Palladium-Catalyzed Synthesis of 4-Oxaspiro[2.4]heptanes via Central Attack of Oxygen Nucleophiles to π-Allylpalladium Intermediates.
Shintani, Ryo; Ito, Tomoaki; Hayashi, Tamio; Organic letters 14 (2012) 2410–2413; doi:10.1021/ol300852v

data_1507644
_publ_section_title
;
 Palladium-Catalyzed Synthesis of 4-Oxaspiro[2.4]heptanes via Central
 Attack of Oxygen Nucleophiles to \p-Allylpalladium Intermediates.
;
_journal_issue                   9
_journal_name_full               'Organic letters'
_journal_page_first              2410
_journal_page_last               2413
_journal_paper_doi               10.1021/ol300852v
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C22 H22 O5 '
_chemical_formula_sum            'C22 H22 O5'
_chemical_formula_weight         366.41
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            8
_cell_length_a                   8.28074(15)
_cell_length_b                   10.78047(19)
_cell_length_c                   41.1730(8)
_cell_measurement_reflns_used    25433
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      3.2
_cell_volume                     3675.52(12)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      93(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.104
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            30322
_diffrn_reflns_theta_full        68.18
_diffrn_reflns_theta_max         68.18
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552.00
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3349
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                2295
_reflns_number_total             3349
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol300852v_si_002.cif
_cod_data_source_block           '_11001yuki'
_cod_original_cell_volume        3675.52(11)
_cod_original_formula_sum        'C22 H22 O5 '
_cod_database_code               1507644