# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2011

data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
#Added by publCIF

_publ_section_title              
;
Title [H~2~N(C~2~H~4~)~2~NH~2~]~1.5
~[(VO)~3~(AsO~4~)F~4~][VF~3~(AsO~4~)].4H~2~O
;

_publ_contact_author_address     
;Department of Chemistry
University of Southampton
Southampton
SO!7 1BJ, UK
;

_publ_contact_author_email       mtw@soton.ac.uk

_publ_contact_author_name        'Weller Mark T.'

_publ_contact_letter             
;
Submission dated :2011-02-10
;
loop_
_publ_author_name
'Eleni Kotsapa'
'Mark Weller'
'Mark Light'

data_2009ek00166trip-1
_database_code_depnum_ccdc_archive 'CCDC 812051'
#TrackingRef '- compound12009ek00166rev1.cif'

_publ_section_exptl_prep         
;
Vanadium(V) oxide (0.1046 g, 0.575 mmol), 85% orthoarsenic acid solution (0.04
mL, 0.575 mmol), 48% hydrofluoric acid solution (0.05 mL, 1.38 mmol),
piperazine (0.0991 g, 1.15 mmol) and distilled water (3 mL, 166.6 mmol) were
mixed in the Teflon liner of a Parr 23 ml hydrothermal vessel; the
final reaction mixture pH was 5.24. The hydrothermal vessel was sealed and
heated to 418 K for 4 days. The pure solid product formed as very dark blue
crystals and was isolated by filtration, washed with distilled water and dried
at 60\%C. SEM/EDAX analysis gave V:As ratio of 1.54:1; theoretical 1.5:1.
;
#Added by publCIF

_audit_update_record             
;
2011-02-09 # Formatted by publCIF
;

_chemical_compound_source        ?

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H21 As2 F3 N3 O13 V3'
_chemical_formula_weight         702.92

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'

_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                   8.5594(2)
_cell_length_b                   10.8001(2)
_cell_length_c                   12.0616(2)
_cell_angle_alpha                65.5917(14)
_cell_angle_beta                 79.8934(13)
_cell_angle_gamma                72.0654(14)
_cell_volume                     964.51(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    13957
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             688
_exptl_absorpt_coefficient_mu    4.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6386
_exptl_absorpt_correction_T_max  0.6386
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15708
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         25.03
_reflns_number_total             3397
_reflns_number_gt                3000
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
Images generated using CrystalMaker: a crystal and molecular
structures program for Mac and Windows. CrystalMaker Software Ltd,
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'
_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^ > 2\s(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.
The hydrogen atoms of the protonated piperazine (the second of which lies
on an inversion centre) were all clearly located in the difference map
and subsequently placed in idealized positions and treated using a riding
model approximation with U(H) fixed at 1.2Ueq of the parent atom. The
coordinates for hydrogen atoms of the water OW1 and the hydroxyl hydrogen
of O6 were obtained from the difference map and subsequently treated as
riding on the parent atom, the U(iso) values were freely refined.

;

_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^)+(0.0000P)^2^+3.8059P] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3397
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0621
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_restrained_S_all      1.109
_refine_ls_shift/su_max          0.003
_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
As1 As 0.49250(5) 0.23210(4) 0.05434(3) 0.00743(10) Uani 1 1 d . . .
As2 As 0.52000(5) 0.76962(4) 0.35188(3) 0.00878(10) Uani 1 1 d . . .
V1 V 0.62947(8) 0.43973(7) 0.11780(6) 0.00770(15) Uani 1 1 d . . .
V2 V 0.64004(8) 0.43251(7) 0.40763(6) 0.00745(15) Uani 1 1 d . . .
V3 V 0.66030(8) 0.02433(7) -0.09314(6) 0.00778(15) Uani 1 1 d . . .
F1 F 0.3834(2) 0.5466(2) 0.43457(18) 0.0089(4) Uani 1 1 d . . .
F2 F 0.3812(2) 0.5505(2) 0.05415(19) 0.0091(4) Uani 1 1 d . . .
F3 F 0.6070(2) -0.0988(2) 0.07078(19) 0.0102(5) Uani 1 1 d . . .
O1 O 0.6494(3) 0.1761(3) -0.0341(2) 0.0098(6) Uani 1 1 d . . .
O2 O 0.8320(3) 0.3537(3) 0.4034(2) 0.0128(6) Uani 1 1 d . . .
O3 O 0.8559(3) -0.0365(3) -0.1021(2) 0.0123(6) Uani 1 1 d . . .
O4 O 0.6635(3) 0.6313(3) 0.3343(2) 0.0101(6) Uani 1 1 d . . .
O5 O 0.5661(3) 0.4523(3) 0.2575(2) 0.0088(5) Uani 1 1 d . . .
O6 O 0.6220(3) 0.8961(3) 0.3191(2) 0.0143(6) Uani 1 1 d . . .
H901 H 0.5722 0.9607 0.2832 0.021 Uiso 1 1 d R . .
O7 O 0.4090(3) 0.0987(3) 0.1501(2) 0.0091(5) Uani 1 1 d . . .
O8 O 0.5538(3) 0.2719(3) 0.1592(2) 0.0089(5) Uani 1 1 d . . .
O9 O 0.3427(3) 0.3675(3) -0.0284(2) 0.0096(6) Uani 1 1 d . . .
O10 O 0.5504(3) 0.2637(3) 0.5012(2) 0.0096(6) Uani 1 1 d . . .
O11 O 0.8216(3) 0.3638(3) 0.1315(2) 0.0110(6) Uani 1 1 d . . .
O12 O 0.3610(3) 0.8339(3) 0.2640(2) 0.0104(6) Uani 1 1 d . . .
N1 N 0.1991(4) 0.6210(3) 0.2464(3) 0.0112(7) Uani 1 1 d . . .
H1A H 0.2662 0.5891 0.3097 0.013 Uiso 1 1 d R . .
H1B H 0.2597 0.6524 0.1743 0.013 Uiso 1 1 d R . .
N2 N -0.1067(4) 0.6828(4) 0.1448(3) 0.0181(8) Uani 1 1 d . . .
H2A H -0.1791 0.6582 0.2111 0.022 Uiso 1 1 d R . .
H2B H -0.1633 0.7169 0.0755 0.022 Uiso 1 1 d R . .
C1 C 0.0580(5) 0.7381(4) 0.2554(4) 0.0162(9) Uani 1 1 d . . .
H1C H 0.0983 0.8132 0.2585 0.019 Uiso 1 1 calc R . .
H1D H -0.0106 0.7034 0.3310 0.019 Uiso 1 1 calc R . .
C2 C -0.0423(5) 0.7958(4) 0.1463(4) 0.0178(9) Uani 1 1 d . . .
H2C H -0.1351 0.8762 0.1497 0.021 Uiso 1 1 calc R . .
H2D H 0.0266 0.8299 0.0709 0.021 Uiso 1 1 calc R . .
C3 C 0.0275(5) 0.5554(5) 0.1479(4) 0.0193(9) Uani 1 1 d . . .
H3C H 0.0942 0.5777 0.0697 0.023 Uiso 1 1 calc R . .
H3D H -0.0212 0.4794 0.1567 0.023 Uiso 1 1 calc R . .
C4 C 0.1372(5) 0.5042(4) 0.2513(4) 0.0189(9) Uani 1 1 d . . .
H4A H 0.0749 0.4687 0.3300 0.023 Uiso 1 1 calc R . .
H4B H 0.2312 0.4257 0.2457 0.023 Uiso 1 1 calc R . .
N3 N 0.1724(5) -0.0026(4) 0.4715(3) 0.0248(9) Uani 1 1 d . . .
H3A H 0.2531 0.0447 0.4476 0.030 Uiso 1 1 d R . .
H3B H 0.2218 -0.0952 0.4825 0.030 Uiso 1 1 d R . .
C5 C 0.0524(5) 0.0609(5) 0.3738(4) 0.0229(10) Uani 1 1 d . . .
H5A H 0.1092 0.0477 0.2990 0.027 Uiso 1 1 calc R . .
H5B H 0.0104 0.1634 0.3543 0.027 Uiso 1 1 calc R . .
C6 C 0.0899(6) 0.0048(5) 0.5879(4) 0.0264(11) Uani 1 1 d . . .
H6A H 0.0497 0.1046 0.5788 0.032 Uiso 1 1 calc R . .
H6B H 0.1704 -0.0446 0.6522 0.032 Uiso 1 1 calc R . .
OW1 O 0.3764(4) 0.1692(3) 0.3860(3) 0.0209(7) Uani 1 1 d . . .
H902 H 0.4210 0.1890 0.3230 0.031 Uiso 1 1 d R . .
H903 H 0.4180 0.1890 0.4300 0.031 Uiso 1 1 d R . .

