# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_sof
_database_code_depnum_ccdc_archive 'CCDC 1027881'
_audit_update_record             
;
2014-10-07 deposited with the CCDC.
2015-06-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_structural     '(N Me4)2 Na2[(W4 V2) O19] * 8(H2 O)'
_chemical_formula_sum            'C8 H40 N2 Na2 O27 V2 W4'
_chemical_formula_weight         1479.68

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma
_symmetry_space_group_name_Hall  ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   18.6008(10)
_cell_length_b                   9.9127(5)
_cell_length_c                   18.2252(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3360.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(2)
_cell_measurement_reflns_used    6863
_cell_measurement_theta_min      2.4586
_cell_measurement_theta_max      30.3334

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.138
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2728
_exptl_absorpt_coefficient_mu    14.292
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.0532
_exptl_absorpt_correction_T_max  0.0998
_exptl_absorpt_process_details   'based on intensities (SADABS, Bruker, 2005)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker DUO CCD detector'
_diffrn_measurement_method       'combined omega- and phi-scans'
_diffrn_detector_area_resol_mean 25
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            23362
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         27.49
_reflns_number_total             4082
_reflns_number_gt                3682
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Apex2 V.1.27 (Bruker, 2005)'
_computing_cell_refinement       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction        'Apex2 V.1.27 (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL V6.22 (Bruker, 2000-2005)'
_computing_publication_material  'local programs'

_refine_special_details          'mixed positions W/V'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0133P)²+87.8184P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4082
_refine_ls_number_parameters     259
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1095
_refine_ls_wR_factor_gt          0.1070
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_restrained_S_all      1.188
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
W1 W 0.30662(3) 0.08656(5) 0.96000(3) 0.02661(13) Uani 0.81 1 d P . .
V1 V 0.30662(3) 0.08656(5) 0.96000(3) 0.02661(13) Uani 0.19 1 d P . .
W2 W 0.16726(3) 0.2500 1.02313(3) 0.02824(17) Uani 0.86 2 d SP . .
V2 V 0.16726(3) 0.2500 1.02313(3) 0.02824(17) Uani 0.14 2 d SP . .
W3 W 0.15707(3) 0.08734(6) 0.86864(3) 0.02760(15) Uani 0.57 1 d P . .
V3 V 0.15707(3) 0.08734(6) 0.86864(3) 0.02760(15) Uani 0.43 1 d P . .
W4 W 0.29287(6) 0.2500 0.80797(5) 0.0271(2) Uani 0.38 2 d SP . .
V4 V 0.29287(6) 0.2500 0.80797(5) 0.0271(2) Uani 0.62 2 d SP . .
O1C O 0.2301(5) 0.2500 0.9172(4) 0.0159(17) Uani 1 2 d S . .
O1 O 0.3624(5) -0.0342(9) 0.9937(5) 0.048(2) Uani 1 1 d . . .
O2 O 0.1218(6) 0.2500 1.1047(6) 0.055(4) Uani 1 2 d S . .
O3 O 0.1036(6) -0.0327(10) 0.8351(5) 0.060(3) Uani 1 1 d . . .
O4 O 0.3396(7) 0.2500 0.7314(6) 0.064(5) Uani 1 2 d S . .
O11 O 0.2224(4) 0.1179(7) 0.7902(4) 0.0284(15) Uani 1 1 d . . .
O12 O 0.2313(5) -0.0158(7) 0.9151(4) 0.0357(18) Uani 1 1 d . . .
O13 O 0.1188(4) 0.1174(9) 0.9652(4) 0.042(2) Uani 1 1 d . . .
O14 O 0.3518(5) 0.2500 0.9906(5) 0.0186(18) Uani 1 2 d S . .
O15 O 0.3435(4) 0.1181(8) 0.8645(4) 0.0343(18) Uani 1 1 d . . .
O16 O 0.1097(6) 0.2500 0.8411(6) 0.033(2) Uani 1 2 d S . .
O17 O 0.2401(4) 0.1165(7) 1.0400(4) 0.0280(15) Uani 1 1 d . . .
O1W O 0.2662(7) 0.2500 1.3315(6) 0.037(3) Uani 1 2 d S . .
O2WA O 0.1113(12) 0.111(2) 1.2915(12) 0.039(5) Uani 0.45 1 d P . .
O2WB O 0.1071(10) 0.0735(17) 1.2544(10) 0.041(4) Uani 0.55 1 d P . .
O3W O 0.2796(4) 0.0918(7) 1.1880(4) 0.0342(17) Uani 1 1 d . . .
O4WA O 0.0750(13) -0.2500 0.6295(12) 0.033(5) Uani 0.50 2 d SP . .
O4WB O 0.076(2) -0.180(4) 0.623(2) 0.046(12) Uiso 0.25 1 d P . .
O5W O 0.0070(9) -0.2159(17) 0.7803(9) 0.046(6) Uani 0.50 1 d P . .
O6WA O -0.0766(19) -0.2500 0.597(2) 0.058(12) Uani 0.40 2 d SP . .
O6WB O -0.0707(18) -0.181(4) 0.613(2) 0.044(8) Uiso 0.30 1 d P . .
Na1 Na 0.1905(3) 0.2500 1.2271(3) 0.0300(13) Uani 1 2 d S . .
Na2 Na 0.1345(4) -0.2500 0.7394(4) 0.0436(17) Uani 1 2 d S . .
N1 N 0.0909(6) -0.2500 1.0510(6) 0.023(2) Uani 1 2 d S . .
N2 N 0.0507(6) 0.2500 0.6428(7) 0.026(3) Uani 1 2 d S . .
C11 C 0.1714(8) -0.2500 1.0482(9) 0.042(4) Uani 1 2 d S . .
H11A H 0.1879 -0.3222 1.0156 0.063 Uiso 0.50 1 calc PR . .
H11B H 0.1907 -0.2649 1.0976 0.063 Uiso 0.50 1 calc PR . .
H11C H 0.1884 -0.1629 1.0296 0.063 Uiso 0.50 1 calc PR . .
C12 C 0.0622(11) -0.2500 0.9745(9) 0.054(5) Uani 1 2 d S . .
H12A H 0.0677 -0.1598 0.9532 0.080 Uiso 0.50 1 calc PR . .
H12B H 0.0112 -0.2746 0.9753 0.080 Uiso 0.50 1 calc PR . .
H12C H 0.0889 -0.3155 0.9449 0.080 Uiso 0.50 1 calc PR . .
C13 C 0.0663(7) -0.1280(11) 1.0906(6) 0.038(3) Uani 1 1 d . . .
H13A H 0.0137 -0.1277 1.0930 0.057 Uiso 1 1 calc R . .
H13B H 0.0829 -0.0474 1.0645 0.057 Uiso 1 1 calc R . .
H13C H 0.0862 -0.1282 1.1404 0.057 Uiso 1 1 calc R . .
C21 C 0.0174(10) 0.2500 0.5697(10) 0.055(5) Uani 1 2 d S . .
H21A H -0.0349 0.2423 0.5748 0.082 Uiso 0.50 1 calc PR . .
H21B H 0.0356 0.1734 0.5413 0.082 Uiso 0.50 1 calc PR . .
H21C H 0.0292 0.3343 0.5444 0.082 Uiso 0.50 1 calc PR . .
C22 C 0.1302(9) 0.2500 0.6391(11) 0.048(5) Uani 1 2 d S . .
H22A H 0.1468 0.1655 0.6169 0.072 Uiso 0.50 1 calc PR . .
H22B H 0.1501 0.2582 0.6887 0.072 Uiso 0.50 1 calc PR . .
H22C H 0.1465 0.3263 0.6092 0.072 Uiso 0.50 1 calc PR . .
