Methyl β-lactoside [methyl β-<small>D</small>-galactopyranosyl-(1\ρightarrow 4)-β-<small>D</small>-glucopyranoside] monohydrate: a solvomorphism study
Lin, Jieye; Oliver, Allen G.; Serianni, Anthony S.; Acta Crystallographica Section C 77 (2021) 668–674; doi:10.1107/S2053229621009499

data_2022467
_publ_section_title
;
 Methyl \b-lactoside [methyl
 \b-<small>D</small>-galactopyranosyl-(1\\rightarrow
 4)-\b-<small>D</small>-glucopyranoside] monohydrate: a solvomorphism
 study
;
_journal_coeditor_code           EQ3002
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              668
_journal_page_last               674
_journal_paper_doi               10.1107/S2053229621009499
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_iupac          'C13 H24 O11, H2 O'
_chemical_formula_moiety         'C13 H24 O11, H2 O'
_chemical_formula_sum            'C13 H26 O12'
_chemical_formula_weight         374.34
_chemical_name_common
;
Methyl
\b-<i>D</i>-galactopyranosyl-(1\\rightarrow4)-\b-<i>D</i>-glucopyranoside
monohydrate
;
_chemical_name_systematic
;
Methyl \b-lactoside monohydrate
;
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 105.5950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.62500(10)
_cell_length_b                   24.0147(7)
_cell_length_c                   7.6617(2)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      70.60
_cell_measurement_theta_min      3.68
_cell_volume                     819.64(4)
_computing_cell_refinement
;
SAINT (Bruker, 2018)
;
_computing_data_collection
;
APEX3 (Bruker, 2018)
;
_computing_data_reduction
;
SAINT (Bruker, 2018)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14059
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.590
_diffrn_reflns_theta_min         3.681
_diffrn_source                   'Ius micro-focus'
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.7376
_exptl_absorpt_correction_T_min  0.5810
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       tablet
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.163
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1459 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3056
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0263
_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^)+(0.0450P)^2^+0.1553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0706
_reflns_number_gt                3031
_reflns_number_total             3056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            eq3002sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2022467
_shelx_estimated_absorpt_t_min   0.816
_shelx_estimated_absorpt_t_max   0.940
_shelx_hkl_checksum              25623
_shelx_res_checksum              19511
_cod_database_fobs_code 2022467