2,2-Dichloro-1-(3,3,6-trimethyl-9-oxo-1,5-diazabicyclo[4.3.0]nonan-5-yl)ethanone
Fu, Ying; Ye, Fei; Acta Crystallographica Section E 67 (2011) o2020–; doi:10.1107/S1600536811027176

data_2231201
_publ_section_title
;
 2,2-Dichloro-1-(3,3,6-trimethyl-9-oxo-1,5-diazabicyclo[4.3.0]nonan-5-yl)ethanone
;
_journal_coeditor_code           LH5271
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2020
_journal_paper_doi               10.1107/S1600536811027176
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C12 H18 Cl2 N2 O2'
_chemical_formula_moiety         'C12 H18 Cl2 N2 O2'
_chemical_formula_sum            'C12 H18 Cl2 N2 O2'
_chemical_formula_weight         293.18
_chemical_name_systematic
;
2,2-Dichloro-1-(3,3,6-trimethyl-9-oxo-1,5-diazabicyclo[4.3.0]nonan-5-yl)ethanone
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 115.067(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4442(18)
_cell_length_b                   14.116(3)
_cell_length_c                   11.7555(16)
_cell_measurement_reflns_used    3515
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.38
_cell_volume                     1419.6(5)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART 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  0.0271
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10829
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.453
_exptl_absorpt_correction_T_max  0.8835
_exptl_absorpt_correction_T_min  0.8324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.478
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3492
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0683P)^2^+0.2384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                2556
_reflns_number_total             3492
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5271.cif
_cod_data_source_block           I
_cod_original_cell_volume        1419.6(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2231201
_cod_database_fobs_code          2231201