#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:52:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179214 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/42/4314290.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_4314290
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         'C56 H48 N8 V2'
_chemical_formula_sum            'C56 H48 N8 V2'
_chemical_formula_weight         934.90
_chemical_melting_point          ?
_chemical_name_systematic
;
 tetrakis(anilinopyridyl-N,N')divanadium(II,II), benzene solvate
;
_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                97.989(2)
_cell_angle_beta                 109.990(2)
_cell_angle_gamma                101.325(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9082(10)
_cell_length_b                   10.1633(10)
_cell_length_c                   12.7609(13)
_cell_measurement_reflns_used    6277
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      27.528
_cell_measurement_theta_min      2.274
_cell_volume                     1154.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 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      213(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_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  0.0128
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7930
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.8499
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             486
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0447P)²+0.4391P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                4651
_reflns_number_total             4987
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic034646esi20030610_035606_6.cif
_cod_data_source_block           compound5
_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_database_code               4314290
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 0.51428(2) 0.57567(2) 0.561651(17) 0.02129(8) Uani 1 1 d . . .
N1 N 0.42910(13) 0.44897(12) 0.65896(10) 0.0262(2) Uani 1 1 d . . .
N2 N 0.40299(13) 0.27757(11) 0.51062(10) 0.0256(2) Uani 1 1 d . . .
N3 N 0.28912(13) 0.58830(12) 0.48746(10) 0.0266(2) Uani 1 1 d . . .
N4 N 0.71775(13) 0.56148(12) 0.66686(9) 0.0262(2) Uani 1 1 d . . .
C1 C 0.42579(16) 0.49308(16) 0.76240(12) 0.0311(3) Uani 1 1 d . . .
H16A H 0.4557 0.5884 0.7936 0.037 Uiso 1 1 calc R . .
C2 C 0.38105(17) 0.40643(17) 0.82490(12) 0.0353(3) Uani 1 1 d . . .
H15A H 0.3794 0.4411 0.8966 0.042 Uiso 1 1 calc R . .
C3 C 0.33834(17) 0.26559(17) 0.77825(13) 0.0356(3) Uani 1 1 d . . .
H14A H 0.3076 0.2033 0.8187 0.043 Uiso 1 1 calc R . .
C4 C 0.34103(17) 0.21743(15) 0.67311(13) 0.0318(3) Uani 1 1 d . . .
H13A H 0.3117 0.1223 0.6415 0.038 Uiso 1 1 calc R . .
C5 C 0.38810(15) 0.31154(14) 0.61228(11) 0.0257(3) Uani 1 1 d . . .
C6 C 0.33480(15) 0.14170(14) 0.44284(11) 0.0265(3) Uani 1 1 d . . .
C7 C 0.18413(17) 0.07810(16) 0.41339(14) 0.0366(3) Uani 1 1 d . . .
H8A H 0.1270 0.1229 0.4441 0.044 Uiso 1 1 calc R . .
C8 C 0.1183(2) -0.05000(18) 0.33967(17) 0.0471(4) Uani 1 1 d . . .
H9A H 0.0173 -0.0920 0.3214 0.057 Uiso 1 1 calc R . .
C9 C 0.2001(2) -0.11674(17) 0.29263(16) 0.0474(4) Uani 1 1 d . . .
H10A H 0.1548 -0.2035 0.2421 0.057 Uiso 1 1 calc R . .
C10 C 0.3486(2) -0.05507(17) 0.32044(15) 0.0424(4) Uani 1 1 d . . .
H11A H 0.4044 -0.0999 0.2883 0.051 Uiso 1 1 calc R . .
C11 C 0.41625(17) 0.07272(15) 0.39559(13) 0.0324(3) Uani 1 1 d . . .
H12A H 0.5179 0.1131 0.4148 0.039 Uiso 1 1 calc R . .
C12 C 0.22335(17) 0.66162(15) 0.54233(13) 0.0331(3) Uani 1 1 d . . .
H7A H 0.2790 0.7087 0.6188 0.040 Uiso 1 1 calc R . .
C13 C 0.08060(18) 0.67129(18) 0.49296(15) 0.0396(4) Uani 1 1 d . . .
