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_7108908
_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 H32 N O6 S'
_chemical_formula_weight         558.65
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.90(3)
_cell_angle_beta                 86.02(3)
_cell_angle_gamma                87.63(3)
_cell_formula_units_Z            2
_cell_length_a                   9.2454(18)
_cell_length_b                   12.053(2)
_cell_length_c                   14.310(3)
_cell_measurement_reflns_used    3751
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9064
_cell_measurement_theta_min      2.7226
_cell_volume                     1493.6(6)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        crystalclear
_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      113(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15369
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
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_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.9703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.067(6)
_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         7008
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_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1550
_reflns_number_gt                3810
_reflns_number_total             7008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc38264h.txt
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed to 'constr'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1493.7(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7108908