data_Baran599 _audit_creation_date 2016-07-28 _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. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C30 H33 F3 O4 S' _chemical_formula_sum 'C30 H33 F3 O4 S' _chemical_formula_weight 546.62 _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 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.6458(2) _cell_length_b 8.1522(3) _cell_length_c 48.2280(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2612.89(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9519 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 68.109 _cell_measurement_theta_min 5.503 _shelx_estimated_absorpt_T_max 0.837 _shelx_estimated_absorpt_T_min 0.766 _exptl_absorpt_coefficient_mu 1.592 _exptl_absorpt_correction_T_max 0.3201 _exptl_absorpt_correction_T_min 0.2155 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0852 before and 0.0676 after correction. The Ratio of minimum to maximum transmission is 0.6732. The \l/2 correction factor is 0.00150. ; _exptl_absorpt_special_details ? _exptl_crystal_colour Colorless _exptl_crystal_colour_primary Colorless _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description Block _exptl_crystal_F_000 1152 _exptl_crystal_size_max 0.177 _exptl_crystal_size_mid 0.153 _exptl_crystal_size_min 0.116 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_unetI/netI 0.0404 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 58 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_number 15810 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 68.000 _diffrn_reflns_theta_max 68.217 _diffrn_reflns_theta_min 1.832 _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker X8 APEX II' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe X-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker Microstar FR-592' _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.692 _reflns_Friedel_fraction_full 0.984 _reflns_Friedel_fraction_max 0.981 _reflns_number_gt 4450 _reflns_number_total 4723 _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 v8.34A (Bruker, 2013)' _computing_data_collection 'APEX2 v2014.11-0 (Bruker, 2014)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _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 0.184 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.038 _refine_ls_abs_structure_details ; Flack x determined using 1706 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.048(9) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 385 _refine_ls_number_reflns 4723 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0391 _refine_ls_restrained_S_all 1.047 _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^)+(0.0362P)^2^+0.9874P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0953 _refine_ls_wR_factor_ref 0.0968 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O4B) = Uanis(O4) Uanis(S1) = Uanis(S1B) Uanis(O3) = Uanis(O3B) Uanis(C5B) = Uanis(C5) 3. Others Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(1) Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1) Sof(S1B)=Sof(O3B)=Sof(O4B)=Sof(H1B)=Sof(H4BC)=Sof(H4BD)=Sof(C5B)=Sof(H5BA)= Sof(H5BB)=1-FVAR(2) Sof(S1)=Sof(O3)=Sof(O4)=Sof(H1A)=Sof(H4AA)=Sof(H4AB)=Sof(C5)=Sof(H5A)= Sof(H5B)=FVAR(2) 4.a Ternary CH refined with riding coordinates: C1(H1A), C1(H1B), C3(H3), C12(H12), C13(H13), C19(H19) 4.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C4(H4AA,H4AB), C4(H4BC,H4BD), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C20(H20A,H20B), C21(H21A,H21B), C5(H5A,H5B), C5B(H5BA,H5BB) 4.c Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C11(H11), C25(H25), C26(H26), C28(H28), C29(H29) 4.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 difmap 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 0.3018(3) 0.6525(2) 0.43059(4) 0.0370(4) Uani 0.750(4) 1 d . . P A 1 S1B S 0.2368(9) 0.6626(9) 0.42771(15) 0.0370(4) Uani 0.250(4) 1 d . . P A 2 F1 F -0.4988(7) 1.0818(7) 0.47253(17) 0.104(3) Uani 0.642(9) 1 d . . P B 1 F2 F -0.2961(10) 1.2776(5) 0.46730(9) 0.0703(16) Uani 0.642(9) 1 d . . P B 1 F3 F -0.2934(14) 1.1506(9) 0.50505(10) 0.086(3) Uani 0.642(9) 1 d . . P B 1 F1B F -0.4517(12) 1.0178(9) 0.49476(15) 0.062(3) Uani 0.358(9) 1 d . . P B 2 F2B F -0.4313(16) 1.1890(18) 0.46255(16) 0.095(5) Uani 0.358(9) 1 d . . P B 2 F3B F -0.262(3) 1.2119(17) 0.4997(4) 0.112(7) Uani 0.358(9) 1 d . . P B 2 O1 O 0.2405(3) 0.2980(3) 0.36957(4) 0.0415(5) Uani 1 1 d . . . . . O2 O 1.5169(3) -0.4065(3) 0.29324(4) 0.0398(5) Uani 1 1 d . . . . . O3 O 0.3654(6) 0.7065(5) 0.40353(6) 0.0494(9) Uani 0.750(4) 1 d . . P A 1 O4 O 0.4507(8) 0.6176(6) 0.45143(8) 0.0442(9) Uani 0.750(4) 1 d . . P A 1 O3B O 0.2356(19) 0.6940(14) 0.39864(19) 0.0494(9) Uani 0.250(4) 1 d . . P A 2 O4B O 0.429(3) 0.656(2) 0.4431(3) 0.0442(9) Uani 0.250(4) 1 d . . P A 2 C1 C 0.1343(5) 0.4764(4) 0.42867(7) 0.0440(8) Uani 1 1 d . . . . . H1A H 0.0629 0.4585 0.4467 0.053 Uiso 0.750(4) 1 calc R . P A 1 H1B H 0.1296 0.4588 0.4492 0.053 Uiso 0.250(4) 1 calc R . P A 2 C2 C 0.2518(5) 0.3229(4) 0.41991(6) 0.0396(8) Uani 1 1 d . . . . . H2A H 0.3921 0.3514 0.4150 0.048 Uiso 1 1 calc R . . . . H2B H 0.2537 0.2409 0.4351 0.048 Uiso 1 1 calc R . . . . C3 C 0.1390(5) 0.2557(5) 0.39458(6) 0.0454(9) Uani 1 1 d . . . . . H3 H 0.1206 0.1343 