(2<i>S</i>,4<i>S</i>)-4-Azido-1-benzyl-2-[(<i>S</i>)-2,2-dimethyl-1,3-dioxolan-4-yl]pyrrolidine
Amy K. S. Chesterton; Sarah F. Jenkinson; Nigel A. Jones; George W. J. Fleet; David J. Watkin; Acta Crystallographica Section E 62 (2006) o2983–o2985; doi:10.1107/S1600536806023105

data_2209496
_publ_section_title
(2<i>S</i>,4<i>S</i>)-4-Azido-1-benzyl-2-[(<i>S</i>)-2,2-dimethyl-1,3-dioxolan-4-yl]pyrrolidine
_journal_coeditor_code           FL2030
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2983
_journal_page_last               o2985
_journal_paper_doi               10.1107/S1600536806023105
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C16 H22 N4 O2'
_chemical_formula_moiety         'C16 H22 N4 O2'
_chemical_formula_sum            'C16 H22 N4 O2'
_chemical_formula_weight         302.38
_chemical_name_systematic
;
(2S,4S)-4-Azido-1-benzyl-2-[(S)-2,2-dimethyl-1,3-dioxolan-4-yl]pyrrolidine
;
_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                 103.577(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6539(4)
_cell_length_b                   6.3289(3)
_cell_length_c                   13.4942(7)
_cell_measurement_reflns_used    1995
_cell_measurement_temperature    150
_cell_measurement_theta_max      30
_cell_measurement_theta_min      5
_cell_volume                     801.44(7)
_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 0.990
_diffrn_measured_fraction_theta_max 0.977
_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  0.064
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7271
_diffrn_reflns_theta_full        27.946
_diffrn_reflns_theta_max         30.050
_diffrn_reflns_theta_min         5.286
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO/SCALEPACK, Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.36
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8553
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         1833
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.000154
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w = 1/[\s^2^(F^2^) + (0.05P)^2^ + 0.1P], where P=[max(Fo^2^,0) + 2Fc^2^]/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1004
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.1004
_reflns_number_gt                1254
_reflns_number_total             2489
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fl2030.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2209496
_cod_database_fobs_code          2209496