#------------------------------------------------------------------------------
#$Date: 2019-04-05 12:48:19 +0300 (Fri, 05 Apr 2019) $
#$Revision: 214500 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/28/2242891.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2242891
loop_
_publ_author_name
'Harlow, Richard L.'
'Oliver, Allen G.'
'Baker, Jonathan M.'
'Marshall, William J.'
'Sammes, Michael P.'
_publ_section_title
;
 Comparison of the C---H···O bonding in two
 crystalline phases of 1,4-dithiane 1,1,4,4-tetraoxide
;
_journal_coeditor_code           JJ2210
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              576
_journal_page_last               579
_journal_paper_doi               10.1107/S2056989019004407
_journal_volume                  75
_journal_year                    2019
_chemical_formula_moiety         'C4 H8 O4 S2'
_chemical_formula_sum            'C4 H8 O4 S2'
_chemical_formula_weight         184.22
_chemical_name_systematic
;
1,4-Dithiane 1,1,4,4-tetraoxide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.138(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.1308(5)
_cell_length_b                   5.7245(4)
_cell_length_c                   8.3760(6)
_cell_measurement_reflns_used    4318
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      3.82
_cell_measurement_theta_min      29.06
_cell_volume                     341.84(4)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009), Crystalmaker (Palmer,
2014)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015)
;
_computing_structure_solution
;
OLEX2 (Dolomanov et al.,  2009)
;
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.34
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Photon-2'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14904
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         31.378
_diffrn_reflns_theta_min         3.811
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_T_max  0.8623
_exptl_absorpt_correction_T_min  0.8108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al.,  2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_description       tablet
_exptl_crystal_F_000             192
_exptl_crystal_size_max          0.044
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.444
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0281
_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/[σ²(Fo²)+(0.0197P)²+0.3362P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                957
_reflns_number_total             1041
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jj2210sup1.cif
_cod_data_source_block           14-disulphone-phase2
_cod_database_code               2242891
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.945
_shelx_estimated_absorpt_t_max   0.979
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
S S1 0.19891(5) 0.14315(6) 0.54564(4) 0.01294(10) Uani d 1
O O1 0.35411(15) 0.14742(19) 0.65934(13) 0.0194(2) Uani d 1
O O2 0.19584(15) 0.31562(19) 0.41982(12) 0.0186(2) Uani d 1
C C1 0.1857(2) -0.1390(2) 0.45787(17) 0.0149(3) Uani d 1
C C2 -0.0137(2) 0.1639(3) 0.65211(17) 0.0147(3) Uani d 1
H H1A 0.186(3) -0.247(4) 0.541(2) 0.024(5) Uiso d 1
H H1B 0.299(3) -0.156(3) 0.401(2) 0.020(5) Uiso d 1
H H2A -0.006(3) 0.049(3) 0.734(2) 0.016(4) Uiso d 1
H H2B -0.008(3) 0.314(4) 0.696(2) 0.024(5) Uiso d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0037 0.0017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0123 0.0065 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1293 0.1308 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle
O1 S1 C1 . 108.75(7)
O1 S1 C2 . 108.51(7)
O2 S1 O1 . 118.00(7)
O2 S1 C1 . 108.65(7)
O2 S1 C2 . 108.65(7)
C1 S1 C2 . 103.29(7)
S1 C1 H1A . 107.1(13)
S1 C1 H1B . 105.4(12)
C2 C1 S1 3_556 111.72(10)
C2 C1 H1A 3_556 112.1(12)
C2 C1 H1B 3_556 111.5(11)
H1A C1 H1B . 108.6(16)
S1 C2 H2A . 106.2(11)
S1 C2 H2B . 103.3(12)
C1 C2 S1 3_556 111.98(10)
C1 C2 H2A 3_556 113.8(11)
C1 C2 H2B 3_556 110.6(12)
H2A C2 H2B . 110.4(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
S1 O1 . 1.4459(11)
S1 O2 . 1.4439(11)
S1 C1 . 1.7762(14)
S1 C2 . 1.7778(14)
C1 C2 3_556 1.5265(19)
C1 H1A . 0.93(2)
C1 H1B . 0.95(2)
C2 H2A . 0.952(19)
C2 H2B . 0.94(2)

_cod_database_fobs_code 2242891
