# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_k
_database_code_depnum_ccdc_archive 'CCDC 2378667'
loop_
_audit_author_name
_audit_author_address
'xiaobing cui'
;jilin university
China
;
_audit_update_record             
;
2024-08-21 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;
_audit_creation_date             2024-08-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(K0.5 Nb12 O45.75 Si V4.25), C24 H64 Cu4 K N16, C24 H72 Cu4 N16, 18(O)'
_chemical_formula_sum            'C48 H199 Cu8 K2 N32 Nb24 O109.50 Si2 V8.50'
_chemical_formula_weight         6282.91
_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'
N N 0.0311 0.0180 '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'
Si Si 0.2541 0.3302 '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'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -0.1121 2.4826 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 '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           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
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                   26.3310(12)
_cell_length_b                   26.3310(12)
_cell_length_c                   27.573(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19117(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9579
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      63.87
_cell_measurement_theta_min      3.36
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    16.827
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.2514
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1335 before and 0.0664 after correction.
The Ratio of minimum to maximum transmission is 0.3341.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Brownish-purple
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       Needle-like
_exptl_crystal_F_000             12258
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            28531
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        63.965
_diffrn_reflns_theta_max         63.965
_diffrn_reflns_theta_min         2.373
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3295
_reflns_number_total             4164
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         1.400
_refine_diff_density_min         -2.329
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       0.000016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4164
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0622
_refine_ls_restrained_S_all      1.088
_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)+(0.0919P)²+543.5092P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1753
_refine_ls_wR_factor_ref         0.1894
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C7, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\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(O14) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: K2(0.125) O1(0.25) V3(0.0625) C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
 C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) O4(0.0625) O3(0.25) O8(0.125)
5.a Ternary CH refined with riding coordinates:
 C31(H31), C32(H32), C36(H36)
5.b Secondary CH2 refined with riding coordinates:
 N27(H27A,H27B), N28(H28A,H28B), N29(H29A,H29B), C30(H30A,H30B)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C2(H2A,H2B,H2C)
;
_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
Nb1 Nb 0.17769(4) 0.12553(4) 0.000000 0.0323(4) Uani 1 2 d S T P . .
Nb2 Nb 0.15919(3) 0.24059(3) 0.06134(3) 0.0318(3) Uani 1 1 d . . . . .
Nb3 Nb 0.28307(3) 0.21693(3) 0.13134(5) 0.0367(4) Uani 1 2 d S T P . .
Nb4 Nb 0.30419(3) 0.10399(3) 0.06842(4) 0.0374(3) Uani 1 1 d . . . . .
Si5 Si 0.27977(11) 0.22023(11) 0.000000 0.0167(10) Uani 1 4 d S T P . .
Cu6 Cu 0.15823(8) -0.02063(8) 0.000000 0.0504(7) Uani 1 2 d S T P . .
Cu Cu 0.32268(8) 0.17732(8) 0.25779(11) 0.0681(8) Uani 1 2 d S T P . .
V8 V 0.20066(10) 0.14228(10) 0.10527(11) 0.0670(7) Uani 1 1 d . . . . .
O2 O 0.2187(3) 0.2092(3) 0.000000 0.0241(19) Uani 1 2 d S T P . .
O5 O 0.2115(3) 0.2146(3) 0.1102(3) 0.0353(16) Uani 1 1 d . . . . .
O7 O 0.3195(4) 0.0933(4) 0.000000 0.045(3) Uani 1 2 d S T P . .
O9 O 0.1465(3) 0.1640(3) 0.0535(3) 0.0377(17) Uani 1 1 d . . . . .
O10 O 0.1226(3) 0.2519(3) 0.000000 0.034(2) Uani 1 2 d S T P . .
O11 O 0.2295(2) 0.1054(2) 0.0497(3) 0.0347(17) Uani 1 1 d . . . . .
O12 O 0.2763(3) 0.2237(3) 0.1951(4) 0.049(3) Uani 1 2 d S T P . .
O13 O 0.1972(3) 0.3028(3) 0.0578(4) 0.034(2) Uani 1 2 d S T P . .
O15 O 0.3079(3) 0.0423(3) 0.0908(4) 0.058(2) Uani 1 1 d . . . . .
O16 O 0.3050(2) 0.1950(2) 0.0490(4) 0.029(2) Uani 1 2 d S T P . .
O17 O 0.1393(4) 0.0712(4) 0.000000 0.041(3) Uani 1 2 d S T P . .
O18 O 0.1113(3) 0.2569(3) 0.1029(3) 0.0432(19) Uani 1 1 d . . . . .
O20 O 0.2780(3) 0.1417(3) 0.1272(3) 0.054(2) Uani 1 1 d . . . . .
N23 N 0.1092(4) -0.0383(4) -0.0530(4) 0.054(3) Uani 1 1 d . . . . .
O24 O 0.3740(3) 0.1260(3) 0.0810(5) 0.059(4) Uani 1 2 d S T P . .
O25 O 0.1691(4) 0.1127(4) 0.1466(4) 0.077(3) Uani 1 1 d . . . . .
N27 N 0.2070(4) -0.0113(4) -0.0544(5) 0.073(4) Uani 1 1 d . . . . .
H27A H 0.222632 0.018469 -0.051158 0.088 Uiso 1 1 calc R U . . .
H27B H 0.230518 -0.035612 -0.053139 0.088 Uiso 1 1 calc R U . . .
N28 N 0.2575(5) 0.1637(5) 0.2900(5) 0.074(4) Uani 1 1 d . . . . .
H28A H 0.262685 0.152232 0.319990 0.089 Uiso 1 1 calc R U . . .
H28B H 0.239074 0.192010 0.291756 0.089 Uiso 1 1 calc R U . . .
N29 N 0.3091(7) 0.1099(5) 0.2263(5) 0.102(6) Uani 1 1 d . . . . .
H29A H 0.303960 0.114601 0.194740 0.123 Uiso 1 1 calc R U . . .
H29B H 0.336288 0.090165 0.229746 0.123 Uiso 1 1 calc R U . . .
C30 C 0.1816(7) -0.0132(7) -0.1007(8) 0.103(7) Uani 1 1 d . . . . .
H30A H 0.191791 0.015935 -0.119874 0.124 Uiso 1 1 calc R U . . .
H30B H 0.192077 -0.043570 -0.117844 0.124 Uiso 1 1 calc R U . . .
C31 C 0.2653(9) 0.0845(6) 0.2470(9) 0.107(7) Uani 1 1 d . U . . .
H31 H 0.277083 0.070312 0.277911 0.128 Uiso 1 1 calc R U . . .
C32 C 0.2306(7) 0.1243(6) 0.2599(6) 0.082(5) Uani 1 1 d . . . . .
H32 H 0.219831 0.140798 0.229754 0.098 Uiso 1 1 calc R U . . .
C36 C 0.1300(7) -0.0133(11) -0.0962(8) 0.124(8) Uani 1 1 d . . . . .
H36 H 0.122137 0.022609 -0.090421 0.149 Uiso 1 1 calc R U . . .
K1 K 0.000000 0.000000 0.000000 0.068(3) Uani 1 8 d S T P . .
K2 K 0.1316(4) 0.3684(4) 0.000000 0.104(6) Uani 0.5 4 d S T P . .
O1 O 0.1697(14) 0.4733(12) 0.000000 0.095(11) Uani 0.5 2 d S T P . .
V3 V 0.3911(4) 0.1089(4) 0.000000 0.059(5) Uani 0.25 4 d S T P . .
O6 O 0.3246(6) -0.0436(6) 0.1399(7) 0.156(7) Uani 1 1 d . . . . .
O14 O 0.3879(15) -0.0321(15) 0.2129(14) 0.350(18) Uani 1 1 d . U . . .
C1 C 0.1875(14) 0.0987(10) 0.2792(12) 0.081(10) Uani 0.5 1 d . . P . .
H1A H 0.197404 0.079705 0.307338 0.121 Uiso 0.5 1 calc R U P . .
H1B H 0.173991 0.076032 0.255181 0.121 Uiso 0.5 1 calc R U P . .
H1C H 0.162101 0.123164 0.288010 0.121 Uiso 0.5 1 calc R U P . .
C7 C 0.232(2) 0.0454(14) 0.2259(13) 0.128(18) Uani 0.5 1 d . U P . .
H7A H 0.235425 0.046004 0.191205 0.192 Uiso 0.5 1 calc R U P . .
H7B H 0.197705 0.051906 0.234831 0.192 Uiso 0.5 1 calc R U P . .
H7C H 0.242304 0.012588 0.237799 0.192 Uiso 0.5 1 calc R U P . .
C2 C 0.1038(9) -0.0237(8) -0.1436(8) 0.122(8) Uani 1 1 d . . . . .
H2A H 0.099519 -0.059694 -0.147611 0.182 Uiso 1 1 calc R U . . .
H2B H 0.123984 -0.010636 -0.169791 0.182 Uiso 1 1 calc R U . . .
H2C H 0.071120 -0.007518 -0.143808 0.182 Uiso 1 1 calc R U . . .
O4 O 0.4331(12) 0.0669(12) 0.000000 0.022(3) Uani 0.25 4 d S TU P . .
O3 O 0.4267(19) 0.0733(19) 0.158(2) 0.23(4) Uani 0.5 2 d S T P . .
O8 O 0.092(2) 0.408(2) 0.080(3) 0.100(4) Uani 0.25 2 d S TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 V8 2.998(3) . ?
Nb1 V8 2.998(3) 18 ?
Nb1 O2 2.454(8) . ?
Nb1 O9 1.970(7) 18 ?
Nb1 O9 1.970(7) . ?
Nb1 O11 2.006(7) 18 ?
Nb1 O11 2.006(7) . ?
Nb1 O17 1.751(9) . ?
Nb2 V8 3.059(3) . ?
Nb2 O2 2.449(6) . ?
Nb2 O5 2.045(7) . ?
Nb2 O9 2.055(7) . ?
Nb2 O10 1.969(5) . ?
Nb2 O13 1.922(3) . ?
Nb2 O18 1.756(7) . ?
Nb2 K2 3.836(11) . ?
Nb3 V8 3.015(3) . ?
Nb3 V8 3.015(3) 31 ?
Nb3 O5 1.974(7) 31 ?
Nb3 O5 1.974(7) . ?
Nb3 O12 1.776(12) . ?
Nb3 O16 2.414(10) . ?
Nb3 O20 1.989(8) 31 ?
Nb3 O20 1.989(8) . ?
Nb4 V8 3.079(3) . ?
Nb4 O7 1.949(3) . ?
Nb4 O11 2.033(7) . ?
Nb4 O15 1.739(7) . ?
Nb4 O16 2.455(6) . ?
Nb4 O20 2.022(9) . ?
Nb4 O24 1.958(5) . ?
Nb4 V3 2.969(8) . ?
Si5 O2 1.635(8) . ?
Si5 O2 1.634(8) 31 ?
Si5 O16 1.646(10) . ?
Si5 O16 1.646(10) 18 ?
Cu6 N23 2.004(11) 18 ?
Cu6 N23 2.004(11) . ?
Cu6 N27 1.989(12) 18 ?
Cu6 N27 1.989(12) . ?
Cu N28 1.965(13) . ?
Cu N28 1.965(14) 31 ?
Cu N29 2.007(15) 31 ?
Cu N29 2.007(15) . ?
V8 O5 1.932(7) . ?
V8 O9 2.097(8) . ?
V8 O11 1.966(8) . ?
V8 O20 2.125(9) . ?
V8 O25 1.611(10) . ?
O7 V3 1.931(13) . ?
O10 K2 3.077(13) . ?
O13 K2 2.915(16) . ?
N23 C36 1.47(2) . ?
N23 K1 3.380(11) . ?
O24 V3 2.322(15) . ?
N27 H27A 0.8900 . ?
N27 H27B 0.8900 . ?
N27 C30 1.44(2) . ?
N28 H28A 0.8900 . ?
N28 H28B 0.8900 . ?
N28 C32 1.508(18) . ?
N29 H29A 0.8900 . ?
N29 H29B 0.8900 . ?
N29 C31 1.45(2) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C30 C36 1.36(2) . ?
C31 H31 0.9800 . ?
C31 C32 1.44(3) . ?
C31 C7 1.47(4) . ?
C32 H32 0.9800 . ?
C32 C1 1.42(3) . ?
C36 H36 0.9800 . ?
C36 C2 1.50(3) . ?
K2 O1 2.94(3) . ?
K2 O1 2.94(3) 31 ?
K2 O8 2.65(7) 18 ?
K2 O8 2.65(7) . ?
V3 O4 1.56(5) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?

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
V8 Nb1 V8 151.08(10) . 18 ?
O2 Nb1 V8 77.24(6) . 18 ?
O2 Nb1 V8 77.24(6) . . ?
O9 Nb1 V8 137.2(2) . 18 ?
O9 Nb1 V8 44.2(2) . . ?
O9 Nb1 V8 44.2(2) 18 18 ?
O9 Nb1 V8 137.2(2) 18 . ?
O9 Nb1 O2 73.8(2) 18 . ?
O9 Nb1 O2 73.8(2) . . ?
