Molecular Ru(II) complexes with universal pH hydrogen evolution performance.
Kumar, Rakesh; Singh, Baghendra; Draksharapu, Apparao; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9346–9351; doi:10.1039/d5dt00880h

data_7718665
_publ_section_title
;
 Molecular Ru(II) complexes with universal pH hydrogen evolution
 performance.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9346
_journal_page_last               9351
_journal_paper_doi               10.1039/d5dt00880h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C38 H41 N9 Ru, 2(F6 P)'
_chemical_formula_sum            'C38 H41 F12 N9 P2 Ru'
_chemical_formula_weight         1014.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-05-06 deposited with the CCDC.	2025-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.506(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.491(3)
_cell_length_b                   20.251(3)
_cell_length_c                   19.737(2)
_cell_measurement_reflns_used    9665
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.98
_cell_measurement_theta_min      2.30
_cell_volume                     10520(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            83605
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_min         2.724
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.435
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6606
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1579 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.8859.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       plate
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.511
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         13053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0991P)^2^+50.0634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.1969
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9561
_reflns_number_total             13053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00880h2.cif
_cod_data_source_block           10febd
_cod_depositor_comments
'Adding full bibliography for 7718665--7718666.cif.'
_cod_database_code               7718665
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.926
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: P2A(0.5) P2B(0.5) F12A(0.5) F9B(0.5) F10A(0.5) F11A(0.5) F7A(0.5)
 F8A(0.5) F9A(0.5) F12B(0.5) F8B(0.5) F10B(0.5) F11B(0.5) F7B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C11(H11a,H11b), C29(H29a,H29b), C30(H30a,H30b), C2(H2a,H2b),
 C1(H1a,H1b)
3.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C17(H17), C18(H18), C16(H16), C22(H22), C6(H6), C23(H23), C7(H7),
 C5(H5), C32(H32), C4(H4), C24(H24), C25(H25), C36(H36), C33(H33), C34(H34),
 C35(H35)
3.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C14(H14a,H14b,H14c), C27(H27a,H27b,H27c), C38(H38a,H38b,H38c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91683
_shelx_hkl_checksum              68916
_shelx_fab_checksum              71516
_olex2_submission_special_instructions 'No special instructions were received'