Unusual intramolecular bridging reaction in thiacalix[4]arene series.
Kundrat, Ondrej; Dvorakova, Hana; Cisarova, Ivana; Pojarova, Michaela; Lhotak, Pavel; Organic letters 11 (2009) 4188–4191; doi:10.1021/ol901812m

data_1504168
_publ_section_title
;
 Unusual intramolecular bridging reaction in thiacalix[4]arene series.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4188
_journal_page_last               4191
_journal_paper_doi               10.1021/ol901812m
_journal_volume                  11
_journal_year                    2009
_chemical_formula_sum            'C39 H40 O6 S4'
_chemical_formula_weight         732.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.82(3)
_cell_angle_beta                 102.15(3)
_cell_angle_gamma                90.23(3)
_cell_formula_units_Z            4
_cell_length_a                   11.784(2)
_cell_length_b                   15.222(3)
_cell_length_c                   20.955(4)
_cell_measurement_temperature    173(2)
_cell_volume                     3605.6(13)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            28533
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.310
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellowish
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         14745
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0959P)^2^+3.2694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1943
_refine_ls_wR_factor_ref         0.2185
_reflns_number_gt                9564
_reflns_number_total             14745
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol901812m_si_002.cif
_cod_data_source_block           ok416a-2-lhotak-vscht
_cod_original_sg_symbol_H-M      p-1
_cod_database_code               1504168