#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305584.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_4305584
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            'C41 H95 N19 O40.5 V4'
_chemical_formula_weight         1706.12
_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                94.517(3)
_cell_angle_beta                 101.466(3)
_cell_angle_gamma                107.133(3)
_cell_formula_units_Z            2
_cell_length_a                   14.0245(4)
_cell_length_b                   15.1826(5)
_cell_length_c                   19.6243(7)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0898
_cell_measurement_theta_min      2.9278
_cell_volume                     3871.2(2)
_computing_cell_refinement
;
'Mon Jun 05 19:37:04 2006'
;
_computing_data_collection
;
'Mon Jun 05 19:37:04 2006'
;
_computing_data_reduction
;
'Mon Jun 05 19:37:04 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 0.902
_diffrn_measured_fraction_theta_max 0.902
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            85717
_diffrn_reflns_theta_full        31.19
_diffrn_reflns_theta_max         31.19
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  0.94042
_exptl_absorpt_correction_T_min  0.86542
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
'Mon Jun 05 19:37:04 2006'
;
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.17313
_exptl_crystal_size_mid          0.10319
_exptl_crystal_size_min          0.05769
_refine_diff_density_max         1.517
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     996
_refine_ls_number_reflns         22650
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1118P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1895
_reflns_number_gt                14841
_reflns_number_total             22650
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800569t-file002_4.cif
_cod_data_source_block           vbiqg50
_cod_original_formula_sum        'C41 H95 N19 O40.50 V4'
_cod_database_code               4305584
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
C11 C 0.5012(2) 0.65624(18) 0.41052(13) 0.0162(5) Uani 1 1 d . . .
H11A H 0.4890 0.5948 0.4245 0.019 Uiso 1 1 calc R . .
H11B H 0.5682 0.6951 0.4378 0.019 Uiso 1 1 calc R . .
O37 O 0.99058(16) 0.42859(16) 0.16661(10) 0.0279(5) Uani 1 1 d . . .
C1 C 0.5233(2) 0.58848(19) 0.11805(13) 0.0172(5) Uani 1 1 d . . .
H1A H 0.5229 0.5243 0.1124 0.021 Uiso 1 1 calc R . .
H1B H 0.4615 0.5914 0.0870 0.021 Uiso 1 1 calc R . .
C31 C 0.7189(2) 0.43949(19) 0.27749(13) 0.0175(5) Uani 1 1 d . . .
H31A H 0.7447 0.5053 0.2742 0.021 Uiso 1 1 calc R . .
H31B H 0.7482 0.4309 0.3246 0.021 Uiso 1 1 calc R . .
C13 C 0.4201(2) 0.6890(2) 0.50248(14) 0.0210(6) Uani 1 1 d . . .
H13A H 0.4635 0.7474 0.5312 0.025 Uiso 1 1 calc R . .
H13B H 0.4476 0.6403 0.5174 0.025 Uiso 1 1 calc R . .
C21 C 0.2811(2) 0.38420(19) 0.24428(14) 0.0177(5) Uani 1 1 d . . .
H21A H 0.2792 0.4476 0.2504 0.021 Uiso 1 1 calc R . .
H21B H 0.2450 0.3562 0.1964 0.021 Uiso 1 1 calc R . .
C35 C 0.9006(2) 0.4214(2) 0.16516(14) 0.0206(5) Uani 1 1 d . . .
C25 C 0.0873(2) 0.33615(19) 0.35217(15) 0.0211(5) Uani 1 1 d . . .
C12 C 0.4426(2) 0.79231(18) 0.41412(15) 0.0197(5) Uani 1 1 d . . .
H12A H 0.4824 0.8018 0.3786 0.024 Uiso 1 1 calc R . .
H12B H 0.4832 0.8344 0.4566 0.024 Uiso 1 1 calc R . .
C2 C 0.6153(2) 0.74562(19) 0.09878(14) 0.0204(5) Uani 1 1 d . A .
H2A H 0.5578 0.7522 0.1169 0.024 Uiso 1 1 calc R . .
H2B H 0.6068 0.7614 0.0515 0.024 Uiso 1 1 calc R . .
C3 C 0.6170(2) 0.6091(2) 0.02517(13) 0.0197(5) Uani 1 1 d . . .
H3A H 0.5732 0.6303 -0.0100 0.024 Uiso 1 1 calc R . .
H3B H 0.5910 0.5416 0.0191 0.024 Uiso 1 1 calc R . .
O16 O 0.35028(16) 0.89839(14) 0.38735(11) 0.0266(5) Uani 1 1 d . . .
