Synthesis of Heterocyclic [3.3.3]Propellanes via a Sequential Four-Component Reaction
Abdolali Alizadeh; Atieh Rezvanian; Long-Guan Zhu; Journal of Organic Chemistry 77 (2012) 4385–4390; doi:10.1021/jo300457m

data_4027181
_publ_section_title
;
 Synthesis of Heterocyclic [3.3.3]Propellanes via a Sequential
 Four-Component Reaction
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4385
_journal_page_last               4390
_journal_paper_doi               10.1021/jo300457m
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C21 H19 N3 O4'
_chemical_formula_weight         377.39
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.614(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6045(5)
_cell_length_b                   17.1080(7)
_cell_length_c                   11.7885(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1919.93(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7857
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.9818
_exptl_absorpt_correction_T_min  0.9711
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.003(3)
_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   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1026
_refine_ls_R_factor_gt           0.0784
_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^)+(0.1478P)^2^+2.2004P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2240
_refine_ls_wR_factor_ref         0.2532
_reflns_number_gt                2485
_reflns_number_total             3406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo300457m_si_002.cif
_cod_data_source_block           120109_enm12
_cod_database_code               4027181