# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2013


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#                                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_1
_database_code_depnum_ccdc_archive 'CCDC 927385'
#TrackingRef '1.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '3(C4 H17 B6 Cu N3 O21 V4),4(H3 O),6.5(H2 O)'
_chemical_formula_sum            'C12 H76 B18 Cu3 N9 O73.5 V12 '
_chemical_formula_weight         2519.27
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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Cubic
_symmetry_space_group_name_H-M   'I a -3'
_symmetry_space_group_name_Hall  '-I 2b 2c 3'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1, -x+1, -y+1/2'
'-z+1, -x+1/2, y+1'
'-z+1/2, x+1, -y+1'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1, -x+1'
'y+1, -z+1, -x+1/2'
'-y+1, -z+1/2, x+1'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
'-z, -x, -y'
'-z-1/2, x-1/2, y'
'z-1/2, x, -y-1/2'
'z, -x-1/2, y-1/2'
'-y, -z, -x'
'y, -z-1/2, x-1/2'
'-y-1/2, z-1/2, x'
'y-1/2, z, -x-1/2'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'
'-z+1/2, -x+1/2, -y+1/2'
'-z, x, y+1/2'
'z, x+1/2, -y'
'z+1/2, -x, y'
'-y+1/2, -z+1/2, -x+1/2'
'y+1/2, -z, x'
'-y, z, x+1/2'
'y, z+1/2, -x'
_cell_length_a                   27.618(3)
_cell_length_b                   27.618(3)
_cell_length_c                   27.618(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     21066(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             9768
_exptl_absorpt_coefficient_mu    1.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7164
_exptl_absorpt_correction_T_max  0.8349
_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       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            42879
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         25.09
_reflns_number_total             3124
_reflns_number_gt                2283
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0808P)^2^+200.6589P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3124
_refine_ls_number_parameters     255
_refine_ls_number_restraints     271
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0559
_refine_ls_wR_factor_ref         0.1888
_refine_ls_wR_factor_gt          0.1488
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.165
_refine_ls_shift/su_max          0.002
_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
Cu1 Cu 0.57090(7) 0.24830(6) 0.45839(7) 0.0517(5) Uani 0.50 1 d PU . .
V1 V 0.49478(3) 0.44194(3) 0.38698(3) 0.0269(3) Uani 1 1 d U . .
V2 V 0.54457(3) 0.37867(3) 0.45969(3) 0.0260(3) Uani 1 1 d U . .
B1 B 0.6022(3) 0.4573(2) 0.3075(2) 0.0321(14) Uani 1 1 d U . .
B2 B 0.6055(2) 0.4475(2) 0.3963(2) 0.0273(13) Uani 1 1 d U . .
B3 B 0.6409(2) 0.4313(2) 0.4769(2) 0.0257(13) Uani 1 1 d U . .
O1 O 0.55635(16) 0.32692(15) 0.43623(16) 0.0407(10) Uani 1 1 d U . .
O2 O 0.47883(14) 0.39666(14) 0.43699(14) 0.0306(9) Uani 1 1 d U . .
O2W O 0.5000 0.2500 0.4904(3) 0.070(2) Uani 1 2 d SU . .
O1W O 0.5000 0.5000 0.5000 0.138(6) Uani 1 6 d SU . .
O3 O 0.60322(13) 0.39792(13) 0.49780(13) 0.0254(8) Uani 1 1 d U . .
O4W O 0.5754(7) 0.3349(6) 0.3237(6) 0.104(5) Uani 0.50 1 d PU . .
O4 O 0.50684(13) 0.37143(14) 0.51844(13) 0.0291(8) Uani 1 1 d U . .
O5 O 0.48982(16) 0.41392(16) 0.33645(15) 0.0403(10) Uani 1 1 d U . .
O6 O 0.55856(14) 0.42901(14) 0.41355(13) 0.0302(9) Uani 1 1 d U . .
O7 O 0.6115(2) 0.43804(17) 0.26272(16) 0.0483(12) Uani 1 1 d U . .
H7 H 0.5975 0.4540 0.2420 0.073 Uiso 1 1 calc R . .
O8 O 0.61457(15) 0.43097(14) 0.34666(14) 0.0332(9) Uani 1 1 d U . .
O9 O 0.64419(13) 0.42948(14) 0.42604(13) 0.0280(8) Uani 1 1 d U . .
O10 O 0.68861(13) 0.41777(14) 0.49736(14) 0.0299(9) Uani 1 1 d U . .
N3 N 0.6143(4) 0.2703(4) 0.5157(5) 0.052(2) Uani 0.50 1 d PDU . .
H3C H 0.6020 0.2970 0.5297 0.062 Uiso 0.50 1 calc PR . .
H3D H 0.6165 0.2468 0.5381 0.062 Uiso 0.50 1 calc PR . .
N1 N 0.5427(5) 0.2116(6) 0.3943(5) 0.072(3) Uani 0.50 1 d PDU . .
H1C H 0.5342 0.1810 0.4013 0.086 Uiso 0.50 1 calc PR . .
H1D H 0.5167 0.2273 0.3825 0.086 Uiso 0.50 1 calc PR . .
N2 N 0.6322(5) 0.2489(6) 0.4205(5) 0.075(2) Uani 0.50 1 d PDU . .
H2C H 0.6333 0.2781 0.4053 0.090 Uiso 0.50 1 calc PR . .
C3 C 0.6704(6) 0.2492(7) 0.4548(6) 0.076(3) Uani 0.50 1 d PDU . .
H3A H 0.6999 0.2599 0.4390 0.091 Uiso 0.50 1 calc PR . .
H3B H 0.6757 0.2164 0.4664 0.091 Uiso 0.50 1 calc PR . .
C4 C 0.6605(6) 0.2803(6) 0.4954(7) 0.075(3) Uani 0.50 1 d PDU . .
H4A H 0.6852 0.2757 0.5199 0.090 Uiso 0.50 1 calc PR . .
H4B H 0.6617 0.3138 0.4849 0.090 Uiso 0.50 1 calc PR . .
C2 C 0.6284(7) 0.2134(7) 0.3831(7) 0.079(3) Uani 0.50 1 d PDU . .
H2A H 0.6351 0.1817 0.3968 0.095 Uiso 0.50 1 calc PR . .
H2B H 0.6528 0.2199 0.3587 0.095 Uiso 0.50 1 calc PR . .
C1 C 0.5816(6) 0.2126(8) 0.3606(7) 0.083(3) Uani 0.50 1 d PDU . .
H1A H 0.5783 0.2410 0.3402 0.100 Uiso 0.50 1 calc PR . .
H1B H 0.5794 0.1843 0.3399 0.100 Uiso 0.50 1 calc PR . .
O5W O 0.6198(3) 0.3020(4) 0.5913(4) 0.053(3) Uani 0.50 1 d PU . .
O3WA O 0.6791(7) 0.3438(7) 0.3816(8) 0.079(5) Uani 0.35 1 d PU . .
O3WB O 0.6971(16) 0.3665(17) 0.3564(17) 0.074(11) Uani 0.15 1 d PU . .
