Concise Assembly of Highly Substituted Furan-Fused 1,4-Thiazepines and Their Diels-Alder Reactions with Benzynes
Hanfeng Ding; Yiping Zhang; Ming Bian; Weijun Yao; Cheng Ma; Journal of Organic Chemistry 73 (2008) 578–584; doi:10.1021/jo702299m

data_4023210
_publ_contact_author_address
; 
Department of Chemistry
Zhejiang University
Hangzhou 310027
People's Republic of China
;
_publ_contact_author_email       mcorg@zju.edu.cn
_publ_contact_author_name        'Prof. Cheng Ma'
_publ_section_title
;
 Concise Assembly of Highly Substituted Furan-Fused
 1,4-Thiazepines and Their Diels-Alder Reactions with Benzynes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              578
_journal_page_last               584
_journal_paper_doi               10.1021/jo702299m
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C39 H34 Br N O4 S'
_chemical_formula_weight         692.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.921(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.596(3)
_cell_length_b                   23.487(6)
_cell_length_c                   12.675(4)
_cell_measurement_temperature    293(2)
_cell_volume                     3426.9(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            32311
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    1.302
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
_refine_diff_density_max         2.756
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.0009(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         7806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.1509
_refine_ls_R_factor_gt           0.0949
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3093
_refine_ls_wR_factor_ref         0.3430
_reflns_number_gt                4467
_reflns_number_total             7806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo702299m-File003_3.cif
_cod_data_source_block           14e
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4023210