# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 2071024'
loop_
_audit_author_name
_audit_author_address
'Jikun Li'
;Taishan University
China
;
_audit_update_record             
;
2021-05-23 deposited with the CCDC.	2021-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H30 N24 Ni3 O21 V6'
_chemical_formula_sum            'C12 H30 N24 Ni3 O21 V6'
_chemical_formula_weight         1328.37

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7600(11)
_cell_length_b                   10.5243(12)
_cell_length_c                   11.4568(13)
_cell_angle_alpha                105.810(2)
_cell_angle_beta                 91.541(2)
_cell_angle_gamma                114.335(2)
_cell_volume                     1018.6(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3634
_cell_measurement_theta_min      2.32
_cell_measurement_theta_max      28.38

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            BLUE
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.166
_exptl_crystal_F_000             660
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    2.770
_shelx_estimated_absorpt_T_min   0.568
_shelx_estimated_absorpt_T_max   0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.613
_exptl_absorpt_correction_T_max  0.717
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6122
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.871
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3792
_reflns_number_gt                3135
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0385P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3792
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0794
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.66199(6) -0.23831(6) 0.37951(5) 0.01976(14) Uani 1 1 d . . . . .
V2 V 1.12182(6) 0.27638(5) 0.39856(5) 0.01892(14) Uani 1 1 d . . . . .
V3 V 1.28781(6) 0.63024(5) 0.41403(5) 0.01967(14) Uani 1 1 d . . . . .
Ni1 Ni 0.71290(4) 0.09201(4) 0.31348(3) 0.01650(11) Uani 1 1 d . . . . .
Ni2 Ni 0.500000 0.000000 0.000000 0.01625(14) Uani 1 2 d S . P . .
O1 O 0.6771(3) -0.0732(2) 0.38885(19) 0.0224(5) Uani 1 1 d . . . . .
O2 O 0.7019(3) -0.3097(3) 0.2489(3) 0.0452(7) Uani 1 1 d . . . . .
O3 O 0.4720(3) -0.3573(3) 0.3888(3) 0.0444(7) Uani 1 1 d . . . . .
O4 O 0.9373(3) 0.1875(2) 0.3855(2) 0.0350(6) Uani 1 1 d . . . . .
O5 O 1.1667(4) 0.2339(4) 0.2639(3) 0.0632(9) Uani 1 1 d . . . . .
O6 O 1.2072(4) 0.2162(3) 0.4972(3) 0.0582(9) Uani 1 1 d . . . . .
O7 O 1.1791(3) 0.4695(2) 0.4567(2) 0.0339(6) Uani 1 1 d . . . . .
O8 O 1.1997(3) 0.6219(3) 0.2878(2) 0.0451(7) Uani 1 1 d . . . . .
O9 O 1.3075(3) 0.7777(2) 0.5237(2) 0.0333(6) Uani 1 1 d . . . . .
O10 O 0.3933(4) 0.5298(3) 0.0933(3) 0.0613(9) Uani 1 1 d . . . . .
H10A H 0.345189 0.521659 0.153656 0.074 Uiso 1 1 d R U . . .
H10B H 0.486497 0.559849 0.121270 0.074 Uiso 1 1 d R U . . .
O11 O 0.5119(7) 0.3636(7) 0.3034(6) 0.0621(18) Uani 0.5 1 d . . P . .
H11A H 0.443166 0.283244 0.307396 0.074 Uiso 0.5 1 d R U P . .
H11B H 0.493177 0.430749 0.349708 0.074 Uiso 0.5 1 d R U P . .
N1 N 0.6632(3) 0.2091(3) 0.1093(2) 0.0219(6) Uani 1 1 d . . . . .
N2 N 0.7402(3) 0.2447(3) 0.2242(2) 0.0211(6) Uani 1 1 d . . . . .
N3 N 0.8271(3) 0.4374(3) 0.1636(2) 0.0219(6) Uani 1 1 d . . . . .
N4 N 0.9138(3) 0.5793(3) 0.1550(3) 0.0294(7) Uani 1 1 d . . . . .
H4A H 0.879638 0.637079 0.198407 0.035 Uiso 1 1 d R U . . .
H4B H 1.004477 0.604662 0.189448 0.035 Uiso 1 1 d R U . . .
N5 N 0.3947(3) -0.0338(3) 0.1537(2) 0.0195(6) Uani 1 1 d . . . . .
N6 N 0.4802(3) 0.0053(3) 0.2665(2) 0.0207(6) Uani 1 1 d . . . . .
N7 N 0.2434(3) -0.0674(3) 0.2894(2) 0.0189(6) Uani 1 1 d . . . . .
N8 N 0.1069(3) -0.1068(3) 0.3403(3) 0.0265(6) Uani 1 1 d . . . . .
H8A H 0.104082 -0.163176 0.383070 0.032 Uiso 1 1 d R U . . .
H8B H 0.108771 -0.028641 0.390780 0.032 Uiso 1 1 d R U . . .
N9 N 0.7412(3) -0.0332(3) 0.1520(2) 0.0202(6) Uani 1 1 d . . . . .
N10 N 0.6461(3) -0.0900(3) 0.0406(2) 0.0203(6) Uani 1 1 d . . . . .
N11 N 0.8177(3) -0.1716(3) 0.0225(2) 0.0220(6) Uani 1 1 d . . . . .
N12 N 0.9129(3) -0.2397(3) -0.0234(3) 0.0301(7) Uani 1 1 d . . . . .
H12A H 0.867176 -0.326798 -0.017769 0.036 Uiso 1 1 d R U . . .
H12B H 0.911537 -0.245394 -0.099763 0.036 Uiso 1 1 d R U . . .
C1 C 0.8380(4) 0.3832(3) 0.2561(3) 0.0239(7) Uani 1 1 d . . . . .
H1 H 0.904268 0.435839 0.330193 0.029 Uiso 1 1 calc R U . . .
C2 C 0.7183(4) 0.3274(3) 0.0751(3) 0.0233(7) Uani 1 1 d . . . . .
H2 H 0.686429 0.333807 0.000505 0.028 Uiso 1 1 calc R U . . .
C3 C 0.2533(4) -0.0771(3) 0.1707(3) 0.0216(7) Uani 1 1 d . . . . .
H3 H 0.170914 -0.109917 0.109567 0.026 Uiso 1 1 calc R U . . .
C4 C 0.3860(3) -0.0156(3) 0.3460(3) 0.0201(7) Uani 1 1 d . . . . .
H4 H 0.413986 0.002863 0.429361 0.024 Uiso 1 1 calc R U . . .
C5 C 0.6946(4) -0.1743(3) -0.0349(3) 0.0238(7) Uani 1 1 d . . . . .
H5 H 0.650381 -0.228009 -0.116243 0.029 Uiso 1 1 calc R U . . .
C6 C 0.8429(4) -0.0832(3) 0.1380(3) 0.0221(7) Uani 1 1 d . . . . .
H6 H 0.921588 -0.061162 0.198793 0.027 Uiso 1 1 calc R U . . .


