data_22019066_0m _audit_creation_date 2019-01-15 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C23 H24 Cl N O3 S' _chemical_formula_sum 'C23 H24 Cl N O3 S' _chemical_formula_weight 429.94 _chemical_melting_point ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _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. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2873(3) _cell_length_b 11.2154(6) _cell_length_c 13.2137(6) _cell_angle_alpha 104.220(2) _cell_angle_beta 107.154(2) _cell_angle_gamma 107.165(2) _cell_volume 1044.15(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3284 _cell_measurement_temperature 100 _cell_measurement_theta_max 26.355 _cell_measurement_theta_min 3.034 _shelx_estimated_absorpt_T_max 0.991 _shelx_estimated_absorpt_T_min 0.955 _exptl_absorpt_coefficient_mu 0.308 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.4025 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1634 before and 0.0834 after correction. The Ratio of minimum to maximum transmission is 0.5400. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 452 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0893 _diffrn_reflns_av_unetI/netI 0.0991 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 11931 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.374 _diffrn_reflns_theta_min 2.646 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3022 _reflns_number_total 4227 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.354 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.077 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 263 _refine_ls_number_reflns 4227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0572 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.4146P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1165 _refine_ls_wR_factor_ref 0.1364 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C12(H12), C11(H11), C13(H13), C14(H14) 2.b Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C9(H9A,H9B), C16(H16A,H16B), C15(H15A,H15B) 2.c Aromatic/amide H refined with riding coordinates: C22(H22), C5(H5), C3(H3), C21(H21), C6(H6), C18(H18), C2(H2), C19(H19), C8(H8) 2.d Idealised Me refined as rotating group: C23(H23A,H23B,H23C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 0.66569(9) 0.39931(7) 0.35732(5) 0.01986(19) Uani 1 1 d . . . . . Cl1 Cl 1.60614(10) 0.87232(8) 0.13151(6) 0.0349(2) Uani 1 1 d . . . . . O3 O 0.6939(2) 0.40404(19) 0.47084(15) 0.0251(5) Uani 1 1 d . . . . . O1 O 0.6794(2) 0.56265(19) 0.25606(15) 0.0256(5) Uani 1 1 d . . . . . O2 O 0.7609(3) 0.33949(19) 0.29981(16) 0.0273(5) Uani 1 1 d . . . . . N1 N 0.7075(3) 0.5598(2) 0.36795(18) 0.0204(5) Uani 1 1 d . . . . . C22 C 0.3111(4) 0.3613(3) 0.3155(2) 0.0220(6) Uani 1 1 d . . . . . H22 H 0.357073 0.421145 0.391862 0.026 Uiso 1 1 calc R . . . . C17 C 0.4301(3) 0.3268(3) 0.2707(2) 0.0180(6) Uani 1 1 d . . . . . C4 C 1.2763(3) 0.8278(3) 0.3486(2) 0.0214(6) Uani 1 1 d . . . . . C20 C 0.0560(4) 0.2206(3) 0.1357(2) 0.0223(6) Uani 1 1 d . . . . . C5 C 1.3150(4) 0.9386(3) 0.3156(2) 0.0243(6) Uani 1 1 d . . . . . H5 H 1.269917 1.004726 0.338596 0.029 Uiso 1 1 calc R . . . . C3 C 1.3481(4) 0.7343(3) 0.3159(2) 0.0233(6) Uani 1 1 d . . . . . H3 H 1.325763 0.659142 0.338733 0.028 Uiso 1 1 calc R . . . . C7 C 1.1585(3) 0.8093(3) 0.4142(2) 0.0218(6) Uani 1 1 d . . . . . C21 C 0.1255(4) 0.3078(3) 0.2481(2) 0.0237(6) Uani 1 1 d . . . . . H21 H 0.043817 0.330764 0.278836 0.028 Uiso 1 1 calc R . . . . C12 C 1.0020(3) 0.6729(3) 0.3702(2) 0.0210(6) Uani 1 1 d . . . . . H12 H 1.053256 0.602352 0.363775 0.025 Uiso 1 1 calc R . . . . C10 C 0.8808(4) 0.7900(3) 0.5016(2) 0.0231(6) Uani 1 1 d . . . . . H10A H 0.809980 0.776686 0.549410 0.028 Uiso 1 1 calc R . . . . H10B H 0.815303 0.817993 0.442143 0.028 Uiso 1 1 calc R . . . . C11 C 0.8948(4) 0.6605(3) 0.4466(2) 0.0217(6) Uani 1 1 d . . . . . H11 H 0.951594 0.627577 0.505939 0.026 Uiso 1 1 calc R . . . . C13 C 0.8539(3) 0.6414(3) 0.2541(2) 0.0218(6) Uani 1 1 d . . . . . H13 H 0.850165 0.727439 0.247287 0.026 Uiso 1 1 calc R . . . . C6 C 1.4172(4) 0.9545(3) 0.2502(2) 0.0266(7) Uani 1 1 d . . . . . H6 H 1.442304 1.030232 0.228182 0.032 Uiso 1 1 calc R . . . . C18 C 0.3646(4) 0.2406(3) 0.1591(2) 0.0228(6) Uani 1 1 d . . . . . H18 H 0.446460 0.217955 0.128354 0.027 Uiso 1 1 calc R . . . . C2 C 1.4509(4) 0.7483(3) 0.2510(2) 0.0249(7) Uani 1 1 d . . . . . H2 H 1.499515 0.683889 0.229702 0.030 Uiso 1 1 calc R . . . . C19 C 0.1772(4) 0.1880(3) 0.0930(2) 0.0243(6) Uani 1 1 d . . . . . H19 H 0.131208 0.128110 0.016688 0.029 Uiso 1 1 calc R . . . . C9 C 1.0730(4) 0.8984(3) 0.5746(2) 0.0265(7) Uani 1 1 d . . . . . H9A H 