N<sub>2</sub>O<sub>2</sub>S-donor redox-active ligand coordinated dinuclear manganese(II) and cobalt(II) complexes: crystal structures, magnetic properties and electrochemical hydrogen evolution.
Ikbal, Asik; Das, Gouri Sankar; Mehta, Sakshi; Agrawalla, Suraj Kumar; Purohit, Chandra Shekhar; Diyali, Nilankar; Mondal, Abhishake; Biswas, Bhaskar; Das, Hari Sankar; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12447–12453; doi:10.1039/d5dt00744e

data_1575262
_publ_section_title
;
 N<sub>2</sub>O<sub>2</sub>S-donor redox-active ligand coordinated
 dinuclear manganese(II) and cobalt(II) complexes: crystal structures,
 magnetic properties and electrochemical hydrogen evolution.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12447
_journal_page_last               12453
_journal_paper_doi               10.1039/d5dt00744e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C52 H36 Co2 N4 O4 S2, 2(C3 H7 N O), H2 O'
_chemical_formula_sum            'C58 H52 Co2 N6 O7 S2'
_chemical_formula_weight         1127.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-03-27 deposited with the CCDC.	2025-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                101.0530(10)
_cell_angle_beta                 108.1640(10)
_cell_angle_gamma                108.1900(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7250(2)
_cell_length_b                   13.2973(2)
_cell_length_c                   17.8496(2)
_cell_measurement_reflns_used    21952
_cell_measurement_temperature    99.95
_cell_measurement_theta_max      75.0280
_cell_measurement_theta_min      3.8010
_cell_volume                     2582.84(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.95
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -50.00  24.00   0.50    1.50    --  -38.50  59.00  10.00  148
  2  \w   -101.00 -26.00   0.50    1.50    --  -38.50 -59.00-129.00  150
  3  \w    -14.00  61.00   0.50    1.50    --   48.81 -59.00-129.00  150
  4  \w     37.00 112.00   0.50    1.50    --   48.81  59.00  10.00  150
  5  \w     39.00 114.00   0.50    4.50    --  102.00 -59.00-129.00  150
  6  \w     90.00 165.00   0.50    4.50    --  102.00  59.00  10.00  150
  7  \w    -44.00  31.00   0.50    1.50    --  -38.50  19.00 -90.00  150
  8  \w   -105.00 -35.00   0.50    1.50    --  -38.50 -38.00 -90.00  140
  9  \w    -86.00  -6.00   0.50    1.50    --  -38.50 125.00  60.00  160
 10  \w      7.00  84.00   0.50    1.50    --   48.81 -99.00  90.00  154
 11  \w     46.00 115.00   0.50    1.50    --   48.81  38.00-120.00  138
 12  \w     98.00 167.00   0.50    4.50    --  102.00  45.00 -60.00  138
 13  \w     34.00 106.00   0.50    4.50    --  102.00 -94.00  30.00  144
 14  \w     97.00 165.00   0.50    4.50    --  102.00 125.00 -60.00  136
 15  \w     39.00 112.00   0.50    4.50    --  102.00-125.00-150.00  146
 16  \w     99.00 170.00   0.50    4.50    --  102.00  30.00-120.00  142
 17  \w     38.00 107.00   0.50    4.50    --  102.00 -45.00-180.00  138
 18  \w     94.00 171.00   0.50    4.50    --  102.00  15.00   0.00  154
 19  \w     38.00 125.00   0.50    4.50    --  102.00 -77.00-120.00  174
 20  \w     39.00 112.00   0.50    4.50    --  102.00-125.00 150.00  146
 21  \w     98.00 167.00   0.50    4.50    --  102.00  45.00-150.00  138
 22  \w     38.00 107.00   0.50    4.50    --  102.00 -45.00 -60.00  138
 23  \w    103.00 167.00   0.50    4.50    --  102.00  77.00  90.00  128
 24  \w     38.00 125.00   0.50    4.50    --  102.00 -77.00   0.00  174
 25  \w     39.00 115.00   0.50    4.50    --  102.00 -61.00 120.00  152
 26  \w     34.00 106.00   0.50    4.50    --  102.00 -94.00-120.00  144
 27  \w     34.00 105.00   0.50    4.50    --  102.00 -30.00   0.00  142
 28  \w     34.00 106.00   0.50    4.50    --  102.00 -94.00 150.00  144
 29  \w     34.00 106.00   0.50    4.50    --  102.00 -94.00 -30.00  144
 30  \w    123.00 152.00   0.50    4.50    --  102.00 125.00 120.00   58
 31  \w     52.00  97.00   0.50    4.50    --  102.00 -94.00-150.00   90
 32  \w    104.00 168.00   0.50    4.50    --  102.00  30.00 -90.00  128
 33  \w     39.00 115.00   0.50    4.50    --  102.00 -61.00  30.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0534137000
_diffrn_orient_matrix_UB_12      -0.1285610000
_diffrn_orient_matrix_UB_13      -0.0344037000
_diffrn_orient_matrix_UB_21      0.1185045000
_diffrn_orient_matrix_UB_22      -0.0004443000
_diffrn_orient_matrix_UB_23      0.0576509000
_diffrn_orient_matrix_UB_31      -0.0490846000
_diffrn_orient_matrix_UB_32      -0.0065054000
_diffrn_orient_matrix_UB_33      0.0684559000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            40445
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.690
_diffrn_reflns_theta_min         3.693
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       needle
_exptl_crystal_F_000             1168
_exptl_crystal_preparation       'As per reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.111
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         10455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0473
_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/[\s^2^(Fo^2^)+(0.0789P)^2^+1.9436P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9288
_reflns_number_total             10455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00744e2.cif
_cod_data_source_block           ska-as-031
_cod_depositor_comments
'Adding full bibliography for 1575261--1575262.cif.'
_cod_database_code               1575262
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N O S Co'
_chemical_oxdiff_usercomment     'red needle'
_shelx_estimated_absorpt_t_max   0.519
_shelx_estimated_absorpt_t_min   0.339
_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, All O(H,H) groups
2.a Free rotating group:
 O7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C35(H35),
 C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46),
  C48(H48), C49(H49), C50(H50), C51(H51), C55(H55), C58(H58)
2.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C)
;
_shelx_res_checksum              82194
_shelx_hkl_checksum              9119
_olex2_exptl_crystal_mounting_method 'Mounted on a loop'
_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 1.631
_oxdiff_exptl_absorpt_empirical_full_min 0.596