_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 O2 1.617(3) . ?
V1 O1 1.656(2) . ?
V1 O6 1.777(3) 2_756 ?
V1 O3 1.785(2) . ?
V2 O5 1.611(3) . ?
V2 O4 1.631(2) . ?
V2 O6 1.774(3) . ?
V2 O7 1.787(2) . ?
V3 O8 1.625(3) . ?
V3 O9 1.644(2) . ?
V3 O3 1.785(2) 1_665 ?
V3 O7 1.795(2) . ?
Ni1 O4 2.031(2) . ?
Ni1 O1 2.055(2) . ?
Ni1 N9 2.058(2) . ?
Ni1 N6 2.059(3) . ?
Ni1 O9 2.062(2) 2_766 ?
Ni1 N2 2.063(3) . ?
Ni2 N5 2.103(2) 2_655 ?
Ni2 N5 2.103(2) . ?
Ni2 N1 2.110(2) 2_655 ?
Ni2 N1 2.110(2) . ?
Ni2 N10 2.113(3) . ?
Ni2 N10 2.113(3) 2_655 ?
N1 C2 1.311(4) . ?
N1 N2 1.373(4) . ?
N2 C1 1.310(4) . ?
N3 C2 1.337(4) . ?
N3 C1 1.354(4) . ?
N3 N4 1.413(3) . ?
N5 C3 1.302(4) . ?
N5 N6 1.379(4) . ?
N6 C4 1.309(4) . ?
N7 C4 1.337(4) . ?
N7 C3 1.345(4) . ?
N7 N8 1.415(3) . ?
N9 C6 1.297(4) . ?
N9 N10 1.383(4) . ?
N10 C5 1.308(4) . ?
N11 C5 1.340(4) . ?
N11 C6 1.341(4) . ?
N11 N12 1.423(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 V1 O1 109.79(12) . . ?
O2 V1 O6 110.64(16) . 2_756 ?
O1 V1 O6 107.17(12) . 2_756 ?
O2 V1 O3 107.71(13) . . ?
O1 V1 O3 110.68(11) . . ?
O6 V1 O3 110.86(15) 2_756 . ?
O5 V2 O4 107.45(15) . . ?
O5 V2 O6 109.09(18) . . ?
O4 V2 O6 108.22(14) . . ?
O5 V2 O7 110.41(15) . . ?
O4 V2 O7 110.01(12) . . ?
O6 V2 O7 111.55(13) . . ?
O8 V3 O9 109.30(14) . . ?
O8 V3 O3 108.51(15) . 1_665 ?
O9 V3 O3 109.00(13) . 1_665 ?
O8 V3 O7 109.38(13) . . ?
O9 V3 O7 109.76(12) . . ?
O3 V3 O7 110.87(12) 1_665 . ?
O4 Ni1 O1 89.63(10) . . ?
O4 Ni1 N9 93.64(10) . . ?
O1 Ni1 N9 89.79(9) . . ?
O4 Ni1 N6 171.61(10) . . ?
O1 Ni1 N6 87.79(9) . . ?
N9 Ni1 N6 94.33(10) . . ?
O4 Ni1 O9 84.50(10) . 2_766 ?
O1 Ni1 O9 90.87(9) . 2_766 ?
N9 Ni1 O9 178.02(10) . 2_766 ?
N6 Ni1 O9 87.56(10) . 2_766 ?
O4 Ni1 N2 93.21(10) . . ?
O1 Ni1 N2 175.31(9) . . ?
N9 Ni1 N2 86.31(10) . . ?
N6 Ni1 N2 89.91(10) . . ?
O9 Ni1 N2 93.11(10) 2_766 . ?
N5 Ni2 N5 180.0 2_655 . ?
N5 Ni2 N1 90.33(10) 2_655 2_655 ?
N5 Ni2 N1 89.67(10) . 2_655 ?
N5 Ni2 N1 89.67(10) 2_655 . ?
N5 Ni2 N1 90.33(10) . . ?
N1 Ni2 N1 180.0 2_655 . ?
N5 Ni2 N10 89.29(10) 2_655 . ?
N5 Ni2 N10 90.71(10) . . ?
N1 Ni2 N10 90.96(10) 2_655 . ?
N1 Ni2 N10 89.04(10) . . ?
N5 Ni2 N10 90.71(10) 2_655 2_655 ?
N5 Ni2 N10 89.29(10) . 2_655 ?
N1 Ni2 N10 89.04(10) 2_655 2_655 ?
N1 Ni2 N10 90.96(10) . 2_655 ?
N10 Ni2 N10 180.0 . 2_655 ?
V1 O1 Ni1 151.34(13) . . ?
V3 O3 V1 145.38(15) 1_445 . ?
V2 O4 Ni1 160.19(16) . . ?
V2 O6 V1 155.44(18) . 2_756 ?
V2 O7 V3 137.88(15) . . ?
V3 O9 Ni1 160.27(15) . 2_766 ?
C2 N1 N2 107.2(2) . . ?
C2 N1 Ni2 125.6(2) . . ?
N2 N1 Ni2 126.99(19) . . ?
C1 N2 N1 107.6(3) . . ?
C1 N2 Ni1 129.0(2) . . ?
N1 N2 Ni1 123.07(18) . . ?
C2 N3 C1 106.6(3) . . ?
C2 N3 N4 124.4(3) . . ?
C1 N3 N4 129.0(3) . . ?
C3 N5 N6 106.7(2) . . ?
C3 N5 Ni2 132.1(2) . . ?
N6 N5 Ni2 120.96(19) . . ?
C4 N6 N5 107.4(2) . . ?
C4 N6 Ni1 123.4(2) . . ?
N5 N6 Ni1 129.18(19) . . ?
C4 N7 C3 106.1(3) . . ?
C4 N7 N8 128.5(3) . . ?
C3 N7 N8 125.5(3) . . ?
C6 N9 N10 107.4(2) . . ?
C6 N9 Ni1 126.6(2) . . ?
N10 N9 Ni1 125.7(2) . . ?
C5 N10 N9 106.6(3) . . ?
