#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:06:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179093 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305583.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_4305583
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            'C37 H66 N13 Na O34 V4'
_chemical_formula_weight         1463.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.404(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3035(11)
_cell_length_b                   10.9657(5)
_cell_length_c                   28.3894(15)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1288
_cell_measurement_theta_min      3.1540
_cell_volume                     5890.7(5)
_computing_cell_refinement
;
'Mon Jun 05 18:53:59 2006'
;
_computing_data_collection
;
'Mon Jun 05 18:53:59 2006'
;
_computing_data_reduction
;
'Mon Jun 05 18:53:59 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 0.936
_diffrn_measured_fraction_theta_max 0.936
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0608
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            87133
_diffrn_reflns_theta_full        31.28
_diffrn_reflns_theta_max         31.28
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.729
_exptl_absorpt_correction_T_max  0.94139
_exptl_absorpt_correction_T_min  0.87518
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
'Mon Jun 05 18:53:59 2006'
;
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.14090
_exptl_crystal_size_mid          0.09630
_exptl_crystal_size_min          0.04378
_refine_diff_density_max         1.326
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.00000(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         18002
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0920
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          5.486
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0987P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1663
_reflns_number_gt                10604
_reflns_number_total             18002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800569t-file002_3.cif
_cod_data_source_block           vbiqna26
_cod_database_code               4305583
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Na1 Na 0.77613(7) 0.29365(12) 0.43533(5) 0.0406(3) Uani 1 1 d . . .
N55 N -0.02429(15) 0.2808(3) 0.20314(11) 0.0460(7) Uani 1 1 d . . .
H55A H -0.0566 0.2648 0.2192 0.055 Uiso 1 1 calc R . .
H55B H 0.0195 0.2700 0.2161 0.055 Uiso 1 1 calc R . .
C102 C -0.04160(18) 0.3214(3) 0.15914(13) 0.0387(7) Uani 1 1 d . . .
N54 N 0.00881(16) 0.3464(3) 0.13520(12) 0.0516(8) Uani 1 1 d . . .
H54A H 0.0524 0.3360 0.1486 0.062 Uiso 1 1 calc R . .
H54B H -0.0020 0.3732 0.1062 0.062 Uiso 1 1 calc R . .
N56 N -0.10881(15) 0.3378(3) 0.13932(11) 0.0482(8) Uani 1 1 d . . .
H56A H -0.1411 0.3218 0.1554 0.058 Uiso 1 1 calc R . .
H56B H -0.1203 0.3645 0.1103 0.058 Uiso 1 1 calc R . .
O1W O 0.88813(18) 0.3057(3) 0.41890(15) 0.0946(13) Uani 1 1 d . . .
O2W O 0.7410(2) 0.1336(4) 0.37970(16) 0.0715(14) Uani 0.758(6) 1 d PU . .
N53 N 0.39362(14) -0.0857(2) 0.02138(9) 0.0337(6) Uani 1 1 d . . .
H53A H 0.4110 -0.1252 0.0002 0.040 Uiso 1 1 calc R . .
H53B H 0.3941 -0.0073 0.0215 0.040 Uiso 1 1 calc R . .
C101 C 0.36618(15) -0.1457(3) 0.05382(10) 0.0286(6) Uani 1 1 d . . .
N51 N 0.36498(13) -0.2653(2) 0.05432(9) 0.0324(6) Uani 1 1 d . . .
H51A H 0.3822 -0.3059 0.0334 0.039 Uiso 1 1 calc R . .
H51B H 0.3470 -0.3031 0.0756 0.039 Uiso 1 1 calc R . .
N52 N 0.33961(15) -0.0834(3) 0.08658(9) 0.0397(7) Uani 1 1 d . . .
H52A H 0.3219 -0.1217 0.1078 0.048 Uiso 1 1 calc R . .
H52B H 0.3402 -0.0050 0.0864 0.048 Uiso 1 1 calc R . .
O90 O 0.94548(18) 0.2062(4) 0.35015(12) 0.0875(11) Uani 1 1 d . . .
H90 H 0.9293 0.1705 0.3250 0.131 Uiso 1 1 calc R . .
