurement_2theta_min     4.5
_cell_measurement_2theta_max     52.0
_computing_corr_abs              DIFABS
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.7291(4) 0.2009(2) 0.5925(2) 0.0507(9) Uani 1 1 d . . .
H1A H 0.8036 0.2303 0.6227 0.076 Uiso 1 1 calc R . .
H1B H 0.6506 0.2391 0.5920 0.076 Uiso 1 1 calc R . .
H1C H 0.7491 0.1930 0.5416 0.076 Uiso 1 1 calc R . .
C2 C 0.8215(3) 0.0555(2) 0.62499(19) 0.0359(7) Uani 1 1 d . . .
H2A H 0.8410 0.0468 0.5741 0.054 Uiso 1 1 calc R . .
H2B H 0.8057 -0.0040 0.6469 0.054 Uiso 1 1 calc R . .
H2C H 0.8962 0.0853 0.6547 0.054 Uiso 1 1 calc R . .
C3 C 0.5660(3) -0.08627(18) 0.57324(15) 0.0303(6) Uani 1 1 d . . .
H3A H 0.6296 -0.1364 0.5786 0.045 Uiso 1 1 calc R . .
H3B H 0.6001 -0.0361 0.5456 0.045 Uiso 1 1 calc R . .
H3C H 0.4827 -0.1079 0.5462 0.045 Uiso 1 1 calc R . .
C4 C 0.4935(3) -0.12694(18) 0.68907(17) 0.0358(7) Uani 1 1 d . . .
H4A H 0.4000 -0.1362 0.6714 0.054 Uiso 1 1 calc R . .
H4B H 0.5045 -0.1107 0.7419 0.054 Uiso 1 1 calc R . .
H4C H 0.5419 -0.1833 0.6823 0.054 Uiso 1 1 calc R . .
C5 C 0.6478(3) 0.31689(19) 0.75846(19) 0.0374(7) Uani 1 1 d . . .
H5A H 0.6430 0.3675 0.7229 0.056 Uiso 1 1 calc R . .
H5B H 0.6935 0.2652 0.7391 0.056 Uiso 1 1 calc R . .
H5C H 0.6959 0.3365 0.8061 0.056 Uiso 1 1 calc R . .
C6 C 0.4418(3) 0.36659(19) 0.79148(19) 0.0386(7) Uani 1 1 d . . .
H6A H 0.4842 0.3901 0.8392 0.058 Uiso 1 1 calc R . .
H6B H 0.3521 0.3472 0.7965 0.058 Uiso 1 1 calc R . .
H6C H 0.4391 0.4147 0.7538 0.058 Uiso 1 1 calc R . .
C7 C 0.2868(3) 0.1764(2) 0.85347(15) 0.0384(7) Uani 1 1 d . . .
H7A H 0.2405 0.2315 0.8663 0.058 Uiso 1 1 calc R . .
H7B H 0.3792 0.1800 0.8753 0.058 Uiso 1 1 calc R . .
H7C H 0.2461 0.1226 0.8729 0.058 Uiso 1 1 calc R . .
C8 C 0.1468(3) 0.1467(2) 0.73900(17) 0.0335(6) Uani 1 1 d . . .
H8A H 0.1224 0.0865 0.7562 0.050 Uiso 1 1 calc R . .
H8B H 0.1438 0.1459 0.6848 0.050 Uiso 1 1 calc R . .
H8C H 0.0851 0.1926 0.7530 0.050 Uiso 1 1 calc R . .
C9 C 0.3188(2) 0.17228(16) 0.58680(12) 0.0191(5) Uani 1 1 d . . .
C10 C 0.3088(3) 0.26147(17) 0.55669(14) 0.0232(5) Uani 1 1 d . . .
C11 C 0.2055(3) 0.28198(19) 0.50156(15) 0.0305(6) Uani 1 1 d . . .
H11 H 0.1987 0.3418 0.4812 0.037 Uiso 1 1 calc R . .
C12 C 0.1132(3) 0.2177(2) 0.47599(16) 0.0357(7) Uani 1 1 d . . .
H12 H 0.0438 0.2328 0.4380 0.043 Uiso 1 1 calc R . .
C13 C 0.1220(3) 0.13064(19) 0.50602(15) 0.0305(6) Uani 1 1 d . . .
