data_a _audit_creation_date 2015-07-21 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _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. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C16 H19 N O3 S' _chemical_formula_sum 'C16 H19 N O3 S' _chemical_formula_weight 305.38 _chemical_absolute_configuration ad _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' '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 'monoclinic' _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.804(2) _cell_length_b 22.592(7) _cell_length_c 6.639(2) _cell_angle_alpha 90 _cell_angle_beta 115.905(4) _cell_angle_gamma 90 _cell_volume 783.1(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2694 _cell_measurement_temperature 173.1500 _cell_measurement_theta_max 27.4526 _cell_measurement_theta_min 1.8028 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.216 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.79599 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_absorpt_special_details ? _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 324 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.18 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_unetI/netI 0.0262 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 8462 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.979 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 27.452 _diffrn_reflns_theta_min 3.529 _diffrn_ambient_temperature 173.1500 _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_details ; scan: Number of images: 360 Slice: -110.0000 - 70.0000 Image width: 0.5000 Exp time: 8.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 270.0000 XTD: 45.1413 2theta: -19.8304 scan: Number of images: 330 Slice: -110.0000 - 55.0000 Image width: 0.5000 Exp time: 8.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 45.1413 2theta: -19.8304 scan: Number of images: 328 Slice: -110.0000 - 54.0000 Image width: 0.5000 Exp time: 8.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 180.0000 XTD: 45.1413 2theta: -19.8304 ; _diffrn_measurement_device ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_device_details ; AFC10: Fixed Chi 2 circle ; _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method '\w scans at fixed \c = 45\%' _diffrn_number_total 1849 _diffrn_orient_matrix_type d*Trek _diffrn_orient_matrix_UB_11 0.1907 _diffrn_orient_matrix_UB_12 -0.0052 _diffrn_orient_matrix_UB_13 0.0175 _diffrn_orient_matrix_UB_21 0.0034 _diffrn_orient_matrix_UB_22 0.0354 _diffrn_orient_matrix_UB_23 -0.0264 _diffrn_orient_matrix_UB_31 0.0644 _diffrn_orient_matrix_UB_32 0.0884 _diffrn_orient_matrix_UB_33 0.1268 _diffrn_radiation_detector CCD _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Sealed Tube' _diffrn_source_current 30.0000 _diffrn_source_power 1.5000 _diffrn_source_voltage 50.0000 _diffrn_special_details ; ? ; _reflns_Friedel_coverage 0.921 _reflns_Friedel_fraction_full 0.975 _reflns_Friedel_fraction_max 0.963 _reflns_number_gt 3485 _reflns_number_total 3532 _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 'CrystalClear (Rigaku Inc., 2007)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'CIFTAB (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL (Sheldrick, 2014)' _computing_structure_solution ; 'SHELXT (Sheldrick, 2014)' ; _refine_diff_density_max 0.221 _refine_diff_density_min -0.201 _refine_diff_density_rms 0.032 _refine_ls_abs_structure_details ; Flack x determined using 1576 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 196 _refine_ls_number_reflns 3532 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0296 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+0.1456P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.0757 _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, All O(H) groups 2.a Ternary CH refined with riding coordinates: C1(H1B) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B) 2.c Aromatic/amide H refined with riding coordinates: C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15) 2.d Idealised Me refined as rotating group: C16(H16A,H16B,H16C) 2.e Idealised tetrahedral OH refined as rotating group: O1(H1) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _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 