Synthesis of functional 1,2-dithiolanes from 1,3-bis-<i>tert</i>-butyl thioethers.
Scheutz, Georg M.; Rowell, Jonathan L.; Wang, Fu-Sheng; Abboud, Khalil A.; Peng, Chi-How; Sumerlin, Brent S.; Organic & biomolecular chemistry 18 (2020) 6509–6513; doi:10.1039/d0ob01577f

data_7157667
_publ_section_title
;
 Synthesis of functional 1,2-dithiolanes from 1,3-bis-<i>tert</i>-butyl
 thioethers.
;
_journal_issue                   33
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              6509
_journal_page_last               6513
_journal_paper_doi               10.1039/d0ob01577f
_journal_volume                  18
_journal_year                    2020
_chemical_formula_sum            'C15 H30 O S2'
_chemical_formula_weight         290.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-06-22 deposited with the CCDC.	2020-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.0392(2)
_cell_length_b                   8.4897(3)
_cell_length_c                   38.3953(13)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     1642.60(10)
_computing_cell_refinement       'Bruker APEX3 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2014)'
_computing_data_reduction        'Bruker Apex3 SAINT (Bruker, 2014)'
_computing_molecular_graphics    'XP in SHELXTL-plus, Bruker 2014'
_computing_publication_material  'SHELXL2014/7, Sheldrick, G. M. 2014'
_computing_structure_refinement  'SHELXL2014/7, Sheldrick G. M. 2014'
_computing_structure_solution    'SHELXL2014/7, Sheldrick G. M. 2014'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            22184
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         31.154
_diffrn_reflns_theta_min         2.457
_diffrn_source                   'I\mS microsource 3.0'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_correction_T_min  0.9490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Sheldrick, G. M., sadabs (2014). Acta Cryst. C71, 3--8.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       plate
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.052
_exptl_transmission_factor_max   0.5648
_exptl_transmission_factor_min   0.5159
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
; 
 Flack x determined using 1758 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.006(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         4854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0301P)^2^+0.3170P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0712
_reflns_Friedel_coverage         0.667
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.879
_reflns_number_gt                4580
_reflns_number_total             4854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob01577f2.cif
_cod_data_source_block           georg7
_cod_depositor_comments
'Adding full bibliography for 7157667--7157668.cif.'
_cod_database_code               7157667
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.984
_shelx_res_checksum              44949
_publcif_funding_html
;
;