Quantitative Analysis on Two-Point Ligand Modulation of Iridium Catalysts for Chemodivergent C-H Amidation.
Hwang, Yeongyu; Jung, Hoimin; Lee, Euijae; Kim, Dongwook; Chang, Sukbok; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c02079

data_4134865
_publ_section_title
;
 Quantitative Analysis on Two-Point Ligand Modulation of Iridium Catalysts
 for Chemodivergent C-H Amidation.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c02079
_journal_year                    2020
_chemical_formula_sum            'C18 H18 Cl Ir N2 O3'
_chemical_formula_weight         537.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                98.91(3)
_cell_angle_beta                 91.70(3)
_cell_angle_gamma                105.15(3)
_cell_formula_units_Z            2
_cell_length_a                   6.1590(12)
_cell_length_b                   8.1880(16)
_cell_length_c                   18.031(4)
_cell_measurement_reflns_used    23437
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      34.080
_cell_measurement_theta_min      0.372
_cell_volume                     864.8(3)
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_computing_data_collection       'PAL BL2D-SMDC Program'
_computing_data_reduction        HKL3000sm
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.650
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
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_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        22.955
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.097
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    6.245
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_description       needle
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.017
_refine_diff_density_max         2.199
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_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0511P)^2^+2.5064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3858
_reflns_number_total             4046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02079_si_003.cif
_cod_data_source_block           PO19096_002
_cod_original_cell_volume        864.7(3)
_cod_database_code               4134865
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.745
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              58536
_shelx_hkl_checksum              5668