O6W O 0.730(2) 0.230(2) 0.270(2) 0.23(5) Uiso 0.25 3 d SP . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0605(11) 0.0385(9) 0.0561(11) -0.0028(8) 0.0171(9) -0.0019(8)
V1 0.0279(5) 0.0280(5) 0.0249(5) -0.0006(4) -0.0011(4) 0.0005(4)
V2 0.0284(5) 0.0244(5) 0.0251(5) -0.0001(4) 0.0026(4) -0.0005(4)
B1 0.036(3) 0.034(3) 0.025(3) 0.002(3) 0.006(3) 0.007(3)
B2 0.025(3) 0.028(3) 0.028(3) 0.004(2) 0.001(2) -0.002(2)
B3 0.023(3) 0.025(3) 0.029(3) 0.005(2) 0.000(2) 0.005(2)
O1 0.047(3) 0.028(2) 0.047(3) -0.0057(19) 0.009(2) 0.0016(18)
O2 0.030(2) 0.035(2) 0.027(2) 0.0025(16) 0.0007(16) -0.0011(16)
O2W 0.090(5) 0.052(4) 0.067(5) 0.000 0.000 -0.004(4)
O1W 0.138(6) 0.138(6) 0.138(6) -0.006(5) -0.006(5) -0.006(5)
O3 0.0246(18) 0.0271(19) 0.0247(18) 0.0017(15) -0.0005(15) 0.0006(15)
O4W 0.122(9) 0.087(8) 0.104(8) -0.013(7) 0.019(7) 0.000(7)
O4 0.0259(19) 0.034(2) 0.0270(19) 0.0034(16) 0.0013(15) 0.0025(16)
O5 0.050(3) 0.042(2) 0.029(2) -0.0053(18) 0.0010(19) 0.002(2)
O6 0.027(2) 0.035(2) 0.028(2) 0.0073(16) -0.0017(16) -0.0010(16)
O7 0.076(3) 0.041(3) 0.028(2) -0.0016(19) 0.001(2) 0.022(2)
O8 0.045(2) 0.028(2) 0.026(2) 0.0010(16) 0.0005(17) 0.0081(18)
O9 0.0257(19) 0.033(2) 0.0255(19) 0.0032(16) 0.0024(15) 0.0045(16)
O10 0.0219(19) 0.035(2) 0.033(2) 0.0049(17) -0.0008(16) 0.0002(16)
N3 0.059(5) 0.036(4) 0.060(5) -0.001(4) 0.015(4) 0.012(4)
N1 0.079(5) 0.068(5) 0.068(5) 0.009(4) 0.024(4) 0.009(5)
N2 0.080(4) 0.065(4) 0.080(4) 0.000(4) 0.017(4) 0.008(4)
C3 0.079(5) 0.068(5) 0.082(5) -0.002(4) 0.017(4) 0.006(4)
C4 0.077(5) 0.065(5) 0.083(5) -0.005(4) 0.009(5) 0.006(4)
C2 0.083(5) 0.075(5) 0.079(5) -0.004(4) 0.018(4) 0.006(4)
C1 0.091(5) 0.079(5) 0.081(5) 0.000(5) 0.017(5) 0.007(5)
O5W 0.037(4) 0.047(5) 0.077(6) 0.026(5) -0.011(4) 0.009(4)
O3WA 0.081(9) 0.065(8) 0.091(9) -0.012(7) -0.003(7) 0.017(7)
O3WB 0.074(14) 0.071(14) 0.077(14) -0.015(9) -0.004(9) 0.014(9)
_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
Cu1 N2 1.990(15) . ?
Cu1 N3 2.076(13) . ?
Cu1 O2W 2.149(4) . ?
Cu1 N1 2.182(16) . ?
Cu1 O1 2.292(5) . ?
V1 O5 1.602(4) . ?
V1 O2 1.912(4) 5 ?
V1 O2 1.915(4) . ?
V1 O6 1.941(4) . ?
V1 O4 1.955(4) 5 ?
V1 V2 2.9962(14) . ?
V1 V2 3.0041(14) 5 ?
V2 O1 1.603(4) . ?
V2 O6 1.925(4) . ?
V2 O4 1.939(4) . ?
V2 O2 1.984(4) . ?
V2 O3 2.003(4) . ?
V2 V1 3.0041(13) 9 ?
B1 O8 1.347(8) . ?
B1 O7 1.370(8) . ?
B1 O10 1.373(8) 33_666 ?
B2 O9 1.436(7) . ?
B2 O8 1.466(8) . ?
B2 O6 1.473(7) . ?
B2 O3 1.514(7) 33_666 ?
B3 O9 1.410(7) . ?
B3 O10 1.480(7) . ?
B3 O4 1.499(7) 33_666 ?
B3 O3 1.505(7) . ?
O2 V1 1.912(4) 9 ?
O2W Cu1 2.149(4) 14_554 ?
O3 B2 1.514(7) 29_666 ?
O4 B3 1.499(7) 29_666 ?
O4 V1 1.955(4) 9 ?
O7 H7 0.8200 . ?
O10 B1 1.373(8) 29_666 ?
N3 C4 1.420(13) . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N1 C1 1.423(13) . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
N2 C3 1.419(13) . ?
N2 C2 1.426(13) . ?
N2 H2C 0.9100 . ?
C3 C4 1.439(19) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C2 C1 1.436(19) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
O5W O3WB 1.34(4) 29_666 ?
O3WA O3WB 1.06(5) . ?
O3WB O5W 1.34(4) 33_666 ?
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
N2 Cu1 N3 84.7(5) . . ?
N2 Cu1 O2W 172.4(5) . . ?
N3 Cu1 O2W 101.9(4) . . ?
N2 Cu1 N1 83.2(5) . . ?
N3 Cu1 N1 163.7(5) . . ?
O2W Cu1 N1 91.1(4) . . ?
N2 Cu1 O1 90.0(5) . . ?
N3 Cu1 O1 91.5(3) . . ?
O2W Cu1 O1 85.97(15) . . ?
N1 Cu1 O1 99.2(4) . . ?
O5 V1 O2 107.9(2) . 5 ?
O5 V1 O2 107.1(2) . . ?
O2 V1 O2 93.2(2) 5 . ?
O5 V1 O6 108.5(2) . . ?
O2 V1 O6 143.37(17) 5 . ?
O2 V1 O6 79.39(16) . . ?
O5 V1 O4 106.3(2) . 5 ?
O2 V1 O4 79.71(16) 5 5 ?
O2 V1 O4 146.52(17) . 5 ?
O6 V1 O4 87.04(16) . 5 ?
O5 V1 V2 109.96(16) . . ?
O2 V1 V2 126.88(13) 5 . ?
O2 V1 V2 40.64(12) . . ?
O6 V1 V2 39.01(11) . . ?
O4 V1 V2 121.89(12) 5 . ?
O5 V1 V2 111.21(16) . 5 ?
O2 V1 V2 40.44(12) 5 5 ?
O2 V1 V2 126.67(12) . 5 ?
O6 V1 V2 119.68(12) . 5 ?
O4 V1 V2 39.31(11) 5 5 ?
V2 V1 V2 138.55(5) . 5 ?
O1 V2 O6 109.6(2) . . ?
O1 V2 O4 110.8(2) . . ?
O6 V2 O4 137.42(17) . . ?
O1 V2 O2 106.3(2) . . ?
O6 V2 O2 78.09(16) . . ?
O4 V2 O2 78.37(16) . . ?
O1 V2 O3 106.6(2) . . ?
O6 V2 O3 89.65(16) . . ?
O4 V2 O3 91.28(16) . . ?
O2 V2 O3 147.08(16) . . ?
O1 V2 V1 110.01(17) . . ?
O6 V2 V1 39.40(11) . . ?
O4 V2 V1 111.99(12) . . ?
O2 V2 V1 38.94(11) . . ?
O3 V2 V1 124.64(11) . . ?
O1 V2 V1 112.97(17) . 9 ?
O6 V2 V1 110.34(12) . 9 ?
O4 V2 V1 39.72(11) . 9 ?
O2 V2 V1 38.69(11) . 9 ?
O3 V2 V1 124.96(11) . 9 ?
V1 V2 V1 74.85(4) . 9 ?
O8 B1 O7 117.9(5) . . ?
O8 B1 O10 122.1(5) . 33_666 ?
O7 B1 O10 120.0(5) . 33_666 ?
O9 B2 O8 107.5(5) . . ?
O9 B2 O6 110.5(5) . . ?
O8 B2 O6 110.2(5) . . ?
O9 B2 O3 112.8(5) . 33_666 ?
O8 B2 O3 109.2(4) . 33_666 ?
O6 B2 O3 106.7(4) . 33_666 ?
O9 B3 O10 108.3(4) . . ?
O9 B3 O4 110.2(4) . 33_666 ?
O10 B3 O4 108.8(5) . 33_666 ?
O9 B3 O3 113.8(5) . . ?
O10 B3 O3 108.4(4) . . ?
O4 B3 O3 107.1(4) 33_666 . ?
V2 O1 Cu1 140.6(3) . . ?
V1 O2 V1 144.7(2) 9 . ?
V1 O2 V2 100.88(17) 9 . ?
V1 O2 V2 100.43(17) . . ?
Cu1 O2W Cu1 131.3(4) 14_554 . ?
B3 O3 B2 114.5(4) . 29_666 ?
