# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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. 
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#######################################################################

data_ni4
_database_code_depnum_ccdc_archive 'CCDC 2141266'
loop_
_audit_author_name
_audit_author_address
WT
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2022-01-11 deposited with the CCDC.	2022-04-18 downloaded from the CCDC.
;
_audit_creation_date             2022-01-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C48 H56 N44 Ni4'
_chemical_formula_sum            'C48 H56 N44 Ni4'
_chemical_formula_weight         1484.20
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_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'
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                   17.2932(4)
_cell_length_b                   17.2932(4)
_cell_length_c                   41.5378(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12422.1(7)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8471
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.00
_cell_measurement_theta_min      4.20
_shelx_estimated_absorpt_T_max   0.810
_shelx_estimated_absorpt_T_min   0.754
_exptl_absorpt_coefficient_mu    1.997
_exptl_absorpt_correction_T_max  0.1621
_exptl_absorpt_correction_T_min  0.0655
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0954 before and 0.0751 after correction. The Ratio of minimum to maximum transmission is 0.4041. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark black'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6112
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0939
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            42028
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.152
_diffrn_reflns_theta_max         65.152
_diffrn_reflns_theta_min         4.257
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2028
_reflns_number_total             2662
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.052
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         2662
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0429
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0576P)²+19.9274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1196
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.60590(3) 0.35590(3) 0.3750 0.0405(2) Uani 1 2 d S T P . .
Ni2 Ni 0.5000 0.2500 0.43427(2) 0.0424(2) Uani 1 2 d S T P . .
N5 N 0.50357(14) 0.34169(15) 0.34932(6) 0.0411(6) Uani 1 1 d . . . . .
N1 N 0.54753(14) 0.40756(14) 0.41295(6) 0.0413(6) Uani 1 1 d . . . . .
N6 N 0.57689(15) 0.52263(14) 0.39002(7) 0.0446(6) Uani 1 1 d . . . . .
N2 N 0.50460(14) 0.36567(15) 0.43458(6) 0.0424(6) Uani 1 1 d . . . . .
N9 N 0.61295(15) 0.47825(15) 0.36668(7) 0.0467(6) Uani 1 1 d . . . . .
N7 N 0.41631(15) 0.35919(16) 0.47540(7) 0.0479(7) Uani 1 1 d . . . . .
N8 N 0.42183(16) 0.28038(16) 0.47125(7) 0.0498(7) Uani 1 1 d . . . . .
N4 N 0.44874(16) 0.48138(16) 0.45577(7) 0.0498(7) Uani 1 1 d . . . . .
N3 N 0.49067(16) 0.52326(16) 0.43299(7) 0.0501(7) Uani 1 1 d . . . . .
N10 N 0.46102(19) 0.3960(2) 0.34526(8) 0.0678(9) Uani 1 1 d . . . . .
C7 C 0.45861(18) 0.40620(19) 0.45404(8) 0.0458(8) Uani 1 1 d . . . . .
C6 C 0.53489(18) 0.48306(17) 0.41361(8) 0.0435(7) Uani 1 1 d . . . . .
C2 C 0.6540(2) 0.5280(2) 0.34931(9) 0.0527(8) Uani 1 1 d . . . . .
C4 C 0.5961(2) 0.59977(18) 0.38706(9) 0.0514(8) Uani 1 1 d . . . . .
C11 C 0.3784(2) 0.2489(2) 0.49413(8) 0.0558(9) Uani 1 1 d . . . . .
C9 C 0.3690(2) 0.3767(2) 0.50065(9) 0.0526(8) Uani 1 1 d . . . . .
C5 C 0.5693(2) 0.6617(2) 0.40885(10) 0.0602(9) Uani 1 1 d . . . . .
H5A H 0.5143 0.6718 0.4050 0.090 Uiso 1 1 calc R U . . .
H5B H 0.5991 0.7090 0.4048 0.090 Uiso 1 1 calc R U . . .
H5C H 0.5768 0.6456 0.4312 0.090 Uiso 1 1 calc R U . . .
C3 C 0.6445(2) 0.6035(2) 0.36127(10) 0.0567(9) Uani 1 1 d . . . . .
H3 H 0.6678 0.6490 0.3529 0.068 Uiso 1 1 calc R U . . .
C1 C 0.7045(2) 0.5011(2) 0.32313(9) 0.0617(10) Uani 1 1 d . . . . .
H1A H 0.7580 0.4986 0.3309 0.093 Uiso 1 1 calc R U . . .
H1B H 0.7013 0.5372 0.3050 0.093 Uiso 1 1 calc R U . . .
H1C H 0.6879 0.4496 0.3161 0.093 Uiso 1 1 calc R U . . .
C10 C 0.3442(2) 0.3078(2) 0.51294(9) 0.0600(10) Uani 1 1 d . . . . .
H10 H 0.3105 0.3008 0.5307 0.072 Uiso 1 1 calc R U . . .
C8 C 0.3528(2) 0.4563(2) 0.51196(9) 0.0656(10) Uani 1 1 d . . . . .
H8A H 0.4017 0.4827 0.5167 0.098 Uiso 1 1 calc R U . . .
H8B H 0.3211 0.4542 0.5315 0.098 Uiso 1 1 calc R U . . .
H8C H 0.3250 0.4847 0.4952 0.098 Uiso 1 1 calc R U . . .
N11 N 0.4220(3) 0.4483(3) 0.34028(13) 0.128(2) Uani 1 1 d . . . . .
C12 C 0.3721(3) 0.1635(2) 0.49785(11) 0.0757(12) Uani 1 1 d . . . . .
