# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_181109a
_database_code_depnum_ccdc_archive 'CCDC 1999276'
loop_
_audit_author_name
_audit_author_address
'Mingyu Dou'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2020-04-26 deposited with the CCDC.	2020-05-21 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            'C56 H98 N16 Ni2 O13 V4'
_chemical_formula_weight         1524.68

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      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

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

_cell_length_a                   14.6250(12)
_cell_length_b                   16.5741(14)
_cell_length_c                   16.2669(14)
_cell_angle_alpha                90
_cell_angle_beta                 107.071(3)
_cell_angle_gamma                90
_cell_volume                     3769.3(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1024
_cell_measurement_theta_min      2.458
_cell_measurement_theta_max      26.312

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_F_000             1596
_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    1.028
_shelx_estimated_absorpt_T_min   0.805
_shelx_estimated_absorpt_T_max   0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  2.458
_exptl_absorpt_correction_T_max  26.312
_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            18504
_diffrn_reflns_av_unetI/netI     0.1486
_diffrn_reflns_av_R_equivalents  0.1036
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.458
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_full        25.020
_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             6667
_reflns_number_gt                2556
_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)+(0.1237P)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         6667
_refine_ls_number_parameters     423
_refine_ls_number_restraints     495
_refine_ls_R_factor_all          0.1794
_refine_ls_R_factor_gt           0.0755
_refine_ls_wR_factor_ref         0.2369
_refine_ls_wR_factor_gt          0.1968
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_restrained_S_all      0.940
_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
Ni1 Ni 0.500000 1.000000 0.500000 0.0493(4) Uani 1 2 d S . P . .
Ni2 Ni 0.500000 0.500000 0.500000 0.0529(5) Uani 1 2 d S . P . .
V1 V 0.44590(12) 0.84352(8) 0.33033(8) 0.0602(5) Uani 1 1 d . . . . .
V2 V 0.54705(12) 0.66025(8) 0.35878(8) 0.0613(5) Uani 1 1 d . . . . .
N1 N 0.3835(6) 0.8926(5) 0.6776(4) 0.077(2) Uani 1 1 d . . . . .
N2 N 0.4530(5) 0.9248(4) 0.5815(4) 0.0628(19) Uani 1 1 d . . . . .
N3 N 0.7700(7) 0.8890(6) 0.5409(6) 0.098(3) Uani 1 1 d . . . . .
N4 N 0.6387(5) 0.9555(4) 0.5403(4) 0.063(2) Uani 1 1 d . . . . .
N5 N 0.6263(7) 0.6020(5) 0.7401(5) 0.085(3) Uani 1 1 d . . . . .
N6 N 0.5478(5) 0.5734(4) 0.6058(4) 0.067(2) Uani 1 1 d . . . . .
N7 N 0.2259(8) 0.6081(7) 0.4078(6) 0.107(3) Uani 1 1 d . . . . .
N8 N 0.3596(5) 0.5418(4) 0.4697(4) 0.063(2) Uani 1 1 d . . . . .
O1 O 0.4882(6) 0.7499(4) 0.3766(4) 0.0995(19) Uani 1 1 d . U . . .
O2 O 0.4705(4) 0.9127(3) 0.4051(3) 0.0625(15) Uani 1 1 d . U . . .
O3 O 0.500000 0.8695(5) 0.250000 0.098(3) Uani 1 2 d S TU P . .
O4 O 0.3323(6) 0.8387(6) 0.2935(6) 0.154(3) Uani 1 1 d . U . . .
O5 O 0.5260(4) 0.5881(3) 0.4209(3) 0.0693(16) Uani 1 1 d . U . . .
O6 O 0.6602(6) 0.6745(6) 0.3838(6) 0.150(3) Uani 1 1 d . U . . .
O7 O 0.500000 0.6315(5) 0.250000 0.094(3) Uani 1 2 d S TU P . .
O8 O 0.1988(7) 0.7415(7) 0.1788(7) 0.082(4) Uani 0.5 1 d . U P . .
H8C H 0.232807 0.773565 0.216135 0.099 Uiso 0.5 1 d R U P . .
H8D H 0.235377 0.716785 0.155125 0.099 Uiso 0.5 1 d R U P . .
C1 C 0.4193(6) 0.9513(5) 0.6429(5) 0.065(2) Uani 1 1 d . U . . .
H1 H 0.420666 1.005023 0.659677 0.078 Uiso 1 1 calc R U . . .
C2 C 0.4330(8) 0.8446(5) 0.5723(6) 0.086(3) Uani 1 1 d . U . . .
H2 H 0.445507 0.810750 0.531277 0.104 Uiso 1 1 calc R U . . .
C3 C 0.3912(9) 0.8224(6) 0.6339(7) 0.107(3) Uani 1 1 d . U . . .
H3 H 0.371854 0.770869 0.644237 0.129 Uiso 1 1 calc R U . . .
C4 C 0.3375(7) 0.9010(6) 0.7458(6) 0.095(3) Uani 1 1 d D U . . .
H4A H 0.355444 0.952324 0.774551 0.114 Uiso 1 1 calc R U . . .
H4B H 0.360080 0.858490 0.787872 0.114 Uiso 1 1 calc R U . . .
C5 C 0.2299(8) 0.8963(7) 0.7107(7) 0.123(3) Uani 1 1 d D U . . .
H5A H 0.202280 0.891260 0.757871 0.147 Uiso 1 1 calc R U . . .
H5B H 0.212014 0.849021 0.674415 0.147 Uiso 1 1 calc R U . . .
C6 C 0.1906(8) 0.9719(8) 0.6585(9) 0.142(4) Uani 1 1 d D U . . .
H6A H 0.218792 1.019289 0.691208 0.171 Uiso 1 1 calc R U . . .
H6B H 0.208833 0.971494 0.605797 0.171 Uiso 1 1 calc R U . . .
C7 C 0.0831(9) 0.9772(12) 0.6365(12) 0.256(9) Uani 1 1 d D U . . .
H7A H 0.054529 0.936186 0.595280 0.384 Uiso 1 1 calc R U . . .
H7B H 0.062185 1.029342 0.612644 0.384 Uiso 1 1 calc R U . . .
H7C H 0.064054 0.969390 0.687660 0.384 Uiso 1 1 calc R U . . .
C8 C 0.6736(9) 0.8881(6) 0.5167(6) 0.090(3) Uani 1 1 d . U . . .
H8 H 0.636215 0.845792 0.487288 0.108 Uiso 1 1 calc R U . . .
C9 C 0.7178(8) 0.9992(6) 0.5816(6) 0.077(3) Uani 1 1 d . U . . .
H9 H 0.716430 1.049564 0.606343 0.092 Uiso 1 1 calc R U . . .
C10 C 0.7984(9) 0.9593(7) 0.5816(7) 0.098(3) Uani 1 1 d . U . . .
H10 H 0.861009 0.976918 0.605056 0.117 Uiso 1 1 calc R U . . .
C11 C 0.8328(10) 0.8222(8) 0.5257(9) 0.145(4) Uani 1 1 d D U . . .
H11A H 0.890888 0.844589 0.517724 0.174 Uiso 1 1 calc R U . . .
H11B H 0.799644 0.792487 0.474133 0.174 Uiso 1 1 calc R U . . .
C12 C 0.8574(11) 0.7658(8) 0.6033(9) 0.181(5) Uani 1 1 d D U . . .
H12A H 0.879557 0.799294 0.654193 0.217 Uiso 1 1 calc R U . . .
H12B H 0.798165 0.740946 0.605541 0.217 Uiso 1 1 calc R U . . .
C13 C 0.9292(14) 0.6993(11) 0.6117(11) 0.264(7) Uani 1 1 d D U . . .
H13A H 0.917548 0.658619 0.650307 0.317 Uiso 1 1 calc R U . . .
H13B H 0.992592 0.721162 0.637913 0.317 Uiso 1 1 calc R U . . .
C14 C 0.9278(17) 0.6589(14) 0.5274(13) 0.301(10) Uani 1 1 d D U . . .
H14A H 0.950367 0.604437 0.538399 0.452 Uiso 1 1 calc R U . . .
H14B H 0.968434 0.688156 0.501093 0.452 Uiso 1 1 calc R U . . .
H14C H 0.863569 0.658611 0.489495 0.452 Uiso 1 1 calc R U . . .
C15 C 0.5791(7) 0.5470(5) 0.6842(6) 0.072(2) Uani 1 1 d . U . . .
H15 H 0.569353 0.494482 0.699795 0.087 Uiso 1 1 calc R U . . .
C16 C 0.5778(9) 0.6513(6) 0.6104(6) 0.100(3) Uani 1 1 d . U . . .
H16 H 0.567089 0.686417 0.563981 0.120 Uiso 1 1 calc R U . . .