C5 N10 Ni2 128.9(2) . . ?
N9 N10 Ni2 122.19(19) . . ?
C5 N11 C6 106.4(3) . . ?
C5 N11 N12 130.0(3) . . ?
C6 N11 N12 123.5(3) . . ?
N2 C1 N3 108.9(3) . . ?
N1 C2 N3 109.6(3) . . ?
N5 C3 N7 110.2(3) . . ?
N6 C4 N7 109.7(3) . . ?
N10 C5 N11 109.8(3) . . ?
N9 C6 N11 109.8(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 V1 O1 Ni1 5.2(3) . . . . ?
O6 V1 O1 Ni1 125.4(3) 2_756 . . . ?
O3 V1 O1 Ni1 -113.6(3) . . . . ?
O2 V1 O3 V3 -125.9(3) . . . 1_445 ?
O1 V1 O3 V3 -5.9(4) . . . 1_445 ?
O6 V1 O3 V3 112.9(3) 2_756 . . 1_445 ?
O5 V2 O4 Ni1 -35.6(5) . . . . ?
O6 V2 O4 Ni1 -153.3(4) . . . . ?
O7 V2 O4 Ni1 84.6(4) . . . . ?
O5 V2 O6 V1 109.4(5) . . . 2_756 ?
O4 V2 O6 V1 -134.0(5) . . . 2_756 ?
O7 V2 O6 V1 -12.8(6) . . . 2_756 ?
O5 V2 O7 V3 -7.7(3) . . . . ?
O4 V2 O7 V3 -126.1(2) . . . . ?
O6 V2 O7 V3 113.8(2) . . . . ?
O8 V3 O7 V2 66.2(3) . . . . ?
O9 V3 O7 V2 -173.9(2) . . . . ?
O3 V3 O7 V2 -53.4(3) 1_665 . . . ?
O8 V3 O9 Ni1 118.3(5) . . . 2_766 ?
O3 V3 O9 Ni1 -123.3(5) 1_665 . . 2_766 ?
O7 V3 O9 Ni1 -1.7(5) . . . 2_766 ?
C2 N1 N2 C1 0.5(4) . . . . ?
Ni2 N1 N2 C1 175.8(2) . . . . ?
C2 N1 N2 Ni1 -173.6(2) . . . . ?
Ni2 N1 N2 Ni1 1.6(3) . . . . ?
C3 N5 N6 C4 -0.3(3) . . . . ?
Ni2 N5 N6 C4 174.2(2) . . . . ?
C3 N5 N6 Ni1 -177.2(2) . . . . ?
Ni2 N5 N6 Ni1 -2.6(3) . . . . ?
C6 N9 N10 C5 1.1(3) . . . . ?
Ni1 N9 N10 C5 -173.8(2) . . . . ?
C6 N9 N10 Ni2 -163.2(2) . . . . ?
Ni1 N9 N10 Ni2 21.9(3) . . . . ?
N1 N2 C1 N3 -0.7(4) . . . . ?
Ni1 N2 C1 N3 172.9(2) . . . . ?
C2 N3 C1 N2 0.6(4) . . . . ?
N4 N3 C1 N2 -177.3(3) . . . . ?
N2 N1 C2 N3 -0.2(4) . . . . ?
Ni2 N1 C2 N3 -175.5(2) . . . . ?
C1 N3 C2 N1 -0.3(4) . . . . ?
N4 N3 C2 N1 177.8(3) . . . . ?
N6 N5 C3 N7 0.1(3) . . . . ?
Ni2 N5 C3 N7 -173.6(2) . . . . ?
C4 N7 C3 N5 0.1(3) . . . . ?
N8 N7 C3 N5 -179.3(3) . . . . ?
N5 N6 C4 N7 0.4(3) . . . . ?
Ni1 N6 C4 N7 177.50(19) . . . . ?
C3 N7 C4 N6 -0.4(3) . . . . ?
N8 N7 C4 N6 179.1(3) . . . . ?
N9 N10 C5 N11 -1.2(3) . . . . ?
Ni2 N10 C5 N11 161.7(2) . . . . ?
C6 N11 C5 N10 0.8(4) . . . . ?
N12 N11 C5 N10 -176.7(3) . . . . ?
N10 N9 C6 N11 -0.7(3) . . . . ?
Ni1 N9 C6 N11 174.2(2) . . . . ?
C5 N11 C6 N9 0.0(4) . . . . ?
N12 N11 C6 N9 177.7(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O10 H10A O3 0.85 2.66 3.222(4) 125.0 1_565 yes
O10 H10A O8 0.85 2.44 3.168(4) 143.9 1_455 yes
O10 H10B O2 0.85 2.19 2.997(4) 158.0 1_565 yes
O11 H11A O5 0.85 2.54 3.035(7) 118.5 1_455 yes
O11 H11B O3 0.85 2.25 3.023(7) 151.3 1_565 yes
N4 H4A O2 0.86 2.08 2.868(4) 151.6 1_565 yes
N4 H4B O8 0.86 2.10 2.944(4) 166.1 . yes
N8 H8B O6 0.86 2.29 3.095(4) 156.3 1_455 yes
N12 H12A O10 0.86 2.48 3.148(4) 134.5 2_655 yes
N12 H12A N4 0.86 2.55 3.153(4) 128.2 1_545 yes
N12 H12B O5 0.86 2.06 2.866(5) 155.1 2_755 yes
C1 H1 O7 0.93 2.66 3.275(4) 124.4 2_766 yes
C2 H2 O10 0.93 2.35 3.159(5) 144.8 2_665 yes
C3 H3 N12 0.93 2.52 3.428(4) 165.3 1_455 yes
C4 H4 O1 0.93 2.34 3.083(4) 136.6 2_656 yes
C5 H5 O5 0.93 2.50 3.017(4) 115.3 2_755 yes
C5 H5 O11 0.93 2.33 3.242(7) 166.7 2_655 yes
C6 H6 N8 0.93 2.67 3.548(4) 158.4 1_655 yes

