data_smz_f2_260 _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 9.1228(4) _cell_length_b 11.6522(6) _cell_length_c 22.8488(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2428.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 260.0(1) _cell_measurement_reflns_used 2090 _cell_measurement_theta_min 4.2270 _cell_measurement_theta_max 28.7410 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.446 _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 0.267 _shelx_estimated_absorpt_T_min 0.878 _shelx_estimated_absorpt_T_max 0.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98515 _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 260.0(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 7159 _diffrn_reflns_av_unetI/netI 0.0368 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.609 _diffrn_reflns_theta_max 29.316 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.856 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.856 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.856 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 2852 _reflns_number_gt 2123 _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 18:18:40 2015' ; _computing_cell_refinement ; 'Tue Feb 03 18:18:40 2015' ; _computing_data_reduction ; 'Tue Feb 03 18:18:40 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^)+(0.0449P)^2^+0.6939P] 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 2852 _refine_ls_number_parameters 176 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0661 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 0.66728(5) 0.34663(4) 0.38977(2) 0.03185(16) Uani 1 1 d . . . . . O1 O 0.80199(15) 0.39721(13) 0.40954(6) 0.0397(4) Uani 1 1 d . . . . . O2 O 0.65746(17) 0.22445(12) 0.38622(7) 0.0432(4) Uani 1 1 d . . . . . N1 N 0.5437(3) 0.53286(19) 0.15520(9) 0.0519(6) Uani 1 1 d D . . . . N2 N 0.54878(19) 0.39487(15) 0.43747(8) 0.0345(4) Uani 1 1 d D . . . . N3 N 0.33399(18) 0.42635(15) 0.48541(8) 0.0348(4) Uani 1 1 d . . . . . N4 N 0.34450(19) 0.28601(14) 0.40921(8) 0.0368(4) Uani 1 1 d . . . . . C1 C 0.6238(2) 0.40438(17) 0.32187(9) 0.0318(4) Uani 1 1 d . . . . . C2 C 0.6665(2) 0.51527(17) 0.30799(10) 0.0360(5) Uani 1 1 d . . . . . H2 H 0.7134 0.5603 0.3359 0.047 Uiso 1 1 calc R U . . . C3 C 0.6396(2) 0.55896(17) 0.25310(11) 0.0402(5) Uani 1 1 d . . . . . H3 H 0.6702 0.6330 0.2440 0.052 Uiso 1 1 calc R U . . . C4 C 0.5667(2) 0.49332(18) 0.21073(10) 0.0385(5) Uani 1 1 d . . . . . C5 C 0.5219(3) 0.38245(19) 0.22590(10) 0.0463(6) Uani 1 1 d . . . . . H5 H 0.4719 0.3378 0.1987 0.060 Uiso 1 1 calc R U . . . C6 C 0.5511(3) 0.33868(19) 0.28059(10) 0.0441(6) Uani 1 1 d . . . . . H6 H 0.5218 0.2644 0.2899 0.057 Uiso 1 1 calc R U . . . C7 C 0.4021(2) 0.36649(16) 0.44335(9) 0.0312(4) Uani 1 1 d . . . . . C8 C 0.1924(2) 0.4012(2) 0.49274(10) 0.0418(5) Uani 1 1 d . . . . . H8 H 0.1398 0.4408 0.5212 0.054 Uiso 1 1 calc R U . . . C9 C 0.1215(2) 0.3202(2) 0.46036(10) 0.0428(5) Uani 1 1 d . . . . . H9 H 0.0228 0.3043 0.4664 0.056 Uiso 1 1 calc R U . . . C10 C 0.2012(2) 0.26253(18) 0.41816(10) 0.0393(5) Uani 1 1 d . . . . . C11 C 0.1343(3) 0.1698(2) 0.38183(12) 0.0581(7) Uani 1 1 d . . . . . H11A H 0.1470 0.1876 0.3411 0.076 Uiso 1 1 calc R U . . . H11B H 0.0316 0.1642 0.3905 0.076 Uiso 1 1 calc R U . . . H11C H 0.1812 0.0980 0.3905 0.076 Uiso 1 1 calc R U . . . H1N1 H 0.550(3) 0.6051(16) 0.1457(13) 0.082(10) Uiso 1 1 d D . . . . H2N1 H 0.480(2) 0.4926(19) 0.1346(11) 0.057(8) Uiso 1 1 d D . . . . H1N2 H 0.579(3) 0.4492(17) 0.4597(9) 0.047(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 0.0320(3) 0.0343(3) 0.0292(3) -0.0030(2) 0.0004(2) 0.0039(2) O1 0.0287(7) 0.0561(9) 0.0343(8) -0.0016(7) -0.0005(6) 0.0030(7) O2 0.0564(10) 0.0333(8) 0.0400(9) -0.0031(7) -0.0003(7) 0.0093(7) N1 0.0683(15) 0.0464(12) 0.0411(11) 0.0067(11) -0.0175(11) -0.0030(11) N2 0.0310(9) 0.0381(9) 0.0344(9) -0.0109(8) 0.0042(8) -0.0054(8) N3 0.0303(9) 0.0421(9) 0.0318(9) -0.0035(8) 0.0029(7) -0.0027(7) N4 0.0370(10) 0.0371(9) 