# Supplementary Information (SI) for RSC Sustainability.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_jrk06a
_database_code_depnum_ccdc_archive 'CCDC 2361136'
loop_
_audit_author_name
_audit_author_address
'Navamoney Arulsamy'
;University of Wyoming
United States of America
;
_audit_update_record             
;
2024-06-06 deposited with the CCDC.	2024-09-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            'Tutton?s salt'
_chemical_melting_point          ?
_chemical_formula_moiety         'Co0.22 H20 N2 Ni0.78 O14 S2'
_chemical_formula_sum            'Co0.22 H20 N2 Ni0.78 O14 S2'
_chemical_formula_weight         395.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

_cell_length_a                   6.2541(4)
_cell_length_b                   12.3277(8)
_cell_length_c                   9.1119(6)
_cell_angle_alpha                90
_cell_angle_beta                 107.006(2)
_cell_angle_gamma                90
_cell_volume                     671.80(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9860
_cell_measurement_theta_min      2.86
_cell_measurement_theta_max      36.42

_exptl_crystal_description       rectangular_prism
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.953
_exptl_crystal_F_000             412
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.262
_exptl_absorpt_coefficient_mu    1.792
_shelx_estimated_absorpt_T_min   0.508
_shelx_estimated_absorpt_T_max   0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6270
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_process_details   'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(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            25862
_diffrn_reflns_av_unetI/netI     0.0151
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.863
_diffrn_reflns_theta_max         36.445
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             3272
_reflns_number_gt                3113
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0208P)²+0.1639P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3272
_refine_ls_number_parameters     130
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0168
_refine_ls_wR_factor_ref         0.0431
_refine_ls_wR_factor_gt          0.0425
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_restrained_S_all      1.093
_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 0.500000 0.500000 0.000000 0.00447(19) Uani 0.7844 2 d S . P A 1
Co1 Co 0.500000 0.500000 0.000000 0.0144(11) Uiso 0.2156 2 d S . P A 2
O1 O 0.46494(9) 0.61229(4) 0.15994(6) 0.01033(8) Uani 1 1 d . . . . .
H1A H 0.502(2) 0.6743(11) 0.1419(15) 0.020(3) Uiso 1 1 d . . . . .
H1B H 0.538(2) 0.5986(12) 0.2511(17) 0.026(3) Uiso 1 1 d . . . . .
O2 O 0.20096(8) 0.43317(4) -0.00131(6) 0.00987(8) Uani 1 1 d . . . . .
H2A H 0.167(2) 0.4425(11) 0.0803(17) 0.026(3) Uiso 1 1 d . . . . .
H2B H 0.181(2) 0.3688(11) -0.0207(16) 0.023(3) Uiso 1 1 d . . . . .
O3 O 0.33752(9) 0.60667(4) -0.17245(6) 0.01033(8) Uani 1 1 d . . . . .
H3A H 0.395(3) 0.6175(11) -0.2412(17) 0.027(3) Uiso 1 1 d . . . . .
H3B H 0.213(3) 0.5887(11) -0.2072(15) 0.022(3) Uiso 1 1 d . . . . .
S1 S 0.23603(3) 0.36791(2) 0.41143(2) 0.00728(4) Uani 1 1 d . . . . .
O4 O 0.28574(10) 0.43251(4) 0.55227(6) 0.01434(9) Uani 1 1 d . . . . .
O5 O 0.44436(8) 0.32494(4) 0.38696(6) 0.01139(8) Uani 1 1 d . . . . .
O6 O 0.08785(9) 0.27585(4) 0.42164(6) 0.01116(8) Uani 1 1 d . . . . .
O7 O 0.11644(8) 0.43627(4) 0.27883(5) 0.00985(8) Uani 1 1 d . . . . .
N1 N 0.85334(10) 0.34215(5) 0.63676(7) 0.00985(9) Uani 1 1 d . . . . .
H1N H 0.944(3) 0.3281(12) 0.5853(17) 0.028(3) Uiso 1 1 d . . . . .
H2N H 0.883(3) 0.3056(13) 0.7108(18) 0.034(4) Uiso 1 1 d . . . . .
H3N H 0.873(3) 0.4055(13) 0.6590(17) 0.029(3) Uiso 1 1 d . . . . .
H4N H 0.730(3) 0.3320(13) 0.5821(18) 0.035(4) Uiso 1 1 d . . . . .


_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 2.0405(5) . ?
Ni1 O2 2.0405(5) 3_665 ?
Ni1 O1 2.0677(5) . ?
Ni1 O1 2.0677(5) 3_665 ?
Ni1 O3 2.0729(5) . ?
Ni1 O3 2.0729(5) 3_665 ?
Co1 O2 2.0405(5) . ?
Co1 O2 2.0405(5) 3_665 ?
Co1 O1 2.0677(5) . ?
Co1 O1 2.0677(5) 3_665 ?
Co1 O3 2.0729(5) . ?
Co1 O3 2.0729(5) 3_665 ?
O1 H1A 0.830(14) . ?
O1 H1B 0.839(15) . ?
O2 H2A 0.839(15) . ?
O2 H2B 0.815(14) . ?
O3 H3A 0.821(15) . ?
O3 H3B 0.780(15) . ?
S1 O4 1.4643(5) . ?
S1 O5 1.4825(5) . ?
S1 O7 1.4834(5) . ?
S1 O6 1.4853(5) . ?
N1 H1N 0.850(15) . ?
N1 H2N 0.787(16) . ?
N1 H3N 0.807(16) . ?
N1 H4N 0.794(17) . ?

