Four novel spirooxazacamphorsultam derivatives
Wilke, Burkhardt I.; Goodenough, Angela K.; Bausch, Cory C.; Cline, Erika N.; Abrams, M. Leigh; Fayer, Effrat L.; Swenson, Dale C.; Cermak, Diana M.; Acta Crystallographica Section C 66 (2010) o600–o605; doi:10.1107/S0108270110041843

data_2017910
_publ_section_title
;
 Four novel spirooxazacamphorsultam derivatives
;
_journal_coeditor_code           GZ3184
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o600
_journal_page_last               o605
_journal_paper_doi               10.1107/S0108270110041843
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C13 H19 N O4 S'
_chemical_formula_moiety         'C13 H19 N O4 S'
_chemical_formula_sum            'C13 H19 N O4 S'
_chemical_formula_weight         285.35
_chemical_name_systematic
;
(7aS,10S,11aR)-12,12-dimethyl-6,6-dioxo-3,4,9,10-tetrahydro-7<i>H</i>-
7a,10-methano-
2<i>H</i>-1,3-oxazino[2,3-<i>i</i>][2,1]benzisothiazol-11(8<i>H</i>)-one
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.145(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.6970(9)
_cell_length_b                   6.9954(8)
_cell_length_c                   12.2852(13)
_cell_measurement_reflns_used    3030
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      1.0
_cell_volume                     654.81(13)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) and SCALEPACK'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15564
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.9
_diffrn_reflns_theta_min         2.7
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_T_max  0.9822
_exptl_absorpt_correction_T_min  0.9455
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.264
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3084
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.0370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0764
_reflns_number_gt                2783
_reflns_number_total             3084
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3184.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2017910
_cod_database_fobs_code          2017910