#============================================================================= data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 14 _journal_issue 1 _journal_year 2023 _journal_page_first 9 _journal_page_last 15 #============================================================================= data_e0381_A2 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ; 2-Phenylaminotetrahydro-1,3-thiazepine hydrochloride monohydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C11 H15 N2 S, Cl, H2 O' _chemical_formula_sum 'C11 H17 Cl N2 O S' _chemical_formula_weight 260.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _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' _cell_length_a 4.97183(14) _cell_length_b 15.1169(4) _cell_length_c 17.7376(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1333.14(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4488 _cell_measurement_theta_min 3.8560 _cell_measurement_theta_max 75.5960 _exptl_crystal_description prism _exptl_crystal_colour colouress _exptl_crystal_density_meas none _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.299 _exptl_crystal_F_000 552 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_absorpt_coefficient_mu 3.859 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_T_min 0.39947 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_probe 'x-ray' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Ruby' _diffrn_detector 'CCD plate' _diffrn_detector_type 'Ruby' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2576 _diffrn_reflns_number 9243 _diffrn_reflns_av_unetI/netI 0.0255 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.842 _diffrn_reflns_theta_max 76.021 _diffrn_reflns_theta_full 67.684 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 2749 _reflns_number_gt 2561 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.670 _reflns_Friedel_fraction_max 0.972 _reflns_Friedel_fraction_full 1.000 _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 1.171.40.84a (Rigaku OD, 2020)' _computing_cell_refinement 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)' _computing_structure_solution 'SHELXT (Sheldrick, 2015a)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015b)' _computing_molecular_graphics 'XP-Molecular Graphics (Siemens, 1994)' _computing_publication_material 'PLATON (Spek, 2020)' _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^)+(0.0469P)^2^+0.3511P] 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 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_extinction_coef 0.0026(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ; Flack x determined using 963 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.391(7) _chemical_absolute_configuration ? _refine_ls_number_reflns 2749 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0911 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Cl1 Cl 