# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2022

####################################################################### 
# 
# 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_1
_audit_block_doi                 10.5517/ccdc.csd.cc2952p8
_database_code_depnum_ccdc_archive 'CCDC 2120049'
loop_
_audit_author_name
_audit_author_address
'fengrui li'
;Northeast Normal University
China
;
_audit_update_record             
;
2021-12-25 deposited with the CCDC.	2022-06-05 downloaded from the CCDC.
;
_audit_creation_date             2021-12-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H40 Mo11 N36 Ni7 O50 P V3.5, 12[H2O]'
_chemical_formula_sum            'C24 H64 Mo11 N36 Ni7 O62 P V3.50'
_chemical_formula_weight         3524.68
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

# start Validation Reply Form
_vrf_PLAT975_1                   
;
PROBLEM: Check Calcd Resid. Dens.  0.57Ang From O18     .       1.81 eA-3  
RESPONSE: Residual density without any chemical sense. 
Modeling of the small residual electron peaks does not make sense 
in this case as the integrity of the refined structure constitutes over 99 %.
;
# end Validation Reply Form

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   17.5370(6)
_cell_length_b                   17.5370(6)
_cell_length_c                   30.2963(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9317.5(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9721
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      57.000
_cell_measurement_theta_min      1.953
_shelx_estimated_absorpt_T_max   0.54
_shelx_estimated_absorpt_T_min   0.21
_exptl_absorpt_coefficient_mu    17.164
_exptl_absorpt_correction_T_max  0.046
_exptl_absorpt_correction_T_min  0.036
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6838
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            61162
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        63.866
_diffrn_reflns_theta_max         63.866
_diffrn_reflns_theta_min         2.911
_diffrn_ambient_temperature      173.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       '0.60\ % \ w and 0.6\ % \ f scans'
_diffrn_radiation_collimation    '0.5 mm double- pinhole'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'equatorially mounted graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Siemens, K FFCU 2K 90'
_diffrn_source_voltage           50.0
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3791
_reflns_number_total             3937
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT(Bruker, 2006)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         3.619
_refine_diff_density_min         -1.738
_refine_diff_density_rms         0.255
_refine_ls_extinction_coef       0.000032(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         3937
_refine_ls_number_restraints     135
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0617
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0874P)²+442.4370P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1687
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Mo4, V2}
3. Uiso/Uaniso restraints and constraints
Mo3: within 3A with sigma of 0.1 and sigma for terminal atoms of 0.3 within 3A
O20 \\sim O14 \\sim O11 \\sim O4: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.03 within 3A
Uanis(O22) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O11)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O18) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O4) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Mo3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(V4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(V5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Mo4) = Uanis(V2)
4. Rigid body (RIGU) restrains
 Mo4, O11, O12, O15
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: Mo4(0.25) V2(0.25) O7(0.5) O12(0.25) O15(0.5) O19(0.4) O21(0.1755)
 O22(0.6) O5(0.0745) V4(0.075) V5(0.05)
6.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Mo1 Mo 0.61971(4) 0.58872(4) 0.92128(2) 0.0220(3) Uani 1 1 d . . . . .
Mo3 Mo 0.64807(4) 0.48414(4) 0.57951(2) 0.0119(2) Uani 1 1 d . U . . .
Mo2 Mo 0.70135(6) 0.46741(6) 1.000000 0.0241(3) Uani 1 2 d S T P B .
Mo4 Mo 0.66011(9) 0.62460(9) 0.500000 0.0243(4) Uani 0.5 2 d S T P A 1
Ni Ni 0.500000 0.500000 0.75060(9) 0.0130(6) Uani 1 4 d S T P B .
Ni2 Ni 0.42045(8) 0.18085(8) 0.81222(5) 0.0171(4) Uani 1 1 d . . . . .
Ni3 Ni 0.250000 0.250000 0.750000 0.0164(5) Uani 1 2 d S . P . .
V1 V 0.500000 0.500000 0.63097(11) 0.0258(8) Uani 1 4 d S T P . .
V2 V 0.66011(9) 0.62460(9) 0.500000 0.0243(4) Uani 0.5 2 d S T P A 2
V3 V 0.500000 0.500000 0.87179(12) 0.0287(8) Uani 1 4 d S T P B .
P P 0.500000 0.500000 1.000000 0.0154(12) Uani 1 8 d S T P . .
P2 P 0.500000 0.500000 0.500000 0.0168(13) Uani 1 8 d S T P A .
O1 O 0.500000 0.500000 0.6843(5) 0.030(3) Uani 1 4 d S T P . .
O2 O 0.4407(4) 0.0774(4) 0.8475(3) 0.0389(19) Uani 1 1 d . . . . .
O4 O 0.5625(5) 0.4206(5) 0.6052(3) 0.0437(19) Uani 1 1 d . U . . .
O6 O 0.500000 0.500000 0.8192(5) 0.031(3) Uani 1 4 d S T P . .
O7 O 0.5707(7) 0.4875(7) 0.9717(4) 0.022(3) Uani 0.5 1 d . U P B .
O8 O 0.5161(5) 0.6007(5) 0.8947(3) 0.048(2) Uani 1 1 d . U . . .
O10 O 0.6706(5) 0.6251(6) 0.8809(3) 0.051(2) Uani 1 1 d . . . . .
O11 O 0.6895(5) 0.5531(5) 0.5436(3) 0.0527(19) Uani 1 1 d . U . . .
O12 O 0.7351(11) 0.6796(11) 0.500000 0.030(3) Uani 0.5 2 d S T P . .
O14 O 0.7109(5) 0.4748(5) 0.6202(3) 0.0406(19) Uani 1 1 d . U . . .
O15 O 0.5559(9) 0.5449(9) 0.5287(5) 0.041(3) Uani 0.5 1 d . U P . .
O16 O 0.7940(6) 0.4543(7) 1.000000 0.049(3) Uani 1 2 d S T P B .
O17 O 0.4707(4) 0.2324(4) 0.8675(2) 0.0328(17) Uani 1 1 d . . . . .
O18 O 0.6898(6) 0.5468(6) 0.9568(4) 0.068(3) Uani 1 1 d . U . . .
O19 O 0.6050(9) 0.6861(10) 0.9491(6) 0.021(4) Uani 0.4 1 d . U P B 2
O20 O 0.6715(6) 0.4015(6) 0.5447(3) 0.056(2) Uani 1 1 d . U . . .
O21 O 0.783(3) 0.663(3) 1.000000 0.067(11) Uani 0.351 2 d S TU P . .
O22 O 0.6015(8) 0.6563(9) 0.9623(5) 0.041(3) Uani 0.6 1 d . U P B 1
N1 N 0.5294(4) 0.1690(4) 0.7836(2) 0.0178(16) Uani 1 1 d . . . . .
N2 N 0.2184(5) 0.2090(6) 0.8866(3) 0.037(2) Uani 1 1 d . . . . .
N3 N 0.3150(4) 0.1973(5) 0.8428(3) 0.0238(17) Uani 1 1 d . . . . .
N4 N 0.4092(4) 0.2849(4) 0.7822(2) 0.0190(16) Uani 1 1 d . . . . .
N5 N 0.6203(4) 0.1353(4) 0.7361(3) 0.0182(16) Uani 1 1 d . . . . .
N6 N 0.6495(4) 0.1902(4) 0.7641(3) 0.0179(16) Uani 1 1 d . . . . .
N7 N 0.2541(4) 0.2250(4) 0.8187(3) 0.0192(16) Uani 1 1 d . . . . .
N8 N 0.3526(4) 0.3072(4) 0.7537(3) 0.0178(16) Uani 1 1 d . . . . .
N9 N 0.4412(4) 0.3979(4) 0.7542(3) 0.0188(16) Uani 1 1 d . . . . .
C1 C 0.5487(5) 0.1254(5) 0.7485(3) 0.022(2) Uani 1 1 d . . . . .
H1 H 0.514513 0.091218 0.734348 0.026 Uiso 1 1 calc R U . . .
C2 C 0.5936(5) 0.2068(5) 0.7914(3) 0.0185(19) Uani 1 1 d . . . . .
H2 H 0.598759 0.242668 0.814696 0.022 Uiso 1 1 calc R U . . .
C3 C 0.3745(5) 0.3743(5) 0.7372(3) 0.0195(19) Uani 1 1 d . . . . .
H3 H 0.346087 0.402263 0.715950 0.023 Uiso 1 1 calc R U . . .
C4 C 0.4599(5) 0.3408(5) 0.7816(3) 0.0181(19) Uani 1 1 d . . . . .
H4 H 0.505064 0.340459 0.798896 0.022 Uiso 1 1 calc R U . . .
C5 C 0.1972(6) 0.2315(6) 0.8459(4) 0.034(2) Uani 1 1 d . . . . .
H5 H 0.147876 0.249503 0.838230 0.041 Uiso 1 1 calc R U . . .
C6 C 0.2919(6) 0.1892(7) 0.8834(4) 0.036(3) Uani 1 1 d . . . . .
H6 H 0.322689 0.171910 0.907153 0.043 Uiso 1 1 calc R U . . .
O5 O 0.532(3) 0.820(3) 0.500000 0.006(10) Uani 0.149 2 d S TU P A .
V4 V 0.5351(15) 0.7236(15) 0.500000 0.058(6) Uani 0.15 2 d S TU P . .
V5 V 0.684(2) 0.625(2) 1.000000 0.053(8) Uani 0.1 2 d S TU P B .


_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
Mo1 V3 3.013(2) . ?
Mo1 O7 2.443(13) 3_655 ?
Mo1 O7 2.493(13) . ?
Mo1 O8 1.998(9) . ?
Mo1 O8 2.034(9) 4_565 ?
Mo1 O10 1.643(8) . ?
Mo1 O18 1.792(11) . ?
Mo1 O19 1.922(17) . ?
Mo1 O22 1.747(14) . ?
Mo1 V5 2.712(18) . ?
Mo3 V1 3.0415(19) . ?
Mo3 O4 2.025(8) . ?
Mo3 O4 1.986(8) 3_655 ?
Mo3 O11 1.782(10) . ?
Mo3 O14 1.663(8) . ?
Mo3 O15 2.478(17) 4_565 ?
Mo3 O15 2.474(17) . ?
Mo3 O20 1.838(10) . ?
Mo3 V4 2.770(13) 11_566 ?
Mo2 O7 2.471(13) . ?
Mo2 O7 2.471(13) 10_557 ?
Mo2 O16 1.641(11) . ?
Mo2 O18 1.921(11) 10_557 ?
Mo2 O18 1.921(11) . ?
Mo2 O19 2.017(17) 4_565 ?
Mo2 O19 2.017(17) 11_567 ?
Mo2 O22 1.841(14) 4_565 ?
Mo2 O22 1.841(14) 11_567 ?
Mo2 V5 2.79(4) . ?
Mo2 V5 2.96(4) 11_567 ?
Mo4 O11 1.893(10) . ?
Mo4 O11 1.892(10) 10_556 ?
Mo4 O12 1.63(2) . ?
Mo4 O15 2.458(16) . ?
Mo4 O15 2.458(16) 10_556 ?
Mo4 O20 1.919(10) 3_655 ?
Mo4 O20 1.919(10) 12_656 ?
Mo4 V4 2.80(3) . ?
Mo4 V4 3.01(3) 11_566 ?
Ni O1 2.008(14) . ?
Ni O6 2.080(15) . ?
Ni N9 2.070(7) 3_655 ?
Ni N9 2.070(7) 2_665 ?
Ni N9 2.070(7) 4_565 ?
Ni N9 2.070(7) . ?
Ni2 O2 2.135(7) . ?
Ni2 O17 2.098(7) . ?
Ni2 N1 2.108(7) . ?
Ni2 N3 2.089(8) . ?
Ni2 N4 2.049(8) . ?
Ni2 N5 2.057(8) 16_546 ?
Ni3 N6 2.095(7) 16_546 ?
Ni3 N6 2.095(7) 4_565 ?
Ni3 N7 2.127(8) . ?
Ni3 N7 2.128(8) 13_556 ?
Ni3 N8 2.063(7) 13_556 ?
Ni3 N8 2.063(7) . ?
V1 O1 1.616(14) . ?
V1 O4 1.936(8) . ?
V1 O4 1.936(8) 2_665 ?
V1 O4 1.936(9) 4_565 ?
V1 O4 1.936(9) 3_655 ?
V2 O11 1.892(10) 10_556 ?
V2 O11 1.893(10) . ?
V2 O12 1.63(2) . ?
V2 O15 2.458(16) . ?
V2 O15 2.458(16) 10_556 ?
V2 O20 1.919(10) 3_655 ?
V2 O20 1.919(10) 12_656 ?
V2 V4 3.01(3) 11_566 ?
V2 V4 2.80(3) . ?
V3 O6 1.592(14) . ?
V3 O8 1.920(9) 2_665 ?
V3 O8 1.920(9) 3_655 ?
V3 O8 1.920(9) . ?
V3 O8 1.920(9) 4_565 ?
P O7 1.524(13) 12_657 ?
P O7 1.524(13) 3_655 ?
P O7 1.524(13) . ?
P O7 1.524(13) 4_565 ?
P O7 1.524(13) 9_667 ?
P O7 1.524(13) 10_557 ?
P O7 1.524(13) 11_567 ?
P O7 1.524(13) 2_665 ?
P2 O15 1.529(16) 9_666 ?
P2 O15 1.529(16) 10_556 ?
P2 O15 1.529(16) . ?
P2 O15 1.529(16) 11_566 ?
P2 O15 1.529(16) 4_565 ?
P2 O15 1.529(16) 3_655 ?
P2 O15 1.529(16) 2_665 ?
P2 O15 1.529(16) 12_656 ?
O7 O7 1.72(3) 10_557 ?
O7 O7 1.782(18) 4_565 ?
O7 O7 1.782(18) 3_655 ?
O11 V4 2.12(2) 11_566 ?
O15 O15 1.74(3) 10_556 ?
O15 O15 1.78(2) 4_565 ?
O15 O15 1.78(2) 3_655 ?
O18 V5 1.90(3) . ?
O19 V5 2.33(3) . ?
O20 V4 1.98(2) 11_566 ?
O21 V5 1.86(6) . ?
O22 V5 1.91(3) . ?
N1 C1 1.353(12) . ?
N1 C2 1.328(12) . ?
N2 C5 1.348(15) . ?
N2 C6 1.338(14) . ?
N3 N7 1.383(11) . ?
N3 C6 1.300(14) . ?
N4 N8 1.372(10) . ?
N4 C4 1.323(12) . ?
N5 N6 1.380(11) . ?
N5 C1 1.322(12) . ?
N6 C2 1.315(12) . ?
N7 C5 1.300(13) . ?
N8 C3 1.335(12) . ?
N9 C3 1.343(12) . ?
N9 C4 1.342(12) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
O5 V4 1.69(5) . ?

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
O7 Mo1 V3 73.0(3) 3_655 . ?
O7 Mo1 V3 72.4(3) . . ?
O7 Mo1 O7 42.3(5) 3_655 . ?
O7 Mo1 V5 76.9(8) . . ?
O7 Mo1 V5 78.4(8) 3_655 . ?
O8 Mo1 V3 39.0(3) 4_565 . ?
O8 Mo1 V3 38.8(3) . . ?
O8 Mo1 O7 64.2(4) . 3_655 ?
O8 Mo1 O7 90.3(4) 4_565 3_655 ?
O8 Mo1 O7 62.8(4) 4_565 . ?
O8 Mo1 O7 90.5(4) . . ?
O8 Mo1 O8 77.7(5) . 4_565 ?
O8 Mo1 V5 134.8(8) . . ?
O8 Mo1 V5 129.0(8) 4_565 . ?
O10 Mo1 V3 102.0(3) . . ?
O10 Mo1 O7 156.8(5) . . ?
O10 Mo1 O7 159.0(5) . 3_655 ?
O10 Mo1 O8 98.8(4) . . ?
O10 Mo1 O8 98.4(4) . 4_565 ?
O10 Mo1 O18 103.6(5) . . ?
O10 Mo1 O19 93.1(7) . . ?
O10 Mo1 O22 111.5(6) . . ?
O10 Mo1 V5 109.8(8) . . ?
O18 Mo1 V3 124.4(4) . . ?
O18 Mo1 O7 95.7(5) . 3_655 ?
O18 Mo1 O7 64.9(5) . . ?
O18 Mo1 O8 155.4(5) . . ?
O18 Mo1 O8 88.8(4) . 4_565 ?
O18 Mo1 O19 101.1(6) . . ?
O18 Mo1 V5 44.4(8) . . ?
O19 Mo1 V3 125.7(5) . . ?
O19 Mo1 O7 108.6(6) . . ?
O19 Mo1 O7 74.8(6) . 3_655 ?
O19 Mo1 O8 87.7(6) . . ?
O19 Mo1 V5 57.3(9) . . ?
O22 Mo1 V3 125.3(5) . . ?
O22 Mo1 O7 60.1(6) . 3_655 ?
O22 Mo1 O7 89.1(6) . . ?
O22 Mo1 O8 92.8(5) . . ?
O22 Mo1 O8 149.8(6) . 4_565 ?
O22 Mo1 O18 88.6(6) . . ?
O22 Mo1 V5 44.6(9) . . ?
V5 Mo1 V3 148.0(7) . . ?
O4 Mo3 V1 38.6(2) 3_655 . ?
O4 Mo3 V1 38.8(2) . . ?