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
As1 0.0095(2) 0.0065(2) 0.0073(2) -0.00296(15) -0.00050(15) -0.00286(15)
As2 0.0107(2) 0.0078(2) 0.0077(2) -0.00245(15) -0.00056(15) -0.00315(15)
V1 0.0086(3) 0.0069(3) 0.0084(3) -0.0028(3) -0.0016(3) -0.0026(3)
V2 0.0082(3) 0.0073(3) 0.0066(3) -0.0026(3) -0.0004(2) -0.0018(3)
V3 0.0082(3) 0.0073(3) 0.0086(3) -0.0035(3) -0.0005(3) -0.0025(3)
F1 0.0081(11) 0.0095(11) 0.0090(11) -0.0033(9) -0.0018(8) -0.0017(8)
F2 0.0107(11) 0.0075(11) 0.0095(11) -0.0037(9) 0.0008(9) -0.0032(9)
F3 0.0096(11) 0.0106(11) 0.0100(11) -0.0038(9) -0.0008(9) -0.0021(9)
O1 0.0102(13) 0.0100(14) 0.0116(14) -0.0072(11) 0.0019(11) -0.0032(11)
O2 0.0113(14) 0.0114(14) 0.0141(15) -0.0054(12) 0.0000(11) -0.0002(11)
O3 0.0114(14) 0.0133(14) 0.0112(14) -0.0045(12) 0.0001(11) -0.0028(11)
O4 0.0112(14) 0.0082(14) 0.0106(14) -0.0033(11) 0.0029(11) -0.0045(11)
O5 0.0140(14) 0.0081(13) 0.0055(13) -0.0024(11) -0.0013(10) -0.0042(11)
O6 0.0170(15) 0.0083(14) 0.0168(15) -0.0034(12) -0.0004(12) -0.0045(11)
O7 0.0111(13) 0.0071(13) 0.0113(14) -0.0044(11) 0.0025(11) -0.0059(11)
O8 0.0140(14) 0.0098(14) 0.0057(13) -0.0030(11) -0.0016(11) -0.0063(11)
O9 0.0103(13) 0.0077(14) 0.0112(14) -0.0021(11) -0.0031(11) -0.0035(11)
O10 0.0154(14) 0.0083(14) 0.0052(13) -0.0016(11) -0.0003(11) -0.0046(11)
O11 0.0110(14) 0.0097(14) 0.0126(14) -0.0039(11) -0.0012(11) -0.0033(11)
O12 0.0083(13) 0.0117(14) 0.0099(14) -0.0021(11) -0.0032(11) -0.0021(11)
N1 0.0121(17) 0.0163(18) 0.0070(16) -0.0051(14) 0.0007(13) -0.0058(14)
N2 0.0102(17) 0.030(2) 0.0121(18) -0.0066(16) -0.0006(14) -0.0050(15)
C1 0.014(2) 0.018(2) 0.019(2) -0.0099(18) 0.0019(17) -0.0060(17)
C2 0.014(2) 0.018(2) 0.019(2) -0.0024(18) -0.0001(17) -0.0080(17)
C3 0.015(2) 0.030(3) 0.024(2) -0.021(2) 0.0028(18) -0.0093(19)
C4 0.018(2) 0.016(2) 0.021(2) -0.0049(18) -0.0007(18) -0.0060(18)
N3 0.023(2) 0.021(2) 0.032(2) -0.0143(18) 0.0060(17) -0.0058(16)
C5 0.024(2) 0.023(2) 0.021(2) -0.013(2) 0.0034(19) -0.0017(19)
C6 0.028(3) 0.031(3) 0.026(3) -0.017(2) -0.002(2) -0.009(2)
OW1 0.0284(17) 0.0285(18) 0.0124(15) -0.0103(13) 0.0007(13) -0.0137(14)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
As1 O1 1.685(2) . ?
As1 O9 1.693(3) . ?
As1 O8 1.697(2) . ?
As1 O7 1.700(2) . ?
As2 O12 1.665(2) . ?
As2 O4 1.681(3) . ?
As2 O10 1.693(2) 2_666 ?
As2 O6 1.718(3) . ?
V1 O11 1.599(3) . ?
V1 O5 1.724(3) . ?
V1 O8 1.954(3) . ?
V1 O9 1.978(3) 2_665 ?
V1 F2 2.050(2) 2_665 ?
V1 F2 2.187(2) . ?
V2 O2 1.604(3) . ?
V2 O5 1.930(3) . ?
V2 F1 1.976(2) 2_666 ?
V2 O10 2.011(3) . ?
V2 O4 2.016(3) . ?
V2 F1 2.205(2) . ?
V3 O3 1.601(3) . ?
V3 F3 1.942(2) . ?
V3 O7 1.993(3) 2_655 ?
V3 O12 1.994(3) 2_665 ?
V3 O1 2.012(3) . ?
V3 F3 2.187(2) 2_655 ?
F1 V2 1.976(2) 2_666 ?
F2 V1 2.050(2) 2_665 ?
F3 V3 2.187(2) 2_655 ?
O7 V3 1.993(3) 2_655 ?
O9 V1 1.978(3) 2_665 ?
O10 As2 1.693(2) 2_666 ?
O12 V3 1.994(3) 2_665 ?
N1 C1 1.483(5) . ?
N1 C4 1.488(5) . ?
N2 C3 1.488(5) . ?
N2 C2 1.493(5) . ?
C1 C2 1.499(6) . ?
C3 C4 1.505(6) . ?
N3 C6 1.478(6) . ?
N3 C5 1.496(6) . ?
C5 C6 1.505(6) 2_556 ?
C6 C5 1.505(6) 2_556 ?

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 As1 O9 112.45(13) . . ?
O1 As1 O8 113.29(12) . . ?
O9 As1 O8 110.97(12) . . ?
O1 As1 O7 111.09(12) . . ?
O9 As1 O7 109.04(12) . . ?
O8 As1 O7 99.20(12) . . ?
O12 As2 O4 114.91(13) . . ?
O12 As2 O10 109.29(13) . 2_666 ?
O4 As2 O10 112.65(12) . 2_666 ?
O12 As2 O6 110.13(13) . . ?
O4 As2 O6 105.34(13) . . ?
O10 As2 O6 103.86(12) 2_666 . ?
O11 V1 O5 102.80(13) . . ?
O11 V1 O8 97.69(12) . . ?
O5 V1 O8 94.28(11) . . ?
O11 V1 O9 95.38(12) . 2_665 ?
O5 V1 O9 97.40(11) . 2_665 ?
O8 V1 O9 160.09(11) . 2_665 ?
O11 V1 F2 96.90(11) . 2_665 ?
O5 V1 F2 160.13(11) . 2_665 ?
O8 V1 F2 80.42(9) . 2_665 ?
O9 V1 F2 83.16(9) 2_665 2_665 ?
O11 V1 F2 166.53(11) . . ?
O5 V1 F2 90.48(10) . . ?
O8 V1 F2 83.34(9) . . ?
O9 V1 F2 80.50(9) 2_665 . ?
F2 V1 F2 69.95(9) 2_665 . ?
O2 V2 O5 103.82(12) . . ?
O2 V2 F1 100.47(11) . 2_666 ?
O5 V2 F1 155.71(10) . 2_666 ?
O2 V2 O10 99.18(12) . . ?
O5 V2 O10 90.90(10) . . ?
F1 V2 O10 85.30(9) 2_666 . ?
O2 V2 O4 97.28(12) . . ?
O5 V2 O4 91.77(11) . . ?
F1 V2 O4 85.03(10) 2_666 . ?
O10 V2 O4 162.17(11) . . ?
O2 V2 F1 172.04(11) . . ?
O5 V2 F1 83.94(10) . . ?
F1 V2 F1 71.78(9) 2_666 . ?
O10 V2 F1 82.24(9) . . ?
O4 V2 F1 80.52(9) . . ?
O3 V3 F3 100.86(11) . . ?
O3 V3 O7 100.02(12) . 2_655 ?
F3 V3 O7 86.29(10) . 2_655 ?
O3 V3 O12 96.70(12) . 2_665 ?
F3 V3 O12 162.01(10) . 2_665 ?
O7 V3 O12 86.84(11) 2_655 2_665 ?
O3 V3 O1 98.97(12) . . ?
F3 V3 O1 90.92(10) . . ?
O7 V3 O1 161.00(11) 2_655 . ?
O12 V3 O1 90.18(11) 2_665 . ?
O3 V3 F3 176.89(12) . 2_655 ?
F3 V3 F3 76.03(9) . 2_655 ?
O7 V3 F3 79.90(9) 2_655 2_655 ?
O12 V3 F3 86.40(9) 2_665 2_655 ?
O1 V3 F3 81.18(9) . 2_655 ?
V2 F1 V2 108.22(9) 2_666 . ?
V1 F2 V1 110.05(9) 2_665 . ?
V3 F3 V3 103.97(9) . 2_655 ?
As1 O1 V3 124.01(14) . . ?
As2 O4 V2 123.98(14) . . ?
V1 O5 V2 144.45(15) . . ?
As1 O7 V3 122.93(14) . 2_655 ?
As1 O8 V1 123.36(14) . . ?
As1 O9 V1 122.33(14) . 2_665 ?
As2 O10 V2 119.60(13) 2_666 . ?
As2 O12 V3 128.77(15) . 2_665 ?
C1 N1 C4 109.4(3) . . ?
C3 N2 C2 112.0(3) . . ?
N1 C1 C2 108.8(3) . . ?
N2 C2 C1 109.4(3) . . ?
N2 C3 C4 111.8(3) . . ?
N1 C4 C3 110.2(3) . . ?
C6 N3 C5 111.1(3) . . ?
N3 C5 C6 111.7(4) . 2_556 ?
N3 C6 C5 111.7(4) . 2_556 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.114

_iucr_refine_instruction_details 
;
TITL 2009ek00166triP-1 in P-1
CELL 0.71073 8.5594 10.8001 12.0616 65.5917 79.8934 72.0654
ZERR 2.00 0.0002 0.0002 0.0002 0.0014 0.0013 0.0014
LATT 1
SFAC C H As F N O V
UNIT 12 42 4 6 6 26 6