0.01638(15) 0.50665(5) 0.78575(4) 0.0480(2) Uani 1 1 d . . . . . S1 S 0.6905(2) 0.32612(6) 0.56884(5) 0.0597(3) Uani 1 1 d . . . . . N3 N 0.4221(6) 0.42580(16) 0.66893(14) 0.0418(6) Uani 1 1 d . . . . . N8 N 0.4654(7) 0.27688(17) 0.69434(14) 0.0482(7) Uani 1 1 d . . . . . C2 C 0.5080(7) 0.34717(19) 0.65122(15) 0.0426(7) Uani 1 1 d . . . . . C4 C 0.5263(7) 0.50968(18) 0.63918(15) 0.0448(7) Uani 1 1 d . . . . . H4A H 0.7208 0.5059 0.6367 0.054 Uiso 1 1 calc R U . . . H4B H 0.4816 0.5565 0.6744 0.054 Uiso 1 1 calc R U . . . C5 C 0.4219(7) 0.5352(2) 0.56239(17) 0.0500(8) Uani 1 1 d . . . . . H5A H 0.4477 0.5983 0.5555 0.060 Uiso 1 1 calc R U . . . H5B H 0.2300 0.5238 0.5608 0.060 Uiso 1 1 calc R U . . . C6 C 0.5541(8) 0.4869(2) 0.49697(17) 0.0549(8) Uani 1 1 d . . . . . H6A H 0.4854 0.5111 0.4501 0.066 Uiso 1 1 calc R U . . . H6B H 0.7461 0.4982 0.4984 0.066 Uiso 1 1 calc R U . . . C7 C 0.5086(10) 0.3886(2) 0.49722(17) 0.0590(9) Uani 1 1 d . . . . . H7A H 0.5583 0.3656 0.4481 0.071 Uiso 1 1 calc R U . . . H7B H 0.3177 0.3778 0.5039 0.071 Uiso 1 1 calc R U . . . C1' C 0.3771(6) 0.27941(18) 0.77146(15) 0.0394(6) Uani 1 1 d . . . . . C2' C 0.5046(7) 0.3333(2) 0.82316(17) 0.0481(7) Uani 1 1 d . . . . . H2'A H 0.6451 0.3700 0.8083 0.058 Uiso 1 1 calc R U . . . C3' C 0.4200(8) 0.3319(2) 0.89755(18) 0.0559(9) Uani 1 1 d . . . . . H3'A H 0.5024 0.3686 0.9327 0.067 Uiso 1 1 calc R U . . . C4' C 0.2165(8) 0.2770(2) 0.91976(19) 0.0590(9) Uani 1 1 d . . . . . H4'A H 0.1615 0.2763 0.9699 0.071 Uiso 1 1 calc R U . . . C5' C 0.0933(8) 0.2229(2) 0.8681(2) 0.0598(9) Uani 1 1 d . . . . . H5'A H -0.0445 0.1853 0.8834 0.072 Uiso 1 1 calc R U . . . C6' C 0.1730(7) 0.2239(2) 0.79343(19) 0.0495(7) Uani 1 1 d . . . . . H6'A H 0.0891 0.1874 0.7584 0.059 Uiso 1 1 calc R U . . . O1W O 0.4882(6) 0.10325(15) 0.64292(14) 0.0528(6) Uani 1 1 d . . . . . H1W H 0.620(11) 0.079(3) 0.660(3) 0.075(16) Uiso 1 1 d . . . . . H2W H 0.348(11) 0.073(3) 0.664(3) 0.076(14) Uiso 1 1 d . . . . . H8 H 0.479(8) 0.228(2) 0.6744(19) 0.049(10) Uiso 1 1 d . . . . . H3 H 0.320(7) 0.430(2) 0.704(2) 0.046(9) 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 Cl1 0.0458(4) 0.0516(4) 0.0467(4) -0.0009(3) 0.0005(3) 0.0056(3) S1 0.0793(6) 0.0484(4) 0.0515(4) 0.0030(4) 0.0279(4) 0.0126(4) N3 0.0595(16) 0.0351(12) 0.0308(12) 0.0027(9) 0.0095(11) 0.0015(11) N8 0.0723(19) 0.0312(12) 0.0410(13) 0.0021(10) 0.0126(13) 0.0004(13) C2 0.0536(17) 0.0384(14) 0.0360(14) 0.0018(11) 0.0083(14) 0.0023(14) C4 0.0657(18) 0.0333(13) 0.0354(13) 0.0005(11) -0.0026(14) -0.0063(15) C5 0.068(2) 0.0426(16) 0.0392(15) 0.0084(12) -0.0041(14) 0.0011(15) C6 0.077(2) 0.0544(18) 0.0336(14) 0.0102(13) 0.0002(15) -0.0046(18) C7 0.086(3) 0.0561(19) 0.0344(15) -0.0057(13) 0.0086(18) -0.010(2) C1' 0.0520(17) 0.0290(13) 0.0372(14) 0.0060(11) 0.0046(12) 0.0053(12) C2' 0.0552(17) 0.0405(15) 0.0485(16) 0.0077(13) -0.0014(15) -0.0054(16) C3' 