data_190k_smz-f1_a _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ' 4-amino-N-(4-methylpyrimidin-2-yl) ' _chemical_name_common ' Sulfamerazine ' _chemical_melting_point ? _chemical_formula_moiety 'C11 H12 N4 O2 S' _chemical_formula_sum 'C11 H12 N4 O2 S' _chemical_formula_weight 264.31 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' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 14.47010(10) _cell_length_b 8.18890(10) _cell_length_c 21.8216(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2585.73(6) _cell_formula_units_Z 8 _cell_measurement_temperature 190 _cell_measurement_reflns_used 5936 _cell_measurement_theta_min 2.5650 _cell_measurement_theta_max 29.5000 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.358 _exptl_crystal_F_000 1104 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_absorpt_coefficient_mu 0.250 _shelx_estimated_absorpt_T_min 0.885 _shelx_estimated_absorpt_T_max 0.952 _exptl_absorpt_correction_T_min 0.95124 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 190 _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type 'Synchrotron' _diffrn_radiation_source 'Diamond Light Source Beamline I19' _diffrn_radiation_monochromator 'double crystal Silicon 111' _diffrn_measurement_specimen_support 'MiTeGen loop' _diffrn_measurement_device 'CrystalLogic Kappa (3 circle)' _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method ; omega rotation with 1 degree frames ; _diffrn_reflns_number 11775 _diffrn_reflns_av_unetI/netI 0.0559 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.575 _diffrn_reflns_theta_max 29.475 _diffrn_reflns_theta_full 24.415 _diffrn_measured_fraction_theta_max 0.942 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_Laue_measured_fraction_max 0.942 _diffrn_reflns_Laue_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.811 _diffrn_reflns_point_group_measured_fraction_full 0.878 _reflns_number_total 6404 _reflns_number_gt 5154 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.682 _reflns_Friedel_fraction_max 0.673 _reflns_Friedel_fraction_full 0.774 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_structure_solution 'SHELXT' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'OSCAIL' _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.3587P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1654 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.01(6) _chemical_absolute_configuration ad _refine_ls_number_reflns 6404 _refine_ls_number_parameters 344 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1319 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.35543(6) 0.50522(10) 0.65615(6) 0.0251(2) Uani 1 1 d . . . . . S2 S 0.42208(6) 0.50253(11) 0.34699(6) 0.0247(2) Uani 1 1 d . . . . . O1 O 0.3122(2) 0.6298(3) 0.69208(16) 0.0341(7) Uani 1 1 d . . . . . O2 O 0.45302(19) 0.4778(3) 0.66281(16) 0.0326(7) Uani 