#------------------------------------------------------------------------------
#$Date: 2015-08-05 20:39:17 +0300 (Wed, 05 Aug 2015) $
#$Revision: 152797 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/39/4343983.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_4343983
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 H45.62 Cl2 N6 O12.31 V2'
_chemical_formula_weight         884.12
_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                   24.9734(4)
_cell_length_b                   24.9734(4)
_cell_length_c                   17.3106(5)
_cell_measurement_temperature    89(2)
_cell_volume                     9349.7(3)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      89(2)
_diffrn_detector_area_resol_mean 16.0288
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'KM4 XCALIBUR2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_laue_measured_fraction_full 0.985
_diffrn_reflns_laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45044
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.097
_diffrn_reflns_theta_min         3.263
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       rod
_exptl_crystal_F_000             4102
_exptl_crystal_size_max          0.4006
_exptl_crystal_size_mid          0.2199
_exptl_crystal_size_min          0.1011
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         6085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0542
_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)+(0.1197P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1565
_refine_ls_wR_factor_ref         0.1697
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4200
_reflns_number_total             6085
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b00571_si_004.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4343981--4343988.cif.'
_cod_original_cell_volume        9349.7(4)
_cod_database_code               4343983
_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 0.73134(2) 0.02772(2) 0.34826(2) 0.02342(13) Uani 1 1 d . . . . .
Cl1 Cl 0.68759(2) 0.04167(3) 0.23698(4) 0.02920(15) Uani 1 1 d . . . . .
O2 O 0.71029(7) 0.06097(7) 0.41089(11) 0.0294(4) Uani 1 1 d . . . . .
O1 O 0.67048(7) -0.05791(6) 0.35717(10) 0.0235(3) Uani 1 1 d . . . . .
N1 N 0.78774(8) -0.00283(8) 0.27357(12) 0.0231(4) Uani 1 1 d . . . . .
N2 N 0.78169(8) 0.00627(8) 0.43015(12) 0.0259(4) Uani 1 1 d . . . . .
N3 N 0.81327(9) 0.10919(8) 0.31782(13) 0.0285(4) Uani 1 1 d . . . . .
C2 C 0.62781(9) -0.16259(9) 0.38845(13) 0.0216(4) Uani 1 1 d . . . . .
H2 H 0.6020 -0.1592 0.4244 0.026 Uiso 1 1 calc R U . . .
O1W O 0.99805(10) 0.11025(11) 0.2530(3) 0.0741(10) Uani 1 1 d . . . A 9
C3 C 0.70800(9) -0.11507(9) 0.28749(13) 0.0206(4) Uani 1 1 d . . . . .
C7 C 0.89540(11) 0.16186(11) 0.22670(17) 0.0345(6) Uani 1 1 d . . . . .
H7 H 0.9167 0.1607 0.1833 0.041 Uiso 1 1 calc R U . . .
C14 C 0.83936(13) -0.03229(13) 0.53564(17) 0.0393(6) Uani 1 1 d . . . . .
H14 H 0.8588 -0.0452 0.5707 0.047 Uiso 1 1 calc R U . . .
C1 C 0.66924(9) -0.10964(9) 0.34399(13) 0.0206(4) Uani 1 1 d . . . . .
C9 C 0.88207(12) 0.21782(11) 0.33044(19) 0.0396(6) Uani 1 1 d . . . . .
H9 H 0.8941 0.2544 0.3571 0.048 Uiso 1 1 calc R U . . .
C4 C 0.74635(10) -0.06201(9) 0.23337(13) 0.0233(4) Uani 1 1 d . . . . .
H4A H 0.7713 -0.0729 0.2013 0.028 Uiso 1 1 calc R U . . .
H4B H 0.7188 -0.0560 0.1996 0.028 Uiso 1 1 calc R U . . .
C6 C 0.84418(10) 0.10842(10) 0.25455(15) 0.0288(5) Uani 1 1 d . . . . .
C12 C 0.82054(10) -0.01298(10) 0.40572(15) 0.0275(5) Uani 1 1 d . . . . .
C15 C 0.80016(12) -0.01177(12) 0.56104(18) 0.0374(6) Uani 1 1 d . . . . .
H15 H 0.7931 -0.0102 0.6135 0.045 Uiso 1 1 calc R U . . .
C10 C 0.83186(11) 0.16274(11) 0.35511(17) 0.0342(6) Uani 1 1 d . . . . .
H10 H 0.8104 0.1629 0.3989 0.041 Uiso 1 1 calc R U . . .
C13 C 0.84920(12) -0.03328(12) 0.45660(17) 0.0353(6) Uani 1 1 d . . . . .
H13 H 0.8748 -0.0475 0.4382 0.042 Uiso 1 1 calc R U . . .
C11 C 0.83477(10) -0.00765(10) 0.32081(15) 0.0279(5) Uani 1 1 d . . . . .
H11A H 0.8749 0.0286 0.3119 0.034 Uiso 1 1 calc R U . . .
H11B H 0.8370 -0.0436 0.3043 0.034 Uiso 1 1 calc R U . . .
C5 C 0.81965(10) 0.04702(10) 0.21505(15) 0.0276(5) Uani 1 1 d . . . . .
H5A H 0.7909 0.0428 0.1746 0.033 Uiso 1 1 calc R U . . .
H5B H 0.8534 0.0440 0.1917 0.033 Uiso 1 1 calc R U . . .