0.33281(9) 0.54364(2) 0.45693(8) 0.02580(13) Uani 1 1 d . . . . . O1 O 1.2513(3) 0.46412(9) 0.9157(3) 0.0344(4) Uani 1 1 d . . . . . H1 H 1.2941 0.4917 1.0048 0.052 Uiso 1 1 calc GR . . . . O2 O 0.0724(3) 0.55234(8) 0.4186(3) 0.0361(4) Uani 1 1 d . . . . . O3 O 0.3988(3) 0.54707(9) 0.2723(2) 0.0339(3) Uani 1 1 d . . . . . N1 N 0.4133(4) 0.47862(8) 0.5675(3) 0.0249(4) Uani 1 1 d . . . . . C1 C 0.6735(4) 0.45538(10) 0.6279(3) 0.0231(4) Uani 1 1 d . . . . . H1B H 0.7654 0.4834 0.5765 0.028 Uiso 1 1 calc R . . . . C2 C 0.8190(4) 0.44926(11) 0.8834(4) 0.0286(5) Uani 1 1 d . . . . . H2A H 0.8284 0.4878 0.9509 0.034 Uiso 1 1 calc R . . . . H2B H 0.7229 0.4233 0.9352 0.034 Uiso 1 1 calc R . . . . C3 C 1.0886(4) 0.42494(11) 0.9633(4) 0.0306(5) Uani 1 1 d . . . . . H3A H 1.1613 0.4181 1.1235 0.037 Uiso 1 1 calc R . . . . H3B H 1.0810 0.3872 0.8911 0.037 Uiso 1 1 calc R . . . . C4 C 0.6518(4) 0.39650(9) 0.5104(4) 0.0239(4) Uani 1 1 d . . . . . C5 C 0.4976(5) 0.35137(10) 0.5276(5) 0.0352(5) Uani 1 1 d . . . . . H5 H 0.4073 0.3572 0.6121 0.042 Uiso 1 1 calc R . . . . C6 C 0.4781(6) 0.29776(11) 0.4193(5) 0.0474(8) Uani 1 1 d . . . . . H6 H 0.3730 0.2681 0.4303 0.057 Uiso 1 1 calc R . . . . C7 C 0.6132(6) 0.28821(12) 0.2959(5) 0.0486(7) Uani 1 1 d . . . . . H7 H 0.5992 0.2522 0.2235 0.058 Uiso 1 1 calc R . . . . C8 C 0.7705(6) 0.33240(13) 0.2795(5) 0.0448(6) Uani 1 1 d . . . . . H8 H 0.8635 0.3259 0.1977 0.054 Uiso 1 1 calc R . . . . C9 C 0.7884(5) 0.38661(11) 0.3863(4) 0.0327(5) Uani 1 1 d . . . . . H9 H 0.8926 0.4163 0.3742 0.039 Uiso 1 1 calc R . . . . C10 C 0.5278(4) 0.59521(9) 0.6592(4) 0.0270(4) Uani 1 1 d . . . . . C11 C 0.4742(5) 0.60601(11) 0.8416(4) 0.0331(5) Uani 1 1 d . . . . . H11 H 0.3346 0.5881 0.8504 0.040 Uiso 1 1 calc R . . . . C12 C 0.6324(6) 0.64384(11) 1.0093(4) 0.0405(6) Uani 1 1 d . . . . . H12 H 0.5979 0.6512 1.1312 0.049 Uiso 1 1 calc R . . . . C13 C 0.8411(5) 0.67092(11) 0.9986(5) 0.0431(7) Uani 1 1 d . . . . . C14 C 0.8904(5) 0.65941(12) 0.8149(5) 0.0417(6) Uani 1 1 d . . . . . H14 H 1.0297 0.6774 0.8060 0.050 Uiso 1 1 calc R . . . . C15 C 0.7354(5) 0.62151(11) 0.6449(5) 0.0337(5) Uani 1 1 d . . . . . H15 H 0.7706 0.6139 0.5234 0.040 Uiso 1 1 calc R . . . . C16 C 1.0132(8) 0.71188(16) 1.1852(6) 0.0706(11) Uani 1 1 d . . . . . H16A H 0.9097 0.7382 1.2250 0.106 Uiso 1 1 calc GR . . . . H16B H 1.1181 0.7346 1.1351 0.106 Uiso 1 1 calc GR . . . . H16C H 1.1206 0.6888 1.3135 0.106 Uiso 1 1 calc GR . . . . H1A H 0.364(6) 0.4753(13) 0.674(5) 0.037(8) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0244(2) 0.0286(2) 0.0220(2) 0.0003(2) 0.00792(17) 0.0025(2) O1 0.0271(8) 0.0505(11) 0.0279(8) -0.0063(7) 0.0142(7) -0.0089(7) O2 0.0252(7) 0.0420(11) 0.0358(8) 0.0006(7) 0.0083(6) 0.0055(7) O3 0.0396(8) 0.0384(8) 0.0242(7) 0.0011(8) 0.0144(6) 0.0000(9) N1 0.0223(9) 0.0280(9) 0.0259(9) -0.0001(7) 0.0120(7) -0.0004(7) C1 0.0195(9) 0.0271(10) 0.0214(10) 0.0003(8) 0.0078(8) -0.0005(8) C2 0.0229(10) 0.0410(13) 0.0211(10) -0.0013(9) 0.0089(8) -0.0036(9) C3 0.0249(10) 0.0390(13) 0.0234(10) 0.0030(9) 0.0064(9) -0.0027(9) C4 0.0208(9) 0.0233(10) 0.0227(9) 0.0021(8) 0.0049(8) 0.0020(7) C5 0.0292(11) 0.0288(11) 0.0438(14) 0.0027(10) 0.0125(10) -0.0008(9) C6 0.0364(14) 0.0254(12) 0.0655(19) 0.0004(12) 0.0084(14) -0.0043(10) C7 0.0434(15) 0.0297(12) 0.0566(17) -0.0145(12) 0.0069(13) 0.0064(11) C8 0.0460(15) 0.0424(14) 0.0419(15) -0.0116(11) 0.0154(12) 0.0079(12) C9 0.0333(12) 0.0343(12) 0.0290(11) -0.0032(9) 0.0122(9) 0.0005(9) C10 0.0286(11) 0.0225(10) 0.0274(11) 0.0004(8) 0.0098(9) 0.0030(8) C11 0.0402(13) 0.0291(11) 0.0307(11) 0.0018(9) 0.0161(10) 0.0011(9) C12 0.0575(17) 0.0317(12) 0.0278(11) -0.0016(10) 0.0146(11) 0.0049(11) C13 0.0433(15) 0.0284(12) 0.0403(14) -0.0038(11) 0.0023(11) 0.0023(11) C14 0.0317(13) 0.0330(12) 0.0544(16) -0.0014(12) 0.0133(12) -0.0018(10) C15 0.0326(12) 0.0305(12) 0.0399(13) 0.0011(10) 0.0175(11) 0.0013(10) C16 0.072(2) 0.053(2) 0.061(2) -0.0209(16) 0.0048(18) -0.0116(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O2 1.4322(18) . ? S1 O3 1.4373(16) . ? S1 N1 1.6172(19) . ? S1 C10 1.765(2) . ? O1 H1 0.8200 . ? O1 C3 1.426(3) . ? N1 C1 1.480(3) . ? N1 H1A 0.87(3) . ? C1 H1B 0.9800 . ? C1 C2 1.536(3) . ? C1 C4 1.519(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C3 1.519(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.394(3) . ? C4 C9 1.388(3) . ? C5 H5 0.9300 . ? C5 C6 1.387(4) . ? C6 H6 0.9300 . ? C6 C7 1.377(5) . ? C7 H7 0.9300 . ? C7 C8 1.389(5) . ? C8 H8 0.9300 . ? C8 C9 1.396(4) . ? C9 H9 0.9300 . ? C10 C11 1.397(3) . ? C10 C15 1.384(3) . ? C11 H11 0.9300 . ? C11 C12 1.385(4) . ? C12 H12 0.9300 . ? C12 C13 1.386(4) . ? C13 C14 1.394(4) . ? C13 C16 1.519(4) . ? C14 H14 0.9300 . ? C14 C15 1.389(4) . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 S1 O3 119.64(10) . . ? O2 S1 N1 106.16(11) . . ? O2 S1 C10 108.71(11) . . ? O3 S1 N1 107.72(11) . . ? O3 S1 C10 107.00(11) . . ? N1 S1 C10 106.99(11) . . ? C3 O1 H1 109.5 . . ? S1 N1 H1A 108(2) . . ? C1 N1 S1 120.22(15) . . ? C1 N1 H1A 114(2) . . ? N1 C1 H1B 108.8 . . ? N1 C1 C2 109.56(18) . . ? N1 C1 C4 109.01(17) . . ? C2 C1 H1B 108.8 . . ? C4 C1 H1B 108.8 . . ? C4 C1 C2 111.75(18) . . ? C1 C2 H2A 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C3 C2 C1 113.79(19) . . ? C3 C2 H2A 108.8 . . ? C3 C2 H2B 108.8 . . ? O1 C3 C2 112.3(2) . . ? O1 C3 H3A 109.1 . . ? O1 C3 H3B 109.2 . . ? C2 C3 H3A 109.2 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C1 120.7(2) . . ? C9 C4 C1 120.3(2) . . ? C9 C4 C5 119.0(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 C4 120.4(3) . . ? C6 C5 H5 119.8 . . ? C5 C6 H6 119.8 . . ? C7 C6 C5 120.4(3) . . ? C7 C6 H6 119.8 . . ? C6 C7 H7 120.0 . . ? C6 C7 C8 119.9(2) . . ? C8 C7 H7 120.0 . . ? C7 C8 H8 120.1 . . ? C7 C8 C9 119.8(3) . . ? C9 C8 H8 120.1 . . ? C4 C9 C8 120.5(2) . . ? C4 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 S1 117.61(18) . . ? C15 C10 S1 121.29(19) . . ? C15 C10 C11 121.0(2) . . ? C10 C11 H11 120.5 . . ? C12 C11 C10 118.9(2) . . ? C12 C11 H11 120.5 . . ? C11 C12 H12 119.4 . . ? C11 C12 C13 121.2(3) . . ? C13 C12 H12 119.4 . . ? C12 C13 C14 118.7(2) . . ? C12 C13 C16 120.4(3) . . ? C14 C13 C16 120.9(3) . . ? C13 C14 H14 119.4 . . ? C15 C14 C13 121.2(3) . . ? C15 C14 H14 119.4 . . ? C10 C15 C14 118.9(3) . . ? C10 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? 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 O1 H1 O3 0.82 2.04 2.842(3) 167.9 1_656 N1 H1A O1 0.87(3) 2.00(3) 2.870(3) 178(3) 1_455 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 S1 N1 C1 C2 113.53(19) . . . . ? S1 N1 C1 C4 -123.90(17) . . . . ? S1 C10 C11 C12 176.55(19) . . . . ? S1 C10 C15 C14 -176.64(19) . . . . ? O2 S1 N1 C1 179.74(16) . . . . ? O2 S1 C10 C11 40.8(2) . . . . ? O2 S1 C10 C15 -142.9(2) . . . . ? O3 S1 N1 C1 50.45(18) . . . . ? O3 S1 C10 C11 171.27(17) . . . . ? O3 S1 C10 C15 -12.4(2) . . . . ? N1 S1 C10 C11 -73.50(19) . . . . ? N1 S1 C10 C15 102.9(2) . . . . ? N1 C1 C2 C3 179.31(19) . . . . ? N1 C1 C4 C5 -52.0(3) . . . . ? N1 C1 C4 C9 128.8(2) . . . . ? C1 C2 C3 O1 65.2(3) . . . . ? C1 C4 C5 C6 179.8(2) . . . . ? C1 C4 C9 C8 179.5(2) . . . . ? C2 C1 C4 C5 69.3(3) . . . . ? C2 C1 C4 C9 -109.9(2) . . . . ? C4 C1 C2 C3 58.4(3) . . . . ? C4 C5 C6 C7 0.8(4) . . . . ? C5 C4 C9 C8 0.3(3) . . . . ? C5 C6 C7 C8 0.1(4) . . . . ? C6 C7 C8 C9 -0.8(4) . . . . ? C7 C8 C9 C4 0.6(4) . . . . ? C9 C4 C5 C6 -1.0(4) . . . . ? C10 S1 N1 C1 -64.29(19) . . . . ? C10 C11 C12 C13 0.1(4) . . . . ? C11 C10 C15 C14 -0.4(4) . . . . ? C11 C12 C13 C14 -0.1(4) . . . . ? C11 C12 C13 C16 -179.5(3) . . . . ? C12 C13 C14 C15 -0.2(4) . . . . ? C13 C14 C15 C10 0.4(4) . . . . ? C15 C10 C11 C12 0.2(4) . . . . ? C16 C13 C14 C15 179.3(3) . . . . ? _shelx_res_file ; a.res created by SHELXL-2014/7 TITL a_a.res in P2(1) CELL 0.71073 5.8043 22.5917 6.6389 90 115.905 90 ZERR 2 0.002 0.007 0.0023 0 0.004 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S UNIT 32 38 2 6 2 EQIV $1 1+X,+Y,1+Z EQIV $2 -1+X,+Y,+Z L.S. 4 0 0 PLAN 20 HTAB O1 O3_$1 HTAB N1 O1_$2 BOND $H LIST 6 fmap 2 53 MORE -1 ACTA 52 CONF HTAB OMIT 0 -2 0 OMIT 0 2 0 REM REM REM WGHT 0.039000 0.145600 FVAR 1.27032 S1 5 0.332808 0.543640 0.456928 11.00000 0.02442 0.02861 = 0.02199 0.00034 0.00792 0.00253 O1 4 1.251275 0.464118 0.915704 11.00000 0.02709 0.05051 = 0.02789 -0.00630 0.01418 -0.00893 AFIX 147 H1 2 1.294079 0.491723 1.004841 11.00000 -1.50000 AFIX 0 O2 4 0.072422 