0.0364(9) -0.0008(8) -0.0031(8) -0.0057(8) C1 0.0324(10) 0.0336(9) 0.0293(10) -0.0031(9) -0.0010(9) 0.0022(8) C2 0.0406(12) 0.0312(10) 0.0362(11) -0.0063(9) -0.0073(9) 0.0013(9) C3 0.0479(13) 0.0298(10) 0.0430(12) 0.0019(10) -0.0066(11) -0.0010(9) C4 0.0393(12) 0.0397(11) 0.0365(11) 0.0005(10) -0.0062(9) 0.0054(9) C5 0.0579(15) 0.0421(12) 0.0389(12) -0.0030(10) -0.0160(12) -0.0098(11) C6 0.0542(14) 0.0374(11) 0.0407(12) 0.0013(11) -0.0078(11) -0.0113(10) C7 0.0320(11) 0.0327(10) 0.0288(10) 0.0028(9) -0.0006(9) -0.0013(9) C8 0.0343(11) 0.0541(13) 0.0371(11) 0.0025(11) 0.0044(10) -0.0009(10) C9 0.0322(12) 0.0560(13) 0.0402(12) 0.0078(12) -0.0015(10) -0.0080(10) C10 0.0386(11) 0.0388(11) 0.0406(12) 0.0092(10) -0.0095(10) -0.0086(9) C11 0.0540(15) 0.0540(14) 0.0663(18) -0.0048(14) -0.0143(14) -0.0164(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 1.4288(15) . ? S1 O1 1.4359(15) . ? S1 N2 1.6348(18) . ? S1 C1 1.737(2) . ? N1 C4 1.366(3) . ? N1 H1N1 0.871(17) . ? N1 H2N1 0.883(16) . ? N2 C7 1.385(3) . ? N2 H1N2 0.858(16) . ? N3 C8 1.335(3) . ? N3 C7 1.340(3) . ? N4 C7 1.328(3) . ? N4 C10 1.351(3) . ? C1 C6 1.384(3) . ? C1 C2 1.386(3) . ? C2 C3 1.375(3) . ? C2 H2 0.9300 . ? C3 C4 1.402(3) . ? C3 H3 0.9300 . ? C4 C5 1.398(3) . ? C5 C6 1.376(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.363(3) . ? C8 H8 0.9300 . ? C9 C10 1.382(3) . ? C9 H9 0.9300 . ? C10 C11 1.493(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 118.72(9) . . ? O2 S1 N2 109.81(9) . . ? O1 S1 N2 102.42(9) . . ? O2 S1 C1 108.72(9) . . ? O1 S1 C1 108.50(9) . . ? N2 S1 C1 108.14(10) . . ? C4 N1 H1N1 123(2) . . ? C4 N1 H2N1 114.6(17) . . ? H1N1 N1 H2N1 115(3) . . ? C7 N2 S1 128.43(15) . . ? C7 N2 H1N2 115.7(17) . . ? S1 N2 H1N2 115.6(17) . . ? C8 N3 C7 115.12(19) . . ? C7 N4 C10 115.89(19) . . ? C6 C1 C2 119.61(19) . . ? C6 C1 S1 120.25(16) . . ? C2 C1 S1 120.09(16) . . ? C3 C2 C1 120.24(19) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.82(19) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? N1 C4 C5 119.8(2) . . ? N1 C4 C3 122.0(2) . . ? C5 C4 C3 118.1(2) . . ? C6 C5 C4 120.7(2) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 120.5(2) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? N4 C7 N3 127.25(19) . . ? N4 C7 N2 119.58(18) . . ? N3 C7 N2 113.16(18) . . ? N3 C8 C9 122.9(2) . . ? N3 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C8 C9 C10 117.8(2) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? N4 C10 C9 121.1(2) . . ? N4 C10 C11 117.3(2) . . ? C9 C10 C11 121.6(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 -173.92(18) . . . . ? C1 S1 N2 C7 71.6(2) . . . . ? O2 S1 C1 C6 17.2(2) . . . . ? O1 S1 C1 C6 147.60(18) . . . . ? N2 S1 C1 C6 -102.02(19) . . . . ? O2 S1 C1 C2 -160.51(17) . . . . ? O1 S1 C1 C2 -30.1(2) . . . . ? N2 S1 C1 C2 80.30(19) . . . . ? C6 C1 C2 C3 -1.4(3) . . . . ? S1 C1 C2 C3 176.28(16) . . . . ? C1 C2 C3 C4 1.1(3) . . . . ? C2 C3 C4 N1 -177.4(2) . . . . ? C2 C3 C4 C5 0.1(3) . . . . ? N1 C4 C5 C6 176.4(2) . . . . ? C3 C4 C5 C6 -1.1(4) . . . . ? C4 C5 C6 C1 0.8(4) . . . . ? C2 C1 C6 C5 0.4(4) . . . . ? S1 C1 C6 C5 -177.27(19) . . . . ? C10 N4 C7 N3 0.1(3) . . . . ? C10 N4 C7 N2 179.29(19) . . . . ? C8 N3 C7 N4 -0.4(3) . . . . ? C8 N3 C7 N2 -179.70(18) . . . . ? S1 N2 C7 N4 3.8(3) . . . . ? S1 N2 C7 N3 -176.84(15) . . . . ? C7 N3 C8 C9 0.5(3) . . . . ? N3 C8 C9 C10 -0.2(3) . . . . ? C7 N4 C10 C9 0.3(3) . . . . ? C7 N4 C10 C11 -178.07(19) . . . . ? C8 C9 C10 N4 -0.2(3) . . . . ? C8 C9 C10 C11 178.1(2) . . . . ? _refine_diff_density_max 0.256 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.053 _shelx_res_file ; smz_f2_260.res created by SHELXL-2014/7 TITL smz_f2_260_a.res in Pbca REM Old TITL smz_f2_260 in Pbca REM SHELXT solution in Pbca REM R1 0.131, Rweak 0.562, Alpha 0.028, Orientation as input REM Formula found by SHELXT: C12 N3 O2 S CELL 0.71073 9.1228 11.6522 22.8488 90.000 90.000 90.000 ZERR 8.000 0.0004 0.0006 0.0010 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 SIZE 0.50 