(<i>rac</i>-5<i>RS</i>,7<i>RS</i>,8S<i>R</i>)-Spiro[7-methoxycarbonyl-1-aza-3-thiabicyclo[3.3.0]octane-8,1'-acenaphthylen]-2'-one
Sundar, T. V.; Parthasarathi, V.; Álvarez-Rúa. C.; García-Granda. S.; Saxena, A.; Pardasani, P.; Pardasani, R. T.; Acta Crystallographica Section E 58 (2002) o1405–o1407; doi:10.1107/S1600536802020846

data_2201534
_publ_section_title
(<i>rac</i>-5<i>RS</i>,7<i>RS</i>,8S<i>R</i>)-Spiro[7-methoxycarbonyl-1-aza-3-thiabicyclo[3.3.0]octane-8,1'-acenaphthylen]-2'-one
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1405
_journal_page_last               o1407
_journal_paper_doi               10.1107/S1600536802020846
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C19 H17 N O3 S'
_chemical_formula_moiety         'C19 H17 N O3 S'
_chemical_formula_sum            'C19 H17 N O3 S'
_chemical_formula_weight         339.40
_chemical_melting_point          445
_chemical_name_systematic
;
[rac-5RS,7RS,8SR]-Spiro-{7-methoxycarbonyl-1-aza-3-thia-bicyclo[3.3.0]
octane-8,1'-acenaphthylene}-2'-one
;
_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                 128.660(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.35970(10)
_cell_length_b                   14.7896(2)
_cell_length_c                   14.91990(10)
_cell_measurement_reflns_used    9012
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.251
_cell_measurement_theta_min      2.209
_cell_volume                     1612.73(12)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2000)'
_computing_data_reduction
'HKL DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics
'WinGX (Version 1.64.02; Farrugia, 1999) and PLATON (Spek, 2002)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0254
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21038
_diffrn_reflns_theta_full        68.21
_diffrn_reflns_theta_max         68.21
_diffrn_reflns_theta_min         4.83
_exptl_absorpt_coefficient_mu    1.928
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboidal
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0531P)^2^+0.4649P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                2567
_reflns_number_total             2926
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6181.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '445 K' was changed to '445' - the
value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '445 K' was changed to '445' - the
value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1612.73(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2201534
_cod_database_fobs_code          2201534