# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

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

data_shelx_1
_database_code_depnum_ccdc_archive 'CCDC 1424795'
_audit_update_record             
;
2015-09-16 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_shelx_1             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow1 Check
RESPONSE: The hydrogens of the water molecule was not added.
;

_vrf_PLAT341_shelx_1             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0367 Ang
RESPONSE: The quality of this crystal was poor.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H46 As8 N18 Ni5 O43 V14'
_chemical_formula_weight         3169.10

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.861(3)
_cell_length_b                   14.142(3)
_cell_length_c                   22.798(5)
_cell_angle_alpha                90
_cell_angle_beta                 106.37(3)
_cell_angle_gamma                90
_cell_volume                     4597.1(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    995
_cell_measurement_theta_min      2.76
_cell_measurement_theta_max      25.06

_exptl_crystal_description       columnar
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.289
_exptl_crystal_F_000             3060
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    5.296
_shelx_estimated_absorpt_T_min   0.363
_shelx_estimated_absorpt_T_max   0.524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.423
_exptl_absorpt_correction_T_max  0.545
_exptl_absorpt_process_details   
'SADABS-2004/1 (Bruker,2004) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25225
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.715
_diffrn_reflns_theta_max         25.189
_diffrn_reflns_theta_full        25.189
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_reflns_number_total             8118
_reflns_number_gt                5601
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1041P)²+90.8226P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8118
_refine_ls_number_parameters     628
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0740
_refine_ls_wR_factor_ref         0.2334
_refine_ls_wR_factor_gt          0.1909
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.09562(9) 0.94697(9) 0.45809(5) 0.0372(3) Uani 1 1 d . . . . .
As2 As -0.04550(9) 1.10830(8) 0.38215(6) 0.0355(3) Uani 1 1 d . . . . .
As3 As 0.16464(10) 0.64565(8) 0.18026(6) 0.0422(3) Uani 1 1 d . . . . .
As4 As 0.30599(9) 0.80748(9) 0.25497(6) 0.0428(3) Uani 1 1 d . . . . .
V5 V 0.0000 1.15125(17) 0.2500 0.0294(6) Uani 1 2 d S T P . .
V6 V 0.0000 0.59992(17) 0.2500 0.0336(6) Uani 1 2 d S T P . .
V7 V 0.12446(14) 0.87604(13) 0.12867(9) 0.0335(4) Uani 1 1 d . . . . .
V8 V 0.24022(14) 0.87661(13) 0.37737(9) 0.0350(5) Uani 1 1 d . . . . .
V9 V 0.20700(14) 1.01857(14) 0.23623(9) 0.0345(5) Uani 1 1 d . . . . .
V10 V 0.16700(13) 1.07407(13) 0.34748(9) 0.0333(5) Uani 1 1 d . . . . .
V11 V 0.17810(15) 0.67864(13) 0.33477(9) 0.0371(5) Uani 1 1 d . . . . .
V12 V 0.04137(15) 0.73474(13) 0.39438(9) 0.0366(5) Uani 1 1 d . . . . .
OW1 O 0.0000 0.8805(7) 0.2500 0.031(2) Uani 1 2 d S T P . .
Ni1 Ni 0.3472(3) 0.5466(5) 0.4234(2) 0.0922(18) Uani 0.5 1 d . . P . .
Ni2 Ni 0.5000 1.0040(4) 0.2500 0.0652(15) Uani 0.5 2 d S T P . .
Ni3 Ni 0.5000 1.0000 0.5000 0.0574(14) Uani 0.5 2 d S . P . .
Ni4 Ni 0.0000 1.5000 0.5000 0.1029(15) Uani 1 2 d S . P . .
Ni5 Ni -0.52467(16) 1.41800(19) 0.31070(12) 0.0813(7) Uani 1 1 d . . . . .
O22 O 0.1276(5) 0.6402(5) 0.2470(3) 0.0353(18) Uani 1 1 d . . . . .
O21 O 0.1290(5) 1.1122(5) 0.2610(3) 0.0325(17) Uani 1 1 d . . . . .
O20 O 0.0355(5) 1.1116(5) 0.3376(4) 0.0349(17) Uani 1 1 d . . . . .
O19 O 0.0510(6) 0.6467(5) 0.3319(4) 0.0378(18) Uani 1 1 d . . . . .
O18 O 0.2223(6) 0.8849(6) 0.2093(4) 0.043(2) Uani 1 1 d . . . . .
O17 O 0.2385(6) 0.9782(6) 0.3201(4) 0.0400(19) Uani 1 1 d . . . . .
O16 O 0.1633(6) 0.7742(6) 0.3918(4) 0.042(2) Uani 1 1 d . . . . .
O15 O 0.0000 1.2637(8) 0.2500 0.044(3) Uani 1 2 d S T P . .
O14 O 0.2525(6) 0.7839(5) 0.3130(4) 0.0394(19) Uani 1 1 d . . . . .
O13 O 0.0261(6) 1.0513(6) 0.4480(4) 0.0410(19) Uani 1 1 d . . . . .
O12 O 0.1782(7) 0.8754(6) 0.0778(4) 0.049(2) Uani 1 1 d . . . . .
O11 O 0.1579(6) 0.9695(5) 0.4040(3) 0.0360(18) Uani 1 1 d . . . . .
O10 O 0.0107(6) 0.8668(6) 0.4137(4) 0.044(2) Uani 1 1 d . . . . .
O9 O -0.1146(6) 1.0105(6) 0.3472(4) 0.044(2) Uani 1 1 d . . . . .
O8 O 0.0000 0.4872(8) 0.2500 0.053(3) Uani 1 2 d S T P . .
O7 O 0.3378(6) 0.8785(7) 0.4287(4) 0.054(2) Uani 1 1 d . . . . .
O6 O 0.0977(6) 0.7426(6) 0.1434(4) 0.050(2) Uani 1 1 d . . . . .
O5 O 0.2363(6) 1.1533(6) 0.3857(4) 0.053(2) Uani 1 1 d . . . . .
O4 O 0.2751(6) 0.7022(7) 0.2115(5) 0.053(2) Uani 1 1 d . . . . .
O3 O 0.2485(7) 0.5960(6) 0.3686(4) 0.055(2) Uani 1 1 d . . . . .
O2 O 0.2949(6) 1.0746(6) 0.2282(5) 0.051(2) Uani 1 1 d . . . . .
O1 O 0.0532(8) 0.6734(7) 0.4551(4) 0.060(3) Uani 1 1 d . . . . .
N8 N -0.6477(9) 1.3774(8) 0.2744(6) 0.060(3) Uani 1 1 d . . . . .
N4 N 0.0611(10) 1.4211(9) 0.4586(6) 0.064(3) Uani 1 1 d . . . . .
N9 N -0.7724(10) 1.2851(9) 0.2548(6) 0.063(3) Uani 1 1 d . . . . .
N6 N -0.4032(10) 1.3613(11) 0.3599(7) 0.074(4) Uani 1 1 d . . . . .
N7 N -0.4582(9) 1.5393(10) 0.3444(7) 0.070(4) Uani 1 1 d . . . . .
C16 C -0.3396(13) 1.4246(15) 0.3922(8) 0.077(5) Uani 1 1 d . . . . .
C10 C 0.1150(19) 1.3665(19) 0.3865(10) 0.113(9) Uani 1 1 d . . . . .
H10A H 0.1302 1.3616 0.3497 0.136 Uiso 1 1 calc R U . . .
N5 N 0.1265(14) 1.3005(11) 0.4311(11) 0.104(6) Uani 1 1 d . . . . .
N3 N 0.5307(14) 0.9968(14) 0.4336(9) 0.110(6) Uani 1 1 d . U . . .
N102 N 0.5477(14) 0.3816(14) 0.5134(8) 0.089(5) Uani 0.5 1 d . . P . .
C2 C 0.5477(14) 0.3816(14) 0.5134(8) 0.089(5) Uani 0.5 1 d . . P . .
N1 N 0.4068(11) 0.4296(12) 0.4495(7) 0.074(4) Uani 0.5 1 d . . P . .
C101 C 0.4068(11) 0.4296(12) 0.4495(7) 0.074(4) Uani 0.5 1 d . . P . .
C23 C -0.8033(13) 1.3773(13) 0.2470(10) 0.079(5) Uani 1 1 d . . . . .
H23A H -0.8650 1.3984 0.2343 0.095 Uiso 1 1 calc R U . . .
C11 C 0.0944(13) 1.3354(11) 0.4740(9) 0.069(5) Uani 1 1 d . . . . .
H11A H 0.0949 1.3046 0.5101 0.083 Uiso 1 1 calc R U . . .
C24 C -0.7244(13) 1.4304(11) 0.2619(8) 0.074(5) Uani 1 1 d . . . . .
H24A H -0.7240 1.4961 0.2631 0.089 Uiso 1 1 calc R U . . .
C18 C -0.3245(15) 1.6014(17) 0.4185(9) 0.086(6) Uani 1 1 d . U . . .
H18A H -0.2672 1.5889 0.4470 0.104 Uiso 1 1 calc R U . . .
C22 C -0.6805(12) 1.2912(11) 0.2713(8) 0.069(5) Uani 1 1 d . . . . .
H22A H -0.6418 1.2383 0.2801 0.083 Uiso 1 1 calc R U . . .
C4 C 0.4418(15) 0.2704(14) 0.4541(10) 0.090(6) Uani 1 1 d . . . . .
H4A H 0.4260 0.2082 0.4423 0.109 Uiso 1 1 calc R U . . .
C5 C 0.3827(14) 0.3385(13) 0.4309(8) 0.078(5) Uani 1 1 d . . . . .
C8 C 0.4824(16) 1.0116(19) 0.3711(10) 0.101(7) Uani 1 1 d . U . . .
H8A H 0.4189 1.0264 0.3575 0.121 Uiso 1 1 calc R U . . .
C21 C -0.4922(16) 1.6268(16) 0.3373(13) 0.107(7) Uani 1 1 d . . . . .
H21A H -0.5516 1.6365 0.3107 0.128 Uiso 1 1 calc R U . . .
N2 N 0.5360(16) 1.0025(16) 0.3339(9) 0.110(6) Uani 1 1 d . . . . .
C17 C -0.3757(13) 1.5279(15) 0.3855(8) 0.077(5) Uani 1 1 d . . . . .
C1 C 0.4886(14) 0.4512(13) 0.4903(7) 0.072(5) Uani 1 1 d . . . . .
C19 C -0.3553(18) 1.6879(19) 0.4104(11) 0.104(7) Uani 1 1 d . U . . .
H19A H -0.3199 1.7373 0.4322 0.124 Uiso 1 1 calc R U . . .
C7 C 0.6233(18) 0.9799(19) 0.4290(12) 0.111(8) Uani 1 1 d . . . . .
H7A H 0.6755 0.9688 0.4620 0.133 Uiso 1 1 calc R U . . .
C20 C -0.4428(19) 1.7055(16) 0.3682(13) 0.112(8) Uani 1 1 d . . . . .
H20A H -0.4671 1.7664 0.3610 0.135 Uiso 1 1 calc R U . . .
C15 C -0.2574(19) 1.397(2) 0.4287(13) 0.144(12) Uani 1 1 d . . . . .
H15A H -0.2170 1.4389 0.4544 0.173 Uiso 1 1 calc R U . . .
C13 C -0.291(2) 1.236(2) 0.3985(14) 0.148(12) Uani 1 1 d . . . . .
H13A H -0.2767 1.1722 0.3998 0.177 Uiso 1 1 calc R U . . .
C6 C 0.624(2) 0.982(2) 0.3707(14) 0.125(9) Uani 1 1 d . . . . .
H6A H 0.6770 0.9716 0.3571 0.150 Uiso 1 1 calc R U . . .
C3 C 0.5260(18) 0.2894(17) 0.4950(10) 0.103(7) Uani 1 1 d . . . . .
C9 C 0.0779(19) 1.4384(14) 0.4068(11) 0.106(8) Uani 1 1 d . . . . .
H9A H 0.0649 1.4959 0.3864 0.128 Uiso 1 1 calc R U . . .
C14 C -0.233(3) 1.297(3) 0.4268(16) 0.190(19) Uani 1 1 d . . . . .
H14A H -0.1723 1.2784 0.4471 0.228 Uiso 1 1 calc R U . . .
C12 C -0.3799(16) 1.2722(17) 0.3647(11) 0.107(8) Uani 1 1 d . . . . .
H12A H -0.4249 1.2287 0.3443 0.129 Uiso 1 1 calc R U . . .


_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 O11 1.768(8) . ?
As1 O13 1.779(8) . ?
As1 O10 1.784(8) . ?
As2 O13 1.770(8) . ?
As2 O9 1.773(8) . ?
As2 O20 1.782(8) . ?
As3 O22 1.758(8) . ?
As3 O6 1.762(8) . ?
As3 O4 1.785(10) . ?
As4 O14 1.757(9) . ?
As4 O18 1.760(8) . ?
As4 O4 1.775(10) . ?
V5 O15 1.590(11) . ?
V5 O21 1.943(8) . ?
V5 O21 1.943(8) 2 ?
V5 O20 1.996(8) 2 ?
V5 O20 1.996(8) . ?
V5 V10 3.030(2) . ?
V5 V10 3.030(2) 2 ?
V6 O8 1.594(11) . ?
V6 O19 1.924(8) 2 ?
V6 O19 1.924(8) . ?
V6 O22 2.001(8) 2 ?
V6 O22 2.001(8) . ?
V6 V11 3.016(2) . ?
V6 V11 3.016(2) 2 ?
V7 O12 1.583(9) . ?
V7 O10 1.973(9) 2 ?
V7 O6 1.977(8) . ?
V7 O9 1.996(8) 2 ?
V7 O18 2.001(9) . ?
V7 V12 3.100(3) 2 ?
V8 O7 1.586(9) . ?
V8 O16 1.930(9) . ?
V8 O17 1.937(8) . ?
V8 O11 2.001(8) . ?
V8 O14 2.014(8) . ?
V8 V10 3.005(3) . ?
V8 V11 3.021(3) . ?
V9 O2 1.581(9) . ?
V9 O17 1.922(8) . ?
V9 O21 1.945(7) . ?
V9 O9 2.011(9) 2 ?
V9 O18 2.020(9) . ?
V9 V10 2.873(3) . ?
V10 O5 1.603(8) . ?
V10 O17 1.931(8) . ?
V10 O21 1.968(8) . ?
V10 O20 1.975(8) . ?
V10 O11 1.990(8) . ?
V11 O3 1.612(8) . ?
V11 O19 1.925(9) . ?
V11 O16 1.930(9) . ?
V11 O14 1.998(8) . ?
V11 O22 2.005(8) . ?
V11 V12 2.857(3) . ?
V12 O1 1.600(9) . ?
V12 O16 1.912(9) . ?
V12 O19 1.927(8) . ?
V12 O10 2.000(8) . ?
V12 O6 2.005(9) 2 ?
V12 V7 3.100(3) 2 ?
Ni1 O3 1.781(9) . ?
Ni1 N1 1.892(17) . ?
Ni1 C2 2.067(19) 3_666 ?
Ni1 N102 2.067(19) 3_666 ?
Ni2 N2 1.84(2) 2_655 ?
Ni2 N2 1.84(2) . ?
Ni3 N3 1.70(2) 3_676 ?
Ni3 N3 1.70(2) . ?
Ni4 N4 1.856(12) 3_586 ?
Ni4 N4 1.856(12) . ?
Ni5 N8 1.872(13) . ?
Ni5 N6 2.005(15) . ?
Ni5 N7 2.020(14) . ?
O10 V7 1.973(9) 2 ?
O9 V7 1.996(8) 2 ?
O9 V9 2.011(9) 2 ?
O6 V12 2.005(9) 2 ?
N8 C22 1.308(18) . ?
N8 C24 1.33(2) . ?
N4 C9 1.30(2) . ?
N4 C11 1.32(2) . ?
N9 C22 1.31(2) . ?
N9 C23 1.38(2) . ?
N6 C12 1.30(3) . ?
N6 C16 1.36(2) . ?
N7 C17 1.33(2) . ?
N7 C21 1.33(3) . ?
C16 C15 1.33(3) . ?
C16 C17 1.55(3) . ?
C10 C9 1.30(3) . ?
C10 N5 1.35(3) . ?
N5 C11 1.30(2) . ?
N3 C8 1.42(3) . ?
N3 C7 1.43(3) . ?
N102 C1 1.33(3) . ?
N102 C3 1.38(3) . ?
N102 Ni1 2.067(19) 3_666 ?
N1 C1 1.34(2) . ?
N1 C5 1.37(2) . ?
C23 C24 1.35(2) . ?
C18 C19 1.30(3) . ?
C18 C17 1.38(3) . ?
C4 C5 1.31(3) . ?
C4 C3 1.36(3) . ?
C8 N2 1.32(3) . ?
C21 C20 1.41(3) . ?
N2 C6 1.38(3) . ?
C1 C1 1.46(4) 3_666 ?
C19 C20 1.40(3) . ?
C7 C6 1.33(3) . ?
C15 C14 1.45(4) . ?
C13 C14 1.26(4) . ?
C13 C12 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
O11 As1 O13 99.2(4) . . ?
O11 As1 O10 98.3(4) . . ?
O13 As1 O10 99.3(4) . . ?
O13 As2 O9 99.2(4) . . ?
O13 As2 O20 98.8(4) . . ?
O9 As2 O20 99.3(4) . . ?
O22 As3 O6 100.0(4) . . ?
O22 As3 O4 98.7(4) . . ?
O6 As3 O4 100.0(4) . . ?
O14 As4 O18 99.8(4) . . ?
O14 As4 O4 99.2(4) . . ?
O18 As4 O4 99.4(4) . . ?
O15 V5 O21 106.5(2) . . ?
O15 V5 O21 106.5(2) . 2 ?
O21 V5 O21 146.9(5) . 2 ?
O15 V5 O20 106.3(2) . 2 ?
O21 V5 O20 91.3(3) . 2 ?
O21 V5 O20 79.5(3) 2 2 ?
O15 V5 O20 106.3(2) . . ?
O21 V5 O20 79.5(3) . . ?
O21 V5 O20 91.3(3) 2 . ?
O20 V5 O20 147.4(5) 2 . ?
O15 V5 V10 111.11(6) . . ?
O21 V5 V10 39.5(2) . . ?
O21 V5 V10 124.5(2) 2 . ?
O20 V5 V10 124.3(2) 2 . ?
O20 V5 V10 40.0(2) . . ?
O15 V5 V10 111.11(6) . 2 ?
O21 V5 V10 124.5(2) . 2 ?
O21 V5 V10 39.5(2) 2 2 ?
O20 V5 V10 40.0(2) 2 2 ?
O20 V5 V10 124.3(2) . 2 ?
V10 V5 V10 137.78(11) . 2 ?
O8 V6 O19 110.1(2) . 2 ?
O8 V6 O19 110.1(2) . . ?
O19 V6 O19 139.8(5) 2 . ?
O8 V6 O22 106.5(2) . 2 ?
O19 V6 O22 79.5(3) 2 2 ?
O19 V6 O22 89.2(3) . 2 ?
O8 V6 O22 106.5(2) . . ?
O19 V6 O22 89.2(3) 2 . ?
O19 V6 O22 79.5(3) . . ?
O22 V6 O22 146.9(4) 2 . ?
O8 V6 V11 111.66(6) . . ?
O19 V6 V11 122.0(3) 2 . ?
O19 V6 V11 38.4(3) . . ?
O22 V6 V11 122.8(2) 2 . ?
O22 V6 V11 41.2(2) . . ?
O8 V6 V11 111.66(6) . 2 ?
O19 V6 V11 38.4(3) 2 2 ?
O19 V6 V11 122.0(3) . 2 ?
O22 V6 V11 41.2(2) 2 2 ?
O22 V6 V11 122.8(2) . 2 ?
V11 V6 V11 136.68(11) . 2 ?
O12 V7 O10 107.2(5) . 2 ?
O12 V7 O6 106.7(5) . . ?
O10 V7 O6 78.1(4) 2 . ?
O12 V7 O9 107.4(4) . 2 ?
O10 V7 O9 93.1(4) 2 2 ?
O6 V7 O9 145.9(4) . 2 ?
O12 V7 O18 106.7(4) . . ?
O10 V7 O18 146.1(4) 2 . ?
O6 V7 O18 91.8(4) . . ?
O9 V7 O18 77.2(3) 2 . ?
O12 V7 V12 114.4(3) . 2 ?
O10 V7 V12 39.0(2) 2 2 ?
O6 V7 V12 39.2(3) . 2 ?
O9 V7 V12 122.9(3) 2 2 ?
O18 V7 V12 122.2(3) . 2 ?
O7 V8 O16 110.5(4) . . ?
O7 V8 O17 108.7(4) . . ?
O16 V8 O17 140.8(4) . . ?
O7 V8 O11 106.0(5) . . ?
O16 V8 O11 89.9(4) . . ?
O17 V8 O11 79.9(3) . . ?
O7 V8 O14 107.2(5) . . ?
O16 V8 O14 79.4(4) . . ?
O17 V8 O14 88.8(3) . . ?
O11 V8 O14 146.8(3) . . ?
O7 V8 V10 110.4(4) . . ?
O16 V8 V10 122.8(3) . . ?
O17 V8 V10 39.0(2) . . ?
O11 V8 V10 41.0(2) . . ?
O14 V8 V10 122.8(2) . . ?
O7 V8 V11 112.7(4) . . ?
O16 V8 V11 38.5(3) . . ?
O17 V8 V11 121.7(3) . . ?
O11 V8 V11 123.2(3) . . ?
O14 V8 V11 41.0(2) . . ?
V10 V8 V11 136.89(9) . . ?
O2 V9 O17 106.6(5) . . ?
O2 V9 O21 105.8(4) . . ?
O17 V9 O21 84.9(3) . . ?
O2 V9 O9 106.6(5) . 2 ?
O17 V9 O9 146.4(4) . 2 ?
O21 V9 O9 90.5(3) . 2 ?
O2 V9 O18 105.4(4) . . ?
O17 V9 O18 90.4(3) . . ?
O21 V9 O18 148.5(4) . . ?
O9 V9 O18 76.4(3) 2 . ?
O2 V9 V10 110.4(4) . . ?
O17 V9 V10 41.9(2) . . ?
O21 V9 V10 43.1(2) . . ?
O9 V9 V10 126.5(3) 2 . ?
O18 V9 V10 126.4(3) . . ?
O5 V10 O17 109.8(4) . . ?
O5 V10 O21 108.2(4) . . ?
O17 V10 O21 84.1(3) . . ?
O5 V10 O20 109.7(4) . . ?
O17 V10 O20 140.2(4) . . ?
O21 V10 O20 79.4(3) . . ?
O5 V10 O11 108.6(4) . . ?
O17 V10 O11 80.3(3) . . ?
O21 V10 O11 143.1(3) . . ?
O20 V10 O11 91.6(3) . . ?
O5 V10 V9 114.2(4) . . ?
O17 V10 V9 41.7(2) . . ?
O21 V10 V9 42.4(2) . . ?
O20 V10 V9 114.6(2) . . ?
O11 V10 V9 115.9(2) . . ?
O5 V10 V8 113.0(3) . . ?
O17 V10 V8 39.1(2) . . ?
O21 V10 V8 117.7(2) . . ?
O20 V10 V8 124.0(2) . . ?
O11 V10 V8 41.3(2) . . ?
V9 V10 V8 78.14(7) . . ?
O5 V10 V5 114.5(4) . . ?
O17 V10 V5 115.3(3) . . ?
O21 V10 V5 38.9(2) . . ?
O20 V10 V5 40.5(2) . . ?
O11 V10 V5 123.5(3) . . ?
V9 V10 V5 77.37(7) . . ?
V8 V10 V5 132.11(9) . . ?
O3 V11 O19 110.2(5) . . ?
O3 V11 O16 111.6(4) . . ?
O19 V11 O16 83.7(4) . . ?
O3 V11 O14 109.2(4) . . ?
O19 V11 O14 140.6(3) . . ?
O16 V11 O14 79.7(4) . . ?
O3 V11 O22 106.9(4) . . ?
O19 V11 O22 79.4(3) . . ?
O16 V11 O22 141.3(3) . . ?
O14 V11 O22 91.8(3) . . ?
O3 V11 V12 115.3(4) . . ?
O19 V11 V12 42.1(2) . . ?
O16 V11 V12 41.7(3) . . ?
O14 V11 V12 115.4(2) . . ?
O22 V11 V12 115.7(2) . . ?
O3 V11 V6 111.9(4) . . ?
O19 V11 V6 38.4(2) . . ?
O16 V11 V6 116.3(3) . . ?
O14 V11 V6 124.3(3) . . ?
O22 V11 V6 41.1(2) . . ?
V12 V11 V6 78.11(7) . . ?
O3 V11 V8 114.8(4) . . ?
O19 V11 V8 115.9(2) . . ?
O16 V11 V8 38.5(3) . . ?
O14 V11 V8 41.4(2) . . ?
O22 V11 V8 124.5(2) . . ?
V12 V11 V8 77.51(7) . . ?
V6 V11 V8 132.96(8) . . ?
O1 V12 O16 108.1(5) . . ?
O1 V12 O19 106.0(5) . . ?
O16 V12 O19 84.1(4) . . ?
O1 V12 O10 106.9(5) . . ?
O16 V12 O10 90.6(4) . . ?
O19 V12 O10 146.6(4) . . ?
O1 V12 O6 104.5(5) . 2 ?
O16 V12 O6 147.2(4) . 2 ?
O19 V12 O6 90.0(4) . 2 ?
O10 V12 O6 76.8(3) . 2 ?
O1 V12 V11 110.0(4) . . ?
O16 V12 V11 42.2(3) . . ?
O19 V12 V11 42.1(3) . . ?
O10 V12 V11 126.9(3) . . ?
O6 V12 V11 126.6(3) 2 . ?
O1 V12 V7 112.6(4) . 2 ?
O16 V12 V7 121.4(3) . 2 ?
O19 V12 V7 120.8(3) . 2 ?
O10 V12 V7 38.4(3) . 2 ?
O6 V12 V7 38.5(2) 2 2 ?
V11 V12 V7 137.42(9) . 2 ?
O3 Ni1 N1 141.6(7) . . ?
O3 Ni1 C2 127.4(7) . 3_666 ?
N1 Ni1 C2 90.9(8) . 3_666 ?
O3 Ni1 N102 127.4(7) . 3_666 ?
N1 Ni1 N102 90.9(8) . 3_666 ?
C2 Ni1 N102 0.0 3_666 3_666 ?
N2 Ni2 N2 178.6(14) 2_655 . ?
N3 Ni3 N3 180.0 3_676 . ?
N4 Ni4 N4 180.0(9) 3_586 . ?
N8 Ni5 N6 137.6(6) . . ?
N8 Ni5 N7 137.7(6) . . ?
N6 Ni5 N7 82.0(6) . . ?
As3 O22 V6 125.0(4) . . ?
As3 O22 V11 137.0(4) . . ?
V6 O22 V11 97.7(4) . . ?
V5 O21 V9 143.5(4) . . ?
V5 O21 V10 101.6(3) . . ?
V9 O21 V10 94.5(3) . . ?
As2 O20 V10 137.2(4) . . ?
As2 O20 V5 123.2(4) . . ?
V10 O20 V5 99.4(4) . . ?
V6 O19 V11 103.2(4) . . ?
V6 O19 V12 148.0(5) . . ?
V11 O19 V12 95.7(4) . . ?
As4 O18 V7 135.6(5) . . ?
As4 O18 V9 121.6(4) . . ?
V7 O18 V9 102.9(4) . . ?
V9 O17 V10 96.4(4) . . ?
V9 O17 V8 147.6(5) . . ?
V10 O17 V8 101.9(4) . . ?
V12 O16 V8 146.7(5) . . ?
V12 O16 V11 96.0(4) . . ?
V8 O16 V11 103.0(4) . . ?
As4 O14 V11 136.7(5) . . ?
As4 O14 V8 125.3(4) . . ?
V11 O14 V8 97.7(4) . . ?
As2 O13 As1 132.5(5) . . ?
As1 O11 V10 136.9(4) . . ?
As1 O11 V8 125.3(4) . . ?
V10 O11 V8 97.7(3) . . ?
As1 O10 V7 134.1(5) . 2 ?
As1 O10 V12 123.4(5) . . ?
V7 O10 V12 102.6(4) 2 . ?
As2 O9 V7 134.2(5) . 2 ?
As2 O9 V9 122.4(4) . 2 ?
V7 O9 V9 103.4(4) 2 2 ?
As3 O6 V7 135.3(5) . . ?
As3 O6 V12 122.5(5) . 2 ?
V7 O6 V12 102.3(4) . 2 ?
As4 O4 As3 131.5(5) . . ?
V11 O3 Ni1 156.2(7) . . ?
C22 N8 C24 103.4(13) . . ?
C22 N8 Ni5 127.7(12) . . ?
C24 N8 Ni5 126.5(11) . . ?
C9 N4 C11 105.1(15) . . ?
C9 N4 Ni4 126.6(13) . . ?
C11 N4 Ni4 128.2(12) . . ?
C22 N9 C23 104.9(13) . . ?
C12 N6 C16 117.7(17) . . ?
C12 N6 Ni5 127.6(14) . . ?
C16 N6 Ni5 114.8(13) . . ?
C17 N7 C21 116.3(18) . . ?
C17 N7 Ni5 114.9(13) . . ?
C21 N7 Ni5 128.1(14) . . ?
C15 C16 N6 121(2) . . ?
C15 C16 C17 125(2) . . ?
N6 C16 C17 113.6(16) . . ?
C9 C10 N5 104.3(17) . . ?
C11 N5 C10 107.9(16) . . ?
C8 N3 C7 100(2) . . ?
C8 N3 Ni3 134.7(17) . . ?
C7 N3 Ni3 125.2(17) . . ?
C1 N102 C3 120.6(18) . . ?
C1 N102 Ni1 101.4(14) . 3_666 ?
C3 N102 Ni1 137.9(16) . 3_666 ?
C1 N1 C5 122.3(17) . . ?
C1 N1 Ni1 105.7(13) . . ?
C5 N1 Ni1 131.8(13) . . ?
C24 C23 N9 105.0(15) . . ?
N5 C11 N4 109.8(17) . . ?
N8 C24 C23 111.8(15) . . ?
C19 C18 C17 121(2) . . ?
N8 C22 N9 114.7(15) . . ?
C5 C4 C3 121(2) . . ?
C4 C5 N1 118.6(18) . . ?
N2 C8 N3 114(2) . . ?
N7 C21 C20 123(2) . . ?
C8 N2 C6 106(2) . . ?
C8 N2 Ni2 128.0(18) . . ?
C6 N2 Ni2 126(2) . . ?
N7 C17 C18 123(2) . . ?
N7 C17 C16 114.2(16) . . ?
C18 C17 C16 122.3(19) . . ?
N102 C1 N1 118.4(17) . . ?
N102 C1 C1 121(2) . 3_666 ?
N1 C1 C1 121(2) . 3_666 ?
C18 C19 C20 119(2) . . ?
C6 C7 N3 111(2) . . ?
C19 C20 C21 117(2) . . ?
C16 C15 C14 118(2) . . ?
C14 C13 C12 115(3) . . ?
C7 C6 N2 110(3) . . ?
C4 C3 N102 119(2) . . ?
N4 C9 C10 112.7(19) . . ?
C13 C14 C15 122(3) . . ?
N6 C12 C13 125(2) . . ?

_refine_diff_density_max         2.050
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.209

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

data_shelx_1a
_database_code_depnum_ccdc_archive 'CCDC 1424796'
_audit_update_record             
;
2015-09-16 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT094_shelx_1a            
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.35 Report
RESPONSE: residual electron density which could not be assigned and should be
due to the disorder of Ni(3).
;

_vrf_PLAT306_shelx_1a            
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... Ow1 Check
RESPONSE: The hydrogens of the water molecule was not added.
;

_vrf_PLAT341_shelx_1a            
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0175 Ang
RESPONSE: The quality of this crystal was poor.
;

_vrf_PLAT430_shelx_1a            
;
PROBLEM: Short Inter D...A Contact O1 .. N14 .. 2.82 Ang.
RESPONSE: There should be a strong hydrogen bond between the
two atoms.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H41 As8 N12 Ni2.50 O43 V14'
_chemical_formula_weight         2909.20

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'
As As 0.0499 2.0058 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   13.80109(15)
_cell_length_b                   23.8678(2)
_cell_length_c                   27.1204(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8933.50(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13245
_cell_measurement_theta_min      3.3410
_cell_measurement_theta_max      28.3080

_exptl_crystal_description       needle-like
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_F_000             5604
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    4.933
_shelx_estimated_absorpt_T_min   0.372
_shelx_estimated_absorpt_T_max   0.525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29903
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.955
_diffrn_reflns_theta_max         29.073
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.865
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_point_group_measured_fraction_full 0.963
_reflns_number_total             19099
_reflns_number_gt                17390
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.708
_reflns_Friedel_fraction_max     0.720
_reflns_Friedel_fraction_full    0.928

