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_4134574
_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 H28 Br N O6 S'
_chemical_formula_sum            'C30 H28 Br N O6 S'
_chemical_formula_weight         610.50
_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-2014/7
_cell_angle_alpha                99.633(3)
_cell_angle_beta                 90.185(3)
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_cell_formula_units_Z            2
_cell_length_a                   7.1258(11)
_cell_length_b                   11.6075(17)
_cell_length_c                   17.716(3)
_cell_measurement_reflns_used    1557
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.669
_cell_measurement_theta_min      2.335
_cell_volume                     1403.1(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7045
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.167
_exptl_absorpt_coefficient_mu    1.583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_transmission_factor_max   0.814
_exptl_transmission_factor_min   0.752
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         4887
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0432P)^2^+1.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1249
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3273
_reflns_number_total             4887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00403_si_004.cif
_cod_data_source_block           xb1282_0m
_cod_database_code               4134574
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.693
_shelx_estimated_absorpt_t_max   0.821
_shelx_res_checksum              88163
_shelx_hkl_checksum              1709