Role of different molecular fragments in formation of the supramolecular architecture of the crystal of 1,1-dioxo-tetrahydro-1λ6-thiopyran-3-one
Shishkin, Oleg V.; Medvediev, Volodymyr V.; Zubatyuk, Roman I.; Shyshkina, Olena O.; Kovalenko, Nataliya V.; Volovenko, Julian M.; CrystEngComm 14 (2012) 8698–; doi:10.1039/c2ce26332g

data_7214735
_publ_section_title
;
 Role of different molecular fragments in formation of the supramolecular
 architecture of the crystal of 1,1-dioxo-tetrahydro-1\l6-thiopyran-3-one
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              8698
_journal_paper_doi               10.1039/c2ce26332g
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C5 H8 O3 S'
_chemical_formula_sum            'C5 H8 O3 S'
_chemical_formula_weight         148.17
_chemical_name_systematic
;
1,1-Dioxo-tetrahydro-1?6-thiopyran-3-one
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-07-20
_audit_creation_method
;
Olex2 1.1
(compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                103.502(12)
_cell_angle_beta                 93.207(11)
_cell_angle_gamma                107.717(12)
_cell_formula_units_Z            2
_cell_length_a                   5.6790(8)
_cell_length_b                   5.8215(8)
_cell_length_c                   10.7072(14)
_cell_measurement_reflns_used    1172
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8925
_cell_measurement_theta_min      3.7948
_cell_volume                     324.78(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.860
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_details
;
1 omega -86.00 -59.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- -20.7749 136.0000 98.0000 27

2 omega -2.00 91.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 22.1812 37.0000 -90.0000 93

3 omega 44.00 79.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 22.1812 179.0000 150.0000 35

4 omega 1.00 80.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 22.1812 -132.0000 31.0000 79

5 omega -45.00 52.00 1.0000 1.5000
omega____ theta____ kappa____ phi______ frames
- 22.1812 -37.0000 90.0000 97
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1120456000
_diffrn_orient_matrix_UB_12      -0.0112619000
_diffrn_orient_matrix_UB_13      0.0278538000
_diffrn_orient_matrix_UB_21      0.0695155000
_diffrn_orient_matrix_UB_22      0.0435776000
_diffrn_orient_matrix_UB_23      0.0628846000
_diffrn_orient_matrix_UB_31      0.0115957000
_diffrn_orient_matrix_UB_32      0.1247154000
_diffrn_orient_matrix_UB_33      -0.0001990000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0145
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2058
_diffrn_reflns_theta_full        28.96
_diffrn_reflns_theta_max         28.96
_diffrn_reflns_theta_min         3.80
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.426
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             156
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         1473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0312P)^2^+0.1876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0987
_reflns_number_gt                1217
_reflns_number_total             1473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26332g.txt
_cod_data_source_block           vol89
_cod_database_code               7214735
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32