1 1 d . . . . . O3 O 0.32427(18) 0.5295(3) 0.34015(15) 0.0306(6) Uani 1 1 d . . . . . O4 O 0.4644(2) 0.3751(3) 0.31181(15) 0.0319(7) Uani 1 1 d . . . . . N1 N 0.1584(3) -0.1169(4) 0.6876(2) 0.0382(9) Uani 1 1 d . . . . . N2 N 0.3462(2) 0.5533(4) 0.58292(19) 0.0297(8) Uani 1 1 d . . . . . N3 N 0.1866(2) 0.5917(4) 0.58292(18) 0.0287(7) Uani 1 1 d . . . . . N4 N 0.2723(3) 0.5695(5) 0.48985(18) 0.0405(10) Uani 1 1 d . . . . . N5 N 0.6199(3) 1.1202(4) 0.3052(2) 0.0463(11) Uani 1 1 d . . . . . H5A H 0.6765 1.1190 0.2931 0.060 Uiso 1 1 calc R U . . . H5B H 0.5925 1.2118 0.3117 0.060 Uiso 1 1 calc R U . . . N6 N 0.4315(2) 0.4602(4) 0.42035(18) 0.0286(8) Uani 1 1 d . . . . . N7 N 0.5905(2) 0.4128(4) 0.41926(18) 0.0319(8) Uani 1 1 d . . . . . N8 N 0.5048(3) 0.4340(6) 0.5124(2) 0.0423(10) Uani 1 1 d . . . . . C1 C 0.2962(3) 0.3225(4) 0.6668(2) 0.0244(8) Uani 1 1 d . . . . . C2 C 0.2063(2) 0.3209(4) 0.6902(2) 0.0268(8) Uani 1 1 d . . . . . H2 H 0.1774 0.4182 0.7010 0.035 Uiso 1 1 calc R U . . . C3 C 0.1609(3) 0.1752(5) 0.6971(2) 0.0270(9) Uani 1 1 d . . . . . H3 H 0.1010 0.1740 0.7126 0.035 Uiso 1 1 calc R U . . . C4 C 0.2040(3) 0.0273(4) 0.68109(19) 0.0264(8) Uani 1 1 d . . . . . C5 C 0.2949(3) 0.0303(4) 0.6576(2) 0.0279(8) Uani 1 1 d . . . . . H5 H 0.3243 -0.0667 0.6472 0.036 Uiso 1 1 calc R U . . . C6 C 0.3398(3) 0.1769(4) 0.6504(2) 0.0290(9) Uani 1 1 d . . . . . H6 H 0.3994 0.1791 0.6344 0.038 Uiso 1 1 calc R U . . . C7 C 0.2643(3) 0.5722(5) 0.5507(2) 0.0292(9) Uani 1 1 d . . . . . C8 C 0.1938(4) 0.5938(9) 0.4589(3) 0.0589(16) Uani 1 1 d . . . . . H8 H 0.1957 0.5954 0.4163 0.077 Uiso 1 1 calc R U . . . C9 C 0.1100(3) 0.6165(8) 0.4877(3) 0.0527(14) Uani 1 1 d . . . . . H9 H 0.0563 0.6341 0.4653 0.069 Uiso 1 1 calc R U . . . C10 C 0.1083(3) 0.6122(5) 0.5505(2) 0.0370(11) Uani 1 1 d . . . . . C11 C 0.0218(3) 0.6317(7) 0.5865(3) 0.0505(13) Uani 1 1 d . . . . . H11A H 0.0172 0.7420 0.6011 0.066 Uiso 1 1 calc R U . . . H11B H 0.0226 0.5582 0.6208 0.066 Uiso 1 1 calc R U . . . H11C H -0.0304 0.6074 0.5609 0.066 Uiso 1 1 calc R U . . . C12 C 0.4807(3) 0.6832(4) 0.33448(19) 0.0246(8) Uani 1 1 d . . . . . C13 C 0.4362(3) 0.8312(4) 0.3449(2) 0.0289(9) Uani 1 1 d . . . . . H13 H 0.3752 0.8322 0.3584 0.038 Uiso 1 1 calc R U . . . C14 C 0.4822(3) 0.9765(4) 0.3353(2) 0.0365(11) Uani 1 1 d . . . . . H14 H 0.4523 1.0750 0.3430 0.047 Uiso 1 1 calc R U . . . C15 C 0.5738(3) 0.9772(4) 0.3140(2) 0.0288(9) Uani 1 1 d . . . . . C16 C 0.6178(3) 0.8275(4) 0.3036(2) 0.0272(9) Uani 1 1 d . . . . . H16 H 0.6788 0.8260 0.2902 0.035 Uiso 1 1 calc R U . . . C17 C 0.5717(3) 0.6822(5) 0.3130(2) 0.0240(8) Uani 1 1 d . . . . . H17 H 0.6012 0.5835 0.3050 0.031 Uiso 1 1 calc R U . . . C18 C 0.5140(3) 0.4336(5) 0.4514(2) 0.0298(9) Uani 1 1 d . . . . . C19 C 0.5829(4) 0.4046(8) 0.5433(3) 0.0560(16) Uani 1 1 d . . . . . H19 H 0.5807 0.4030 