# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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 1468900'
_audit_update_record             
;
2016-05-11 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_shelx_1             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1w Check
RESPONSE: The hydrogens of the water molecule was not added.
;

_vrf_PLAT342_shelx_1             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.064 Ang
RESPONSE: The quality of this crystal was poor.
;

_vrf_PLAT430_shelx_1             
;
PROBLEM: Short Inter D...A Contact O1w .. O6 .. 2.76 Ang.
RESPONSE: There should be a strong hydrogen bond between the
two atoms.
;

_vrf_PLAT601_shelx_1             
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .187 Ang3  
RESPONSE: The existance of large voids containing loosely bound water solvent is
typical for POM structures
;

_vrf_PLAT971_shelx_1             
;
PROBLEM: Check Calcd Residual Density  1.81A From   O4W  1.88 eA-3   
RESPONSE: These residuals are considered to be due largely to poor crystal quality.
;
# 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            'C18 H90 Cd3 N18 O51 Sb6 V15'
_chemical_formula_weight         3206.87

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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 2'
_space_group_name_Hall           'C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   18.188(4)
_cell_length_b                   22.992(5)
_cell_length_c                   14.357(3)
_cell_angle_alpha                90
_cell_angle_beta                 125.36(3)
_cell_angle_gamma                90
_cell_volume                     4896(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    20603
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.53

_exptl_crystal_description       bulk
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.175
_exptl_crystal_F_000             3054
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    3.698
_shelx_estimated_absorpt_T_min   0.497
_shelx_estimated_absorpt_T_max   0.607
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.0547
_exptl_absorpt_correction_T_max  1.0000
_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  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24039
_diffrn_reflns_av_unetI/netI     0.1541
_diffrn_reflns_av_R_equivalents  0.1110
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.992
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10856
_reflns_number_gt                7941
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.953
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.999