0.40 0.20 ACTA CONF HTAB LIST 4 WGHT 0.044900 0.693900 FVAR 0.57785 S1 5 0.667279 0.346632 0.389767 11.00000 0.03196 0.03434 = 0.02925 -0.00300 0.00044 0.00392 O1 4 0.801994 0.397209 0.409535 11.00000 0.02868 0.05614 = 0.03430 -0.00155 -0.00053 0.00296 O2 4 0.657456 0.224455 0.386218 11.00000 0.05639 0.03328 = 0.03998 -0.00312 -0.00035 0.00926 N1 3 0.543736 0.532862 0.155196 11.00000 0.06826 0.04639 = 0.04113 0.00667 -0.01749 -0.00302 N2 3 0.548779 0.394874 0.437468 11.00000 0.03102 0.03806 = 0.03441 -0.01088 0.00417 -0.00542 N3 3 0.333987 0.426351 0.485407 11.00000 0.03033 0.04214 = 0.03184 -0.00352 0.00291 -0.00270 N4 3 0.344504 0.286006 0.409206 11.00000 0.03704 0.03707 = 0.03640 -0.00085 -0.00308 -0.00568 C1 1 0.623828 0.404378 0.321869 11.00000 0.03238 0.03364 = 0.02934 -0.00313 -0.00098 0.00225 C2 1 0.666469 0.515273 0.307989 11.00000 0.04063 0.03118 = 0.03625 -0.00630 -0.00726 0.00134 AFIX 43 H2 2 0.713408 0.560295 0.335887 11.00000 -1.30000 AFIX 0 C3 1 0.639604 0.558957 0.253104 11.00000 0.04793 0.02977 = 0.04297 0.00188 -0.00658 -0.00105 AFIX 43 H3 2 0.670193 0.632967 0.243994 11.00000 -1.30000 AFIX 0 C4 1 0.566702 0.493319 0.210734 11.00000 0.03928 0.03974 = 0.03647 0.00049 -0.00619 0.00538 C5 1 0.521949 0.382446 0.225897 11.00000 0.05788 0.04207 = 0.03890 -0.00304 -0.01604 -0.00984 AFIX 43 H5 2 0.471899 0.337810 0.198709 11.00000 -1.30000 AFIX 0 C6 1 0.551143 0.338680 0.280585 11.00000 0.05424 0.03742 = 0.04066 0.00132 -0.00783 -0.01134 AFIX 43 H6 2 0.521839 0.264440 0.289879 11.00000 -1.30000 AFIX 0 C7 1 0.402090 0.366491 0.443354 11.00000 0.03203 0.03270 = 0.02875 0.00279 -0.00064 -0.00125 C8 1 0.192375 0.401249 0.492737 11.00000 0.03429 0.05409 = 0.03709 0.00253 0.00440 -0.00090 AFIX 43 H8 2 0.139805 0.440793 0.521188 11.00000 -1.30000 AFIX 0 C9 1 0.121506 0.320234 0.460357 11.00000 0.03219 0.05602 = 0.04023 0.00785 -0.00150 -0.00798 AFIX 43 H9 2 0.022788 0.304293 0.466444 11.00000 -1.30000 AFIX 0 C10 1 0.201229 0.262531 0.418162 11.00000 0.03861 0.03880 = 0.04055 0.00917 -0.00950 -0.00862 C11 1 0.134284 0.169795 0.381828 11.00000 0.05396 0.05397 = 0.06632 -0.00479 -0.01428 -0.01636 AFIX 137 H11A 2 0.146981 0.187560 0.341115 11.00000 -1.30000 H11B 2 0.031589 0.164166 0.390536 11.00000 -1.30000 H11C 2 0.181242 0.098040 0.390473 11.00000 -1.30000 AFIX 0 H1N1 2 0.550061 0.605110 0.145676 11.00000 0.08239 H2N1 2 0.480029 0.492573 0.134608 11.00000 0.05695 H1N2 2 0.579424 0.449157 0.459687 11.00000 0.04674 HKLF 4 REM smz_f2_260_a.res in Pbca REM R1 = 0.0449 for 2123 Fo > 4sig(Fo) and 0.0661 for all 2852 data REM 176 parameters refined using 3 restraints END WGHT 0.0454 0.6782 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 0.256, deepest hole -0.447, 1-sigma level 0.053 Q1 1 0.6317 0.3774 0.3505 11.00000 0.05 0.26 Q2 1 0.5918 0.5185 0.2354 11.00000 0.05 0.18 Q3 1 0.5570 0.4368 0.2152 11.00000 0.05 0.18 Q4 1 0.6337 0.5401 0.2812 11.00000 0.05 0.17 Q5 1 0.3654 0.3343 0.4170 11.00000 0.05 0.17 Q6 1 0.3019 0.3586 0.3588 11.00000 0.05 0.17 Q7 1 0.4388 0.2831 0.3163 11.00000 0.05 0.16 Q8 1 0.8694 0.3995 0.4087 11.00000 0.05 0.16 Q9 1 0.0163 0.2047 0.3694 11.00000 0.05 0.16 Q10 1 0.6098 0.4601 0.3258 11.00000 0.05 0.16 Q11 1 0.1486 0.0785 0.4272 11.00000 0.05 0.16 Q12 1 0.2732 0.1827 0.4930 11.00000 0.05 0.15 Q13 1 0.3835 0.1359 0.4977 11.00000 0.05 0.15 Q14 1 0.6842 0.5183 0.2734 11.00000 0.05 0.15 Q15 1 0.3848 0.5215 0.1513 11.00000 0.05 0.15 Q16 1 0.5859 0.3808 0.4113 11.00000 0.05 0.15 Q17 1 0.1832 0.2643 0.4532 11.00000 0.05 0.15 Q18 1 0.3519 0.4926 0.1578 11.00000 0.05 0.15 Q19 1 0.3685 0.2983 0.3784 11.00000 0.05 0.15 Q20 1 0.6040 0.6544 0.2499 11.00000 0.05 0.15 Q21 1 0.0771 0.0971 0.4096 11.00000 0.05 0.15 Q22 1 0.2900 0.3038 0.4010 11.00000 0.05 0.15 Q23 1 0.6582 0.1608 0.3277 11.00000 0.05 0.14 Q24 1 0.7458 0.1411 0.3666 11.00000 0.05 0.14 Q25 1 0.2926 0.2664 0.4289 11.00000 0.05 0.14 Q26 1 0.3628 0.2669 0.3664 11.00000 0.05 0.14 Q27 1 0.7730 0.5482 0.3280 11.00000 0.05 0.14 Q28 1 0.2468 0.1967 