#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:06:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179093 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305581.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_4305581
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            'C18 H44 N8 O21 V2'
_chemical_formula_weight         810.49
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.586(12)
_cell_angle_beta                 111.185(16)
_cell_angle_gamma                109.918(14)
_cell_formula_units_Z            2
_cell_length_a                   10.5707(18)
_cell_length_b                   13.5589(18)
_cell_length_c                   13.801(2)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0966
_cell_measurement_theta_min      3.0285
_cell_volume                     1694.7(5)
_computing_cell_refinement
;
'Mon Jun 05 18:31:17 2006'
;
_computing_data_collection
;
'Mon Jun 05 18:31:17 2006'
;
_computing_data_reduction
;
'Mon Jun 05 18:31:17 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 0.869
_diffrn_measured_fraction_theta_max 0.869
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24636
_diffrn_reflns_theta_full        31.39
_diffrn_reflns_theta_max         31.39
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.646
_exptl_absorpt_correction_T_max  0.93739
_exptl_absorpt_correction_T_min  0.90327
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
'Mon Jun 05 18:31:17 2006'
;
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.09470
_exptl_crystal_size_mid          0.07330
_exptl_crystal_size_min          0.04610
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0076(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         9729
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          3.687
_refine_ls_shift/su_mean         0.024
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0714P)²+3.9250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1786
_refine_ls_wR_factor_ref         0.1899
_reflns_number_gt                6022
_reflns_number_total             9729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800569t-file002_1.cif
_cod_data_source_block           v4biq
_cod_database_code               4305581
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
V1 V 0.30031(7) 0.57758(5) 0.70041(5) 0.02217(17) Uani 1 1 d . . .
V11 V 0.19985(7) 0.80066(5) 0.92692(5) 0.02178(17) Uani 1 1 d . . .
O17 O 0.5210(3) 1.0597(2) 1.1613(2) 0.0298(7) Uani 1 1 d . . .
O14 O 0.0316(3) 0.8030(2) 0.9610(2) 0.0281(6) Uani 1 1 d . . .
O7 O -0.0100(3) 0.3417(2) 0.4381(2) 0.0302(6) Uani 1 1 d . . .
O4 O 0.4684(3) 0.5444(2) 0.6959(2) 0.0292(6) Uani 1 1 d . . .
O13 O 0.1157(3) 0.6441(2) 0.8906(2) 0.0241(6) Uani 1 1 d . . .
O16 O -0.0747(3) 0.8039(3) 1.0731(3) 0.0386(8) Uani 1 1 d . . .
O5 O 0.1725(3) 0.4913(2) 0.5474(2) 0.0253(6) Uani 1 1 d . . .
O11 O 0.1360(3) 0.8278(2) 0.8116(2) 0.0304(6) Uani 1 1 d . . .
O15 O 0.3287(3) 0.9534(2) 1.0143(2) 0.0248(6) Uani 1 1 d . . .
O1 O 0.3600(3) 0.6946(2) 0.6755(2) 0.0296(6) Uani 1 1 d . . .
N55 N 0.3047(4) 0.2105(3) 0.1396(3) 0.0337(8) Uani 1 1 d . . .
H55A H 0.3956 0.2538 0.1628 0.040 Uiso 1 1 calc R . .
H55B H 0.2408 0.2153 0.0820 0.040 Uiso 1 1 calc R . .
O3 O 0.3876(3) 0.6120(2) 0.8556(2) 0.0243(6) Uani 1 1 d . . .
N54 N 0.3590(4) 0.1275(3) 0.2808(3) 0.0376(9) Uani 1 1 d . . .
H54A H 0.4503 0.1701 0.3052 0.045 Uiso 1 1 calc R . .
H54B H 0.3301 0.0789 0.3141 0.045 Uiso 1 1 calc R . .
N53 N 0.1939(4) 0.3544(3) 0.2861(3) 0.0360(9) Uani 1 1 d . . .
H53A H 0.1035 0.3303 0.2410 0.043 Uiso 1 1 calc R . .
H53B H 0.2571 0.4122 0.2820 0.043 Uiso 1 1 calc R . .
C63 C 0.0735(4) 0.5153(3) 1.1096(3) 0.0223(8) Uani 1 1 d . . .
H63 H 0.1225 0.5256 1.1829 0.027 Uiso 1 1 calc R . .
N51 N 0.1395(4) 0.2137(3) 0.3688(3) 0.0371(9) Uani 1 1 d . . .
H51A H 0.0489 0.1892 0.3239 0.045 Uiso 1 1 calc R . .
H51B H 0.1673 0.1803 0.4182 0.045 Uiso 1 1 calc R . .
N56 N 0.1229(4) 0.0685(3) 0.1543(3) 0.0354(9) Uani 1 1 d . . .
H56A H 0.0954 0.0193 0.1873 0.042 Uiso 1 1 calc R . .
