# Supplementary Information (SI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_aa_a
_database_code_depnum_ccdc_archive 'CCDC 2433919'
loop_
_audit_author_name
_audit_author_address
'Zongjing Xiao'
;Nanjing Normal University
China
;
_audit_update_record             
;
2025-03-25 deposited with the CCDC.	2025-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C72 H100 Cu4 I0 N4 O24'
_chemical_formula_weight         1659.71

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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'

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

_cell_length_a                   9.610(3)
_cell_length_b                   10.687(4)
_cell_length_c                   20.153(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2069.8(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    8676
_cell_measurement_theta_min      2.16
_cell_measurement_theta_max      26.92

_exptl_crystal_description       rod
_exptl_crystal_colour            blue-green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_F_000             868
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    1.086
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_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      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13114
_diffrn_reflns_av_unetI/netI     0.0100
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.021
_diffrn_reflns_theta_max         27.003
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1265
_reflns_number_gt                1208
_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-2014/7 (Sheldrick, 2014)'
_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)+(0.0444P)²+1.1917P] 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         1265
_refine_ls_number_parameters     162
_refine_ls_number_restraints     143
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0211
_refine_ls_wR_factor_ref         0.0613
_refine_ls_wR_factor_gt          0.0597
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.054
_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
Cu1 Cu 0.63711(3) 0.5000 0.5000 0.01703(11) Uani 1 4 d S TU P C .
O2 O 0.61509(14) 0.31831(13) 0.5000 0.0446(4) Uani 1 2 d S TU P . .
O3 O 0.61509(15) 0.5000 0.40293(7) 0.0464(4) Uani 1 2 d S TU P . .
O005 O 0.5000 0.39706(17) 0.06516(8) 0.0688(6) Uani 1 2 d S TU P . .
H005 H 0.5000 0.4090 0.0250 0.103 Uiso 0.5 2 calc R U P . .
C6 C 0.5000 0.2647(2) 0.5000 0.0250(5) Uani 1 4 d S TU P B .
C22 C 0.5000 0.1219(2) 0.5000 0.0260(5) Uani 1 4 d S TU P . .
C11 C 0.5000 0.5000 0.37459(12) 0.0285(5) Uani 1 4 d S TU P A .
C12 C 0.5000 0.5000 0.29892(13) 0.0327(6) Uani 1 4 d S TU P . .
C11A C 0.4594(8) 0.6262(8) 0.2743(4) 0.045(2) Uani 0.25 1 d . U P A -1
H11A H 0.5248 0.6878 0.2910 0.054 Uiso 0.25 1 calc R U P A -1
H11B H 0.3679 0.6472 0.2913 0.054 Uiso 0.25 1 calc R U P A -1
C11B C 0.6435(8) 0.4622(8) 0.2702(4) 0.044(2) Uani 0.25 1 d . U P A -1
H11C H 0.7142 0.5200 0.2857 0.053 Uiso 0.25 1 calc R U P A -1
