Direct Asymmetric Hydrogenation of N-Methyl and N-Alkyl Imines with an Ir(III)H Catalyst.
Salomó, Ernest; Gallen, Albert; Sciortino, Giuseppe; Ujaque, Gregori; Grabulosa, Arnald; Lledós, Agustí; Riera, Antoni; Verdaguer, Xavier; Journal of the American Chemical Society 140 (2018) 16967–16970; doi:10.1021/jacs.8b11547

data_4133601
_publ_section_title
;
 Direct Asymmetric Hydrogenation of N-Methyl and N-Alkyl Imines with an
 Ir(III)H Catalyst.
;
_journal_issue                   49
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16967
_journal_page_last               16970
_journal_paper_doi               10.1021/jacs.8b11547
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_sum            'C64 H65 B F24 Ir N3 O P2'
_chemical_formula_weight         1613.14
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_atom_sites_solution_hydrogens   mixed
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_cell_angle_gamma                62.6282(10)
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_cell_length_c                   22.0101(2)
_cell_measurement_reflns_used    183515
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      1.7510
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_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
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_computing_structure_solution    Sir2014
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_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_unetI/netI     0.0233
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       20
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_diffrn_reflns_limit_l_min       -35
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_max         34.747
_diffrn_reflns_theta_min         1.725
_diffrn_source                   'Microfocus rotating anode X-ray tube'
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_exptl_crystal_description       block
_exptl_crystal_F_000             1612
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
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_refine_diff_density_max         4.850
_refine_diff_density_min         -5.292
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.0215(16)
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         83414
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_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^)+(0.1168P)^2^+4.4404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1878
_reflns_Friedel_coverage         0.974
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                65175
_reflns_number_total             83414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11547_si_002.cif
_cod_data_source_block           AGO158_twin1_hklf5
_cod_original_cell_volume        3346.24(7)
_cod_database_code               4133601
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.673
_shelx_estimated_absorpt_t_max   0.738
_shelx_res_checksum              95565
_shelx_hkl_checksum              71582