#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:06:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179093 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305582.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_4305582
loop_
_publ_author_name
'Chryssoula Drouza'
'Anastasios D. Keramidas'
_publ_section_title
;
Solid State and Aqueous Solution Characterization of Rectangular
Tetranuclear VIV/V-p-Semiquinonate/Hydroquinonate Complexes Exhibiting a
Proton Induced Electron Transfer
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7211
_journal_page_last               7224
_journal_paper_doi               10.1021/ic800569t
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C21 H36 N8 O16 V2'
_chemical_formula_weight         758.46
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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
_cell_angle_beta                 98.816(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.4212(9)
_cell_length_b                   11.0769(5)
_cell_length_c                   29.3388(10)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1596
_cell_measurement_theta_min      3.1543
_cell_volume                     6237.0(5)
_computing_cell_refinement
;
'Mon Jun 05 18:43:11 2006'
;
_computing_data_collection
;
'Mon Jun 05 18:43:11 2006'
;
_computing_data_reduction
;
'Mon Jun 05 18:43:11 2006'
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0288
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            38164
_diffrn_reflns_theta_full        31.16
_diffrn_reflns_theta_max         31.16
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.90382
_exptl_absorpt_correction_T_min  0.83188
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
'Mon Jun 05 18:43:11 2006'
;
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.14545
_exptl_crystal_size_mid          0.11353
_exptl_crystal_size_min          0.07112
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         9293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0526P)²+18.1997P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                7863
_reflns_number_total             9293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800569t-file002_2.cif
_cod_data_source_block           o
_cod_database_code               4305582
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.99996(8) 0.32186(13) 0.15752(5) 0.0173(3) Uani 1 1 d . . .
O15 O 1.24696(8) 0.26257(13) 0.13125(5) 0.0191(3) Uani 1 1 d . . .
O13 O 1.16951(8) 0.11781(13) 0.23002(5) 0.0187(3) Uani 1 1 d . . .
O14 O 1.30327(8) 0.16635(14) 0.20970(5) 0.0226(3) Uani 1 1 d . . .
O1 O 1.07738(8) 0.40600(13) 0.09672(5) 0.0206(3) Uani 1 1 d . . .
O4 O 0.95314(8) 0.29851(14) 0.06820(5) 0.0230(3) Uani 1 1 d . . .
O11 O 1.21465(8) 0.03554(13) 0.15332(5) 0.0230(3) Uani 1 1 d . . .
N11 N 1.21334(9) 0.34960(14) 0.21142(5) 0.0151(3) Uani 1 1 d . . .
O5 O 1.07423(8) 0.19284(13) 0.05652(5) 0.0208(3) Uani 1 1 d . . .
N1 N 0.99389(9) 0.09170(15) 0.11203(5) 0.0159(3) Uani 1 1 d . . .
C1 C 0.99045(10) 0.05463(17) 0.16053(6) 0.0160(3) Uani 1 1 d . . .
H1A H 1.0384 0.0479 0.1775 0.019 Uiso 1 1 calc R . .
H1B H 0.9686 -0.0262 0.1603 0.019 Uiso 1 1 calc R . .
C51 C 0.95841(10) 0.26801(17) 0.18376(6) 0.0145(3) Uani 1 1 d . . .
C61 C 0.87170(10) 0.17264(17) 0.24334(6) 0.0141(3) Uani 1 1 d . . .
C4 C 0.90650(11) 0.2155(2) 0.06131(7) 0.0213(4) Uani 1 1 d . . .
C14 C 1.26097(11) 0.37567(19) 0.13753(7) 0.0202(4) Uani 1 1 d . . .
C63 C 0.92331(10) 0.34361(17) 0.21116(6) 0.0155(3) Uani 1 1 d . . .
H63 H 0.9288 0.4285 0.2090 0.019 Uiso 1 1 calc R . .
C52 C 0.94984(10) 0.14155(17) 0.18584(6) 0.0144(3) Uani 1 1 d . . .
C53 C 0.90622(10) 0.09666(17) 0.21531(6) 0.0148(3) Uani 1 1 d . . .
H53 H 0.8994 0.0119 0.2166 0.018 Uiso 1 1 calc R . .
C12 C 1.23078(11) 0.43676(18) 0.17663(7) 0.0190(4) Uani 1 1 d . . .
H12A H 1.2650 0.4959 0.1920 0.023 Uiso 1 1 calc R . .
