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_7133020
_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         'C62 H47 Cl N6 O2 P2 Ru2, 2(Cl O4)'
_chemical_formula_sum            'C62 H47 Cl3 N6 O10 P2 Ru2'
_chemical_formula_weight         1406.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-29
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-01-02 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.604(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.7908(5)
_cell_length_b                   15.1911(4)
_cell_length_c                   23.1446(8)
_cell_measurement_reflns_used    6522
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      19.6720
_cell_measurement_theta_min      1.6390
_cell_volume                     6632.4(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -101.42  30.58   0.50   10.00    --   -1.51 -59.25 164.08  264
  2  \w   -101.42  30.58   0.50   10.00    --   -1.51 -59.25  92.08  264
  3  \w   -101.42  30.58   0.50   10.00    --   -1.51 -59.25  20.08  264
  4  \f    -14.27 194.73   0.50   10.00  89.34  -1.51  31.50    --   418
;
_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      -0.0340339000
_diffrn_orient_matrix_UB_12      -0.0142685000
_diffrn_orient_matrix_UB_13      0.0002432000
_diffrn_orient_matrix_UB_21      0.0026084000
_diffrn_orient_matrix_UB_22      -0.0369771000
_diffrn_orient_matrix_UB_23      -0.0179058000
_diffrn_orient_matrix_UB_31      0.0157791000
_diffrn_orient_matrix_UB_32      -0.0246697000
_diffrn_orient_matrix_UB_33      0.0267141000
_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  0.1481
_diffrn_reflns_av_unetI/netI     0.0934
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            104037
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.628
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.01764
_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 yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       needle
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.687
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         11661
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0683P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1281
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6875
_reflns_number_total             11661
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01173b2.cif
_cod_data_source_block           '[1](ClO4)2'
_cod_depositor_comments
'Adding full bibliography for 7133020--7133023.cif.'
_cod_original_cell_volume        6632.4(3)
_cod_database_code               7133020
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.796
_reflns_odcompleteness_completeness 88.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.75
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C48-C53
 1.45 with sigma of 0.02
 C53-C48
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(Cl3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
4. Others
 Fixed Sof: O8(0.5) O10(0.5) O9(0.5) O12(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C24(H24), C23(H23), C22(H22), C1(H1), C62(H62), C30(H30), C10(H10),
 C47(H47), C26(H26), C7(H7), C43(H43), C38(H38), C39(H39), C18(H18), C55(H55),
 C59(H59), C2(H2), C27(H27), C4(H4), C41(H41), C3(H3), C46(H46), C40(H40),
 C9(H9), C28(H28), C45(H45), C36(H36), C29(H29), C15(H15), C58(H58), C57(H57),
 C32(H32), C16(H16), C17(H17), C8(H8), C56(H56), C44(H44), C34(H34), C49(H49),
 C50(H50), C33(H33), C51(H51), C35(H35), C52(H52), C53(H53)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              83550
_shelx_hkl_checksum              67893
_shelx_fab_checksum              90511
_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 34.567
_oxdiff_exptl_absorpt_empirical_full_min 0.539