Crystal structures of three bicyclic carbohydrate derivatives
Schilde, Uwe; Kelling, Alexandra; Umbreen, Sumaira; Linker, Torsten; Acta Crystallographica Section E 72 (2016) 1839–1844; doi:10.1107/S2056989016018727

data_2241968
_publ_section_title
;
 Crystal structures of three bicyclic carbohydrate derivatives
;
_journal_coeditor_code           ZL2684
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1839
_journal_page_last               1844
_journal_paper_doi               10.1107/S2056989016018727
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C14 H19 N O8'
_chemical_formula_moiety         'C14 H19 N O8'
_chemical_formula_sum            'C14 H19 N O8'
_chemical_formula_weight         329.30
_chemical_name_systematic
'[(3a<i>R</i>,5<i>R</i>,6<i>R</i>,7<i>R</i>,7a<i>S</i>)-6,7-Bis(acetyloxy)-2-oxooctahydropyrano[3,2-<i>b</i>]pyrrol-5-yl]methyl acetate'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.476(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0784(5)
_cell_length_b                   6.1454(3)
_cell_length_c                   18.5176(12)
_cell_measurement_reflns_used    7167
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.61
_cell_measurement_theta_min      2.23
_cell_volume                     792.08(9)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2011)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2011)
;
_computing_data_reduction
;
X-RED (Stoe & Cie, 2011)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and
DIAMOND (Brandenburg, 2016)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      210(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5216
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.237
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.6071
_exptl_absorpt_correction_T_min  0.4227
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-RED; Stoe & Cie, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             348
_exptl_crystal_size_max          1.300
_exptl_crystal_size_mid          0.580
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.196
_refine_ls_extinction_coef       0.036(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         2527
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0762P)^2^+0.0852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1122
_reflns_number_gt                2394
_reflns_number_total             2527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2684sup1.cif
_cod_data_source_block           III
_cod_database_code               2241968
_cod_database_fobs_code          2241968
_shelx_estimated_absorpt_t_min   0.866
_shelx_estimated_absorpt_t_max   0.975
_shelx_hkl_checksum              8746
_shelx_res_checksum              68586