Free-Radical Carbo-alkenylation of Enamides and Ene-carbamates.
Poittevin, Clément; Liautard, Virginie; Beniazza, Redouane; Robert, Frédéric; Landais, Yannick; Organic letters 15 (2013) 2814–2817; doi:10.1021/ol401147w

data_1512105
_publ_section_title
;
 Free-Radical Carbo-alkenylation of Enamides and Ene-carbamates.
;
_journal_issue                   11
_journal_name_full               'Organic letters'
_journal_page_first              2814
_journal_page_last               2817
_journal_paper_doi               10.1021/ol401147w
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C24 H27 N O4 S'
_chemical_formula_sum            'C24 H27 N O4 S'
_chemical_formula_weight         425.53
_chemical_name_common            CP254PPP
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3759(12)
_cell_length_b                   11.6984(12)
_cell_length_c                   15.9768(16)
_cell_measurement_reflns_used    5321
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.81
_cell_measurement_theta_min      1.74
_cell_volume                     2126.2(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker AXS Inc.)'
_computing_data_collection       'APEX2 2012.2 (Bruker AXS Inc.)'
_computing_data_reduction        'SAINT v7.68A (Bruker AXS Inc.)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX Duo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayer QUAZAR mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33042
_diffrn_reflns_theta_full        28.81
_diffrn_reflns_theta_max         28.81
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.9783
_exptl_absorpt_correction_T_min  0.9253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'translucent cube'
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5506
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.2437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                5321
_reflns_number_total             5506
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ol401147w_si_003.cif
_cod_data_source_block           mo_cp254pppjoseph_0m
_cod_original_sg_symbol_H-M      Pca21
_cod_database_code               1512105