C91 C 0.9926(3) 0.2992(5) 0.3411(2) 0.0793(15) Uani 1 1 d . . .
H91A H 1.0114 0.3421 0.3708 0.095 Uiso 1 1 calc R . .
H91B H 0.9672 0.3576 0.3184 0.095 Uiso 1 1 calc R . .
N58 N 0.30497(14) 0.3805(3) 0.52418(9) 0.0371(6) Uani 1 1 d . . .
H58A H 0.2899 0.4175 0.5469 0.045 Uiso 1 1 calc R . .
H58B H 0.3290 0.4197 0.5066 0.045 Uiso 1 1 calc R . .
C90 C 1.0533(3) 0.2447(5) 0.32087(19) 0.0816(15) Uani 1 1 d . . .
H90A H 1.0846 0.3085 0.3152 0.122 Uiso 1 1 calc R . .
H90B H 1.0347 0.2036 0.2912 0.122 Uiso 1 1 calc R . .
H90C H 1.0787 0.1874 0.3435 0.122 Uiso 1 1 calc R . .
N59 N 0.25442(14) 0.2031(3) 0.54300(9) 0.0378(6) Uani 1 1 d . . .
H59A H 0.2392 0.2395 0.5658 0.045 Uiso 1 1 calc R . .
H59B H 0.2456 0.1269 0.5376 0.045 Uiso 1 1 calc R . .
N57 N 0.31279(15) 0.2070(3) 0.48031(10) 0.0424(7) Uani 1 1 d . . .
H57A H 0.3358 0.2464 0.4622 0.051 Uiso 1 1 calc R . .
H57B H 0.3037 0.1308 0.4752 0.051 Uiso 1 1 calc R . .
C103 C 0.29122(15) 0.2640(3) 0.51625(10) 0.0317(7) Uani 1 1 d . . .
O7W O 0.2289(3) 0.4501(5) 0.0152(2) 0.0721(13) Uiso 0.623(7) 1 d PU . .
O3W O 0.4699(6) -0.1040(8) 0.4801(3) 0.0815(14) Uiso 0.417(7) 1 d PU . .
O5W O 0.2605(3) 0.7395(5) 0.3854(2) 0.086(2) Uani 0.601(7) 1 d P . .
O8W' O 0.0886(5) 0.5418(7) -0.0517(3) 0.097(3) Uani 0.471(8) 1 d PU . .
O6W O 0.3421(4) 0.8699(7) 0.4201(2) 0.057(2) Uani 0.399(7) 1 d P . .
O4W O 0.3805(4) -0.2265(7) 0.4399(3) 0.080(3) Uani 0.459(8) 1 d PU . .
O4W' O 0.3270(4) -0.2410(9) 0.4103(3) 0.116(3) Uani 0.541(8) 1 d PU . .
O8W O 0.1369(3) 0.4772(6) -0.0664(3) 0.075(2) Uani 0.529(8) 1 d PU . .
O2W' O 0.7856(6) 0.0729(11) 0.4314(5) 0.079(4) Uani 0.242(6) 1 d PU . .
O3W' O 0.5103(4) -0.1310(6) 0.4715(2) 0.0815(14) Uiso 0.583(7) 1 d PU . .
O7W' O 0.2474(5) 0.4668(8) -0.0072(4) 0.0721(13) Uiso 0.377(7) 1 d PU . .
V21 V 0.52132(2) 0.17008(4) 0.097082(15) 0.01949(11) Uani 1 1 d . . .
V31 V 0.29524(2) 0.32572(4) 0.322238(15) 0.01802(10) Uani 1 1 d . . .
V11 V 0.68454(2) 0.27721(4) 0.167609(15) 0.01958(11) Uani 1 1 d . . .
V1 V 0.45665(2) 0.22280(5) 0.396042(16) 0.02332(11) Uani 1 1 d . . .
O12 O 0.60143(9) 0.22857(17) 0.13950(6) 0.0223(4) Uani 1 1 d . . .
O2 O 0.37515(9) 0.27586(17) 0.35810(6) 0.0220(4) Uani 1 1 d . . .
O23 O 0.47664(10) 0.13343(17) 0.14619(6) 0.0228(4) Uani 1 1 d . . .