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0767P)²+14.8542P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_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 x determined using 6734 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         19099
_refine_ls_number_parameters     1162
_refine_ls_number_restraints     828
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1323
_refine_ls_wR_factor_gt          0.1273
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As8 As 0.02191(8) 0.71151(4) 0.36898(3) 0.0357(2) Uani 1 1 d . . . . .
As7 As 0.02597(7) 0.71492(4) 0.24912(3) 0.0345(2) Uani 1 1 d . . . . .
As6 As 0.34014(7) 0.87881(4) 0.37474(3) 0.0349(2) Uani 1 1 d . . . . .
As5 As 0.34792(7) 0.88312(4) 0.25635(3) 0.0359(2) Uani 1 1 d . . . . .
As4 As -0.03343(8) 1.03399(4) 0.42796(3) 0.0402(2) Uani 1 1 d . . . . .
As3 As -0.20747(8) 0.94322(4) 0.42325(4) 0.0409(2) Uani 1 1 d . . . . .
As2 As -0.02256(9) 1.04065(4) 0.20635(3) 0.0413(2) Uani 1 1 d . . . . .
As1 As -0.19800(8) 0.94993(4) 0.20244(4) 0.0414(2) Uani 1 1 d . . . . .
Ni2 Ni 1.01565(9) 0.70830(5) 0.91966(4) 0.0359(2) Uani 1 1 d . . . . .
Ni1 Ni 0.44696(10) 0.87049(5) 0.43961(5) 0.0422(3) Uani 1 1 d . . . . .
V14 V 0.15802(11) 0.82007(6) 0.20651(5) 0.0303(3) Uani 1 1 d . . . . .
V13 V -0.11246(12) 0.81979(7) 0.20832(5) 0.0328(3) Uani 1 1 d . . . . .
V12 V 0.21491(11) 0.77672(6) 0.31223(6) 0.0315(3) Uani 1 1 d . . . . .
V11 V 0.14912(12) 0.81437(6) 0.41865(5) 0.0330(3) Uani 1 1 d . . . . .
V10 V 0.01959(13) 0.89599(6) 0.46169(5) 0.0350(3) Uani 1 1 d . . . . .
V9 V -0.11837(12) 0.81388(7) 0.41269(5) 0.0338(3) Uani 1 1 d . . . . .
V8 V -0.17030(11) 0.77823(6) 0.30898(6) 0.0340(3) Uani 1 1 d . . . . .
V7 V 0.07118(12) 1.05289(6) 0.31883(6) 0.0362(3) Uani 1 1 d . . . . .
V6 V 0.17945(12) 0.96893(6) 0.42112(5) 0.0345(3) Uani 1 1 d . . . . .
V5 V 0.25564(12) 1.00081(7) 0.32040(6) 0.0367(3) Uani 1 1 d . . . . .
V4 V 0.03311(12) 0.90355(6) 0.16703(5) 0.0334(3) Uani 1 1 d . . . . .
V3 V -0.14472(12) 1.01199(6) 0.31502(6) 0.0371(3) Uani 1 1 d . . . . .
V2 V -0.23725(11) 0.89300(7) 0.31147(6) 0.0362(3) Uani 1 1 d . . . . .
V1 V 0.18884(13) 0.97451(6) 0.21651(5) 0.0349(3) Uani 1 1 d . . . . .
Ni3 Ni 0.3347(3) 0.59793(19) 0.35382(16) 0.0870(10) Uani 0.5 1 d . U P . .
N11 N 0.2607(8) 0.6150(6) 0.4060(4) 0.053(4) Uani 0.5 1 d G U P . .
C51 C 0.2873(7) 0.6587(5) 0.4387(5) 0.047(4) Uani 0.5 1 d G U P . .
C52 C 0.2151(8) 0.6625(4) 0.4759(4) 0.020(2) Uani 0.5 1 d G U P . .
N12 N 0.1438(7) 0.6211(5) 0.4661(4) 0.037(3) Uani 0.5 1 d G U P . .
C53 C 0.1720(8) 0.5917(4) 0.4228(4) 0.027(3) Uani 0.5 1 d G U P . .
O42 O 0.1198(5) 0.7644(3) 0.2584(2) 0.0350(14) Uani 1 1 d . . . . .
O41 O 0.2555(5) 0.8322(3) 0.2613(2) 0.0347(13) Uani 1 1 d . . . . .
O40 O 0.1607(5) 0.8996(2) 0.1942(2) 0.0343(13) Uani 1 1 d . . . . .
O39 O 0.2782(5) 0.9431(3) 0.2670(2) 0.0387(15) Uani 1 1 d . . . . .
O38 O -0.0772(5) 0.7575(3) 0.3620(2) 0.0362(14) Uani 1 1 d . . . . .
O37 O 0.0136(5) 0.8205(2) 0.4353(2) 0.0360(13) Uani 1 1 d . . . . .
O36 O 0.0218(4) 0.8272(2) 0.1894(2) 0.0328(12) Uani 1 1 d . . . . .
O35 O -0.0731(5) 0.7608(3) 0.2572(2) 0.0368(14) Uani 1 1 d . . . . .
O34 O -0.1970(5) 0.8356(3) 0.3569(2) 0.0374(14) Uani 1 1 d . . . . .
O33 O -0.0364(5) 1.0334(3) 0.2712(2) 0.0426(15) Uani 1 1 d . . . . .
O32 O 0.0255(5) 0.6828(2) 0.3085(2) 0.0394(14) Uani 1 1 d . . . . .
O31 O -0.1059(5) 0.9019(3) 0.1901(2) 0.0396(14) Uani 1 1 d . . . . .
O30 O -0.1965(5) 0.8382(3) 0.2632(2) 0.0370(14) Uani 1 1 d . . . . .
O29 O 0.1502(5) 0.8924(3) 0.4366(2) 0.0406(15) Uani 1 1 d . . . . .
O28 O 0.1561(5) 1.0212(3) 0.3676(2) 0.0392(14) Uani 1 1 d . . . . .
O27 O 0.1614(5) 1.0228(3) 0.2714(2) 0.0391(15) Uani 1 1 d . . . . .
O26 O -0.1885(5) 0.9516(3) 0.3587(2) 0.0417(15) Uani 1 1 d . . . . .
O25 O 0.3978(4) 0.8756(3) 0.3168(3) 0.0399(14) Uani 1 1 d . . . . .
O24 O 0.1158(5) 0.7621(3) 0.3626(2) 0.0374(14) Uani 1 1 d . . . . .
O23 O 0.0492(5) 0.9812(3) 0.1941(2) 0.0381(14) Uani 1 1 d . . . . .
O22 O 0.0380(5) 0.9738(3) 0.4383(2) 0.0392(14) Uani 1 1 d . . . . .
O21 O -0.1868(5) 0.9536(3) 0.2673(2) 0.0412(15) Uani 1 1 d . . . . .
O20 O -0.1368(6) 1.0135(3) 0.1865(3) 0.0485(17) Uani 1 1 d . . . . .
O19 O 0.0364(6) 0.9062(3) 0.1079(2) 0.0445(16) Uani 1 1 d . . . . .
O18 O 0.2757(5) 0.9418(3) 0.3708(2) 0.0398(15) Uani 1 1 d . . . . .
O17 O -0.2562(5) 0.7324(3) 0.3079(3) 0.0458(16) Uani 1 1 d . . . . .
O16 O 0.2446(5) 0.8312(3) 0.3648(2) 0.0369(14) Uani 1 1 d . . . . .
O15 O -0.1141(5) 0.8942(3) 0.4352(2) 0.0395(15) Uani 1 1 d . . . . .
O14 O 0.0175(7) 0.8965(3) 0.5209(2) 0.0514(19) Uani 1 1 d . . . . .
O13 O -0.1824(6) 0.7800(3) 0.4522(3) 0.0485(17) Uani 1 1 d . . . . .
O12 O 0.2897(5) 0.7268(3) 0.3137(3) 0.0496(17) Uani 1 1 d . . . . .
O11 O -0.0412(5) 1.0317(3) 0.3622(2) 0.0410(15) Uani 1 1 d . . . . .
O10 O -0.1720(5) 0.7888(3) 0.1654(3) 0.0475(17) Uani 1 1 d . . . . .
O9 O -0.3534(5) 0.8966(3) 0.3118(3) 0.0532(18) Uani 1 1 d . . . . .
O8 O 0.2048(6) 0.7801(3) 0.4601(3) 0.0493(18) Uani 1 1 d . . . . .
O7 O 0.2379(6) 0.9980(3) 0.4645(3) 0.0482(18) Uani 1 1 d . . . . .
O5 O 0.2111(6) 0.7881(3) 0.1620(2) 0.0452(16) Uani 1 1 d . . . . .
N3 N 0.5236(7) 0.8030(4) 0.4313(3) 0.0447(19) Uani 1 1 d . . . . .
N10 N 1.0141(6) 0.7202(4) 0.8445(3) 0.0405(18) Uani 1 1 d . . . . .
O6 O 0.0846(6) 1.1192(3) 0.3194(3) 0.0514(18) Uani 1 1 d . . . . .
O4 O -0.2219(6) 1.0608(3) 0.3157(3) 0.058(2) Uani 1 1 d . . . . .
O3 O 0.2557(6) 1.0067(3) 0.1777(3) 0.0507(18) Uani 1 1 d . . . . .
O2 O -0.1495(6) 1.0053(3) 0.4433(3) 0.0467(17) Uani 1 1 d . . . . .
N8 N 0.9433(6) 0.6315(3) 0.9162(3) 0.0407(18) Uani 1 1 d . . . . .
N2 N 0.3918(6) 0.8903(4) 0.5069(3) 0.0408(18) Uani 1 1 d . . . . .
O1 O 0.3424(6) 1.0443(3) 0.3240(3) 0.057(2) Uani 1 1 d . . . . .
N9 N 0.8939(6) 0.7604(3) 0.9118(3) 0.0396(18) Uani 1 1 d . . . . .
N7 N 1.1300(6) 0.6504(4) 0.9237(3) 0.0429(19) Uani 1 1 d . . . . .
N6 N 1.0085(7) 0.7131(3) 0.9967(3) 0.0395(18) Uani 1 1 d . . . . .
N5 N 1.1009(7) 0.7780(4) 0.9336(4) 0.052(2) Uani 1 1 d . . . . .
C31 C 1.2266(8) 0.6624(6) 0.9227(4) 0.055(2) Uani 1 1 d . U . . .
H31A H 1.2457 0.6993 0.9174 0.066 Uiso 1 1 calc R U . . .
C11 C 0.5155(12) 0.7535(5) 0.4561(5) 0.068(3) Uani 1 1 d . U . . .
H11A H 0.4802 0.7488 0.4850 0.081 Uiso 1 1 calc R U . . .
C46 C 0.9459(8) 0.7564(4) 0.8282(3) 0.0421(17) Uani 1 1 d . U . . .
C49 C 1.0667(9) 0.7089(5) 0.7614(4) 0.054(2) Uani 1 1 d . U . . .
H49A H 1.1113 0.6937 0.7394 0.064 Uiso 1 1 calc R U . . .
C45 C 0.8819(7) 0.7821(4) 0.8662(3) 0.0396(17) Uani 1 1 d . U . . .
C48 C 0.9956(9) 0.7426(5) 0.7445(4) 0.050(2) Uani 1 1 d . U . . .
H48A H 0.9870 0.7483 0.7109 0.060 Uiso 1 1 calc R U . . .
C47 C 0.9362(8) 0.7682(5) 0.7784(4) 0.0468(19) Uani 1 1 d . U . . .
H47A H 0.8894 0.7936 0.7679 0.056 Uiso 1 1 calc R U . . .
C13 C 0.5769(10) 0.7903(6) 0.3921(5) 0.061(3) Uani 1 1 d . U . . .
H13A H 0.5921 0.8155 0.3671 0.073 Uiso 1 1 calc R U . . .
C40 C 0.8481(9) 0.6251(5) 0.9078(4) 0.051(2) Uani 1 1 d . U . . .
H40A H 0.8119 0.6562 0.8985 0.061 Uiso 1 1 calc R U . . .
C10 C 0.3422(9) 0.8555(5) 0.5357(4) 0.050(2) Uani 1 1 d . U . . .
H10A H 0.3208 0.8215 0.5229 0.060 Uiso 1 1 calc R U . . .
C36 C 0.9983(8) 0.5875(5) 0.9261(4) 0.0479(18) Uani 1 1 d . U . . .
N1 N 0.4976(6) 0.9517(4) 0.4452(3) 0.046(2) Uani 1 1 d . . . . .
C6 C 0.4188(8) 0.9400(5) 0.5229(4) 0.0467(18) Uani 1 1 d . U . . .
C8 C 0.3498(9) 0.9183(5) 0.6022(5) 0.059(2) Uani 1 1 d . U . . .
H8A H 0.3361 0.9277 0.6347 0.070 Uiso 1 1 calc R U . . .
C35 C 1.1038(8) 0.5984(5) 0.9300(4) 0.0509(19) Uani 1 1 d . U . . .
C7 C 0.3999(9) 0.9559(5) 0.5719(4) 0.056(2) Uani 1 1 d . U . . .
H7A H 0.4200 0.9905 0.5839 0.067 Uiso 1 1 calc R U . . .
C37 C 0.9552(10) 0.5334(5) 0.9327(5) 0.059(2) Uani 1 1 d . U . . .
H37A H 0.9927 0.5025 0.9411 0.071 Uiso 1 1 calc R U . . .
C5 C 0.4731(9) 0.9758(5) 0.4874(4) 0.0487(19) Uani 1 1 d . U . . .
C32 C 1.2966(10) 0.6225(6) 0.9292(4) 0.062(2) Uani 1 1 d . U . . .
H32A H 1.3618 0.6323 0.9287 0.074 Uiso 1 1 calc R U . . .
C39 C 0.8022(10) 0.5744(5) 0.9125(4) 0.057(2) Uani 1 1 d . U . . .
H39A H 0.7361 0.5707 0.9068 0.068 Uiso 1 1 calc R U . . .
C50 C 1.0741(8) 0.6965(5) 0.8121(4) 0.0512(19) Uani 1 1 d . U . . .
H50A H 1.1211 0.6715 0.8231 0.061 Uiso 1 1 calc R U . . .
C44 C 0.8151(8) 0.8219(5) 0.8563(4) 0.0473(19) Uani 1 1 d . U . . .
H44A H 0.8098 0.8365 0.8246 0.057 Uiso 1 1 calc R U . . .
C26 C 1.0545(9) 0.7562(5) 1.0166(4) 0.0542(19) Uani 1 1 d . U . . .
C43 C 0.7548(9) 0.8410(5) 0.8933(4) 0.050(2) Uani 1 1 d . U . . .
H43A H 0.7080 0.8681 0.8869 0.060 Uiso 1 1 calc R U . . .
C42 C 0.7653(8) 0.8190(5) 0.9394(4) 0.050(2) Uani 1 1 d . U . . .
H42A H 0.7265 0.8314 0.9652 0.060 Uiso 1 1 calc R U . . .
N4 N 0.6059(10) 0.7371(6) 0.3926(5) 0.088(4) Uani 1 1 d . . . . .
C41 C 0.8337(8) 0.7787(5) 0.9471(4) 0.0482(19) Uani 1 1 d . U . . .
H41A H 0.8388 0.7631 0.9784 0.058 Uiso 1 1 calc R U . . .
C38 C 0.8595(10) 0.5287(6) 0.9263(5) 0.062(2) Uani 1 1 d . U . . .
H38A H 0.8302 0.4940 0.9312 0.074 Uiso 1 1 calc R U . . .
C2 C 0.5681(10) 1.0369(6) 0.4160(6) 0.067(3) Uani 1 1 d . U . . .
H2A H 0.6013 1.0565 0.3917 0.081 Uiso 1 1 calc R U . . .
C25 C 1.1048(9) 0.7945(5) 0.9807(5) 0.057(2) Uani 1 1 d . U . . .
C12 C 0.5624(12) 0.7141(5) 0.4345(5) 0.069(3) Uani 1 1 d . U . . .
H12A H 0.5667 0.6771 0.4449 0.083 Uiso 1 1 calc R U . . .
C34 C 1.1713(9) 0.5555(6) 0.9374(5) 0.061(2) Uani 1 1 d . U . . .
H34A H 1.1526 0.5186 0.9429 0.073 Uiso 1 1 calc R U . . .
C1 C 0.5435(9) 0.9813(5) 0.4105(5) 0.057(2) Uani 1 1 d . U . . .
H1A H 0.5596 0.9635 0.3811 0.068 Uiso 1 1 calc R U . . .
C9 C 0.3218(9) 0.8687(6) 0.5843(4) 0.057(2) Uani 1 1 d . U . . .
H9A H 0.2888 0.8434 0.6042 0.068 Uiso 1 1 calc R U . . .
C27 C 1.0475(10) 0.7681(6) 1.0670(5) 0.063(2) Uani 1 1 d . U . . .
H27A H 1.0756 0.8003 1.0801 0.075 Uiso 1 1 calc R U . . .
C30 C 0.9604(10) 0.6788(5) 1.0266(4) 0.054(2) Uani 1 1 d . U . . .
H30A H 0.9305 0.6479 1.0124 0.065 Uiso 1 1 calc R U . . .
C4 C 0.4942(9) 1.0323(5) 0.4963(5) 0.059(2) Uani 1 1 d . U . . .
H4A H 0.4770 1.0488 0.5261 0.070 Uiso 1 1 calc R U . . .
C29 C 0.9512(10) 0.6851(6) 1.0757(4) 0.059(2) Uani 1 1 d . U . . .
H29A H 0.9155 0.6602 1.0947 0.071 Uiso 1 1 calc R U . . .
C3 C 0.5402(10) 1.0626(6) 0.4610(5) 0.063(2) Uani 1 1 d . U . . .
H3A H 0.5534 1.1003 0.4662 0.076 Uiso 1 1 calc R U . . .
C28 C 0.9987(10) 0.7316(6) 1.0966(5) 0.064(2) Uani 1 1 d . U . . .
H28A H 0.9967 0.7374 1.1305 0.077 Uiso 1 1 calc R U . . .
C33 C 1.2718(10) 0.5721(7) 0.9358(5) 0.069(3) Uani 1 1 d . U . . .
H33A H 1.3195 0.5450 0.9398 0.083 Uiso 1 1 calc R U . . .
C22 C 1.1954(11) 0.8600(6) 0.9128(6) 0.074(3) Uani 1 1 d . U . . .
H22A H 1.2271 0.8814 0.8892 0.088 Uiso 1 1 calc R U . . .
C21 C 1.1451(10) 0.8098(6) 0.8998(5) 0.064(2) Uani 1 1 d . U . . .
H21A H 1.1430 0.7990 0.8669 0.077 Uiso 1 1 calc R U . . .
O1W O 0.5407(16) 0.6036(8) 0.6861(8) 0.172(8) Uani 1 1 d . . . . .
C23 C 1.1952(12) 0.8753(6) 0.9617(6) 0.075(3) Uani 1 1 d . U . . .
H23A H 1.2245 0.9086 0.9714 0.090 Uiso 1 1 calc R U . . .
C24 C 1.1536(11) 0.8429(6) 0.9950(6) 0.069(2) Uani 1 1 d . U . . .
H24A H 1.1569 0.8525 1.0282 0.083 Uiso 1 1 calc R U . . .
N13 N 0.4193(13) 0.5852(9) 0.3050(7) 0.075(6) Uani 0.5 1 d G U P . .
C54 C 0.3948(13) 0.5621(11) 0.2584(8) 0.098(7) Uani 0.5 1 d G U P . .
C55 C 0.4772(16) 0.5664(11) 0.2273(6) 0.096(7) Uani 0.5 1 d G U P . .
N14 N 0.5527(12) 0.5922(9) 0.2546(7) 0.071(6) Uani 0.5 1 d G U P . .
C56 C 0.5170(14) 0.6038(10) 0.3027(7) 0.101(7) Uani 0.5 1 d G U P . .


_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
As8 O38 1.764(7) . ?
As8 O32 1.778(6) . ?
As8 O24 1.779(7) . ?
As7 O35 1.765(7) . ?
As7 O42 1.772(6) . ?
As7 O32 1.784(7) . ?
As6 O18 1.750(7) . ?
As6 O16 1.762(6) . ?
As6 O25 1.764(7) . ?
As6 Ni1 2.3039(15) . ?
As5 O39 1.748(7) . ?
As5 O41 1.768(6) . ?
As5 O25 1.786(7) . ?
As4 O22 1.763(7) . ?
As4 O11 1.788(6) . ?
As4 O2 1.791(8) . ?
As3 O2 1.769(7) . ?
As3 O15 1.770(7) . ?
As3 O26 1.782(7) . ?
As2 O23 1.763(6) . ?
As2 O33 1.778(7) . ?
As2 O20 1.787(8) . ?
As1 O31 1.745(6) . ?
As1 O21 1.769(6) . ?
As1 O20 1.790(7) . ?
Ni2 N10 2.059(8) . ?
Ni2 N5 2.072(9) . ?
Ni2 N8 2.089(8) . ?
Ni2 N6 2.096(7) . ?
Ni2 N7 2.101(9) . ?
Ni2 N9 2.102(9) . ?
Ni1 N3 1.939(9) . ?
Ni1 N2 2.032(8) . ?
Ni1 N1 2.066(9) . ?
V14 O5 1.605(7) . ?
V14 O40 1.928(6) . ?
V14 O36 1.943(6) . ?
V14 O42 2.006(6) . ?
V14 O41 2.026(6) . ?
V14 V4 2.844(2) . ?
V13 O10 1.605(7) . ?
V13 O36 1.931(6) . ?
V13 O30 1.937(7) . ?
V13 O35 2.010(7) . ?
V13 O31 2.023(7) . ?
V13 V8 3.012(2) . ?
V13 V4 3.048(2) . ?
V12 O12 1.577(7) . ?
V12 O24 1.964(7) . ?
V12 O16 1.973(6) . ?
V12 O42 1.984(6) . ?
V12 O41 1.992(6) . ?
V11 O8 1.589(7) . ?
V11 O29 1.925(7) . ?
V11 O37 1.930(7) . ?
V11 O16 2.007(7) . ?
V11 O24 2.021(6) . ?
V11 V10 2.890(2) . ?
V10 O14 1.607(7) . ?
V10 O29 1.929(7) . ?
V10 O37 1.940(6) . ?
V10 O22 1.980(6) . ?
V10 O15 1.980(7) . ?
V10 V6 3.018(2) . ?
V10 V9 3.038(2) . ?
V9 O13 1.609(7) . ?
V9 O37 1.929(7) . ?
V9 O34 1.934(7) . ?
V9 O38 2.006(6) . ?
V9 O15 2.013(6) . ?
V9 V8 3.025(2) . ?
V8 O17 1.613(6) . ?
V8 O34 1.924(6) . ?
V8 O30 1.930(7) . ?
V8 O35 1.986(7) . ?
V8 O38 1.990(7) . ?
V8 V2 2.892(2) . ?
V7 O6 1.594(7) . ?
V7 O28 1.922(7) . ?
V7 O27 1.929(7) . ?
V7 O11 2.011(7) . ?
V7 O33 2.022(7) . ?
V7 V5 2.833(2) . ?
V6 O7 1.586(7) . ?
V6 O29 1.917(7) . ?
V6 O28 1.941(7) . ?
V6 O22 2.011(7) . ?
V6 O18 2.012(7) . ?
V6 V5 3.024(2) . ?
V5 O1 1.587(7) . ?
V5 O27 1.932(7) . ?
V5 O28 1.940(7) . ?
V5 O18 1.982(6) . ?
V5 O39 2.023(7) . ?
V5 V1 3.030(2) . ?
V4 O19 1.604(6) . ?
V4 O40 1.911(6) . ?
V4 O36 1.928(6) . ?
V4 O23 2.005(6) . ?
V4 O31 2.018(7) . ?
V4 V1 3.048(2) . ?
V3 O4 1.578(7) . ?
V3 O26 1.961(7) . ?
V3 O11 1.974(7) . ?
V3 O33 1.976(7) . ?
V3 O21 1.988(7) . ?
V3 V2 3.115(2) . ?
V2 O9 1.605(7) . ?
V2 O34 1.923(7) . ?
V2 O30 1.935(6) . ?
V2 O21 2.002(7) . ?
V2 O26 2.012(7) . ?
V1 O3 1.597(7) . ?
V1 O27 1.920(6) . ?
V1 O40 1.927(6) . ?
V1 O39 1.989(6) . ?
V1 O23 2.027(7) . ?
Ni3 N11 1.792(8) . ?
Ni3 N13 1.792(15) . ?
N11 C53 1.4200 . ?
N11 C51 1.4200 . ?
C51 C52 1.4200 . ?
C52 N12 1.4200 . ?
N12 C53 1.4200 . ?
N3 C13 1.330(15) . ?
N3 C11 1.365(15) . ?
N10 C50 1.332(14) . ?
N10 C46 1.351(13) . ?
N8 C36 1.323(14) . ?
N8 C40 1.342(15) . ?
N2 C6 1.318(13) . ?
N2 C10 1.330(15) . ?
N9 C41 1.341(13) . ?
N9 C45 1.351(12) . ?
N7 C35 1.303(15) . ?
N7 C31 1.364(15) . ?
N6 C26 1.323(14) . ?
N6 C30 1.329(15) . ?
N5 C21 1.338(16) . ?
N5 C25 1.338(16) . ?
C31 C32 1.368(17) . ?
C11 C12 1.281(19) . ?
C46 C47 1.386(14) . ?
C46 C45 1.491(14) . ?
C49 C48 1.349(17) . ?
C49 C50 1.411(15) . ?
C45 C44 1.351(15) . ?
C48 C47 1.375(16) . ?
C13 N4 1.329(18) . ?
C40 C39 1.372(16) . ?
C10 C9 1.384(16) . ?
C36 C37 1.433(17) . ?
C36 C35 1.484(17) . ?
N1 C5 1.324(14) . ?
N1 C1 1.337(15) . ?
C6 C7 1.407(15) . ?
C6 C5 1.490(17) . ?
C8 C9 1.335(17) . ?
C8 C7 1.398(18) . ?
C35 C34 1.399(16) . ?
C37 C38 1.336(19) . ?
C5 C4 1.400(15) . ?
C32 C33 1.26(2) . ?
C39 C38 1.400(19) . ?
C44 C43 1.381(15) . ?
C26 C27 1.400(16) . ?
C26 C25 1.505(18) . ?
C43 C42 1.364(16) . ?
C42 C41 1.364(16) . ?
N4 C12 1.399(19) . ?
C2 C1 1.378(17) . ?
C2 C3 1.42(2) . ?
C25 C24 1.393(17) . ?
C34 C33 1.44(2) . ?
C27 C28 1.362(19) . ?
C30 C29 1.345(15) . ?
C4 C3 1.359(18) . ?
C29 C28 1.409(19) . ?
C22 C23 1.38(2) . ?
C22 C21 1.428(18) . ?
C23 C24 1.32(2) . ?
N13 C56 1.4200 . ?
N13 C54 1.4200 . ?
C54 C55 1.4200 . ?
C55 N14 1.4200 . ?
N14 C56 1.4200 . ?

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
O38 As8 O32 99.3(3) . . ?
O38 As8 O24 97.6(3) . . ?
O32 As8 O24 98.7(3) . . ?
O35 As7 O42 97.8(3) . . ?
O35 As7 O32 98.7(3) . . ?
O42 As7 O32 99.2(3) . . ?
O18 As6 O16 99.5(3) . . ?
O18 As6 O25 102.3(3) . . ?
O16 As6 O25 100.0(3) . . ?
O18 As6 Ni1 116.5(2) . . ?
O16 As6 Ni1 122.7(2) . . ?
O25 As6 Ni1 112.8(2) . . ?
O39 As5 O41 98.8(3) . . ?
O39 As5 O25 98.3(3) . . ?
O41 As5 O25 98.0(3) . . ?
O22 As4 O11 99.6(3) . . ?
O22 As4 O2 98.7(3) . . ?
O11 As4 O2 99.6(3) . . ?
O2 As3 O15 99.6(3) . . ?
O2 As3 O26 98.2(3) . . ?
O15 As3 O26 98.4(3) . . ?
O23 As2 O33 99.6(3) . . ?
O23 As2 O20 98.5(3) . . ?
O33 As2 O20 99.6(3) . . ?
O31 As1 O21 99.2(3) . . ?
O31 As1 O20 99.6(3) . . ?
O21 As1 O20 99.0(3) . . ?
N10 Ni2 N5 94.3(4) . . ?
N10 Ni2 N8 94.2(3) . . ?
N5 Ni2 N8 169.7(3) . . ?
N10 Ni2 N6 168.4(3) . . ?
N5 Ni2 N6 78.5(4) . . ?
N8 Ni2 N6 94.0(3) . . ?
N10 Ni2 N7 98.7(3) . . ?
N5 Ni2 N7 95.3(4) . . ?
N8 Ni2 N7 77.5(4) . . ?
N6 Ni2 N7 91.1(3) . . ?
N10 Ni2 N9 79.0(3) . . ?
N5 Ni2 N9 89.8(3) . . ?
N8 Ni2 N9 97.6(3) . . ?
N6 Ni2 N9 91.8(3) . . ?
N7 Ni2 N9 174.5(3) . . ?
N3 Ni1 N2 120.1(3) . . ?
N3 Ni1 N1 127.1(4) . . ?
N2 Ni1 N1 81.0(4) . . ?
N3 Ni1 As6 109.4(3) . . ?
N2 Ni1 As6 115.2(2) . . ?
N1 Ni1 As6 101.0(2) . . ?
O5 V14 O40 109.2(3) . . ?
O5 V14 O36 107.7(3) . . ?
O40 V14 O36 83.8(3) . . ?
O5 V14 O42 109.5(3) . . ?
O40 V14 O42 141.1(3) . . ?
O36 V14 O42 88.4(3) . . ?
O5 V14 O41 108.4(3) . . ?
O40 V14 O41 88.5(3) . . ?
O36 V14 O41 143.6(3) . . ?
O42 V14 O41 75.7(3) . . ?
O5 V14 V4 109.1(3) . . ?
O40 V14 V4 41.98(19) . . ?
O36 V14 V4 42.51(17) . . ?
O42 V14 V4 124.7(2) . . ?
O41 V14 V4 125.39(19) . . ?
O10 V13 O36 110.0(3) . . ?
O10 V13 O30 110.7(3) . . ?
O36 V13 O30 139.3(3) . . ?
O10 V13 O35 107.1(3) . . ?
O36 V13 O35 88.8(3) . . ?
O30 V13 O35 79.3(3) . . ?
O10 V13 O31 107.0(3) . . ?
O36 V13 O31 78.7(3) . . ?
O30 V13 O31 89.7(3) . . ?
O35 V13 O31 145.9(3) . . ?
O10 V13 V8 111.7(3) . . ?
O36 V13 V8 121.66(18) . . ?
O30 V13 V8 38.7(2) . . ?
O35 V13 V8 40.77(19) . . ?
O31 V13 V8 123.5(2) . . ?
O10 V13 V4 111.9(3) . . ?
O36 V13 V4 37.80(18) . . ?
O30 V13 V4 121.9(2) . . ?
O35 V13 V4 121.6(2) . . ?
O31 V13 V4 41.0(2) . . ?
V8 V13 V4 136.36(6) . . ?
O12 V12 O24 107.7(3) . . ?
O12 V12 O16 110.1(4) . . ?
O24 V12 O16 76.1(3) . . ?
O12 V12 O42 109.8(4) . . ?
O24 V12 O42 91.4(3) . . ?
O16 V12 O42 140.0(3) . . ?
O12 V12 O41 109.6(3) . . ?
O24 V12 O41 142.7(3) . . ?
O16 V12 O41 90.3(3) . . ?
O42 V12 O41 77.0(3) . . ?
O8 V11 O29 108.4(3) . . ?
O8 V11 O37 110.0(4) . . ?
O29 V11 O37 82.8(3) . . ?
O8 V11 O16 107.5(4) . . ?
O29 V11 O16 89.2(3) . . ?
O37 V11 O16 142.3(3) . . ?
O8 V11 O24 108.9(3) . . ?
O29 V11 O24 142.2(3) . . ?
O37 V11 O24 90.1(3) . . ?
O16 V11 O24 74.1(3) . . ?
O8 V11 V10 111.1(3) . . ?
O29 V11 V10 41.5(2) . . ?
O37 V11 V10 41.82(19) . . ?
O16 V11 V10 124.4(2) . . ?
O24 V11 V10 125.4(2) . . ?
O14 V10 O29 111.7(4) . . ?
O14 V10 O37 112.0(3) . . ?
O29 V10 O37 82.5(3) . . ?
O14 V10 O22 108.5(3) . . ?
O29 V10 O22 79.0(3) . . ?
O37 V10 O22 139.4(3) . . ?
O14 V10 O15 110.3(4) . . ?
O29 V10 O15 137.9(3) . . ?
O37 V10 O15 78.9(3) . . ?
O22 V10 O15 91.3(3) . . ?
O14 V10 V11 114.8(3) . . ?
O29 V10 V11 41.4(2) . . ?
O37 V10 V11 41.6(2) . . ?
O22 V10 V11 115.1(2) . . ?
O15 V10 V11 114.52(19) . . ?
O14 V10 V6 111.9(3) . . ?
O29 V10 V6 38.2(2) . . ?
O37 V10 V6 115.6(2) . . ?
O22 V10 V6 41.2(2) . . ?
O15 V10 V6 124.1(2) . . ?
V11 V10 V6 77.84(6) . . ?
O14 V10 V9 115.5(3) . . ?
O29 V10 V9 113.8(2) . . ?
O37 V10 V9 38.1(2) . . ?
O22 V10 V9 123.0(2) . . ?
O15 V10 V9 40.86(19) . . ?
V11 V10 V9 77.07(5) . . ?
V6 V10 V9 132.12(6) . . ?
O13 V9 O37 110.4(4) . . ?
O13 V9 O34 110.4(4) . . ?
O37 V9 O34 139.2(3) . . ?
O13 V9 O38 106.0(3) . . ?
O37 V9 O38 90.3(3) . . ?
O34 V9 O38 78.6(3) . . ?
O13 V9 O15 107.1(3) . . ?
O37 V9 O15 78.3(3) . . ?
O34 V9 O15 89.9(3) . . ?
O38 V9 O15 147.0(3) . . ?
O13 V9 V8 110.4(3) . . ?
O37 V9 V8 122.89(19) . . ?
O34 V9 V8 38.25(19) . . ?
O38 V9 V8 40.62(19) . . ?
O15 V9 V8 123.8(2) . . ?
O13 V9 V10 112.2(3) . . ?
O37 V9 V10 38.37(18) . . ?
O34 V9 V10 121.4(2) . . ?
O38 V9 V10 123.7(2) . . ?
O15 V9 V10 40.1(2) . . ?
V8 V9 V10 137.44(7) . . ?
O17 V8 O34 110.8(3) . . ?
O17 V8 O30 110.7(3) . . ?
O34 V8 O30 82.6(3) . . ?
O17 V8 O35 109.9(3) . . ?
O34 V8 O35 139.1(3) . . ?
O30 V8 O35 80.1(3) . . ?
O17 V8 O38 108.6(3) . . ?
O34 V8 O38 79.2(3) . . ?
O30 V8 O38 140.4(3) . . ?
O35 V8 O38 91.3(3) . . ?
O17 V8 V2 114.1(3) . . ?
O34 V8 V2 41.3(2) . . ?
O30 V8 V2 41.63(19) . . ?
O35 V8 V2 115.5(2) . . ?
O38 V8 V2 115.1(2) . . ?
O17 V8 V13 113.6(3) . . ?
O34 V8 V13 115.4(2) . . ?
O30 V8 V13 38.91(19) . . ?
O35 V8 V13 41.38(19) . . ?
O38 V8 V13 124.4(2) . . ?
V2 V8 V13 78.10(6) . . ?
O17 V8 V9 112.5(3) . . ?
O34 V8 V9 38.5(2) . . ?
O30 V8 V9 115.8(2) . . ?
O35 V8 V9 123.8(2) . . ?
O38 V8 V9 41.01(18) . . ?
V2 V8 V9 77.73(6) . . ?
V13 V8 V9 133.42(7) . . ?
O6 V7 O28 108.3(4) . . ?
O6 V7 O27 107.5(4) . . ?
O28 V7 O27 85.3(3) . . ?
O6 V7 O11 109.5(4) . . ?
O28 V7 O11 88.3(3) . . ?
O27 V7 O11 142.6(3) . . ?
O6 V7 O33 108.7(4) . . ?
O28 V7 O33 142.8(3) . . ?
O27 V7 O33 87.8(3) . . ?
O11 V7 O33 75.5(3) . . ?
O6 V7 V5 109.3(3) . . ?
O28 V7 V5 43.1(2) . . ?
O27 V7 V5 42.8(2) . . ?
O11 V7 V5 125.1(2) . . ?
O33 V7 V5 124.6(2) . . ?
O7 V6 O29 111.1(3) . . ?
O7 V6 O28 111.0(3) . . ?
O29 V6 O28 137.9(3) . . ?
O7 V6 O22 107.3(4) . . ?
O29 V6 O22 78.5(3) . . ?
O28 V6 O22 88.5(3) . . ?
O7 V6 O18 107.9(4) . . ?
O29 V6 O18 88.9(3) . . ?
O28 V6 O18 79.0(3) . . ?
O22 V6 O18 144.8(3) . . ?
O7 V6 V10 110.7(3) . . ?
O29 V6 V10 38.4(2) . . ?
O28 V6 V10 121.5(2) . . ?
O22 V6 V10 40.48(18) . . ?
O18 V6 V10 123.0(2) . . ?
O7 V6 V5 112.5(3) . . ?
O29 V6 V5 120.7(2) . . ?
O28 V6 V5 38.8(2) . . ?
O22 V6 V5 122.1(2) . . ?
O18 V6 V5 40.42(18) . . ?
V10 V6 V5 136.77(6) . . ?
O1 V5 O27 111.9(4) . . ?
O1 V5 O28 109.2(4) . . ?
O27 V5 O28 84.8(3) . . ?
O1 V5 O18 108.4(4) . . ?
O27 V5 O18 139.6(3) . . ?
O28 V5 O18 79.8(3) . . ?
O1 V5 O39 111.9(4) . . ?
O27 V5 O39 78.2(3) . . ?
O28 V5 O39 138.8(3) . . ?
O18 V5 O39 89.4(3) . . ?
O1 V5 V7 113.1(3) . . ?
O27 V5 V7 42.7(2) . . ?
O28 V5 V7 42.6(2) . . ?
O18 V5 V7 116.6(2) . . ?
O39 V5 V7 115.2(2) . . ?
O1 V5 V6 111.7(3) . . ?
O27 V5 V6 117.1(2) . . ?
O28 V5 V6 38.82(19) . . ?
O18 V5 V6 41.1(2) . . ?
O39 V5 V6 121.9(2) . . ?
V7 V5 V6 79.13(6) . . ?
O1 V5 V1 115.0(3) . . ?
O27 V5 V1 37.99(19) . . ?
O28 V5 V1 116.8(2) . . ?
O18 V5 V1 122.5(2) . . ?
O39 V5 V1 40.53(18) . . ?
V7 V5 V1 78.67(6) . . ?
V6 V5 V1 132.99(7) . . ?
O19 V4 O40 111.2(3) . . ?
O19 V4 O36 110.8(3) . . ?
O40 V4 O36 84.6(3) . . ?
O19 V4 O23 109.1(3) . . ?
O40 V4 O23 78.6(3) . . ?
O36 V4 O23 140.1(3) . . ?
O19 V4 O31 109.7(3) . . ?
O40 V4 O31 139.1(3) . . ?
O36 V4 O31 78.9(3) . . ?
O23 V4 O31 90.6(3) . . ?
O19 V4 V14 112.8(3) . . ?
O40 V4 V14 42.43(18) . . ?
O36 V4 V14 42.93(19) . . ?
O23 V4 V14 116.24(19) . . ?
O31 V4 V14 116.47(19) . . ?
O19 V4 V13 114.3(3) . . ?
O40 V4 V13 115.70(19) . . ?
O36 V4 V13 37.87(19) . . ?
O23 V4 V13 123.0(2) . . ?
O31 V4 V13 41.11(18) . . ?
V14 V4 V13 78.56(5) . . ?
O19 V4 V1 113.5(3) . . ?
O40 V4 V1 37.62(18) . . ?
O36 V4 V1 116.34(19) . . ?
O23 V4 V1 41.17(19) . . ?
O31 V4 V1 123.0(2) . . ?
V14 V4 V1 78.23(6) . . ?
V13 V4 V1 131.89(6) . . ?
O4 V3 O26 109.1(4) . . ?
O4 V3 O11 107.7(4) . . ?
O26 V3 O11 90.4(3) . . ?
O4 V3 O33 109.1(4) . . ?
O26 V3 O33 141.8(3) . . ?
O11 V3 O33 77.3(3) . . ?
O4 V3 O21 109.1(4) . . ?
O26 V3 O21 77.7(3) . . ?
O11 V3 O21 143.2(3) . . ?
O33 V3 O21 90.6(3) . . ?
O4 V3 V2 113.4(3) . . ?
O26 V3 V2 38.9(2) . . ?
O11 V3 V2 122.3(2) . . ?
O33 V3 V2 121.8(2) . . ?
O21 V3 V2 38.8(2) . . ?
O9 V2 O34 108.8(4) . . ?
O9 V2 O30 109.3(4) . . ?
O34 V2 O30 82.4(3) . . ?
O9 V2 O21 108.2(4) . . ?
O34 V2 O21 142.8(3) . . ?
O30 V2 O21 89.0(3) . . ?
O9 V2 O26 107.0(4) . . ?
O34 V2 O26 89.5(3) . . ?
O30 V2 O26 143.5(3) . . ?
O21 V2 O26 76.3(3) . . ?
O9 V2 V8 111.7(3) . . ?
O34 V2 V8 41.27(19) . . ?
O30 V2 V8 41.5(2) . . ?
O21 V2 V8 124.0(2) . . ?
O26 V2 V8 124.5(2) . . ?
O9 V2 V3 111.1(3) . . ?
O34 V2 V3 120.7(2) . . ?
O30 V2 V3 121.2(2) . . ?
O21 V2 V3 38.51(19) . . ?
O26 V2 V3 37.79(19) . . ?
V8 V2 V3 137.16(7) . . ?
O3 V1 O27 109.7(4) . . ?
O3 V1 O40 110.8(3) . . ?
O27 V1 O40 139.5(3) . . ?
O3 V1 O39 106.1(4) . . ?
O27 V1 O39 79.3(3) . . ?
O40 V1 O39 89.5(3) . . ?
O3 V1 O23 108.3(4) . . ?
O27 V1 O23 89.9(3) . . ?
O40 V1 O23 77.7(3) . . ?
O39 V1 O23 145.6(3) . . ?
O3 V1 V5 109.8(3) . . ?
O27 V1 V5 38.3(2) . . ?
O40 V1 V5 123.06(19) . . ?
O39 V1 V5 41.39(19) . . ?
O23 V1 V5 123.47(19) . . ?
O3 V1 V4 112.6(3) . . ?
O27 V1 V4 122.4(2) . . ?
O40 V1 V4 37.26(19) . . ?
O39 V1 V4 122.1(2) . . ?
O23 V1 V4 40.63(17) . . ?
V5 V1 V4 137.65(7) . . ?
N11 Ni3 N13 173.6(8) . . ?
C53 N11 C51 108.0 . . ?
C53 N11 Ni3 131.1(7) . . ?
C51 N11 Ni3 120.9(7) . . ?
C52 C51 N11 108.0 . . ?
C51 C52 N12 108.0 . . ?
C52 N12 C53 108.0 . . ?
N11 C53 N12 108.0 . . ?
As7 O42 V12 133.4(3) . . ?
As7 O42 V14 122.2(3) . . ?
V12 O42 V14 104.2(3) . . ?
As5 O41 V12 135.5(3) . . ?
As5 O41 V14 121.4(3) . . ?
V12 O41 V14 103.1(3) . . ?
V4 O40 V1 105.1(3) . . ?
V4 O40 V14 95.6(3) . . ?
V1 O40 V14 149.6(3) . . ?
As5 O39 V1 122.4(3) . . ?
As5 O39 V5 139.5(4) . . ?
V1 O39 V5 98.1(3) . . ?
As8 O38 V8 137.1(3) . . ?
As8 O38 V9 124.3(3) . . ?
V8 O38 V9 98.4(3) . . ?
V9 O37 V11 146.5(4) . . ?
V9 O37 V10 103.5(3) . . ?
V11 O37 V10 96.6(3) . . ?
V4 O36 V13 104.3(3) . . ?
V4 O36 V14 94.6(3) . . ?
V13 O36 V14 149.0(3) . . ?
As7 O35 V8 137.9(4) . . ?
As7 O35 V13 124.2(3) . . ?
V8 O35 V13 97.8(3) . . ?
V2 O34 V8 97.5(3) . . ?
V2 O34 V9 148.7(4) . . ?
V8 O34 V9 103.3(3) . . ?
As2 O33 V3 134.5(4) . . ?
As2 O33 V7 122.0(4) . . ?
V3 O33 V7 103.4(3) . . ?
As8 O32 As7 131.9(3) . . ?
As1 O31 V4 137.7(4) . . ?
As1 O31 V13 123.8(4) . . ?
V4 O31 V13 97.9(3) . . ?
V8 O30 V2 96.9(3) . . ?
V8 O30 V13 102.4(3) . . ?
V2 O30 V13 147.9(4) . . ?
V6 O29 V11 150.2(4) . . ?
V6 O29 V10 103.4(3) . . ?
V11 O29 V10 97.2(3) . . ?
V7 O28 V5 94.4(3) . . ?
V7 O28 V6 150.3(4) . . ?
V5 O28 V6 102.4(3) . . ?
V1 O27 V7 150.2(4) . . ?
V1 O27 V5 103.8(3) . . ?
V7 O27 V5 94.4(3) . . ?
As3 O26 V3 136.1(4) . . ?
As3 O26 V2 119.9(4) . . ?
V3 O26 V2 103.3(3) . . ?
As6 O25 As5 129.7(4) . . ?
As8 O24 V12 134.1(4) . . ?
As8 O24 V11 120.8(3) . . ?
V12 O24 V11 104.7(3) . . ?
As2 O23 V4 138.7(4) . . ?
As2 O23 V1 122.8(3) . . ?
V4 O23 V1 98.2(3) . . ?
As4 O22 V10 138.0(4) . . ?
As4 O22 V6 123.6(3) . . ?
V10 O22 V6 98.3(3) . . ?
As1 O21 V3 135.0(4) . . ?
As1 O21 V2 121.9(4) . . ?
V3 O21 V2 102.6(3) . . ?
As2 O20 As1 130.6(4) . . ?
As6 O18 V5 136.3(4) . . ?
As6 O18 V6 124.8(3) . . ?
V5 O18 V6 98.4(3) . . ?
As6 O16 V12 133.7(4) . . ?
As6 O16 V11 120.6(3) . . ?
V12 O16 V11 105.0(3) . . ?
As3 O15 V10 136.9(4) . . ?
As3 O15 V9 123.5(4) . . ?
V10 O15 V9 99.1(3) . . ?
As4 O11 V3 134.2(4) . . ?
As4 O11 V7 121.9(4) . . ?
V3 O11 V7 103.9(3) . . ?
C13 N3 C11 103.9(10) . . ?
C13 N3 Ni1 125.8(8) . . ?
C11 N3 Ni1 128.2(9) . . ?
C50 N10 C46 119.3(9) . . ?
C50 N10 Ni2 125.9(7) . . ?
C46 N10 Ni2 114.8(6) . . ?
As3 O2 As4 130.8(4) . . ?
C36 N8 C40 120.4(10) . . ?
C36 N8 Ni2 114.4(7) . . ?
C40 N8 Ni2 125.1(8) . . ?
C6 N2 C10 120.9(10) . . ?
C6 N2 Ni1 113.5(8) . . ?
C10 N2 Ni1 125.1(7) . . ?
C41 N9 C45 116.9(9) . . ?
C41 N9 Ni2 128.0(7) . . ?
C45 N9 Ni2 114.7(6) . . ?
C35 N7 C31 118.3(10) . . ?
C35 N7 Ni2 115.2(7) . . ?
C31 N7 Ni2 126.5(8) . . ?
C26 N6 C30 118.0(9) . . ?
C26 N6 Ni2 115.2(8) . . ?
C30 N6 Ni2 126.7(7) . . ?
C21 N5 C25 118.0(11) . . ?
C21 N5 Ni2 126.2(9) . . ?
C25 N5 Ni2 115.6(8) . . ?
N7 C31 C32 122.8(12) . . ?
C12 C11 N3 111.7(12) . . ?
N10 C46 C47 121.1(10) . . ?
N10 C46 C45 116.7(8) . . ?
C47 C46 C45 122.2(10) . . ?
C48 C49 C50 120.5(11) . . ?
N9 C45 C44 122.4(9) . . ?
N9 C45 C46 113.8(9) . . ?
C44 C45 C46 123.7(9) . . ?
C49 C48 C47 118.2(10) . . ?
C48 C47 C46 120.2(11) . . ?
N4 C13 N3 112.1(12) . . ?
N8 C40 C39 122.5(11) . . ?
N2 C10 C9 121.4(11) . . ?
N8 C36 C37 120.2(10) . . ?
N8 C36 C35 116.1(10) . . ?
C37 C36 C35 123.8(11) . . ?
C5 N1 C1 120.1(10) . . ?
C5 N1 Ni1 112.6(8) . . ?
C1 N1 Ni1 127.2(8) . . ?
N2 C6 C7 120.2(11) . . ?
N2 C6 C5 116.4(9) . . ?
C7 C6 C5 123.3(10) . . ?
C9 C8 C7 119.9(11) . . ?
N7 C35 C34 122.1(11) . . ?
N7 C35 C36 115.4(10) . . ?
C34 C35 C36 122.4(11) . . ?
C8 C7 C6 118.2(11) . . ?
C38 C37 C36 118.1(12) . . ?
N1 C5 C4 120.9(12) . . ?
N1 C5 C6 116.0(9) . . ?
C4 C5 C6 123.0(11) . . ?
C33 C32 C31 119.3(13) . . ?
C40 C39 C38 116.9(12) . . ?
N10 C50 C49 120.5(10) . . ?
C45 C44 C43 119.8(10) . . ?
N6 C26 C27 121.5(12) . . ?
N6 C26 C25 115.4(10) . . ?
C27 C26 C25 122.7(11) . . ?
C42 C43 C44 118.4(11) . . ?
C41 C42 C43 119.0(11) . . ?
C13 N4 C12 104.7(11) . . ?
N9 C41 C42 123.3(10) . . ?
C37 C38 C39 121.7(12) . . ?
C1 C2 C3 116.4(13) . . ?
N5 C25 C24 121.9(13) . . ?
N5 C25 C26 114.9(10) . . ?
C24 C25 C26 123.2(12) . . ?
C11 C12 N4 107.5(12) . . ?
C35 C34 C33 115.7(13) . . ?
N1 C1 C2 123.2(13) . . ?
C8 C9 C10 119.3(13) . . ?
C28 C27 C26 118.7(12) . . ?
N6 C30 C29 125.6(12) . . ?
C3 C4 C5 119.2(12) . . ?
C30 C29 C28 116.3(13) . . ?
C4 C3 C2 120.2(12) . . ?
C27 C28 C29 119.7(11) . . ?
C32 C33 C34 121.8(13) . . ?
C23 C22 C21 117.4(14) . . ?
N5 C21 C22 121.8(13) . . ?
C24 C23 C22 120.3(14) . . ?
C23 C24 C25 120.4(15) . . ?
C56 N13 C54 108.0 . . ?
C56 N13 Ni3 126.7(13) . . ?
C54 N13 Ni3 124.6(13) . . ?
N13 C54 C55 108.0 . . ?
N14 C55 C54 108.0 . . ?
C55 N14 C56 108.0 . . ?
N13 C56 N14 108.0 . . ?

