#------------------------------------------------------------------------------
#$Date: 2015-08-05 20:39:17 +0300 (Wed, 05 Aug 2015) $
#$Revision: 152797 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/39/4343981.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_4343981
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 H50.16 Cl2 N6 O14.58 V2'
_chemical_formula_weight         925.07
_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
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   24.9994(5)
_cell_length_b                   24.9994(5)
_cell_length_c                   17.3225(4)
_cell_measurement_reflns_used    12836
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.8065
_cell_measurement_theta_min      3.0058
_cell_volume                     9375.6(3)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'KM4 XCALIBUR2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0977
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61155
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.866
_diffrn_reflns_theta_min         3.012
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             4326
_exptl_crystal_size_max          0.4278
_exptl_crystal_size_mid          0.2083
_exptl_crystal_size_min          0.0992
_refine_diff_density_max         1.693
_refine_diff_density_min         -1.192
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         8389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1131P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1731
_refine_ls_wR_factor_ref         0.1935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4294
_reflns_number_total             8389
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b00571_si_005.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4343981--4343988.cif.'
_cod_original_cell_volume        9375.6(4)
_cod_database_code               4343981
_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
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 0.73115(2) 0.02758(2) 0.84807(3) 0.02297(12) Uani 1 1 d . . . . .
Cl1 Cl 0.68735(3) 0.04153(3) 0.73714(4) 0.02936(16) Uani 1 1 d . . . . .
O2 O 0.71013(9) 0.06070(8) 0.91060(11) 0.0288(4) Uani 1 1 d . . . . .
O1 O 0.67041(8) -0.05791(8) 0.85692(10) 0.0233(4) Uani 1 1 d . . . . .
N2 N 0.78165(10) 0.00609(10) 0.92941(13) 0.0254(4) Uani 1 1 d . . . . .
N1 N 0.78733(9) -0.00303(9) 0.77364(12) 0.0226(4) Uani 1 1 d . . . . .
N3 N 0.81304(10) 0.10867(10) 0.81746(13) 0.0272(5) Uani 1 1 d . . . . .
C9 C 0.79965(15) -0.01235(14) 1.05990(18) 0.0374(7) Uani 1 1 d . . . . .
H9 H 0.7925 -0.0111 1.1124 0.045 Uiso 1 1 calc R U . . .
C2 C 0.62775(11) -0.16258(11) 0.88792(14) 0.0209(4) Uani 1 1 d . . . . .
H2 H 0.6018 -0.1592 0.9236 0.025 Uiso 1 1 calc R U . . .
C3 C 0.70792(11) -0.11498(11) 0.78767(13) 0.0197(4) Uani 1 1 d . . . . .
C13 C 0.89511(13) 0.16173(13) 0.72682(18) 0.0343(6) Uani 1 1 d . . . . .
H13 H 0.9163 0.1607 0.6833 0.041 Uiso 1 1 calc R U . . .
C15 C 0.88212(14) 0.21744(13) 0.83056(19) 0.0381(7) Uani 1 1 d . . . . .
H15 H 0.8945 0.2540 0.8575 0.046 Uiso 1 1 calc R U . . .
C1 C 0.66917(11) -0.10972(11) 0.84372(13) 0.0196(4) Uani 1 1 d . . . . .
C7 C 0.84883(14) -0.03377(13) 0.95588(18) 0.0350(6) Uani 1 1 d . . . . .
H7 H 0.8744 -0.0480 0.9376 0.042 Uiso 1 1 calc R U . . .
C6 C 0.82039(12) -0.01329(11) 0.90513(16) 0.0265(5) Uani 1 1 d . . . . .
C16 C 0.83175(13) 0.16283(12) 0.85467(18) 0.0333(6) Uani 1 1 d . . . . .
H16 H 0.8099 0.1632 0.8979 0.040 Uiso 1 1 calc R U . . .
C12 C 0.84403(12) 0.10826(12) 0.75424(17) 0.0291(6) Uani 1 1 d . . . . .
C8 C 0.83874(14) -0.03279(14) 1.03460(18) 0.0388(7) Uani 1 1 d . . . . .
H8 H 0.8581 -0.0457 1.0698 0.047 Uiso 1 1 calc R U . . .
C4 C 0.74586(11) -0.06216(11) 0.73356(14) 0.0226(5) Uani 1 1 d . . . . .
H4A H 0.7707 -0.0731 0.7013 0.027 Uiso 1 1 calc R U . . .
H4B H 0.7182 -0.0562 0.7000 0.027 Uiso 1 1 calc R U . . .
C5 C 0.83436(12) -0.00782(12) 0.82049(16) 0.0275(5) Uani 1 1 d . . . . .
H5A H 0.8744 0.0285 0.8115 0.033 Uiso 1 1 calc R U . . .
H5B H 0.8366 -0.0437 0.8038 0.033 Uiso 1 1 calc R U . . .
C10 C 0.77151(13) 0.00609(13) 1.00637(16) 0.0310(6) Uani 1 1 d . . . . .
H10 H 0.7446 0.0190 1.0235 0.037 Uiso 1 1 calc R U . . .
C14 C 0.91362(14) 0.21668(13) 0.76600(19) 0.0380(7) Uani 1 1 d . . . . .
H14 H 0.9474 0.2531 0.7485 0.046 Uiso 1 1 calc R U . . .
C11 C 0.81899(12) 0.04680(12) 0.71509(15) 0.0279(5) Uani 1 1 d . . . . .