0.5859 0.073 Uiso 1 1 calc R U . . . C20 C 0.6662(3) 0.3766(8) 0.5149(3) 0.0571(16) Uani 1 1 d . . . . . H20 H 0.7192 0.3534 0.5374 0.074 Uiso 1 1 calc R U . . . C21 C 0.6680(3) 0.3842(6) 0.4515(2) 0.0371(10) Uani 1 1 d . . . . . C22 C 0.7547(3) 0.3639(7) 0.4149(3) 0.0511(13) Uani 1 1 d . . . . . H22A H 0.7517 0.2637 0.3922 0.066 Uiso 1 1 calc R U . . . H22B H 0.8069 0.3610 0.4420 0.066 Uiso 1 1 calc R U . . . H22C H 0.7610 0.4539 0.3870 0.066 Uiso 1 1 calc R U . . . H1N1 H 0.108(3) -0.125(6) 0.707(2) 0.038(13) Uiso 1 1 d . . . . . H2N1 H 0.190(3) -0.206(6) 0.687(2) 0.042(13) Uiso 1 1 d . . . . . H1N2 H 0.388(3) 0.513(5) 0.564(3) 0.031(13) Uiso 1 1 d . . . . . H1N6 H 0.378(5) 0.501(8) 0.443(4) 0.09(2) Uiso 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 S1 0.0236(4) 0.0261(4) 0.0255(6) 0.0026(4) -0.0013(4) -0.0014(3) S2 0.0224(4) 0.0263(4) 0.0253(6) 0.0030(4) -0.0005(4) -0.0014(3) O1 0.0366(16) 0.0271(13) 0.039(2) -0.0045(12) -0.0022(14) -0.0005(11) O2 0.0253(13) 0.0395(14) 0.0330(19) 0.0046(14) -0.0072(14) -0.0029(11) O3 0.0237(13) 0.0391(14) 0.0290(18) 0.0057(13) -0.0032(13) -0.0032(11) O4 0.0364(16) 0.0255(12) 0.0338(18) -0.0029(12) -0.0029(13) -0.0010(11) N1 0.0348(19) 0.0277(16) 0.052(3) -0.0048(17) 0.0137(19) -0.0043(14) N2 0.0207(15) 0.0363(17) 0.032(2) 0.0055(16) -0.0027(15) 0.0018(13) N3 0.0233(15) 0.0314(16) 0.032(2) 0.0012(14) 0.0008(14) 0.0032(12) N4 0.0319(19) 0.066(3) 0.024(2) 0.0035(19) -0.0038(16) 0.0107(18) N5 0.041(2) 0.0283(16) 0.070(3) -0.0044(18) 0.020(2) -0.0074(15) N6 0.0216(15) 0.0396(18) 0.025(2) 0.0076(15) 0.0026(14) 0.0015(13) N7 0.0248(16) 0.0361(17) 0.035(2) 0.0029(16) 0.0031(15) 0.0036(13) N8 0.0288(18) 0.066(3) 0.032(3) 0.0033(19) 0.0001(17) 0.0107(18) C1 0.0225(17) 0.0265(16) 0.024(2) 0.0025(15) 0.0019(16) 0.0009(13) C2 0.0233(17) 0.0268(16) 0.030(2) 0.0006(15) -0.0011(16) 0.0027(13) C3 0.0244(18) 0.0303(19) 0.026(3) -0.0018(17) 0.0027(17) 0.0031(14) C4 0.0299(19) 0.0273(16) 0.022(2) -0.0013(14) -0.0001(16) -0.0007(13) C5 0.0253(18) 0.0288(16) 0.030(2) -0.0041(17) 0.0029(19) 0.0029(13) C6 0.0219(16) 0.0303(17) 0.035(3) -0.0010(18) 0.0060(17) 0.0028(13) C7 0.0264(19) 0.0293(18) 0.032(3) 0.0059(16) -0.0033(17) 0.0023(14) C8 0.039(3) 0.103(5) 0.035(3) 0.001(3) -0.011(2) 0.022(3) C9 0.028(2) 0.089(4) 0.041(4) -0.004(3) -0.015(2) 0.011(2) C10 0.024(2) 0.041(2) 0.046(3) -0.002(2) -0.0042(19) 0.0056(16) C11 0.028(2) 0.061(3) 0.062(4) -0.006(3) -0.001(2) 0.008(2) C12 0.0262(17) 0.0246(15) 0.023(2) 0.0012(14) 0.0015(16) 0.0002(13) C13 0.0236(18) 0.0284(17) 0.035(3) -0.0009(18) 0.0050(19) 0.0032(13) C14 0.033(2) 0.0232(16) 0.053(3) -0.0008(18) 0.005(2) 0.0047(14) C15 0.030(2) 0.0271(16) 0.029(3) 0.0006(15) 0.0045(17) -0.0011(14) C16 0.0245(18) 0.0284(17) 0.029(3) -0.0035(16) 0.0062(16) -0.0018(13) C17 0.0260(19) 0.0273(17) 0.019(2) -0.0006(15) 0.0062(16) 0.0008(13) C18 