Crystal structure and identification of a pyrimido[6,1-b][1,3]oxazin-6-one derivative from the reaction of acrolein with 5-(phenoxymethyl)-2-amino-2-oxazoline
Guillon, Jean; Rubio, Sandra; Savrimoutou, Solène; Hallé, François; Moreau, Stéphane; Sonnet, Pascal; Marchivie, Mathieu; Comptes Rendus Chimie 21 (2018) 987–992; doi:10.1016/j.crci.2018.09.013

data_1566109
_publ_section_title
;
 Crystal structure and identification of a
 pyrimido[6,1-b][1,3]oxazin-6-one derivative from the reaction of acrolein
 with 5-(phenoxymethyl)-2-amino-2-oxazoline
;
_journal_issue                   11
_journal_name_full               'Comptes Rendus Chimie'
_journal_page_first              987
_journal_page_last               992
_journal_paper_doi               10.1016/j.crci.2018.09.013
_journal_volume                  21
_journal_year                    2018
_chemical_formula_sum            'C26 H32 N4 O6'
_chemical_formula_weight         496.56
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 103.041(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.3337(10)
_cell_length_b                   11.3712(7)
_cell_length_c                   10.4936(7)
_cell_measurement_reflns_used    4497
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      72.31
_cell_measurement_theta_min      2.13
_cell_volume                     2480.0(3)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku RAXIS Rapid'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Rigaku VariMax mirror'
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0289
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32457
_diffrn_reflns_theta_full        72.31
_diffrn_reflns_theta_max         72.31
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.786
_exptl_absorpt_correction_T_max  0.8912
_exptl_absorpt_correction_T_min  0.8586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.239
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4802
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+0.6898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1584
_refine_ls_wR_factor_ref         0.1878
_reflns_number_gt                4497
_reflns_number_total             4802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            CRC-2018-21-987.CIF
_cod_data_source_block           jg504
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1566109
_symmetry_absolute_configuration ad