O7 O 0.74297(16) 0.64157(17) -0.04435(11) 0.0302(5) Uani 1 1 d . . .
C23 C 0.1238(2) 0.3417(2) 0.28436(14) 0.0232(6) Uani 1 1 d . . .
H23A H 0.0757 0.2929 0.2481 0.028 Uiso 1 1 calc R . .
H23B H 0.1256 0.4012 0.2690 0.028 Uiso 1 1 calc R . .
C22 C 0.2225(2) 0.23343(19) 0.28447(15) 0.0231(6) Uani 1 1 d . . .
H22A H 0.2699 0.2262 0.2562 0.028 Uiso 1 1 calc R . .
H22B H 0.1540 0.1955 0.2592 0.028 Uiso 1 1 calc R . .
C14 C 0.3448(2) 0.81568(19) 0.38899(14) 0.0195(5) Uani 1 1 d . . .
C5 C 0.7256(2) 0.6399(2) 0.01475(14) 0.0205(5) Uani 1 1 d . . .
C33 C 0.8676(2) 0.4333(2) 0.23411(14) 0.0216(6) Uani 1 1 d . . .
H33A H 0.9058 0.4073 0.2693 0.026 Uiso 1 1 calc R . .
H33B H 0.8844 0.4992 0.2505 0.026 Uiso 1 1 calc R . .
O17 O 0.29931(16) 0.68628(15) 0.57359(10) 0.0259(4) Uani 1 1 d . . .
O1W O 0.15897(18) 0.5852(2) 0.16746(12) 0.0371(6) Uani 1 1 d D . .
C15 C 0.3124(2) 0.66806(19) 0.51411(14) 0.0199(5) Uani 1 1 d . . .
O91 O 0.43178(17) 0.83486(15) 0.66153(12) 0.0312(5) Uani 1 1 d . . .
H91 H 0.4429 0.8760 0.6368 0.047 Uiso 1 1 calc R . .
O2W O 0.4030(2) 0.19133(16) 0.06647(13) 0.0358(5) Uani 1 1 d D . .
O26 O 0.2342(2) 0.11430(15) 0.35395(13) 0.0399(6) Uani 1 1 d . . .
C32 C 0.7344(2) 0.2892(2) 0.23769(15) 0.0233(6) Uani 1 1 d . . .
H32A H 0.6796 0.2733 0.2625 0.028 Uiso 1 1 calc R . .
H32B H 0.7950 0.2818 0.2672 0.028 Uiso 1 1 calc R . .
C34 C 0.7035(3) 0.2225(2) 0.16994(16) 0.0282(6) Uani 1 1 d . . .
O3W O 0.4503(2) 0.9669(2) 0.56991(15) 0.0438(7) Uani 1 1 d . . .
N53 N 0.0826(2) 0.76891(18) 0.27746(16) 0.0364(7) Uani 1 1 d . . .
H53A H 0.1355 0.7572 0.3002 0.044 Uiso 1 1 calc R . .
H53B H 0.0269 0.7241 0.2591 0.044 Uiso 1 1 calc R . .
O36 O 0.7045(3) 0.14226(18) 0.17174(14) 0.0580(9) Uani 1 1 d . . .
C24 C 0.2493(2) 0.1987(2) 0.35381(16) 0.0253(6) Uani 1 1 d . . .
N51 N 0.0054(2) 0.8738(2) 0.23468(16) 0.0386(7) Uani 1 1 d . . .
H51A H -0.0502 0.8292 0.2157 0.046 Uiso 1 1 calc R . .
H51B H 0.0087 0.9305 0.2304 0.046 Uiso 1 1 calc R . .
N52 N 0.1734(2) 0.92389(19) 0.29933(17) 0.0384(7) Uani 1 1 d . . .
H52A H 0.2260 0.9117 0.3221 0.046 Uiso 1 1 calc R . .
H52B H 0.1767 0.9806 0.2951 0.046 Uiso 1 1 calc R . .
C101 C 0.0869(2) 0.8550(2) 0.27074(17) 0.0302(7) Uani 1 1 d . . .
N60 N 0.4224(3) 0.01381(19) 0.07677(15) 0.0389(7) Uani 1 1 d . . .
H60A H 0.4502 -0.0026 0.1147 0.047 Uiso 1 1 calc R . .
H60B H 0.4178 0.0691 0.0772 0.047 Uiso 1 1 calc R . .
C103 C 0.2854(3) 0.0933(2) 0.53709(17) 0.0325(7) Uani 1 1 d . . .
N58 N 0.3043(3) 0.0633(2) 0.59876(17) 0.0508(9) Uani 1 1 d . . .
H58A H 0.3377 0.0240 0.6040 0.061 Uiso 1 1 calc R . .
