# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_ddb
_database_code_depnum_ccdc_archive 'CCDC 1983449'
loop_
_audit_author_name
_audit_author_address
'Dong-Bin Dang'
;Henan University
China
;
_audit_update_record             
;
2022-01-08 deposited with the CCDC.	2022-01-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C96 H425 Cu16 K2 N64 Nb48 O233 V21'
_chemical_formula_weight         12830.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 '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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'

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

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

_cell_length_a                   26.3773(17)
_cell_length_b                   26.3773(17)
_cell_length_c                   27.4429(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19094(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7325
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      25.35

_exptl_crystal_description       stick
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.232
_exptl_crystal_F_000             12532
_exptl_transmission_factor_min   0.4631
_exptl_transmission_factor_max   0.7457
_exptl_crystal_size_max          0.440
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    2.853
_shelx_estimated_absorpt_T_min   0.367
_shelx_estimated_absorpt_T_max   0.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24395
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.484
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        24.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4452
_reflns_number_gt                2987
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0886P)²+393.6107P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.000016(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4452
_refine_ls_number_parameters     302
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_gt           0.0644
_refine_ls_wR_factor_ref         0.1925
_refine_ls_wR_factor_gt          0.1714
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.72025(8) 0.77975(8) 0.500000 0.0243(6) Uani 1 4 d S T P . .
V2 V 0.64296(9) 0.70115(10) 0.60513(9) 0.0722(7) Uani 1 1 d . . . . .
Nb1 Nb 0.71735(4) 0.78265(4) 0.63289(5) 0.0505(4) Uani 1 2 d S T P . .
Nb2 Nb 0.74097(3) 0.65792(3) 0.56238(3) 0.0373(3) Uani 1 1 d . . . . .
Nb3 Nb 0.62434(5) 0.67710(5) 0.500000 0.0415(4) Uani 1 2 d S T P . .
Nb4 Nb 0.60268(4) 0.80430(4) 0.56920(4) 0.0464(3) Uani 1 1 d . . . . .
O1 O 0.7249(3) 0.7751(3) 0.6951(4) 0.059(3) Uani 1 2 d S T P . .
O2 O 0.7573(3) 0.6098(3) 0.6038(3) 0.0525(19) Uani 1 1 d . . . . .
O3 O 0.5706(3) 0.6384(3) 0.500000 0.042(2) Uani 1 2 d S T P . .
O4 O 0.5412(3) 0.8074(3) 0.5926(4) 0.069(3) Uani 1 1 d . . . . .
O5 O 0.6134(4) 0.6698(4) 0.6460(4) 0.083(3) Uani 1 1 d . . . . .
O6 O 0.6258(3) 0.8742(3) 0.5809(5) 0.064(3) Uani 1 2 d S T P . .
O7 O 0.6417(3) 0.7780(3) 0.6266(3) 0.059(2) Uani 1 1 d . . . . .
O8 O 0.7153(2) 0.7109(3) 0.6097(2) 0.0403(16) Uani 1 1 d . . . . .
O9 O 0.8025(3) 0.6975(3) 0.5580(3) 0.040(2) Uani 1 2 d S T P . .
O10 O 0.5934(4) 0.8190(4) 0.500000 0.049(3) Uani 1 2 d S T P . .
O11 O 0.6646(2) 0.6472(2) 0.4459(2) 0.0414(16) Uani 1 1 d . . . . .
O12 O 0.7518(4) 0.6229(4) 0.500000 0.041(2) Uani 1 2 d S T P . .
O13 O 0.6056(2) 0.7295(3) 0.4505(2) 0.0385(15) Uani 1 1 d . . . . .
O14 O 0.6939(2) 0.8061(2) 0.5499(3) 0.035(2) Uani 1 2 d S T P . .
O15 O 0.7093(3) 0.7163(3) 0.500000 0.0314(19) Uani 1 2 d S T P . .
V3 V 0.6092(5) 0.8908(5) 0.500000 0.053(4) Uiso 0.25 4 d S . P . .
O16 O 0.5645(14) 0.9355(14) 0.500000 0.035(11) Uiso 0.25 4 d S . P . .
K1 K 0.500000 0.500000 0.500000 0.073(2) Uani 1 8 d S T P B .
Cu1 Cu 0.67519(8) 0.82481(8) 0.75805(9) 0.0807(8) Uani 1 2 d S T P . .
Cu2 Cu 0.65858(7) 0.52139(7) 0.500000 0.0571(6) Uani 1 2 d S T P B .