H12A H 0.3721 0.1391 0.4766 0.114 Uiso 1 1 calc R U . . .
H12B H 0.3238 0.1508 0.5091 0.114 Uiso 1 1 calc R U . . .
H12C H 0.4161 0.1443 0.5104 0.114 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 N5 2.081(3) 7_545 ?
Ni1 N5 2.081(3) . ?
Ni1 N1 2.074(3) . ?
Ni1 N1 2.074(3) 7_545 ?
Ni1 N9 2.147(3) . ?
Ni1 N9 2.147(3) 7_545 ?
Ni2 N5 2.113(2) 7_545 ?
Ni2 N5 2.113(2) 16 ?
Ni2 N2 2.002(3) . ?
Ni2 N2 2.002(3) 10_554 ?
Ni2 N8 2.112(3) 10_554 ?
Ni2 N8 2.112(3) . ?
N5 Ni2 2.113(2) 7_545 ?
N5 N10 1.205(4) . ?
N1 N2 1.372(3) . ?
N1 C6 1.324(4) . ?
N6 N9 1.385(4) . ?
N6 C6 1.399(4) . ?
N6 C4 1.380(4) . ?
N2 C7 1.333(4) . ?
N9 C2 1.328(4) . ?
N7 N8 1.377(4) . ?
N7 C7 1.408(4) . ?
N7 C9 1.365(4) . ?
N8 C11 1.328(4) . ?
N4 N3 1.395(4) . ?
N4 C7 1.313(4) . ?
N3 C6 1.310(4) . ?
N10 N11 1.149(5) . ?
C2 C3 1.406(5) . ?
C2 C1 1.471(5) . ?
C4 C5 1.477(5) . ?
C4 C3 1.361(5) . ?
C11 C10 1.413(5) . ?
C11 C12 1.490(5) . ?
C9 C10 1.365(5) . ?
C9 C8 1.481(5) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C3 H3 0.9500 . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C10 H10 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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
N5 Ni1 N5 93.56(14) . 7_545 ?
N5 Ni1 N9 94.72(10) 7_545 7_545 ?
N5 Ni1 N9 94.71(10) . . ?
N5 Ni1 N9 157.99(10) . 7_545 ?
N5 Ni1 N9 157.99(10) 7_545 . ?
N1 Ni1 N5 85.37(10) 7_545 . ?
N1 Ni1 N5 91.53(10) 7_545 7_545 ?
N1 Ni1 N5 85.36(10) . 7_545 ?
N1 Ni1 N5 91.53(10) . . ?
N1 Ni1 N1 175.47(14) 7_545 . ?
N1 Ni1 N9 74.06(10) 7_545 7_545 ?
N1 Ni1 N9 109.44(10) . 7_545 ?
N1 Ni1 N9 109.43(10) 7_545 . ?
N1 Ni1 N9 74.07(10) . . ?
N9 Ni1 N9 85.06(14) 7_545 . ?
N5 Ni2 N5 97.36(14) 16 7_545 ?
N2 Ni2 N5 86.86(10) . 7_545 ?
N2 Ni2 N5 86.86(10) 10_554 16 ?
N2 Ni2 N5 93.63(10) . 16 ?
N2 Ni2 N5 93.63(10) 10_554 7_545 ?
N2 Ni2 N2 179.27(15) 10_554 . ?
N2 Ni2 N8 76.84(11) . . ?
N2 Ni2 N8 76.84(11) 10_554 10_554 ?
N2 Ni2 N8 102.61(11) . 10_554 ?
N2 Ni2 N8 102.62(11) 10_554 . ?
N8 Ni2 N5 162.37(10) . 7_545 ?
N8 Ni2 N5 162.37(10) 10_554 16 ?
N8 Ni2 N5 90.41(11) 10_554 7_545 ?
N8 Ni2 N5 90.41(11) . 16 ?
N8 Ni2 N8 86.71(16) . 10_554 ?
Ni1 N5 Ni2 116.87(12) . 7_545 ?
N10 N5 Ni1 120.0(2) . . ?
N10 N5 Ni2 118.3(2) . 7_545 ?
N2 N1 Ni1 122.24(19) . . ?
C6 N1 Ni1 121.4(2) . . ?
C6 N1 N2 114.7(3) . . ?
N9 N6 C6 116.9(2) . . ?
C4 N6 N9 111.4(3) . . ?
C4 N6 C6 131.3(3) . . ?
N1 N2 Ni2 123.01(19) . . ?
C7 N2 Ni2 120.4(2) . . ?
C7 N2 N1 116.2(3) . . ?
N6 N9 Ni1 114.08(19) . . ?
C2 N9 Ni1 139.1(2) . . ?
C2 N9 N6 105.1(3) . . ?
N8 N7 C7 117.2(3) . . ?
C9 N7 N8 111.0(3) . . ?
C9 N7 C7 131.9(3) . . ?
N7 N8 Ni2 112.4(2) . . ?
C11 N8 Ni2 141.3(3) . . ?
C11 N8 N7 106.0(3) . . ?
C7 N4 N3 114.2(3) . . ?
C6 N3 N4 116.4(3) . . ?
N11 N10 N5 177.3(5) . . ?
N2 C7 N7 112.9(3) . . ?
N4 C7 N2 129.1(3) . . ?
N4 C7 N7 118.0(3) . . ?
N1 C6 N6 112.5(3) . . ?
N3 C6 N1 129.2(3) . . ?
N3 C6 N6 118.3(3) . . ?
N9 C2 C3 110.3(3) . . ?
N9 C2 C1 120.9(3) . . ?
C3 C2 C1 128.6(3) . . ?
