3,3'-Dihydroxy-5,5,5',5'-tetramethyl-2,2'-thiodicyclohex-2-en-1-one
Imashiro, Fumio; Acta Crystallographica Section C 62 (2006) o410–o411; doi:10.1107/S010827010601866X

data_2015430
_publ_section_title
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 3,3'-Dihydroxy-5,5,5',5'-tetramethyl-2,2'-thiodicyclohex-2-en-1-one
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_journal_coeditor_code           GA3008
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o410
_journal_page_last               o411
_journal_paper_doi               10.1107/S010827010601866X
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C16 H22 O4 S'
_chemical_formula_moiety         'C16 H22 O4 S'
_chemical_formula_sum            'C16 H22 O4 S'
_chemical_formula_weight         310.41
_chemical_melting_point          505.5(15)
_chemical_name_systematic
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3,3'-Dihydroxy-5,5,5',5'-tetramethyl-2,2'-thiodicyclohex-2-en-1-one
;
_space_group_IT_number           106
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4c -2ab'
_symmetry_space_group_name_H-M   'P 42 b c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3426(14)
_cell_length_b                   13.3426(14)
_cell_length_c                   9.049(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      13.6
_cell_volume                     1610.9(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
'MSC/AFC Diffractometer Control Software (Rigaku/MSC & Rigaku, 2001)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC & Rigaku, 2001)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC-7S'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1251
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0.41
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.9585
_exptl_absorpt_correction_T_min  0.8149
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             664
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.188
_refine_ls_abs_structure_details 'Flack (1983), ? Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(17)
_refine_ls_extinction_coef       0.014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1251
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0547P)^2^+0.1022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                1004
_reflns_number_total             1251
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga3008.cif
_cod_data_source_block           I
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '504--507' was changed to '505.5(15)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '504--507' was changed to '505.5(15)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2015430
_cod_database_fobs_code          2015430