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 180.0 . 3_665 ?
O2 Ni1 O1 89.34(2) . . ?
O2 Ni1 O1 90.66(2) 3_665 . ?
O2 Ni1 O1 90.66(2) . 3_665 ?
O2 Ni1 O1 89.34(2) 3_665 3_665 ?
O1 Ni1 O1 180.0 . 3_665 ?
O2 Ni1 O3 90.37(2) . . ?
O2 Ni1 O3 89.63(2) 3_665 . ?
O1 Ni1 O3 88.86(2) . . ?
O1 Ni1 O3 91.14(2) 3_665 . ?
O2 Ni1 O3 89.63(2) . 3_665 ?
O2 Ni1 O3 90.37(2) 3_665 3_665 ?
O1 Ni1 O3 91.14(2) . 3_665 ?
O1 Ni1 O3 88.86(2) 3_665 3_665 ?
O3 Ni1 O3 180.0 . 3_665 ?
O2 Co1 O2 180.0 . 3_665 ?
O2 Co1 O1 89.34(2) . . ?
O2 Co1 O1 90.66(2) 3_665 . ?
O2 Co1 O1 90.66(2) . 3_665 ?
O2 Co1 O1 89.34(2) 3_665 3_665 ?
O1 Co1 O1 180.0 . 3_665 ?
O2 Co1 O3 90.37(2) . . ?
O2 Co1 O3 89.63(2) 3_665 . ?
O1 Co1 O3 88.86(2) . . ?
O1 Co1 O3 91.14(2) 3_665 . ?
O2 Co1 O3 89.63(2) . 3_665 ?
O2 Co1 O3 90.37(2) 3_665 3_665 ?
O1 Co1 O3 91.14(2) . 3_665 ?
O1 Co1 O3 88.86(2) 3_665 3_665 ?
O3 Co1 O3 180.0 . 3_665 ?
Co1 O1 H1A 112.5(9) . . ?
Ni1 O1 H1A 112.5(9) . . ?
Co1 O1 H1B 115.2(10) . . ?
Ni1 O1 H1B 115.2(10) . . ?
H1A O1 H1B 106.2(13) . . ?
Co1 O2 H2A 114.1(10) . . ?
Ni1 O2 H2A 114.1(10) . . ?
Co1 O2 H2B 118.4(10) . . ?
Ni1 O2 H2B 118.4(10) . . ?
H2A O2 H2B 105.3(14) . . ?
Co1 O3 H3A 117.0(10) . . ?
Ni1 O3 H3A 117.0(10) . . ?
Co1 O3 H3B 109.7(10) . . ?
Ni1 O3 H3B 109.7(10) . . ?
H3A O3 H3B 110.3(14) . . ?
O4 S1 O5 110.82(3) . . ?
O4 S1 O7 109.40(3) . . ?
O5 S1 O7 109.66(3) . . ?
O4 S1 O6 109.70(3) . . ?
O5 S1 O6 109.16(3) . . ?
O7 S1 O6 108.05(3) . . ?
H1N N1 H2N 109.0(14) . . ?
H1N N1 H3N 104.9(14) . . ?
H2N N1 H3N 111.0(15) . . ?
H1N N1 H4N 107.4(14) . . ?
H2N N1 H4N 113.0(16) . . ?
H3N N1 H4N 111.0(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1A O5 0.830(14) 1.918(14) 2.7420(7) 171.6(13) 2_655 yes
O1 H1B O4 0.839(15) 1.849(15) 2.6872(7) 176.2(14) 3_666 yes
O2 H2A O7 0.839(15) 1.927(15) 2.7543(7) 168.6(14) . yes
O2 H2B S1 0.815(14) 3.023(14) 3.8156(6) 164.9(12) 4_565 yes
O2 H2B O6 0.815(14) 1.901(14) 2.7096(7) 171.2(14) 4_565 yes
O3 H3A O5 0.821(15) 2.012(15) 2.8198(7) 167.7(14) 3_665 yes
O3 H3B S1 0.780(15) 2.931(15) 3.6246(6) 149.5(12) 3_565 yes
O3 H3B O7 0.780(15) 1.997(15) 2.7696(7) 170.8(14) 3_565 yes
N1 H1N S1 0.850(15) 2.791(15) 3.5943(6) 158.1(13) 1_655 yes
N1 H1N O4 0.850(15) 2.589(15) 3.2194(8) 131.9(12) 1_655 yes
N1 H1N O6 0.850(15) 2.059(15) 2.8884(8) 164.8(14) 1_655 yes
N1 H2N O6 0.787(16) 2.213(16) 2.9628(8) 159.4(15) 4_666 yes
N1 H3N S1 0.807(16) 2.902(16) 3.6244(6) 150.1(13) 3_666 yes
N1 H3N O7 0.807(16) 2.027(16) 2.8291(8) 172.5(15) 3_666 yes
N1 H4N O5 0.794(17) 2.124(17) 2.8918(8) 162.8(16) . yes

_refine_diff_density_max         0.442
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.074



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Water at pH 3 - 4'