H12B H 1.1882 0.4815 0.1636 0.023 Uiso 1 1 calc R . .
C11 C 0.85151(10) 0.38932(17) 0.27168(6) 0.0156(3) Uani 1 1 d . . .
H11A H 0.8874 0.4071 0.2987 0.019 Uiso 1 1 calc R . .
H11B H 0.8417 0.4653 0.2542 0.019 Uiso 1 1 calc R . .
C62 C 0.88091(10) 0.29867(17) 0.24136(6) 0.0138(3) Uani 1 1 d . . .
O7 O 1.09387(9) 0.02059(15) 0.02212(6) 0.0279(4) Uani 1 1 d . . .
O6 O 0.84882(9) 0.22967(16) 0.03758(6) 0.0284(3) Uani 1 1 d . . .
O17 O 1.29393(11) 0.43536(16) 0.11298(6) 0.0349(4) Uani 1 1 d . . .
O16 O 1.38906(9) 0.27113(19) 0.25080(6) 0.0348(4) Uani 1 1 d . . .
C13 C 1.27131(11) 0.33821(19) 0.25004(7) 0.0196(4) Uani 1 1 d . . .
H13A H 1.2536 0.3063 0.2776 0.024 Uiso 1 1 calc R . .
H13B H 1.2922 0.4186 0.2579 0.024 Uiso 1 1 calc R . .
C5 C 1.07184(11) 0.07631(19) 0.05306(7) 0.0194(4) Uani 1 1 d . . .
C3 C 1.04210(11) 0.01100(18) 0.09146(7) 0.0191(4) Uani 1 1 d . . .
H3A H 1.0167 -0.0622 0.0788 0.023 Uiso 1 1 calc R . .
H3B H 1.0806 -0.0146 0.1156 0.023 Uiso 1 1 calc R . .
C2 C 0.92417(11) 0.09416(19) 0.08349(7) 0.0186(4) Uani 1 1 d . . .
H2A H 0.8887 0.0733 0.1031 0.022 Uiso 1 1 calc R . .
H2B H 0.9223 0.0320 0.0591 0.022 Uiso 1 1 calc R . .
C15 C 1.32632(12) 0.2532(2) 0.23648(8) 0.0246(4) Uani 1 1 d . . .
N51 N 0.84393(12) 0.80796(18) 0.03768(7) 0.0285(4) Uani 1 1 d . . .
N52 N 0.83206(13) 0.6503(2) -0.01453(8) 0.0343(5) Uani 1 1 d . . .
C101 C 0.81987(13) 0.6989(2) 0.02512(8) 0.0256(4) Uani 1 1 d . . .
N53 N 0.78385(12) 0.63559(19) 0.05230(7) 0.0273(4) Uani 1 1 d . . .
N56 N 0.39902(12) 0.1174(2) 0.14073(8) 0.0382(5) Uani 1 1 d . . .
H56A H 0.3696 0.1278 0.1604 0.046 Uiso 1 1 calc R . .
H56B H 0.3846 0.0850 0.1135 0.046 Uiso 1 1 calc R . .
C102 C 0.46525(14) 0.1505(2) 0.15204(9) 0.0334(5) Uani 1 1 d . . .
N54 N 0.48504(13) 0.1981(3) 0.19248(9) 0.0543(8) Uani 1 1 d . . .
H54A H 0.5286 0.2208 0.2006 0.065 Uiso 1 1 calc R . .
H54B H 0.4548 0.2075 0.2117 0.065 Uiso 1 1 calc R . .
O2W O 0.23711(10) 0.57933(16) 0.99855(7) 0.0293(4) Uani 1 1 d . . .
O90 O 0.65537(11) 0.2028(2) 0.15155(7) 0.0429(5) Uani 1 1 d . . .
N55 N 0.51008(14) 0.1360(3) 0.12303(10) 0.0460(6) Uani 1 1 d . . .
H55A H 0.5537 0.1586 0.1310 0.055 Uiso 1 1 calc R . .
H55B H 0.4964 0.1038 0.0957 0.055 Uiso 1 1 calc R . .
C90 C 0.68560(15) 0.2347(2) 0.12022(9) 0.0333(5) Uani 1 1 d . . .
C92 C 0.76221(15) 0.2579(3) 0.12747(10) 0.0394(6) Uani 1 1 d . . .
H92A H 0.7814 0.2437 0.1599 0.059 Uiso 1 1 calc R . .
H92B H 0.7709 0.3418 0.1194 0.059 Uiso 1 1 calc R . .
