A kinetic resolution strategy for the synthesis of chiral octahedral NHC-iridium(III) catalysts
Basle, Olivier; Mauduit, Marc; Crassous, Jeanne; Favereau, Ludovic; Miqueu, Karinne; crevisy, C; Dorcet, Vincent; Roisnel, Thierry; Vivès, Thomas; Tarrieu, Robert; Pichon, Delphine; Manguin, Romane; Chemical Communications  (2019) –; doi:10.1039/C9CC02434D

data_7123326
_publ_section_title
;
 A kinetic resolution strategy for the synthesis of chiral octahedral
 NHC-iridium(III) catalysts
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02434D
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C40 H38 Ir N4 O2, C H Cl3, C H2 Cl2'
_chemical_formula_sum            'C42 H41 Cl5 Ir N4 O2'
_chemical_formula_weight         1003.24
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2019-02-08 deposited with the CCDC.    2019-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3124(9)
_cell_length_b                   16.7999(17)
_cell_length_c                   26.446(2)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.50
_cell_measurement_wavelength     0.71073
_cell_volume                     4137.4(7)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2016)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2019)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            35441
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         2.319
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.591
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       stick
_exptl_crystal_F_000             1996
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.060
_refine_diff_density_max         3.808
_refine_diff_density_min         -2.021
_refine_diff_density_rms         0.188
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(12)
_refine_ls_extinction_coef       0.0040(2)
_refine_ls_extinction_method     'SHELXL-2018_3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         9467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0176P)^2^+52.5974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.795
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                9325
_reflns_number_total             9467
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc02434d2.cif
_cod_data_source_block           RT519
_cod_original_cell_volume        4137.3(7)
_cod_database_code               7123326
_shelx_res_checksum              55039
_shelx_fab_checksum              12916