#------------------------------------------------------------------------------ #$Date: 2017-06-13 05:12:32 +0300 (Tue, 13 Jun 2017) $ #$Revision: 197754 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/84/7228454.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7228454 loop_ _publ_author_name 'Braun, Doris Elfriede' 'Griesser, Ulrich J.' _publ_section_title ; Prediction and Experimental Validation of Solid Solutions and Isopolymorphs of Cytosine/5-Flucytosine ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C7CE00939A _journal_year 2017 _chemical_formula_moiety 'C4 H4.393 F0.607 N3 O1' _chemical_formula_sum 'C4 H4.393 F0.607 N3 O' _chemical_formula_weight 122.023 _chemical_name_common 'cytosine/5-flucytosine solid solution I' _chemical_name_systematic ; 4-aminopyrimidin-2(1H)-one/4-amino-5-fluoro-pyrimidin-2(1H)-one ; _space_group_IT_number 92 _symmetry_cell_setting tetragonal _symmetry_Int_Tables_number 92 _symmetry_space_group_name_Hall 'P 4abw 2nw' _symmetry_space_group_name_H-M 'P 41 21 2' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 6.67372(5) _cell_length_b 6.67372(5) _cell_length_c 23.6290(3) _cell_measurement_temperature 298(2) _cell_measurement_wavelength 1.54180 _cell_volume 1052.401(17) _diffrn_ambient_temperature 298(2) _diffrn_measurement_device_type 'Panalytical X?Pert PRO' _diffrn_radiation_wavelength 1.54180 _exptl_absorpt_coefficient_mu 0.130 _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 503 _exptl_crystal_preparation ; anhydrate I crystals were obtained by slurry experiments in nBuOH in between 283 to 313 K. Powder X-ray diffraction (PXRD) patterns were obtained using an X?Pert PRO diffractometer (PANalytical, Almelo, NL) equipped with a theta/theta coupled goniometer in transmission geometry, programmable XYZ stage with well plate holder, Cu-Ka1,2 radiation source with a focussing mirror and a solid state PIXcel detector. The patterns were recorded at a tube voltage of 40 kV and tube current of 40 mA, applying a step size of 2theta = 0.013? with 400 s per step in the 2theta range between 2? and 70? Collection was made at room temperature. ; _pd_char_colour colourless _pd_char_particle_morphology powder _pd_meas_2theta_range_inc 0.013 _pd_meas_2theta_range_max 69.98157 _pd_meas_2theta_range_min 2.00457 _pd_meas_number_of_points 5230 _pd_proc_ls_background_function Chebychev _pd_proc_ls_profile_function 'fundamental parameters' _pd_proc_ls_prof_R_factor 0.0451 _pd_proc_ls_prof_wR_expected 0.0317 _pd_proc_ls_prof_wR_factor 0.0629 _pd_spec_mount_mode transmission _pd_spec_shape flat_sheet _refine_ls_goodness_of_fit_all 1.9830 _cod_data_source_file c7ce00939a2.cif _cod_data_source_block cyt_fcyt_I _cod_original_cell_volume 1052.40(2) _cod_original_formula_sum 'C4 H4.393 F0.607 N3 O1' _cod_database_code 7228454 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-y,1/2+x,1/4+z 3 -x,-y,1/2+z 4 1/2+y,1/2-x,3/4+z 5 1/2+x,1/2-y,3/4-z 6 y,x,-z 7 1/2-x,1/2+y,1/4-z 8 -y,-x,1/2-z loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv F14 F Uiso 0.387(2) 0.536(2) 0.3805(5) 0.607(11) 0.0412 O8 O Uiso 0.7757(7) 0.8701(7) 0.2065(3) 1.000 0.0412 N1 N Uiso 0.5179(17) 0.8764(9) 0.2701(5) 1.000 0.0412 N3 N Uiso 0.7594(11) 0.6183(14) 0.2713(4) 1.000 0.0412 N7 N Uiso 0.7359(9) 0.3660(14) 0.3376(3) 1.000 0.0412 C2 C Uiso 0.6880(18) 0.7866(16) 0.2469(3) 1.000 0.0412 C4 C Uiso 0.662(2) 0.5319(13) 0.3149(4) 1.000 0.0412 C5 C Uiso 0.487(3) 0.624(3) 0.3370(5) 1.000 0.0412 C6 C Uiso 0.4165(11) 0.794(3) 0.3139(6) 1.000 0.0412 H9 H Uiso 0.467(8) 0.997(7) 0.254(3) 1.000 0.0507 H10 H Uiso 0.669(7) 0.300(8) 0.368(3) 1.000 0.0507 H11 H Uiso 0.852(9) 0.306(8) 0.3218(18) 1.000 0.0507 H12 H Uiso 0.306(6) 0.859(9) 0.326(3) 1.000 0.0507 H1 H Uiso 0.42(5) 0.57(5) 0.365(11) 0.393(11) 0.0507 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag C2 N1 C6 122.2(10) yes C2 N3 C4 120.8(9) yes C2 N1 H9 120(4) no C6 N1 H9 118(4) no C4 N7 H10 121(3) no H10 N7 H11 119(4) no C4 N7 H11 120(3) no O8 C2 N3 122.1(10) yes N1 C2 N3 118.5(8) yes O8 C2 N1 119.3(9) yes N3 C4 C5 119.5(10) yes N7 C4 C5 121.3(10) yes N3 C4 N7 119.2(10) yes C4 C5 C6 120.3(13) no F14 C5 C4 119.7(15) yes F14 C5 C6 120.0(16) yes N1 C6 C5 118.6(12) yes C4 C5 H1 121.00 no C6 C5 H1 118.00 no N1 C6 H12 117(4) no C5 C6 H12 124(4) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag F14 C5 1.36(2) yes O8 C2 1.251(11) yes N1 C2 1.396(15) yes N1 C6 1.353(18) yes N3 C2 1.349(14) yes N3 C4 1.348(14) yes N7 C4 1.325(13) yes N1 H9 0.95(5) no N7 H10 0.95(6) no N7 H11 0.95(6) no C4 C5 1.42(2) no C5 C6 1.34(3) no C5 H1 0.9(3) no C6 H12 0.90(5) no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag C6 N1 C2 O8 -179.9(11) no C6 N1 C2 N3 -3.9(16) no C2 N1 C6 C5 3(2) no C4 N3 C2 N1 4.0(15) no C2 N3 C4 N7 179.6(9) no C4 N3 C2 O8 179.8(9) no C2 N3 C4 C5 -2.8(16) no N3 C4 C5 C6 1(2) no N7 C4 C5 F14 -3(2) no N3 C4 C5 F14 179.2(12) no N7 C4 C5 C6 178.9(13) no F14 C5 C6 N1 -179.1(13) no C4 C5 C6 N1 -1(2) no