# Electronic Supplementary Material (ESI) for CrystEngComm
# 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_k

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C80 H66 As8 Cu4 N16 O43 V14'
_chemical_formula_weight         3506.17

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   28.369(4)
_cell_length_b                   28.369(4)
_cell_length_c                   14.436(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11618(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6816
_exptl_absorpt_coefficient_mu    4.130
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_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            54802
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_sigmaI/netI    0.0589
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.00
_diffrn_reflns_theta_max         27.48
_reflns_number_total             6639
_reflns_number_gt                2914
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1184P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6639
_refine_ls_number_parameters     373
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.1513
_refine_ls_R_factor_gt           0.0654
_refine_ls_wR_factor_ref         0.2244
_refine_ls_wR_factor_gt          0.1817
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.53864(3) 0.13636(4) 0.08895(6) 0.0969(4) Uani 1 1 d . . .
As2 As 0.42636(3) 0.15531(4) 0.08800(6) 0.0949(4) Uani 1 1 d . . .
V1 V 0.63865(5) 0.22755(5) -0.13393(10) 0.0842(4) Uani 1 1 d . . .
V2 V 0.59929(5) 0.23303(6) 0.04747(10) 0.0871(5) Uani 1 1 d . . .
V3 V 0.61201(5) 0.33026(5) -0.12494(9) 0.0815(4) Uani 1 1 d . . .
V4 V 0.5000 0.2500 0.13447(12) 0.0908(7) Uani 1 2 d S . .
Cu1 Cu 0.83806(5) 0.41097(5) 0.05944(13) 0.1380(6) Uani 1 1 d . . .
O1 O 0.60761(18) 0.18673(18) -0.0479(4) 0.0814(14) Uani 1 1 d . . .
O2 O 0.62270(19) 0.2763(2) -0.0460(4) 0.0852(15) Uani 1 1 d . . .
O3 O 0.53068(18) 0.1273(2) -0.0303(4) 0.0857(15) Uani 1 1 d . . .
O4 O 0.6943(2) 0.2200(2) -0.1320(4) 0.1066(19) Uani 1 1 d U . .
O5 O 0.6379(2) 0.2245(2) 0.1250(5) 0.1076(19) Uani 1 1 d U . .
O6 O 0.4796(2) 0.1291(2) 0.1276(4) 0.0961(17) Uani 1 1 d U . .
O7 O 0.5000 0.2500 0.2420(6) 0.110(3) Uani 1 2 d SU . .
O8 O 0.4441(2) 0.2151(2) 0.0891(4) 0.0922(16) Uani 1 1 d U . .
O9 O 0.6572(2) 0.3628(2) -0.1262(4) 0.0999(17) Uani 1 1 d U . .
O10 O 0.54140(19) 0.1987(2) 0.0882(4) 0.0891(15) Uani 1 1 d U . .
O11 O 0.43222(18) 0.1437(2) -0.0305(4) 0.0846(15) Uani 1 1 d . . .
N3 N 0.7952(3) 0.3591(3) 0.0981(6) 0.104(2) Uani 1 1 d U . .
N2 N 0.9055(3) 0.4034(4) 0.0978(7) 0.117(3) Uani 1 1 d U . .
N4 N 0.8082(3) 0.3993(3) -0.0626(7) 0.114(3) Uani 1 1 d U . .
N1 N 0.8471(4) 0.4697(4) 0.1331(8) 0.146(3) Uani 1 1 d U . .
OW1 O 0.5000 0.2500 -0.1250 0.233(11) Uani 1 4 d S . .
C1 C 0.8134(7) 0.5047(7) 0.1366(13) 0.207(7) Uani 1 1 d U . .
H1A H 0.7837 0.5011 0.1105 0.248 Uiso 1 1 calc R . .
C2 C 0.8285(9) 0.5510(8) 0.1876(16) 0.237(9) Uani 1 1 d U . .
H2A H 0.8105 0.5784 0.1906 0.285 Uiso 1 1 calc R . .
C3 C 0.8702(7) 0.5458(7) 0.2252(14) 0.205(7) Uani 1 1 d U . .
H3A H 0.8788 0.5709 0.2631 0.246 Uiso 1 1 calc R . .
C4 C 0.9040(7) 0.5108(7) 0.2205(12) 0.192(6) Uani 1 1 d U . .
H4A H 0.9332 0.5138 0.2491 0.230 Uiso 1 1 calc R . .
C5 C 0.8920(5) 0.4718(4) 0.1713(8) 0.121(4) Uani 1 1 d . . .
C6 C 0.9233(5) 0.4341(4) 0.1560(7) 0.121(4) Uani 1 1 d . . .
C7 C 0.9682(5) 0.4322(5) 0.1950(8) 0.123(4) Uani 1 1 d . . .
H7A H 0.9791 0.4549 0.2361 0.148 Uiso 1 1 calc R . .
C8 C 0.9948(6) 0.3947(6) 0.1689(10) 0.148(5) Uani 1 1 d . . .
H8A H 1.0251 0.3923 0.1928 0.177 Uiso 1 1 calc R . .
C9 C 0.9800(6) 0.3616(7) 0.1116(11) 0.166(6) Uani 1 1 d . . .
H9A H 0.9986 0.3360 0.0941 0.200 Uiso 1 1 calc R . .
C10 C 0.9350(5) 0.3681(5) 0.0801(9) 0.144(5) Uani 1 1 d . . .
H10A H 0.9235 0.3447 0.0411 0.173 Uiso 1 1 calc R . .
C11 C 0.7871(6) 0.3429(4) 0.1774(10) 0.144(5) Uani 1 1 d . . .
H11A H 0.8062 0.3541 0.2248 0.173 Uiso 1 1 calc R . .
C12 C 0.7535(6) 0.3107(6) 0.2032(12) 0.163(6) Uani 1 1 d . . .
H12A H 0.7510 0.3003 0.2641 0.196 Uiso 1 1 calc R . .
C13 C 0.7251(5) 0.2950(5) 0.1379(16) 0.162(7) Uani 1 1 d . . .
H13A H 0.7012 0.2739 0.1526 0.194 Uiso 1 1 calc R . .
C14 C 0.7309(3) 0.3101(4) 0.0473(13) 0.136(5) Uani 1 1 d . . .
H14A H 0.7113 0.2991 0.0004 0.163 Uiso 1 1 calc R . .
C15 C 0.7676(3) 0.3429(3) 0.0278(8) 0.097(3) Uani 1 1 d . . .
C16 C 0.7788(3) 0.3625(4) -0.0630(9) 0.106(3) Uani 1 1 d . . .
C17 C 0.7609(5) 0.3447(6) -0.1454(13) 0.160(6) Uani 1 1 d . . .
H17A H 0.7401 0.3193 -0.1454 0.192 Uiso 1 1 calc R . .
C18 C 0.7750(6) 0.3663(11) -0.2293(15) 0.214(12) Uani 1 1 d U . .
H18A H 0.7627 0.3557 -0.2852 0.257 Uiso 1 1 calc R . .
C19 C 0.8028(6) 0.3981(11) -0.2285(16) 0.215(12) Uani 1 1 d U . .
H19A H 0.8146 0.4094 -0.2844 0.258 Uiso 1 1 calc R . .
C20 C 0.8183(4) 0.4191(5) -0.1443(13) 0.148(5) Uani 1 1 d . . .
H20A H 0.8357 0.4469 -0.1461 0.178 Uiso 1 1 calc 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 0.0877(6) 0.1265(8) 0.0765(6) 0.0382(5) -0.0189(5) -0.0249(5)
As2 0.0839(6) 0.1268(8) 0.0740(6) 0.0168(5) -0.0028(4) -0.0330(5)
V1 0.0778(9) 0.0878(9) 0.0868(10) 0.0139(7) 0.0107(7) 0.0037(7)
V2 0.0770(9) 0.1154(12) 0.0689(9) 0.0142(8) -0.0077(7) -0.0219(8)
V3 0.0777(9) 0.0846(9) 0.0822(9) 0.0058(7) 0.0173(7) -0.0049(7)
V4 0.0814(13) 0.1392(19) 0.0517(10) 0.000 0.000 -0.0324(12)
Cu1 0.1066(10) 0.1288(11) 0.1784(15) -0.0358(10) -0.0223(9) -0.0446(8)
O1 0.078(3) 0.092(4) 0.074(3) 0.018(3) -0.008(3) -0.008(3)
O2 0.078(3) 0.103(4) 0.075(3) 0.008(3) 0.008(3) -0.011(3)
O3 0.083(3) 0.105(4) 0.069(3) 0.019(3) -0.009(3) -0.010(3)
O4 0.106(2) 0.107(2) 0.107(2) 0.0015(10) 0.0007(10) 0.0003(10)
O5 0.107(2) 0.109(2) 0.107(2) 0.0014(10) -0.0022(10) -0.0017(10)
O6 0.0958(19) 0.0979(19) 0.0945(19) 0.0038(10) -0.0013(10) -0.0026(10)
O7 0.110(3) 0.111(3) 0.109(3) 0.000 0.000 -0.0009(10)
O8 0.0916(18) 0.0937(18) 0.0913(18) 0.0001(10) -0.0007(10) -0.0024(10)
O9 0.0991(19) 0.0998(19) 0.1009(19) 0.0009(10) 0.0022(10) -0.0007(10)
O10 0.0887(17) 0.0906(17) 0.0881(17) 0.0012(10) 0.0000(10) -0.0037(10)
O11 0.082(3) 0.104(4) 0.068(3) 0.009(3) -0.010(3) -0.016(3)
N3 0.104(2) 0.103(3) 0.104(2) -0.0012(10) 0.0004(10) -0.0009(10)
N2 0.117(3) 0.118(3) 0.117(3) -0.0004(10) 0.0000(10) -0.0008(10)
N4 0.113(3) 0.115(3) 0.115(3) 0.0000(10) -0.0007(10) 0.0003(10)
N1 0.145(4) 0.145(4) 0.146(4) -0.0007(10) 0.0003(10) -0.0007(10)
OW1 0.262(18) 0.262(18) 0.18(2) 0.000 0.000 0.000
C1 0.206(7) 0.206(7) 0.207(7) -0.0004(10) 0.0001(10) -0.0005(10)
C2 0.237(9) 0.237(9) 0.237(9) -0.0005(10) 0.0002(10) 0.0002(10)
C3 0.205(7) 0.205(7) 0.205(7) -0.0004(10) -0.0001(10) -0.0001(10)
C4 0.192(6) 0.192(6) 0.192(6) -0.0004(10) 0.0001(10) -0.0003(10)
C5 0.144(10) 0.111(8) 0.109(8) -0.034(6) -0.003(7) -0.076(8)
C6 0.171(12) 0.117(9) 0.075(6) -0.026(6) 0.023(7) -0.056(8)
C7 0.111(8) 0.171(12) 0.089(7) 0.029(8) -0.025(6) -0.070(8)
C8 0.168(14) 0.180(15) 0.095(9) 0.035(10) -0.003(9) -0.018(12)
C9 0.167(15) 0.208(17) 0.123(12) 0.041(11) -0.017(10) -0.025(13)
C10 0.127(10) 0.188(13) 0.118(9) 0.019(9) -0.043(8) -0.046(10)
C11 0.178(13) 0.102(8) 0.153(12) -0.036(8) 0.010(9) -0.025(8)
C12 0.155(14) 0.165(14) 0.169(14) -0.048(11) 0.058(11) -0.020(11)
C13 0.119(11) 0.102(9) 0.27(2) 0.016(12) 0.077(13) -0.015(8)
C14 0.061(6) 0.106(8) 0.242(16) -0.060(10) -0.010(8) -0.004(5)
C15 0.062(5) 0.100(6) 0.130(9) -0.041(6) -0.010(5) 0.003(4)
C16 0.056(5) 0.118(8) 0.144(10) -0.051(7) -0.011(5) 0.015(5)
C17 0.097(9) 0.197(14) 0.185(15) -0.077(12) -0.034(10) 0.042(9)
C18 0.089(11) 0.42(4) 0.137(14) -0.060(19) -0.013(12) 0.108(15)
C19 0.081(10) 0.41(4) 0.160(16) 0.03(2) 0.017(12) 0.085(16)
C20 0.090(8) 0.174(13) 0.180(14) 0.029(11) -0.005(9) 0.025(8)

_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
As1 O3 1.755(5) . ?