C23 C 0.0273(9) 0.131(2) 0.6827(11) 0.093(7) Uani 1 1 d . . .
H23A H -0.0253 0.1257 0.6821 0.139 Uiso 1 1 calc R . .
H23B H 0.0442 0.1358 0.7336 0.139 Uiso 1 1 calc R . .
H23C H 0.0472 0.0498 0.6593 0.139 Uiso 1 1 calc R . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
W1 W4 3.2198(10) . ?
W1 O1C 2.293(6) . ?
W1 O1 1.698(8) . ?
W1 O12 1.913(7) . ?
W1 O14 1.908(5) . ?
W1 O15 1.896(7) . ?
W1 O17 1.935(7) . ?
W2 O1C 2.257(8) . ?
W2 O2 1.710(11) . ?
W2 O13 1.912(8) . ?
W2 O13 1.912(8) 7_565 ?
W2 O17 1.919(7) 7_565 ?
W2 O17 1.919(7) . ?
W3 W3 3.2247(13) 7_565 ?
W3 W4 3.1942(11) . ?
W3 O1C 2.287(6) . ?
W3 O3 1.667(8) . ?
W3 O11 1.901(7) . ?
W3 O12 1.916(8) . ?
W3 O13 1.922(8) . ?
W3 O16 1.905(5) . ?
W4 W1 3.2198(10) 7_565 ?
W4 W3 3.1942(11) 7_565 ?
W4 O1C 2.308(8) . ?
W4 O4 1.645(12) . ?
W4 O11 1.881(7) . ?
W4 O11 1.881(7) 7_565 ?
W4 O15 1.913(8) 7_565 ?
W4 O15 1.913(8) . ?
O1C W1 2.293(6) 7_565 ?
O1C V1 2.293(6) 7_565 ?
O1C W3 2.287(6) 7_565 ?
O1C V3 2.287(6) 7_565 ?
O2 Na1 2.571(13) . ?
O3 Na2 2.830(12) . ?
O14 W1 1.908(5) 7_565 ?
O14 V1 1.908(5) 7_565 ?
O16 W3 1.905(5) 7_565 ?
O16 V3 1.905(5) 7_565 ?
O1W Na1 2.367(13) . ?
O1W Na2 2.496(13) 2 ?
O2WA O2WB 0.78(2) . ?
O2WA Na1 2.33(2) . ?
O2WB Na1 2.392(17) . ?
O3W Na1 2.390(9) . ?
O3W Na2 2.427(9) 2 ?
O4WA O4WB 0.71(4) 7 ?
O4WA O4WB 0.71(4) . ?
O4WA Na2 2.29(2) . ?
O4WB O4WB 1.39(8) 7 ?
O4WB Na2 2.49(4) . ?
O5W O5W 0.68(3) 7 ?
O5W Na2 2.507(18) . ?
O6WA O6WB 0.75(3) . ?
O6WA O6WB 0.75(3) 7 ?
O6WB O6WB 1.36(7) 7 ?
Na1 O2WA 2.33(2) 7_565 ?
Na1 O2WB 2.392(17) 7_565 ?
Na1 O3W 2.390(9) 7_565 ?
Na1 Na2 3.263(9) 2 ?
Na2 O3 2.830(12) 7 ?
Na2 O1W 2.496(13) 2_554 ?
Na2 O3W 2.427(9) 2_554 ?
Na2 O3W 2.427(9) 8_655 ?
Na2 O4WB 2.49(4) 7 ?
Na2 O5W 2.507(18) 7 ?
Na2 Na1 3.263(9) 2_554 ?
N1 C11 1.499(18) . ?
N1 C12 1.492(18) . ?
N1 C13 1.480(12) . ?
N1 C13 1.480(12) 7 ?
N2 C21 1.47(2) . ?
N2 C22 1.480(19) . ?
N2 C23 1.456(17) . ?
N2 C23 1.456(17) 7_565 ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

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
O1C W1 W4 45.8(2) . . ?
O1 W1 W4 135.6(3) . . ?
O1 W1 O1C 178.7(4) . . ?
O1 W1 O12 103.2(4) . . ?
O1 W1 O14 102.9(4) . . ?
O1 W1 O15 103.1(4) . . ?
O1 W1 O17 103.1(4) . . ?
O12 W1 W4 80.8(2) . . ?
O12 W1 O1C 77.0(3) . . ?
O12 W1 O17 86.4(3) . . ?
O14 W1 W4 81.9(2) . . ?
O14 W1 O1C 76.9(3) . . ?
O14 W1 O12 153.8(3) . . ?
O14 W1 O17 86.0(3) . . ?
O15 W1 W4 32.5(2) . . ?
O15 W1 O1C 78.2(3) . . ?
O15 W1 O12 87.7(3) . . ?
O15 W1 O14 88.2(4) . . ?
O15 W1 O17 153.8(3) . . ?
O17 W1 W4 121.4(2) . . ?
O17 W1 O1C 75.6(3) . . ?
O2 W2 O1C 178.5(4) . . ?
O2 W2 O13 104.3(4) . . ?
O2 W2 O13 104.3(4) . 7_565 ?
O2 W2 O17 102.1(3) . 7_565 ?
O2 W2 O17 102.1(3) . . ?
O13 W2 O1C 76.8(3) . . ?
O13 W2 O1C 76.8(3) 7_565 . ?
O13 W2 O13 86.9(5) . 7_565 ?
O13 W2 O17 153.6(3) . 7_565 ?
O13 W2 O17 87.0(3) 7_565 7_565 ?
O13 W2 O17 87.0(3) . . ?
O13 W2 O17 153.6(3) 7_565 . ?
O17 W2 O1C 76.8(2) 7_565 . ?
O17 W2 O1C 76.8(2) . . ?
O17 W2 O17 87.2(4) 7_565 . ?
W4 W3 W3 59.683(16) . 7_565 ?
O1C W3 W3 45.16(15) . 7_565 ?
O1C W3 W4 46.2(2) . . ?
O3 W3 W3 135.6(4) . 7_565 ?
O3 W3 W4 134.8(4) . . ?
O3 W3 O1C 178.7(4) . . ?
O3 W3 O11 102.6(4) . . ?
O3 W3 O12 102.2(4) . . ?
O3 W3 O13 103.0(4) . . ?
O3 W3 O16 103.4(4) . . ?
O11 W3 W3 80.8(2) . 7_565 ?
O11 W3 W4 32.2(2) . . ?
O11 W3 O1C 78.4(3) . . ?
O11 W3 O12 87.5(3) . . ?
O11 W3 O13 154.3(3) . . ?
O11 W3 O16 87.8(4) . . ?
O12 W3 W3 122.3(2) . 7_565 ?
O12 W3 W4 81.5(2) . . ?
O12 W3 O1C 77.1(3) . . ?
O12 W3 O13 86.9(4) . . ?
O13 W3 W3 81.1(3) . 7_565 ?
O13 W3 W4 122.1(2) . . ?
O13 W3 O1C 75.9(3) . . ?
O16 W3 W3 32.2(3) . 7_565 ?
O16 W3 W4 81.2(3) . . ?
O16 W3 O1C 77.3(3) . . ?
O16 W3 O12 154.4(3) . . ?
O16 W3 O13 86.5(4) . . ?
W1 W4 W1 60.42(3) 7_565 . ?
W3 W4 W1 91.09(3) . 7_565 ?
W3 W4 W1 60.72(2) 7_565 7_565 ?
W3 W4 W1 60.72(2) . . ?
W3 W4 W1 91.09(3) 7_565 . ?
W3 W4 W3 60.63(3) . 7_565 ?
O1C W4 W1 45.40(15) . 7_565 ?
O1C W4 W1 45.40(15) . . ?
