# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

####################################################################### 
# 
# 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 1875916'
loop_
_audit_author_name
_audit_author_address
'Xianqiang Huang'
;Liaocheng University
China
;
_audit_update_record             
;
2019-03-11 deposited with the CCDC.	2019-03-12 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         ?
_chemical_formula_sum            'C40 H50 N16 O15 V6'
_chemical_formula_weight         1300.60

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.4908(13)
_cell_length_b                   12.5546(12)
_cell_length_c                   15.4384(14)
_cell_angle_alpha                90
_cell_angle_beta                 106.662(2)
_cell_angle_gamma                90
_cell_volume                     2690.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3157
_cell_measurement_theta_min      2.350
_cell_measurement_theta_max      23.340

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_F_000             1320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.077
_shelx_estimated_absorpt_T_min   0.790
_shelx_estimated_absorpt_T_max   0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7897
_exptl_absorpt_correction_T_max  0.8134
_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            13273
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.350
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_full        25.018
_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             4738
_reflns_number_gt                3008
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0603P)²+1.2268P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4738
_refine_ls_number_parameters     359
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0448
_refine_ls_wR_factor_ref         0.1266
_refine_ls_wR_factor_gt          0.1050
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.011
_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 0.93046(5) 0.94657(5) 0.12573(4) 0.0333(2) Uani 1 1 d . . . . .
V2 V 1.08530(5) 0.85251(5) 0.02340(5) 0.0402(2) Uani 1 1 d . . . . .
V3 V 0.74413(5) 0.73853(6) 0.11938(5) 0.0450(2) Uani 1 1 d . . . . .
N1 N 0.8534(3) 0.6235(3) 0.1308(2) 0.0464(9) Uani 1 1 d . . . . .
N2 N 0.9846(3) 0.5438(3) 0.1196(3) 0.0520(10) Uani 1 1 d . . . . .
N3 N 0.7171(2) 0.7394(3) -0.0230(3) 0.0506(10) Uani 1 1 d . . . . .
N4 N 0.7278(3) 0.7688(3) -0.1600(3) 0.0610(11) Uani 1 1 d . . . . .
N5 N 0.6470(3) 0.8672(3) 0.1097(3) 0.0532(10) Uani 1 1 d . . . . .
N6 N 0.5207(3) 0.9554(5) 0.1232(3) 0.0788(14) Uani 1 1 d D U . . .
N7 N 0.7809(3) 0.7590(3) 0.2607(3) 0.0484(9) Uani 1 1 d . . . . .
N8 N 0.8399(3) 0.8214(3) 0.3987(3) 0.0544(10) Uani 1 1 d . . . . .
O1 O 0.85021(18) 0.8481(2) 0.12085(17) 0.0396(7) Uani 1 1 d . . . . .
O2 O 0.9505(2) 1.0051(2) 0.22255(19) 0.0566(8) Uani 1 1 d . . . . .
O3 O 0.8820(2) 1.0350(2) 0.0347(2) 0.0555(8) Uani 1 1 d . . . . .
O4 O 1.04093(19) 0.8936(2) 0.11753(19) 0.0498(8) Uani 1 1 d . . . . .
O5 O 1.0020(3) 0.7841(3) -0.0456(2) 0.0768(11) Uani 1 1 d . . . . .
O6 O 1.1774(2) 0.7766(3) 0.0632(2) 0.0729(11) Uani 1 1 d . . . . .
O7 O 0.6630(2) 0.6502(3) 0.1165(2) 0.0671(9) Uani 1 1 d . . . . .
O8 O 1.0039(7) 0.2213(7) 0.2353(7) 0.131(4) Uani 0.5 1 d . . P . .
H8C H 0.988324 0.156961 0.240856 0.157 Uiso 0.5 1 d R U P . .
H8D H 1.004984 0.230521 0.181016 0.157 Uiso 0.5 1 d R U P . .
C1 C 0.9383(3) 0.6361(3) 0.1183(3) 0.0513(12) Uani 1 1 d . . . . .
H1 H 0.963634 0.701963 0.109608 0.062 Uiso 1 1 calc R U . . .
C2 C 0.8451(4) 0.5153(4) 0.1413(4) 0.0667(15) Uani 1 1 d . . . . .
H2 H 0.791879 0.481576 0.151112 0.080 Uiso 1 1 calc R U . . .
C3 C 0.9243(4) 0.4659(4) 0.1353(4) 0.0695(15) Uani 1 1 d . . . . .
H3 H 0.936630 0.393110 0.140629 0.083 Uiso 1 1 calc R U . . .
C4 C 1.0758(4) 0.5337(4) 0.1043(4) 0.0652(14) Uani 1 1 d . . . . .
H4 H 1.105194 0.595403 0.091941 0.078 Uiso 1 1 calc R U . . .
C5 C 1.1207(4) 0.4453(5) 0.1063(4) 0.0861(18) Uani 1 1 d . . . . .
H5A H 1.093380 0.382105 0.118468 0.103 Uiso 1 1 calc R U . . .
H5B H 1.180709 0.444449 0.095607 0.103 Uiso 1 1 calc R U . . .
C6 C 0.7636(3) 0.7893(4) -0.0722(3) 0.0544(12) Uani 1 1 d . . . . .
H6 H 0.815858 0.834067 -0.048353 0.065 Uiso 1 1 calc R U . . .
C7 C 0.6465(4) 0.6839(5) -0.0860(4) 0.0774(17) Uani 1 1 d . . . . .
H7 H 0.600232 0.640873 -0.072368 0.093 Uiso 1 1 calc R U . . .
C8 C 0.6539(4) 0.7006(5) -0.1694(4) 0.0765(17) Uani 1 1 d . . . . .