_refine_diff_density_max         2.751
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.143

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

data_shelx_2
_database_code_depnum_ccdc_archive 'CCDC 1424797'
_audit_update_record             
;
2015-09-16 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_shelx_2             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1w Check
RESPONSE: The hydrogens of the water molecule was not added.
;

_vrf_PLAT341_shelx_2             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0562 Ang
RESPONSE: The quality of this crystal was poor.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H36 As8 N8 Ni2 O44 V14'
_chemical_formula_weight         2786.73

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.169(2)
_cell_length_b                   16.057(3)
_cell_length_c                   40.244(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7863(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1008
_cell_measurement_theta_min      2.3887
_cell_measurement_theta_max      19.6442

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.354
_exptl_crystal_F_000             5352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    5.483
_shelx_estimated_absorpt_T_min   0.230
_shelx_estimated_absorpt_T_max   0.536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.348
_exptl_absorpt_correction_T_max  0.523
_exptl_absorpt_process_details   
'SADABS-2004/1 (Bruker,2004) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            44504
_diffrn_reflns_av_unetI/netI     0.1788
_diffrn_reflns_av_R_equivalents  0.1618
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.365
_diffrn_reflns_theta_max         25.217
_diffrn_reflns_theta_full        25.217
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             14059
_reflns_number_gt                8411
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.992

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0948P)²+11.9765P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00049(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.04(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         14059
_refine_ls_number_parameters     1041
_refine_ls_number_restraints     163
_refine_ls_R_factor_all          0.1534
_refine_ls_R_factor_gt           0.0875
_refine_ls_wR_factor_ref         0.2262
_refine_ls_wR_factor_gt          0.1915
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.5494(3) -0.26030(19) 0.94217(8) 0.0357(7) Uani 1 1 d . . . . .
As2 As 0.4419(3) -0.43516(19) 0.91973(8) 0.0366(7) Uani 1 1 d . . . . .
As3 As 1.0584(3) -0.3661(2) 0.97168(7) 0.0366(8) Uani 1 1 d . . . . .
As7 As 0.7612(2) -0.2296(2) 0.80736(8) 0.0353(8) Uani 1 1 d . . . . .
As8 As 0.6518(3) -0.4055(2) 0.78594(8) 0.0389(8) Uani 1 1 d . . . . .
Ni1 Ni 1.0552(3) -0.0124(2) 0.93917(9) 0.0283(8) Uani 1 1 d . . . . .
As6 As 0.9669(3) -0.6773(2) 0.85934(9) 0.0437(9) Uani 1 1 d . . . . .
As4 As 1.1691(2) -0.35287(19) 0.89918(8) 0.0328(7) Uani 1 1 d . . . . .
Ni2 Ni 0.3106(3) -0.5559(2) 0.80061(9) 0.0291(9) Uani 1 1 d . . . . .
As5 As 0.8535(3) -0.6924(2) 0.93207(9) 0.0458(9) Uani 1 1 d . . . . .
V11 V 1.0527(4) -0.5405(3) 0.92089(12) 0.0290(11) Uani 1 1 d . . . . .
V12 V 0.9362(4) -0.4031(3) 0.79908(12) 0.0344(12) Uani 1 1 d . . . . .
V13 V 0.9979(4) -0.2623(3) 0.84653(12) 0.0300(12) Uani 1 1 d . . . . .
V14 V 0.9489(4) -0.2164(3) 0.91760(12) 0.0290(11) Uani 1 1 d . . . . .
V15 V 0.5482(4) -0.5050(3) 0.85041(12) 0.0326(12) Uani 1 1 d . . . . .
V16 V 0.8078(4) -0.5636(3) 0.80894(14) 0.0371(13) Uani 1 1 d . . . . .
V17 V 0.7383(4) -0.1933(3) 0.88813(12) 0.0332(12) Uani 1 1 d . . . . .
V18 V 0.6584(4) -0.4426(3) 0.97783(13) 0.0335(12) Uani 1 1 d . . . . .
V19 V 1.0683(4) -0.4889(3) 0.84672(12) 0.0297(11) Uani 1 1 d . . . . .
V20 V 0.5603(4) -0.3125(3) 0.85898(12) 0.0275(10) Uani 1 1 d . . . . .
V21 V 0.6135(4) -0.5930(3) 0.93390(14) 0.0357(13) Uani 1 1 d . . . . .
V22 V 0.8720(4) -0.5176(3) 0.97477(13) 0.0380(13) Uani 1 1 d . . . . .
V23 V 0.6828(4) -0.6485(3) 0.86503(14) 0.0430(14) Uani 1 1 d . . . . .
V24 V 0.8033(4) -0.2906(3) 0.97046(13) 0.0341(12) Uani 1 1 d . . . . .
O15 O 0.5442(15) -0.4806(11) 0.9436(4) 0.030(4) Uani 1 1 d . . . . .
O14 O 0.6005(15) -0.2572(12) 0.9009(5) 0.032(5) Uani 1 1 d . U . . .
O13 O 1.0406(15) -0.3753(11) 0.8332(4) 0.028(4) Uani 1 1 d . . . . .
O12 O 0.9582(16) -0.3005(12) 0.9552(5) 0.039(5) Uani 1 1 d . . . . .
O11 O 1.0785(14) -0.1969(12) 0.8293(5) 0.034(5) Uani 1 1 d . . . . .
O10 O 0.7027(19) -0.1005(13) 0.8867(5) 0.049(6) Uani 1 1 d . . . . .
O9 O 0.5159(16) -0.4134(11) 0.8822(5) 0.039(5) Uani 1 1 d . . . . .
O8 O 0.5360(19) -0.6596(13) 0.9500(6) 0.051(6) Uani 1 1 d . . . . .
O7 O 0.8055(15) -0.4103(12) 0.9818(4) 0.029(4) Uani 1 1 d . . . . .
O6 O 0.4508(16) -0.2716(13) 0.8459(5) 0.040(5) Uani 1 1 d . . . . .
O5 O 1.1648(16) -0.3500(13) 0.9423(5) 0.044(5) Uani 1 1 d . . . . .
O4 O 0.5972(15) -0.4038(12) 0.8269(5) 0.033(5) Uani 1 1 d . U . . .
O3 O 0.6463(15) -0.3266(11) 0.9604(5) 0.032(5) Uani 1 1 d . . . . .
O2 O 1.0090(15) -0.1308(11) 0.9282(4) 0.027(4) Uani 1 1 d . U . . .
O1 O 1.0597(15) -0.2813(11) 0.8923(5) 0.031(5) Uani 1 1 d . . . . .
O30 O 0.9525(16) -0.5172(12) 0.8166(5) 0.033(5) Uani 1 1 d . . . . .
O29 O 0.7340(15) -0.6546(12) 0.9124(5) 0.037(5) Uani 1 1 d . . . . .
O28 O 1.1847(14) -0.5144(13) 0.8337(6) 0.042(5) Uani 1 1 d . . . . .
O27 O 0.7958(15) -0.2191(11) 0.9307(5) 0.032(5) Uani 1 1 d . U . . .
O26 O 0.8397(17) -0.6442(14) 0.8477(6) 0.048(6) Uani 1 1 d . U . . .
O25 O 0.8879(14) -0.2098(11) 0.8748(4) 0.024(4) Uani 1 1 d . U . . .
O24 O 0.5747(16) -0.5796(13) 0.8880(5) 0.039(5) Uani 1 1 d . . . . .
O23 O 0.9175(15) -0.5950(13) 0.9387(5) 0.040(5) Uani 1 1 d . . . . .
O22 O 0.9339(16) -0.7249(12) 0.8963(5) 0.042(5) Uani 1 1 d . U . . .
O21 O 0.8765(13) -0.2908(12) 0.8131(4) 0.028(4) Uani 1 1 d . . . . .
O20 O 0.6659(13) -0.5648(12) 0.8308(5) 0.032(5) Uani 1 1 d . . . . .
O19 O 0.4440(16) -0.3328(12) 0.9361(5) 0.041(5) Uani 1 1 d . . . . .
O18 O 0.6895(16) -0.2483(12) 0.8452(5) 0.038(5) Uani 1 1 d . . . . .
O17 O 0.4351(18) -0.5267(17) 0.8340(5) 0.058(7) Uani 1 1 d . . . . .
O16 O 1.0046(15) -0.4612(13) 0.9562(5) 0.038(5) Uani 1 1 d . . . . .
O42 O 1.0142(14) -0.5816(12) 0.8760(5) 0.034(5) Uani 1 1 d . . . . .
O41 O 0.6879(14) -0.2997(13) 0.7818(5) 0.037(5) Uani 1 1 d . . . . .
O40 O 0.6020(15) -0.4491(13) 1.0147(5) 0.037(5) Uani 1 1 d . . . . .
O39 O 1.0939(16) -0.4454(14) 0.8920(5) 0.040(5) Uani 1 1 d . . . . .
O38 O 0.7991(19) -0.6168(14) 0.7751(6) 0.056(7) Uani 1 1 d . . . . .
O37 O 1.160(2) -0.5856(13) 0.9323(7) 0.060(7) Uani 1 1 d . . . . .
O36 O 0.800(2) -0.2367(17) 1.0026(5) 0.060(7) Uani 1 1 d . . . . .
O35 O 0.7802(16) -0.4435(14) 0.7942(5) 0.042(6) Uani 1 1 d . . . . .
O34 O 0.7206(16) -0.5454(12) 0.9652(5) 0.035(5) Uani 1 1 d . . . . .
O33 O 0.9914(19) -0.3945(14) 0.7626(6) 0.054(6) Uani 1 1 d . . . . .
O32 O 0.6283(18) -0.7353(14) 0.8540(7) 0.060(7) Uani 1 1 d . . . . .
O31 O 0.9067(18) -0.5539(17) 1.0087(5) 0.053(7) Uani 1 1 d . . . . .
C1 C 0.864(2) 0.0021(18) 0.9863(5) 0.069(13) Uani 1 1 d G . . . .
H1A H 0.9098 -0.0234 1.0016 0.083 Uiso 1 1 calc R U . . .
C2 C 0.758(2) 0.026(2) 0.9955(6) 0.115(18) Uani 1 1 d G U . . .
H2A H 0.7336 0.0159 1.0171 0.138 Uiso 1 1 calc R U . . .
C3 C 0.6889(17) 0.064(2) 0.9726(9) 0.119(19) Uani 1 1 d G U . . .
H3A H 0.6182 0.0793 0.9788 0.143 Uiso 1 1 calc R U . . .
C4 C 0.7253(18) 0.0780(17) 0.9404(8) 0.093(14) Uani 1 1 d G U . . .
H4A H 0.6791 0.1034 0.9250 0.112 Uiso 1 1 calc R U . . .
C5 C 0.8309(18) 0.0545(15) 0.9311(5) 0.063(11) Uani 1 1 d G U . . .
N1 N 0.9000(13) 0.0165(13) 0.9541(5) 0.040(6) Uani 1 1 d G U . . .
N2 N 0.9854(18) 0.0308(13) 0.8947(5) 0.052(8) Uani 1 1 d G U . . .
C6 C 0.8793(18) 0.0618(16) 0.8981(6) 0.071(13) Uani 1 1 d G U . . .
C7 C 0.8235(18) 0.0921(19) 0.8705(8) 0.093(15) Uani 1 1 d G U . . .
H7A H 0.7526 0.1128 0.8728 0.111 Uiso 1 1 calc R U . . .
C8 C 0.874(3) 0.091(2) 0.8395(6) 0.102(15) Uani 1 1 d G U . . .
H8A H 0.8365 0.1116 0.8210 0.123 Uiso 1 1 calc R U . . .
C9 C 0.980(3) 0.060(2) 0.8361(5) 0.108(15) Uani 1 1 d G U . . .
H9A H 1.0135 0.0599 0.8154 0.130 Uiso 1 1 calc R U . . .
C10 C 1.0357(17) 0.0301(17) 0.8637(7) 0.083(14) Uani 1 1 d G U . . .
H10A H 1.1066 0.0093 0.8614 0.100 Uiso 1 1 calc R U . . .
C11 C 1.077(3) 0.1662(19) 0.9648(9) 0.058(11) Uani 1 1 d . . . . .
H11A H 1.0045 0.1635 0.9716 0.069 Uiso 1 1 calc R U . . .
C12 C 1.144(4) 0.240(3) 0.9700(11) 0.075(12) Uani 1 1 d . U . . .
H12A H 1.1133 0.2854 0.9810 0.090 Uiso 1 1 calc R U . . .
C13 C 1.253(4) 0.246(2) 0.9589(10) 0.073(11) Uani 1 1 d . U . . .
H13A H 1.2927 0.2947 0.9623 0.088 Uiso 1 1 calc R U . . .
C14 C 1.304(3) 0.178(2) 0.9429(11) 0.071(12) Uani 1 1 d . . . . .
H14A H 1.3757 0.1803 0.9351 0.085 Uiso 1 1 calc R U . . .
C15 C 1.234(3) 0.1062(19) 0.9396(9) 0.042(8) Uani 1 1 d . . . . .
C16 C 1.280(3) 0.029(2) 0.9245(8) 0.043(8) Uani 1 1 d . U . . .
C17 C 1.387(4) 0.031(3) 0.9120(10) 0.083(14) Uani 1 1 d . U . . .
H17A H 1.4280 0.0798 0.9112 0.100 Uiso 1 1 calc R U . . .
C18 C 1.428(3) -0.048(3) 0.9006(10) 0.069(11) Uani 1 1 d . U . . .
H18A H 1.5020 -0.0555 0.8954 0.083 Uiso 1 1 calc R U . . .
C19 C 1.347(4) -0.119(3) 0.8975(11) 0.091(15) Uani 1 1 d . . . . .
H19A H 1.3673 -0.1700 0.8889 0.110 Uiso 1 1 calc R U . . .
C20 C 1.248(3) -0.105(3) 0.9071(10) 0.063(11) Uani 1 1 d . . . . .
H20A H 1.1984 -0.1485 0.9045 0.076 Uiso 1 1 calc R U . . .
C21 C 0.360(3) -0.711(3) 0.8419(10) 0.076(14) Uani 1 1 d . . . . .
H21A H 0.4025 -0.6762 0.8554 0.091 Uiso 1 1 calc R U . . .
C22 C 0.365(4) -0.794(3) 0.8479(15) 0.097(18) Uani 1 1 d . . . . .
H22A H 0.4204 -0.8167 0.8609 0.117 Uiso 1 1 calc R U . . .
C23 C 0.288(5) -0.840(4) 0.8344(15) 0.116(19) Uani 1 1 d . U . . .
H23A H 0.2790 -0.8942 0.8419 0.139 Uiso 1 1 calc R U . . .
C24 C 0.219(4) -0.811(4) 0.8095(14) 0.102(15) Uani 1 1 d . U . . .
H24A H 0.1732 -0.8454 0.7970 0.122 Uiso 1 1 calc R U . . .
C25 C 0.227(3) -0.724(2) 0.8051(9) 0.051(9) Uani 1 1 d . U . . .
C26 C 0.153(3) -0.682(2) 0.7789(8) 0.041(8) Uani 1 1 d . U . . .
C27 C 0.065(3) -0.719(3) 0.7655(11) 0.064(12) Uani 1 1 d . . . . .
H27A H 0.0446 -0.7725 0.7712 0.077 Uiso 1 1 calc R U . . .
C28 C 0.007(4) -0.674(4) 0.7435(11) 0.10(2) Uani 1 1 d . U . . .
H28A H -0.0534 -0.6991 0.7338 0.117 Uiso 1 1 calc R U . . .
C29 C 0.029(3) -0.598(4) 0.7345(9) 0.085(15) Uani 1 1 d . U . . .
H29A H -0.0124 -0.5694 0.7188 0.103 Uiso 1 1 calc R U . . .
C30 C 0.124(2) -0.561(2) 0.7513(9) 0.045(9) Uani 1 1 d . . . . .
H30A H 0.1422 -0.5063 0.7469 0.054 Uiso 1 1 calc R U . . .
C31 C 0.266(3) -0.369(2) 0.7865(9) 0.054(9) Uani 1 1 d . U . . .
H31A H 0.2308 -0.3665 0.8070 0.065 Uiso 1 1 calc R U . . .
C32 C 0.265(3) -0.301(2) 0.7676(10) 0.056(10) Uani 1 1 d . U . . .
H32A H 0.2328 -0.2529 0.7761 0.067 Uiso 1 1 calc R U . . .
C33 C 0.305(3) -0.297(2) 0.7388(9) 0.057(10) Uani 1 1 d . U . . .
H33A H 0.3004 -0.2498 0.7258 0.068 Uiso 1 1 calc R U . . .
C34 C 0.361(3) -0.374(3) 0.7269(10) 0.067(12) Uani 1 1 d . U . . .
C35 C 0.409(5) -0.383(4) 0.6963(15) 0.117(16) Uani 1 1 d . U . . .
H35A H 0.3967 -0.3413 0.6807 0.140 Uiso 1 1 calc R U . . .
C36 C 0.480(4) -0.454(3) 0.6860(12) 0.095(14) Uani 1 1 d . U . . .
H36A H 0.5278 -0.4525 0.6679 0.114 Uiso 1 1 calc R U . . .
C37 C 0.466(4) -0.528(2) 0.7073(8) 0.059(11) Uani 1 1 d . U . . .
C38 C 0.517(3) -0.602(3) 0.7001(9) 0.057(10) Uani 1 1 d . . . . .
H38A H 0.5537 -0.6083 0.6800 0.069 Uiso 1 1 calc R U . . .
C39 C 0.514(2) -0.666(2) 0.7213(9) 0.048(9) Uani 1 1 d . . . . .
H39A H 0.5402 -0.7185 0.7156 0.057 Uiso 1 1 calc R U . . .
C40 C 0.468(2) -0.649(2) 0.7539(8) 0.047(9) Uani 1 1 d . . . . .
H40A H 0.4762 -0.6892 0.7703 0.056 Uiso 1 1 calc R U . . .
C41 C 0.417(3) -0.518(2) 0.7383(7) 0.039(8) Uani 1 1 d . . . . .
C42 C 0.367(3) -0.4418(19) 0.7488(8) 0.038(7) Uani 1 1 d . U . . .
N3 N 1.129(3) 0.0995(16) 0.9491(7) 0.049(8) Uani 1 1 d . . . . .
N4 N 1.210(2) -0.0333(15) 0.9208(6) 0.038(6) Uani 1 1 d . . . . .
N5 N 0.302(2) -0.6752(16) 0.8193(7) 0.048(7) Uani 1 1 d . . . . .
N6 N 0.185(3) -0.6035(19) 0.7724(7) 0.054(8) Uani 1 1 d . . . . .
N7 N 0.3135(19) -0.4401(14) 0.7780(6) 0.033(6) Uani 1 1 d . . . . .
N8 N 0.415(2) -0.5812(16) 0.7617(6) 0.039(6) Uani 1 1 d . U . . .
O2W O -0.214(4) -0.555(3) 0.6952(13) 0.162(18) Uani 1 1 d . . . . .
O1W O 0.809(4) -0.431(3) 0.8891(11) 0.158(18) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O19 1.750(19) . ?
As1 O3 1.750(18) . ?
As1 O14 1.776(19) . ?
As2 O15 1.734(18) . ?
As2 O19 1.77(2) . ?
As2 O9 1.79(2) . ?
As3 O12 1.74(2) . ?
As3 O5 1.77(2) . ?
As3 O16 1.77(2) . ?
As7 O21 1.728(17) . ?
As7 O41 1.77(2) . ?
As7 O18 1.78(2) . ?
As8 O35 1.71(2) . ?
As8 O41 1.76(2) . ?
As8 O4 1.776(19) . ?
Ni1 O2 2.031(17) . ?
Ni1 N1 2.035(17) . ?
Ni1 O40 2.04(2) 4_547 ?
Ni1 N3 2.05(3) . ?
Ni1 N4 2.05(2) . ?
Ni1 N2 2.098(19) . ?
As6 O26 1.70(2) . ?
As6 O22 1.72(2) . ?
As6 O42 1.773(19) . ?
As4 O5 1.74(2) . ?
As4 O39 1.77(2) . ?
As4 O1 1.780(17) . ?
Ni2 N6 2.05(3) . ?
Ni2 N8 2.05(2) . ?
Ni2 N5 2.06(3) . ?
Ni2 N7 2.07(2) . ?
Ni2 O17 2.08(2) . ?
Ni2 O28 2.14(2) 1_455 ?
As5 O29 1.764(19) . ?
As5 O23 1.77(2) . ?
As5 O22 1.82(2) . ?
V11 O37 1.56(2) . ?
V11 O42 1.98(2) . ?
V11 O39 1.98(2) . ?
V11 O16 2.00(2) . ?
V11 O23 1.997(19) . ?
V11 V19 3.104(7) . ?
V11 V22 3.110(7) . ?
V12 O33 1.62(2) . ?
V12 O13 1.924(17) . ?
V12 O30 1.97(2) . ?
V12 O35 2.02(2) . ?
V12 O21 2.025(19) . ?
V12 V19 2.857(7) . ?
V12 V16 3.040(8) . ?
V12 V13 3.053(7) . ?
V13 O11 1.595(18) . ?
V13 O25 1.951(19) . ?
V13 O13 1.960(18) . ?
V13 O1 2.013(19) . ?
V13 O21 2.050(17) . ?
V13 V14 3.014(7) . ?
V14 O2 1.614(17) . ?
V14 O25 1.877(18) . ?
V14 O27 1.936(19) . ?
V14 O1 1.985(19) . ?
V14 O12 2.03(2) . ?
V14 V17 2.848(7) . ?
V14 V24 3.013(7) . ?
V15 O17 1.56(2) . ?
V15 O20 1.897(18) . ?
V15 O24 1.96(2) . ?
V15 O4 1.97(2) . ?
V15 O9 1.99(2) . ?
V15 V23 2.887(8) . ?
V15 V20 3.114(7) . ?
V16 O38 1.61(2) . ?
V16 O20 1.937(18) . ?
V16 O30 1.94(2) . ?
V16 O35 2.04(2) . ?
V16 O26 2.06(2) . ?
V16 V23 3.044(8) . ?
V17 O10 1.55(2) . ?
V17 O27 1.897(19) . ?
V17 O25 1.916(18) . ?
V17 O18 2.03(2) . ?
V17 O14 2.031(19) . ?
V17 V20 3.120(7) . ?
V18 O40 1.64(2) . ?
V18 O7 1.870(19) . ?
V18 O34 1.89(2) . ?
V18 O3 1.996(19) . ?
V18 O15 2.050(19) . ?
V18 V22 2.867(7) . ?
V18 V24 3.026(7) . ?
V18 V21 3.042(8) . ?
V19 O28 1.565(19) . ?
V19 O30 1.912(19) . ?
V19 O13 1.933(18) . ?
V19 O39 1.97(2) . ?
V19 O42 2.01(2) . ?
V20 O6 1.58(2) . ?
V20 O9 1.95(2) . ?
V20 O18 1.96(2) . ?
V20 O14 1.967(18) . ?
V20 O4 2.006(18) . ?
V21 O8 1.57(2) . ?
V21 O24 1.92(2) . ?
V21 O34 1.97(2) . ?
V21 O29 1.970(19) . ?
V21 O15 2.029(18) . ?
V21 V23 3.031(8) . ?
V22 O31 1.54(2) . ?
V22 O7 1.92(2) . ?
V22 O34 1.93(2) . ?
V22 O23 1.99(2) . ?
V22 O16 2.00(2) . ?
V23 O32 1.61(2) . ?
V23 O20 1.94(2) . ?
V23 O24 1.95(2) . ?
V23 O29 2.01(2) . ?
V23 O26 2.03(2) . ?
V24 O36 1.56(2) . ?
V24 O27 1.971(19) . ?
V24 O7 1.977(19) . ?
V24 O12 1.99(2) . ?
V24 O3 2.037(19) . ?
O28 Ni2 2.14(2) 1_655 ?
O40 Ni1 2.04(2) 4_447 ?
C1 C2 1.3900 . ?
C1 N1 1.3900 . ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 N1 1.3900 . ?
C5 C6 1.46(3) . ?
N2 C6 1.3900 . ?
N2 C10 1.3900 . ?
C6 C7 1.3900 . ?
C7 C8 1.3900 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C11 N3 1.39(4) . ?
C11 C12 1.45(5) . ?
C12 C13 1.41(6) . ?
C13 C14 1.40(6) . ?
C14 C15 1.44(4) . ?
C15 N3 1.34(4) . ?
C15 C16 1.48(5) . ?
C16 N4 1.32(4) . ?
C16 C17 1.40(5) . ?
C17 C18 1.45(6) . ?
C18 C19 1.51(6) . ?
C19 C20 1.27(5) . ?
C20 N4 1.36(4) . ?
C21 N5 1.29(4) . ?
C21 C22 1.36(5) . ?
C22 C23 1.32(7) . ?
C23 C24 1.38(7) . ?
C24 C25 1.42(6) . ?
C25 N5 1.33(4) . ?
C25 C26 1.54(5) . ?
C26 N6 1.34(4) . ?
C26 C27 1.34(4) . ?
C27 C28 1.34(7) . ?
C28 C29 1.29(7) . ?
C29 C30 1.46(6) . ?
C30 N6 1.31(4) . ?
C31 N7 1.32(4) . ?
C31 C32 1.33(5) . ?
C32 C33 1.26(5) . ?
C33 C34 1.49(6) . ?
C34 C35 1.37(6) . ?
C34 C42 1.40(5) . ?
C35 C36 1.49(7) . ?
C36 C37 1.47(6) . ?
C37 C38 1.37(5) . ?
C37 C41 1.40(4) . ?
C38 C39 1.33(5) . ?
C39 C40 1.45(5) . ?
C40 N8 1.30(4) . ?
C41 N8 1.39(4) . ?
C41 C42 1.42(4) . ?
C42 N7 1.35(4) . ?