0.3275 11.00000 0.05 0.14 Q29 1 0.6924 0.7132 0.2304 11.00000 0.05 0.14 Q30 1 0.8156 0.5801 0.3075 11.00000 0.05 0.14 Q31 1 0.7751 0.4565 0.4002 11.00000 0.05 0.14 Q32 1 0.0938 0.2173 0.3468 11.00000 0.05 0.14 ; _shelx_res_checksum 5116 _shelx_hkl_file ; 0 0 -5 4.17 3.05 0 0 -6 7642.28 45.44 0 0 -7 70.07 6.50 0 0 -8 1096.63 20.01 0 0 -9 34.47 5.71 0 0 -10 5491.89 49.79 0 0 -11 95.48 9.75 0 0 -12 3.92 1.79 0 0 -13 3.90 3.30 0 0 -14 850.52 23.46 0 0 14 871.64 21.61 0 0 15 41.16 5.46 0 0 -15 25.46 4.97 0 0 -16 10.29 2.42 0 0 16 21.30 4.05 0 0 17 9.77 3.58 0 0 -17 9.25 4.47 0 0 18 1367.01 31.08 0 0 -18 1406.92 35.01 0 0 19 55.25 7.26 0 0 -19 61.15 8.34 0 0 -20 138.10 11.89 0 0 20 148.63 10.98 0 0 21 7.31 3.48 0 0 -21 3.04 3.46 0 0 22 183.73 12.58 0 0 -22 179.75 14.24 0 0 23 5.49 2.42 0 0 -23 8.59 4.37 0 0 -24 72.47 9.76 0 0 24 80.95 8.74 0 0 -25 -4.33 3.77 0 0 -26 30.19 6.44 0 0 -27 -3.92 3.81 0 0 -28 40.47 8.06 0 1 4 0.71 0.71 0 -1 -4 0.74 0.63 0 -1 -4 0.24 0.96 0 1 4 1.05 1.13 0 -1 -5 2.38 1.10 0 1 5 0.17 0.91 0 -1 -5 5.39 2.18 0 1 5 -2.70 1.89 0 -1 -6 -0.17 1.94 0 1 6 -0.08 1.09 0 1 7 0.54 0.96 0 1 -7 -0.12 1.25 0 -1 -7 0.64 1.66 0 -1 -8 -3.29 2.46 0 1 8 -1.10 1.30 0 1 -8 -0.60 1.52 0 1 9 0.84 0.97 0 -1 -9 -2.07 2.19 0 1 -9 -1.58 1.89 0 1 -10 -1.05 1.59 0 -1 -10 -0.12 2.22 0 1 10 -0.63 1.14 0 1 -11 -0.79 1.86 0 1 11 -0.78 1.43 0 -1 -11 -1.34 2.41 0 1 -12 -1.23 1.96 0 -1 -12 -2.03 3.07 0 1 12 -1.13 1.59 0 1 13 0.69 1.34 0 1 -13 1.12 1.78 0 1 -14 1.18 2.03 0 1 14 -2.13 1.70 0 -1 -14 -5.37 4.04 0 -1 -15 -4.41 4.06 0 1 15 -0.55 1.51 0 1 -15 -3.95 2.93 0 -1 -16 -2.48 3.75 0 1 -16 0.99 2.60 0 1 16 0.03 1.60 0 1 17 -2.61 2.55 0 -1 -17 -4.36 3.23 0 1 -17 1.69 2.69 0 1 18 -3.12 2.91 0 -1 -18 -2.58 3.61 0 1 -18 0.14 2.72 0 1 -19 -6.45 3.47 0 -1 -19 -5.17 4.28 0 1 19 -0.34 1.67 0 -1 -20 -6.98 4.51 0 1 20 0.03 2.02 0 -1 20 0.42 2.37 0 1 -20 -3.83 3.47 0 -1 -21 -2.27 3.67 0 1 21 -2.86 2.37 0 1 -21 -5.81 3.83 0 -1 21 6.84 3.22 0 -1 -22 3.71 2.97 0 1 22 -4.71 3.07 0 1 -22 1.97 2.38 0 -1 22 -0.79 1.90 0 -1 23 0.68 1.88 0 1 -23 -1.08 2.26 0 -1 -23 -1.89 3.46 0 1 23 -1.07 2.29 0 -1 -24 -3.10 3.72 0 -1 24 1.72 2.89 0 1 -24 -0.57 2.44 0 -1 25 -0.08 2.52 0 -1 -25 -3.75 4.67 0 1 -25 0.48 2.58 0 1 -26 0.23 2.59 0 -1 -26 0.88 2.74 0 -1 -27 1.44 3.87 0 -1 -28 -3.04 3.81 0 -1 -29 2.20 3.14 0 -2 -1 7932.43 42.18 0 2 1 7757.96 39.11 0 2 1 7479.69 40.58 0 2 2 4493.50 32.56 0 2 2 4351.73 32.11 0 -2 -2 4466.43 32.95 0 -2 -2 4502.27 32.58 0 -2 -3 9999.00 51.60 0 -2 -3 9960.71 52.52 0 2 4 8057.96 51.27 0 -2 -4 8022.27 39.95 0 -2 -5 8314.55 41.59 0 -2 -5 8520.01 55.74 0 2 5 8400.50 55.87 0 2 6 8026.91 57.91 0 2 6 8170.05 42.75 0 -2 -6 8211.23 58.29 0 -2 -6 8028.44 42.88 0 2 7 72.50 4.32 0 2 7 72.65 5.84 0 2 8 573.28 12.54 0 -2 -8 571.92 12.62 0 -2 -8 608.97 17.88 0 -2 -9 1920.92 32.68 0 2 -9 1828.54 22.60 0 2 9 1843.98 23.45 0 -2 -9 1825.21 23.56 0 2 10 943.21 17.69 0 2 -10 948.34 17.68 0 -2 -11 1389.79 30.37 0 2 -11 1346.06 22.44 0 2 11 1369.99 22.28 0 2 -12 618.94 16.22 0 2 12 589.18 15.31 0 -2 -12 651.84 21.58 0 2 13 150.87 8.28 0 2 -13 155.70 8.76 0 -2 -14 690.76 23.80 0 2 14 692.17 17.83 0 2 -14 702.48 19.02 0 -2 -15 29.53 5.90 0 2 -15 33.97 5.29 0 2 15 22.95 4.16 0 2 -16 72.48 6.70 0 2 16 82.95 6.82 0 -2 -16 89.32 9.26 0 2 -17 507.28 18.33 0 2 17 509.23 17.01 0 -2 -17 511.49 22.59 0 2 -18 235.49 13.28 0 2 18 247.56 12.58 0 -2 -18 273.40 17.27 0 -2 -19 721.87 28.30 0 2 19 677.97 20.79 0 2 -19 655.43 22.71 0 2 -20 82.10 8.77 0 -2 -20 97.42 11.21 0 2 20 85.06 8.21 0 2 -21 79.02 8.72 0 2 21 79.21 7.61 0 -2 -21 82.33 10.30 0 -2 -22 11.71 5.62 0 2 22 9.50 3.40 0 2 -22 14.59 4.51 0 2 23 424.50 18.24 0 2 -23 431.73 20.74 0 -2 23 430.63 21.57 0 -2 -23 424.90 24.04 0 -2 -24 27.75 7.59 0 2 -24 29.15 6.29 0 -2 24 24.45 5.99 0 2 -25 20.98 5.18 0 -2 25 11.15 3.95 0 -2 -25 15.58 5.33 0 -2 26 80.86 9.90 0 -2 -26 93.93 12.25 0 -2 -27 3.36 3.60 0 -2 -28 11.49 5.62 0 -2 -29 69.90 11.43 0 -2 -30 6.44 4.57 0 3 0 -1.48 1.37 0 -3 0 5.34 2.29 0 -3 0 2.71 1.69 0 3 0 0.21 