O33 O 0.33702(10) 0.36519(17) 0.26984(6) 0.0242(4) Uani 1 1 d . . .
O34 O 0.20042(10) 0.33327(18) 0.27554(7) 0.0283(4) Uani 1 1 d . . .
O3 O 0.49618(10) 0.16943(17) 0.34638(6) 0.0238(4) Uani 1 1 d . . .
O21 O 0.54490(10) 0.03719(17) 0.08244(7) 0.0277(4) Uani 1 1 d . . .
O13 O 0.65843(10) 0.33883(16) 0.22282(6) 0.0232(4) Uani 1 1 d . . .
N31 N 0.28327(11) 0.13551(19) 0.28847(7) 0.0177(4) Uani 1 1 d . . .
O35 O 0.23760(10) 0.23911(17) 0.36276(6) 0.0229(4) Uani 1 1 d . . .
O24 O 0.42674(10) 0.16492(18) 0.05163(7) 0.0290(4) Uani 1 1 d . . .
N11 N 0.69879(11) 0.0973(2) 0.21036(7) 0.0202(4) Uani 1 1 d . . .
O11 O 0.69828(10) 0.40236(17) 0.14055(7) 0.0273(4) Uani 1 1 d . . .
O14 O 0.78960(10) 0.27804(19) 0.20423(7) 0.0304(4) Uani 1 1 d . . .
O15 O 0.72760(10) 0.16719(18) 0.12505(7) 0.0260(4) Uani 1 1 d . . .
O25 O 0.55497(10) 0.25527(17) 0.04414(7) 0.0257(4) Uani 1 1 d . . .
C73 C 0.40252(13) 0.3739(2) 0.20933(9) 0.0179(5) Uani 1 1 d . . .
H73 H 0.3985 0.4584 0.2100 0.021 Uiso 1 1 calc R . .
O31 O 0.28289(10) 0.45963(17) 0.34255(7) 0.0271(4) Uani 1 1 d . . .
C72 C 0.44003(13) 0.3220(2) 0.17758(9) 0.0177(5) Uani 1 1 d . . .
O4 O 0.55468(11) 0.2167(2) 0.43637(7) 0.0412(6) Uani 1 1 d . . .
N21 N 0.48015(11) 0.3658(2) 0.10040(7) 0.0189(4) Uani 1 1 d . . .
O5 O 0.43395(11) 0.3265(2) 0.44869(7) 0.0341(5) Uani 1 1 d . . .
N1 N 0.50410(12) 0.4124(2) 0.38434(8) 0.0278(5) Uani 1 1 d . . .
C51 C 0.53587(13) 0.2149(2) 0.31704(9) 0.0197(5) Uani 1 1 d . . .
C61 C 0.61876(13) 0.2927(2) 0.25256(9) 0.0191(5) Uani 1 1 d . . .
O17 O 0.75655(11) -0.01819(19) 0.10451(7) 0.0330(5) Uani 1 1 d . . .
C31 C 0.34946(13) 0.0931(2) 0.27440(9) 0.0186(5) Uani 1 1 d . . .
H31A H 0.3416 0.0124 0.2604 0.022 Uiso 1 1 calc R . .
H31B H 0.3861 0.0863 0.3030 0.022 Uiso 1 1 calc R . .
O27 O 0.58849(11) 0.42687(19) 0.01372(7) 0.0323(5) Uani 1 1 d . . .
C21 C 0.48129(13) 0.4043(2) 0.15089(9) 0.0183(5) Uani 1 1 d . . .
H21A H 0.4622 0.4862 0.1506 0.022 Uiso 1 1 calc R . .
H21B H 0.5300 0.4070 0.1681 0.022 Uiso 1 1 calc R . .
C12 C 0.75942(14) 0.1142(3) 0.25070(9) 0.0247(6) Uani 1 1 d . . .
H12A H 0.7812 0.0359 0.2600 0.030 Uiso 1 1 calc R . .
H12B H 0.7429 0.1478 0.2781 0.030 Uiso 1 1 calc R . .
C11 C 0.63329(13) 0.0679(2) 0.22848(9) 0.0199(5) Uani 1 1 d . . .
