The isomer-sensitive electrochemical HER of ruthenium(II)-hydrido complexes involving redox-active azoheteroaromatics.
Seikh, Liton; Dhara, Suman; Singh, Ajit Kumar; Singh, Aditi; Dey, Sanchaita; Indra, Arindam; Lahiri, Goutam Kumar; Dalton transactions (Cambridge, England : 2003) 53 (2024) 1746–1756; doi:10.1039/d3dt02925e

data_7714714
_publ_section_title
;
 The isomer-sensitive electrochemical HER of ruthenium(II)-hydrido
 complexes involving redox-active azoheteroaromatics.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1746
_journal_page_last               1756
_journal_paper_doi               10.1039/d3dt02925e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C45 H41 N6 O P2 Ru, Cl O4'
_chemical_formula_sum            'C45 H41 Cl N6 O5 P2 Ru'
_chemical_formula_weight         944.30
_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             2022-08-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2023-08-15 deposited with the CCDC.	2023-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                92.2110(10)
_cell_angle_beta                 100.2750(10)
_cell_angle_gamma                114.235(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7897(2)
_cell_length_b                   12.8924(3)
_cell_length_c                   15.6424(2)
_cell_measurement_reflns_used    23205
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.0520
_cell_measurement_theta_min      1.9660
_cell_volume                     2116.67(8)
_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  \f   -349.73  10.07   0.70    1.00   6.61  -9.84 -31.50    --   514
  2  \w    -60.89   0.01   0.70    1.00    --  -14.77  94.56 -34.84   87
  3  \w    -65.46   0.34   0.70    1.00    --  -19.34  94.56 145.16   94
  4  \w   -100.81  15.39   0.70    1.00    --   -9.84 -59.25 -51.92  166
  5  \w    -65.46   0.34   0.70    1.00    --  -19.34  94.56  73.16   94
  6  \f    -10.27 349.53   0.70    1.00  81.02  -9.84  31.50    --   514
  7  \w    -65.46   0.34   0.70    1.00    --  -19.34  94.56   1.16   94
  8  \w   -100.81  15.39   0.70    1.00    --   -9.84 -59.25 164.08  166
  9  \f   -339.72  20.08   0.70    1.00  15.81  -9.84 -59.25    --   514
;
_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      0.0099530000
_diffrn_orient_matrix_UB_12      -0.0279941000
_diffrn_orient_matrix_UB_13      0.0368572000
_diffrn_orient_matrix_UB_21      0.0667918000
_diffrn_orient_matrix_UB_22      0.0302581000
_diffrn_orient_matrix_UB_23      0.0045101000
_diffrn_orient_matrix_UB_31      0.0000157000
_diffrn_orient_matrix_UB_32      0.0447038000
_diffrn_orient_matrix_UB_33      0.0279002000
_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  0.0688
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            91374
_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         1.746
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56431
_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 pinkish pink'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_description       plate
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.088
_refine_diff_density_max         2.154
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         7441
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0579
_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^)+(0.0789P)^2^+7.8808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6166
_reflns_number_total             7441
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02925e2.cif
_cod_data_source_block           '[1b]ClO4'
_cod_depositor_comments
'Adding full bibliography for 7714712--7714715.cif.'
_cod_original_cell_volume        2116.67(7)
_cod_database_code               7714714
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.952
_shelx_estimated_absorpt_t_min   0.885
_reflns_odcompleteness_completeness 80.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.86
_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. Restrained distances
 Ru1-H
 1.48 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Fixed Uiso: H(0.001)
5.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C35(H35), C45(H45), C21(H21), C23(H23), C33(H33), C27(H27),
 C20(H20), C32(H32), C31(H31), C17(H17), C39(H39), C44(H44), C30(H30), C3(H3),
 C2(H2), C36(H36), C38(H38), C19(H19), C43(H43), C11(H11), C18(H18), C41(H41),
 C15(H15), C42(H42), C37(H37), C24(H24), C26(H26), C7(H7), C25(H25), C12(H12),
 C13(H13), C6(H6), C14(H14)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21022
_shelx_hkl_checksum              44985
_shelx_fab_checksum              54442
_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 1.454
_oxdiff_exptl_absorpt_empirical_full_min 0.628