B3 O3 V2 121.4(3) . . ?
B2 O3 V2 121.0(3) 29_666 . ?
B3 O4 V2 129.7(3) 29_666 . ?
B3 O4 V1 129.3(3) 29_666 9 ?
V2 O4 V1 100.97(17) . 9 ?
B2 O6 V2 129.9(3) . . ?
B2 O6 V1 127.8(3) . . ?
V2 O6 V1 101.60(18) . . ?
B1 O7 H7 109.5 . . ?
B1 O8 B2 122.7(5) . . ?
B3 O9 B2 120.7(4) . . ?
B1 O10 B3 121.2(4) 29_666 . ?
C4 N3 Cu1 105.9(10) . . ?
C4 N3 H3C 110.6 . . ?
Cu1 N3 H3C 110.6 . . ?
C4 N3 H3D 110.6 . . ?
Cu1 N3 H3D 110.6 . . ?
H3C N3 H3D 108.7 . . ?
C1 N1 Cu1 104.6(12) . . ?
C1 N1 H1C 110.8 . . ?
Cu1 N1 H1C 110.8 . . ?
C1 N1 H1D 110.8 . . ?
Cu1 N1 H1D 110.8 . . ?
H1C N1 H1D 108.9 . . ?
C3 N2 C2 122.7(16) . . ?
C3 N2 Cu1 106.4(11) . . ?
C2 N2 Cu1 108.2(11) . . ?
C3 N2 H2C 106.2 . . ?
C2 N2 H2C 106.2 . . ?
Cu1 N2 H2C 106.2 . . ?
N2 C3 C4 112.5(15) . . ?
N2 C3 H3A 109.1 . . ?
C4 C3 H3A 109.1 . . ?
N2 C3 H3B 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
N3 C4 C3 111.3(14) . . ?
N3 C4 H4A 109.4 . . ?
C3 C4 H4A 109.4 . . ?
N3 C4 H4B 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
N2 C2 C1 113.0(16) . . ?
N2 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
N2 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N1 C1 C2 113.3(16) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
O3WA O3WB O5W 102(4) . 33_666 ?
_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.128


data_3
_database_code_depnum_ccdc_archive 'CCDC 927386'
#TrackingRef '3.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(B18 H30 Na6 O73 V12), 2(C4 H16 N3)'
_chemical_formula_sum            'C8 H62 B18 N6 Na6 O73 V12'
_chemical_formula_weight         2354.39
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   14.083(3)
_cell_length_b                   17.226(3)
_cell_length_c                   18.264(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 128.755(19)
_cell_angle_gamma                90.00
_cell_volume                     3455.2(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2292
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7132
_exptl_absorpt_correction_T_max  0.8196
_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       \w
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19293
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0204
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.85
_diffrn_reflns_theta_max         25.10
_reflns_number_total             6148
_reflns_number_gt                5589
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0527P)^2^+6.7574P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6148
_refine_ls_number_parameters     556
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0313
_refine_ls_wR_factor_ref         0.0953
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_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 0.61147(5) 0.38815(3) 0.71773(3) 0.01293(13) Uani 1 1 d . . .
V2 V 0.78863(4) 0.42921(3) 0.68457(3) 0.01188(12) Uani 1 1 d . . .
V3 V 0.80245(4) 0.52796(3) 0.55437(3) 0.01236(12) Uani 1 1 d . . .
V4 V 0.65111(4) 0.38959(3) 0.43649(3) 0.01250(12) Uani 1 1 d . . .
V5 V 0.52642(4) 0.29629(3) 0.54451(3) 0.01252(12) Uani 1 1 d . . .
V6 V 0.40118(5) 0.32877(3) 0.34256(3) 0.01245(12) Uani 1 1 d . . .
Na1 Na 1.28545(17) 0.49986(11) 1.00343(15) 0.0530(5) Uani 1 1 d . . .
Na2 Na 0.74358(17) 0.63636(10) 0.28382(13) 0.0439(4) Uani 1 1 d . . .
Na3 Na 0.48929(14) 0.78148(8) 0.26537(10) 0.0318(3) Uani 1 1 d . . .
O1 O 0.5510(2) 0.20374(13) 0.56705(17) 0.0250(5) Uani 1 1 d . . .
O2 O 0.7174(2) 0.33369(13) 0.40964(16) 0.0233(5) Uani 1 1 d . . .
O2W O 1.3848(5) 0.6218(3) 1.0631(3) 0.0858(14) Uani 1 1 d . . .
O3 O 0.9217(2) 0.39097(13) 0.76722(15) 0.0198(5) Uani 1 1 d . . .
O3W O 1.4124(4) 0.4390(3) 0.9705(3) 0.0817(13) Uani 1 1 d . . .
O4 O 0.3852(2) 0.24978(13) 0.28788(16) 0.0224(5) Uani 1 1 d . . .
O4W O 0.9351(3) 0.58598(17) 0.4315(2) 0.0426(7) Uani 1 1 d . . .
O5 O 0.24522(18) 0.39135(12) 0.25333(14) 0.0127(4) Uani 1 1 d . . .
O5W O 1.1668(3) 0.51689(18) 0.8335(2) 0.0487(8) Uani 1 1 d . . .
O6 O 0.66702(19) 0.35307(12) 0.64864(14) 0.0161(4) Uani 1 1 d . . .
O7 O 0.46742(19) 0.33638(13) 0.60964(14) 0.0165(4) Uani 1 1 d . . .
O7W O 0.8347(3) 0.63550(16) 0.21505(19) 0.0359(6) Uani 1 1 d . . .
O8 O 0.74532(18) 0.63855(12) 0.52170(14) 0.0135(4) Uani 1 1 d . . .
O9 O 0.72481(19) 0.46924(12) 0.74620(14) 0.0149(4) Uani 1 1 d . . .
O10 O 0.51105(19) 0.46608(12) 0.72289(14) 0.0143(4) Uani 1 1 d . . .
O11 O 0.68187(19) 0.49796(12) 0.42453(14) 0.0159(4) Uani 1 1 d . . .
O12 O 0.76902(19) 0.41991(12) 0.56890(14) 0.0141(4) Uani 1 1 d . . .
O13 O 0.48496(19) 0.40185(13) 0.32062(14) 0.0167(4) Uani 1 1 d . . .
O14 O 0.8045(2) 0.53570(12) 0.66104(14) 0.0154(4) Uani 1 1 d . . .
O15 O 0.36244(19) 0.31133(13) 0.42578(14) 0.0161(4) Uani 1 1 d . . .
O16 O 0.56281(19) 0.32539(13) 0.46274(14) 0.0174(5) Uani 1 1 d . . .
O17 O 0.6708(2) 0.33001(13) 0.80748(16) 0.0236(5) Uani 1 1 d . . .
O18 O 0.9386(2) 0.52995(14) 0.58592(17) 0.0249(5) Uani 1 1 d . . .
O19 O 0.96620(19) 0.58284(12) 0.81596(15) 0.0166(4) Uani 1 1 d . . .
O20 O 0.6655(2) 0.51294(13) 0.28436(15) 0.0190(5) Uani 1 1 d . . .
O21 O 0.7794(2) 0.77072(12) 0.57792(15) 0.0179(5) Uani 1 1 d . . .
O22 O 0.66484(19) 0.62255(12) 0.35902(14) 0.0148(4) Uani 1 1 d . . .
O23 O 0.5011(2) 0.42273(13) 0.19877(16) 0.0190(5) Uani 1 1 d . . .
O24 O 0.31432(19) 0.44800(12) 0.16934(14) 0.0134(4) Uani 1 1 d . . .
O25 O 0.85258(18) 0.67017(12) 0.68793(14) 0.0136(4) Uani 1 1 d . . .
O26 O 0.6599(2) 0.42233(16) 0.1868(2) 0.0345(6) Uani 1 1 d . . .
O27 O 1.1012(2) 0.54258(15) 0.97342(16) 0.0266(5) Uani 1 1 d . . .
H27 H 1.1000 0.5210 1.0150 0.032 Uiso 1 1 d R . .
O28 O 0.7731(2) 0.87133(13) 0.48997(16) 0.0254(5) Uani 1 1 d . . .
H28 H 0.7589 0.8870 0.4460 0.030 Uiso 1 1 d R . .
