Rapid and selective spiro-cyclisations of O-centred radicals onto aromatic acceptors
McBurney, Roy T.; Eisenschmidt, Annika; Slawin, Alexandra M. Z.; Walton, John C.; Chemical Science 4 (2013) 2028–; doi:10.1039/c3sc50500f

data_1514708
_publ_section_title
;
 Rapid and selective spiro-cyclisations of O-centred radicals onto
 aromatic acceptors
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              2028
_journal_paper_doi               10.1039/c3sc50500f
_journal_volume                  4
_journal_year                    2013
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C15 H8 F5 N O3'
_chemical_formula_sum            'C15 H8 F5 N O3'
_chemical_formula_weight         345.23
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 102.65(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   7.89(3)
_cell_length_b                   5.60(2)
_cell_length_c                   16.51(6)
_cell_measurement_reflns_used    366
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      5.49
_cell_volume                     712(5)
_computing_cell_refinement       'CrystalClear-SM Expert 2.1 b6'
_computing_data_collection       'CrystalClear-SM Expert 2.1 b6 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.1 b6'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1756
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7300
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             348.00
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.420
_refine_ls_extinction_coef       0.12(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2479
_refine_ls_number_restraints     1
_refine_ls_R_factor_gt           0.1561
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.4300
_reflns_number_gt                864
_reflns_number_total             2479
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3sc50500f.txt
_cod_data_source_block           1
_cod_database_code               1514708