H92C H 0.7846 0.2035 0.1079 0.059 Uiso 1 1 calc R . .
C91 C 0.64662(19) 0.2517(4) 0.07264(11) 0.0552(9) Uani 1 1 d . . .
H91A H 0.5972 0.2339 0.0725 0.083 Uiso 1 1 calc R . .
H91B H 0.6654 0.1970 0.0513 0.083 Uiso 1 1 calc R . .
H91C H 0.6518 0.3354 0.0629 0.083 Uiso 1 1 calc R . .
O1W O 0.9529(2) 0.5269(3) 0.03726(14) 0.1038(14) Uani 1 1 d . . .
H1WA H 0.9819 0.4605 0.0279 0.125 Uiso 1 1 calc R . .
H1WB H 0.9556 0.5961 0.0163 0.125 Uiso 1 1 calc R . .
H2 H 0.8276(16) 0.847(3) 0.0590(11) 0.032(8) Uiso 1 1 d . . .
H1 H 0.8617(15) 0.851(3) 0.0189(10) 0.023(7) Uiso 1 1 d . . .
H3 H 0.7683(17) 0.671(3) 0.0743(11) 0.036(8) Uiso 1 1 d . . .
H4 H 0.7678(16) 0.564(3) 0.0418(10) 0.031(8) Uiso 1 1 d . . .
H2WB H 0.271(2) 0.610(3) 1.0113(13) 0.047(10) Uiso 1 1 d . . .
H21 H 0.8156(18) 0.578(3) -0.0216(11) 0.043(9) Uiso 1 1 d . . .
H22 H 0.8555(18) 0.684(3) -0.0284(12) 0.037(9) Uiso 1 1 d . . .
H2WA H 0.210(2) 0.633(3) 0.9820(13) 0.048(10) Uiso 1 1 d . . .
V11 V 1.201058(17) 0.16445(3) 0.175707(11) 0.01445(8) Uani 1 1 d . . .
V1 V 1.045534(17) 0.27953(3) 0.109988(11) 0.01504(8) Uani 1 1 d . . .
O2 O 1.11915(8) 0.20991(13) 0.14781(5) 0.0184(3) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C51 O3 V1 137.03(12) . . ?
C14 O15 V11 122.56(12) . . ?
C61 O13 V11 132.31(12) 2_755 . ?
C15 O14 V11 121.35(14) . . ?
C4 O4 V1 124.00(14) . . ?
C13 N11 C12 110.92(16) . . ?
C13 N11 C11 110.77(14) . 2_755 ?
C12 N11 C11 109.33(15) . 2_755 ?
C13 N11 V11 106.68(12) . . ?
C12 N11 V11 106.63(11) . . ?
C11 N11 V11 112.42(11) 2_755 . ?
C5 O5 V1 122.10(12) . . ?
C2 N1 C3 111.11(15) . . ?
C2 N1 C1 111.97(15) . . ?
C3 N1 C1 110.13(15) . . ?
C2 N1 V1 109.33(12) . . ?
C3 N1 V1 103.14(11) . . ?
C1 N1 V1 110.82(11) . . ?
N1 C1 C52 113.35(16) . . ?
O3 C51 C63 116.82(16) . . ?
O3 C51 C52 123.53(17) . . ?
C63 C51 C52 119.64(16) . . ?
O13 C61 C62 124.15(16) 2_755 . ?
O13 C61 C53 116.48(16) 2_755 . ?
C62 C61 C53 119.36(16) . . ?
O6 C4 O4 123.7(2) . . ?
O6 C4 C2 118.89(19) . . ?
O4 C4 C2 117.45(19) . . ?
O17 C14 O15 123.87(19) . . ?
O17 C14 C12 119.86(19) . . ?
O15 C14 C12 116.20(17) . . ?
C62 C63 C51 122.47(17) . . ?
C53 C52 C51 117.92(17) . . ?
C53 C52 C1 119.41(16) . . ?
C51 C52 C1 122.47(16) . . ?
C52 C53 C61 122.42(17) . . ?
N11 C12 C14 112.60(16) . . ?
N11 C11 C62 114.52(15) 2_755 . ?
C63 C62 C61 118.17(16) . . ?
C63 C62 C11 116.83(16) . . ?
C61 C62 C11 124.90(16) . . ?
N11 C13 C15 109.65(16) . . ?
O7 C5 O5 123.12(18) . . ?
O7 C5 C3 121.48(19) . . ?
