Chiral CNN pincer Ir(III)-H complexes. Transient ligand and counterion influences in the asymmetric hydrogenation of imines and quinolines.
Wen, Yisong; Cabré, Albert; Benet-Buchholz, Jordi; Riera, Antoni; Verdaguer, Xavier; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10246–10253; doi:10.1039/d5dt00667h

data_7718837
_publ_section_title
;
 Chiral CNN pincer Ir(III)-H complexes. Transient ligand and counterion
 influences in the asymmetric hydrogenation of imines and quinolines.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10246
_journal_page_last               10253
_journal_paper_doi               10.1039/d5dt00667h
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_sum
'C9.29 H9.03 B0.13 F3.1 Ir0.13 N0.39 O0.13 P0.13'
_chemical_formula_weight         217.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-03-11 deposited with the CCDC.	2025-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            31
_cell_length_a                   13.1050(2)
_cell_length_b                   20.1498(3)
_cell_length_c                   27.2687(3)
_cell_measurement_reflns_used    32182
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.7560
_cell_measurement_theta_min      2.4400
_cell_volume                     7200.66(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35 (Rigaku OD, 2018)'
_computing_molecular_graphics
;
 SHELXle: C.B. Huebschle, G.M. Sheldrick & B. Dittrich
 J.Appl.Cryst. (2011) 44, 1281-1284.
;
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution
;
  SHELXT V2018/2 (Sheldrick 2018); G.M. Sheldrick (2015)
 "SHELXT - Integrated space-group and crystal-structure
 determination", Acta Cryst., A71, 3-8. 
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  '1/4chi goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_radiation_monochromator  'Confocal Max Flux optic'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            64017
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.977
_diffrn_reflns_theta_min         2.381
_diffrn_source                   'Microfocus rotating anode X-ray tube'
_diffrn_source_current           24
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Rigaku MicroMax-007HF'
_exptl_absorpt_coefficient_mu    1.984
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.157
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 8754 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0119(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         22797
_refine_ls_number_restraints     441
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+0.7660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0673
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.869
_reflns_number_gt                21186
_reflns_number_total             22797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00667h2.cif
_cod_data_source_block           ACMM96ABDLT
_cod_depositor_comments
'Adding full bibliography for 7718837--7718838.cif.'
_cod_original_formula_sum
'C9.29 H9.03 B0.13 F3.10 Ir0.13 N0.39 O0.13 P0.13'
_cod_database_code               7718837
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              77619
_shelx_hkl_checksum              88360