Organocatalyzed [3 + 2] Annulation of Cyclopropenones and β-Ketoesters: An Approach to Substituted Butenolides with a Quaternary Center.
Li, Xuanyi; Han, Chunhua; Yao, Hequan; Lin, Aijun; Organic letters 19 (2017) 778–781; doi:10.1021/acs.orglett.6b03737

data_1545460
_publ_section_title
;
 Organocatalyzed [3 + 2] Annulation of Cyclopropenones and \b-Ketoesters:
 An Approach to Substituted Butenolides with a Quaternary Center.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              778
_journal_page_last               781
_journal_paper_doi               10.1021/acs.orglett.6b03737
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C26 H21 N O6'
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
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_cell_length_c                   10.403(10)
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_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      20.958
_cell_measurement_theta_min      2.5575
_cell_volume                     2196(4)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
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_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_Laue_measured_fraction_full 0.980
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_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
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_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.999
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_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.278
_exptl_absorpt_coefficient_mu    0.096
_exptl_crystal_colour            COLORLESS
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_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.162
_refine_diff_density_min         -0.162
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       0.0071(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         3893
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.1022
_refine_ls_R_factor_gt           0.0496
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0527P)^2^+0.1714P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
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_reflns_number_gt                2253
_reflns_number_total             3893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b03737_si_002.cif
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_shelx_estimated_absorpt_t_min   0.989
_shelx_estimated_absorpt_t_max   0.992
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