3,9-Diisopropyl-2,4,8,10-tetrathiaspiro[5.5]undecane
Gâz, Şerban Andrei; Dobra, Ioana; Woiczechowski-Pop, Adrian; Varga, Richard A.; Grosu, Ion; Acta Crystallographica Section E 66 (2010) o2618–; doi:10.1107/S1600536810037281

data_2227707
_publ_section_title
;
 3,9-Diisopropyl-2,4,8,10-tetrathiaspiro[5.5]undecane
;
_journal_coeditor_code           JH2201
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2618
_journal_paper_doi               10.1107/S1600536810037281
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C13 H24 S4'
_chemical_formula_moiety         'C13 H24 S4'
_chemical_formula_sum            'C13 H24 S4'
_chemical_formula_weight         308.56
_chemical_melting_point_gt       416
_chemical_melting_point_lt       418
_chemical_name_systematic
;
3,9-Diisopropyl-2,4,8,10-tetrathiaspiro[5.5]undecane
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 128.418(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.701(5)
_cell_length_b                   10.241(3)
_cell_length_c                   12.063(3)
_cell_measurement_reflns_used    3441
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.53
_cell_volume                     1616.5(8)
_computing_cell_refinement       'SMART (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg & Putz, 2004)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7606
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  0.8573
_exptl_absorpt_correction_T_min  0.8393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.282
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         1432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0678
_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^)+(0.0592P)^2^+2.6050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1492
_refine_ls_wR_factor_ref         0.1525
_reflns_number_gt                1311
_reflns_number_total             1432
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jh2201.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2227707
_cod_database_fobs_code          2227707