# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1478107'
_audit_update_record             
;
2017-06-05 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_audit_creation_date             2017-06-04
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'4(C4 H16 Cu N4 2+), 2(C4 H20 Cu N4 O2 2+), Nb12 O42 P V2 10-, 2(O H 1-), 11(H2 O)'
_chemical_formula_sum            'C24 H128 Cu6 N24 Nb12 O59 P V2'
_chemical_formula_weight         3326.51
_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'
Cu Cu 0.3201 1.2651 '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'
Nb Nb -2.0727 0.6215 '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'

_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           128
_space_group_name_H-M_alt        'P 4/m n c'
_space_group_name_Hall           '-P 4 2n'
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                   14.5498(3)
_cell_length_b                   14.5498(3)
_cell_length_c                   22.9484(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4858.1(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9005
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.800
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.939
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0769 before and 0.0547 after correction. The Ratio of minimum to maximum transmission is 0.8985. The λ/2 correction factor is 0.00150.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.274
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3278
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0657
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48594
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.657
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2023
_reflns_number_total             2563
_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 v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.792
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2563
_refine_ls_number_restraints     138
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0489
_refine_ls_restrained_S_all      1.105
_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)+(0.0398P)²+40.1219P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1216
_refine_special_details          
;
The structure contained large void, and the solvent and the negative 
ions located in the void couldn't be identified as 
they were highly disordered, thus it has small residual peaks. Therefore, 
SQUEEZE in PLATON program was performed to remove the highly 
disordered solvent and ions. The numbers of masked ions and 
solvent molecules were confirmed by TG analysis. After calculation, 
the ions and solvent molecules were added in the
 _chemical_formula_moiety, _chemical_formula_sum 
and other relative items.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N4-C4 = C3-N3
 1.4 with sigma of 0.02
 C4-C3
 1.5 with sigma of 0.02
 N4-C3 = C4-N3
 2.4 with sigma of 0.02
 C2A-N2 = N2-C2
 1.4 with sigma of 0.02
 C1-N1 = N1-C1A
 1.4 with sigma of 0.02
 C2A-C1A = C2-C1
 1.5 with sigma of 0.02
 H13B-O12_$2
 2.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C1A) \\sim Ueq, Uanis(C2A)
\\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N1) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C3, Cu2, N4, N3, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, Cu1, N1, N2, C2A, C1A, C2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O13, Cu2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H1BC)=Sof(H1BD)=Sof(H2BD)=Sof(H2BC)=Sof(C2A)=Sof(H2AC)=Sof(H2AD)=Sof(C1A)=
 Sof(H1AC)=Sof(H1AD)=1-FVAR(1)
 Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H1AA)=Sof(H1AB)=
 Sof(H2AA)=Sof(H2AB)=FVAR(1)
 Fixed Sof: O3(0.5) N4(0.5) H4A(0.5) H4B(0.5) N3(0.5) H3A(0.5) H3B(0.5)
 C4(0.5) H4C(0.5) H4D(0.5) C3(0.5) H3C(0.5) H3D(0.5) O13(0.5) H13A(0.5)
 H13B(0.5)
6.a Rotating group:
 O13(H13A,H13B)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), N1(H1AA,H1AB), N1(H1BC,H1BD), N2(H2AA,H2AB),
 N2(H2BD,H2BC), N4(H4A,H4B), N3(H3A,H3B), C4(H4C,H4D), C3(H3C,H3D), C2A(H2AC,
 H2AD), C1A(H1AC,H1AD)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
C1 C 0.1717(18) 0.8011(18) 0.3570(13) 0.152(8) Uani 0.71(4) 1 d D U . A 1
H1A H 0.214809 0.853190 0.352146 0.183 Uiso 0.71(4) 1 calc R . . A 1
H1B H 0.154633 0.796016 0.398676 0.183 Uiso 0.71(4) 1 calc R . . A 1
C2 C 0.0865(19) 0.813(3) 0.3188(8) 0.161(8) Uani 0.71(4) 1 d D U . A 1
H2A H 0.040192 0.765836 0.328266 0.194 Uiso 0.71(4) 1 calc R . . A 1
H2B H 0.058829 0.874595 0.325617 0.194 Uiso 0.71(4) 1 calc R . . A 1
Cu1 Cu 0.21323(11) 0.71323(11) 0.250000 0.1079(8) Uani 1 2 d S TU P A .
Cu2 Cu 0.000000 0.500000 0.000000 0.0722(7) Uani 1 4 d S TU P . .
N1 N 0.2124(9) 0.7153(9) 0.3358(5) 0.144(4) Uani 1 1 d D U . . .
H1AA H 0.179457 0.666707 0.349463 0.172 Uiso 0.71(4) 1 calc R . . A 1
H1AB H 0.270944 0.710141 0.349393 0.172 Uiso 0.71(4) 1 calc R . . A 1
H1BC H 0.203277 0.657257 0.349375 0.172 Uiso 0.29(4) 1 calc R . . A 2
H1BD H 0.268160 0.734812 0.348868 0.172 Uiso 0.29(4) 1 calc R . . A 2
N2 N 0.1151(10) 0.8048(9) 0.2588(6) 0.162(5) Uani 1 1 d D U . . .
H2AA H 0.135506 0.860282 0.245737 0.194 Uiso 0.71(4) 1 calc R . . A 1
H2AB H 0.066076 0.788110 0.236573 0.194 Uiso 0.71(4) 1 calc R . . A 1
H2BD H 0.115800 0.845921 0.228874 0.194 Uiso 0.29(4) 1 calc R . . A 2
H2BC H 0.058926 0.777509 0.260367 0.194 Uiso 0.29(4) 1 calc R . . A 2
Nb1 Nb 0.03098(4) 0.18181(4) 0.10728(3) 0.03835(19) Uani 1 1 d . . . . .
Nb2 Nb 0.20875(5) 0.14793(5) 0.000000 0.0369(2) Uani 1 2 d S T P . .
O2 O 0.1015(4) 0.0715(3) 0.1430(2) 0.0572(14) Uani 1 1 d . . . . .
O3 O -0.0523(5) 0.0721(5) 0.0395(3) 0.0285(17) Uani 0.5 1 d . . . . .
O5 O -0.0547(4) 0.2411(4) 0.0591(3) 0.079(2) Uani 1 1 d . . . . .
O8 O 0.1337(5) 0.2070(4) 0.0589(3) 0.083(2) Uani 1 1 d . . . . .
O10 O 0.000000 0.000000 0.2470(5) 0.063(3) Uani 1 4 d S T P . .
O11 O 0.0446(5) 0.2607(4) 0.1644(3) 0.0736(19) Uani 1 1 d . . . . .
O12 O 0.3081(5) 0.2149(5) 0.000000 0.067(3) Uani 1 2 d DS T P . .
P1 P 0.000000 0.000000 0.000000 0.0151(7) Uani 1 8 d S T P . .
V5 V 0.000000 0.000000 0.17535(10) 0.0401(5) Uani 1 4 d S T P . .
N4 N -0.0796(8) 0.6069(8) 0.0233(7) 0.087(7) Uani 0.5 1 d D U . B -1
H4A H -0.071612 0.619929 0.061746 0.105 Uiso 0.5 1 calc R . . B -1
H4B H -0.064338 0.657622 0.002164 0.105 Uiso 0.5 1 calc R . . B -1
N3 N -0.1093(11) 0.4680(9) -0.0515(8) 0.078(4) Uani 0.5 1 d D U . B -1
H3A H -0.090183 0.460431 -0.088948 0.094 Uiso 0.5 1 calc R . . B -1
H3B H -0.134876 0.414250 -0.039269 0.094 Uiso 0.5 1 calc R . . B -1
C4 C -0.1726(10) 0.5817(11) 0.0123(10) 0.097(8) Uani 0.5 1 d D U . B -1
H4C H -0.212916 0.636411 0.014924 0.116 Uiso 0.5 1 calc R . . B -1
H4D H -0.193511 0.536019 0.041387 0.116 Uiso 0.5 1 calc R . . B -1
C3 C -0.1768(14) 0.5410(14) -0.0486(10) 0.111(8) Uani 0.5 1 d D U . B -1
H3C H -0.238951 0.516313 -0.056466 0.133 Uiso 0.5 1 calc R . . B -1
H3D H -0.162857 0.588765 -0.078032 0.133 Uiso 0.5 1 calc R . . B -1
O13 O -0.0689(16) 0.4283(14) 0.0900(10) 0.136(6) Uani 0.5 1 d . U . B -2
H13A H -0.024243 0.400096 0.114114 0.205 Uiso 0.5 1 d GR . . B -2
H13B H -0.112070 0.381819 0.081083 0.205 Uiso 0.5 1 d DGR . . B -2
C2A C 0.137(6) 0.848(3) 0.3127(15) 0.135(9) Uani 0.29(4) 1 d D U . A 2
H2AC H 0.088996 0.893418 0.323235 0.162 Uiso 0.29(4) 1 calc R . . A 2
H2AD H 0.196629 0.880989 0.309591 0.162 Uiso 0.29(4) 1 calc R . . A 2
C1A C 0.143(4) 0.774(4) 0.358(3) 0.139(9) Uani 0.29(4) 1 d D U . A 2
H1AC H 0.160759 0.799301 0.396730 0.167 Uiso 0.29(4) 1 calc R . . A 2
H1AD H 0.083744 0.740838 0.362295 0.167 Uiso 0.29(4) 1 calc R . . A 2


_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
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.529(18) . ?