N6 C4 C5 124.8(3) . . ?
C3 C4 N6 105.3(3) . . ?
C3 C4 C5 129.9(3) . . ?
N8 C11 C10 109.7(3) . . ?
N8 C11 C12 121.5(3) . . ?
C10 C11 C12 128.8(3) . . ?
N7 C9 C10 106.3(3) . . ?
N7 C9 C8 124.3(3) . . ?
C10 C9 C8 129.3(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C3 H3 126.1 . . ?
C4 C3 C2 107.8(3) . . ?
C4 C3 H3 126.1 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C11 C10 H10 126.5 . . ?
C9 C10 C11 106.9(3) . . ?
C9 C10 H10 126.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N1 N2 Ni2 5.0(3) . . . . ?
Ni1 N1 N2 C7 -167.9(2) . . . . ?
Ni1 N1 C6 N6 -11.3(4) . . . . ?
Ni1 N1 C6 N3 169.5(3) . . . . ?
Ni1 N9 C2 C3 -163.5(3) . . . . ?
Ni1 N9 C2 C1 12.7(6) . . . . ?
Ni2 N2 C7 N7 6.6(4) . . . . ?
Ni2 N2 C7 N4 -173.8(3) . . . . ?
Ni2 N8 C11 C10 174.4(3) . . . . ?
Ni2 N8 C11 C12 -4.3(6) . . . . ?
N1 N2 C7 N7 179.7(2) . . . . ?
N1 N2 C7 N4 -0.7(5) . . . . ?
N6 N9 C2 C3 0.0(4) . . . . ?
N6 N9 C2 C1 176.2(3) . . . . ?
N6 C4 C3 C2 -0.5(4) . . . . ?
N2 N1 C6 N6 -176.8(2) . . . . ?
N2 N1 C6 N3 4.0(5) . . . . ?
N9 N6 C6 N1 11.0(4) . . . . ?
N9 N6 C6 N3 -169.7(3) . . . . ?
N9 N6 C4 C5 -177.9(3) . . . . ?
N9 N6 C4 C3 0.5(4) . . . . ?
N9 C2 C3 C4 0.3(4) . . . . ?
N7 N8 C11 C10 0.5(4) . . . . ?
N7 N8 C11 C12 -178.2(3) . . . . ?
N7 C9 C10 C11 0.0(4) . . . . ?
N8 N7 C7 N2 -6.3(4) . . . . ?
N8 N7 C7 N4 174.1(3) . . . . ?
N8 N7 C9 C10 0.3(4) . . . . ?
N8 N7 C9 C8 178.2(3) . . . . ?
N8 C11 C10 C9 -0.3(4) . . . . ?
N4 N3 C6 N1 -2.0(5) . . . . ?
N4 N3 C6 N6 178.9(3) . . . . ?
N3 N4 C7 N2 2.7(5) . . . . ?
N3 N4 C7 N7 -177.8(3) . . . . ?
C7 N7 N8 Ni2 3.3(3) . . . . ?
C7 N7 N8 C11 179.2(3) . . . . ?
C7 N7 C9 C10 -179.3(3) . . . . ?
C7 N7 C9 C8 -1.5(6) . . . . ?
C7 N4 N3 C6 -1.3(4) . . . . ?
C6 N1 N2 Ni2 170.4(2) . . . . ?
C6 N1 N2 C7 -2.5(4) . . . . ?
C6 N6 N9 Ni1 -6.2(3) . . . . ?
C6 N6 N9 C2 -174.5(3) . . . . ?
C6 N6 C4 C5 -4.9(6) . . . . ?
C6 N6 C4 C3 173.5(3) . . . . ?
C4 N6 N9 Ni1 168.0(2) . . . . ?
C4 N6 N9 C2 -0.3(4) . . . . ?
C4 N6 C6 N1 -161.7(3) . . . . ?
C4 N6 C6 N3 17.5(5) . . . . ?
C9 N7 N8 Ni2 -176.4(2) . . . . ?
C9 N7 N8 C11 -0.5(4) . . . . ?
C9 N7 C7 N2 173.3(3) . . . . ?
C9 N7 C7 N4 -6.3(5) . . . . ?
C5 C4 C3 C2 177.9(4) . . . . ?
C1 C2 C3 C4 -175.5(4) . . . . ?
C8 C9 C10 C11 -177.7(4) . . . . ?
C12 C11 C10 C9 178.2(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_ni3
_database_code_depnum_ccdc_archive 'CCDC 2141308'
loop_
_audit_author_name
_audit_author_address
'te wang'
;Southern University of Science and Technology
China
;
_audit_update_record             
;
2022-01-11 deposited with the CCDC.	2022-04-18 downloaded from the CCDC.
;
_audit_creation_date             2022-01-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C93 H63 Cl3 N42 Ni3, 9.294(O), 1.301(C O)'
_chemical_formula_sum            'C94.30 H63 Cl3 N42 Ni3 O10.60'
_chemical_formula_weight         2236.48
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3'
_space_group_name_Hall           '-R 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   19.7747(6)
_cell_length_b                   19.7747(6)
_cell_length_c                   48.334(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     16368.2(12)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    9941
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      65.01
_cell_measurement_theta_min      2.74
_shelx_estimated_absorpt_T_max   0.880
_shelx_estimated_absorpt_T_min   0.727
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dull brownish black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6855
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.069
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0990
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            41376
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        65.267
_diffrn_reflns_theta_max         65.267
_diffrn_reflns_theta_min         2.737
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4601
_reflns_number_total             6123
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00056(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         6123
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0789
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1852P)²+0.9493P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2375
_refine_ls_wR_factor_ref         0.2548
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(O6)=1-FVAR(1)
 Sof(O1)=0.33333*(1-FVAR(2))
 Sof(O4)=Sof(C32)=FVAR(1)
 Sof(O5)=1-FVAR(2)
 Sof(O3)=FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C1(H1), C5(H5), C26(H26), C3(H3), C20(H20), C4(H4), C21(H21),
 C2(H2), C12(H12), C22(H22), C29(H29), C13(H13), C23(H23), C16(H16), C28(H28),
 C24(H24), C19(H19), C18(H18), C17(H17)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.50095(4) 0.11841(4) 0.72607(2) 0.0562(3) Uani 1 1 d . . . . .
