Tris[(6<i>S</i>)-6-hydroxy-4-<i>epi</i>-shikimic acid] monohydrate: an enantiomerically pure hydroxylated shikimic acid derived from methyl shikimate
Griesbeck, Axel G.; Miara, Claus; Neudörfl, Jörg-M.; Acta Crystallographica Section E 68 (2012) o3149–o3150; doi:10.1107/S1600536812041256

data_2236214
_publ_section_title
;
 Tris[(6<i>S</i>)-6-hydroxy-4-<i>epi</i>-shikimic acid] monohydrate: an
 enantiomerically pure hydroxylated shikimic acid derived from methyl
 shikimate
;
_journal_coeditor_code           GG2099
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3149
_journal_page_last               o3150
_journal_paper_doi               10.1107/S1600536812041256
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '3C7 H10 O6 , H2 O'
_chemical_formula_moiety         '3(C7 H10 O6) , H2 O'
_chemical_formula_sum            'C7 H10.667 O6.333'
_chemical_formula_weight         196.16
_chemical_name_systematic
;
Tris[(6<i>S</i>)-6-hydroxy-4-<i>epi</i>-shikimic acid] monohydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 91.672(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   11.2561(17)
_cell_length_b                   7.7049(11)
_cell_length_c                   13.9688(14)
_cell_measurement_reflns_used    5629
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.29
_cell_volume                     1211.0(3)
_computing_cell_refinement       'DENZO (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Hooft 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'SCHAKAL99 (Keller 1999)'
_computing_publication_material  'PLATON (Spek 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0848
_diffrn_reflns_av_sigmaI/netI    0.1926
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5629
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.272
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.881
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         2786
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.881
_refine_ls_R_factor_all          0.1503
_refine_ls_R_factor_gt           0.0535
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                1399
_reflns_number_total             2786
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg2099.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2236214
_cod_database_fobs_code          2236214