Phosphine-catalyzed [3+2] annulation of α-substituted allenoates with ester-activated α,β-unsaturated imines: a novel variation of the Lu [3+2] cycloaddition reaction
Tian, Junjun; He, Zhengjie; Chemical Communications (Cambridge, United Kingdom) 49 (2013) 2058–2060; doi:10.1039/c3cc38264h

data_7108907
_publ_section_title
;
 Phosphine-catalyzed [3+2] annulation of \a-substituted allenoates with
 ester-activated \a,\b-unsaturated imines: a novel variation of the Lu
 [3+2] cycloaddition reaction
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   20
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2058
_journal_page_last               2060
_journal_paper_doi               10.1039/c3cc38264h
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C32 H33 N O6 S'
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_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
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_cell_angle_beta                 94.20(3)
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
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_diffrn_reflns_theta_max         27.92
_diffrn_reflns_theta_min         2.69
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_exptl_absorpt_correction_T_max  0.9786
_exptl_absorpt_correction_T_min  0.9696
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_exptl_absorpt_process_details   crystalclear
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_exptl_crystal_density_method    'not measured'
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_refine_ls_extinction_coef       0.052(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_number_reflns         6863
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_refine_ls_R_factor_all          0.0845
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_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc38264h.txt
_cod_data_source_block           r120522b1
_cod_original_cell_volume        1461.1(5)
_cod_original_sg_symbol_H-M      P-1
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