Redetermination of ethyl (3a-<i>cis</i>)-3a,8b-dihydroxy-2-methyl-4-oxo-3a,8b-dihydro-4<i>H</i>-indeno[1,2-<i>b</i>]furan-3-carboxylate monohydrate
Pereira Silva, P. S.; Ghalib, Raza Murad; Mehdi, Sayed Hasan; Hashim, Rokiah; Sulaiman, Othman; Acta Crystallographica Section E 65 (2009) o2616–; doi:10.1107/S1600536809039403

data_2223627
_publ_section_title
;Redetermination of ethyl
 (3a-<i>cis</i>)-3a,8b-dihydroxy-2-methyl-4-oxo-3a,8b-dihydro-4<i>H</i>-indeno[1,2-<i>b</i>]furan-3-carboxylate
 monohydrate
;
_journal_coeditor_code           BT5075
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2616
_journal_paper_doi               10.1107/S1600536809039403
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C15 H14 O6, H2 O1'
_chemical_formula_moiety         'C15 H14 O6, H2 O1'
_chemical_formula_sum            'C15 H16 O7'
_chemical_formula_weight         308.28
_chemical_melting_point_gt       373
_chemical_melting_point_lt       376
_chemical_name_systematic
;
ethyl (3a-<i>cis</i>)-3a,8b-dihydroxy-2-methyl-
4-oxo-3a,8b-dihydro-4<i>H</i>-indeno[1,2-<i>b</i>]furan-3-carboxylate
monohydrate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 98.833(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.9740(4)
_cell_length_b                   16.7524(8)
_cell_length_c                   11.0041(5)
_cell_measurement_reflns_used    5159
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8569
_cell_measurement_theta_min      2.2329
_cell_volume                     1452.53(12)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0127
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            21608
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.23
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3509
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0682P)^2^+0.9584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1543
_reflns_number_gt                2820
_reflns_number_total             3509
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5075.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2223627
_cod_database_fobs_code          2223627