# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

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

data_w
_audit_block_doi                 10.5517/ccdc.csd.cc1kx64t
_database_code_depnum_ccdc_archive 'CCDC 1457066'
_audit_update_record             
;
2016-03-15 deposited with the CCDC.
2017-01-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B36 H12 Li20 O120 V24'
_chemical_formula_weight         3682.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
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           cubic
_symmetry_space_group_name_H-M   Pn-3

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

_cell_length_a                   18.880(2)
_cell_length_b                   18.880(2)
_cell_length_c                   18.880(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6730.2(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3584
_cell_measurement_theta_min      2.984
_cell_measurement_theta_max      28.961

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3528
_exptl_absorpt_coefficient_mu    1.694
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.7070
_exptl_absorpt_correction_T_max  0.7503
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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 Saturn724 CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            59185
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.40
_reflns_number_total             2564
_reflns_number_gt                2317
_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. 
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.004 -0.003 -0.003 988 201 ' '
2 0.100 0.250 0.750 15 9 ' '
3 0.250 0.600 0.750 15 9 ' '
4 0.250 0.750 0.400 15 9 ' '
5 0.250 0.750 0.100 15 9 ' '
6 0.250 0.900 0.750 15 9 ' '
7 0.400 0.250 0.750 15 9 ' '
8 0.600 0.750 0.250 15 9 ' '
9 0.750 0.100 0.250 15 9 ' '
10 0.750 0.250 0.600 15 9 ' '
11 0.750 0.250 0.900 15 9 ' '
12 0.750 0.400 0.250 15 9 ' '
13 0.900 0.750 0.250 15 9 ' '
_platon_squeeze_details          
;
;

_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)+(0.1188P)²+38.8739P] where P=(Fo²+2Fc²)/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         2564
_refine_ls_number_parameters     155
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0591
_refine_ls_wR_factor_ref         0.1835
_refine_ls_wR_factor_gt          0.1756
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_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
B1 B 0.6883(3) 1.0349(3) 0.3995(3) 0.0138(9) Uani 1 1 d . . .
B2 B 0.8091(3) 0.9908(3) 0.3716(3) 0.0115(9) Uani 1 1 d . . .
B3 B 0.9080(3) 0.9592(3) 0.2922(2) 0.0118(9) Uani 1 1 d . . .
O1 O 0.61668(19) 1.0370(2) 0.3870(2) 0.0266(9) Uani 1 1 d . . .
H1 H 0.607(4) 1.013(4) 0.352(4) 0.040 Uiso 1 1 d . . .
O2 O 0.71474(17) 1.08083(18) 0.44843(18) 0.0160(7) Uani 1 1 d . . .
O3 O 0.73050(17) 0.98862(18) 0.36346(17) 0.0157(7) Uani 1 1 d . . .
O4 O 0.83266(18) 0.94168(17) 0.42715(17) 0.0148(7) Uani 1 1 d . . .
O5 O 0.83468(16) 0.97101(16) 0.30306(16) 0.0119(6) Uani 1 1 d . . .
O6 O 0.93488(16) 0.89350(16) 0.33026(16) 0.0118(6) Uani 1 1 d . . .
O7 O 0.95003(17) 1.02055(17) 0.31686(17) 0.0146(7) Uani 1 1 d . . .
O8 O 1.02101(17) 1.11670(17) 0.36669(17) 0.0156(7) Uani 1 1 d . . .
O9 O 1.0819(2) 1.0505(2) 0.2422(2) 0.0264(8) Uani 1 1 d . . .
O10 O 0.83645(19) 0.79269(19) 0.3936(2) 0.0228(8) Uani 1 1 d . . .
V1 V 0.88922(4) 0.85610(4) 0.41880(4) 0.0107(2) Uani 1 1 d . . .
V2 V 1.05248(4) 1.03046(4) 0.32126(4) 0.0111(2) Uani 1 1 d . . .
Li1 Li 0.8165(7) 0.6474(6) 0.4189(9) 0.050(3) Uani 1 1 d U . .
Li2 Li 0.7500 0.8432(8) 0.2500 0.049(4) Uani 1 2 d SU . .
Li3 Li 1.0000 1.0000 0.5000 0.068(10) Uani 1 6 d S . .


