Structural properties of <small>D</small>-mannopyranosyl rings containing <i>O</i>-acetyl side-chains
Turney, Toby; Zhang, Wenhui; Oliver, Allen G.; Serianni, Anthony S.; Acta Crystallographica Section C 75 (2019) 1166–1174; doi:10.1107/S2053229619008817

data_2021738
_publ_section_title
;
 Structural properties of <small>D</small>-mannopyranosyl rings containing
 <i>O</i>-acetyl side-chains
;
_journal_coeditor_code           FP3073
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1166
_journal_page_last               1174
_journal_paper_doi               10.1107/S2053229619008817
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_iupac          'C40 H54 O27'
_chemical_formula_moiety         'C40 H54 O27'
_chemical_formula_sum            'C40 H54 O27'
_chemical_formula_weight         966.83
_chemical_name_systematic
;
2,3,4,6-Tetra-<i>O</i>-acetyl-\a-<i>D</i>-mannopyranosyl-(1\\rightarrow2)-\
3,4,6-tri-<i>O</i>-acetyl-\a-<i>D</i>-mannopyranosyl-(1\\rightarrow3)-\
1,2,4,6-tetra-<i>O</i>-acetyl-\a-<i>D</i>-mannopyranose
;
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 91.8362(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1043(2)
_cell_length_b                   21.4770(5)
_cell_length_c                   13.8106(3)
_cell_measurement_reflns_used    9335
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.56
_cell_measurement_theta_min      3.81
_cell_volume                     2699.04(10)
_computing_cell_refinement
;
SAINT (Bruker, 2015)
;
_computing_data_collection
;
APEX2 (Bruker, 2015)
;
_computing_data_reduction
;
SAINT (Bruker, 2015)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (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 CCD'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_monochromator  'MONTEL Multi-layer'
_diffrn_radiation_source         'Incoatec micro-focus'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0223
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            72001
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.679
_diffrn_reflns_theta_min         3.201
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.9504
_exptl_absorpt_correction_T_min  0.8636
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.122
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.202
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4517 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.069(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         9999
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+0.5800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                9956
_reflns_number_total             9999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fp3073sup1.cif
_cod_data_source_block           III
_cod_database_code               2021738
_cod_database_fobs_code          2021738
_shelx_estimated_absorpt_t_min   0.849
_shelx_estimated_absorpt_t_max   0.901
_shelx_hkl_checksum              85993
_shelx_res_checksum              29728
_shelx_fab_checksum              29027