data_smz_f2_230 _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 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' _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+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' _cell_length_a 9.1074(3) _cell_length_b 11.6193(5) _cell_length_c 22.8456(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2417.56(16) _cell_formula_units_Z 8 _cell_measurement_temperature 229.9(1) _cell_measurement_reflns_used 2206 _cell_measurement_theta_min 4.2030 _cell_measurement_theta_max 29.0350 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.452 _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 0.268 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98008 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; crysalispro, agilent technologies, version 1.171.37.33 (release 27-03-2014 crysalis171 .net) (compiled mar 27 2014,17:12:48) empirical absorption correction using spherical harmonics, implemented in scale3 abspack scaling algorithm. ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 229.9(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1048 _diffrn_reflns_number 7239 _diffrn_reflns_av_unetI/netI 0.0371 _diffrn_reflns_av_R_equivalents 0.0247 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.507 _diffrn_reflns_theta_max 29.370 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.866 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.866 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.866 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 2885 _reflns_number_gt 2185 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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 ; 'Tue Feb 03 15:46:58 2015' ; _computing_cell_refinement ; 'Tue Feb 03 15:46:58 2015' ; _computing_data_reduction ; 'Tue Feb 03 15:46:58 2015' ; _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^)+(0.0422P)^2^+0.9545P] 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_number_reflns 2885 _refine_ls_number_parameters 176 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1113 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.001 _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 0.66764(5) 0.34635(4) 0.38969(2) 0.02799(15) Uani 1 1 d . . . . . O1 O 0.80253(14) 0.39718(13) 0.40966(6) 0.0348(4) Uani 1 1 d . . . . . O2 O 0.65789(17) 0.22400(12) 0.38633(7) 0.0380(4) Uani 1 1 d . . . . . N1 N 0.5443(2) 0.5327(2) 0.15495(9) 0.0454(5) Uani 1 1 d D . . . . N2 N 0.54881(18) 0.39490(15) 0.43742(8) 0.0303(4) Uani 1 1 d D . . . . N3 N 0.33381(17) 0.42621(15) 0.48533(7) 0.0310(4) Uani 1 1 d . . . . . N4 N 0.34448(18) 0.28554(14) 0.40902(8) 0.0325(4) Uani 1 1 d . . . . . C1 C 0.6245(2) 0.40399(17) 0.32166(9) 0.0287(4) Uani 1 1 d . . . . . C2 C 0.6678(2) 0.51514(18) 0.30789(9) 0.0317(5) Uani 1 1 d . . . . . H2 H 0.7151 0.5602 0.3358 0.041 Uiso 1 1 calc R U . . . C3 C 0.6406(2) 0.55881(18) 0.25285(10) 0.0350(5) Uani 1 1 