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_1514707
_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         'C17 H17 N O6 S'
_chemical_formula_sum            'C17 H17 N O6 S'
_chemical_formula_weight         363.38
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                98.61(6)
_cell_angle_beta                 91.40(8)
_cell_angle_gamma                91.03(3)
_cell_formula_units_Z            2
_cell_length_a                   5.707(7)
_cell_length_b                   7.877(11)
_cell_length_c                   18.99(3)
_cell_measurement_reflns_used    821
_cell_measurement_temperature    173
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      21.09
_cell_volume                     844(2)
_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 0.949
_diffrn_measured_fraction_theta_max 0.941
_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  0.1733
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11643
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         68.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.371
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             380.00
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.410
_refine_ls_extinction_coef       0.046(9)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2905
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.1261
_refine_ls_shift/su_max          0.034
_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         0.4028
_reflns_number_gt                1673
_reflns_number_total             2905
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c3sc50500f.txt
_cod_data_source_block           13
_cod_original_cell_volume        843(2)
_cod_database_code               1514707