Hydrogen production via aqueous-phase reforming of methanol catalyzed by ruthenium(ii) complexes with Schiff-base pincer ligands
Ma, Chong; Xia, Yihao; Ding, Xue; Qin, Lei; Zheng, Zhiping; Dalton Transactions 54 (2025) 7785–7792; doi:10.1039/D5DT00387C

data_7718527
_publ_section_title
;
 Hydrogen production via aqueous-phase reforming of methanol catalyzed by
 ruthenium(ii) complexes with Schiff-base pincer ligands
;
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              7785
_journal_page_last               7792
_journal_paper_doi               10.1039/D5DT00387C
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C43 H42 Cl2 N3 P Ru, 2(C H4 O)'
_chemical_formula_sum            'C45 H50 Cl2 N3 O2 P Ru'
_chemical_formula_weight         867.82
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-25
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-25 deposited with the CCDC.	2025-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.756(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9459(13)
_cell_length_b                   14.1401(9)
_cell_length_c                   14.5156(9)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.52
_cell_volume                     4046.1(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0699
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            105981
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         2.519
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.601
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1107 before and 0.0797 after correction.
The Ratio of minimum to maximum transmission is 0.8484.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.065
_refine_diff_density_max         2.804
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0191P)^2^+21.0780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1028
_refine_ls_wR_factor_ref         0.1062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6502
_reflns_number_total             7115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00387c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7718527--7718528.cif.'
_cod_database_code               7718527
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.881
_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, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C20(H20), C23(H23), C5(H5), C1(H1), C2(H2), C6(H6), C13(H13),
 C10(H10), C43(H43), C42(H42), C41(H41), C40(H40), C39(H39), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C37(H37), C36(H36), C35(H35), C34(H34), C33(H33)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C19(H19A,H19B,H19C), C15(H15A,H15B,
 H15C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C2S(H2SA,H2SB,H2SC), C1S(H1SA,
 H1SB,H1SC)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O2(H2A)
;
_shelx_res_checksum              55090
_shelx_hkl_checksum              80299
_olex2_submission_special_instructions 'No special instructions were received'