H11A H 0.6416 -0.0058 0.2477 0.024 Uiso 1 1 calc R . .
H11B H 0.5957 0.0506 0.2012 0.024 Uiso 1 1 calc R . .
C82 C 0.37492(13) 0.1753(2) 0.23937(8) 0.0180(5) Uani 1 1 d . . .
C32 C 0.22428(14) 0.1375(3) 0.24637(9) 0.0228(5) Uani 1 1 d . . .
H32A H 0.1954 0.0653 0.2470 0.027 Uiso 1 1 calc R . .
H32B H 0.2434 0.1347 0.2172 0.027 Uiso 1 1 calc R . .
C1 C 0.50400(14) 0.4348(3) 0.33269(9) 0.0239(6) Uani 1 1 d . . .
H1A H 0.5243 0.5145 0.3293 0.029 Uiso 1 1 calc R . .
H1B H 0.4555 0.4360 0.3151 0.029 Uiso 1 1 calc R . .
O1 O 0.43231(10) 0.0977(2) 0.41671(7) 0.0328(5) Uani 1 1 d . . .
O36 O 0.12330(12) 0.2551(2) 0.21474(8) 0.0429(6) Uani 1 1 d . . .
C71 C 0.44270(13) 0.1934(2) 0.17534(9) 0.0185(5) Uani 1 1 d . . .
C23 C 0.53034(14) 0.4426(2) 0.08025(9) 0.0228(5) Uani 1 1 d . . .
H23A H 0.5687 0.4680 0.1058 0.027 Uiso 1 1 calc R . .
H23B H 0.5063 0.5152 0.0658 0.027 Uiso 1 1 calc R . .
C33 C 0.26743(14) 0.0556(2) 0.32687(9) 0.0223(5) Uani 1 1 d . . .
H33A H 0.3112 0.0244 0.3457 0.027 Uiso 1 1 calc R . .
H33B H 0.2394 -0.0133 0.3126 0.027 Uiso 1 1 calc R . .
C83 C 0.40949(13) 0.1231(2) 0.20596(9) 0.0188(5) Uani 1 1 d . . .
H83 H 0.4108 0.0385 0.2037 0.023 Uiso 1 1 calc R . .
C25 C 0.55994(14) 0.3723(3) 0.04263(9) 0.0241(6) Uani 1 1 d . . .
C52 C 0.54459(13) 0.3406(2) 0.31058(9) 0.0210(5) Uani 1 1 d . . .
O16 O 0.87596(11) 0.1902(2) 0.25645(9) 0.0456(6) Uani 1 1 d . . .
O7 O 0.40341(13) 0.5093(2) 0.47147(8) 0.0508(7) Uani 1 1 d . . .
C3 C 0.45553(17) 0.4983(3) 0.40195(11) 0.0358(7) Uani 1 1 d . . .
H3A H 0.4155 0.5156 0.3763 0.043 Uiso 1 1 calc R . .
H3B H 0.4800 0.5744 0.4114 0.043 Uiso 1 1 calc R . .
C81 C 0.37024(13) 0.3045(2) 0.24059(8) 0.0176(5) Uani 1 1 d . . .
C35 C 0.22728(14) 0.1243(3) 0.35950(9) 0.0234(5) Uani 1 1 d . . .
C34 C 0.17847(15) 0.2491(3) 0.24521(10) 0.0286(6) Uani 1 1 d . . .
O37 O 0.18988(13) 0.06886(19) 0.38255(8) 0.0396(5) Uani 1 1 d . . .
C53 C 0.58811(13) 0.3765(2) 0.27923(9) 0.0201(5) Uani 1 1 d . . .
H53 H 0.5970 0.4592 0.2760 0.024 Uiso 1 1 calc R . .
C13 C 0.71211(16) 0.0011(3) 0.17657(10) 0.0277(6) Uani 1 1 d . . .
H13A H 0.6694 -0.0468 0.1668 0.033 Uiso 1 1 calc R . .
H13B H 0.7487 -0.0530 0.1932 0.033 Uiso 1 1 calc R . .
C62 C 0.60851(13) 0.1662(2) 0.25817(8) 0.0183(5) Uani 1 1 d . . .