C1 N1 1.465(17) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 N2 1.445(17) . ?
Cu1 N1 1.970(12) 7_455 ?
Cu1 N1 1.970(12) . ?
Cu1 N2 1.963(12) . ?
Cu1 N2 1.963(12) 7_455 ?
Cu2 N4 2.011(12) . ?
Cu2 N3 2.035(16) . ?
Cu2 O13 2.52(2) 10 ?
Cu2 O13 2.52(2) . ?
N1 H1AA 0.9100 . ?
N1 H1AB 0.9100 . ?
N1 H1BC 0.9100 . ?
N1 H1BD 0.9100 . ?
N1 C1A 1.42(2) . ?
N2 H2AA 0.9100 . ?
N2 H2AB 0.9100 . ?
N2 H2BD 0.9100 . ?
N2 H2BC 0.9100 . ?
N2 C2A 1.43(2) . ?
Nb1 O2 2.064(5) 3 ?
Nb1 O2 2.075(5) . ?
Nb1 O3 2.537(7) . ?
Nb1 O3 2.516(8) 4 ?
Nb1 O5 1.877(6) . ?
Nb1 O8 1.897(6) . ?
Nb1 O11 1.755(5) . ?
Nb1 V5 3.1050(13) . ?
Nb2 O5 1.974(6) 4 ?
Nb2 O5 1.974(6) 11 ?
Nb2 O8 1.939(6) 10 ?
Nb2 O8 1.939(6) . ?
Nb2 O12 1.744(7) . ?
O2 V5 1.953(5) . ?
O3 O3 1.813(16) 10 ?
O3 P1 1.581(7) . ?
O10 V5 1.644(11) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 C4 1.425(15) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 C3 1.449(16) . ?
C4 H4C 0.9900 . ?
C4 H4D 0.9900 . ?
C4 C3 1.520(18) . ?
C3 H3C 0.9900 . ?
C3 H3D 0.9900 . ?
O13 H13A 0.9470 . ?
O13 H13B 0.9455 . ?
C2A H2AC 0.9900 . ?
C2A H2AD 0.9900 . ?
C2A C1A 1.51(2) . ?
C1A H1AC 0.9900 . ?
C1A H1AD 0.9900 . ?

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
H1A C1 H1B 109.0 . . ?
C2 C1 H1A 111.0 . . ?
C2 C1 H1B 111.0 . . ?
N1 C1 H1A 111.0 . . ?
N1 C1 H1B 111.0 . . ?
N1 C1 C2 103.7(19) . . ?
C1 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
H2A C2 H2B 108.5 . . ?
N2 C2 C1 108(2) . . ?
N2 C2 H2A 110.2 . . ?
N2 C2 H2B 110.2 . . ?
N1 Cu1 N1 179.2(9) . 7_455 ?
N2 Cu1 N1 83.3(5) . . ?
N2 Cu1 N1 83.3(5) 7_455 7_455 ?
N2 Cu1 N1 96.8(5) 7_455 . ?
N2 Cu1 N1 96.8(5) . 7_455 ?
N2 Cu1 N2 176.1(9) . 7_455 ?
N4 Cu2 N3 83.2(5) . . ?
N4 Cu2 O13 108.0(7) . 10 ?
N3 Cu2 O13 28.2(6) . 10 ?
O13 Cu2 O13 110.0(10) 10 . ?
C1 N1 Cu1 110.4(14) . . ?
C1 N1 H1AA 109.6 . . ?
C1 N1 H1AB 109.6 . . ?
Cu1 N1 H1AA 109.6 . . ?
Cu1 N1 H1AB 109.6 . . ?
Cu1 N1 H1BC 109.2 . . ?
Cu1 N1 H1BD 109.2 . . ?
H1AA N1 H1AB 108.1 . . ?
H1BC N1 H1BD 107.9 . . ?
C1A N1 Cu1 112(3) . . ?
C1A N1 H1BC 109.2 . . ?
C1A N1 H1BD 109.2 . . ?
C2 N2 Cu1 111.4(13) . . ?
C2 N2 H2AA 109.3 . . ?
C2 N2 H2AB 109.3 . . ?
Cu1 N2 H2AA 109.3 . . ?
Cu1 N2 H2AB 109.3 . . ?
Cu1 N2 H2BD 111.1 . . ?
Cu1 N2 H2BC 111.1 . . ?
H2AA N2 H2AB 108.0 . . ?
H2BD N2 H2BC 109.1 . . ?
C2A N2 Cu1 103(3) . . ?
C2A N2 H2BD 111.1 . . ?
C2A N2 H2BC 111.1 . . ?
O2 Nb1 O2 76.2(3) 3 . ?
O2 Nb1 O3 89.5(2) . . ?
O2 Nb1 O3 62.8(2) 3 . ?
O2 Nb1 O3 89.6(2) 3 4 ?
O2 Nb1 O3 63.1(2) . 4 ?
O2 Nb1 V5 38.10(14) 3 . ?
O2 Nb1 V5 38.15(14) . . ?
O3 Nb1 O3 42.5(3) 4 . ?
O3 Nb1 V5 72.72(18) . . ?
O3 Nb1 V5 72.98(18) 4 . ?
O5 Nb1 O2 90.8(2) . 3 ?
O5 Nb1 O2 156.6(3) . . ?
O5 Nb1 O3 97.9(3) . 4 ?
O5 Nb1 O3 67.1(3) . . ?
O5 Nb1 O8 95.1(3) . . ?
O5 Nb1 V5 126.26(16) . . ?
O8 Nb1 O2 89.5(2) . . ?
O8 Nb1 O2 155.6(3) . 3 ?
O8 Nb1 O3 66.2(3) . 4 ?
O8 Nb1 O3 98.0(3) . . ?
O8 Nb1 V5 124.97(17) . . ?
O11 Nb1 O2 98.9(3) . . ?
O11 Nb1 O2 98.9(3) . 3 ?
O11 Nb1 O3 157.8(3) . 4 ?
O11 Nb1 O3 157.6(3) . . ?
O11 Nb1 O5 102.4(3) . . ?
O11 Nb1 O8 102.8(3) . . ?
O11 Nb1 V5 101.4(2) . . ?
O5 Nb2 O5 86.7(4) 11 4 ?
O8 Nb2 O5 87.7(2) . 4 ?
O8 Nb2 O5 156.5(3) 10 4 ?
O8 Nb2 O5 156.5(3) . 11 ?
O8 Nb2 O5 87.7(2) 10 11 ?
O8 Nb2 O8 88.4(4) 10 . ?
O12 Nb2 O5 100.7(3) . 4 ?
O12 Nb2 O5 100.7(3) . 11 ?
O12 Nb2 O8 102.7(3) . 10 ?
O12 Nb2 O8 102.7(3) . . ?
Nb1 O2 Nb1 133.0(3) 4 . ?
V5 O2 Nb1 100.8(2) . . ?
V5 O2 Nb1 101.2(2) . 4 ?
Nb1 O3 Nb1 97.4(3) 3 . ?
O3 O3 Nb1 127.82(18) 10 . ?
O3 O3 Nb1 128.19(18) 10 3 ?
P1 O3 Nb1 123.9(4) . 3 ?
P1 O3 Nb1 122.6(4) . . ?
P1 O3 O3 55.0(3) . 10 ?
Nb1 O5 Nb2 138.7(4) . 3 ?
Nb1 O8 Nb2 140.0(4) . . ?
O3 P1 O3 109.2(3) 4 10 ?
O3 P1 O3 109.2(3) 3 10 ?
O3 P1 O3 180.0 9 . ?
O3 P1 O3 70.8(3) 4 2 ?
O3 P1 O3 109.2(3) 12 . ?
O3 P1 O3 109.2(3) 11 2 ?
O3 P1 O3 70.8(3) 3 . ?
O3 P1 O3 70.8(3) 12 10 ?
O3 P1 O3 109.2(3) 12 2 ?
O3 P1 O3 180.0(8) 12 4 ?
O3 P1 O3 70.0(6) 9 2 ?
O3 P1 O3 70.8(3) 12 9 ?
O3 P1 O3 70.8(3) 3 2 ?
O3 P1 O3 109.2(3) 4 9 ?
O3 P1 O3 70.0(6) 10 . ?
O3 P1 O3 110.0(6) 9 10 ?
O3 P1 O3 70.8(3) 11 10 ?
O3 P1 O3 70.0(6) 4 11 ?
O3 P1 O3 180.0(8) 2 10 ?
O3 P1 O3 70.8(3) 9 11 ?
O3 P1 O3 70.8(3) 4 . ?
O3 P1 O3 70.0(6) 12 3 ?
O3 P1 O3 109.2(3) 11 . ?
O3 P1 O3 110.0(6) 4 3 ?
O3 P1 O3 110.0(6) 2 . ?
O3 P1 O3 109.2(3) 9 3 ?
O3 P1 O3 180.0(8) 11 3 ?
O3 P1 O3 110.0(6) 12 11 ?
Nb1 V5 Nb1 119.59(8) . 2 ?
