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

#######################################################################
#
#                 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_ans

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H28 B10 N6 O25.15 V3 Zn'
_chemical_formula_weight         937.05

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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.8651(19)
_cell_length_b                   13.2312(18)
_cell_length_c                   13.2880(16)
_cell_angle_alpha                61.735(14)
_cell_angle_beta                 79.118(11)
_cell_angle_gamma                65.680(14)
_cell_volume                     1674.3(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             936.3
_exptl_absorpt_coefficient_mu    1.621
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_T_max  0.9070
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_diffrn_ambient_temperature      298(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  ?
_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            11786
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0831
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         25.03
_reflns_number_total             5918
_reflns_number_gt                4414
_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)+(0.1000P)²+0.0000P] 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         5904
_refine_ls_number_parameters     490
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0615
_refine_ls_wR_factor_ref         0.1805
_refine_ls_wR_factor_gt          0.1675
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_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
Zn1 Zn 1.0000 0.5000 0.0000 0.0423(4) Uani 1 2 d S . .
V1 V 1.47781(8) 0.07334(8) 0.18924(8) 0.0105(2) Uani 1 1 d . . .
Zn2 Zn 1.5000 0.0000 0.5000 0.0265(3) Uani 1 2 d S . .
V2 V 1.27842(8) 0.21262(8) 0.01181(8) 0.0111(2) Uani 1 1 d . . .
V3 V 1.70100(8) -0.14057(8) 0.17784(8) 0.0110(2) Uani 1 1 d . . .
O1 O 1.4351(3) 0.3799(3) -0.1445(3) 0.0126(8) Uani 1 1 d . . .
O2 O 1.3670(3) 0.4226(3) -0.3200(3) 0.0154(9) Uani 1 1 d . . .
O3 O 1.6177(3) 0.2053(3) -0.0575(3) 0.0139(9) Uani 1 1 d . . .
O4 O 1.1397(3) 0.0281(4) 0.2598(4) 0.0183(9) Uani 1 1 d . . .
O5 O 1.5216(4) -0.2905(4) 0.4106(3) 0.0149(9) Uani 1 1 d . . .
O6 O 1.3416(4) -0.1182(3) 0.3257(3) 0.0137(9) Uani 1 1 d . . .
O7 O 1.2257(3) 0.1143(4) -0.0289(3) 0.0135(9) Uani 1 1 d . . .
O8 O 1.7195(3) 0.2038(3) 0.0836(3) 0.0136(9) Uani 1 1 d . . .
O9 O 1.4248(3) 0.2232(3) 0.0453(3) 0.0116(8) Uani 1 1 d . . .
O10 O 1.2723(3) -0.0736(3) 0.1472(3) 0.0127(9) Uani 1 1 d . . .
O11 O 1.7229(4) 0.2794(4) -0.2381(3) 0.0180(9) Uani 1 1 d . . .
O12 O 1.5366(3) 0.2349(3) -0.2226(3) 0.0123(8) Uani 1 1 d . . .
O13 O 1.3309(3) 0.2573(3) -0.1466(3) 0.0119(8) Uani 1 1 d . . .
O14 O 1.8095(4) -0.2166(4) 0.2696(4) 0.0237(10) Uani 1 1 d . . .
O15 O 1.3196(3) 0.0782(4) 0.1648(3) 0.0147(9) Uani 1 1 d . . .
O16 O 1.5410(3) -0.1071(3) 0.2536(3) 0.0128(9) Uani 1 1 d . . .
O17 O 1.8193(3) 0.0575(4) 0.0091(3) 0.0137(9) Uani 1 1 d . . .
O18 O 1.1592(4) 0.3240(4) 0.0208(4) 0.0221(10) Uani 1 1 d . . .
O19 O 1.0608(3) 0.0562(4) 0.0928(3) 0.0176(9) Uani 1 1 d . . .
O20 O 1.5275(3) 0.3637(3) 0.0066(3) 0.0135(9) Uani 1 1 d . . .
O21 O 1.6466(3) 0.0368(3) 0.1346(3) 0.0125(8) Uani 1 1 d . . .
O22 O 1.3540(5) 0.4988(4) -0.5155(4) 0.0358(13) Uani 1 1 d . . .
O23 O 1.4634(4) 0.1119(4) 0.2902(3) 0.0184(9) Uani 1 1 d . . .
O24 O 1.6646(4) 0.3939(4) 0.0873(4) 0.0274(11) Uani 1 1 d . . .
O25 O 0.9276(4) 0.1227(5) 0.2213(4) 0.0296(12) Uani 1 1 d . . .
B1 B 1.7060(6) 0.1206(6) 0.0466(6) 0.0145(14) Uani 1 1 d . . .
B2 B 1.1841(6) 0.0111(6) 0.0457(6) 0.0127(14) Uani 1 1 d . . .
B3 B 1.4134(6) 0.3270(6) -0.2060(6) 0.0123(14) Uani 1 1 d . . .
B4 B 1.2684(6) -0.0206(6) 0.2287(6) 0.0134(14) Uani 1 1 d . . .
B5 B 1.4654(6) -0.1847(6) 0.3051(6) 0.0123(14) Uani 1 1 d . . .
B6 B 1.6526(6) 0.2023(6) -0.1686(5) 0.0113(13) Uani 1 1 d . . .
B7 B 1.4007(6) 0.4012(6) -0.4143(6) 0.0186(15) Uani 1 1 d . . .
B8 B 1.0476(6) 0.0672(7) 0.1891(6) 0.0195(16) Uani 1 1 d . . .
B9 B 1.6360(6) 0.3189(6) 0.0590(6) 0.0146(14) Uani 1 1 d . . .
B10 B 1.4966(6) 0.2952(6) -0.0382(6) 0.0123(14) Uani 1 1 d . . .
N1 N 0.9045(5) 0.4077(5) 0.1251(5) 0.0355(15) Uani 1 1 d . C .
H1A H 0.8231 0.4489 0.1090 0.043 Uiso 1 1 calc R . .
H1B H 0.9258 0.3325 0.1284 0.043 Uiso 1 1 calc R . .
N2 N 1.0780(6) 0.4946(7) 0.1360(7) 0.052(2) Uani 1 1 d . . .
H2 H 1.1612 0.4690 0.1251 0.063 Uiso 1 1 calc R A 1
N3 N 1.0499(5) 0.7878(5) 0.1380(6) 0.0340(15) Uani 1 1 d . . .
H3A H 1.0948 0.8010 0.1737 0.051 Uiso 1 1 calc R B 1
H3B H 0.9722 0.8075 0.1625 0.051 Uiso 1 1 calc R B 1
H3C H 1.0512 0.8342 0.0630 0.051 Uiso 1 1 calc R B 1
N4 N 1.6355(5) -0.1417(6) 0.4810(5) 0.0342(15) Uani 1 1 d . . .
H4A H 1.6459 -0.2121 0.5458 0.041 Uiso 1 1 calc R . .
H4B H 1.6167 -0.1508 0.4240 0.041 Uiso 1 1 calc R . .
N5 N 1.6383(5) 0.0649(5) 0.4866(5) 0.0268(13) Uani 1 1 d . . .
H5 H 1.6290 0.0822 0.5470 0.032 Uiso 1 1 calc R . .
N6 N 1.6859(6) 0.3026(6) 0.4436(5) 0.0344(15) Uani 1 1 d . . .
H6A H 1.7415 0.3355 0.4339 0.052 Uiso 1 1 calc R . .
H6B H 1.6882 0.2464 0.5159 0.052 Uiso 1 1 calc R . .
H6C H 1.6108 0.3618 0.4272 0.052 Uiso 1 1 calc R . .
C1 C 0.9285(8) 0.3932(10) 0.2364(8) 0.057(3) Uani 1 1 d . . .
H1C H 0.9209 0.3174 0.2966 0.069 Uiso 1 1 calc R C .
H1D H 0.8682 0.4619 0.2499 0.069 Uiso 1 1 calc R . .
C2 C 1.0552(9) 0.3892(11) 0.2385(8) 0.069(3) Uani 1 1 d . C .
H2A H 1.1155 0.3116 0.2406 0.083 Uiso 1 1 calc R . .
H2B H 1.0659 0.3926 0.3073 0.083 Uiso 1 1 calc R . .
C3A C 1.0326(19) 0.6331(17) 0.1036(19) 0.034(3) Uani 0.405(10) 1 d P C 1
H3A1 H 1.0406 0.6786 0.0219 0.041 Uiso 0.405(10) 1 calc PR C 1
H3A2 H 0.9458 0.6626 0.1227 0.041 Uiso 0.405(10) 1 calc PR C 1
C4A C 1.1020(19) 0.6555(18) 0.162(2) 0.037(3) Uani 0.405(10) 1 d P C 1
H4A1 H 1.1876 0.6330 0.1383 0.044 Uiso 0.405(10) 1 calc PR C 1
H4A2 H 1.0999 0.6048 0.2440 0.044 Uiso 0.405(10) 1 calc PR C 1
C3B C 1.0391(13) 0.5819(11) 0.1855(12) 0.034(3) Uani 0.595(10) 1 d P C -1
H3B1 H 1.0839 0.5467 0.2557 0.041 Uiso 0.595(10) 1 calc PR C -1
H3B2 H 0.9509 0.6083 0.2004 0.041 Uiso 0.595(10) 1 calc PR C -1
C4B C 1.0727(13) 0.6861(13) 0.0919(13) 0.037(3) Uani 0.595(10) 1 d P C -1
H4B1 H 1.0220 0.7241 0.0248 0.044 Uiso 0.595(10) 1 calc PR C -1
H4B2 H 1.1588 0.6552 0.0714 0.044 Uiso 0.595(10) 1 calc PR C -1
C5 C 1.7496(8) -0.1152(10) 0.4541(10) 0.065(3) Uani 1 1 d . . .
H5A H 1.8202 -0.1928 0.4821 0.078 Uiso 1 1 calc R . .
H5B H 1.7569 -0.0733 0.3718 0.078 Uiso 1 1 calc R . .
C6 C 1.7533(8) -0.0384(9) 0.5042(9) 0.054(2) Uani 1 1 d . . .
H6D H 1.7703 -0.0885 0.5855 0.064 Uiso 1 1 calc R . .
H6E H 1.8198 -0.0083 0.4698 0.064 Uiso 1 1 calc R . .
C7 C 1.6276(9) 0.1814(8) 0.3815(6) 0.045(2) Uani 1 1 d . . .
H7A H 1.5441 0.2406 0.3780 0.054 Uiso 1 1 calc R . .
H7B H 1.6374 0.1643 0.3164 0.054 Uiso 1 1 calc R . .
C8 C 1.7146(8) 0.2429(8) 0.3669(7) 0.043(2) Uani 1 1 d . . .
H8A H 1.7983 0.1818 0.3821 0.051 Uiso 1 1 calc R . .
H8B H 1.7107 0.3047 0.2883 0.051 Uiso 1 1 calc R . .
O26 O 1.5001(8) -0.0001(8) 0.0000(7) 0.044(10) Uiso 0.29(2) 2 d SPR . .