0.3960 0.055 Uiso 1 1 calc R . . . . C4 C -0.0617(5) 0.3429(6) 0.39459(8) 0.0627(12) Uani 1 1 d . . . . . H4AA H -0.1194 0.3460 0.3757 0.075 Uiso 0.750(4) 1 calc R . P A 1 H4AB H -0.1579 0.2869 0.4071 0.075 Uiso 0.750(4) 1 calc R . P A 1 H4BC H -0.1711 0.2609 0.3931 0.075 Uiso 0.250(4) 1 calc R . P A 2 H4BD H -0.0697 0.4161 0.3783 0.075 Uiso 0.250(4) 1 calc R . P A 2 C6 C 0.4111(4) 0.2107(4) 0.36232(5) 0.0335(7) Uani 1 1 d . . . . . C7 C 0.4678(5) 0.0636(4) 0.37412(6) 0.0362(7) Uani 1 1 d . . . . . H7 H 0.3922 0.0177 0.3889 0.043 Uiso 1 1 calc R . . . . C8 C 0.6376(4) -0.0164(4) 0.36398(5) 0.0324(6) Uani 1 1 d . . . . . H8 H 0.6755 -0.1182 0.3720 0.039 Uiso 1 1 calc R . . . . C9 C 0.7538(4) 0.0469(3) 0.34257(5) 0.0268(6) Uani 1 1 d . . . . . C10 C 0.6936(4) 0.1977(3) 0.33088(5) 0.0264(6) Uani 1 1 d . . . . . C11 C 0.5217(4) 0.2767(4) 0.34081(5) 0.0305(6) Uani 1 1 d . . . . . H11 H 0.4803 0.3773 0.3327 0.037 Uiso 1 1 calc R . . . . C12 C 0.9497(4) -0.0358(3) 0.33361(5) 0.0244(6) Uani 1 1 d . . . . . H12 H 1.0540 -0.0007 0.3473 0.029 Uiso 1 1 calc R . . . . C13 C 1.0221(4) 0.0273(3) 0.30507(5) 0.0225(5) Uani 1 1 d . . . . . H13 H 0.9252 -0.0114 0.2906 0.027 Uiso 1 1 calc R . . . . C14 C 1.0240(4) 0.2135(3) 0.30483(5) 0.0254(6) Uani 1 1 d . . . . . H14A H 1.0845 0.2533 0.2873 0.030 Uiso 1 1 calc R . . . . H14B H 1.1067 0.2547 0.3204 0.030 Uiso 1 1 calc R . . . . C15 C 0.8094(4) 0.2782(3) 0.30748(5) 0.0273(6) Uani 1 1 d . . . . . H15A H 0.8139 0.3981 0.3107 0.033 Uiso 1 1 calc R . . . . H15B H 0.7372 0.2590 0.2898 0.033 Uiso 1 1 calc R . . . . C16 C 0.9447(4) -0.2242(3) 0.33475(6) 0.0286(6) Uani 1 1 d . . . . . H16A H 0.8380 -0.2645 0.3221 0.034 Uiso 1 1 calc R . . . . H16B H 0.9094 -0.2591 0.3538 0.034 Uiso 1 1 calc R . . . . C17 C 1.1469(4) -0.3036(3) 0.32648(5) 0.0287(6) Uani 1 1 d . . . . . H17A H 1.2502 -0.2777 0.3406 0.034 Uiso 1 1 calc R . . . . H17B H 1.1315 -0.4243 0.3256 0.034 Uiso 1 1 calc R . . . . C18 C 1.2143(4) -0.2392(3) 0.29827(5) 0.0265(6) Uani 1 1 d . . . . . C19 C 1.2259(4) -0.0507(3) 0.29934(5) 0.0239(5) Uani 1 1 d . . . . . H19 H 1.3135 -0.0228 0.3155 0.029 Uiso 1 1 calc R . . . . C20 C 1.3442(4) -0.0026(4) 0.27335(6) 0.0293(6) Uani 1 1 d . . . . . H20A H 1.4031 0.1084 0.2752 0.035 Uiso 1 1 calc R . . . . H20B H 1.2582 -0.0063 0.2566 0.035 Uiso 1 1 calc R . . . . C21 C 1.5080(4) -0.1348(4) 0.27240(6) 0.0332(6) Uani 1 1 d . . . . . H21A H 1.5360 -0.1673 0.2530 0.040 Uiso 1 1 calc R . . . . H21B H 1.6341 -0.0936 0.2808 0.040 Uiso 1 1 calc R . . . . C22 C 1.4269(4) -0.2802(4) 0.28882(6) 0.0298(6) Uani 1 1 d . . . . . C23 C 1.0789(4) -0.3067(4) 0.27490(5) 0.0296(6) Uani 1 1 d . . . . . H23A H 0.9378 -0.2822 0.2791 0.044 Uiso 1 1 calc GR . . . . H23B H 1.0969 -0.4257 0.2735 0.044 Uiso 1 1 calc GR . . . . H23C H 1.1159 -0.2550 0.2573 0.044 Uiso 1 1 calc GR . . . . C24 C 0.1203(6) 0.8029(4) 0.44425(6) 0.0455(8) Uani 1 1 d . . . . . C25 C -0.0217(8) 0.8734(5) 0.42738(7) 0.0651(12) Uani 1 1 d . . . . . H25 H -0.0219 0.8511 0.4080 0.078 Uiso 1 1 calc R . . . . C26 C -0.1649(7) 0.9773(4) 0.43873(7) 0.0577(11) Uani 1 1 d . . . . . H26 H -0.2659 1.0243 0.4273 0.069 Uiso 1 1 calc R . . . . C27 C -0.1599(5) 1.0123(4) 0.46693(6) 0.0399(7) Uani 1 1 d . . . . . C28 C -0.0111(5) 0.9449(4) 0.48351(6) 0.0399(7) Uani 1 1 d . . . . . H28 H -0.0046 0.9722 0.5026 0.048 Uiso 1 1 calc R . . . . C29 C 0.1280(5) 0.8379(4) 0.47225(6) 0.0370(7) Uani 1 1 d . . . . . H29 H 0.2279 0.7890 0.4837 0.044 Uiso 1 1 calc R . . . . C30 C -0.3139(6) 1.1222(5) 0.47902(8) 0.0539(9) Uani 1 1 d . . . . . C5 C -0.0200(7) 0.5040(6) 0.40421(8) 0.0405(10) Uani 0.750(4) 1 d . . P A 1 H5A H -0.1439 0.5583 0.4110 0.049 Uiso 0.750(4) 1 calc R . P A 1 H5B H 0.0403 0.5718 0.3893 0.049 Uiso 0.750(4) 1 calc R . P A 1 C5B C -0.092(2) 0.4453(18) 0.4213(2) 0.0405(10) Uani 0.250(4) 1 d . . P A 2 H5BA H -0.1624 0.3823 0.4360 0.049 Uiso 0.250(4) 1 calc R . P A 2 H5BB H -0.1655 0.5488 0.4177 0.049 Uiso 0.250(4) 1 calc R . P A 2 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 0.0424(12) 0.0420(5) 0.0267(6) 0.0027(4) 0.0013(9) 0.0077(8) S1B 0.0424(12) 0.0420(5) 0.0267(6) 0.0027(4) 0.0013(9) 0.0077(8) F1 0.046(3) 0.086(4) 0.182(9) -0.007(5) -0.016(3) -0.004(3) F2 0.097(4) 0.044(2) 0.070(3) 0.0109(17) 0.017(2) 0.021(2) F3 0.104(6) 0.116(7) 0.038(2) 0.015(3) 0.014(3) 0.066(6) F1B 0.067(5) 0.058(4) 0.062(5) 0.006(3) 0.017(4) -0.005(4) F2B 0.074(7) 0.145(13) 0.065(5) 0.049(6) 0.010(5) 0.053(9) F3B 0.069(6) 0.080(9) 0.188(16) -0.094(10) -0.031(10) 0.017(7) O1 0.0315(11) 0.0675(15) 0.0256(9) -0.0093(9) -0.0002(8) 0.0132(12) O2 0.0374(12) 0.0352(12) 0.0468(12) 0.0034(9) 0.0007(10) 0.0136(10) O3 0.058(2) 0.0555(18) 0.0346(15) 0.0075(13) 0.0097(16) 0.003(2) O4 0.0456(19) 0.052(3) 0.035(3) 0.0000(16) -0.007(2) 0.0068(19) O3B 0.058(2) 0.0555(18) 0.0346(15) 0.0075(13) 0.0097(16) 0.003(2) O4B 0.0456(19) 0.052(3) 0.035(3) 0.0000(16) -0.007(2) 0.0068(19) C1 0.0441(19) 0.0443(19) 0.0435(17) -0.0106(15) -0.0055(15) 0.0056(16) C2 0.0489(19) 0.0436(18) 0.0264(13) -0.0041(12) -0.0004(13) 0.0075(16) C3 0.0314(17) 0.070(2) 0.0345(16) -0.0168(16) 0.0074(13) -0.0006(17) C4 0.0305(18) 0.112(4) 0.0459(19) -0.033(2) 0.0034(15) 0.011(2) C6 0.0262(14) 0.0524(18) 0.0219(12) -0.0096(12) -0.0023(11) 0.0072(14) C7 