(4a<i>SR</i>,7<i>SR</i>,9a<i>SR</i>)-7-<i>tert</i>-Butyl-9a-methyl-5,5-dioxo-1,2,4a,9a-tetrahydro-8-oxa-5λ^6^-thiabenzocycloheptan-9-one
Zeller, Matthias; Hunter, Allen D.; Sampson, Paul; Chumachenko, Nataliya; Acta Crystallographica Section E 62 (2006) o368–o369; doi:10.1107/S1600536805041140

data_2207894
_publ_section_title
(4a<i>SR</i>,7<i>SR</i>,9a<i>SR</i>)-7-<i>tert</i>-Butyl-9a-methyl-5,5-dioxo-1,2,4a,9a-tetrahydro-8-oxa-5\l^6^-thiabenzocycloheptan-9-one
_journal_coeditor_code           SJ6181
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o368
_journal_page_last               o369
_journal_paper_doi               10.1107/S1600536805041140
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C14 H22 O4 S'
_chemical_formula_moiety         'C14 H22 O4 S'
_chemical_formula_sum            'C14 H22 O4 S'
_chemical_formula_weight         286.38
_chemical_name_systematic
;
(4aSR,7SR,9aSR)-7-tert-Butyl-9a-methyl-5,5-dioxo-1,2,4a,9a-tetrahydro-8-oxa-
5\l^6^-thiabenzocycloheptan-9-one
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.539(2)
_cell_angle_beta                 90.278(2)
_cell_angle_gamma                100.160(2)
_cell_formula_units_Z            2
_cell_length_a                   5.6949(5)
_cell_length_b                   11.1309(10)
_cell_length_c                   12.3085(11)
_cell_measurement_reflns_used    6500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      3.19
_cell_volume                     707.08(11)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11949
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.8702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS in SAINT-Plus; Bruker, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.386
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         11919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.3942P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1176
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                11372
_reflns_number_total             11919
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj6181.cif
_cod_data_source_block           II
_cod_original_cell_volume        707.07(11)
_cod_database_code               2207894
_cod_database_fobs_code          2207894