Nb1 V5 Nb1 75.34(3) 2 3 ?
Nb1 V5 Nb1 75.34(3) . 3 ?
Nb1 V5 Nb1 75.34(3) . 4 ?
Nb1 V5 Nb1 119.59(8) 3 4 ?
Nb1 V5 Nb1 75.34(3) 2 4 ?
O2 V5 Nb1 112.10(18) 3 2 ?
O2 V5 Nb1 112.10(18) 2 4 ?
O2 V5 Nb1 40.70(15) 4 2 ?
O2 V5 Nb1 111.87(17) 2 . ?
O2 V5 Nb1 111.87(17) 3 4 ?
O2 V5 Nb1 40.70(15) 2 3 ?
O2 V5 Nb1 41.02(15) 2 2 ?
O2 V5 Nb1 112.10(18) 4 . ?
O2 V5 Nb1 41.02(15) 4 4 ?
O2 V5 Nb1 40.70(15) 3 . ?
O2 V5 Nb1 40.70(15) . 4 ?
O2 V5 Nb1 112.10(18) . 3 ?
O2 V5 Nb1 41.02(15) . . ?
O2 V5 Nb1 111.87(17) 4 3 ?
O2 V5 Nb1 41.02(15) 3 3 ?
O2 V5 Nb1 111.87(17) . 2 ?
O2 V5 O2 81.72(13) 4 . ?
O2 V5 O2 81.72(13) 2 3 ?
O2 V5 O2 135.4(4) 2 . ?
O2 V5 O2 81.72(13) 3 . ?
O2 V5 O2 135.4(4) 4 3 ?
O2 V5 O2 81.72(13) 2 4 ?
O10 V5 Nb1 120.20(4) . . ?
O10 V5 Nb1 120.21(4) . 3 ?
O10 V5 Nb1 120.21(4) . 4 ?
O10 V5 Nb1 120.21(4) . 2 ?
O10 V5 O2 112.31(18) . 3 ?
O10 V5 O2 112.31(18) . 4 ?
O10 V5 O2 112.31(18) . . ?
O10 V5 O2 112.31(18) . 2 ?
Cu2 N4 H4A 110.2 . . ?
Cu2 N4 H4B 110.2 . . ?
H4A N4 H4B 108.5 . . ?
C4 N4 Cu2 107.5(9) . . ?
C4 N4 H4A 110.2 . . ?
C4 N4 H4B 110.2 . . ?
Cu2 N3 H3A 109.8 . . ?
Cu2 N3 H3B 109.8 . . ?
H3A N3 H3B 108.2 . . ?
C3 N3 Cu2 109.6(10) . . ?
C3 N3 H3A 109.8 . . ?
C3 N3 H3B 109.8 . . ?
N4 C4 H4C 110.2 . . ?
N4 C4 H4D 110.2 . . ?
N4 C4 C3 107.5(14) . . ?
H4C C4 H4D 108.5 . . ?
C3 C4 H4C 110.2 . . ?
C3 C4 H4D 110.2 . . ?
N3 C3 C4 107.5(14) . . ?
N3 C3 H3C 110.2 . . ?
N3 C3 H3D 110.2 . . ?
C4 C3 H3C 110.2 . . ?
C4 C3 H3D 110.2 . . ?
H3C C3 H3D 108.5 . . ?
Cu2 O13 H13A 112.6 . . ?
Cu2 O13 H13B 112.5 . . ?
H13A O13 H13B 105.8 . . ?
N2 C2A H2AC 110.3 . . ?
N2 C2A H2AD 110.3 . . ?
N2 C2A C1A 107(4) . . ?
H2AC C2A H2AD 108.5 . . ?
C1A C2A H2AC 110.3 . . ?
C1A C2A H2AD 110.3 . . ?
N1 C1A C2A 103(4) . . ?
N1 C1A H1AC 111.3 . . ?
N1 C1A H1AD 111.3 . . ?
C2A C1A H1AC 111.3 . . ?
C2A C1A H1AD 111.3 . . ?
H1AC C1A H1AD 109.2 . . ?

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
C1 C2 N2 Cu1 36(4) . . . . ?
C2 C1 N1 Cu1 45(3) . . . . ?
Cu1 N1 C1A C2A -32(6) . . . . ?
Cu1 N2 C2A C1A -56(6) . . . . ?
Cu2 N4 C4 C3 -47.6(17) . . . . ?
Cu2 N3 C3 C4 -33(2) . . . . ?
N1 C1 C2 N2 -51(4) . . . . ?
N2 C2A C1A N1 59(8) . . . . ?
Nb1 O3 P1 O3 55.9(2) 3 . . 12 ?
Nb1 O3 P1 O3 -116.1(4) . . . 10 ?
Nb1 O3 P1 O3 -64.0(4) 3 . . 2 ?
Nb1 O3 P1 O3 -124.1(2) 3 . . 4 ?
Nb1 O3 P1 O3 116.0(4) 3 . . 10 ?
Nb1 O3 P1 O3 3.7(5) . . . 4 ?
Nb1 O3 P1 O3 124.04(18) . . . 3 ?
Nb1 O3 P1 O3 176.2(6) 3 . . 11 ?
Nb1 O3 P1 O3 63.9(4) . . . 2 ?
Nb1 O3 P1 O3 -55.96(18) . . . 11 ?
Nb1 O3 P1 O3 -3.8(6) 3 . . 3 ?
Nb1 O3 P1 O3 -176.3(5) . . . 12 ?
O2 Nb1 O5 Nb2 -56.0(6) 3 . . 3 ?
O2 Nb1 O5 Nb2 -0.3(11) . . . 3 ?
O2 Nb1 O8 Nb2 58.1(6) . . . . ?
O2 Nb1 O8 Nb2 4.7(11) 3 . . . ?
O3 Nb1 O5 Nb2 33.7(6) 4 . . 3 ?
O3 Nb1 O5 Nb2 3.8(5) . . . 3 ?
O3 Nb1 O8 Nb2 -31.3(6) . . . . ?
O3 Nb1 O8 Nb2 -2.5(5) 4 . . . ?
O3 O3 P1 O3 -119.83(18) 10 . . 3 ?
O3 O3 P1 O3 60.17(18) 10 . . 11 ?
O3 O3 P1 O3 -60.17(18) 10 . . 12 ?
O3 O3 P1 O3 119.83(18) 10 . . 4 ?
O3 O3 P1 O3 180.0 10 . . 2 ?
O5 Nb1 O8 Nb2 -98.8(6) . . . . ?
O8 Nb1 O5 Nb2 100.3(6) . . . 3 ?
O11 Nb1 O5 Nb2 -155.3(6) . . . 3 ?
O11 Nb1 O8 Nb2 157.2(6) . . . . ?
V5 Nb1 O5 Nb2 -40.9(7) . . . 3 ?
V5 Nb1 O8 Nb2 43.1(7) . . . . ?
N4 C4 C3 N3 54(2) . . . . ?

_shelx_SHELXL_version_number     2016/6
_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_2
_database_code_depnum_ccdc_archive 'CCDC 1478108'
_audit_update_record             
;
2017-06-05 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
_audit_creation_date             2017-06-03
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'(Nb12 O42 P V2 H2.5 7.5-), 2(C6 H24 Co N6 3+), [Co (C2 N2 H8)2 (H2 O)2, 3+]0.5, 20(H2 O)'
_chemical_formula_sum            'C14 H100.50 Co2.50 N14 Nb12 O63 P V2'
_chemical_formula_weight         2868.67
_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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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'

_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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.8884(4)
_cell_length_b                   14.1118(5)
_cell_length_c                   14.5289(5)
_cell_angle_alpha                93.4430(10)
_cell_angle_beta                 105.1070(10)
_cell_angle_gamma                117.0460(10)
_cell_volume                     2222.65(13)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    7326
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.94
_cell_measurement_theta_min      2.44
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.256
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_primary    'light yellow'
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1407
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0347
_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       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22166
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         1.656
_diffrn_ambient_temperature      293.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6012
_reflns_number_total             8414
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         2.290
_refine_diff_density_min         -2.468
_refine_diff_density_rms         0.187
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         8414
_refine_ls_number_restraints     627
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0635
_refine_ls_restrained_S_all      1.065
_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)+(0.0934P)²+23.7442P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1704
_refine_ls_wR_factor_ref         0.1965
_refine_special_details          
;
The structure contained large void, and the solvent and the positive 
ions located in the void couldnï?1/2ï?1/2t be identified as 
they were highly disordered, thus it had small residual peaks. Therefore, 
SQUEEZE in PLATON program was performed to remove the highly 
disordered solvent and ions. The numbers of masked ions and 
solvent molecules were confirmed by TG analysis. After calculation, 
the ions and solvent molecules were added in the
 _chemical_formula_moiety, _chemical_formula_sum 
and other relative items. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O1P(0.5) O2P(0.5) O3P(0.5) O4P(0.5) Co2(0.25) O1W(0.5) H1WA(0.5)
 H1WB(0.5) N7(0.5) H7A(0.5) H7B(0.5) N8(0.5) H8A(0.5) H8B(0.5) C7(0.5) H7C(0.5)
 H7D(0.5) C8(0.5) H8C(0.5) H8D(0.5) O3W(0.5) H3WA(0.5) H3WB(0.5) O4W(0.5)
 H4WA(0.5) H4WB(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
4.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 C1(H1C,H1D), C2(H2C,H2D), C3(H3C,H3D), C4(H4C,H4D), C5(H5C,H5D), C6(H6C,H6D),
 N7(H7A,H7B), N8(H8A,H8B), C7(H7C,H7D), C8(H8C,H8D)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Nb1 Nb 0.47375(6) 0.23559(6) 0.02001(6) 0.0301(2) Uani 1 1 d . U . . .
