#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/39/4343982.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_4343982
loop_
_publ_author_name
'Stylianou, Marios'
'Drouza, Chryssoula'
'Giapintzakis, John'
'Athanasopoulos, Georgios I.'
'Keramidas, Anastasios D.'
_publ_section_title
;
 Aerial Oxidation of a V(IV)-Iminopyridine Hydroquinonate Complex: A Trap
 for the V(IV)-Semiquinonate Radical Intermediate.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7218
_journal_page_last               7229
_journal_paper_doi               10.1021/acs.inorgchem.5b00571
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C32 H30 N6 O6 V2'
_chemical_formula_weight         696.50
_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                97.637(10)
_cell_angle_beta                 101.977(11)
_cell_angle_gamma                102.252(11)
_cell_formula_units_Z            1
_cell_length_a                   6.5655(9)
_cell_length_b                   10.0810(13)
_cell_length_c                   11.7778(14)
_cell_measurement_temperature    100
_cell_volume                     732.32(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.697
_diffrn_measurement_device_type  'KM4 XCALIBUR2'
_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  0.0671
_diffrn_reflns_av_sigmaI/netI    0.0945
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9306
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.75
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.1524
_exptl_crystal_size_mid          0.1044
_exptl_crystal_size_min          0.0642
_refine_diff_density_max         1.202
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4414
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0787
_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)+(0.1257P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1998
_refine_ls_wR_factor_ref         0.2325
_reflns_number_gt                2757
_reflns_number_total             4414
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00571_si_008.cif
_cod_data_source_block           V4
_cod_depositor_comments
'Adding full bibliography for 4343981--4343988.cif.'
_cod_original_cell_volume        732.32(16)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4343982
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
V1 V 0.46862(10) 0.21958(6) 0.20930(5) 0.0190(2) Uani 1 1 d .
O2 O 0.3498(5) 0.3433(3) 0.1860(2) 0.0238(6) Uani 1 1 d .
O3 O 0.3044(4) 0.0747(3) 0.1310(2) 0.0228(6) Uani 1 1 d .
O1 O 0.4549(4) 0.2027(3) 0.3668(2) 0.0196(5) Uani 1 1 d .
N1 N 0.7408(5) 0.1092(3) 0.2472(2) 0.0171(6) Uani 1 1 d .
N2 N 0.7826(5) 0.3871(3) 0.2995(2) 0.0198(6) Uani 1 1 d .
N3 N 0.6304(5) 0.2514(3) 0.0697(3) 0.0198(6) Uani 1 1 d .
C2 C 0.4018(6) 0.1016(4) 0.5314(3) 0.0185(7) Uani 1 1 d .
H2 H 0.3342 0.1702 0.5521 0.022 Uiso 1 1 calc R
C10 C 0.7981(7) 0.5230(4) 0.3055(3) 0.0224(8) Uani 1 1 d .
H10 H 0.6757 0.5520 0.2756 0.027 Uiso 1 1 calc R
C11 C 0.8007(6) 0.0754(4) 0.1338(3) 0.0189(7) Uani 1 1 d .
H11A H 0.7045 -0.0106 0.0883 0.023 Uiso 1 1 calc R
H11B H 0.9457 0.0628 0.1498 0.023 Uiso 1 1 calc R
C9 C 0.9903(7) 0.6220(4) 0.3549(3) 0.0282(9) Uani 1 1 d .
H9 H 0.9960 0.7156 0.3603 0.034 Uiso 1 1 calc R
C7 C 1.1579(6) 0.4385(4) 0.3878(3) 0.0246(8) Uani 1 1 d .
H7 H 1.2789 0.4063 0.4137 0.030 Uiso 1 1 calc R
C12 C 0.7885(6) 0.1880(4) 0.0630(3) 0.0189(7) Uani 1 1 d .
C6 C 0.9586(6) 0.3468(4) 0.3404(3) 0.0188(7) Uani 1 1 d .
C3 C 0.5769(6) -0.0051(4) 0.3957(3) 0.0194(7) Uani 1 1 d .
C4 C 0.6526(6) -0.0230(4) 0.2838(3) 0.0198(7) Uani 1 1 d .
H4A H 0.7627 -0.0740 0.2943 0.024 Uiso 1 1 calc R
H4B H 0.5331 -0.0780 0.2205 0.024 Uiso 1 1 calc R
C15 C 0.7268(7) 0.3796(4) -0.0760(3) 0.0256(8) Uani 1 1 d .