C17 C 0.6262(10) 0.6702(7) 0.6937(7) 0.120(3) Uani 1 1 d . U . . .
H17 H 0.653428 0.719648 0.714341 0.144 Uiso 1 1 calc R U . . .
C18 C 0.6792(8) 0.5922(6) 0.8320(6) 0.099(3) Uani 1 1 d D U . . .
H18A H 0.653759 0.545931 0.854635 0.119 Uiso 1 1 calc R U . . .
H18B H 0.669176 0.639523 0.863315 0.119 Uiso 1 1 calc R U . . .
C19 C 0.7855(8) 0.5803(7) 0.8468(7) 0.140(4) Uani 1 1 d D U . . .
H19A H 0.817741 0.584242 0.907915 0.167 Uiso 1 1 calc R U . . .
H19B H 0.809146 0.623649 0.818460 0.167 Uiso 1 1 calc R U . . .
C20 C 0.8112(9) 0.5002(8) 0.8141(9) 0.157(5) Uani 1 1 d D U . . .
H20A H 0.788725 0.501321 0.751756 0.188 Uiso 1 1 calc R U . . .
H20B H 0.775761 0.458211 0.832941 0.188 Uiso 1 1 calc R U . . .
C21 C 0.9164(10) 0.4757(11) 0.8408(12) 0.235(8) Uani 1 1 d D U . . .
H21A H 0.929012 0.443559 0.796286 0.352 Uiso 1 1 calc R U . . .
H21B H 0.930779 0.445026 0.893101 0.352 Uiso 1 1 calc R U . . .
H21C H 0.955690 0.523248 0.849905 0.352 Uiso 1 1 calc R U . . .
C22 C 0.3227(10) 0.6101(7) 0.4309(7) 0.096(3) Uani 1 1 d . U . . .
H22 H 0.358485 0.653375 0.421120 0.115 Uiso 1 1 calc R U . . .
C23 C 0.2017(10) 0.5381(8) 0.4314(8) 0.108(3) Uani 1 1 d . U . . .
H23 H 0.139597 0.519920 0.423388 0.129 Uiso 1 1 calc R U . . .
C24 C 0.2819(9) 0.4970(6) 0.4691(7) 0.088(3) Uani 1 1 d . U . . .
H24 H 0.283903 0.445270 0.491700 0.106 Uiso 1 1 calc R U . . .
C25 C 0.1634(11) 0.6740(8) 0.3652(9) 0.155(4) Uani 1 1 d D U . . .
H25A H 0.100945 0.652314 0.335012 0.186 Uiso 1 1 calc R U . . .
H25B H 0.189599 0.698669 0.322997 0.186 Uiso 1 1 calc R U . . .
C26 C 0.1516(12) 0.7396(9) 0.4295(9) 0.203(5) Uani 1 1 d D U . . .
H26A H 0.142163 0.712156 0.479030 0.244 Uiso 1 1 calc R U . . .
H26B H 0.211680 0.768616 0.449278 0.244 Uiso 1 1 calc R U . . .
C27 C 0.0733(13) 0.8011(10) 0.4002(12) 0.253(7) Uani 1 1 d D U . . .
H27A H 0.014983 0.770874 0.375046 0.304 Uiso 1 1 calc R U . . .
H27B H 0.066329 0.826014 0.451923 0.304 Uiso 1 1 calc R U . . .
C28 C 0.0735(10) 0.8686(9) 0.3391(10) 0.337(11) Uani 1 1 d D U . . .
H28A H 0.128690 0.901917 0.362370 0.505 Uiso 1 1 calc R U . . .
H28B H 0.016596 0.900371 0.330851 0.505 Uiso 1 1 calc DR U . . .
H28C H 0.075155 0.846763 0.284896 0.505 Uiso 1 1 calc DR 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
Ni1 O2 2.067(5) 3_676 ?
Ni1 O2 2.067(5) . ?
Ni1 N4 2.076(7) 3_676 ?
Ni1 N4 2.076(7) . ?
Ni1 N2 2.079(7) . ?
Ni1 N2 2.079(7) 3_676 ?
Ni2 O5 2.054(5) 3_666 ?
Ni2 O5 2.054(5) . ?
Ni2 N6 2.056(7) 3_666 ?
Ni2 N6 2.056(7) . ?
Ni2 N8 2.084(7) 3_666 ?
Ni2 N8 2.084(7) . ?
V1 O4 1.594(8) . ?
V1 O2 1.633(5) . ?
V1 O1 1.756(6) . ?
V1 O3 1.768(2) . ?
V2 O6 1.602(8) . ?
V2 O5 1.652(5) . ?
V2 O7 1.765(3) . ?
V2 O1 1.783(6) . ?
N1 C1 1.308(10) . ?
N1 C3 1.385(11) . ?
N1 C4 1.462(10) . ?
N2 C1 1.312(9) . ?
N2 C2 1.360(10) . ?
N3 C10 1.344(13) . ?
N3 C8 1.348(12) . ?
N3 C11 1.505(13) . ?
N4 C8 1.330(11) . ?
N4 C9 1.362(11) . ?
N5 C15 1.329(11) . ?
N5 C17 1.358(12) . ?
N5 C18 1.476(11) . ?
N6 C15 1.297(9) . ?
N6 C16 1.357(11) . ?
N7 C23 1.302(14) . ?
N7 C22 1.354(13) . ?
N7 C25 1.463(13) . ?
N8 C22 1.330(11) . ?
N8 C24 1.356(11) . ?
O8 H8C 0.8500 . ?
O8 H8D 0.8499 . ?
C1 H1 0.9300 . ?
C2 C3 1.369(13) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.511(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.527(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.509(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 H8 0.9300 . ?
C9 C10 1.352(13) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.527(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 C13 1.499(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.521(9) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15 0.9300 . ?
C16 C17 1.368(13) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.515(8) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.518(9) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.526(9) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22 0.9300 . ?
C23 C24 1.339(14) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.552(9) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.501(9) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.497(10) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 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
O2 Ni1 O2 180.0 3_676 . ?
O2 Ni1 N4 87.6(3) 3_676 3_676 ?
O2 Ni1 N4 92.4(3) . 3_676 ?
O2 Ni1 N4 92.4(3) 3_676 . ?
O2 Ni1 N4 87.6(3) . . ?
N4 Ni1 N4 180.0 3_676 . ?
O2 Ni1 N2 88.8(2) 3_676 . ?
O2 Ni1 N2 91.2(2) . . ?
N4 Ni1 N2 86.5(3) 3_676 . ?
N4 Ni1 N2 93.5(3) . . ?
O2 Ni1 N2 91.2(2) 3_676 3_676 ?
O2 Ni1 N2 88.8(2) . 3_676 ?
N4 Ni1 N2 93.5(3) 3_676 3_676 ?
N4 Ni1 N2 86.5(3) . 3_676 ?
N2 Ni1 N2 180.0 . 3_676 ?
O5 Ni2 O5 180.0 3_666 . ?
O5 Ni2 N6 91.3(2) 3_666 3_666 ?
O5 Ni2 N6 88.7(2) . 3_666 ?
O5 Ni2 N6 88.7(2) 3_666 . ?
O5 Ni2 N6 91.3(2) . . ?
N6 Ni2 N6 180.0(3) 3_666 . ?
O5 Ni2 N8 88.0(3) 3_666 3_666 ?
O5 Ni2 N8 92.0(3) . 3_666 ?
N6 Ni2 N8 94.1(3) 3_666 3_666 ?
N6 Ni2 N8 85.9(3) . 3_666 ?
O5 Ni2 N8 92.0(3) 3_666 . ?
O5 Ni2 N8 88.0(3) . . ?
N6 Ni2 N8 85.9(3) 3_666 . ?
N6 Ni2 N8 94.1(3) . . ?
N8 Ni2 N8 180.0 3_666 . ?
O4 V1 O2 107.0(4) . . ?
O4 V1 O1 108.3(5) . . ?
O2 V1 O1 109.2(3) . . ?
O4 V1 O3 112.2(4) . . ?
O2 V1 O3 109.3(3) . . ?
O1 V1 O3 110.7(3) . . ?
O6 V2 O5 108.4(4) . . ?
O6 V2 O7 111.3(4) . . ?
O5 V2 O7 109.3(3) . . ?
O6 V2 O1 110.3(5) . . ?
O5 V2 O1 108.6(3) . . ?
O7 V2 O1 108.9(3) . . ?
C1 N1 C3 107.5(7) . . ?
C1 N1 C4 126.0(8) . . ?
C3 N1 C4 126.4(8) . . ?
C1 N2 C2 107.1(7) . . ?
C1 N2 Ni1 123.6(6) . . ?
C2 N2 Ni1 128.0(6) . . ?
C10 N3 C8 107.4(9) . . ?