Nb2 Nb 0.38507(7) 0.62758(6) 0.15058(7) 0.0387(2) Uani 1 1 d . U . . .
Nb3 Nb 0.68072(8) 0.46079(8) 0.22291(8) 0.0453(3) Uani 1 1 d . U . . .
Nb4 Nb 0.17220(8) 0.40703(7) -0.05430(10) 0.0627(4) Uani 1 1 d . U . . .
Nb5 Nb 0.35704(9) 0.36466(9) 0.17232(8) 0.0557(3) Uani 1 1 d . U . . .
Nb6 Nb 0.71195(9) 0.72608(7) 0.20851(8) 0.0503(3) Uani 1 1 d . U . . .
V1 V 0.21460(13) 0.21059(12) -0.02708(14) 0.0424(4) Uani 1 1 d . U . . .
P1 P 0.5000 0.5000 0.0000 0.0236(6) Uani 1 2 d S TU P . .
O1 O 0.4478(6) 0.1031(6) 0.0253(7) 0.066(2) Uani 1 1 d . U . . .
O1P O 0.6283(10) 0.5542(10) 0.0935(9) 0.033(2) Uani 0.5 1 d . U . . .
O2 O 0.5732(6) 0.2704(6) -0.0612(5) 0.0454(16) Uani 1 1 d . U . . .
O2P O 0.4791(10) 0.3968(9) -0.0468(9) 0.031(2) Uani 0.5 1 d . U . . .
O3 O 0.3181(5) 0.1989(5) -0.0952(5) 0.0411(14) Uani 1 1 d . U . . .
O3P O 0.4003(9) 0.4838(9) 0.0550(9) 0.032(2) Uani 0.5 1 d . U . . .
O4 O 0.5618(6) 0.7000(7) 0.2237(5) 0.0561(19) Uani 1 1 d . U . . .
O4P O 0.5042(9) 0.5826(8) -0.0586(8) 0.026(2) Uani 0.5 1 d . U . . .
O5 O 0.0129(5) 0.3468(5) -0.0774(5) 0.0387(14) Uani 1 1 d . U . . .
O6 O 0.2082(6) 0.3211(5) 0.0499(6) 0.0608(18) Uani 1 1 d . U . . .
O7 O 0.3504(6) 0.2424(7) 0.0845(5) 0.0531(17) Uani 1 1 d . U . . .
O8 O 0.2805(7) 0.2928(6) 0.2469(6) 0.0580(19) Uani 1 1 d . U . . .
O9 O 0.5200(7) 0.4096(8) 0.2456(5) 0.065(2) Uani 1 1 d . U . . .
O10 O 0.6056(6) 0.3186(7) 0.1381(6) 0.0590(19) Uani 1 1 d . U . . .
O11 O 0.0994(7) 0.0936(6) -0.0365(6) 0.0569(19) Uani 1 1 d . U . . .
O12 O 0.8148(8) 0.8358(7) 0.3001(7) 0.075(2) Uani 1 1 d . U . . .
O13 O 0.7647(8) 0.4432(7) 0.3279(6) 0.072(2) Uani 1 1 d . U . . .
O14 O 0.3345(9) 0.6857(9) 0.2244(7) 0.080(3) Uani 1 1 d . U . . .
O15 O 0.1777(8) 0.2790(7) -0.1290(7) 0.072(2) Uani 1 1 d . U . . .
O16 O 0.2003(11) 0.4843(8) -0.1534(10) 0.105(3) Uani 1 1 d . U . . .
O17 O 0.7143(10) 0.6101(8) 0.2617(9) 0.092(3) Uani 1 1 d . U . . .
O19 O 0.3681(9) 0.4992(7) 0.2078(8) 0.088(3) Uani 1 1 d . U . . .
O20 O 0.2344(8) 0.5283(6) 0.0423(8) 0.092(3) Uani 1 1 d . U . . .
Co1 Co 0.83406(11) 0.19055(9) 0.09795(10) 0.0399(3) Uani 1 1 d . U . . .
N1 N 0.8717(8) 0.3339(7) 0.0664(8) 0.058(2) Uani 1 1 d . U . . .
H1A H 0.8893 0.3374 0.0110 0.069 Uiso 1 1 calc R . . . .
H1B H 0.8063 0.3432 0.0582 0.069 Uiso 1 1 calc R . . . .
N2 N 0.9110(7) 0.1600(7) 0.0099(7) 0.0501(19) Uani 1 1 d . U . . .
H2A H 0.9603 0.2217 -0.0044 0.060 Uiso 1 1 calc R . . . .
H2B H 0.9568 0.1316 0.0390 0.060 Uiso 1 1 calc R . . . .
N3 N 0.9936(8) 0.2697(7) 0.2041(8) 0.063(2) Uani 1 1 d . U . . .
H3A H 0.9810 0.2736 0.2613 0.076 Uiso 1 1 calc R . . . .
H3B H 1.0363 0.2347 0.2051 0.076 Uiso 1 1 calc R . . . .
N4 N 0.8002(8) 0.0515(7) 0.1385(7) 0.0500(19) Uani 1 1 d . U . . .
H4A H 0.7447 -0.0037 0.0891 0.060 Uiso 1 1 calc R . . . .
H4B H 0.8689 0.0467 0.1558 0.060 Uiso 1 1 calc R . . . .
N5 N 0.7459(9) 0.2053(8) 0.1857(7) 0.058(2) Uani 1 1 d . U . . .
H5A H 0.7993 0.2537 0.2403 0.069 Uiso 1 1 calc R . . . .
H5B H 0.6941 0.2282 0.1570 0.069 Uiso 1 1 calc R . . . .
N6 N 0.6841(7) 0.1222(6) -0.0147(6) 0.0377(16) Uani 1 1 d . U . . .
H6A H 0.6335 0.0560 -0.0084 0.045 Uiso 1 1 calc R . . . .
H6B H 0.6458 0.1614 -0.0181 0.045 Uiso 1 1 calc R . . . .
C1 C 0.7156(9) 0.1142(9) -0.1055(8) 0.049(2) Uani 1 1 d . U . . .
H1C H 0.7442 0.1832 -0.1261 0.059 Uiso 1 1 calc R . . . .
H1D H 0.6442 0.0590 -0.1576 0.059 Uiso 1 1 calc R . . . .
C2 C 0.8170(9) 0.0835(8) -0.0806(9) 0.049(2) Uani 1 1 d . U . . .
H2C H 0.7845 0.0092 -0.0710 0.059 Uiso 1 1 calc R . . . .
H2D H 0.8522 0.0894 -0.1328 0.059 Uiso 1 1 calc R . . . .
C3 C 0.9763(12) 0.4198(10) 0.1450(12) 0.082(4) Uani 1 1 d . U . . .
H3C H 0.9478 0.4391 0.1948 0.098 Uiso 1 1 calc R . . . .
H3D H 1.0171 0.4840 0.1196 0.098 Uiso 1 1 calc R . . . .
C4 C 0.6787(14) 0.1005(12) 0.2080(12) 0.078(4) Uani 1 1 d . U . . .
H4C H 0.6015 0.0566 0.1557 0.093 Uiso 1 1 calc R . . . .
H4D H 0.6606 0.1096 0.2676 0.093 Uiso 1 1 calc R . . . .
C5 C 1.0637(11) 0.3812(9) 0.1875(12) 0.079(4) Uani 1 1 d . U . . .
H5C H 1.1227 0.4299 0.2488 0.095 Uiso 1 1 calc R . . . .
H5D H 1.1085 0.3801 0.1436 0.095 Uiso 1 1 calc R . . . .
C6 C 0.7543(15) 0.0456(12) 0.2198(11) 0.079(4) Uani 1 1 d . U . . .
H6C H 0.8226 0.0808 0.2803 0.095 Uiso 1 1 calc R . . . .
H6D H 0.7048 -0.0298 0.2223 0.095 Uiso 1 1 calc R . . . .
Co2 Co 0.5000 0.5000 0.5000 0.0371(8) Uani 0.5 2 d S TU P . .
O1W O 0.5819(14) 0.5879(13) 0.4128(11) 0.060(4) Uani 0.5 1 d . U . . .
H1WA H 0.5418 0.6152 0.3745 0.091 Uiso 0.5 1 d R . . . .
H1WB H 0.5983 0.5430 0.3843 0.091 Uiso 0.5 1 d R . . . .
O2W O 0.3854(8) 0.1752(6) 0.4768(5) 0.058(2) Uani 1 1 d . U . . .
H2WA H 0.3626 0.1350 0.5148 0.087 Uiso 1 1 d R . . . .
H2WB H 0.3452 0.1389 0.4177 0.087 Uiso 1 1 d R . . . .
N7 N 0.6636(17) 0.5390(19) 0.5900(12) 0.061(4) Uani 0.5 1 d . U . . .