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
O19 As1 O3 98.5(9) . . ?
O19 As1 O14 98.3(9) . . ?
O3 As1 O14 100.0(9) . . ?
O15 As2 O19 100.0(9) . . ?
O15 As2 O9 100.8(9) . . ?
O19 As2 O9 97.2(9) . . ?
O12 As3 O5 99.7(10) . . ?
O12 As3 O16 97.4(9) . . ?
O5 As3 O16 99.2(9) . . ?
O21 As7 O41 97.2(8) . . ?
O21 As7 O18 100.8(9) . . ?
O41 As7 O18 98.3(9) . . ?
O35 As8 O41 97.7(10) . . ?
O35 As8 O4 99.7(9) . . ?
O41 As8 O4 99.6(9) . . ?
O2 Ni1 N1 91.2(8) . . ?
O2 Ni1 O40 89.5(8) . 4_547 ?
N1 Ni1 O40 93.5(8) . 4_547 ?
O2 Ni1 N3 170.1(10) . . ?
N1 Ni1 N3 98.5(10) . . ?
O40 Ni1 N3 88.0(10) 4_547 . ?
O2 Ni1 N4 91.3(9) . . ?
N1 Ni1 N4 174.7(9) . . ?
O40 Ni1 N4 91.2(9) 4_547 . ?
N3 Ni1 N4 79.1(11) . . ?
O2 Ni1 N2 90.7(8) . . ?
N1 Ni1 N2 78.4(9) . . ?
O40 Ni1 N2 171.9(9) 4_547 . ?
N3 Ni1 N2 93.1(10) . . ?
N4 Ni1 N2 96.9(10) . . ?
O26 As6 O22 99.5(10) . . ?
O26 As6 O42 97.4(9) . . ?
O22 As6 O42 97.7(9) . . ?
O5 As4 O39 99.8(9) . . ?
O5 As4 O1 96.6(10) . . ?
O39 As4 O1 97.5(9) . . ?
N6 Ni2 N8 87.9(11) . . ?
N6 Ni2 N5 79.5(12) . . ?
N8 Ni2 N5 97.3(11) . . ?
N6 Ni2 N7 96.0(11) . . ?
N8 Ni2 N7 80.4(10) . . ?
N5 Ni2 N7 175.0(11) . . ?
N6 Ni2 O17 170.0(11) . . ?
N8 Ni2 O17 95.1(9) . . ?
N5 Ni2 O17 90.7(11) . . ?
N7 Ni2 O17 93.9(10) . . ?
N6 Ni2 O28 85.8(10) . 1_455 ?
N8 Ni2 O28 168.1(9) . 1_455 ?
N5 Ni2 O28 91.4(10) . 1_455 ?
N7 Ni2 O28 90.3(9) . 1_455 ?
O17 Ni2 O28 92.8(8) . 1_455 ?
O29 As5 O23 97.2(9) . . ?
O29 As5 O22 100.8(9) . . ?
O23 As5 O22 97.9(9) . . ?
O37 V11 O42 108.2(11) . . ?
O37 V11 O39 108.6(11) . . ?
O42 V11 O39 77.4(8) . . ?
O37 V11 O16 109.3(11) . . ?
O42 V11 O16 142.4(8) . . ?
O39 V11 O16 90.0(9) . . ?
O37 V11 O23 112.3(11) . . ?
O42 V11 O23 89.3(9) . . ?
O39 V11 O23 139.1(9) . . ?
O16 V11 O23 77.4(9) . . ?
O37 V11 V19 110.9(10) . . ?
O42 V11 V19 39.3(6) . . ?
O39 V11 V19 38.3(6) . . ?
O16 V11 V19 122.1(6) . . ?
O23 V11 V19 120.9(7) . . ?
O37 V11 V22 116.1(10) . . ?
O42 V11 V22 120.6(5) . . ?
O39 V11 V22 119.7(7) . . ?
O16 V11 V22 38.8(6) . . ?
O23 V11 V22 38.6(6) . . ?
V19 V11 V22 133.0(2) . . ?
O33 V12 O13 110.7(11) . . ?
O33 V12 O30 111.2(10) . . ?
O13 V12 O30 83.9(8) . . ?
O33 V12 O35 109.2(10) . . ?
O13 V12 O35 140.0(8) . . ?
O30 V12 O35 80.3(9) . . ?
O33 V12 O21 109.0(10) . . ?
O13 V12 O21 80.3(7) . . ?
O30 V12 O21 139.7(8) . . ?
O35 V12 O21 88.7(8) . . ?
O33 V12 V19 114.6(9) . . ?
O13 V12 V19 42.3(5) . . ?
O30 V12 V19 41.9(6) . . ?
O35 V12 V19 116.1(7) . . ?
O21 V12 V19 116.4(5) . . ?
O33 V12 V16 113.8(8) . . ?
O13 V12 V16 116.3(6) . . ?
O30 V12 V16 38.6(6) . . ?
O35 V12 V16 41.9(7) . . ?
O21 V12 V16 122.3(6) . . ?
V19 V12 V16 78.05(19) . . ?
O33 V12 V13 113.7(8) . . ?
O13 V12 V13 38.6(5) . . ?
O30 V12 V13 116.0(6) . . ?
O35 V12 V13 122.1(6) . . ?
O21 V12 V13 41.8(5) . . ?
V19 V12 V13 78.39(18) . . ?
V16 V12 V13 132.3(2) . . ?
O11 V13 O25 113.1(9) . . ?
O11 V13 O13 109.1(9) . . ?
O25 V13 O13 137.8(8) . . ?
O11 V13 O1 105.6(9) . . ?
O25 V13 O1 77.7(7) . . ?
O13 V13 O1 90.6(7) . . ?
O11 V13 O21 107.7(9) . . ?
O25 V13 O21 89.1(7) . . ?
O13 V13 O21 78.8(7) . . ?
O1 V13 O21 146.7(8) . . ?
O11 V13 V14 111.9(8) . . ?
O25 V13 V14 37.2(5) . . ?
O13 V13 V14 122.5(6) . . ?
O1 V13 V14 40.7(5) . . ?
O21 V13 V14 122.3(5) . . ?
O11 V13 V12 111.5(8) . . ?
O25 V13 V12 121.1(5) . . ?
O13 V13 V12 37.8(5) . . ?
O1 V13 V12 123.5(5) . . ?
O21 V13 V12 41.2(5) . . ?
V14 V13 V12 136.6(2) . . ?
O2 V14 O25 111.9(8) . . ?
O2 V14 O27 112.5(9) . . ?
O25 V14 O27 82.5(8) . . ?
O2 V14 O1 105.9(9) . . ?
O25 V14 O1 80.1(8) . . ?
O27 V14 O1 141.4(8) . . ?
O2 V14 O12 110.1(8) . . ?
O25 V14 O12 138.0(8) . . ?
O27 V14 O12 80.6(8) . . ?
O1 V14 O12 89.7(8) . . ?
O2 V14 V17 114.0(7) . . ?
O25 V14 V17 41.8(6) . . ?
O27 V14 V17 41.5(6) . . ?
O1 V14 V17 117.8(5) . . ?
O12 V14 V17 116.6(6) . . ?
O2 V14 V24 114.6(7) . . ?
O25 V14 V24 115.9(6) . . ?
O27 V14 V24 40.0(6) . . ?
O1 V14 V24 123.6(6) . . ?
O12 V14 V24 40.9(6) . . ?
V17 V14 V24 79.42(19) . . ?
O2 V14 V13 111.7(7) . . ?
O25 V14 V13 38.9(6) . . ?
O27 V14 V13 116.3(6) . . ?
O1 V14 V13 41.4(5) . . ?
O12 V14 V13 122.3(6) . . ?
V17 V14 V13 79.33(18) . . ?
V24 V14 V13 133.6(2) . . ?
O17 V15 O20 112.1(10) . . ?
O17 V15 O24 109.6(11) . . ?
O20 V15 O24 83.5(9) . . ?
O17 V15 O4 104.3(11) . . ?
O20 V15 O4 89.3(8) . . ?
O24 V15 O4 145.6(8) . . ?
O17 V15 O9 105.2(11) . . ?
O20 V15 O9 142.3(8) . . ?
O24 V15 O9 89.3(9) . . ?
O4 V15 O9 76.1(8) . . ?
O17 V15 V23 114.1(10) . . ?
O20 V15 V23 41.6(6) . . ?
O24 V15 V23 42.3(6) . . ?
O4 V15 V23 125.7(6) . . ?
O9 V15 V23 124.8(6) . . ?
O17 V15 V20 108.0(10) . . ?
O20 V15 V20 120.8(7) . . ?
O24 V15 V20 120.9(6) . . ?
O4 V15 V20 38.9(5) . . ?
O9 V15 V20 37.3(6) . . ?
V23 V15 V20 137.9(2) . . ?
O38 V16 O20 108.7(10) . . ?
O38 V16 O30 113.5(10) . . ?
O20 V16 O30 137.8(8) . . ?
O38 V16 O35 104.1(11) . . ?
O20 V16 O35 89.7(8) . . ?
O30 V16 O35 80.4(8) . . ?
O38 V16 O26 108.6(12) . . ?
O20 V16 O26 79.5(8) . . ?
O30 V16 O26 87.1(8) . . ?
O35 V16 O26 147.4(8) . . ?
O38 V16 V12 111.9(9) . . ?
O20 V16 V12 121.7(6) . . ?
O30 V16 V12 39.4(6) . . ?
O35 V16 V12 41.2(6) . . ?
O26 V16 V12 122.3(6) . . ?
O38 V16 V23 110.9(9) . . ?
O20 V16 V23 38.2(6) . . ?
O30 V16 V23 120.5(6) . . ?
O35 V16 V23 123.8(6) . . ?
O26 V16 V23 41.7(6) . . ?
V12 V16 V23 137.1(2) . . ?
O10 V17 O27 110.2(10) . . ?
O10 V17 O25 112.8(10) . . ?
O27 V17 O25 82.6(8) . . ?
O10 V17 O18 107.8(10) . . ?
O27 V17 O18 141.4(8) . . ?
O25 V17 O18 88.8(8) . . ?
O10 V17 O14 105.3(10) . . ?
O27 V17 O14 88.1(8) . . ?
O25 V17 O14 141.7(8) . . ?
O18 V17 O14 75.7(8) . . ?
O10 V17 V14 113.0(9) . . ?
O27 V17 V14 42.5(6) . . ?
O25 V17 V14 40.8(5) . . ?
O18 V17 V14 124.1(6) . . ?
O14 V17 V14 124.9(6) . . ?
O10 V17 V20 112.4(9) . . ?
O27 V17 V20 117.5(6) . . ?
O25 V17 V20 118.0(6) . . ?
O18 V17 V20 37.8(6) . . ?
O14 V17 V20 38.0(5) . . ?
V14 V17 V20 134.5(2) . . ?
O40 V18 O7 110.0(9) . . ?
O40 V18 O34 110.9(10) . . ?
O7 V18 O34 83.2(9) . . ?
O40 V18 O3 110.3(9) . . ?
O7 V18 O3 80.9(8) . . ?
O34 V18 O3 138.8(8) . . ?
O40 V18 O15 107.8(9) . . ?
O7 V18 O15 142.0(8) . . ?
O34 V18 O15 80.2(8) . . ?
O3 V18 O15 89.5(8) . . ?
O40 V18 V22 113.1(7) . . ?
O7 V18 V22 41.6(6) . . ?
O34 V18 V22 42.0(6) . . ?
O3 V18 V22 116.4(6) . . ?
O15 V18 V22 117.4(5) . . ?
O40 V18 V24 112.6(8) . . ?
O7 V18 V24 39.4(6) . . ?
O34 V18 V24 116.5(6) . . ?
O3 V18 V24 41.9(5) . . ?
O15 V18 V24 124.7(6) . . ?
V22 V18 V24 78.83(19) . . ?
O40 V18 V21 113.6(8) . . ?
O7 V18 V21 116.2(6) . . ?
O34 V18 V21 38.8(6) . . ?
O3 V18 V21 121.6(6) . . ?
O15 V18 V21 41.5(5) . . ?
V22 V18 V21 78.74(19) . . ?
V24 V18 V21 133.5(2) . . ?
O28 V19 O30 113.1(10) . . ?
O28 V19 O13 108.1(10) . . ?
O30 V19 O13 85.3(8) . . ?
O28 V19 O39 105.0(10) . . ?
O30 V19 O39 141.6(8) . . ?
O13 V19 O39 87.3(8) . . ?
O28 V19 O42 107.4(10) . . ?
O30 V19 O42 87.4(8) . . ?
O13 V19 O42 143.7(8) . . ?
O39 V19 O42 76.8(8) . . ?
O28 V19 V12 114.2(8) . . ?
O30 V19 V12 43.5(6) . . ?
O13 V19 V12 42.1(5) . . ?
O39 V19 V12 122.5(7) . . ?
O42 V19 V12 124.5(6) . . ?
O28 V19 V11 108.0(8) . . ?
O30 V19 V11 120.0(6) . . ?
O13 V19 V11 120.8(6) . . ?
O39 V19 V11 38.5(6) . . ?
O42 V19 V11 38.5(6) . . ?
V12 V19 V11 137.7(2) . . ?
O6 V20 O9 105.8(10) . . ?
O6 V20 O18 111.4(10) . . ?
O9 V20 O18 142.8(9) . . ?
O6 V20 O14 107.9(9) . . ?
O9 V20 O14 91.9(8) . . ?
O18 V20 O14 78.8(8) . . ?
O6 V20 O4 106.2(9) . . ?
O9 V20 O4 76.4(9) . . ?
O18 V20 O4 91.3(8) . . ?
O14 V20 O4 145.8(8) . . ?
O6 V20 V15 109.7(8) . . ?
O9 V20 V15 38.2(6) . . ?
O18 V20 V15 121.9(6) . . ?
O14 V20 V15 123.7(6) . . ?
O4 V20 V15 38.1(6) . . ?
O6 V20 V17 117.2(8) . . ?
O9 V20 V17 121.5(6) . . ?
O18 V20 V17 39.4(6) . . ?
O14 V20 V17 39.5(6) . . ?
O4 V20 V17 122.4(6) . . ?
V15 V20 V17 133.1(2) . . ?
O8 V21 O24 109.1(11) . . ?
O8 V21 O34 113.5(11) . . ?
O24 V21 O34 137.4(8) . . ?
O8 V21 O29 106.7(11) . . ?
O24 V21 O29 79.4(9) . . ?
O34 V21 O29 89.0(8) . . ?
O8 V21 O15 106.1(10) . . ?
O24 V21 O15 89.0(8) . . ?
O34 V21 O15 78.8(8) . . ?
O29 V21 O15 147.2(8) . . ?
O8 V21 V23 110.2(9) . . ?
O24 V21 V23 38.8(7) . . ?
O34 V21 V23 121.0(6) . . ?
O29 V21 V23 40.8(6) . . ?
O15 V21 V23 123.6(6) . . ?
O8 V21 V18 114.2(9) . . ?
O24 V21 V18 121.0(6) . . ?
O34 V21 V18 36.9(6) . . ?
O29 V21 V18 121.4(6) . . ?
O15 V21 V18 42.0(5) . . ?
V23 V21 V18 135.6(2) . . ?
O31 V22 O7 108.9(11) . . ?
O31 V22 O34 110.4(11) . . ?
O7 V22 O34 80.5(8) . . ?
O31 V22 O23 109.5(12) . . ?
O7 V22 O23 141.6(8) . . ?
O34 V22 O23 88.6(8) . . ?
O31 V22 O16 106.4(11) . . ?
O7 V22 O16 89.3(8) . . ?
O34 V22 O16 143.1(9) . . ?
O23 V22 O16 77.6(8) . . ?
O31 V22 V18 111.6(9) . . ?
O7 V22 V18 40.2(6) . . ?
O34 V22 V18 40.7(6) . . ?
O23 V22 V18 123.1(6) . . ?
O16 V22 V18 123.9(6) . . ?
O31 V22 V11 112.3(9) . . ?
O7 V22 V11 120.4(6) . . ?
O34 V22 V11 120.5(6) . . ?
O23 V22 V11 38.8(6) . . ?
O16 V22 V11 38.8(6) . . ?
V18 V22 V11 136.1(2) . . ?
O32 V23 O20 111.2(12) . . ?
O32 V23 O24 110.2(10) . . ?
O20 V23 O24 82.6(8) . . ?
O32 V23 O29 110.4(12) . . ?
O20 V23 O29 138.0(8) . . ?
O24 V23 O29 77.7(8) . . ?
O32 V23 O26 108.7(10) . . ?
O20 V23 O26 80.3(9) . . ?
O24 V23 O26 140.9(9) . . ?
O29 V23 O26 92.1(9) . . ?
O32 V23 V15 113.7(9) . . ?
O20 V23 V15 40.6(5) . . ?
O24 V23 V15 42.4(6) . . ?
O29 V23 V15 114.1(6) . . ?
O26 V23 V15 115.8(7) . . ?
O32 V23 V21 113.2(10) . . ?
O20 V23 V21 114.7(6) . . ?
O24 V23 V21 38.1(6) . . ?
O29 V23 V21 39.9(5) . . ?
O26 V23 V21 124.4(7) . . ?
V15 V23 V21 78.10(19) . . ?
O32 V23 V16 112.9(10) . . ?
O20 V23 V16 38.2(5) . . ?
O24 V23 V16 115.7(6) . . ?
O29 V23 V16 124.8(6) . . ?
O26 V23 V16 42.4(7) . . ?
V15 V23 V16 77.0(2) . . ?
V21 V23 V16 133.3(2) . . ?
O36 V24 O27 110.5(12) . . ?
O36 V24 O7 110.5(12) . . ?
O27 V24 O7 139.0(8) . . ?
O36 V24 O12 108.8(11) . . ?
O27 V24 O12 80.8(8) . . ?
O7 V24 O12 88.9(8) . . ?
O36 V24 O3 107.5(11) . . ?
O27 V24 O3 87.8(8) . . ?
O7 V24 O3 77.4(8) . . ?
O12 V24 O3 143.7(8) . . ?
O36 V24 V14 112.3(10) . . ?
O27 V24 V14 39.1(6) . . ?
O7 V24 V14 122.6(5) . . ?
O12 V24 V14 42.0(6) . . ?
O3 V24 V14 121.6(6) . . ?
O36 V24 V18 110.7(10) . . ?
O27 V24 V18 121.5(5) . . ?
O7 V24 V18 36.9(6) . . ?
O12 V24 V18 121.2(6) . . ?
O3 V24 V18 40.9(5) . . ?
V14 V24 V18 136.9(2) . . ?
As2 O15 V21 124.5(10) . . ?
As2 O15 V18 137.2(10) . . ?
V21 O15 V18 96.5(8) . . ?
As1 O14 V20 134.6(10) . . ?
As1 O14 V17 122.7(9) . . ?
V20 O14 V17 102.6(9) . . ?
V12 O13 V19 95.6(8) . . ?
V12 O13 V13 103.6(8) . . ?
V19 O13 V13 147.4(10) . . ?
As3 O12 V24 126.5(11) . . ?
As3 O12 V14 136.4(11) . . ?
V24 O12 V14 97.1(9) . . ?
As2 O9 V20 135.0(11) . . ?
As2 O9 V15 119.8(10) . . ?
V20 O9 V15 104.5(10) . . ?
V18 O7 V22 98.2(9) . . ?
V18 O7 V24 103.7(9) . . ?
V22 O7 V24 147.5(10) . . ?
As4 O5 As3 133.2(11) . . ?
As8 O4 V15 123.1(10) . . ?
As8 O4 V20 133.9(12) . . ?
V15 O4 V20 103.0(9) . . ?
As1 O3 V18 139.9(11) . . ?
As1 O3 V24 122.9(10) . . ?
V18 O3 V24 97.2(8) . . ?
V14 O2 Ni1 168.5(12) . . ?
As4 O1 V14 140.1(11) . . ?
As4 O1 V13 121.3(10) . . ?
V14 O1 V13 97.8(8) . . ?
V19 O30 V16 149.6(11) . . ?
V19 O30 V12 94.6(9) . . ?
V16 O30 V12 102.0(9) . . ?
As5 O29 V21 126.1(12) . . ?
As5 O29 V23 134.4(11) . . ?
V21 O29 V23 99.3(8) . . ?
V19 O28 Ni2 160.0(13) . 1_655 ?
V17 O27 V14 96.0(9) . . ?
V17 O27 V24 151.3(10) . . ?
V14 O27 V24 100.9(8) . . ?
As6 O26 V23 138.4(13) . . ?
As6 O26 V16 125.2(12) . . ?
V23 O26 V16 96.0(9) . . ?
V14 O25 V17 97.3(9) . . ?
V14 O25 V13 103.9(8) . . ?
V17 O25 V13 151.1(10) . . ?
V21 O24 V23 103.1(10) . . ?
V21 O24 V15 148.6(11) . . ?
V23 O24 V15 95.3(9) . . ?
As5 O23 V22 122.8(10) . . ?
As5 O23 V11 134.1(12) . . ?
V22 O23 V11 102.6(10) . . ?
As6 O22 As5 133.1(12) . . ?
As7 O21 V12 139.5(10) . . ?
As7 O21 V13 123.1(10) . . ?
V12 O21 V13 97.0(7) . . ?
V15 O20 V23 97.8(9) . . ?
V15 O20 V16 149.0(12) . . ?
V23 O20 V16 103.6(8) . . ?
As1 O19 As2 132.9(12) . . ?
As7 O18 V20 136.4(11) . . ?
As7 O18 V17 120.7(10) . . ?
V20 O18 V17 102.9(9) . . ?
V15 O17 Ni2 164.4(14) . . ?
As3 O16 V11 133.8(11) . . ?
As3 O16 V22 123.8(11) . . ?
V11 O16 V22 102.4(9) . . ?
As6 O42 V11 135.3(12) . . ?
As6 O42 V19 121.7(11) . . ?
V11 O42 V19 102.2(8) . . ?
As8 O41 As7 133.1(12) . . ?
V18 O40 Ni1 164.1(13) . 4_447 ?
As4 O39 V19 122.0(10) . . ?
As4 O39 V11 132.9(11) . . ?
V19 O39 V11 103.2(10) . . ?
As8 O35 V12 139.8(13) . . ?
As8 O35 V16 122.9(11) . . ?
V12 O35 V16 97.0(9) . . ?
V18 O34 V22 97.3(9) . . ?
V18 O34 V21 104.3(10) . . ?
V22 O34 V21 148.0(11) . . ?
C2 C1 N1 120.0 . . ?
C3 C2 C1 120.0 . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C4 C5 N1 120.0 . . ?
C4 C5 C6 126.6(18) . . ?
N1 C5 C6 113.3(18) . . ?
C5 N1 C1 120.0 . . ?
C5 N1 Ni1 117.8(12) . . ?
C1 N1 Ni1 122.2(12) . . ?
C6 N2 C10 120.0 . . ?
C6 N2 Ni1 114.2(14) . . ?
C10 N2 Ni1 125.8(14) . . ?
C7 C6 N2 120.0 . . ?
C7 C6 C5 124.0(18) . . ?
N2 C6 C5 115.9(18) . . ?
C6 C7 C8 120.0 . . ?
C9 C8 C7 120.0 . . ?
C10 C9 C8 120.0 . . ?
C9 C10 N2 120.0 . . ?
N3 C11 C12 116(4) . . ?
C13 C12 C11 122(4) . . ?
C14 C13 C12 121(4) . . ?
C13 C14 C15 114(4) . . ?
N3 C15 C14 127(3) . . ?
N3 C15 C16 114(3) . . ?
C14 C15 C16 120(3) . . ?
N4 C16 C17 125(4) . . ?
N4 C16 C15 116(3) . . ?
C17 C16 C15 118(3) . . ?
C16 C17 C18 115(5) . . ?
C17 C18 C19 117(4) . . ?
C20 C19 C18 118(4) . . ?
C19 C20 N4 126(4) . . ?
N5 C21 C22 126(5) . . ?
C23 C22 C21 117(5) . . ?
C22 C23 C24 123(6) . . ?
C23 C24 C25 112(5) . . ?
N5 C25 C24 125(4) . . ?
N5 C25 C26 116(3) . . ?
C24 C25 C26 119(4) . . ?
N6 C26 C27 124(4) . . ?
N6 C26 C25 112(3) . . ?
C27 C26 C25 123(4) . . ?
C28 C27 C26 117(4) . . ?
C29 C28 C27 126(5) . . ?
C28 C29 C30 114(5) . . ?
N6 C30 C29 123(4) . . ?
N7 C31 C32 124(4) . . ?
C33 C32 C31 124(4) . . ?
C32 C33 C34 116(4) . . ?
C35 C34 C42 118(5) . . ?
C35 C34 C33 125(4) . . ?
C42 C34 C33 118(3) . . ?
C34 C35 C36 125(5) . . ?
C37 C36 C35 113(4) . . ?
C38 C37 C41 119(3) . . ?
C38 C37 C36 122(4) . . ?
C41 C37 C36 119(4) . . ?
C39 C38 C37 121(3) . . ?
C38 C39 C40 116(3) . . ?
N8 C40 C39 124(3) . . ?
N8 C41 C37 122(3) . . ?
N8 C41 C42 115(3) . . ?
C37 C41 C42 123(3) . . ?
N7 C42 C34 120(3) . . ?
N7 C42 C41 119(3) . . ?
C34 C42 C41 120(3) . . ?
C15 N3 C11 120(3) . . ?
C15 N3 Ni1 116(2) . . ?
C11 N3 Ni1 124(3) . . ?
C16 N4 C20 118(3) . . ?
C16 N4 Ni1 115(2) . . ?
C20 N4 Ni1 127(2) . . ?
C21 N5 C25 115(3) . . ?
C21 N5 Ni2 130(3) . . ?
C25 N5 Ni2 115(2) . . ?
C30 N6 C26 117(3) . . ?
C30 N6 Ni2 126(3) . . ?
C26 N6 Ni2 117(2) . . ?
C31 N7 C42 117(3) . . ?
C31 N7 Ni2 131(2) . . ?
C42 N7 Ni2 111.9(19) . . ?
C40 N8 C41 116(3) . . ?
C40 N8 Ni2 131(2) . . ?
C41 N8 Ni2 112.5(19) . . ?

_refine_diff_density_max         1.656
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.267

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

data_shelx_3
_database_code_depnum_ccdc_archive 'CCDC 1424798'
_audit_update_record             
;
2015-09-16 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_shelx_3             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1w Check
RESPONSE: The hydrogens of the water molecule was not added.
;

_vrf_PLAT341_shelx_3             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0192 Ang
RESPONSE: The quality of this crystal was poor.
;

_vrf_PLAT430_shelx               
;
PROBLEM: Short Inter D...A Contact O2w .. O6 .. 2.83 Ang.
RESPONSE: There should be a strong hydrogen bond between the
two atoms.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C52 H58 As8 N16 Ni2 O49 V14'
_chemical_formula_weight         3121.08

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_H-M_alt        'I 41/a'
_space_group_name_Hall           '-I 4ad'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_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                   15.5647(10)
_cell_length_b                   15.5647(10)
_cell_length_c                   38.904(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9424.8(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4243
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      22.59

_exptl_crystal_description       octahedron
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.200
_exptl_crystal_F_000             6064
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.015
_exptl_absorpt_coefficient_mu    4.594
_shelx_estimated_absorpt_T_min   0.289
_shelx_estimated_absorpt_T_max   0.934
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29809
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_theta_min         2.044
_diffrn_reflns_theta_max         28.265
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5835
_reflns_number_gt                2882
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1464P)²+79.0246P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5835
_refine_ls_number_parameters     296
_refine_ls_number_restraints     20
_refine_ls_R_factor_all          0.1694
_refine_ls_R_factor_gt           0.0809
_refine_ls_wR_factor_ref         0.2892
_refine_ls_wR_factor_gt          0.2220
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.78150(9) 0.25943(9) 0.04493(3) 0.0721(5) Uani 1 1 d . . . . .
As2 As 0.81205(8) 0.13926(9) 0.20488(3) 0.0707(4) Uani 1 1 d . . . . .
Ni1 Ni 1.0000 -0.2500 0.28475(6) 0.0611(5) Uani 1 2 d S TU P . .
V4 V 0.84155(12) 0.34385(13) 0.18830(5) 0.0635(6) Uani 1 1 d . . . . .
V5 V 1.0000 0.2500 0.22037(6) 0.0654(8) Uani 1 2 d S T P . .
V6 V 0.75729(12) 0.18719(12) 0.12485(5) 0.0597(5) Uani 1 1 d . . . . .
V7 V 0.78071(12) 0.37886(12) 0.11994(5) 0.0608(5) Uani 1 1 d . . . . .
O11 O 0.8589(5) 0.4295(5) 0.15306(19) 0.0615(19) Uani 1 1 d . . . . .
O10 O 0.7728(5) 0.2870(5) 0.15345(18) 0.0612(19) Uani 1 1 d . . . . .
O9 O 0.7727(5) 0.2789(5) 0.08932(19) 0.066(2) Uani 1 1 d . . . . .
O8 O 0.8818(5) 0.2292(6) 0.2045(2) 0.074(2) Uani 1 1 d . . . . .
O7 O 0.8862(6) 0.0611(6) 0.2195(2) 0.085(3) Uani 1 1 d . . . . .
O6 O 0.6592(5) 0.1617(6) 0.1249(3) 0.090(3) Uani 1 1 d . . . . .
O5 O 0.8139(4) 0.1164(5) 0.16050(19) 0.0597(19) Uani 1 1 d . . . . .
O4 O 1.0000 0.2500 0.2612(3) 0.094(4) Uani 1 2 d S T P . .
O3 O 0.6906(6) 0.4292(6) 0.1185(3) 0.087(3) Uani 1 1 d . . . . .
O2 O 1.0381(5) 0.1356(5) 0.20531(18) 0.071(2) Uani 1 1 d . . . . .
N3 N 1.0845(5) -0.3006(6) 0.3197(3) 0.082(3) Uani 1 1 d G . . . .
C11 C 1.1532(7) -0.2586(7) 0.3351(3) 0.125(7) Uani 1 1 d G . . . .
H11A H 1.1565 -0.1990 0.3345 0.151 Uiso 1 1 calc R U . . .
C12 C 1.2171(7) -0.3058(12) 0.3515(4) 0.234(17) Uani 1 1 d G . . . .
H12A H 1.2631 -0.2777 0.3618 0.281 Uiso 1 1 calc R U . . .
C13 C 1.2122(8) -0.3949(12) 0.3524(5) 0.256(15) Uani 1 1 d G U . . .
H13A H 1.2550 -0.4265 0.3633 0.307 Uiso 1 1 calc R U . . .
C14 C 1.1435(9) -0.4369(7) 0.3369(5) 0.220(15) Uani 1 1 d G U . . .
H14A H 1.1403 -0.4965 0.3375 0.264 Uiso 1 1 calc R U . . .
C15 C 1.0796(7) -0.3897(6) 0.3206(3) 0.113(6) Uani 1 1 d G . . . .
O1 O 0.7787(6) 0.3798(7) 0.2161(2) 0.094(3) Uani 1 1 d . . . . .
N2 N 1.0785(7) -0.2884(8) 0.2438(3) 0.084(3) Uani 1 1 d . . . . .
N1 N 1.0443(6) -0.1286(5) 0.2880(2) 0.080(3) Uani 1 1 d G . . . .
C1 C 0.9920(5) -0.0702(6) 0.3051(3) 0.106(6) Uani 1 1 d G . . . .
C2 C 1.0137(7) 0.0164(6) 0.3058(3) 0.120(6) Uani 1 1 d G U . . .
H2A H 0.9787 0.0554 0.3173 0.144 Uiso 1 1 calc R U . . .
C3 C 1.0879(8) 0.0446(5) 0.2894(3) 0.121(6) Uani 1 1 d G U . . .
H3A H 1.1024 0.1026 0.2899 0.145 Uiso 1 1 calc R U . . .
C4 C 1.1402(7) -0.0137(8) 0.2723(3) 0.141(7) Uani 1 1 d G U . . .
H4A H 1.1898 0.0052 0.2613 0.169 Uiso 1 1 calc R U . . .
C5 C 1.1185(6) -0.1003(7) 0.2716(3) 0.119(7) Uani 1 1 d G . . . .
H5A H 1.1535 -0.1393 0.2601 0.143 Uiso 1 1 calc R U . . .
O1W O 1.0000 0.2500 0.1250 0.116(7) Uani 1 4 d S T P . .
N4 N 1.0908(12) -0.3044(12) 0.1886(4) 0.119(6) Uani 1 1 d . . . . .
H4B H 1.0818 -0.3006 0.1668 0.142 Uiso 1 1 calc R U . . .
C8 C 1.1535(11) -0.3330(11) 0.2371(5) 0.105(5) Uani 1 1 d . . . . .
H8A H 1.1941 -0.3521 0.2529 0.126 Uiso 1 1 calc R U . . .
C6 C 1.0410(10) -0.2721(11) 0.2137(4) 0.100(5) Uani 1 1 d . . . . .
C7 C 1.1550(16) -0.3425(14) 0.2035(7) 0.136(8) Uani 1 1 d . . . . .
H7A H 1.1971 -0.3730 0.1918 0.164 Uiso 1 1 calc R U . . .
O3W O 1.0967(9) 0.3070(13) 0.3174(4) 0.179(7) Uani 1 1 d . . . . .
O2W O 1.0000 -0.2500 0.1260(7) 0.57(7) Uani 1 2 d S T P . .


_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 O9 1.759(7) . ?
As1 O7 1.779(10) 15_665 ?
As1 O2 1.782(7) 15_665 ?
As2 O5 1.763(7) . ?
As2 O8 1.772(7) . ?
As2 O7 1.771(11) . ?
Ni1 N1 2.016(7) . ?
Ni1 N1 2.016(7) 6_644 ?
Ni1 N3 2.048(8) 6_644 ?
Ni1 N3 2.048(8) . ?
Ni1 N2 2.095(11) 6_644 ?
Ni1 N2 2.095(11) . ?
V4 O1 1.562(8) . ?
V4 O11 1.931(8) . ?
V4 O10 1.940(7) . ?
V4 O8 1.994(10) . ?
V4 O2 2.012(8) 6_654 ?
V4 V7 2.875(3) . ?
V5 O4 1.589(12) . ?
V5 O2 1.966(9) 6_654 ?
V5 O2 1.966(9) . ?
V5 O8 1.967(8) . ?
V5 O8 1.967(8) 6_654 ?
V6 O6 1.578(9) . ?
V6 O11 1.906(7) 12_756 ?
V6 O10 1.926(7) . ?
V6 O5 1.978(8) . ?
V6 O9 2.002(9) . ?
V6 V7 3.012(3) . ?
V6 V7 3.019(3) 12_756 ?
V7 O3 1.607(9) . ?
V7 O10 1.938(8) . ?
V7 O11 1.940(8) . ?
V7 O9 1.963(7) . ?
V7 O5 1.994(8) 15_665 ?
V7 V6 3.019(3) 15_665 ?
O11 V6 1.906(7) 15_665 ?
O7 As1 1.779(10) 12_756 ?
O5 V7 1.994(8) 12_756 ?
O2 As1 1.782(7) 12_756 ?
O2 V4 2.012(8) 6_654 ?
N3 C11 1.3900 . ?
N3 C15 1.3900 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C1 1.41(3) 6_644 ?
N2 C6 1.33(2) . ?
N2 C8 1.383(19) . ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
C1 C2 1.3900 . ?
C1 C15 1.41(4) 6_644 ?
C2 C3 1.3900 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
N4 C7 1.30(3) . ?
N4 C6 1.34(2) . ?
C8 C7 1.31(3) . ?
C6 C6 1.45(4) 6_644 ?

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
O9 As1 O7 99.9(4) . 15_665 ?
O9 As1 O2 98.5(3) . 15_665 ?
O7 As1 O2 98.2(4) 15_665 15_665 ?
O5 As2 O8 98.1(3) . . ?
O5 As2 O7 99.5(4) . . ?
O8 As2 O7 98.4(4) . . ?
N1 Ni1 N1 172.8(6) . 6_644 ?
N1 Ni1 N3 79.5(4) . 6_644 ?
N1 Ni1 N3 95.7(3) 6_644 6_644 ?
N1 Ni1 N3 95.7(3) . . ?
N1 Ni1 N3 79.5(4) 6_644 . ?
N3 Ni1 N3 96.9(5) 6_644 . ?
N1 Ni1 N2 88.8(4) . 6_644 ?
N1 Ni1 N2 96.6(4) 6_644 6_644 ?
N3 Ni1 N2 91.2(4) 6_644 6_644 ?
N3 Ni1 N2 171.3(5) . 6_644 ?
N1 Ni1 N2 96.6(4) . . ?
N1 Ni1 N2 88.8(4) 6_644 . ?
N3 Ni1 N2 171.3(5) 6_644 . ?
N3 Ni1 N2 91.2(4) . . ?
N2 Ni1 N2 81.0(7) 6_644 . ?
O1 V4 O11 109.4(5) . . ?
O1 V4 O10 107.5(4) . . ?
O11 V4 O10 84.0(3) . . ?
O1 V4 O8 107.4(5) . . ?
O11 V4 O8 143.0(3) . . ?
O10 V4 O8 89.2(3) . . ?
O1 V4 O2 107.4(4) . 6_654 ?
O11 V4 O2 89.6(3) . 6_654 ?
O10 V4 O2 144.7(3) . 6_654 ?
O8 V4 O2 75.3(3) . 6_654 ?
O1 V4 V7 111.5(4) . . ?
O11 V4 V7 42.2(2) . . ?
O10 V4 V7 42.1(2) . . ?
O8 V4 V7 124.5(2) . . ?
O2 V4 V7 125.5(2) 6_654 . ?
O4 V5 O2 107.3(2) . 6_654 ?
O4 V5 O2 107.3(2) . . ?
O2 V5 O2 145.3(4) 6_654 . ?
O4 V5 O8 108.3(2) . . ?
O2 V5 O8 76.9(3) 6_654 . ?
O2 V5 O8 92.3(3) . . ?
O4 V5 O8 108.3(2) . 6_654 ?
O2 V5 O8 92.3(3) 6_654 6_654 ?
O2 V5 O8 76.9(3) . 6_654 ?
O8 V5 O8 143.4(5) . 6_654 ?
O6 V6 O11 109.8(4) . 12_756 ?
O6 V6 O10 108.9(4) . . ?
O11 V6 O10 141.3(3) 12_756 . ?
O6 V6 O5 106.9(5) . . ?
O11 V6 O5 79.2(3) 12_756 . ?
O10 V6 O5 89.3(3) . . ?
O6 V6 O9 107.2(5) . . ?
O11 V6 O9 90.0(3) 12_756 . ?
O10 V6 O9 78.9(3) . . ?
O5 V6 O9 145.9(3) . . ?
O6 V6 V7 111.5(4) . . ?
O11 V6 V7 122.3(3) 12_756 . ?
O10 V6 V7 39.0(2) . . ?
O5 V6 V7 122.8(2) . . ?
O9 V6 V7 40.1(2) . . ?
O6 V6 V7 111.4(4) . 12_756 ?
O11 V6 V7 38.7(2) 12_756 12_756 ?
O10 V6 V7 122.6(3) . 12_756 ?
O5 V6 V7 40.7(2) . 12_756 ?
O9 V6 V7 123.5(2) . 12_756 ?
V7 V6 V7 137.09(9) . 12_756 ?
O3 V7 O10 109.1(5) . . ?
O3 V7 O11 111.9(4) . . ?
O10 V7 O11 83.8(3) . . ?
O3 V7 O9 108.0(4) . . ?
O10 V7 O9 79.6(3) . . ?
O11 V7 O9 139.9(3) . . ?
O3 V7 O5 110.2(4) . 15_665 ?
O10 V7 O5 140.5(3) . 15_665 ?
O11 V7 O5 78.1(3) . 15_665 ?
O9 V7 O5 92.1(3) . 15_665 ?
O3 V7 V4 114.3(4) . . ?
O10 V7 V4 42.2(2) . . ?
O11 V7 V4 41.9(2) . . ?
O9 V7 V4 115.6(2) . . ?
O5 V7 V4 114.4(2) 15_665 . ?
O3 V7 V6 112.3(4) . . ?
O10 V7 V6 38.7(2) . . ?
O11 V7 V6 115.9(3) . . ?
O9 V7 V6 41.1(2) . . ?
O5 V7 V6 124.1(2) 15_665 . ?
V4 V7 V6 78.07(7) . . ?
O3 V7 V6 114.9(4) . 15_665 ?
O10 V7 V6 116.0(2) . 15_665 ?
O11 V7 V6 37.9(2) . 15_665 ?
O9 V7 V6 123.8(3) . 15_665 ?
O5 V7 V6 40.3(2) 15_665 15_665 ?
V4 V7 V6 77.49(7) . 15_665 ?
V6 V7 V6 132.44(9) . 15_665 ?
V6 O11 V4 148.2(4) 15_665 . ?
V6 O11 V7 103.4(4) 15_665 . ?
V4 O11 V7 95.9(3) . . ?
V6 O10 V7 102.4(3) . . ?
V6 O10 V4 147.1(5) . . ?
V7 O10 V4 95.7(3) . . ?
As1 O9 V7 136.7(5) . . ?
As1 O9 V6 124.3(4) . . ?
V7 O9 V6 98.8(3) . . ?
As2 O8 V5 134.5(5) . . ?
As2 O8 V4 121.1(5) . . ?
V5 O8 V4 104.2(3) . . ?
As2 O7 As1 132.2(5) . 12_756 ?
As2 O5 V6 124.5(4) . . ?
As2 O5 V7 136.4(4) . 12_756 ?
V6 O5 V7 98.9(3) . 12_756 ?
As1 O2 V5 134.4(5) 12_756 . ?
As1 O2 V4 122.0(5) 12_756 6_654 ?
V5 O2 V4 103.6(3) . 6_654 ?
C11 N3 C15 120.0 . . ?
C11 N3 Ni1 126.9(6) . . ?
C15 N3 Ni1 111.4(6) . . ?
N3 C11 C12 120.0 . . ?
C11 C12 C13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C14 C15 N3 120.0 . . ?
C14 C15 C1 121.7(12) . 6_644 ?
N3 C15 C1 118.2(12) . 6_644 ?
C6 N2 C8 107.5(14) . . ?
C6 N2 Ni1 111.0(10) . . ?
C8 N2 Ni1 141.2(12) . . ?
C1 N1 C5 120.0 . . ?
C1 N1 Ni1 116.2(6) . . ?
C5 N1 Ni1 123.5(6) . . ?
C2 C1 N1 120.0 . . ?
C2 C1 C15 127.8(10) . 6_644 ?
N1 C1 C15 112.2(10) . 6_644 ?
C1 C2 C3 120.0 . . ?
C4 C3 C2 120.0 . . ?
C3 C4 C5 120.0 . . ?
C4 C5 N1 120.0 . . ?
C7 N4 C6 106.9(18) . . ?
C7 C8 N2 105(2) . . ?
N2 C6 N4 108.3(17) . . ?
N2 C6 C6 118.5(9) . 6_644 ?
N4 C6 C6 133.3(12) . 6_644 ?
N4 C7 C8 112(2) . . ?

_refine_diff_density_max         1.991
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.171

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

data_shelx_4
_database_code_depnum_ccdc_archive 'CCDC 1430182'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_shelx_4             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1w Check
RESPONSE: The hydrogens of the water molecule was not added.
;

_vrf_PLAT430_shelx_4             
;
PROBLEM: Short Inter D...A Contact O3w .. O6 .. 2.78 Ang.
RESPONSE: There should be a strong hydrogen bond between the
two atoms.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C68 H58 As8 Cd2 N12 O47 V14'
_chemical_formula_weight         3332.58

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5263(9)
_cell_length_b                   15.2606(11)
_cell_length_c                   15.8895(12)
_cell_angle_alpha                106.2380(10)
_cell_angle_beta                 95.3720(10)
_cell_angle_gamma                102.4660(10)
_cell_volume                     2584.6(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5840
_cell_measurement_theta_min      2.5122
_cell_measurement_theta_max      28.2951

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.141
_exptl_crystal_F_000             1608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    4.237
_shelx_estimated_absorpt_T_min   0.569
_shelx_estimated_absorpt_T_max   0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_T_max  0.655
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16505
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.437
_diffrn_reflns_theta_max         28.352
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             12049
_reflns_number_gt                8860
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0996P)²+4.3496P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12049
_refine_ls_number_parameters     745
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1751
_refine_ls_wR_factor_gt          0.1548
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.78369(4) 0.34744(3) 0.10351(3) 0.04049(13) Uani 1 1 d . . . . .
As1 As -0.19848(9) -0.13054(8) 0.21085(7) 0.0282(2) Uani 0.5 1 d . . P . .
As2 As -0.29114(10) -0.19603(8) 0.27050(7) 0.0312(2) Uani 0.5 1 d . . P . .
As3 As 0.07540(9) -0.09273(8) 0.74327(7) 0.0277(2) Uani 0.5 1 d . . P . .
As4 As 0.06705(11) -0.21420(9) 0.64594(9) 0.0365(3) Uani 0.5 1 d . . P . .
As5 As 0.17015(11) -0.25748(8) 0.46012(9) 0.0362(3) Uani 0.5 1 d . . P . .
As6 As 0.27176(9) -0.17003(7) 0.40024(7) 0.0259(2) Uani 0.5 1 d . . P . .
As7 As -0.39350(9) -0.05514(7) 0.55327(7) 0.0244(2) Uani 0.5 1 d . . P . .
As8 As -0.39972(10) -0.15617(8) 0.45519(8) 0.0301(2) Uani 0.5 1 d . . P . .
V1 V -0.09018(16) -0.01156(13) 0.26064(12) 0.0300(4) Uani 0.5 1 d . . P . .
V2 V -0.27688(16) 0.06254(13) 0.59002(12) 0.0287(4) Uani 0.5 1 d . . P . .
V3 V -0.29773(15) -0.18094(12) 0.38566(11) 0.0243(3) Uani 0.5 1 d . . P . .
V4 V 0.07973(15) -0.21361(11) 0.53530(11) 0.0223(3) Uani 0.5 1 d . . P . .
V5 V -0.15338(10) -0.27592(7) 0.44345(7) 0.0414(3) Uani 1 1 d . . . . .
V6 V 0.13022(10) -0.05126(7) 0.27227(6) 0.0345(2) Uani 1 1 d . . . . .
V7 V -0.01759(8) -0.22907(6) 0.30117(6) 0.0300(2) Uani 1 1 d . . . . .
V8 V -0.19547(8) -0.15691(6) 0.61920(6) 0.0275(2) Uani 1 1 d . . . . .
V9 V 0.27865(8) -0.02979(6) 0.61250(6) 0.02536(19) Uani 1 1 d . . . . .
O21 O 0.2241(4) -0.1338(3) 0.5003(3) 0.0341(8) Uani 1 1 d . . . . .
O20 O 0.0657(3) 0.0623(3) 0.2922(2) 0.0338(8) Uani 1 1 d . . . . .
O19 O -0.2730(4) -0.2221(3) 0.6672(3) 0.0419(10) Uani 1 1 d . . . . .
O18 O -0.2387(4) -0.0832(3) 0.3127(3) 0.0444(10) Uani 1 1 d . . . . .
O17 O 0.3976(4) -0.0403(3) 0.6622(3) 0.0404(10) Uani 1 1 d . . . . .
O16 O -0.2541(4) -0.0431(3) 0.6331(3) 0.0397(10) Uani 1 1 d . . . . .
O15 O -0.0768(4) -0.2211(3) 0.5690(3) 0.0441(11) Uani 1 1 d . . . . .
O14 O 0.1381(3) -0.0988(3) 0.6495(3) 0.0348(9) Uani 1 1 d . . . . .
O13 O 0.0097(4) -0.2574(3) 0.4137(3) 0.0407(10) Uani 1 1 d . . . . .
O12 O 0.1311(5) -0.2875(4) 0.5595(3) 0.0561(13) Uani 1 1 d . . . . .
O11 O -0.2627(4) -0.2002(3) 0.4927(3) 0.0402(10) Uani 1 1 d . . . . .
O10 O -0.1774(4) -0.2364(3) 0.3370(3) 0.0414(10) Uani 1 1 d . . . . .
O9 O -0.1483(4) 0.1479(3) 0.6711(3) 0.0345(9) Uani 1 1 d . . . . .
O8 O -0.3208(4) -0.0480(3) 0.4645(3) 0.0406(10) Uani 1 1 d . . . . .
O7 O -0.0370(4) -0.1256(3) 0.2543(3) 0.0416(10) Uani 1 1 d . . . . .
O6 O -0.2159(5) -0.3867(3) 0.4220(3) 0.0580(14) Uani 1 1 d . . . . .
O5 O -0.0264(5) -0.3219(3) 0.2197(3) 0.0524(12) Uani 1 1 d . . . . .
O4 O 0.1832(5) -0.0704(3) 0.1813(3) 0.0518(12) Uani 1 1 d . . . . .
O3 O -0.1537(5) -0.0182(4) 0.1788(4) 0.0682(16) Uani 1 1 d . . . . .
O2 O -0.3913(5) 0.0771(4) 0.6010(4) 0.0670(14) Uani 1 1 d . U . . .
O1 O -0.4172(5) -0.2242(4) 0.3392(4) 0.0707(15) Uani 1 1 d . U . . .
N1 N 0.9328(5) 0.4080(3) 0.2288(3) 0.0383(11) Uani 1 1 d . . . . .
N5 N 0.6372(5) 0.2261(4) -0.0096(3) 0.0391(11) Uani 1 1 d . . . . .
N6 N 0.6522(6) 0.2564(4) 0.1708(3) 0.0455(13) Uani 1 1 d . . . . .
N4 N 0.6843(6) 0.4685(4) 0.1398(4) 0.0479(13) Uani 1 1 d . . . . .
N2 N 0.9317(5) 0.2638(4) 0.0839(4) 0.0475(14) Uani 1 1 d . . . . .
C6 C 1.0165(5) 0.3591(4) 0.2342(4) 0.0383(13) Uani 1 1 d . . . . .
C21 C 0.6797(6) 0.5185(4) 0.0803(4) 0.0406(14) Uani 1 1 d . . . . .
N3 N 0.8130(5) 0.4340(4) 0.0012(4) 0.0455(13) Uani 1 1 d . . . . .
C34 C 0.5510(5) 0.1736(4) 0.0207(4) 0.0373(13) Uani 1 1 d . . . . .
C33 C 0.5587(6) 0.1902(4) 0.1156(4) 0.0381(13) Uani 1 1 d . . . . .
C26 C 0.4557(6) 0.1010(5) -0.0379(4) 0.0451(15) Uani 1 1 d . . . . .
C20 C 0.6244(8) 0.4871(5) 0.2069(5) 0.058(2) Uani 1 1 d . . . . .
H20A H 0.6253 0.4526 0.2467 0.070 Uiso 1 1 calc R U . . .
C22 C 0.7447(6) 0.4981(4) 0.0072(4) 0.0421(14) Uani 1 1 d . . . . .
C5 C 1.0179(6) 0.2820(4) 0.1535(4) 0.0388(13) Uani 1 1 d . . . . .
C10 C 0.9303(7) 0.4790(5) 0.3003(4) 0.0501(16) Uani 1 1 d . . . . .
H10A H 0.8727 0.5128 0.2972 0.060 Uiso 1 1 calc R U . . .
C29 C 0.4699(6) 0.1347(5) 0.1478(5) 0.0460(15) Uani 1 1 d . . . . .
C32 C 0.6598(8) 0.2690(6) 0.2578(5) 0.061(2) Uani 1 1 d . . . . .
H32A H 0.7250 0.3143 0.2957 0.073 Uiso 1 1 calc R U . . .
C23 C 0.6309(6) 0.2064(5) -0.0975(4) 0.0456(15) Uani 1 1 d . . . . .
H23A H 0.6904 0.2421 -0.1187 0.055 Uiso 1 1 calc R U . . .
C31 C 0.5772(9) 0.2191(6) 0.2942(5) 0.065(2) Uani 1 1 d . . . . .
H31A H 0.5856 0.2316 0.3555 0.078 Uiso 1 1 calc R U . . .
C24 C 0.5418(6) 0.1364(5) -0.1589(4) 0.0497(17) Uani 1 1 d . . . . .
H24A H 0.5421 0.1256 -0.2195 0.060 Uiso 1 1 calc R U . . .
C25 C 0.4539(6) 0.0839(5) -0.1297(5) 0.0491(16) Uani 1 1 d . . . . .
H25A H 0.3927 0.0367 -0.1701 0.059 Uiso 1 1 calc R U . . .
C9 C 1.0108(8) 0.5039(7) 0.3791(5) 0.072(3) Uani 1 1 d . . . . .
H9A H 1.0067 0.5529 0.4282 0.086 Uiso 1 1 calc R U . . .
C30 C 0.4819(8) 0.1506(6) 0.2399(5) 0.058(2) Uani 1 1 d . . . . .
H30A H 0.4257 0.1151 0.2637 0.070 Uiso 1 1 calc R U . . .
C7 C 1.0988(7) 0.3824(7) 0.3099(5) 0.072(3) Uani 1 1 d . . . . .
H7A H 1.1572 0.3492 0.3123 0.087 Uiso 1 1 calc R U . . .
C14 C 0.7352(7) 0.5429(5) -0.0585(5) 0.0563(19) Uani 1 1 d . . . . .
C4 C 1.1028(7) 0.2309(6) 0.1505(5) 0.061(2) Uani 1 1 d . . . . .
H4A H 1.1619 0.2437 0.1994 0.074 Uiso 1 1 calc R U . . .
C17 C 0.6141(8) 0.5859(5) 0.0890(5) 0.0538(18) Uani 1 1 d . . . . .
C27 C 0.3660(7) 0.0482(6) -0.0012(6) 0.0590(19) Uani 1 1 d . . . . .
H27A H 0.3016 0.0022 -0.0394 0.071 Uiso 1 1 calc R U . . .
C28 C 0.3729(7) 0.0633(6) 0.0853(6) 0.059(2) Uani 1 1 d . . . . .
H28A H 0.3138 0.0272 0.1065 0.071 Uiso 1 1 calc R U . . .
C18 C 0.5552(9) 0.6050(5) 0.1619(5) 0.067(2) Uani 1 1 d . . . . .
H18A H 0.5129 0.6513 0.1704 0.080 Uiso 1 1 calc R U . . .
C11 C 0.8717(7) 0.4163(5) -0.0655(6) 0.061(2) Uani 1 1 d . . . . .
H11A H 0.9217 0.3757 -0.0671 0.074 Uiso 1 1 calc R U . . .
C1 C 0.9284(8) 0.1939(6) 0.0092(5) 0.075(3) Uani 1 1 d . . . . .
H1A H 0.8672 0.1807 -0.0385 0.089 Uiso 1 1 calc R U . . .
C13 C 0.7950(9) 0.5180(7) -0.1307(7) 0.080(3) Uani 1 1 d . . . . .
H13A H 0.7881 0.5445 -0.1764 0.096 Uiso 1 1 calc R U . . .
C19 C 0.5598(9) 0.5558(5) 0.2206(5) 0.068(2) Uani 1 1 d . . . . .
H19A H 0.5204 0.5678 0.2695 0.082 Uiso 1 1 calc R U . . .
C15 C 0.6653(9) 0.6123(6) -0.0478(6) 0.070(2) Uani 1 1 d . . . . .
H15A H 0.6591 0.6428 -0.0906 0.085 Uiso 1 1 calc R U . . .
C16 C 0.6088(8) 0.6337(5) 0.0235(6) 0.065(2) Uani 1 1 d . . . . .
H16A H 0.5663 0.6798 0.0299 0.078 Uiso 1 1 calc R U . . .
C8 C 1.0940(9) 0.4556(9) 0.3824(6) 0.102(4) Uani 1 1 d . . . . .
H8A H 1.1493 0.4716 0.4342 0.122 Uiso 1 1 calc R U . . .
C12 C 0.8627(9) 0.4556(6) -0.1343(7) 0.075(3) Uani 1 1 d . . . . .
H12A H 0.9030 0.4391 -0.1821 0.091 Uiso 1 1 calc R U . . .
C2 C 1.0121(10) 0.1413(7) 0.0008(6) 0.095(4) Uani 1 1 d . . . . .
H2A H 1.0098 0.0948 -0.0521 0.114 Uiso 1 1 calc R U . . .
C3 C 1.0981(10) 0.1593(7) 0.0722(7) 0.096(4) Uani 1 1 d . . . . .
H3A H 1.1544 0.1236 0.0689 0.116 Uiso 1 1 calc R U . . .
O2W O -0.6004(9) -0.6165(7) 0.2866(9) 0.179(6) Uani 1 1 d . . . . .
H1O2 H -0.5290 -0.6025 0.3147 0.215 Uiso 1 1 d R U . . .
H2O2 H -0.6393 -0.6663 0.2955 0.215 Uiso 1 1 d R U . . .
O1W O 0.0000 0.0000 0.5000 0.150(5) Uani 1 2 d S . P . .
O3W O -0.399(2) -0.5360(13) 0.4282(12) 0.180(11) Uani 0.5 1 d . . P . .
O4W O 0.3152(15) -0.2945(12) 0.2631(11) 0.115(6) Uani 0.5 1 d . . P . .


