S-Alkylation of Thiacalixarenes: How the Regio- and Stereoselectivities Depend on the Starting Conformation
Ondrej Kundrat; Hana Dvorakova; Stanislav Böhm; Vaclav Eigner; Pavel Lhotak; Journal of Organic Chemistry 77 (2012) 2272–2278; doi:10.1021/jo202571h

data_4027039
_publ_section_title
;
 S-Alkylation of Thiacalixarenes: How the Regio- and Stereoselectivities
 Depend on the Starting Conformation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2272
_journal_page_last               2278
_journal_paper_doi               10.1021/jo202571h
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C37 H43 O4 S4, C F3 O3 S'
_chemical_formula_sum            'C38 H43 F3 O7 S5'
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_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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_cell_angle_gamma                98.4990(9)
_cell_formula_units_Z            4
_cell_length_a                   8.8000(2)
_cell_length_b                   18.1200(2)
_cell_length_c                   25.4650(4)
_cell_measurement_reflns_used    17816
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     4003.36(12)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
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_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
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_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
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_diffrn_reflns_limit_l_min       -33
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_diffrn_reflns_theta_min         1.140
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_type   none
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_exptl_crystal_description       prism
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_refine_diff_density_min         -0.78
_refine_ls_extinction_method     none
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_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.0062973
_refine_ls_shift/su_mean         2.9498725
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.07P)^2^ + 2.82P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_gt          0.1196
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_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              23
_reflns_limit_k_min              -23
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_reflns_limit_l_min              0
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_reflns_threshold_expression     I>2.0\s(I)
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_oxford_refine_ls_scale          0.3056(2)
_oxford_reflns_number_all        18346
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            jo202571h_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4027039