As1 O10 1.770(6) . ?
As1 O6 1.776(6) . ?
As2 O11 1.750(5) . ?
As2 O8 1.771(6) . ?
As2 O6 1.779(6) . ?
V1 O4 1.594(6) . ?
V1 O1 1.912(5) . ?
V1 O2 1.932(6) . ?
V1 O3 2.003(5) 16_655 ?
V1 O11 2.005(6) 16_655 ?
V1 V2 2.851(2) . ?
V1 V3 3.013(2) . ?
V1 V3 3.036(2) 11_665 ?
V2 O5 1.585(7) . ?
V2 O1 1.918(6) . ?
V2 O2 1.942(5) . ?
V2 O10 1.998(6) . ?
V2 O8 2.009(6) 6_554 ?
V3 O9 1.581(6) . ?
V3 O2 1.932(6) . ?
V3 O1 1.937(6) 16_655 ?
V3 O3 1.985(5) 16_655 ?
V3 O11 1.995(5) 6_554 ?
V3 V1 3.036(2) 16_655 ?
V4 O7 1.552(9) . ?
V4 O8 1.980(6) . ?
V4 O8 1.980(6) 6_554 ?
V4 O10 1.986(6) 6_554 ?
V4 O10 1.986(6) . ?
Cu1 N4 1.983(10) . ?
Cu1 N3 1.989(9) . ?
Cu1 N1 1.992(11) . ?
Cu1 N2 2.004(10) . ?
O1 V3 1.937(6) 11_665 ?
O3 V3 1.985(5) 11_665 ?
O3 V1 2.003(5) 11_665 ?
O8 V2 2.009(6) 6_554 ?
O11 V3 1.995(5) 6_554 ?
O11 V1 2.005(6) 11_665 ?
N3 C11 1.256(15) . ?
N3 C15 1.359(11) . ?
N2 C6 1.311(12) . ?
N2 C10 1.330(16) . ?
N4 C16 1.336(13) . ?
N4 C20 1.336(16) . ?
N1 C1 1.38(2) . ?
N1 C5 1.389(15) . ?
C1 C2 1.57(2) . ?
C2 C3 1.31(2) . ?
C3 C4 1.38(2) . ?
C4 C5 1.358(19) . ?
C5 C6 1.407(16) . ?
C6 C7 1.394(16) . ?
C7 C8 1.356(18) . ?
C8 C9 1.322(19) . ?
C9 C10 1.368(18) . ?
C11 C12 1.370(19) . ?
C12 C13 1.32(2) . ?
C13 C14 1.39(2) . ?
C14 C15 1.427(15) . ?
C15 C16 1.459(14) . ?
C16 C17 1.389(16) . ?
C17 C18 1.41(3) . ?
C18 C19 1.20(4) . ?
C19 C20 1.42(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 As1 O10 98.4(3) . . ?
O3 As1 O6 99.8(3) . . ?
O10 As1 O6 99.2(3) . . ?
O11 As2 O8 99.4(3) . . ?
O11 As2 O6 98.9(3) . . ?
O8 As2 O6 99.0(3) . . ?
O4 V1 O1 111.3(3) . . ?
O4 V1 O2 108.5(3) . . ?
O1 V1 O2 84.2(2) . . ?
O4 V1 O3 109.6(3) . 16_655 ?
O1 V1 O3 138.8(2) . 16_655 ?
O2 V1 O3 79.3(2) . 16_655 ?
O4 V1 O11 112.2(3) . 16_655 ?
O1 V1 O11 78.5(2) . 16_655 ?
O2 V1 O11 139.2(2) . 16_655 ?
O3 V1 O11 89.9(2) 16_655 16_655 ?
O4 V1 V2 112.3(2) . . ?
O1 V1 V2 41.97(17) . . ?
O2 V1 V2 42.75(16) . . ?
O3 V1 V2 115.99(16) 16_655 . ?
O11 V1 V2 114.93(16) 16_655 . ?
O4 V1 V3 112.2(2) . . ?
O1 V1 V3 116.24(18) . . ?
O2 V1 V3 38.74(16) . . ?
O3 V1 V3 40.71(15) 16_655 . ?
O11 V1 V3 122.15(16) 16_655 . ?
V2 V1 V3 79.01(5) . . ?
O4 V1 V3 115.3(2) . 11_665 ?
O1 V1 V3 38.24(17) . 11_665 ?
O2 V1 V3 116.37(16) . 11_665 ?
O3 V1 V3 122.18(18) 16_655 11_665 ?
O11 V1 V3 40.49(15) 16_655 11_665 ?
V2 V1 V3 78.07(5) . 11_665 ?
V3 V1 V3 132.12(7) . 11_665 ?
O5 V2 O1 108.5(3) . . ?
O5 V2 O2 110.5(3) . . ?
O1 V2 O2 83.8(2) . . ?
O5 V2 O10 106.7(3) . . ?
O1 V2 O10 88.8(2) . . ?
O2 V2 O10 142.6(2) . . ?
O5 V2 O8 108.9(3) . 6_554 ?
O1 V2 O8 142.3(2) . 6_554 ?
O2 V2 O8 87.4(2) . 6_554 ?
O10 V2 O8 76.4(2) . 6_554 ?
O5 V2 V1 111.7(3) . . ?
O1 V2 V1 41.82(15) . . ?
O2 V2 V1 42.47(17) . . ?
O10 V2 V1 124.43(18) . . ?
O8 V2 V1 123.68(18) 6_554 . ?
O9 V3 O2 110.0(3) . . ?
O9 V3 O1 109.8(3) . 16_655 ?
O2 V3 O1 140.2(2) . 16_655 ?
O9 V3 O3 106.4(3) . 16_655 ?
O2 V3 O3 79.7(2) . 16_655 ?
O1 V3 O3 89.8(2) 16_655 16_655 ?
O9 V3 O11 107.6(3) . 6_554 ?
O2 V3 O11 89.4(2) . 6_554 ?
O1 V3 O11 78.2(2) 16_655 6_554 ?
O3 V3 O11 146.0(2) 16_655 6_554 ?
O9 V3 V1 111.1(2) . . ?
O2 V3 V1 38.74(17) . . ?
O1 V3 V1 122.79(17) 16_655 . ?
O3 V3 V1 41.15(15) 16_655 . ?
O11 V3 V1 123.08(17) 6_554 . ?
O9 V3 V1 111.2(2) . 16_655 ?
O2 V3 V1 122.60(17) . 16_655 ?
O1 V3 V1 37.66(15) 16_655 16_655 ?
O3 V3 V1 122.90(18) 16_655 16_655 ?
O11 V3 V1 40.75(17) 6_554 16_655 ?
V1 V3 V1 137.68(7) . 16_655 ?
O7 V4 O8 109.30(17) . . ?
O7 V4 O8 109.30(17) . 6_554 ?
O8 V4 O8 141.4(3) . 6_554 ?
O7 V4 O10 109.67(17) . 6_554 ?
O8 V4 O10 77.4(2) . 6_554 ?
O8 V4 O10 89.8(2) 6_554 6_554 ?
O7 V4 O10 109.67(17) . . ?
O8 V4 O10 89.8(2) . . ?
O8 V4 O10 77.4(2) 6_554 . ?
O10 V4 O10 140.7(3) 6_554 . ?
N4 Cu1 N3 82.2(4) . . ?
N4 Cu1 N1 132.0(4) . . ?
N3 Cu1 N1 123.2(4) . . ?
N4 Cu1 N2 129.5(4) . . ?
N3 Cu1 N2 115.3(4) . . ?
N1 Cu1 N2 79.6(5) . . ?
V1 O1 V2 96.2(2) . . ?
V1 O1 V3 104.1(3) . 11_665 ?
V2 O1 V3 148.4(3) . 11_665 ?
V3 O2 V1 102.5(3) . . ?
V3 O2 V2 149.0(3) . . ?
V1 O2 V2 94.8(2) . . ?
As1 O3 V3 124.2(3) . 11_665 ?
As1 O3 V1 137.4(3) . 11_665 ?
V3 O3 V1 98.1(2) 11_665 11_665 ?
As1 O6 As2 130.7(4) . . ?
As2 O8 V4 135.2(3) . . ?
As2 O8 V2 121.6(3) . 6_554 ?
V4 O8 V2 102.9(3) . 6_554 ?
As1 O10 V4 134.7(3) . . ?
As1 O10 V2 121.7(3) . . ?
V4 O10 V2 103.2(3) . . ?
As2 O11 V3 122.6(3) . 6_554 ?
As2 O11 V1 138.5(3) . 11_665 ?
V3 O11 V1 98.8(2) 6_554 11_665 ?
C11 N3 C15 116.8(10) . . ?
C11 N3 Cu1 129.7(9) . . ?
C15 N3 Cu1 113.1(7) . . ?
C6 N2 C10 112.5(12) . . ?
C6 N2 Cu1 118.2(10) . . ?
C10 N2 Cu1 128.9(8) . . ?
C16 N4 C20 117.3(12) . . ?
C16 N4 Cu1 113.6(8) . . ?
C20 N4 Cu1 128.5(10) . . ?
C1 N1 C5 126.0(14) . . ?
C1 N1 Cu1 122.2(11) . . ?
C5 N1 Cu1 111.5(9) . . ?
N1 C1 C2 115.6(18) . . ?
C3 C2 C1 110(2) . . ?
C2 C3 C4 133(2) . . ?
C5 C4 C3 115.9(19) . . ?
C4 C5 N1 118.3(15) . . ?
C4 C5 C6 122.8(14) . . ?
N1 C5 C6 118.9(10) . . ?
N2 C6 C7 125.7(14) . . ?
N2 C6 C5 111.3(13) . . ?
C7 C6 C5 122.9(11) . . ?
C8 C7 C6 115.3(13) . . ?
C9 C8 C7 123.7(18) . . ?
C8 C9 C10 114.1(19) . . ?
N2 C10 C9 128.7(15) . . ?
N3 C11 C12 128.2(14) . . ?
C13 C12 C11 117.2(17) . . ?
C12 C13 C14 119.8(14) . . ?
C13 C14 C15 118.4(13) . . ?
N3 C15 C14 119.5(12) . . ?
N3 C15 C16 114.6(9) . . ?
C14 C15 C16 125.8(10) . . ?
N4 C16 C17 121.1(14) . . ?
N4 C16 C15 115.4(9) . . ?
C17 C16 C15 123.5(12) . . ?
C16 C17 C18 118.1(18) . . ?
C19 C18 C17 120(2) . . ?
C18 C19 C20 122(2) . . ?