Cl1 Cl 0.18049(7) 0.01632(9) 0.73872(3) 0.0947(5) Uani 1 1 d . . . . .
N10 N 0.51958(17) 0.21632(18) 0.68002(6) 0.0545(7) Uani 1 1 d . . . . .
N4 N 0.56441(18) 0.37893(19) 0.72258(6) 0.0561(7) Uani 1 1 d . . . . .
N12 N 0.49165(17) 0.13769(18) 0.68330(6) 0.0556(7) Uani 1 1 d . . . . .
N11 N 0.59422(19) 0.46178(19) 0.76856(6) 0.0578(8) Uani 1 1 d . . . . .
N3 N 0.55981(18) 0.33735(18) 0.69892(6) 0.0552(7) Uani 1 1 d . . . . .
N1 N 0.49933(18) 0.22015(18) 0.72632(6) 0.0562(7) Uani 1 1 d . . . . .
N13 N 0.5455(2) 0.38271(19) 0.76926(6) 0.0607(8) Uani 1 1 d . . . . .
N2 N 0.50604(19) 0.26231(19) 0.74991(6) 0.0592(8) Uani 1 1 d . . . . .
N9 N 0.4969(2) 0.00887(19) 0.73092(7) 0.0652(9) Uani 1 1 d . . . . .
N6 N 0.3240(2) 0.0552(2) 0.73038(7) 0.0697(9) Uani 1 1 d . . . . .
N5 N 0.3858(2) 0.0413(2) 0.73371(6) 0.0638(8) Uani 1 1 d . . . . .
N14 N 0.4320(2) -0.0396(2) 0.74535(7) 0.0712(9) Uani 1 1 d . . . . .
C11 C 0.5380(2) 0.3381(2) 0.74571(8) 0.0546(8) Uani 1 1 d . . . . .
N7 N 0.3040(2) -0.0794(2) 0.75650(8) 0.0794(11) Uani 1 1 d . . . . .
C10 C 0.5269(2) 0.2616(2) 0.70296(7) 0.0529(8) Uani 1 1 d . . . . .
C9 C 0.5402(2) 0.2382(2) 0.65310(8) 0.0586(9) Uani 1 1 d . . . . .
H9 H 0.5617 0.2895 0.6458 0.070 Uiso 1 1 calc R U . . .
N8 N 0.2432(2) -0.0628(2) 0.75552(8) 0.0825(12) Uani 1 1 d . . . . .
C7 C 0.4931(2) 0.1106(2) 0.65822(8) 0.0575(9) Uani 1 1 d . . . . .
C8 C 0.5242(2) 0.1730(2) 0.63879(8) 0.0587(9) Uani 1 1 d . . . . .
H8 H 0.5321 0.1696 0.6196 0.070 Uiso 1 1 calc R U . A -1
C6 C 0.4591(2) 0.0267(2) 0.65247(8) 0.0592(9) Uani 1 1 d . . . . .
C1 C 0.4056(2) -0.0292(2) 0.67054(9) 0.0654(10) Uani 1 1 d . . . . .
H1 H 0.3932 -0.0130 0.6874 0.078 Uiso 1 1 calc R U . . .
C25 C 0.6252(3) 0.0249(3) 0.72316(10) 0.0753(12) Uani 1 1 d . . . . .
C14 C 0.5923(3) 0.4863(3) 0.79407(9) 0.0688(11) Uani 1 1 d . . . . .
C30 C 0.3693(3) -0.0261(2) 0.74555(8) 0.0682(11) Uani 1 1 d . . . . .
C5 C 0.4781(2) 0.0024(3) 0.62837(9) 0.0649(10) Uani 1 1 d . . . . .
H5 H 0.5157 0.0397 0.6161 0.078 Uiso 1 1 calc R U . . .
C26 C 0.6369(3) 0.0490(3) 0.69568(11) 0.0774(12) Uani 1 1 d . . . . .
H26 H 0.5929 0.0371 0.6844 0.093 Uiso 1 1 calc R U . . .
C27 C 0.5480(3) -0.0150(3) 0.73580(9) 0.0731(12) Uani 1 1 d . . . . .
C3 C 0.3896(3) -0.1312(3) 0.64015(10) 0.0697(11) Uani 1 1 d . . . . .
H3 H 0.3663 -0.1853 0.6360 0.084 Uiso 1 1 calc R U . . .
C31 C 0.2586(2) 0.0006(3) 0.74187(9) 0.0726(12) Uani 1 1 d . . . . .
C20 C 0.7164(3) 0.6125(3) 0.79307(9) 0.0751(12) Uani 1 1 d . . . . .
H20 H 0.7357 0.5927 0.7791 0.090 Uiso 1 1 calc R U . . .
C15 C 0.6410(3) 0.5671(3) 0.80284(8) 0.0741(12) Uani 1 1 d . . . . .