O1C W4 W3 45.69(15) . . ?
O1C W4 W3 45.69(15) . 7_565 ?
O4 W4 W1 133.5(3) . 7_565 ?
O4 W4 W1 133.5(3) . . ?
O4 W4 W3 135.4(3) . . ?
O4 W4 W3 135.4(3) . 7_565 ?
O4 W4 O1C 178.5(5) . . ?
O4 W4 O11 102.8(4) . . ?
O4 W4 O11 102.8(4) . 7_565 ?
O4 W4 O15 101.4(4) . 7_565 ?
O4 W4 O15 101.4(4) . . ?
O11 W4 W1 123.7(2) . 7_565 ?
O11 W4 W1 81.6(2) 7_565 7_565 ?
O11 W4 W1 81.6(2) . . ?
O11 W4 W1 123.7(2) 7_565 . ?
O11 W4 W3 32.6(2) . . ?
O11 W4 W3 82.0(2) 7_565 . ?
O11 W4 W3 82.0(2) . 7_565 ?
O11 W4 W3 32.6(2) 7_565 7_565 ?
O11 W4 O1C 78.3(3) . . ?
O11 W4 O1C 78.3(3) 7_565 . ?
O11 W4 O11 88.3(4) . 7_565 ?
O11 W4 O15 155.8(3) . 7_565 ?
O11 W4 O15 87.7(3) 7_565 7_565 ?
O11 W4 O15 87.7(3) . . ?
O11 W4 O15 155.8(3) 7_565 . ?
O15 W4 W1 32.1(2) 7_565 7_565 ?
O15 W4 W1 80.9(2) . 7_565 ?
O15 W4 W1 80.9(2) 7_565 . ?
O15 W4 W1 32.1(2) . . ?
O15 W4 W3 123.2(2) 7_565 . ?
O15 W4 W3 81.8(2) . . ?
O15 W4 W3 81.8(2) 7_565 7_565 ?
O15 W4 W3 123.2(2) . 7_565 ?
O15 W4 O1C 77.5(3) 7_565 . ?
O15 W4 O1C 77.5(3) . . ?
O15 W4 O15 86.2(5) 7_565 . ?
W1 O1C W1 89.9(3) 7_565 . ?
W1 O1C W4 88.8(3) 7_565 . ?
W1 O1C W4 88.8(3) . . ?
V1 O1C W1 0.00(3) 7_565 7_565 ?
V1 O1C W1 89.9(3) 7_565 . ?
V1 O1C W4 88.8(3) 7_565 . ?
W2 O1C W1 91.7(2) . 7_565 ?
W2 O1C W1 91.7(2) . . ?
W2 O1C V1 91.7(2) . 7_565 ?
W2 O1C W3 91.3(3) . . ?
W2 O1C W3 91.3(3) . 7_565 ?
W2 O1C V3 91.3(3) . 7_565 ?
W2 O1C W4 179.2(4) . . ?
W3 O1C W1 176.9(4) . 7_565 ?
W3 O1C W1 90.13(2) 7_565 7_565 ?
W3 O1C W1 90.13(2) . . ?
W3 O1C W1 176.9(4) 7_565 . ?
W3 O1C V1 176.9(4) . 7_565 ?
W3 O1C V1 90.13(2) 7_565 7_565 ?
W3 O1C W3 89.7(3) . 7_565 ?
W3 O1C V3 89.7(3) . 7_565 ?
W3 O1C W4 88.1(2) . . ?
W3 O1C W4 88.1(2) 7_565 . ?
V3 O1C W1 90.13(2) 7_565 7_565 ?
V3 O1C W1 176.9(4) 7_565 . ?
V3 O1C V1 90.13(2) 7_565 7_565 ?
V3 O1C W3 0.00(3) 7_565 7_565 ?
V3 O1C W4 88.1(2) 7_565 . ?
W2 O2 Na1 120.5(6) . . ?
W3 O3 Na2 130.4(6) . . ?
W4 O11 W3 115.2(3) . . ?
W1 O12 W3 115.7(4) . . ?
W2 O13 W3 115.9(4) . . ?
W1 O14 W1 116.2(4) . 7_565 ?
W1 O14 V1 116.2(4) . 7_565 ?
V1 O14 W1 0.00(4) 7_565 7_565 ?
W1 O15 W4 115.4(3) . . ?
W3 O16 W3 115.7(5) 7_565 . ?
V3 O16 W3 0.00(4) 7_565 7_565 ?
V3 O16 W3 115.7(5) 7_565 . ?
W2 O17 W1 115.9(3) . . ?
Na1 O1W Na2 84.3(4) . 2 ?
O2WB O2WA Na1 85(2) . . ?
O2WA O2WB Na1 76(2) . . ?
Na1 O3W Na2 85.3(3) . 2 ?
O4WB O4WA O4WB 159(8) 7 . ?
O4WB O4WA Na2 98(4) 7 . ?
O4WB O4WA Na2 98(4) . . ?
O4WA O4WB O4WB 11(4) . 7 ?
O4WA O4WB Na2 65(4) . . ?
O4WB O4WB Na2 73.8(9) 7 . ?
O5W O5W Na2 82.2(4) 7 . ?
O6WB O6WA O6WB 131(10) . 7 ?
O6WA O6WB O6WB 24(5) . 7 ?
O2 Na1 Na2 123.8(3) . 2 ?
O1W Na1 O2 173.3(5) . . ?
O1W Na1 O2WB 102.6(5) . . ?
O1W Na1 O2WB 102.6(5) . 7_565 ?
O1W Na1 O3W 80.0(3) . 7_565 ?
O1W Na1 O3W 80.0(3) . . ?
O1W Na1 Na2 49.5(3) . 2 ?
O2WA Na1 O2 97.0(6) 7_565 . ?
O2WA Na1 O2 97.0(6) . . ?
O2WA Na1 O1W 88.3(6) 7_565 . ?
O2WA Na1 O1W 88.3(6) . . ?
O2WA Na1 O2WA 72.3(11) 7_565 . ?
O2WA Na1 O2WB 85.2(7) 7_565 . ?
O2WA Na1 O2WB 18.9(5) . . ?
O2WA Na1 O2WB 18.9(5) 7_565 7_565 ?
O2WA Na1 O2WB 85.2(7) . 7_565 ?
O2WA Na1 O3W 101.6(6) 7_565 7_565 ?
O2WA Na1 O3W 167.1(6) . 7_565 ?
O2WA Na1 O3W 167.1(6) 7_565 . ?
O2WA Na1 O3W 101.6(6) . . ?
O2WA Na1 Na2 126.5(6) 7_565 2 ?
O2WA Na1 Na2 126.5(6) . 2 ?
O2WB Na1 O2 81.8(5) . . ?
O2WB Na1 O2 81.8(5) 7_565 . ?
O2WB Na1 O2WB 94.0(9) . 7_565 ?
O2WB Na1 Na2 129.3(5) . 2 ?
O2WB Na1 Na2 129.3(5) 7_565 2 ?
O3W Na1 O2 95.0(3) 7_565 . ?
O3W Na1 O2 95.0(3) . . ?
O3W Na1 O2WB 172.8(5) 7_565 . ?
O3W Na1 O2WB 91.8(5) . . ?
O3W Na1 O2WB 91.8(5) 7_565 7_565 ?
O3W Na1 O2WB 172.8(5) . 7_565 ?
O3W Na1 O3W 82.0(4) 7_565 . ?
O3W Na1 Na2 47.8(2) 7_565 2 ?
O3W Na1 Na2 47.8(2) . 2 ?
O3 Na2 O3 99.1(4) . 7 ?
O3 Na2 Na1 104.2(3) . 2_554 ?