H11D H 0.6680 0.3790 0.2855 0.053 Uiso 0.25 1 calc R U P A -1
C11C C 0.3922(9) 0.4006(9) 0.2723(4) 0.0391(19) Uani 0.25 1 d . U P A -1
H11E H 0.4196 0.3175 0.2865 0.047 Uiso 0.25 1 calc R U P A -1
H11F H 0.3007 0.4182 0.2904 0.047 Uiso 0.25 1 calc R U P A -1
C12A C 0.3867(10) 0.4056(9) 0.1963(4) 0.042(2) Uani 0.25 1 d . U P A -1
H12A H 0.2950 0.4325 0.1820 0.051 Uiso 0.25 1 calc R U P A -1
H12B H 0.4038 0.3230 0.1782 0.051 Uiso 0.25 1 calc R U P A -1
C12B C 0.6379(10) 0.4642(8) 0.1939(5) 0.044(2) Uani 0.25 1 d . U P A -1
H12C H 0.7065 0.5229 0.1773 0.053 Uiso 0.25 1 calc R U P A -1
H12D H 0.6613 0.3818 0.1771 0.053 Uiso 0.25 1 calc R U P A -1
C12C C 0.4569(9) 0.6316(7) 0.1979(4) 0.048(2) Uani 0.25 1 d . U P A -1
H12E H 0.5212 0.6951 0.1823 0.058 Uiso 0.25 1 calc R U P A -1
H12F H 0.3643 0.6533 0.1826 0.058 Uiso 0.25 1 calc R U P A -1
C13A C 0.4618(9) 0.0714(12) 0.5653(7) 0.037(4) Uani 0.25 1 d . U P B -1
H13B H 0.5274 0.1003 0.5978 0.056 Uiso 0.25 1 d R U P B -1
H13C H 0.3703 0.1003 0.5768 0.056 Uiso 0.25 1 d R U P B -1
C13B C 0.4016(13) 0.0725(9) 0.4456(6) 0.038(3) Uani 0.25 1 d . U P B -1
H13E H 0.3095 0.1021 0.4552 0.057 Uiso 0.25 1 d R U P B -1
H13F H 0.4296 0.1021 0.4026 0.057 Uiso 0.25 1 d R U P B -1
C13C C 0.6491(7) 0.0718(7) 0.4814(5) 0.042(3) Uani 0.25 1 d . U P B -1
H13H H 0.6746 0.1012 0.4381 0.064 Uiso 0.25 1 d R U P B -1
H13I H 0.7154 0.1012 0.5134 0.064 Uiso 0.25 1 d R U P B -1
C17 C 0.5000 0.5000 0.16969(13) 0.0395(7) Uani 1 4 d S TU P . .
C18 C 0.5000 0.5000 0.09467(14) 0.0411(7) Uani 1 4 d S TU P A .
N1 N 0.86598(19) 0.5000 0.5000 0.0216(4) Uani 1 4 d DS TU P . .
C24 C 0.9189(10) 0.6243(6) 0.4836(4) 0.041(4) Uani 0.25 1 d D U P C -1
H24A H 0.8851 0.6848 0.5156 0.049 Uiso 0.25 1 d R U P C -1
H24B H 0.8851 0.6486 0.4401 0.049 Uiso 0.25 1 d R U P C -1
C25 C 0.9213(11) 0.4602(8) 0.5652(3) 0.037(3) Uani 0.25 1 d D U P C -1
H25A H 0.8874 0.3775 0.5766 0.044 Uiso 0.25 1 d R U P C -1
H25B H 0.8874 0.5188 0.5982 0.044 Uiso 0.25 1 d R U P C -1
C23 C 0.9195(9) 0.4076(6) 0.4517(4) 0.035(3) Uani 0.25 1 d D U P C -1
H23A H 0.8854 0.4301 0.4080 0.043 Uiso 0.25 1 d R U P C -1
H23B H 0.8854 0.3246 0.4624 0.043 Uiso 0.25 1 d R U P C -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
Cu1 O2 1.9532(15) . ?
Cu1 O2 1.9532(15) 11_565 ?
Cu1 O3 1.9676(16) . ?
Cu1 O3 1.9677(16) 10_556 ?
Cu1 N1 2.199(2) . ?
Cu1 Cu1 2.6352(10) 9_666 ?
O2 C6 1.2455(17) . ?
O3 C11 1.2448(18) . ?
O005 C18 1.251(2) . ?
O005 H005 0.8200 . ?
C6 O2 1.2455(17) 3_656 ?
C6 C22 1.527(3) . ?
C22 C13A 1.469(15) . ?
C22 C13B 1.541(13) . ?
C22 C13C 1.575(7) . ?
C11 O3 1.2448(18) 2_665 ?
C11 C12 1.525(3) . ?
C12 C11A 1.489(9) . ?
C12 C11B 1.549(8) . ?
C12 C11C 1.578(9) . ?
C11A C12C 1.542(10) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C11B C12B 1.539(11) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C11C C12A 1.534(12) . ?
C11C H11E 0.9700 . ?
C11C H11F 0.9700 . ?
C12A C17 1.578(10) . ?
C12A H12A 0.9700 . ?
C12A H12B 0.9700 . ?
C12B C17 1.464(9) . ?
C12B H12C 0.9700 . ?
C12B H12D 0.9700 . ?
C12C C17 1.572(8) . ?