O5 C5 C3 115.35(16) . . ?
N1 C3 C5 110.34(16) . . ?
N1 C2 C4 112.88(16) . . ?
O16 C15 O14 124.1(2) . . ?
O16 C15 C13 120.3(2) . . ?
O14 C15 C13 115.60(19) . . ?
N51 C101 N52 120.4(2) . . ?
N51 C101 N53 120.4(2) . . ?
N52 C101 N53 119.1(2) . . ?
N54 C102 N55 120.4(3) . . ?
N54 C102 N56 118.6(2) . . ?
N55 C102 N56 121.0(3) . . ?
O90 C90 C92 121.9(3) . . ?
O90 C90 C91 120.6(3) . . ?
C92 C90 C91 117.5(2) . . ?
O11 V11 O2 105.03(8) . . ?
O11 V11 O13 101.43(7) . . ?
O2 V11 O13 94.90(7) . . ?
O11 V11 O15 95.64(7) . . ?
O2 V11 O15 90.14(7) . . ?
O13 V11 O15 160.25(6) . . ?
O11 V11 O14 90.00(8) . . ?
O2 V11 O14 162.67(7) . . ?
O13 V11 O14 90.42(7) . . ?
O15 V11 O14 79.65(6) . . ?
O11 V11 N11 164.79(7) . . ?
O2 V11 N11 88.82(6) . . ?
O13 V11 N11 83.27(6) . . ?
O15 V11 N11 77.74(6) . . ?
O14 V11 N11 75.41(6) . . ?
O1 V1 O3 102.23(7) . . ?
O1 V1 O2 102.72(7) . . ?
O3 V1 O2 94.01(7) . . ?
O1 V1 O5 93.72(7) . . ?
O3 V1 O5 162.55(6) . . ?
O2 V1 O5 89.28(7) . . ?
O1 V1 O4 95.79(7) . . ?
O3 V1 O4 86.97(7) . . ?
O2 V1 O4 160.79(7) . . ?
O5 V1 O4 84.39(7) . . ?
O1 V1 N1 167.59(7) . . ?
O3 V1 N1 87.01(6) . . ?
O2 V1 N1 84.65(6) . . ?
O5 V1 N1 76.22(6) . . ?
O4 V1 N1 76.23(6) . . ?
V11 O2 V1 166.09(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 C51 1.338(2) . ?
O3 V1 1.8235(14) . ?
O15 C14 1.289(2) . ?
O15 V11 2.0089(14) . ?
O13 C61 1.346(2) 2_755 ?
O13 V11 1.8659(13) . ?
O14 C15 1.279(3) . ?
O14 V11 2.0805(16) . ?
O1 V1 1.6033(15) . ?
O4 C4 1.285(3) . ?
O4 V1 2.0231(16) . ?
O11 V11 1.6100(15) . ?
N11 C13 1.475(3) . ?
N11 C12 1.482(2) . ?
N11 C11 1.489(2) 2_755 ?
N11 V11 2.2981(16) . ?
O5 C5 1.295(2) . ?
O5 V1 1.9898(14) . ?
N1 C2 1.479(3) . ?
N1 C3 1.487(2) . ?
N1 C1 1.492(2) . ?
N1 V1 2.3144(17) . ?
C1 C52 1.510(3) . ?
C51 C63 1.407(3) . ?
C51 C52 1.413(3) . ?
C61 O13 1.346(2) 2_755 ?
C61 C62 1.410(3) . ?
C61 C53 1.415(2) . ?
C4 O6 1.235(3) . ?
C4 C2 1.510(3) . ?
C14 O17 1.228(2) . ?
C14 C12 1.524(3) . ?
C63 C62 1.391(2) . ?
C52 C53 1.392(2) . ?
C11 N11 1.489(2) 2_755 ?
C11 C62 1.510(2) . ?
O7 C5 1.227(2) . ?
O16 C15 1.242(3) . ?
C13 C15 1.522(3) . ?
C5 C3 1.525(3) . ?
N51 C101 1.327(3) . ?
N52 C101 1.335(3) . ?
C101 N53 1.337(3) . ?
N56 C102 1.330(4) . ?
C102 N54 1.301(4) . ?
C102 N55 1.317(3) . ?
O90 C90 1.217(3) . ?
C90 C92 1.493(4) . ?
C90 C91 1.494(4) . ?
V11 O2 1.7481(15) . ?
V1 O2 1.8400(15) . ?