0.079(2) 0.0459(17) 0.0428(16) 0.0014(14) -0.0089(16) 0.0039(18) C4' 0.086(3) 0.0497(18) 0.0415(16) 0.0062(14) 0.0140(17) 0.0126(19) C5' 0.070(2) 0.0478(18) 0.061(2) 0.0116(16) 0.0214(18) -0.0045(17) C6' 0.0596(19) 0.0374(15) 0.0514(17) -0.0013(13) 0.0056(16) -0.0059(15) O1W 0.0562(15) 0.0420(12) 0.0602(14) 0.0061(10) 0.0033(13) 0.0030(13) _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 C2 1.749(3) . ? S1 C7 1.823(4) . ? N3 C2 1.301(4) . ? N3 C4 1.468(4) . ? N3 H3 0.81(4) . ? N8 C2 1.326(4) . ? N8 C1' 1.437(4) . ? N8 H8 0.82(4) . ? C4 C5 1.508(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.520(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.504(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C1' C6' 1.373(5) . ? C1' C2' 1.381(4) . ? C2' C3' 1.385(4) . ? C2' H2'A 0.9300 . ? C3' C4' 1.366(5) . ? C3' H3'A 0.9300 . ? C4' C5' 1.373(5) . ? C4' H4'A 0.9300 . ? C5' C6' 1.383(5) . ? C5' H5'A 0.9300 . ? C6' H6'A 0.9300 . ? O1W H1W 0.81(5) . ? O1W H2W 0.91(5) . ? 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 C2 S1 C7 103.31(16) . . ? C2 N3 C4 125.9(3) . . ? C2 N3 H3 118(2) . . ? C4 N3 H3 115(2) . . ? C2 N8 C1' 125.2(2) . . ? C2 N8 H8 117(2) . . ? C1' N8 H8 117(2) . . ? N3 C2 N8 122.7(3) . . ? N3 C2 S1 122.5(2) . . ? N8 C2 S1 114.8(2) . . ? N3 C4 C5 115.1(3) . . ? N3 C4 H4A 108.5 . . ? C5 C4 H4A 108.5 . . ? N3 C4 H4B 108.5 . . ? C5 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C4 C5 C6 114.7(3) . . ? C4 C5 H5A 108.6 . . ? C6 C5 H5A 108.6 . . ? C4 C5 H5B 108.6 . . ? C6 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C7 C6 C5 114.0(3) . . ? C7 C6 H6A 108.8 . . ? C5 C6 H6A 108.8 . . ? C7 C6 H6B 108.8 . . ? C5 C6 H6B 108.8 . . ? H6A C6 H6B 107.6 . . ? C6 C7 S1 116.1(3) . . ? C6 C7 H7A 108.3 . . ? S1 C7 H7A 108.3 . . ? C6 C7 H7B 108.3 . . ? S1 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C6' C1' C2' 120.7(3) . . ? C6' C1' N8 118.7(3) . . ? C2' C1' N8 120.5(3) . . ? C1' C2' C3' 119.0(3) . . ? C1' C2' H2'A 120.5 . . ? C3' C2' H2'A 120.5 . . ? C4' C3' C2' 120.6(3) . . ? C4' C3' H3'A 119.7 . . ? C2' C3' H3'A 119.7 . . ? C3' C4' C5' 120.0(3) . . ? C3' C4' H4'A 120.0 . . ? C5' C4' H4'A 120.0 . . ? C4' C5' C6' 120.3(3) . . ? C4' C5' H5'A 119.9 . . ? C6' C5' H5'A 119.9 . . ? C1' C6' C5' 119.4(3) . . ? C1' C6' H6'A 120.3 . . ? C5' C6' H6'A 120.3 . . ? H1W O1W H2W 104(4) . . ? _refine_diff_density_max 0.187 _refine_diff_density_min -0.169 _refine_diff_density_rms 0.035 _shelx_res_file ; e0381_A2.res created by SHELXL-2014/7 TITL e0381_a2_a.res in P2(1)2(1)2(1) CELL 1.54184 4.971829 15.116938 17.73762 90 90 90 ZERR 4 0.000143 0.000391 0.000472 0 0 0 LATT -1 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 Cl S UNIT 44 68 8 4 4 4 ACTA L.S. 4 0 0 PLAN 20 BOND $H list 4 fmap 2 53 WGHT 0.046900 0.351100 EXTI 0.002630 FVAR 9.50157 CL1 5 0.016380 0.506653 0.785747 11.00000 0.04584 