N1 N 0.6786(11) 0.8885(10) 0.7210(10) 0.076(8) Uiso 0.5 1 d D . P A 1
H1A H 0.683062 0.882363 0.689396 0.091 Uiso 0.5 1 calc R U P A 1
H1B H 0.650303 0.906433 0.724827 0.091 Uiso 0.5 1 calc R U P A 1
C1 C 0.7231(9) 0.9164(9) 0.7415(10) 0.062(7) Uiso 0.5 1 d D . P A 1
H1C H 0.712364 0.936919 0.768957 0.075 Uiso 0.5 1 calc R U P A 1
H1D H 0.737253 0.938676 0.716954 0.075 Uiso 0.5 1 calc R U P A 1
C2 C 0.7625(9) 0.8793(9) 0.7578(11) 0.068(10) Uiso 0.5 1 d D . P A 1
H2C H 0.774266 0.861358 0.728613 0.081 Uiso 0.5 1 calc R U P A 1
C3 C 0.8085(10) 0.9015(11) 0.7817(10) 0.077(8) Uiso 0.5 1 d D . P A 1
H3A H 0.832696 0.875142 0.788054 0.116 Uiso 0.5 1 calc R U P A 1
H3B H 0.798877 0.917262 0.811879 0.116 Uiso 0.5 1 calc R U P A 1
H3C H 0.823354 0.926400 0.760570 0.116 Uiso 0.5 1 calc R U P A 1
N2 N 0.7344(9) 0.8414(9) 0.7882(9) 0.059(7) Uiso 0.5 1 d D . P A 1
H2A H 0.727937 0.854479 0.817450 0.071 Uiso 0.5 1 calc R U P A 1
H2B H 0.753258 0.813735 0.792227 0.071 Uiso 0.5 1 calc R U P A 1
N1' N 0.7499(10) 0.8344(9) 0.7938(9) 0.062(7) Uiso 0.5 1 d D . P A 2
H1'A H 0.746396 0.845853 0.824127 0.074 Uiso 0.5 1 calc R U P A 2
H1'B H 0.766934 0.805247 0.794516 0.074 Uiso 0.5 1 calc R U P A 2
C1' C 0.7761(11) 0.8724(9) 0.7624(12) 0.070(9) Uiso 0.5 1 d D . P A 2
H1'C H 0.789113 0.855102 0.733853 0.084 Uiso 0.5 1 calc R U P A 2
H1'D H 0.804947 0.885668 0.780245 0.084 Uiso 0.5 1 calc R U P A 2
C2' C 0.7442(9) 0.9162(10) 0.7458(11) 0.090(10) Uiso 0.5 1 d D . P A 2
H2'C H 0.732679 0.931209 0.776540 0.108 Uiso 0.5 1 calc R U P A 2
C3' C 0.7685(13) 0.9608(10) 0.7199(14) 0.149(17) Uiso 0.5 1 d D . P A 2
H3'A H 0.769766 0.954185 0.685504 0.224 Uiso 0.5 1 calc R U P A 2
H3'B H 0.802308 0.965697 0.732007 0.224 Uiso 0.5 1 calc R U P A 2
H3'C H 0.748868 0.990866 0.725712 0.224 Uiso 0.5 1 calc R U P A 2
N2' N 0.6964(10) 0.8938(11) 0.7252(11) 0.081(9) Uiso 0.5 1 d D . P A 2
H2'A H 0.700666 0.888711 0.693375 0.098 Uiso 0.5 1 calc R U P A 2
H2'B H 0.671297 0.916027 0.728823 0.098 Uiso 0.5 1 calc R U P A 2
N3 N 0.7075(4) 0.5108(4) 0.5562(4) 0.076(3) Uani 1 1 d D U . . .
H3D H 0.724662 0.481583 0.552300 0.091 Uiso 1 1 d R U . B .
H3E H 0.730032 0.536433 0.557340 0.091 Uiso 1 1 d R U . . .
C4 C 0.6833(6) 0.5159(11) 0.6044(6) 0.082(7) Uiso 0.7 1 d D U P B 1
H4B H 0.689537 0.549394 0.617797 0.098 Uiso 0.7 1 calc R U P B 1
H4C H 0.696767 0.490849 0.626872 0.098 Uiso 0.7 1 calc R U P B 1
C5 C 0.6278(6) 0.5078(7) 0.5967(5) 0.071(5) Uiso 0.7 1 d D U P B 1
H5A H 0.621671 0.471711 0.590478 0.086 Uiso 0.7 1 calc R U P B 1
C6 C 0.6016(8) 0.5227(8) 0.6431(6) 0.083(6) Uiso 0.7 1 d D . P B 1
H6A H 0.566381 0.513843 0.641006 0.124 Uiso 0.7 1 calc R U P B 1
H6B H 0.604858 0.558582 0.647821 0.124 Uiso 0.7 1 calc R U P B 1
H6C H 0.616851 0.505136 0.669989 0.124 Uiso 0.7 1 calc R U P B 1
C4' C 0.6732(17) 0.5038(18) 0.5992(13) 0.081(18) Uiso 0.3 1 d D . P B 2
H4'A H 0.693433 0.503780 0.628705 0.097 Uiso 0.3 1 calc R U P B 2
H4'B H 0.656676 0.471085 0.596681 0.097 Uiso 0.3 1 calc R U P B 2
C5' C 0.6335(18) 0.5443(16) 0.6031(10) 0.16(2) Uiso 0.3 1 d D U P B 2
H5'A H 0.608346 0.528933 0.624880 0.187 Uiso 0.3 1 calc R U P B 2
C6' C 0.642(3) 0.596(2) 0.626(2) 0.17(2) Uiso 0.3 1 d D U P B 2
H6'A H 0.610876 0.614874 0.623855 0.254 Uiso 0.3 1 calc R U P B 2
H6'B H 0.651599 0.591709 0.659004 0.254 Uiso 0.3 1 calc R U P B 2
H6'C H 0.667978 0.613142 0.608101 0.254 Uiso 0.3 1 calc R U P B 2
N4 N 0.6096(4) 0.5382(4) 0.5537(4) 0.064(3) Uani 1 1 d D . . . .