O4 Mo3 O4 77.3(5) 3_655 . ?
O4 Mo3 O15 89.6(5) . . ?
O4 Mo3 O15 89.8(5) 3_655 4_565 ?
O4 Mo3 O15 63.3(5) 3_655 . ?
O4 Mo3 O15 62.7(5) . 4_565 ?
O4 Mo3 V4 135.7(6) 3_655 11_566 ?
O4 Mo3 V4 128.5(6) . 11_566 ?
O11 Mo3 V1 126.8(3) . . ?
O11 Mo3 O4 155.6(4) . . ?
O11 Mo3 O4 91.0(4) . 3_655 ?
O11 Mo3 O15 96.4(5) . 4_565 ?
O11 Mo3 O15 66.0(5) . . ?
O11 Mo3 O20 95.4(4) . . ?
O11 Mo3 V4 50.0(6) . 11_566 ?
O14 Mo3 V1 101.2(3) . . ?
O14 Mo3 O4 100.4(4) . 3_655 ?
O14 Mo3 O4 98.7(4) . . ?
O14 Mo3 O11 104.4(4) . . ?
O14 Mo3 O15 156.5(5) . 4_565 ?
O14 Mo3 O15 159.7(5) . . ?
O14 Mo3 O20 101.5(4) . . ?
O14 Mo3 V4 108.4(6) . 11_566 ?
O15 Mo3 V1 73.8(4) 4_565 . ?
O15 Mo3 V1 73.9(4) . . ?
O15 Mo3 O15 42.1(7) . 4_565 ?
O15 Mo3 V4 76.9(6) 4_565 11_566 ?
O15 Mo3 V4 79.8(6) . 11_566 ?
O20 Mo3 V1 123.8(3) . . ?
O20 Mo3 O4 154.9(4) . 3_655 ?
O20 Mo3 O4 87.3(4) . . ?
O20 Mo3 O15 65.4(5) . 4_565 ?
O20 Mo3 O15 97.4(5) . . ?
O20 Mo3 V4 45.4(6) . 11_566 ?
V4 Mo3 V1 149.9(5) 11_566 . ?
O7 Mo2 O7 40.6(6) . 10_557 ?
O7 Mo2 V5 75.8(8) 10_557 . ?
O7 Mo2 V5 73.2(7) . 11_567 ?
O7 Mo2 V5 75.8(8) . . ?
O7 Mo2 V5 73.2(7) 10_557 11_567 ?
O16 Mo2 O7 159.7(3) . 10_557 ?
O16 Mo2 O7 159.7(3) . . ?
O16 Mo2 O18 101.9(5) . . ?
O16 Mo2 O18 101.9(5) . 10_557 ?
O16 Mo2 O19 92.4(6) . 4_565 ?
O16 Mo2 O19 92.4(6) . 11_567 ?
O16 Mo2 O22 109.5(6) . 11_567 ?
O16 Mo2 O22 109.5(6) . 4_565 ?
O16 Mo2 V5 108.6(8) . 11_567 ?
O16 Mo2 V5 104.5(9) . . ?
O18 Mo2 O7 92.0(5) 10_557 . ?
O18 Mo2 O7 64.0(5) . . ?
O18 Mo2 O7 64.0(5) 10_557 10_557 ?
O18 Mo2 O7 92.0(5) . 10_557 ?
O18 Mo2 O18 85.8(7) 10_557 . ?
O18 Mo2 O19 164.5(6) . 11_567 ?
O18 Mo2 O19 85.5(6) 10_557 11_567 ?
O18 Mo2 O19 164.5(6) 10_557 4_565 ?
O18 Mo2 O19 85.5(6) . 4_565 ?
O18 Mo2 V5 42.9(3) 10_557 . ?
O18 Mo2 V5 42.9(3) . . ?
O18 Mo2 V5 126.9(5) 10_557 11_567 ?
O18 Mo2 V5 126.9(5) . 11_567 ?
O19 Mo2 O7 72.6(6) 4_565 . ?
O19 Mo2 O7 103.5(6) 11_567 . ?
O19 Mo2 O7 72.6(6) 11_567 10_557 ?
O19 Mo2 O7 103.5(6) 4_565 10_557 ?
O19 Mo2 O19 99.9(10) 4_565 11_567 ?
O19 Mo2 V5 51.5(5) 11_567 11_567 ?
O19 Mo2 V5 51.5(5) 4_565 11_567 ?
O19 Mo2 V5 127.7(5) 4_565 . ?
O19 Mo2 V5 127.7(5) 11_567 . ?
O22 Mo2 O7 58.7(6) 4_565 . ?
O22 Mo2 O7 84.9(6) 11_567 . ?
O22 Mo2 O7 84.9(6) 4_565 10_557 ?
O22 Mo2 O7 58.7(6) 11_567 10_557 ?
O22 Mo2 O18 148.5(6) 4_565 10_557 ?
O22 Mo2 O18 90.5(6) 11_567 10_557 ?
O22 Mo2 O18 148.5(6) 11_567 . ?
O22 Mo2 O18 90.5(6) 4_565 . ?
O22 Mo2 O19 19.1(5) 11_567 11_567 ?
O22 Mo2 O19 19.1(5) 4_565 4_565 ?
O22 Mo2 O19 90.2(7) 4_565 11_567 ?
O22 Mo2 O19 90.2(7) 11_567 4_565 ?
O22 Mo2 O22 76.6(10) 4_565 11_567 ?
O22 Mo2 V5 127.2(7) 4_565 . ?
O22 Mo2 V5 38.8(5) 11_567 11_567 ?
O22 Mo2 V5 127.2(7) 11_567 . ?
O22 Mo2 V5 38.8(5) 4_565 11_567 ?
V5 Mo2 V5 146.9(13) . 11_567 ?
O11 Mo4 O11 88.5(6) 10_556 . ?
O11 Mo4 O15 65.1(5) . . ?
O11 Mo4 O15 94.2(5) 10_556 . ?
O11 Mo4 O15 65.1(5) 10_556 10_556 ?
O11 Mo4 O15 94.2(5) . 10_556 ?
O11 Mo4 O20 158.5(4) . 12_656 ?
O11 Mo4 O20 86.8(4) 10_556 12_656 ?
O11 Mo4 O20 158.5(4) 10_556 3_655 ?
O11 Mo4 O20 86.8(4) . 3_655 ?
O11 Mo4 V4 128.7(4) 10_556 . ?
O11 Mo4 V4 128.7(4) . . ?
O11 Mo4 V4 44.3(3) 10_556 11_566 ?
O11 Mo4 V4 44.3(3) . 11_566 ?
O12 Mo4 O11 99.9(5) . . ?
O12 Mo4 O11 99.9(5) . 10_556 ?
O12 Mo4 O15 159.3(4) . 10_556 ?
O12 Mo4 O15 159.3(4) . . ?
O12 Mo4 O20 101.6(5) . 3_655 ?
O12 Mo4 O20 101.6(5) . 12_656 ?
O12 Mo4 V4 104.5(8) . 11_566 ?
O12 Mo4 V4 105.4(8) . . ?
O15 Mo4 O15 41.4(8) 10_556 . ?
O15 Mo4 V4 75.3(6) 10_556 11_566 ?
O15 Mo4 V4 76.7(6) . . ?
O15 Mo4 V4 75.3(6) . 11_566 ?
O15 Mo4 V4 76.7(6) 10_556 . ?
O20 Mo4 O15 64.9(5) 3_655 . ?
O20 Mo4 O15 94.3(5) 12_656 . ?
O20 Mo4 O15 64.9(5) 12_656 10_556 ?
O20 Mo4 O15 94.3(5) 3_655 10_556 ?
O20 Mo4 O20 89.9(6) 12_656 3_655 ?
O20 Mo4 V4 127.4(4) 12_656 11_566 ?
O20 Mo4 V4 44.9(3) 12_656 . ?
O20 Mo4 V4 127.4(4) 3_655 11_566 ?
O20 Mo4 V4 44.9(3) 3_655 . ?
V4 Mo4 V4 150.1(9) . 11_566 ?
O1 Ni O6 180.0 . . ?
O1 Ni N9 93.0(2) . 2_665 ?
O1 Ni N9 93.0(2) . 4_565 ?
O1 Ni N9 93.0(2) . 3_655 ?
O1 Ni N9 93.0(2) . . ?
N9 Ni O6 87.0(2) . . ?
N9 Ni O6 87.0(2) 3_655 . ?
N9 Ni O6 87.0(2) 2_665 . ?
N9 Ni O6 87.0(2) 4_565 . ?
N9 Ni N9 174.0(5) 2_665 . ?
N9 Ni N9 89.84(3) 3_655 . ?
N9 Ni N9 174.0(5) 4_565 3_655 ?
N9 Ni N9 89.84(3) 2_665 3_655 ?
N9 Ni N9 89.84(3) 2_665 4_565 ?
N9 Ni N9 89.84(3) 4_565 . ?
O17 Ni2 O2 84.1(3) . . ?
O17 Ni2 N1 89.4(3) . . ?
N1 Ni2 O2 88.4(3) . . ?
N3 Ni2 O2 92.4(3) . . ?
N3 Ni2 O17 87.6(3) . . ?
N3 Ni2 N1 176.8(3) . . ?
N4 Ni2 O2 174.4(3) . . ?
N4 Ni2 O17 90.7(3) . . ?
N4 Ni2 N1 89.6(3) . . ?
N4 Ni2 N3 89.4(3) . . ?
N4 Ni2 N5 95.6(3) . 16_546 ?
N5 Ni2 O2 89.8(3) 16_546 . ?
N5 Ni2 O17 172.4(3) 16_546 . ?
N5 Ni2 N1 95.0(3) 16_546 . ?
N5 Ni2 N3 88.1(3) 16_546 . ?
N6 Ni3 N6 180.0(4) 16_546 4_565 ?
N6 Ni3 N7 90.5(3) 16_546 . ?
N6 Ni3 N7 90.5(3) 4_565 13_556 ?
N6 Ni3 N7 89.5(3) 16_546 13_556 ?
N6 Ni3 N7 89.5(3) 4_565 . ?
N7 Ni3 N7 180.0 . 13_556 ?
N8 Ni3 N6 89.0(3) . 16_546 ?
N8 Ni3 N6 91.0(3) . 4_565 ?
N8 Ni3 N6 89.0(3) 13_556 4_565 ?
N8 Ni3 N6 91.0(3) 13_556 16_546 ?
N8 Ni3 N7 91.1(3) 13_556 13_556 ?
N8 Ni3 N7 88.9(3) 13_556 . ?
N8 Ni3 N7 91.1(3) . . ?
N8 Ni3 N7 88.9(3) . 13_556 ?
N8 Ni3 N8 180.0(3) . 13_556 ?
Mo3 V1 Mo3 118.33(11) 4_565 3_655 ?
Mo3 V1 Mo3 118.32(11) 2_665 . ?
Mo3 V1 Mo3 74.77(5) 4_565 . ?
Mo3 V1 Mo3 74.77(5) 2_665 3_655 ?
Mo3 V1 Mo3 74.77(5) 4_565 2_665 ?
Mo3 V1 Mo3 74.76(5) 3_655 . ?
O1 V1 Mo3 120.84(6) . 2_665 ?
O1 V1 Mo3 120.84(6) . . ?
O1 V1 Mo3 120.84(6) . 3_655 ?
O1 V1 Mo3 120.84(6) . 4_565 ?
O1 V1 O4 113.8(3) . 2_665 ?
O1 V1 O4 113.8(3) . 4_565 ?
O1 V1 O4 113.8(3) . 3_655 ?
O1 V1 O4 113.8(3) . . ?
O4 V1 Mo3 110.8(3) 3_655 2_665 ?
O4 V1 Mo3 110.8(3) 4_565 . ?
O4 V1 Mo3 110.0(3) 2_665 . ?
O4 V1 Mo3 110.8(3) 2_665 4_565 ?
O4 V1 Mo3 110.0(3) 3_655 4_565 ?
O4 V1 Mo3 110.0(3) . 2_665 ?
O4 V1 Mo3 39.7(3) . 4_565 ?
O4 V1 Mo3 110.0(3) 4_565 3_655 ?
O4 V1 Mo3 39.7(3) 3_655 . ?
O4 V1 Mo3 40.9(2) 3_655 3_655 ?
O4 V1 Mo3 40.9(3) . . ?
O4 V1 Mo3 39.7(3) 2_665 3_655 ?
O4 V1 Mo3 39.7(3) 4_565 2_665 ?
O4 V1 Mo3 40.9(2) 4_565 4_565 ?
O4 V1 Mo3 40.9(3) 2_665 2_665 ?
O4 V1 Mo3 110.8(3) . 3_655 ?
O4 V1 O4 132.4(6) 2_665 . ?
O4 V1 O4 80.6(2) 4_565 . ?
O4 V1 O4 132.4(6) 4_565 3_655 ?
O4 V1 O4 80.6(2) 4_565 2_665 ?
O4 V1 O4 80.6(2) 3_655 2_665 ?
O4 V1 O4 80.6(2) 3_655 . ?
O11 V2 O11 88.5(6) 10_556 . ?
O11 V2 O15 94.2(5) 10_556 . ?
O11 V2 O15 65.1(5) . . ?
O11 V2 O15 94.2(5) . 10_556 ?
O11 V2 O15 65.1(5) 10_556 10_556 ?
O11 V2 O20 158.5(4) 10_556 3_655 ?
O11 V2 O20 86.8(4) . 3_655 ?
O11 V2 O20 158.5(4) . 12_656 ?
O11 V2 O20 86.8(4) 10_556 12_656 ?
O11 V2 V4 128.7(4) 10_556 . ?
O11 V2 V4 44.3(3) 10_556 11_566 ?
O11 V2 V4 44.3(3) . 11_566 ?
O11 V2 V4 128.7(4) . . ?
O12 V2 O11 99.9(5) . 10_556 ?
O12 V2 O11 99.9(5) . . ?
O12 V2 O15 159.3(4) . 10_556 ?
O12 V2 O15 159.3(4) . . ?
O12 V2 O20 101.6(5) . 12_656 ?
O12 V2 O20 101.6(5) . 3_655 ?
O12 V2 V4 104.5(8) . 11_566 ?
O12 V2 V4 105.4(8) . . ?
O15 V2 O15 41.4(8) 10_556 . ?
O15 V2 V4 76.7(6) 10_556 . ?
O15 V2 V4 75.3(6) . 11_566 ?
O15 V2 V4 76.7(6) . . ?
O15 V2 V4 75.3(6) 10_556 11_566 ?
O20 V2 O15 64.9(5) 12_656 10_556 ?
O20 V2 O15 94.3(5) 12_656 . ?
O20 V2 O15 64.9(5) 3_655 . ?
O20 V2 O15 94.3(5) 3_655 10_556 ?
O20 V2 O20 89.9(6) 12_656 3_655 ?
O20 V2 V4 127.4(4) 12_656 11_566 ?
O20 V2 V4 44.9(3) 12_656 . ?
O20 V2 V4 44.9(3) 3_655 . ?
O20 V2 V4 127.4(4) 3_655 11_566 ?
V4 V2 V4 150.1(9) . 11_566 ?
Mo1 V3 Mo1 120.31(12) . 2_665 ?
Mo1 V3 Mo1 75.66(5) . 3_655 ?
Mo1 V3 Mo1 75.66(5) 2_665 4_565 ?
Mo1 V3 Mo1 75.66(5) 3_655 2_665 ?
Mo1 V3 Mo1 75.66(5) . 4_565 ?
Mo1 V3 Mo1 120.31(12) 3_655 4_565 ?
O6 V3 Mo1 119.85(6) . 3_655 ?
O6 V3 Mo1 119.85(6) . 4_565 ?
O6 V3 Mo1 119.85(6) . 2_665 ?
O6 V3 Mo1 119.85(6) . . ?
O6 V3 O8 111.2(3) . . ?
O6 V3 O8 111.2(3) . 2_665 ?
O6 V3 O8 111.2(3) . 4_565 ?
O6 V3 O8 111.2(3) . 3_655 ?
O8 V3 Mo1 112.6(3) 2_665 3_655 ?
O8 V3 Mo1 112.6(3) 3_655 . ?
O8 V3 Mo1 41.8(3) 2_665 4_565 ?
O8 V3 Mo1 113.4(3) 2_665 . ?
O8 V3 Mo1 40.7(3) 4_565 4_565 ?
O8 V3 Mo1 40.7(3) . . ?
O8 V3 Mo1 113.4(3) 3_655 4_565 ?
O8 V3 Mo1 112.6(3) 4_565 2_665 ?
O8 V3 Mo1 112.6(3) . 4_565 ?
O8 V3 Mo1 41.8(3) 4_565 . ?
O8 V3 Mo1 41.8(3) . 3_655 ?
O8 V3 Mo1 41.8(3) 3_655 2_665 ?
O8 V3 Mo1 40.7(3) 2_665 2_665 ?
O8 V3 Mo1 113.4(3) . 2_665 ?
O8 V3 Mo1 40.7(3) 3_655 3_655 ?
O8 V3 Mo1 113.4(3) 4_565 3_655 ?
O8 V3 O8 82.5(2) 4_565 2_665 ?
O8 V3 O8 137.5(6) . 2_665 ?
O8 V3 O8 82.5(2) 2_665 3_655 ?
O8 V3 O8 82.5(2) . 4_565 ?
O8 V3 O8 82.5(2) . 3_655 ?
O8 V3 O8 137.5(6) 4_565 3_655 ?