H58B H 0.2832 0.0832 0.6333 0.061 Uiso 1 1 calc R . .
C104 C 0.3868(3) -0.0461(2) 0.01759(17) 0.0315(7) Uani 1 1 d . . .
N61 N 0.3945(2) -0.13038(19) 0.01776(14) 0.0362(7) Uani 1 1 d . . .
H61A H 0.3716 -0.1697 -0.0204 0.043 Uiso 1 1 calc R . .
H61B H 0.4223 -0.1462 0.0560 0.043 Uiso 1 1 calc R . .
N62 N 0.3441(2) -0.0207(2) -0.04087(15) 0.0382(7) Uani 1 1 d . . .
H62A H 0.3211 -0.0595 -0.0792 0.046 Uiso 1 1 calc R . .
H62B H 0.3395 0.0345 -0.0405 0.046 Uiso 1 1 calc R . .
N59 N 0.3174(2) 0.06329(19) 0.48425(15) 0.0351(6) Uani 1 1 d . . .
H59A H 0.3056 0.0833 0.4446 0.042 Uiso 1 1 calc R . .
H59B H 0.3503 0.0236 0.4892 0.042 Uiso 1 1 calc R . .
N57 N 0.2350(2) 0.1544(2) 0.52903(15) 0.0367(7) Uani 1 1 d . . .
H57A H 0.2234 0.1741 0.4893 0.044 Uiso 1 1 calc R . .
H57B H 0.2138 0.1743 0.5635 0.044 Uiso 1 1 calc R . .
C94 C 0.5270(3) 0.8277(3) 0.6989(2) 0.0443(9) Uani 1 1 d . . .
H94A H 0.5640 0.8116 0.6655 0.053 Uiso 1 1 calc R . .
H94B H 0.5137 0.7783 0.7275 0.053 Uiso 1 1 calc R . .
C4 C 0.7126(3) 0.8120(2) 0.1439(2) 0.0519(12) Uani 1 1 d . . .
C93 C 0.5901(4) 0.9148(3) 0.7436(3) 0.0632(14) Uani 1 1 d . . .
H93A H 0.6533 0.9079 0.7680 0.095 Uiso 1 1 calc R . .
H93B H 0.5540 0.9304 0.7771 0.095 Uiso 1 1 calc R . .
H93C H 0.6044 0.9636 0.7151 0.095 Uiso 1 1 calc R . .
C92 C 0.4696(5) 0.8618(3) 0.2234(2) 0.0637(15) Uani 1 1 d . . .
H92A H 0.4891 0.9093 0.2641 0.076 Uiso 1 1 calc R . .
H92B H 0.4974 0.8124 0.2362 0.076 Uiso 1 1 calc R . .
N63 N 0.0411(2) 0.3692(2) 0.03752(13) 0.0342(7) Uani 1 1 d . . .
H63A H 0.0245 0.3772 0.0769 0.041 Uiso 1 1 calc R . .
H63B H 0.0980 0.3590 0.0367 0.041 Uiso 1 1 calc R . .
N64 N 0.0024(2) 0.3581(2) -0.08315(14) 0.0409(8) Uani 1 1 d . . .
H64A H -0.0389 0.3588 -0.1218 0.049 Uiso 1 1 calc R . .
H64B H 0.0593 0.3479 -0.0840 0.049 Uiso 1 1 calc R . .
N56 N 0.9101(2) 0.4260(2) 0.42545(15) 0.0353(6) Uani 1 1 d . . .
H56A H 0.9477 0.4041 0.4037 0.042 Uiso 1 1 calc R . .
H56B H 0.8668 0.3897 0.4445 0.042 Uiso 1 1 calc R . .
N54 N 0.9851(2) 0.5728(2) 0.40064(16) 0.0397(7) Uani 1 1 d . . .
H54A H 1.0234 0.5523 0.3787 0.048 Uiso 1 1 calc R . .
H54B H 0.9897 0.6308 0.4039 0.048 Uiso 1 1 calc R . .
N65 N -0.1089(2) 0.3883(2) -0.02134(14) 0.0369(7) Uani 1 1 d . . .
H65A H -0.1500 0.3890 -0.0600 0.044 Uiso 1 1 calc R . .
H65B H -0.1247 0.3979 0.0181 0.044 Uiso 1 1 calc R . .
N55 N 0.8586(2) 0.5471(2) 0.46229(16) 0.0410(7) Uani 1 1 d . . .
H55A H 0.8147 0.5098 0.4804 0.049 Uiso 1 1 calc R . .
H55B H 0.8637 0.6052 0.4653 0.049 Uiso 1 1 calc R . .
