data_exp_489 _audit_creation_date 2021-04-16 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C13 H11 F3 O3' _chemical_formula_sum 'C13 H11 F3 O3' _chemical_formula_weight 272.22 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_formula 'C H F O' _chemical_oxdiff_usercomment SKP-ester 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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.14490(10) _cell_length_b 8.4717(2) _cell_length_c 13.8636(2) _cell_angle_alpha 90 _cell_angle_beta 91.1750(10) _cell_angle_gamma 90 _cell_volume 604.13(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8025 _cell_measurement_temperature 93.15 _cell_measurement_theta_max 74.8020 _cell_measurement_theta_min 6.0990 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.186 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.46861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 280 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_unetI/netI 0.0316 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.964 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 11222 _diffrn_reflns_point_group_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 0.929 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.635 _diffrn_reflns_theta_min 3.188 _diffrn_ambient_temperature 93.15 _diffrn_detector 'Rigaku HyPix-6000 area detector' _diffrn_detector_area_resol_mean 10.0 _diffrn_detector_type 'HPC area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.964 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w 35.00 122.00 0.50 0.05 -- 47.95 33.00 -64.00 174 2 \w 93.00 174.00 0.50 0.05 -- 106.49 33.00 -64.00 162 3 \w 142.00 174.00 0.50 0.05 -- 106.49 77.00 0.00 64 4 \w 84.00 110.00 0.50 0.05 -- 106.49 77.00 0.00 52 5 \w 33.00 63.00 0.50 0.05 -- 106.49 -33.00 136.00 60 6 \w 70.00 123.00 0.50 0.05 -- 106.49 -61.00 90.00 106 7 \w 36.00 121.00 0.50 0.05 -- 47.95 38.00 0.00 170 8 \w 32.00 60.00 0.50 0.05 -- 106.49 -30.00 0.00 56 9 \w 32.00 57.00 0.50 0.05 -- 106.49 -30.00 30.00 50 10 \w 25.00 120.00 0.50 0.05 -- 47.95 77.00 60.00 190 11 \w -61.00 26.00 0.50 0.05 -- -47.95 33.00 -64.00 174 12 \w -69.00 -26.00 0.50 0.05 -- -100.00 33.00 -64.00 86 13 \w -96.00 -20.00 0.50 0.05 -- -47.95 125.00 0.00 152 14 \w -67.00 -25.00 0.50 0.05 -- -100.00 30.00 60.00 84 15 \w -67.00 -25.00 0.50 0.05 -- -100.00 30.00 90.00 84 16 \w -81.00 -28.00 0.50 0.05 -- -100.00 45.00 120.00 106 17 \w -122.00 -35.00 0.50 0.05 -- -47.95 -33.00 136.00 174 18 \w -116.00 -27.00 0.50 0.05 -- -100.00 61.00 120.00 178 19 \w -121.00 -36.00 0.50 0.05 -- -47.95 -38.00 0.00 170 20 \w -120.00 -25.00 0.50 0.05 -- -47.95 -77.00 90.00 190 21 \w -123.00 -27.00 0.50 0.05 -- -100.00 77.00 120.00 192 22 \w -173.00 -86.00 0.50 0.05 -- -100.00 -33.00 136.00 174 23 \w -172.00 -85.00 0.50 0.05 -- -100.00 -55.00 -11.78 174 24 \w -172.00 -87.00 0.50 0.05 -- -100.00 -45.00 30.00 170 25 \w -173.00 -77.00 0.50 0.05 -- -100.00 -77.00 90.00 192 26 \w -172.00 -85.00 0.50 0.05 -- -100.00 -57.00 11.72 174 27 \w -173.00 -81.00 0.50 0.05 -- -100.00 -67.00 70.38 184 28 \w -173.00 -77.00 0.50 0.05 -- -100.00 -77.00 120.00 192 29 \w -172.00 -84.00 0.50 0.05 -- -100.00 -59.00 54.29 176 30 \w -173.00 -78.00 0.50 0.05 -- -100.00 -74.00 1.84 190 31 \w -173.00 -83.00 0.50 0.05 -- -100.00 -61.00 90.00 180 32 \w -173.00 -77.00 0.50 0.05 -- -100.00 -77.00 60.00 192 33 \w -172.00 -84.00 0.50 0.05 -- -100.00 -60.00 3.63 176 34 \w -173.00 -80.00 0.50 0.05 -- -100.00 -70.00 46.05 186 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-Custom' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0522593000 _diffrn_orient_matrix_UB_12 -0.0619375000 _diffrn_orient_matrix_UB_13 0.1030336000 _diffrn_orient_matrix_UB_21 -0.2887647000 _diffrn_orient_matrix_UB_22 -0.0452103000 _diffrn_orient_matrix_UB_23 0.0079030000 _diffrn_orient_matrix_UB_31 0.0594436000 _diffrn_orient_matrix_UB_32 -0.1649480000 _diffrn_orient_matrix_UB_33 -0.0409221000 _diffrn_radiation_monochromator 'multi-layer mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'rotating anode X-ray generator' _diffrn_source_type micromax007 _reflns_Friedel_coverage 0.801 _reflns_Friedel_fraction_full 0.960 _reflns_Friedel_fraction_max 0.889 _reflns_number_gt 2284 _reflns_number_total 2381 _reflns_odcompleteness_completeness 100.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _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 'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 0.203 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.050 _refine_ls_abs_structure_details ; Flack x determined using 982 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.02(9) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 173 _refine_ls_number_reflns 2381 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0387 _refine_ls_R_factor_gt 0.0374 _refine_ls_restrained_S_all 1.113 _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^)+(0.0680P)^2^+0.0709P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.1042 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C00A(H00A), C00F(H00F), C00H(H00H) 2.b Aromatic/amide H refined with riding coordinates: C00B(H00B), C00C(H00C), C00D(H00D), C00G(H00G), C00I(H00I) 2.c Idealised Me refined as rotating group: C00J(H00E,H00J,H00K) ; _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 F001 F 1.0831(3) 0.7296(2) 0.51449(11) 0.0333(4) Uani 1 1 d . . . . . F002 F 0.7992(4) 0.5938(2) 0.43380(12) 0.0396(5) Uani 1 1 d . . . . . F003 F 0.7205(3) 0.8363(2) 0.46879(13) 0.0393(5) Uani 1 1 d . . . . . O004 O 0.3785(3) 0.8091(2) 0.73450(13) 0.0284(5) Uani 1 1 d . . . . . O005 O 0.8324(4) 0.2836(2) 0.71065(14) 0.0306(4) Uani 1 1 d . . . . . O006 O 0.4763(4) 0.4308(3) 0.73809(13) 0.0300(4) Uani 