#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:52:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179214 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/42/4314288.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_4314288
loop_
_publ_author_name
'F. Albert Cotton'
'Elizabeth A. Hillard'
'Carlos A. Murillo'
'Xiaoping Wang'
_publ_section_title
;
 New Chemistry of the Triply Bonded Divanadium (V24+) Unit and Reduction
 to an Unprecedented V23+ Core
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6063
_journal_page_last               6070
_journal_paper_doi               10.1021/ic034646e
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C52 H36 Cl8 N8 V2'
_chemical_formula_sum            'C52 H36 Cl8 N8 V2'
_chemical_formula_weight         1158.37
_chemical_melting_point          ?
_chemical_name_systematic
;
 tetrakis(N,N'-di(p-chlorophenyl)formamidinate)divanadium(II,II)
;
_space_group_IT_number           70
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
_symmetry_space_group_name_H-M   'F d d d :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   26.5959(17)
_cell_length_b                   27.2378(17)
_cell_length_c                   29.7981(19)
_cell_measurement_reflns_used    6873
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.974
_cell_measurement_theta_min      2.54
_cell_volume                     21586(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELTXL v5.05 (Siemens, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART area detector'
_diffrn_measurement_method       /w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            27664
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.8424
_exptl_absorpt_correction_T_min  0.8100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       red
_exptl_crystal_F_000             9376
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0369
_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)+(0.0399P)²+74.0101P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                3467
_reflns_number_total             4772
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic034646esi20030610_035606_4.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

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      'F d d d'
_cod_database_code               4314288
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+3/4, -y+3/4, z'
'-x+3/4, y, -z+3/4'
'x, -y+3/4, -z+3/4'
'x, y+1/2, z+1/2'
'-x+3/4, -y+5/4, z+1/2'
'-x+3/4, y+1/2, -z+5/4'
'x, -y+5/4, -z+5/4'
'x+1/2, y, z+1/2'
'-x+5/4, -y+3/4, z+1/2'
'-x+5/4, y, -z+5/4'
'x+1/2, -y+3/4, -z+5/4'
'x+1/2, y+1/2, z'
'-x+5/4, -y+5/4, z'
'-x+5/4, y+1/2, -z+3/4'
'x+1/2, -y+5/4, -z+3/4'
'-x, -y, -z'
'x-3/4, y-3/4, -z'
'x-3/4, -y, z-3/4'
'-x, y-3/4, z-3/4'
'-x, -y+1/2, -z+1/2'
'x-3/4, y-1/4, -z+1/2'
'x-3/4, -y+1/2, z-1/4'
'-x, y-1/4, z-1/4'
'-x+1/2, -y, -z+1/2'
'x-1/4, y-3/4, -z+1/2'
'x-1/4, -y, z-1/4'
'-x+1/2, y-3/4, z-1/4'
'-x+1/2, -y+1/2, -z'
'x-1/4, y-1/4, -z'
'x-1/4, -y+1/2, z-3/4'
'-x+1/2, y-1/4, z-3/4'
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 0.1250 0.58876(2) 0.1250 0.02582(15) Uani 1 2 d S . .
V2 V 0.6250 0.58862(2) 0.1250 0.02981(16) Uani 1 2 d S . .
Cl1 Cl -0.07044(4) 0.41414(3) 0.05138(3) 0.0740(3) Uani 1 1 d . . .
Cl2 Cl 0.21838(4) 0.39487(3) -0.02206(3) 0.0801(3) Uani 1 1 d . . .
Cl3 Cl 0.44181(5) 0.39374(3) 0.08863(4) 0.0861(4) Uani 1 1 d . . .
Cl4 Cl 0.66235(4) 0.39937(4) -0.04868(5) 0.0972(4) Uani 1 1 d . . .
N1 N 0.06485(8) 0.58489(8) 0.07856(7) 0.0336(5) Uani 1 1 d . . .
