Crystal structure of the cage derivative pentacyclo[5.4.0.0^2,6^.0^3,10^.0^5,9^]undeca-8,11-dione ethylene dithioketal
Kotha, Sambasivarao; Sreenivasachary, Nampalli; Deodhar, Deepak; Shaikh, Mobin; Acta Crystallographica Section E 70 (2014) 246–248; doi:10.1107/S1600536814020790

data_2240022
_publ_section_title
;
 Crystal structure of the cage derivative
 pentacyclo[5.4.0.0^2,6^.0^3,10^.0^5,9^]undeca-8,11-dione ethylene
 dithioketal
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              246
_journal_page_last               248
_journal_paper_doi               10.1107/S1600536814020790
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C13 H14 O S2'
_chemical_formula_moiety         'C13 H14 O S2'
_chemical_formula_sum            'C13 H14 O S2'
_chemical_formula_weight         250.36
_chemical_name_systematic
;
Pentacyclo[5.4.0.0^2,6^.0^3,10^.0^5,9^]undeca-8,11-dione ethylene
dithioketal
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.405(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1332(2)
_cell_length_b                   13.9220(3)
_cell_length_c                   11.4066(3)
_cell_measurement_reflns_used    8769
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.7321
_cell_measurement_theta_min      3.4316
_cell_volume                     1110.40(5)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur-S'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0137
_diffrn_reflns_av_sigmaI/netI    0.0108
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7821
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  0.9032
_exptl_absorpt_correction_T_min  0.8689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0452P)^2^+0.6547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0821
_reflns_number_gt                1828
_reflns_number_total             1963
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gw2148sup1.cf
_cod_data_source_block           2
_cod_database_code               2240022
_cod_database_fobs_code          2240022