_refine_diff_density_max         0.596
_refine_diff_density_min         -0.565
_refine_diff_density_rms         0.089

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2
_database_code_depnum_ccdc_archive 'CCDC 2071025'
loop_
_audit_author_name
_audit_author_address
'Jikun Li'
;Taishan University
China
;
_audit_update_record             
;
2021-05-23 deposited with the CCDC.	2021-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H30 Co3 N24 O21 V6'
_chemical_formula_sum            'C12 H30 Co3 N24 O21 V6'
_chemical_formula_weight         1329.03

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8362(12)
_cell_length_b                   10.5565(13)
_cell_length_c                   11.5359(15)
_cell_angle_alpha                105.886(2)
_cell_angle_beta                 91.581(2)
_cell_angle_gamma                114.190(2)
_cell_volume                     1037.5(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4537
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      28.22

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.127
_exptl_crystal_F_000             657
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.558
_shelx_estimated_absorpt_T_min   0.579
_shelx_estimated_absorpt_T_max   0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.581
_exptl_absorpt_correction_T_max  0.681
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6128
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.859
_diffrn_reflns_theta_max         25.494
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3850
_reflns_number_gt                3382
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0475P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3850
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0910
_refine_ls_wR_factor_gt          0.0886
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_restrained_S_all      1.179
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.21256(6) 0.37085(5) 1.08967(5) 0.01946(14) Uani 1 1 d . . . . .
V2 V 0.15942(6) -0.24267(5) 0.88027(5) 0.02062(14) Uani 1 1 d . . . . .
V3 V 0.62311(6) 0.27784(5) 0.89925(5) 0.01962(14) Uani 1 1 d . . . . .
Co1 Co 0.000000 0.000000 0.500000 0.01709(14) Uani 1 2 d S . P . .
Co2 Co 0.21510(4) 0.09259(4) 0.81937(3) 0.01699(12) Uani 1 1 d . . . . .
O1 O 0.1925(3) 0.2217(2) 0.9823(2) 0.0359(6) Uani 1 1 d . . . . .
O2 O 0.2996(3) 0.3804(3) 1.2160(2) 0.0455(7) Uani 1 1 d . . . . .
O3 O 0.1764(2) -0.0768(2) 0.88992(19) 0.0238(5) Uani 1 1 d . . . . .
O4 O 0.0301(3) 0.3609(2) 1.1159(3) 0.0430(7) Uani 1 1 d . . . . .
O5 O 0.2034(3) -0.3126(3) 0.7520(3) 0.0487(7) Uani 1 1 d . . . . .
O6 O 0.4399(3) 0.1897(2) 0.8941(2) 0.0367(6) Uani 1 1 d . . . . .
O7 O 0.6800(3) 0.4713(2) 0.9548(2) 0.0352(6) Uani 1 1 d . . . . .
O8 O 0.6592(4) 0.2303(4) 0.7623(3) 0.0638(9) Uani 1 1 d . . . . .
O9 O 0.7172(4) 0.2218(3) 0.9934(3) 0.0606(10) Uani 1 1 d . . . . .
O10 O 0.1028(4) 0.4700(3) 0.4088(3) 0.0623(9) Uani 1 1 d . . . . .
H10C H 0.160961 0.450118 0.361521 0.075 Uiso 1 1 d R U . . .
H10D H 0.014021 0.428848 0.368631 0.075 Uiso 1 1 d R U . . .
O11 O 0.9947(7) 0.6416(7) 0.1935(6) 0.0588(16) Uani 0.5 1 d . . P . .
H11A H 0.938544 0.631216 0.248158 0.071 Uiso 0.5 1 d R U P . .
H11B H 1.008824 0.565036 0.168078 0.071 Uiso 0.5 1 d R U P . .
N1 N -0.0216(3) 0.0064(3) 0.7690(2) 0.0219(5) Uani 1 1 d . . . . .
N2 N -0.1066(3) -0.0346(3) 0.6556(2) 0.0211(5) Uani 1 1 d . . . . .
N3 N -0.2568(3) -0.0670(3) 0.7906(2) 0.0201(5) Uani 1 1 d . . . . .
N4 N -0.3913(3) -0.1050(3) 0.8419(2) 0.0266(6) Uani 1 1 d . . . . .
H4A H -0.390258 -0.165041 0.879103 0.032 Uiso 1 1 d R U . . .
H4B H -0.397146 -0.032361 0.894063 0.032 Uiso 1 1 d R U . . .
N5 N 0.2439(3) 0.2477(3) 0.7266(2) 0.0227(6) Uani 1 1 d . . . . .
N6 N 0.1653(3) 0.2118(3) 0.6119(2) 0.0236(6) Uani 1 1 d . . . . .
N7 N 0.3294(3) 0.4389(2) 0.6657(2) 0.0225(6) Uani 1 1 d . . . . .
N8 N 0.4162(3) 0.5800(3) 0.6568(3) 0.0306(7) Uani 1 1 d . . . . .
H8A H 0.509921 0.615793 0.687024 0.037 Uiso 1 1 d R U . . .
H8B H 0.383231 0.641743 0.693774 0.037 Uiso 1 1 d R U . . .
N9 N 0.2439(3) -0.0340(3) 0.6529(2) 0.0215(6) Uani 1 1 d . . . . .
N10 N 0.1486(3) -0.0912(3) 0.5417(2) 0.0218(6) Uani 1 1 d . . . . .
N11 N 0.3197(3) -0.1724(3) 0.5233(2) 0.0226(6) Uani 1 1 d . . . . .
N12 N 0.4127(3) -0.2417(3) 0.4776(3) 0.0314(7) Uani 1 1 d . . . . .
H12B H 0.429289 -0.243935 0.404397 0.038 Uiso 1 1 d R U . . .
H12A H 0.359369 -0.330185 0.476457 0.038 Uiso 1 1 d R U . . .
C1 C -0.2472(3) -0.0783(3) 0.6728(3) 0.0233(7) Uani 1 1 d . . . . .
H1 H -0.329077 -0.112540 0.611847 0.028 Uiso 1 1 calc R U . . .
C2 C -0.1149(3) -0.0140(3) 0.8473(3) 0.0220(6) Uani 1 1 d . . . . .
H2 H -0.087275 0.005398 0.930228 0.026 Uiso 1 1 calc R U . . .
C3 C 0.2205(4) 0.3305(3) 0.5779(3) 0.0241(7) Uani 1 1 d . . . . .
H3 H 0.188488 0.337506 0.504323 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3394(4) 0.3846(3) 0.7571(3) 0.0249(7) Uani 1 1 d . . . . .
H4 H 0.404899 0.437288 0.830792 0.030 Uiso 1 1 calc R U . . .
C5 C 0.1972(4) -0.1745(3) 0.4664(3) 0.0251(7) Uani 1 1 d . . . . .
H5 H 0.153592 -0.227487 0.385384 0.030 Uiso 1 1 calc R U . . .
C6 C 0.3443(4) -0.0840(3) 0.6387(3) 0.0244(7) Uani 1 1 d . . . . .
H6 H 0.422145 -0.062229 0.699181 0.029 Uiso 1 1 calc R U . . .