C15 C 0.73470(14) 0.0511(3) 0.13191(10) 0.0261(6) Uani 1 1 d . . .
C24 C 0.38519(15) 0.2583(3) 0.04314(11) 0.0306(6) Uani 1 1 d . . .
C63 C 0.56826(13) 0.1308(2) 0.29123(9) 0.0205(5) Uani 1 1 d . . .
H63 H 0.5626 0.0480 0.2964 0.025 Uiso 1 1 calc R . .
C22 C 0.40789(14) 0.3729(3) 0.07067(9) 0.0238(6) Uani 1 1 d . . .
H22A H 0.4060 0.4400 0.0482 0.029 Uiso 1 1 calc R . .
H22B H 0.3748 0.3905 0.0914 0.029 Uiso 1 1 calc R . .
C2 C 0.57629(16) 0.4199(4) 0.41349(10) 0.0417(9) Uani 1 1 d . . .
H2A H 0.5772 0.4805 0.4385 0.050 Uiso 1 1 calc R . .
H2B H 0.6084 0.4466 0.3932 0.050 Uiso 1 1 calc R . .
O26 O 0.32830(12) 0.2567(2) 0.01440(10) 0.0522(7) Uani 1 1 d . . .
C14 C 0.81302(15) 0.1985(3) 0.23652(11) 0.0316(7) Uani 1 1 d . . .
O6 O 0.66448(12) 0.2892(4) 0.45393(10) 0.0727(10) Uani 1 1 d . . .
C4 C 0.60130(17) 0.3023(4) 0.43590(11) 0.0482(10) Uani 1 1 d . . .
C5 C 0.42948(16) 0.4439(3) 0.44467(11) 0.0369(8) Uani 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'
Na Na 0.0362 0.0249 '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
O1W Na1 O6 177.47(14) . . ?
O1W Na1 O26 87.97(14) . 4_666 ?
O6 Na1 O26 91.13(10) . 4_666 ?
O1W Na1 O2W 93.66(14) . . ?
O6 Na1 O2W 88.85(14) . . ?
O26 Na1 O2W 118.52(14) 4_666 . ?
O1W Na1 O17 91.45(12) . 2_655 ?
O6 Na1 O17 87.44(11) . 2_655 ?
O26 Na1 O17 133.25(10) 4_666 2_655 ?
O2W Na1 O17 108.17(13) . 2_655 ?
O1W Na1 O2W' 88.0(3) . . ?
O6 Na1 O2W' 94.1(4) . . ?
O26 Na1 O2W' 77.7(3) 4_666 . ?
O2W Na1 O2W' 41.1(3) . . ?
O17 Na1 O2W' 149.0(3) 2_655 . ?
N55 C102 N56 119.9(3) . . ?
N55 C102 N54 119.2(3) . . ?
N56 C102 N54 120.9(3) . . ?
O2W' O2W Na1 71.5(4) . . ?
N51 C101 N53 121.0(3) . . ?
N51 C101 N52 119.6(3) . . ?
N53 C101 N52 119.5(3) . . ?
O90 C91 C90 110.6(4) . . ?
N58 C103 N59 120.5(3) . . ?
N58 C103 N57 120.3(3) . . ?
N59 C103 N57 119.3(3) . . ?
O4W' O6W O4W 54.7(5) 1_565 1_565 ?
O4W' O4W O6W 59.3(6) . 1_545 ?
O4W O4W' O6W 66.0(6) . 1_545 ?
O4W O4W' O5W 167.8(10) . 1_545 ?
O6W O4W' O5W 114.7(7) 1_545 1_545 ?
O2W O2W' Na1 67.4(4) . . ?
O21 V21 O23 101.48(9) . . ?
O21 V21 O12 103.68(9) . . ?
O23 V21 O12 92.24(8) . . ?
O21 V21 O25 94.54(9) . . ?
O23 V21 O25 163.31(8) . . ?
O12 V21 O25 88.47(8) . . ?
O21 V21 O24 94.36(9) . . ?
O23 V21 O24 88.73(8) . . ?
O12 V21 O24 161.34(8) . . ?
O25 V21 O24 85.37(8) . . ?
