Superior electrocatalytic hydrogen evolution activity of a triply bridged diruthenium(II) complex on a carbon cloth support.
Arya, Yogita; Ansari, Toufik; Bera, Sudip Kumar; Panda, Sanjib; Indra, Arindam; Lahiri, Goutam Kumar; Chemical communications (Cambridge, England) 60 (2024) 6011–6014; doi:10.1039/d4cc01173b

data_7133023
_publ_section_title
;
 Superior electrocatalytic hydrogen evolution activity of a triply bridged
 diruthenium(II) complex on a carbon cloth support.
;
_journal_issue                   47
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6011
_journal_page_last               6014
_journal_paper_doi               10.1039/d4cc01173b
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C58 H49 N4 O2 P2 Ru, Cl O4'
_chemical_formula_sum            'C58 H49 Cl N4 O6 P2 Ru'
_chemical_formula_weight         1096.47
_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             2024-01-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-01-03 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                110.1520(10)
_cell_angle_beta                 101.1340(10)
_cell_angle_gamma                99.6610(10)
_cell_formula_units_Z            4
_cell_length_a                   15.6010(2)
_cell_length_b                   21.1050(3)
_cell_length_c                   22.1703(3)
_cell_measurement_reflns_used    41333
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      23.8890
_cell_measurement_theta_min      1.7840
_cell_volume                     6502.66(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -349.73   9.47   0.80    2.00   6.61  -9.84 -31.50    --   449
  2  \w    -60.89  -0.09   0.80    2.00    --  -14.77  94.56 -34.84   76
  3  \w    -65.46   0.14   0.80    2.00    --  -19.34  94.56 145.16   82
  4  \w   -100.81  15.19   0.80    2.00    --   -9.84 -59.25 -51.92  145
  5  \f    -10.27 348.93   0.80    2.00  81.02  -9.84  31.50    --   449
  6  \w    -65.46   0.14   0.80    2.00    --  -19.34  94.56  73.16   82
  7  \w    -65.46   0.14   0.80    2.00    --  -19.34  94.56   1.16   82
  8  \w   -100.81  15.19   0.80    2.00    --   -9.84 -59.25  92.08  145
  9  \f   -340.02  19.18   0.80    2.00  15.81  -9.84 -59.25    --   449
 10  \w   -100.81  15.19   0.80    2.00    --   -9.84 -59.25-123.92  145
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0082958000
_diffrn_orient_matrix_UB_12      -0.0296302000
_diffrn_orient_matrix_UB_13      0.0083062000
_diffrn_orient_matrix_UB_21      0.0093242000
_diffrn_orient_matrix_UB_22      0.0221891000
_diffrn_orient_matrix_UB_23      0.0341147000
_diffrn_orient_matrix_UB_31      -0.0462599000
_diffrn_orient_matrix_UB_32      0.0000316000
_diffrn_orient_matrix_UB_33      -0.0045562000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0872
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            303607
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.733
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       plate
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.48
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1306
_refine_ls_number_reflns         22925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0545
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+9.2073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1438
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16302
_reflns_number_total             22925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01173b2.cif
_cod_data_source_block           '[2]ClO4'
_cod_depositor_comments
'Adding full bibliography for 7133020--7133023.cif.'
_cod_original_cell_volume        6502.66(16)
_cod_database_code               7133023
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.817
_reflns_odcompleteness_completeness 79.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.95
_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:
 C5(H5), C53(H53), C41(H41), C83(H83), C95(H95), C60(H60), C97(H97), C54(H54),
 C57(H57), C39(H39), C101(H101), C10(H10), C98(H98), C47(H47), C99(H99),
 C110(H110), C75(H75), C4(H4), C3(H3), C51(H51), C103(H103), C85(H85), C73(H73),
  C35(H35), C113(H113), C23(H23), C48(H48), C100(H100), C109(H109), C32(H32),
 C112(H112), C27(H27), C42(H42), C79(H79), C74(H74), C91(H91), C43(H43),
 C107(H107), C29(H29), C94(H94), C82(H82), C24(H24), C38(H38), C86(H86),
 C31(H31), C25(H25), C111(H111), C89(H89), C55(H55), C45(H45), C26(H26),
 C50(H50), C56(H56), C80(H80), C93(H93), C33(H33), C49(H49), C104(H104),
 C44(H44), C87(H87), C11(H11), C88(H88), C92(H92), C106(H106), C37(H37),
 C36(H36), C61(H61), C12(H12), C105(H105), C81(H81), C17(H17), C19(H19),
 C30(H30), C18(H18), C62(H62), C67(H67), C69(H69), C68(H68)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C77(H77A,H77B,H77C), C14(H14A,H14B,H14C), C64(H64A,H64B,
 H64C), C21(H21A,H21B,H21C), C71(H71A,H71B,H71C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56393
_shelx_hkl_checksum              5963
_shelx_fab_checksum              97167
_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 1.440
_oxdiff_exptl_absorpt_empirical_full_min 0.601