O29 O 0.88809(19) 0.53303(13) 0.89043(14) 0.0177(5) Uani 1 1 d . . .
O30 O 0.6862(2) 0.74903(12) 0.41685(15) 0.0167(4) Uani 1 1 d . . .
B1 B 0.6263(3) 0.5432(2) 0.3377(2) 0.0149(7) Uani 1 1 d . . .
B2 B 0.4447(3) 0.4522(2) 0.2404(2) 0.0147(7) Uani 1 1 d . . .
B3 B 0.7538(3) 0.69088(19) 0.5915(2) 0.0131(7) Uani 1 1 d . . .
B4 B 0.7603(3) 0.5403(2) 0.8033(2) 0.0132(7) Uani 1 1 d . . .
B5 B 0.6578(3) 0.6662(2) 0.4210(2) 0.0136(7) Uani 1 1 d . . .
B6 B 0.8441(3) 0.60035(19) 0.7268(2) 0.0124(6) Uani 1 1 d . . .
B7 B 0.7433(3) 0.7968(2) 0.4937(2) 0.0161(7) Uani 1 1 d . . .
B8 B 0.9836(3) 0.5517(2) 0.8921(2) 0.0156(7) Uani 1 1 d . . .
B9 B 0.6069(3) 0.4530(2) 0.2238(3) 0.0193(7) Uani 1 1 d . . .
N1 N 0.9371(3) 0.3077(2) 0.9098(2) 0.0387(8) Uani 1 1 d . . .
H1A H 0.9570 0.3469 0.8871 0.046 Uiso 1 1 d R . .
H1B H 0.8640 0.3099 0.8931 0.046 Uiso 1 1 d R . .
H1C H 0.9848 0.3139 0.9709 0.046 Uiso 1 1 d R . .
N2 N 0.9352(3) 0.23257(17) 0.7483(2) 0.0271(7) Uani 1 1 d . . .
H2A H 1.0061 0.2080 0.7731 0.032 Uiso 1 1 d R . .
H2B H 0.9521 0.2850 0.7601 0.032 Uiso 1 1 d R . .
N3 N 0.9488(3) 0.32033(18) 0.6138(2) 0.0289(7) Uani 1 1 d . . .
H3A H 0.9709 0.3330 0.5749 0.035 Uiso 1 1 d R . .
H3B H 0.8919 0.3529 0.5989 0.035 Uiso 1 1 d R . .
H3C H 1.0142 0.3280 0.6722 0.035 Uiso 1 1 d R . .
C1 C 0.9498(4) 0.2239(3) 0.8916(3) 0.0459(11) Uani 1 1 d . . .
H1D H 1.0351 0.2131 0.9232 0.055 Uiso 1 1 calc R . .
H1E H 0.9237 0.1902 0.9186 0.055 Uiso 1 1 calc R . .
C2 C 0.8774(4) 0.2049(3) 0.7895(3) 0.0424(10) Uani 1 1 d . . .
H2C H 0.8668 0.1490 0.7816 0.051 Uiso 1 1 calc R . .
H2D H 0.7973 0.2281 0.7552 0.051 Uiso 1 1 calc R . .
C3 C 0.8466(3) 0.2234(2) 0.6434(3) 0.0333(9) Uani 1 1 d . . .
H3D H 0.8152 0.1707 0.6283 0.040 Uiso 1 1 calc R . .
H3E H 0.7784 0.2583 0.6180 0.040 Uiso 1 1 calc R . .
C4 C 0.9032(4) 0.2400(2) 0.5976(3) 0.0324(8) Uani 1 1 d . . .
H4A H 0.9701 0.2043 0.6219 0.039 Uiso 1 1 calc R . .
H4B H 0.8433 0.2312 0.5305 0.039 Uiso 1 1 calc R . .
O6W O 0.8679(2) 0.77006(16) 0.39457(18) 0.0324(6) Uani 1 1 d . . .
H1 H 0.8130 0.7620 0.4011 0.039 Uiso 1 1 d R . .
H2 H 0.8310 0.8060 0.3431 0.039 Uiso 1 1 d R . .
O1W O 0.5000 0.5000 0.5000 0.139(3) Uani 1 2 d S . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
V1 0.0147(3) 0.0122(3) 0.0108(2) 0.00145(19) 0.0075(2) -0.00119(19)
V2 0.0133(3) 0.0105(3) 0.0117(2) 0.00054(19) 0.0078(2) 0.00019(19)
V3 0.0134(3) 0.0127(3) 0.0124(2) -0.00089(19) 0.0088(2) -0.00070(19)
V4 0.0143(3) 0.0116(3) 0.0123(2) -0.00100(19) 0.0086(2) -0.00037(19)
V5 0.0141(3) 0.0107(3) 0.0124(2) 0.00108(19) 0.0081(2) 0.00011(19)
V6 0.0151(3) 0.0112(3) 0.0123(2) -0.00166(19) 0.0092(2) -0.00121(19)
Na1 0.0442(10) 0.0373(10) 0.0825(14) 0.0088(9) 0.0420(10) 0.0008(8)
Na2 0.0581(11) 0.0347(9) 0.0684(12) 0.0129(8) 0.0539(10) 0.0083(8)
Na3 0.0345(8) 0.0273(8) 0.0335(8) 0.0046(6) 0.0212(7) -0.0018(6)
O1 0.0253(12) 0.0152(11) 0.0274(12) 0.0049(10) 0.0131(11) 0.0017(9)
O2 0.0269(13) 0.0218(12) 0.0254(12) -0.0029(10) 0.0184(11) 0.0017(10)
O2W 0.119(4) 0.083(3) 0.077(3) -0.026(2) 0.072(3) -0.041(3)
O3 0.0186(11) 0.0190(12) 0.0182(11) 0.0031(9) 0.0098(10) 0.0022(9)
O3W 0.057(2) 0.084(3) 0.103(4) 0.035(3) 0.050(3) 0.019(2)
O4 0.0278(13) 0.0167(11) 0.0244(12) -0.0054(9) 0.0172(11) -0.0019(9)
O4W 0.0491(18) 0.0403(17) 0.0535(18) 0.0089(14) 0.0394(16) 0.0042(14)
O5 0.0149(10) 0.0125(10) 0.0139(10) 0.0002(8) 0.0106(9) -0.0003(8)
O5W 0.0517(19) 0.0394(17) 0.068(2) 0.0056(15) 0.0440(18) 0.0067(14)
O6 0.0169(11) 0.0167(11) 0.0163(10) -0.0030(9) 0.0111(9) -0.0035(9)
O7 0.0142(11) 0.0208(11) 0.0146(10) -0.0031(9) 0.0091(9) -0.0017(9)
O7W 0.0476(17) 0.0351(15) 0.0308(14) 0.0075(12) 0.0273(14) 0.0052(13)
O8 0.0155(10) 0.0139(10) 0.0106(10) -0.0003(8) 0.0080(9) -0.0005(8)
O9 0.0174(11) 0.0141(11) 0.0163(10) -0.0025(8) 0.0121(9) -0.0034(8)
O10 0.0148(10) 0.0136(10) 0.0132(10) -0.0006(8) 0.0081(9) -0.0021(8)
O11 0.0199(11) 0.0125(10) 0.0139(10) -0.0009(8) 0.0100(9) -0.0024(9)
O12 0.0168(10) 0.0129(10) 0.0137(10) -0.0005(8) 0.0101(9) -0.0002(8)
O13 0.0143(10) 0.0187(11) 0.0145(10) 0.0030(9) 0.0077(9) -0.0017(9)
O14 0.0242(11) 0.0118(10) 0.0152(10) -0.0007(8) 0.0148(10) -0.0023(9)
O15 0.0152(11) 0.0220(11) 0.0119(10) 0.0015(8) 0.0089(9) 0.0012(9)
O16 0.0162(11) 0.0211(12) 0.0149(10) 0.0011(9) 0.0097(9) -0.0024(9)
O17 0.0281(13) 0.0215(12) 0.0176(11) 0.0059(9) 0.0124(10) 0.0009(10)
