data_Baran571 _audit_creation_date 2016-03-08 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155) ; _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 'C11 H10 F2 O2 S' _chemical_formula_sum 'C11 H10 F2 O2 S' _chemical_formula_weight 244.25 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 '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 6.7986(6) _cell_length_b 11.0791(9) _cell_length_c 13.9050(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1047.36(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6290 _cell_measurement_temperature 100.0 _cell_measurement_theta_max 25.377 _cell_measurement_theta_min 2.350 _shelx_estimated_absorpt_T_max 0.933 _shelx_estimated_absorpt_T_min 0.924 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_T_max 0.2363 _exptl_absorpt_correction_T_min 0.1946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1416 before and 0.0941 after correction. The Ratio of minimum to maximum transmission is 0.8235. 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 1.549 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description Block _exptl_crystal_F_000 504 _exptl_crystal_size_max 0.253 _exptl_crystal_size_mid 0.249 _exptl_crystal_size_min 0.221 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0827 _diffrn_reflns_av_unetI/netI 0.0488 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 18098 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.376 _diffrn_reflns_theta_min 2.350 _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 8.258 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker APEX II TXS' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe X-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker TXS' _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.692 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 1800 _reflns_number_total 1925 _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 0.269 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.067 _refine_ls_abs_structure_details ; Flack x determined using 710 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.06(8) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 1925 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0376 _refine_ls_restrained_S_all 1.050 _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^)+(0.0560P)^2^+0.1588P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0953 _refine_ls_wR_factor_ref 0.0978 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Ternary CH refined with riding coordinates: C4(H4) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B) 2.c Aromatic/amide