Ethyl 1-<i>O</i>-<i>tert</i>-butyldimethylsilyl-2,3-<i>O</i>-isopropylidene-5-[(2'<i>S</i>)-tetrahydropyran-2-yloxy]-<small>D</small>-<i>glycero</i>-α-<small>D</small>-<i>manno</i>-heptofuronate
Soengas, Raquel G.; Valencia, Laura; Estévez, Juan C.; Estévez, Ramón J.; Acta Crystallographica Section E 64 (2008) o1478–; doi:10.1107/S1600536808021193

data_2218932
_publ_section_title
;Ethyl
 1-<i>O</i>-<i>tert</i>-butyldimethylsilyl-2,3-<i>O</i>-isopropylidene-5-[(2'<i>S</i>)-tetrahydropyran-2-yloxy]-<small>D</small>-<i>glycero</i>-\a-<small>D</small>-<i>manno</i>-heptofuronate
;
_journal_coeditor_code           CF2203
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1478
_journal_paper_doi               10.1107/S1600536808021193
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C23 H41 N1 O10 Si'
_chemical_formula_moiety         'C23 H41 N1 O10 Si'
_chemical_formula_sum            'C23 H41 N O10 Si'
_chemical_formula_weight         519.66
_chemical_name_common
;
Ethyl
1-<i>O</i>-tert-butyldimethylsilyl-2,3-<i>O</i>-isopropylidene-
5-[(2'<i>S</i>)-tetrahydropyran-2-yloxy]-D-<i>glycero</i>-
\a-D-<i>manno</i>-heptofuronate
;
_chemical_name_systematic
;
(2<i>S</i>,3<i>R</i>)-ethyl
3-[(3a<i>S</i>,4<i>R</i>,6<i>S</i>,6a<i>S</i>)-6-<i>tert-
</i>butyldimethylsilyloxy-2,2-dimethylperhydrofuro[3,4-<i>d</i>][1,3]dioxol-
4-yl]-2-nitro-3-[(<i>S</i>)-tetrahydro-2<i>H</i>-pyran-2-yloxy]propanoate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.593(3)
_cell_length_b                   9.563(4)
_cell_length_c                   19.690(3)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.16
_cell_measurement_theta_min      17.64
_cell_volume                     2936.1(14)
_computing_cell_refinement       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD-4 EXPRESS (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius TurboCAD-4'
_diffrn_measurement_method       'Non-profiled \w/2\q'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6473
_diffrn_reflns_theta_full        73.35
_diffrn_reflns_theta_max         73.35
_diffrn_reflns_theta_min         3.62
_diffrn_standards_decay_%        4
_diffrn_standards_interval_count 167
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.128
_exptl_absorpt_correction_T_max  0.714
_exptl_absorpt_correction_T_min  0.614
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.266
_refine_ls_abs_structure_details 'Flack (1983), 2569 Friedel pairs'
_refine_ls_abs_structure_Flack   0.04(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1249P)^2^+1.1254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2083
_refine_ls_wR_factor_ref         0.2639
_reflns_number_gt                3434
_reflns_number_total             5898
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cf2203.cif
_cod_data_source_block           I
_cod_original_cell_volume        2935.9(15)
_cod_original_formula_sum        'C23 H41 N1 O10 Si'
_cod_database_code               2218932
_cod_database_fobs_code          2218932