O18 0.0202(12) 0.0279(13) 0.0293(13) -0.0014(10) 0.0167(11) 0.0001(10)
O19 0.0143(10) 0.0190(11) 0.0150(11) 0.0035(9) 0.0085(9) 0.0003(9)
O20 0.0226(11) 0.0203(12) 0.0204(11) -0.0065(9) 0.0165(10) -0.0054(9)
O21 0.0267(12) 0.0125(11) 0.0149(10) -0.0005(8) 0.0132(10) -0.0029(9)
O22 0.0203(11) 0.0134(10) 0.0142(10) -0.0025(8) 0.0124(9) -0.0040(8)
O23 0.0198(11) 0.0206(11) 0.0215(11) -0.0072(9) 0.0154(10) -0.0053(9)
O24 0.0136(10) 0.0168(11) 0.0114(10) -0.0027(8) 0.0085(9) -0.0019(8)
O25 0.0154(10) 0.0133(10) 0.0115(10) 0.0004(8) 0.0081(9) -0.0018(8)
O26 0.0328(14) 0.0407(16) 0.0455(16) -0.0251(13) 0.0320(14) -0.0153(12)
O27 0.0174(12) 0.0404(15) 0.0186(12) 0.0114(10) 0.0095(10) 0.0002(10)
O28 0.0421(14) 0.0153(11) 0.0163(11) 0.0001(9) 0.0171(11) -0.0077(10)
O29 0.0151(11) 0.0230(12) 0.0135(10) 0.0032(9) 0.0082(9) -0.0002(9)
O30 0.0228(11) 0.0132(11) 0.0147(10) -0.0002(8) 0.0121(10) -0.0021(9)
B1 0.0173(17) 0.0155(17) 0.0147(16) -0.0015(13) 0.0114(15) -0.0007(13)
B2 0.0176(17) 0.0130(16) 0.0149(16) -0.0005(13) 0.0110(15) -0.0010(13)
B3 0.0153(16) 0.0106(16) 0.0126(16) 0.0006(13) 0.0083(14) -0.0001(13)
B4 0.0126(16) 0.0134(16) 0.0115(15) 0.0018(13) 0.0065(14) -0.0001(13)
B5 0.0138(16) 0.0128(17) 0.0115(16) 0.0000(13) 0.0066(14) -0.0024(13)
B6 0.0155(16) 0.0114(16) 0.0114(15) 0.0008(12) 0.0088(14) 0.0005(13)
B7 0.0160(17) 0.0162(17) 0.0156(16) 0.0022(14) 0.0097(14) 0.0006(13)
B8 0.0158(17) 0.0146(17) 0.0150(16) 0.0003(13) 0.0089(15) -0.0014(13)
B9 0.0220(18) 0.0213(19) 0.0201(18) -0.0038(14) 0.0157(16) -0.0023(15)
N1 0.045(2) 0.045(2) 0.0300(17) 0.0031(15) 0.0254(16) 0.0048(16)
N2 0.0312(16) 0.0196(15) 0.0381(17) 0.0007(13) 0.0254(15) 0.0018(12)
N3 0.0278(16) 0.0304(17) 0.0305(16) 0.0035(13) 0.0192(14) 0.0073(13)
C1 0.047(3) 0.047(3) 0.042(2) 0.009(2) 0.028(2) 0.000(2)
C2 0.050(3) 0.037(2) 0.049(3) -0.0022(19) 0.035(2) -0.008(2)
C3 0.0236(18) 0.0249(19) 0.042(2) 0.0010(17) 0.0162(18) 0.0018(15)
C4 0.036(2) 0.0261(19) 0.0278(19) 0.0022(15) 0.0162(18) 0.0084(16)
O6W 0.0288(14) 0.0399(15) 0.0313(14) 0.0084(12) 0.0202(12) 0.0064(11)
O1W 0.122(7) 0.120(7) 0.146(8) -0.003(6) 0.069(7) 0.019(6)
_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 O17 1.635(2) . ?
V1 O9 1.931(2) . ?
V1 O7 1.948(2) . ?
V1 O6 1.951(2) . ?
V1 O10 1.995(2) . ?
V1 V2 2.9972(9) . ?
V1 V5 3.0336(11) . ?
V1 Na3 3.3461(16) 3_666 ?
V2 O3 1.638(2) . ?
V2 O6 1.918(2) . ?
V2 O14 1.929(2) . ?
V2 O9 1.954(2) . ?
V2 O12 1.958(2) . ?
V2 V3 3.0274(10) . ?
V3 O18 1.621(2) . ?
V3 O11 1.932(2) . ?
V3 O14 1.935(2) . ?
V3 O12 1.978(2) . ?
V3 O8 2.008(2) . ?
V3 V4 3.0190(9) . ?
V4 O2 1.616(2) . ?
V4 O16 1.935(2) . ?
V4 O13 1.949(2) . ?
V4 O11 1.959(2) . ?
V4 O12 1.962(2) . ?
V4 V6 2.9782(11) . ?
V4 Na3 3.4415(18) 2_645 ?
V5 O1 1.629(2) . ?
V5 O16 1.924(2) . ?
V5 O6 1.944(2) . ?
V5 O7 1.954(2) . ?
V5 O15 1.958(2) . ?
V5 V6 2.9805(14) . ?
V6 O4 1.618(2) . ?
V6 O13 1.931(2) . ?
V6 O15 1.933(2) . ?
V6 O16 1.936(2) . ?
V6 O5 2.040(2) . ?
V6 Na3 3.2766(17) 2_645 ?
Na1 O2W 2.376(5) . ?
Na1 O28 2.392(3) 2_746 ?
Na1 O27 2.408(3) . ?
Na1 O3W 2.450(5) . ?
Na1 O5W 2.453(4) . ?
Na1 O24 2.933(3) 1_656 ?
Na2 O22 2.254(3) . ?
Na2 O7W 2.289(3) . ?
Na2 O20 2.396(3) . ?
Na2 O4 2.418(3) 2_655 ?
Na2 O4W 2.488(4) . ?
Na2 O6W 2.833(3) . ?
Na2 B1 2.881(4) . ?
Na3 O30 2.460(3) . ?
Na3 O23 2.501(3) 2_655 ?
Na3 O4 2.554(3) 2_655 ?
Na3 O17 2.605(3) 3_666 ?
Na3 O13 2.759(3) 2_655 ?
Na3 O2 2.802(3) 2_655 ?
Na3 O7 2.822(3) 3_666 ?
Na3 B5 3.035(4) . ?
Na3 B2 3.106(4) 2_655 ?
Na3 V6 3.2766(17) 2_655 ?
Na3 V1 3.3461(16) 3_666 ?
Na3 V4 3.4415(18) 2_655 ?
O2 Na3 2.802(3) 2_645 ?
O4 Na2 2.418(3) 2_645 ?
O4 Na3 2.554(3) 2_645 ?
O5 B6 1.519(4) 3_666 ?
O5 B4 1.536(4) 3_666 ?
O7 B5 1.480(4) 3_666 ?
O7 Na3 2.822(3) 3_666 ?
O8 B3 1.503(4) . ?
O8 B5 1.514(4) . ?
O9 B4 1.478(4) . ?
O10 B2 1.515(4) 3_666 ?
O10 B1 1.521(4) 3_666 ?
O11 B1 1.477(4) . ?
O13 B2 1.476(4) . ?
O13 Na3 2.759(3) 2_645 ?
O14 B6 1.468(4) . ?
O15 B3 1.462(4) 3_666 ?
O17 Na3 2.605(3) 3_666 ?
O19 B8 1.361(4) . ?
O19 B6 1.481(4) . ?
O20 B9 1.352(4) . ?
O20 B1 1.482(4) . ?
O21 B7 1.360(4) . ?
O21 B3 1.481(4) . ?
O22 B5 1.413(4) . ?
O22 B1 1.432(4) . ?
O23 B9 1.360(4) . ?
O23 B2 1.491(4) . ?
O23 Na3 2.501(3) 2_645 ?
O24 B4 1.433(4) 3_666 ?
O24 B2 1.441(4) . ?
O24 Na1 2.933(3) 1_454 ?
O25 B6 1.439(4) . ?
O25 B3 1.448(4) . ?
O26 B9 1.387(4) . ?
O27 B8 1.376(4) . ?
O27 H27 0.8549 . ?
O28 B7 1.366(4) . ?
O28 Na1 2.392(3) 2_756 ?