C4 C 0.4418(3) -0.0771(3) 0.62207(10) 0.0726(11) Uani 1 1 d . . . . .
H4 H 0.4535 -0.0936 0.6052 0.087 Uiso 1 1 calc R U . . .
C21 C 0.7104(3) 0.0897(3) 0.68448(12) 0.0837(14) Uani 1 1 d . . . . .
H21 H 0.7173 0.1043 0.6655 0.100 Uiso 1 1 calc R U . . .
C2 C 0.3704(3) -0.1076(3) 0.66449(9) 0.0682(10) Uani 1 1 d . . . . .
H2 H 0.3334 -0.1452 0.6769 0.082 Uiso 1 1 calc R U . . .
C12 C 0.5124(3) 0.3582(3) 0.79431(9) 0.0813(13) Uani 1 1 d . . . . .
H12 H 0.4762 0.3060 0.7995 0.098 Uiso 1 1 calc R U . . .
C22 C 0.7750(3) 0.1091(3) 0.70132(15) 0.0925(17) Uani 1 1 d . . . . .
H22 H 0.8262 0.1395 0.6940 0.111 Uiso 1 1 calc R U . . .
C29 C 0.4430(4) -0.0933(3) 0.76012(11) 0.0883(15) Uani 1 1 d . . . . .
H29 H 0.4069 -0.1324 0.7723 0.106 Uiso 1 1 calc R U . . .
C13 C 0.5407(4) 0.4224(3) 0.81061(10) 0.0892(15) Uani 1 1 d . . . . .
H13 H 0.5282 0.4240 0.8295 0.107 Uiso 1 1 calc R U . . .
C23 C 0.7651(4) 0.0845(4) 0.72850(15) 0.0962(17) Uani 1 1 d . . . . .
H23 H 0.8093 0.0970 0.7397 0.115 Uiso 1 1 calc R U . . .
C16 C 0.6142(4) 0.5980(3) 0.82347(10) 0.0916(17) Uani 1 1 d . . . . .
H16 H 0.5624 0.5677 0.8303 0.110 Uiso 1 1 calc R U . . .
C28 C 0.5148(4) -0.0791(3) 0.75376(12) 0.0893(15) Uani 1 1 d . . . . .
H28 H 0.5388 -0.1073 0.7602 0.107 Uiso 1 1 calc R U . . .
C24 C 0.6912(4) 0.0419(3) 0.73942(12) 0.0905(15) Uani 1 1 d . . . . .
H24 H 0.6846 0.0238 0.7580 0.109 Uiso 1 1 calc R U . . .
C19 C 0.7642(4) 0.6876(3) 0.80370(11) 0.0953(18) Uani 1 1 d . . . . .
H19 H 0.8157 0.7189 0.7968 0.114 Uiso 1 1 calc R U . . .
C18 C 0.7373(6) 0.7163(4) 0.82399(12) 0.118(3) Uani 1 1 d . . . . .
H18 H 0.7703 0.7670 0.8313 0.142 Uiso 1 1 calc R U . . .
C17 C 0.6619(5) 0.6714(4) 0.83387(12) 0.114(2) Uani 1 1 d . . . . .
H17 H 0.6432 0.6914 0.8479 0.137 Uiso 1 1 calc R U . . .
O2 O 0.1144(4) -0.1578(5) 0.78852(18) 0.205(4) Uani 1 1 d . . . . .
O3 O 0.2198(6) -0.2199(5) 0.7890(2) 0.190(6) Uani 0.681(14) 1 d . . P B 1
O1 O 0.6667 0.3333 0.5840(3) 0.098(4) Uani 0.566(10) 3 d S T P C 2
O4 O 0.1495(7) 0.1355(7) 0.7689(3) 0.127(5) Uani 0.434(10) 1 d . . P C 1
O6 O 0.1316(12) 0.0606(11) 0.8191(4) 0.277(12) Uani 0.566(10) 1 d . . P C 2
O8 O 0.0838(7) -0.0783(10) 0.8285(3) 0.090(6) Uani 0.250(13) 1 d . . . D 1
O5 O 0.4239(15) -0.2424(15) 0.7969(4) 0.168(10) Uani 0.319(14) 1 d . . P B 2
O9 O 0.6667 0.3333 0.8031(5) 0.114(14) Uani 0.28(3) 3 d S T . . .
C32 C 0.096(2) 0.1107(15) 0.7850(5) 0.174(10) Uani 0.434(10) 1 d . . 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 N4 2.069(3) 2_655 ?
Ni1 N12 2.127(3) . ?
Ni1 N11 2.152(3) 2_655 ?
Ni1 N1 2.028(3) . ?
Ni1 N9 2.140(3) . ?
Ni1 N5 2.043(3) . ?
Cl1 C31 1.727(5) . ?
N10 N12 1.374(4) . ?
N10 C10 1.387(5) . ?
N10 C9 1.367(5) . ?
N4 Ni1 2.069(3) 3_665 ?
N4 N3 1.384(4) . ?
N4 C11 1.324(5) . ?
N12 C7 1.331(5) . ?
N11 Ni1 2.153(3) 3_665 ?
N11 N13 1.367(5) . ?
N11 C14 1.333(5) . ?
N3 C10 1.316(5) . ?
N1 N2 1.379(4) . ?
N1 C10 1.340(5) . ?
N13 C11 1.402(5) . ?
N13 C12 1.346(5) . ?
N2 C11 1.318(5) . ?
N9 N14 1.350(5) . ?
N9 C27 1.333(6) . ?
N6 N5 1.391(5) . ?
N6 C31 1.323(5) . ?
N5 C30 1.333(5) . ?
