# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'B18 V12 O54 (O H)6 (H2 O) [K6 (H2 O)12], 2(C4 H15 N3),3(H2 O)'
_chemical_formula_sum            'C8 H68 B18 K6 N6 O76 V12 '
_chemical_formula_weight         2505.09

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'
B B 0.0013 0.0007 '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'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   19.49(2)
_cell_length_b                   19.16(2)
_cell_length_c                   20.09(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.785(12)
_cell_angle_gamma                90.00
_cell_volume                     7499(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            RED
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4830
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6919
_exptl_absorpt_correction_T_max  0.7909
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23100
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.49
_diffrn_reflns_theta_max         26.50
_reflns_number_total             7718
_reflns_number_gt                6665
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0500P)²+60.0089P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    NONE
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7718
_refine_ls_number_parameters     673
_refine_ls_number_restraints     427
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0482
_refine_ls_wR_factor_ref         0.1330
_refine_ls_wR_factor_gt          0.1275
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.164
_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
V1 V 0.93734(3) 0.27158(3) 0.55271(3) 0.01354(15) Uani 1 1 d . . .
V2 V 0.85303(3) 0.40150(3) 0.52296(3) 0.01411(15) Uani 1 1 d . . .
V3 V 0.71161(3) 0.43960(3) 0.46595(3) 0.01509(15) Uani 1 1 d . . .
V4 V 0.68459(3) 0.38296(3) 0.60118(3) 0.01400(15) Uani 1 1 d . . .
V5 V 0.67996(3) 0.24390(4) 0.67149(3) 0.01475(15) Uani 1 1 d . . .
V6 V 0.83169(3) 0.27295(3) 0.65839(3) 0.01380(15) Uani 1 1 d . . .
K1 K 0.41054(6) 0.44629(6) 0.43703(6) 0.0377(3) Uani 1 1 d . . .
K3 K 0.9970(2) 0.25435(14) 0.76927(14) 0.0510(9) Uani 0.50 1 d P . .
K4 K 0.4829(3) 0.2849(2) 0.7449(5) 0.0790(19) Uani 0.50 1 d P . .
O1 O 0.86729(16) 0.28891(18) 0.73167(15) 0.0270(7) Uani 1 1 d . . .
O2 O 0.89863(16) 0.47215(16) 0.53888(17) 0.0266(7) Uani 1 1 d . . .
O3 O 1.01409(15) 0.28976(16) 0.58291(16) 0.0250(7) Uani 1 1 d . . .
O4 O 0.69849(17) 0.52360(16) 0.46548(17) 0.0280(7) Uani 1 1 d . . .
O5 O 0.75976(14) 0.41675(15) 0.55053(14) 0.0183(6) Uani 1 1 d . . .
O6 O 0.89292(14) 0.20798(14) 0.61285(14) 0.0162(6) Uani 1 1 d . . .
O7 O 0.80315(14) 0.41477(15) 0.43727(14) 0.0182(6) Uani 1 1 d . D .
O8 O 0.62284(14) 0.30318(15) 0.61409(14) 0.0179(6) Uani 1 1 d . D .
O9 O 0.74294(14) 0.32046(14) 0.65335(14) 0.0172(6) Uani 1 1 d . . .
O10 O 0.63865(14) 0.39616(15) 0.51428(14) 0.0188(6) Uani 1 1 d . . .
O11 O 0.87108(15) 0.33410(14) 0.59312(14) 0.0183(6) Uani 1 1 d . . .
O12 O 0.95072(14) 0.19286(14) 0.48692(13) 0.0146(5) Uani 1 1 d . . .
O13 O 0.66981(14) 0.40112(14) 0.37951(13) 0.0147(5) Uani 1 1 d . D .
O14 O 0.63059(13) 0.15821(14) 0.63574(14) 0.0158(6) Uani 1 1 d . . .
O15 O 0.91366(15) 0.33504(15) 0.47915(14) 0.0180(6) Uani 1 1 d . . .
O16 O 0.76781(14) 0.19540(14) 0.66859(15) 0.0188(6) Uani 1 1 d . . .
O17 O 0.50615(16) 0.34603(15) 0.62059(15) 0.0219(6) Uani 1 1 d . . .
O18 O 0.67548(15) 0.39048(16) 0.25871(14) 0.0194(6) Uani 1 1 d . D .
O19 O 0.65583(18) 0.2512(2) 0.74836(16) 0.0320(8) Uani 1 1 d . . .
O20 O 0.88126(15) 0.46837(15) 0.36111(15) 0.0221(6) Uani 1 1 d . D .
O21 O 0.97789(15) 0.39909(15) 0.39851(16) 0.0223(6) Uani 1 1 d . . .
O22 O 0.52607(14) 0.22530(14) 0.60563(14) 0.0166(6) Uani 1 1 d . . .
O23 O 0.55336(14) 0.39793(14) 0.42438(13) 0.0151(6) Uani 1 1 d . D .
O24 O 0.77716(14) 0.41844(14) 0.31973(14) 0.0168(6) Uani 1 1 d . D .
O25 O 0.56618(14) 0.38044(15) 0.30877(14) 0.0183(6) Uani 1 1 d . . .
O26 O 0.98715(18) 0.52275(18) 0.3785(2) 0.0439(10) Uani 1 1 d . D .
O27 O 0.57442(16) 0.3964(2) 0.19145(16) 0.0331(8) Uani 1 1 d . . .
O28 O 0.4596(2) 0.45952(18) 0.62854(18) 0.0364(8) Uani 1 1 d . . .
O29 O 0.52062(15) 0.42914(15) 0.53266(14) 0.0203(6) Uani 1 1 d . . .
O30 O 0.66165(16) 0.44844(15) 0.64893(15) 0.0230(6) Uani 1 1 d . . .
B1 B 0.5511(2) 0.2940(2) 0.5883(2) 0.0151(9) Uani 1 1 d . . .
B2 B 0.4963(3) 0.4106(3) 0.5931(2) 0.0221(10) Uani 1 1 d . . .
B3 B 0.5656(2) 0.3826(2) 0.4944(2) 0.0141(8) Uani 1 1 d . . .
B4 B 0.5982(2) 0.3682(2) 0.3768(2) 0.0147(8) Uani 1 1 d . . .
B5 B 0.6054(2) 0.3893(2) 0.2540(2) 0.0179(9) Uani 1 1 d . . .
B6 B 0.7144(2) 0.3789(2) 0.3235(2) 0.0163(9) Uani 1 1 d . . .
B7 B 0.8313(2) 0.4110(2) 0.3704(2) 0.0160(9) Uani 1 1 d . . .
B8 B 0.9487(2) 0.4612(3) 0.3800(3) 0.0229(10) Uani 1 1 d . . .
B9 B 0.9342(2) 0.3358(2) 0.4088(2) 0.0164(9) Uani 1 1 d . . .
O8W O 0.1520(5) 0.2817(6) 0.6317(5) 0.103(3) Uani 0.70 1 d P A 1
O9W O 0.2754(8) 0.6616(15) 0.8623(9) 0.165(11) Uani 0.50 1 d P B 1
O7W O 0.2907(6) 0.2766(6) 0.5627(5) 0.087(3) Uiso 0.60 1 d P C 1
N1 N 0.3660(5) 0.4049(7) 0.7250(6) 0.040(3) Uani 0.50 1 d PDU D 1
N2 N 0.2263(3) 0.4752(3) 0.7597(3) 0.0252(15) Uani 0.50 1 d PDU D 1
N3 N 0.1310(5) 0.6029(4) 0.7942(4) 0.042(2) Uani 0.50 1 d PDU D 1
C1 C 0.3067(5) 0.4225(5) 0.6796(4) 0.037(2) Uani 0.50 1 d PDU D 1
C2 C 0.2377(4) 0.4155(5) 0.7137(5) 0.033(2) Uani 0.50 1 d PDU D 1
C3 C 0.1573(5) 0.4749(4) 0.7909(7) 0.035(3) Uani 0.50 1 d PDU D 1
C4 C 0.1488(6) 0.5402(4) 0.8347(4) 0.040(2) Uani 0.50 1 d PDU D 1
N1B N 0.1536(7) 0.3922(6) 0.6788(5) 0.069(3) Uani 0.50 1 d PDU E 2
N2B N 0.2213(5) 0.5221(4) 0.8022(4) 0.043(2) Uani 0.50 1 d PDU E 2
N3B N 0.2525(6) 0.6805(5) 0.8365(5) 0.037(3) Uani 0.50 1 d PDU E 2
C1B C 0.2083(6) 0.4210(6) 0.7250(6) 0.047(3) Uani 0.50 1 d PDU E 2
C2B C 0.1744(6) 0.4632(6) 0.7814(6) 0.041(3) Uani 0.50 1 d PDU E 2
C3B C 0.1919(5) 0.5666(4) 0.8554(5) 0.048(2) Uani 0.50 1 d PDU E 2
C4B C 0.2432(7) 0.6209(5) 0.8822(5) 0.049(3) Uani 0.50 1 d PDU E 2
O11W O 0.3988(5) 0.4024(7) 0.7269(6) 0.050(3) Uani 0.50 1 d P . 2
O10W O 0.3229(7) 0.3514(7) 0.6206(8) 0.097(4) Uani 0.50 1 d P F 2
O8W' O 0.1842(11) 0.2950(16) 0.5740(12) 0.110(10) Uani 0.30 1 d P . 2
O7W' O 0.3651(5) 0.2726(5) 0.5325(5) 0.040(2) Uiso 0.40 1 d P D 2
O2W O 0.7500 0.2500 0.5000 0.146(5) Uani 1 2 d S . .
O3W O 1.0000 0.3983(4) 0.7500 0.102(3) Uani 1 2 d S . .
O4W O 0.3920(3) 0.3125(3) 0.4920(5) 0.118(3) Uani 1 1 d . . .
O5W O 0.5000 0.1296(5) 0.7500 0.099(3) Uani 1 2 d S . .
K2 K 0.92840(11) 0.60379(9) 0.49055(10) 0.0763(5) Uani 1 1 d . . .
O6W O 0.8044(9) 0.6250(10) 0.4600(8) 0.092(5) Uani 0.40 1 d P G 1
O1W O 0.8913(2) 0.7098(3) 0.5996(3) 0.0721(15) Uani 1 1 d . . .
O6W' O 0.7814(5) 0.6274(5) 0.5143(6) 0.084(3) Uani 0.60 1 d P H 2


_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
V1 O3 1.634(3) . ?