H6A H 0.0395 0.7247 0.5337 0.048 Uiso 1 1 calc R . .
C14 C -0.00177(17) 0.59926(18) 0.38028(15) 0.0388(3) Uani 1 1 d . . .
H5A H -0.1004 0.6033 0.3439 0.047 Uiso 1 1 calc R . .
C15 C 0.06042(16) 0.52234(16) 0.32204(13) 0.0328(3) Uani 1 1 d . . .
H4A H 0.0045 0.4737 0.2460 0.039 Uiso 1 1 calc R . .
C16 C 0.20951(15) 0.51660(14) 0.37710(11) 0.0258(3) Uani 1 1 d . . .
C17 C 0.77139(15) 0.61531(15) 0.78614(11) 0.0275(3) Uani 1 1 d . . .
C18 C 0.80548(17) 0.53310(17) 0.86565(13) 0.0363(3) Uani 1 1 d . . .
H18A H 0.7998 0.4400 0.8404 0.044 Uiso 1 1 calc R . .
C19 C 0.84764(19) 0.5875(2) 0.98167(14) 0.0451(4) Uani 1 1 d . . .
H19A H 0.8713 0.5312 1.0342 0.054 Uiso 1 1 calc R . .
C20 C 0.85506(18) 0.7231(2) 1.02023(13) 0.0477(4) Uani 1 1 d . . .
H22A H 0.8837 0.7594 1.0988 0.057 Uiso 1 1 calc R . .
C21 C 0.82018(19) 0.80551(19) 0.94273(14) 0.0447(4) Uani 1 1 d . . .
H20A H 0.8246 0.8980 0.9687 0.054 Uiso 1 1 calc R . .
C22 C 0.77846(17) 0.75218(16) 0.82615(13) 0.0348(3) Uani 1 1 d . . .
H21A H 0.7549 0.8091 0.7741 0.042 Uiso 1 1 calc R . .
C1S C 0.1955(2) 0.7980(2) 0.93717(19) 0.0576(5) Uani 1 1 d . . .
H1SA H 0.1228 0.7720 0.9675 0.069 Uiso 1 1 calc R . .
C2S C 0.1631(3) 0.8577(2) 0.84505(19) 0.0592(5) Uani 1 1 d . . .
H2SA H 0.0686 0.8728 0.8120 0.071 Uiso 1 1 calc R . .
C3S C 0.2706(3) 0.8956(2) 0.80089(18) 0.0610(6) Uani 1 1 d . . .
H3SA H 0.2491 0.9361 0.7373 0.073 Uiso 1 1 calc R . .
C4S C 0.4103(3) 0.8737(2) 0.85051(19) 0.0617(6) Uani 1 1 d . . .
H4SA H 0.4837 0.9002 0.8209 0.074 Uiso 1 1 calc R . .
C5S C 0.4413(2) 0.8135(2) 0.94265(17) 0.0553(5) Uani 1 1 d . . .
H5SA H 0.5357 0.7982 0.9761 0.066 Uiso 1 1 calc R . .
C6S C 0.3341(2) 0.7756(2) 0.98587(18) 0.0538(5) Uani 1 1 d . . .
H6SA H 0.3552 0.7342 1.0490 0.065 Uiso 1 1 calc R . .
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
V1 V1 N2 93.81(3) 2_666 2_666 ?
V1 V1 N4 95.63(3) 2_666 . ?
N2 V1 N4 95.55(5) 2_666 . ?
V1 V1 N3 92.88(3) 2_666 . ?
N2 V1 N3 94.68(5) 2_666 . ?
N4 V1 N3 166.21(4) . . ?
V1 V1 N1 95.63(3) 2_666 . ?
N2 V1 N1 170.52(4) 2_666 . ?
N4 V1 N1 84.37(5) . . ?
N3 V1 N1 84.02(4) . . ?
C1 N1 C5 119.49(12) . . ?
C1 N1 V1 126.05(10) . . ?
C5 N1 V1 114.20(9) . . ?
C5 N2 C6 119.38(11) . . ?
C5 N2 V1 121.47(9) . 2_666 ?