H15 H 0.7013 0.4436 -0.1238 0.031 Uiso 1 1 calc R
C5 C 0.9289(6) 0.1938(4) 0.3391(3) 0.0188(7) Uani 1 1 d .
H5A H 1.0569 0.1673 0.3259 0.023 Uiso 1 1 calc R
H5B H 0.9121 0.1749 0.4157 0.023 Uiso 1 1 calc R
C16 C 0.5971(7) 0.3441(4) -0.0002(3) 0.0247(8) Uani 1 1 d .
H16 H 0.4839 0.3855 0.0025 0.030 Uiso 1 1 calc R
C13 C 0.9268(6) 0.2212(4) -0.0099(3) 0.0233(8) Uani 1 1 d .
H13 H 1.0388 0.1784 -0.0116 0.028 Uiso 1 1 calc R
C1 C 0.4778(6) 0.1006(4) 0.4275(3) 0.0181(7) Uani 1 1 d .
C14 C 0.8956(7) 0.3174(4) -0.0789(3) 0.0260(8) Uani 1 1 d .
H14 H 0.9871 0.3411 -0.1276 0.031 Uiso 1 1 calc R
C8 C 1.1734(7) 0.5776(4) 0.3958(3) 0.0267(8) Uani 1 1 d .
H8 H 1.3049 0.6412 0.4283 0.032 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'
O O 0.0106 0.0060 '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
O2 V1 O3 107.26(14) .
O2 V1 O1 102.57(12) .
O3 V1 O1 102.80(13) .
O2 V1 N3 92.05(12) .
O3 V1 N3 92.26(13) .
O1 V1 N3 154.63(12) .
O2 V1 N1 159.35(13) .
O3 V1 N1 90.32(12) .
O1 V1 N1 83.38(10) .
N3 V1 N1 76.15(11) .
O2 V1 N2 88.22(13) .
O3 V1 N2 160.74(13) .
O1 V1 N2 84.32(11) .
N3 V1 N2 75.42(11) .
N1 V1 N2 72.56(11) .
C1 O1 V1 131.6(2) .
C5 N1 C11 110.8(3) .
C5 N1 C4 110.5(3) .
C11 N1 C4 108.2(3) .
C5 N1 V1 112.6(2) .
C11 N1 V1 106.8(2) .
C4 N1 V1 107.8(2) .
C6 N2 C10 118.3(3) .
C6 N2 V1 118.4(2) .
C10 N2 V1 123.2(3) .
C12 N3 C16 119.2(3) .
C12 N3 V1 117.6(2) .
C16 N3 V1 122.7(3) .
C3 C2 C1 123.3(3) 2_656
N2 C10 C9 122.4(4) .
N1 C11 C12 111.1(3) .
C8 C9 C10 118.4(4) .
C8 C7 C6 118.9(4) .
N3 C12 C13 121.5(3) .
N3 C12 C11 116.1(3) .
C13 C12 C11 122.3(3) .
N2 C6 C7 122.9(4) .
N2 C6 C5 116.0(3) .
C7 C6 C5 121.0(3) .
C2 C3 C1 118.7(3) 2_656
C2 C3 C4 117.9(3) 2_656
C1 C3 C4 123.3(3) .
N1 C4 C3 114.3(3) .
C16 C15 C14 118.5(4) .
N1 C5 C6 112.7(3) .
N3 C16 C15 121.9(4) .
C14 C13 C12 119.1(4) .
O1 C1 C3 124.3(3) .
O1 C1 C2 117.7(3) .
C3 C1 C2 118.0(3) .
C13 C14 C15 119.7(4) .
C7 C8 C9 119.1(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O2 1.630(3) .
V1 O3 1.645(3) .
V1 O1 1.903(2) .
V1 N3 2.157(3) .
V1 N1 2.297(3) .
V1 N2 2.317(3) .
O1 C1 1.345(4) .
N1 C5 1.475(4) .
N1 C11 1.486(4) .
N1 C4 1.491(5) .
N2 C6 1.324(5) .
N2 C10 1.343(5) .
N3 C12 1.340(5) .
N3 C16 1.348(5) .
C2 C3 1.390(5) 2_656
C2 C1 1.415(5) .
C10 C9 1.390(6) .
C11 C12 1.501(5) .
C9 C8 1.386(6) .
C7 C8 1.373(6) .
C7 C6 1.388(5) .
C12 C13 1.395(5) .
C6 C5 1.511(5) .
C3 C2 1.390(5) 2_656
C3 C1 1.410(5) .
C3 C4 1.505(5) .
C15 C16 1.386(6) .
C15 C14 1.389(6) .
C13 C14 1.366(5) .