1.62 0 -3 -1 -0.49 1.52 0 3 -1 0.92 1.50 0 3 1 -0.52 1.21 0 3 1 -0.61 1.66 0 3 -1 1.64 0.94 0 3 2 -1.06 1.31 0 3 2 1.57 1.46 0 3 -2 3.67 1.42 0 -3 -2 0.99 1.10 0 -3 -2 -1.32 1.90 0 3 -2 0.63 1.41 0 -3 -3 -0.11 1.54 0 -3 -3 -0.59 1.80 0 3 3 -0.21 1.67 0 3 3 -1.63 1.62 0 -3 -4 -2.76 2.56 0 -3 -4 -0.17 1.09 0 3 4 -0.17 1.12 0 -3 -5 -2.21 2.44 0 -3 -5 0.62 1.34 0 -3 -5 -0.81 1.14 0 3 5 -1.66 1.74 0 3 6 2.23 1.40 0 -3 -6 3.42 1.34 0 -3 -6 -0.11 1.99 0 -3 -7 -3.19 3.08 0 3 7 -2.20 2.20 0 -3 -7 0.78 0.99 0 -3 -8 1.32 1.20 0 3 8 -2.38 2.43 0 -3 -8 -5.57 3.53 0 -3 -9 -4.12 3.64 0 -3 -9 -1.71 1.43 0 -3 -10 -0.43 2.97 0 -3 -10 -0.20 1.10 0 3 10 -0.70 1.51 0 3 11 3.36 1.55 0 -3 -11 1.65 1.49 0 3 -11 0.27 1.14 0 3 -12 -0.14 1.05 0 3 12 -1.67 1.26 0 -3 -12 1.22 1.23 0 3 13 -1.12 1.51 0 -3 -13 -1.01 3.67 0 3 -13 -0.23 1.18 0 3 14 -0.57 1.27 0 3 -14 -0.15 1.38 0 -3 -14 -1.38 3.32 0 3 15 -1.96 1.68 0 -3 -15 1.65 2.70 0 3 -15 0.30 1.41 0 -3 -16 -2.38 3.30 0 3 16 -1.37 1.74 0 3 -16 -4.26 2.42 0 3 -17 -0.26 1.78 0 3 17 0.59 1.37 0 -3 -17 -3.14 3.56 0 3 -18 -2.70 2.78 0 -3 -18 -3.73 4.11 0 3 18 -0.52 1.74 0 -3 -19 -4.80 3.98 0 3 19 -2.21 1.95 0 3 -19 1.31 1.87 0 3 20 4.06 2.45 0 3 -20 -3.73 2.60 0 3 21 3.79 1.95 0 3 -21 -2.50 2.32 0 -3 -21 0.11 3.91 0 3 22 1.71 1.78 0 -3 -22 -0.31 3.45 0 3 -22 3.39 2.85 0 -3 -23 4.30 4.23 0 3 -23 0.78 1.74 0 -3 -24 4.58 4.80 0 -3 -25 11.54 6.07 0 -3 26 -0.52 2.85 0 -3 -26 -2.17 4.05 0 -3 -27 1.47 3.43 0 -3 -28 7.30 5.48 0 -3 -29 6.24 4.84 0 -3 -30 6.02 5.14 0 4 0 4262.39 36.23 0 4 0 4275.63 43.28 0 -4 0 4298.86 43.71 0 4 1 1593.55 23.53 0 -4 -1 1597.84 23.53 0 -4 -1 1587.58 26.58 0 4 -1 1588.97 20.60 0 4 1 1566.88 26.51 0 4 -1 1563.44 26.57 0 4 -2 1819.14 20.59 0 4 -2 1863.17 29.43 0 4 2 1823.63 28.80 0 4 2 1850.05 26.85 0 -4 -2 1909.67 29.18 0 -4 -2 1845.13 26.67 0 -4 -3 117.45 7.36 0 4 3 115.33 7.10 0 -4 -3 114.90 7.43 0 4 3 114.10 7.11 0 4 -3 103.22 7.29 0 4 -3 112.77 4.69 0 4 -4 234.61 6.20 0 -4 -4 244.06 11.00 0 4 4 228.66 10.44 0 -4 -4 241.30 10.82 0 4 4 237.76 10.69 0 -4 -5 290.26 12.16 0 4 5 280.66 12.11 0 -4 -5 271.70 12.30 0 -4 -6 850.34 22.12 0 4 6 852.03 21.96 0 -4 -6 828.23 17.94 0 -4 -6 854.28 21.66 0 4 7 348.25 14.66 0 -4 -7 362.71 11.82 0 -4 -7 360.68 14.34 0 -4 -7 354.10 15.05 0 -4 -8 267.98 10.25 0 -4 -8 278.30 13.65 0 -4 -9 6.94 4.10 0 -4 -9 12.05 2.37 0 -4 -10 5.16 4.15 0 -4 -10 4.06 1.64 0 -4 -11 107.06 6.71 0 -4 -11 101.39 9.14 0 4 -11 102.49 4.93 0 -4 -12 0.05 1.39 0 4 -12 4.54 1.20 0 -4 -12 3.71 3.26 0 4 -13 2.74 1.27 0 -4 -13 4.83 1.92 0 -4 -13 3.15 2.90 0 -4 -14 188.09 9.76 0 4 -14 193.55 8.24 0 -4 -14 209.80 14.31 0 -4 -15 89.94 10.17 0 4 -15 96.85 6.37 0 4 -16 149.64 8.28 0 -4 -16 171.85 14.26 0 4 -17 587.61 17.17 0 -4 -17 589.90 26.77 0 4 -18 1379.90 27.34 0 -4 -18 1490.46 42.92 0 -4 -19 403.86 23.40 0 4 -19 394.22 15.46 0 4 -20 4.22 2.89 0 -4 -20 10.42 5.38 0 4 -21 43.93 5.45 0 -4 -21 38.79 7.90 0 -4 -22 0.86 3.41 0 -4 -23 108.45 13.53 0 -4 -24 270.49 21.07 0 -4 -25 130.58 15.30 0 -4 -26 15.35 6.41 0 -4 -27 6.27 4.83 0 -4 -28 41.47 9.71 0 -4 -29 39.22 9.44 0 -5 0 0.91 1.90 0 5 0 0.23 1.84 0 5 0 -0.10 1.36 0 5 1 -0.69 1.20 0 5 -1 2.49 1.95 0 -5 -1 1.61 1.85 0 5 -1 -0.20 1.06 0 5 1 0.71 2.58 0 -5 -1 3.10 2.60 0 5 -2 -1.71 1.93 0 -5 -2 0.03 1.37 0 5 -2 -0.28 0.94 0 -5 -2 0.91 2.38 0 5 2 -0.66 1.89 0 5 2 0.81 1.20 0 -5 -3 0.37 1.03 0 5 3 0.02 1.66 0 5 -3 0.13 2.35 0 5 3 0.59 1.33 0 5 -3 -0.09 1.09 0 -5 -4 1.92 2.21 0 5 4 -2.35 2.53 0 5 4 -0.44 1.39 0 5 -4 -1.84 2.27 0 5 -4 0.52 0.80 0 -5 -4 -0.66 1.93 0 5 -5 0.14 0.84 0 5 5 1.68 1.43 0 -5 -5 -2.24 2.61 0 -5 -5 -0.83 1.37 0 -5 -6 0.51 1.57 0 -5 -6 -1.12 2.06 0 5 -6 1.79 1.07 0 -5 -7 1.98 1.24 0 -5 -7 -4.82 3.51 0 -5 -8 0.03 1.01 0 -5 -8 -2.65 3.17 0 -5 -9 4.58 2.22 0 -5 -9 1.36 2.88 0 -5 -10 2.58 3.09 0 -5 -10 1.59 1.25 0 -5 -11 -0.67 3.21 0 5 -11 -0.37 0.65 0 -5 -11 0.68 1.34 0 -5 -12 -1.44 3.29 0 -5 -12 0.17 1.23 0 5 -12 -0.14 0.76 0 5 -13 0.16 0.85 0 -5 -13 1.26 1.26 0 -5 -13 1.98 3.94 0 5 -14 -1.15 1.13 0 -5 -14 0.63 3.23 0 -5 -14 0.16 1.34 0 -5 -15 0.70 1.70 0 -5 -15 1.27 2.66 0 5 -15 -1.49 1.36 0 5 -16 1.00 1.10 0 -5 -16 2.66 2.39 0 -5 -17 3.47 3.73 0 5 -17 0.30 1.24 0 5 -18 0.12 1.59 0 -5 -18 -3.03 3.87 0 5 -19 0.98 1.26 0 -5 -19 0.05 2.96 0 -5 -20 8.00 4.67 0 -5 -21 1.12 3.90 0 -5 -22 -2.17 4.38 0 -5 -23 -0.18 3.16 0 -5 -24 9.59 5.14 0 -5 -25 7.77 5.46 0 -5 -26 5.58 5.25 0 -5 -27 10.46 6.39 0 6 0 24.58 4.90 0 6 0 24.43 3.80 0 6 -1 4105.62 52.95 0 6 -1 4069.73 41.55 0 6 1 4071.38 45.20 0 6 1 4020.30 52.35 0 6 -2 1271.19 22.05 0 6 2 1301.25 27.00 0 6 2 1330.05 30.03 0 6 -2 1315.83 30.16 0 -6 -2 1315.92 27.04 0 6 3 235.72 11.84 0 -6 -3 235.32 12.24 0 6 3 239.15 12.94 0 6 -3 239.95 9.06 0 6 -3 235.70 13.10 0 6 4 636.39 20.08 0 6 -4 592.11 13.35 0 6 4 618.64 20.92 0 -6 -4 602.87 19.80 0 6 -4 597.85 21.21 0 -6 -5 33.81 5.35 0 6 5 24.41 3.88 0 6 -5 26.38 2.60 0 6 -5 31.36 4.99 0 6 -6 7.36 1.47 0 -6 -6 6.14 3.08 0 6 -7 301.51 7.50 0 -6 -7 301.48 15.56 0 6 -8 44.63 2.63 0 -6 -8 57.08 5.85 0 -6 -8 50.56 6.88 0 6 -9 46.00 2.41 0 -6 -9 56.63 5.85 0 -6 -9 57.65 7.48 0 -6 -10 72.80 8.62 0 -6 -10 68.26 6.41 0 -6 -11 28.46 8.36 0 -6 -11 2.46 1.82 0 -6 -12 3086.78 56.85 0 -6 -12 3006.40 42.41 0 -6 -13 41.48 9.73 0 -6 -13 3.91 2.33 0 -6 -14 280.14 13.14 0 6 -14 250.11 6.06 0 -6 -14 297.46 18.88 0 -6 -15 606.73 27.62 0 -6 -15 573.88 19.01 0 6 -16 66.77 3.76 0 -6 -16 79.93 11.11 0 -6 -17 108.93 12.88 0 -6 -18 469.75 25.90 0 -6 -19 285.76 21.22 0 -6 -20 98.21 13.46 0 -6 -21 384.55 25.32 0 -6 -22 224.63 19.86 0 -6 -23 19.49 7.67 0 -6 -24 53.52 11.04 0 -6 -25 110.31 15.59 0 -6 -26 152.90 17.95 0 7 0 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8 -3 0 44.79 7.10 8 -3 -1 34.94 6.13 8 -3 1 50.19 7.55 8 -3 -2 17.35 4.56 8 -3 2 12.88 3.78 8 -3 -3 156.27 12.08 8 -3 3 140.86 12.98 8 3 4 109.47 12.22 8 -3 -4 95.04 9.32 8 -3 4 108.84 11.73 8 3 5 21.07 6.26 8 -3 -5 25.01 4.84 8 -3 5 27.74 6.40 8 3 -5 29.00 4.85 8 3 -6 345.27 16.08 8 3 6 354.53 22.58 8 -3 -6 341.56 16.34 8 -3 6 357.93 22.25 8 3 -7 137.36 10.20 8 -3 -7 139.91 10.15 8 3 7 129.08 14.07 8 -3 7 155.28 14.72 8 3 8 123.98 13.99 8 -3 8 126.31 13.55 8 3 -8 141.67 10.49 8 3 9 2.29 3.44 8 -3 9 2.21 4.56 8 3 -9 -0.16 1.90 8 3 10 11.86 4.52 8 -3 10 10.10 4.98 8 3 11 119.02 13.97 8 -3 11 127.30 14.37 8 3 12 -3.73 5.07 8 -3 12 1.75 2.66 8 3 13 10.61 4.95 8 -3 13 14.84 5.39 8 3 14 11.97 3.87 8 -3 14 17.81 6.30 8 3 15 47.06 9.60 8 -3 15 55.11 10.09 8 3 16 24.90 6.68 8 -3 16 29.92 7.58 8 3 17 116.31 14.95 8 -3 17 120.69 15.46 8 3 18 5.98 5.07 8 -3 18 12.47 6.48 8 3 19 129.43 16.13 8 -3 19 152.19 17.71 8 3 20 8.27 5.11 8 -4 0 19.18 3.38 8 -4 -1 39.65 6.63 8 -4 1 45.15 7.38 8 -4 -2 178.43 13.46 8 -4 2 191.70 15.03 8 -4 -3 2.04 3.08 8 -4 3 3.86 3.07 8 -4 -4 44.85 6.86 8 -4 4 32.44 7.04 8 4 -4 37.35 6.21 8 4 -5 227.76 14.32 8 -4 -5 232.96 13.94 8 -4 5 247.63 17.98 8 4 -6 59.38 7.41 8 -4 -6 60.62 6.94 8 -4 6 64.91 9.82 8 -4 -7 68.16 7.17 8 -4 7 58.79 9.62 8 4 -7 69.68 8.14 8 4 8 116.47 13.82 8 -4 8 120.86 13.24 8 4 -8 127.52 11.01 8 4 9 32.06 7.47 8 -4 9 35.89 7.80 8 4 -9 39.70 6.16 8 4 10 43.47 8.45 8 4 -10 37.41 5.93 8 -4 10 38.29 8.01 8 4 11 24.52 6.60 8 4 -11 30.83 5.76 8 -4 11 22.22 6.08 8 4 12 4.45 3.56 8 -4 12 3.26 3.52 8 4 13 -1.39 3.71 8 -4 13 -3.84 5.57 8 4 14 6.74 4.23 8 -4 14 4.54 3.75 8 4 15 13.02 5.69 8 -4 15 27.45 8.02 8 4 16 -11.04 6.74 8 -4 16 2.47 3.84 8 4 17 32.06 8.27 8 -4 17 18.52 6.74 8 4 18 55.54 11.10 8 -4 18 53.82 10.68 8 4 19 38.20 9.14 8 -5 0 1142.08 35.62 8 -5 -1 36.32 7.25 8 -5 1 36.79 7.63 8 -5 -2 9.97 3.71 8 -5 2 4.85 3.02 8 5 -3 99.66 10.29 8 -5 -3 102.71 9.98 8 -5 3 93.78 11.32 8 5 -4 87.67 9.60 8 -5 -4 92.77 9.36 8 -5 4 104.11 11.88 8 5 -5 82.48 9.50 8 -5 -5 74.84 8.08 8 -5 5 72.92 10.35 8 5 -6 119.04 11.36 8 -5 -6 140.10 10.58 8 -5 6 127.25 14.00 8 -5 7 88.45 12.02 8 5 -7 75.49 9.15 8 -5 8 66.17 10.32 8 5 -8 55.80 7.72 8 5 -9 26.83 5.24 8 -5 9 26.75 7.04 8 -5 10 80.33 11.58 8 5 -10 85.99 9.65 8 5 -11 30.82 6.33 8 -5 11 23.12 6.37 8 5 -12 3.06 3.34 8 -5 12 3.55 4.22 8 -5 13 13.82 