H4A H 0.608029 0.572293 0.553855 0.077 Uiso 1 1 d R U . B 1
O3W O 0.3336(15) 0.9715(12) 0.500000 0.241(15) Uani 1 2 d S T P . .
O4W O 0.506(5) 0.874(4) 0.690(4) 0.28(5) Uiso 0.25 1 d . . P C 1
O5W O 0.378(2) 0.878(2) 0.683(3) 0.25(3) Uiso 0.5 2 d S . P . .
O6W O 0.4563(6) 0.8278(6) 0.6380(6) 0.157(6) Uani 1 1 d . U . . .
O7W O 0.412(3) 0.912(3) 0.569(3) 0.16(3) Uiso 0.25 2 d S . P D 1
O8W O 0.460(4) 0.960(4) 0.598(5) 0.24(6) Uiso 0.25 2 d S . P E 2
O9W O 0.544(5) 0.956(5) 0.609(7) 0.29(8) Uiso 0.25 2 d S . P F 2
O10W O 0.5729(16) 0.9271(16) 0.659(2) 0.20(2) Uiso 0.5 2 d S . P G 1
O11W O 0.4634(17) 0.8880(17) 0.7195(15) 0.202(16) Uiso 0.5 1 d . . P H 2
O12W O 0.3709(11) 0.8709(11) 0.500000 0.163(12) Uiso 1 4 d S . P I 1
O13W O 0.338(3) 0.838(3) 0.500000 0.22(4) Uiso 0.5 4 d S . P J 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
V1 O14 1.685(9) 18_556 ?
V1 O14 1.685(9) . ?
V1 O15 1.699(8) 31_665 ?
V1 O15 1.699(8) . ?
V2 O5 1.597(10) . ?
V2 O8 1.930(7) . ?
V2 O13 1.964(7) 18_556 ?
V2 O11 2.076(7) 18_556 ?
V2 O7 2.111(9) . ?
V2 Nb3 2.995(3) . ?
V2 Nb1 3.009(2) . ?
V2 Nb2 3.060(3) . ?
V2 Nb4 3.083(3) . ?
Nb1 O1 1.731(11) . ?
Nb1 O8 1.998(7) . ?
Nb1 O8 1.998(7) 31_665 ?
Nb1 O7 2.006(7) 31_665 ?
Nb1 O7 2.006(7) . ?
Nb1 O14 2.440(9) . ?
Nb2 O2 1.758(7) . ?
Nb2 O9 1.934(2) . ?
Nb2 O12 1.966(5) . ?
Nb2 O8 2.024(7) . ?
Nb2 O11 2.048(7) 18_556 ?
Nb2 O15 2.449(6) . ?
Nb3 O3 1.746(9) . ?
Nb3 O11 1.987(7) . ?
Nb3 O11 1.987(7) 18_556 ?
Nb3 O13 2.001(7) 18_556 ?
Nb3 O13 2.001(7) . ?
Nb3 O15 2.467(8) . ?
Nb4 O4 1.746(7) . ?
Nb4 O10 1.954(3) . ?
Nb4 O6 1.968(5) . ?
Nb4 O7 2.007(8) . ?
Nb4 O13 2.046(7) 18_556 ?
Nb4 O14 2.464(6) . ?
Nb4 V3 2.973(8) . ?
O6 V3 2.305(14) . ?
O10 V3 1.938(13) . ?
V3 O16 1.67(5) . ?
K1 N4 3.399(10) . ?
K1 N4 3.399(10) 17_666 ?
K1 N4 3.399(10) 19_566 ?
K1 N4 3.399(10) 3_655 ?
K1 N4 3.399(10) 2_665 ?
K1 N4 3.399(10) 18_556 ?
K1 N4 3.399(10) 20_656 ?