N2 N 0.17617(8) 0.58140(7) 0.07319(7) 0.0334(5) Uani 1 1 d . . .
N3 N 0.54610(9) 0.58272(8) 0.12425(7) 0.0358(5) Uani 1 1 d . . .
N4 N 0.62556(9) 0.58258(7) 0.05405(7) 0.0346(5) Uani 1 1 d . . .
C1 C 0.03240(11) 0.54420(9) 0.07126(9) 0.0348(6) Uani 1 1 d . . .
C2 C -0.01765(11) 0.54606(11) 0.08481(10) 0.0434(7) Uani 1 1 d . . .
H2A H -0.0301 0.5745 0.0980 0.052 Uiso 1 1 calc R . .
C3 C -0.04920(13) 0.50606(11) 0.07887(11) 0.0513(8) Uani 1 1 d . . .
H3A H -0.0827 0.5076 0.0878 0.062 Uiso 1 1 calc R . .
C4 C -0.03031(13) 0.46412(11) 0.05963(10) 0.0484(8) Uani 1 1 d . . .
C5 C 0.01888(13) 0.46090(10) 0.04645(10) 0.0473(8) Uani 1 1 d . . .
H5A H 0.0312 0.4321 0.0339 0.057 Uiso 1 1 calc R . .
C6 C 0.05022(12) 0.50117(10) 0.05209(9) 0.0423(7) Uani 1 1 d . . .
H6A H 0.0836 0.4993 0.0429 0.051 Uiso 1 1 calc R . .
C7 C 0.19890(10) 0.62248(10) 0.06136(9) 0.0355(6) Uani 1 1 d . . .
H7A H 0.2250 0.6214 0.0406 0.043 Uiso 1 1 calc R . .
C8 C 0.18630(10) 0.53756(9) 0.04940(9) 0.0346(6) Uani 1 1 d . . .
C9 C 0.19100(11) 0.53625(11) 0.00289(9) 0.0437(7) Uani 1 1 d . . .
H9A H 0.1882 0.5651 -0.0136 0.052 Uiso 1 1 calc R . .
C10 C 0.19987(13) 0.49228(12) -0.01909(10) 0.0528(9) Uani 1 1 d . . .
H10A H 0.2031 0.4916 -0.0502 0.063 Uiso 1 1 calc R . .
C11 C 0.20383(12) 0.44975(11) 0.00522(11) 0.0488(8) Uani 1 1 d . . .
C12 C 0.19785(12) 0.44961(10) 0.05121(10) 0.0470(8) Uani 1 1 d . . .
H12A H 0.1997 0.4204 0.0673 0.056 Uiso 1 1 calc R . .
C13 C 0.18901(11) 0.49352(10) 0.07288(10) 0.0401(7) Uani 1 1 d . . .
H13A H 0.1848 0.4937 0.1039 0.048 Uiso 1 1 calc R . .
C15 C 0.51853(11) 0.53878(10) 0.11726(9) 0.0388(7) Uani 1 1 d . . .
C16 C 0.53361(11) 0.49590(10) 0.13805(9) 0.0395(7) Uani 1 1 d . . .
H16A H 0.5602 0.4969 0.1583 0.047 Uiso 1 1 calc R . .
C17 C 0.51035(12) 0.45160(10) 0.12962(10) 0.0443(7) Uani 1 1 d . . .
H17A H 0.5214 0.4232 0.1439 0.053 Uiso 1 1 calc R . .
C18 C 0.47113(14) 0.44964(11) 0.10036(12) 0.0560(9) Uani 1 1 d . . .
C19 C 0.45474(17) 0.49127(14) 0.07970(17) 0.0988(18) Uani 1 1 d . . .
H19A H 0.4279 0.4899 0.0598 0.119 Uiso 1 1 calc R . .
C20 C 0.47826(16) 0.53582(13) 0.08845(14) 0.0825(14) Uani 1 1 d . . .