0.552336 0.418565 11.00000 0.02518 0.04198 = 0.03585 0.00058 0.00834 0.00546 O3 4 0.398785 0.547071 0.272272 11.00000 0.03956 0.03844 = 0.02417 0.00106 0.01442 0.00004 N1 3 0.413259 0.478616 0.567500 11.00000 0.02227 0.02804 = 0.02594 -0.00014 0.01202 -0.00037 C1 1 0.673544 0.455381 0.627872 11.00000 0.01950 0.02714 = 0.02137 0.00028 0.00782 -0.00048 AFIX 13 H1B 2 0.765367 0.483409 0.576464 11.00000 -1.20000 AFIX 0 C2 1 0.819035 0.449257 0.883444 11.00000 0.02294 0.04104 = 0.02112 -0.00130 0.00888 -0.00356 AFIX 23 H2A 2 0.828411 0.487806 0.950945 11.00000 -1.20000 H2B 2 0.722902 0.423310 0.935247 11.00000 -1.20000 AFIX 0 C3 1 1.088614 0.424940 0.963258 11.00000 0.02489 0.03899 = 0.02343 0.00303 0.00636 -0.00267 AFIX 23 H3A 2 1.161297 0.418146 1.123481 11.00000 -1.20000 H3B 2 1.080980 0.387180 0.891052 11.00000 -1.20000 AFIX 0 C4 1 0.651850 0.396502 0.510409 11.00000 0.02076 0.02327 = 0.02270 0.00214 0.00494 0.00202 C5 1 0.497610 0.351371 0.527601 11.00000 0.02924 0.02878 = 0.04379 0.00270 0.01251 -0.00084 AFIX 43 H5 2 0.407251 0.357233 0.612149 11.00000 -1.20000 AFIX 0 C6 1 0.478078 0.297762 0.419346 11.00000 0.03638 0.02539 = 0.06551 0.00038 0.00841 -0.00432 AFIX 43 H6 2 0.373034 0.268091 0.430256 11.00000 -1.20000 AFIX 0 C7 1 0.613209 0.288210 0.295880 11.00000 0.04337 0.02969 = 0.05663 -0.01447 0.00688 0.00635 AFIX 43 H7 2 0.599198 0.252203 0.223534 11.00000 -1.20000 AFIX 0 C8 1 0.770460 0.332403 0.279494 11.00000 0.04598 0.04243 = 0.04190 -0.01159 0.01539 0.00786 AFIX 43 H8 2 0.863515 0.325908 0.197652 11.00000 -1.20000 AFIX 0 C9 1 0.788384 0.386613 0.386290 11.00000 0.03325 0.03429 = 0.02904 -0.00323 0.01221 0.00048 AFIX 43 H9 2 0.892555 0.416321 0.374202 11.00000 -1.20000 AFIX 0 C10 1 0.527772 0.595209 0.659231 11.00000 0.02860 0.02247 = 0.02743 0.00042 0.00983 0.00297 C11 1 0.474197 0.606012 0.841624 11.00000 0.04017 0.02911 = 0.03069 0.00179 0.01608 0.00106 AFIX 43 H11 2 0.334584 0.588099 0.850364 11.00000 -1.20000 AFIX 0 C12 1 0.632400 0.643840 1.009280 11.00000 0.05748 0.03173 = 0.02784 -0.00158 0.01457 0.00493 AFIX 43 H12 2 0.597933 0.651201 1.131249 11.00000 -1.20000 AFIX 0 C13 1 0.841090 0.670922 0.998639 11.00000 0.04329 0.02838 = 0.04034 -0.00382 0.00233 0.00225 C14 1 0.890384 0.659408 0.814912 11.00000 0.03173 0.03301 = 0.05441 -0.00136 0.01335 -0.00182 AFIX 43 H14 2 1.029669 0.677438 0.805983 11.00000 -1.20000 AFIX 0 C15 1 0.735391 0.621509 0.644884 11.00000 0.03262 0.03046 = 0.03991 0.00115 0.01751 0.00128 AFIX 43 H15 2 0.770569 0.613937 0.523435 11.00000 -1.20000 AFIX 0 C16 1 1.013203 0.711880 1.185213 11.00000 0.07173 0.05304 = 0.06087 -0.02091 0.00478 -0.01162 AFIX 137 H16A 2 0.909706 0.738153 1.225002 11.00000 -1.50000 H16B 2 1.118126 0.734569 1.135068 11.00000 -1.50000 H16C 2 1.120555 0.688804 1.313487 11.00000 -1.50000 AFIX 0 H1A 2 0.364387 0.475277 0.673944 11.00000 0.03687 HKLF 4 REM a_a.res in P2(1) REM R1 = 0.0296 for 3485 Fo > 4sig(Fo) and 0.0301 for all 3532 data REM 196 parameters refined using 1 restraints END WGHT 0.0390 0.1456 REM Instructions for potential hydrogen bonds HTAB O1 O3_$1 EQIV $3 x+1, y, z HTAB C15 O2_$3 HTAB N1 O1_$2 REM Highest difference peak 0.221, deepest hole -0.201, 1-sigma level 0.032 Q1 1 0.4250 0.5760 0.5544 11.00000 0.05 0.22 Q2 1 0.3921 0.5153 0.5471 11.00000 0.05 0.21 Q3 1 0.7619 0.4576 0.7565 11.00000 0.05 0.16 Q4 1 0.5726 0.6185 0.6203 11.00000 0.05 0.14 Q5 1 0.5429 0.3783 0.4734 11.00000 0.05 0.14 Q6 1 0.9478 0.4411 0.9137 11.00000 0.05 0.14 Q7 1 0.8131 0.6364 0.7560 11.00000 0.05 0.14 Q8 1 1.2061 0.6990 1.2191 11.00000 0.05 0.13 Q9 1 0.5157 0.6371 0.9026 11.00000 0.05 0.13 Q10 1 0.1275 0.5436 0.5301 11.00000 0.05 0.12 Q11 1 0.6432 0.4218 0.5561 11.00000 0.05 0.12 Q12 1 0.6012 0.6218 0.9430 11.00000 0.05 0.12 Q13 1 -0.0183 0.5435 0.5980 11.00000 0.05 0.12 Q14 1 0.5210 0.5997 0.7377 11.00000 0.05 0.11 Q15 1 0.9676 0.7464 1.1207 11.00000 0.05 0.11 Q16 1 0.6808 0.4016 0.4199 11.00000 0.05 0.11 Q17 1 0.5806 0.2944 0.3834 11.00000 0.05 0.11 Q18 1 0.5198 0.3227 0.4830 11.00000 0.05 0.11 Q19 1 0.9620 0.7147 1.3470 11.00000 0.05 0.11 Q20 1 0.1672 0.5470 0.3954 11.00000 0.05 0.10 ; _shelx_res_checksum 96578 _shelx_hkl_file ; 0 0 -2 2327.32 20.49 0 0 2 2293.20 20.18 0 0 -2 2346.11 