O28 H28 0.7461 . ?
O29 B8 1.365(4) . ?
O29 B4 1.484(4) . ?
O30 B7 1.371(4) . ?
O30 B5 1.497(4) . ?
B1 O10 1.521(4) 3_666 ?
B2 O10 1.515(4) 3_666 ?
B2 Na3 3.106(4) 2_645 ?
B3 O15 1.462(4) 3_666 ?
B4 O24 1.433(4) 3_666 ?
B4 O5 1.536(4) 3_666 ?
B5 O7 1.480(4) 3_666 ?
B6 O5 1.519(4) 3_666 ?
N1 C1 1.518(6) . ?
N1 H1A 0.9230 . ?
N1 H1B 0.8725 . ?
N1 H1C 0.8772 . ?
N2 C2 1.491(5) . ?
N2 C3 1.503(5) . ?
N2 H2A 0.9028 . ?
N2 H2B 0.9244 . ?
N3 C4 1.475(5) . ?
N3 H3A 0.9623 . ?
N3 H3B 0.8705 . ?
N3 H3C 0.8795 . ?
C1 C2 1.498(6) . ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C4 1.501(6) . ?
C3 H3D 0.9700 . ?
C3 H3E 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
O6W H1 0.8639 . ?
O6W H2 0.9621 . ?
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
O17 V1 O9 110.82(11) . . ?
O17 V1 O7 106.87(11) . . ?
O9 V1 O7 139.90(9) . . ?
O17 V1 O6 107.36(11) . . ?
O9 V1 O6 78.45(9) . . ?
O7 V1 O6 77.73(9) . . ?
O17 V1 O10 107.31(11) . . ?
O9 V1 O10 89.51(9) . . ?
O7 V1 O10 92.10(9) . . ?
O6 V1 O10 145.33(9) . . ?
O17 V1 V2 112.29(9) . . ?
O9 V1 V2 39.79(6) . . ?
O7 V1 V2 111.95(7) . . ?
O6 V1 V2 38.81(6) . . ?
O10 V1 V2 123.73(6) . . ?
O17 V1 V5 110.26(9) . . ?
O9 V1 V5 112.23(6) . . ?
O7 V1 V5 39.05(6) . . ?
O6 V1 V5 38.76(6) . . ?
O10 V1 V5 124.86(7) . . ?
V2 V1 V5 75.38(3) . . ?
O17 V1 Na3 49.67(9) . 3_666 ?
O9 V1 Na3 158.99(7) . 3_666 ?
O7 V1 Na3 57.37(7) . 3_666 ?
O6 V1 Na3 98.86(7) . 3_666 ?
O10 V1 Na3 103.25(7) . 3_666 ?
V2 V1 Na3 132.80(3) . 3_666 ?
V5 V1 Na3 74.17(3) . 3_666 ?
O3 V2 O6 107.56(11) . . ?
O3 V2 O14 111.27(11) . . ?
O6 V2 O14 141.02(10) . . ?
O3 V2 O9 106.53(11) . . ?
O6 V2 O9 78.70(9) . . ?
O14 V2 O9 87.23(9) . . ?
O3 V2 O12 105.59(10) . . ?
O6 V2 O12 94.72(9) . . ?
O14 V2 O12 78.19(9) . . ?
O9 V2 O12 147.71(9) . . ?
O3 V2 V1 109.61(8) . . ?
O6 V2 V1 39.61(6) . . ?
O14 V2 V1 119.77(7) . . ?
O9 V2 V1 39.24(6) . . ?
O12 V2 V1 128.73(7) . . ?
O3 V2 V3 110.54(8) . . ?
O6 V2 V3 126.75(7) . . ?
O14 V2 V3 38.49(6) . . ?
O9 V2 V3 122.22(7) . . ?
O12 V2 V3 39.97(6) . . ?
V1 V2 V3 139.66(2) . . ?
O18 V3 O11 112.16(11) . . ?
O18 V3 O14 111.85(11) . . ?
O11 V3 O14 134.57(10) . . ?
O18 V3 O12 107.47(11) . . ?
O11 V3 O12 79.22(9) . . ?
O14 V3 O12 77.55(9) . . ?
O18 V3 O8 104.50(11) . . ?
O11 V3 O8 90.47(9) . . ?
O14 V3 O8 89.11(9) . . ?
O12 V3 O8 147.98(9) . . ?
O18 V3 V4 114.84(9) . . ?
O11 V3 V4 39.45(6) . . ?
O14 V3 V4 109.34(7) . . ?
O12 V3 V4 39.80(6) . . ?
O8 V3 V4 124.37(6) . . ?
O18 V3 V2 112.09(9) . . ?
O11 V3 V2 112.00(7) . . ?
O14 V3 V2 38.33(6) . . ?
O12 V3 V2 39.49(6) . . ?
O8 V3 V2 123.76(6) . . ?
V4 V3 V2 75.68(3) . . ?
O2 V4 O16 108.51(11) . . ?
O2 V4 O13 105.30(11) . . ?
O16 V4 O13 79.05(9) . . ?
O2 V4 O11 108.89(11) . . ?
O16 V4 O11 142.49(9) . . ?
O13 V4 O11 88.54(9) . . ?
O2 V4 O12 109.19(11) . . ?
O16 V4 O12 91.50(9) . . ?
O13 V4 O12 145.47(9) . . ?
O11 V4 O12 78.94(9) . . ?
O2 V4 V6 108.32(9) . . ?
O16 V4 V6 39.71(7) . . ?
O13 V4 V6 39.65(6) . . ?
O11 V4 V6 122.34(7) . . ?
O12 V4 V6 125.92(7) . . ?
O2 V4 V3 113.76(9) . . ?
O16 V4 V3 123.42(7) . . ?
O13 V4 V3 121.36(7) . . ?
O11 V4 V3 38.79(6) . . ?
O12 V4 V3 40.18(6) . . ?
V6 V4 V3 137.79(2) . . ?
O2 V4 Na3 53.57(9) . 2_645 ?
O16 V4 Na3 85.92(7) . 2_645 ?
O13 V4 Na3 53.22(7) . 2_645 ?
O11 V4 Na3 114.52(7) . 2_645 ?
O12 V4 Na3 160.01(7) . 2_645 ?
V6 V4 Na3 60.88(3) . 2_645 ?
V3 V4 Na3 150.10(3) . 2_645 ?
O1 V5 O16 109.49(11) . . ?
O1 V5 O6 108.68(11) . . ?
O16 V5 O6 91.45(9) . . ?
O1 V5 O7 107.21(11) . . ?
O16 V5 O7 143.29(10) . . ?
O6 V5 O7 77.73(9) . . ?
O1 V5 O15 109.02(11) . . ?
O16 V5 O15 78.95(9) . . ?
O6 V5 O15 142.17(10) . . ?
O7 V5 O15 88.35(9) . . ?
O1 V5 V6 111.35(9) . . ?
O16 V5 V6 39.59(7) . . ?
O6 V5 V6 124.58(7) . . ?
O7 V5 V6 122.63(7) . . ?
O15 V5 V6 39.69(6) . . ?
O1 V5 V1 111.36(9) . . ?
O16 V5 V1 123.40(7) . . ?
O6 V5 V1 38.92(6) . . ?
O7 V5 V1 38.90(6) . . ?
O15 V5 V1 120.53(7) . . ?
V6 V5 V1 137.23(3) . . ?
O4 V6 O13 106.68(11) . . ?
O4 V6 O15 110.86(11) . . ?
O13 V6 O15 140.75(10) . . ?
O4 V6 O16 106.56(11) . . ?
O13 V6 O16 79.48(9) . . ?
O15 V6 O16 79.29(9) . . ?
O4 V6 O5 106.69(11) . . ?
O13 V6 O5 88.96(9) . . ?
O15 V6 O5 91.01(9) . . ?
O16 V6 O5 146.68(9) . . ?
O4 V6 V4 107.99(9) . . ?
O13 V6 V4 40.09(6) . . ?
O15 V6 V4 114.54(7) . . ?
O16 V6 V4 39.70(6) . . ?
O5 V6 V4 124.58(6) . . ?
O4 V6 V5 110.60(9) . . ?
O13 V6 V5 114.46(7) . . ?
O15 V6 V5 40.31(7) . . ?