H20A H 0.4665 0.5642 0.0746 0.099 Uiso 1 1 calc R . .
C21 C 0.6250 0.6250 0.03266(12) 0.0338(8) Uani 1 2 d S . .
H21A H 0.6250 0.6250 0.0015 0.041 Uiso 1 2 calc SR . .
C22 C 0.63349(10) 0.53962(10) 0.02790(9) 0.0341(6) Uani 1 1 d . . .
C23 C 0.60903(12) 0.49642(11) 0.03872(10) 0.0475(8) Uani 1 1 d . . .
H23A H 0.5861 0.4964 0.0623 0.057 Uiso 1 1 calc R . .
C24 C 0.61757(12) 0.45340(11) 0.01561(11) 0.0503(8) Uani 1 1 d . . .
H24A H 0.6009 0.4247 0.0235 0.060 Uiso 1 1 calc R . .
C25 C 0.65111(12) 0.45371(11) -0.01928(12) 0.0521(8) Uani 1 1 d . . .
C26 C 0.67574(12) 0.49601(12) -0.03125(12) 0.0586(9) Uani 1 1 d . . .
H26A H 0.6981 0.4959 -0.0553 0.070 Uiso 1 1 calc R . .
C27 C 0.66723(11) 0.53865(11) -0.00752(10) 0.0437(7) Uani 1 1 d . . .
H27A H 0.6844 0.5671 -0.0154 0.052 Uiso 1 1 calc R . .
C28 C 0.52169(15) 0.6250 0.1250 0.0380(9) Uani 1 2 d S . .
H28A H 0.4867 0.6250 0.1250 0.046 Uiso 1 2 calc SR . .
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
V1 V1 N2 95.56(6) 14_455 11_454 ?
V1 V1 N2 95.56(6) 14_455 . ?
N2 V1 N2 168.88(12) 11_454 . ?
V1 V1 N1 92.86(6) 14_455 11_454 ?
N2 V1 N1 90.25(9) 11_454 11_454 ?
N2 V1 N1 89.19(9) . 11_454 ?
V1 V1 N1 92.86(6) 14_455 . ?
N2 V1 N1 89.19(9) 11_454 . ?
N2 V1 N1 90.25(9) . . ?
N1 V1 N1 174.29(11) 11_454 . ?
V2 V2 N3 94.38(6) 14 . ?
V2 V2 N3 94.38(6) 14 11_554 ?
N3 V2 N3 171.24(12) . 11_554 ?
V2 V2 N4 94.45(6) 14 . ?
N3 V2 N4 89.46(9) . . ?
N3 V2 N4 89.86(9) 11_554 . ?
V2 V2 N4 94.45(6) 14 11_554 ?
N3 V2 N4 89.86(9) . 11_554 ?
N3 V2 N4 89.46(9) 11_554 11_554 ?
N4 V2 N4 171.10(11) . 11_554 ?
C7 N1 C1 117.2(2) 14_455 . ?
C7 N1 V1 114.76(17) 14_455 . ?
C1 N1 V1 126.70(16) . . ?
C7 N2 C8 119.7(2) . . ?
C7 N2 V1 114.75(17) . . ?
C8 N2 V1 125.54(17) . . ?
C28 N3 C15 118.9(3) . . ?
C28 N3 V2 115.0(2) . . ?
C15 N3 V2 125.54(18) . . ?
C21 N4 C22 117.2(2) . . ?
C21 N4 V2 114.42(18) . . ?
C22 N4 V2 127.69(17) . . ?
C6 C1 C2 118.5(3) . . ?
C6 C1 N1 120.9(3) . . ?
C2 C1 N1 120.5(3) . . ?
C3 C2 C1 120.9(3) . . ?
C4 C3 C2 119.0(3) . . ?
C5 C4 C3 121.5(3) . . ?
C5 C4 Cl1 119.6(3) . . ?
C3 C4 Cl1 118.9(3) . . ?
