Studies on the double alkylation of 2,2-disubstituted-1,3-dithiacycloalkane-S-oxides: synthesis of tertiary thiol derivatives
Fuchs, Christian; Edgar, Mark; Elsegood, Mark R. J.; Weaver, George W.; RSC Advances 3 (2013) 21911–; doi:10.1039/c3ra43688h

data_7239230
_publ_section_title
;
 Studies on the double alkylation of
 2,2-disubstituted-1,3-dithiacycloalkane-S-oxides: synthesis of tertiary
 thiol derivatives
;
_journal_issue                   44
_journal_name_full               'RSC Advances'
_journal_page_first              21911
_journal_paper_doi               10.1039/c3ra43688h
_journal_volume                  3
_journal_year                    2013
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C20 H30 O S2'
_chemical_formula_sum            'C20 H30 O S2'
_chemical_formula_weight         350.56
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 90.152(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.490(3)
_cell_length_b                   20.303(6)
_cell_length_c                   11.090(3)
_cell_measurement_reflns_used    9628
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.35
_cell_measurement_theta_min      2.40
_cell_volume                     1911.6(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX 2 CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0565
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19844
_diffrn_reflns_theta_full        29.73
_diffrn_reflns_theta_max         29.73
_diffrn_reflns_theta_min         1.00
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.938
_exptl_absorpt_correction_T_min  0.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/1, Sheldrick, G.M., (2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.56
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881; 5074 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.30(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         10576
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0793
_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^)+(0.1512P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2225
_reflns_number_gt                8841
_reflns_number_total             10576
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3ra43688h.txt
_cod_data_source_block           24b
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7239230