C12C H12E 0.9700 . ?
C12C H12F 0.9700 . ?
C13A H13B 0.9600 . ?
C13A H13C 0.9599 . ?
C13B H13E 0.9600 . ?
C13B H13F 0.9599 . ?
C13C H13H 0.9600 . ?
C13C H13I 0.9600 . ?
C17 C18 1.512(4) . ?
C18 O005 1.251(2) 11_565 ?
N1 C24 1.460(6) . ?
N1 C23 1.480(6) . ?
N1 C25 1.479(6) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9701 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9699 . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Cu1 O2 167.56(8) . 11_565 ?
O2 Cu1 O3 89.333(7) . . ?
O2 Cu1 O3 89.333(7) 11_565 . ?
O2 Cu1 O3 89.333(7) . 10_556 ?
O2 Cu1 O3 89.333(7) 11_565 10_556 ?
O3 Cu1 O3 167.66(9) . 10_556 ?
O2 Cu1 N1 96.22(4) . . ?
O2 Cu1 N1 96.22(4) 11_565 . ?
O3 Cu1 N1 96.17(4) . . ?
O3 Cu1 N1 96.17(4) 10_556 . ?
O2 Cu1 Cu1 83.78(4) . 9_666 ?
O2 Cu1 Cu1 83.78(4) 11_565 9_666 ?
O3 Cu1 Cu1 83.83(4) . 9_666 ?
O3 Cu1 Cu1 83.83(4) 10_556 9_666 ?
N1 Cu1 Cu1 180.0 . 9_666 ?
C6 O2 Cu1 123.59(13) . . ?
C11 O3 Cu1 123.48(14) . . ?
C18 O005 H005 109.5 . . ?
O2 C6 O2 125.2(2) 3_656 . ?
O2 C6 C22 117.38(11) 3_656 . ?
O2 C6 C22 117.38(11) . . ?
C13A C22 C6 111.6(5) . . ?
C13A C22 C13B 111.0(6) . . ?
C6 C22 C13B 110.0(4) . . ?
C13A C22 C13C 108.4(4) . . ?
C6 C22 C13C 109.9(3) . . ?
C13B C22 C13C 105.8(6) . . ?
O3 C11 O3 125.4(2) . 2_665 ?
O3 C11 C12 117.31(12) . . ?
O3 C11 C12 117.31(12) 2_665 . ?
C11A C12 C11 109.4(3) . . ?
C11A C12 C11B 110.2(4) . . ?
C11 C12 C11B 111.9(3) . . ?
C11A C12 C11C 108.9(5) . . ?
C11 C12 C11C 109.9(3) . . ?
C11B C12 C11C 106.4(5) . . ?
C12 C11A C12C 111.7(6) . . ?
C12 C11A H11A 109.3 . . ?
C12C C11A H11A 109.3 . . ?
C12 C11A H11B 109.3 . . ?
C12C C11A H11B 109.3 . . ?
H11A C11A H11B 107.9 . . ?
C12B C11B C12 109.8(6) . . ?
C12B C11B H11C 109.7 . . ?
C12 C11B H11C 109.7 . . ?
C12B C11B H11D 109.7 . . ?
C12 C11B H11D 109.7 . . ?
H11C C11B H11D 108.2 . . ?
C12A C11C C12 109.8(6) . . ?
C12A C11C H11E 109.7 . . ?
C12 C11C H11E 109.7 . . ?
C12A C11C H11F 109.7 . . ?
C12 C11C H11F 109.7 . . ?
H11E C11C H11F 108.2 . . ?
C11C C12A C17 109.7(6) . . ?
C11C C12A H12A 109.7 . . ?
C17 C12A H12A 109.7 . . ?
C11C C12A H12B 109.7 . . ?
C17 C12A H12B 109.7 . . ?
H12A C12A H12B 108.2 . . ?
C17 C12B C11B 111.6(6) . . ?
C17 C12B H12C 109.3 . . ?
C11B C12B H12C 109.3 . . ?
C17 C12B H12D 109.3 . . ?
C11B C12B H12D 109.3 . . ?
H12C C12B H12D 108.0 . . ?