C10 N3 C11 127.1(11) . . ?
C8 N3 C11 125.5(11) . . ?
C8 N4 C9 104.3(9) . . ?
C8 N4 Ni1 129.0(8) . . ?
C9 N4 Ni1 125.2(6) . . ?
C15 N5 C17 105.9(8) . . ?
C15 N5 C18 129.0(8) . . ?
C17 N5 C18 124.8(9) . . ?
C15 N6 C16 104.6(8) . . ?
C15 N6 Ni2 123.9(6) . . ?
C16 N6 Ni2 129.3(6) . . ?
C23 N7 C22 106.9(10) . . ?
C23 N7 C25 128.2(13) . . ?
C22 N7 C25 124.8(12) . . ?
C22 N8 C24 103.8(10) . . ?
C22 N8 Ni2 129.1(8) . . ?
C24 N8 Ni2 125.8(7) . . ?
V1 O1 V2 142.5(4) . . ?
V1 O2 Ni1 179.3(3) . . ?
V1 O3 V1 151.8(5) 2_655 . ?
V2 O5 Ni2 178.9(3) . . ?
V2 O7 V2 148.7(5) . 2_655 ?
H8C O8 H8D 108.1 . . ?
N1 C1 N2 111.5(8) . . ?
N1 C1 H1 124.3 . . ?
N2 C1 H1 124.3 . . ?
N2 C2 C3 108.0(8) . . ?
N2 C2 H2 126.0 . . ?
C3 C2 H2 126.0 . . ?
C2 C3 N1 105.7(9) . . ?
C2 C3 H3 127.2 . . ?
N1 C3 H3 127.2 . . ?
N1 C4 C5 111.7(8) . . ?
N1 C4 H4A 109.3 . . ?
C5 C4 H4A 109.3 . . ?
N1 C4 H4B 109.3 . . ?
C5 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
C4 C5 C6 110.4(9) . . ?
C4 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C7 C6 C5 112.0(10) . . ?
C7 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
C7 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N4 C8 N3 111.3(10) . . ?
N4 C8 H8 124.4 . . ?
N3 C8 H8 124.4 . . ?
C10 C9 N4 110.7(10) . . ?
C10 C9 H9 124.6 . . ?
N4 C9 H9 124.6 . . ?
N3 C10 C9 106.3(11) . . ?
N3 C10 H10 126.9 . . ?
C9 C10 H10 126.9 . . ?
N3 C11 C12 108.7(10) . . ?
N3 C11 H11A 109.9 . . ?
C12 C11 H11A 109.9 . . ?
N3 C11 H11B 109.9 . . ?
C12 C11 H11B 109.9 . . ?
H11A C11 H11B 108.3 . . ?
C13 C12 C11 120.9(11) . . ?
C13 C12 H12A 107.1 . . ?
C11 C12 H12A 107.1 . . ?
C13 C12 H12B 107.1 . . ?
C11 C12 H12B 107.1 . . ?
H12A C12 H12B 106.8 . . ?
C12 C13 C14 114.7(11) . . ?
C12 C13 H13A 108.6 . . ?
C14 C13 H13A 108.6 . . ?
C12 C13 H13B 108.6 . . ?
C14 C13 H13B 108.6 . . ?
H13A C13 H13B 107.6 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N6 C15 N5 113.8(8) . . ?
N6 C15 H15 123.1 . . ?
N5 C15 H15 123.1 . . ?
N6 C16 C17 109.7(9) . . ?
N6 C16 H16 125.2 . . ?
C17 C16 H16 125.2 . . ?
N5 C17 C16 106.0(10) . . ?
N5 C17 H17 127.0 . . ?
C16 C17 H17 127.0 . . ?
N5 C18 C19 112.5(8) . . ?
N5 C18 H18A 109.1 . . ?
C19 C18 H18A 109.1 . . ?
N5 C18 H18B 109.1 . . ?
C19 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C18 C19 C20 114.0(9) . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
C20 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 C21 117.8(11) . . ?
C19 C20 H20A 107.9 . . ?
C21 C20 H20A 107.9 . . ?
C19 C20 H20B 107.9 . . ?
C21 C20 H20B 107.9 . . ?
H20A C20 H20B 107.2 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N8 C22 N7 111.0(11) . . ?
N8 C22 H22 124.5 . . ?
N7 C22 H22 124.5 . . ?
N7 C23 C24 108.2(13) . . ?
N7 C23 H23 125.9 . . ?
C24 C23 H23 125.9 . . ?
C23 C24 N8 110.1(11) . . ?
C23 C24 H24 125.0 . . ?
N8 C24 H24 125.0 . . ?
N7 C25 C26 112.5(10) . . ?
N7 C25 H25A 109.1 . . ?
C26 C25 H25A 109.1 . . ?
N7 C25 H25B 109.1 . . ?
C26 C25 H25B 109.1 . . ?
H25A C25 H25B 107.8 . . ?
C27 C26 C25 119.1(11) . . ?
C27 C26 H26A 107.5 . . ?
C25 C26 H26A 107.5 . . ?
C27 C26 H26B 107.5 . . ?
C25 C26 H26B 107.5 . . ?
H26A C26 H26B 107.0 . . ?
C28 C27 C26 124.7(13) . . ?
C28 C27 H27A 106.2 . . ?
C26 C27 H27A 106.2 . . ?
C28 C27 H27B 106.2 . . ?
C26 C27 H27B 106.2 . . ?
H27A C27 H27B 106.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_refine_diff_density_max         0.867
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.108

####################################################################### 
# 
# 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_180718a
_database_code_depnum_ccdc_archive 'CCDC 1999279'
loop_
_audit_author_name
_audit_author_address
'Mingyu Dou'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2020-04-26 deposited with the CCDC.	2020-05-21 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            'C20 H54 N8 Ni2 O38 V10'
_chemical_formula_weight         1641.53

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      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                   11.8760(9)
_cell_length_b                   12.2282(11)
_cell_length_c                   17.4796(14)
_cell_angle_alpha                90
_cell_angle_beta                 101.696(3)
_cell_angle_gamma                90
_cell_volume                     2485.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1024
_cell_measurement_theta_min      2.409
_cell_measurement_theta_max      26.888

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            GREEN
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_F_000             1640
_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    2.639
_shelx_estimated_absorpt_T_min   0.594
_shelx_estimated_absorpt_T_max   0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_T_max  0.647
_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            11767
_diffrn_reflns_av_unetI/netI     0.1343
_diffrn_reflns_av_R_equivalents  0.1355
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.308
_diffrn_reflns_theta_max         25.011
_diffrn_reflns_theta_full        25.011
_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             4369
_reflns_number_gt                2657
_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)+(0.1370P)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         4369
_refine_ls_number_parameters     354
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0856
_refine_ls_wR_factor_ref         0.2432
_refine_ls_wR_factor_gt          0.2204
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      0.999
_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 0.56933(12) 0.95572(11) 0.64241(8) 0.0281(4) Uani 1 1 d . . . . .
V1 V 0.38072(15) 0.50052(14) 0.53270(10) 0.0232(4) Uani 1 1 d . . . . .
V2 V 0.50591(15) 0.71851(14) 0.51225(10) 0.0247(5) Uani 1 1 d . . . . .
V3 V 0.61296(16) 0.56052(14) 0.64172(10) 0.0260(5) Uani 1 1 d . . . . .
V4 V 0.27975(16) 0.65532(14) 0.39929(10) 0.0278(5) Uani 1 1 d . . . . .
V5 V 0.49379(16) 0.34226(14) 0.65962(10) 0.0287(5) Uani 1 1 d . . . . .
O1 O 0.2604(6) 0.5669(6) 0.4938(4) 0.0272(16) Uani 1 1 d . . . . .
O2 O 0.3542(6) 0.4303(6) 0.6083(4) 0.0298(17) Uani 1 1 d . . . . .
O3 O 0.3571(6) 0.3812(5) 0.4580(4) 0.0230(15) Uani 1 1 d . . . . .
O4 O 0.4488(7) 0.2839(7) 0.7277(4) 0.043(2) Uani 1 1 d . . . . .
O5 O 0.5463(6) 0.4318(5) 0.5559(4) 0.0238(15) Uani 1 1 d . . . . .
O6 O 0.5480(6) 0.4765(6) 0.7046(4) 0.0307(18) Uani 1 1 d . . . . .
O7 O 0.7422(6) 0.4775(5) 0.6528(4) 0.0260(16) Uani 1 1 d . . . . .
O8 O 0.6609(6) 0.6623(5) 0.6972(4) 0.0290(17) Uani 1 1 d . . . . .
O9 O 0.4622(6) 0.6176(5) 0.5887(4) 0.0242(15) Uani 1 1 d . . . . .