0.05165 = 0.04665 -0.00087 0.00049 0.00563 S1 6 0.690540 0.326123 0.568839 11.00000 0.07926 0.04844 = 0.05147 0.00298 0.02790 0.01259 N3 3 0.422131 0.425797 0.668933 11.00000 0.05948 0.03514 = 0.03079 0.00267 0.00952 0.00148 N8 3 0.465367 0.276882 0.694335 11.00000 0.07233 0.03117 = 0.04097 0.00214 0.01257 0.00041 C2 1 0.507955 0.347171 0.651216 11.00000 0.05355 0.03837 = 0.03598 0.00184 0.00831 0.00227 C4 1 0.526270 0.509681 0.639179 11.00000 0.06568 0.03327 = 0.03539 0.00055 -0.00262 -0.00631 AFIX 23 H4A 2 0.720828 0.505902 0.636690 11.00000 -1.20000 H4B 2 0.481552 0.556470 0.674440 11.00000 -1.20000 AFIX 0 C5 1 0.421873 0.535171 0.562388 11.00000 0.06824 0.04260 = 0.03924 0.00842 -0.00406 0.00109 AFIX 23 H5A 2 0.447748 0.598262 0.555544 11.00000 -1.20000 H5B 2 0.229958 0.523769 0.560846 11.00000 -1.20000 AFIX 0 C6 1 0.554095 0.486946 0.496969 11.00000 0.07681 0.05438 = 0.03363 0.01018 0.00025 -0.00462 AFIX 23 H6A 2 0.485378 0.511087 0.450105 11.00000 -1.20000 H6B 2 0.746101 0.498201 0.498406 11.00000 -1.20000 AFIX 0 C7 1 0.508559 0.388586 0.497220 11.00000 0.08650 0.05613 = 0.03437 -0.00568 0.00858 -0.01031 AFIX 23 H7A 2 0.558291 0.365576 0.448111 11.00000 -1.20000 H7B 2 0.317706 0.377820 0.503897 11.00000 -1.20000 AFIX 0 C1' 1 0.377144 0.279407 0.771459 11.00000 0.05196 0.02899 = 0.03718 0.00600 0.00459 0.00527 C2' 1 0.504595 0.333292 0.823161 11.00000 0.05519 0.04054 = 0.04847 0.00775 -0.00142 -0.00544 AFIX 43 H2'A 2 0.645064 0.369971 0.808276 11.00000 -1.20000 AFIX 0 C3' 1 0.419967 0.331866 0.897547 11.00000 0.07901 0.04586 = 0.04280 0.00142 -0.00888 0.00391 AFIX 43 H3'A 2 0.502391 0.368595 0.932695 11.00000 -1.20000 AFIX 0 C4' 1 0.216499 0.276992 0.919758 11.00000 0.08586 0.04965 = 0.04153 0.00623 0.01395 0.01259 AFIX 43 H4'A 2 0.161502 0.276314 0.969868 11.00000 -1.20000 AFIX 0 C5' 1 0.093252 0.222861 0.868117 11.00000 0.07006 0.04776 = 0.06146 0.01164 0.02143 -0.00448 AFIX 43 H5'A 2 -0.044495 0.185315 0.883423 11.00000 -1.20000 AFIX 0 C6' 1 0.172990 0.223906 0.793432 11.00000 0.05963 0.03740 = 0.05140 -0.00134 0.00561 -0.00589 AFIX 43 H6'A 2 0.089141 0.187363 0.758408 11.00000 -1.20000 AFIX 0 O1W 4 0.488214 0.103254 0.642919 11.00000 0.05617 0.04203 = 0.06020 0.00612 0.00332 0.00304 H1W 2 0.619668 0.078663 0.660013 11.00000 0.07492 H2W 2 0.348000 0.073395 0.663723 11.00000 0.07625 H8 2 0.479208 0.228300 0.674428 11.00000 0.04894 H3 2 0.320122 0.430136 0.704436 11.00000 0.04567 HKLF 4 REM e0381_a2_a.res in P2(1)2(1)2(1) REM R1 = 0.0351 for 2561 Fo > 4sig(Fo) and 0.0387 for all 2749 data REM 162 parameters refined using 0 restraints END WGHT 0.0469 0.3511 REM Highest difference peak 0.187, deepest hole -0.169, 1-sigma level 0.035 Q1 1 0.8145 0.3205 0.6006 11.00000 0.05 0.19 Q2 1 0.1366 0.5537 0.7803 11.00000 0.05 0.18 Q3 1 0.1327 0.4559 0.8036 11.00000 0.05 0.17 Q4 1 0.7611 0.3597 0.5984 11.00000 0.05 0.17 Q5 1 -0.1282 0.5587 0.7824 11.00000 0.05 0.17 Q6 1 0.6259 0.3622 0.5203 11.00000 0.05 0.14 Q7 1 0.5542 0.2910 0.5773 11.00000 0.05 0.14 Q8 1 0.7816 0.3807 0.5698 11.00000 0.05 0.14 Q9 1 0.5874 0.3776 0.5408 11.00000 0.05 0.13 Q10 1 0.3411 0.3187 0.7812 11.00000 0.05 0.13 Q11 1 0.5551 0.0007 0.7026 11.00000 0.05 0.12 Q12 1 0.3127 0.2361 0.7853 11.00000 0.05 0.12 Q13 1 0.2546 0.2597 0.7837 11.00000 0.05 0.12 Q14 1 0.6214 0.1568 0.6272 11.00000 0.05 0.12 Q15 1 0.5913 0.3458 0.6213 11.00000 0.05 0.11 Q16 1 0.3800 0.5477 0.6838 11.00000 0.05 0.11 Q17 1 0.1021 0.2211 0.7814 11.00000 0.05 0.11 Q18 1 -0.1547 0.4569 0.7800 11.00000 0.05 0.11 Q19 1 0.5339 0.3182 0.6825 11.00000 0.05 0.11 Q20 1 -0.1583 0.1839 0.8560 11.00000 0.05 0.11 ; _shelx_res_checksum 45529 _shelx_hkl_file ; 0 0 -2 168047. 2527.98 20 0 0 -3 101.349 66.1093 20 0 0 -4 24539.9 505.123 20 0 0 -5 19.9468 92.1524 20 0 0 -6 46775.0 905.044 20 0 0 -7 974.036 152.232 20 0 0 -8 143069. 2397.83 20 0 0 -9-44.5953 149.913 20 0 0 -10 10175.9 408.640 20 0 0 -11 40.8352 134.239 20 0 0 -12 2041.53 224.151 20 0 0 -13-8.35484 139.408 20 0 0 14 324263. 6872.81 15 0 0 -14 312274. 5172.69 20 0 0 -14 330140. 7127.62 12 0 0 -15 123.257 147.050 20 0 0 -15-62.5106 371.399 12 0 0 15 222.862 349.054 15 0 0 -16 1879.74 571.182 12 0 0 16 2586.68 539.986 15 0 0 17-512.414 339.526 15 0 0 -17 258.977 286.270 12 0 0 -18 15302.8 1125.37 12 0 0 18 12206.6 984.629 15 0 0 -19-453.554 367.395 12 0 0 19-124.261 254.282 15 0 0 -20 104.696 215.081 12 0 0 20 376.718 261.358 15 0 0 21 234.988 219.487 14 0 0 21-160.712 163.088 15 0 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358.651 350.880 2 0 12 13 599.478 357.334 18 0 -12 13 132.768 401.376 11 0 12 -14 4439.37 632.142 2 0 12 14 4707.71 644.026 5 0 12 15 6691.34 700.407 6 0 12 -15 7986.52 762.519 10 0 12 15 7459.76 715.066 5 0 12 16 1732.09 363.873 5 0 12 16 1514.87 364.322 6 0 12 -16 1638.91 307.491 10 0 12 17 460.409 201.244 6 0 12 17 962.658 234.218 5 0 13 0-112.969 185.044 19 0 13 0 889.558 543.821 9 0 13 0 972.279 551.455 8 0 13 1 24231.3 1657.79 9 0 13 1 26592.1 1601.02 6 0 13 -1 23826.6 1687.95 9 0 13 1 24811.5 1670.43 8 0 13 -1 26065.0 809.434 19 0 13 1 26652.5 815.093 19 0 13 2 3026.90 629.901 9 0 13 2 3604.27 712.285 8 0 13 -2 2534.05 657.264 9 0 13 2 2791.69 552.536 6 0 13 3 1605.09 522.490 6 0 13 -3 1020.62 540.824 9 0 13 3 1770.99 550.136 8 0 13 -3 1100.19 599.331 3 0 13 -4 10765.9 1159.14 3 0 13 4 11560.2 1081.21 6 0 13 4 11358.8 1096.05 8 0 13 -4 11343.8 1166.80 9 0 13 -5 339.946 366.011 3 0 13 -5 1023.54 514.841 9 0 13 5-105.904 378.874 6 0 13 5-263.890 348.502 8 0 13 6 28269.5 1687.35 6 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490.239 398.041 3 0 14 -7 709.084 553.409 2 0 14 8 1936.66 571.629 6 0 -14 8 3254.97 656.734 11 0 14 8 2514.62 581.799 8 0 14 8 2611.53 558.938 5 0 14 -8 2569.91 721.695 2 0 14 9 5304.92 774.158 6 0 