#======================================================================= # AUTHOR AND JOURNAL INFORMATION _publ_contact_author_name 'Katarzyna N. Jarzembska' _publ_contact_author_address ; Department of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warszawa, Poland; ; _publ_contact_author_email 'katarzyna.jarzembska@gmail.com' loop_ _publ_author_name _publ_author_address 'Katarzyna N. Jarzembska' ; Department of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warszawa, Poland ; 'Marcin Kubsik' ; Department of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warszawa, Poland ; 'Radoslaw Kaminski' ; Department of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warszawa, Poland ; 'Krzysztof Wozniak' ; Department of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warszawa, Poland ; 'Paulina M. Dominiak' ; Department of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warszawa, Poland ; _publ_requested_journal 'Crystal Growth & Design' _publ_section_title ; From a single molecule to molecular crystal architectures - structural and energetic studies of selected uracil derivatives ; #======================================================================= data_4tU #======================================================================= # CHEMICAL DATA _chemical_formula_moiety 'C4 H4 N2 O S' _chemical_formula_sum 'C4 H4 N2 O S' _chemical_formula_weight 128.15 #======================================================================= # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 4.2588(12) _cell_length_b 12.419(4) _cell_length_c 9.844(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.289(9) _cell_angle_gamma 90.00 _cell_volume 520.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _exptl_crystal_density_diffrn 1.635 _exptl_crystal_F_000 264 _exptl_absorpt_coefficient_mu 0.501 _exptl_crystal_description unspecified _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_colour yellow _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Absorption correction done by SORTAV Blessing, R. H.: (1995) Acta Cryst. A51, 33-38 ; _exptl_absorpt_correction_T_min 0.9377 _exptl_absorpt_correction_T_max 0.9610 #======================================================================= # EXPERIMENTAL DATA _diffrn_ambient_temperature 100(1) _diffrn_radiation_type 'Mo-K\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Agilent Technologies KM4CCD \k-axis diffractometer' _diffrn_measurement_device_type 'Opal CCD detector' _diffrn_measurement_method '\w-scans' _diffrn_reflns_number 10911 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 30.02 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_av_r_equivalents 0.0629 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 #====================================================================== # REFINEMENT DATA _reflns_number_total 1479 _reflns_number_gt 1031 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqr _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_number_reflns 1479 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.0502P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_hydrogen_treatment constr _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_extinction_method none _refine_diff_density_max +0.37 _refine_diff_density_min -0.32 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #======================================================================= # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S4 S 0.00717(12) 0.42125(4) 0.15833(5) 0.02310(16) Uani 1 1 d . . . O2 O 0.7155(3) 0.39140(11) 0.55517(14) 0.0232(3) Uani 1 1 d . . . C4 C 0.2100(4) 0.34417(15) 0.26892(19) 0.0188(4) Uani 1 1 d . . . C2 C 0.5676(4) 0.34224(15) 0.46665(19) 0.0193(4) Uani 1 1 d . . . N1 N 0.5922(4) 0.23351(12) 0.45038(17) 0.0209(4) Uani 1 1 d . . . H1 H 0.7176 0.1972 0.5059 0.025 Uiso 1 1 calc R . . N3 N 0.3672(4) 0.39229(12) 0.37582(16) 0.0193(4) Uani 1 1 d . . . H3 H 0.3365 0.4618 0.3872 0.023 Uiso 1 1 calc R . . C6 C 0.4298(5) 0.17927(15) 0.35149(19) 0.0216(4) Uani 1 1 d . . . H6 H 0.4505 0.1032 0.3459 0.026 Uiso 1 1 calc R . . C5 C 0.2406(5) 0.23052(15) 0.2613(2) 0.0210(4) Uani 1 1 d . . . H5 H 0.1285 0.1910 0.1933 0.025 Uiso 1 1 calc R . . 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 S4 0.0266(3) 0.0191(2) 0.0230(3) 0.0001(2) -0.0103(2) 0.00135(19) O2 0.0277(8) 0.0189(6) 0.0226(8) 0.0006(6) -0.0103(6) -0.0016(5) C4 0.0192(9) 0.0209(9) 0.0161(9) -0.0006(7) -0.0018(8) -0.0008(7) C2 0.0198(9) 0.0201(9) 0.0179(10) 0.0033(7) -0.0011(8) -0.0005(7) N1 0.0238(8) 0.0182(7) 0.0203(8) 0.0014(6) -0.0067(7) 0.0016(6) N3 0.0221(8) 0.0166(7) 0.0191(9) 0.0000(6) -0.0051(7) 0.0001(6) C6 0.0251(10) 0.0178(9) 0.0219(11) -0.0028(8) -0.0013(8) -0.0006(7) C5 0.0230(9) 0.0202(9) 0.0197(10) -0.0029(7) -0.0035(8) -0.0004(7) #======================================================================= # MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S4 C4 1.6748(19) . ? O2 C2 1.226(2) . ? C4 N3 1.371(2) . ? C4 C5 1.420(3) . ? C2 N1 1.364(2) . ? C2 N3 1.371(2) . ? N1 C6 1.360(2) . ? C6 C5 1.345(3) . ? 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_3 _geom_angle_publ_flag N3 C4 C5 115.46(17) . . ? N3 C4 S4 119.04(14) . . ? C5 C4 S4 125.50(15) . . ? O2 C2 N1 122.46(17) . . ? O2 C2 N3 122.68(17) . . ? N1 C2 N3 114.86(16) . . ? C6 N1 C2 122.36(16) . . ? C2 N3 C4 126.07(16) . . ? C5 C6 N1 121.69(17) . . ? C6 C5 C4 119.34(17) . . ?