data_180k_smz-f2_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 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 9.0972(2) _cell_length_b 11.5751(2) _cell_length_c 22.8531(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2406.45(7) _cell_formula_units_Z 8 _cell_measurement_temperature 180 _cell_measurement_reflns_used 8097 _cell_measurement_theta_min 2.7640 _cell_measurement_theta_max 29.4760 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.459 _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 0.269 _shelx_estimated_absorpt_T_min 0.877 _shelx_estimated_absorpt_T_max 0.948 _exptl_absorpt_correction_T_min 0.95712 _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 180 _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_detector_area_resol_mean ? _diffrn_reflns_number 21374 _diffrn_reflns_av_unetI/netI 0.0430 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.727 _diffrn_reflns_theta_max 29.476 _diffrn_reflns_theta_full 24.415 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_point_group_measured_fraction_full 0.989 _reflns_number_total 3566 _reflns_number_gt 2723 _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 ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) ; _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^)+(0.0463P)^2^+1.4827P] 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 3566 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 0.33166(5) 0.34596(3) 0.38969(2) 0.02317(12) Uani 1 1 d . . . . . O2 O 0.19650(14) 0.39701(11) 0.40966(5) 0.0290(3) Uani 1 1 d . . . . . O1 O 0.34165(16) 0.22293(10) 0.38651(5) 0.0309(3) Uani 1 1 d . . . . . N4 N 0.66689(17) 0.42609(13) 0.48540(6) 0.0260(3) Uani 1 1 d . . . . . N3 N 0.65588(18) 0.28478(12) 0.40880(6) 0.0269(3) Uani 1 1 d . . . . . N2 N 0.45135(18) 0.39512(13) 0.43725(6) 0.0255(3) Uani 1 1 d . . . . . N1 N 0.4543(2) 0.53251(16) 0.15447(7) 0.0361(4) Uani 1 1 d . . . . . C1 C 0.3745(2) 0.40360(14) 0.32150(7) 0.0246(4) Uani 1 1 d . . . . . C2 C 0.4477(2) 0.33653(15) 0.28013(8) 0.0311(4) Uani 1 1 d . . . . . H2 H 0.4769 0.2618 0.2895 0.040 Uiso 1 1 calc R U . . . C3 C 0.4767(2) 0.38080(15) 0.22538(8) 0.0331(4) Uani 1 1 d . . . . . H3 H 0.5270 0.3359 0.1982 0.043 Uiso 1 1 calc R U . . . C4 C 0.4315(2) 0.49272(15) 0.20990(7) 0.0282(4) Uani 1 1 d . . . . . C5 C 0.3580(2) 0.55928(14) 0.25229(8) 0.0296(4) Uani 1 1 d . . . . . H5 H 0.3275 0.6337 0.2431 0.038 Uiso 1 1 calc R U . . . C6 C 0.3307(2) 0.51548(14) 0.30748(7) 0.0266(4) Uani 1 1 d . . . . . H6 H 0.2831 0.5607 0.3353 0.035 Uiso 1 1 calc R U . . . C7 C 0.5980(2) 0.36592(14) 0.44309(7) 0.0234(3) Uani 1 1 d . . . . . C8 C 0.8086(2) 0.40058(17) 0.49302(8) 0.0298(4) Uani 1 1 d . . . . . H8 H 0.8611 0.4400 0.5216 0.039 Uiso 1 1 calc R U . . . C9 C 0.8801(2) 0.31833(17) 0.46026(8) 0.0307(4) Uani 1 1 d . . . . . H9 H 0.9791 0.3022 0.4662 0.040 Uiso 1 1 calc R U . . . C10 C 0.7995(2) 0.26056(15) 0.41818(8) 0.0291(4) Uani 1 1 d . . . . . C11 C 0.8670(3) 0.16732(18) 0.38135(10) 0.0411(5) Uani 1 1 d . . . . . H11A H 0.8200 0.0949 0.3897 0.053 Uiso 1 1 calc R U . . . H11B H 0.9700 0.1616 0.3901 0.053 Uiso 1 1 calc R U . . . H11C H 0.8543 0.1858 0.3407 0.053 Uiso 1 1 calc R U . . . H1N2 H 0.416(3) 0.4442(19) 0.4586(10) 0.035(6) Uiso 1 1 d . . . . . H1N1 H 0.515(3) 0.493(2) 0.1338(11) 0.041(6) Uiso 1 1 d . . . . . H2N1 H 0.447(3) 0.603(2) 0.1468(11) 0.054(8) 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 0.0240(3) 0.0243(2) 0.02115(18) -0.00167(13) -0.00034(15) -0.00280(16) O2 0.0218(7) 0.0401(7) 0.0251(6) -0.0020(5) 0.0003(5) -0.0014(5) O1 0.0408(9) 0.0238(6) 0.0282(6) -0.0005(4) -0.0012(6) -0.0052(5) N4 0.0246(9) 0.0292(7) 0.0243(6) -0.0024(5) -0.0027(6) 0.0009(6) N3 0.0275(9) 0.0263(7) 0.0270(7) -0.0011(5) 0.0024(6) 0.0033(6) N2 0.0234(9) 0.0280(7) 0.0252(7) -0.0079(5) -0.0020(6) 0.0041(6) N1 0.0470(12) 0.0318(8) 0.0293(8) 0.0043(6) 0.0112(7) 0.0029(8) C1 0.0264(10) 0.0253(7) 0.0221(7) -0.0017(6) -0.0001(6) -0.0017(7) C2 0.0376(12) 0.0274(8) 0.0282(8) -0.0003(6) 0.0055(8) 0.0069(8) C3 0.0422(13) 0.0284(8) 0.0289(8) -0.0024(6) 0.0099(8) 0.0057(8) C4 0.0301(11) 0.0286(8) 0.0257(8) -0.0004(6) 0.0034(7) -0.0048(7) C5 0.0361(12) 0.0216(7) 0.0312(8) -0.0002(6) 0.0039(8) -0.0001(7) C6 0.0289(10) 0.0228(7) 0.0280(8) -0.0037(6) 0.0037(7) -0.0011(7) C7 0.0243(10) 0.0246(7) 0.0212(7) 0.0021(6) 0.0000(6) -0.0002(7) C8 0.0223(10) 0.0398(10) 0.0273(8) 0.0015(7) -0.0033(7) 0.0000(8) C9 0.0204(10) 0.0413(10) 0.0304(9) 0.0064(7) 0.0012(7) 0.0051(8) C10 0.0294(11) 0.0283(8) 0.0297(8) 