O9 Nb1 O9 97.0(4) . 18 ?
O9 Nb1 O11 84.7(3) . . ?
O9 Nb1 O11 84.7(3) 18 18 ?
O9 Nb1 O11 158.8(3) 18 . ?
O9 Nb1 O11 158.8(3) . 18 ?
O11 Nb1 V8 40.5(2) 18 18 ?
O11 Nb1 V8 124.3(2) . 18 ?
O11 Nb1 V8 124.3(2) 18 . ?
O11 Nb1 V8 40.5(2) . . ?
O11 Nb1 O2 86.5(2) 18 . ?
O11 Nb1 O2 86.5(2) . . ?
O11 Nb1 O11 86.3(4) . 18 ?
O17 Nb1 V8 103.68(6) . 18 ?
O17 Nb1 V8 103.68(6) . . ?
O17 Nb1 O2 170.9(4) . . ?
O17 Nb1 O9 100.4(3) . 18 ?
O17 Nb1 O9 100.4(3) . . ?
O17 Nb1 O11 100.1(3) . 18 ?
O17 Nb1 O11 100.1(3) . . ?
V8 Nb2 K2 169.88(14) . . ?
O2 Nb2 V8 76.11(17) . . ?
O2 Nb2 K2 96.4(2) . . ?
O5 Nb2 V8 38.37(19) . . ?
O5 Nb2 O2 85.0(2) . . ?
O5 Nb2 O9 81.4(3) . . ?
O5 Nb2 K2 135.35(19) . . ?
O9 Nb2 V8 43.1(2) . . ?
O9 Nb2 O2 72.6(3) . . ?
O9 Nb2 K2 141.6(2) . . ?
O10 Nb2 V8 130.0(3) . . ?
O10 Nb2 O2 76.7(3) . . ?
O10 Nb2 O5 161.2(3) . . ?
O10 Nb2 O9 88.7(3) . . ?
O10 Nb2 K2 52.9(3) . . ?
O13 Nb2 V8 123.8(3) . . ?
O13 Nb2 O2 85.4(3) . . ?
O13 Nb2 O5 88.2(4) . . ?
O13 Nb2 O9 156.3(3) . . ?
O13 Nb2 O10 94.7(4) . . ?
O13 Nb2 K2 47.8(3) . . ?
O18 Nb2 V8 101.8(3) . . ?
O18 Nb2 O2 172.7(3) . . ?
O18 Nb2 O5 97.7(3) . . ?
O18 Nb2 O9 101.0(3) . . ?
O18 Nb2 O10 99.9(3) . . ?
O18 Nb2 O13 101.4(4) . . ?
O18 Nb2 K2 86.4(3) . . ?
V8 Nb3 V8 151.84(12) 31 . ?
O5 Nb3 V8 125.1(2) . 31 ?
O5 Nb3 V8 39.0(2) 31 31 ?
O5 Nb3 V8 39.0(2) . . ?
O5 Nb3 V8 125.1(2) 31 . ?
O5 Nb3 O5 88.4(4) . 31 ?
O5 Nb3 O16 86.8(3) 31 . ?
O5 Nb3 O16 86.8(3) . . ?
O5 Nb3 O20 83.6(3) . . ?
O5 Nb3 O20 83.6(3) 31 31 ?
O5 Nb3 O20 159.5(3) . 31 ?
O5 Nb3 O20 159.5(3) 31 . ?
O12 Nb3 V8 103.25(7) . . ?
O12 Nb3 V8 103.25(7) . 31 ?
O12 Nb3 O5 101.5(3) . 31 ?
O12 Nb3 O5 101.5(3) . . ?
O12 Nb3 O16 168.4(4) . . ?
O12 Nb3 O20 98.6(4) . 31 ?
O12 Nb3 O20 98.6(4) . . ?
O16 Nb3 V8 77.99(7) . . ?
O16 Nb3 V8 77.99(7) . 31 ?
O20 Nb3 V8 44.7(3) 31 31 ?
O20 Nb3 V8 44.7(3) . . ?
O20 Nb3 V8 138.3(3) . 31 ?
O20 Nb3 V8 138.3(3) 31 . ?
O20 Nb3 O16 73.9(3) 31 . ?
O20 Nb3 O16 73.9(3) . . ?
O20 Nb3 O20 97.5(5) 31 . ?
O7 Nb4 V8 123.3(3) . . ?
O7 Nb4 O11 87.5(4) . . ?
O7 Nb4 O16 85.8(4) . . ?
O7 Nb4 O20 156.5(4) . . ?
O7 Nb4 O24 91.1(5) . . ?
O7 Nb4 V3 39.8(3) . . ?
O11 Nb4 V8 38.9(2) . . ?
O11 Nb4 O16 86.3(2) . . ?
O11 Nb4 V3 125.7(3) . . ?
O15 Nb4 V8 103.8(3) . . ?
O15 Nb4 O7 101.3(4) . . ?
O15 Nb4 O11 99.3(3) . . ?
O15 Nb4 O16 171.0(4) . . ?
O15 Nb4 O20 101.2(4) . . ?
O15 Nb4 O24 99.3(4) . . ?
O15 Nb4 V3 102.8(4) . . ?
O16 Nb4 V8 76.15(18) . . ?
O16 Nb4 V3 79.2(3) . . ?
O20 Nb4 V8 43.4(3) . . ?
O20 Nb4 O11 82.2(3) . . ?
O20 Nb4 O16 72.5(3) . . ?
O20 Nb4 V3 138.7(2) . . ?
O24 Nb4 V8 132.5(4) . . ?
O24 Nb4 O11 161.3(3) . . ?
O24 Nb4 O16 75.0(3) . . ?
O24 Nb4 O20 91.9(5) . . ?
O24 Nb4 V3 51.4(4) . . ?
V3 Nb4 V8 151.4(3) . . ?
O2 Si5 O2 110.4(6) 31 . ?
O2 Si5 O16 109.0(2) 31 18 ?
O2 Si5 O16 109.0(2) . 18 ?
O2 Si5 O16 109.0(2) 31 . ?
O2 Si5 O16 109.0(2) . . ?
O16 Si5 O16 110.3(7) . 18 ?
N23 Cu6 N23 93.6(6) . 18 ?
N27 Cu6 N23 84.0(5) . . ?
N27 Cu6 N23 173.6(4) 18 . ?
N27 Cu6 N23 84.0(5) 18 18 ?
N27 Cu6 N23 173.6(4) . 18 ?
N27 Cu6 N27 97.8(8) 18 . ?
N28 Cu N28 96.5(7) 31 . ?
N28 Cu N29 178.7(6) 31 . ?
N28 Cu N29 178.7(6) . 31 ?
N28 Cu N29 83.1(7) 31 31 ?
N28 Cu N29 83.1(7) . . ?
N29 Cu N29 97.4(11) 31 . ?
Nb1 V8 Nb2 70.68(7) . . ?
Nb1 V8 Nb3 118.17(9) . . ?
Nb1 V8 Nb4 79.10(8) . . ?
Nb2 V8 Nb4 117.54(9) . . ?
Nb3 V8 Nb2 78.44(7) . . ?
Nb3 V8 Nb4 69.81(6) . . ?
O5 V8 Nb1 104.1(2) . . ?
O5 V8 Nb2 41.1(2) . . ?
O5 V8 Nb3 40.0(2) . . ?
O5 V8 Nb4 102.5(2) . . ?
O5 V8 O9 83.1(3) . . ?
O5 V8 O11 119.1(3) . . ?
O5 V8 O20 81.1(3) . . ?
O9 V8 Nb1 40.9(2) . . ?
O9 V8 Nb2 42.00(19) . . ?
O9 V8 Nb3 118.3(2) . . ?
O9 V8 Nb4 117.8(2) . . ?
O9 V8 O20 148.0(3) . . ?
O11 V8 Nb1 41.5(2) . . ?
O11 V8 Nb2 104.4(2) . . ?
O11 V8 Nb3 103.3(2) . . ?
O11 V8 Nb4 40.5(2) . . ?
O11 V8 O9 82.4(3) . . ?
O11 V8 O20 81.3(3) . . ?
O20 V8 Nb1 117.9(3) . . ?
O20 V8 Nb2 117.4(2) . . ?
O20 V8 Nb3 41.1(2) . . ?
O20 V8 Nb4 40.8(2) . . ?
O25 V8 Nb1 120.7(4) . . ?
O25 V8 Nb2 120.3(4) . . ?
O25 V8 Nb3 121.2(4) . . ?
O25 V8 Nb4 122.1(4) . . ?
O25 V8 O5 120.2(5) . . ?
O25 V8 O9 105.2(4) . . ?
O25 V8 O11 120.7(5) . . ?
O25 V8 O20 106.8(5) . . ?
Nb2 O2 Nb1 91.2(2) 18 . ?
Nb2 O2 Nb1 91.2(2) . . ?
Nb2 O2 Nb2 87.4(3) . 18 ?
Si5 O2 Nb1 126.3(5) . . ?
Si5 O2 Nb2 124.7(3) . 18 ?
Si5 O2 Nb2 124.7(3) . . ?
Nb3 O5 Nb2 145.8(4) . . ?
V8 O5 Nb2 100.6(3) . . ?
V8 O5 Nb3 101.1(3) . . ?
Nb4 O7 Nb4 150.8(6) 18 . ?
V3 O7 Nb4 99.9(3) . . ?
V3 O7 Nb4 99.9(3) . 18 ?
Nb1 O9 Nb2 121.0(3) . . ?
Nb1 O9 V8 94.9(3) . . ?
Nb2 O9 V8 94.9(3) . . ?
Nb2 O10 Nb2 118.4(4) 18 . ?
Nb2 O10 K2 96.5(3) . . ?
Nb2 O10 K2 96.5(3) 18 . ?
Nb1 O11 Nb4 146.7(4) . . ?
V8 O11 Nb1 98.0(3) . . ?
V8 O11 Nb4 100.7(3) . . ?
Nb2 O13 Nb2 152.2(6) 31 . ?
Nb2 O13 K2 103.0(3) 31 . ?
Nb2 O13 K2 103.0(3) . . ?
Nb3 O16 Nb4 91.5(3) . 31 ?
Nb3 O16 Nb4 91.5(3) . . ?
Nb4 O16 Nb4 88.3(3) . 31 ?
Si5 O16 Nb3 125.3(5) . . ?
Si5 O16 Nb4 124.7(3) . . ?
Si5 O16 Nb4 124.7(3) . 31 ?
Nb3 O20 Nb4 120.8(4) . . ?
Nb3 O20 V8 94.2(4) . . ?
Nb4 O20 V8 95.9(4) . . ?
Cu6 N23 K1 99.4(4) . . ?
C36 N23 Cu6 104.4(10) . . ?
C36 N23 K1 122.2(10) . . ?
Nb4 O24 Nb4 121.7(5) 31 . ?
Nb4 O24 V3 87.4(5) 31 . ?
Nb4 O24 V3 87.4(5) . . ?
Cu6 N27 H27A 109.4 . . ?
Cu6 N27 H27B 109.4 . . ?
H27A N27 H27B 108.0 . . ?
C30 N27 Cu6 111.2(9) . . ?
C30 N27 H27A 109.4 . . ?
C30 N27 H27B 109.4 . . ?
Cu N28 H28A 110.4 . . ?
Cu N28 H28B 110.4 . . ?
H28A N28 H28B 108.6 . . ?
C32 N28 Cu 106.7(10) . . ?
C32 N28 H28A 110.4 . . ?
C32 N28 H28B 110.4 . . ?
Cu N29 H29A 109.1 . . ?
Cu N29 H29B 109.1 . . ?
H29A N29 H29B 107.9 . . ?
C31 N29 Cu 112.3(12) . . ?
C31 N29 H29A 109.1 . . ?
C31 N29 H29B 109.1 . . ?
N27 C30 H30A 109.1 . . ?
N27 C30 H30B 109.1 . . ?
H30A C30 H30B 107.8 . . ?
C36 C30 N27 112.5(17) . . ?
C36 C30 H30A 109.1 . . ?
C36 C30 H30B 109.1 . . ?
N29 C31 H31 105.4 . . ?
N29 C31 C7 130(3) . . ?
C32 C31 N29 105.5(14) . . ?
C32 C31 H31 105.4 . . ?
C32 C31 C7 104(2) . . ?
C7 C31 H31 105.4 . . ?
N28 C32 H32 107.3 . . ?
C31 C32 N28 109.8(15) . . ?
C31 C32 H32 107.3 . . ?
C1 C32 N28 119.7(19) . . ?
C1 C32 C31 104.7(19) . . ?
C1 C32 H32 107.3 . . ?
N23 C36 H36 102.8 . . ?
N23 C36 C2 117.0(18) . . ?
C30 C36 N23 116.4(18) . . ?
C30 C36 H36 102.8 . . ?
C30 C36 C2 112(2) . . ?
C2 C36 H36 102.8 . . ?
N23 K1 N23 79.23(15) 20 17 ?
N23 K1 N23 100.77(15) . 19 ?
N23 K1 N23 180.0(5) 3 19 ?
N23 K1 N23 100.77(15) 3 17 ?
N23 K1 N23 100.77(15) 2 19 ?