_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
Zn1 N1 2.011(6) . ?
Zn1 N1 2.011(6) 2_765 ?
Zn1 N2 2.140(7) . ?
Zn1 N2 2.140(7) 2_765 ?
Zn1 O18 2.244(4) . ?
Zn1 O18 2.244(4) 2_765 ?
V1 O23 1.607(4) . ?
V1 O15 1.935(4) . ?
V1 O21 1.938(4) . ?
V1 O9 1.955(4) . ?
V1 O16 1.957(4) . ?
V1 V2 2.9920(14) . ?
V1 V3 3.0212(14) . ?
Zn2 N4 1.994(5) . ?
Zn2 N4 1.994(5) 2_856 ?
Zn2 N5 2.090(6) 2_856 ?
Zn2 N5 2.090(6) . ?
Zn2 O23 2.484(4) 2_856 ?
Zn2 O23 2.484(4) . ?
V2 O18 1.604(4) . ?
V2 O15 1.942(4) . ?
V2 O9 1.945(4) . ?
V2 O13 1.948(4) . ?
V2 O7 1.959(4) . ?
V2 V3 3.0284(13) 2_855 ?
V3 O14 1.587(4) . ?
V3 O7 1.935(4) 2_855 ?
V3 O16 1.955(4) . ?
V3 O13 1.962(4) 2_855 ?
V3 O21 1.967(4) . ?
V3 V2 3.0284(13) 2_855 ?
O1 B3 1.413(7) . ?
O1 B10 1.414(7) . ?
O2 B7 1.365(8) . ?
O2 B3 1.457(7) . ?
O3 B6 1.471(7) . ?
O3 B10 1.512(7) . ?
O3 B1 1.542(7) . ?
O4 B8 1.343(8) . ?
O4 B4 1.456(7) . ?
O5 B7 1.355(8) 2_855 ?
O5 B5 1.447(7) . ?
O6 B4 1.416(8) . ?
O6 B5 1.421(7) . ?
O7 B2 1.477(8) . ?
O7 V3 1.935(4) 2_855 ?
O8 B9 1.347(7) . ?
O8 B1 1.473(7) . ?
O9 B10 1.474(8) . ?
O10 B6 1.470(7) 2_855 ?
O10 B2 1.518(7) . ?
O10 B4 1.530(7) . ?
O11 B6 1.452(8) . ?
O12 B6 1.478(7) . ?
O12 B3 1.529(7) . ?
O12 B5 1.535(7) 2_855 ?
O13 B3 1.481(8) . ?
O13 V3 1.962(4) 2_855 ?
O15 B4 1.487(8) . ?
O16 B5 1.479(8) . ?
O17 B1 1.404(8) . ?
O17 B2 1.421(7) 2_855 ?
O19 B8 1.329(8) . ?
O19 B2 1.476(8) . ?
O20 B9 1.345(8) . ?
O20 B10 1.478(7) . ?
O21 B1 1.482(8) . ?
O22 B7 1.353(8) . ?
O24 B9 1.386(8) . ?
O25 B8 1.399(8) . ?
B2 O17 1.421(7) 2_855 ?
B5 O12 1.535(7) 2_855 ?
B6 O10 1.470(7) 2_855 ?
B7 O5 1.355(8) 2_855 ?
N1 C1 1.467(10) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 C3B 1.465(13) . ?
N2 C2 1.499(13) . ?
N2 C3A 1.537(19) . ?
N2 H2 0.9100 . ?
N3 C4A 1.48(2) . ?
N3 C4B 1.635(14) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
N4 C5 1.474(11) . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
N5 C6 1.438(10) . ?
N5 C7 1.487(9) . ?
N5 H5 0.9100 . ?
N6 C8 1.480(8) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 H6C 0.8900 . ?
C1 C2 1.487(12) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3A C4A 1.43(3) . ?
C3A H3A1 0.9700 . ?
C3A H3A2 0.9700 . ?
C4A H4A1 0.9700 . ?
C4A H4A2 0.9700 . ?
C3B C4B 1.50(2) . ?
C3B H3B1 0.9700 . ?
C3B H3B2 0.9700 . ?
C4B H4B1 0.9700 . ?
C4B H4B2 0.9700 . ?
C5 C6 1.472(11) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6D 0.9700 . ?
C6 H6E 0.9700 . ?
C7 C8 1.493(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 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
N1 Zn1 N1 180.0(6) . 2_765 ?
N1 Zn1 N2 84.5(3) . . ?
N1 Zn1 N2 95.5(3) 2_765 . ?
N1 Zn1 N2 95.5(3) . 2_765 ?
N1 Zn1 N2 84.5(3) 2_765 2_765 ?
N2 Zn1 N2 180.0(4) . 2_765 ?
N1 Zn1 O18 92.0(2) . . ?
N1 Zn1 O18 88.0(2) 2_765 . ?
N2 Zn1 O18 88.1(2) . . ?
N2 Zn1 O18 91.9(2) 2_765 . ?
N1 Zn1 O18 88.0(2) . 2_765 ?
N1 Zn1 O18 92.0(2) 2_765 2_765 ?
N2 Zn1 O18 91.9(2) . 2_765 ?
N2 Zn1 O18 88.1(2) 2_765 2_765 ?
O18 Zn1 O18 180.0 . 2_765 ?
O23 V1 O15 108.42(19) . . ?
O23 V1 O21 109.94(19) . . ?
O15 V1 O21 141.63(16) . . ?
O23 V1 O9 108.95(18) . . ?
O15 V1 O9 78.81(16) . . ?
O21 V1 O9 89.22(16) . . ?
O23 V1 O16 108.97(19) . . ?
O15 V1 O16 88.94(16) . . ?
O21 V1 O16 78.41(16) . . ?
O9 V1 O16 142.08(16) . . ?
O23 V1 V2 119.50(15) . . ?
O15 V1 V2 39.56(12) . . ?
O21 V1 V2 116.47(12) . . ?
O9 V1 V2 39.78(11) . . ?
O16 V1 V2 116.36(12) . . ?
O23 V1 V3 121.07(15) . . ?
O15 V1 V3 115.59(12) . . ?
O21 V1 V3 39.67(11) . . ?
O9 V1 V3 116.21(12) . . ?
O16 V1 V3 39.41(11) . . ?
V2 V1 V3 119.42(4) . . ?
N4 Zn2 N4 180.0(4) . 2_856 ?
N4 Zn2 N5 94.1(2) . 2_856 ?
N4 Zn2 N5 85.9(2) 2_856 2_856 ?
N4 Zn2 N5 85.9(2) . . ?
N4 Zn2 N5 94.1(2) 2_856 . ?
N5 Zn2 N5 180.0(3) 2_856 . ?
N4 Zn2 O23 90.2(2) . 2_856 ?
N4 Zn2 O23 89.8(2) 2_856 2_856 ?
N5 Zn2 O23 92.28(18) 2_856 2_856 ?
N5 Zn2 O23 87.72(18) . 2_856 ?
N4 Zn2 O23 89.8(2) . . ?
N4 Zn2 O23 90.2(2) 2_856 . ?
N5 Zn2 O23 87.72(18) 2_856 . ?
N5 Zn2 O23 92.28(18) . . ?
O23 Zn2 O23 180.000(1) 2_856 . ?
O18 V2 O15 107.8(2) . . ?
O18 V2 O9 108.43(19) . . ?
O15 V2 O9 78.87(16) . . ?
O18 V2 O13 110.3(2) . . ?
O15 V2 O13 141.90(16) . . ?
O9 V2 O13 89.48(16) . . ?
O18 V2 O7 109.3(2) . . ?
O15 V2 O7 89.75(16) . . ?
O9 V2 O7 142.26(15) . . ?
O13 V2 O7 77.54(16) . . ?
O18 V2 V1 118.71(16) . . ?
O15 V2 V1 39.39(12) . . ?
O9 V2 V1 40.01(12) . . ?
O13 V2 V1 116.94(11) . . ?
O7 V2 V1 116.88(12) . . ?
O18 V2 V3 120.74(16) . 2_855 ?
O15 V2 V3 116.41(12) . 2_855 ?
O9 V2 V3 116.96(12) . 2_855 ?
O13 V2 V3 39.42(11) . 2_855 ?
O7 V2 V3 38.66(12) . 2_855 ?
V1 V2 V3 120.53(4) . 2_855 ?
O14 V3 O7 108.1(2) . 2_855 ?
O14 V3 O16 109.9(2) . . ?
O7 V3 O16 141.94(16) 2_855 . ?
O14 V3 O13 108.4(2) . 2_855 ?
O7 V3 O13 77.78(16) 2_855 2_855 ?
O16 V3 O13 89.88(16) . 2_855 ?
O14 V3 O21 109.5(2) . . ?
O7 V3 O21 90.12(17) 2_855 . ?
O16 V3 O21 77.77(16) . . ?
O13 V3 O21 142.11(16) 2_855 . ?
O14 V3 V1 121.21(16) . . ?
O7 V3 V1 116.40(12) 2_855 . ?
O16 V3 V1 39.45(11) . . ?
O13 V3 V1 116.67(11) 2_855 . ?
O21 V3 V1 38.98(11) . . ?
O14 V3 V2 118.74(15) . 2_855 ?
O7 V3 V2 39.23(12) 2_855 2_855 ?
