Crystal structure of the α-racemate of methohexital
Gelbrich, Thomas; Griesser, Ulrich J.; Acta Crystallographica Section E 71 (2015) 206–209; doi:10.1107/S205698901500105X

data_2240415
_publ_section_title
;
 Crystal structure of the \a-racemate of methohexital
;
_journal_coeditor_code           WM5105
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              206
_journal_page_last               209
_journal_paper_doi               10.1107/S205698901500105X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C14 H18 N2 O3'
_chemical_formula_moiety         'C14 H18 N2 O3'
_chemical_formula_sum            'C14 H18 N2 O3'
_chemical_formula_weight         262.30
_chemical_name_common
;
 Methohexital
;
_chemical_name_systematic
5-Allyl-5-(hex-3-yn-2-yl)-1-methylpyrimidine-2,4,6(1<i>H</i>,3<i>H</i>,5<i>H</i>)-trione
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                93.713(6)
_cell_angle_beta                 96.226(6)
_cell_angle_gamma                113.314(7)
_cell_formula_units_Z            2
_cell_length_a                   7.7502(6)
_cell_length_b                   7.9792(5)
_cell_length_c                   12.6881(10)
_cell_measurement_reflns_used    1814
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8410
_cell_measurement_theta_min      4.4050
_cell_volume                     711.32(10)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014/6 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3575
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur (Ruby, Gemini ultra)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6896
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.378
_diffrn_reflns_theta_min         2.799
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis PRO</i>; Agilent, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_description       prism
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.222
_refine_diff_density_min         -0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+0.1234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1353
_reflns_number_gt                2462
_reflns_number_total             3363
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5105sup1.cif
_cod_data_source_block           I
_cod_database_code               2240415
_cod_database_fobs_code          2240415
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.983
_shelx_hkl_checksum              65313
_shelx_res_checksum              53858
_shelxl_version_number           2014/6