O7 P O7 180.0 12_657 4_565 ?
O7 P O7 108.5(5) 4_565 9_667 ?
O7 P O7 111.5(9) 2_665 . ?
O7 P O7 71.5(5) 12_657 10_557 ?
O7 P O7 108.5(5) 3_655 9_667 ?
O7 P O7 108.5(5) 4_565 10_557 ?
O7 P O7 180.0 11_567 3_655 ?
O7 P O7 108.5(5) 12_657 2_665 ?
O7 P O7 68.5(9) 2_665 9_667 ?
O7 P O7 71.5(5) 4_565 2_665 ?
O7 P O7 71.5(5) 4_565 . ?
O7 P O7 180.0 10_557 2_665 ?
O7 P O7 71.5(5) 3_655 . ?
O7 P O7 111.5(9) 12_657 11_567 ?
O7 P O7 71.5(5) 12_657 9_667 ?
O7 P O7 68.5(9) 4_565 11_567 ?
O7 P O7 111.5(9) 10_557 9_667 ?
O7 P O7 71.5(5) 10_557 11_567 ?
O7 P O7 71.5(5) 11_567 9_667 ?
O7 P O7 108.5(5) 2_665 11_567 ?
O7 P O7 108.5(5) 12_657 . ?
O7 P O7 68.5(10) 12_657 3_655 ?
O7 P O7 68.5(10) 10_557 . ?
O7 P O7 111.5(9) 4_565 3_655 ?
O7 P O7 108.5(5) 11_567 . ?
O7 P O7 108.5(5) 10_557 3_655 ?
O7 P O7 71.5(5) 2_665 3_655 ?
O7 P O7 180.0 9_667 . ?
O15 P2 O15 71.2(6) 9_666 11_566 ?
O15 P2 O15 110.8(12) 3_655 4_565 ?
O15 P2 O15 69.2(12) 10_556 . ?
O15 P2 O15 108.8(6) 9_666 3_655 ?
O15 P2 O15 180.0 9_666 . ?
O15 P2 O15 180.0(10) 11_566 3_655 ?
O15 P2 O15 108.8(6) 9_666 4_565 ?
O15 P2 O15 69.2(12) 9_666 2_665 ?
O15 P2 O15 108.8(6) 10_556 4_565 ?
O15 P2 O15 108.8(6) 11_566 2_665 ?
O15 P2 O15 71.2(6) 3_655 . ?
O15 P2 O15 71.2(6) 3_655 2_665 ?
O15 P2 O15 71.2(6) 4_565 . ?
O15 P2 O15 110.8(12) 9_666 10_556 ?
O15 P2 O15 69.2(12) 11_566 4_565 ?
O15 P2 O15 71.2(6) 11_566 10_556 ?
O15 P2 O15 71.2(6) 2_665 4_565 ?
O15 P2 O15 108.8(6) 3_655 10_556 ?
O15 P2 O15 180.0(10) 12_656 4_565 ?
O15 P2 O15 180.0(10) 2_665 10_556 ?
O15 P2 O15 108.8(6) 11_566 . ?
O15 P2 O15 71.2(6) 9_666 12_656 ?
O15 P2 O15 110.8(12) 2_665 . ?
O15 P2 O15 110.8(12) 11_566 12_656 ?
O15 P2 O15 108.8(6) 12_656 . ?
O15 P2 O15 108.8(6) 2_665 12_656 ?
O15 P2 O15 71.2(6) 10_556 12_656 ?
O15 P2 O15 69.2(12) 3_655 12_656 ?
V1 O1 Ni 180.0 . . ?
Mo3 O4 Mo3 134.1(5) 4_565 . ?
V1 O4 Mo3 100.3(4) . . ?
V1 O4 Mo3 101.7(4) . 4_565 ?
V3 O6 Ni 180.0 . . ?
Mo1 O7 Mo1 96.9(4) 4_565 . ?
Mo1 O7 Mo2 89.3(4) 4_565 . ?
Mo2 O7 Mo1 89.7(4) . . ?
P O7 Mo1 121.5(7) . . ?
P O7 Mo1 124.6(7) . 4_565 ?
P O7 Mo2 125.4(7) . . ?
P O7 O7 55.7(5) . 10_557 ?
P O7 O7 54.2(2) . 3_655 ?
P O7 O7 54.2(2) . 4_565 ?
O7 O7 Mo1 133.7(4) 4_565 . ?
O7 O7 Mo1 67.3(6) 3_655 . ?
O7 O7 Mo1 70.4(6) 4_565 4_565 ?
O7 O7 Mo1 127.8(3) 10_557 . ?
O7 O7 Mo1 128.7(3) 10_557 4_565 ?
O7 O7 Mo1 134.8(3) 3_655 4_565 ?
O7 O7 Mo2 69.7(3) 10_557 . ?
O7 O7 Mo2 130.5(8) 3_655 . ?
O7 O7 Mo2 132.6(8) 4_565 . ?
O7 O7 O7 89.998(9) 10_557 4_565 ?
O7 O7 O7 90.000(1) 10_557 3_655 ?
O7 O7 O7 89.998(6) 3_655 4_565 ?
Mo1 O8 Mo1 132.9(5) . 3_655 ?
V3 O8 Mo1 99.2(4) . 3_655 ?
V3 O8 Mo1 100.5(4) . . ?
Mo3 O11 Mo4 139.8(6) . . ?
Mo3 O11 V2 139.8(6) . . ?
Mo3 O11 V4 90.0(7) . 11_566 ?
Mo4 O11 V4 97.2(6) . 11_566 ?
V2 O11 V4 97.2(6) . 11_566 ?
Mo3 O15 Mo3 96.5(6) . 3_655 ?
Mo4 O15 Mo3 88.8(5) . . ?
Mo4 O15 Mo3 90.9(5) . 3_655 ?
V2 O15 Mo3 90.9(5) . 3_655 ?
V2 O15 Mo3 88.8(5) . . ?
P2 O15 Mo3 123.4(9) . . ?
P2 O15 Mo3 123.2(9) . 3_655 ?
P2 O15 Mo4 124.7(9) . . ?
P2 O15 V2 124.7(9) . . ?
P2 O15 O15 54.4(3) . 3_655 ?
P2 O15 O15 54.4(3) . 4_565 ?
P2 O15 O15 55.4(6) . 10_556 ?
O15 O15 Mo3 134.1(5) 3_655 . ?
O15 O15 Mo3 134.0(5) 4_565 3_655 ?
O15 O15 Mo3 128.5(4) 10_556 . ?
O15 O15 Mo3 128.4(4) 10_556 3_655 ?
O15 O15 Mo3 68.8(8) 3_655 3_655 ?
O15 O15 Mo3 69.1(8) 4_565 . ?
O15 O15 Mo4 69.3(4) 10_556 . ?
O15 O15 Mo4 132.6(10) 3_655 . ?
O15 O15 Mo4 130.2(10) 4_565 . ?
O15 O15 V2 132.6(10) 3_655 . ?
O15 O15 V2 69.3(4) 10_556 . ?
O15 O15 V2 130.2(10) 4_565 . ?
O15 O15 O15 89.996(5) 10_556 4_565 ?
O15 O15 O15 90.000(6) 3_655 4_565 ?
O15 O15 O15 89.997(6) 10_556 3_655 ?
Mo1 O18 Mo2 141.2(7) . . ?
Mo1 O18 V5 94.4(10) . . ?
V5 O18 Mo2 93.6(9) . . ?
Mo1 O19 Mo2 122.5(10) . 3_655 ?
Mo1 O19 V5 78.7(10) . . ?
Mo2 O19 V5 85.7(9) 3_655 . ?
Mo3 O20 Mo4 138.9(6) . 11_566 ?
Mo3 O20 V4 93.1(8) . 11_566 ?
Mo4 O20 V4 91.8(7) 11_566 11_566 ?
Mo1 O22 Mo2 148.5(9) . 3_655 ?
Mo1 O22 V5 95.5(11) . . ?
Mo2 O22 V5 104.2(10) 3_655 . ?
C1 N1 Ni2 127.3(6) . . ?
C2 N1 Ni2 130.3(6) . . ?
C2 N1 C1 102.1(7) . . ?
C6 N2 C5 105.9(9) . . ?
N7 N3 Ni2 119.8(6) . . ?
C6 N3 Ni2 132.8(7) . . ?
C6 N3 N7 107.3(8) . . ?
N8 N4 Ni2 127.1(6) . . ?
C4 N4 Ni2 126.9(6) . . ?
C4 N4 N8 105.5(7) . . ?
N6 N5 Ni2 125.2(5) . 15_556 ?
C1 N5 Ni2 129.0(6) . 15_556 ?
C1 N5 N6 105.7(7) . . ?
N5 N6 Ni3 122.4(6) . 3_655 ?
C2 N6 Ni3 130.1(6) . 3_655 ?
C2 N6 N5 105.3(7) . . ?
N3 N7 Ni3 128.1(6) . . ?
C5 N7 Ni3 125.2(7) . . ?
C5 N7 N3 106.7(8) . . ?
N4 N8 Ni3 121.8(6) . . ?
C3 N8 Ni3 131.2(6) . . ?
C3 N8 N4 106.2(7) . . ?
C3 N9 Ni 132.8(6) . . ?
C4 N9 Ni 123.8(6) . . ?
C4 N9 C3 102.7(7) . . ?
N1 C1 H1 123.6 . . ?
N5 C1 N1 112.7(8) . . ?
N5 C1 H1 123.6 . . ?
N1 C2 H2 122.9 . . ?
N6 C2 N1 114.2(8) . . ?
N6 C2 H2 122.9 . . ?
N8 C3 N9 112.2(8) . . ?
N8 C3 H3 123.9 . . ?
N9 C3 H3 123.9 . . ?
N4 C4 N9 113.3(8) . . ?
N4 C4 H4 123.3 . . ?
N9 C4 H4 123.3 . . ?
N2 C5 H5 125.0 . . ?
N7 C5 N2 110.1(9) . . ?
N7 C5 H5 125.0 . . ?
N2 C6 H6 125.0 . . ?
N3 C6 N2 109.9(9) . . ?
N3 C6 H6 125.0 . . ?
Mo3 V4 Mo3 120.8(9) 12_656 3_655 ?
Mo3 V4 Mo4 73.1(5) 12_656 3_655 ?
Mo3 V4 Mo4 78.4(6) 3_655 . ?
Mo3 V4 Mo4 78.4(6) 12_656 . ?
Mo3 V4 Mo4 73.1(5) 3_655 3_655 ?
Mo3 V4 V2 78.4(6) 12_656 . ?
Mo3 V4 V2 78.4(6) 3_655 . ?
Mo4 V4 Mo4 119.9(9) . 3_655 ?
V2 V4 Mo4 119.9(9) . 3_655 ?
O11 V4 Mo3 108.5(10) 3_655 12_656 ?
O11 V4 Mo3 40.1(3) 3_655 3_655 ?
O11 V4 Mo3 108.5(10) 12_656 3_655 ?
O11 V4 Mo3 40.1(3) 12_656 12_656 ?
O11 V4 Mo4 38.5(5) 3_655 3_655 ?
O11 V4 Mo4 38.5(5) 12_656 3_655 ?
O11 V4 Mo4 113.4(9) 3_655 . ?
O11 V4 Mo4 113.4(9) 12_656 . ?
O11 V4 V2 113.4(9) 12_656 . ?
O11 V4 V2 113.4(9) 3_655 . ?
O11 V4 O11 77.1(10) 12_656 3_655 ?
O20 V4 Mo3 41.5(4) 3_655 3_655 ?
O20 V4 Mo3 116.3(11) 12_656 3_655 ?
O20 V4 Mo3 41.5(4) 12_656 12_656 ?
O20 V4 Mo3 116.3(11) 3_655 12_656 ?
O20 V4 Mo4 43.3(6) 12_656 . ?
O20 V4 Mo4 43.3(6) 3_655 . ?
O20 V4 Mo4 110.6(9) 3_655 3_655 ?
O20 V4 Mo4 110.6(9) 12_656 3_655 ?
O20 V4 V2 43.3(6) 12_656 . ?
O20 V4 V2 43.3(6) 3_655 . ?
O20 V4 O11 81.5(6) 12_656 12_656 ?
O20 V4 O11 135.0(14) 3_655 12_656 ?
O20 V4 O11 81.5(6) 3_655 3_655 ?
O20 V4 O11 135.0(14) 12_656 3_655 ?
O20 V4 O20 86.6(12) 3_655 12_656 ?
O5 V4 Mo3 118.3(6) . 12_656 ?
O5 V4 Mo3 118.3(6) . 3_655 ?
O5 V4 Mo4 110(2) . 3_655 ?
O5 V4 Mo4 130(2) . . ?
O5 V4 V2 130(2) . . ?
O5 V4 O11 105.0(17) . 3_655 ?
O5 V4 O11 105.0(17) . 12_656 ?
O5 V4 O20 118.7(15) . 12_656 ?
O5 V4 O20 118.7(15) . 3_655 ?
Mo1 V5 Mo1 123.1(14) 10_557 . ?
Mo1 V5 Mo2 79.1(8) 10_557 . ?
Mo1 V5 Mo2 79.1(8) . . ?
Mo1 V5 Mo2 74.8(8) . 3_655 ?
Mo1 V5 Mo2 74.8(8) 10_557 3_655 ?
Mo2 V5 Mo2 123.1(13) . 3_655 ?
O18 V5 Mo1 117.1(16) . 10_557 ?
O18 V5 Mo1 117.1(16) 10_557 . ?
O18 V5 Mo1 41.2(5) 10_557 10_557 ?
O18 V5 Mo1 41.2(5) . . ?
O18 V5 Mo2 112.1(13) 10_557 3_655 ?
O18 V5 Mo2 112.1(13) . 3_655 ?
O18 V5 Mo2 43.4(8) 10_557 . ?
O18 V5 Mo2 43.4(8) . . ?
O18 V5 O18 86.8(16) 10_557 . ?
O18 V5 O19 84.8(8) 10_557 10_557 ?
O18 V5 O19 145(2) . 10_557 ?
O18 V5 O19 84.8(8) . . ?
O18 V5 O19 145(2) 10_557 . ?
O18 V5 O22 131(2) . 10_557 ?
O18 V5 O22 131(2) 10_557 . ?
O18 V5 O22 80.7(10) . . ?
O18 V5 O22 80.7(10) 10_557 10_557 ?
O19 V5 Mo1 44.0(5) 10_557 10_557 ?
O19 V5 Mo1 116.6(15) . 10_557 ?
O19 V5 Mo1 116.6(15) 10_557 . ?
O19 V5 Mo1 44.0(5) . . ?
O19 V5 Mo2 121.4(12) 10_557 . ?
O19 V5 Mo2 42.7(7) . 3_655 ?
O19 V5 Mo2 121.4(12) . . ?
O19 V5 Mo2 42.7(7) 10_557 3_655 ?
O19 V5 O19 83.1(14) 10_557 . ?
O21 V5 Mo1 118.0(7) . . ?
O21 V5 Mo1 118.0(7) . 10_557 ?
O21 V5 Mo2 104(2) . . ?
O21 V5 Mo2 133(2) . 3_655 ?
O21 V5 O18 101.6(18) . . ?
O21 V5 O18 101.6(18) . 10_557 ?
O21 V5 O19 113.2(17) . 10_557 ?
O21 V5 O19 113.2(17) . . ?
O21 V5 O22 127.2(18) . 10_557 ?
O21 V5 O22 127.2(18) . . ?
O22 V5 Mo1 106.3(15) . 10_557 ?
O22 V5 Mo1 39.9(5) . . ?
O22 V5 Mo1 106.3(15) 10_557 . ?
O22 V5 Mo1 39.9(5) 10_557 10_557 ?
O22 V5 Mo2 37.0(8) . 3_655 ?
O22 V5 Mo2 111.4(14) . . ?
O22 V5 Mo2 111.4(14) 10_557 . ?
O22 V5 Mo2 37.0(8) 10_557 3_655 ?
O22 V5 O19 14.1(6) 10_557 10_557 ?
O22 V5 O19 79.7(14) . 10_557 ?
O22 V5 O22 73.2(16) . 10_557 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni N9 C3 N8 -170.3(6) . . . . ?
Ni N9 C4 N4 172.2(6) . . . . ?
Ni2 N1 C1 N5 174.4(6) . . . . ?
Ni2 N1 C2 N6 -173.1(6) . . . . ?
Ni2 N3 N7 Ni3 3.4(10) . . . . ?
Ni2 N3 N7 C5 -178.2(7) . . . . ?
Ni2 N3 C6 N2 178.4(8) . . . . ?
Ni2 N4 N8 Ni3 18.8(10) . . . . ?
Ni2 N4 N8 C3 -170.6(6) . . . . ?
Ni2 N4 C4 N9 171.1(6) . . . . ?
Ni2 N5 N6 Ni3 19.3(9) 15_556 . . 3_655 ?
Ni2 N5 N6 C2 -175.9(6) 15_556 . . . ?
Ni2 N5 C1 N1 175.9(6) 15_556 . . . ?
Ni3 N6 C2 N1 161.9(6) 3_655 . . . ?
Ni3 N7 C5 N2 178.3(7) . . . . ?
Ni3 N8 C3 N9 167.8(6) . . . . ?
V1 Mo3 O11 Mo4 -40.3(10) . . . . ?
V1 Mo3 O11 V2 -40.3(10) . . . . ?