_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
Cd1 N1 2.328(5) . ?
Cd1 N2 2.335(5) . ?
Cd1 N4 2.346(6) . ?
Cd1 N6 2.365(6) . ?
Cd1 N3 2.369(6) . ?
Cd1 N5 2.394(5) . ?
As1 O18 1.729(4) . ?
As1 As2 1.8156(16) . ?
As1 V1 1.875(2) . ?
As1 O7 1.901(5) . ?
As1 O3 1.903(6) . ?
As2 O18 1.615(5) . ?
As2 V3 1.790(2) . ?
As2 O10 1.915(5) . ?
As2 O1 1.943(6) . ?
As3 V1 1.583(2) 2_556 ?
As3 O14 1.704(4) . ?
As3 O3 1.781(5) 2_556 ?
As3 O20 1.865(4) 2_556 ?
As3 As4 2.0320(17) . ?
As4 O14 1.758(4) . ?
As4 V4 1.780(2) . ?
As4 O12 1.836(5) . ?
As4 O15 1.931(5) . ?
As5 V4 1.746(2) . ?
As5 O21 1.761(4) . ?
As5 O12 1.831(5) . ?
As5 O13 1.927(5) . ?
As5 As6 2.0741(16) . ?
As6 V2 1.592(2) 2_556 ?
As6 O21 1.714(4) . ?
As6 O2 1.757(6) 2_556 ?
As6 O9 1.882(4) 2_556 ?
As7 O8 1.724(4) . ?
As7 As8 1.8435(15) . ?
As7 O16 1.894(4) . ?
As7 V2 1.897(2) . ?
As7 O2 1.940(6) . ?
As8 O8 1.663(4) . ?
As8 V3 1.717(2) . ?
As8 O1 1.812(6) . ?
As8 O11 1.951(5) . ?
V1 O3 1.398(5) . ?
V1 As3 1.583(2) 2_556 ?
V1 O20 1.841(4) . ?
V1 O7 1.946(4) . ?
V1 O14 2.094(4) 2_556 ?
V1 O18 2.185(5) . ?
V1 V6 2.738(2) . ?
V2 O2 1.402(6) . ?
V2 As6 1.592(2) 2_556 ?
V2 O9 1.850(4) . ?
V2 O16 1.976(4) . ?
V2 O21 2.089(4) 2_556 ?
V2 O8 2.153(5) . ?
V2 V6 2.705(2) 2_556 ?
V2 V9 3.113(2) 2_556 ?
V3 O1 1.422(6) . ?
V3 O11 1.828(5) . ?
V3 O10 1.892(4) . ?
V3 O8 2.152(5) . ?
V3 O18 2.169(5) . ?
V3 V5 2.686(2) . ?
V4 O12 1.502(5) . ?
V4 O13 1.894(4) . ?
V4 O15 1.919(4) . ?
V4 O21 2.058(4) . ?
V4 O14 2.074(4) . ?
V4 V5 2.764(2) . ?
V4 V9 3.0664(18) . ?
V5 O6 1.612(4) . ?
V5 O11 1.961(5) . ?
V5 O13 1.962(4) . ?
V5 O10 1.964(5) . ?
V5 O15 1.969(5) . ?
V5 V8 3.0215(13) . ?
V5 V7 3.0258(14) . ?
V6 O4 1.598(4) . ?
V6 O7 1.964(5) . ?
V6 O9 1.967(4) 2_556 ?
V6 O16 1.968(5) 2_556 ?
V6 O20 1.987(4) . ?
V6 V2 2.705(2) 2_556 ?
V6 V8 3.0485(13) 2_556 ?
V6 V7 3.0536(14) . ?
V7 O5 1.607(4) . ?
V7 O13 1.966(4) . ?
V7 O10 1.968(4) . ?
V7 O7 1.970(4) . ?
V7 O9 1.975(4) 2_556 ?
V8 O19 1.593(4) . ?
V8 O15 1.952(4) . ?
V8 O11 1.955(4) . ?
V8 O16 1.960(4) . ?
V8 O20 1.960(4) 2_556 ?
V8 V6 3.0486(13) 2_556 ?
V9 O17 1.579(4) . ?
V9 O8 1.954(4) 2_556 ?
V9 O14 1.966(4) . ?
V9 O21 1.967(4) . ?
V9 O18 1.974(4) 2_556 ?
V9 V2 3.113(2) 2_556 ?
O21 V2 2.089(4) 2_556 ?
O20 As3 1.866(4) 2_556 ?
O20 V8 1.960(4) 2_556 ?
O18 V9 1.974(4) 2_556 ?
O16 V6 1.968(5) 2_556 ?
O14 V1 2.094(4) 2_556 ?
O9 As6 1.882(4) 2_556 ?
O9 V6 1.967(4) 2_556 ?
O9 V7 1.975(4) 2_556 ?
O8 V9 1.954(4) 2_556 ?
O3 As3 1.781(5) 2_556 ?
O2 As6 1.757(6) 2_556 ?
N1 C10 1.340(8) . ?
N1 C6 1.351(8) . ?
N5 C23 1.336(8) . ?
N5 C34 1.349(8) . ?
N6 C32 1.333(9) . ?
N6 C33 1.345(8) . ?
N4 C20 1.321(9) . ?
N4 C21 1.375(8) . ?
N2 C5 1.338(8) . ?
N2 C1 1.347(8) . ?
C6 C7 1.370(9) . ?
C6 C5 1.483(8) . ?
C21 C17 1.387(9) . ?
C21 C22 1.437(9) . ?
N3 C11 1.308(9) . ?
N3 C22 1.371(8) . ?
C34 C26 1.416(9) . ?
C34 C33 1.449(8) . ?
C33 C29 1.411(9) . ?
C26 C25 1.406(10) . ?
C26 C27 1.440(10) . ?
C20 C19 1.393(11) . ?
C22 C14 1.407(10) . ?
C5 C4 1.372(9) . ?
C10 C9 1.391(10) . ?
C29 C30 1.403(10) . ?
C29 C28 1.444(11) . ?
C32 C31 1.362(11) . ?
C23 C24 1.380(9) . ?
C31 C30 1.366(12) . ?
C24 C25 1.353(10) . ?
C9 C8 1.336(13) . ?
C7 C8 1.378(12) . ?
C14 C13 1.398(12) . ?
C14 C15 1.446(11) . ?
C4 C3 1.394(12) . ?
C17 C18 1.390(11) . ?
C17 C16 1.432(11) . ?
C27 C28 1.320(11) . ?
C18 C19 1.355(11) . ?
C11 C12 1.392(12) . ?
C1 C2 1.376(11) . ?
C13 C12 1.347(13) . ?
C15 C16 1.355(12) . ?
C2 C3 1.357(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Cd1 N2 70.80(18) . . ?
N1 Cd1 N4 96.58(19) . . ?
N2 Cd1 N4 163.3(2) . . ?
N1 Cd1 N6 93.49(19) . . ?
N2 Cd1 N6 100.5(2) . . ?
N4 Cd1 N6 90.9(2) . . ?
N1 Cd1 N3 112.46(18) . . ?
N2 Cd1 N3 102.4(2) . . ?
N4 Cd1 N3 71.72(19) . . ?
N6 Cd1 N3 149.8(2) . . ?
N1 Cd1 N5 155.46(18) . . ?
N2 Cd1 N5 93.14(18) . . ?
N4 Cd1 N5 102.16(19) . . ?
N6 Cd1 N5 70.72(18) . . ?
N3 Cd1 N5 88.59(18) . . ?
O18 As1 As2 54.13(17) . . ?
O18 As1 V1 74.55(17) . . ?
As2 As1 V1 126.03(8) . . ?
O18 As1 O7 96.96(19) . . ?
As2 As1 O7 105.34(14) . . ?
V1 As1 O7 62.03(15) . . ?
O18 As1 O3 98.9(3) . . ?
As2 As1 O3 148.2(2) . . ?
V1 As1 O3 43.43(15) . . ?
O7 As1 O3 93.5(2) . . ?
O18 As2 V3 78.95(17) . . ?
O18 As2 As1 60.19(16) . . ?
V3 As2 As1 134.10(9) . . ?
O18 As2 O10 99.3(2) . . ?
V3 As2 O10 61.30(14) . . ?
As1 As2 O10 103.40(14) . . ?
O18 As2 O1 103.0(2) . . ?
V3 As2 O1 44.53(18) . . ?
As1 As2 O1 157.5(2) . . ?
O10 As2 O1 93.6(2) . . ?
V1 As3 O14 79.02(15) 2_556 . ?
V1 As3 O3 48.68(19) 2_556 2_556 ?
O14 As3 O3 105.6(3) . 2_556 ?
V1 As3 O20 63.93(14) 2_556 2_556 ?
O14 As3 O20 98.95(19) . 2_556 ?
O3 As3 O20 99.2(2) 2_556 2_556 ?
V1 As3 As4 130.50(9) 2_556 . ?
O14 As3 As4 55.29(14) . . ?
O3 As3 As4 153.1(2) 2_556 . ?
O20 As3 As4 102.29(13) 2_556 . ?
O14 As4 V4 71.77(15) . . ?
O14 As4 O12 103.1(2) . . ?
V4 As4 O12 49.07(16) . . ?
O14 As4 O15 94.34(19) . . ?
V4 As4 O15 62.11(14) . . ?
O12 As4 O15 95.9(2) . . ?
O14 As4 As3 52.85(13) . . ?
V4 As4 As3 120.66(9) . . ?
O12 As4 As3 152.12(19) . . ?
O15 As4 As3 99.52(13) . . ?
V4 As5 O21 71.89(14) . . ?
V4 As5 O12 49.60(15) . . ?
O21 As5 O12 102.7(2) . . ?
V4 As5 O13 61.86(14) . . ?
O21 As5 O13 95.44(19) . . ?
O12 As5 O13 96.0(2) . . ?
V4 As5 As6 120.25(8) . . ?
O21 As5 As6 52.33(13) . . ?
O12 As5 As6 150.9(2) . . ?
O13 As5 As6 100.64(14) . . ?
V2 As6 O21 78.29(15) 2_556 . ?
V2 As6 O2 49.2(2) 2_556 2_556 ?
O21 As6 O2 106.1(2) . 2_556 ?
V2 As6 O9 63.71(14) 2_556 2_556 ?
O21 As6 O9 97.92(18) . 2_556 ?
O2 As6 O9 99.2(2) 2_556 2_556 ?
V2 As6 As5 128.31(9) 2_556 . ?
O21 As6 As5 54.40(13) . . ?
O2 As6 As5 154.1(2) 2_556 . ?
O9 As6 As5 100.30(13) 2_556 . ?
O8 As7 As8 55.46(15) . . ?
O8 As7 O16 96.09(19) . . ?
As8 As7 O16 106.09(13) . . ?
O8 As7 V2 72.82(16) . . ?
As8 As7 V2 126.21(8) . . ?
O16 As7 V2 62.84(15) . . ?
O8 As7 O2 98.2(2) . . ?
As8 As7 O2 148.17(18) . . ?
O16 As7 O2 93.1(2) . . ?
V2 As7 O2 42.84(18) . . ?
O8 As8 V3 79.09(17) . . ?
O8 As8 O1 106.2(3) . . ?
V3 As8 O1 47.42(19) . . ?
O8 As8 As7 58.62(15) . . ?
V3 As8 As7 132.28(9) . . ?
O1 As8 As7 158.8(2) . . ?
O8 As8 O11 95.9(2) . . ?
V3 As8 O11 59.40(13) . . ?
O1 As8 O11 94.6(2) . . ?
As7 As8 O11 101.35(13) . . ?
O3 V1 As3 73.1(2) . 2_556 ?
O3 V1 O20 117.4(3) . . ?
As3 V1 O20 65.51(15) 2_556 . ?
O3 V1 As1 69.4(2) . . ?
As3 V1 As1 138.77(13) 2_556 . ?
O20 V1 As1 149.75(17) . . ?
O3 V1 O7 110.9(3) . . ?
As3 V1 O7 154.71(18) 2_556 . ?
O20 V1 O7 91.9(2) . . ?
As1 V1 O7 59.65(15) . . ?
O3 V1 O14 103.5(3) . 2_556 ?
As3 V1 O14 53.04(12) 2_556 2_556 ?
O20 V1 O14 87.02(18) . 2_556 ?
As1 V1 O14 121.26(14) . 2_556 ?
O7 V1 O14 141.47(19) . 2_556 ?
O3 V1 O18 98.5(3) . . ?
As3 V1 O18 122.64(16) 2_556 . ?
O20 V1 O18 143.15(19) . . ?
As1 V1 O18 49.68(12) . . ?
O7 V1 O18 82.15(18) . . ?
O14 V1 O18 76.14(16) 2_556 . ?
O3 V1 V6 121.0(3) . . ?
As3 V1 V6 109.89(10) 2_556 . ?
O20 V1 V6 46.52(13) . . ?
As1 V1 V6 103.70(9) . . ?
O7 V1 V6 45.83(15) . . ?
O14 V1 V6 125.53(14) 2_556 . ?
O18 V1 V6 121.53(14) . . ?
O2 V2 As6 71.6(2) . 2_556 ?
O2 V2 O9 116.3(3) . . ?
As6 V2 O9 65.82(15) 2_556 . ?
O2 V2 As7 70.2(3) . . ?
As6 V2 As7 138.15(12) 2_556 . ?
O9 V2 As7 149.65(17) . . ?
O2 V2 O16 109.8(3) . . ?
As6 V2 O16 154.91(17) 2_556 . ?
O9 V2 O16 92.9(2) . . ?
As7 V2 O16 58.50(15) . . ?
O2 V2 O21 103.5(3) . 2_556 ?
As6 V2 O21 53.47(12) 2_556 2_556 ?
O9 V2 O21 86.92(17) . 2_556 ?
As7 V2 O21 121.54(14) . 2_556 ?
O16 V2 O21 142.74(18) . 2_556 ?
O2 V2 O8 100.3(3) . . ?
As6 V2 O8 123.63(16) 2_556 . ?
O9 V2 O8 142.52(19) . . ?
As7 V2 O8 49.88(11) . . ?
O16 V2 O8 81.27(17) . . ?
O21 V2 O8 76.70(16) 2_556 . ?
O2 V2 V6 120.1(3) . 2_556 ?
As6 V2 V6 110.01(10) 2_556 2_556 ?
O9 V2 V6 46.63(13) . 2_556 ?
As7 V2 V6 103.49(9) . 2_556 ?
O16 V2 V6 46.57(14) . 2_556 ?
O21 V2 V6 125.78(13) 2_556 2_556 ?
O8 V2 V6 120.72(14) . 2_556 ?
O2 V2 V9 102.7(3) . 2_556 ?
As6 V2 V9 87.57(9) 2_556 2_556 ?
O9 V2 V9 119.78(14) . 2_556 ?
As7 V2 V9 84.68(7) . 2_556 ?
O16 V2 V9 115.58(13) . 2_556 ?
O21 V2 V9 38.47(11) 2_556 2_556 ?
O8 V2 V9 38.38(11) . 2_556 ?
V6 V2 V9 136.85(7) 2_556 2_556 ?
O1 V3 As8 69.8(2) . . ?
O1 V3 As2 73.5(3) . . ?
As8 V3 As2 135.91(12) . . ?
O1 V3 O11 116.2(3) . . ?
As8 V3 O11 66.68(15) . . ?
As2 V3 O11 155.24(18) . . ?
O1 V3 O10 115.5(3) . . ?
As8 V3 O10 158.31(18) . . ?
As2 V3 O10 62.61(16) . . ?
O11 V3 O10 93.3(2) . . ?
O1 V3 O8 100.1(3) . . ?
As8 V3 O8 49.36(12) . . ?
As2 V3 O8 117.23(14) . . ?
O11 V3 O8 84.64(18) . . ?
O10 V3 O8 140.85(18) . . ?
O1 V3 O18 99.9(3) . . ?
As8 V3 O18 117.68(14) . . ?
As2 V3 O18 46.94(12) . . ?
O11 V3 O18 141.17(19) . . ?
O10 V3 O18 82.97(19) . . ?
O8 V3 O18 75.02(16) . . ?
O1 V3 V5 123.4(3) . . ?
As8 V3 V5 111.81(9) . . ?
As2 V3 V5 108.40(8) . . ?
O11 V3 V5 46.89(14) . . ?
O10 V3 V5 46.96(15) . . ?
O8 V3 V5 123.97(13) . . ?
O18 V3 V5 122.70(13) . . ?
O12 V4 As5 68.1(2) . . ?
O12 V4 As4 67.4(2) . . ?
As5 V4 As4 133.20(11) . . ?
O12 V4 O13 110.1(3) . . ?
As5 V4 O13 63.77(15) . . ?
As4 V4 O13 148.24(16) . . ?
O12 V4 O15 109.1(3) . . ?
As5 V4 O15 148.98(16) . . ?
As4 V4 O15 62.80(16) . . ?
O13 V4 O15 90.5(2) . . ?
O12 V4 O21 102.8(2) . . ?
As5 V4 O21 54.39(12) . . ?
As4 V4 O21 124.43(14) . . ?
O13 V4 O21 87.30(17) . . ?
O15 V4 O21 146.7(2) . . ?
O12 V4 O14 102.6(2) . . ?
As5 V4 O14 125.70(14) . . ?
As4 V4 O14 53.62(12) . . ?
O13 V4 O14 146.5(2) . . ?
O15 V4 O14 85.31(17) . . ?
O21 V4 O14 78.58(16) . . ?
O12 V4 V5 115.6(2) . . ?
As5 V4 V5 106.16(8) . . ?
As4 V4 V5 105.49(8) . . ?
O13 V4 V5 45.18(13) . . ?
O15 V4 V5 45.43(14) . . ?
O21 V4 V5 125.84(13) . . ?
O14 V4 V5 124.21(13) . . ?
O12 V4 V9 105.1(2) . . ?
As5 V4 V9 89.46(7) . . ?
As4 V4 V9 88.40(7) . . ?
O13 V4 V9 121.38(14) . . ?
O15 V4 V9 119.97(14) . . ?
O21 V4 V9 39.29(11) . . ?
O14 V4 V9 39.33(11) . . ?
V5 V4 V9 139.32(7) . . ?
O6 V5 O11 110.4(2) . . ?
O6 V5 O13 110.5(2) . . ?
O11 V5 O13 139.08(18) . . ?
O6 V5 O10 110.6(2) . . ?
O11 V5 O10 87.16(18) . . ?
O13 V5 O10 79.19(18) . . ?
O6 V5 O15 110.1(2) . . ?
O11 V5 O15 78.56(17) . . ?
O13 V5 O15 87.05(17) . . ?
O10 V5 O15 139.24(19) . . ?
O6 V5 V3 113.6(2) . . ?
O11 V5 V3 42.91(13) . . ?
O13 V5 V3 117.30(14) . . ?
O10 V5 V3 44.77(12) . . ?
O15 V5 V3 115.43(14) . . ?
O6 V5 V4 115.9(2) . . ?
O11 V5 V4 114.67(12) . . ?
O13 V5 V4 43.24(12) . . ?
O10 V5 V4 114.67(13) . . ?
O15 V5 V4 43.96(12) . . ?
V3 V5 V4 130.50(6) . . ?
O6 V5 V8 112.96(18) . . ?
O11 V5 V8 39.44(12) . . ?
O13 V5 V8 119.53(12) . . ?
O10 V5 V8 119.70(13) . . ?
O15 V5 V8 39.40(12) . . ?
V3 V5 V8 80.01(5) . . ?
V4 V5 V8 80.17(5) . . ?
O6 V5 V7 114.04(18) . . ?
O11 V5 V7 119.46(13) . . ?
O13 V5 V7 39.66(13) . . ?
O10 V5 V7 39.73(12) . . ?
O15 V5 V7 119.40(13) . . ?
V3 V5 V7 81.81(5) . . ?
V4 V5 V7 79.57(5) . . ?
V8 V5 V7 133.00(4) . . ?
O4 V6 O7 111.1(2) . . ?
O4 V6 O9 110.1(2) . 2_556 ?
O7 V6 O9 78.27(17) . 2_556 ?
O4 V6 O16 108.7(2) . 2_556 ?
O7 V6 O16 140.10(17) . 2_556 ?
O9 V6 O16 89.63(17) 2_556 2_556 ?
O4 V6 O20 110.0(2) . . ?
O7 V6 O20 87.16(17) . . ?
O9 V6 O20 139.91(16) 2_556 . ?
O16 V6 O20 78.00(16) 2_556 . ?
O4 V6 V2 113.7(2) . 2_556 ?
O7 V6 V2 114.77(13) . 2_556 ?
O9 V6 V2 43.14(12) 2_556 2_556 ?
O16 V6 V2 46.81(12) 2_556 2_556 ?
O20 V6 V2 117.30(12) . 2_556 ?
O4 V6 V1 114.3(2) . . ?
O7 V6 V1 45.28(13) . . ?
O9 V6 V1 116.92(13) 2_556 . ?
O16 V6 V1 114.42(12) 2_556 . ?
O20 V6 V1 42.26(12) . . ?
V2 V6 V1 131.93(6) 2_556 . ?
O4 V6 V8 113.00(18) . 2_556 ?
O7 V6 V8 119.04(12) . 2_556 ?
O9 V6 V8 120.74(12) 2_556 2_556 ?
O16 V6 V8 38.99(11) 2_556 2_556 ?
O20 V6 V8 39.11(11) . 2_556 ?
V2 V6 V8 82.48(5) 2_556 2_556 ?
V1 V6 V8 78.71(5) . 2_556 ?
O4 V6 V7 113.93(18) . . ?
O7 V6 V7 39.15(12) . . ?
O9 V6 V7 39.33(12) 2_556 . ?
O16 V6 V7 121.61(12) 2_556 . ?
O20 V6 V7 119.50(12) . . ?
V2 V6 V7 79.70(5) 2_556 . ?
V1 V6 V7 81.77(5) . . ?
V8 V6 V7 133.07(4) 2_556 . ?
O5 V7 O13 109.2(2) . . ?
O5 V7 O10 108.3(2) . . ?
O13 V7 O10 78.99(19) . . ?
O5 V7 O7 109.2(2) . . ?
O13 V7 O7 141.54(17) . . ?
O10 V7 O7 89.36(19) . . ?
O5 V7 O9 109.3(2) . 2_556 ?
O13 V7 O9 89.29(16) . 2_556 ?
O10 V7 O9 142.46(16) . 2_556 ?
O7 V7 O9 77.92(18) . 2_556 ?
O5 V7 V5 111.52(19) . . ?
O13 V7 V5 39.56(13) . . ?
O10 V7 V5 39.63(14) . . ?
O7 V7 V5 122.16(12) . . ?
O9 V7 V5 122.43(12) 2_556 . ?
O5 V7 V6 112.00(19) . . ?
O13 V7 V6 121.84(12) . . ?
O10 V7 V6 122.18(13) . . ?
O7 V7 V6 39.01(14) . . ?
O9 V7 V6 39.12(12) 2_556 . ?
V5 V7 V6 136.49(4) . . ?
O19 V8 O15 107.4(2) . . ?
O19 V8 O11 108.9(2) . . ?
O15 V8 O11 79.09(19) . . ?
O19 V8 O16 108.8(2) . . ?
O15 V8 O16 143.81(19) . . ?
O11 V8 O16 89.51(18) . . ?
O19 V8 O20 108.8(2) . 2_556 ?
O15 V8 O20 89.44(17) . 2_556 ?
O11 V8 O20 142.34(17) . 2_556 ?
O16 V8 O20 78.84(18) . 2_556 ?
O19 V8 V5 110.20(17) . . ?
O15 V8 V5 39.81(14) . . ?
O11 V8 V5 39.56(14) . . ?
O16 V8 V5 123.45(12) . . ?
O20 V8 V5 123.00(12) 2_556 . ?
O19 V8 V6 112.36(17) . 2_556 ?
O15 V8 V6 122.76(12) . 2_556 ?
O11 V8 V6 121.77(13) . 2_556 ?
O16 V8 V6 39.19(13) . 2_556 ?
O20 V8 V6 39.76(12) 2_556 2_556 ?
V5 V8 V6 137.43(4) . 2_556 ?
O17 V9 O8 109.3(2) . 2_556 ?
O17 V9 O14 109.4(2) . . ?
O8 V9 O14 141.29(18) 2_556 . ?
O17 V9 O21 109.2(2) . . ?
O8 V9 O21 84.36(18) 2_556 . ?
O14 V9 O21 83.40(17) . . ?
O17 V9 O18 107.6(2) . 2_556 ?
O8 V9 O18 84.1(2) 2_556 2_556 ?
O14 V9 O18 84.11(19) . 2_556 ?
O21 V9 O18 143.19(18) . 2_556 ?
O17 V9 V4 114.69(17) . . ?
O8 V9 V4 118.07(13) 2_556 . ?
O14 V9 V4 41.95(12) . . ?
O21 V9 V4 41.50(12) . . ?
O18 V9 V4 119.06(14) 2_556 . ?
O17 V9 V2 113.53(16) . 2_556 ?
O8 V9 V2 43.18(14) 2_556 2_556 ?
O14 V9 V2 117.91(13) . 2_556 ?
O21 V9 V2 41.34(12) . 2_556 ?
O18 V9 V2 120.68(14) 2_556 2_556 ?
V4 V9 V2 79.45(5) . 2_556 ?
As6 O21 As5 73.27(15) . . ?
As6 O21 V9 137.7(2) . . ?
As5 O21 V9 140.9(2) . . ?
As6 O21 V4 122.8(2) . . ?
As5 O21 V4 53.72(12) . . ?
V9 O21 V4 99.20(17) . . ?
As6 O21 V2 48.24(12) . 2_556 ?
As5 O21 V2 118.1(2) . 2_556 ?
V9 O21 V2 100.20(17) . 2_556 ?
V4 O21 V2 144.4(2) . 2_556 ?
V1 O20 As3 50.56(12) . 2_556 ?
V1 O20 V8 150.6(2) . 2_556 ?
As3 O20 V8 120.6(2) 2_556 2_556 ?
V1 O20 V6 91.21(18) . . ?
As3 O20 V6 138.1(2) 2_556 . ?
V8 O20 V6 101.13(18) 2_556 . ?
As2 O18 As1 65.68(16) . . ?
As2 O18 V9 141.7(3) . 2_556 ?
As1 O18 V9 143.0(3) . 2_556 ?
As2 O18 V3 54.11(15) . . ?
As1 O18 V3 116.4(2) . . ?
V9 O18 V3 99.61(18) 2_556 . ?
As2 O18 V1 119.1(2) . . ?
As1 O18 V1 55.77(14) . . ?
V9 O18 V1 98.0(2) 2_556 . ?
V3 O18 V1 147.1(2) . . ?
As7 O16 V8 116.3(2) . . ?
As7 O16 V6 141.7(2) . 2_556 ?
V8 O16 V6 101.82(19) . 2_556 ?
As7 O16 V2 58.66(13) . . ?
V8 O16 V2 150.0(2) . . ?
V6 O16 V2 86.62(18) 2_556 . ?
V4 O15 As4 55.09(13) . . ?
V4 O15 V8 149.1(2) . . ?
As4 O15 V8 119.1(2) . . ?
V4 O15 V5 90.61(18) . . ?
As4 O15 V5 140.1(2) . . ?
V8 O15 V5 100.8(2) . . ?
As3 O14 As4 71.86(16) . . ?
As3 O14 V9 138.4(2) . . ?
As4 O14 V9 140.2(2) . . ?
As3 O14 V4 122.3(2) . . ?
As4 O14 V4 54.61(13) . . ?
V9 O14 V4 98.72(17) . . ?
As3 O14 V1 47.93(12) . 2_556 ?
As4 O14 V1 117.0(2) . 2_556 ?
V9 O14 V1 101.43(18) . 2_556 ?
V4 O14 V1 145.6(2) . 2_556 ?
V4 O13 As5 54.37(13) . . ?
V4 O13 V5 91.58(18) . . ?
As5 O13 V5 140.3(2) . . ?
V4 O13 V7 148.0(2) . . ?
As5 O13 V7 118.9(2) . . ?
V5 O13 V7 100.8(2) . . ?
V4 O12 As5 62.26(19) . . ?
V4 O12 As4 63.52(19) . . ?
As5 O12 As4 123.9(3) . . ?
V3 O11 As8 53.92(14) . . ?
V3 O11 V8 152.8(2) . . ?
As8 O11 V8 118.0(2) . . ?
V3 O11 V5 90.21(18) . . ?
As8 O11 V5 140.9(2) . . ?
V8 O11 V5 101.0(2) . . ?
V3 O10 As2 56.09(14) . . ?
V3 O10 V5 88.27(18) . . ?
As2 O10 V5 142.0(2) . . ?
V3 O10 V7 152.4(2) . . ?
As2 O10 V7 117.1(2) . . ?
V5 O10 V7 100.6(2) . . ?
V2 O9 As6 50.48(13) . 2_556 ?
V2 O9 V6 90.24(17) . 2_556 ?
As6 O9 V6 136.7(2) 2_556 2_556 ?
V2 O9 V7 150.6(2) . 2_556 ?
As6 O9 V7 121.6(2) 2_556 2_556 ?
V6 O9 V7 101.55(19) 2_556 2_556 ?
As8 O8 As7 65.93(15) . . ?
As8 O8 V9 138.3(3) . 2_556 ?
As7 O8 V9 143.4(3) . 2_556 ?
As8 O8 V3 51.56(14) . . ?
As7 O8 V3 113.9(2) . . ?
V9 O8 V3 100.85(19) 2_556 . ?
As8 O8 V2 121.3(2) . . ?
As7 O8 V2 57.30(14) . . ?
V9 O8 V2 98.4(2) 2_556 . ?
V3 O8 V2 148.0(2) . . ?
As1 O7 V1 58.31(13) . . ?
As1 O7 V6 143.1(2) . . ?
V1 O7 V6 88.89(19) . . ?
As1 O7 V7 115.1(2) . . ?
V1 O7 V7 151.9(2) . . ?
V6 O7 V7 101.8(2) . . ?
V1 O3 As3 58.25(19) . 2_556 ?
V1 O3 As1 67.2(2) . . ?
As3 O3 As1 123.0(3) 2_556 . ?
V2 O2 As6 59.2(2) . 2_556 ?
V2 O2 As7 66.9(3) . . ?
As6 O2 As7 123.6(3) 2_556 . ?
V3 O1 As8 62.8(2) . . ?
V3 O1 As2 62.0(2) . . ?
As8 O1 As2 119.8(3) . . ?
C10 N1 C6 118.4(6) . . ?
C10 N1 Cd1 124.0(5) . . ?
C6 N1 Cd1 116.9(4) . . ?
C23 N5 C34 117.6(5) . . ?
C23 N5 Cd1 127.4(4) . . ?
C34 N5 Cd1 115.0(4) . . ?
C32 N6 C33 118.3(6) . . ?
C32 N6 Cd1 125.6(5) . . ?
C33 N6 Cd1 115.9(4) . . ?
C20 N4 C21 117.8(6) . . ?
C20 N4 Cd1 126.2(5) . . ?
C21 N4 Cd1 115.7(4) . . ?
C5 N2 C1 119.2(6) . . ?
C5 N2 Cd1 117.4(4) . . ?
C1 N2 Cd1 123.2(5) . . ?
N1 C6 C7 121.2(6) . . ?
N1 C6 C5 117.0(5) . . ?
C7 C6 C5 121.8(6) . . ?
N4 C21 C17 121.8(6) . . ?
N4 C21 C22 117.8(6) . . ?
C17 C21 C22 120.4(6) . . ?
C11 N3 C22 119.2(6) . . ?
C11 N3 Cd1 126.2(5) . . ?
C22 N3 Cd1 113.8(4) . . ?
N5 C34 C26 121.8(6) . . ?
N5 C34 C33 118.9(5) . . ?
C26 C34 C33 119.3(6) . . ?
N6 C33 C29 121.6(6) . . ?
N6 C33 C34 119.1(6) . . ?
C29 C33 C34 119.3(6) . . ?
C25 C26 C34 117.9(6) . . ?
C25 C26 C27 123.1(7) . . ?
C34 C26 C27 119.0(6) . . ?
N4 C20 C19 123.0(7) . . ?
N3 C22 C14 120.7(6) . . ?
N3 C22 C21 119.9(6) . . ?
C14 C22 C21 119.4(6) . . ?
N2 C5 C4 121.5(6) . . ?
N2 C5 C6 116.8(6) . . ?
C4 C5 C6 121.7(6) . . ?
N1 C10 C9 122.3(7) . . ?
C30 C29 C33 117.9(7) . . ?
C30 C29 C28 123.0(7) . . ?
C33 C29 C28 119.2(6) . . ?
N6 C32 C31 123.7(8) . . ?
N5 C23 C24 124.1(7) . . ?
C32 C31 C30 119.4(7) . . ?
C25 C24 C23 119.0(6) . . ?
C24 C25 C26 119.5(6) . . ?
C8 C9 C10 118.3(7) . . ?
C31 C30 C29 119.1(7) . . ?
C6 C7 C8 119.1(8) . . ?
C13 C14 C22 117.8(8) . . ?
C13 C14 C15 123.5(8) . . ?
C22 C14 C15 118.7(7) . . ?
C5 C4 C3 118.3(7) . . ?
C21 C17 C18 118.4(7) . . ?
C21 C17 C16 119.7(7) . . ?
C18 C17 C16 121.9(7) . . ?
C28 C27 C26 121.7(7) . . ?
C27 C28 C29 121.5(7) . . ?
C19 C18 C17 119.7(7) . . ?
N3 C11 C12 122.9(8) . . ?
N2 C1 C2 122.4(7) . . ?
C12 C13 C14 120.2(8) . . ?
C18 C19 C20 119.2(7) . . ?
C16 C15 C14 121.1(7) . . ?
C15 C16 C17 120.6(7) . . ?
C9 C8 C7 120.7(8) . . ?
C13 C12 C11 119.1(8) . . ?
C3 C2 C1 117.9(8) . . ?
C2 C3 C4 120.7(8) . . ?