O16 V3 V2 116.77(11) . 2_855 ?
O13 V3 V2 39.08(11) 2_855 2_855 ?
O21 V3 V2 117.13(12) . 2_855 ?
V1 V3 V2 120.05(4) . 2_855 ?
B3 O1 B10 115.6(4) . . ?
B7 O2 B3 122.2(5) . . ?
B6 O3 B10 122.9(4) . . ?
B6 O3 B1 121.9(4) . . ?
B10 O3 B1 115.1(4) . . ?
B8 O4 B4 120.7(5) . . ?
B7 O5 B5 122.3(5) 2_855 . ?
B4 O6 B5 116.8(5) . . ?
B2 O7 V3 124.9(3) . 2_855 ?
B2 O7 V2 129.5(3) . . ?
V3 O7 V2 102.11(19) 2_855 . ?
B9 O8 B1 123.3(5) . . ?
B10 O9 V2 125.9(3) . . ?
B10 O9 V1 129.8(3) . . ?
V2 O9 V1 100.21(18) . . ?
B6 O10 B2 120.2(4) 2_855 . ?
B6 O10 B4 123.3(4) 2_855 . ?
B2 O10 B4 116.2(4) . . ?
B6 O12 B3 122.1(4) . . ?
B6 O12 B5 121.8(4) . 2_855 ?
B3 O12 B5 116.0(4) . 2_855 ?
B3 O13 V2 125.4(3) . . ?
B3 O13 V3 129.7(3) . 2_855 ?
V2 O13 V3 101.51(18) . 2_855 ?
B4 O15 V1 127.2(3) . . ?
B4 O15 V2 128.8(3) . . ?
V1 O15 V2 101.05(19) . . ?
B5 O16 V3 128.9(3) . . ?
B5 O16 V1 125.8(3) . . ?
V3 O16 V1 101.14(18) . . ?
B1 O17 B2 116.7(4) . 2_855 ?
V2 O18 Zn1 169.5(3) . . ?
B8 O19 B2 121.5(5) . . ?
B9 O20 B10 122.4(4) . . ?
B1 O21 V1 130.0(3) . . ?
B1 O21 V3 124.9(3) . . ?
V1 O21 V3 101.35(18) . . ?
V1 O23 Zn2 135.8(2) . . ?
O17 B1 O8 110.9(5) . . ?
O17 B1 O21 113.0(5) . . ?
O8 B1 O21 112.3(5) . . ?
O17 B1 O3 107.3(5) . . ?
O8 B1 O3 105.7(5) . . ?
O21 B1 O3 107.0(4) . . ?
O17 B2 O19 108.9(5) 2_855 . ?
O17 B2 O7 113.9(5) 2_855 . ?
O19 B2 O7 110.7(5) . . ?
O17 B2 O10 109.7(4) 2_855 . ?
O19 B2 O10 106.1(5) . . ?
O7 B2 O10 107.2(5) . . ?
O1 B3 O2 109.6(5) . . ?
O1 B3 O13 113.7(5) . . ?
O2 B3 O13 111.6(5) . . ?
O1 B3 O12 108.7(5) . . ?
O2 B3 O12 106.3(4) . . ?
O13 B3 O12 106.6(4) . . ?
O6 B4 O4 111.2(5) . . ?
O6 B4 O15 111.9(5) . . ?
O4 B4 O15 111.9(5) . . ?
O6 B4 O10 107.7(5) . . ?
O4 B4 O10 107.5(5) . . ?
O15 B4 O10 106.4(5) . . ?
O6 B5 O5 109.7(5) . . ?
O6 B5 O16 112.8(4) . . ?
O5 B5 O16 110.4(5) . . ?
O6 B5 O12 108.6(5) . 2_855 ?
O5 B5 O12 107.0(4) . 2_855 ?
O16 B5 O12 108.2(5) . 2_855 ?
O11 B6 O10 109.0(5) . 2_855 ?
O11 B6 O3 112.7(5) . . ?
O10 B6 O3 108.1(5) 2_855 . ?
O11 B6 O12 114.3(5) . . ?
O10 B6 O12 106.1(4) 2_855 . ?
O3 B6 O12 106.3(4) . . ?
O22 B7 O5 120.1(6) . 2_855 ?
O22 B7 O2 116.4(6) . . ?
O5 B7 O2 123.5(6) 2_855 . ?
O19 B8 O4 125.7(6) . . ?
O19 B8 O25 117.6(6) . . ?
O4 B8 O25 116.6(6) . . ?
O20 B9 O8 122.5(6) . . ?
O20 B9 O24 119.2(5) . . ?
O8 B9 O24 118.3(5) . . ?
O1 B10 O9 113.2(5) . . ?
O1 B10 O20 108.6(5) . . ?
O9 B10 O20 111.2(5) . . ?
O1 B10 O3 108.8(5) . . ?
O9 B10 O3 108.0(4) . . ?
O20 B10 O3 106.8(4) . . ?
C1 N1 Zn1 111.5(5) . . ?
C1 N1 H1A 109.3 . . ?
Zn1 N1 H1A 109.3 . . ?
C1 N1 H1B 109.3 . . ?
Zn1 N1 H1B 109.3 . . ?
H1A N1 H1B 108.0 . . ?
C3B N2 C2 97.7(8) . . ?
C3B N2 C3A 37.6(8) . . ?
C2 N2 C3A 132.0(11) . . ?
C3B N2 Zn1 131.0(7) . . ?
C2 N2 Zn1 102.5(5) . . ?
C3A N2 Zn1 101.1(9) . . ?
C3B N2 H2 110.1 . . ?
C2 N2 H2 106.3 . . ?
C3A N2 H2 106.3 . . ?
Zn1 N2 H2 106.3 . . ?
C4A N3 C4B 33.1(8) . . ?
C4A N3 H3A 109.5 . . ?
C4B N3 H3A 136.0 . . ?
C4A N3 H3B 109.5 . . ?
C4B N3 H3B 106.8 . . ?
H3A N3 H3B 109.5 . . ?
C4A N3 H3C 109.5 . . ?
C4B N3 H3C 80.1 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
C5 N4 Zn2 107.8(5) . . ?
C5 N4 H4A 110.1 . . ?
Zn2 N4 H4A 110.1 . . ?
C5 N4 H4B 110.1 . . ?
Zn2 N4 H4B 110.1 . . ?
H4A N4 H4B 108.5 . . ?
C6 N5 C7 116.7(7) . . ?
C6 N5 Zn2 105.8(5) . . ?
C7 N5 Zn2 113.4(4) . . ?
C6 N5 H5 106.8 . . ?
C7 N5 H5 106.8 . . ?
Zn2 N5 H5 106.8 . . ?
C8 N6 H6A 109.5 . . ?
C8 N6 H6B 109.5 . . ?
H6A N6 H6B 109.5 . . ?
C8 N6 H6C 109.5 . . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
N1 C1 C2 109.7(7) . . ?
N1 C1 H1C 109.7 . . ?
C2 C1 H1C 109.7 . . ?
N1 C1 H1D 109.7 . . ?
C2 C1 H1D 109.7 . . ?
H1C C1 H1D 108.2 . . ?
C1 C2 N2 111.6(8) . . ?
C1 C2 H2A 109.3 . . ?
N2 C2 H2A 109.3 . . ?
C1 C2 H2B 109.3 . . ?
N2 C2 H2B 109.3 . . ?
H2A C2 H2B 108.0 . . ?
C4A C3A N2 111.1(16) . . ?
C4A C3A H3A1 109.4 . . ?
N2 C3A H3A1 109.4 . . ?
C4A C3A H3A2 109.4 . . ?
N2 C3A H3A2 109.4 . . ?
H3A1 C3A H3A2 108.0 . . ?
C3A C4A N3 110.3(16) . . ?
C3A C4A H4A1 109.6 . . ?
N3 C4A H4A1 109.6 . . ?
C3A C4A H4A2 109.6 . . ?
N3 C4A H4A2 109.6 . . ?
H4A1 C4A H4A2 108.1 . . ?
N2 C3B C4B 101.1(10) . . ?
N2 C3B H3B1 111.5 . . ?
C4B C3B H3B1 111.5 . . ?
N2 C3B H3B2 111.5 . . ?
C4B C3B H3B2 111.5 . . ?
H3B1 C3B H3B2 109.4 . . ?
C3B C4B N3 108.3(10) . . ?
C3B C4B H4B1 110.0 . . ?
N3 C4B H4B1 110.0 . . ?
C3B C4B H4B2 110.0 . . ?
N3 C4B H4B2 110.0 . . ?
H4B1 C4B H4B2 108.4 . . ?
C6 C5 N4 113.2(7) . . ?
C6 C5 H5A 108.9 . . ?
N4 C5 H5A 108.9 . . ?
C6 C5 H5B 108.9 . . ?
N4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
N5 C6 C5 111.4(7) . . ?
N5 C6 H6D 109.3 . . ?
C5 C6 H6D 109.3 . . ?
N5 C6 H6E 109.3 . . ?
C5 C6 H6E 109.3 . . ?
H6D C6 H6E 108.0 . . ?
N5 C7 C8 118.5(7) . . ?
N5 C7 H7A 107.7 . . ?
C8 C7 H7A 107.7 . . ?
N5 C7 H7B 107.7 . . ?
C8 C7 H7B 107.7 . . ?
H7A C7 H7B 107.1 . . ?
N6 C8 C7 112.5(6) . . ?
N6 C8 H8A 109.1 . . ?
C7 C8 H8A 109.1 . . ?
N6 C8 H8B 109.1 . . ?
C7 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.000 0.495 0.500 165 35 ' '
2 0.381 0.428 0.242 35 17 ' '
3 0.619 0.572 0.758 35 17 ' '
_platon_squeeze_details          ?


