#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/39/4343985.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_4343985
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            'C38 H42 Cl2 N6 O6 V2'
_chemical_formula_weight         851.56
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.365(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.6604(7)
_cell_length_b                   15.3134(16)
_cell_length_c                   18.6871(19)
_cell_measurement_temperature    100
_cell_volume                     1900.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16.0288
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.910
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.1371
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34224
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         34.81
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.251
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.423
_refine_diff_density_min         -0.497
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.934
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         7518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0460
_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)+(0.0644P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1262
_reflns_number_gt                3916
_reflns_number_total             7518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00571_si_007.cif
_cod_data_source_block           V2a
_cod_depositor_comments
'Adding full bibliography for 4343981--4343988.cif.'
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4343985
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
V V 0.55059(5) 0.17868(2) 0.829821(18) 0.01509(9) Uani 1 1 d .
Cl Cl 0.57870(8) 0.09449(3) 0.72467(3) 0.02111(12) Uani 1 1 d .
O1 O 0.6630(2) 0.08176(9) 0.88660(8) 0.0188(3) Uani 1 1 d .
O2 O 0.7256(2) 0.25004(9) 0.82434(8) 0.0197(3) Uani 1 1 d .
N1 N 0.2400(2) 0.12152(11) 0.84515(8) 0.0154(3) Uani 1 1 d .
N2 N 0.4711(2) 0.23127(11) 0.92970(9) 0.0168(4) Uani 1 1 d .
N3 N 0.3311(3) 0.25603(11) 0.76689(9) 0.0164(3) Uani 1 1 d .
O3 O 0.9799(3) 0.08368(13) 0.57660(14) 0.0560(6) Uani 1 1 d .
C4 C 0.2551(3) 0.02841(13) 0.86666(11) 0.0193(4) Uani 1 1 d .
H4A H 0.3134 -0.0045 0.8290 0.023 Uiso 1 1 calc R
H4B H 0.1208 0.0057 0.8716 0.023 Uiso 1 1 calc R
C2 C 0.3807(3) 0.01479(13) 0.93602(11) 0.0166(4) Uani 1 1 d .
C8 C 0.0546(4) 0.34125(14) 0.67395(12) 0.0251(5) Uani 1 1 d .
H8 H -0.0373 0.3694 0.6418 0.030 Uiso 1 1 calc R
C15 C 0.5694(3) 0.29661(14) 1.04275(12) 0.0247(5) Uani 1 1 d .
H15 H 0.6682 0.3238 1.0728 0.030 Uiso 1 1 calc R
C11 C 0.1395(3) 0.17334(13) 0.89988(11) 0.0177(4) Uani 1 1 d .
H11A H 0.0576 0.2186 0.8760 0.021 Uiso 1 1 calc R
H11B H 0.0512 0.1354 0.9248 0.021 Uiso 1 1 calc R
C1 C 0.5822(3) 0.04286(12) 0.94116(11) 0.0173(4) Uani 1 1 d .
C6 C 0.1545(3) 0.21842(13) 0.74617(10) 0.0161(4) Uani 1 1 d .
C7 C 0.0111(3) 0.25888(14) 0.69958(11) 0.0200(4) Uani 1 1 d .
H7 H -0.1106 0.2316 0.6859 0.024 Uiso 1 1 calc R
C12 C 0.2891(3) 0.21423(13) 0.95301(11) 0.0175(4) Uani 1 1 d .
C3 C 0.3007(3) -0.02784(13) 0.99377(11) 0.0181(4) Uani 1 1 d .
H3 H 0.1676 -0.0467 0.9892 0.022 Uiso 1 1 calc R
C9 C 0.2337(4) 0.38141(14) 0.69613(12) 0.0245(5) Uani 1 1 d .
H9 H 0.2626 0.4372 0.6802 0.029 Uiso 1 1 calc R
C10 C 0.3693(3) 0.33719(13) 0.74239(12) 0.0212(5) Uani 1 1 d .
H10 H 0.4908 0.3639 0.7572 0.025 Uiso 1 1 calc R
C5 C 0.1218(3) 0.12860(13) 0.77544(10) 0.0168(4) Uani 1 1 d .
H5A H -0.0200 0.1195 0.7816 0.020 Uiso 1 1 calc R
H5B H 0.1654 0.0848 0.7425 0.020 Uiso 1 1 calc R
C13 C 0.2392(3) 0.23933(14) 1.02046(11) 0.0228(5) Uani 1 1 d .
H13 H 0.1113 0.2280 1.0351 0.027 Uiso 1 1 calc R
C16 C 0.6093(3) 0.27134(14) 0.97511(11) 0.0212(4) Uani 1 1 d .
