Pd-Catalyzed One-Pot Synthesis of Polysubstituted Acrylamidines from Isocyanides, Diazo Compounds, and Imines
Yan, Xu; Liao, Jinxi; Lu, Yongzhi; Liu, Jinsong; Zeng, Youlin; Cai, Qian; Organic Letters 15 (2013) 2478–; doi:10.1021/ol4009552

data_1512062
_publ_section_title
;
 Pd-Catalyzed One-Pot Synthesis of Polysubstituted Acrylamidines from
 Isocyanides, Diazo Compounds, and Imines
;
_journal_issue                   10
_journal_name_full               'Organic Letters'
_journal_page_first              2478
_journal_paper_doi               10.1021/ol4009552
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C23 H28 N2 O4 S'
_chemical_formula_sum            'C23 H28 N2 O4 S'
_chemical_formula_weight         428.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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_date             2013-04-28
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.05.09 svn.r2324, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.5885(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.54807(18)
_cell_length_b                   13.6451(3)
_cell_length_c                   17.5212(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2278.26(8)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22986
_diffrn_reflns_theta_full        66.51
_diffrn_reflns_theta_max         66.51
_diffrn_reflns_theta_min         4.11
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.513
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             912
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         4018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0551P)^2^+0.9617P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                3330
_reflns_number_total             4018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4009552_si_002.cif
_cod_data_source_block           d
_cod_database_code               1512062