C6 N2 V1 118.09(9) . 2_666 ?
C12 N3 C16 119.21(12) . . ?
C12 N3 V1 124.43(10) . . ?
C16 N3 V1 116.36(9) . . ?
C16 N4 C17 120.09(11) 2_666 . ?
C16 N4 V1 118.83(9) 2_666 . ?
C17 N4 V1 120.46(9) . . ?
N1 C1 C2 123.64(14) . . ?
C1 C2 C3 117.61(13) . . ?
C4 C3 C2 120.11(14) . . ?
C3 C4 C5 119.91(14) . . ?
N2 C5 N1 114.84(12) . . ?
N2 C5 C4 125.86(13) . . ?
N1 C5 C4 119.24(12) . . ?
C11 C6 C7 118.24(13) . . ?
C11 C6 N2 119.35(13) . . ?
C7 C6 N2 122.18(13) . . ?
C8 C7 C6 120.70(15) . . ?
C7 C8 C9 120.45(16) . . ?
C10 C9 C8 119.52(15) . . ?
C9 C10 C11 120.49(15) . . ?
C10 C11 C6 120.60(15) . . ?
N3 C12 C13 123.76(14) . . ?
C12 C13 C14 117.70(14) . . ?
C15 C14 C13 120.31(14) . . ?
C14 C15 C16 119.70(14) . . ?
N4 C16 N3 114.33(12) 2_666 . ?
N4 C16 C15 126.23(13) 2_666 . ?
N3 C16 C15 119.31(13) . . ?
C22 C17 C18 118.24(14) . . ?
C22 C17 N4 119.18(13) . . ?
C18 C17 N4 122.33(13) . . ?
C19 C18 C17 120.69(16) . . ?
C20 C19 C18 120.53(16) . . ?
C19 C20 C21 119.59(15) . . ?
C20 C21 C22 120.38(17) . . ?
C17 C22 C21 120.57(16) . . ?
C2S C1S C6S 120.46(19) . . ?
C1S C2S C3S 119.4(2) . . ?
C2S C3S C4S 120.0(2) . . ?
C5S C4S C3S 120.05(19) . . ?
C4S C5S C6S 119.8(2) . . ?
C5S C6S C1S 120.3(2) . . ?
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 1.9425(4) 2_666 ?
V1 N2 2.0412(11) 2_666 ?
V1 N4 2.0506(11) . ?
V1 N3 2.1429(12) . ?
V1 N1 2.1555(11) . ?
N1 C1 1.3473(17) . ?
N1 C5 1.3606(18) . ?
N2 C5 1.3601(17) . ?
N2 C6 1.4190(17) . ?
N2 V1 2.0412(11) 2_666 ?
N3 C12 1.3520(18) . ?
N3 C16 1.3660(17) . ?
N4 C16 1.3569(17) 2_666 ?
N4 C17 1.4141(17) . ?
C1 C2 1.375(2) . ?
C2 C3 1.391(2) . ?
C3 C4 1.374(2) . ?
C4 C5 1.4191(19) . ?
C6 C11 1.394(2) . ?
C6 C7 1.399(2) . ?
C7 C8 1.383(2) . ?
C8 C9 1.383(3) . ?
C9 C10 1.379(3) . ?
C10 C11 1.389(2) . ?
C12 C13 1.367(2) . ?
C13 C14 1.393(2) . ?
C14 C15 1.373(2) . ?
C15 C16 1.4195(19) . ?
C16 N4 1.3569(17) 2_666 ?
C17 C22 1.393(2) . ?
C17 C18 1.398(2) . ?
C18 C19 1.390(2) . ?
C19 C20 1.376(3) . ?
C20 C21 1.382(3) . ?
C21 C22 1.395(2) . ?
C1S C2S 1.368(3) . ?
C1S C6S 1.379(3) . ?
C2S C3S 1.381(3) . ?
C3S C4S 1.388(3) . ?
C4S C5S 1.370(3) . ?
C5S C6S 1.371(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 V1 V1 N3 -10.86(5) . . 2_666 2_666 ?
N1 V1 V1 N2 -0.84(4) . . 2_666 . ?
