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_1514706
_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_formula_moiety         'C15 H12 F N O3'
_chemical_formula_sum            'C15 H12 F N O3'
_chemical_formula_weight         273.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.309(4)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.6982(17)
_cell_length_b                   4.5311(5)
_cell_length_c                   19.448(3)
_cell_measurement_reflns_used    9159
_cell_measurement_temperature    173
_cell_measurement_theta_max      67.56
_cell_measurement_theta_min      4.01
_cell_volume                     1284.7(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r2'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla, et al., 2005)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 29.257
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15766
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             568.00
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.780
_refine_diff_density_min         -1.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2261
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.1206
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1764P)^2^+10.2369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.3223
_reflns_number_gt                2011
_reflns_number_total             2261
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3sc50500f.txt
_cod_data_source_block           14
_cod_database_code               1514706