1.064336 0.985711 0.602843 0.032 Uiso 1 1 calc R . . . . H9B H 1.130484 0.877255 0.641146 0.032 Uiso 1 1 calc R . . . . C23 C -0.1473(4) 0.1664(3) 0.0639(2) 0.0316(7) Uani 1 1 d . . . . . H23A H -0.217145 0.131816 0.106127 0.047 Uiso 1 1 calc GR . . . . H23B H -0.177851 0.093820 -0.006562 0.047 Uiso 1 1 calc GR . . . . H23C H -0.178978 0.238202 0.045522 0.047 Uiso 1 1 calc GR . . . . C1 C 1.4820(4) 0.8572(3) 0.2176(2) 0.0252(7) Uani 1 1 d . . . . . C14 C 0.8725(4) 0.5647(3) 0.1525(2) 0.0296(7) Uani 1 1 d . . . . . H14 H 0.901657 0.485074 0.156098 0.036 Uiso 1 1 calc R . . . . C8 C 1.1909(4) 0.9083(3) 0.5068(2) 0.0248(6) Uani 1 1 d . . . . . H8 H 1.294338 0.989843 0.531765 0.030 Uiso 1 1 calc R . . . . C16 C 0.7521(4) 0.5533(3) 0.0359(2) 0.0366(8) Uani 1 1 d . . . . . H16A H 0.707457 0.468087 -0.028535 0.044 Uiso 1 1 calc R . . . . H16B H 0.665316 0.598283 0.032010 0.044 Uiso 1 1 calc R . . . . C15 C 0.9539(4) 0.6399(4) 0.0874(2) 0.0378(8) Uani 1 1 d . . . . . H15A H 0.991083 0.738290 0.114928 0.045 Uiso 1 1 calc R . . . . H15B H 1.033201 0.608168 0.054417 0.045 Uiso 1 1 calc R . . . . 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 0.0144(3) 0.0219(4) 0.0227(3) 0.0075(3) 0.0068(3) 0.0074(3) Cl1 0.0262(4) 0.0463(5) 0.0287(4) 0.0118(3) 0.0140(3) 0.0081(4) O3 0.0227(10) 0.0289(11) 0.0229(10) 0.0122(8) 0.0067(8) 0.0094(9) O1 0.0170(10) 0.0321(11) 0.0243(10) 0.0152(9) 0.0055(8) 0.0039(9) O2 0.0217(10) 0.0289(11) 0.0326(11) 0.0073(9) 0.0110(9) 0.0147(9) N1 0.0163(11) 0.0213(12) 0.0214(11) 0.0083(9) 0.0051(9) 0.0064(10) C22 0.0187(14) 0.0244(15) 0.0212(13) 0.0056(11) 0.0085(11) 0.0079(12) C17 0.0144(13) 0.0181(14) 0.0216(13) 0.0085(11) 0.0065(11) 0.0063(11) C4 0.0093(13) 0.0240(15) 0.0219(13) 0.0057(11) 0.0008(10) 0.0021(11) C20 0.0173(14) 0.0203(15) 0.0254(14) 0.0094(11) 0.0060(11) 0.0038(12) C5 0.0190(14) 0.0239(15) 0.0267(14) 0.0067(12) 0.0072(12) 0.0082(12) C3 0.0155(14) 0.0202(15) 0.0261(14) 0.0060(12) 0.0041(11) 0.0026(12) C7 0.0136(13) 0.0230(15) 0.0253(14) 0.0086(12) 0.0048(11) 0.0055(12) C21 0.0181(14) 0.0303(16) 0.0271(14) 0.0118(12) 0.0126(12) 0.0103(12) C12 0.0152(13) 0.0219(15) 0.0227(13) 0.0067(11) 0.0063(11) 0.0057(12) C10 0.0202(14) 0.0244(15) 0.0227(14) 0.0062(12) 0.0095(11) 0.0069(12) C11 0.0157(13) 0.0234(15) 0.0212(13) 0.0075(11) 0.0039(11) 0.0052(12) C13 0.0157(13) 0.0229(15) 0.0243(14) 0.0099(12) 0.0079(11) 0.0031(12) C6 0.0228(15) 0.0250(16) 0.0277(15) 0.0112(12) 0.0065(12) 0.0059(13) C18 0.0208(14) 0.0234(15) 0.0245(14) 0.0061(11) 0.0102(11) 0.0100(12) C2 0.0165(14) 0.0291(17) 0.0223(14) 0.0035(12) 0.0046(11) 0.0082(12) C19 0.0238(15) 0.0218(15) 0.0199(13) 0.0031(11) 0.0053(12) 0.0065(12) C9 0.0249(15) 0.0246(16) 0.0253(14) 0.0055(12) 0.0092(12) 0.0075(13) C23 0.0189(15) 0.0360(18) 0.0314(16) 0.0103(13) 0.0057(12) 0.0054(14) C1 0.0180(14) 0.0300(16) 0.0200(13) 0.0063(12) 0.0052(11) 0.0040(12) C14 0.0202(15) 0.0289(17) 0.0310(16) 0.0053(13) 0.0072(12) 0.0059(13) C8 0.0187(14) 0.0232(15) 0.0273(14) 0.0081(12) 0.0068(12) 0.0046(12) C16 0.0239(16) 0.046(2) 0.0215(15) 0.0018(14) 0.0056(13) 0.0011(15) C15 0.0260(17) 0.051(2) 0.0248(15) 0.0078(14) 0.0099(13) 0.0058(15) _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 O3 1.4332(19) . ? S1 O2 1.4372(19) . ? S1 N1 1.690(2) . ? S1 C17 1.752(3) . ? Cl1 C1 1.751(3) . ? O1 N1 1.437(3) . ? O1 C13 1.467(3) . ? N1 C11 1.484(3) . ? C22 H22 0.9500 . ? C22 C17 1.390(4) . ? C22 C21 1.380(4) . ? C17 C18 1.386(3) . ? C4 C5 1.397(4) . ? C4 C3 1.391(4) . ? C4 C7 1.488(4) . ? C20 C21 1.394(4) . ? C20 C19 1.383(4) . ? C20 C23 1.509(4) . ? C5 H5 0.9500 . ? C5 C6 1.384(4) . ? C3 H3 0.9500 . ? C3 C2 1.380(4) . ? C7 C12 1.519(4) . ? C7 C8 1.329(4) . ? C21 H21 0.9500 . ? C12 H12 1.0000 . ? C12 C11 1.534(4) . ? C12 C13 1.533(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.511(4) . ? C10 C9 1.523(4) . ? C11 H11 1.0000 . ? C13 H13 1.0000 . ? C13 C14 1.483(4) . ? C6 H6 0.9500 . ? C6 C1 1.383(4) . ? C18 H18 0.9500 . ? C18 C19 1.389(4) . ? C2 H2 0.9500 . ? C2 C1 1.378(4) . ? C19 H19 0.9500 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C8 1.506(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C14 H14 1.0000 . ? C14 C16 1.518(4) . ? C14 C15 1.506(4) . ? C8 H8 0.9500 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C15 1.500(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? 