Synthesis of nitrogen-containing fused-polycyclic compounds from tyramine derivatives using phenol dearomatization and cascade cyclization
Takuya Yokosaka; Tetsuhiro Nemoto; Hiroki Nakayama; Naoki Shiga; Yasumasa Hamada; Chem.Commun. 50 (2014) 12775–; doi:10.1039/C4cc04809A

data_7115775
_publ_section_title
;
 Synthesis of nitrogen-containing fused-polycyclic compounds from tyramine
 derivatives using phenol dearomatization and cascade cyclization
;
_journal_name_full               Chem.Commun.
_journal_page_first              12775
_journal_paper_doi               10.1039/C4cc04809A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C32 H30 N2 O5 S2'
_chemical_formula_sum            'C32 H30 N2 O5 S2'
_chemical_formula_weight         586.72
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                103.7575(16)
_cell_angle_beta                 92.1867(16)
_cell_angle_gamma                107.0971(15)
_cell_formula_units_Z            4
_cell_length_a                   11.7659(3)
_cell_length_b                   13.1216(4)
_cell_length_c                   19.8185(5)
_cell_measurement_reflns_used    14603
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      3.65
_cell_volume                     2821.30(14)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30140
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.085
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1232.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.640
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     739
_refine_ls_number_reflns         10086
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0439P)^2^+3.1177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1915
_reflns_number_gt                6385
_reflns_number_total             10086
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc04809a2.cif
_cod_data_source_block           130521nemoto01
_cod_original_cell_volume        2821.29(13)
_cod_database_code               7115775