0.0064(6) 0.0060(7) 0.0064(7) C11 0.0378(14) 0.0404(11) 0.0452(11) -0.0042(8) 0.0092(9) 0.0132(9) _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 1.4288(12) . ? S1 O2 1.4386(14) . ? S1 N2 1.6403(15) . ? S1 C1 1.7395(17) . ? N4 C8 1.334(2) . ? N4 C7 1.346(2) . ? N3 C7 1.332(2) . ? N3 C10 1.353(3) . ? N2 C7 1.383(2) . ? N2 H1N2 0.82(2) . ? N1 C4 1.364(2) . ? N1 H1N1 0.86(3) . ? N1 H2N1 0.84(3) . ? C1 C6 1.392(2) . ? C1 C2 1.392(2) . ? C2 C3 1.378(2) . ? C2 H2 0.9300 . ? C3 C4 1.405(2) . ? C3 H3 0.9300 . ? C4 C5 1.406(2) . ? C5 C6 1.382(2) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.375(3) . ? C8 H8 0.9300 . ? C9 C10 1.382(3) . ? C9 H9 0.9300 . ? C10 C11 1.500(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 O1 S1 O2 118.68(8) . . ? O1 S1 N2 109.71(8) . . ? O2 S1 N2 102.39(8) . . ? O1 S1 C1 108.81(8) . . ? O2 S1 C1 108.57(8) . . ? N2 S1 C1 108.17(8) . . ? C8 N4 C7 115.39(15) . . ? C7 N3 C10 115.75(16) . . ? C7 N2 S1 128.29(12) . . ? C7 N2 H1N2 119.7(17) . . ? S1 N2 H1N2 112.0(17) . . ? C4 N1 H1N1 115.3(16) . . ? C4 N1 H2N1 120.7(18) . . ? H1N1 N1 H2N1 117(2) . . ? C6 C1 C2 119.94(16) . . ? C6 C1 S1 119.91(13) . . ? C2 C1 S1 120.10(13) . . ? C3 C2 C1 120.06(16) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 121.04(16) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? N1 C4 C3 120.05(17) . . ? N1 C4 C5 121.81(17) . . ? C3 C4 C5 118.10(16) . . ? C6 C5 C4 120.87(16) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 119.98(16) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? N3 C7 N4 127.14(17) . . ? N3 C7 N2 119.79(15) . . ? N4 C7 N2 113.07(15) . . ? N4 C8 C9 122.66(18) . . ? N4 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? C8 C9 C10 117.58(18) . . ? C8 C9 H9 121.2 . . ? C10 C9 H9 121.2 . . ? N3 C10 C9 121.48(17) . . ? N3 C10 C11 117.11(18) . . ? C9 C10 C11 121.40(19) . . ? 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 O1 S1 N2 C7 46.46(17) . . . . ? O2 S1 N2 C7 173.38(15) . . . . ? C1 S1 N2 C7 -72.09(17) . . . . ? O1 S1 C1 C6 160.36(15) . . . . ? O2 S1 C1 C6 29.87(17) . . . . ? N2 S1 C1 C6 -80.52(17) . . . . ? O1 S1 C1 C2 -17.20(19) . . . . ? O2 S1 C1 C2 -147.68(16) . . . . ? N2 S1 C1 C2 101.92(17) . . . . ? C6 C1 C2 C3 0.0(3) . . . . ? S1 C1 C2 C3 177.58(16) . . . . ? C1 C2 C3 C4 -1.1(3) . . . . ? C2 C3 C4 N1 -176.4(2) . . . . ? C2 C3 C4 C5 1.2(3) . . . . ? N1 C4 C5 C6 177.31(19) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C4 C5 C6 C1 -0.8(3) . . . . ? C2 C1 C6 C5 0.9(3) . . . . ? S1 C1 C6 C5 -176.68(15) . . . . ? C10 N3 C7 N4 0.4(3) . . . . ? C10 N3 C7 N2 -179.01(15) . . . . ? C8 N4 C7 N3 0.2(3) . . . . ? C8 N4 C7 N2 179.62(15) . . . . ? S1 N2 C7 N3 -3.0(2) . . . . ? S1 N2 C7 N4 177.49(12) . . . . ? C7 N4 C8 C9 -0.2(3) . . . . ? N4 C8 C9 C10 -0.3(3) . . . . ? C7 N3 C10 C9 -0.9(2) . . . . ? C7 N3 C10 C11 178.43(16) . . . . ? C8 C9 C10 N3 0.9(3) . . . . ? C8 C9 C10 C11 -178.44(18) . . . . ? 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 C6 H6 O1 0.93 2.49 3.389(2) 163.6 8_665 C8 H8 O2 0.93 2.51 3.231(2) 134.6 5_666 C9 H9 O2 0.93 2.61 3.233(2) 125.3 1_655 N2 H1N2 N4 0.82(2) 2.11(2) 2.927(2) 177(2) 5_666 N1 H1N1 O2 0.86(3) 2.22(3) 3.076(2) 171(2) 6_656 N1 H2N1 O1 0.84(3) 2.49(3) 3.030(2) 123(2) 3_655 N1 H2N1 N3 0.84(3) 2.63(3) 3.409(2) 155(2) 3_655 _refine_diff_density_max 0.402 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.064 _shelx_res_file ; 180k_smz-f2_a.res created by SHELXL-2014/7 TITL 180k_smz-f2_a.res in Pbca REM Old TITL 044_180K_SulfamerazineF2_ in Pbca REM SHELXT solution in Pbca REM R1 0.107, Rweak 0.261, Alpha 0.021, Orientation as input REM Formula found by SHELXT: C12 N3 O2 S CELL 0.68890 9.0972 11.5751 22.8531 90.000 90.000 90.000 ZERR 8.000 0.0002 0.0002 0.0003 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 FMAP 2 PLAN -32 BOND $H L.S. 12 SIZE 0.50 0.40 0.20 ACTA CONF REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, y+1/2, z HTAB C6 O1_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB C8 O2_$2 EQIV $3 x+1, y, z HTAB C9 O2_$3 HTAB N2 N4_$2 EQIV $4 x+1/2, y, -z+1/2 HTAB N1 O2_$4 EQIV $5 -x+1, y+1/2, -z+1/2 HTAB N1 O1_$5 HTAB N1 N3_$5 LIST 4 WGHT 0.046300 1.482700 FVAR 0.55510 S1 5 0.331665 0.345962 0.389685 11.00000 0.02404 0.02431 = 0.02115 -0.00167 -0.00034 -0.00280 O2 4 0.196505 0.397014 0.409663 11.00000 0.02175 0.04006 = 0.02511 -0.00204 0.00035 -0.00137 O1 4 0.341650 0.222934 0.386507 11.00000 0.04081 0.02377 = 0.02822 -0.00055 -0.00117 -0.00517 N4 3 0.666890 0.426090 0.485404 11.00000 0.02463 0.02916 = 