H7A H 0.7224 0.5892 0.5713 0.073 Uiso 0.5 1 calc R . . . .
H7B H 0.6716 0.5656 0.6501 0.073 Uiso 0.5 1 calc R . . . .
N8 N 0.4960(18) 0.3686(16) 0.4390(12) 0.051(4) Uani 0.5 1 d . U . . .
H8A H 0.4294 0.3093 0.4398 0.061 Uiso 0.5 1 calc R . . . .
H8B H 0.4930 0.3704 0.3772 0.061 Uiso 0.5 1 calc R . . . .
C7 C 0.673(4) 0.442(3) 0.588(3) 0.135(14) Uani 0.5 1 d . U . . .
H7C H 0.6400 0.4050 0.6359 0.162 Uiso 0.5 1 calc R . . . .
H7D H 0.7594 0.4624 0.6071 0.162 Uiso 0.5 1 calc R . . . .
C8 C 0.611(5) 0.365(4) 0.495(3) 0.18(2) Uani 0.5 1 d . U . . .
H8C H 0.5887 0.2926 0.5064 0.219 Uiso 0.5 1 calc R . . . .
H8D H 0.6664 0.3830 0.4571 0.219 Uiso 0.5 1 calc R . . . .
O3W O 0.8503(12) 0.2953(14) 0.7341(10) 0.061(5) Uani 0.5 1 d . U . . .
H3WA H 0.9144 0.3280 0.7856 0.092 Uiso 0.5 1 d R . . . .
H3WB H 0.7947 0.3097 0.7472 0.092 Uiso 0.5 1 d R . . . .
O4W O 0.430(3) 0.135(2) 0.2776(14) 0.134(12) Uani 0.5 1 d . U . . .
H4WA H 0.4570 0.1792 0.3283 0.201 Uiso 0.5 1 d R . . . .
H4WB H 0.4088 0.1604 0.2267 0.201 Uiso 0.5 1 d R . . . .
O5W O 0.0666(9) 0.0899(8) 0.1906(10) 0.103(4) Uani 1 1 d . U . . .
H5WA H 0.1335 0.1442 0.1877 0.154 Uiso 1 1 d R . . . .
H5WB H 0.0208 0.0437 0.1314 0.154 Uiso 1 1 d R . . . .


_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
Nb1 V1 3.0753(16) . ?
Nb1 O1 1.753(7) . ?
Nb1 O2 1.888(7) . ?
Nb1 O2P 2.506(11) . ?
Nb1 O3 2.073(6) . ?
Nb1 O4P 2.462(10) 2_665 ?
Nb1 O7 2.079(7) . ?
Nb1 O10 1.906(7) . ?
Nb2 O2 1.983(7) 2_665 ?
Nb2 O3P 2.500(12) . ?
Nb2 O4 1.962(7) . ?
Nb2 O14 1.730(9) . ?
Nb2 O19 1.984(9) . ?
Nb2 O20 1.968(9) . ?
Nb3 O1P 2.484(12) . ?
Nb3 O9 1.986(7) . ?
Nb3 O10 1.949(9) . ?
Nb3 O13 1.729(8) . ?
Nb3 O16 1.947(8) 2_665 ?
Nb3 O17 1.961(10) . ?
Nb4 V1 3.0881(17) . ?
Nb4 O5 1.753(6) . ?
Nb4 O6 2.085(8) . ?
Nb4 O15 2.090(9) . ?
Nb4 O16 1.869(10) . ?
Nb4 O20 1.849(10) . ?
Nb5 V1 3.055(2) . ?
Nb5 O3P 2.456(12) . ?
Nb5 O6 2.059(7) . ?
Nb5 O7 2.038(8) . ?
Nb5 O8 1.719(7) . ?
Nb5 O9 1.868(7) . ?
Nb5 O19 1.868(9) . ?
Nb6 V1 3.075(2) 2_665 ?
Nb6 O1P 2.456(13) . ?
Nb6 O3 2.057(7) 2_665 ?
Nb6 O4 1.875(7) . ?
Nb6 O12 1.700(9) . ?
Nb6 O15 2.074(8) 2_665 ?
Nb6 O17 1.860(9) . ?
V1 Nb6 3.075(2) 2_665 ?
V1 O3 1.912(7) . ?
V1 O6 1.910(8) . ?
V1 O7 1.901(7) . ?
V1 O11 1.608(7) . ?
V1 O15 1.890(8) . ?
P1 O1P 1.649(12) 2_665 ?
P1 O1P 1.649(12) . ?
P1 O2P 1.444(11) 2_665 ?
P1 O2P 1.444(11) . ?
P1 O3P 1.623(12) . ?
P1 O3P 1.623(12) 2_665 ?
P1 O4P 1.473(11) 2_665 ?
P1 O4P 1.473(11) . ?
O1P O2P 1.815(15) 2_665 ?
O2 Nb2 1.983(7) 2_665 ?
O2P O1P 1.815(15) 2_665 ?
O2P O3P 1.735(15) 2_665 ?
O2P O4P 1.481(17) 2_665 ?
O3 Nb6 2.057(7) 2_665 ?
O3P O2P 1.735(15) 2_665 ?
O4P Nb1 2.462(10) 2_665 ?
O4P O2P 1.481(17) 2_665 ?
O15 Nb6 2.074(8) 2_665 ?
O16 Nb3 1.947(8) 2_665 ?
Co1 N1 1.968(9) . ?
Co1 N2 1.947(9) . ?
Co1 N3 1.976(9) . ?
Co1 N4 1.971(8) . ?
Co1 N5 1.975(10) . ?
Co1 N6 1.952(8) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C3 1.461(15) . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C2 1.474(14) . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C5 1.489(16) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C6 1.443(16) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 C4 1.442(16) . ?
N6 H6A 0.8900 . ?
N6 H6B 0.8900 . ?
N6 C1 1.490(13) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C1 C2 1.521(13) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C3 C5 1.477(16) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C4 C6 1.480(17) . ?
C5 H5C 0.9700 . ?
C5 H5D 0.9700 . ?
C6 H6C 0.9700 . ?
C6 H6D 0.9700 . ?
Co2 O1W 1.989(15) 2_666 ?
Co2 O1W 1.988(15) . ?
Co2 N7 1.969(17) . ?
Co2 N7 1.969(17) 2_666 ?
Co2 N8 1.979(17) 2_666 ?
Co2 N8 1.979(17) . ?
O1W H1WA 0.8845 . ?
O1W H1WB 0.8683 . ?
O2W H2WA 0.8262 . ?
O2W H2WB 0.8614 . ?
N7 H7A 0.8900 . ?
N7 H7B 0.8900 . ?
N7 C7 1.43(4) . ?
N8 H8A 0.8900 . ?
N8 H8B 0.8900 . ?
N8 C8 1.52(4) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C7 C8 1.44(5) . ?
C8 H8C 0.9700 . ?
C8 H8D 0.9700 . ?
O3W H3WA 0.8626 . ?
O3W H3WB 0.8889 . ?
O4W H4WA 0.8126 . ?
O4W H4WB 0.8704 . ?
O5W H5WA 0.8681 . ?
O5W H5WB 0.9112 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nb1 V1 103.2(2) . . ?
O1 Nb1 O2 99.4(4) . . ?
O1 Nb1 O2P 160.9(4) . . ?
O1 Nb1 O3 99.0(3) . . ?
O1 Nb1 O4P 162.8(4) . 2_665 ?
O1 Nb1 O7 101.0(3) . . ?
O1 Nb1 O10 102.1(4) . . ?
O2 Nb1 V1 127.1(2) . . ?
O2 Nb1 O2P 70.9(3) . . ?
O2 Nb1 O3 92.1(3) . . ?
O2 Nb1 O4P 96.5(3) . 2_665 ?
O2 Nb1 O7 157.4(3) . . ?
O2 Nb1 O10 95.6(3) . . ?
O2P Nb1 V1 72.3(2) . . ?
O3 Nb1 V1 37.63(19) . . ?
O3 Nb1 O2P 65.9(3) . . ?
O3 Nb1 O4P 87.0(3) . 2_665 ?
O3 Nb1 O7 75.0(3) . . ?
O4P Nb1 V1 71.8(2) 2_665 . ?
O4P Nb1 O2P 34.7(4) 2_665 . ?
O7 Nb1 V1 37.3(2) . . ?
O7 Nb1 O2P 86.7(3) . . ?
O7 Nb1 O4P 64.8(3) . 2_665 ?
O10 Nb1 V1 124.6(2) . . ?
O10 Nb1 O2P 95.3(4) . . ?
O10 Nb1 O3 156.0(3) . . ?
O10 Nb1 O4P 69.6(4) . 2_665 ?
O10 Nb1 O7 89.9(3) . . ?
O2 Nb2 O3P 94.9(3) 2_665 . ?
O2 Nb2 O19 157.1(4) 2_665 . ?
O4 Nb2 O2 87.3(3) . 2_665 ?
O4 Nb2 O3P 91.2(3) . . ?
O4 Nb2 O19 87.9(4) . . ?
O4 Nb2 O20 155.4(4) . . ?
O14 Nb2 O2 102.4(4) . 2_665 ?
O14 Nb2 O3P 159.4(4) . . ?
