Synthesis of All Stereoisomers of Sulfinylcalix[4]arenes
Naoya Morohashi; Hiroshi Katagiri; Nobuhiko Iki; Yusuke Yamane; Chizuko Kabuto; Tetsutaro Hattori; Sotaro Miyano; Journal of Organic Chemistry 68 (2003) 2324–2333; doi:10.1021/jo026801x

data_4022352
_publ_section_title
;
 Synthesis of All Stereoisomers of Sulfinylcalix[4]arenes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2324
_journal_page_last               2333
_journal_paper_doi               10.1021/jo026801x
_journal_volume                  68
_journal_year                    2003
_chemical_formula_sum            'C69 H73 Cl3 O6 S4'
_chemical_formula_weight         1232.93
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                84.004(3)
_cell_angle_beta                 78.644(3)
_cell_angle_gamma                68.0693(9)
_cell_formula_units_Z            2
_cell_length_a                   13.6278(7)
_cell_length_b                   14.325(1)
_cell_length_c                   18.048(1)
_cell_measurement_reflns_used    7714
_cell_measurement_temperature    223.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_cell_volume                     3202.7(4)
_computing_cell_refinement       P
_computing_data_collection       P
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.9421
_diffrn_measured_fraction_theta_max 0.9421
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       -17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26431
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_exptl_absorpt_coefficient_mu    0.324
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.38
_refine_ls_abs_structure_Flack   0.00000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.209
_refine_ls_number_parameters     734
_refine_ls_number_reflns         6854
_refine_ls_R_factor_gt           0.0626
_refine_ls_shift/su_max          1.0381
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      unit
_refine_ls_wR_factor_ref         0.0672
_reflns_number_gt                6854
_reflns_number_total             11863
_reflns_threshold_expression     F^2^>4.0\s(F^2^)
_cod_data_source_file            jo026801xsi20030127_123539_3.cif
_cod_data_source_block           compound_14
_cod_original_formula_sum        'C69 H73 Cl3 O6 S4 '
_cod_database_code               4022352