data_220k_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 9.1158(2) _cell_length_b 11.6222(2) _cell_length_c 22.8715(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2423.14(7) _cell_formula_units_Z 8 _cell_measurement_temperature 220 _cell_measurement_reflns_used 8200 _cell_measurement_theta_min 1.7270 _cell_measurement_theta_max 29.5650 _exptl_crystal_description Parallelepiped _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.449 _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 0.948 _exptl_absorpt_correction_T_min 0.94486 _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 220 _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 21617 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _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 1.726 _diffrn_reflns_theta_max 29.476 _diffrn_reflns_theta_full 24.415 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_point_group_measured_fraction_full 0.990 _reflns_number_total 3595 _reflns_number_gt 2629 _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 3595 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 0.33209(5) 0.34620(4) 0.38972(2) 0.02865(13) Uani 1 1 d . . . . . O2 O 0.19738(15) 0.39699(12) 0.40957(6) 0.0357(3) Uani 1 1 d . . . . . O1 O 0.34214(17) 0.22362(11) 0.38644(6) 0.0383(3) Uani 1 1 d . . . . . N4 N 0.66666(18) 0.42625(14) 0.48542(7) 0.0329(4) Uani 1 1 d . . . . . N3 N 0.65589(19) 0.28520(13) 0.40897(7) 0.0330(4) Uani 1 1 d . . . . . N2 N 0.45152(19) 0.39501(13) 0.43744(7) 0.0314(4) Uani 1 1 d . . . . . N1 N 0.4553(2) 0.53266(18) 0.15487(8) 0.0462(5) Uani 1 1 d . . . . . C1 C 0.3756(2) 0.40401(15) 0.32165(7) 0.0298(4) Uani 1 1 d . . . . . C2 C 0.4479(2) 0.33725(17) 0.28026(8) 0.0388(5) Uani 1 1 d . . . . . H2 H 0.4766 0.2626 0.2894 0.050 Uiso 1 1 calc R U . . . C3 C 0.4770(3) 0.38180(17) 0.22567(9) 0.0404(5) Uani 1 1 d . . . . . H3 H 0.5275 0.3373 0.1985 0.052 Uiso 1 1 calc R U . . . C4 C 0.4319(2) 0.49297(16) 0.21032(8) 0.0344(4) Uani 1 1 d . . . . . C5 C 0.3591(2) 0.55928(15) 0.25288(9) 0.0362(4) Uani 1 1 d . . . . . H5 H 0.3288 0.6336 0.2438 0.047 Uiso 1 1 calc R U . . . C6 C 0.3322(2) 0.51552(15) 0.30777(8) 0.0325(4) Uani 1 1 d . . . . . H6 H 0.2849 0.5605 0.3356 0.042 Uiso 1 1 calc R U . . . C7 C 0.5980(2) 0.36603(14) 0.44333(7) 0.0282(4) Uani 1 1 d . . . . . C8 C 0.8082(2) 0.40071(18) 0.49300(9) 0.0374(4) Uani 1 1 d . . . . . H8 H 0.8606 0.4398 0.5217 0.049 Uiso 1 1 calc R U . . . C9 C 0.8796(2) 0.31939(18) 0.46027(9) 0.0385(5) Uani 1 1 d . . . . . H9 H 0.9785 0.3036 0.4661 0.050 Uiso 1 1 calc R U . . . C10 C 0.7988(2) 0.26156(16) 0.41814(8) 0.0354(4) Uani 1 1 d . . . . . C11 C 0.8662(3) 0.1686(2) 0.38154(11) 0.0513(6) Uani 1 1 d . . . . . H11A H 0.8214 0.0962 0.3909 0.067 Uiso 1 1 calc R U . . . H11B H 0.9695 0.1646 0.3893 0.067 Uiso 1 1 calc R U . . . H11C H 0.8508 0.1855 0.3409 0.067 Uiso 1 1 calc R U . . . H1N2 H 0.419(3) 0.448(2) 0.4589(11) 0.049(7) Uiso 1 1 d . . . . . H1N1 H 0.511(3) 0.494(2) 0.1341(12) 0.053(7) Uiso 1 1 d . . . . . H2N1 H 0.449(3) 0.605(2) 0.1477(11) 0.056(7) 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 0.0294(3) 0.0303(2) 0.0262(2) -0.00199(15) -0.00035(17) -0.00357(17) O2 0.0270(8) 0.0493(8) 0.0309(6) -0.0021(6) 0.0004(5) -0.0024(6) O1 0.0508(10) 0.0286(6) 0.0354(7) -0.0013(5) -0.0009(6) -0.0065(6) N4 0.0306(10) 0.0379(8) 0.0301(7) -0.0036(6) -0.0026(6) 0.0022(7) N3 