H13 H 0.0569 0.0866 0.4889 0.037 Uiso 1 1 calc R . .
C14 C 0.2241(2) 0.10636(17) 0.56067(13) 0.0209(5) Uani 1 1 d . . .
C15 C 0.4061(3) 0.33472(18) 0.58341(17) 0.0357(7) Uani 1 1 d . . .
H15A H 0.4848 0.3279 0.5588 0.054 Uiso 1 1 calc R . .
H15B H 0.4301 0.3293 0.6373 0.054 Uiso 1 1 calc R . .
H15C H 0.3667 0.3948 0.5716 0.054 Uiso 1 1 calc R . .
C16 C 0.2303(3) 0.01096(17) 0.59110(15) 0.0272(6) Uani 1 1 d . . .
H16A H 0.1467 -0.0202 0.5754 0.041 Uiso 1 1 calc R . .
H16B H 0.2464 0.0132 0.6455 0.041 Uiso 1 1 calc R . .
H16C H 0.3017 -0.0224 0.5723 0.041 Uiso 1 1 calc R . .
C17 C 0.6236(3) 0.03140(16) 0.83446(13) 0.0206(5) Uani 1 1 d . . .
C18 C 0.5500(3) -0.02824(18) 0.87423(15) 0.0282(6) Uani 1 1 d . . .
C19 C 0.6137(3) -0.0752(2) 0.93508(16) 0.0391(7) Uani 1 1 d . . .
H19 H 0.5645 -0.1151 0.9620 0.047 Uiso 1 1 calc R . .
C20 C 0.7469(3) -0.0653(2) 0.95739(15) 0.0399(8) Uani 1 1 d . . .
H20 H 0.7890 -0.0992 0.9984 0.048 Uiso 1 1 calc R . .
C21 C 0.8176(3) -0.00594(19) 0.91983(15) 0.0338(7) Uani 1 1 d . . .
H21 H 0.9090 0.0014 0.9357 0.041 Uiso 1 1 calc R . .
C22 C 0.7591(3) 0.04377(17) 0.85909(14) 0.0249(6) Uani 1 1 d . . .
C23 C 0.4044(3) -0.0433(2) 0.85442(18) 0.0379(7) Uani 1 1 d . . .
H23A H 0.3868 -0.1088 0.8477 0.057 Uiso 1 1 calc R . .
H23B H 0.3733 -0.0110 0.8082 0.057 Uiso 1 1 calc R . .
H23C H 0.3583 -0.0201 0.8945 0.057 Uiso 1 1 calc R . .
C24 C 0.8386(3) 0.1125(2) 0.82401(18) 0.0418(8) Uani 1 1 d . . .
H24A H 0.8156 0.1740 0.8393 0.063 Uiso 1 1 calc R . .
H24B H 0.8201 0.1074 0.7698 0.063 Uiso 1 1 calc R . .
H24C H 0.9322 0.1014 0.8399 0.063 Uiso 1 1 calc R . .
N1 N 0.4195(2) 0.14875(13) 0.64407(11) 0.0193(4) Uani 1 1 d . . .
N2 N 0.5648(2) 0.07782(13) 0.77069(11) 0.0198(4) Uani 1 1 d . . .
N3 N 0.7052(2) 0.11221(14) 0.62399(12) 0.0242(5) Uani 1 1 d . . .
N4 N 0.5441(2) -0.05389(14) 0.64706(12) 0.0245(5) Uani 1 1 d . . .
N5 N 0.5159(2) 0.28932(14) 0.76924(12) 0.0264(5) Uani 1 1 d . . .
N6 N 0.2786(2) 0.16922(14) 0.77298(12) 0.0245(5) Uani 1 1 d . . .
V1 V 0.56208(4) 0.07048(3) 0.66752(2) 0.01766(11) Uani 1 1 d . . .
V2 V 0.44544(4) 0.17376(3) 0.74634(2) 0.01832(11) 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 0.0000 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'
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
C14 C9 N1 119.2(2) . . ?
C14 C9 C10 119.5(2) . . ?
N1 C9 C10 121.3(2) . . ?
C11 C10 C9 119.1(2) . . ?
C11 C10 C15 119.3(2) . . ?
