Methyl 4,6-<i>O</i>-benzylidene-2,3-dideoxy-3-hydroxyimino-α-<small>D</small>-<i>erythro</i>-pyranoside methanol solvate
Davies, Melari; Goette, Sebastian; Klüfers, Peter; Schwarz, Thomas; Acta Crystallographica Section E 63 (2007) o4765–o4765; doi:10.1107/S1600536807059521

data_2216644
_publ_section_title
;Methyl
 4,6-<i>O</i>-benzylidene-2,3-dideoxy-3-hydroxyimino-\a-<small>D</small>-<i>erythro</i>-pyranoside
 methanol solvate
;
_journal_coeditor_code           LN2001
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4765
_journal_page_last               o4765
_journal_paper_doi               10.1107/S1600536807059521
_journal_volume                  63
_journal_year                    2007
_chemical_formula_moiety         'C14 H17 N O5, C H4 O'
_chemical_formula_sum            'C15 H21 N O6'
_chemical_formula_weight         311.33
_chemical_name_systematic
;Methyl
 4,6-<i>O</i>-benzylidene-2,3-dideoxy-3-hydroxyimino-\a-D-<i>erythro</i>-\
pyranoside
 methanol solvate
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_cell_angle_alpha                90.00
_cell_angle_beta                 109.009(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8696(12)
_cell_length_b                   4.7001(2)
_cell_length_c                   16.0494(8)
_cell_measurement_reflns_used    8876
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     1559.74(14)
_computing_cell_refinement       'Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius 2004)'
_computing_data_reduction        'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD; rotation images; thick slices'
_diffrn_radiation_monochromator  'MONTEL, graded multilayered X-ray optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6634
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         3.73
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.184
_refine_diff_density_min         -0.235
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2006
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0963
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0692P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1277
_reflns_number_gt                1238
_reflns_number_total             2006
_reflns_threshold_expression     'I >2\s(I)'
_cod_data_source_file            ln2001.cif
_cod_data_source_block           I
_cod_original_cell_volume        1559.74(13)
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               2216644
_cod_database_fobs_code          2216644