Crystal structure of 7,8,15,16,17-pentathiadispiro[5.2.5^9^.3^6^]heptadecane
Hofstetter, Robert; Elvers, Benedict J.; Potlitz, Felix; Link, Andreas; Schulzke, Carola; Acta Crystallographica Section E 75 (2019) 888–891; doi:10.1107/S2056989019007138

data_2242956
_publ_section_title
;
 Crystal structure of
 7,8,15,16,17-pentathiadispiro[5.2.5^9^.3^6^]heptadecane
;
_journal_coeditor_code           FY2136
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              888
_journal_page_last               891
_journal_paper_doi               10.1107/S2056989019007138
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C12 H20 S5'
_chemical_formula_moiety         'C12 H20 S5'
_chemical_formula_sum            'C12 H20 S5'
_chemical_formula_weight         324.58
_chemical_name_systematic
;
7,8,15,16,17-Pentathiadispiro[5.2.5^9^.3^6^]heptadecane
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 98.94(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4174(19)
_cell_length_b                   9.970(2)
_cell_length_c                   15.877(3)
_cell_measurement_reflns_used    16821
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      58.9
_cell_measurement_theta_min      6.3
_cell_volume                     1472.6(5)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2010)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2010)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2010)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
<i>CIFTAB</i> (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS2T'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16257
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.421
_diffrn_reflns_theta_min         3.126
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.357
_exptl_crystal_size_min          0.279
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         4048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+0.4842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0710
_reflns_number_gt                3534
_reflns_number_total             4048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fy2136sup1.cif
_cod_data_source_block           I
_cod_database_code               2242956
_cod_database_fobs_code          2242956
_shelx_estimated_absorpt_t_min   0.755
_shelx_estimated_absorpt_t_max   0.815
_shelx_hkl_checksum              93059
_shelx_res_checksum              21258