0.0247(18) 0.0313(18) 0.033(3) -0.0012(17) 0.0010(17) 0.0021(14) C19 0.039(3) 0.095(4) 0.034(3) 0.005(3) -0.004(2) 0.020(3) C20 0.032(2) 0.091(4) 0.048(4) -0.009(3) -0.007(2) 0.025(3) C21 0.026(2) 0.045(2) 0.040(3) -0.004(2) 0.0007(18) 0.0056(17) C22 0.028(2) 0.070(3) 0.054(4) -0.006(3) 0.007(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 S1 O1 1.431(3) . ? S1 O2 1.437(3) . ? S1 N2 1.651(4) . ? S1 C1 1.740(4) . ? S2 O4 1.433(3) . ? S2 O3 1.440(3) . ? S2 N6 1.644(4) . ? S2 C12 1.727(4) . ? N1 C4 1.360(5) . ? N1 H1N1 0.85(5) . ? N1 H2N1 0.86(5) . ? N2 C7 1.387(5) . ? N2 H1N2 0.80(5) . ? N3 C7 1.336(5) . ? N3 C10 1.345(5) . ? N4 C7 1.333(6) . ? N4 C8 1.337(6) . ? N5 C15 1.362(5) . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? N6 C18 1.390(5) . ? N6 H1N6 0.97(7) . ? N7 C18 1.321(5) . ? N7 C21 1.345(6) . ? N8 C19 1.337(6) . ? N8 C18 1.337(6) . ? C1 C6 1.396(5) . ? C1 C2 1.398(5) . ? C2 C3 1.370(5) . ? C2 H2 0.9300 . ? C3 C4 1.406(5) . ? C3 H3 0.9300 . ? C4 C5 1.412(5) . ? C5 C6 1.374(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.378(7) . ? C8 H8 0.9300 . ? C9 C10 1.370(8) . ? C9 H9 0.9300 . ? C10 C11 1.487(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.391(5) . ? C12 C17 1.399(5) . ? C13 C14 1.380(5) . ? C13 H13 0.9300 . ? C14 C15 1.403(6) . ? C14 H14 0.9300 . ? C15 C16 1.400(5) . ? C16 C17 1.379(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C19 C20 1.375(7) . ? C19 H19 0.9300 . ? C20 C21 1.386(8) . ? C20 H20 0.9300 . ? C21 C22 1.496(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 O1 S1 O2 119.04(19) . . ? O1 S1 N2 109.0(2) . . ? O2 S1 N2 102.41(19) . . ? O1 S1 C1 109.0(2) . . ? O2 S1 C1 109.64(17) . . ? N2 S1 C1 107.1(2) . . ? O4 S2 O3 118.43(19) . . ? O4 S2 N6 109.43(19) . . ? O3 S2 N6 102.41(18) . . ? O4 S2 C12 109.27(19) . . ? O3 S2 C12 109.53(17) . . ? N6 S2 C12 107.1(2) . . ? C4 N1 H1N1 123(3) . . ? C4 N1 H2N1 119(3) . . ? H1N1 N1 H2N1 114(4) . . ? C7 N2 S1 125.9(3) . . ? C7 N2 H1N2 115(4) . . ? S1 N2 H1N2 110(4) . . ? C7 N3 C10 116.5(4) . . ? C7 N4 C8 115.2(4) . . ? C15 N5 H5A 120.0 . . ? C15 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C18 N6 S2 125.4(3) . . ? C18 N6 H1N6 119(4) . . ? S2 N6 H1N6 111(4) . . ? C18 N7 C21 116.3(4) . . ? C19 N8 C18 114.7(4) . . ? C6 C1 C2 120.4(3) . . ? C6 C1 S1 118.6(3) . . ? C2 C1 S1 121.0(3) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? N1 C4 C3 120.4(4) . . ? N1 C4 C5 120.3(3) . . ? C3 C4 C5 119.2(3) . . ? C6 C5 C4 119.8(3) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 120.2(3) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? N4 C7 N3 126.9(4) . . ? N4 C7 N2 115.4(4) . . ? N3 C7 N2 117.8(4) . . ? N4 C8 C9 122.4(5) . . ? N4 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? C10 C9 C8 118.0(4) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? N3 C10 C9 120.9(4) . . ? N3 C10 C11 116.4(5) . . ? C9 C10 C11 122.7(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 119.8(3) . . ? C13 C12 S2 119.6(3) . . ? C17 C12 S2 120.7(3) . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.6(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? N5 C15 C16 120.4(4) . . ? N5 C15 C14 120.9(3) . . ? C16 C15 C14 118.7(3) . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C12 120.0(3) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? N7 C18 N8 127.8(4) . . ? N7 C18 N6 118.7(4) . . ? N8 C18 N6 113.5(4) . . ? N8 C19 C20 122.9(5) . . ? N8 C19 H19 118.5 . . ? C20 C19 H19 118.5 . . ? C19 C20 C21 117.3(5) . . ? C19 C20 H20 121.3 . . ? C21 C20 H20 121.3 . . ? N7 C21 C20 121.0(4) . . ? N7 C21 C22 116.1(5) . . ? C20 C21 C22 123.0(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? 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 O1 S1 N2 C7 -61.5(4) . . . . ? O2 S1 N2 C7 171.6(3) . . . . ? C1 S1 N2 C7 56.2(4) . . . . ? O4 S2 N6 C18 57.6(4) . . . . ? O3 S2 N6 C18 -176.0(3) . . . . ? C12 S2 N6 C18 -60.8(4) . . . . ? O1 S1 C1 C6 -162.5(4) . . . . ? O2 S1 C1 C6 -30.6(4) . . . . ? N2 S1 C1 C6 79.8(4) . . . . ? O1 S1 C1 C2 18.7(4) . . . . ? O2 S1 C1 C2 150.5(4) . . . . ? N2 S1 C1 C2 -99.1(4) . . . . ? C6 C1 C2 C3 0.1(6) . . . . ? S1 C1 C2 C3 179.0(3) . . . . ? C1 C2 C3 C4 0.2(7) . . . . ? C2 C3 C4 N1 -179.5(4) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? N1 C4 C5 C6 179.0(4) . . . . ? C3 C4 C5 C6 -0.5(7) . . . . ? C4 C5 C6 C1 0.8(7) . . . . ? C2 C1 C6 C5 -0.6(7) . . . . ? S1 C1 C6 C5 -179.5(4) . . . . ? C8 N4 C7 N3 2.0(7) . . . . ? C8 N4 C7 N2 -177.6(5) . . . . ? C10 N3 C7 N4 -0.6(6) . . . . ? C10 N3 C7 N2 179.0(4) . . . . ? S1 N2 C7 N4 -163.5(3) . . . . ? S1 N2 C7 N3 16.8(5) . . . . ? C7 N4 C8 C9 -1.3(9) . . . . ? N4 C8 C9 C10 -0.6(10) . . . . ? C7 N3 C10 C9 -1.6(6) . . . . ? C7 N3 C10 C11 179.2(4) . . . . ? C8 C9 C10 N3 2.1(8) . . . . ? C8 C9 C10 C11 -178.7(6) . . . . ? O4 S2 C12 C13 157.3(3) . . . . ? O3 S2 C12 C13 26.0(4) . . . . ? N6 S2 C12 C13 -84.3(4) . . . . ? O4 S2 C12 C17 -21.6(4) . . . . ? O3 S2 C12 C17 -152.8(3) . . . . ? N6 S2 C12 C17 96.8(4) . . . . ? C17 C12 C13 C14 -1.3(7) . . . . ? S2 C12 C13 C14 179.8(4) . . . . ? C12 C13 C14 C15 1.0(7) . . . . ? C13 C14 C15 N5 -179.1(5) . . . . ? C13 C14 C15 C16 -0.9(7) . . . . ? N5 C15 C16 C17 179.4(4) . . . . ? C14 C15 C16 C17 1.2(7) . . . . ? C15 C16 C17 C12 -1.5(6) . . . . ? C13 C12 C17 C16 1.6(6) . . . . ? S2 C12 C17 C16 -179.6(3) . . . . ? C21 N7 C18 N8 2.0(7) . . . . ? C21 N7 C18 N6 -178.7(4) . . . . ? C19 N8 C18 N7 -2.2(7) . . . . ? C19 N8 C18 N6 178.4(5) . . . . ? S2 N6 C18 N7 -12.1(5) . . . . ? S2 N6 C18 N8 167.3(3) . . . . ? C18 N8 C19 C20 0.2(9) . . . . ? N8 C19 C20 C21 1.8(10) . . . . ? C18 N7 C21 C20 0.3(7) . . . . ? C18 N7 C21 C22 -178.9(4) . . . . ? C19 C20 C21 N7 -2.0(9) . . . . ? C19 C20 C21 C22 177.1(6) . . . . ? 