0.0346(10) 0.0323(7) 0.0322(7) -0.0021(6) 0.0031(7) 0.0040(7) N2 0.0291(9) 0.0341(8) 0.0312(7) -0.0089(6) -0.0024(6) 0.0033(7) N1 0.0623(14) 0.0409(10) 0.0355(9) 0.0052(7) 0.0143(9) 0.0031(10) C1 0.0315(11) 0.0305(8) 0.0275(8) -0.0016(6) 0.0022(7) -0.0022(7) C2 0.0479(13) 0.0341(9) 0.0344(9) 0.0005(7) 0.0080(9) 0.0084(9) C3 0.0500(14) 0.0370(10) 0.0341(9) -0.0023(7) 0.0136(9) 0.0071(9) C4 0.0355(12) 0.0354(9) 0.0323(9) -0.0009(7) 0.0040(8) -0.0052(8) C5 0.0431(13) 0.0268(8) 0.0386(9) 0.0014(7) 0.0053(8) -0.0001(8) C6 0.0362(11) 0.0278(8) 0.0335(8) -0.0052(6) 0.0071(8) -0.0018(7) C7 0.0281(10) 0.0299(8) 0.0266(7) 0.0025(6) 0.0015(7) 0.0015(7) C8 0.0300(12) 0.0484(11) 0.0339(9) 0.0015(8) -0.0035(8) 0.0020(9) C9 0.0299(12) 0.0484(11) 0.0373(10) 0.0072(8) 0.0026(8) 0.0067(9) C10 0.0345(12) 0.0356(9) 0.0359(9) 0.0069(7) 0.0080(8) 0.0084(8) C11 0.0491(16) 0.0479(12) 0.0568(14) -0.0041(10) 0.0103(11) 0.0155(11) _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 1.4296(13) . ? S1 O2 1.4361(14) . ? S1 N2 1.6427(16) . ? S1 C1 1.7413(18) . ? N4 C8 1.336(3) . ? N4 C7 1.345(2) . ? N3 C7 1.334(2) . ? N3 C10 1.348(3) . ? N2 C7 1.383(2) . ? N2 H1N2 0.84(3) . ? N1 C4 1.366(2) . ? N1 H1N1 0.83(3) . ? N1 H2N1 0.86(3) . ? C1 C2 1.390(3) . ? C1 C6 1.392(2) . ? C2 C3 1.378(3) . ? C2 H2 0.9300 . ? C3 C4 1.401(3) . ? C3 H3 0.9300 . ? C4 C5 1.408(3) . ? C5 C6 1.377(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C9 1.370(3) . ? C8 H8 0.9300 . ? C9 C10 1.386(3) . ? C9 H9 0.9300 . ? C10 C11 1.498(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 118.75(9) . . ? O1 S1 N2 109.67(8) . . ? O2 S1 N2 102.40(8) . . ? O1 S1 C1 108.84(8) . . ? O2 S1 C1 108.58(9) . . ? N2 S1 C1 108.06(9) . . ? C8 N4 C7 115.28(16) . . ? C7 N3 C10 115.75(17) . . ? C7 N2 S1 128.33(13) . . ? C7 N2 H1N2 117.4(18) . . ? S1 N2 H1N2 114.1(18) . . ? C4 N1 H1N1 116.3(18) . . ? C4 N1 H2N1 120.0(17) . . ? H1N1 N1 H2N1 117(3) . . ? C2 C1 C6 119.94(16) . . ? C2 C1 S1 120.09(14) . . ? C6 C1 S1 119.90(14) . . ? C3 C2 C1 119.92(18) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 121.16(17) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? N1 C4 C3 119.90(18) . . ? N1 C4 C5 122.04(19) . . ? C3 C4 C5 118.04(17) . . ? C6 C5 C4 120.83(17) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C1 120.09(16) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? N3 C7 N4 127.16(18) . . ? N3 C7 N2 119.75(17) . . ? N4 C7 N2 113.09(15) . . ? N4 C8 C9 122.8(2) . . ? N4 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C8 C9 C10 117.5(2) . . ? C8 C9 H9 121.2 . . ? C10 C9 H9 121.2 . . ? N3 C10 C9 121.51(18) . . ? N3 C10 C11 117.1(2) . . ? C9 C10 C11 121.3(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 O1 S1 N2 C7 46.54(18) . . . . ? O2 S1 N2 C7 173.53(16) . . . . ? C1 S1 N2 C7 -71.96(18) . . . . ? O1 S1 C1 C2 -16.7(2) . . . . ? O2 S1 C1 C2 -147.33(17) . . . . ? N2 S1 C1 C2 102.30(18) . . . . ? O1 S1 C1 C6 160.49(16) . . . . ? O2 S1 C1 C6 29.88(19) . . . . ? N2 S1 C1 C6 -80.48(18) . . . . ? C6 C1 C2 C3 0.3(3) . . . . ? S1 C1 C2 C3 177.47(17) . . . . ? C1 C2 C3 C4 -1.5(3) . . . . ? C2 C3 C4 N1 -176.5(2) . . . . ? C2 C3 C4 C5 1.6(3) . . . . ? N1 C4 C5 C6 177.5(2) . . . . ? C3 C4 C5 C6 -0.5(3) . . . . ? C4 C5 C6 C1 -0.7(3) . . . . ? C2 C1 C6 C5 0.8(3) . . . . ? S1 C1 C6 C5 -176.37(16) . . . . ? C10 N3 C7 N4 0.5(3) . . . . ? C10 N3 C7 N2 -179.29(16) . . . . ? C8 N4 C7 N3 -0.2(3) . . . . ? C8 N4 C7 N2 179.59(16) . . . . ? S1 N2 C7 N3 -3.2(3) . . . . ? S1 N2 C7 N4 177.06(13) . . . . ? C7 N4 C8 C9 0.3(3) . . . . ? N4 C8 C9 C10 -0.6(3) . . . . ? C7 N3 C10 C9 -0.8(3) . . . . ? C7 N3 C10 C11 178.18(17) . . . . ? C8 C9 C10 N3 0.9(3) . . . . ? C8 C9 C10 C11 -178.0(2) . . . . ? 