d . . . . . H3 H 0.6712 0.6330 0.2437 0.045 Uiso 1 1 calc R U . . . C4 C 0.5673(2) 0.49300(18) 0.21035(9) 0.0335(5) Uani 1 1 d . . . . . C5 C 0.5223(3) 0.38173(19) 0.22582(10) 0.0409(5) Uani 1 1 d . . . . . H5 H 0.4719 0.3369 0.1987 0.053 Uiso 1 1 calc R U . . . C6 C 0.5515(2) 0.3379(2) 0.28045(10) 0.0383(5) Uani 1 1 d . . . . . H6 H 0.5222 0.2635 0.2898 0.050 Uiso 1 1 calc R U . . . C7 C 0.4017(2) 0.36620(17) 0.44328(8) 0.0275(4) Uani 1 1 d . . . . . C8 C 0.1918(2) 0.4009(2) 0.49278(10) 0.0367(5) Uani 1 1 d . . . . . H8 H 0.1391 0.4405 0.5212 0.048 Uiso 1 1 calc R U . . . C9 C 0.1211(2) 0.3194(2) 0.46034(10) 0.0388(5) Uani 1 1 d . . . . . H9 H 0.0222 0.3033 0.4664 0.050 Uiso 1 1 calc R U . . . C10 C 0.2007(2) 0.26164(19) 0.41823(10) 0.0347(5) Uani 1 1 d . . . . . C11 C 0.1337(3) 0.1692(2) 0.38158(12) 0.0515(7) Uani 1 1 d . . . . . H11A H 0.1482 0.1869 0.3409 0.067 Uiso 1 1 calc R U . . . H11B H 0.0305 0.1645 0.3897 0.067 Uiso 1 1 calc R U . . . H11C H 0.1794 0.0969 0.3905 0.067 Uiso 1 1 calc R U . . . H1N1 H 0.552(3) 0.6055(16) 0.1466(12) 0.064(9) Uiso 1 1 d D . . . . H2N1 H 0.482(2) 0.493(2) 0.1339(11) 0.056(8) Uiso 1 1 d D . . . . H1N2 H 0.584(3) 0.4471(17) 0.4603(10) 0.044(7) Uiso 1 1 d 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 0.0284(3) 0.0304(3) 0.0252(2) -0.0024(2) 0.00037(18) 0.0036(2) O1 0.0259(7) 0.0484(9) 0.0300(8) -0.0020(7) 0.0000(6) 0.0029(7) O2 0.0497(9) 0.0281(8) 0.0363(8) -0.0021(6) 0.0005(7) 0.0069(7) N1 0.0600(13) 0.0407(12) 0.0354(11) 0.0047(9) -0.0150(9) -0.0027(11) N2 0.0274(8) 0.0340(10) 0.0296(9) -0.0100(8) 0.0029(7) -0.0035(8) N3 0.0279(8) 0.0365(10) 0.0286(9) -0.0027(8) 0.0026(7) -0.0017(8) N4 0.0335(9) 0.0327(10) 0.0312(9) -0.0014(7) -0.0035(7) -0.0045(8) C1 0.0302(9) 0.0295(10) 0.0264(10) -0.0007(8) -0.0004(8) 0.0012(9) C2 0.0347(10) 0.0289(11) 0.0315(10) -0.0063(9) -0.0065(8) 0.0013(9) C3 0.0424(11) 0.0253(11) 0.0373(11) 0.0014(9) -0.0053(9) -0.0006(9) C4 0.0361(10) 0.0339(11) 0.0304(11) -0.0003(9) -0.0062(9) 0.0054(9) C5 0.0507(13) 0.0369(12) 0.0350(12) -0.0027(10) -0.0145(10) -0.0076(11) C6 0.0468(12) 0.0324(12) 0.0356(12) 0.0008(10) -0.0066(10) -0.0087(10) C7 0.0281(9) 0.0296(11) 0.0247(9) 0.0034(8) 0.0007(8) -0.0005(9) C8 0.0299(10) 0.0474(14) 0.0327(11) 0.0026(10) 0.0044(8) -0.0006(10) C9 0.0281(10) 0.0494(14) 0.0389(12) 0.0091(11) -0.0016(9) -0.0076(10) C10 0.0352(10) 0.0342(11) 0.0347(11) 0.0084(10) -0.0097(9) -0.0079(10) C11 0.0475(13) 0.0497(15) 0.0572(16) -0.0044(13) -0.0115(12) -0.0140(12) _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 O2 1.4265(15) . ? S1 O1 1.4374(14) . ? S1 N2 1.6366(17) . ? S1 C1 1.737(2) . ? N1 C4 1.363(3) . ? N1 H1N1 0.870(17) . ? N1 H2N1 0.875(17) . ? N2 C7 1.387(2) . ? N2 H1N2 0.863(16) . ? N3 C8 1.337(2) . ? N3 C7 1.338(2) . ? N4 C7 1.327(2) . ? N4 C10 1.355(3) . ? C1 C6 1.385(3) . ? C1 C2 1.386(3) . ? C2 C3 1.378(3) . ? C2 H2 0.9300 . ? C3 C4 1.404(3) . ? C3 H3 0.9300 . ? C4 C5 