_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.691
_refine_diff_density_min         -1.984
_refine_diff_density_rms         0.143

# start Validation Reply Form
_vrf_PLAT232_ans                 
;
PROBLEM: Hirshfeld Test Diff (M-X) Zn1 -- O18 .. 12.5 su 
RESPONSE: Due to the disorder of the organic amine.
;
_vrf_PLAT341_ans                 
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0163 Ang. 
RESPONSE: Disorder effect of the organic amine.
;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 1002140'
#######################################################################
#
#                 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_r-3sqd

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H86 B6 Cu3 N18 O73 P12 V12'
_chemical_formula_weight         3033.51

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'
O O 0.0106 0.0060 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   18.0955(2)
_cell_length_b                   18.0955(2)
_cell_length_c                   30.0074(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     8509.42(19)
_cell_formula_units_Z            3
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4539
_exptl_absorpt_coefficient_mu    1.761
_exptl_absorpt_correction_T_min  0.8165
_exptl_absorpt_correction_T_max  0.9171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      298(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  ?
_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            39485
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         4.28
_diffrn_reflns_theta_max         26.36
_reflns_number_total             3863
_reflns_number_gt                3035
_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)+(0.1219P)²+47.3114P] 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         3863
_refine_ls_number_parameters     240
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0674
_refine_ls_wR_factor_ref         0.2177
_refine_ls_wR_factor_gt          0.2060
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.110
_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 -0.1521(4) 0.6604(4) -0.0004(2) 0.0390(14) Uani 1 1 d . . .
C1 C -0.1755(5) 0.3971(6) 0.0152(3) 0.082(3) Uani 1 1 d . . .
H1C H -0.1763 0.3440 0.0094 0.098 Uiso 1 1 calc R . .
H1D H -0.2335 0.3868 0.0135 0.098 Uiso 1 1 calc R . .
C2 C -0.1375(6) 0.4317(7) 0.0609(3) 0.088(3) Uani 1 1 d . . .
H2A H -0.1441 0.4803 0.0680 0.105 Uiso 1 1 calc R . .
H2B H -0.1676 0.3881 0.0833 0.105 Uiso 1 1 calc R . .
C3 C -0.0341(7) 0.3949(6) 0.0820(3) 0.078(2) Uani 1 1 d . . .
H3D H 0.0225 0.4071 0.0732 0.094 Uiso 1 1 calc R . .
H3E H -0.0746 0.3387 0.0707 0.094 Uiso 1 1 calc R . .
C4 C -0.0392(8) 0.3930(6) 0.1340(3) 0.087(3) Uani 1 1 d . . .
H4A H 0.0029 0.4483 0.1456 0.104 Uiso 1 1 calc R . .
H4B H -0.0951 0.3823 0.1431 0.104 Uiso 1 1 calc R . .
N1 N -0.1207(4) 0.4626(4) -0.0171(2) 0.0643(16) Uani 1 1 d . . .
H1A H -0.1300 0.5070 -0.0162 0.077 Uiso 1 1 calc R . .
H1B H -0.1316 0.4410 -0.0449 0.077 Uiso 1 1 calc R . .
N2 N -0.0511(5) 0.4563(4) 0.0615(2) 0.0706(18) Uani 1 1 d . . .
H2 H -0.0261 0.5028 0.0796 0.085 Uiso 1 1 calc R . .
N3 N -0.0246(6) 0.3294(5) 0.1521(2) 0.084(2) Uani 1 1 d . . .
H3A H 0.0285 0.3535 0.1626 0.126 Uiso 1 1 calc R . .
H3B H -0.0317 0.2918 0.1311 0.126 Uiso 1 1 calc R . .
H3C H -0.0613 0.3029 0.1742 0.126 Uiso 1 1 calc R . .
O1 O -0.1961(2) 0.7075(2) -0.00265(12) 0.0377(9) Uani 1 1 d . . .
O2 O -0.0597(2) 0.7186(3) 0.00191(13) 0.0398(9) Uani 1 1 d . . .
O3 O -0.1713(3) 0.6038(3) -0.04027(16) 0.0497(11) Uani 1 1 d . . .
O4 O -0.1805(2) 0.6015(3) 0.03854(14) 0.0439(10) Uani 1 1 d . . .
O5 O -0.0636(3) 0.6895(3) 0.09288(14) 0.0508(11) Uani 1 1 d . . .
O6 O -0.1927(3) 0.7062(3) 0.08933(15) 0.0594(13) Uani 1 1 d . . .
O7 O -0.0667(3) 0.7202(4) -0.08974(15) 0.0674(15) Uani 1 1 d . . .
O8 O -0.2211(3) 0.6760(3) -0.09332(14) 0.0500(11) Uani 1 1 d . . .
O9A O 0.0252(3) 0.6333(3) 0.03358(17) 0.0512(12) Uani 0.941(2) 1 d P . 1
O9B O 0.008(5) 0.855(5) 0.073(3) 0.0512(12) Uani 0.059(2) 1 d P . -1
O10 O -0.2061(3) 0.5711(4) 0.12013(18) 0.0683(15) Uani 1 1 d . . .
O11 O 0.0139(4) 0.8820(4) -0.04650(18) 0.0776(17) Uani 1 1 d . . .
O12 O -0.1708(4) 0.5799(4) -0.12217(18) 0.0809(18) Uani 1 1 d . . .
P1 P -0.16156(10) 0.64080(11) 0.08675(6) 0.0458(4) Uani 1 1 d . . .
P2 P -0.15799(10) 0.64400(12) -0.08769(6) 0.0472(5) Uani 1 1 d . . .
V1A V 0.02050(6) 0.71726(6) 0.04428(3) 0.0335(3) Uani 0.941(2) 1 d P . 1
V1B V 0.0167(10) 0.7748(10) 0.0600(5) 0.0335(3) Uani 0.059(2) 1 d P . -1
V2A V 0.01649(7) 0.79475(7) -0.04484(3) 0.0383(3) Uani 0.929(2) 1 d P . 1
V2B V 0.0187(9) 0.7161(9) -0.0356(4) 0.0383(3) Uani 0.071(2) 1 d P . -1
Cu1 Cu 0.0000 0.5000 0.0000 0.0516(4) Uani 1 2 d S . .
O13 O 0.0000 1.0000 0.0000 0.113(6) Uani 1 6 d SD . .
H13 H -0.01(4) 1.03(4) 0.022(7) 0.169 Uiso 0.33 1 d PD . .