H refined with riding coordinates: C7(H7), C9(H9), C11(H11) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 0.49139(10) 0.74082(6) 0.22301(5) 0.0128(2) Uani 1 1 d . . . . . F1 F 0.4238(3) 0.53716(17) 0.54798(13) 0.0265(5) Uani 1 1 d . . . . . F2 F 0.4697(3) 0.95878(17) 0.54439(12) 0.0264(5) Uani 1 1 d . . . . . O1 O 0.3946(3) 0.63169(19) 0.19220(16) 0.0171(5) Uani 1 1 d . . . . . O2 O 0.4209(4) 0.85552(19) 0.18838(15) 0.0183(6) Uani 1 1 d . . . . . C1 C 0.7393(4) 0.7284(3) 0.19506(19) 0.0134(6) Uani 1 1 d . . . . . C2 C 0.8792(5) 0.8325(3) 0.1719(2) 0.0184(7) Uani 1 1 d . . . . . H2A H 0.9811 0.8462 0.2216 0.022 Uiso 1 1 calc R . . . . H2B H 0.8116 0.9087 0.1550 0.022 Uiso 1 1 calc R . . . . C3 C 0.9537(5) 0.7595(3) 0.0832(2) 0.0215(7) Uani 1 1 d . . . . . H3A H 0.9249 0.7989 0.0209 0.026 Uiso 1 1 calc R . . . . H3B H 1.0942 0.7366 0.0874 0.026 Uiso 1 1 calc R . . . . C4 C 0.8138(5) 0.6569(3) 0.1073(2) 0.0166(7) Uani 1 1 d . . . . . H4 H 0.7257 0.6169 0.0594 0.020 Uiso 1 1 calc R . . . . C5 C 0.8488(5) 0.6105(3) 0.2063(2) 0.0168(7) Uani 1 1 d . . . . . H5A H 0.9849 0.6140 0.2315 0.020 Uiso 1 1 calc R . . . . H5B H 0.7725 0.5390 0.2272 0.020 Uiso 1 1 calc R . . . . C6 C 0.4768(4) 0.7444(3) 0.35070(19) 0.0130(6) Uani 1 1 d . . . . . C7 C 0.4605(5) 0.6348(3) 0.3991(2) 0.0147(7) Uani 1 1 d . . . . . H7 H 0.4595 0.5599 0.3659 0.018 Uiso 1 1 calc R . . . . C8 C 0.4458(5) 0.6412(3) 0.4983(2) 0.0180(8) Uani 1 1 d . . . . . C9 C 0.4492(4) 0.7482(3) 0.5490(2) 0.0179(7) Uani 1 1 d . . . . . H9 H 0.4397 0.7498 0.6172 0.021 Uiso 1 1 calc R . . . . C10 C 0.4668(5) 0.8523(3) 0.4961(2) 0.0172(7) Uani 1 1 d . . . . . C11 C 0.4816(6) 0.8548(3) 0.3975(2) 0.0153(7) Uani 1 1 d . . . . . H11 H 0.4944 0.9285 0.3632 0.018 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 0.0119(4) 0.0129(4) 0.0135(4) -0.0002(3) 0.0000(3) 0.0009(3) F1 0.0343(12) 0.0188(10) 0.0263(11) 0.0120(9) 0.0052(9) 0.0038(9) F2 0.0377(13) 0.0200(10) 0.0215(10) -0.0088(8) -0.0008(10) -0.0012(9) O1 0.0152(12) 0.0175(12) 0.0185(11) -0.0036(9) -0.0016(9) -0.0025(10) O2 0.0196(12) 0.0165(12) 0.0187(12) 0.0034(10) -0.0005(9) 0.0047(10) C1 0.0143(14) 0.0134(15) 0.0126(14) 0.0008(13) -0.0002(11) 0.0017(12) C2 0.0168(17) 0.0181(17) 0.0204(17) 0.0015(14) 0.0027(14) -0.0034(14) C3 0.0171(15) 0.0295(19) 0.0178(15) 0.0022(15) 0.0016(12) 0.0002(17) C4 0.0136(16) 0.0201(17) 0.0162(16) -0.0040(13) 0.0022(13) 0.0033(13) C5 0.0132(16) 0.0162(16) 0.0211(17) 0.0002(14) 0.0007(14) 0.0020(13) C6 0.0098(13) 0.0160(15) 0.0130(13) 0.0021(12) 0.0006(11) -0.0012(17) C7 0.0113(18) 0.0130(15) 0.0198(15) -0.0024(12) -0.0011(14) 