Novel synthesis of 1-aryl-3-chloro-3-phenylazetidin-2-one-4-spiro-5′-4′-chloro-5′H-1′,2′,3′-dithiazoles and bis(2-oxo-azetidin-4-yl) trisulfides
Jeon, Moon-Kook; Kim, Kyongtae; Park, Yung Ja; Chemical Communications  (2001) 1412–; doi:10.1039/b103974c

data_7114728
_publ_section_title
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 Novel synthesis of
 1-aryl-3-chloro-3-phenylazetidin-2-one-4-spiro-5&#x2032;-4&#x2032;-chloro-5&#x2032;H-1&#x2032;,2&#x2032;,3&#x2032;-dithiazoles
 and bis(2-oxo-azetidin-4-yl) trisulfides
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1412
_journal_paper_doi               10.1039/b103974c
_journal_year                    2001
_chemical_formula_sum            'C16 H9 Cl3 N2 O S2'
_chemical_formula_weight         415.72
_space_group_IT_number           13
_symmetry_cell_setting           P2/k
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 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                 113.080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.946(2)
_cell_length_b                   7.4460(5)
_cell_length_c                   15.026(3)
_cell_measurement_temperature    295(2)
_cell_volume                     1744.2(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_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  0.0088
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3189
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.770
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PRISM
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.622mm
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.282
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+1.6903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1257
_reflns_number_gt                2499
_reflns_number_total             3057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103974c.txt
_cod_data_source_block           a
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+1.6903P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+1.6903P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               7114728