_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 O2 1.627(2) . ?
V1 O1 1.648(2) . ?
V1 O7 1.792(2) 2_667 ?
V1 O4 1.794(2) . ?
V2 O5 1.619(3) . ?
V2 O3 1.6612(19) . ?
V2 O9 1.776(3) 2_657 ?
V2 O4 1.779(2) 2_557 ?
V3 O8 1.618(3) . ?
V3 O6 1.645(2) . ?
V3 O9 1.769(2) . ?
V3 O7 1.795(2) . ?
Co1 N2 2.145(3) . ?
Co1 N2 2.145(3) 2_556 ?
Co1 N6 2.153(2) . ?
Co1 N6 2.153(2) 2_556 ?
Co1 N10 2.160(2) . ?
Co1 N10 2.160(2) 2_556 ?
Co2 O6 2.058(2) . ?
Co2 O3 2.064(2) . ?
Co2 O1 2.076(2) . ?
Co2 N1 2.118(2) . ?
Co2 N9 2.119(2) . ?
Co2 N5 2.122(3) . ?
O10 H10C 0.8500 . ?
O10 H10D 0.8500 . ?
O11 H11A 0.8501 . ?
O11 H11B 0.8500 . ?
N1 C2 1.301(4) . ?
N1 N2 1.390(3) . ?
N2 C1 1.307(4) . ?
N3 C2 1.340(4) . ?
N3 C1 1.341(4) . ?
N3 N4 1.414(4) . ?
N4 H4A 0.8599 . ?
N4 H4B 0.8600 . ?
N5 C4 1.298(4) . ?
N5 N6 1.386(3) . ?
N6 C3 1.319(4) . ?
N7 C3 1.335(4) . ?
N7 C4 1.350(4) . ?
N7 N8 1.416(3) . ?
N8 H8A 0.8600 . ?
N8 H8B 0.8601 . ?
N9 C6 1.293(4) . ?
N9 N10 1.390(3) . ?
N10 C5 1.306(4) . ?
N11 C5 1.345(4) . ?
N11 C6 1.348(4) . ?
N11 N12 1.419(4) . ?
N12 H12B 0.8599 . ?
N12 H12A 0.8599 . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 V1 O1 109.02(13) . . ?
O2 V1 O7 109.71(13) . 2_667 ?
O1 V1 O7 109.86(12) . 2_667 ?
O2 V1 O4 107.91(15) . . ?
O1 V1 O4 109.48(12) . . ?
O7 V1 O4 110.82(11) 2_667 . ?
O5 V2 O3 109.70(13) . . ?
O5 V2 O9 111.45(16) . 2_657 ?
O3 V2 O9 106.76(11) . 2_657 ?
O5 V2 O4 107.53(13) . 2_557 ?
O3 V2 O4 110.77(11) . 2_557 ?
O9 V2 O4 110.66(15) 2_657 2_557 ?
O8 V3 O6 107.55(15) . . ?
O8 V3 O9 108.16(18) . . ?
O6 V3 O9 108.91(15) . . ?
O8 V3 O7 110.78(16) . . ?
O6 V3 O7 109.71(12) . . ?
O9 V3 O7 111.62(12) . . ?
N2 Co1 N2 180.0 . 2_556 ?
N2 Co1 N6 90.17(10) . . ?
N2 Co1 N6 89.83(10) 2_556 . ?
N2 Co1 N6 89.83(10) . 2_556 ?
N2 Co1 N6 90.17(10) 2_556 2_556 ?
N6 Co1 N6 180.0 . 2_556 ?
N2 Co1 N10 90.60(10) . . ?
N2 Co1 N10 89.40(10) 2_556 . ?
N6 Co1 N10 88.53(9) . . ?
N6 Co1 N10 91.47(9) 2_556 . ?
N2 Co1 N10 89.40(10) . 2_556 ?
N2 Co1 N10 90.60(10) 2_556 2_556 ?
N6 Co1 N10 91.47(9) . 2_556 ?
N6 Co1 N10 88.53(9) 2_556 2_556 ?
N10 Co1 N10 180.0 . 2_556 ?
O6 Co2 O3 90.54(9) . . ?
O6 Co2 O1 84.28(10) . . ?
O3 Co2 O1 91.77(9) . . ?
O6 Co2 N1 171.41(10) . . ?
O3 Co2 N1 87.94(9) . . ?
O1 Co2 N1 87.32(10) . . ?
O6 Co2 N9 94.52(10) . . ?
O3 Co2 N9 89.37(9) . . ?
O1 Co2 N9 178.35(10) . . ?
N1 Co2 N9 93.91(10) . . ?
O6 Co2 N5 93.26(10) . . ?
O3 Co2 N5 173.28(9) . . ?
O1 Co2 N5 94.11(10) . . ?
N1 Co2 N5 89.11(10) . . ?
N9 Co2 N5 84.82(10) . . ?
V1 O1 Co2 158.75(16) . . ?
V2 O3 Co2 152.71(13) . . ?
V2 O4 V1 145.04(14) 2_557 . ?
V3 O6 Co2 156.57(16) . . ?
V1 O7 V3 137.82(16) 2_667 . ?
V3 O9 V2 156.59(17) . 2_657 ?
H10C O10 H10D 108.2 . . ?
H11A O11 H11B 108.2 . . ?
C2 N1 N2 107.4(2) . . ?
C2 N1 Co2 122.8(2) . . ?
N2 N1 Co2 129.8(2) . . ?
C1 N2 N1 106.2(3) . . ?
C1 N2 Co1 132.4(2) . . ?
N1 N2 Co1 121.12(19) . . ?
C2 N3 C1 106.0(3) . . ?
C2 N3 N4 128.1(3) . . ?
C1 N3 N4 125.9(2) . . ?
N3 N4 H4A 105.2 . . ?
N3 N4 H4B 114.0 . . ?
H4A N4 H4B 108.3 . . ?
C4 N5 N6 107.3(2) . . ?
C4 N5 Co2 129.4(2) . . ?
N6 N5 Co2 123.17(18) . . ?
C3 N6 N5 106.8(2) . . ?
C3 N6 Co1 125.3(2) . . ?
N5 N6 Co1 127.61(19) . . ?
C3 N7 C4 106.6(2) . . ?
C3 N7 N8 124.1(3) . . ?
C4 N7 N8 129.2(2) . . ?
N7 N8 H8A 113.3 . . ?
N7 N8 H8B 111.9 . . ?
H8A N8 H8B 106.8 . . ?
C6 N9 N10 107.4(2) . . ?