C11A C12C C17 108.9(6) . . ?
C11A C12C H12E 109.9 . . ?
C17 C12C H12E 109.9 . . ?
C11A C12C H12F 109.9 . . ?
C17 C12C H12F 109.9 . . ?
H12E C12C H12F 108.3 . . ?
C22 C13A H13B 109.2 . . ?
C22 C13A H13C 109.1 . . ?
H13B C13A H13C 109.5 . . ?
C22 C13B H13E 108.0 . . ?
C22 C13B H13F 110.9 . . ?
H13E C13B H13F 109.5 . . ?
C22 C13C H13H 109.7 . . ?
C22 C13C H13I 109.4 . . ?
H13H C13C H13I 109.5 . . ?
C12B C17 C18 109.5(4) . . ?
C12B C17 C12C 110.6(4) . . ?
C18 C17 C12C 111.2(3) . . ?
C12B C17 C12A 110.1(5) . . ?
C18 C17 C12A 109.8(3) . . ?
C12C C17 C12A 105.5(5) . . ?
O005 C18 O005 123.2(3) . 11_565 ?
O005 C18 C17 118.39(14) . . ?
O005 C18 C17 118.39(14) 11_565 . ?
C24 N1 C23 109.7(5) . . ?
C24 N1 C25 109.7(4) . . ?
C23 N1 C25 105.5(6) . . ?
C24 N1 Cu1 110.4(4) . . ?
C23 N1 Cu1 110.4(3) . . ?
C25 N1 Cu1 111.1(4) . . ?
N1 C24 H24A 109.8 . . ?
N1 C24 H24B 109.4 . . ?
H24A C24 H24B 108.2 . . ?
N1 C25 H25A 110.6 . . ?
N1 C25 H25B 107.6 . . ?
H25A C25 H25B 108.2 . . ?
N1 C23 H23A 108.4 . . ?
N1 C23 H23B 110.3 . . ?
H23A C23 H23B 108.3 . . ?

_refine_diff_density_max         0.374
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.046

####################################################################### 
# 
# 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_NNM_1_Ni_a
_database_code_depnum_ccdc_archive 'CCDC 2433920'
loop_
_audit_author_name
_audit_author_address
'Zongjing Xiao'
;Nanjing Normal University
China
;
_audit_update_record             
;
2025-03-25 deposited with the CCDC.	2025-06-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H50 I0 N2 Ni2 O12'
_chemical_formula_weight         820.20

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'
Ni Ni 0.3393 1.1124 '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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'

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

_cell_length_a                   9.339(2)
_cell_length_b                   10.761(3)
_cell_length_c                   20.275(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2037.6(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4132
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      24.13

_exptl_crystal_description       rod
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.983
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_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      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12537
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.009
_diffrn_reflns_theta_max         25.872
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1140
_reflns_number_gt                1055
_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-2014/7 (Sheldrick, 2014)'
_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)+(0.0444P)²+1.1917P] 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         1140
_refine_ls_number_parameters     162
_refine_ls_number_restraints     137
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0225
_refine_ls_wR_factor_ref         0.0604
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_restrained_S_all      0.967
_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 0.64092(3) 0.5000 0.5000 0.01581(13) Uani 1 4 d S TU P C .
O2 O 0.61796(16) 0.31665(15) 0.5000 0.0462(5) Uani 1 2 d S TU P . .
O3 O 0.61819(16) 0.5000 0.40167(8) 0.0469(5) Uani 1 2 d S TU P . .
O005 O 0.5000 0.39693(18) 0.06495(8) 0.0556(6) Uani 1 2 d S TU P . .
H005 H 0.5000 0.4090 0.0250 0.083 Uiso 0.5 2 calc R U P . .
C6 C 0.5000 0.2628(3) 0.5000 0.0241(6) Uani 1 4 d S TU P B .
C22 C 0.5000 0.1212(3) 0.5000 0.0241(6) Uani 1 4 d S TU P . .
C11 C 0.5000 0.5000 0.37336(14) 0.0272(6) Uani 1 4 d S TU P A .
C12 C 0.5000 0.5000 0.29775(14) 0.0301(7) Uani 1 4 d S TU P . .