14 9 6362.73 776.276 5 0 -14 9 6148.76 799.471 11 0 14 9 6226.32 777.415 8 0 14 -9 4759.03 794.755 2 0 14 10 7559.96 844.505 5 0 14 10 6825.26 844.760 6 0 14 -10 6672.62 855.778 2 0 -14 10 8391.90 868.023 11 0 14 11 9751.01 901.256 6 0 14 -11 10009.2 1000.92 2 0 14 11 11692.5 953.944 5 0 14 -12 9225.20 890.876 2 0 14 12 9039.88 832.649 6 0 14 12 10168.9 861.094 5 0 14 13 9643.44 787.020 6 0 14 13 10311.8 784.142 5 0 14 -13 9088.90 784.215 2 0 14 -14 302.860 231.183 10 0 14 14 316.697 280.923 6 0 14 14 563.467 245.968 5 0 14 15 1309.96 232.776 6 0 15 0-104.311 401.002 9 0 15 0-166.506 407.955 3 0 15 1 3681.65 708.114 9 0 15 -1 4764.89 797.904 3 0 15 -1 3986.63 746.261 9 0 15 2 279.767 426.125 9 0 15 -2 395.868 497.152 3 0 15 -2 831.772 510.041 9 0 15 -3 4245.36 798.372 9 0 15 -3 3526.41 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310.386 11 -5 -8 4 1501.12 339.995 17 -5 8 -4 1468.06 376.264 3 -5 8 -4 1439.70 410.650 4 -5 -8 5 5877.91 580.145 17 -5 8 -5 6841.43 678.369 4 -5 8 -5 7017.36 676.529 3 -5 -8 5 6159.12 557.266 11 -5 -8 6 2224.50 313.658 11 -5 -8 6 1918.38 351.332 17 -5 8 -6 1805.48 409.392 3 -5 -8 7 58.4348 225.433 17 -5 8 -7-138.994 273.119 3 -5 8 -8 775.858 337.177 3 -5 -8 8 956.828 248.179 17 -5 -8 9 3045.22 322.090 17 -5 -9 -8 2092.38 302.359 11 -5 -9 -7 1259.77 302.746 11 -5 -9 -6 354.332 244.445 11 -5 9 6 50.0985 229.127 4 -5 -9 -5 9980.87 756.878 11 -5 9 5 9153.16 694.232 4 -5 -9 -4 280.210 298.080 11 -5 9 4 563.532 326.195 4 -5 -9 -3 3143.14 509.254 11 -5 9 3 3123.63 480.916 4 -5 -9 -2 2908.23 484.885 11 -5 9 2 2395.94 483.148 4 -5 -9 -1 1421.03 385.497 11 -5 9 1 1186.52 423.358 4 -5 -9 0 619.378 305.741 11 -5 9 0 503.281 370.707 4 -5 -9 1 996.866 343.510 11 -5 -9 1 1174.12 274.219 17 -5 9 -1 1111.34 429.104 4 -5 -9 2 2514.65 437.733 11 -5 -9 2 2746.25 364.256 17 -5 9 -2 2948.12 500.111 4 -5 -9 3 2460.21 430.077 11 -5 -9 3 2119.70 380.678 17 -5 9 -3 2653.59 461.441 4 -5 -9 4 60.6512 198.593 11 -5 -9 4 665.791 237.717 17 -5 9 -4 640.538 234.909 3 -5 9 -4-177.007 288.003 4 -5 -9 5 9538.89 647.765 17 -5 9 -5 10014.3 713.376 4 -5 9 -5 9691.96 710.377 3 -5 -9 5 10337.9 666.216 11 -5 -9 6 15.5899 136.479 11 -5 -9 6 141.795 185.884 17 -5 9 -6 20.6925 191.833 3 -5 9 -7 1376.56 262.253 3 -5 -9 7 1306.60 256.280 17 -5 -9 8 1619.87 246.938 17 -5 -10 -6 1459.79 276.809 11 -5 -10 -5 1379.00 296.991 11 -5 10 5 1372.47 280.503 4 -5 -10 -4 1778.91 350.234 11 -5 10 4 1397.50 318.726 4 -5 -10 -3 4434.91 507.766 11 -5 10 3 3850.72 483.857 4 -5 -10 -2 740.046 295.872 11 -5 10 2 1128.98 362.177 4 -5 -10 -1 4512.07 539.901 11 -5 10 1 4077.49 538.136 4 -5 -10 0 918.145 325.809 11 -5 10 0 778.847 362.974 4 -5 -10 1 4457.45 526.706 11 -5 10 -1 4704.68 558.835 4 -5 -10 2 1254.11 353.987 11 -5 -10 2 732.443 209.684 17 -5 10 -2 633.254 312.478 4 -5 -10 3 4890.66 483.311 11 -5 -10 3 3694.99 403.783 17 -5 10 -3 4936.92 529.967 