O14 Nb2 O4 100.7(4) . . ?
O14 Nb2 O19 100.6(5) . . ?
O14 Nb2 O20 103.9(5) . . ?
O19 Nb2 O3P 62.8(4) . . ?
O20 Nb2 O2 87.3(3) . 2_665 ?
O20 Nb2 O3P 65.4(4) . . ?
O20 Nb2 O19 87.8(3) . . ?
O9 Nb3 O1P 92.6(3) . . ?
O10 Nb3 O1P 96.3(4) . . ?
O10 Nb3 O9 86.4(3) . . ?
O10 Nb3 O17 156.9(4) . . ?
O13 Nb3 O1P 158.6(4) . . ?
O13 Nb3 O9 100.7(4) . . ?
O13 Nb3 O10 101.2(4) . . ?
O13 Nb3 O16 101.9(5) . 2_665 ?
O13 Nb3 O17 101.9(5) . . ?
O16 Nb3 O1P 66.3(4) 2_665 . ?
O16 Nb3 O9 157.4(4) 2_665 . ?
O16 Nb3 O10 88.2(4) 2_665 . ?
O16 Nb3 O17 88.6(4) 2_665 . ?
O17 Nb3 O1P 61.6(5) . . ?
O17 Nb3 O9 87.9(4) . . ?
O5 Nb4 V1 101.2(2) . . ?
O5 Nb4 O6 97.5(3) . . ?
O5 Nb4 O15 99.0(3) . . ?
O5 Nb4 O16 104.5(4) . . ?
O5 Nb4 O20 103.2(4) . . ?
O6 Nb4 V1 37.3(2) . . ?
O6 Nb4 O15 74.2(3) . . ?
O15 Nb4 V1 36.8(2) . . ?
O16 Nb4 V1 125.0(3) . . ?
O16 Nb4 O6 155.2(4) . . ?
O16 Nb4 O15 91.1(4) . . ?
O20 Nb4 V1 124.7(3) . . ?
O20 Nb4 O6 90.5(4) . . ?
O20 Nb4 O15 154.6(4) . . ?
O20 Nb4 O16 95.3(5) . . ?
O3P Nb5 V1 75.4(3) . . ?
O6 Nb5 V1 37.9(2) . . ?
O6 Nb5 O3P 65.8(3) . . ?
O7 Nb5 V1 37.55(18) . . ?
O7 Nb5 O3P 92.0(4) . . ?
O7 Nb5 O6 75.4(3) . . ?
O8 Nb5 V1 103.3(3) . . ?
O8 Nb5 O3P 157.5(4) . . ?
O8 Nb5 O6 99.0(4) . . ?
O8 Nb5 O7 100.4(3) . . ?
O8 Nb5 O9 100.9(4) . . ?
O8 Nb5 O19 100.6(5) . . ?
O9 Nb5 V1 126.2(3) . . ?
O9 Nb5 O3P 97.6(4) . . ?
O9 Nb5 O6 157.8(3) . . ?
O9 Nb5 O7 91.2(3) . . ?
O19 Nb5 V1 126.6(3) . . ?
O19 Nb5 O3P 65.1(5) . . ?
O19 Nb5 O6 91.7(3) . . ?
O19 Nb5 O7 156.9(4) . . ?
O19 Nb5 O9 94.4(4) . . ?
O1P Nb6 V1 74.1(3) . 2_665 ?
O3 Nb6 V1 37.54(17) 2_665 2_665 ?
O3 Nb6 O1P 90.8(3) 2_665 . ?
O3 Nb6 O15 74.5(3) 2_665 2_665 ?
O4 Nb6 V1 124.3(2) . 2_665 ?
O4 Nb6 O1P 96.1(3) . . ?
O4 Nb6 O3 89.9(3) . 2_665 ?
O4 Nb6 O15 154.0(4) . 2_665 ?
O12 Nb6 V1 104.6(3) . 2_665 ?
O12 Nb6 O1P 158.5(4) . . ?
O12 Nb6 O3 100.9(3) . 2_665 ?
O12 Nb6 O4 101.8(4) . . ?
O12 Nb6 O15 101.5(5) . 2_665 ?
O12 Nb6 O17 103.1(5) . . ?
O15 Nb6 V1 37.0(2) 2_665 2_665 ?
O15 Nb6 O1P 64.1(4) 2_665 . ?
O17 Nb6 V1 124.6(3) . 2_665 ?
O17 Nb6 O1P 63.3(5) . . ?
O17 Nb6 O3 154.0(4) . 2_665 ?
O17 Nb6 O4 94.8(4) . . ?
O17 Nb6 O15 90.9(3) . 2_665 ?
Nb1 V1 Nb4 121.09(5) . . ?
Nb1 V1 Nb6 75.86(4) . 2_665 ?
Nb5 V1 Nb1 75.92(5) . . ?
Nb5 V1 Nb4 76.04(5) . . ?
Nb5 V1 Nb6 121.46(5) . 2_665 ?
Nb6 V1 Nb4 76.52(5) 2_665 . ?
O3 V1 Nb1 41.43(19) . . ?
O3 V1 Nb4 113.5(2) . . ?
O3 V1 Nb5 113.55(19) . . ?
O3 V1 Nb6 40.9(2) . 2_665 ?
O6 V1 Nb1 113.7(2) . . ?
O6 V1 Nb4 41.5(2) . . ?
O6 V1 Nb5 41.5(2) . . ?
O6 V1 Nb6 114.3(3) . 2_665 ?
O6 V1 O3 138.5(3) . . ?
O7 V1 Nb1 41.5(2) . . ?
O7 V1 Nb4 113.0(3) . . ?
O7 V1 Nb5 40.8(2) . . ?
O7 V1 Nb6 113.5(2) . 2_665 ?
O7 V1 O3 83.0(3) . . ?
O7 V1 O6 82.3(3) . . ?
O11 V1 Nb1 119.5(3) . . ?
O11 V1 Nb4 119.4(3) . . ?
O11 V1 Nb5 118.9(3) . . ?
O11 V1 Nb6 119.6(3) . 2_665 ?
O11 V1 O3 111.3(4) . . ?
O11 V1 O6 110.2(4) . . ?
O11 V1 O7 110.9(4) . . ?
O11 V1 O15 111.6(4) . . ?
O15 V1 Nb1 113.1(2) . . ?
O15 V1 Nb4 41.5(3) . . ?
O15 V1 Nb5 113.5(3) . . ?
O15 V1 Nb6 41.3(2) . 2_665 ?
O15 V1 O3 82.3(3) . . ?
O15 V1 O6 83.0(4) . . ?
O15 V1 O7 137.5(4) . . ?
O1P P1 O1P 180.0 . 2_665 ?
O2P P1 O1P 108.5(6) . . ?
O2P P1 O1P 108.5(6) 2_665 2_665 ?
O2P P1 O1P 71.5(6) . 2_665 ?
O2P P1 O1P 71.5(6) 2_665 . ?
O2P P1 O2P 180.0(9) . 2_665 ?
O2P P1 O3P 68.6(6) . 2_665 ?
O2P P1 O3P 111.4(6) . . ?
O2P P1 O3P 68.6(6) 2_665 . ?
O2P P1 O3P 111.4(6) 2_665 2_665 ?
O2P P1 O4P 119.0(6) . . ?
O2P P1 O4P 119.0(6) 2_665 2_665 ?
O2P P1 O4P 61.0(6) 2_665 . ?
O2P P1 O4P 61.0(6) . 2_665 ?
O3P P1 O1P 79.2(6) . 2_665 ?
O3P P1 O1P 100.8(6) . . ?
O3P P1 O1P 100.8(6) 2_665 2_665 ?
O3P P1 O1P 79.2(6) 2_665 . ?
O3P P1 O3P 180.0 . 2_665 ?
O4P P1 O1P 108.7(6) 2_665 2_665 ?
O4P P1 O1P 71.3(6) 2_665 . ?
O4P P1 O1P 108.7(6) . . ?
O4P P1 O1P 71.3(6) . 2_665 ?
O4P P1 O3P 73.1(5) . 2_665 ?
O4P P1 O3P 106.9(5) 2_665 2_665 ?
O4P P1 O3P 106.9(5) . . ?
O4P P1 O3P 73.1(5) 2_665 . ?
O4P P1 O4P 180.0 2_665 . ?
Nb6 O1P Nb3 93.7(4) . . ?
P1 O1P Nb3 125.7(6) . . ?
P1 O1P Nb6 125.1(6) . . ?
P1 O1P O2P 49.0(5) . 2_665 ?
O2P O1P Nb3 140.9(7) 2_665 . ?
O2P O1P Nb6 76.2(5) 2_665 . ?
Nb1 O2 Nb2 136.4(4) . 2_665 ?
P1 O2P Nb1 131.5(7) . . ?
P1 O2P O1P 59.5(6) . 2_665 ?
P1 O2P O3P 60.6(6) . 2_665 ?
P1 O2P O4P 60.5(6) . 2_665 ?
O1P O2P Nb1 137.3(6) 2_665 . ?
O3P O2P Nb1 131.9(6) 2_665 . ?
O3P O2P O1P 90.5(7) 2_665 2_665 ?
O4P O2P Nb1 71.1(6) 2_665 . ?
