2<i>H</i>,10<i>H</i>-1,4-Dioxepino[5',6':4,5]thieno[3,2-<i>e</i>][1,4]dioxepine-5,7(3<i>H</i>,9<i>H</i>)-dione
Tomura, Masaaki; Ono, Katsuhiko; Kaiden, Masanori; Tsukamoto, Kenichi; Saito, Katsuhiro; Acta Crystallographica Section E 63 (2007) o4568–o4569; doi:10.1107/S1600536807054001

data_2216677
_publ_section_title
2<i>H</i>,10<i>H</i>-1,4-Dioxepino[5',6':4,5]thieno[3,2-<i>e</i>][1,4]dioxepine-5,7(3<i>H</i>,9<i>H</i>)-dione
_journal_coeditor_code           NG2356
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4568
_journal_page_last               o4569
_journal_paper_doi               10.1107/S1600536807054001
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C10 H8 O6 S'
_chemical_formula_moiety         'C10 H8 O6 S'
_chemical_formula_sum            'C10 H8 O6 S'
_chemical_formula_weight         256.22
_chemical_melting_point_gt       573
_chemical_name_systematic
;
2<i>H</i>,10<i>H</i>-1,4-Dioxepino[5',6':4,5]thieno[3,2-
<i>e</i>][1,4]dioxepine-5,7(3<i>H</i>,9<i>H</i>)-dione
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   20.301(2)
_cell_length_b                   6.9037(8)
_cell_length_c                   7.3463(8)
_cell_measurement_reflns_used    2531
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0088
_cell_volume                     1029.60(19)
_computing_cell_refinement
;
CrystalClear (Molecular Structure Corporation & Rigaku, 2001)
;
_computing_data_collection
;
CrystalClear (Molecular Structure Corporation & Rigaku,2001)
;
_computing_data_reduction
;
TEXSAN (Molecular Structure Corporation & Rigaku, 2000)
;
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 14.6199
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            7769
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.42
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.284
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1246
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1532P)^2^+1.2875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1506
_reflns_number_gt                1222
_reflns_number_total             1246
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ng2356.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>573' was changed to
'573' - it should be numeric and without a unit designator.

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

The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>573' was changed to
'573' - it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1029.6(2)
_cod_database_code               2216677
_cod_database_fobs_code          2216677