MERG 2
SHEL 7 0.84
FMAP 2
PLAN 25
SIZE 0.10 0.10 0.10
ACTA
BOND
L.S. 4
TEMP -153.00
WGHT 0.000000 3.805900
FVAR 0.45369
AS1 3 0.492495 0.232100 0.054344 11.00000 0.00949 0.00648 =
0.00725 -0.00296 -0.00050 -0.00286
AS2 3 0.520004 0.769617 0.351882 11.00000 0.01074 0.00784 =
0.00774 -0.00245 -0.00056 -0.00315
V1 7 0.629467 0.439732 0.117801 11.00000 0.00863 0.00692 =
0.00835 -0.00284 -0.00164 -0.00261
V2 7 0.640036 0.432506 0.407631 11.00000 0.00817 0.00727 =
0.00662 -0.00260 -0.00036 -0.00175
V3 7 0.660303 0.024330 -0.093141 11.00000 0.00817 0.00734 =
0.00864 -0.00353 -0.00051 -0.00247
F1 4 0.383405 0.546620 0.434574 11.00000 0.00807 0.00946 =
0.00899 -0.00329 -0.00178 -0.00169
F2 4 0.381203 0.550510 0.054152 11.00000 0.01069 0.00755 =
0.00946 -0.00367 0.00081 -0.00322
F3 4 0.606988 -0.098809 0.070784 11.00000 0.00963 0.01063 =
0.01001 -0.00383 -0.00075 -0.00214
O1 6 0.649410 0.176096 -0.034090 11.00000 0.01022 0.00998 =
0.01162 -0.00717 0.00186 -0.00321
O2 6 0.832035 0.353689 0.403378 11.00000 0.01126 0.01136 =
0.01407 -0.00542 -0.00001 -0.00019
O3 6 0.855857 -0.036503 -0.102136 11.00000 0.01139 0.01334 =
0.01122 -0.00449 0.00015 -0.00282
O4 6 0.663456 0.631287 0.334266 11.00000 0.01124 0.00818 =
0.01056 -0.00326 0.00295 -0.00450
O5 6 0.566074 0.452329 0.257450 11.00000 0.01400 0.00810 =
0.00546 -0.00240 -0.00133 -0.00417
O6 6 0.621953 0.896141 0.319055 11.00000 0.01696 0.00828 =
0.01682 -0.00345 -0.00037 -0.00453
AFIX 3
H901 2 0.572153 0.960741 0.283155 11.00000 -1.50000
AFIX 0
O7 6 0.409023 0.098689 0.150078 11.00000 0.01110 0.00705 =
0.01126 -0.00438 0.00246 -0.00589
O8 6 0.553760 0.271908 0.159174 11.00000 0.01403 0.00985 =
0.00572 -0.00300 -0.00164 -0.00629
O9 6 0.342690 0.367507 -0.028381 11.00000 0.01032 0.00765 =
0.01125 -0.00210 -0.00309 -0.00354
O10 6 0.550372 0.263718 0.501193 11.00000 0.01536 0.00825 =
0.00517 -0.00164 -0.00027 -0.00457
O11 6 0.821638 0.363756 0.131502 11.00000 0.01098 0.00970 =
0.01264 -0.00388 -0.00120 -0.00332
O12 6 0.361015 0.833940 0.264019 11.00000 0.00829 0.01169 =
0.00988 -0.00211 -0.00318 -0.00212
N1 5 0.199130 0.620999 0.246405 11.00000 0.01209 0.01632 =
0.00701 -0.00510 0.00071 -0.00581
AFIX 3
H1A 2 0.266230 0.589099 0.309705 11.00000 -1.20000
H1B 2 0.259730 0.652399 0.174305 11.00000 -1.20000
AFIX 0
N2 5 -0.106669 0.682760 0.144800 11.00000 0.01020 0.03012 =
0.01211 -0.00660 -0.00057 -0.00505
AFIX 3
H2A 2 -0.179069 0.658160 0.211100 11.00000 -1.20000
H2B 2 -0.163269 0.716860 0.075500 11.00000 -1.20000
AFIX 0
C1 1 0.057967 0.738099 0.255446 11.00000 0.01444 0.01776 =
0.01928 -0.00986 0.00188 -0.00595
AFIX 23
H1C 2 0.098298 0.813183 0.258542 11.00000 -1.20000
H1D 2 -0.010582 0.703397 0.330962 11.00000 -1.20000
AFIX 0
C2 1 -0.042321 0.795753 0.146300 11.00000 0.01396 0.01844 =
0.01855 -0.00240 -0.00011 -0.00805
AFIX 23
H2C 2 -0.135121 0.876192 0.149659 11.00000 -1.20000
H2D 2 0.026597 0.829901 0.070867 11.00000 -1.20000
AFIX 0
C3 1 0.027519 0.555369 0.147850 11.00000 0.01477 0.03047 =
0.02441 -0.02085 0.00278 -0.00932
AFIX 23
H3C 2 0.094196 0.577684 0.069721 11.00000 -1.20000
H3D 2 -0.021155 0.479416 0.156737 11.00000 -1.20000
AFIX 0
C4 1 0.137197 0.504231 0.251314 11.00000 0.01814 0.01634 =
0.02092 -0.00492 -0.00065 -0.00605
AFIX 23
H4A 2 0.074878 0.468702 0.330010 11.00000 -1.20000
H4B 2 0.231215 0.425652 0.245713 11.00000 -1.20000
AFIX 0
N3 5 0.172408 -0.002554 0.471489 11.00000 0.02293 0.02050 =
0.03242 -0.01434 0.00602 -0.00582
AFIX 3
H3A 2 0.253108 0.044746 0.447589 11.00000 -1.20000
H3B 2 0.221808 -0.095154 0.482489 11.00000 -1.20000
AFIX 0
C5 1 0.052370 0.060908 0.373750 11.00000 0.02398 0.02274 =
0.02117 -0.01261 0.00341 -0.00167
AFIX 23
H5A 2 0.109228 0.047671 0.298989 11.00000 -1.20000
H5B 2 0.010385 0.163431 0.354317 11.00000 -1.20000
AFIX 0
C6 1 0.089933 0.004800 0.587891 11.00000 0.02807 0.03123 =
0.02647 -0.01659 -0.00153 -0.00911
AFIX 23
H6A 2 0.049697 0.104628 0.578828 11.00000 -1.20000
H6B 2 0.170411 -0.044554 0.652208 11.00000 -1.20000
AFIX 0
OW1 6 0.376360 0.169174 0.386009 11.00000 0.02836 0.02845 =
0.01241 -0.01028 0.00068 -0.01368
AFIX 3
H902 2 0.420960 0.188974 0.323009 11.00000 -1.50000
H903 2 0.417960 0.188974 0.430009 11.00000 -1.50000
HKLF 4

REM 2009ek00166triP-1 in P-1
REM R1 = 0.0291 for 3000 Fo > 4sig(Fo) and 0.0371 for all 3397 data
REM 271 parameters refined using 0 restraints

END

WGHT 0.0000 3.7670
REM Highest difference peak 0.562, deepest hole -0.493, 1-sigma level 0.114
Q1 1 0.0737 0.1072 0.4414 11.00000 0.05 0.56
Q2 1 0.6476 0.2049 0.5199 11.00000 0.05 0.49
Q3 1 0.6168 0.6935 0.3260 11.00000 0.05 0.46
Q4 1 0.4293 0.8065 0.3034 11.00000 0.05 0.45
Q5 1 0.5246 0.3608 0.4625 11.00000 0.05 0.44
Q6 1 0.7239 0.3554 0.1136 11.00000 0.05 0.42
Q7 1 0.1045 0.2471 0.2682 11.00000 0.05 0.41
Q8 1 0.5221 0.9969 0.2180 11.00000 0.05 0.41
Q9 1 0.1290 0.6804 0.2597 11.00000 0.05 0.40
Q10 1 0.6490 0.4752 0.2413 11.00000 0.05 0.40
Q11 1 0.7888 -0.1447 -0.0750 11.00000 0.05 0.40
Q12 1 0.5646 0.4477 0.2058 11.00000 0.05 0.40
Q13 1 0.5428 0.2629 0.1054 11.00000 0.05 0.39
Q14 1 0.6841 0.7083 0.2449 11.00000 0.05 0.39
Q15 1 0.4064 -0.0932 0.4251 11.00000 0.05 0.39
Q16 1 0.3977 0.0811 0.1955 11.00000 0.05 0.39
Q17 1 0.5296 0.2503 0.4539 11.00000 0.05 0.39
Q18 1 0.7444 0.6228 0.3335 11.00000 0.05 0.37
Q19 1 0.1737 -0.1250 0.7825 11.00000 0.05 0.37
Q20 1 0.4170 0.0205 0.4264 11.00000 0.05 0.37
Q21 1 0.1263 -0.0558 0.7634 11.00000 0.05 0.37
Q22 1 0.2748 0.3325 0.4355 11.00000 0.05 0.37
Q23 1 0.4994 0.3407 0.1553 11.00000 0.05 0.37
Q24 1 0.2572 0.3618 -0.0209 11.00000 0.05 0.37
Q25 1 0.9107 0.0019 -0.1020 11.00000 0.05 0.36
;

# Attachment '- compound22009ek00173rev1.cif'

data_2009ek00173mono
_database_code_depnum_ccdc_archive 'CCDC 812052'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H26 As2 F7 N3 O15 V4'
_chemical_formula_weight         866.90

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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 0.0000 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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                   16.8763(6)
_cell_length_b                   14.1659(5)
_cell_length_c                   10.7198(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.894(2)
_cell_angle_gamma                90.00
_cell_volume                     2556.84(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    46571
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       Slab
_exptl_crystal_colour            'Dark green'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1696
_exptl_absorpt_coefficient_mu    4.104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6387
_exptl_absorpt_correction_T_max  0.7349
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25614
_diffrn_reflns_av_R_equivalents  0.1003
_diffrn_reflns_av_sigmaI/netI    0.0632
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         25.03
_reflns_number_total             4513
_reflns_number_gt                3388
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
Images generated using CrystalMaker: a crystal and molecular
structures program for Mac and Windows. CrystalMaker Software Ltd,
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'

_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^ > 2\s(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^)+(0.0697P)^2^+42.2332P] 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    none
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4513
_refine_ls_number_parameters     322
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0676
_refine_ls_wR_factor_ref         0.1845
_refine_ls_wR_factor_gt          0.1606
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.001