C6 N9 Co2 126.2(2) . . ?
N10 N9 Co2 126.11(18) . . ?
C5 N10 N9 106.7(2) . . ?
C5 N10 Co1 128.6(2) . . ?
N9 N10 Co1 122.35(17) . . ?
C5 N11 C6 106.0(3) . . ?
C5 N11 N12 130.0(3) . . ?
C6 N11 N12 124.0(3) . . ?
N11 N12 H12B 115.3 . . ?
N11 N12 H12A 102.2 . . ?
H12B N12 H12A 107.6 . . ?
N2 C1 N3 110.5(3) . . ?
N2 C1 H1 124.8 . . ?
N3 C1 H1 124.8 . . ?
N1 C2 N3 110.0(3) . . ?
N1 C2 H2 125.0 . . ?
N3 C2 H2 125.0 . . ?
N6 C3 N7 109.5(3) . . ?
N6 C3 H3 125.3 . . ?
N7 C3 H3 125.3 . . ?
N5 C4 N7 109.8(3) . . ?
N5 C4 H4 125.1 . . ?
N7 C4 H4 125.1 . . ?
N10 C5 N11 109.9(3) . . ?
N10 C5 H5 125.0 . . ?
N11 C5 H5 125.0 . . ?
N9 C6 N11 110.1(3) . . ?
N9 C6 H6 125.0 . . ?
N11 C6 H6 125.0 . . ?

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
O2 V1 O1 Co2 -119.0(4) . . . . ?
O7 V1 O1 Co2 1.3(5) 2_667 . . . ?
O4 V1 O1 Co2 123.2(4) . . . . ?
O5 V2 O3 Co2 6.0(3) . . . . ?
O9 V2 O3 Co2 126.9(3) 2_657 . . . ?
O4 V2 O3 Co2 -112.5(3) 2_557 . . . ?
O2 V1 O4 V2 -84.3(3) . . . 2_557 ?
O1 V1 O4 V2 34.3(4) . . . 2_557 ?
O7 V1 O4 V2 155.6(3) 2_667 . . 2_557 ?
O8 V3 O6 Co2 -33.0(4) . . . . ?
O9 V3 O6 Co2 -150.0(3) . . . . ?
O7 V3 O6 Co2 87.5(4) . . . . ?
O8 V3 O7 V1 -10.7(3) . . . 2_667 ?
O6 V3 O7 V1 -129.3(2) . . . 2_667 ?
O9 V3 O7 V1 109.8(2) . . . 2_667 ?
O8 V3 O9 V2 124.2(6) . . . 2_657 ?
O6 V3 O9 V2 -119.2(6) . . . 2_657 ?
O7 V3 O9 V2 2.1(7) . . . 2_657 ?
C2 N1 N2 C1 -0.4(3) . . . . ?
Co2 N1 N2 C1 -178.8(2) . . . . ?
C2 N1 N2 Co1 173.71(19) . . . . ?
Co2 N1 N2 Co1 -4.7(3) . . . . ?
C4 N5 N6 C3 1.1(3) . . . . ?
Co2 N5 N6 C3 -174.5(2) . . . . ?
C4 N5 N6 Co1 175.6(2) . . . . ?
Co2 N5 N6 Co1 0.0(3) . . . . ?
C6 N9 N10 C5 0.5(3) . . . . ?
Co2 N9 N10 C5 -173.3(2) . . . . ?
C6 N9 N10 Co1 -163.1(2) . . . . ?
Co2 N9 N10 Co1 23.0(3) . . . . ?
N1 N2 C1 N3 0.3(3) . . . . ?
Co1 N2 C1 N3 -172.87(19) . . . . ?
C2 N3 C1 N2 -0.1(3) . . . . ?
N4 N3 C1 N2 -179.7(3) . . . . ?
N2 N1 C2 N3 0.3(3) . . . . ?
Co2 N1 C2 N3 178.90(18) . . . . ?
C1 N3 C2 N1 -0.2(3) . . . . ?
N4 N3 C2 N1 179.5(3) . . . . ?
N5 N6 C3 N7 -0.1(3) . . . . ?
Co1 N6 C3 N7 -174.8(2) . . . . ?
C4 N7 C3 N6 -0.8(4) . . . . ?
N8 N7 C3 N6 177.6(3) . . . . ?
N6 N5 C4 N7 -1.6(4) . . . . ?
Co2 N5 C4 N7 173.6(2) . . . . ?
C3 N7 C4 N5 1.5(4) . . . . ?
N8 N7 C4 N5 -176.8(3) . . . . ?
N9 N10 C5 N11 -0.6(4) . . . . ?
Co1 N10 C5 N11 161.7(2) . . . . ?
C6 N11 C5 N10 0.5(4) . . . . ?
N12 N11 C5 N10 -177.8(3) . . . . ?
N10 N9 C6 N11 -0.3(4) . . . . ?
Co2 N9 C6 N11 173.6(2) . . . . ?
C5 N11 C6 N9 -0.1(4) . . . . ?
N12 N11 C6 N9 178.3(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O10 H10C O2 0.85 2.34 3.190(5) 174.2 1_554 yes
O10 H10D O5 0.85 2.18 3.029(4) 173.5 2_556 yes
O11 H11A N5 0.85 2.58 3.083(7) 119.2 2_666 yes
O11 H11A N6 0.85 2.53 3.194(7) 135.5 2_666 yes
O11 H11B O4 0.85 2.17 3.018(6) 174.2 1_654 yes
N4 H4B O9 0.86 2.36 3.111(4) 146.7 1_455 yes
N8 H8A O2 0.86 2.14 2.937(4) 154.8 2_667 yes
N8 H8B O5 0.86 2.10 2.874(4) 149.9 1_565 yes
N12 H12B O8 0.86 2.15 2.883(4) 142.5 2_656 yes
N12 H12A O10 0.86 2.46 3.182(4) 141.9 1_545 yes
N12 H12A N8 0.86 2.64 3.162(4) 119.9 1_545 yes
C1 H1 N12 0.93 2.55 3.459(4) 166.2 1_455 yes
C2 H2 O3 0.93 2.33 3.076(4) 137.0 2_557 yes
C3 H3 O10 0.93 2.38 3.188(4) 145.9 . yes
C5 H5 O8 0.93 2.55 3.055(4) 114.8 2_656 yes
C5 H5 O11 0.93 2.37 3.284(7) 167.5 1_445 yes
C6 H6 N4 0.93 2.68 3.568(4) 159.1 1_655 yes