1.402(3) . ? C5 C6 1.374(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.364(3) . ? C8 H8 0.9300 . ? C9 C10 1.379(3) . ? C9 H9 0.9300 . ? C10 C11 1.492(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 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 O2 S1 O1 118.67(9) . . ? O2 S1 N2 109.77(9) . . ? O1 S1 N2 102.25(9) . . ? O2 S1 C1 108.78(9) . . ? O1 S1 C1 108.59(9) . . ? N2 S1 C1 108.27(9) . . ? C4 N1 H1N1 121.3(19) . . ? C4 N1 H2N1 115.4(18) . . ? H1N1 N1 H2N1 116(3) . . ? C7 N2 S1 128.33(14) . . ? C7 N2 H1N2 118.1(16) . . ? S1 N2 H1N2 113.5(17) . . ? C8 N3 C7 115.06(18) . . ? C7 N4 C10 115.62(18) . . ? C6 C1 C2 119.92(19) . . ? C6 C1 S1 120.19(16) . . ? C2 C1 S1 119.85(15) . . ? C3 C2 C1 119.92(19) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 121.05(19) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? N1 C4 C5 120.1(2) . . ? N1 C4 C3 122.1(2) . . ? C5 C4 C3 117.83(19) . . ? C6 C5 C4 120.9(2) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 120.3(2) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? N4 C7 N3 127.57(18) . . ? N4 C7 N2 119.46(18) . . ? N3 C7 N2 112.96(17) . . ? N3 C8 C9 122.7(2) . . ? N3 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C8 C9 C10 117.9(2) . . ? C8 C9 H9 121.0 . . ? C10 C9 H9 121.0 . . ? N4 C10 C9 121.1(2) . . ? N4 C10 C11 117.1(2) . . ? C9 C10 C11 121.8(2) . . ? 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 . . ? 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 O2 S1 N2 C7 -46.9(2) . . . . ? O1 S1 N2 C7 -173.78(18) . . . . ? C1 S1 N2 C7 71.7(2) . . . . ? O2 S1 C1 C6 17.3(2) . . . . ? O1 S1 C1 C6 147.81(17) . . . . ? N2 S1 C1 C6 -101.90(18) . . . . ? O2 S1 C1 C2 -160.40(16) . . . . ? O1 S1 C1 C2 -29.92(19) . . . . ? N2 S1 C1 C2 80.36(18) . . . . ? C6 C1 C2 C3 -1.2(3) . . . . ? S1 C1 C2 C3 176.52(16) . . . . ? C1 C2 C3 C4 0.9(3) . . . . ? C2 C3 C4 N1 -177.4(2) . . . . ? C2 C3 C4 C5 0.3(3) . . . . ? N1 C4 C5 C6 176.5(2) . . . . ? C3 C4 C5 C6 -1.2(3) . . . . ? C4 C5 C6 C1 1.0(4) . . . . ? C2 C1 C6 C5 0.3(3) . . . . ? S1 C1 C6 C5 -177.47(18) . . . . ? C10 N4 C7 N3 -0.2(3) . . . . ? C10 N4 C7 N2 179.05(18) . . . . ? C8 N3 C7 N4 -0.3(3) . . . . ? C8 N3 C7 N2 -179.63(18) . . . . ? S1 N2 C7 N4 3.6(3) . . . . ? S1 N2 C7 N3 -176.96(15) . . . . ? C7 N3 C8 C9 0.5(3) . . . . ? N3 C8 C9 C10 -0.1(3) . . . . ? C7 N4 C10 C9 0.6(3) . . . . ? C7 N4 C10 C11 -178.44(19) . . . . ? C8 C9 C10 N4 -0.4(3) . . . . ? C8 C9 C10 C11 178.6(2) . . . . ? _refine_diff_density_max 0.286 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.055 _shelx_res_file ; smz_f2_230.res created by SHELXL-2014/7 TITL smz_f2_230_a.res in Pbca REM Old TITL smz_f2_230 in Pbca REM SHELXT solution in Pbca REM R1 0.127, Rweak 0.517, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C12 N3 O2 S CELL 0.71073 9.1074 11.6193 22.8456 90.000 90.000 90.000 ZERR 8.000 0.0003 0.0005 0.0009 0.000 0.000 0.000 REM SG 61 8 8 Pbca P21/b21/c21/a PGmmm Orthorhombic