H56B H 0.0597 0.0739 0.0967 0.042 Uiso 1 1 calc R . .
N11 N 0.2712(3) 0.7863(2) 1.1035(3) 0.0235(7) Uani 1 1 d . . .
O6 O 0.5790(3) 0.4335(3) 0.6929(3) 0.0400(8) Uani 1 1 d . . .
N52 N 0.3749(4) 0.3419(3) 0.4330(3) 0.0363(9) Uani 1 1 d . . .
H52A H 0.4023 0.3096 0.4834 0.044 Uiso 1 1 calc R . .
H52B H 0.4376 0.3997 0.4285 0.044 Uiso 1 1 calc R . .
N1 N 0.2333(3) 0.3992(3) 0.7127(2) 0.0224(7) Uani 1 1 d . . .
C1 C 0.2230(4) 0.3850(3) 0.8164(3) 0.0229(8) Uani 1 1 d . . .
H1A H 0.1902 0.3092 0.8178 0.027 Uiso 1 1 calc R . .
H1B H 0.1499 0.4100 0.8225 0.027 Uiso 1 1 calc R . .
C53 C 0.4275(4) 0.3904(3) 0.9844(3) 0.0207(7) Uani 1 1 d . . .
H53 H 0.3793 0.3164 0.9733 0.025 Uiso 1 1 calc R . .
C3 C 0.0872(4) 0.3441(3) 0.6238(3) 0.0266(8) Uani 1 1 d . . .
H3A H 0.0117 0.3494 0.6455 0.032 Uiso 1 1 calc R . .
H3B H 0.0679 0.2687 0.6051 0.032 Uiso 1 1 calc R . .
C11 C 0.2799(4) 0.6809(3) 1.1162(3) 0.0226(8) Uani 1 1 d . . .
H11A H 0.3146 0.6786 1.1911 0.027 Uiso 1 1 calc R . .
H11B H 0.3508 0.6724 1.0907 0.027 Uiso 1 1 calc R . .
C52 C 0.3685(4) 0.4454(3) 0.9102(3) 0.0209(7) Uani 1 1 d . . .
C62 C 0.1323(4) 0.5889(3) 1.0559(3) 0.0205(7) Uani 1 1 d . . .
C61 C 0.0591(4) 0.5744(3) 0.9456(3) 0.0217(8) Uani 1 1 d . . .
C102 C 0.2633(5) 0.1365(3) 0.1924(4) 0.0309(9) Uani 1 1 d . . .
C51 C 0.4426(4) 0.5559(3) 0.9252(3) 0.0202(7) Uani 1 1 d . . .
C5 C 0.0817(4) 0.3945(3) 0.5282(3) 0.0254(8) Uiso 1 1 d . . .
C2 C 0.3405(5) 0.3611(3) 0.6969(3) 0.0294(9) Uani 1 1 d . . .
H2A H 0.2921 0.3093 0.6299 0.035 Uiso 1 1 calc R . .
H2B H 0.3740 0.3249 0.7533 0.035 Uiso 1 1 calc R . .
C4 C 0.4752(5) 0.4528(4) 0.6959(3) 0.0300(9) Uani 1 1 d . . .
C15 C 0.4244(4) 0.9707(3) 1.1091(3) 0.0241(8) Uani 1 1 d . . .
C12 C 0.1652(5) 0.8035(3) 1.1430(3) 0.0288(9) Uani 1 1 d . . .
H12A H 0.2133 0.8719 1.1930 0.035 Uiso 1 1 calc R . .
H12B H 0.1361 0.7476 1.1805 0.035 Uiso 1 1 calc R . .
C14 C 0.0298(5) 0.8022(3) 1.0539(4) 0.0302(9) Uani 1 1 d . . .
C101 C 0.2359(5) 0.3025(4) 0.3619(4) 0.0321(9) Uani 1 1 d . . .
C13 C 0.4193(4) 0.8738(3) 1.1584(3) 0.0259(8) Uani 1 1 d . . .
H13A H 0.4931 0.8495 1.1527 0.031 Uiso 1 1 calc R . .
H13B H 0.4410 0.8930 1.2332 0.031 Uiso 1 1 calc R . .
O12 O 0.3891(3) 0.7915(2) 0.9369(2) 0.0236(6) Uani 1 1 d D . .
O2 O 0.1107(3) 0.5640(2) 0.7111(2) 0.0234(6) Uani 1 1 d D . .
O3W O 0.7563(4) 0.9049(3) 0.1220(3) 0.0409(8) Uani 1 1 d D . .
O4W O 0.7404(4) 0.3744(3) 0.5922(3) 0.0449(9) Uani 1 1 d . . .
O6W O 0.7647(6) 0.1307(3) 0.3691(3) 0.0564(11) Uani 1 1 d D . .
