# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2022

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

data_mr1157
_database_code_depnum_ccdc_archive 'CCDC 2128841'
loop_
_audit_author_name
_audit_author_address
'Christian Nather'
;University of Kiel
Germany
;
_audit_update_record             
;
2021-12-15 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H48 As8 N12 Ni2 O26 V6'
_chemical_formula_weight         1799.04

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'
Ni Ni 0.3393 1.1124 '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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_H-M_alt        'I 41/a c d'
_space_group_name_Hall           '-I 4bd 2c'

_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, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   20.3058(5)
_cell_length_b                   20.3058(5)
_cell_length_c                   24.3847(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10054.4(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    33243
_cell_measurement_theta_min      2.393
_cell_measurement_theta_max      26.004

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.377
_exptl_crystal_F_000             6960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    7.109
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.2530
_exptl_absorpt_correction_T_max  0.4475
_exptl_absorpt_process_details   'X-Red and X-Shape (STOE, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS-2'
_diffrn_measurement_method       'Omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33243
_diffrn_reflns_av_unetI/netI     0.0275
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.393
_diffrn_reflns_theta_max         26.004
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2477
_reflns_number_gt                2245
_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       'X-AREA (STOE, 2008)'
_computing_cell_refinement       'X-AREA (STOE, 2008)'
_computing_data_reduction        'X-AREA (STOE, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_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)+(0.0348P)²+25.0415P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2477
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0950
_refine_ls_wR_factor_gt          0.0917
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_restrained_S_all      1.198
_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
As1 As 0.65814(2) 0.80757(3) 0.44612(2) 0.05474(16) Uani 1 1 d . . . . .
As2 As 0.53970(3) 0.91250(2) 0.44802(2) 0.05476(16) Uani 1 1 d . . . . .
V1 V 0.59531(4) 0.85663(4) 0.32975(3) 0.0521(2) Uani 1 1 d . . . . .
V2 V 0.5000 0.7500 0.46719(5) 0.0490(3) Uani 1 2 d S T P . .
O1 O 0.66443(16) 0.83333(17) 0.37960(13) 0.0557(8) Uani 1 1 d . . . . .
O2 O 0.59117(16) 0.74878(16) 0.44081(13) 0.0546(8) Uani 1 1 d . . . . .
O3 O 0.60950(17) 0.87149(17) 0.47731(14) 0.0573(8) Uani 1 1 d . . . . .
O4 O 0.56511(17) 0.92276(16) 0.38103(13) 0.0548(8) Uani 1 1 d . . . . .
O5 O 0.48818(16) 0.84102(16) 0.44233(13) 0.0544(8) Uani 1 1 d . . . . .
O6 O 0.62906(18) 0.89664(18) 0.28077(14) 0.0601(9) Uani 1 1 d . . . . .
O7 O 0.5000 0.7500 0.5329(2) 0.0547(11) Uani 1 2 d S T P . .
Ni1 Ni 0.36048(3) 0.88952(3) 0.6250 0.0525(2) Uani 1 2 d S T P . .
N1 N 0.4461(2) 0.8756(2) 0.57698(17) 0.0589(10) Uani 1 1 d . . . . .
H1N H 0.4560 0.8319 0.5757 0.071 Uiso 1 1 calc R U . . .
H2N H 0.4382 0.8894 0.5421 0.071 Uiso 1 1 calc R U . . .
C1 C 0.5030(3) 0.9123(3) 0.5997(2) 0.0614(12) Uani 1 1 d . . . . .
H1A H 0.5048 0.9570 0.5834 0.074 Uiso 1 1 calc R U . . .
H1B H 0.5445 0.8891 0.5906 0.074 Uiso 1 1 calc R U . . .
C2 C 0.4955(3) 0.9173(3) 0.6610(2) 0.0583(12) Uani 1 1 d . . . . .
H2A H 0.5013 0.8734 0.6780 0.070 Uiso 1 1 calc R U . . .
H2B H 0.5294 0.9473 0.6762 0.070 Uiso 1 1 calc R U . . .
N2 N 0.4293(2) 0.9430(2) 0.67338(17) 0.0568(10) Uani 1 1 d . . . . .
H3N H 0.4271 0.9867 0.6652 0.068 Uiso 1 1 calc R U . . .
H4N H 0.4201 0.9377 0.7096 0.068 Uiso 1 1 calc R U . . .
N3 N 0.2783(2) 0.9203(2) 0.67248(19) 0.0646(11) Uani 1 1 d . . . . .
H5N H 0.2440 0.8923 0.6671 0.078 Uiso 1 1 calc R U . . .
H6N H 0.2890 0.9197 0.7087 0.078 Uiso 1 1 calc R U . . .
C3 C 0.2592(3) 0.9870(3) 0.6564(3) 0.0787(18) Uani 1 1 d . . . . .
H3A H 0.2894 1.0196 0.6730 0.094 Uiso 1 1 calc R U . . .
H3B H 0.2139 0.9966 0.6689 0.094 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
As1 O1 1.709(3) . ?
As1 O3 1.800(3) . ?
As1 O2 1.814(3) . ?
As2 O4 1.726(3) . ?
As2 O3 1.792(3) . ?
As2 O5 1.795(3) . ?
V1 O6 1.599(4) . ?
V1 O1 1.916(3) . ?
V1 O4 1.935(3) . ?
V1 O2 2.000(3) 28_656 ?
V1 O5 2.001(3) 19_576 ?
V2 O7 1.602(5) . ?
V2 O5 1.960(3) 10_564 ?
V2 O5 1.960(3) . ?
V2 O2 1.960(3) . ?
V2 O2 1.960(3) 10_564 ?
O2 V1 2.000(3) 19_576 ?
O5 V1 2.001(3) 28_656 ?
Ni1 N1 2.115(4) . ?
Ni1 N1 2.115(4) 8_666 ?
Ni1 N3 2.125(4) 8_666 ?
Ni1 N3 2.125(4) . ?
Ni1 N2 2.127(4) . ?
Ni1 N2 2.127(4) 8_666 ?
N1 C1 1.483(6) . ?
C1 C2 1.507(7) . ?
C2 N2 1.472(6) . ?
N3 C3 1.462(7) . ?
C3 C3 1.533(14) 8_666 ?

