3,5-Dibromo-4-oxo-2,2,6,6-tetramethylpiperidin-1-yl oxide
Zhu, Guang-Zhou; Xu, Suo-Ping; Li, Cui-Yun; Acta Crystallographica Section E 67 (2011) o3262–; doi:10.1107/S1600536811046812

data_2232611
_publ_section_title
;
 3,5-Dibromo-4-oxo-2,2,6,6-tetramethylpiperidin-1-yl oxide
;
_journal_coeditor_code           BX2376
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3262
_journal_paper_doi               10.1107/S1600536811046812
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C9 H14 Br2 N O2'
_chemical_formula_moiety         'C9 H14 Br2 N O2'
_chemical_formula_sum            'C9 H14 Br2 N O2'
_chemical_formula_weight         328.03
_chemical_name_systematic
;
3,5-Dibromo-4-oxo-2,2,6,6-tetramethylpiperidin-1-yl oxide
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   11.6745(9)
_cell_length_b                   16.0848(14)
_cell_length_c                   5.9301(4)
_cell_measurement_reflns_used    1704
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.615
_cell_measurement_theta_min      3.489
_cell_volume                     1113.57(15)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1175
_diffrn_reflns_av_sigmaI/netI    0.0682
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            5193
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    7.255
_exptl_absorpt_correction_T_max  0.3551
_exptl_absorpt_correction_T_min  0.1388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.635
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0335
_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^)+(0.0364P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0886
_reflns_number_gt                774
_reflns_number_total             1018
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bx2376.cif
_cod_data_source_block           I
_cod_database_code               2232611
_cod_database_fobs_code          2232611