_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
B1 O2 1.363(6) . ?
B1 O3 1.364(6) . ?
B1 O1 1.372(6) . ?
B2 O5 1.431(6) . ?
B2 O4 1.468(6) . ?
B2 O3 1.493(6) . ?
B2 O6 1.517(6) 20_675 ?
B3 O5 1.417(6) . ?
B3 O7 1.479(6) . ?
B3 O2 1.492(5) 23_765 ?
B3 O6 1.520(6) . ?
O1 H1 0.82(8) . ?
O2 B3 1.492(5) 20_675 ?
O4 V1 1.943(3) . ?
O4 V2 1.965(3) 20_675 ?
O6 B2 1.517(6) 23_765 ?
O6 V1 2.009(3) . ?
O7 V2 1.945(3) . ?
O7 V1 1.949(3) 20_675 ?
O8 V2 1.932(3) 11_566 ?
O8 V2 1.934(3) . ?
O8 V1 1.943(3) 20_675 ?
O9 V2 1.637(4) . ?
O10 V1 1.629(4) . ?
V1 O8 1.943(3) 23_765 ?
V1 O7 1.949(3) 23_765 ?
V1 V2 3.0116(11) 20_675 ?
V1 V2 3.0170(11) 23_765 ?
V2 O8 1.932(3) 8_656 ?
V2 O4 1.965(3) 23_765 ?
V2 V1 3.0116(11) 23_765 ?
V2 V1 3.0170(11) 20_675 ?
Li1 Li2 3.431(17) 2_665 ?
Li2 Li1 3.431(17) 4_565 ?
Li2 Li1 3.431(17) 2_665 ?
Li2 Li2 3.52(3) 2_665 ?