V1 O6 1.939(3) . ?
V1 O11 1.956(3) . ?
V1 O15 1.958(3) . ?
V1 O12 2.028(3) . ?
V1 V6 3.003(2) . ?
V1 V2 3.032(3) . ?
V1 K2 3.667(3) 5_766 ?
V1 K3 3.775(5) 2_756 ?
V2 O2 1.645(3) . ?
V2 O11 1.936(3) . ?
V2 O5 1.939(3) . ?
V2 O15 1.964(3) . ?
V2 O7 1.967(3) . ?
V2 V3 3.040(3) . ?
V3 O4 1.630(4) . ?
V3 O10 1.935(3) . ?
V3 O7 1.951(3) . ?
V3 O5 1.965(3) . ?
V3 O13 2.033(3) . ?
V3 V4 2.987(3) . ?
V3 K1 3.813(3) 5_666 ?
V4 O30 1.650(3) . ?
V4 O5 1.922(3) . ?
V4 O9 1.937(3) . ?
V4 O10 1.953(3) . ?
V4 O8 1.968(3) . ?
V4 V5 3.019(3) . ?
V4 K1 3.827(3) 5_666 ?
V5 O19 1.634(4) . ?
V5 O8 1.944(3) . ?
V5 O16 1.951(3) . ?
V5 O9 1.954(3) . ?
V5 O14 2.024(3) . ?
V5 V6 3.029(3) . ?
V5 K4 3.722(8) 2_656 ?
V6 O1 1.636(3) . ?
V6 O11 1.935(3) . ?
V6 O16 1.954(3) . ?
V6 O9 1.955(3) . ?
V6 O6 1.970(3) . ?
V6 K3 3.617(5) 2_756 ?
V6 K3 3.875(5) . ?
K1 O27 2.776(4) 2_655 ?
K1 O29 2.796(4) 5_666 ?
K1 O4W 2.819(7) . ?
K1 O29 2.854(4) . ?
K1 O23 2.952(4) . ?
K1 O30 2.980(4) 5_666 ?
K1 O4 2.990(4) 5_666 ?
K1 O10 3.324(4) 5_666 ?
K1 B2 3.355(6) 5_666 ?
K1 O28 3.407(5) 5_666 ?
K1 B3 3.425(5) . ?
K1 B2 3.572(6) . ?
K3 K3 0.787(6) 2_756 ?
K3 O1 2.698(6) . ?
K3 O1 2.728(6) 2_756 ?
K3 O3W 2.787(9) . ?
K3 O25 3.009(5) 8_556 ?
K3 O3 3.060(5) 2_756 ?
K3 O25 3.244(5) 7_656 ?
K3 O6 3.269(5) 2_756 ?
K3 O27 3.312(6) 7_656 ?
K3 B5 3.423(6) 7_656 ?
K3 B5 3.490(6) 8_556 ?
K3 V6 3.617(5) 2_756 ?
K4 K4 0.691(10) 2_656 ?
K4 O19 2.788(7) 2_656 ?
K4 O11W 2.803(13) . ?
K4 O17 2.807(10) . ?
K4 O17 2.948(10) 2_656 ?
K4 O5W 2.995(11) . ?
K4 O22 3.159(10) . ?
K4 O22 3.223(10) 2_656 ?
K4 N1 3.255(12) . ?
K4 O11W 3.260(13) 2_656 ?
K4 O19 3.430(7) . ?
K4 B1 3.440(12) 2_656 ?
O1 K3 2.728(6) 2_756 ?
O2 K2 2.771(4) . ?
O3 K2 2.775(4) 5_766 ?
O3 K3 3.060(5) 2_756 ?
O4 K1 2.990(4) 5_666 ?
O6 B4 1.484(5) 7_656 ?
O6 K3 3.269(5) 2_756 ?
O7 B7 1.469(5) . ?
O8 B1 1.486(5) . ?
O10 B3 1.490(5) . ?
O10 K1 3.324(4) 5_666 ?
O12 B3 1.529(5) 7_656 ?
O12 B1 1.532(5) 7_656 ?
O13 B6 1.505(5) . ?
O13 B4 1.532(5) . ?
O14 B7 1.527(5) 7_656 ?
O14 B9 1.528(5) 7_656 ?
O15 B9 1.481(5) . ?
O15 K2 3.332(5) 5_766 ?
O16 B6 1.473(5) 7_656 ?
O17 B2 1.366(6) . ?
O17 B1 1.489(5) . ?
O17 K4 2.948(10) 2_656 ?
O18 B5 1.366(6) . ?
O18 B6 1.502(5) . ?
O19 K4 2.788(7) 2_656 ?
O20 B8 1.364(6) . ?
O20 B7 1.483(5) . ?
O21 B8 1.366(6) . ?
O21 B9 1.501(5) . ?
O21 K2 2.837(4) 5_766 ?
O22 B9 1.438(5) 7_656 ?
O22 B1 1.449(5) . ?
O22 K4 3.223(10) 2_656 ?
O23 B4 1.432(5) . ?
O23 B3 1.449(5) . ?
O24 B6 1.443(5) . ?
O24 B7 1.450(5) . ?
O25 B5 1.369(6) . ?
O25 B4 1.503(5) . ?
O25 K3 3.009(5) 8_455 ?
O25 K3 3.244(5) 7_656 ?
O26 B8 1.398(6) . ?
O26 K2 2.992(6) . ?
O27 B5 1.384(6) . ?
O27 K1 2.776(4) 2_655 ?
O27 K3 3.312(6) 7_656 ?
O28 B2 1.389(6) . ?
O28 K1 3.407(5) 5_666 ?
O29 B2 1.364(6) . ?
O29 B3 1.482(5) . ?
O29 K1 2.796(4) 5_666 ?
O30 K1 2.980(4) 5_666 ?
B1 O12 1.532(5) 7_656 ?
B1 K4 3.440(12) 2_656 ?
B2 K1 3.355(6) 5_666 ?
B3 O12 1.529(5) 7_656 ?
B3 K1 3.582(6) 5_666 ?
B4 O6 1.484(5) 7_656 ?
B5 K3 3.423(6) 7_656 ?
B5 K3 3.490(6) 8_455 ?
B6 O16 1.473(5) 7_656 ?
B7 O14 1.527(5) 7_656 ?
B8 K2 3.551(6) . ?
B9 O22 1.438(5) 7_656 ?
B9 O14 1.528(5) 7_656 ?
B9 K2 3.503(6) 5_766 ?
N1 C1 1.488(8) . ?
N2 C2 1.491(7) . ?
N2 C3 1.501(7) . ?
N3 C4 1.487(7) . ?
C1 C2 1.534(8) . ?
C3 C4 1.542(8) . ?
N1B C1B 1.497(8) . ?
N2B C3B 1.495(7) . ?
N2B C2B 1.504(7) . ?
N3B C4B 1.479(8) . ?
C1B C2B 1.557(9) . ?
C3B C4B 1.529(8) . ?
O11W K4 3.260(13) 2_656 ?
O8W' K2 3.17(2) 5_666 ?
O7W' O4W 1.244(11) . ?
O3W K3 2.787(9) 2_756 ?
O5W K4 2.995(11) 2_656 ?
K2 O6W 2.507(18) . ?
K2 O3 2.775(4) 5_766 ?
K2 O21 2.837(4) 5_766 ?
K2 O6W' 2.954(11) . ?
K2 O1W 3.090(6) . ?
K2 O8W' 3.17(2) 5_666 ?
K2 O15 3.332(5) 5_766 ?
K2 B9 3.503(6) 5_766 ?
K2 V1 3.667(3) 5_766 ?

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
O3 V1 O6 108.91(15) . . ?
O3 V1 O11 108.89(16) . . ?
O6 V1 O11 79.23(13) . . ?
O3 V1 O15 109.83(15) . . ?
O6 V1 O15 139.59(13) . . ?
O11 V1 O15 77.85(13) . . ?
O3 V1 O12 105.41(15) . . ?
O6 V1 O12 90.42(14) . . ?
O11 V1 O12 145.69(12) . . ?
O15 V1 O12 90.13(14) . . ?
O3 V1 V6 112.06(14) . . ?
O6 V1 V6 40.17(9) . . ?
O11 V1 V6 39.23(9) . . ?
O15 V1 V6 112.17(10) . . ?
O12 V1 V6 124.90(9) . . ?
O3 V1 V2 112.47(13) . . ?
O6 V1 V2 112.90(10) . . ?
O11 V1 V2 38.58(9) . . ?
O15 V1 V2 39.44(9) . . ?
O12 V1 V2 124.22(10) . . ?
V6 V1 V2 75.69(5) . . ?
O3 V1 K2 45.37(12) . 5_766 ?
O6 V1 K2 153.22(10) . 5_766 ?
O11 V1 K2 100.63(12) . 5_766 ?
O15 V1 K2 64.52(10) . 5_766 ?
O12 V1 K2 102.88(10) . 5_766 ?
V6 V1 K2 132.21(6) . 5_766 ?
V2 V1 K2 78.74(9) . 5_766 ?
O3 V1 K3 52.23(13) . 2_756 ?
O6 V1 K3 59.98(11) . 2_756 ?
O11 V1 K3 82.49(11) . 2_756 ?
O15 V1 K3 146.54(10) . 2_756 ?
O12 V1 K3 120.37(10) . 2_756 ?
V6 V1 K3 63.31(10) . 2_756 ?
V2 V1 K3 115.10(5) . 2_756 ?
K2 V1 K3 93.33(8) 5_766 2_756 ?
O2 V2 O11 108.83(16) . . ?
O2 V2 O5 109.02(16) . . ?
O11 V2 O5 92.49(13) . . ?
O2 V2 O15 106.97(16) . . ?
O11 V2 O15 78.19(13) . . ?
O5 V2 O15 143.92(13) . . ?
O2 V2 O7 108.24(15) . . ?
O11 V2 O7 142.85(13) . . ?
O5 V2 O7 77.77(13) . . ?
O15 V2 O7 88.83(13) . . ?
O2 V2 V1 110.56(14) . . ?
O11 V2 V1 39.07(9) . . ?
O5 V2 V1 125.07(9) . . ?
O15 V2 V1 39.28(9) . . ?
O7 V2 V1 121.92(9) . . ?
O2 V2 V3 110.69(13) . . ?
O11 V2 V3 125.20(9) . . ?
O5 V2 V3 39.14(10) . . ?
