Methyl β-<small>D</small>-galactopyranosyl-(1→ 4)-β-<small>D</small>-allopyranoside tetrahydrate
Zhang, Wenhui; Oliver, Allen G.; Serianni, Anthony S.; Acta Crystallographica Section C 66 (2010) o484–o487; doi:10.1107/S0108270110029471

data_2017875
_publ_section_title
;
 Methyl \b-<small>D</small>-galactopyranosyl-(1\\rightarrow
 4)-\b-<small>D</small>-allopyranoside tetrahydrate
;
_journal_coeditor_code           UK3025
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o484
_journal_page_last               o487
_journal_paper_doi               10.1107/S0108270110029471
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C13 H24 O11 , 4H2 O'
_chemical_formula_moiety         'C13 H24 O11 , 4H2 O'
_chemical_formula_sum            'C13 H32 O15'
_chemical_formula_weight         428.39
_chemical_name_systematic
;
Methyl \b-D-galactopyranosyl-(1\\rightarrow4)-\b-D-allopyranoside tetrahydrate
;
_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                   4.7071(5)
_cell_length_b                   20.125(2)
_cell_length_c                   20.903(2)
_cell_measurement_reflns_used    8643
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.15
_cell_measurement_theta_min      2.39
_cell_volume                     1980.1(3)
_computing_cell_refinement       'SAINT (Bruker Nonius, 2009)'
_computing_data_collection       'APEX2 (Bruker Nonius, 2009)'
_computing_data_reduction        'SAINT (Bruker Nonius, 2009)'
_computing_molecular_graphics
;
XP (Sheldrick, 2008), POV-RAY (Cason, 2003) and DIAMOND
(Brandenburg, 2009)
;
_computing_publication_material
;
XCIF (Sheldrick, 2008), enCIFer (Allen <i>et al.</i>, 2004) and
publCIF
(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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.77490
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_sigmaI/netI    0.0585
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            28515
_diffrn_reflns_theta_full        33.58
_diffrn_reflns_theta_max         33.58
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.9951
_exptl_absorpt_correction_T_min  0.9878
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.201
_refine_ls_abs_structure_details 'Flack (1983), with 2548 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.1(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5985
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                5510
_reflns_number_total             5985
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            uk3025.cif
_cod_data_source_block           I
_cod_original_cell_volume        1980.1(4)
_cod_database_code               2017875
_cod_database_fobs_code          2017875