Molecular Rods Based on Oligo-spiro-thioketals.
Wessig, P.; Gerngroß, M; Freyse, D.; Bruhns, P.; Przezdziak, M.; Schilde, U.; Kelling, A.; The Journal of organic chemistry 81 (2016) 1125–1136; doi:10.1021/acs.joc.5b02670

data_4031913
_publ_section_title
;
 Molecular Rods Based on Oligo-spiro-thioketals.
;
_journal_issue                   3
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1125
_journal_page_last               1136
_journal_paper_doi               10.1021/acs.joc.5b02670
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C17 H28 S4'
_chemical_formula_sum            'C17 H28 S4'
_chemical_formula_weight         360.63
_chemical_melting_point          482
_chemical_name_systematic
;
 7,11,18,21-Tetrathiatrispiro[5.2.2.512.29.26]henicosane
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9887(2)
_cell_length_b                   10.5588(3)
_cell_length_c                   28.4505(9)
_cell_measurement_reflns_used    31043
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      1.93
_cell_volume                     1799.02(10)
_computing_cell_refinement       'X-AREA (Stoe, 2004)'
_computing_data_collection       'X-AREA (Stoe, 2004)'
_computing_data_reduction        'X-RED (Stoe, 2004)'
_computing_publication_material
; 
 SHELXL-2013 (Sheldrick, 2013)
 Diamond (Blankenburg, 2015)
 ORTEP for windows (Farrugia, 2013) 
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
; 
 360 frames, detector distance = 100 mm, 1 min exposure time
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scan, \d \w = 1.0 deg'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0150
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            4780
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.228
_diffrn_reflns_theta_min         3.691
_exptl_absorpt_coefficient_mu    0.52
_exptl_absorpt_correction_T_max  0.9232
_exptl_absorpt_correction_T_min  0.5522
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             776
_exptl_crystal_size_max          1.80
_exptl_crystal_size_mid          0.94
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0066(11)
_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   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         2401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0489P)^2^+0.7571P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                2172
_reflns_number_total             2401
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo5b02670_si_002.cif
_cod_data_source_block           br1
_cod_database_code               4031913