6.09 8 5 14 51.81 10.09 8 -5 14 50.11 9.78 8 5 15 -7.95 6.66 8 -5 15 -1.40 5.19 8 5 16 -1.26 5.00 8 -5 16 -3.06 3.50 8 5 17 6.57 3.75 8 -5 17 14.56 6.38 8 5 18 75.32 12.82 8 -5 18 67.62 12.44 8 -6 0 1.04 2.82 8 -6 -1 3.52 3.85 8 -6 1 0.99 3.78 8 -6 -2 443.80 21.91 8 -6 2 463.10 24.46 8 6 -3 124.59 12.50 8 -6 -3 135.86 11.88 8 -6 3 143.51 14.52 8 -6 -4 8.80 2.70 8 -6 4 7.92 4.49 8 6 -4 9.98 4.25 8 -6 -5 4.21 3.19 8 -6 5 4.70 4.06 8 6 -5 -0.68 2.58 8 -6 6 1.70 3.75 8 6 -6 -0.01 2.61 8 -6 7 2.30 2.93 8 6 -7 6.52 3.33 8 -6 8 -0.48 2.58 8 6 -8 3.24 2.61 8 6 -9 1.74 1.96 8 -6 9 -1.15 3.19 8 6 -10 10.71 4.12 8 -6 10 11.53 5.28 8 6 -11 24.95 6.20 8 -6 11 24.98 7.81 8 6 -12 38.92 7.36 8 -6 12 39.08 8.81 8 6 -13 -2.08 3.27 8 -6 13 5.00 5.27 8 -6 14 34.39 8.98 8 -6 15 -1.76 3.39 8 -6 16 -6.51 4.86 8 -7 0 19.86 7.18 8 -7 -1 214.79 16.00 8 -7 1 230.73 17.34 8 -7 -2 7.68 4.14 8 -7 2 20.35 6.57 8 7 -2 20.50 6.45 8 7 -3 328.10 21.00 8 -7 -3 331.62 18.70 8 -7 3 353.28 22.30 8 -7 -4 35.64 6.22 8 -7 4 43.24 9.13 8 7 -4 36.26 7.31 8 -7 5 16.56 6.87 8 7 -5 1.26 3.02 8 -7 6 8.26 5.30 8 7 -6 -3.32 3.48 8 -7 7 93.10 12.42 8 7 -7 80.69 10.36 8 7 -8 64.41 9.51 8 -7 8 77.99 11.54 8 7 -9 10.83 3.88 8 -7 9 19.60 6.98 8 -7 10 73.13 11.86 8 7 -10 74.54 10.49 8 -7 11 215.64 20.02 8 7 -11 188.99 16.47 8 7 -12 3.47 2.66 8 -7 12 7.67 5.58 8 7 -13 32.68 7.37 8 -7 13 25.40 8.13 8 7 -14 13.24 4.97 8 -7 14 16.12 6.96 8 -7 15 14.03 6.51 8 -8 0 158.44 14.71 8 -8 -1 49.25 8.63 8 -8 1 51.57 9.00 8 -8 -2 5.12 3.30 8 -8 2 3.70 4.62 8 8 -2 1.37 2.35 8 -8 -3 12.83 3.72 8 -8 3 18.93 5.69 8 8 -3 16.11 5.33 8 -8 4 11.78 5.61 8 8 -4 5.22 3.51 8 -8 5 48.26 8.97 8 8 -5 48.74 8.78 8 -8 6 35.38 8.29 8 8 -6 43.47 8.18 8 -8 7 61.15 10.48 8 8 -7 48.32 8.76 8 8 -8 -0.25 2.44 8 -8 8 6.84 5.93 8 8 -9 0.10 2.29 8 -8 9 4.98 4.65 8 8 -10 8.86 5.07 8 -8 10 6.50 5.48 8 -8 11 65.97 12.20 8 8 -11 71.23 11.07 8 8 -12 15.44 5.35 8 -8 12 11.89 5.97 8 8 -13 -3.38 4.04 8 -8 13 4.55 5.99 8 8 -14 7.67 3.94 8 -9 0 96.97 11.65 8 -9 -1 51.31 8.48 8 -9 1 60.29 9.77 8 -9 2 26.17 6.87 8 9 -2 20.00 5.91 8 -9 3 59.74 10.14 8 9 -3 48.46 9.26 8 -9 4 10.56 5.37 8 9 -4 1.55 2.74 8 -9 5 24.85 6.89 8 9 -5 20.76 6.89 8 -9 6 40.15 9.45 8 9 -6 26.08 7.10 8 -9 7 246.18 21.23 8 9 -7 228.69 19.86 8 -9 8 93.48 13.87 8 9 -8 72.83 11.60 8 9 -9 -0.14 3.07 8 -9 9 11.49 6.50 8 9 -10 14.48 5.11 8 -9 10 18.08 6.71 8 9 -11 54.93 10.22 8 -9 11 57.92 11.52 8 9 -12 14.04 5.34 8 -9 12 33.28 8.91 8 9 -13 46.66 9.66 8 9 -14 25.61 7.28 8 9 -15 25.63 7.38 8 -10 0 13.39 6.07 8 -10 1 5.11 3.76 8 -10 2 1.26 3.25 8 10 -2 -8.30 5.69 8 -10 3 19.66 6.76 8 10 -3 14.07 5.77 8 -10 4 75.28 11.66 8 10 -4 71.69 11.69 8 10 -5 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9 111.20 15.39 9 -10 3 15.58 6.58 9 -10 4 15.22 5.94 9 10 -4 12.10 5.87 9 -10 5 1.91 3.95 9 10 -5 -2.67 3.69 9 -10 6 4.86 3.15 9 10 -6 8.64 5.49 9 -10 7 1.23 3.36 9 10 -7 0.51 3.00 9 -11 4 -2.82 2.80 10 0 0 144.80 14.79 10 0 -1 8.85 4.76 10 0 1 9.70 5.13 10 0 2 65.55 9.92 10 0 3 -0.50 3.34 10 0 4 37.04 7.98 10 0 5 -2.14 3.89 10 0 6 1.08 2.83 10 0 7 5.28 4.24 10 0 8 75.49 12.00 10 0 9 -4.15 4.65 10 0 10 15.09 6.52 10 0 11 -3.51 3.17 10 0 12 64.15 11.62 10 0 13 2.34 4.26 10 0 14 20.72 6.99 10 -1 0 5.19 3.57 10 1 1 4.05 3.45 10 -1 -1 8.34 4.29 10 -1 1 9.31 4.17 10 1 2 -1.71 3.72 10 -1 -2 -0.52 3.14 10 -1 2 3.86 3.49 10 -1 -3 17.62 5.33 10 1 3 18.99 6.17 10 -1 3 14.40 5.70 10 1 4 96.97 12.88 10 -1 4 97.45 12.75 10 1 5 27.82 7.45 10 -1 5 22.75 6.46 10 1 6 27.73 7.26 10 -1 6 29.14 7.82 10 -1 7 82.47 12.40 10 1 7 71.75 11.99 10 1 8 109.63 14.25 10 -1 8 115.95 14.88 10 1 9 19.44 5.41 10 -1 9 22.74 7.46 10 1 10 69.00 12.17 10 -1 10 49.39 9.91 10 1 11 101.45 14.28 10 -1 11 114.51 15.34 10 1 12 2.67 4.58 10 -1 12 8.89 5.78 10 1 13 10.43 5.72 10 -1 13 19.06 7.04 10 -1 14 30.14 8.01 10 -2 0 -3.71 4.51 10 -2 -1 2.94 2.69 10 -2 1 -3.46 3.50 10 -2 -2 3.81 3.07 10 -2 2 -0.03 2.92 10 2 3 0.17 3.59 10 -2 -3 -4.20 3.13 10 -2 3 3.82 4.00 10 2 4 41.31 8.92 10 -2 -4 55.28 8.24 10 -2 4 52.98 