0.02426 -0.00236 -0.00265 0.00092 N3 3 0.655878 0.284782 0.408799 11.00000 0.02749 0.02634 = 0.02700 -0.00113 0.00242 0.00328 N2 3 0.451350 0.395116 0.437246 11.00000 0.02337 0.02800 = 0.02518 -0.00790 -0.00197 0.00414 N1 3 0.454308 0.532514 0.154472 11.00000 0.04699 0.03184 = 0.02933 0.00434 0.01115 0.00291 C1 1 0.374535 0.403601 0.321495 11.00000 0.02640 0.02530 = 0.02211 -0.00171 -0.00009 -0.00174 C2 1 0.447655 0.336528 0.280127 11.00000 0.03757 0.02743 = 0.02824 -0.00028 0.00549 0.00688 AFIX 43 H2 2 0.476909 0.261783 0.289465 11.00000 -1.30000 AFIX 0 C3 1 0.476699 0.380800 0.225376 11.00000 0.04221 0.02837 = 0.02886 -0.00240 0.00994 0.00571 AFIX 43 H3 2 0.527038 0.335870 0.198235 11.00000 -1.30000 AFIX 0 C4 1 0.431477 0.492724 0.209903 11.00000 0.03015 0.02864 = 0.02567 -0.00041 0.00340 -0.00479 C5 1 0.358047 0.559280 0.252291 11.00000 0.03606 0.02155 = 0.03118 -0.00015 0.00386 -0.00015 AFIX 43 H5 2 0.327475 0.633748 0.243055 11.00000 -1.30000 AFIX 0 C6 1 0.330728 0.515484 0.307478 11.00000 0.02892 0.02280 = 0.02798 -0.00368 0.00368 -0.00111 AFIX 43 H6 2 0.283092 0.560727 0.335251 11.00000 -1.30000 AFIX 0 C7 1 0.598038 0.365921 0.443091 11.00000 0.02430 0.02458 = 0.02125 0.00215 -0.00002 -0.00021 C8 1 0.808572 0.400580 0.493016 11.00000 0.02234 0.03980 = 0.02730 0.00153 -0.00331 0.00004 AFIX 43 H8 2 0.861119 0.440028 0.521640 11.00000 -1.30000 AFIX 0 C9 1 0.880079 0.318331 0.460262 11.00000 0.02043 0.04134 = 0.03036 0.00643 0.00118 0.00515 AFIX 43 H9 2 0.979094 0.302154 0.466208 11.00000 -1.30000 AFIX 0 C10 1 0.799470 0.260559 0.418176 11.00000 0.02935 0.02833 = 0.02969 0.00636 0.00605 0.00644 C11 1 0.867040 0.167322 0.381352 11.00000 0.03776 0.04044 = 0.04520 -0.00417 0.00922 0.01322 AFIX 137 H11A 2 0.820009 0.094943 0.389729 11.00000 -1.30000 H11B 2 0.970021 0.161594 0.390054 11.00000 -1.30000 H11C 2 0.854328 0.185769 0.340711 11.00000 -1.30000 AFIX 0 H1N2 2 0.415720 0.444192 0.458596 11.00000 0.03550 H1N1 2 0.514862 0.492818 0.133845 11.00000 0.04112 H2N1 2 0.447365 0.603453 0.146827 11.00000 0.05355 HKLF 4 REM 180k_smz-f2_a.res in Pbca REM R1 = 0.0458 for 2723 Fo > 4sig(Fo) and 0.0653 for all 3566 data REM 176 parameters refined using 0 restraints END WGHT 0.0488 0.8762 REM Highest difference peak 0.402, deepest hole -0.413, 1-sigma level 0.064 Q1 1 0.3581 0.3783 0.3517 11.00000 0.05 0.40 Q2 1 0.3844 0.3605 0.3012 11.00000 0.05 0.34 Q3 1 0.6355 0.3865 0.4692 11.00000 0.05 0.30 Q4 1 0.4307 0.3622 0.2513 11.00000 0.05 0.28 Q5 1 0.4792 0.4467 0.2244 11.00000 0.05 0.27 Q6 1 0.8328 0.2207 0.3967 11.00000 0.05 0.25 Q7 1 0.6398 0.3342 0.4220 11.00000 0.05 0.25 Q8 1 0.3363 0.5353 0.2812 11.00000 0.05 0.25 Q9 1 0.3386 0.4420 0.3127 11.00000 0.05 0.25 Q10 1 0.8328 0.3665 0.4725 11.00000 0.05 0.24 Q11 1 0.5970 0.2512 0.3895 11.00000 0.05 0.24 Q12 1 0.3807 0.5249 0.2328 11.00000 0.05 0.24 Q13 1 0.6191 0.4421 0.5128 11.00000 0.05 0.23 Q14 1 0.8410 0.2840 0.4413 11.00000 0.05 0.22 Q15 1 0.1819 0.3640 0.4523 11.00000 0.05 0.21 Q16 1 0.4289 0.4992 0.1888 11.00000 0.05 0.21 Q17 1 0.1024 0.3080 0.3908 11.00000 0.05 0.21 Q18 1 0.7409 0.2894 0.4089 11.00000 0.05 0.21 Q19 1 0.3473 0.1619 0.3360 11.00000 0.05 0.20 Q20 1 0.2059 0.3462 0.3922 11.00000 0.05 0.20 Q21 1 0.3819 0.4638 0.1067 11.00000 0.05 0.20 Q22 1 0.1556 0.3930 0.4121 11.00000 0.05 0.20 Q23 1 0.2227 0.1446 0.4382 11.00000 0.05 0.19 Q24 1 0.8545 0.4604 0.5398 11.00000 0.05 0.19 Q25 1 0.6371 0.3028 0.2019 11.00000 0.05 0.19 Q26 1 0.1647 0.4814 0.4496 11.00000 0.05 0.19 Q27 1 0.3410 0.2715 0.3709 11.00000 0.05 0.18 Q28 1 0.6476 0.4445 0.2920 11.00000 0.05 0.18 Q29 1 0.7282 0.4021 0.4859 11.00000 0.05 0.18 Q30 1 0.3806 0.1958 0.3602 11.00000 0.05 0.18 Q31 1 0.5500 0.3040 0.3080 11.00000 0.05 0.18 Q32 1 0.3000 0.7196 0.2751 11.00000 0.05 0.18 ; _shelx_res_checksum 17188 _shelx_hkl_file ; 0 0 2 876.94 15.57 0 0 3 -0.87 1.48 0 0 3 1.56 0.80 0 0 4 2967.92 40.96 0 0 4 2966.61 40.12 0 0 5 -1.43 1.47 0 0 5 -2.55 1.61 0 0 6 7762.93 80.14 0 0 6 7976.77 79.93 0 0 7 0.85 1.60 0 0 7 -0.27 0.98 0 0 8 1170.50 35.57 0 0 8 1209.42 36.28 0 0 9 2.70 3.63 0 0 9 0.37 1.87 0 0 10 6118.17 90.43 0 0 11 -2.71 2.37 0 0 11 0.96 2.88 0 0 12 -1.83 4.26 0 0 12 -1.12 3.41 0 0 13 -1.86 2.91 0 0 13 -1.18 4.21 0 0 14 868.82 41.34 0 0 14 794.67 38.29 0 0 15 -0.58 3.72 0 0 15 1.45 5.29 0 0 16 15.27 6.00 0 0 16 18.15 7.10 0 0 17 8.09 5.62 0 0 17 -0.37 2.31 0 0 18 1502.43 59.62 0 0 18 1535.89 61.98 0 0 19 -3.26 4.62 0 0 19 8.67 7.60 0 0 20 208.86 23.24 0 0 20 182.31 22.23 0 0 21 -3.11 5.03 0 0 21 -3.76 5.52 0 0 