C9 C10 C15 121.6(2) . . ?
C12 C11 C10 121.4(3) . . ?
C11 C12 C13 119.5(2) . . ?
C12 C13 C14 121.3(2) . . ?
C13 C14 C9 119.1(2) . . ?
C13 C14 C16 119.4(2) . . ?
C9 C14 C16 121.4(2) . . ?
N2 C17 C18 121.2(2) . . ?
N2 C17 C22 119.6(2) . . ?
C18 C17 C22 119.2(2) . . ?
C19 C18 C17 119.0(3) . . ?
C19 C18 C23 117.7(3) . . ?
C17 C18 C23 123.3(2) . . ?
C20 C19 C18 121.7(3) . . ?
C21 C20 C19 119.3(3) . . ?
C20 C21 C22 121.7(3) . . ?
C21 C22 C17 119.1(3) . . ?
C21 C22 C24 119.3(3) . . ?
C17 C22 C24 121.5(2) . . ?
C9 N1 V1 142.81(17) . . ?
C9 N1 V2 132.56(17) . . ?
V1 N1 V2 83.70(8) . . ?
C17 N2 V1 137.96(17) . . ?
C17 N2 V2 138.59(18) . . ?
V1 N2 V2 83.40(8) . . ?
C1 N3 C2 109.6(2) . . ?
C1 N3 V1 130.1(2) . . ?
C2 N3 V1 120.03(18) . . ?
C4 N4 C3 110.5(2) . . ?
C4 N4 V1 130.51(19) . . ?
C3 N4 V1 118.37(17) . . ?
C6 N5 C5 110.7(2) . . ?
C6 N5 V2 124.61(19) . . ?
C5 N5 V2 124.30(18) . . ?
C8 N6 C7 111.7(2) . . ?
C8 N6 V2 138.16(19) . . ?
C7 N6 V2 109.22(17) . . ?
N3 V1 N1 109.96(9) . . ?
N3 V1 N4 107.41(10) . . ?
N1 V1 N4 120.14(9) . . ?
N3 V1 N2 119.88(9) . . ?
N1 V1 N2 95.73(9) . . ?
N4 V1 N2 104.08(9) . . ?
N3 V1 V2 120.69(7) . . ?
N1 V1 V2 48.37(6) . . ?
N4 V1 V2 131.66(7) . . ?
N2 V1 V2 48.40(6) . . ?
N6 V2 N5 108.70(10) . . ?
N6 V2 N1 103.77(9) . . ?
N5 V2 N1 113.41(10) . . ?
N6 V2 N2 120.77(9) . . ?
N5 V2 N2 113.89(9) . . ?
N1 V2 N2 95.11(9) . . ?
N6 V2 V1 131.50(7) . . ?
N5 V2 V1 118.46(8) . . ?
N1 V2 V1 47.93(6) . . ?
N2 V2 V1 48.20(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 N3 1.453(4) . ?
C2 N3 1.453(3) . ?
C3 N4 1.467(3) . ?
C4 N4 1.450(3) . ?
C5 N5 1.451(4) . ?
C6 N5 1.451(4) . ?
C7 N6 1.456(3) . ?
C8 N6 1.448(3) . ?
C9 C14 1.407(3) . ?
C9 N1 1.408(3) . ?
C9 C10 1.415(3) . ?
C10 C11 1.391(3) . ?
C10 C15 1.502(4) . ?
C11 C12 1.372(4) . ?
C12 C13 1.386(4) . ?
C13 C14 1.391(3) . ?
C14 C16 1.501(3) . ?
C17 N2 1.408(3) . ?
C17 C18 1.415(4) . ?
C17 C22 1.415(4) . ?
C18 C19 1.389(4) . ?
C18 C23 1.507(4) . ?
C19 C20 1.381(5) . ?
C20 C21 1.371(5) . ?
C21 C22 1.390(4) . ?
C22 C24 1.492(4) . ?
N1 V1 1.864(2) . ?
N1 V2 1.877(2) . ?
N2 V1 1.873(2) . ?
N2 V2 1.878(2) . ?
N3 V1 1.862(2) . ?
N4 V1 1.864(2) . ?
N5 V2 1.866(2) . ?
N6 V2 1.842(2) . ?
V1 V2 2.4955(6) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30661062