H8 H 0.615754 0.671016 -0.223010 0.092 Uiso 1 1 calc R U . . .
C9 C 0.7596(5) 0.8102(6) -0.2324(4) 0.0876(19) Uani 1 1 d . . . . .
H9 H 0.731226 0.783720 -0.290115 0.105 Uiso 1 1 calc R U . . .
C10 C 0.8247(6) 0.8814(8) -0.2231(5) 0.137(3) Uani 1 1 d . . . . .
H10A H 0.854524 0.909525 -0.166268 0.164 Uiso 1 1 calc R U . . .
H10B H 0.842207 0.905055 -0.273267 0.164 Uiso 1 1 calc R U . . .
C11 C 0.5623(4) 0.8606(5) 0.1253(4) 0.0747(16) Uani 1 1 d . . . . .
H11 H 0.534891 0.796941 0.136433 0.090 Uiso 1 1 calc R U . . .
C12 C 0.6585(4) 0.9737(4) 0.0975(4) 0.0674(15) Uani 1 1 d . . . . .
H12 H 0.711950 1.004169 0.085371 0.081 Uiso 1 1 calc R U . . .
C13 C 0.5816(4) 1.0279(5) 0.1055(4) 0.0884(19) Uani 1 1 d . . . . .
H13 H 0.572110 1.101172 0.099904 0.106 Uiso 1 1 calc R U . . .
C14 C 0.4315(6) 0.9960(8) 0.1366(8) 0.089(3) Uani 0.696(9) 1 d D U P A 1
H14 H 0.417979 1.068472 0.134710 0.106 Uiso 0.696(9) 1 calc R U P A 1
C15 C 0.3719(7) 0.9256(8) 0.1515(7) 0.101(3) Uani 0.696(9) 1 d D U P A 1
H15A H 0.387146 0.853528 0.153070 0.121 Uiso 0.696(9) 1 calc R U P A 1
H15B H 0.313983 0.947367 0.160488 0.121 Uiso 0.696(9) 1 calc R U P A 1
C14' C 0.4267(11) 0.9330(16) 0.137(2) 0.089(3) Uani 0.304(9) 1 d D . P A 2
H14' H 0.406322 0.863096 0.138793 0.106 Uiso 0.304(9) 1 calc R U P A 2
C15' C 0.3710(17) 1.0132(18) 0.1462(17) 0.101(3) Uani 0.304(9) 1 d D . P A 2
H15C H 0.391697 1.082994 0.144125 0.121 Uiso 0.304(9) 1 calc R U P A 2
H15D H 0.311192 0.999621 0.154851 0.121 Uiso 0.304(9) 1 calc R U P A 2
C16 C 0.8438(3) 0.8233(4) 0.3131(3) 0.0538(12) Uani 1 1 d . . . . .
H16 H 0.886420 0.865444 0.293111 0.065 Uiso 1 1 calc R U . . .
C17 C 0.7320(4) 0.7137(4) 0.3168(4) 0.0618(14) Uani 1 1 d . . . . .
H17 H 0.681985 0.664718 0.298695 0.074 Uiso 1 1 calc R U . . .
C18 C 0.7678(4) 0.7512(4) 0.4012(4) 0.0619(14) Uani 1 1 d . . . . .
H18 H 0.747853 0.733376 0.451412 0.074 Uiso 1 1 calc R U . . .
C19 C 0.8980(4) 0.8822(5) 0.4706(4) 0.0785(16) Uani 1 1 d . . . . .
H19 H 0.944756 0.925645 0.458344 0.094 Uiso 1 1 calc R U . . .
C20 C 0.8912(5) 0.8821(5) 0.5517(4) 0.0928(19) Uani 1 1 d . . . . .
H20A H 0.845261 0.839624 0.566468 0.111 Uiso 1 1 calc R U . . .
H20B H 0.932093 0.924419 0.595736 0.111 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 1.615(3) . ?
V1 O1 1.684(2) . ?
V1 O3 1.771(3) . ?
V1 O4 1.771(3) . ?
V2 O5 1.610(3) . ?
V2 O6 1.611(3) . ?
V2 O3 1.808(3) 3_775 ?
V2 O4 1.824(3) . ?
V3 O7 1.607(3) . ?
V3 O1 2.058(2) . ?
V3 N7 2.109(4) . ?
V3 N1 2.112(4) . ?
V3 N3 2.119(4) . ?
V3 N5 2.120(4) . ?
N1 C1 1.308(5) . ?
N1 C2 1.378(5) . ?
N2 C1 1.337(5) . ?
N2 C3 1.378(6) . ?
N2 C4 1.413(6) . ?
N3 C6 1.310(6) . ?
N3 C7 1.382(6) . ?
N4 C6 1.331(6) . ?
N4 C8 1.346(6) . ?
N4 C9 1.423(7) . ?
N5 C11 1.319(6) . ?
N5 C12 1.366(6) . ?
N6 C11 1.331(7) . ?
N6 C13 1.350(7) . ?
N6 C14 1.458(7) . ?
N6 C14' 1.463(10) . ?
N7 C16 1.309(6) . ?
N7 C17 1.389(5) . ?
N8 C16 1.339(5) . ?
N8 C18 1.375(6) . ?
N8 C19 1.410(6) . ?
C2 C3 1.331(7) . ?
C4 C5 1.283(7) . ?
C7 C8 1.340(8) . ?
C9 C10 1.276(9) . ?
C12 C13 1.341(7) . ?
C14 C15 1.302(8) . ?
C14' C15' 1.324(10) . ?
C17 C18 1.341(7) . ?
C19 C20 1.285(7) . ?

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 108.27(14) . . ?
O2 V1 O3 112.02(16) . . ?
O1 V1 O3 108.24(13) . . ?
O2 V1 O4 108.11(15) . . ?