H11A H 0.7900 0.0426 0.6751 0.033 Uiso 1 1 calc R U . . .
H11B H 0.8524 0.0436 0.6913 0.033 Uiso 1 1 calc R U . . .
O6 O 0.3333 0.6667 0.8171(3) 0.091(2) Uani 1 3 d S T P A 12
O5 O 0.44365(14) -0.22167(14) 0.9186(2) 0.0634(8) Uiso 1 1 d . . . B 8
O3 O 0.5059(2) -0.1441(2) 1.1888(4) 0.074(3) Uiso 0.626(14) 1 d . . P C 9
O4 O 0.5142(4) -0.2168(5) 1.0671(6) 0.288(5) Uani 1 1 d . . . D 10
O7 O 0.3333 0.6667 0.6667 0.188(6) Uani 1 6 d S T P E 11
O9 O 0.9827(8) 0.0921(9) 0.6363(10) 0.166(11) Uiso 0.35(2) 1 d . . P F 1
O8 O 0.4140(8) 0.8438(8) 0.1052(10) 0.118(8) Uiso 0.292(13) 1 d . . P G 2
O5P O 0.4320(3) -0.2256(3) 0.8696(4) 0.068(3) Uiso 0.458(12) 1 d . . P H 3
O3P O 0.4986(6) -0.1405(6) 1.1334(9) 0.107(6) Uiso 0.363(16) 1 d . . P I 4
O1P O 0.9160(6) 0.0010(6) 0.6218(7) 0.114(7) Uiso 0.352(14) 1 d . . P J 5
O6P O 1.0000 0.0000 0.5000 0.48(6) Uiso 0.87(11) 6 d S . P K 6
O2P O 0.2923(6) 0.6582(6) 0.8397(8) 0.057(5) Uiso 0.207(10) 1 d . . P L 7
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
_geom_angle_site_symmetry_3
O2 V1 O1 103.95(9) . .
O2 V1 N3 94.88(9) . .
O1 V1 N3 160.65(8) . .
O2 V1 N2 94.13(10) . .
O1 V1 N2 84.53(8) . .
N3 V1 N2 89.76(9) . .
O2 V1 N1 164.26(9) . .
O1 V1 N1 87.07(7) . .
N3 V1 N1 73.60(8) . .
N2 V1 N1 75.51(8) . .
O2 V1 Cl1 100.40(7) . .
O1 V1 Cl1 93.64(6) . .
N3 V1 Cl1 87.23(7) . .
N2 V1 Cl1 165.36(7) . .
N1 V1 Cl1 89.90(6) . .
C1 O1 V1 135.22(16) . .
C6 N2 C10 118.3(2) . .
C6 N2 V1 120.43(18) . .
C10 N2 V1 121.00(19) . .
C5 N1 C4 111.3(2) . .
C5 N1 C11 109.2(2) . .
C4 N1 C11 109.16(19) . .
C5 N1 V1 111.15(15) . .
C4 N1 V1 110.75(15) . .
C11 N1 V1 105.11(15) . .
C12 N3 C16 118.9(2) . .
C12 N3 V1 118.98(18) . .
C16 N3 V1 121.75(19) . .
C10 C9 C8 119.0(3) . .
C3 C2 C1 121.5(2) 16_646 .
C2 C3 C1 119.0(2) 16_646 .
C2 C3 C4 120.5(2) 16_646 .
C1 C3 C4 120.2(2) . .
C14 C13 C12 118.4(3) . .
C14 C15 C16 118.6(3) . .
O1 C1 C3 122.2(2) . .
O1 C1 C2 118.2(2) . .
C3 C1 C2 119.5(2) . .
C6 C7 C8 119.1(3) . .
N2 C6 C7 122.0(3) . .
N2 C6 C5 116.7(2) . .
C7 C6 C5 121.2(2) . .
N3 C16 C15 122.2(3) . .
N3 C12 C13 121.8(3) . .
N3 C12 C11 115.4(2) . .
C13 C12 C11 122.8(3) . .
C9 C8 C7 119.1(3) . .
N1 C4 C3 113.7(2) . .
N1 C5 C6 112.7(2) . .
N2 C10 C9 122.4(3) . .
C15 C14 C13 120.1(3) . .
N1 C11 C12 108.9(2) . .
O2P O2P O2P 60.001(4) 3_565 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O2 1.6030(19) .
V1 O1 1.9110(17) .
V1 N3 2.105(2) .
V1 N2 2.132(2) .
V1 N1 2.301(2) .
V1 Cl1 2.3226(8) .
O1 C1 1.300(3) .
N2 C6 1.348(3) .
N2 C10 1.357(4) .
N1 C5 1.482(3) .
N1 C4 1.487(3) .
N1 C11 1.490(3) .
N3 C12 1.344(4) .
N3 C16 1.354(4) .
C9 C10 1.375(4) .
C9 C8 1.381(5) .
C2 C3 1.375(3) 16_646
C2 C1 1.427(3) .
C3 C2 1.375(3) 16_646
C3 C1 1.423(3) .
C3 C4 1.506(3) .
C13 C14 1.388(4) .
C13 C12 1.391(4) .
C15 C14 1.373(5) .
C15 C16 1.380(4) .
C7 C6 1.380(4) .
C7 C8 1.389(4) .
C6 C5 1.497(4) .
C12 C11 1.500(4) .
O2P O2P 1.62(2) 3_565
O2P O2P 1.62(2) 2_665