22 306.60 30.41 0 0 22 270.32 27.94 0 0 23 2.89 6.36 0 0 23 3.52 5.02 0 0 24 114.14 20.38 0 0 24 98.17 16.85 0 0 25 -1.95 7.51 0 0 25 3.12 3.38 0 0 26 90.23 17.96 0 0 26 60.50 13.77 0 0 27 -6.00 7.23 0 0 27 3.55 3.35 0 0 28 75.40 17.25 0 0 28 91.71 18.05 0 0 29 -1.61 6.90 0 0 29 -7.83 8.25 0 0 30 280.63 33.92 0 0 30 424.34 38.87 0 0 31 5.03 3.79 0 0 31 3.01 5.22 0 0 32 15.61 12.19 0 0 32 -4.89 5.03 0 -1 0 0.01 0.28 0 -1 0 0.64 0.82 0 -1 1 -0.34 0.82 0 1 1 0.07 0.72 0 -1 1 0.51 0.94 0 -1 -1 0.40 0.46 0 -1 2 -0.42 0.66 0 1 2 -0.33 0.62 0 1 2 0.15 0.65 0 -1 2 0.48 0.78 0 -1 3 -0.01 0.71 0 1 3 0.81 0.84 0 1 3 0.02 0.59 0 -1 3 0.38 0.76 0 -1 4 0.79 0.95 0 -1 4 -0.60 0.99 0 1 4 -1.45 1.78 0 -1 4 -0.64 0.56 0 1 4 0.93 1.14 0 -1 5 1.03 0.97 0 1 5 1.66 1.39 0 1 5 1.30 2.31 0 -1 5 1.50 2.11 0 -1 5 -0.27 1.72 0 -1 6 -1.25 1.94 0 1 6 -0.56 1.13 0 1 6 -1.10 1.38 0 -1 6 0.27 1.13 0 -1 7 -0.68 1.86 0 -1 7 -1.63 1.86 0 1 7 1.77 3.05 0 1 7 1.86 2.14 0 1 8 -0.33 2.50 0 1 8 1.17 1.01 0 -1 8 -0.35 1.78 0 -1 8 2.29 3.15 0 -1 9 -0.92 2.73 0 -1 9 3.25 3.94 0 1 9 -1.20 1.14 0 1 9 -0.06 2.68 0 -1 10 3.67 3.39 0 -1 10 1.58 2.57 0 1 10 -0.02 2.15 0 1 10 1.74 3.00 0 -1 11 0.75 2.54 0 -1 11 -0.51 1.43 0 1 11 -1.59 2.90 0 1 11 0.76 3.99 0 1 12 -0.80 2.91 0 1 12 4.37 1.39 0 -1 12 2.36 2.75 0 -1 12 0.94 1.40 0 -1 13 8.67 5.33 0 1 13 -0.07 1.84 0 1 13 0.96 2.48 0 -1 13 0.76 3.45 0 1 14 -1.28 4.31 0 1 14 -0.03 2.45 0 -1 14 0.31 2.93 0 -1 14 -2.62 4.12 0 1 15 0.43 3.56 0 1 15 -0.94 3.81 0 -1 15 -3.97 3.67 0 -1 15 -1.02 3.72 0 1 16 0.37 5.42 0 -1 16 3.14 4.20 0 1 16 -0.81 2.47 0 -1 16 2.37 2.43 0 -1 17 3.50 4.38 0 -1 17 3.56 4.82 0 1 17 -0.29 2.70 0 1 17 -1.53 3.41 0 -1 18 -4.54 7.69 0 -1 18 4.87 5.88 0 1 18 2.24 4.40 0 1 18 1.14 4.75 0 -1 19 -4.02 2.89 0 -1 19 1.10 2.53 0 1 19 0.19 5.58 0 1 19 1.19 3.50 0 -1 20 -5.04 5.84 0 1 20 -0.18 3.91 0 1 20 2.11 2.88 0 -1 20 1.32 4.80 0 -1 21 1.78 3.89 0 -1 21 -8.52 4.48 0 1 21 0.33 8.35 0 1 21 2.32 6.35 0 -1 22 7.37 7.08 0 1 22 -2.76 5.49 0 1 22 -2.69 3.67 0 -1 22 0.45 3.87 0 -1 23 -3.12 3.18 0 -1 23 1.48 5.00 0 1 23 -1.88 3.26 0 1 23 -4.00 5.92 0 -1 24 0.18 2.00 0 -1 24 -1.31 4.94 0 1 24 -0.50 3.02 0 -1 25 -1.47 4.51 0 1 25 6.47 8.46 0 1 25 -0.32 4.23 0 -1 25 5.84 7.85 0 -1 26 -2.09 2.83 0 1 26 4.26 10.63 0 1 26 3.12 4.56 0 -1 26 -0.08 5.52 0 1 27 -2.49 6.50 0 1 27 -3.54 5.06 0 -1 27 1.29 3.32 0 -1 27 -5.36 5.55 0 1 28 3.78 5.08 0 -1 28 1.99 6.19 0 -1 28 -3.65 5.45 0 1 28 0.42 5.22 0 -1 29 6.99 7.15 0 1 29 -10.00 8.83 0 -1 29 -3.97 8.53 0 1 29 -2.57 3.19 0 -1 30 1.73 6.78 0 1 30 2.78 6.89 0 -1 30 3.01 2.84 0 1 30 -6.48 5.20 0 -1 31 6.45 6.68 0 -1 31 15.93 13.10 0 1 31 -0.67 5.66 0 1 31 0.22 5.86 0 1 32 5.70 3.35 0 -1 32 1.00 6.14 0 -1 32 -0.86 6.26 0 1 32 -1.68 3.32 0 -2 0 7.10 2.22 0 -2 0 5.78 1.85 0 -2 1 8159.27 67.50 0 -2 1 8246.59 69.56 0 -2 -1 8255.62 68.61 0 -2 2 4255.75 52.61 0 -2 -2 4397.20 51.60 0 -2 2 4393.04 52.44 0 -2 3 9686.66 83.15 0 2 3 9727.52 68.44 0 2 3 9999.00 79.47 0 -2 3 9731.14 80.03 0 -2 -3 9708.59 83.18 0 -2 4 7602.85 78.05 0 2 4 7993.28 68.48 0 2 4 7768.33 75.41 0 -2 -4 7887.01 77.54 0 -2 4 7801.44 74.39 0 -2 5 8609.90 81.88 0 2 5 8361.04 83.43 0 2 5 8432.46 77.63 0 -2 6 8784.87 92.37 0 -2 6 8492.44 88.93 0 2 6 8359.06 89.50 0 2 6 8173.95 84.49 0 -2 6 8619.31 87.76 0 -2 7 94.00 10.07 0 2 7 106.79 10.70 0 2 7 93.76 9.92 0 -2 7 90.70 9.88 0 -2 7 105.93 10.66 0 2 8 508.63 24.26 0 2 8 600.36 25.91 0 -2 8 555.59 25.49 0 -2 8 616.47 27.07 0 -2 8 570.75 26.71 0 2 9 1960.73 49.92 0 -2 9 1902.01 50.61 0 -2 9 1906.89 49.28 0 2 10 1005.92 37.32 0 2 10 896.88 35.43 0 -2 10 966.81 36.57 0 -2 10 1020.07 38.53 0 -2 11 1362.80 45.43 0 -2 11 1321.81 46.03 0 2 11 1291.65 44.70 0 2 11 1289.67 44.48 0 -2 12 547.70 30.01 0 2 12 609.91 32.17 0 2 12 559.45 30.71 0 -2 12 532.53 30.72 0 -2 13 142.59 16.03 0 2 13 143.33 16.06 0 2 13 143.23 16.32 0 -2 13 154.97 16.98 0 2 14 919.16 42.78 0 2 14 794.95 38.58 0 -2 14 911.17 41.02 0 -2 14 814.39 41.05 0 -2 15 31.78 9.31 0 2 15 31.05 8.26 0 -2 15 36.70 8.31 0 2 15 37.00 8.19 0 -2 16 89.44 14.60 0 -2 16 120.83 16.11 0 2 16 72.61 13.92 0 2 16 109.04 15.46 0 2 17 576.49 36.82 0 2 17 546.52 35.37 0 -2 17 607.91 37.35 0 -2 17 554.78 37.20 0 2 18 343.90 29.01 0 2 18 382.84 30.35 0 -2 18 332.97 29.40 0 -2 18 307.41 27.10 0 2 19 855.59 48.05 0 2 19 771.17 43.59 0 -2 19 831.24 45.59 0 -2 19 701.32 43.21 0 2 20 126.07 18.65 0 2 20 129.06 18.42 0 -2 20 100.34 17.01 0 -2 20 138.24 19.43 0 -2 21 73.77 15.88 0 2 21 60.45 12.11 0 -2 21 77.70 13.93 0 2 21 65.54 12.68 0 2 22 4.86 4.37 