O15 V2 V3 122.54(10) . . ?
O7 V2 V3 38.90(8) . . ?
V1 V2 V3 138.65(3) . . ?
O4 V3 O10 108.07(16) . . ?
O4 V3 O7 112.58(15) . . ?
O10 V3 O7 137.43(13) . . ?
O4 V3 O5 107.20(15) . . ?
O10 V3 O5 78.98(14) . . ?
O7 V3 O5 77.55(13) . . ?
O4 V3 O13 107.14(15) . . ?
O10 V3 O13 89.50(13) . . ?
O7 V3 O13 90.29(13) . . ?
O5 V3 O13 145.64(13) . . ?
O4 V3 V4 109.39(13) . . ?
O10 V3 V4 40.03(9) . . ?
O7 V3 V4 111.63(9) . . ?
O5 V3 V4 39.25(10) . . ?
O13 V3 V4 124.57(10) . . ?
O4 V3 V2 112.31(12) . . ?
O10 V3 V2 112.30(11) . . ?
O7 V3 V2 39.28(10) . . ?
O5 V3 V2 38.53(8) . . ?
O13 V3 V2 124.68(9) . . ?
V4 V3 V2 75.74(5) . . ?
O4 V3 K1 48.41(12) . 5_666 ?
O10 V3 K1 60.66(11) . 5_666 ?
O7 V3 K1 151.91(9) . 5_666 ?
O5 V3 K1 88.56(11) . 5_666 ?
O13 V3 K1 113.86(10) . 5_666 ?
V4 V3 K1 67.23(6) . 5_666 ?
V2 V3 K1 121.22(6) . 5_666 ?
O30 V4 O5 106.04(15) . . ?
O30 V4 O9 108.72(16) . . ?
O5 V4 O9 92.89(14) . . ?
O30 V4 O10 107.22(15) . . ?
O5 V4 O10 79.57(14) . . ?
O9 V4 O10 143.96(13) . . ?
O30 V4 O8 109.66(15) . . ?
O5 V4 O8 144.19(13) . . ?
O9 V4 O8 78.43(14) . . ?
O10 V4 O8 87.32(13) . . ?
O30 V4 V3 108.12(13) . . ?
O5 V4 V3 40.30(9) . . ?
O9 V4 V3 126.83(10) . . ?
O10 V4 V3 39.57(10) . . ?
O8 V4 V3 121.87(9) . . ?
O30 V4 V5 112.76(13) . . ?
O5 V4 V5 125.42(9) . . ?
O9 V4 V5 39.34(9) . . ?
O10 V4 V5 120.86(9) . . ?
O8 V4 V5 39.21(9) . . ?
V3 V4 V5 139.02(3) . . ?
O30 V4 K1 47.76(12) . 5_666 ?
O5 V4 K1 88.75(11) . 5_666 ?
O9 V4 K1 155.48(9) . 5_666 ?
O10 V4 K1 60.28(9) . 5_666 ?
O8 V4 K1 113.35(12) . 5_666 ?
V3 V4 K1 66.73(4) . 5_666 ?
V5 V4 K1 145.82(5) . 5_666 ?
O19 V5 O8 109.52(17) . . ?
O19 V5 O16 110.34(16) . . ?
O8 V5 O16 138.39(13) . . ?
O19 V5 O9 108.24(16) . . ?
O8 V5 O9 78.59(14) . . ?
O16 V5 O9 78.18(14) . . ?
O19 V5 O14 104.89(16) . . ?
O8 V5 O14 90.38(14) . . ?
O16 V5 O14 90.62(13) . . ?
O9 V5 O14 146.87(12) . . ?
O19 V5 V4 112.36(14) . . ?
O8 V5 V4 39.79(9) . . ?
O16 V5 V4 111.57(9) . . ?
O9 V5 V4 38.92(9) . . ?
O14 V5 V4 124.83(10) . . ?
O19 V5 V6 112.14(13) . . ?
O8 V5 V6 112.56(10) . . ?
O16 V5 V6 39.16(10) . . ?
O9 V5 V6 39.22(9) . . ?
O14 V5 V6 124.97(8) . . ?
V4 V5 V6 75.73(3) . . ?
O19 V5 K4 44.00(18) . 2_656 ?
O8 V5 K4 70.35(16) . 2_656 ?
O16 V5 K4 151.15(15) . 2_656 ?
O9 V5 K4 118.38(12) . 2_656 ?
O14 V5 K4 85.90(12) . 2_656 ?
V4 V5 K4 93.64(10) . 2_656 ?
V6 V5 K4 148.15(10) . 2_656 ?
O1 V6 O11 109.28(16) . . ?
O1 V6 O16 107.55(16) . . ?
O11 V6 O16 143.07(13) . . ?
O1 V6 O9 108.01(15) . . ?
O11 V6 O9 92.98(13) . . ?
O16 V6 O9 78.11(14) . . ?
O1 V6 O6 106.85(15) . . ?
O11 V6 O6 79.00(13) . . ?
O16 V6 O6 88.00(14) . . ?
O9 V6 O6 144.93(13) . . ?
O1 V6 V1 110.89(14) . . ?
O11 V6 V1 39.75(9) . . ?
O16 V6 V1 121.38(10) . . ?
O9 V6 V1 126.34(10) . . ?
O6 V6 V1 39.42(9) . . ?
O1 V6 V5 110.12(12) . . ?
O11 V6 V5 125.40(9) . . ?
O16 V6 V5 39.09(9) . . ?
O9 V6 V5 39.21(10) . . ?
O6 V6 V5 122.11(10) . . ?
V1 V6 V5 138.82(5) . . ?
O1 V6 K3 45.32(12) . 2_756 ?
O11 V6 K3 87.20(11) . 2_756 ?
O16 V6 K3 117.79(11) . 2_756 ?
O9 V6 K3 150.58(10) . 2_756 ?
O6 V6 K3 63.85(11) . 2_756 ?
V1 V6 K3 68.80(9) . 2_756 ?
V5 V6 K3 146.99(7) . 2_756 ?
O1 V6 K3 34.78(12) . . ?
O11 V6 K3 96.02(12) . . ?
O16 V6 K3 113.00(11) . . ?
O9 V6 K3 142.29(10) . . ?
O6 V6 K3 72.78(11) . . ?
V1 V6 K3 80.18(10) . . ?
V5 V6 K3 136.85(7) . . ?
K3 V6 K3 11.39(10) 2_756 . ?
O27 K1 O29 115.64(11) 2_655 5_666 ?
O27 K1 O4W 94.0(2) 2_655 . ?
O29 K1 O4W 139.2(2) 5_666 . ?
O27 K1 O29 119.15(11) 2_655 . ?
O29 K1 O29 66.81(11) 5_666 . ?
O4W K1 O29 74.59(18) . . ?
O27 K1 O23 71.62(9) 2_655 . ?
O29 K1 O23 80.76(10) 5_666 . ?
O4W K1 O23 83.16(14) . . ?
O29 K1 O23 47.99(9) . . ?
O27 K1 O30 75.90(12) 2_655 5_666 ?
O29 K1 O30 76.28(11) 5_666 5_666 ?
O4W K1 O30 141.15(17) . 5_666 ?
O29 K1 O30 143.08(10) . 5_666 ?
O23 K1 O30 126.31(9) . 5_666 ?
O27 K1 O4 140.62(11) 2_655 5_666 ?
O29 K1 O4 92.21(10) 5_666 5_666 ?
O4W K1 O4 79.43(16) . 5_666 ?
O29 K1 O4 96.67(12) . 5_666 ?
O23 K1 O4 143.91(10) . 5_666 ?
O30 K1 O4 85.21(11) 5_666 5_666 ?
O27 K1 O10 128.77(10) 2_655 5_666 ?
O29 K1 O10 45.68(10) 5_666 5_666 ?
O4W K1 O10 131.99(18) . 5_666 ?
O29 K1 O10 97.14(9) . 5_666 ?
O23 K1 O10 126.28(8) . 5_666 ?
O30 K1 O10 54.57(10) 5_666 5_666 ?
O4 K1 O10 54.18(8) 5_666 5_666 ?
O27 K1 B2 92.33(13) 2_655 5_666 ?
O29 K1 B2 23.44(11) 5_666 5_666 ?
O4W K1 B2 152.97(17) . 5_666 ?
O29 K1 B2 79.39(12) . 5_666 ?
O23 K1 B2 73.99(12) . 5_666 ?
O30 K1 B2 65.82(13) 5_666 5_666 ?
O4 K1 B2 111.10(12) 5_666 5_666 ?
O10 K1 B2 58.20(12) 5_666 5_666 ?
O27 K1 O28 73.86(11) 2_655 5_666 ?
O29 K1 O28 43.50(9) 5_666 5_666 ?
O4W K1 O28 137.65(14) . 5_666 ?
O29 K1 O28 76.66(12) . 5_666 ?
O23 K1 O28 54.49(10) . 5_666 ?
O30 K1 O28 76.13(11) 5_666 5_666 ?
O4 K1 O28 134.63(10) 5_666 5_666 ?
O10 K1 O28 81.78(10) 5_666 5_666 ?
B2 K1 O28 23.70(10) 5_666 5_666 ?
O27 K1 B3 94.14(11) 2_655 . ?
O29 K1 B3 79.57(12) 5_666 . ?
O4W K1 B3 70.50(16) . . ?
O29 K1 B3 25.27(9) . . ?
O23 K1 B3 24.88(9) . . ?
O30 K1 B3 146.30(10) 5_666 . ?
O4 K1 B3 119.07(12) 5_666 . ?
O10 K1 B3 118.97(10) 5_666 . ?
B2 K1 B3 82.85(13) 5_666 . ?
O28 K1 B3 70.17(12) 5_666 . ?
O27 K1 B2 133.59(12) 2_655 . ?
O29 K1 B2 76.37(11) 5_666 . ?
O4W K1 B2 62.9(2) . . ?
O29 K1 B2 20.92(10) . . ?
O23 K1 B2 66.35(11) . . ?
O30 K1 B2 146.90(11) 5_666 . ?
O4 K1 B2 77.58(13) 5_666 . ?
O10 K1 B2 92.70(10) 5_666 . ?
B2 K1 B2 94.23(13) 5_666 . ?
O28 K1 B2 96.19(13) 5_666 . ?
B3 K1 B2 41.65(11) . . ?
K3 K3 O1 83.8(6) 2_756 . ?