20.78 0 0 2 2301.35 20.07 0 0 -2 2308.45 20.12 0 0 -3 16.26 1.32 0 0 3 16.66 0.91 0 0 -3 16.93 1.96 0 0 3 14.55 0.82 0 0 -3 13.69 0.76 0 0 -4 16.82 1.33 0 0 -4 18.78 1.80 0 0 4 14.18 0.86 0 0 -4 11.76 0.78 0 0 -5 2.96 1.69 0 0 -5 2.83 0.71 0 0 5 4.52 0.88 0 0 -6 0.63 1.16 0 0 -6 1.76 0.84 0 0 6 1.79 0.89 0 0 -7 42.74 2.53 0 0 -7 47.25 4.56 0 -1 0 -0.11 0.05 0 -1 0 -0.29 0.07 0 1 0 -0.25 0.07 0 1 1 1150.91 10.19 0 -1 1 1183.27 10.34 0 -1 -1 1161.51 10.29 0 1 -1 1140.17 10.13 0 1 1 1149.73 9.98 0 -1 1 1156.32 10.16 0 -1 -2 2156.08 19.11 0 1 -2 2147.48 18.91 0 -1 2 2116.92 18.62 0 -1 -2 2126.53 18.91 0 1 -2 2129.77 18.98 0 1 2 2114.10 18.43 0 -1 2 2135.62 18.75 0 -1 -2 2116.20 18.43 0 1 -2 2126.03 18.64 0 -1 -3 719.94 12.13 0 1 -3 727.99 12.18 0 1 3 676.19 11.38 0 -1 3 696.32 11.64 0 -1 -3 709.07 12.00 0 1 -3 720.35 12.23 0 1 3 715.75 11.79 0 -1 3 682.35 11.33 0 -1 -3 681.73 11.22 0 1 -3 707.37 11.70 0 1 -4 432.24 7.81 0 -1 -4 427.64 7.85 0 -1 -4 410.12 7.56 0 1 -4 435.62 8.16 0 1 4 433.15 7.54 0 -1 4 419.78 7.40 0 -1 -4 416.71 7.24 0 -1 -5 604.91 14.81 0 1 -5 634.00 15.33 0 -1 -5 587.06 14.52 0 1 -5 596.66 14.67 0 1 5 596.45 14.19 0 -1 5 614.18 14.69 0 -1 -6 189.72 7.04 0 1 -6 206.96 7.65 0 -1 -6 185.05 8.54 0 1 -6 190.89 7.27 0 1 6 193.39 6.86 0 -1 6 193.75 6.94 0 1 -7 19.13 1.58 0 -1 -7 20.03 1.56 0 -1 -7 22.90 3.00 0 1 -7 27.41 3.65 0 -2 0 0.19 0.12 0 2 0 0.21 0.16 0 -2 0 -0.22 0.19 0 2 0 -0.19 0.18 0 2 1 2033.23 17.74 0 2 -2 2501.18 21.84 0 -2 2 2502.49 21.82 0 -2 -2 2547.02 22.51 0 2 -2 2506.24 22.22 0 2 2 2531.34 21.94 0 -2 -2 2526.99 21.88 0 -2 2 2555.27 22.39 0 2 -2 2455.64 21.50 0 -2 -3 62.62 2.01 0 2 -3 56.90 1.69 0 -2 -3 63.22 1.93 0 2 -3 47.33 1.63 0 2 3 56.83 1.35 0 -2 3 60.38 1.71 0 -2 -3 57.34 1.41 0 2 -3 55.15 1.56 0 -2 -4 75.04 2.41 0 2 -4 84.51 2.50 0 -2 -4 89.03 6.59 0 2 -4 78.69 2.36 0 2 4 75.88 1.83 0 -2 4 74.01 1.99 0 -2 -4 76.66 1.83 0 -2 -5 189.81 5.49 0 2 -5 186.00 5.18 0 -2 -5 190.18 5.45 0 2 -5 188.93 5.70 0 2 5 183.56 4.75 0 -2 5 182.39 4.88 0 -2 -6 202.84 7.54 0 2 -6 203.21 7.75 0 -2 -6 226.00 8.74 0 2 -6 231.73 12.44 0 2 6 190.87 7.55 0 -2 6 209.75 7.54 0 -2 -7 44.21 2.81 0 2 -7 41.11 2.58 0 -2 -7 50.97 4.46 0 2 -7 47.76 5.69 0 3 0 4.27 0.31 0 3 1 761.08 7.07 0 3 -1 752.97 6.66 0 -3 -1 745.35 6.87 0 3 1 768.83 7.04 0 -3 1 732.86 6.84 0 -3 -1 733.66 6.55 0 -3 1 728.38 6.76 0 3 2 350.53 3.93 0 3 -2 351.79 3.61 0 -3 2 345.47 3.57 0 -3 -2 362.53 3.97 0 3 2 352.66 4.27 0 3 -2 353.32 4.12 0 3 2 357.60 3.49 0 -3 -2 346.12 3.38 0 3 -2 343.57 3.71 0 -3 -3 1038.09 17.27 0 3 -3 1020.82 16.73 0 -3 3 976.28 15.99 0 3 -3 1032.72 17.21 0 3 3 1025.19 16.69 0 -3 -3 990.41 16.08 0 3 -3 953.83 15.68 0 -3 -4 352.71 6.76 0 3 -4 356.85 6.57 0 -3 -4 347.14 6.55 0 3 -4 356.34 6.91 0 3 4 343.05 6.03 0 -3 4 361.82 6.60 0 -3 -4 346.52 6.05 0 -3 -5 1073.14 25.55 0 3 -5 1097.31 25.88 0 -3 -5 1055.82 25.25 0 3 -5 1081.92 25.99 0 3 5 1044.41 24.44 0 -3 5 1051.68 24.77 0 -3 -6 277.76 10.08 0 3 -6 283.59 10.16 0 -3 -6 288.53 10.61 0 3 -6 272.64 9.98 0 -3 6 270.68 9.57 0 -3 -7 113.38 4.17 0 3 -7 96.30 3.48 0 -3 -7 104.30 10.27 0 3 -7 99.48 8.72 0 -4 0 442.55 4.15 0 4 0 456.79 4.25 0 -4 0 441.20 4.20 0 4 0 469.30 4.44 0 -4 -2 344.67 4.01 0 4 2 325.66 3.81 0 4 -2 335.00 3.44 0 -4 2 335.21 3.39 0 -4 -2 347.62 3.90 0 4 2 328.14 3.70 0 4 2 333.46 3.50 0 -4 -2 339.33 3.35 0 4 -2 325.08 3.69 0 -4 -3 190.64 4.07 0 4 -3 174.81 3.41 0 -4 3 176.40 3.37 0 -4 -3 193.73 4.02 0 4 -3 179.90 3.88 0 4 3 166.35 3.71 0 -4 -3 175.85 3.18 0 -4 3 170.30 3.48 0 4 -3 160.90 3.24 0 -4 -4 194.28 4.39 0 4 -4 197.47 3.97 0 -4 -4 207.03 4.42 0 4 -4 202.05 4.38 0 4 4 193.39 3.86 0 -4 4 189.53 3.89 0 -4 -4 189.58 3.55 0 -4 -5 118.72 3.96 0 4 -5 106.73 3.26 0 -4 -5 136.19 7.92 0 4 -5 110.31 3.68 0 4 5 111.55 3.27 0 -4 5 115.22 3.42 0 -4 -6 266.65 9.68 0 4 -6 271.65 9.63 0 -4 -6 296.13 10.74 0 4 -6 273.99 10.21 0 -4 6 269.87 9.62 0 -4 -7 105.78 4.06 0 -4 -7 101.31 7.19 0 4 -7 93.23 9.78 0 -5 0 2.55 0.42 0 5 0 2.81 0.54 0 -5 0 5.36 1.25 0 5 0 2.34 0.89 0 5 2 202.15 2.56 0 -5 -3 1196.91 19.86 0 5 -3 1164.23 18.95 0 -5 3 1155.47 18.77 0 -5 -3 1133.35 18.77 0 5 -3 1206.05 20.05 0 5 3 1134.04 18.37 0 -5 -3 1137.56 18.40 0 -5 3 1161.42 19.16 0 -5 -4 159.66 3.74 0 5 -4 156.95 3.37 