0 2 22 2.04 7.32 0 -2 22 8.55 7.06 0 -2 22 8.56 7.70 0 2 23 582.91 43.39 0 -2 23 594.88 43.03 0 -2 23 606.31 43.18 0 2 23 669.09 44.47 0 2 24 26.21 8.86 0 -2 24 21.29 12.29 0 -2 24 7.30 3.61 0 2 24 6.48 5.03 0 2 25 21.79 8.23 0 -2 25 8.87 4.47 0 2 25 5.42 5.62 0 -2 25 13.91 7.22 0 -2 26 144.56 22.55 0 2 26 132.00 19.70 0 2 26 167.25 23.92 0 -2 26 148.49 23.93 0 2 27 15.73 8.45 0 -2 27 -0.10 4.43 0 -2 27 13.16 7.67 0 -2 28 13.92 4.92 0 2 28 20.29 10.02 0 2 28 14.29 8.43 0 -2 28 12.92 8.35 0 -2 29 109.53 19.19 0 2 29 109.76 19.79 0 2 29 91.84 18.55 0 -2 29 96.54 20.06 0 2 30 -0.25 7.05 0 -2 30 2.33 6.69 0 2 30 7.47 6.42 0 -2 30 17.80 5.94 0 -2 31 18.06 12.85 0 -2 31 -1.62 8.70 0 2 31 3.30 8.84 0 2 31 19.14 9.11 0 -2 32 59.19 17.51 0 -2 32 72.28 15.61 0 2 32 46.59 10.79 0 2 32 58.53 16.42 0 -3 0 0.75 1.39 0 -3 0 0.48 1.57 0 -3 1 -0.79 0.87 0 3 1 -0.68 1.38 0 -3 1 3.58 2.42 0 -3 -1 2.03 2.71 0 3 2 0.76 0.87 0 -3 -2 0.87 1.45 0 -3 2 0.05 2.11 0 -3 2 1.17 1.55 0 3 2 -1.84 1.21 0 -3 -3 -0.87 2.06 0 3 3 -0.73 1.34 0 -3 3 -1.21 2.25 0 3 3 -1.47 1.97 0 -3 3 0.53 2.63 0 -3 4 -1.42 2.18 0 3 4 -1.67 2.97 0 -3 -4 1.12 2.56 0 -3 4 -0.47 1.57 0 3 4 1.77 2.00 0 -3 -5 1.32 1.73 0 3 5 -3.19 2.69 0 3 5 -0.89 2.14 0 -3 5 -1.50 2.71 0 -3 5 -1.52 1.09 0 3 6 -0.18 2.10 0 -3 6 1.98 1.07 0 3 6 -0.09 0.98 0 -3 -6 -0.97 1.39 0 -3 6 -0.47 2.41 0 -3 7 1.25 2.11 0 3 7 2.67 2.96 0 -3 7 -0.34 1.84 0 3 7 -1.25 2.26 0 3 8 1.89 2.48 0 -3 8 -0.32 2.46 0 -3 8 -0.54 1.74 0 3 8 1.52 2.54 0 -3 8 -0.29 1.68 0 3 9 1.87 3.96 0 -3 9 -0.88 1.91 0 3 9 3.94 3.57 0 -3 9 -1.11 1.95 0 -3 9 0.93 2.99 0 3 10 -0.96 2.16 0 3 10 -0.54 2.76 0 -3 10 0.30 1.53 0 -3 10 -0.86 3.27 0 -3 10 1.36 3.82 0 -3 11 2.33 4.52 0 -3 11 1.19 1.37 0 -3 11 3.97 2.80 0 3 11 1.65 3.13 0 3 11 -0.76 2.63 0 -3 12 2.53 5.73 0 -3 12 3.52 3.35 0 3 12 -0.63 1.97 0 3 12 -1.97 4.69 0 -3 12 1.05 2.61 0 -3 13 -0.94 4.07 0 3 13 -3.70 4.73 0 -3 13 -1.11 2.38 0 3 13 0.36 5.41 0 -3 14 1.76 5.99 0 3 14 1.28 2.79 0 3 14 0.29 2.93 0 -3 14 -0.57 2.69 0 3 15 1.37 3.06 0 3 15 -1.00 2.39 0 -3 15 2.83 2.86 0 -3 15 1.50 3.30 0 3 16 -2.43 5.53 0 -3 16 0.02 2.89 0 -3 16 2.48 5.64 0 3 16 1.49 5.32 0 -3 17 1.28 3.07 0 3 17 -2.73 3.16 0 -3 17 -2.08 3.38 0 3 17 0.42 7.20 0 -3 18 5.12 6.32 0 3 18 -0.69 2.33 0 3 18 -0.50 1.93 0 -3 18 0.55 4.32 0 -3 19 -0.65 2.75 0 3 19 3.12 3.87 0 -3 19 -1.55 2.30 0 3 19 4.83 2.46 0 -3 20 -0.77 3.06 0 3 20 2.19 5.40 0 -3 20 -0.90 4.78 0 3 20 -0.34 5.50 0 3 21 6.76 5.62 0 -3 21 -1.84 2.91 0 -3 21 -0.38 4.31 0 3 21 -1.93 5.89 0 -3 22 1.71 2.76 0 3 22 2.11 4.01 0 -3 22 3.99 6.35 0 3 22 -0.24 4.66 0 -3 23 1.42 8.15 0 3 23 4.08 3.95 0 3 23 6.15 5.74 0 -3 23 -1.39 5.05 0 3 24 7.08 9.34 0 3 24 -0.12 3.24 0 -3 24 4.85 4.27 0 -3 24 5.53 9.54 0 3 25 7.37 5.05 0 3 25 2.70 6.99 0 -3 25 -2.49 2.86 0 -3 25 1.87 4.36 0 -3 26 -0.43 4.80 0 3 26 -2.96 8.34 0 -3 26 3.00 5.59 0 3 26 3.06 4.06 0 3 27 1.99 7.81 0 -3 27 5.76 8.73 0 -3 27 3.13 6.52 0 3 27 -0.42 3.32 0 -3 28 -8.30 6.77 0 -3 28 -2.87 4.48 0 3 28 -0.17 3.80 0 3 28 -0.80 6.08 0 -3 29 -2.52 4.21 0 3 29 7.17 5.13 0 -3 29 -3.11 6.96 0 3 29 -3.44 5.94 0 -3 30 -4.92 6.32 0 -3 30 1.85 4.20 0 3 30 -7.82 7.26 0 3 30 -2.42 5.82 0 -3 31 -4.86 5.99 0 3 31 -1.99 5.65 0 -3 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126.02 18.02 2 -1 16 112.87 16.29 -2 1 17 49.25 10.71 -2 -1 17 51.77 11.46 2 -1 17 45.42 10.43 2 1 17 64.35 12.40 2 1 17 37.25 9.54 -2 1 17 55.47 12.23 2 -1 17 41.64 10.24 -2 -1 17 62.74 13.57 2 -1 18 1523.27 61.43 -2 -1 18 1522.97 63.03 -2 1 18 1472.23 60.43 2 1 18 1483.60 60.06 -2 -1 18 1519.61 59.64 -2 1 18 1359.95 56.15 2 1 18 1334.82 57.39 2 -1 18 1517.29 61.26 2 -1 19 -0.92 2.54 2 -1 19 -1.98 4.90 2 1 19 4.73 6.96 -2 1 19 3.35 4.41 -2 -1 19 4.69 3.14 -2 1 19 -8.24 8.45 -2 -1 19 -0.47 3.25 2 1 19 3.61 6.03 -2 -1 20 125.30 18.41 -2 -1 20 132.67 18.52 2 1 20 118.20 18.19 2 -1 20 142.20 19.16 -2 1 20 80.59 14.21 2 1 20 150.37 20.82 2 -1 20 162.20 20.21 -2 1 20 172.39 21.42 -2 1 21 69.46 14.49 2 -1 21 84.12 15.90 2 1 21 88.04 15.56 -2 -1 21 94.00 17.68 2 1 21 127.22 19.15 -2 -1 21 99.61 17.13 2 -1 21 114.61 17.61 -2 1 21 70.22 13.20 -2 -1 22 379.55 32.72 2 1 22 293.75 28.94 2 -1 22 312.60 30.24 2 -1 22 273.81 29.11 -2 1 22 269.84 27.30 2 1 22 310.99 30.93 -2 1 22 272.95 29.10 -2 -1 22 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29 243.07 31.77 -2 -1 29 212.07 28.59 -2 1 29 245.32 30.64 2 -1 29 205.45 28.47 2 1 29 240.75 28.71 -2 1 29 171.05 25.20 -2 -1 29 178.36 25.37 2 -1 29 225.70 28.10 -2 1 30 18.16 12.40 -2 1 30 25.52 10.72 -2 -1 30 