0.0322(16) 0.0560(19) 0.0203(13) 0.0003(12) 0.0027(12) -0.0010(15) C8 0.0326(15) 0.0411(16) 0.0236(13) 0.0038(12) -0.0018(11) 0.0004(13) C9 0.0273(14) 0.0316(14) 0.0213(12) -0.0017(10) -0.0022(11) -0.0010(12) C10 0.0266(13) 0.0293(14) 0.0233(12) -0.0034(10) -0.0030(10) 0.0007(12) C11 0.0296(14) 0.0341(15) 0.0279(13) -0.0068(11) -0.0040(11) 0.0040(13) C12 0.0266(14) 0.0260(13) 0.0208(12) 0.0012(10) -0.0020(11) 0.0008(11) C13 0.0206(13) 0.0250(13) 0.0219(12) 0.0008(10) -0.0006(10) 0.0002(11) C14 0.0248(14) 0.0253(13) 0.0261(12) 0.0002(10) 0.0002(11) 0.0010(12) C15 0.0250(13) 0.0269(13) 0.0301(13) 0.0007(11) 0.0000(11) 0.0032(12) C16 0.0297(14) 0.0300(14) 0.0263(13) 0.0047(11) 0.0011(11) 0.0025(13) C17 0.0314(15) 0.0251(14) 0.0296(13) 0.0033(11) -0.0021(11) 0.0027(12) C18 0.0279(14) 0.0254(14) 0.0263(12) -0.0009(10) -0.0017(11) 0.0030(12) C19 0.0236(13) 0.0243(13) 0.0237(12) -0.0003(9) -0.0035(11) -0.0002(11) C20 0.0283(14) 0.0290(15) 0.0304(14) 0.0009(11) 0.0048(12) 0.0008(12) C21 0.0276(15) 0.0323(15) 0.0396(15) -0.0023(12) 0.0041(12) 0.0029(13) C22 0.0285(14) 0.0326(15) 0.0283(13) -0.0048(12) -0.0041(11) 0.0029(13) C23 0.0275(14) 0.0313(15) 0.0300(13) -0.0039(11) -0.0021(11) -0.0002(12) C24 0.071(2) 0.0348(17) 0.0301(15) 0.0023(13) 0.0021(15) -0.0003(18) C25 0.122(4) 0.044(2) 0.0296(16) 0.0005(14) -0.018(2) 0.017(2) C26 0.089(3) 0.041(2) 0.0432(19) 0.0027(15) -0.0284(19) 0.010(2) C27 0.049(2) 0.0316(16) 0.0395(16) 0.0050(13) -0.0073(14) -0.0072(15) C28 0.0459(19) 0.0450(19) 0.0288(15) -0.0013(13) -0.0039(13) -0.0048(16) C29 0.0421(17) 0.0366(17) 0.0322(15) -0.0011(12) -0.0042(13) -0.0052(15) C30 0.050(2) 0.056(2) 0.056(2) 0.0076(18) -0.0099(18) 0.002(2) C5 0.042(2) 0.050(2) 0.0292(19) -0.0035(17) 0.0020(17) 0.008(2) C5B 0.042(2) 0.050(2) 0.0292(19) -0.0035(17) 0.0020(17) 0.008(2) _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 1.440(4) . ? S1 O4 1.439(4) . ? S1 C1 1.819(4) . ? S1 C24 1.842(4) . ? S1B O3B 1.425(12) . ? S1B O4B 1.479(18) . ? S1B C1 1.664(8) . ? S1B C24 1.595(8) . ? F1 C30 1.310(6) . ? F2 C30 1.392(6) . ? F3 C30 1.284(7) . ? F1B C30 1.463(8) . ? F2B C30 1.239(8) . ? F3B C30 1.283(13) . ? O1 C3 1.424(4) . ? O1 C6 1.383(3) . ? O2 C22 1.209(3) . ? C1 H1A 1.0000 . ? C1 H1B 1.0000 . ? C1 C2 1.535(4) . ? C1 C5 1.579(5) . ? C1 C5B 1.567(14) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.534(4) . ? C3 H3 1.0000 . ? C3 C4 1.512(5) . ? C4 H4AA 0.9900 . ? C4 H4AB 0.9900 . ? C4 H4BC 0.9900 . ? C4 H4BD 0.9900 . ? C4 C5 1.420(6) . ? C4 C5B 1.549(12) . ? C6 C7 1.380(5) . ? C6 C11 1.381(4) . ? C7 H7 0.9500 . ? C7 C8 1.392(4) . ? C8 H8 0.9500 . ? C8 C9 1.388(4) . ? C9 C10 1.410(4) . ? C9 C12 1.528(4) . ? C10 C11 1.396(4) . ? C10 C15 1.515(4) . ? C11 H11 0.9500 . ? C12 H12 1.0000 . ? C12 C13 1.546(3) . ? C12 C16 1.537(4) . ? C13 H13 1.0000 . ? C13 C14 1.518(4) . ? C13 C19 1.521(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.526(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.544(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.525(4) . ? C18 C19 1.539(3) . ? C18 C22 1.522(4) . ? C18 C23 1.544(4) . ? C19 H19 1.0000 . ? C19 C20 1.530(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.533(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.524(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.372(5) . ? C24 C29 1.381(4) . ? C25 H25 0.9500 . ? C25 C26 1.387(6) . ? C26 H26 0.9500 . ? C26 C27 1.390(4) . ? C27 C28 1.386(5) . ? C27 C30 1.480(5) . ? C28 H28 0.9500 . ? C28 C29 1.382(5) . ? C29 H29 0.9500 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5B H5BA 0.9900 . ? C5B H5BB 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 C1 112.0(2) . . ? O3 S1 C24 108.2(2) . . ? O4 S1 O3 119.4(3) . . ? O4 S1 C1 107.5(3) . . ? O4 S1 C24 109.4(2) . . ? C1 S1 C24 98.17(19) . . ? O3B S1B O4B 120.4(9) . . ? O3B S1B C1 100.9(7) . . ? O3B S1B C24 111.2(6) . . ? O4B S1B C1 107.9(8) . . ? O4B S1B C24 101.0(8) . . ? C24 S1B C1 116.2(5) . . ? C6 O1 C3 118.6(3) . . ? S1 C1 H1A 111.2 . . ? S1B C1 H1B 99.9 . . ? C2 C1 S1 110.2(2) . . ? C2 C1 S1B 121.9(3) . . ? C2 C1 H1A 111.2 . . ? C2 C1 H1B 99.9 . . ? C2 C1 C5 103.9(3) . . ? C2 C1 C5B 107.1(6) . . ? C5 C1 S1 108.8(3) . . ? C5 C1 H1A 111.2 . . ? C5B C1 S1B 122.3(6) . . ? C5B C1 H1B 99.9 . . ? C1 C2 H2A 110.7 . . ? C1 C2 H2B 110.7 . . ? H2A C2 H2B 108.8 . . ? C3 C2 C1 105.2(3) . . ? C3 C2 H2A 110.7 . . ? C3 C2 H2B 110.7 . . ? O1 C3 C2 110.9(3) . . ? O1 C3 H3 110.9 . . ? O1 C3 C4 107.7(3) . . ? C2 C3 H3 110.9 . . ? C4 C3 C2 105.2(3) . . ? C4 C3 H3 110.9 . . ? C3 C4 H4AA 110.7 . . ? C3 C4 H4AB 110.7 . . ? C3 C4 H4BC 109.3 . . ? C3 C4 H4BD 109.3 . . ? C3 C4 C5B 111.7(6) . . ? H4AA C4 H4AB 108.8 . . ? H4BC C4 H4BD 107.9 . . ? C5 C4 C3 105.2(3) . . ? C5 C4 H4AA 110.7 . . ? C5 C4 H4AB 110.7 . . ? C5B C4 H4BC 109.3 . . ? C5B C4 H4BD 109.3 . . ? C7 C6 O1 124.5(3) . . ? C7 C6 C11 120.2(3) . . ? C11 C6 O1 115.2(3) . . ? C6 C7 H7 120.5 . . ? C6 C7 C8 118.9(3) . . ? C8 C7 H7 120.5 . . ? C7 C8 H8 118.7 . . ? C9 C8 C7 122.5(3) . . ? C9 C8 H8 118.7 . . ? C8 C9 C10 117.6(3) . . ? C8 C9 C12 121.3(3) . . ? C10 C9 C12 120.9(2) . . ? C9 C10 C15 122.1(2) . . ? C11 C10 C9 119.8(3) . . ? C11 C10 C15 118.1(2) . . ? C6 C11 C10 120.9(3) . . ? C6 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C9 C12 H12 