Synthesis of N-Styrenyl Amidines from α,β-Unsaturated Nitrones and Isocyanates through CO2 Elimination and Styrenyl Migration.
Mo, Dong-Liang; Pecak, Wiktoria H.; Zhao, Meng; Wink, Donald J.; Anderson, Laura L.; Organic letters 16 (2014) 3696–; doi:10.1021/ol501503a

data_1516965
_publ_section_title
;
 Synthesis of N-Styrenyl Amidines from \a,\b-Unsaturated Nitrones and
 Isocyanates through CO2 Elimination and Styrenyl Migration.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3696
_journal_paper_doi               10.1021/ol501503a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C27 H21 N2'
_chemical_formula_weight         388.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_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                 96.671(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5166(9)
_cell_length_b                   15.4363(15)
_cell_length_c                   15.1805(15)
_cell_measurement_temperature    298(2)
_cell_volume                     2214.9(4)
_computing_cell_refinement       'SAINT (Bruker)'
_computing_data_collection       'SMART (Bruker)'
_computing_data_reduction        'SAINT (Bruker)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16828
_diffrn_reflns_theta_full        24.80
_diffrn_reflns_theta_max         24.80
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.066
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.130
_refine_diff_density_rms         0.025
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0416
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1499
_reflns_number_gt                2438
_reflns_number_total             3805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol501503a_si_002.cif
_cod_data_source_block           compound9a
_cod_depositor_comments          'Adding full bibliography for 1516965.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1516965