Pseudopolymorphs of chelidamic acid and its dimethyl ester
Tutughamiarso, Maya; Pisternick, Thorsten; Egert, Ernst; Acta Crystallographica Section C 68 (2012) o344–o350; doi:10.1107/S0108270112031691

data_2018603
_publ_section_title
;
 Pseudopolymorphs of chelidamic acid and its dimethyl ester
;
_journal_coeditor_code           EG3095
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o344
_journal_page_last               o350
_journal_paper_doi               10.1107/S0108270112031691
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C9 H9 N O5, H2 O'
_chemical_formula_moiety         'C9 H9 N O5, H2 O'
_chemical_formula_sum            'C9 H11 N O6'
_chemical_formula_weight         229.19
_chemical_name_common            'chelidamic acid dimethyl ester monohydrate'
_chemical_name_systematic
;
dimethyl 4-hydroxypyridine-2,6-dicarboxylate monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.96(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.241(3)
_cell_length_b                   6.1519(12)
_cell_length_c                   20.710(4)
_cell_measurement_reflns_used    4497
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.84
_cell_measurement_theta_min      3.47
_cell_volume                     2089.6(8)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics
'Mercury (Macrae <i>et al.</i>, 2008) and XP (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       \w
_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  0.0796
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            5752
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.70
_diffrn_reflns_theta_min         3.47
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1951
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0477P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                1474
_reflns_number_total             1951
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3095.cif
_cod_data_source_block           IIa
_cod_original_cell_volume        2089.6(7)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               2018603
_cod_database_fobs_code          2018603