_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)+(0.1165P)²+16.9675P] 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 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10856
_refine_ls_number_parameters     513
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0830
_refine_ls_wR_factor_ref         0.2305
_refine_ls_wR_factor_gt          0.2124
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_restrained_S_all      1.020
_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
Sb1 Sb 1.49907(10) 1.49095(7) 1.66520(13) 0.0346(3) Uani 1 1 d . . . . .
Sb2 Sb 1.61565(10) 1.38364(6) 1.88101(13) 0.0334(3) Uani 1 1 d . . . . .
Sb3 Sb 1.41184(13) 1.73625(7) 2.01890(17) 0.0448(4) Uani 1 1 d . . . . .
Cd1 Cd 1.28644(14) 1.19826(10) 1.7216(2) 0.0527(5) Uani 1 1 d . . . . .
V7 V 1.5000 1.3688(2) 2.0000 0.0276(10) Uani 1 2 d S T P . .
V6 V 1.2834(2) 1.45442(17) 1.8614(3) 0.0309(8) Uani 1 1 d . . . . .
V5 V 1.3763(2) 1.41734(16) 1.7618(3) 0.0298(7) Uani 1 1 d . . . . .
V4 V 1.3287(2) 1.54356(17) 1.6834(3) 0.0307(7) Uani 1 1 d . . . . .
V3 V 1.3055(2) 1.53485(18) 2.0455(3) 0.0327(8) Uani 1 1 d . . . . .
V2 V 1.4521(3) 1.62107(17) 2.1937(4) 0.0335(8) Uani 1 1 d . . . . .
V8 V 1.2811(3) 1.61587(18) 1.8759(4) 0.0348(8) Uani 1 1 d . . . . .
V1 V 1.3742(3) 1.66018(18) 1.7695(4) 0.0366(8) Uani 1 1 d . . . . .
O20 O 1.5783(11) 1.5994(7) 2.2774(15) 0.035(3) Uani 1 1 d . . . . .
O19 O 1.4122(12) 1.4803(7) 1.7022(14) 0.039(4) Uani 1 1 d . . . . .
O18 O 1.4966(11) 1.6803(7) 2.1363(15) 0.037(4) Uani 1 1 d . . . . .
O17 O 1.3297(11) 1.4540(8) 2.0254(14) 0.035(3) Uani 1 1 d . . . . .
O16 O 1.3773(9) 1.3979(6) 1.8954(13) 0.026(3) Uani 1 1 d . . . . .
O15 O 1.5053(10) 1.3904(8) 1.8710(12) 0.036(3) Uani 1 1 d . . . . .
O14 O 1.2998(11) 1.4812(8) 1.7472(15) 0.038(4) Uani 1 1 d . . . . .
O13 O 1.4191(10) 1.5401(8) 2.1983(14) 0.037(3) Uani 1 1 d . . . . .
O12 O 1.2647(10) 1.5333(8) 1.8883(14) 0.035(3) Uani 1 1 d . . . . .
O11 O 1.3440(10) 1.6132(7) 2.0435(15) 0.034(3) Uani 1 1 d . . . . .
O10 O 1.2504(12) 1.5486(9) 1.5477(16) 0.047(4) Uani 1 1 d . . . . .
O9 O 1.1875(11) 1.4181(8) 1.7946(16) 0.041(4) Uani 1 1 d . . . . .
O8 O 1.2992(12) 1.5991(7) 1.7595(16) 0.039(4) Uani 1 1 d . . . . .
O7 O 1.3204(11) 1.3692(7) 1.6605(15) 0.040(4) Uani 1 1 d . . . . .
O6 O 1.1832(13) 1.6461(9) 1.8184(19) 0.053(5) Uani 1 1 d . . . . .
O5 O 1.5000 1.7706(11) 2.0000 0.048(6) Uani 1 2 d S T P . .
O4 O 1.3651(12) 1.6792(8) 1.8956(16) 0.041(4) Uani 1 1 d . . . . .
O3 O 1.5676(14) 1.4202(8) 1.7333(16) 0.045(4) Uani 1 1 d . . . . .
O2 O 1.3170(14) 1.7095(9) 1.6679(19) 0.055(5) Uani 1 1 d . . . . .
O1 O 1.5000 1.2972(11) 2.0000 0.035(5) Uani 1 2 d S T P . .
N2 N 1.4392(16) 1.205(2) 1.815(3) 0.092(13) Uani 1 1 d . . . . .
H2A H 1.4636 1.2205 1.8843 0.110 Uiso 1 1 calc R U . . .
H2B H 1.4625 1.1701 1.8237 0.110 Uiso 1 1 calc R U . . .
N6 N 1.1342(12) 1.1732(11) 1.5914(19) 0.043(5) Uani 1 1 d . . . . .
H6A H 1.1068 1.1724 1.6264 0.052 Uiso 1 1 calc R U . . .
H6B H 1.1065 1.1992 1.5353 0.052 Uiso 1 1 calc R U . . .
N7 N 1.2878(17) 1.0968(13) 1.684(3) 0.062(7) Uani 1 1 d . . . . .
H7C H 1.2991 1.0916 1.6319 0.075 Uiso 1 1 calc R U . . .
H7D H 1.3294 1.0779 1.7474 0.075 Uiso 1 1 calc R U . . .
N4 N 1.298(2) 1.1745(12) 1.894(3) 0.062(7) Uani 1 1 d . . . . .
H4A H 1.2518 1.1523 1.8772 0.074 Uiso 1 1 calc R U . . .
H4B H 1.3490 1.1555 1.9424 0.074 Uiso 1 1 calc R U . . .
N1 N 1.3020(18) 1.2433(15) 1.582(3) 0.070(8) Uani 1 1 d . . . . .
H1A H 1.2629 1.2285 1.5124 0.084 Uiso 1 1 calc R U . . .
H1B H 1.2943 1.2816 1.5795 0.084 Uiso 1 1 calc R U . . .
C3 C 1.226(2) 1.2727(14) 1.854(3) 0.062(9) Uani 1 1 d . . . . .
H3A H 1.1671 1.2546 1.8162 0.075 Uiso 1 1 calc R U . . .
H3B H 1.2251 1.3082 1.8902 0.075 Uiso 1 1 calc R U . . .
C5 C 1.1305(18) 1.1147(14) 1.545(3) 0.057(8) Uani 1 1 d D . . . .
H5C H 1.0688 1.1008 1.4986 0.068 Uiso 1 1 calc R U . . .
H5D H 1.1512 1.1173 1.4957 0.068 Uiso 1 1 calc R U . . .
C4 C 1.296(2) 1.2320(18) 1.945(2) 0.067(9) Uani 1 1 d . . . . .
H4C H 1.2841 1.2248 2.0010 0.080 Uiso 1 1 calc R U . . .
H4D H 1.3553 1.2503 1.9833 0.080 Uiso 1 1 calc R U . . .
N3 N 1.244(3) 1.2874(12) 1.768(3) 0.079(10) Uani 1 1 d . . . . .
H3C H 1.2883 1.3134 1.7965 0.095 Uiso 1 1 calc R U . . .
H3D H 1.1948 1.3024 1.7057 0.095 Uiso 1 1 calc R U . . .
C1 C 1.399(2) 1.228(2) 1.627(3) 0.080(11) Uani 1 1 d D . . . .
H1C H 1.4037 1.1860 1.6218 0.096 Uiso 1 1 calc R U . . .
H1D H 1.4142 1.2462 1.5793 0.096 Uiso 1 1 calc R U . . .
Cd2 Cd 1.0000 1.5094(2) 1.5000 0.0728(11) Uani 1 2 d DS T P . .
C6 C 1.187(3) 1.0741(14) 1.636(3) 0.081(12) Uani 1 1 d D . . . .
H6C H 1.1767 1.0345 1.6082 0.098 Uiso 1 1 calc R U . . .
H6D H 1.1756 1.0764 1.6948 0.098 Uiso 1 1 calc R U . . .
N5 N 1.1072(17) 1.4394(15) 1.533(2) 0.074(9) Uani 1 1 d . . . . .
H5A H 1.1621 1.4525 1.5873 0.088 Uiso 1 1 calc R U . . .
H5B H 1.0981 1.4070 1.5592 0.088 Uiso 1 1 calc R U . . .
C2 C 1.462(2) 1.2460(16) 1.744(3) 0.082(13) Uani 1 1 d D . . . .
H2C H 1.4543 1.2868 1.7528 0.099 Uiso 1 1 calc R U . . .
H2D H 1.5240 1.2399 1.7681 0.099 Uiso 1 1 calc R U . . .
N9 N 1.095(2) 1.5955(14) 1.562(3) 0.088(11) Uani 1 1 d D . . . .
H9C H 1.1397 1.5918 1.6359 0.105 Uiso 1 1 calc R U . . .
H9D H 1.1190 1.5981 1.5234 0.105 Uiso 1 1 calc R U . . .
C9 C 1.045(3) 1.6491(7) 1.546(5) 0.13(3) Uani 1 1 d D . . . .
H9A H 1.0490 1.6566 1.6152 0.153 Uiso 1 1 calc R U . . .
H9B H 1.0751 1.6810 1.5363 0.153 Uiso 1 1 calc R U . . .
C8 C 1.060(4) 1.470(3) 1.345(6) 0.141(18) Uani 1 1 d D U . . .
H8A H 1.1037 1.5004 1.3644 0.170 Uiso 1 1 calc R U . . .
H8B H 1.0450 1.4522 1.2742 0.170 Uiso 1 1 calc R U . . .
C7 C 1.104(4) 1.426(2) 1.434(4) 0.110(16) Uani 1 1 d D U . . .
H7A H 1.0716 1.3895 1.4025 0.132 Uiso 1 1 calc R U . . .
H7B H 1.1646 1.4203 1.4560 0.132 Uiso 1 1 calc R U . . .
O41 O 1.2222(13) 1.5357(9) 2.0554(18) 0.050(4) Uani 1 1 d . . . . .
O40 O 1.4340(16) 1.6582(9) 2.275(2) 0.059(6) Uani 1 1 d . . . . .
O2W O 1.039(3) 1.259(2) 1.369(4) 0.133(14) Uani 1 1 d . U . . .
O1W O 1.052(3) 1.6027(19) 1.839(4) 0.123(12) Uani 1 1 d . U . . .
O5W O 1.5000 1.528(4) 2.0000 0.17(3) Uani 1 2 d S TU P . .
O4W O 1.768(6) 1.390(5) 1.878(9) 0.14(3) Uani 0.5 1 d . U P . .
O6W O 1.359(6) 1.406(4) 1.481(8) 0.23(3) Uani 1 1 d . U . . .
O7W O 1.806(5) 1.335(4) 1.724(7) 0.12(2) Uani 0.5 1 d . U P . .
N10 N 0.9797(15) 1.496(2) 1.324(3) 0.104(15) Uani 1 1 d D . . . .
H10A H 0.9324 1.4732 1.2787 0.125 Uiso 1 1 calc R U . . .
H10B H 0.9697 1.5302 1.2890 0.125 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
Sb1 O3 1.934(19) . ?
Sb1 O19 1.953(18) . ?
Sb1 O13 1.989(16) 2_859 ?
Sb2 O15 1.934(16) . ?
Sb2 O3 1.956(19) . ?
Sb2 O17 1.966(18) 2_859 ?
Sb3 O5 1.943(11) . ?
Sb3 O4 1.958(18) . ?
Sb3 O18 1.966(16) . ?
Cd1 N2 2.29(2) . ?
Cd1 N6 2.345(18) . ?
Cd1 N7 2.40(3) . ?
Cd1 N1 2.42(3) . ?
Cd1 N3 2.42(3) . ?
Cd1 N4 2.42(3) . ?
V7 O1 1.64(2) . ?
V7 O16 1.950(14) . ?
V7 O16 1.951(14) 2_859 ?
V7 O15 1.973(16) 2_859 ?
V7 O15 1.973(17) . ?
V7 V5 3.016(4) . ?
V7 V5 3.016(4) 2_859 ?
V6 O9 1.650(17) . ?
V6 O12 1.924(18) . ?
V6 O14 1.929(17) . ?
V6 O16 1.970(14) . ?
V6 O17 1.990(17) . ?
V6 V5 2.903(5) . ?
V6 V3 3.056(6) . ?
V5 O7 1.631(17) . ?
V5 O14 1.949(16) . ?
V5 O16 1.959(15) . ?
V5 O19 1.973(17) . ?
V5 O15 2.022(16) . ?
V5 V4 3.051(5) . ?
V4 O10 1.621(19) . ?
V4 O20 1.929(17) 2_859 ?
V4 O14 1.931(18) . ?
V4 O8 1.946(17) . ?
V4 O19 2.006(17) . ?
V4 V1 2.866(6) . ?
V3 O41 1.602(17) . ?
V3 O12 1.926(17) . ?
V3 O11 1.938(17) . ?
V3 O13 1.962(17) . ?
V3 O17 1.970(17) . ?
V3 V8 2.889(6) . ?
V3 V2 3.000(6) . ?
V2 O40 1.624(18) . ?
V2 O11 1.909(18) . ?
V2 O20 1.941(17) . ?
V2 O13 1.968(19) . ?
V2 O18 1.990(17) . ?
V2 V1 3.022(6) 2_859 ?
V8 O6 1.622(17) . ?
V8 O8 1.920(18) . ?
V8 O12 1.947(18) . ?
V8 O11 1.979(18) . ?
V8 O4 2.010(19) . ?
V8 V1 3.039(6) . ?
V1 O2 1.65(2) . ?
V1 O8 1.904(18) . ?
V1 O20 1.956(16) 2_859 ?
V1 O4 1.961(19) . ?
V1 O18 1.971(17) 2_859 ?
V1 V2 3.022(6) 2_859 ?
O20 V4 1.929(17) 2_859 ?
O20 V1 1.956(16) 2_859 ?