N4 C20 C19 120.8(17) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.089
_database_code_depnum_ccdc_archive 'CCDC 973724'
#######################################################################
#
#                 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_k

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H66 As8 Cu4 N16 O43 V14'
_chemical_formula_weight         3698.33

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Aba2

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

_cell_length_a                   26.4776(12)
_cell_length_b                   16.8267(11)
_cell_length_c                   27.5248(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     12263.1(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7200
_exptl_absorpt_coefficient_mu    3.919
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_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            36617
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0657
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         27.13
_reflns_number_total             12718
_reflns_number_gt                9099
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0919P)^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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.435(13)
_refine_ls_number_reflns         12718
_refine_ls_number_parameters     819
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.1519
_refine_ls_wR_factor_gt          0.1337
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.009
_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 0.12263(3) 0.94276(6) 0.14192(10) 0.0338(2) Uani 1 1 d . . .
As2 As 0.09760(3) 1.13138(6) 0.14078(10) 0.0343(2) Uani 1 1 d . . .
As3 As -0.03497(4) 0.80572(6) 0.36538(10) 0.0420(2) Uani 1 1 d . . .
As4 As -0.08416(4) 1.15234(6) 0.36490(10) 0.0424(2) Uani 1 1 d . . .
Cu2 Cu 0.25721(6) 0.63355(8) 0.50171(11) 0.0567(4) Uani 1 1 d . . .
V1 V 0.03231(5) 0.76811(9) 0.25774(11) 0.0354(3) Uani 1 1 d . . .
V2 V 0.02169(5) 0.83251(9) 0.16297(11) 0.0324(3) Uani 1 1 d . . .
V3 V -0.12433(5) 1.12485(9) 0.25326(11) 0.0355(3) Uani 1 1 d . . .
V4 V -0.10434(6) 0.96170(10) 0.34254(11) 0.0356(3) Uani 1 1 d . . .
V5 V -0.08068(5) 0.80066(9) 0.25319(11) 0.0332(3) Uani 1 1 d . . .
V6 V 0.0000 1.0000 0.38830(12) 0.0327(5) Uani 1 2 d S . .
V7 V 0.0000 1.0000 0.11718(12) 0.0300(4) Uani 1 2 d S . .
V8 V -0.14688(5) 0.94831(9) 0.24863(11) 0.0323(3) Uani 1 1 d . . .
Cu1 Cu -0.24082(5) 1.10838(9) 0.50269(11) 0.0595(4) Uani 1 1 d . . .
O1 O -0.1750(2) 1.1765(4) 0.2527(3) 0.0506(17) Uani 1 1 d . . .
O2 O -0.0782(3) 1.1720(4) 0.3027(3) 0.0441(16) Uani 1 1 d . . .
O3 O 0.0283(3) 0.7970(4) 0.3862(3) 0.0473(17) Uani 1 1 d . . .
O4 O 0.1272(2) 1.0416(4) 0.1205(2) 0.0348(14) Uani 1 1 d . . .
O5 O -0.0398(2) 0.9100(4) 0.3641(3) 0.0397(14) Uani 1 1 d . . .
O6 O 0.0745(2) 0.8236(4) 0.2117(2) 0.0324(13) Uani 1 1 d . . .
O7 O 0.0278(2) 0.7668(4) 0.1222(3) 0.0437(16) Uani 1 1 d . . .
O8 O -0.1329(2) 1.0311(4) 0.2943(2) 0.0369(14) Uani 1 1 d . . .
O9 O -0.0256(2) 0.7860(4) 0.3034(2) 0.0362(14) Uani 1 1 d . . .
O10 O -0.0618(2) 1.0540(4) 0.3656(3) 0.0444(15) Uani 1 1 d . . .
O11 O -0.0215(2) 0.7910(4) 0.2126(2) 0.0358(14) Uani 1 1 d . . .
O12 O 0.1318(2) 0.9601(3) 0.2045(2) 0.0343(14) Uani 1 1 d . . .
O13 O 0.1112(2) 1.1266(4) 0.2026(2) 0.0355(14) Uani 1 1 d . . .
O14 O 0.0000 1.0000 0.4473(3) 0.046(2) Uani 1 2 d S . .
O15 O 0.03452(18) 1.0960(4) 0.1420(2) 0.0341(13) Uani 1 1 d . . .
O16 O -0.1108(2) 0.8815(4) 0.2934(2) 0.0326(13) Uani 1 1 d . . .
O17 O 0.05627(19) 0.9326(3) 0.1402(3) 0.0350(13) Uani 1 1 d . . .
O18 O 0.0000 1.0000 0.0602(3) 0.042(2) Uani 1 2 d S . .
O19 O 0.0462(3) 0.6755(4) 0.2575(3) 0.0542(18) Uani 1 1 d . . .
O20 O -0.1131(2) 0.7215(4) 0.2543(3) 0.0511(17) Uani 1 1 d . . .
O21 O -0.1440(3) 0.9446(4) 0.3838(3) 0.0485(17) Uani 1 1 d . . .
O22 O -0.2054(2) 0.9291(4) 0.2479(3) 0.0458(16) Uani 1 1 d . . .
N5 N 0.2625(3) 0.6741(5) 0.4318(3) 0.045(2) Uani 1 1 d . . .
N4 N -0.1684(3) 1.1546(5) 0.5112(3) 0.046(2) Uani 1 1 d . . .
N8 N 0.3267(3) 0.5991(4) 0.5265(3) 0.0428(19) Uani 1 1 d D . .
N6 N 0.1857(3) 0.6023(4) 0.4791(3) 0.050(2) Uani 1 1 d D . .
N1 N -0.3159(3) 1.1454(5) 0.5047(3) 0.049(2) Uani 1 1 d . . .
N2 N -0.2600(3) 1.0816(4) 0.4336(3) 0.059(2) Uani 1 1 d D . .
C18 C -0.1130(4) 1.1007(5) 0.6484(4) 0.068(3) Uani 1 1 d D . .
H18A H -0.1020 1.0895 0.6797 0.082 Uiso 1 1 calc R . .
C47 C 0.3364(4) 0.6220(5) 0.5722(4) 0.049(3) Uani 1 1 d D . .
C38 C 0.2172(4) 0.7331(6) 0.6442(5) 0.056(3) Uani 1 1 d . . .
H38A H 0.1892 0.7566 0.6588 0.067 Uiso 1 1 calc R . .
C42 C 0.3874(4) 0.6378(5) 0.6451(4) 0.064(3) Uani 1 1 d D . .
H42A H 0.4180 0.6299 0.6610 0.076 Uiso 1 1 calc R . .
C24 C -0.1475(3) 1.1330(4) 0.5541(3) 0.038(2) Uani 1 1 d D . .
C35 C 0.1768(4) 0.6246(4) 0.4319(3) 0.045(2) Uani 1 1 d D . .
C41 C 0.3498(4) 0.6744(5) 0.6685(4) 0.057(3) Uani 1 1 d D . .
H41A H 0.3548 0.6913 0.7003 0.068 Uiso 1 1 calc R . .
C43 C 0.3818(4) 0.6105(5) 0.5961(4) 0.049(3) Uani 1 1 d D . .
C48 C 0.2963(3) 0.6616(4) 0.5981(3) 0.038(2) Uani 1 1 d D . .
N7 N 0.2526(3) 0.6755(5) 0.5724(3) 0.0394(18) Uani 1 1 d . . .
C19 C -0.1606(3) 1.0728(5) 0.6342(4) 0.052(3) Uani 1 1 d D . .
C16 C -0.1001(4) 1.1596(5) 0.5701(4) 0.053(3) Uani 1 1 d D . .
N3 N -0.2247(3) 1.0642(4) 0.5704(3) 0.047(2) Uani 1 1 d D . .
C31 C 0.1302(5) 0.6148(5) 0.4090(4) 0.061(3) Uani 1 1 d D . .
C40 C 0.3020(4) 0.6880(5) 0.6458(4) 0.046(2) Uani 1 1 d D . .
C36 C 0.2198(4) 0.6586(4) 0.4058(3) 0.048(3) Uani 1 1 d D . .
C28 C 0.2134(5) 0.6816(5) 0.3564(3) 0.059(3) Uani 1 1 d D . .
C46 C 0.3650(5) 0.5617(5) 0.5025(4) 0.065(3) Uani 1 1 d D . .
H46A H 0.3594 0.5451 0.4707 0.078 Uiso 1 1 calc R . .
C6 C -0.3868(5) 1.0913(6) 0.3705(5) 0.076(4) Uani 1 1 d D . .
H6A H -0.4014 1.0797 0.3406 0.092 Uiso 1 1 calc R . .
C39 C 0.2611(5) 0.7215(7) 0.6700(5) 0.061(3) Uani 1 1 d . . .
H39A H 0.2633 0.7357 0.7026 0.074 Uiso 1 1 calc R . .
C27 C 0.2556(6) 0.7146(7) 0.3347(5) 0.074(4) Uani 1 1 d . . .
H27A H 0.2536 0.7304 0.3024 0.089 Uiso 1 1 calc R . .
C13 C -0.1398(5) 1.1939(7) 0.4811(4) 0.061(3) Uani 1 1 d . . .
H13A H -0.1522 1.2049 0.4503 0.074 Uiso 1 1 calc R . .
C12 C -0.3403(4) 1.1268(4) 0.4630(4) 0.049(3) Uani 1 1 d D . .
C21 C -0.2395(5) 1.0053(5) 0.6484(5) 0.073(4) Uani 1 1 d D . .
H21A H -0.2611 0.9768 0.6686 0.087 Uiso 1 1 calc R . .
C11 C -0.3105(4) 1.0931(4) 0.4243(4) 0.046(2) Uani 1 1 d D . .
C20 C -0.1929(5) 1.0302(5) 0.6644(4) 0.065(3) Uani 1 1 d D . .
H20A H -0.1828 1.0183 0.6960 0.078 Uiso 1 1 calc R . .
C4 C -0.3929(4) 1.1422(5) 0.4549(5) 0.059(3) Uani 1 1 d D . .
C23 C -0.1788(4) 1.0883(4) 0.5869(4) 0.044(2) Uani 1 1 d D . .
C1 C -0.3425(6) 1.1773(6) 0.5413(5) 0.073(4) Uani 1 1 d . . .
H1A H -0.3267 1.1893 0.5706 0.087 Uiso 1 1 calc R . .
C32 C 0.0897(4) 0.5800(5) 0.4359(5) 0.070(4) Uani 1 1 d D . .
H32A H 0.0581 0.5726 0.4218 0.084 Uiso 1 1 calc R . .
C34 C 0.1468(4) 0.5698(5) 0.5033(4) 0.062(3) Uani 1 1 d D . .
H34A H 0.1522 0.5543 0.5353 0.075 Uiso 1 1 calc R . .
C9 C -0.2481(6) 1.0338(6) 0.3531(5) 0.089(5) Uani 1 1 d D . .
H9A H -0.2255 1.0140 0.3303 0.106 Uiso 1 1 calc R . .
C22 C -0.2532(4) 1.0241(5) 0.6013(4) 0.052(3) Uani 1 1 d D . .
H22A H -0.2847 1.0072 0.5905 0.062 Uiso 1 1 calc R . .
C5 C -0.4143(5) 1.1235(7) 0.4082(6) 0.088(5) Uani 1 1 d D . .
H5A H -0.4485 1.1337 0.4032 0.106 Uiso 1 1 calc R . .
C33 C 0.0986(5) 0.5576(6) 0.4833(5) 0.079(4) Uani 1 1 d D . .