O1 V1 O4 110.33(13) . . ?
O3 V1 O4 109.86(14) . . ?
O5 V2 O6 108.6(2) . . ?
O5 V2 O3 109.99(16) . 3_775 ?
O6 V2 O3 110.19(16) . 3_775 ?
O5 V2 O4 108.02(16) . . ?
O6 V2 O4 107.82(15) . . ?
O3 V2 O4 112.13(14) 3_775 . ?
O7 V3 O1 178.09(15) . . ?
O7 V3 N7 94.49(16) . . ?
O1 V3 N7 86.60(12) . . ?
O7 V3 N1 93.19(15) . . ?
O1 V3 N1 85.20(12) . . ?
N7 V3 N1 92.07(14) . . ?
O7 V3 N3 93.39(16) . . ?
O1 V3 N3 85.60(12) . . ?
N7 V3 N3 171.70(14) . . ?
N1 V3 N3 90.09(14) . . ?
O7 V3 N5 93.33(16) . . ?
O1 V3 N5 88.29(13) . . ?
N7 V3 N5 86.89(14) . . ?
N1 V3 N5 173.46(14) . . ?
N3 V3 N5 90.05(14) . . ?
C1 N1 C2 104.7(4) . . ?
C1 N1 V3 128.2(3) . . ?
C2 N1 V3 126.6(3) . . ?
C1 N2 C3 106.1(4) . . ?
C1 N2 C4 124.4(4) . . ?
C3 N2 C4 129.5(4) . . ?
C6 N3 C7 103.5(4) . . ?
C6 N3 V3 129.1(3) . . ?
C7 N3 V3 127.4(4) . . ?
C6 N4 C8 107.4(5) . . ?
C6 N4 C9 127.5(5) . . ?
C8 N4 C9 125.1(5) . . ?
C11 N5 C12 104.1(4) . . ?
C11 N5 V3 124.9(4) . . ?
C12 N5 V3 130.6(3) . . ?
C11 N6 C13 106.9(5) . . ?
C11 N6 C14 136.3(7) . . ?
C13 N6 C14 116.8(6) . . ?
C11 N6 C14' 105.0(9) . . ?
C13 N6 C14' 148.0(9) . . ?
C16 N7 C17 104.9(4) . . ?
C16 N7 V3 129.7(3) . . ?
C17 N7 V3 124.9(3) . . ?
C16 N8 C18 106.6(4) . . ?
C16 N8 C19 125.6(4) . . ?
C18 N8 C19 127.7(4) . . ?
V1 O1 V3 174.33(16) . . ?
V1 O3 V2 141.52(18) . 3_775 ?
V1 O4 V2 134.05(17) . . ?
N1 C1 N2 112.5(4) . . ?
C3 C2 N1 110.2(4) . . ?
C2 C3 N2 106.5(4) . . ?
C5 C4 N2 124.5(5) . . ?
N3 C6 N4 112.5(4) . . ?
C8 C7 N3 110.5(5) . . ?
C7 C8 N4 106.1(5) . . ?
C10 C9 N4 124.3(6) . . ?
N5 C11 N6 112.2(5) . . ?
C13 C12 N5 110.3(5) . . ?
C12 C13 N6 106.5(5) . . ?
C15 C14 N6 116.6(9) . . ?
C15' C14' N6 119.5(18) . . ?
N7 C16 N8 112.3(4) . . ?
C18 C17 N7 109.6(5) . . ?
C17 C18 N8 106.5(4) . . ?
C20 C19 N8 124.8(6) . . ?

_refine_diff_density_max         0.502
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.079

####################################################################### 
# 
# 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_180602b
_database_code_depnum_ccdc_archive 'CCDC 1875917'
loop_
_audit_author_name
_audit_author_address
'Xianqiang Huang'
;Liaocheng University
China
;
_audit_update_record             
;
2019-03-11 deposited with the CCDC.	2019-03-12 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         ?
_chemical_formula_sum            'C16 H57 N8 Ni3 O45.50 V10'
_chemical_formula_weight         1775.22

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'
Ni Ni 0.3393 1.1124 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   19.5903(17)
_cell_length_b                   9.3317(8)
_cell_length_c                   15.8463(12)
_cell_angle_alpha                90
_cell_angle_beta                 110.430(2)
_cell_angle_gamma                90
_cell_volume                     2714.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1670
_cell_measurement_theta_min      2.448
_cell_measurement_theta_max      25.569

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_F_000             1774
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    2.768
_shelx_estimated_absorpt_T_min   0.581
_shelx_estimated_absorpt_T_max   0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5815
_exptl_absorpt_correction_T_max  0.6361
_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            6800
_diffrn_reflns_av_unetI/netI     0.0790
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.219
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_full        25.019
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             2546
_reflns_number_gt                1801
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1377P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2546
_refine_ls_number_parameters     264
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0713
_refine_ls_wR_factor_ref         0.2063
_refine_ls_wR_factor_gt          0.1905
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_restrained_S_all      0.993
_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
Ni1 Ni 0.000000 0.500000 0.500000 0.0325(5) Uani 1 4 d S T P . .
Ni2 Ni 0.33360(6) 1.000000 1.10483(8) 0.0256(4) Uani 1 2 d S T P . .
V1 V -0.05876(6) 0.83612(15) 0.79106(8) 0.0379(4) Uani 1 1 d . . . . .
V2 V 0.08469(8) 1.000000 0.89560(10) 0.0238(4) Uani 1 2 d S T P . .
V3 V 0.000000 0.82493(15) 1.000000 0.0218(4) Uani 1 2 d S T P . .
V4 V 0.14380(8) 1.000000 1.10486(10) 0.0218(4) Uani 1 2 d S T P . .
