Azadiene Diels-Alder cycloaddition of fulvenes: a facile approach to the [1]pyrindine system
Hong, Bor-Cherng; Wu, Jian-Lin; Gupta, Arun Kumar; Hallur, Mahanandeesha Siddappa; Liao, Ju-Hsiou; Organic Letters 6 (2004) 3453–3456; doi:10.1021/ol048762c

data_1507032
_publ_section_title
;
 Azadiene Diels-Alder cycloaddition of fulvenes: a facile approach
 to the [1]pyrindine system
;
_journal_coden_ASTM              ORLEF7
_journal_issue                   20
_journal_name_full               'Organic Letters'
_journal_page_first              3453
_journal_page_last               3456
_journal_paper_doi               10.1021/ol048762c
_journal_volume                  6
_journal_year                    2004
_chemical_formula_sum            'C34 H27 Br2 N O2 S'
_chemical_formula_weight         673.45
_space_group_IT_number           14
_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                 110.9240(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.5841(15)
_cell_length_b                   9.7852(8)
_cell_length_c                   18.2955(15)
_cell_measurement_temperature    298(2)
_cell_volume                     2940.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34131
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    2.860
_exptl_absorpt_correction_T_max  0.4033
_exptl_absorpt_correction_T_min  0.3266
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.39
_refine_diff_density_max         1.617
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         7166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+2.0703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                5487
_reflns_number_total             7166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol048762csi20040629_083838.cif
_cod_data_source_block           jlw912
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-09-20
;
_cod_database_code               1507032