K3 K3 O1 79.5(6) 2_756 2_756 ?
O1 K3 O1 147.01(17) . 2_756 ?
K3 K3 O3W 81.89(7) 2_756 . ?
O1 K3 O3W 75.03(11) . . ?
O1 K3 O3W 74.57(11) 2_756 . ?
K3 K3 O25 100.4(3) 2_756 8_556 ?
O1 K3 O25 133.86(15) . 8_556 ?
O1 K3 O25 77.49(14) 2_756 8_556 ?
O3W K3 O25 151.07(17) . 8_556 ?
K3 K3 O3 166.4(2) 2_756 2_756 ?
O1 K3 O3 97.09(14) . 2_756 ?
O1 K3 O3 92.90(13) 2_756 2_756 ?
O3W K3 O3 85.28(10) . 2_756 ?
O25 K3 O3 88.80(11) 8_556 2_756 ?
K3 K3 O25 65.8(3) 2_756 7_656 ?
O1 K3 O25 73.87(13) . 7_656 ?
O1 K3 O25 122.92(14) 2_756 7_656 ?
O3W K3 O25 136.93(13) . 7_656 ?
O25 K3 O25 66.68(13) 8_556 7_656 ?
O3 K3 O25 127.47(13) 2_756 7_656 ?
K3 K3 O6 126.7(6) 2_756 2_756 ?
O1 K3 O6 149.06(15) . 2_756 ?
O1 K3 O6 57.05(12) 2_756 2_756 ?
O3W K3 O6 110.70(12) . 2_756 ?
O25 K3 O6 45.32(9) 8_556 2_756 ?
O3 K3 O6 54.68(10) 2_756 2_756 ?
O25 K3 O6 111.36(12) 7_656 2_756 ?
K3 K3 O27 108.1(3) 2_756 7_656 ?
O1 K3 O27 83.33(15) . 7_656 ?
O1 K3 O27 128.92(14) 2_756 7_656 ?
O3W K3 O27 155.13(17) . 7_656 ?
O25 K3 O27 51.45(11) 8_556 7_656 ?
O3 K3 O27 85.38(12) 2_756 7_656 ?
O25 K3 O27 42.68(10) 7_656 7_656 ?
O6 K3 O27 82.04(11) 2_756 7_656 ?
K3 K3 B5 88.3(4) 2_756 7_656 ?
O1 K3 B5 67.80(15) . 7_656 ?
O1 K3 B5 139.07(16) 2_756 7_656 ?
O3W K3 B5 142.36(16) . 7_656 ?
O25 K3 B5 66.44(13) 8_556 7_656 ?
O3 K3 B5 104.62(14) 2_756 7_656 ?
O25 K3 B5 23.51(10) 7_656 7_656 ?
O6 K3 B5 104.30(13) 2_756 7_656 ?
O27 K3 B5 23.64(10) 7_656 7_656 ?
K3 K3 B5 78.7(4) 2_756 8_556 ?
O1 K3 B5 137.19(15) . 8_556 ?
O1 K3 B5 66.48(15) 2_756 8_556 ?
O3W K3 B5 138.88(17) . 8_556 ?
O25 K3 B5 22.82(10) 8_556 8_556 ?
O3 K3 B5 108.75(13) 2_756 8_556 ?
O25 K3 B5 63.33(12) 7_656 8_556 ?
O6 K3 B5 57.56(11) 2_756 8_556 ?
O27 K3 B5 65.99(13) 7_656 8_556 ?
B5 K3 B5 72.88(18) 7_656 8_556 ?
K3 K3 V6 103.3(6) 2_756 2_756 ?
O1 K3 V6 158.95(12) . 2_756 ?
O1 K3 V6 25.25(8) 2_756 2_756 ?
O3W K3 V6 86.27(9) . 2_756 ?
O25 K3 V6 65.05(10) 8_556 2_756 ?
O3 K3 V6 71.37(10) 2_756 2_756 ?
O25 K3 V6 127.17(11) 7_656 2_756 ?
O6 K3 V6 32.74(7) 2_756 2_756 ?
O27 K3 V6 112.31(11) 7_656 2_756 ?
B5 K3 V6 131.37(12) 7_656 2_756 ?
B5 K3 V6 63.84(11) 8_556 2_756 ?
K4 K4 O19 155.8(16) 2_656 2_656 ?
K4 K4 O11W 126.4(3) 2_656 . ?
O19 K4 O11W 68.2(3) 2_656 . ?
K4 K4 O17 94.9(15) 2_656 . ?
O19 K4 O17 108.9(2) 2_656 . ?
O11W K4 O17 70.1(3) . . ?
K4 K4 O17 71.6(15) 2_656 2_656 ?
O19 K4 O17 95.1(3) 2_656 2_656 ?
O11W K4 O17 79.8(3) . 2_656 ?
O17 K4 O17 129.81(19) . 2_656 ?
K4 K4 O5W 83.38(10) 2_656 . ?
O19 K4 O5W 82.83(14) 2_656 . ?
O11W K4 O5W 150.1(3) . . ?
O17 K4 O5W 115.1(3) . . ?
O17 K4 O5W 111.0(3) 2_656 . ?
K4 K4 O22 89.1(16) 2_656 . ?
O19 K4 O22 104.2(2) 2_656 . ?
O11W K4 O22 110.3(4) . . ?
O17 K4 O22 46.28(18) . . ?
O17 K4 O22 160.4(2) 2_656 . ?
O5W K4 O22 68.86(16) . . ?
K4 K4 O22 78.5(16) 2_656 2_656 ?
O19 K4 O22 78.0(2) 2_656 2_656 ?
O11W K4 O22 110.8(4) . 2_656 ?
O17 K4 O22 172.5(2) . 2_656 ?
O17 K4 O22 44.83(17) 2_656 2_656 ?
O5W K4 O22 67.99(15) . 2_656 ?
O22 K4 O22 136.12(17) . 2_656 ?
K4 K4 N1 134.5(4) 2_656 . ?
O19 K4 N1 59.5(3) 2_656 . ?
O11W K4 N1 8.6(4) . . ?
O17 K4 N1 74.2(3) . . ?
O17 K4 N1 82.0(3) 2_656 . ?
O5W K4 N1 141.6(3) . . ?
O22 K4 N1 110.6(3) . . ?
O22 K4 N1 107.8(3) 2_656 . ?
K4 K4 O11W 43.8(3) 2_656 2_656 ?
O19 K4 O11W 146.4(3) 2_656 2_656 ?
O11W K4 O11W 82.8(5) . 2_656 ?
O17 K4 O11W 74.5(3) . 2_656 ?
O17 K4 O11W 62.3(3) 2_656 2_656 ?
O5W K4 O11W 127.1(3) . 2_656 ?
O22 K4 O11W 101.4(3) . 2_656 ?
O22 K4 O11W 98.1(3) 2_656 2_656 ?
N1 K4 O11W 91.2(3) . 2_656 ?
K4 K4 O19 19.4(13) 2_656 . ?
O19 K4 O19 155.4(2) 2_656 . ?
O11W K4 O19 136.4(3) . . ?
O17 K4 O19 84.9(2) . . ?
O17 K4 O19 90.75(18) 2_656 . ?
O5W K4 O19 72.80(12) . . ?
O22 K4 O19 70.23(17) . . ?
O22 K4 O19 89.78(17) 2_656 . ?
N1 K4 O19 145.0(3) . . ?
O11W K4 O19 55.8(2) 2_656 . ?
K4 K4 B1 85.5(17) 2_656 2_656 ?
O19 K4 B1 75.4(2) 2_656 2_656 ?
O11W K4 B1 87.4(3) . 2_656 ?
O17 K4 B1 152.40(19) . 2_656 ?
O17 K4 B1 25.50(13) 2_656 2_656 ?
O5W K4 B1 92.4(2) . 2_656 ?
O22 K4 B1 160.97(17) . 2_656 ?
O22 K4 B1 24.85(12) 2_656 2_656 ?
N1 K4 B1 85.9(3) . 2_656 ?
O11W K4 B1 87.3(3) 2_656 2_656 ?
O19 K4 B1 102.0(2) . 2_656 ?
V6 O1 K3 124.97(17) . . ?
V6 O1 K3 109.42(16) . 2_756 ?
K3 O1 K3 16.66(12) . 2_756 ?
V2 O2 K2 143.01(18) . . ?
V1 O3 K2 109.85(16) . 5_766 ?
V1 O3 K3 102.80(16) . 2_756 ?
K2 O3 K3 136.13(13) 5_766 2_756 ?
V3 O4 K1 107.54(15) . 5_666 ?
V4 O5 V2 146.86(17) . . ?
V4 O5 V3 100.45(15) . . ?
V2 O5 V3 102.32(14) . . ?
B4 O6 V1 130.7(2) 7_656 . ?
B4 O6 V6 128.8(2) 7_656 . ?
V1 O6 V6 100.41(14) . . ?
B4 O6 K3 95.4(2) 7_656 2_756 ?
V1 O6 K3 89.12(13) . 2_756 ?
V6 O6 K3 83.41(13) . 2_756 ?
B7 O7 V3 130.8(2) . . ?
B7 O7 V2 127.3(3) . . ?
V3 O7 V2 101.82(14) . . ?
B1 O8 V5 130.7(2) . . ?
B1 O8 V4 128.3(2) . . ?
V5 O8 V4 101.01(14) . . ?
V4 O9 V5 101.74(15) . . ?
V4 O9 V6 145.06(16) . . ?
V5 O9 V6 101.57(15) . . ?
B3 O10 V3 130.7(2) . . ?
B3 O10 V4 128.6(2) . . ?
V3 O10 V4 100.40(15) . . ?
B3 O10 K1 87.5(2) . 5_666 ?
V3 O10 K1 88.86(12) . 5_666 ?
V4 O10 K1 89.03(11) . 5_666 ?
V6 O11 V2 146.14(17) . . ?
V6 O11 V1 101.02(14) . . ?
V2 O11 V1 102.35(15) . . ?
B3 O12 B1 113.5(3) 7_656 7_656 ?
B3 O12 V1 120.8(2) 7_656 . ?
B1 O12 V1 121.4(2) 7_656 . ?
B6 O13 B4 113.8(3) . . ?
B6 O13 V3 121.1(2) . . ?
B4 O13 V3 121.3(2) . . ?
B7 O14 B9 114.4(3) 7_656 7_656 ?
B7 O14 V5 120.4(2) 7_656 . ?
