data_baran605 _audit_creation_date 2016-08-09 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.07.26 svn.r3321 for OlexSys, GUI svn.r5206) ; _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 'C18 H18 F2 O3 S2' _chemical_formula_sum 'C18 H18 F2 O3 S2' _chemical_formula_weight 384.44 _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' 0.0181 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' 'F' 'F' 0.0727 0.0534 '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' 'S' 'S' 0.3331 0.5567 '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 7.8306(11) _cell_length_b 5.4318(7) _cell_length_c 20.139(3) _cell_angle_alpha 90 _cell_angle_beta 98.442(6) _cell_angle_gamma 90 _cell_volume 847.33(19) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7313 _cell_measurement_temperature 100 _cell_measurement_theta_max 68.069 _cell_measurement_theta_min 2.212 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 3.181 _exptl_absorpt_correction_T_max 0.3200 _exptl_absorpt_correction_T_min 0.1783 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1125 before and 0.0627 after correction. The Ratio of minimum to maximum transmission is 0.5572. 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 1.507 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 400 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_unetI/netI 0.0452 _diffrn_reflns_Laue_measured_fraction_full 0.984 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 7769 _diffrn_reflns_point_group_measured_fraction_full 0.948 _diffrn_reflns_point_group_measured_fraction_max 0.945 _diffrn_reflns_theta_full 68.000 _diffrn_reflns_theta_max 68.505 _diffrn_reflns_theta_min 2.218 _diffrn_ambient_temperature 100 _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.6 _diffrn_detector_type 'Bruker SMART CCD 6000 area detector' _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART CCD 6000 area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'sealed X-ray tube' _diffrn_source_target Mo _diffrn_standards_number 0 _reflns_Friedel_coverage 0.729 _reflns_Friedel_fraction_full 0.902 _reflns_Friedel_fraction_max 0.899 _reflns_number_gt 2922 _reflns_number_total 2963 _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 ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.267 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.050 _refine_ls_abs_structure_details ; Flack x determined using 1215 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.048(7) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 2963 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0269 _refine_ls_restrained_S_all 1.055 _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^)+(0.0354P)^2^+0.1044P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.0675 _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: C5(H5), C7(H7) 2.b Secondary CH2 refined with riding coordinates: C6(H6A,H6B), C13(H13A,H13B), C14(H14A,H14B) 2.c Aromatic/amide H refined with riding coordinates: C1(H1), C3(H3), C9(H9), C10(H10), C16(H16), C17(H17), C18(H18) 2.d Idealised Me refined as rotating group: C12(H12A,H12B,H12C) ; _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 0.03012(6) 0.41946(10) 0.21524(3) 0.01984(15) Uani 1 1 d . . . . . S2 S 0.58183(7) 0.07590(9) 0.29492(3) 0.02146(15) Uani 1 1 d . . . . . F1 F -0.3857(2) 1.0175(3) 0.08178(9) 0.0356(4) Uani 1 1 d . . . . . F2 F -0.1709(3) 0.3756(4) -0.03549(9) 0.0487(5) Uani 1 1 d . . . . . O1 O 0.8132(2) 0.2251(3) 0.58512(8) 0.0241(4) Uani 1 1 d . . . . . O2 O -0.0658(2) 0.4805(4) 0.26833(9) 0.0301(4) Uani 1 1 d . . . . . O3 O 0.0664(2) 0.1656(3) 0.20257(10) 0.0290(4) Uani 1 1 d . . . . . C1 C -0.2805(3) 0.7003(5) 0.02187(13) 0.0274(5) Uani 1 1 d . . . . . H1 H -0.3466 0.7577 -0.0185 0.033 Uiso 1 1 calc R . . . . C2 C -0.2832(3) 0.8176(5) 0.08182(13) 0.0244(5) Uani 1 1 d . . . . . C3 C -0.1888(3) 0.7436(4) 0.14151(12) 0.0212(5) Uani 1 1 d . . . . . H3 H -0.1926 0.8309 0.1821 0.025 Uiso 1 1 calc R . . . . C4 C -0.0879(3) 0.5348(4) 0.13933(12) 0.0197(5) Uani 1 1 d . . . . . C5 C 0.2283(3) 0.5863(4) 0.22890(11) 0.0180(4) Uani 1 1 d . . . . . H5 H 0.2059 0.7625 0.2391 0.022 Uiso 1 1 calc R . . . . C6 C 0.3432(3) 0.4656(4) 0.28940(11) 0.0206(5) Uani 1 1 d . . . . . H6A H 0.3758 0.5875 0.3256 0.025 Uiso 1 1 calc R . . . . H6B H 0.2815 0.3276 0.3076 0.025 Uiso 1 1 calc R . . . . C7 C 0.5038(3) 0.3717(4) 0.26162(11) 0.0182(5) Uani 1 1 d . . . . . H7 H 0.5984 0.4962 0.2708 0.022 Uiso 1 1 calc R . . . . C8 C 0.6464(3) 0.1420(4) 0.38123(12) 0.0189(5) Uani 1 1 d . . . . . C9 C 0.7534(3) 0.3385(4) 0.40301(12) 0.0202(5) Uani 1 1 d . . . . . H9 H 0.7880 0.4497 0.3711 0.024 Uiso 1 1 calc R . . . . C10 C 0.8105(3) 0.3742(4) 0.47089(12) 0.0200(5) Uani 1 1 d . . . . . H10 H 0.8821 0.5109 0.4853 0.024 Uiso 1 1 calc R . . . . C11 C 0.7628(3) 0.2096(5) 0.51760(12) 0.0182(5) Uani 1 1 d . . . . . C12 C 0.9257(3) 0.4221(5) 0.60891(12) 0.0274(5) Uani 1 1 d . . . . . H12A H 1.0329 0.4087 0.5895 0.041 Uiso 1 1 calc GR . . . . H12B H 0.9521 0.4139 0.6580 0.041 Uiso 1 1 calc GR . . . . H12C H 0.8695 0.5795 0.5957 0.041 Uiso 1 1 calc GR . . . . C13 C 0.4496(3) 0.3484(4) 0.18579(11) 0.0199(5) Uani 1 1 d . . . . . H13A H 0.5507 0.3574 0.1616 0.024 Uiso 1 1 calc R . . . . H13B H 0.3872 0.1921 0.1742 0.024 Uiso 1 1 calc R . . . . C14 C 0.3309(3) 0.5699(5) 0.16967(11) 0.0206(4) Uani 1 1 d . . . . . H14A H 0.2526 0.5446 0.1269 0.025 Uiso 1 1 calc R . . . . H14B H 0.3989 0.7218 0.1661 0.025 Uiso 1 1 calc R . . . . C15 C -0.1771(3) 0.4946(5) 0.02298(13) 0.0296(6) Uani 1 1 d . . . . . C16 C -0.0799(3) 0.4076(5) 0.08048(13) 0.0255(5) Uani 1 1 d . . . . . H16 H -0.0098 0.2652 0.0798 0.031 Uiso 1 1 calc R . . . . C17 C 0.5963(3) -0.0189(4) 0.42850(12) 0.0207(5) Uani 1 1 d . . . . . H17 H 0.5206 -0.1515 0.4142 0.025 Uiso 1 1 calc R . . . . C18 C 0.6557(3) 0.0123(4) 0.49622(13) 0.0207(5) Uani 1 1 d . . . . . H18 H 0.6232 -0.1012 0.5280 0.025 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 0.0167(2) 0.0205(3) 0.0221(3) 0.0025(2) 0.00223(19) -0.0026(2) S2 0.0268(3) 0.0157(3) 0.0209(3) -0.0008(2) 0.0001(2) 0.0028(2) F1 0.0335(8) 0.0336(9) 0.0376(8) -0.0013(7) -0.0023(6) 0.0143(7) F2 0.0590(11) 0.0565(13) 0.0271(9) -0.0204(8) -0.0058(8) 0.0131(9) O1 0.0224(8) 0.0305(9) 0.0190(8) 0.0035(7) 0.0019(6) -0.0055(7) O2 0.0216(8) 0.0446(11) 0.0251(9) 0.0061(8) 0.0063(7) -0.0029(8) O3 0.0287(9) 0.0183(8) 0.0383(10) 0.0031(7) -0.0011(8) -0.0043(7) C1 0.0248(12) 0.0323(13) 0.0234(13) -0.0012(10) -0.0026(9) -0.0014(11) C2 0.0173(10) 0.0240(11) 0.0309(13) -0.0009(10) 0.0007(9) 0.0005(9) C3 0.0183(10) 0.0219(11) 0.0237(12) -0.0043(9) 0.0036(9) -0.0020(9) C4 0.0156(9) 0.0211(11) 0.0223(11) -0.0007(9) 0.0024(8) -0.0029(9) C5 0.0180(9) 0.0162(10) 0.0196(10) -0.0009(9) 0.0019(8) 0.0007(9) C6 0.0197(10) 0.0240(12) 0.0180(11) -0.0003(9) 0.0026(8) 0.0029(9) C7 0.0185(10) 0.0164(11) 0.0194(11) 0.0004(8) 0.0021(8) -0.0003(8) C8 0.0164(10) 0.0182(10) 0.0217(11) 0.0004(9) 0.0019(8) 0.0043(8) C9 0.0218(10) 0.0174(10) 0.0217(11) 0.0041(9) 0.0042(8) 0.0004(9) C10 0.0178(10) 0.0188(11) 0.0235(12) 0.0008(9) 0.0040(8) -0.0019(8) C11 0.0137(10) 0.0219(11) 0.0191(11) 0.0009(9) 0.0026(8) 0.0035(8) C12 0.0294(12) 0.0289(12) 0.0231(12) -0.0022(11) 0.0018(9) -0.0077(11) C13 0.0207(10) 0.0230(11) 0.0168(11) -0.0009(9) 0.0051(8) 0.0003(9) C14 0.0206(10) 0.0214(11) 0.0199(11) 0.0032(10) 0.0032(8) -0.0008(10) C15 0.0312(13) 0.0335(14) 0.0228(13) -0.0089(10) -0.0004(10) -0.0017(10) C16 0.0236(10) 0.0234(11) 0.0291(12) -0.0058(10) 0.0026(9) 0.0009(10) C17 0.0167(9) 0.0179(10) 0.0272(12) 0.0014(9) 0.0018(8) 0.0000(8) C18 0.0172(10) 0.0199(11) 0.0256(12) 0.0054(9) 0.0048(8) -0.0018(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O2 1.4325(19) . ? S1 O3 1.4383(19) . ? S1 C4 1.780(2) . ? S1 C5 1.784(2) . ? S2 C7 1.812(2) . ? S2 C8 1.774(2) . ? F1 C2 1.350(3) . ? F2 C15 1.350(3) . ? O1 C11 1.362(3) . ? O1 C12 1.424(3) . ? C1 H1 0.9500 . ? C1 C2 1.368(4) . ? C1 C15 1.378(4) . ? C2 C3 1.376(4) . ? C3 H3 0.9500 . ? C3 C4 1.386(3) . ? C4 C16 1.381(4) . ? C5 H5 1.0000 . ? C5 C6 1.550(3) . ? C5 C14 1.535(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.537(3) . ? C7 H7 1.0000 . ? C7 C13 1.529(3) . ? C8 C9 1.388(3) . ? C8 C17 1.391(3) . ? C9 H9 0.9500 . ? C9 C10 1.388(3) . ? C10 H10 0.9500 . ? C10 C11 1.388(3) . ? C11 C18 1.390(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.526(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.373(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C17 C18 1.385(4) . ? C18 H18 0.9500 . ? 