H33A H 0.0730 0.5347 0.5018 0.094 Uiso 1 1 calc R . .
C26 C 0.2987(6) 0.7246(7) 0.3583(5) 0.071(4) Uani 1 1 d . . .
H26A H 0.3271 0.7451 0.3428 0.085 Uiso 1 1 calc R . .
C8 C -0.2982(7) 1.0441(5) 0.3420(4) 0.089(5) Uani 1 1 d D . .
H8A H -0.3102 1.0313 0.3112 0.106 Uiso 1 1 calc R . .
C3 C -0.4182(5) 1.1772(8) 0.4932(7) 0.082(5) Uani 1 1 d . . .
H3A H -0.4522 1.1904 0.4900 0.099 Uiso 1 1 calc R . .
C10 C -0.2321(5) 1.0540(5) 0.3997(5) 0.085(5) Uani 1 1 d D . .
H10A H -0.1981 1.0467 0.4068 0.101 Uiso 1 1 calc R . .
C7 C -0.3334(4) 1.0764(5) 0.3801(4) 0.056(3) Uani 1 1 d D . .
C17 C -0.0824(5) 1.1427(6) 0.6190(5) 0.076(4) Uani 1 1 d D . .
H17A H -0.0510 1.1603 0.6296 0.091 Uiso 1 1 calc R . .
C37 C 0.2154(4) 0.7087(6) 0.5956(4) 0.050(3) Uani 1 1 d . . .
H37A H 0.1855 0.7168 0.5787 0.060 Uiso 1 1 calc R . .
C25 C 0.2999(5) 0.7032(7) 0.4075(5) 0.060(3) Uani 1 1 d . . .
H25A H 0.3301 0.7106 0.4241 0.072 Uiso 1 1 calc R . .
C2 C -0.3939(6) 1.1924(8) 0.5355(6) 0.082(5) Uani 1 1 d . . .
H2A H -0.4120 1.2136 0.5613 0.098 Uiso 1 1 calc R . .
OW1 O 0.0000 1.0000 0.2504(9) 0.153(7) Uani 1 2 d S . .
C30 C 0.1243(6) 0.6383(5) 0.3591(4) 0.073(4) Uani 1 1 d D . .
H30A H 0.0935 0.6322 0.3434 0.087 Uiso 1 1 calc R . .
C45 C 0.4104(5) 0.5479(6) 0.5227(5) 0.080(4) Uani 1 1 d D . .
H45A H 0.4354 0.5223 0.5050 0.096 Uiso 1 1 calc R . .
C15 C -0.0699(6) 1.2046(8) 0.5357(6) 0.082(4) Uani 1 1 d . . .
H15A H -0.0374 1.2217 0.5431 0.098 Uiso 1 1 calc R . .
C14 C -0.0915(5) 1.2201(8) 0.4930(5) 0.076(4) Uani 1 1 d . . .
H14A H -0.0736 1.2497 0.4702 0.091 Uiso 1 1 calc R . .
C44 C 0.4201(5) 0.5728(6) 0.5714(5) 0.081(4) Uani 1 1 d D . .
H44A H 0.4512 0.5638 0.5860 0.098 Uiso 1 1 calc R . .
C29 C 0.1656(6) 0.6706(5) 0.3348(4) 0.072(4) Uani 1 1 d D . .
H29A H 0.1614 0.6857 0.3025 0.087 Uiso 1 1 calc 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 0.0274(4) 0.0479(5) 0.0260(4) -0.0069(4) 0.0024(4) 0.0010(4)
As2 0.0307(4) 0.0455(5) 0.0267(4) 0.0034(4) 0.0022(4) -0.0063(4)
As3 0.0487(5) 0.0447(5) 0.0326(5) 0.0093(4) 0.0007(4) -0.0039(4)
As4 0.0426(5) 0.0504(6) 0.0342(5) -0.0061(5) 0.0069(4) 0.0054(4)
Cu2 0.0722(9) 0.0661(9) 0.0317(7) 0.0002(6) -0.0105(6) -0.0066(7)
V1 0.0354(8) 0.0338(8) 0.0368(8) 0.0011(7) 0.0001(7) 0.0052(6)
V2 0.0289(7) 0.0390(8) 0.0292(8) -0.0049(6) 0.0044(6) -0.0005(6)
V3 0.0342(7) 0.0424(9) 0.0300(7) 0.0022(7) 0.0016(7) 0.0077(6)
V4 0.0346(8) 0.0477(9) 0.0245(8) 0.0021(6) 0.0032(6) 0.0012(7)
V5 0.0332(7) 0.0376(8) 0.0289(7) 0.0020(7) 0.0020(6) -0.0040(6)
V6 0.0313(10) 0.0462(13) 0.0206(10) 0.000 0.000 -0.0013(9)
V7 0.0227(9) 0.0438(13) 0.0234(10) 0.000 0.000 -0.0032(9)
V8 0.0251(6) 0.0440(9) 0.0278(8) 0.0037(7) 0.0018(6) 0.0023(6)
Cu1 0.0600(8) 0.0668(9) 0.0517(8) -0.0046(7) -0.0066(7) 0.0081(7)
O1 0.050(4) 0.053(4) 0.049(4) 0.007(4) 0.010(4) 0.019(3)
O2 0.047(4) 0.051(4) 0.035(4) 0.001(3) -0.002(3) 0.001(3)
O3 0.052(4) 0.055(4) 0.034(4) 0.012(3) -0.003(3) 0.005(3)
O4 0.030(3) 0.054(4) 0.021(3) -0.001(3) 0.007(2) -0.001(3)
O5 0.045(3) 0.045(4) 0.030(3) -0.002(3) -0.009(3) -0.004(3)
O6 0.026(3) 0.039(4) 0.032(3) -0.001(3) -0.001(2) 0.005(3)
O7 0.039(3) 0.049(4) 0.043(4) -0.015(3) 0.011(3) -0.006(3)
O8 0.033(3) 0.048(4) 0.030(3) 0.003(3) 0.003(2) 0.012(3)
O9 0.037(3) 0.046(4) 0.025(3) 0.000(3) -0.001(2) 0.002(3)
O10 0.050(4) 0.045(4) 0.038(4) 0.003(3) 0.001(3) 0.005(3)
O11 0.037(3) 0.039(4) 0.032(3) 0.000(3) 0.002(3) 0.000(3)
O12 0.047(4) 0.032(3) 0.025(3) -0.001(2) -0.002(3) 0.000(3)
O13 0.031(3) 0.046(4) 0.029(3) 0.002(3) 0.001(2) 0.000(3)
O14 0.044(5) 0.077(7) 0.018(5) 0.000 0.000 -0.004(5)
O15 0.020(2) 0.052(4) 0.031(3) -0.001(3) 0.004(3) -0.008(2)
O16 0.032(3) 0.041(4) 0.025(3) -0.004(2) 0.004(2) 0.005(3)
O17 0.023(3) 0.043(3) 0.039(3) 0.003(3) -0.001(3) -0.003(2)
O18 0.028(4) 0.067(7) 0.032(5) 0.000 0.000 -0.013(4)
O19 0.069(5) 0.037(4) 0.057(5) 0.004(3) 0.004(4) 0.015(3)
O20 0.051(4) 0.052(4) 0.050(4) 0.001(4) 0.007(4) -0.009(3)
O21 0.053(4) 0.063(5) 0.029(4) 0.004(3) 0.001(3) 0.000(3)
O22 0.032(3) 0.060(4) 0.046(4) 0.014(3) 0.001(3) -0.001(3)
N5 0.056(5) 0.043(5) 0.036(5) 0.002(4) 0.000(4) 0.000(4)
N4 0.050(5) 0.044(5) 0.045(5) -0.005(4) 0.018(4) 0.002(4)
N8 0.049(5) 0.054(5) 0.025(4) -0.007(4) 0.003(3) -0.003(4)
N6 0.067(6) 0.049(5) 0.034(5) 0.001(4) -0.009(4) -0.006(4)
N1 0.063(5) 0.032(4) 0.052(5) 0.005(4) 0.009(5) 0.006(4)
N2 0.055(5) 0.072(7) 0.049(6) -0.018(5) 0.000(4) 0.017(5)
C18 0.077(8) 0.077(9) 0.051(8) 0.010(6) -0.009(6) 0.012(7)
C47 0.064(7) 0.045(6) 0.038(6) 0.003(4) 0.003(5) -0.014(5)
C38 0.054(6) 0.054(7) 0.060(7) -0.009(6) 0.024(6) -0.002(5)
C42 0.043(6) 0.087(9) 0.062(8) 0.008(7) -0.020(6) -0.023(6)
C24 0.045(5) 0.031(5) 0.038(5) 0.000(4) 0.008(4) 0.002(4)
C35 0.070(7) 0.025(5) 0.039(6) 0.007(4) -0.001(5) -0.006(5)
C41 0.057(7) 0.073(8) 0.041(6) -0.015(5) -0.004(5) -0.025(6)
C43 0.036(5) 0.069(7) 0.040(6) 0.006(5) 0.003(4) -0.006(5)
C48 0.038(5) 0.043(5) 0.034(5) 0.001(4) 0.004(4) -0.007(4)
N7 0.046(4) 0.047(5) 0.025(4) 0.002(3) -0.003(3) -0.004(4)
C19 0.059(6) 0.051(6) 0.048(7) -0.001(5) -0.003(5) 0.003(5)
C16 0.065(7) 0.046(6) 0.047(6) -0.003(5) 0.005(5) -0.004(5)
N3 0.036(4) 0.048(5) 0.056(5) -0.003(4) 0.010(4) 0.001(4)
C31 0.094(9) 0.040(6) 0.048(7) -0.004(5) -0.010(6) 0.010(6)
C40 0.056(6) 0.046(6) 0.037(5) 0.000(5) 0.000(5) -0.003(5)
C36 0.079(8) 0.037(6) 0.029(5) -0.004(4) 0.000(5) 0.003(5)
C28 0.106(10) 0.044(6) 0.027(6) 0.010(4) -0.001(6) 0.011(6)
C46 0.101(10) 0.049(7) 0.045(7) -0.001(5) 0.014(7) 0.011(6)
C6 0.078(9) 0.074(9) 0.078(10) 0.004(8) -0.003(8) -0.006(7)
C39 0.071(8) 0.066(8) 0.047(7) -0.020(6) 0.007(6) -0.008(6)
C27 0.127(13) 0.057(8) 0.039(7) 0.010(6) 0.018(8) 0.000(8)
C13 0.081(9) 0.058(7) 0.045(7) 0.011(5) 0.018(6) 0.007(6)
C12 0.065(7) 0.031(5) 0.052(7) -0.001(4) 0.011(5) 0.004(5)
C21 0.074(8) 0.052(7) 0.093(11) 0.013(7) 0.051(8) 0.003(6)
C11 0.051(6) 0.033(5) 0.053(6) -0.004(4) 0.013(5) 0.003(5)
C20 0.079(9) 0.057(7) 0.058(7) 0.025(6) 0.010(6) 0.023(6)
C4 0.051(6) 0.047(7) 0.078(9) 0.017(6) 0.014(6) 0.022(5)
C23 0.051(6) 0.039(5) 0.042(6) -0.003(4) 0.013(5) -0.001(5)
C1 0.119(11) 0.040(7) 0.059(8) -0.012(5) 0.058(8) -0.002(7)
C32 0.043(6) 0.076(9) 0.092(11) 0.009(8) -0.021(6) -0.004(6)
C34 0.070(8) 0.075(8) 0.042(7) 0.005(6) 0.012(6) 0.001(6)
C9 0.093(11) 0.108(12) 0.066(10) -0.020(8) 0.000(8) 0.028(9)
C22 0.045(5) 0.050(6) 0.060(7) 0.018(5) 0.021(5) 0.012(5)
C5 0.055(8) 0.099(12) 0.111(13) 0.028(10) -0.030(8) -0.013(8)
C33 0.055(7) 0.087(10) 0.094(12) -0.022(8) 0.015(7) -0.027(7)
C26 0.096(10) 0.051(7) 0.065(9) 0.012(6) 0.036(8) 0.004(7)
C8 0.156(16) 0.074(9) 0.036(7) -0.010(6) 0.007(8) -0.035(10)
C3 0.065(8) 0.065(9) 0.117(14) 0.000(9) 0.035(9) 0.021(7)
C10 0.075(9) 0.103(12) 0.075(10) -0.019(8) 0.030(8) 0.039(8)
C7 0.059(7) 0.048(6) 0.062(8) 0.013(5) -0.016(6) 0.004(5)
C17 0.062(8) 0.093(11) 0.074(9) 0.015(8) -0.007(7) -0.006(7)
C37 0.055(6) 0.045(6) 0.049(6) 0.003(5) -0.006(5) -0.001(5)
C25 0.063(7) 0.047(7) 0.069(8) -0.005(6) 0.011(6) 0.008(6)
C2 0.086(10) 0.063(9) 0.096(12) 0.002(8) 0.059(9) 0.020(8)
OW1 0.127(15) 0.20(2) 0.135(18) 0.000 0.000 0.016(14)
C30 0.097(10) 0.059(8) 0.062(9) 0.013(6) -0.031(8) 0.009(7)
C45 0.059(8) 0.111(12) 0.069(9) -0.011(8) 0.026(7) 0.012(8)
C15 0.078(9) 0.052(8) 0.117(13) 0.001(8) 0.033(9) -0.027(7)
C14 0.087(10) 0.075(9) 0.065(9) 0.012(7) 0.026(7) -0.023(8)
C44 0.046(6) 0.107(11) 0.092(11) 0.001(9) 0.009(7) -0.010(7)
C29 0.123(12) 0.063(8) 0.031(6) 0.012(5) -0.013(7) 0.016(8)

_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
As1 O12 1.763(6) . ?