31.62 9.69 2 1 30 31.08 10.27 2 -1 30 38.33 11.49 2 1 30 34.05 13.05 2 -1 30 20.34 10.69 -2 -1 30 12.26 7.92 -2 -1 31 13.87 9.27 2 1 31 11.35 7.97 2 -1 31 5.45 5.10 2 -1 31 2.62 4.84 -2 1 31 3.35 3.89 2 1 31 10.83 5.01 -2 -1 31 6.88 3.89 -2 1 31 -0.03 5.84 2 1 32 138.72 22.40 -2 -1 32 151.24 25.50 2 -1 32 110.82 20.92 -2 -1 32 134.96 23.45 -2 1 32 75.26 17.53 2 1 32 115.54 25.53 -2 1 32 85.72 19.26 2 -1 32 111.68 22.74 -2 -2 0 1283.50 29.91 2 -2 0 1301.20 25.23 -2 2 0 1457.34 37.01 -2 -2 0 1179.76 19.15 2 2 0 1444.56 19.26 2 -2 0 1263.93 33.38 -2 -2 1 247.85 13.61 2 -2 1 244.97 10.96 -2 -2 -1 240.64 12.48 2 -2 1 251.28 15.50 2 -2 -1 257.68 11.89 -2 2 1 253.76 15.66 -2 2 -1 250.20 15.53 -2 -2 1 309.20 10.81 2 2 1 251.34 9.23 2 -2 -1 239.28 14.26 2 2 2 8.65 2.11 2 -2 2 9.47 2.48 -2 -2 2 7.13 1.96 -2 -2 2 11.65 2.34 2 -2 2 7.10 2.82 2 -2 -2 5.60 1.79 2 -2 -2 6.87 2.56 -2 2 2 6.68 2.37 -2 -2 -2 9.62 3.30 -2 -2 3 3628.85 56.32 2 -2 3 3716.95 60.27 -2 -2 -3 3500.21 49.76 -2 2 3 3784.00 60.31 -2 -2 3 3528.79 46.24 2 2 3 3733.82 46.42 -2 -2 3 3659.73 34.01 -2 2 3 3527.20 54.41 2 -2 3 3796.63 45.94 2 2 4 3018.81 45.57 2 -2 4 2759.75 54.22 2 -2 4 2975.62 43.30 -2 2 4 2917.91 50.58 -2 2 4 2961.38 56.02 -2 -2 4 2910.05 35.51 -2 -2 4 2857.24 52.01 -2 -2 -4 2805.75 46.53 -2 -2 5 1785.12 43.32 2 2 5 1713.94 37.91 -2 2 5 1881.77 42.53 -2 -2 -5 1838.02 40.14 -2 -2 5 1753.56 31.51 2 -2 5 1743.42 35.84 -2 2 5 1783.22 44.58 2 -2 5 1842.01 44.20 -2 -2 6 452.63 21.23 2 2 6 449.97 20.75 -2 2 6 472.15 21.89 -2 -2 6 511.84 18.74 2 -2 6 500.94 23.81 -2 -2 6 510.35 23.91 -2 -2 -6 483.48 21.00 -2 2 6 403.48 21.74 2 -2 6 498.93 20.17 -2 2 7 624.51 28.14 2 2 7 598.37 25.58 -2 -2 7 679.28 23.84 2 -2 7 683.39 25.90 -2 2 7 642.71 26.63 -2 -2 7 651.13 28.57 -2 -2 7 695.78 28.24 2 -2 7 681.10 29.29 2 2 7 719.76 26.02 -2 -2 8 1.00 2.73 -2 2 8 3.37 2.33 -2 -2 8 2.04 2.60 2 2 8 3.83 1.68 -2 -2 8 6.87 3.16 2 2 8 4.62 2.80 2 -2 8 -0.02 1.61 -2 2 8 4.34 1.30 2 -2 8 6.48 2.62 -2 -2 9 26.98 5.61 2 -2 9 15.60 5.86 -2 2 9 28.15 7.10 2 2 9 21.58 4.93 -2 2 9 25.32 6.20 -2 -2 9 16.61 4.85 2 2 9 29.96 5.46 -2 -2 9 15.46 4.52 2 2 10 13.06 3.38 -2 2 10 12.24 2.97 2 2 10 13.88 4.85 -2 -2 10 12.18 4.39 -2 2 10 13.13 5.56 -2 -2 10 17.68 6.34 2 -2 10 9.54 5.01 2 -2 11 608.79 32.10 2 2 11 618.89 31.62 -2 2 11 602.71 30.99 -2 2 11 619.57 32.94 2 2 11 647.37 30.59 -2 -2 11 567.38 31.28 -2 -2 11 608.09 29.61 -2 2 12 5.62 5.01 2 2 12 4.96 2.98 -2 2 12 1.25 2.87 -2 -2 12 5.18 3.18 2 2 12 3.73 1.48 2 -2 12 -0.20 3.33 -2 -2 12 12.22 6.54 2 2 13 2013.11 61.11 -2 2 13 1867.27 58.31 -2 2 13 1954.26 62.69 2 -2 13 2064.33 62.41 -2 -2 13 2026.04 58.06 -2 -2 13 1764.96 59.25 2 2 13 2066.22 59.89 -2 2 14 6.00 3.98 2 2 14 9.36 5.89 2 2 14 16.98 5.84 2 -2 14 9.88 3.06 -2 -2 14 12.19 5.77 -2 -2 14 14.51 6.25 2 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19.27 -2 2 21 100.11 17.05 -2 -2 21 149.63 22.00 -2 2 21 150.80 20.96 2 -2 21 176.60 23.81 2 2 21 147.19 21.12 -2 -2 21 151.82 19.77 -2 -2 22 75.22 15.10 2 2 22 91.63 16.11 2 -2 22 92.90 16.47 -2 2 22 103.15 16.49 2 2 22 52.62 12.67 -2 -2 22 83.74 16.22 -2 2 22 96.73 17.37 2 -2 22 103.99 17.92 2 2 23 4.39 7.83 -2 2 23 4.57 4.97 2 2 23 6.18 5.92 -2 -2 23 4.29 5.59 2 -2 23 0.53 2.60 2 -2 23 9.63 9.71 -2 -2 23 6.72 10.14 -2 2 23 5.68 7.70 -2 -2 24 17.12 8.85 -2 2 24 5.18 3.52 2 2 24 5.47 8.35 2 -2 24 9.69 9.06 -2 2 24 3.84 7.26 2 -2 24 4.60 5.55 2 2 24 2.44 5.02 -2 -2 24 0.90 4.35 2 2 25 -0.96 3.70 -2 2 25 -1.29 4.67 2 2 25 0.66 7.24 -2 -2 25 11.83 10.39 -2 -2 25 0.27 6.45 2 -2 25 15.44 10.38 -2 2 25 5.83 7.76 2 -2 25 -0.80 4.99 2 -2 26 19.41 8.54 -2 2 26 18.69 8.27 2 2 26 8.13 6.10 2 -2 26 15.90 9.24 -2 2 26 30.59 11.47 -2 -2 26 33.97 11.96 2 2 26 18.65 8.42 -2 -2 26 43.44 13.05 2 2 27 53.66 13.61 -2 -2 27 44.98 12.81 2 -2 27 39.90 11.16 -2 2 27 30.18 7.04 -2 -2 27 48.63 13.46 -2 2 27 28.04 12.42 2 2 27 54.40 13.53 2 -2 27 12.22 8.69 -2 2 28 -2.11 7.55 -2 2 28 33.53 14.50 2 2 28 13.27 5.41 -2 -2 28 18.70 11.09 2 -2 28 12.69 5.37 -2 -2 28 20.89 10.81 2 2 28 -2.06 9.61 2 -2 28 13.72 10.26 2 -2 29 54.51 14.41 2 2 29 64.81 16.13 -2 2 29 64.38 16.46 -2 -2 29 62.51 16.58 2 -2 29 43.84 12.73 -2 2 29 66.49 15.67 -2 -2 29 73.86 17.00 2 2 29 49.75 14.12 2 2 30 19.62 8.83 2 2 30 9.28 11.09 -2 -2 30 6.33 8.62 2 -2 30 4.28 5.74 -2 2 30 15.58 7.99 -2 -2 30 12.67 8.93 -2 2 30 15.84 9.65 2 -2 30 12.29 9.48 -2 2 31 33.17 13.04 2 2 31 42.70 13.90 -2 -2 31 18.65 7.14 2 -2 31 15.25 3.85 2 -2 31 38.02 12.84 2 2 31 23.27 11.59 -2 -2 31 19.63 11.87 -2 2 31 