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 O3 S1 O2 118.94(13) . . ? O3 S1 N1 103.62(11) . . ? O3 S1 C17 110.35(12) . . ? O2 S1 N1 113.97(12) . . ? O2 S1 C17 109.33(12) . . ? N1 S1 C17 98.69(12) . . ? N1 O1 C13 110.17(18) . . ? O1 N1 S1 106.83(15) . . ? O1 N1 C11 107.68(19) . . ? C11 N1 S1 116.21(18) . . ? C17 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C21 C22 C17 119.4(2) . . ? C22 C17 S1 118.30(19) . . ? C18 C17 S1 120.9(2) . . ? C18 C17 C22 120.8(2) . . ? C5 C4 C7 120.9(3) . . ? C3 C4 C5 117.7(3) . . ? C3 C4 C7 121.4(3) . . ? C21 C20 C23 119.5(2) . . ? C19 C20 C21 118.5(2) . . ? C19 C20 C23 122.0(2) . . ? C4 C5 H5 119.1 . . ? C6 C5 C4 121.7(3) . . ? C6 C5 H5 119.1 . . ? C4 C3 H3 119.2 . . ? C2 C3 C4 121.6(3) . . ? C2 C3 H3 119.2 . . ? C4 C7 C12 116.8(2) . . ? C8 C7 C4 120.8(2) . . ? C8 C7 C12 122.4(2) . . ? C22 C21 C20 121.0(2) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C7 C12 H12 108.9 . . ? C7 C12 C11 113.2(2) . . ? C7 C12 C13 113.1(2) . . ? C11 C12 H12 108.9 . . ? C13 C12 H12 108.9 . . ? C13 C12 C11 103.6(2) . . ? H10A C10 H10B 108.2 . . ? C11 C10 H10A 109.7 . . ? C11 C10 H10B 109.7 . . ? C11 C10 C9 109.6(2) . . ? C9 C10 H10A 109.7 . . ? C9 C10 H10B 109.7 . . ? N1 C11 C12 104.30(19) . . ? N1 C11 C10 108.7(2) . . ? N1 C11 H11 110.3 . . ? C12 C11 H11 110.3 . . ? C10 C11 C12 112.9(2) . . ? C10 C11 H11 110.3 . . ? O1 C13 C12 105.5(2) . . ? O1 C13 H13 108.7 . . ? O1 C13 C14 108.4(2) . . ? C12 C13 H13 108.7 . . ? C14 C13 C12 116.7(2) . . ? C14 C13 H13 108.7 . . ? C5 C6 H6 120.8 . . ? C1 C6 C5 118.3(3) . . ? C1 C6 H6 120.8 . . ? C17 C18 H18 120.6 . . ? C17 C18 C19 118.8(2) . . ? C19 C18 H18 120.6 . . ? C3 C2 H2 120.5 . . ? C1 C2 C3 118.9(3) . . ? C1 C2 H2 120.5 . . ? C20 C19 C18 121.5(2) . . ? C20 C19 H19 119.2 . . ? C18 C19 H19 119.2 . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C8 C9 C10 110.6(2) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C6 C1 Cl1 119.3(2) . . ? C2 C1 Cl1 119.0(2) . . ? C2 C1 C6 121.7(3) . . ? C13 C14 H14 116.0 . . ? C13 C14 C16 118.8(3) . . ? C13 C14 C15 118.6(3) . . ? C16 C14 H14 116.0 . . ? C15 C14 H14 116.0 . . ? C15 C14 C16 59.4(2) . . ? C7 C8 C9 123.7(3) . . ? C7 C8 H8 118.2 . . ? C9 C8 H8 118.2 . . ? C14 C16 H16A 117.8 . . ? C14 C16 H16B 117.8 . . ? H16A C16 H16B 114.9 . . ? C15 C16 C14 59.9(2) . . ? C15 C16 H16A 117.8 . . ? C15 C16 H16B 117.8 . . ? C14 C15 H15A 117.7 . . ? C14 C15 H15B 117.7 . . ? C16 C15 C14 60.7(2) . . ? C16 C15 H15A 117.7 . . ? C16 C15 H15B 117.7 . . ? H15A C15 H15B 114.8 . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -1 0 0 56.09 6.8 1 0 0 50.09 6.6 -2 0 0 2007.1 142.19 -2 0 0 1660.53 140.59 2 0 0 1745.73 141.49 -3 0 0 1097.79 89.19 -3 0 0 1176.68 91.19 -3 0 0 1121.29 92.09 3 0 0 1003.1 91.39 -4 0 0 1246.68 103.09 -4 0 0 1277.77 101.79 -4 0 0 1196.48 92.69 4 0 0 1108.19 102.19 -5 0 0 301.97 34.1 -5 0 0 279.87 32.5 5 0 0 275.77 33.7 -6 0 0 260.97 32.4 -6 0 0 272.17 34.7 -7 0 0 111.49 23 -7 0 0 81.29 21.9 -8 0 0 29.4 15.3 -8 0 0 12.2 14.9 -9 1 0 598.44 67.89 -9 1 0 539.75 60.59 -8 1 0 269.67 32.8 -8 1 0 172.78 36.5 -7 1 0 425.46 49.7 -7 1 0 421.66 45.7 -6 1 0 108.69 23.5 -6 1 0 130.89 13.6 -6 1 0 125.89 19.3 -5 1 0 869.81 74.99 -5 1 0 807.32 78.09 -5 1 0 880.61 76.69 -4 1 0 147.99 17.7 -4 1 0 136.69 21.9 3 -1 0 3.9 4.7 -3 1 0 -2.8 5.3 -3 1 0 10.5 4.8 2 -1 0 2932.71 249.08 -2 1 0 3348.66 250.57 1 -1 0 81.39 13.5 1 -1 0 89.09 7.7 -1 1 0 83.59 7.5 -1 1 0 82.19 13.7 -1 -1 0 299.77 27.8 -1 -1 0 313.77 29.2 -1 -1 0 294.77 26.9 1 1 0 330.47 27.5 1 1 0 301.27 27.1 -2 -1 0 286.37 28 -2 -1 0 293.27 26.1 -2 -1 0 284.67 27.4 2 1 0 256.87 27.2 -3 -1 0 6749.72 513.85 -3 -1 0 7231.18 515.25 3 1 0 6039.2 513.55 -4 -1 0 28.2 9.4 -4 -1 0 25.7 9.8 4 1 0 15.8 5.7 -5 -1 0 1056.89 85.29 -5 -1 0 924.21 83.59 5 1 0 761.52 82.49 -6 -1 0 521.05 52.19 -6 -1 0 474.55 52.19 6 1 0 428.16 51.49 -7 -1 0 237.28 35 -7 -1 0 212.28 36.3 -8 -1 0 45.3 15.4 -9 2 0 1.4 11.6 -9 2 0 18.8 13 -9 2 0 -6.6 11.4 -8 2 0 284.37 43.1 -8 2 0 375.46 39.5 -7 2 0 59.29 13.9 -7 2 0 37.4 11.1 -7 2 0 56.99 16.4 -6 2 0 709.13 64.79 -6 2 0 654.43 70.69 -6 2 0 810.92 74.99 -5 2 0 508.35 45.6 -5 2 0 468.05 50.99 -5 2 0 532.75 58.29 4 -2 0 102.99 26.9 -4 2 0 144.89 19.3 -4 2 0 132.39 25.5 3 -2 0 454.65 58.39 -3 2 0 604.04 62.69 -3 2 0 597.34 46.6 2 -2 0 9111.09 665.83 2 -2 0 7528.65 680.63 -2 2 0 9528.45 665.43 -2 2 0 8874.01 683.83 1 -2 0 2421.66 223.78 1 -2 0 2914.01 211.18 -1 2 0 2925.81 211.18 -1 2 0 2723.33 211.68 0 -2 0 1637.34 124.39 0 -2 0 1400.06 133.29 0 -2 0 1585.94 122.79 0 2 0 1662.33 134.19 0 2 0 1530.85 124.29 0 2 0 1671.63 122.99 -1 -2 0 0.8 2.9 -1 -2 0 -0.2 2.6 -1 -2 0 -0.7 4.6 1 2 0 0.8 3.4 1 2 0 3.7 4.8 -2 -2 0 803.02 67.19 -2 -2 0 736.43 71.59 -2 -2 0 809.22 69.29 2 2 0 827.72 66.49 2 2 0 791.72 67.79 -3 -2 0 908.41 74.59 -3 -2 0 797.22 73.79 -3 -2 0 975.9 77.59 3 2 0 764.02 74.19 -4 -2 0 56.59 15 -4 -2 0 37.2 10.8 4 2 0 18.2 8.1 -5 -2 0 15.9 7.6 -5 -2 0 -2.4 5.3 5 2 0 -0.4 4.7 -6 -2 0 535.45 70.09 -6 -2 0 458.45 53.29 -7 -2 0 21.9 13.8 -8 -2 0 -14.4 8.1 -9 3 0 805.22 89.29 -9 3 0 886.81 78.19 -8 3 0 89.29 20.4 -8 3 0 98.29 21.9 -8 3 0 112.49 20.6 -8 3 0 73.09 22.3 -7 3 0 242.48 36.7 -7 3 0 188.88 26.6 -7 3 0 255.67 41.2 -7 3 0 219.88 24.7 6 -3 0 8.1 16.2 -6 3 0 8.6 14.6 -6 3 0 11.3 8.3 -6 3 0 20.6 6.5 -6 3 0 6.8 6.6 -5 3 0 2.5 6.1 -5 3 0 7 3.5 -5 3 0 1.6 4 -5 3 0 -2.8 4.8 4 -3 0 28.1 16.8 -4 3 0 27.6 15.2 -4 3 0 22.9 5.5 3 -3 0 565.34 71.79 -3 3 0 694.13 52.39 -3 3 0 683.43 75.59 2 -3 0 -4.8 6.5 2 -3 0 2.3 1.7 -2 3 0 0.8 1.9 -2 3 0 2.1 8.5 1 -3 0 16.7 4.6 1 -3 0 20.2 5.2 1 -3 0 10.5 9.3 -1 3 0 17.3 11.8 -1 3 0 15.3 4.7 -1 3 0 21.1 5.4 0 -3 0 13.6 5.4 0 -3 0 7.2 7.4 0 -3 0 9.9 3.7 0 3 0 5.3 3.9 0 3 0 3 3.3 0 3 0 10.7 8.9 -1 -3 0 315.87 43.7 -1 -3 0 376.06 35.7 -1 -3 0 354.76 32.7 1 3 0 394.86 42.5 1 3 0 348.37 33.2 -2 -3 0 342.97 36.1 -2 -3 0 309.47 42.4 -2 -3 0 343.47 33.5 2 3 0 312.47 34 2 3 0 394.46 37.7 -3 -3 0 390.56 40.5 -3 -3 0 324.07 42.4 -3 -3 0 394.56 37.3 3 3 0 361.16 34.1 3 3 0 314.87 36.6 -4 -3 0 424.36 40.5 -4 -3 0 376.26 42.3 -4 -3 0 348.07 37.2 4 3 0 299.37 39 -5 -3 0 94.79 19.8 -5 -3 0 97.89 23.7 5 3 0 100.59 22.7 -6 -3 0 46.6 14.7 -7 -3 0 100.49 23.9 -9 4 0 40.3 11.1 -9 4 0 29.3 10.4 -9 4 0 34.7 15.2 -9 4 0 -0.8 13.3 -8 4 0 19.9 14.1 -8 4 0 13.1 14.2 -8 4 0 4.9 6.1 -8 4 0 5.1 6.7 7 -4 0 28.2 19.7 -7 4 0 23.8 17.8 -7 4 0 21.7 7.2 -7 4 0 25.3 6.3 -7 4 0 2.3 8 6 -4 0 254.07 52.89 -6 4 0 422.86 33.3 -6 4 0 380.46 58.69 -6 4 0 406.46 46.2 -6 4 0 372.96 33.5 5 -4 0 45.8 21.9 -5 4 0 51.69 6.6 -5 4 0 63.99 26 4 -4 0 52.39 27.4 -4 4 0 73.09 7.9 -4 4 0 78.99 28.5 3 -4 0 17.7 13.6 3 -4 0 3.4 2.9 -3 4 0 6.8 2.9 -3 4 0 1.1 6.9 2 -4 0 346.27 30.1 2 -4 0 274.07 46.2 -2 4 0 337.97 30.1 -2 4 0 350.76 50.79 -2 4 0 324.47 30.9 1 -4 0 331.57 30.2 1 -4 0 265.67 45.3 1 -4 0 326.47 30.8 -1 4 0 326.97 31.3 -1 4 0 342.87 48.5 -1 4 0 338.37 30 0 -4 0 4069.19 320.77 0 -4 0 3875.61 342.27 0 -4 0 4179.08 318.47 0 4 0 4338.07 318.77 0 4 0 4189.88 339.47 0 4 0 4091.69 321.77 -1 -4 0 398.06 38.2 -1 -4 0 389.86 55.19 -1 -4 0 410.66 41.6 1 4 0 437.06 39.7 1 4 0 445.76 51.59 -2 -4 0 59.89 12.4 -2 -4 0 64.19 14.9 -2 -4 0 39.9 19.3 2 4 0 52.29 12.1 2 4 0 69.69 18 -3 -4 0 387.06 54.29 -3 -4 0 457.75 48.2 -3 -4 0 498.95 45 3 4 0 454.05 44.6 3 4 0 397.46 44.9 -4 -4 0 57.19 19 -4 -4 0 67.69 16.1 4 4 0 62.79 12.3 -5 -4 0 67.39 20.4 -5 -4 0 96.49 24.4 -6 -4 0 3.6 4.4 -7 -4 0 3.6 9.8 -9 5 0 321.67 48.5 -9 5 0 198.88 44.6 -8 5 0 353.36 56.89 -8 5 0 228.88 43.9 7 -5 0 -1.4 14.1 -7 5 0 3.4 14 -7 5 0 -7.2 7.5 6 -5 0 356.36 62.49 -6 5 0 417.76 64.29 5 -5 0 372.16 66.19 -5 5 0 498.05 73.49 -5 5 0 482.55 37.2 4 -5 0 43.5 8.4 4 -5 0 42.9 23.5 -4 5 0 71.89 30.8 -4 5 0 71.69 8.3 3 -5 0 359.16 32.9 3 -5 0 281.47 52.79 -3 5 0 382.56 68.39 -3 5 0 367.06 32.7 -3 5 0 380.86 35.9 2 -5 0 241.58 54.49 2 -5 0 243.28 24.6 -2 5 0 237.88 24.9 -2 5 0 248.08 25.1 -2 5 0 222.88 42.6 1 -5 0 42.3 10 1 -5 0 37.4 9 1 -5 0 41.9 22 -1 5 0 45.1 9 -1 5 0 34.2 9.9 -1 5 0 38.5 20.4 0 -5 0 652.43 59.39 0 -5 0 563.84 79.09 0 -5 0 695.73 58.39 0 5 0 659.83 60.69 0 5 0 664.93 57.09 0 5 0 642.44 76.79 -1 -5 0 8 19.9 -1 -5 0 12.4 6.8 -1 -5 0 10.9 5.2 1 5 0 6.6 9.8 1 5 0 9.9 4.8 -2 -5 0 1218.98 99.29 -2 -5 0 1011.2 119.39 -2 -5 0 1259.17 104.89 2 5 0 1170.58 100.79 -3 -5 0 1548.95 125.99 -3 -5 0 1301.17 143.09 3 5 0 1693.33 131.59 3 5 0 1369.86 127.49 -4 -5 0 124.99 31.9 -4 -5 0 159.48 25.8 -4 -5 0 134.09 27.9 4 5 0 129.89 19.1 -5 -5 0 396.66 44.9 -6 -5 0 465.05 52.79 -7 -5 0 -14.9 10.4 -9 6 0 32.8 21.4 -9 6 0 -28.2 11 8 -6 0 73.59 45.3 -8 6 0 213.48 53.29 -8 6 0 118.89 29 7 -6 0 390.56 83.99 6 -6 0 121.69 46.7 -6 6 0 190.98 53.49 -5 6 0 671.43 53.19 -5 6 0 593.14 90.49 4 -6 0 152.48 17.5 4 -6 0 117.39 42.6 -4 6 0 140.29 20.7 -4 6 0 170.58 17.8 -4 6 0 155.18 46.5 3 -6 0 945.31 125.09 3 -6 0 1122.79 95.19 -3 6 0 1159.08 129.09 -3 6 0 1258.87 96.49 -3 6 0 1236.98 98.09 2 -6 0 2303.27 244.88 2 -6 0 2483.35 210.78 2 -6 0 2653.53 211.08 -2 6 0 2945.31 250.77 -2 6 0 2825.82 211.18 -2 6 0 2825.32 213.18 1 -6 0 9.7 4.9 1 -6 0 9.2 4.9 1 -6 0 -4.9 9.9 -1 6 0 22.3 16.1 -1 6 0 -0.4 3.4 0 -6 0 56.09 29.4 0 -6 0 96.79 18.5 0 -6 0 94.29 15.7 0 6 0 86.79 15.1 0 6 0 91.59 29.5 -1 -6 0 1602.54 173.28 -1 -6 0 1673.93 140.39 -1 -6 0 1691.73 145.19 1 6 0 1657.93 141.59 1 6 0 2012.2 168.28 -2 -6 0 394.96 40.7 -2 -6 0 338.87 60.19 2 6 0 456.75 64.49 -3 -6 0 647.44 66.49 -3 -6 0 620.44 59.89 -3 -6 0 498.85 78.29 3 6 0 563.34 61.89 3 6 0 722.93 69.09 -4 -6 0 70.09 13.8 -4 -6 0 45.6 22 4 6 0 74.39 18.5 -5 -6 0 8.1 8.8 -6 -6 0 107.69 24.2 9 -7 0 30.4 43.1 -9 7 0 53.39 20.4 -9 7 0 103.89 39 8 -7 0 102.59 42.1 -8 7 0 210.48 58.29 7 -7 0 278.47 