_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 O1 1.429(7) . ?
B1 O2 1.467(7) . ?
B1 O4 1.490(8) . ?
B1 O3 1.498(8) . ?
C1 N1 1.467(10) . ?
C1 C2 1.522(13) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 N2 1.394(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.431(10) . ?
C3 C4 1.563(11) . ?
C3 V2B 2.572(16) 10_565 ?
C3 H3D 0.9700 . ?
C3 H3E 0.9700 . ?
C4 N3 1.412(11) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
N1 Cu1 2.004(6) . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 Cu1 2.039(6) . ?
N2 H2 0.9100 . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 H3C 0.8900 . ?
O1 V2B 1.892(14) 11_455 ?
O1 V1A 1.936(4) 11_455 ?
O1 V2A 1.977(4) 11_455 ?
O1 V1B 2.136(16) 11_455 ?
O2 V2B 1.827(14) . ?
O2 V1A 1.938(4) . ?
O2 V2A 1.966(4) . ?
O2 V1B 2.140(16) . ?
O3 P2 1.561(5) . ?
O4 P1 1.572(5) . ?
O5 P1 1.547(4) . ?
O5 V1B 1.795(16) . ?
O5 V1A 1.982(4) . ?
O6 P1 1.546(5) . ?
O6 V2A 1.958(4) 11_455 ?
O6 V2B 2.256(14) 11_455 ?
O7 P2 1.536(5) . ?
O7 V2A 1.967(5) . ?
O7 V2B 2.269(14) . ?
O8 P2 1.526(5) . ?
O8 V1B 1.822(16) 11_455 ?
O8 V1A 1.993(4) 11_455 ?
O9A V1A 1.595(4) . ?
O9A Cu1 2.438(4) . ?
O9B V1B 1.58(7) . ?
O10 P1 1.493(5) . ?
O11 V2A 1.604(6) . ?
O12 P2 1.484(5) . ?
V1A V1B 1.177(15) . ?
V1A O1 1.936(4) 12_665 ?
V1A O8 1.993(4) 12_665 ?
V1A V2B 2.396(13) . ?
V1A V2A 3.0371(14) . ?
V1B O8 1.822(16) 12_665 ?
V1B O1 2.136(16) 12_665 ?
V1B V2B 3.07(2) . ?
V2A V2B 1.469(14) . ?
V2A O6 1.958(4) 12_665 ?
V2A O1 1.977(4) 12_665 ?
V2B O1 1.892(14) 12_665 ?
V2B O6 2.256(14) 12_665 ?
V2B C3 2.572(16) 10_565 ?
Cu1 N1 2.004(6) 10_565 ?
Cu1 N2 2.039(6) 10_565 ?
Cu1 O9A 2.438(4) 10_565 ?
O13 H13 0.91(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 B1 O2 110.5(5) . . ?
O1 B1 O4 111.5(5) . . ?
O2 B1 O4 109.7(5) . . ?
O1 B1 O3 111.3(5) . . ?
O2 B1 O3 108.6(5) . . ?
O4 B1 O3 105.0(5) . . ?
N1 C1 C2 106.2(7) . . ?
N1 C1 H1C 110.5 . . ?
C2 C1 H1C 110.5 . . ?
N1 C1 H1D 110.5 . . ?
C2 C1 H1D 110.5 . . ?
H1C C1 H1D 108.7 . . ?
N2 C2 C1 110.3(8) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N2 C3 C4 114.3(7) . . ?
N2 C3 V2B 121.6(6) . 10_565 ?
C4 C3 V2B 123.5(6) . 10_565 ?
N2 C3 H3D 108.7 . . ?
C4 C3 H3D 108.7 . . ?
V2B C3 H3D 61.1 10_565 . ?
N2 C3 H3E 108.7 . . ?
C4 C3 H3E 108.7 . . ?
V2B C3 H3E 46.6 10_565 . ?
H3D C3 H3E 107.6 . . ?
N3 C4 C3 111.8(7) . . ?
N3 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
N3 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C1 N1 Cu1 106.6(5) . . ?
C1 N1 H1A 110.4 . . ?
Cu1 N1 H1A 110.4 . . ?
C1 N1 H1B 110.4 . . ?
Cu1 N1 H1B 110.4 . . ?
H1A N1 H1B 108.6 . . ?
C2 N2 C3 113.6(8) . . ?
C2 N2 Cu1 109.3(6) . . ?
C3 N2 Cu1 117.2(6) . . ?
C2 N2 H2 105.2 . . ?
C3 N2 H2 105.2 . . ?
Cu1 N2 H2 105.2 . . ?
C4 N3 H3A 109.5 . . ?
C4 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C4 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
B1 O1 V2B 127.3(5) . 11_455 ?
B1 O1 V1A 129.4(4) . 11_455 ?
V2B O1 V1A 77.5(4) 11_455 11_455 ?
B1 O1 V2A 127.2(4) . 11_455 ?
V2B O1 V2A 44.6(4) 11_455 11_455 ?
V1A O1 V2A 101.79(17) 11_455 11_455 ?
B1 O1 V1B 128.5(5) . 11_455 ?
V2B O1 V1B 98.9(6) 11_455 11_455 ?
V1A O1 V1B 33.1(4) 11_455 11_455 ?
V2A O1 V1B 100.7(4) 11_455 11_455 ?
B1 O2 V2B 125.0(6) . . ?
B1 O2 V1A 128.0(4) . . ?
V2B O2 V1A 79.0(4) . . ?
B1 O2 V2A 128.1(4) . . ?
V2B O2 V2A 45.4(4) . . ?
V1A O2 V2A 102.13(17) . . ?
B1 O2 V1B 127.9(6) . . ?
V2B O2 V1B 100.9(6) . . ?
V1A O2 V1B 33.1(4) . . ?
V2A O2 V1B 100.9(4) . . ?
B1 O3 P2 118.7(4) . . ?
B1 O4 P1 118.7(4) . . ?
P1 O5 V1B 129.0(6) . . ?
P1 O5 V1A 124.9(3) . . ?
V1B O5 V1A 35.9(5) . . ?
P1 O6 V2A 133.2(3) . 11_455 ?
P1 O6 V2B 116.4(4) . 11_455 ?
V2A O6 V2B 40.0(4) 11_455 11_455 ?
P2 O7 V2A 134.4(3) . . ?
P2 O7 V2B 112.7(5) . . ?
V2A O7 V2B 39.8(4) . . ?
P2 O8 V1B 126.3(5) . 11_455 ?
P2 O8 V1A 125.8(3) . 11_455 ?
V1B O8 V1A 35.6(5) 11_455 11_455 ?
V1A O9A Cu1 162.3(3) . . ?
O10 P1 O6 111.3(3) . . ?
O10 P1 O5 112.5(3) . . ?
O6 P1 O5 108.1(3) . . ?
O10 P1 O4 109.4(3) . . ?
O6 P1 O4 108.1(2) . . ?
O5 P1 O4 107.2(2) . . ?
O12 P2 O8 111.5(3) . . ?
O12 P2 O7 110.6(3) . . ?
O8 P2 O7 109.1(3) . . ?