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 119.56(12) . . ? O2 S1 C4 107.25(11) . . ? O2 S1 C5 107.87(11) . . ? O3 S1 C4 106.03(11) . . ? O3 S1 C5 108.93(11) . . ? C4 S1 C5 106.49(10) . . ? C8 S2 C7 102.42(10) . . ? C11 O1 C12 117.19(18) . . ? C2 C1 H1 121.7 . . ? C2 C1 C15 116.7(2) . . ? C15 C1 H1 121.7 . . ? F1 C2 C1 117.4(2) . . ? F1 C2 C3 118.6(2) . . ? C1 C2 C3 124.0(2) . . ? C2 C3 H3 121.7 . . ? C2 C3 C4 116.6(2) . . ? C4 C3 H3 121.7 . . ? C3 C4 S1 119.15(18) . . ? C16 C4 S1 118.53(19) . . ? C16 C4 C3 122.3(2) . . ? S1 C5 H5 110.1 . . ? C6 C5 S1 107.31(15) . . ? C6 C5 H5 110.1 . . ? C14 C5 S1 113.17(16) . . ? C14 C5 H5 110.1 . . ? C14 C5 C6 106.08(17) . . ? C5 C6 H6A 110.7 . . ? C5 C6 H6B 110.7 . . ? H6A C6 H6B 108.8 . . ? C7 C6 C5 105.41(18) . . ? C7 C6 H6A 110.7 . . ? C7 C6 H6B 110.7 . . ? S2 C7 H7 109.3 . . ? C6 C7 S2 114.14(16) . . ? C6 C7 H7 109.3 . . ? C13 C7 S2 108.99(15) . . ? C13 C7 C6 105.58(18) . . ? C13 C7 H7 109.3 . . ? C9 C8 S2 122.50(18) . . ? C9 C8 C17 119.0(2) . . ? C17 C8 S2 118.36(17) . . ? C8 C9 H9 119.6 . . ? C8 C9 C10 120.7(2) . . ? C10 C9 H9 119.6 . . ? C9 C10 H10 120.1 . . ? C11 C10 C9 119.8(2) . . ? C11 C10 H10 120.1 . . ? O1 C11 C10 124.7(2) . . ? O1 C11 C18 115.5(2) . . ? C10 C11 C18 119.8(2) . . ? O1 C12 H12A 109.5 . . ? O1 C12 H12B 109.5 . . ? O1 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C13 H13A 111.2 . . ? C7 C13 H13B 111.2 . . ? H13A C13 H13B 109.2 . . ? C14 C13 C7 102.63(18) . . ? C14 C13 H13A 111.2 . . ? C14 C13 H13B 111.2 . . ? C5 C14 H14A 110.8 . . ? C5 C14 H14B 110.8 . . ? C13 C14 C5 104.60(18) . . ? C13 C14 H14A 110.8 . . ? C13 C14 H14B 110.8 . . ? H14A C14 H14B 108.9 . . ? F2 C15 C1 118.0(2) . . ? F2 C15 C16 119.0(2) . . ? C16 C15 C1 123.0(2) . . ? C4 C16 H16 121.2 . . ? C15 C16 C4 117.5(2) . . ? C15 C16 H16 121.2 . . ? C8 C17 H17 119.7 . . ? C18 C17 C8 120.6(2) . . ? C18 C17 H17 119.7 . . ? C11 C18 H18 120.0 . . ? C17 C18 C11 120.0(2) . . ? C17 C18 H18 120.0 . . ? 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 C4 C16 C15 177.6(2) . . . . ? S1 C5 C6 C7 118.32(17) . . . . ? S1 C5 C14 C13 -91.41(18) . . . . ? S2 C7 C13 C14 160.26(15) . . . . ? S2 C8 C9 C10 -175.57(17) . . . . ? S2 C8 C17 C18 174.34(17) . . . . ? F1 C2 C3 C4 178.8(2) . . . . ? F2 C15 C16 C4 179.4(2) . . . . ? O1 C11 C18 C17 179.6(2) . . . . ? O2 S1 C4 C3 30.2(2) . . . . ? O2 S1 C4 C16 -147.70(19) . . . . ? O2 S1 C5 C6 72.52(17) . . . . ? O2 S1 C5 C14 -170.80(16) . . . . ? O3 S1 C4 C3 158.98(18) . . . . ? O3 S1 C4 C16 -18.9(2) . . . . ? O3 S1 C5 C6 -58.67(18) . . . . ? O3 S1 C5 C14 58.01(19) . . . . ? C1 C2 C3 C4 -0.9(4) . . . . ? C1 C15 C16 C4 -0.1(4) . . . . ? C2 C1 C15 F2 -179.6(2) . . . . ? C2 C1 C15 C16 -0.1(4) . . . . ? C2 C3 C4 S1 -177.11(18) . . . . ? C2 C3 C4 C16 0.7(3) . . . . ? C3 C4 C16 C15 -0.2(4) . . . . ? C4 S1 C5 C6 -172.63(15) . . . . ? C4 S1 C5 C14 -55.95(19) . . . . ? C5 S1 C4 C3 -85.1(2) . . . . ? C5 S1 C4 C16 97.0(2) . . . . ? C5 C6 C7 S2 -140.89(16) . . . . ? C5 C6 C7 C13 -21.2(2) . . . . ? C6 C5 C14 C13 26.0(2) . . . . ? C6 C7 C13 C14 37.2(2) . . . . ? C7 S2 C8 C9 -50.4(2) . . . . ? C7 S2 C8 C17 133.81(18) . . . . ? C7 C13 C14 C5 -38.9(2) . . . . ? C8 S2 C7 C6 -64.69(18) . . . . ? C8 S2 C7 C13 177.57(15) . . . . ? C8 C9 C10 C11 1.1(3) . . . . ? C8 C17 C18 C11 1.7(3) . . . . ? C9 C8 C17 C18 -1.6(3) . . . . ? C9 C10 C11 O1 179.1(2) . . . . ? C9 C10 C11 C18 -1.1(3) . . . . ? C10 C11 C18 C17 -0.3(3) . . . . ? C12 O1 C11 C10 -1.3(3) . . . . ? C12 O1 C11 C18 178.8(2) . . . . ? C14 C5 C6 C7 -2.9(2) . . . . ? C15 C1 C2 F1 -179.1(2) . . . . ? C15 C1 C2 C3 0.7(4) . . . . ? C17 C8 C9 C10 0.2(3) . . . . ? _shelx_res_file ; baran605.res created by SHELXL-2014/7 TITL baran605_a.res in P2(1) CELL 1.54184 7.8306 5.4318 20.1393 90 98.442 90 ZERR 2 0.0011 0.0007 0.0025 0 0.006 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H F O S UNIT 36 36 4 6 4 L.S. 10 PLAN -4 0 0 TEMP -173.15 HTAB BOND $H CONF MORE -1 fmap 2 acta 136 OMIT -2 -1 0 OMIT 1 -1 -1 OMIT -1 0 3 OMIT 2 1 0 OMIT -1 1 1 OMIT 2 -1 0 OMIT -1 -1 1 OMIT -2 0 2 REM REM REM WGHT 0.035400 0.104400 FVAR 0.51154 S1 5 0.030118 0.419461 0.215245 11.00000 0.01672 0.02055 = 0.02206 0.00255 0.00223 -0.00259 S2 5 0.581829 0.075901 0.294915 11.00000 0.02680 0.01568 = 0.02088 -0.00085 0.00008 0.00278 F1 3 -0.385695 1.017493 0.081780 11.00000 0.03351 0.03359 = 0.03757 -0.00126 -0.00233 0.01431 F2 3 -0.170948 0.375605 -0.035494 11.00000 0.05899 0.05648 = 0.02711 -0.02041 -0.00580 0.01308 O1 4 0.813248 0.225128 0.585116 11.00000 0.02241 0.03049 = 0.01904 0.00353 0.00188 -0.00549 O2 4 -0.065760 0.480528 0.268326 11.00000 0.02162 0.04456 = 0.02509 0.00606 0.00633 -0.00288 O3 4 0.066401 0.165597 0.202569 11.00000 0.02866 0.01832 = 0.03826 0.00313 -0.00111 -0.00426 C1 1 -0.280490 0.700291 0.021870 11.00000 0.02476 0.03231 = 0.02339 -0.00118 -0.00262 -0.00144 AFIX 43 H1 2 -0.346569 0.757732 -0.018497 11.00000 -1.20000 AFIX 0 C2 1 -0.283223 0.817644 0.081825 11.00000 0.01732 0.02403 = 0.03092 -0.00093 0.00068 0.00052 C3 1 -0.188807 0.743555 0.141514 11.00000 0.01831 0.02185 = 0.02365 -0.00427 0.00359 -0.00202 AFIX 43 H3 2 -0.192558 0.830929 0.182137 11.00000 -1.20000 AFIX 0 C4 1 -0.087911 0.534829 0.139327 11.00000 0.01564 0.02105 = 0.02235 -0.00073 0.00240 -0.00292 C5 1 0.228341 0.586311 0.228895 11.00000 0.01803 0.01624 = 0.01961 -0.00086 0.00194 0.00073 AFIX 13 H5 2 0.205893 0.762544 0.239089 11.00000 -1.20000 AFIX 0 C6 1 0.343153 0.465575 0.289401 11.00000 0.01968 0.02397 = 0.01802 -0.00033 0.00265 0.00288 AFIX 23 H6A 2 0.375829 0.587524 0.325569 11.00000 -1.20000 H6B 2 0.281515 0.327629 0.307566 11.00000 -1.20000 AFIX 0 C7 1 0.503838 0.371663 0.261624 11.00000 0.01849 0.01645 = 0.01939 0.00038 0.00211 -0.00032 AFIX 13 H7 2 0.598378 0.496231 0.270846 11.00000 -1.20000 AFIX 0 C8 1 0.646394 0.142040 0.381232 11.00000 0.01642 0.01824 = 0.02166 0.00043 0.00192 0.00426 C9 1 0.753441 0.338466 0.403010 11.00000 0.02177 0.01745 = 0.02172 0.00410 0.00420 0.00040 AFIX 43 H9 2 0.788034 0.449736 0.371110 11.00000 -1.20000 AFIX 0 C10 1 0.810541 0.374191 0.470887 11.00000 0.01784 0.01880 = 0.02349 0.00082 0.00397 -0.00191 AFIX 43 H10 2 0.882105 0.510930 0.485337 11.00000 -1.20000 AFIX 0 C11 1 0.762819 0.209629 0.517599 11.00000 0.01373 0.02188 = 0.01911 0.00087 0.00261 0.00348 C12 1 0.925702 0.422147 0.608911 11.00000 0.02943 0.02892 = 0.02310 -0.00215 0.00179 -0.00771 AFIX 137 H12A 2 1.032931 0.408689 0.589461 11.00000 -1.50000 H12B 2 0.952072 0.413899 0.657957 11.00000 -1.50000 H12C 2 0.869518 0.579486 0.595697 11.00000 -1.50000 AFIX 0 C13 1 0.449559 0.348379 0.185792 11.00000 0.02069 0.02298 = 0.01680 -0.00089 0.00513 0.00031 AFIX 23 H13A 2 0.550681 0.357402 0.161599 11.00000 -1.20000 H13B 2 0.387240 0.192093 0.174162 11.00000 -1.20000 AFIX 0 C14 1 0.330911 0.569905 0.169672 11.00000 0.02058 0.02139 = 0.01989 0.00324 0.00319 -0.00080 AFIX 23 H14A 2 0.252641 0.544645 0.126943 11.00000 -1.20000 H14B 2 0.398869 0.721797 0.166134 11.00000 -1.20000 AFIX 0 C15 1 -0.177088 0.494616 0.022977 11.00000 0.03124 0.03354 = 0.02278 -0.00891 -0.00037 -0.00170 C16 1 -0.079932 0.407601 0.080483 11.00000 0.02358 0.02340 = 0.02913 -0.00581 0.00262 0.00090 AFIX 43 H16 2 -0.009810 0.265153 0.079827 11.00000 -1.20000 AFIX 0 C17 1 0.596312 -0.018903 0.428502 11.00000 0.01666 0.01787 = 0.02724 0.00137 0.00177 -0.00005 AFIX 43 H17 2 0.520647 -0.151493 0.414213 11.00000 -1.20000 AFIX 