K1 N4 3.399(10) 4_565 ?
Cu1 N2 1.82(3) . ?
Cu1 N2 1.82(3) 31_665 ?
Cu1 N1 1.97(3) . ?
Cu1 N1 1.97(3) 31_665 ?
Cu1 N2' 2.11(3) 31_665 ?
Cu1 N2' 2.11(3) . ?
Cu1 N1' 2.22(3) 31_665 ?
Cu1 N1' 2.22(3) . ?
Cu2 N4 2.010(11) 18_556 ?
Cu2 N4 2.010(11) . ?
Cu2 N3 2.031(10) . ?
Cu2 N3 2.031(10) 18_556 ?
N1 C1 1.495(10) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C1 C2 1.496(10) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 N2 1.498(10) . ?
C2 C3 1.499(10) . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N1' C1' 1.491(10) . ?
N1' H1'A 0.8900 . ?
N1' H1'B 0.8900 . ?
C1' C2' 1.501(10) . ?
C1' H1'C 0.9700 . ?
C1' H1'D 0.9700 . ?
C2' N2' 1.503(10) . ?
C2' C3' 1.517(10) . ?
C2' H2'C 0.9800 . ?
C3' H3'A 0.9600 . ?
C3' H3'B 0.9600 . ?
C3' H3'C 0.9600 . ?
N2' H2'A 0.8900 . ?
N2' H2'B 0.8900 . ?
N3 C4 1.476(10) . ?
N3 C4' 1.498(10) . ?
N3 H3D 0.8998 . ?
N3 H3E 0.9001 . ?
C4 C5 1.495(10) . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C5 C6 1.499(10) . ?
C5 N4 1.506(9) . ?
C5 H5A 0.9800 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C4' C5' 1.500(10) . ?
C4' H4'A 0.9700 . ?
C4' H4'B 0.9700 . ?
C5' N4 1.503(10) . ?
C5' C6' 1.503(10) . ?
C5' H5'A 0.9800 . ?
C6' H6'A 0.9600 . ?
C6' H6'B 0.9600 . ?
C6' H6'C 0.9600 . ?
N4 H4A 0.8999 . ?

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
O14 V1 O14 108.7(6) 18_556 . ?
O14 V1 O15 109.6(2) 18_556 31_665 ?
O14 V1 O15 109.6(2) . 31_665 ?
O14 V1 O15 109.6(2) 18_556 . ?
O14 V1 O15 109.6(2) . . ?
O15 V1 O15 109.6(6) 31_665 . ?
O5 V2 O8 120.4(5) . . ?
O5 V2 O13 119.8(5) . 18_556 ?
O8 V2 O13 119.7(3) . 18_556 ?
O5 V2 O11 104.7(4) . 18_556 ?
O8 V2 O11 82.2(3) . 18_556 ?
O13 V2 O11 82.8(3) 18_556 18_556 ?
O5 V2 O7 107.1(4) . . ?
O8 V2 O7 82.5(3) . . ?
O13 V2 O7 81.0(3) 18_556 . ?
O11 V2 O7 148.3(3) 18_556 . ?
O5 V2 Nb3 119.1(4) . . ?
O8 V2 Nb3 104.7(2) . . ?
O13 V2 Nb3 41.4(2) 18_556 . ?
O11 V2 Nb3 41.39(19) 18_556 . ?
O7 V2 Nb3 118.0(2) . . ?
O5 V2 Nb1 120.7(4) . . ?
O8 V2 Nb1 40.8(2) . . ?
O13 V2 Nb1 104.5(2) 18_556 . ?
O11 V2 Nb1 118.8(2) 18_556 . ?
O7 V2 Nb1 41.7(2) . . ?
Nb3 V2 Nb1 120.15(9) . . ?
O5 V2 Nb2 119.3(4) . . ?
O8 V2 Nb2 40.4(2) . . ?
O13 V2 Nb2 105.5(2) 18_556 . ?
O11 V2 Nb2 41.75(19) 18_556 . ?
O7 V2 Nb2 118.6(2) . . ?
Nb3 V2 Nb2 71.95(6) . . ?
Nb1 V2 Nb2 79.18(7) . . ?
O5 V2 Nb4 120.9(4) . . ?
O8 V2 Nb4 104.2(2) . . ?
O13 V2 Nb4 40.7(2) 18_556 . ?
O11 V2 Nb4 118.9(2) 18_556 . ?
O7 V2 Nb4 40.3(2) . . ?
Nb3 V2 Nb4 79.76(7) . . ?
Nb1 V2 Nb4 71.04(6) . . ?
Nb2 V2 Nb4 119.83(8) . . ?
O1 Nb1 O8 102.0(3) . . ?
O1 Nb1 O8 102.0(3) . 31_665 ?
O8 Nb1 O8 87.1(4) . 31_665 ?