O12 P2 O3 110.1(3) . . ?
O8 P2 O3 107.9(2) . . ?
O7 P2 O3 107.5(3) . . ?
V1B V1A O9A 167.9(8) . . ?
V1B V1A O1 82.8(8) . 12_665 ?
O9A V1A O1 106.7(2) . 12_665 ?
V1B V1A O2 82.9(8) . . ?
O9A V1A O2 106.0(2) . . ?
O1 V1A O2 78.41(16) 12_665 . ?
V1B V1A O5 63.4(8) . . ?
O9A V1A O5 107.8(2) . . ?
O1 V1A O5 145.42(19) 12_665 . ?
O2 V1A O5 90.08(17) . . ?
V1B V1A O8 64.3(8) . 12_665 ?
O9A V1A O8 107.5(2) . 12_665 ?
O1 V1A O8 89.65(17) 12_665 12_665 ?
O2 V1A O8 146.39(19) . 12_665 ?
O5 V1A O8 82.13(18) . 12_665 ?
V1B V1A V2B 113.7(8) . . ?
O9A V1A V2B 78.3(4) . . ?
O1 V1A V2B 50.4(4) 12_665 . ?
O2 V1A V2B 48.5(3) . . ?
O5 V1A V2B 136.7(3) . . ?
O8 V1A V2B 138.3(4) 12_665 . ?
V1B V1A V2A 85.4(8) . . ?
O9A V1A V2A 106.69(19) . . ?
O1 V1A V2A 39.59(11) 12_665 . ?
O2 V1A V2A 39.27(12) . . ?
O5 V1A V2A 124.90(13) . . ?
O8 V1A V2A 125.15(13) 12_665 . ?
V2B V1A V2A 28.4(3) . . ?
V1A V1B O9B 170(3) . . ?
V1A V1B O5 80.8(8) . . ?
O9B V1B O5 104(3) . . ?
V1A V1B O8 80.1(8) . 12_665 ?
O9B V1B O8 108(3) . 12_665 ?
O5 V1B O8 92.4(7) . 12_665 ?
V1A V1B O1 64.1(7) . 12_665 ?
O9B V1B O1 109(3) . 12_665 ?
O5 V1B O1 144.2(9) . 12_665 ?
O8 V1B O1 88.5(7) 12_665 12_665 ?
V1A V1B O2 64.0(7) . . ?
O9B V1B O2 107(3) . . ?
O5 V1B O2 89.2(6) . . ?
O8 V1B O2 143.3(9) 12_665 . ?
O1 V1B O2 69.9(5) 12_665 . ?
V1A V1B V2B 45.7(7) . . ?
O9B V1B V2B 124(3) . . ?
O5 V1B V2B 111.1(7) . . ?
O8 V1B V2B 111.7(7) 12_665 . ?
O1 V1B V2B 37.6(4) 12_665 . ?
O2 V1B V2B 35.8(4) . . ?
V2B V2A O11 170.9(6) . . ?
V2B V2A O6 81.0(5) . 12_665 ?
O11 V2A O6 105.7(3) . 12_665 ?
V2B V2A O2 62.3(5) . . ?
O11 V2A O2 110.9(2) . . ?
O6 V2A O2 143.3(2) 12_665 . ?
V2B V2A O7 81.2(6) . . ?
O11 V2A O7 105.3(3) . . ?
O6 V2A O7 84.18(19) 12_665 . ?
O2 V2A O7 88.87(19) . . ?
V2B V2A O1 64.6(5) . 12_665 ?
O11 V2A O1 108.7(3) . 12_665 ?
O6 V2A O1 89.13(18) 12_665 12_665 ?
O2 V2A O1 76.77(16) . 12_665 ?
O7 V2A O1 145.9(2) . 12_665 ?
V2B V2A V1A 50.8(5) . . ?
O11 V2A V1A 120.1(2) . . ?
O6 V2A V1A 117.14(16) 12_665 . ?
O2 V2A V1A 38.60(11) . . ?
O7 V2A V1A 118.25(17) . . ?
O1 V2A V1A 38.62(11) 12_665 . ?
V2A V2B O2 72.3(6) . . ?
V2A V2B O1 70.8(6) . 12_665 ?
O2 V2B O1 82.3(6) . 12_665 ?
V2A V2B O6 59.0(5) . 12_665 ?
O2 V2B O6 131.3(8) . 12_665 ?
O1 V2B O6 83.0(5) 12_665 12_665 ?
V2A V2B O7 59.0(5) . . ?
O2 V2B O7 83.8(5) . . ?
O1 V2B O7 129.7(7) 12_665 . ?
O6 V2B O7 71.1(4) 12_665 . ?
V2A V2B V1A 100.8(7) . . ?
O2 V2B V1A 52.5(4) . . ?
O1 V2B V1A 52.1(3) 12_665 . ?
O6 V2B V1A 135.0(7) 12_665 . ?
O7 V2B V1A 136.3(6) . . ?
V2A V2B C3 136.1(8) . 10_565 ?
O2 V2B C3 137.8(8) . 10_565 ?
O1 V2B C3 131.2(7) 12_665 10_565 ?
O6 V2B C3 83.9(5) 12_665 10_565 ?
O7 V2B C3 88.8(5) . 10_565 ?
V1A V2B C3 122.8(6) . 10_565 ?
V2A V2B V1B 80.3(6) . . ?
O2 V2B V1B 43.3(4) . . ?
O1 V2B V1B 43.5(4) 12_665 . ?
O6 V2B V1B 122.3(6) 12_665 . ?
O7 V2B V1B 122.2(6) . . ?
V1A V2B V1B 20.6(3) . . ?
C3 V2B V1B 143.3(6) 10_565 . ?
N1 Cu1 N1 180.0(4) 10_565 . ?
N1 Cu1 N2 83.9(3) 10_565 10_565 ?
N1 Cu1 N2 96.1(3) . 10_565 ?
N1 Cu1 N2 96.1(3) 10_565 . ?
N1 Cu1 N2 83.9(3) . . ?
N2 Cu1 N2 180.0(4) 10_565 . ?
N1 Cu1 O9A 85.8(2) 10_565 . ?
N1 Cu1 O9A 94.2(2) . . ?
N2 Cu1 O9A 99.6(2) 10_565 . ?
N2 Cu1 O9A 80.4(2) . . ?
N1 Cu1 O9A 94.2(2) 10_565 10_565 ?
N1 Cu1 O9A 85.8(2) . 10_565 ?
N2 Cu1 O9A 80.4(2) 10_565 10_565 ?
N2 Cu1 O9A 99.6(2) . 10_565 ?
O9A Cu1 O9A 180.0(2) . 10_565 ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 0.000 0.000 0.168 167 28 ' '
2 0.000 0.000 0.500 355 57 ' '
3 0.000 0.000 0.832 167 28 ' '
4 0.333 0.667 0.167 355 57 ' '
5 0.333 0.667 0.834 166 28 ' '
6 0.333 0.667 0.499 166 28 ' '
7 0.667 0.333 0.833 355 57 ' '
8 0.667 0.333 0.501 166 28 ' '
9 0.667 0.333 0.166 166 28 ' '
_platon_squeeze_details          ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        26.36
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.048
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.123
_database_code_depnum_ccdc_archive 'CCDC 1002141'
#######################################################################
#
#                 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_st1_sq_d