LATT 1 REM SG ASUN 1 .5 .5 .5 REM SG ORGN at Inv.cen. SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O S UNIT 88 96 32 16 8 DFIX 0.89 .02 N1 H1N1 N1 H2N1 N2 H1N2 FMAP 2 PLAN -32 BOND $H L.S. 12 ACTA CONF HTAB LIST 4 WGHT 0.042200 0.954500 FVAR 0.57551 S1 5 0.667645 0.346349 0.389693 11.00000 0.02839 0.03042 = 0.02516 -0.00238 0.00037 0.00356 O1 4 0.802531 0.397185 0.409657 11.00000 0.02590 0.04841 = 0.02999 -0.00201 -0.00005 0.00286 O2 4 0.657893 0.223998 0.386334 11.00000 0.04970 0.02807 = 0.03630 -0.00208 0.00052 0.00691 N1 3 0.544310 0.532708 0.154945 11.00000 0.06004 0.04072 = 0.03545 0.00470 -0.01504 -0.00270 N2 3 0.548810 0.394901 0.437423 11.00000 0.02745 0.03397 = 0.02963 -0.01001 0.00285 -0.00347 N3 3 0.333808 0.426206 0.485332 11.00000 0.02793 0.03650 = 0.02864 -0.00272 0.00259 -0.00169 N4 3 0.344480 0.285543 0.409024 11.00000 0.03354 0.03273 = 0.03119 -0.00137 -0.00353 -0.00447 C1 1 0.624488 0.403994 0.321662 11.00000 0.03021 0.02953 = 0.02640 -0.00074 -0.00037 0.00116 C2 1 0.667776 0.515144 0.307889 11.00000 0.03466 0.02888 = 0.03154 -0.00634 -0.00647 0.00125 AFIX 43 H2 2 0.715117 0.560181 0.335751 11.00000 -1.30000 AFIX 0 C3 1 0.640560 0.558808 0.252853 11.00000 0.04239 0.02531 = 0.03729 0.00139 -0.00531 -0.00062 AFIX 43 H3 2 0.671170 0.633025 0.243720 11.00000 -1.30000 AFIX 0 C4 1 0.567344 0.493004 0.210352 11.00000 0.03611 0.03393 = 0.03036 -0.00027 -0.00619 0.00535 C5 1 0.522312 0.381729 0.225816 11.00000 0.05067 0.03694 = 0.03504 -0.00267 -0.01452 -0.00764 AFIX 43 H5 2 0.471930 0.336929 0.198713 11.00000 -1.30000 AFIX 0 C6 1 0.551544 0.337888 0.280452 11.00000 0.04675 0.03241 = 0.03563 0.00076 -0.00662 -0.00867 AFIX 43 H6 2 0.522198 0.263461 0.289798 11.00000 -1.30000 AFIX 0 C7 1 0.401676 0.366202 0.443282 11.00000 0.02805 0.02959 = 0.02475 0.00337 0.00073 -0.00053 C8 1 0.191817 0.400911 0.492782 11.00000 0.02994 0.04739 = 0.03272 0.00258 0.00436 -0.00060 AFIX 43 H8 2 0.139111 0.440507 0.521244 11.00000 -1.30000 AFIX 0 C9 1 0.121070 0.319391 0.460342 11.00000 0.02807 0.04941 = 0.03887 0.00906 -0.00160 -0.00761 AFIX 43 H9 2 0.022222 0.303272 0.466436 11.00000 -1.30000 AFIX 0 C10 1 0.200728 0.261639 0.418232 11.00000 0.03522 0.03421 = 0.03468 0.00844 -0.00970 -0.00793 C11 1 0.133729 0.169241 0.381579 11.00000 0.04755 0.04969 = 0.05717 -0.00442 -0.01150 -0.01403 AFIX 137 H11A 2 0.148209 0.186851 0.340932 11.00000 -1.30000 H11B 2 0.030476 0.164533 0.389687 11.00000 -1.30000 H11C 2 0.179395 0.096888 0.390537 11.00000 -1.30000 AFIX 0 H1N1 2 0.551913 0.605544 0.146633 11.00000 0.06417 H2N1 2 0.481984 0.492886 0.133949 11.00000 0.05624 H1N2 2 0.584182 0.447123 0.460291 11.00000 0.04445 HKLF 4 REM smz_f2_230_a.res in Pbca REM R1 = 0.0435 for 2185 Fo > 4sig(Fo) and 0.0635 for all 2885 data REM 176 parameters refined using 3 restraints END WGHT 0.0400 0.9697 REM Instructions for potential hydrogen bonds EQIV $1 -x+3/2, y+1/2, z HTAB C2 