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_4023155
_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 H14 O S7'
_chemical_formula_weight         422.67
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.133(6)
_cell_length_b                   17.525(12)
_cell_length_c                   25.441(12)
_cell_measurement_temperature    296(2)
_cell_volume                     4072(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0945
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13183
_diffrn_reflns_theta_full        20.00
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.7478
_exptl_absorpt_correction_T_min  0.7478
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0047(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         1883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0828P)^2^+2.9383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                1581
_reflns_number_total             1883
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo701757s-File004.cif
_cod_data_source_block           Compound_6
_cod_database_code               4023155