Weakly Coordinating tert-Amide Assisted Rh(III)-Catalyzed C4-Cyanation of Indoles: Application in Photophysical Studies
Sarkar, Souradip; Biswas, Aniruddha; Das, Sarbojit; Sanyal, Bortika; Sahoo, Rajkumar; Samanta, Rajarshi; Chemical Communications  (2023) –; doi:10.1039/D3CC03075J

data_7132035
_publ_section_title
;
 Weakly Coordinating tert-Amide Assisted Rh(III)-Catalyzed C4-Cyanation of
 Indoles: Application in Photophysical Studies
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03075J
_journal_year                    2023
_chemical_formula_sum            'C21 H17 Cl N3 O'
_chemical_formula_weight         362.83
_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
_audit_update_record
;
2023-06-02 deposited with the CCDC.	2023-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                99.80(4)
_cell_angle_beta                 90.05(5)
_cell_angle_gamma                94.96(3)
_cell_formula_units_Z            2
_cell_length_a                   8.059(9)
_cell_length_b                   8.883(10)
_cell_length_c                   12.824(18)
_cell_measurement_reflns_used    5203
_cell_measurement_temperature    274(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.5
_cell_volume                     901.1(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      274(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            37573
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.050
_diffrn_reflns_theta_min         2.537
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       Cubic
_exptl_crystal_F_000             378
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5203
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.2887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4080
_reflns_number_total             5203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03075j2.cif
_cod_data_source_block           shelx
_cod_database_code               7132035
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details   'SADABS 2.10 (Bruker 2003)'
_shelx_res_checksum              97982
_shelx_hkl_checksum              26930