O2_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C8 O1_$2 EQIV $3 x-1, y, z HTAB C9 O1_$3 EQIV $4 -x+1, y+1/2, -z+1/2 HTAB N1 O2_$4 HTAB N1 N4_$4 EQIV $5 x-1/2, y, -z+1/2 HTAB N1 O1_$5 HTAB N2 N3_$2 REM Highest difference peak 0.286, deepest hole -0.426, 1-sigma level 0.055 Q1 1 0.6402 0.3782 0.3494 11.00000 0.05 0.29 Q2 1 0.5955 0.5167 0.2373 11.00000 0.05 0.22 Q3 1 0.6136 0.5472 0.2813 11.00000 0.05 0.20 Q4 1 0.6142 0.4562 0.3221 11.00000 0.05 0.20 Q5 1 0.3758 0.3953 0.5297 11.00000 0.05 0.18 Q6 1 0.3605 0.2899 0.3714 11.00000 0.05 0.18 Q7 1 0.4062 0.4788 0.5015 11.00000 0.05 0.17 Q8 1 0.6321 0.3683 0.2985 11.00000 0.05 0.17 Q9 1 0.4031 0.2330 0.3812 11.00000 0.05 0.17 Q10 1 0.2732 0.2642 0.4290 11.00000 0.05 0.17 Q11 1 -0.1381 0.1588 0.3863 11.00000 0.05 0.17 Q12 1 0.7674 0.1573 0.3617 11.00000 0.05 0.16 Q13 1 0.1523 0.0945 0.4209 11.00000 0.05 0.16 Q14 1 0.6650 0.1550 0.3188 11.00000 0.05 0.16 Q15 1 0.6621 0.1968 0.3600 11.00000 0.05 0.16 Q16 1 0.5648 0.3352 0.5080 11.00000 0.05 0.15 Q17 1 0.6838 0.1201 0.3625 11.00000 0.05 0.15 Q18 1 0.5542 0.4332 0.4419 11.00000 0.05 0.15 Q19 1 0.5449 0.2114 0.3622 11.00000 0.05 0.15 Q20 1 0.7348 0.6182 0.2301 11.00000 0.05 0.15 Q21 1 0.3667 0.3449 0.4163 11.00000 0.05 0.15 Q22 1 0.5584 0.4307 0.2155 11.00000 0.05 0.15 Q23 1 0.1356 0.3131 0.4295 11.00000 0.05 0.15 Q24 1 0.6828 0.6147 0.1679 11.00000 0.05 0.15 Q25 1 0.6799 0.7046 0.2171 11.00000 0.05 0.15 Q26 1 0.3662 0.3748 0.4706 11.00000 0.05 0.15 Q27 1 0.3248 0.2220 0.5116 11.00000 0.05 0.15 Q28 1 0.3404 0.1339 0.4475 11.00000 0.05 0.14 Q29 1 0.6318 0.6155 0.2510 11.00000 0.05 0.14 Q30 1 0.5513 0.5175 0.1006 11.00000 0.05 0.14 Q31 1 0.6402 0.5814 0.3976 11.00000 0.05 0.14 Q32 1 0.0035 0.2228 0.4881 11.00000 0.05 0.14 ; _shelx_res_checksum 19920 _shelx_hkl_file ; 0 0 -4 2907.80 20.72 0 0 -5 11.31 3.15 0 0 -6 7302.25 40.81 0 0 -7 19.30 4.57 0 0 -8 1185.89 18.84 0 0 -9 14.24 3.09 0 0 -10 5711.85 46.23 0 0 -11 95.45 7.25 0 0 -12 2.03 1.44 0 0 -13 1.24 1.83 0 0 -14 864.02 21.44 0 0 -15 24.99 4.16 0 0 -16 18.79 3.32 0 0 17 22.30 6.92 0 0 18 1531.42 39.85 0 0 19 65.36 10.49 0 0 20 163.83 13.90 0 0 21 11.45 5.33 0 0 22 248.58 18.21 0 0 23 10.74 6.12 0 0 24 84.15 11.52 0 0 25 6.39 4.22 0 0 26 54.37 10.56 0 0 27 -0.48 3.66 0 0 28 55.46 10.77 0 0 29 9.15 5.89 0 1 -4 0.23 1.22 0 -1 4 26.86 3.37 0 1 -5 1.05 1.07 0 1 5 -1.30 1.22 0 -1 5 1.35 1.21 0 1 6 0.91 1.30 0 -1 6 -2.21 1.79 0 1 7 3.89 1.74 0 -1 7 -2.38 1.91 0 -1 8 -0.59 1.86 0 1 8 4.75 2.04 0 -1 9 -2.12 1.45 0 -1 10 -0.42 2.50 0 -1 11 -4.46 3.20 0 1 -12 5.11 2.60 0 -1 12 -0.07 2.72 0 -1 13 -0.52 1.92 0 1 -13 1.68 2.41 0 -1 14 0.24 2.34 0 1 -14 6.29 3.14 0 -1 15 -1.57 3.16 0 1 -15 2.21 2.40 0 -1 16 4.60 3.88 0 -1 17 0.03 3.32 0 -1 18 -0.46 3.69 0 -1 19 -1.86 3.77 0 -1 20 -7.14 4.51 0 -1 21 -1.35 3.05 0 1 22 -5.35 4.48 0 -1 22 1.34 2.89 0 -1 23 -1.84 3.46 0 1 23 -2.95 4.71 0 -1 24 -1.10 4.13 0 1 24 -2.27 4.42 0 1 25 3.81 4.98 0 -1 25 6.45 4.24 0 1 26 -2.65 5.11 0 -1 26 4.42 4.21 0 1 27 -4.61 4.61 0 -1 27 -0.75 3.48 0 -1 28 3.82 3.98 0 1 28 0.83 3.69 0 -1 29 0.22 3.22 0 1 29 -6.55 6.32 0 2 0 6.54 1.36 0 2 -1 7339.10 37.79 0 2 1 7201.61 39.51 0 2 2 4524.37 33.49 0 -2 2 4532.51 30.05 0 -2 3 9999.00 47.47 0 2 -3 9902.38 51.43 0 2 -4 8016.74 48.54 0 -2 4 8298.03 49.33 0 2 -5 8344.43 52.78 0 -2 5 8358.50 52.71 0 -2 6 8183.63 55.16 0 2 -6 8192.11 55.74 0 -2 7 85.45 6.29 0 2 -7 78.04 5.79 0 2 8 572.30 12.46 0 2 -8 593.65 16.65 0 -2 8 591.14 16.53 0 2 9 1971.82 24.29 0 -2 9 1960.84 31.77 0 2 10 981.16 18.04 0 -2 10 1023.92 24.21 0 -2 11 1451.30 30.52 0 2 11 1386.45 22.40 0 2 12 608.47 15.60 0 -2 12 668.61 21.66 0 -2 13 170.23 11.98 0 -2 14 791.89 25.38 0 -2 15 47.67 7.69 0 -2 16 93.10 9.98 0 -2 17 548.20 23.61 0 -2 18 303.18 18.80 0 -2 19 813.42 30.39 0 -2 20 133.62 13.30 0 -2 21 85.62 11.13 0 -2 22 17.73 6.79 0 -2 23 502.62 27.14 0 -2 24 30.79 7.92 0 -2 25 24.59 7.29 0 -2 26 115.97 14.16 0 2 26 100.19 13.49 0 -2 27 15.91 6.03 0 2 27 14.00 6.27 0 -2 28 11.73 6.04 0 2 28 20.30 7.57 0 2 29 71.01 12.27 0 -2 29 83.85 13.10 0 -3 0 -0.66 1.52 0 3 0 0.76 1.24 0 -3 1 0.13 1.39 0 3 1 -0.85 1.39 0 3 -1 0.91 1.18 0 -3 -1 2.84 1.57 0 -3 2 0.08 1.35 0 3 -2 -0.15 1.36 0 3 2 0.10 1.39 0 -3 -2 2.84 1.94 0 3 3 0.30 1.09 0 3 -3 1.77 1.56 0 3 4 1.20 1.43 0 -3 4 0.24 1.62 0 3 -4 -0.91 1.58 0 -3 5 3.95 2.24 0 3 -5 1.33 1.45 0 -3 6 12.21 4.00 0 3 -6 3.44 1.62 0 3 -7 1.34 1.60 0 -3 7 -0.75 1.56 0 -3 8 2.62 2.22 0 3 -8 0.59 1.34 0 -3 9 1.73 2.23 0 3 -9 -1.16 1.32 0 -3 10 1.98 2.02 0 3 -10 -0.58 1.89 0 3 11 -1.27 1.77 0 -3 11 1.32 2.54 0 -3 12 0.00 2.06 0 3 12 -1.59 1.81 0 3 13 2.34 1.52 0 -3 13 -1.17 2.26 0 3 14 1.57 2.35 0 -3 14 -1.97 2.71 0 3 15 1.47 2.33 0 -3 15 1.98 2.75 0 -3 16 -1.57 2.75 0 -3 17 1.67 2.39 0 -3 18 4.39 3.51 0 -3 19 0.95 2.64 0 -3 20 1.59 3.29 0 -3 21 5.08 4.11 0 -3 22 -6.04 4.15 0 -3 23 -3.65 4.19 0 -3 24 2.62 3.04 0 -3 25 -6.54 4.82 0 -3 26 -1.18 3.12 0 -3 27 -2.11 4.22 0 3 28 -5.63 5.00 0 -3 28 2.68 4.69 0 -3 29 -0.84 3.88 0 -4 0 4260.29 40.81 0 4 0 4412.95 41.89 0 4 1 1622.91 25.74 0 -4 1 1579.68 24.73 0 -4 -1 1528.44 25.18 0 4 -1 1625.11 25.10 0 -4 -2 1941.34 28.80 0 4 -2 1873.77 26.80 0 -4 2 1822.88 26.65 0 4 2 1829.09 28.06 0 4 3 125.73 7.65 0 -4 -3 130.42 7.72 0 -4 3 121.47 6.96 0 4 -3 133.42 7.39 0 -4 4 238.85 9.92 0 4 -4 243.92 10.07 0 4 4 235.56 10.85 0 4 -5 275.25 11.94 0 4 5 299.01 12.49 0 -4 5 282.80 11.08 0 4 6 862.05 22.09 0 -4 6 826.10 19.56 0 4 -6 850.86 21.34 0 4 -7 373.75 14.51 0 4 7 371.37 15.06 0 -4 7 376.35 13.80 0 -4 8 284.28 12.44 0 4 -8 274.26 12.83 0 -4 9 15.33 3.44 0 -4 9 15.55 3.73 0 -4 10 4.31 2.88 0 -4 11 109.06 9.01 0 -4 12 7.08 3.62 0 4 13 1.31 2.18 0 -4 13 2.47 3.05 0 4 14 194.02 9.89 0 -4 14 214.29 13.99 0 4 15 99.88 7.34 0 -4 15 110.27 10.54 0 -4 16 182.06 13.90 0 4 16 178.62 10.07 0 -4 17 627.15 26.56 0 4 17 638.32 19.35 0 -4 18 1615.46 42.74 0 -4 19 449.37 24.45 0 -4 20 12.93 6.25 0 -4 21 45.96 