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_2241967
_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          'C11 H15 N O6'
_chemical_formula_moiety         'C11 H15 N O6'
_chemical_formula_sum            'C11 H15 N O6'
_chemical_formula_weight         257.24
_chemical_name_systematic
;
(1<i>S</i>,4<i>R</i>,5<i>S</i>,6<i>R</i>)-\
5-Acetyloxy-7-hydroxyimino-2-oxabicyclo[4.2.0]octan-4-yl 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                 101.742(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9910(3)
_cell_length_b                   9.6231(5)
_cell_length_c                   14.4915(6)
_cell_measurement_reflns_used    16172
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.11
_cell_volume                     1227.59(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 0.993
_diffrn_measured_fraction_theta_max 0.991
_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  0.0375
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8812
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.314
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9974
_exptl_absorpt_correction_T_min  0.7803
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-RED; Stoe & Cie, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.550
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         4765
_refine_ls_number_restraints     401
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0759P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                4363
_reflns_number_total             4765
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2684sup1.cif
_cod_data_source_block           II
_cod_database_code               2241967
_cod_database_fobs_code          2241967
_shelx_estimated_absorpt_t_min   0.929
_shelx_estimated_absorpt_t_max   0.956
_shelx_hkl_checksum              28303
_shelx_res_checksum              92387