Novel ruthenium(II) hexachloromacrobicyclic complexes and their first polyaromatic-terminated diaminoclathrochelate derivative: preparation, structure, redox and adsorption characteristics, and electrocatalytic activity in the hydrogen evolution reaction.
Voloshin, Yan Z.; Chuprin, Alexander S.; Mosov, Danila O.; Vologzhanina, Anna V.; Dorovatovskii, Pavel V.; Budnikova, Yulia H.; Khrizanforova, Vera V.; Dedov, Alexey G.; Kottsov, Sergey Yu; Teplonogova, Maria A.; Ivanov, Vladimir K.; Dalton transactions (Cambridge, England : 2003) 55 (2026) 1765–1780; doi:10.1039/d5dt02479j

data_7720801
_publ_section_title
;
 Novel ruthenium(II) hexachloromacrobicyclic complexes and their first
 polyaromatic-terminated diaminoclathrochelate derivative: preparation,
 structure, redox and adsorption characteristics, and electrocatalytic
 activity in the hydrogen evolution reaction.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1765
_journal_page_last               1780
_journal_paper_doi               10.1039/d5dt02479j
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C60 H58 B2 Cl4 N8 O6 Ru, 1.5(C6 H6)'
_chemical_formula_sum            'C69 H67 B2 Cl4 N8 O6 Ru'
_chemical_formula_weight         1368.79
_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
_audit_creation_date             2025-04-02
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-10-01 deposited with the CCDC.	2025-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                113.28(3)
_cell_angle_beta                 99.85(3)
_cell_angle_gamma                94.30(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1700(16)
_cell_length_b                   19.690(4)
_cell_length_c                   22.190(4)
_cell_measurement_reflns_used    947
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.843
_cell_measurement_theta_min      2.005
_cell_volume                     3190.3(14)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rayonix CCD'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7517
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            43568
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        26.809
_diffrn_reflns_theta_max         31.126
_diffrn_reflns_theta_min         1.927
_diffrn_source                   'Belok bemline of NRC Kurchatov Institute'
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.793
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   XDS
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       prism
_exptl_crystal_F_000             1414
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.574
_refine_diff_density_min         -1.471
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         16984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0655
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+19.0806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1678
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13173
_reflns_number_total             16984
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02479j2.cif
_cod_data_source_block           ac
_cod_original_cell_volume        3190.4(13)
_cod_database_code               7720801
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
;
1.a Riding coordinates:
 N8(H8)
1.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B)
1.c Aromatic/amide H refined with riding coordinates:
 N7(H7), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20),
 C21(H21), C23(H23), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), C38(H38), C40(H40), C42(H42), C43(H43), C45(H45), C46(H46),
 C52(H52), C53(H53), C55(H55), C56(H56), C61(H61), C62(H62), C63(H63), C64(H64),
  C65(H65), C66(H66), C67(H67), C68(H68), C69(H69)
1.d Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              87499
_olex2_submission_special_instructions 'No special instructions were received'