# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 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_a
_database_code_depnum_ccdc_archive 'CCDC 2192783'
loop_
_audit_author_name
_audit_author_address
'Yuquan Feng'
;Nanyang Normal University
China
;
_audit_update_record             
;
2022-07-26 deposited with the CCDC.	2022-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H104 B32 Cu6 N24 O104 V12'
_chemical_formula_weight         3731.75

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

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

_cell_length_a                   19.183(2)
_cell_length_b                   19.183(2)
_cell_length_c                   19.669(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7237.9(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.712
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3716
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.6107
_exptl_absorpt_correction_T_max  0.6648
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17414
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.56
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3205
_reflns_number_gt                2484
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0070P)²+380.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3205
_refine_ls_number_parameters     245
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.1364
_refine_ls_R_factor_gt           0.1098
_refine_ls_wR_factor_ref         0.2467
_refine_ls_wR_factor_gt          0.2372
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.092
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.65495(12) 0.75137(11) 1.0000 0.0210(5) Uani 1 2 d S . .
V2 V 0.51013(11) 0.79490(11) 1.0000 0.0190(5) Uani 1 2 d S . .
V3 V 0.36563(12) 0.76114(11) 1.0000 0.0208(5) Uani 1 2 d S . .
Cu1 Cu 0.5000 1.0000 1.0000 0.0384(7) Uani 1 4 d SD . .
Cu2 Cu 0.2500 0.7500 0.7500 0.1382(19) Uani 1 2 d SU . .
B1 B 0.5095(6) 0.8428(6) 0.8068(6) 0.025(2) Uani 1 1 d . . .
B2 B 0.5736(6) 0.7469(6) 0.8638(5) 0.024(2) Uani 1 1 d . . .
B3 B 0.4457(6) 0.7487(6) 0.8633(6) 0.024(2) Uani 1 1 d . . .
B4 B 0.3332(6) 0.6788(5) 0.8714(5) 0.021(2) Uani 1 1 d . . .
O1 O 0.5128(4) 0.9041(4) 0.7735(4) 0.0364(18) Uani 1 1 d . . .
H1E H 0.4732 0.9179 0.7653 0.055 Uiso 1 1 calc R . .
O1W O 0.0969(9) 0.6664(10) 0.8877(11) 0.139(6) Uani 1 1 d . . .
O2 O 0.5716(3) 0.8151(3) 0.8260(3) 0.0244(15) Uani 1 1 d . . .
O2W O 0.0968(7) 0.9940(8) 0.5669(8) 0.101(4) Uani 1 1 d . . .
O3 O 0.4467(3) 0.8145(3) 0.8238(4) 0.0268(15) Uani 1 1 d . . .
O3W O 0.1255(13) 0.0004(16) 0.7570(12) 0.098(9) Uani 0.50 1 d P . .
O4 O 0.5091(3) 0.7101(3) 0.8512(3) 0.0239(14) Uani 1 1 d . . .
O5 O 0.5806(3) 0.7621(3) 0.9363(3) 0.0244(14) Uani 1 1 d . . .
O6 O 0.4396(3) 0.7651(3) 0.9363(3) 0.0223(14) Uani 1 1 d . . .
O7 O 0.3865(4) 0.7078(4) 0.8389(3) 0.0284(15) Uani 1 1 d . . .
O8 O 0.3182(3) 0.6972(3) 0.9381(3) 0.0276(15) Uani 1 1 d . . .
O9 O 0.2930(4) 0.6322(4) 0.8385(3) 0.0279(15) Uani 1 1 d . . .
O10 O 0.3232(6) 0.8338(5) 1.0000 0.035(2) Uani 1 2 d S . .
O11 O 0.7032(6) 0.8195(6) 1.0000 0.039(3) Uani 1 2 d S . .
O12 O 0.5121(5) 0.8776(5) 1.0000 0.030(2) Uani 1 2 d S . .
C1 C 0.6359(10) 1.0054(18) 1.0381(5) 0.153(11) Uani 1 1 d DU . .
H1C H 0.6635 1.0451 1.0524 0.183 Uiso 1 1 calc R . .
H1D H 0.6611 0.9640 1.0524 0.183 Uiso 1 1 calc R . .
