# Electronic Supplementary Material (ESI) for Chemical Science.
# 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_mh21
_database_code_depnum_ccdc_archive 'CCDC 1432847'
_audit_update_record             
;
2015-10-23 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
  '[Ni(C2H8N2)3]3{V15Sb6O42(H2O)}*9H2O'
;
_chemical_name_common            '[Ni(ethylendiamine)3]3{V15Sb6O42(H2O)}*9H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'V15Sb6O42, NiC6H24N6, C2H8N2, H2O'
_chemical_formula_sum            'C18 H92 N18 Ni3 O52 Sb6 V15'
_chemical_formula_weight         3063.82

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      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                   18.2404(7)
_cell_length_b                   22.7636(7)
_cell_length_c                   14.3542(5)
_cell_angle_alpha                90
_cell_angle_beta                 126.449(3)
_cell_angle_gamma                90
_cell_volume                     4794.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8392
_cell_measurement_theta_min      1.65
_cell_measurement_theta_max      27.00

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_F_000             2954
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    3.702
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.4902
_exptl_absorpt_correction_T_max  0.6693
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 2014)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14462
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.651
_diffrn_reflns_theta_max         27.002
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_point_group_measured_fraction_full 0.810
_reflns_number_total             8392
_reflns_number_gt                7488
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.580
_reflns_Friedel_fraction_max     0.602
_reflns_Friedel_fraction_full    0.622