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 N2 H1N2 N8 0.80(5) 2.13(5) 2.931(6) 174(4) . N6 H1N6 N4 0.97(7) 1.93(7) 2.900(5) 177(6) . _refine_diff_density_max 0.279 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.054 _shelx_res_file ; 190k_smz-f1_a.res created by SHELXL-2014/7 TITL 190k_smz-f1_a.res in Pna2(1) REM Old TITL 013_190K_SulfamerazineF1_ in Pna2(1) REM SHELXT solution in Pna2(1) REM R1 0.106, Rweak 0.033, Alpha 0.003, Orientation as input REM Flack x = -0.022 ( 0.076 ) from Parsons' quotients REM Formula found by SHELXT: C26 N4 O4 S2 CELL 0.68890 14.4701 8.1889 21.8216 90.000 90.000 90.000 ZERR 8.000 0.0001 0.0001 0.0004 0.000 0.000 0.000 REM SG 33 4 4 Pna21 PGmm2 Orthorhombic LATT -1 REM SG ASUN 1 .5 .5 1. REM SG ORGN on 2(1) SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC C H N O S UNIT 88.00 96.00 32.00 16.00 8.00 L.S. 10 SIZE 0.50 0.40 0.20 BOND $H FMAP 2 PLAN 20 ACTA CONF EQIV $1 x, y-1, z HTAB N5 O4_$1 EQIV $2 -x+3/2, y+1/2, z-1/2 HTAB N1 O4_$2 EQIV $3 x, y+1, z HTAB N1 O1_$3 HTAB N2 N8 HTAB N6 N4 LIST 4 WGHT 0.054100 0.358700 FVAR 0.58269 0.35344 S1 5 0.355435 0.505220 0.656148 11.00000 0.02365 0.02608 = 0.02546 0.00258 -0.00134 -0.00141 S2 5 0.422082 0.502533 0.346986 11.00000 0.02243 0.02629 = 0.02530 0.00301 -0.00047 -0.00140 O1 4 0.312243 0.629830 0.692082 11.00000 0.03662 0.02712 = 0.03856 -0.00452 -0.00223 -0.00052 O2 4 0.453022 0.477777 0.662805 11.00000 0.02528 0.03954 = 0.03297 0.00459 -0.00717 -0.00289 O3 4 0.324266 0.529547 0.340151 11.00000 0.02370 0.03911 = 0.02902 0.00571 -0.00325 -0.00321 O4 4 0.464365 0.375056 0.311811 11.00000 0.03641 0.02548 = 0.03384 -0.00288 -0.00294 -0.00095 N1 3 0.158378 -0.116932 0.687624 11.00000 0.03482 0.02765 = 0.05226 -0.00480 0.01368 -0.00434 N2 3 0.346162 0.553297 0.582919 11.00000 0.02073 0.03627 = 0.03220 0.00553 -0.00266 0.00181 N3 3 0.186554 0.591711 0.582917 11.00000 0.02326 0.03142 = 0.03155 0.00125 0.00081 0.00321 N4 3 0.272323 0.569493 0.489850 11.00000 0.03190 0.06589 = 0.02368 0.00355 -0.00384 0.01071 N5 3 0.619924 1.120229 0.305182 11.00000 0.04082 0.02828 = 0.06979 -0.00438 0.01982 -0.00737 AFIX 93 H5A 2 0.676506 1.118991 0.293130 11.00000 -1.30000 H5B 2 0.592491 1.211778 0.311663 11.00000 -1.30000 AFIX 0 N6 3 0.431526 0.460215 0.420347 11.00000 0.02163 0.03959 = 0.02467 0.00760 0.00256 0.00152 N7 3 0.590473 0.412821 0.419262 11.00000 0.02485 0.03613 = 0.03477 0.00294 0.00307 0.00364 N8 3 0.504813 0.434038 0.512422 11.00000 0.02880 0.06628 = 0.03176 0.00332 0.00010 0.01074 C1 1 0.296206 0.322527 0.666771 11.00000 0.02250 0.02653 = 0.02404 0.00245 0.00190 0.00093 C2 1 0.206264 0.320885 0.690196 11.00000 0.02332 0.02681 = 0.03035 0.00065 -0.00105 0.00275 AFIX 43 H2 2 0.177391 0.418164 0.701017 11.00000 -1.30000 AFIX 0 C3 1 0.160893 0.175154 0.697119 11.00000 0.02439 0.03030 = 0.02631 -0.00182 0.00274 