O7 O 1.0000 0.0000 0.3475(3) 0.0887(16) Uani 1 3 d S T P B 1
C8 C 0.91374(12) 0.21728(11) 0.26602(18) 0.0377(6) Uani 1 1 d . . . . .
H8 H 0.9474 0.2538 0.2485 0.045 Uiso 1 1 calc R U . . .
C16 C 0.77160(11) 0.00637(11) 0.50656(16) 0.0322(5) Uani 1 1 d . . . . .
H16 H 0.7444 0.0191 0.5235 0.039 Uiso 1 1 calc R U . . .
O2W O 0.9827(2) 0.1716(2) -0.0224(4) 0.070(2) Uiso 0.632(14) 1 d . . P C 2
O2A O 0.9721(5) 0.1643(5) 0.0313(9) 0.104(5) Uiso 0.368(14) 1 d . . P C 2
O5W O 1.0614(4) 0.1768(5) 0.1048(5) 0.250(4) Uani 1 1 d . . . D 3
O6 O 0.0000 0.0000 0.5000 0.252(11) Uani 1 6 d S T P E 4
O1P O 0.9668(5) -0.0400(5) 0.3264(7) 0.026(4) Uiso 0.146(8) 1 d . . P F 5
O2P O 0.9902(6) 0.0902(7) 0.3045(8) 0.048(5) Uiso 0.180(12) 1 d . . P G 6
O3P O 0.9128(8) -0.0021(8) 0.1225(10) 0.102(8) Uiso 0.244(15) 1 d . . P H 7
O4P O 0.9081(9) 0.0867(9) 0.0708(12) 0.028(6) Uiso 0.087(8) 1 d . . P I 8
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 103.96(8) . .
O2 V1 N3 94.61(8) . .
O1 V1 N3 160.92(7) . .
O2 V1 N2 93.88(9) . .
O1 V1 N2 84.51(7) . .
N3 V1 N2 89.94(8) . .
O2 V1 N1 164.22(8) . .
O1 V1 N1 87.17(6) . .
N3 V1 N1 73.76(7) . .
N2 V1 N1 75.83(7) . .
O2 V1 Cl1 100.48(7) . .
O1 V1 Cl1 93.67(5) . .
N3 V1 Cl1 87.15(6) . .
N2 V1 Cl1 165.52(6) . .
N1 V1 Cl1 89.75(5) . .
C1 O1 V1 135.19(13) . .
C11 N1 C4 111.25(17) . .
C11 N1 C5 109.14(17) . .
C4 N1 C5 109.14(18) . .
C11 N1 V1 110.91(15) . .
C4 N1 V1 110.83(13) . .
C5 N1 V1 105.37(13) . .
C16 N2 C12 118.5(2) . .
C16 N2 V1 121.18(16) . .
C12 N2 V1 120.04(17) . .
C10 N3 C6 119.4(2) . .
C10 N3 V1 121.82(18) . .
C6 N3 V1 118.47(15) . .
C3 C2 C1 121.36(19) 16_645 .
C2 C3 C1 119.16(18) 16_645 .
C2 C3 C4 120.32(19) 16_645 .
C1 C3 C4 120.23(18) . .
C6 C7 C8 118.0(3) . .
C15 C14 C13 118.8(2) . .
O1 C1 C2 118.19(19) . .
O1 C1 C3 122.33(18) . .
C2 C1 C3 119.47(18) . .
C8 C9 C10 118.7(3) . .
N1 C4 C3 113.74(19) . .
N3 C6 C7 121.8(2) . .
N3 C6 C5 116.18(19) . .
C7 C6 C5 122.1(2) . .
N2 C12 C13 121.9(2) . .
N2 C12 C11 117.1(2) . .
C13 C12 C11 120.9(2) . .
C14 C15 C16 118.6(3) . .
N3 C10 C9 122.1(3) . .
C12 C13 C14 119.4(2) . .
N1 C11 C12 112.60(18) . .
N1 C5 C6 108.6(2) . .
C9 C8 C7 120.0(2) . .
N2 C16 C15 122.6(2) . .
O1P O1P O1P 60.001(2) 3_765 2_645
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
V1 O2 1.6055(17) .
V1 O1 1.9122(15) .
V1 N3 2.1072(19) .
V1 N2 2.133(2) .
V1 N1 2.3046(19) .
V1 Cl1 2.3252(7) .
O1 C1 1.297(2) .
N1 C11 1.485(3) .
N1 C4 1.486(3) .
N1 C5 1.490(3) .
N2 C16 1.347(3) .
N2 C12 1.348(3) .
N3 C10 1.342(3) .
N3 C6 1.346(3) .
C2 C3 1.370(3) 16_645
C2 C1 1.429(3) .
C3 C2 1.370(3) 16_645
C3 C1 1.429(3) .
C3 C4 1.510(3) .
C7 C6 1.394(3) .
C7 C8 1.398(4) .
C14 C15 1.384(4) .
C14 C13 1.392(4) .
C9 C8 1.371(4) .
C9 C10 1.386(3) .
C6 C5 1.502(3) .
C12 C13 1.381(4) .
C12 C11 1.502(4) .
C15 C16 1.388(4) .
O2W O2A 0.958(13) .
O1P O1P 1.603(19) 3_765
O1P O1P 1.60(2) 2_645