8.04 0 -4 22 0.68 2.73 0 -4 23 119.38 14.09 0 -4 24 334.52 23.21 0 -4 25 139.05 15.49 0 -4 26 9.94 5.64 0 -4 27 2.46 4.44 0 -4 28 46.23 9.82 0 5 0 -0.09 1.62 0 -5 0 -1.41 2.03 0 -5 -1 1.87 1.94 0 5 1 -0.22 1.56 0 -5 1 -0.76 1.91 0 5 -1 -0.03 1.65 0 5 2 1.94 1.64 0 -5 -2 -0.04 1.91 0 5 -2 -0.64 1.29 0 -5 2 -3.38 1.85 0 5 3 -0.10 1.35 0 -5 3 2.05 2.12 0 5 -3 0.68 1.41 0 -5 -3 1.05 1.75 0 5 -4 -0.39 1.35 0 -5 4 -1.19 1.86 0 5 4 2.72 1.77 0 5 5 -0.10 1.95 0 -5 5 -2.74 1.94 0 5 -5 -0.97 1.57 0 -5 6 -4.63 3.01 0 5 -6 0.01 1.50 0 -5 7 -0.62 2.00 0 -5 8 0.86 1.99 0 -5 9 0.90 2.65 0 -5 10 0.88 2.01 0 -5 11 -1.38 2.11 0 -5 12 3.38 3.10 0 -5 13 2.09 3.48 0 -5 13 6.01 3.61 0 5 14 -2.49 2.67 0 -5 14 8.31 4.23 0 -5 15 -1.40 3.00 0 5 15 -2.26 2.63 0 -5 16 -1.00 3.45 0 5 16 -1.11 2.39 0 -5 17 4.98 4.00 0 5 17 3.61 2.87 0 -5 18 -4.91 3.89 0 5 18 4.57 2.72 0 5 19 4.33 2.90 0 -5 19 -1.41 3.78 0 -5 20 3.91 3.70 0 -5 21 -0.85 3.21 0 -5 22 -0.09 3.83 0 -5 23 -3.49 3.87 0 -5 24 -3.85 4.99 0 -5 25 2.05 4.05 0 -5 26 0.58 3.25 0 -5 27 2.67 3.12 0 -5 28 17.63 7.33 0 -6 0 17.67 3.60 0 6 0 24.27 3.85 0 -6 1 4171.76 49.58 0 6 1 4246.27 51.11 0 6 -1 4225.92 50.23 0 -6 -1 4169.17 51.08 0 -6 -2 1421.99 30.34 0 6 -2 1409.75 29.07 0 -6 2 1428.35 28.95 0 -6 3 271.23 12.72 0 6 -3 273.28 12.96 0 -6 -3 265.05 13.14 0 -6 4 660.96 19.90 0 6 -4 684.28 20.38 0 6 -5 29.38 4.57 0 -6 5 28.12 4.05 0 -6 6 5.38 2.48 0 -6 7 346.01 15.23 0 -6 8 60.23 6.47 0 -6 9 53.87 6.34 0 -6 10 67.28 7.22 0 -6 11 7.82 4.29 0 -6 12 3406.64 53.29 0 -6 13 7.50 4.53 0 -6 14 310.94 17.42 0 -6 15 616.49 24.79 0 -6 16 87.19 9.77 0 6 16 65.34 6.55 0 -6 17 109.48 11.79 0 6 17 85.19 7.53 0 -6 18 576.15 26.18 0 6 18 512.35 18.55 0 6 19 323.40 14.89 0 -6 19 321.57 20.15 0 -6 20 88.78 12.51 0 -6 20 78.80 11.08 0 -6 21 435.91 25.48 0 -6 21 417.76 24.16 0 -6 22 265.68 20.77 0 -6 22 302.06 21.25 0 -6 23 14.12 5.27 0 -6 23 15.27 6.23 0 -6 24 62.22 10.79 0 -6 25 149.73 16.84 0 -6 26 184.21 18.82 0 -6 27 13.61 7.27 0 -6 27 7.43 5.48 0 -6 28 113.45 15.03 0 -7 0 -1.72 2.62 0 -7 -1 3.78 3.12 0 -7 1 1.79 2.06 0 -7 -2 3.77 3.24 0 -7 2 -1.91 2.70 0 -7 -3 1.89 2.76 0 -7 3 2.50 2.81 0 -7 4 -3.34 2.94 0 -7 5 3.77 2.81 0 -7 6 0.90 1.92 0 -7 7 1.92 2.21 0 -7 8 -3.83 3.34 0 -7 9 -1.69 3.19 0 -7 10 -5.23 4.48 0 -7 11 1.68 3.08 0 -7 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22 336.43 23.93 0 -10 23 0.41 3.31 0 -11 0 0.72 2.65 0 -11 1 -0.71 3.50 0 -11 -1 1.12 2.76 0 -11 2 -2.59 2.99 0 -11 -2 0.67 3.01 0 -11 3 2.31 3.20 0 -11 4 -3.36 3.33 0 -11 5 0.33 2.68 0 -11 6 0.01 2.65 0 -11 7 2.00 3.81 0 -11 8 -1.10 2.78 0 -11 9 -2.37 3.68 0 -11 10 1.27 3.59 0 -11 11 -2.67 3.22 0 -11 12 1.63 2.83 0 -11 13 -2.00 3.14 0 -11 14 -4.39 3.83 0 -11 15 -3.35 3.32 0 -11 16 -4.24 4.24 0 -11 17 -2.29 3.72 0 -11 18 2.81 3.85 0 -11 19 -3.64 4.03 0 -11 20 3.40 4.70 0 -11 21 0.59 3.11 0 -12 0 192.04 16.42 0 -12 -1 8.50 4.86 0 -12 1 2.26 3.88 0 -12 2 1.33 3.79 0 -12 -2 2.14 3.29 0 -12 