Application of α-alkoxy bridgehead radical for coupling of oxygenated carbocycles.
Urabe, Daisuke; Yamaguchi, Hiroki; Inoue, Masayuki; Organic letters 13 (2011) 4778–4781; doi:10.1021/ol201758a

data_1502389
_publ_section_title
;
 Application of \a-alkoxy bridgehead radical for coupling of oxygenated
 carbocycles.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4778
_journal_page_last               4781
_journal_paper_doi               10.1021/ol201758a
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C17 H24 O4'
_chemical_formula_sum            'C17 H24 O4'
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_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 114.727(8)
_cell_angle_gamma                90.0000
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_cell_length_b                   10.05307(10)
_cell_length_c                   12.4057(2)
_cell_measurement_reflns_used    14941
_cell_measurement_temperature    123
_cell_measurement_theta_max      68.25
_cell_measurement_theta_min      3.75
_cell_volume                     1469.43(14)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO'
_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      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0217
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
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_diffrn_reflns_limit_l_min       -14
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_diffrn_reflns_theta_max         68.25
_diffrn_standards_number         0
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_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632.00
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_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.300
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_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_method     SHELXL
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_refine_ls_number_reflns         2682
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_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.5895P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                2471
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_cod_data_source_file            ol201758a_si_002.cif
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