O4P O2P O1P 100.3(8) 2_665 2_665 ?
O4P O2P O3P 101.1(9) 2_665 2_665 ?
Nb6 O3 Nb1 132.6(3) 2_665 . ?
V1 O3 Nb1 100.9(3) . . ?
V1 O3 Nb6 101.5(3) . 2_665 ?
Nb5 O3P Nb2 93.3(4) . . ?
P1 O3P Nb2 127.9(6) . . ?
P1 O3P Nb5 123.7(6) . . ?
P1 O3P O2P 50.8(5) . 2_665 ?
O2P O3P Nb2 77.1(6) 2_665 . ?
O2P O3P Nb5 138.3(7) 2_665 . ?
Nb6 O4 Nb2 140.9(4) . . ?
P1 O4P Nb1 132.7(7) . 2_665 ?
P1 O4P O2P 58.5(6) . 2_665 ?
O2P O4P Nb1 74.3(6) 2_665 2_665 ?
Nb5 O6 Nb4 131.9(4) . . ?
V1 O6 Nb4 101.2(4) . . ?
V1 O6 Nb5 100.6(3) . . ?
Nb5 O7 Nb1 132.7(4) . . ?
V1 O7 Nb1 101.1(3) . . ?
V1 O7 Nb5 101.6(3) . . ?
Nb5 O9 Nb3 137.6(4) . . ?
Nb1 O10 Nb3 138.3(4) . . ?
Nb6 O15 Nb4 132.9(4) 2_665 . ?
V1 O15 Nb4 101.7(4) . . ?
V1 O15 Nb6 101.7(3) . 2_665 ?
Nb4 O16 Nb3 139.5(5) . 2_665 ?
Nb6 O17 Nb3 141.1(7) . . ?
Nb5 O19 Nb2 138.5(7) . . ?
Nb4 O20 Nb2 140.8(5) . . ?
N1 Co1 N3 85.5(4) . . ?
N1 Co1 N4 176.3(4) . . ?
N1 Co1 N5 92.4(4) . . ?
N2 Co1 N1 93.0(4) . . ?
N2 Co1 N3 91.6(4) . . ?
N2 Co1 N4 89.6(4) . . ?
N2 Co1 N5 174.1(4) . . ?
N2 Co1 N6 85.3(3) . . ?
N4 Co1 N3 91.8(4) . . ?
N4 Co1 N5 85.1(4) . . ?
N5 Co1 N3 91.3(4) . . ?
N6 Co1 N1 90.0(3) . . ?
N6 Co1 N3 174.4(4) . . ?
N6 Co1 N4 92.9(3) . . ?
N6 Co1 N5 92.3(4) . . ?
Co1 N1 H1A 109.6 . . ?
Co1 N1 H1B 109.6 . . ?
H1A N1 H1B 108.2 . . ?
C3 N1 Co1 110.1(8) . . ?
C3 N1 H1A 109.6 . . ?
C3 N1 H1B 109.6 . . ?
Co1 N2 H2A 109.5 . . ?
Co1 N2 H2B 109.5 . . ?
H2A N2 H2B 108.1 . . ?
C2 N2 Co1 110.7(6) . . ?
C2 N2 H2A 109.5 . . ?
C2 N2 H2B 109.5 . . ?
Co1 N3 H3A 109.9 . . ?
Co1 N3 H3B 109.9 . . ?
H3A N3 H3B 108.3 . . ?
C5 N3 Co1 108.8(8) . . ?
C5 N3 H3A 109.9 . . ?
C5 N3 H3B 109.9 . . ?
Co1 N4 H4A 109.8 . . ?
Co1 N4 H4B 109.8 . . ?
H4A N4 H4B 108.3 . . ?
C6 N4 Co1 109.3(7) . . ?
C6 N4 H4A 109.8 . . ?
C6 N4 H4B 109.8 . . ?
Co1 N5 H5A 110.0 . . ?
Co1 N5 H5B 110.0 . . ?
H5A N5 H5B 108.4 . . ?
C4 N5 Co1 108.4(8) . . ?
C4 N5 H5A 110.0 . . ?
C4 N5 H5B 110.0 . . ?
Co1 N6 H6A 109.7 . . ?
Co1 N6 H6B 109.7 . . ?
H6A N6 H6B 108.2 . . ?
C1 N6 Co1 109.8(6) . . ?
C1 N6 H6A 109.7 . . ?
C1 N6 H6B 109.7 . . ?
N6 C1 H1C 110.5 . . ?
N6 C1 H1D 110.5 . . ?
N6 C1 C2 106.1(8) . . ?
H1C C1 H1D 108.7 . . ?
C2 C1 H1C 110.5 . . ?
C2 C1 H1D 110.5 . . ?
N2 C2 C1 106.5(8) . . ?
N2 C2 H2C 110.4 . . ?
N2 C2 H2D 110.4 . . ?
C1 C2 H2C 110.4 . . ?
C1 C2 H2D 110.4 . . ?
H2C C2 H2D 108.6 . . ?
N1 C3 H3C 109.8 . . ?
N1 C3 H3D 109.8 . . ?
N1 C3 C5 109.4(9) . . ?
H3C C3 H3D 108.2 . . ?
C5 C3 H3C 109.8 . . ?
C5 C3 H3D 109.8 . . ?
N5 C4 H4C 109.9 . . ?
N5 C4 H4D 109.9 . . ?
N5 C4 C6 109.0(11) . . ?
H4C C4 H4D 108.3 . . ?
C6 C4 H4C 109.9 . . ?
C6 C4 H4D 109.9 . . ?
N3 C5 H5C 109.9 . . ?
N3 C5 H5D 109.9 . . ?
C3 C5 N3 108.9(10) . . ?
C3 C5 H5C 109.9 . . ?
C3 C5 H5D 109.9 . . ?
H5C C5 H5D 108.3 . . ?
N4 C6 C4 109.1(11) . . ?
N4 C6 H6C 109.9 . . ?
N4 C6 H6D 109.9 . . ?
C4 C6 H6C 109.9 . . ?
C4 C6 H6D 109.9 . . ?
H6C C6 H6D 108.3 . . ?
O1W Co2 O1W 180.0(10) . 2_666 ?
N7 Co2 O1W 88.8(8) . . ?
N7 Co2 O1W 91.2(8) 2_666 . ?
N7 Co2 O1W 91.2(8) . 2_666 ?
N7 Co2 O1W 88.8(8) 2_666 2_666 ?
N7 Co2 N7 180.0 2_666 . ?
N7 Co2 N8 92.7(8) 2_666 . ?
N7 Co2 N8 87.3(8) 2_666 2_666 ?
N7 Co2 N8 92.7(8) . 2_666 ?
N7 Co2 N8 87.3(8) . . ?
N8 Co2 O1W 92.3(7) 2_666 2_666 ?
N8 Co2 O1W 87.7(7) 2_666 . ?
N8 Co2 O1W 87.7(7) . 2_666 ?
N8 Co2 O1W 92.3(7) . . ?
N8 Co2 N8 180.0 2_666 . ?
Co2 O1W H1WA 116.9 . . ?
Co2 O1W H1WB 100.4 . . ?
H1WA O1W H1WB 116.7 . . ?
H2WA O2W H2WB 109.4 . . ?
Co2 N7 H7A 110.3 . . ?
Co2 N7 H7B 110.3 . . ?
H7A N7 H7B 108.6 . . ?
C7 N7 Co2 107.0(18) . . ?
C7 N7 H7A 110.3 . . ?
C7 N7 H7B 110.3 . . ?
Co2 N8 H8A 109.9 . . ?
Co2 N8 H8B 109.9 . . ?
H8A N8 H8B 108.3 . . ?
C8 N8 Co2 108.9(18) . . ?
C8 N8 H8A 109.9 . . ?
C8 N8 H8B 109.9 . . ?
N7 C7 H7C 108.2 . . ?
N7 C7 H7D 108.2 . . ?
N7 C7 C8 116(3) . . ?
H7C C7 H7D 107.4 . . ?
C8 C7 H7C 108.2 . . ?
C8 C7 H7D 108.2 . . ?
N8 C8 H8C 109.5 . . ?
N8 C8 H8D 109.5 . . ?
C7 C8 N8 111(3) . . ?
C7 C8 H8C 109.5 . . ?
C7 C8 H8D 109.5 . . ?
H8C C8 H8D 108.0 . . ?
H3WA O3W H3WB 104.9 . . ?
H4WA O4W H4WB 112.5 . . ?
H5WA O5W H5WB 111.3 . . ?

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
Nb1 V1 O15 Nb4 -111.4(3) . . . . ?
Nb1 V1 O15 Nb6 27.4(5) . . . 2_665 ?
Nb4 V1 O15 Nb6 138.8(6) . . . 2_665 ?
Nb5 V1 O15 Nb4 -27.3(4) . . . . ?
Nb5 V1 O15 Nb6 111.5(3) . . . 2_665 ?
Nb6 V1 O15 Nb4 -138.8(6) 2_665 . . . ?
V1 Nb1 O2 Nb2 41.5(6) . . . 2_665 ?
V1 Nb4 O16 Nb3 -39.9(13) . . . 2_665 ?
V1 Nb4 O20 Nb2 40.8(11) . . . . ?
V1 Nb5 O9 Nb3 44.1(10) . . . . ?
