Redetermination of the Structures of 1,4,7-Trioxa-10,13-dithiacyclopentadecane and 1,4,7,10-Tetraoxa-13,16-dithiacyclooctadecane
Blake, A. J.; Radek, C.; Schröder, M.; Acta Crystallographica Section C 51 (1995) 2668–2671; doi:10.1107/S0108270195008079

data_2004299
_publ_section_title
;
 Redetermination of the Structures of
 1,4,7-Trioxa-10,13-dithiacyclopentadecane and
 1,4,7,10-Tetraoxa-13,16-dithiacyclooctadecane
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2668
_journal_page_last               2671
_journal_paper_doi               10.1107/S0108270195008079
_journal_volume                  51
_journal_year                    1995
_chemical_formula_structural     'C12 H24 O4 S2'
_chemical_formula_sum            'C12 H24 O4 S2'
_chemical_formula_weight         296.43
_chemical_melting_point          328.0(10)
_chemical_name_common            '[18]aneS2O4'
_chemical_name_systematic
;
1,4,7,10-Tetraoxa-13,16-dithiacyclooctadecane
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 124.351(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.9074(12)
_cell_length_b                   9.5181(8)
_cell_length_c                   12.5255(10)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      15
_cell_volume                     1565.7(2)
_computing_cell_refinement       'Stoe DIF4 (Stoe & Cie, 1990a)'
_computing_data_collection       'Stoe DIF4 (Stoe & Cie, 1990a)'
_computing_data_reduction        'Stoe REDU4 (Stoe & Cie, 1990b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Stoe Stadi-4 four circle diffractometer'
_diffrn_measurement_method
'\w-2\q scans [width (0.90 + 0.35tan\q)\% in \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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0136
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1268
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        <0.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Column
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.39
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.300
_refine_ls_extinction_coef       0.029(3)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.030
_refine_ls_goodness_of_fit_obs   1.060
_refine_ls_hydrogen_treatment    'H atoms in fixed, calculated positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1266
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.060
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_obs          0.0386
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.072P)^2^+0.636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1194
_refine_ls_wR_factor_obs         0.1058
_reflns_number_observed          998
_reflns_number_total             1268
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1189.cif
_cod_data_source_block           18s2o4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '327-329K' was changed to '328.0(10)'
- the average value was taken and precision was
estimated.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.072P)^2^+0.636P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.072P)^2^+0.636P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2004299
_cod_database_fobs_code          2004299