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_4128015
_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            'C64.82 H48.65 B Cl1.65 F24 Ir N3 O3'
_chemical_formula_weight         1635.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90.91(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.818(3)
_cell_length_b                   14.861(3)
_cell_length_c                   35.425(7)
_cell_measurement_reflns_used    140476
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      33.941
_cell_measurement_theta_min      0.384
_cell_volume                     6747(2)
_computing_cell_refinement       HKL3000sm
_computing_data_collection       'PAL BL2D-SMDC Program'
_computing_data_reduction        HKL3000sm
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.670
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            94328
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        23.703
_diffrn_reflns_theta_max         33.624
_diffrn_reflns_theta_min         1.401
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'HKL3000sm Scalepack'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       plate
_exptl_crystal_F_000             3235
_exptl_crystal_size_max          0.072
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.264
_refine_diff_density_min         -2.112
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1114
_refine_ls_number_reflns         26674
_refine_ls_number_restraints     1735
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0899P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15144
_reflns_number_total             26674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04317_si_003.cif
_cod_data_source_block           P091_014RT
_cod_database_code               4128015
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.879
_shelx_estimated_absorpt_t_max   0.940
_shelx_res_checksum              75845
_shelx_hkl_checksum              27493