0 C18 1 0.655696 0.012267 0.496219 11.00000 0.01720 0.01991 = 0.02558 0.00538 0.00479 -0.00180 AFIX 43 H18 2 0.623236 -0.101164 0.528030 11.00000 -1.20000 AFIX 0 HKLF 4 REM baran605_a.res in P2(1) REM R1 = 0.0269 for 2922 Fo > 4sig(Fo) and 0.0272 for all 2963 data REM 227 parameters refined using 1 restraints END WGHT 0.0354 0.1044 REM Instructions for potential hydrogen bonds EQIV $1 -x-1, y-1/2, -z HTAB C1 F1_$1 EQIV $2 x, y+1, z HTAB C5 O3_$2 EQIV $3 -x+1, y+1/2, -z+1 HTAB C6 O1_$3 EQIV $4 x+1, y, z HTAB C7 O2_$4 HTAB C9 O2_$4 EQIV $5 x+1, y-1, z HTAB C13 F1_$5 EQIV $6 -x, y+1/2, -z HTAB C14 F2_$6 REM Highest difference peak 0.267, deepest hole -0.243, 1-sigma level 0.050 Q1 1 0.5866 0.2261 0.2729 11.00000 0.05 0.27 Q2 1 0.4303 0.0484 0.2969 11.00000 0.05 0.24 Q3 1 0.7382 0.0993 0.2863 11.00000 0.05 0.23 Q4 1 0.1274 0.5443 0.2191 11.00000 0.05 0.23 ; _shelx_res_checksum 61905 _shelx_hkl_file ; -1 0 0 62.3862 3.53891 6 -1 0 0 62.2867 3.54643 6 -1 0 0 60.8550 3.62141 3 -1 0 0 61.4269 3.61792 3 -2 0 0 1.63855 0.43232 3 -2 0 0 1.48022 0.29585 6 -2 0 0 1.78763 0.30207 6 -2 0 0 1.18799 0.39286 3 -3 0 0 52.8999 3.61976 3 -4 0 0 13.8532 1.56706 3 6 0 0 28.8961 2.04624 7 6 0 0 30.9111 1.93869 9 6 0 0 29.2154 1.90780 4 7 0 0 47.6427 3.07507 7 7 0 0 49.2924 2.94727 9 -7 0 0 44.4849 3.27874 5 7 0 0 48.7374 2.91672 4 8 0 0 55.1485 3.32010 9 -8 0 0 56.1151 3.52565 5 8 0 0 56.0630 3.42258 7 8 0 0 54.7296 3.29674 4 -9 0 0 11.2278 0.96786 5 9 0 0 11.4230 0.81845 9 0 -1 0 0.09378 0.11279 3 0 1 0 0.10108 0.28808 6 0 1 0 0.05721 0.26107 6 0 1 0 0.14723 0.11203 3 1 -1 0 509.093 25.3355 3 -1 -1 0 462.074 25.5105 3 1 1 0 436.470 25.5057 6 -1 1 0 452.408 25.2192 3 -1 1 0 461.391 25.9097 6 1 1 0 447.770 25.2137 3 1 1 0 449.519 25.8188 6 -1 1 0 434.456 25.9656 6 2 -1 0 9877.88 596.497 3 -2 -1 0 9902.07 591.273 3 2 1 0 8975.65 549.594 6 2 1 0 8309.98 542.098 6 -2 1 0 9999.99 675.692 6 -3 -1 0 98.9932 5.68036 3 -3 1 0 76.4075 5.85371 6 -3 1 0 86.5657 5.57116 3 -4 -1 0 257.775 15.7473 3 -4 1 0 276.112 15.7382 3 -5 -1 0 36.9093 2.51133 5 6 -1 0 55.8538 3.62017 4 6 -1 0 55.1955 3.84833 7 6 -1 0 58.1425 3.65515 9 -6 -1 0 58.0647 3.92257 5 6 1 0 71.6644 3.88964 7 6 1 0 66.1136 3.73275 9 6 1 0 68.9851 3.74248 4 -7 -1 0 22.7452 1.83626 5 7 -1 0 25.0067 1.58108 9 7 -1 0 23.6225 1.55391 4 7 1 0 21.2202 1.57773 9 7 1 0 21.2260 1.58613 4 7 1 0 22.4932 1.72611 7 8 -1 0 65.7510 3.94955 4 8 -1 0 74.2644 4.00678 9 -8 -1 0 75.2756 4.28686 5 8 1 0 62.0910 3.98247 4 8 1 0 65.1702 4.11244 7 8 1 0 66.8733 4.00020 9 9 -1 0 33.0564 2.01284 9 -9 -1 0 29.4279 2.03750 4 -9 -1 0 33.4321 2.19083 5 9 1 0 35.8135 2.10053 7 9 1 0 38.6757 2.04016 9 0 2 0 678.994 36.5391 6 0 2 0 593.278 35.0948 3 1 -2 0 312.658 16.8155 3 -1 -2 0 329.698 16.8792 3 -1 2 0 316.522 18.2684 6 1 2 0 262.685 16.7648 3 -1 2 0 259.428 16.7673 3 1 2 0 314.957 17.8805 6 2 -2 0 543.046 30.3802 3 -2 -2 0 515.513 30.3266 3 -2 2 0 579.538 31.9184 6 2 2 0 538.896 30.8538 6 -3 -2 0 274.312 16.4778 3 -3 2 0 294.655 17.9080 6 -4 -2 0 331.092 20.0793 3 -4 -2 0 366.471 19.2595 5 -4 2 0 329.508 19.9086 3 5 -2 0 16.4564 1.22232 4 -5 -2 0 17.4682 1.59949 5 5 -2 0 16.8362 1.22189 9 5 2 0 17.8553 1.31369 9 5 2 0 19.3011 1.41420 7 5 2 0 17.7274 1.28077 1 5 2 0 19.1625 1.40011 4 -6 -2 0 74.0633 4.59959 5 6 -2 0 70.6800 4.17741 9 6 -2 0 67.6015 4.13745 4 6 2 0 75.8087 4.30093 4 6 2 0 64.3472 4.17344 1 6 2 0 72.2008 4.36704 7 6 2 0 75.4254 4.26597 9 7 -2 0 1.69185 0.39093 4 7 -2 0 1.20687 0.34428 9 -7 -2 0 1.37100 0.55459 5 7 2 0 2.79332 0.58880 7 7 2 0 2.71576 0.48521 9 -8 -2 0 0.99779 0.41762 5 8 -2 0 0.98378 0.28616 9 -8 -2 0 0.78556 0.34566 4 8 2 0 0.81801 0.38945 7 8 2 0 0.71843 0.27082 9 1 3 0 209.698 13.9153 6 -1 3 0 211.973 14.3286 6 2 3 0 110.555 6.31667 5 -2 3 0 109.868 8.78977 6 4 -3 0 40.9811 2.68515 2 -4 -3 0 45.8848 2.79432 4 4 -3 0 44.3355 2.58047 8 4 -3 0 38.3172 2.54840 4 4 3 0 43.7432 2.76699 7 4 3 0 42.6892 2.66908 1 5 -3 0 12.6846 0.97245 8 -5 -3 0 13.8128 1.23288 4 5 -3 0 