O18 V1 1.971(17) 2_859 ?
O17 Sb2 1.966(17) 2_859 ?
O13 Sb1 1.989(16) 2_859 ?
O5 Sb3 1.942(10) 2_859 ?
N2 C2 1.62(6) . ?
N6 C5 1.49(4) . ?
N7 C6 1.64(5) . ?
N4 C4 1.52(4) . ?
N1 C1 1.53(4) . ?
C3 N3 1.49(4) . ?
C3 C4 1.51(5) . ?
C5 C6 1.445(14) . ?
C1 C2 1.442(14) . ?
Cd2 N5 2.35(3) . ?
Cd2 N5 2.35(3) 2_758 ?
Cd2 N10 2.36(3) 2_758 ?
Cd2 N10 2.36(3) . ?
Cd2 N9 2.43(4) 2_758 ?
Cd2 N9 2.43(4) . ?
N5 C7 1.43(6) . ?
N9 C9 1.463(14) . ?
C9 C9 1.39(9) 2_758 ?
C8 N10 1.446(14) . ?
C8 C7 1.449(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Sb1 O19 98.2(7) . . ?
O3 Sb1 O13 94.8(8) . 2_859 ?
O19 Sb1 O13 93.7(6) . 2_859 ?
O15 Sb2 O3 95.3(7) . . ?
O15 Sb2 O17 94.4(7) . 2_859 ?
O3 Sb2 O17 96.8(8) . 2_859 ?
O5 Sb3 O4 96.2(7) . . ?
O5 Sb3 O18 94.9(7) . . ?
O4 Sb3 O18 93.0(8) . . ?
N2 Cd1 N6 163.4(11) . . ?
N2 Cd1 N7 92.0(14) . . ?
N6 Cd1 N7 75.1(9) . . ?
N2 Cd1 N1 76.8(12) . . ?
N6 Cd1 N1 95.5(8) . . ?
N7 Cd1 N1 102.0(11) . . ?
N2 Cd1 N3 104.5(14) . . ?
N6 Cd1 N3 90.6(11) . . ?
N7 Cd1 N3 159.1(9) . . ?
N1 Cd1 N3 94.3(11) . . ?
N2 Cd1 N4 93.4(11) . . ?
N6 Cd1 N4 97.0(9) . . ?
N7 Cd1 N4 90.3(10) . . ?
N1 Cd1 N4 164.4(10) . . ?
N3 Cd1 N4 76.2(10) . . ?
O1 V7 O16 110.1(4) . . ?
O1 V7 O16 110.1(4) . 2_859 ?
O16 V7 O16 139.8(8) . 2_859 ?
O1 V7 O15 104.6(5) . 2_859 ?
O16 V7 O15 88.9(6) . 2_859 ?
O16 V7 O15 81.1(6) 2_859 2_859 ?
O1 V7 O15 104.6(5) . . ?
O16 V7 O15 81.1(6) . . ?
O16 V7 O15 88.9(6) 2_859 . ?
O15 V7 O15 150.8(10) 2_859 . ?
O1 V7 V5 111.74(11) . . ?
O16 V7 V5 39.6(4) . . ?
O16 V7 V5 121.0(5) 2_859 . ?
O15 V7 V5 124.1(5) 2_859 . ?
O15 V7 V5 41.6(5) . . ?
O1 V7 V5 111.74(11) . 2_859 ?
O16 V7 V5 121.0(4) . 2_859 ?
O16 V7 V5 39.6(4) 2_859 2_859 ?
O15 V7 V5 41.6(5) 2_859 2_859 ?
O15 V7 V5 124.1(5) . 2_859 ?
V5 V7 V5 136.5(2) . 2_859 ?
O9 V6 O12 110.1(8) . . ?
O9 V6 O14 107.4(9) . . ?
O12 V6 O14 90.1(7) . . ?
O9 V6 O16 106.5(8) . . ?
O12 V6 O16 143.1(7) . . ?
O14 V6 O16 83.2(7) . . ?
O9 V6 O17 105.5(8) . . ?
O12 V6 O17 76.7(7) . . ?
O14 V6 O17 147.1(8) . . ?
O16 V6 O17 89.5(6) . . ?
O9 V6 V5 106.6(7) . . ?
O12 V6 V5 126.6(5) . . ?
O14 V6 V5 41.8(5) . . ?
O16 V6 V5 42.2(4) . . ?
O17 V6 V5 127.8(5) . . ?
O9 V6 V3 112.0(7) . . ?
O12 V6 V3 37.5(5) . . ?
O14 V6 V3 122.3(5) . . ?
O16 V6 V3 121.6(5) . . ?
O17 V6 V3 39.3(5) . . ?
V5 V6 V3 141.38(16) . . ?
O7 V5 O14 112.1(8) . . ?
O7 V5 O16 111.5(8) . . ?
O14 V5 O16 83.0(7) . . ?
O7 V5 O19 107.6(8) . . ?
O14 V5 O19 78.2(7) . . ?
O16 V5 O19 140.6(7) . . ?
O7 V5 O15 109.2(8) . . ?
O14 V5 O15 138.6(7) . . ?
O16 V5 O15 79.7(6) . . ?
O19 V5 O15 92.0(8) . . ?
O7 V5 V6 113.4(7) . . ?
O14 V5 V6 41.3(5) . . ?
O16 V5 V6 42.5(4) . . ?
O19 V5 V6 115.5(5) . . ?
O15 V5 V6 116.9(5) . . ?
O7 V5 V7 115.5(6) . . ?
O14 V5 V7 114.7(5) . . ?
O16 V5 V7 39.4(4) . . ?
O19 V5 V7 123.1(5) . . ?
O15 V5 V7 40.4(5) . . ?
V6 V5 V7 79.34(13) . . ?
O7 V5 V4 114.8(6) . . ?
O14 V5 V4 37.9(5) . . ?
O16 V5 V4 114.7(4) . . ?
O19 V5 V4 40.3(5) . . ?
O15 V5 V4 122.1(5) . . ?
V6 V5 V4 77.31(14) . . ?
V7 V5 V4 129.54(17) . . ?
O10 V4 O20 108.4(8) . 2_859 ?
O10 V4 O14 109.4(9) . . ?
O20 V4 O14 142.1(8) 2_859 . ?
O10 V4 O8 107.0(9) . . ?
O20 V4 O8 83.1(7) 2_859 . ?
O14 V4 O8 89.0(7) . . ?
O10 V4 O19 106.5(9) . . ?
O20 V4 O19 88.6(6) 2_859 . ?
O14 V4 O19 77.9(7) . . ?
O8 V4 O19 146.5(8) . . ?
O10 V4 V1 106.5(8) . . ?
O20 V4 V1 42.8(5) 2_859 . ?
O14 V4 V1 125.5(5) . . ?
O8 V4 V1 41.3(5) . . ?
O19 V4 V1 127.8(5) . . ?
O10 V4 V5 112.1(8) . . ?
O20 V4 V5 120.7(5) 2_859 . ?
O14 V4 V5 38.4(5) . . ?
O8 V4 V5 121.9(5) . . ?
O19 V4 V5 39.5(5) . . ?
V1 V4 V5 141.38(17) . . ?
O41 V3 O12 111.2(9) . . ?
O41 V3 O11 111.0(9) . . ?
O12 V3 O11 84.1(8) . . ?
O41 V3 O13 109.8(9) . . ?
O12 V3 O13 138.9(7) . . ?
O11 V3 O13 78.7(7) . . ?
O41 V3 O17 109.1(9) . . ?
O12 V3 O17 77.1(7) . . ?
O11 V3 O17 139.6(7) . . ?
O13 V3 O17 92.4(7) . . ?
O41 V3 V8 112.1(8) . . ?
O12 V3 V8 42.0(5) . . ?
O11 V3 V8 43.0(5) . . ?
O13 V3 V8 116.8(5) . . ?
O17 V3 V8 115.0(5) . . ?
O41 V3 V2 115.3(8) . . ?
O12 V3 V2 115.1(5) . . ?
O11 V3 V2 38.4(5) . . ?
O13 V3 V2 40.3(5) . . ?
O17 V3 V2 123.0(5) . . ?
V8 V3 V2 79.15(16) . . ?
O41 V3 V6 115.2(8) . . ?
O12 V3 V6 37.4(5) . . ?
O11 V3 V6 114.6(5) . . ?
O13 V3 V6 122.0(5) . . ?
O17 V3 V6 39.7(5) . . ?
V8 V3 V6 77.40(14) . . ?
V2 V3 V6 129.13(15) . . ?
O40 V2 O11 110.9(10) . . ?
O40 V2 O20 110.4(10) . . ?
O11 V2 O20 138.7(7) . . ?
O40 V2 O13 106.3(10) . . ?
O11 V2 O13 79.2(7) . . ?
O20 V2 O13 90.6(6) . . ?
O40 V2 O18 103.8(10) . . ?
O11 V2 O18 89.8(7) . . ?
O20 V2 O18 79.3(7) . . ?
O13 V2 O18 150.0(7) . . ?
O40 V2 V3 112.9(9) . . ?
O11 V2 V3 39.1(5) . . ?
O20 V2 V3 121.1(5) . . ?
O13 V2 V3 40.2(5) . . ?
O18 V2 V3 124.5(6) . . ?
O40 V2 V1 110.1(8) . 2_859 ?
O11 V2 V1 121.0(5) . 2_859 ?
O20 V2 V1 39.3(5) . 2_859 ?
O13 V2 V1 125.7(5) . 2_859 ?
O18 V2 V1 40.0(5) . 2_859 ?
V3 V2 V1 136.95(16) . 2_859 ?
O6 V8 O8 109.5(10) . . ?
O6 V8 O12 106.5(9) . . ?
O8 V8 O12 89.8(7) . . ?
O6 V8 O11 108.9(9) . . ?
O8 V8 O11 141.5(7) . . ?
O12 V8 O11 82.5(7) . . ?
O6 V8 O4 106.4(10) . . ?
O8 V8 O4 76.6(8) . . ?
O12 V8 O4 147.0(7) . . ?
O11 V8 O4 89.7(7) . . ?
O6 V8 V3 107.0(8) . . ?
O8 V8 V3 125.8(5) . . ?
O12 V8 V3 41.5(5) . . ?
O11 V8 V3 41.9(5) . . ?
O4 V8 V3 128.0(6) . . ?
O6 V8 V1 111.6(8) . . ?
O8 V8 V1 37.2(5) . . ?
O12 V8 V1 122.2(5) . . ?
O11 V8 V1 121.6(5) . . ?
O4 V8 V1 39.5(5) . . ?
V3 V8 V1 141.39(17) . . ?
O2 V1 O8 112.4(10) . . ?
O2 V1 O20 111.4(10) . 2_859 ?
O8 V1 O20 83.5(7) . 2_859 ?
O2 V1 O4 108.3(10) . . ?
O8 V1 O4 78.2(8) . . ?
O20 V1 O4 140.1(7) 2_859 . ?
O2 V1 O18 109.6(10) . 2_859 ?
O8 V1 O18 137.9(8) . 2_859 ?
O20 V1 O18 79.4(7) 2_859 2_859 ?
O4 V1 O18 91.0(7) . 2_859 ?
O2 V1 V4 112.6(8) . . ?
O8 V1 V4 42.5(5) . . ?
O20 V1 V4 42.1(5) 2_859 . ?
O4 V1 V4 116.7(6) . . ?
O18 V1 V4 116.6(5) 2_859 . ?
O2 V1 V2 114.7(8) . 2_859 ?
O8 V1 V2 115.1(5) . 2_859 ?
O20 V1 V2 39.0(5) 2_859 2_859 ?
O4 V1 V2 122.9(6) . 2_859 ?
O18 V1 V2 40.5(5) 2_859 2_859 ?
V4 V1 V2 78.99(14) . 2_859 ?
O2 V1 V8 115.1(8) . . ?
O8 V1 V8 37.6(5) . . ?
O20 V1 V8 114.7(5) 2_859 . ?
O4 V1 V8 40.7(5) . . ?
O18 V1 V8 121.6(6) 2_859 . ?
V4 V1 V8 78.28(15) . . ?
V2 V1 V8 129.98(17) 2_859 . ?
V4 O20 V2 151.0(9) 2_859 . ?
V4 O20 V1 95.1(7) 2_859 2_859 ?
V2 O20 V1 101.7(8) . 2_859 ?
Sb1 O19 V5 137.1(9) . . ?
Sb1 O19 V4 122.7(8) . . ?
V5 O19 V4 100.1(8) . . ?
Sb3 O18 V1 140.7(9) . 2_859 ?
Sb3 O18 V2 119.8(8) . . ?
V1 O18 V2 99.4(7) 2_859 . ?
Sb2 O17 V3 138.1(9) 2_859 . ?
Sb2 O17 V6 120.9(8) 2_859 . ?
V3 O17 V6 101.0(8) . . ?
V7 O16 V5 101.0(6) . . ?
V7 O16 V6 149.2(8) . . ?
V5 O16 V6 95.3(6) . . ?
Sb2 O15 V7 121.5(8) . . ?
Sb2 O15 V5 140.4(9) . . ?
V7 O15 V5 98.1(7) . . ?
V6 O14 V4 149.1(10) . . ?
V6 O14 V5 96.9(8) . . ?
V4 O14 V5 103.7(7) . . ?
V3 O13 V2 99.5(7) . . ?
V3 O13 Sb1 140.3(10) . 2_859 ?
V2 O13 Sb1 120.1(9) . 2_859 ?
V6 O12 V3 105.1(8) . . ?
V6 O12 V8 147.9(9) . . ?
V3 O12 V8 96.5(8) . . ?
V2 O11 V3 102.5(8) . . ?
V2 O11 V8 149.7(9) . . ?
V3 O11 V8 95.0(8) . . ?
V1 O8 V8 105.3(9) . . ?
V1 O8 V4 96.2(8) . . ?
V8 O8 V4 149.5(9) . . ?
Sb3 O5 Sb3 132.0(14) 2_859 . ?
Sb3 O4 V1 139.5(10) . . ?
Sb3 O4 V8 120.6(10) . . ?
V1 O4 V8 99.9(8) . . ?
Sb1 O3 Sb2 131.5(9) . . ?
C2 N2 Cd1 110(2) . . ?
C5 N6 Cd1 107.8(15) . . ?
C6 N7 Cd1 104.4(18) . . ?
C4 N4 Cd1 106.4(19) . . ?
C1 N1 Cd1 102(2) . . ?
N3 C3 C4 112(3) . . ?
C6 C5 N6 110(3) . . ?
C3 C4 N4 112(2) . . ?
C3 N3 Cd1 107(2) . . ?
C2 C1 N1 112(3) . . ?
N5 Cd2 N5 93.7(15) . 2_758 ?
N5 Cd2 N10 95.6(12) . 2_758 ?
N5 Cd2 N10 74.1(13) 2_758 2_758 ?
N5 Cd2 N10 74.1(13) . . ?
N5 Cd2 N10 95.6(12) 2_758 . ?
N10 Cd2 N10 165(3) 2_758 . ?
N5 Cd2 N9 163.6(12) . 2_758 ?
N5 Cd2 N9 98.9(9) 2_758 2_758 ?
N10 Cd2 N9 97.9(14) 2_758 2_758 ?
N10 Cd2 N9 94.2(14) . 2_758 ?
N5 Cd2 N9 98.9(9) . . ?
N5 Cd2 N9 163.6(12) 2_758 . ?
N10 Cd2 N9 94.2(15) 2_758 . ?
N10 Cd2 N9 97.9(14) . . ?
N9 Cd2 N9 71.0(11) 2_758 . ?
C5 C6 N7 102(3) . . ?
C7 N5 Cd2 113(2) . . ?
C1 C2 N2 104(3) . . ?
C9 N9 Cd2 112.7(19) . . ?
C9 C9 N9 116(3) 2_758 . ?
N10 C8 C7 116(4) . . ?
N5 C7 C8 115(4) . . ?
C8 N10 Cd2 109(3) . . ?