0.0010(13) C8 0.0142(19) 0.0180(16) 0.0217(18) 0.0081(13) 0.0021(13) 0.0026(14) C9 0.0130(13) 0.0263(18) 0.0144(14) 0.0031(14) -0.0002(11) 0.0020(16) C10 0.0131(19) 0.0181(15) 0.0205(17) -0.0049(13) -0.0018(14) 0.0005(14) C11 0.0141(16) 0.0118(14) 0.0200(15) 0.0020(12) -0.0015(15) -0.0006(14) _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 O1 1.442(2) . ? S1 O2 1.441(2) . ? S1 C1 1.735(3) . ? S1 C6 1.779(3) . ? F1 C8 1.352(4) . ? F2 C10 1.358(3) . ? C1 C2 1.529(4) . ? C1 C4 1.540(4) . ? C1 C5 1.512(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.560(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.519(4) . ? C4 H4 1.0000 . ? C4 C5 1.488(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.393(4) . ? C6 C11 1.385(4) . ? C7 H7 0.9500 . ? C7 C8 1.385(4) . ? C8 C9 1.379(4) . ? C9 H9 0.9500 . ? C9 C10 1.374(4) . ? C10 C11 1.375(4) . ? C11 H11 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 O1 S1 C1 108.08(14) . . ? O1 S1 C6 106.85(14) . . ? O2 S1 O1 119.24(13) . . ? O2 S1 C1 108.55(15) . . ? O2 S1 C6 107.18(14) . . ? C1 S1 C6 106.23(13) . . ? C2 C1 S1 126.3(2) . . ? C2 C1 C4 91.0(2) . . ? C4 C1 S1 122.5(2) . . ? C5 C1 S1 121.6(2) . . ? C5 C1 C2 111.5(3) . . ? C5 C1 C4 58.4(2) . . ? C1 C2 H2A 113.9 . . ? C1 C2 H2B 113.9 . . ? C1 C2 C3 88.7(2) . . ? H2A C2 H2B 111.1 . . ? C3 C2 H2A 113.9 . . ? C3 C2 H2B 113.9 . . ? C2 C3 H3A 113.5 . . ? C2 C3 H3B 113.5 . . ? H3A C3 H3B 110.8 . . ? C4 C3 C2 90.6(2) . . ? C4 C3 H3A 113.5 . . ? C4 C3 H3B 113.5 . . ? C1 C4 H4 124.0 . . ? C3 C4 C1 89.8(2) . . ? C3 C4 H4 124.0 . . ? C5 C4 C1 59.87(19) . . ? C5 C4 C3 111.3(3) . . ? C5 C4 H4 124.0 . . ? C1 C5 H5A 117.6 . . ? C1 C5 H5B 117.6 . . ? C4 C5 C1 61.8(2) . . ? C4 C5 H5A 117.6 . . ? C4 C5 H5B 117.6 . . ? H5A C5 H5B 114.7 . . ? C7 C6 S1 117.8(2) . . ? C11 C6 S1 119.2(2) . . ? C11 C6 C7 123.0(3) . . ? C6 C7 H7 121.9 . . ? C8 C7 C6 116.2(3) . . ? C8 C7 H7 121.9 . . ? F1 C8 C7 118.2(3) . . ? F1 C8 C9 118.2(3) . . ? C9 C8 C7 123.5(3) . . ? C8 C9 H9 121.7 . . ? C10 C9 C8 116.7(3) . . ? C10 C9 H9 121.7 . . ? F2 C10 C9 117.8(3) . . ? F2 C10 C11 118.4(3) . . ? C9 C10 C11 123.9(3) . . ? C6 C11 H11 121.7 . . ? C10 C11 C6 116.7(3) . . ? C10 C11 H11 121.7 . . ? _shelx_res_file ; baran571.res created by SHELXL-2014/7 TITL Baran571 in P2(1)2(1)2(1) #19 REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.070, Rweak 0.012, Alpha 0.004, Orientation as input REM Flack x = 0.065 ( 0.072 ) from Parsons' quotients REM Formula found by SHELXT: C11 O2 F2 S CELL 0.71073 6.7986 11.0791 13.905 90 90 90 ZERR 4 0.0006 0.0009 0.0011 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 