Molecular Transformations of Unsaturated Thiacrown Ethers
Takahiro Tsuchiya; Yosuke Okada; Toshio Shimizu; Kazunori Hirabayashi; Nobumasa Kamigata; Journal of Organic Chemistry 73 (2008) 76–80; doi:10.1021/jo701757s

data_4023157
_publ_section_title
;
 Molecular Transformations of Unsaturated Thiacrown Ethers
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              76
_journal_page_last               80
_journal_paper_doi               10.1021/jo701757s
_journal_volume                  73
_journal_year                    2008
_chemical_formula_sum            'C14 H18 O2 S6'
_chemical_formula_weight         410.64
_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                97.196(12)
_cell_angle_beta                 94.448(13)
_cell_angle_gamma                118.116(8)
_cell_formula_units_Z            4
_cell_length_a                   11.025(3)
_cell_length_b                   11.127(2)
_cell_length_c                   18.890(4)
_cell_measurement_temperature    296(2)
_cell_volume                     2002.8(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_av_sigmaI/netI    0.0694
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9769
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         21.00
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.9347
_exptl_absorpt_correction_T_min  0.7713
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         4256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0822P)^2^+2.1873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1510
_refine_ls_wR_factor_ref         0.1661
_reflns_number_gt                3197
_reflns_number_total             4256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo701757s-File006.cif
_cod_data_source_block           Compound_12
_cod_database_code               4023157