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_7115776
_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           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.0238(9)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.76675(19)
_cell_length_b                   17.8920(4)
_cell_length_c                   14.4006(3)
_cell_measurement_reflns_used    19490
_cell_measurement_temperature    93
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      3.94
_cell_volume                     2772.38(10)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0755
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29210
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.122
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232.00
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.570
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5055
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0252P)^2^+6.1629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                3459
_reflns_number_total             5055
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c4cc04809a2.cif
_cod_data_source_block           140606nemoto17
_cod_original_cell_volume        2772.38(9)
_cod_database_code               7115776