Rh(III)-Catalyzed Asymmetric Synthesis of Axially Chiral Biindolyls by Merging C-H Activation and Nucleophilic Cyclization.
Tian, Miaomiao; Bai, Dachang; Zheng, Guangfan; Chang, Junbiao; Li, Xingwei; Journal of the American Chemical Society 141 (2019) 9527–9532; doi:10.1021/jacs.9b04711

data_4127454
_publ_section_title
;
 Rh(III)-Catalyzed Asymmetric Synthesis of Axially Chiral Biindolyls by
 Merging C-H Activation and Nucleophilic Cyclization.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9527
_journal_page_last               9532
_journal_paper_doi               10.1021/jacs.9b04711
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C42 H33 I N3 O2 Rh'
_chemical_formula_weight         841.52
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0127(2)
_cell_length_b                   13.6575(2)
_cell_length_c                   30.8925(5)
_cell_measurement_reflns_used    27185
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.5400
_cell_measurement_theta_min      3.5630
_cell_volume                     4224.50(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            88758
_diffrn_reflns_theta_full        29.73
_diffrn_reflns_theta_max         29.73
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    1.169
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14439
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_platon_squeeze_details
;
;
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.646
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         11284
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.646
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+2.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1837
_reflns_number_gt                7815
_reflns_number_total             11284
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja9b04711_si_003.cif
_cod_data_source_block           1
_cod_database_code               4127454