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
O1 As1 O3 102.79(16) . . ?
O1 As1 O2 100.94(16) . . ?
O3 As1 O2 95.36(15) . . ?
O4 As2 O3 101.36(16) . . ?
O4 As2 O5 101.46(15) . . ?
O3 As2 O5 96.66(15) . . ?
O6 V1 O1 106.59(17) . . ?
O6 V1 O4 105.43(17) . . ?
O1 V1 O4 89.64(15) . . ?
O6 V1 O2 107.57(16) . 28_656 ?
O1 V1 O2 145.09(14) . 28_656 ?
O4 V1 O2 88.18(14) . 28_656 ?
O6 V1 O5 107.85(17) . 19_576 ?
O1 V1 O5 87.99(14) . 19_576 ?
O4 V1 O5 145.88(14) . 19_576 ?
O2 V1 O5 74.92(14) 28_656 19_576 ?
O7 V2 O5 108.02(10) . 10_564 ?
O7 V2 O5 108.02(10) . . ?
O5 V2 O5 144.0(2) 10_564 . ?
O7 V2 O2 109.16(10) . . ?
O5 V2 O2 76.75(14) 10_564 . ?
O5 V2 O2 91.49(14) . . ?
O7 V2 O2 109.16(10) . 10_564 ?
O5 V2 O2 91.49(14) 10_564 10_564 ?
O5 V2 O2 76.75(14) . 10_564 ?
O2 V2 O2 141.7(2) . 10_564 ?
As1 O1 V1 128.53(19) . . ?
As1 O2 V2 132.55(18) . . ?
As1 O2 V1 121.92(17) . 19_576 ?
V2 O2 V1 104.05(15) . 19_576 ?
As2 O3 As1 126.92(19) . . ?
As2 O4 V1 128.52(18) . . ?
As2 O5 V2 131.87(18) . . ?
As2 O5 V1 123.12(17) . 28_656 ?
V2 O5 V1 104.02(15) . 28_656 ?
N1 Ni1 N1 94.9(3) . 8_666 ?
N1 Ni1 N3 92.61(18) . 8_666 ?
N1 Ni1 N3 170.55(18) 8_666 8_666 ?
N1 Ni1 N3 170.55(18) . . ?
N1 Ni1 N3 92.61(18) 8_666 . ?
N3 Ni1 N3 80.5(3) 8_666 . ?
N1 Ni1 N2 80.52(16) . . ?
N1 Ni1 N2 91.40(16) 8_666 . ?
N3 Ni1 N2 95.45(17) 8_666 . ?
N3 Ni1 N2 93.64(17) . . ?
N1 Ni1 N2 91.40(16) . 8_666 ?
N1 Ni1 N2 80.52(16) 8_666 8_666 ?
N3 Ni1 N2 93.64(17) 8_666 8_666 ?
N3 Ni1 N2 95.44(17) . 8_666 ?
N2 Ni1 N2 168.1(2) . 8_666 ?
C1 N1 Ni1 111.5(3) . . ?
N1 C1 C2 109.0(4) . . ?
N2 C2 C1 108.6(4) . . ?
C2 N2 Ni1 107.8(3) . . ?
C3 N3 Ni1 109.5(4) . . ?
N3 C3 C3 107.5(4) . 8_666 ?

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
N1 H1N O7 0.91 2.16 2.975(5) 149.2 .
N1 H2N O6 0.91 2.48 3.233(6) 139.9 28_656
N2 H3N O4 0.91 2.16 3.034(5) 159.9 17_676
N2 H4N O6 0.91 2.17 3.024(5) 156.5 22_656
N3 H5N O4 0.91 2.31 3.191(6) 163.9 32_455
N3 H6N O6 0.91 2.46 3.277(6) 148.8 22_656
C3 H3A O6 0.99 2.63 3.616(7) 178.2 17_676

_refine_diff_density_max         0.388
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.071

_shelxl_version_number           2014-3