O10 O 0.5544(6) 0.7526(6) 0.4240(4) 0.0284(17) Uani 1 1 d . . . . .
O11 O 0.5467(6) 0.8233(5) 0.5679(4) 0.0267(16) Uani 1 1 d . . . . .
O12 O 0.3592(6) 0.7525(5) 0.4732(4) 0.0235(15) Uani 1 1 d . . . . .
O13 O 0.3591(6) 0.7076(6) 0.3277(4) 0.0272(16) Uani 1 1 d . . . . .
O14 O 0.1583(6) 0.7127(6) 0.3756(4) 0.039(2) Uani 1 1 d . . . . .
O15 O 0.7201(6) 0.8762(6) 0.6880(4) 0.0330(18) Uani 1 1 d . . . . .
H15A H 0.709044 0.832667 0.723706 0.049 Uiso 1 1 d R U . . .
H15C H 0.770934 0.922947 0.707316 0.049 Uiso 1 1 d R U . . .
O16 O 0.6644(6) 1.0342(6) 0.5698(4) 0.0349(18) Uani 1 1 d . . . . .
H16A H 0.686322 1.096415 0.588846 0.052 Uiso 1 1 d R U . . .
H16B H 0.722742 0.995436 0.566886 0.052 Uiso 1 1 d R U . . .
O17 O 0.6137(6) 1.0795(6) 0.7222(4) 0.0352(19) Uani 1 1 d . . . . .
H17C H 0.565332 1.028369 0.708572 0.042 Uiso 1 1 d R U . . .
H17D H 0.593671 1.134808 0.693111 0.042 Uiso 1 1 d R U . . .
O18 O 0.4261(6) 1.0343(6) 0.5839(4) 0.0343(18) Uani 1 1 d . . . . .
H18B H 0.436337 1.102980 0.588431 0.051 Uiso 1 1 d R U . . .
H18C H 0.414547 1.016680 0.535931 0.051 Uiso 1 1 d R U . . .
O19 O 0.8924(7) 0.0528(7) 0.6429(5) 0.046(2) Uani 1 1 d . . . . .
H19C H 0.905276 0.027861 0.689267 0.055 Uiso 1 1 d R U . . .
H19B H 0.910806 0.119961 0.643107 0.055 Uiso 1 1 d R U . . .
N1 N 0.4725(8) 0.8938(8) 0.7139(5) 0.036(2) Uani 1 1 d . . . . .
N2 N 0.3683(9) 0.7834(9) 0.7710(7) 0.052(3) Uani 1 1 d . . . . .
N3 N 0.9835(11) 0.2306(10) 0.4175(9) 0.071(4) Uani 1 1 d . . . . .
N4 N 1.1413(11) 0.3156(11) 0.4329(7) 0.065(3) Uani 1 1 d . . . . .
H4 H 1.213445 0.329213 0.437544 0.078 Uiso 1 1 calc R U . . .
C1 C 0.9631(15) 0.3317(15) 0.4363(13) 0.098(7) Uani 1 1 d . . . . .
H1 H 0.892454 0.359162 0.442431 0.118 Uiso 1 1 calc R U . . .
C2 C 1.0593(17) 0.3871(18) 0.4451(12) 0.097(6) Uani 1 1 d . U . . .
H2 H 1.069431 0.460998 0.457231 0.116 Uiso 1 1 calc R U . . .
C3 C 1.0911(13) 0.2230(14) 0.4129(9) 0.067(5) Uani 1 1 d . . . . .
H3 H 1.126219 0.161064 0.397609 0.080 Uiso 1 1 calc R U . . .
C4 C 0.8985(19) 0.1430(18) 0.3879(13) 0.110(7) Uani 1 1 d D U . . .
H4A H 0.849480 0.165979 0.339167 0.133 Uiso 1 1 calc R U . . .
H4B H 0.938340 0.076848 0.378084 0.133 Uiso 1 1 calc R U . . .
C5 C 0.832(2) 0.123(2) 0.4434(15) 0.154(10) Uani 1 1 d D U . . .
H5A H 0.881841 0.107491 0.492814 0.231 Uiso 1 1 calc R U . . .
H5B H 0.783083 0.061267 0.427436 0.231 Uiso 1 1 calc R U . . .
H5C H 0.786283 0.186053 0.448331 0.231 Uiso 1 1 calc R U . . .
C6 C 0.4419(11) 0.7913(9) 0.7227(7) 0.038(3) Uani 1 1 d . . . . .
H8 H 0.468424 0.731888 0.698183 0.046 Uiso 1 1 calc R U . . .
C7 C 0.3526(14) 0.8884(13) 0.7950(9) 0.068(5) Uani 1 1 d . . . . .
H6 H 0.307055 0.910188 0.829724 0.082 Uiso 1 1 calc R U . . .
C8 C 0.4171(13) 0.9539(12) 0.7578(8) 0.060(4) Uani 1 1 d . . . . .
H8A H 0.421755 1.029639 0.762441 0.072 Uiso 1 1 calc R U . . .
C9 C 0.3185(14) 0.6822(15) 0.7934(11) 0.083(6) Uani 1 1 d . . . . .
H9A H 0.237544 0.679872 0.768946 0.100 Uiso 1 1 calc R U . . .
H9B H 0.355858 0.620527 0.774123 0.100 Uiso 1 1 calc R U . . .
C10 C 0.330(2) 0.6719(18) 0.8761(14) 0.123(9) Uani 1 1 d . . . . .
H10A H 0.410038 0.671423 0.900577 0.184 Uiso 1 1 calc R U . . .
H10B H 0.294906 0.604888 0.887817 0.184 Uiso 1 1 calc R U . . .
H10C H 0.292742 0.732553 0.895586 0.184 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
Ni1 N1 2.010(9) . ?
Ni1 O18 2.039(7) . ?
Ni1 O15 2.051(7) . ?
Ni1 O17 2.053(7) . ?
Ni1 O11 2.062(7) . ?
Ni1 O16 2.095(7) . ?
Ni1 H17C 1.4667 . ?
V1 O2 1.659(7) . ?
V1 O1 1.663(7) . ?
V1 O9 1.887(7) . ?
V1 O3 1.940(7) . ?
V1 O5 2.093(7) 3_666 ?
V1 O5 2.100(7) . ?
V2 O11 1.622(7) . ?
V2 O12 1.787(7) . ?
V2 O10 1.802(7) . ?
V2 O9 1.965(7) . ?
V2 O3 2.015(7) 3_666 ?
V2 O5 2.210(7) 3_666 ?
V2 V5 3.096(2) 3_666 ?
V3 O8 1.609(7) . ?
V3 O6 1.789(7) . ?
V3 O7 1.818(7) . ?
V3 O9 1.969(7) . ?
V3 O3 1.981(7) 3_666 ?
V3 O5 2.207(7) . ?
V3 V4 3.078(2) 3_666 ?
V4 O14 1.582(7) . ?
V4 O13 1.827(7) . ?
V4 O7 1.854(7) 3_666 ?
V4 O12 1.865(6) . ?
V4 O1 2.027(7) . ?
V4 O5 2.316(7) 3_666 ?
V4 V5 3.069(3) 3_666 ?
V5 O4 1.570(7) . ?
V5 O13 1.822(7) 3_666 ?
V5 O10 1.863(7) 3_666 ?
V5 O6 1.877(7) . ?
V5 O2 2.027(7) . ?
V5 O5 2.309(7) . ?
O15 H15A 0.8498 . ?
O15 H15C 0.8500 . ?
O16 H16A 0.8500 . ?
O16 H16B 0.8500 . ?
O17 H17C 0.8500 . ?
O17 H17D 0.8501 . ?
O18 H18B 0.8499 . ?
O18 H18C 0.8500 . ?
O19 H19C 0.8501 . ?
O19 H19B 0.8499 . ?
N1 C6 1.322(14) . ?
N1 C8 1.330(15) . ?
N2 C6 1.336(15) . ?
N2 C7 1.375(18) . ?
N2 C9 1.459(19) . ?
N3 C3 1.300(18) . ?
N3 C1 1.31(2) . ?
N3 C4 1.49(2) . ?
N4 C3 1.294(18) . ?
N4 C2 1.36(2) . ?
N4 H4 0.8600 . ?
C1 C2 1.31(2) . ?
C1 H1 0.9300 . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.389(16) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H8 0.9300 . ?
C7 C8 1.362(18) . ?
C7 H6 0.9300 . ?
C8 H8A 0.9300 . ?
C9 C10 1.43(3) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 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
N1 Ni1 O18 88.0(3) . . ?
N1 Ni1 O15 98.3(3) . . ?
O18 Ni1 O15 172.8(3) . . ?
N1 Ni1 O17 87.5(3) . . ?
O18 Ni1 O17 93.8(3) . . ?
O15 Ni1 O17 90.1(3) . . ?