V1 Mo3 O11 V4 -141.5(6) . . . 11_566 ?
V1 Mo3 O20 Mo4 47.1(10) . . . 11_566 ?
V1 Mo3 O20 V4 143.3(7) . . . 11_566 ?
V3 Mo1 O18 Mo2 -38.9(12) . . . . ?
V3 Mo1 O18 V5 -140.3(10) . . . . ?
V3 Mo1 O22 Mo2 11(2) . . . 3_655 ?
V3 Mo1 O22 V5 139.6(10) . . . . ?
O4 Mo3 O11 Mo4 4.7(16) . . . . ?
O4 Mo3 O11 Mo4 -55.7(9) 3_655 . . . ?
O4 Mo3 O11 V2 4.7(16) . . . . ?
O4 Mo3 O11 V2 -55.7(9) 3_655 . . . ?
O4 Mo3 O11 V4 -96.5(11) . . . 11_566 ?
O4 Mo3 O11 V4 -156.9(7) 3_655 . . 11_566 ?
O4 Mo3 O20 Mo4 60.8(8) . . . 11_566 ?
O4 Mo3 O20 Mo4 9.1(16) 3_655 . . 11_566 ?
O4 Mo3 O20 V4 157.0(8) . . . 11_566 ?
O4 Mo3 O20 V4 105.3(11) 3_655 . . 11_566 ?
O7 Mo1 O18 Mo2 34.4(11) 3_655 . . . ?
O7 Mo1 O18 Mo2 4.5(9) . . . . ?
O7 Mo1 O18 V5 -96.8(11) . . . . ?
O7 Mo1 O18 V5 -67.0(11) 3_655 . . . ?
O7 Mo1 O22 Mo2 -56.8(19) . . . 3_655 ?
O7 Mo1 O22 Mo2 -24.3(17) 3_655 . . 3_655 ?
O7 Mo1 O22 V5 72.1(12) . . . . ?
O7 Mo1 O22 V5 104.6(13) 3_655 . . . ?
O7 P O7 Mo1 -177.5(9) 11_567 . . . ?
O7 P O7 Mo1 -56.2(3) 12_657 . . . ?
O7 P O7 Mo1 2.5(9) 3_655 . . . ?
O7 P O7 Mo1 116.7(6) 10_557 . . 4_565 ?
O7 P O7 Mo1 -2.7(9) 4_565 . . 4_565 ?
O7 P O7 Mo1 56.1(3) 11_567 . . 4_565 ?
O7 P O7 Mo1 -63.3(6) 2_665 . . 4_565 ?
O7 P O7 Mo1 -116.8(6) 10_557 . . . ?
O7 P O7 Mo1 -123.9(3) 3_655 . . 4_565 ?
O7 P O7 Mo1 123.8(3) 4_565 . . . ?
O7 P O7 Mo1 177.3(9) 12_657 . . 4_565 ?
O7 P O7 Mo1 63.2(6) 2_665 . . . ?
O7 P O7 Mo2 -1.4(10) 10_557 . . . ?
O7 P O7 Mo2 118.0(11) 3_655 . . . ?
O7 P O7 Mo2 178.6(10) 2_665 . . . ?
O7 P O7 Mo2 -62.0(11) 11_567 . . . ?
O7 P O7 Mo2 59.2(11) 12_657 . . . ?
O7 P O7 Mo2 -120.8(11) 4_565 . . . ?
O7 P O7 O7 -60.6(3) 2_665 . . 4_565 ?
O7 P O7 O7 60.6(3) 12_657 . . 10_557 ?
O7 P O7 O7 60.6(3) 2_665 . . 3_655 ?
O7 P O7 O7 -119.4(3) 4_565 . . 10_557 ?
O7 P O7 O7 119.4(3) 3_655 . . 10_557 ?
O7 P O7 O7 180.000(1) 12_657 . . 4_565 ?
O7 P O7 O7 -58.8(6) 12_657 . . 3_655 ?
O7 P O7 O7 180.000(6) 11_567 . . 3_655 ?
O7 P O7 O7 -60.6(3) 11_567 . . 10_557 ?
O7 P O7 O7 -119.4(3) 10_557 . . 3_655 ?
O7 P O7 O7 119.4(3) 10_557 . . 4_565 ?
O7 P O7 O7 180.000(10) 2_665 . . 10_557 ?
O7 P O7 O7 121.2(6) 4_565 . . 3_655 ?
O7 P O7 O7 58.8(6) 11_567 . . 4_565 ?
O7 P O7 O7 -121.2(6) 3_655 . . 4_565 ?
O8 Mo1 O18 Mo2 -55.8(10) 4_565 . . . ?
O8 Mo1 O18 Mo2 0.5(19) . . . . ?
O8 Mo1 O18 V5 -100.8(14) . . . . ?
O8 Mo1 O18 V5 -157.1(11) 4_565 . . . ?
O8 Mo1 O22 Mo2 33.7(19) . . . 3_655 ?
O8 Mo1 O22 Mo2 -37(3) 4_565 . . 3_655 ?
O8 Mo1 O22 V5 162.6(12) . . . . ?
O8 Mo1 O22 V5 92.4(14) 4_565 . . . ?
O10 Mo1 O18 Mo2 -154.1(10) . . . . ?
O10 Mo1 O18 V5 104.5(11) . . . . ?
O10 Mo1 O22 Mo2 134.2(18) . . . 3_655 ?
O10 Mo1 O22 V5 -96.9(12) . . . . ?
O11 Mo3 O20 Mo4 -94.9(9) . . . 11_566 ?
O11 Mo3 O20 V4 1.3(8) . . . 11_566 ?
O11 Mo4 O11 Mo3 -99.6(8) 10_556 . . . ?
O11 Mo4 O11 V4 -1.0(9) 10_556 . . 11_566 ?
O11 V2 O11 Mo3 -99.6(8) 10_556 . . . ?
O11 V2 O11 V4 -1.0(9) 10_556 . . 11_566 ?
O12 Mo4 O11 Mo3 160.6(9) . . . . ?
O12 Mo4 O11 V4 -100.7(9) . . . 11_566 ?
O12 V2 O11 Mo3 160.6(9) . . . . ?
O12 V2 O11 V4 -100.7(9) . . . 11_566 ?
O14 Mo3 O11 Mo4 -156.7(8) . . . . ?
O14 Mo3 O11 V2 -156.7(8) . . . . ?
O14 Mo3 O11 V4 102.1(7) . . . 11_566 ?
O14 Mo3 O20 Mo4 159.2(8) . . . 11_566 ?
O14 Mo3 O20 V4 -104.6(8) . . . 11_566 ?
O15 Mo3 O11 Mo4 4.3(8) . . . . ?
O15 Mo3 O11 Mo4 34.2(9) 4_565 . . . ?
O15 Mo3 O11 V2 4.3(8) . . . . ?
O15 Mo3 O11 V2 34.2(9) 4_565 . . . ?
O15 Mo3 O11 V4 -97.0(8) . . . 11_566 ?
O15 Mo3 O11 V4 -67.0(8) 4_565 . . 11_566 ?
O15 Mo3 O20 Mo4 -28.4(9) . . . 11_566 ?
O15 Mo3 O20 Mo4 -0.3(8) 4_565 . . 11_566 ?
O15 Mo3 O20 V4 95.9(9) 4_565 . . 11_566 ?
O15 Mo3 O20 V4 67.8(8) . . . 11_566 ?
O15 Mo4 O11 Mo3 -4.3(8) . . . . ?
O15 Mo4 O11 Mo3 -34.6(9) 10_556 . . . ?
O15 Mo4 O11 V4 94.3(9) . . . 11_566 ?
O15 Mo4 O11 V4 64.0(9) 10_556 . . 11_566 ?
O15 V2 O11 Mo3 -4.3(8) . . . . ?
O15 V2 O11 Mo3 -34.6(9) 10_556 . . . ?
O15 V2 O11 V4 94.3(9) . . . 11_566 ?
O15 V2 O11 V4 64.0(9) 10_556 . . 11_566 ?
O15 P2 O15 Mo3 123.6(4) 3_655 . . . ?
O15 P2 O15 Mo3 63.2(8) 2_665 . . . ?
O15 P2 O15 Mo3 116.8(8) 10_556 . . 3_655 ?
O15 P2 O15 Mo3 -123.6(4) 4_565 . . 3_655 ?
O15 P2 O15 Mo3 2.8(11) 4_565 . . . ?
O15 P2 O15 Mo3 -56.4(4) 11_566 . . . ?
O15 P2 O15 Mo3 -116.8(8) 10_556 . . . ?
O15 P2 O15 Mo3 177.2(11) 11_566 . . 3_655 ?
O15 P2 O15 Mo3 -177.2(11) 12_656 . . . ?
O15 P2 O15 Mo3 -2.8(11) 3_655 . . 3_655 ?
O15 P2 O15 Mo3 -63.2(8) 2_665 . . 3_655 ?
O15 P2 O15 Mo3 56.4(4) 12_656 . . 3_655 ?
O15 P2 O15 Mo4 118.1(14) 4_565 . . . ?
O15 P2 O15 Mo4 -61.9(14) 12_656 . . . ?
O15 P2 O15 Mo4 -1.5(13) 10_556 . . . ?
O15 P2 O15 Mo4 -121.1(14) 3_655 . . . ?
O15 P2 O15 Mo4 178.5(13) 2_665 . . . ?
O15 P2 O15 Mo4 58.9(14) 11_566 . . . ?
O15 P2 O15 V2 -121.1(14) 3_655 . . . ?
O15 P2 O15 V2 58.9(14) 11_566 . . . ?
O15 P2 O15 V2 118.1(14) 4_565 . . . ?
O15 P2 O15 V2 -1.5(13) 10_556 . . . ?
O15 P2 O15 V2 -61.9(14) 12_656 . . . ?
O15 P2 O15 V2 178.5(13) 2_665 . . . ?
O15 P2 O15 O15 -59.2(8) 11_566 . . 4_565 ?
O15 P2 O15 O15 -60.4(4) 12_656 . . 10_556 ?
O15 P2 O15 O15 119.6(4) 10_556 . . 3_655 ?
O15 P2 O15 O15 120.8(8) 3_655 . . 4_565 ?
O15 P2 O15 O15 180.000(2) 11_566 . . 3_655 ?
O15 P2 O15 O15 60.4(4) 2_665 . . 4_565 ?
O15 P2 O15 O15 180.0 2_665 . . 10_556 ?
O15 P2 O15 O15 -119.6(4) 10_556 . . 4_565 ?
O15 P2 O15 O15 -120.8(8) 4_565 . . 3_655 ?
O15 P2 O15 O15 180.000(5) 12_656 . . 4_565 ?
O15 P2 O15 O15 -60.4(4) 2_665 . . 3_655 ?
O15 P2 O15 O15 60.4(4) 11_566 . . 10_556 ?
O15 P2 O15 O15 59.2(8) 12_656 . . 3_655 ?
O15 P2 O15 O15 -119.6(4) 3_655 . . 10_556 ?
O15 P2 O15 O15 119.6(4) 4_565 . . 10_556 ?
O18 Mo1 O22 Mo2 -121.7(19) . . . 3_655 ?
O18 Mo1 O22 V5 7.2(12) . . . . ?
O19 Mo1 O18 Mo2 110.0(11) . . . . ?
O19 Mo1 O18 V5 8.6(12) . . . . ?
O20 Mo3 O11 Mo4 100.0(9) . . . . ?
O20 Mo3 O11 V2 100.0(9) . . . . ?
O20 Mo3 O11 V4 -1.2(8) . . . 11_566 ?
O20 Mo4 O11 Mo3 59.4(9) 3_655 . . . ?
O20 Mo4 O11 Mo3 -22.1(18) 12_656 . . . ?
O20 Mo4 O11 V4 76.5(14) 12_656 . . 11_566 ?
O20 Mo4 O11 V4 158.0(8) 3_655 . . 11_566 ?
O20 V2 O11 Mo3 59.4(9) 3_655 . . . ?
O20 V2 O11 Mo3 -22.1(18) 12_656 . . . ?
O20 V2 O11 V4 158.0(8) 3_655 . . 11_566 ?
O20 V2 O11 V4 76.5(14) 12_656 . . 11_566 ?
O22 Mo1 O18 Mo2 94.2(11) . . . . ?
O22 Mo1 O18 V5 -7.2(12) . . . . ?
N3 N7 C5 N2 -0.2(12) . . . . ?
N4 N8 C3 N9 -1.5(10) . . . . ?
N5 N6 C2 N1 -1.3(10) . . . . ?
N6 N5 C1 N1 -1.4(10) . . . . ?
N7 N3 C6 N2 1.2(13) . . . . ?
N8 N4 C4 N9 -0.9(10) . . . . ?
C1 N1 C2 N6 0.5(10) . . . . ?
C1 N5 N6 Ni3 -163.2(6) . . . 3_655 ?
C1 N5 N6 C2 1.6(9) . . . . ?
C2 N1 C1 N5 0.6(10) . . . . ?
C3 N9 C4 N4 0.0(10) . . . . ?
C4 N4 N8 Ni3 -169.2(6) . . . . ?
C4 N4 N8 C3 1.4(10) . . . . ?
C4 N9 C3 N8 0.9(10) . . . . ?
C5 N2 C6 N3 -1.3(14) . . . . ?
C6 N2 C5 N7 0.9(13) . . . . ?
C6 N3 N7 Ni3 -179.0(8) . . . . ?
C6 N3 N7 C5 -0.6(11) . . . . ?
V4 Mo3 O11 Mo4 101.2(11) 11_566 . . . ?
V4 Mo3 O11 V2 101.2(11) 11_566 . . . ?
V4 Mo3 O20 Mo4 -96.2(11) 11_566 . . 11_566 ?
V4 Mo4 O11 Mo3 41.7(12) . . . . ?
V4 Mo4 O11 Mo3 -98.6(12) 11_566 . . . ?
V4 Mo4 O11 V4 140.3(12) . . . 11_566 ?
V4 V2 O11 Mo3 -98.6(12) 11_566 . . . ?
V4 V2 O11 Mo3 41.7(12) . . . . ?
V4 V2 O11 V4 140.3(12) . . . 11_566 ?
V5 Mo1 O18 Mo2 101.4(15) . . . . ?
V5 Mo1 O22 Mo2 -129(3) . . . 3_655 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.000 349.6 119.0 '12 H2O'
2 0.000 0.500 0.500 349.6 119.0 '12 H2O'
3 0.500 0.000 0.500 349.6 119.0 '12 H2O'
4 0.500 1.000 0.000 349.6 119.0 '12 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_b
_audit_block_doi                 10.5517/ccdc.csd.cc28cgy2
_database_code_depnum_ccdc_archive 'CCDC 2096404'
loop_
_audit_author_name
_audit_author_address
'fengrui li'
;Northeast Normal University
China
;
_audit_update_record             
;
2021-12-25 deposited with the CCDC.	2022-06-05 downloaded from the CCDC.
;
_audit_creation_date             2021-12-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C24 H41 Mo8 N36 Ni7 O50 P V6, 17[H2O]'
_chemical_formula_sum            'C24 H75 Mo8 N36 Ni7 O67 P V6'
_chemical_formula_weight         3422.99
_chemical_melting_point          ?
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'
Mo Mo -1.6832 0.6857 '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'
Ni Ni 0.3393 1.1124 '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'
P P 0.1023 0.0942 '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'

# start Validation Reply Form
_vrf_PLAT975_b                   
;
PROBLEM: Check Calcd Resid. Dens.  0.54Ang From O9      .       2.09 eA-3  
RESPONSE: Residual density without any chemical sense. 
Modeling of the small residual electron peaks does not make sense 
in this case as the integrity of the refined structure constitutes over 99 %.
;
# end Validation Reply Form

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   17.5443(19)
_cell_length_b                   17.5443(19)
_cell_length_c                   30.317(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9332(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9394
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_shelx_estimated_absorpt_T_max   0.574
_shelx_estimated_absorpt_T_min   0.521
_exptl_absorpt_coefficient_mu    3.121
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6768
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0286
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            26105
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.072
_diffrn_reflns_theta_max         25.072
_diffrn_reflns_theta_min         1.341
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5° ω and 0.5° φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3828
_reflns_number_total             4241
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         2.524
_refine_diff_density_min         -0.961
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.000111(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4241
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0417
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0502P)²+151.7508P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1107
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O3) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O13(0.5) O14(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C5(H5)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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
Mo1 Mo 1.12194(3) 0.91046(3) 0.57794(2) 0.02535(16) Uani 1 1 d . . . . .
Mo2 Mo 1.01465(3) 0.85006(3) 0.92094(2) 0.02540(16) Uani 1 1 d . . . . .
Ni1 Ni 1.000000 1.000000 0.74993(4) 0.0104(3) Uani 1 4 d S T P . .
Ni3 Ni 0.68129(4) 0.92021(4) 0.68794(2) 0.01572(17) Uani 1 1 d . . . . .
Ni2 Ni 0.750000 0.750000 0.750000 0.0149(2) Uani 1 2 d S . P . .
V1 V 1.000000 1.000000 0.86960(6) 0.0230(4) Uani 1 4 d S T P . .
V2 V 1.000000 1.000000 0.62912(6) 0.0210(4) Uani 1 4 d S T P . .
V3 V 1.20360(7) 1.03328(7) 0.500000 0.0158(3) Uani 1 2 d S T P . .
O1 O 1.000000 1.000000 0.6821(3) 0.0281(18) Uani 1 4 d S T P . .
