Stereodefined Access to Lactams via Olefin Difunctionalization: Iridium Nitrenoids as a Motif of LUMO-Controlled Dipoles.
Hong, Seung Youn; Chang, Sukbok; Journal of the American Chemical Society 141 (2019) 10399–10408; doi:10.1021/jacs.9b04317

data_4128022
_publ_section_title
;
 Stereodefined Access to Lactams via Olefin Difunctionalization: Iridium
 Nitrenoids as a Motif of LUMO-Controlled Dipoles.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10399
_journal_page_last               10408
_journal_paper_doi               10.1021/jacs.9b04317
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C64 H47 B F24 Ir N3 O3'
_chemical_formula_weight         1565.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                75.85(3)
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_cell_angle_gamma                77.93(3)
_cell_formula_units_Z            2
_cell_length_a                   13.756(3)
_cell_length_b                   15.303(3)
_cell_length_c                   16.367(3)
_cell_measurement_reflns_used    62045
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_cell_volume                     3245.0(12)
_computing_cell_refinement       HKL3000sm
_computing_data_collection       'PAL BL2D-SMDC Program'
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_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.750
_diffrn_reflns_av_R_equivalents  0.0161
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26598
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.744
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.363
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.934
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_description       needle
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.098
_exptl_crystal_size_mid          0.022
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.970
_refine_diff_density_min         -1.026
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     983
_refine_ls_number_reflns         13306
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+3.2301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12099
_reflns_number_total             13306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04317_si_002.cif
_cod_data_source_block           P095_002
_cod_original_cell_volume        3245.0(13)
_cod_database_code               4128022
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.793
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              6810
_shelx_hkl_checksum              70448