C2 C 0.185(3) 0.825(2) 0.844(2) 0.25(2) Uani 1 1 d DU . .
H2C H 0.1868 0.8036 0.8889 0.305 Uiso 1 1 calc R . .
H2D H 0.1470 0.8586 0.8454 0.305 Uiso 1 1 calc R . .
C3 C 0.252(2) 0.866(3) 0.835(2) 0.24(2) Uani 1 1 d DU . .
H3C H 0.2421 0.9145 0.8241 0.289 Uiso 1 1 calc R . .
H3D H 0.2795 0.8655 0.8769 0.289 Uiso 1 1 calc R . .
N1 N 0.5685(12) 1.007(2) 1.0792(12) 0.34(3) Uani 1 1 d DU . .
H1A H 0.5636 1.0476 1.1023 0.412 Uiso 1 1 calc R . .
H1B H 0.5649 0.9711 1.1079 0.412 Uiso 1 1 calc R . .
N2 N 0.1656(17) 0.7688(17) 0.7934(18) 0.196(12) Uani 1 1 d DU . .
H2A H 0.1335 0.7843 0.7637 0.235 Uiso 1 1 calc R . .
H2B H 0.1491 0.7307 0.8146 0.235 Uiso 1 1 calc R . .
N3 N 0.2919(16) 0.8320(16) 0.7783(16) 0.177(10) Uani 1 1 d DU . .
H3A H 0.3356 0.8227 0.7923 0.213 Uiso 1 1 calc R . .
H3B H 0.2947 0.8616 0.7430 0.213 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O11 1.602(10) . ?
V1 O5 1.908(6) . ?
V1 O5 1.908(6) 11_557 ?
V1 O8 1.981(7) 10_567 ?
V1 O8 1.981(7) 4_565 ?
V1 V2 2.901(3) . ?
V1 V3 3.031(3) 10_567 ?
V2 O12 1.586(9) . ?
V2 O6 1.931(6) . ?
V2 O6 1.931(6) 11_557 ?
V2 O5 1.948(7) 11_557 ?
V2 O5 1.948(7) . ?
V2 V3 2.847(3) . ?
V3 O10 1.614(10) . ?
V3 O6 1.894(7) 11_557 ?
V3 O6 1.894(7) . ?
V3 O8 1.953(7) . ?
V3 O8 1.953(7) 11_557 ?
V3 V1 3.031(3) 2_655 ?
Cu1 N1 2.04(2) 11_557 ?
Cu1 N1 2.04(2) . ?
Cu1 N1 2.04(2) 9_677 ?
Cu1 N1 2.04(2) 3_675 ?
Cu1 O12 2.360(9) 9_677 ?
Cu1 O12 2.360(9) . ?
Cu2 N3 1.85(3) . ?
Cu2 N3 1.85(3) 13_566 ?
Cu2 N2 1.87(3) 13_566 ?
Cu2 N2 1.87(3) . ?
B1 O1 1.348(13) . ?
B1 O2 1.358(13) . ?
B1 O3 1.361(13) . ?
B2 O4 1.447(13) . ?
B2 O9 1.449(12) 4_565 ?
B2 O5 1.461(13) . ?
B2 O2 1.505(12) . ?
B3 O4 1.443(13) . ?
B3 O7 1.461(13) . ?
B3 O6 1.476(13) . ?
B3 O3 1.483(12) . ?
B4 O7 1.327(13) . ?
B4 O9 1.345(13) . ?
B4 O8 1.389(12) . ?
O1 H1E 0.8200 . ?
O8 V1 1.981(7) 2_655 ?
O9 B2 1.449(12) 2_655 ?
C1 C1 1.50(2) 11_557 ?
C1 N1 1.53(2) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 N2 1.521(19) . ?
C2 C3 1.52(2) . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 N3 1.507(19) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
N1 H1A 0.9000 . ?
N1 H1B 0.9000 . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?

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
O11 V1 O5 110.1(4) . . ?
O11 V1 O5 110.1(4) . 11_557 ?
O5 V1 O5 82.0(4) . 11_557 ?
O11 V1 O8 108.3(4) . 10_567 ?
O5 V1 O8 141.4(3) . 10_567 ?