N1 N 0.8979(2) 0.9415(2) 0.74632(15) 0.0176(9) Uani 1 1 d . . . . .
O2 O 1.1724(3) 0.8747(3) 0.61915(16) 0.0440(12) Uani 1 1 d . . . . .
O3 O 1.0999(3) 1.0161(3) 0.60526(15) 0.0364(11) Uani 1 1 d . U . . .
N3 N 0.9715(2) 0.6682(2) 0.71666(15) 0.0195(9) Uani 1 1 d . . . . .
O4 O 1.2936(3) 1.0461(4) 0.500000 0.0463(19) Uani 1 2 d S T P . .
N4 N 0.8804(2) 0.6358(2) 0.76444(15) 0.0191(9) Uani 1 1 d . . . . .
N5 N 0.6984(3) 0.8152(3) 0.65695(16) 0.0244(10) Uani 1 1 d . . . . .
O1W O 0.5785(3) 0.9418(3) 0.65198(17) 0.0442(12) Uani 1 1 d . . . . .
O2W O 0.7342(3) 0.9717(3) 0.63300(15) 0.0369(11) Uani 1 1 d . . . . .
O5 O 0.9367(3) 0.9223(3) 0.89430(17) 0.0404(12) Uani 1 1 d . . . . .
O6 O 1.000000 1.000000 0.8163(3) 0.0311(19) Uani 1 4 d S T P . .
O7 O 1.0225(3) 0.7876(3) 0.87981(15) 0.0454(13) Uani 1 1 d . . . . .
O8 O 1.0964(3) 0.8254(3) 0.95504(19) 0.0568(14) Uani 1 1 d . U . . .
N6 N 0.8511(2) 0.6897(2) 0.73634(15) 0.0185(9) Uani 1 1 d . . . . .
N2 N 0.7252(3) 0.7541(2) 0.68093(16) 0.0213(10) Uani 1 1 d . . . . .
O9 O 1.1928(3) 0.9543(3) 0.5434(2) 0.0573(14) Uani 1 1 d . U . . .
O10 O 0.9443(4) 0.8102(4) 0.9561(2) 0.0623(15) Uani 1 1 d . U . . .
O11 O 1.1707(4) 1.1036(3) 0.4563(2) 0.070(2) Uani 1 1 d . . . . .
V4 V 1.15938(8) 0.87187(8) 1.000000 0.0224(3) Uani 1 2 d S T P . .
N8 N 0.7114(4) 0.7184(3) 0.61273(19) 0.0389(13) Uani 1 1 d . . . . .
N9 N 0.8076(2) 0.8527(2) 0.74654(15) 0.0182(9) Uani 1 1 d . . . . .
C1 C 0.7319(4) 0.6976(3) 0.6534(2) 0.0309(14) Uani 1 1 d . . . . .
H1 H 0.748820 0.649120 0.660977 0.037 Uiso 1 1 calc R U . . .
C2 C 0.6906(4) 0.7920(4) 0.6163(2) 0.0366(15) Uani 1 1 d . . . . .
H2 H 0.673202 0.822046 0.593166 0.044 Uiso 1 1 calc R U . . .
P2 P 1.000000 1.000000 0.500000 0.0147(7) Uani 1 8 d S T P . .
P1 P 1.000000 1.000000 1.000000 0.0166(8) Uani 1 8 d S T P . .
C3 C 0.8409(3) 0.9600(3) 0.71882(18) 0.0190(11) Uani 1 1 d . . . . .
H3 H 0.840528 1.004208 0.701929 0.023 Uiso 1 1 calc R U . . .
O12 O 1.2288(4) 0.8152(4) 1.000000 0.055(2) Uani 1 2 d S T P . .
C4 C 0.9065(3) 0.7063(3) 0.70860(19) 0.0199(11) Uani 1 1 d . . . . .
H4 H 0.901081 0.741124 0.685661 0.024 Uiso 1 1 calc R U . . .
C6 C 0.8741(3) 0.8743(3) 0.76264(19) 0.0193(11) Uani 1 1 d . . . . .
H6 H 0.901560 0.845947 0.783118 0.023 Uiso 1 1 calc R U . . .
O13 O 0.9545(4) 0.9441(4) 0.9714(2) 0.0198(16) Uani 0.5 1 d . . P . .
O14 O 1.0118(4) 0.9290(4) 0.5287(2) 0.0184(16) Uani 0.5 1 d . . P . .
C5 C 0.9522(3) 0.6261(3) 0.75204(19) 0.0206(12) Uani 1 1 d . . . . .
H5 H 0.985829 0.593529 0.766365 0.025 Uiso 1 1 calc R U . . .
N7 N 0.7854(2) 0.9093(2) 0.71806(15) 0.0183(9) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mo1 V2 3.0745(11) . ?
Mo1 O2 1.654(4) . ?
Mo1 O3 2.066(5) . ?
Mo1 O3 2.042(5) 4_575 ?
Mo1 O9 1.798(6) . ?
Mo1 O11 1.793(5) 11_576 ?
Mo1 O14 2.487(7) 3_755 ?
Mo1 O14 2.464(7) . ?
Mo2 O5 2.046(5) 3_755 ?
Mo2 O5 2.032(5) . ?
Mo2 O7 1.666(4) . ?
Mo2 O8 1.819(6) . ?
Mo2 O10 1.774(6) . ?
Mo2 O13 2.485(7) . ?
Mo2 O13 2.495(7) 3_755 ?
Ni1 O1 2.057(8) . ?
Ni1 N1 2.068(4) . ?
Ni1 N1 2.068(4) 3_755 ?
Ni1 N1 2.068(4) 4_575 ?
Ni1 N1 2.068(4) 2_775 ?
Ni1 O6 2.011(8) . ?
Ni3 N3 2.102(4) 4_575 ?
Ni3 N4 2.055(4) 13_666 ?
Ni3 N5 2.090(5) . ?
Ni3 O1W 2.142(4) . ?
Ni3 O2W 2.110(4) . ?
Ni3 N7 2.051(4) . ?
Ni2 N6 2.107(4) . ?
Ni2 N6 2.107(4) 13_666 ?
Ni2 N2 2.140(5) 13_666 ?
Ni2 N2 2.140(5) . ?
Ni2 N9 2.069(4) 13_666 ?
Ni2 N9 2.069(4) . ?
V1 O5 1.911(4) 3_755 ?
V1 O5 1.911(4) 4_575 ?
V1 O5 1.911(4) 2_775 ?
V1 O5 1.911(4) . ?
V1 O6 1.617(8) . ?
V2 O1 1.606(8) . ?
V2 O3 1.917(5) 2_775 ?
V2 O3 1.917(5) 3_755 ?
V2 O3 1.917(5) . ?
V2 O3 1.917(5) 4_575 ?
V3 O4 1.594(6) . ?
V3 O9 1.920(6) . ?
V3 O9 1.920(6) 10_556 ?
V3 O11 1.899(5) 10_556 ?
V3 O11 1.899(5) . ?
N1 C3 1.342(7) . ?
N1 C6 1.345(7) . ?
N3 C4 1.345(7) . ?
N3 C5 1.346(7) . ?
N4 N6 1.372(6) . ?
N4 C5 1.325(7) . ?
N5 N2 1.377(6) . ?
N5 C2 1.304(8) . ?
O8 V4 1.935(6) . ?
N6 C4 1.317(7) . ?
N2 C1 1.302(7) . ?
O10 V4 1.917(6) 11_577 ?
V4 O12 1.572(7) . ?
N8 C1 1.334(9) . ?
N8 C2 1.346(9) . ?
N9 C6 1.319(7) . ?
N9 N7 1.372(6) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
P2 O14 1.533(7) 12_756 ?
P2 O14 1.533(7) . ?
P2 O14 1.533(7) 2_775 ?
P2 O14 1.533(7) 9_776 ?
P2 O14 1.533(7) 4_575 ?
P2 O14 1.533(7) 11_576 ?
P2 O14 1.533(7) 3_755 ?
P2 O14 1.533(7) 10_556 ?
P1 O13 1.533(7) . ?
P1 O13 1.533(7) 2_775 ?
P1 O13 1.533(7) 3_755 ?
P1 O13 1.533(7) 9_777 ?
P1 O13 1.533(7) 10_557 ?
P1 O13 1.533(7) 12_757 ?
P1 O13 1.533(7) 11_577 ?
P1 O13 1.533(7) 4_575 ?
C3 H3 0.9300 . ?
C3 N7 1.318(7) . ?
C4 H4 0.9300 . ?
C6 H6 0.9300 . ?
O13 O13 1.789(10) 3_755 ?
O13 O13 1.733(14) 10_557 ?
O13 O13 1.789(10) 4_575 ?
O14 O14 1.741(14) 10_556 ?
O14 O14 1.785(10) 4_575 ?
O14 O14 1.785(10) 3_755 ?
C5 H5 0.9300 . ?

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 Mo1 V2 100.64(18) . . ?
O2 Mo1 O3 97.9(2) . . ?
O2 Mo1 O3 98.4(2) . 4_575 ?
O2 Mo1 O9 103.5(3) . . ?
O2 Mo1 O11 103.5(3) . 11_576 ?
O2 Mo1 O14 156.4(3) . 3_755 ?
O2 Mo1 O14 158.0(3) . . ?
O3 Mo1 V2 37.60(13) 4_575 . ?
O3 Mo1 V2 37.73(13) . . ?
O3 Mo1 O3 75.3(2) 4_575 . ?
O3 Mo1 O14 88.7(2) . . ?
O3 Mo1 O14 62.1(2) . 3_755 ?
O3 Mo1 O14 62.8(2) 4_575 . ?
O3 Mo1 O14 88.8(2) 4_575 3_755 ?
O9 Mo1 V2 123.82(19) . . ?
O9 Mo1 O3 154.6(2) . 4_575 ?
O9 Mo1 O3 88.8(2) . . ?
O9 Mo1 O14 66.0(2) . 3_755 ?
O9 Mo1 O14 97.6(3) . . ?
O11 Mo1 V2 125.01(16) 11_576 . ?
O11 Mo1 O3 90.1(2) 11_576 4_575 ?
O11 Mo1 O3 155.7(2) 11_576 . ?
O11 Mo1 O9 97.2(3) 11_576 . ?
O11 Mo1 O14 98.9(3) 11_576 3_755 ?
O11 Mo1 O14 67.2(3) 11_576 . ?
O14 Mo1 V2 72.07(17) . . ?
O14 Mo1 V2 71.79(16) 3_755 . ?
O14 Mo1 O14 42.3(3) . 3_755 ?
O5 Mo2 O5 75.2(2) . 3_755 ?
O5 Mo2 O13 62.6(2) 3_755 3_755 ?
O5 Mo2 O13 62.9(2) . . ?
O5 Mo2 O13 88.9(2) . 3_755 ?
O5 Mo2 O13 88.8(2) 3_755 . ?
O7 Mo2 O5 99.7(2) . . ?
O7 Mo2 O5 98.5(2) . 3_755 ?
O7 Mo2 O8 101.7(3) . . ?
O7 Mo2 O10 104.3(3) . . ?
O7 Mo2 O13 158.9(3) . . ?
O7 Mo2 O13 156.7(3) . 3_755 ?
O8 Mo2 O5 154.7(2) . . ?
O8 Mo2 O5 88.6(2) . 3_755 ?
O8 Mo2 O13 98.2(3) . . ?
O8 Mo2 O13 66.3(2) . 3_755 ?
O10 Mo2 O5 154.9(3) . 3_755 ?
O10 Mo2 O5 90.9(2) . . ?
O10 Mo2 O8 96.5(3) . . ?
O10 Mo2 O13 97.1(3) . 3_755 ?
O10 Mo2 O13 66.2(3) . . ?
O13 Mo2 O13 42.1(3) . 3_755 ?
O1 Ni1 N1 86.97(13) . 4_575 ?
O1 Ni1 N1 86.97(13) . 3_755 ?
O1 Ni1 N1 86.97(13) . 2_775 ?
O1 Ni1 N1 86.96(13) . . ?
N1 Ni1 N1 89.840(14) 2_775 4_575 ?
N1 Ni1 N1 89.839(14) . 4_575 ?
N1 Ni1 N1 89.840(14) 2_775 3_755 ?
N1 Ni1 N1 173.9(3) . 2_775 ?
N1 Ni1 N1 89.840(14) . 3_755 ?
N1 Ni1 N1 173.9(3) 4_575 3_755 ?
O6 Ni1 O1 180.0 . . ?
O6 Ni1 N1 93.03(13) . 2_775 ?
O6 Ni1 N1 93.03(13) . 3_755 ?
O6 Ni1 N1 93.04(13) . . ?
O6 Ni1 N1 93.03(13) . 4_575 ?
N3 Ni3 O1W 87.66(19) 4_575 . ?
N3 Ni3 O2W 89.31(18) 4_575 . ?
N4 Ni3 N3 94.80(18) 13_666 4_575 ?
N4 Ni3 N5 88.26(19) 13_666 . ?
N4 Ni3 O1W 89.91(19) 13_666 . ?
N4 Ni3 O2W 172.39(19) 13_666 . ?
N5 Ni3 N3 176.91(19) . 4_575 ?
N5 Ni3 O1W 92.7(2) . . ?
N5 Ni3 O2W 87.69(19) . . ?
O2W Ni3 O1W 83.9(2) . . ?
N7 Ni3 N3 89.83(17) . 4_575 ?
N7 Ni3 N4 96.41(18) . 13_666 ?
N7 Ni3 N5 89.43(18) . . ?
N7 Ni3 O1W 173.37(19) . . ?
N7 Ni3 O2W 89.99(19) . . ?
N6 Ni2 N6 180.00(19) 13_666 . ?
N6 Ni2 N2 89.76(18) . . ?
N6 Ni2 N2 90.24(18) 13_666 . ?
N6 Ni2 N2 90.24(18) . 13_666 ?
N6 Ni2 N2 89.77(18) 13_666 13_666 ?
N2 Ni2 N2 180.0 13_666 . ?
N9 Ni2 N6 89.08(17) 13_666 . ?
N9 Ni2 N6 90.92(17) . . ?
N9 Ni2 N6 90.91(17) 13_666 13_666 ?
N9 Ni2 N6 89.09(17) . 13_666 ?
N9 Ni2 N2 91.18(17) . . ?
N9 Ni2 N2 88.82(17) . 13_666 ?
N9 Ni2 N2 91.17(17) 13_666 13_666 ?
N9 Ni2 N2 88.83(17) 13_666 . ?
N9 Ni2 N9 180.0 . 13_666 ?
Mo2 V1 Mo2 119.02(6) 3_755 4_575 ?
Mo2 V1 Mo2 75.08(3) 3_755 2_775 ?
Mo2 V1 Mo2 75.08(3) 2_775 4_575 ?
O5 V1 Mo2 111.36(16) . 2_775 ?
O5 V1 Mo2 40.81(14) 2_775 3_755 ?
O5 V1 Mo2 111.36(16) 4_575 3_755 ?
O5 V1 Mo2 111.06(16) 2_775 4_575 ?
O5 V1 Mo2 40.81(14) . 4_575 ?
O5 V1 Mo2 111.36(16) 3_755 4_575 ?
O5 V1 Mo2 111.06(16) . 3_755 ?
O5 V1 Mo2 40.37(14) 4_575 4_575 ?
O5 V1 Mo2 111.05(16) 3_755 2_775 ?
O5 V1 Mo2 40.81(14) 4_575 2_775 ?
O5 V1 Mo2 40.37(14) 2_775 2_775 ?
O5 V1 Mo2 40.37(14) 3_755 3_755 ?
O5 V1 O5 81.17(12) . 3_755 ?
O5 V1 O5 133.9(3) . 2_775 ?
O5 V1 O5 81.17(12) 2_775 4_575 ?
O5 V1 O5 81.17(12) 2_775 3_755 ?
O5 V1 O5 81.17(12) . 4_575 ?
O5 V1 O5 133.9(3) 3_755 4_575 ?
O6 V1 Mo2 120.49(3) . 4_575 ?
O6 V1 Mo2 120.49(3) . 3_755 ?
O6 V1 Mo2 120.49(3) . 2_775 ?
O6 V1 O5 113.07(17) . 3_755 ?
O6 V1 O5 113.07(17) . . ?
O6 V1 O5 113.07(17) . 4_575 ?
O6 V1 O5 113.07(17) . 2_775 ?
Mo1 V2 Mo1 119.38(6) 2_775 . ?
Mo1 V2 Mo1 75.24(3) 4_575 . ?
Mo1 V2 Mo1 75.24(3) 2_775 3_755 ?
Mo1 V2 Mo1 75.24(3) 4_575 2_775 ?
Mo1 V2 Mo1 119.38(6) 4_575 3_755 ?
Mo1 V2 Mo1 75.24(3) 3_755 . ?
O1 V2 Mo1 120.31(3) . 3_755 ?
O1 V2 Mo1 120.31(3) . . ?
O1 V2 Mo1 120.31(3) . 4_575 ?
O1 V2 Mo1 120.31(3) . 2_775 ?
O1 V2 O3 112.18(15) . 4_575 ?
O1 V2 O3 112.18(15) . 2_775 ?
O1 V2 O3 112.18(15) . 3_755 ?
O1 V2 O3 112.18(15) . . ?
O3 V2 Mo1 111.75(15) . 2_775 ?
O3 V2 Mo1 112.27(15) . 4_575 ?