_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       'STOE-IPDS Program Package'
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0623P)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 
;
 Flack x determined using 2492 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(13)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8392
_refine_ls_number_parameters     508
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0923
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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 0.00141(4) 0.59353(3) 0.83579(5) 0.03109(15) Uani 1 1 d . . . . .
Sb2 Sb -0.11551(5) 0.70164(3) 0.61722(6) 0.03968(18) Uani 1 1 d . . . . .
Sb3 Sb 0.08888(5) 0.34646(4) 0.48378(7) 0.04385(19) Uani 1 1 d . . . . .
V1 V 0.12488(9) 0.66743(7) 0.74237(13) 0.0255(3) Uani 1 1 d . . . . .
V2 V 0.0000 0.71591(10) 0.5000 0.0242(5) Uani 1 2 d S T P . .
V3 V 0.21773(9) 0.63103(7) 0.64411(13) 0.0249(3) Uani 1 1 d . . . . .
V4 V 0.19635(9) 0.55046(8) 0.46007(13) 0.0286(3) Uani 1 1 d . . . . .
V5 V 0.04934(10) 0.46282(8) 0.31086(13) 0.0276(3) Uani 1 1 d . . . . .
V6 V 0.22317(10) 0.46846(8) 0.63275(13) 0.0278(3) Uani 1 1 d . . . . .
V7 V 0.12626(10) 0.42295(8) 0.73269(14) 0.0290(3) Uani 1 1 d . . . . .
V8 V 0.17305(9) 0.54054(7) 0.82150(12) 0.0249(3) Uani 1 1 d . . . . .
O1 O -0.0689(5) 0.6641(3) 0.7613(6) 0.0370(17) Uani 1 1 d . . . . .
O2 O 0.0883(4) 0.6042(3) 0.8005(6) 0.0303(15) Uani 1 1 d . . . . .
O3 O -0.0809(4) 0.5451(3) 0.6960(5) 0.0325(15) Uani 1 1 d . . . . .
O4 O -0.0030(4) 0.6933(3) 0.6312(5) 0.0309(15) Uani 1 1 d . . . . .
O5 O -0.1683(4) 0.6320(3) 0.5235(6) 0.0309(15) Uani 1 1 d . . . . .
O6 O 0.2021(4) 0.6046(3) 0.7606(5) 0.0271(14) Uani 1 1 d . . . . .
O7 O 0.1821(5) 0.7156(4) 0.8427(6) 0.0392(18) Uani 1 1 d . . . . .
O8 O 0.1229(4) 0.6869(3) 0.6083(5) 0.0278(14) Uani 1 1 d . . . . .
O9 O 0.0000 0.7861(5) 0.5000 0.038(2) Uani 1 2 d S T P . .
O10 O 0.2367(4) 0.5511(3) 0.6175(5) 0.0295(14) Uani 1 1 d . . . . .
O11 O 0.3135(4) 0.6662(3) 0.7114(6) 0.0350(16) Uani 1 1 d . . . . .
O12 O 0.1608(4) 0.4708(3) 0.4653(5) 0.0318(15) Uani 1 1 d . . . . .
O13 O 0.2814(5) 0.5511(4) 0.4521(7) 0.0470(19) Uani 1 1 d . . . . .
O14 O 0.0056(4) 0.4031(3) 0.3682(6) 0.0343(16) Uani 1 1 d . . . . .
O15 O 0.0772(4) 0.4838(3) 0.7754(6) 0.0270(13) Uani 1 1 d . . . . .
O16 O 0.0675(5) 0.4252(4) 0.2315(6) 0.0434(19) Uani 1 1 d . . . . .
O17 O 0.1391(5) 0.4035(4) 0.6095(6) 0.0371(17) Uani 1 1 d . . . . .
O18 O 0.2031(4) 0.4849(3) 0.7467(6) 0.0297(14) Uani 1 1 d . . . . .
O19 O 0.3221(4) 0.4392(4) 0.6947(7) 0.0415(19) Uani 1 1 d . . . . .
O20 O 0.1809(6) 0.3752(4) 0.8355(7) 0.048(2) Uani 1 1 d . . . . .
O21 O 0.2505(4) 0.5345(4) 0.9578(6) 0.0360(17) Uani 1 1 d . . . . .
O22 O 0.0000 0.3129(6) 0.5000 0.049(3) Uani 1 2 d S T P . .
Ni1 Ni 0.28271(8) 0.38830(6) 0.22211(11) 0.0353(3) Uani 1 1 d . . . . .
N1 N 0.2853(7) 0.4776(5) 0.1781(9) 0.048(2) Uani 1 1 d . . . . .
H1N H 0.3285 0.4973 0.2409 0.057 Uiso 1 1 calc R U . . .
H2N H 0.2973 0.4791 0.1264 0.057 Uiso 1 1 calc R U . . .
C1 C 0.1988(9) 0.5028(6) 0.1311(13) 0.056(3) Uani 1 1 d . . . . .
H1A H 0.1925 0.5398 0.0935 0.067 Uiso 1 1 calc R U . . .
H1B H 0.1918 0.5102 0.1920 0.067 Uiso 1 1 calc R U . . .
C2 C 0.1285(8) 0.4603(7) 0.0456(11) 0.056(4) Uani 1 1 d . . . . .
H2A H 0.0683 0.4755 0.0140 0.067 Uiso 1 1 calc R U . . .
H2B H 0.1334 0.4554 -0.0177 0.067 Uiso 1 1 calc R U . . .
N2 N 0.1410(6) 0.4040(5) 0.1007(8) 0.043(2) Uani 1 1 d . . . . .
H3N H 0.1155 0.3756 0.0477 0.052 Uiso 1 1 calc R U . . .
H4N H 0.1145 0.4045 0.1365 0.052 Uiso 1 1 calc R U . . .
N11 N 0.2904(7) 0.3492(5) 0.0937(9) 0.049(2) Uani 1 1 d . . . . .
H5N H 0.2778 0.3110 0.0876 0.059 Uiso 1 1 calc R U . . .
H6N H 0.2507 0.3660 0.0252 0.059 Uiso 1 1 calc R U . . .
C11 C 0.3816(11) 0.3578(8) 0.1297(16) 0.069(4) Uani 1 1 d . . . . .
H11A H 0.3889 0.3983 0.1152 0.083 Uiso 1 1 calc R U . . .
H11B H 0.3924 0.3327 0.0845 0.083 Uiso 1 1 calc R U . . .
C12 C 0.4476(9) 0.3448(8) 0.2513(15) 0.071(5) Uani 1 1 d . . . . .
H12A H 0.5082 0.3546 0.2750 0.085 Uiso 1 1 calc R U . . .
H12B H 0.4463 0.3030 0.2641 0.085 Uiso 1 1 calc R U . . .
N12 N 0.4274(7) 0.3785(6) 0.3224(9) 0.056(3) Uani 1 1 d . . . . .
H7N H 0.4541 0.4136 0.3402 0.067 Uiso 1 1 calc R U . . .
H8N H 0.4484 0.3594 0.3879 0.067 Uiso 1 1 calc R U . . .
N21 N 0.2875(6) 0.4154(5) 0.3688(8) 0.046(2) Uani 1 1 d . . . . .
H9N H 0.3346 0.4394 0.4132 0.055 Uiso 1 1 calc R U . . .
H10N H 0.2367 0.4347 0.3450 0.055 Uiso 1 1 calc R U . . .
C21 C 0.2969(8) 0.3637(6) 0.4349(10) 0.045(3) Uani 1 1 d . . . . .
H21A H 0.2798 0.3732 0.4855 0.054 Uiso 1 1 calc R U . . .
H21B H 0.3597 0.3504 0.4824 0.054 Uiso 1 1 calc R U . . .
C22 C 0.2350(8) 0.3154(5) 0.3506(10) 0.042(3) Uani 1 1 d . . . . .
H22A H 0.2434 0.2796 0.3924 0.051 Uiso 1 1 calc R U . . .
H22B H 0.1717 0.3273 0.3076 0.051 Uiso 1 1 calc R U . . .
N22 N 0.2599(7) 0.3055(5) 0.2700(9) 0.047(2) Uani 1 1 d . . . . .
H11N H 0.2151 0.2865 0.2072 0.056 Uiso 1 1 calc R U . . .
H12N H 0.3101 0.2836 0.3045 0.056 Uiso 1 1 calc R U . . .
Ni2 Ni 0.5000 0.56737(10) 1.0000 0.0417(5) Uani 1 2 d S T P . .
N31 N 0.5327(7) 0.5720(6) 1.1690(8) 0.052(3) Uani 1 1 d . . . . .
H13N H 0.5416 0.5360 1.1981 0.063 Uiso 1 1 calc R U . . .
H14N H 0.5838 0.5924 1.2154 0.063 Uiso 1 1 calc R U . . .
C31 C 0.4580(10) 0.6003(9) 1.1630(13) 0.072(5) Uani 1 1 d . . . . .
H31A H 0.4790 0.6137 1.2393 0.087 Uiso 1 1 calc R U . . .
H31B H 0.4086 0.5726 1.1353 0.087 Uiso 1 1 calc R U . . .
C32 C 0.4254(11) 0.6512(8) 1.0819(14) 0.073(5) Uani 1 1 d . . . . .
H32A H 0.4722 0.6813 1.1154 0.088 Uiso 1 1 calc R U . . .
H32B H 0.3715 0.6680 1.0700 0.088 Uiso 1 1 calc R U . . .
N32 N 0.4033(6) 0.6317(6) 0.9683(9) 0.055(3) Uani 1 1 d . . . . .
H15N H 0.4053 0.6623 0.9311 0.066 Uiso 1 1 calc R U . . .
H16N H 0.3473 0.6166 0.9242 0.066 Uiso 1 1 calc R U . . .
N41 N 0.5891(6) 0.4958(5) 1.0428(9) 0.050(3) Uani 1 1 d . . . . .
H17N H 0.6211 0.5024 1.0154 0.060 Uiso 1 1 calc R U . . .
H18N H 0.6279 0.4925 1.1195 0.060 Uiso 1 1 calc R U . . .
C41 C 0.5370(9) 0.4410(8) 0.9934(16) 0.067(4) Uani 1 1 d . . . . .
H41A H 0.5119 0.4383 0.9121 0.080 Uiso 1 1 calc R U . . .
H41B H 0.5765 0.4075 1.0334 0.080 Uiso 1 1 calc R U . . .
O31 O 0.4449(9) 0.4784(8) 0.6480(16) 0.113(6) Uani 1 1 d . . . . .
O32 O -0.0393(11) 0.3202(8) 0.1287(15) 0.113(5) Uani 1 1 d . . . . .
O33 O 0.1160(13) 0.6850(9) 0.9881(16) 0.123(6) Uani 1 1 d . . . . .
O34 O 0.1351(13) 0.8181(9) 1.2265(18) 0.143(7) Uani 1 1 d . . . . .
O35 O 0.0000 0.7723(11) 1.0000 0.132(9) Uani 1 2 d S T P . .
O36 O 0.0000 0.553(2) 0.5000 0.211(18) Uani 1 2 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sb1 O1 1.935(7) . ?
Sb1 O2 1.944(7) . ?
Sb1 O3 1.978(7) . ?
Sb2 O1 1.908(7) . ?
Sb2 O5 1.927(7) . ?
Sb2 O4 1.949(7) . ?
Sb3 O22 1.927(5) . ?
Sb3 O14 1.930(7) . ?
Sb3 O17 1.953(8) . ?
V1 O7 1.607(7) . ?
V1 O6 1.913(7) . ?
V1 O8 1.954(7) . ?
V1 O2 1.968(7) . ?
V1 O4 1.978(6) . ?
V1 V3 2.895(2) . ?
V1 V2 3.0155(17) . ?
V1 V8 3.036(2) . ?
V2 O9 1.597(11) . ?
V2 O8 1.932(6) . ?
V2 O8 1.932(6) 2_556 ?
V2 O4 1.984(7) . ?
V2 O4 1.984(7) 2_556 ?
V2 V1 3.0155(17) 2_556 ?
V3 O11 1.619(7) . ?
V3 O10 1.931(8) . ?
V3 O6 1.951(7) . ?
V3 O8 1.955(7) . ?
V3 O5 2.006(7) 2_556 ?
V3 V4 3.045(2) . ?
V4 O13 1.621(8) . ?
V4 O10 1.916(7) . ?
V4 O12 1.941(8) . ?
V4 O3 1.965(6) 2_556 ?
V4 O5 1.975(7) 2_556 ?
V4 V6 2.903(2) . ?
V4 V5 2.989(2) . ?
V5 O16 1.610(8) . ?
V5 O15 1.921(6) 2_556 ?
V5 O12 1.930(6) . ?
V5 O3 1.980(8) 2_556 ?
V5 O14 1.985(8) . ?
V5 V7 3.016(2) 2_556 ?
V6 O19 1.607(7) . ?
V6 O18 1.912(7) . ?
V6 O10 1.927(8) . ?
V6 O12 1.956(7) . ?
V6 O17 2.011(8) . ?
V6 V7 3.044(2) . ?
V7 O20 1.614(8) . ?
V7 O18 1.913(7) . ?
V7 O15 1.936(7) . ?
V7 O17 1.967(8) . ?
V7 O14 1.987(7) 2_556 ?
V7 V8 2.868(2) . ?
V7 V5 3.016(2) 2_556 ?
V8 O21 1.600(7) . ?
V8 O6 1.929(7) . ?
V8 O18 1.939(7) . ?
V8 O15 1.946(6) . ?
V8 O2 2.008(7) . ?
O3 V4 1.965(6) 2_556 ?
O3 V5 1.980(8) 2_556 ?
O5 V4 1.976(7) 2_556 ?
O5 V3 2.006(7) 2_556 ?
O14 V7 1.987(7) 2_556 ?
O15 V5 1.921(6) 2_556 ?
O22 Sb3 1.927(5) 2_556 ?
Ni1 N2 2.120(8) . ?
Ni1 N11 2.125(11) . ?
Ni1 N22 2.131(11) . ?
Ni1 N1 2.137(11) . ?
Ni1 N12 2.139(10) . ?
Ni1 N21 2.146(11) . ?
N1 C1 1.418(16) . ?
C1 C2 1.49(2) . ?
C2 N2 1.451(18) . ?
N11 C11 1.431(18) . ?
C11 C12 1.45(2) . ?
C12 N12 1.49(2) . ?
N21 C21 1.457(16) . ?
C21 C22 1.524(18) . ?
C22 N22 1.489(16) . ?
Ni2 N41 2.117(11) 2_657 ?
Ni2 N41 2.117(11) . ?
Ni2 N32 2.124(11) . ?
Ni2 N32 2.124(12) 2_657 ?
Ni2 N31 2.129(10) 2_657 ?
Ni2 N31 2.129(10) . ?
N31 C31 1.46(2) . ?
C31 C32 1.49(3) . ?
C32 N32 1.496(19) . ?
N41 C41 1.47(2) . ?
C41 C41 1.47(3) 2_657 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sb1 O2 97.3(3) . . ?
O1 Sb1 O3 92.7(3) . . ?
O2 Sb1 O3 92.9(3) . . ?
O1 Sb2 O5 96.0(3) . . ?
O1 Sb2 O4 94.7(3) . . ?
O5 Sb2 O4 92.9(3) . . ?
O22 Sb3 O14 94.6(3) . . ?
O22 Sb3 O17 96.8(3) . . ?
O14 Sb3 O17 92.8(3) . . ?
O7 V1 O6 110.7(3) . . ?
O7 V1 O8 110.5(4) . . ?
O6 V1 O8 83.5(3) . . ?
O7 V1 O2 108.8(4) . . ?
O6 V1 O2 78.7(3) . . ?
O8 V1 O2 140.4(3) . . ?
O7 V1 O4 110.3(4) . . ?
O6 V1 O4 138.8(3) . . ?
O8 V1 O4 79.3(3) . . ?
O2 V1 O4 91.5(3) . . ?
O7 V1 V3 112.0(3) . . ?
O6 V1 V3 42.0(2) . . ?
O8 V1 V3 42.22(19) . . ?
O2 V1 V3 116.2(2) . . ?
O4 V1 V3 116.3(2) . . ?
O7 V1 V2 115.3(3) . . ?
O6 V1 V2 114.9(2) . . ?
O8 V1 V2 38.85(17) . . ?
O2 V1 V2 122.86(19) . . ?
O4 V1 V2 40.5(2) . . ?
V3 V1 V2 78.60(5) . . ?
O7 V1 V8 115.1(3) . . ?
O6 V1 V8 38.0(2) . . ?
O8 V1 V8 114.6(2) . . ?
O2 V1 V8 40.70(19) . . ?
O4 V1 V8 121.7(2) . . ?
V3 V1 V8 77.70(6) . . ?
V2 V1 V8 129.20(7) . . ?
O9 V2 O8 110.0(2) . . ?
O9 V2 O8 110.0(2) . 2_556 ?
O8 V2 O8 140.1(4) . 2_556 ?
O9 V2 O4 105.0(2) . . ?
O8 V2 O4 79.7(3) . . ?
O8 V2 O4 90.1(3) 2_556 . ?
O9 V2 O4 105.0(2) . 2_556 ?
O8 V2 O4 90.1(3) . 2_556 ?
O8 V2 O4 79.7(3) 2_556 2_556 ?
O4 V2 O4 150.0(5) . 2_556 ?
O9 V2 V1 111.46(5) . . ?
O8 V2 V1 39.4(2) . . ?
O8 V2 V1 121.5(2) 2_556 . ?
O4 V2 V1 40.38(17) . . ?
O4 V2 V1 124.9(2) 2_556 . ?
O9 V2 V1 111.46(5) . 2_556 ?
O8 V2 V1 121.5(2) . 2_556 ?
O8 V2 V1 39.4(2) 2_556 2_556 ?
O4 V2 V1 124.9(2) . 2_556 ?
O4 V2 V1 40.38(17) 2_556 2_556 ?
V1 V2 V1 137.07(10) . 2_556 ?
O11 V3 O10 109.1(3) . . ?
O11 V3 O6 107.2(3) . . ?
O10 V3 O6 90.8(3) . . ?
O11 V3 O8 107.9(3) . . ?
O10 V3 O8 142.7(3) . . ?
O6 V3 O8 82.5(3) . . ?
O11 V3 O5 105.5(4) . 2_556 ?
O10 V3 O5 77.2(3) . 2_556 ?
O6 V3 O5 147.3(3) . 2_556 ?
O8 V3 O5 88.9(3) . 2_556 ?
O11 V3 V1 107.7(3) . . ?
O10 V3 V1 126.2(2) . . ?
O6 V3 V1 40.97(19) . . ?
O8 V3 V1 42.2(2) . . ?
O5 V3 V1 127.2(2) 2_556 . ?
O11 V3 V4 110.7(3) . . ?
O10 V3 V4 37.52(19) . . ?
O6 V3 V4 123.3(2) . . ?
O8 V3 V4 121.79(19) . . ?
O5 V3 V4 39.8(2) 2_556 . ?
V1 V3 V4 141.69(6) . . ?
O13 V4 O10 111.7(4) . . ?
O13 V4 O12 111.5(4) . . ?
O10 V4 O12 82.2(3) . . ?
O13 V4 O3 110.0(4) . 2_556 ?
O10 V4 O3 138.2(3) . 2_556 ?
O12 V4 O3 80.2(3) . 2_556 ?
O13 V4 O5 109.1(4) . 2_556 ?
O10 V4 O5 78.3(3) . 2_556 ?
O12 V4 O5 139.2(3) . 2_556 ?
O3 V4 O5 90.9(3) 2_556 2_556 ?
O13 V4 V6 112.5(3) . . ?
O10 V4 V6 41.1(2) . . ?
O12 V4 V6 42.0(2) . . ?
O3 V4 V6 117.2(2) 2_556 . ?
O5 V4 V6 115.2(2) 2_556 . ?
O13 V4 V5 116.3(3) . . ?
O10 V4 V5 113.7(2) . . ?
O12 V4 V5 39.34(19) . . ?
O3 V4 V5 40.9(2) 2_556 . ?
O5 V4 V5 121.8(2) 2_556 . ?
V6 V4 V5 78.87(6) . . ?
O13 V4 V3 114.9(3) . . ?
O10 V4 V3 37.9(2) . . ?
O12 V4 V3 113.7(2) . . ?
O3 V4 V3 121.6(2) 2_556 . ?
O5 V4 V3 40.5(2) 2_556 . ?
V6 V4 V3 77.10(6) . . ?
V5 V4 V3 128.44(7) . . ?
O16 V5 O15 110.5(3) . 2_556 ?
O16 V5 O12 110.1(3) . . ?
O15 V5 O12 139.4(3) 2_556 . ?
O16 V5 O3 106.3(4) . 2_556 ?
O15 V5 O3 90.3(3) 2_556 2_556 ?
O12 V5 O3 80.1(3) . 2_556 ?
O16 V5 O14 103.3(4) . . ?
O15 V5 O14 79.2(3) 2_556 . ?
O12 V5 O14 89.8(3) . . ?
O3 V5 O14 150.4(3) 2_556 . ?
O16 V5 V4 112.8(3) . . ?
O15 V5 V4 121.2(2) 2_556 . ?
O12 V5 V4 39.6(2) . . ?
O3 V5 V4 40.56(17) 2_556 . ?
O14 V5 V4 124.8(2) . . ?
O16 V5 V7 109.5(3) . 2_556 ?
O15 V5 V7 38.8(2) 2_556 2_556 ?
O12 V5 V7 122.1(2) . 2_556 ?
O3 V5 V7 125.4(2) 2_556 2_556 ?
O14 V5 V7 40.64(19) . 2_556 ?
V4 V5 V7 137.70(7) . 2_556 ?
O19 V6 O18 109.3(4) . . ?
O19 V6 O10 106.9(4) . . ?
O18 V6 O10 90.5(3) . . ?
O19 V6 O12 109.5(4) . . ?
O18 V6 O12 141.1(3) . . ?
O10 V6 O12 81.6(3) . . ?
O19 V6 O17 106.4(4) . . ?
O18 V6 O17 76.8(3) . . ?
O10 V6 O17 146.7(3) . . ?
O12 V6 O17 89.2(3) . . ?
O19 V6 V4 107.6(3) . . ?
O18 V6 V4 125.7(2) . . ?
O10 V6 V4 40.8(2) . . ?
O12 V6 V4 41.7(2) . . ?
O17 V6 V4 127.3(2) . . ?
O19 V6 V7 111.9(3) . . ?
O18 V6 V7 37.3(2) . . ?
O10 V6 V7 122.3(2) . . ?
O12 V6 V7 120.8(2) . . ?
O17 V6 V7 39.5(2) . . ?
V4 V6 V7 140.42(7) . . ?
O20 V7 O18 112.6(4) . . ?
O20 V7 O15 110.1(4) . . ?
O18 V7 O15 83.5(3) . . ?
O20 V7 O17 109.4(4) . . ?
O18 V7 O17 77.8(3) . . ?
O15 V7 O17 140.4(3) . . ?
O20 V7 O14 109.6(4) . 2_556 ?
O18 V7 O14 137.6(3) . 2_556 ?
O15 V7 O14 78.8(3) . 2_556 ?
O17 V7 O14 91.9(3) . 2_556 ?
O20 V7 V8 111.3(3) . . ?
O18 V7 V8 42.2(2) . . ?
O15 V7 V8 42.51(19) . . ?
O17 V7 V8 116.6(2) . . ?
O14 V7 V8 116.6(2) 2_556 . ?
O20 V7 V5 113.3(3) . 2_556 ?
O18 V7 V5 115.0(2) . 2_556 ?
O15 V7 V5 38.40(18) . 2_556 ?
O17 V7 V5 124.1(2) . 2_556 ?
O14 V7 V5 40.6(2) 2_556 2_556 ?
V8 V7 V5 79.06(6) . 2_556 ?
O20 V7 V6 116.4(3) . . ?
O18 V7 V6 37.3(2) . . ?
O15 V7 V6 114.4(2) . . ?
O17 V7 V6 40.6(2) . . ?
O14 V7 V6 121.6(2) 2_556 . ?
V8 V7 V6 77.82(6) . . ?
V5 V7 V6 129.97(7) 2_556 . ?
O21 V8 O6 109.8(3) . . ?
O21 V8 O18 106.6(3) . . ?
O6 V8 O18 89.9(3) . . ?
O21 V8 O15 108.7(4) . . ?
O6 V8 O15 141.3(3) . . ?
O18 V8 O15 82.6(3) . . ?
O21 V8 O2 106.7(3) . . ?
O6 V8 O2 77.3(3) . . ?
O18 V8 O2 146.6(3) . . ?
O15 V8 O2 88.4(3) . . ?
O21 V8 V7 106.1(3) . . ?
O6 V8 V7 126.4(2) . . ?
O18 V8 V7 41.5(2) . . ?
O15 V8 V7 42.2(2) . . ?
O2 V8 V7 127.4(2) . . ?
O21 V8 V1 112.8(3) . . ?
O6 V8 V1 37.60(19) . . ?
O18 V8 V1 121.9(2) . . ?
O15 V8 V1 120.13(19) . . ?
O2 V8 V1 39.7(2) . . ?
V7 V8 V1 141.08(6) . . ?
Sb2 O1 Sb1 133.9(4) . . ?
Sb1 O2 V1 137.4(4) . . ?
Sb1 O2 V8 123.0(4) . . ?
V1 O2 V8 99.6(3) . . ?
V4 O3 Sb1 140.8(4) 2_556 . ?
V4 O3 V5 98.5(3) 2_556 2_556 ?
Sb1 O3 V5 120.6(3) . 2_556 ?
Sb2 O4 V1 141.0(4) . . ?
Sb2 O4 V2 119.9(3) . . ?
V1 O4 V2 99.1(3) . . ?
Sb2 O5 V4 138.4(4) . 2_556 ?
Sb2 O5 V3 121.9(4) . 2_556 ?
V4 O5 V3 99.7(3) 2_556 2_556 ?
V1 O6 V8 104.4(3) . . ?
V1 O6 V3 97.1(3) . . ?
V8 O6 V3 147.2(4) . . ?
V2 O8 V1 101.8(3) . . ?
V2 O8 V3 148.9(4) . . ?
V1 O8 V3 95.6(3) . . ?
V4 O10 V6 98.1(3) . . ?
V4 O10 V3 104.6(3) . . ?
V6 O10 V3 147.9(4) . . ?
V5 O12 V4 101.1(3) . . ?
V5 O12 V6 148.8(4) . . ?
V4 O12 V6 96.3(3) . . ?
Sb3 O14 V5 120.6(3) . . ?
Sb3 O14 V7 140.5(4) . 2_556 ?
V5 O14 V7 98.8(3) . 2_556 ?
V5 O15 V7 102.8(3) 2_556 . ?
V5 O15 V8 151.3(4) 2_556 . ?
V7 O15 V8 95.2(3) . . ?
Sb3 O17 V7 137.7(4) . . ?
Sb3 O17 V6 122.3(4) . . ?
V7 O17 V6 99.8(3) . . ?
V6 O18 V7 105.5(3) . . ?
V6 O18 V8 149.6(4) . . ?
V7 O18 V8 96.2(3) . . ?
Sb3 O22 Sb3 133.3(7) . 2_556 ?
N2 Ni1 N11 92.0(4) . . ?
N2 Ni1 N22 92.2(4) . . ?
N11 Ni1 N22 92.0(4) . . ?
N2 Ni1 N1 80.0(4) . . ?
N11 Ni1 N1 96.8(4) . . ?
N22 Ni1 N1 168.4(4) . . ?
N2 Ni1 N12 170.2(4) . . ?
N11 Ni1 N12 81.3(4) . . ?
N22 Ni1 N12 95.2(4) . . ?
N1 Ni1 N12 93.6(4) . . ?
N2 Ni1 N21 94.4(4) . . ?
N11 Ni1 N21 170.5(4) . . ?
N22 Ni1 N21 80.8(4) . . ?
N1 Ni1 N21 91.2(4) . . ?
N12 Ni1 N21 93.2(4) . . ?
C1 N1 Ni1 108.2(8) . . ?
N1 C1 C2 107.4(12) . . ?
N2 C2 C1 110.2(9) . . ?
C2 N2 Ni1 108.5(8) . . ?
C11 N11 Ni1 106.9(9) . . ?
N11 C11 C12 111.3(13) . . ?
C11 C12 N12 110.7(11) . . ?
C12 N12 Ni1 107.5(8) . . ?
C21 N21 Ni1 109.1(8) . . ?
N21 C21 C22 108.6(9) . . ?
N22 C22 C21 107.7(10) . . ?
C22 N22 Ni1 108.9(7) . . ?
N41 Ni2 N41 79.5(6) 2_657 . ?
N41 Ni2 N32 94.1(4) 2_657 . ?
N41 Ni2 N32 171.5(5) . . ?
N41 Ni2 N32 171.5(5) 2_657 2_657 ?
N41 Ni2 N32 94.1(4) . 2_657 ?
N32 Ni2 N32 92.8(7) . 2_657 ?
N41 Ni2 N31 93.4(5) 2_657 2_657 ?
N41 Ni2 N31 90.9(4) . 2_657 ?
N32 Ni2 N31 95.0(4) . 2_657 ?
N32 Ni2 N31 81.1(5) 2_657 2_657 ?
N41 Ni2 N31 90.9(4) 2_657 . ?
N41 Ni2 N31 93.4(5) . . ?
N32 Ni2 N31 81.1(5) . . ?
N32 Ni2 N31 95.0(4) 2_657 . ?
N31 Ni2 N31 174.4(7) 2_657 . ?
C31 N31 Ni2 109.5(8) . . ?
N31 C31 C32 108.3(13) . . ?
C31 C32 N32 110.1(14) . . ?
C32 N32 Ni2 108.6(9) . . ?
C41 N41 Ni2 110.4(7) . . ?
C41 C41 N41 108.5(11) 2_657 . ?

