Palladium-catalyzed decarboxylative [4 + 3] cyclization of gamma-methylidene-delta-valerolactones with 1,1-dicyanocyclopropanes.
Shintani, Ryo; Murakami, Masataka; Tsuji, Takaoki; Tanno, Hideyuki; Hayashi, Tamio; Organic letters 11 (2009) 5642–5645; doi:10.1021/ol902326s

data_1504290
_publ_section_title
;
 Palladium-catalyzed decarboxylative [4 + 3] cyclization of
 gamma-methylidene-delta-valerolactones with 1,1-dicyanocyclopropanes.
;
_journal_issue                   24
_journal_name_full               'Organic letters'
_journal_page_first              5642
_journal_page_last               5645
_journal_paper_doi               10.1021/ol902326s
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C28 H32 N2 O3 '
_chemical_formula_sum            'C28 H32 N2 O3'
_chemical_formula_weight         444.57
_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                   12.587(3)
_cell_length_b                   12.897(4)
_cell_length_c                   30.669(7)
_cell_measurement_reflns_used    32286
_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     4979(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_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           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
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_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
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_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       unknown
_exptl_crystal_F_000             1904.00
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
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_refine_ls_number_reflns         28856
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0786
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_reflns_threshold_expression     F^2^>2.0\s(F^2^)
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_cod_data_source_block           '_90826yuki'
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_cod_original_formula_sum        'C28 H32 N2 O3 '
_cod_database_code               1504290