0.00314 AFIX 43 H3 2 0.101002 0.174047 0.712576 11.00000 -1.30000 AFIX 0 C4 1 0.203972 0.027272 0.681092 11.00000 0.02987 0.02728 = 0.02216 -0.00125 -0.00009 -0.00070 C5 1 0.294901 0.030255 0.657641 11.00000 0.02529 0.02878 = 0.02965 -0.00407 0.00288 0.00294 AFIX 43 H5 2 0.324347 -0.066747 0.647152 11.00000 -1.30000 AFIX 0 C6 1 0.339774 0.176892 0.650357 11.00000 0.02190 0.03034 = 0.03485 -0.00098 0.00603 0.00276 AFIX 43 H6 2 0.399378 0.179087 0.634435 11.00000 -1.30000 AFIX 0 C7 1 0.264256 0.572165 0.550696 11.00000 0.02638 0.02931 = 0.03186 0.00591 -0.00326 0.00225 C8 1 0.193760 0.593765 0.458889 11.00000 0.03914 0.10300 = 0.03469 0.00074 -0.01138 0.02250 AFIX 43 H8 2 0.195702 0.595393 0.416294 11.00000 -1.30000 AFIX 0 C9 1 0.110041 0.616452 0.487746 11.00000 0.02833 0.08921 = 0.04058 -0.00401 -0.01467 0.01128 AFIX 43 H9 2 0.056322 0.634129 0.465308 11.00000 -1.30000 AFIX 0 C10 1 0.108343 0.612176 0.550520 11.00000 0.02403 0.04132 = 0.04576 -0.00247 -0.00417 0.00557 C11 1 0.021782 0.631654 0.586509 11.00000 0.02842 0.06146 = 0.06161 -0.00578 -0.00061 0.00827 AFIX 137 H11A 2 0.017238 0.741996 0.601060 11.00000 -1.30000 H11B 2 0.022635 0.558157 0.620778 11.00000 -1.30000 H11C 2 -0.030412 0.607383 0.560925 11.00000 -1.30000 AFIX 0 C12 1 0.480656 0.683243 0.334485 11.00000 0.02620 0.02464 = 0.02284 0.00122 0.00147 0.00017 C13 1 0.436180 0.831202 0.344926 11.00000 0.02363 0.02843 = 0.03453 -0.00090 0.00501 0.00324 AFIX 43 H13 2 0.375230 0.832210 0.358442 11.00000 -1.30000 AFIX 0 C14 1 0.482231 0.976548 0.335288 11.00000 0.03288 0.02318 = 0.05349 -0.00079 0.00502 0.00468 AFIX 43 H14 2 0.452333 1.074975 0.342967 11.00000 -1.30000 AFIX 0 C15 1 0.573758 0.977191 0.314007 11.00000 0.02986 0.02706 = 0.02939 0.00064 0.00448 -0.00106 C16 1 0.617802 0.827494 0.303584 11.00000 0.02450 0.02842 = 0.02857 -0.00346 0.00620 -0.00183 AFIX 43 H16 2 0.678810 0.826015 0.290188 11.00000 -1.30000 AFIX 0 C17 1 0.571699 0.682193 0.312966 11.00000 0.02598 0.02732 = 0.01865 -0.00062 0.00620 0.00082 AFIX 43 H17 2 0.601156 0.583524 0.304982 11.00000 -1.30000 AFIX 0 C18 1 0.514042 0.433625 0.451439 11.00000 0.02471 0.03127 = 0.03346 -0.00117 0.00101 0.00212 C19 1 0.582856 0.404609 0.543336 11.00000 0.03876 0.09530 = 0.03380 0.00471 -0.00445 0.02019 AFIX 43 H19 2 0.580661 0.403027 0.585926 11.00000 -1.30000 AFIX 0 C20 1 0.666212 0.376581 0.514947 11.00000 0.03173 0.09116 = 0.04844 -0.00919 -0.00652 0.02463 AFIX 43 H20 2 0.719234 0.353440 0.537414 11.00000 -1.30000 AFIX 0 C21 1 0.668025 0.384208 0.451500 11.00000 0.02587 0.04516 = 0.04012 -0.00371 0.00067 0.00563 C22 1 0.754661 0.363884 0.414898 11.00000 0.02847 0.07045 = 0.05427 -0.00556 0.00732 0.01003 AFIX 137 H22A 2 0.751669 0.263668 0.392158 11.00000 -1.30000 H22B 2 0.806883 0.361040 0.442011 11.00000 -1.30000 H22C 2 0.761037 0.453900 0.387034 11.00000 -1.30000 AFIX 0 H1N1 2 