12.9894 0.97268 4 -5 -3 0 10.3659 1.32796 5 5 3 0 13.9472 1.19712 7 5 3 0 12.7378 1.05673 1 -6 -3 0 21.2257 1.80102 4 6 3 0 27.1613 1.85937 7 6 3 0 25.4450 1.70426 1 6 3 0 26.6107 1.74309 9 -7 -3 0 31.0834 1.96859 4 7 3 0 26.5854 1.92280 7 -8 -3 0 7.65119 0.64990 4 8 3 0 7.07454 0.70055 7 0 -4 0 13.0569 1.00065 4 0 -4 0 12.2609 1.13639 1 0 -4 0 12.7768 0.97328 8 0 -4 0 12.9522 1.17383 2 1 -4 0 322.777 17.9905 8 1 -4 0 321.846 18.1497 1 -1 -4 0 339.580 18.1906 1 -1 -4 0 303.725 17.9706 8 -1 -4 0 295.855 18.0691 2 1 -4 0 324.977 18.0029 4 1 -4 0 347.763 18.1989 2 -1 -4 0 320.787 18.0337 4 1 4 0 352.321 18.1992 5 -1 4 0 317.723 18.1608 5 2 -4 0 63.7759 4.33975 1 2 -4 0 76.5665 4.42089 2 2 -4 0 73.6905 4.23484 8 2 -4 0 69.8999 4.20800 4 -2 -4 0 75.6212 4.32019 4 2 4 0 71.6324 4.32870 1 2 4 0 75.3683 4.32859 5 3 -4 0 26.3785 1.75159 8 3 -4 0 25.6888 1.88870 2 -3 -4 0 25.8229 1.86388 4 3 -4 0 24.7006 1.70771 4 3 4 0 28.5961 1.92635 7 3 4 0 29.1616 1.88039 1 4 -4 0 60.0437 3.47296 2 4 -4 0 60.9398 3.33049 8 -4 -4 0 61.3165 3.56477 4 4 4 0 48.0407 3.36288 1 4 4 0 48.0461 3.41435 7 -5 -4 0 4.54392 0.78592 4 5 -4 0 4.47702 0.61411 2 5 -4 0 5.06810 0.57232 8 5 4 0 3.49222 0.59501 1 5 4 0 3.28698 0.65665 7 -6 -4 0 30.6247 1.96861 4 6 4 0 26.5832 1.79753 1 6 4 0 27.8683 1.88971 7 -7 -4 0 16.8793 1.10599 4 7 4 0 15.0341 1.07944 1 7 4 0 14.8709 1.10518 7 0 -5 0 0.16932 0.35400 2 0 -5 0 0.14237 0.30326 4 -1 -5 0 1.30889 0.35467 8 1 -5 0 2.38197 0.43684 4 1 -5 0 1.74453 0.50389 2 -1 -5 0 1.93515 0.49132 2 1 5 0 1.56489 0.45241 5 -1 5 0 0.88815 0.41675 5 1 5 0 1.24877 0.42181 1 2 -5 0 18.1344 1.43717 2 2 -5 0 17.7458 1.23691 8 -2 -5 0 17.7286 1.31779 4 2 5 0 15.0305 1.22787 5 -2 5 0 15.0721 1.34156 5 2 5 0 16.5648 1.32719 1 3 -5 0 38.9162 2.51211 2 -3 -5 0 41.3222 2.54304 4 3 -5 0 38.7308 2.36300 8 3 5 0 34.8764 2.44652 1 4 -5 0 9.77821 0.88346 2 4 -5 0 9.68411 0.77982 8 -4 -5 0 8.78818 0.95935 4 4 5 0 7.60297 0.80500 1 -5 -5 0 51.9824 3.08232 4 5 -5 0 47.4028 2.95435 2 5 -5 0 51.9758 2.91931 8 5 5 0 49.7329 2.97690 1 -6 -5 0 9.25795 0.80632 4 6 5 0 13.2947 0.79278 1 0 -6 0 69.6058 3.62571 8 0 -6 0 67.2318 3.70617 2 0 6 0 54.9009 3.65455 1 0 6 0 57.3830 3.70603 5 -1 -6 0 13.0069 0.89997 4 1 -6 0 12.7105 0.90337 8 1 -6 0 12.1234 1.02136 2 1 6 0 10.4856 0.88746 5 -1 6 0 11.1613 1.00136 5 1 6 0 11.3422 0.98183 1 2 -6 0 20.8765 1.45895 8 -2 -6 0 22.0590 1.49888 4 2 -6 0 22.8368 1.60206 2 -2 6 0 24.2132 1.59975 5 2 6 0 25.8801 1.57039 1 -3 -6 0 20.0516 1.39833 4 3 -6 0 22.6559 1.45863 2 3 -6 0 20.0328 1.34621 8 -3 6 0 24.2779 1.45493 5 -9 0 1 28.9200 1.92882 5 9 0 -1 30.2706 1.77894 9 9 0 -1 27.4138 1.74661 4 -8 0 1 6.72543 0.89139 5 8 0 -1 7.63860 0.81667 7 8 0 -1 7.59979 0.75624 4 8 0 -1 7.48908 0.73037 9 -7 0 1 247.574 14.9057 5 7 0 -1 268.993 14.7526 4 7 0 -1 279.790 14.7853 9 7 0 -1 261.985 14.8809 7 6 0 -1 47.0486 3.02218 7 6 0 -1 46.5243 2.87805 4 6 0 -1 49.2351 2.90956 9 -4 0 1 152.568 9.37989 3 -3 0 1 78.0064 4.87853 3 -3 0 1 68.3815 4.34159 6 -3 0 1 79.3548 4.37184 6 -2 0 1 277.797 15.5258 3 -2 0 1 247.066 15.4692 3 -2 0 1 289.386 15.3576 6 -2 0 1 284.457 15.4010 6 1 0 -1 121.442 6.66594 3 -1 0 1 120.273 6.67224 6 -1 0 1 116.861 6.65330 3 1 0 -1 110.149 6.65056 6 0 0 -1 25.2504 1.55622 3 0 0 1 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1.55784 2 -4 5 9 23.0664 1.59639 5 4 5 -9 22.1366 1.50975 1 4 5 -9 22.4497 1.60388 7 3 -5 -9 42.5697 2.66468 2 3 -5 -9 43.5572 2.57811 8 -3 -5 9 41.6017 2.63967 8 3 -5 -9 43.6936 2.60688 4 3 5 -9 43.3439 2.65874 1 -3 5 9 42.6379 2.72677 5 3 5 -9 43.5894 2.74770 7 2 -5 -9 17.2777 1.21066 4 2 -5 -9 16.6773 1.18298 8 -2 -5 9 17.6623 1.33442 8 2 -5 -9 19.2588 1.35222 2 2 5 -9 15.6011 1.23141 5 -2 5 9 17.0426 1.34559 5 2 5 -9 15.0939 1.33728 7 1 -5 -9 63.5137 3.84325 4 1 -5 -9 66.3470 3.94789 2 -1 -5 9 65.1835 4.00332 1 1 -5 -9 70.4577 3.92759 8 -1 -5 9 67.8735 4.00908 2 -1 -5 9 69.9039 3.95122 8 1 -5 -9 57.8528 3.79030 9 -1 5 9 64.4007 3.97968 5 1 5 -9 62.9717 3.99868 