2-Azido-(<i>R</i>)-3,5-<i>O</i>-benzylidene-2-deoxy-2-<i>C</i>-methyl-D-xylono-1,4-lactone [(2<i>S</i>,4a<i>R</i>,7<i>R</i>,7a<i>R</i>)-7-azido-7-methyl-2-phenyldihydro-4<i>H</i>-furo[3,2-<i>d</i>][1,3]dioxin-6(4a<i>H</i>)-one]
Hotchkiss, David J.; Jenkinson, Sarah F.; Booth, Kathrine V.; Fleet, George J. W.; Watkin, David J.; Acta Crystallographica Section E 63 (2007) o2168–o2170; doi:10.1107/S1600536807014560

data_2213449
_publ_section_title
;2-Azido-(<i>R</i>)-3,5-<i>O</i>-benzylidene-2-deoxy-2-<i>C</i>-methyl-D-xylono-1,4-lactone
 [(2<i>S</i>,4a<i>R</i>,7<i>R</i>,7a<i>R</i>)-7-azido-7-methyl-2-phenyldihydro-4<i>H</i>-furo[3,2-<i>d</i>][1,3]dioxin-6(4a<i>H</i>)-one]
;
_journal_coeditor_code           LH2348
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2168
_journal_page_last               o2170
_journal_paper_doi               10.1107/S1600536807014560
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C13 H13 N3 O4'
_chemical_formula_moiety         'C13 H13 N3 O4'
_chemical_formula_sum            'C13 H13 N3 O4'
_chemical_formula_weight         275.26
_chemical_name_common
;
[(2<i>S</i>,4a<i>R</i>,7<i>R</i>,7a<i>R</i>)-7-azido-7-methyl-2-
phenyldihydro-4<i>H</i>-furo[3,2-<i>d</i>][1,3]dioxin-6(4a<i>H</i>)-one]
;
_chemical_name_systematic
;2-Azido-(<i>R</i>)-3,5-<i>O</i>-benzylidene-2-deoxy-2-<i>C</i>-methyl-D-xylono-
1,4-lactone
;
_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
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.7507(2)
_cell_length_b                   10.4263(2)
_cell_length_c                   26.4090(5)
_cell_measurement_reflns_used    3025
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     2684.84(9)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>,  1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.958
_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  0.055
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12730
_diffrn_reflns_theta_full        27.005
_diffrn_reflns_theta_max         27.557
_diffrn_reflns_theta_min         5.405
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       plate
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.18
_refine_ls_extinction_coef       3314.893
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.8647
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         3360
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.003611
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(F^2^) + (0.05P)^2^ + 0.85P], where P=[max(Fo^2^,0) + 2Fc^2^]/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1193
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1193
_reflns_number_gt                2414
_reflns_number_total             3360
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh2348.cif
_cod_data_source_block           5
_cod_database_code               2213449
_cod_database_fobs_code          2213449