O16 V6 V5 39.31(6) . . ?
O5 V6 V5 126.51(6) . . ?
V4 V6 V5 77.45(3) . . ?
O4 V6 Na3 49.87(9) . 2_645 ?
O13 V6 Na3 57.20(7) . 2_645 ?
O15 V6 Na3 154.87(7) . 2_645 ?
O16 V6 Na3 90.71(8) . 2_645 ?
O5 V6 Na3 109.13(7) . 2_645 ?
V4 V6 Na3 66.56(4) . 2_645 ?
V5 V6 Na3 124.13(4) . 2_645 ?
O2W Na1 O28 156.59(16) . 2_746 ?
O2W Na1 O27 94.34(16) . . ?
O28 Na1 O27 86.45(10) 2_746 . ?
O2W Na1 O3W 100.35(17) . . ?
O28 Na1 O3W 86.79(13) 2_746 . ?
O27 Na1 O3W 157.40(17) . . ?
O2W Na1 O5W 102.33(15) . . ?
O28 Na1 O5W 101.02(12) 2_746 . ?
O27 Na1 O5W 83.81(11) . . ?
O3W Na1 O5W 76.37(14) . . ?
O2W Na1 O24 97.73(13) . 1_656 ?
O28 Na1 O24 59.69(8) 2_746 1_656 ?
O27 Na1 O24 76.16(9) . 1_656 ?
O3W Na1 O24 118.21(13) . 1_656 ?
O5W Na1 O24 152.58(11) . 1_656 ?
O22 Na2 O7W 172.81(12) . . ?
O22 Na2 O20 60.13(8) . . ?
O7W Na2 O20 114.37(11) . . ?
O22 Na2 O4 85.81(9) . 2_655 ?
O7W Na2 O4 101.31(11) . 2_655 ?
O20 Na2 O4 121.91(11) . 2_655 ?
O22 Na2 O4W 85.16(10) . . ?
O7W Na2 O4W 89.60(11) . . ?
O20 Na2 O4W 82.81(10) . . ?
O4 Na2 O4W 143.63(12) 2_655 . ?
O22 Na2 O6W 88.33(9) . . ?
O7W Na2 O6W 95.09(11) . . ?
O20 Na2 O6W 142.98(10) . . ?
O4 Na2 O6W 69.44(9) 2_655 . ?
O4W Na2 O6W 75.14(11) . . ?
O22 Na2 B1 29.26(9) . . ?
O7W Na2 B1 145.22(12) . . ?
O20 Na2 B1 30.91(9) . . ?
O4 Na2 B1 103.83(11) 2_655 . ?
O4W Na2 B1 84.25(11) . . ?
O6W Na2 B1 116.06(10) . . ?
O22 Na2 Na3 52.57(7) . . ?
O7W Na2 Na3 134.56(9) . . ?
O20 Na2 Na3 99.09(7) . . ?
O4 Na2 Na3 33.26(6) 2_655 . ?
O4W Na2 Na3 125.81(9) . . ?
O6W Na2 Na3 71.87(7) . . ?
B1 Na2 Na3 73.57(8) . . ?
O30 Na3 O23 95.07(9) . 2_655 ?
O30 Na3 O4 79.51(9) . 2_655 ?
O23 Na3 O4 111.76(9) 2_655 2_655 ?
O30 Na3 O17 114.39(9) . 3_666 ?
O23 Na3 O17 137.61(10) 2_655 3_666 ?
O4 Na3 O17 103.41(9) 2_655 3_666 ?
O30 Na3 O13 110.71(9) . 2_655 ?
O23 Na3 O13 54.06(7) 2_655 2_655 ?
O4 Na3 O13 64.84(7) 2_655 2_655 ?
O17 Na3 O13 130.06(9) 3_666 2_655 ?
O30 Na3 O2 172.16(9) . 2_655 ?
O23 Na3 O2 80.43(8) 2_655 2_655 ?
O4 Na3 O2 96.11(9) 2_655 2_655 ?
O17 Na3 O2 72.85(8) 3_666 2_655 ?
O13 Na3 O2 61.45(7) 2_655 2_655 ?
O30 Na3 O7 53.57(7) . 3_666 ?
O23 Na3 O7 122.63(9) 2_655 3_666 ?
O4 Na3 O7 107.68(8) 2_655 3_666 ?
O17 Na3 O7 64.05(8) 3_666 3_666 ?
O13 Na3 O7 164.26(9) 2_655 3_666 ?
O2 Na3 O7 134.27(8) 2_655 3_666 ?
O30 Na3 B5 29.30(8) . . ?
O23 Na3 B5 120.60(10) 2_655 . ?
O4 Na3 B5 83.96(9) 2_655 . ?
O17 Na3 B5 85.14(9) 3_666 . ?
O13 Na3 B5 136.11(10) 2_655 . ?
O2 Na3 B5 157.43(10) 2_655 . ?
O7 Na3 B5 28.98(8) 3_666 . ?
O30 Na3 B2 95.90(9) . 2_655 ?
O23 Na3 B2 28.31(8) 2_655 2_655 ?
O4 Na3 B2 84.04(9) 2_655 2_655 ?
O17 Na3 B2 149.59(10) 3_666 2_655 ?
O13 Na3 B2 28.37(8) 2_655 2_655 ?
O2 Na3 B2 77.08(9) 2_655 2_655 ?
O7 Na3 B2 142.29(9) 3_666 2_655 ?
B5 Na3 B2 125.20(10) . 2_655 ?
O30 Na3 V6 96.27(7) . 2_655 ?
O23 Na3 V6 86.96(6) 2_655 2_655 ?
O4 Na3 V6 28.98(5) 2_655 2_655 ?
O17 Na3 V6 117.32(7) 3_666 2_655 ?
O13 Na3 V6 36.05(5) 2_655 2_655 ?
O2 Na3 V6 77.17(6) 2_655 2_655 ?
O7 Na3 V6 136.13(7) 3_666 2_655 ?
B5 Na3 V6 109.85(8) . 2_655 ?
B2 Na3 V6 58.69(7) 2_655 2_655 ?
O30 Na3 V1 86.70(7) . 3_666 ?
O23 Na3 V1 141.44(7) 2_655 3_666 ?
O4 Na3 V1 106.44(7) 2_655 3_666 ?
O17 Na3 V1 28.58(5) 3_666 3_666 ?
O13 Na3 V1 157.42(7) 2_655 3_666 ?
O2 Na3 V1 100.83(7) 2_655 3_666 ?
O7 Na3 V1 35.55(5) 3_666 3_666 ?
B5 Na3 V1 58.01(7) . 3_666 ?
B2 Na3 V1 169.51(8) 2_655 3_666 ?
V6 Na3 V1 131.23(5) 2_655 3_666 ?
O30 Na3 V4 144.58(7) . 2_655 ?
O23 Na3 V4 69.80(6) 2_655 2_655 ?
O4 Na3 V4 77.18(7) 2_655 2_655 ?
O17 Na3 V4 96.81(7) 3_666 2_655 ?
O13 Na3 V4 34.46(5) 2_655 2_655 ?
O2 Na3 V4 27.65(5) 2_655 2_655 ?
O7 Na3 V4 160.79(7) 3_666 2_655 ?
B5 Na3 V4 160.99(8) . 2_655 ?
B2 Na3 V4 55.57(7) 2_655 2_655 ?
V6 Na3 V4 52.56(3) 2_655 2_655 ?
V1 Na3 V4 125.38(5) 3_666 2_655 ?
V4 O2 Na3 98.78(11) . 2_645 ?
V6 O4 Na2 141.35(14) . 2_645 ?
V6 O4 Na3 101.15(11) . 2_645 ?
Na2 O4 Na3 115.46(10) 2_645 2_645 ?
B6 O5 B4 112.8(2) 3_666 3_666 ?
B6 O5 V6 119.83(17) 3_666 . ?
B4 O5 V6 121.23(17) 3_666 . ?
V2 O6 V5 145.43(12) . . ?
V2 O6 V1 101.58(10) . . ?
V5 O6 V1 102.32(10) . . ?
B5 O7 V1 129.45(18) 3_666 . ?
B5 O7 V5 128.29(18) 3_666 . ?
V1 O7 V5 102.05(10) . . ?
