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_4134576
_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         'C29 H27 Cl N2 O6 S'
_chemical_formula_sum            'C29 H27 Cl N2 O6 S'
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
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_cell_angle_alpha                72.823(4)
_cell_angle_beta                 78.115(4)
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_cell_length_b                   11.446(3)
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_cell_measurement_reflns_used    1101
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.1887
_cell_measurement_theta_min      2.186
_cell_volume                     1382.0(6)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  \w
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0967
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
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_diffrn_reflns_number            6916
_diffrn_reflns_point_group_measured_fraction_full 0.990
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_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
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_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.160
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_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
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_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1177
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.2922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.2242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2829
_reflns_number_total             4808
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00403_si_002.cif
_cod_data_source_block           xb2407_0m
_cod_original_cell_volume        1382.1(5)
_cod_database_code               4134576
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.972
_shelx_res_checksum              48086
_shelx_hkl_checksum              54413