3 143.76 14.51 0 -12 4 9.48 4.45 0 -12 5 111.07 12.27 0 -12 6 2.54 3.99 0 -12 7 30.50 6.88 0 -12 8 25.83 6.43 0 -12 9 25.63 7.02 0 -12 10 352.50 22.65 0 -12 11 153.88 15.05 0 -12 12 44.47 8.21 0 -12 13 1.05 3.03 0 -12 14 15.12 5.69 0 -12 15 -0.59 3.36 0 -12 16 6.45 4.11 0 -12 17 11.39 5.32 0 -12 18 13.86 5.76 0 -13 0 2.85 3.34 0 -13 1 0.42 3.59 0 -13 -1 4.42 3.92 0 -13 2 2.60 3.42 0 -13 3 0.33 4.10 0 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11.29 6.89 11 -1 13 33.61 8.22 11 -1 14 21.52 6.96 11 -1 15 -1.31 3.52 -11 2 0 -3.15 4.44 -11 2 -1 42.83 8.73 -11 2 1 38.81 8.65 -11 2 2 84.98 13.03 -11 2 -2 96.82 13.33 -11 2 3 -5.73 4.99 -11 2 -3 -5.00 5.37 -11 2 4 34.05 8.51 -11 2 -4 19.52 6.21 -11 2 5 24.94 7.81 -11 2 -5 25.67 6.95 -11 2 6 0.47 3.31 -11 2 7 7.30 5.00 -11 2 8 20.16 7.29 11 -2 9 37.76 8.42 11 -2 10 41.89 8.60 11 -2 11 67.79 11.07 11 -2 12 4.81 3.73 11 -2 13 29.90 7.79 11 -2 14 -4.40 4.83 -11 3 0 -6.22 5.46 -11 3 -1 2.51 4.41 -11 3 1 -0.98 5.18 -11 3 -2 2.19 3.25 -11 3 2 -2.27 3.41 -11 3 -3 -6.47 5.11 -11 3 3 4.70 4.34 -11 3 -4 -1.12 4.66 -11 3 4 -4.72 4.58 11 -3 5 53.99 9.12 -11 3 -5 41.79 8.37 -11 3 5 38.68 9.54 -11 3 6 9.70 5.48 -11 3 -6 4.17 3.26 11 -3 6 15.31 5.47 -11 3 7 5.23 3.96 11 -3 7 -3.42 3.40 11 -3 8 -1.91 3.38 11 -3 9 0.97 2.90 11 -3 10 15.39 6.04 11 -3 11 -4.40 4.62 11 -3 12 -2.74 4.34 11 -3 13 43.03 9.54 -11 4 0 2.48 3.98 -11 4 -1 100.37 13.86 -11 4 1 76.32 12.14 -11 4 -2 4.16 3.67 -11 4 2 16.17 6.30 11 -4 3 4.47 2.68 -11 4 -3 5.66 4.58 11 -4 4 2.40 2.65 -11 4 -4 5.29 3.14 -11 4 4 1.35 5.56 11 -4 5 -2.16 3.88 -11 4 -5 -4.25 3.82 -11 4 5 -3.40 4.89 11 -4 6 0.49 2.98 11 -4 7 4.33 3.04 11 -4 8 16.39 5.35 11 -4 9 15.11 5.82 11 -4 10 84.19 12.83 11 -4 11 -0.02 3.00 -11 5 0 6.65 4.90 11 -5 0 -1.68 3.30 11 -5 1 40.40 8.85 -11 5 1 50.50 10.82 -11 5 2 114.31 15.57 11 -5 2 108.89 13.46 11 -5 3 2.03 2.91 11 -5 4 17.62 5.71 11 -5 5 4.69 4.45 11 -5 6 38.66 8.84 11 -5 7 -2.86 4.39 11 -5 8 1.89 3.32 11 -5 9 2.10 3.24 11 -6 0 1.61 3.35 11 -6 1 57.02 10.46 11 -6 -1 51.14 9.93 11 -6 -2 108.67 13.67 11 -6 2 107.84 14.39 11 -6 3 9.53 4.99 11 -6 4 12.77 6.13 11 -6 5 -1.94 4.13 11 -6 6 23.22 7.41 11 -6 7 2.45 4.41 11 -7 0 5.06 5.26 11 -7 -1 54.26 10.41 11 -7 1 44.18 9.65 11 -7 2 30.25 8.02 11 -7 -2 36.75 8.67 11 -7 3 0.44 3.77 11 -7 -3 13.46 5.59 -12 0 0 17.92 6.62 -12 0 1 -2.15 3.75 -12 0 2 11.75 6.81 -12 0 3 7.67 6.32 -12 1 0 3.26 4.96 -12 1 1 24.65 7.81 -12 1 -1 16.18 6.22 -12 1 2 3.75 4.31 -12 1 3 4.27 4.56 -12 2 0 -0.80 3.27 -12 2 -1 0.29 3.51 -12 2 1 8.23 5.41 -12 2 -2 0.18 3.98 -12 3 -1 5.95 5.17 -12 3 -2 16.99 6.46 -12 3 -3 -2.17 3.92 0 0 0 0.00 0.00 TITL smz_f2_230 in Pbca REM Pbca (#61 in standard setting) CELL 0.71073 9.107372 11.619345 22.845585 90.0000 90.0000 90.0000 ZERR 6.00 0.000324 0.000549 0.000877 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O S UNIT 90.00 90.00 24.00 12.00 6.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 68460