O3 V2 Mo1 112.27(15) 3_755 . ?
O3 V2 Mo1 41.27(14) 2_775 2_775 ?
O3 V2 Mo1 111.75(15) 2_775 . ?
O3 V2 Mo1 112.27(15) 4_575 2_775 ?
O3 V2 Mo1 41.27(14) 4_575 4_575 ?
O3 V2 Mo1 40.54(14) 3_755 2_775 ?
O3 V2 Mo1 41.27(14) . . ?
O3 V2 Mo1 40.54(14) . 3_755 ?
O3 V2 Mo1 40.54(14) 4_575 . ?
O3 V2 Mo1 112.27(15) 2_775 3_755 ?
O3 V2 Mo1 40.54(14) 2_775 4_575 ?
O3 V2 Mo1 111.75(15) 4_575 3_755 ?
O3 V2 Mo1 111.75(15) 3_755 4_575 ?
O3 V2 Mo1 41.27(14) 3_755 3_755 ?
O3 V2 O3 135.6(3) 4_575 3_755 ?
O3 V2 O3 81.81(11) . 4_575 ?
O3 V2 O3 81.81(11) 2_775 3_755 ?
O3 V2 O3 81.81(11) 2_775 4_575 ?
O3 V2 O3 81.81(11) . 3_755 ?
O3 V2 O3 135.6(3) . 2_775 ?
O4 V3 O9 101.5(3) . . ?
O4 V3 O9 101.5(3) . 10_556 ?
O4 V3 O11 102.1(3) . 10_556 ?
O4 V3 O11 102.1(3) . . ?
O9 V3 O9 86.5(4) 10_556 . ?
O11 V3 O9 87.8(2) . 10_556 ?
O11 V3 O9 156.4(3) . . ?
O11 V3 O9 156.4(3) 10_556 10_556 ?
O11 V3 O9 87.8(2) 10_556 . ?
O11 V3 O11 88.4(4) 10_556 . ?
V2 O1 Ni1 180.0 . . ?
C3 N1 Ni1 124.0(4) . . ?
C3 N1 C6 102.1(4) . . ?
C6 N1 Ni1 133.2(4) . . ?
Mo1 O3 Mo1 132.1(2) 3_755 . ?
V2 O3 Mo1 101.0(2) . . ?
V2 O3 Mo1 101.9(2) . 3_755 ?
C4 N3 Ni3 129.6(4) . 3_755 ?
C4 N3 C5 101.7(4) . . ?
C5 N3 Ni3 128.2(4) . 3_755 ?
N6 N4 Ni3 124.6(3) . 13_666 ?
C5 N4 Ni3 129.7(4) . 13_666 ?
C5 N4 N6 105.5(4) . . ?
N2 N5 Ni3 119.8(3) . . ?
C2 N5 Ni3 133.2(4) . . ?
C2 N5 N2 107.0(5) . . ?
Mo2 O5 Mo2 132.9(3) . 4_575 ?
V1 O5 Mo2 102.1(2) . . ?
V1 O5 Mo2 101.6(2) . 4_575 ?
V1 O6 Ni1 180.0 . . ?
Mo2 O8 V4 138.6(3) . . ?
N4 N6 Ni2 122.6(3) . . ?
C4 N6 Ni2 129.4(4) . . ?
C4 N6 N4 105.8(4) . . ?
N5 N2 Ni2 127.7(3) . . ?
C1 N2 Ni2 125.7(4) . . ?
C1 N2 N5 106.5(5) . . ?
Mo1 O9 V3 140.9(3) . . ?
Mo2 O10 V4 140.3(4) . 11_577 ?
Mo1 O11 V3 139.7(4) 12_756 . ?
O8 V4 O8 89.6(4) . 10_557 ?
O10 V4 O8 158.1(3) 3_755 10_557 ?
O10 V4 O8 87.1(3) 12_757 10_557 ?
O10 V4 O8 158.1(3) 12_757 . ?
O10 V4 O8 87.1(3) 3_755 . ?
O10 V4 O10 88.1(4) 12_757 3_755 ?
O12 V4 O8 100.1(3) . . ?
O12 V4 O8 100.1(3) . 10_557 ?
O12 V4 O10 101.8(3) . 3_755 ?
O12 V4 O10 101.8(3) . 12_757 ?
C1 N8 C2 105.1(5) . . ?
C6 N9 Ni2 131.5(4) . . ?
C6 N9 N7 106.1(4) . . ?
N7 N9 Ni2 121.5(3) . . ?
N2 C1 N8 111.1(5) . . ?
N2 C1 H1 124.4 . . ?
N8 C1 H1 124.4 . . ?
N5 C2 N8 110.3(6) . . ?
N5 C2 H2 124.8 . . ?
N8 C2 H2 124.8 . . ?
O14 P2 O14 180.0 9_776 . ?
O14 P2 O14 71.2(3) 10_556 12_756 ?
O14 P2 O14 110.8(5) 10_556 9_776 ?
O14 P2 O14 108.8(3) 10_556 4_575 ?
O14 P2 O14 71.2(3) 11_576 9_776 ?
O14 P2 O14 180.0 12_756 4_575 ?
O14 P2 O14 71.2(3) 12_756 9_776 ?
O14 P2 O14 108.8(3) 11_576 . ?
O14 P2 O14 108.8(3) 2_775 12_756 ?
O14 P2 O14 110.8(5) 2_775 . ?
O14 P2 O14 108.8(3) 3_755 9_776 ?
O14 P2 O14 71.2(3) 4_575 . ?
O14 P2 O14 69.2(5) 2_775 9_776 ?
O14 P2 O14 110.8(5) 11_576 12_756 ?
O14 P2 O14 69.2(5) 3_755 12_756 ?
O14 P2 O14 110.8(5) 3_755 4_575 ?
O14 P2 O14 180.0(4) 11_576 3_755 ?
O14 P2 O14 71.2(3) 2_775 4_575 ?
O14 P2 O14 71.2(3) 11_576 10_556 ?
O14 P2 O14 108.8(3) 9_776 4_575 ?
O14 P2 O14 108.8(3) 3_755 10_556 ?
O14 P2 O14 69.2(5) 10_556 . ?
O14 P2 O14 108.8(3) 11_576 2_775 ?
O14 P2 O14 108.8(3) 12_756 . ?
O14 P2 O14 71.2(3) 3_755 2_775 ?
O14 P2 O14 69.2(5) 11_576 4_575 ?
O14 P2 O14 180.0(4) 10_556 2_775 ?
O14 P2 O14 71.2(3) 3_755 . ?
O13 P1 O13 180.0(8) . 9_777 ?
O13 P1 O13 68.8(5) 12_757 3_755 ?
O13 P1 O13 108.6(3) 2_775 11_577 ?
O13 P1 O13 108.6(3) . 12_757 ?
O13 P1 O13 108.6(3) . 11_577 ?
O13 P1 O13 71.4(3) 9_777 12_757 ?
O13 P1 O13 180.0(4) 2_775 10_557 ?
O13 P1 O13 71.4(3) . 4_575 ?
O13 P1 O13 71.4(3) 2_775 3_755 ?
O13 P1 O13 108.6(3) 9_777 4_575 ?
O13 P1 O13 111.2(5) 12_757 11_577 ?
O13 P1 O13 180.0 12_757 4_575 ?
O13 P1 O13 180.0 3_755 11_577 ?
O13 P1 O13 111.2(5) . 2_775 ?
O13 P1 O13 71.4(3) . 3_755 ?
O13 P1 O13 68.8(5) 9_777 2_775 ?
O13 P1 O13 111.2(5) 4_575 3_755 ?
O13 P1 O13 108.6(3) 12_757 2_775 ?
O13 P1 O13 108.6(3) 10_557 3_755 ?
O13 P1 O13 71.4(3) 4_575 2_775 ?
O13 P1 O13 71.4(3) 9_777 11_577 ?
O13 P1 O13 68.8(5) . 10_557 ?
O13 P1 O13 68.8(5) 4_575 11_577 ?
O13 P1 O13 111.2(5) 9_777 10_557 ?
O13 P1 O13 71.4(3) 10_557 11_577 ?
O13 P1 O13 71.4(3) 12_757 10_557 ?
O13 P1 O13 108.6(3) 4_575 10_557 ?
O13 P1 O13 108.6(3) 9_777 3_755 ?
N1 C3 H3 123.3 . . ?
N7 C3 N1 113.5(5) . . ?
N7 C3 H3 123.3 . . ?
N3 C4 H4 123.2 . . ?
N6 C4 N3 113.5(5) . . ?
N6 C4 H4 123.2 . . ?
N1 C6 H6 123.5 . . ?
N9 C6 N1 112.9(5) . . ?
N9 C6 H6 123.5 . . ?
Mo2 O13 Mo2 97.3(2) . 4_575 ?
P1 O13 Mo2 123.5(4) . . ?
P1 O13 Mo2 122.9(4) . 4_575 ?
P1 O13 O13 54.31(13) . 4_575 ?
P1 O13 O13 55.6(3) . 10_557 ?
P1 O13 O13 54.31(13) . 3_755 ?
O13 O13 Mo2 128.02(17) 10_557 . ?
O13 O13 Mo2 134.5(2) 3_755 4_575 ?
O13 O13 Mo2 68.7(4) 4_575 4_575 ?
O13 O13 Mo2 127.84(16) 10_557 4_575 ?
O13 O13 Mo2 134.7(2) 4_575 . ?
O13 O13 Mo2 69.3(4) 3_755 . ?
O13 O13 O13 90.002(3) 10_557 4_575 ?
O13 O13 O13 90.000(6) 4_575 3_755 ?
O13 O13 O13 90.001(5) 10_557 3_755 ?
Mo1 O14 Mo1 98.6(2) . 4_575 ?
P2 O14 Mo1 122.4(4) . 4_575 ?
P2 O14 Mo1 123.8(4) . . ?
P2 O14 O14 54.40(13) . 4_575 ?
P2 O14 O14 55.4(3) . 10_556 ?
P2 O14 O14 54.41(13) . 3_755 ?
O14 O14 Mo1 127.28(17) 10_556 . ?
O14 O14 Mo1 135.1(2) 3_755 4_575 ?
O14 O14 Mo1 126.87(16) 10_556 4_575 ?
O14 O14 Mo1 69.6(4) 3_755 . ?
O14 O14 Mo1 135.6(2) 4_575 . ?
O14 O14 Mo1 68.2(4) 4_575 4_575 ?
O14 O14 O14 89.999(2) 3_755 4_575 ?
O14 O14 O14 89.998(3) 10_556 3_755 ?
O14 O14 O14 89.995(1) 10_556 4_575 ?
N3 C5 H5 123.3 . . ?
N4 C5 N3 113.3(5) . . ?
N4 C5 H5 123.3 . . ?
N9 N7 Ni3 126.9(3) . . ?
C3 N7 Ni3 127.0(4) . . ?
C3 N7 N9 105.5(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N1 C3 N7 171.7(4) . . . . ?
Ni1 N1 C6 N9 -169.9(4) . . . . ?
Ni3 N3 C4 N6 -172.3(4) 3_755 . . . ?
Ni3 N3 C5 N4 173.8(4) 3_755 . . . ?
Ni3 N4 N6 Ni2 20.7(6) 13_666 . . . ?
Ni3 N4 N6 C4 -174.4(4) 13_666 . . . ?
Ni3 N4 C5 N3 173.9(4) 13_666 . . . ?
Ni3 N5 N2 Ni2 2.3(6) . . . . ?
Ni3 N5 N2 C1 -178.5(4) . . . . ?
Ni3 N5 C2 N8 178.0(4) . . . . ?
Ni2 N6 C4 N3 162.3(4) . . . . ?
Ni2 N2 C1 N8 179.5(4) . . . . ?
Ni2 N9 C6 N1 168.4(4) . . . . ?
Ni2 N9 N7 Ni3 18.6(6) . . . . ?
Ni2 N9 N7 C3 -169.5(4) . . . . ?
V2 Mo1 O9 V3 -42.5(6) . . . . ?
N1 C3 N7 Ni3 170.9(4) . . . . ?
N1 C3 N7 N9 -0.9(6) . . . . ?
O2 Mo1 O9 V3 -155.4(5) . . . . ?
O3 Mo1 O9 V3 -57.5(5) . . . . ?
O3 Mo1 O9 V3 -6.8(10) 4_575 . . . ?
O4 V3 O11 Mo1 162.0(6) . . . 12_756 ?
N4 N6 C4 N3 -1.1(6) . . . . ?
N5 N2 C1 N8 0.3(7) . . . . ?
O5 Mo2 O8 V4 11.4(9) . . . . ?
O5 Mo2 O8 V4 60.5(5) 3_755 . . . ?
O5 Mo2 O10 V4 -56.2(6) . . . 11_577 ?
O5 Mo2 O10 V4 -1.0(10) 3_755 . . 11_577 ?
O7 Mo2 O8 V4 159.0(5) . . . . ?
O7 Mo2 O10 V4 -156.5(5) . . . 11_577 ?
O8 Mo2 O10 V4 99.6(6) . . . 11_577 ?
N6 N4 C5 N3 -2.1(6) . . . . ?
N2 N5 C2 N8 -0.1(8) . . . . ?
O9 V3 O11 Mo1 60.7(6) 10_556 . . 12_756 ?
O9 V3 O11 Mo1 -15.3(11) . . . 12_756 ?
O10 Mo2 O8 V4 -94.9(5) . . . . ?
O11 Mo1 O9 V3 98.9(6) 11_576 . . . ?
O11 V3 O11 Mo1 -96.0(5) 10_556 . . 12_756 ?
C1 N8 C2 N5 0.3(8) . . . . ?
C2 N5 N2 Ni2 -179.3(4) . . . . ?
C2 N5 N2 C1 -0.1(7) . . . . ?
C2 N8 C1 N2 -0.4(8) . . . . ?
C3 N1 C6 N9 0.0(6) . . . . ?
C4 N3 C5 N4 1.4(6) . . . . ?
C6 N1 C3 N7 0.6(6) . . . . ?
C6 N9 N7 Ni3 -171.0(4) . . . . ?
C6 N9 N7 C3 0.9(6) . . . . ?
O13 Mo2 O8 V4 0.0(4) 3_755 . . . ?
O13 Mo2 O8 V4 -28.1(5) . . . . ?
O13 Mo2 O10 V4 32.8(6) 3_755 . . 11_577 ?
O13 Mo2 O10 V4 3.5(5) . . . 11_577 ?
O13 P1 O13 Mo2 176.8(5) 12_757 . . 4_575 ?
O13 P1 O13 Mo2 -3.2(5) 4_575 . . 4_575 ?
O13 P1 O13 Mo2 -55.70(17) 12_757 . . . ?
O13 P1 O13 Mo2 -116.2(3) 10_557 . . . ?
O13 P1 O13 Mo2 63.8(3) 2_775 . . . ?
O13 P1 O13 Mo2 116.3(3) 10_557 . . 4_575 ?
O13 P1 O13 Mo2 -63.7(3) 2_775 . . 4_575 ?
O13 P1 O13 Mo2 -124.27(16) 3_755 . . 4_575 ?
O13 P1 O13 Mo2 55.73(16) 11_577 . . 4_575 ?
O13 P1 O13 Mo2 3.2(5) 3_755 . . . ?
O13 P1 O13 Mo2 -176.8(5) 11_577 . . . ?
O13 P1 O13 Mo2 124.30(17) 4_575 . . . ?
O13 P1 O13 O13 60.53(16) 12_757 . . 10_557 ?
O13 P1 O13 O13 180.000(2) 2_775 . . 10_557 ?
O13 P1 O13 O13 -60.53(16) 2_775 . . 4_575 ?
O13 P1 O13 O13 58.9(3) 11_577 . . 4_575 ?
O13 P1 O13 O13 -60.53(16) 11_577 . . 10_557 ?
O13 P1 O13 O13 -58.9(3) 12_757 . . 3_755 ?
O13 P1 O13 O13 -119.47(16) 4_575 . . 10_557 ?
O13 P1 O13 O13 121.1(3) 4_575 . . 3_755 ?
O13 P1 O13 O13 119.47(16) 3_755 . . 10_557 ?
O13 P1 O13 O13 60.53(16) 2_775 . . 3_755 ?
O13 P1 O13 O13 180.000(4) 12_757 . . 4_575 ?
O13 P1 O13 O13 -119.47(16) 10_557 . . 3_755 ?
O13 P1 O13 O13 119.47(16) 10_557 . . 4_575 ?
O13 P1 O13 O13 180.000(3) 11_577 . . 3_755 ?
O13 P1 O13 O13 -121.1(3) 3_755 . . 4_575 ?
O14 Mo1 O9 V3 2.3(5) 3_755 . . . ?
O14 Mo1 O9 V3 31.0(6) . . . . ?
O14 P2 O14 Mo1 64.8(3) 2_775 . . 4_575 ?
O14 P2 O14 Mo1 -4.5(5) 3_755 . . . ?
O14 P2 O14 Mo1 175.5(5) 11_576 . . . ?
O14 P2 O14 Mo1 115.0(3) 10_556 . . . ?
O14 P2 O14 Mo1 -115.2(3) 10_556 . . 4_575 ?
O14 P2 O14 Mo1 4.4(5) 4_575 . . 4_575 ?
O14 P2 O14 Mo1 -175.6(5) 12_756 . . 4_575 ?
O14 P2 O14 Mo1 54.64(18) 12_756 . . . ?
