Redetermination and absolute configuration of pruniflorone M monohydrate
Fun, Hoong-Kun; Chantrapromma, Suchada; Boonnak, Nawong; Karalai, Chatchanok; Chantrapromma, Kan; Acta Crystallographica Section E 67 (2011) o1916–o1917; doi:10.1107/S1600536811025177

data_2231304
_publ_section_title
;
 Redetermination and absolute configuration of pruniflorone M
 monohydrate
;
_journal_coeditor_code           SJ5174
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1916
_journal_page_last               o1917
_journal_paper_doi               10.1107/S1600536811025177
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C18 H16 O6, H2 O'
_chemical_formula_moiety         'C18 H16 O6, H2 O'
_chemical_formula_sum            'C18 H18 O7'
_chemical_formula_weight         346.32
_chemical_melting_point_gt       508
_chemical_melting_point_lt       510
_chemical_name_common
;
Pruniflorone M monohydrate
;
_chemical_name_systematic
;
(2<i>R</i>)-5,10-Dihydroxy-2-hydroxymethyl-1,1-dimethyl-1<i>H</i>-
furo[2,3-<i>c</i>]xanthen-6-one monohydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.8887(3)
_cell_length_b                   15.6028(4)
_cell_length_c                   20.4857(5)
_cell_measurement_reflns_used    4981
_cell_measurement_temperature    100
_cell_measurement_theta_max      63.48
_cell_measurement_theta_min      5.30
_cell_volume                     3160.77(15)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX DUO CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13449
_diffrn_reflns_theta_full        63.48
_diffrn_reflns_theta_max         63.48
_diffrn_reflns_theta_min         5.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.951
_exptl_absorpt_correction_T_max  0.9126
_exptl_absorpt_correction_T_min  0.6272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.231
_refine_ls_abs_structure_details 'Flack (1983), 2102 Friedel pairs'
_refine_ls_abs_structure_Flack   0.06(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         4981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+0.9688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1204
_reflns_number_gt                4753
_reflns_number_total             4981
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5174.cif
_cod_data_source_block           I
_cod_database_code               2231304
_cod_database_fobs_code          2231304