#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2007155.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_2007155 loop_ _publ_author_name 'Palmer, M. H.' 'Parsons, S.' 'Smith, S.' 'Blake, A. J.' 'Guest, M. F.' _publ_section_title ; 3-Methylthio-1,2,4-triazine: a Comparison of Experimental and Theoretical Structures ; _journal_issue 4 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 550 _journal_page_last 553 _journal_volume 54 _journal_year 1998 _chemical_formula_moiety 'C4 H5 N3 S' _chemical_formula_sum 'C4 H5 N3 S' _chemical_formula_weight 127.17 _chemical_melting_point 304 _chemical_name_systematic ; 3-Methyl-thio-1,2,4-triazine ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 108.14(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.808(2) _cell_length_b 7.056(2) _cell_length_c 11.090(3) _cell_measurement_reflns_used 38 _cell_measurement_temperature 150.0(2) _cell_measurement_theta_max 16 _cell_measurement_theta_min 14 _cell_volume 580.6(3) _computing_cell_refinement DIF4 _computing_data_collection 'DIF4 (Stoe & Cie, 1990a)' _computing_data_reduction 'REDU4 (Stoe & Cie, 1990b)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution 'SHELXTL (Sheldrick, 1995)' _diffrn_ambient_temperature 150.0(2) _diffrn_measurement_device ; Stoe Stadi-4 four-circle diffractometer equipped with an Oxford Cryosystems low-temperature device (Cosier & Glazer, 1986) ; _diffrn_measurement_method ; \w-2\q scans ; _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 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 2493 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_min 2.82 _diffrn_standards_decay_% <3 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 0.441 _exptl_absorpt_correction_T_max 0.892 _exptl_absorpt_correction_T_min 0.831 _exptl_absorpt_correction_type ; \y scans (North, Phillips & Mathews, 1968) ; _exptl_crystal_colour 'Pale yellow' _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_meas 'Not measured' _exptl_crystal_description Tablet _exptl_crystal_F_000 264 _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.26 _refine_diff_density_max 0.318 _refine_diff_density_min -0.301 _refine_ls_extinction_coef 0.013(5) _refine_ls_extinction_method 'SHELXTL (Sheldrick, 1995)' _refine_ls_goodness_of_fit_all 1.055 _refine_ls_goodness_of_fit_obs 1.072 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 94 _refine_ls_number_reflns 1026 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_restrained_S_obs 1.072 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_obs 0.0290 _refine_ls_shift/esd_max -0.047 _refine_ls_shift/esd_mean 0.006 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w =1/[\s^2^(Fo^2^)+(0.0556P)^2^+0.1168P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_all 0.0827 _refine_ls_wR_factor_obs 0.0777 _reflns_number_observed 910 _reflns_number_total 1029 _reflns_observed_criterion >2sigma(I) _[local]_cod_data_source_file cf1207.cif _[local]_cod_data_source_block nnnsme _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2007155 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 N1 0.0272(7) 0.0284(7) 0.0206(7) -0.0002(5) 0.0007(6) 0.0045(6) N2 0.0224(6) 0.0299(7) 0.0190(6) -0.0014(5) 0.0014(5) -0.0004(5) C3 0.0215(7) 0.0223(8) 0.0201(8) 0.0004(6) 0.0075(6) -0.0028(6) N4 0.0243(7) 0.0278(7) 0.0193(7) 0.0005(5) 0.0006(5) 0.0028(5) C5 0.0237(8) 0.0300(9) 0.0199(8) -0.0027(6) -0.0014(7) 0.0007(6) C6 0.0275(8) 0.0243(8) 0.0219(8) -0.0029(7) 0.0012(6) 0.0021(7) S 0.0389(3) 0.0270(3) 0.0332(3) -0.0087(2) 0.0121(2) 0.0000(2) C1M 0.0460(12) 0.0516(12) 0.0400(11) -0.0267(11) 0.0119(9) -0.0141(10) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_occupancy _atom_site_type_symbol N1 0.1033(2) -0.2611(2) 0.96742(13) 0.0269(3) Uani d 1 N N2 0.1715(2) -0.0897(2) 0.95348(12) 0.0249(3) Uani d 1 N C3 0.0930(2) 0.0039(2) 0.84644(14) 0.0211(4) Uani d 1 C N4 -0.0524(2) -0.0519(2) 0.75059(12) 0.0252(3) Uani d 1 N C5 -0.1152(2) -0.2197(2) 0.7664(2) 0.0264(4) Uani d 1 C H5 -0.215(3) -0.267(3) 0.703(2) 0.038(5) Uiso d 1 H C6 -0.0356(2) -0.3257(2) 0.8758(2) 0.0260(4) Uani d 1 C H6 -0.076(2) -0.447(3) 0.8884(17) 0.030(5) Uiso d 1 H S 0.17669(6) 0.22431(6) 0.81889(4) 0.0328(2) Uani d 1 S C1M 0.3629(3) 0.2602(4) 0.9601(2) 0.0462(5) Uani d 1 C H1M1 0.415(4) 0.372(5) 0.950(3) 0.103(11) Uiso d 1 H H1M2 0.457(4) 0.170(4) 0.958(3) 0.071(8) Uiso d 1 H H1M3 0.327(4) 0.253(3) 1.032(3) 0.061(7) Uiso d 1 H 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' S S 0.1246 0.1234 '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 _geom_angle_publ_flag C6 N1 N2 118.79(14) n N1 N2 C3 117.30(13) n N2 C3 N4 126.79(14) n C3 N4 C5 114.53(13) n N4 C5 C6 121.03(15) n C5 C6 N1 121.51(15) n N2 C3 S 120.25(12) n N4 C3 S 112.96(11) n C3 S C1M 102.60(9) n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag N1 N2 1.350(2) n N2 C3 1.330(2) n C3 N4 1.350(2) n N4 C5 1.314(2) n C5 C6 1.395(2) n C6 N1 1.315(2) n C3 S 1.750(2) n S C1M 1.792(2) n 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_publ_flag C6 N1 N2 C3 -0.1(2) ? N1 N2 C3 N4 2.0(2) ? N1 N2 C3 S -178.29(10) ? N2 C3 N4 C5 -2.4(2) ? S C3 N4 C5 177.94(10) ? C3 N4 C5 C6 0.9(2) ? N2 N1 C6 C5 -1.2(2) ? N4 C5 C6 N1 0.8(2) ? N2 C3 S C1M -0.37(15) n N4 C3 S C1M 179.34(12) n