O1 Nb1 O7 101.0(4) . 31_665 ?
O8 Nb1 O7 156.5(3) . 31_665 ?
O8 Nb1 O7 83.6(3) 31_665 31_665 ?
O1 Nb1 O7 101.0(4) . . ?
O8 Nb1 O7 83.6(3) . . ?
O8 Nb1 O7 156.5(3) 31_665 . ?
O7 Nb1 O7 96.6(5) 31_665 . ?
O1 Nb1 O14 168.3(5) . . ?
O8 Nb1 O14 86.4(2) . . ?
O8 Nb1 O14 86.4(2) 31_665 . ?
O7 Nb1 O14 71.6(3) 31_665 . ?
O7 Nb1 O14 71.6(3) . . ?
O1 Nb1 V2 104.04(7) . 31_665 ?
O8 Nb1 V2 123.8(2) . 31_665 ?
O8 Nb1 V2 39.19(19) 31_665 31_665 ?
O7 Nb1 V2 44.4(2) 31_665 31_665 ?
O7 Nb1 V2 136.8(3) . 31_665 ?
O14 Nb1 V2 77.26(6) . 31_665 ?
O1 Nb1 V2 104.04(7) . . ?
O8 Nb1 V2 39.19(19) . . ?
O8 Nb1 V2 123.8(2) 31_665 . ?
O7 Nb1 V2 136.8(3) 31_665 . ?
O7 Nb1 V2 44.4(2) . . ?
O14 Nb1 V2 77.26(6) . . ?
V2 Nb1 V2 150.22(11) 31_665 . ?
O2 Nb2 O9 103.0(4) . . ?
O2 Nb2 O12 100.9(4) . . ?
O9 Nb2 O12 94.4(4) . . ?
O2 Nb2 O8 99.5(3) . . ?
O9 Nb2 O8 87.0(3) . . ?
O12 Nb2 O8 158.7(3) . . ?
O2 Nb2 O11 102.3(3) . 18_556 ?
O9 Nb2 O11 153.3(3) . 18_556 ?
O12 Nb2 O11 88.9(3) . 18_556 ?
O8 Nb2 O11 80.7(3) . 18_556 ?
O2 Nb2 O15 171.7(3) . . ?
O9 Nb2 O15 84.5(3) . . ?
O12 Nb2 O15 74.7(3) . . ?
O8 Nb2 O15 84.3(2) . . ?
O11 Nb2 O15 70.9(3) 18_556 . ?
O2 Nb2 V2 103.2(3) . . ?
O9 Nb2 V2 122.1(3) . . ?
O12 Nb2 V2 129.2(3) . . ?
O8 Nb2 V2 38.21(19) . . ?
O11 Nb2 V2 42.5(2) 18_556 . ?
O15 Nb2 V2 75.24(17) . . ?
O3 Nb3 O11 101.6(3) . . ?
O3 Nb3 O11 101.6(3) . 18_556 ?
O11 Nb3 O11 96.6(4) . 18_556 ?
O3 Nb3 O13 101.8(3) . 18_556 ?
O11 Nb3 O13 155.9(3) . 18_556 ?
O11 Nb3 O13 84.2(3) 18_556 18_556 ?
O3 Nb3 O13 101.8(3) . . ?
O11 Nb3 O13 84.2(3) . . ?
O11 Nb3 O13 155.9(3) 18_556 . ?
O13 Nb3 O13 85.6(4) 18_556 . ?
O3 Nb3 O15 169.0(4) . . ?
O11 Nb3 O15 71.4(2) . . ?
O11 Nb3 O15 71.4(2) 18_556 . ?
O13 Nb3 O15 86.2(2) 18_556 . ?
O13 Nb3 O15 86.3(2) . . ?
O3 Nb3 V2 104.89(6) . 18_556 ?
O11 Nb3 V2 43.7(2) . 18_556 ?
O11 Nb3 V2 135.7(2) 18_556 18_556 ?
O13 Nb3 V2 123.3(2) 18_556 18_556 ?
O13 Nb3 V2 40.5(2) . 18_556 ?
O15 Nb3 V2 76.25(6) . 18_556 ?
O3 Nb3 V2 104.89(6) . . ?
O11 Nb3 V2 135.7(2) . . ?
O11 Nb3 V2 43.7(2) 18_556 . ?
O13 Nb3 V2 40.5(2) 18_556 . ?
O13 Nb3 V2 123.3(2) . . ?
O15 Nb3 V2 76.25(6) . . ?
V2 Nb3 V2 148.92(10) 18_556 . ?
O4 Nb4 O10 103.4(4) . . ?
O4 Nb4 O6 100.6(4) . . ?
O10 Nb4 O6 90.6(5) . . ?
O4 Nb4 O7 101.7(4) . . ?
O10 Nb4 O7 153.7(4) . . ?
O6 Nb4 O7 92.1(5) . . ?