As1 O17 1.766(5) . ?
As1 O4 1.769(6) . ?
As2 O13 1.741(6) . ?
As2 O15 1.774(5) . ?
As2 O4 1.791(6) . ?
As3 O9 1.756(6) . ?
As3 O5 1.760(6) . ?
As3 O3 1.777(7) . ?
As4 O2 1.752(7) . ?
As4 O10 1.757(6) . ?
As4 O3 1.804(7) 2_575 ?
Cu2 N8 2.047(8) . ?
Cu2 N5 2.048(8) . ?
Cu2 N6 2.062(9) . ?
Cu2 N7 2.073(8) . ?
V1 O19 1.602(6) . ?
V1 O11 1.928(6) . ?
V1 O6 1.930(6) . ?
V1 O9 2.005(6) . ?
V1 O2 2.006(7) 2_575 ?
V1 V2 2.839(2) . ?
V1 V3 3.032(2) 2_575 ?
V1 V5 3.044(2) . ?
V2 O7 1.585(6) . ?
V2 O11 1.914(6) . ?
V2 O6 1.943(6) . ?
V2 O15 1.999(6) 2_575 ?
V2 O17 2.017(6) . ?
V3 O1 1.598(6) . ?
V3 O6 1.950(6) 2_575 ?
V3 O8 1.952(6) . ?
V3 O12 1.972(6) 2_575 ?
V3 O2 1.992(7) . ?
V3 V1 3.032(2) 2_575 ?
V3 V8 3.033(2) . ?
V4 O21 1.572(7) . ?
V4 O16 1.919(6) . ?
V4 O8 1.925(6) . ?
V4 O5 2.007(6) . ?
V4 O10 2.021(7) . ?
V4 V8 2.829(2) . ?
V4 V6 3.1040(17) . ?
V5 O20 1.586(7) . ?
V5 O16 1.926(6) . ?
V5 O11 1.931(6) . ?
V5 O13 2.022(6) 2_575 ?
V5 O9 2.023(6) . ?
V5 V8 3.043(2) . ?
V6 O14 1.623(9) . ?
V6 O5 1.962(6) . ?
V6 O5 1.962(6) 2_575 ?
V6 O10 1.974(6) 2_575 ?
V6 O10 1.974(6) . ?
V6 V4 3.1040(17) 2_575 ?
V7 O18 1.569(9) . ?
V7 O17 1.977(6) 2_575 ?
V7 O17 1.977(6) . ?
V7 O15 1.977(6) . ?
V7 O15 1.977(6) 2_575 ?
V8 O22 1.584(6) . ?
V8 O8 1.912(7) . ?
V8 O16 1.922(6) . ?
V8 O12 2.002(6) 2_575 ?
V8 O13 2.021(6) 2_575 ?
Cu1 N2 2.019(9) . ?
Cu1 N3 2.052(9) . ?
Cu1 N4 2.082(9) . ?
Cu1 N1 2.083(9) . ?
O2 V1 2.006(7) 2_575 ?
O3 As4 1.804(7) 2_575 ?
O6 V3 1.950(6) 2_575 ?
O12 V3 1.972(6) 2_575 ?
O12 V8 2.002(6) 2_575 ?
O13 V8 2.021(6) 2_575 ?
O13 V5 2.022(6) 2_575 ?
O15 V2 1.999(6) 2_575 ?
N5 C25 1.290(14) . ?
N5 C36 1.362(13) . ?
N4 C13 1.302(13) . ?
N4 C24 1.356(13) . ?
N8 C47 1.339(12) . ?
N8 C46 1.364(14) . ?
N6 C34 1.342(14) . ?
N6 C35 1.372(12) . ?
N1 C1 1.342(12) . ?
N1 C12 1.356(14) . ?
N2 C10 1.277(14) . ?
N2 C11 1.375(14) . ?
C18 C17 1.346(17) . ?
C18 C19 1.399(14) . ?
C47 C43 1.382(14) . ?
C47 C48 1.443(14) . ?
C38 C39 1.375(17) . ?
C38 C37 1.399(15) . ?
C42 C41 1.338(16) . ?
C42 C43 1.433(16) . ?
C24 C16 1.404(15) . ?
C24 C23 1.437(13) . ?
C35 C31 1.397(16) . ?
C35 C36 1.463(15) . ?
C41 C40 1.429(14) . ?
C43 C44 1.374(17) . ?
C48 N7 1.377(12) . ?
C48 C40 1.394(13) . ?
N7 C37 1.299(13) . ?
C19 C20 1.394(15) . ?
C19 C23 1.413(15) . ?
C16 C15 1.452(17) . ?
C16 C17 1.452(17) . ?
N3 C22 1.321(13) . ?
N3 C23 1.357(13) . ?
C31 C32 1.429(17) . ?
C31 C30 1.437(16) . ?
C40 C39 1.392(15) . ?
C36 C28 1.425(13) . ?
C28 C27 1.383(18) . ?
C28 C29 1.411(18) . ?
C46 C45 1.345(19) . ?
C6 C5 1.38(2) . ?
C6 C7 1.461(16) . ?
C27 C26 1.325(19) . ?
C13 C14 1.390(18) . ?
C12 C4 1.432(15) . ?
C12 C11 1.442(14) . ?
C21 C20 1.375(18) . ?
C21 C22 1.385(17) . ?
C11 C7 1.389(15) . ?
C4 C3 1.384(18) . ?
C4 C5 1.44(2) . ?
C1 C2 1.39(2) . ?
C32 C33 1.378(19) . ?
C34 C33 1.407(17) . ?
C9 C8 1.37(2) . ?
C9 C10 1.393(19) . ?
C26 C25 1.403(17) . ?
C8 C7 1.504(19) . ?
C3 C2 1.35(2) . ?
C30 C29 1.392(19) . ?
C45 C44 1.429(19) . ?
C15 C14 1.34(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
O12 As1 O17 100.3(3) . . ?
O12 As1 O4 99.2(3) . . ?
O17 As1 O4 98.7(3) . . ?
O13 As2 O15 99.3(3) . . ?
O13 As2 O4 100.1(3) . . ?
O15 As2 O4 97.7(3) . . ?
O9 As3 O5 100.3(3) . . ?
O9 As3 O3 99.5(3) . . ?
O5 As3 O3 99.1(3) . . ?
O2 As4 O10 99.1(3) . . ?
O2 As4 O3 98.9(3) . 2_575 ?
O10 As4 O3 99.5(3) . 2_575 ?
N8 Cu2 N5 110.3(3) . . ?
N8 Cu2 N6 148.7(2) . . ?
N5 Cu2 N6 82.2(3) . . ?
N8 Cu2 N7 80.6(3) . . ?
N5 Cu2 N7 140.6(3) . . ?
N6 Cu2 N7 108.4(3) . . ?
O19 V1 O11 111.2(3) . . ?
O19 V1 O6 109.6(3) . . ?
O11 V1 O6 84.7(3) . . ?
O19 V1 O9 108.9(3) . . ?
O11 V1 O9 78.9(2) . . ?
O6 V1 O9 141.4(3) . . ?
O19 V1 O2 110.6(3) . 2_575 ?
O11 V1 O2 138.1(3) . 2_575 ?
O6 V1 O2 79.1(3) . 2_575 ?
O9 V1 O2 90.1(3) . 2_575 ?
O19 V1 V2 113.0(3) . . ?
O11 V1 V2 42.17(18) . . ?
O6 V1 V2 43.04(17) . . ?
O9 V1 V2 116.25(18) . . ?
O2 V1 V2 115.8(2) 2_575 . ?
O19 V1 V3 113.2(3) . 2_575 ?
O11 V1 V3 116.6(2) . 2_575 ?
O6 V1 V3 38.84(18) . 2_575 ?
O9 V1 V3 123.42(19) . 2_575 ?
O2 V1 V3 40.50(19) 2_575 2_575 ?
V2 V1 V3 79.37(6) . 2_575 ?
O19 V1 V5 113.6(3) . . ?
O11 V1 V5 37.97(18) . . ?
O6 V1 V5 117.03(18) . . ?
O9 V1 V5 41.14(17) . . ?
O2 V1 V5 122.0(2) 2_575 . ?
V2 V1 V5 78.24(5) . . ?
V3 V1 V5 132.93(6) 2_575 . ?
O7 V2 O11 108.2(3) . . ?
O7 V2 O6 111.2(3) . . ?
O11 V2 O6 84.7(3) . . ?
O7 V2 O15 106.9(3) . 2_575 ?
O11 V2 O15 88.9(3) . 2_575 ?
O6 V2 O15 141.4(3) . 2_575 ?
O7 V2 O17 108.4(3) . . ?
O11 V2 O17 142.9(3) . . ?
O6 V2 O17 87.2(2) . . ?
O15 V2 O17 75.3(2) 2_575 . ?
O7 V2 V1 112.0(3) . . ?
O11 V2 V1 42.56(18) . . ?
O6 V2 V1 42.69(18) . . ?
O15 V2 V1 124.69(19) 2_575 . ?
O17 V2 V1 124.0(2) . . ?
O1 V3 O6 108.7(3) . 2_575 ?