_refine_diff_density_max         1.258
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.136

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.255 0.000 7.8 4.8
2 0.500 0.755 0.000 7.8 4.8
3 0.500 0.672 0.500 327.7 33.5
4 1.000 0.172 0.500 327.7 33.5
5 0.000 0.545 0.500 21.9 5.5
6 0.500 0.045 0.500 21.9 5.5
_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_mh133
_database_code_depnum_ccdc_archive 'CCDC 1432848'
_audit_update_record             
;
2015-10-23 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 '[Co(C2H8N2)3]3{V15Sb6O42}*9H2O'  
;
_chemical_name_common            '[Co(ethylendiamine)3]3{V15Sb6O42}*9H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'V15Sb6O42, CoC6H24N6, C2H8N2, H2O'
_chemical_formula_sum            'C18 H90 Co3 N18 O51 Sb6 V15'
_chemical_formula_weight         3046.47

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2

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

_cell_length_a                   18.2302(14)
_cell_length_b                   22.6142(16)
_cell_length_c                   14.4067(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 126.360(7)
_cell_angle_gamma                90.00
_cell_volume                     4783.0(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    10404
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      28.00

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2928
_exptl_absorpt_coefficient_mu    3.639
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5249
_exptl_absorpt_correction_T_max  0.6407
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            19592
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         28.00
_reflns_number_total             10404
_reflns_number_gt                9465
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'STOE-IPDS Program Package'
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0854P)²+1.8281P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(3)
_refine_ls_number_reflns         10404
_refine_ls_number_parameters     503
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.1187
_refine_ls_wR_factor_gt          0.1149
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.99968(3) 0.40575(2) 0.16602(4) 0.02197(10) Uani 1 1 d . . .
Sb2 Sb 1.11696(3) 0.29728(2) 0.38515(4) 0.02378(11) Uani 1 1 d . . .
Sb3 Sb 0.91058(4) 0.65538(2) 0.51602(6) 0.03440(14) Uani 1 1 d . . .
V1 V 0.87502(7) 0.33235(5) 0.25858(10) 0.0172(2) Uani 1 1 d . . .
V2 V 1.0000 0.28389(7) 0.5000 0.0164(3) Uani 1 2 d S . .
V3 V 0.78113(7) 0.36900(5) 0.35438(10) 0.0170(2) Uani 1 1 d . . .
V4 V 0.80239(8) 0.44970(5) 0.53783(11) 0.0201(2) Uani 1 1 d . . .
V5 V 0.94987(8) 0.53769(5) 0.68700(11) 0.0222(2) Uani 1 1 d . . .
V6 V 0.77609(8) 0.53288(5) 0.36672(12) 0.0219(2) Uani 1 1 d . . .
V7 V 0.87374(9) 0.57806(5) 0.26736(12) 0.0244(3) Uani 1 1 d . . .
V8 V 0.82689(8) 0.46017(5) 0.17887(10) 0.0190(2) Uani 1 1 d . . .
O1 O 1.0722(4) 0.3342(2) 0.2404(5) 0.0246(10) Uani 1 1 d . . .
O2 O 0.9122(3) 0.3961(2) 0.2014(5) 0.0221(10) Uani 1 1 d . . .
O3 O 1.0816(3) 0.4547(2) 0.3083(5) 0.0229(10) Uani 1 1 d . . .
O4 O 1.0032(3) 0.3070(2) 0.3698(4) 0.0203(9) Uani 1 1 d . . .
O5 O 1.1709(4) 0.3678(2) 0.4795(5) 0.0252(11) Uani 1 1 d . . .
O6 O 0.7968(3) 0.3962(2) 0.2384(4) 0.0190(9) Uani 1 1 d . . .
O7 O 0.8184(4) 0.2838(2) 0.1576(5) 0.0284(11) Uani 1 1 d . . .
O8 O 0.8770(3) 0.3125(2) 0.3921(4) 0.0188(9) Uani 1 1 d . . .
O9 O 1.0000 0.2133(3) 0.5000 0.0239(14) Uani 1 2 d S . .
O10 O 0.7616(3) 0.4491(2) 0.3809(5) 0.0224(10) Uani 1 1 d . . .
O11 O 0.6850(3) 0.3336(2) 0.2871(5) 0.0265(11) Uani 1 1 d . . .
O12 O 0.8381(4) 0.5301(2) 0.5333(5) 0.0248(10) Uani 1 1 d . . .
O13 O 0.7162(4) 0.4491(3) 0.5443(5) 0.0324(12) Uani 1 1 d . . .
O14 O 0.9953(4) 0.5971(2) 0.6307(6) 0.0294(12) Uani 1 1 d . . .
O15 O 0.9232(4) 0.5167(2) 0.2246(5) 0.0250(10) Uani 1 1 d . . .
O16 O 0.9314(4) 0.5754(3) 0.7666(6) 0.0316(12) Uani 1 1 d . . .
O17 O 0.8602(4) 0.5984(2) 0.3902(5) 0.0293(12) Uani 1 1 d . . .
O18 O 0.7958(4) 0.5158(2) 0.2529(5) 0.0238(10) Uani 1 1 d . . .
O19 O 0.6764(4) 0.5629(3) 0.3033(6) 0.0333(13) Uani 1 1 d . . .
O20 O 0.8207(5) 0.6268(3) 0.1661(6) 0.0376(14) Uani 1 1 d . . .
O21 O 0.7502(4) 0.4665(3) 0.0431(5) 0.0295(12) Uani 1 1 d . . .
O22 O 1.0000 0.6897(4) 0.5000 0.043(2) Uani 1 2 d S . .
Co1 Co 0.71731(7) 0.61129(5) 0.77756(10) 0.0275(2) Uani 1 1 d . . .
N1 N 0.7133(5) 0.5183(3) 0.8191(8) 0.0369(16) Uani 1 1 d . . .
H1N H 0.6991 0.5157 0.8706 0.044 Uiso 1 1 calc R . .
H2N H 0.6701 0.4977 0.7535 0.044 Uiso 1 1 calc R . .
C1 C 0.8032(8) 0.4943(4) 0.8694(10) 0.045(2) Uani 1 1 d . . .
H1A H 0.8115 0.4875 0.8083 0.054 Uiso 1 1 calc R . .
H1B H 0.8100 0.4560 0.9069 0.054 Uiso 1 1 calc R . .
C2 C 0.8737(6) 0.5371(4) 0.9567(9) 0.039(2) Uani 1 1 d . . .
H2A H 0.8678 0.5419 1.0203 0.046 Uiso 1 1 calc R . .
H2B H 0.9353 0.5215 0.9895 0.046 Uiso 1 1 calc R . .
N2 N 0.8614(5) 0.5945(3) 0.9016(7) 0.0318(15) Uani 1 1 d . . .
H3N H 0.8892 0.5941 0.8652 0.038 Uiso 1 1 calc R . .
H4N H 0.8876 0.6239 0.9563 0.038 Uiso 1 1 calc R . .
N11 N 0.7099(6) 0.6515(4) 0.9085(7) 0.0398(17) Uani 1 1 d . . .
H5N H 0.7522 0.6348 0.9793 0.048 Uiso 1 1 calc R . .
H6N H 0.7210 0.6915 0.9130 0.048 Uiso 1 1 calc R . .
C11 C 0.6192(8) 0.6408(5) 0.8743(10) 0.046(2) Uani 1 1 d . . .
H11A H 0.6078 0.6657 0.9211 0.055 Uiso 1 1 calc R . .
H11B H 0.6133 0.5989 0.8885 0.055 Uiso 1 1 calc R . .
C12 C 0.5518(7) 0.6545(4) 0.7520(11) 0.049(3) Uani 1 1 d . . .
H12A H 0.5532 0.6974 0.7393 0.059 Uiso 1 1 calc R . .
H12B H 0.4901 0.6445 0.7289 0.059 Uiso 1 1 calc R . .
N12 N 0.5705(5) 0.6205(4) 0.6792(8) 0.0423(19) Uani 1 1 d . . .
H7N H 0.5477 0.6403 0.6114 0.051 Uiso 1 1 calc R . .
H8N H 0.5434 0.5838 0.6618 0.051 Uiso 1 1 calc R . .
N21 N 0.7114(6) 0.5846(3) 0.6274(7) 0.0364(16) Uani 1 1 d . . .
H9N H 0.7635 0.5645 0.6504 0.044 Uiso 1 1 calc R . .
H10N H 0.6622 0.5602 0.5806 0.044 Uiso 1 1 calc R . .
C21 C 0.7026(6) 0.6387(4) 0.5649(8) 0.0341(18) Uani 1 1 d . . .
H21A H 0.6394 0.6537 0.5210 0.041 Uiso 1 1 calc R . .
H21B H 0.7167 0.6299 0.5097 0.041 Uiso 1 1 calc R . .
C22 C 0.7673(6) 0.6846(3) 0.6496(8) 0.0308(17) Uani 1 1 d . . .
H22A H 0.8308 0.6702 0.6925 0.037 Uiso 1 1 calc R . .
H22B H 0.7618 0.7214 0.6087 0.037 Uiso 1 1 calc R . .
N22 N 0.7437(6) 0.6960(3) 0.7298(7) 0.0348(15) Uani 1 1 d . . .
H11N H 0.6928 0.7197 0.6949 0.042 Uiso 1 1 calc R . .
H12N H 0.7909 0.7152 0.7945 0.042 Uiso 1 1 calc R . .
Co2 Co 0.5000 0.43093(7) 0.0000 0.0288(3) Uani 1 2 d S . .
N31 N 0.4702(5) 0.4255(4) -0.1703(7) 0.0361(16) Uani 1 1 d . . .
H13N H 0.4180 0.4038 -0.2192 0.043 Uiso 1 1 calc R . .
H14N H 0.4619 0.4627 -0.2008 0.043 Uiso 1 1 calc R . .
C31 C 0.5497(8) 0.3960(6) -0.1557(10) 0.056(3) Uani 1 1 d . . .
H31A H 0.6005 0.4245 -0.1241 0.068 Uiso 1 1 calc R . .
H31B H 0.5325 0.3821 -0.2314 0.068 Uiso 1 1 calc R . .
C32 C 0.5793(8) 0.3447(5) -0.0754(10) 0.048(2) Uani 1 1 d . . .
H32A H 0.5309 0.3142 -0.1114 0.058 Uiso 1 1 calc R . .
H32B H 0.6350 0.3269 -0.0605 0.058 Uiso 1 1 calc R . .
N32 N 0.5975(5) 0.3638(4) 0.0324(7) 0.0379(17) Uani 1 1 d . . .
H15N H 0.6556 0.3788 0.0799 0.045 Uiso 1 1 calc R . .
H16N H 0.5934 0.3320 0.0690 0.045 Uiso 1 1 calc R . .
N41 N 0.4084(5) 0.5053(4) -0.0466(8) 0.0418(19) Uani 1 1 d . . .
H17N H 0.3693 0.5089 -0.1255 0.050 Uiso 1 1 calc R . .
H18N H 0.3743 0.4992 -0.0195 0.050 Uiso 1 1 calc R . .
C41 C 0.4625(8) 0.5590(6) 0.0037(14) 0.063(4) Uani 1 1 d . . .
H41A H 0.4235 0.5940 -0.0374 0.076 Uiso 1 1 calc R . .
H41B H 0.4858 0.5619 0.0855 0.076 Uiso 1 1 calc R . .
O31 O 0.5575(7) 0.5213(4) 0.3497(11) 0.071(3) Uani 1 1 d . . .
O32 O 1.0401(7) 0.6765(4) 0.8742(11) 0.077(3) Uani 1 1 d . . .
O33 O 0.8911(8) 0.3179(4) 0.0201(8) 0.066(2) Uani 1 1 d . . .
O34 O 0.8737(8) 0.1846(5) -0.2221(11) 0.081(3) Uani 1 1 d . . .
O35 O 1.0000 0.2307(7) 0.0000 0.117(8) Uani 1 2 d S . .


_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 O2 1.953(5) . ?
Sb1 O1 1.958(5) . ?
Sb1 O3 2.007(5) . ?
Sb2 O1 1.921(6) . ?
Sb2 O5 1.942(6) . ?
Sb2 O4 1.963(5) . ?
Sb3 O22 1.939(3) . ?
Sb3 O17 1.953(6) . ?
Sb3 O14 1.956(6) . ?
V1 O7 1.615(5) . ?
V1 O6 1.927(5) . ?
V1 O8 1.955(5) . ?
V1 O2 1.969(5) . ?
V1 O4 1.979(5) . ?
V1 V3 2.8848(15) . ?
V1 V2 3.0155(13) . ?
V1 V8 3.0413(16) . ?
V2 O9 1.597(7) . ?
V2 O8 1.931(5) 2_756 ?
V2 O8 1.931(5) . ?
V2 O4 1.981(5) . ?
V2 O4 1.981(5) 2_756 ?
V2 V1 3.0155(13) 2_756 ?
V3 O11 1.624(5) . ?
V3 O10 1.928(5) . ?
V3 O6 1.954(5) . ?
V3 O8 1.963(5) . ?
V3 O5 2.003(6) 2_756 ?
V3 V4 3.0417(17) . ?
V4 O13 1.628(5) . ?
V4 O10 1.916(5) . ?
V4 O12 1.945(6) . ?
V4 O3 1.960(5) 2_756 ?
V4 O5 1.969(5) 2_756 ?
V4 V6 2.9058(17) . ?
V4 V5 2.9925(17) . ?
V5 O16 1.616(5) . ?
V5 O15 1.926(5) 2_756 ?
V5 O12 1.932(6) . ?
V5 O3 1.975(5) 2_756 ?
V5 O14 1.986(6) . ?
V5 V7 3.0165(16) 2_756 ?
V6 O19 1.621(5) . ?
V6 O18 1.914(5) . ?
V6 O10 1.940(5) . ?
V6 O12 1.956(6) . ?
V6 O17 2.012(6) . ?
V6 V7 3.0469(16) . ?
V7 O20 1.614(6) . ?
V7 O18 1.922(5) . ?
V7 O15 1.943(5) . ?
V7 O14 1.971(6) 2_756 ?
V7 O17 1.981(6) . ?
V7 V8 2.8585(18) . ?
V7 V5 3.0165(16) 2_756 ?
V8 O21 1.600(6) . ?
V8 O6 1.920(5) . ?
V8 O18 1.939(5) . ?
V8 O15 1.944(5) . ?
V8 O2 2.007(5) . ?
O3 V4 1.960(5) 2_756 ?
O3 V5 1.975(5) 2_756 ?
O5 V4 1.969(5) 2_756 ?
O5 V3 2.003(6) 2_756 ?
O14 V7 1.971(6) 2_756 ?
O15 V5 1.926(5) 2_756 ?
O22 Sb3 1.939(3) 2_756 ?
Co1 N2 2.162(7) . ?
Co1 N11 2.169(7) . ?
Co1 N12 2.172(7) . ?
Co1 N22 2.184(7) . ?
Co1 N21 2.186(8) . ?
Co1 N1 2.201(7) . ?
N1 C1 1.448(12) . ?
C1 C2 1.500(16) . ?
C2 N2 1.468(10) . ?
N11 C11 1.438(13) . ?
C11 C12 1.464(17) . ?
C12 N12 1.494(14) . ?
N21 C21 1.470(11) . ?
C21 C22 1.500(13) . ?
C22 N22 1.477(11) . ?
Co2 N32 2.168(8) 2_655 ?
Co2 N32 2.168(8) . ?
Co2 N41 2.177(8) 2_655 ?
Co2 N41 2.177(8) . ?
Co2 N31 2.180(8) . ?
Co2 N31 2.180(8) 2_655 ?
N31 C31 1.493(14) . ?
C31 C32 1.495(18) . ?
C32 N32 1.449(13) . ?
N41 C41 1.458(16) . ?
C41 C41 1.43(2) 2_655 ?

