3,4,6-Tri-<i>O</i>-acetyl-1,2-<i>O</i>-[1-(<i>exo</i>-ethoxy)ethylidene]-β-<small>D</small>-mannopyranose 0.11-hydrate
Liu, Ya-Ling; Zou, Pei; Wu, Hao; Xie, Min-Hao; Luo, Shi-Neng; Acta Crystallographica Section C 68 (2012) o338–o340; doi:10.1107/S0108270112032076

data_2018588
_publ_section_title
;
 3,4,6-Tri-<i>O</i>-acetyl-1,2-<i>O</i>-[1-(<i>exo</i>-ethoxy)ethylidene]-\b-<small>D</small>-mannopyranose
 0.11-hydrate
;
_journal_coeditor_code           BI3042
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o338
_journal_page_last               o340
_journal_paper_doi               10.1107/S0108270112032076
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C16 H24 O10 , 0.11H2 O'
_chemical_formula_moiety         'C16 H24 O10, 0.11(H2 O)'
_chemical_formula_sum            'C16 H24.22 O10.11'
_chemical_formula_weight         378.35
_chemical_melting_point          375.0(10)
_chemical_name_systematic
;
3,4,6-Tri-<i>O</i>-acetyl-1,2-<i>O</i>-[1-(<i>exo</i>-ethoxy)ethylidene]-
\b-D-mannopyranose 0.11-hydrate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.232(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.6353(14)
_cell_length_b                   30.987(8)
_cell_length_c                   10.817(3)
_cell_measurement_reflns_used    6897
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.127
_cell_measurement_theta_min      1.891
_cell_volume                     1881.0(9)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku AFC10/Saturn724+ CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16933
_diffrn_reflns_theta_full        29.11
_diffrn_reflns_theta_max         29.11
_diffrn_reflns_theta_min         2.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9904
_exptl_absorpt_correction_T_min  0.9484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             804.1
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9788
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.1260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                7008
_reflns_number_total             9788
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi3042.cif
_cod_data_source_block           I
_cod_original_cell_volume        1881.0(8)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2018588
_cod_database_fobs_code          2018588