B9 O14 V5 121.4(2) 7_656 . ?
B9 O15 V1 131.4(2) . . ?
B9 O15 V2 127.3(2) . . ?
V1 O15 V2 101.28(14) . . ?
B9 O15 K2 84.0(2) . 5_766 ?
V1 O15 K2 83.45(11) . 5_766 ?
V2 O15 K2 104.79(13) . 5_766 ?
B6 O16 V5 131.4(2) 7_656 . ?
B6 O16 V6 126.7(3) 7_656 . ?
V5 O16 V6 101.74(15) . . ?
B2 O17 B1 120.5(3) . . ?
B2 O17 K4 135.5(3) . . ?
B1 O17 K4 102.7(2) . . ?
B2 O17 K4 137.4(3) . 2_656 ?
B1 O17 K4 96.1(2) . 2_656 ?
K4 O17 K4 13.5(2) . 2_656 ?
B5 O18 B6 122.3(3) . . ?
V5 O19 K4 112.0(3) . 2_656 ?
V5 O19 K4 107.9(2) . . ?
K4 O19 K4 4.7(3) 2_656 . ?
B8 O20 B7 121.4(3) . . ?
B8 O21 B9 120.6(3) . . ?
B8 O21 K2 118.9(3) . 5_766 ?
B9 O21 K2 103.4(2) . 5_766 ?
B9 O22 B1 120.2(3) 7_656 . ?
B9 O22 K4 129.2(3) 7_656 . ?
B1 O22 K4 89.1(2) . . ?
B9 O22 K4 121.4(2) 7_656 2_656 ?
B1 O22 K4 86.0(2) . 2_656 ?
K4 O22 K4 12.37(18) . 2_656 ?
B4 O23 B3 118.8(3) . . ?
B4 O23 K1 141.1(2) . . ?
B3 O23 K1 96.2(2) . . ?
B6 O24 B7 120.8(3) . . ?
B5 O25 B4 121.6(3) . . ?
B5 O25 K3 98.7(3) . 8_455 ?
B4 O25 K3 106.0(2) . 8_455 ?
B5 O25 K3 85.6(3) . 7_656 ?
B4 O25 K3 117.1(2) . 7_656 ?
K3 O25 K3 13.80(11) 8_455 7_656 ?
B8 O26 K2 101.8(3) . . ?
B5 O27 K1 145.3(3) . 2_655 ?
B5 O27 K3 82.7(3) . 7_656 ?
K1 O27 K3 125.40(13) 2_655 7_656 ?
B2 O28 K1 76.0(3) . 5_666 ?
B2 O29 B3 122.1(3) . . ?
B2 O29 K1 101.9(3) . 5_666 ?
B3 O29 K1 109.9(2) . 5_666 ?
B2 O29 K1 110.7(3) . . ?
B3 O29 K1 99.5(2) . . ?
K1 O29 K1 113.19(11) 5_666 . ?
V4 O30 K1 108.04(16) . 5_666 ?
O22 B1 O8 110.2(3) . . ?
O22 B1 O17 107.3(3) . . ?
O8 B1 O17 109.2(3) . . ?
O22 B1 O12 112.9(3) . 7_656 ?
O8 B1 O12 108.4(3) . 7_656 ?
O17 B1 O12 108.8(3) . 7_656 ?
O22 B1 K4 69.2(2) . 2_656 ?
O8 B1 K4 82.8(2) . 2_656 ?
O17 B1 K4 58.4(2) . 2_656 ?
O12 B1 K4 166.0(3) 7_656 2_656 ?
O22 B1 K4 66.1(2) . . ?
O8 B1 K4 94.2(2) . . ?
O17 B1 K4 52.42(19) . . ?
O12 B1 K4 155.3(3) 7_656 . ?
K4 B1 K4 11.49(17) 2_656 . ?
O29 B2 O17 123.2(4) . . ?
O29 B2 O28 118.6(4) . . ?
O17 B2 O28 118.2(4) . . ?
O29 B2 K1 54.6(2) . 5_666 ?
O17 B2 K1 138.0(3) . 5_666 ?
O28 B2 K1 80.3(3) . 5_666 ?
O29 B2 K1 48.3(2) . . ?
O17 B2 K1 125.8(3) . . ?
O28 B2 K1 94.9(3) . . ?
K1 B2 K1 85.77(12) 5_666 . ?
O23 B3 O29 107.4(3) . . ?
O23 B3 O10 110.6(3) . . ?
O29 B3 O10 109.3(3) . . ?
O23 B3 O12 113.7(3) . 7_656 ?
O29 B3 O12 108.1(3) . 7_656 ?
O10 B3 O12 107.7(3) . 7_656 ?
O23 B3 K1 58.97(19) . . ?
O29 B3 K1 55.26(19) . . ?
O10 B3 K1 148.6(3) . . ?
O12 B3 K1 103.4(2) 7_656 . ?
O23 B3 K1 101.7(2) . 5_666 ?
O29 B3 K1 47.23(18) . 5_666 ?
O10 B3 K1 68.0(2) . 5_666 ?
O12 B3 K1 142.8(3) 7_656 5_666 ?
K1 B3 K1 84.58(11) . 5_666 ?
O23 B4 O6 111.7(3) . 7_656 ?
O23 B4 O25 107.5(3) . . ?
O6 B4 O25 108.9(3) 7_656 . ?
O23 B4 O13 112.8(3) . . ?
O6 B4 O13 107.3(3) 7_656 . ?
O25 B4 O13 108.6(3) . . ?
O18 B5 O25 121.9(4) . . ?
O18 B5 O27 117.9(4) . . ?
O25 B5 O27 120.2(4) . . ?
O18 B5 K3 126.9(3) . 7_656 ?
O25 B5 K3 70.9(2) . 7_656 ?
O27 B5 K3 73.7(3) . 7_656 ?
O18 B5 K3 127.9(3) . 8_455 ?
O25 B5 K3 58.5(2) . 8_455 ?
O27 B5 K3 84.8(3) . 8_455 ?
K3 B5 K3 13.02(10) 7_656 8_455 ?
O24 B6 O16 108.4(3) . 7_656 ?
O24 B6 O18 106.5(3) . . ?
O16 B6 O18 110.3(3) 7_656 . ?
O24 B6 O13 113.6(3) . . ?
O16 B6 O13 109.4(3) 7_656 . ?
O18 B6 O13 108.6(3) . . ?
O24 B7 O7 110.6(3) . . ?
O24 B7 O20 107.8(3) . . ?
O7 B7 O20 110.1(3) . . ?
O24 B7 O14 111.9(3) . 7_656 ?
O7 B7 O14 108.2(3) . 7_656 ?
O20 B7 O14 108.1(3) . 7_656 ?
O20 B8 O21 123.6(4) . . ?
O20 B8 O26 114.9(4) . . ?
O21 B8 O26 121.5(4) . . ?
O20 B8 K2 88.3(3) . . ?
O21 B8 K2 123.6(3) . . ?
O26 B8 K2 55.6(3) . . ?
O22 B9 O15 110.3(3) 7_656 . ?
O22 B9 O21 108.6(3) 7_656 . ?
O15 B9 O21 108.0(3) . . ?
O22 B9 O14 112.6(3) 7_656 7_656 ?
O15 B9 O14 108.5(3) . 7_656 ?
O21 B9 O14 108.7(3) . 7_656 ?
O22 B9 K2 88.7(2) 7_656 5_766 ?
O15 B9 K2 71.1(2) . 5_766 ?
O21 B9 K2 52.01(19) . 5_766 ?
O14 B9 K2 156.3(3) 7_656 5_766 ?
C1 N1 K4 139.7(8) . . ?
C2 N2 C3 114.2(6) . . ?
N1 C1 C2 112.4(6) . . ?
N2 C2 C1 111.1(6) . . ?
N2 C3 C4 110.4(6) . . ?
N3 C4 C3 111.8(7) . . ?
C3B N2B C2B 112.6(6) . . ?
N1B C1B C2B 109.4(7) . . ?
N2B C2B C1B 108.9(7) . . ?
N2B C3B C4B 112.3(6) . . ?
N3B C4B C3B 113.5(7) . . ?
K4 O11W K4 9.82(15) . 2_656 ?
K3 O3W K3 16.23(13) 2_756 . ?
O7W' O4W K1 151.3(6) . . ?
K4 O5W K4 13.24(19) . 2_656 ?
O6W K2 O2 91.3(4) . . ?
O6W K2 O3 98.8(4) . 5_766 ?
O2 K2 O3 161.47(13) . 5_766 ?
O6W K2 O21 141.9(4) . 5_766 ?
O2 K2 O21 81.01(11) . 5_766 ?
O3 K2 O21 99.86(12) 5_766 5_766 ?
O6W K2 O6W' 23.5(4) . . ?
O2 K2 O6W' 82.4(2) . . ?
O3 K2 O6W' 112.5(2) 5_766 . ?
O21 K2 O6W' 118.7(3) 5_766 . ?
O6W K2 O26 106.8(4) . . ?
O2 K2 O26 83.13(13) . . ?
O3 K2 O26 79.11(13) 5_766 . ?
O21 K2 O26 109.20(13) 5_766 . ?
O6W' K2 O26 126.7(2) . . ?
O6W K2 O1W 79.8(4) . . ?
O2 K2 O1W 107.09(16) . . ?
O3 K2 O1W 90.06(16) 5_766 . ?
O21 K2 O1W 67.34(14) 5_766 . ?
O6W' K2 O1W 62.3(2) . . ?
O26 K2 O1W 168.02(13) . . ?
O6W K2 O8W' 32.1(6) . 5_666 ?
O2 K2 O8W' 123.3(6) . 5_666 ?
O3 K2 O8W' 67.6(6) 5_766 5_666 ?
O21 K2 O8W' 138.8(4) 5_766 5_666 ?
O6W' K2 O8W' 46.5(6) . 5_666 ?
O26 K2 O8W' 106.6(4) . 5_666 ?
O1W K2 O8W' 73.4(4) . 5_666 ?
O6W K2 O15 149.9(4) . 5_766 ?
O2 K2 O15 117.30(10) . 5_766 ?
O3 K2 O15 56.79(9) 5_766 5_766 ?
O21 K2 O15 45.17(9) 5_766 5_766 ?
O6W' K2 O15 144.3(2) . 5_766 ?
O26 K2 O15 86.97(11) . 5_766 ?
O1W K2 O15 82.78(12) . 5_766 ?
