Conformational analysis of the disaccharide methyl α-D-mannopyranosyl-(1→ 3)-2-O-acetyl-β-D-mannopyranoside monohydrate
Zhang, Wenhui; Wu, Qingquan; Oliver, Allen G.; Serianni, Anthony S.; Acta Crystallographica Section C Structural Chemistry 75 (2019) –; doi:10.1107/S2053229619004728

data_2021618
_publ_section_title
;
 Conformational analysis of the disaccharide methyl
 \a-D-mannopyranosyl-(1\\rightarrow 3)-2-O-acetyl-\b-D-mannopyranoside
 monohydrate
;
_journal_coeditor_code           QS3082
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section C Structural Chemistry'
_journal_paper_doi               10.1107/S2053229619004728
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_iupac          'C15 H26 O12, H2 O'
_chemical_formula_moiety         'C15 H26 O12, H2 O'
_chemical_formula_sum            'C15 H28 O13'
_chemical_formula_weight         416.37
_chemical_name_systematic
;
Methyl
\a-<i>D</i>-mannopyranosyl-(1-3)-2-<i>O</i>-Acetyl-\b-<i>D</i>-mannopyranoside
monohydrate
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           170
_space_group_name_Hall           'P 65'
_space_group_name_H-M_alt        'P 65'
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_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                120
_cell_formula_units_Z            6
_cell_length_a                   7.8682(3)
_cell_length_b                   7.8682(3)
_cell_length_c                   52.555(3)
_cell_measurement_reflns_used    9714
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.23
_cell_measurement_theta_min      6.50
_cell_volume                     2817.7(2)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX-3 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0106
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            37134
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.591
_diffrn_reflns_theta_min         5.049
_diffrn_source                   'Incoatec micro-focus'
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.9074
_exptl_absorpt_correction_T_min  0.8158
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.136
_refine_diff_density_max         0.204
_refine_diff_density_min         -0.160
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1835 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.028(14)
_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     287
_refine_ls_number_reflns         3719
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+0.5721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                3719
_reflns_number_total             3719
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            qs3082sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2817.7(3)
_cod_database_code               2021618
_cod_database_fobs_code          2021618
_shelx_estimated_absorpt_t_min   0.727
_shelx_estimated_absorpt_t_max   0.861
_shelx_hkl_checksum              34009
_shelx_res_checksum              99801