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
N3 N 0.0616(5) 0.4490(7) 0.5692(8) 0.034(2) Uani 1 1 d . . .
H3A H 0.0965 0.4438 0.6386 0.041 Uiso 1 1 calc R . .
H3B H 0.0686 0.3974 0.5191 0.041 Uiso 1 1 calc R . .
N1 N 0.3068(5) 0.3868(6) 0.4535(7) 0.0285(19) Uani 1 1 d . . .
H1A H 0.2643 0.3851 0.3952 0.034 Uiso 1 1 calc R . .
H1B H 0.3508 0.3657 0.4155 0.034 Uiso 1 1 calc R . .
N2 N 0.3737(6) 0.4254(8) 0.6999(9) 0.048(3) Uani 1 1 d . . .
H2A H 0.3302 0.4471 0.7388 0.058 Uiso 1 1 calc R . .
H2B H 0.4168 0.4267 0.7572 0.058 Uiso 1 1 calc R . .
C1 C -0.0207(7) 0.4490(8) 0.6088(10) 0.036(3) Uani 1 1 d . . .
H1C H -0.0265 0.4996 0.6713 0.043 Uiso 1 1 calc R . .
H1D H -0.0317 0.3879 0.6489 0.043 Uiso 1 1 calc R . .
C3 C 0.2911(6) 0.3227(8) 0.5585(9) 0.034(2) Uani 1 1 d . . .
H3C H 0.2840 0.2574 0.5268 0.041 Uiso 1 1 calc R . .
H3D H 0.2416 0.3421 0.5957 0.041 Uiso 1 1 calc R . .
C6 C 0.0794(7) 0.5356(8) 0.5003(11) 0.037(3) Uani 1 1 d . . .
H6A H 0.1335 0.5308 0.4702 0.044 Uiso 1 1 calc R . .
H6B H 0.0785 0.5904 0.5574 0.044 Uiso 1 1 calc R . .
C2 C 0.3588(7) 0.3256(9) 0.6562(10) 0.040(3) Uani 1 1 d . . .
H2C H 0.4072 0.3002 0.6212 0.048 Uiso 1 1 calc R . .
H2D H 0.3463 0.2856 0.7280 0.048 Uiso 1 1 calc R . .
C5 C 0.3205(7) 0.4861(8) 0.4960(12) 0.039(3) Uani 1 1 d . . .
H5A H 0.2721 0.5112 0.5313 0.047 Uiso 1 1 calc R . .
H5B H 0.3328 0.5262 0.4241 0.047 Uiso 1 1 calc R . .
C4 C 0.3887(7) 0.4882(9) 0.5937(11) 0.044(3) Uani 1 1 d . . .
H4A H 0.4379 0.4679 0.5559 0.052 Uiso 1 1 calc R . .
H4B H 0.3968 0.5536 0.6245 0.052 Uiso 1 1 calc R . .
F6 F 0.5775(5) 0.1520(7) 0.6714(9) 0.077(3) Uani 1 1 d . . .
F7 F 0.5240(5) 0.2099(6) 0.4437(11) 0.084(3) Uani 1 1 d . . .
As1 As 0.88269(5) -0.21743(7) 0.19173(8) 0.0195(3) Uani 1 1 d . . .
As2 As 0.65415(6) -0.04515(7) 0.43597(9) 0.0229(3) Uani 1 1 d . . .
V3 V 0.95939(9) -0.16201(11) 0.47270(14) 0.0207(4) Uani 1 1 d . . .
V1 V 0.81289(9) -0.07361(12) 0.62311(14) 0.0219(4) Uani 1 1 d . . .
V4 V 0.82704(10) -0.02011(12) 0.32838(15) 0.0228(4) Uani 1 1 d . . .
V2 V 0.53068(12) 0.10776(14) 0.5376(2) 0.0415(5) Uani 1 1 d . . .
F1 F 0.9440(3) -0.0439(4) 0.3736(5) 0.0285(13) Uani 1 1 d . . .
O4 O 0.7130(4) -0.0483(5) 0.3147(6) 0.0256(15) Uani 1 1 d . . .
O3 O 0.8063(4) -0.0142(5) 0.7510(6) 0.0292(16) Uani 1 1 d . . .
F3 F 0.8343(3) -0.1447(4) 0.4462(5) 0.0209(11) Uani 1 1 d . . .
F5 F 0.5301(3) -0.0273(4) 0.6035(5) 0.0300(13) Uani 1 1 d . . .
F2 F 0.8172(4) 0.0314(5) 0.4990(6) 0.0390(15) Uani 1 1 d . . .
O5 O 0.9327(4) -0.2203(4) 0.0592(5) 0.0196(13) Uani 1 1 d . . .
F4 F 0.9310(4) -0.0899(4) 0.6241(6) 0.0383(15) Uani 1 1 d . . .
O6 O 1.0551(4) -0.1584(5) 0.4932(6) 0.0293(16) Uani 1 1 d . . .
O7 O 0.9494(4) -0.2338(5) 0.3145(6) 0.0240(14) Uani 1 1 d . . .
O8 O 0.8395(4) -0.1090(4) 0.1869(6) 0.0212(14) Uani 1 1 d . . .
O9 O 0.7002(4) -0.0891(5) 0.5677(6) 0.0278(15) Uani 1 1 d . . .
O11 O 0.8086(4) -0.2034(5) 0.6883(6) 0.0228(14) Uani 1 1 d . . .
O10 O 0.8325(4) 0.0772(5) 0.2533(6) 0.0290(16) Uani 1 1 d . . .
O2 O 0.6272(4) 0.0686(5) 0.4569(6) 0.0285(16) Uani 1 1 d . . .
O12 O 0.4238(4) 0.1163(5) 0.6034(6) 0.0284(15) Uani 1 1 d . . .
O1W O 0.4467(5) 0.3608(6) 0.3584(8) 0.0488(12) Uani 1 1 d . . .
O2W O 0.8909(5) 0.2840(6) 0.2710(8) 0.0488(12) Uani 1 1 d . . .
O3W O 0.2527(10) 0.6949(13) 0.8795(16) 0.0488(12) Uani 0.50 1 d P . .
O4W O 0.4411(10) 0.6377(13) 1.3190(16) 0.0488(12) Uani 0.50 1 d P . .
O5W O 0.3055(10) 0.7902(13) 1.0974(16) 0.0488(12) Uani 0.50 1 d P . .
O6W O 0.2960(10) 0.7902(13) 0.6690(16) 0.0488(12) Uani 0.50 1 d P . .

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
N3 0.033(5) 0.045(5) 0.024(4) -0.001(4) -0.003(4) 0.012(4)
N1 0.026(4) 0.039(5) 0.019(4) 0.000(4) -0.003(3) -0.003(4)
N2 0.029(5) 0.090(8) 0.025(5) -0.019(5) 0.005(4) -0.021(5)
C1 0.047(7) 0.031(6) 0.030(6) -0.002(5) 0.013(5) 0.000(5)
C3 0.032(6) 0.048(7) 0.021(5) 0.004(5) 0.000(4) -0.007(5)
C6 0.037(6) 0.032(6) 0.042(7) -0.010(5) 0.000(5) 0.002(5)
C2 0.034(6) 0.062(8) 0.021(5) 0.010(5) -0.011(5) -0.010(6)
C5 0.031(6) 0.037(6) 0.050(7) 0.001(5) 0.002(5) -0.009(5)
C4 0.042(7) 0.052(7) 0.037(6) -0.008(6) 0.001(5) -0.014(6)
F6 0.054(5) 0.097(7) 0.082(6) -0.045(5) 0.013(5) -0.031(5)
F7 0.063(5) 0.057(5) 0.138(9) 0.041(6) 0.047(6) 0.023(4)
As1 0.0207(5) 0.0242(5) 0.0133(4) 0.0002(4) -0.0011(4) -0.0012(4)
As2 0.0199(5) 0.0311(6) 0.0173(5) 0.0015(4) -0.0010(4) 0.0031(4)
V3 0.0199(8) 0.0263(9) 0.0153(8) -0.0011(6) -0.0026(6) -0.0008(6)
V1 0.0229(9) 0.0276(9) 0.0150(8) -0.0007(7) -0.0008(6) 0.0029(7)
V4 0.0255(9) 0.0252(9) 0.0175(8) 0.0001(7) 0.0003(7) -0.0010(7)
V2 0.0324(11) 0.0337(11) 0.0604(14) -0.0112(10) 0.0179(10) -0.0050(8)
F1 0.032(3) 0.034(3) 0.019(3) 0.001(2) 0.000(2) -0.007(2)
O4 0.020(3) 0.040(4) 0.017(3) -0.003(3) 0.003(3) 0.003(3)
O3 0.032(4) 0.035(4) 0.020(3) 0.000(3) 0.000(3) 0.005(3)
F3 0.020(3) 0.028(3) 0.014(2) -0.002(2) -0.004(2) -0.002(2)
F5 0.025(3) 0.041(3) 0.022(3) 0.004(3) -0.003(2) 0.002(3)
F2 0.043(4) 0.044(4) 0.030(3) 0.001(3) 0.001(3) 0.004(3)
O5 0.019(3) 0.030(3) 0.010(3) 0.001(3) 0.000(2) -0.003(3)
F4 0.041(4) 0.041(4) 0.032(3) 0.002(3) -0.003(3) 0.001(3)
O6 0.024(4) 0.037(4) 0.027(4) -0.002(3) -0.003(3) -0.003(3)
O7 0.024(3) 0.029(4) 0.018(3) 0.000(3) -0.001(3) 0.008(3)
O8 0.021(3) 0.022(3) 0.020(3) 0.004(3) -0.003(3) 0.002(3)
O9 0.022(3) 0.042(4) 0.019(3) 0.009(3) 0.000(3) 0.007(3)
O11 0.024(3) 0.025(3) 0.019(3) 0.003(3) 0.002(3) 0.007(3)
O10 0.034(4) 0.030(4) 0.022(3) 0.004(3) -0.001(3) 0.001(3)
O2 0.028(4) 0.028(4) 0.030(4) 0.003(3) 0.005(3) 0.002(3)
O12 0.021(3) 0.034(4) 0.029(4) -0.002(3) 0.000(3) 0.001(3)
O1W 0.046(3) 0.053(3) 0.046(3) 0.007(2) 0.000(2) 0.002(2)
O2W 0.046(3) 0.053(3) 0.046(3) 0.007(2) 0.000(2) 0.002(2)
O3W 0.046(3) 0.053(3) 0.046(3) 0.007(2) 0.000(2) 0.002(2)
O4W 0.046(3) 0.053(3) 0.046(3) 0.007(2) 0.000(2) 0.002(2)
O5W 0.046(3) 0.053(3) 0.046(3) 0.007(2) 0.000(2) 0.002(2)
O6W 0.046(3) 0.053(3) 0.046(3) 0.007(2) 0.000(2) 0.002(2)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
N3 C6 1.473(15) . ?
N3 C1 1.478(14) . ?
N1 C3 1.484(13) . ?
N1 C5 1.493(14) . ?
N2 C4 1.480(16) . ?
N2 C2 1.505(16) . ?
C1 C6 1.497(16) 3_566 ?
C3 C2 1.497(14) . ?
C6 C1 1.497(16) 3_566 ?
C5 C4 1.503(17) . ?
F6 V2 1.708(9) . ?
F7 V2 1.762(8) . ?
As1 O11 1.678(6) 4 ?
As1 O7 1.689(6) . ?
As1 O8 1.700(6) . ?
As1 O5 1.702(6) . ?
As2 O9 1.684(6) . ?
As2 O12 1.689(7) 3_656 ?
As2 O4 1.689(6) . ?
As2 O2 1.693(7) . ?
V3 O6 1.616(7) . ?
V3 O7 1.975(7) . ?
V3 O5 1.975(6) 4_556 ?
V3 F1 1.989(6) . ?
V3 F4 2.003(6) . ?
V3 F3 2.125(5) . ?
V1 O3 1.618(7) . ?
V1 O9 1.966(7) . ?
V1 O11 1.970(7) . ?
V1 F2 2.000(6) . ?
V1 F4 2.006(7) . ?
V1 F3 2.199(5) . ?
V4 O10 1.602(7) . ?
V4 O4 1.961(7) . ?
V4 F2 1.987(6) . ?
V4 O8 1.993(6) . ?
V4 F1 2.029(6) . ?
V4 F3 2.169(5) . ?
V2 O2 1.975(7) . ?
V2 O12 1.984(7) . ?
V2 F5 2.039(6) . ?
V2 F5 2.105(6) 3_656 ?
F5 V2 2.105(6) 3_656 ?
O5 V3 1.975(6) 4 ?
O11 As1 1.678(6) 4_556 ?
O12 As2 1.689(7) 3_656 ?
O5W O6W 1.39(2) 4_576 ?
O6W O5W 1.39(2) 4_575 ?

