Crystal structure of 6-azido-6-deoxy-1,2-<i>O</i>-isopropylidene-α-<small>D</small>-glucofuranose
Wood, Adam; Bernhardt, Paul V.; van Altena, Ian; Simone, Michela I.; Acta Crystallographica Section E 76 (2020) 1653–1656; doi:10.1107/S2056989020012438

data_2243597
_publ_section_title
;
 Crystal structure of
 6-azido-6-deoxy-1,2-<i>O</i>-isopropylidene-\a-<small>D</small>-glucofuranose
;
_journal_coeditor_code           HB7940
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1653
_journal_page_last               1656
_journal_paper_doi               10.1107/S2056989020012438
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_iupac          'C9 H15 N3 O5'
_chemical_formula_moiety         'C9 H15 N3 O5'
_chemical_formula_sum            'C9 H15 N3 O5'
_chemical_formula_weight         245.24
_chemical_name_systematic
;
6-Azido-6-deoxy-1,2-<i>O</i>-isopropylidene-\a-<i>D</i>-glucofuranose
;
_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_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_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 101.255(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.7615(4)
_cell_length_b                   9.7752(8)
_cell_length_c                   10.6833(9)
_cell_measurement_reflns_used    1783
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      60.573
_cell_measurement_theta_min      6.168
_cell_volume                     590.11(8)
_computing_cell_refinement
;
CrysAlisPro (Rigaku, 2015)
;
_computing_data_collection
;
CrysAlisPro (Rigaku, 2015)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku, 2015)
;
_computing_molecular_graphics
;
Ortep-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
WinGX publication routines (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR92 (Altomare et al., 1994)
;
_diffrn_ambient_temperature      190(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0217
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Xcalibur, EosS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3705
_diffrn_reflns_theta_full        61.53
_diffrn_reflns_theta_max         61.53
_diffrn_reflns_theta_min         4.22
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.74124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku, 2015)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.38
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.134
_refine_diff_density_min         -0.145
_refine_ls_abs_structure_details
;
Flack (1983)
;
_refine_ls_abs_structure_Flack   -0.4(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         1788
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.0212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                1674
_reflns_number_total             1788
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            hb7940sup1.cif
_cod_data_source_block           I
_cod_database_code               2243597
_cod_database_fobs_code          2243597