Impact of linking groups in chelating bis-carbene iridium catalysts for transfer hydrogenation of inorganic carbonates with glycerol
Richter, Marvin L.; Peris, Eduardo; Gonell, Sergio; Green Chemistry 28 (2026) 2385–2394; doi:10.1039/D5GC05119C

data_7251692
_publ_section_title
;
 Impact of linking groups in chelating bis-carbene iridium catalysts for
 transfer hydrogenation of inorganic carbonates with glycerol
;
_journal_issue                   5
_journal_name_full               'Green Chemistry'
_journal_page_first              2385
_journal_page_last               2394
_journal_paper_doi               10.1039/D5GC05119C
_journal_volume                  28
_journal_year                    2026
_chemical_formula_moiety
'C12 H14 Br Ir N4 O2, 1[C5H12], 0.25[C5H12], 0.3[C5H12]'
_chemical_formula_sum            'C19.75 H32.6 Br Ir N4 O2'
_chemical_formula_weight         630.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-19 deposited with the CCDC.	2025-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.932(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8821(15)
_cell_length_b                   10.1194(9)
_cell_length_c                   24.188(2)
_cell_measurement_reflns_used    9320
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      35.74
_cell_measurement_theta_min      2.40
_cell_volume                     3803.4(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0834
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            355155
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.318
_diffrn_reflns_theta_min         2.189
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.148
_exptl_absorpt_correction_T_max  0.6499
_exptl_absorpt_correction_T_min  0.4645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1153 before and 0.0736 after correction.
The Ratio of minimum to maximum transmission is 0.7147.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_description       plate
_exptl_crystal_F_000             2457
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         8.021
_refine_diff_density_min         -3.972
_refine_diff_density_rms         0.396
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         18462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0565
_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^)+(0.0930P)^2^+51.5154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14764
_reflns_number_total             18462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5gc05119c2.cif
_cod_data_source_block           24pfa001
_cod_original_cell_volume        3803.5(6)
_cod_original_formula_sum        'C19.75 H32.60 Br Ir N4 O2'
_cod_database_code               7251692
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.407
_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.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C21(H21A,H21B), C9(H9A,H9B), C10(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C6(H6), C24(H24), C7(H7), C19(H19), C20(H20), C11(H11), C12(H12)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C18(H18A,H18B,H18C)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 540 electrons were found in a volume of 972\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 1.55[C5H9] per formula unit which account for 384 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9965
_shelx_hkl_checksum              85528
_shelx_fab_checksum              60253
_olex2_submission_special_instructions 'No special instructions were received'