O8W' K2 O15 118.8(6) 5_666 5_766 ?
O6W K2 B9 143.3(4) . 5_766 ?
O2 K2 B9 105.28(12) . 5_766 ?
O3 K2 B9 75.50(12) 5_766 5_766 ?
O21 K2 B9 24.64(9) 5_766 5_766 ?
O6W' K2 B9 125.7(3) . 5_766 ?
O26 K2 B9 107.60(14) . 5_766 ?
O1W K2 B9 64.19(13) . 5_766 ?
O8W' K2 B9 122.7(5) 5_666 5_766 ?
O15 K2 B9 24.87(9) 5_766 5_766 ?
O6W K2 B8 95.6(4) . . ?
O2 K2 B8 63.08(13) . . ?
O3 K2 B8 100.28(14) 5_766 . ?
O21 K2 B8 113.24(13) 5_766 . ?
O6W' K2 B8 110.3(2) . . ?
O26 K2 B8 22.67(10) . . ?
O1W K2 B8 169.24(14) . . ?
O8W' K2 B8 107.7(4) 5_666 . ?
O15 K2 B8 105.34(11) 5_766 . ?
B9 K2 B8 121.16(13) 5_766 . ?
O6W K2 V1 121.7(4) . 5_766 ?
O2 K2 V1 146.58(10) . 5_766 ?
O3 K2 V1 24.78(7) 5_766 5_766 ?
O21 K2 V1 75.65(9) 5_766 5_766 ?
O6W' K2 V1 129.9(2) . 5_766 ?
O26 K2 V1 82.37(10) . 5_766 ?
O1W K2 V1 85.65(12) . 5_766 ?
O8W' K2 V1 89.7(6) 5_666 5_766 ?
O15 K2 V1 32.03(6) 5_766 5_766 ?
B9 K2 V1 51.90(9) 5_766 5_766 ?
B8 K2 V1 104.99(11) . 5_766 ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.376
_refine_diff_density_min         -2.300
_refine_diff_density_rms         0.133
_database_code_depnum_ccdc_archive 'CCDC 968042'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'B20 V6 O42 (O H)8 (H2 O) [K (H2 O)]2, 2(C4 H16 N3), 6(H2 O)'
_chemical_formula_sum            'C8 H58 B20 K2 N6 O59 V6'
_chemical_formula_weight         1782.60

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'
B B 0.0013 0.0007 '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'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   22.3371(10)
_cell_length_b                   12.5753(6)
_cell_length_c                   22.3967(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 116.8640(10)
_cell_angle_gamma                90.00
_cell_volume                     5612.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2484
_exptl_absorpt_coefficient_mu    1.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6877
_exptl_absorpt_correction_T_max  0.7995
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20774
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.10
_reflns_number_total             4958
_reflns_number_gt                4703
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_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)+(0.0795P)²+98.4276P] 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         4958
_refine_ls_number_parameters     467
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0632
_refine_ls_wR_factor_ref         0.1645
_refine_ls_wR_factor_gt          0.1626
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_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
V2 V 0.44560(4) 0.72431(6) 0.47129(4) 0.0101(2) Uani 1 1 d . . .
V3 V 0.49596(4) 0.63393(6) 0.61192(4) 0.0101(2) Uani 1 1 d . . .
V1 V 0.44945(4) 0.59046(6) 0.36056(4) 0.0100(2) Uani 1 1 d . . .
O1 O 0.42020(19) 0.6354(3) 0.28537(17) 0.0225(8) Uani 1 1 d . . .
O1W O 0.5000 0.5000 0.5000 0.40(2) Uani 1 2 d S . .
O2 O 0.6810(2) 0.8540(3) 0.74028(19) 0.0339(11) Uani 1 1 d . . .
O2W O 0.8131(9) 0.664(2) 0.7894(17) 0.050(6) Uani 0.80(14) 1 d P . .
O3 O 0.49388(19) 0.7011(3) 0.67248(18) 0.0222(8) Uani 1 1 d . . .
O3W O 0.7824(3) -0.0712(5) 0.6873(3) 0.0534(14) Uani 1 1 d . . .
O4W O 0.3218(2) 0.0456(4) 0.6699(3) 0.0424(11) Uani 1 1 d . . .
O4 O 0.5996(3) 0.7786(3) 0.3063(2) 0.0326(10) Uani 1 1 d . . .
O5 O 0.41605(18) 0.8440(3) 0.45604(18) 0.0206(8) Uani 1 1 d . . .
O5W O 0.4269(3) 0.8763(4) 0.7031(3) 0.0500(13) Uani 1 1 d . . .
O6 O 0.62462(17) 0.8156(3) 0.62793(16) 0.0145(7) Uani 1 1 d . . .
O7 O 0.53149(16) 0.5110(3) 0.38313(16) 0.0133(7) Uani 1 1 d . . .
O8 O 0.78948(19) 0.2271(3) 0.60130(18) 0.0250(9) Uani 1 1 d . . .
O9 O 0.72375(17) 0.6401(3) 0.55193(17) 0.0174(7) Uani 1 1 d . . .
O10 O 0.58602(16) 0.3478(3) 0.47131(16) 0.0125(7) Uani 1 1 d . . .
O11 O 0.70508(16) 0.3286(3) 0.51574(16) 0.0135(7) Uani 1 1 d . . .
O12 O 0.61056(17) 0.6151(3) 0.36371(17) 0.0154(7) Uani 1 1 d . . .
O13 O 0.67559(16) 0.6726(3) 0.70585(16) 0.0143(7) Uani 1 1 d . . .
O14 O 0.72643(16) 0.3455(3) 0.63034(16) 0.0141(7) Uani 1 1 d . . .
O15 O 0.61002(16) 0.6215(3) 0.47190(16) 0.0115(7) Uani 1 1 d . . .
O16 O 0.69237(16) 0.5034(3) 0.66605(16) 0.0121(7) Uani 1 1 d . . .
O17 O 0.58858(17) 0.7791(3) 0.40445(17) 0.0149(7) Uani 1 1 d . . .
O18 O 0.58164(16) 0.5568(3) 0.64789(16) 0.0123(7) Uani 1 1 d . . .
O19 O 0.59597(16) 0.7922(3) 0.51240(16) 0.0119(7) Uani 1 1 d . . .
O21 O 0.61076(16) 0.3692(3) 0.60256(16) 0.0130(7) Uani 1 1 d . . .
O22 O 0.50080(16) 0.7018(3) 0.42519(16) 0.0126(7) Uani 1 1 d . . .
O23 O 0.52525(16) 0.7200(3) 0.55747(16) 0.0125(7) Uani 1 1 d . . .
O24 O 0.64917(16) 0.4663(3) 0.43686(16) 0.0123(7) Uani 1 1 d . . .
O25 O 0.66088(16) 0.4793(3) 0.54910(15) 0.0119(7) Uani 1 1 d . . .
O26 O 0.63458(16) 0.6427(3) 0.58682(16) 0.0117(7) Uani 1 1 d . . .
B1 B 0.5725(3) 0.7264(4) 0.4540(3) 0.0117(10) Uani 1 1 d . . .
B2 B 0.6471(3) 0.5903(4) 0.6534(3) 0.0111(10) Uani 1 1 d . . .
B3 B 0.6494(3) 0.4050(4) 0.4906(3) 0.0117(10) Uani 1 1 d . . .
B4 B 0.6609(3) 0.7777(4) 0.6912(3) 0.0150(11) Uani 1 1 d . . .
B5 B 0.6600(3) 0.5968(4) 0.5409(3) 0.0117(10) Uani 1 1 d . . .
B6 B 0.5992(3) 0.7216(5) 0.3581(3) 0.0163(11) Uani 1 1 d . . .
B7 B 0.6730(3) 0.4249(4) 0.6148(3) 0.0117(10) Uani 1 1 d . . .
B8 B 0.7392(3) 0.3013(4) 0.5815(3) 0.0137(10) Uani 1 1 d . . .
B9 B 0.5935(3) 0.7458(4) 0.5695(3) 0.0110(10) Uani 1 1 d . . .
B10 B 0.6011(3) 0.5495(4) 0.4128(3) 0.0115(10) Uani 1 1 d . . .
K1 K 0.88325(9) 0.08541(16) 0.70200(9) 0.0527(5) Uani 1 1 d . . .
N1 N 0.4163(3) 0.9815(5) 0.3603(3) 0.0499(16) Uani 1 1 d . . .
H1C H 0.3818 0.9549 0.3244 0.075 Uiso 1 1 calc R . .
H1D H 0.4083 1.0494 0.3653 0.075 Uiso 1 1 calc R . .
H1E H 0.4217 0.9450 0.3964 0.075 Uiso 1 1 calc R . .
N2 N 0.5975(3) 0.9951(5) 0.4097(3) 0.0499(16) Uani 1 1 d . . .
H2C H 0.5939 1.0156 0.3697 0.060 Uiso 1 1 calc R . .
H2D H 0.6036 0.9242 0.4123 0.060 Uiso 1 1 calc R . .
N3 N 0.7175(3) 0.8936(5) 0.5407(3) 0.0499(16) Uani 1 1 d . . .
H3C H 0.7302 0.8747 0.5830 0.075 Uiso 1 1 calc R . .
H3D H 0.7534 0.8974 0.5333 0.075 Uiso 1 1 calc R . .
H3E H 0.6890 0.8455 0.5134 0.075 Uiso 1 1 calc R . .
C1 C 0.4777(4) 0.9735(7) 0.3517(4) 0.0499(18) Uani 1 1 d . . .
H1A H 0.4866 0.8997 0.3459 0.060 Uiso 1 1 calc R . .
H1B H 0.4721 1.0127 0.3122 0.060 Uiso 1 1 calc R . .
C2 C 0.5322(4) 1.0163(7) 0.4094(4) 0.0499(18) Uani 1 1 d . . .
H2A H 0.5324 0.9854 0.4492 0.060 Uiso 1 1 calc R . .
H2B H 0.5262 1.0925 0.4108 0.060 Uiso 1 1 calc R . .
C3 C 0.6597(4) 1.0441(7) 0.4621(4) 0.0499(18) Uani 1 1 d . . .
H3A H 0.6946 1.0389 0.4478 0.060 Uiso 1 1 calc R . .
H3B H 0.6512 1.1191 0.4652 0.060 Uiso 1 1 calc R . .
C4 C 0.6845(4) 0.9977(6) 0.5281(4) 0.0499(18) Uani 1 1 d . . .