0 -5 4 143.52 3.02 0 -5 -4 177.57 4.20 0 5 -4 174.08 3.99 0 5 4 160.17 3.49 0 -5 -4 155.26 2.98 0 -5 4 161.71 3.59 0 -5 -5 283.04 7.56 0 5 -5 306.15 7.73 0 -5 -5 298.55 7.92 0 5 -5 302.24 8.18 0 5 5 273.22 6.78 0 -5 5 292.73 7.49 0 -5 -6 114.26 4.22 0 5 -6 121.28 4.09 0 -5 -6 125.15 10.49 0 5 -6 137.61 8.99 0 -5 6 121.33 4.18 0 -5 -7 70.80 4.69 0 -5 -7 75.89 8.15 0 5 -7 75.31 6.07 0 -6 0 120.66 1.71 0 6 0 115.32 1.55 0 6 0 120.68 2.02 0 -6 0 112.96 1.86 0 6 0 115.17 1.76 0 -6 1 3360.61 28.96 0 -6 -1 3370.27 29.49 0 -6 1 3256.67 28.49 0 -6 1 3389.48 29.74 0 -6 -1 3471.18 30.04 0 6 -2 123.43 1.55 0 -6 -2 128.43 2.24 0 6 -2 121.67 1.72 0 6 2 121.38 4.37 0 -6 -2 126.78 1.62 0 -6 2 122.35 2.28 0 6 -2 119.88 2.05 0 -6 -3 872.61 16.76 0 6 -3 869.16 16.30 0 -6 3 856.96 16.02 0 -6 -3 843.29 16.14 0 6 -3 836.94 16.15 0 6 3 863.76 16.09 0 -6 -3 829.50 15.47 0 -6 3 868.12 16.55 0 -6 -4 868.59 16.69 0 6 -4 850.05 15.92 0 -6 -4 866.81 16.51 0 6 -4 879.21 16.97 0 6 4 816.91 15.20 0 -6 -4 810.49 14.99 0 -6 4 853.33 16.22 0 -6 -5 24.14 1.95 0 6 -5 27.44 1.43 0 -6 -5 30.02 3.85 0 6 -5 30.41 1.85 0 -6 5 28.00 1.58 0 -6 -6 11.36 1.41 0 6 -6 10.16 1.01 0 -6 -6 15.01 2.32 0 6 -6 10.37 1.45 0 -6 6 14.91 1.38 0 -6 -7 34.26 6.06 0 6 -7 37.93 6.43 0 -7 0 0.82 1.06 0 -7 0 3.29 2.00 0 7 0 1.39 1.14 0 -7 -1 4646.38 40.36 0 -7 1 4468.51 38.84 0 7 1 4657.69 40.36 0 -7 1 4738.39 41.25 0 7 -2 1848.43 16.24 0 7 -2 1865.64 16.36 0 7 2 1807.05 16.42 0 7 -2 1842.19 16.93 0 -7 -2 1813.59 16.06 0 -7 2 1824.25 16.74 0 7 -3 1895.21 34.94 0 -7 -3 1923.61 31.82 0 7 -3 1912.00 31.16 0 -7 -3 1919.83 31.61 0 7 -3 1905.21 35.66 0 -7 -3 1845.95 34.04 0 -7 3 1965.01 32.43 0 -7 -4 600.60 12.00 0 7 -4 608.01 11.61 0 -7 4 551.90 10.42 0 -7 -4 602.31 12.80 0 7 -4 621.73 12.36 0 7 4 592.69 11.10 0 -7 -4 563.70 10.56 0 -7 4 572.84 11.23 0 -7 -5 109.89 4.04 0 7 -5 101.21 3.33 0 -7 -5 105.01 3.88 0 7 -5 106.13 3.92 0 -7 5 108.68 3.68 0 -7 -6 172.47 5.78 0 7 -6 157.91 4.88 0 -7 -6 161.32 8.30 0 7 -6 180.67 6.20 0 -7 6 164.11 5.32 0 -7 -7 12.74 1.99 0 -7 -7 7.54 1.78 0 7 -7 13.97 2.60 0 -7 7 10.46 1.57 0 8 0 1912.44 17.12 0 8 -1 215.32 2.39 0 8 1 204.26 3.16 0 8 -1 234.20 3.41 0 -8 1 221.01 3.01 0 8 1 231.20 3.07 0 -8 -1 242.37 3.03 0 8 -2 556.84 9.19 0 8 -2 556.98 9.18 0 8 2 523.23 8.85 0 -8 -2 547.87 9.09 0 -8 2 564.15 9.80 0 -8 -2 579.91 9.66 0 8 -3 2.67 0.31 0 8 -3 5.07 1.05 0 -8 -3 10.67 1.09 0 8 -3 8.53 1.99 0 -8 3 2.56 1.25 0 8 -4 653.38 12.21 0 -8 -4 706.95 13.86 0 8 -4 694.68 13.07 0 -8 -4 732.49 14.20 0 8 -4 696.10 13.64 0 -8 -4 644.59 12.02 0 -8 4 721.18 13.98 0 -8 -5 30.47 1.92 0 8 -5 31.34 1.50 0 -8 -5 29.98 3.14 0 8 -5 30.17 1.89 0 -8 5 30.23 1.74 0 -8 -6 67.08 3.73 0 -8 -6 61.12 5.27 0 8 -6 70.34 3.77 0 -8 6 56.67 2.88 0 -8 -7 59.57 4.39 0 -8 -7 49.22 7.12 0 8 -7 60.19 8.30 0 -8 7 53.70 3.83 0 9 0 7.06 2.01 0 -9 0 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18.59 3.62 6 4 1 12.46 3.46 6 -4 1 18.36 3.65 -6 -4 0 23.78 2.56 -6 4 0 24.66 2.66 6 4 0 23.74 3.18 6 -4 0 24.68 4.42 -6 -4 1 22.92 2.48 -6 4 1 28.29 2.73 6 4 -1 29.43 6.50 6 -4 -1 20.97 3.71 -6 -4 2 150.77 6.82 -6 4 2 161.23 7.24 -6 4 2 161.42 5.17 6 4 -2 140.46 11.29 6 -4 -2 160.37 7.12 -6 -4 3 84.39 3.83 -6 4 3 85.95 4.00 -6 4 3 78.11 3.14 6 4 -3 77.62 3.24 6 -4 -3 79.12 3.21 -6 -4 4 2.88 1.16 -6 4 4 4.43 1.47 -6 4 4 2.27 1.87 6 -4 -4 1.82 0.79 -6 -4 5 6.72 1.78 -6 4 5 5.67 2.40 -6 4 5 2.91 1.26 6 -4 -5 2.48 0.79 6 -4 -6 28.61 2.05 -6 4 6 29.30 2.54 -6 -4 6 22.49 1.73 6 -4 -7 9.85 1.67 -6 -5 -1 12.61 2.75 -6 5 -1 7.06 2.45 6 5 1 9.52 1.90 6 -5 1 11.08 2.44 -6 -5 0 3.51 3.31 -6 5 0 9.78 2.69 6 5 0 4.72 1.22 6 -5 0 4.50 1.60 -6 -5 1 25.32 3.19 -6 5 1 15.58 2.48 6 5 -1 16.92 2.20 6 -5 -1 17.09 2.66 -6 -5 2 39.34 2.78 -6 5 2 34.39 3.39 -6 5 2 35.65 2.32 6 5 -2 33.16 5.45 6 -5 -2 41.17 6.19 -6 -5 3 132.37 5.04 -6 5 3 127.90 5.15 -6 5 3 113.52 4.06 6 5 -3 114.27 4.40 6 -5 -3 121.78 4.45 -6 -5 4 146.21 6.39 -6 5 4 156.08 6.98 -6 5 4 148.73 6.67 6 -5 -4 128.67 10.60 -6 -5 5 3.65 1.29 -6 5 5 2.57 1.35 6 -5 -5 1.35 0.77 6 -5 -6 52.36 2.33 -6 5 6 54.20 3.06 -6 -5 6 59.85 2.72 6 -5 -7 3.15 0.73 -6 5 7 3.07 1.45 -6 -6 -1 105.78 6.57 -6 6 -1 99.32 6.16 6 6 1 89.55 12.44 6 -6 1 95.16 7.77 -6 -6 0 88.60 4.50 -6 6 0 89.55 4.45 6 