N23 K1 N23 51.2(4) 20 3 ?
N23 K1 N23 79.23(15) 2 3 ?
N23 K1 N23 51.2(4) 2 17 ?
N23 K1 N23 100.77(15) . 20 ?
N23 K1 N23 79.23(15) . 3 ?
N23 K1 N23 79.23(15) . 4 ?
N23 K1 N23 128.8(4) 4 3 ?
N23 K1 N23 180.0(4) 20 4 ?
N23 K1 N23 100.77(15) 18 3 ?
N23 K1 N23 128.8(4) . 2 ?
N23 K1 N23 128.8(4) 20 19 ?
N23 K1 N23 100.77(15) 20 2 ?
N23 K1 N23 79.23(15) 18 19 ?
N23 K1 N23 79.23(15) 4 2 ?
N23 K1 N23 180.0 . 17 ?
N23 K1 N23 51.2(4) . 18 ?
N23 K1 N23 100.77(15) 4 17 ?
N23 K1 N23 79.23(15) 20 18 ?
N23 K1 N23 128.8(4) 18 17 ?
N23 K1 N23 100.77(15) 4 18 ?
N23 K1 N23 79.23(15) 19 17 ?
N23 K1 N23 180.0(5) 2 18 ?
N23 K1 N23 51.2(4) 4 19 ?
Nb2 K2 Nb2 58.22(18) 31 . ?
Nb2 K2 Nb2 58.22(18) 18 16_554 ?
Nb2 K2 Nb2 52.34(16) 31 16_554 ?
Nb2 K2 Nb2 82.1(3) 16_554 . ?
Nb2 K2 Nb2 82.1(3) 31 18 ?
Nb2 K2 Nb2 52.33(16) 18 . ?
O10 K2 Nb2 30.67(13) . . ?
O10 K2 Nb2 30.67(13) 31 16_554 ?
O10 K2 Nb2 83.1(3) 31 18 ?
O10 K2 Nb2 83.1(3) . 31 ?
O10 K2 Nb2 30.67(13) . 18 ?
O10 K2 Nb2 30.67(13) 31 31 ?
O10 K2 Nb2 83.1(3) 31 . ?
O10 K2 Nb2 83.1(3) . 16_554 ?
O10 K2 O10 98.9(5) . 31 ?
O13 K2 Nb2 67.0(3) 18 31 ?
O13 K2 Nb2 67.0(3) . 16_554 ?
O13 K2 Nb2 29.24(10) . 31 ?
O13 K2 Nb2 29.24(10) 18 16_554 ?
O13 K2 Nb2 29.24(10) 18 18 ?
O13 K2 Nb2 67.0(3) 18 . ?
O13 K2 Nb2 29.24(10) . . ?
O13 K2 Nb2 67.0(3) . 18 ?
O13 K2 O10 57.0(3) . . ?
O13 K2 O10 57.0(3) 18 . ?
O13 K2 O10 57.0(3) 18 31 ?
O13 K2 O10 57.0(3) . 31 ?
O13 K2 O13 66.3(5) 18 . ?
O13 K2 O1 110.8(6) 18 31 ?
O13 K2 O1 110.8(6) 18 . ?
O13 K2 O1 110.8(6) . 31 ?
O13 K2 O1 110.8(6) . . ?
O1 K2 Nb2 139.5(6) 31 31 ?
O1 K2 Nb2 83.0(7) . 31 ?
O1 K2 Nb2 83.0(7) 31 . ?
O1 K2 Nb2 83.0(7) . 16_554 ?
O1 K2 Nb2 139.5(6) . . ?
O1 K2 Nb2 83.0(7) 31 18 ?
O1 K2 Nb2 139.5(6) . 18 ?
O1 K2 Nb2 139.5(6) 31 16_554 ?
O1 K2 O10 164.5(9) . . ?
O1 K2 O10 65.6(8) 31 . ?
O1 K2 O10 164.5(9) 31 31 ?
O1 K2 O10 65.6(8) . 31 ?
O1 K2 O1 129.9(16) 31 . ?
O8 K2 Nb2 93.0(14) . 31 ?
O8 K2 Nb2 141.8(10) 18 . ?
O8 K2 Nb2 93.0(14) 18 18 ?
O8 K2 Nb2 141.8(10) 18 31 ?
O8 K2 Nb2 93.0(14) 18 16_554 ?
O8 K2 Nb2 93.0(14) . . ?
O8 K2 Nb2 141.8(10) . 16_554 ?
O8 K2 Nb2 141.8(10) . 18 ?
O8 K2 O10 111.2(9) . . ?
O8 K2 O10 111.2(9) 18 . ?
O8 K2 O10 111.2(9) . 31 ?
O8 K2 O10 111.2(9) 18 31 ?
O8 K2 O13 90.6(16) 18 18 ?
O8 K2 O13 156.9(17) 18 . ?
O8 K2 O13 156.9(17) . 18 ?
O8 K2 O13 90.6(16) . . ?
O8 K2 O1 76.4(7) 18 31 ?
O8 K2 O1 76.4(7) 18 . ?
O8 K2 O1 76.4(7) . 31 ?
O8 K2 O1 76.4(7) . . ?
O8 K2 O8 113(3) 18 . ?
Nb4 V3 Nb4 118.1(5) 18 31 ?
Nb4 V3 Nb4 70.3(2) 31 . ?
Nb4 V3 Nb4 78.9(2) 31 16_554 ?
Nb4 V3 Nb4 78.9(2) 18 . ?
Nb4 V3 Nb4 70.3(2) 18 16_554 ?
Nb4 V3 Nb4 118.1(5) 16_554 . ?
O7 V3 Nb4 101.9(5) . 31 ?
O7 V3 Nb4 101.9(5) 31 18 ?
O7 V3 Nb4 40.30(15) . . ?
O7 V3 Nb4 40.30(15) . 18 ?
O7 V3 Nb4 101.9(5) . 16_554 ?
O7 V3 Nb4 101.9(5) 31 . ?
O7 V3 Nb4 40.30(15) 31 31 ?
O7 V3 Nb4 40.30(15) 31 16_554 ?
O7 V3 O7 114.5(9) 31 . ?
O7 V3 O24 81.4(3) 31 . ?
O7 V3 O24 81.4(3) . . ?
O7 V3 O24 81.4(3) 31 18 ?
O7 V3 O24 81.4(3) . 18 ?
O24 V3 Nb4 41.20(17) . . ?
O24 V3 Nb4 41.20(17) . 31 ?
O24 V3 Nb4 118.0(5) . 18 ?
O24 V3 Nb4 41.20(17) 18 18 ?
O24 V3 Nb4 118.0(5) 18 . ?
O24 V3 Nb4 118.0(5) . 16_554 ?
O24 V3 Nb4 118.0(5) 18 31 ?
O24 V3 Nb4 41.20(17) 18 16_554 ?
O24 V3 O24 148.1(9) 18 . ?
O4 V3 Nb4 121.0(2) . . ?
O4 V3 Nb4 121.0(2) . 16_554 ?
O4 V3 Nb4 121.0(2) . 31 ?
O4 V3 Nb4 121.0(2) . 18 ?
O4 V3 O7 122.8(5) . . ?
O4 V3 O7 122.8(5) . 31 ?
O4 V3 O24 106.0(4) . . ?
O4 V3 O24 106.0(4) . 18 ?
C32 C1 H1A 109.5 . . ?
C32 C1 H1B 109.5 . . ?
C32 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C31 C7 H7A 109.5 . . ?
C31 C7 H7B 109.5 . . ?
C31 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C36 C2 H2A 109.5 . . ?
C36 C2 H2B 109.5 . . ?
C36 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

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
Cu6 N23 C36 C30 38(2) . . . . ?
Cu6 N23 C36 C2 174.3(17) . . . . ?
Cu6 N27 C30 C36 9(2) . . . . ?
Cu N28 C32 C31 45.4(17) . . . . ?
Cu N28 C32 C1 167(2) . . . . ?
Cu N29 C31 C32 33.9(19) . . . . ?
Cu N29 C31 C7 157(3) . . . . ?
O2 Si5 O2 Nb1 180.0 31 . . . ?
O2 Si5 O2 Nb2 57.2(4) 31 . . 18 ?
O2 Si5 O2 Nb2 -57.2(4) 31 . . . ?
O2 Si5 O16 Nb3 -60.3(3) . . . . ?
O2 Si5 O16 Nb3 60.3(3) 31 . . . ?
O2 Si5 O16 Nb4 61.8(6) . . . . ?
O2 Si5 O16 Nb4 -177.6(4) 31 . . . ?
O2 Si5 O16 Nb4 177.6(4) . . . 31 ?
O2 Si5 O16 Nb4 -61.8(6) 31 . . 31 ?
O16 Si5 O2 Nb1 60.2(3) 18 . . . ?
O16 Si5 O2 Nb1 -60.2(3) . . . . ?
O16 Si5 O2 Nb2 -62.6(6) 18 . . 18 ?
O16 Si5 O2 Nb2 62.6(6) . . . . ?
O16 Si5 O2 Nb2 177.0(4) . . . 18 ?
O16 Si5 O2 Nb2 -177.0(4) 18 . . . ?
O16 Si5 O16 Nb3 180.000(0) 18 . . . ?
O16 Si5 O16 Nb4 57.9(4) 18 . . 31 ?
O16 Si5 O16 Nb4 -57.9(4) 18 . . . ?
N27 C30 C36 N23 -32(3) . . . . ?
N27 C30 C36 C2 -170.7(17) . . . . ?
N29 C31 C32 N28 -51(2) . . . . ?
N29 C31 C32 C1 179(2) . . . . ?
K1 N23 C36 C30 148.9(16) . . . . ?
K1 N23 C36 C2 -74(2) . . . . ?
C7 C31 C32 N28 170(2) . . . . ?
C7 C31 C32 C1 40(3) . . . . ?

_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_k_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2378668'
loop_
_audit_author_name
_audit_author_address
'xiaobing cui'
;jilin university
China
;
_audit_update_record             
;
2024-08-21 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT971_k                   
;
PROBLEM: Check Calcd Resid. Dens. 1.78Ang From O19 4.22 eA-3 
RESPONSE: There exists severe disorder around O19 which can not 
be solved.
;

# end Validation Reply Form

_audit_creation_date             2024-08-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(C12 H36 Cu2 K0.5 N8 Nb12 O45 P V2), C24 H64 Cu4 K N16, 19(O)'
_chemical_formula_sum            'C48 H214 Cu8 K2 N32 Nb24 O109 P2 V4'
_chemical_formula_weight         6066.56
_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'
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'
Cu Cu 0.3201 1.2651 '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'
K K 0.2009 0.2494 '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           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
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                   26.3917(6)
_cell_length_b                   26.3917(6)
_cell_length_c                   27.4474(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19117.7(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    299.00
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.44
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.585
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5968
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0655 before and 0.0538 after correction.
The Ratio of minimum to maximum transmission is 0.8009.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Brownish-Purple
_exptl_crystal_density_diffrn    2.108
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       Needle-like
_exptl_crystal_F_000             11896
_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  0.0474
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            36985
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.365
_diffrn_reflns_theta_min         2.440
_diffrn_ambient_temperature      299.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3734
_reflns_number_total             4613
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         4.016
_refine_diff_density_min         -1.641
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.00003(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4613
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0642
_refine_ls_restrained_S_all      1.114
_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)+(0.1102P)²+343.4725P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1778
_refine_ls_wR_factor_ref         0.2061
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: V8(0.5) O15(0.5) K16(0.125) O18(0.25) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) O19(0.25) O16(0.125)
3.a Ternary CH refined with riding coordinates:
 C16(H16), C6(H6), C7(H7)
3.b Secondary CH2 refined with riding coordinates:
 N5(H5A,H5B), C11(H11A,H11B), N3(H3A,H3B), N1(H1A,H1B)
3.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C)
;
_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
Nb1 Nb 0.15897(3) 0.24039(3) 0.43712(3) 0.0341(3) Uani 1 1 d . . . . .
P2 P 0.28014(8) 0.21986(8) 0.500000 0.0161(6) Uani 1 4 d S T P . .
Nb3 Nb 0.17779(4) 0.12396(4) 0.500000 0.0394(3) Uani 1 2 d S T P . .
Nb4 Nb 0.30425(3) 0.10221(3) 0.43151(3) 0.0388(3) Uani 1 1 d . . . . .
Nb5 Nb 0.28297(3) 0.21703(3) 0.36767(4) 0.0400(3) Uani 1 2 d S T P . .
Cu6 Cu 0.15810(6) -0.02158(6) 0.500000 0.0551(5) Uani 1 2 d S T P . .
V8 V 0.20196(10) 0.14237(10) 0.39598(10) 0.0319(6) Uani 0.5 1 d . . P . .
Cu7 Cu 0.32271(6) 0.17729(6) 0.24286(7) 0.0650(6) Uani 1 2 d S T P . .
O2 O 0.2204(3) 0.2095(3) 0.500000 0.0311(16) Uani 1 2 d S T P . .
O3 O 0.2296(2) 0.1048(2) 0.4502(2) 0.0365(12) Uani 1 1 d . . . . .