C105 C -0.0217(2) 0.3727(3) -0.02255(16) 0.0318(7) Uani 1 1 d . . .
C102 C 0.9190(3) 0.5148(3) 0.42948(16) 0.0324(7) Uani 1 1 d . . .
O6' O 0.7050(4) 0.8911(3) 0.1623(3) 0.0410(18) Uani 0.639(13) 1 d PU A 5
O6 O 0.7464(6) 0.9020(4) 0.1224(7) 0.045(4) Uani 0.361(13) 1 d PU A 6
C91 C 0.3563(4) 0.8243(3) 0.1996(3) 0.0623(14) Uani 1 1 d . . .
H91A H 0.3281 0.7974 0.2368 0.094 Uiso 1 1 calc R . .
H91B H 0.3377 0.7773 0.1593 0.094 Uiso 1 1 calc R . .
H91C H 0.3295 0.8738 0.1873 0.094 Uiso 1 1 calc R . .
O92 O 0.5086(2) 0.90059(18) 0.16713(15) 0.0524(7) Uani 1 1 d . . .
H92 H 0.4851 0.9425 0.1568 0.079 Uiso 1 1 calc R . .
O4W O 0.2200(3) 0.1895(2) 0.10078(17) 0.0587(8) Uani 1 1 d D . .
O10W O 0.1643(3) 0.2021(3) 0.65650(16) 0.0712(11) Uani 1 1 d D . .
O9W O 0.9644(3) 0.7487(3) 0.4385(2) 0.0859(11) Uiso 1 1 d . . .
O11W O 0.1808(5) 0.0477(4) 0.7023(3) 0.1222(17) Uani 1 1 d . . .
O5W O -0.0050(5) 1.0601(4) 0.2106(3) 0.038(2) Uiso 0.408(11) 1 d P . .
O5W' O -0.0628(9) 1.0321(8) 0.1585(7) 0.150(5) Uiso 0.592(11) 1 d P . .
O8W O 0.3480(19) -0.016(2) 0.7363(14) 0.238(9) Uiso 0.55(2) 1 d P . .
O7W O -0.1174(6) 1.1360(5) 0.2755(5) 0.042(3) Uiso 0.353(16) 1 d P . .
O7W' O -0.1083(12) 1.1118(12) 0.3125(12) 0.221(7) Uiso 0.647(16) 1 d P . .
O3P O 1.0660(8) 0.8374(7) 0.4717(5) 0.126(5) Uiso 0.606(17) 1 d P . .
O4P O 1.1393(7) 0.8128(6) 0.5127(5) 0.081(4) Uiso 0.470(13) 1 d P . .
O6W O -0.0618(9) 1.1580(8) 0.1209(6) 0.263(5) Uiso 1 1 d . . .
O1P O 0.0635(10) 1.0201(9) 0.0705(7) 0.057(5) Uiso 0.248(11) 1 d P . .
O2P O -0.0089(14) 1.0403(13) 0.3727(10) 0.178(11) Uiso 0.42(2) 1 d P . .
O8W' O 0.3173(6) -0.0616(6) 0.7103(4) 0.058(4) Uiso 0.45(2) 1 d P . .
H1WA H 0.2105(17) 0.602(2) 0.2028(12) 0.032(9) Uiso 1 1 d D . .
H1WB H 0.120(3) 0.534(2) 0.177(2) 0.11(2) Uiso 1 1 d D . .
H2WB H 0.389(6) 0.168(4) 0.1030(18) 0.18(4) Uiso 1 1 d D . .
H2WA H 0.446(3) 0.2459(16) 0.082(2) 0.071(16) Uiso 1 1 d D . .
H3WB H 0.440(3) 0.927(3) 0.595(2) 0.049(13) Uiso 1 1 d . . .
H3WB H 0.517(3) 1.011(3) 0.590(2) 0.044(11) Uiso 1 1 d . . .
H4WA H 0.181(3) 0.1385(16) 0.0721(18) 0.070(16) Uiso 1 1 d D . .
H4WB H 0.217(4) 0.2328(19) 0.0751(19) 0.081(19) Uiso 1 1 d D . .
H10C H 0.202(4) 0.2424(17) 0.6925(14) 0.10(2) Uiso 1 1 d D . .
H10D H 0.154(2) 0.1491(11) 0.6719(14) 0.007(8) Uiso 1 1 d D . .
V11 V 0.26232(3) 0.60735(3) 0.36363(2) 0.01522(10) Uani 1 1 d . . .
V21 V 0.30721(3) 0.39639(3) 0.41071(2) 0.01649(10) Uani 1 1 d . . .