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
O2 Sb1 O1 98.9(2) . . ?
O2 Sb1 O3 91.3(2) . . ?
O1 Sb1 O3 92.6(2) . . ?
O1 Sb2 O5 96.7(2) . . ?
O1 Sb2 O4 95.1(2) . . ?
O5 Sb2 O4 92.9(2) . . ?
O22 Sb3 O17 96.9(2) . . ?
O22 Sb3 O14 94.1(2) . . ?
O17 Sb3 O14 92.3(2) . . ?
O7 V1 O6 110.7(3) . . ?
O7 V1 O8 111.1(3) . . ?
O6 V1 O8 84.3(2) . . ?
O7 V1 O2 108.4(3) . . ?
O6 V1 O2 78.21(19) . . ?
O8 V1 O2 140.3(2) . . ?
O7 V1 O4 110.4(3) . . ?
O6 V1 O4 138.8(2) . . ?
O8 V1 O4 79.2(2) . . ?
O2 V1 O4 91.0(2) . . ?
O7 V1 V3 112.5(2) . . ?
O6 V1 V3 42.35(14) . . ?
O8 V1 V3 42.70(14) . . ?
O2 V1 V3 116.03(14) . . ?
O4 V1 V3 116.52(15) . . ?
O7 V1 V2 115.7(2) . . ?
O6 V1 V2 115.60(15) . . ?
O8 V1 V2 38.83(13) . . ?
O2 V1 V2 122.44(16) . . ?
O4 V1 V2 40.43(14) . . ?
V3 V1 V2 79.02(4) . . ?
O7 V1 V8 114.8(2) . . ?
O6 V1 V8 37.67(14) . . ?
O8 V1 V8 114.98(14) . . ?
O2 V1 V8 40.55(13) . . ?
O4 V1 V8 121.28(15) . . ?
V3 V1 V8 77.72(4) . . ?
V2 V1 V8 129.23(5) . . ?
O9 V2 O8 109.59(14) . 2_756 ?
O9 V2 O8 109.59(14) . . ?
O8 V2 O8 140.8(3) 2_756 . ?
O9 V2 O4 105.27(15) . . ?
O8 V2 O4 90.1(2) 2_756 . ?
O8 V2 O4 79.7(2) . . ?
O9 V2 O4 105.27(15) . 2_756 ?
O8 V2 O4 79.7(2) 2_756 2_756 ?
O8 V2 O4 90.1(2) . 2_756 ?
O4 V2 O4 149.5(3) . 2_756 ?
O9 V2 V1 111.31(3) . 2_756 ?
O8 V2 V1 39.40(15) 2_756 2_756 ?
O8 V2 V1 121.94(15) . 2_756 ?
O4 V2 V1 124.77(15) . 2_756 ?
O4 V2 V1 40.39(14) 2_756 2_756 ?
O9 V2 V1 111.31(3) . . ?
O8 V2 V1 121.94(15) 2_756 . ?
O8 V2 V1 39.40(15) . . ?
O4 V2 V1 40.39(14) . . ?
O4 V2 V1 124.77(15) 2_756 . ?
V1 V2 V1 137.38(7) 2_756 . ?
O11 V3 O10 108.7(2) . . ?
O11 V3 O6 107.3(3) . . ?
O10 V3 O6 90.6(2) . . ?
O11 V3 O8 108.3(2) . . ?
O10 V3 O8 142.7(2) . . ?
O6 V3 O8 83.4(2) . . ?
O11 V3 O5 105.0(3) . 2_756 ?
O10 V3 O5 77.1(2) . 2_756 ?
O6 V3 O5 147.6(2) . 2_756 ?
O8 V3 O5 88.5(2) . 2_756 ?
O11 V3 V1 108.0(2) . . ?
O10 V3 V1 126.63(15) . . ?
O6 V3 V1 41.64(14) . . ?
O8 V3 V1 42.47(15) . . ?
O5 V3 V1 127.23(16) 2_756 . ?
O11 V3 V4 110.5(2) . . ?
O10 V3 V4 37.55(16) . . ?
O6 V3 V4 123.09(15) . . ?
O8 V3 V4 121.04(16) . . ?
O5 V3 V4 39.61(15) 2_756 . ?
V1 V3 V4 141.45(5) . . ?
O13 V4 O10 110.8(3) . . ?
O13 V4 O12 111.3(3) . . ?
O10 V4 O12 82.6(2) . . ?
O13 V4 O3 111.5(3) . 2_756 ?
O10 V4 O3 137.6(2) . 2_756 ?
O12 V4 O3 79.9(2) . 2_756 ?
O13 V4 O5 108.6(3) . 2_756 ?
O10 V4 O5 78.2(2) . 2_756 ?
O12 V4 O5 139.6(2) . 2_756 ?
O3 V4 O5 90.9(2) 2_756 2_756 ?
O13 V4 V6 112.0(2) . . ?
O10 V4 V6 41.42(15) . . ?
O12 V4 V6 41.99(17) . . ?
O3 V4 V6 116.53(15) 2_756 . ?
O5 V4 V6 115.48(17) 2_756 . ?
O13 V4 V5 116.8(2) . . ?
O10 V4 V5 114.01(16) . . ?
O12 V4 V5 39.33(17) . . ?
O3 V4 V5 40.68(15) 2_756 . ?
O5 V4 V5 122.15(17) 2_756 . ?
V6 V4 V5 78.75(5) . . ?
O13 V4 V3 114.5(2) . . ?
O10 V4 V3 37.82(15) . . ?
O12 V4 V3 113.84(17) . . ?
O3 V4 V3 120.88(16) 2_756 . ?
O5 V4 V3 40.43(17) 2_756 . ?
V6 V4 V3 77.25(4) . . ?
V5 V4 V3 128.34(5) . . ?
O16 V5 O15 109.5(3) . 2_756 ?
O16 V5 O12 109.8(3) . . ?
O15 V5 O12 140.6(2) 2_756 . ?
O16 V5 O3 106.9(3) . 2_756 ?
O15 V5 O3 90.1(2) 2_756 2_756 ?
O12 V5 O3 79.9(2) . 2_756 ?
O16 V5 O14 104.2(3) . . ?
O15 V5 O14 78.9(2) 2_756 . ?
O12 V5 O14 90.2(2) . . ?
O3 V5 O14 148.9(2) 2_756 . ?
O16 V5 V4 112.6(2) . . ?
O15 V5 V4 121.80(16) 2_756 . ?
O12 V5 V4 39.64(16) . . ?
O3 V5 V4 40.31(16) 2_756 . ?
O14 V5 V4 124.84(19) . . ?
O16 V5 V7 109.2(2) . 2_756 ?
O15 V5 V7 38.97(17) 2_756 2_756 ?
O12 V5 V7 122.68(17) . 2_756 ?
O3 V5 V7 124.99(16) 2_756 2_756 ?
O14 V5 V7 40.15(18) . 2_756 ?
V4 V5 V7 138.21(5) . 2_756 ?
O19 V6 O18 108.6(3) . . ?
O19 V6 O10 106.9(3) . . ?
O18 V6 O10 90.0(2) . . ?
O19 V6 O12 110.2(3) . . ?
O18 V6 O12 141.2(2) . . ?
O10 V6 O12 81.7(2) . . ?
O19 V6 O17 105.9(3) . . ?
O18 V6 O17 77.4(2) . . ?
O10 V6 O17 147.1(2) . . ?
O12 V6 O17 89.3(2) . . ?
O19 V6 V4 108.3(2) . . ?
O18 V6 V4 125.17(16) . . ?
O10 V6 V4 40.78(16) . . ?
O12 V6 V4 41.71(16) . . ?
O17 V6 V4 127.45(18) . . ?
O19 V6 V7 111.5(2) . . ?
O18 V6 V7 37.50(16) . . ?
O10 V6 V7 122.07(15) . . ?
O12 V6 V7 120.89(17) . . ?
O17 V6 V7 39.89(17) . . ?
V4 V6 V7 140.10(5) . . ?
O20 V7 O18 113.2(3) . . ?
O20 V7 O15 110.1(3) . . ?
O18 V7 O15 84.0(2) . . ?
O20 V7 O14 109.6(3) . 2_756 ?
O18 V7 O14 137.1(2) . 2_756 ?
O15 V7 O14 78.9(2) . 2_756 ?
O20 V7 O17 108.9(3) . . ?
O18 V7 O17 78.0(2) . . ?
O15 V7 O17 140.9(2) . . ?
O14 V7 O17 91.2(3) 2_756 . ?
O20 V7 V8 111.9(3) . . ?
O18 V7 V8 42.47(15) . . ?
O15 V7 V8 42.67(15) . . ?
O14 V7 V8 116.47(17) 2_756 . ?
O17 V7 V8 116.93(17) . . ?
O20 V7 V5 113.2(2) . 2_756 ?
O18 V7 V5 115.23(15) . 2_756 ?
O15 V7 V5 38.56(16) . 2_756 ?
O14 V7 V5 40.52(17) 2_756 2_756 ?
O17 V7 V5 123.84(19) . 2_756 ?
V8 V7 V5 79.22(4) . 2_756 ?
O20 V7 V6 116.7(2) . . ?
O18 V7 V6 37.33(16) . . ?
O15 V7 V6 114.81(16) . . ?
O14 V7 V6 120.69(18) 2_756 . ?
O17 V7 V6 40.65(17) . . ?
V8 V7 V6 78.08(4) . . ?
V5 V7 V6 129.82(5) 2_756 . ?
O21 V8 O6 109.9(3) . . ?
O21 V8 O18 106.6(3) . . ?
O6 V8 O18 89.4(2) . . ?
O21 V8 O15 108.3(3) . . ?
O6 V8 O15 141.6(2) . . ?
O18 V8 O15 83.5(2) . . ?
O21 V8 O2 107.1(3) . . ?
O6 V8 O2 77.49(19) . . ?
O18 V8 O2 146.2(2) . . ?
O15 V8 O2 87.9(2) . . ?
O21 V8 V7 106.0(2) . . ?
O6 V8 V7 126.32(16) . . ?
O18 V8 V7 42.00(15) . . ?
O15 V8 V7 42.65(16) . . ?
O2 V8 V7 127.11(16) . . ?
O21 V8 V1 113.2(2) . . ?
O6 V8 V1 37.85(13) . . ?
O18 V8 V1 121.49(16) . . ?
O15 V8 V1 119.79(16) . . ?
O2 V8 V1 39.65(14) . . ?
V7 V8 V1 140.81(6) . . ?
Sb2 O1 Sb1 131.9(3) . . ?
Sb1 O2 V1 136.7(2) . . ?
Sb1 O2 V8 123.5(2) . . ?
V1 O2 V8 99.8(2) . . ?
V4 O3 V5 99.0(2) 2_756 2_756 ?
V4 O3 Sb1 140.7(3) 2_756 . ?
V5 O3 Sb1 120.3(3) 2_756 . ?
Sb2 O4 V1 141.7(3) . . ?
Sb2 O4 V2 119.1(2) . . ?
V1 O4 V2 99.2(2) . . ?
Sb2 O5 V4 138.1(3) . 2_756 ?
Sb2 O5 V3 121.9(3) . 2_756 ?
V4 O5 V3 100.0(2) 2_756 2_756 ?
V8 O6 V1 104.5(2) . . ?
V8 O6 V3 147.6(3) . . ?
V1 O6 V3 96.0(2) . . ?
V2 O8 V1 101.8(2) . . ?
V2 O8 V3 149.2(3) . . ?
V1 O8 V3 94.8(2) . . ?
V4 O10 V3 104.6(2) . . ?
V4 O10 V6 97.8(2) . . ?
V3 O10 V6 147.6(3) . . ?
V5 O12 V4 101.0(3) . . ?
V5 O12 V6 148.6(3) . . ?
V4 O12 V6 96.3(2) . . ?
Sb3 O14 V7 141.0(3) . 2_756 ?
Sb3 O14 V5 119.3(3) . . ?
V7 O14 V5 99.3(3) 2_756 . ?
V5 O15 V7 102.5(3) 2_756 . ?
V5 O15 V8 151.1(3) 2_756 . ?
V7 O15 V8 94.7(2) . . ?
Sb3 O17 V7 138.0(3) . . ?
Sb3 O17 V6 122.3(3) . . ?
V7 O17 V6 99.5(3) . . ?
V6 O18 V7 105.2(3) . . ?
V6 O18 V8 150.0(3) . . ?
V7 O18 V8 95.5(2) . . ?
Sb3 O22 Sb3 132.8(5) . 2_756 ?
N2 Co1 N11 91.5(3) . . ?
N2 Co1 N12 168.4(3) . . ?
N11 Co1 N12 80.7(3) . . ?
N2 Co1 N22 91.6(3) . . ?
N11 Co1 N22 92.6(3) . . ?
N12 Co1 N22 97.3(3) . . ?
N2 Co1 N21 95.3(3) . . ?
N11 Co1 N21 169.8(3) . . ?
N12 Co1 N21 93.6(3) . . ?
N22 Co1 N21 79.7(3) . . ?
N2 Co1 N1 80.1(3) . . ?
N11 Co1 N1 97.7(3) . . ?
N12 Co1 N1 92.4(3) . . ?
N22 Co1 N1 166.9(3) . . ?
N21 Co1 N1 90.9(3) . . ?
C1 N1 Co1 106.4(6) . . ?
N1 C1 C2 109.4(7) . . ?
N2 C2 C1 109.6(8) . . ?
C2 N2 Co1 108.8(5) . . ?
C11 N11 Co1 106.5(7) . . ?
N11 C11 C12 110.6(8) . . ?
C11 C12 N12 111.0(8) . . ?
C12 N12 Co1 107.3(6) . . ?
C21 N21 Co1 107.5(5) . . ?
N21 C21 C22 109.3(7) . . ?
N22 C22 C21 107.7(7) . . ?
C22 N22 Co1 108.3(5) . . ?
N32 Co2 N32 91.0(4) 2_655 . ?
N32 Co2 N41 171.4(3) 2_655 2_655 ?
N32 Co2 N41 95.4(3) . 2_655 ?
N32 Co2 N41 95.4(3) 2_655 . ?
N32 Co2 N41 171.4(3) . . ?
N41 Co2 N41 78.8(4) 2_655 . ?
N32 Co2 N31 95.3(3) 2_655 . ?
N32 Co2 N31 80.1(3) . . ?
N41 Co2 N31 91.4(3) 2_655 . ?
N41 Co2 N31 93.6(3) . . ?
N32 Co2 N31 80.1(3) 2_655 2_655 ?
N32 Co2 N31 95.3(3) . 2_655 ?
N41 Co2 N31 93.6(3) 2_655 2_655 ?
N41 Co2 N31 91.4(3) . 2_655 ?
N31 Co2 N31 173.5(4) . 2_655 ?
C31 N31 Co2 107.1(6) . . ?
N31 C31 C32 109.2(8) . . ?
N32 C32 C31 110.3(8) . . ?
C32 N32 Co2 109.9(6) . . ?
C41 N41 Co2 108.8(6) . . ?
C41 C41 N41 110.9(9) 2_655 . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.867
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.177
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.500 0.328 0.500 320.8 47.2
2 1.000 0.828 0.500 320.8 47.2
3 0.000 0.454 0.500 21.9 10.7
4 0.500 0.954 0.500 21.9 10.7
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_mh231
_database_code_depnum_ccdc_archive 'CCDC 1432849'
_audit_update_record             
;
2015-10-23 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 '[Fe(C2H8N2)3]3{V15Sb6O42}*9H2O'  
;
_chemical_name_common            '[Fe(ethylendiamine)3]3{V15Sb6O42}*9H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'V15Sb6O42, NiC6H24N6, C2H8N2, H2O'
_chemical_formula_sum            'C18 H90 Fe3 N18 O51 Sb6 V15'
_chemical_formula_weight         3037.23

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'
Fe Fe 0.3463 0.8444 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2

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

_cell_length_a                   18.1991(4)
_cell_length_b                   22.6260(6)
_cell_length_c                   14.3614(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 126.1930(10)
_cell_angle_gamma                90.00
_cell_volume                     4772.49(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    11411
_cell_measurement_theta_min      1.65
_cell_measurement_theta_max      27.94

