Palladium-Catalysed Atom-Economical Synthesis of Conjugated Dienals from Terminal Acetylenes and Acrolein
Hearne, Zoë; Li, Chao-Jun; Chem. Commun.  (2017) –; doi:10.1039/C7CC02767B

data_7120131
_publ_section_title
;
 Palladium-Catalysed Atom-Economical Synthesis of Conjugated Dienals from
 Terminal Acetylenes and Acrolein
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02767B
_journal_year                    2017
_chemical_formula_moiety         C10H9NO
_chemical_formula_sum            'C10 H9 N O'
_chemical_formula_weight         159.19
_chemical_name_systematic        (2E,4E)-5-(pyridin-3-yl)penta-2,4-dienal
_chemical_properties_physical    ', Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-16 deposited with the CCDC.
2017-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_length_b                   11.6684(12)
_cell_length_c                   7.2988(7)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54
_cell_measurement_theta_min      0.1
_cell_volume                     823.47(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       multi-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            33032
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.785
_diffrn_reflns_theta_min         2.736
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1, G. Sheldrick'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_description       needle
_exptl_crystal_F_000             336
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methylacetate'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.3100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1536
_reflns_number_total             2135
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {3912ed6f-5141-4bf3-993c-1fef587efc1e}
_cod_data_source_file            c7cc02767b3.cif
_cod_data_source_block           mo_DT95_0ma
_cod_database_code               7120131
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              19949
_shelx_hkl_checksum              12770