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_2021737
_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          'C16 H22 O11'
_chemical_formula_moiety         'C16 H22 O11'
_chemical_formula_sum            'C16 H22 O11'
_chemical_formula_weight         390.33
_chemical_name_systematic
;
1,2,3,4,6-Penta-<i>O</i>-acetyl-\a-<i>D</i>-mannopyranose
;
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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            12
_cell_length_a                   8.8434(4)
_cell_length_b                   15.1918(6)
_cell_length_c                   43.0639(17)
_cell_measurement_reflns_used    9740
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.675
_cell_measurement_theta_min      3.561
_cell_volume                     5785.5(4)
_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)
;
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;
SHELXS97 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      120
_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       '\f and \w scans'
_diffrn_radiation_type           CuK\a
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_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            78838
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.975
_diffrn_reflns_theta_min         2.052
_diffrn_source                   'Incoatec micro-focus'
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.9388
_exptl_absorpt_correction_T_min  0.6922
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       needle
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.165
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.022
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.252
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 4495 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.07(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         11335
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.5960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                10694
_reflns_number_total             11335
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fp3073sup1.cif
_cod_data_source_block           I
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_shelx_estimated_absorpt_t_min   0.853
_shelx_estimated_absorpt_t_max   0.978
_shelx_hkl_checksum              80439
_shelx_res_checksum              94963
_cod_database_fobs_code 2021737