O21 V21 N21 167.59(9) . . ?
O23 V21 N21 87.41(8) . . ?
O12 V21 N21 84.39(8) . . ?
O25 V21 N21 76.05(7) . . ?
O24 V21 N21 77.04(8) . . ?
O31 V31 O2 104.53(10) . . ?
O31 V31 O33 100.98(9) . . ?
O2 V31 O33 93.74(8) . . ?
O31 V31 O35 95.08(8) . . ?
O2 V31 O35 92.50(8) . . ?
O33 V31 O35 160.70(8) . . ?
O31 V31 O34 91.05(9) . . ?
O2 V31 O34 163.95(8) . . ?
O33 V31 O34 86.94(8) . . ?
O35 V31 O34 82.11(8) . . ?
O31 V31 N31 165.96(9) . . ?
O2 V31 N31 87.91(8) . . ?
O33 V31 N31 84.37(8) . . ?
O35 V31 N31 77.63(7) . . ?
O34 V31 N31 76.18(8) . . ?
O11 V11 O12 105.46(9) . . ?
O11 V11 O13 100.86(9) . . ?
O12 V11 O13 96.86(8) . . ?
O11 V11 O15 95.62(9) . . ?
O12 V11 O15 89.63(8) . . ?
O13 V11 O15 159.94(8) . . ?
O11 V11 O14 89.91(9) . . ?
O12 V11 O14 162.26(9) . . ?
O13 V11 O14 88.69(8) . . ?
O15 V11 O14 79.91(8) . . ?
O11 V11 N11 164.04(9) . . ?
O12 V11 N11 88.98(8) . . ?
O13 V11 N11 83.77(8) . . ?
O15 V11 N11 77.36(8) . . ?
O14 V11 N11 74.83(8) . . ?
O1 V1 O2 102.09(9) . . ?
O1 V1 O3 101.90(10) . . ?
O2 V1 O3 95.15(8) . . ?
O1 V1 O5 95.17(10) . . ?
O2 V1 O5 88.23(8) . . ?
O3 V1 O5 161.45(9) . . ?
O1 V1 O4 94.27(10) . . ?
O2 V1 O4 162.81(10) . . ?
O3 V1 O4 86.51(9) . . ?
O5 V1 O4 85.04(9) . . ?
O1 V1 N1 166.81(10) . . ?
O2 V1 N1 87.04(9) . . ?
O3 V1 N1 86.54(8) . . ?
O5 V1 N1 75.41(8) . . ?
O4 V1 N1 75.97(9) . . ?
V11 O12 V21 166.94(11) . . ?
V31 O2 V1 178.75(12) . . ?
C71 O23 V21 137.23(17) . . ?
C81 O33 V31 135.88(17) . . ?
C34 O34 V31 123.03(18) . . ?
C51 O3 V1 137.78(17) . . ?
C61 O13 V11 132.28(17) . . ?
C33 N31 C32 111.5(2) . . ?
C33 N31 C31 109.09(19) . . ?
C32 N31 C31 110.65(19) . . ?
C33 N31 V31 104.48(14) . . ?
C32 N31 V31 108.86(15) . . ?
C31 N31 V31 112.14(15) . . ?
C35 O35 V31 121.72(16) . . ?
C24 O24 V21 123.12(18) . . ?
C12 N11 C13 112.2(2) . . ?
C12 N11 C11 110.80(19) . . ?
C13 N11 C11 109.7(2) . . ?
C12 N11 V11 107.12(16) . . ?
C13 N11 V11 106.65(15) . . ?
C11 N11 V11 110.23(15) . . ?
C14 O14 V11 121.58(19) . . ?
C15 O15 V11 123.21(17) . . ?
C25 O25 V21 122.13(17) . . ?
C72 C73 C81 122.9(2) . . ?
C73 C72 C71 117.9(2) . . ?
C73 C72 C21 118.6(2) . . ?
C71 C72 C21 123.3(2) . . ?
C4 O4 V1 123.0(2) . . ?
C23 N21 C22 111.3(2) . . ?
C23 N21 C21 108.9(2) . . ?
C22 N21 C21 111.47(19) . . ?
C23 N21 V21 104.90(14) . . ?