O1 V3 O8 110.3(3) . . ?
O6 V3 O8 141.0(2) 2_575 . ?
O1 V3 O12 107.7(3) . 2_575 ?
O6 V3 O12 89.5(3) 2_575 2_575 ?
O8 V3 O12 78.2(2) . 2_575 ?
O1 V3 O2 107.7(3) . . ?
O6 V3 O2 79.0(3) 2_575 . ?
O8 V3 O2 89.9(3) . . ?
O12 V3 O2 144.6(3) 2_575 . ?
O1 V3 V1 110.6(3) . 2_575 ?
O6 V3 V1 38.37(18) 2_575 2_575 ?
O8 V3 V1 123.36(19) . 2_575 ?
O12 V3 V1 122.61(19) 2_575 2_575 ?
O2 V3 V1 40.8(2) . 2_575 ?
O1 V3 V8 111.5(3) . . ?
O6 V3 V8 122.96(19) 2_575 . ?
O8 V3 V8 37.83(19) . . ?
O12 V3 V8 40.63(17) 2_575 . ?
O2 V3 V8 122.6(2) . . ?
V1 V3 V8 137.88(6) 2_575 . ?
O21 V4 O16 108.7(3) . . ?
O21 V4 O8 110.3(3) . . ?
O16 V4 O8 84.6(3) . . ?
O21 V4 O5 106.0(3) . . ?
O16 V4 O5 88.8(3) . . ?
O8 V4 O5 143.3(3) . . ?
O21 V4 O10 106.6(3) . . ?
O16 V4 O10 144.3(3) . . ?
O8 V4 O10 88.2(3) . . ?
O5 V4 O10 76.5(3) . . ?
O21 V4 V8 112.3(3) . . ?
O16 V4 V8 42.62(18) . . ?
O8 V4 V8 42.3(2) . . ?
O5 V4 V8 125.1(2) . . ?
O10 V4 V8 124.7(2) . . ?
O21 V4 V6 109.8(3) . . ?
O16 V4 V6 120.77(18) . . ?
O8 V4 V6 120.3(2) . . ?
O5 V4 V6 38.02(17) . . ?
O10 V4 V6 38.48(17) . . ?
V8 V4 V6 137.88(7) . . ?
O20 V5 O16 111.0(3) . . ?
O20 V5 O11 112.3(3) . . ?
O16 V5 O11 136.7(3) . . ?
O20 V5 O13 107.7(3) . 2_575 ?
O16 V5 O13 78.6(2) . 2_575 ?
O11 V5 O13 88.7(3) . 2_575 ?
O20 V5 O9 106.0(3) . . ?
O16 V5 O9 89.6(3) . . ?
O11 V5 O9 78.4(2) . . ?
O13 V5 O9 146.3(3) 2_575 . ?
O20 V5 V8 112.0(3) . . ?
O16 V5 V8 37.69(18) . . ?
O11 V5 V8 120.8(2) . . ?
O13 V5 V8 41.18(17) 2_575 . ?
O9 V5 V8 122.87(19) . . ?
O20 V5 V1 112.4(3) . . ?
O16 V5 V1 120.71(19) . . ?
O11 V5 V1 37.89(18) . . ?
O13 V5 V1 122.03(18) 2_575 . ?
O9 V5 V1 40.69(17) . . ?
V8 V5 V1 135.62(6) . . ?
O14 V6 O5 109.9(2) . . ?
O14 V6 O5 109.9(2) . 2_575 ?
O5 V6 O5 140.3(4) . 2_575 ?
O14 V6 O10 108.5(2) . 2_575 ?
O5 V6 O10 89.0(3) . 2_575 ?
O5 V6 O10 78.6(3) 2_575 2_575 ?
O14 V6 O10 108.5(2) . . ?
O5 V6 O10 78.6(3) . . ?
O5 V6 O10 89.0(3) 2_575 . ?
O10 V6 O10 143.1(4) 2_575 . ?
O14 V6 V4 113.94(4) . . ?
O5 V6 V4 39.06(18) . . ?
O5 V6 V4 120.0(2) 2_575 . ?
O10 V6 V4 120.9(2) 2_575 . ?
O10 V6 V4 39.57(19) . . ?
O14 V6 V4 113.94(4) . 2_575 ?
O5 V6 V4 120.0(2) . 2_575 ?
O5 V6 V4 39.06(18) 2_575 2_575 ?
O10 V6 V4 39.57(19) 2_575 2_575 ?
O10 V6 V4 120.9(2) . 2_575 ?
V4 V6 V4 132.12(9) . 2_575 ?
O18 V7 O17 108.7(2) . 2_575 ?
O18 V7 O17 108.7(2) . . ?
O17 V7 O17 142.5(4) 2_575 . ?
O18 V7 O15 110.20(19) . . ?
O17 V7 O15 76.6(2) 2_575 . ?
O17 V7 O15 90.5(2) . . ?
O18 V7 O15 110.20(19) . 2_575 ?
O17 V7 O15 90.5(2) 2_575 2_575 ?
O17 V7 O15 76.6(2) . 2_575 ?
O15 V7 O15 139.6(4) . 2_575 ?
O22 V8 O8 110.3(3) . . ?
O22 V8 O16 112.1(3) . . ?
O8 V8 O16 84.8(3) . . ?
O22 V8 O12 110.1(3) . 2_575 ?
O8 V8 O12 78.4(2) . 2_575 ?
O16 V8 O12 137.7(3) . 2_575 ?
O22 V8 O13 108.8(3) . 2_575 ?
O8 V8 O13 140.9(2) . 2_575 ?
O16 V8 O13 78.7(2) . 2_575 ?
O12 V8 O13 90.4(3) 2_575 2_575 ?
O22 V8 V4 114.7(3) . . ?
O8 V8 V4 42.68(18) . . ?
O16 V8 V4 42.54(18) . . ?
O12 V8 V4 114.45(18) 2_575 . ?
O13 V8 V4 115.88(18) 2_575 . ?
O22 V8 V3 113.1(2) . . ?
O8 V8 V3 38.77(19) . . ?
O16 V8 V3 116.65(19) . . ?
O12 V8 V3 39.89(17) 2_575 . ?
O13 V8 V3 123.07(18) 2_575 . ?
V4 V8 V3 78.76(6) . . ?
O22 V8 V5 113.5(2) . . ?
O8 V8 V5 117.17(18) . . ?
O16 V8 V5 37.77(17) . . ?
O12 V8 V5 122.56(18) 2_575 . ?
O13 V8 V5 41.20(18) 2_575 . ?
V4 V8 V5 78.34(6) . . ?
V3 V8 V5 133.20(6) . . ?
N2 Cu1 N3 145.8(3) . . ?
N2 Cu1 N4 114.8(3) . . ?
N3 Cu1 N4 80.9(3) . . ?
N2 Cu1 N1 81.5(4) . . ?
N3 Cu1 N1 106.4(3) . . ?
N4 Cu1 N1 139.8(3) . . ?
As4 O2 V3 122.5(4) . . ?
As4 O2 V1 138.8(4) . 2_575 ?
V3 O2 V1 98.7(3) . 2_575 ?
As3 O3 As4 129.0(4) . 2_575 ?
As1 O4 As2 131.2(3) . . ?
As3 O5 V6 136.3(3) . . ?
As3 O5 V4 120.0(3) . . ?
V6 O5 V4 102.9(3) . . ?
V1 O6 V2 94.3(2) . . ?
V1 O6 V3 102.8(3) . 2_575 ?
V2 O6 V3 149.1(3) . 2_575 ?
V8 O8 V4 95.0(3) . . ?
V8 O8 V3 103.4(3) . . ?
V4 O8 V3 147.5(4) . . ?
As3 O9 V1 138.1(3) . . ?
As3 O9 V5 122.6(3) . . ?
V1 O9 V5 98.2(3) . . ?
As4 O10 V6 135.8(4) . . ?
As4 O10 V4 122.2(3) . . ?
V6 O10 V4 102.0(3) . . ?
V2 O11 V1 95.3(3) . . ?
V2 O11 V5 150.1(4) . . ?
V1 O11 V5 104.1(3) . . ?
As1 O12 V3 122.1(3) . 2_575 ?
As1 O12 V8 138.4(3) . 2_575 ?
V3 O12 V8 99.5(3) 2_575 2_575 ?
As2 O13 V8 137.5(4) . 2_575 ?
As2 O13 V5 124.2(3) . 2_575 ?
V8 O13 V5 97.6(3) 2_575 2_575 ?
As2 O15 V7 134.7(3) . . ?
As2 O15 V2 120.3(3) . 2_575 ?
V7 O15 V2 104.3(2) . 2_575 ?
V4 O16 V8 94.8(3) . . ?
V4 O16 V5 149.8(3) . . ?
V8 O16 V5 104.5(3) . . ?
As1 O17 V7 134.6(3) . . ?
As1 O17 V2 121.6(3) . . ?
V7 O17 V2 103.7(2) . . ?
C25 N5 C36 116.0(9) . . ?
C25 N5 Cu2 131.7(8) . . ?
C36 N5 Cu2 111.8(7) . . ?
C13 N4 C24 116.9(9) . . ?
C13 N4 Cu1 130.9(8) . . ?
C24 N4 Cu1 111.9(6) . . ?
C47 N8 C46 116.4(10) . . ?
C47 N8 Cu2 113.9(7) . . ?
C46 N8 Cu2 129.5(8) . . ?
C34 N6 C35 116.7(9) . . ?
C34 N6 Cu2 131.2(7) . . ?
C35 N6 Cu2 111.9(7) . . ?
C1 N1 C12 118.5(11) . . ?
C1 N1 Cu1 129.9(9) . . ?
C12 N1 Cu1 111.4(7) . . ?
C10 N2 C11 118.5(11) . . ?
C10 N2 Cu1 128.6(10) . . ?
C11 N2 Cu1 112.8(7) . . ?
C17 C18 C19 123.3(12) . . ?
N8 C47 C43 125.0(10) . . ?
N8 C47 C48 117.1(10) . . ?
C43 C47 C48 118.0(9) . . ?
C39 C38 C37 118.7(10) . . ?
C41 C42 C43 121.7(9) . . ?
N4 C24 C16 123.5(9) . . ?
N4 C24 C23 116.9(9) . . ?
C16 C24 C23 119.1(9) . . ?
N6 C35 C31 123.1(10) . . ?
N6 C35 C36 116.0(9) . . ?
C31 C35 C36 120.9(9) . . ?
C42 C41 C40 121.4(10) . . ?
C44 C43 C47 118.1(11) . . ?
C44 C43 C42 122.4(11) . . ?
C47 C43 C42 119.6(9) . . ?
N7 C48 C40 121.4(9) . . ?
N7 C48 C47 116.3(8) . . ?
C40 C48 C47 122.2(9) . . ?
C37 N7 C48 117.2(8) . . ?
C37 N7 Cu2 130.8(7) . . ?
C48 N7 Cu2 112.0(6) . . ?
C20 C19 C18 124.0(11) . . ?
C20 C19 C23 115.8(10) . . ?
C18 C19 C23 120.3(10) . . ?
C24 C16 C15 117.1(11) . . ?
C24 C16 C17 121.1(10) . . ?
C15 C16 C17 121.9(12) . . ?
C22 N3 C23 116.7(10) . . ?
C22 N3 Cu1 130.5(7) . . ?
C23 N3 Cu1 112.4(7) . . ?
C35 C31 C32 118.5(10) . . ?
C35 C31 C30 119.6(12) . . ?