106.1 . . ? C9 C12 C13 111.7(2) . . ? C9 C12 C16 114.3(2) . . ? C13 C12 H12 106.1 . . ? C16 C12 H12 106.1 . . ? C16 C12 C13 111.8(2) . . ? C12 C13 H13 108.4 . . ? C14 C13 C12 110.0(2) . . ? C14 C13 H13 108.4 . . ? C14 C13 C19 114.1(2) . . ? C19 C13 C12 107.5(2) . . ? C19 C13 H13 108.4 . . ? C13 C14 H14A 109.7 . . ? C13 C14 H14B 109.7 . . ? C13 C14 C15 109.7(2) . . ? H14A C14 H14B 108.2 . . ? C15 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? C10 C15 C14 112.8(2) . . ? C10 C15 H15A 109.0 . . ? C10 C15 H15B 109.0 . . ? C14 C15 H15A 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C12 C16 H16A 109.0 . . ? C12 C16 H16B 109.0 . . ? C12 C16 C17 113.0(2) . . ? H16A C16 H16B 107.8 . . ? C17 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? C16 C17 H17A 109.7 . . ? C16 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? C18 C17 C16 110.0(2) . . ? C18 C17 H17A 109.7 . . ? C18 C17 H17B 109.7 . . ? C17 C18 C19 109.2(2) . . ? C17 C18 C23 110.9(2) . . ? C19 C18 C23 114.1(2) . . ? C22 C18 C17 117.7(2) . . ? C22 C18 C19 100.5(2) . . ? C22 C18 C23 104.1(2) . . ? C13 C19 C18 112.2(2) . . ? C13 C19 H19 106.4 . . ? C13 C19 C20 119.9(2) . . ? C18 C19 H19 106.4 . . ? C20 C19 C18 104.7(2) . . ? C20 C19 H19 106.4 . . ? C19 C20 H20A 111.4 . . ? C19 C20 H20B 111.4 . . ? C19 C20 C21 102.1(2) . . ? H20A C20 H20B 109.2 . . ? C21 C20 H20A 111.4 . . ? C21 C20 H20B 111.4 . . ? C20 C21 H21A 110.5 . . ? C20 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? C22 C21 C20 106.3(2) . . ? C22 C21 H21A 110.5 . . ? C22 C21 H21B 110.5 . . ? O2 C22 C18 126.4(3) . . ? O2 C22 C21 125.4(3) . . ? C18 C22 C21 108.3(2) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 S1 121.1(3) . . ? C25 C24 S1B 109.7(3) . . ? C25 C24 C29 121.3(3) . . ? C29 C24 S1 117.6(3) . . ? C29 C24 S1B 128.3(4) . . ? C24 C25 H25 120.2 . . ? C24 C25 C26 119.6(3) . . ? C26 C25 H25 120.2 . . ? C25 C26 H26 120.2 . . ? C25 C26 C27 119.7(3) . . ? C27 C26 H26 120.2 . . ? C26 C27 C30 119.6(3) . . ? C28 C27 C26 120.0(3) . . ? C28 C27 C30 120.4(3) . . ? C27 C28 H28 120.0 . . ? C29 C28 C27 120.0(3) . . ? C29 C28 H28 120.0 . . ? C24 C29 C28 119.3(3) . . ? C24 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? F1 C30 F2 102.2(5) . . ? F1 C30 C27 113.7(4) . . ? F2 C30 C27 109.4(4) . . ? F3 C30 F1 112.2(6) . . ? F3 C30 F2 102.9(5) . . ? F3 C30 C27 114.9(5) . . ? F1B C30 C27 106.6(4) . . ? F2B C30 F1B 101.2(7) . . ? F2B C30 F3B 114.7(10) . . ? F2B C30 C27 116.7(5) . . ? F3B C30 F1B 95.6(9) . . ? F3B C30 C27 117.6(8) . . ? C1 C5 H5A 111.0 . . ? C1 C5 H5B 111.0 . . ? C4 C5 C1 103.8(3) . . ? C4 C5 H5A 111.0 . . ? C4 C5 H5B 111.0 . . ? H5A C5 H5B 109.0 . . ? C1 C5B H5BA 112.0 . . ? C1 C5B H5BB 112.0 . . ? C4 C5B C1 98.6(8) . . ? C4 C5B H5BA 112.0 . . ? C4 C5B H5BB 112.0 . . ? H5BA C5B H5BB 109.7 . . ? _shelx_res_file ; baran599.res created by SHELXL-2014/7 TITL Baran599 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.168, Rweak 0.034, Alpha 0.012, Orientation as input REM Flack x = 0.141 ( 0.010 ) from Parsons' quotients REM Formula found by SHELXT: C34 O4 S CELL 1.54178 6.6458 8.1522 48.228 90 90 90 ZERR 4 0.0002 0.0003 0.0015 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H F O S UNIT 120 132 12 16 4 EADP O4B O4 EADP S1 S1B EADP O3 O3B EADP C5B C5 L.S. 10 PLAN 20 SIZE 0.177 0.153 0.116 TEMP -173.15 BOND $H ACTA 136 fmap 2 REM REM REM WGHT 0.036200 0.987400 FVAR 0.60811 0.64159 0.75050 PART 1 S1 5 0.301840 0.652454 0.430586 31.00000 0.04243 0.04203 = 0.02666 0.00268 0.00133 0.00769 PART 0 PART 2 S1B 5 0.236769 0.662639 0.427706 -31.00000 0.04243 0.04203 = 0.02666 0.00268 0.00133 0.00769 PART 0 PART 1 F1 3 -0.498774 1.081774 0.472531 21.00000 0.04567 0.08577 = 0.18195 -0.00661 -0.01637 -0.00362 F2 3 -0.296062 1.277588 0.467299 21.00000 0.09678 0.04368 = 0.07037 0.01093 0.01727 0.02067 F3 3 -0.293434 1.150606 0.505049 21.00000 0.10430 0.11613 = 0.03775 0.01518 0.01397 0.06634 PART 0 PART 2 F1B 3 -0.451693 1.017763 0.494763 -21.00000 0.06695 0.05770 = 0.06214 0.00576 0.01733 -0.00469 F2B 3 -0.431284 1.188964 0.462553 -21.00000 0.07381 0.14547 = 0.06520 0.04887 0.01036 0.05281 F3B 3 -0.261537 1.211858 0.499663 -21.00000 0.06913 0.07967 = 0.18806 -0.09405 -0.03120 0.01682 PART 0 O1 4 0.240514 0.297951 0.369571 11.00000 0.03147 0.06749 = 0.02559 -0.00930 -0.00022 0.01324 O2 4 1.516910 -0.406451 0.293236 11.00000 0.03738 0.03516 = 0.04684 0.00338 0.00066 0.01361 PART 1 O3 4 0.365398 0.706451 0.403532 31.00000 0.05795 0.05554 = 0.03460 0.00750 0.00969 0.00281 O4 4 0.450724 0.617564 0.451426 31.00000 0.04562 0.05223 = 0.03467 -0.00003 -0.00661 0.00680 PART 0 PART 2 O3B 4 0.235595 0.694010 0.398641 -31.00000 0.05795 0.05554 = 0.03460 0.00750 0.00969 0.00281 O4B 4 0.428821 0.656414 0.443147 -31.00000 0.04562 0.05223 = 0.03467 -0.00003 -0.00661 0.00680 PART 0 C1 1 0.134269 0.476434 0.428674 11.00000 0.04410 0.04429 = 0.04354 -0.01062 -0.00554 0.00563 PART 1 AFIX 13 H1A 2 0.062889 0.458549 0.446675 31.00000 -1.20000 AFIX 13 PART 0 PART 2 H1B 2 0.129632 0.458845 0.449184 -31.00000 -1.20000 AFIX 0 PART 0 C2 1 0.251760 0.322854 0.419909 11.00000 0.04889 0.04362 = 0.02635 -0.00407 -0.00040 0.00753 AFIX 23 H2A 2 0.392118 0.351367 0.415004 11.00000 -1.20000 H2B 2 0.253719 0.240942 0.435062 11.00000 -1.20000 AFIX 