O F S UNIT 44 40 8 8 4 L.S. 10 PLAN 20 SIZE 0.253 0.249 0.221 TEMP -173.15 BOND $H fmap 2 ACTA 50 REM REM REM WGHT 0.056000 0.158800 FVAR 0.52115 S1 5 0.491391 0.740821 0.223014 11.00000 0.01190 0.01295 = 0.01347 -0.00021 0.00002 0.00092 F1 4 0.423815 0.537157 0.547976 11.00000 0.03427 0.01885 = 0.02631 0.01199 0.00516 0.00383 F2 4 0.469699 0.958778 0.544390 11.00000 0.03774 0.01998 = 0.02149 -0.00880 -0.00081 -0.00125 O1 3 0.394592 0.631689 0.192204 11.00000 0.01521 0.01750 = 0.01851 -0.00362 -0.00155 -0.00250 O2 3 0.420888 0.855519 0.188384 11.00000 0.01962 0.01652 = 0.01873 0.00340 -0.00050 0.00474 C1 1 0.739305 0.728403 0.195060 11.00000 0.01427 0.01338 = 0.01262 0.00082 -0.00015 0.00165 C2 1 0.879192 0.832475 0.171944 11.00000 0.01683 0.01807 = 0.02037 0.00146 0.00271 -0.00338 AFIX 23 H2A 2 0.981055 0.846239 0.221627 11.00000 -1.20000 H2B 2 0.811581 0.908697 0.154974 11.00000 -1.20000 AFIX 0 C3 1 0.953732 0.759451 0.083194 11.00000 0.01708 0.02954 = 0.01775 0.00219 0.00161 0.00024 AFIX 23 H3A 2 0.924937 0.798865 0.020867 11.00000 -1.20000 H3B 2 1.094229 0.736562 0.087402 11.00000 -1.20000 AFIX 0 C4 1 0.813809 0.656899 0.107340 11.00000 0.01364 0.02011 = 0.01615 -0.00402 0.00220 0.00330 AFIX 13 H4 2 0.725713 0.616874 0.059384 11.00000 -1.20000 AFIX 0 C5 1 0.848836 0.610485 0.206325 11.00000 0.01324 0.01617 = 0.02111 0.00017 0.00066 0.00204 AFIX 23 H5A 2 0.984918 0.613983 0.231512 11.00000 -1.20000 H5B 2 0.772497 0.539030 0.227169 11.00000 -1.20000 AFIX 0 C6 1 0.476808 0.744414 0.350696 11.00000 0.00985 0.01603 = 0.01303 0.00209 0.00058 -0.00116 C7 1 0.460499 0.634797 0.399063 11.00000 0.01132 0.01304 = 0.01982 -0.00236 -0.00110 0.00097 AFIX 43 H7 2 0.459490 0.559852 0.365871 11.00000 -1.20000 AFIX 0 C8 1 0.445834 0.641194 0.498289 11.00000 0.01418 0.01805 = 0.02167 0.00805 0.00215 0.00261 C9 1 0.449163 0.748176 0.549012 11.00000 0.01301 0.02631 = 0.01436 0.00305 -0.00024 0.00198 AFIX 43 H9 2 0.439742 0.749768 0.617165 11.00000 -1.20000 AFIX 0 C10 1 0.466777 0.852288 0.496073 11.00000 0.01314 0.01805 = 0.02054 -0.00491 -0.00176 0.00054 C11 1 0.481568 0.854768 0.397496 11.00000 0.01413 0.01177 = 0.01998 0.00197 -0.00151 -0.00061 AFIX 43 H11 2 0.494414 0.928487 0.363172 11.00000 -1.20000 AFIX 0 HKLF 4 REM Baran571 in P2(1)2(1)2(1) #19 REM R1 = 0.0376 for 1800 Fo > 4sig(Fo) and 0.0401 for all 1925 data REM 145 parameters refined using 0 restraints END WGHT 0.0560 0.1588 REM Highest difference peak 0.269, deepest hole -0.410, 1-sigma level 0.067 Q1 1 0.6413 0.7398 0.2010 11.00000 0.05 0.27 Q2 1 0.4930 0.7418 0.2889 11.00000 