3-Azido-3-deoxy-2,2':5,6-di-<i>O</i>-isopropylidene-2-<i>C</i>-hydroxmethyl-<small>D</small>-gulono-1,4-lactone
Christopher C. Harding; Howard Shallard-Brown; David J. Watkin; Raquel Soengas; George W. J. Fleet; Acta Crystallographica Section E 60 (2004) o2334–o2336; doi:10.1107/S1600536804029113

data_2204739
_publ_section_title
3-Azido-3-deoxy-2,2':5,6-di-<i>O</i>-isopropylidene-2-<i>C</i>-hydroxmethyl-<small>D</small>-gulono-1,4-lactone
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2334
_journal_page_last               o2336
_journal_paper_doi               10.1107/S1600536804029113
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C13 H19 N3 O6'
_chemical_formula_moiety         'C13 H19 N3 O6'
_chemical_formula_sum            'C13 H19 N3 O6'
_chemical_formula_weight         313.31
_chemical_name_systematic
;
3-Azido-3-deoxy-2,2':5,6-di-O-isopropylidene-2-C-hydroxmethyl-D-
gulono-1,4-lactone
;
_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
_cell_angle_alpha                90
_cell_angle_beta                 106.9659(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7755(2)
_cell_length_b                   7.6452(2)
_cell_length_c                   12.2232(3)
_cell_measurement_reflns_used    1734
_cell_measurement_temperature    120
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     784.37(3)
_computing_cell_refinement       DENZO/SCALEPACK
_computing_data_collection       'COLLECT (Nonius, 1997--2001)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS '
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'User-defined structure solution (reference?)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.015
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3320
_diffrn_reflns_theta_full        25.058
_diffrn_reflns_theta_max         27.536
_diffrn_reflns_theta_min         5.232
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       plate
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.42
_refine_ls_extinction_coef       30E1(5)
_refine_ls_extinction_method     'Larson 1970 Crystallographic Computing eq 22'
_refine_ls_goodness_of_fit_ref   0.9324
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         1866
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000326
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method: SHELXL97 (Sheldrick, 1997);
w = 1/[\s^2^(f)+(0.0522p)^2^+0.571p], where p = [max(F~0~^2^,0)+2F~c~^2^]/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1085
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                1655
_reflns_number_total             1869
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh6302.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21 '
_cod_database_code               2204739
_cod_database_fobs_code          2204739