0 C3 1 0.139046 0.255717 0.394581 11.00000 0.03140 0.07045 = 0.03445 -0.01679 0.00738 -0.00062 AFIX 13 H3 2 0.120574 0.134286 0.396041 11.00000 -1.20000 AFIX 0 C4 1 -0.061719 0.342912 0.394590 11.00000 0.03048 0.11157 = 0.04593 -0.03274 0.00344 0.01105 PART 1 AFIX 23 H4AA 2 -0.119430 0.345973 0.375673 31.00000 -1.20000 H4AB 2 -0.157930 0.286942 0.407084 31.00000 -1.20000 AFIX 23 PART 0 PART 2 H4BC 2 -0.171053 0.260935 0.393051 -31.00000 -1.20000 H4BD 2 -0.069664 0.416137 0.378251 -31.00000 -1.20000 AFIX 0 PART 0 C6 1 0.411093 0.210738 0.362322 11.00000 0.02623 0.05239 = 0.02189 -0.00960 -0.00233 0.00721 C7 1 0.467799 0.063650 0.374117 11.00000 0.03221 0.05599 = 0.02034 0.00034 0.00270 -0.00098 AFIX 43 H7 2 0.392184 0.017698 0.388919 11.00000 -1.20000 AFIX 0 C8 1 0.637647 -0.016361 0.363975 11.00000 0.03257 0.04109 = 0.02359 0.00381 -0.00183 0.00039 AFIX 43 H8 2 0.675505 -0.118175 0.372013 11.00000 -1.20000 AFIX 0 C9 1 0.753809 0.046889 0.342572 11.00000 0.02731 0.03164 = 0.02135 -0.00167 -0.00220 -0.00096 C10 1 0.693628 0.197657 0.330879 11.00000 0.02663 0.02929 = 0.02327 -0.00344 -0.00303 0.00069 C11 1 0.521720 0.276722 0.340812 11.00000 0.02956 0.03411 = 0.02791 -0.00685 -0.00402 0.00400 AFIX 43 H11 2 0.480332 0.377289 0.332657 11.00000 -1.20000 AFIX 0 C12 1 0.949686 -0.035828 0.333608 11.00000 0.02661 0.02596 = 0.02077 0.00123 -0.00199 0.00079 AFIX 13 H12 2 1.054042 -0.000721 0.347317 11.00000 -1.20000 AFIX 0 C13 1 1.022102 0.027270 0.305074 11.00000 0.02064 0.02501 = 0.02190 0.00079 -0.00061 0.00018 AFIX 13 H13 2 0.925169 -0.011370 0.290622 11.00000 -1.20000 AFIX 0 C14 1 1.024049 0.213523 0.304831 11.00000 0.02480 0.02529 = 0.02611 0.00022 0.00019 0.00095 AFIX 23 H14A 2 1.084508 0.253302 0.287316 11.00000 -1.20000 H14B 2 1.106661 0.254664 0.320433 11.00000 -1.20000 AFIX 0 C15 1 0.809372 0.278227 0.307481 11.00000 0.02505 0.02689 = 0.03009 0.00075 -0.00004 0.00318 AFIX 23 H15A 2 0.813850 0.398104 0.310705 11.00000 -1.20000 H15B 2 0.737192 0.259022 0.289820 11.00000 -1.20000 AFIX 0 C16 1 0.944658 -0.224224 0.334747 11.00000 0.02967 0.02996 = 0.02629 0.00475 0.00113 0.00255 AFIX 23 H16A 2 0.838021 -0.264547 0.322138 11.00000 -1.20000 H16B 2 0.909406 -0.259114 0.353800 11.00000 -1.20000 AFIX 0 C17 1 1.146920 -0.303587 0.326477 11.00000 0.03138 0.02506 = 0.02962 0.00334 -0.00208 0.00267 AFIX 23 H17A 2 1.250229 -0.277671 0.340602 11.00000 -1.20000 H17B 2 1.131472 -0.424272 0.325647 11.00000 -1.20000 AFIX 0 C18 1 1.214307 -0.239173 0.298275 11.00000 0.02786 0.02542 = 0.02628 -0.00095 -0.00165 0.00302 C19 1 1.225880 -0.050694 0.299336 11.00000 0.02357 0.02428 = 0.02371 -0.00028 -0.00350 -0.00025 AFIX 13 H19 2 1.313534 -0.022840 0.315519 11.00000 -1.20000 AFIX 0 C20 1 1.344161 -0.002596 0.273350 11.00000 0.02835 0.02903 = 0.03041 0.00090 0.00479 0.00076 AFIX 23 H20A 2 1.403123 0.108395 0.275188 11.00000 -1.20000 H20B 2 1.258199 -0.006297 0.256597 11.00000 -1.20000 AFIX 0 C21 1 1.508024 -0.134812 0.272400 11.00000 0.02763 0.03228 = 0.03955 -0.00234 0.00408 0.00293 AFIX 23 H21A 2 1.536041 -0.167279 0.253000 11.00000 -1.20000 H21B 2 1.634054 -0.093551 0.280833 11.00000 -1.20000 AFIX 0 C22 1 1.426937 -0.280165 0.288823 11.00000 0.02850 0.03258 = 0.02829 -0.00479 -0.00412 0.00288 C23 1 1.078854 -0.306655 0.274900 11.00000 0.02753 0.03127 = 0.02998 -0.00391 -0.00209 -0.00022 AFIX 137 H23A 2 0.937780 -0.282171 0.279127 11.00000 -1.50000 H23B 2 1.096878 -0.425661 0.273457 11.00000 -1.50000 H23C 2 1.115929 -0.254966 0.257280 11.00000 -1.50000 AFIX 0 C24 1 0.120263 0.802854 0.444254 11.00000 0.07146 0.03483 = 0.03015 0.00226 0.00208 -0.00025 C25 1 -0.021688 0.873372 0.427375 11.00000 0.12198 0.04378 = 0.02956 0.00046 -0.01769 0.01656 AFIX 43 H25 2 -0.021862 0.851145 0.408039 11.00000 -1.20000 AFIX 0 C26 1 -0.164872 0.977284 0.438727 11.00000 0.08935 0.04062 = 0.04324 0.00270 -0.02839 0.01011 AFIX 43 H26 2 -0.265910 1.024335 0.427285 11.00000 -1.20000 AFIX 0 C27 1 -0.159864 1.012275 0.466926 11.00000 0.04876 0.03163 = 0.03946 0.00496 -0.00732 -0.00719 C28 1 -0.011053 0.944879 0.483514 11.00000 0.04589 0.04499 = 0.02883 -0.00127 -0.00389 -0.00480 AFIX 43 H28 2 -0.004611 0.972230 0.502642 11.00000 -1.20000 AFIX 0 C29 1 0.127981 0.837907 0.472250 11.00000 0.04211 0.03665 = 0.03223 -0.00107 -0.00423 -0.00516 AFIX 43 H29 2 0.227894 0.788957 0.483651 11.00000 -1.20000 AFIX 0 C30 1 -0.313859 1.122159 0.479017 11.00000 0.04960 0.05597 = 0.05598 0.00759 -0.00992 0.00237 PART 1 C5 1 -0.019962 0.504029 0.404214 31.00000 0.04187 0.05032 = 0.02925 -0.00351 0.00205 0.00839 AFIX 23 H5A 2 -0.143895 0.558313 0.410961 31.00000 -1.20000 H5B 2 0.040311 0.571783 0.389340 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C5B 1 -0.092186 0.445346 0.421320 -31.00000 0.04187 0.05032 = 0.02925 -0.00351 0.00205 0.00839 AFIX 23 H5BA 2 -0.162412 0.382335 0.435958 -31.00000 -1.20000 H5BB 2 -0.165511 0.548817 0.417662 -31.00000 -1.20000 AFIX 0 HKLF 4 REM Baran599 in P2(1)2(1)2(1) REM R1 = 0.0391 for 4450 Fo > 4sig(Fo) and 0.0414 for all 4723 data REM 385 parameters refined using 0 restraints END WGHT 0.0362 0.9875 REM Highest difference peak 0.184, deepest hole -0.285, 1-sigma level 0.038 Q1 1 1.2131 -0.1500 0.2989 11.00000 0.05 0.18 Q2 1 1.1433 -0.2672 0.2880 11.00000 0.05 0.18 Q3 1 -0.1476 0.3021 0.3799 11.00000 0.05 0.18 Q4 1 -0.1498 0.8509 0.4340 11.00000 0.05 0.18 Q5 1 1.2914 -0.0247 0.2871 11.00000 0.05 0.17 Q6 1 1.1681 -0.2708 0.3106 11.00000 0.05 0.16 Q7 1 0.0087 0.5332 0.3852 11.00000 0.05 0.16 Q8 1 1.6048 -0.0803 0.2912 11.00000 0.05 0.15 Q9 1 0.0053 0.7913 0.4426 11.00000 0.05 0.15 Q10 1 -0.0380 0.4411 0.3868 11.00000 0.05 0.14 Q11 1 0.9961 0.0053 0.3196 11.00000 0.05 0.14 Q12 1 0.2017 0.6821 0.4138 11.00000 0.05 0.14 Q13 1 0.1620 0.7339 0.4421 11.00000 0.05 0.13 Q14 1 0.7473 0.2398 0.3212 11.00000 0.05 0.13 Q15 1 0.4884 0.8167 0.4167 11.00000 0.05 0.13 Q16 1 0.6340 0.6581 0.3876 11.00000 0.05 0.13 Q17 1 -0.2740 0.9624 0.4440 11.00000 0.05 0.13 Q18 1 1.5760 -0.1352 0.2601 11.00000 0.05 0.13 Q19 1 -0.3446 1.2379 0.4844 11.00000 0.05 0.12 Q20 1 -0.2441 0.9495 0.4520 11.00000 0.05 0.12 ; _shelx_res_checksum 82708 _shelx_hkl_file ; 1 0 0 0.70 1.00 2 0 0 166.88 10.70 3 0 0 -0.20 1.70 3 0 0 1.10 2.30 4 0 0 1698.13 90.69 4 0 0 1606.24 90.79 5 0 0 -0.40 2.60 5 0 0 2.50 2.90 6 0 0 51.09 5.80 6 0 0 61.59 6.10 7 0 0 1.50 2.80 8 0 0 14.00 2.40 1 -1 0 5549.04 291.97 1 1 0 5479.65 292.47 1 -1 0 5217.38 292.47 2 -1 0 355.26 19.90 2 1 0 376.56 20.90 2 -1 0 349.47 20.90 2 -1 0 354.36 20.10 3 -1 0 34.50 4.50 3 -1 0 42.40 3.80 3 1 0 39.00 4.90 4 -1 0 26.50 3.80 4 -1 0 32.00 3.90 4 -1 0 21.50 4.20 4 1 0 23.60 3.60 4 1 0 15.60 3.70 5 -1 0 4.00 2.80 5 1 0 1.70 2.90 5 -1 0 8.90 3.10 5 1 0 3.40 2.30 6 1 0 153.78 10.40 6 1 0 153.68 10.30 6 -1 0 160.58 10.70 6 -1 0 150.78 10.60 6 1 0 156.78 10.70 -6 -1 0 119.09 13.00 7 1 0 4.30 2.50 7 -1 0 7.70 2.80 7 1 0 5.70 2.60 7 -1 0 10.60 3.30 -7 -1 0 4.80 2.90 0 -2 0 3661.43 201.88 0 2 0 3812.02 201.88 1 -2 0 7083.09 380.26 1 -2 0 6880.91 380.56 1 -2 0 7071.69 380.86 -1 2 0 7189.68 380.26 2 -2 0 2108.29 114.89 2 2 0 2103.09 114.89 2 -2 0 2102.99 114.19 3 -2 0 66.29 6.10 3 2 0 58.49 5.90 3 -2 0 62.19 4.90 4 -2 0 12.70 2.80 -4 -2 0 12.60 3.20 4 2 0 7.70 3.10 4 -2 0 10.70 2.90 5 -2 0 196.58 12.20 5 2 0 184.58 13.60 5 2 0 186.48 12.40 5 -2 0 207.98 13.50 6 2 0 214.28 14.00 6 -2 0 248.18 14.90 6 2 0 221.18 14.20 6 -2 0 209.68 14.20 7 -2 0 71.69 6.90 7 2 0 88.29 6.40 7 -2 0 98.39 7.50 0 -3 0 0.40 1.30 1 -3 0 1465.15 84.29 1 -3 0 1553.64 82.19 1 -3 0 1503.15 82.19 -1 -3 0 1523.25 82.39 2 -3 0 63.09 4.50 2 -3 0 60.89 4.70 2 -3 0 64.09 5.40 -2 -3 0 47.50 4.10 -3 -3 0 825.32 45.10 -3 -3 0 784.92 46.10 3 -3 0 863.71 45.70 3 -3 0 805.52 46.70 -4 -3 0 91.09 7.40 4 -3 0 84.99 6.80 5 -3 0 184.18 11.40 5 3 0 163.98 11.10 -5 -3 0 165.68 12.50 6 3 0 5.10 2.20 -6 -3 0 7.50 3.50 6 -3 0 7.00 2.60 6 -3 0 12.70 3.70 6 3 0 9.30 2.90 7 -3 0 4.60 2.70 7 3 0 9.60 2.10 -7 -3 0 7.80 2.40 0 -4 0 3221.88 174.38 0 -4 0 3216.18 174.08 1 -4 0 143.59 9.30 1 -4 0 153.08 9.40 -1 -4 0 155.18 9.20 -1 -4 0 152.98 9.40 -2 -4 0 105.09 6.90 -2 -4 0 100.19 7.80 2 -4 0 108.89 7.20 2 -4 0 112.69 7.30 -3 -4 0 1273.67 67.59 3 -4 0 1210.88 67.99 -3 -4 0 1212.58 68.59 4 4 0 151.78 10.10 -4 -4 0 139.39 10.80 4 -4 0 169.38 10.70 -5 -4 0 62.29 6.80 -5 -4 0 48.50 6.10 5 4 0 47.20 5.10 5 4 0 41.10 5.50 -6 -4 0 0.70 2.40 -7 -4 0 45.80 4.30 0 -5 0 1.40 1.70 1 -5 0 424.76 23.60 -1 -5 0 403.46 23.50 -1 -5 0 396.66 23.10 1 -5 0 412.06 23.50 -2 -5 0 38.00 4.30 2 -5 0 40.20 4.30 2 -5 0 39.60 4.10 -2 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91.09 6.40 -2 -4 28 70.29 6.00 2 -4 -28 68.89 6.70 2 4 28 67.99 6.00 2 -4 -28 68.19 6.60 -3 -4 -28 78.89 8.30 -3 -4 -28 94.09 7.30 -3 -4 28 101.39 7.70 3 -4 -28 109.19 11.50 3 -4 -28 89.19 7.80 3 4 28 99.29 7.40 -4 -4 -28 228.58 16.80 -4 -4 -28 254.77 15.10 -4 -4 -28 262.17 17.30 4 4 28 266.17 16.80 4 -4 -28 253.37 16.30 -4 -4 28 267.37 17.20 4 -4 -28 282.67 16.50 -5 -4 -28 39.10 3.40 -5 -4 -28 33.40 4.80 5 -4 -28 43.90 4.60 -6 -4 -28 1.80 1.90 -6 -4 -28 0.90 1.00 6 -4 -28 0.90 1.50 6 4 28 0.60 2.30 0 -5 -28 48.20 5.30 0 -5 28 47.20 5.10 0 -5 28 42.20 5.00 -1 5 28 124.49 10.30 1 -5 28 132.09 9.70 1 -5 28 129.79 8.90 -1 -5 -28 126.39 9.10 -1 -5 28 121.59 8.80 -1 -5 28 125.29 9.90 -1 -5 28 110.49 9.30 1 -5 -28 129.59 9.10 1 -5 -28 137.29 9.30 -2 -5 -28 4.80 2.80 2 -5 28 5.50 3.30 -2 -5 -28 5.10 2.20 -2 -5 -28 1.70 2.80 2 -5 28 4.00 3.40 2 -5 28 5.70 2.60 -2 -5 28 4.10 2.40 -2 -5 28 4.90 3.10 2 -5 -28 8.80 3.50 -2 -5 28 7.60 2.90 -2 -5 28 4.80 3.20 2 -5 -28 3.80 2.90 -3 -5 -28 23.30 3.00 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-4 -6 -28 17.40 3.40 -4 -6 -28 20.00 3.20 -4 -6 28 26.10 3.10 4 -6 -28 24.20 3.80 4 -6 -28 24.00 3.00 -5 -6 -28 38.40 2.90 -5 -6 -28 38.10 3.80 5 -6 -28 36.50 3.40 5 6 28 47.00 5.30 0 -7 -28 10.00 2.90 0 -7 28 7.30 2.90 0 -7 -28 6.80 2.70 0 -7 -28 9.10 2.30 0 -7 28 6.40 3.00 -1 -7 -28 31.00 4.70 1 -7 28 34.50 5.20 1 -7 28 29.60 4.70 -1 -7 -28 35.80 3.90 -1 -7 -28 34.00 4.40 1 -7 -28 41.10 4.90 -1 -7 28 39.20 4.00 -1 -7 28 42.20 5.00 -1 -7 28 38.00 4.90 1 -7 -28 38.30 4.00 -2 -7 -28 9.50 2.20 -2 -7 -28 7.90 2.50 -2 -7 -28 11.00 2.90 -2 -7 28 9.60 3.10 -2 -7 28 7.50 2.70 2 -7 -28 9.30 2.30 2 -7 -28 10.60 2.90 -2 -7 28 10.00 2.40 -3 -7 -28 18.50 3.10 -3 -7 -28 21.60 2.70 3 7 -28 16.80 3.20 3 -7 -28 19.90 3.30 3 -7 -28 21.40 2.90 -3 -7 28 23.50 3.40 -3 -7 28 20.10 3.10 -3 -7 28 19.00 2.70 -4 -7 -28 9.50 1.80 -4 -7 -28 9.80 1.50 4 -7 -28 6.90 1.80 4 -7 -28 8.80 1.70 0 -8 28 17.60 