O3 Na2 Na1 104.2(3) 7 2_554 ?
O1W Na2 O3 74.7(3) 2_554 . ?
O1W Na2 O3 74.7(3) 2_554 7 ?
O1W Na2 O5W 120.0(5) 2_554 7 ?
O1W Na2 O5W 120.0(5) 2_554 . ?
O1W Na2 Na1 46.2(3) 2_554 2_554 ?
O3W Na2 O3 83.1(3) 2_554 . ?
O3W Na2 O3 149.7(4) 8_655 . ?
O3W Na2 O3 149.7(4) 2_554 7 ?
O3W Na2 O3 83.1(3) 8_655 7 ?
O3W Na2 O1W 76.8(3) 2_554 2_554 ?
O3W Na2 O1W 76.8(3) 8_655 2_554 ?
O3W Na2 O3W 80.5(4) 2_554 8_655 ?
O3W Na2 O4WB 97.9(9) 2_554 7 ?
O3W Na2 O4WB 77.2(9) 8_655 7 ?
O3W Na2 O4WB 77.2(9) 2_554 . ?
O3W Na2 O4WB 97.9(9) 8_655 . ?
O3W Na2 O5W 145.5(4) 2_554 7 ?
O3W Na2 O5W 130.5(4) 8_655 7 ?
O3W Na2 O5W 130.5(4) 2_554 . ?
O3W Na2 O5W 145.5(4) 8_655 . ?
O3W Na2 Na1 46.9(2) 2_554 2_554 ?
O3W Na2 Na1 46.9(2) 8_655 2_554 ?
O4WA Na2 O3 116.2(4) . . ?
O4WA Na2 O3 116.2(4) . 7 ?
O4WA Na2 O1W 161.1(7) . 2_554 ?
O4WA Na2 O3W 88.9(5) . 2_554 ?
O4WA Na2 O3W 88.9(5) . 8_655 ?
O4WA Na2 O4WB 16.3(9) . 7 ?
O4WA Na2 O4WB 16.3(9) . . ?
O4WA Na2 O5W 78.7(7) . 7 ?
O4WA Na2 O5W 78.7(7) . . ?
O4WA Na2 Na1 114.9(6) . 2_554 ?
O4WB Na2 O3 130.5(9) 7 . ?
O4WB Na2 O3 103.1(9) . . ?
O4WB Na2 O3 103.1(9) 7 7 ?
O4WB Na2 O3 130.5(9) . 7 ?
O4WB Na2 O1W 154.0(9) 7 2_554 ?
O4WB Na2 O1W 154.0(9) . 2_554 ?
O4WB Na2 O4WB 32.3(18) 7 . ?
O4WB Na2 O5W 78.6(10) 7 7 ?
O4WB Na2 O5W 83.0(10) . 7 ?
O4WB Na2 O5W 83.0(10) 7 . ?
O4WB Na2 O5W 78.6(10) . . ?
O4WB Na2 Na1 112.2(9) 7 2_554 ?
O4WB Na2 Na1 112.2(9) . 2_554 ?
O5W Na2 O3 74.2(5) 7 . ?
O5W Na2 O3 61.5(4) . . ?
O5W Na2 O3 61.5(4) 7 7 ?
O5W Na2 O3 74.2(5) . 7 ?
O5W Na2 O5W 15.5(8) 7 . ?
O5W Na2 Na1 164.5(4) 7 2_554 ?
O5W Na2 Na1 164.5(4) . 2_554 ?
C12 N1 C11 109.0(13) . . ?
C13 N1 C11 109.0(8) . . ?
C13 N1 C11 109.0(8) 7 . ?
C13 N1 C12 110.2(8) . . ?
C13 N1 C12 110.2(8) 7 . ?
C13 N1 C13 109.6(12) . 7 ?
C21 N2 C22 112.3(13) . . ?
C23 N2 C21 109.0(10) . . ?
C23 N2 C21 109.0(10) 7_565 . ?
C23 N2 C22 108.8(10) . . ?
C23 N2 C22 108.8(10) 7_565 . ?
C23 N2 C23 109(2) . 7_565 ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N2 C23 H23A 109.5 . . ?
N2 C23 H23B 109.5 . . ?
N2 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.870
_refine_diff_density_min         -2.557
_refine_diff_density_rms         0.245
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_14
_database_code_depnum_ccdc_archive 'CCDC 1028644'
_audit_update_record             
;
2014-10-10 deposited with the CCDC.
2015-06-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_structural     
'(N Me4)4.83 [(Se W4.57 V4.43 O33)2 (W O (H2O)) (V O)2.6] * 10.57(H2 O)'
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19.32 H81.10 N4.83 O81.17 Se2 V11.46 W10.14'
_chemical_formula_weight         4286.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_IT_number  34
_symmetry_space_group_name_H-M   'P n n 2'
_symmetry_space_group_name_Hall  'P 2 -2n'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   19.4257(11)
_cell_length_b                   21.2136(11)
_cell_length_c                   12.9194(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5323.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8210
_cell_measurement_theta_min      4.00
_cell_measurement_theta_max      67.10

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.674
_exptl_crystal_F_000             3924
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    29.320
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.1438
_exptl_absorpt_correction_T_max  0.3197
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_measurement_device_type  'Bruker DUO CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 25
_diffrn_reflns_number            39238
_diffrn_reflns_av_unetI/netI     0.0587
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.083
_diffrn_reflns_theta_max         67.831
_diffrn_reflns_theta_full        67.500
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             8396
_reflns_number_gt                6877
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_max     0.981
_reflns_Friedel_fraction_full    0.986

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Apex2 V.1.27 (Bruker, 2005)'
_computing_cell_refinement       'Apex2 V.1.27 (Bruker, 2005)'
_computing_data_reduction        'Apex2 V.1.27 (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0792P)²+29.2398P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8396
_refine_ls_number_parameters     642
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1464
_refine_ls_wR_factor_gt          0.1306
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
W1 W 0.81023(10) 0.78943(8) 0.88257(12) 0.0492(4) Uani 0.55 1 d . . P . .
V1 V 0.81023(10) 0.78943(8) 0.88257(12) 0.0492(4) Uani 0.45 1 d . . P . .
W2 W 0.73563(8) 0.84165(8) 0.63612(13) 0.0481(4) Uani 0.6 1 d . . P . .
V2 V 0.73563(8) 0.84165(8) 0.63612(13) 0.0481(4) Uani 0.4 1 d . . P . .
W3 W 0.88151(8) 0.73229(6) 0.63750(11) 0.0459(4) Uani 0.66 1 d . . P . .
V3 V 0.88151(8) 0.73229(6) 0.63750(11) 0.0459(4) Uani 0.34 1 d . . P . .
W4 W 0.97101(8) 0.83032(7) 0.48069(11) 0.0454(3) Uani 0.7 1 d . . P . .
V4 V 0.97101(8) 0.83032(7) 0.48069(11) 0.0454(3) Uani 0.3 1 d . . P . .
W5 W 0.82414(7) 0.93904(7) 0.47837(11) 0.0456(3) Uani 0.73 1 d . . P . .
V5 V 0.82414(7) 0.93904(7) 0.47837(11) 0.0456(3) Uani 0.27 1 d . . P . .
W6 W 0.75836(10) 0.99161(10) 0.70680(17) 0.0462(5) Uani 0.35 1 d . . P . .
V6 V 0.75836(10) 0.99161(10) 0.70680(17) 0.0462(5) Uani 0.65 1 d . . P . .
W7 W 0.83129(12) 0.93946(11) 0.95076(15) 0.0465(5) Uani 0.33 1 d . . P A .
V7 V 0.83129(12) 0.93946(11) 0.95076(15) 0.0465(5) Uani 0.67 1 d . . P A .
