Butallylonal 1,4-dioxane hemisolvate
Gelbrich, Thomas; Rossi, Denise; Griesser, Ulrich J.; Acta Crystallographica Section E 66 (2010) o2688–; doi:10.1107/S1600536810038651

data_2227423
_publ_section_title
;
 Butallylonal 1,4-dioxane hemisolvate
;
_journal_coeditor_code           FJ2340
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2688
_journal_paper_doi               10.1107/S1600536810038651
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C11 H15 Br N2 O3, 0.5C4 H8 O2'
_chemical_formula_moiety         'C11 H15 Br N2 O3, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C13 H19 Br N2 O4'
_chemical_formula_weight         347.21
_chemical_name_common            'butallylonal 1,4-dioxane hemisolvate'
_chemical_name_systematic
;
5-(1-bromoprop-2-en-1-yl)-5-<i>sec</i>-butylpyrimidine-2,4,6-trione
1,4-dioxane hemisolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.294(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.494(2)
_cell_length_b                   6.7679(8)
_cell_length_c                   21.864(3)
_cell_measurement_reflns_used    837
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5424
_cell_measurement_theta_min      2.5293
_cell_volume                     1540.3(4)
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis Pro (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis Pro (Oxford Diffraction, 2007)'
_computing_molecular_graphics
;XP in SHELXTL (Sheldrick, 2008) and
<i>Mercury</i> (Bruno <i>et al.</i>, 2002)
;
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3575
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Ruby Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1001
_diffrn_reflns_av_sigmaI/netI    0.1206
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            9189
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.15
_exptl_absorpt_coefficient_mu    2.683
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis Pro; Oxford Diffraction, 2007)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2714
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1756
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0409P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                1171
_reflns_number_total             2714
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fj2340.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2227423
_cod_database_fobs_code          2227423