β-<small>D</small>-Galactopyranosyl-(1→ 4)–2-amino-2-deoxy-α-<small>D</small>-glucopyranose hydrochloride monohydrate (lactosamine)
Mossine, Valeri V.; Kelley, Steven P.; Mawhinney, Thomas P.; IUCrData 7 (2022) x220061–; doi:10.1107/S241431462200061X

data_1566189
_publ_section_title
;
 \b-<small>D</small>-Galactopyranosyl-(1\\rightarrow
 4)--2-amino-2-deoxy-\a-<small>D</small>-glucopyranose hydrochloride
 monohydrate (lactosamine)
;
_journal_coeditor_code           GG4007
_journal_issue                   1
_journal_name_full               IUCrData
_journal_page_first              x220061
_journal_paper_doi               10.1107/S241431462200061X
_journal_volume                  7
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C12 H24 N O10 +, Cl- , H2 O'
_chemical_formula_moiety         'C12 H24 N O10, Cl, H2 O'
_chemical_formula_sum            'C12 H26 Cl N O11'
_chemical_formula_weight         395.79
_chemical_name_common            lactosamine
_chemical_name_systematic
'\b-<i>D</i>-Galactopyranosyl-(1\\rightarrow4)--2-amino-2-deoxy-\a-<i>D</i>-glucopyranose hydrochloride 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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 93.940(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.785(4)
_cell_length_b                   13.523(11)
_cell_length_c                   13.254(11)
_cell_measurement_reflns_used    1276
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      20.56
_cell_measurement_theta_min      3.01
_cell_volume                     855.6(12)
_computing_cell_refinement
;
APEX3 and SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
APEX3 and SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov et al., 2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
<i>SHELXL2017/1</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
ShelXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEXII area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1328
_diffrn_reflns_av_unetI/netI     0.1478
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11475
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.187
_diffrn_reflns_theta_min         1.540
_diffrn_source                   'Sealed Source Mo with TRIUMPH optics'
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>AXScale</i>; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             420
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.370
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 729 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.02(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3787
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1519
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0475P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                2216
_reflns_number_total             3787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            gg4007sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        855.5(12)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1566189
_shelx_estimated_absorpt_t_min   0.978
_shelx_estimated_absorpt_t_max   0.997
_shelx_hkl_checksum              51447
_shelx_res_checksum              49693
_cod_database_fobs_code 1566189