Methyl 4-<i>O</i>-β-<small>D</small>-galactopyranosyl α-<small>D</small>-mannopyranoside methanol 0.375-solvate
Hu, Xiaosong; Pan, Qingfeng; Noll, Bruce C.; Oliver, Allen G.; Serianni, Anthony S.; Acta Crystallographica Section C 66 (2010) o67–o70; doi:10.1107/S0108270109055012

data_2017518
_publ_section_title
;
 Methyl 4-<i>O</i>-\b-<small>D</small>-galactopyranosyl
 \a-<small>D</small>-mannopyranoside methanol 0.375-solvate
;
_journal_coeditor_code           GZ3172
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o67
_journal_page_last               o70
_journal_paper_doi               10.1107/S0108270109055012
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C13 H24 O11 , 0.375C H4 O'
_chemical_formula_moiety         'C13 H24 O11 , 0.375C H4 O'
_chemical_formula_sum            'C13.375 H25.5 O11.375'
_chemical_formula_weight         368.34
_chemical_name_systematic
;
Methyl \b-D-galactopyranosyl-(1\\rightarrow 4)-\a-D-mannopyranoside
methanol 0.375-solvate
;
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.1789(4)
_cell_length_b                   20.1789(4)
_cell_length_c                   8.4712(2)
_cell_measurement_reflns_used    6886
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.00
_cell_measurement_theta_min      4.38
_cell_volume                     3449.37(13)
_computing_cell_refinement
;
APEX2 (Bruker Nonius, 2008) and SAINT (Bruker Nonius, 2008)
;
_computing_data_collection       'APEX2 (Bruker Nonius, 2008)'
_computing_data_reduction
;
SAINT (Bruker Nonius, 2008) and XPREP (Sheldrick, 2008)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008), POV-RAY (Version 3.6.2; Cason,
2003) and
DIAMOND (Version 3.2c; Brandenburg, 2009)
;
_computing_publication_material
;
XCIF (Sheldrick, 2008), enCIFer (Allen <i>et al.</i>, 2004) and
publCIF
(Westrip, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12483
_diffrn_reflns_theta_full        69.36
_diffrn_reflns_theta_max         69.36
_diffrn_reflns_theta_min         4.38
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.9489
_exptl_absorpt_correction_T_min  0.7761
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1574
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.261
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs?'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2783
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0467P)^2^+5.8376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1037
_reflns_number_gt                2650
_reflns_number_total             2783
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gz3172.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C13.375 H25.50 O11.375'
_cod_database_code               2017518
_cod_database_fobs_code          2017518