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_7714715
_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 H39 I2 N6 O P2 Ru, Cl O4'
_chemical_formula_sum            'C45 H39 Cl I2 N6 O5 P2 Ru'
_chemical_formula_weight         1196.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-08-15 deposited with the CCDC.	2023-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.94190(10)
_cell_length_b                   20.4204(2)
_cell_length_c                   18.68460(10)
_cell_measurement_reflns_used    49034
_cell_measurement_temperature    104.00(10)
_cell_measurement_theta_max      33.1490
_cell_measurement_theta_min      1.9630
_cell_volume                     4547.24(6)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     14.27 198.47   0.60    2.00   6.61  -9.84 -31.50    --   307
  2  \f   -151.92  32.28   0.60    2.00  15.81  -9.84 -59.25    --   307
  3  \w   -100.81  15.59   0.60    2.00    --   -9.84 -59.25-123.92  194
  4  \w   -100.81  15.59   0.60    2.00    --   -9.84 -59.25 164.08  194
  5  \f   -106.56  94.44   0.60    2.00  81.02  -9.84  31.50    --   335
;
_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      0.0562169000
_diffrn_orient_matrix_UB_12      0.0006776000
_diffrn_orient_matrix_UB_13      -0.0101431000
_diffrn_orient_matrix_UB_21      -0.0115774000
_diffrn_orient_matrix_UB_22      0.0290483000
_diffrn_orient_matrix_UB_23      -0.0199235000
_diffrn_orient_matrix_UB_31      0.0156978000
_diffrn_orient_matrix_UB_32      0.0190253000
_diffrn_orient_matrix_UB_33      0.0307889000
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            101826
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.969
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44880
_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            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       plate
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.535
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         7989
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0358P)^2^+30.0248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7733
_reflns_number_total             7989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02925e2.cif
_cod_data_source_block           '[2a]ClO4'
_cod_depositor_comments
'Adding full bibliography for 7714712--7714715.cif.'
_cod_database_code               7714715
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.621
_shelx_estimated_absorpt_t_min   0.418
_reflns_odcompleteness_completeness 90.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.72
_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
 1.51 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C20(H20), C7(H7), C35(H35), C37(H37), C38(H38), C44(H44), C45(H45),
 C17(H17), C39(H39), C2(H2), C26(H26), C36(H36), C27(H27), C18(H18), C19(H19),
 C15(H15), C41(H41), C25(H25), C29(H29), C33(H33), C23(H23), C42(H42), C31(H31),
  C14(H14), C32(H32), C43(H43), C13(H13), C30(H30), C11(H11), C24(H24), C12(H12)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              99778
_shelx_hkl_checksum              51748
_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 1.628
_oxdiff_exptl_absorpt_empirical_full_min 0.570