#------------------------------------------------------------------------------ #$Date: 2014-07-12 05:32:21 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120110 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/50/46/4504656.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_4504656 loop_ _publ_author_name 'Hulme, Ashley T.' 'Tocher, Derek A.' _publ_section_title ; The Discovery of New Crystal Forms of 5-Fluorocytosine Consistent with the Results of Computational Crystal Structure Prediction ; _journal_issue 2 _journal_name_full 'Crystal Growth & Design' _journal_page_first 481 _journal_volume 6 _journal_year 2006 _chemical_formula_moiety 'C4 H4 F N3 O' _chemical_formula_sum 'C4 H4 F N3 O' _chemical_formula_weight 129.10 _chemical_name_systematic ; 5-fluorocytosine Form I ; _space_group_IT_number 92 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'P 4abw 2nw' _symmetry_space_group_name_H-M 'P 41 21 2' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 6.6387(4) _cell_length_b 6.6387(4) _cell_length_c 23.471(3) _cell_measurement_reflns_used 4809 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.1835 _cell_measurement_theta_min 3.192 _cell_volume 1034.42(16) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker SMART APEX diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0097 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 820 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 28.24 _diffrn_reflns_theta_min 3.19 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_T_max 0.9723 _exptl_absorpt_correction_T_min 0.9647 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _refine_diff_density_max 0.336 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.046 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 98 _refine_ls_number_reflns 820 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0334 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0479P)^2^+0.3473P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.0860 _reflns_number_gt 805 _reflns_number_total 820 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cg050398gsi20050809_092734.cif _[local]_cod_data_source_block str0336 _[local]_cod_cif_authors_sg_H-M P41212 _cod_original_cell_volume 1034.41(16) _cod_database_code 4504656 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag F5 F 1.12791(16) 0.03278(17) 0.87079(5) 0.0302(3) Uani 1 1 d O2 O 0.73437(19) 0.38141(19) 1.04285(4) 0.0244(3) Uani 1 1 d N4 N 0.7767(2) -0.1335(2) 0.91375(6) 0.0224(3) Uani 1 1 d H2 H 0.662(3) -0.178(3) 0.9292(7) 0.018(5) Uiso 1 1 d H3 H 0.825(4) -0.173(3) 0.8846(9) 0.029(5) Uiso 1 1 d N3 N 0.7523(2) 0.1248(2) 0.97874(5) 0.0185(3) Uani 1 1 d N1 N 0.9922(2) 0.3853(2) 0.97971(5) 0.0204(3) Uani 1 1 d H1 H 1.033(3) 0.503(4) 0.9953(8) 0.031(5) Uiso 1 1 d C6 C 1.0965(3) 0.2980(3) 0.93648(7) 0.0213(3) Uani 1 1 d H4 H 1.217(3) 0.360(3) 0.9255(7) 0.018(5) Uiso 1 1 d C5 C 1.0288(3) 0.1262(3) 0.91391(6) 0.0204(3) Uani 1 1 d C4 C 0.8495(2) 0.0363(2) 0.93540(6) 0.0180(3) Uani 1 1 d C2 C 0.8208(2) 0.2996(2) 1.00202(7) 0.0184(3) Uani 1 1 d loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F5 0.0313(6) 0.0272(6) 0.0321(5) -0.0113(4) 0.0151(5) -0.0046(4) O2 0.0275(6) 0.0248(6) 0.0208(5) -0.0054(5) 0.0076(5) -0.0076(5) N4 0.0250(7) 0.0207(7) 0.0216(6) -0.0050(5) 0.0044(6) -0.0058(6) N3 0.0195(6) 0.0184(7) 0.0177(5) -0.0001(5) 0.0013(5) -0.0044(5) N1 0.0230(7) 0.0183(7) 0.0199(6) -0.0028(5) 0.0048(6) -0.0072(6) C6 0.0210(8) 0.0212(8) 0.0218(7) 0.0003(6) 0.0053(6) -0.0044(7) C5 0.0217(8) 0.0206(8) 0.0189(6) -0.0008(6) 0.0045(6) 0.0000(6) C4 0.0202(8) 0.0176(7) 0.0164(6) 0.0022(6) -0.0008(6) -0.0010(6) C2 0.0203(7) 0.0191(7) 0.0159(5) 0.0011(6) 0.0008(6) -0.0035(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C4 N4 H2 115.7(13) C4 N4 H3 117.4(16) H2 N4 H3 126(2) C4 N3 C2 121.18(14) C6 N1 C2 121.98(14) C6 N1 H1 121.2(14) C2 N1 H1 116.9(14) C5 C6 N1 119.26(15) C5 C6 H4 123.8(12) N1 C6 H4 116.9(12) C6 C5 F5 121.51(15) C6 C5 C4 119.95(14) F5 C5 C4 118.54(14) N4 C4 N3 119.16(15) N4 C4 C5 121.66(14) N3 C4 C5 119.18(14) O2 C2 N3 121.92(14) O2 C2 N1 119.65(14) N3 C2 N1 118.43(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance F5 C5 1.3574(18) O2 C2 1.242(2) N4 C4 1.328(2) N4 H2 0.89(2) N4 H3 0.80(2) N3 C4 1.3401(19) N3 C2 1.361(2) N1 C6 1.358(2) N1 C2 1.3762(19) N1 H1 0.91(2) C6 C5 1.336(2) C6 H4 0.93(2) C5 C4 1.424(2) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H2 O2 0.89(2) 2.06(2) 2.9484(19) 173.7(17) 7_547 N4 H3 O2 0.80(2) 2.22(2) 2.9975(18) 163(2) 4_554 N1 H1 N3 0.91(2) 1.87(2) 2.7681(19) 175.2(18) 7_657 _journal_paper_doi 10.1021/cg050398g