_refine_diff_density_max         1.925
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.254

####################################################################### 
# 
# 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 1468901'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-05-13 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_PLAT342_shelx_2             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.065 Ang
RESPONSE: The quality of this crystal was poor.
;

_vrf_PLAT430_shelx_2             
;
PROBLEM: Short Inter D...A Contact O1 .. O4w .. 2.80 Ang.
RESPONSE: There should be a strong hydrogen bond between the
two atoms.
;

_vrf_PLAT601_shelx_2             
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .167 Ang3  
RESPONSE: The existance of large voids containing loosely bound water solvent is
typical for POM structures
;

_vrf_PLAT971_shelx_2             
;
PROBLEM:  Check Calcd Residual Density  1.62A From   V1  3.84 eA-3     
RESPONSE: These residuals are considered to be due largely to poor crystal
 quality.
;

_vrf_PLAT973_shelx_2             
;
PROBLEM:  Check Calcd Positive Residual Density on  Sb2 3.08 eA-3     
RESPONSE: These residuals are considered to be due largely to poor crystal 
quality.
;
# 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            'C12 H62 N12 Ni2 O48 Sb6 V15'
_chemical_formula_weight         2754.75

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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   12.4887(7)
_cell_length_b                   12.4887(7)
_cell_length_c                   39.986(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5401.0(9)
_cell_formula_units_Z            3
_cell_measurement_temperature    292(2)
_cell_measurement_reflns_used    9937
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      28.28

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.541
_exptl_crystal_F_000             3927
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    4.656
_shelx_estimated_absorpt_T_min   0.285
_shelx_estimated_absorpt_T_max   0.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.366
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      292(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17120
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_av_R_equivalents  0.1301
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_theta_min         2.141
_diffrn_reflns_theta_max         28.290
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5859
_reflns_number_gt                5296
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.999

_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          
;
 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)+(0.1449P)²+364.4051P] 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 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.26(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5859
_refine_ls_number_parameters     286
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0890
_refine_ls_wR_factor_ref         0.2432
_refine_ls_wR_factor_gt          0.2245
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.074
_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
Sb1 Sb 0.39770(13) 0.02701(14) 0.29546(3) 0.0207(3) Uani 1 1 d . . . . .
Sb2 Sb 0.21285(14) -0.23267(14) 0.24407(3) 0.0212(3) Uani 1 1 d . . . . .
V5 V 0.1442(3) 0.1897(3) 0.19346(8) 0.0159(7) Uani 1 1 d . . . . .
V4 V 0.1940(3) 0.0630(3) 0.34354(8) 0.0139(6) Uani 1 1 d . . . . .
V3 V 0.2058(3) 0.2915(3) 0.32404(9) 0.0170(7) Uani 1 1 d . . . . .
V2 V 0.2900(3) 0.0767(4) 0.21377(9) 0.0178(7) Uani 1 1 d . . . . .
V1 V 0.3517(3) 0.2613(3) 0.26860(8) 0.0169(7) Uani 1 1 d . . . . .
Ni2 Ni 0.0000 0.0000 0.08069(12) 0.0216(10) Uani 1 3 d S T P . .
Ni1 Ni 0.3333 0.6667 0.11939(12) 0.0209(9) Uani 1 3 d S T P . .
O14 O 0.0448(14) -0.0975(14) 0.3483(4) 0.017(3) Uani 1 1 d . . . . .
O13 O 0.1934(15) -0.1033(16) 0.2211(4) 0.025(3) Uani 1 1 d . . . . .
O12 O 0.0893(15) -0.2638(17) 0.2779(4) 0.021(3) Uani 1 1 d . . . . .
O11 O 0.2909(15) 0.2003(15) 0.3128(3) 0.017(3) Uani 1 1 d . . . . .
O10 O 0.3583(15) -0.1220(15) 0.2704(4) 0.022(3) Uani 1 1 d . . . . .
O9 O 0.1404(16) 0.0333(13) 0.1900(4) 0.020(3) Uani 1 1 d . . . . .
O8 O 0.2802(16) 0.2245(15) 0.2241(4) 0.021(3) Uani 1 1 d . . . . .
O7 O 0.0440(15) 0.2770(16) 0.3149(4) 0.025(3) Uani 1 1 d . . . . .
O6 O 0.2728(14) 0.0893(17) 0.3777(4) 0.024(3) Uani 1 1 d . . . . .
O5 O 0.2024(16) 0.2648(15) 0.1593(4) 0.025(3) Uani 1 1 d . . . . .
O4 O 0.3576(15) 0.1080(15) 0.2595(4) 0.019(3) Uani 1 1 d . . . . .
N2 N 0.197(2) 0.516(2) 0.1480(5) 0.036(5) Uani 1 1 d . . . . .
H2C H 0.2249 0.4656 0.1542 0.043 Uiso 1 1 calc R U . . .
H2D H 0.1774 0.5431 0.1662 0.043 Uiso 1 1 calc R U . . .
O1W O 0.0000 0.0000 0.2690(14) 0.071(14) Uani 1 3 d S T P . .
O3 O 0.2812(18) 0.4039(19) 0.3499(5) 0.035(4) Uani 1 1 d . . . . .
N4 N -0.001(3) -0.144(3) 0.0509(7) 0.041(6) Uani 1 1 d . U . . .
O2 O 0.4941(17) 0.3682(19) 0.2676(5) 0.033(4) Uani 1 1 d . . . . .
N3 N -0.031(2) 0.124(2) 0.1104(5) 0.028(4) Uani 1 1 d . . . . .
H3C H -0.0574 0.0919 0.1306 0.034 Uiso 1 1 calc R U . . .
H3D H 0.0395 0.1954 0.1127 0.034 Uiso 1 1 calc R U . . .
N1 N 0.1759(19) 0.6298(18) 0.0906(5) 0.027(4) Uani 1 1 d . . . . .
H1C H 0.1762 0.7001 0.0865 0.033 Uiso 1 1 calc R U . . .
H1D H 0.1782 0.5969 0.0710 0.033 Uiso 1 1 calc R U . . .
O1 O 0.4029(18) 0.108(2) 0.1886(5) 0.036(4) Uani 1 1 d . . . . .
C1 C 0.064(3) 0.545(3) 0.1085(6) 0.038(6) Uani 1 1 d . . . . .
H1A H -0.0052 0.5062 0.0931 0.046 Uiso 1 1 calc R U . . .
H1B H 0.0454 0.5892 0.1253 0.046 Uiso 1 1 calc R U . . .
C2 C 0.084(3) 0.448(3) 0.1250(8) 0.041(7) Uani 1 1 d . . . . .
H2A H 0.0991 0.4004 0.1082 0.049 Uiso 1 1 calc R U . . .
H2B H 0.0117 0.3911 0.1378 0.049 Uiso 1 1 calc R U . . .
C3 C -0.121(4) 0.145(4) 0.0943(10) 0.055(8) Uani 1 1 d . U . . .
H3A H -0.1679 0.1588 0.1115 0.066 Uiso 1 1 calc R U . . .
H3B H -0.0784 0.2201 0.0813 0.066 Uiso 1 1 calc R U . . .
C4 C -0.051(6) -0.256(6) 0.0734(15) 0.086(14) Uani 1 1 d . U . . .
H4A H -0.0829 -0.3301 0.0598 0.104 Uiso 1 1 calc R U . . .
H4B H 0.0157 -0.2510 0.0870 0.104 Uiso 1 1 calc R U . . .
O4W O 0.028(4) 0.553(5) 0.1927(8) 0.099(14) Uani 1 1 d . . . . .
O3W O 0.0000 0.0000 -0.0169(13) 0.072(15) Uani 1 3 d S T P . .
O5W O 0.6667 0.3333 0.210(3) 0.18(5) Uiso 1 3 d S . 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
Sb1 O10 1.948(16) . ?
Sb1 O7 1.948(15) 3 ?
Sb1 O4 1.962(14) . ?
Sb2 O12 1.940(14) . ?
Sb2 O10 1.952(17) . ?
Sb2 O13 1.976(17) . ?
V5 O5 1.611(16) . ?
V5 O9 1.926(15) 2 ?
V5 O9 1.935(15) . ?
V5 O8 1.960(16) . ?
V5 O13 1.987(16) 2 ?
V5 V2 2.922(5) . ?
V5 V2 3.028(5) 2 ?
V4 O6 1.617(15) . ?
V4 O14 1.914(15) 2 ?
V4 O14 1.947(15) . ?
V4 O11 1.959(15) . ?
V4 O7 1.997(17) 3 ?
V4 V3 2.891(5) . ?
V4 V3 3.027(5) 3 ?
V3 O3 1.612(18) . ?
V3 O14 1.930(16) 2 ?
V3 O11 1.959(16) . ?
V3 O7 1.971(16) . ?
V3 O12 1.990(15) 2 ?
V3 V1 3.011(5) . ?
V3 V4 3.027(5) 2 ?
V2 O1 1.614(19) . ?
V2 O9 1.918(17) . ?
V2 O8 1.954(17) . ?
V2 O4 1.969(15) . ?
V2 O13 1.971(17) . ?
V2 V1 2.990(5) . ?
V2 V5 3.028(5) 3 ?
V1 O2 1.604(19) . ?
V1 O11 1.926(14) . ?
V1 O8 1.940(15) . ?
V1 O12 1.979(17) 2 ?
V1 O4 1.986(16) . ?
Ni2 N3 2.13(2) 3 ?
Ni2 N3 2.13(2) 2 ?
Ni2 N3 2.13(2) . ?
Ni2 N4 2.16(3) 3 ?
Ni2 N4 2.16(3) 2 ?
Ni2 N4 2.16(3) . ?
Ni1 N1 2.12(2) . ?
Ni1 N1 2.12(2) 3_565 ?
Ni1 N1 2.12(2) 2_665 ?
Ni1 N2 2.13(2) 3_565 ?
Ni1 N2 2.13(2) . ?
Ni1 N2 2.13(2) 2_665 ?
O14 V4 1.914(15) 3 ?
O14 V3 1.930(16) 3 ?
O13 V5 1.987(16) 3 ?
O12 V1 1.979(17) 3 ?
O12 V3 1.990(15) 3 ?
O9 V5 1.926(15) 3 ?
O7 Sb1 1.948(15) 2 ?
O7 V4 1.997(17) 2 ?
N2 C2 1.54(4) . ?
N4 C4 1.51(7) . ?
N3 C3 1.43(4) . ?
N1 C1 1.45(3) . ?
C1 C2 1.51(4) . ?
C3 C4 1.39(7) 3 ?
C4 C3 1.39(7) 2 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Sb1 O7 93.7(7) . 3 ?
O10 Sb1 O4 96.2(7) . . ?
O7 Sb1 O4 92.5(7) 3 . ?
O12 Sb2 O10 97.5(7) . . ?
O12 Sb2 O13 94.4(7) . . ?
O10 Sb2 O13 97.1(7) . . ?
O5 V5 O9 108.3(8) . 2 ?
O5 V5 O9 107.6(8) . . ?
O9 V5 O9 90.8(10) 2 . ?
O5 V5 O8 108.2(8) . . ?
O9 V5 O8 143.3(7) 2 . ?
O9 V5 O8 81.3(7) . . ?
O5 V5 O13 105.8(9) . 2 ?
O9 V5 O13 77.7(7) 2 2 ?
O9 V5 O13 146.5(8) . 2 ?
O8 V5 O13 89.4(7) . 2 ?
O5 V5 V2 107.9(7) . . ?
O9 V5 V2 126.1(5) 2 . ?
O9 V5 V2 40.4(5) . . ?
O8 V5 V2 41.6(5) . . ?
O13 V5 V2 127.0(5) 2 . ?
O5 V5 V2 109.8(7) . 2 ?
O9 V5 V2 37.9(5) 2 2 ?
O9 V5 V2 123.6(5) . 2 ?
O8 V5 V2 122.8(5) . 2 ?
O13 V5 V2 39.9(5) 2 2 ?
V2 V5 V2 142.26(17) . 2 ?
O6 V4 O14 106.7(8) . 2 ?
O6 V4 O14 107.4(8) . . ?
O14 V4 O14 89.9(9) 2 . ?
O6 V4 O11 107.7(8) . . ?
O14 V4 O11 83.3(7) 2 . ?
O14 V4 O11 144.8(7) . . ?
O6 V4 O7 107.0(9) . 3 ?
O14 V4 O7 146.2(8) 2 3 ?
O14 V4 O7 78.2(6) . 3 ?
O11 V4 O7 88.6(6) . 3 ?
O6 V4 V3 107.6(7) . . ?
O14 V4 V3 41.4(5) 2 . ?
O14 V4 V3 126.4(5) . . ?
O11 V4 V3 42.5(5) . . ?
O7 V4 V3 126.6(5) 3 . ?
O6 V4 V3 109.3(7) . 3 ?
O14 V4 V3 123.5(5) 2 3 ?
O14 V4 V3 38.4(5) . 3 ?
O11 V4 V3 123.2(5) . 3 ?
O7 V4 V3 40.0(4) 3 3 ?
V3 V4 V3 143.08(17) . 3 ?
O3 V3 O14 109.9(9) . 2 ?
O3 V3 O11 113.7(9) . . ?
O14 V3 O11 82.8(6) 2 . ?
O3 V3 O7 109.0(10) . . ?
O14 V3 O7 79.2(6) 2 . ?
O11 V3 O7 137.1(8) . . ?
O3 V3 O12 108.4(9) . 2 ?
O14 V3 O12 141.5(7) 2 2 ?
O11 V3 O12 79.3(6) . 2 ?
O7 V3 O12 91.2(7) . 2 ?
O3 V3 V4 113.9(8) . . ?
O14 V3 V4 41.0(4) 2 . ?
O11 V3 V4 42.4(4) . . ?
O7 V3 V4 114.5(5) . . ?
O12 V3 V4 117.4(5) 2 . ?
O3 V3 V1 117.0(8) . . ?
O14 V3 V1 115.1(5) 2 . ?
O11 V3 V1 38.8(4) . . ?
O7 V3 V1 120.5(6) . . ?
O12 V3 V1 40.5(5) 2 . ?
V4 V3 V1 79.05(13) . . ?
O3 V3 V4 112.5(8) . 2 ?
O14 V3 V4 38.9(4) 2 2 ?
O11 V3 V4 114.7(5) . 2 ?
O7 V3 V4 40.6(5) . 2 ?
O12 V3 V4 124.3(5) 2 2 ?
V4 V3 V4 77.53(15) . 2 ?
V1 V3 V4 130.29(15) . 2 ?
O1 V2 O9 111.6(9) . . ?
O1 V2 O8 111.3(10) . . ?
O9 V2 O8 81.9(7) . . ?
O1 V2 O4 107.2(9) . . ?
O9 V2 O4 141.0(7) . . ?
O8 V2 O4 80.7(6) . . ?
O1 V2 O13 109.3(10) . . ?
O9 V2 O13 78.3(6) . . ?
O8 V2 O13 139.0(8) . . ?
O4 V2 O13 92.6(7) . . ?
O1 V2 V5 113.0(7) . . ?
O9 V2 V5 40.9(4) . . ?
O8 V2 V5 41.8(5) . . ?
O4 V2 V5 118.1(5) . . ?
O13 V2 V5 114.7(5) . . ?
O1 V2 V1 114.5(8) . . ?
O9 V2 V1 114.9(5) . . ?
O8 V2 V1 39.7(4) . . ?
O4 V2 V1 41.1(4) . . ?
O13 V2 V1 123.0(6) . . ?
V5 V2 V1 79.28(13) . . ?
O1 V2 V5 114.4(8) . 3 ?
O9 V2 V5 38.1(4) . 3 ?
O8 V2 V5 114.0(5) . 3 ?
O4 V2 V5 124.5(5) . 3 ?
O13 V2 V5 40.3(5) . 3 ?
V5 V2 V5 77.13(16) . 3 ?
V1 V2 V5 130.74(15) . 3 ?
O2 V1 O11 113.9(8) . . ?
O2 V1 O8 111.3(9) . . ?
O11 V1 O8 134.8(7) . . ?
O2 V1 O12 103.1(10) . 2 ?
O11 V1 O12 80.4(6) . 2 ?
O8 V1 O12 89.3(7) . 2 ?
O2 V1 O4 103.8(9) . . ?
O11 V1 O4 89.1(6) . . ?
O8 V1 O4 80.7(7) . . ?
O12 V1 O4 153.1(7) 2 . ?
O2 V1 V2 112.1(7) . . ?
O11 V1 V2 118.0(5) . . ?
O8 V1 V2 40.0(5) . . ?
O12 V1 V2 125.5(5) 2 . ?
O4 V1 V2 40.7(4) . . ?
O2 V1 V3 113.7(7) . . ?
O11 V1 V3 39.6(5) . . ?
O8 V1 V3 118.0(5) . . ?
O12 V1 V3 40.8(4) 2 . ?
O4 V1 V3 124.9(5) . . ?
V2 V1 V3 134.27(15) . . ?
N3 Ni2 N3 92.1(9) 3 2 ?
N3 Ni2 N3 92.1(9) 3 . ?
N3 Ni2 N3 92.1(9) 2 . ?
N3 Ni2 N4 170.7(9) 3 3 ?
N3 Ni2 N4 94.9(9) 2 3 ?
N3 Ni2 N4 81.4(9) . 3 ?
N3 Ni2 N4 81.4(9) 3 2 ?
N3 Ni2 N4 170.7(9) 2 2 ?
N3 Ni2 N4 94.9(9) . 2 ?
N4 Ni2 N4 92.4(10) 3 2 ?
N3 Ni2 N4 94.9(9) 3 . ?
N3 Ni2 N4 81.4(9) 2 . ?
N3 Ni2 N4 170.7(9) . . ?
N4 Ni2 N4 92.4(10) 3 . ?
N4 Ni2 N4 92.4(10) 2 . ?
N1 Ni1 N1 93.3(8) . 3_565 ?
N1 Ni1 N1 93.3(8) . 2_665 ?
N1 Ni1 N1 93.3(8) 3_565 2_665 ?
N1 Ni1 N2 91.4(9) . 3_565 ?
N1 Ni1 N2 81.7(8) 3_565 3_565 ?
N1 Ni1 N2 173.3(9) 2_665 3_565 ?
N1 Ni1 N2 81.7(8) . . ?
N1 Ni1 N2 173.3(9) 3_565 . ?
N1 Ni1 N2 91.4(9) 2_665 . ?
N2 Ni1 N2 93.9(9) 3_565 . ?
N1 Ni1 N2 173.3(9) . 2_665 ?
N1 Ni1 N2 91.4(9) 3_565 2_665 ?
N1 Ni1 N2 81.7(8) 2_665 2_665 ?
N2 Ni1 N2 93.9(9) 3_565 2_665 ?
N2 Ni1 N2 93.9(9) . 2_665 ?
V4 O14 V3 97.6(7) 3 3 ?
V4 O14 V4 147.6(9) 3 . ?
V3 O14 V4 102.7(7) 3 . ?
V2 O13 Sb2 138.3(9) . . ?
V2 O13 V5 99.8(8) . 3 ?
Sb2 O13 V5 121.8(8) . 3 ?
Sb2 O12 V1 123.2(8) . 3 ?
Sb2 O12 V3 137.2(9) . 3 ?
V1 O12 V3 98.7(6) 3 3 ?
V1 O11 V3 101.6(7) . . ?
V1 O11 V4 150.6(9) . . ?
V3 O11 V4 95.1(6) . . ?
Sb1 O10 Sb2 130.9(8) . . ?
V2 O9 V5 104.0(7) . 3 ?
V2 O9 V5 98.7(7) . . ?
V5 O9 V5 147.9(10) 3 . ?
V1 O8 V2 100.3(7) . . ?
V1 O8 V5 150.6(10) . . ?
V2 O8 V5 96.6(7) . . ?
Sb1 O7 V3 140.6(9) 2 . ?
Sb1 O7 V4 118.7(8) 2 2 ?
V3 O7 V4 99.4(7) . 2 ?
Sb1 O4 V2 140.6(9) . . ?
Sb1 O4 V1 120.3(8) . . ?
V2 O4 V1 98.2(6) . . ?
C2 N2 Ni1 105.9(15) . . ?
C4 N4 Ni2 106(3) . . ?
C3 N3 Ni2 109(2) . . ?
C1 N1 Ni1 109.8(16) . . ?
N1 C1 C2 108(2) . . ?
C1 C2 N2 107(2) . . ?
C4 C3 N3 117(4) 3 . ?
C3 C4 N4 112(4) 2 . ?

