Peri-selectivity in Thermolysis of Acyloxybenzocyclobutenes Possessing α,β-Unsaturated Carbonyl Group: Synthesis of 2-Benzoxocin Derivatives
Hamura, Toshiyuki; Kawano, Nobuyuki; Matsumoto, Takashi; Suzuki, Keisuke; Chemistry Letters 35 (2006) 730–; doi:10.1246/cl.2006.730

data_8000126
_publ_section_title
;
 Peri-selectivity in Thermolysis of Acyloxybenzocyclobutenes Possessing
 \a,\b-Unsaturated Carbonyl Group: Synthesis of 2-Benzoxocin Derivatives
;
_journal_issue                   7
_journal_name_full               'Chemistry Letters'
_journal_page_first              730
_journal_paper_doi               10.1246/cl.2006.730
_journal_volume                  35
_journal_year                    2006
_chemical_formula_sum            'C15 H16 O4'
_chemical_formula_weight         260.28
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.954(5)
_cell_angle_beta                 95.431(7)
_cell_angle_gamma                96.397(11)
_cell_formula_units_Z            2
_cell_length_a                   7.1817(15)
_cell_length_b                   7.7763(14)
_cell_length_c                   12.0743(15)
_cell_measurement_temperature    173(2)
_cell_volume                     635.23(19)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Rigaku R-Axis RAPID'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0263
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5813
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8959
_exptl_absorpt_correction_type   multi-run
_exptl_absorpt_process_details   scalepack
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         2779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0555
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+0.1842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                2600
_reflns_number_total             2779
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            35-730sup1.cif
_cod_data_source_block           s1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8000126