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 2.51 3.408(2) 163.1 8_665 C8 H8 O2 0.93 2.52 3.240(2) 134.5 5_666 C9 H9 O2 0.93 2.61 3.248(3) 126.0 1_655 N2 H1N2 N4 0.84(3) 2.09(3) 2.931(2) 177(2) 5_666 N1 H1N1 O2 0.83(3) 2.27(3) 3.087(3) 169(3) 6_656 N1 H2N1 O1 0.86(3) 2.47(3) 3.038(2) 124(2) 3_655 N1 H2N1 N3 0.86(3) 2.64(3) 3.431(3) 153(2) 3_655 _refine_diff_density_max 0.366 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.058 _shelx_res_file ; 220k_smz-f2_a.res created by SHELXL-2014/7 TITL 220k_smz-f2_a.res in Pbca REM Old TITL 038_220K_SulfamerazineF2_ in Pbca REM SHELXT solution in Pbca REM R1 0.113, Rweak 0.246, Alpha 0.020, Orientation as input REM Formula found by SHELXT: C12 N3 O2 S CELL 0.68890 9.1158 11.6222 22.8715 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 0.54405 S1 5 0.332088 0.346204 0.389720 11.00000 0.02942 0.03030 = 0.02622 -0.00199 -0.00035 -0.00357 O2 4 0.197377 0.396989 0.409571 11.00000 0.02698 0.04929 = 0.03093 -0.00209 0.00038 -0.00242 O1 4 0.342140 0.223618 0.386438 11.00000 0.05076 0.02861 = 0.03540 -0.00132 -0.00087 -0.00650 N4 3 0.666660 0.426253 0.485424 11.00000 0.03062 0.03787 = 0.03008 -0.00356 -0.00265 0.00216 N3 3 0.655891 0.285201 0.408968 11.00000 0.03456 0.03231 = 0.03221 -0.00214 0.00311 0.00396 N2 3 0.451525 0.395010 0.437441 11.00000 0.02914 0.03405 = 0.03115 -0.00892 -0.00238 0.00333 N1 3 0.455262 0.532662 0.154874 11.00000 0.06225 0.04091 = 0.03547 0.00520 0.01432 0.00315 C1 1 0.375557 0.404006 0.321648 11.00000 0.03146 0.03050 = 0.02748 -0.00157 0.00223 -0.00223 C2 1 0.447890 0.337252 0.280260 11.00000 0.04791 0.03406 = 0.03437 0.00049 0.00797 0.00841 AFIX 43 H2 2 0.476587 0.262609 0.289421 11.00000 -1.30000 AFIX 0 C3 1 0.477008 0.381797 0.225666 11.00000 0.04998 0.03702 = 0.03415 -0.00233 0.01357 0.00709 AFIX 43 H3 2 0.527489 0.337271 0.198525 11.00000 -1.30000 AFIX 0 C4 1 0.431919 0.492974 0.210317 11.00000 0.03554 0.03538 = 0.03235 -0.00089 0.00398 -0.00518 C5 1 0.359101 0.559278 0.252875 11.00000 0.04314 0.02684 = 0.03865 0.00139 0.00534 -0.00011 AFIX 43 H5 2 0.328808 0.633568 0.243792 11.00000 -1.30000 AFIX 0 C6 1 0.332176 0.515522 0.307768 11.00000 0.03623 0.02776 = 0.03349 -0.00517 0.00707 -0.00180 AFIX 43 H6 2 0.284933 0.560543 0.335615 11.00000 -1.30000 AFIX 0 C7 1 0.597968 0.366033 0.443326 11.00000 0.02807 0.02985 = 0.02657 0.00252 0.00151 0.00154 C8 1 0.808236 0.400710 0.493001 11.00000 0.02999 0.04837 = 0.03392 0.00150 -0.00348 0.00200 AFIX 43 H8 2 0.860591 0.439773 0.521705 11.00000 -1.30000 AFIX 0 C9 1 0.879573 0.319387 0.460269 11.00000 0.02992 0.04841 = 0.03728 0.00720 0.00258 0.00673 AFIX 43 H9 2 0.978505 0.303557 0.466089 11.00000 -1.30000 AFIX 0 C10 1 0.798805 0.261564 0.418143 11.00000 0.03455 0.03562 = 0.03592 0.00694 0.00803 0.00838 C11 1 0.866171 0.168634 0.381542 11.00000 0.04914 0.04786 = 0.05681 -0.00410 0.01027 0.01554 AFIX 137 H11A 2 0.821392 0.096182 0.390911 11.00000 -1.30000 H11B 2 0.969522 0.164634 0.389343 11.00000 -1.30000 H11C 2 0.850767 0.185536 0.340918 11.00000 -1.30000 AFIX 0 H1N2 2 0.419289 0.447883 0.458863 