O1 O 0.1445(2) 1.1432(5) 1.1812(3) 0.0315(11) Uani 1 1 d . . . . .
O2 O 0.2274(3) 1.000000 1.1040(4) 0.0254(14) Uani 1 2 d S T P . .
O3 O 0.3609(3) 1.1579(5) 1.2030(3) 0.0378(13) Uani 1 1 d . . . . .
H3A H 0.381539 1.214629 1.177671 0.045 Uiso 1 1 d R U . . .
H3B H 0.392969 1.123659 1.249910 0.045 Uiso 1 1 d R U . . .
O4 O 0.4408(4) 1.000000 1.1136(5) 0.0407(18) Uani 1 2 d S T P . .
H4A H 0.464131 1.073760 1.107481 0.049 Uiso 0.5 1 d R U P . .
O5 O 0.3084(2) 1.1573(5) 1.0046(3) 0.0280(11) Uani 1 1 d . . . . .
H5A H 0.298429 1.100775 0.959868 0.034 Uiso 0.5 1 d R U P . .
H5B H 0.270729 1.204765 1.002198 0.034 Uiso 0.5 1 d R U P . .
H5C H 0.341259 1.216226 1.003738 0.034 Uiso 1 1 d R U . . .
O6 O -0.0798(3) 0.7062(8) 0.7199(4) 0.065(2) Uani 1 1 d . . . . .
O7 O -0.0780(4) 1.000000 0.7241(4) 0.043(2) Uani 1 2 d S T P . .
O8 O 0.0421(2) 0.8540(5) 0.8187(3) 0.0339(12) Uani 1 1 d . . . . .
O9 O 0.1665(3) 1.000000 0.8965(4) 0.0307(16) Uani 1 2 d S T P . .
O10 O 0.0257(2) 0.7161(5) 1.0916(3) 0.0347(12) Uani 1 1 d . . . . .
O11 O 0.0962(2) 0.8678(5) 0.9994(3) 0.0228(10) Uani 1 1 d . . . . .
O12 O -0.0259(3) 1.000000 0.9108(4) 0.0225(14) Uani 1 2 d S T P . .
O13 O 0.0108(4) 0.500000 0.6411(5) 0.0413(18) Uani 1 2 d S T P . .
H13 H -0.007405 0.426410 0.656799 0.050 Uiso 1 1 d R U . . .
O14A O 0.2584(8) 0.156(2) 0.8106(13) 0.055(4) Uani 0.6 1 d . . P A 1
H14C H 0.215651 0.177890 0.808365 0.082 Uiso 0.6 1 d R U P A 1
H14D H 0.263861 0.201760 0.766913 0.082 Uiso 0.6 1 d R U P A 1
O14B O 0.2356(14) 0.174(4) 0.780(2) 0.055(4) Uani 0.4 1 d . . P B 2
H14A H 0.262892 0.103738 0.778738 0.082 Uiso 0.4 1 d R U P B 2
H14B H 0.228902 0.226218 0.733729 0.082 Uiso 0.4 1 d R U P B 2
O15 O 0.356(3) 1.000000 0.871(3) 0.087(13) Uani 0.25 2 d S T P . .
H15 H 0.382753 0.926320 0.879654 0.105 Uiso 0.25 1 d R U P . .
O16 O 0.2087(17) 0.500000 0.3319(19) 0.136(10) Uani 0.5 2 d S T P . .
H16 H 0.181407 0.426380 0.320922 0.163 Uiso 0.5 1 d R U P . .
N5 N -0.0768(7) 0.0788(15) 0.4174(9) 0.047(3) Uani 0.5 1 d . . P C .
N6 N 0.2071(8) 0.3216(16) 0.5440(11) 0.060(4) Uani 0.5 1 d . . P C -1
N3 N -0.0336(6) 0.2870(12) 0.4815(8) 0.035(3) Uani 0.5 1 d . . P . .
N4 N 0.1093(6) 0.4387(13) 0.5388(8) 0.042(3) Uani 0.5 1 d . . P C -1
C1 C 0.2486(18) 0.221(3) 0.5180(19) 0.096(9) Uiso 0.5 1 d . . P C -1
H1A H 0.299298 0.244623 0.544484 0.144 Uiso 0.5 1 calc R U P C -1
H1B H 0.234591 0.220862 0.453538 0.144 Uiso 0.5 1 calc R U P C -1
H1C H 0.240417 0.127231 0.537914 0.144 Uiso 0.5 1 calc R U P C -1
C2 C 0.2263(9) 0.413(2) 0.6122(13) 0.063(5) Uani 0.5 1 d . . P C -1
H2 H 0.274058 0.419301 0.657155 0.075 Uiso 0.5 1 d R U P C -1
C3 C 0.1672(7) 0.481(7) 0.6103(9) 0.036(10) Uani 0.5 1 d . . P C -1
H3 H 0.166000 0.559846 0.648547 0.043 Uiso 0.5 1 d R U P C -1
C4 C 0.1339(8) 0.3414(19) 0.4987(12) 0.050(5) Uani 0.5 1 d . . P C -1
H4 H 0.104909 0.289075 0.446215 0.060 Uiso 0.5 1 d R U P C -1
C5 C -0.0598(10) 0.2096(19) 0.5376(11) 0.052(5) Uani 0.5 1 d . . P . .
H5 H -0.060557 0.243331 0.594504 0.062 Uiso 0.5 1 d R U P C .
C6 C -0.0873(11) 0.085(2) 0.4993(13) 0.066(6) Uani 0.5 1 d . . P C .
H6 H -0.109881 0.000002 0.524000 0.079 Uiso 1 2 d R U P . .
C7 C -0.0455(10) 0.2032(19) 0.4115(11) 0.051(4) Uani 0.5 1 d . . P . .