O11 O 0.14166(14) 0.57191(14) 0.32336(10) 0.0213(4) Uani 1 1 d . . .
O23 O 0.43051(14) 0.41583(13) 0.38128(9) 0.0179(4) Uani 1 1 d . . .
O14 O 0.26252(15) 0.74696(13) 0.36838(10) 0.0214(4) Uani 1 1 d . . .
O24 O 0.29063(16) 0.25899(14) 0.40935(11) 0.0247(4) Uani 1 1 d . . .
O13 O 0.32261(14) 0.62771(13) 0.28648(9) 0.0175(4) Uani 1 1 d . . .
O25 O 0.15642(15) 0.35558(14) 0.40917(10) 0.0226(4) Uani 1 1 d . . .
O12 O 0.29282(14) 0.50970(13) 0.38084(10) 0.0192(4) Uani 1 1 d . . .
O15 O 0.23808(15) 0.62594(14) 0.46109(10) 0.0222(4) Uani 1 1 d . . .
O21 O 0.34785(15) 0.42617(14) 0.49374(10) 0.0224(4) Uani 1 1 d . . .
C72 C 0.3904(2) 0.38652(17) 0.25453(13) 0.0155(5) Uani 1 1 d . . .
V1 V 0.76174(3) 0.63714(3) 0.16433(2) 0.01567(10) Uani 1 1 d . . .
V31 V 0.68293(3) 0.38839(3) 0.10838(2) 0.01575(10) Uani 1 1 d . . .
O33 O 0.55749(15) 0.36644(13) 0.14101(9) 0.0200(4) Uani 1 1 d . A .
O3 O 0.70270(14) 0.64361(15) 0.24176(10) 0.0221(4) Uani 1 1 d . A .
O4 O 0.78183(17) 0.78080(15) 0.17296(12) 0.0311(5) Uani 1 1 d . A .
O1 O 0.87963(14) 0.65732(14) 0.20660(10) 0.0206(4) Uani 1 1 d . A .
O5 O 0.79693(15) 0.66141(14) 0.07159(10) 0.0210(4) Uani 1 1 d . A .
O31 O 0.63689(15) 0.37491(14) 0.02517(10) 0.0214(4) Uani 1 1 d . A .
O35 O 0.83091(15) 0.40772(15) 0.10864(10) 0.0225(4) Uani 1 1 d . A .
O34 O 0.67394(17) 0.25318(14) 0.11328(10) 0.0255(4) Uani 1 1 d . A .
O2 O 0.71422(14) 0.52040(13) 0.13767(9) 0.0188(4) Uani 1 1 d . A .
N31 N 0.75611(17) 0.38712(16) 0.22651(12) 0.0182(5) Uani 1 1 d . A .
N1 N 0.61402(17) 0.64754(15) 0.09621(11) 0.0166(4) Uani 1 1 d . A .
C62 C 0.5034(2) 0.64846(17) 0.33406(13) 0.0155(5) Uani 1 1 d . . .
N11 N 0.42242(17) 0.69552(15) 0.42850(11) 0.0161(4) Uani 1 1 d . . .
C71 C 0.4599(2) 0.40811(18) 0.32217(13) 0.0166(5) Uani 1 1 d . A .
C81 C 0.5330(2) 0.38349(18) 0.20046(13) 0.0161(5) Uani 1 1 d . . .
C73 C 0.4279(2) 0.37298(18) 0.19667(13) 0.0170(5) Uani 1 1 d . A .
H73 H 0.3824 0.3561 0.1528 0.020 Uiso 1 1 calc R . .
C61 C 0.41625(19) 0.62998(17) 0.27760(13) 0.0154(5) Uani 1 1 d . A .
C82 C 0.6039(2) 0.41192(18) 0.26737(13) 0.0164(5) Uani 1 1 d . A .
C83 C 0.5650(2) 0.42202(18) 0.32592(13) 0.0170(5) Uani 1 1 d . . .
H83 H 0.6103 0.4388 0.3699 0.020 Uiso 1 1 calc R A .
C63 C 0.5968(2) 0.65332(18) 0.31802(13) 0.0167(5) Uani 1 1 d . A .
H63 H 0.6546 0.6675 0.3548 0.020 Uiso 1 1 calc R . .
N21 N 0.22662(17) 0.33140(16) 0.29358(12) 0.0180(4) Uani 1 1 d . . .
O27 O -0.00588(16) 0.31662(16) 0.34891(12) 0.0287(5) Uani 1 1 d . . .
C51 C 0.6081(2) 0.63797(18) 0.24972(14) 0.0167(5) Uani 1 1 d . . .