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
C6 N3 C1 111.8(8) . . ?
C3 N1 C5 112.2(8) . . ?
C4 N2 C2 111.0(8) . . ?
N3 C1 C6 111.1(9) . 3_566 ?
N1 C3 C2 110.3(9) . . ?
N3 C6 C1 111.5(9) . 3_566 ?
C3 C2 N2 110.3(10) . . ?
N1 C5 C4 109.0(10) . . ?
N2 C4 C5 111.1(9) . . ?
O11 As1 O7 112.4(3) 4 . ?
O11 As1 O8 106.6(3) 4 . ?
O7 As1 O8 114.2(3) . . ?
O11 As1 O5 112.2(3) 4 . ?
O7 As1 O5 107.8(3) . . ?
O8 As1 O5 103.4(3) . . ?
O9 As2 O12 107.2(3) . 3_656 ?
O9 As2 O4 111.9(3) . . ?
O12 As2 O4 106.3(3) 3_656 . ?
O9 As2 O2 110.7(3) . . ?
O12 As2 O2 112.9(3) 3_656 . ?
O4 As2 O2 107.7(3) . . ?
O6 V3 O7 99.1(3) . . ?
O6 V3 O5 102.7(3) . 4_556 ?
O7 V3 O5 87.7(3) . 4_556 ?
O6 V3 F1 98.0(3) . . ?
O7 V3 F1 88.5(3) . . ?
O5 V3 F1 159.3(2) 4_556 . ?
O6 V3 F4 99.6(3) . . ?
O7 V3 F4 161.3(3) . . ?
O5 V3 F4 88.6(3) 4_556 . ?
F1 V3 F4 88.5(2) . . ?
O6 V3 F3 171.6(3) . . ?
O7 V3 F3 85.3(2) . . ?
O5 V3 F3 84.5(2) 4_556 . ?
F1 V3 F3 74.9(2) . . ?
F4 V3 F3 76.1(2) . . ?
O3 V1 O9 101.2(3) . . ?
O3 V1 O11 100.3(3) . . ?
O9 V1 O11 86.9(3) . . ?
O3 V1 F2 100.6(3) . . ?
O9 V1 F2 87.7(3) . . ?
O11 V1 F2 159.1(3) . . ?
O3 V1 F4 100.4(3) . . ?
O9 V1 F4 158.3(3) . . ?
O11 V1 F4 87.2(3) . . ?
F2 V1 F4 90.4(3) . . ?
O3 V1 F3 173.3(3) . . ?
O9 V1 F3 84.3(2) . . ?
O11 V1 F3 83.7(2) . . ?
F2 V1 F3 75.6(2) . . ?
F4 V1 F3 74.4(2) . . ?
O10 V4 O4 103.1(3) . . ?
O10 V4 F2 99.1(3) . . ?
O4 V4 F2 90.0(3) . . ?
O10 V4 O8 98.6(3) . . ?
O4 V4 O8 88.2(3) . . ?
F2 V4 O8 162.2(3) . . ?
O10 V4 F1 100.1(3) . . ?
O4 V4 F1 156.6(3) . . ?
F2 V4 F1 88.9(2) . . ?
O8 V4 F1 85.7(2) . . ?
O10 V4 F3 171.8(3) . . ?
O4 V4 F3 83.9(2) . . ?
F2 V4 F3 76.6(2) . . ?
O8 V4 F3 85.7(2) . . ?
F1 V4 F3 73.1(2) . . ?
F6 V2 F7 100.7(5) . . ?
F6 V2 O2 97.1(4) . . ?
F7 V2 O2 90.2(3) . . ?
F6 V2 O12 93.4(3) . . ?
F7 V2 O12 97.4(3) . . ?
O2 V2 O12 165.8(3) . . ?
F6 V2 F5 93.8(4) . . ?
F7 V2 F5 165.1(4) . . ?
O2 V2 F5 84.9(3) . . ?
O12 V2 F5 84.8(3) . . ?
F6 V2 F5 167.7(4) . 3_656 ?
F7 V2 F5 91.5(4) . 3_656 ?
O2 V2 F5 84.8(3) . 3_656 ?
O12 V2 F5 83.0(3) . 3_656 ?
F5 V2 F5 74.2(2) . 3_656 ?
V3 F1 V4 110.9(3) . . ?
As2 O4 V4 124.2(4) . . ?
V3 F3 V4 100.9(2) . . ?
V3 F3 V1 99.1(2) . . ?
V4 F3 V1 97.1(2) . . ?
V2 F5 V2 105.8(2) . 3_656 ?
V4 F2 V1 110.4(3) . . ?
As1 O5 V3 123.6(3) . 4 ?
V3 F4 V1 110.3(3) . . ?
As1 O7 V3 127.7(4) . . ?
As1 O8 V4 127.9(3) . . ?
As2 O9 V1 126.4(4) . . ?
As1 O11 V1 125.9(4) 4_556 . ?
As2 O2 V2 124.2(4) . . ?
As2 O12 V2 125.9(4) 3_656 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.925
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.212

_vrf_PLAT306_I                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1W
RESPONSE: Solvent water molecules -- hydrogen positions not located.
;

# end Validation Reply Form

# Attachment '- compound32009ek00210rev1.cif'

data_2009ek00210
_database_code_depnum_ccdc_archive 'CCDC 817730'
#TrackingRef '- compound32009ek00210rev1.cif'

_audit_update_record             
;
2011-02-10 # Formatted by publCIF
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'As12 F27 O99.69 V36'
_chemical_formula_weight         4840.92

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
As As 0.0499 2.0058 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P6(3)/m

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

_cell_length_a                   32.3426(8)
_cell_length_b                   32.3426(8)
_cell_length_c                   10.6928(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     9686.6(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    141811
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4582
_exptl_absorpt_coefficient_mu    3.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8638
_exptl_absorpt_correction_T_max  0.9633
_exptl_absorpt_process_details   
;
SADABS V2.10 (Sheldrick, G.M., 2003)
;

_exptl_special_details           ?