H7 H -0.032905 0.229152 0.360115 0.062 Uiso 0.5 1 d R U P C .
C8 C -0.1004(11) -0.035(2) 0.3504(13) 0.070(9) Uani 0.5 1 d . . P . .
H8A H -0.085292 -0.012173 0.300458 0.104 Uiso 0.5 1 d R U P C .
H8B H -0.078532 -0.123983 0.376808 0.104 Uiso 0.5 1 d R U P . .
H8C H -0.152462 -0.043903 0.329648 0.104 Uiso 0.5 1 d R U 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
Ni1 N3 2.082(12) 5_566 ?
Ni1 N3 2.082(12) 6_565 ?
Ni1 N3 2.082(11) 2_556 ?
Ni1 N3 2.082(12) . ?
Ni1 N4 2.090(12) . ?
Ni1 O13 2.171(7) 5_566 ?
Ni1 O13 2.171(7) . ?
Ni2 O4 2.056(7) . ?
Ni2 O3 2.073(5) 6_575 ?
Ni2 O3 2.073(5) . ?
Ni2 O2 2.077(6) . ?
Ni2 O5 2.092(4) 6_575 ?
Ni2 O5 2.092(4) . ?
V1 O6 1.608(5) . ?
V1 O7 1.824(4) . ?
V1 O8 1.876(5) . ?
V1 O1 1.888(5) 5_577 ?
V1 O10 2.072(5) 2_557 ?
V1 O12 2.345(5) . ?
V1 V1 3.059(3) 6_575 ?
V1 V3 3.1044(12) . ?
V1 V2 3.1193(17) . ?
V2 O9 1.599(6) . ?
V2 O8 1.824(5) 6_575 ?
V2 O8 1.824(5) . ?
V2 O11 2.005(4) 6_575 ?
V2 O11 2.005(4) . ?
V2 O12 2.261(6) . ?
V2 V4 3.107(2) . ?
V3 O10 1.697(5) 2_557 ?
V3 O10 1.697(5) . ?
V3 O11 1.931(4) 2_557 ?
V3 O11 1.931(4) . ?
V3 O12 2.103(4) . ?
V3 O12 2.103(4) 5_577 ?
V4 O2 1.642(6) . ?
V4 O1 1.799(5) . ?
V4 O1 1.799(5) 6_575 ?
V4 O11 2.024(4) . ?
V4 O11 2.024(4) 6_575 ?
V4 O12 2.236(6) 5_577 ?
O3 H3A 0.8470 . ?
O3 H3B 0.8501 . ?
O4 H4A 0.8499 . ?
O4 H4A 0.8500 6_575 ?
O5 H5A 0.8495 . ?
O5 H5B 0.8505 . ?
O5 H5C 0.8500 . ?
O13 H13 0.8499 . ?
O13 H13 0.8500 6_565 ?
O14A H14C 0.8499 . ?
O14A H14D 0.8501 . ?
O14B H14A 0.8502 . ?
O14B H14B 0.8499 . ?
O15 H15 0.8500 . ?
O15 H15 0.8500 6_575 ?
O16 H16 0.8500 . ?
O16 H16 0.8500 6_565 ?
N5 C8 1.08(2) 6 ?
N5 C7 1.33(2) . ?
N5 C6 1.39(2) . ?
N5 C8 1.46(2) . ?
N5 N5 1.47(3) 6 ?
N5 H8B 0.76(2) 6 ?
N6 C2 1.32(2) . ?
N6 C4 1.37(2) . ?
N6 C1 1.40(3) . ?
N3 N3 1.24(2) 2_556 ?
N3 C7 1.31(2) . ?
N3 C5 1.376(19) . ?
N4 C4 1.295(19) . ?
N4 C3 1.35(3) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.31(4) . ?
C2 H2 0.9599 . ?
C3 H3 0.9599 . ?
C4 H4 0.9599 . ?
C5 C6 1.34(2) . ?
C5 C7 1.93(2) 2_556 ?
C5 H5 0.9601 . ?
C6 C6 1.58(4) 6 ?
C6 H6 1.0470 . ?
C7 C8 1.96(3) 6 ?
C7 H7 0.9598 . ?
C7 H8B 1.01(3) 6 ?
C8 C8 0.65(4) 6 ?
C8 H8A 0.9604 . ?
C8 H8B 0.9602 . ?
C8 H8C 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
N3 Ni1 N3 34.6(6) 5_566 6_565 ?
N3 Ni1 N3 145.4(6) 5_566 2_556 ?
N3 Ni1 N3 180.0 6_565 2_556 ?
N3 Ni1 N3 180.0 5_566 . ?
N3 Ni1 N3 145.4(6) 6_565 . ?
N3 Ni1 N3 34.6(6) 2_556 . ?
N3 Ni1 N4 88.8(5) 5_566 . ?
N3 Ni1 N4 122.9(5) 6_565 . ?
N3 Ni1 N4 57.1(5) 2_556 . ?
N3 Ni1 N4 91.2(5) . . ?
N3 Ni1 O13 93.3(3) 5_566 5_566 ?
N3 Ni1 O13 86.7(3) 6_565 5_566 ?
N3 Ni1 O13 93.3(3) 2_556 5_566 ?
N3 Ni1 O13 86.7(3) . 5_566 ?
N4 Ni1 O13 91.4(4) . 5_566 ?
N3 Ni1 O13 86.7(3) 5_566 . ?
N3 Ni1 O13 93.3(3) 6_565 . ?
N3 Ni1 O13 86.7(3) 2_556 . ?
N3 Ni1 O13 93.3(3) . . ?
N4 Ni1 O13 88.6(4) . . ?
O13 Ni1 O13 180.0 5_566 . ?
O4 Ni2 O3 87.7(2) . 6_575 ?