1 1 d . . . . . C007 C 0.6707(5) 0.7651(3) 0.86531(18) 0.0234(5) Uani 1 1 d . . . . . C008 C 0.5918(5) 0.7631(3) 0.76120(18) 0.0242(5) Uani 1 1 d . . . . . C009 C 0.6941(5) 0.4169(3) 0.70779(17) 0.0241(5) Uani 1 1 d . . . . . C00A C 0.7928(5) 0.7153(3) 0.68889(17) 0.0220(5) Uani 1 1 d . . . . . H00A H 0.947241 0.786719 0.686246 0.026 Uiso 1 1 calc R U . . . C00B C 0.5191(5) 0.8511(3) 0.92927(19) 0.0262(5) Uani 1 1 d . . . . . H00B H 0.371013 0.907274 0.905825 0.031 Uiso 1 1 calc R U . . . C00C C 0.8880(5) 0.6817(3) 0.90051(19) 0.0253(5) Uani 1 1 d . . . . . H00C H 0.994318 0.624658 0.857409 0.030 Uiso 1 1 calc R U . . . C00D C 0.9471(5) 0.6827(4) 0.9987(2) 0.0273(6) Uani 1 1 d . . . . . H00D H 1.091356 0.623755 1.022942 0.033 Uiso 1 1 calc R U . . . C00E C 0.8263(5) 0.7026(4) 0.50309(19) 0.0287(6) Uani 1 1 d . . . . . C00F C 0.7026(5) 0.6530(4) 0.59417(19) 0.0258(6) Uani 1 1 d . . . . . H00F H 0.511196 0.633375 0.588527 0.031 Uiso 1 1 calc R U . . . C00G C 0.5842(5) 0.8548(3) 1.0270(2) 0.0288(6) Uani 1 1 d . . . . . H00G H 0.483437 0.915626 1.069981 0.035 Uiso 1 1 calc R U . . . C00H C 0.8472(5) 0.5443(3) 0.66343(17) 0.0237(5) Uani 1 1 d . . . . . H00H H 1.030558 0.517998 0.647036 0.028 Uiso 1 1 calc R U . . . C00I C 0.7967(5) 0.7695(4) 1.06181(19) 0.0285(6) Uani 1 1 d . . . . . H00I H 0.839260 0.770406 1.128815 0.034 Uiso 1 1 calc R U . . . C00J C 0.7011(7) 0.1460(4) 0.7467(2) 0.0379(7) Uani 1 1 d . . . . . H00E H 0.553458 0.120106 0.703840 0.057 Uiso 1 1 calc R U . . . H00J H 0.638287 0.167648 0.811679 0.057 Uiso 1 1 calc R U . . . H00K H 0.822312 0.056821 0.749232 0.057 Uiso 1 1 calc R U . . . 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 F001 0.0225(7) 0.0485(11) 0.0292(8) 0.0081(7) 0.0039(5) -0.0046(7) F002 0.0456(10) 0.0485(11) 0.0247(8) -0.0020(7) 0.0029(7) -0.0098(9) F003 0.0343(9) 0.0456(11) 0.0383(8) 0.0200(8) 0.0029(7) 0.0052(8) O004 0.0174(8) 0.0367(12) 0.0310(9) 0.0008(8) -0.0009(7) 0.0015(8) O005 0.0339(10) 0.0264(10) 0.0317(10) 0.0028(8) 0.0053(8) -0.0016(8) O006 0.0239(9) 0.0357(11) 0.0304(9) 0.0042(8) 0.0046(7) -0.0046(8) C007 0.0176(10) 0.0263(13) 0.0263(12) 0.0007(10) 0.0015(8) -0.0023(10) C008 0.0180(10) 0.0256(13) 0.0291(13) 0.0024(10) 0.0024(9) -0.0028(10) C009 0.0257(12) 0.0269(13) 0.0198(10) -0.0006(9) 0.0000(9) -0.0006(11) C00A 0.0168(11) 0.0257(13) 0.0235(11) 0.0028(10) 0.0004(8) -0.0017(10) C00B 0.0203(11) 0.0267(14) 0.0317(12) 0.0010(11) 0.0022(10) -0.0015(10) C00C 0.0184(10) 0.0298(14) 0.0279(12) -0.0003(11) 0.0026(9) 0.0013(10) C00D 0.0204(12) 0.0324(15) 0.0291(12) 0.0018(11) -0.0010(9) -0.0002(10) C00E 0.0227(12) 0.0382(16) 0.0251(12) 0.0051(11) -0.0004(9) -0.0012(11) C00F 0.0201(11) 0.0333(15) 0.0239(11) 0.0033(10) 0.0000(9) -0.0013(11) C00G 0.0254(12) 0.0307(15) 0.0305(12) -0.0041(11) 0.0058(10) -0.0011(11) C00H 0.0203(11) 0.0296(15) 0.0213(11) 0.0024(10) 