Formal [4+1] annulation of alpha,alpha-dialkyl beta-oxo amides and dimethylsulfoxonium methylide: a synthetic route to beta-hydroxy-gamma-lactams
Dingyuan Zhang; Qian Zhang; Ning Zhang; Rui Zhang; Yongjiu Liang; Dewen Dong; Chem.Commun. 49 (2013) 7358–; doi:10.1039/c3cc43317j

data_7109617
_publ_section_title
;
 Formal [4+1] annulation of alpha,alpha-dialkyl beta-oxo amides and
 dimethylsulfoxonium methylide: a synthetic route to
 beta-hydroxy-gamma-lactams
;
_journal_name_full               Chem.Commun.
_journal_page_first              7358
_journal_paper_doi               10.1039/c3cc43317j
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C14 H17 N O2'
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.790(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6775(18)
_cell_length_b                   18.791(4)
_cell_length_c                   7.5798(16)
_cell_measurement_temperature    273(2)
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_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
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_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
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_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
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_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.168
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_refine_ls_extinction_method     none
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.2602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc43317j.txt
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_cod_original_cell_volume        1233.2(4)
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