Multicomponent Radical Processes: Synthesis of Substituted Piperidinones
Edouard Godineau; Yannick Landais; Journal of the American Chemical Society 129 (2007) 12662–12663; doi:10.1021/ja075755l

data_4110073
_publ_contact_author_address
;
LCr1-IPMC-FSB
\'Ecole Polytechnique F\'ed\'erale de Lausanne
Le Cubotron, Room 521
Dorigny
CH-1015 Lausanne
Switzerland
;
_publ_contact_author_email       Kurt.Schenk@EPFL.CH
_publ_contact_author_fax         '+41 21 693 0405'
_publ_contact_author_name        'Kurt J. Schenk'
_publ_contact_author_phone       '+41 21 693 0635'
_publ_section_title
;
 Multicomponent Radical Processes: Synthesis of Substituted Piperidinones
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12662
_journal_page_last               12663
_journal_paper_doi               10.1021/ja075755l
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C20 H27 N O4'
_chemical_formula_sum            'C20 H27 N O4'
_chemical_formula_weight         345.43
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             19/3/2007
_audit_creation_method           'from SHELXL97 CIF and IUCr SHELXL97-template'
_cell_angle_alpha                75.690(12)
_cell_angle_beta                 80.240(12)
_cell_angle_gamma                80.226(12)
_cell_formula_units_Z            2
_cell_length_a                   6.1617(9)
_cell_length_b                   9.7621(15)
_cell_length_c                   16.390(3)
_cell_measurement_reflns_used    21140
_cell_measurement_temperature    94(1)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.18
_cell_volume                     933.0(3)
_computing_cell_refinement       'X_Area, 1.36 (Stoe, 2006)'
_computing_data_collection       'X_Area, 1.36 (Stoe, 2006)'
_computing_data_reduction        'X_Area, 1.36 (Stoe, 2006)'
_computing_molecular_graphics    'Bruker SHELXTL, (Bruker, 1996)'
_computing_publication_material  'Bruker SHELXTL, PLATON (Spek, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      94(1)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      ' 360 frames, detector distance = 100 mm'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17762
_diffrn_reflns_theta_full        29.31
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         2.17
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           43
_diffrn_source_power             2.37
_diffrn_source_voltage           55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.9942
_exptl_absorpt_correction_T_min  0.9710
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Stoe XRed32 1.31, Stoe (2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       platelet
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.333
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.416
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.022(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   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         5057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0493
_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^)+(0.0535P)^2^+0.3980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1244
_reflns_number_gt                3948
_reflns_number_total             5057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja075755lsi20070808_042509.cif
_cod_data_source_block           Structure_piperidinone_10a
_cod_database_code               4110073