O4 O 0.2847(2) 0.2882(2) 0.3897(2) 0.0382(12) Uani 1 1 d . . . . .
O5 O 0.1468(2) 0.1648(2) 0.4472(2) 0.0426(14) Uani 1 1 d . . . . .
O6 O 0.1256(3) 0.2526(3) 0.500000 0.0387(18) Uani 1 2 d S T P . .
O7 O 0.3190(3) 0.0930(3) 0.500000 0.044(2) Uani 1 2 d S T P . .
O9 O 0.1970(2) 0.3030(2) 0.4412(3) 0.0375(18) Uani 1 2 d S T P . .
O10 O 0.1107(2) 0.2561(2) 0.3957(2) 0.0485(15) Uani 1 1 d . . . . .
O11 O 0.2802(3) 0.1419(2) 0.3734(2) 0.0513(16) Uani 1 1 d . . . . .
O12 O 0.3738(2) 0.1262(2) 0.4189(3) 0.046(2) Uani 1 2 d S T P . .
O13 O 0.3082(3) 0.0403(2) 0.4090(3) 0.0584(18) Uani 1 1 d . . . . .
O14 O 0.3044(2) 0.1956(2) 0.4531(3) 0.0332(16) Uani 1 2 d S T P . .
O1 O 0.1389(3) 0.0701(3) 0.500000 0.045(2) Uani 1 2 d S T P . .
N4 N 0.1088(4) -0.0389(4) 0.5527(4) 0.063(2) Uani 1 1 d . . . . .
N5 N 0.2070(4) -0.0115(3) 0.5555(4) 0.075(3) Uani 1 1 d . . . . .
H5A H 0.230436 -0.035766 0.554956 0.090 Uiso 1 1 calc R U . . .
H5B H 0.222590 0.018225 0.552284 0.090 Uiso 1 1 calc R U . . .
C11 C 0.1804(6) -0.0129(7) 0.6009(6) 0.103(5) Uani 1 1 d . . . . .
H11A H 0.192040 -0.042178 0.619126 0.123 Uiso 1 1 calc R U . . .
H11B H 0.189381 0.017008 0.619427 0.123 Uiso 1 1 calc R U . . .
C16 C 0.1278(6) -0.0153(12) 0.5977(7) 0.167(12) Uani 1 1 d . . . . .
H16 H 0.119277 0.020377 0.592123 0.200 Uiso 1 1 calc R U . . .
C18 C 0.1029(7) -0.0248(8) 0.6427(8) 0.129(7) Uani 1 1 d . . . . .
H18A H 0.066915 -0.022978 0.637981 0.193 Uiso 1 1 calc R U . . .
H18B H 0.113116 0.000151 0.666161 0.193 Uiso 1 1 calc R U . . .
H18C H 0.111889 -0.057921 0.654207 0.193 Uiso 1 1 calc R U . . .
O8 O 0.2763(3) 0.2237(3) 0.3046(3) 0.049(2) Uani 1 2 d S T P . .
O15 O 0.1698(4) 0.1133(4) 0.3551(4) 0.036(2) Uani 0.5 1 d . . P . .
N3 N 0.2575(4) 0.1632(4) 0.2090(3) 0.069(3) Uani 1 1 d . . . . .
H3A H 0.239516 0.191522 0.205946 0.083 Uiso 1 1 calc R U . . .
H3B H 0.263231 0.150560 0.179475 0.083 Uiso 1 1 calc R U . . .
C6 C 0.2289(6) 0.1250(5) 0.2400(5) 0.079(4) Uani 1 1 d . . . . .
H6 H 0.216519 0.142445 0.269142 0.095 Uiso 1 1 calc R U . . .
C7 C 0.2665(8) 0.0861(5) 0.2555(6) 0.102(6) Uani 1 1 d . . . . .
H7 H 0.277941 0.070792 0.224896 0.123 Uiso 1 1 calc R U . . .
N1 N 0.3120(5) 0.1107(4) 0.2749(4) 0.086(4) Uani 1 1 d . . . . .
H1A H 0.338832 0.090929 0.269824 0.103 Uiso 1 1 calc R U . . .
H1B H 0.308657 0.115087 0.306915 0.103 Uiso 1 1 calc R U . . .
K16 K 0.1334(3) 0.3666(3) 0.500000 0.068(3) Uani 0.5 4 d S T P . .
K17 K 0.000000 0.000000 0.500000 0.074(2) Uani 1 8 d S T P . .
O17 O 0.1678(13) 0.4719(10) 0.500000 0.213(13) Uani 1 2 d S T P . .
O18 O 0.0937(12) 0.4063(12) 0.4165(11) 0.125(13) Uani 0.5 2 d S T P . .
O20 O 0.3270(5) -0.0459(4) 0.3623(5) 0.131(5) Uani 1 1 d . . . . .
O21 O 0.3876(8) 0.0394(10) 0.2187(7) 0.234(11) Uani 1 1 d . . . . .
C2 C 0.1895(11) 0.1006(10) 0.2193(9) 0.075(7) Uani 0.5 1 d . . P . .
H2A H 0.161224 0.123331 0.216619 0.112 Uiso 0.5 1 calc R U P . .
H2B H 0.180181 0.072118 0.239093 0.112 Uiso 0.5 1 calc R U P . .
H2C H 0.199031 0.089020 0.187426 0.112 Uiso 0.5 1 calc R U P . .
C4 C 0.2345(17) 0.0466(12) 0.2781(11) 0.120(14) Uani 0.5 1 d . . P . .
H4A H 0.224848 0.057109 0.310280 0.180 Uiso 0.5 1 calc R U P . .
H4B H 0.253272 0.015454 0.280096 0.180 Uiso 0.5 1 calc R U P . .
H4C H 0.204738 0.041471 0.258683 0.180 Uiso 0.5 1 calc R U P . .
O19 O 0.0366(9) 0.5115(10) 0.500000 0.123(12) Uani 0.5 2 d S T P A 1
O16 O -0.074(2) 0.586(2) 3.836(2) 0.06(2) Uani 0.125 1 d . . P B -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
Nb1 V8 3.042(3) . ?
Nb1 O2 2.504(5) . ?
Nb1 O4 2.019(6) 31 ?
Nb1 O5 2.040(6) . ?
Nb1 O6 1.965(4) . ?
Nb1 O9 1.937(2) . ?
Nb1 O10 1.757(6) . ?
Nb1 K16 3.813(7) . ?
P2 O2 1.600(7) 31 ?
P2 O2 1.600(7) . ?
P2 O14 1.574(8) . ?
P2 O14 1.574(8) 18_556 ?
Nb3 V8 2.965(3) 18_556 ?
Nb3 V8 2.965(3) . ?
Nb3 O2 2.523(7) . ?
Nb3 O3 1.998(6) . ?
Nb3 O3 1.998(6) 18_556 ?
Nb3 O5 1.983(6) 18_556 ?
Nb3 O5 1.983(6) . ?
Nb3 O1 1.753(8) . ?
Nb4 V8 3.060(3) . ?
Nb4 O3 2.038(5) . ?
Nb4 O7 1.935(2) . ?
Nb4 O11 2.011(7) . ?
Nb4 O12 1.973(4) . ?
Nb4 O13 1.751(6) . ?
Nb4 O14 2.535(5) . ?
Nb5 V8 3.010(3) 31 ?
Nb5 V8 3.010(3) . ?
Nb5 O4 1.974(6) . ?
Nb5 O4 1.974(6) 31 ?
Nb5 O11 1.989(6) 31 ?
Nb5 O11 1.989(6) . ?
Nb5 O14 2.477(8) . ?
Nb5 O8 1.750(9) . ?
Cu6 N4 1.998(10) . ?
Cu6 N4 1.998(10) 18_556 ?
Cu6 N5 2.015(10) 18_556 ?
Cu6 N5 2.015(10) . ?
V8 O3 1.933(6) . ?
V8 O4 1.950(6) 31 ?
V8 O5 2.109(7) . ?
V8 O11 2.156(8) . ?
V8 O15 1.602(11) . ?
Cu7 O8 2.423(9) . ?
Cu7 N3 1.992(11) 31 ?
Cu7 N3 1.992(11) . ?
Cu7 N1 1.986(12) 31 ?
Cu7 N1 1.986(12) . ?
O6 K16 3.017(11) . ?
O9 K16 2.870(12) . ?
N4 C16 1.471(19) . ?
N4 K17 3.375(10) . ?
N5 H5A 0.8900 . ?
N5 H5B 0.8900 . ?
N5 C11 1.431(19) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C16 1.39(2) . ?
C16 H16 0.9800 . ?
C16 C18 1.42(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
N3 H3A 0.8900 . ?
N3 H3B 0.8900 . ?
N3 C6 1.517(15) . ?
C6 H6 0.9800 . ?
C6 C7 1.49(2) . ?
C6 C2 1.35(3) . ?
C7 H7 0.9800 . ?
C7 N1 1.46(2) . ?
C7 C4 1.48(4) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
K16 O17 2.92(2) 31 ?
K16 O17 2.92(2) . ?
K16 O18 2.73(4) . ?
K16 O18 2.73(4) 18_556 ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
O19 O19 0.94(5) 15_455 ?
O19 O19 1.80(5) 31 ?

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
V8 Nb1 K16 167.76(11) . . ?
O2 Nb1 V8 74.81(15) . . ?
O2 Nb1 K16 94.98(17) . . ?
O4 Nb1 V8 39.14(16) 31 . ?
O4 Nb1 O2 83.8(2) 31 . ?
O4 Nb1 O5 82.9(2) 31 . ?
O4 Nb1 K16 134.49(16) 31 . ?
O5 Nb1 V8 43.74(19) . . ?
O5 Nb1 O2 72.0(2) . . ?
O5 Nb1 K16 139.94(18) . . ?
O6 Nb1 V8 129.3(2) . . ?
O6 Nb1 O2 74.8(2) . . ?
O6 Nb1 O4 158.5(3) . 31 ?
O6 Nb1 O5 88.3(3) . . ?
O6 Nb1 K16 51.7(2) . . ?
O9 Nb1 V8 123.7(2) . . ?
O9 Nb1 O2 84.4(3) . . ?
O9 Nb1 O4 87.7(3) . 31 ?
O9 Nb1 O5 155.3(3) . . ?
O9 Nb1 O6 92.4(3) . . ?
O9 Nb1 K16 47.1(2) . . ?
O10 Nb1 V8 103.4(2) . . ?
O10 Nb1 O2 172.8(3) . . ?
O10 Nb1 O4 99.3(3) . 31 ?
O10 Nb1 O5 101.8(3) . . ?
O10 Nb1 O6 101.7(3) . . ?
O10 Nb1 O9 102.2(3) . . ?
O10 Nb1 K16 87.5(2) . . ?
O2 P2 O2 109.6(5) 31 . ?
O14 P2 O2 109.36(19) 18_556 . ?
O14 P2 O2 109.36(19) . . ?
O14 P2 O2 109.36(19) . 31 ?
O14 P2 O2 109.36(19) 18_556 31 ?
O14 P2 O14 109.8(6) . 18_556 ?
V8 Nb3 V8 148.63(10) 18_556 . ?
O2 Nb3 V8 75.97(6) . . ?
O2 Nb3 V8 75.97(6) . 18_556 ?
O3 Nb3 V8 40.19(17) . . ?
O3 Nb3 V8 40.20(17) 18_556 18_556 ?
O3 Nb3 V8 123.54(17) 18_556 . ?
O3 Nb3 V8 123.54(17) . 18_556 ?
O3 Nb3 O2 85.5(2) . . ?
O3 Nb3 O2 85.5(2) 18_556 . ?
O3 Nb3 O3 86.3(3) . 18_556 ?
O5 Nb3 V8 45.26(19) . . ?
O5 Nb3 V8 45.26(19) 18_556 18_556 ?
O5 Nb3 V8 134.71(18) . 18_556 ?
O5 Nb3 V8 134.71(18) 18_556 . ?
O5 Nb3 O2 72.4(2) 18_556 . ?
O5 Nb3 O2 72.4(2) . . ?
O5 Nb3 O3 85.5(3) . . ?
O5 Nb3 O3 85.5(3) 18_556 18_556 ?
O5 Nb3 O3 156.9(2) 18_556 . ?
O5 Nb3 O3 156.9(2) . 18_556 ?
O5 Nb3 O5 93.9(4) . 18_556 ?
O1 Nb3 V8 104.99(6) . 18_556 ?
O1 Nb3 V8 104.99(6) . . ?
O1 Nb3 O2 170.6(3) . . ?
O1 Nb3 O3 101.3(3) . . ?
O1 Nb3 O3 101.3(3) . 18_556 ?
O1 Nb3 O5 101.5(3) . . ?
O1 Nb3 O5 101.5(3) . 18_556 ?
O3 Nb4 V8 38.34(17) . . ?
O3 Nb4 O14 84.85(19) . . ?
O7 Nb4 V8 122.0(2) . . ?
O7 Nb4 O3 87.3(3) . . ?
O7 Nb4 O11 154.1(3) . . ?
O7 Nb4 O12 91.3(4) . . ?
O7 Nb4 O14 84.0(3) . . ?