0.0026(9) -0.0015(10) C00I 0.0262(12) 0.0350(15) 0.0244(11) -0.0009(11) 0.0008(9) -0.0061(11) C00J 0.0414(16) 0.0309(16) 0.0414(15) 0.0063(12) 0.0046(13) -0.0044(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 F001 C00E 1.347(3) . ? F002 C00E 1.337(4) . ? F003 C00E 1.340(4) . ? O004 C008 1.215(3) . ? O005 C009 1.334(3) . ? O005 C00J 1.442(4) . ? O006 C009 1.211(3) . ? C007 C008 1.491(3) . ? C007 C00B 1.398(4) . ? C007 C00C 1.402(4) . ? C008 C00A 1.510(3) . ? C009 C00H 1.478(4) . ? C00A H00A 1.0000 . ? C00A C00F 1.481(3) . ? C00A C00H 1.519(4) . ? C00B H00B 0.9500 . ? C00B C00G 1.389(4) . ? C00C H00C 0.9500 . ? C00C C00D 1.389(4) . ? C00D H00D 0.9500 . ? C00D C00I 1.390(4) . ? C00E C00F 1.486(4) . ? C00F H00F 1.0000 . ? C00F C00H 1.515(4) . ? C00G H00G 0.9500 . ? C00G C00I 1.389(4) . ? C00H H00H 1.0000 . ? C00I H00I 0.9500 . ? C00J H00E 0.9800 . ? C00J H00J 0.9800 . ? C00J H00K 0.9800 . ? 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 C009 O005 C00J 116.2(2) . . ? C00B C007 C008 118.4(2) . . ? C00B C007 C00C 119.6(2) . . ? C00C C007 C008 122.0(2) . . ? O004 C008 C007 121.2(2) . . ? O004 C008 C00A 120.7(2) . . ? C007 C008 C00A 118.0(2) . . ? O005 C009 C00H 110.0(2) . . ? O006 C009 O005 124.7(3) . . ? O006 C009 C00H 125.3(3) . . ? C008 C00A H00A 114.7 . . ? C008 C00A C00H 122.8(2) . . ? C00F C00A C008 118.5(2) . . ? C00F C00A H00A 114.7 . . ? C00F C00A C00H 60.64(17) . . ? C00H C00A H00A 114.7 . . ? C007 C00B H00B 119.9 . . ? C00G C00B C007 120.3(3) . . ? C00G C00B H00B 119.9 . . ? C007 C00C H00C 120.2 . . ? C00D C00C C007 119.7(2) . . ? C00D C00C H00C 120.2 . . ? C00C C00D H00D 119.8 . . ? C00C C00D C00I 120.4(2) . . ? C00I C00D H00D 119.8 . . ? F001 C00E C00F 112.6(2) . . ? F002 C00E F001 106.8(2) . . ? F002 C00E F003 107.0(2) . . ? F002 C00E C00F 112.0(2) . . ? F003 C00E F001 106.8(2) . . ? F003 C00E C00F 111.3(2) . . ? C00A C00F C00E 121.4(2) . . ? C00A C00F H00F 114.7 . . ? C00A C00F C00H 60.91(18) . . ? C00E C00F H00F 114.7 . . ? C00E C00F C00H 119.8(2) . . ? C00H C00F H00F 114.7 . . ? C00B C00G H00G 120.0 . . ? C00I C00G C00B 120.0(2) . . ? C00I C00G H00G 120.0 . . ? C009 C00H C00A 119.9(2) . . ? C009 C00H C00F 116.7(2) . . ? C009 C00H H00H 116.4 . . ? C00A C00H H00H 116.4 . . ? C00F C00H C00A 58.46(17) . . ? C00F C00H H00H 116.4 . . ? C00D C00I H00I 120.0 . . ? C00G C00I C00D 120.1(2) . . ? C00G C00I H00I 120.0 . . ? O005 C00J H00E 109.5 . . ? O005 C00J H00J 109.5 . . ? O005 C00J H00K 109.5 . . ? H00E C00J H00J 109.5 . . ? H00E C00J H00K 109.5 . . ? H00J C00J H00K 109.5 . . ? 