_refine_diff_density_max         3.827
_refine_diff_density_min         -1.652
_refine_diff_density_rms         0.369

####################################################################### 
# 
# 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 1468902'
_audit_update_record             
;
2016-05-11 deposited with the CCDC.
2016-05-13 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_PLAT342_shelx_3             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.035 Ang
RESPONSE: The quality of this crystal was poor.
;

_vrf_PLAT601_shelx_3             
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .162 Ang3  
RESPONSE: The existance of large voids containing loosely bound water solvent is
typical for POM structures
;

_vrf_PLAT934_shelx_3             
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers .... 2 Check 
RESPONSE: We believe that these reflections are probably (0 2 1) and (-2 2 -1). 
Being only two, no action was taken.
;

_vrf_PLAT971_shelx_3             
;
PROBLEM: Check Calcd Residual Density  2.92A From      O2       1.83 eA-3    
RESPONSE: These residuals are considered to be due largely to poor crystal quality.
;
# 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            'C12 H62 Co2 N12 O48 Sb6 V15'
_chemical_formula_weight         2755.19

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   12.4543(18)
_cell_length_b                   12.4543(18)
_cell_length_c                   39.916(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     5361.9(19)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    15141
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      27.52

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.560
_exptl_crystal_F_000             3921
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    4.628
_shelx_estimated_absorpt_T_min   0.416
_shelx_estimated_absorpt_T_max   0.607
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5005
_exptl_absorpt_correction_T_max  1.0000
_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  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17328
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_theta_min         3.062
_diffrn_reflns_theta_max         27.477
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5447
_reflns_number_gt                4591
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_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)+(0.0870P)²] 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 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.44(7)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5447
_refine_ls_number_parameters     287
_refine_ls_number_restraints     26
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1415
_refine_ls_wR_factor_gt          0.1324
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.012
_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
Sb1 Sb 0.60121(9) 0.62610(9) 0.25083(2) 0.0332(3) Uani 1 1 d . . . . .
Sb2 Sb 0.78852(10) 0.55354(9) 0.30253(2) 0.0349(3) Uani 1 1 d . . . . .
V5 V 0.8048(2) 0.8676(2) 0.20250(6) 0.0258(5) Uani 1 1 d . . . . .
V4 V 0.8553(2) 1.0455(2) 0.35330(6) 0.0288(5) Uani 1 1 d . . . . .
V3 V 0.7928(2) 1.0856(2) 0.22212(6) 0.0297(5) Uani 1 1 d . . . . .
V2 V 0.6468(2) 0.9077(2) 0.27788(6) 0.0296(5) Uani 1 1 d . . . . .
V1 V 0.7086(2) 0.7854(3) 0.33273(6) 0.0322(6) Uani 1 1 d . . . . .
Co2 Co 1.0000 1.0000 0.09315(9) 0.0328(7) Uani 1 3 d S T P . .
Co1 Co 0.3333 0.6667 0.13308(9) 0.0316(7) Uani 1 3 d S T P . .
O14 O 0.9536(9) 0.8550(10) 0.1979(2) 0.030(2) Uani 1 1 d . . . . .
O13 O 0.8053(11) 0.7008(11) 0.3257(3) 0.037(2) Uani 1 1 d . . . . .
O12 O 0.7068(10) 0.9095(10) 0.2335(2) 0.030(2) Uani 1 1 d . . . . .
O11 O 0.9109(9) 0.6477(9) 0.2687(2) 0.031(2) Uani 1 1 d . . . . .
O10 O 0.7204(10) 0.9452(10) 0.3222(2) 0.031(2) Uani 1 1 d . . . . .
O9 O 0.9557(11) 1.2316(11) 0.2306(3) 0.040(3) Uani 1 1 d . . . . .
O8 O 0.7966(11) 1.0631(11) 0.3874(3) 0.038(2) Uani 1 1 d . . . . .
O7 O 0.8583(11) 0.8919(10) 0.3576(3) 0.036(2) Uani 1 1 d . . . . .
O6 O 0.6450(11) 0.5169(10) 0.2757(3) 0.041(3) Uani 1 1 d . . . . .
O5 O 0.7247(10) 0.8154(10) 0.1685(3) 0.035(2) Uani 1 1 d . . . . .
O4 O 0.6405(11) 0.7485(10) 0.2869(3) 0.036(2) Uani 1 1 d . . . . .
O1W O 0.3333 0.6667 0.3269(5) 0.036(4) Uani 1 3 d S T P . .
O3 O 0.5025(11) 0.8699(13) 0.2793(3) 0.047(3) Uani 1 1 d . . . . .
O2 O 0.7155(12) 1.1237(14) 0.1965(3) 0.052(3) Uani 1 1 d . . . . .
N3 N 0.8762(13) 1.0342(12) 0.1219(3) 0.036(3) Uani 1 1 d . . . . .
H3C H 0.8060 0.9631 0.1253 0.044 Uiso 1 1 calc R U . . .
H3D H 0.9099 1.0648 0.1418 0.044 Uiso 1 1 calc R U . . .
N1 N 0.4761(16) 0.8126(16) 0.1636(5) 0.059(4) Uani 1 1 d . U . . .
H1C H 0.4578 0.7975 0.1852 0.071 Uiso 1 1 calc R U . . .
H1D H 0.5492 0.8182 0.1599 0.071 Uiso 1 1 calc R U . . .
O1 O 0.5933(13) 0.7097(12) 0.3580(3) 0.054(3) Uani 1 1 d . . . . .
C3 C 0.8487(18) 1.1217(18) 0.1049(5) 0.049(4) Uani 1 1 d . . . . .
H3A H 0.8223 1.1622 0.1210 0.059 Uiso 1 1 calc R U . . .
H3B H 0.7828 1.0786 0.0886 0.059 Uiso 1 1 calc R U . . .
C1 C 0.479(3) 0.926(3) 0.1536(7) 0.093(7) Uani 1 1 d D U . . .
H1A H 0.4187 0.9345 0.1668 0.112 Uiso 1 1 calc R U . . .
H1B H 0.5604 0.9952 0.1589 0.112 Uiso 1 1 calc R U . . .
N2 N 0.3640(12) 0.8249(12) 0.1034(3) 0.038(3) Uani 1 1 d . . . . .
H2C H 0.3890 0.8194 0.0829 0.045 Uiso 1 1 calc R U . . .
H2D H 0.2940 0.8273 0.1017 0.045 Uiso 1 1 calc R U . . .
C2 C 0.455(3) 0.932(2) 0.1193(6) 0.082(7) Uani 1 1 d D U . . .
H2A H 0.4318 0.9951 0.1168 0.098 Uiso 1 1 calc R U . . .
H2B H 0.5317 0.9600 0.1071 0.098 Uiso 1 1 calc R U . . .
N4 N 1.0120(15) 1.1539(16) 0.0644(4) 0.048(3) Uani 1 1 d . . . . .
C4 C 0.969(2) 1.2186(18) 0.0871(5) 0.055(5) Uani 1 1 d . . . . .
H4A H 0.9535 1.2757 0.0743 0.066 Uiso 1 1 calc R U . . .
H4B H 1.0327 1.2659 0.1036 0.066 Uiso 1 1 calc R U . . .
O3W O 1.0000 1.0000 0.2762(4) 0.026(3) Uani 1 3 d S T P . .
O2W O 0.3333 0.6667 0.2317(10) 0.094(4) Uani 1 3 d S TU P . .
O4W O 0.472(3) 0.442(3) 0.3542(8) 0.132(9) Uani 1 1 d . 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
Sb1 O6 1.969(13) . ?
Sb1 O4 1.973(11) . ?
Sb1 O9 1.985(11) 2_765 ?
Sb2 O11 1.932(10) . ?
Sb2 O6 1.932(13) . ?
Sb2 O13 1.969(11) . ?
V5 O5 1.614(10) . ?
V5 O14 1.939(10) 3_675 ?
V5 O14 1.945(10) . ?
V5 O9 1.960(12) 2_765 ?
V5 O12 1.982(10) . ?
V5 V3 2.901(3) . ?
V5 V3 3.032(4) 2_765 ?
V4 O8 1.610(10) . ?
V4 O7 1.933(11) 3_675 ?
V4 O7 1.940(11) . ?
V4 O10 1.955(11) . ?
V4 O13 1.997(12) 3_675 ?
V4 V1 2.931(4) . ?
V4 V1 3.035(4) 3_675 ?
V3 O2 1.630(12) . ?
V3 O14 1.914(10) 3_675 ?
V3 O12 1.953(11) . ?
V3 O9 1.961(12) . ?
V3 O11 1.994(10) 3_675 ?
V3 V2 3.023(4) . ?
V3 V5 3.032(4) 3_675 ?
V2 O3 1.615(11) . ?
V2 O12 1.919(10) . ?
V2 O10 1.941(11) . ?
V2 O4 1.978(11) . ?
V2 O11 1.990(11) 3_675 ?
V2 V1 2.980(4) . ?
V1 O1 1.616(12) . ?
V1 O7 1.935(12) . ?
V1 O10 1.967(11) . ?
V1 O4 1.972(11) . ?
V1 O13 1.977(11) . ?
V1 V4 3.035(4) 2_765 ?
Co2 N3 2.129(14) 3_675 ?
Co2 N3 2.129(14) 2_765 ?
Co2 N3 2.129(14) . ?
Co2 N4 2.173(16) . ?
Co2 N4 2.173(16) 2_765 ?
Co2 N4 2.173(16) 3_675 ?
Co1 N2 2.162(14) 2_665 ?
Co1 N2 2.162(14) . ?
Co1 N2 2.162(14) 3_565 ?
Co1 N1 2.171(15) 2_665 ?
Co1 N1 2.171(15) . ?
Co1 N1 2.171(15) 3_565 ?
O14 V3 1.914(10) 2_765 ?
O14 V5 1.939(10) 2_765 ?
O13 V4 1.997(12) 2_765 ?
O11 V2 1.990(11) 2_765 ?
O11 V3 1.994(10) 2_765 ?
O9 V5 1.960(12) 3_675 ?
O9 Sb1 1.985(11) 3_675 ?
O7 V4 1.933(11) 2_765 ?
N3 C3 1.46(2) . ?
N1 C1 1.44(3) . ?
C3 C4 1.55(3) . ?
C1 C2 1.42(2) . ?
N2 C2 1.39(3) . ?
N4 C4 1.48(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
O6 Sb1 O4 96.8(5) . . ?
O6 Sb1 O9 93.6(5) . 2_765 ?
O4 Sb1 O9 92.5(5) . 2_765 ?
O11 Sb2 O6 96.4(4) . . ?
O11 Sb2 O13 94.5(5) . . ?
O6 Sb2 O13 97.8(5) . . ?
O5 V5 O14 106.7(5) . 3_675 ?
O5 V5 O14 108.1(5) . . ?
O14 V5 O14 90.9(6) 3_675 . ?
O5 V5 O9 107.3(6) . 2_765 ?
O14 V5 O9 146.0(5) 3_675 2_765 ?
O14 V5 O9 77.0(4) . 2_765 ?
O5 V5 O12 107.0(5) . . ?
O14 V5 O12 82.3(4) 3_675 . ?
O14 V5 O12 144.8(4) . . ?
O9 V5 O12 89.5(5) 2_765 . ?
O5 V5 V3 107.0(4) . . ?
O14 V5 V3 40.8(3) 3_675 . ?
O14 V5 V3 126.7(3) . . ?
O9 V5 V3 127.0(4) 2_765 . ?
O12 V5 V3 42.1(3) . . ?
O5 V5 V3 110.0(4) . 2_765 ?
O14 V5 V3 123.8(3) 3_675 2_765 ?
O14 V5 V3 37.8(3) . 2_765 ?
O9 V5 V3 39.4(3) 2_765 2_765 ?
O12 V5 V3 123.5(3) . 2_765 ?
V3 V5 V3 142.93(12) . 2_765 ?
O8 V4 O7 107.5(6) . 3_675 ?
O8 V4 O7 107.1(5) . . ?
O7 V4 O7 91.2(7) 3_675 . ?
O8 V4 O10 108.6(5) . . ?
O7 V4 O10 143.7(5) 3_675 . ?
O7 V4 O10 81.9(5) . . ?
O8 V4 O13 105.0(6) . 3_675 ?
O7 V4 O13 78.2(5) 3_675 3_675 ?
O7 V4 O13 147.8(5) . 3_675 ?
O10 V4 O13 88.9(4) . 3_675 ?
O8 V4 V1 108.2(4) . . ?
O7 V4 V1 126.7(4) 3_675 . ?
O7 V4 V1 40.8(3) . . ?
O10 V4 V1 41.8(3) . . ?
O13 V4 V1 127.0(4) 3_675 . ?
O8 V4 V1 109.7(4) . 3_675 ?
O7 V4 V1 38.3(3) 3_675 3_675 ?
O7 V4 V1 124.2(4) . 3_675 ?
O10 V4 V1 122.0(3) . 3_675 ?
O13 V4 V1 40.0(3) 3_675 3_675 ?
V1 V4 V1 142.10(12) . 3_675 ?
O2 V3 O14 110.7(6) . 3_675 ?
O2 V3 O12 113.6(6) . . ?
O14 V3 O12 83.7(4) 3_675 . ?
O2 V3 O9 109.0(7) . . ?
O14 V3 O9 77.7(4) 3_675 . ?
O12 V3 O9 137.1(5) . . ?
O2 V3 O11 108.4(6) . 3_675 ?
O14 V3 O11 140.9(5) 3_675 3_675 ?
O12 V3 O11 78.9(4) . 3_675 ?
O9 V3 O11 91.7(5) . 3_675 ?
O2 V3 V5 114.7(5) . . ?
O14 V3 V5 41.5(3) 3_675 . ?
O12 V3 V5 42.9(3) . . ?
O9 V3 V5 113.6(4) . . ?
O11 V3 V5 117.0(3) 3_675 . ?
O2 V3 V2 116.7(5) . . ?
O14 V3 V2 115.3(3) 3_675 . ?
O12 V3 V2 38.3(3) . . ?
O9 V3 V2 121.1(4) . . ?
O11 V3 V2 40.6(3) 3_675 . ?
V5 V3 V2 78.84(9) . . ?
O2 V3 V5 113.0(5) . 3_675 ?
O14 V3 V5 38.6(3) 3_675 3_675 ?
O12 V3 V5 115.3(3) . 3_675 ?
O9 V3 V5 39.3(3) . 3_675 ?
O11 V3 V5 123.5(3) 3_675 3_675 ?
V5 V3 V5 77.69(11) . 3_675 ?
V2 V3 V5 130.18(10) . 3_675 ?
O3 V2 O12 113.9(6) . . ?
O3 V2 O10 111.2(6) . . ?
O12 V2 O10 134.9(4) . . ?
O3 V2 O4 102.7(6) . . ?
O12 V2 O4 90.0(5) . . ?
O10 V2 O4 81.5(4) . . ?
O3 V2 O11 104.5(6) . 3_675 ?
O12 V2 O11 79.8(4) . 3_675 ?
O10 V2 O11 88.0(4) . 3_675 ?
O4 V2 O11 152.7(5) . 3_675 ?
O3 V2 V1 111.1(5) . . ?
O12 V2 V1 119.0(3) . . ?
O10 V2 V1 40.6(3) . . ?
O4 V2 V1 40.9(3) . . ?
O11 V2 V1 124.9(3) 3_675 . ?
O3 V2 V3 114.4(5) . . ?
O12 V2 V3 39.1(3) . . ?
O10 V2 V3 117.2(3) . . ?
O4 V2 V3 125.2(4) . . ?
O11 V2 V3 40.7(3) 3_675 . ?
V1 V2 V3 134.52(10) . . ?
O1 V1 O7 110.6(6) . . ?
O1 V1 O10 108.5(6) . . ?
O7 V1 O10 81.7(5) . . ?
O1 V1 O4 106.8(7) . . ?
O7 V1 O4 142.2(5) . . ?
O10 V1 O4 81.0(5) . . ?
O1 V1 O13 112.2(7) . . ?
O7 V1 O13 78.7(5) . . ?
O10 V1 O13 138.8(5) . . ?
O4 V1 O13 92.9(5) . . ?
O1 V1 V4 110.5(5) . . ?
O7 V1 V4 40.9(3) . . ?
O10 V1 V4 41.5(3) . . ?
O4 V1 V4 118.4(3) . . ?
O13 V1 V4 114.9(4) . . ?
O1 V1 V2 112.0(6) . . ?
O7 V1 V2 115.6(4) . . ?
O10 V1 V2 40.0(3) . . ?
O4 V1 V2 41.1(3) . . ?
O13 V1 V2 123.4(4) . . ?
V4 V1 V2 79.51(9) . . ?
O1 V1 V4 116.6(6) . 2_765 ?
O7 V1 V4 38.3(3) . 2_765 ?
O10 V1 V4 113.3(3) . 2_765 ?
O4 V1 V4 124.7(4) . 2_765 ?
O13 V1 V4 40.4(3) . 2_765 ?
V4 V1 V4 76.93(11) . 2_765 ?
V2 V1 V4 130.79(11) . 2_765 ?
N3 Co2 N3 93.7(5) 3_675 2_765 ?
N3 Co2 N3 93.7(5) 3_675 . ?
N3 Co2 N3 93.7(5) 2_765 . ?
N3 Co2 N4 90.8(6) 3_675 . ?
N3 Co2 N4 173.3(6) 2_765 . ?
N3 Co2 N4 81.1(5) . . ?
N3 Co2 N4 173.3(6) 3_675 2_765 ?
N3 Co2 N4 81.1(5) 2_765 2_765 ?
N3 Co2 N4 90.8(6) . 2_765 ?
N4 Co2 N4 94.7(5) . 2_765 ?
N3 Co2 N4 81.1(5) 3_675 3_675 ?
N3 Co2 N4 90.8(6) 2_765 3_675 ?
N3 Co2 N4 173.3(6) . 3_675 ?
N4 Co2 N4 94.7(5) . 3_675 ?
N4 Co2 N4 94.7(5) 2_765 3_675 ?
N2 Co1 N2 92.9(5) 2_665 . ?
N2 Co1 N2 92.9(5) 2_665 3_565 ?
N2 Co1 N2 92.9(5) . 3_565 ?
N2 Co1 N1 81.1(6) 2_665 2_665 ?
N2 Co1 N1 95.1(7) . 2_665 ?
N2 Co1 N1 170.3(6) 3_565 2_665 ?
N2 Co1 N1 170.3(6) 2_665 . ?
N2 Co1 N1 81.1(6) . . ?
N2 Co1 N1 95.0(7) 3_565 . ?
N1 Co1 N1 91.7(7) 2_665 . ?
N2 Co1 N1 95.0(7) 2_665 3_565 ?
N2 Co1 N1 170.3(6) . 3_565 ?
N2 Co1 N1 81.1(6) 3_565 3_565 ?
N1 Co1 N1 91.7(7) 2_665 3_565 ?
N1 Co1 N1 91.7(7) . 3_565 ?
V3 O14 V5 97.7(5) 2_765 2_765 ?
V3 O14 V5 103.6(4) 2_765 . ?
V5 O14 V5 146.9(6) 2_765 . ?
Sb2 O13 V1 138.9(6) . . ?
Sb2 O13 V4 121.4(6) . 2_765 ?
V1 O13 V4 99.6(5) . 2_765 ?
V2 O12 V3 102.6(5) . . ?
V2 O12 V5 149.4(6) . . ?
V3 O12 V5 95.0(4) . . ?
Sb2 O11 V2 122.9(5) . 2_765 ?
Sb2 O11 V3 137.8(6) . 2_765 ?
V2 O11 V3 98.7(4) 2_765 2_765 ?
V2 O10 V4 152.1(6) . . ?
V2 O10 V1 99.4(5) . . ?
V4 O10 V1 96.7(5) . . ?
V5 O9 V3 101.3(5) 3_675 . ?
V5 O9 Sb1 119.1(6) 3_675 3_675 ?
V3 O9 Sb1 138.4(6) . 3_675 ?
V4 O7 V1 103.4(5) 2_765 . ?
V4 O7 V4 146.8(7) 2_765 . ?
V1 O7 V4 98.3(5) . . ?
Sb2 O6 Sb1 131.3(6) . . ?
V1 O4 Sb1 140.3(6) . . ?
V1 O4 V2 98.0(5) . . ?
Sb1 O4 V2 120.8(5) . . ?
C3 N3 Co2 111.2(10) . . ?
C1 N1 Co1 105.9(13) . . ?
N3 C3 C4 107.3(15) . . ?
C2 C1 N1 115(2) . . ?
C2 N2 Co1 108.2(12) . . ?
N2 C2 C1 119(2) . . ?
C4 N4 Co2 105.9(10) . . ?
N4 C4 C3 109.2(16) . . ?

_refine_diff_density_max         1.780
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.194

####################################################################### 
# 
# 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 1468903'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT973_shelx_4             
;
PROBLEM: Check Calcd Positive Residual Density on     Sb4       2.06 eA-3     
RESPONSE: These residuals are considered to be due largely to poor crystal quality.
;

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

_vrf_PLAT971_shelx_4             
;
PROBLEM: Check Calcd Residual Density  0.98A From      V2       2.88 eA-3       
RESPONSE: These residuals are considered to be due largely to poor crystal quality.
;

_vrf_PLAT601_shelx_4             
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .157 Ang3  
RESPONSE: The existence of large voids containing loosely bound water solvent is
typical for POM structures
;
# end Validation Reply Form

# 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            'H16 O48 Sb8 V14'
_chemical_formula_weight         2471.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.6766(10)
_cell_length_b                   11.9042(5)
_cell_length_c                   19.2758(15)
_cell_angle_alpha                90
_cell_angle_beta                 109.348(9)
_cell_angle_gamma                90
_cell_volume                     2961.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4048
_cell_measurement_theta_min      3.42
_cell_measurement_theta_max      27.33

