2,10,12-Trimethyl-12<i>H</i>-5,7-dioxa-6-thiadibenzo[<i>a</i>,<i>d</i>]cyclooctene 6-oxide
Dong, Su-Lan; Xu, Bing; Feng, Zhi-Qiang; Wang, Jin-Tang; Acta Crystallographica Section E 63 (2007) o2992–; doi:10.1107/S1600536807023859

data_2213826
_publ_section_title
;2,10,12-Trimethyl-12<i>H</i>-5,7-dioxa-6-thiadibenzo[<i>a</i>,<i>d</i>]cyclooctene
 6-oxide
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2992
_journal_paper_doi               10.1107/S1600536807023859
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C16 H16 O3 S'
_chemical_formula_moiety         'C16 H16 O3 S'
_chemical_formula_sum            'C16 H16 O3 S'
_chemical_formula_weight         288.36
_chemical_melting_point          401
_chemical_name_systematic
;
2,10,12-Trimethyl-12H-5,7-dioxa-6-thiadibenzo[a,d]cyclooctene 6-oxide
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.122(3)
_cell_length_b                   8.0880(16)
_cell_length_c                   25.343(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     2894.6(10)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '\w/2\q 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  0.021
_diffrn_reflns_av_sigmaI/netI    0.0499
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            3213
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  0.9576
_exptl_absorpt_correction_T_min  0.9149
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.142
_refine_ls_abs_structure_details 'Flack (1983), 208 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.06(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         2890
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1121
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0400P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                1444
_reflns_number_total             2890
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk2239.cif
_cod_data_source_block           I
_cod_database_code               2213826
_cod_database_fobs_code          2213826