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
O2 B1 O3 122.1(4) . . ?
O2 B1 O1 117.4(4) . . ?
O3 B1 O1 120.6(4) . . ?
O5 B2 O4 112.3(4) . . ?
O5 B2 O3 103.6(3) . . ?
O4 B2 O3 111.0(4) . . ?
O5 B2 O6 113.5(4) . 20_675 ?
O4 B2 O6 108.1(3) . 20_675 ?
O3 B2 O6 108.4(3) . 20_675 ?
O5 B3 O7 110.8(4) . . ?
O5 B3 O2 107.5(4) . 23_765 ?
O7 B3 O2 109.8(4) . 23_765 ?
O5 B3 O6 112.7(4) . . ?
O7 B3 O6 108.2(3) . . ?
O2 B3 O6 107.7(3) 23_765 . ?
B1 O1 H1 109(6) . . ?
B1 O2 B3 122.8(4) . 20_675 ?
B1 O3 B2 120.8(4) . . ?
B2 O4 V1 129.3(3) . . ?
B2 O4 V2 129.8(3) . 20_675 ?
V1 O4 V2 100.80(15) . 20_675 ?
B3 O5 B2 120.1(3) . . ?
B2 O6 B3 114.0(3) 23_765 . ?
B2 O6 V1 121.4(3) 23_765 . ?
B3 O6 V1 122.4(3) . . ?
B3 O7 V2 128.5(3) . . ?
B3 O7 V1 129.9(3) . 20_675 ?
V2 O7 V1 101.57(15) . 20_675 ?
V2 O8 V2 146.35(19) 11_566 . ?
V2 O8 V1 102.00(15) 11_566 20_675 ?
V2 O8 V1 102.18(15) . 20_675 ?
O10 V1 O4 107.38(17) . . ?
O10 V1 O8 109.30(18) . 23_765 ?
O4 V1 O8 78.60(14) . 23_765 ?
O10 V1 O7 110.10(16) . 23_765 ?
O4 V1 O7 140.52(14) . 23_765 ?
O8 V1 O7 77.82(14) 23_765 23_765 ?
O10 V1 O6 106.14(17) . . ?
O4 V1 O6 90.63(13) . . ?
O8 V1 O6 144.57(14) 23_765 . ?
O7 V1 O6 90.59(13) 23_765 . ?
O10 V1 V2 111.41(14) . 20_675 ?
O4 V1 V2 39.87(10) . 20_675 ?
O8 V1 V2 38.87(10) 23_765 20_675 ?
O7 V1 V2 112.24(10) 23_765 20_675 ?
O6 V1 V2 124.32(9) . 20_675 ?
O10 V1 V2 113.05(14) . 23_765 ?
O4 V1 V2 112.93(10) . 23_765 ?
O8 V1 V2 38.80(10) 23_765 23_765 ?
O7 V1 V2 39.17(10) 23_765 23_765 ?
O6 V1 V2 123.85(9) . 23_765 ?
V2 V1 V2 75.73(3) 20_675 23_765 ?
O9 V2 O8 107.81(18) . 8_656 ?
O9 V2 O8 108.33(18) . . ?
O8 V2 O8 92.95(19) 8_656 . ?
O9 V2 O7 108.73(18) . . ?
O8 V2 O7 143.37(15) 8_656 . ?
O8 V2 O7 78.14(14) . . ?
O9 V2 O4 108.04(18) . 23_765 ?
O8 V2 O4 78.33(14) 8_656 23_765 ?
O8 V2 O4 143.54(15) . 23_765 ?
O7 V2 O4 87.99(14) . 23_765 ?
O9 V2 V1 110.81(14) . 23_765 ?
O8 V2 V1 39.14(10) 8_656 23_765 ?
O8 V2 V1 125.20(10) . 23_765 ?
O7 V2 V1 121.39(10) . 23_765 ?
O4 V2 V1 39.33(9) 23_765 23_765 ?
O9 V2 V1 111.53(14) . 20_675 ?
O8 V2 V1 125.10(10) 8_656 20_675 ?
O8 V2 V1 39.02(10) . 20_675 ?
O7 V2 V1 39.26(10) . 20_675 ?
O4 V2 V1 121.46(10) 23_765 20_675 ?
V1 V2 V1 137.60(4) 23_765 20_675 ?
Li1 Li2 Li1 174.1(6) 4_565 2_665 ?
Li1 Li2 Li2 93.0(3) 4_565 2_665 ?
Li1 Li2 Li2 93.0(3) 2_665 2_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 B1 O2 B3 9.2(7) . . . 20_675 ?
O1 B1 O2 B3 -170.4(4) . . . 20_675 ?
O2 B1 O3 B2 -5.5(7) . . . . ?
O1 B1 O3 B2 174.1(4) . . . . ?
O5 B2 O3 B1 -146.3(4) . . . . ?
O4 B2 O3 B1 93.0(5) . . . . ?
O6 B2 O3 B1 -25.5(6) 20_675 . . . ?
O5 B2 O4 V1 -1.8(6) . . . . ?
O3 B2 O4 V1 113.6(4) . . . . ?
