Radical-Mediated 5-Exo-Trig Cyclizations of 3-Silylhepta-1,6-dienes
Philippe James; Kurt Schenk; Yannick Landais; Journal of Organic Chemistry 71 (2006) 3630–3633; doi:10.1021/jo060024+

data_4021658
_publ_section_title
;
 Radical-Mediated 5-Exo-Trig Cyclizations of 3-Silylhepta-1,6-dienes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3630
_journal_page_last               3633
_journal_paper_doi               10.1021/jo060024+
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C30 H36 O4 S Se Si'
_chemical_formula_weight         599.70
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Kurt Schenk'
_audit_contact_author_address
;
    Kurt Schenk
    LCr1 - IPMC - FSB - EPFL
    BSP Dorigny, Room 521
    CH-1015 Lausanne
    Suisse
;
_audit_contact_author_email      Kurt:Schenk@EPFL.CH
_audit_creation_date             2-05-2005
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 119.869(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   28.734(5)
_cell_length_b                   9.253(5)
_cell_length_c                   25.670(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5918(4)
_computing_cell_refinement       'Stoe X_Area'
_computing_data_collection       'Stoe X_Area'
_computing_data_reduction        'Stoe X_Area'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22031
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.412
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2496
_refine_diff_density_max         3.078
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.002(2)
_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   3.204
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         5651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      3.204
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.1419
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.009
_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          0.4052
_refine_ls_wR_factor_ref         0.4093
_reflns_number_gt                4677
_reflns_number_total             5651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo060024+si20060110_111322.cif
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4021658