11.00000 0.04934 H1N1 2 0.510775 0.493853 0.134128 11.00000 0.05306 H2N1 2 0.449461 0.605001 0.147655 11.00000 0.05566 HKLF 4 REM 220k_smz-f2_a.res in Pbca REM R1 = 0.0459 for 2629 Fo > 4sig(Fo) and 0.0691 for all 3595 data REM 176 parameters refined using 0 restraints END WGHT 0.0431 0.9966 REM Highest difference peak 0.366, deepest hole -0.324, 1-sigma level 0.058 Q1 1 0.3669 0.3775 0.3512 11.00000 0.05 0.37 Q2 1 0.3748 0.4578 0.3165 11.00000 0.05 0.31 Q3 1 0.3869 0.3631 0.3042 11.00000 0.05 0.27 Q4 1 0.8455 0.3785 0.4619 11.00000 0.05 0.27 Q5 1 0.3992 0.5287 0.2345 11.00000 0.05 0.26 Q6 1 0.3478 0.5212 0.2771 11.00000 0.05 0.26 Q7 1 0.4232 0.3744 0.4119 11.00000 0.05 0.23 Q8 1 0.6616 0.4018 0.4596 11.00000 0.05 0.23 Q9 1 0.4580 0.5173 0.1894 11.00000 0.05 0.22 Q10 1 0.7791 0.0808 0.3516 11.00000 0.05 0.20 Q11 1 0.5979 0.4576 0.5023 11.00000 0.05 0.20 Q12 1 0.6089 0.2660 0.3828 11.00000 0.05 0.20 Q13 1 0.8494 0.3000 0.4311 11.00000 0.05 0.20 Q14 1 0.1646 0.4822 0.2602 11.00000 0.05 0.20 Q15 1 0.3415 0.1800 0.3685 11.00000 0.05 0.19 Q16 1 0.3566 0.2005 0.3606 11.00000 0.05 0.19 Q17 1 0.6631 0.3588 0.2084 11.00000 0.05 0.19 Q18 1 0.2451 0.3852 0.3984 11.00000 0.05 0.19 Q19 1 0.5917 0.3478 0.2100 11.00000 0.05 0.19 Q20 1 0.6164 0.3037 0.4293 11.00000 0.05 0.19 Q21 1 0.4588 0.3419 0.4924 11.00000 0.05 0.19 Q22 1 0.3716 0.1997 0.3954 11.00000 0.05 0.19 Q23 1 0.8561 0.4821 0.5191 11.00000 0.05 0.18 Q24 1 0.2186 0.3427 0.4111 11.00000 0.05 0.18 Q25 1 0.3907 0.3443 0.2377 11.00000 0.05 0.18 Q26 1 0.6474 0.3533 0.4173 11.00000 0.05 0.18 Q27 1 0.5972 0.5580 0.2515 11.00000 0.05 0.18 Q28 1 0.1779 0.4711 0.3989 11.00000 0.05 0.18 Q29 1 0.3381 0.1582 0.3279 11.00000 0.05 0.18 Q30 1 0.1496 0.3975 0.4118 11.00000 0.05 0.18 Q31 1 0.4323 0.4247 0.2170 11.00000 0.05 0.18 Q32 1 0.3150 0.2625 0.3671 11.00000 0.05 0.17 ; _shelx_res_checksum 45310 _shelx_hkl_file ; 0 0 2 663.59 13.11 0 0 2 535.06 11.64 0 0 3 1.13 1.10 0 0 3 1.04 1.27 0 0 4 2867.91 38.81 0 0 4 2850.21 38.09 0 0 5 -0.74 1.14 0 0 5 0.13 0.54 0 0 6 7347.62 74.62 0 0 6 7301.37 76.40 0 0 7 6.60 3.13 0 0 7 1.92 2.41 0 0 8 1045.37 32.30 0 0 8 1115.19 34.27 0 0 9 4.07 3.84 0 0 9 -0.13 0.95 0 0 10 5223.32 80.44 0 0 10 5544.62 85.06 0 0 11 0.51 3.58 0 0 11 0.51 3.05 0 0 12 -2.14 3.90 0 0 12 -0.61 1.62 0 0 13 0.05 1.88 0 0 13 -1.86 2.73 0 0 14 727.76 36.84 0 0 14 751.78 35.61 0 0 15 1.09 1.89 0 0 15 1.53 2.74 0 0 16 18.92 6.64 0 0 16 14.57 5.90 0 0 17 0.34 1.48 0 0 17 -1.20 2.44 0 0 18 1323.45 54.54 0 0 18 1397.43 56.83 0 0 19 8.53 7.17 0 0 19 -2.46 2.60 0 0 20 140.24 19.38 0 0 20 95.15 15.56 0 0 21 9.00 4.51 0 0 21 5.04 7.21 0 0 22 193.08 23.21 0 0 22 188.85 22.37 0 0 23 -1.12 4.76 0 0 23 1.81 4.97 0 0 24 75.81 14.59 0 0 24 82.05 15.50 0 0 25 -2.18 2.70 0 0 25 -2.29 3.96 0 0 26 64.87 14.34 0 0 26 49.33 12.50 0 0 27 2.41 3.58 0 0 27 6.48 4.37 0 0 28 73.77 14.86 0 0 28 52.30 14.53 0 0 29 -0.58 1.74 0 0 29 -0.83 2.36 0 0 30 266.32 30.78 0 0 30 267.91 30.64 0 0 31 1.35 6.28 0 0 31 5.07 4.05 0 0 32 -0.03 2.41 0 0 32 -8.76 7.21 0 -1 0 -0.22 0.36 0 -1 0 -0.87 0.70 0 -1 1 -1.60 1.03 0 1 1 0.33 0.84 0 -1 1 0.26 0.52 0 -1 -1 -0.38 0.39 0 -1 2 0.56 0.45 0 1 2 0.53 0.56 0 1 2 0.35 0.96 0 -1 2 0.17 0.70 0 -1 3 -0.69 1.10 0 1 3 -0.46 0.89 0 1 3 0.57 0.49 0 -1 3 0.35 0.96 0 1 4 1.86 1.67 0 -1 4 -1.41 1.60 0 -1 4 0.49 1.52 0 1 4 -0.74 0.99 0 -1 4 0.79 0.86 0 -1 5 0.25 1.20 0 -1 5 -1.66 1.58 