Alkyldisulfanium Salts: Isolable, Electrophilic Sulfur Reagents Competent for Polyene Cyclizations.
Schevenels, Florian T.; Shen, Minxing; Snyder, Scott A.; Organic letters 19 (2017) 2–5; doi:10.1021/acs.orglett.6b02059

data_1544965
_publ_section_title
;
 Alkyldisulfanium Salts: Isolable, Electrophilic Sulfur Reagents Competent
 for Polyene Cyclizations.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              2
_journal_page_last               5
_journal_paper_doi               10.1021/acs.orglett.6b02059
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C8 H12 Cl7 F6 S2 Sb'
_chemical_formula_weight         656.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.836(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3672(9)
_cell_length_b                   12.0980(6)
_cell_length_c                   10.2133(6)
_cell_measurement_reflns_used    9758
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.985
_cell_measurement_theta_min      2.244
_cell_volume                     2125.9(2)
_computing_cell_refinement       'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX2 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.34A Bruker-AXS, Madison WI'
_computing_molecular_graphics
;
Bruker SHELXTL Bruker-AXS, Madison WI
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
and local programs
;
_computing_publication_material  'Bruker SHELXTL Bruker-AXS, Madison WI'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXT 2014/4 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2189
_diffrn_reflns_point_group_measured_fraction_full 0.500
_diffrn_reflns_point_group_measured_fraction_max 0.499
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         29.081
_diffrn_reflns_theta_min         2.244
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    3.033
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 - Bruker AXS, Madison WI'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2189
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0149P)^2^+11.9018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                2004
_reflns_number_total             2189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol6b02059_si_002.cif
_cod_data_source_block           flocl13
_cod_depositor_comments          'Adding full bibliography for 1544965.cif.'
_cod_database_code               1544965
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.793
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              1703
_shelx_hkl_checksum              50482