4,5-Dibromo-2,7-di-<i>tert</i>-butyl-9,9-dimethyl-9<i>H</i>-thioxanthene
Rubio, Omayra H.; Fuentes de Arriba, Angel L.; Sanz, Francisca; Muniz, Francisco M.; Morán, Joaquín R.; Acta Crystallographica Section E 68 (2012) o1814–; doi:10.1107/S1600536812020624

data_2235170
_publ_section_title
;
 4,5-Dibromo-2,7-di-<i>tert</i>-butyl-9,9-dimethyl-9<i>H</i>-thioxanthene
;
_journal_coeditor_code           NG5262
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1814
_journal_paper_doi               10.1107/S1600536812020624
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C23 H28 Br2 S'
_chemical_formula_moiety         'C23 H28 Br2 S'
_chemical_formula_sum            'C23 H28 Br2 S'
_chemical_formula_weight         496.33
_chemical_name_systematic
;
4,5-Dibromo-2,7-di-<i>tert</i>-butyl-9,9-dimethyl-9<i>H</i>-thioxanthene
;
_space_group_IT_number           110
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_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            16
_cell_length_a                   21.8234(2)
_cell_length_b                   21.8234
_cell_length_c                   18.8025(5)
_cell_measurement_reflns_used    6340
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      65.04
_cell_measurement_theta_min      4.05
_cell_volume                     8954.9(3)
_computing_cell_refinement       'SAINT (Bruker 2006)'
_computing_data_collection       'APEX2 (Bruker 2006)'
_computing_data_reduction        'SAINT (Bruker 2006)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26972
_diffrn_reflns_theta_full        67.10
_diffrn_reflns_theta_max         67.10
_diffrn_reflns_theta_min         4.05
_exptl_absorpt_coefficient_mu    5.477
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4032
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.825
_refine_ls_abs_structure_details 'Flack (1983), 2739 Friedel pairs'
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3272
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0690P)^2^+8.5510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                3038
_reflns_number_total             3272
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ng5262.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'I 41 cd'
_cod_database_code               2235170
_cod_database_fobs_code          2235170