# CIF-file generated for

#==============================================================================
data_cyt_fcyt_I
#==============================================================================
 
 # SUBMISSION DETAILS
_publ_contact_author_name             'Doris E. Braun'
_publ_contact_author_address
;
Institute of Pharmacy
University of Innsbruck
Innrain 52c
6020 Innsbruck
Austria
;
_publ_contact_author_phone            '43 (0)512 507 58653'
_publ_contact_author_fax              '43 (0)512 507 58499'
_publ_contact_author_email            'doris.braun@uibk.ac.at'
_publ_requested_journal               'CrystEngComm'

# TITLE AND AUTHOR LIST

_publ_section_title
;
Prediction and Experimental Validation of Solid Solutions 
and Isopolymorphs of Cytosine/5-Flucytosine
;
loop_
_publ_author_name
_publ_author_address
'Doris E. Braun'
;
Institute of Pharmacy
University of Innsbruck
Innrain 52
6020 Innsbruck
Austria
;
'Ulrich J. Griesser'
;
Institute of Pharmacy
University of Innsbruck
Innrain 52
6020 Innsbruck
Austria
;
_chemical_name_systematic
;
4-aminopyrimidin-2(1H)-one/4-amino-5-fluoro-pyrimidin-2(1H)-one
;
_chemical_name_common        'cytosine/5-flucytosine solid solution I'
_chemical_formula_sum        'C4 H4.393 F0.607 N3 O1'
_chemical_formula_moiety     'C4 H4.393 F0.607 N3 O1'
_chemical_formula_weight     122.023
_exptl_crystal_colour        colourless
_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.   
;


#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting                              tetragonal
_symmetry_space_group_name_Hall                   'P 4abw 2nw'
_symmetry_space_group_name_H-M                    'P 41 21 2'
_symmetry_Int_Tables_number                              92

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
 
_cell_length_a                          6.67372(5)
_cell_length_b                          6.67372(5)
_cell_length_c                          23.6290(3)
_cell_angle_alpha                       90
_cell_angle_beta                        90
_cell_angle_gamma                       90
_cell_volume                            1052.40(2)
_cell_formula_units_Z                   8
_cell_measurement_temperature           298(2)
_cell_measurement_wavelength            1.54180

_diffrn_ambient_temperature             298(2)
_diffrn_radiation_wavelength            1.54180
_exptl_crystal_density_diffrn           1.540
_exptl_crystal_density_method       'Not Measured'  
_exptl_crystal_F_000                                    503
_exptl_absorpt_coefficient_mu                         0.130
_diffrn_measurement_device_type      'Panalytical X?Pert PRO'
_pd_meas_number_of_points         5230
_pd_meas_2theta_range_min         2.00457
_pd_meas_2theta_range_max         69.98157
_pd_meas_2theta_range_inc         0.013

_pd_spec_mount_mode               'transmission'
_pd_spec_shape                    'flat_sheet' 
_pd_char_particle_morphology      'powder'
_pd_char_colour                   'colourless'      

_pd_proc_ls_profile_function      'fundamental parameters'         
_pd_proc_ls_background_function   Chebychev 

_pd_proc_ls_prof_R_factor 0.0451
_pd_proc_ls_prof_wR_factor 0.0629
_pd_proc_ls_prof_wR_expected   0.0317
_refine_ls_R_I_factor             ?
_refine_ls_R_Fsqd_factor          ?
_refine_ls_R_factor_all           ?
_refine_ls_goodness_of_fit_all  1.9830

#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

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
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
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 . . . .


#===============================================================================
 
# 10. MOLECULAR GEOMETRY
 
_geom_special_details
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;
 
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_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_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_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_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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_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
 
 
_refine_special_details
;
A restrained Rietveld refinement was carried out using the best solution 
returned from the simulated annealing in TOPAS V5. The final refinement 
included a total of 74 parameters (20 profile, 2 cell, 1 scale, 8 preferred 
orientation, 1 occupancy factor, 42 positon), yielding a final 
Rwp= 6.18.
;

#===END
