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_4134575
_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         'C27 H23 I N2 Pd'
_chemical_formula_sum            'C27 H23 I N2 Pd'
_chemical_formula_weight         608.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.045(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4805(19)
_cell_length_b                   14.527(3)
_cell_length_c                   15.293(3)
_cell_measurement_reflns_used    4487
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.743
_cell_measurement_theta_min      2.600
_cell_volume                     2292.7(8)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11002
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.189
_exptl_absorpt_coefficient_mu    2.173
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       block
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.770
_exptl_transmission_factor_min   0.720
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+1.0254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3414
_reflns_number_total             4022
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00403_si_008.cif
_cod_data_source_block           xb2509_0m
_cod_original_cell_volume        2292.7(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4134575
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.613
_shelx_estimated_absorpt_t_max   0.781
_shelx_res_checksum              69673
_shelx_hkl_checksum              93842