C22 N21 V21 108.64(16) . . ?
C21 N21 V21 111.38(14) . . ?
C5 O5 V1 121.46(18) . . ?
C2 N1 C3 111.4(2) . . ?
C2 N1 C1 111.2(2) . . ?
C3 N1 C1 110.5(2) . . ?
C2 N1 V1 109.0(2) . . ?
C3 N1 V1 103.10(16) . . ?
C1 N1 V1 111.44(16) . . ?
O3 C51 C63 116.8(2) . . ?
O3 C51 C52 123.1(2) . . ?
C63 C51 C52 120.1(2) . . ?
O13 C61 C53 116.6(2) . . ?
O13 C61 C62 123.3(2) . . ?
C53 C61 C62 120.1(2) . . ?
C15 O17 Na1 138.65(19) . 2_645 ?
N31 C31 C82 113.8(2) . . ?
N21 C21 C72 114.0(2) . . ?
N11 C12 C14 110.6(2) . . ?
N11 C11 C62 115.1(2) . . ?
C83 C82 C81 118.0(2) . . ?
C83 C82 C31 118.2(2) . . ?
C81 C82 C31 123.7(2) . . ?
N31 C32 C34 112.6(2) . . ?
N1 C1 C52 113.5(2) . . ?
O23 C71 C83 117.1(2) . . ?
O23 C71 C72 123.3(2) . . ?
C83 C71 C72 119.6(2) . . ?
N21 C23 C25 110.4(2) . . ?
N31 C33 C35 111.2(2) . . ?
C82 C83 C71 122.4(2) . . ?
O27 C25 O25 123.6(2) . . ?
O27 C25 C23 120.2(3) . . ?
O25 C25 C23 116.2(2) . . ?
C53 C52 C51 117.6(2) . . ?
C53 C52 C1 120.0(2) . . ?
C51 C52 C1 122.2(2) . . ?
N1 C3 C5 110.5(3) . . ?
O33 C81 C73 117.0(2) . . ?
O33 C81 C82 123.9(2) . . ?
C73 C81 C82 119.1(2) . . ?
O37 C35 O35 123.4(3) . . ?
O37 C35 C33 120.3(2) . . ?
O35 C35 C33 116.2(2) . . ?
O36 C34 O34 124.0(3) . . ?
O36 C34 C32 118.7(3) . . ?
O34 C34 C32 117.2(2) . . ?
C61 C53 C52 122.2(2) . . ?
N11 C13 C15 113.4(2) . . ?
C63 C62 C61 117.4(2) . . ?
C63 C62 C11 117.5(2) . . ?
C61 C62 C11 124.9(2) . . ?
O17 C15 O15 123.9(3) . . ?
O17 C15 C13 119.9(3) . . ?
O15 C15 C13 116.2(2) . . ?
O26 C24 O24 123.4(3) . . ?
O26 C24 C22 119.2(3) . . ?
O24 C24 C22 117.4(2) . . ?
C62 C63 C51 122.5(2) . . ?
N21 C22 C24 113.5(2) . . ?
N1 C2 C4 112.6(3) . . ?
C24 O26 Na1 142.9(2) . 4_565 ?
O16 C14 O14 123.5(3) . . ?
O16 C14 C12 119.9(3) . . ?
O14 C14 C12 116.5(2) . . ?
C4 O6 Na1 142.2(2) . . ?
O6 C4 O4 122.7(4) . . ?
O6 C4 C2 119.5(4) . . ?
O4 C4 C2 117.8(3) . . ?
O7 C5 O5 123.8(3) . . ?
O7 C5 C3 120.5(3) . . ?
O5 C5 C3 115.6(3) . . ?
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
Na1 O1W 2.304(3) . ?
Na1 O6 2.319(3) . ?
Na1 O26 2.338(3) 4_666 ?
Na1 O2W 2.369(4) . ?
Na1 O17 2.377(3) 2_655 ?
Na1 O2W' 2.432(11) . ?
N55 C102 1.306(4) . ?
C102 N56 1.321(4) . ?
C102 N54 1.321(4) . ?
O2W O2W' 1.685(14) . ?
N53 C101 1.324(4) . ?
