Electrocatalytic Water Oxidation by heteroleptic Ruthenium complexes of 2,6-bis(benzimidazolyl) pyridine Scaffold: A mechanistic investigation
Khan, Sahanwaj; Sengupta, Swaraj; Khan, Mohammad adnan; Sk, Md Palashuddin; Naskar, Subhendu; Dalton Transactions  (2023) –; doi:10.1039/D3DT00128H

data_7712894
_publ_section_title
;
 Electrocatalytic Water Oxidation by heteroleptic Ruthenium complexes of
 2,6-bis(benzimidazolyl) pyridine Scaffold: A mechanistic investigation
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00128H
_journal_year                    2023
_chemical_formula_moiety         'C26 H22 N7 O3 Ru S, Cl O6, 2(H2 O), C2 H6 O S'
_chemical_formula_sum            'C28 H32 Cl N7 O12 Ru S2'
_chemical_formula_weight         859.24
_chemical_name_systematic        Ru_LL_1
_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             2021-10-25
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289)
;
_audit_update_record
;
2022-11-28 deposited with the CCDC.	2023-04-28 downloaded from the CCDC.
;
_cell_angle_alpha                74.414(3)
_cell_angle_beta                 72.884(2)
_cell_angle_gamma                74.855(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7530(2)
_cell_length_b                   12.5652(4)
_cell_length_c                   14.8182(5)
_cell_measurement_reflns_used    17834
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.4000
_cell_measurement_theta_min      3.6550
_cell_volume                     1806.65(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4324
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -16.00  80.00   1.00   31.00    --   10.07  57.00 -30.00   96
  2  \w    -24.00  50.00   1.00   31.00    --   10.07 -99.00 -60.00   74
  3  \w    -12.00  83.00   1.00   31.00    --   10.07  38.00-120.00   95
  4  \w    -58.00  37.00   1.00   31.00    --   10.07 -57.00-180.00   95
  5  \w    -50.00  20.00   1.00   31.00    --  -10.22  98.00  62.54   70
  6  \w    -79.00  15.00   1.00   31.00    --  -10.22 -77.00  60.00   94
  7  \w    -70.00 -15.00   1.00   31.00    --  -10.22 132.00 -24.45   55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0088438000
_diffrn_orient_matrix_UB_12      -0.0476505000
_diffrn_orient_matrix_UB_13      -0.0199002000
_diffrn_orient_matrix_UB_21      0.0239707000
_diffrn_orient_matrix_UB_22      -0.0354852000
_diffrn_orient_matrix_UB_23      0.0399190000
_diffrn_orient_matrix_UB_31      -0.0656136000
_diffrn_orient_matrix_UB_32      -0.0066882000
_diffrn_orient_matrix_UB_33      0.0251457000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26541
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         3.430
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         6316
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0648P)^2^+2.0973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5917
_reflns_number_total             6316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00128h2.cif
_cod_data_source_block           snskrull1
_cod_database_code               7712894
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Restrained distances
 S0AA-O00T
 1.89 with sigma of 0.02
 S0AA-C1AA
 1.5 with sigma of 0.02
3. Others
 Sof(H1AD)=Sof(H1AE)=Sof(H1AF)=Sof(S1A)=Sof(C5AB)=1-FVAR(1)
 Sof(S0AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C5AA)=FVAR(1)
 Fixed Sof: O01A(0.5) O01C(0.35) O2AA(0.5) O3AA(0.65)
4.a Free rotating group:
 O007(H00A,H00B), O00C(H00C,H00D)
4.b Me refined with riding coordinates:
 C1AA(H1AA,H1AB,H1AC), C1AA(H1AD,H1AE,H1AF)
4.c Aromatic/amide H refined with riding coordinates:
 N6(H6), N5(H5), C24(H24), C16(H16), C11(H11), C15(H15), C17(H17), C10(H10),
 C9(H9), C22(H22), C2(H2), C18(H18), C23(H23), C3(H3), C5(H5A), C4(H4)
4.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C5AA(H5AA,H5AB,H5AC)
;
_olex2_date_sample_data_collection 2019-01-22
_olex2_exptl_crystal_mounting_method Manually
_olex2_submission_original_sample_id Ru_LL_1
_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 1.460
_oxdiff_exptl_absorpt_empirical_full_min 0.544