C52 C 0.5208(2) 0.61679(18) 0.19317(13) 0.0157(5) Uani 1 1 d . A .
C53 C 0.4276(2) 0.61464(17) 0.20850(13) 0.0155(5) Uani 1 1 d . . .
H53 H 0.3703 0.6026 0.1715 0.019 Uiso 1 1 calc R A .
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
N11 C11 C62 114.7(2) . . ?
N1 C1 C52 113.8(2) . . ?
N31 C31 C82 115.5(2) . . ?
N11 C13 C15 112.2(2) . . ?
N21 C21 C72 113.6(2) . . ?
O37 C35 O35 124.2(3) . . ?
O37 C35 C33 119.6(2) . . ?
O35 C35 C33 116.2(2) . . ?
O27 C25 O25 124.6(3) . . ?
O27 C25 C23 118.6(2) . . ?
O25 C25 C23 116.7(2) . . ?
N11 C12 C14 112.4(2) . . ?
N1 C2 C4 112.3(2) . . ?
N1 C3 C5 110.8(2) . . ?
N21 C23 C25 111.4(2) . . ?
N21 C22 C24 112.7(2) . . ?
O16 C14 O14 124.7(3) . . ?
O16 C14 C12 118.8(2) . . ?
O14 C14 C12 116.4(2) . . ?
O7 C5 O5 123.2(3) . . ?
O7 C5 C3 121.6(2) . . ?
O5 C5 C3 115.2(2) . . ?
N31 C33 C35 112.4(2) . . ?
O17 C15 O15 122.9(3) . . ?
O17 C15 C13 120.2(2) . . ?
O15 C15 C13 116.8(2) . . ?
N31 C32 C34 112.9(2) . . ?
O36 C34 O34 123.4(3) . . ?
O36 C34 C32 119.5(3) . . ?
O34 C34 C32 117.0(3) . . ?
O26 C24 O24 123.0(3) . . ?
O26 C24 C22 118.8(3) . . ?
O24 C24 C22 118.1(2) . . ?
N53 C101 N52 119.6(3) . . ?
N53 C101 N51 120.4(3) . . ?
N52 C101 N51 120.0(3) . . ?
N59 C103 N57 119.6(3) . . ?
N59 C103 N58 120.2(3) . . ?
N57 C103 N58 120.2(3) . . ?
N61 C104 N62 120.7(3) . . ?
N61 C104 N60 119.3(3) . . ?
N62 C104 N60 120.0(3) . . ?
O91 C94 C93 111.3(3) . . ?
O4 C4 O6' 125.3(3) . . ?
O4 C4 O6 116.3(5) . . ?
O6' C4 O6 45.6(4) . . ?
O4 C4 C2 119.2(3) . . ?
O6' C4 C2 113.0(3) . . ?
O6 C4 C2 115.7(4) . . ?
O92 C92 C91 107.9(3) . . ?
N65 C105 N64 119.9(3) . . ?
N65 C105 N63 120.0(3) . . ?
N64 C105 N63 120.1(3) . . ?
N56 C102 N54 121.5(3) . . ?
N56 C102 N55 119.1(3) . . ?
N54 C102 N55 119.4(3) . . ?
O4P O3P O9W 112.0(8) . . ?
O11 V11 O12 106.00(10) . . ?
O11 V11 O13 100.07(9) . . ?
O12 V11 O13 97.02(9) . . ?
O11 V11 O15 95.47(9) . . ?
O12 V11 O15 90.43(9) . . ?
O13 V11 O15 160.16(8) . . ?
O11 V11 O14 89.90(9) . . ?
O12 V11 O14 162.64(8) . . ?
O13 V11 O14 86.77(8) . . ?
O15 V11 O14 80.96(8) . . ?
O11 V11 N11 163.69(9) . . ?
O12 V11 N11 88.95(9) . . ?
O13 V11 N11 84.18(8) . . ?
O15 V11 N11 77.57(8) . . ?
O14 V11 N11 74.54(8) . . ?
O21 V21 O23 101.80(9) . . ?
O21 V21 O12 101.76(9) . . ?
O23 V21 O12 91.46(8) . . ?
O21 V21 O25 96.79(9) . . ?
O23 V21 O25 161.13(8) . . ?
O12 V21 O25 87.90(8) . . ?
O21 V21 O24 96.94(9) . . ?
O23 V21 O24 90.47(9) . . ?
O12 V21 O24 160.39(8) . . ?
O25 V21 O24 84.03(9) . . ?
O21 V21 N21 170.23(10) . . ?
O23 V21 N21 85.42(8) . . ?
O12 V21 N21 84.45(8) . . ?