C11A C 0.4573(9) 0.6266(9) 0.2737(5) 0.041(2) Uani 0.25 1 d . U P A -1
H11A H 0.5240 0.6881 0.2905 0.049 Uiso 0.25 1 calc R U P A -1
H11B H 0.3627 0.6469 0.2902 0.049 Uiso 0.25 1 calc R U P A -1
C11B C 0.6478(9) 0.4612(8) 0.2694(4) 0.039(2) Uani 0.25 1 d . U P A -1
H11C H 0.7212 0.5175 0.2854 0.047 Uiso 0.25 1 calc R U P A -1
H11D H 0.6716 0.3780 0.2842 0.047 Uiso 0.25 1 calc R U P A -1
C11C C 0.3905(10) 0.4021(9) 0.2715(5) 0.037(2) Uani 0.25 1 d . U P A -1
H11E H 0.4192 0.3196 0.2855 0.045 Uiso 0.25 1 calc R U P A -1
H11F H 0.2964 0.4190 0.2897 0.045 Uiso 0.25 1 calc R U P A -1
C12A C 0.3842(11) 0.4078(9) 0.1955(5) 0.036(2) Uani 0.25 1 d . U P A -1
H12A H 0.2900 0.4350 0.1815 0.044 Uiso 0.25 1 calc R U P A -1
H12B H 0.4012 0.3257 0.1773 0.044 Uiso 0.25 1 calc R U P A -1
C12B C 0.6434(11) 0.4645(8) 0.1934(5) 0.039(3) Uani 0.25 1 d . U P A -1
H12C H 0.7135 0.5238 0.1773 0.047 Uiso 0.25 1 calc R U P A -1
H12D H 0.6684 0.3833 0.1761 0.047 Uiso 0.25 1 calc R U P A -1
C12C C 0.4565(9) 0.6306(8) 0.1975(4) 0.043(2) Uani 0.25 1 d . U P A -1
H12E H 0.5234 0.6931 0.1822 0.052 Uiso 0.25 1 calc R U P A -1
H12F H 0.3617 0.6528 0.1819 0.052 Uiso 0.25 1 calc R U P A -1
C13A C 0.4582(10) 0.0689(13) 0.5640(7) 0.031(4) Uani 0.25 1 d . U P B -1
H13B H 0.5238 0.0978 0.5964 0.047 Uiso 0.25 1 d R U P B -1
H13C H 0.3667 0.0978 0.5755 0.047 Uiso 0.25 1 d R U P B -1
C13B C 0.3974(12) 0.0731(11) 0.4450(7) 0.034(3) Uani 0.25 1 d . U P B -1
H13E H 0.3053 0.1027 0.4547 0.051 Uiso 0.25 1 d R U P B -1
H13F H 0.4254 0.1027 0.4020 0.051 Uiso 0.25 1 d R U P B -1
C13C C 0.6536(8) 0.0717(7) 0.4825(5) 0.038(3) Uani 0.25 1 d . U P B -1
H13H H 0.6791 0.1012 0.4392 0.056 Uiso 0.25 1 d R U P B -1
H13I H 0.7199 0.1012 0.5145 0.056 Uiso 0.25 1 d R U P B -1
C17 C 0.5000 0.5000 0.16936(14) 0.0362(7) Uani 1 4 d S TU P . .
C18 C 0.5000 0.5000 0.09476(15) 0.0371(8) Uani 1 4 d S TU P A .
N1 N 0.8614(2) 0.5000 0.5000 0.0189(5) Uani 1 4 d DS TU P . .
C24 C 0.9177(12) 0.6243(7) 0.4838(4) 0.037(4) Uani 0.25 1 d D U P C -1
H24A H 0.8840 0.6848 0.5159 0.044 Uiso 0.25 1 d R U P C -1
H24B H 0.8840 0.6486 0.4403 0.044 Uiso 0.25 1 d R U P C -1
C25 C 0.9186(12) 0.4595(8) 0.5650(4) 0.030(3) Uani 0.25 1 d D U P C -1
H25A H 0.8847 0.3768 0.5764 0.036 Uiso 0.25 1 d R U P C -1
H25B H 0.8847 0.5181 0.5980 0.036 Uiso 0.25 1 d R U P C -1
C23 C 0.9167(10) 0.4081(7) 0.4515(4) 0.030(3) Uani 0.25 1 d D U P C -1
H23A H 0.8826 0.4306 0.4078 0.036 Uiso 0.25 1 d R U P C -1
H23B H 0.8826 0.3251 0.4622 0.036 Uiso 0.25 1 d R U P C -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 O2 1.9846(16) . ?
