Crystal structures of the anhydrous and two solvated forms of methyl 4-(4-fluorophenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate
Cleetus, Annie; Rani, Gulshan; Dharma Rao, G. B.; Chopra, Deepak; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620009560

data_2022209
_publ_section_title
;
 Crystal structures of the anhydrous and two solvated forms of methyl
 4-(4-fluorophenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate
;
_journal_coeditor_code           CU3165
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620009560
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'C13 H13 F N2 O3, 0.5C4 H8 O2'
_chemical_formula_moiety         'C13 H13 F N2 O3, 0.5(C4 H8 O2)'
_chemical_formula_sum            'C15 H17 F N2 O4'
_chemical_formula_weight         308.30
_chemical_name_systematic
;
Methyl
4-(4-fluorophenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate
ethyl acetate hemisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                82.389(2)
_cell_angle_beta                 79.380(2)
_cell_angle_gamma                65.898(2)
_cell_formula_units_Z            2
_cell_length_a                   7.3353(2)
_cell_length_b                   8.9091(2)
_cell_length_c                   12.5006(4)
_cell_measurement_reflns_used    3724
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.74
_cell_measurement_theta_min      2.51
_cell_volume                     731.44(4)
_computing_cell_refinement
;
SAINT (Bruker, 2012)
;
_computing_data_collection
;
APEX2 (Bruker, 2012)
;
_computing_data_reduction
;
SAINT (Bruker, 2012)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), PLATON (Spek, 2020) and PARST
(Nardelli, 1995)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015) and
WinGX (Farrugia (2012)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008) and
SIR2014 (Burla <i>et al.</i>, 2015)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14325
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.877
_diffrn_reflns_theta_min         1.661
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       rod
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.270
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.341
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3475
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0610P)^2^+0.4490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                2647
_reflns_number_total             3475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cu3165sup1.cif
_cod_data_source_block           S2
_cod_database_code               2022209
_shelx_estimated_absorpt_t_min   0.954
_shelx_estimated_absorpt_t_max   0.971
_shelx_hkl_checksum              6261
_shelx_res_checksum              95963
_cod_database_fobs_code 2022209