V1 Nb5 O19 Nb2 -39.7(10) . . . . ?
V1 Nb6 O4 Nb2 42.2(9) 2_665 . . . ?
V1 Nb6 O17 Nb3 -37.2(11) 2_665 . . . ?
O1 Nb1 O2 Nb2 156.0(5) . . . 2_665 ?
O1P Nb6 O4 Nb2 -32.7(8) . . . . ?
O1P Nb6 O17 Nb3 6.6(7) . . . . ?
O1P P1 O2P Nb1 -128.2(9) 2_665 . . . ?
O1P P1 O2P Nb1 51.8(9) . . . . ?
O1P P1 O2P O1P 180.001(2) . . . 2_665 ?
O1P P1 O2P O3P -69.9(6) . . . 2_665 ?
O1P P1 O2P O3P 110.1(6) 2_665 . . 2_665 ?
O1P P1 O2P O4P -124.9(7) 2_665 . . 2_665 ?
O1P P1 O2P O4P 55.1(7) . . . 2_665 ?
O1P P1 O3P Nb2 -115.5(8) 2_665 . . . ?
O1P P1 O3P Nb2 64.5(8) . . . . ?
O1P P1 O3P Nb5 117.2(7) 2_665 . . . ?
O1P P1 O3P Nb5 -62.8(7) . . . . ?
O1P P1 O3P O2P 65.1(7) . . . 2_665 ?
O1P P1 O3P O2P -114.9(7) 2_665 . . 2_665 ?
O1P P1 O4P Nb1 121.4(8) 2_665 . . 2_665 ?
O1P P1 O4P Nb1 -58.6(8) . . . 2_665 ?
O1P P1 O4P O2P -55.2(7) . . . 2_665 ?
O1P P1 O4P O2P 124.8(7) 2_665 . . 2_665 ?
O2P Nb1 O2 Nb2 -7.0(5) . . . 2_665 ?
O2P P1 O1P Nb3 129.9(9) 2_665 . . . ?
O2P P1 O1P Nb3 -50.1(9) . . . . ?
O2P P1 O1P Nb6 2.9(7) 2_665 . . . ?
O2P P1 O1P Nb6 -177.1(7) . . . . ?
O2P P1 O1P O2P 179.999(3) . . . 2_665 ?
O2P P1 O3P Nb2 -0.5(7) 2_665 . . . ?
O2P P1 O3P Nb2 179.5(7) . . . . ?
O2P P1 O3P Nb5 -127.9(8) 2_665 . . . ?
O2P P1 O3P Nb5 52.1(8) . . . . ?
O2P P1 O3P O2P 180.002(1) . . . 2_665 ?
O2P P1 O4P Nb1 -3.4(6) 2_665 . . 2_665 ?
O2P P1 O4P Nb1 176.6(6) . . . 2_665 ?
O2P P1 O4P O2P 180.000(4) . . . 2_665 ?
O3 Nb1 O2 Nb2 56.6(5) . . . 2_665 ?
O3 Nb6 O4 Nb2 58.2(8) 2_665 . . . ?
O3 Nb6 O17 Nb3 1.3(15) 2_665 . . . ?
O3 V1 O15 Nb4 -139.6(4) . . . . ?
O3 V1 O15 Nb6 -0.9(4) . . . 2_665 ?
O3P Nb5 O9 Nb3 -33.4(9) . . . . ?
O3P Nb5 O19 Nb2 6.5(7) . . . . ?
O3P P1 O1P Nb3 67.0(8) . . . . ?
O3P P1 O1P Nb3 -113.0(8) 2_665 . . . ?
O3P P1 O1P Nb6 120.0(8) 2_665 . . . ?
O3P P1 O1P Nb6 -60.0(8) . . . . ?
O3P P1 O1P O2P 117.1(6) 2_665 . . 2_665 ?
O3P P1 O1P O2P -62.9(6) . . . 2_665 ?
O3P P1 O2P Nb1 -58.3(9) . . . . ?
O3P P1 O2P Nb1 121.7(9) 2_665 . . . ?
O3P P1 O2P O1P 69.9(6) . . . 2_665 ?
O3P P1 O2P O1P -110.1(6) 2_665 . . 2_665 ?
O3P P1 O2P O3P 180.001(1) . . . 2_665 ?
O3P P1 O2P O4P -55.0(7) . . . 2_665 ?
O3P P1 O2P O4P 125.0(7) 2_665 . . 2_665 ?
O3P P1 O4P Nb1 -130.5(9) 2_665 . . 2_665 ?
O3P P1 O4P Nb1 49.5(9) . . . 2_665 ?
O3P P1 O4P O2P -127.1(7) 2_665 . . 2_665 ?
O3P P1 O4P O2P 52.9(7) . . . 2_665 ?
O4 Nb6 O17 Nb3 101.0(9) . . . . ?
O4P Nb1 O2 Nb2 -30.7(6) 2_665 . . 2_665 ?
O4P P1 O1P Nb3 -0.9(6) 2_665 . . . ?
O4P P1 O1P Nb3 179.1(6) . . . . ?
O4P P1 O1P Nb6 -127.9(8) 2_665 . . . ?
O4P P1 O1P Nb6 52.1(8) . . . . ?
O4P P1 O1P O2P -130.8(7) 2_665 . . 2_665 ?
O4P P1 O1P O2P 49.2(7) . . . 2_665 ?
O4P P1 O2P Nb1 -3.3(6) 2_665 . . . ?
O4P P1 O2P Nb1 176.7(6) . . . . ?
O4P P1 O2P O1P -55.1(7) . . . 2_665 ?
O4P P1 O2P O1P 124.9(7) 2_665 . . 2_665 ?
O4P P1 O2P O3P -125.0(7) 2_665 . . 2_665 ?
O4P P1 O2P O3P 55.0(7) . . . 2_665 ?
O4P P1 O2P O4P 179.998(2) . . . 2_665 ?
O4P P1 O3P Nb2 -49.0(8) . . . . ?
O4P P1 O3P Nb2 131.0(8) 2_665 . . . ?
O4P P1 O3P Nb5 3.7(6) 2_665 . . . ?
O4P P1 O3P Nb5 -176.3(6) . . . . ?
O4P P1 O3P O2P 131.5(7) 2_665 . . 2_665 ?
O4P P1 O3P O2P -48.5(7) . . . 2_665 ?
O5 Nb4 O16 Nb3 -155.1(10) . . . 2_665 ?
O5 Nb4 O20 Nb2 154.7(9) . . . . ?
O6 Nb4 O16 Nb3 -3(2) . . . 2_665 ?
O6 Nb4 O20 Nb2 56.8(10) . . . . ?
O6 Nb5 O9 Nb3 6.6(16) . . . . ?
O6 Nb5 O19 Nb2 -55.7(8) . . . . ?
O6 V1 O15 Nb4 1.5(3) . . . . ?
O6 V1 O15 Nb6 140.2(4) . . . 2_665 ?
O7 Nb1 O2 Nb2 2.4(11) . . . 2_665 ?
O7 Nb5 O9 Nb3 58.8(8) . . . . ?
O7 Nb5 O19 Nb2 -0.5(15) . . . . ?
O7 V1 O15 Nb4 -69.0(5) . . . . ?
O7 V1 O15 Nb6 69.8(7) . . . 2_665 ?
O8 Nb5 O9 Nb3 159.5(8) . . . . ?
O8 Nb5 O19 Nb2 -155.2(7) . . . . ?
O9 Nb5 O19 Nb2 102.9(7) . . . . ?
O10 Nb1 O2 Nb2 -100.7(5) . . . 2_665 ?
O11 V1 O15 Nb4 110.5(4) . . . . ?
O11 V1 O15 Nb6 -110.8(4) . . . 2_665 ?
O12 Nb6 O4 Nb2 159.3(7) . . . . ?
O12 Nb6 O17 Nb3 -155.6(9) . . . . ?
O15 Nb4 O16 Nb3 -55.5(11) . . . 2_665 ?
O15 Nb4 O20 Nb2 4.8(17) . . . . ?
O15 Nb6 O4 Nb2 5.8(14) 2_665 . . . ?
O15 Nb6 O17 Nb3 -53.6(9) 2_665 . . . ?
O16 Nb4 O20 Nb2 -99.1(10) . . . . ?
O17 Nb6 O4 Nb2 -96.2(8) . . . . ?
O19 Nb5 O9 Nb3 -98.8(8) . . . . ?
O20 Nb4 O16 Nb3 99.8(11) . . . 2_665 ?
Co1 N1 C3 C5 34.6(16) . . . . ?
Co1 N2 C2 C1 38.2(9) . . . . ?
Co1 N3 C5 C3 35.5(14) . . . . ?
Co1 N4 C6 C4 34.5(14) . . . . ?
Co1 N5 C4 C6 38.4(14) . . . . ?
Co1 N6 C1 C2 39.6(9) . . . . ?
N1 C3 C5 N3 -46.0(18) . . . . ?
N5 C4 C6 N4 -48.6(17) . . . . ?
N6 C1 C2 N2 -49.9(10) . . . . ?
Co2 N7 C7 C8 34(5) . . . . ?
Co2 N8 C8 C7 14(6) . . . . ?
N7 C7 C8 N8 -32(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
