#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/39/4343988.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_4343988
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 H45.9 Cl2 N6 O12.45 V2'
_chemical_formula_weight         886.70
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90.000(4)
_cell_angle_beta                 90.000(3)
_cell_angle_gamma                120.000(5)
_cell_formula_units_Z            9
_cell_length_a                   24.9740(11)
_cell_length_b                   24.9740(14)
_cell_length_c                   17.5048(6)
_cell_measurement_temperature    100(2)
_cell_volume                     9455.1(9)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measurement_device_type  'KM4 XCALIBUR2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42805
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.246
_diffrn_reflns_theta_min         3.263
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       plate
_exptl_crystal_F_000             4117
_exptl_crystal_size_max          0.3210
_exptl_crystal_size_mid          0.1562
_exptl_crystal_size_min          0.0845
_refine_diff_density_max         1.363
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         6055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0881P)²+31.1333P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5291
_reflns_number_total             6055
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b00571_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4343981--4343988.cif.'
_cod_original_cell_volume        9455.0(9)
_cod_original_formula_sum        'C32 H45.90 Cl2 N6 O12.45 V2'
_cod_database_code               4343988
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.29672(2) 0.02741(2) 0.34690(2) 0.01969(11) Uani 1 1 d . . . . .
Cl1 Cl 0.35518(2) 0.04198(2) 0.23648(3) 0.02566(13) Uani 1 1 d . . . . .
O2 O 0.35037(7) 0.06065(7) 0.40949(9) 0.0270(3) Uani 1 1 d . . . . .
O1 O 0.27248(6) -0.05812(6) 0.35485(9) 0.0220(3) Uani 1 1 d . . . . .
N1 N 0.20997(8) -0.00338(7) 0.27243(10) 0.0204(3) Uani 1 1 d . . . . .
N2 N 0.22440(8) 0.00521(8) 0.42702(11) 0.0240(3) Uani 1 1 d . . . . .
C3 C 0.17734(9) -0.11542(8) 0.28695(11) 0.0190(3) Uani 1 1 d . . . . .
N3 N 0.29553(9) 0.10852(8) 0.31647(11) 0.0265(4) Uani 1 1 d . . . . .
C2 C 0.20959(9) -0.16231(8) 0.38768(11) 0.0193(3) Uani 1 1 d . . . . .
H2 H 0.2388 -0.1587 0.4233 0.023 Uiso 1 1 calc R U . . .
C4 C 0.19235(9) -0.06276(9) 0.23294(11) 0.0210(4) Uani 1 1 d . . . . .
H4A H 0.2261 -0.0569 0.2000 0.025 Uiso 1 1 calc R U . . .
H4B H 0.1567 -0.0738 0.2008 0.025 Uiso 1 1 calc R U . . .
C13 C 0.26637(12) 0.16104(11) 0.22619(15) 0.0332(5) Uani 1 1 d . . . . .
H13 H 0.2445 0.1597 0.1826 0.040 Uiso 1 1 calc R U . . .
C15 C 0.33419(15) 0.21689(11) 0.32943(17) 0.0415(6) Uani 1 1 d . . . . .
H15 H 0.3583 0.2535 0.3561 0.050 Uiso 1 1 calc R U . . .
C12 C 0.26399(10) 0.10762(9) 0.25362(13) 0.0265(4) Uani 1 1 d . . . . .
C1 C 0.22151(9) -0.10997(8) 0.34275(11) 0.0186(3) Uani 1 1 d . . . . .
C10 C 0.23436(12) 0.00504(11) 0.50324(13) 0.0302(4) Uani 1 1 d . . . . .
H10 H 0.2743 0.0185 0.5205 0.036 Uiso 1 1 calc R U . . .
C8 C 0.12723(13) -0.03579(12) 0.52986(16) 0.0379(5) Uani 1 1 d . . . . .
H8 H 0.0946 -0.0494 0.5643 0.045 Uiso 1 1 calc R U . . .
C9 C 0.18711(13) -0.01445(13) 0.55588(15) 0.0367(5) Uani 1 1 d . . . . .
H9 H 0.1952 -0.0133 0.6079 0.044 Uiso 1 1 calc R U . . .
C5 C 0.15773(10) -0.00853(10) 0.31903(13) 0.0250(4) Uani 1 1 d . . . . .
H5A H 0.1195 -0.0441 0.3020 0.030 Uiso 1 1 calc R U . . .
H5B H 0.1542 0.0280 0.3110 0.030 Uiso 1 1 calc R U . . .
C6 C 0.16625(10) -0.01503(9) 0.40215(13) 0.0248(4) Uani 1 1 d . . . . .
C14 C 0.30189(14) 0.21627(11) 0.26486(16) 0.0385(6) Uani 1 1 d . . . . .
H14 H 0.3040 0.2525 0.2476 0.046 Uiso 1 1 calc R U . . .
C7 C 0.11666(11) -0.03658(11) 0.45281(15) 0.0329(5) Uani 1 1 d . . . . .
H7 H 0.0767 -0.0514 0.4345 0.039 Uiso 1 1 calc R U . . .
C11 C 0.22786(10) 0.04627(9) 0.21426(13) 0.0250(4) Uani 1 1 d . . . . .