6 0 81.92 8.32 6 -6 0 81.01 3.45 -6 -6 1 26.40 3.46 -6 6 1 25.11 3.10 -6 6 1 21.63 1.99 6 6 -1 18.32 4.19 6 -6 -1 17.62 2.27 -6 -6 2 49.83 3.39 -6 6 2 49.99 3.55 -6 6 2 49.19 2.86 6 6 -2 55.47 3.19 6 -6 -2 41.40 6.73 -6 -6 3 122.91 5.79 -6 6 3 137.21 6.74 -6 6 3 126.07 5.63 6 6 -3 127.31 5.67 6 -6 -3 128.73 10.43 -6 -6 4 135.61 5.95 -6 6 4 141.84 6.65 -6 6 4 130.24 5.96 6 -6 -4 130.24 5.85 6 -6 -5 9.90 1.52 -6 -6 5 7.86 1.24 -6 6 5 13.39 2.06 6 -6 -5 6.78 1.37 6 -6 -6 6.65 1.20 -6 -6 6 9.25 1.52 6 -6 -7 1.33 0.98 -6 6 7 1.69 1.41 -6 -7 -1 38.81 3.43 6 7 1 39.59 7.04 6 -7 1 37.73 6.43 -6 -7 0 2.72 1.92 -6 7 0 4.74 2.60 6 7 0 4.94 1.77 6 -7 0 4.23 1.35 -6 -7 1 14.27 2.44 -6 7 1 17.44 2.90 -6 7 1 14.36 1.83 6 -7 -1 17.24 2.89 -6 -7 2 5.61 2.31 -6 7 2 4.06 1.26 6 7 -2 3.44 1.39 6 -7 -2 2.71 0.68 -6 -7 3 49.28 3.45 -6 7 3 44.85 3.51 -6 7 3 39.04 2.62 6 -7 -3 36.73 5.08 -6 -7 4 88.75 4.42 -6 7 4 86.22 4.61 -6 7 4 82.17 4.15 6 -7 -4 77.49 7.34 6 -7 -5 28.44 2.88 -6 7 5 26.48 3.01 -6 -7 5 27.18 2.97 6 -7 -6 6.53 1.32 -6 7 6 7.41 1.93 -6 -7 6 8.23 1.67 6 -7 -7 12.70 3.01 -6 7 7 20.26 2.80 -6 -8 -1 61.10 4.30 -6 8 -1 57.21 3.88 6 8 1 48.95 8.39 6 -8 1 44.02 6.77 -6 -8 0 38.60 3.58 6 8 0 37.00 5.30 6 -8 0 32.68 4.99 -6 -8 1 69.97 3.96 -6 8 1 62.82 3.78 -6 8 1 63.64 3.30 6 8 -1 69.36 3.85 6 -8 -1 62.92 6.57 -6 -8 2 47.68 3.59 -6 8 2 50.13 4.31 6 8 -2 41.98 2.98 6 -8 -2 42.46 4.85 -6 -8 3 62.25 3.79 -6 8 3 50.62 3.72 -6 8 3 55.34 4.86 6 -8 -3 58.60 4.71 -6 -8 4 99.39 4.66 -6 8 4 92.30 4.48 -6 8 4 91.27 4.41 6 -8 -4 86.93 7.70 6 -8 -5 5.77 1.11 -6 8 5 5.40 1.63 -6 -8 5 4.65 1.91 6 -8 -6 20.28 4.01 -6 8 6 21.29 3.14 -6 -8 6 23.68 3.04 6 -8 -7 5.98 1.56 -6 8 7 9.94 1.75 -6 -9 -1 27.71 2.69 -6 9 -1 32.44 2.92 6 9 1 25.82 4.76 -6 -9 0 32.69 4.49 -6 9 0 27.16 4.16 -6 9 0 28.56 3.39 6 9 0 23.28 2.98 6 -9 0 27.62 4.39 -6 -9 1 9.85 2.98 -6 9 1 2.65 1.86 6 9 -1 1.03 0.94 6 -9 -1 2.43 1.30 -6 -9 2 17.72 2.77 -6 9 2 10.85 1.98 -6 9 2 16.37 2.21 6 -9 -2 17.65 3.10 -6 -9 3 64.50 3.52 -6 9 3 68.49 3.80 -6 9 3 64.92 3.52 6 -9 -3 64.37 6.32 -6 -9 4 26.83 2.68 -6 9 4 30.22 3.49 6 -9 -4 20.09 3.75 6 -9 -5 13.06 1.77 -6 9 5 9.96 2.27 -6 -9 5 6.64 1.34 6 -9 -6 10.88 2.40 -6 9 6 12.21 2.21 -6 -9 6 17.54 2.79 6 -9 -7 81.30 5.68 -6 9 7 105.74 5.98 -6 -10 0 22.28 3.40 -6 10 0 26.58 4.21 -6 10 0 22.07 3.16 6 10 0 23.23 3.53 6 -10 0 18.46 4.08 -6 -10 1 21.37 2.61 -6 10 1 17.63 2.06 -6 10 1 20.66 1.98 6 10 -1 12.67 1.41 6 -10 -1 17.80 3.25 -6 -10 2 17.98 2.70 -6 10 2 22.08 3.34 -6 10 2 22.50 2.62 6 -10 -2 17.12 2.72 -6 -10 3 69.14 3.96 -6 10 3 69.08 4.20 -6 10 3 58.76 3.46 6 -10 -3 55.22 5.43 6 -10 -4 13.52 1.73 -6 -10 4 15.77 1.85 -6 10 4 15.75 2.44 6 -10 -4 15.53 2.85 6 -10 -5 5.74 1.29 -6 10 5 11.47 2.04 -6 -10 5 8.49 1.66 6 -10 -6 11.34 3.14 -6 10 6 19.88 3.32 -6 -10 6 15.55 2.37 -6 -11 0 7.67 2.44 -6 11 0 0.39 1.56 -6 11 0 2.27 1.16 6 11 0 0.43 0.99 6 -11 0 1.27 1.41 -6 -11 1 14.67 2.67 -6 11 1 21.14 2.99 -6 11 1 13.57 2.25 6 -11 -1 14.26 3.34 -6 -11 2 18.11 2.54 -6 11 2 17.58 2.30 6 -11 -2 11.38 2.32 -6 -11 3 52.01 3.15 -6 11 3 65.75 4.36 -6 11 3 66.58 3.94 6 -11 -3 57.41 5.57 -6 11 4 46.74 3.37 6 -11 -4 29.87 5.77 6 -11 -5 18.43 3.73 -6 11 5 25.18 3.80 -6 -11 5 28.22 3.86 6 -11 -6 28.24 5.39 -6 11 6 31.48 3.18 -6 -11 6 31.94 2.82 -6 -12 0 68.00 4.74 -6 12 0 66.29 5.00 -6 12 0 64.49 4.00 6 -12 0 66.40 4.25 -6 -12 1 15.79 2.43 -6 12 1 20.73 2.93 6 -12 -1 21.78 2.82 -6 -12 2 98.56 4.00 -6 12 2 105.67 4.93 -6 12 2 105.52 4.33 6 -12 -2 101.69 4.03 -6 -12 3 96.56 3.95 -6 12 3 96.78 4.36 -6 12 3 100.78 4.41 6 -12 -3 88.54 7.00 6 -12 -4 56.36 3.24 -6 12 4 53.28 3.39 6 -12 -4 41.45 6.61 -6 -12 4 47.36 3.11 6 -12 -5 3.40 0.83 -6 12 5 5.59 2.46 -6 -12 5 2.88 1.64 6 -12 -6 5.22 1.68 -6 12 6 14.17 2.37 -6 -12 6 11.39 2.15 -6 -13 0 3.08 1.38 -6 13 0 7.59 1.69 -6 13 0 5.38 1.77 6 -13 0 5.90 1.61 -6 -13 1 12.48 2.66 -6 13 1 12.58 2.47 -6 13 1 12.53 2.29 6 -13 -1 10.53 2.04 -6 -13 2 24.18 3.60 -6 13 2 13.40 2.88 -6 13 2 14.02 2.30 6 -13 -2 18.49 2.80 -6 -13 3 81.22 3.46 -6 13 3 86.81 4.01 -6 13 3 90.87 4.26 6 -13 -3 58.01 6.83 6 -13 -4 70.61 4.92 -6 13 4 63.47 4.87 6 -13 -4 57.20 6.87 -6 -13 4 82.81 5.97 6 -13 -5 59.48 8.27 -6 13 5 59.84 4.77 -6 -13 5 62.31 4.59 6 -13 -6 37.36 6.08 -6 