7 0 -5 -9 36.8730 2.34692 4 0 -5 -9 43.3801 2.44984 2 0 -5 9 38.9208 2.60469 2 0 -5 9 41.5475 2.56871 1 0 -5 -9 38.2349 2.32604 9 0 5 9 33.6116 2.38828 5 0 5 -9 35.7028 2.53391 5 0 5 -9 35.2334 2.50781 7 1 -5 9 25.0208 1.85138 1 1 -5 9 22.7331 1.56451 8 -1 -5 -9 24.4143 1.60054 4 -1 -5 -9 23.1091 1.56849 9 1 -5 9 25.2170 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9 -2 -3 19 8.14120 0.77315 8 -2 -3 19 9.63597 0.90073 2 2 3 -19 7.97591 0.84621 7 -2 3 19 7.96747 0.80937 2 1 -3 -19 1.26729 0.34148 9 -1 -3 19 1.18106 0.45962 2 -1 -3 19 0.95483 0.31651 8 -1 3 19 2.02701 0.41879 2 0 -3 19 6.91805 0.86663 7 0 -3 -19 7.40360 0.68182 9 0 -3 19 7.49411 0.88672 2 0 3 -19 7.58121 0.81980 5 0 3 19 8.45441 0.77662 2 1 -3 19 96.7597 5.61623 2 1 -3 19 91.8090 5.52056 1 -1 -3 -19 102.982 5.49328 9 1 -3 19 99.1680 5.62483 7 -1 3 -19 91.6901 5.60772 5 2 -3 19 6.45253 0.73115 7 2 -3 19 7.01006 0.70610 1 -2 -3 -19 6.40248 0.57862 9 2 -3 19 7.29664 0.68373 2 -2 3 -19 6.07464 0.70643 5 -2 -4 19 31.5389 1.94222 8 2 -4 -19 30.3766 1.93610 9 2 4 -19 35.1527 2.04612 7 -2 4 19 34.4470 1.98259 2 1 -4 -19 17.5442 1.03579 9 -1 -4 19 16.7313 1.02575 8 -1 -4 19 16.4163 1.10933 2 -1 4 19 14.4991 1.04814 2 1 4 -19 14.1928 1.10601 7 0 -4 -19 69.3623 3.95147 9 0 4 -19 69.6829 4.04185 7 -6 0 20 2.69755 0.40211 8 -5 0 20 0.47153 0.30517 8 -4 0 20 0.12002 0.28090 8 -4 0 20 0.02476 0.28679 2 -3 0 20 30.4667 1.95508 8 -3 0 20 30.1752 2.04674 2 -2 0 20 1.07337 0.35817 8 -2 0 20 1.47937 0.48013 2 -1 0 20 2.23729 0.55454 2 0 0 20 27.8607 1.98059 2 1 0 20 37.7382 2.47051 2 -2 0 -20 33.0783 2.27235 5 2 0 20 37.5350 2.25669 2 -3 0 -20 42.2716 2.66603 5 3 0 20 44.1758 2.64525 1 4 0 20 13.5726 0.97489 1 -6 -1 20 10.9865 0.83345 8 -6 1 20 13.0438 0.85278 8 -5 -1 20 37.0421 2.21645 8 -5 1 20 35.5396 2.19334 8 -4 -1 20 42.0043 2.32417 8 -4 1 20 36.1988 2.26266 8 -4 1 20 32.7701 2.29749 2 -3 -1 20 0.86071 0.39703 2 -3 -1 20 0.78748 0.37855 8 -3 1 20 1.51271 0.39257 8 -3 1 20 1.52335 0.41168 2 -2 -1 20 33.3973 2.26723 8 -2 -1 20 31.4469 2.36806 2 -2 1 20 39.7972 2.36773 8 -2 1 20 40.4313 2.41473 2 -1 -1 20 19.8311 1.55642 2 -1 1 20 19.4115 1.51780 2 0 -1 20 127.635 7.43448 2 0 1 20 128.312 7.37815 2 1 -1 20 42.8543 2.54751 2 1 1 20 38.1293 2.45569 2 -1 1 -20 34.9504 2.48638 5 2 -1 20 27.1581 1.79807 2 2 -1 20 24.2798 1.79557 7 2 -1 20 25.3812 1.77626 1 -2 1 -20 29.0654 1.90738 5 3 -1 20 17.9592 1.34069 1 3 -1 20 18.7688 1.35674 7 -3 1 -20 20.5917 1.43614 5 -5 -2 20 5.78879 0.53652 8 5 -2 -20 5.61557 0.48834 9 -5 2 20 5.50656 0.52053 8 4 -2 -20 38.6201 2.51437 9 -4 -2 20 41.9355 2.57420 8 -4 2 20 44.5403 2.60199 2 -4 2 20 45.7916 2.54149 8 3 -2 -20 19.5082 1.30615 9 -3 -2 20 19.1399 1.40947 2 -3 -2 20 19.9891 1.37305 8 -3 2 20 20.8377 1.42275 2 -3 2 20 18.9773 1.29580 8 2 -2 -20 30.6175 1.89168 9 -2 -2 20 30.1072 2.05028 2 -2 -2 20 29.7581 1.92801 8 -2 2 20 29.9693 2.00190 2 -1 -2 20 32.2138 2.08363 8 1 -2 -20 36.0402 2.09891 9 -1 -2 20 35.4508 2.30248 2 -1 2 20 31.0323 2.18428 2 0 -2 -20 12.5859 0.97067 9 0 -2 20 12.3925 1.16458 2 0 -2 20 12.8910 1.16634 7 0 2 -20 14.1069 1.13357 5 0 2 20 14.0518 1.12337 2 1 -2 20 19.6000 1.46219 2 -1 -2 -20 17.7249 1.26709 9 1 -2 20 18.5901 1.43697 7 -1 2 -20 20.3547 1.47565 5 1 2 20 19.8827 1.35746 2 -2 -2 -20 63.4746 3.62516 9 2 -2 20 62.3926 3.76282 7 2 -2 20 65.4434 3.73976 2 2 -2 20 62.0836 3.71605 1 -2 2 -20 62.5894 3.80511 5 3 -2 20 20.5437 1.47377 7 3 -2 20 20.2643 1.43360 1 -3 2 -20 25.3683 1.54080 5 -4 -3 20 5.03140 0.47403 8 4 -3 -20 4.37040 0.42172 9 -4 3 20 4.03896 0.45959 2 -4 3 20 3.60491 0.41355 8 3 -3 -20 18.4281 1.21106 9 -3 -3 20 16.4857 1.22407 8 -3 3 20 21.3338 1.29007 2 3 3 -20 18.4215 1.26313 7 -2 -3 20 5.90091 0.58252 8 -2 -3 20 5.83094 0.67673 2 2 -3 -20 6.05566 0.57132 9 2 3 -20 5.96544 0.66363 7 -2 3 20 6.17886 0.64080 2 -1 -3 20 72.5916 4.16961 8 1 -3 -20 79.0901 4.20072 9 -1 -3 20 75.0126 4.32437 2 1 3 -20 69.7443 4.29301 7 -1 3 20 69.0718 4.23106 2 0 -3 -20 8.28797 0.65278 