O4 Nb4 O13 100.2(3) . 18_556 ?
O10 Nb4 O13 86.6(3) . 18_556 ?
O6 Nb4 O13 159.1(3) . 18_556 ?
O7 Nb4 O13 81.6(3) . 18_556 ?
O4 Nb4 O14 170.0(4) . . ?
O10 Nb4 O14 84.8(4) . . ?
O6 Nb4 O14 73.4(3) . . ?
O7 Nb4 O14 71.0(3) . . ?
O13 Nb4 O14 85.7(2) 18_556 . ?
O4 Nb4 V3 104.6(4) . . ?
O10 Nb4 V3 40.0(3) . . ?
O6 Nb4 V3 50.8(4) . . ?
O7 Nb4 V3 137.5(2) . . ?
O13 Nb4 V3 124.7(3) 18_556 . ?
O14 Nb4 V3 78.0(3) . . ?
O4 Nb4 V2 104.1(3) . . ?
O10 Nb4 V2 122.0(3) . . ?
O6 Nb4 V2 131.9(4) . . ?
O7 Nb4 V2 42.8(2) . . ?
O13 Nb4 V2 38.79(19) 18_556 . ?
O14 Nb4 V2 75.49(18) . . ?
V3 Nb4 V2 149.5(3) . . ?
Nb4 O6 Nb4 123.7(5) . 31_665 ?
Nb4 O6 V3 87.8(5) . . ?
Nb4 O6 V3 87.8(5) 31_665 . ?
Nb1 O7 Nb4 123.8(4) . . ?
Nb1 O7 V2 93.9(3) . . ?
Nb4 O7 V2 96.9(3) . . ?
V2 O8 Nb1 100.0(3) . . ?
V2 O8 Nb2 101.3(3) . . ?
Nb1 O8 Nb2 148.1(3) . . ?
Nb2 O9 Nb2 154.5(6) . 31_665 ?
V3 O10 Nb4 99.6(3) . 18_556 ?
V3 O10 Nb4 99.6(3) . . ?
Nb4 O10 Nb4 152.8(6) 18_556 . ?
Nb3 O11 Nb2 123.6(3) . 18_556 ?
Nb3 O11 V2 94.9(3) . 18_556 ?
Nb2 O11 V2 95.8(3) 18_556 18_556 ?
Nb2 O12 Nb2 121.1(5) 18_556 . ?
V2 O13 Nb3 98.1(3) 18_556 . ?
V2 O13 Nb4 100.5(3) 18_556 18_556 ?
Nb3 O13 Nb4 148.7(4) . 18_556 ?
V1 O14 Nb1 123.3(5) . . ?
V1 O14 Nb4 124.7(3) . . ?
Nb1 O14 Nb4 92.4(3) . . ?
V1 O14 Nb4 124.7(3) . 31_665 ?
Nb1 O14 Nb4 92.4(3) . 31_665 ?
Nb4 O14 Nb4 89.5(3) . 31_665 ?
V1 O15 Nb2 124.1(3) . 18_556 ?
V1 O15 Nb2 124.1(3) . . ?
Nb2 O15 Nb2 88.7(3) 18_556 . ?
V1 O15 Nb3 124.6(4) . . ?
Nb2 O15 Nb3 92.7(2) 18_556 . ?
Nb2 O15 Nb3 92.7(2) . . ?
O16 V3 O10 122.6(5) . . ?
O16 V3 O10 122.6(5) . 31_665 ?
O10 V3 O10 114.8(10) . 31_665 ?
O16 V3 O6 105.6(5) . . ?
O10 V3 O6 81.7(3) . . ?
O10 V3 O6 81.7(3) 31_665 . ?
O16 V3 O6 105.6(5) . 18_556 ?
O10 V3 O6 81.7(3) . 18_556 ?
O10 V3 O6 81.7(3) 31_665 18_556 ?
O6 V3 O6 148.8(10) . 18_556 ?
O16 V3 Nb4 120.1(3) . 18_556 ?
O10 V3 Nb4 40.38(16) . 18_556 ?
O10 V3 Nb4 102.8(6) 31_665 18_556 ?
O6 V3 Nb4 118.7(5) . 18_556 ?
O6 V3 Nb4 41.40(19) 18_556 18_556 ?
O16 V3 Nb4 120.1(3) . 31_665 ?
O10 V3 Nb4 102.8(6) . 31_665 ?
O10 V3 Nb4 40.37(16) 31_665 31_665 ?
O6 V3 Nb4 41.40(19) . 31_665 ?
O6 V3 Nb4 118.7(5) 18_556 31_665 ?
Nb4 V3 Nb4 119.8(6) 18_556 31_665 ?
O16 V3 Nb4 120.1(3) . 16_665 ?
O10 V3 Nb4 102.8(6) . 16_665 ?
