#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2012268.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2012268 loop_ _publ_author_name 'Lynch, Daniel E.' _publ_section_title ; 2-Amino-5-methyl-1,3,4-thiadiazole and 2-amino-5-ethyl-1,3,4-thiadiazole ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1201 _journal_page_last 1203 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety 'C4 H7 N3 S' _chemical_formula_sum 'C4 H7 N3 S' _chemical_formula_weight 129.19 _chemical_melting_point 474.5(15) _chemical_name_systematic ; 2-amino-5-ethyl-1,3,4-thiadiazole ; _space_group_IT_number 61 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 7.2752(3) _cell_length_b 10.7294(4) _cell_length_c 15.4991(7) _cell_measurement_reflns_used 6797 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 45.29 _cell_measurement_theta_min 2.91 _cell_volume 1209.84(9) _computing_cell_refinement 'DENZO and COLLECT' _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1998)' _computing_data_reduction 'DENZO and COLLECT' _computing_molecular_graphics 'PLUTON94 (Spek, 1994) and PLATON97 (Spek, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 9.091 _diffrn_measured_fraction_theta_full 1.00 _diffrn_measured_fraction_theta_max 1.00 _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enraf Nonius FR591 rotating anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .041 _diffrn_reflns_av_sigmaI/netI .036 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 7813 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 3.63 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu .424 _exptl_absorpt_correction_T_max .971 _exptl_absorpt_correction_T_min .866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SORTAV; Blessing, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 544 _exptl_crystal_size_max .35 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .07 _refine_diff_density_max .26 _refine_diff_density_min -.33 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 82 _refine_ls_number_reflns 1385 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all .048 _refine_ls_R_factor_gt .036 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0438P)^2^+0.4846P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .092 _reflns_number_gt 1125 _reflns_number_total 1385 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gg1069.cif _[local]_cod_data_source_block II _[local]_cod_cif_authors_sg_H-M Pbca _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '473-476 K' was changed to '474.5(15)' - the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2012268 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol S1 .11939(6) .16283(4) .12883(3) .02593(17) Uani d . 1 S C2 .3003(2) .09453(14) .07287(10) .0237(3) Uani d . 1 C N21 .4472(2) .16103(14) .04870(11) .0327(4) Uani d . 1 N H21 .531(3) .126(2) .0179(14) .047(6) Uiso d . 1 H H22 .448(3) .240(2) .0578(13) .041(5) Uiso d . 1 H N3 .27772(18) -.02507(12) .05862(9) .0266(3) Uani d . 1 N N4 .11361(18) -.06880(13) .09304(9) .0265(3) Uani d . 1 N C5 .0180(2) .01614(15) .13126(10) .0251(4) Uani d . 1 C C51 -.1606(3) -.00415(18) .17678(14) .0378(4) Uani d . 1 C H51 -.2535 .0529 .1520 .047 Uiso calc R 1 H H52 -.1451 .0182 .2383 .047 Uiso calc R 1 H C52 -.2327(3) -.13618(19) .17130(13) .0382(4) Uani d . 1 C H53 -.3459 -.1432 .2052 .048 Uiso calc R 1 H H54 -.1404 -.1939 .1942 .048 Uiso calc R 1 H H55 -.2584 -.1570 .1109 .048 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 .0278(2) .0184(3) .0316(3) .00372(15) .00348(15) -.00314(15) C2 .0255(8) .0198(8) .0260(8) .0035(6) -.0003(6) -.0003(6) N21 .0328(8) .0188(8) .0466(10) -.0026(6) .0123(7) -.0052(6) N3 .0258(7) .0187(7) .0354(8) -.0007(5) .0065(6) -.0030(5) N4 .0258(7) .0215(7) .0322(8) -.0009(5) .0041(6) -.0011(6) C5 .0260(8) .0208(8) .0287(9) .0014(6) -.0002(6) -.0012(6) C51 .0321(9) .0362(10) .0450(11) .0011(8) .0120(8) -.0054(8) C52 .0327(9) .0446(11) .0372(10) -.0108(8) .0074(8) -.0028(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 '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 C2 S1 C5 87.15(8) N3 C2 N21 125.01(15) N3 C2 S1 113.68(12) N21 C2 S1 121.30(12) C2 N21 H21 118.9(14) C2 N21 H22 118.9(14) H21 N21 H22 122(2) C2 N3 N4 111.90(13) C5 N4 N3 113.63(13) N4 C5 C51 125.62(15) N4 C5 S1 113.63(13) C51 C5 S1 120.73(13) C5 C51 C52 114.29(15) C5 C51 H51 108.7 C52 C51 H51 108.7 C5 C51 H52 108.7 C52 C51 H52 108.7 H51 C51 H52 107.6 C51 C52 H53 109.5 C51 C52 H54 109.5 H53 C52 H54 109.5 C51 C52 H55 109.5 H53 C52 H55 109.5 H54 C52 H55 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 C2 1.7380(16) S1 C5 1.7385(16) C2 N3 1.312(2) C2 N21 1.339(2) N21 H21 .86(2) N21 H22 .85(2) N3 N4 1.3893(18) N4 C5 1.290(2) C5 C51 1.494(2) C51 C52 1.513(3) C51 H51 .99 C51 H52 .99 C52 H53 .98 C52 H54 .98 C52 H55 .98 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N21 H21 N3 5_655 .86(2) 2.12(2) 2.983(2) 175(2) yes N21 H22 N4 8_665 .85(2) 2.17(2) 3.012(2) 167(2) yes 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 C5 S1 C2 N3 .76(13) C5 S1 C2 N21 -178.51(15) N21 C2 N3 N4 178.55(16) S1 C2 N3 N4 -.69(17) C2 N3 N4 C5 .2(2) N3 N4 C5 C51 -177.75(16) N3 N4 C5 S1 .42(18) C2 S1 C5 N4 -.66(13) C2 S1 C5 C51 177.61(15) N4 C5 C51 C52 -3.3(3) S1 C5 C51 C52 178.69(14)