O11 Nb4 V8 44.6(2) . . ?
O11 Nb4 O3 83.0(3) . . ?
O11 Nb4 O14 71.2(2) . . ?
O12 Nb4 V8 130.9(3) . . ?
O12 Nb4 O3 159.0(3) . . ?
O12 Nb4 O11 89.3(3) . . ?
O12 Nb4 O14 74.2(2) . . ?
O13 Nb4 V8 105.3(3) . . ?
O13 Nb4 O3 100.2(3) . . ?
O13 Nb4 O7 102.3(4) . . ?
O13 Nb4 O11 103.1(3) . . ?
O13 Nb4 O12 100.5(3) . . ?
O13 Nb4 O14 172.0(3) . . ?
O14 Nb4 V8 74.86(15) . . ?
V8 Nb5 V8 149.72(11) . 31 ?
O4 Nb5 V8 124.10(17) 31 31 ?
O4 Nb5 V8 39.63(17) . 31 ?
O4 Nb5 V8 124.09(17) . . ?
O4 Nb5 V8 39.63(17) 31 . ?
O4 Nb5 O4 87.1(3) 31 . ?
O4 Nb5 O11 85.3(3) . 31 ?
O4 Nb5 O11 85.3(3) 31 . ?
O4 Nb5 O11 157.6(3) 31 31 ?
O4 Nb5 O11 157.6(3) . . ?
O4 Nb5 O14 85.6(2) 31 . ?
O4 Nb5 O14 85.6(2) . . ?
O11 Nb5 V8 45.7(2) 31 31 ?
O11 Nb5 V8 135.3(2) . 31 ?
O11 Nb5 V8 135.3(2) 31 . ?
O11 Nb5 V8 45.7(2) . . ?
O11 Nb5 O11 93.8(4) . 31 ?
O11 Nb5 O14 72.9(2) 31 . ?
O11 Nb5 O14 72.9(2) . . ?
O14 Nb5 V8 76.60(6) . . ?
O14 Nb5 V8 76.60(6) . 31 ?
O8 Nb5 V8 104.47(6) . . ?
O8 Nb5 V8 104.47(6) . 31 ?
O8 Nb5 O4 102.0(3) . . ?
O8 Nb5 O4 102.0(3) . 31 ?
O8 Nb5 O11 100.1(3) . . ?
O8 Nb5 O11 100.1(3) . 31 ?
O8 Nb5 O14 169.4(4) . . ?
N4 Cu6 N4 92.8(5) 18_556 . ?
N4 Cu6 N5 174.2(4) 18_556 . ?
N4 Cu6 N5 84.2(4) 18_556 18_556 ?
N4 Cu6 N5 84.3(4) . . ?
N4 Cu6 N5 174.2(4) . 18_556 ?
N5 Cu6 N5 98.3(7) 18_556 . ?
Nb1 V8 Nb4 120.35(8) . . ?
Nb3 V8 Nb1 72.65(6) . . ?
Nb3 V8 Nb4 79.99(7) . . ?
Nb3 V8 Nb5 120.57(9) . . ?
Nb5 V8 Nb1 78.70(7) . . ?
Nb5 V8 Nb4 71.47(6) . . ?
O3 V8 Nb1 106.94(19) . . ?
O3 V8 Nb3 41.84(17) . . ?
O3 V8 Nb4 40.85(17) . . ?
O3 V8 Nb5 105.49(19) . . ?
O3 V8 O4 121.7(3) . 31 ?
O3 V8 O5 83.7(3) . . ?
O3 V8 O11 81.8(3) . . ?
O4 V8 Nb1 40.81(18) 31 . ?
O4 V8 Nb3 106.02(19) 31 . ?
O4 V8 Nb4 104.67(19) 31 . ?
O4 V8 Nb5 40.22(18) 31 . ?
O4 V8 O5 82.8(2) 31 . ?
O4 V8 O11 81.5(3) 31 . ?
O5 V8 Nb1 41.97(16) . . ?
O5 V8 Nb3 41.90(17) . . ?
O5 V8 Nb4 119.61(19) . . ?
O5 V8 Nb5 118.62(19) . . ?
O5 V8 O11 148.7(3) . . ?
O11 V8 Nb1 117.92(19) . . ?
O11 V8 Nb3 118.8(2) . . ?
O11 V8 Nb4 40.94(18) . . ?
O11 V8 Nb5 41.30(17) . . ?
O15 V8 Nb1 118.0(4) . . ?
O15 V8 Nb3 118.9(4) . . ?
O15 V8 Nb4 121.6(4) . . ?
O15 V8 Nb5 120.5(4) . . ?
O15 V8 O3 119.6(5) . . ?
O15 V8 O4 118.7(5) . 31 ?
O15 V8 O5 103.6(4) . . ?
O15 V8 O11 107.6(4) . . ?
N3 Cu7 O8 89.0(3) 31 . ?
N3 Cu7 O8 89.0(3) . . ?
N3 Cu7 N3 96.1(5) . 31 ?
N1 Cu7 O8 93.8(3) 31 . ?
N1 Cu7 O8 93.8(3) . . ?
N1 Cu7 N3 176.9(5) . 31 ?
N1 Cu7 N3 176.9(5) 31 . ?
N1 Cu7 N3 85.3(5) 31 31 ?
N1 Cu7 N3 85.3(5) . . ?
N1 Cu7 N1 93.2(8) 31 . ?
Nb1 O2 Nb1 87.2(2) . 18_556 ?
Nb1 O2 Nb3 90.1(2) 18_556 . ?
Nb1 O2 Nb3 90.1(2) . . ?
P2 O2 Nb1 125.6(2) . . ?
P2 O2 Nb1 125.6(2) . 18_556 ?
P2 O2 Nb3 126.3(4) . . ?
Nb3 O3 Nb4 147.4(3) . . ?
V8 O3 Nb3 98.0(3) . . ?
V8 O3 Nb4 100.8(3) . . ?
Nb5 O4 Nb1 147.8(3) . 31 ?
V8 O4 Nb1 100.0(3) 31 31 ?
V8 O4 Nb5 100.1(3) 31 . ?
Nb1 O5 V8 94.3(3) . . ?
Nb3 O5 Nb1 124.4(3) . . ?
Nb3 O5 V8 92.8(3) . . ?
Nb1 O6 Nb1 122.9(4) . 18_556 ?
Nb1 O6 K16 97.6(3) 18_556 . ?
Nb1 O6 K16 97.6(3) . . ?
Nb4 O7 Nb4 152.6(5) 18_556 . ?
Nb1 O9 Nb1 151.7(5) . 31 ?
Nb1 O9 K16 103.2(2) 31 . ?
Nb1 O9 K16 103.2(2) . . ?
Nb4 O11 V8 94.4(3) . . ?
Nb5 O11 Nb4 124.8(3) . . ?
Nb5 O11 V8 93.0(3) . . ?
Nb4 O12 Nb4 124.5(4) . 31 ?
P2 O14 Nb4 125.9(3) . . ?
P2 O14 Nb4 125.9(3) . 31 ?
P2 O14 Nb5 126.1(4) . . ?
Nb4 O14 Nb4 87.0(2) 31 . ?
Nb5 O14 Nb4 90.0(2) . . ?
Nb5 O14 Nb4 90.0(2) . 31 ?
Cu6 N4 K17 100.0(4) . . ?
C16 N4 Cu6 106.8(9) . . ?
C16 N4 K17 121.4(11) . . ?
Cu6 N5 H5A 109.7 . . ?
Cu6 N5 H5B 109.7 . . ?
H5A N5 H5B 108.2 . . ?
C11 N5 Cu6 109.8(8) . . ?
C11 N5 H5A 109.7 . . ?
C11 N5 H5B 109.7 . . ?
N5 C11 H11A 108.3 . . ?
N5 C11 H11B 108.3 . . ?
H11A C11 H11B 107.4 . . ?
C16 C11 N5 115.9(14) . . ?
C16 C11 H11A 108.3 . . ?
C16 C11 H11B 108.3 . . ?
N4 C16 H16 101.4 . . ?
C11 C16 N4 114.4(15) . . ?
C11 C16 H16 101.4 . . ?
C11 C16 C18 114.5(17) . . ?
C18 C16 N4 119.8(18) . . ?
C18 C16 H16 101.4 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Nb5 O8 Cu7 126.1(5) . . ?
Cu7 N3 H3A 110.3 . . ?
Cu7 N3 H3B 110.3 . . ?
H3A N3 H3B 108.6 . . ?
C6 N3 Cu7 107.1(8) . . ?
C6 N3 H3A 110.3 . . ?
C6 N3 H3B 110.3 . . ?
N3 C6 H6 108.1 . . ?
C7 C6 N3 106.6(12) . . ?
C7 C6 H6 108.1 . . ?
C2 C6 N3 117.7(15) . . ?
C2 C6 H6 108.1 . . ?
C2 C6 C7 107.8(16) . . ?
C6 C7 H7 104.1 . . ?
N1 C7 C6 110.3(11) . . ?
N1 C7 H7 104.1 . . ?
N1 C7 C4 129(2) . . ?
C4 C7 C6 103(2) . . ?
C4 C7 H7 104.1 . . ?
Cu7 N1 H1A 109.6 . . ?
Cu7 N1 H1B 109.6 . . ?
C7 N1 Cu7 110.3(9) . . ?
C7 N1 H1A 109.6 . . ?
C7 N1 H1B 109.6 . . ?
H1A N1 H1B 108.1 . . ?
Nb1 K16 Nb1 59.02(13) . 31 ?
Nb1 K16 Nb1 59.02(13) 16 18_556 ?
Nb1 K16 Nb1 53.83(11) 16 31 ?
Nb1 K16 Nb1 84.0(2) 31 18_556 ?
Nb1 K16 Nb1 53.83(11) . 18_556 ?
Nb1 K16 Nb1 84.0(2) . 16 ?
O6 K16 Nb1 83.3(2) . 31 ?
O6 K16 Nb1 30.71(10) . 18_556 ?
O6 K16 Nb1 30.71(10) 31 16 ?
O6 K16 Nb1 30.71(10) 31 31 ?
O6 K16 Nb1 83.3(2) 31 18_556 ?
O6 K16 Nb1 83.3(2) . 16 ?
O6 K16 Nb1 30.71(10) . . ?
O6 K16 Nb1 83.3(2) 31 . ?
O6 K16 O6 97.8(4) . 31 ?
O9 K16 Nb1 29.64(7) . 31 ?
O9 K16 Nb1 68.9(2) 18_556 . ?
O9 K16 Nb1 68.9(2) . 18_556 ?
O9 K16 Nb1 29.64(7) 18_556 16 ?
O9 K16 Nb1 68.9(2) . 16 ?
O9 K16 Nb1 29.64(7) . . ?
O9 K16 Nb1 68.9(2) 18_556 31 ?
O9 K16 Nb1 29.64(7) 18_556 18_556 ?
O9 K16 O6 57.1(2) 18_556 . ?
O9 K16 O6 57.1(2) . 31 ?
O9 K16 O6 57.1(2) 18_556 31 ?
O9 K16 O6 57.1(2) . . ?
O9 K16 O9 68.4(4) 18_556 . ?
O9 K16 O17 112.0(6) 18_556 31 ?
O9 K16 O17 112.0(6) . 31 ?
O9 K16 O17 112.0(6) 18_556 . ?
O9 K16 O17 112.0(6) . . ?
O17 K16 Nb1 140.9(5) 31 31 ?
O17 K16 Nb1 84.1(6) 31 18_556 ?
O17 K16 Nb1 140.9(5) . . ?
O17 K16 Nb1 84.1(6) . 16 ?
O17 K16 Nb1 84.1(6) . 31 ?
O17 K16 Nb1 140.9(5) . 18_556 ?
O17 K16 Nb1 84.1(6) 31 . ?
O17 K16 Nb1 140.9(5) 31 16 ?
O17 K16 O6 165.8(8) . . ?
O17 K16 O6 165.8(8) 31 31 ?
O17 K16 O6 68.0(7) 31 . ?
O17 K16 O6 68.0(7) . 31 ?
O17 K16 O17 126.2(15) . 31 ?
O18 K16 Nb1 141.6(5) 18_556 . ?
O18 K16 Nb1 91.3(7) . . ?
O18 K16 Nb1 141.6(5) . 18_556 ?
O18 K16 Nb1 141.6(5) . 16 ?
O18 K16 Nb1 141.6(5) 18_556 31 ?
O18 K16 Nb1 91.3(7) 18_556 16 ?
O18 K16 Nb1 91.3(7) . 31 ?
O18 K16 Nb1 91.3(7) 18_556 18_556 ?
O18 K16 O6 110.9(5) . 31 ?
O18 K16 O6 110.9(5) . . ?
O18 K16 O6 110.9(5) 18_556 31 ?
O18 K16 O6 110.9(5) 18_556 . ?
O18 K16 O9 88.7(9) . . ?
O18 K16 O9 88.7(9) 18_556 18_556 ?
O18 K16 O9 157.1(9) . 18_556 ?
O18 K16 O9 157.1(9) 18_556 . ?
O18 K16 O17 75.8(5) 18_556 . ?
O18 K16 O17 75.8(5) 18_556 31 ?