_refine_diff_density_max         0.805
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.090

####################################################################### 
# 
# 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_201028a
_database_code_depnum_ccdc_archive 'CCDC 2071026'
loop_
_audit_author_name
_audit_author_address
'Jikun Li'
;Taishan University
China
;
_audit_update_record             
;
2021-05-23 deposited with the CCDC.	2021-07-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H17 Cu3 N12 O18 V5'
_chemical_formula_sum            'C6 H17 Cu3 N12 O18 V5'
_chemical_formula_weight         990.63

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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5295(8)
_cell_length_b                   12.5511(11)
_cell_length_c                   12.5513(12)
_cell_angle_alpha                86.213(4)
_cell_angle_beta                 75.886(2)
_cell_angle_gamma                75.883(2)
_cell_volume                     1263.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2347
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.89

_exptl_crystal_description       needle
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.603
_exptl_crystal_F_000             966
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    4.343
_shelx_estimated_absorpt_T_min   0.526
_shelx_estimated_absorpt_T_max   0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6209
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.358
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_full        24.993
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.964
_reflns_number_total             4267
_reflns_number_gt                3035
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1620P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4267
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0970
_refine_ls_wR_factor_ref         0.2584
_refine_ls_wR_factor_gt          0.2410
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.110
_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_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
Cu1 Cu 0.46797(18) 0.38160(11) 0.33471(10) 0.0263(4) Uani 1 1 d . . . . .
Cu2 Cu 0.42961(19) 0.23161(11) 0.13587(11) 0.0299(4) Uani 1 1 d . . . . .
Cu3 Cu 0.3021(2) 0.16299(11) 0.39764(11) 0.0324(4) Uani 1 1 d . . . . .
V1 V 0.3438(2) 0.64276(16) 0.31495(15) 0.0273(5) Uani 1 1 d . . . . .
V2 V 0.1519(2) 0.74573(15) 0.56406(15) 0.0260(5) Uani 1 1 d . . . . .
V3 V 0.2285(2) -0.01745(15) 0.59968(15) 0.0264(5) Uani 1 1 d . . . . .
V4 V 0.2374(3) 0.02659(16) 0.83784(16) 0.0296(5) Uani 1 1 d . . . . .
V5 V 0.3894(3) 0.22853(15) 0.87147(15) 0.0263(5) Uani 1 1 d . . . . .
N1 N 0.5790(13) 0.3992(8) 0.1814(7) 0.032(2) Uani 1 1 d . . . . .
N2 N 0.5467(12) 0.3481(8) 0.1016(7) 0.028(2) Uani 1 1 d . . . . .
N3 N 0.7323(13) 0.4344(8) 0.0336(8) 0.035(2) Uani 1 1 d . . . . .
N4 N 0.8654(15) 0.4648(10) -0.0363(9) 0.048(3) Uani 1 1 d . . . . .
H4A H 0.831297 0.531588 -0.063101 0.072 Uiso 1 1 d R U . . .
H4B H 0.907493 0.417069 -0.091206 0.072 Uiso 1 1 d R U . . .
N5 N 0.3343(11) 0.1046(8) 0.1746(8) 0.028(2) Uani 1 1 d . . . . .
N6 N 0.2890(12) 0.0756(8) 0.2819(8) 0.030(2) Uani 1 1 d . . . . .
N7 N 0.2405(12) -0.0351(7) 0.1799(8) 0.031(2) Uani 1 1 d . . . . .
N8 N 0.1996(14) -0.1252(8) 0.1480(10) 0.040(3) Uani 1 1 d . U . . .
H8A H 0.214782 -0.138068 0.079347 0.048 Uiso 1 1 calc R U . . .
H8B H 0.158769 -0.168824 0.196710 0.048 Uiso 1 1 calc R U . . .
N9 N 0.2734(13) 0.2716(8) 0.5037(8) 0.030(2) Uani 1 1 d . . . . .
N10 N 0.3282(12) 0.3653(8) 0.4779(8) 0.031(2) Uani 1 1 d . . . . .
N11 N 0.1707(13) 0.3857(9) 0.6351(8) 0.036(2) Uani 1 1 d . . . . .
N12 N 0.0815(14) 0.4337(9) 0.7337(8) 0.043(3) Uani 1 1 d . . . . .
H12A H 0.133484 0.405122 0.786166 0.064 Uiso 1 1 d R U . . .
H12C H 0.074526 0.505735 0.728822 0.064 Uiso 1 1 d R U . . .
O1 O 0.2104(12) 0.7243(8) 0.4207(7) 0.046(2) Uani 1 1 d . . . . .
O2 O 0.4495(11) 0.5319(6) 0.3643(6) 0.0314(19) Uani 1 1 d . . . . .
O3 O 0.2399(13) 0.6062(8) 0.2428(8) 0.050(2) Uani 1 1 d . . . . .
O4 O 0.4904(12) 0.7076(7) 0.2300(7) 0.044(2) Uani 1 1 d . . . . .
O5 O -0.0184(10) 0.7087(6) 0.6158(7) 0.0334(19) Uani 1 1 d . . . . .
O6 O 0.2952(11) 0.6745(7) 0.6169(7) 0.037(2) Uani 1 1 d . . . . .
O7 O 0.1224(11) 0.8844(7) 0.5902(8) 0.039(2) Uani 1 1 d . . . . .
O8 O 0.1427(11) 0.0518(7) 0.7268(7) 0.0346(19) Uani 1 1 d . . . . .
O9 O 0.2039(11) 0.0753(7) 0.5035(6) 0.0314(18) Uani 1 1 d . . . . .
O10 O 0.4170(12) -0.0726(7) 0.5910(7) 0.042(2) Uani 1 1 d . . . . .
O11 O 0.3925(11) 0.0996(7) 0.8245(8) 0.041(2) Uani 1 1 d . . . . .
O12 O 0.0960(11) 0.0723(8) 0.9441(7) 0.041(2) Uani 1 1 d . . . . .
O13 O 0.3084(12) -0.1020(7) 0.8553(8) 0.045(2) Uani 1 1 d . . . . .
O14 O 0.4597(11) 0.2094(7) 0.9841(6) 0.037(2) Uani 1 1 d . . . . .
O15 O 0.2077(12) 0.3038(8) 0.8979(8) 0.051(3) Uani 1 1 d . . . . .
O16 O 0.4368(10) 0.2433(6) 0.2906(6) 0.0246(16) Uani 1 1 d . . . . .
H16 H 0.532812 0.202503 0.289085 0.030 Uiso 1 1 d R U . . .
O17 O 0.1582(12) 0.3376(7) 0.1711(8) 0.045(2) Uani 1 1 d . . . . .
H17B H 0.114530 0.332322 0.239169 0.054 Uiso 1 1 d R U . . .
H17C H 0.104040 0.310092 0.136039 0.054 Uiso 1 1 d R U . . .
O18 O 0.9498(13) 0.2306(9) 0.0995(10) 0.068(3) Uani 1 1 d . . . . .
H18C H 1.013196 0.189695 0.047229 0.082 Uiso 1 1 d R U . . .
H18D H 0.864027 0.205155 0.123839 0.082 Uiso 1 1 d R U . . .
C1 C 0.6431(16) 0.3706(10) 0.0120(9) 0.035(3) Uani 1 1 d . U . . .
H1 H 0.649040 0.345563 -0.057279 0.042 Uiso 1 1 calc R U . . .
C2 C 0.6881(16) 0.4516(11) 0.1390(10) 0.038(3) Uani 1 1 d . U . . .
H2 H 0.730077 0.495192 0.176763 0.046 Uiso 1 1 calc R U . . .
C3 C 0.2329(15) -0.0104(9) 0.2828(10) 0.034(3) Uani 1 1 d . U . . .
H3 H 0.193386 -0.049185 0.345225 0.040 Uiso 1 1 calc R U . . .
C4 C 0.3025(15) 0.0378(9) 0.1176(10) 0.029(3) Uani 1 1 d . U . . .
H4 H 0.320848 0.040379 0.041463 0.035 Uiso 1 1 calc R U . . .
C5 C 0.2654(16) 0.4300(10) 0.5565(9) 0.031(3) Uani 1 1 d . U . . .
H5 H 0.283567 0.499864 0.558641 0.038 Uiso 1 1 calc R U . . .
C6 C 0.1763(16) 0.2877(9) 0.6010(9) 0.031(3) Uani 1 1 d . U . . .
H6 H 0.119435 0.237811 0.640612 0.037 Uiso 1 1 calc R U . . .


