(<i>R</i>)-2-[1-(2,6-Dichloro-3,4,5-trimethoxybenzoyl)pyrrolidin-2-yl]-4,4,5,5-tetramethyl-4,5-dihydro-1<i>H</i>-imidazole-1-oxyl 3-oxide
Wang, Hai-Bo; Xiang, Zhuo; Jing, Lin-Lin; Tian, Min; Sun, Xiao-Li; Acta Crystallographica Section E 67 (2011) o985–o986; doi:10.1107/S1600536811010270

data_2229622
_publ_section_title
;
 (<i>R</i>)-2-[1-(2,6-Dichloro-3,4,5-trimethoxybenzoyl)pyrrolidin-2-yl]-4,4,5,5-tetramethyl-4,5-dihydro-1<i>H</i>-imidazole-1-oxyl
 3-oxide
;
_journal_coeditor_code           DN2666
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o985
_journal_page_last               o986
_journal_paper_doi               10.1107/S1600536811010270
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C21 H28 Cl2 N3 O6'
_chemical_formula_moiety         'C21 H28 Cl2 N3 O6'
_chemical_formula_sum            'C21 H28 Cl2 N3 O6'
_chemical_formula_weight         489.36
_chemical_name_systematic
;
(<i>R</i>)-2-[1-(2,6-Dichloro-3,4,5-trimethoxybenzoyl)pyrrolidin-2-yl]-\
4,4,5,5-tetramethyl-4,5-dihydro-1<i>H</i>-imidazole-1-oxyl 3-oxide
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.975(2)
_cell_length_b                   12.255(3)
_cell_length_c                   17.741(4)
_cell_measurement_reflns_used    1127
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      16.86
_cell_measurement_theta_min      2.30
_cell_volume                     2386.1(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0669
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12018
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_T_max  0.9522
_exptl_absorpt_correction_T_min  0.8916
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.162
_refine_ls_abs_structure_details 'Flack (1983), 1834 Friedel pairs'
_refine_ls_abs_structure_Flack   0.01(10)
_refine_ls_extinction_coef       0.0025(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0533
_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^)+(0.0400P)^2^+0.1713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                2217
_reflns_number_total             4252
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn2666.cif
_cod_data_source_block           I
_cod_original_cell_volume        2386.2(8)
_cod_database_code               2229622
_cod_database_fobs_code          2229622