2,2-Dimethyl-5-(phenylthiomethylene)-1,3-dioxane-4,6-dione
Blake, Alexander J.; McNab, Hamish; Morrow, Mark; Acta Crystallographica Section C 50 (1994) 1716–1717; doi:10.1107/S0108270194004804

data_2010175
_publ_section_title
;
 2,2-Dimethyl-5-(phenylthiomethylene)-1,3-dioxane-4,6-dione
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1716
_journal_page_last               1717
_journal_paper_doi               10.1107/S0108270194004804
_journal_volume                  50
_journal_year                    1994
_chemical_formula_structural     'C13 H12 O4 S'
_chemical_formula_sum            'C13 H12 O4 S'
_chemical_formula_weight         264.29
_chemical_melting_point          407.5(5)
_chemical_name_common            '5-phenylthiomethylene (Meldrum's acid)'
_chemical_name_systematic
' 2,2-Dimethyl-5-(phenylthiomethylene)-1,3-dioxane-4,6-dione'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 110.744(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2742(14)
_cell_length_b                   7.1069(6)
_cell_length_c                   12.5036(13)
_cell_measurement_reflns_used    84
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      11
_cell_volume                     1269.3(2)
_computing_cell_refinement       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_collection       'DIF4 (Stoe & Cie, 1988a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1988b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1992)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Stoe Stadi-4'
_diffrn_measurement_method       '\w-2\q scans'
_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  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0453
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2333
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         2.85
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.258
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       Plate
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.250
_refine_ls_extinction_coef       0.0060(13)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1994)'
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.146
_refine_ls_hydrogen_treatment
' H atoms were included in calculated positions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.305
_refine_ls_restrained_S_obs      1.146
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_obs          0.0559
_refine_ls_shift/esd_max         -0.042
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
; calc w = 1/[\s^2^(F~o~^2^) + (0.0359P)^2^ + 4.4915P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1880
_refine_ls_wR_factor_obs         0.1356
_reflns_number_observed          1147
_reflns_number_total             1663
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            ha1114.cif
_cod_data_source_block           melsph
_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 '407-408' was changed to '407.5(5)' -
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 '407-408' was changed to '407.5(5)' -
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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2010175
_cod_database_fobs_code          2010175