W8 W 0.96655(13) 0.83838(11) 0.95309(16) 0.0465(6) Uani 0.3 1 d . . P A .
V8 V 0.96655(13) 0.83838(11) 0.95309(16) 0.0465(6) Uani 0.7 1 d . . P A .
W9 W 1.03862(11) 0.78291(9) 0.71143(19) 0.0472(5) Uani 0.35 1 d . . P . .
V9 V 1.03862(11) 0.78291(9) 0.71143(19) 0.0472(5) Uani 0.65 1 d . . P . .
W10 W 1.0000 1.0000 0.52212(15) 0.0622(5) Uani 1 2 d S T P . .
O1L O 1.0000 1.0000 0.3458(16) 0.054(7) Uani 1 2 d S T P . .
O2L O 1.0000 1.0000 0.652(2) 0.076(9) Uani 1 2 d S T P . .
Se1 Se 0.90986(12) 0.90044(10) 0.7154(2) 0.0426(5) Uani 1 1 d . . . . .
O1S O 0.8825(9) 0.8703(8) 0.8298(12) 0.049(4) Uani 1 1 d . . . . .
O2S O 0.9350(9) 0.8326(7) 0.6577(12) 0.051(4) Uani 1 1 d . . . . .
O3S O 0.8322(9) 0.9105(8) 0.6562(11) 0.048(4) Uani 1 1 d . . . . .
V11 V 1.0000 1.0000 0.9392(8) 0.039(2) Uani 0.6 2 d S T P A 1
O11V O 1.0000 1.0000 1.057(3) 0.054(10) Uiso 0.6 2 d S . P A 1
O1WV O 0.9704(15) 1.0208(14) 0.993(2) 0.015(6) Uiso 0.35 1 d . . P B 2
V12 V 1.1033(3) 0.9218(2) 0.8158(4) 0.0532(11) Uani 1 1 d . . . . .
O12V O 1.1576(12) 0.8809(10) 0.8769(15) 0.067(5) Uani 1 1 d . . . . .
O1 O 0.7601(13) 0.7350(10) 0.9388(16) 0.077(6) Uani 1 1 d . . . . .
O2 O 0.6611(11) 0.8048(11) 0.6109(17) 0.079(6) Uani 1 1 d . . . . .
O3 O 0.8578(10) 0.6577(9) 0.6131(15) 0.066(5) Uani 1 1 d . . . . .
O4 O 0.8024(14) 0.9820(11) 1.0465(17) 0.089(7) Uani 1 1 d . . . . .
O5 O 1.0136(13) 0.8191(12) 1.0529(15) 0.084(7) Uani 1 1 d . . . . .
O6 O 1.1069(13) 0.7393(10) 0.732(2) 0.087(7) Uani 1 1 d . . . . .
O7 O 0.9975(11) 0.8161(9) 0.3593(15) 0.063(5) Uani 1 1 d . . . . .
O8 O 0.8035(10) 0.9591(10) 0.3571(15) 0.065(5) Uani 1 1 d . . . . .
O9 O 0.7001(10) 1.0454(10) 0.7265(19) 0.077(6) Uani 1 1 d . . . . .
O11 O 1.0059(10) 0.7950(9) 0.8467(13) 0.057(4) Uani 1 1 d . . . . .
O12 O 0.8910(10) 0.7827(9) 0.9667(13) 0.062(5) Uani 1 1 d . . . . .
O13 O 0.7733(10) 0.9982(9) 0.5589(14) 0.060(5) Uani 1 1 d . . . . .
O14 O 0.7018(11) 0.9214(9) 0.6818(13) 0.067(5) Uani 1 1 d . . . . .
O15 O 0.7844(12) 0.8630(9) 0.9645(14) 0.072(6) Uani 1 1 d . . . . .
O16 O 0.7767(9) 0.9649(9) 0.8390(14) 0.059(5) Uani 1 1 d . . . . .
O17 O 0.7553(10) 0.8782(8) 0.5082(12) 0.057(5) Uani 1 1 d . . . . .
O18 O 0.9096(11) 0.9024(9) 1.0191(14) 0.062(5) Uani 1 1 d . . . . .
O19 O 0.9204(10) 0.7541(8) 0.5091(12) 0.055(4) Uani 1 1 d . . . . .
O20 O 0.8549(12) 0.7422(9) 0.7797(13) 0.066(6) Uani 1 1 d . . . . .
O23 O 0.8866(9) 0.8734(8) 0.4577(14) 0.054(4) Uani 1 1 d . . . . .
O24 O 0.8021(9) 0.7786(8) 0.5994(13) 0.053(4) Uani 1 1 d . . . . .
O25 O 1.0449(10) 0.7960(8) 0.5631(14) 0.057(5) Uani 1 1 d . . . . .
O26 O 0.7497(10) 0.8208(10) 0.7761(14) 0.063(5) Uani 1 1 d . . . . .
O27 O 0.9732(10) 0.7188(8) 0.6850(16) 0.067(5) Uani 1 1 d . . . . .
O111 O 0.8453(9) 1.0361(9) 0.7198(16) 0.062(4) Uani 1 1 d . . . . .
O112 O 1.0082(9) 0.9115(7) 0.5048(17) 0.060(5) Uani 1 1 d . . . . .
O113 O 0.9040(8) 0.9888(8) 0.5035(13) 0.053(4) Uani 1 1 d . . . . .
O114 O 0.9039(10) 0.9971(9) 0.8914(14) 0.059(5) Uani 1 1 d . . . . .
O115 O 1.0166(11) 0.9146(8) 0.8969(13) 0.059(5) Uani 1 1 d . . . . .
O116 O 1.0680(8) 0.8676(7) 0.7256(13) 0.050(4) Uani 1 1 d . . . . .
N1 N 0.8335(11) 1.1269(10) 0.2165(19) 0.060(5) Uani 1 1 d . . . . .
C11 C 0.890(2) 1.0805(14) 0.227(4) 0.101(12) Uani 1 1 d . . . . .
H11A H 0.8894 1.0626 0.2974 0.152 Uiso 1 1 calc R U . . .
H11B H 0.9343 1.1015 0.2155 0.152 Uiso 1 1 calc R U . . .
H11C H 0.8840 1.0466 0.1766 0.152 Uiso 1 1 calc R U . . .
C12 C 0.8217(17) 1.1400(19) 0.101(3) 0.084(10) Uani 1 1 d . . . . .
H12A H 0.8573 1.1688 0.0755 0.126 Uiso 1 1 calc R U . . .
H12B H 0.7763 1.1592 0.0913 0.126 Uiso 1 1 calc R U . . .
H12C H 0.8239 1.1003 0.0623 0.126 Uiso 1 1 calc R U . . .
C13 C 0.8532(17) 1.1867(15) 0.262(3) 0.080(10) Uani 1 1 d . . . . .
H13A H 0.8676 1.1800 0.3342 0.120 Uiso 1 1 calc R U . . .
H13B H 0.8139 1.2157 0.2608 0.120 Uiso 1 1 calc R U . . .
H13C H 0.8915 1.2050 0.2230 0.120 Uiso 1 1 calc R U . . .
C14 C 0.7691(18) 1.1014(16) 0.263(3) 0.091(11) Uani 1 1 d . . . . .
H14A H 0.7790 1.0858 0.3332 0.136 Uiso 1 1 calc R U . . .
H14B H 0.7516 1.0668 0.2206 0.136 Uiso 1 1 calc R U . . .
H14C H 0.7345 1.1350 0.2671 0.136 Uiso 1 1 calc R U . . .
