# CIF-file generated for

#==============================================================================
data_cyt_fcyt_II
#==============================================================================
 
 # 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 H4.359 F0.641 N3 O1'
_chemical_formula_moiety     'C4 H4.359 F0.641 N3 O1'
_chemical_formula_weight     122.635
_exptl_crystal_colour        colourless
_exptl_crystal_preparation
; 
anhydrate I crystals were obtained by dehydration the monohydrate over 
P2O5.
Powder X-ray diffraction (PXRD) patterns were obtained using an 
XPert 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                              monoclinic
_symmetry_space_group_name_Hall                   '-P 2yn'
_symmetry_space_group_name_H-M                    'P 21/n'
_symmetry_Int_Tables_number                              14

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
   1 x,y,z
   2 1/2-x,1/2+y,1/2-z
   3 -x,-y,-z
   4 1/2+x,1/2-y,1/2+z
 
_cell_length_a                                       4.00808(9)
_cell_length_b                                      9.43931(11)
_cell_length_c                                       13.0306(2)
_cell_angle_alpha                                            90
_cell_angle_beta                                      91.179(2)
_cell_angle_gamma                                            90
_cell_volume                                        492.889(15)
_cell_formula_units_Z                                 4
_cell_measurement_temperature           298(2)
_cell_measurement_wavelength            1.54180

_diffrn_ambient_temperature             298(2)
_diffrn_radiation_wavelength            1.54180
_exptl_crystal_density_diffrn           1.653
_exptl_crystal_density_method       'Not Measured'  
_exptl_crystal_F_000                                    253
_exptl_absorpt_coefficient_mu                         0.140
_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  0.0441               
_pd_proc_ls_prof_wR_factor 0.0605
_pd_proc_ls_prof_wR_expected   0.0336
_refine_ls_R_I_factor             ?
_refine_ls_R_Fsqd_factor          ?
_refine_ls_R_factor_all           ?
_refine_ls_goodness_of_fit_all  1.798

#===============================================================================
# 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 0.378(4) 0.130(2) 0.0055(8) 0.641(9) 0.0412 . . . .
O8 O Uiso -0.3389(11) 0.1448(7) 0.3498(5) 1.000 0.0412 . . . .
N1 N Uiso -0.069(2) 0.0149(11) 0.2266(10) 1.000 0.0412 . . . .
N3 N Uiso -0.097(2) 0.2670(8) 0.2172(7) 1.000 0.0412 . . . .
N7 N Uiso 0.1359(19) 0.3814(8) 0.0737(5) 1.000 0.0412 . . . .
C2 C Uiso -0.182(2) 0.1442(19) 0.2670(6) 1.000 0.0412 . . . .
C4 C Uiso 0.074(2) 0.2621(11) 0.1279(9) 1.000 0.0412 . . . .
C5 C Uiso 0.195(3) 0.130(2) 0.0909(10) 1.000 0.0412 . . . .
C6 C Uiso 0.106(3) 0.0063(14) 0.1379(11) 1.000 0.0412 . . . .
H9 H Uiso -0.118(15) -0.067(6) 0.260(5) 1.000 0.0494 . . . .
H10 H Uiso 0.252(13) 0.373(7) 0.015(4) 1.000 0.0494 . . . .
H11 H Uiso 0.107(13) 0.468(5) 0.104(5) 1.000 0.0494 . . . .
H12 H Uiso 0.175(13) -0.086(6) 0.117(4) 1.000 0.0494 . . . .
H1 H Uiso 0.32(11) 0.13(6) 0.03(2) 0.359(9) 0.0494 . . . .
 
#===============================================================================
 
# 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        1.345(18)                     .       .                   yes
 O8      C2        1.260(10)                     .       .                   yes
 N1      C2        1.408(19)                     .       .                   yes
 N1      C6        1.367(18)                     .       .                   yes
 N3      C2        1.375(18)                     .       .                   yes
 N3      C4        1.363(14)                     .       .                   yes
 N7      C4        1.355(13)                     .       .                   yes
 N1      H9          0.91(6)                     .       .                   no
 N7      H10         0.91(5)                     .       .                   no
 N7      H11         0.92(5)                     .       .                   no
 C4      C5          1.43(2)                     .       .                   no
 C5      C6          1.37(2)                     .       .                   no
 C5      H1           1.0(4)                     .       .                   no
 C6      H12         0.96(6)                     .       .                   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        122.9(11)             .       .       .           yes
 C2      N3      C4         120.5(9)             .       .       .           yes
 C2      N1      H9           119(4)             .       .       .           no
 C6      N1      H9           118(4)             .       .       .           no
 C4      N7      H10          118(4)             .       .       .           no
 H10     N7      H11          121(6)             .       .       .           no
 C4      N7      H11          119(4)             .       .       .           no
 O8      C2      N3        122.2(13)             .       .       .           yes
 N1      C2      N3         118.0(8)             .       .       .           yes
 O8      C2      N1        119.6(13)             .       .       .           yes
 N3      C4      C5        119.9(10)             .       .       .           yes
 N7      C4      C5        118.9(10)             .       .       .           yes
 N3      C4      N7         121.2(9)             .       .       .           yes
 C4      C5      C6        120.1(11)             .       .       .           no
 F14     C5      C4        118.4(15)             .       .       .           yes
 F14     C5      C6        121.4(16)             .       .       .           yes
 N1      C6      C5        118.1(12)             .       .       .           yes
 C4      C5      H1           118.00             .       .       .           no
 C6      C5      H1           122.00             .       .       .           no
 N1      C6      H12          117(3)             .       .       .           no
 C5      C6      H12          125(3)             .       .       .           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        -179.2(9)     .       .       .       .   no
 C6      N1      C2      N3         -3.3(14)     .       .       .       .   no
 C2      N1      C6      C5          4.9(17)     .       .       .       .   no
 C4      N3      C2      N1          4.0(13)     .       .       .       .   no
 C2      N3      C4      N7         174.6(8)     .       .       .       .   no
 C4      N3      C2      O8         179.8(8)     .       .       .       .   no
 C2      N3      C4      C5         -6.3(14)     .       .       .       .   no
 N3      C4      C5      C6          7.9(16)     .       .       .       .   no
 N7      C4      C5      F14         2.6(16)     .       .       .       .   no
 N3      C4      C5      F14      -176.5(11)     .       .       .       .   no
 N7      C4      C5      C6       -173.0(10)     .       .       .       .   no
 F14     C5      C6      N1        177.5(12)     .       .       .       .   no
 C4      C5      C6      N1         -7.0(18)     .       .       .       .   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 69 parameters (20 profile, 4 cell, 1 scale, 1 preferred 
orientation, 1 occupancy factor, 42 positon), yielding a final 
Rwp= 6.18.
;

#===END
 