O4 Ni2 O3 87.7(2) . . ?
O3 Ni2 O3 90.6(3) 6_575 . ?
O4 Ni2 O2 176.7(3) . . ?
O3 Ni2 O2 90.04(19) 6_575 . ?
O3 Ni2 O2 90.04(19) . . ?
O4 Ni2 O5 90.9(2) . 6_575 ?
O3 Ni2 O5 90.10(19) 6_575 6_575 ?
O3 Ni2 O5 178.4(2) . 6_575 ?
O2 Ni2 O5 91.43(18) . 6_575 ?
O4 Ni2 O5 90.9(2) . . ?
O3 Ni2 O5 178.4(2) 6_575 . ?
O3 Ni2 O5 90.10(19) . . ?
O2 Ni2 O5 91.43(18) . . ?
O5 Ni2 O5 89.1(2) 6_575 . ?
O6 V1 O7 105.9(3) . . ?
O6 V1 O8 102.8(2) . . ?
O7 V1 O8 92.8(3) . . ?
O6 V1 O1 102.1(3) . 5_577 ?
O7 V1 O1 91.7(3) . 5_577 ?
O8 V1 O1 152.4(2) . 5_577 ?
O6 V1 O10 98.4(3) . 2_557 ?
O7 V1 O10 155.8(2) . 2_557 ?
O8 V1 O10 82.2(2) . 2_557 ?
O1 V1 O10 82.59(19) 5_577 2_557 ?
O6 V1 O12 171.7(3) . . ?
O7 V1 O12 82.34(19) . . ?
O8 V1 O12 77.5(2) . . ?
O1 V1 O12 76.13(19) 5_577 . ?
O10 V1 O12 73.42(16) 2_557 . ?
O6 V1 V1 138.9(3) . 6_575 ?
O7 V1 V1 33.04(17) . 6_575 ?
O8 V1 V1 84.90(16) . 6_575 ?
O1 V1 V1 84.12(15) 5_577 6_575 ?
O10 V1 V1 122.72(13) 2_557 6_575 ?
O12 V1 V1 49.30(10) . 6_575 ?
O6 V1 V3 129.2(3) . . ?
O7 V1 V3 124.96(17) . . ?
O8 V1 V3 77.63(14) . . ?
O1 V1 V3 77.52(14) 5_577 . ?
O10 V1 V3 30.80(13) 2_557 . ?
O12 V1 V3 42.63(10) . . ?
V1 V1 V3 91.93(3) 6_575 . ?
O6 V1 V2 134.8(2) . . ?
O7 V1 V2 82.13(19) . . ?
O8 V1 V2 32.03(14) . . ?
O1 V1 V2 122.39(14) 5_577 . ?
O10 V1 V2 81.20(13) 2_557 . ?
O12 V1 V2 46.26(14) . . ?
V1 V1 V2 60.64(3) 6_575 . ?
V3 V1 V2 61.33(4) . . ?
O9 V2 O8 103.3(2) . 6_575 ?
O9 V2 O8 103.3(2) . . ?
O8 V2 O8 96.6(3) 6_575 . ?
O9 V2 O11 99.6(2) . 6_575 ?
O8 V2 O11 89.0(2) 6_575 6_575 ?
O8 V2 O11 154.4(2) . 6_575 ?
O9 V2 O11 99.6(2) . . ?
O8 V2 O11 154.4(2) 6_575 . ?
O8 V2 O11 89.0(2) . . ?
O11 V2 O11 76.0(2) 6_575 . ?
O9 V2 O12 173.8(3) . . ?
O8 V2 O12 80.75(17) 6_575 . ?
O8 V2 O12 80.75(17) . . ?
O11 V2 O12 75.56(17) 6_575 . ?
O11 V2 O12 75.56(17) . . ?
O9 V2 V4 89.5(2) . . ?
O8 V2 V4 128.75(16) 6_575 . ?
O8 V2 V4 128.75(16) . . ?
O11 V2 V4 39.75(12) 6_575 . ?
O11 V2 V4 39.75(12) . . ?
O12 V2 V4 84.28(15) . . ?
O9 V2 V1 136.02(17) . 6_575 ?
O8 V2 V1 33.04(14) 6_575 6_575 ?
O8 V2 V1 83.92(16) . 6_575 ?
O11 V2 V1 87.52(12) 6_575 6_575 ?
O11 V2 V1 124.07(13) . 6_575 ?
O12 V2 V1 48.53(11) . 6_575 ?
V4 V2 V1 119.86(5) . 6_575 ?
O9 V2 V1 136.02(18) . . ?
O8 V2 V1 83.92(16) 6_575 . ?
O8 V2 V1 33.04(14) . . ?
O11 V2 V1 124.07(13) 6_575 . ?
O11 V2 V1 87.53(12) . . ?
O12 V2 V1 48.53(11) . . ?
V4 V2 V1 119.86(5) . . ?
V1 V2 V1 58.72(6) 6_575 . ?
O10 V3 O10 106.5(4) 2_557 . ?
O10 V3 O11 97.43(19) 2_557 2_557 ?
O10 V3 O11 96.82(19) . 2_557 ?
O10 V3 O11 96.82(19) 2_557 . ?
O10 V3 O11 97.43(19) . . ?
O11 V3 O11 156.1(3) 2_557 . ?
O10 V3 O12 87.7(2) 2_557 . ?
O10 V3 O12 165.8(2) . . ?
O11 V3 O12 80.5(2) 2_557 . ?
O11 V3 O12 80.9(2) . . ?
O10 V3 O12 165.8(2) 2_557 5_577 ?
O10 V3 O12 87.7(2) . 5_577 ?
O11 V3 O12 80.9(2) 2_557 5_577 ?