N2 N 0.800(2) 0.7426(19) 1.250(2) 0.079(12) Uani 0.715 1 d . . P C 1
C21 C 0.782(3) 0.737(4) 1.358(3) 0.14(3) Uani 0.715 1 d . . P C 1
H21A H 0.8100 0.7669 1.3982 0.214 Uiso 0.715 1 calc R U P C 1
H21B H 0.7917 0.6940 1.3813 0.214 Uiso 0.715 1 calc R U P C 1
H21C H 0.7334 0.7465 1.3668 0.214 Uiso 0.715 1 calc R U P C 1
C22 C 0.783(3) 0.808(3) 1.214(5) 0.101(15) Uiso 0.715 1 d . . P C 1
H22A H 0.7870 0.8375 1.2721 0.152 Uiso 0.715 1 calc R U P C 1
H22B H 0.7359 0.8089 1.1871 0.152 Uiso 0.715 1 calc R U P C 1
H22C H 0.8152 0.8204 1.1591 0.152 Uiso 0.715 1 calc R U P C 1
C23 C 0.761(2) 0.6994(17) 1.184(3) 0.060(10) Uani 0.715 1 d . . P C 1
H23A H 0.7637 0.6565 1.2116 0.090 Uiso 0.715 1 calc R U P C 1
H23B H 0.7794 0.7004 1.1136 0.090 Uiso 0.715 1 calc R U P C 1
H23C H 0.7123 0.7127 1.1825 0.090 Uiso 0.715 1 calc R U P C 1
C24 C 0.871(2) 0.736(3) 1.226(4) 0.11(2) Uani 0.715 1 d . . P C 1
H24A H 0.8860 0.6931 1.2423 0.169 Uiso 0.715 1 calc R U P C 1
H24B H 0.8977 0.7662 1.2671 0.169 Uiso 0.715 1 calc R U P C 1
H24C H 0.8780 0.7444 1.1523 0.169 Uiso 0.715 1 calc R U P C 1
O9W O 0.801(4) 0.788(4) 1.380(7) 0.08(2) Uiso 0.285 1 d . . P D 2
N3 N 0.5751(17) 0.8760(17) 0.939(3) 0.065(9) Uani 0.7 1 d . . P . .
C31 C 0.563(3) 0.833(3) 0.857(5) 0.106(18) Uiso 0.7 1 d . . P . .
H31A H 0.6060 0.8101 0.8418 0.159 Uiso 0.7 1 calc R U P . .
H31B H 0.5490 0.8565 0.7948 0.159 Uiso 0.7 1 calc R U P . .
H31C H 0.5273 0.8034 0.8765 0.159 Uiso 0.7 1 calc R U P . .
C32 C 0.609(2) 0.9331(16) 0.901(4) 0.069(12) Uani 0.7 1 d . . P . .
H32A H 0.6521 0.9219 0.8670 0.104 Uiso 0.7 1 calc R U P . .
H32B H 0.6180 0.9613 0.9594 0.104 Uiso 0.7 1 calc R U P . .
H32C H 0.5785 0.9545 0.8513 0.104 Uiso 0.7 1 calc R U P . .
C33 C 0.505(3) 0.892(3) 0.968(4) 0.087(14) Uiso 0.7 1 d . . P . .
H33A H 0.5053 0.9229 1.0245 0.131 Uiso 0.7 1 calc R U P . .
H33B H 0.4808 0.8536 0.9919 0.131 Uiso 0.7 1 calc R U P . .
H33C H 0.4801 0.9095 0.9086 0.131 Uiso 0.7 1 calc R U P . .
C34 C 0.613(4) 0.857(3) 1.024(6) 0.13(2) Uiso 0.7 1 d . . P . .
H34A H 0.6604 0.8489 1.0041 0.188 Uiso 0.7 1 calc R U P . .
H34B H 0.5925 0.8180 1.0526 0.188 Uiso 0.7 1 calc R U P . .
H34C H 0.6113 0.8899 1.0774 0.188 Uiso 0.7 1 calc R U P . .
O1W O 1.0711(13) 1.0826(11) 1.2341(15) 0.082(6) Uani 1 1 d . . . . .
O21W O 0.8410(12) 1.1175(12) 0.5227(16) 0.054(6) Uani 0.75 1 d . . P . .
O22W O 0.891(3) 1.076(3) 0.595(4) 0.037(13) Uiso 0.25 1 d . . P . .
O31W O 0.813(3) 0.597(2) 0.985(4) 0.056(12) Uiso 0.35 1 d . . P . .
O32W O 0.830(8) 0.564(7) 0.950(12) 0.04(3) Uiso 0.1 1 d . . P . .
O41W O 0.647(7) 1.030(6) 1.073(10) 0.06(3) Uiso 0.15 1 d . . P . .
O42W O 0.649(6) 1.054(6) 0.999(10) 0.09(3) Uiso 0.2 1 d . . P . .
O43W O 0.594(5) 1.033(5) 1.142(9) 0.07(3) Uiso 0.2 1 d . . P . .
O5W O 0.547(4) 1.061(4) 0.724(7) 0.07(2) Uiso 0.25 1 d . . P . .
O6W O 1.147(4) 0.616(3) 0.856(5) 0.054(17) Uiso 0.25 1 d . . P . .
O71W O 0.989(9) 0.599(8) 0.822(14) 0.11(5) Uiso 0.2 1 d . . P . .
O72W O 1.007(6) 0.607(5) 0.778(8) 0.12(4) Uiso 0.35 1 d . . P . .
O8W O 0.689(4) 0.954(4) 1.183(7) 0.06(2) Uiso 0.2 1 d . . P . .
O10W O 0.581(6) 0.960(6) 0.602(9) 0.08(3) Uiso 0.2 1 d . . P . .
O11W O 0.938(5) 0.652(5) 0.961(8) 0.07(3) Uiso 0.2 1 d . . P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
W1 O1 1.676(18) . ?
W1 O20 1.878(19) . ?
W1 O12 1.913(18) . ?
W1 O26 1.928(19) . ?
W1 O15 1.95(2) . ?
W1 O1S 2.320(16) . ?
W2 O2 1.68(2) . ?
W2 O17 1.865(16) . ?
W2 O26 1.882(18) . ?
W2 O14 1.91(2) . ?
W2 O24 1.919(18) . ?
W2 O3S 2.392(16) . ?
W3 O3 1.68(2) . ?
W3 O19 1.881(17) . ?
W3 O24 1.894(19) . ?
W3 O27 1.906(19) . ?
W3 O20 1.920(17) . ?
W3 O2S 2.382(16) . ?
W4 O7 1.678(19) . ?
W4 O112 1.893(15) . ?
W4 O23 1.901(18) . ?
W4 O19 1.927(17) . ?
W4 O25 1.929(19) . ?
W4 O2S 2.392(16) . ?
W5 O8 1.672(19) . ?
W5 O23 1.866(18) . ?
W5 O17 1.898(17) . ?
W5 O113 1.904(16) . ?
W5 O13 1.905(18) . ?
W5 O3S 2.381(15) . ?
W6 O9 1.63(2) . ?
W6 O16 1.834(19) . ?
W6 O14 1.878(19) . ?
W6 O13 1.938(18) . ?
W6 O111 1.943(17) . ?
W6 O3S 2.333(17) . ?
W7 O4 1.63(2) . ?
W7 O15 1.868(17) . ?
W7 O16 1.87(2) . ?
W7 O18 1.93(2) . ?
W7 O114 2.018(18) . ?
W7 O1S 2.364(17) . ?
W8 O5 1.632(19) . ?
W8 O11 1.82(2) . ?
W8 O12 1.893(17) . ?
W8 O18 1.95(2) . ?
W8 O115 2.021(17) . ?
W8 O1S 2.379(17) . ?
W9 O6 1.64(2) . ?