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Bruker Nonius FR591 Rotating Anode'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_device_type  'Bruker-Nonius CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans to fill the asymmetric unit'
_diffrn_detector_area_resol_mean 9.091
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6027
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1600
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         25.03
_reflns_number_total             6027
_reflns_number_gt                2644
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
;
Images generated using CrystalMaker: a crystal and molecular
structures program for Mac and Windows. CrystalMaker Software Ltd,
Oxford, England (www.crystalmaker.com)
;
_computing_publication_material  'WINGX (Farrugia, 1998)'

_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^ > 2\s(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^)+(0.1691P)^2^+0.0000P] 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    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6027
_refine_ls_number_parameters     298
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.1736
_refine_ls_R_factor_gt           0.1006
_refine_ls_wR_factor_ref         0.2950
_refine_ls_wR_factor_gt          0.2663
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_restrained_S_all      0.943
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001

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
V6A V 0.0857(3) 0.2577(3) 0.4213(7) 0.0947(11) Uani 0.50 1 d P . 1
V6B V 0.0018(3) 0.2278(3) 0.4231(7) 0.0947(11) Uani 0.50 1 d P . 1
V6C V 0.1143(3) 0.2874(3) 0.3566(7) 0.0947(11) Uani 0.50 1 d P . 1
V6D V -0.0202(3) 0.2387(3) 0.3586(7) 0.0947(11) Uani 0.50 1 d P . 1
As1 As -0.03838(7) 0.32215(8) 0.2500 0.0559(6) Uani 1 2 d S . .
As2 As -0.17995(6) 0.33284(6) 0.49980(14) 0.0615(5) Uani 1 1 d . . .
As3 As 0.16605(7) 0.39546(8) 0.2500 0.0516(6) Uani 1 2 d SD . .
V1 V -0.06938(8) 0.38856(9) 0.39722(18) 0.0494(7) Uani 1 1 d . . .
V2 V -0.14904(12) 0.40034(11) 0.2500 0.0475(9) Uani 1 2 d S . .
V3 V 0.32310(12) 0.56618(12) 0.2500 0.0516(9) Uani 1 2 d S . .
V4 V 0.22867(9) 0.49397(10) 0.39929(19) 0.0536(7) Uani 1 1 d . . .
V5 V 0.06126(11) 0.34623(12) 0.3856(3) 0.0806(10) Uani 1 1 d . . .
O1 O 0.0221(4) 0.3569(6) 0.2500 0.068(4) Uani 1 2 d SU . .
O2 O -0.0563(7) 0.2637(7) 0.2500 0.059(7) Uani 1 2 d SU . .
O3 O -0.0603(4) 0.3325(4) 0.3830(10) 0.078(3) Uani 1 1 d U . .
O4 O -0.0288(3) 0.4192(4) 0.5000(9) 0.077(3) Uani 1 1 d U . .
O5 O -0.1225(4) 0.3488(4) 0.5062(9) 0.082(3) Uani 1 1 d U . .
O6 O -0.1660(5) 0.4398(5) 0.2500 0.070(4) Uani 1 2 d SU . .
O7 O -0.1928(3) 0.3557(3) 0.3727(9) 0.067(3) Uani 1 1 d U . .
O8 O -0.1921(4) 0.3548(3) 0.6309(10) 0.072(3) Uani 1 1 d U . .
O9 O 0.2722(3) 0.4846(4) 0.5063(9) 0.074(3) Uani 1 1 d U . .
O10 O 0.3574(5) 0.6227(6) 0.2500 0.077(4) Uani 1 2 d SU . .
O11 O 0.1967(4) 0.5006(5) 0.5032(8) 0.086(4) Uani 1 1 d U . .
O12 O 0.1940(3) 0.4232(4) 0.3793(8) 0.065(3) Uani 1 1 d U . .
O13 O 0.1628(5) 0.3426(4) 0.2500 0.092(5) Uani 1 2 d SDU . .
O14 O 0.1092(4) 0.3866(6) 0.2500 0.066(4) Uani 1 2 d SU . .
O15 O 0.0690(4) 0.3815(4) 0.4896(9) 0.074(3) Uani 1 1 d U . .
O16 O 0.0060(5) 0.2871(5) 0.4444(16) 0.134(6) Uani 1 1 d U . .
O17 O 0.1006(5) 0.3208(5) 0.4586(11) 0.112(4) Uani 1 1 d U . .
F1 F 0.0528(4) 0.2935(5) 0.2500 0.082(4) Uani 1 2 d S . .
F2 F -0.0348(4) 0.4125(4) 0.2500 0.059(3) Uani 1 2 d S . .
F3 F -0.0999(3) 0.4264(3) 0.3726(7) 0.075(3) Uani 1 1 d . . .
F4 F -0.1211(3) 0.3495(4) 0.2500 0.058(3) Uani 1 2 d S . .
F5 F 0.1991(3) 0.4976(4) 0.2500 0.051(3) Uani 1 2 d S . .
F6 F 0.2719(3) 0.4892(4) 0.2500 0.049(3) Uani 1 2 d S . .
F7 F 0.2795(3) 0.5590(3) 0.3776(8) 0.079(3) Uani 1 1 d . . .
OX1 O -0.0129(13) 0.2495(13) 0.2500 0.034(16) Uiso 0.31(4) 2 d SP . .
OX2 O -0.0278(16) 0.2028(18) 0.2500 0.10(2) Uiso 0.40(5) 2 d SP . .
OX4 O 0.107(3) 0.260(3) 0.2500 0.20(5) Uiso 0.42(9) 2 d SP . .
OX5 O 0.1507(16) 0.2778(15) 0.438(4) 0.15(2) Uiso 0.40(4) 1 d P . .
OX6 O -0.035(2) 0.191(2) 0.532(5) 0.09(3) Uiso 0.20(4) 1 d P . .
OX7 O 0.1126(18) 0.2443(19) 0.557(5) 0.07(2) Uiso 0.19(3) 1 d P . .
OX9 O -0.067(2) 0.196(2) 0.429(6) 0.13(3) Uiso 0.26(4) 1 d P . .
OX10 O 0.0425(4) 0.2339(4) 0.4327(9) 0.064(3) Uiso 1 1 d . . .

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
V6A 0.109(3) 0.085(3) 0.094(3) 0.004(2) 0.010(2) 0.051(2)
V6B 0.109(3) 0.085(3) 0.094(3) 0.004(2) 0.010(2) 0.051(2)
V6C 0.109(3) 0.085(3) 0.094(3) 0.004(2) 0.010(2) 0.051(2)
V6D 0.109(3) 0.085(3) 0.094(3) 0.004(2) 0.010(2) 0.051(2)
As1 0.0316(12) 0.0568(15) 0.0701(14) 0.000 0.000 0.0152(11)
As2 0.0534(10) 0.0555(10) 0.0714(10) 0.0277(8) 0.0298(8) 0.0242(8)
As3 0.0339(11) 0.0675(15) 0.0497(11) 0.000 0.000 0.0227(11)
V1 0.0433(14) 0.0645(17) 0.0323(11) 0.0073(11) 0.0016(10) 0.0208(13)
V2 0.050(2) 0.0394(19) 0.0496(18) 0.000 0.000 0.0194(17)
V3 0.048(2) 0.052(2) 0.068(2) 0.000 0.000 0.0352(19)
V4 0.0506(15) 0.0781(19) 0.0346(11) 0.0073(12) -0.0012(11) 0.0341(14)
V5 0.066(2) 0.097(2) 0.0706(18) -0.0071(17) 0.0075(15) 0.0342(18)
O1 0.021(7) 0.103(11) 0.047(7) 0.000 0.000 0.007(7)
O2 0.052(14) 0.069(14) 0.073(17) 0.000 0.000 0.054(12)
O3 0.071(7) 0.080(8) 0.094(8) 0.029(6) 0.019(6) 0.046(6)
O4 0.044(6) 0.126(10) 0.054(5) 0.016(6) 0.000(5) 0.037(6)
O5 0.092(8) 0.094(8) 0.082(7) 0.052(6) 0.043(6) 0.062(7)
O6 0.069(10) 0.059(9) 0.088(9) 0.000 0.000 0.037(8)
O7 0.034(5) 0.069(7) 0.091(7) 0.040(6) 0.017(5) 0.021(5)
O8 0.057(6) 0.046(6) 0.091(7) 0.001(5) 0.045(6) 0.010(5)
O9 0.053(6) 0.080(7) 0.071(6) 0.022(5) -0.032(5) 0.020(6)
O10 0.059(9) 0.075(10) 0.101(10) 0.000 0.000 0.037(8)
O11 0.099(9) 0.122(10) 0.039(5) 0.009(6) 0.006(5) 0.057(8)
O12 0.052(6) 0.074(7) 0.047(5) 0.019(5) -0.015(4) 0.016(5)
O13 0.047(9) 0.088(12) 0.107(11) 0.000 0.000 0.008(8)
O14 0.020(6) 0.138(13) 0.034(6) 0.000 0.000 0.036(8)
O15 0.069(7) 0.092(8) 0.057(6) -0.021(5) 0.013(5) 0.037(6)
O16 0.109(11) 0.104(11) 0.169(13) -0.035(10) 0.028(10) 0.039(9)
O17 0.105(10) 0.144(12) 0.082(8) -0.019(8) -0.020(7) 0.058(9)
F1 0.059(8) 0.103(10) 0.061(7) 0.000 0.000 0.023(8)
F2 0.052(7) 0.058(7) 0.048(6) 0.000 0.000 0.014(6)
F3 0.074(6) 0.094(7) 0.050(5) -0.003(4) -0.001(4) 0.036(5)
F4 0.032(6) 0.041(6) 0.074(7) 0.000 0.000 -0.002(5)
F5 0.040(6) 0.087(8) 0.046(5) 0.000 0.000 0.047(6)
F6 0.044(6) 0.066(7) 0.060(6) 0.000 0.000 0.044(6)
F7 0.067(6) 0.093(7) 0.065(5) -0.006(5) 0.003(4) 0.033(5)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
V6A V6C 1.170(9) . ?
V6A OX10 1.218(11) . ?
V6A OX7 1.85(5) . ?
V6A OX5 1.87(5) . ?
V6A O17 1.892(17) . ?
V6A OX4 1.95(3) . ?
V6A V6B 2.384(11) . ?
V6A V6C 3.118(11) 10_556 ?
V6B V6D 1.163(9) . ?
V6B OX10 1.236(11) . ?
V6B OX6 1.67(6) . ?
V6B O16 1.865(17) . ?
V6B OX9 1.93(6) . ?
V6B OX2 2.05(2) . ?
V6B OX1 2.116(19) . ?
V6C OX4 1.40(5) . ?
V6C OX5 1.61(4) . ?
V6C O17 1.740(16) . ?
V6C O13 2.035(13) . ?
V6C OX10 2.243(13) . ?
V6C V6C 2.280(15) 10_556 ?
V6C F1 2.384(14) . ?
V6C V6A 3.118(11) 10_556 ?
V6D OX1 1.201(12) . ?
V6D OX2 1.57(3) . ?
V6D OX9 1.63(6) . ?
V6D O16 1.638(16) . ?
V6D O2 2.077(18) . ?
V6D OX10 2.253(13) . ?
V6D OX6 2.32(6) . ?
V6D V6D 2.322(15) 10_556 ?
V6D F1 2.425(13) . ?
As1 O2 1.68(2) . ?
As1 O3 1.696(11) 10_556 ?
As1 O3 1.696(11) . ?
As1 O1 1.700(12) . ?
As2 O5 1.663(11) . ?
As2 O7 1.695(9) . ?
As2 O9 1.702(10) 9_556 ?
As2 O8 1.703(9) . ?
As3 O12 1.650(9) . ?
As3 O12 1.650(9) 10_556 ?
As3 O13 1.661(9) . ?
As3 O14 1.712(11) . ?
V1 O4 1.616(10) . ?
V1 F2 1.861(6) . ?
V1 F3 1.934(9) . ?
V1 O5 1.937(10) . ?
V1 O3 1.981(11) . ?
V1 F4 2.181(7) . ?
V2 O6 1.621(14) . ?
V2 F3 1.903(9) . ?
V2 F3 1.903(9) 10_556 ?
V2 O7 1.940(9) 10_556 ?
V2 O7 1.940(9) . ?
V2 F4 2.238(12) . ?
V3 O10 1.594(16) . ?
V3 F7 1.891(9) 10_556 ?
V3 F7 1.891(9) . ?
V3 O8 1.924(9) 8_556 ?
V3 O8 1.924(9) 5_554 ?
V3 F6 2.194(11) . ?
V4 O11 1.604(11) . ?
V4 F5 1.894(5) . ?
V4 F7 1.929(9) . ?
V4 O9 1.951(9) . ?
V4 O12 1.993(10) . ?
V4 F6 2.178(6) . ?
V5 O15 1.522(10) . ?
V5 O16 1.956(15) . ?
V5 O17 1.988(15) . ?
V5 O14 2.047(10) . ?
V5 O1 2.066(11) . ?
V5 F1 2.149(11) . ?
V5 V5 2.901(6) 10_556 ?
O1 V5 2.066(11) 10_556 ?
O2 OX1 1.68(4) . ?
O2 V6D 2.077(18) 10_556 ?
O8 V3 1.924(9) 9_556 ?
O9 As2 1.702(10) 8_556 ?
O13 V6C 2.035(13) 10_556 ?
O14 V5 2.047(10) 10_556 ?
F1 V5 2.149(11) 10_556 ?
F1 V6C 2.384(14) 10_556 ?
F1 V6D 2.425(13) 10_556 ?
F2 V1 1.861(6) 10_556 ?
F4 V1 2.181(7) 10_556 ?
F5 V4 1.894(5) 10_556 ?
F6 V4 2.178(6) 10_556 ?
OX1 V6D 1.201(12) 10_556 ?
OX1 OX2 1.34(5) . ?
OX1 V6B 2.116(19) 10_556 ?
OX2 V6D 1.57(3) 10_556 ?
OX2 V6B 2.05(2) 10_556 ?
OX4 V6C 1.40(5) 10_556 ?
OX4 V6A 1.95(3) 10_556 ?
OX5 OX7 1.72(7) . ?
OX6 OX9 1.59(8) . ?

