# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_1_sq
_database_code_depnum_ccdc_archive 'CCDC 2061508'
loop_
_audit_author_name
_audit_author_address
'Xiaohui Wang'
;Northeast Normal University
China
;
_audit_update_record             
;
2021-02-06 deposited with the CCDC.	2022-12-29 downloaded from the CCDC.
;
_audit_creation_date             2020-09-21
_audit_creation_method           
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6129)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30.001 H18.001 Ni3 O16.001 S6'
_chemical_formula_sum            'C42 H57 N3 Ni3 O19 S6'
_chemical_formula_weight         1276.44
_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 0.0033 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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'

_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      hexagonal
_space_group_IT_number           194
_space_group_name_H-M_alt        'P 63/m m c'
_space_group_name_Hall           '-P 6c 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, x-y, z'

_cell_length_a                   16.9072(13)
_cell_length_b                   16.9072(13)
_cell_length_c                   19.713(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4880.1(11)
_cell_formula_units_Z            1.99992
_cell_measurement_reflns_used    5872
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      57.000
_cell_measurement_theta_min      1.953
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    0.869
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1505
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44225
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.491
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1241
_reflns_number_total             1640
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.633
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1640
_refine_ls_number_restraints     380
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_gt           0.0646
_refine_ls_restrained_S_all      0.982
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1295P)²+11.9902P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1933
_refine_ls_wR_factor_ref         0.2214
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C2-C3 = C4-C5 = C7-C6
 1.38 with sigma of 0.01
 C6-C5 = C3-C5
 1.45 with sigma of 0.01
 C3-C6
 2.65 with sigma of 0.01
 C4-C3
 2.34 with sigma of 0.01
 C4-C2
 2.44 with sigma of 0.01
 C6-S2
 2.61 with sigma of 0.01
 C2-C7
 4.6 with sigma of 0.01
 C9-C3 = C8-C6
 1.5 with sigma of 0.01
 C9-C8
 3.35 with sigma of 0.01
 S1-S2
 3.12 with sigma of 0.01
 S1-C3
 2.61 with sigma of 0.01
3. Restrained planarity
 C1, C2, S1, C4, C6, C8, C5, C3, C9, C7, S2
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C4 \\sim C6 \\sim C8 \\sim C5 \\sim C3 \\sim C9 \\sim C7
\\sim S1 \\sim S2 \\sim O1 \\sim O2 \\sim O1W: within 3.8A with sigma of 0.01
and sigma for terminal atoms of 0.03 within 3.8A
5. Rigid body (RIGU) restrains
 C2, S1, C4, C6, C8, C5, C3, C9, C7, S2, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C2(0.25) S1(0.25) C4(0.25) C6(0.25) C8(0.25) H8A(0.25) H8B(0.25)
 H8C(0.25) C5(0.25) C3(0.25) C9(0.25) H9A(0.25) H9B(0.25) H9C(0.25) C7(0.25)
 S2(0.25)
7.a Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_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 0.53023(7) 0.26511(3) 0.250000 0.0241(4) Uani 1 4 d S T P . .
O1 O 0.666667 0.333333 0.250000 0.041(2) Uani 1 12 d S TU P . .
O2 O 0.5229(2) 0.3458(2) 0.17451(17) 0.0521(10) Uani 1 1 d . U . . .
O1W O 0.3816(6) 0.1908(3) 0.250000 0.091(3) Uani 1 4 d S TU P . .
C1 C 0.5771(2) 0.4229(2) 0.1531(3) 0.0380(13) Uani 1 2 d S TU P . .
C2 C 0.5450(10) 0.4521(8) 0.0927(8) 0.044(2) Uani 0.25 1 d D U P A -1
S1 S 0.4303(6) 0.3827(5) 0.0725(4) 0.0486(19) Uani 0.25 1 d D U P A -1
C4 C 0.4418(7) 0.4509(8) 0.0055(9) 0.047(2) Uani 0.25 1 d D U P A -1
C6 C 0.5352(8) 0.5792(9) -0.0592(9) 0.048(3) Uani 0.25 1 d D U P A -1
C8 C 0.6205(12) 0.6644(11) -0.0819(8) 0.063(6) Uani 0.25 1 d D U P A -1
H8A H 0.640678 0.709467 -0.046583 0.094 Uiso 0.25 1 calc R U P A -1
H8B H 0.607566 0.688023 -0.122093 0.094 Uiso 0.25 1 calc R U P A -1
H8C H 0.667547 0.650000 -0.091488 0.094 Uiso 0.25 1 calc R U P A -1
C5 C 0.5289(8) 0.5238(7) -0.0020(9) 0.048(2) Uani 0.25 1 d D U P A -1
C3 C 0.5901(8) 0.5251(7) 0.0491(9) 0.046(2) Uani 0.25 1 d D U P A -1
C9 C 0.6896(10) 0.5965(11) 0.0538(8) 0.061(6) Uani 0.25 1 d D U P A -1
H9A H 0.714816 0.587877 0.094923 0.092 Uiso 0.25 1 calc R U P A -1
H9B H 0.695750 0.656109 0.053994 0.092 Uiso 0.25 1 calc R U P A -1
H9C H 0.721724 0.591098 0.015564 0.092 Uiso 0.25 1 calc R U P A -1
C7 C 0.4534(14) 0.5473(16) -0.0932(9) 0.045(3) Uani 0.25 1 d D U P A -1
S2 S 0.3662(6) 0.4465(6) -0.0546(4) 0.052(2) Uani 0.25 1 d D 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 O1 1.9978(10) . ?
Ni1 O2 2.064(3) 16_556 ?
Ni1 O2 2.064(3) . ?
Ni1 O2 2.064(3) 24 ?
Ni1 O2 2.064(3) 9 ?
Ni1 O1W 2.177(9) . ?
O2 C1 1.233(4) . ?
C1 C2 1.49(2) . ?
C2 S1 1.737(16) . ?
C2 C3 1.379(10) . ?
S1 C4 1.70(2) . ?
C4 C5 1.376(9) . ?
C4 S2 1.72(2) . ?
C6 C8 1.510(10) . ?
C6 C5 1.436(9) . ?
C6 C7 1.380(10) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C5 C3 1.437(9) . ?
C3 C9 1.505(10) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C7 S2 1.77(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
O1 Ni1 O2 92.99(10) . 24 ?
O1 Ni1 O2 92.99(10) . . ?
O1 Ni1 O2 92.99(10) . 9 ?
O1 Ni1 O2 92.99(10) . 16_556 ?
O1 Ni1 O1W 180.00(7) . . ?
O2 Ni1 O2 87.4(2) 24 . ?
O2 Ni1 O2 92.3(2) 24 9 ?
O2 Ni1 O2 92.3(2) . 16_556 ?
O2 Ni1 O2 174.0(2) 9 . ?
O2 Ni1 O2 174.0(2) 24 16_556 ?
O2 Ni1 O2 87.4(2) 9 16_556 ?
O2 Ni1 O1W 87.01(10) 24 . ?
O2 Ni1 O1W 87.01(10) 16_556 . ?
O2 Ni1 O1W 87.01(10) . . ?
O2 Ni1 O1W 87.01(10) 9 . ?
Ni1 O1 Ni1 120.0 3_655 . ?
Ni1 O1 Ni1 120.0 . 14_666 ?
Ni1 O1 Ni1 120.0 3_655 14_666 ?
C1 O2 Ni1 133.3(3) . . ?
O2 C1 O2 128.3(6) . 22_665 ?
O2 C1 C2 114.9(6) . . ?
O2 C1 C2 116.8(6) 22_665 . ?
C1 C2 S1 115.3(8) . . ?
C3 C2 C1 131.6(11) . . ?
C3 C2 S1 113.1(9) . . ?
C4 S1 C2 90.5(5) . . ?
S1 C4 S2 132.6(7) . . ?
C5 C4 S1 113.6(9) . . ?
C5 C4 S2 113.8(12) . . ?
C5 C6 C8 125.4(12) . . ?
C7 C6 C8 121.4(17) . . ?
C7 C6 C5 113.2(12) . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C5 C6 111.5(12) . . ?
C4 C5 C3 112.2(9) . . ?
C6 C5 C3 136.3(8) . . ?
C2 C3 C5 110.6(8) . . ?
C2 C3 C9 125.1(14) . . ?
C5 C3 C9 124.3(12) . . ?
C3 C9 H9A 109.5 . . ?
C3 C9 H9B 109.5 . . ?
C3 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C6 C7 S2 110.8(12) . . ?
C4 S2 C7 90.7(7) . . ?

