#------------------------------------------------------------------------------
#$Date: 2026-03-05 04:43:07 +0100 (Thu 05 de Mar de 2026) $
#$Revision: 304828 $
#$URL: svn://www.crystallography.net/cod/cif/7/25/17/7251708.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7251708
loop_
_publ_author_name
'Derison, Femke'
'Jia, Xu'
'Van Meervelt, Luc'
'Binnemans, Koen'
'Lommelen, Rayco'
_publ_section_title
;
 Phase equilibria and thermodynamic properties of the nickel(II)
 methanesulfonate-methanesulfonic acid-water system.
;
_journal_issue                   5
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              3401
_journal_page_last               3414
_journal_paper_doi               10.1039/d5cp03992d
_journal_volume                  28
_journal_year                    2026
_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
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-07-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-09-02 deposited with the CCDC.	2026-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   9.2073(4)
_cell_length_b                   9.2073(4)
_cell_length_c                   21.4213(8)
_cell_measurement_reflns_used    1418
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8200
_cell_measurement_theta_min      4.4120
_cell_volume                     1572.68(11)
_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)'
_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_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
_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_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.473
_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
_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_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0259
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                641
_reflns_number_total             712
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5cp03992d2.cif
_cod_data_source_block           kb3002
_cod_original_cell_volume        1572.68(15)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7251708
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         Ni1C2O6H8S2
_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.
;
_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)
;
_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
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'
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
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'
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 . . ?
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 . ?