_exptl_crystal_description       block
_exptl_crystal_colour            red-brown
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2922
_exptl_absorpt_coefficient_mu    3.582
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.3124
_exptl_absorpt_correction_T_max  0.7136
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            37515
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.65
_diffrn_reflns_theta_max         27.94
_reflns_number_total             11411
_reflns_number_gt                10527
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'STOE-IPDS Program Package'
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0452P)²+3.0716P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(19)
_refine_ls_number_reflns         11411
_refine_ls_number_parameters     503
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0768
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb1 Sb 0.99931(2) 0.405869(14) 0.16513(3) 0.02989(7) Uani 1 1 d . . .
Sb2 Sb 1.11668(2) 0.297537(14) 0.38426(3) 0.02994(7) Uani 1 1 d . . .
Sb3 Sb 0.91084(3) 0.654938(16) 0.51669(4) 0.04313(9) Uani 1 1 d . . .
V1 V 0.87509(5) 0.33244(3) 0.25883(7) 0.02494(15) Uani 1 1 d . . .
V2 V 1.0000 0.28374(4) 0.5000 0.0229(2) Uani 1 2 d S . .
V3 V 0.78147(5) 0.36902(3) 0.35552(7) 0.02503(15) Uani 1 1 d . . .
V4 V 0.80293(5) 0.44992(4) 0.53945(7) 0.02835(16) Uani 1 1 d . . .
V5 V 0.95052(6) 0.53763(4) 0.68882(8) 0.03029(17) Uani 1 1 d . . .
V6 V 0.77671(6) 0.53261(4) 0.36836(8) 0.03101(18) Uani 1 1 d . . .
V7 V 0.87356(6) 0.57778(4) 0.26719(8) 0.03359(18) Uani 1 1 d . . .
V8 V 0.82685(5) 0.46013(4) 0.17900(7) 0.02716(16) Uani 1 1 d . . .
O1 O 1.0718(2) 0.33476(16) 0.2390(3) 0.0328(7) Uani 1 1 d . . .
O2 O 0.9121(2) 0.39603(14) 0.2012(3) 0.0296(7) Uani 1 1 d . . .
O3 O 1.0811(2) 0.45512(16) 0.3067(3) 0.0308(7) Uani 1 1 d . . .
O4 O 1.0029(2) 0.30706(16) 0.3695(3) 0.0300(7) Uani 1 1 d . . .
O5 O 1.1707(2) 0.36807(15) 0.4783(3) 0.0304(7) Uani 1 1 d . . .
O6 O 0.7977(2) 0.39575(15) 0.2399(3) 0.0281(7) Uani 1 1 d . . .
O7 O 0.8194(2) 0.28403(16) 0.1583(3) 0.0350(8) Uani 1 1 d . . .
O8 O 0.8767(2) 0.31244(14) 0.3922(3) 0.0255(6) Uani 1 1 d . . .
O9 O 1.0000 0.2125(2) 0.5000 0.0333(10) Uani 1 2 d S . .
O10 O 0.7627(2) 0.44936(16) 0.3830(3) 0.0305(7) Uani 1 1 d . . .
O11 O 0.6856(2) 0.33406(17) 0.2885(3) 0.0340(8) Uani 1 1 d . . .
O12 O 0.8388(2) 0.53020(15) 0.5355(3) 0.0316(7) Uani 1 1 d . . .
O13 O 0.7175(3) 0.44970(19) 0.5478(4) 0.0429(9) Uani 1 1 d . . .
O14 O 0.9954(3) 0.59685(16) 0.6322(4) 0.0385(8) Uani 1 1 d . . .
O15 O 0.9235(2) 0.51621(16) 0.2244(3) 0.0331(7) Uani 1 1 d . . .
O16 O 0.9320(3) 0.57560(18) 0.7686(3) 0.0402(8) Uani 1 1 d . . .
O17 O 0.8605(3) 0.59796(17) 0.3911(4) 0.0386(8) Uani 1 1 d . . .
O18 O 0.7962(2) 0.51562(15) 0.2540(3) 0.0310(7) Uani 1 1 d . . .
O19 O 0.6776(3) 0.56285(19) 0.3064(4) 0.0456(10) Uani 1 1 d . . .
O20 O 0.8205(3) 0.62723(19) 0.1662(4) 0.0500(10) Uani 1 1 d . . .
O21 O 0.7495(2) 0.46589(18) 0.0434(3) 0.0392(9) Uani 1 1 d . . .
O22 O 1.0000 0.6898(3) 0.5000 0.0548(16) Uani 1 2 d S . .
Fe1 Fe 0.71565(5) 0.61155(4) 0.77546(7) 0.03925(18) Uani 1 1 d . . .
N1 N 0.7136(3) 0.5166(2) 0.8172(5) 0.0456(11) Uani 1 1 d . . .
H1N H 0.7001 0.5135 0.8694 0.055 Uiso 1 1 calc R . .
H2N H 0.6703 0.4962 0.7515 0.055 Uiso 1 1 calc R . .
C1 C 0.8029(5) 0.4927(3) 0.8655(6) 0.0525(16) Uani 1 1 d . . .
H1A H 0.8116 0.4875 0.8042 0.063 Uiso 1 1 calc R . .
H1B H 0.8096 0.4537 0.9011 0.063 Uiso 1 1 calc R . .
C2 C 0.8722(4) 0.5353(3) 0.9552(6) 0.0497(15) Uani 1 1 d . . .
H2A H 0.8647 0.5390 1.0178 0.060 Uiso 1 1 calc R . .
H2B H 0.9342 0.5201 0.9891 0.060 Uiso 1 1 calc R . .
N2 N 0.8612(3) 0.5935(2) 0.9033(4) 0.0396(10) Uani 1 1 d . . .
H3N H 0.8902 0.5940 0.8682 0.047 Uiso 1 1 calc R . .
H4N H 0.8868 0.6222 0.9596 0.047 Uiso 1 1 calc R . .
N11 N 0.7054(4) 0.6529(3) 0.9069(5) 0.0550(13) Uani 1 1 d . . .
H5N H 0.7481 0.6368 0.9784 0.066 Uiso 1 1 calc R . .
H6N H 0.7159 0.6929 0.9104 0.066 Uiso 1 1 calc R . .
C11 C 0.6167(6) 0.6423(4) 0.8751(8) 0.072(2) Uani 1 1 d . . .
H11A H 0.6058 0.6672 0.9225 0.087 Uiso 1 1 calc R . .
H11B H 0.6111 0.6004 0.8898 0.087 Uiso 1 1 calc R . .
C12 C 0.5500(5) 0.6556(4) 0.7550(8) 0.068(2) Uani 1 1 d . . .
H12A H 0.5524 0.6983 0.7420 0.082 Uiso 1 1 calc R . .
H12B H 0.4885 0.6466 0.7334 0.082 Uiso 1 1 calc R . .
N12 N 0.5663(4) 0.6196(3) 0.6771(5) 0.0587(15) Uani 1 1 d . . .
H7N H 0.5421 0.6389 0.6084 0.070 Uiso 1 1 calc R . .
H8N H 0.5398 0.5828 0.6618 0.070 Uiso 1 1 calc R . .
N21 N 0.7089(3) 0.5873(2) 0.6198(4) 0.0434(11) Uani 1 1 d . . .
H9N H 0.7600 0.5662 0.6416 0.052 Uiso 1 1 calc R . .
H10N H 0.6587 0.5639 0.5715 0.052 Uiso 1 1 calc R . .
C21 C 0.7030(4) 0.6411(3) 0.5593(5) 0.0434(13) Uani 1 1 d . . .
H21A H 0.6401 0.6569 0.5140 0.052 Uiso 1 1 calc R . .
H21B H 0.7187 0.6323 0.5054 0.052 Uiso 1 1 calc R . .
C22 C 0.7687(4) 0.6863(2) 0.6478(5) 0.0400(12) Uani 1 1 d . . .
H22A H 0.8319 0.6713 0.6900 0.048 Uiso 1 1 calc R . .
H22B H 0.7644 0.7235 0.6087 0.048 Uiso 1 1 calc R . .
N22 N 0.7460(4) 0.6974(2) 0.7297(5) 0.0444(11) Uani 1 1 d . . .
H11N H 0.6961 0.7220 0.6964 0.053 Uiso 1 1 calc R . .
H12N H 0.7941 0.7156 0.7951 0.053 Uiso 1 1 calc R . .
Fe2 Fe 0.5000 0.43029(6) 0.0000 0.0408(3) Uani 1 2 d S . .
N31 N 0.4723(3) 0.4237(3) -0.1715(4) 0.0486(12) Uani 1 1 d . . .
H13N H 0.4209 0.4013 -0.2198 0.058 Uiso 1 1 calc R . .
H14N H 0.4622 0.4608 -0.2032 0.058 Uiso 1 1 calc R . .
C31 C 0.5503(5) 0.3964(4) -0.1597(6) 0.067(2) Uani 1 1 d . . .
H31A H 0.6006 0.4253 -0.1279 0.081 Uiso 1 1 calc R . .
H31B H 0.5328 0.3832 -0.2360 0.081 Uiso 1 1 calc R . .
C32 C 0.5807(6) 0.3440(4) -0.0793(7) 0.069(2) Uani 1 1 d . . .
H32A H 0.5324 0.3135 -0.1152 0.083 Uiso 1 1 calc R . .
H32B H 0.6362 0.3265 -0.0656 0.083 Uiso 1 1 calc R . .
N32 N 0.6000(3) 0.3628(3) 0.0315(5) 0.0492(12) Uani 1 1 d . . .
H15N H 0.6579 0.3781 0.0783 0.059 Uiso 1 1 calc R . .
H16N H 0.5968 0.3307 0.0683 0.059 Uiso 1 1 calc R . .
N41 N 0.4079(3) 0.5067(3) -0.0483(5) 0.0526(14) Uani 1 1 d . . .
H17N H 0.3686 0.5097 -0.1274 0.063 Uiso 1 1 calc R . .
H18N H 0.3739 0.5013 -0.0206 0.063 Uiso 1 1 calc R . .
C41 C 0.4623(6) 0.5617(4) 0.0007(11) 0.091(3) Uani 1 1 d . . .
H41A H 0.4233 0.5960 -0.0440 0.110 Uiso 1 1 calc R . .
H41B H 0.4827 0.5663 0.0813 0.110 Uiso 1 1 calc R . .
O31 O 0.5567(4) 0.5208(3) 0.3505(6) 0.0836(18) Uani 1 1 d . . .
O32 O 1.0419(5) 0.6764(3) 0.8746(6) 0.0874(19) Uani 1 1 d . . .
O33 O 0.8887(5) 0.3170(3) 0.0183(5) 0.0798(17) Uani 1 1 d . . .
O34 O 0.8689(6) 0.1852(4) -0.2236(8) 0.119(3) Uani 1 1 d . . .
O35 O 1.0000 0.2295(4) 0.0000 0.119(4) Uani 1 2 d S . .


