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_7720800
_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         'C13 H7 B2 Cl6 F N6 O6 Ru, 2(C2 H3 N)'
_chemical_formula_sum            'C17 H13 B2 Cl6 F N8 O6 Ru'
_chemical_formula_weight         779.74
_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   geom
_audit_creation_date             2025-08-01
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-10-01 deposited with the CCDC.	2025-12-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.306(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3997(3)
_cell_length_b                   10.6405(3)
_cell_length_c                   25.1400(7)
_cell_measurement_reflns_used    9622
_cell_measurement_temperature    100
_cell_measurement_theta_max      38.04
_cell_measurement_theta_min      2.53
_cell_volume                     2737.06(13)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker D8 Quest PHOTON detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            58903
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.978
_diffrn_reflns_theta_min         2.084
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0904 before and 0.0452 after correction.
The Ratio of minimum to maximum transmission is 0.8689.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.840
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         14831
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+2.8894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12706
_reflns_number_total             14831
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02479j2.cif
_cod_data_source_block           ac148
_cod_database_code               7720800
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.776
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C11(H11), C12(H12)
1.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              67356
_olex2_submission_special_instructions 'No special instructions were received'