O10 V3 Nb4 40.37(16) 31_665 16_665 ?
O6 V3 Nb4 118.7(5) . 16_665 ?
O6 V3 Nb4 41.40(19) 18_556 16_665 ?
Nb4 V3 Nb4 71.4(2) 18_556 16_665 ?
Nb4 V3 Nb4 79.4(3) 31_665 16_665 ?
O16 V3 Nb4 120.1(3) . . ?
O10 V3 Nb4 40.38(16) . . ?
O10 V3 Nb4 102.8(6) 31_665 . ?
O6 V3 Nb4 41.40(19) . . ?
O6 V3 Nb4 118.7(5) 18_556 . ?
Nb4 V3 Nb4 79.4(3) 18_556 . ?
Nb4 V3 Nb4 71.4(2) 31_665 . ?
Nb4 V3 Nb4 119.8(6) 16_665 . ?
N4 K1 N4 180.0 . 17_666 ?
N4 K1 N4 100.85(14) . 19_566 ?
N4 K1 N4 79.15(14) 17_666 19_566 ?
N4 K1 N4 79.15(14) . 3_655 ?
N4 K1 N4 100.85(14) 17_666 3_655 ?
N4 K1 N4 180.0(3) 19_566 3_655 ?
N4 K1 N4 128.6(4) . 2_665 ?
N4 K1 N4 51.4(4) 17_666 2_665 ?
N4 K1 N4 100.85(14) 19_566 2_665 ?
N4 K1 N4 79.15(14) 3_655 2_665 ?
N4 K1 N4 51.4(4) . 18_556 ?
N4 K1 N4 128.6(4) 17_666 18_556 ?
N4 K1 N4 79.15(14) 19_566 18_556 ?
N4 K1 N4 100.85(14) 3_655 18_556 ?
N4 K1 N4 180.0 2_665 18_556 ?
N4 K1 N4 100.86(14) . 20_656 ?
N4 K1 N4 79.15(14) 17_666 20_656 ?
N4 K1 N4 128.6(4) 19_566 20_656 ?
N4 K1 N4 51.4(4) 3_655 20_656 ?
N4 K1 N4 100.85(14) 2_665 20_656 ?
N4 K1 N4 79.15(14) 18_556 20_656 ?
N4 K1 N4 79.14(14) . 4_565 ?
N4 K1 N4 100.85(14) 17_666 4_565 ?
N4 K1 N4 51.4(4) 19_566 4_565 ?
N4 K1 N4 128.6(4) 3_655 4_565 ?
N4 K1 N4 79.15(14) 2_665 4_565 ?
N4 K1 N4 100.85(14) 18_556 4_565 ?
N4 K1 N4 180.0(3) 20_656 4_565 ?
N2 Cu1 N2 101.9(14) . 31_665 ?
N2 Cu1 N1 89.4(10) . . ?
N2 Cu1 N1 168.3(11) 31_665 . ?
N2 Cu1 N1 168.3(11) . 31_665 ?
N2 Cu1 N1 89.4(10) 31_665 31_665 ?
N1 Cu1 N1 79.1(14) . 31_665 ?
N2 Cu1 N2' 177.9(10) . 31_665 ?
N2 Cu1 N2' 76.1(10) 31_665 31_665 ?
N1 Cu1 N2' 92.6(11) . 31_665 ?
N1 Cu1 N2' 13.6(10) 31_665 31_665 ?
N2' Cu1 N2' 106.0(15) 31_665 . ?
N2 Cu1 N1' 96.3(7) . 31_665 ?
N2 Cu1 N1' 7.5(12) 31_665 31_665 ?
N1 Cu1 N1' 173.9(9) . 31_665 ?
N1 Cu1 N1' 95.2(9) 31_665 31_665 ?
N2' Cu1 N1' 81.7(9) 31_665 31_665 ?
N2' Cu1 N1' 171.1(10) . 31_665 ?
N2' Cu1 N1' 171.1(10) 31_665 . ?
N2' Cu1 N1' 81.7(9) . . ?
N1' Cu1 N1' 90.4(11) 31_665 . ?
N4 Cu2 N4 94.4(6) 18_556 . ?
N4 Cu2 N3 175.0(4) 18_556 . ?
N4 Cu2 N3 83.2(4) . . ?
N4 Cu2 N3 83.2(4) 18_556 18_556 ?
N4 Cu2 N3 175.0(4) . 18_556 ?
N3 Cu2 N3 98.8(6) . 18_556 ?
C1 N1 Cu1 105.1(17) . . ?
C1 N1 H1A 110.7 . . ?
Cu1 N1 H1A 110.7 . . ?
C1 N1 H1B 110.7 . . ?
Cu1 N1 H1B 110.7 . . ?
H1A N1 H1B 108.8 . . ?
N1 C1 C2 110(2) . . ?