H4A H 0.6469 0.9920 0.5385 0.060 Uiso 1 1 calc R . .
H4B H 0.7160 1.0476 0.5598 0.060 Uiso 1 1 calc R . .
O2W' O 0.804(4) 0.635(9) 0.810(7) 0.05(3) Uani 0.20(14) 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
V2 O5 1.617(4) . ?
V2 O23 1.947(3) . ?
V2 O10 1.948(3) 5_666 ?
V2 O22 1.954(3) . ?
V2 O21 1.955(3) 5_666 ?
V2 V1 3.0305(11) . ?
V2 V3 3.0456(11) . ?
V3 O3 1.616(3) . ?
V3 O7 1.942(3) 5_666 ?
V3 O10 1.948(3) 5_666 ?
V3 O23 1.951(3) . ?
V3 O18 1.965(3) . ?
V3 V1 3.0249(11) 5_666 ?
V3 K1 3.8547(19) 4_656 ?
V3 K1 3.921(2) 3_455 ?
V1 O1 1.609(3) . ?
V1 O21 1.937(3) 5_666 ?
V1 O7 1.943(3) . ?
V1 O18 1.956(3) 5_666 ?
V1 O22 1.968(3) . ?
V1 V3 3.0249(11) 5_666 ?
V1 K1 3.866(2) 8_455 ?
O1 K1 3.238(4) 8_455 ?
O2 B4 1.372(7) . ?
O2W O2W' 0.69(17) . ?
O3 K1 3.184(4) 3_455 ?
O3 K1 3.253(4) 4_656 ?
O3W K1 2.896(6) . ?
O4 B6 1.368(7) . ?
O6 B4 1.362(7) . ?
O6 B9 1.464(6) . ?
O7 B10 1.470(6) . ?
O7 V3 1.942(3) 5_666 ?
O8 B8 1.370(7) . ?
O8 K1 2.895(4) . ?
O9 B5 1.439(6) . ?
O10 B3 1.468(6) . ?
O10 V2 1.948(3) 5_666 ?
O10 V3 1.948(3) 5_666 ?
O11 B8 1.361(6) . ?
O11 B3 1.468(6) . ?
O12 B6 1.358(7) . ?
O12 B10 1.464(6) . ?
O12 K1 2.954(4) 7_656 ?
O13 B4 1.365(7) . ?
O13 B2 1.478(6) . ?
O13 K1 3.105(4) 4_656 ?
O14 B8 1.368(6) . ?
O14 B7 1.472(6) . ?
O15 B5 1.474(6) . ?
O15 B1 1.518(6) . ?
O15 B10 1.540(6) . ?
O16 B7 1.425(6) . ?
O16 B2 1.426(6) . ?
O17 B6 1.371(7) . ?
O17 B1 1.469(6) . ?
O18 B2 1.474(6) . ?
O18 V1 1.956(3) 5_666 ?
O18 K1 3.109(4) 4_656 ?
O19 B9 1.429(6) . ?
O19 B1 1.432(6) . ?
O21 B7 1.467(6) . ?
O21 V1 1.937(3) 5_666 ?
O21 V2 1.955(3) 5_666 ?
O22 B1 1.464(6) . ?
O23 B9 1.461(6) . ?
O24 B10 1.420(6) . ?
O24 B3 1.427(6) . ?
O24 K1 2.930(4) 7_656 ?
O25 B5 1.488(6) . ?
O25 B7 1.531(6) . ?
O25 B3 1.534(6) . ?
O26 B5 1.496(6) . ?
O26 B9 1.533(6) . ?
O26 B2 1.535(6) . ?
B10 K1 3.229(5) 7_656 ?
K1 O24 2.930(4) 7_656 ?
K1 O12 2.954(4) 7_656 ?
K1 O13 3.105(4) 4_646 ?
K1 O18 3.109(4) 4_646 ?
K1 O3 3.184(4) 3_545 ?
K1 B10 3.229(5) 7_656 ?
K1 O1 3.238(4) 8_556 ?
K1 O3 3.253(4) 4_646 ?
K1 V3 3.8547(19) 4_646 ?
K1 V1 3.866(2) 8_556 ?
N1 C1 1.472(10) . ?
N1 H1C 0.8900 . ?
N1 H1D 0.8900 . ?
N1 H1E 0.8900 . ?
N2 C2 1.480(10) . ?
N2 C3 1.488(10) . ?
N2 H2C 0.9000 . ?
N2 H2D 0.9000 . ?
N3 C4 1.466(10) . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
C1 C2 1.422(11) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.447(11) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?

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
O5 V2 O23 109.78(17) . . ?
O5 V2 O10 109.72(17) . 5_666 ?
O23 V2 O10 76.95(13) . 5_666 ?
O5 V2 O22 108.53(17) . . ?
O23 V2 O22 90.44(14) . . ?
O10 V2 O22 141.75(14) 5_666 . ?
O5 V2 O21 109.63(17) . 5_666 ?
O23 V2 O21 140.59(14) . 5_666 ?
O10 V2 O21 89.52(14) 5_666 5_666 ?
O22 V2 O21 77.57(14) . 5_666 ?
O5 V2 V1 120.27(13) . . ?
O23 V2 V1 116.40(10) . . ?
O10 V2 V1 115.76(10) 5_666 . ?
O22 V2 V1 39.57(10) . . ?
O21 V2 V1 38.65(10) 5_666 . ?
O5 V2 V3 119.38(13) . . ?
O23 V2 V3 38.68(10) . . ?
O10 V2 V3 38.59(10) 5_666 . ?
O22 V2 V3 117.79(10) . . ?
O21 V2 V3 116.49(10) 5_666 . ?
V1 V2 V3 120.35(3) . . ?
O3 V3 O7 108.24(17) . 5_666 ?
O3 V3 O10 111.72(17) . 5_666 ?
O7 V3 O10 88.92(14) 5_666 5_666 ?
O3 V3 O23 112.30(18) . . ?
O7 V3 O23 139.45(14) 5_666 . ?
O10 V3 O23 76.83(13) 5_666 . ?
O3 V3 O18 107.82(17) . . ?
O7 V3 O18 77.71(14) 5_666 . ?
O10 V3 O18 140.44(14) 5_666 . ?
O23 V3 O18 89.46(14) . . ?
O3 V3 V1 118.58(14) . 5_666 ?
O7 V3 V1 38.87(10) 5_666 5_666 ?
O10 V3 V1 115.04(10) 5_666 5_666 ?
O23 V3 V1 115.25(10) . 5_666 ?
O18 V3 V1 39.41(10) . 5_666 ?
O3 V3 V2 122.38(14) . . ?
O7 V3 V2 115.51(10) 5_666 . ?
O10 V3 V2 38.57(10) 5_666 . ?
O23 V3 V2 38.57(9) . . ?
O18 V3 V2 116.39(10) . . ?
V1 V3 V2 119.04(3) 5_666 . ?
O3 V3 K1 56.42(14) . 4_656 ?
O7 V3 K1 82.79(10) 5_666 4_656 ?
O10 V3 K1 161.66(10) 5_666 4_656 ?
O23 V3 K1 119.67(10) . 4_656 ?
O18 V3 K1 53.29(10) . 4_656 ?
V1 V3 K1 67.12(4) 5_666 4_656 ?
V2 V3 K1 158.15(4) . 4_656 ?
O3 V3 K1 51.75(14) . 3_455 ?
O7 V3 K1 62.09(10) 5_666 3_455 ?
O10 V3 K1 88.07(10) 5_666 3_455 ?
O23 V3 K1 151.95(10) . 3_455 ?
O18 V3 K1 116.44(10) . 3_455 ?
V1 V3 K1 92.49(4) 5_666 3_455 ?
V2 V3 K1 124.56(4) . 3_455 ?
K1 V3 K1 73.59(5) 4_656 3_455 ?
O1 V1 O21 108.82(17) . 5_666 ?
O1 V1 O7 110.01(17) . . ?
O21 V1 O7 141.14(14) 5_666 . ?
O1 V1 O18 105.82(17) . 5_666 ?
O21 V1 O18 90.25(14) 5_666 5_666 ?
O7 V1 O18 77.91(14) . 5_666 ?
O1 V1 O22 110.24(17) . . ?
O21 V1 O22 77.66(14) 5_666 . ?
O7 V1 O22 90.39(14) . . ?
O18 V1 O22 143.93(14) 5_666 . ?
O1 V1 V3 118.46(14) . 5_666 ?
O21 V1 V3 116.80(11) 5_666 5_666 ?
O7 V1 V3 38.87(10) . 5_666 ?
O18 V1 V3 39.62(9) 5_666 5_666 ?
O22 V1 V3 117.83(10) . 5_666 ?
O1 V1 V2 120.89(14) . . ?
O21 V1 V2 39.08(10) 5_666 . ?
O7 V1 V2 116.41(10) . . ?
O18 V1 V2 117.69(10) 5_666 . ?
O22 V1 V2 39.23(10) . . ?
V3 V1 V2 120.62(3) 5_666 . ?
O1 V1 K1 55.49(14) . 8_455 ?
O21 V1 K1 119.37(10) 5_666 8_455 ?
O7 V1 K1 82.48(10) . 8_455 ?
O18 V1 K1 52.98(10) 5_666 8_455 ?
O22 V1 K1 159.53(10) . 8_455 ?
V3 V1 K1 66.74(4) 5_666 8_455 ?
V2 V1 K1 158.28(4) . 8_455 ?
V1 O1 K1 100.35(17) . 8_455 ?
V3 O3 K1 104.76(17) . 3_455 ?
V3 O3 K1 99.12(16) . 4_656 ?
K1 O3 K1 92.70(11) 3_455 4_656 ?
B4 O6 B9 122.7(4) . . ?
B10 O7 V3 125.5(3) . 5_666 ?
B10 O7 V1 129.0(3) . . ?
V3 O7 V1 102.26(15) 5_666 . ?
B8 O8 K1 150.5(3) . . ?
B3 O10 V2 128.5(3) . 5_666 ?
B3 O10 V3 126.0(3) . 5_666 ?
V2 O10 V3 102.83(15) 5_666 5_666 ?
B8 O11 B3 122.9(4) . . ?
B6 O12 B10 122.7(4) . . ?
B6 O12 K1 147.6(3) . 7_656 ?
B10 O12 K1 87.0(3) . 7_656 ?
B4 O13 B2 121.1(4) . . ?
