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_7251691
_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         'C16 H14 Ir N4 O2, F6 P, 2(C3 H6 O)'
_chemical_formula_sum            'C22 H26 F6 Ir N4 O4 P'
_chemical_formula_weight         747.64
_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     direct
_audit_creation_date             2024-05-15
_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                 90.034(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6538(3)
_cell_length_b                   27.3149(8)
_cell_length_c                   10.2280(3)
_cell_measurement_reflns_used    10543
_cell_measurement_temperature    149.9(3)
_cell_measurement_theta_max      71.4400
_cell_measurement_theta_min      4.5560
_cell_volume                     2697.05(14)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.117a (release 26-03-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.9(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_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    -20.00  34.00   0.30    3.00    --  -40.59  37.00   0.00  180
  2  \w    -20.00  34.00   0.30    3.00    --  -40.59  37.00 150.00  180
  3  \w     -5.00  37.90   0.30    3.00    --  -40.59  19.00 120.00  143
  4  \w    -20.00  34.00   0.30    3.00    --  -40.59  37.00-150.00  180
  5  \w      6.00  78.90   0.30    3.00    --   40.59 -99.00 150.00  243
  6  \w     32.00 110.90   0.30   10.00    --  103.14-125.00  60.00  263
  7  \w     50.00 176.90   0.30   10.00    --  103.14  15.00   0.00  423
  8  \w     31.00  91.90   0.30   10.00    --  103.14 -61.00   0.00  203
  9  \w     74.00 173.90   0.30   10.00    --  103.14  61.00  90.00  333
 10  \w   -113.00 -13.10   0.30    3.00    --  -40.59 -57.00  60.00  333
 11  \w   -113.00 -13.10   0.30    3.00    --  -40.59 -57.00-150.00  333
 12  \w   -113.00 -59.00   0.30    3.00    --  -40.59 -57.00 -30.00  180
 13  \w     61.00 127.90   0.30    3.00    --   40.59 178.00   0.00  223
;
_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      0.0330969000
_diffrn_orient_matrix_UB_12      -0.0551674000
_diffrn_orient_matrix_UB_13      -0.0033431000
_diffrn_orient_matrix_UB_21      0.0091126000
_diffrn_orient_matrix_UB_22      0.0019959000
_diffrn_orient_matrix_UB_23      -0.1502016000
_diffrn_orient_matrix_UB_31      0.1558845000
_diffrn_orient_matrix_UB_32      0.0116246000
_diffrn_orient_matrix_UB_33      0.0096387000
_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  0.0409
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12867
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        58.915
_diffrn_reflns_theta_max         58.915
_diffrn_reflns_theta_min         4.323
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.852
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
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    1.841
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.859
_refine_diff_density_min         -1.583
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         3732
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0699P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0923
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3590
_reflns_number_total             3732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5gc05119c2.cif
_cod_data_source_block           str2297_autored
_cod_database_code               7251691
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Ir P F'
_shelx_estimated_absorpt_t_max   0.647
_shelx_estimated_absorpt_t_min   0.220
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4532(13)
 0.5468(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C11(H11), C9(H9), C10(H10), C15(H15), C14(H14), C7(H7), C6(H6)
3.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C16(H16A,H16B,H16C), C19(H19A,H19B,H19C), C17(H17A,H17B,
 H17C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              15283
_shelx_hkl_checksum              44193
_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 2.481
_oxdiff_exptl_absorpt_empirical_full_min 0.705