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_7714713
_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 H38.828 I2 N6 O P2 Ru, Cl O4'
_chemical_formula_sum            'C45 H38.83 Cl I2 N6 O5 P2 Ru'
_chemical_formula_weight         1195.91
_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
_audit_creation_date             2023-01-29
_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                 111.826(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0163(5)
_cell_length_b                   16.9641(4)
_cell_length_c                   17.1008(5)
_cell_measurement_reflns_used    17254
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      21.9350
_cell_measurement_theta_min      1.8610
_cell_volume                     4582.6(2)
_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_temperature      150.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48316
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.762
_exptl_absorpt_coefficient_mu    1.870
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.849
_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 brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       needle
_exptl_crystal_F_000             2351
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.162
_refine_diff_density_min         -1.834
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.00101(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     575
_refine_ls_number_reflns         8051
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0284P)^2^+30.0467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7813
_reflns_number_total             8051
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02925e2.cif
_cod_data_source_block           '[2b]ClO4'
_cod_depositor_comments
'Adding full bibliography for 7714712--7714715.cif.'
_cod_database_code               7714713
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.946
_shelx_estimated_absorpt_t_min   0.835
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(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
 C3-I1A
 1.8 with sigma of 0.02
3. Others
 Sof(I1A)=1-FVAR(1)
 Sof(I1)=Sof(H2)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C39(H39), C23(H23), C24(H24), C11(H11), C41(H41), C33(H33), C7(H7), C15(H15),
 C27(H27), C45(H45), C19(H19), C2(H2), C42(H42), C29(H29), C44(H44), C21(H21),
 C38(H38), C37(H37), C36(H36), C25(H25), C20(H20), C32(H32), C12(H12), C17(H17),
  C31(H31), C43(H43), C26(H26), C14(H14), C35(H35), C30(H30), C18(H18), C13(H13)
4.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              72996
_shelx_hkl_checksum              13443
_olex2_submission_special_instructions 'No special instructions were received'