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 F001 C00E C00F C00A 34.0(4) . . . . ? F001 C00E C00F C00H -38.1(4) . . . . ? F002 C00E C00F C00A 154.4(2) . . . . ? F002 C00E C00F C00H 82.3(3) . . . . ? F003 C00E C00F C00A -85.8(3) . . . . ? F003 C00E C00F C00H -157.9(2) . . . . ? O004 C008 C00A C00F -28.5(4) . . . . ? O004 C008 C00A C00H -100.2(3) . . . . ? O005 C009 C00H C00A -153.7(2) . . . . ? O005 C009 C00H C00F 139.0(2) . . . . ? O006 C009 C00H C00A 25.6(4) . . . . ? O006 C009 C00H C00F -41.6(4) . . . . ? C007 C008 C00A C00F 156.6(2) . . . . ? C007 C008 C00A C00H 84.9(3) . . . . ? C007 C00B C00G C00I -1.7(4) . . . . ? C007 C00C C00D C00I -1.8(4) . . . . ? C008 C007 C00B C00G 179.3(2) . . . . ? C008 C007 C00C C00D -177.6(3) . . . . ? C008 C00A C00F C00E 137.2(3) . . . . ? C008 C00A C00F C00H -113.7(3) . . . . ? C008 C00A C00H C009 2.1(3) . . . . ? C008 C00A C00H C00F 106.8(2) . . . . ? C00A C00F C00H C009 110.2(2) . . . . ? C00B C007 C008 O004 -13.5(4) . . . . ? C00B C007 C008 C00A 161.4(2) . . . . ? C00B C007 C00C C00D 1.3(4) . . . . ? C00B C00G C00I C00D 1.2(4) . . . . ? C00C C007 C008 O004 165.4(3) . . . . ? C00C C007 C008 C00A -19.7(4) . . . . ? C00C C007 C00B C00G 0.4(4) . . . . ? C00C C00D C00I C00G 0.6(4) . . . . ? C00E C00F C00H C009 -138.2(3) . . . . ? C00E C00F C00H C00A 111.6(3) . . . . ? C00F C00A C00H C009 -104.8(2) . . . . ? C00H C00A C00F C00E -109.1(3) . . . . ? C00J O005 C009 O006 4.4(4) . . . . ? C00J O005 C009 C00H -176.2(2) . . . . ? _shelx_res_file ; TITL exp_489_a.res in P2(1) exp_489.res created by SHELXL-2018/3 at 14:46:05 on 16-Apr-2021 REM Old TITL exp_489_a.res in P2(1) REM SHELXT solution in P2(1): R1 0.082, Rweak 0.027, Alpha 0.001 REM 0.700 for 5 systematic absences, Orientation as input REM Flack x = -0.005 ( 0.083 ) from 991 Parsons' quotients REM Formula found by SHELXT: C13 F3 O3 CELL 1.54184 5.1449 8.4717 13.8636 90 91.175 90 ZERR 2 0.0001 0.0002 0.0002 0 0.001 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H F O UNIT 26 22 6 6 L.S. 20 PLAN 20 TEMP -180 CONF BOND list 4 fmap 2 acta MORE -1 BOND $H REM REM REM WGHT 0.068000 0.070900 FVAR 1.25441 F001 3 1.083050 0.729609 0.514495 11.00000 0.02249 0.04849 = 0.02916 0.00806 0.00390 -0.00459 F002 3 0.799154 0.593781 0.433805 11.00000 0.04559 0.04854 = 0.02470 -0.00204 0.00285 -0.00976 F003 3 0.720458 0.836348 0.468792 11.00000 0.03426 0.04560 = 0.03827 0.02001 0.00287 0.00517 O004 4 0.378453 0.809105 0.734500 11.00000 0.01740 0.03669 = 0.03095 0.00076 -0.00089 0.00146 O005 4 0.832402 0.283640 0.710645 11.00000 0.03386 0.02636 = 0.03172 0.00277 0.00526 -0.00159 O006 4 0.476333 0.430801 0.738086 11.00000 0.02394 0.03574 = 0.03042 0.00423 0.00458 -0.00456 C007 1 0.670699 0.765148 0.865310 11.00000 0.01756 0.02632 = 0.02627 0.00075 0.00152 -0.00226 C008 1 0.591766 0.763127 0.761204 11.00000 0.01800 0.02558 = 0.02914 0.00235 0.00244 -0.00275 C009 1 0.694148 0.416859 0.707792 11.00000 0.02572 0.02690 = 0.01978 -0.00058 0.00004 -0.00063 C00A 1 0.792752 0.715337 0.688895 11.00000 0.01679 0.02567 = 0.02347 0.00281 0.00043 -0.00166 AFIX 13 H00A 2 0.947241 0.786719 0.686246 11.00000 -1.20000 AFIX 0 C00B 