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
V6C V6A OX10 139.7(9) . . ?
V6C V6A OX7 112.6(18) . . ?
OX10 V6A OX7 107.4(17) . . ?
V6C V6A OX5 58.8(14) . . ?
OX10 V6A OX5 160.8(15) . . ?
OX7 V6A OX5 55(2) . . ?
V6C V6A O17 64.3(6) . . ?
OX10 V6A O17 104.6(8) . . ?
OX7 V6A O17 101.1(17) . . ?
OX5 V6A O17 88.2(14) . . ?
V6C V6A OX4 45(2) . . ?
OX10 V6A OX4 113(2) . . ?
OX7 V6A OX4 123(3) . . ?
OX5 V6A OX4 76(3) . . ?
O17 V6A OX4 106(2) . . ?
V6C V6A V6B 127.5(7) . . ?
OX10 V6A V6B 13.8(6) . . ?
OX7 V6A V6B 118.2(17) . . ?
OX5 V6A V6B 173.4(14) . . ?
O17 V6A V6B 93.4(5) . . ?
OX4 V6A V6B 110(2) . . ?
V6C V6A V6C 36.2(4) . 10_556 ?
OX10 V6A V6C 111.1(6) . 10_556 ?
OX7 V6A V6C 135.8(17) . 10_556 ?
OX5 V6A V6C 82.8(13) . 10_556 ?
O17 V6A V6C 89.5(5) . 10_556 ?
OX4 V6A V6C 18(2) . 10_556 ?
V6B V6A V6C 103.6(3) . 10_556 ?
V6D V6B OX10 139.8(9) . . ?
V6D V6B OX6 109(2) . . ?
OX10 V6B OX6 112(2) . . ?
V6D V6B O16 60.3(7) . . ?
OX10 V6B O16 107.5(8) . . ?
OX6 V6B O16 109(2) . . ?
V6D V6B OX9 57.5(18) . . ?
OX10 V6B OX9 160(2) . . ?
OX6 V6B OX9 52(3) . . ?
O16 V6B OX9 90.8(19) . . ?
V6D V6B OX2 49.5(14) . . ?
OX10 V6B OX2 112.7(14) . . ?
OX6 V6B OX2 109(2) . . ?
O16 V6B OX2 107.2(15) . . ?
OX9 V6B OX2 69(2) . . ?
V6D V6B OX1 27.0(10) . . ?
OX10 V6B OX1 114.7(11) . . ?
OX6 V6B OX1 131(2) . . ?
O16 V6B OX1 71.3(11) . . ?
OX9 V6B OX1 79(2) . . ?
V6D V6B V6A 128.0(7) . . ?
OX6 V6B V6A 123(2) . . ?
O16 V6B V6A 95.8(6) . . ?
OX9 V6B V6A 173.1(18) . . ?
OX2 V6B V6A 111.3(12) . . ?
OX1 V6B V6A 104.9(10) . . ?
V6A V6C OX4 98(3) . . ?
V6A V6C OX5 82.8(16) . . ?
OX4 V6C OX5 102(3) . . ?
V6A V6C O17 78.4(7) . . ?
OX4 V6C O17 154(3) . . ?
OX5 V6C O17 102.7(17) . . ?
V6A V6C O13 175.9(7) . . ?
OX4 V6C O13 85(3) . . ?
OX5 V6C O13 98.8(16) . . ?
O17 V6C O13 97.5(6) . . ?
OX4 V6C OX10 92(3) . . ?
OX5 V6C OX10 103.2(16) . . ?
O17 V6C OX10 76.4(6) . . ?
O13 V6C OX10 157.9(6) . . ?
V6A V6C V6C 126.2(5) . 10_556 ?
OX5 V6C V6C 122.5(16) . 10_556 ?
O17 V6C V6C 128.8(5) . 10_556 ?
O13 V6C V6C 55.9(3) . 10_556 ?
OX10 V6C V6C 111.3(3) . 10_556 ?
V6A V6C F1 90.1(6) . . ?
OX4 V6C F1 78(3) . . ?
OX5 V6C F1 172.9(16) . . ?
O17 V6C F1 76.5(6) . . ?
O13 V6C F1 88.2(5) . . ?
OX10 V6C F1 69.7(4) . . ?
V6C V6C F1 61.4(2) 10_556 . ?
V6A V6C V6A 108.6(7) . 10_556 ?
OX5 V6C V6A 125.8(16) . 10_556 ?
O17 V6C V6A 131.4(6) . 10_556 ?
O13 V6C V6A 73.5(3) . 10_556 ?
OX10 V6C V6A 94.3(4) . 10_556 ?
F1 V6C V6A 55.9(3) . 10_556 ?
V6B V6D OX1 127.0(19) . . ?
V6B V6D OX2 96.3(16) . . ?
OX1 V6D OX2 55.7(19) . . ?
V6B V6D OX9 85(2) . . ?
OX1 V6D OX9 131(3) . . ?
OX2 V6D OX9 89(3) . . ?
V6B V6D O16 81.6(9) . . ?
OX1 V6D O16 109.3(18) . . ?
OX2 V6D O16 159.1(18) . . ?
OX9 V6D O16 111(2) . . ?
V6B V6D O2 175.2(9) . . ?
OX1 V6D O2 54.0(17) . . ?
OX2 V6D O2 87.9(16) . . ?
OX9 V6D O2 97(2) . . ?
O16 V6D O2 93.7(9) . . ?
OX1 V6D OX10 108.0(18) . . ?
OX2 V6D OX10 91.3(16) . . ?
OX9 V6D OX10 106(2) . . ?
O16 V6D OX10 79.3(7) . . ?
O2 V6D OX10 157.6(7) . . ?
V6B V6D OX6 43.0(16) . . ?
OX1 V6D OX6 156(2) . . ?
OX2 V6D OX6 101.0(19) . . ?
OX9 V6D OX6 43(3) . . ?
O16 V6D OX6 91.6(16) . . ?
O2 V6D OX6 138.3(16) . . ?
OX10 V6D OX6 63.7(15) . . ?
V6B V6D V6D 126.4(5) . 10_556 ?
OX1 V6D V6D 14.9(17) . 10_556 ?
OX2 V6D V6D 42.4(13) . 10_556 ?
OX9 V6D V6D 117(2) . 10_556 ?
O16 V6D V6D 124.1(7) . 10_556 ?
O2 V6D V6D 56.0(4) . 10_556 ?
OX10 V6D V6D 110.6(3) . 10_556 ?
OX6 V6D V6D 143.3(14) . 10_556 ?
V6B V6D F1 89.3(7) . . ?
OX1 V6D F1 49.3(17) . . ?
OX2 V6D F1 85.5(16) . . ?
OX9 V6D F1 172(2) . . ?
O16 V6D F1 73.7(6) . . ?
O2 V6D F1 88.8(6) . . ?
OX10 V6D F1 68.8(4) . . ?
OX6 V6D F1 132.1(16) . . ?
V6D V6D F1 61.4(2) 10_556 . ?
O2 As1 O3 106.2(5) . 10_556 ?
O2 As1 O3 106.2(5) . . ?
O3 As1 O3 114.0(7) 10_556 . ?
O2 As1 O1 112.4(9) . . ?
O3 As1 O1 109.0(5) 10_556 . ?
O3 As1 O1 109.0(5) . . ?
O5 As2 O7 112.1(4) . . ?
O5 As2 O9 108.0(6) . 9_556 ?
O7 As2 O9 109.1(5) . 9_556 ?
O5 As2 O8 107.0(5) . . ?
O7 As2 O8 108.7(5) . . ?
O9 As2 O8 112.0(4) 9_556 . ?
O12 As3 O12 113.8(6) . 10_556 ?
O12 As3 O13 107.2(4) . . ?
O12 As3 O13 107.2(4) 10_556 . ?
O12 As3 O14 110.0(4) . . ?
O12 As3 O14 110.0(4) 10_556 . ?
O13 As3 O14 108.5(8) . . ?
O4 V1 F2 100.7(4) . . ?
O4 V1 F3 102.6(5) . . ?
F2 V1 F3 90.7(4) . . ?
O4 V1 O5 100.2(5) . . ?
F2 V1 O5 159.1(5) . . ?
F3 V1 O5 86.5(4) . . ?
O4 V1 O3 99.6(6) . . ?
F2 V1 O3 89.0(5) . . ?
F3 V1 O3 157.4(4) . . ?