0.05 0.24 Q3 1 0.2590 0.6256 0.2190 11.00000 0.05 0.22 Q4 1 0.4065 0.6435 0.4448 11.00000 0.05 0.22 Q5 1 0.5130 0.7945 0.3844 11.00000 0.05 0.20 Q6 1 0.5358 0.5777 0.2640 11.00000 0.05 0.20 Q7 1 0.7925 0.7834 0.1879 11.00000 0.05 0.20 Q8 1 0.7785 0.9445 0.1007 11.00000 0.05 0.19 Q9 1 0.2684 0.7436 0.3348 11.00000 0.05 0.19 Q10 1 1.1464 0.7370 0.2759 11.00000 0.05 0.19 Q11 1 1.1803 0.6750 0.2370 11.00000 0.05 0.19 Q12 1 0.5142 0.6933 0.3777 11.00000 0.05 0.18 Q13 1 0.4355 0.8562 0.4442 11.00000 0.05 0.18 Q14 1 0.2803 0.4618 0.4774 11.00000 0.05 0.18 Q15 1 0.8235 0.4230 0.1320 11.00000 0.05 0.17 Q16 1 0.2209 0.5823 0.3014 11.00000 0.05 0.16 Q17 1 1.2123 0.8237 0.2579 11.00000 0.05 0.16 Q18 1 0.1821 0.5933 0.1260 11.00000 0.05 0.16 Q19 1 0.2922 1.0589 0.6050 11.00000 0.05 0.16 Q20 1 0.7323 0.9232 0.3167 11.00000 0.05 0.16 ; _shelx_res_checksum 86271 _shelx_hkl_file ; -1 0 0 -13.80 0.40 1 0 0 -13.80 0.40 1 0 0 -13.10 0.60 1 0 0 -13.60 0.30 1 0 0 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5 35.30 4.40 3 -6 -5 34.50 6.90 3 -6 -5 28.00 6.50 -3 -6 5 35.60 6.70 3 -6 -5 33.60 8.40 3 6 5 36.10 4.30 3 -6 -5 29.40 8.40 4 -6 5 46.20 11.00 4 6 -5 48.10 11.00 4 -6 5 51.89 9.80 4 -6 5 53.09 10.30 4 -6 5 55.89 10.50 -4 6 5 68.19 11.00 -4 6 5 53.29 10.00 4 6 5 71.79 11.00 -4 6 -5 39.60 9.30 4 6 5 43.80 7.30 -4 6 -5 60.19 8.80 4 6 5 72.09 9.30 4 6 5 51.79 10.20 4 -6 -5 60.29 8.70 4 6 5 56.69 7.40 4 -6 -5 64.39 12.10 4 6 5 62.29 7.50 -4 -6 5 69.29 10.40 4 -6 -5 81.99 13.70 4 -6 -5 56.69 10.20 -4 6 -5 57.79 10.20 -4 6 -5 56.09 9.70 4 -6 -5 45.10 9.00 4 -6 -5 43.40 9.60 -4 -6 5 50.29 9.30 -5 6 5 19.20 6.50 -5 6 5 40.20 8.20 5 -6 5 18.40 6.60 5 6 -5 28.10 8.30 5 -6 5 23.90 6.70 5 -6 5 29.90 7.00 5 -6 5 17.70 5.70 -5 6 -5 20.90 6.50 5 6 5 33.40 5.50 5 -6 -5 38.00 9.60 5 6 5 28.60 5.20 5 6 5 18.60 5.90 5 -6 -5 29.10 7.20 -5 -6 5 16.10 5.10 5 -6 -5 26.70 8.00 5 6 5 18.20 4.70 -5 6 -5 23.90 5.60 5 6 5 18.90 5.80 -5 -6 5 18.40 5.50 -5 6 -5 17.90 5.80 5 -6 -5 17.70 6.50 -5 6 -5 26.40 6.10 6 -6 5 60.99 11.60 6 -6 5 67.89 12.00 6 -6 5 43.40 11.20 -6 6 5 63.39 12.10 -6 6 5 50.49 11.50 6 6 -5 49.70 11.90 6 -6 5 53.09 10.90 6 -6 -5 47.70 11.50 -6 -6 5 63.49 10.20 6 -6 -5 49.40 10.80 -6 6 -5 71.09 12.20 6 6 5 39.20 8.70 6 -6 -5 47.30 11.90 6 -6 -5 53.09 11.70 -6 6 -5 76.19 12.20 0 7 -5 336.47 41.40 0 7 -5 290.87 40.00 0 -7 5 337.77 40.50 0 -7 5 349.07 39.20 0 7 5 387.96 38.00 0 -7 -5 362.06 39.20 0 7 5 328.97 40.60 0 7 5 379.26 38.00 0 7 -5 346.97 41.00 0 7 -5 306.67 40.20 0 7 5 324.87 40.10 0 -7 5 310.47 41.30 0 7 5 346.87 38.40 0 7 -5 350.56 39.90 0 -7 -5 385.26 