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_7133022
_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         'C55 H40 Br3 N4 O2 P2 Ru, Cl O4, C H Cl3'
_chemical_formula_sum            'C56 H41 Br3 Cl4 N4 O6 P2 Ru'
_chemical_formula_weight         1410.47
_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                 100.8040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3915(2)
_cell_length_b                   14.4654(2)
_cell_length_c                   20.9301(3)
_cell_measurement_reflns_used    25603
_cell_measurement_temperature    111.5(7)
_cell_measurement_theta_max      29.6180
_cell_measurement_theta_min      1.7470
_cell_volume                     5469.55(13)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      111.5(7)
_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  \f    -97.38 124.62   0.60    2.00  83.51  -7.35  31.50    --   370
  2  \w    -98.32  18.08   0.60    2.00    --   -7.35 -59.25  20.08  194
  3  \f     38.27 221.87   0.60    2.00   9.10  -7.35 -31.50    --   306
  4  \w    -98.32  18.08   0.60    2.00    --   -7.35 -59.25  92.08  194
;
_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      -0.0180726000
_diffrn_orient_matrix_UB_12      -0.0192665000
_diffrn_orient_matrix_UB_13      0.0239941000
_diffrn_orient_matrix_UB_21      -0.0001128000
_diffrn_orient_matrix_UB_22      0.0439755000
_diffrn_orient_matrix_UB_23      0.0149425000
_diffrn_orient_matrix_UB_31      -0.0348726000
_diffrn_orient_matrix_UB_32      0.0098255000
_diffrn_orient_matrix_UB_33      -0.0198029000
_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  0.0620
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            100107
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.721
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.787
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64018
_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    1.713
_exptl_crystal_description       plate
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.970
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         9625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0411P)^2^+11.7615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8512
_reflns_number_total             9625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01173b2.cif
_cod_data_source_block           '[3]ClO4'
_cod_depositor_comments
'Adding full bibliography for 7133020--7133023.cif.'
_cod_database_code               7133022
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.592
_shelx_estimated_absorpt_t_min   0.542
_reflns_odcompleteness_completeness 86.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.90
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Ternary CH refined with riding coordinates:
 C024(H024)
2.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C36(H36), C38(H38), C39(H39), C12(H12), C13(H13), C32(H32),
 C26(H26), C34(H34), C22(H22), C35(H35), C54(H54), C11(H11), C48(H48), C21(H21),
  C30(H30), C33(H33), C29(H29), C50(H50), C20(H20), C47(H47), C28(H28),
 C53(H53), C6(H6), C23(H23), C15(H15), C4(H4), C44(H44), C27(H27), C51(H51),
 C40(H40), C52(H52), C5(H5), C42(H42), C17(H17), C46(H46), C45(H45), C16(H16),
 C41(H41)
;
_shelx_res_checksum              27700
_shelx_hkl_checksum              82560
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.348
_oxdiff_exptl_absorpt_empirical_full_min 0.779