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B20 O50 V6'
_chemical_formula_weight         1321.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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           Monoclinic
_symmetry_space_group_name_H-M   C2/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                   20.1280(11)
_cell_length_b                   13.3625(9)
_cell_length_c                   21.5590(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.256(5)
_cell_angle_gamma                90.00
_cell_volume                     5752.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2552
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9795
_exptl_absorpt_correction_T_max  0.9897

_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.6998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_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            20647
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_sigmaI/netI    0.1435
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4713
_reflns_number_gt                3106
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4713
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.2143
_refine_ls_wR_factor_gt          0.1971
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_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
B1 B 0.3729(4) 0.6143(5) 0.1086(3) 0.0198(16) Uani 1 1 d . . .
B2 B 0.4307(4) 0.7061(5) 0.0334(3) 0.0186(15) Uani 1 1 d . . .
B3 B 0.5162(4) 0.8196(5) 0.0012(4) 0.0177(15) Uani 1 1 d . . .
B4 B 0.4057(4) 0.8943(6) 0.0140(3) 0.0189(15) Uani 1 1 d . . .
B5 B 0.2368(4) 0.6191(5) -0.1500(3) 0.0144(14) Uani 1 1 d . . .
B6 B 0.1756(4) 0.5198(5) -0.0710(3) 0.0164(14) Uani 1 1 d . . .
B7 B 0.2168(4) 0.4376(6) -0.1617(4) 0.0236(17) Uani 1 1 d . . .
B8 B 0.1225(4) 0.6896(6) -0.1189(4) 0.0238(17) Uani 1 1 d . . .
B9 B 0.2876(4) 0.7035(5) 0.1677(3) 0.0164(14) Uani 1 1 d . . .
B10 B 0.3445(4) 0.5517(5) 0.2093(4) 0.0199(16) Uani 1 1 d . . .
O1 O 0.5795(2) 0.8320(3) -0.0151(2) 0.0245(10) Uani 1 1 d . . .
O2 O 0.4995(2) 0.7264(3) 0.0200(2) 0.0209(10) Uani 1 1 d . . .
O3 O 0.4738(2) 0.8988(3) -0.0015(2) 0.0216(10) Uani 1 1 d . . .
O4 O 0.4019(2) 0.8025(3) 0.0567(2) 0.0211(10) Uani 1 1 d . . .
O5 O 0.4345(2) 0.6329(3) 0.0826(2) 0.0201(10) Uani 1 1 d . . .
O6 O 0.3887(2) 0.6752(3) -0.0228(2) 0.0196(10) Uani 1 1 d . . .
O7 O 0.3210(2) 0.5740(3) 0.0607(2) 0.0215(10) Uani 1 1 d . . .
O8 O 0.3824(2) 0.5454(3) 0.1618(2) 0.0206(10) Uani 1 1 d . . .
O9 O 0.3460(2) 0.7121(3) 0.13060(19) 0.0183(10) Uani 1 1 d . . .
O10 O 0.3030(2) 0.6298(3) 0.2171(2) 0.0223(10) Uani 1 1 d . . .
O11 O 0.3483(3) 0.4725(4) 0.2503(2) 0.0301(11) Uani 1 1 d . . .
O12 O 0.2296(2) 0.6678(3) 0.12452(19) 0.0187(10) Uani 1 1 d . . .
O13 O 0.1409(2) 0.6237(3) 0.0435(2) 0.0176(9) Uani 1 1 d . . .
O14 O 0.2319(2) 0.5274(3) -0.0220(2) 0.0205(10) Uani 1 1 d . . .
O15 O 0.2982(2) 0.6344(3) -0.10558(19) 0.0181(9) Uani 1 1 d . . .
O16 O 0.2258(2) 0.7005(3) -0.1934(2) 0.0195(10) Uani 1 1 d . . .
O17 O 0.2415(2) 0.5254(3) -0.18250(19) 0.0196(10) Uani 1 1 d . . .
O18 O 0.1779(2) 0.6142(3) -0.11185(19) 0.0168(9) Uani 1 1 d . . .
O19 O 0.1121(2) 0.5193(3) -0.0466(2) 0.0188(10) Uani 1 1 d . . .
O20 O 0.1816(2) 0.4345(3) -0.1107(2) 0.0212(10) Uani 1 1 d . . .
O21 O 0.2249(3) 0.3506(4) -0.1911(2) 0.0342(13) Uani 1 1 d . . .
O22 O 0.0713(2) 0.6625(4) -0.1671(2) 0.0260(11) Uani 1 1 d . . .
O23 O 0.3639(2) 0.4594(3) -0.0425(2) 0.0262(11) Uani 1 1 d . . .
O24 O 0.2188(2) 0.4548(3) 0.1048(2) 0.0277(11) Uani 1 1 d . . .
O25 O 0.0957(3) 0.7351(4) 0.1433(2) 0.0284(11) Uani 1 1 d . . .
V1 V 0.22653(6) 0.55692(7) 0.06629(5) 0.0171(3) Uani 1 1 d . . .
V2 V 0.32513(5) 0.56243(7) -0.02854(5) 0.0163(3) Uani 1 1 d . . .
V3 V 0.14879(5) 0.74342(8) 0.09454(5) 0.0169(3) Uani 1 1 d . . .


_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 O8 1.464(8) . ?
B1 O5 1.447(9) . ?
B1 O7 1.475(9) . ?
B1 O9 1.513(9) . ?
B2 O5 1.437(9) . ?
B2 O6 1.447(9) . ?
B2 O2 1.477(9) . ?
B2 O4 1.524(9) . ?
B3 O3 1.356(9) . ?
B3 O2 1.364(8) . ?
B3 O1 1.374(9) . ?
B4 O19 1.421(9) 7_565 ?
B4 O3 1.454(9) . ?
B4 O13 1.475(8) 7_565 ?
B4 O4 1.541(8) . ?
B5 O16 1.434(8) . ?
B5 O17 1.444(8) . ?
B5 O15 1.479(9) . ?
B5 O18 1.527(8) . ?
B6 O20 1.439(8) . ?
B6 O14 1.451(9) . ?
B6 O19 1.444(8) . ?
B6 O18 1.542(8) . ?
B7 O21 1.343(9) . ?
B7 O20 1.383(9) . ?
B7 O17 1.373(9) . ?
B8 O22 1.414(10) . ?
B8 O9 1.493(9) 7_565 ?
B8 O4 1.491(9) 7_565 ?
B8 O18 1.496(9) . ?
B9 O16 1.436(8) 7_565 ?
B9 O10 1.455(8) . ?
B9 O12 1.478(9) . ?
B9 O9 1.508(9) . ?
B10 O8 1.354(9) . ?
B10 O10 1.360(9) . ?
B10 O11 1.375(9) . ?
O4 B8 1.491(9) 7_565 ?
O6 V3 1.962(5) 7_565 ?
O6 V2 1.970(4) . ?
O7 V1 1.934(5) . ?
O7 V2 1.942(4) . ?
O9 B8 1.493(9) 7_565 ?
O12 V1 1.938(4) . ?
O12 V3 1.954(4) . ?
O13 B4 1.475(8) 7_565 ?
O13 V3 1.937(4) . ?
O13 V1 1.948(4) . ?
O14 V1 1.960(4) . ?
O14 V2 1.957(5) . ?
O15 V2 1.936(4) . ?
O15 V3 1.948(4) 7_565 ?
O16 B9 1.436(8) 7_565 ?
O19 B4 1.421(9) 7_565 ?
O23 V2 1.629(5) . ?
O24 V1 1.615(5) . ?
O25 V3 1.594(5) . ?
V1 V2 3.0247(15) . ?
V1 V3 3.0447(15) . ?
V2 V3 3.0362(14) 7_565 ?
V3 O15 1.948(4) 7_565 ?
V3 O6 1.962(5) 7_565 ?
V3 V2 3.0362(14) 7_565 ?

