A phosphine-catalyzed [3 + 2] annulation reaction of modified allylic compounds and N-tosylimines.
Zheng, Suqing; Lu, Xiyan; Organic letters 10 (2008) 4481–4484; doi:10.1021/ol801661y

data_1504880
_publ_section_title
;
 A phosphine-catalyzed [3 + 2] annulation reaction of modified allylic
 compounds and N-tosylimines.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              4481
_journal_page_last               4484
_journal_paper_doi               10.1021/ol801661y
_journal_volume                  10
_journal_year                    2008
_chemical_formula_sum            'C26 H24 Cl N O4 S'
_chemical_formula_weight         481.97
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.841(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9179(17)
_cell_length_b                   13.694(3)
_cell_length_c                   22.370(5)
_cell_measurement_reflns_used    3840
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      52.593
_cell_measurement_theta_min      4.722
_cell_volume                     2408.3(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      292(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            13451
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.278
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70129
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.435
_exptl_crystal_size_mid          0.402
_exptl_crystal_size_min          0.281
_refine_diff_density_max         0.258
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_refine_ls_extinction_method     none
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_refine_ls_number_parameters     308
_refine_ls_number_reflns         5212
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_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0638P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                3681
_reflns_number_total             5212
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol801661y_si_003.cif
_cod_data_source_block           cd26280
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
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_sg_symbol_H-M      P2(1)/c
_cod_database_code               1504880