41.90 0 -7 5 314.47 39.90 -1 7 5 14.90 3.50 -1 7 5 12.40 3.10 1 7 -5 10.40 4.10 1 -7 5 13.40 3.70 1 -7 5 21.20 5.90 1 -7 5 10.20 5.10 1 -7 5 19.30 5.50 1 7 -5 13.60 4.80 -1 7 5 13.70 3.20 1 7 -5 15.30 5.30 -1 -7 5 14.50 4.80 1 7 5 7.50 3.70 -1 7 -5 12.10 4.80 -1 7 -5 14.40 5.00 1 7 5 12.40 3.00 -1 7 -5 14.90 4.90 1 7 5 14.50 1.90 -1 -7 5 23.90 4.50 1 7 5 14.40 1.90 -1 7 -5 12.10 4.80 1 7 5 14.70 1.90 1 -7 -5 10.70 3.70 1 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-3 5 14 8.00 4.60 3 5 -14 4.50 3.60 3 -5 14 3.70 4.20 -3 5 -14 5.70 4.20 -3 5 -14 4.70 4.20 -3 -5 14 2.00 3.00 3 -5 -14 5.80 4.90 3 -5 -14 4.40 4.40 0 6 -14 226.88 31.20 0 6 -14 217.18 30.60 0 -6 -14 221.38 29.90 0 6 14 291.17 29.50 0 -6 -14 229.48 29.90 1 -6 14 38.00 10.60 1 -6 14 28.00 8.10 -1 6 14 31.70 7.20 1 6 -14 19.30 8.60 1 6 -14 25.40 8.50 1 -6 -14 36.50 8.60 1 -6 -14 16.60 6.80 -1 6 -14 33.90 9.50 -1 -6 14 27.10 7.80 -1 6 -14 28.30 8.80 2 6 -14 88.39 16.60 2 6 -14 107.29 17.50 -2 6 14 66.49 12.60 2 -6 14 71.29 15.30 2 -6 14 50.09 12.40 -2 6 -14 96.99 15.50 -2 -6 14 71.19 13.90 2 -6 -14 89.59 15.50 -2 6 -14 45.20 12.40 2 -6 -14 71.69 14.10 0 7 -14 0.60 4.20 0 -7 -14 3.80 4.30 0 -7 -14 0.30 3.30 0 7 -14 -0.10 4.10 0 -7 14 2.90 3.60 1 7 -14 45.80 11.50 1 -7 14 35.50 8.80 1 -7 14 22.40 8.70 1 7 -14 28.80 9.50 -1 7 -14 25.40 9.00 -1 -7 14 26.70 7.90 1 -7 -14 22.30 8.20 1 -7 -14 21.70 7.40 -1 7 -14 19.40 8.20 0 0 15 0.50 2.80 0 0 -15 -0.90 2.40 0 0 -15 1.60 2.30 0 0 -15 1.20 2.90 0 0 -15 -0.70 1.60 1 0 -15 152.78 21.00 1 0 -15 169.18 21.20 1 0 -15 163.28 22.20 1 0 15 164.28 22.10 -1 0 -15 191.88 21.40 -1 0 15 207.68 23.30 -1 0 -15 160.48 21.10 1 0 -15 132.29 21.50 2 0 -15 2.10 3.40 -2 0 15 4.90 3.90 2 0 -15 1.80 2.90 -2 0 -15 0.90 2.30 -2 0 -15 -0.50 2.00 2 0 15 -0.50 2.60 2 0 -15 2.50 3.50 2 0 -15 4.40 4.50 3 0 -15 121.99 19.70 3 0 -15 149.79 21.30 -3 0 15 158.48 21.00 3 0 -15 140.49 21.10 3 0 15 137.59 19.40 3 0 -15 168.88 20.60 0 1 -15 6.80 4.50 0 -1 -15 8.10 3.70 0 -1 -15 6.20 3.60 0 -1 -15 9.70 3.90 0 1 -15 10.70 4.70 0 1 15 2.60 3.20 0 -1 15 12.50 5.10 0 -1 -15 6.30 2.90 0 1 -15 7.70 3.30 0 1 -15 11.20 4.50 1 1 -15 10.90 4.90 1 -1 15 4.90 3.90 -1 -1 -15 5.40 2.80 -1 1 15 6.50 4.50 -1 -1 -15 6.70 3.00 1 1 -15 7.60 3.50 1 1 -15 12.00 5.40 1 1 -15 5.60 3.10 -1 1 -15 7.90 4.10 1 -1 -15 8.70 3.70 -1 -1 15 3.90 4.10 -1 1 -15 4.50 3.70 1 -1 -15 6.30 3.70 1 1 15 7.90 4.30 1 -1 -15 7.20 3.80 1 -1 -15 8.90 3.90 2 1 -15 41.30 8.80 -2 1 15 35.60 9.10 2 1 -15 32.80 9.00 2 1 -15 33.90 8.40 2 -1 15 66.99 10.80 2 1 -15 47.10 10.60 2 -1 -15 38.50 8.70 2 -1 -15 38.30 9.20 2 1 15 26.40 