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
O8 B1 O5 112.2(5) . . ?
O8 B1 O7 109.3(5) . . ?
O5 B1 O7 110.9(5) . . ?
O8 B1 O9 108.4(5) . . ?
O5 B1 O9 109.3(5) . . ?
O7 B1 O9 106.6(5) . . ?
O5 B2 O6 113.3(6) . . ?
O5 B2 O2 107.8(5) . . ?
O6 B2 O2 110.6(5) . . ?
O5 B2 O4 108.7(5) . . ?
O6 B2 O4 108.1(5) . . ?
O2 B2 O4 108.3(5) . . ?
O3 B3 O2 123.3(6) . . ?
O3 B3 O1 119.5(6) . . ?
O2 B3 O1 117.2(6) . . ?
O19 B4 O3 112.6(5) 7_565 . ?
O19 B4 O13 112.1(6) 7_565 7_565 ?
O3 B4 O13 109.4(5) . 7_565 ?
O19 B4 O4 108.4(5) 7_565 . ?
O3 B4 O4 106.8(5) . . ?
O13 B4 O4 107.3(5) 7_565 . ?
O16 B5 O17 110.8(5) . . ?
O16 B5 O15 111.4(5) . . ?
O17 B5 O15 109.4(5) . . ?
O16 B5 O18 108.5(5) . . ?
O17 B5 O18 109.1(5) . . ?
O15 B5 O18 107.4(5) . . ?
O20 B6 O14 111.9(5) . . ?
O20 B6 O19 110.9(5) . . ?
O14 B6 O19 112.4(5) . . ?
O20 B6 O18 107.3(5) . . ?
O14 B6 O18 106.4(5) . . ?
O19 B6 O18 107.7(5) . . ?
O21 B7 O20 117.1(6) . . ?
O21 B7 O17 121.0(6) . . ?
O20 B7 O17 121.9(6) . . ?
O22 B8 O9 112.8(5) . 7_565 ?
O22 B8 O4 112.7(6) . 7_565 ?
O9 B8 O4 106.5(5) 7_565 7_565 ?
O22 B8 O18 111.5(6) . . ?
O9 B8 O18 106.5(5) 7_565 . ?
O4 B8 O18 106.4(5) 7_565 . ?
O16 B9 O10 110.8(5) 7_565 . ?
O16 B9 O12 111.1(5) 7_565 . ?
O10 B9 O12 108.7(5) . . ?
O16 B9 O9 109.5(5) 7_565 . ?
O10 B9 O9 109.3(5) . . ?
O12 B9 O9 107.3(5) . . ?
O8 B10 O10 123.6(6) . . ?
O8 B10 O11 116.6(6) . . ?
O10 B10 O11 119.8(6) . . ?
B3 O2 B2 119.9(5) . . ?
B3 O3 B4 124.3(5) . . ?
B8 O4 B2 122.5(5) 7_565 . ?
B8 O4 B4 121.9(5) 7_565 . ?
B2 O4 B4 115.3(5) . . ?
B2 O5 B1 115.7(5) . . ?
B2 O6 V3 128.9(4) . 7_565 ?
B2 O6 V2 125.2(4) . . ?
V3 O6 V2 101.1(2) 7_565 . ?
B1 O7 V1 127.9(4) . . ?
B1 O7 V2 127.4(4) . . ?
V1 O7 V2 102.6(2) . . ?
B10 O8 B1 121.5(5) . . ?
B8 O9 B1 122.1(5) 7_565 . ?
B8 O9 B9 122.2(5) 7_565 . ?
B1 O9 B9 115.7(5) . . ?
B10 O10 B9 120.5(5) . . ?
B9 O12 V1 127.8(4) . . ?
B9 O12 V3 126.8(4) . . ?
V1 O12 V3 103.0(2) . . ?
B4 O13 V3 127.6(4) 7_565 . ?
B4 O13 V1 125.8(4) 7_565 . ?
V3 O13 V1 103.2(2) . . ?
B6 O14 V1 126.0(4) . . ?
B6 O14 V2 129.1(4) . . ?
V1 O14 V2 101.1(2) . . ?
B5 O15 V2 127.4(4) . . ?
B5 O15 V3 126.5(4) . 7_565 ?
V2 O15 V3 102.8(2) . 7_565 ?
B5 O16 B9 116.5(5) . 7_565 ?
B7 O17 B5 122.3(5) . . ?
B8 O18 B5 122.4(4) . . ?
B8 O18 B6 122.2(5) . . ?
B5 O18 B6 115.1(4) . . ?
B4 O19 B6 117.8(5) 7_565 . ?
B7 O20 B6 122.6(5) . . ?
O24 V1 O12 108.0(2) . . ?
O24 V1 O7 106.9(2) . . ?
O12 V1 O7 89.96(18) . . ?
O24 V1 O13 112.2(2) . . ?
O12 V1 O13 76.61(18) . . ?
O7 V1 O13 140.88(18) . . ?
O24 V1 O14 110.5(2) . . ?
O12 V1 O14 141.44(18) . . ?
O7 V1 O14 77.77(18) . . ?
O13 V1 O14 90.13(19) . . ?
O24 V1 V2 118.83(17) . . ?
O12 V1 V2 116.71(13) . . ?
O7 V1 V2 38.79(13) . . ?
O13 V1 V2 116.96(13) . . ?
O14 V1 V2 39.42(14) . . ?
O24 V1 V3 120.22(17) . . ?
O12 V1 V3 38.72(13) . . ?
O7 V1 V3 116.74(14) . . ?
O13 V1 V3 38.29(13) . . ?
O14 V1 V3 116.85(14) . . ?
V2 V1 V3 120.85(4) . . ?
O23 V2 O15 110.5(2) . . ?
O23 V2 O7 109.3(2) . . ?
O15 V2 O7 140.14(19) . . ?
O23 V2 O14 107.3(2) . . ?
O15 V2 O14 90.77(18) . . ?
O7 V2 O14 77.64(19) . . ?
O23 V2 O6 109.6(2) . . ?
O15 V2 O6 77.50(18) . . ?
O7 V2 O6 89.17(18) . . ?
O14 V2 O6 143.08(19) . . ?
O23 V2 V1 118.32(17) . . ?
O15 V2 V1 117.09(13) . . ?
O7 V2 V1 38.60(14) . . ?
O14 V2 V1 39.49(13) . . ?
O6 V2 V1 116.88(13) . . ?
O23 V2 V3 121.37(17) . 7_565 ?
O15 V2 V3 38.74(13) . 7_565 ?
O7 V2 V3 115.32(14) . 7_565 ?
O14 V2 V3 117.54(14) . 7_565 ?
O6 V2 V3 39.36(13) . 7_565 ?
V1 V2 V3 120.30(4) . 7_565 ?
O25 V3 O13 107.6(2) . . ?
O25 V3 O15 112.3(2) . 7_565 ?
O13 V3 O15 140.00(18) . 7_565 ?
O25 V3 O12 110.1(2) . . ?
O13 V3 O12 76.47(18) . . ?
O15 V3 O12 88.46(18) 7_565 . ?
O25 V3 O6 109.6(2) . 7_565 ?
O13 V3 O6 90.80(18) . 7_565 ?
O15 V3 O6 77.39(18) 7_565 7_565 ?
O12 V3 O6 140.21(19) . 7_565 ?
O25 V3 V1 118.59(18) . . ?
O13 V3 V1 38.54(13) . . ?
O15 V3 V1 115.02(14) 7_565 . ?
O12 V3 V1 38.33(13) . . ?
O6 V3 V1 116.87(13) 7_565 . ?
O25 V3 V2 122.60(18) . 7_565 ?
O13 V3 V2 116.49(13) . 7_565 ?
O15 V3 V2 38.46(13) 7_565 7_565 ?
O12 V3 V2 114.28(13) . 7_565 ?
O6 V3 V2 39.54(13) 7_565 7_565 ?
V1 V3 V2 118.82(4) . 7_565 ?

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.025 -0.014 0.011 2323 459 ' '
_platon_squeeze_details          ?


_diffrn_measured_fraction_theta_max 0.927
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.927
_refine_diff_density_max         1.071
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.137
# start Validation Reply Form
_vrf_PLAT029_st1_sq_d            
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.927 Note 
RESPONSE: Due to the small crystal size, we tried our best to get 
this reasonable data for this phase in synchrotron light source 
Diamond I19.However, due to the relatively large unit cell and 
low symmetry, the completeness of this dataset is still lacking,
 but it should be enough to confirm the cluster type.    
;
_database_code_depnum_ccdc_archive 'CCDC 1002142'