O18 K16 O17 75.8(5) . 31 ?
O18 K16 O17 75.8(5) . . ?
O18 K16 O18 114.3(17) . 18_556 ?
N4 K17 N4 79.42(13) . 3 ?
N4 K17 N4 50.7(3) 19_556 4 ?
N4 K17 N4 100.58(13) 4 18_556 ?
N4 K17 N4 129.3(3) 17_556 18_556 ?
N4 K17 N4 100.58(13) . 20_556 ?
N4 K17 N4 79.42(13) 19_556 18_556 ?
N4 K17 N4 100.58(13) 19_556 2 ?
N4 K17 N4 79.42(13) 17_556 20_556 ?
N4 K17 N4 129.3(3) 3 4 ?
N4 K17 N4 100.58(13) 20_556 2 ?
N4 K17 N4 180.00(17) 20_556 4 ?
N4 K17 N4 100.58(13) 17_556 4 ?
N4 K17 N4 180.0(3) 19_556 3 ?
N4 K17 N4 129.3(3) . 2 ?
N4 K17 N4 50.7(3) 17_556 2 ?
N4 K17 N4 79.42(13) 3 2 ?
N4 K17 N4 79.42(13) 19_556 17_556 ?
N4 K17 N4 79.42(13) 4 2 ?
N4 K17 N4 180.0 . 17_556 ?
N4 K17 N4 50.7(3) . 18_556 ?
N4 K17 N4 100.58(13) 3 17_556 ?
N4 K17 N4 100.58(13) 3 18_556 ?
N4 K17 N4 129.3(3) 19_556 20_556 ?
N4 K17 N4 79.42(13) 20_556 18_556 ?
N4 K17 N4 50.7(3) 3 20_556 ?
N4 K17 N4 180.0 2 18_556 ?
N4 K17 N4 79.42(13) . 4 ?
N4 K17 N4 100.58(13) . 19_556 ?
C6 C2 H2A 109.5 . . ?
C6 C2 H2B 109.5 . . ?
C6 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C7 C4 H4A 109.5 . . ?
C7 C4 H4B 109.5 . . ?
C7 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O19 O19 O19 89.997(4) 15_455 31 ?

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
Cu6 N4 C16 C11 -33(3) . . . . ?
Cu6 N4 C16 C18 -174(2) . . . . ?
Cu6 N5 C11 C16 -7(2) . . . . ?
V8 Nb5 O8 Cu7 94.49(10) 31 . . . ?
V8 Nb5 O8 Cu7 -94.49(10) . . . . ?
Cu7 N3 C6 C7 -43.5(12) . . . . ?
Cu7 N3 C6 C2 -164.6(16) . . . . ?
O2 P2 O2 Nb1 -58.0(3) 31 . . 18_556 ?
O2 P2 O2 Nb1 58.0(3) 31 . . . ?
O2 P2 O2 Nb3 180.0 31 . . . ?
O2 P2 O14 Nb4 61.8(5) 31 . . 31 ?
O2 P2 O14 Nb4 178.2(4) 31 . . . ?
O2 P2 O14 Nb4 -178.2(4) . . . 31 ?
O2 P2 O14 Nb4 -61.8(5) . . . . ?
O2 P2 O14 Nb5 60.0(3) . . . . ?
O2 P2 O14 Nb5 -60.0(3) 31 . . . ?
O4 Nb5 O8 Cu7 -135.19(18) 31 . . . ?
O4 Nb5 O8 Cu7 135.19(18) . . . . ?
O11 Nb5 O8 Cu7 47.9(2) 31 . . . ?
O11 Nb5 O8 Cu7 -47.9(2) . . . . ?
O14 P2 O2 Nb1 177.9(4) 18_556 . . . ?
O14 P2 O2 Nb1 61.8(5) 18_556 . . 18_556 ?
O14 P2 O2 Nb1 -177.9(4) . . . 18_556 ?
O14 P2 O2 Nb1 -61.8(5) . . . . ?
O14 P2 O2 Nb3 60.1(3) . . . . ?
O14 P2 O2 Nb3 -60.1(3) 18_556 . . . ?
O14 P2 O14 Nb4 58.2(4) 18_556 . . . ?
O14 P2 O14 Nb4 -58.2(4) 18_556 . . 31 ?
O14 P2 O14 Nb5 180.000(1) 18_556 . . . ?
O14 Nb5 O8 Cu7 0.000(7) . . . . ?
N5 C11 C16 N4 27(3) . . . . ?
N5 C11 C16 C18 170.5(19) . . . . ?
N3 C6 C7 N1 48.5(14) . . . . ?
N3 C6 C7 C4 -171.0(15) . . . . ?
C6 C7 N1 Cu7 -30.1(13) . . . . ?
K17 N4 C16 C11 -146.3(17) . . . . ?
K17 N4 C16 C18 72(3) . . . . ?
C2 C6 C7 N1 175.7(15) . . . . ?
C2 C6 C7 C4 -44(2) . . . . ?
C4 C7 N1 Cu7 -157(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_k_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2378669'
loop_
_audit_author_name
_audit_author_address
'xiaobing cui'
;jilin university
China
;
_audit_update_record             
;
2024-08-21 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT601_k                   
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        469 Ang**3 
RESPONSE: The crystal data of this compound are poor, so there is one 
water molecule which can not be located by the crsytal analysis. However,
the absence of one lattice molecule has little influence to the chemical 
formula of this compound, so we did not change the chemical formula of
this compound.
;

_vrf_PLAT973_k                   
;
PROBLEM: Check Calcd Positive Resid. Density on       Nb2       5.78 eA-3  
RESPONSE: The crystal data of this compound are poor. these Alerts are 
caused by the poor data.
;
# end Validation Reply Form


_audit_creation_date             2024-08-21
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'2(K0.5 Nb12 O45 V3), C24 H64 Cu4 K N16, 4(C6 H15 Cu N4), 19(O)'
_chemical_formula_sum            'C48 H214 Cu8 K2 N32 Nb24 O109 V6'
_chemical_formula_weight         6106.50
_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'
K K 0.2009 0.2494 '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'
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           140
_space_group_name_H-M_alt        'I 4/m c m'
_space_group_name_Hall           '-I 4 2c'
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                   26.3856(7)
_cell_length_b                   26.3856(7)
_cell_length_c                   27.5212(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19160.3(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9014
_cell_measurement_temperature    299.00
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.44
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.654
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6106
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0699 before and 0.0571 after correction.
The Ratio of minimum to maximum transmission is 0.8194.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Brownish-Purple
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       Needle-like
_exptl_crystal_F_000             11960
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            60533
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.362
_diffrn_reflns_theta_min         2.441
_diffrn_ambient_temperature      299.00
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3181
_reflns_number_total             4630
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         4.317
_refine_diff_density_min         -1.302
_refine_diff_density_rms         0.227
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.637
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4630
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1367
_refine_ls_R_factor_gt           0.1007
_refine_ls_restrained_S_all      1.637
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2867
_refine_ls_wR_factor_ref         0.3811
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7-C3
 2.33 with sigma of 0.04
3. Restrained planarity
 C8, C7, C1, C3
 with sigma of 0.1
4. Rigid bond restraints
 C12, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\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
6. Others
 Fixed Sof: V3(0.5) O23(0.5) K2(0.125) O14(0.25) C1(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) H3C(0.5) O21(0.5) O19(0.125)
7.a Ternary CH refined with riding coordinates:
 C30(H30), C7(H7), C8(H8)
7.b Secondary CH2 refined with riding coordinates:
 N22(H22A,H22B), C25(H25A,H25B), N4(H4A,H4B), N1(H1A,H1B)
7.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C3(H3A,H3B,H3C)
;
_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
V1 V 0.28042(8) 0.21958(8) 0.000000 0.0492(17) Uani 1 4 d S T P . .
Nb2 Nb 0.15843(4) 0.24042(4) 0.06248(4) 0.0615(15) Uani 1 1 d . . . . .
Nb3 Nb 0.17810(5) 0.12391(5) 0.000000 0.0721(16) Uani 1 2 d S T P . .
Nb4 Nb 0.30559(4) 0.10178(4) 0.06822(5) 0.0721(16) Uani 1 1 d . . . . .
Nb5 Nb 0.28355(4) 0.21645(4) 0.13244(6) 0.0746(16) Uani 1 2 d S T P . .
Cu6 Cu 0.15835(8) -0.02130(8) 0.000000 0.0857(17) Uani 1 2 d S T P . .
Cu7 Cu 0.32295(8) 0.17705(8) 0.25756(12) 0.1057(18) Uani 1 2 d S T P . .
V3 V 0.20339(13) 0.14264(13) 0.10272(16) 0.0656(18) Uani 0.5 1 d . . P . .
O5 O 0.2306(3) 0.1057(3) 0.0497(3) 0.066(2) Uani 1 1 d . . . . .
O6 O 0.1243(3) 0.2534(4) 0.000000 0.064(3) Uani 1 2 d S T P . .
O7 O 0.2849(3) 0.2875(3) 0.1094(3) 0.063(2) Uani 1 1 d . . . . .
O8 O 0.3086(3) 0.0398(3) 0.0908(5) 0.099(4) Uani 1 1 d . . . . .
O9 O 0.1108(3) 0.2573(3) 0.1044(3) 0.079(3) Uani 1 1 d . . . . .
O10 O 0.1463(3) 0.1647(3) 0.0533(3) 0.072(3) Uani 1 1 d . . . . .
O11 O 0.1975(3) 0.3025(3) 0.0585(4) 0.064(3) Uani 1 2 d S T P . .
O12 O 0.3751(3) 0.1249(3) 0.0814(5) 0.079(4) Uani 1 2 d S T P . .
O13 O 0.2912(3) 0.2840(3) 0.000000 0.062(3) Uani 1 2 d S T P . .
O15 O 0.1396(4) 0.0694(4) 0.000000 0.072(3) Uani 1 2 d S T P . .
O16 O 0.3061(3) 0.1939(3) 0.0495(4) 0.065(3) Uani 1 2 d S T P . .
O17 O 0.3205(4) 0.0945(4) 0.000000 0.088(4) Uani 1 2 d S T P . .
O18 O 0.2766(4) 0.2234(4) 0.1945(5) 0.086(4) Uani 1 2 d S T P . .
N19 N 0.1084(4) -0.0397(4) -0.0518(5) 0.088(3) Uani 1 1 d . . . . .
O20 O 0.2808(4) 0.1410(3) 0.1271(4) 0.088(3) Uani 1 1 d . . . . .
N22 N 0.2065(5) -0.0104(4) -0.0570(6) 0.108(5) Uani 1 1 d . . . . .
H22A H 0.220646 0.020075 -0.054532 0.129 Uiso 1 1 calc R U . . .
H22B H 0.231039 -0.033479 -0.055870 0.129 Uiso 1 1 calc R U . . .
O23 O 0.1723(5) 0.1152(5) 0.1428(6) 0.061(4) Uani 0.5 1 d . . P . .
C25 C 0.1799(8) -0.0143(8) -0.1034(9) 0.136(8) Uani 1 1 d . . . . .
H25A H 0.188453 0.015055 -0.123017 0.163 Uiso 1 1 calc R U . . .
H25B H 0.192201 -0.044077 -0.120438 0.163 Uiso 1 1 calc R U . . .
C30 C 0.1268(9) -0.0175(15) -0.0998(11) 0.222(18) Uani 1 1 d . U . . .
H30 H 0.118746 0.018305 -0.094297 0.267 Uiso 1 1 calc R U . . .
C12 C 0.1017(8) -0.0249(9) -0.1416(10) 0.157(9) Uani 1 1 d . U . . .
H12A H 0.066069 -0.027734 -0.134992 0.235 Uiso 1 1 calc R U . . .
H12B H 0.113468 -0.055584 -0.156594 0.235 Uiso 1 1 calc R U . . .
H12C H 0.107585 0.003162 -0.162974 0.235 Uiso 1 1 calc R U . . .
N4 N 0.2574(6) 0.1625(5) 0.2933(5) 0.106(4) Uani 1 1 d . . . . .
H4A H 0.263540 0.150503 0.322937 0.128 Uiso 1 1 calc R U . . .
H4B H 0.238525 0.190288 0.295692 0.128 Uiso 1 1 calc R U . . .
C7 C 0.2315(9) 0.1226(8) 0.2617(7) 0.135(7) Uani 1 1 d D . . . .
H7 H 0.223463 0.142486 0.232623 0.163 Uiso 1 1 calc R U . . .
C8 C 0.2674(10) 0.0865(7) 0.2424(9) 0.144(8) Uani 1 1 d . . . . .
H8 H 0.281420 0.075233 0.273592 0.173 Uiso 1 1 calc R U . . .
K2 K 0.1326(2) 0.3674(2) 0.000000 0.072(3) Uani 0.5 4 d S T P . .
K1 K 0.000000 0.000000 0.000000 0.103(3) Uani 1 8 d S T P . .
O1 O 0.4284(5) 0.0716(5) 0.000000 0.103(6) Uani 1 4 d S T P . .
O2 O 0.3281(8) -0.0457(7) 0.1368(9) 0.239(12) Uani 1 1 d . . . . .