O25 V21 N21 75.74(8) . . ?
O24 V21 N21 76.25(8) . . ?
C71 O23 V21 138.12(17) . . ?
C14 O14 V11 122.19(17) . . ?
C24 O24 V21 123.18(19) . . ?
C61 O13 V11 131.78(16) . . ?
C25 O25 V21 122.33(19) . . ?
V11 O12 V21 168.81(12) . . ?
C15 O15 V11 121.29(18) . . ?
C73 C72 C71 118.1(2) . . ?
C73 C72 C21 118.9(2) . . ?
C71 C72 C21 122.9(2) . . ?
O1 V1 O2 105.71(10) . . ?
O1 V1 O3 98.64(9) . . ?
O2 V1 O3 99.01(9) . . ?
O1 V1 O5 94.71(9) . . ?
O2 V1 O5 92.15(9) . . ?
O3 V1 O5 159.55(9) . . ?
O1 V1 O4 91.04(9) . . ?
O2 V1 O4 162.36(9) . . ?
O3 V1 O4 83.57(10) . . ?
O5 V1 O4 80.76(9) . . ?
O1 V1 N1 164.39(9) . . ?
O2 V1 N1 87.39(8) . . ?
O3 V1 N1 87.39(8) . . ?
O5 V1 N1 75.99(8) . . ?
O4 V1 N1 75.26(8) . . ?
O31 V31 O2 103.82(9) . . ?
O31 V31 O33 99.86(9) . . ?
O2 V31 O33 88.95(8) . . ?
O31 V31 O35 99.20(9) . . ?
O2 V31 O35 90.19(8) . . ?
O33 V31 O35 160.56(8) . . ?
O31 V31 O34 96.07(9) . . ?
O2 V31 O34 160.04(8) . . ?
O33 V31 O34 89.32(9) . . ?
O35 V31 O34 84.91(9) . . ?
O31 V31 N31 171.28(9) . . ?
O2 V31 N31 84.23(8) . . ?
O33 V31 N31 83.45(8) . . ?
O35 V31 N31 77.13(8) . . ?
O34 V31 N31 75.82(8) . . ?
C81 O33 V31 136.43(17) . . ?
C51 O3 V1 134.80(16) . . ?
C4 O4 V1 122.0(2) . . ?
C5 O5 V1 120.27(18) . . ?
C35 O35 V31 122.94(18) . . ?
C34 O34 V31 123.83(19) . . ?
V1 O2 V31 170.73(12) . . ?
C32 N31 C33 111.3(2) . . ?
C32 N31 C31 110.6(2) . . ?
C33 N31 C31 109.2(2) . . ?
C32 N31 V31 107.55(16) . . ?
C33 N31 V31 104.22(15) . . ?
C31 N31 V31 113.86(15) . . ?
C2 N1 C3 110.9(2) . . ?
C2 N1 C1 111.5(2) . . ?
C3 N1 C1 110.5(2) . . ?
C2 N1 V1 111.13(16) . . ?
C3 N1 V1 102.27(15) . . ?
C1 N1 V1 110.17(15) . . ?
C63 C62 C61 118.0(2) . . ?
C63 C62 C11 117.0(2) . . ?
C61 C62 C11 124.8(2) . . ?
C13 N11 C12 111.6(2) . . ?
C13 N11 C11 109.2(2) . . ?
C12 N11 C11 110.9(2) . . ?
C13 N11 V11 106.12(16) . . ?
C12 N11 V11 108.91(15) . . ?
C11 N11 V11 109.97(15) . . ?
O23 C71 C83 118.2(2) . . ?
O23 C71 C72 123.0(2) . . ?
C83 C71 C72 118.8(2) . . ?
O33 C81 C73 116.5(2) . . ?
O33 C81 C82 124.6(2) . . ?
C73 C81 C82 118.9(2) . . ?
C72 C73 C81 123.1(2) . . ?
O13 C61 C53 117.8(2) . . ?
O13 C61 C62 123.4(2) . . ?
C53 C61 C62 118.8(2) . . ?
C83 C82 C81 117.7(2) . . ?
C83 C82 C31 118.0(2) . . ?
C81 C82 C31 124.1(2) . . ?
C82 C83 C71 123.2(2) . . ?
C62 C63 C51 123.2(2) . . ?
C22 N21 C23 112.3(2) . . ?
C22 N21 C21 111.5(2) . . ?
C23 N21 C21 109.3(2) . . ?
C22 N21 V21 108.36(16) . . ?
C23 N21 V21 104.08(15) . . ?
C21 N21 V21 111.16(15) . . ?
