Methyl 4-<i>O</i>-β-<small>D</small>-xylopyranosyl β-<small>D</small>-mannopyranoside, a core disaccharide of an antifreeze glycolipid
Zhang, Wenhui; Oliver, Allen G.; Vu, Henry M.; Duman, John G.; Serianni, Anthony S.; Acta Crystallographica Section C 69 (2013) 1047–1050; doi:10.1107/S0108270113019021

data_2019131
_publ_section_title
;
 Methyl 4-<i>O</i>-\b-<small>D</small>-xylopyranosyl
 \b-<small>D</small>-mannopyranoside, a core disaccharide of an antifreeze
 glycolipid
;
_journal_coeditor_code           FN3140
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1047
_journal_page_last               1050
_journal_paper_doi               10.1107/S0108270113019021
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C12 H22 O10'
_chemical_formula_moiety         'C12 H22 O10'
_chemical_formula_sum            'C12 H22 O10'
_chemical_formula_weight         326.29
_chemical_name_systematic
;
Methyl 4-<i>O</i>-\b-<i>D</i>-xylopyranosyl \b-<i>D</i>-mannopyranoside
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     vecmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 97.406(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9763(9)
_cell_length_b                   7.4575(7)
_cell_length_c                   11.0026(11)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.38
_cell_measurement_theta_min      4.05
_cell_volume                     730.38(12)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics
'POV-ray (Cason, 2003) and DIAMOND (Brandenburg, 2009)'
_computing_publication_material
'enCIFer (Allen <i>et al.</i>, 2004) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2012 (Sheldrick, 2012<i>b</i>)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012<i>a</i>)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'combination of \w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10641
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.418
_diffrn_reflns_theta_min         4.052
_exptl_absorpt_coefficient_mu    1.132
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9089
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.207
_refine_ls_abs_structure_details
;
Flack x determined using 1029 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_coef       0.0085(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2571
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0431P)^2^+0.1364P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0688
_reflns_number_gt                2567
_reflns_number_total             2571
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3140.cif
_cod_data_source_block           II
_cod_database_code               2019131
_cod_database_fobs_code          2019131
_shelx_estimated_absorpt_t_min   0.716
_shelx_estimated_absorpt_t_max   0.889
_shelxl_version_number           .000002012