O5 V1 O8 88.5(3) 11_557 10_567 ?
O11 V1 O8 108.3(4) . 4_565 ?
O5 V1 O8 88.5(3) . 4_565 ?
O5 V1 O8 141.4(3) 11_557 4_565 ?
O8 V1 O8 75.9(4) 10_567 4_565 ?
O11 V1 V2 108.6(4) . . ?
O5 V1 V2 41.74(19) . . ?
O5 V1 V2 41.74(19) 11_557 . ?
O8 V1 V2 125.9(2) 10_567 . ?
O8 V1 V2 125.9(2) 4_565 . ?
O11 V1 V3 102.5(4) . 10_567 ?
O5 V1 V3 125.6(2) . 10_567 ?
O5 V1 V3 125.6(2) 11_557 10_567 ?
O8 V1 V3 39.3(2) 10_567 10_567 ?
O8 V1 V3 39.3(2) 4_565 10_567 ?
V2 V1 V3 148.95(10) . 10_567 ?
O12 V2 O6 108.2(3) . . ?
O12 V2 O6 108.2(3) . 11_557 ?
O6 V2 O6 80.9(4) . 11_557 ?
O12 V2 O5 107.9(3) . 11_557 ?
O6 V2 O5 143.9(3) . 11_557 ?
O6 V2 O5 88.5(3) 11_557 11_557 ?
O12 V2 O5 107.9(3) . . ?
O6 V2 O5 88.5(3) . . ?
O6 V2 O5 143.9(3) 11_557 . ?
O5 V2 O5 80.0(4) 11_557 . ?
O12 V2 V3 104.5(4) . . ?
O6 V2 V3 41.41(19) . . ?
O6 V2 V3 41.41(19) 11_557 . ?
O5 V2 V3 127.1(2) 11_557 . ?
O5 V2 V3 127.1(2) . . ?
O12 V2 V1 105.4(4) . . ?
O6 V2 V1 125.9(2) . . ?
O6 V2 V1 125.9(2) 11_557 . ?
O5 V2 V1 40.71(19) 11_557 . ?
O5 V2 V1 40.71(19) . . ?
V3 V2 V1 150.12(10) . . ?
O10 V3 O6 110.1(3) . 11_557 ?
O10 V3 O6 110.1(3) . . ?
O6 V3 O6 82.8(4) 11_557 . ?
O10 V3 O8 107.9(4) . . ?
O6 V3 O8 141.9(3) 11_557 . ?
O6 V3 O8 87.8(3) . . ?
O10 V3 O8 107.9(4) . 11_557 ?
O6 V3 O8 87.8(3) 11_557 11_557 ?
O6 V3 O8 141.9(3) . 11_557 ?
O8 V3 O8 77.2(4) . 11_557 ?
O10 V3 V2 107.1(4) . . ?
O6 V3 V2 42.41(19) 11_557 . ?
O6 V3 V2 42.41(19) . . ?
O8 V3 V2 126.6(2) . . ?
O8 V3 V2 126.6(2) 11_557 . ?
O10 V3 V1 101.9(4) . 2_655 ?
O6 V3 V1 125.5(2) 11_557 2_655 ?
O6 V3 V1 125.5(2) . 2_655 ?
O8 V3 V1 39.9(2) . 2_655 ?
O8 V3 V1 39.9(2) 11_557 2_655 ?
V2 V3 V1 150.92(10) . 2_655 ?
N1 Cu1 N1 99.4(16) 11_557 . ?
N1 Cu1 N1 80.6(16) 11_557 9_677 ?
N1 Cu1 N1 180.000(7) . 9_677 ?
N1 Cu1 N1 180.000(8) 11_557 3_675 ?
N1 Cu1 N1 80.6(16) . 3_675 ?
N1 Cu1 N1 99.4(16) 9_677 3_675 ?
N1 Cu1 O12 89.7(11) 11_557 9_677 ?
N1 Cu1 O12 89.7(11) . 9_677 ?
N1 Cu1 O12 90.3(11) 9_677 9_677 ?
N1 Cu1 O12 90.3(11) 3_675 9_677 ?
N1 Cu1 O12 90.3(11) 11_557 . ?
N1 Cu1 O12 90.3(11) . . ?