3.10 0 -8 -28 20.90 3.30 0 -8 28 20.10 3.10 0 -8 -28 20.10 2.40 -1 -8 -28 14.00 2.40 -1 -8 -28 15.70 2.20 1 -8 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260.47 15.50 -1 -1 29 271.17 15.80 1 1 29 257.17 14.70 -2 1 29 136.99 10.10 2 1 -29 126.79 8.90 2 -1 29 133.29 10.10 2 -1 29 126.19 8.40 2 -1 29 130.09 9.60 2 1 29 123.29 8.30 2 1 29 123.09 9.90 2 -1 -29 132.89 9.00 2 1 29 125.19 9.60 -2 -1 29 138.39 10.00 -3 1 29 59.99 6.80 3 1 -29 51.79 5.80 3 -1 29 64.99 5.50 3 1 -29 56.69 5.80 3 -1 29 65.79 7.30 3 -1 -29 68.79 6.30 -3 -1 29 66.99 7.30 3 -1 -29 73.69 6.10 3 1 29 64.99 7.00 3 1 29 67.99 5.60 4 -1 29 171.98 12.50 4 -1 29 167.58 11.30 -4 1 29 174.08 12.70 4 1 -29 136.29 10.80 4 1 -29 145.99 11.00 4 -1 29 170.98 10.60 4 1 -29 152.78 11.00 -4 -1 29 153.78 11.00 4 1 29 150.28 12.10 4 -1 -29 168.68 11.30 4 -1 -29 164.58 11.10 4 -1 -29 180.88 11.60 -4 -1 29 157.08 12.50 4 1 29 171.38 10.70 5 -1 29 168.98 12.60 5 -1 29 169.18 11.90 -5 1 29 169.48 12.70 5 1 -29 175.48 11.70 5 1 -29 168.18 11.60 5 -1 -29 154.28 11.60 5 1 29 163.78 12.10 5 1 29 158.18 12.30 -5 -1 29 158.48 12.60 5 -1 -29 170.98 11.50 6 1 -29 43.80 4.70 6 1 -29 46.40 4.70 6 -1 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3.10 -6 -2 29 5.70 2.40 6 -2 -29 9.10 3.00 6 -2 -29 12.30 2.60 0 -3 29 136.29 8.90 -1 3 29 24.10 4.70 1 -3 29 21.70 3.40 1 -3 -29 26.50 3.70 -1 -3 29 25.50 3.30 1 -3 -29 25.60 5.40 -2 3 29 154.48 11.40 -2 -3 -29 140.69 9.80 2 -3 29 167.78 10.00 2 -3 -29 144.69 10.20 2 -3 -29 147.69 10.40 2 3 29 151.68 9.70 3 3 -29 53.89 5.50 3 -3 29 56.39 4.90 -3 -3 -29 54.69 5.40 -3 3 29 54.89 6.80 3 -3 -29 41.20 5.20 3 -3 -29 49.70 5.70 3 3 29 42.80 4.70 -3 -3 29 46.40 5.50 -3 -3 29 45.00 6.30 -4 -3 -29 55.49 4.90 4 -3 29 57.59 6.60 -4 -3 -29 63.49 6.30 4 3 -29 65.39 6.10 4 -3 -29 61.59 6.30 -4 -3 29 57.99 5.80 4 -3 -29 56.59 6.00 4 3 29 49.60 6.40 -4 -3 29 57.69 7.10 4 -3 -29 57.89 7.40 4 3 29 54.19 6.60 -5 -3 -29 30.10 5.50 -5 -3 -29 41.60 3.80 5 3 29 38.60 5.50 5 -3 -29 44.30 5.40 5 -3 -29 40.80 4.80 -6 -3 -29 16.00 3.00 -6 -3 -29 17.50 2.20 6 3 29 27.30 4.30 6 -3 -29 21.50 2.90 0 -4 -29 45.20 4.80 0 -4 29 37.10 4.40 -1 -4 -29 241.78 16.40 1 -4 29 265.47 16.20 -1 4 29 264.87 17.60 1 -4 -29 294.27 16.70 -1 -4 29 280.67 16.30 1 -4 -29 279.17 16.60 -2 4 29 81.59 8.40 2 -4 29 93.69 7.20 -2 -4 -29 96.99 7.40 2 -4 -29 95.19 7.60 -2 -4 29 105.29 7.90 -2 -4 29 89.99 7.00 2 4 29 97.29 7.10 2 -4 -29 99.19 7.80 -3 -4 -29 63.99 6.60 -3 -4 -29 53.39 4.70 3 -4 29 66.69 7.00 -3 -4 -29 65.29 5.80 3 4 29 54.29 5.50 -3 -4 29 58.79 6.10 3 -4 -29 58.99 6.80 -3 -4 29 63.59 5.90 3 -4 -29 66.59 6.40 -4 -4 -29 313.37 18.00 -4 -4 -29 310.97 19.00 -4 -4 29 287.77 19.70 4 -4 -29 325.87 19.30 4 4 29 318.37 19.40 4 -4 -29 310.27 19.10 -5 -4 -29 94.39 9.00 -5 -4 -29 80.79 6.00 5 -4 -29 82.99 6.90 5 4 29 102.89 8.40 -6 -4 -29 1.60 1.70 -6 -4 -29 1.60 1.00 6 4 29 1.80 2.20 6 -4 -29 2.30 1.40 0 -5 29 2.20 2.60 0 -5 29 1.20 2.70 0 -5 29 0.80 2.90 0 -5 -29 2.80 2.70 -1 5 29 79.89 8.00 1 -5 29 80.59 6.70 1 -5 29 78.39 7.30 -1 -5 -29 78.29 6.70 -1 -5 29 84.09 6.70 1 -5 -29 75.89 6.80 -1 -5 29 86.49 7.10 1 -5 -29 83.69 6.80 -1 -5 29 88.99 7.70 2 -5 29 180.38 12.60 -2 -5 -29 192.58 12.50 -2 -5 -29 165.88 10.70 2 -5 29 167.58 11.10 -2 -5 -29 175.88 11.50 2 -5 29 180.78 12.00 -2 -5 29 174.08 11.90 -2 -5 29 154.78 11.30 -2 -5 29 167.88 11.80 2 -5 -29 165.88 12.00 -2 -5 29 180.28 11.30 2 -5 -29 177.08 11.90 -3 -5 -29 113.89 7.80 3 -5 29 115.79 9.60 -3 -5 -29 120.99 9.30 -3 -5 -29 114.49 8.50 3 -5 -29 116.19 9.10 -3 -5 29 121.09 8.80 3 -5 -29 117.09 9.10 -3 -5 29 121.69 8.60 -4 -5 -29 30.80 5.40 -4 -5 -29 46.00 3.60 -4 -5 -29 32.10 5.40 4 -5 -29 43.00 4.90 -5 -5 -29 10.80 1.70 -5 -5 -29 10.90 3.20 5 5 29 13.00 3.60 5 -5 -29 8.50 2.30 0 -6 -29 31.90 3.90 0 -6 -29 36.80 4.80 0 -6 29 32.90 5.20 0 -6 29 29.80 4.70 0 6 29 27.10 5.20 0 -6 -29 32.60 4.80 -1 -6 -29 28.20 4.10 -1 -6 -29 17.60 3.50 -1 -6 -29 16.10 2.70 -1 -6 -29 13.50 3.70 1 -6 29 24.40 4.40 1 -6 29 19.20 4.20 1 -6 -29 16.80 2.90 -1 -6 29 23.40 4.10 1 -6 -29 21.20 3.90 -1 -6 29 19.70 4.00 -1 -6 29 19.50 3.20 1 -6 -29 18.50 3.70 -2 -6 -29 39.10 5.60 2 -6 29 44.20 5.60 2 -6 29 41.10 5.40 -2 -6 -29 41.80 3.90 -2 -6 -29 42.00 5.20 -2 -6 29 33.70 4.80 -2 -6 29 28.30 4.00 2 -6 -29 37.80 5.30 -2 -6 29 38.30 5.00 2 -6 -29 38.00 4.10 2 -6 -29 43.80 5.60 -3 -6 -29 55.39 6.90 -3 -6 -29 86.99 7.20 -3 -6 -29 75.49 5.30 3 6 -29 64.69 6.40 -3 -6 29 74.69 5.80 3 -6 -29 67.29 5.40 3 -6 -29 70.09 6.60 -3 -6 29 64.09 6.00 -4 -6 -29 5.80 1.60 -4 -6 -29 5.50 2.70 -4 -6 29 4.50 2.00 4 -6 -29 6.00 2.40 0 -7 -29 3.00 2.60 0 -7 -29 3.30 2.00 0 -7 29 1.40 2.60 0 -7 -29 2.70 2.40 0 -7 29 1.60 2.70 1 -7 29 17.80 3.60 -1 -7 -29 23.80 3.50 1 -7 29 24.20 3.70 -1 -7 -29 18.50 2.70 -1 -7 -29 26.00 3.70 -1 -7 29 22.50 3.00 -1 -7 29 21.00 3.60 1 -7 -29 21.00 3.50 -1 -7 29 21.10 3.70 1 -7 -29 17.50 2.60 -2 -7 -29 32.70 4.10 -2 -7 -29 26.40 4.00 -2 -7 -29 30.70 3.30 -2 -7 29 38.80 3.80 -2 -7 29 26.70 4.20 2 -7 -29 29.60 3.40 -2 -7 29 29.50 4.20 2 -7 -29 30.90 4.30 -3 -7 -29 22.60 3.10 -3 -7 -29 23.20 2.70 3 7 -29 23.30 3.50 3 -7 -29 22.90 3.60 3 -7 -29 24.60 2.90 -3 -7 29 21.70 3.50 -3 -7 29 23.20 3.20 -3 -7 29 20.70 2.80 0 -8 -29 0.70 1.50 0 -8 -29 0.20 1.80 