0 1 5 -0.42 1.18 0 -1 5 -1.12 1.42 0 1 5 -1.09 0.62 0 -1 6 -1.55 1.08 0 -1 6 0.71 0.84 0 1 6 0.01 1.64 0 1 6 3.07 2.72 0 1 7 -0.51 0.97 0 -1 7 -0.86 0.95 0 1 7 -0.57 1.02 0 -1 7 2.19 1.26 0 1 8 -1.19 1.95 0 -1 8 -0.61 2.04 0 1 8 -1.56 1.09 0 -1 8 0.80 1.56 0 -1 9 1.32 2.88 0 -1 9 3.58 0.94 0 1 9 0.99 2.23 0 1 9 1.89 2.69 0 1 10 -2.85 2.56 0 -1 10 2.06 2.16 0 -1 10 -2.10 2.76 0 1 10 -0.61 1.50 0 1 11 1.66 1.10 0 1 11 -0.90 1.56 0 -1 11 0.26 1.61 0 -1 11 2.47 3.03 0 -1 12 0.95 1.20 0 1 12 4.24 3.36 0 1 12 -0.71 2.29 0 -1 12 4.08 4.87 0 -1 13 1.78 2.11 0 -1 13 0.24 2.80 0 1 13 -0.72 2.08 0 1 13 -2.44 3.53 0 -1 14 -2.02 1.60 0 1 14 -0.30 3.41 0 1 14 -1.73 2.18 0 -1 14 0.90 1.80 0 1 15 -0.04 1.79 0 -1 15 -2.58 1.63 0 1 15 0.24 1.87 0 -1 15 0.69 3.15 0 1 16 8.63 4.93 0 1 16 3.02 2.69 0 -1 16 -2.89 3.72 0 -1 16 -0.89 2.92 0 1 17 -1.15 3.25 0 1 17 -0.85 4.07 0 -1 17 -1.67 4.60 0 -1 17 0.27 3.72 0 1 18 1.44 2.64 0 -1 18 6.83 6.15 0 1 18 -2.48 2.08 0 -1 18 -0.96 2.78 0 1 19 1.07 4.43 0 -1 19 -2.22 2.33 0 1 19 4.72 5.18 0 -1 19 6.57 5.77 0 1 20 -3.11 4.02 0 -1 20 -1.82 2.43 0 1 20 -1.23 4.02 0 -1 20 1.28 1.69 0 1 21 5.33 5.56 0 -1 21 -4.02 6.39 0 -1 21 0.47 3.51 0 1 21 1.74 3.66 0 1 22 0.48 5.92 0 1 22 -3.23 3.46 0 -1 22 4.24 6.99 0 -1 22 1.50 2.11 0 -1 23 -0.71 3.09 0 -1 23 1.03 5.11 0 1 23 -4.19 3.78 0 1 23 -1.87 3.86 0 -1 24 -0.22 4.05 0 1 24 3.70 5.15 0 1 24 3.19 3.42 0 -1 24 0.53 3.46 0 -1 25 5.56 7.76 0 1 25 10.65 5.88 0 1 25 2.36 2.80 0 -1 25 -3.79 5.23 0 1 26 0.57 3.11 0 -1 26 3.19 5.27 0 -1 26 5.90 5.82 0 1 26 7.01 7.49 0 1 27 7.69 6.12 0 -1 27 0.97 6.17 0 1 27 -5.25 6.77 0 -1 27 -2.19 6.22 0 -1 28 -1.51 4.42 0 1 28 6.69 8.25 0 1 28 -7.31 6.73 0 -1 28 -3.71 5.81 0 1 29 2.78 1.90 0 -1 29 -3.64 3.40 0 1 29 -5.50 7.39 0 -1 29 2.53 2.61 0 1 30 -3.59 4.17 0 1 30 3.64 6.78 0 -1 30 -0.60 3.27 0 -1 30 5.65 6.45 0 -1 31 0.68 4.37 0 -1 31 6.45 5.89 0 1 31 1.52 2.02 0 1 31 1.74 8.07 0 1 32 10.92 11.29 0 -1 32 -1.09 2.78 0 1 32 3.29 2.66 0 -1 32 2.04 6.88 0 -2 0 5.78 1.98 0 -2 0 4.73 1.34 0 2 1 8107.13 62.40 0 -2 1 7972.18 63.26 0 -2 -1 8077.64 66.08 0 2 2 4068.64 45.63 0 -2 2 4149.90 50.03 0 -2 2 4099.46 45.77 0 -2 -2 4108.73 48.51 0 2 2 4068.94 37.16 0 -2 3 9320.59 72.91 0 -2 -3 9663.10 79.70 0 -2 3 9826.59 79.89 0 2 3 9527.99 75.96 0 2 3 9999.00 64.77 0 -2 4 7817.99 70.82 0 -2 4 7878.74 76.49 0 2 4 7914.38 66.15 0 -2 -4 8033.42 76.95 0 2 4 7854.22 73.06 0 -2 5 7908.91 76.74 0 2 5 7971.18 79.80 0 -2 6 7713.81 80.99 0 -2 6 7800.86 82.42 0 2 6 7870.05 78.23 0 2 6 7742.89 83.04 0 2 7 77.60 8.88 0 -2 7 76.78 9.18 0 2 7 66.75 8.00 0 -2 7 83.75 8.99 0 2 8 522.89 23.92 0 -2 8 480.25 23.27 0 2 8 535.42 23.26 0 -2 8 533.83 24.63 0 -2 8 512.29 24.28 0 -2 9 1841.42 47.59 0 -2 9 1755.46 45.61 0 -2 9 1839.72 48.16 0 2 9 1828.05 45.82 0 2 9 1721.62 45.59 0 2 10 892.65 33.94 0 2 10 923.08 34.77 0 -2 10 830.81 34.01 0 -2 10 876.60 33.87 0 -2 11 1226.56 41.37 0 2 11 1232.74 41.84 0 2 11 1246.10 42.22 0 -2 11 1194.85 42.73 0 -2 12 539.88 29.20 0 -2 12 547.85 29.04 0 2 12 544.28 28.74 0 2 12 536.57 28.97 0 2 13 125.96 14.36 0 -2 13 156.96 16.87 0 2 13 161.89 16.23 0 -2 13 130.31 15.05 0 2 14 733.00 36.05 0 -2 14 746.45 37.63 0 -2 14 701.51 35.71 0 2 14 657.90 34.47 0 -2 15 20.64 5.99 0 2 15 23.45 6.25 0 2 15 29.14 7.70 0 -2 15 23.79 7.56 0 -2 16 55.49 10.78 0 2 16 82.48 13.12 0 2 16 87.89 13.59 0 2 17 499.04 32.97 0 2 17 451.68 30.92 0 -2 17 