A potential intermediate for the aza-Corey-Chaykovsky reaction: synthesis, structure, and thermolysis of a pentacoordinate 1,2-thiazetidine 1-oxide.
Kano, Naokazu; Daicho, Yuya; Kawashima, Takayuki; Organic letters 8 (2006) 4625–4627; doi:10.1021/ol0618499

data_1506211
_publ_section_title
;
 A potential intermediate for the aza-Corey-Chaykovsky reaction:
 synthesis, structure, and thermolysis of a pentacoordinate
 1,2-thiazetidine 1-oxide.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              4625
_journal_page_last               4627
_journal_paper_doi               10.1021/ol0618499
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C25 H15 F12 N O S'
_chemical_formula_sum            'C25 H15 F12 N O S'
_chemical_formula_weight         605.44
_chemical_name_common            'Compound 8'
_chemical_name_systematic
; 
Tetracoordinate thiazetidine 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 109.7490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   34.902(9)
_cell_length_b                   9.072(2)
_cell_length_c                   33.401(9)
_cell_measurement_reflns_used    8868
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.1021
_cell_measurement_theta_min      3.0539
_cell_volume                     9954(4)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics
'ORTEP-3 for Windows ver 1.08 (Farrugia, 1997-2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_details
;
scan:
    Number of images: 720
               Slice: -74.0000 - 106.0000
         Image width: 0.2500
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 53.9593
              2theta: 15.7434
scan:
    Number of images: 720
               Slice: -74.0000 - 106.0000
         Image width: 0.2500
            Exp time: 15.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 53.9593
              2theta: 15.7434

;
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC8: Eulerian 3-circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0207
_diffrn_orient_matrix_UB_12      0.0100
_diffrn_orient_matrix_UB_13      0.0199
_diffrn_orient_matrix_UB_21      -0.0100
_diffrn_orient_matrix_UB_22      -0.0935
_diffrn_orient_matrix_UB_23      0.0576
_diffrn_orient_matrix_UB_31      0.0291
_diffrn_orient_matrix_UB_32      -0.0089
_diffrn_orient_matrix_UB_33      -0.0094
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            27679
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.12
_diffrn_source_current           40.0000
_diffrn_source_power             2.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  0.9648
_exptl_absorpt_correction_T_min  0.8495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998) Private communication
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4864
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         8307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0728P)^2^+1.0384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                5707
_reflns_number_total             8307
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol0618499si20060726_112731.cif
_cod_data_source_block           compound8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_cell_volume        9954(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1506211