N14 C30 1.394(6) . ?
N14 C29 1.384(6) . ?
N7 N8 1.396(6) . ?
N7 C30 1.302(6) . ?
C9 H9 0.9500 . ?
C9 C8 1.353(6) . ?
N8 C31 1.311(6) . ?
C7 C8 1.423(6) . ?
C7 C6 1.472(6) . ?
C8 H8 0.9500 . ?
C6 C1 1.391(6) . ?
C6 C5 1.381(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.377(6) . ?
C25 C26 1.391(7) . ?
C25 C27 1.456(7) . ?
C25 C24 1.412(7) . ?
C14 C15 1.455(7) . ?
C14 C13 1.410(7) . ?
C5 H5 0.9500 . ?
C5 C4 1.396(6) . ?
C26 H26 0.9500 . ?
C26 C21 1.373(7) . ?
C27 C28 1.399(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.368(7) . ?
C3 C2 1.386(6) . ?
C20 H20 0.9500 . ?
C20 C15 1.383(8) . ?
C20 C19 1.401(7) . ?
C15 C16 1.405(7) . ?
C4 H4 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.396(8) . ?
C2 H2 0.9500 . ?
C12 H12 0.9500 . ?
C12 C13 1.354(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.380(9) . ?
C29 H29 0.9500 . ?
C29 C28 1.337(8) . ?
C13 H13 0.9500 . ?
C23 H23 0.9500 . ?
C23 C24 1.375(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.371(9) . ?
C28 H28 0.9500 . ?
C24 H24 0.9500 . ?
C19 H19 0.9500 . ?
C19 C18 1.367(9) . ?
C18 H18 0.9500 . ?
C18 C17 1.383(11) . ?
C17 H17 0.9500 . ?
O4 C32 1.20(3) . ?

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
N4 Ni1 N12 88.87(12) 2_655 . ?
N4 Ni1 N11 77.63(12) 2_655 2_655 ?
N4 Ni1 N9 96.16(14) 2_655 . ?
N12 Ni1 N11 163.54(13) . 2_655 ?
N12 Ni1 N9 108.97(13) . . ?
N1 Ni1 N4 86.97(13) . 2_655 ?
N1 Ni1 N12 77.42(12) . . ?
N1 Ni1 N11 92.33(13) . 2_655 ?
N1 Ni1 N9 172.87(13) . . ?
N1 Ni1 N5 100.08(14) . . ?
N9 Ni1 N11 82.12(13) . 2_655 ?
N5 Ni1 N4 170.81(13) . 2_655 ?
N5 Ni1 N12 98.37(12) . . ?
N5 Ni1 N11 96.07(12) . 2_655 ?
N5 Ni1 N9 76.18(15) . . ?
N12 N10 C10 119.4(3) . . ?
C9 N10 N12 110.8(3) . . ?
C9 N10 C10 129.7(3) . . ?
N3 N4 Ni1 126.5(2) . 3_665 ?
C11 N4 Ni1 116.8(3) . 3_665 ?
C11 N4 N3 116.5(3) . . ?
N10 N12 Ni1 107.0(2) . . ?
C7 N12 Ni1 142.3(3) . . ?
C7 N12 N10 105.8(3) . . ?
N13 N11 Ni1 108.9(2) . 3_665 ?
C14 N11 Ni1 142.9(3) . 3_665 ?
C14 N11 N13 105.2(3) . . ?
C10 N3 N4 113.7(3) . . ?
N2 N1 Ni1 124.1(2) . . ?
C10 N1 Ni1 113.5(2) . . ?
C10 N1 N2 116.1(3) . . ?
N11 N13 C11 119.5(3) . . ?
C12 N13 N11 111.8(3) . . ?
C12 N13 C11 128.6(4) . . ?
C11 N2 N1 114.0(3) . . ?
N14 N9 Ni1 108.5(3) . . ?
C27 N9 Ni1 136.6(3) . . ?
C27 N9 N14 106.1(4) . . ?
C31 N6 N5 112.8(4) . . ?
N6 N5 Ni1 126.4(3) . . ?
C30 N5 Ni1 116.7(3) . . ?
C30 N5 N6 116.6(3) . . ?
N9 N14 C30 119.3(3) . . ?
N9 N14 C29 110.7(4) . . ?
C29 N14 C30 129.8(4) . . ?
N4 C11 N13 114.6(3) . . ?
N2 C11 N4 129.9(4) . . ?
N2 C11 N13 115.5(3) . . ?
C30 N7 N8 114.8(4) . . ?
N3 C10 N10 116.7(3) . . ?
N3 C10 N1 129.8(3) . . ?
N1 C10 N10 113.6(3) . . ?
N10 C9 H9 126.4 . . ?
C8 C9 N10 107.1(3) . . ?
C8 C9 H9 126.4 . . ?
C31 N8 N7 115.2(4) . . ?
N12 C7 C8 109.8(3) . . ?
N12 C7 C6 122.4(4) . . ?
C8 C7 C6 127.5(4) . . ?
C9 C8 C7 106.4(3) . . ?
C9 C8 H8 126.8 . . ?
C7 C8 H8 126.8 . . ?
C1 C6 C7 120.9(4) . . ?
C5 C6 C7 120.1(4) . . ?
C5 C6 C1 118.9(4) . . ?
C6 C1 H1 119.4 . . ?
C2 C1 C6 121.1(4) . . ?
C2 C1 H1 119.4 . . ?
C26 C25 C27 122.4(4) . . ?
C26 C25 C24 118.3(5) . . ?
C24 C25 C27 119.3(5) . . ?
N11 C14 C15 123.1(4) . . ?