472.40 32.25 0 -2 17 504.02 33.52 0 -2 18 233.32 23.25 0 2 18 236.66 23.47 0 2 18 228.59 22.79 0 -2 18 251.97 24.87 0 -2 19 693.58 42.13 0 -2 19 685.22 40.04 0 2 19 630.20 37.99 0 2 19 706.90 41.00 0 -2 20 86.04 14.40 0 2 20 81.69 14.78 0 2 20 87.17 14.07 0 -2 20 79.00 13.80 0 2 21 59.52 12.94 0 -2 21 68.17 12.84 0 2 21 51.18 11.19 0 -2 21 70.98 14.15 0 -2 22 2.31 4.49 0 -2 22 2.91 5.11 0 2 22 -1.75 4.00 0 2 22 5.91 6.51 0 -2 23 500.01 37.98 0 2 23 460.63 36.26 0 -2 23 467.11 35.76 0 2 23 479.76 35.99 0 -2 24 5.49 4.46 0 -2 24 0.66 2.21 0 2 24 0.20 3.34 0 -2 25 7.55 5.03 0 2 25 7.52 4.44 0 -2 25 17.48 5.70 0 2 25 5.68 1.72 0 2 26 74.47 15.24 0 -2 26 87.87 16.30 0 2 26 100.67 17.68 0 -2 26 93.21 16.67 0 -2 27 8.28 3.69 0 2 27 19.98 7.93 0 2 27 8.24 4.84 0 -2 27 12.46 7.80 0 2 28 24.20 8.42 0 -2 28 10.61 3.26 0 -2 28 8.82 4.48 0 2 28 21.55 9.21 0 2 29 103.26 18.42 0 -2 29 66.18 13.57 0 -2 29 56.89 14.11 0 2 29 73.88 16.21 0 2 30 -3.81 8.09 0 -2 30 1.35 5.99 0 -2 30 7.53 8.73 0 2 30 5.87 6.53 0 2 31 -1.69 7.85 0 2 31 7.94 6.59 0 -2 31 -0.98 2.72 0 -2 31 -2.80 7.21 0 2 32 65.10 17.09 0 2 32 26.20 10.11 0 -2 32 25.37 10.94 0 -2 32 38.00 11.58 0 -3 0 0.29 1.40 0 -3 0 3.61 2.07 0 -3 1 -0.48 1.31 0 3 1 1.72 1.22 0 -3 1 -0.26 1.30 0 -3 -1 3.27 3.03 0 3 2 0.97 1.88 0 -3 -2 1.35 1.34 0 -3 2 -0.43 0.72 0 3 2 -1.35 1.40 0 -3 2 1.98 2.07 0 -3 -3 0.98 1.69 0 3 3 0.38 1.10 0 3 3 -1.20 1.05 0 -3 3 2.91 2.49 0 -3 3 -0.25 1.67 0 -3 -4 -1.83 1.00 0 3 4 0.42 1.41 0 3 4 -0.08 1.19 0 -3 4 0.60 2.45 0 -3 4 -1.00 0.99 0 3 5 -1.57 1.33 0 -3 -5 -0.69 1.78 0 -3 5 -0.53 1.43 0 -3 5 0.06 2.03 0 3 5 -1.60 2.53 0 -3 6 0.22 2.28 0 -3 6 -0.04 1.58 0 3 6 0.95 2.04 0 -3 -6 -0.89 2.26 0 3 6 1.61 1.34 0 3 7 -0.39 0.84 0 3 7 1.18 1.87 0 -3 7 -1.91 1.42 0 -3 7 -0.95 1.46 0 3 8 0.38 2.20 0 -3 8 0.14 1.43 0 -3 8 0.62 1.23 0 -3 8 -1.61 2.32 0 3 8 -0.43 2.63 0 -3 9 3.51 3.41 0 -3 9 0.75 3.25 0 3 9 1.19 1.89 0 -3 9 2.50 3.33 0 3 9 -1.64 1.95 0 -3 10 -1.53 1.82 0 3 10 -0.87 2.21 0 -3 10 0.87 3.79 0 3 10 0.54 2.24 0 -3 10 0.53 3.29 0 -3 11 0.09 3.02 0 -3 11 1.28 2.93 0 -3 11 0.07 3.26 0 3 11 1.98 3.65 0 3 11 6.30 4.42 0 3 12 1.25 1.63 0 3 12 1.50 1.75 0 -3 12 1.86 2.77 0 -3 12 -1.85 2.67 0 -3 12 0.12 1.85 0 3 13 0.49 1.41 0 -3 13 1.50 1.75 0 3 13 -0.87 2.12 0 -3 13 -2.03 1.70 0 -3 14 4.30 3.38 0 3 14 1.59 3.05 0 3 14 -3.56 2.35 0 -3 14 -2.06 1.85 0 3 15 -0.94 4.00 0 -3 15 -0.80 1.27 0 3 15 1.50 3.94 0 -3 15 -2.06 1.71 0 -3 16 2.54 3.18 0 3 16 0.27 3.81 0 3 16 -1.12 3.07 0 -3 16 1.13 3.61 0 3 17 4.03 4.90 0 -3 17 0.85 2.11 0 -3 17 -0.05 2.26 0 3 17 3.49 6.47 0 3 18 0.19 3.95 0 3 18 0.91 3.89 0 -3 18 -0.19 1.95 0 -3 18 2.83 2.25 0 3 19 2.61 4.22 0 3 19 3.04 4.57 0 -3 19 5.46 6.38 0 -3 19 -0.32 3.05 0 -3 20 -1.11 3.73 0 -3 20 -2.33 4.60 0 3 20 1.53 3.80 0 3 20 1.82 4.20 0 3 21 1.95 3.30 0 -3 21 -0.55 2.09 0 -3 21 -0.02 2.31 0 3 21 4.07 2.90 0 -3 22 -2.03 2.83 0 3 22 3.50 6.31 0 3 22 0.11 3.57 0 -3 22 -0.15 3.44 0 3 23 4.55 7.66 0 -3 23 -0.83 1.81 0 3 23 6.40 7.10 0 -3 23 2.28 3.16 0 -3 24 0.34 2.00 0 3 24 1.74 3.82 0 3 24 1.72 7.51 0 -3 24 3.39 3.39 0 3 25 8.93 5.53 0 3 25 -2.00 5.73 0 -3 25 -1.09 3.59 0 -3 25 -3.03 5.22 0 -3 26 -3.17 5.77 0 3 26 -4.70 5.13 0 -3 26 -4.83 7.50 0 3 26 3.73 4.76 0 3 27 1.19 4.98 0 -3 27 -0.65 2.79 0 -3 27 -2.51 8.01 0 3 27 3.20 7.43 0 3 28 2.18 5.77 0 -3 28 -4.57 6.59 0 3 28 1.28 3.37 0 -3 28 -6.61 7.09 0 -3 29 0.43 3.65 0 3 29 