B4 O13 K1 111.9(3) . 4_656 ?
B2 O13 K1 97.0(3) . 4_656 ?
B8 O14 B7 121.8(4) . . ?
B5 O15 B1 121.8(4) . . ?
B5 O15 B10 121.4(4) . . ?
B1 O15 B10 116.2(3) . . ?
B7 O16 B2 116.1(4) . . ?
B6 O17 B1 121.2(4) . . ?
B2 O18 V1 125.0(3) . 5_666 ?
B2 O18 V3 129.8(3) . . ?
V1 O18 V3 100.97(15) 5_666 . ?
B2 O18 K1 97.0(2) . 4_656 ?
V1 O18 K1 96.85(12) 5_666 4_656 ?
V3 O18 K1 96.27(12) . 4_656 ?
B9 O19 B1 115.8(4) . . ?
B7 O21 V1 125.2(3) . 5_666 ?
B7 O21 V2 129.7(3) . 5_666 ?
V1 O21 V2 102.27(15) 5_666 5_666 ?
B1 O22 V2 124.2(3) . . ?
B1 O22 V1 129.2(3) . . ?
V2 O22 V1 101.21(15) . . ?
B9 O23 V2 125.9(3) . . ?
B9 O23 V3 128.7(3) . . ?
V2 O23 V3 102.75(15) . . ?
B10 O24 B3 115.6(4) . . ?
B10 O24 K1 88.8(2) . 7_656 ?
B3 O24 K1 132.9(3) . 7_656 ?
B5 O25 B7 123.2(4) . . ?
B5 O25 B3 120.8(4) . . ?
B7 O25 B3 116.0(4) . . ?
B5 O26 B9 121.4(4) . . ?
B5 O26 B2 122.8(4) . . ?
B9 O26 B2 115.8(3) . . ?
O19 B1 O22 113.6(4) . . ?
O19 B1 O17 108.4(4) . . ?
O22 B1 O17 110.8(4) . . ?
O19 B1 O15 109.3(4) . . ?
O22 B1 O15 107.2(4) . . ?
O17 B1 O15 107.3(4) . . ?
O16 B2 O18 112.6(4) . . ?
O16 B2 O13 111.5(4) . . ?
O18 B2 O13 108.7(4) . . ?
O16 B2 O26 109.0(4) . . ?
O18 B2 O26 107.6(4) . . ?
O13 B2 O26 107.2(4) . . ?
O24 B3 O10 112.4(4) . . ?
O24 B3 O11 110.9(4) . . ?
O10 B3 O11 109.3(4) . . ?
O24 B3 O25 109.1(4) . . ?
O10 B3 O25 108.5(4) . . ?
O11 B3 O25 106.5(4) . . ?
O6 B4 O13 123.6(4) . . ?
O6 B4 O2 114.5(5) . . ?
O13 B4 O2 121.9(5) . . ?
O9 B5 O15 108.8(4) . . ?
O9 B5 O25 113.4(4) . . ?
O15 B5 O25 107.4(4) . . ?
O9 B5 O26 112.9(4) . . ?
O15 B5 O26 107.3(4) . . ?
O25 B5 O26 106.7(4) . . ?
O12 B6 O4 121.5(5) . . ?
O12 B6 O17 122.7(5) . . ?
O4 B6 O17 115.8(5) . . ?
O16 B7 O21 113.5(4) . . ?
O16 B7 O14 111.1(4) . . ?
O21 B7 O14 108.6(4) . . ?
O16 B7 O25 108.8(4) . . ?
O21 B7 O25 107.0(4) . . ?
O14 B7 O25 107.6(4) . . ?
O11 B8 O14 123.1(4) . . ?
O11 B8 O8 119.9(4) . . ?
O14 B8 O8 117.0(4) . . ?
O19 B9 O23 112.6(4) . . ?
O19 B9 O6 111.2(4) . . ?
O23 B9 O6 109.4(4) . . ?
O19 B9 O26 108.2(4) . . ?
O23 B9 O26 108.3(4) . . ?
O6 B9 O26 107.0(4) . . ?
O24 B10 O12 111.1(4) . . ?
O24 B10 O7 113.1(4) . . ?
O12 B10 O7 109.2(4) . . ?
O24 B10 O15 109.0(4) . . ?
O12 B10 O15 108.0(4) . . ?
O7 B10 O15 106.3(4) . . ?
O24 B10 K1 65.1(2) . 7_656 ?
O12 B10 K1 66.0(2) . 7_656 ?
O7 B10 K1 86.6(3) . 7_656 ?
O15 B10 K1 167.1(3) . 7_656 ?
O8 K1 O3W 94.50(15) . . ?
O8 K1 O24 64.20(10) . 7_656 ?
O3W K1 O24 85.55(13) . 7_656 ?
O8 K1 O12 108.52(11) . 7_656 ?
O3W K1 O12 64.68(14) . 7_656 ?
O24 K1 O12 47.67(9) 7_656 7_656 ?
O8 K1 O13 85.74(11) . 4_646 ?
O3W K1 O13 76.97(14) . 4_646 ?
O24 K1 O13 143.91(11) 7_656 4_646 ?
O12 K1 O13 139.62(11) 7_656 4_646 ?
O8 K1 O18 130.84(11) . 4_646 ?
O3W K1 O18 81.20(13) . 4_646 ?
O24 K1 O18 160.54(12) 7_656 4_646 ?
O12 K1 O18 113.21(11) 7_656 4_646 ?
O13 K1 O18 45.40(9) 4_646 4_646 ?
O8 K1 O3 85.02(12) . 3_545 ?
O3W K1 O3 157.49(14) . 3_545 ?
O24 K1 O3 73.96(10) 7_656 3_545 ?
O12 K1 O3 94.08(10) 7_656 3_545 ?
O13 K1 O3 125.31(11) 4_646 3_545 ?
O18 K1 O3 115.93(10) 4_646 3_545 ?
O8 K1 B10 90.22(13) . 7_656 ?
O3W K1 B10 84.88(15) . 7_656 ?
O24 K1 B10 26.09(11) 7_656 7_656 ?
O12 K1 B10 26.92(11) 7_656 7_656 ?
O13 K1 B10 161.01(13) 4_646 7_656 ?
O18 K1 B10 137.31(13) 4_646 7_656 ?
O3 K1 B10 72.63(12) 3_545 7_656 ?
O8 K1 O1 152.05(13) . 8_556 ?
O3W K1 O1 57.65(14) . 8_556 ?
O24 K1 O1 107.36(11) 7_656 8_556 ?
O12 K1 O1 59.88(10) 7_656 8_556 ?
O13 K1 O1 89.65(10) 4_646 8_556 ?
O18 K1 O1 53.35(9) 4_646 8_556 ?
O3 K1 O1 119.48(11) 3_545 8_556 ?
B10 K1 O1 85.26(12) 7_656 8_556 ?
O8 K1 O3 115.39(12) . 4_646 ?
O3W K1 O3 135.34(13) . 4_646 ?
O24 K1 O3 136.38(11) 7_656 4_646 ?
O12 K1 O3 126.96(12) 7_656 4_646 ?
O13 K1 O3 73.31(10) 4_646 4_646 ?
O18 K1 O3 54.21(9) 4_646 4_646 ?
O3 K1 O3 62.88(12) 3_545 4_646 ?
B10 K1 O3 124.80(13) 7_656 4_646 ?
O1 K1 O3 89.40(10) 8_556 4_646 ?
O8 K1 V3 130.65(10) . 4_646 ?
O3W K1 V3 111.02(11) . 4_646 ?
O24 K1 V3 154.07(9) 7_656 4_646 ?
O12 K1 V3 120.42(9) 7_656 4_646 ?
O13 K1 V3 61.65(7) 4_646 4_646 ?
O18 K1 V3 30.44(6) 4_646 4_646 ?
O3 K1 V3 85.55(8) 3_545 4_646 ?
B10 K1 V3 132.02(11) 7_656 4_646 ?
O1 K1 V3 68.95(7) 8_556 4_646 ?
O3 K1 V3 24.46(6) 4_646 4_646 ?
O8 K1 V1 155.46(10) . 8_556 ?
O3W K1 V1 70.75(11) . 8_556 ?
O24 K1 V1 131.06(9) 7_656 8_556 ?
O12 K1 V1 83.38(8) 7_656 8_556 ?
O13 K1 V1 72.10(7) 4_646 8_556 ?
O18 K1 V1 30.16(6) 4_646 8_556 ?
O3 K1 V1 116.21(9) 3_545 8_556 ?
B10 K1 V1 107.26(11) 7_656 8_556 ?
O1 K1 V1 24.16(6) 8_556 8_556 ?
O3 K1 V1 68.83(7) 4_646 8_556 ?
V3 K1 V1 46.13(3) 4_646 8_556 ?
C1 N1 H1C 109.5 . . ?
C1 N1 H1D 109.5 . . ?
H1C N1 H1D 109.5 . . ?
C1 N1 H1E 109.5 . . ?
H1C N1 H1E 109.5 . . ?
H1D N1 H1E 109.5 . . ?
C2 N2 C3 119.7(6) . . ?
C2 N2 H2C 107.4 . . ?
C3 N2 H2C 107.4 . . ?
C2 N2 H2D 107.4 . . ?
C3 N2 H2D 107.4 . . ?
H2C N2 H2D 106.9 . . ?
C4 N3 H3C 109.5 . . ?
C4 N3 H3D 109.5 . . ?
H3C N3 H3D 109.5 . . ?
C4 N3 H3E 109.5 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C2 C1 N1 108.7(7) . . ?
C2 C1 H1A 109.9 . . ?
N1 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
N1 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
C1 C2 N2 111.9(7) . . ?
C1 C2 H2A 109.2 . . ?
N2 C2 H2A 109.2 . . ?
C1 C2 H2B 109.2 . . ?
N2 C2 H2B 109.2 . . ?
H2A C2 H2B 107.9 . . ?
C4 C3 N2 115.4(7) . . ?
C4 C3 H3A 108.4 . . ?
N2 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
N2 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
C3 C4 N3 118.9(7) . . ?
C3 C4 H4A 107.6 . . ?
N3 C4 H4A 107.6 . . ?
C3 C4 H4B 107.6 . . ?
N3 C4 H4B 107.6 . . ?
H4A C4 H4B 107.0 . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.725
_refine_diff_density_min         -1.311
_refine_diff_density_rms         0.162
_database_code_depnum_ccdc_archive 'CCDC 968043'