H16 H 0.7366 0.2821 0.9598 0.025 Uiso 1 1 calc R
C14 C 0.3809(4) 0.28124(15) 1.06584(12) 0.0270(5) Uani 1 1 d .
H14 H 0.3498 0.2989 1.1113 0.032 Uiso 1 1 calc R
C18 C 0.9465(4) 0.00876(17) 0.59215(15) 0.0417(7) Uani 1 1 d .
C17 C 0.7473(5) -0.0335(2) 0.57505(18) 0.0594(9) Uani 1 1 d .
H17A H 0.6565 0.0078 0.5513 0.089 Uiso 1 1 calc R
H17B H 0.6939 -0.0528 0.6186 0.089 Uiso 1 1 calc R
H17C H 0.7631 -0.0826 0.5442 0.089 Uiso 1 1 calc R
C19 C 1.1087(7) -0.0464(2) 0.6290(2) 0.0873(14) Uani 1 1 d .
H19A H 1.2293 -0.0124 0.6372 0.131 Uiso 1 1 calc R
H19B H 1.1348 -0.0956 0.5993 0.131 Uiso 1 1 calc R
H19C H 1.0661 -0.0666 0.6740 0.131 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'
Cl Cl 0.1484 0.1585 '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_3
O2 V O1 107.65(7) .
O2 V N2 91.62(7) .
O1 V N2 85.52(6) .
O2 V N3 93.25(7) .
O1 V N3 159.10(6) .
N2 V N3 93.80(6) .
O2 V N1 159.53(7) .
O1 V N1 87.37(6) .
N2 V N1 75.40(6) .
N3 V N1 72.31(6) .
O2 V Cl 102.35(6) .
O1 V Cl 89.17(5) .
N2 V Cl 165.99(5) .
N3 V Cl 86.56(5) .
N1 V Cl 91.43(5) .
C1 O1 V 126.85(12) .
C5 N1 C4 109.31(15) .
C5 N1 C11 109.24(15) .
C4 N1 C11 110.52(15) .
C5 N1 V 106.80(12) .
C4 N1 V 111.03(12) .
C11 N1 V 109.86(12) .
C12 N2 C16 118.20(18) .
C12 N2 V 119.97(13) .
C16 N2 V 121.18(14) .
C6 N3 C10 118.66(18) .
C6 N3 V 117.69(13) .
C10 N3 V 123.40(14) .
N1 C4 C2 112.88(16) .
C3 C2 C1 120.45(18) .
C3 C2 C4 120.64(18) .
C1 C2 C4 118.87(18) .
C9 C8 C7 120.0(2) .
C16 C15 C14 119.1(2) .
C12 C11 N1 111.61(16) .
O1 C1 C2 121.65(18) .
O1 C1 C3 120.25(19) 3_657
C2 C1 C3 118.09(18) 3_657
N3 C6 C7 122.44(19) .
N3 C6 C5 115.88(17) .
C7 C6 C5 121.67(19) .
C8 C7 C6 118.0(2) .
N2 C12 C13 121.79(19) .
N2 C12 C11 116.05(18) .
C13 C12 C11 121.98(19) .
C2 C3 C1 121.45(19) 3_657
C8 C9 C10 118.7(2) .
N3 C10 C9 122.1(2) .
N1 C5 C6 107.85(16) .
C14 C13 C12 119.3(2) .
N2 C16 C15 122.6(2) .
C15 C14 C13 119.0(2) .
O3 C18 C17 122.5(3) .
O3 C18 C19 120.5(3) .
C17 C18 C19 117.0(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V O2 1.6064(15) .
V O1 1.9407(14) .
V N2 2.1367(17) .
V N3 2.1587(17) .
V N1 2.2841(17) .
V Cl 2.3701(6) .
O1 C1 1.329(2) .
N1 C5 1.474(2) .
N1 C4 1.483(3) .
N1 C11 1.493(3) .
N2 C12 1.344(3) .
N2 C16 1.351(3) .
N3 C6 1.340(3) .
N3 C10 1.355(3) .
O3 C18 1.208(3) .
C4 C2 1.503(3) .
C2 C3 1.400(3) .
C2 C1 1.405(3) .
C8 C9 1.378(3) .
C8 C7 1.387(3) .
C15 C16 1.367(3) .
C15 C14 1.378(3) .
C11 C12 1.490(3) .
C1 C3 1.413(3) 3_657
C6 C7 1.388(3) .
C6 C5 1.502(3) .
C12 C13 1.383(3) .
C3 C1 1.413(3) 3_657
C9 C10 1.379(3) .
C13 C14 1.379(3) .
C18 C17 1.489(4) .
C18 C19 1.497(5) .