W9 O11 1.877(18) . ?
W9 O27 1.892(18) . ?
W9 O116 1.894(15) . ?
W9 O25 1.940(18) . ?
W9 O2S 2.377(18) . ?
W10 O2L 1.68(3) . ?
W10 O113 1.896(16) . ?
W10 O113 1.896(16) 2_775 ?
W10 O112 1.898(15) . ?
W10 O112 1.898(16) 2_775 ?
W10 O1L 2.28(2) . ?
Se1 O2S 1.693(16) . ?
Se1 O1S 1.695(16) . ?
Se1 O3S 1.705(17) . ?
V11 O11V 1.52(4) . ?
V11 O115 1.920(18) 2_775 ?
V11 O115 1.920(18) . ?
V11 O114 1.97(2) 2_775 ?
V11 O114 1.97(2) . ?
V11 V12 3.053(7) 2_775 ?
V11 V12 3.053(7) . ?
O1WV O1WV 1.45(6) 2_775 ?
V12 O12V 1.58(2) . ?
V12 O116 1.774(17) . ?
V12 O111 1.825(19) 2_775 ?
V12 O114 1.984(19) 2_775 ?
V12 O115 1.989(19) . ?
O111 V12 1.825(19) 2_775 ?
O114 V12 1.984(19) 2_775 ?
N1 C13 1.45(4) . ?
N1 C11 1.48(4) . ?
N1 C14 1.49(4) . ?
N1 C12 1.54(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N2 C24 1.42(6) . ?
N2 C21 1.43(5) . ?
N2 C23 1.47(4) . ?
N2 C22 1.50(7) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N3 C34 1.39(7) . ?
N3 C31 1.41(7) . ?
N3 C32 1.46(5) . ?
N3 C33 1.46(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O21W O22W 1.60(6) . ?
O31W O32W 0.89(15) . ?
O41W O42W 1.09(15) . ?
O41W O43W 1.36(16) . ?
O71W O72W 0.68(18) . ?

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 W1 O20 102.0(10) . . ?
O1 W1 O12 100.3(10) . . ?
O20 W1 O12 89.0(9) . . ?
O1 W1 O26 101.1(10) . . ?
O20 W1 O26 87.8(9) . . ?
O12 W1 O26 158.6(7) . . ?
O1 W1 O15 99.6(9) . . ?
O20 W1 O15 158.4(7) . . ?
O12 W1 O15 87.8(9) . . ?
O26 W1 O15 87.4(9) . . ?
O1 W1 O1S 171.4(8) . . ?
O20 W1 O1S 84.7(7) . . ?
O12 W1 O1S 74.1(7) . . ?
O26 W1 O1S 84.5(7) . . ?
O15 W1 O1S 73.9(7) . . ?
O2 W2 O17 101.4(9) . . ?
O2 W2 O26 101.7(9) . . ?
O17 W2 O26 156.9(8) . . ?
O2 W2 O14 100.2(10) . . ?
O17 W2 O14 88.6(8) . . ?
O26 W2 O14 87.8(9) . . ?
O2 W2 O24 102.0(9) . . ?
O17 W2 O24 86.1(8) . . ?
O26 W2 O24 88.6(8) . . ?
O14 W2 O24 157.8(8) . . ?
O2 W2 O3S 169.3(9) . . ?
O17 W2 O3S 71.5(6) . . ?
O26 W2 O3S 85.7(7) . . ?
O14 W2 O3S 72.2(7) . . ?
O24 W2 O3S 85.7(6) . . ?
O3 W3 O19 100.2(8) . . ?
O3 W3 O24 102.5(8) . . ?
O19 W3 O24 88.3(8) . . ?
O3 W3 O27 100.1(9) . . ?
O19 W3 O27 86.9(9) . . ?
O24 W3 O27 157.3(7) . . ?
O3 W3 O20 102.0(8) . . ?
O19 W3 O20 157.7(7) . . ?
O24 W3 O20 88.5(9) . . ?
O27 W3 O20 87.7(9) . . ?
O3 W3 O2S 169.3(8) . . ?
O19 W3 O2S 72.6(6) . . ?
O24 W3 O2S 85.4(6) . . ?
O27 W3 O2S 72.0(7) . . ?
O20 W3 O2S 85.1(7) . . ?
O7 W4 O112 101.5(10) . . ?
O7 W4 O23 101.8(9) . . ?
O112 W4 O23 85.3(8) . . ?
O7 W4 O19 100.6(9) . . ?
O112 W4 O19 157.9(8) . . ?
O23 W4 O19 89.6(8) . . ?
O7 W4 O25 102.7(9) . . ?
O112 W4 O25 88.2(8) . . ?
O23 W4 O25 155.4(8) . . ?
O19 W4 O25 87.6(8) . . ?
O7 W4 O2S 170.8(7) . . ?
O112 W4 O2S 86.3(7) . . ?
O23 W4 O2S 83.5(7) . . ?
O19 W4 O2S 71.7(6) . . ?
O25 W4 O2S 72.4(7) . . ?
O8 W5 O23 102.2(9) . . ?
O8 W5 O17 101.2(8) . . ?
O23 W5 O17 88.8(8) . . ?
O8 W5 O113 102.4(8) . . ?
O23 W5 O113 84.8(7) . . ?
O17 W5 O113 156.4(8) . . ?
O8 W5 O13 102.7(10) . . ?
O23 W5 O13 155.0(8) . . ?
O17 W5 O13 88.4(8) . . ?
O113 W5 O13 87.9(8) . . ?
O8 W5 O3S 169.9(8) . . ?
O23 W5 O3S 84.6(7) . . ?
O17 W5 O3S 71.2(6) . . ?
O113 W5 O3S 85.6(7) . . ?
O13 W5 O3S 71.0(7) . . ?
O9 W6 O16 101.9(10) . . ?
O9 W6 O14 100.1(10) . . ?
O16 W6 O14 91.6(8) . . ?
O9 W6 O13 102.0(10) . . ?
O16 W6 O13 155.7(8) . . ?
O14 W6 O13 88.6(8) . . ?
O9 W6 O111 104.5(9) . . ?
O16 W6 O111 84.3(8) . . ?
O14 W6 O111 155.4(9) . . ?
O13 W6 O111 85.4(8) . . ?
O9 W6 O3S 171.3(9) . . ?
O16 W6 O3S 85.0(7) . . ?
O14 W6 O3S 74.2(8) . . ?
O13 W6 O3S 71.6(7) . . ?
O111 W6 O3S 81.3(7) . . ?
O4 W7 O15 103.9(11) . . ?
O4 W7 O16 103.4(11) . . ?
O15 W7 O16 92.7(9) . . ?
O4 W7 O18 98.6(11) . . ?
O15 W7 O18 89.2(9) . . ?
O16 W7 O18 156.7(8) . . ?
O4 W7 O114 101.1(10) . . ?
O15 W7 O114 154.5(8) . . ?
O16 W7 O114 85.9(8) . . ?
O18 W7 O114 82.5(8) . . ?
O4 W7 O1S 171.9(10) . . ?
O15 W7 O1S 74.3(8) . . ?
O16 W7 O1S 84.7(7) . . ?
O18 W7 O1S 73.6(7) . . ?
O114 W7 O1S 80.2(6) . . ?
O5 W8 O11 103.5(10) . . ?
O5 W8 O12 101.8(11) . . ?
O11 W8 O12 94.6(8) . . ?
O5 W8 O18 98.4(11) . . ?
O11 W8 O18 157.0(8) . . ?
O12 W8 O18 87.3(9) . . ?
O5 W8 O115 102.4(11) . . ?
O11 W8 O115 86.1(8) . . ?
O12 W8 O115 154.9(8) . . ?
