1-(2-Cyclohex-2-enylpropionyl)-3-methylurea, 2-ethyl-5-methylhexanamide and 2-ethylpentanamide: three products of barbiturate decomposition
Nichol, Gary S.; Clegg, William; Acta Crystallographica Section C 67 (2011) o13–o17; doi:10.1107/S0108270110049322

data_2017948
_publ_section_title
;
 1-(2-Cyclohex-2-enylpropionyl)-3-methylurea,
 2-ethyl-5-methylhexanamide and 2-ethylpentanamide: three products of
 barbiturate decomposition
;
_journal_coeditor_code           SK3397
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o13
_journal_page_last               o17
_journal_paper_doi               10.1107/S0108270110049322
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C11 H18 N2 O2'
_chemical_formula_moiety         'C11 H18 N2 O2'
_chemical_formula_sum            'C11 H18 N2 O2'
_chemical_formula_weight         210.27
_chemical_name_systematic
;
1-(2-Cyclohex-2-enylpropionyl)-3-methylurea
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.52(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.108(2)
_cell_length_b                   21.824(4)
_cell_length_c                   10.393(2)
_cell_measurement_reflns_used    28727
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2290.4(8)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999) and
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
'SHELXTL (Sheldrick, 2008), publCIF (Westrip, 2010) and local programs'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_source         'Enraf--Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            37076
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.231
_refine_ls_extinction_coef       0.0065(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4030
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0578
_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^)+(0.0417P)^2^+2.3454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1401
_reflns_number_gt                3184
_reflns_number_total             4030
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3397.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017948
_cod_database_fobs_code          2017948