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73.39 0 -1 30 1353.46 73.99 0 -1 30 1371.46 74.39 0 1 30 1296.37 74.29 1 1 -30 284.67 17.40 1 -1 30 273.27 17.00 1 -1 30 300.17 18.00 1 -1 30 307.47 18.50 -1 1 30 281.57 18.20 1 -1 -30 292.07 17.40 -1 -1 30 293.77 18.00 1 1 30 307.17 17.90 1 1 30 307.87 17.10 2 1 -30 105.49 7.70 -2 1 30 108.19 8.70 2 -1 30 118.09 8.80 2 -1 30 109.79 7.40 2 1 30 104.39 8.60 2 -1 -30 99.79 7.80 2 1 30 105.49 7.20 -2 -1 30 100.09 8.60 2 1 30 101.69 9.30 -3 1 30 13.40 4.40 3 1 -30 8.80 2.80 3 -1 30 13.10 2.80 3 1 -30 12.00 3.00 3 -1 30 19.40 4.50 3 -1 -30 12.50 3.30 3 1 30 8.20 3.70 -3 -1 30 8.10 3.90 3 -1 -30 5.50 2.70 3 1 30 6.50 2.40 4 -1 30 110.09 8.90 4 1 -30 113.89 9.00 4 -1 30 110.29 10.10 4 -1 30 121.49 8.40 4 1 -30 118.89 9.00 -4 1 30 122.59 10.60 4 1 -30 108.89 8.80 4 -1 -30 122.59 11.60 4 1 30 127.19 8.60 4 1 30 123.39 10.20 -4 -1 30 130.39 10.70 -4 -1 30 129.19 9.00 4 -1 -30 114.19 8.80 4 -1 -30 121.99 9.30 4 -1 -30 119.89 9.10 5 -1 30 92.59 8.20 5 1 -30 94.79 7.70 -5 1 30 94.99 8.90 5 1 -30 98.89 8.00 5 -1 30 88.69 8.90 5 -1 -30 94.09 7.80 5 1 30 95.49 8.70 -5 -1 30 96.29 9.20 5 -1 -30 99.59 8.00 5 1 30 104.69 8.60 6 1 -30 44.10 4.50 6 1 -30 45.80 4.40 6 1 30 30.90 5.60 6 -1 -30 39.00 4.30 -6 -1 30 29.70 4.60 0 2 30 180.28 12.30 0 -2 30 181.78 11.20 0 -2 30 188.38 12.50 0 -2 30 188.08 12.00 1 -2 30 41.10 4.00 -1 2 30 39.20 5.10 1 -2 30 44.30 5.10 1 -2 30 44.50 5.20 -1 -2 30 45.20 4.90 -1 -2 30 41.90 4.00 1 2 30 46.70 4.00 1 -2 -30 37.30 4.30 2 -2 30 143.09 10.40 2 -2 30 140.39 9.30 -2 2 30 143.09 10.90 2 -2 -30 140.59 9.90 2 2 30 140.09 9.20 -2 -2 30 139.09 10.50 2 -2 -30 143.19 9.80 3 -2 30 192.18 12.10 -3 2 30 197.68 14.00 3 2 -30 191.38 12.70 3 -2 30 186.88 13.60 3 2 -30 174.38 12.50 3 -2 -30 190.28 12.70 3 2 30 208.48 12.40 3 -2 -30 196.38 12.80 -3 -2 30 200.28 13.90 4 -2 30 114.09 9.50 -4 2 30 121.79 10.50 4 -2 30 119.09 10.20 4 2 -30 113.69 8.90 4 2 30 114.19 8.50 -4 -2 30 120.99 8.80 4 2 30 110.49 9.60 -4 -2 30 121.59 10.50 4 -2 -30 122.79 10.50 4 -2 -30 129.49 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23.90 3.30 0 -1 52 29.50 3.80 0 1 -52 27.80 4.10 1 -1 52 11.50 2.50 1 1 -52 13.80 3.10 -1 1 52 9.90 2.40 -1 1 -52 12.30 2.60 -1 -1 52 13.00 2.60 2 1 -52 40.40 4.20 2 -1 52 39.90 4.40 -2 1 -52 37.50 3.80 -2 -1 52 42.70 3.80 -2 -1 52 35.60 4.00 -3 1 52 6.40 2.30 3 -1 52 5.40 1.90 3 -1 52 6.30 2.10 3 1 52 6.80 2.00 -3 -1 52 5.40 1.90 0 -2 52 -0.10 1.90 0 2 -52 0.30 2.20 1 -2 52 45.30 4.20 1 -2 52 42.40 4.50 1 2 -52 42.70 4.50 -1 -2 52 45.30 4.20 -1 2 -52 52.19 4.60 1 -2 -52 45.60 5.10 2 -2 52 0.30 2.10 2 2 -52 1.50 2.00 -2 -2 52 1.80 1.70 -2 -2 52 1.60 1.80 2 -2 -52 1.50 2.30 -2 2 -52 1.30 1.70 3 -2 52 -0.20 2.40 3 -2 52 1.20 1.60 0 -3 52 5.30 1.90 0 -3 -52 4.70 2.40 0 3 -52 5.20 2.20 1 -3 52 5.40 2.20 -1 -3 -52 7.30 2.50 1 3 -52 8.30 2.30 1 -3 52 5.00 1.80 -1 -3 52 7.50 1.90 -1 3 -52 5.60 2.00 1 -3 -52 7.70 2.60 2 -3 52 5.90 2.00 2 -3 52 7.10 2.00 2 -3 -52 5.40 2.30 -2 -3 52 5.70 1.60 0 -4 52 61.09 4.30 0 -4 -52 64.69 5.20 -1 -4 -52 8.60 2.30 -1 -4 52 10.30 1.70 1 -4 -52 14.70 2.80 0 0 53 1.30 2.10 1 0 53 33.60 3.80 1 0 -53 36.10 4.10 -1 0 53 34.60 3.90 2 0 53 4.30 1.90 2 0 -53 3.40 2.30 2 0 53 4.50 2.30 3 0 53 6.70 2.80 0 1 -53 32.20 4.20 0 -1 53 35.00 4.00 1 1 -53 46.00 4.50 -1 1 53 43.00 4.20 1 -1 53 40.90 4.00 -1 -1 53 45.80 4.30 -1 1 -53 43.60 4.20 2 1 -53 195.38 11.80 2 -1 53 192.28 11.80 -2 -1 53 192.38 11.40 0 2 -53 3.50 2.20 0 -2 53 2.50 2.00 1 -2 53 10.50 2.20 1 2 -53 12.80 2.50 -1 -2 53 9.80 2.10 -1 2 -53 8.90 2.30 1 -2 -53 11.30 2.80 2 -2 53 56.09 4.60 -2 -2 53 63.19 5.50 2 -2 -53 53.79 5.00 -2 -2 53 58.89 4.30 0 -3 -53 -0.40 2.00 0 -3 53 0.20 1.60 0 3 -53 -0.60 2.80 1 -3 53 10.40 1.90 1 -3 53 7.90 2.20 -1 -3 -53 10.00 2.30 -1 -3 53 8.40 1.90 1 -3 -53 9.30 2.60 -2 -3 53 40.70 3.30 2 -3 -53 43.70 4.20 0 -4 -53 7.00 2.90 0 -4 53 4.90 1.70 0 0 54 4.10 2.10 1 0 54 38.60 3.70 -1 0 54 33.70 3.80 2 0 54 2.20 1.70 0 -1 54 1.50 1.80 0 1 -54 -0.40 2.00 0 1 54 -1.00 1.80 -1 1 54 0.40 1.70 1 -1 54 0.70 1.80 1 1 -54 2.70 2.10 -1 -1 54 1.60 1.80 -1 1 -54 -0.10 1.80 2 -1 54 36.70 3.70 -2 -1 54 40.60 3.30 0 -2 54 6.00 1.90 0 2 -54 10.40 2.40 1 -2 54 42.10 3.50 1 2 -54 42.50 4.60 -1 -2 54 35.30 3.40 -1 2 -54 36.10 4.40 1 -2 -54 37.20 4.30 2 -2 54 73.49 5.50 2 -2 -54 62.59 5.20 -2 -2 54 66.89 4.60 0 -3 -54 13.20 2.60 0 -3 54 10.00 1.80 1 -3 54 42.10 3.30 -1 -3 54 40.40 3.40 1 -3 -54 37.40 4.00 0 0 55 -0.50 1.70 -1 0 55 2.90 1.80 1 0 55 3.40 1.80 2 0 55 1.60 1.50 0 1 -55 20.70 3.20 0 -1 55 22.90 3.10 0 1 55 25.90 3.20 1 -1 55 48.80 4.00 -1 1 55 48.70 3.90 -1 -1 55 40.80 3.80 1 1 55 48.40 3.90 2 1 55 35.50 3.10 -2 -1 55 33.40 3.10 0 -2 55 72.89 5.20 1 -2 55 6.90 1.70 -1 -2 55 5.80 1.60 0 -3 55 1.30 1.30 0 0 56 58.59 4.40 1 0 56 6.00 1.80 -1 0 56 4.10 1.60 0 -1 56 1.10 1.70 0 1 56 1.40 1.60 1 -1 56 39.20 3.40 -1 1 56 43.30 3.30 -1 -1 56 34.40 3.30 1 1 56 40.20 3.50 0 -2 56 -0.30 1.40 0 2 56 0.90 1.40 1 -2 56 7.00 1.60 -1 -2 56 5.70 1.50 0 0 57 0.10 1.50 1 0 57 47.00 3.60 -1 0 57 44.80 3.50 0 1 57 1.80 1.50 0 -1 57 0.80 1.40 1 -1 57 11.90 1.90 -1 -1 57 13.60 1.90 1 1 57 13.20 1.90 0 0 58 108.49 6.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 46964 _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received'