N11 C14 C13 109.7(4) . . ?
C13 C14 C15 127.1(4) . . ?
N5 C30 N14 113.1(4) . . ?
N7 C30 N5 129.2(5) . . ?
N7 C30 N14 117.8(4) . . ?
C6 C5 H5 120.0 . . ?
C6 C5 C4 120.0(4) . . ?
C4 C5 H5 120.0 . . ?
C25 C26 H26 119.2 . . ?
C21 C26 C25 121.5(5) . . ?
C21 C26 H26 119.2 . . ?
N9 C27 C25 120.5(4) . . ?
N9 C27 C28 109.5(5) . . ?
C28 C27 C25 129.9(5) . . ?
C4 C3 H3 119.8 . . ?
C4 C3 C2 120.3(4) . . ?
C2 C3 H3 119.8 . . ?
N6 C31 Cl1 114.4(4) . . ?
N8 C31 Cl1 114.6(3) . . ?
N8 C31 N6 131.1(5) . . ?
C15 C20 H20 120.0 . . ?
C15 C20 C19 120.0(5) . . ?
C19 C20 H20 120.0 . . ?
C20 C15 C14 121.3(4) . . ?
C20 C15 C16 118.6(5) . . ?
C16 C15 C14 119.8(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 C5 120.2(4) . . ?
C3 C4 H4 119.9 . . ?
C26 C21 H21 120.4 . . ?
C26 C21 C22 119.1(6) . . ?
C22 C21 H21 120.4 . . ?
C1 C2 C3 119.4(4) . . ?
C1 C2 H2 120.3 . . ?
C3 C2 H2 120.3 . . ?
N13 C12 H12 126.6 . . ?
N13 C12 C13 106.7(4) . . ?
C13 C12 H12 126.6 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.6(6) . . ?
C23 C22 H22 119.7 . . ?
N14 C29 H29 127.0 . . ?
C28 C29 N14 106.1(5) . . ?
C28 C29 H29 127.0 . . ?
C14 C13 H13 126.7 . . ?
C12 C13 C14 106.6(4) . . ?
C12 C13 H13 126.7 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 120.1(6) . . ?
C24 C23 H23 120.0 . . ?
C15 C16 H16 119.6 . . ?
C17 C16 C15 120.7(6) . . ?
C17 C16 H16 119.6 . . ?
C27 C28 H28 126.2 . . ?
C29 C28 C27 107.6(5) . . ?
C29 C28 H28 126.2 . . ?
C25 C24 H24 119.9 . . ?
C23 C24 C25 120.3(6) . . ?
C23 C24 H24 119.9 . . ?
C20 C19 H19 119.8 . . ?
C18 C19 C20 120.5(7) . . ?
C18 C19 H19 119.8 . . ?
C19 C18 H18 120.0 . . ?
C19 C18 C17 120.0(6) . . ?
C17 C18 H18 120.0 . . ?
C16 C17 C18 120.2(5) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N4 N3 C10 176.0(2) 3_665 . . . ?
Ni1 N4 C11 N13 4.0(4) 3_665 . . . ?
Ni1 N4 C11 N2 -175.9(3) 3_665 . . . ?
Ni1 N12 C7 C8 -148.5(3) . . . . ?
Ni1 N12 C7 C6 37.1(6) . . . . ?
Ni1 N11 N13 C11 18.6(4) 3_665 . . . ?
Ni1 N11 N13 C12 -163.7(3) 3_665 . . . ?
Ni1 N11 C14 C15 -28.5(8) 3_665 . . . ?
Ni1 N11 C14 C13 154.8(4) 3_665 . . . ?
Ni1 N1 N2 C11 151.1(3) . . . . ?
Ni1 N1 C10 N10 25.9(4) . . . . ?
Ni1 N1 C10 N3 -153.2(3) . . . . ?
Ni1 N9 N14 C30 23.0(4) . . . . ?
Ni1 N9 N14 C29 -151.6(3) . . . . ?
Ni1 N9 C27 C25 -38.5(6) . . . . ?
Ni1 N9 C27 C28 141.2(4) . . . . ?
Ni1 N5 C30 N14 -13.0(4) . . . . ?
Ni1 N5 C30 N7 168.0(4) . . . . ?
N10 N12 C7 C8 1.5(4) . . . . ?
N10 N12 C7 C6 -172.9(3) . . . . ?
N10 C9 C8 C7 -0.1(4) . . . . ?
N4 N3 C10 N10 179.3(3) . . . . ?
N4 N3 C10 N1 -1.6(5) . . . . ?
N12 N10 C10 N3 174.6(3) . . . . ?
N12 N10 C10 N1 -4.7(4) . . . . ?
N12 N10 C9 C8 1.1(4) . . . . ?
N12 C7 C8 C9 -0.9(4) . . . . ?
N12 C7 C6 C1 18.1(6) . . . . ?
N12 C7 C6 C5 -164.3(4) . . . . ?
N11 N13 C11 N4 -15.9(5) . . . . ?
N11 N13 C11 N2 164.0(3) . . . . ?
N11 N13 C12 C13 -0.8(6) . . . . ?
N11 C14 C15 C20 -35.8(7) . . . . ?
N11 C14 C15 C16 150.0(5) . . . . ?
N11 C14 C13 C12 0.9(6) . . . . ?
N3 N4 C11 N13 178.5(3) . . . . ?
N3 N4 C11 N2 -1.4(6) . . . . ?
N1 N2 C11 N4 -0.3(6) . . . . ?
N1 N2 C11 N13 179.8(3) . . . . ?
N13 N11 C14 C15 175.3(4) . . . . ?