Ni1 O2 1.9847(16) 11_565 ?
Ni1 O3 2.0049(16) . ?
Ni1 O3 2.0049(16) 10_556 ?
Ni1 N1 2.059(2) . ?
Ni1 Ni1 2.6322(9) 9_666 ?
O2 C6 1.2445(19) . ?
O3 C11 1.244(2) . ?
O005 C18 1.263(2) . ?
O005 H005 0.8200 . ?
C6 O2 1.2445(19) 3_656 ?
C6 C22 1.524(4) . ?
C22 C13A 1.467(15) . ?
C22 C13B 1.558(14) . ?
C22 C13C 1.570(7) . ?
C11 O3 1.244(2) 2_665 ?
C11 C12 1.533(4) . ?
C12 C11A 1.501(10) . ?
C12 C11B 1.552(8) . ?
C12 C11C 1.562(10) . ?
C11A C12C 1.545(11) . ?
C11A H11A 0.9700 . ?
C11A H11B 0.9700 . ?
C11B C12B 1.543(12) . ?
C11B H11C 0.9700 . ?
C11B H11D 0.9700 . ?
C11C C12A 1.544(13) . ?
C11C H11E 0.9700 . ?
C11C H11F 0.9700 . ?
C12A C17 1.560(11) . ?
C12A H12A 0.9700 . ?
C12A H12B 0.9700 . ?
C12B C17 1.475(10) . ?
C12B H12C 0.9700 . ?
C12B H12D 0.9700 . ?
C12C C17 1.570(8) . ?
C12C H12E 0.9700 . ?
C12C H12F 0.9700 . ?
C13A H13B 0.9518 . ?
C13A H13C 0.9383 . ?
C13B H13E 0.9380 . ?
C13B H13F 0.9633 . ?
C13C H13H 0.9638 . ?
C13C H13I 0.9516 . ?
C17 C18 1.512(4) . ?
C18 O005 1.263(2) 11_565 ?
N1 C24 1.475(7) . ?
N1 C25 1.487(6) . ?
N1 C23 1.487(6) . ?
C24 H24A 0.9726 . ?
C24 H24B 0.9724 . ?
C25 H25A 0.9728 . ?
C25 H25B 0.9725 . ?
C23 H23A 0.9722 . ?
C23 H23B 0.9728 . ?

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 167.59(9) . 11_565 ?
O2 Ni1 O3 89.344(7) . . ?
O2 Ni1 O3 89.344(7) 11_565 . ?
O2 Ni1 O3 89.344(7) . 10_556 ?
O2 Ni1 O3 89.344(7) 11_565 10_556 ?
O3 Ni1 O3 167.84(9) . 10_556 ?
O2 Ni1 N1 96.20(5) . . ?
O2 Ni1 N1 96.20(5) 11_565 . ?
O3 Ni1 N1 96.08(5) . . ?
O3 Ni1 N1 96.08(5) 10_556 . ?
O2 Ni1 Ni1 83.80(5) . 9_666 ?
O2 Ni1 Ni1 83.80(5) 11_565 9_666 ?
O3 Ni1 Ni1 83.92(5) . 9_666 ?
O3 Ni1 Ni1 83.92(5) 10_556 9_666 ?
N1 Ni1 Ni1 180.0 . 9_666 ?
C6 O2 Ni1 123.93(15) . . ?
C11 O3 Ni1 123.56(15) . . ?
C18 O005 H005 109.5 . . ?
O2 C6 O2 124.5(3) 3_656 . ?
O2 C6 C22 117.73(13) 3_656 . ?
O2 C6 C22 117.73(13) . . ?
C13A C22 C6 112.6(5) . . ?
C13A C22 C13B 110.0(5) . . ?