O18 W8 O115 82.7(8) . . ?
O5 W8 O1S 169.8(10) . . ?
O11 W8 O1S 85.8(7) . . ?
O12 W8 O1S 73.0(7) . . ?
O18 W8 O1S 72.9(7) . . ?
O115 W8 O1S 82.1(7) . . ?
O6 W9 O11 101.5(11) . . ?
O6 W9 O27 99.6(10) . . ?
O11 W9 O27 92.2(9) . . ?
O6 W9 O116 106.0(9) . . ?
O11 W9 O116 83.3(7) . . ?
O27 W9 O116 154.4(8) . . ?
O6 W9 O25 101.0(11) . . ?
O11 W9 O25 157.1(8) . . ?
O27 W9 O25 88.1(8) . . ?
O116 W9 O25 86.6(7) . . ?
O6 W9 O2S 169.6(9) . . ?
O11 W9 O2S 85.7(7) . . ?
O27 W9 O2S 72.4(7) . . ?
O116 W9 O2S 82.1(6) . . ?
O25 W9 O2S 72.6(7) . . ?
O2L W10 O113 97.3(5) . . ?
O2L W10 O113 97.3(5) . 2_775 ?
O113 W10 O113 165.4(10) . 2_775 ?
O2L W10 O112 96.8(7) . . ?
O113 W10 O112 86.8(8) . . ?
O113 W10 O112 91.5(8) 2_775 . ?
O2L W10 O112 96.8(7) . 2_775 ?
O113 W10 O112 91.5(8) . 2_775 ?
O113 W10 O112 86.8(8) 2_775 2_775 ?
O112 W10 O112 166.4(13) . 2_775 ?
O2L W10 O1L 180.000(11) . . ?
O113 W10 O1L 82.7(5) . . ?
O113 W10 O1L 82.7(5) 2_775 . ?
O112 W10 O1L 83.2(7) . . ?
O112 W10 O1L 83.2(7) 2_775 . ?
O2S Se1 O1S 98.8(8) . . ?
O2S Se1 O3S 99.4(8) . . ?
O1S Se1 O3S 99.3(8) . . ?
Se1 O1S W1 136.5(9) . . ?
Se1 O1S W7 118.3(8) . . ?
W1 O1S W7 90.6(6) . . ?
Se1 O1S W8 118.4(9) . . ?
W1 O1S W8 90.5(5) . . ?
W7 O1S W8 91.3(6) . . ?
Se1 O2S W9 119.5(8) . . ?
Se1 O2S W3 133.0(9) . . ?
W9 O2S W3 90.3(6) . . ?
Se1 O2S W4 121.5(8) . . ?
W9 O2S W4 91.3(6) . . ?
W3 O2S W4 90.3(5) . . ?
Se1 O3S W6 120.7(8) . . ?
Se1 O3S W5 121.5(8) . . ?
W6 O3S W5 92.4(6) . . ?
Se1 O3S W2 131.8(9) . . ?
W6 O3S W2 89.9(6) . . ?
W5 O3S W2 89.9(6) . . ?
O11V V11 O115 106.5(6) . 2_775 ?
O11V V11 O115 106.5(6) . . ?
O115 V11 O115 146.9(11) 2_775 . ?
O11V V11 O114 108.3(6) . 2_775 ?
O115 V11 O114 92.3(8) 2_775 2_775 ?
O115 V11 O114 77.3(8) . 2_775 ?
O11V V11 O114 108.3(6) . . ?
O115 V11 O114 77.3(8) 2_775 . ?
O115 V11 O114 92.3(8) . . ?
O114 V11 O114 143.4(11) 2_775 . ?
O11V V11 V12 121.49(18) . 2_775 ?
O115 V11 V12 39.5(6) 2_775 2_775 ?
O115 V11 V12 118.3(7) . 2_775 ?
O114 V11 V12 116.3(6) 2_775 2_775 ?
O114 V11 V12 39.6(6) . 2_775 ?
O11V V11 V12 121.49(18) . . ?
O115 V11 V12 118.3(7) 2_775 . ?
O115 V11 V12 39.5(6) . . ?
O114 V11 V12 39.6(6) 2_775 . ?
O114 V11 V12 116.3(6) . . ?
V12 V11 V12 117.0(4) 2_775 . ?
O12V V12 O116 103.3(9) . . ?
O12V V12 O111 104.1(10) . 2_775 ?
O116 V12 O111 94.7(9) . 2_775 ?
O12V V12 O114 106.1(9) . 2_775 ?
O116 V12 O114 149.2(8) . 2_775 ?
O111 V12 O114 87.0(8) 2_775 2_775 ?
O12V V12 O115 105.1(10) . . ?
O116 V12 O115 88.3(7) . . ?
O111 V12 O115 149.2(9) 2_775 . ?
O114 V12 O115 75.4(8) 2_775 . ?
O12V V12 V11 118.5(8) . . ?
O116 V12 V11 116.2(6) . . ?
O111 V12 V11 116.6(7) 2_775 . ?
O114 V12 V11 39.2(6) 2_775 . ?
O115 V12 V11 37.8(5) . . ?
W8 O11 W9 155.9(11) . . ?
W8 O12 W1 122.5(9) . . ?
W5 O13 W6 124.7(10) . . ?
W6 O14 W2 123.7(11) . . ?
W7 O15 W1 121.1(10) . . ?
W6 O16 W7 156.6(11) . . ?
W2 O17 W5 127.3(9) . . ?
W7 O18 W8 122.2(10) . . ?
W3 O19 W4 125.4(9) . . ?
W1 O20 W3 149.3(12) . . ?
W5 O23 W4 153.8(10) . . ?
W3 O24 W2 147.7(9) . . ?
W4 O25 W9 123.5(10) . . ?
W2 O26 W1 148.8(11) . . ?
W9 O27 W3 125.3(9) . . ?
V12 O111 W6 140.6(11) 2_775 . ?
W4 O112 W10 152.5(11) . . ?
W10 O113 W5 153.2(10) . . ?
V11 O114 V12 101.2(8) . 2_775 ?
V11 O114 W7 124.2(10) . . ?
V12 O114 W7 131.6(11) 2_775 . ?
V11 O115 V12 102.7(8) . . ?
V11 O115 W8 124.9(10) . . ?
V12 O115 W8 131.1(10) . . ?
V12 O116 W9 142.6(10) . . ?
C13 N1 C11 110(2) . . ?
C13 N1 C14 112(2) . . ?
C11 N1 C14 110(3) . . ?
C13 N1 C12 106(3) . . ?
C11 N1 C12 109(3) . . ?
C14 N1 C12 110(3) . . ?
N1 C11 H11A 109.5 . . ?
N1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C24 N2 C21 116(5) . . ?
C24 N2 C23 109(4) . . ?
C21 N2 C23 113(3) . . ?
C24 N2 C22 104(4) . . ?
C21 N2 C22 109(5) . . ?
C23 N2 C22 106(4) . . ?
N2 C21 H21A 109.5 . . ?
N2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
N2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C22 H22A 109.5 . . ?
N2 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N2 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N2 C23 H23A 109.5 . . ?
N2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 H24A 109.5 . . ?
N2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C34 N3 C31 120(5) . . ?
C34 N3 C32 106(4) . . ?
C31 N3 C32 111(4) . . ?
C34 N3 C33 110(4) . . ?
C31 N3 C33 101(4) . . ?
C32 N3 C33 109(4) . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N3 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N3 C34 H34A 109.5 . . ?
N3 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N3 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O42W O41W O43W 127(10) . . ?

_refine_diff_density_max         1.171
_refine_diff_density_min         -2.586
_refine_diff_density_rms         0.223

_shelxl_version_number           2013-2


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
