Disorder and conformational analysis of methyl β-<small>D</small>-galactopyranosyl-(1→ 4)-β-<small>D</small>-xylopyranoside
Zhang, Wenhui; Oliver, Allen G.; Serianni, Anthony S.; Acta Crystallographica Section C 68 (2012) o7–o11; doi:10.1107/S0108270111048347

data_2018358
_publ_section_title
;
 Disorder and conformational analysis of methyl
 \b-<small>D</small>-galactopyranosyl-(1\\rightarrow
 4)-\b-<small>D</small>-xylopyranoside
;
_journal_coeditor_code           TP3005
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o7
_journal_page_last               o11
_journal_paper_doi               10.1107/S0108270111048347
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C12 H22 O10'
_chemical_formula_moiety         'C12 H22 O10'
_chemical_formula_sum            'C12 H22 O10'
_chemical_formula_weight         326.30
_chemical_name_systematic
;
Methyl \b-D-galactopyranosyl-(1\\rightarrow4)-\b-D-xylopyranoside
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7878(14)
_cell_length_b                   22.892(2)
_cell_length_c                   4.6367(5)
_cell_measurement_reflns_used    3223
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      44.38
_cell_measurement_theta_min      3.01
_cell_volume                     1463.5(3)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
;
XP (Sheldrick, 2008), POV-ray (Cason, 2003) and DIAMOND
(Brandenburg, 2009)
;
_computing_publication_material
;
<i>XCIF</i> (Sheldrick, 2008) and <i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'combination of \w and \f scans'
_diffrn_radiation_monochromator  'channel-cut Si-<111> crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.23990
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            11197
_diffrn_reflns_theta_full        45.28
_diffrn_reflns_theta_max         45.28
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.7489
_exptl_absorpt_correction_T_min  0.5658
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.272
_refine_ls_abs_structure_details 'Flack (1983), 920 Friedel pairs'
_refine_ls_abs_structure_Flack   0.6(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         2300
_refine_ls_number_restraints     299
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+2.2462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                1900
_reflns_number_total             2300
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tp3005.cif
_cod_data_source_block           II
_cod_database_code               2018358
_cod_database_fobs_code          2018358