C32 C31 C30 121.9(12) . . ?
C39 C40 C48 119.7(10) . . ?
C39 C40 C41 123.0(10) . . ?
C48 C40 C41 117.2(9) . . ?
N5 C36 C28 123.2(10) . . ?
N5 C36 C35 117.6(8) . . ?
C28 C36 C35 118.8(11) . . ?
C27 C28 C29 126.5(11) . . ?
C27 C28 C36 115.2(12) . . ?
C29 C28 C36 118.3(11) . . ?
C45 C46 N8 122.9(12) . . ?
C5 C6 C7 116.3(13) . . ?
C38 C39 C40 117.9(11) . . ?
C26 C27 C28 122.4(12) . . ?
N4 C13 C14 123.2(12) . . ?
N1 C12 C4 123.7(10) . . ?
N1 C12 C11 117.0(10) . . ?
C4 C12 C11 119.3(11) . . ?
C20 C21 C22 117.7(10) . . ?
N2 C11 C7 124.0(10) . . ?
N2 C11 C12 116.8(10) . . ?
C7 C11 C12 119.1(10) . . ?
C21 C20 C19 121.1(11) . . ?
C3 C4 C12 115.5(13) . . ?
C3 C4 C5 125.6(13) . . ?
C12 C4 C5 118.9(11) . . ?
N3 C23 C19 124.0(9) . . ?
N3 C23 C24 117.6(9) . . ?
C19 C23 C24 118.4(10) . . ?
N1 C1 C2 120.0(14) . . ?
C33 C32 C31 118.3(11) . . ?
N6 C34 C33 124.2(11) . . ?
C8 C9 C10 118.0(13) . . ?
N3 C22 C21 124.7(11) . . ?
C6 C5 C4 123.3(13) . . ?
C32 C33 C34 119.0(12) . . ?
C27 C26 C25 117.4(12) . . ?
C9 C8 C7 119.3(12) . . ?
C2 C3 C4 120.3(13) . . ?
N2 C10 C9 125.8(14) . . ?
C11 C7 C6 123.1(12) . . ?
C11 C7 C8 114.4(11) . . ?
C6 C7 C8 122.4(12) . . ?
C18 C17 C16 117.7(12) . . ?
N7 C37 C38 124.8(10) . . ?
N5 C25 C26 125.5(13) . . ?
C3 C2 C1 122.0(12) . . ?
C29 C30 C31 118.9(12) . . ?
C46 C45 C44 119.9(12) . . ?
C14 C15 C16 116.1(13) . . ?
C15 C14 C13 122.6(12) . . ?
C43 C44 C45 117.8(12) . . ?
C30 C29 C28 123.5(11) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.13
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.210
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.147
_database_code_depnum_ccdc_archive 'CCDC 973725'
#######################################################################
#
#                 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_k

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H50 As8 N24 Ni2 O49 V14'
_chemical_formula_weight         3032.94

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'
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'
Ni Ni 0.3393 1.1124 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   I4(1)/a

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'

_cell_length_a                   15.118(2)
_cell_length_b                   15.118(2)
_cell_length_c                   38.962(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8905(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5872
_exptl_absorpt_coefficient_mu    4.861
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_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            42022
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         27.47
_reflns_number_total             5056
_reflns_number_gt                3909
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+4.2952P] 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         5056
_refine_ls_number_parameters     302
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.1084
_refine_ls_wR_factor_gt          0.1029
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.011
_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 0.11943(3) 0.05938(3) 0.044716(11) 0.04985(13) Uani 1 1 d . . .
As2 As -0.22594(3) 0.25461(3) 0.045090(11) 0.05004(13) Uani 1 1 d . . .
V3 V -0.24779(4) 0.18012(4) 0.125455(17) 0.04086(16) Uani 1 1 d . . .
V4 V -0.12822(4) 0.02196(4) 0.129545(17) 0.04041(16) Uani 1 1 d . . .
V5 V -0.09390(4) 0.08512(4) 0.061034(17) 0.04472(17) Uani 1 1 d . . .
V6 V 0.0000 0.2500 0.02911(2) 0.0457(2) Uani 1 2 d S . .
Ni1 Ni 0.0000 -0.2500 0.29016(2) 0.0540(2) Uani 1 2 d S . .
O11 O -0.23505(16) 0.27445(16) 0.08967(7) 0.0442(6) Uani 1 1 d . . .
O10 O 0.0000 0.2500 -0.01179(11) 0.0685(13) Uani 1 2 d S . .
O9 O -0.03379(16) 0.01592(16) 0.09607(7) 0.0430(6) Uani 1 1 d . . .
O8 O -0.18150(16) 0.10065(16) 0.09668(7) 0.0434(6) Uani 1 1 d . . .
O7 O 0.19874(19) 0.1379(2) 0.03050(7) 0.0574(7) Uani 1 1 d . . .
O6 O 0.02426(17) 0.12870(19) 0.04487(7) 0.0508(7) Uani 1 1 d . . .
O5 O 0.14254(16) 0.06327(17) 0.08922(7) 0.0443(6) Uani 1 1 d . . .
O4 O -0.18124(18) -0.07107(17) 0.13045(8) 0.0547(7) Uani 1 1 d . . .
O3 O -0.11702(17) 0.20913(19) 0.04497(7) 0.0496(6) Uani 1 1 d . . .
O2 O -0.34943(18) 0.15111(19) 0.12630(9) 0.0624(8) Uani 1 1 d . . .
O1 O -0.1313(2) 0.0184(2) 0.03341(9) 0.0696(9) Uani 1 1 d . . .
N3 N -0.0925(2) -0.2050(2) 0.32473(11) 0.0578(9) Uani 1 1 d . . .
N1 N -0.0375(3) -0.3858(3) 0.29431(12) 0.0714(12) Uani 1 1 d . . .
N5 N -0.0828(3) -0.2158(3) 0.24881(12) 0.0713(11) Uani 1 1 d . . .
N2 N 0.0042(4) -0.5194(3) 0.30915(18) 0.106(2) Uani 1 1 d . . .
H2A H 0.0348 -0.5615 0.3181 0.128 Uiso 1 1 calc R . .
N4 N -0.1604(4) -0.0907(4) 0.34648(16) 0.106(2) Uani 1 1 d . . .
H5A H -0.1733 -0.0369 0.3516 0.127 Uiso 1 1 calc R . .
C6 C -0.0914(3) -0.1169(3) 0.32730(15) 0.0730(15) Uani 1 1 d . . .
C9 C -0.0437(4) -0.2294(4) 0.21913(14) 0.0776(15) Uani 1 1 d . . .
C3 C 0.0214(4) -0.4306(3) 0.31079(17) 0.0786(17) Uani 1 1 d . . .
C7 C -0.1608(4) -0.1740(4) 0.24200(18) 0.0835(17) Uani 1 1 d . . .
H7A H -0.2022 -0.1563 0.2582 0.100 Uiso 1 1 calc R . .
C4 C -0.1634(3) -0.2352(4) 0.34317(15) 0.0756(14) Uani 1 1 d . . .
H4A H -0.1793 -0.2942 0.3461 0.091 Uiso 1 1 calc R . .
C1 C -0.0976(5) -0.4481(4) 0.28099(19) 0.099(2) Uani 1 1 d . . .
H1A H -0.1470 -0.4345 0.2678 0.119 Uiso 1 1 calc R . .
C2 C -0.0736(6) -0.5277(5) 0.2898(2) 0.121(3) Uani 1 1 d . . .
H2B H -0.1027 -0.5801 0.2844 0.145 Uiso 1 1 calc R . .
C5 C -0.2070(5) -0.1640(6) 0.35662(18) 0.106(2) Uani 1 1 d . . .
H5B H -0.2580 -0.1650 0.3700 0.127 Uiso 1 1 calc R . .
OW2 O 0.0837(3) -0.6803(3) 0.32142(12) 0.0984(13) Uani 1 1 d . . .
OW1 O -0.5000 0.2500 0.1155(2) 0.130(3) Uani 1 2 d SU . .
C17 C -0.1677(6) -0.1626(5) 0.2075(2) 0.106(2) Uani 1 1 d . . .
H17B H -0.2141 -0.1357 0.1959 0.127 Uiso 1 1 calc R . .
N6 N -0.0941(4) -0.1979(4) 0.19345(14) 0.0969(18) Uani 1 1 d . . .
H17A H -0.0817 -0.1999 0.1719 0.116 Uiso 1 1 calc R . .
OW3 O 0.0000 0.2500 0.1250 0.1650(17) Uani 1 4 d SU . .

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 0.0505(2) 0.0585(2) 0.0405(2) -0.01142(17) -0.00211(17) 0.01935(19)
As2 0.0437(2) 0.0654(3) 0.0410(2) -0.01040(18) -0.01142(16) 0.01524(18)
V3 0.0367(3) 0.0399(3) 0.0460(4) -0.0104(3) 0.0014(2) -0.0016(2)
V4 0.0392(3) 0.0371(3) 0.0449(4) -0.0067(3) -0.0063(3) -0.0036(2)
V5 0.0438(3) 0.0534(4) 0.0369(4) -0.0138(3) -0.0089(3) 0.0115(3)
V6 0.0476(5) 0.0642(6) 0.0253(4) 0.000 0.000 0.0191(4)
Ni1 0.0630(5) 0.0402(4) 0.0587(5) 0.000 0.000 0.0063(3)
O11 0.0481(14) 0.0443(13) 0.0404(15) -0.0064(11) 0.0010(11) 0.0062(11)
O10 0.074(3) 0.100(3) 0.032(2) 0.000 0.000 0.032(3)
O9 0.0396(12) 0.0447(13) 0.0446(15) -0.0087(11) -0.0078(11) 0.0089(11)
O8 0.0415(13) 0.0478(13) 0.0410(14) -0.0091(11) -0.0060(11) 0.0082(11)
O7 0.0537(15) 0.0756(19) 0.0430(16) -0.0072(14) 0.0112(13) 0.0222(14)
O6 0.0457(14) 0.0635(17) 0.0433(16) -0.0014(13) 0.0005(11) 0.0189(13)
O5 0.0418(13) 0.0505(14) 0.0407(14) -0.0008(11) -0.0061(11) 0.0036(11)
O4 0.0515(15) 0.0420(14) 0.071(2) -0.0067(13) -0.0085(14) -0.0096(12)
O3 0.0436(14) 0.0664(17) 0.0389(15) -0.0025(12) -0.0015(11) 0.0191(13)
O2 0.0396(14) 0.0543(16) 0.093(3) -0.0154(15) 0.0002(14) -0.0053(13)
O1 0.075(2) 0.078(2) 0.056(2) -0.0315(16) -0.0174(16) 0.0124(18)
N3 0.057(2) 0.0481(19) 0.069(3) -0.0141(17) -0.0067(18) 0.0138(16)
N1 0.083(3) 0.047(2) 0.084(3) -0.009(2) 0.029(2) -0.001(2)
N5 0.077(3) 0.068(2) 0.069(3) 0.008(2) -0.011(2) -0.015(2)
N2 0.137(5) 0.042(2) 0.140(6) 0.007(3) 0.074(4) 0.009(3)
N4 0.109(4) 0.082(3) 0.126(5) -0.044(3) -0.022(4) 0.045(3)
C6 0.077(3) 0.056(3) 0.087(4) -0.026(3) -0.028(3) 0.030(3)
C9 0.106(4) 0.073(3) 0.053(3) 0.010(2) -0.011(3) -0.041(3)
C3 0.093(4) 0.039(2) 0.104(4) -0.002(3) 0.048(3) 0.001(3)
C7 0.085(4) 0.068(3) 0.097(5) 0.016(3) -0.027(3) -0.015(3)
C4 0.067(3) 0.084(3) 0.076(4) -0.016(3) 0.003(3) 0.013(3)
C1 0.115(5) 0.077(4) 0.107(5) -0.037(4) 0.054(4) -0.029(4)
C2 0.139(7) 0.077(4) 0.145(7) -0.033(4) 0.077(6) -0.027(5)
C5 0.081(4) 0.144(7) 0.094(5) -0.040(5) 0.006(4) 0.051(4)
OW2 0.091(3) 0.105(3) 0.099(3) -0.005(2) -0.038(2) -0.003(2)
OW1 0.129(3) 0.132(3) 0.129(3) 0.000 0.000 0.0020(10)
C17 0.118(6) 0.100(5) 0.098(6) 0.026(4) -0.046(5) -0.039(5)
N6 0.121(4) 0.104(4) 0.065(3) 0.016(3) -0.020(3) -0.050(4)
OW3 0.1652(17) 0.1652(17) 0.164(2) 0.000 0.000 0.000

_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
As1 O5 1.770(3) . ?