N1 C1 H1C 109.7 . . ?
C2 C1 H1C 109.7 . . ?
N1 C1 H1D 109.7 . . ?
C2 C1 H1D 109.7 . . ?
H1C C1 H1D 108.2 . . ?
C1 C2 N2 105(2) . . ?
C1 C2 C3 116(2) . . ?
N2 C2 C3 115(2) . . ?
C1 C2 H2C 106.9 . . ?
N2 C2 H2C 106.9 . . ?
C3 C2 H2C 106.9 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 N2 Cu1 109.4(16) . . ?
C2 N2 H2A 109.8 . . ?
Cu1 N2 H2A 109.8 . . ?
C2 N2 H2B 109.8 . . ?
Cu1 N2 H2B 109.8 . . ?
H2A N2 H2B 108.2 . . ?
C1' N1' Cu1 103.4(19) . . ?
C1' N1' H1'A 111.1 . . ?
Cu1 N1' H1'A 111.1 . . ?
C1' N1' H1'B 111.1 . . ?
Cu1 N1' H1'B 111.1 . . ?
H1'A N1' H1'B 109.0 . . ?
N1' C1' C2' 116(2) . . ?
N1' C1' H1'C 108.3 . . ?
C2' C1' H1'C 108.3 . . ?
N1' C1' H1'D 108.3 . . ?
C2' C1' H1'D 108.3 . . ?
H1'C C1' H1'D 107.4 . . ?
C1' C2' N2' 106(2) . . ?
C1' C2' C3' 120.2(16) . . ?
N2' C2' C3' 118.9(15) . . ?
C1' C2' H2'C 102.9 . . ?
N2' C2' H2'C 102.9 . . ?
C3' C2' H2'C 102.9 . . ?
C2' C3' H3'A 109.5 . . ?
C2' C3' H3'B 109.5 . . ?
H3'A C3' H3'B 109.5 . . ?
C2' C3' H3'C 109.5 . . ?
H3'A C3' H3'C 109.5 . . ?
H3'B C3' H3'C 109.5 . . ?
C2' N2' Cu1 113.7(17) . . ?
C2' N2' H2'A 108.8 . . ?
Cu1 N2' H2'A 108.8 . . ?
C2' N2' H2'B 108.8 . . ?
Cu1 N2' H2'B 108.8 . . ?
H2'A N2' H2'B 107.7 . . ?
C4 N3 Cu2 113.2(9) . . ?
C4' N3 Cu2 103(2) . . ?
C4 N3 H3D 113.7 . . ?
C4' N3 H3D 107.0 . . ?
Cu2 N3 H3D 110.3 . . ?
C4 N3 H3E 100.7 . . ?
C4' N3 H3E 117.6 . . ?
Cu2 N3 H3E 110.0 . . ?
H3D N3 H3E 108.4 . . ?
N3 C4 C5 106.5(13) . . ?
N3 C4 H4B 110.4 . . ?
C5 C4 H4B 110.4 . . ?
N3 C4 H4C 110.4 . . ?
C5 C4 H4C 110.4 . . ?
H4B C4 H4C 108.6 . . ?
C4 C5 C6 107.1(14) . . ?
C4 C5 N4 110.3(14) . . ?
C6 C5 N4 112.1(14) . . ?
C4 C5 H5A 109.1 . . ?
C6 C5 H5A 109.1 . . ?
N4 C5 H5A 109.1 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C4' C5' 113(3) . . ?
N3 C4' H4'A 109.0 . . ?
C5' C4' H4'A 109.0 . . ?
N3 C4' H4'B 109.0 . . ?
C5' C4' H4'B 109.0 . . ?
H4'A C4' H4'B 107.8 . . ?
C4' C5' N4 99(3) . . ?
C4' C5' C6' 124.7(19) . . ?
N4 C5' C6' 121.8(18) . . ?
C4' C5' H5'A 102.8 . . ?
N4 C5' H5'A 102.8 . . ?
C6' C5' H5'A 102.8 . . ?
C5' C6' H6'A 109.5 . . ?
C5' C6' H6'B 109.5 . . ?
H6'A C6' H6'B 109.5 . . ?
C5' C6' H6'C 109.5 . . ?
H6'A C6' H6'C 109.5 . . ?
H6'B C6' H6'C 109.5 . . ?
C5' N4 Cu2 115(2) . . ?
C5 N4 Cu2 104.6(8) . . ?
C5' N4 K1 141(2) . . ?
C5 N4 K1 117.0(9) . . ?
Cu2 N4 K1 99.4(4) . . ?
C5 N4 H4A 123.0 . . ?
Cu2 N4 H4A 104.6 . . ?
K1 N4 H4A 105.0 . . ?

_refine_diff_density_max         1.550
_refine_diff_density_min         -1.864
_refine_diff_density_rms         0.194