C4 C5 C6 119.3(3) . . ?
C1 C6 C5 120.8(3) . . ?
N2 C7 N1 121.0(2) . 14_455 ?
C13 C8 C9 118.3(2) . . ?
C13 C8 N2 119.1(2) . . ?
C9 C8 N2 122.5(2) . . ?
C10 C9 C8 120.5(3) . . ?
C11 C10 C9 119.6(3) . . ?
C10 C11 C12 121.3(3) . . ?
C10 C11 Cl2 119.7(2) . . ?
C12 C11 Cl2 119.1(2) . . ?
C13 C12 C11 118.8(3) . . ?
C12 C13 C8 121.4(3) . . ?
C20 C15 C16 117.2(3) . . ?
C20 C15 N3 122.9(3) . . ?
C16 C15 N3 119.8(2) . . ?
C17 C16 C15 121.9(3) . . ?
C18 C17 C16 119.7(3) . . ?
C17 C18 C19 120.1(3) . . ?
C17 C18 Cl3 120.3(2) . . ?
C19 C18 Cl3 119.5(3) . . ?
C18 C19 C20 119.9(3) . . ?
C15 C20 C19 121.3(3) . . ?
N4 C21 N4 122.3(3) . 14 ?
C23 C22 C27 117.8(3) . . ?
C23 C22 N4 120.2(2) . . ?
C27 C22 N4 122.0(2) . . ?
C24 C23 C22 122.0(3) . . ?
C25 C24 C23 118.8(3) . . ?
C24 C25 C26 120.9(3) . . ?
C24 C25 Cl4 119.2(3) . . ?
C26 C25 Cl4 120.0(3) . . ?
C25 C26 C27 119.7(3) . . ?
C26 C27 C22 120.9(3) . . ?
N3 C28 N3 121.2(4) 8_554 . ?
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 V1 1.9742(11) 14_455 ?
V1 N2 2.068(2) 11_454 ?
V1 N2 2.068(2) . ?
V1 N1 2.118(2) 11_454 ?
V1 N1 2.118(2) . ?
V2 V2 1.9820(12) 14 ?
V2 N3 2.105(2) . ?
V2 N3 2.105(2) 11_554 ?
V2 N4 2.121(2) . ?
V2 N4 2.121(2) 11_554 ?
Cl1 C4 1.747(3) . ?
Cl2 C11 1.745(3) . ?
Cl3 C18 1.746(3) . ?
Cl4 C25 1.746(3) . ?
N1 C7 1.321(3) 14_455 ?
N1 C1 1.421(3) . ?
N2 C7 1.320(3) . ?
N2 C8 1.415(3) . ?
N3 C28 1.322(3) . ?
N3 C15 1.419(3) . ?
N4 C21 1.320(3) . ?
N4 C22 1.421(3) . ?
C1 C6 1.387(4) . ?
C1 C2 1.392(4) . ?
C2 C3 1.387(4) . ?
C3 C4 1.373(4) . ?
C4 C5 1.369(5) . ?
C5 C6 1.388(4) . ?
C7 N1 1.321(3) 14_455 ?
C8 C13 1.390(4) . ?
C8 C9 1.392(4) . ?
C9 C10 1.385(4) . ?
C10 C11 1.370(4) . ?
C11 C12 1.380(4) . ?
C12 C13 1.380(4) . ?
C15 C20 1.375(4) . ?
C15 C16 1.382(4) . ?
C16 C17 1.379(4) . ?
C17 C18 1.361(4) . ?
C18 C19 1.362(5) . ?
C19 C20 1.390(5) . ?
C21 N4 1.320(3) 14 ?
C22 C23 1.383(4) . ?
C22 C27 1.386(4) . ?
C23 C24 1.378(4) . ?
C24 C25 1.370(4) . ?
C25 C26 1.373(5) . ?
C26 C27 1.378(4) . ?
C28 N3 1.322(3) 8_554 ?
