8,10-Diiodo-2,6-dioxo-4λ^3^-ioda-3,5-dioxatricyclo[5.3.1.0^4,11^]undeca-1(11),7,9-triene-9-carboxylic acid
Sheng, Daopeng; Han, Lu; Zhang, Yi; Yang, Yanzhao; Acta Crystallographica Section E 68 (2012) o706–; doi:10.1107/S1600536812005351

data_2233813
_publ_section_title
;
 8,10-Diiodo-2,6-dioxo-4\l^3^-ioda-3,5-dioxatricyclo[5.3.1.0^4,11^]undeca-1(11),7,9-triene-9-carboxylic
 acid
;
_journal_coeditor_code           GK2447
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o706
_journal_paper_doi               10.1107/S1600536812005351
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C9 H I3 O6, 2H2 O'
_chemical_formula_moiety         'C9 H I3 O6, 2(H2 O)'
_chemical_formula_sum            'C9 H5 I3 O8'
_chemical_formula_weight         621.83
_chemical_melting_point          573
_chemical_name_common
;
5,7-Diiodo-1,4-dioxo-1<i>H</i>,4<i>H</i>-2a\l^3^-ioda-2,3-
dioxacyclopenta[<i>cd</i>]indene-6-carboxylic acid dihydrate
;
_chemical_name_systematic
;
8,10-diiodo-2,6-dioxo-4\l^3^-ioda-3,5-dioxatricyclo[5.3.1.0^4,11^]undeca-
1(11),7,9-triene-9-carboxylic acid
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 127.4236(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7667(8)
_cell_length_b                   11.9890(6)
_cell_length_c                   9.7419(5)
_cell_measurement_reflns_used    3350
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.43
_cell_volume                     1369.68(12)
_computing_cell_refinement       'APEX2 (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'APEX2 (Bruker, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4078
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         2.43
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.879
_exptl_absorpt_correction_T_max  0.492
_exptl_absorpt_correction_T_min  0.217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(APEX2; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.360
_refine_diff_density_min         -2.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.228
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0157P)^2^+40.7765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                1515
_reflns_number_total             1547
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gk2447.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2233813
_cod_database_fobs_code          2233813