O5W O 0.7075(8) 0.1660(4) 0.5412(4) 0.0883(18) Uani 1 1 d . . .
O7W O 0.1448(10) 0.9588(4) 0.3426(5) 0.110(2) Uani 1 1 d D . .
O2W O 0.8496(8) 0.9618(5) 0.3332(4) 0.099(2) Uani 1 1 d D . .
O1W O 0.6829(8) 0.8541(5) 0.4547(5) 0.100(2) Uani 1 1 d D . .
O1P O 0.425(2) 0.0367(14) 0.4568(14) 0.088(8) Uiso 0.316(17) 1 d PU . .
O2P O 0.505(3) 0.0345(19) 0.5771(19) 0.048(9) Uiso 0.157(13) 1 d PU . .
O3P O 0.091(3) 0.056(2) 0.475(2) 0.079(11) Uiso 0.197(16) 1 d P . .
H4WB H 0.692(7) 0.399(5) 0.620(5) 0.054(17) Uiso 1 1 d . . .
H4WA H 0.745(10) 0.404(7) 0.529(8) 0.12(3) Uiso 1 1 d . . .
H12D H 0.398(4) 0.738(2) 0.909(3) 0.016(10) Uiso 1 1 d D . .
H12C H 0.440(7) 0.848(2) 0.923(6) 0.10(3) Uiso 1 1 d D . .
H2C H 0.064(5) 0.584(4) 0.659(2) 0.035(14) Uiso 1 1 d D . .
H2D H 0.112(6) 0.588(4) 0.768(2) 0.048(16) Uiso 1 1 d D . .
H3BW H 0.799(6) 0.869(4) 0.100(4) 0.07(2) Uiso 1 1 d D . .
H3AW H 0.740(6) 0.944(4) 0.076(4) 0.054(18) Uiso 1 1 d D . .
H1AW H 0.594(2) 0.810(3) 0.448(3) 0.000(9) Uiso 1 1 d D . .
H2BW H 0.766(3) 0.954(3) 0.340(3) 0.000(9) Uiso 1 1 d D . .
H6BW H 0.692(5) 0.120(5) 0.309(3) 0.09(3) Uiso 1 1 d D . .
H1BW H 0.667(7) 0.904(13) 0.42(2) 0.50(19) Uiso 1 1 d D . .
H6AW H 0.819(6) 0.198(2) 0.386(5) 0.09(3) Uiso 1 1 d D . .
H5WB H 0.735(8) 0.176(6) 0.467(6) 0.09(2) Uiso 1 1 d . . .
H7BW H 0.09(3) 0.95(2) 0.38(2) 1.5(9) Uiso 1 1 d D . .
H7AW H 0.197(7) 0.921(5) 0.363(6) 0.08(2) Uiso 1 1 d D . .
H2AW H 0.819(6) 0.952(7) 0.2633(18) 0.12(3) Uiso 1 1 d D . .
H5WA H 0.612(4) 0.171(3) 0.527(3) 0.000(8) 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
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'
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
O1 V1 O3 100.85(13) . . ?
O1 V1 O4 93.65(14) . . ?
O3 V1 O4 92.00(12) . . ?
O1 V1 O2 104.09(14) . . ?
O3 V1 O2 85.92(12) . . ?
O4 V1 O2 162.22(12) . . ?
O1 V1 O5 98.78(13) . . ?
O3 V1 O5 160.14(12) . . ?
O4 V1 O5 89.72(11) . . ?
O2 V1 O5 86.42(11) . . ?
O1 V1 N1 168.24(14) . . ?
O3 V1 N1 86.64(11) . . ?
O4 V1 N1 76.91(12) . . ?
O2 V1 N1 85.34(12) . . ?
O5 V1 N1 74.49(11) . . ?
O11 V11 O13 100.88(14) . . ?
O11 V11 O12 103.03(14) . . ?
O13 V11 O12 86.38(11) . . ?
O11 V11 O14 93.95(14) . . ?
O13 V11 O14 91.53(12) . . ?
O12 V11 O14 162.98(12) . . ?
O11 V11 O15 98.99(14) . . ?
O13 V11 O15 159.74(12) . . ?
O12 V11 O15 85.36(11) . . ?
O14 V11 O15 90.97(11) . . ?
O11 V11 N11 167.68(14) . . ?
O13 V11 N11 86.90(11) . . ?
O12 V11 N11 86.85(12) . . ?
O14 V11 N11 76.16(12) . . ?
O15 V11 N11 74.20(11) . . ?
C14 O14 V11 124.2(3) . . ?
C4 O4 V1 124.8(3) . . ?
C61 O13 V11 128.2(2) . . ?
C5 O5 V1 121.1(3) . . ?
C15 O15 V11 121.0(2) . . ?
C51 O3 V1 129.8(2) . . ?
