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_1575261
_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 Mn2 N4 O4 S2, C2 H3 N'
_chemical_formula_sum            'C54 H39 Mn2 N5 O4 S2'
_chemical_formula_weight         995.90
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-25
_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                65.970(2)
_cell_angle_beta                 89.3660(10)
_cell_angle_gamma                89.621(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8991(2)
_cell_length_b                   13.3726(3)
_cell_length_c                   14.7277(2)
_cell_measurement_reflns_used    22811
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.0380
_cell_measurement_theta_min      3.6020
_cell_volume                     2320.12(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_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    -79.00   5.00   0.50    1.00    --  -38.50 112.00-150.00  168
  2  \w     17.00  89.00   0.50    1.00    --   49.06-112.00 116.00  144
  3  \w    104.00 168.00   0.50    3.00    --  102.00 112.00-150.00  128
  4  \w     37.00 109.00   0.50    3.00    --  102.00-112.00 116.00  144
  5  \w    -44.00  31.00   0.50    1.00    --  -38.50  19.00  60.00  150
  6  \w   -101.00 -27.00   0.50    1.00    --  -38.50 -57.00 150.00  148
  7  \w    -44.00  31.00   0.50    1.00    --  -38.50  19.00 -30.00  150
  8  \w    -50.00  24.00   0.50    1.00    --  -38.50  57.00 -30.00  148
  9  \w   -101.00 -27.00   0.50    1.00    --  -38.50 -57.00  60.00  148
 10  \w    -15.00  72.00   0.50    1.00    --   49.06 -77.00-150.00  174
 11  \w    -17.00  52.00   0.50    1.00    --   49.06 -38.00 -90.00  138
 12  \w     39.00 112.00   0.50    3.00    --  102.00-125.00  60.00  146
 13  \w     94.00 171.00   0.50    3.00    --  102.00  15.00-120.00  154
 14  \w     99.00 170.00   0.50    3.00    --  102.00  30.00 -90.00  142
 15  \w     34.00 110.00   0.50    3.00    --  102.00 -15.00  60.00  152
 16  \w     39.00 115.00   0.50    3.00    --  102.00 -61.00-120.00  152
 17  \w     38.00 125.00   0.50    3.00    --  102.00 -77.00-120.00  174
 18  \w     34.00 105.00   0.50    3.00    --  102.00 -30.00  90.00  142
 19  \w     39.00 112.00   0.50    3.00    --  102.00-125.00  90.00  146
 20  \w     34.00 106.00   0.50    3.00    --  102.00 -94.00 150.00  144
 21  \w     34.00 105.00   0.50    3.00    --  102.00 -30.00   0.00  142
 22  \w     34.00 106.00   0.50    3.00    --  102.00 -94.00 -30.00  144
 23  \w     38.00 125.00   0.50    3.00    --  102.00 -77.00  90.00  174
 24  \w     38.00 107.00   0.50    3.00    --  102.00 -45.00-180.00  138
 25  \w     97.00 165.00   0.50    3.00    --  102.00 125.00-180.00  136
 26  \w    103.00 167.00   0.50    3.00    --  102.00  77.00  90.00  128
 27  \w     34.00 105.00   0.50    3.00    --  102.00 -30.00 -90.00  142
 28  \w     40.00 106.00   0.50    3.00    --  102.00 -94.00-120.00  132
 29  \w     38.00  86.00   0.50    3.00    --  102.00 -45.00 -60.00   96
 30  \w     34.00 101.00   0.50    3.00    --  102.00 -15.00 120.00  134
 31  \w     62.00  99.00   0.50    3.00    --  102.00 -94.00-180.00   74
 32  \w     96.00 170.00   0.50    3.00    --  102.00  15.00 -30.00  148
;
_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      0.0398946000
_diffrn_orient_matrix_UB_12      -0.0571108000
_diffrn_orient_matrix_UB_13      0.1072492000
_diffrn_orient_matrix_UB_21      0.1062132000
_diffrn_orient_matrix_UB_22      0.0554984000
_diffrn_orient_matrix_UB_23      -0.0338461000
_diffrn_orient_matrix_UB_31      -0.0373238000
_diffrn_orient_matrix_UB_32      0.0978177000
_diffrn_orient_matrix_UB_33      0.0216841000
_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  0.0412
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36011
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.126
_diffrn_reflns_theta_min         3.286
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.698
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
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    1.426
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_preparation       'As per reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.7852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8805
_reflns_number_total             9377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00744e2.cif
_cod_data_source_block           ska-as-022_auto
_cod_depositor_comments
'Adding full bibliography for 1575261--1575262.cif.'
_cod_original_cell_volume        2320.13(8)
_cod_database_code               1575261
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C H N O S Mn'
_chemical_oxdiff_usercomment     'light red block'
_shelx_estimated_absorpt_t_max   0.395
_shelx_estimated_absorpt_t_min   0.367
_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
2.a 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)
2.b Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C)
;
_shelx_res_checksum              8405
_shelx_hkl_checksum              19649
_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 1.727
_oxdiff_exptl_absorpt_empirical_full_min 0.724