O14 P2 O14 Mo1 -65.0(3) 2_775 . . . ?
O14 P2 O14 Mo1 -54.75(17) 11_576 . . 4_575 ?
O14 P2 O14 Mo1 125.25(17) 3_755 . . 4_575 ?
O14 P2 O14 Mo1 -125.36(18) 4_575 . . . ?
O14 P2 O14 O14 -60.41(16) 2_775 . . 3_755 ?
O14 P2 O14 O14 180.000(3) 12_756 . . 4_575 ?
O14 P2 O14 O14 -119.59(16) 3_755 . . 10_556 ?
O14 P2 O14 O14 59.2(3) 12_756 . . 3_755 ?
O14 P2 O14 O14 180.000(1) 11_576 . . 3_755 ?
O14 P2 O14 O14 -60.41(16) 12_756 . . 10_556 ?
O14 P2 O14 O14 60.41(16) 2_775 . . 4_575 ?
O14 P2 O14 O14 -120.8(3) 4_575 . . 3_755 ?
O14 P2 O14 O14 119.59(16) 10_556 . . 3_755 ?
O14 P2 O14 O14 -59.2(3) 11_576 . . 4_575 ?
O14 P2 O14 O14 60.41(16) 11_576 . . 10_556 ?
O14 P2 O14 O14 120.8(3) 3_755 . . 4_575 ?
O14 P2 O14 O14 180.000(5) 2_775 . . 10_556 ?
O14 P2 O14 O14 -119.59(16) 10_556 . . 4_575 ?
O14 P2 O14 O14 119.59(16) 4_575 . . 10_556 ?
C5 N3 C4 N6 -0.1(6) . . . . ?
C5 N4 N6 Ni2 -163.0(4) . . . . ?
C5 N4 N6 C4 1.9(6) . . . . ?
N7 N9 C6 N1 -0.6(6) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 0.000 463.5 175.8 '17 H2O'
2 0.000 0.500 0.500 463.5 175.8 '17 H2O'
3 0.500 1.000 0.500 463.5 175.8 '17 H2O'
4 0.500 0.000 0.000 463.5 175.8 '17 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_1_CCDC1
_audit_block_doi                 10.5517/ccdc.csd.cc2952q9
_database_code_depnum_ccdc_archive 'CCDC 2120050'
loop_
_audit_author_name
_audit_author_address
'fengrui li'
;Northeast Normal University
China
;
_audit_update_record             
;
2021-12-25 deposited with the CCDC.	2022-06-05 downloaded from the CCDC.
;
_audit_creation_date             2021-12-25
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_shelx_SHELXL_version_number     2018/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'P2 Mo16 V12 O84 H6, C40 H48 N8, 12H2O'
_chemical_formula_sum            'C40 H78 Mo16 N8 O96 P2 V12'
_chemical_formula_weight         4414.32
_chemical_melting_point          ?
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'
Mo Mo -1.6832 0.6857 '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'
P P 0.1023 0.0942 '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'

# start Validation Reply Form
_vrf_PLAT975_1                   
;
PROBLEM: Check Calcd Resid. Dens.  0.66Ang From O8      .       1.55 eA-3  
RESPONSE: Residual density without any chemical sense. 
Modeling of the small residual electron peaks does not make sense 
in this case as the integrity of the refined structure constitutes over 99 %.
;
# end Validation Reply Form

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   12.910(3)
_cell_length_b                   13.921(3)
_cell_length_c                   16.910(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3039.1(14)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7476
_cell_measurement_temperature    295.04
_cell_measurement_theta_max      25.127
_cell_measurement_theta_min      1.628
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.600
_exptl_absorpt_correction_T_max  0.87
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.413
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15730
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.081
_diffrn_reflns_theta_max         25.081
_diffrn_reflns_theta_min         2.926
_diffrn_ambient_temperature      295.04
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5° ω and 0.5° φ scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.9
_diffrn_source_power             0.0405
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_diffrn_standards_number         .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1174
_reflns_number_total             1529
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.533
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.234
_refine_ls_extinction_coef       0.00051(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1529
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0764
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0541P)²+190.0169P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1903
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Shared sites
{Mo3, V2}
3. Restrained distances
 V1-O2B
 0.001 with sigma of 1.98
4. Uiso/Uaniso restraints and constraints
O8: within 2A with sigma of 0.1 and sigma for terminal atoms of 0.3 within 2A
Uanis(O8) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O9) \\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O2B) \\sim Ueq, Uanis(O2A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Mo3) = Uanis(V2)
5. Others
 Sof(O2B)=1-FVAR(1)
 Sof(O2A)=FVAR(1)
 Fixed Sof: Mo3(0.5) V1(0.25) V2(0.5) O7(0.25) O9(0.25) O10(0.25) N1(0.375)
 H1A(0.375) H1B(0.375) C1(0.375) C3(0.75) H3(0.75) C2(0.75) H2(0.75) O11(0.125)
6.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Mo1 Mo 0.000000 0.000000 0.21137(12) 0.0431(6) Uani 1 4 d S T P A .
Mo2 Mo 0.000000 0.25630(14) 0.000000 0.0518(7) Uani 1 4 d S T P A .
Mo3 Mo 0.20190(9) 0.12508(8) 0.10224(8) 0.0354(5) Uani 0.5 1 d . . P A 1
V1 V 0.000000 0.2052(3) 0.1667(3) 0.0367(12) Uani 0.5 2 d DS T P A .
P1 P 0.000000 0.000000 0.000000 0.0093(11) Uani 1 8 d S T P . .
V2 V 0.20190(9) 0.12508(8) 0.10224(8) 0.0354(5) Uani 0.5 1 d . . P A 2
O1 O 0.2867(6) 0.1855(6) 0.1535(6) 0.059(2) Uani 1 1 d . . . . .
O2B O 0.092(3) 0.095(2) 0.178(3) 0.040(8) Uani 0.55(15) 1 d D U P A 2
O3 O 0.000000 0.3762(11) 0.000000 0.056(5) Uani 1 4 d S T P . .
O4 O 0.000000 0.000000 0.3087(9) 0.059(5) Uani 1 4 d S T P A .
O5 O 0.1006(7) 0.2275(8) 0.0802(5) 0.067(3) Uani 1 1 d . . . . .
O6 O 0.2448(13) 0.1335(12) 0.000000 0.084(5) Uani 1 2 d S TU P . .
O7 O 0.000000 0.2906(13) 0.2316(11) 0.030(4) Uani 0.5 2 d S TU P A .
O8 O 0.2480(12) 0.000000 0.1152(9) 0.072(4) Uani 1 2 d S TU P A 1
O9 O 0.0691(13) 0.000000 0.0726(10) 0.020(4) Uani 0.5 2 d S TU P A .
O10 O 0.0709(14) 0.0903(12) 0.000000 0.029(4) Uani 0.5 2 d S T P A .
N1 N 0.2648(16) 0.000000 0.2974(11) 0.045(5) Uani 0.75 2 d S T P . .
H1A H 0.210716 0.000001 0.264776 0.054 Uiso 0.75 2 calc R U P . .
H1B H 0.321172 0.000000 0.267107 0.054 Uiso 0.75 2 calc R U P . .
C1 C 0.2596(15) 0.000000 0.4562(11) 0.031(4) Uani 0.75 2 d S T P . .
C3 C 0.2635(14) 0.0829(12) 0.3344(10) 0.055(4) Uani 0.75 1 d . . P . .
H3 H 0.266291 0.140013 0.305876 0.066 Uiso 0.75 1 calc R U P . .
C2 C 0.2580(15) 0.0847(10) 0.4132(11) 0.056(5) Uani 0.75 1 d . . P . .
H2 H 0.253151 0.143246 0.439395 0.068 Uiso 0.75 1 calc R U P . .
O11 O 0.500000 0.000000 0.337(2) 0.056(9) Uani 0.5 4 d S T P . .
O2A O 0.110(3) 0.100(2) 0.203(4) 0.038(9) Uani 0.45(15) 1 d . U P A 1


_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
Mo1 V1 2.955(5) 2 ?
Mo1 O2B 1.86(3) 11 ?
Mo1 O2B 1.86(3) 2 ?
Mo1 O2B 1.86(3) 12 ?
Mo1 O2B 1.86(3) . ?
Mo1 O4 1.646(15) . ?
Mo1 O9 2.510(17) 2 ?
Mo1 O9 2.510(17) . ?
Mo1 O2A 2.00(3) 12 ?
Mo1 O2A 2.00(3) 11 ?
Mo1 O2A 2.00(3) 2 ?
Mo1 O2A 2.00(3) . ?
Mo2 V1 2.907(6) . ?
Mo2 V1 2.907(6) 10 ?
Mo2 O3 1.669(16) . ?
Mo2 O5 1.920(8) 11 ?
Mo2 O5 1.920(8) . ?
Mo2 O5 1.920(8) 4 ?
Mo2 O5 1.920(8) 10 ?
Mo2 O10 2.486(17) 11 ?
Mo2 O10 2.486(17) . ?
Mo3 V1 3.037(3) . ?
Mo3 O1 1.630(8) . ?
Mo3 O5 1.970(9) . ?
Mo3 O6 1.819(6) . ?
Mo3 O8 1.853(5) . ?
Mo3 O9 2.494(12) . ?
Mo3 O10 2.467(13) . ?
Mo3 O2A 2.10(4) . ?
V1 V2 3.037(3) . ?
V1 O2B 1.95(3) 11 ?
V1 O2B 1.95(3) . ?
V1 O5 1.980(10) 11 ?
V1 O5 1.980(10) . ?
V1 O7 1.618(19) . ?
V1 O2A 2.12(5) 11 ?
V1 O2A 2.12(5) . ?
P1 O9 1.518(16) 9 ?
P1 O9 1.518(16) . ?
P1 O9 1.518(16) 2 ?
P1 O9 1.518(16) 10 ?
P1 O10 1.554(17) . ?
P1 O10 1.554(17) 3 ?
P1 O10 1.554(17) 9 ?
P1 O10 1.554(17) 11 ?
V2 O1 1.630(8) . ?
V2 O2B 1.96(2) . ?
V2 O5 1.970(9) . ?
V2 O6 1.819(6) . ?
V2 O10 2.467(13) . ?
O9 O9 1.78(3) 2 ?
O9 O10 1.757(16) 3 ?
O9 O10 1.757(16) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C3 1.313(19) 12 ?
N1 C3 1.313(19) . ?
C1 C1 1.48(4) 10_556 ?
C1 C2 1.386(18) 12 ?
C1 C2 1.386(18) . ?
C3 H3 0.9300 . ?
C3 C2 1.33(2) . ?
C2 H2 0.9300 . ?

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
O2B Mo1 O2B 144(4) 2 . ?
O2B Mo1 O2B 90.4(15) 12 . ?
O2B Mo1 O2B 79(2) 11 . ?
O2B Mo1 O9 87(2) 2 . ?
O2B Mo1 O9 59.3(18) . . ?
O2B Mo1 O9 87(2) 11 . ?
O2B Mo1 O9 59.3(18) 12 . ?
O2B Mo1 O2A 86.1(17) 2 12 ?
O2B Mo1 O2A 91.4(6) . 12 ?
O2B Mo1 O2A 158(4) 11 12 ?
O2B Mo1 O2A 14.0(9) 12 12 ?
O4 Mo1 V1 104.81(11) . 2 ?
O4 Mo1 O2B 108(2) . . ?
O4 Mo1 O2B 108(2) . 2 ?
O4 Mo1 O2B 108(2) . 12 ?
O4 Mo1 O2B 108(2) . 11 ?
O4 Mo1 O9 159.2(4) . 2 ?
O4 Mo1 O9 159.2(4) . . ?
O4 Mo1 O2A 94(2) . 2 ?
O4 Mo1 O2A 94(2) . 12 ?
O4 Mo1 O2A 94(2) . 11 ?
O4 Mo1 O2A 94(2) . . ?
O9 Mo1 V1 76.18(11) 2 2 ?
O9 Mo1 V1 76.18(11) . 2 ?
O9 Mo1 O9 41.6(7) . 2 ?
O2A Mo1 V1 131.2(9) 11 2 ?
O2A Mo1 V1 45.9(14) 2 2 ?
O2A Mo1 V1 45.9(14) 12 2 ?
O2A Mo1 V1 131.2(9) . 2 ?
O2A Mo1 O9 71.3(18) 2 2 ?
O2A Mo1 O9 71.3(18) 11 2 ?
O2A Mo1 O9 101(2) 12 2 ?
O2A Mo1 O9 101(2) . 2 ?
O2A Mo1 O9 101(2) 11 . ?
O2A Mo1 O9 101(2) 2 . ?
O2A Mo1 O9 71.3(18) 12 . ?
O2A Mo1 O9 71.3(18) . . ?
O2A Mo1 O2A 90(2) 2 12 ?
O2A Mo1 O2A 88.9(19) 2 11 ?
O2A Mo1 O2A 90(2) 11 . ?
O2A Mo1 O2A 172(4) 2 . ?
O2A Mo1 O2A 88.9(19) 12 . ?
O2A Mo1 O2A 172(4) 12 11 ?
V1 Mo2 V1 151.7(2) 10 . ?
O3 Mo2 V1 104.16(10) . . ?
O3 Mo2 V1 104.16(10) . 10 ?
O3 Mo2 O5 102.1(3) . 11 ?
O3 Mo2 O5 102.1(3) . 4 ?
O3 Mo2 O5 102.1(3) . 10 ?
O3 Mo2 O5 102.1(3) . . ?
O3 Mo2 O10 158.4(4) . . ?
O3 Mo2 O10 158.4(4) . 11 ?
O5 Mo2 V1 42.6(3) 10 10 ?
O5 Mo2 V1 129.3(3) 4 . ?
O5 Mo2 V1 42.6(3) 4 10 ?
O5 Mo2 V1 129.3(3) 11 10 ?
O5 Mo2 V1 129.3(3) 10 . ?
O5 Mo2 V1 129.3(3) . 10 ?
O5 Mo2 V1 42.6(3) . . ?
O5 Mo2 V1 42.6(3) 11 . ?
O5 Mo2 O5 155.9(7) . 4 ?
O5 Mo2 O5 85.1(6) 4 10 ?
O5 Mo2 O5 155.9(7) 10 11 ?
O5 Mo2 O5 85.1(6) . 11 ?
O5 Mo2 O5 89.9(5) 4 11 ?
O5 Mo2 O5 89.9(5) . 10 ?
O5 Mo2 O10 93.1(5) 4 . ?
O5 Mo2 O10 93.1(5) 10 11 ?
O5 Mo2 O10 63.7(4) . . ?
O5 Mo2 O10 63.7(4) 10 . ?
O5 Mo2 O10 63.7(4) 11 11 ?
O5 Mo2 O10 93.1(5) 11 . ?
O5 Mo2 O10 63.7(4) 4 11 ?
O5 Mo2 O10 93.1(5) . 11 ?
O10 Mo2 V1 76.85(10) . . ?
O10 Mo2 V1 76.85(10) . 10 ?
O10 Mo2 V1 76.85(10) 11 10 ?
O10 Mo2 V1 76.85(10) 11 . ?
O10 Mo2 O10 43.2(8) 11 . ?
O1 Mo3 V1 101.3(3) . . ?
O1 Mo3 O5 100.0(4) . . ?
O1 Mo3 O6 105.5(6) . . ?
O1 Mo3 O8 101.9(5) . . ?
O1 Mo3 O9 158.2(5) . . ?
O1 Mo3 O10 159.2(5) . . ?
O1 Mo3 O2A 91.9(18) . . ?
O5 Mo3 V1 39.9(3) . . ?
O5 Mo3 O9 90.6(4) . . ?
O5 Mo3 O10 63.5(5) . . ?
O5 Mo3 O2A 84.0(13) . . ?
O6 Mo3 V1 125.4(5) . . ?
O6 Mo3 O5 88.6(6) . . ?
O6 Mo3 O8 94.3(7) . . ?
O6 Mo3 O9 93.6(6) . . ?
O6 Mo3 O10 63.6(6) . . ?
O6 Mo3 O2A 162.0(19) . . ?
O8 Mo3 V1 125.3(5) . . ?
O8 Mo3 O5 156.3(6) . . ?
O8 Mo3 O9 65.7(5) . . ?
O8 Mo3 O10 96.8(6) . . ?
O8 Mo3 O2A 86.2(10) . . ?
O9 Mo3 V1 74.9(3) . . ?
O10 Mo3 V1 74.6(4) . . ?
O10 Mo3 O9 41.5(5) . . ?
O2A Mo3 V1 44.3(13) . . ?
O2A Mo3 O9 70.1(16) . . ?
O2A Mo3 O10 98.5(19) . . ?
Mo1 V1 Mo3 74.74(10) . 11 ?
Mo1 V1 Mo3 74.74(10) . . ?
Mo1 V1 V2 74.74(10) . . ?
Mo2 V1 Mo1 118.97(18) . . ?
Mo2 V1 Mo3 75.04(11) . 11 ?
Mo2 V1 Mo3 75.04(11) . . ?
Mo2 V1 V2 75.04(11) . . ?
Mo3 V1 Mo3 118.21(17) 11 . ?
O2B V1 Mo1 38.1(8) . . ?
O2B V1 Mo1 38.1(8) 11 . ?
O2B V1 Mo2 106.6(15) 11 . ?
O2B V1 Mo2 106.6(15) . . ?
O2B V1 V2 39.1(7) . . ?
O2B V1 V2 105.5(16) 11 . ?