N13 N11 C14 C13 -1.4(5) . . . . ?
N13 C12 C13 C14 -0.1(6) . . . . ?
N2 N1 C10 N10 179.2(3) . . . . ?
N2 N1 C10 N3 0.0(5) . . . . ?
N9 N14 C30 N5 -8.0(5) . . . . ?
N9 N14 C30 N7 171.1(4) . . . . ?
N9 N14 C29 C28 -2.3(6) . . . . ?
N9 C27 C28 C29 -0.9(6) . . . . ?
N6 N5 C30 N14 173.3(3) . . . . ?
N6 N5 C30 N7 -5.7(6) . . . . ?
N5 N6 C31 Cl1 179.0(3) . . . . ?
N5 N6 C31 N8 0.0(7) . . . . ?
N14 N9 C27 C25 179.8(4) . . . . ?
N14 N9 C27 C28 -0.5(5) . . . . ?
N14 C29 C28 C27 1.9(6) . . . . ?
C11 N4 N3 C10 2.1(4) . . . . ?
C11 N13 C12 C13 176.6(4) . . . . ?
N7 N8 C31 Cl1 175.5(3) . . . . ?
N7 N8 C31 N6 -5.5(7) . . . . ?
C10 N10 N12 Ni1 -17.1(4) . . . . ?
C10 N10 N12 C7 -178.5(3) . . . . ?
C10 N10 C9 C8 177.5(3) . . . . ?
C10 N1 N2 C11 1.0(5) . . . . ?
C9 N10 N12 Ni1 159.8(2) . . . . ?
C9 N10 N12 C7 -1.6(4) . . . . ?
C9 N10 C10 N3 -1.5(5) . . . . ?
C9 N10 C10 N1 179.2(3) . . . . ?
N8 N7 C30 N5 0.1(6) . . . . ?
N8 N7 C30 N14 -178.8(3) . . . . ?
C7 C6 C1 C2 176.3(4) . . . . ?
C7 C6 C5 C4 -175.7(4) . . . . ?
C8 C7 C6 C1 -155.3(4) . . . . ?
C8 C7 C6 C5 22.4(6) . . . . ?
C6 C7 C8 C9 173.2(4) . . . . ?
C6 C1 C2 C3 1.0(6) . . . . ?
C6 C5 C4 C3 -2.3(6) . . . . ?
C1 C6 C5 C4 2.0(6) . . . . ?
C25 C26 C21 C22 -1.9(7) . . . . ?
C25 C27 C28 C29 178.7(5) . . . . ?
C14 N11 N13 C11 -176.3(3) . . . . ?
C14 N11 N13 C12 1.4(5) . . . . ?
C14 C15 C16 C17 173.8(5) . . . . ?
C30 N14 C29 C28 -176.2(4) . . . . ?
C30 N7 N8 C31 5.1(6) . . . . ?
C5 C6 C1 C2 -1.4(6) . . . . ?
C26 C25 C27 N9 -42.4(6) . . . . ?
C26 C25 C27 C28 138.0(5) . . . . ?
C26 C25 C24 C23 3.1(7) . . . . ?
C26 C21 C22 C23 3.3(7) . . . . ?
C27 N9 N14 C30 176.3(4) . . . . ?
C27 N9 N14 C29 1.7(5) . . . . ?
C27 C25 C26 C21 177.1(4) . . . . ?
C27 C25 C24 C23 -175.3(5) . . . . ?
C31 N6 N5 Ni1 -167.7(3) . . . . ?
C31 N6 N5 C30 5.3(5) . . . . ?
C20 C15 C16 C17 -0.6(8) . . . . ?
C20 C19 C18 C17 -0.9(9) . . . . ?
C15 C14 C13 C12 -175.6(5) . . . . ?
C15 C20 C19 C18 0.8(8) . . . . ?
C15 C16 C17 C18 0.5(10) . . . . ?
C4 C3 C2 C1 -1.2(6) . . . . ?
C21 C22 C23 C24 -1.4(8) . . . . ?
C2 C3 C4 C5 1.9(7) . . . . ?
C12 N13 C11 N4 166.8(4) . . . . ?
C12 N13 C11 N2 -13.3(6) . . . . ?
C22 C23 C24 C25 -1.8(8) . . . . ?
C29 N14 C30 N5 165.4(4) . . . . ?
C29 N14 C30 N7 -15.5(7) . . . . ?
C13 C14 C15 C20 140.3(5) . . . . ?
C13 C14 C15 C16 -33.9(8) . . . . ?
C24 C25 C26 C21 -1.2(7) . . . . ?
C24 C25 C27 N9 135.9(5) . . . . ?
C24 C25 C27 C28 -43.7(7) . . . . ?
C19 C20 C15 C14 -174.4(4) . . . . ?
C19 C20 C15 C16 -0.1(7) . . . . ?
C19 C18 C17 C16 0.3(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'

# start Validation Reply Form
_vrf_PLAT306_ni3                 
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O2 Check 
RESPONSE: Hydrogen atoms of partially disordered crystal water molecules could 
not be located properly. Thus we preferred to refine only the oxygen atoms.
;
_vrf_PLAT430_ni3                 
;
PROBLEM: Short Inter D...A Contact  O2       ..O8       .       2.74 Ang.  
RESPONSE: There should be a strong hydrogen bond between the two atoms.
;
_vrf_PLAT601_ni3                 
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        196 Ang**3
RESPONSE: : We have located several lattice solvents in accordance to 
the results of thermal and elemental analyses. This is a 
microporous structure and is expected to have some voids.
;
# end Validation Reply Form
