(<i>Z</i>)-4,5-Di-bromo-3,3,6,6-tetra-methyl-2,3,6,7-tetra-hydro-thiepine-1,1-dione.
Schollmeyer, Dieter; Detert, Heiner; IUCrData 8 (2023) x230042–; doi:10.1107/S2414314623000421

data_1569776
_publ_section_title
;
 (<i>Z</i>)-4,5-Di-bromo-3,3,6,6-tetra-methyl-2,3,6,7-tetra-hydro-thiepine-1,1-dione.
;
_journal_coeditor_code           BT4132
_journal_issue                   'Pt 1'
_journal_name_full               IUCrData
_journal_page_first              x230042
_journal_paper_doi               10.1107/S2414314623000421
_journal_volume                  8
_journal_year                    2023
_chemical_formula_iupac          'C10 H16 Br2 O2 S'
_chemical_formula_moiety         'C10 H16 Br2 O2 S'
_chemical_formula_sum            'C10 H16 Br2 O2 S'
_chemical_formula_weight         360.11
_chemical_name_systematic
;
(<i>Z</i>)-4,5-Dibromo-3,3,6,6-tetramethyl-2,3,6,7-tetrahydrothiepine-1,1-dione
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                94.804(6)
_cell_angle_beta                 102.448(5)
_cell_angle_gamma                99.356(5)
_cell_formula_units_Z            2
_cell_length_a                   5.9685(4)
_cell_length_b                   8.9642(6)
_cell_length_c                   12.4927(9)
_cell_measurement_reflns_used    18448
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.69
_cell_volume                     639.09(8)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (Stoe & Cie, 2019)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (Stoe & Cie, 2019)
;
_computing_data_reduction
;
X-Area Integrate 1.77.0.0 (Stoe & Cie, 2019)
;
_computing_publication_material
;
PLATON (Spek, 2020)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8129
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.112
_diffrn_reflns_theta_min         2.693
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    6.485
_exptl_absorpt_correction_T_max  0.5530
_exptl_absorpt_correction_T_min  0.0884
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(XRED; Stoe et al., 2019)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.871
_exptl_crystal_description       plate
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.670
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.894
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3038
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0307P)^2^+1.4492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                2686
_reflns_number_total             3038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4132.cif
_cod_data_source_block           I
_cod_database_code               1569776
_shelx_estimated_absorpt_t_min   0.098
_shelx_estimated_absorpt_t_max   0.625
_shelx_hkl_checksum              4976
_shelx_res_checksum              12618