9.02 10 -2 -5 7.21 3.41 10 2 5 2.41 3.01 10 -2 5 10.55 5.14 10 2 6 5.27 4.43 10 -2 6 11.92 4.75 10 2 7 15.28 5.84 10 -2 7 15.70 6.24 10 2 8 36.59 8.82 10 -2 8 39.58 8.96 10 2 9 4.38 4.05 10 -2 9 -3.86 4.62 10 2 10 60.50 11.18 10 -2 10 57.29 10.91 10 2 11 29.33 8.26 10 -2 11 32.59 8.32 10 2 12 5.82 5.10 10 -2 12 2.75 3.35 10 2 13 3.41 3.33 10 -2 13 11.64 6.41 10 -3 0 1.61 3.02 10 -3 -1 6.08 2.47 10 -3 1 4.95 2.85 10 -3 -2 7.20 3.79 10 -3 2 8.69 5.05 10 -3 -3 133.00 13.00 10 -3 3 156.88 15.67 10 -3 -4 18.04 5.54 10 -3 4 6.96 5.25 10 -3 5 58.38 10.32 10 -3 6 40.32 9.13 10 3 7 282.95 23.12 10 -3 7 309.92 23.41 10 3 8 29.31 8.32 10 -3 8 29.30 8.69 10 3 9 5.29 3.97 10 -3 9 13.44 6.30 10 3 10 -3.59 4.21 10 -3 10 5.18 5.30 10 3 11 30.34 7.90 10 -3 11 36.55 8.83 10 3 12 6.15 4.45 10 -3 12 2.58 3.23 10 -3 13 43.11 9.79 10 -4 0 23.20 6.20 10 -4 -1 45.97 8.21 10 -4 1 48.98 8.92 10 -4 -2 -3.33 2.66 10 -4 2 1.72 3.74 10 -4 -3 -2.77 3.51 10 -4 3 0.78 2.73 10 -4 4 5.92 3.63 10 -4 5 3.80 3.41 10 -4 6 10.69 4.79 10 -4 7 77.16 12.28 10 -4 8 0.63 4.07 10 -4 9 5.13 4.54 10 -4 10 1.41 3.35 10 4 11 4.35 3.55 10 -4 11 0.60 4.08 10 -4 12 15.51 6.36 10 -5 0 85.90 11.56 10 -5 -1 70.34 9.99 10 -5 1 81.35 11.27 10 -5 2 24.39 6.89 10 -5 3 23.88 7.14 10 -5 4 103.95 13.31 10 -5 5 1.86 3.10 10 -5 6 -2.81 5.39 10 -5 7 -5.50 4.35 10 -5 8 27.71 7.82 10 -5 9 15.81 5.27 10 -5 10 137.24 16.74 10 -5 11 7.76 5.70 10 -6 0 98.70 12.08 10 -6 1 8.53 4.79 10 -6 2 9.04 4.37 10 -6 3 1.59 3.34 10 -6 4 42.78 8.55 10 -6 5 -1.42 4.84 10 -6 6 5.13 4.01 10 -6 7 1.08 3.14 10 -6 8 10.65 3.37 10 -6 9 16.58 6.83 10 -6 10 106.51 14.97 10 -7 1 115.00 13.60 10 -7 2 19.28 6.47 10 -7 3 51.93 9.57 10 -7 4 13.21 5.10 10 -7 5 -3.90 4.07 10 -7 6 7.40 4.10 10 -7 7 31.29 8.28 10 -7 8 -2.83 3.12 10 -7 9 -0.73 3.34 10 -8 2 7.61 4.17 10 -8 3 8.10 4.95 10 -8 4 1.19 3.26 10 -8 5 1.52 3.58 10 -8 6 11.78 5.40 10 -8 7 83.19 13.46 10 -9 4 57.62 10.94 10 -9 5 27.20 7.93 11 0 0 0.41 2.45 11 0 1 4.96 4.81 11 0 2 93.40 13.13 11 0 3 11.02 5.98 11 0 4 44.29 9.30 11 0 5 3.42 4.35 11 0 6 37.78 9.31 11 0 7 -0.02 3.51 11 0 8 14.14 6.32 11 0 9 2.52 3.94 11 -1 0 0.16 2.52 11 -1 -1 2.38 3.87 11 -1 1 -4.42 4.07 11 1 2 14.57 5.90 11 -1 -2 7.50 3.74 11 -1 2 11.71 4.93 11 1 3 0.93 3.82 11 -1 3 -0.22 3.47 11 1 4 9.57 5.15 11 -1 4 8.86 4.68 11 1 5 7.73 4.95 11 -1 5 7.73 4.33 11 1 6 21.48 6.28 11 -1 6 22.69 7.13 11 1 7 8.86 4.81 11 -1 7 7.52 4.24 11 1 8 3.51 3.72 11 -1 8 6.95 4.17 11 1 9 9.48 4.77 11 -1 9 6.95 5.65 11 -2 0 -0.25 2.54 11 -2 -1 31.55 7.11 11 -2 1 31.77 7.34 11 -2 -2 58.94 9.39 11 -2 2 57.48 10.14 11 -2 3 -1.38 3.45 11 -2 4 20.60 6.11 11 2 5 39.78 9.64 11 -2 5 21.24 7.05 11 2 6 3.50 3.89 11 -2 6 1.69 3.06 11 2 7 1.86 4.35 11 -2 7 -2.10 3.13 11 2 8 9.82 5.73 11 -2 8 14.09 5.99 11 -2 9 26.26 8.08 11 -3 0 -6.20 4.85 11 -3 -1 -0.67 3.20 11 -3 1 7.56 4.26 11 -3 2 -1.25 3.01 11 -3 3 -2.38 3.41 11 -3 4 4.08 3.26 11 -3 5 37.12 8.55 11 -3 6 2.81 3.40 11 -3 7 -1.88 3.85 11 -3 8 1.76 3.40 11 -3 9 0.21 3.54 11 -4 0 3.95 3.56 11 -4 1 72.78 11.05 11 -4 2 4.68 3.58 11 -4 3 1.54 3.21 11 -4 4 1.74 2.69 11 -4 5 -4.34 4.56 11 -4 6 -8.83 4.78 11 -4 7 -4.50 4.09 11 -4 8 4.66 3.92 11 -5 1 31.74 8.24 11 -5 2 88.26 12.55 11 -5 3 -0.77 3.07 11 -5 4 19.09 6.46 11 -5 5 8.86 5.22 11 -5 6 32.83 8.41 11 -5 7 1.37 3.32 11 -6 2 103.97 13.45 11 -6 3 5.05 3.97 11 -6 4 10.37 4.97 11 -6 5 13.62 6.25 11 -6 6 13.47 5.74 11 -7 4 16.32 5.84 11 -7 5 20.24 7.05 12 0 2 6.38 3.27 12 0 3 -2.60 3.70 12 0 4 31.55 8.27 12 -1 0 0.81 2.72 12 -1 1 5.88 3.96 12 -1 2 1.75 3.33 12 -1 3 -6.02 4.95 12 -1 4 4.18 4.34 12 -1 5 16.56 6.30 12 -2 1 2.29 3.46 12 -2 2 -3.47 3.58 12 -2 3 26.14 7.91 12 -2 4 43.83 9.82 12 -2 5 17.71 6.52 12 -3 2 6.74 4.46 12 -3 3 -4.16 4.39 12 -3 4 26.54 7.26 12 -4 3 45.46 9.65 12 -4 4 36.10 9.14 0 0 0 0.00 0.00 TITL smz_f2_260 in Pbca REM Pbca (#61 in standard setting) CELL 0.71073 9.122814 11.652160 22.848827 90.0000 90.0000 90.0000 ZERR 6.00 0.000443 0.000558 0.000980 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 86462