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.772
_exptl_crystal_F_000             2260
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    5.764
_shelx_estimated_absorpt_T_min   0.392
_shelx_estimated_absorpt_T_max   0.545
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83285
_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            16739
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.157
_diffrn_reflns_theta_max         29.187
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.854
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.854
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.854
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6841
_reflns_number_gt                4914
_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 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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          'SHELXL-2014/7 (Sheldrick, 2014)'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0879P)²+86.6103P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6841
_refine_ls_number_parameters     334
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0676
_refine_ls_wR_factor_ref         0.2071
_refine_ls_wR_factor_gt          0.1731
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.019
_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
Sb4 Sb 0.71304(6) 0.04471(7) -0.22214(5) 0.0334(2) Uani 1 1 d . . . . .
Sb3 Sb 1.10146(7) 0.38786(7) 0.03924(5) 0.0367(2) Uani 1 1 d . . . . .
Sb2 Sb 0.95032(7) 0.09928(7) -0.25280(5) 0.0367(2) Uani 1 1 d . . . . .
Sb1 Sb 0.85962(7) 0.33791(7) 0.06729(5) 0.0402(2) Uani 1 1 d . . . . .
V7 V 0.88450(17) 0.26755(16) -0.11252(12) 0.0323(5) Uani 1 1 d . . . . .
V6 V 1.08589(17) 0.17591(16) 0.17643(12) 0.0336(5) Uani 1 1 d . . . . .
V5 V 0.73254(17) 0.13654(19) -0.05394(13) 0.0365(5) Uani 1 1 d . . . . .
V4 V 0.75023(17) -0.16344(18) -0.09875(13) 0.0364(5) Uani 1 1 d . . . . .
V3 V 0.88756(19) -0.22522(19) 0.09951(14) 0.0417(6) Uani 1 1 d . . . . .
V2 V 0.86906(19) 0.0756(2) 0.14183(15) 0.0436(6) Uani 1 1 d . . . . .
V1 V 0.7305(2) -0.0660(3) 0.0313(2) 0.0622(8) Uani 1 1 d . . . . .
O21 O 0.7868(7) 0.1401(7) -0.1362(5) 0.0347(19) Uani 1 1 d . . . . .
O20 O 0.7966(7) -0.0863(7) -0.1715(5) 0.037(2) Uani 1 1 d . . . . .
O19 O 0.9396(7) 0.2127(7) 0.1231(5) 0.041(2) Uani 1 1 d . . . . .
O18 O 0.8345(8) 0.2592(7) -0.0262(5) 0.041(2) Uani 1 1 d . . . . .
O17 O 0.9697(7) 0.1931(7) -0.1638(5) 0.038(2) Uani 1 1 d . . . . .
O16 O 1.0271(7) 0.3004(7) -0.0491(5) 0.038(2) Uani 1 1 d . . . . .
O15 O 1.0152(7) 0.0411(7) 0.1935(5) 0.038(2) Uani 1 1 d . . . . .
O14 O 1.1306(7) 0.2527(7) 0.1028(5) 0.039(2) Uani 1 1 d . . . . .
O13 O 0.8348(7) 0.3787(7) -0.1569(5) 0.042(2) Uani 1 1 d . . . . .
O12 O 0.9734(7) 0.4276(7) 0.0577(6) 0.044(2) Uani 1 1 d . . . . .
O11 O 0.7074(7) -0.0221(7) -0.0719(5) 0.038(2) Uani 1 1 d . . . . .
O10 O 0.8015(8) 0.0845(8) -0.2783(5) 0.042(2) Uani 1 1 d . . . . .
O9 O 0.7859(8) -0.2026(8) 0.0030(6) 0.045(2) Uani 1 1 d . . . . .
O8 O 0.8434(7) -0.0823(8) 0.1237(6) 0.042(2) Uani 1 1 d . . . . .
O7 O 0.6464(8) -0.2285(8) -0.1411(6) 0.048(2) Uani 1 1 d . . . . .
O6 O 1.1177(8) 0.2500(8) 0.2488(5) 0.046(2) Uani 1 1 d . . . . .
O5 O 0.7664(7) 0.0934(8) 0.0475(5) 0.042(2) Uani 1 1 d . . . . .
O4 O 0.6214(8) 0.1940(9) -0.0794(6) 0.055(3) Uani 1 1 d . . . . .
O3 O 0.8426(9) -0.3212(9) 0.1380(7) 0.060(3) Uani 1 1 d . . . . .
O2 O 0.8185(10) 0.1067(10) 0.2027(7) 0.065(3) Uani 1 1 d . . . . .
O1 O 0.6192(11) -0.0892(14) 0.0419(9) 0.087(4) Uani 1 1 d . . . . .
O1W O 0.8667(12) 0.9333(14) 0.6239(9) 0.090(4) Uani 1 1 d . U . . .
O2W O 0.963(4) 0.547(4) 0.359(3) 0.148(16) Uani 0.5 1 d . U P . .
O3W O 0.619(6) 0.615(7) 0.126(5) 0.25(3) Uani 0.5 1 d . U P . .
O4W O 0.805(6) 0.328(7) 0.285(4) 0.27(3) Uani 0.5 1 d . U P . .
O5W O 0.959(4) -0.014(5) 0.015(3) 0.155(17) Uani 0.5 1 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
Sb4 O10 1.930(10) . ?
Sb4 O21 1.985(8) . ?
Sb4 O20 1.988(8) . ?
Sb3 O12 1.957(10) . ?
Sb3 O16 1.967(8) . ?
Sb3 O14 1.982(9) . ?
Sb2 O10 1.938(10) . ?
Sb2 O17 1.991(9) . ?
Sb2 O15 1.991(9) 3_755 ?
Sb1 O12 1.946(10) . ?
Sb1 O19 1.948(9) . ?
Sb1 O18 1.958(9) . ?
V7 O13 1.600(9) . ?
V7 O16 1.967(9) . ?
V7 O17 1.969(10) . ?
V7 O21 1.973(9) . ?
V7 O18 2.000(10) . ?
V7 V3 3.085(3) 3_755 ?
V7 V5 3.095(3) . ?
V6 O6 1.585(9) . ?
V6 O14 1.949(9) . ?
V6 O15 1.957(9) . ?
V6 O20 1.958(9) 3_755 ?
V6 O19 1.972(9) . ?
V6 V2 3.059(3) . ?
V6 V4 3.084(3) 3_755 ?
V5 O4 1.589(10) . ?
V5 O5 1.924(10) . ?
V5 O11 1.931(9) . ?
V5 O21 1.961(9) . ?
V5 O18 1.967(9) . ?
V5 V1 2.922(4) . ?
V4 O7 1.586(10) . ?
V4 O11 1.908(9) . ?
V4 O9 1.915(11) . ?
V4 O20 1.950(9) . ?
V4 O14 1.969(9) 3_755 ?
V4 V1 2.854(4) . ?
V4 V6 3.084(3) 3_755 ?
V3 O3 1.592(11) . ?
V3 O8 1.914(10) . ?
V3 O9 1.937(10) . ?
V3 O16 1.965(9) 3_755 ?
V3 O17 1.972(9) 3_755 ?
V3 V1 2.840(4) . ?
V3 V7 3.085(3) 3_755 ?
V2 O2 1.591(12) . ?
V2 O5 1.905(10) . ?
V2 O8 1.922(9) . ?
V2 O15 1.959(9) . ?
V2 O19 1.989(9) . ?
V2 V1 2.880(4) . ?
V1 O1 1.625(14) . ?
V1 O8 1.943(10) . ?
V1 O9 1.947(10) . ?
V1 O5 1.958(10) . ?
V1 O11 1.977(10) . ?
O20 V6 1.957(9) 3_755 ?
O17 V3 1.972(9) 3_755 ?
O16 V3 1.965(9) 3_755 ?
O15 Sb2 1.991(9) 3_755 ?
O14 V4 1.969(9) 3_755 ?
O5W O5W 1.45(9) 3_755 ?

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
O10 Sb4 O21 95.0(4) . . ?
O10 Sb4 O20 95.9(4) . . ?
O21 Sb4 O20 89.3(4) . . ?
O12 Sb3 O16 92.7(4) . . ?
O12 Sb3 O14 95.3(4) . . ?
O16 Sb3 O14 92.6(4) . . ?
O10 Sb2 O17 95.6(4) . . ?
O10 Sb2 O15 95.7(4) . 3_755 ?
O17 Sb2 O15 92.1(4) . 3_755 ?
O12 Sb1 O19 98.8(4) . . ?
O12 Sb1 O18 94.4(4) . . ?
O19 Sb1 O18 92.2(4) . . ?
O13 V7 O16 109.0(4) . . ?
O13 V7 O17 108.7(5) . . ?
O16 V7 O17 76.8(4) . . ?
O13 V7 O21 112.1(4) . . ?
O16 V7 O21 138.8(4) . . ?
O17 V7 O21 90.3(4) . . ?
O13 V7 O18 106.5(5) . . ?
O16 V7 O18 92.0(4) . . ?
O17 V7 O18 144.8(4) . . ?
O21 V7 O18 76.2(4) . . ?
O13 V7 V3 114.7(4) . 3_755 ?
O16 V7 V3 38.3(3) . 3_755 ?
O17 V7 V3 38.5(3) . 3_755 ?
O21 V7 V3 118.8(3) . 3_755 ?
O18 V7 V3 122.6(3) . 3_755 ?
O13 V7 V5 113.2(4) . . ?
O16 V7 V5 121.4(3) . . ?
O17 V7 V5 122.4(3) . . ?
O21 V7 V5 38.0(3) . . ?
O18 V7 V5 38.3(3) . . ?
V3 V7 V5 132.11(9) 3_755 . ?
O6 V6 O14 108.6(5) . . ?
O6 V6 O15 108.4(5) . . ?
O14 V6 O15 143.0(4) . . ?
O6 V6 O20 110.8(5) . 3_755 ?
O14 V6 O20 76.1(4) . 3_755 ?
O15 V6 O20 91.2(4) . 3_755 ?
O6 V6 O19 105.7(5) . . ?
O14 V6 O19 91.5(4) . . ?
O15 V6 O19 78.3(4) . . ?
O20 V6 O19 143.5(4) 3_755 . ?
O6 V6 V2 111.9(4) . . ?
O14 V6 V2 122.7(3) . . ?
O15 V6 V2 38.7(3) . . ?
O20 V6 V2 121.9(3) 3_755 . ?
O19 V6 V2 39.6(3) . . ?
O6 V6 V4 115.0(4) . 3_755 ?
O14 V6 V4 38.3(3) . 3_755 ?
O15 V6 V4 121.4(3) . 3_755 ?
O20 V6 V4 37.8(3) 3_755 3_755 ?
O19 V6 V4 122.2(3) . 3_755 ?
V2 V6 V4 133.11(10) . 3_755 ?
O4 V5 O5 108.2(5) . . ?
O4 V5 O11 105.7(5) . . ?
O5 V5 O11 83.6(4) . . ?
O4 V5 O21 108.7(5) . . ?
O5 V5 O21 143.1(4) . . ?
O11 V5 O21 88.2(4) . . ?
O4 V5 O18 106.5(5) . . ?
O5 V5 O18 90.7(4) . . ?
O11 V5 O18 147.5(4) . . ?
O21 V5 O18 77.3(4) . . ?
O4 V5 V1 110.0(5) . . ?
O5 V5 V1 41.6(3) . . ?
O11 V5 V1 42.2(3) . . ?
O21 V5 V1 123.3(3) . . ?
O18 V5 V1 126.7(3) . . ?
O4 V5 V7 111.1(5) . . ?
O5 V5 V7 122.7(3) . . ?
O11 V5 V7 121.9(3) . . ?
O21 V5 V7 38.3(2) . . ?
O18 V5 V7 39.1(3) . . ?
V1 V5 V7 138.86(11) . . ?
O7 V4 O11 105.5(5) . . ?
O7 V4 O9 106.8(5) . . ?
O11 V4 O9 86.2(4) . . ?
O7 V4 O20 108.0(5) . . ?
O11 V4 O20 89.0(4) . . ?
O9 V4 O20 144.9(4) . . ?
O7 V4 O14 109.2(5) . 3_755 ?
O11 V4 O14 145.0(4) . 3_755 ?
O9 V4 O14 88.6(4) . 3_755 ?
O20 V4 O14 75.8(4) . 3_755 ?
O7 V4 V1 108.8(4) . . ?
O11 V4 V1 43.7(3) . . ?
O9 V4 V1 42.8(3) . . ?
O20 V4 V1 126.0(3) . . ?
O14 V4 V1 125.1(3) 3_755 . ?
O7 V4 V6 113.4(4) . 3_755 ?
O11 V4 V6 120.8(3) . 3_755 ?
O9 V4 V6 120.4(3) . 3_755 ?
O20 V4 V6 38.0(3) . 3_755 ?
O14 V4 V6 37.8(3) 3_755 3_755 ?
V1 V4 V6 137.82(11) . 3_755 ?
O3 V3 O8 108.8(6) . . ?
O3 V3 O9 106.4(5) . . ?
O8 V3 O9 85.8(4) . . ?
O3 V3 O16 106.7(5) . 3_755 ?
O8 V3 O16 144.4(4) . 3_755 ?
O9 V3 O16 86.7(4) . 3_755 ?
O3 V3 O17 107.5(5) . 3_755 ?
O8 V3 O17 90.1(4) . 3_755 ?
O9 V3 O17 145.3(4) . 3_755 ?
O16 V3 O17 76.8(4) 3_755 3_755 ?
O3 V3 V1 110.2(5) . . ?
O8 V3 V1 43.0(3) . . ?
O9 V3 V1 43.2(3) . . ?
O16 V3 V1 123.9(3) 3_755 . ?
O17 V3 V1 126.9(3) 3_755 . ?
O3 V3 V7 112.4(5) . 3_755 ?
O8 V3 V7 121.2(3) . 3_755 ?
O9 V3 V7 119.0(3) . 3_755 ?
O16 V3 V7 38.3(3) 3_755 3_755 ?
O17 V3 V7 38.5(3) 3_755 3_755 ?
V1 V3 V7 137.34(12) . 3_755 ?
O2 V2 O5 108.3(6) . . ?
O2 V2 O8 105.3(6) . . ?
O5 V2 O8 84.4(4) . . ?
O2 V2 O15 107.1(6) . . ?
O5 V2 O15 144.5(4) . . ?
O8 V2 O15 89.0(4) . . ?
O2 V2 O19 107.3(6) . . ?
O5 V2 O19 89.1(4) . . ?
O8 V2 O19 147.2(4) . . ?
O15 V2 O19 77.9(4) . . ?
O2 V2 V1 110.0(5) . . ?
O5 V2 V1 42.5(3) . . ?
O8 V2 V1 42.1(3) . . ?
O15 V2 V1 124.3(3) . . ?
O19 V2 V1 125.9(3) . . ?
O2 V2 V6 112.1(5) . . ?
O5 V2 V6 121.3(3) . . ?
O8 V2 V6 121.8(3) . . ?
O15 V2 V6 38.6(3) . . ?
O19 V2 V6 39.2(3) . . ?
V1 V2 V6 137.94(12) . . ?
O1 V1 O8 111.1(7) . . ?
O1 V1 O9 111.1(7) . . ?
O8 V1 O9 84.8(4) . . ?
O1 V1 O5 109.9(7) . . ?
O8 V1 O5 82.5(4) . . ?
O9 V1 O5 138.9(4) . . ?
O1 V1 O11 109.1(7) . . ?
O8 V1 O11 139.7(4) . . ?
O9 V1 O11 83.5(4) . . ?
O5 V1 O11 81.6(4) . . ?
O1 V1 V3 115.1(6) . . ?
O8 V1 V3 42.2(3) . . ?
O9 V1 V3 42.9(3) . . ?
O5 V1 V3 117.5(3) . . ?
O11 V1 V3 119.1(3) . . ?
O1 V1 V4 114.0(6) . . ?
O8 V1 V4 119.2(3) . . ?
O9 V1 V4 41.9(3) . . ?
O5 V1 V4 116.3(3) . . ?
O11 V1 V4 41.8(3) . . ?
V3 V1 V4 81.86(11) . . ?
O1 V1 V2 114.8(6) . . ?
O8 V1 V2 41.6(3) . . ?
O9 V1 V2 118.3(3) . . ?
O5 V1 V2 41.1(3) . . ?
O11 V1 V2 115.9(3) . . ?
V3 V1 V2 80.59(11) . . ?
V4 V1 V2 131.09(13) . . ?
O1 V1 V5 113.2(6) . . ?
O8 V1 V5 116.5(3) . . ?
O9 V1 V5 117.1(3) . . ?
O5 V1 V5 40.7(3) . . ?
O11 V1 V5 41.0(3) . . ?
V3 V1 V5 131.65(13) . . ?
V4 V1 V5 79.67(11) . . ?
V2 V1 V5 78.87(10) . . ?
V5 O21 V7 103.8(4) . . ?
V5 O21 Sb4 116.0(4) . . ?
V7 O21 Sb4 138.6(5) . . ?
V4 O20 V6 104.2(4) . 3_755 ?
V4 O20 Sb4 116.9(5) . . ?
V6 O20 Sb4 138.7(5) 3_755 . ?
Sb1 O19 V6 138.1(5) . . ?
Sb1 O19 V2 120.7(5) . . ?
V6 O19 V2 101.1(4) . . ?
Sb1 O18 V5 119.8(5) . . ?
Sb1 O18 V7 137.6(5) . . ?
V5 O18 V7 102.6(4) . . ?
V7 O17 V3 103.0(4) . 3_755 ?
V7 O17 Sb2 138.9(5) . . ?
V3 O17 Sb2 118.1(5) 3_755 . ?
V3 O16 V7 103.4(4) 3_755 . ?
V3 O16 Sb3 116.6(4) 3_755 . ?
V7 O16 Sb3 139.9(5) . . ?
V6 O15 V2 102.7(4) . . ?
V6 O15 Sb2 138.5(5) . 3_755 ?
V2 O15 Sb2 118.4(4) . 3_755 ?
V6 O14 V4 103.9(4) . 3_755 ?
V6 O14 Sb3 141.6(5) . . ?
V4 O14 Sb3 114.4(5) 3_755 . ?
Sb1 O12 Sb3 132.6(5) . . ?
V4 O11 V5 149.2(5) . . ?
V4 O11 V1 94.5(4) . . ?
V5 O11 V1 96.8(4) . . ?
Sb4 O10 Sb2 132.9(5) . . ?
V4 O9 V3 151.1(6) . . ?
V4 O9 V1 95.3(4) . . ?
V3 O9 V1 94.0(5) . . ?
V3 O8 V2 149.3(6) . . ?
V3 O8 V1 94.8(4) . . ?
V2 O8 V1 96.3(4) . . ?
V2 O5 V5 148.5(6) . . ?
V2 O5 V1 96.4(4) . . ?
V5 O5 V1 97.6(5) . . ?