N1 Ni1 O11 94.5(3) . . ?
O18 Ni1 O11 93.7(3) . . ?
O15 Ni1 O11 82.2(3) . . ?
O17 Ni1 O11 172.3(3) . . ?
N1 Ni1 O16 174.8(4) . . ?
O18 Ni1 O16 88.7(3) . . ?
O15 Ni1 O16 85.3(3) . . ?
O17 Ni1 O16 88.7(3) . . ?
O11 Ni1 O16 89.6(3) . . ?
N1 Ni1 H17C 67.9 . . ?
O18 Ni1 H17C 87.3 . . ?
O15 Ni1 H17C 98.4 . . ?
O17 Ni1 H17C 20.4 . . ?
O11 Ni1 H17C 162.4 . . ?
O16 Ni1 H17C 107.9 . . ?
O2 V1 O1 107.0(4) . . ?
O2 V1 O9 98.0(3) . . ?
O1 V1 O9 98.6(3) . . ?
O2 V1 O3 97.0(3) . . ?
O1 V1 O3 95.5(3) . . ?
O9 V1 O3 155.4(3) . . ?
O2 V1 O5 165.5(3) . 3_666 ?
O1 V1 O5 87.4(3) . 3_666 ?
O9 V1 O5 80.7(3) . 3_666 ?
O3 V1 O5 79.9(3) . 3_666 ?
O2 V1 O5 87.7(3) . . ?
O1 V1 O5 165.2(3) . . ?
O9 V1 O5 80.9(3) . . ?
O3 V1 O5 80.3(3) . . ?
O5 V1 O5 77.8(3) 3_666 . ?
O11 V2 O12 101.3(3) . . ?
O11 V2 O10 102.8(3) . . ?
O12 V2 O10 94.3(3) . . ?
O11 V2 O9 100.2(3) . . ?
O12 V2 O9 91.9(3) . . ?
O10 V2 O9 154.5(3) . . ?
O11 V2 O3 101.3(3) . 3_666 ?
O12 V2 O3 155.9(3) . 3_666 ?
O10 V2 O3 88.8(3) . 3_666 ?
O9 V2 O3 75.9(3) . 3_666 ?
O11 V2 O5 175.8(3) . 3_666 ?
O12 V2 O5 80.9(3) . 3_666 ?
O10 V2 O5 80.4(3) . 3_666 ?
O9 V2 O5 76.1(3) . 3_666 ?
O3 V2 O5 76.1(3) 3_666 3_666 ?
O11 V2 V5 135.4(2) . 3_666 ?
O12 V2 V5 83.0(2) . 3_666 ?
O10 V2 V5 33.0(2) . 3_666 ?
O9 V2 V5 124.2(2) . 3_666 ?
O3 V2 V5 86.87(19) 3_666 3_666 ?
O5 V2 V5 48.12(17) 3_666 3_666 ?
O8 V3 O6 102.6(3) . . ?
O8 V3 O7 100.4(3) . . ?
O6 V3 O7 94.2(3) . . ?
O8 V3 O9 100.7(3) . . ?
O6 V3 O9 91.6(3) . . ?
O7 V3 O9 156.3(3) . . ?
O8 V3 O3 98.5(3) . 3_666 ?
O6 V3 O3 157.5(3) . 3_666 ?
O7 V3 O3 89.8(3) . 3_666 ?
O9 V3 O3 76.5(3) . 3_666 ?
O8 V3 O5 174.4(3) . . ?
O6 V3 O5 82.4(3) . . ?
O7 V3 O5 81.6(3) . . ?
O9 V3 O5 76.5(3) . . ?
O3 V3 O5 76.3(3) 3_666 . ?
O8 V3 V4 133.7(3) . 3_666 ?
O6 V3 V4 84.3(2) . 3_666 ?
O7 V3 V4 33.4(2) . 3_666 ?
O9 V3 V4 125.0(2) . 3_666 ?
O3 V3 V4 86.95(19) 3_666 3_666 ?
O5 V3 V4 48.61(18) . 3_666 ?
O14 V4 O13 103.6(4) . . ?
O14 V4 O7 103.3(4) . 3_666 ?
O13 V4 O7 90.6(3) . 3_666 ?
O14 V4 O12 101.8(4) . . ?
O13 V4 O12 89.6(3) . . ?
O7 V4 O12 154.1(3) 3_666 . ?
O14 V4 O1 101.6(4) . . ?
O13 V4 O1 154.7(3) . . ?
O7 V4 O1 84.6(3) 3_666 . ?
O12 V4 O1 84.3(3) . . ?
O14 V4 O5 175.1(4) . 3_666 ?
O13 V4 O5 81.0(3) . 3_666 ?
O7 V4 O5 77.9(3) 3_666 3_666 ?
O12 V4 O5 76.6(3) . 3_666 ?
O1 V4 O5 73.7(3) . 3_666 ?
O14 V4 V5 136.3(3) . 3_666 ?
O13 V4 V5 32.7(2) . 3_666 ?
O7 V4 V5 83.6(2) 3_666 3_666 ?
O12 V4 V5 82.6(2) . 3_666 ?
O1 V4 V5 122.0(2) . 3_666 ?
O5 V4 V5 48.34(17) 3_666 3_666 ?
O14 V4 V3 135.9(3) . 3_666 ?
O13 V4 V3 81.1(2) . 3_666 ?
O7 V4 V3 32.7(2) 3_666 3_666 ?
O12 V4 V3 122.2(2) . 3_666 ?
O1 V4 V3 81.5(2) . 3_666 ?
O5 V4 V3 45.65(17) 3_666 3_666 ?
V5 V4 V3 59.85(6) 3_666 3_666 ?
O4 V5 O13 102.8(4) . 3_666 ?
O4 V5 O10 102.4(4) . 3_666 ?
O13 V5 O10 91.2(3) 3_666 3_666 ?
O4 V5 O6 102.7(4) . . ?
O13 V5 O6 90.2(3) 3_666 . ?
O10 V5 O6 153.9(3) 3_666 . ?
O4 V5 O2 101.7(4) . . ?
O13 V5 O2 155.5(3) 3_666 . ?
O10 V5 O2 83.7(3) 3_666 . ?
O6 V5 O2 84.3(3) . . ?
O4 V5 O5 175.8(4) . . ?
O13 V5 O5 81.3(3) 3_666 . ?
O10 V5 O5 76.6(3) 3_666 . ?
O6 V5 O5 77.9(3) . . ?
O2 V5 O5 74.2(3) . . ?
O4 V5 V4 135.6(3) . 3_666 ?
O13 V5 V4 32.8(2) 3_666 3_666 ?
O10 V5 V4 83.9(2) 3_666 3_666 ?
O6 V5 V4 83.3(2) . 3_666 ?
O2 V5 V4 122.7(2) . 3_666 ?
O5 V5 V4 48.52(17) . 3_666 ?
O4 V5 V2 133.9(3) . 3_666 ?
O13 V5 V2 81.2(2) 3_666 3_666 ?
O10 V5 V2 31.8(2) 3_666 3_666 ?
O6 V5 V2 123.3(2) . 3_666 ?
O2 V5 V2 81.9(2) . 3_666 ?
O5 V5 V2 45.44(17) . 3_666 ?
V4 V5 V2 60.21(6) 3_666 3_666 ?
V1 O1 V4 111.3(4) . . ?
V1 O2 V5 110.9(4) . . ?
V1 O3 V3 107.1(3) . 3_666 ?
V1 O3 V2 106.4(3) . 3_666 ?
V3 O3 V2 99.5(3) 3_666 3_666 ?
V1 O5 V1 102.2(3) 3_666 . ?
V1 O5 V3 94.3(3) 3_666 . ?
V1 O5 V3 92.2(3) . . ?
V1 O5 V2 92.4(3) 3_666 3_666 ?
V1 O5 V2 94.5(3) . 3_666 ?
V3 O5 V2 169.2(3) . 3_666 ?
V1 O5 V5 170.7(4) 3_666 . ?
V1 O5 V5 87.2(2) . . ?
V3 O5 V5 85.5(2) . . ?
V2 O5 V5 86.4(2) 3_666 . ?
V1 O5 V4 87.5(2) 3_666 3_666 ?
V1 O5 V4 170.2(3) . 3_666 ?
V3 O5 V4 85.7(2) . 3_666 ?
V2 O5 V4 86.1(2) 3_666 3_666 ?
V5 O5 V4 83.1(2) . 3_666 ?
V3 O6 V5 113.5(4) . . ?
V3 O7 V4 113.9(4) . 3_666 ?
V1 O9 V2 107.6(3) . . ?
V1 O9 V3 107.3(3) . . ?
V2 O9 V3 101.6(3) . . ?
V2 O10 V5 115.3(4) . 3_666 ?