O6 B2 O4 V1 -127.8(3) 20_675 . . . ?
O5 B2 O4 V2 173.6(3) . . . 20_675 ?
O3 B2 O4 V2 -71.0(5) . . . 20_675 ?
O6 B2 O4 V2 47.7(5) 20_675 . . 20_675 ?
O7 B3 O5 B2 -53.1(5) . . . . ?
O2 B3 O5 B2 -173.1(4) 23_765 . . . ?
O6 B3 O5 B2 68.3(5) . . . . ?
O4 B2 O5 B3 -53.0(5) . . . . ?
O3 B2 O5 B3 -172.8(4) . . . . ?
O6 B2 O5 B3 69.9(5) 20_675 . . . ?
O5 B3 O6 B2 169.2(3) . . . 23_765 ?
O7 B3 O6 B2 -67.9(4) . . . 23_765 ?
O2 B3 O6 B2 50.8(5) 23_765 . . 23_765 ?
O5 B3 O6 V1 -27.4(5) . . . . ?
O7 B3 O6 V1 95.5(4) . . . . ?
O2 B3 O6 V1 -145.8(3) 23_765 . . . ?
O5 B3 O7 V2 175.1(3) . . . . ?
O2 B3 O7 V2 -66.3(4) 23_765 . . . ?
O6 B3 O7 V2 51.1(5) . . . . ?
O5 B3 O7 V1 -2.6(5) . . . 20_675 ?
O2 B3 O7 V1 116.0(4) 23_765 . . 20_675 ?
O6 B3 O7 V1 -126.6(3) . . . 20_675 ?
B2 O4 V1 O10 -80.7(4) . . . . ?
V2 O4 V1 O10 102.83(19) 20_675 . . . ?
B2 O4 V1 O8 172.4(4) . . . 23_765 ?
V2 O4 V1 O8 -4.04(15) 20_675 . . 23_765 ?
B2 O4 V1 O7 118.1(4) . . . 23_765 ?
V2 O4 V1 O7 -58.3(3) 20_675 . . 23_765 ?
B2 O4 V1 O6 26.4(4) . . . . ?
V2 O4 V1 O6 -150.04(15) 20_675 . . . ?
B2 O4 V1 V2 176.5(4) . . . 20_675 ?
B2 O4 V1 V2 154.0(3) . . . 23_765 ?
V2 O4 V1 V2 -22.48(16) 20_675 . . 23_765 ?
B2 O6 V1 O10 -100.1(3) 23_765 . . . ?
B3 O6 V1 O10 97.7(3) . . . . ?
B2 O6 V1 O4 151.5(3) 23_765 . . . ?
B3 O6 V1 O4 -10.6(3) . . . . ?
B2 O6 V1 O8 80.5(4) 23_765 . . 23_765 ?
B3 O6 V1 O8 -81.6(4) . . . 23_765 ?
B2 O6 V1 O7 11.0(3) 23_765 . . 23_765 ?
B3 O6 V1 O7 -151.1(3) . . . 23_765 ?
B2 O6 V1 V2 128.7(3) 23_765 . . 20_675 ?
B3 O6 V1 V2 -33.4(3) . . . 20_675 ?
B2 O6 V1 V2 33.1(3) 23_765 . . 23_765 ?
B3 O6 V1 V2 -129.1(3) . . . 23_765 ?
V2 O8 V2 O9 -123.1(4) 11_566 . . . ?
V1 O8 V2 O9 101.8(2) 20_675 . . . ?
V2 O8 V2 O8 -13.2(4) 11_566 . . 8_656 ?
V1 O8 V2 O8 -148.30(7) 20_675 . . 8_656 ?
V2 O8 V2 O7 130.9(4) 11_566 . . . ?
V1 O8 V2 O7 -4.18(15) 20_675 . . . ?
V2 O8 V2 O4 61.0(4) 11_566 . . 23_765 ?
V1 O8 V2 O4 -74.0(3) 20_675 . . 23_765 ?
V2 O8 V2 V1 10.7(4) 11_566 . . 23_765 ?
V1 O8 V2 V1 -124.38(11) 20_675 . . 23_765 ?
V2 O8 V2 V1 135.1(4) 11_566 . . 20_675 ?
B3 O7 V2 O9 80.4(4) . . . . ?
V1 O7 V2 O9 -101.4(2) 20_675 . . . ?
B3 O7 V2 O8 -95.2(4) . . . 8_656 ?
V1 O7 V2 O8 83.0(3) 20_675 . . 8_656 ?
B3 O7 V2 O8 -174.0(4) . . . . ?
V1 O7 V2 O8 4.16(15) 20_675 . . . ?
B3 O7 V2 O4 -28.0(3) . . . 23_765 ?
V1 O7 V2 O4 150.22(16) 20_675 . . 23_765 ?
B3 O7 V2 V1 -49.8(4) . . . 23_765 ?
V1 O7 V2 V1 128.34(10) 20_675 . . 23_765 ?
B3 O7 V2 V1 -178.2(4) . . . 20_675 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.40
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         2.217
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.171
