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_2022208
_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          '4C13 H13 F N2 O3, C1 Cl4'
_chemical_formula_moiety         '4(C13 H13 F N2 O3), C1 Cl4'
_chemical_formula_sum            'C53 H52 Cl4 F4 N8 O12'
_chemical_formula_weight         1210.82
_chemical_name_systematic
;
Methyl
4-(4-fluorophenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate
carbon tetrachloride 0.25-solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 91.607(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.2070(7)
_cell_length_b                   9.1642(4)
_cell_length_c                   17.9630(7)
_cell_measurement_reflns_used    4823
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.55
_cell_measurement_theta_min      2.50
_cell_volume                     2666.89(19)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0509
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20706
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.669
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.574
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         4601
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1858P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2424
_reflns_number_gt                3571
_reflns_number_total             4601
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cu3165sup1.cif
_cod_data_source_block           S1
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               2022208
_shelx_estimated_absorpt_t_min   0.874
_shelx_estimated_absorpt_t_max   0.933
_shelx_hkl_checksum              947
_shelx_res_checksum              47940
_cod_database_fobs_code 2022208