O11 V3 O12 80.5(2) . 5_577 ?
O12 V3 O12 78.1(2) . 5_577 ?
O10 V3 V1 145.17(19) 2_557 2_557 ?
O10 V3 V1 38.69(18) . 2_557 ?
O11 V3 V1 89.25(12) 2_557 2_557 ?
O11 V3 V1 89.95(12) . 2_557 ?
O12 V3 V1 127.10(13) . 2_557 ?
O12 V3 V1 49.04(12) 5_577 2_557 ?
O10 V3 V1 38.69(18) 2_557 . ?
O10 V3 V1 145.17(19) . . ?
O11 V3 V1 89.95(12) 2_557 . ?
O11 V3 V1 89.25(12) . . ?
O12 V3 V1 49.04(12) . . ?
O12 V3 V1 127.11(13) 5_577 . ?
V1 V3 V1 176.15(7) 2_557 . ?
O2 V4 O1 103.4(2) . . ?
O2 V4 O1 103.4(2) . 6_575 ?
O1 V4 O1 95.9(3) . 6_575 ?
O2 V4 O11 99.6(2) . . ?
O1 V4 O11 154.3(2) . . ?
O1 V4 O11 89.8(2) 6_575 . ?
O2 V4 O11 99.6(2) . 6_575 ?
O1 V4 O11 89.76(19) . 6_575 ?
O1 V4 O11 154.3(2) 6_575 6_575 ?
O11 V4 O11 75.1(2) . 6_575 ?
O2 V4 O12 173.6(3) . 5_577 ?
O1 V4 O12 80.76(17) . 5_577 ?
O1 V4 O12 80.75(17) 6_575 5_577 ?
O11 V4 O12 75.42(17) . 5_577 ?
O11 V4 O12 75.42(17) 6_575 5_577 ?
O2 V4 V2 89.6(2) . . ?
O1 V4 V2 129.05(15) . . ?
O1 V4 V2 129.05(15) 6_575 . ?
O11 V4 V2 39.30(13) . . ?
O11 V4 V2 39.30(13) 6_575 . ?
O12 V4 V2 84.02(15) 5_577 . ?
V4 O1 V1 115.7(2) . 5_577 ?
V4 O2 Ni2 179.2(4) . . ?
Ni2 O3 H3A 97.4 . . ?
Ni2 O3 H3B 107.9 . . ?
H3A O3 H3B 108.7 . . ?
Ni2 O4 H4A 124.7 . . ?
Ni2 O4 H4A 124.69(4) . 6_575 ?
H4A O4 H4A 108.2 . 6_575 ?
Ni2 O5 H5A 97.0 . . ?
Ni2 O5 H5B 111.7 . . ?
H5A O5 H5B 110.0 . . ?
Ni2 O5 H5C 119.1 . . ?
H5A O5 H5C 110.1 . . ?
H5B O5 H5C 108.2 . . ?
V1 O7 V1 113.9(3) . 6_575 ?
V2 O8 V1 114.9(2) . . ?
V3 O10 V1 110.5(3) . 2_557 ?
V3 O11 V2 107.51(19) . . ?
V3 O11 V4 106.9(2) . . ?
V2 O11 V4 100.95(19) . . ?
V3 O12 V3 101.9(2) 5_577 . ?
V3 O12 V4 94.12(19) 5_577 5_577 ?
V3 O12 V4 94.12(19) . 5_577 ?
V3 O12 V2 93.24(17) 5_577 . ?
V3 O12 V2 93.24(17) . . ?
V4 O12 V2 168.3(3) 5_577 . ?
V3 O12 V1 88.33(5) 5_577 6_575 ?
V3 O12 V1 169.7(2) . 6_575 ?
V4 O12 V1 85.92(17) 5_577 6_575 ?
V2 O12 V1 85.22(18) . 6_575 ?
V3 O12 V1 169.7(2) 5_577 . ?
V3 O12 V1 88.33(5) . . ?
V4 O12 V1 85.92(17) 5_577 . ?
V2 O12 V1 85.22(18) . . ?
V1 O12 V1 81.4(2) 6_575 . ?
Ni1 O13 H13 113.7 . . ?
Ni1 O13 H13 113.66(9) . 6_565 ?
H13 O13 H13 107.8 . 6_565 ?
H14C O14A H14D 104.5 . . ?
H14A O14B H14B 109.5 . . ?
H15 O15 H15 108.0 . 6_575 ?
H16 O16 H16 107.8 . 6_565 ?
C8 N5 C7 108.1(17) 6 . ?
C8 N5 C6 141.7(19) 6 . ?
C7 N5 C6 104.7(14) . . ?
C8 N5 C8 24.5(18) 6 . ?
C7 N5 C8 128.4(15) . . ?
C6 N5 C8 126.8(15) . . ?
C8 N5 N5 67.8(14) 6 6 ?
C7 N5 N5 150.7(10) . 6 ?
C6 N5 N5 92.3(10) . 6 ?
C8 N5 N5 43.2(9) . 6 ?
C8 N5 H8B 60.0(13) 6 6 ?
C7 N5 H8B 48.9(18) . 6 ?
C6 N5 H8B 142(2) . 6 ?
C8 N5 H8B 83(2) . 6 ?
N5 N5 H8B 123.7(19) 6 6 ?
C2 N6 C4 106.8(15) . . ?
C2 N6 C1 130(2) . . ?
C4 N6 C1 123(2) . . ?
N3 N3 C7 104.3(13) 2_556 . ?
N3 N3 C5 105.5(14) 2_556 . ?
C7 N3 C5 103.8(13) . . ?
N3 N3 Ni1 72.7(3) 2_556 . ?
C7 N3 Ni1 130.0(11) . . ?
C5 N3 Ni1 125.5(10) . . ?