As1 O7 1.776(3) . ?
As1 O6 1.780(2) . ?
As2 O11 1.768(3) . ?
As2 O7 1.770(3) 6_454 ?
As2 O3 1.785(2) . ?
V3 O2 1.598(3) . ?
V3 O8 1.925(2) . ?
V3 O9 1.931(2) 15 ?
V3 O5 1.988(3) 15 ?
V3 O11 2.004(3) . ?
V3 V4 3.0016(9) . ?
V3 V4 3.0160(9) 15 ?
V4 O4 1.619(3) . ?
V4 O8 1.925(3) . ?
V4 O9 1.936(3) . ?
V4 O11 1.978(3) 12_666 ?
V4 O5 1.983(3) 15 ?
V4 V5 2.8821(11) . ?
V4 V3 3.0160(9) 12_666 ?
V5 O1 1.579(3) . ?
V5 O8 1.933(3) . ?
V5 O9 1.945(3) . ?
V5 O6 2.005(3) . ?
V5 O3 2.007(3) . ?
V6 O10 1.593(4) . ?
V6 O6 1.968(3) 6_454 ?
V6 O6 1.968(3) . ?
V6 O3 1.973(3) 6_454 ?
V6 O3 1.973(3) . ?
Ni1 N3 2.057(4) . ?
Ni1 N3 2.057(4) 6_444 ?
Ni1 N5 2.104(4) 6_444 ?
Ni1 N5 2.104(4) . ?
Ni1 N1 2.136(4) 6_444 ?
Ni1 N1 2.136(4) . ?
O11 V4 1.978(3) 15 ?
O9 V3 1.931(2) 12_666 ?
O7 As2 1.770(3) 6_454 ?
O5 V4 1.983(3) 12_666 ?
O5 V3 1.988(3) 12_666 ?
N3 C6 1.336(6) . ?
N3 C4 1.369(7) . ?
N1 C3 1.290(7) . ?
N1 C1 1.408(7) . ?
N5 C9 1.315(7) . ?
N5 C7 1.364(7) . ?
N2 C3 1.370(6) . ?
N2 C2 1.403(11) . ?
N4 C6 1.343(8) . ?
N4 C5 1.371(9) . ?
C6 C3 1.431(8) 6_444 ?
C9 N6 1.345(7) . ?
C9 C9 1.460(12) 6_444 ?
C3 C6 1.431(8) 6_444 ?
C7 C17 1.358(9) . ?
C4 C5 1.367(8) . ?
C1 C2 1.303(10) . ?
C17 N6 1.350(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 As1 O7 98.64(13) . . ?
O5 As1 O6 97.86(12) . . ?
O7 As1 O6 98.82(13) . . ?
O11 As2 O7 100.25(13) . 6_454 ?
O11 As2 O3 98.04(12) . . ?
O7 As2 O3 97.96(13) 6_454 . ?
O2 V3 O8 109.95(13) . . ?
O2 V3 O9 108.30(13) . 15 ?
O8 V3 O9 141.75(11) . 15 ?
O2 V3 O5 106.29(15) . 15 ?
O8 V3 O5 79.43(11) . 15 ?
O9 V3 O5 90.06(11) 15 15 ?
O2 V3 O11 107.58(15) . . ?
O8 V3 O11 89.36(11) . . ?
O9 V3 O11 79.16(11) 15 . ?
O5 V3 O11 146.13(11) 15 . ?
O2 V3 V4 111.05(11) . . ?
O8 V3 V4 38.76(8) . . ?
O9 V3 V4 123.46(8) 15 . ?
O5 V3 V4 40.85(7) 15 . ?
O11 V3 V4 123.09(8) . . ?
O2 V3 V4 111.65(11) . 15 ?
O8 V3 V4 122.05(8) . 15 ?
O9 V3 V4 38.80(8) 15 15 ?
O5 V3 V4 123.19(7) 15 15 ?
O11 V3 V4 40.43(7) . 15 ?
V4 V3 V4 137.29(3) . 15 ?
O4 V4 O8 110.13(13) . . ?
O4 V4 O9 109.80(13) . . ?
O8 V4 O9 83.66(11) . . ?
O4 V4 O11 109.45(13) . 12_666 ?
O8 V4 O11 140.23(11) . 12_666 ?
O9 V4 O11 79.69(11) . 12_666 ?
O4 V4 O5 109.39(13) . 15 ?
O8 V4 O5 79.56(11) . 15 ?
O9 V4 O5 140.62(11) . 15 ?
O11 V4 O5 90.95(11) 12_666 15 ?
O4 V4 V5 113.39(12) . . ?
O8 V4 V5 41.78(8) . . ?
O9 V4 V5 42.17(8) . . ?
O11 V4 V5 115.89(8) 12_666 . ?
O5 V4 V5 115.63(8) 15 . ?
O4 V4 V3 113.27(10) . . ?
O8 V4 V3 38.76(7) . . ?
O9 V4 V3 116.48(8) . . ?
O11 V4 V3 123.54(8) 12_666 . ?
O5 V4 V3 40.96(8) 15 . ?
V5 V4 V3 78.19(2) . . ?
O4 V4 V3 114.02(10) . 12_666 ?
O8 V4 V3 115.71(8) . 12_666 ?
O9 V4 V3 38.69(7) . 12_666 ?
O11 V4 V3 41.08(8) 12_666 12_666 ?
O5 V4 V3 123.16(8) 15 12_666 ?
V5 V4 V3 78.12(2) . 12_666 ?
V3 V4 V3 132.33(3) . 12_666 ?
O1 V5 O8 108.78(15) . . ?
O1 V5 O9 107.60(15) . . ?
O8 V5 O9 83.18(11) . . ?
O1 V5 O6 108.33(16) . . ?
O8 V5 O6 142.74(11) . . ?
O9 V5 O6 88.92(11) . . ?
O1 V5 O3 108.74(16) . . ?
O8 V5 O3 89.50(11) . . ?
O9 V5 O3 143.37(11) . . ?
O6 V5 O3 75.54(11) . . ?
O1 V5 V4 110.82(15) . . ?
O8 V5 V4 41.55(8) . . ?
O9 V5 V4 41.92(8) . . ?
O6 V5 V4 124.07(8) . . ?
O3 V5 V4 124.53(8) . . ?
O10 V6 O6 108.17(8) . 6_454 ?
O10 V6 O6 108.17(8) . . ?
O6 V6 O6 143.65(16) 6_454 . ?
O10 V6 O3 108.25(8) . 6_454 ?
O6 V6 O3 77.15(11) 6_454 6_454 ?
O6 V6 O3 91.55(11) . 6_454 ?
O10 V6 O3 108.25(8) . . ?
O6 V6 O3 91.55(11) 6_454 . ?
O6 V6 O3 77.15(11) . . ?
O3 V6 O3 143.50(16) 6_454 . ?
N3 Ni1 N3 98.2(2) . 6_444 ?
N3 Ni1 N5 170.62(17) . 6_444 ?
N3 Ni1 N5 90.91(17) 6_444 6_444 ?
N3 Ni1 N5 90.91(17) . . ?
N3 Ni1 N5 170.62(17) 6_444 . ?
N5 Ni1 N5 80.1(3) 6_444 . ?
N3 Ni1 N1 79.23(17) . 6_444 ?
N3 Ni1 N1 95.03(15) 6_444 6_444 ?
N5 Ni1 N1 97.81(18) 6_444 6_444 ?
N5 Ni1 N1 88.86(16) . 6_444 ?
N3 Ni1 N1 95.03(15) . . ?
N3 Ni1 N1 79.23(17) 6_444 . ?
N5 Ni1 N1 88.86(16) 6_444 . ?
N5 Ni1 N1 97.81(18) . . ?
N1 Ni1 N1 171.3(3) 6_444 . ?
As2 O11 V4 136.57(15) . 15 ?
As2 O11 V3 124.78(13) . . ?
V4 O11 V3 98.49(12) 15 . ?
V3 O9 V4 102.51(13) 12_666 . ?
V3 O9 V5 147.13(15) 12_666 . ?
V4 O9 V5 95.91(11) . . ?
V4 O8 V3 102.48(12) . . ?
V4 O8 V5 96.67(11) . . ?
V3 O8 V5 148.31(15) . . ?
As2 O7 As1 132.09(16) 6_454 . ?
As1 O6 V6 134.27(16) . . ?
As1 O6 V5 121.84(15) . . ?
V6 O6 V5 103.78(11) . . ?
As1 O5 V4 138.12(15) . 12_666 ?
As1 O5 V3 123.62(13) . 12_666 ?
V4 O5 V3 98.19(12) 12_666 12_666 ?
As2 O3 V6 135.03(16) . . ?
As2 O3 V5 121.32(15) . . ?
V6 O3 V5 103.53(11) . . ?
C6 N3 C4 107.6(4) . . ?
C6 N3 Ni1 111.8(4) . . ?
C4 N3 Ni1 140.0(3) . . ?
C3 N1 C1 106.1(5) . . ?
C3 N1 Ni1 111.0(4) . . ?
C1 N1 Ni1 141.9(5) . . ?
C9 N5 C7 106.8(5) . . ?
C9 N5 Ni1 111.6(4) . . ?
C7 N5 Ni1 141.0(4) . . ?
C3 N2 C2 105.8(6) . . ?
C6 N4 C5 108.8(5) . . ?
N3 C6 N4 109.0(6) . . ?
N3 C6 C3 118.4(5) . 6_444 ?
N4 C6 C3 132.6(5) . 6_444 ?
N5 C9 N6 110.1(6) . . ?
N5 C9 C9 118.2(3) . 6_444 ?
N6 C9 C9 131.6(4) . 6_444 ?
N1 C3 N2 111.1(6) . . ?
N1 C3 C6 118.1(4) . 6_444 ?
N2 C3 C6 130.8(6) . 6_444 ?
C17 C7 N5 108.5(7) . . ?
C5 C4 N3 108.5(6) . . ?
C2 C1 N1 110.0(8) . . ?
C1 C2 N2 107.0(7) . . ?
C4 C5 N4 106.1(6) . . ?
N6 C17 C7 106.8(6) . . ?
C9 N6 C17 107.7(6) . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.099
_database_code_depnum_ccdc_archive 'CCDC 973726'