O3 C51 C63 117.1(2) . . ?
O3 C51 C52 124.0(2) . . ?
C63 C51 C52 119.0(2) . . ?
C53 C52 C51 118.2(2) . . ?
C53 C52 C1 119.0(2) . . ?
C51 C52 C1 122.6(2) . . ?
C52 C53 C61 122.7(2) . . ?
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
C11 N11 1.487(3) . ?
C11 C62 1.503(3) . ?
O37 C35 1.229(3) . ?
C1 N1 1.487(4) . ?
C1 C52 1.513(4) . ?
C31 N31 1.494(3) . ?
C31 C82 1.509(4) . ?
C13 N11 1.469(3) . ?
C13 C15 1.516(4) . ?
C21 N21 1.489(4) . ?
C21 C72 1.494(4) . ?
C35 O35 1.281(3) . ?
C35 C33 1.529(4) . ?
C25 O27 1.240(3) . ?
C25 O25 1.275(3) . ?
C25 C23 1.518(4) . ?
C12 N11 1.473(3) . ?
C12 C14 1.515(4) . ?
C2 N1 1.481(3) . ?
C2 C4 1.494(4) . ?
C3 N1 1.482(3) . ?
C3 C5 1.517(4) . ?
O16 C14 1.239(3) . ?
O7 C5 1.232(3) . ?
C23 N21 1.473(4) . ?
C22 N21 1.467(3) . ?
C22 C24 1.516(4) . ?
C14 O14 1.274(3) . ?
C5 O5 1.287(3) . ?
C33 N31 1.484(4) . ?
O17 C15 1.240(3) . ?
C15 O15 1.284(3) . ?
O91 C94 1.429(4) . ?
O26 C24 1.235(4) . ?
C32 N31 1.471(4) . ?
C32 C34 1.510(4) . ?
C34 O36 1.226(4) . ?
C34 O34 1.279(4) . ?
N53 C101 1.309(4) . ?
C24 O24 1.281(4) . ?
N51 C101 1.338(4) . ?
N52 C101 1.330(4) . ?
N60 C104 1.327(4) . ?
C103 N59 1.310(4) . ?
C103 N57 1.322(4) . ?
C103 N58 1.332(4) . ?
C104 N61 1.316(4) . ?
C104 N62 1.325(4) . ?
C94 C93 1.456(5) . ?
C4 O4 1.259(4) . ?
C4 O6' 1.268(5) . ?
C4 O6 1.435(9) . ?
C92 O92 1.420(5) . ?
C92 C91 1.483(7) . ?
N63 C105 1.339(4) . ?
N64 C105 1.319(4) . ?
N56 C102 1.311(5) . ?
N54 C102 1.327(5) . ?
N65 C105 1.316(4) . ?
N55 C102 1.335(4) . ?
O9W O3P 1.621(10) . ?
O5W O5W' 1.132(12) . ?
O8W O8W' 0.78(3) . ?
O7W O7W' 0.84(2) . ?
O3P O4P 1.336(12) . ?
V11 O11 1.6255(19) . ?
V11 O12 1.7001(19) . ?
V11 O13 1.8792(19) . ?
V11 O15 2.0207(19) . ?
V11 O14 2.1135(19) . ?
V11 N11 2.298(2) . ?
V21 O21 1.5960(19) . ?
V21 O23 1.8798(19) . ?
V21 O12 1.9131(19) . ?
V21 O25 2.014(2) . ?
V21 O24 2.027(2) . ?
V21 N21 2.343(2) . ?
O23 C71 1.314(3) . ?
O13 C61 1.350(3) . ?
C72 C73 1.369(4) . ?
C72 C71 1.431(3) . ?
V1 O1 1.6222(19) . ?
V1 O2 1.6967(19) . ?
V1 O3 1.8785(19) . ?
V1 O5 2.012(2) . ?
V1 O4 2.104(2) . ?
V1 N1 2.287(2) . ?
V31 O31 1.6049(19) . ?
V31 O2 1.9339(19) . ?
V31 O33 1.937(2) . ?
V31 O35 2.007(2) . ?
V31 O34 2.030(2) . ?
V31 N31 2.345(2) . ?
O33 C81 1.308(3) . ?
O3 C51 1.346(3) . ?
C62 C63 1.390(4) . ?
C62 C61 1.418(3) . ?
C71 C83 1.413(4) . ?
C81 C73 1.420(4) . ?
C81 C82 1.428(3) . ?
C61 C53 1.405(4) . ?
C82 C83 1.383(4) . ?
C63 C51 1.390(4) . ?
C51 C52 1.416(3) . ?
C52 C53 1.390(4) . ?