V2 O11 Ni1 169.8(4) . . ?
V2 O12 V4 115.7(4) . . ?
V5 O13 V4 114.5(4) 3_666 . ?
Ni1 O15 H15A 109.3 . . ?
Ni1 O15 H15C 109.2 . . ?
H15A O15 H15C 109.5 . . ?
Ni1 O16 H16A 109.4 . . ?
Ni1 O16 H16B 109.1 . . ?
H16A O16 H16B 109.5 . . ?
Ni1 O17 H17C 37.0 . . ?
Ni1 O17 H17D 100.3 . . ?
H17C O17 H17D 109.1 . . ?
Ni1 O18 H18B 109.3 . . ?
Ni1 O18 H18C 109.1 . . ?
H18B O18 H18C 109.5 . . ?
H19C O19 H19B 110.3 . . ?
C6 N1 C8 106.1(10) . . ?
C6 N1 Ni1 129.4(8) . . ?
C8 N1 Ni1 124.2(9) . . ?
C6 N2 C7 105.8(11) . . ?
C6 N2 C9 125.8(12) . . ?
C7 N2 C9 128.4(12) . . ?
C3 N3 C1 108.4(13) . . ?
C3 N3 C4 122.1(15) . . ?
C1 N3 C4 128.1(15) . . ?
C3 N4 C2 107.4(14) . . ?
C3 N4 H4 126.3 . . ?
C2 N4 H4 126.3 . . ?
C2 C1 N3 108.4(16) . . ?
C2 C1 H1 125.8 . . ?
N3 C1 H1 125.8 . . ?
C1 C2 N4 106.5(18) . . ?
C1 C2 H2 126.8 . . ?
N4 C2 H2 126.8 . . ?
N4 C3 N3 109.0(14) . . ?
N4 C3 H3 125.5 . . ?
N3 C3 H3 125.5 . . ?
C5 C4 N3 108.8(19) . . ?
C5 C4 H4A 109.9 . . ?
N3 C4 H4A 109.9 . . ?
C5 C4 H4B 109.9 . . ?
N3 C4 H4B 109.9 . . ?
H4A C4 H4B 108.3 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 N2 111.9(11) . . ?
N1 C6 H8 124.1 . . ?
N2 C6 H8 124.1 . . ?
C8 C7 N2 106.2(12) . . ?
C8 C7 H6 126.9 . . ?
N2 C7 H6 126.9 . . ?
N1 C8 C7 110.0(13) . . ?
N1 C8 H8A 125.0 . . ?
C7 C8 H8A 125.0 . . ?
C10 C9 N2 112.7(18) . . ?
C10 C9 H9A 109.1 . . ?
N2 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
N2 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?

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
C9 H9A O4 0.97 2.56 3.360(18) 139.3 2_556 yes
C7 H6 O2 0.93 2.40 3.291(15) 161.5 2_556 yes
C6 H8 O9 0.93 2.36 3.206(14) 151.5 . yes
C6 H8 O8 0.93 2.44 3.149(14) 132.9 . yes
C5 H5C O12 0.96 2.53 3.31(3) 138.8 3_666 yes
C4 H4B O19 0.97 2.64 3.57(3) 159.5 3_756 yes
C4 H4A O4 0.97 2.55 3.11(2) 116.9 4_665 yes
C3 H3 O15 0.93 2.62 3.349(16) 135.2 3_766 yes
C2 H2 O1 0.93 2.58 3.23(2) 127.7 1_655 yes
C1 H1 O1 0.93 2.49 3.375(19) 160.2 3_666 yes
N4 H4 O3 0.86 1.79 2.635(14) 168.5 1_655 yes
O19 H19B O14 0.85 2.20 2.935(11) 144.0 3_666 yes
O19 H19C O6 0.85 1.93 2.777(11) 173.6 2_646 yes
O18 H18C O16 0.85 1.99 2.812(10) 161.0 3_676 yes
O18 H18B O10 0.85 1.79 2.622(10) 167.8 3_676 yes
O17 H17D O13 0.85 2.06 2.785(10) 142.8 3_676 yes
O17 H17D O4 0.85 2.66 3.189(11) 121.7 1_565 yes
O16 H16B O19 0.85 2.29 2.760(11) 115.3 1_565 yes
O16 H16A O12 0.85 2.16 2.713(10) 123.0 3_676 yes
O15 H15C O19 0.85 2.56 3.183(11) 131.5 1_565 yes
O15 H15C O7 0.85 2.57 2.994(10) 112.1 2_656 yes
O15 H15C O6 0.85 2.47 3.243(11) 152.3 2_656 yes
O15 H15A O13 0.85 2.33 2.846(10) 119.9 4_676 yes
O15 H15A O8 0.85 2.18 2.721(10) 120.9 . yes

_refine_diff_density_max         1.583
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.229

####################################################################### 
# 
# 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_180720e
_database_code_depnum_ccdc_archive 'CCDC 1999282'
loop_
_audit_author_name
_audit_author_address
'Mingyu Dou'
;Beijing Institute of Technology
China
;
_audit_update_record             
;
2020-04-26 deposited with the CCDC.	2020-05-21 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            'C12 H50 N4 Ni2 O42 V10'
_chemical_formula_weight         1549.38

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      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                   19.4747(16)
_cell_length_b                   9.2565(8)
_cell_length_c                   14.0833(12)
_cell_angle_alpha                90
_cell_angle_beta                 106.177(2)
_cell_angle_gamma                90
_cell_volume                     2438.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2288
_cell_measurement_theta_min      2.455
_cell_measurement_theta_max      28.1791

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_F_000             1544
_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    2.687
_shelx_estimated_absorpt_T_min   0.589
_shelx_estimated_absorpt_T_max   0.643
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(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            6064
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.455
_diffrn_reflns_theta_max         25.011
_diffrn_reflns_theta_full        25.012
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2277
_reflns_number_gt                1666
_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)+(0.1043P)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         2277
_refine_ls_number_parameters     208
_refine_ls_number_restraints     145
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1720
_refine_ls_wR_factor_gt          0.1546
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.002

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 0.21942(5) 0.500000 0.61475(8) 0.0239(3) Uani 1 2 d S T P . .
V1 V 0.40861(7) 0.500000 0.61399(10) 0.0197(4) Uani 1 2 d S T P . .
V2 V 0.54593(5) 0.33501(11) 0.72892(7) 0.0260(3) Uani 1 1 d . . . . .
V3 V 0.63771(7) 0.500000 0.61516(10) 0.0215(4) Uani 1 2 d S T P . .
V4 V 0.500000 0.67587(14) 0.500000 0.0189(4) Uani 1 2 d S T P . .
N1 N 0.7734(7) 0.0451(15) 0.9883(10) 0.147(5) Uani 0.5 1 d D U P A -1
N2 N 0.6655(8) -0.0579(18) 0.9622(12) 0.151(5) Uani 0.5 1 d D U P A -1
H2 H 0.623895 -0.091447 0.932455 0.181 Uiso 0.5 1 calc R U P A -1
O1 O 0.5189(3) 0.500000 0.5981(4) 0.0195(12) Uani 1 2 d S T P . .
O2 O 0.44557(19) 0.3553(4) 0.6988(3) 0.0236(9) Uani 1 1 d . . . . .
O3 O 0.3235(3) 0.500000 0.6109(4) 0.0235(13) Uani 1 2 d S T P . .
O4 O 0.63449(19) 0.3538(4) 0.7009(3) 0.0252(9) Uani 1 1 d . . . . .
O5 O 0.5200(2) 0.2150(4) 0.6006(3) 0.0259(9) Uani 1 1 d . . . . .
O6 O 0.5603(3) 0.500000 0.8016(4) 0.0264(13) Uani 1 2 d S T P . .
O7 O 0.5618(2) 0.2081(5) 0.8084(3) 0.0379(11) Uani 1 1 d . . . . .
O8 O 0.59662(18) 0.6335(4) 0.5009(3) 0.0188(8) Uani 1 1 d . . . . .
O9 O 0.7193(3) 0.500000 0.6138(4) 0.0293(14) Uani 1 2 d S T P . .
O10 O 0.2417(2) 0.6601(4) 0.7211(3) 0.0333(10) Uani 1 1 d . . . . .
H10C H 0.205903 0.715700 0.714799 0.040 Uiso 1 1 d R U . . .
H10D H 0.277843 0.711890 0.721799 0.040 Uiso 1 1 d R U . . .
O11 O 0.1932(2) 0.6564(4) 0.5050(3) 0.0310(10) Uani 1 1 d . . . . .
H11C H 0.159611 0.715480 0.504303 0.037 Uiso 1 1 d R U . . .
H11D H 0.229781 0.704760 0.502633 0.037 Uiso 0.5 1 d R U P . .
