Hydroxylamines as Bifunctional Single-Nitrogen Sources for the Rapid Assembly of Diverse Tricyclic Indole Scaffolds.
Fan, Liangxin; Hao, Jiamao; Yu, Jingxun; Ma, Xiaojun; Liu, Jingjing; Luan, Xinjun; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00403

data_4134578
_publ_section_title
;
 Hydroxylamines as Bifunctional Single-Nitrogen Sources for the Rapid
 Assembly of Diverse Tricyclic Indole Scaffolds.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00403
_journal_year                    2020
_chemical_formula_moiety         'C30 H26 N2 O4 S2'
_chemical_formula_sum            'C30 H26 N2 O4 S2'
_chemical_formula_weight         542.65
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 94.555(5)
_cell_angle_gamma                90
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_cell_length_a                   18.317(4)
_cell_length_b                   15.482(4)
_cell_length_c                   18.981(4)
_cell_measurement_reflns_used    1096
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.078
_cell_measurement_theta_min      2.631
_cell_volume                     5366(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1136
_diffrn_reflns_av_unetI/netI     0.1421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26457
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.115
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.972
_exptl_transmission_factor_min   0.942
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.321
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         9448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1810
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+1.6072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4147
_reflns_number_total             9448
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00403_si_003.cif
_cod_data_source_block           xb1283_0m
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4134578
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              329
_shelx_hkl_checksum              30798