A fused [3.3.0]-neoglycoside lactone derived from glucuronic acid
Schombs, Matthew W.; Davis, Ryan A.; Fettinger, James C.; Gervay-Hague, Jacquelyn; Acta Crystallographica Section C 69 (2013) 1062–1066; doi:10.1107/S0108270113013723

data_2019117
_publ_section_title
;
 A fused [3.3.0]-neoglycoside lactone derived from glucuronic acid
;
_journal_coeditor_code           EB5024
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1062
_journal_page_last               1066
_journal_paper_doi               10.1107/S0108270113013723
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C20 H41 N O6 Si2'
_chemical_formula_moiety         'C20 H41 N O6 Si2'
_chemical_formula_sum            'C20 H41 N O6 Si2'
_chemical_formula_weight         447.72
_chemical_name_systematic
(3<i>S</i>,3a<i>S</i>,5<i>R</i>,6<i>R</i>,6a<i>S</i>)-5-[methoxy(methyl)amino]-3,6-bis[(triethylsilyl)oxy]-hexahydrofuro[3,2-<i>b</i>]furan-2-one
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.022(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.0523(8)
_cell_length_b                   28.1562(19)
_cell_length_c                   14.5558(10)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      68.36
_cell_measurement_theta_min      3.14
_cell_volume                     4939.5(6)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker DUO APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27457
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  0.8528
_exptl_absorpt_correction_T_min  0.4510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.295
_refine_ls_abs_structure_details 'Flack (1983), 7580 Friedel pairs'
_refine_ls_abs_structure_Flack   0.004(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1085
_refine_ls_number_reflns         16785
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0833P)^2^+0.0985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                16549
_reflns_number_total             16785
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            eb5024.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2019117
_cod_database_fobs_code          2019117