7.10 2 -1 -15 33.40 8.70 -2 -1 15 52.59 10.50 -2 1 -15 34.00 7.50 2 -1 -15 29.80 7.90 -2 1 -15 36.10 7.50 3 1 -15 0.50 2.60 3 1 -15 4.90 4.90 3 -1 15 0.70 2.30 3 1 -15 1.30 3.20 3 1 -15 -1.90 3.50 -3 1 15 2.70 3.90 -3 -1 15 5.50 4.60 3 1 15 -1.00 2.50 3 -1 -15 3.50 3.30 3 -1 -15 3.80 4.00 3 -1 -15 2.10 3.40 3 -1 -15 1.90 3.50 -3 1 -15 0.10 2.60 -3 1 -15 0.60 2.40 0 2 -15 4.60 3.00 0 2 -15 1.50 4.00 0 -2 -15 3.30 3.00 0 -2 -15 5.70 4.90 0 2 15 1.80 3.30 0 -2 -15 3.40 3.50 0 2 -15 2.00 3.60 0 2 -15 3.10 2.80 0 -2 15 6.60 4.30 0 -2 -15 4.10 3.10 1 2 -15 32.90 9.10 1 -2 15 37.90 8.30 1 2 -15 36.20 7.80 -1 2 15 28.10 7.90 1 2 -15 41.40 10.10 1 2 -15 36.70 7.70 -1 2 -15 48.60 9.40 1 -2 -15 35.90 8.00 1 -2 -15 38.80 8.00 -1 -2 15 46.00 10.00 1 2 15 43.50 8.90 1 -2 -15 37.60 8.30 -1 2 -15 28.70 8.00 1 -2 -15 34.40 7.50 -2 2 15 20.80 6.80 2 2 -15 18.90 6.60 2 2 -15 2.70 4.50 2 2 -15 11.50 4.80 2 2 -15 6.30 3.90 2 -2 15 15.40 5.50 2 2 15 16.90 5.40 2 -2 -15 11.20 5.00 -2 -2 15 27.90 7.40 2 -2 -15 15.10 5.90 -2 2 -15 9.10 4.60 2 -2 -15 6.00 4.40 2 -2 -15 15.10 5.70 -2 2 -15 12.90 5.10 3 -2 15 36.90 9.10 3 2 -15 46.80 10.30 3 2 -15 49.60 12.00 3 2 -15 47.20 9.90 3 2 -15 42.30 11.00 -3 2 15 46.70 10.80 3 -2 -15 60.59 11.70 3 2 15 40.60 8.80 -3 -2 15 65.29 12.30 3 -2 -15 47.20 11.00 3 -2 -15 47.30 10.40 -3 2 -15 44.70 8.80 3 -2 -15 48.50 10.40 -3 2 -15 47.60 9.00 0 3 15 56.39 10.90 0 3 -15 56.79 10.50 0 3 -15 50.69 11.80 0 3 -15 55.69 12.30 0 -3 -15 73.99 12.10 0 -3 15 50.49 11.00 -1 3 15 10.50 4.60 1 3 -15 9.60 5.40 1 3 -15 0.80 4.40 1 -3 15 7.20 4.60 1 3 -15 0.00 2.50 1 3 -15 6.40 3.80 -1 3 -15 4.80 4.20 1 3 15 7.10 3.90 -1 3 -15 10.50 5.00 1 -3 -15 4.80 3.50 1 -3 -15 6.90 4.30 -1 -3 15 5.20 3.80 2 -3 15 79.79 14.40 2 3 -15 80.19 13.20 2 3 -15 84.29 15.80 2 -3 15 58.19 12.70 2 3 -15 105.29 13.30 2 3 -15 76.89 15.60 -2 3 15 91.29 14.70 -2 -3 15 120.69 16.70 2 -3 -15 70.09 13.50 2 -3 -15 79.79 14.50 2 -3 -15 53.29 11.40 -2 3 -15 58.69 12.80 -2 3 -15 65.89 13.00 2 -3 -15 73.19 14.00 2 3 15 77.79 12.90 3 3 -15 -0.20 2.90 3 -3 15 0.40 3.20 3 3 -15 1.00 4.20 3 3 -15 -1.00 3.20 -3 3 15 3.60 3.80 3 -3 15 0.10 3.10 3 3 -15 4.80 4.90 -3 3 -15 0.10 3.70 3 -3 -15 3.40 4.10 -3 3 -15 -0.60 2.70 3 -3 -15 2.20 3.50 3 -3 -15 -0.40 3.60 -3 -3 15 -1.10 3.20 3 3 15 1.50 2.70 3 -3 -15 2.30 3.80 0 4 -15 3.50 4.40 0 -4 15 -1.50 1.20 0 4 15 -1.50 2.10 0 4 -15 3.10 4.10 1 4 -15 233.08 29.30 -1 4 15 274.17 30.70 1 -4 15 223.18 30.60 1 4 -15 250.67 29.60 1 4 -15 207.98 31.40 1 -4 -15 249.18 30.70 -1 4 -15 259.67 31.50 1 4 15 220.48 29.40 1 -4 -15 244.98 30.30 -1 -4 15 222.88 30.70 -1 4 -15 292.07 32.40 -2 4 15 14.50 5.70 2 4 -15 21.80 6.40 2 4 -15 24.40 6.50 2 -4 15 18.40 6.60 2 -4 15 27.50 8.10 2 4 -15 26.50 9.00 2 4 -15 27.60 8.90 -2 4 -15 13.80 6.30 2 -4 -15 16.90 6.30 -2 4 -15 24.40 7.60 2 -4 -15 12.00 5.80 -2 -4 15 29.00 8.00 2 4 15 19.50 5.70 0 -5 15 5.50 4.30 0 5 -15 8.80 5.60 0 5 15 4.80 3.80 0 5 -15 6.90 5.30 1 -5 15 18.50 6.20 -1 5 15 13.00 5.70 1 5 -15 21.70 7.80 1 5 -15 25.00 6.00 1 5 -15 25.00 8.40 1 5 -15 17.60 5.70 1 -5 -15 19.70 6.30 1 -5 -15 24.10 6.80 -1 5 -15 17.10 6.40 -1 5 -15 9.30 6.10 1 5 15 16.30 6.70 -1 -5 15 18.60 6.80 2 -5 15 45.90 10.90 2 5 -15 42.60 12.20 -2 -5 15 52.79 11.70 -2 5 -15 81.39 14.10 0 0 16 30.50 7.90 0 0 -16 20.60 6.20 0 0 -16 17.50 6.00 -1 0 -16 -1.60 2.70 1 0 -16 8.80 4.50 1 0 16 5.80 4.00 -1 0 16 6.00 4.40 1 0 -16 1.30 3.10 1 0 -16 7.20 3.70 1 0 -16 2.10 2.80 -1 0 -16 2.60 2.90 2 0 -16 61.09 14.00 -2 0 16 71.49 14.50 2 0 -16 82.49 14.40 2 0 16 76.09 13.70 2 0 -16 74.89 14.60 2 0 -16 121.09 14.40 0 1 16 0.40 3.00 0 -1 -16 5.40 3.80 0 1 -16 1.40 3.40 0 1 -16 -0.30 2.90 0 -1 -16 2.20 3.10 0 -1 16 1.10 3.60 1 1 -16 40.10 8.80 1 1 -16 44.10 10.10 1 -1 16 39.00 9.40 1 1 -16 42.40 8.50 1 1 -16 54.49 10.70 -1 1 16 42.60 9.80 1 -1 -16 33.70 8.60 -1 1 -16 36.40 8.80 1 -1 -16 41.20 9.90 -1 1 -16 43.70 9.00 -1 -1 16 41.70 9.90 1 1 16 40.50 9.40 1 -1 -16 51.29 9.00 2 -1 16 3.30 3.50 2 1 -16 8.60 5.10 2 1 -16 1.90 3.30 -2 1 16 2.90 3.80 2 1 -16 2.80 3.50 2 1 -16 1.20 3.60 -2 1 -16 4.50 3.10 2 1 16 4.10 3.50 -2 1 -16 3.00 3.30 2 -1 -16 3.40 4.00 2 -1 -16 0.40 3.20 2 -1 -16 0.40 2.90 -2 -1 16 -2.20 2.50 2 -1 -16 4.80 4.70 0 2 -16 64.29 12.50 0 2 16 52.39 11.00 0 -2 16 51.59 11.60 0 2 -16 61.09 12.20 1 2 -16 1.60 2.80 1 2 -16 0.70 3.20 -1 2 16 -1.40 2.60 1 2 -16 1.20 3.80 1 -2 16 -0.90 2.50 1 2 16 2.00 3.40 1 -2 -16 0.50 2.60 1 -2 -16 1.40 4.10 -1 2 -16 1.80 3.00 -1 -2 16 0.30 2.60 -1 2 -16 1.60 3.20 -2 2 16 149.88 18.50 2 2 -16 116.99 17.00 2 -2 16 114.59 17.20 2 2 -16 108.29 19.90 2 2 -16 114.19 16.80 2 2 -16 113.69 20.30 2 -2 -16 132.39 17.30 2 2 16 153.88 17.50 -2 -2 16 176.18 20.10 -2 2 -16 99.99 16.30 -2 2 -16 126.99 16.90 2 -2 -16 104.59 17.00 2 -2 -16 89.19 17.00 2 -2 -16 109.89 16.80 0 3 16 -1.10 2.70 0 3 -16 -1.80 3.70 0 -3 16 -0.50 3.00 0 3 -16 -0.80 4.00 -1 3 16 26.10 7.80 1 -3 16 36.20 8.90 1 3 -16 49.99 11.20 1 3 -16 37.20 10.20 -1 3 -16 27.40 8.10 -1 3 -16 32.70 8.70 1 3 16 46.50 9.10 1 -3 -16 31.40 9.30 -1 -3 16 39.10 9.60 0 -4 16 204.98 26.20 0 4 -16 188.68 27.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 43441 _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received'