70.49 6 -7 0 35.9 23.5 -6 7 0 46.3 32.3 5 -7 0 154.78 19.1 5 -7 0 133.29 47.8 -5 7 0 250.97 63.09 -5 7 0 206.58 20.2 -5 7 0 217.88 26.1 4 -7 0 89.59 14 4 -7 0 72.89 30.7 -4 7 0 103.19 19.3 -4 7 0 105.99 39.3 -4 7 0 137.29 16.1 3 -7 0 184.38 54.29 -3 7 0 245.38 28 -3 7 0 253.97 27.8 -3 7 0 269.57 63.59 2 -7 0 41.6 10.7 2 -7 0 41.5 11 2 -7 0 29 21.1 -2 7 0 45.3 12.8 -2 7 0 49.2 26.8 -2 7 0 57.19 12.4 1 -7 0 80.19 16 1 -7 0 51.19 32.2 1 -7 0 92.89 18 -1 7 0 106.09 16.9 -1 7 0 125.79 39.7 -1 7 0 70.39 16.8 0 -7 0 6.6 5.5 0 -7 0 8.6 16.7 0 -7 0 5.2 6.8 0 7 0 10.5 12.6 0 7 0 5.7 6.1 -1 -7 0 1120.29 112.59 -1 -7 0 1137.39 140.49 -1 -7 0 1331.57 108.59 1 7 0 1550.44 139.09 1 7 0 1231.68 109.39 -2 -7 0 33.9 21.1 -2 -7 0 6 6.7 -2 -7 0 -8.1 7.4 2 7 0 5.1 11.5 -3 -7 0 32.4 27.3 -3 -7 0 72.79 16.7 3 7 0 65.39 21 -4 -7 0 123.39 39.8 -4 -7 0 177.48 23.2 -5 -7 0 -9.2 11.4 -9 8 0 25.7 33 -8 8 0 56.69 34.1 7 -8 0 690.53 110.39 6 -8 0 55.79 9.9 6 -8 0 72.99 36.3 -6 8 0 116.09 23.1 -6 8 0 92.89 41.7 5 -8 0 412.36 41.2 5 -8 0 367.26 87.79 -5 8 0 514.05 48.9 -5 8 0 474.35 82.59 4 -8 0 687.53 113.39 4 -8 0 947.71 84.89 -4 8 0 1068.39 130.09 -4 8 0 977.7 84.59 -4 8 0 1006.7 83.19 3 -8 0 7.7 4.1 3 -8 0 -9.6 12.8 -3 8 0 2.2 14.9 -3 8 0 -5.4 4.4 -3 8 0 -1.1 4.7 2 -8 0 763.92 114.79 2 -8 0 830.62 77.69 2 -8 0 816.42 77.89 -2 8 0 997.4 78.89 -2 8 0 1013.6 119.19 1 -8 0 1387.06 119.99 1 -8 0 1377.06 118.09 1 -8 0 1278.87 158.88 -1 8 0 1558.34 158.28 0 -8 0 -2.3 18.5 0 -8 0 19.5 7.3 0 -8 0 13.9 6.9 0 8 0 26.8 19.8 0 8 0 8.6 7.8 -1 -8 0 39.7 12.2 -1 -8 0 11.2 21.1 1 8 0 56.89 25.5 -2 -8 0 -24.8 18.7 -2 -8 0 8.4 6.7 2 8 0 14.5 15 -3 -8 0 257.47 34 -3 -8 0 240.58 66.09 3 8 0 328.07 47.8 -4 -8 0 65.49 36.4 -4 -8 0 62.49 16.6 4 8 0 48.9 18.1 -5 -8 0 -2.1 7.9 -9 9 0 62.29 37.8 -8 9 0 305.27 82.49 -7 9 0 57.89 38.9 6 -9 0 102.89 14.4 -6 9 0 87.89 48.6 5 -9 0 27.6 10.1 -5 9 0 26.3 11.3 -5 9 0 19.1 21.3 4 -9 0 216.68 27.3 4 -9 0 185.98 53.69 -4 9 0 248.58 29.6 -4 9 0 301.27 74.09 3 -9 0 -16.6 21.3 3 -9 0 30.3 10.4 -3 9 0 29.7 25.6 -3 9 0 63.39 12.6 2 -9 0 -3.3 5.5 2 -9 0 -5.8 20.5 2 -9 0 -1.1 5.4 -2 9 0 1 5.2 -2 9 0 -0.4 12.3 1 -9 0 489.15 54.89 1 -9 0 588.84 55.19 1 -9 0 494.65 91.79 -1 9 0 581.74 54.49 0 -9 0 73.69 19.6 0 -9 0 33.8 34.5 0 9 0 148.69 45.7 -1 -9 0 -4.6 4.2 -1 -9 0 -19.8 26.1 1 9 0 10.7 12.6 -2 -9 0 247.28 31.9 -2 -9 0 198.58 65.79 2 9 0 275.77 59.49 -3 -9 0 -9.5 32.5 -3 -9 0 12.9 11.3 3 9 0 19.1 15.6 -4 -9 0 8.3 29 -4 -9 0 13.9 13.5 4 9 0 31.9 21.4 -9 10 0 5.2 37.4 -8 10 0 10 32.2 -7 10 0 191.48 67.89 6 -10 0 54.19 13.4 -6 10 0 96.69 43.5 5 -10 0 71.49 15.5 -5 10 0 90.99 38.8 4 -10 0 13.6 9.2 -4 10 0 29.9 32.7 3 -10 0 207.78 28.4 -3 10 0 224.28 67.49 2 -10 0 118.89 24.1 2 -10 0 94.39 22.5 -2 10 0 139.09 56.89 1 -10 0 497.65 54.89 -1 10 0 647.64 94.29 0 -10 0 19.1 10.9 0 10 0 12.4 22.2 -1 -10 0 57.79 16.8 1 10 0 59.09 29.8 -2 -10 0 -3.4 6.3 2 10 0 2.6 15.8 -3 -10 0 158.18 46.2 -3 -10 0 30.8 11.2 3 10 0 52.79 30.7 -8 11 0 30.5 38.1 7 -11 0 11 8 -7 11 0 -6.9 34.5 6 -11 0 5.9 9.5 -6 11 0 24.8 31.1 5 -11 0 37.9 12.6 -5 11 0 69.59 35.4 4 -11 0 18.2 11.5 -4 11 0 25.9 26.7 3 -11 0 132.99 25.8 -3 11 0 235.78 70.59 2 -11 0 41.6 13.5 -2 11 0 64.29 33.8 1 -11 0 57.79 15.4 -1 11 0 65.49 36.4 0 -11 0 42.8 14.2 0 11 0 54.09 33.1 -1 -11 0 178.58 32.1 1 11 0 272.27 67.39 -2 -11 0 103.89 26.5 2 11 0 87.39 35.2 -7 12 0 211.38 74.79 6 -12 0 14 13.9 -6 12 0 66.59 39.7 -5 12 0 188.48 66.99 4 -12 0 294.77 38.2 -4 12 0 374.96 91.89 -3 12 0 39.3 35.5 2 -12 0 121.49 27.5 -2 12 0 204.58 62.39 1 -12 0 105.99 22.7 -1 12 0 126.69 53.69 0 -12 0 47.8 21 0 12 0 5.6 26.1 -6 13 0 102.49 56.69 -4 13 0 92.69 47.8 -3 13 0 -3.3 18.2 2 -13 0 16.9 13.2 -2 13 0 32.1 30.8 -1 13 -1 15.1 23.3 1 -13 1 -14.3 8 -2 13 -1 219.28 67.39 2 -13 1 100.59 24.3 -3 13 -1 31.3 36.9 -4 13 -1 38.2 39.4 -5 13 -1 184.58 65.59 5 -13 1 89.69 22.7 -6 13 -1 -39.6 32.2 6 -13 1 -11.4 13.3 1 12 -1 16.3 26.3 -1 -12 1 25 13 0 -12 1 370.86 45.2 -1 12 -1 -11.2 20.9 1 -12 1 -9.3 6.7 2 -12 1 519.85 56.69 -3 12 -1 369.16 90.89 -4 12 -1 -16.7 22.4 4 -12 1 12.5 8.9 -5 12 -1 25.1 30.7 5 -12 1 53.19 14.8 -6 12 -1 17.5 24.1 6 -12 1 -2.1 10.2 -7 12 -1 6.4 33 7 -12 1 0.7 5.1 2 11 -1 80.49 40.1 -1 -11 1 8.3 9.1 0 11 -1 184.98 53.79 0 -11 1 113.79 25.2 -1 11 -1 43.7 26.4 -2 11 -1 19 25.3 2 -11 1 28.8 10.7 3 -11 1 366.36 41.4 -4 11 -1 13.7 22.7 4 -11 1 3 8.1 -5 11 -1 236.08 73.79 5 -11 1 167.08 24 -6 11 -1 197.98 67.69 6 -11 1 142.69 19.9 -7 11 -1 50.09 43.2 -8 11 -1 10.6 27.9 3 10 -1 124.09 32.1 -3 -10 1 76.09 20 -3 -10 1 85.89 41.7 2 10 -1 678.63 85.59 -2 -10 1 553.14 61.49 1 10 -1 -3.2 16.3 -1 -10 1 0 5.8 0 10 -1 195.88 56.09 0 -10 1 201.88 28.5 -1 10 -1 12.8 16.1 1 -10 1 8.6 7.5 1 -10 1 25.6 8.4 2 -10 1 458.65 49.6 -3 10 -1 32.7 41.4 3 -10 1 10.7 6.7 -4 10 -1 381.76 87.89 4 -10 1 249.88 29.8 -5 10 -1 7.3 18.4 5 -10 1 8.1 6.1 -6 10 -1 15 20.5 6 -10 1 15.9 5.9 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-5 3 13 81.99 24.5 -5 3 13 59.29 28.4 -4 3 13 152.08 64.29 -4 3 13 123.29 30.5 3 -3 -13 50.89 9.1 -3 3 13 89.49 46.8 -3 3 13 66.69 22.7 2 -3 -13 33 8.8 -2 3 13 41.4 16.6 -2 3 13 -20.5 31.2 1 -3 -13 32.4 10.6 -1 3 13 18.1 14.6 -1 3 13 36.1 37.5 0 -3 -13 15.7 10.1 0 3 13 -0.1 35.2 0 3 13 40.9 19.8 -7 4 13 14.7 14.7 -7 4 13 24.4 33.1 -6 4 13 88.89 25.6 -6 4 13 53.59 46.1 -5 4 13 108.89 64.89 -5 4 13 185.98 39.3 -4 4 13 157.68 22.1 -4 4 13 38 41.5 -3 4 13 40.5 36.2 -3 4 13 24.1 14.1 2 -4 -13 44.3 11.3 -2 4 13 20.7 51.09 1 -4 -13 275.47 30.4 -1 4 13 201.58 58.89 -1 4 13 229.78 47.5 -6 5 13 90.49 48.9 -6 5 13 33.3 21.1 -5 5 13 -16.2 15.1 -4 5 13 51.19 13.4 -4 5 13 65.99 57.69 3 -5 -13 1.4 7.2 -3 5 13 10.8 10 -3 5 13 44 14.5 -3 5 13 -27.3 35.2 -1 -10 14 53.79 22.2 0 -10 14 124.59 28.3 -3 -9 14 -25.4 17.6 2 9 -14 28.9 15.6 -2 -9 14 13.7 20.4 -1 -9 14 112.59 34.3 0 -9 14 76.09 22.4 1 -9 14 23.8 12.9 4 8 -14 -1.5 12.5 -4 -8 14 -12.6 23.7 3 8 -14 158.08 23.2 -3 -8 14 158.18 43.5 2 8 -14 -21.5 9.1 -2 -8 14 -12.4 11.3 1 8 -14 37.5 15.9 -1 -8 14 53.59 19.7 0 8 -14 61.89 17.7 0 -8 14 63.39 18.3 1 -8 14 46.4 19.3 -2 8 -14 119.09 28.3 2 -8 14 135.29 28.3 5 7 -14 4 8.4 -5 -7 14 4.6 22.8 4 7 -14 9.9 8.9 -4 -7 14 10 23.3 3 7 -14 4.8 7.9 -3 -7 14 -28.4 14 2 7 -14 29.4 11.9 -2 -7 14 53.19 18.5 1 7 -14 -4.1 7.6 -1 -7 14 5.3 14.7 0 7 -14 8.4 10.5 0 -7 14 2.3 11.9 -1 7 -14 21.3 15.2 1 -7 14 18.5 14.8 -2 7 -14 71.49 19.8 2 -7 14 78.69 17.6 -6 -6 14 31.9 24.2 5 6 -14 158.08 18.4 -5 -6 14 208.18 46.4 4 6 -14 68.29 11.2 -4 -6 14 54.89 25.7 -3 -6 14 115.09 30.6 2 6 -14 62.89 11.8 -2 -6 14 66.39 25.5 1 6 -14 21.7 9.9 1 6 -14 30.8 9.6 -1 -6 14 18.3 16.2 0 6 -14 -9.3 8 0 6 -14 -6.4 12.6 0 -6 14 7.5 10.7 -1 6 -14 10.6 7.5 1 -6 14 -12.8 9.8 -2 6 -14 -13.2 10.1 2 -6 14 -2.3 10.7 -6 -5 14 183.28 51.69 -5 -5 14 56.89 27.5 -4 -5 14 24.6 21.5 3 5 -14 1.4 4 3 5 -14 6.5 4.7 -3 -5 14 18.4 12.4 2 5 -14 2.7 5.9 -2 -5 14 -3.8 8.8 1 5 -14 21 7.9 1 5 -14 29.6 9.3 -1 -5 14 28 14.4 0 5 -14 3.2 7.5 0 5 -14 -4.4 11 0 -5 14 -1.3 9.8 -1 5 -14 132.09 24.1 1 -5 14 141.29 31.5 -2 5 -14 25.3 14.8 2 -5 14 27.6 13.9 -7 -4 14 0.8 15.5 -6 -4 14 23.6 19.7 -5 -4 14 37.5 17.1 -4 -4 14 33.4 21.6 -3 -4 14 36.6 18 2 4 -14 208.18 19.3 2 4 -14 154.88 19 -2 -4 14 164.18 39.9 1 4 -14 -2.9 6 1 4 -14 3.7 7.5 -1 -4 14 27.9 15.8 0 4 -14 398.36 40.8 0 -4 14 372.86 50.19 -1 4 -14 199.28 29.1 1 -4 14 253.37 35.5 -2 4 -14 261.27 37.3 2 -4 14 351.46 41.7 -7 -3 14 64.59 33.6 -6 -3 14 62.19 23.3 -5 -3 14 16.4 11.7 -4 -3 14 368.16 55.59 -3 -3 14 11.5 10.6 2 3 -14 2.8 3.8 2 3 -14 10.7 4.6 -2 -3 14 8.2 11.3 1 3 -14 -7.8 5 -1 -3 14 -4.2 8.4 0 3 -14 199.18 24.8 0 -3 14 163.28 35.6 -1 3 -14 51.29 12.9 1 -3 14 69.79 21.9 -2 3 -14 15.1 10.7 2 -3 14 30.3 14.8 -7 -2 14 -1.1 14.3 -6 -2 14 14.6 18.5 -5 -2 14 579.54 73.69 -4 -2 14 227.78 46.6 -3 -2 14 17.2 10.9 2 2 -14 392.96 33.9 2 2 -14 426.86 35.1 -2 -2 14 372.96 52.99 1 2 -14 147.69 18.9 -1 -2 14 170.18 34.1 0 2 -14 61.89 15.1 0 -2 14 107.29 26 1 -2 14 65.99 18.5 -7 -1 14 -0.7 17.3 -6 -1 14 56.69 19.7 -5 -1 14 -5.7 15.9 -4 -1 14 31.9 15.7 -3 -1 14 97.39 25.4 -2 -1 14 39.1 14.3 1 1 -14 27.9 8.4 -1 -1 14 63.29 19.5 0 1 -14 21.3 8.6 0 -1 14 7.9 15.7 1 -1 14 113.59 30 -7 0 14 -3.5 35.4 -7 0 14 96.49 28.8 -6 0 14 52.09 22.1 -5 0 14 92.99 28.9 -4 0 14 48.2 19.3 -3 0 14 62.09 24.7 2 0 -14 45.3 7.6 -2 0 14 87.39 23.1 1 0 -14 20 8.2 -1 0 14 22.2 15.6 0 0 -14 61.59 14.7 0 0 14 61.89 21.6 -7 1 14 78.39 57.39 -7 1 14 39.7 24 -6 1 14 6.6 13.7 -5 1 14 -30 31.7 -5 1 14 9.4 10.4 -4 1 14 43.8 38 -4 1 14 13.8 15 -3 1 14 35.1 41.8 -3 1 14 41.9 18.6 2 -1 -14 -8.4 4.2 -2 1 14 -9.4 25.6 -2 1 14 -0.7 10.3 1 -1 -14 85.89 15 -1 1 14 129.19 32 -1 1 14 70.39 45 0 -1 -14 -2 7.9 0 1 14 -8.2 12 0 1 14 -30.7 30.7 -7 2 14 29.2 20.4 -7 2 14 92.39 72.39 -6 2 14 66.39 24.8 -6 2 14 74.19 57.59 -5 2 14 112.09 70.29 -4 2 14 88.69 27.1 -4 2 14 102.49 50.69 3 -2 -14 1.4 3.5 -3 2 14 -5.8 31 -3 2 14 1.1 11.8 2 -2 -14 140.39 18.1 -2 2 14 111.29 55.59 -2 2 14 216.78 41.8 1 -2 -14 48.5 11.9 -1 2 14 46.8 44 -7 3 14 60.89 32.5 -7 3 14 103.59 56.79 -6 3 14 75.09 56.89 -5 3 14 29.4 19.8 -5 3 14 17.5 19.4 -4 3 14 35.2 21.1 -4 3 14 27 29.2 3 -3 -14 31.1 8 -3 3 14 -7.8 39.9 -3 3 14 70.79 35.8 2 -3 -14 8.2 6.4 -2 3 14 3.6 11.6 -2 3 14 -16 42.8 -5 4 14 7.7 46.8 -5 4 14 0.1 11.6 -4 4 14 73.79 62.89 -4 4 14 29.2 19.7 3 8 -15 143.49 21.6 -3 -8 15 93.69 34 2 8 -15 1.8 12.2 -2 -8 15 