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_7251690
_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         'C15 H17 Ir N6 O2, 2(B F4), C3, O'
_chemical_formula_sum            'C18 H23 B2 F8 Ir N6 O3'
_chemical_formula_weight         737.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-03-10
_audit_creation_method
;
Olex2 1.5
(compiled 2025.02.27 svn.r83f5de26 for OlexSys, GUI svn.r7172)
;
_audit_update_record
;
2025-06-19 deposited with the CCDC.	2025-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.579(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3330(2)
_cell_length_b                   10.8804(2)
_cell_length_c                   12.1379(3)
_cell_measurement_reflns_used    7758
_cell_measurement_temperature    240(2)
_cell_measurement_theta_max      71.8790
_cell_measurement_theta_min      4.1250
_cell_volume                     1307.90(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_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_environment      N~2~
_diffrn_ambient_temperature      240(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -5.00  35.00   0.20    1.00    --  -43.17  19.00 -90.00  200
  2  \w     -5.00  35.00   0.20    1.00    --  -43.17  19.00 120.00  200
  3  \w    -21.00  30.00   0.20    1.00    --  -43.17  37.00 -30.00  255
  4  \w     -5.00  35.00   0.20    1.00    --  -43.17  19.00-150.00  200
  5  \w     -5.00  35.00   0.20    1.00    --  -43.17  19.00  60.00  200
  6  \w     -2.00  38.00   0.20    1.00    --  -43.17  13.00 179.00  200
  7  \w    -87.00  -6.00   0.20    1.00    --  -43.17 125.00  30.00  405
  8  \w     33.00 112.00   0.20    1.00    --  102.06-125.00 -90.00  395
  9  \w     57.00 178.00   0.20    1.00    --  102.06  15.00  30.00  605
 10  \w     27.00  57.00   0.20    1.00    --  102.06 -30.00  60.00  150
 11  \w     32.00  93.00   0.20    1.00    --  102.06 -61.00 -60.00  305
 12  \w     97.00 172.00   0.20    1.00    --  102.06 125.00  60.00  375
 13  \w     31.00  72.00   0.20    1.00    --  102.06 -45.00  60.00  205
 14  \w     27.00  57.00   0.20    1.00    --  102.06 -30.00  30.00  150
 15  \w     27.00  57.00   0.20    1.00    --  102.06 -30.00  90.00  150
 16  \w     21.00 107.00   0.20    1.00    --  102.06 -94.00  90.00  430
 17  \w   -113.00 -17.00   0.20    1.00    --  -43.17 -57.00  60.00  480
 18  \w   -113.00 -17.00   0.20    1.00    --  -43.17 -57.00 -90.00  480
 19  \w   -113.00 -36.00   0.20    1.00    --  -43.17 -57.00   0.00  385
 20  \w   -113.00 -17.00   0.20    1.00    --  -43.17 -57.00-180.00  480
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0291315000
_diffrn_orient_matrix_UB_12      0.0016896000
_diffrn_orient_matrix_UB_13      -0.1317625000
_diffrn_orient_matrix_UB_21      -0.1504813000
_diffrn_orient_matrix_UB_22      -0.0247597000
_diffrn_orient_matrix_UB_23      -0.0134289000
_diffrn_orient_matrix_UB_31      -0.0263608000
_diffrn_orient_matrix_UB_32      0.1394086000
_diffrn_orient_matrix_UB_33      -0.0007088000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9457
_diffrn_reflns_point_group_measured_fraction_full 0.809
_diffrn_reflns_point_group_measured_fraction_max 0.808
_diffrn_reflns_theta_full        66.598
_diffrn_reflns_theta_max         66.598
_diffrn_reflns_theta_min         3.800
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.712
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.117a (Rigaku Oxford Diffraction, 2024)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.872
_exptl_crystal_description       plate
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.444
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 1197 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.473(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         3729
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0614P)^2^+2.5114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.528
_reflns_Friedel_fraction_full    0.594
_reflns_Friedel_fraction_max     0.593
_reflns_number_gt                3575
_reflns_number_total             3729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5gc05119c2.cif
_cod_data_source_block           str2311_auto
_cod_database_code               7251690
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Ir B F'
_shelx_estimated_absorpt_t_max   0.517
_shelx_estimated_absorpt_t_min   0.109
_diffrn_oxdiff_digest_hkl
;
4371d5cedce98262b680e13e355a8f7eb52e40
;
_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
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C6(H6), C13(H13), C14(H14)
3.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              38128
_shelx_hkl_checksum              5819
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.966
_oxdiff_exptl_absorpt_empirical_full_min 0.653