20.84 9.35 -2 -2 32 4.79 7.94 -2 2 32 7.11 3.46 2 2 32 17.96 12.33 -2 -2 32 9.22 3.41 2 -2 32 10.31 8.59 2 -2 32 -2.27 10.73 -2 2 32 27.10 11.18 2 2 32 -2.16 9.38 -2 -3 0 1078.52 32.04 2 -3 0 1060.88 28.75 -2 -3 0 1094.28 23.69 -2 3 0 1067.92 34.61 2 -3 0 1085.41 35.00 2 -3 -1 533.85 24.22 2 -3 1 498.22 24.33 2 -3 1 562.67 21.02 -2 -3 -1 535.59 22.53 -2 3 1 595.36 25.40 2 3 1 547.50 17.56 -2 -3 1 525.80 23.05 -2 -3 1 627.80 13.32 -2 -3 1 561.06 16.83 2 -3 -1 572.12 21.25 2 -3 2 26.94 5.70 2 -3 -2 26.73 5.49 -2 -3 2 25.11 3.88 -2 -3 -2 28.40 5.27 2 -3 -2 31.93 5.19 -2 -3 2 20.73 3.17 -2 3 2 17.41 4.49 2 -3 2 25.86 4.73 -2 -3 2 25.86 4.99 2 3 2 25.11 4.38 -2 -3 3 93.63 7.10 2 -3 3 85.75 8.29 -2 -3 3 81.99 9.36 2 -3 -3 77.13 8.56 -2 -3 -3 95.60 9.80 2 -3 3 91.06 10.87 -2 -3 3 111.17 8.12 2 3 3 72.21 4.57 2 3 3 113.78 8.79 -2 3 3 90.15 10.00 2 -3 4 35.19 5.69 2 3 4 19.71 3.79 -2 3 4 26.19 5.69 -2 -3 4 24.05 5.45 -2 -3 4 33.67 4.43 -2 -3 -4 25.97 5.67 -2 3 4 27.37 5.84 2 -3 -4 24.64 5.26 -2 -3 4 33.23 5.43 2 3 4 26.66 3.58 2 -3 4 29.07 5.85 -2 -3 5 222.70 16.98 2 -3 5 225.10 14.84 2 -3 5 211.97 16.49 2 -3 -5 240.63 16.13 -2 3 5 227.76 17.04 -2 -3 -5 223.64 15.57 -2 -3 5 214.55 11.97 -2 -3 5 238.14 14.80 -2 3 5 193.28 14.94 2 3 5 181.46 10.36 2 3 5 201.81 13.96 2 -3 6 343.34 20.98 -2 -3 -6 341.58 19.93 2 3 6 385.73 20.55 -2 3 6 372.92 21.97 -2 -3 6 362.00 16.98 -2 3 6 360.10 20.98 2 3 6 355.87 15.89 2 -3 6 315.46 18.04 -2 -3 6 318.60 20.44 2 -3 7 20.39 4.99 -2 -3 7 16.37 4.37 -2 -3 7 17.06 5.49 -2 3 7 23.00 5.79 -2 3 7 22.73 5.35 2 -3 7 21.10 5.31 -2 -3 -7 18.68 4.79 -2 -3 7 22.18 5.95 2 3 7 13.99 4.99 2 3 7 15.19 3.71 2 -3 8 634.38 27.72 -2 -3 8 659.07 31.09 -2 -3 8 704.18 30.31 -2 -3 -8 616.15 28.56 -2 -3 8 628.24 25.51 -2 3 8 688.77 31.52 2 3 8 710.63 30.38 2 -3 8 590.82 29.55 -2 3 8 629.00 29.57 2 3 8 531.96 23.14 -2 -3 9 324.77 22.75 -2 3 9 368.29 24.26 -2 -3 9 386.36 21.41 2 3 9 353.09 22.12 -2 3 9 335.60 22.22 -2 -3 -9 337.29 21.85 2 -3 9 369.46 24.24 2 -3 9 353.25 21.55 2 3 9 351.46 20.36 -2 -3 9 378.12 23.51 2 3 10 151.44 13.95 -2 -3 10 155.02 14.20 -2 -3 10 180.78 17.00 2 -3 10 172.50 17.15 -2 -3 10 151.20 16.05 -2 3 10 136.10 15.88 2 3 10 153.19 14.83 -2 3 10 166.17 16.32 2 3 11 411.85 26.01 -2 -3 11 498.67 29.58 2 3 11 440.63 25.49 -2 -3 11 424.48 24.44 -2 3 11 441.79 28.05 -2 3 11 423.10 26.67 2 -3 11 349.20 25.11 -2 -3 11 423.73 28.89 -2 3 12 9.02 5.59 -2 -3 12 0.51 1.88 2 3 12 1.96 3.42 -2 -3 12 2.30 2.83 2 3 12 7.23 1.66 -2 3 12 8.48 3.47 2 -3 12 2.07 2.32 -2 -3 12 5.89 4.35 -2 3 13 120.73 15.32 -2 -3 13 131.92 16.38 -2 -3 13 115.64 13.94 2 3 13 105.67 13.31 -2 3 13 113.23 15.12 2 -3 13 105.43 14.31 2 3 13 123.88 15.91 -2 -3 14 15.23 6.62 -2 -3 14 11.33 5.59 2 3 14 4.97 3.25 -2 3 14 11.79 8.46 -2 3 14 2.40 3.47 2 3 14 8.95 3.85 2 -3 14 18.05 7.29 2 3 15 111.47 15.36 -2 -3 15 70.49 13.11 -2 3 15 59.11 11.85 -2 -3 15 94.24 14.14 2 -3 15 110.10 15.81 2 3 15 86.97 14.04 2 -3 15 97.22 14.86 -2 3 15 85.82 14.89 -2 3 16 -0.46 2.80 2 -3 16 0.22 5.37 2 3 16 1.08 2.36 -2 -3 16 6.00 7.73 -2 -3 16 -1.06 2.66 -2 3 16 6.21 5.69 2 -3 16 2.19 4.44 2 3 16 2.33 5.19 -2 3 17 354.87 28.36 -2 -3 17 377.57 29.35 2 -3 17 388.98 30.74 -2 -3 17 350.37 30.20 2 3 17 372.15 29.12 2 3 17 386.58 30.09 2 -3 17 436.46 32.72 -2 3 17 389.94 31.90 -2 -3 18 153.49 19.33 2 -3 18 186.92 21.04 2 3 18 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7.63 10 -5 7 0.59 6.24 -10 5 7 -8.36 8.90 10 -5 8 54.49 12.59 -10 5 8 66.55 16.01 10 -5 9 49.04 14.96 -10 5 9 41.23 12.11 -10 5 10 158.72 23.61 10 -5 10 157.56 24.07 10 -5 11 20.42 11.50 -10 5 11 40.43 13.83 10 -5 12 14.51 8.40 -10 5 12 -0.41 7.00 -10 5 13 -5.58 10.38 10 -5 13 -9.18 5.25 -10 5 14 42.15 10.57 10 -5 14 65.02 16.12 -10 5 15 -1.82 3.20 10 -5 15 -1.47 3.25 -10 5 16 -3.56 4.63 10 -5 16 9.62 7.65 -10 5 17 10.36 5.44 10 -5 17 28.45 13.04 -10 5 18 39.08 12.17 10 -5 18 44.15 14.31 10 -6 3 6.89 6.95 10 -6 4 64.43 14.47 10 -6 5 6.58 4.39 -10 6 5 14.57 6.03 10 -6 6 10.75 7.11 -10 6 6 9.55 6.35 10 -6 7 13.55 9.16 -10 6 7 -3.36 4.44 10 -6 8 24.24 9.15 -10 6 8 11.83 7.32 10 -6 9 41.81 12.18 -10 6 9 14.54 4.34 -10 6 10 171.31 25.66 10 -6 10 166.42 24.07 10 -6 11 7.99 8.40 -10 6 11 -3.92 5.51 10 -6 12 5.75 7.55 -10 6 12 7.21 5.65 10 -6 13 -4.01 8.00 -10 6 13 -5.44 7.24 10 -6 14 4.17 6.72 -10 6 14 23.41 12.08 -10 6 15 45.42 15.57 10 -6 15 -0.33 7.07 -10 6 16 28.23 9.50 10 -6 16 50.60 14.30 -10 6 17 0.98 10.72 10 -6 17 18.25 11.78 10 -7 0 17.99 6.85 10 -7 1 261.06 30.09 10 -7 -1 165.71 25.40 10 -7 2 