4 -5 -10 4 1570.48 274.661 11 -5 -10 4 1272.86 249.215 17 -5 10 -4 1225.04 316.521 4 -5 -10 5 998.419 220.559 11 -5 -10 5 963.124 213.652 17 -5 -11 -3 396.417 189.175 11 -5 11 3 217.216 159.623 4 -5 -11 -2 219.916 180.162 11 -5 11 2 393.135 205.896 4 -5 -11 -1 906.108 265.562 11 -5 11 1 889.747 248.253 4 -5 -11 0-112.331 182.747 11 -5 11 0-102.576 174.749 4 -5 -11 1 613.872 250.797 11 -5 11 -1 1165.60 296.270 4 -5 -11 2 181.140 185.096 11 -5 11 -2 381.215 223.542 4 -5 -11 3 278.093 158.625 11 -6 0 0 9634.06 727.277 13 -6 0 1 226.385 245.598 13 -6 0 -1-175.607 285.614 13 -6 0 2 3624.88 468.240 13 -6 0 -2 4543.52 536.156 13 -6 0 3 1967.29 345.385 13 -6 0 -3 2353.08 403.110 13 -6 0 4 1740.89 299.777 13 -6 0 -4 1514.26 345.685 13 -6 0 5 4339.17 398.536 13 -6 0 -5 4347.82 455.891 13 -6 0 -6-43.9936 193.076 13 -6 1 6 2906.39 311.222 13 -6 -1 -6 3699.01 402.501 13 -6 1 5 159.136 184.490 13 -6 -1 -5 832.034 275.709 13 -6 1 4 2920.32 377.055 13 -6 -1 -4 3590.42 459.896 13 -6 1 3-10.6271 210.481 13 -6 -1 -3 304.984 238.624 13 -6 1 2 1293.18 317.796 13 -6 -1 -2 1670.12 411.890 13 -6 1 1 3782.09 466.273 13 -6 -1 -1 3850.12 519.037 13 -6 1 0 621.063 264.704 13 -6 -1 0 718.898 301.431 13 -6 -1 1 5221.87 532.327 13 -6 1 -1 4233.34 510.368 13 -6 -1 2 1091.57 317.431 13 -6 1 -2 1541.73 338.110 13 -6 -1 3 293.008 225.350 13 -6 1 -3 316.594 260.393 13 -6 -1 4 3740.46 389.083 13 -6 1 -4 3159.29 401.718 13 -6 -1 5 530.093 209.727 13 -6 1 -5 219.378 186.906 13 -6 2 5-99.7656 148.835 13 -6 -2 -5 169.542 191.115 13 -6 2 4 333.168 207.413 13 -6 -2 -4 778.158 319.128 13 -6 2 3 288.763 210.464 13 -6 -2 -3 358.030 238.988 13 -6 2 2 3081.12 412.911 13 -6 -2 -2 3748.27 482.350 13 -6 2 1-560.644 248.555 13 -6 -2 -1-363.331 292.825 13 -6 2 0 361.757 269.900 13 -6 -2 0 1189.50 351.544 13 -6 -2 1 113.622 224.082 13 -6 2 -1 83.0660 213.258 13 -6 2 -2 2813.69 399.909 13 -6 -2 2 2381.27 383.035 13 -6 -2 3-23.3614 174.587 13 -6 2 -3 195.239 227.081 13 -6 -2 4 762.270 177.852 13 -6 2 -4 411.000 211.537 13 -6 3 5 246.113 147.366 13 -6 3 4-19.0161 149.304 13 -6 -3 -4 469.691 243.290 13 -6 3 3 2531.56 331.816 13 -6 -3 -3 2234.65 356.665 13 -6 3 2 1778.55 315.270 13 -6 -3 -2 2251.40 372.242 13 -6 3 1 569.865 229.688 13 -6 -3 -1 429.122 249.536 13 -6 3 0 186.690 214.429 13 -6 -3 0 386.876 233.276 13 -6 3 -1 177.677 199.993 13 -6 -3 1 361.241 221.974 13 -6 -3 2 1842.47 298.226 13 -6 3 -2 827.359 260.725 13 -6 3 -3 1890.63 302.068 13 -6 4 3 408.261 143.553 13 -6 4 2 3379.54 349.649 13 -6 4 1 1338.92 253.954 13 -6 4 0 991.403 204.437 13 -6 4 -1 500.015 176.258 13 0 0 0 0.00 0.00 0 TITL e0381_A2 in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 1.54184 4.971829 15.116938 17.737620 90.0000 90.0000 90.0000 ZERR 6.00 0.000143 0.000391 0.000472 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 UNIT 66.00 60.00 6.00 6.00 TREF HKLF 4 END ; _shelx_hkl_checksum 52608