13 6 44.06 3.23 -6 -13 6 47.30 3.35 -6 -14 1 20.75 3.20 -6 14 1 20.35 3.67 -6 14 1 13.56 2.30 6 -14 -1 15.63 2.17 -6 -14 2 85.28 5.76 -6 14 2 81.15 5.73 -6 14 2 78.62 5.57 6 -14 -2 75.21 5.01 -6 14 3 80.86 6.41 -6 14 3 67.19 4.95 6 -14 -3 58.62 7.30 6 -14 -4 24.07 3.41 -6 14 4 22.96 3.52 -6 -14 4 28.14 3.65 6 -14 -5 9.37 2.94 -6 14 5 12.07 1.90 -6 -14 5 8.49 1.85 -6 -15 1 16.73 2.61 -6 15 1 21.99 3.87 -6 15 1 12.82 2.17 6 -15 -1 11.02 1.84 -6 -15 2 57.08 4.31 -6 15 2 68.67 5.56 -6 15 2 70.90 5.34 6 -15 -2 58.35 4.18 -6 15 3 61.16 4.99 6 -15 -3 42.79 5.83 -6 -15 3 63.98 4.92 6 -15 -4 23.71 3.34 -6 15 4 31.27 4.81 -6 -15 4 21.73 3.73 6 -15 -5 12.84 3.48 -6 15 5 12.03 2.20 -6 -15 5 17.82 2.65 -6 -16 1 78.44 4.61 -6 16 1 74.81 4.58 6 -16 -1 87.39 4.85 -6 -16 2 20.06 2.64 -6 16 2 16.41 2.66 6 -16 -2 17.18 2.25 -6 16 3 30.03 2.59 6 -16 -3 28.60 3.45 -6 -16 3 32.42 3.01 6 -16 -4 16.19 2.37 -6 16 4 18.18 3.00 -6 -16 4 20.09 2.88 -6 16 5 7.17 2.45 -6 17 2 15.66 2.24 -6 17 2 24.57 2.73 6 -17 -2 22.39 2.12 -6 -17 2 24.16 2.49 6 -17 -3 62.91 4.11 -6 17 3 71.79 4.99 6 -17 -3 64.13 3.57 -6 -17 3 66.82 4.95 6 -17 -4 77.15 4.60 -6 17 4 70.94 4.60 -6 -17 4 86.82 5.40 -7 0 1 156.55 8.28 7 0 -1 153.08 7.75 -7 0 2 153.27 10.24 7 0 -2 130.29 14.47 -7 0 3 296.07 35.37 7 0 -3 284.58 17.55 -7 0 4 20.79 3.43 7 0 -4 17.48 3.34 -7 0 5 90.82 6.34 -7 1 1 18.45 2.86 -7 -1 1 21.80 3.12 7 1 -1 8.02 1.93 7 -1 -1 13.75 2.79 -7 1 2 25.44 4.01 -7 -1 2 27.48 4.34 7 -1 -2 16.99 3.82 7 1 -2 16.85 3.97 -7 -1 3 15.75 3.04 -7 1 3 14.32 3.04 7 1 -3 6.51 1.61 7 -1 -3 3.34 1.43 -7 -1 4 13.17 2.42 -7 1 4 16.20 2.82 7 1 -4 15.77 2.20 7 -1 -4 9.80 2.16 -7 -1 5 61.61 4.65 -7 1 5 56.45 4.43 7 -1 -5 41.67 3.08 -7 1 6 5.37 1.62 -7 -2 1 58.58 3.99 -7 2 1 49.32 3.60 7 2 -1 40.17 6.08 7 -2 -1 52.82 5.05 -7 -2 2 36.33 3.67 -7 2 2 19.41 3.45 7 2 -2 27.85 6.35 7 -2 -2 23.26 5.02 -7 -2 3 171.43 10.57 -7 2 3 192.52 11.99 7 2 -3 159.85 14.74 7 -2 -3 173.86 10.59 -7 -2 4 24.58 3.42 -7 2 4 17.88 2.96 7 2 -4 22.55 2.82 7 -2 -4 18.19 3.89 -7 -2 5 17.21 2.65 -7 2 5 17.12 2.91 7 -2 -5 14.79 2.23 -7 2 6 18.28 1.78 -7 -3 1 16.03 2.17 -7 3 1 15.39 2.29 7 3 -1 15.79 3.31 7 -3 -1 17.06 3.11 -7 -3 2 50.80 4.71 -7 3 2 38.52 3.51 7 3 -2 39.52 5.55 7 -3 -2 31.35 6.31 -7 -3 3 6.75 2.40 -7 3 3 9.94 2.71 7 3 -3 1.78 0.97 7 -3 -3 2.98 1.12 -7 -3 4 22.19 3.20 -7 3 4 30.24 4.14 7 3 -4 31.29 3.83 7 -3 -4 25.27 5.25 -7 -3 5 38.87 3.33 -7 3 5 47.91 4.10 7 -3 -5 45.39 3.39 -7 3 6 5.88 1.34 -7 -4 1 38.93 3.84 -7 4 1 35.87 3.02 7 4 -1 24.99 5.67 7 -4 -1 27.57 3.69 -7 -4 2 88.38 6.46 -7 4 2 85.70 6.49 7 4 -2 64.90 9.34 7 -4 -2 64.85 7.41 -7 -4 3 48.20 4.19 -7 4 3 33.01 4.48 7 4 -3 36.39 3.02 7 -4 -3 31.01 6.34 -7 -4 4 79.28 5.50 -7 4 4 75.71 5.26 7 -4 -4 69.61 7.93 -7 -4 5 14.43 2.60 -7 4 5 13.15 2.69 7 -4 -5 9.35 1.56 -7 4 6 5.28 1.47 -7 -5 1 14.58 2.64 -7 5 1 11.00 2.24 7 5 -1 7.87 1.60 -7 -5 2 59.99 4.26 -7 5 2 57.86 4.15 7 5 -2 47.26 7.09 7 -5 -2 45.02 6.41 -7 -5 3 4.50 2.16 -7 5 3 7.77 2.04 7 5 -3 2.07 1.06 -7 -5 4 19.69 3.22 -7 5 4 19.12 3.41 7 -5 -4 17.38 3.17 -7 5 5 10.13 2.25 -7 5 6 17.71 1.90 -7 5 6 29.53 2.44 -7 -6 2 82.38 5.33 -7 6 2 81.72 5.50 7 6 -2 82.20 5.15 7 -6 -2 75.91 7.56 -7 -6 3 14.38 2.85 -7 6 3 9.37 2.11 7 6 -3 15.15 2.53 7 -6 -3 13.51 2.49 -7 -6 4 95.11 6.71 -7 6 4 90.16 6.61 7 -6 -4 85.02 5.77 -7 6 5 17.16 2.83 -7 -7 2 16.79 2.84 -7 7 2 12.46 3.13 7 7 -2 14.36 2.14 7 -7 -2 11.87 2.77 -7 -7 3 4.37 2.11 -7 7 3 1.51 1.86 7 -7 -3 1.58 1.05 -7 -7 4 54.27 4.04 -7 7 4 56.43 4.33 7 -7 -4 34.07 5.39 -7 7 5 11.40 3.07 -7 7 5 7.90 2.38 -7 -8 2 75.55 4.45 -7 8 2 79.75 5.19 7 8 -2 74.97 4.26 7 -8 -2 58.61 5.73 -7 -8 3 51.74 3.87 -7 8 3 49.94 4.17 7 -8 -3 40.47 7.37 -7 -8 4 49.12 3.65 -7 8 4 51.46 3.90 7 -8 -4 35.74 7.07 -7 8 5 11.09 1.68 -7 8 5 10.52 1.75 -7 -9 2 16.18 1.91 -7 9 2 21.97 2.91 7 -9 -2 17.95 2.68 -7 -9 3 18.70 3.17 -7 9 3 19.93 3.49 7 -9 -3 9.44 2.89 -7 9 4 22.49 3.11 -7 9 4 27.81 3.74 7 -9 -4 16.33 3.77 -7 9 5 18.68 2.33 -7 9 5 18.43 2.21 -7 -9 5 11.56 1.88 -7 -10 3 102.30 5.44 -7 10 3 109.88 6.20 7 -10 -3 80.14 9.37 -7 10 4 75.37 5.09 -7 10 4 64.06 4.13 7 -10 -4 36.30 6.62 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 21082 _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received'