Direct C–H functionalization of tetrahydro-γ-carbolines at the α-position
Zhang, Yahui; Chen, Yi; Guo, Mei; Sun, Ge; Que, Rongbin; Cui, Ranran; Gao, Yu; Chen, Haijun; New Journal of Chemistry 46 (2022) 9511–9514; doi:10.1039/D2NJ00928E

data_7061492
_publ_section_title
;
 Direct C--H functionalization of tetrahydro-\g-carbolines at the
 \a-position
;
_journal_issue                   20
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9511
_journal_page_last               9514
_journal_paper_doi               10.1039/D2NJ00928E
_journal_volume                  46
_journal_year                    2022
_chemical_formula_sum            'C27 H24 N3 O2 S'
_chemical_formula_weight         454.55
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-08-14 deposited with the CCDC.	2022-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_b                   10.825(3)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.28
_cell_volume                     4640(2)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
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_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'BRUKER D8 VENTURE PHOTON 100'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0874
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27906
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.445
_diffrn_reflns_theta_min         2.153
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4587
_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_density_diffrn    1.301
_exptl_crystal_description       block
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_refine_diff_density_max         0.355
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.7(2)
_refine_ls_extinction_coef       0.0134(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1175
_refine_ls_number_reflns         8352
_refine_ls_number_restraints     1942
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1068
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0761P)^2^+5.9404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1635
_refine_ls_wR_factor_ref         0.1882
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                5755
_reflns_number_total             8352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00928e2.cif
_cod_data_source_block           FZU4007_0m
_cod_depositor_comments
'Adding full bibliography for 7061492--7061493.cif.'
_cod_database_code               7061492
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.967
_shelx_res_checksum              85409