H11A H 0.1912 0.0430 0.1906 0.030 Uiso 1 1 calc R U . . .
H11B H 0.2529 0.0423 0.1747 0.030 Uiso 1 1 calc R U . . .
C16 C 0.32995(13) 0.16226(11) 0.35360(15) 0.0349(5) Uani 1 1 d . . . . .
H16 H 0.3516 0.1626 0.3970 0.042 Uiso 1 1 calc R U . . .
O1W O 0.99576(9) 0.88597(10) 0.2637(2) 0.0581(7) Uani 1 1 d . . . A 10
O6 O 1.0000 1.0000 0.3437(5) 0.140(3) Uani 1 3 d S T P B 1
O7 O 0.0000 0.0000 0.5000 0.139(5) Uani 1 6 d S T P C 2
O1P O 0.9593(4) 1.0071(4) 0.3262(5) 0.043(3) Uiso 0.238(10) 1 d . . P D 3
O2P O 1.0372(6) 0.8836(7) 0.1497(8) 0.137(7) Uiso 0.49(2) 1 d . . P E 4
O5P O 0.0755(6) 0.0047(7) 0.1487(8) 0.116(7) Uiso 0.347(16) 1 d . . P F 5
O3P O 0.9877(5) 0.8966(5) 0.3041(6) 0.085(4) Uiso 0.392(14) 1 d . . P G 6
O4P O 0.2886(10) -0.1878(11) 0.5513(14) 0.137(11) Uiso 0.29(2) 1 d . . P H 7
O6P O 0.4900(11) 0.3482(11) 0.3103(14) 0.053(9) Uiso 0.111(14) 1 d . . P I 8
O7P O 0.5122(12) 0.3533(11) 0.3533(17) 0.41(2) Uiso 0.86(5) 1 d . . P J 9
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'
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
O2 V1 O1 104.16(7) .
O2 V1 N3 94.85(8) .
O1 V1 N3 160.52(7) .
O2 V1 N2 93.73(8) .
O1 V1 N2 84.70(7) .
N3 V1 N2 89.94(7) .
O2 V1 N1 163.96(7) .
O1 V1 N1 87.06(6) .
N3 V1 N1 73.46(7) .
N2 V1 N1 75.66(7) .
O2 V1 Cl1 100.90(6) .
O1 V1 Cl1 93.34(5) .
N3 V1 Cl1 87.09(6) .
N2 V1 Cl1 165.26(6) .
N1 V1 Cl1 89.66(5) .
C1 O1 V1 134.88(12) .
C5 N1 C4 111.01(16) .
C5 N1 C11 109.37(15) .
C4 N1 C11 109.14(16) .
C5 N1 V1 110.83(13) .
C4 N1 V1 110.78(11) .
C11 N1 V1 105.55(12) .
C6 N2 C10 118.72(19) .
C6 N2 V1 119.94(15) .
C10 N2 V1 121.00(15) .
C2 C3 C1 118.84(16) 16_545
C2 C3 C4 120.72(17) 16_545
C1 C3 C4 120.18(16) .
C16 N3 C12 119.21(19) .
C16 N3 V1 121.84(17) .
C12 N3 V1 118.64(14) .
C3 C2 C1 121.59(17) 16_545
N1 C4 C3 113.49(16) .
C14 C13 C12 119.0(2) .
C16 C15 C14 118.9(2) .
N3 C12 C13 121.5(2) .
N3 C12 C11 116.11(17) .
C13 C12 C11 122.4(2) .
O1 C1 C2 118.37(17) .
O1 C1 C3 122.06(16) .
C2 C1 C3 119.56(16) .
N2 C10 C9 122.1(2) .
C7 C8 C9 119.3(2) .
C10 C9 C8 118.9(2) .
N1 C5 C6 112.19(17) .
N2 C6 C7 121.4(2) .
N2 C6 C5 117.35(18) .
C7 C6 C5 121.0(2) .
C15 C14 C13 119.3(2) .
C8 C7 C6 119.5(2) .
N1 C11 C12 108.22(17) .
N3 C16 C15 122.2(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O2 1.6038(16) .
V1 O1 1.9118(14) .
V1 N3 2.1090(18) .
V1 N2 2.1295(18) .
V1 N1 2.3063(17) .
V1 Cl1 2.3387(6) .
O1 C1 1.301(2) .
N1 C5 1.489(3) .
N1 C4 1.489(2) .
N1 C11 1.490(2) .
N2 C6 1.349(3) .
N2 C10 1.358(3) .
C3 C2 1.371(3) 16_545
C3 C1 1.428(3) .
C3 C4 1.507(3) .
N3 C16 1.345(3) .
N3 C12 1.347(3) .
C2 C3 1.371(3) 16_545
C2 C1 1.424(2) .
C13 C14 1.387(4) .
C13 C12 1.391(3) .
C15 C16 1.381(3) .
C15 C14 1.384(4) .
C12 C11 1.501(3) .
C10 C9 1.380(3) .
C8 C7 1.373(4) .
C8 C9 1.390(4) .
C5 C6 1.491(3) .
C6 C7 1.394(3) .
