Gold-Catalyzed Cycloisomerization/1,5-H Migration/Diels-Alder Reaction Cascade: Synthesis of Complex Nitrogen-Containing Heterocycles.
Zhang, Shuyao; Cheng, Beiming; Wang, Shen-An; Zhou, Ling; Tung, Chen-Ho; Wang, Jianwu; Xu, Zhenghu; Organic letters 19 (2017) 1072–1075; doi:10.1021/acs.orglett.7b00090

data_1545445
_publ_section_title
;
 Gold-Catalyzed Cycloisomerization/1,5-H Migration/Diels-Alder Reaction
 Cascade: Synthesis of Complex Nitrogen-Containing Heterocycles.
;
_journal_issue                   5
_journal_name_full               'Organic letters'
_journal_page_first              1072
_journal_page_last               1075
_journal_paper_doi               10.1021/acs.orglett.7b00090
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C28 H26 N2 O5 S'
_chemical_formula_weight         502.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                68.18(3)
_cell_angle_beta                 67.74(3)
_cell_angle_gamma                70.59(3)
_cell_formula_units_Z            2
_cell_length_a                   10.430(5)
_cell_length_b                   11.137(5)
_cell_length_c                   12.934(5)
_cell_measurement_reflns_used    1426
_cell_measurement_temperature    571(2)
_cell_measurement_theta_max      19.736
_cell_measurement_theta_min      2.611
_cell_volume                     1258.3(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      571(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11533
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.611
_exptl_absorpt_coefficient_mu    0.170
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4395
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0798P)^2^+0.7152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2465
_reflns_number_total             4395
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b00090_si_002.cif
_cod_data_source_block           p
_cod_original_cell_volume        1258.4(10)
_cod_database_code               1545445
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.967
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              93820
_shelx_hkl_checksum              9636