51.59 14.85 10 -7 3 70.74 15.90 10 -7 4 3.46 6.11 10 -7 5 17.39 8.01 -10 7 5 4.66 4.44 10 -7 6 22.29 8.99 -10 7 6 34.57 11.35 10 -7 7 79.03 17.00 -10 7 7 64.67 18.18 10 -7 8 14.08 8.79 -10 7 8 13.00 7.38 10 -7 9 14.90 10.41 -10 7 9 -6.60 7.34 10 -7 10 2.28 3.74 -10 7 10 14.20 3.42 -10 7 11 185.65 27.28 10 -7 11 209.18 27.97 10 -7 12 8.72 4.80 -10 7 12 28.83 12.76 10 -7 13 58.01 17.56 -10 7 13 75.70 16.06 10 -7 14 -6.30 8.82 -10 7 14 16.52 11.31 10 -7 15 72.45 17.20 -10 7 15 63.95 17.54 10 -8 0 57.40 15.81 10 -8 1 12.99 5.45 10 -8 -1 3.33 4.88 10 -8 -2 11.13 9.71 10 -8 2 24.06 9.94 10 -8 -3 8.09 9.85 10 -8 3 -6.57 5.29 10 -8 -4 6.97 6.87 10 -8 4 -10.13 4.23 10 -8 5 6.68 5.01 10 -8 6 42.27 12.79 -10 8 6 37.63 12.73 10 -8 7 79.35 16.11 -10 8 7 152.85 24.32 10 -8 8 0.85 4.22 -10 8 8 -2.02 9.93 10 -8 9 15.90 8.78 -10 8 9 12.92 7.94 10 -8 10 -7.72 4.20 -10 8 10 -2.21 5.65 10 -8 11 109.04 18.85 -10 8 11 86.61 18.28 10 -8 12 57.00 15.67 -10 8 12 35.56 13.42 10 -8 13 -0.39 5.51 -10 8 13 24.50 12.32 10 -9 0 122.39 22.70 10 -9 1 29.61 10.29 10 -9 -1 24.99 7.89 10 -9 -2 16.77 9.28 10 -9 2 22.23 9.28 10 -9 3 124.88 22.96 10 -9 -3 71.54 18.60 10 -9 -4 45.60 14.68 10 -9 4 68.81 16.40 10 -9 -5 65.42 17.81 10 -9 5 37.71 13.98 10 -9 -6 11.19 8.03 10 -9 6 4.05 6.45 10 -9 7 149.10 24.79 10 -9 8 14.19 7.90 -10 9 8 14.64 10.21 10 -9 9 11.68 6.51 -10 9 9 5.95 8.97 10 -9 10 3.34 7.42 -10 9 10 0.39 7.37 10 -10 0 8.28 6.70 10 -10 1 4.24 6.58 10 -10 -1 17.06 6.11 10 -10 -2 16.18 10.76 10 -10 2 -2.88 7.26 10 -10 -3 24.02 9.23 10 -10 3 -8.04 8.43 10 -10 -4 13.29 4.87 10 -10 4 7.29 7.27 10 -10 -5 19.75 13.56 10 -10 5 13.43 11.15 10 -10 -6 7.78 8.57 10 -10 6 -8.19 8.66 -11 0 4 55.97 15.38 -11 0 5 2.37 7.85 -11 0 6 32.13 13.85 -11 0 7 -4.14 8.82 -11 0 8 16.68 9.57 -11 0 9 1.40 3.92 -11 0 10 94.69 16.70 -11 0 11 -6.05 4.73 -11 0 12 -3.14 4.66 -11 0 13 -1.67 6.60 -11 0 14 99.00 20.45 -11 0 15 0.67 9.20 -11 0 16 282.44 34.06 -11 0 17 11.67 5.48 -11 1 4 26.99 12.28 -11 -1 5 21.73 14.26 -11 1 5 0.68 3.75 -11 -1 6 36.87 12.94 -11 1 6 61.66 16.09 -11 1 7 15.14 7.77 -11 -1 7 5.65 4.56 -11 1 8 -2.80 5.23 -11 -1 8 3.57 5.82 -11 1 9 5.13 4.97 -11 -1 9 4.96 6.18 -11 1 10 86.09 18.91 -11 -1 10 42.91 12.10 -11 1 11 -0.21 7.99 -11 -1 11 19.32 9.91 -11 1 12 28.46 10.49 -11 -1 12 16.13 5.06 -11 1 13 55.05 15.81 -11 -1 13 18.02 10.74 -11 1 14 49.76 13.92 -11 -1 14 21.45 10.64 -11 1 15 15.62 5.04 -11 -1 15 14.12 10.62 -11 1 16 61.00 16.29 -11 -1 16 34.55 8.43 -11 1 17 13.20 11.72 -11 -1 17 -8.58 11.04 -11 2 4 17.50 7.39 -11 2 5 23.44 9.45 -11 2 6 -9.70 10.49 -11 2 7 5.02 5.30 -11 2 8 7.43 9.12 -11 2 9 52.74 16.32 -11 2 10 38.74 11.21 -11 2 11 86.17 20.14 -11 2 12 16.29 7.66 -11 2 13 33.03 10.89 -11 2 14 -2.32 9.38 -11 2 15 8.96 7.09 -11 2 16 -1.18 9.31 -11 3 5 74.52 16.86 -11 3 6 15.19 9.27 -11 3 7 8.15 7.32 -11 3 8 8.56 4.53 -11 3 9 20.30 11.24 -11 3 10 38.56 11.36 -11 3 11 7.74 6.18 -11 3 12 -1.12 4.85 -11 3 13 44.44 12.71 -11 3 14 2.28 5.42 -11 3 15 15.61 10.69 -11 3 16 10.85 11.76 -11 4 5 0.87 5.32 -11 4 6 0.18 7.40 -11 4 7 -1.61 5.32 -11 4 8 32.75 12.42 -11 4 9 9.51 4.79 -11 4 10 97.25 20.01 -11 4 11 -4.20 10.21 -11 4 12 2.56 4.47 -11 4 13 56.32 16.13 -11 4 14 -0.65 4.64 -11 4 15 23.73 14.35 -11 5 6 51.23 14.90 -11 5 7 0.34 7.17 -11 5 8 19.25 10.60 -11 5 9 6.80 7.86 -11 5 10 5.83 7.36 -11 5 11 22.55 8.95 -11 5 12 29.30 11.43 -11 5 13 -6.23 7.27 -11 5 14 42.02 13.63 -11 6 6 -2.68 4.95 -11 6 7 -6.31 5.57 -11 6 8 2.88 7.58 -11 6 9 57.22 15.42 -11 6 10 31.23 11.65 -11 6 11 1.08 4.49 -11 6 12 146.82 24.08 -11 7 7 -0.03 6.30 -11 7 8 5.33 3.70 -11 7 9 5.89 7.96 -11 7 10 -6.18 8.93 -12 0 6 26.52 14.52 -12 0 7 -0.46 5.40 -12 0 8 157.93 26.56 -12 0 9 3.58 5.29 -12 0 10 241.79 31.52 -12 0 11 -3.99 9.63 -12 0 12 32.70 12.59 -12 1 6 14.61 12.49 -12 1 7 -1.08 6.44 -12 1 8 0.80 6.17 -12 1 9 17.28 11.60 -12 1 10 18.88 9.76 -12 1 11 17.24 6.77 -12 1 12 19.11 12.31 -12 2 6 34.47 12.51 -12 2 7 135.12 24.07 -12 2 8 34.45 11.18 -12 2 9 31.74 12.72 -12 2 10 26.62 12.14 -12 2 11 104.76 21.01 -12 3 6 42.10 15.33 -12 3 7 -1.78 6.74 -12 3 8 111.70 21.94 -12 3 9 -0.63 5.58 -12 3 10 13.03 6.42 -12 3 11 32.28 15.95 -12 4 7 125.26 23.51 -12 4 8 106.16 21.88 -12 4 9 87.91 19.89 -12 5 7 3.29 3.76 0 0 0 0.00 0.00 TITL 044_180K_SulfamerazineF2_ in Pbca REM Pbca (#61 in standard setting) CELL 0.68890 9.097248 11.575065 22.853058 90.0000 90.0000 90.0000 ZERR 8.00 0.000239 0.000184 0.000306 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 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 63056