O3 O 0.0296(14) 0.3373(14) 0.000000 0.235(16) Uani 1 2 d S T P . .
O4 O 0.4182(12) 0.0818(12) 0.1604(18) 0.307(4) Uani 1 2 d S TU P . .
O14 O 0.100(2) 0.400(2) 0.0809(13) 0.20(3) Uani 0.5 2 d S T P . .
N1 N 0.3120(8) 0.1095(6) 0.2242(7) 0.134(6) Uani 1 1 d . . . . .
H1A H 0.309159 0.114193 0.192304 0.161 Uiso 1 1 calc R U . . .
H1B H 0.338507 0.089416 0.229582 0.161 Uiso 1 1 calc R U . . .
C1 C 0.1846(18) 0.0957(15) 0.2690(19) 0.17(2) Uani 0.5 1 d . . P . .
C3 C 0.242(2) 0.0431(13) 0.2313(16) 0.170(18) Uani 0.5 1 d D U P . .
H3A H 0.219068 0.034824 0.257152 0.254 Uiso 0.5 1 calc R U P . .
H3B H 0.265821 0.015924 0.227034 0.254 Uiso 0.5 1 calc R U P . .
H3C H 0.223257 0.047887 0.201729 0.254 Uiso 0.5 1 calc R U P . .
O21 O 0.3891(15) 0.0355(16) 0.2814(17) 0.197(15) Uani 0.5 1 d . . P . .
O19 O 0.109(6) 0.391(6) 0.184(7) 0.333(4) Uani 0.25 2 d S TU P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O13 1.723(9) 31 ?
V1 O13 1.723(9) . ?
V1 O16 1.667(11) 18 ?
V1 O16 1.667(11) . ?
Nb2 V3 3.048(4) . ?
Nb2 O6 1.971(5) . ?
Nb2 O7 2.036(7) 31 ?
Nb2 O9 1.763(8) . ?
Nb2 O10 2.038(7) . ?
Nb2 O11 1.939(3) . ?
Nb2 O13 2.441(6) 31 ?
Nb2 K2 3.826(6) . ?
Nb3 V3 2.947(4) . ?
Nb3 V3 2.947(4) 18 ?
Nb3 O5 2.005(7) . ?
Nb3 O5 2.005(7) 18 ?
Nb3 O10 2.003(8) 18 ?
Nb3 O10 2.003(8) . ?
Nb3 O13 2.454(9) 31 ?
Nb3 O15 1.760(10) . ?
Nb4 V3 3.056(4) . ?
Nb4 O5 2.047(7) . ?
Nb4 O8 1.752(8) . ?
Nb4 O12 1.967(5) . ?
Nb4 O16 2.484(7) . ?
Nb4 O17 1.928(3) . ?
Nb4 O20 2.030(10) . ?
Nb5 V3 2.989(4) 31 ?
Nb5 V3 2.989(4) . ?
Nb5 O7 1.980(7) . ?
Nb5 O7 1.980(7) 31 ?
Nb5 O16 2.432(12) . ?
Nb5 O18 1.727(14) . ?
Nb5 O20 1.996(8) . ?
Nb5 O20 1.996(8) 31 ?
Cu6 N19 2.001(13) . ?
Cu6 N19 2.001(13) 18 ?
Cu6 N22 2.038(14) 18 ?
Cu6 N22 2.038(14) . ?
Cu7 N4 2.025(17) 31 ?
Cu7 N4 2.025(17) . ?
Cu7 N1 2.024(19) 31 ?
Cu7 N1 2.024(19) . ?
V3 O5 1.896(9) . ?
V3 O7 1.936(7) 31 ?
V3 O10 2.112(9) . ?
V3 O20 2.151(10) . ?
V3 O23 1.552(17) . ?
O6 K2 3.014(11) . ?
O11 K2 2.906(13) . ?
N19 C30 1.52(3) . ?
N19 K1 3.364(12) . ?
N22 H22A 0.8900 . ?
N22 H22B 0.8900 . ?
N22 C25 1.46(3) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C30 1.41(3) . ?
C30 H30 0.9800 . ?
C30 C12 1.34(3) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N4 C7 1.53(2) . ?
C7 H7 0.9800 . ?
C7 C8 1.45(3) . ?
C7 C1 1.44(5) . ?
C8 H8 0.9800 . ?
C8 N1 1.42(3) . ?
C8 C3 1.36(4) . ?
K2 O3 2.83(3) . ?
K2 O3 2.83(3) 31 ?
K2 O14 2.53(5) 18 ?
K2 O14 2.53(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

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
O13 V1 O13 109.0(6) 31 . ?
O16 V1 O13 109.5(2) . . ?
O16 V1 O13 109.5(2) 18 31 ?
O16 V1 O13 109.5(2) 18 . ?
O16 V1 O13 109.5(2) . 31 ?
O16 V1 O16 109.8(7) 18 . ?
V3 Nb2 K2 166.79(11) . . ?
O6 Nb2 V3 130.0(3) . . ?
O6 Nb2 O7 158.5(3) . 31 ?
O6 Nb2 O10 89.5(4) . . ?
O6 Nb2 O13 74.3(3) . 31 ?
O6 Nb2 K2 51.3(3) . . ?
O7 Nb2 V3 38.7(2) 31 . ?
O7 Nb2 O10 82.4(3) 31 . ?
O7 Nb2 O13 84.2(3) 31 31 ?
O7 Nb2 K2 134.16(19) 31 . ?
O9 Nb2 V3 104.7(3) . . ?
O9 Nb2 O6 101.6(4) . . ?
O9 Nb2 O7 99.6(4) . 31 ?
O9 Nb2 O10 102.6(3) . . ?
O9 Nb2 O11 101.7(4) . . ?
O9 Nb2 O13 172.2(3) . 31 ?
O9 Nb2 K2 86.9(3) . . ?
O10 Nb2 V3 43.7(3) . . ?
O10 Nb2 O13 71.0(3) . 31 ?
O10 Nb2 K2 140.7(3) . . ?
O11 Nb2 V3 122.0(3) . . ?
O11 Nb2 O6 92.6(4) . . ?
O11 Nb2 O7 86.6(4) . 31 ?
O11 Nb2 O10 154.7(4) . . ?
O11 Nb2 O13 85.3(4) . 31 ?
O11 Nb2 K2 47.9(3) . . ?
O13 Nb2 V3 74.01(19) 31 . ?
O13 Nb2 K2 95.3(2) 31 . ?
V3 Nb3 V3 147.26(15) . 18 ?
O5 Nb3 V3 39.6(2) 18 18 ?
O5 Nb3 V3 122.6(2) . 18 ?
O5 Nb3 V3 39.6(2) . . ?
O5 Nb3 V3 122.6(2) 18 . ?
O5 Nb3 O5 86.0(5) . 18 ?
O5 Nb3 O13 86.4(3) . 31 ?
O5 Nb3 O13 86.4(3) 18 31 ?
O10 Nb3 V3 45.8(3) 18 18 ?
O10 Nb3 V3 135.0(2) . 18 ?
O10 Nb3 V3 45.8(3) . . ?
O10 Nb3 V3 135.0(2) 18 . ?
O10 Nb3 O5 85.3(3) 18 18 ?
O10 Nb3 O5 156.5(3) . 18 ?
O10 Nb3 O5 85.3(3) . . ?
O10 Nb3 O5 156.5(3) 18 . ?
O10 Nb3 O10 94.1(5) . 18 ?
O10 Nb3 O13 71.3(2) . 31 ?
O10 Nb3 O13 71.3(2) 18 31 ?
O13 Nb3 V3 75.79(8) 31 18 ?
O13 Nb3 V3 75.79(8) 31 . ?
O15 Nb3 V3 105.53(8) . 18 ?
O15 Nb3 V3 105.53(8) . . ?
O15 Nb3 O5 101.7(3) . 18 ?
O15 Nb3 O5 101.7(3) . . ?
O15 Nb3 O10 101.4(3) . 18 ?
O15 Nb3 O10 101.4(3) . . ?
O15 Nb3 O13 168.8(4) . 31 ?
O5 Nb4 V3 37.4(2) . . ?
O5 Nb4 O16 84.5(2) . . ?
O8 Nb4 V3 105.0(3) . . ?
O8 Nb4 O5 100.3(3) . . ?
O8 Nb4 O12 100.5(4) . . ?
O8 Nb4 O16 170.7(5) . . ?
O8 Nb4 O17 104.1(5) . . ?
O8 Nb4 O20 102.0(5) . . ?
O12 Nb4 V3 131.0(4) . . ?
O12 Nb4 O5 158.8(3) . . ?
O12 Nb4 O16 74.3(3) . . ?
O12 Nb4 O20 89.7(5) . . ?
O16 Nb4 V3 74.0(2) . . ?
O17 Nb4 V3 121.2(3) . . ?
O17 Nb4 O5 87.7(4) . . ?
O17 Nb4 O12 91.2(5) . . ?
O17 Nb4 O16 83.9(4) . . ?
O17 Nb4 O20 153.2(4) . . ?
O20 Nb4 V3 44.6(3) . . ?
O20 Nb4 O5 82.0(4) . . ?
O20 Nb4 O16 70.6(4) . . ?
V3 Nb5 V3 147.90(18) 31 . ?
O7 Nb5 V3 39.7(2) . 31 ?
O7 Nb5 V3 39.7(2) 31 . ?
O7 Nb5 V3 122.8(2) 31 31 ?
O7 Nb5 V3 122.8(2) . . ?
O7 Nb5 O7 86.1(4) 31 . ?
O7 Nb5 O16 85.8(3) 31 . ?
O7 Nb5 O16 85.8(3) . . ?
O7 Nb5 O20 157.1(4) . . ?
O7 Nb5 O20 85.7(3) . 31 ?
O7 Nb5 O20 157.1(4) 31 31 ?
O7 Nb5 O20 85.7(3) 31 . ?
O16 Nb5 V3 75.94(10) . . ?
O16 Nb5 V3 75.94(10) . 31 ?
O18 Nb5 V3 105.34(10) . . ?
O18 Nb5 V3 105.34(10) . 31 ?
O18 Nb5 O7 102.5(4) . . ?
O18 Nb5 O7 102.5(4) . 31 ?
O18 Nb5 O16 168.4(5) . . ?
O18 Nb5 O20 100.1(4) . . ?
O18 Nb5 O20 100.1(4) . 31 ?
O20 Nb5 V3 46.0(3) 31 31 ?
O20 Nb5 V3 135.1(3) . 31 ?
O20 Nb5 V3 46.0(3) . . ?
O20 Nb5 V3 135.1(3) 31 . ?
O20 Nb5 O16 72.2(3) 31 . ?
O20 Nb5 O16 72.3(3) . . ?
O20 Nb5 O20 93.8(5) 31 . ?
N19 Cu6 N19 90.9(7) . 18 ?
N19 Cu6 N22 173.0(5) . 18 ?
N19 Cu6 N22 173.0(5) 18 . ?
N19 Cu6 N22 84.0(6) 18 18 ?
N19 Cu6 N22 84.0(6) . . ?
N22 Cu6 N22 100.6(9) 18 . ?
N4 Cu7 N4 95.1(7) . 31 ?
N1 Cu7 N4 86.1(6) . . ?
N1 Cu7 N4 176.4(7) 31 . ?
N1 Cu7 N4 86.1(6) 31 31 ?
N1 Cu7 N4 176.4(7) . 31 ?
N1 Cu7 N1 92.6(11) 31 . ?
Nb2 V3 Nb4 121.96(13) . . ?
Nb3 V3 Nb2 72.85(10) . . ?
Nb3 V3 Nb4 80.94(11) . . ?
Nb3 V3 Nb5 122.15(14) . . ?
Nb5 V3 Nb2 79.82(9) . . ?
Nb5 V3 Nb4 71.97(9) . . ?
O5 V3 Nb2 107.6(3) . . ?
O5 V3 Nb3 42.3(2) . . ?
O5 V3 Nb4 41.0(2) . . ?
O5 V3 Nb5 106.1(3) . . ?
O5 V3 O7 122.3(4) . 31 ?
O5 V3 O10 85.1(4) . . ?
O5 V3 O20 82.5(4) . . ?
O7 V3 Nb2 41.1(2) 31 . ?
O7 V3 Nb3 106.6(3) 31 . ?
O7 V3 Nb4 105.6(2) 31 . ?
O7 V3 Nb5 40.8(2) 31 . ?
O7 V3 O10 82.9(3) 31 . ?
O7 V3 O20 82.7(3) 31 . ?
O10 V3 Nb2 41.8(2) . . ?
O10 V3 Nb3 42.8(2) . . ?
O10 V3 Nb4 121.7(3) . . ?
O10 V3 Nb5 120.1(2) . . ?
O10 V3 O20 152.1(4) . . ?
O20 V3 Nb2 120.0(2) . . ?
O20 V3 Nb3 120.7(3) . . ?
O20 V3 Nb4 41.5(3) . . ?
O20 V3 Nb5 41.9(2) . . ?
O23 V3 Nb2 116.6(5) . . ?
O23 V3 Nb3 118.9(5) . . ?
O23 V3 Nb4 121.5(5) . . ?