C6 C22 C13B 109.4(4) . . ?
C13A C22 C13C 108.2(4) . . ?
C6 C22 C13C 109.8(3) . . ?
C13B C22 C13C 106.7(6) . . ?
O3 C11 O3 125.0(3) 2_665 . ?
O3 C11 C12 117.48(13) 2_665 . ?
O3 C11 C12 117.48(13) . . ?
C11A C12 C11 109.0(4) . . ?
C11A C12 C11B 111.1(4) . . ?
C11 C12 C11B 111.7(3) . . ?
C11A C12 C11C 109.1(5) . . ?
C11 C12 C11C 109.9(4) . . ?
C11B C12 C11C 106.0(5) . . ?
C12 C11A C12C 110.6(7) . . ?
C12 C11A H11A 109.5 . . ?
C12C C11A H11A 109.5 . . ?
C12 C11A H11B 109.5 . . ?
C12C C11A H11B 109.5 . . ?
H11A C11A H11B 108.1 . . ?
C12B C11B C12 109.8(6) . . ?
C12B C11B H11C 109.7 . . ?
C12 C11B H11C 109.7 . . ?
C12B C11B H11D 109.7 . . ?
C12 C11B H11D 109.7 . . ?
H11C C11B H11D 108.2 . . ?
C12A C11C C12 109.8(7) . . ?
C12A C11C H11E 109.7 . . ?
C12 C11C H11E 109.7 . . ?
C12A C11C H11F 109.7 . . ?
C12 C11C H11F 109.7 . . ?
H11E C11C H11F 108.2 . . ?
C11C C12A C17 109.7(7) . . ?
C11C C12A H12A 109.7 . . ?
C17 C12A H12A 109.7 . . ?
C11C C12A H12B 109.7 . . ?
C17 C12A H12B 109.7 . . ?
H12A C12A H12B 108.2 . . ?
C17 C12B C11B 111.1(7) . . ?
C17 C12B H12C 109.4 . . ?
C11B C12B H12C 109.4 . . ?
C17 C12B H12D 109.4 . . ?
C11B C12B H12D 109.4 . . ?
H12C C12B H12D 108.0 . . ?
C11A C12C C17 109.7(6) . . ?
C11A C12C H12E 109.7 . . ?
C17 C12C H12E 109.7 . . ?
C11A C12C H12F 109.7 . . ?
C17 C12C H12F 109.7 . . ?
H12E C12C H12F 108.2 . . ?
C22 C13A H13B 108.4 . . ?
C22 C13A H13C 109.5 . . ?
H13B C13A H13C 107.8 . . ?
C22 C13B H13E 107.6 . . ?
C22 C13B H13F 111.8 . . ?
H13E C13B H13F 109.0 . . ?
C22 C13C H13H 108.7 . . ?
C22 C13C H13I 109.1 . . ?
H13H C13C H13I 110.5 . . ?
C12B C17 C18 109.3(4) . . ?
C12B C17 C12A 110.6(5) . . ?
C18 C17 C12A 109.8(4) . . ?
C12B C17 C12C 110.2(5) . . ?
C18 C17 C12C 111.3(3) . . ?
C12A C17 C12C 105.5(6) . . ?
O005 C18 O005 122.8(3) . 11_565 ?
O005 C18 C17 118.59(15) . . ?
O005 C18 C17 118.59(15) 11_565 . ?
C24 N1 C25 109.5(4) . . ?
C24 N1 C23 109.4(5) . . ?
C25 N1 C23 105.4(6) . . ?
C24 N1 Ni1 110.9(5) . . ?
C25 N1 Ni1 111.1(5) . . ?
C23 N1 Ni1 110.3(4) . . ?
N1 C24 H24A 110.1 . . ?
N1 C24 H24B 109.3 . . ?
H24A C24 H24B 108.8 . . ?
N1 C25 H25A 111.2 . . ?
N1 C25 H25B 107.6 . . ?
H25A C25 H25B 108.9 . . ?
N1 C23 H23A 108.9 . . ?
N1 C23 H23B 110.5 . . ?
H23A C23 H23B 108.9 . . ?

_refine_diff_density_max         0.325
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.044

