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_2004298
_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     'C10 H20 O3 S2'
_chemical_formula_sum            'C10 H20 O3 S2'
_chemical_formula_weight         252.38
_chemical_melting_point          325-325K
_chemical_name_common            '[15]aneS2O3'
_chemical_name_systematic
;
 1,4,7-trioxa-10,13-dithiacyclopentdecane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                80.49(3)
_cell_angle_beta                 86.85(3)
_cell_angle_gamma                74.32(2)
_cell_formula_units_Z            2
_cell_length_a                   7.213(2)
_cell_length_b                   9.102(3)
_cell_length_c                   10.080(4)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      14
_cell_volume                     628.4(4)
_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      150.0(2)
_diffrn_measurement_device       'Stoe Stadi-4 four circle diffractometer'
_diffrn_measurement_method
'\w-2\q scans with on-line profile fitting (Clegg, 1981)'
_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  0.0127
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            3173
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.87
_diffrn_standards_decay_%        <0.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.410
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.776
_exptl_absorpt_correction_type   'semi-empirical (\y scans)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             272
_exptl_crystal_size_max          0.540
_exptl_crystal_size_mid          0.424
_exptl_crystal_size_min          0.386
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.223
_refine_ls_extinction_coef       0.008(2)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.037
_refine_ls_goodness_of_fit_obs   1.032
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_restrained_S_obs      1.032
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_obs          0.0248
_refine_ls_shift/esd_max         -0.062
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.034P)^2^+0.242P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0666
_refine_ls_wR_factor_obs         0.0622
_reflns_number_observed          1998
_reflns_number_total             2173
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1189.cif
_cod_data_source_block           15s2o3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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^)+(0.034P)^2^+0.242P] 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^)+(0.034P)^2^+0.242P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2004298