_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 O1 1.950(4) . ?
Sb1 O2 1.952(3) . ?
Sb1 O3 2.005(3) . ?
Sb2 O1 1.928(4) . ?
Sb2 O5 1.941(3) . ?
Sb2 O4 1.964(3) . ?
Sb3 O22 1.942(3) . ?
Sb3 O17 1.950(4) . ?
Sb3 O14 1.958(4) . ?
V1 O7 1.607(3) . ?
V1 O6 1.913(3) . ?
V1 O8 1.951(3) . ?
V1 O2 1.966(3) . ?
V1 O4 1.975(3) . ?
V1 V3 2.8828(11) . ?
V1 V2 3.0131(8) . ?
V1 V8 3.0404(11) . ?
V2 O9 1.612(5) . ?
V2 O8 1.937(3) 2_756 ?
V2 O8 1.937(3) . ?
V2 O4 1.978(3) 2_756 ?
V2 O4 1.978(3) . ?
V2 V1 3.0131(8) 2_756 ?
V3 O11 1.616(3) . ?
V3 O10 1.933(4) . ?
V3 O6 1.946(3) . ?
V3 O8 1.960(3) . ?
V3 O5 2.001(4) 2_756 ?
V3 V4 3.0433(12) . ?
V4 O13 1.628(4) . ?
V4 O10 1.907(4) . ?
V4 O12 1.942(4) . ?
V4 O3 1.960(3) 2_756 ?
V4 O5 1.967(4) 2_756 ?
V4 V6 2.8949(12) . ?
V4 V5 2.9916(12) . ?
V5 O16 1.618(4) . ?
V5 O15 1.916(4) 2_756 ?
V5 O12 1.930(4) . ?
V5 O3 1.966(4) 2_756 ?
V5 O14 1.977(4) . ?
V5 V7 3.0143(11) 2_756 ?
V6 O19 1.619(4) . ?
V6 O18 1.914(4) . ?
V6 O10 1.929(4) . ?
V6 O12 1.959(4) . ?
V6 O17 2.007(4) . ?
V6 V7 3.0475(12) . ?
V7 O20 1.622(4) . ?
V7 O18 1.918(4) . ?
V7 O15 1.950(4) . ?
V7 O14 1.972(4) 2_756 ?
V7 O17 1.982(4) . ?
V7 V8 2.8533(12) . ?
V7 V5 3.0143(11) 2_756 ?
V8 O21 1.598(4) . ?
V8 O6 1.929(3) . ?
V8 O18 1.938(4) . ?
V8 O15 1.942(4) . ?
V8 O2 2.007(3) . ?
O3 V4 1.960(3) 2_756 ?
O3 V5 1.966(4) 2_756 ?
O5 V4 1.967(4) 2_756 ?
O5 V3 2.001(4) 2_756 ?
O14 V7 1.972(4) 2_756 ?
O15 V5 1.916(4) 2_756 ?
O22 Sb3 1.942(3) 2_756 ?
Fe1 N2 2.193(5) . ?
Fe1 N12 2.210(5) . ?
Fe1 N11 2.211(5) . ?
Fe1 N22 2.223(5) . ?
Fe1 N21 2.234(5) . ?
Fe1 N1 2.237(5) . ?
N1 C1 1.442(8) . ?
C1 C2 1.504(10) . ?
C2 N2 1.467(7) . ?
N11 C11 1.415(10) . ?
C11 C12 1.438(13) . ?
C12 N12 1.547(10) . ?
N21 C21 1.463(8) . ?
C21 C22 1.515(9) . ?
C22 N22 1.483(7) . ?
Fe2 N31 2.208(5) . ?
Fe2 N31 2.208(5) 2_655 ?
Fe2 N32 2.210(5) 2_655 ?
Fe2 N32 2.210(5) . ?
Fe2 N41 2.215(5) 2_655 ?
Fe2 N41 2.215(5) . ?
N31 C31 1.464(10) . ?
C31 C32 1.512(13) . ?
C32 N32 1.474(10) . ?
N41 C41 1.483(11) . ?
C41 C41 1.385(18) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Sb1 O2 99.02(14) . . ?
O1 Sb1 O3 92.75(14) . . ?
O2 Sb1 O3 91.60(14) . . ?
O1 Sb2 O5 96.33(15) . . ?
O1 Sb2 O4 95.12(14) . . ?
O5 Sb2 O4 93.07(14) . . ?
O22 Sb3 O17 97.19(16) . . ?
O22 Sb3 O14 94.66(16) . . ?
O17 Sb3 O14 92.57(16) . . ?
O7 V1 O6 111.22(16) . . ?
O7 V1 O8 111.07(17) . . ?
O6 V1 O8 84.01(14) . . ?
O7 V1 O2 108.14(17) . . ?
O6 V1 O2 78.40(14) . . ?
O8 V1 O2 140.59(14) . . ?
O7 V1 O4 110.05(17) . . ?
O6 V1 O4 138.66(15) . . ?
O8 V1 O4 79.35(13) . . ?
O2 V1 O4 91.04(14) . . ?
O7 V1 V3 112.94(14) . . ?
O6 V1 V3 42.10(10) . . ?
O8 V1 V3 42.63(9) . . ?
O2 V1 V3 116.06(10) . . ?
O4 V1 V3 116.51(11) . . ?
O7 V1 V2 115.52(14) . . ?
O6 V1 V2 115.43(10) . . ?
O8 V1 V2 39.03(9) . . ?
O2 V1 V2 122.56(10) . . ?
O4 V1 V2 40.37(10) . . ?
V3 V1 V2 79.08(3) . . ?
O7 V1 V8 114.86(14) . . ?
O6 V1 V8 37.86(10) . . ?
O8 V1 V8 115.09(10) . . ?
O2 V1 V8 40.56(9) . . ?
O4 V1 V8 121.35(11) . . ?
V3 V1 V8 77.74(3) . . ?
V2 V1 V8 129.40(4) . . ?
O9 V2 O8 109.59(10) . 2_756 ?
O9 V2 O8 109.59(10) . . ?
O8 V2 O8 140.83(19) 2_756 . ?
O9 V2 O4 105.47(11) . 2_756 ?
O8 V2 O4 79.63(13) 2_756 2_756 ?
O8 V2 O4 90.07(13) . 2_756 ?
O9 V2 O4 105.47(11) . . ?
O8 V2 O4 90.07(13) 2_756 . ?
O8 V2 O4 79.63(13) . . ?
O4 V2 O4 149.1(2) 2_756 . ?
O9 V2 V1 111.45(2) . 2_756 ?
O8 V2 V1 39.38(10) 2_756 2_756 ?
O8 V2 V1 121.86(10) . 2_756 ?
O4 V2 V1 40.30(9) 2_756 2_756 ?
O4 V2 V1 124.58(10) . 2_756 ?
O9 V2 V1 111.45(2) . . ?
O8 V2 V1 121.86(10) 2_756 . ?
O8 V2 V1 39.38(10) . . ?
O4 V2 V1 124.58(10) 2_756 . ?
O4 V2 V1 40.30(9) . . ?
V1 V2 V1 137.10(5) 2_756 . ?
O11 V3 O10 108.83(17) . . ?
O11 V3 O6 107.34(17) . . ?
O10 V3 O6 90.95(14) . . ?
O11 V3 O8 108.20(16) . . ?
O10 V3 O8 142.61(14) . . ?
O6 V3 O8 82.93(14) . . ?
O11 V3 O5 105.16(17) . 2_756 ?
O10 V3 O5 76.76(14) . 2_756 ?
O6 V3 O5 147.45(14) . 2_756 ?
O8 V3 O5 88.84(14) . 2_756 ?
O11 V3 V1 108.04(14) . . ?
O10 V3 V1 126.50(11) . . ?
O6 V3 V1 41.23(10) . . ?
O8 V3 V1 42.41(10) . . ?
O5 V3 V1 127.39(10) 2_756 . ?
O11 V3 V4 110.58(14) . . ?
O10 V3 V4 37.30(10) . . ?
O6 V3 V4 123.17(10) . . ?
O8 V3 V4 121.31(10) . . ?
O5 V3 V4 39.50(10) 2_756 . ?
V1 V3 V4 141.38(3) . . ?
O13 V4 O10 111.55(18) . . ?
O13 V4 O12 110.89(19) . . ?
O10 V4 O12 82.77(16) . . ?
O13 V4 O3 110.86(18) . 2_756 ?
O10 V4 O3 137.48(14) . 2_756 ?
O12 V4 O3 79.64(15) . 2_756 ?
O13 V4 O5 108.85(19) . 2_756 ?
O10 V4 O5 78.17(15) . 2_756 ?
O12 V4 O5 139.92(14) . 2_756 ?
O3 V4 O5 91.13(15) 2_756 2_756 ?
O13 V4 V6 112.25(15) . . ?
O10 V4 V6 41.29(11) . . ?
O12 V4 V6 42.33(11) . . ?
O3 V4 V6 116.50(11) 2_756 . ?
O5 V4 V6 115.42(11) 2_756 . ?
O13 V4 V5 116.17(16) . . ?
O10 V4 V5 114.00(11) . . ?
O12 V4 V5 39.26(11) . . ?
O3 V4 V5 40.43(11) 2_756 . ?
O5 V4 V5 122.21(10) 2_756 . ?
V6 V4 V5 78.94(3) . . ?
O13 V4 V3 115.05(16) . . ?
O10 V4 V3 37.89(11) . . ?
O12 V4 V3 114.24(11) . . ?
O3 V4 V3 121.02(11) 2_756 . ?
O5 V4 V3 40.32(10) 2_756 . ?
V6 V4 V3 77.27(3) . . ?
V5 V4 V3 128.47(3) . . ?
O16 V5 O15 110.10(18) . 2_756 ?
O16 V5 O12 109.51(18) . . ?
O15 V5 O12 140.36(15) 2_756 . ?
O16 V5 O3 107.08(18) . 2_756 ?
O15 V5 O3 90.00(15) 2_756 2_756 ?
O12 V5 O3 79.78(14) . 2_756 ?
O16 V5 O14 103.93(19) . . ?
O15 V5 O14 79.16(17) 2_756 . ?
O12 V5 O14 90.16(16) . . ?
O3 V5 O14 148.99(16) 2_756 . ?
O16 V5 V4 112.69(15) . . ?
O15 V5 V4 121.43(11) 2_756 . ?
O12 V5 V4 39.55(10) . . ?
O3 V5 V4 40.27(10) 2_756 . ?
O14 V5 V4 124.66(13) . . ?
O16 V5 V7 109.32(15) . 2_756 ?
O15 V5 V7 39.16(11) 2_756 2_756 ?
O12 V5 V7 122.60(11) . 2_756 ?
O3 V5 V7 125.08(10) 2_756 2_756 ?
O14 V5 V7 40.19(12) . 2_756 ?
V4 V5 V7 137.98(4) . 2_756 ?
O19 V6 O18 108.95(19) . . ?
O19 V6 O10 107.23(18) . . ?
O18 V6 O10 90.09(15) . . ?
O19 V6 O12 109.53(19) . . ?
O18 V6 O12 141.38(15) . . ?
O10 V6 O12 81.76(15) . . ?
O19 V6 O17 105.73(19) . . ?
O18 V6 O17 77.24(16) . . ?
O10 V6 O17 146.97(15) . . ?
O12 V6 O17 89.34(16) . . ?
O19 V6 V4 108.15(15) . . ?
O18 V6 V4 125.29(11) . . ?
O10 V6 V4 40.73(10) . . ?
O12 V6 V4 41.87(10) . . ?
O17 V6 V4 127.54(12) . . ?
O19 V6 V7 111.52(15) . . ?
O18 V6 V7 37.36(11) . . ?
O10 V6 V7 122.07(11) . . ?
O12 V6 V7 121.08(11) . . ?
O17 V6 V7 39.90(12) . . ?
V4 V6 V7 140.31(4) . . ?
O20 V7 O18 113.7(2) . . ?
O20 V7 O15 110.7(2) . . ?
O18 V7 O15 84.02(15) . . ?
O20 V7 O14 109.1(2) . 2_756 ?
O18 V7 O14 137.03(16) . 2_756 ?
O15 V7 O14 78.50(15) . 2_756 ?
O20 V7 O17 108.6(2) . . ?
O18 V7 O17 77.75(16) . . ?
O15 V7 O17 140.56(16) . . ?
O14 V7 O17 91.48(17) 2_756 . ?
O20 V7 V8 112.49(18) . . ?
O18 V7 V8 42.53(11) . . ?
O15 V7 V8 42.75(11) . . ?
O14 V7 V8 116.34(11) 2_756 . ?
O17 V7 V8 116.80(12) . . ?
O20 V7 V5 113.14(17) . 2_756 ?
O18 V7 V5 115.22(11) . 2_756 ?
O15 V7 V5 38.37(11) . 2_756 ?
O14 V7 V5 40.32(11) 2_756 2_756 ?
O17 V7 V5 123.84(12) . 2_756 ?
V8 V7 V5 79.23(3) . 2_756 ?
O20 V7 V6 116.79(17) . . ?
O18 V7 V6 37.27(11) . . ?
O15 V7 V6 114.75(11) . . ?
O14 V7 V6 120.88(13) 2_756 . ?
O17 V7 V6 40.50(11) . . ?
V8 V7 V6 78.12(3) . . ?
V5 V7 V6 129.85(4) 2_756 . ?
O21 V8 O6 109.54(18) . . ?
O21 V8 O18 106.82(18) . . ?
O6 V8 O18 89.47(14) . . ?
O21 V8 O15 109.09(18) . . ?
O6 V8 O15 141.11(15) . . ?
O18 V8 O15 83.70(15) . . ?
O21 V8 O2 107.09(18) . . ?
O6 V8 O2 77.07(13) . . ?
O18 V8 O2 146.01(15) . . ?
O15 V8 O2 87.56(14) . . ?
O21 V8 V7 106.38(16) . . ?
O6 V8 V7 126.37(11) . . ?
O18 V8 V7 42.00(11) . . ?
O15 V8 V7 42.95(11) . . ?
O2 V8 V7 127.17(10) . . ?
O21 V8 V1 112.79(16) . . ?
O6 V8 V1 37.50(9) . . ?
O18 V8 V1 121.33(11) . . ?
O15 V8 V1 119.44(11) . . ?
O2 V8 V1 39.59(9) . . ?
V7 V8 V1 140.82(4) . . ?
Sb2 O1 Sb1 131.86(19) . . ?
Sb1 O2 V1 136.84(17) . . ?
Sb1 O2 V8 123.30(17) . . ?
V1 O2 V8 99.85(14) . . ?
V4 O3 V5 99.29(16) 2_756 2_756 ?
V4 O3 Sb1 140.40(19) 2_756 . ?
V5 O3 Sb1 120.29(16) 2_756 . ?
Sb2 O4 V1 141.66(18) . . ?
Sb2 O4 V2 118.99(15) . . ?
V1 O4 V2 99.32(15) . . ?
Sb2 O5 V4 138.26(19) . 2_756 ?
Sb2 O5 V3 121.56(18) . 2_756 ?
V4 O5 V3 100.18(16) 2_756 2_756 ?
V1 O6 V8 104.64(15) . . ?
V1 O6 V3 96.67(15) . . ?
V8 O6 V3 147.46(19) . . ?
V2 O8 V1 101.59(14) . . ?
V2 O8 V3 148.98(18) . . ?
V1 O8 V3 94.96(14) . . ?
V4 O10 V6 97.97(17) . . ?
V4 O10 V3 104.81(16) . . ?
V6 O10 V3 147.65(19) . . ?
V5 O12 V4 101.19(16) . . ?
V5 O12 V6 148.4(2) . . ?
V4 O12 V6 95.81(16) . . ?
Sb3 O14 V7 140.6(2) . 2_756 ?
Sb3 O14 V5 119.6(2) . . ?
V7 O14 V5 99.49(18) 2_756 . ?
V5 O15 V8 151.9(2) 2_756 . ?
V5 O15 V7 102.47(18) 2_756 . ?
V8 O15 V7 94.30(15) . . ?
Sb3 O17 V7 137.9(2) . . ?
Sb3 O17 V6 122.29(19) . . ?
V7 O17 V6 99.60(18) . . ?
V6 O18 V7 105.37(18) . . ?
V6 O18 V8 150.1(2) . . ?
V7 O18 V8 95.47(15) . . ?
Sb3 O22 Sb3 132.0(3) . 2_756 ?
N2 Fe1 N12 166.43(19) . . ?
N2 Fe1 N11 91.9(2) . . ?
N12 Fe1 N11 79.6(2) . . ?
N2 Fe1 N22 91.29(19) . . ?
N12 Fe1 N22 99.5(2) . . ?
N11 Fe1 N22 92.5(2) . . ?
N2 Fe1 N21 96.74(18) . . ?
N12 Fe1 N21 93.5(2) . . ?
N11 Fe1 N21 167.40(19) . . ?
N22 Fe1 N21 78.23(18) . . ?
N2 Fe1 N1 78.44(18) . . ?
N12 Fe1 N1 92.4(2) . . ?
N11 Fe1 N1 98.9(2) . . ?
N22 Fe1 N1 164.87(19) . . ?
N21 Fe1 N1 91.8(2) . . ?
C1 N1 Fe1 107.2(4) . . ?
N1 C1 C2 108.0(5) . . ?
N2 C2 C1 110.2(5) . . ?
C2 N2 Fe1 109.1(4) . . ?
C11 N11 Fe1 107.9(5) . . ?
N11 C11 C12 110.3(7) . . ?
C11 C12 N12 111.8(6) . . ?
C12 N12 Fe1 105.7(4) . . ?
C21 N21 Fe1 109.3(4) . . ?
N21 C21 C22 108.6(5) . . ?
N22 C22 C21 109.1(5) . . ?
C22 N22 Fe1 108.7(3) . . ?
N31 Fe2 N31 172.3(3) . 2_655 ?
N31 Fe2 N32 96.2(2) . 2_655 ?
N31 Fe2 N32 78.4(2) 2_655 2_655 ?
N31 Fe2 N32 78.4(2) . . ?
N31 Fe2 N32 96.2(2) 2_655 . ?
N32 Fe2 N32 92.5(3) 2_655 . ?
N31 Fe2 N41 91.9(2) . 2_655 ?
N31 Fe2 N41 94.1(2) 2_655 2_655 ?
N32 Fe2 N41 169.6(2) 2_655 2_655 ?
N32 Fe2 N41 95.5(2) . 2_655 ?
N31 Fe2 N41 94.1(2) . . ?
N31 Fe2 N41 91.9(2) 2_655 . ?
N32 Fe2 N41 95.5(2) 2_655 . ?
N32 Fe2 N41 169.6(2) . . ?
N41 Fe2 N41 77.4(3) 2_655 . ?
C31 N31 Fe2 109.4(4) . . ?
N31 C31 C32 108.2(6) . . ?
N32 C32 C31 110.2(7) . . ?
C32 N32 Fe2 109.6(5) . . ?
C41 N41 Fe2 109.6(4) . . ?
C41 C41 N41 112.5(8) 2_655 . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.94
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.169
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.109
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.741 0.000 6.9 6.7
2 0.500 0.241 0.000 6.9 6.7
3 0.500 0.328 0.500 312.7 81.4
4 1.000 0.828 0.500 312.7 81.4
5 0.000 0.455 0.500 21.8 8.8
6 0.500 0.955 0.500 21.8 8.8
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_mh1117
_database_code_depnum_ccdc_archive 'CCDC 1432850'
_audit_update_record             
;
2015-10-23 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 '[Ni(C2H8N2)3]3{V15Sb6O42}*xH2O' 
;
_chemical_name_common            '[Ni(ethylendiamine)3]3{V15Sb6O42}*xH2O'
_chemical_melting_point          ?
_chemical_formula_moiety         'V15Sb6O42, NiC6H24N6, C2H8N2, H2O'
_chemical_formula_sum            'C18 H72 N18 Ni3 O42 Sb6 V15'
_chemical_formula_weight         2883.66

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'
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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_H-M_alt        'P 3 2 1'
_space_group_name_Hall           'P 3 2"'

_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'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -z'

_cell_length_a                   23.7437(5)
_cell_length_b                   23.7437(5)
_cell_length_c                   14.9586(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     7303.3(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    38040
_cell_measurement_theta_min      1.361
_cell_measurement_theta_max      25.002

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_F_000             4131
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    3.631
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5900
_exptl_absorpt_correction_T_max  0.6543
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 2013)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            38040
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.361
_diffrn_reflns_theta_max         25.002
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             8614
_reflns_number_gt                7047
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    0.973