_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
Cu1 O2 1.908(8) . ?
Cu1 N10 1.928(10) . ?
Cu1 N1 1.950(9) . ?
Cu1 O16 1.953(7) . ?
Cu1 O6 2.189(9) 2_666 ?
Cu2 O14 1.889(8) 1_554 ?
Cu2 N2 1.934(10) . ?
Cu2 N5 1.943(10) . ?
Cu2 O16 1.974(7) . ?
Cu2 O17 2.324(9) . ?
Cu3 O9 1.842(8) . ?
Cu3 N9 1.899(10) . ?
Cu3 N6 1.917(10) . ?
Cu3 O16 1.943(8) . ?
Cu3 O10 2.422(9) 2_656 ?
V1 O3 1.569(9) . ?
V1 O2 1.637(8) . ?
V1 O1 1.726(9) . ?
V1 O4 1.759(9) . ?
V2 O6 1.587(8) . ?
V2 O5 1.605(8) . ?
V2 O7 1.738(8) . ?
V2 O1 1.766(9) . ?
V3 O10 1.568(9) . ?
V3 O9 1.635(7) . ?
V3 O7 1.723(9) 1_545 ?
V3 O8 1.772(8) . ?
V4 O12 1.594(9) . ?
V4 O13 1.601(8) . ?
V4 O8 1.749(8) . ?
V4 O11 1.756(8) . ?
V5 O15 1.575(9) . ?
V5 O14 1.648(8) . ?
V5 O4 1.716(8) 2_666 ?
V5 O11 1.750(8) . ?
N1 C2 1.262(16) . ?
N1 N2 1.341(13) . ?
N2 C1 1.280(15) . ?
N3 C2 1.301(16) . ?
N3 C1 1.312(16) . ?
N3 N4 1.372(15) . ?
N4 H4A 0.8900 . ?
N4 H4B 0.8900 . ?
N5 C4 1.255(15) . ?
N5 N6 1.358(13) . ?
N6 C3 1.281(15) . ?
N7 C4 1.291(15) . ?
N7 C3 1.331(16) . ?
N7 N8 1.371(13) . ?
N8 H8A 0.8600 . ?
N8 H8B 0.8600 . ?
N9 C6 1.295(15) . ?
N9 N10 1.360(14) . ?
N10 C5 1.248(15) . ?
N11 C5 1.300(15) . ?
N11 C6 1.315(15) . ?
N11 N12 1.376(13) . ?
N12 H12A 0.8900 . ?
N12 H12C 0.8900 . ?
O16 H16 0.8499 . ?
O17 H17B 0.8500 . ?
O17 H17C 0.8500 . ?
O18 H18C 0.8500 . ?
O18 H18D 0.8500 . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 N10 90.5(4) . . ?
O2 Cu1 N1 91.5(4) . . ?
N10 Cu1 N1 171.2(4) . . ?
O2 Cu1 O16 165.5(3) . . ?
N10 Cu1 O16 89.4(4) . . ?
N1 Cu1 O16 86.6(4) . . ?
O2 Cu1 O6 93.4(3) . 2_666 ?
N10 Cu1 O6 96.1(4) . 2_666 ?
N1 Cu1 O6 92.3(4) . 2_666 ?
O16 Cu1 O6 101.0(3) . 2_666 ?
O14 Cu2 N2 89.6(4) 1_554 . ?
O14 Cu2 N5 92.1(4) 1_554 . ?
N2 Cu2 N5 173.6(4) . . ?
O14 Cu2 O16 170.7(4) 1_554 . ?
N2 Cu2 O16 87.8(3) . . ?
N5 Cu2 O16 89.5(3) . . ?
O14 Cu2 O17 98.4(4) 1_554 . ?
N2 Cu2 O17 99.0(4) . . ?
N5 Cu2 O17 86.9(4) . . ?
O16 Cu2 O17 90.8(3) . . ?
O9 Cu3 N9 91.1(4) . . ?
O9 Cu3 N6 91.7(4) . . ?
N9 Cu3 N6 167.1(4) . . ?
O9 Cu3 O16 171.5(3) . . ?
N9 Cu3 O16 89.3(4) . . ?
N6 Cu3 O16 89.8(3) . . ?
O9 Cu3 O10 94.4(3) . 2_656 ?
N9 Cu3 O10 95.0(4) . 2_656 ?
N6 Cu3 O10 97.4(4) . 2_656 ?
O16 Cu3 O10 77.1(3) . 2_656 ?
O3 V1 O2 107.9(5) . . ?
O3 V1 O1 109.3(5) . . ?
O2 V1 O1 110.2(4) . . ?
O3 V1 O4 108.9(5) . . ?
O2 V1 O4 106.7(4) . . ?
O1 V1 O4 113.7(5) . . ?
O6 V2 O5 109.5(4) . . ?
O6 V2 O7 110.3(4) . . ?
O5 V2 O7 109.0(4) . . ?
O6 V2 O1 108.6(4) . . ?
O5 V2 O1 110.0(5) . . ?
O7 V2 O1 109.3(4) . . ?
O10 V3 O9 111.5(5) . . ?
O10 V3 O7 110.1(5) . 1_545 ?
O9 V3 O7 109.4(4) . 1_545 ?
O10 V3 O8 109.4(4) . . ?
O9 V3 O8 106.6(4) . . ?
O7 V3 O8 109.9(4) 1_545 . ?
O12 V4 O13 108.4(5) . . ?
O12 V4 O8 106.4(5) . . ?
O13 V4 O8 111.7(4) . . ?
O12 V4 O11 107.1(5) . . ?
O13 V4 O11 111.4(5) . . ?
O8 V4 O11 111.6(4) . . ?
O15 V5 O14 109.4(5) . . ?
O15 V5 O4 107.6(5) . 2_666 ?
O14 V5 O4 112.0(5) . 2_666 ?
O15 V5 O11 111.2(5) . . ?
O14 V5 O11 107.9(4) . . ?
O4 V5 O11 108.8(4) 2_666 . ?
C2 N1 N2 108.8(10) . . ?
C2 N1 Cu1 130.6(9) . . ?
N2 N1 Cu1 120.5(8) . . ?
C1 N2 N1 106.1(10) . . ?
C1 N2 Cu2 130.3(8) . . ?
N1 N2 Cu2 120.8(7) . . ?
C2 N3 C1 107.2(10) . . ?
C2 N3 N4 124.6(11) . . ?
C1 N3 N4 127.5(10) . . ?
N3 N4 H4A 109.2 . . ?
N3 N4 H4B 109.2 . . ?
H4A N4 H4B 109.5 . . ?
C4 N5 N6 108.1(10) . . ?
C4 N5 Cu2 132.3(9) . . ?
N6 N5 Cu2 119.6(8) . . ?
C3 N6 N5 106.1(10) . . ?
C3 N6 Cu3 132.2(8) . . ?
N5 N6 Cu3 121.6(8) . . ?
C4 N7 C3 106.7(10) . . ?
C4 N7 N8 127.6(11) . . ?
C3 N7 N8 125.6(11) . . ?
N7 N8 H8A 120.0 . . ?
N7 N8 H8B 120.0 . . ?
H8A N8 H8B 120.0 . . ?
C6 N9 N10 105.3(9) . . ?
C6 N9 Cu3 130.7(9) . . ?
N10 N9 Cu3 122.5(7) . . ?
C5 N10 N9 108.5(10) . . ?
C5 N10 Cu1 131.6(9) . . ?
N9 N10 Cu1 119.8(7) . . ?
C5 N11 C6 106.7(10) . . ?
C5 N11 N12 126.0(11) . . ?
C6 N11 N12 127.3(10) . . ?
N11 N12 H12A 109.1 . . ?
N11 N12 H12C 109.2 . . ?
H12A N12 H12C 109.5 . . ?
V1 O1 V2 145.6(6) . . ?
V1 O2 Cu1 129.0(5) . . ?
V5 O4 V1 168.8(7) 2_666 . ?
V2 O6 Cu1 161.4(5) . 2_666 ?
V3 O7 V2 142.3(6) 1_565 . ?
V4 O8 V3 123.2(5) . . ?
V3 O9 Cu3 146.9(5) . . ?
V3 O10 Cu3 172.7(5) . 2_656 ?
V5 O11 V4 132.5(6) . . ?
V5 O14 Cu2 150.7(6) . 1_556 ?
Cu3 O16 Cu1 118.5(4) . . ?
Cu3 O16 Cu2 116.2(4) . . ?
Cu1 O16 Cu2 116.9(4) . . ?
Cu3 O16 H16 99.7 . . ?
Cu1 O16 H16 99.7 . . ?
Cu2 O16 H16 99.7 . . ?
Cu2 O17 H17B 108.3 . . ?
Cu2 O17 H17C 108.0 . . ?
H17B O17 H17C 107.4 . . ?
H18C O18 H18D 107.9 . . ?
N2 C1 N3 109.2(10) . . ?
N2 C1 H1 125.4 . . ?
N3 C1 H1 125.4 . . ?
N1 C2 N3 108.7(12) . . ?
N1 C2 H2 125.7 . . ?
N3 C2 H2 125.7 . . ?
N6 C3 N7 108.8(11) . . ?
N6 C3 H3 125.6 . . ?
N7 C3 H3 125.6 . . ?
N5 C4 N7 110.3(11) . . ?
N5 C4 H4 124.9 . . ?
N7 C4 H4 124.9 . . ?
N10 C5 N11 110.2(11) . . ?
N10 C5 H5 124.9 . . ?
N11 C5 H5 124.9 . . ?
N9 C6 N11 109.4(10) . . ?
N9 C6 H6 125.3 . . ?
N11 C6 H6 125.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N4 H4A O17 0.89 2.06 2.902(15) 156.6 2_665 yes
N4 H4B N12 0.89 2.36 3.014(15) 130.3 1_654 yes
N4 H4B O3 0.89 2.59 3.186(15) 125.1 2_665 yes
N4 H4B O15 0.89 2.58 3.075(16) 115.6 1_654 yes
N12 H12A O15 0.89 1.95 2.801(15) 160.4 . yes
N12 H12C O17 0.89 2.57 3.200(14) 128.7 2_566 yes
O16 H16 O10 0.85 2.18 2.746(11) 123.7 2_656 yes
O16 H16 O13 0.85 2.23 2.797(12) 124.1 2_656 yes
O17 H17B O5 0.85 1.90 2.737(13) 168.5 2_566 yes
O17 H17C O18 0.85 1.98 2.806(15) 162.6 1_455 yes
O18 H18C O12 0.85 1.91 2.725(14) 160.4 1_654 yes
O18 H18D O13 0.85 2.15 2.963(15) 161.3 2_656 yes
C1 H1 O3 0.93 2.39 3.126(14) 136.2 2_665 yes
C2 H2 N12 0.93 2.52 3.420(18) 162.9 2_666 yes
C4 H4 O12 0.93 2.46 3.067(14) 123.3 1_554 yes
C5 H5 O6 0.93 2.39 3.292(15) 164.0 . yes
C6 H6 O8 0.93 2.49 3.305(14) 146.2 . yes

_refine_diff_density_max         2.238
_refine_diff_density_min         -2.144
_refine_diff_density_rms         0.331