B5 O7 Na3 83.52(16) 3_666 3_666 ?
V1 O7 Na3 87.08(8) . 3_666 ?
V5 O7 Na3 106.22(10) . 3_666 ?
B3 O8 B5 114.4(2) . . ?
B3 O8 V3 120.84(17) . . ?
B5 O8 V3 121.97(17) . . ?
B4 O9 V1 130.31(18) . . ?
B4 O9 V2 128.63(18) . . ?
V1 O9 V2 100.97(10) . . ?
B2 O10 B1 113.8(2) 3_666 3_666 ?
B2 O10 V1 122.59(18) 3_666 . ?
B1 O10 V1 120.79(18) 3_666 . ?
B1 O11 V3 130.16(19) . . ?
B1 O11 V4 128.08(19) . . ?
V3 O11 V4 101.76(10) . . ?
V2 O12 V4 142.22(12) . . ?
V2 O12 V3 100.55(9) . . ?
V4 O12 V3 100.02(9) . . ?
B2 O13 V6 133.14(19) . . ?
B2 O13 V4 126.54(19) . . ?
V6 O13 V4 100.26(10) . . ?
B2 O13 Na3 89.00(17) . 2_645 ?
V6 O13 Na3 86.75(9) . 2_645 ?
V4 O13 Na3 92.31(9) . 2_645 ?
B6 O14 V2 125.27(18) . . ?
B6 O14 V3 129.34(18) . . ?
V2 O14 V3 103.18(10) . . ?
B3 O15 V6 131.61(18) 3_666 . ?
B3 O15 V5 128.38(18) 3_666 . ?
V6 O15 V5 100.00(10) . . ?
V5 O16 V4 149.96(12) . . ?
V5 O16 V6 101.10(10) . . ?
V4 O16 V6 100.59(10) . . ?
V1 O17 Na3 101.75(11) . 3_666 ?
B8 O19 B6 123.1(2) . . ?
B9 O20 B1 121.2(3) . . ?
B9 O20 Na2 136.1(2) . . ?
B1 O20 Na2 92.94(18) . . ?
B7 O21 B3 122.6(2) . . ?
B5 O22 B1 121.4(2) . . ?
B5 O22 Na2 137.74(19) . . ?
B1 O22 Na2 100.47(18) . . ?
B9 O23 B2 121.3(3) . . ?
B9 O23 Na3 114.6(2) . 2_645 ?
B2 O23 Na3 99.00(17) . 2_645 ?
B4 O24 B2 118.5(2) 3_666 . ?
B4 O24 Na1 131.31(18) 3_666 1_454 ?
B2 O24 Na1 100.95(17) . 1_454 ?
B6 O25 B3 119.5(2) . . ?
B8 O27 Na1 132.7(2) . . ?
B8 O27 H27 109.3 . . ?
Na1 O27 H27 106.4 . . ?
B7 O28 Na1 137.9(2) . 2_756 ?
B7 O28 H28 120.6 . . ?
Na1 O28 H28 81.5 2_756 . ?
B8 O29 B4 121.3(2) . . ?
B7 O30 B5 121.6(2) . . ?
B7 O30 Na3 122.7(2) . . ?
B5 O30 Na3 97.15(17) . . ?
O22 B1 O11 110.8(3) . . ?
O22 B1 O20 106.3(2) . . ?
O11 B1 O20 110.8(3) . . ?
O22 B1 O10 113.0(3) . 3_666 ?
O11 B1 O10 107.6(2) . 3_666 ?
O20 B1 O10 108.2(2) . 3_666 ?
O22 B1 Na2 50.27(14) . . ?
O11 B1 Na2 129.0(2) . . ?
O20 B1 Na2 56.15(15) . . ?
O10 B1 Na2 123.4(2) 3_666 . ?
O24 B2 O13 110.2(3) . . ?
O24 B2 O23 107.9(2) . . ?
O13 B2 O23 108.0(2) . . ?
O24 B2 O10 112.6(3) . 3_666 ?
O13 B2 O10 108.1(2) . 3_666 ?
O23 B2 O10 109.8(2) . 3_666 ?
O24 B2 Na3 99.29(18) . 2_645 ?
O13 B2 Na3 62.63(15) . 2_645 ?
O23 B2 Na3 52.69(14) . 2_645 ?
O10 B2 Na3 147.7(2) 3_666 2_645 ?
O25 B3 O15 110.4(2) . 3_666 ?
O25 B3 O21 106.5(2) . . ?
O15 B3 O21 110.1(2) 3_666 . ?
O25 B3 O8 112.9(2) . . ?
O15 B3 O8 108.5(2) 3_666 . ?
O21 B3 O8 108.3(2) . . ?
O24 B4 O9 111.4(2) 3_666 . ?
O24 B4 O29 107.4(2) 3_666 . ?
O9 B4 O29 109.5(2) . . ?
O24 B4 O5 112.8(2) 3_666 3_666 ?
O9 B4 O5 107.9(2) . 3_666 ?
O29 B4 O5 107.7(2) . 3_666 ?
O22 B5 O7 110.3(2) . 3_666 ?
O22 B5 O30 108.2(2) . . ?
O7 B5 O30 107.6(2) 3_666 . ?
O22 B5 O8 113.2(3) . . ?
O7 B5 O8 108.7(2) 3_666 . ?
O30 B5 O8 108.7(2) . . ?
O22 B5 Na3 90.22(17) . . ?
O7 B5 Na3 67.50(15) 3_666 . ?
O30 B5 Na3 53.54(14) . . ?
O8 B5 Na3 155.3(2) . . ?
O25 B6 O14 109.7(2) . . ?
O25 B6 O19 108.4(2) . . ?
O14 B6 O19 109.3(2) . . ?
O25 B6 O5 112.1(2) . 3_666 ?
O14 B6 O5 108.6(2) . 3_666 ?
O19 B6 O5 108.7(2) . 3_666 ?
O21 B7 O28 117.2(3) . . ?
O21 B7 O30 121.6(3) . . ?
O28 B7 O30 121.0(3) . . ?
O19 B8 O29 121.7(3) . . ?
O19 B8 O27 118.3(3) . . ?
O29 B8 O27 120.0(3) . . ?
O20 B9 O23 123.2(3) . . ?
O20 B9 O26 116.8(3) . . ?
O23 B9 O26 120.1(3) . . ?
C1 N1 H1A 119.2 . . ?
C1 N1 H1B 103.9 . . ?
H1A N1 H1B 115.8 . . ?
C1 N1 H1C 107.0 . . ?
H1A N1 H1C 106.0 . . ?
H1B N1 H1C 103.6 . . ?
C2 N2 C3 109.3(3) . . ?
C2 N2 H2A 112.2 . . ?
C3 N2 H2A 111.4 . . ?
C2 N2 H2B 109.7 . . ?
C3 N2 H2B 106.7 . . ?
H2A N2 H2B 107.4 . . ?
C4 N3 H3A 111.4 . . ?
C4 N3 H3B 110.0 . . ?
H3A N3 H3B 106.4 . . ?
C4 N3 H3C 112.2 . . ?
H3A N3 H3C 106.5 . . ?
H3B N3 H3C 110.0 . . ?
C2 C1 N1 113.5(4) . . ?
C2 C1 H1D 108.9 . . ?
N1 C1 H1D 108.9 . . ?
C2 C1 H1E 108.9 . . ?
N1 C1 H1E 108.9 . . ?
H1D C1 H1E 107.7 . . ?
N2 C2 C1 113.4(4) . . ?
N2 C2 H2C 108.9 . . ?
C1 C2 H2C 108.9 . . ?
N2 C2 H2D 108.9 . . ?
C1 C2 H2D 108.9 . . ?
H2C C2 H2D 107.7 . . ?
C4 C3 N2 112.5(3) . . ?
C4 C3 H3D 109.1 . . ?
N2 C3 H3D 109.1 . . ?
C4 C3 H3E 109.1 . . ?
N2 C3 H3E 109.1 . . ?
H3D C3 H3E 107.8 . . ?
N3 C4 C3 112.5(3) . . ?
N3 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
N3 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
Na2 O6W H1 76.1 . . ?
Na2 O6W H2 96.3 . . ?
H1 O6W H2 104.8 . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.308
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.090