_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       'STOE-IPDS Program Package'
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component 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)+(0.0896P)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 
;
 Flack x determined using 2597 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.028(19)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8614
_refine_ls_number_parameters     463
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0580
_refine_ls_wR_factor_ref         0.1438
_refine_ls_wR_factor_gt          0.1369
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_restrained_S_all      0.987
_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 0.77388(5) 0.93029(6) 0.93085(8) 0.0500(3) Uani 1 1 d . . . . .
V1 V 0.84358(14) 0.92426(14) 1.15092(18) 0.0462(6) Uani 1 1 d . . . . .
V2 V 0.83775(17) 0.83775(17) 1.0000 0.0462(9) Uani 1 2 d S T P . .
V3 V 0.89599(14) 0.94162(14) 0.79469(18) 0.0452(6) Uani 1 1 d . . . . .
O1 O 0.7766(7) 1.0000 1.0000 0.055(4) Uani 1 2 d S T P . .
O2 O 0.8150(6) 0.9045(6) 1.0244(8) 0.054(3) Uani 1 1 d . . . . .
O3 O 0.8539(6) 0.9830(6) 0.8686(7) 0.052(3) Uani 1 1 d . . . . .
O4 O 0.7818(6) 0.8936(6) 1.2172(9) 0.061(3) Uani 1 1 d . . . . .
O5 O 0.7677(7) 0.7677(7) 1.0000 0.060(5) Uani 1 2 d S T P . .
O6 O 0.8620(6) 0.8709(6) 0.8822(8) 0.055(3) Uani 1 1 d . . . . .
O7 O 0.8546(7) 0.9171(7) 0.7036(8) 0.063(3) Uani 1 1 d . . . . .
O8 O 0.9580(6) 1.0331(6) 0.7864(8) 0.057(3) Uani 1 1 d . . . . .
Sb11 Sb 0.47573(6) 0.89612(6) 0.53629(8) 0.0553(3) Uani 1 1 d . . . . .
Sb12 Sb 0.55542(6) 0.83672(6) 0.67489(8) 0.0587(3) Uani 1 1 d . . . . .
V11 V 0.48894(14) 0.75789(15) 0.45487(19) 0.0508(7) Uani 1 1 d . . . . .
V12 V 0.37119(14) 0.76938(14) 0.39847(18) 0.0472(6) Uani 1 1 d . . . . .
V13 V 0.31808(16) 0.82034(14) 0.6050(2) 0.0513(7) Uani 1 1 d . . . . .
V14 V 0.40256(16) 0.82300(15) 0.7561(2) 0.0547(7) Uani 1 1 d . . . . .
V15 V 0.43743(15) 0.72074(15) 0.81116(18) 0.0509(7) Uani 1 1 d . . . . .
O11 O 0.5465(7) 0.9015(7) 0.6039(9) 0.068(4) Uani 1 1 d . . . . .
O12 O 0.4530(6) 0.8166(6) 0.4716(9) 0.060(3) Uani 1 1 d . . . . .
O13 O 0.4094(6) 0.8514(7) 0.6292(7) 0.058(3) Uani 1 1 d . . . . .
O14 O 0.5174(6) 0.7693(6) 0.5803(8) 0.055(3) Uani 1 1 d . . . . .
O15 O 0.4737(6) 0.8019(6) 0.7386(8) 0.056(3) Uani 1 1 d . . . . .
O16 O 0.5507(6) 0.7902(7) 0.3891(9) 0.071(4) Uani 1 1 d . . . . .
O17 O 0.3823(6) 0.8077(6) 0.3061(8) 0.054(3) Uani 1 1 d . . . . .
O18 O 0.2853(6) 0.6951(6) 0.3901(8) 0.053(3) Uani 1 1 d . . . . .
O19 O 0.3291(5) 0.7972(5) 0.4836(7) 0.045(2) Uani 1 1 d . . . . .
O20 O 0.3097(8) 0.8834(6) 0.6052(9) 0.068(4) Uani 1 1 d . . . . .
O21 O 0.4270(7) 0.8855(7) 0.8219(9) 0.065(4) Uani 1 1 d . . . . .
O22 O 0.4798(6) 0.7409(6) 0.9050(7) 0.057(3) Uani 1 1 d . . . . .
O23 O 0.3732(6) 0.6281(6) 0.8194(7) 0.050(3) Uani 1 1 d . . . . .
O24 O 0.4767(5) 0.6859(6) 0.7282(8) 0.054(3) Uani 1 1 d . . . . .
Ni1 Ni 0.6667 0.3333 0.8948(2) 0.0523(9) Uani 1 3 d DS T P . .
N1 N 0.7518(8) 0.3733(7) 0.9734(11) 0.061(4) Uani 1 1 d D . . . .
H1N1 H 0.7452 0.3918 1.0291 0.073 Uiso 1 1 calc R U . . .
H2N1 H 0.7618 0.3389 0.9899 0.073 Uiso 1 1 calc R U . . .
C1 C 0.8071(10) 0.4254(10) 0.9212(13) 0.066(5) Uani 1 1 d D . . . .
H1A H 0.8433 0.4540 0.9616 0.079 Uiso 1 1 calc R U . . .
H1B H 0.8235 0.4060 0.8770 0.079 Uiso 1 1 calc R U . . .
N2 N 0.5808(8) 0.3028(10) 0.8189(10) 0.072(5) Uani 1 1 d . . . . .
H1N2 H 0.5911 0.3265 0.7614 0.087 Uiso 1 1 calc R U . . .
H2N2 H 0.5596 0.2556 0.8062 0.087 Uiso 1 1 calc R U . . .
C2 C 0.5367(11) 0.3177(11) 0.8749(13) 0.069(5) Uani 1 1 d . . . . .
H2A H 0.5033 0.3185 0.8360 0.082 Uiso 1 1 calc R U . . .
H2B H 0.5140 0.2829 0.9199 0.082 Uiso 1 1 calc R U . . .
Ni11 Ni 0.69167(12) 0.65250(13) 0.76762(16) 0.0613(6) Uani 1 1 d . . . . .
N3 N 0.6692(9) 0.6460(8) 0.6302(9) 0.065(4) Uani 1 1 d . . . . .
H1N3 H 0.6439 0.6679 0.6180 0.078 Uiso 1 1 calc R U . . .
H2N3 H 0.7098 0.6679 0.5947 0.078 Uiso 1 1 calc R U . . .
C3 C 0.6314(13) 0.5777(12) 0.6044(12) 0.079(7) Uani 1 1 d . . . . .
H3A H 0.6604 0.5594 0.5959 0.094 Uiso 1 1 calc R U . . .
H3B H 0.6081 0.5732 0.5476 0.094 Uiso 1 1 calc R U . . .
C4 C 0.5823(14) 0.5416(12) 0.6808(16) 0.088(8) Uani 1 1 d . . . . .
H4A H 0.5521 0.5587 0.6874 0.105 Uiso 1 1 calc R U . . .
H4B H 0.5564 0.4945 0.6672 0.105 Uiso 1 1 calc R U . . .
N4 N 0.6202(11) 0.5522(9) 0.7657(14) 0.083(6) Uani 1 1 d . . . . .
H1N4 H 0.6410 0.5250 0.7663 0.100 Uiso 1 1 calc R U . . .
H2N4 H 0.5912 0.5408 0.8184 0.100 Uiso 1 1 calc R U . . .
N5 N 0.7733(9) 0.6413(9) 0.7414(12) 0.068(4) Uani 1 1 d . . . . .
H1N5 H 0.7650 0.6127 0.6890 0.081 Uiso 1 1 calc R U . . .
H2N5 H 0.8124 0.6840 0.7293 0.081 Uiso 1 1 calc R U . . .
C5 C 0.7827(16) 0.6112(13) 0.8239(19) 0.097(8) Uani 1 1 d . . . . .
H5A H 0.8251 0.6128 0.8216 0.116 Uiso 1 1 calc R U . . .
H5B H 0.7479 0.5651 0.8285 0.116 Uiso 1 1 calc R U . . .
C6 C 0.7803(14) 0.6497(15) 0.9054(16) 0.093(8) Uani 1 1 d . . . . .
H6A H 0.7836 0.6295 0.9617 0.112 Uiso 1 1 calc R U . . .
H6B H 0.8166 0.6952 0.9032 0.112 Uiso 1 1 calc R U . . .
N6 N 0.7189(10) 0.6476(9) 0.9005(13) 0.086(6) Uani 1 1 d . . . . .
H1N6 H 0.7216 0.6844 0.9350 0.103 Uiso 1 1 calc R U . . .
H2N6 H 0.6850 0.6068 0.9283 0.103 Uiso 1 1 calc R U . . .
N7 N 0.7491(10) 0.7562(9) 0.7568(17) 0.090(6) Uani 1 1 d . . . . .
H1N7 H 0.7791 0.7746 0.8083 0.108 Uiso 1 1 calc R U . . .
H2N7 H 0.7750 0.7688 0.7011 0.108 Uiso 1 1 calc R U . . .
C7 C 0.7033(10) 0.7795(9) 0.7561(14) 0.068(5) Uani 1 1 d . . . . .
H7A H 0.7271 0.8270 0.7671 0.082 Uiso 1 1 calc R U . . .
H7B H 0.6832 0.7719 0.6961 0.082 Uiso 1 1 calc R U . . .
C8 C 0.6534(15) 0.7486(13) 0.8214(12) 0.085(8) Uani 1 1 d . . . . .
H8A H 0.6217 0.7640 0.8165 0.102 Uiso 1 1 calc R U . . .
H8B H 0.6722 0.7584 0.8823 0.102 Uiso 1 1 calc R U . . .
N8 N 0.6213(10) 0.6783(8) 0.8037(13) 0.076(5) Uani 1 1 d . . . . .
H1N8 H 0.5894 0.6668 0.7546 0.091 Uiso 1 1 calc R U . . .
H2N8 H 0.5977 0.6539 0.8578 0.091 Uiso 1 1 calc R U . . .
Ni3 Ni 1.0000 1.0000 0.5000 0.164(6) Uani 1 6 d DS T P . .
N9 N 0.948(2) 1.032(2) 0.5774(17) 0.192(18) Uani 1 1 d D . . . .
H1N9 H 0.9265 1.0023 0.6284 0.230 Uiso 1 1 calc R U . . .
H2N9 H 0.9771 1.0761 0.6012 0.230 Uiso 1 1 calc R U . . .
C9 C 0.897(2) 1.033(3) 0.519(3) 0.18(2) Uani 1 1 d D . . . .
H9A H 0.8670 1.0417 0.5539 0.221 Uiso 1 1 calc R U . . .
H9B H 0.9176 1.0666 0.4714 0.221 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 1.915(12) . ?
Sb1 O1 1.926(7) . ?
Sb1 O2 1.971(12) . ?
V1 O4 1.611(12) . ?
V1 O8 1.919(13) 6_677 ?
V1 O6 1.953(12) 4_557 ?
V1 O3 1.982(12) 6_677 ?
V1 O2 1.986(12) . ?
V1 V3 2.845(4) 4_557 ?
V1 V2 3.008(3) . ?
V1 V3 3.057(4) 6_677 ?
V2 O5 1.664(18) . ?
V2 O6 1.898(13) 4_557 ?
V2 O6 1.898(13) . ?
V2 O2 1.948(12) . ?
V2 O2 1.948(12) 4_557 ?
V2 V1 3.008(3) 4_557 ?
V3 O7 1.609(12) . ?
V3 O8 1.917(13) 2_765 ?
V3 O8 1.924(14) . ?
V3 O6 1.957(13) . ?
V3 O3 2.041(12) . ?
V3 V1 2.845(4) 4_557 ?
V3 V1 3.057(4) 6_677 ?
O1 Sb1 1.926(7) 6_677 ?
O3 V1 1.982(12) 6_677 ?
O6 V1 1.953(12) 4_557 ?
O8 V3 1.917(13) 3_675 ?
O8 V1 1.919(12) 6_677 ?
Sb11 O11 1.909(14) . ?
Sb11 O12 1.942(13) . ?
Sb11 O13 1.967(13) . ?
Sb12 O15 1.938(14) . ?
Sb12 O11 1.966(15) . ?
Sb12 O14 1.984(12) . ?
V11 O16 1.608(12) . ?
V11 O18 1.896(12) 3_565 ?
V11 O19 1.917(11) 3_565 ?
V11 O14 1.966(12) . ?
V11 O12 1.981(13) . ?
V11 V12 2.854(4) 3_565 ?
V11 V13 2.995(4) 3_565 ?
V11 V12 3.060(4) . ?
V12 O17 1.602(12) . ?
V12 O18 1.920(12) . ?
V12 O19 1.927(11) . ?
V12 O18 1.933(13) 3_565 ?
V12 O12 2.013(14) . ?
V12 V11 2.854(4) 2_665 ?
V13 O20 1.605(12) . ?
V13 O13 1.943(13) . ?
V13 O19 1.952(10) . ?
V13 O14 1.956(13) 2_665 ?
V13 O24 1.958(12) 2_665 ?
V13 V11 2.995(4) 2_665 ?
V13 V14 3.001(5) . ?
V14 O21 1.628(12) . ?
V14 O23 1.872(12) 2_665 ?
V14 O24 1.888(14) 2_665 ?
V14 O13 1.993(12) . ?
V14 O15 2.003(14) . ?
V14 V15 2.869(5) 2_665 ?
V14 V15 3.045(5) . ?
V15 O22 1.653(11) . ?
V15 O23 1.915(12) 2_665 ?
V15 O23 1.956(12) . ?
V15 O24 1.965(12) . ?
V15 O15 1.994(13) . ?
V15 V14 2.869(5) 3_565 ?
O14 V13 1.956(13) 3_565 ?
O18 V11 1.896(12) 2_665 ?
O18 V12 1.933(13) 2_665 ?
O19 V11 1.917(11) 2_665 ?
O23 V14 1.872(12) 3_565 ?
O23 V15 1.915(12) 3_565 ?
O24 V14 1.888(14) 3_565 ?
O24 V13 1.958(12) 3_565 ?
Ni1 N1 2.110(17) 3_665 ?
Ni1 N1 2.110(17) 2_655 ?
Ni1 N1 2.110(17) . ?
Ni1 N2 2.119(17) 3_665 ?
Ni1 N2 2.119(17) . ?
Ni1 N2 2.119(17) 2_655 ?
N1 C1 1.50(2) . ?
C1 C2 1.49(3) 3_665 ?
N2 C2 1.52(3) . ?
C2 C1 1.49(3) 2_655 ?
Ni11 N3 2.110(13) . ?
Ni11 N6 2.112(19) . ?
Ni11 N8 2.12(2) . ?
Ni11 N5 2.121(16) . ?
Ni11 N4 2.12(2) . ?
Ni11 N7 2.14(2) . ?
N3 C3 1.46(3) . ?
C3 C4 1.55(4) . ?
C4 N4 1.50(3) . ?
N5 C5 1.50(3) . ?
C5 C6 1.54(4) . ?
C6 N6 1.44(3) . ?
N7 C7 1.44(3) . ?
C7 C8 1.43(3) . ?
C8 N8 1.47(3) . ?
Ni3 N9 2.10(3) . ?
Ni3 N9 2.10(3) 3_675 ?
Ni3 N9 2.10(3) 6_676 ?
Ni3 N9 2.10(3) 4_556 ?
Ni3 N9 2.10(3) 5_766 ?
Ni3 N9 2.10(3) 2_765 ?
N9 C9 1.49(3) . ?
C9 C9 1.48(9) 6_676 ?