O5 V1 O3 85.8(4) . . ?
O4 V1 F4 176.6(4) . . ?
F2 V1 F4 76.0(3) . . ?
F3 V1 F4 77.4(4) . . ?
O5 V1 F4 83.2(4) . . ?
O3 V1 F4 80.6(5) . . ?
O6 V2 F3 100.9(5) . . ?
O6 V2 F3 100.9(5) . 10_556 ?
F3 V2 F3 87.1(5) . 10_556 ?
O6 V2 O7 100.2(5) . 10_556 ?
F3 V2 O7 158.8(4) . 10_556 ?
F3 V2 O7 90.0(4) 10_556 10_556 ?
O6 V2 O7 100.2(5) . . ?
F3 V2 O7 90.0(4) . . ?
F3 V2 O7 158.8(4) 10_556 . ?
O7 V2 O7 85.1(6) 10_556 . ?
O6 V2 F4 176.5(6) . . ?
F3 V2 F4 76.6(3) . . ?
F3 V2 F4 76.6(3) 10_556 . ?
O7 V2 F4 82.3(4) 10_556 . ?
O7 V2 F4 82.3(4) . . ?
O10 V3 F7 100.9(5) . 10_556 ?
O10 V3 F7 100.9(5) . . ?
F7 V3 F7 92.3(6) 10_556 . ?
O10 V3 O8 101.2(5) . 8_556 ?
F7 V3 O8 157.4(5) 10_556 8_556 ?
F7 V3 O8 88.2(4) . 8_556 ?
O10 V3 O8 101.2(5) . 5_554 ?
F7 V3 O8 88.2(4) 10_556 5_554 ?
F7 V3 O8 157.4(5) . 5_554 ?
O8 V3 O8 82.9(7) 8_556 5_554 ?
O10 V3 F6 176.2(6) . . ?
F7 V3 F6 76.5(3) 10_556 . ?
F7 V3 F6 76.5(3) . . ?
O8 V3 F6 81.6(4) 8_556 . ?
O8 V3 F6 81.6(4) 5_554 . ?
O11 V4 F5 101.3(4) . . ?
O11 V4 F7 101.1(5) . . ?
F5 V4 F7 90.7(4) . . ?
O11 V4 O9 100.2(5) . . ?
F5 V4 O9 158.3(4) . . ?
F7 V4 O9 87.2(4) . . ?
O11 V4 O12 101.4(5) . . ?
F5 V4 O12 88.2(4) . . ?
F7 V4 O12 157.2(4) . . ?
O9 V4 O12 85.4(4) . . ?
O11 V4 F6 175.6(5) . . ?
F5 V4 F6 75.4(3) . . ?
F7 V4 F6 76.2(4) . . ?
O9 V4 F6 83.2(4) . . ?
O12 V4 F6 81.5(4) . . ?
O15 V5 O16 103.1(6) . . ?
O15 V5 O17 97.1(6) . . ?
O16 V5 O17 86.0(7) . . ?
O15 V5 O14 104.6(6) . . ?
O16 V5 O14 151.8(6) . . ?
O17 V5 O14 95.9(6) . . ?
O15 V5 O1 105.8(6) . . ?
O16 V5 O1 93.0(7) . . ?
O17 V5 O1 156.6(5) . . ?
O14 V5 O1 74.2(4) . . ?
O15 V5 F1 174.9(6) . . ?
O16 V5 F1 75.5(5) . . ?
O17 V5 F1 77.9(5) . . ?
O14 V5 F1 77.4(5) . . ?
O1 V5 F1 79.3(5) . . ?
O15 V5 V5 136.9(4) . 10_556 ?
O16 V5 V5 108.7(5) . 10_556 ?
O17 V5 V5 113.1(4) . 10_556 ?
O14 V5 V5 44.9(3) . 10_556 ?
O1 V5 V5 45.4(3) . 10_556 ?
F1 V5 V5 47.5(3) . 10_556 ?
As1 O1 V5 119.2(6) . . ?
As1 O1 V5 119.2(6) . 10_556 ?
V5 O1 V5 89.2(6) . 10_556 ?
As1 O2 OX1 116.2(18) . . ?
As1 O2 V6D 119.6(9) . . ?
As1 O2 V6D 119.6(9) . 10_556 ?
V6D O2 V6D 67.9(7) . 10_556 ?
As1 O3 V1 120.9(5) . . ?
As2 O5 V1 131.6(6) . . ?
As2 O7 V2 128.3(5) . . ?
As2 O8 V3 129.6(5) . 9_556 ?
As2 O9 V4 128.5(5) 8_556 . ?
As3 O12 V4 123.7(5) . . ?
As3 O13 V6C 121.8(6) . 10_556 ?
As3 O13 V6C 121.8(6) . . ?
V6C O13 V6C 68.1(6) 10_556 . ?
As3 O14 V5 121.0(6) . 10_556 ?
As3 O14 V5 121.0(6) . . ?
V5 O14 V5 90.3(6) 10_556 . ?
V6D O16 V5 122.5(9) . . ?
V6B O16 V5 121.9(8) . . ?
V6C O17 V5 115.1(7) . . ?
V6A O17 V5 119.6(7) . . ?
V5 F1 V5 84.9(5) 10_556 . ?
V5 F1 V6C 127.5(6) 10_556 . ?
V5 F1 V6C 87.9(3) . . ?
V5 F1 V6C 87.9(3) 10_556 10_556 ?
V5 F1 V6C 127.5(6) . 10_556 ?
V6C F1 V6C 57.1(5) . 10_556 ?
V5 F1 V6D 87.0(3) 10_556 10_556 ?
V5 F1 V6D 126.5(6) . 10_556 ?
V6C F1 V6D 135.7(7) . 10_556 ?
V6C F1 V6D 104.9(4) 10_556 10_556 ?
V5 F1 V6D 126.5(6) 10_556 . ?
V5 F1 V6D 87.0(3) . . ?
V6C F1 V6D 104.9(4) . . ?
V6C F1 V6D 135.7(7) 10_556 . ?
V6D F1 V6D 57.2(5) 10_556 . ?
V1 F2 V1 115.6(6) 10_556 . ?
V2 F3 V1 113.1(4) . . ?
V1 F4 V1 92.4(4) . 10_556 ?
V1 F4 V2 92.8(4) . . ?
V1 F4 V2 92.8(4) 10_556 . ?
V4 F5 V4 114.9(5) . 10_556 ?
V4 F6 V4 94.3(4) 10_556 . ?
V4 F6 V3 93.8(3) 10_556 . ?
V4 F6 V3 93.8(3) . . ?
V3 F7 V4 113.4(5) . . ?
V6D OX1 V6D 150(3) 10_556 . ?
V6D OX1 OX2 76.3(17) 10_556 . ?
V6D OX1 OX2 76.3(17) . . ?
V6D OX1 O2 90.6(18) 10_556 . ?
V6D OX1 O2 90.6(18) . . ?
OX2 OX1 O2 116(3) . . ?
V6D OX1 V6B 142(3) 10_556 . ?
OX2 OX1 V6B 68.8(12) . . ?
O2 OX1 V6B 116.5(9) . . ?
V6D OX1 V6B 142(3) . 10_556 ?
OX2 OX1 V6B 68.8(12) . 10_556 ?
O2 OX1 V6B 116.5(9) . 10_556 ?
V6B OX1 V6B 122.1(17) . 10_556 ?
OX1 OX2 V6D 48.0(14) . 10_556 ?
OX1 OX2 V6D 48.0(14) . . ?
V6D OX2 V6D 95(3) 10_556 . ?
OX1 OX2 V6B 73.8(15) . . ?
V6D OX2 V6B 120(3) 10_556 . ?
OX1 OX2 V6B 73.8(15) . 10_556 ?
V6D OX2 V6B 120(3) . 10_556 ?
V6B OX2 V6B 129(2) . 10_556 ?
V6C OX4 V6C 109(6) . 10_556 ?
V6C OX4 V6A 137(5) . 10_556 ?
V6C OX4 V6A 137(5) 10_556 . ?
V6A OX4 V6A 140(4) 10_556 . ?
V6C OX5 OX7 99(3) . . ?
OX7 OX5 V6A 62(2) . . ?
OX9 OX6 V6B 72(3) . . ?
OX9 OX6 V6D 45(3) . . ?
OX5 OX7 V6A 63(2) . . ?
OX6 OX9 V6D 92(4) . . ?
V6A OX10 V6B 152.6(11) . . ?
V6B OX10 V6C 134.7(8) . . ?
V6A OX10 V6D 135.2(8) . . ?
V6C OX10 V6D 116.0(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.505
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.183