H11A H 0.180631 0.600990 0.455003 0.037 Uiso 0.5 1 d R U P . .
O12 O 0.1185(3) 0.500000 0.6291(5) 0.0419(17) Uani 1 2 d S T P . .
H12 H 0.091855 0.574350 0.621174 0.050 Uiso 1 1 d R U . . .
O13 O 0.3534(3) 0.8447(6) 0.7240(6) 0.103(3) Uani 1 1 d . . . . .
H13C H 0.388331 0.796535 0.715215 0.123 Uiso 1 1 d R U . . .
H13D H 0.362521 0.934205 0.721675 0.123 Uiso 0.5 1 d R U P B 1
H13B H 0.328686 0.892774 0.674877 0.123 Uiso 0.5 1 d R U P C 2
C1 C 0.7123(9) 0.006(2) 0.9154(10) 0.143(5) Uani 0.5 1 d D U P A -1
H1 H 0.703993 0.018882 0.847676 0.172 Uiso 0.5 1 calc R U P A -1
C2 C 0.6959(10) -0.059(2) 1.0638(12) 0.148(5) Uani 0.5 1 d D U P A -1
H2A H 0.675510 -0.095346 1.111267 0.177 Uiso 0.5 1 calc R U P A -1
C3 C 0.7637(9) 0.005(3) 1.0807(10) 0.144(5) Uani 0.5 1 d D U P A -1
H3 H 0.796533 0.019067 1.142052 0.173 Uiso 0.5 1 calc R U P A -1
C4 C 0.8375(9) 0.115(2) 0.9789(15) 0.149(5) Uani 0.5 1 d D U P A -1
H4A H 0.867091 0.136430 1.045035 0.179 Uiso 0.5 1 calc R U P A -1
H4B H 0.823502 0.206636 0.945861 0.179 Uiso 0.5 1 calc R U P A -1
C5 C 0.8835(10) 0.037(3) 0.9251(15) 0.156(5) Uani 0.5 1 d D U P A -1
H5A H 0.858161 0.029187 0.855498 0.188 Uiso 0.5 1 calc R U P A -1
H5B H 0.894203 -0.059282 0.951744 0.188 Uiso 0.5 1 calc R U P A -1
C6 C 0.9531(12) 0.121(3) 0.937(2) 0.196(9) Uani 0.5 1 d D U P A -1
H6A H 0.982352 0.071938 0.902940 0.294 Uiso 0.5 1 calc R U P A -1
H6B H 0.942248 0.216599 0.910154 0.294 Uiso 0.5 1 calc R U P A -1
H6C H 0.978197 0.128360 1.006149 0.294 Uiso 0.5 1 calc R U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O12 2.032(6) . ?
Ni1 O3 2.042(5) . ?
Ni1 O10 2.066(4) . ?
Ni1 O10 2.066(4) 6_565 ?
Ni1 O11 2.075(4) 6_565 ?
Ni1 O11 2.075(4) . ?
V1 O3 1.647(5) . ?
V1 O2 1.806(4) . ?
V1 O2 1.806(4) 6_565 ?
V1 O8 2.015(4) 5_666 ?
V1 O8 2.015(4) 2_656 ?
V1 O1 2.221(5) . ?
V1 V3 3.0994(19) 5_666 ?
V1 V2 3.1132(15) 6_565 ?
V1 V2 3.1132(15) . ?
V2 O7 1.593(4) . ?
V2 O6 1.816(3) . ?
V2 O4 1.881(4) . ?
V2 O2 1.890(4) . ?
V2 O5 2.061(4) . ?
V2 O1 2.337(4) . ?
V2 V2 3.054(2) 6_565 ?
V2 V4 3.0980(10) 5_666 ?
V2 V3 3.1127(14) . ?
V3 O9 1.595(5) . ?
V3 O4 1.826(4) 6_565 ?
V3 O4 1.826(4) . ?
V3 O8 2.010(4) . ?
V3 O8 2.010(4) 6_565 ?
V3 O1 2.258(5) . ?
V4 O5 1.695(4) 6_565 ?
V4 O5 1.695(4) 5_666 ?
V4 O8 1.919(3) 2_656 ?
V4 O8 1.919(3) . ?
V4 O1 2.100(3) . ?
V4 O1 2.100(3) 5_666 ?
N1 C1 1.388(9) . ?
N1 C3 1.415(9) . ?
N1 C4 1.443(10) . ?
N2 C2 1.387(9) . ?
N2 C1 1.394(9) . ?
N2 H2 0.8600 . ?
O10 H10C 0.8500 . ?
O10 H10D 0.8499 . ?
O11 H11C 0.8500 . ?
O11 H11D 0.8501 . ?
O11 H11A 0.8500 . ?
O12 H12 0.8500 . ?
O12 H12 0.8501 6_565 ?
O13 H13C 0.8500 . ?
O13 H13D 0.8500 . ?
O13 H13B 0.8500 . ?
C1 H1 0.9300 . ?
C2 C3 1.407(10) . ?
C2 H2A 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.508(10) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.529(10) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 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
O12 Ni1 O3 175.9(2) . . ?
O12 Ni1 O10 86.61(18) . . ?
O3 Ni1 O10 90.57(15) . . ?
O12 Ni1 O10 86.61(18) . 6_565 ?
O3 Ni1 O10 90.57(15) . 6_565 ?
O10 Ni1 O10 91.7(2) . 6_565 ?
O12 Ni1 O11 91.72(18) . 6_565 ?
O3 Ni1 O11 91.19(15) . 6_565 ?
O10 Ni1 O11 177.62(16) . 6_565 ?
O10 Ni1 O11 89.87(17) 6_565 6_565 ?
O12 Ni1 O11 91.72(18) . . ?
O3 Ni1 O11 91.18(15) . . ?
O10 Ni1 O11 89.87(17) . . ?
O10 Ni1 O11 177.62(16) 6_565 . ?
O11 Ni1 O11 88.5(2) 6_565 . ?
O3 V1 O2 103.31(17) . . ?
O3 V1 O2 103.31(17) . 6_565 ?
O2 V1 O2 95.8(2) . 6_565 ?
O3 V1 O8 98.83(18) . 5_666 ?
O2 V1 O8 89.85(16) . 5_666 ?
O2 V1 O8 155.16(16) 6_565 5_666 ?
O3 V1 O8 98.83(18) . 2_656 ?
O2 V1 O8 155.16(16) . 2_656 ?
O2 V1 O8 89.85(16) 6_565 2_656 ?
O8 V1 O8 75.6(2) 5_666 2_656 ?
O3 V1 O1 173.0(2) . . ?
O2 V1 O1 81.26(15) . . ?
O2 V1 O1 81.26(15) 6_565 . ?
O8 V1 O1 75.72(15) 5_666 . ?
O8 V1 O1 75.72(15) 2_656 . ?
O3 V1 V3 88.51(19) . 5_666 ?
O2 V1 V3 129.44(12) . 5_666 ?
O2 V1 V3 129.44(12) 6_565 5_666 ?
O8 V1 V3 39.59(11) 5_666 5_666 ?
O8 V1 V3 39.59(11) 2_656 5_666 ?
O1 V1 V3 84.51(14) . 5_666 ?
O3 V1 V2 136.59(14) . 6_565 ?
O2 V1 V2 83.91(13) . 6_565 ?
O2 V1 V2 33.46(12) 6_565 6_565 ?
O8 V1 V2 124.20(11) 5_666 6_565 ?
O8 V1 V2 87.74(11) 2_656 6_565 ?
O1 V1 V2 48.51(11) . 6_565 ?
V3 V1 V2 120.00(4) 5_666 6_565 ?
O3 V1 V2 136.59(14) . . ?
O2 V1 V2 33.46(12) . . ?
O2 V1 V2 83.91(13) 6_565 . ?
O8 V1 V2 87.74(11) 5_666 . ?
O8 V1 V2 124.20(11) 2_656 . ?
O1 V1 V2 48.51(11) . . ?
V3 V1 V2 120.00(4) 5_666 . ?
V2 V1 V2 58.76(4) 6_565 . ?
O7 V2 O6 104.8(2) . . ?
O7 V2 O4 101.9(2) . . ?
O6 V2 O4 92.0(2) . . ?
O7 V2 O2 102.5(2) . . ?
O6 V2 O2 91.7(2) . . ?
O4 V2 O2 153.45(18) . . ?
O7 V2 O5 99.8(2) . . ?
O6 V2 O5 155.40(19) . . ?
O4 V2 O5 83.18(16) . . ?
O2 V2 O5 82.58(16) . . ?
O7 V2 O1 173.2(2) . . ?
O6 V2 O1 81.97(16) . . ?
O4 V2 O1 78.02(16) . . ?
O2 V2 O1 76.50(16) . . ?
O5 V2 O1 73.43(15) . . ?
