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

data_4028900
_publ_section_title
;
 Molecular Transformations of Unsaturated Thiacrown Ethers
;
_journal_issue                   1
_journal_name_full               'The 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            'C12 H12 S6'
_chemical_formula_weight         348.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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                100.96
_cell_angle_beta                 101.06
_cell_angle_gamma                100.08
_cell_formula_units_Z            4
_cell_length_a                   9.121
_cell_length_b                   9.651
_cell_length_c                   18.764
_cell_measurement_temperature    293(2)
_cell_volume                     1552.675
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9787
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.860
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.90(7)
_refine_ls_extinction_coef       0.0000(3)
_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   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         7351
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          7.396
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+2.2992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                6906
_reflns_number_total             7351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo701757ssup3.cif
_cod_data_source_block           Compound_7
_cod_original_cell_volume        1552.6
_cod_database_code               4028900
_cod_duplicate_entry 4023156