10.8 20.5 1 8 -15 129.69 24.7 -1 -8 15 72.29 23.7 0 -8 15 60.99 20.8 -4 -7 15 -49.6 18.3 3 7 -15 -6 8.5 -3 -7 15 11.4 14.8 2 7 -15 -8.8 8 -2 -7 15 -3.2 18.2 1 7 -15 68.59 16 1 7 -15 57.69 13.6 -1 -7 15 39.5 23.4 0 7 -15 15.1 12.8 0 7 -15 12.1 14.2 0 -7 15 -4.1 14.3 -1 7 -15 15.2 14.6 1 -7 15 -7.9 10.4 -5 -6 15 45.6 27.5 4 6 -15 200.88 20.3 4 6 -15 234.58 20 -4 -6 15 258.97 54.59 3 6 -15 49.2 9.7 3 6 -15 57.09 11.1 -3 -6 15 96.29 31.9 2 6 -15 9.5 7.6 2 6 -15 36.1 9.7 -2 -6 15 34.8 20.6 1 6 -15 15.7 12.1 1 6 -15 49.5 13.2 -1 -6 15 45.1 21 0 6 -15 52.69 15 0 6 -15 35.8 17.4 0 -6 15 92.09 23.6 -1 6 -15 251.87 36.4 1 -6 15 260.87 39.6 -4 -5 15 -4.5 13 3 5 -15 16.4 4.1 3 5 -15 30.3 4.5 -3 -5 15 42.4 22.9 -2 -5 15 3.1 14.8 1 5 -15 62.79 15.4 1 5 -15 29.1 11.4 -1 -5 15 15.8 18.1 0 5 -15 19.1 9.5 0 -5 15 -17.7 11.7 -1 5 -15 26.7 18.1 1 -5 15 39.5 16.8 -6 -4 15 97.89 34.9 -5 -4 15 134.59 35.2 -4 -4 15 706.13 87.69 -3 -4 15 59.49 24 2 4 -15 14.2 5.2 2 4 -15 25.6 6.4 -2 -4 15 13.1 16.8 1 4 -15 35.5 11 1 4 -15 30 8.9 -1 -4 15 -3.4 11.1 0 4 -15 15.9 8.8 0 -4 15 -4.3 10.3 -1 4 -15 120.89 25.9 1 -4 15 105.79 24 -6 -3 15 -9.9 11.7 -5 -3 15 9 14.6 -4 -3 15 11.7 14.8 -3 -3 15 34.1 11.8 2 3 -15 -1.4 3.5 2 3 -15 7.2 4.6 -2 -3 15 -4 12.5 1 3 -15 252.17 26.7 -1 -3 15 218.58 44 0 3 -15 11.5 8.6 0 -3 15 -18.5 12.5 -5 -2 15 6.6 21.6 -4 -2 15 -11.4 13.3 -3 -2 15 121.99 35.5 2 2 -15 25.8 5.7 2 2 -15 39.7 7 -2 -2 15 35.5 16.5 1 2 -15 -8.7 6 -1 -2 15 3.3 13.8 0 2 -15 59.29 12.8 0 -2 15 47.7 19.7 -5 -1 15 21.3 17.7 -4 -1 15 7.7 11.7 -3 -1 15 46 22.2 2 1 -15 9 4.1 -2 -1 15 -9.1 12.7 1 1 -15 57.89 12 -1 -1 15 40.6 20.4 0 1 -15 205.68 27.4 0 -1 15 223.88 41.4 -5 0 15 26.6 15.2 -4 0 15 313.37 48 -3 0 15 7 11 2 0 -15 153.78 16.2 -2 0 15 189.28 40.7 1 0 -15 119.69 16.3 -1 0 15 85.09 27.6 -6 1 15 10.6 19.6 -6 1 15 -31.5 37.8 -5 1 15 -23.1 13.6 -4 1 15 46.3 20.1 -4 1 15 34.7 55.89 -3 1 15 32.8 20.9 -3 1 15 17.4 37.2 2 -1 -15 102.79 13.9 -2 1 15 156.48 57.69 -5 2 15 1.8 14.5 -5 2 15 -42.2 45.8 -4 2 15 -32.2 36.9 -4 2 15 -24.8 11.7 -3 2 15 59.49 59.99 3 6 -16 -9.8 5.2 3 6 -16 4.2 5.3 2 6 -16 10.2 9.3 -2 -6 16 18.6 16.8 1 6 -16 14.5 10.1 1 6 -16 -1.1 11.7 -1 -6 16 1.4 14.8 -4 -5 16 38 26.2 -3 -5 16 54.39 23.5 2 5 -16 144.99 16 2 5 -16 114.69 16.2 -2 -5 16 138.39 31.5 1 5 -16 211.38 25.9 1 5 -16 127.39 21.5 -1 -5 16 132.99 33.9 -4 -4 16 26.2 18.3 -3 -4 16 115.79 35.2 2 4 -16 8 4.9 2 4 -16 -3.7 4.4 -2 -4 16 -8.5 16.3 1 4 -16 21.7 7.7 1 4 -16 26.2 12 -1 -4 16 -8.8 15.4 -5 -3 16 52.89 23.5 -3 -3 16 126.19 34.9 2 3 -16 -0.4 3.5 2 3 -16 2.7 4.5 -2 -3 16 15 15.1 1 3 -16 17.2 8.2 1 3 -16 -10.9 14 -1 -3 16 26.5 18.4 -5 -2 16 329.97 48.9 -4 -2 16 68.39 27.3 -3 -2 16 9.6 23.7 2 2 -16 24.5 5.9 2 2 -16 21.7 4.3 -2 -2 16 28.2 19.5 -5 -1 16 233.38 49.1 -4 -1 16 -3.4 15.6 -3 -1 16 2.1 12.5 -4 0 16 30.9 12.5 _iucr_refine_instructions_details ; TITL 22019066_0m_a.res in P-1 22019066_0m.res created by SHELXL-2018/3 at 09:25:38 on 15-Jan-2019 REM Old TITL 22019066_0m in P-1 REM SHELXT solution in P-1 REM R1 0.140, Rweak 0.007, Alpha 0.039, Orientation as input REM Formula found by SHELXT: C23 N O3 S Cl CELL 0.71073 8.2873 11.2154 13.2137 104.22 107.154 107.165 ZERR 2 0.0003 0.0006 0.0006 0.002 0.002 0.002 LATT 1 SFAC C H Cl N O S UNIT 46 48 2 2 6 2 L.S. 4 PLAN 20 SIZE 0.15 0.08 0.03 TEMP -173.15 BOND $H list 4 fmap 2 ACTA REM REM REM WGHT 0.040900 0.414600 FVAR 0.97399 S1 6 0.665688 0.399313 0.357323 11.00000 0.01444 0.02187 = 0.02266 0.00750 0.00683 0.00743 CL1 3 1.606137 0.872320 0.131509 11.00000 0.02621 0.04631 = 0.02868 0.01179 0.01397 0.00808 O3 5 0.693899 0.404042 0.470839 11.00000 0.02269 0.02893 = 0.02287 0.01217 0.00669 0.00942 O1 5 0.679411 0.562649 0.256059 11.00000 0.01701 0.03209 = 0.02431 0.01518 0.00547 0.00395 O2 5 0.760875 0.339491 0.299807 11.00000 0.02171 0.02894 = 0.03260 0.00732 0.01104 0.01470 N1 4 0.707484 0.559765 0.367946 11.00000 0.01630 0.02134 = 0.02137 0.00833 0.00506 0.00645 C22 1 0.311095 0.361321 0.315536 11.00000 0.01866 0.02438 = 0.02123 0.00564 0.00853 0.00794 AFIX 43 H22 2 0.357073 0.421145 0.391862 11.00000 -1.20000 AFIX 0 C17 1 0.430135 0.326847 0.270681 11.00000 0.01444 0.01814 = 0.02162 0.00850 0.00655 0.00628 C4 1 1.276290 0.827757 0.348639 11.00000 0.00933 0.02396 = 0.02185 0.00574 0.00077 0.00207 C20 1 0.055963 0.220640 0.135741 11.00000 0.01733 0.02031 = 0.02542 0.00942 0.00596 0.00385 C5 1 1.314985 0.938557 0.315573 11.00000 0.01899 0.02390 = 0.02670 0.00669 0.00723 0.00819 AFIX 43 H5 2 1.269917 1.004726 0.338596 11.00000 -1.20000 AFIX 0 C3 1 1.348080 0.734335 0.315886 11.00000 0.01551 0.02024 = 0.02606 0.00604 0.00407 0.00260 AFIX 43 H3 2 1.325763 0.659142 0.338733 