O7 V2 V2 137.54(17) . 6_565 ?
O6 V2 V2 32.77(14) . 6_565 ?
O4 V2 V2 84.68(12) . 6_565 ?
O2 V2 V2 84.31(12) . 6_565 ?
O5 V2 V2 122.63(11) . 6_565 ?
O1 V2 V2 49.20(9) . 6_565 ?
O7 V2 V4 130.60(17) . 5_666 ?
O6 V2 V4 124.63(14) . 5_666 ?
O4 V2 V4 78.49(12) . 5_666 ?
O2 V2 V4 77.80(12) . 5_666 ?
O5 V2 V4 30.77(11) . 5_666 ?
O1 V2 V4 42.67(9) . 5_666 ?
V2 V2 V4 91.86(3) 6_565 5_666 ?
O7 V2 V3 134.21(16) . . ?
O6 V2 V3 81.80(16) . . ?
O4 V2 V3 32.35(12) . . ?
O2 V2 V3 122.80(12) . . ?
O5 V2 V3 81.31(11) . . ?
O1 V2 V3 46.31(12) . . ?
V2 V2 V3 60.62(2) 6_565 . ?
V4 V2 V3 61.38(3) 5_666 . ?
O7 V2 V1 134.22(16) . . ?
O6 V2 V1 81.69(15) . . ?
O4 V2 V1 123.39(12) . . ?
O2 V2 V1 31.78(12) . . ?
O5 V2 V1 80.98(11) . . ?
O1 V2 V1 45.37(12) . . ?
V2 V2 V1 60.62(2) 6_565 . ?
V4 V2 V1 61.17(3) 5_666 . ?
V3 V2 V1 91.43(4) . . ?
O9 V3 O4 103.06(18) . 6_565 ?
O9 V3 O4 103.06(18) . . ?
O4 V3 O4 95.6(3) 6_565 . ?
O9 V3 O8 99.54(19) . . ?
O4 V3 O8 89.70(16) 6_565 . ?
O4 V3 O8 154.92(17) . . ?
O9 V3 O8 99.54(19) . 6_565 ?
O4 V3 O8 154.92(17) 6_565 6_565 ?
O4 V3 O8 89.70(16) . 6_565 ?
O8 V3 O8 75.9(2) . 6_565 ?
O9 V3 O1 173.5(3) . . ?
O4 V3 O1 81.23(15) 6_565 . ?
O4 V3 O1 81.23(15) . . ?
O8 V3 O1 75.37(15) . . ?
O8 V3 O1 75.37(15) 6_565 . ?
O9 V3 V1 89.4(2) . 5_666 ?
O4 V3 V1 129.41(13) 6_565 5_666 ?
O4 V3 V1 129.41(13) . 5_666 ?
O8 V3 V1 39.72(11) . 5_666 ?
O8 V3 V1 39.72(11) 6_565 5_666 ?
O1 V3 V1 84.09(14) . 5_666 ?
O9 V3 V2 136.33(15) . 6_565 ?
O4 V3 V2 33.46(11) 6_565 6_565 ?
O4 V3 V2 83.85(12) . 6_565 ?
O8 V3 V2 87.31(10) . 6_565 ?
O8 V3 V2 123.80(11) 6_565 6_565 ?
O1 V3 V2 48.44(10) . 6_565 ?
V1 V3 V2 119.58(4) 5_666 6_565 ?
O9 V3 V2 136.33(15) . . ?
O4 V3 V2 83.85(13) 6_565 . ?
O4 V3 V2 33.46(11) . . ?
O8 V3 V2 123.80(11) . . ?
O8 V3 V2 87.31(10) 6_565 . ?
O1 V3 V2 48.44(10) . . ?
V1 V3 V2 119.58(4) 5_666 . ?
V2 V3 V2 58.77(4) 6_565 . ?
O5 V4 O5 106.8(3) 6_565 5_666 ?
O5 V4 O8 97.09(16) 6_565 2_656 ?
O5 V4 O8 96.90(16) 5_666 2_656 ?
O5 V4 O8 96.90(16) 6_565 . ?
O5 V4 O8 97.10(16) 5_666 . ?
O8 V4 O8 156.4(2) 2_656 . ?
O5 V4 O1 87.41(17) 6_565 . ?
O5 V4 O1 165.78(19) 5_666 . ?
O8 V4 O1 80.66(17) 2_656 . ?
O8 V4 O1 81.12(17) . . ?
O5 V4 O1 165.78(19) 6_565 5_666 ?
O5 V4 O1 87.41(17) 5_666 5_666 ?
O8 V4 O1 81.12(17) 2_656 5_666 ?
O8 V4 O1 80.66(17) . 5_666 ?
O1 V4 O1 78.4(2) . 5_666 ?
O5 V4 V2 145.27(15) 6_565 5_666 ?
O5 V4 V2 38.46(14) 5_666 5_666 ?
O8 V4 V2 89.34(10) 2_656 5_666 ?
O8 V4 V2 89.90(10) . 5_666 ?
O1 V4 V2 127.32(12) . 5_666 ?
O1 V4 V2 48.95(11) 5_666 5_666 ?
O5 V4 V2 38.46(14) 6_565 6_565 ?
O5 V4 V2 145.27(15) 5_666 6_565 ?
O8 V4 V2 89.90(10) 2_656 6_565 ?
O8 V4 V2 89.34(10) . 6_565 ?
O1 V4 V2 48.95(11) . 6_565 ?
O1 V4 V2 127.32(12) 5_666 6_565 ?
V2 V4 V2 176.27(6) 5_666 6_565 ?
C1 N1 C3 107.7(9) . . ?
C1 N1 C4 129.5(11) . . ?
C3 N1 C4 122.8(10) . . ?
C2 N2 C1 110.1(9) . . ?
C2 N2 H2 124.9 . . ?
C1 N2 H2 124.9 . . ?
V4 O1 V4 101.6(2) 5_666 . ?
V4 O1 V1 93.96(16) 5_666 . ?
V4 O1 V1 93.96(16) . . ?
V4 O1 V3 93.24(15) 5_666 . ?
V4 O1 V3 93.24(15) . . ?
V1 O1 V3 168.6(3) . . ?
V4 O1 V2 170.0(2) 5_666 6_565 ?
V4 O1 V2 88.38(4) . 6_565 ?
V1 O1 V2 86.12(15) . 6_565 ?
V3 O1 V2 85.25(16) . 6_565 ?
V4 O1 V2 88.38(4) 5_666 . ?
V4 O1 V2 170.0(2) . . ?
V1 O1 V2 86.12(15) . . ?
V3 O1 V2 85.25(16) . . ?
V2 O1 V2 81.60(18) 6_565 . ?
V1 O2 V2 114.76(19) . . ?
V1 O3 Ni1 177.1(3) . . ?
V3 O4 V2 114.18(19) . . ?
V4 O5 V2 110.8(2) 5_666 . ?
V2 O6 V2 114.5(3) . 6_565 ?
V4 O8 V3 107.55(16) . . ?
V4 O8 V1 106.86(17) . 5_666 ?
V3 O8 V1 100.69(17) . 5_666 ?
Ni1 O10 H10C 111.0 . . ?
Ni1 O10 H10D 114.7 . . ?
H10C O10 H10D 108.2 . . ?
Ni1 O11 H11C 119.1 . . ?
Ni1 O11 H11D 111.2 . . ?
H11C O11 H11D 108.2 . . ?
Ni1 O11 H11A 98.6 . . ?
H11C O11 H11A 109.7 . . ?
H11D O11 H11A 109.6 . . ?
Ni1 O12 H12 123.9 . . ?
Ni1 O12 H12 123.94(4) . 6_565 ?
H12 O12 H12 108.1 . 6_565 ?
H13C O13 H13D 108.8 . . ?
H13C O13 H13B 116.9 . . ?
N1 C1 N2 107.5(9) . . ?
N1 C1 H1 126.3 . . ?
N2 C1 H1 126.3 . . ?
N2 C2 C3 106.3(9) . . ?
N2 C2 H2A 126.8 . . ?
C3 C2 H2A 126.8 . . ?
C2 C3 N1 108.4(9) . . ?
C2 C3 H3 125.8 . . ?
N1 C3 H3 125.8 . . ?
N1 C4 C5 118.9(12) . . ?
N1 C4 H4A 107.6 . . ?
C5 C4 H4A 107.6 . . ?
N1 C4 H4B 107.6 . . ?
C5 C4 H4B 107.6 . . ?
H4A C4 H4B 107.0 . . ?
C4 C5 C6 109.5(14) . . ?
C4 C5 H5A 109.8 . . ?
C6 C5 H5A 109.8 . . ?
C4 C5 H5B 109.8 . . ?
C6 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.4 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_refine_diff_density_max         1.580
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.157

