γ-Methylidene-δ-valerolactones as a Coupling Partner for Cycloaddition: Palladium-Catalyzed [4 + 3] Cycloaddition with Nitrones
Ryo Shintani; Masataka Murakami; Tamio Hayashi; Journal of the American Chemical Society 129 (2007) 12356–12357; doi:10.1021/ja073997f

data_4110017
_publ_section_title
;
 \g-Methylidene-\d-valerolactones as a Coupling Partner for Cycloaddition:
 Palladium-Catalyzed [4 + 3] Cycloaddition with Nitrones
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12356
_journal_page_last               12357
_journal_paper_doi               10.1021/ja073997f
_journal_volume                  129
_journal_year                    2007
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C33 H30 Cl N O5 '
_chemical_formula_sum            'C33 H30 Cl N O5'
_chemical_formula_weight         556.06
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 106.781(18)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   9.509(4)
_cell_length_b                   12.566(6)
_cell_length_c                   12.510(8)
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_cell_measurement_temperature    123.1
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.2
_cell_volume                     1431.2(13)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
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_diffrn_measured_fraction_theta_max 0.996
_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  0.050
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_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_theta_max         27.47
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
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_exptl_crystal_description       prism
_exptl_crystal_F_000             584.00
_exptl_crystal_size_max          0.50
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_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.76
_refine_diff_density_min         -1.08
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2915 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    refall
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_refine_ls_number_reflns         10085
_refine_ls_R_factor_gt           0.0520
_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
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_reflns_threshold_expression     F^2^>2.0\s(F^2^)
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_cod_data_source_block           '_70528yuki'
_cod_original_cell_volume        1431.1(13)
_cod_original_formula_sum        'C33 H30 Cl N O5 '
_cod_database_code               4110017