9 0 -3 20 7.73602 0.80412 2 0 3 20 6.99656 0.69711 2 1 -3 20 57.6988 3.49133 2 1 -3 20 61.7327 3.50680 7 -1 -3 -20 58.5632 3.38035 9 -1 3 -20 57.4488 3.47201 5 -5 0 21 11.5648 0.85877 8 -4 0 21 7.30372 0.67371 8 -4 0 21 6.10385 0.70145 2 -3 0 21 19.9760 1.37152 8 -3 0 21 20.4088 1.47363 2 -2 0 21 1.20169 0.40937 2 -2 0 21 2.12817 0.41363 8 -1 0 21 70.2832 4.24975 2 0 0 21 10.2132 1.00479 2 1 0 21 15.3290 1.21364 2 2 0 21 39.0999 2.39296 2 -5 -1 21 11.9404 0.85234 8 -5 1 21 11.2584 0.84219 8 -4 -1 21 38.0533 2.21387 8 -4 1 21 36.0848 2.18463 8 -4 1 21 33.9132 2.22224 2 -3 -1 21 0.45127 0.32331 2 -3 -1 21 0.10482 0.30887 8 -3 1 21 0.11941 0.28938 8 -3 1 21 0.28870 0.33560 2 -2 -1 21 6.03292 0.65024 8 -2 -1 21 5.89397 0.77649 2 -2 1 21 5.44488 0.73084 2 -1 -1 21 4.39502 0.75048 2 -1 1 21 5.83301 0.75681 2 0 -1 21 62.7330 3.90492 2 0 1 21 65.8596 3.87874 2 1 -1 21 3.62762 0.62214 2 1 1 21 2.72084 0.47367 2 2 -1 21 59.3975 3.25986 2 -2 1 -21 49.9287 3.24402 5 3 -1 21 1.43940 0.32711 1 -4 -2 21 24.3635 1.48322 8 -4 2 21 22.7013 1.50114 2 -4 2 21 23.0250 1.44169 8 3 -2 -21 0.50680 0.24110 9 -3 -2 21 0.22011 0.29219 2 -3 -2 21 0.25396 0.25214 8 -3 2 21 0.34143 0.43516 8 -3 2 21 0.12843 0.25496 2 2 -2 -21 48.5889 2.87333 9 -2 -2 21 46.8543 2.89481 8 -2 -2 21 50.9088 3.02675 2 -2 2 21 49.9110 2.98977 2 1 -2 -21 12.0721 0.93580 9 -1 -2 21 13.4762 1.14182 2 -1 2 21 14.8785 1.10750 2 0 -2 -21 32.2003 2.08176 9 0 -2 21 34.6421 2.25309 2 0 2 21 36.6344 2.18566 2 1 -2 21 39.4921 2.47879 7 1 -2 21 44.4022 2.53868 2 1 2 21 39.3156 2.41128 2 -1 2 -21 37.8054 2.45859 5 2 -2 21 13.2353 0.95737 2 2 -2 21 12.5077 0.96226 7 3 -3 -21 6.61761 0.51939 9 -3 -3 21 6.93950 0.53931 8 -3 3 21 5.71910 0.54793 2 -2 -3 21 4.66750 0.49712 2 -2 -3 21 4.52366 0.46355 8 2 -3 -21 4.80691 0.44292 9 2 3 -21 4.50393 0.50477 7 -2 3 21 5.43835 0.53229 2 -1 -3 21 21.0257 1.34840 2 1 -3 -21 19.2373 1.23277 9 -1 -3 21 18.2415 1.38756 8 1 3 -21 19.6114 1.32053 7 -1 3 21 19.7626 1.30541 2 0 -3 -21 6.20739 0.50348 9 0 -3 21 6.55655 0.64049 2 0 3 -21 7.07615 0.63678 7 0 3 21 6.08458 0.58392 2 -5 0 22 14.3920 0.95907 8 -4 0 22 2.62608 0.45474 2 -4 0 22 2.10084 0.35159 8 -3 0 22 14.7955 1.04907 8 -3 0 22 14.7791 1.12102 2 -2 0 22 24.4894 1.70833 2 -1 0 22 8.79588 0.89297 2 0 0 22 14.9859 1.20382 2 1 0 22 24.8048 1.65011 2 -4 -1 22 18.9591 1.19520 8 -4 1 22 17.5011 1.20124 2 -4 1 22 17.8067 1.16756 8 -3 -1 22 9.89447 0.82102 2 -3 -1 22 10.0963 0.78049 8 -3 1 22 9.19201 0.83425 2 -3 1 22 8.04371 0.71234 8 -2 -1 22 74.3858 4.51413 8 -2 -1 22 79.7731 4.66309 2 -2 1 22 84.1300 4.66287 2 -1 -1 22 14.7646 1.21630 2 -1 1 22 16.2569 1.22201 2 0 -1 22 9.14731 0.90534 2 0 1 22 9.92184 0.87988 2 1 -1 22 19.8808 1.34485 2 1 1 22 18.2220 1.29225 2 2 -1 22 21.2236 1.36170 2 -3 -2 22 4.49520 0.50860 2 -3 -2 22 4.52385 0.47143 8 -3 2 22 3.78050 0.49802 2 -2 -2 22 10.0357 0.78037 8 -2 -2 22 11.5214 0.89848 2 -2 2 22 10.5752 0.88658 2 -1 -2 22 24.5237 1.64687 2 -1 2 22 23.8886 1.60323 2 0 -2 22 18.6158 1.34418 2 0 2 22 18.9058 1.27985 2 1 -2 22 32.5670 2.01502 2 -4 0 23 18.2570 1.15384 8 -3 0 23 36.3870 2.09715 2 -3 0 23 30.8997 1.97831 8 -2 0 23 0.31265 0.30004 2 -1 0 23 14.0661 1.09760 2 0 0 23 47.8569 2.89684 2 1 0 23 1.52362 0.29891 2 -3 -1 23 7.04809 0.60599 8 -3 -1 23 8.03183 0.67398 2 -3 1 23 8.36617 0.70736 2 -2 -1 23 15.9656 1.13278 2 -2 1 23 14.3026 1.10362 2 -1 -1 23 20.1993 1.41421 2 -1 1 23 20.5200 1.41178 2 0 -1 23 53.6658 3.13111 2 0 1 23 51.1480 3.10236 2 1 -1 23 9.50373 0.73136 2 1 1 23 7.19151 0.74402 2 -2 -2 23 38.6017 2.42460 2 -2 2 23 43.6757 2.45554 2 -1 -2 23 12.9680 0.98086 2 -1 2 23 13.9890 0.96848 2 -2 0 24 14.4361 1.03380 2 -1 0 24 30.0262 1.88130 2 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.3200 _exptl_absorpt_correction_T_min 0.1783 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54180 7.840 5.438 20.142 89.980 98.451 89.978 ) ; _shelx_hkl_checksum 81879 _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received'