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 O1 96.0(5) . . ?
O3 Sb1 O2 93.7(5) . . ?
O1 Sb1 O2 94.4(5) . . ?
O4 V1 O8 112.8(6) . 6_677 ?
O4 V1 O6 112.7(6) . 4_557 ?
O8 V1 O6 84.0(6) 6_677 4_557 ?
O4 V1 O3 108.1(6) . 6_677 ?
O8 V1 O3 78.5(5) 6_677 6_677 ?
O6 V1 O3 139.1(5) 4_557 6_677 ?
O4 V1 O2 110.7(6) . . ?
O8 V1 O2 136.5(5) 6_677 . ?
O6 V1 O2 77.5(5) 4_557 . ?
O3 V1 O2 90.3(5) 6_677 . ?
O4 V1 V3 112.6(5) . 4_557 ?
O8 V1 V3 42.1(4) 6_677 4_557 ?
O6 V1 V3 43.4(4) 4_557 4_557 ?
O3 V1 V3 116.9(4) 6_677 4_557 ?
O2 V1 V3 116.1(4) . 4_557 ?
O4 V1 V2 115.6(5) . . ?
O8 V1 V2 114.7(4) 6_677 . ?
O6 V1 V2 38.0(4) 4_557 . ?
O3 V1 V2 121.7(3) 6_677 . ?
O2 V1 V2 39.7(4) . . ?
V3 V1 V2 79.47(10) 4_557 . ?
O4 V1 V3 115.0(5) . 6_677 ?
O8 V1 V3 37.3(4) 6_677 6_677 ?
O6 V1 V3 114.7(4) 4_557 6_677 ?
O3 V1 V3 41.3(4) 6_677 6_677 ?
O2 V1 V3 120.9(4) . 6_677 ?
V3 V1 V3 77.89(13) 4_557 6_677 ?
V2 V1 V3 129.25(13) . 6_677 ?
O5 V2 O6 111.0(4) . 4_557 ?
O5 V2 O6 111.1(4) . . ?
O6 V2 O6 137.9(8) 4_557 . ?
O5 V2 O2 105.6(4) . . ?
O6 V2 O2 79.7(5) 4_557 . ?
O6 V2 O2 89.2(5) . . ?
O5 V2 O2 105.6(4) . 4_557 ?
O6 V2 O2 89.2(5) 4_557 4_557 ?
O6 V2 O2 79.7(5) . 4_557 ?
O2 V2 O2 148.8(8) . 4_557 ?
O5 V2 V1 111.37(9) . . ?
O6 V2 V1 39.3(4) 4_557 . ?
O6 V2 V1 120.8(4) . . ?
O2 V2 V1 40.6(4) . . ?
O2 V2 V1 124.3(4) 4_557 . ?
O5 V2 V1 111.37(9) . 4_557 ?
O6 V2 V1 120.8(4) 4_557 4_557 ?
O6 V2 V1 39.3(4) . 4_557 ?
O2 V2 V1 124.3(4) . 4_557 ?
O2 V2 V1 40.6(4) 4_557 4_557 ?
V1 V2 V1 137.27(17) . 4_557 ?
O7 V3 O8 108.2(6) . 2_765 ?
O7 V3 O8 109.8(6) . . ?
O8 V3 O8 88.4(7) 2_765 . ?
O7 V3 O6 109.9(6) . . ?
O8 V3 O6 84.0(5) 2_765 . ?
O8 V3 O6 140.0(5) . . ?
O7 V3 O3 106.0(6) . . ?
O8 V3 O3 145.7(5) 2_765 . ?
O8 V3 O3 77.0(5) . . ?
O6 V3 O3 87.6(5) . . ?
O7 V3 V1 107.3(5) . 4_557 ?
O8 V3 V1 42.2(4) 2_765 4_557 ?
O8 V3 V1 125.5(4) . 4_557 ?
O6 V3 V1 43.3(4) . 4_557 ?
O3 V3 V1 127.7(3) . 4_557 ?
O7 V3 V1 111.2(5) . 6_677 ?
O8 V3 V1 120.8(4) 2_765 6_677 ?
O8 V3 V1 37.2(4) . 6_677 ?
O6 V3 V1 119.8(4) . 6_677 ?
O3 V3 V1 39.8(3) . 6_677 ?
V1 V3 V1 141.47(14) 4_557 6_677 ?
Sb1 O1 Sb1 133.3(9) 6_677 . ?
V2 O2 Sb1 120.1(6) . . ?
V2 O2 V1 99.8(6) . . ?
Sb1 O2 V1 140.1(7) . . ?
Sb1 O3 V1 140.2(7) . 6_677 ?
Sb1 O3 V3 120.9(6) . . ?
V1 O3 V3 98.9(5) 6_677 . ?
V2 O6 V1 102.7(6) . 4_557 ?
V2 O6 V3 152.5(7) . . ?
V1 O6 V3 93.4(6) 4_557 . ?
V3 O8 V1 95.7(6) 3_675 6_677 ?
V3 O8 V3 150.4(7) 3_675 . ?
V1 O8 V3 105.4(6) 6_677 . ?
O11 Sb11 O12 97.8(6) . . ?
O11 Sb11 O13 95.9(6) . . ?
O12 Sb11 O13 94.0(5) . . ?
O15 Sb12 O11 97.0(6) . . ?
O15 Sb12 O14 93.0(5) . . ?
O11 Sb12 O14 93.5(5) . . ?
O16 V11 O18 111.5(6) . 3_565 ?
O16 V11 O19 109.6(7) . 3_565 ?
O18 V11 O19 83.0(5) 3_565 3_565 ?
O16 V11 O14 110.5(7) . . ?
O18 V11 O14 137.9(5) 3_565 . ?
O19 V11 O14 79.7(5) 3_565 . ?
O16 V11 O12 110.6(7) . . ?
O18 V11 O12 77.7(5) 3_565 . ?
O19 V11 O12 139.5(5) 3_565 . ?
O14 V11 O12 91.2(5) . . ?
O16 V11 V12 110.5(6) . 3_565 ?
O18 V11 V12 41.9(4) 3_565 3_565 ?
O19 V11 V12 42.2(3) 3_565 3_565 ?
O14 V11 V12 116.9(4) . 3_565 ?
O12 V11 V12 115.7(4) . 3_565 ?
O16 V11 V13 113.6(6) . 3_565 ?
O18 V11 V13 115.6(4) 3_565 3_565 ?
O19 V11 V13 39.7(3) 3_565 3_565 ?
O14 V11 V13 40.1(4) . 3_565 ?
O12 V11 V13 122.8(4) . 3_565 ?
V12 V11 V13 79.94(11) 3_565 3_565 ?
O16 V11 V12 116.4(6) . . ?
O18 V11 V12 37.4(4) 3_565 . ?
O19 V11 V12 113.7(4) 3_565 . ?
O14 V11 V12 121.1(4) . . ?
O12 V11 V12 40.4(4) . . ?
V12 V11 V12 77.37(13) 3_565 . ?
V13 V11 V12 129.55(13) 3_565 . ?
O17 V12 O18 105.2(6) . . ?
O17 V12 O19 110.0(6) . . ?
O18 V12 O19 82.2(5) . . ?
O17 V12 O18 109.1(6) . 3_565 ?
O18 V12 O18 91.2(7) . 3_565 ?
O19 V12 O18 140.7(5) . 3_565 ?
O17 V12 O12 108.2(6) . . ?
O18 V12 O12 146.5(5) . . ?
O19 V12 O12 88.3(5) . . ?
O18 V12 O12 76.1(5) 3_565 . ?
O17 V12 V11 106.4(5) . 2_665 ?
O18 V12 V11 41.3(4) . 2_665 ?
O19 V12 V11 41.9(3) . 2_665 ?
O18 V12 V11 126.8(4) 3_565 2_665 ?
O12 V12 V11 126.9(4) . 2_665 ?
O17 V12 V11 112.9(5) . . ?
O18 V12 V11 122.3(4) . . ?
O19 V12 V11 120.1(3) . . ?
O18 V12 V11 36.5(4) 3_565 . ?
O12 V12 V11 39.6(4) . . ?
V11 V12 V11 140.66(15) 2_665 . ?
O20 V13 O13 106.2(7) . . ?
O20 V13 O19 111.2(6) . . ?
O13 V13 O19 89.9(5) . . ?
O20 V13 O14 104.3(7) . 2_665 ?
O13 V13 O14 149.4(6) . 2_665 ?
O19 V13 O14 79.0(5) . 2_665 ?
O20 V13 O24 109.0(6) . 2_665 ?
O13 V13 O24 78.8(5) . 2_665 ?
O19 V13 O24 139.8(5) . 2_665 ?
O14 V13 O24 91.4(5) 2_665 2_665 ?
O20 V13 V11 110.5(5) . 2_665 ?
O13 V13 V11 124.9(4) . 2_665 ?
O19 V13 V11 38.9(3) . 2_665 ?
O14 V13 V11 40.3(3) 2_665 2_665 ?
O24 V13 V11 123.2(4) 2_665 2_665 ?
O20 V13 V14 111.8(5) . . ?
O13 V13 V14 40.9(4) . . ?
O19 V13 V14 121.6(4) . . ?
O14 V13 V14 124.4(4) 2_665 . ?
O24 V13 V14 37.9(4) 2_665 . ?
V11 V13 V14 137.67(13) 2_665 . ?
O21 V14 O23 112.4(6) . 2_665 ?
O21 V14 O24 108.7(6) . 2_665 ?
O23 V14 O24 84.7(5) 2_665 2_665 ?
O21 V14 O13 109.6(7) . . ?
O23 V14 O13 137.9(5) 2_665 . ?
O24 V14 O13 79.2(5) 2_665 . ?
O21 V14 O15 110.2(6) . . ?
O23 V14 O15 77.2(5) 2_665 . ?
O24 V14 O15 140.9(5) 2_665 . ?
O13 V14 O15 91.4(5) . . ?
O21 V14 V15 111.7(5) . 2_665 ?
O23 V14 V15 42.6(4) 2_665 2_665 ?
O24 V14 V15 42.9(4) 2_665 2_665 ?
O13 V14 V15 116.5(4) . 2_665 ?
O15 V14 V15 115.7(4) . 2_665 ?
O21 V14 V13 113.9(6) . . ?
O23 V14 V13 115.8(4) 2_665 . ?
O24 V14 V13 39.5(4) 2_665 . ?
O13 V14 V13 39.7(4) . . ?
O15 V14 V13 122.3(4) . . ?
V15 V14 V13 79.66(12) 2_665 . ?
O21 V14 V15 116.6(6) . . ?
O23 V14 V15 37.0(4) 2_665 . ?
O24 V14 V15 115.3(4) 2_665 . ?
O13 V14 V15 121.3(4) . . ?
O15 V14 V15 40.3(4) . . ?
V15 V14 V15 77.61(14) 2_665 . ?
V13 V14 V15 129.22(13) . . ?
O22 V15 O23 109.1(6) . 2_665 ?
O22 V15 O23 107.0(6) . . ?
O23 V15 O23 92.3(7) 2_665 . ?
O22 V15 O24 108.0(6) . . ?
O23 V15 O24 142.7(5) 2_665 . ?
O23 V15 O24 80.4(5) . . ?
O22 V15 O15 106.1(6) . . ?
O23 V15 O15 76.5(5) 2_665 . ?
O23 V15 O15 147.0(5) . . ?
O24 V15 O15 89.8(5) . . ?
O22 V15 V14 107.1(5) . 3_565 ?
O23 V15 V14 127.2(4) 2_665 3_565 ?
O23 V15 V14 40.3(4) . 3_565 ?
O24 V15 V14 40.8(4) . 3_565 ?
O15 V15 V14 127.1(4) . 3_565 ?
O22 V15 V14 111.6(5) . . ?
O23 V15 V14 36.0(4) 2_665 . ?
O23 V15 V14 122.9(4) . . ?
O24 V15 V14 122.7(4) . . ?
O15 V15 V14 40.5(4) . . ?
V14 V15 V14 141.30(15) 3_565 . ?
Sb11 O11 Sb12 132.0(7) . . ?
Sb11 O12 V11 137.7(7) . . ?
Sb11 O12 V12 122.3(7) . . ?
V11 O12 V12 100.0(6) . . ?
V13 O13 Sb11 120.9(6) . . ?
V13 O13 V14 99.4(6) . . ?
Sb11 O13 V14 139.7(7) . . ?
V13 O14 V11 99.6(5) 3_565 . ?
V13 O14 Sb12 119.3(6) 3_565 . ?
V11 O14 Sb12 141.1(7) . . ?
Sb12 O15 V15 122.4(7) . . ?
Sb12 O15 V14 138.4(7) . . ?
V15 O15 V14 99.2(6) . . ?
V11 O18 V12 96.8(6) 2_665 . ?
V11 O18 V12 106.1(6) 2_665 2_665 ?
V12 O18 V12 147.7(7) . 2_665 ?
V11 O19 V12 95.9(4) 2_665 . ?
V11 O19 V13 101.4(5) 2_665 . ?
V12 O19 V13 151.3(6) . . ?
V14 O23 V15 107.0(6) 3_565 3_565 ?
V14 O23 V15 97.1(6) 3_565 . ?
V15 O23 V15 146.7(7) 3_565 . ?
V14 O24 V13 102.6(6) 3_565 3_565 ?
V14 O24 V15 96.2(5) 3_565 . ?
V13 O24 V15 147.0(7) 3_565 . ?
N1 Ni1 N1 92.0(6) 3_665 2_655 ?
N1 Ni1 N1 92.0(6) 3_665 . ?
N1 Ni1 N1 92.0(6) 2_655 . ?
N1 Ni1 N2 173.6(7) 3_665 3_665 ?
N1 Ni1 N2 91.7(7) 2_655 3_665 ?
N1 Ni1 N2 82.7(6) . 3_665 ?
N1 Ni1 N2 91.7(7) 3_665 . ?
N1 Ni1 N2 82.7(6) 2_655 . ?
N1 Ni1 N2 173.6(7) . . ?
N2 Ni1 N2 94.0(6) 3_665 . ?
N1 Ni1 N2 82.7(6) 3_665 2_655 ?
N1 Ni1 N2 173.6(7) 2_655 2_655 ?
N1 Ni1 N2 91.7(7) . 2_655 ?
N2 Ni1 N2 94.0(6) 3_665 2_655 ?
N2 Ni1 N2 94.0(6) . 2_655 ?
C1 N1 Ni1 109.1(12) . . ?
C2 C1 N1 106.5(16) 3_665 . ?
C2 N2 Ni1 106.4(11) . . ?
C1 C2 N2 111.0(18) 2_655 . ?
N3 Ni11 N6 170.5(7) . . ?
N3 Ni11 N8 93.6(7) . . ?
N6 Ni11 N8 94.8(8) . . ?
N3 Ni11 N5 91.4(6) . . ?
N6 Ni11 N5 81.0(8) . . ?
N8 Ni11 N5 170.6(7) . . ?
N3 Ni11 N4 82.7(7) . . ?
N6 Ni11 N4 92.6(8) . . ?
N8 Ni11 N4 91.4(7) . . ?
N5 Ni11 N4 97.2(8) . . ?
N3 Ni11 N7 90.2(8) . . ?
N6 Ni11 N7 95.6(8) . . ?
N8 Ni11 N7 80.0(8) . . ?
N5 Ni11 N7 92.0(8) . . ?
N4 Ni11 N7 168.6(7) . . ?
C3 N3 Ni11 109.4(12) . . ?
N3 C3 C4 107.1(17) . . ?
N4 C4 C3 108(2) . . ?
C4 N4 Ni11 105.9(15) . . ?
C5 N5 Ni11 105.7(15) . . ?
N5 C5 C6 108.2(18) . . ?
N6 C6 C5 106(2) . . ?
C6 N6 Ni11 112.3(17) . . ?
C7 N7 Ni11 105.8(13) . . ?
C8 C7 N7 113(2) . . ?
C7 C8 N8 106.6(17) . . ?
C8 N8 Ni11 109.8(16) . . ?
N9 Ni3 N9 92.6(12) . 3_675 ?
N9 Ni3 N9 79(2) . 6_676 ?
N9 Ni3 N9 167(3) 3_675 6_676 ?
N9 Ni3 N9 167(3) . 4_556 ?
N9 Ni3 N9 98(2) 3_675 4_556 ?
N9 Ni3 N9 92.6(12) 6_676 4_556 ?
N9 Ni3 N9 98(2) . 5_766 ?
N9 Ni3 N9 79(2) 3_675 5_766 ?
N9 Ni3 N9 92.6(12) 6_676 5_766 ?
N9 Ni3 N9 92.6(12) 4_556 5_766 ?
N9 Ni3 N9 92.6(12) . 2_765 ?
N9 Ni3 N9 92.6(12) 3_675 2_765 ?
N9 Ni3 N9 98(2) 6_676 2_765 ?
N9 Ni3 N9 79(2) 4_556 2_765 ?
N9 Ni3 N9 167(3) 5_766 2_765 ?
C9 N9 Ni3 108(2) . . ?
C9 C9 N9 102(4) 6_676 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N1 O22 0.99 2.36 3.23(2) 146.3 4_557
N1 H1N1 O23 0.99 2.32 3.104(19) 135.8 6_667
N1 H2N1 O22 0.99 2.31 3.15(2) 142.4 6_667
N2 H1N2 O17 0.99 2.33 3.19(2) 144.6 5_656
N2 H1N2 O18 0.99 2.32 3.132(19) 138.5 6_666
N2 H2N2 O17 0.99 2.40 3.16(2) 133.8 6_666
N3 H1N3 O20 0.99 2.00 2.963(19) 164.9 3_565
C3 H3A O19 0.99 2.59 3.44(3) 143.7 5_656
N4 H1N4 O17 0.99 2.40 3.17(2) 133.9 5_656
N5 H1N5 O16 0.99 2.18 3.08(2) 149.1 4_556
N5 H2N5 O4 0.99 2.30 3.18(2) 148.8 4_557
C6 H6B O4 0.99 2.66 3.46(3) 139.0 4_557
N6 H1N6 O5 0.99 1.97 2.90(2) 154.3 .
N7 H1N7 O6 0.99 2.41 3.29(2) 147.1 .
N8 H1N8 O20 0.99 2.38 3.24(2) 145.1 3_565
N9 H1N9 O7 0.99 2.19 3.14(4) 159.5 .
N9 H1N9 O8 0.99 2.48 3.14(3) 123.7 .
N9 H2N9 O7 0.99 2.41 3.30(5) 149.3 3_675
C9 H9B O7 0.99 2.65 3.50(5) 143.6 6_676

_refine_diff_density_max         1.338
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.138

# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 21.7 12.0
2 0.000 1.000 -0.186 1951.8 681.9
3 0.667 0.333 0.393 22.6 9.9
4 0.333 0.667 0.607 22.6 9.9
_shelxl_version_number           2013-4