N1 Cu1 O12 89.7(11) 9_677 . ?
N1 Cu1 O12 89.7(11) 3_675 . ?
O12 Cu1 O12 180.000(2) 9_677 . ?
N3 Cu2 N3 180.000(5) . 13_566 ?
N3 Cu2 N2 85.7(14) . 13_566 ?
N3 Cu2 N2 94.3(14) 13_566 13_566 ?
N3 Cu2 N2 94.3(14) . . ?
N3 Cu2 N2 85.7(14) 13_566 . ?
N2 Cu2 N2 180.000(7) 13_566 . ?
O1 B1 O2 115.8(9) . . ?
O1 B1 O3 120.6(9) . . ?
O2 B1 O3 123.4(9) . . ?
O4 B2 O9 110.3(8) . 4_565 ?
O4 B2 O5 110.1(8) . . ?
O9 B2 O5 111.6(8) 4_565 . ?
O4 B2 O2 108.5(8) . . ?
O9 B2 O2 108.0(7) 4_565 . ?
O5 B2 O2 108.2(8) . . ?
O4 B3 O7 109.0(8) . . ?
O4 B3 O6 109.6(8) . . ?
O7 B3 O6 111.8(8) . . ?
O4 B3 O3 109.9(8) . . ?
O7 B3 O3 107.2(8) . . ?
O6 B3 O3 109.2(8) . . ?
O7 B4 O9 119.2(9) . . ?
O7 B4 O8 120.5(9) . . ?
O9 B4 O8 120.3(9) . . ?
B1 O1 H1E 109.5 . . ?
B1 O2 B2 120.0(7) . . ?
B1 O3 B3 118.7(8) . . ?
B3 O4 B2 116.2(7) . . ?
B2 O5 V1 133.5(6) . . ?
B2 O5 V2 128.8(6) . . ?
V1 O5 V2 97.6(3) . . ?
B3 O6 V3 134.1(6) . . ?
B3 O6 V2 129.7(6) . . ?
V3 O6 V2 96.2(3) . . ?
B4 O7 B3 131.7(8) . . ?
B4 O8 V3 130.7(6) . . ?
B4 O8 V1 128.1(6) . 2_655 ?
V3 O8 V1 100.8(3) . 2_655 ?
B4 O9 B2 130.8(8) . 2_655 ?
V2 O12 Cu1 173.0(6) . . ?
C1 C1 N1 122.0(9) 11_557 . ?
C1 C1 H1C 106.8 11_557 . ?
N1 C1 H1C 106.8 . . ?
C1 C1 H1D 106.8 11_557 . ?
N1 C1 H1D 106.8 . . ?
H1C C1 H1D 106.7 . . ?
N2 C2 C3 120(4) . . ?
N2 C2 H2C 107.3 . . ?
C3 C2 H2C 107.3 . . ?
N2 C2 H2D 107.3 . . ?
C3 C2 H2D 107.3 . . ?
H2C C2 H2D 106.9 . . ?
N3 C3 C2 107(4) . . ?
N3 C3 H3C 110.4 . . ?
C2 C3 H3C 110.4 . . ?
N3 C3 H3D 110.4 . . ?
C2 C3 H3D 110.4 . . ?
H3C C3 H3D 108.6 . . ?
C1 N1 Cu1 98.0(14) . . ?
C1 N1 H1A 112.2 . . ?
Cu1 N1 H1A 112.2 . . ?
C1 N1 H1B 112.2 . . ?
Cu1 N1 H1B 112.2 . . ?
H1A N1 H1B 109.8 . . ?
C2 N2 Cu2 103(3) . . ?
C2 N2 H2A 111.1 . . ?
Cu2 N2 H2A 111.1 . . ?
C2 N2 H2B 111.1 . . ?
Cu2 N2 H2B 111.1 . . ?
H2A N2 H2B 109.1 . . ?
C3 N3 Cu2 112(3) . . ?
C3 N3 H3A 109.2 . . ?
Cu2 N3 H3A 109.2 . . ?
C3 N3 H3B 109.2 . . ?
Cu2 N3 H3B 109.2 . . ?
H3A N3 H3B 107.9 . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.934
_refine_diff_density_min         -1.397
_refine_diff_density_rms         0.187
