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_2241966
_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 H18 O8'
_chemical_formula_moiety         'C14 H18 O8'
_chemical_formula_sum            'C14 H18 O8'
_chemical_formula_weight         314.28
_chemical_name_systematic
'[(1<i>R</i>,3<i>R</i>,4<i>R</i>,5<i>R</i>,6<i>S</i>)-4,5-Bis(acetyloxy)-7-oxo-2-oxabicyclo[4.2.0]octan-3-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                 96.837(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5538(6)
_cell_length_b                   8.3655(3)
_cell_length_c                   19.1395(10)
_cell_measurement_reflns_used    15828
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.14
_cell_volume                     1518.80(14)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0255
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10373
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         2.143
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.8896
_exptl_absorpt_correction_T_min  0.8001
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(X-RED; Stoe & Cie, 2011)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.780
_exptl_crystal_size_mid          0.370
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.164
_refine_diff_density_min         -0.175
_refine_ls_extinction_coef       0.0067(15)
_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   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         5034
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.0259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0816
_reflns_number_gt                4398
_reflns_number_total             5034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2684sup1.cif
_cod_data_source_block           I
_cod_database_code               2241966
_cod_database_fobs_code          2241966
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.984
_shelx_hkl_checksum              22896
_shelx_res_checksum              97940