<i>syn</i>-6,15-Dihydroxy-2,11-dithia[3.3]metacyclophane ethyl acetate monosolvate
Moriguchi, Tetsuji; Miyamoto, Daisuke; Jalli, Ventakaprasad; Yoza, Kenji; Tsuge, Akihiko; IUCrData 1 (2016) x160082–; doi:10.1107/S2414314616000821

data_1542497
_publ_section_title
;
 <i>syn</i>-6,15-Dihydroxy-2,11-dithia[3.3]metacyclophane ethyl acetate
 monosolvate
;
_journal_coeditor_code           BH4001
_journal_issue                   1
_journal_name_full               IUCrData
_journal_page_first              x160082
_journal_paper_doi               10.1107/S2414314616000821
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          'C16 H16 O2 S2, C4 H8 O2'
_chemical_formula_moiety         'C16 H16 O2 S2, C4 H8 O2'
_chemical_formula_sum            'C20 H24 O4 S2'
_chemical_formula_weight         392.51
_chemical_name_systematic
;
<i>syn</i>-6,15-Dihydroxy-2,11-dithia[3.3]metacyclophane
ethyl acetate monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'APEX2 v2010.1-2'
_cell_angle_alpha                90
_cell_angle_beta                 99.8180(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1691(9)
_cell_length_b                   13.1263(10)
_cell_length_c                   12.2750(9)
_cell_measurement_reflns_used    3174
_cell_measurement_temperature    120.(2)
_cell_measurement_theta_max      24.1402
_cell_measurement_theta_min      2.1782
_cell_volume                     1932.0(2)
_computing_cell_refinement
;
SAINT (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT (Bruker, 2009)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.6666
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18213
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+1.9210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                2628
_reflns_number_total             3400
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh4001sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 1542497.cif.'
_cod_database_code               1542497
_cod_database_fobs_code          1542497