C62 C63 C61 120.7(3) . 2_567 ?
C11 N11 C13 110.3(3) . . ?
C11 N11 C12 111.1(3) . . ?
C13 N11 C12 111.0(3) . . ?
C11 N11 V11 111.2(2) . . ?
C13 N11 V11 104.1(2) . . ?
C12 N11 V11 108.9(3) . . ?
C2 N1 C3 110.2(3) . . ?
C2 N1 C1 112.3(3) . . ?
C3 N1 C1 110.4(3) . . ?
C2 N1 V1 108.3(2) . . ?
C3 N1 V1 104.3(2) . . ?
C1 N1 V1 111.1(2) . . ?
N1 C1 C52 112.3(3) . . ?
C51 C53 C52 121.2(3) 2_667 . ?
N1 C3 C5 110.2(3) . . ?
N11 C11 C62 112.0(3) . . ?
C53 C52 C51 119.6(3) . . ?
C53 C52 C1 119.5(3) . . ?
C51 C52 C1 120.9(3) . . ?
C63 C62 C61 120.1(3) . . ?
C63 C62 C11 119.6(3) . . ?
C61 C62 C11 120.2(3) . . ?
O13 C61 C62 121.3(3) . . ?
O13 C61 C63 119.4(3) . 2_567 ?
C62 C61 C63 119.2(3) . 2_567 ?
N54 C102 N55 121.3(4) . . ?
N54 C102 N56 119.4(4) . . ?
N55 C102 N56 119.3(4) . . ?
O3 C51 C53 119.6(3) . 2_667 ?
O3 C51 C52 121.1(3) . . ?
C53 C51 C52 119.2(3) 2_667 . ?
O7 C5 O5 124.3(4) . . ?
O7 C5 C3 119.5(4) . . ?
O5 C5 C3 116.2(3) . . ?
N1 C2 C4 112.8(3) . . ?
O6 C4 O4 124.1(4) . . ?
O6 C4 C2 119.4(4) . . ?
O4 C4 C2 116.4(4) . . ?
O17 C15 O15 124.8(4) . . ?
O17 C15 C13 118.8(4) . . ?
O15 C15 C13 116.5(3) . . ?
N11 C12 C14 111.9(3) . . ?
O16 C14 O14 123.1(4) . . ?
O16 C14 C12 119.2(4) . . ?
O14 C14 C12 117.6(4) . . ?
N51 C101 N53 120.4(4) . . ?
N51 C101 N52 120.1(4) . . ?
N53 C101 N52 119.5(4) . . ?
N11 C13 C15 109.9(3) . . ?
O2P O1P O2P 90.8(16) 2_656 . ?
O1P O2P O1P 89.2(16) 2_656 . ?
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
V1 O1 1.605(3) . ?
V1 O3 1.952(3) . ?
V1 O4 1.997(3) . ?
V1 O2 2.009(3) . ?
V1 O5 2.051(3) . ?
V1 N1 2.313(3) . ?
V11 O11 1.609(3) . ?
V11 O13 1.951(3) . ?
V11 O12 2.002(3) . ?
V11 O14 2.007(3) . ?
V11 O15 2.044(3) . ?
V11 N11 2.319(3) . ?
O17 C15 1.241(4) . ?
O14 C14 1.289(5) . ?
O7 C5 1.242(5) . ?
O4 C4 1.268(5) . ?
O13 C61 1.365(4) . ?
O16 C14 1.232(5) . ?
O5 C5 1.276(5) . ?
O15 C15 1.279(5) . ?
N55 C102 1.324(6) . ?
O3 C51 1.351(4) . ?
N54 C102 1.319(6) . ?
N53 C101 1.325(6) . ?
C63 C62 1.391(5) . ?
C63 C61 1.406(5) 2_567 ?
N51 C101 1.321(6) . ?
N56 C102 1.331(5) . ?
N11 C11 1.481(5) . ?
N11 C13 1.482(5) . ?
N11 C12 1.487(5) . ?
O6 C4 1.226(5) . ?
N52 C101 1.329(6) . ?
N1 C2 1.470(5) . ?
N1 C3 1.476(5) . ?
N1 C1 1.494(5) . ?
C1 C52 1.511(5) . ?
C53 C51 1.393(5) 2_667 ?
C53 C52 1.395(5) . ?
C3 C5 1.516(6) . ?
C11 C62 1.512(5) . ?
C52 C51 1.395(5) . ?
C62 C61 1.401(5) . ?
C61 C63 1.406(5) 2_567 ?
C51 C53 1.393(5) 2_667 ?
C2 C4 1.543(6) . ?
C15 C13 1.511(6) . ?
C12 C14 1.507(6) . ?
O1P O2P 1.54(3) 2_656 ?
O1P O2P 1.58(3) . ?
O2P O1P 1.54(3) 2_656 ?
