2-[1-(<i>tert</i>-Butoxycarbonyl)pyrrolidin-2-yl]-4,4,5,5-tetramethyl-4,5-dihydro-1<i>H</i>-imidazole-1-oxyl 3-oxide
Jiang, Ru; Wang, Hai-Bo; Gao, Peng; Jing, Lin-Lin; Sun, Xiao-Li; Acta Crystallographica Section E 66 (2010) o1954–; doi:10.1107/S1600536810020672

data_2226838
_publ_section_title
;
 2-[1-(<i>tert</i>-Butoxycarbonyl)pyrrolidin-2-yl]-4,4,5,5-tetramethyl-4,5-dihydro-1<i>H</i>-imidazole-1-oxyl
 3-oxide
;
_journal_coeditor_code           DN2566
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1954
_journal_paper_doi               10.1107/S1600536810020672
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C16 H28 N3 O4'
_chemical_formula_moiety         'C16 H28 N3 O4'
_chemical_formula_sum            'C16 H28 N3 O4'
_chemical_formula_weight         326.41
_chemical_name_systematic
;
2-[1-(<i>tert</i>-Butoxycarbonyl)pyrrolidin-2-yl]-4,4,5,5-tetramethyl-4,5-
dihydro-1<i>H</i>-imidazole-1-oxyl 3-oxide
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.312(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.1016(12)
_cell_length_b                   10.392(2)
_cell_length_c                   14.488(3)
_cell_measurement_reflns_used    1546
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.61
_cell_measurement_theta_min      2.43
_cell_volume                     900.8(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek,2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4494
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9858
_exptl_absorpt_correction_T_min  0.9697
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             354
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.195
_refine_ls_extinction_coef       0.022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         1686
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1040
_reflns_number_gt                1347
_reflns_number_total             1686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            dn2566.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2226838
_cod_database_fobs_code          2226838