_refine_diff_density_max         2.219
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.249

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

data_shelx_5
_database_code_depnum_ccdc_archive 'CCDC 1430183'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_shelx_5             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O3w Check
RESPONSE: The hydrogens of the water molecule was not added.
;

_vrf_PLAT342_shelx_5             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0280 Ang
RESPONSE: The quality of this crystal was poor.
;

_vrf_PLAT430_shelx_5             
;
PROBLEM: Short Inter D...A Contact O2w .. O5w .. 2.73 Ang.
RESPONSE: There should be a strong hydrogen bond between the
two atoms.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H50 As6 Cd4 N8 O55 V15'
_chemical_formula_weight         3306.20

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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.541(2)
_cell_length_b                   12.565(2)
_cell_length_c                   14.238(3)
_cell_angle_alpha                83.592(2)
_cell_angle_beta                 79.184(3)
_cell_angle_gamma                81.137(2)
_cell_volume                     2169.4(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5580
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      27.23

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.531
_exptl_crystal_F_000             1581
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    4.867
_shelx_estimated_absorpt_T_min   0.549
_shelx_estimated_absorpt_T_max   0.570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.526
_exptl_absorpt_correction_T_max  0.544
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13153
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.019
_diffrn_reflns_theta_max         27.305
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             9417
_reflns_number_gt                7956
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0003P)²+171.7019P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0024(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9417
_refine_ls_number_parameters     653
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0967
_refine_ls_wR_factor_ref         0.2426
_refine_ls_wR_factor_gt          0.2365
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.018
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
N4 N 0.7850(10) 0.8549(10) 0.2355(10) 0.029(3) Uani 1 1 d . . . . .
N3 N 0.9228(10) 0.6721(10) 0.2639(9) 0.027(3) Uani 1 1 d . . . . .
C24 C 0.8367(12) 0.6934(12) 0.3320(11) 0.026(3) Uani 1 1 d . . . . .
N1 N 1.0133(12) 1.0391(11) -0.3339(10) 0.034(3) Uani 1 1 d . . . . .
C19 C 0.6755(14) 0.8219(15) 0.3949(13) 0.039(4) Uani 1 1 d . . . . .
C23 C 0.7651(13) 0.7947(13) 0.3182(11) 0.028(3) Uani 1 1 d . . . . .
C25 C 1.0113(11) 0.9703(11) -0.0449(10) 0.021(3) Uani 1 1 d . . . . .
N2 N 1.1728(13) 0.8754(15) -0.3810(11) 0.046(4) Uani 1 1 d . . . . .
C13 C 0.9925(13) 0.5814(12) 0.2765(12) 0.030(3) Uani 1 1 d . . . . .
H13A H 1.0527 0.5660 0.2285 0.036 Uiso 1 1 calc R U . . .
C16 C 0.8156(14) 0.6227(15) 0.4183(12) 0.037(4) Uani 1 1 d . . . . .
C22 C 0.7196(14) 0.9495(14) 0.2247(13) 0.036(4) Uani 1 1 d . . . . .
H22A H 0.7342 0.9918 0.1671 0.044 Uiso 1 1 calc R U . . .
C14 C 0.9789(15) 0.5104(14) 0.3571(13) 0.038(4) Uani 1 1 d . . . . .
H14A H 1.0306 0.4500 0.3646 0.046 Uiso 1 1 calc R U . . .
C21 C 0.6345(14) 0.9879(14) 0.2908(14) 0.038(4) Uani 1 1 d . . . . .
H21A H 0.5937 1.0552 0.2807 0.045 Uiso 1 1 calc R U . . .
C20 C 0.6121(14) 0.9243(18) 0.3713(16) 0.052(6) Uani 1 1 d . . . . .
H20A H 0.5508 0.9475 0.4157 0.062 Uiso 1 1 calc R U . . .
C15 C 0.8903(15) 0.5297(15) 0.4244(13) 0.040(4) Uani 1 1 d . . . . .
H15A H 0.8783 0.4793 0.4769 0.048 Uiso 1 1 calc R U . . .
C1 C 0.9311(19) 1.1173(16) -0.3103(16) 0.055(6) Uani 1 1 d . . . . .
H1A H 0.8874 1.1093 -0.2501 0.066 Uiso 1 1 calc R U . . .
C10 C 1.2534(19) 0.794(2) -0.4077(15) 0.067(8) Uani 1 1 d . . . . .
H10A H 1.2630 0.7355 -0.3620 0.081 Uiso 1 1 calc R U . . .
C4 C 1.0612(13) 1.1399(8) -0.4827(11) 0.061(6) Uani 1 1 d G . . . .
C5 C 1.1299(16) 1.1485(12) -0.5712(10) 0.095(11) Uani 1 1 d G . . . .
H5A H 1.1195 1.2096 -0.6135 0.114 Uiso 1 1 calc R U . . .
C6 C 1.2143(13) 1.0657(16) -0.5964(7) 0.098(11) Uani 1 1 d G U . . .
H6A H 1.2603 1.0714 -0.6556 0.117 Uiso 1 1 calc R U . . .
C7 C 1.2300(10) 0.9744(13) -0.5332(9) 0.061(6) Uani 1 1 d G U . . .
C11 C 1.1612(10) 0.9658(9) -0.4447(8) 0.035(4) Uani 1 1 d G U . . .
C12 C 1.0769(9) 1.0486(9) -0.4195(7) 0.036(4) Uani 1 1 d G . . . .
C2 C 0.907(2) 1.2062(15) -0.3669(18) 0.063(7) Uani 1 1 d . . . . .
H2A H 0.8484 1.2584 -0.3475 0.076 Uiso 1 1 calc R U . . .
C18 C 0.654(2) 0.756(2) 0.4724(17) 0.071(7) Uani 1 1 d . . . . .
H18A H 0.5939 0.7751 0.5195 0.086 Uiso 1 1 calc R U . . .
C3 C 0.974(3) 1.2178(16) -0.456(2) 0.073(8) Uani 1 1 d . . . . .
H3A H 0.9594 1.2783 -0.4985 0.087 Uiso 1 1 calc R U . . .
C17 C 0.721(3) 0.657(2) 0.4846(16) 0.082(9) Uani 1 1 d . . . . .
H17A H 0.7022 0.6110 0.5393 0.099 Uiso 1 1 calc R U . . .
C8 C 1.313(2) 0.888(3) -0.5567(17) 0.089(11) Uani 1 1 d . . . . .
H8A H 1.3633 0.8944 -0.6131 0.107 Uiso 1 1 calc R U . . .
C9 C 1.319(2) 0.787(3) -0.491(2) 0.100(12) Uani 1 1 d . . . . .
H9A H 1.3664 0.7248 -0.5083 0.120 Uiso 1 1 calc R U . . .
V1 V 1.2619(2) 0.3877(2) 0.1431(2) 0.0290(6) Uani 1 1 d . . . . .
V2 V 1.32652(19) 0.27898(19) -0.03727(19) 0.0229(5) Uani 1 1 d . . . . .
V3 V 1.32514(19) 0.5481(2) 0.25256(17) 0.0215(5) Uani 1 1 d . . . . .
V4 V 1.30913(18) 0.72881(19) -0.12311(17) 0.0187(5) Uani 1 1 d . . . . .
V5 V 1.24756(18) 0.68443(18) 0.08815(18) 0.0198(5) Uani 1 1 d . . . . .
V6 V 1.2535(2) 0.5059(2) -0.10452(19) 0.0286(6) Uani 1 1 d . . . . .
V7 V 1.4887(4) 0.6275(4) -0.2636(3) 0.0211(10) Uani 0.5 1 d . . P . .
V8 V 1.5113(4) 0.1856(3) 0.0583(3) 0.0171(9) Uani 0.5 1 d . . P . .
V9 V 1.5048(4) 0.3083(4) -0.2021(3) 0.0181(9) Uani 0.5 1 d . . P . .
As1 As 1.5800(2) 0.1957(2) -0.1800(2) 0.0204(6) Uani 0.5 1 d . . P . .
As2 As 1.5638(2) 0.7282(2) -0.2764(2) 0.0206(6) Uani 0.5 1 d . . P . .
As3 As 1.4399(2) 0.1662(2) 0.1716(2) 0.0222(6) Uani 0.5 1 d . . P . .
As4 As 1.5895(2) 0.1246(2) -0.0354(2) 0.0202(6) Uani 0.5 1 d . . P . .
As5 As 1.4180(2) 0.5484(2) -0.3081(2) 0.0204(6) Uani 0.5 1 d . . P . .
As6 As 1.4186(2) 0.3843(2) -0.2795(2) 0.0228(6) Uani 0.5 1 d . . P . .
Cd1 Cd 1.05909(9) 0.88599(9) -0.22895(8) 0.0239(3) Uani 1 1 d . . . . .
Cd2 Cd 0.93275(9) 0.78996(8) 0.11957(8) 0.0246(3) Uani 1 1 d . . . . .
O1 O 1.1414(9) 0.5163(12) -0.1462(9) 0.043(3) Uani 1 1 d . . . . .
O2 O 1.1321(8) 0.7568(8) 0.1225(8) 0.030(2) Uani 1 1 d . . . . .
O3 O 1.2207(9) 0.8148(9) -0.1717(8) 0.031(2) Uani 1 1 d . . . . .
O4 O 1.2425(9) 0.1972(9) -0.0475(9) 0.035(3) Uani 1 1 d . . . . .
O5 O 1.3507(9) 0.3748(9) -0.1513(8) 0.032(3) Uani 1 1 d . . . . .
O6 O 1.5207(9) 0.4599(8) -0.2699(8) 0.027(2) Uani 1 1 d . . . . .
O7 O 1.2375(8) 0.6305(8) -0.0316(7) 0.021(2) Uani 1 1 d . . . . .
O8 O 0.9991(9) 0.8752(8) -0.0398(8) 0.028(2) Uani 1 1 d . . . . .
O9 O 1.3635(8) 0.3943(9) 0.2322(8) 0.030(2) Uani 1 1 d . . . . .
O10 O 1.2442(8) 0.4089(8) 0.0103(9) 0.029(2) Uani 1 1 d . . . . .
O11 O 1.3453(8) 0.6003(9) -0.1938(8) 0.027(2) Uani 1 1 d . . . . .
O12 O 1.3625(8) 0.2617(8) 0.0915(9) 0.031(2) Uani 1 1 d . . . . .
O13 O 1.0420(9) 1.0249(8) -0.1234(7) 0.027(2) Uani 1 1 d . . . . .
O14 O 1.2442(8) 0.5424(8) 0.1515(7) 0.022(2) Uani 1 1 d . . . . .
O15 O 1.5402(8) 0.2442(8) 0.1798(8) 0.025(2) Uani 1 1 d . . . . .
O16 O 1.4817(8) 0.2159(8) -0.0770(8) 0.025(2) Uani 1 1 d . . . . .
O17 O 1.6600(8) 0.2225(8) 0.0068(7) 0.022(2) Uani 1 1 d . . . . .
O18 O 1.6530(8) 0.3119(8) -0.1796(7) 0.023(2) Uani 1 1 d . . . . .
O19 O 1.4879(11) 0.6708(11) -0.3549(11) 0.050(3) Uani 1 1 d . . . . .
O20 O 1.5180(10) 0.0721(10) 0.0805(8) 0.035(3) Uani 1 1 d . . . . .
O21 O 1.2443(11) 0.5612(11) 0.3535(9) 0.044(3) Uani 1 1 d . . . . .
O22 O 1.5034(10) 0.2450(11) -0.2763(10) 0.044(3) Uani 1 1 d . . . . .
O23 O 1.1555(10) 0.3404(10) 0.2052(12) 0.051(4) Uani 1 1 d . . . . .
O1W O 1.0516(10) 0.7062(10) -0.2417(11) 0.049(4) Uani 1 1 d . . . . .
H1O1 H 1.0863 0.6473 -0.2211 0.059 Uiso 1 1 d R U . . .
H2O1 H 0.9835 0.7011 -0.2270 0.059 Uiso 1 1 d R U . . .
O2W O 0.8636(11) 0.8864(12) -0.1870(12) 0.056(4) Uani 1 1 d . . . . .
O3W O 1.5000 0.5000 0.0000 0.131(14) Uani 1 2 d S . P . .
O4W O 0.9818(10) 0.6504(10) 0.0296(10) 0.044(3) Uani 1 1 d . . . . .
H1O4 H 1.0193 0.6418 -0.0260 0.053 Uiso 1 1 d R U . . .
H2O4 H 0.9417 0.6002 0.0437 0.053 Uiso 1 1 d R U . . .
O5W O 1.775(3) 0.015(2) -0.042(3) 0.20(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N4 C23 1.33(2) . ?
N4 C22 1.35(2) . ?
N4 Cd2 2.347(14) . ?
N3 C24 1.323(19) . ?
N3 C13 1.343(19) . ?
N3 Cd2 2.390(13) . ?
C24 C16 1.44(2) . ?
C24 C23 1.46(2) . ?
N1 C12 1.329(18) . ?
N1 C1 1.33(2) . ?
N1 Cd1 2.367(13) . ?
C19 C18 1.32(3) . ?
C19 C23 1.44(2) . ?
C19 C20 1.45(3) . ?
C25 O8 1.220(17) . ?
C25 O13 1.271(18) . ?
C25 C25 1.51(3) 2_775 ?
N2 C10 1.36(2) . ?
N2 C11 1.380(19) . ?
N2 Cd1 2.363(15) . ?
C13 C14 1.37(2) . ?
C16 C15 1.39(2) . ?
C16 C17 1.41(3) . ?
C22 C21 1.35(2) . ?
C14 C15 1.33(2) . ?
C21 C20 1.33(3) . ?
C1 C2 1.33(3) . ?
C10 C9 1.32(3) . ?
C4 C3 1.38(3) . ?
C4 C5 1.3900 . ?
C4 C12 1.3900 . ?
C5 C6 1.3900 . ?
C6 C7 1.3900 . ?
C7 C11 1.3900 . ?
C7 C8 1.40(4) . ?
C11 C12 1.3900 . ?
C2 C3 1.39(4) . ?
C18 C17 1.41(4) . ?
C8 C9 1.49(5) . ?
V1 O23 1.613(12) . ?
V1 O10 1.929(12) . ?
V1 O14 1.936(10) . ?
V1 O9 1.975(11) . ?
V1 O12 1.984(11) . ?
V1 V3 2.961(4) . ?
V1 V2 2.964(4) . ?
V2 O4 1.616(10) . ?
V2 O10 1.911(10) . ?
V2 O5 1.915(13) . ?
V2 O12 1.950(12) . ?
V2 O16 1.987(10) . ?
V2 V8 2.930(5) . ?
V2 V9 2.956(5) . ?
V2 V6 2.966(4) . ?
V3 O21 1.605(12) . ?
V3 O14 1.923(10) . ?
V3 O9 1.958(11) . ?
V3 O18 1.971(11) 2_865 ?
V3 O6 1.981(11) 2_865 ?
V3 V9 2.940(5) 2_865 ?
V3 V5 2.968(3) . ?
V3 V7 2.969(5) 2_865 ?
V4 O3 1.621(10) . ?
V4 O7 1.890(10) . ?
V4 O11 1.947(11) . ?
V4 O17 1.951(10) 2_865 ?
V4 O15 1.975(10) 2_865 ?
V4 V7 2.948(5) . ?
V4 V6 2.961(4) . ?
V4 V8 2.972(5) 2_865 ?
V4 V5 2.973(4) . ?
V5 O2 1.610(10) . ?
V5 O14 1.910(10) . ?
V5 O7 1.936(10) . ?
V5 O18 1.973(10) 2_865 ?
V5 O17 2.004(10) 2_865 ?
V6 O1 1.608(11) . ?
V6 O10 1.924(12) . ?
V6 O7 1.938(10) . ?
V6 O11 1.971(11) . ?
V6 O5 1.991(11) . ?
V7 O19 1.352(16) . ?
V7 As2 1.665(6) . ?
V7 As5 1.673(6) . ?
V7 O11 1.945(12) . ?
V7 O9 1.960(11) 2_865 ?
V7 O15 2.059(11) 2_865 ?
V7 O6 2.091(11) . ?
V7 V3 2.969(5) 2_865 ?
V8 O20 1.419(12) . ?
V8 As4 1.684(5) . ?
V8 As3 1.703(6) . ?
V8 O12 1.960(11) . ?
V8 O17 1.977(11) . ?
V8 O16 2.013(11) . ?
V8 O15 2.067(12) . ?
V8 V4 2.972(5) 2_865 ?
V9 O22 1.395(14) . ?
V9 As1 1.610(5) . ?
V9 As6 1.785(5) . ?
V9 O18 1.953(11) . ?
V9 O16 2.014(12) . ?
V9 O5 2.017(12) . ?
V9 O6 2.058(12) . ?
V9 V3 2.940(5) 2_865 ?
As1 O16 1.744(11) . ?
As1 O22 1.819(13) . ?
As1 O18 1.841(11) . ?
As1 As4 2.167(4) . ?
As2 O15 1.733(11) 2_865 ?
As2 O9 1.779(11) 2_865 ?
As2 O19 1.860(14) . ?
As2 As3 2.095(4) 2_865 ?
As3 O15 1.737(10) . ?
As3 O12 1.854(11) . ?
As3 O20 1.884(12) . ?
As3 As2 2.095(4) 2_865 ?
As4 O16 1.778(10) . ?
As4 O20 1.829(12) . ?
As4 O17 1.833(10) . ?
As5 O6 1.697(11) . ?
As5 O11 1.844(11) . ?
As5 O19 1.884(15) . ?
As5 As6 2.055(4) . ?
As6 O6 1.740(11) . ?
As6 O5 1.863(12) . ?
As6 O22 1.904(13) . ?
Cd1 O1W 2.305(12) . ?
Cd1 O3 2.339(10) . ?
Cd1 O13 2.388(10) . ?
Cd1 O2W 2.411(14) . ?
Cd2 O4W 2.229(12) . ?
Cd2 O13 2.404(10) 2_775 ?
Cd2 O8 2.452(11) . ?
Cd2 O2 2.478(10) . ?
Cd2 O4 2.571(11) 2_765 ?
O4 Cd2 2.571(11) 2_765 ?
O6 V3 1.981(11) 2_865 ?
O9 As2 1.779(11) 2_865 ?
O9 V7 1.960(11) 2_865 ?
O13 Cd2 2.404(10) 2_775 ?
O15 As2 1.733(11) 2_865 ?
O15 V4 1.975(10) 2_865 ?
O15 V7 2.059(11) 2_865 ?
O17 V4 1.951(10) 2_865 ?
O17 V5 2.004(10) 2_865 ?
O18 V3 1.971(11) 2_865 ?
O18 V5 1.973(10) 2_865 ?

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
C23 N4 C22 117.6(14) . . ?
C23 N4 Cd2 117.8(10) . . ?
C22 N4 Cd2 124.7(11) . . ?
C24 N3 C13 118.4(14) . . ?
C24 N3 Cd2 117.0(10) . . ?
C13 N3 Cd2 124.3(11) . . ?
N3 C24 C16 122.3(14) . . ?
N3 C24 C23 117.1(14) . . ?
C16 C24 C23 120.5(14) . . ?
C12 N1 C1 118.9(16) . . ?
C12 N1 Cd1 117.3(9) . . ?
C1 N1 Cd1 123.7(14) . . ?
C18 C19 C23 122.1(18) . . ?
C18 C19 C20 126.5(18) . . ?
C23 C19 C20 111.2(16) . . ?
N4 C23 C19 124.3(15) . . ?
N4 C23 C24 118.3(14) . . ?
C19 C23 C24 117.4(15) . . ?
O8 C25 O13 123.4(13) . . ?
O8 C25 C25 120.2(17) . 2_775 ?
O13 C25 C25 116.4(15) . 2_775 ?
C10 N2 C11 117.8(17) . . ?
C10 N2 Cd1 126.2(15) . . ?
C11 N2 Cd1 115.7(10) . . ?
N3 C13 C14 122.9(15) . . ?
C15 C16 C17 128.7(18) . . ?
C15 C16 C24 115.5(14) . . ?
C17 C16 C24 115.8(17) . . ?
N4 C22 C21 125.3(17) . . ?
C15 C14 C13 118.9(16) . . ?
C20 C21 C22 116.5(17) . . ?
C21 C20 C19 125.1(16) . . ?
C14 C15 C16 121.9(17) . . ?
N1 C1 C2 124(2) . . ?
C9 C10 N2 127(3) . . ?
C3 C4 C5 121.9(15) . . ?
C3 C4 C12 118.0(15) . . ?
C5 C4 C12 120.0 . . ?
C6 C5 C4 120.0 . . ?
C5 C6 C7 120.0 . . ?
C6 C7 C11 120.0 . . ?
C6 C7 C8 121.7(15) . . ?
C11 C7 C8 118.2(15) . . ?
N2 C11 C12 118.4(10) . . ?
N2 C11 C7 121.6(10) . . ?
C12 C11 C7 120.0 . . ?
N1 C12 C11 118.8(10) . . ?
N1 C12 C4 121.2(10) . . ?
C11 C12 C4 120.0 . . ?
C1 C2 C3 117(2) . . ?
C19 C18 C17 120(2) . . ?
C4 C3 C2 120.1(17) . . ?
C18 C17 C16 124(2) . . ?
C7 C8 C9 120(2) . . ?
C10 C9 C8 114(3) . . ?
O23 V1 O10 108.4(7) . . ?
O23 V1 O14 109.0(6) . . ?
O10 V1 O14 91.1(4) . . ?
O23 V1 O9 107.3(7) . . ?
O10 V1 O9 144.3(5) . . ?
O14 V1 O9 80.0(4) . . ?
O23 V1 O12 106.2(6) . . ?
O10 V1 O12 79.6(5) . . ?
O14 V1 O12 144.7(5) . . ?
O9 V1 O12 87.9(5) . . ?
O23 V1 V3 108.7(6) . . ?
O10 V1 V3 125.9(3) . . ?
O14 V1 V3 39.7(3) . . ?
O9 V1 V3 40.9(3) . . ?
O12 V1 V3 124.4(3) . . ?
O23 V1 V2 108.5(6) . . ?
O10 V1 V2 39.3(3) . . ?
O14 V1 V2 125.2(3) . . ?
O9 V1 V2 123.5(3) . . ?
O12 V1 V2 40.7(3) . . ?
V3 V1 V2 142.76(11) . . ?
O4 V2 O10 108.9(5) . . ?
O4 V2 O5 110.5(6) . . ?
O10 V2 O5 80.8(5) . . ?
O4 V2 O12 111.1(6) . . ?
O10 V2 O12 80.9(5) . . ?
O5 V2 O12 138.0(5) . . ?
O4 V2 O16 111.9(5) . . ?
O10 V2 O16 139.2(4) . . ?
O5 V2 O16 85.2(5) . . ?
O12 V2 O16 84.6(4) . . ?
O4 V2 V8 116.0(5) . . ?
O10 V2 V8 115.7(4) . . ?
O5 V2 V8 119.7(4) . . ?
O12 V2 V8 41.6(3) . . ?
O16 V2 V8 43.2(3) . . ?
O4 V2 V9 116.6(5) . . ?
O10 V2 V9 115.8(4) . . ?
O5 V2 V9 42.6(3) . . ?
O12 V2 V9 118.2(3) . . ?
O16 V2 V9 42.7(3) . . ?
V8 V2 V9 82.07(14) . . ?
O4 V2 V1 112.3(4) . . ?
O10 V2 V1 39.7(4) . . ?
O5 V2 V1 114.6(3) . . ?
O12 V2 V1 41.5(3) . . ?
O16 V2 V1 119.4(3) . . ?
V8 V2 V1 80.54(12) . . ?
V9 V2 V1 130.87(13) . . ?
O4 V2 V6 112.9(4) . . ?
O10 V2 V6 39.5(4) . . ?
O5 V2 V6 41.6(3) . . ?
O12 V2 V6 113.9(3) . . ?
O16 V2 V6 119.3(3) . . ?
V8 V2 V6 130.79(13) . . ?
V9 V2 V6 80.84(12) . . ?
V1 V2 V6 76.81(9) . . ?
O21 V3 O14 110.9(6) . . ?
O21 V3 O9 109.3(6) . . ?
O14 V3 O9 80.8(4) . . ?
O21 V3 O18 112.6(6) . 2_865 ?
O14 V3 O18 79.9(4) . 2_865 ?
O9 V3 O18 137.8(5) . 2_865 ?
O21 V3 O6 110.1(6) . 2_865 ?
O14 V3 O6 138.9(4) . 2_865 ?
O9 V3 O6 85.1(4) . 2_865 ?
O18 V3 O6 85.4(4) 2_865 2_865 ?
O21 V3 V9 116.9(5) . 2_865 ?
O14 V3 V9 113.9(3) . 2_865 ?
O9 V3 V9 119.6(3) . 2_865 ?
O18 V3 V9 41.2(3) 2_865 2_865 ?
O6 V3 V9 44.3(3) 2_865 2_865 ?
O21 V3 V1 111.5(5) . . ?
O14 V3 V1 40.1(3) . . ?
O9 V3 V1 41.4(3) . . ?
O18 V3 V1 114.7(3) 2_865 . ?
O6 V3 V1 120.2(3) 2_865 . ?
V9 V3 V1 131.43(13) 2_865 . ?
O21 V3 V5 114.5(5) . . ?
O14 V3 V5 39.1(3) . . ?
O9 V3 V5 114.3(3) . . ?
O18 V3 V5 41.2(3) 2_865 . ?
O6 V3 V5 119.9(3) 2_865 . ?
V9 V3 V5 79.60(12) 2_865 . ?
V1 V3 V5 77.38(9) . . ?
O21 V3 V7 112.9(5) . 2_865 ?
O14 V3 V7 115.2(3) . 2_865 ?
O9 V3 V7 40.8(3) . 2_865 ?
O18 V3 V7 121.1(3) 2_865 2_865 ?
O6 V3 V7 44.7(3) 2_865 2_865 ?
V9 V3 V7 84.96(15) 2_865 2_865 ?
V1 V3 V7 79.97(12) . 2_865 ?
V5 V3 V7 132.22(13) . 2_865 ?
O3 V4 O7 110.6(5) . . ?
O3 V4 O11 109.4(5) . . ?
O7 V4 O11 80.7(5) . . ?
O3 V4 O17 112.2(5) . 2_865 ?
O7 V4 O17 81.1(4) . 2_865 ?
O11 V4 O17 138.2(4) . 2_865 ?
O3 V4 O15 110.4(5) . 2_865 ?
O7 V4 O15 139.0(4) . 2_865 ?
O11 V4 O15 84.7(4) . 2_865 ?
O17 V4 O15 85.0(4) 2_865 2_865 ?
O3 V4 V7 113.6(4) . . ?
O7 V4 V7 114.7(3) . . ?
O11 V4 V7 40.7(3) . . ?
O17 V4 V7 120.3(3) 2_865 . ?
O15 V4 V7 44.2(3) 2_865 . ?
O3 V4 V6 111.9(4) . . ?
O7 V4 V6 39.9(3) . . ?
O11 V4 V6 41.2(3) . . ?
O17 V4 V6 115.4(3) 2_865 . ?
O15 V4 V6 119.4(3) 2_865 . ?
V7 V4 V6 79.49(13) . . ?
O3 V4 V8 117.7(4) . 2_865 ?
O7 V4 V8 114.2(3) . 2_865 ?
O11 V4 V8 118.5(3) . 2_865 ?
O17 V4 V8 41.2(3) 2_865 2_865 ?
O15 V4 V8 43.9(3) 2_865 2_865 ?
V7 V4 V8 83.70(14) . 2_865 ?
V6 V4 V8 130.31(12) . 2_865 ?
O3 V4 V5 114.2(4) . . ?
O7 V4 V5 39.6(3) . . ?
O11 V4 V5 114.5(3) . . ?
O17 V4 V5 41.9(3) 2_865 . ?
O15 V4 V5 120.0(3) 2_865 . ?
V7 V4 V5 131.70(13) . . ?
V6 V4 V5 77.53(9) . . ?
V8 V4 V5 79.86(12) 2_865 . ?
O2 V5 O14 108.6(5) . . ?
O2 V5 O7 106.7(5) . . ?
O14 V5 O7 90.3(4) . . ?
O2 V5 O18 109.6(5) . 2_865 ?
O14 V5 O18 80.2(4) . 2_865 ?
O7 V5 O18 143.6(4) . 2_865 ?
O2 V5 O17 107.6(5) . 2_865 ?
O14 V5 O17 143.8(4) . 2_865 ?
O7 V5 O17 78.7(4) . 2_865 ?
O18 V5 O17 88.5(4) 2_865 2_865 ?
O2 V5 V3 110.9(4) . . ?
O14 V5 V3 39.4(3) . . ?
O7 V5 V3 124.3(3) . . ?
O18 V5 V3 41.2(3) 2_865 . ?
O17 V5 V3 124.2(3) 2_865 . ?
O2 V5 V4 108.1(4) . . ?
O14 V5 V4 123.7(3) . . ?
O7 V5 V4 38.5(3) . . ?
O18 V5 V4 123.8(3) 2_865 . ?
O17 V5 V4 40.6(3) 2_865 . ?
V3 V5 V4 140.97(10) . . ?
O1 V6 O10 109.2(6) . . ?
O1 V6 O7 105.1(6) . . ?
O10 V6 O7 91.8(4) . . ?
O1 V6 O11 105.2(6) . . ?
O10 V6 O11 145.6(4) . . ?
O7 V6 O11 78.9(4) . . ?
O1 V6 O5 108.5(6) . . ?
O10 V6 O5 78.6(5) . . ?
O7 V6 O5 146.4(4) . . ?
O11 V6 O5 90.9(5) . . ?
O1 V6 V4 105.2(6) . . ?
O10 V6 V4 125.9(3) . . ?
O7 V6 V4 38.7(3) . . ?
O11 V6 V4 40.6(3) . . ?
O5 V6 V4 127.0(3) . . ?
O1 V6 V2 111.4(6) . . ?
O10 V6 V2 39.2(3) . . ?
O7 V6 V2 125.8(3) . . ?
O11 V6 V2 125.1(3) . . ?
O5 V6 V2 39.6(4) . . ?
V4 V6 V2 143.36(11) . . ?
O19 V7 As2 75.3(6) . . ?
O19 V7 As5 76.2(6) . . ?
As2 V7 As5 151.4(4) . . ?
O19 V7 O11 113.9(7) . . ?
As2 V7 O11 135.8(4) . . ?
As5 V7 O11 60.7(4) . . ?
O19 V7 O9 111.7(7) . 2_865 ?
As2 V7 O9 58.1(4) . 2_865 ?
As5 V7 O9 132.8(4) . 2_865 ?
O11 V7 O9 134.5(5) . 2_865 ?
O19 V7 O15 106.2(7) . 2_865 ?
As2 V7 O15 54.2(3) . 2_865 ?
As5 V7 O15 139.1(4) . 2_865 ?
O11 V7 O15 82.5(5) . 2_865 ?
O9 V7 O15 85.4(5) 2_865 2_865 ?
O19 V7 O6 106.3(7) . . ?
As2 V7 O6 135.8(4) . . ?
As5 V7 O6 52.1(3) . . ?
O11 V7 O6 85.1(5) . . ?
O9 V7 O6 82.1(5) 2_865 . ?
O15 V7 O6 147.5(5) 2_865 . ?
O19 V7 V4 113.6(6) . . ?
As2 V7 V4 95.2(2) . . ?
As5 V7 V4 98.7(2) . . ?
O11 V7 V4 40.8(3) . . ?
O9 V7 V4 117.4(4) 2_865 . ?
O15 V7 V4 42.0(3) 2_865 . ?
O6 V7 V4 121.8(4) . . ?
O19 V7 V3 111.5(6) . 2_865 ?
As2 V7 V3 95.5(2) . 2_865 ?
As5 V7 V3 92.3(2) . 2_865 ?
O11 V7 V3 117.5(4) . 2_865 ?
O9 V7 V3 40.7(3) 2_865 2_865 ?
O15 V7 V3 122.3(3) 2_865 2_865 ?
O6 V7 V3 41.7(3) . 2_865 ?
V4 V7 V3 134.98(18) . 2_865 ?
O20 V8 As4 71.7(5) . . ?
O20 V8 As3 73.6(5) . . ?
As4 V8 As3 145.2(3) . . ?
O20 V8 O12 113.2(6) . . ?
As4 V8 O12 138.1(4) . . ?
As3 V8 O12 60.3(4) . . ?
O20 V8 O17 108.9(6) . . ?
As4 V8 O17 59.4(3) . . ?
As3 V8 O17 133.3(4) . . ?
O12 V8 O17 137.8(5) . . ?
O20 V8 O16 106.8(6) . . ?
As4 V8 O16 56.7(3) . . ?
As3 V8 O16 138.7(4) . . ?
O12 V8 O16 83.6(5) . . ?
O17 V8 O16 86.7(4) . . ?
O20 V8 O15 104.7(6) . . ?
As4 V8 O15 135.4(4) . . ?
As3 V8 O15 53.8(3) . . ?
O12 V8 O15 85.2(5) . . ?
O17 V8 O15 82.0(4) . . ?
O16 V8 O15 148.4(5) . . ?
O20 V8 V2 113.8(5) . . ?
As4 V8 V2 97.4(2) . . ?
As3 V8 V2 98.2(2) . . ?
O12 V8 V2 41.3(4) . . ?
O17 V8 V2 120.4(3) . . ?
O16 V8 V2 42.6(3) . . ?
O15 V8 V2 122.5(3) . . ?
O20 V8 V4 110.8(5) . 2_865 ?
As4 V8 V4 96.7(2) . 2_865 ?
As3 V8 V4 93.7(2) . 2_865 ?
O12 V8 V4 117.4(4) . 2_865 ?
O17 V8 V4 40.5(3) . 2_865 ?
O16 V8 V4 122.4(4) . 2_865 ?
O15 V8 V4 41.5(3) . 2_865 ?
V2 V8 V4 135.47(17) . 2_865 ?
O22 V9 As1 74.1(6) . . ?
O22 V9 As6 72.4(6) . . ?
As1 V9 As6 146.5(3) . . ?
O22 V9 O18 112.4(6) . . ?
As1 V9 O18 61.3(4) . . ?
As6 V9 O18 135.2(4) . . ?
O22 V9 O16 108.3(7) . . ?
As1 V9 O16 56.2(3) . . ?
As6 V9 O16 135.8(4) . . ?
O18 V9 O16 86.8(5) . . ?
O22 V9 O5 109.6(6) . . ?
As1 V9 O5 135.2(5) . . ?
As6 V9 O5 58.3(4) . . ?
O18 V9 O5 137.9(5) . . ?
O16 V9 O5 81.9(5) . . ?
O22 V9 O6 104.2(7) . . ?
As1 V9 O6 139.5(4) . . ?
As6 V9 O6 53.3(3) . . ?
O18 V9 O6 83.8(5) . . ?
O16 V9 O6 147.3(5) . . ?
O5 V9 O6 84.4(5) . . ?
O22 V9 V3 112.2(6) . 2_865 ?
As1 V9 V3 99.7(2) . 2_865 ?
As6 V9 V3 94.0(2) . 2_865 ?
O18 V9 V3 41.7(3) . 2_865 ?
O16 V9 V3 123.3(3) . 2_865 ?
O5 V9 V3 117.8(4) . 2_865 ?
O6 V9 V3 42.3(3) . 2_865 ?
O22 V9 V2 112.9(6) . . ?
As1 V9 V2 96.2(2) . . ?
As6 V9 V2 95.5(2) . . ?
O18 V9 V2 119.7(4) . . ?
O16 V9 V2 42.0(3) . . ?
O5 V9 V2 40.0(4) . . ?
O6 V9 V2 120.1(3) . . ?
V3 V9 V2 134.74(16) 2_865 . ?
V9 As1 O16 73.7(4) . . ?
V9 As1 O22 47.5(5) . . ?
O16 As1 O22 103.0(6) . . ?
V9 As1 O18 68.6(4) . . ?
O16 As1 O18 99.0(5) . . ?
O22 As1 O18 99.8(6) . . ?
V9 As1 As4 122.7(2) . . ?
O16 As1 As4 52.7(3) . . ?
O22 As1 As4 151.7(5) . . ?
O18 As1 As4 98.6(3) . . ?
V7 As2 O15 74.6(4) . 2_865 ?
V7 As2 O9 69.3(4) . 2_865 ?
O15 As2 O9 101.8(5) 2_865 2_865 ?
V7 As2 O19 44.7(5) . . ?
O15 As2 O19 100.3(6) 2_865 . ?
O9 As2 O19 98.7(6) 2_865 . ?
V7 As2 As3 124.9(2) . 2_865 ?
O15 As2 As3 52.9(3) 2_865 2_865 ?
O9 As2 As3 103.4(4) 2_865 2_865 ?
O19 As2 As3 148.2(4) . 2_865 ?
V8 As3 O15 73.8(4) . . ?
V8 As3 O12 66.7(4) . . ?
O15 As3 O12 98.8(5) . . ?
V8 As3 O20 46.3(4) . . ?
O15 As3 O20 100.6(5) . . ?
O12 As3 O20 98.7(5) . . ?
V8 As3 As2 121.7(2) . 2_865 ?
O15 As3 As2 52.8(4) . 2_865 ?
O12 As3 As2 97.4(4) . 2_865 ?
O20 As3 As2 150.8(4) . 2_865 ?
V8 As4 O16 71.0(4) . . ?
V8 As4 O20 47.4(4) . . ?
O16 As4 O20 100.8(5) . . ?
V8 As4 O17 68.3(4) . . ?
O16 As4 O17 98.7(5) . . ?
O20 As4 O17 98.9(5) . . ?
V8 As4 As1 119.3(2) . . ?
O16 As4 As1 51.3(4) . . ?
O20 As4 As1 148.1(4) . . ?
O17 As4 As1 100.5(3) . . ?
V7 As5 O6 76.7(4) . . ?
V7 As5 O11 66.9(4) . . ?
O6 As5 O11 100.9(5) . . ?
V7 As5 O19 44.2(5) . . ?
O6 As5 O19 102.3(6) . . ?
O11 As5 O19 96.5(5) . . ?
V7 As5 As6 127.6(2) . . ?
O6 As5 As6 54.2(4) . . ?
O11 As5 As6 102.4(4) . . ?
O19 As5 As6 152.2(4) . . ?
O6 As6 V9 71.4(4) . . ?
O6 As6 O5 98.8(5) . . ?
V9 As6 O5 67.1(4) . . ?
O6 As6 O22 98.1(5) . . ?
V9 As6 O22 44.3(4) . . ?
O5 As6 O22 96.5(6) . . ?
O6 As6 As5 52.3(4) . . ?
V9 As6 As5 120.6(2) . . ?
O5 As6 As5 101.6(4) . . ?
O22 As6 As5 147.1(5) . . ?
O1W Cd1 O3 82.3(4) . . ?
O1W Cd1 N2 83.6(6) . . ?
O3 Cd1 N2 83.7(5) . . ?
O1W Cd1 N1 129.4(5) . . ?
O3 Cd1 N1 132.7(5) . . ?
N2 Cd1 N1 69.2(5) . . ?
O1W Cd1 O13 146.4(5) . . ?
O3 Cd1 O13 86.4(4) . . ?
N2 Cd1 O13 126.5(5) . . ?
N1 Cd1 O13 80.4(4) . . ?
O1W Cd1 O2W 80.8(5) . . ?
O3 Cd1 O2W 140.5(5) . . ?
N2 Cd1 O2W 129.1(5) . . ?
N1 Cd1 O2W 84.5(5) . . ?
O13 Cd1 O2W 88.3(4) . . ?
O4W Cd2 N4 138.4(5) . . ?
O4W Cd2 N3 91.6(5) . . ?
N4 Cd2 N3 69.3(4) . . ?
O4W Cd2 O13 142.2(4) . 2_775 ?
N4 Cd2 O13 76.8(4) . 2_775 ?
N3 Cd2 O13 119.7(4) . 2_775 ?
O4W Cd2 O8 76.8(4) . . ?
N4 Cd2 O8 128.4(4) . . ?
N3 Cd2 O8 161.9(4) . . ?
O13 Cd2 O8 67.3(3) 2_775 . ?
O4W Cd2 O2 80.1(4) . . ?
N4 Cd2 O2 130.6(4) . . ?
N3 Cd2 O2 83.3(4) . . ?
O13 Cd2 O2 82.9(4) 2_775 . ?
O8 Cd2 O2 81.0(4) . . ?
O4W Cd2 O4 81.2(4) . 2_765 ?
N4 Cd2 O4 72.6(4) . 2_765 ?
N3 Cd2 O4 110.9(4) . 2_765 ?
O13 Cd2 O4 104.1(3) 2_775 2_765 ?
O8 Cd2 O4 81.4(4) . 2_765 ?
O2 Cd2 O4 156.7(4) . 2_765 ?
V5 O2 Cd2 146.7(6) . . ?
V4 O3 Cd1 159.6(7) . . ?
V2 O4 Cd2 136.2(7) . 2_765 ?
As6 O5 V2 144.3(6) . . ?
As6 O5 V6 116.7(6) . . ?
V2 O5 V6 98.8(5) . . ?
As6 O5 V9 54.6(3) . . ?
V2 O5 V9 97.4(6) . . ?
V6 O5 V9 146.7(6) . . ?
As5 O6 As6 73.4(4) . . ?
As5 O6 V3 140.8(6) . 2_865 ?
As6 O6 V3 144.7(6) . 2_865 ?
As5 O6 V9 125.3(6) . . ?
As6 O6 V9 55.3(3) . . ?
V3 O6 V9 93.4(5) 2_865 . ?
As5 O6 V7 51.1(3) . . ?
As6 O6 V7 121.6(6) . . ?
V3 O6 V7 93.6(5) 2_865 . ?
V9 O6 V7 148.3(6) . . ?
V4 O7 V5 102.0(5) . . ?
V4 O7 V6 101.3(5) . . ?
V5 O7 V6 147.1(5) . . ?
C25 O8 Cd2 117.1(10) . . ?
As2 O9 V3 142.5(6) 2_865 . ?
As2 O9 V7 52.6(3) 2_865 2_865 ?
V3 O9 V7 98.6(5) . 2_865 ?
As2 O9 V1 118.9(6) 2_865 . ?
V3 O9 V1 97.7(4) . . ?
V7 O9 V1 151.2(6) 2_865 . ?
V2 O10 V6 101.3(5) . . ?
V2 O10 V1 101.0(5) . . ?
V6 O10 V1 145.9(6) . . ?
As5 O11 V7 52.3(3) . . ?
As5 O11 V4 143.6(6) . . ?
V7 O11 V4 98.5(5) . . ?
As5 O11 V6 117.9(6) . . ?
V7 O11 V6 149.6(6) . . ?
V4 O11 V6 98.2(5) . . ?
As3 O12 V2 141.5(6) . . ?
As3 O12 V8 53.0(3) . . ?
V2 O12 V8 97.1(5) . . ?
As3 O12 V1 120.2(6) . . ?
V2 O12 V1 97.8(5) . . ?
V8 O12 V1 150.0(6) . . ?
C25 O13 Cd1 98.2(8) . . ?
C25 O13 Cd2 119.0(9) . 2_775 ?
Cd1 O13 Cd2 142.8(5) . 2_775 ?
V5 O14 V3 101.5(4) . . ?
V5 O14 V1 148.9(6) . . ?
V3 O14 V1 100.2(5) . . ?
As2 O15 As3 74.3(4) 2_865 . ?
As2 O15 V4 142.5(6) 2_865 2_865 ?
As3 O15 V4 142.8(6) . 2_865 ?
As2 O15 V7 51.2(3) 2_865 2_865 ?
As3 O15 V7 123.0(6) . 2_865 ?
V4 O15 V7 93.9(4) 2_865 2_865 ?
As2 O15 V8 121.7(6) 2_865 . ?
As3 O15 V8 52.3(3) . . ?
V4 O15 V8 94.6(5) 2_865 . ?
V7 O15 V8 146.4(6) 2_865 . ?
As1 O16 As4 75.9(4) . . ?
As1 O16 V2 140.7(6) . . ?
As4 O16 V2 142.1(6) . . ?
As1 O16 V8 124.9(5) . . ?
As4 O16 V8 52.3(3) . . ?
V2 O16 V8 94.2(5) . . ?
As1 O16 V9 50.1(3) . . ?
As4 O16 V9 122.4(6) . . ?
V2 O16 V9 95.2(4) . . ?
V8 O16 V9 147.3(6) . . ?
As4 O17 V4 142.4(6) . 2_865 ?
As4 O17 V8 52.3(3) . . ?
V4 O17 V8 98.3(5) 2_865 . ?
As4 O17 V5 119.9(5) . 2_865 ?
V4 O17 V5 97.5(4) 2_865 2_865 ?
V8 O17 V5 146.9(5) . 2_865 ?
As1 O18 V9 50.1(3) . . ?
As1 O18 V3 140.0(5) . 2_865 ?
V9 O18 V3 97.1(5) . 2_865 ?
As1 O18 V5 122.3(6) . 2_865 ?
V9 O18 V5 148.9(6) . 2_865 ?
V3 O18 V5 97.6(5) 2_865 2_865 ?
V7 O19 As2 60.0(6) . . ?
V7 O19 As5 59.6(6) . . ?
As2 O19 As5 119.5(8) . . ?
V8 O20 As4 60.9(5) . . ?
V8 O20 As3 60.1(5) . . ?
As4 O20 As3 121.0(6) . . ?
V9 O22 As1 58.4(5) . . ?
V9 O22 As6 63.3(6) . . ?
As1 O22 As6 121.7(7) . . ?