C101 N51 1.312(4) . ?
C101 N52 1.335(4) . ?
O90 C91 1.424(6) . ?
C91 C90 1.525(7) . ?
N58 C103 1.315(4) . ?
N59 C103 1.320(4) . ?
N57 C103 1.331(4) . ?
O7W O7W' 0.810(9) . ?
O3W O3W' 0.913(9) . ?
O5W O4W' 1.355(9) 1_565 ?
O8W' O8W 1.303(10) . ?
O6W O4W' 1.269(10) 1_565 ?
O6W O4W 1.349(10) 1_565 ?
O4W O4W' 1.206(9) . ?
O4W O6W 1.349(10) 1_545 ?
O4W' O6W 1.269(10) 1_545 ?
O4W' O5W 1.355(9) 1_545 ?
V21 O21 1.6057(19) . ?
V21 O23 1.8232(18) . ?
V21 O12 1.8753(19) . ?
V21 O25 1.9849(19) . ?
V21 O24 2.017(2) . ?
V21 N21 2.297(2) . ?
V31 O31 1.6125(19) . ?
V31 O2 1.7589(18) . ?
V31 O33 1.8775(17) . ?
V31 O35 1.9924(18) . ?
V31 O34 2.038(2) . ?
V31 N31 2.288(2) . ?
V11 O11 1.6199(19) . ?
V11 O12 1.7288(19) . ?
V11 O13 1.8654(18) . ?
V11 O15 2.0009(18) . ?
V11 O14 2.088(2) . ?
V11 N11 2.304(2) . ?
V1 O1 1.599(2) . ?
V1 O2 1.8176(18) . ?
V1 O3 1.8269(18) . ?
V1 O5 1.995(2) . ?
V1 O4 2.010(2) . ?
V1 N1 2.322(2) . ?
O23 C71 1.327(3) . ?
O33 C81 1.325(3) . ?
O34 C34 1.276(3) . ?
O3 C51 1.335(3) . ?
O13 C61 1.346(3) . ?
N31 C33 1.477(3) . ?
N31 C32 1.479(3) . ?
N31 C31 1.487(3) . ?
O35 C35 1.275(3) . ?
O24 C24 1.293(3) . ?
N11 C12 1.478(3) . ?
N11 C13 1.482(3) . ?
N11 C11 1.492(3) . ?
O14 C14 1.282(4) . ?
O15 C15 1.291(3) . ?
O25 C25 1.288(3) . ?
C73 C72 1.385(3) . ?
C73 C81 1.405(3) . ?
C72 C71 1.413(4) . ?
C72 C21 1.504(3) . ?
O4 C4 1.302(4) . ?
N21 C23 1.481(3) . ?
N21 C22 1.483(3) . ?
N21 C21 1.490(3) . ?
O5 C5 1.294(4) . ?
N1 C2 1.476(4) . ?
N1 C3 1.484(4) . ?
N1 C1 1.486(3) . ?
C51 C63 1.400(4) . ?
C51 C52 1.405(4) . ?
C61 C53 1.395(4) . ?
C61 C62 1.414(4) . ?
O17 C15 1.220(3) . ?
O17 Na1 2.377(3) 2_645 ?
C31 C82 1.495(3) . ?
O27 C25 1.230(3) . ?
C12 C14 1.500(4) . ?
C11 C62 1.504(3) . ?
C82 C83 1.387(3) . ?
C82 C81 1.421(4) . ?
C32 C34 1.507(4) . ?
C1 C52 1.506(4) . ?
O36 C34 1.234(3) . ?
C71 C83 1.408(3) . ?
C23 C25 1.517(4) . ?
C33 C35 1.520(4) . ?
C52 C53 1.396(3) . ?
O16 C14 1.238(4) . ?
O7 C5 1.224(4) . ?
C3 C5 1.523(4) . ?
C35 O37 1.227(3) . ?
C13 C15 1.522(4) . ?
C62 C63 1.387(3) . ?
C24 O26 1.232(4) . ?
C24 C22 1.499(4) . ?
C2 C4 1.476(6) . ?
O26 Na1 2.338(3) 4_565 ?
O6 C4 1.234(4) . ?