_refine_diff_density_max         3.242
_refine_diff_density_min         -2.367
_refine_diff_density_rms         0.301

####################################################################### 
# 
# 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 1468904'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-05-13 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT306_shelx_5             
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1w Check
RESPONSE: The hydrogens of the water molecule was not added.
;

_vrf_PLAT342_shelx_5             
;
PROBLEM: Low Bond Precision on C-C Bonds .........0.02217 Ang
RESPONSE: The quality of this crystal was poor.
;

_vrf_PLAT910_shelx_5             
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)   14 Note  
RESPONSE: The quality of this crystal was poor. Beamstop theta-min 
limit set too high, large unitcell etc
;

_vrf_PLAT971_shelx_5             
;
PROBLEM:  Check Calcd Residual Density  1.55A From  C3   1.92 eA-3
RESPONSE:  These residuals are considered to be due largely to poor 
crystal quality.
;

_vrf_PLAT975_shelx_5             
;
PROBLEM:  Check Calcd Residual Density  1.04A From  O3W  0.65 eA-3
RESPONSE:  These residuals are considered to be due largely to poor 
crystal quality.
;

_vrf_PLAT976_shelx_5             
;
PROBLEM:  Check Calcd Residual Density  0.58A From  O2W  -0.62 eA-3 
RESPONSE:  These residuals are considered to be due largely to poor 
crystal quality.
;
# 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            'C18 H70 Co2 N12 O47 Sb8 V14'
_chemical_formula_weight         3011.88

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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 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+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   29.050(6)
_cell_length_b                   15.812(3)
_cell_length_c                   21.821(4)
_cell_angle_alpha                90
_cell_angle_beta                 128.43(3)
_cell_angle_gamma                90
_cell_volume                     7852(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    31845
_cell_measurement_theta_min      2.99
_cell_measurement_theta_max      27.57