11.00000 -1.20000 AFIX 0 C7 1 1.158529 0.809256 0.414239 11.00000 0.01358 0.02299 = 0.02526 0.00864 0.00483 0.00552 C21 1 0.125512 0.307824 0.248149 11.00000 0.01807 0.03026 = 0.02706 0.01176 0.01263 0.01030 AFIX 43 H21 2 0.043817 0.330764 0.278836 11.00000 -1.20000 AFIX 0 C12 1 1.002023 0.672897 0.370179 11.00000 0.01521 0.02191 = 0.02270 0.00674 0.00633 0.00569 AFIX 13 H12 2 1.053256 0.602352 0.363775 11.00000 -1.20000 AFIX 0 C10 1 0.880825 0.790016 0.501575 11.00000 0.02017 0.02438 = 0.02273 0.00624 0.00954 0.00687 AFIX 23 H10A 2 0.809980 0.776686 0.549410 11.00000 -1.20000 H10B 2 0.815303 0.817993 0.442143 11.00000 -1.20000 AFIX 0 C11 1 0.894804 0.660490 0.446579 11.00000 0.01572 0.02339 = 0.02120 0.00751 0.00387 0.00520 AFIX 13 H11 2 0.951594 0.627577 0.505939 11.00000 -1.20000 AFIX 0 C13 1 0.853933 0.641356 0.254097 11.00000 0.01569 0.02288 = 0.02433 0.00987 0.00795 0.00311 AFIX 13 H13 2 0.850165 0.727439 0.247287 11.00000 -1.20000 AFIX 0 C6 1 1.417225 0.954459 0.250171 11.00000 0.02277 0.02496 = 0.02765 0.01119 0.00646 0.00587 AFIX 43 H6 2 1.442304 1.030232 0.228182 11.00000 -1.20000 AFIX 0 C18 1 0.364641 0.240614 0.159074 11.00000 0.02079 0.02344 = 0.02450 0.00612 0.01023 0.01001 AFIX 43 H18 2 0.446460 0.217955 0.128354 11.00000 -1.20000 AFIX 0 C2 1 1.450902 0.748315 0.251017 11.00000 0.01654 0.02910 = 0.02235 0.00353 0.00463 0.00817 AFIX 43 H2 2 1.499515 0.683889 0.229702 11.00000 -1.20000 AFIX 0 C19 1 0.177208 0.187962 0.093006 11.00000 0.02382 0.02183 = 0.01992 0.00308 0.00528 0.00650 AFIX 43 H19 2 0.131208 0.128110 0.016688 11.00000 -1.20000 AFIX 0 C9 1 1.072968 0.898445 0.574556 11.00000 0.02488 0.02462 = 0.02532 0.00555 0.00920 0.00748 AFIX 23 H9A 2 1.064336 0.985711 0.602843 11.00000 -1.20000 H9B 2 1.130484 0.877255 0.641146 11.00000 -1.20000 AFIX 0 C23 1 -0.147319 0.166363 0.063912 11.00000 0.01889 0.03596 = 0.03139 0.01034 0.00572 0.00536 AFIX 137 H23A 2 -0.217145 0.131816 0.106127 11.00000 -1.50000 H23B 2 -0.177851 0.093820 -0.006562 11.00000 -1.50000 H23C 2 -0.178978 0.238202 0.045522 11.00000 -1.50000 AFIX 0 C1 1 1.481962 0.857237 0.217635 11.00000 0.01803 0.02997 = 0.01995 0.00629 0.00523 0.00403 C14 1 0.872516 0.564714 0.152461 11.00000 0.02020 0.02890 = 0.03100 0.00528 0.00719 0.00586 AFIX 13 H14 2 0.901657 0.485074 0.156098 11.00000 -1.20000 AFIX 0 C8 1 1.190948 0.908266 0.506844 11.00000 0.01870 0.02318 = 0.02727 0.00806 0.00678 0.00464 AFIX 43 H8 2 1.294338 0.989843 0.531765 11.00000 -1.20000 AFIX 0 C16 1 0.752095 0.553262 0.035882 11.00000 0.02392 0.04566 = 0.02150 0.00183 0.00559 0.00109 AFIX 23 H16A 2 0.707457 0.468087 -0.028535 11.00000 -1.20000 H16B 2 0.665316 0.598283 0.032010 11.00000 -1.20000 AFIX 0 C15 1 0.953875 0.639938 0.087404 11.00000 0.02597 0.05133 = 0.02485 0.00784 0.00990 0.00576 AFIX 23 H15A 2 0.991083 0.738290 0.114928 11.00000 -1.20000 H15B 2 1.033201 0.608168 0.054417 11.00000 -1.20000 AFIX 0 HKLF 4 REM 22019066_0m_a.res in P-1 REM wR2 = 0.1364, GooF = S = 1.032, Restrained GooF = 1.032 for all data REM R1 = 0.0572 for 3022 Fo > 4sig(Fo) and 0.0876 for all 4227 data REM 263 parameters refined using 0 restraints END WGHT 0.0407 0.4354 REM Highest difference peak 0.354, deepest hole -0.401, 1-sigma level 0.077 Q1 1 0.7647 0.3654 0.3395 11.00000 0.05 0.35 Q2 1 0.5820 0.5570 0.3588 11.00000 0.05 0.35 Q3 1 0.5209 0.3640 0.3002 11.00000 0.05 0.34 Q4 1 -0.2641 0.1938 0.0854 11.00000 0.05 0.31 Q5 1 0.5750 0.4206 0.4851 11.00000 0.05 0.30 Q6 1 1.4977 0.8983 0.1261 11.00000 0.05 0.29 Q7 1 0.3113 0.4079 0.2379 11.00000 0.05 0.28 Q8 1 0.9565 0.6142 0.1498 11.00000 0.05 0.28 Q9 1 1.7320 0.8622 0.1574 11.00000 0.05 0.28 Q10 1 0.3474 0.3992 0.3376 11.00000 0.05 0.27 Q11 1 1.5436 0.9420 0.2791 11.00000 0.05 0.27 Q12 1 0.7360 0.2588 0.3217 11.00000 0.05 0.26 Q13 1 -0.0294 0.3971 0.2206 11.00000 0.05 0.25 Q14 1 0.8627 0.3823 0.4708 11.00000 0.05 0.25 Q15 1 1.1120 0.8572 0.4057 11.00000 0.05 0.25 Q16 1 1.0410 0.5458 0.1331 11.00000 0.05 0.25 Q17 1 1.5891 0.9595 0.1253 11.00000 0.05 0.25 Q18 1 0.7919 0.6023 0.4063 11.00000 0.05 0.25 Q19 1 1.6856 0.8080 0.0760 11.00000 0.05 0.24 Q20 1 1.2360 0.8140 0.4016 11.00000 0.05 0.24 REM The information below was added by Olex2. REM REM R1 = 0.0572 for 3022 Fo > 4sig(Fo) and 0.0876 for all 11931 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.35, deepest hole -0.40 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0876 REM R1_gt = 0.0572 REM wR_ref = 0.1364 REM GOOF = 1.032 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 11931 REM Reflections_gt = 3022 REM Parameters = n/a REM Hole = -0.40 REM Peak = 0.35 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received'