O23 V3 Nb5 118.9(5) . . ?
O23 V3 O5 120.4(6) . . ?
O23 V3 O7 117.3(6) . 31 ?
O23 V3 O10 102.1(5) . . ?
O23 V3 O20 105.7(5) . . ?
Nb3 O5 Nb4 148.2(4) . . ?
V3 O5 Nb3 98.1(3) . . ?
V3 O5 Nb4 101.5(4) . . ?
Nb2 O6 Nb2 121.4(5) 18 . ?
Nb2 O6 K2 98.1(3) 18 . ?
Nb2 O6 K2 98.1(3) . . ?
Nb5 O7 Nb2 149.4(4) . 31 ?
V3 O7 Nb2 100.2(3) 31 31 ?
V3 O7 Nb5 99.5(3) 31 . ?
Nb2 O10 V3 94.5(4) . . ?
Nb3 O10 Nb2 123.6(4) . . ?
Nb3 O10 V3 91.4(3) . . ?
Nb2 O11 Nb2 153.5(6) . 31 ?
Nb2 O11 K2 102.5(3) . . ?
Nb2 O11 K2 102.5(3) 31 . ?
Nb4 O12 Nb4 123.0(5) . 31 ?
V1 O13 Nb2 123.9(3) . 16_554 ?
V1 O13 Nb2 123.9(3) . 31 ?
V1 O13 Nb3 123.5(5) . 31 ?
Nb2 O13 Nb2 89.6(3) 31 16_554 ?
Nb2 O13 Nb3 93.3(2) 31 31 ?
Nb2 O13 Nb3 93.3(2) 16_554 31 ?
V1 O16 Nb4 124.4(4) . . ?
V1 O16 Nb4 124.4(4) . 31 ?
V1 O16 Nb5 124.6(5) . . ?
Nb4 O16 Nb4 88.2(3) . 31 ?
Nb5 O16 Nb4 92.5(3) . . ?
Nb5 O16 Nb4 92.5(3) . 31 ?
Nb4 O17 Nb4 153.8(6) . 18 ?
Cu6 N19 K1 100.5(5) . . ?
C30 N19 Cu6 108.4(14) . . ?
C30 N19 K1 121.1(12) . . ?
Nb4 O20 V3 93.9(4) . . ?
Nb5 O20 Nb4 123.8(5) . . ?
Nb5 O20 V3 92.2(4) . . ?
Cu6 N22 H22A 109.3 . . ?
Cu6 N22 H22B 109.3 . . ?
H22A N22 H22B 108.0 . . ?
C25 N22 Cu6 111.4(10) . . ?
C25 N22 H22A 109.3 . . ?
C25 N22 H22B 109.3 . . ?
N22 C25 H25A 108.6 . . ?
N22 C25 H25B 108.6 . . ?
H25A C25 H25B 107.5 . . ?
C30 C25 N22 114.8(19) . . ?
C30 C25 H25A 108.6 . . ?
C30 C25 H25B 108.6 . . ?
N19 C30 H30 99.7 . . ?
C25 C30 N19 113.6(19) . . ?
C25 C30 H30 99.7 . . ?
C12 C30 N19 122(3) . . ?
C12 C30 C25 116(2) . . ?
C12 C30 H30 99.7 . . ?
C30 C12 H12A 109.5 . . ?
C30 C12 H12B 109.5 . . ?
C30 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Cu7 N4 H4A 111.0 . . ?
Cu7 N4 H4B 111.0 . . ?
H4A N4 H4B 109.0 . . ?
C7 N4 Cu7 103.8(13) . . ?
C7 N4 H4A 111.0 . . ?
C7 N4 H4B 111.0 . . ?
N4 C7 H7 101.2 . . ?
C8 C7 N4 111.6(18) . . ?
C8 C7 H7 101.2 . . ?
C1 C7 N4 130(3) . . ?
C1 C7 H7 101.2 . . ?
C1 C7 C8 107(2) . . ?
C7 C8 H8 97.3 . . ?
N1 C8 C7 113.2(17) . . ?
N1 C8 H8 97.3 . . ?
C3 C8 C7 108(3) . . ?
C3 C8 H8 97.3 . . ?
C3 C8 N1 134(3) . . ?
Nb2 K2 Nb2 83.71(16) . 16_554 ?
Nb2 K2 Nb2 53.41(10) 31 16_554 ?
Nb2 K2 Nb2 83.71(16) 18 31 ?
Nb2 K2 Nb2 59.10(10) 18 16_554 ?
Nb2 K2 Nb2 59.10(10) . 31 ?
Nb2 K2 Nb2 53.41(10) . 18 ?
O6 K2 Nb2 30.67(10) 31 31 ?
O6 K2 Nb2 30.67(10) 31 16_554 ?
O6 K2 Nb2 30.67(10) . 18 ?
O6 K2 Nb2 83.5(2) . 31 ?
O6 K2 Nb2 83.5(2) . 16_554 ?
O6 K2 Nb2 30.67(10) . . ?
O6 K2 Nb2 83.5(2) 31 . ?
O6 K2 Nb2 83.5(2) 31 18 ?
O6 K2 O6 98.4(4) 31 . ?
O11 K2 Nb2 29.65(6) 18 18 ?
O11 K2 Nb2 68.2(2) 18 . ?
O11 K2 Nb2 68.2(2) 18 31 ?
O11 K2 Nb2 68.2(2) . 18 ?
O11 K2 Nb2 29.65(6) . . ?
O11 K2 Nb2 29.65(6) 18 16_554 ?
O11 K2 Nb2 29.65(6) . 31 ?
O11 K2 Nb2 68.2(2) . 16_554 ?
O11 K2 O6 57.0(2) . . ?
O11 K2 O6 57.0(2) 18 . ?
O11 K2 O6 57.0(2) . 31 ?
O11 K2 O6 57.0(2) 18 31 ?
O11 K2 O11 67.2(5) 18 . ?
O3 K2 Nb2 142.2(6) . 16_554 ?
O3 K2 Nb2 85.7(8) . . ?
O3 K2 Nb2 142.2(6) 31 . ?
O3 K2 Nb2 142.2(6) . 31 ?
O3 K2 Nb2 85.7(8) 31 31 ?
O3 K2 Nb2 85.7(8) . 18 ?
O3 K2 Nb2 142.2(6) 31 18 ?
O3 K2 Nb2 85.7(8) 31 16_554 ?
O3 K2 O6 167.9(9) . 31 ?
O3 K2 O6 69.5(8) . . ?
O3 K2 O6 69.5(8) 31 31 ?
O3 K2 O6 167.9(9) 31 . ?
O3 K2 O11 113.6(7) 31 . ?
O3 K2 O11 113.6(7) 31 18 ?
O3 K2 O11 113.6(7) . 18 ?
O3 K2 O11 113.6(7) . . ?
O3 K2 O3 122.5(17) . 31 ?
O14 K2 Nb2 138.6(10) 18 . ?
O14 K2 Nb2 138.6(10) . 18 ?
O14 K2 Nb2 87.7(13) . . ?
O14 K2 Nb2 87.7(13) 18 18 ?
O14 K2 Nb2 87.7(13) 18 16_554 ?
O14 K2 Nb2 138.6(10) . 16_554 ?
O14 K2 Nb2 87.7(13) . 31 ?
O14 K2 Nb2 138.6(10) 18 31 ?
O14 K2 O6 108.1(9) . 31 ?
O14 K2 O6 108.1(9) . . ?
O14 K2 O6 108.1(9) 18 31 ?
O14 K2 O6 108.1(9) 18 . ?
O14 K2 O11 84.8(15) 18 18 ?
O14 K2 O11 152.1(16) . 18 ?
O14 K2 O11 84.8(15) . . ?
O14 K2 O11 152.1(16) 18 . ?
O14 K2 O3 76.8(7) . . ?
O14 K2 O3 76.8(7) 18 . ?
O14 K2 O3 76.8(7) 18 31 ?
O14 K2 O3 76.8(7) . 31 ?
O14 K2 O14 123(3) 18 . ?
N19 K1 N19 79.65(17) . 4 ?
N19 K1 N19 50.1(4) 4 19 ?
N19 K1 N19 129.9(4) 18 17 ?
N19 K1 N19 180.0(4) 20 4 ?
N19 K1 N19 180.0 . 17 ?
N19 K1 N19 129.9(4) . 2 ?
N19 K1 N19 100.35(17) . 19 ?
N19 K1 N19 100.35(17) 20 2 ?
N19 K1 N19 79.65(17) 18 19 ?
N19 K1 N19 79.65(17) 4 2 ?
N19 K1 N19 100.35(17) 4 17 ?
N19 K1 N19 50.1(4) . 18 ?
N19 K1 N19 79.65(17) 19 17 ?
N19 K1 N19 79.65(17) 20 18 ?
N19 K1 N19 129.9(4) 20 19 ?
N19 K1 N19 100.35(17) 4 18 ?
N19 K1 N19 100.35(17) 2 19 ?
N19 K1 N19 180.0(6) 2 18 ?
N19 K1 N19 180.0(6) 3 19 ?
N19 K1 N19 79.65(17) . 3 ?
N19 K1 N19 79.65(17) 20 17 ?
N19 K1 N19 50.1(4) 20 3 ?
N19 K1 N19 50.1(4) 2 17 ?
N19 K1 N19 129.9(4) 4 3 ?
N19 K1 N19 100.35(17) 3 17 ?
N19 K1 N19 79.65(17) 2 3 ?
N19 K1 N19 100.35(17) 18 3 ?
N19 K1 N19 100.35(17) . 20 ?
Cu7 N1 H1A 109.8 . . ?
Cu7 N1 H1B 109.8 . . ?
C8 N1 Cu7 109.6(14) . . ?
C8 N1 H1A 109.8 . . ?
C8 N1 H1B 109.8 . . ?
H1A N1 H1B 108.2 . . ?
C8 C3 H3A 109.5 . . ?
C8 C3 H3B 109.5 . . ?
C8 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

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
Nb2 V3 O5 Nb3 -36.1(3) . . . . ?
Nb2 V3 O5 Nb4 118.8(3) . . . . ?
Nb3 V3 O5 Nb4 154.9(5) . . . . ?
Nb4 V3 O5 Nb3 -154.9(5) . . . . ?
Nb5 V3 O5 Nb3 -120.3(2) . . . . ?
Nb5 V3 O5 Nb4 34.6(3) . . . . ?
Cu6 N19 C30 C25 31(3) . . . . ?
Cu6 N19 C30 C12 178(3) . . . . ?
Cu6 N22 C25 C30 8(3) . . . . ?
Cu7 N4 C7 C8 39.1(18) . . . . ?
Cu7 N4 C7 C1 177(3) . . . . ?
O7 V3 O5 Nb3 -78.9(4) 31 . . . ?
O7 V3 O5 Nb4 76.0(4) 31 . . . ?
O10 V3 O5 Nb3 -0.4(3) . . . . ?
O10 V3 O5 Nb4 154.5(3) . . . . ?
O13 V1 O13 Nb2 58.0(4) 31 . . 31 ?
O13 V1 O13 Nb2 -58.0(4) 31 . . 16_554 ?
O13 V1 O13 Nb3 180.0 31 . . 31 ?
O13 V1 O16 Nb4 177.7(4) 31 . . 31 ?
O13 V1 O16 Nb4 -62.8(6) . . . 31 ?
O13 V1 O16 Nb4 62.8(6) 31 . . . ?
O13 V1 O16 Nb4 -177.8(4) . . . . ?
O13 V1 O16 Nb5 -59.7(3) 31 . . . ?
O13 V1 O16 Nb5 59.7(3) . . . . ?
O16 V1 O13 Nb2 -61.7(6) . . . 31 ?
O16 V1 O13 Nb2 -177.8(4) . . . 16_554 ?
O16 V1 O13 Nb2 61.7(6) 18 . . 16_554 ?
O16 V1 O13 Nb2 177.8(4) 18 . . 31 ?
O16 V1 O13 Nb3 60.2(4) . . . 31 ?
O16 V1 O13 Nb3 -60.2(4) 18 . . 31 ?
O16 V1 O16 Nb4 -57.5(5) 18 . . . ?
O16 V1 O16 Nb4 57.5(5) 18 . . 31 ?
O16 V1 O16 Nb5 180.000(0) 18 . . . ?
O20 V3 O5 Nb3 -155.3(3) . . . . ?
O20 V3 O5 Nb4 -0.4(3) . . . . ?
N22 C25 C30 N19 -26(4) . . . . ?
N22 C25 C30 C12 -175(3) . . . . ?
O23 V3 O5 Nb3 100.8(6) . . . . ?
O23 V3 O5 Nb4 -104.3(6) . . . . ?
N4 C7 C8 N1 -44(2) . . . . ?
N4 C7 C8 C3 157(2) . . . . ?
C7 C8 N1 Cu7 25(2) . . . . ?
K1 N19 C30 C25 146(2) . . . . ?
K1 N19 C30 C12 -67(4) . . . . ?
C1 C7 C8 N1 168(3) . . . . ?
C1 C7 C8 C3 9(2) . . . . ?
C3 C8 N1 Cu7 177(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