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.548
_exptl_crystal_F_000             5688
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    4.778
_shelx_estimated_absorpt_T_min   0.381
_shelx_estimated_absorpt_T_max   0.534
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.3399
_exptl_absorpt_correction_T_max  1.0000
_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  'Bruker P4'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35205
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.117
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8977
_reflns_number_gt                7301
_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)+(0.0383P)²+99.4410P] 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         8977
_refine_ls_number_parameters     458
_refine_ls_number_restraints     204
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.0988
_refine_ls_wR_factor_gt          0.0949
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Sb4 Sb 0.20671(2) 0.78170(3) 0.89030(2) 0.02201(9) Uani 1 1 d . . . . .
Sb3 Sb -0.01052(2) 0.89238(2) 0.52451(2) 0.02135(9) Uani 1 1 d . . . . .
Sb2 Sb -0.13970(2) 0.61814(2) 0.57725(2) 0.02208(9) Uani 1 1 d . . . . .
Sb1 Sb -0.08193(2) 1.05578(2) 0.55036(2) 0.02256(9) Uani 1 1 d . . . . .
V8 V -0.13131(4) 0.83807(6) 0.53063(6) 0.0205(2) Uani 1 1 d . . . . .
V7 V -0.03165(4) 0.71042(6) 0.58175(6) 0.0198(2) Uani 1 1 d . . . . .
V6 V 0.08102(4) 0.65916(6) 0.71917(6) 0.0206(2) Uani 1 1 d . . . . .
V5 V 0.0000 0.58775(9) 0.7500 0.0205(3) Uani 1 2 d S T P . .
V4 V 0.0000 1.08486(9) 0.7500 0.0194(3) Uani 1 2 d S T P . .
V3 V 0.14215(4) 0.96614(6) 0.87066(6) 0.0212(2) Uani 1 1 d . . . . .
V2 V 0.07567(4) 1.01516(6) 0.71001(6) 0.0204(2) Uani 1 1 d . . . . .
V1 V 0.10888(4) 0.83681(6) 0.70185(6) 0.0207(2) Uani 1 1 d . . . . .
O20 O 0.0000 1.1877(4) 0.7500 0.0306(14) Uani 1 2 d S T P . .
O19 O -0.10656(19) 0.7193(3) 0.5654(3) 0.0265(9) Uani 1 1 d . . . . .
O18 O 0.00111(18) 0.6333(3) 0.8323(2) 0.0233(9) Uani 1 1 d . . . . .
O17 O -0.00667(18) 1.0518(3) 0.6565(2) 0.0261(9) Uani 1 1 d . . . . .
O16 O 0.04887(19) 0.9226(3) 0.6338(2) 0.0262(9) Uani 1 1 d . . . . .
O15 O 0.07816(18) 1.0421(3) 0.7991(2) 0.0224(8) Uani 1 1 d . . . . .
O14 O 0.0000 0.4857(4) 0.7500 0.0341(15) Uani 1 2 d S T P . .
O13 O -0.11342(19) 0.9571(3) 0.5664(2) 0.0245(9) Uani 1 1 d . . . . .
O12 O -0.08493(18) 0.6196(3) 0.6911(2) 0.0251(9) Uani 1 1 d . . . . .
O11 O 0.04867(17) 0.7510(3) 0.6440(2) 0.0225(8) Uani 1 1 d . . . . .
O10 O -0.0533(2) 0.9989(3) 0.4997(2) 0.0274(9) Uani 1 1 d . . . . .
O9 O 0.12954(18) 0.9249(3) 0.7772(2) 0.0227(8) Uani 1 1 d . . . . .
O8 O -0.1865(2) 0.8376(3) 0.4393(3) 0.0357(11) Uani 1 1 d . . . . .
O7 O 0.15897(19) 0.8484(3) 0.9076(2) 0.0265(9) Uani 1 1 d . . . . .
O6 O -0.05877(19) 0.8275(3) 0.5430(3) 0.0273(9) Uani 1 1 d . . . . .
O5 O 0.20533(18) 0.6806(3) 0.9409(3) 0.0272(9) Uani 1 1 d . . . . .
O4 O 0.13896(18) 0.7493(3) 0.7835(2) 0.0250(9) Uani 1 1 d . . . . .
O3 O 0.1099(2) 0.5878(3) 0.7000(3) 0.0362(11) Uani 1 1 d . . . . .
O2 O 0.1063(2) 1.0879(3) 0.6948(3) 0.0346(11) Uani 1 1 d . . . . .
O1 O 0.1521(2) 0.8367(3) 0.6788(3) 0.0380(11) Uani 1 1 d . . . . .
O1W O 0.0000 0.8348(15) 0.7500 0.219(11) Uani 1 2 d S T P . .
Co1 Co 0.11461(5) 0.33835(6) 0.71299(5) 0.0359(2) Uani 1 1 d . . . . .
N6 N 0.1390(4) 0.2804(6) 0.6478(4) 0.073(3) Uani 1 1 d . . . . .
H6C H 0.1495 0.2269 0.6632 0.087 Uiso 1 1 calc R U . . .
H6D H 0.1082 0.2803 0.5972 0.087 Uiso 1 1 calc R U . . .
C1 C -0.0121(3) 0.2952(5) 0.5842(5) 0.0403(16) Uani 1 1 d . U . . .
H1A H -0.0487 0.2731 0.5700 0.048 Uiso 1 1 calc R U . . .
H1B H -0.0098 0.2801 0.5431 0.048 Uiso 1 1 calc R U . . .
C5 C 0.1837(6) 0.4150(9) 0.6697(9) 0.094(4) Uani 1 1 d . U . . .
H5C H 0.1454 0.4334 0.6224 0.113 Uiso 1 1 calc R U . . .
O2W O -0.1820(4) 1.0366(9) 0.3906(6) 0.143(5) Uani 1 1 d . . . . .
C6 C 0.1873(7) 0.3256(11) 0.6596(10) 0.119(5) Uani 1 1 d . U . . .
H6A H 0.2242 0.3035 0.7054 0.142 Uiso 1 1 calc R U . . .
H6B H 0.1863 0.3169 0.6147 0.142 Uiso 1 1 calc R U . . .
O22 O -0.0449(2) 0.6561(3) 0.5101(3) 0.0345(11) Uani 1 1 d . . . . .
O21 O 0.2032(2) 1.0178(3) 0.9235(3) 0.0392(12) Uani 1 1 d . . . . .
N2 N 0.0467(3) 0.4198(3) 0.6192(4) 0.0348(13) Uani 1 1 d . . . . .
H2A H 0.0526 0.4727 0.6366 0.042 Uiso 1 1 calc R U . . .
H2B H 0.0487 0.4191 0.5801 0.042 Uiso 1 1 calc R U . . .
N1 N 0.0370(3) 0.2571(4) 0.6576(4) 0.0437(15) Uani 1 1 d . . . . .
H1C H 0.0447 0.2062 0.6484 0.052 Uiso 1 1 calc R U . . .
H1D H 0.0278 0.2509 0.6893 0.052 Uiso 1 1 calc R U . . .
C2 C -0.0118(3) 0.3911(4) 0.5907(4) 0.0355(15) Uani 1 1 d . U . . .
H2C H -0.0168 0.4056 0.6299 0.043 Uiso 1 1 calc R U . . .
O3W O 0.2225(3) 0.5064(5) 0.9106(4) 0.077(2) Uani 1 1 d . . . . .
N5 N 0.1807(3) 0.4259(5) 0.7377(4) 0.0540(18) Uani 1 1 d . . . . .
H5A H 0.1708 0.4787 0.7393 0.065 Uiso 1 1 calc R U . . .
H5B H 0.2152 0.4140 0.7834 0.065 Uiso 1 1 calc R U . . .
N3 N 0.1122(4) 0.3945(6) 0.8005(5) 0.067(2) Uani 1 1 d . . . . .
H3C H 0.1385 0.4361 0.8240 0.080 Uiso 1 1 calc R U . . .
H3D H 0.0768 0.4171 0.7774 0.080 Uiso 1 1 calc R U . . .
C7 C -0.0618(4) 0.4336(6) 0.5123(6) 0.060(2) Uani 1 1 d . U . . .
H7A H -0.0990 0.4132 0.4959 0.090 Uiso 1 1 calc R U . . .
H7B H -0.0599 0.4938 0.5193 0.090 Uiso 1 1 calc R U . . .
H7C H -0.0574 0.4201 0.4733 0.090 Uiso 1 1 calc R U . . .
N4 N 0.1677(5) 0.2494(6) 0.8064(4) 0.088(3) Uani 1 1 d . . . . .
H4A H 0.1511 0.1985 0.7924 0.106 Uiso 1 1 calc R U . . .
H4B H 0.2032 0.2455 0.8190 0.106 Uiso 1 1 calc R U . . .
C4 C 0.1721(8) 0.2832(11) 0.8756(10) 0.116(5) Uani 1 1 d . U . . .
H4C H 0.2077 0.3180 0.9068 0.139 Uiso 1 1 calc R U . . .
C3 C 0.1239(7) 0.3365(10) 0.8564(8) 0.108(4) Uani 1 1 d . U . . .
H3A H 0.0893 0.3024 0.8360 0.129 Uiso 1 1 calc R U . . .
H3B H 0.1347 0.3658 0.9028 0.129 Uiso 1 1 calc R U . . .
C9 C 0.2286(8) 0.4753(11) 0.6790(10) 0.130(5) Uani 1 1 d . U . . .
H9A H 0.2202 0.5320 0.6851 0.194 Uiso 1 1 calc R U . . .
H9B H 0.2673 0.4597 0.7244 0.194 Uiso 1 1 calc R U . . .
H9C H 0.2266 0.4723 0.6334 0.194 Uiso 1 1 calc R U . . .
C8 C 0.1759(10) 0.2183(14) 0.9344(13) 0.178(7) Uani 1 1 d . U . . .
H8A H 0.2068 0.1782 0.9523 0.267 Uiso 1 1 calc R U . . .
H8B H 0.1841 0.2486 0.9783 0.267 Uiso 1 1 calc R U . . .
H8C H 0.1392 0.1890 0.9080 0.267 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
Sb4 O5 1.956(4) . ?
Sb4 O7 1.957(4) . ?
Sb4 O4 1.966(4) . ?
Sb3 O16 1.943(4) . ?
Sb3 O10 1.960(4) . ?
Sb3 O6 1.971(4) . ?
Sb2 O12 1.947(4) . ?
Sb2 O5 1.958(4) 2_556 ?
Sb2 O19 1.965(4) . ?
Sb1 O13 1.947(4) . ?
Sb1 O17 1.963(4) . ?
Sb1 O10 1.965(4) . ?
V8 O8 1.603(5) . ?
V8 O7 1.958(4) 2_556 ?
V8 O6 1.958(4) . ?
V8 O13 1.980(4) . ?
V8 O19 1.985(4) . ?
V8 V3 3.1118(15) 2_556 ?
V8 V7 3.1122(15) . ?
V7 O22 1.607(5) . ?
V7 O18 1.929(4) 2_556 ?
V7 O11 1.939(4) . ?
V7 O19 1.979(4) . ?
V7 O6 1.984(4) . ?
V7 V6 2.857(2) . ?
V6 O3 1.608(5) . ?
V6 O11 1.941(4) . ?
V6 O18 1.947(4) 2_556 ?
V6 O4 1.974(4) . ?
V6 O12 1.990(4) 2_556 ?
V6 V1 3.0113(15) . ?
V6 V5 3.0389(12) . ?
V5 O14 1.613(6) . ?
V5 O18 1.917(4) . ?
V5 O18 1.917(4) 2_556 ?
V5 O12 2.013(4) . ?
V5 O12 2.013(4) 2_556 ?
V5 V6 3.0390(12) 2_556 ?
V4 O20 1.626(6) . ?
V4 O15 1.933(4) . ?
V4 O15 1.933(4) 2_556 ?
V4 O17 1.997(4) . ?
V4 O17 1.997(4) 2_556 ?
V4 V2 3.0320(12) . ?
V4 V2 3.0321(12) 2_556 ?
V3 O21 1.613(5) . ?
V3 O15 1.931(4) . ?
V3 O9 1.947(4) . ?
V3 O7 1.966(4) . ?
V3 O13 2.007(4) 2_556 ?
V3 V2 2.8643(18) . ?
V3 V8 3.1118(15) 2_556 ?
V2 O2 1.610(4) . ?
V2 O9 1.945(4) . ?
V2 O15 1.947(4) . ?
V2 O16 1.977(4) . ?
V2 O17 1.987(4) . ?
V2 V1 3.0213(15) . ?
V1 O1 1.616(5) . ?
V1 O11 1.937(4) . ?
V1 O9 1.943(4) . ?
V1 O16 1.966(4) . ?
V1 O4 1.979(4) . ?
O18 V7 1.929(4) 2_556 ?
O18 V6 1.947(4) 2_556 ?
O13 V3 2.007(4) 2_556 ?
O12 V6 1.991(4) 2_556 ?
O7 V8 1.958(4) 2_556 ?
O5 Sb2 1.958(4) 2_556 ?
Co1 N4 2.145(8) . ?
Co1 N3 2.146(7) . ?
Co1 N5 2.147(7) . ?
Co1 N6 2.147(8) . ?
Co1 N2 2.172(6) . ?
Co1 N1 2.192(7) . ?
N6 C6 1.450(17) . ?
C1 N1 1.457(10) . ?
C1 C2 1.523(10) . ?
C5 C6 1.444(19) . ?
C5 C9 1.523(19) . ?
C5 N5 1.551(14) . ?
N2 C2 1.473(9) . ?
C2 C7 1.548(11) . ?
N3 C3 1.390(15) . ?
N4 C4 1.529(18) . ?
C4 C3 1.46(2) . ?
C4 C8 1.59(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O5 Sb4 O7 93.78(18) . . ?
O5 Sb4 O4 95.70(18) . . ?
O7 Sb4 O4 93.56(18) . . ?
O16 Sb3 O10 93.15(18) . . ?
O16 Sb3 O6 94.51(19) . . ?
O10 Sb3 O6 95.38(18) . . ?
O12 Sb2 O5 99.93(18) . 2_556 ?
O12 Sb2 O19 94.58(18) . . ?
O5 Sb2 O19 93.32(18) 2_556 . ?
O13 Sb1 O17 93.74(18) . . ?
O13 Sb1 O10 98.32(18) . . ?
O17 Sb1 O10 95.64(18) . . ?
O8 V8 O7 109.5(2) . 2_556 ?
O8 V8 O6 109.3(2) . . ?
O7 V8 O6 141.16(19) 2_556 . ?
O8 V8 O13 108.0(2) . . ?
O7 V8 O13 76.61(17) 2_556 . ?
O6 V8 O13 91.75(18) . . ?
O8 V8 O19 108.4(2) . . ?
O7 V8 O19 91.26(19) 2_556 . ?
O6 V8 O19 76.32(17) . . ?
O13 V8 O19 143.58(19) . . ?
O8 V8 V3 114.19(19) . 2_556 ?
O7 V8 V3 37.62(12) 2_556 2_556 ?
O6 V8 V3 121.54(14) . 2_556 ?
O13 V8 V3 38.99(12) . 2_556 ?
O19 V8 V3 121.29(13) . 2_556 ?
O8 V8 V7 115.59(19) . . ?
O7 V8 V7 119.72(14) 2_556 . ?
O6 V8 V7 38.14(12) . . ?
O13 V8 V7 121.17(13) . . ?
O19 V8 V7 38.21(12) . . ?
V3 V8 V7 130.22(5) 2_556 . ?
O22 V7 O18 107.2(2) . 2_556 ?
O22 V7 O11 108.3(2) . . ?
O18 V7 O11 84.38(18) 2_556 . ?
O22 V7 O19 106.9(2) . . ?
O18 V7 O19 90.57(18) 2_556 . ?
O11 V7 O19 144.32(18) . . ?
O22 V7 O6 107.0(2) . . ?
O18 V7 O6 145.56(19) 2_556 . ?
O11 V7 O6 88.63(18) . . ?
O19 V7 O6 75.87(17) . . ?
O22 V7 V6 107.15(19) . . ?
O18 V7 V6 42.75(12) 2_556 . ?
O11 V7 V6 42.61(12) . . ?
O19 V7 V6 128.56(14) . . ?
O6 V7 V6 127.20(14) . . ?
O22 V7 V8 113.02(19) . . ?
O18 V7 V8 121.43(13) 2_556 . ?
O11 V7 V8 118.88(13) . . ?
O19 V7 V8 38.34(12) . . ?
O6 V7 V8 37.56(12) . . ?
V6 V7 V8 139.81(5) . . ?
O3 V6 O11 111.2(2) . . ?
O3 V6 O18 110.7(2) . 2_556 ?
O11 V6 O18 83.88(18) . 2_556 ?
O3 V6 O4 109.8(2) . . ?
O11 V6 O4 79.17(18) . . ?
O18 V6 O4 139.40(18) 2_556 . ?
O3 V6 O12 108.4(2) . 2_556 ?
O11 V6 O12 140.23(18) . 2_556 ?
O18 V6 O12 78.57(18) 2_556 2_556 ?
O4 V6 O12 91.45(18) . 2_556 ?
O3 V6 V7 111.59(19) . . ?
O11 V6 V7 42.56(12) . . ?
O18 V6 V7 42.28(12) 2_556 . ?
O4 V6 V7 117.12(13) . . ?
O12 V6 V7 116.72(13) 2_556 . ?
O3 V6 V1 113.41(19) . . ?
O11 V6 V1 39.00(12) . . ?
O18 V6 V1 116.87(13) 2_556 . ?
O4 V6 V1 40.45(12) . . ?
O12 V6 V1 124.14(13) 2_556 . ?
V7 V6 V1 79.96(4) . . ?
O3 V6 V5 113.43(19) . . ?
O11 V6 V5 115.50(13) . . ?
O18 V6 V5 37.79(12) 2_556 . ?
O4 V6 V5 123.10(13) . . ?
O12 V6 V5 40.89(13) 2_556 . ?
V7 V6 V5 78.35(4) . . ?
V1 V6 V5 132.84(4) . . ?
O14 V5 O18 112.09(13) . . ?
O14 V5 O18 112.09(13) . 2_556 ?
O18 V5 O18 135.8(3) . 2_556 ?
O14 V5 O12 104.48(13) . . ?
O18 V5 O12 78.72(17) . . ?
O18 V5 O12 90.44(17) 2_556 . ?
O14 V5 O12 104.48(13) . 2_556 ?
O18 V5 O12 90.44(18) . 2_556 ?
O18 V5 O12 78.72(17) 2_556 2_556 ?
O12 V5 O12 151.0(3) . 2_556 ?
O14 V5 V6 111.81(3) . . ?
O18 V5 V6 120.22(14) . . ?
O18 V5 V6 38.48(13) 2_556 . ?
O12 V5 V6 125.20(13) . . ?
O12 V5 V6 40.34(12) 2_556 . ?
O14 V5 V6 111.81(3) . 2_556 ?
O18 V5 V6 38.48(13) . 2_556 ?
O18 V5 V6 120.22(14) 2_556 2_556 ?
O12 V5 V6 40.34(12) . 2_556 ?
O12 V5 V6 125.20(13) 2_556 2_556 ?
V6 V5 V6 136.37(6) . 2_556 ?
O20 V4 O15 110.46(13) . . ?
O20 V4 O15 110.46(13) . 2_556 ?
O15 V4 O15 139.1(3) . 2_556 ?
O20 V4 O17 105.19(13) . . ?
O15 V4 O17 79.01(18) . . ?
O15 V4 O17 90.42(17) 2_556 . ?
O20 V4 O17 105.19(13) . 2_556 ?
O15 V4 O17 90.42(17) . 2_556 ?
O15 V4 O17 79.01(18) 2_556 2_556 ?
O17 V4 O17 149.6(3) . 2_556 ?
O20 V4 V2 111.31(3) . . ?
O15 V4 V2 38.78(12) . . ?
O15 V4 V2 121.69(13) 2_556 . ?
O17 V4 V2 40.32(12) . . ?
O17 V4 V2 124.89(13) 2_556 . ?
O20 V4 V2 111.31(3) . 2_556 ?
O15 V4 V2 121.70(13) . 2_556 ?
O15 V4 V2 38.79(12) 2_556 2_556 ?
O17 V4 V2 124.89(13) . 2_556 ?
O17 V4 V2 40.32(12) 2_556 2_556 ?
V2 V4 V2 137.37(6) . 2_556 ?
O21 V3 O15 110.0(2) . . ?
O21 V3 O9 109.0(2) . . ?
O15 V3 O9 84.34(18) . . ?
O21 V3 O7 107.7(2) . . ?
O15 V3 O7 142.17(19) . . ?
O9 V3 O7 87.13(18) . . ?
O21 V3 O13 106.7(2) . 2_556 ?
O15 V3 O13 89.82(17) . 2_556 ?
O9 V3 O13 143.67(18) . 2_556 ?
O7 V3 O13 75.81(17) . 2_556 ?
O21 V3 V2 110.1(2) . . ?
O15 V3 V2 42.62(12) . . ?
O9 V3 V2 42.57(12) . . ?
O7 V3 V2 124.41(14) . . ?
O13 V3 V2 127.30(13) 2_556 . ?
O21 V3 V8 111.96(19) . 2_556 ?
O15 V3 V8 120.26(13) . 2_556 ?
O9 V3 V8 118.25(13) . 2_556 ?
O7 V3 V8 37.44(13) . 2_556 ?
O13 V3 V8 38.37(12) 2_556 2_556 ?
V2 V3 V8 137.90(5) . 2_556 ?
O2 V2 O9 113.0(2) . . ?
O2 V2 O15 111.6(2) . . ?
O9 V2 O15 83.97(17) . . ?
O2 V2 O16 109.5(2) . . ?
O9 V2 O16 78.61(18) . . ?
O15 V2 O16 138.88(18) . . ?
O2 V2 O17 106.8(2) . . ?
O9 V2 O17 140.14(18) . . ?
O15 V2 O17 78.91(18) . . ?
O16 V2 O17 91.16(18) . . ?
O2 V2 V3 114.02(19) . . ?
O9 V2 V3 42.64(12) . . ?
O15 V2 V3 42.18(12) . . ?
O16 V2 V3 116.29(13) . . ?
O17 V2 V3 116.63(13) . . ?
O2 V2 V1 114.62(18) . . ?
O9 V2 V1 38.99(12) . . ?
O15 V2 V1 116.62(13) . . ?
O16 V2 V1 39.85(13) . . ?
O17 V2 V1 123.30(13) . . ?
V3 V2 V1 79.77(4) . . ?
O2 V2 V4 113.12(18) . . ?
O9 V2 V4 115.94(13) . . ?
O15 V2 V4 38.44(12) . . ?
O16 V2 V4 122.32(14) . . ?
O17 V2 V4 40.56(12) . . ?
V3 V2 V4 78.70(4) . . ?
V1 V2 V4 132.17(4) . . ?
O1 V1 O11 110.9(2) . . ?
O1 V1 O9 111.9(2) . . ?
O11 V1 O9 137.14(18) . . ?
O1 V1 O16 105.1(2) . . ?
O11 V1 O16 88.46(18) . . ?
O9 V1 O16 78.90(18) . . ?
O1 V1 O4 106.6(2) . . ?
O11 V1 O4 79.15(18) . . ?
O9 V1 O4 90.48(17) . . ?
O16 V1 O4 148.26(19) . . ?
O1 V1 V6 111.07(19) . . ?
O11 V1 V6 39.10(12) . . ?
O9 V1 V6 121.89(13) . . ?
O16 V1 V6 123.84(14) . . ?
O4 V1 V6 40.33(12) . . ?
O1 V1 V2 110.93(19) . . ?
O11 V1 V2 120.03(13) . . ?
O9 V1 V2 39.02(12) . . ?
O16 V1 V2 40.12(13) . . ?
O4 V1 V2 125.31(13) . . ?
V6 V1 V2 137.96(4) . . ?
Sb2 O19 V7 119.5(2) . . ?
Sb2 O19 V8 136.9(2) . . ?
V7 O19 V8 103.45(19) . . ?
V5 O18 V7 151.4(2) . 2_556 ?
V5 O18 V6 103.74(19) . 2_556 ?
V7 O18 V6 94.97(18) 2_556 2_556 ?
Sb1 O17 V2 139.0(2) . . ?
Sb1 O17 V4 121.8(2) . . ?
V2 O17 V4 99.12(19) . . ?
Sb3 O16 V1 116.9(2) . . ?
Sb3 O16 V2 143.1(2) . . ?
V1 O16 V2 100.03(19) . . ?
V3 O15 V4 151.0(2) . . ?
V3 O15 V2 95.21(18) . . ?
V4 O15 V2 102.77(19) . . ?
Sb1 O13 V8 136.7(2) . . ?
Sb1 O13 V3 120.5(2) . 2_556 ?
V8 O13 V3 102.64(18) . 2_556 ?
Sb2 O12 V6 139.5(2) . 2_556 ?
Sb2 O12 V5 121.1(2) . . ?
V6 O12 V5 98.77(18) 2_556 . ?
V1 O11 V7 153.4(2) . . ?
V1 O11 V6 101.90(19) . . ?
V7 O11 V6 94.83(18) . . ?
Sb3 O10 Sb1 131.0(2) . . ?
V1 O9 V2 101.98(19) . . ?
V1 O9 V3 152.2(2) . . ?
V2 O9 V3 94.79(18) . . ?
Sb4 O7 V8 137.0(2) . 2_556 ?
Sb4 O7 V3 117.1(2) . . ?
V8 O7 V3 104.94(19) 2_556 . ?
V8 O6 Sb3 140.2(2) . . ?
V8 O6 V7 104.29(19) . . ?
Sb3 O6 V7 115.4(2) . . ?
Sb4 O5 Sb2 131.1(2) . 2_556 ?
Sb4 O4 V6 144.5(2) . . ?
Sb4 O4 V1 116.2(2) . . ?
V6 O4 V1 99.22(19) . . ?
N4 Co1 N3 80.1(4) . . ?
N4 Co1 N5 100.4(4) . . ?
N3 Co1 N5 91.6(3) . . ?
N4 Co1 N6 90.6(4) . . ?
N3 Co1 N6 166.4(3) . . ?
N5 Co1 N6 80.2(3) . . ?
N4 Co1 N2 168.3(4) . . ?
N3 Co1 N2 94.6(3) . . ?
N5 Co1 N2 90.0(3) . . ?
N6 Co1 N2 96.3(3) . . ?
N4 Co1 N1 91.5(3) . . ?
N3 Co1 N1 98.2(3) . . ?
N5 Co1 N1 165.7(3) . . ?
N6 Co1 N1 91.9(3) . . ?
N2 Co1 N1 78.9(2) . . ?
C6 N6 Co1 110.7(7) . . ?
N1 C1 C2 111.4(6) . . ?
C6 C5 C9 119.8(12) . . ?
C6 C5 N5 107.9(11) . . ?
C9 C5 N5 110.8(12) . . ?
C5 C6 N6 110.9(11) . . ?
C2 N2 Co1 110.4(4) . . ?
C1 N1 Co1 109.4(4) . . ?
N2 C2 C1 106.5(6) . . ?
N2 C2 C7 112.2(6) . . ?
C1 C2 C7 112.5(7) . . ?
C5 N5 Co1 105.2(6) . . ?
C3 N3 Co1 112.6(8) . . ?
C4 N4 Co1 106.2(9) . . ?
C3 C4 N4 116.4(13) . . ?
C3 C4 C8 100.1(15) . . ?
N4 C4 C8 119.4(14) . . ?
N3 C3 C4 107.4(12) . . ?

_refine_diff_density_max         1.934
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.172

