Glycosidic linkage, <i>N</i>-acetyl side-chain, and other structural properties of methyl 2-acetamido-2-deoxy-β-<small>D</small>-glucopyranosyl-(1→ 4)-β-<small>D</small>-mannopyranoside monohydrate and related compounds
Zhang, Wenhui; Meredith, Reagan J.; Oliver, Allen G.; Carmichael, Ian; Serianni, Anthony S.; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620001515

data_2021989
_publ_section_title
;
 Glycosidic linkage, <i>N</i>-acetyl side-chain, and other structural
 properties of methyl
 2-acetamido-2-deoxy-\b-<small>D</small>-glucopyranosyl-(1\\rightarrow
 4)-\b-<small>D</small>-mannopyranoside monohydrate and related compounds
;
_journal_coeditor_code           OP3003
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620001515
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_iupac          'C15 H27 N O11, H2 O'
_chemical_formula_moiety         'C15 H27 N O11, H2 O'
_chemical_formula_sum            'C15 H29 N O12'
_chemical_formula_weight         415.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4170(6)
_cell_length_b                   12.6782(6)
_cell_length_c                   13.2102(7)
_cell_measurement_reflns_used    9648
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.12
_cell_measurement_theta_min      3.35
_cell_volume                     1912.14(17)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2020)
;
_computing_publication_material
;
CIFTAB (Sheldrick, 2015b),
PLATON (Spek, 2009) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker PHOTON-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            31774
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.193
_diffrn_reflns_theta_min         4.834
_diffrn_source                   'Incoatec micro-focus'
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8625
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.363
_refine_ls_abs_structure_details
;
Flack x determined using 1469 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   -0.07(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3635
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.055
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0702P)^2^+1.0254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                3510
_reflns_number_total             3635
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            op3003sup1.cif
_cod_data_source_block           I
_cod_database_code               2021989
_cod_database_fobs_code          2021989
_shelx_estimated_absorpt_t_min   0.870
_shelx_estimated_absorpt_t_max   0.900
_shelx_hkl_checksum              20130
_shelx_res_checksum              78306