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 O2 C1 O2 -3.4(11) . . . 22_665 ?
Ni1 O2 C1 C2 175.1(3) . . . . ?
O2 C1 C2 S1 -170.0(5) 22_665 . . . ?
O2 C1 C2 S1 11.3(4) . . . . ?
O2 C1 C2 C3 -168.7(5) . . . . ?
O2 C1 C2 C3 10.0(5) 22_665 . . . ?
C1 C2 S1 C4 179.98(15) . . . . ?
C1 C2 C3 C5 180.0(2) . . . . ?
C1 C2 C3 C9 0.1(5) . . . . ?
C2 S1 C4 C5 0.0(3) . . . . ?
C2 S1 C4 S2 179.9(4) . . . . ?
S1 C2 C3 C5 -0.1(4) . . . . ?
S1 C2 C3 C9 -179.9(3) . . . . ?
S1 C4 C5 C6 179.9(3) . . . . ?
S1 C4 C5 C3 -0.1(5) . . . . ?
S1 C4 S2 C7 -180.0(4) . . . . ?
C4 C5 C3 C2 0.1(5) . . . . ?
C4 C5 C3 C9 180.0(4) . . . . ?
C6 C5 C3 C2 -179.9(5) . . . . ?
C6 C5 C3 C9 0.0(8) . . . . ?
C6 C7 S2 C4 0.2(4) . . . . ?
C8 C6 C5 C4 179.8(4) . . . . ?
C8 C6 C5 C3 -0.2(8) . . . . ?
C8 C6 C7 S2 -180.0(4) . . . . ?
C5 C4 S2 C7 -0.1(4) . . . . ?
C5 C6 C7 S2 -0.2(5) . . . . ?
C3 C2 S1 C4 0.0(2) . . . . ?
C7 C6 C5 C4 0.1(6) . . . . ?
C7 C6 C5 C3 -179.9(5) . . . . ?
S2 C4 C5 C6 0.0(5) . . . . ?
S2 C4 C5 C3 -180.0(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
