SmI2-H2O-mediated 5-exo/6-exo lactone radical cyclisation cascades
Irem Yalavac; Sarah E. Lyons; Michael R. Webb; David J. Procter; Chem.Commun. 50 (2014) 12863–; doi:10.1039/C4cc05404K

data_7115811
_publ_section_title
;
 SmI2-H2O-mediated 5-exo/6-exo lactone radical cyclisation cascades
;
_journal_name_full               Chem.Commun.
_journal_page_first              12863
_journal_paper_doi               10.1039/C4cc05404K
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C26 H33 Br O2'
_chemical_formula_weight         457.43
_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_method           SHELXL-97
_cell_angle_alpha                91.8580(10)
_cell_angle_beta                 97.4580(10)
_cell_angle_gamma                94.8630(10)
_cell_formula_units_Z            4
_cell_length_a                   11.0845(3)
_cell_length_b                   12.9326(3)
_cell_length_c                   15.6251(4)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.16
_cell_measurement_theta_min      3.43
_cell_volume                     2210.80(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19984
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         72.15
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    2.672
_exptl_absorpt_correction_T_max  0.8350
_exptl_absorpt_correction_T_min  0.712437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+1.6481P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                7565
_reflns_number_total             8306
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc05404k2.cif
_cod_data_source_block           s4056ma
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115811