0.08 4.44 0 3 29 3.11 5.28 0 -3 29 9.93 9.79 0 3 30 1.43 4.24 0 -3 30 -2.66 4.60 0 3 30 -2.29 5.65 0 -3 30 -5.73 7.72 0 -3 31 9.46 6.80 0 3 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9 82.40 12.97 -2 7 9 106.42 14.44 -2 -7 9 105.87 13.01 -2 -7 -9 115.98 15.16 -2 7 9 117.42 15.79 2 -7 -9 106.49 15.46 -2 -7 9 76.92 13.39 2 7 9 100.59 14.35 -2 -7 9 109.68 13.73 2 7 9 95.97 10.66 2 -7 9 107.18 14.31 -2 -7 10 55.55 9.89 -2 -7 10 54.73 11.78 -2 -7 -10 71.55 12.78 2 -7 10 67.60 11.45 2 -7 -10 75.77 13.49 -2 7 10 63.67 11.40 2 7 10 61.08 7.97 -2 7 10 74.05 12.36 2 7 10 71.36 11.58 -2 -7 10 55.30 9.57 2 -7 10 50.73 10.53 2 -7 11 1964.71 66.21 -2 -7 11 2137.72 64.83 -2 -7 11 1988.49 67.79 -2 -7 -11 1988.20 67.44 -2 7 11 1996.58 64.03 2 -7 -11 2015.94 67.02 -2 -7 11 2029.26 60.84 2 7 11 1922.49 52.04 -2 7 11 2037.66 66.31 2 -7 11 2047.93 66.16 2 7 11 1817.42 61.78 -2 7 12 428.50 30.44 2 -7 12 359.58 28.89 2 -7 -12 351.38 29.17 -2 -7 -12 430.83 31.21 -2 7 12 356.44 26.64 -2 -7 12 370.29 26.45 -2 -7 12 362.30 27.10 2 7 12 387.16 28.94 2 -7 12 401.77 29.40 -2 -7 12 393.10 29.87 2 7 12 386.19 24.01 2 -7 13 150.96 18.73 -2 -7 13 111.05 17.15 -2 -7 -13 140.51 18.32 2 -7 -13 126.11 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5 15 14.71 8.67 10 -5 15 2.44 5.23 -10 5 16 -5.96 6.12 10 -5 16 -0.46 5.22 -10 5 17 -5.10 6.62 10 -5 17 11.30 9.65 -10 5 18 35.83 11.60 10 -5 18 37.31 12.06 10 -6 0 88.33 16.53 10 -6 1 -10.54 7.02 10 -6 2 12.42 6.56 10 -6 3 -4.46 3.90 10 -6 4 51.19 13.93 10 -6 5 10.58 4.72 -10 6 5 13.14 8.37 10 -6 6 3.17 5.17 -10 6 6 4.84 5.59 10 -6 7 16.28 6.66 -10 6 7 4.36 8.28 10 -6 8 25.27 9.53 -10 6 8 14.65 5.25 10 -6 9 22.46 8.80 -10 6 9 6.45 8.67 -10 6 10 122.19 21.15 10 -6 10 97.98 18.01 10 -6 11 -1.31 5.45 -10 6 11 -10.20 4.53 10 -6 12 1.21 5.49 -10 6 12 3.00 6.05 10 -6 13 4.71 8.17 -10 6 13 5.50 2.29 10 -6 14 0.28 5.69 -10 6 14 5.93 8.75 -10 6 15 29.40 12.96 10 -6 15 -0.23 6.28 -10 6 16 25.44 12.96 10 -6 16 8.93 6.72 -10 6 17 -0.44 6.26 10 -6 17 0.65 5.64 10 -7 0 14.56 9.02 10 -7 1 110.00 17.95 10 -7 -1 121.42 20.76 10 -7 2 20.55 6.43 10 -7 -2 22.73 8.27 10 -7 -3 83.77 16.21 10 -7 3 56.53 13.74 10 -7 -4 1.96 5.44 10 -7 4 11.61 7.15 10 -7 5 -3.75 2.48 10 -7 6 12.22 7.60 -10 7 6 3.28 4.17 10 -7 7 35.69 11.79 -10 7 7 51.48 13.87 10 -7 8 -5.62 4.48 -10 7 8 5.21 7.46 10 -7 9 4.14 6.20 -10 7 9 -2.92 5.47 10 -7 10 13.61 7.80 -10 7 10 5.94 6.49 -10 7 11 151.49 25.12 10 -7 11 135.20 21.94 10 -7 12 14.05 6.46 -10 7 12 -2.86 5.00 10 -7 13 35.51 11.79 -10 7 13 40.69 13.59 10 -7 14 8.92 6.98 -10 7 14 5.23 7.82 10 -7 15 38.71 11.58 -10 7 15 39.61 10.53 10 -8 0 37.70 10.54 10 -8 1 5.10 4.36 10 -8 -1 4.86 5.79 10 -8 -2 16.17 6.00 10 -8 2 5.28 4.65 10 -8 -3 8.74 7.21 10 -8 3 6.19 3.68 10 -8 -4 4.40 2.45 10 -8 4 1.15 5.28 10 -8 -5 0.69 4.79 10 -8 5 5.25 4.65 10 -8 -6 36.81 13.53 10 -8 6 43.10 11.92 -10 8 6 35.56 12.94 10 -8 7 77.64 16.56 -10 8 7 69.74 15.35 10 -8 8 -2.26 5.67 -10 8 8 -5.63 10.46 10 -8 9 7.96 5.55 -10 8 9 6.27 6.33 10 -8 10 -2.82 4.05 -10 8 10 0.82 5.40 10 -8 11 45.99 13.38 -10 8 11 37.77 14.51 10 -8 12 28.67 9.28 -10 8 12 53.70 16.14 10 -8 13 16.01 8.78 -10 8 13 24.41 10.73 10 -9 0 54.50 14.30 10 -9 1 1.90 4.19 10 -9 -1 18.94 7.17 10 -9 -2 17.07 9.64 10 -9 2 14.09 5.80 10 -9 -3 45.04 13.55 10 -9 3 45.45 12.70 10 -9 -4 35.23 11.35 10 -9 4 74.07 16.43 10 -9 -5 10.43 6.01 10 -9 5 23.65 10.18 10 -9 -6 -1.99 4.56 10 -9 6 -2.82 2.93 10 -9 7 95.49 18.53 10 -9 -7 94.39 19.18 10 -9 8 22.32 7.96 -10 9 8 27.23 10.12 10 -9 -8 9.44 8.63 10 -9 9 3.65 3.60 10 -9 -9 -9.45 9.75 10 -9 10 -6.06 7.69 -10 9 10 11.74 9.09 10 -9 11 -6.93 6.22 -10 9 11 18.48 9.46 10 -10 0 -3.74 6.29 10 -10 1 19.95 9.10 10 -10 -1 -0.55 2.60 10 -10 -2 8.14 7.60 10 -10 2 7.83 4.12 10 -10 -3 25.35 11.66 10 -10 3 12.22 8.73 10 -10 -4 4.35 5.21 10 -10 4 6.36 5.11 10 -10 -5 4.75 2.92 10 -10 5 6.90 7.78 10 -10 -6 -2.56 5.36 10 -10 6 4.69 2.25 10 -10 -7 12.90 10.34 10 -10 7 3.38 4.39 -11 0 4 47.07 13.10 -11 0 5 -2.59 4.55 -11 0 6 28.45 11.95 -11 0 7 -5.42 6.25 -11 0 8 18.51 10.51 -11 0 9 -6.34 7.40 -11 0 10 49.55 13.39 -11 0 11 -6.86 5.46 -11 0 12 -6.96 8.25 -11 0 13 -3.82 6.02 -11 0 14 64.97 16.00 -11 0 15 5.07 3.42 -11 0 16 125.12 22.39 -11 0 17 7.35 5.88 -11 1 4 23.47 8.50 -11 -1 5 3.50 7.05 -11 1 5 16.90 8.48 -11 -1 6 40.19 12.59 -11 1 6 29.39 10.96 -11 1 7 -7.81 6.35 -11 -1 7 -5.70 8.58 -11 1 8 7.83 8.95 -11 -1 8 -0.90 3.58 -11 1 9 -2.25 4.24 -11 -1 9 2.97 3.43 -11 1 10 43.78 14.46 -11 -1 10 39.50 14.67 -11 1 11 4.19 4.00 -11 -1 11 9.94 8.48 -11 1 12 22.21 11.66 -11 -1 12 18.20 9.36 -11 1 13 12.44 6.32 -11 -1 13 46.51 14.42 -11 1 14 28.61 10.96 -11 -1 14 11.44 5.85 -11 1 15 0.85 4.52 -11 -1 15 15.41 11.18 -11 1 16 35.52 12.53 -11 -1 16 21.55 11.53 -11 1 17 2.96 6.69 -11 -1 17 3.91 5.46 -11 2 4 7.47 3.43 -11 2 5 18.89 8.32 -11 2 6 9.01 7.98 -11 2 7 3.09 6.94 -11 2 8 15.51 9.65 -11 2 9 39.96 13.33 -11 2 10 40.01 12.36 -11 2 11 51.92 14.29 -11 2 12 9.02 5.69 -11 2 13 18.77 9.68 -11 2 14 -0.78 6.42 -11 2 15 1.21 2.83 -11 2 16 -8.97 6.97 -11 2 17 54.02 15.60 -11 3 5 79.32 17.99 -11 3 6 -0.99 4.73 -11 3 7 13.09 10.01 -11 3 8 2.48 5.62 -11 3 9 11.15 8.68 -11 3 10 22.91 10.88 -11 3 11 3.88 6.93 -11 3 12 14.47 6.75 -11 3 13 60.04 14.47 -11 3 14 4.43 5.24 -11 3 15 12.71 3.12 -11 3 16 10.26 8.07 -11 4 5 0.20 3.42 -11 4 6 4.03 8.93 -11 4 7 -1.85 7.68 -11 4 8 14.98 9.30 -11 4 9 12.31 7.76 -11 4 10 75.11 16.79 -11 4 11 16.01 10.54 -11 4 12 7.16 9.21 -11 4 13 22.38 10.21 -11 4 14 2.80 3.58 -11 4 15 11.53 10.10 -11 5 6 39.48 12.65 -11 5 7 -1.34 2.99 -11 5 8 3.05 6.58 -11 5 9 7.22 4.36 -11 5 10 1.42 6.24 -11 5 11 20.58 10.80 -11 5 12 14.60 9.42 -11 5 13 5.67 6.89 -11 5 14 17.63 8.85 -11 6 6 16.03 9.92 -11 6 7 6.05 6.92 -11 6 8 9.18 10.72 -11 6 9 50.07 15.61 -11 6 10 11.96 9.93 -11 6 11 -1.07 2.78 -11 6 12 46.61 13.12 -11 7 7 10.82 9.05 -11 7 8 2.92 4.38 -11 7 9 3.74 5.17 -11 7 10 5.73 6.35 11 -8 7 -9.31 9.11 -12 0 6 -7.66 9.44 -12 0 7 2.85 9.81 -12 0 8 82.90 18.39 -12 0 9 -7.52 9.16 -12 0 10 105.77 20.99 -12 0 11 -10.57 8.27 -12 0 12 29.79 12.22 -12 1 6 6.32 6.50 -12 1 7 -1.20 8.18 -12 1 8 6.82 7.04 -12 1 9 10.16 9.26 -12 1 10 21.63 11.58 -12 1 11 19.11 8.89 -12 1 12 16.43 9.17 -12 2 6 5.15 5.43 -12 2 7 129.28 22.27 -12 2 8 -0.06 4.59 -12 2 9 19.68 8.79 -12 2 10 8.19 8.29 -12 2 11 79.36 17.60 -12 2 12 0.60 5.02 -12 3 6 33.06 11.71 -12 3 7 1.00 5.42 -12 3 8 57.80 14.98 -12 3 9 -0.35 3.79 -12 3 10 3.38 3.55 -12 3 11 14.96 8.23 -12 4 7 49.30 15.01 -12 4 8 43.68 13.65 -12 4 9 53.85 15.83 -12 5 7 9.98 6.04 -12 5 8 4.29 8.54 0 0 0 0.00 0.00 TITL 038_220K_SulfamerazineF2_ in Pbca REM Pbca (#61 in standard setting) CELL 0.68890 9.115816 11.622157 22.871549 90.0000 90.0000 90.0000 ZERR 8.00 0.000207 0.000181 0.000316 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 40728