# Supplementary Information (SI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2026

####################################################################### 
# 
# 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_kb3002
_database_code_depnum_ccdc_archive 'CCDC 2484546'
loop_
_audit_author_name
_audit_author_address
'Luc Van Meervelt'
;KU Leuven
Belgium
;
_audit_update_record             
;
2025-09-02 deposited with the CCDC.	2026-01-09 downloaded from the CCDC.
;
_audit_creation_date             2025-07-16
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2019/1
loop_
_audit_author_email
luc.vanmeervelt@kuleuven.be
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'H12 Ni O6, 2(C H3 O3 S), 6(H2 O)'
_chemical_formula_sum            'C2 H30 Ni O18 S2'
_chemical_formula_weight         465.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         Ni1C2O6H8S2
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'

_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                   9.2073(4)
_cell_length_b                   9.2073(4)
_cell_length_c                   21.4213(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1572.68(15)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    1418
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8200
_cell_measurement_theta_min      4.4120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.4
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            2293
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.354
_diffrn_reflns_theta_min         4.427
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9566
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -90.00  56.00   1.00    1.00    --  -17.30   0.00  60.00  146
  2  ω     -2.00  73.00   1.00    1.00    --   19.02  57.00 -60.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_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                641
_reflns_number_total             712
_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       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0218(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         712
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0259
_refine_ls_restrained_S_all      1.094
_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)+(0.0270P)²+0.5892P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0635
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 Ni1-H1D \\sim Ni1-H1E
 with sigma of 0.02
2. Others
 Fixed Sof: H1C(0.3333) H1A(0.3333) H1B(0.3333)
3.a Free rotating group:
 O1(H1D,H1E), O3(H3A,H3B)
3.b Idealised Me refined as rotating group:
 C1(H1C,H1A,H1B)
;
_atom_sites_solution_hydrogens   mixed
_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 0.666667 0.333333 0.333333 0.0317(2) Uani 1 6 d DS T P . .
S1 S 0.333333 0.666667 0.37332(3) 0.0412(3) Uani 1 3 d S T P . .
O1 O 0.64039(18) 0.50132(19) 0.38691(6) 0.0524(4) Uani 1 1 d G . . . .
H1D H 0.551553 0.508025 0.387569 0.079 Uiso 1 1 d DG U . . .
H1E H 0.681591 0.531325 0.423286 0.079 Uiso 1 1 d DG U . . .
O3 O 0.21099(18) 0.34395(19) 0.50098(6) 0.0536(4) Uani 1 1 d G . . . .
H3A H 0.105153 0.302086 0.500596 0.080 Uiso 1 1 d G U . . .
H3B H 0.243800 0.396428 0.466540 0.080 Uiso 1 1 d G U . . .
O2 O 0.3539(2) 0.52849(19) 0.39325(7) 0.0643(4) Uani 1 1 d . . . . .
C1 C 0.333333 0.666667 0.2916(2) 0.112(2) Uani 1 3 d S T P . .
H1C H 0.437146 0.678818 0.276634 0.167 Uiso 0.3333 1 calc R U P A -1
H1A H 0.321182 0.758328 0.276634 0.167 Uiso 0.3333 1 calc R U P A -1
H1B H 0.241672 0.562854 0.276634 0.167 Uiso 0.3333 1 calc R U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.0352(12) . ?
Ni1 O1 2.0352(12) 3_665 ?
Ni1 O1 2.0353(12) 17 ?
Ni1 O1 2.0352(12) 2_655 ?
Ni1 O1 2.0352(12) 18_545 ?
Ni1 O1 2.0353(12) 16_655 ?
S1 O2 1.4411(14) 3_565 ?
S1 O2 1.4411(14) 2_665 ?
S1 O2 1.4411(14) . ?
S1 C1 1.751(4) . ?
O1 H1D 0.8506 . ?
O1 H1E 0.8501 . ?
O3 H3A 0.8501 . ?
O3 H3B 0.8503 . ?
C1 H1C 0.9600 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 O1 91.32(6) . 3_665 ?
O1 Ni1 O1 88.68(6) 3_665 16_655 ?
O1 Ni1 O1 88.68(6) 3_665 17 ?
O1 Ni1 O1 91.32(6) 3_665 2_655 ?
O1 Ni1 O1 180.0 3_665 18_545 ?
O1 Ni1 O1 88.68(6) . 17 ?
O1 Ni1 O1 88.68(6) . 18_545 ?
O1 Ni1 O1 180.0 2_655 17 ?
O1 Ni1 O1 91.32(6) 17 16_655 ?
O1 Ni1 O1 88.68(6) 18_545 2_655 ?
O1 Ni1 O1 91.32(6) 18_545 17 ?
O1 Ni1 O1 88.68(6) 2_655 16_655 ?
O1 Ni1 O1 180.0 . 16_655 ?
O1 Ni1 O1 91.32(6) . 2_655 ?
O1 Ni1 O1 91.32(6) 18_545 16_655 ?
O2 S1 O2 111.61(6) 3_565 2_665 ?
O2 S1 O2 111.61(6) 3_565 . ?
O2 S1 O2 111.61(6) 2_665 . ?
O2 S1 C1 107.23(7) 3_565 . ?
O2 S1 C1 107.23(7) 2_665 . ?
O2 S1 C1 107.23(7) . . ?
Ni1 O1 H1D 123.3 . . ?
Ni1 O1 H1E 124.1 . . ?
H1D O1 H1E 104.5 . . ?
H3A O3 H3B 104.5 . . ?
S1 C1 H1C 109.5 . . ?
S1 C1 H1A 109.5 . . ?
S1 C1 H1B 109.5 . . ?
H1C C1 H1A 109.5 . . ?
H1C C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?


_olex2_date_sample_data_collection 2025-05-24
_olex2_date_sample_submission    2025-05-24
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.228
_oxdiff_exptl_absorpt_empirical_full_min 0.822