O2B V1 O2B 75(2) 11 . ?
O2B V1 O5 126(2) 11 . ?
O2B V1 O5 78.2(9) . . ?
O5 V1 Mo1 109.9(3) 11 . ?
O5 V1 Mo1 109.9(3) . . ?
O5 V1 Mo2 41.0(3) . . ?
O5 V1 Mo2 41.0(3) 11 . ?
O5 V1 Mo3 110.8(3) 11 . ?
O5 V1 Mo3 39.6(3) . . ?
O5 V1 Mo3 39.6(3) 11 11 ?
O5 V1 Mo3 110.8(3) . 11 ?
O5 V1 V2 39.6(3) . . ?
O5 V1 V2 110.8(3) 11 . ?
O5 V1 O5 82.0(5) 11 . ?
O5 V1 O2A 139.2(18) . 11 ?
O5 V1 O2A 139.3(18) 11 . ?
O5 V1 O2A 83.2(11) . . ?
O5 V1 O2A 83.2(11) 11 11 ?
O7 V1 Mo1 122.5(7) . . ?
O7 V1 Mo2 118.5(7) . . ?
O7 V1 Mo3 120.88(9) . 11 ?
O7 V1 Mo3 120.88(9) . . ?
O7 V1 V2 120.88(9) . . ?
O7 V1 O2B 121(2) . . ?
O7 V1 O2B 121(2) . 11 ?
O7 V1 O5 112.7(6) . 11 ?
O7 V1 O5 112.7(6) . . ?
O7 V1 O2A 108.1(19) . 11 ?
O7 V1 O2A 108.0(19) . . ?
O2A V1 Mo1 42.5(9) . . ?
O2A V1 Mo1 42.5(9) 11 . ?
O2A V1 Mo2 116.5(15) . . ?
O2A V1 Mo2 116.5(15) 11 . ?
O2A V1 Mo3 43.8(12) . . ?
O2A V1 Mo3 115.1(13) . 11 ?
O2A V1 Mo3 43.8(12) 11 11 ?
O2A V1 Mo3 115.1(13) 11 . ?
O2A V1 O2A 83.8(15) 11 . ?
O9 P1 O9 108.0(12) 9 2 ?
O9 P1 O9 72.0(12) 9 10 ?
O9 P1 O9 108.0(12) 10 . ?
O9 P1 O9 180.0(12) 10 2 ?
O9 P1 O9 180.0 9 . ?
O9 P1 O9 72.0(12) 2 . ?
O9 P1 O10 110.2(5) 2 3 ?
O9 P1 O10 110.2(5) 10 11 ?
O9 P1 O10 110.2(5) . 9 ?
O9 P1 O10 110.2(5) 2 . ?
O9 P1 O10 110.2(5) . 11 ?
O9 P1 O10 69.8(5) . . ?
O9 P1 O10 69.8(5) 9 11 ?
O9 P1 O10 69.8(5) 9 9 ?
O9 P1 O10 69.8(5) 2 11 ?
O9 P1 O10 110.2(5) 10 9 ?
O9 P1 O10 110.2(5) 9 3 ?
O9 P1 O10 69.8(5) 2 9 ?
O9 P1 O10 110.2(5) 9 . ?
O9 P1 O10 69.8(5) . 3 ?
O9 P1 O10 69.8(5) 10 . ?
O9 P1 O10 69.8(5) 10 3 ?
O10 P1 O10 107.9(14) 9 11 ?
O10 P1 O10 72.1(14) . 11 ?
O10 P1 O10 180.0(13) 11 3 ?
O10 P1 O10 180.0 . 9 ?
O10 P1 O10 107.9(14) . 3 ?
O10 P1 O10 72.1(14) 9 3 ?
O1 V2 V1 101.3(3) . . ?
O1 V2 O2B 104.6(19) . . ?
O1 V2 O5 100.0(4) . . ?
O1 V2 O6 105.5(6) . . ?
O1 V2 O10 159.2(5) . . ?
O2B V2 V1 38.8(8) . . ?
O2B V2 O5 78.2(10) . . ?
O2B V2 O10 85(2) . . ?
O5 V2 V1 39.9(3) . . ?
O5 V2 O10 63.5(5) . . ?
O6 V2 V1 125.4(5) . . ?
O6 V2 O2B 149(2) . . ?
O6 V2 O5 88.6(6) . . ?
O6 V2 O10 63.6(6) . . ?
O10 V2 V1 74.6(4) . . ?
Mo1 O2B V1 101.7(14) . . ?
Mo1 O2B V2 144(3) . . ?
V1 O2B V2 102.1(13) . . ?
Mo2 O5 Mo3 137.2(5) . . ?
Mo2 O5 V1 96.4(4) . . ?
Mo2 O5 V2 137.2(5) . . ?
Mo3 O5 V1 100.5(4) . . ?
V2 O5 V1 100.5(4) . . ?
Mo3 O6 Mo3 143.7(10) . 10 ?
Mo3 O8 Mo3 140.0(9) 12 . ?
Mo3 O9 Mo1 93.2(5) 12 . ?
Mo3 O9 Mo1 93.2(5) . . ?
Mo3 O9 Mo3 88.5(5) 12 . ?
P1 O9 Mo1 123.2(9) . . ?
P1 O9 Mo3 124.5(5) . 12 ?
P1 O9 Mo3 124.5(5) . . ?
P1 O9 O9 54.0(6) . 2 ?
P1 O9 O10 56.1(7) . 3 ?
P1 O9 O10 56.1(7) . . ?
O9 O9 Mo1 69.2(4) 2 . ?
O9 O9 Mo3 133.4(3) 2 . ?
O9 O9 Mo3 133.4(3) 2 12 ?
O10 O9 Mo1 131.1(7) 3 . ?
O10 O9 Mo1 131.1(7) . . ?
O10 O9 Mo3 68.4(6) . . ?
O10 O9 Mo3 68.4(6) 3 12 ?
O10 O9 Mo3 129.1(10) . 12 ?
O10 O9 Mo3 129.1(10) 3 . ?
O10 O9 O9 90.7(8) . 2 ?
O10 O9 O9 90.7(8) 3 2 ?
O10 O9 O10 91.3(11) . 3 ?
Mo3 O10 Mo2 94.0(5) 10 . ?
Mo3 O10 Mo2 94.0(5) . . ?
Mo3 O10 Mo3 89.0(6) 10 . ?
P1 O10 Mo2 122.3(10) . . ?
P1 O10 Mo3 124.2(6) . 10 ?
P1 O10 Mo3 124.2(6) . . ?
P1 O10 V2 124.2(6) . . ?
P1 O10 O9 54.1(7) . . ?
P1 O10 O9 54.1(7) . 10 ?
V2 O10 Mo2 94.0(5) . . ?
O9 O10 Mo2 131.3(7) . . ?
O9 O10 Mo2 131.3(7) 10 . ?
O9 O10 Mo3 70.1(6) 10 10 ?
O9 O10 Mo3 70.1(6) . . ?
O9 O10 Mo3 129.7(11) . 10 ?
O9 O10 Mo3 129.7(11) 10 . ?
O9 O10 V2 70.1(6) . . ?
O9 O10 V2 129.7(11) 10 . ?
O9 O10 O9 88.7(11) 10 . ?
H1A N1 H1B 106.5 . . ?
C3 N1 H1A 106.6 12 . ?
C3 N1 H1A 106.6 . . ?
C3 N1 H1B 106.6 . . ?
C3 N1 H1B 106.6 12 . ?
C3 N1 C3 123(2) 12 . ?
C2 C1 C1 121.7(10) 12 10_556 ?
C2 C1 C1 121.7(10) . 10_556 ?
C2 C1 C2 116.6(19) . 12 ?
N1 C3 H3 120.3 . . ?
N1 C3 C2 119.5(16) . . ?
C2 C3 H3 120.3 . . ?
C1 C2 H2 119.7 . . ?
C3 C2 C1 120.5(16) . . ?
C3 C2 H2 119.7 . . ?
Mo1 O2A Mo3 125(3) . . ?
Mo1 O2A V1 92(2) . . ?
Mo3 O2A V1 92(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mo1 O9 O10 Mo2 -3(2) . . . . ?
Mo1 O9 O10 Mo3 74.7(11) . . . . ?
Mo1 O9 O10 Mo3 145.7(8) . . . 10 ?
Mo1 O9 O10 P1 -106.8(12) . . . . ?
Mo1 O9 O10 V2 74.7(11) . . . . ?
Mo1 O9 O10 O9 -151.8(5) . . . 10 ?
Mo3 O9 O10 Mo2 -146.4(9) 12 . . . ?
Mo3 O9 O10 Mo2 -77.3(11) . . . . ?
Mo3 O9 O10 Mo3 -69.1(8) 12 . . . ?
Mo3 O9 O10 Mo3 1.9(16) 12 . . 10 ?
Mo3 O9 O10 Mo3 71.0(9) . . . 10 ?
Mo3 O9 O10 P1 178.6(7) . . . . ?
Mo3 O9 O10 P1 109.5(10) 12 . . . ?
Mo3 O9 O10 O9 133.5(9) . . . 10 ?
Mo3 O9 O10 O9 64.4(14) 12 . . 10 ?
V1 Mo1 O2B V1 142.2(10) 2 . . . ?
V1 Mo1 O2B V2 11(7) 2 . . . ?
V1 Mo3 O6 Mo3 -41.1(19) . . . 10 ?
V1 Mo3 O8 Mo3 50.9(15) . . . 12 ?
P1 O9 O10 Mo2 104.1(13) . . . . ?
P1 O9 O10 Mo3 -178.6(7) . . . . ?
P1 O9 O10 Mo3 -107.6(9) . . . 10 ?
P1 O9 O10 V2 -178.6(7) . . . . ?
P1 O9 O10 O9 -45.1(9) . . . 10 ?
O1 Mo3 O6 Mo3 -157.6(15) . . . 10 ?
O1 Mo3 O8 Mo3 164.1(12) . . . 12 ?
O2B Mo1 O2B V1 13(4) 11 . . . ?
O2B Mo1 O2B V1 88(2) 2 . . . ?
O2B Mo1 O2B V1 159.1(4) 12 . . . ?
O2B Mo1 O2B V2 -43(5) 2 . . . ?
O2B Mo1 O2B V2 28(7) 12 . . . ?
O2B Mo1 O2B V2 -118(4) 11 . . . ?
O4 Mo1 O2B V1 -92(2) . . . . ?
O4 Mo1 O2B V2 137(5) . . . . ?
O5 Mo3 O6 Mo3 -57.7(16) . . . 10 ?
O5 Mo3 O8 Mo3 7(2) . . . 12 ?
O6 Mo3 O8 Mo3 -89.0(14) . . . 12 ?
O8 Mo3 O6 Mo3 98.7(17) . . . 10 ?
O9 Mo1 O2B V1 106(3) . . . . ?
O9 Mo1 O2B V1 73(2) 2 . . . ?
O9 Mo1 O2B V2 -59(5) 2 . . . ?
O9 Mo1 O2B V2 -25(4) . . . . ?
O9 Mo3 O6 Mo3 32.9(17) . . . 10 ?
O9 Mo3 O8 Mo3 3.1(12) . . . 12 ?
O9 P1 O9 Mo1 0.000(0) 2 . . . ?
O9 P1 O9 Mo1 180.0 10 . . . ?
O9 P1 O9 Mo3 57.9(7) 10 . . . ?
O9 P1 O9 Mo3 -57.9(7) 10 . . 12 ?
O9 P1 O9 Mo3 -122.1(7) 2 . . . ?
O9 P1 O9 Mo3 122.1(7) 2 . . 12 ?
O9 P1 O9 O9 180.0 10 . . 2 ?
O9 P1 O9 O10 -120.5(7) 2 . . . ?
O9 P1 O9 O10 120.5(7) 2 . . 3 ?
O9 P1 O9 O10 -59.5(7) 10 . . 3 ?
O9 P1 O9 O10 59.5(7) 10 . . . ?
O9 P1 O10 Mo2 -59.6(6) 2 . . . ?
O9 P1 O10 Mo2 59.6(6) 9 . . . ?
O9 P1 O10 Mo2 120.4(6) 10 . . . ?
O9 P1 O10 Mo2 -120.4(6) . . . . ?
O9 P1 O10 Mo3 -1.6(8) 10 . . 10 ?
O9 P1 O10 Mo3 -117.5(12) 10 . . . ?
O9 P1 O10 Mo3 62.5(12) 2 . . . ?
O9 P1 O10 Mo3 178.4(8) 2 . . 10 ?
O9 P1 O10 Mo3 1.6(8) . . . . ?
O9 P1 O10 Mo3 117.5(12) . . . 10 ?
O9 P1 O10 Mo3 -178.4(8) 9 . . . ?
O9 P1 O10 Mo3 -62.5(12) 9 . . 10 ?
O9 P1 O10 V2 -178.4(8) 9 . . . ?
O9 P1 O10 V2 1.6(8) . . . . ?
O9 P1 O10 V2 -117.5(12) 10 . . . ?
O9 P1 O10 V2 62.5(12) 2 . . . ?
O9 P1 O10 O9 119.1(12) . . . 10 ?
O9 P1 O10 O9 60.9(12) 2 . . . ?
O9 P1 O10 O9 179.998(0) 9 . . . ?
O9 P1 O10 O9 -119.1(12) 10 . . . ?
O9 P1 O10 O9 180.0 2 . . 10 ?
O9 P1 O10 O9 -60.9(12) 9 . . 10 ?
O9 O9 O10 Mo2 59.9(11) 2 . . . ?
O9 O9 O10 Mo3 137.2(3) 2 . . . ?
O9 O9 O10 Mo3 -151.8(8) 2 . . 10 ?
O9 O9 O10 P1 -44.2(5) 2 . . . ?
O9 O9 O10 V2 137.2(3) 2 . . . ?
O9 O9 O10 O9 -89.3(8) 2 . . 10 ?
O10 Mo3 O6 Mo3 3.3(14) . . . 10 ?
O10 Mo3 O8 Mo3 -25.1(14) . . . 12 ?
O10 P1 O9 Mo1 120.5(7) . . . . ?
O10 P1 O9 Mo1 -120.5(7) 3 . . . ?
O10 P1 O9 Mo1 59.5(7) 11 . . . ?
O10 P1 O9 Mo1 -59.5(7) 9 . . . ?
O10 P1 O9 Mo3 62.6(11) 9 . . 12 ?
O10 P1 O9 Mo3 1.6(8) 3 . . 12 ?
O10 P1 O9 Mo3 117.4(11) 3 . . . ?
O10 P1 O9 Mo3 -62.6(11) 11 . . . ?
O10 P1 O9 Mo3 -117.4(11) . . . 12 ?
O10 P1 O9 Mo3 -1.6(8) . . . . ?
O10 P1 O9 Mo3 178.4(8) 9 . . . ?
O10 P1 O9 Mo3 -178.4(8) 11 . . 12 ?
O10 P1 O9 O9 120.5(7) . . . 2 ?
O10 P1 O9 O9 -120.5(7) 3 . . 2 ?
O10 P1 O9 O9 -59.5(7) 9 . . 2 ?
O10 P1 O9 O9 59.5(7) 11 . . 2 ?
O10 P1 O9 O10 180.000(0) 9 . . . ?
O10 P1 O9 O10 61.0(13) 9 . . 3 ?
O10 P1 O9 O10 180.000(0) 11 . . 3 ?
O10 P1 O9 O10 -61.0(13) 11 . . . ?
O10 P1 O9 O10 119.0(13) 3 . . . ?
O10 P1 O9 O10 -119.0(13) . . . 3 ?
O10 P1 O10 Mo2 180.0 3 . . . ?
O10 P1 O10 Mo2 0.0 11 . . . ?
O10 P1 O10 Mo3 122.0(8) 11 . . . ?
O10 P1 O10 Mo3 58.0(8) 3 . . 10 ?
O10 P1 O10 Mo3 -122.0(8) 11 . . 10 ?
O10 P1 O10 Mo3 -58.0(8) 3 . . . ?
O10 P1 O10 V2 122.0(8) 11 . . . ?
O10 P1 O10 V2 -58.0(8) 3 . . . ?
O10 P1 O10 O9 -120.4(6) 11 . . 10 ?
O10 P1 O10 O9 -59.6(6) 3 . . . ?
O10 P1 O10 O9 120.4(6) 11 . . . ?
O10 P1 O10 O9 59.6(6) 3 . . 10 ?
O10 O9 O10 Mo2 150.7(5) 3 . . . ?
O10 O9 O10 Mo3 -61.0(15) 3 . . 10 ?
O10 O9 O10 Mo3 -132.0(8) 3 . . . ?
O10 O9 O10 P1 46.6(10) 3 . . . ?
O10 O9 O10 V2 -132.0(8) 3 . . . ?
O10 O9 O10 O9 1.5(16) 3 . . 10 ?
N1 C3 C2 C1 4(3) . . . . ?
C1 C1 C2 C3 176.5(14) 10_556 . . . ?
C3 N1 C3 C2 -2(4) 12 . . . ?
C2 C1 C2 C3 -5(4) 12 . . . ?
O2A Mo3 O6 Mo3 8(4) . . . 10 ?
O2A Mo3 O8 Mo3 73(2) . . . 12 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.012 0.500 303.8 100.2 '0.5 C10N2H10,5 H2O'
2 0.500 -0.852 0.000 303.8 100.2 '0.5 C10N2H10,5 H2O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