C4 N4 C3 106(2) . . ?
C4 N4 Ni1 124.5(10) . . ?
C3 N4 Ni1 129.9(18) . . ?
N6 C1 H1A 109.5 . . ?
N6 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N6 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 N6 107(2) . . ?
C3 C2 H2 127.6 . . ?
N6 C2 H2 125.0 . . ?
C2 C3 N4 111(3) . . ?
C2 C3 H3 125.1 . . ?
N4 C3 H3 123.6 . . ?
N4 C4 N6 109.7(15) . . ?
N4 C4 H4 125.0 . . ?
N6 C4 H4 125.3 . . ?
C6 C5 N3 110.2(14) . . ?
C6 C5 C7 111.4(15) . 2_556 ?
N3 C5 C7 72.7(10) . 2_556 ?
C6 C5 H5 125.1 . . ?
N3 C5 H5 124.5 . . ?
C7 C5 H5 89.0 2_556 . ?
C5 C6 N5 107.0(14) . . ?
C5 C6 C6 150.6(12) . 6 ?
N5 C6 C6 87.7(10) . 6 ?
C5 C6 H6 130.2 . . ?
N5 C6 H6 122.7 . . ?
C6 C6 H6 40.9 6 . ?
N3 C7 N5 114.3(15) . . ?
N3 C7 C5 77.3(11) . 2_556 ?
N5 C7 C5 116.6(13) . 2_556 ?
N3 C7 C8 143.3(15) . 6 ?
N5 C7 C8 31.6(8) . 6 ?
C5 C7 C8 123.6(12) 2_556 6 ?
N3 C7 H7 123.0 . . ?
N5 C7 H7 122.7 . . ?
C5 C7 H7 78.1 2_556 . ?
C8 C7 H7 92.4 6 . ?
N3 C7 H8B 142(2) . 6 ?
N5 C7 H8B 34.5(13) . 6 ?
C5 C7 H8B 130(2) 2_556 6 ?
C8 C7 H8B 6.4(8) 6 6 ?
H7 C7 H8B 91.7 . 6 ?
C8 C8 N5 112.2(14) 6 6 ?
C8 C8 N5 43.2(9) 6 . ?
N5 C8 N5 69.0(16) 6 . ?
C8 C8 C7 143.3(8) 6 6 ?
N5 C8 C7 40.3(12) 6 6 ?
N5 C8 C7 104.1(12) . 6 ?
C8 C8 H8A 77.1 6 . ?
N5 C8 H8A 138.2 6 . ?
N5 C8 H8A 109.1 . . ?
C7 C8 H8A 108.2 6 . ?
C8 C8 H8B 149.8 6 . ?
N5 C8 H8B 43.2 6 . ?
N5 C8 H8B 109.4 . . ?
C7 C8 H8B 6.7 6 . ?
H8A C8 H8B 109.4 . . ?
C8 C8 H8C 94.9 6 . ?
N5 C8 H8C 110.1 6 . ?
N5 C8 H8C 109.9 . . ?
C7 C8 H8C 115.8 6 . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C8 C8 H8B 18.0(5) 6 6 ?
N5 C8 H8B 96.5(11) 6 6 ?
N5 C8 H8B 28.9(8) . 6 ?
C7 C8 H8B 125.3(7) 6 6 ?
H8A C8 H8B 82.8 . 6 ?
H8B C8 H8B 131.8 . 6 ?
H8C C8 H8B 109.4 . 6 ?

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
O3 H3A O8 0.85 1.97 2.744(7) 151.9 4_557 yes
O3 H3B O13 0.85 2.37 3.202(8) 168.2 7_567 yes
O4 H4A O10 0.85 1.87 2.713(6) 171.2 3 yes
O5 H5A O5 0.85 2.50 2.936(9) 112.9 6_575 yes
O5 H5A O9 0.85 2.60 3.081(7) 117.1 . yes
O5 H5A O14A^a 0.85 2.28 2.88(2) 128.4 1_565 yes
O5 H5A O15 0.85 2.29 2.98(3) 138.5 . yes
O5 H5B O5 0.85 1.99 2.832(9) 171.0 7_577 yes
O5 H5C O11 0.85 1.88 2.727(6) 171.6 4_557 yes
O13 H13 O6 0.85 2.35 3.155(8) 157.9 6_565 yes
O14A^a H14C^a O3 0.85 2.11 2.858(18) 146.9 7_567 yes
O14A^a H14C^a O9 0.85 2.56 2.99(3) 112.0 1_545 yes
O14B^b H14A^b O14B^b 0.85 2.65 3.25(8) 128.7 6 yes
O14B^b H14A^b O15 0.85 2.13 2.81(5) 136.8 1_545 yes
O14B^b H14A^b O16 0.85 2.24 2.88(5) 132.9 7_556 yes
O15 H15 O10 0.85 2.15 2.98(3) 164.2 7_567 yes
O16 H16 O6 0.85 2.24 3.05(2) 159.6 5_566 yes
C1^a H1C^a O16 0.96 2.29 3.04(3) 134.3 7_556 yes
C2^a H2^a O1 0.96 2.57 3.408(17) 146.2 7_567 yes
C4^a H4^a O6 0.96 2.50 3.279(18) 137.8 5_566 yes
C5 H5 O6 0.96 2.20 3.147(16) 169.4 6_565 yes
C7 H7 O13 0.96 2.57 3.037(18) 110.4 5_566 yes
C8 H8A O8 0.96 2.64 3.42(2) 138.8 2_546 yes
C8 H8B N3 0.96 2.20 3.11(2) 158.2 6 yes
C8 H8C O14B^b 0.96 2.27 3.02(4) 134.4 5_556 yes

_refine_diff_density_max         1.813
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.230