_refine_diff_density_max         1.532
_refine_diff_density_min         -1.470
_refine_diff_density_rms         0.270

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

data_shelx_6
_database_code_depnum_ccdc_archive 'CCDC 1430184'
_audit_update_record             
;
2015-10-08 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT430_shelx_6             
;
PROBLEM:  Short Inter D...A Contact  O1W ..O1W .. 1.38 Ang
RESPONSE: O1w was disorderedly distributed over two positions
with occupancy factor of 0.5; There should be a strong 
hydrogen bond between the two atoms, N6 is disorderedly 
distributed and the hydrogen atoms were not added.
;

_vrf_PLAT341_shelx_6             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.0160 Ang
RESPONSE: The quality of this crystal was poor.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C60 H52 As8 Co2 N12 O49 V14'
_chemical_formula_weight         3155.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6254(3)
_cell_length_b                   14.4554(4)
_cell_length_c                   14.6510(4)
_cell_angle_alpha                99.363(2)
_cell_angle_beta                 97.293(2)
_cell_angle_gamma                91.069(2)
_cell_volume                     2407.70(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7028
_cell_measurement_theta_min      3.5310
_cell_measurement_theta_max      27.5010

_exptl_crystal_description       columnar
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_F_000             1528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    4.449
_shelx_estimated_absorpt_T_min   0.575
_shelx_estimated_absorpt_T_max   0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.61380
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20076
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.955
_diffrn_reflns_theta_max         28.977
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10917
_reflns_number_gt                7881
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1235P)²+17.3512P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10917
_refine_ls_number_parameters     736
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0714
_refine_ls_wR_factor_ref         0.2307
_refine_ls_wR_factor_gt          0.2029
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As4 As 0.87176(11) 0.59445(9) 0.99793(10) 0.0320(3) Uani 0.8 1 d . . P . .
As44 As 0.8648(4) 0.5734(4) 0.9531(5) 0.0390(12) Uani 0.2 1 d . . P . .
As3 As 0.43158(16) 0.80233(12) 0.96203(11) 0.0354(4) Uani 0.8 1 d . . P . .
As33 As 0.4230(7) 0.7866(5) 0.9217(5) 0.0419(16) Uani 0.2 1 d . . P . .
As2 As 0.33421(8) 0.65663(7) 0.77318(7) 0.0414(2) Uani 0.9 1 d . . P . .
As22 As 0.3230(7) 0.5858(6) 0.7905(5) 0.0317(15) Uani 0.1 1 d . . P . .
As1 As 0.77875(9) 0.44835(7) 0.80845(7) 0.0410(2) Uani 0.9 1 d . . P . .
As11 As 0.6935(7) 0.4088(6) 0.8169(6) 0.0380(18) Uani 0.1 1 d . . P . .
V2 V 0.60273(14) 0.27944(11) 0.84447(11) 0.0239(3) Uani 0.7 1 d . . P . .
V22 V 0.5959(4) 0.2066(4) 0.8599(4) 0.0481(13) Uani 0.3 1 d . . P . .
V1 V 0.22695(13) 0.45829(11) 0.81918(11) 0.0311(3) Uani 0.8 1 d . . P . .
V11 V 0.1372(5) 0.4257(4) 0.8293(4) 0.0239(11) Uani 0.2 1 d . . P . .
Co1 Co 0.87982(10) 0.06093(8) 0.34784(8) 0.0390(3) Uani 1 1 d . . . . .
V7 V 0.23210(10) 0.62727(8) 0.98005(8) 0.0278(3) Uani 1 1 d . . . . .
V6 V 0.62826(11) 0.65414(9) 0.85481(9) 0.0301(3) Uani 1 1 d . . . . .
V5 V 0.32535(11) 0.26229(9) 0.93459(9) 0.0338(3) Uani 1 1 d . . . . .
V4 V 0.50524(12) 0.47893(10) 0.72944(9) 0.0369(3) Uani 1 1 d . . . . .
V3 V 0.37895(13) 0.31429(12) 0.75859(10) 0.0458(4) Uani 1 1 d . . . . .
O56 O 0.2518(5) 0.1654(4) 0.9196(4) 0.0456(14) Uani 1 1 d . . . . .
O15 O 0.7311(6) 0.3770(5) 0.8853(4) 0.0503(15) Uani 1 1 d . . . . .
O17 O 0.1150(5) 0.6806(4) 0.9707(4) 0.0416(13) Uani 1 1 d . . . . .
O16 O 0.6587(5) 0.5239(4) 0.8009(4) 0.0392(12) Uani 1 1 d . . . . .
O57 O 0.5159(6) 0.4801(5) 0.6223(4) 0.0554(17) Uani 1 1 d . . . . .
O18 O 0.6851(5) 0.7196(4) 0.7942(4) 0.0443(14) Uani 1 1 d . . . . .
O3 O 0.7429(5) 0.6527(4) 0.9667(4) 0.0347(11) Uani 1 1 d . . . . .
O7 O 0.4754(5) 0.6100(4) 0.7856(4) 0.0355(12) Uani 1 1 d . . . . .
O58 O 0.3474(5) 0.4424(4) 0.7383(4) 0.0394(13) Uani 1 1 d . . . . .
O59 O 0.3286(7) 0.2424(5) 0.6667(5) 0.0644(19) Uani 1 1 d . . . . .
O36 O 1.0502(5) 0.0680(5) 0.4254(5) 0.0489(15) Uani 1 1 d . . . . .
O60 O 0.4470(5) 0.2445(4) 0.8549(4) 0.0366(12) Uani 1 1 d . . . . .
O61 O 0.2610(5) 0.3350(4) 0.8414(4) 0.0363(12) Uani 1 1 d . . . . .
O34 O 0.8532(5) -0.0159(4) 0.4552(4) 0.0447(14) Uani 1 1 d . . . . .
O8 O 0.5593(5) 0.7373(4) 0.9520(4) 0.0354(11) Uani 1 1 d . . . . .
O9 O 0.2709(6) 0.5948(5) 0.8500(5) 0.0496(15) Uani 1 1 d . . . . .
O62 O 0.5367(5) 0.3543(4) 0.7540(4) 0.0371(12) Uani 1 1 d . . . . .
C9 C 0.9839(9) -0.2210(7) 0.2279(8) 0.058(3) Uani 1 1 d . . . . .
H9A H 0.9767 -0.2823 0.2387 0.069 Uiso 1 1 calc R U . . .
O10 O 0.6443(5) 0.2731(4) 0.9806(5) 0.0491(15) Uani 1 1 d . . . . .
O4 O 0.1901(5) 0.4912(4) 0.9487(4) 0.0470(14) Uani 1 1 d . . . . .
O63 O 0.6587(7) 0.1913(6) 0.7877(6) 0.069(2) Uani 1 1 d . . . . .
N1 N 0.9534(6) 0.1216(5) 0.2460(5) 0.0431(16) Uani 1 1 d . . . . .
N2 N 0.9324(6) -0.0602(5) 0.2642(5) 0.0407(15) Uani 1 1 d . . . . .
N3 N 0.7019(6) 0.0641(5) 0.2965(5) 0.0407(15) Uani 1 1 d . . . . .
O13 O 0.8796(6) 0.5245(5) 0.8844(5) 0.0564(17) Uani 1 1 d . U . . .
C7 C 1.0623(8) -0.1057(7) 0.1492(6) 0.049(2) Uani 1 1 d . U . . .
C11 C 1.0016(7) -0.0384(6) 0.2014(6) 0.0377(17) Uani 1 1 d . . . . .
O12 O 0.3601(6) 0.7665(5) 0.8452(5) 0.0589(18) Uani 1 1 d . . . . .
C4 C 1.0799(8) 0.0845(8) 0.1264(7) 0.054(2) Uani 1 1 d . . . . .
C2 C 1.0289(10) 0.2410(8) 0.1735(8) 0.062(3) Uani 1 1 d . . . . .
H2A H 1.0337 0.3043 0.1690 0.074 Uiso 1 1 calc R U . . .
O64 O 0.1056(6) 0.4492(6) 0.7532(5) 0.0653(19) Uani 1 1 d . . . . .
C3 C 1.0845(10) 0.1801(9) 0.1186(8) 0.065(3) Uani 1 1 d . . . . .
H3A H 1.1263 0.2007 0.0751 0.079 Uiso 1 1 calc R U . . .
N4 N 0.8306(7) 0.1843(5) 0.4340(5) 0.0493(18) Uani 1 1 d . . . . .
C10 C 0.9246(8) -0.1495(6) 0.2755(7) 0.047(2) Uani 1 1 d . . . . .
H10A H 0.8769 -0.1651 0.3176 0.056 Uiso 1 1 calc R U . . .
C15 C 0.4646(9) 0.0827(8) 0.2511(7) 0.056(2) Uani 1 1 d . . . . .
H15A H 0.3852 0.0881 0.2354 0.067 Uiso 1 1 calc R U . . .
C6 C 1.1314(9) -0.0778(9) 0.0822(8) 0.066(3) Uani 1 1 d . U . . .
H6A H 1.1701 -0.1224 0.0456 0.079 Uiso 1 1 calc R U . . .
C14 C 0.5195(10) 0.0153(9) 0.2049(9) 0.069(3) Uani 1 1 d . . . . .
H14A H 0.4785 -0.0268 0.1564 0.083 Uiso 1 1 calc R U . . .
C12 C 1.0101(7) 0.0577(6) 0.1914(6) 0.0406(18) Uani 1 1 d . . . . .
C8 C 1.0519(9) -0.1993(7) 0.1659(8) 0.056(2) Uani 1 1 d . . . . .
H8A H 1.0924 -0.2461 0.1337 0.067 Uiso 1 1 calc R U . . .
C24 C 0.6463(7) 0.1348(6) 0.3446(6) 0.0370(17) Uani 1 1 d . . . . .
O1W O 0.5145(7) 0.5295(7) 0.0422(7) 0.030(2) Uani 0.5 1 d . . P . .
C20 C 0.7318(12) 0.3274(8) 0.5434(8) 0.076(4) Uani 1 1 d . . . . .
H20A H 0.6994 0.3759 0.5804 0.091 Uiso 1 1 calc R U . . .
C25 C 1.0571(7) 0.0234(6) 0.4915(6) 0.0375(17) Uani 1 1 d . . . . .
C5 C 1.1395(10) 0.0128(11) 0.0729(8) 0.074(4) Uani 1 1 d . . . . .
H5A H 1.1854 0.0299 0.0303 0.089 Uiso 1 1 calc R U . . .
C16 C 0.5274(9) 0.1471(6) 0.3249(6) 0.048(2) Uani 1 1 d . . . . .
C23 C 0.7149(8) 0.1973(6) 0.4185(6) 0.0422(19) Uani 1 1 d . . . . .
C21 C 0.8480(12) 0.3125(8) 0.5594(9) 0.076(4) Uani 1 1 d . . . . .
H21A H 0.8958 0.3501 0.6074 0.091 Uiso 1 1 calc R U . . .
C22 C 0.8922(10) 0.2399(8) 0.5021(8) 0.064(3) Uani 1 1 d . . . . .
H22A H 0.9713 0.2303 0.5129 0.076 Uiso 1 1 calc R U . . .
C13 C 0.6412(9) 0.0060(7) 0.2283(7) 0.056(2) Uani 1 1 d . . . . .
H13A H 0.6782 -0.0421 0.1947 0.067 Uiso 1 1 calc R U . . .
C18 C 0.5379(11) 0.2797(9) 0.4498(8) 0.071(3) Uani 1 1 d . . . . .
H18A H 0.5012 0.3269 0.4849 0.085 Uiso 1 1 calc R U . . .
C19 C 0.6633(10) 0.2699(7) 0.4720(7) 0.056(2) Uani 1 1 d . . . . .
C17 C 0.4765(10) 0.2222(9) 0.3805(7) 0.063(3) Uani 1 1 d . . . . .
H17A H 0.3975 0.2309 0.3674 0.076 Uiso 1 1 calc R U . . .
N7 N 0.6012(14) 0.9568(11) 0.4890(12) 0.099(4) Uani 0.5 1 d . . P . .
C31 C 0.6012(14) 0.9568(11) 0.4890(12) 0.099(4) Uani 0.5 1 d . . P . .
N8 N 0.711(3) 1.050(2) 0.627(2) 0.115(10) Uani 0.5 1 d . . P . .
C33 C 0.5026(17) 0.9243(13) 0.4284(15) 0.113(6) Uani 1 1 d . . . . .
C1 C 0.9626(9) 0.2115(7) 0.2389(8) 0.057(3) Uani 1 1 d . . . . .
H1A H 0.9251 0.2556 0.2771 0.068 Uiso 1 1 calc R U . . .
O2W O 0.209(2) 0.2319(17) 0.4736(17) 0.247(10) Uani 1 1 d . U . . .
H1O2 H 0.2488 0.2300 0.5262 0.297 Uiso 1 1 d R U . . .
H2O2 H 0.1708 0.1799 0.4567 0.297 Uiso 1 1 d R U . . .
C32 C 0.6029(17) 1.0281(13) 0.5585(13) 0.103(5) Uani 1 1 d . U . . .
C26 C 0.0719(14) 0.4363(11) 0.3633(7) 0.073(5) Uani 0.5 1 d G U P . .
C27 C 0.1844(14) 0.4062(11) 0.3800(9) 0.072(5) Uani 0.5 1 d G U P . .
C28 C 0.2409(11) 0.4171(12) 0.4708(10) 0.087(6) Uani 0.5 1 d G U P . .
N5 N 0.1850(10) 0.4581(11) 0.5448(8) 0.075(5) Uani 0.5 1 d DG U P . .
C29 C 0.0726(10) 0.4882(11) 0.5280(7) 0.068(5) Uani 0.5 1 d DG U P . .
C30 C 0.0161(10) 0.4773(11) 0.4373(8) 0.058(4) Uani 0.5 1 d DG U P . .
N6 N 0.0174(16) 0.5310(18) 0.5996(10) 0.087(6) Uani 0.5 1 d D U P . .


_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
As4 As44 0.672(6) . ?
As4 O4 1.757(6) 2_667 ?
As4 O3 1.778(5) . ?
As4 O13 1.815(7) . ?
As4 V11 2.610(6) 2_667 ?
As44 O13 1.166(9) . ?
As44 O3 1.849(7) . ?
As44 O4 1.999(9) 2_667 ?
As44 As1 2.628(7) . ?
As3 As33 0.593(6) . ?
As3 O10 1.767(7) 2_667 ?
As3 O8 1.781(5) . ?
As3 O12 1.795(7) . ?
As3 V22 2.692(6) 2_667 ?
As33 O12 1.246(10) . ?
As33 O8 1.784(9) . ?
As33 O10 2.017(10) 2_667 ?
As33 As2 2.713(7) . ?
As2 As22 1.103(8) . ?
As2 O12 1.755(8) . ?
As2 O9 1.766(6) . ?
As2 O7 1.785(5) . ?
As22 O9 1.116(10) . ?
As22 O7 1.811(9) . ?
As22 O58 2.127(10) . ?
As22 V1 2.262(8) . ?
As22 V4 2.798(8) . ?
As1 As11 1.164(8) . ?
As1 O13 1.745(7) . ?
As1 O15 1.776(7) . ?
As1 O16 1.791(6) . ?
As11 O15 1.206(11) . ?
As11 O16 1.764(11) . ?
As11 O62 2.020(10) . ?
As11 V2 2.249(9) . ?
As11 V4 2.693(9) . ?
V2 V22 1.116(6) . ?
V2 O63 1.600(7) . ?
V2 O60 1.902(6) . ?
V2 O62 1.938(6) . ?
V2 O15 1.998(7) . ?
V2 O10 2.009(7) . ?
V2 V3 2.834(2) . ?
V2 V7 3.104(2) 2_667 ?
V22 O63 1.350(9) . ?
V22 O60 1.822(7) . ?
V22 O10 1.882(8) . ?
V22 As3 2.692(6) 2_667 ?
V1 V11 1.173(6) . ?
V1 O64 1.596(7) . ?
V1 O61 1.903(6) . ?
V1 O58 1.940(6) . ?
V1 O4 1.983(7) . ?
V1 O9 1.994(7) . ?
V1 V3 2.860(2) . ?
V1 V7 3.100(2) . ?
V11 O64 1.231(9) . ?
V11 O4 1.872(8) . ?
V11 O61 1.976(8) . ?
V11 As4 2.610(6) 2_667 ?
Co1 N1 2.109(7) . ?
Co1 N3 2.113(7) . ?
Co1 N2 2.116(7) . ?
Co1 O34 2.117(6) . ?
Co1 N4 2.143(7) . ?
Co1 O36 2.147(6) . ?
V7 O17 1.579(5) . ?
V7 O15 1.976(6) 2_667 ?
V7 O10 1.979(6) 2_667 ?
V7 O4 1.983(7) . ?
V7 O9 1.997(7) . ?
V7 V2 3.104(2) 2_667 ?
V6 O18 1.588(6) . ?
V6 O7 1.971(5) . ?
V6 O8 1.971(5) . ?
V6 O16 1.976(6) . ?
V6 O3 1.981(5) . ?
V6 V4 3.0851(19) . ?
V6 V5 3.1001(18) 2_667 ?
V5 O56 1.596(6) . ?
V5 O61 1.940(6) . ?
V5 O60 1.941(6) . ?
V5 O3 1.995(5) 2_667 ?
V5 O8 1.997(5) 2_667 ?
V5 V3 2.937(2) . ?
V5 V6 3.1001(18) 2_667 ?
V4 O57 1.593(6) . ?
V4 O58 1.926(6) . ?
V4 O62 1.926(6) . ?
V4 O16 1.991(6) . ?
V4 O7 1.994(6) . ?
V4 V3 2.892(2) . ?
V3 O59 1.599(7) . ?
V3 O62 1.925(6) . ?
V3 O61 1.939(6) . ?
V3 O58 1.957(6) . ?
V3 O60 1.960(6) . ?
O15 V7 1.976(6) 2_667 ?
O3 V5 1.995(5) 2_667 ?
O36 C25 1.243(10) . ?
O34 C25 1.239(10) 2_756 ?
O8 V5 1.997(5) 2_667 ?
C9 C8 1.347(15) . ?
C9 C10 1.395(13) . ?
C9 H9A 0.9300 . ?
O10 As3 1.767(7) 2_667 ?
O10 V7 1.979(6) 2_667 ?
O10 As33 2.017(10) 2_667 ?
O4 As4 1.757(6) 2_667 ?
O4 As44 1.999(9) 2_667 ?
N1 C1 1.323(12) . ?
N1 C12 1.358(12) . ?
N2 C10 1.330(11) . ?
N2 C11 1.366(10) . ?
N3 C13 1.316(12) . ?
N3 C24 1.365(10) . ?
C7 C11 1.397(12) . ?
C7 C8 1.419(15) . ?
C7 C6 1.446(14) . ?
C11 C12 1.423(12) . ?
C4 C3 1.406(16) . ?
C4 C12 1.421(12) . ?
C4 C5 1.439(17) . ?
C2 C3 1.327(17) . ?
C2 C1 1.415(15) . ?
C2 H2A 0.9300 . ?
C3 H3A 0.9300 . ?
N4 C22 1.301(13) . ?
N4 C23 1.356(12) . ?
C10 H10A 0.9300 . ?
C15 C14 1.317(15) . ?
C15 C16 1.420(14) . ?
C15 H15A 0.9300 . ?
C6 C5 1.341(18) . ?
C6 H6A 0.9300 . ?
C14 C13 1.427(15) . ?
C14 H14A 0.9300 . ?
C8 H8A 0.9300 . ?
C24 C16 1.397(12) . ?
C24 C23 1.435(12) . ?
O1W O1W 1.38(2) 2_665 ?
C20 C21 1.368(18) . ?
C20 C19 1.380(16) . ?
C20 H20A 0.9300 . ?
C25 O34 1.239(10) 2_756 ?
C25 C25 1.545(15) 2_756 ?
C5 H5A 0.9300 . ?
C16 C17 1.432(14) . ?
C23 C19 1.397(12) . ?
C21 C22 1.384(15) . ?
C21 H21A 0.9300 . ?
C22 H22A 0.9300 . ?
C13 H13A 0.9300 . ?
C18 C17 1.323(16) . ?
C18 C19 1.466(16) . ?
C18 H18A 0.9300 . ?
C17 H17A 0.9300 . ?
N7 C32 1.32(2) . ?
N7 C33 1.38(2) . ?
N8 C32 1.50(3) . ?
C33 C32 1.44(2) 2_676 ?
C1 H1A 0.9300 . ?
O2W H1O2 0.8507 . ?
O2W H2O2 0.8509 . ?
C32 C33 1.43(2) 2_676 ?
C26 N6 1.30(2) 2_566 ?
C26 C27 1.3900 . ?
C26 C30 1.3900 . ?
C27 C28 1.3900 . ?
C28 N5 1.3900 . ?
N5 C29 1.3900 . ?
C29 C30 1.28(2) 2_566 ?
C29 N6 1.367(6) . ?
C29 C30 1.3900 . ?
C29 C29 1.84(2) 2_566 ?
C30 N6 0.62(2) 2_566 ?
C30 C29 1.28(2) 2_566 ?
C30 C30 1.93(3) 2_566 ?
N6 C30 0.62(3) 2_566 ?
N6 C26 1.30(2) 2_566 ?