0.108033 -0.125053 0.707306 11.00000 0.03797 H2N1 2 0.189534 -0.205620 0.686507 11.00000 0.04186 H1N2 2 0.387792 0.513468 0.563805 11.00000 0.03105 H1N6 2 0.378453 0.500748 0.443233 11.00000 0.08620 HKLF 4 REM 190k_smz-f1_a.res in Pna2(1) REM R1 = 0.0481 for 5154 Fo > 4sig(Fo) and 0.0626 for all 6404 data REM 344 parameters refined using 1 restraints END WGHT 0.0507 0.6034 REM Highest difference peak 0.279, deepest hole -0.346, 1-sigma level 0.054 Q1 1 0.1956 0.1042 0.7011 11.00000 0.05 0.28 Q2 1 0.4662 0.7587 0.3368 11.00000 0.05 0.25 Q3 1 0.1917 0.2389 0.7019 11.00000 0.05 0.25 Q4 1 0.3234 0.4086 0.6693 11.00000 0.05 0.23 Q5 1 0.5761 0.7762 0.3027 11.00000 0.05 0.21 Q6 1 0.4657 0.4399 0.5405 11.00000 0.05 0.21 Q7 1 0.3232 0.5704 0.6807 11.00000 0.05 0.21 Q8 1 0.4652 0.9022 0.3476 11.00000 0.05 0.20 Q9 1 0.2422 0.0420 0.6485 11.00000 0.05 0.20 Q10 1 0.6794 0.4397 0.4917 11.00000 0.05 0.20 Q11 1 0.8030 0.4410 0.4297 11.00000 0.05 0.19 Q12 1 0.7992 0.4729 0.3414 11.00000 0.05 0.19 Q13 1 0.4712 0.5748 0.3475 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-19 -4 2 14.55 6.71 -19 4 2 33.44 12.50 -19 -4 3 0.72 3.58 -19 -4 4 11.24 4.93 -19 -4 5 3.64 5.08 -19 -4 6 1.58 3.50 -20 0 -7 16.90 6.85 -20 0 -6 -2.04 3.24 -20 0 -5 146.45 18.24 -20 0 -4 432.67 30.38 -20 0 -3 12.25 4.44 -20 0 -2 479.32 31.62 -20 0 -1 60.57 11.98 -20 0 0 -0.24 3.79 -20 0 1 45.43 10.31 -20 0 2 443.66 31.08 -20 0 3 11.82 5.14 -20 0 4 389.62 30.55 -20 0 5 195.00 21.56 -20 0 6 -6.09 5.15 -20 -1 -7 3.96 3.16 -20 1 -7 0.08 3.42 -20 -1 -6 3.32 2.74 -20 1 -6 0.95 2.78 -20 -1 -5 3.70 4.49 -20 1 -5 13.87 7.49 -20 -1 -4 -0.92 4.10 -20 1 -4 1.08 4.25 -20 -1 -3 62.84 11.98 -20 1 -3 32.82 9.22 -20 -1 -2 13.24 7.18 -20 1 -2 7.62 7.01 -20 -1 -1 5.20 5.03 -20 1 -1 4.03 3.47 -20 -1 0 7.26 4.26 -20 1 0 -3.68 4.27 -20 -1 1 3.05 2.70 -20 1 1 6.36 3.97 -20 -1 2 22.83 8.63 -20 1 2 8.88 6.57 -20 -1 3 45.59 10.74 -20 1 3 62.62 12.45 -20 -1 4 -6.66 5.47 -20 1 4 -2.88 3.05 -20 -1 5 11.90 7.25 -20 1 5 7.96 6.13 -20 -1 6 1.67 3.36 -20 -1 7 6.44 4.44 -20 -2 -5 4.26 5.66 -20 2 -5 7.98 4.58 -20 -2 -4 39.62 10.51 -20 2 -4 26.98 10.24 -20 -2 -3 16.30 7.45 -20 2 -3 8.85 4.88 -20 -2 -2 192.77 20.48 -20 2 -2 154.36 18.75 -20 -2 -1 4.55 3.37 -20 2 -1 8.34 6.54 -20 -2 0 0.55 3.90 -20 2 0 0.84 4.95 -20 -2 1 15.86 7.07 -20 2 1 12.25 6.65 -20 -2 2 156.41 19.11 -20 2 2 200.24 21.12 -20 -2 3 29.82 9.25 -20 2 3 13.17 6.76 -20 -2 4 24.37 7.73 -20 -2 5 2.33 4.14 0 0 0 0.00 0.00 TITL 013_190K_SulfamerazineF1_ in Pna2(1) REM Pna2(1) (#33, found as Pbn2(1) in ba-c setting) CELL 0.68890 14.470070 8.188921 21.821636 90.0000 90.0000 90.0000 ZERR 8.00 0.000146 0.000085 0.000354 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z+1/2 SYMM x+1/2,-y+1/2, z SYMM -x+1/2, y+1/2, z+1/2 SFAC C H N O S UNIT 88.00 96.00 32.00 16.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 32560