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
As44 As4 O4 101.2(6) . 2_667 ?
As44 As4 O3 85.4(5) . . ?
O4 As4 O3 98.1(3) 2_667 . ?
As44 As4 O13 12.0(5) . . ?
O4 As4 O13 98.9(3) 2_667 . ?
O3 As4 O13 97.4(3) . . ?
As44 As4 V11 146.1(6) . 2_667 ?
O4 As4 V11 45.8(2) 2_667 2_667 ?
O3 As4 V11 104.3(2) . 2_667 ?
O13 As4 V11 140.2(3) . 2_667 ?
As4 As44 O13 161.1(8) . . ?
As4 As44 O3 73.4(5) . . ?
O13 As44 O3 125.5(6) . . ?
As4 As44 O4 59.5(5) . 2_667 ?
O13 As44 O4 115.5(5) . 2_667 ?
O3 As44 O4 87.7(3) . 2_667 ?
As4 As44 As1 155.9(6) . . ?
O13 As44 As1 31.6(4) . . ?
O3 As44 As1 102.0(3) . . ?
O4 As44 As1 97.1(3) 2_667 . ?
As33 As3 O10 106.4(9) . 2_667 ?
As33 As3 O8 80.7(9) . . ?
O10 As3 O8 98.5(3) 2_667 . ?
As33 As3 O12 18.2(9) . . ?
O10 As3 O12 99.1(3) 2_667 . ?
O8 As3 O12 98.3(3) . . ?
As33 As3 V22 150.6(9) . 2_667 ?
O10 As3 V22 44.1(2) 2_667 2_667 ?
O8 As3 V22 100.1(2) . 2_667 ?
O12 As3 V22 140.9(3) . 2_667 ?
As3 As33 O12 153.2(13) . . ?
As3 As33 O8 80.1(9) . . ?
O12 As33 O8 125.5(6) . . ?
As3 As33 O10 57.2(8) . 2_667 ?
O12 As33 O10 110.2(6) . 2_667 ?
O8 As33 O10 89.8(4) . 2_667 ?
As3 As33 As2 153.7(10) . . ?
O12 As33 As2 30.4(4) . . ?
O8 As33 As2 100.0(4) . . ?
O10 As33 As2 96.6(3) 2_667 . ?
As22 As2 O12 131.0(5) . . ?
As22 As2 O9 37.5(5) . . ?
O12 As2 O9 99.4(3) . . ?
As22 As2 O7 73.5(4) . . ?
O12 As2 O7 100.8(3) . . ?
O9 As2 O7 98.2(3) . . ?
As22 As2 As33 113.5(4) . . ?
O12 As2 As33 21.1(3) . . ?
O9 As2 As33 89.0(3) . . ?
O7 As2 As33 84.3(2) . . ?
As2 As22 O9 105.5(7) . . ?
As2 As22 O7 70.8(4) . . ?
O9 As22 O7 131.5(7) . . ?
As2 As22 O58 141.2(6) . . ?
O9 As22 O58 112.6(7) . . ?
O7 As22 O58 88.6(4) . . ?
As2 As22 V1 157.3(6) . . ?
O9 As22 V1 61.8(5) . . ?
O7 As22 V1 131.9(4) . . ?
O58 As22 V1 52.4(2) . . ?
As2 As22 V4 107.9(5) . . ?
O9 As22 V4 138.9(6) . . ?
O7 As22 V4 45.3(2) . . ?
O58 As22 V4 43.4(2) . . ?
V1 As22 V4 92.3(3) . . ?
As11 As1 O13 134.2(5) . . ?
As11 As1 O15 42.4(5) . . ?
O13 As1 O15 101.2(3) . . ?
As11 As1 O16 69.6(5) . . ?
O13 As1 O16 99.5(3) . . ?
O15 As1 O16 99.4(3) . . ?
As11 As1 As44 115.3(4) . . ?
O13 As1 As44 20.5(3) . . ?
O15 As1 As44 89.6(2) . . ?
O16 As1 As44 84.9(2) . . ?
As1 As11 O15 97.0(7) . . ?
As1 As11 O16 72.1(5) . . ?
O15 As11 O16 131.8(7) . . ?
As1 As11 O62 146.1(6) . . ?
O15 As11 O62 114.8(6) . . ?
O16 As11 O62 93.0(5) . . ?
As1 As11 V2 149.7(7) . . ?
O15 As11 V2 62.3(5) . . ?
O16 As11 V2 138.1(5) . . ?
O62 As11 V2 53.7(3) . . ?
As1 As11 V4 111.7(5) . . ?
O15 As11 V4 144.5(6) . . ?
O16 As11 V4 47.6(3) . . ?
O62 As11 V4 45.5(2) . . ?
V2 As11 V4 96.4(3) . . ?
V22 V2 O63 56.3(4) . . ?
V22 V2 O60 68.7(3) . . ?
O63 V2 O60 108.0(4) . . ?
V22 V2 O62 139.7(3) . . ?
O63 V2 O62 107.0(3) . . ?
O60 V2 O62 86.2(2) . . ?
V22 V2 O15 129.7(3) . . ?
O63 V2 O15 106.0(4) . . ?
O60 V2 O15 145.7(3) . . ?
O62 V2 O15 88.7(3) . . ?
V22 V2 O10 67.2(3) . . ?
O63 V2 O10 106.7(4) . . ?
O60 V2 O10 88.6(3) . . ?
O62 V2 O10 145.8(3) . . ?
O15 V2 O10 76.9(3) . . ?
V22 V2 As11 156.1(4) . . ?
O63 V2 As11 106.8(4) . . ?
O60 V2 As11 135.2(3) . . ?
O62 V2 As11 57.1(3) . . ?
O15 V2 As11 32.3(3) . . ?
O10 V2 As11 107.2(3) . . ?
V22 V2 V3 105.2(3) . . ?
O63 V2 V3 112.3(3) . . ?
O60 V2 V3 43.62(17) . . ?
O62 V2 V3 42.64(17) . . ?
O15 V2 V3 124.3(2) . . ?
O10 V2 V3 125.0(2) . . ?
As11 V2 V3 96.9(2) . . ?
V22 V2 V7 99.8(3) . 2_667 ?
O63 V2 V7 112.1(3) . 2_667 ?
O60 V2 V7 120.21(17) . 2_667 ?
O62 V2 V7 120.22(18) . 2_667 ?
O15 V2 V7 38.39(19) . 2_667 ?
O10 V2 V7 38.53(18) . 2_667 ?
As11 V2 V7 69.2(2) . 2_667 ?
V3 V2 V7 135.58(7) . 2_667 ?
V2 V22 O63 80.3(5) . . ?
V2 V22 O60 76.5(3) . . ?
O63 V22 O60 126.3(5) . . ?
V2 V22 O10 79.7(4) . . ?
O63 V22 O10 127.3(5) . . ?
O60 V22 O10 95.1(3) . . ?
V2 V22 As3 114.2(3) . 2_667 ?
O63 V22 As3 150.8(5) . 2_667 ?
O60 V22 As3 82.6(3) . 2_667 ?
O10 V22 As3 40.8(2) . 2_667 ?
V11 V1 O64 50.0(4) . . ?
V11 V1 O61 75.8(3) . . ?
O64 V1 O61 106.3(3) . . ?
V11 V1 O58 141.8(3) . . ?
O64 V1 O58 107.0(3) . . ?
O61 V1 O58 85.4(3) . . ?
V11 V1 O4 67.2(3) . . ?
O64 V1 O4 106.1(4) . . ?
O61 V1 O4 89.6(3) . . ?
O58 V1 O4 146.6(3) . . ?
V11 V1 O9 124.2(4) . . ?
O64 V1 O9 106.4(3) . . ?
O61 V1 O9 147.0(3) . . ?
O58 V1 O9 88.9(3) . . ?
O4 V1 O9 77.6(3) . . ?
V11 V1 As22 146.1(3) . . ?
O64 V1 As22 106.4(3) . . ?
O61 V1 As22 138.0(3) . . ?
O58 V1 As22 60.2(3) . . ?
O4 V1 As22 105.8(3) . . ?
O9 V1 As22 29.6(3) . . ?
V11 V1 V3 110.8(3) . . ?
O64 V1 V3 111.9(3) . . ?
O61 V1 V3 42.38(17) . . ?
O58 V1 V3 43.02(18) . . ?
O4 V1 V3 124.68(19) . . ?
O9 V1 V3 124.8(2) . . ?
As22 V1 V3 100.4(2) . . ?
V11 V1 V7 96.0(3) . . ?
O64 V1 V7 110.8(3) . . ?
O61 V1 V7 122.22(17) . . ?
O58 V1 V7 121.98(18) . . ?
O4 V1 V7 38.57(19) . . ?
O9 V1 V7 39.07(19) . . ?
As22 V1 V7 67.8(2) . . ?
V3 V1 V7 137.35(7) . . ?
V1 V11 O64 83.1(5) . . ?
V1 V11 O4 77.5(3) . . ?
O64 V11 O4 134.3(6) . . ?
V1 V11 O61 69.0(3) . . ?
O64 V11 O61 120.2(6) . . ?
O4 V11 O61 90.7(3) . . ?
V1 V11 As4 112.1(3) . 2_667 ?
O64 V11 As4 157.7(5) . 2_667 ?
O4 V11 As4 42.3(2) . 2_667 ?
O61 V11 As4 81.4(2) . 2_667 ?
N1 Co1 N3 99.9(3) . . ?
N1 Co1 N2 79.3(3) . . ?
N3 Co1 N2 102.4(3) . . ?
N1 Co1 O34 163.7(3) . . ?
N3 Co1 O34 95.1(3) . . ?
N2 Co1 O34 91.4(3) . . ?
N1 Co1 N4 100.4(3) . . ?
N3 Co1 N4 78.9(3) . . ?
N2 Co1 N4 178.7(3) . . ?
O34 Co1 N4 88.6(3) . . ?
N1 Co1 O36 87.9(3) . . ?
N3 Co1 O36 169.0(3) . . ?
N2 Co1 O36 86.6(3) . . ?
O34 Co1 O36 78.2(2) . . ?
N4 Co1 O36 92.1(3) . . ?
O17 V7 O15 105.0(3) . 2_667 ?
O17 V7 O10 105.3(3) . 2_667 ?
O15 V7 O10 78.1(3) 2_667 2_667 ?
O17 V7 O4 106.8(3) . . ?
O15 V7 O4 93.0(3) 2_667 . ?
O10 V7 O4 147.9(3) 2_667 . ?
O17 V7 O9 105.2(3) . . ?
O15 V7 O9 149.8(3) 2_667 . ?
O10 V7 O9 94.7(3) 2_667 . ?
O4 V7 O9 77.6(3) . . ?
O17 V7 V1 110.4(2) . . ?
O15 V7 V1 126.0(2) 2_667 . ?
O10 V7 V1 126.9(2) 2_667 . ?
O4 V7 V1 38.58(19) . . ?
O9 V7 V1 38.99(19) . . ?
O17 V7 V2 110.7(2) . 2_667 ?
O15 V7 V2 38.9(2) 2_667 2_667 ?
O10 V7 V2 39.22(19) 2_667 2_667 ?
O4 V7 V2 124.57(19) . 2_667 ?
O9 V7 V2 126.9(2) . 2_667 ?
V1 V7 V2 138.85(6) . 2_667 ?
O18 V6 O7 106.5(3) . . ?
O18 V6 O8 107.0(3) . . ?
O7 V6 O8 92.8(2) . . ?
O18 V6 O16 106.2(3) . . ?
O7 V6 O16 78.3(2) . . ?
O8 V6 O16 146.9(2) . . ?
O18 V6 O3 105.9(3) . . ?
O7 V6 O3 147.6(2) . . ?
O8 V6 O3 77.9(2) . . ?
O16 V6 O3 92.6(2) . . ?
O18 V6 V4 110.9(2) . . ?
O7 V6 V4 39.19(16) . . ?
O8 V6 V4 125.15(17) . . ?
O16 V6 V4 39.12(17) . . ?
O3 V6 V4 125.25(17) . . ?
O18 V6 V5 111.0(2) . 2_667 ?
O7 V6 V5 125.25(16) . 2_667 ?
O8 V6 V5 38.93(16) . 2_667 ?
O16 V6 V5 124.77(17) . 2_667 ?
O3 V6 V5 38.92(15) . 2_667 ?
V4 V6 V5 138.13(6) . 2_667 ?
O56 V5 O61 108.4(3) . . ?
O56 V5 O60 107.3(3) . . ?
O61 V5 O60 82.2(2) . . ?
O56 V5 O3 105.5(3) . 2_667 ?
O61 V5 O3 90.5(2) . 2_667 ?
O60 V5 O3 147.0(2) . 2_667 ?
O56 V5 O8 106.2(3) . 2_667 ?
O61 V5 O8 145.2(2) . 2_667 ?
O60 V5 O8 91.0(2) . 2_667 ?
O3 V5 O8 76.9(2) 2_667 2_667 ?
O56 V5 V3 112.8(2) . . ?
O61 V5 V3 40.79(17) . . ?
O60 V5 V3 41.42(17) . . ?
O3 V5 V3 124.74(17) 2_667 . ?
O8 V5 V3 124.88(17) 2_667 . ?
O56 V5 V6 110.1(2) . 2_667 ?
O61 V5 V6 122.28(17) . 2_667 ?
O60 V5 V6 123.22(17) . 2_667 ?
O3 V5 V6 38.59(15) 2_667 2_667 ?
O8 V5 V6 38.34(15) 2_667 2_667 ?
V3 V5 V6 137.13(6) . 2_667 ?
O57 V4 O58 107.8(3) . . ?
O57 V4 O62 107.8(3) . . ?
O58 V4 O62 83.6(3) . . ?
O57 V4 O16 106.7(3) . . ?
O58 V4 O16 145.3(2) . . ?
O62 V4 O16 89.2(2) . . ?
O57 V4 O7 106.6(3) . . ?
O58 V4 O7 89.5(2) . . ?
O62 V4 O7 145.3(2) . . ?
O16 V4 O7 77.4(2) . . ?
O57 V4 As11 111.9(3) . . ?
O58 V4 As11 124.5(3) . . ?
O62 V4 As11 48.4(2) . . ?
O16 V4 As11 40.9(2) . . ?
O7 V4 As11 113.5(2) . . ?
O57 V4 As22 112.2(3) . . ?
O58 V4 As22 49.4(2) . . ?
O62 V4 As22 125.0(2) . . ?
O16 V4 As22 112.6(2) . . ?
O7 V4 As22 40.2(2) . . ?
As11 V4 As22 134.1(2) . . ?
O57 V4 V3 112.9(3) . . ?
O58 V4 V3 42.27(18) . . ?
O62 V4 V3 41.31(17) . . ?
O16 V4 V3 123.34(18) . . ?
O7 V4 V3 124.34(17) . . ?
As11 V4 V3 86.32(19) . . ?
As22 V4 V3 88.00(17) . . ?
O57 V4 V6 111.2(3) . . ?
O58 V4 V6 121.62(17) . . ?
O62 V4 V6 121.53(17) . . ?
O16 V4 V6 38.78(16) . . ?
O7 V4 V6 38.64(15) . . ?
As11 V4 V6 76.97(19) . . ?
As22 V4 V6 76.02(17) . . ?
V3 V4 V6 135.93(6) . . ?
O59 V3 O62 111.3(3) . . ?
O59 V3 O61 109.6(3) . . ?
O62 V3 O61 139.1(2) . . ?
O59 V3 O58 109.1(3) . . ?
O62 V3 O58 82.8(2) . . ?
O61 V3 O58 84.0(2) . . ?
O59 V3 O60 109.6(3) . . ?
O62 V3 O60 84.9(2) . . ?
O61 V3 O60 81.7(2) . . ?
O58 V3 O60 141.2(2) . . ?
O59 V3 V2 116.3(3) . . ?
O62 V3 V2 43.01(17) . . ?
O61 V3 V2 115.45(17) . . ?
O58 V3 V2 117.98(18) . . ?
O60 V3 V2 42.00(16) . . ?
O59 V3 V1 115.5(3) . . ?
O62 V3 V1 116.18(18) . . ?
O61 V3 V1 41.42(17) . . ?
O58 V3 V1 42.57(17) . . ?
O60 V3 V1 115.51(17) . . ?
V2 V3 V1 128.20(7) . . ?
O59 V3 V4 116.1(3) . . ?
O62 V3 V4 41.34(17) . . ?
O61 V3 V4 116.64(18) . . ?
O58 V3 V4 41.45(17) . . ?
O60 V3 V4 118.27(17) . . ?
V2 V3 V4 80.41(6) . . ?
V1 V3 V4 79.25(6) . . ?
O59 V3 V5 115.1(3) . . ?
O62 V3 V5 117.08(17) . . ?
O61 V3 V5 40.82(16) . . ?
O58 V3 V5 117.26(17) . . ?
O60 V3 V5 40.91(16) . . ?
V2 V3 V5 78.59(6) . . ?
V1 V3 V5 78.26(6) . . ?
V4 V3 V5 128.81(6) . . ?
As11 O15 As1 40.6(4) . . ?
As11 O15 V7 156.8(6) . 2_667 ?
As1 O15 V7 134.9(4) . 2_667 ?
As11 O15 V2 85.4(5) . . ?
As1 O15 V2 122.3(3) . . ?
V7 O15 V2 102.7(3) 2_667 . ?
As11 O16 As1 38.2(3) . . ?
As11 O16 V6 149.5(4) . . ?
As1 O16 V6 136.0(3) . . ?
As11 O16 V4 91.4(4) . . ?
As1 O16 V4 121.8(3) . . ?
V6 O16 V4 102.1(2) . . ?
As4 O3 As44 21.22(19) . . ?
As4 O3 V6 138.1(3) . . ?
As44 O3 V6 116.9(3) . . ?
As4 O3 V5 119.2(3) . 2_667 ?
As44 O3 V5 140.4(4) . 2_667 ?
V6 O3 V5 102.5(2) . 2_667 ?
As2 O7 As22 35.7(3) . . ?
As2 O7 V6 135.6(3) . . ?
As22 O7 V6 147.3(4) . . ?
As2 O7 V4 122.0(3) . . ?
As22 O7 V4 94.5(4) . . ?
V6 O7 V4 102.2(2) . . ?
V4 O58 V1 143.2(3) . . ?
V4 O58 V3 96.3(2) . . ?
V1 O58 V3 94.4(3) . . ?
V4 O58 As22 87.2(3) . . ?
V1 O58 As22 67.4(3) . . ?
V3 O58 As22 150.8(4) . . ?
C25 O36 Co1 113.5(5) . . ?
V22 O60 V2 34.8(2) . . ?
V22 O60 V5 139.0(4) . . ?
V2 O60 V5 144.1(3) . . ?
V22 O60 V3 121.9(3) . . ?
V2 O60 V3 94.4(3) . . ?
V5 O60 V3 97.7(2) . . ?
V1 O61 V3 96.2(3) . . ?
V1 O61 V5 144.3(3) . . ?
V3 O61 V5 98.4(2) . . ?
V1 O61 V11 35.1(2) . . ?
V3 O61 V11 123.8(3) . . ?
V5 O61 V11 136.9(3) . . ?
C25 O34 Co1 113.3(5) 2_756 . ?
As3 O8 As33 19.1(2) . . ?
As3 O8 V6 138.1(3) . . ?
As33 O8 V6 119.0(4) . . ?
As3 O8 V5 119.1(3) . 2_667 ?
As33 O8 V5 138.3(4) . 2_667 ?
V6 O8 V5 102.7(2) . 2_667 ?
As22 O9 As2 37.0(5) . . ?
As22 O9 V1 88.7(6) . . ?
As2 O9 V1 123.1(4) . . ?
As22 O9 V7 159.9(7) . . ?
As2 O9 V7 134.9(4) . . ?
V1 O9 V7 101.9(3) . . ?
V3 O62 V4 97.3(2) . . ?
V3 O62 V2 94.4(3) . . ?
V4 O62 V2 146.0(3) . . ?
V3 O62 As11 151.5(4) . . ?
V4 O62 As11 86.1(3) . . ?
V2 O62 As11 69.2(3) . . ?
C8 C9 C10 118.6(9) . . ?
C8 C9 H9A 120.7 . . ?
C10 C9 H9A 120.7 . . ?
As3 O10 V22 95.0(4) 2_667 . ?
As3 O10 V7 135.2(4) 2_667 2_667 ?
V22 O10 V7 128.2(4) . 2_667 ?
As3 O10 V2 122.3(3) 2_667 . ?
V22 O10 V2 33.1(2) . . ?
V7 O10 V2 102.2(3) 2_667 . ?
As3 O10 As33 16.4(2) 2_667 2_667 ?
V22 O10 As33 111.4(4) . 2_667 ?
V7 O10 As33 119.3(4) 2_667 2_667 ?
V2 O10 As33 137.3(4) . 2_667 ?
As4 O4 V11 91.9(3) 2_667 . ?
As4 O4 V7 137.2(4) 2_667 . ?
V11 O4 V7 125.6(4) . . ?
As4 O4 V1 119.9(3) 2_667 . ?
V11 O4 V1 35.3(2) . . ?
V7 O4 V1 102.9(3) . . ?
As4 O4 As44 19.23(18) 2_667 2_667 ?
V11 O4 As44 110.9(4) . 2_667 ?
V7 O4 As44 118.6(4) . 2_667 ?
V1 O4 As44 138.4(4) . 2_667 ?
V22 O63 V2 43.4(3) . . ?
C1 N1 C12 119.6(8) . . ?
C1 N1 Co1 128.2(7) . . ?
C12 N1 Co1 111.5(5) . . ?
C10 N2 C11 117.7(7) . . ?
C10 N2 Co1 129.1(6) . . ?
C11 N2 Co1 112.1(6) . . ?
C13 N3 C24 118.6(8) . . ?
C13 N3 Co1 128.1(6) . . ?
C24 N3 Co1 113.2(5) . . ?
As44 O13 As1 127.9(6) . . ?
As44 O13 As4 6.9(3) . . ?
As1 O13 As4 132.0(4) . . ?
C11 C7 C8 116.9(9) . . ?
C11 C7 C6 119.5(10) . . ?
C8 C7 C6 123.6(9) . . ?
N2 C11 C7 122.6(8) . . ?
N2 C11 C12 116.7(7) . . ?
C7 C11 C12 120.7(8) . . ?
As33 O12 As2 128.5(6) . . ?
As33 O12 As3 8.5(4) . . ?
As2 O12 As3 132.9(4) . . ?
C3 C4 C12 117.0(10) . . ?
C3 C4 C5 124.6(10) . . ?
C12 C4 C5 118.3(10) . . ?
C3 C2 C1 121.4(10) . . ?
C3 C2 H2A 119.3 . . ?
C1 C2 H2A 119.3 . . ?
V11 O64 V1 46.9(4) . . ?
C2 C3 C4 119.7(10) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C22 N4 C23 118.1(8) . . ?
C22 N4 Co1 129.4(7) . . ?
C23 N4 Co1 112.1(6) . . ?
N2 C10 C9 123.6(9) . . ?
N2 C10 H10A 118.2 . . ?
C9 C10 H10A 118.2 . . ?
C14 C15 C16 119.6(10) . . ?
C14 C15 H15A 120.2 . . ?
C16 C15 H15A 120.2 . . ?
C5 C6 C7 119.8(10) . . ?
C5 C6 H6A 120.1 . . ?
C7 C6 H6A 120.1 . . ?
C15 C14 C13 120.8(10) . . ?
C15 C14 H14A 119.6 . . ?
C13 C14 H14A 119.6 . . ?
N1 C12 C4 121.8(8) . . ?
N1 C12 C11 119.0(7) . . ?
C4 C12 C11 119.2(9) . . ?
C9 C8 C7 120.5(9) . . ?
C9 C8 H8A 119.7 . . ?
C7 C8 H8A 119.7 . . ?
N3 C24 C16 122.6(8) . . ?
N3 C24 C23 117.4(7) . . ?
C16 C24 C23 120.0(8) . . ?
C21 C20 C19 119.4(10) . . ?
C21 C20 H20A 120.3 . . ?
C19 C20 H20A 120.3 . . ?
O34 C25 O36 125.1(7) 2_756 . ?
O34 C25 C25 118.6(9) 2_756 2_756 ?
O36 C25 C25 116.3(9) . 2_756 ?
C6 C5 C4 122.4(10) . . ?
C6 C5 H5A 118.8 . . ?
C4 C5 H5A 118.8 . . ?
C24 C16 C15 117.1(8) . . ?
C24 C16 C17 118.5(9) . . ?
C15 C16 C17 124.4(9) . . ?
N4 C23 C19 121.4(9) . . ?
N4 C23 C24 118.2(7) . . ?
C19 C23 C24 120.4(9) . . ?
C20 C21 C22 118.1(11) . . ?
C20 C21 H21A 120.9 . . ?
C22 C21 H21A 120.9 . . ?
N4 C22 C21 124.3(11) . . ?
N4 C22 H22A 117.8 . . ?
C21 C22 H22A 117.8 . . ?
N3 C13 C14 121.2(9) . . ?
N3 C13 H13A 119.4 . . ?
C14 C13 H13A 119.4 . . ?
C17 C18 C19 120.8(9) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C20 C19 C23 118.6(10) . . ?
C20 C19 C18 123.5(9) . . ?
C23 C19 C18 117.9(10) . . ?
C18 C17 C16 122.4(10) . . ?
C18 C17 H17A 118.8 . . ?
C16 C17 H17A 118.8 . . ?
C32 N7 C33 123.6(16) . . ?
N7 C33 C32 117.6(19) . 2_676 ?
N1 C1 C2 120.5(10) . . ?
N1 C1 H1A 119.8 . . ?
C2 C1 H1A 119.8 . . ?
H1O2 O2W H2O2 107.6 . . ?
N7 C32 C33 118.8(18) . 2_676 ?
N7 C32 N8 119.1(19) . . ?
C33 C32 N8 122(2) 2_676 . ?
N6 C26 C27 145.7(11) 2_566 . ?
N6 C26 C30 26.3(11) 2_566 . ?
C27 C26 C30 120.0 . . ?
C26 C27 C28 120.0 . . ?
N5 C28 C27 120.0 . . ?
C29 N5 C28 120.0 . . ?
C30 C29 N6 26.7(13) 2_566 . ?
C30 C29 C30 92.7(14) 2_566 . ?
N6 C29 C30 119.1(6) . . ?
C30 C29 N5 147.2(14) 2_566 . ?
N6 C29 N5 120.9(6) . . ?
C30 C29 N5 120.0 . . ?
C30 C29 C29 48.8(7) 2_566 2_566 ?
N6 C29 C29 75.3(10) . 2_566 ?
C30 C29 C29 43.9(11) . 2_566 ?
N5 C29 C29 163.8(11) . 2_566 ?
N6 C30 C29 84(2) 2_566 2_566 ?
N6 C30 C29 168(3) 2_566 . ?
C29 C30 C29 87.3(14) 2_566 . ?
N6 C30 C26 68(2) 2_566 . ?
C29 C30 C26 152.6(14) 2_566 . ?
C29 C30 C26 120.0 . . ?
N6 C30 C30 130(2) 2_566 2_566 ?
C29 C30 C30 45.9(8) 2_566 2_566 ?
C29 C30 C30 41.4(8) . 2_566 ?
C26 C30 C30 161.3(8) . 2_566 ?
C30 N6 C26 85(2) 2_566 2_566 ?
C30 N6 C29 68.9(19) 2_566 . ?
C26 N6 C29 154.3(14) 2_566 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 As4 As44 O13 -80(3) 2_667 . . . ?
O3 As4 As44 O13 -177(3) . . . . ?
V11 As4 As44 O13 -68(3) 2_667 . . . ?
O4 As4 As44 O3 97.3(3) 2_667 . . . ?
O13 As4 As44 O3 177(3) . . . . ?
V11 As4 As44 O3 109.0(8) 2_667 . . . ?
O3 As4 As44 O4 -97.3(3) . . . 2_667 ?
O13 As4 As44 O4 80(3) . . . 2_667 ?
V11 As4 As44 O4 11.6(7) 2_667 . . 2_667 ?
O4 As4 As44 As1 15.3(16) 2_667 . . . ?
O3 As4 As44 As1 -82.1(15) . . . . ?
O13 As4 As44 As1 95(3) . . . . ?
V11 As4 As44 As1 27(2) 2_667 . . . ?
O10 As3 As33 O12 68(3) 2_667 . . . ?
O8 As3 As33 O12 165(3) . . . . ?
V22 As3 As33 O12 70(4) 2_667 . . . ?
O10 As3 As33 O8 -96.2(4) 2_667 . . . ?
O12 As3 As33 O8 -165(3) . . . . ?
V22 As3 As33 O8 -94.1(17) 2_667 . . . ?
O8 As3 As33 O10 96.2(4) . . . 2_667 ?
O12 As3 As33 O10 -68(3) . . . 2_667 ?
V22 As3 As33 O10 2.1(14) 2_667 . . 2_667 ?
O10 As3 As33 As2 -4(2) 2_667 . . . ?
O8 As3 As33 As2 93(2) . . . . ?
O12 As3 As33 As2 -72(3) . . . . ?
V22 As3 As33 As2 -1(4) 2_667 . . . ?
O12 As2 As22 O9 39.1(9) . . . . ?
O7 As2 As22 O9 129.2(7) . . . . ?
As33 As2 As22 O9 53.2(7) . . . . ?
O12 As2 As22 O7 -90.0(5) . . . . ?
O9 As2 As22 O7 -129.2(7) . . . . ?
As33 As2 As22 O7 -75.9(4) . . . . ?
O12 As2 As22 O58 -151.8(7) . . . . ?
O9 As2 As22 O58 169.1(14) . . . . ?
O7 As2 As22 O58 -61.8(8) . . . . ?
As33 As2 As22 O58 -137.7(8) . . . . ?
O12 As2 As22 V1 91.6(15) . . . . ?
O9 As2 As22 V1 52.4(13) . . . . ?
O7 As2 As22 V1 -178.4(16) . . . . ?
As33 As2 As22 V1 105.7(14) . . . . ?
O12 As2 As22 V4 -116.5(5) . . . . ?
O9 As2 As22 V4 -155.7(9) . . . . ?
O7 As2 As22 V4 -26.5(3) . . . . ?
As33 As2 As22 V4 -102.4(4) . . . . ?
O13 As1 As11 O15 -48.4(10) . . . . ?
O16 As1 As11 O15 -131.8(7) . . . . ?
As44 As1 As11 O15 -58.0(7) . . . . ?
O13 As1 As11 O16 83.4(6) . . . . ?
O15 As1 As11 O16 131.8(7) . . . . ?
As44 As1 As11 O16 73.8(4) . . . . ?
O13 As1 As11 O62 151.1(9) . . . . ?
O15 As1 As11 O62 -160.6(16) . . . . ?
O16 As1 As11 O62 67.6(11) . . . . ?
As44 As1 As11 O62 141.4(10) . . . . ?
O13 As1 As11 V2 -92.6(12) . . . . ?
O15 As1 As11 V2 -44.2(9) . . . . ?
O16 As1 As11 V2 -176.0(13) . . . . ?
As44 As1 As11 V2 -102.2(11) . . . . ?
O13 As1 As11 V4 110.5(6) . . . . ?
O15 As1 As11 V4 158.8(9) . . . . ?
O16 As1 As11 V4 27.1(3) . . . . ?
As44 As1 As11 V4 100.9(4) . . . . ?
O60 V2 V22 O63 131.2(5) . . . . ?
O62 V2 V22 O63 76.0(6) . . . . ?
O15 V2 V22 O63 -82.9(5) . . . . ?
O10 V2 V22 O63 -131.0(5) . . . . ?
As11 V2 V22 O63 -49.9(10) . . . . ?
V3 V2 V22 O63 106.9(4) . . . . ?
V7 V2 V22 O63 -110.1(4) 2_667 . . . ?
O63 V2 V22 O60 -131.2(5) . . . . ?
O62 V2 V22 O60 -55.2(5) . . . . ?
O15 V2 V22 O60 145.9(4) . . . . ?
O10 V2 V22 O60 97.8(3) . . . . ?
As11 V2 V22 O60 178.9(8) . . . . ?
V3 V2 V22 O60 -24.3(2) . . . . ?
V7 V2 V22 O60 118.7(2) 2_667 . . . ?
O63 V2 V22 O10 131.0(5) . . . . ?
O60 V2 V22 O10 -97.8(3) . . . . ?
O62 V2 V22 O10 -153.0(4) . . . . ?
O15 V2 V22 O10 48.1(4) . . . . ?
As11 V2 V22 O10 81.1(9) . . . . ?
V3 V2 V22 O10 -122.1(2) . . . . ?
V7 V2 V22 O10 20.9(3) 2_667 . . . ?
O63 V2 V22 As3 153.4(5) . . . 2_667 ?
O60 V2 V22 As3 -75.4(3) . . . 2_667 ?
O62 V2 V22 As3 -130.6(4) . . . 2_667 ?
O15 V2 V22 As3 70.5(5) . . . 2_667 ?
O10 V2 V22 As3 22.4(3) . . . 2_667 ?
As11 V2 V22 As3 103.5(8) . . . 2_667 ?
V3 V2 V22 As3 -99.7(2) . . . 2_667 ?
V7 V2 V22 As3 43.3(3) 2_667 . . 2_667 ?
O61 V1 V11 O64 -126.1(5) . . . . ?
O58 V1 V11 O64 -63.2(7) . . . . ?
O4 V1 V11 O64 138.3(5) . . . . ?
O9 V1 V11 O64 82.9(5) . . . . ?
As22 V1 V11 O64 53.8(8) . . . . ?
V3 V1 V11 O64 -101.6(5) . . . . ?
V7 V1 V11 O64 112.1(4) . . . . ?
O64 V1 V11 O4 -138.3(5) . . . . ?
O61 V1 V11 O4 95.6(3) . . . . ?
O58 V1 V11 O4 158.5(4) . . . . ?
O9 V1 V11 O4 -55.4(4) . . . . ?
As22 V1 V11 O4 -84.5(6) . . . . ?
V3 V1 V11 O4 120.0(2) . . . . ?
V7 V1 V11 O4 -26.2(2) . . . . ?
O64 V1 V11 O61 126.1(5) . . . . ?
O58 V1 V11 O61 62.9(5) . . . . ?
O4 V1 V11 O61 -95.6(3) . . . . ?
O9 V1 V11 O61 -151.0(3) . . . . ?
As22 V1 V11 O61 179.9(6) . . . . ?
V3 V1 V11 O61 24.5(2) . . . . ?
V7 V1 V11 O61 -121.75(18) . . . . ?
O64 V1 V11 As4 -163.1(6) . . . 2_667 ?
O61 V1 V11 As4 70.8(3) . . . 2_667 ?
O58 V1 V11 As4 133.7(4) . . . 2_667 ?
O4 V1 V11 As4 -24.8(3) . . . 2_667 ?
O9 V1 V11 As4 -80.3(4) . . . 2_667 ?
As22 V1 V11 As4 -109.3(5) . . . 2_667 ?
V3 V1 V11 As4 95.2(3) . . . 2_667 ?
V7 V1 V11 As4 -51.0(3) . . . 2_667 ?
O16 As11 O15 As1 -72.3(8) . . . . ?
O62 As11 O15 As1 168.2(10) . . . . ?
V2 As11 O15 As1 156.6(5) . . . . ?
V4 As11 O15 As1 -144.7(14) . . . . ?
As1 As11 O15 V7 91.6(16) . . . 2_667 ?
O16 As11 O15 V7 19(2) . . . 2_667 ?
O62 As11 O15 V7 -100.2(16) . . . 2_667 ?
V2 As11 O15 V7 -111.8(16) . . . 2_667 ?
V4 As11 O15 V7 -53(2) . . . 2_667 ?
As1 As11 O15 V2 -156.6(5) . . . . ?
O16 As11 O15 V2 131.1(8) . . . . ?
O62 As11 O15 V2 11.6(5) . . . . ?
V4 As11 O15 V2 58.7(10) . . . . ?
O13 As1 O15 As11 146.9(7) . . . . ?
O16 As1 O15 As11 45.1(7) . . . . ?
As44 As1 O15 As11 129.9(7) . . . . ?
As11 As1 O15 V7 -146.3(9) . . . 2_667 ?
O13 As1 O15 V7 0.6(6) . . . 2_667 ?
O16 As1 O15 V7 -101.2(5) . . . 2_667 ?
As44 As1 O15 V7 -16.4(5) . . . 2_667 ?
As11 As1 O15 V2 27.9(7) . . . . ?
O13 As1 O15 V2 174.8(4) . . . . ?
O16 As1 O15 V2 73.1(4) . . . . ?
As44 As1 O15 V2 157.9(4) . . . . ?
O15 As11 O16 As1 83.4(9) . . . . ?
O62 As11 O16 As1 -148.9(6) . . . . ?
V2 As11 O16 As1 177.0(10) . . . . ?
V4 As11 O16 As1 -145.1(4) . . . . ?
As1 As11 O16 V6 -97.8(8) . . . . ?
O15 As11 O16 V6 -14.5(15) . . . . ?
O62 As11 O16 V6 113.2(8) . . . . ?
V2 As11 O16 V6 79.1(11) . . . . ?
V4 As11 O16 V6 117.1(8) . . . . ?
As1 As11 O16 V4 145.1(4) . . . . ?
O15 As11 O16 V4 -131.5(8) . . . . ?
O62 As11 O16 V4 -3.8(3) . . . . ?
V2 As11 O16 V4 -37.9(7) . . . . ?
O13 As1 O16 As11 -133.8(5) . . . . ?
O15 As1 O16 As11 -30.6(5) . . . . ?
As44 As1 O16 As11 -119.4(5) . . . . ?
As11 As1 O16 V6 133.5(6) . . . . ?
O13 As1 O16 V6 -0.3(5) . . . . ?
O15 As1 O16 V6 102.9(5) . . . . ?
As44 As1 O16 V6 14.2(4) . . . . ?
As11 As1 O16 V4 -42.3(5) . . . . ?
O13 As1 O16 V4 -176.1(4) . . . . ?
O15 As1 O16 V4 -72.9(4) . . . . ?
As44 As1 O16 V4 -161.7(4) . . . . ?
O4 As4 O3 As44 -100.7(6) 2_667 . . . ?
O13 As4 O3 As44 -0.6(6) . . . . ?
V11 As4 O3 As44 -147.0(6) 2_667 . . . ?
As44 As4 O3 V6 1.6(7) . . . . ?
O4 As4 O3 V6 -99.1(5) 2_667 . . . ?
O13 As4 O3 V6 1.0(5) . . . . ?
V11 As4 O3 V6 -145.4(4) 2_667 . . . ?
As44 As4 O3 V5 176.1(6) . . . 2_667 ?
O4 As4 O3 V5 75.4(4) 2_667 . . 2_667 ?
O13 As4 O3 V5 175.5(3) . . . 2_667 ?
V11 As4 O3 V5 29.1(4) 2_667 . . 2_667 ?
O13 As44 O3 As4 178.9(10) . . . . ?
O4 As44 O3 As4 58.8(5) 2_667 . . . ?
As1 As44 O3 As4 155.6(7) . . . . ?
As4 As44 O3 V6 -178.8(5) . . . . ?
O13 As44 O3 V6 0.1(8) . . . . ?
O4 As44 O3 V6 -120.0(4) 2_667 . . . ?
As1 As44 O3 V6 -23.2(4) . . . . ?
As4 As44 O3 V5 -5.4(8) . . . 2_667 ?
O13 As44 O3 V5 173.5(6) . . . 2_667 ?
O4 As44 O3 V5 53.5(6) 2_667 . . 2_667 ?
As1 As44 O3 V5 150.2(4) . . . 2_667 ?
O12 As2 O7 As22 129.8(5) . . . . ?
O9 As2 O7 As22 28.5(5) . . . . ?
As33 As2 O7 As22 116.7(5) . . . . ?
As22 As2 O7 V6 -129.8(6) . . . . ?
O12 As2 O7 V6 0.0(5) . . . . ?
O9 As2 O7 V6 -101.3(5) . . . . ?
As33 As2 O7 V6 -13.1(4) . . . . ?
As22 As2 O7 V4 44.6(5) . . . . ?
O12 As2 O7 V4 174.4(4) . . . . ?
O9 As2 O7 V4 73.1(4) . . . . ?
As33 As2 O7 V4 161.3(4) . . . . ?
O9 As22 O7 As2 -94.0(10) . . . . ?
O58 As22 O7 As2 146.5(5) . . . . ?
V1 As22 O7 As2 179.2(8) . . . . ?
V4 As22 O7 As2 143.3(4) . . . . ?
As2 As22 O7 V6 95.7(7) . . . . ?
O9 As22 O7 V6 1.7(14) . . . . ?
O58 As22 O7 V6 -117.8(7) . . . . ?
V1 As22 O7 V6 -85.1(9) . . . . ?
V4 As22 O7 V6 -120.9(8) . . . . ?
As2 As22 O7 V4 -143.3(4) . . . . ?
O9 As22 O7 V4 122.7(9) . . . . ?
O58 As22 O7 V4 3.2(3) . . . . ?
V1 As22 O7 V4 35.8(6) . . . . ?
O63 V22 O60 V2 -67.0(7) . . . . ?
O10 V22 O60 V2 78.1(3) . . . . ?
As3 V22 O60 V2 117.1(3) 2_667 . . . ?
V2 V22 O60 V5 -120.5(5) . . . . ?
O63 V22 O60 V5 172.5(6) . . . . ?
O10 V22 O60 V5 -42.4(6) . . . . ?
As3 V22 O60 V5 -3.4(5) 2_667 . . . ?
V2 V22 O60 V3 42.5(4) . . . . ?
O63 V22 O60 V3 -24.5(8) . . . . ?
O10 V22 O60 V3 120.6(4) . . . . ?
As3 V22 O60 V3 159.5(3) 2_667 . . . ?
O10 As3 O8 As33 105.4(9) 2_667 . . . ?
O12 As3 O8 As33 4.8(9) . . . . ?
V22 As3 O8 As33 150.1(9) 2_667 . . . ?
As33 As3 O8 V6 -1.6(10) . . . . ?
O10 As3 O8 V6 103.8(5) 2_667 . . . ?
O12 As3 O8 V6 3.2(5) . . . . ?
V22 As3 O8 V6 148.5(4) 2_667 . . . ?
As33 As3 O8 V5 -179.7(9) . . . 2_667 ?
O10 As3 O8 V5 -74.3(4) 2_667 . . 2_667 ?
O12 As3 O8 V5 -174.9(4) . . . 2_667 ?
V22 As3 O8 V5 -29.6(3) 2_667 . . 2_667 ?
O12 As33 O8 As3 -171.6(15) . . . . ?
O10 As33 O8 As3 -56.7(8) 2_667 . . . ?
As2 As33 O8 As3 -153.3(11) . . . . ?
As3 As33 O8 V6 178.8(8) . . . . ?
O12 As33 O8 V6 7.2(10) . . . . ?
O10 As33 O8 V6 122.1(4) 2_667 . . . ?
As2 As33 O8 V6 25.5(5) . . . . ?
As3 As33 O8 V5 0.4(12) . . . 2_667 ?
O12 As33 O8 V5 -171.2(6) . . . 2_667 ?
O10 As33 O8 V5 -56.3(7) 2_667 . . 2_667 ?
As2 As33 O8 V5 -153.0(4) . . . 2_667 ?
O7 As22 O9 As2 77.9(9) . . . . ?
O58 As22 O9 As2 -172.6(9) . . . . ?
V1 As22 O9 As2 -159.7(5) . . . . ?
V4 As22 O9 As2 143.4(13) . . . . ?
As2 As22 O9 V1 159.7(5) . . . . ?
O7 As22 O9 V1 -122.4(8) . . . . ?
O58 As22 O9 V1 -12.9(5) . . . . ?
V4 As22 O9 V1 -57.0(9) . . . . ?
As2 As22 O9 V7 -77.7(19) . . . . ?
O7 As22 O9 V7 0(2) . . . . ?
O58 As22 O9 V7 109.7(18) . . . . ?
V1 As22 O9 V7 122.6(19) . . . . ?
V4 As22 O9 V7 66(2) . . . . ?
O12 As2 O9 As22 -151.1(7) . . . . ?
O7 As2 O9 As22 -48.7(7) . . . . ?
As33 As2 O9 As22 -132.7(7) . . . . ?
As22 As2 O9 V1 -24.5(7) . . . . ?
O12 As2 O9 V1 -175.6(4) . . . . ?
O7 As2 O9 V1 -73.2(4) . . . . ?
As33 As2 O9 V1 -157.2(4) . . . . ?
As22 As2 O9 V7 151.7(10) . . . . ?
O12 As2 O9 V7 0.6(5) . . . . ?
O7 As2 O9 V7 103.0(5) . . . . ?
As33 As2 O9 V7 19.0(5) . . . . ?
V2 V22 O10 As3 147.9(4) . . . 2_667 ?
O63 V22 O10 As3 -142.9(6) . . . 2_667 ?
O60 V22 O10 As3 72.6(4) . . . 2_667 ?
V2 V22 O10 V7 -44.6(5) . . . 2_667 ?
O63 V22 O10 V7 24.6(9) . . . 2_667 ?
O60 V22 O10 V7 -119.9(5) . . . 2_667 ?
As3 V22 O10 V7 167.5(6) 2_667 . . 2_667 ?
O63 V22 O10 V2 69.2(7) . . . . ?
O60 V22 O10 V2 -75.3(3) . . . . ?
As3 V22 O10 V2 -147.9(4) 2_667 . . . ?
V2 V22 O10 As33 147.4(4) . . . 2_667 ?
O63 V22 O10 As33 -143.3(7) . . . 2_667 ?
O60 V22 O10 As33 72.2(5) . . . 2_667 ?
As3 V22 O10 As33 -0.4(3) 2_667 . . 2_667 ?
V1 V11 O4 As4 -144.7(3) . . . 2_667 ?
O64 V11 O4 As4 148.0(7) . . . 2_667 ?
O61 V11 O4 As4 -76.3(3) . . . 2_667 ?
V1 V11 O4 V7 57.5(5) . . . . ?
O64 V11 O4 V7 -9.8(10) . . . . ?
O61 V11 O4 V7 125.8(4) . . . . ?
As4 V11 O4 V7 -157.9(6) 2_667 . . . ?
O64 V11 O4 V1 -67.3(7) . . . . ?
O61 V11 O4 V1 68.3(3) . . . . ?
As4 V11 O4 V1 144.7(3) 2_667 . . . ?
V1 V11 O4 As44 -147.8(4) . . . 2_667 ?
O64 V11 O4 As44 144.9(7) . . . 2_667 ?
O61 V11 O4 As44 -79.5(4) . . . 2_667 ?
As4 V11 O4 As44 -3.2(2) 2_667 . . 2_667 ?
O60 V22 O63 V2 65.2(5) . . . . ?
O10 V22 O63 V2 -69.0(6) . . . . ?
As3 V22 O63 V2 -123.0(10) 2_667 . . . ?
O60 V2 O63 V22 -47.5(5) . . . . ?
O62 V2 O63 V22 -139.0(4) . . . . ?
O15 V2 O63 V22 127.4(4) . . . . ?
O10 V2 O63 V22 46.6(5) . . . . ?
As11 V2 O63 V22 161.1(4) . . . . ?
V3 V2 O63 V22 -93.9(4) . . . . ?
V7 V2 O63 V22 87.2(4) 2_667 . . . ?
As4 As44 O13 As1 129(2) . . . . ?
O3 As44 O13 As1 -47.5(10) . . . . ?
O4 As44 O13 As1 59.1(8) 2_667 . . . ?
O3 As44 O13 As4 -177(3) . . . . ?
O4 As44 O13 As4 -70(3) 2_667 . . . ?
As1 As44 O13 As4 -129(2) . . . . ?
As11 As1 O13 As44 -25.6(11) . . . . ?
O15 As1 O13 As44 -56.5(8) . . . . ?
O16 As1 O13 As44 45.2(8) . . . . ?
As11 As1 O13 As4 -18.4(10) . . . . ?
O15 As1 O13 As4 -49.3(6) . . . . ?
O16 As1 O13 As4 52.4(6) . . . . ?
As44 As1 O13 As4 7.2(4) . . . . ?
O4 As4 O13 As44 102(3) 2_667 . . . ?
O3 As4 O13 As44 3(3) . . . . ?
V11 As4 O13 As44 126(3) 2_667 . . . ?
As44 As4 O13 As1 -56(3) . . . . ?
O4 As4 O13 As1 46.8(6) 2_667 . . . ?
O3 As4 O13 As1 -52.7(6) . . . . ?
V11 As4 O13 As1 70.5(7) 2_667 . . . ?
C10 N2 C11 C7 0.5(12) . . . . ?
Co1 N2 C11 C7 169.3(6) . . . . ?
C10 N2 C11 C12 -179.1(8) . . . . ?
Co1 N2 C11 C12 -10.3(9) . . . . ?
C8 C7 C11 N2 -1.7(13) . . . . ?
C6 C7 C11 N2 178.3(8) . . . . ?
C8 C7 C11 C12 177.9(8) . . . . ?
C6 C7 C11 C12 -2.1(13) . . . . ?
As3 As33 O12 As2 -124(3) . . . . ?
O8 As33 O12 As2 37.5(11) . . . . ?
O10 As33 O12 As2 -67.4(9) 2_667 . . . ?
O8 As33 O12 As3 161(3) . . . . ?
O10 As33 O12 As3 56(3) 2_667 . . . ?
As2 As33 O12 As3 124(3) . . . . ?
As22 As2 O12 As33 38.4(11) . . . . ?
O9 As2 O12 As33 61.4(8) . . . . ?
O7 As2 O12 As33 -39.0(8) . . . . ?
As22 As2 O12 As3 28.7(9) . . . . ?
O9 As2 O12 As3 51.6(6) . . . . ?
O7 As2 O12 As3 -48.7(6) . . . . ?
As33 As2 O12 As3 -9.7(5) . . . . ?
O10 As3 O12 As33 -115(3) 2_667 . . . ?
O8 As3 O12 As33 -15(3) . . . . ?
V22 As3 O12 As33 -133(3) 2_667 . . . ?
As33 As3 O12 As2 63(3) . . . . ?
O10 As3 O12 As2 -52.8(6) 2_667 . . . ?
O8 As3 O12 As2 47.2(6) . . . . ?
V22 As3 O12 As2 -70.2(7) 2_667 . . . ?
O4 V11 O64 V1 65.1(6) . . . . ?
O61 V11 O64 V1 -60.8(4) . . . . ?
As4 V11 O64 V1 134.9(14) 2_667 . . . ?
O61 V1 O64 V11 54.7(5) . . . . ?
O58 V1 O64 V11 144.8(5) . . . . ?
O4 V1 O64 V11 -39.7(5) . . . . ?
O9 V1 O64 V11 -121.2(5) . . . . ?
As22 V1 O64 V11 -152.0(5) . . . . ?
V3 V1 O64 V11 99.3(5) . . . . ?
V7 V1 O64 V11 -80.1(5) . . . . ?
C1 C2 C3 C4 -1.4(16) . . . . ?
C12 C4 C3 C2 2.8(14) . . . . ?
C5 C4 C3 C2 -177.9(10) . . . . ?
C11 N2 C10 C9 0.8(14) . . . . ?
Co1 N2 C10 C9 -165.7(7) . . . . ?
C8 C9 C10 N2 -0.9(16) . . . . ?
C11 C7 C6 C5 2.2(15) . . . . ?
C8 C7 C6 C5 -177.8(10) . . . . ?
C16 C15 C14 C13 0.2(18) . . . . ?
C1 N1 C12 C4 0.2(12) . . . . ?
Co1 N1 C12 C4 -171.2(6) . . . . ?
C1 N1 C12 C11 178.6(8) . . . . ?
Co1 N1 C12 C11 7.1(9) . . . . ?
C3 C4 C12 N1 -2.2(13) . . . . ?
C5 C4 C12 N1 178.4(8) . . . . ?
C3 C4 C12 C11 179.4(8) . . . . ?
C5 C4 C12 C11 0.0(12) . . . . ?
N2 C11 C12 N1 2.2(11) . . . . ?
C7 C11 C12 N1 -177.4(8) . . . . ?
N2 C11 C12 C4 -179.4(7) . . . . ?
C7 C11 C12 C4 1.0(12) . . . . ?
C10 C9 C8 C7 -0.3(15) . . . . ?
C11 C7 C8 C9 1.5(14) . . . . ?
C6 C7 C8 C9 -178.5(10) . . . . ?
C13 N3 C24 C16 0.7(13) . . . . ?
Co1 N3 C24 C16 -177.1(6) . . . . ?
C13 N3 C24 C23 -179.8(8) . . . . ?
Co1 N3 C24 C23 2.3(9) . . . . ?
Co1 O36 C25 O34 178.6(7) . . . 2_756 ?
Co1 O36 C25 C25 -3.0(11) . . . 2_756 ?
C7 C6 C5 C4 -1.2(17) . . . . ?
C3 C4 C5 C6 -179.3(11) . . . . ?
C12 C4 C5 C6 0.1(16) . . . . ?
N3 C24 C16 C15 -0.4(12) . . . . ?
C23 C24 C16 C15 -179.9(8) . . . . ?
N3 C24 C16 C17 178.8(8) . . . . ?
C23 C24 C16 C17 -0.7(12) . . . . ?
C14 C15 C16 C24 0.0(15) . . . . ?
C14 C15 C16 C17 -179.2(11) . . . . ?
C22 N4 C23 C19 2.0(14) . . . . ?
Co1 N4 C23 C19 175.4(7) . . . . ?
C22 N4 C23 C24 -178.7(9) . . . . ?
Co1 N4 C23 C24 -5.3(10) . . . . ?
N3 C24 C23 N4 2.1(12) . . . . ?
C16 C24 C23 N4 -178.4(8) . . . . ?
N3 C24 C23 C19 -178.6(8) . . . . ?
C16 C24 C23 C19 0.9(13) . . . . ?
C19 C20 C21 C22 0(2) . . . . ?
C23 N4 C22 C21 -0.9(18) . . . . ?
Co1 N4 C22 C21 -173.0(9) . . . . ?
C20 C21 C22 N4 0(2) . . . . ?
C24 N3 C13 C14 -0.5(15) . . . . ?
Co1 N3 C13 C14 177.0(8) . . . . ?
C15 C14 C13 N3 0.1(19) . . . . ?
C21 C20 C19 C23 0.6(19) . . . . ?
C21 C20 C19 C18 179.5(13) . . . . ?
N4 C23 C19 C20 -1.9(15) . . . . ?
C24 C23 C19 C20 178.9(10) . . . . ?
N4 C23 C19 C18 179.2(9) . . . . ?
C24 C23 C19 C18 -0.1(14) . . . . ?
C17 C18 C19 C20 -179.8(12) . . . . ?
C17 C18 C19 C23 -1.0(17) . . . . ?
C19 C18 C17 C16 1.2(19) . . . . ?
C24 C16 C17 C18 -0.4(16) . . . . ?
C15 C16 C17 C18 178.8(11) . . . . ?
C32 N7 C33 C32 1(3) . . . 2_676 ?
C12 N1 C1 C2 1.3(14) . . . . ?
Co1 N1 C1 C2 171.2(7) . . . . ?
C3 C2 C1 N1 -0.7(16) . . . . ?
C33 N7 C32 C33 -1(3) . . . 2_676 ?
C33 N7 C32 N8 172.5(19) . . . . ?
N6 C26 C27 C28 -8(3) 2_566 . . . ?
C30 C26 C27 C28 0.0 . . . . ?
C26 C27 C28 N5 0.0 . . . . ?
C27 C28 N5 C29 0.0 . . . . ?
C28 N5 C29 C30 175(5) . . . 2_566 ?
C28 N5 C29 N6 -178.2(18) . . . . ?
C28 N5 C29 C30 0.0 . . . . ?
C28 N5 C29 C29 6(6) . . . 2_566 ?
C30 C29 C30 N6 -46(13) 2_566 . . 2_566 ?
N6 C29 C30 N6 -50(15) . . . 2_566 ?
N5 C29 C30 N6 131(14) . . . 2_566 ?
C29 C29 C30 N6 -46(13) 2_566 . . 2_566 ?
C30 C29 C30 C29 0.0(12) 2_566 . . 2_566 ?
N6 C29 C30 C29 -4(2) . . . 2_566 ?
N5 C29 C30 C29 177(3) . . . 2_566 ?
C30 C29 C30 C26 -177(3) 2_566 . . . ?
N6 C29 C30 C26 178.2(18) . . . . ?
N5 C29 C30 C26 0.0 . . . . ?
C29 C29 C30 C26 -177(3) 2_566 . . . ?
N6 C29 C30 C30 -4(2) . . . 2_566 ?
N5 C29 C30 C30 177(3) . . . 2_566 ?
C29 C29 C30 C30 0.0(12) 2_566 . . 2_566 ?
C27 C26 C30 N6 -170(4) . . . 2_566 ?
N6 C26 C30 C29 -4(4) 2_566 . . 2_566 ?
C27 C26 C30 C29 -174(6) . . . 2_566 ?
N6 C26 C30 C29 170(4) 2_566 . . . ?
C27 C26 C30 C29 0.0 . . . . ?
N6 C26 C30 C30 165(8) 2_566 . . 2_566 ?
C27 C26 C30 C30 -5(5) . . . 2_566 ?
C30 C29 N6 C30 10(4) . . . 2_566 ?
N5 C29 N6 C30 -172(5) . . . 2_566 ?
C29 C29 N6 C30 7(3) 2_566 . . 2_566 ?
C30 C29 N6 C26 4(5) 2_566 . . 2_566 ?
C30 C29 N6 C26 14(7) . . . 2_566 ?
N5 C29 N6 C26 -168(5) . . . 2_566 ?
C29 C29 N6 C26 11(5) 2_566 . . 2_566 ?

_refine_diff_density_max         2.744
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.188