1 0.519133 0.851120 0.929266 11.00000 0.02034 0.02669 = 0.03175 0.00104 0.00217 -0.00151 AFIX 43 H00B 2 0.371013 0.907274 0.905825 11.00000 -1.20000 AFIX 0 C00C 1 0.888047 0.681652 0.900509 11.00000 0.01844 0.02979 = 0.02791 -0.00032 0.00263 0.00130 AFIX 43 H00C 2 0.994318 0.624658 0.857409 11.00000 -1.20000 AFIX 0 C00D 1 0.947144 0.682718 0.998727 11.00000 0.02038 0.03238 = 0.02908 0.00177 -0.00095 -0.00017 AFIX 43 H00D 2 1.091356 0.623755 1.022942 11.00000 -1.20000 AFIX 0 C00E 1 0.826266 0.702611 0.503091 11.00000 0.02272 0.03821 = 0.02513 0.00509 -0.00038 -0.00122 C00F 1 0.702567 0.653000 0.594168 11.00000 0.02013 0.03331 = 0.02389 0.00333 -0.00005 -0.00125 AFIX 13 H00F 2 0.511196 0.633375 0.588527 11.00000 -1.20000 AFIX 0 C00G 1 0.584230 0.854783 1.026990 11.00000 0.02545 0.03068 = 0.03046 -0.00413 0.00584 -0.00112 AFIX 43 H00G 2 0.483437 0.915626 1.069981 11.00000 -1.20000 AFIX 0 C00H 1 0.847208 0.544312 0.663431 11.00000 0.02031 0.02962 = 0.02134 0.00241 0.00264 -0.00149 AFIX 13 H00H 2 1.030558 0.517998 0.647036 11.00000 -1.20000 AFIX 0 C00I 1 0.796704 0.769469 1.061813 11.00000 0.02622 0.03500 = 0.02440 -0.00090 0.00080 -0.00612 AFIX 43 H00I 2 0.839260 0.770406 1.128815 11.00000 -1.20000 AFIX 0 C00J 1 0.701096 0.146030 0.746741 11.00000 0.04143 0.03093 = 0.04142 0.00632 0.00461 -0.00443 AFIX 137 H00E 2 0.553458 0.120106 0.703840 11.00000 -1.50000 H00J 2 0.638287 0.167648 0.811679 11.00000 -1.50000 H00K 2 0.822312 0.056821 0.749232 11.00000 -1.50000 AFIX 0 HKLF 4 REM exp_489_a.res in P2(1) REM wR2 = 0.1042, GooF = S = 1.113, Restrained GooF = 1.113 for all data REM R1 = 0.0374 for 2284 Fo > 4sig(Fo) and 0.0387 for all 2381 data REM 173 parameters refined using 1 restraints END WGHT 0.0681 0.0710 REM Highest difference peak 0.203, deepest hole -0.299, 1-sigma level 0.050 Q1 1 0.6372 0.7555 0.8170 11.00000 0.05 0.20 Q2 1 0.7242 0.6180 0.3587 11.00000 0.05 0.20 Q3 1 0.5509 0.8268 0.9777 11.00000 0.05 0.18 Q4 1 0.7234 0.7159 0.6370 11.00000 0.05 0.17 Q5 1 0.6241 0.8340 0.3945 11.00000 0.05 0.17 Q6 1 0.7898 0.8775 0.5522 11.00000 0.05 0.16 Q7 1 0.3015 0.7764 0.6581 11.00000 0.05 0.16 Q8 1 1.1049 0.5379 1.0388 11.00000 0.05 0.15 Q9 1 0.3983 0.8830 1.0851 11.00000 0.05 0.15 Q10 1 0.7970 0.6645 0.5514 11.00000 0.05 0.14 Q11 1 0.6711 0.8757 1.1168 11.00000 0.05 0.14 Q12 1 1.0274 0.7245 0.4371 11.00000 0.05 0.14 Q13 1 0.3078 0.9634 0.7027 11.00000 0.05 0.14 Q14 1 1.1888 0.5403 1.1204 11.00000 0.05 0.14 Q15 1 0.7399 0.4288 0.5390 11.00000 0.05 0.14 Q16 1 0.3537 1.0451 0.8713 11.00000 0.05 0.13 Q17 1 0.9733 0.4296 1.0416 11.00000 0.05 0.13 Q18 1 0.7866 0.1274 0.8201 11.00000 0.05 0.13 Q19 1 0.7180 0.7335 0.7141 11.00000 0.05 0.13 Q20 1 0.3592 0.7364 0.6810 11.00000 0.05 0.13 ; _shelx_res_checksum 7902 _shelx_hkl_file ; 0 -10 0 23.92 2.47 0 -10 1 101.72 5.17 0 -10 -1 92.28 4.89 0 -10 2 9.48 1.66 0 -10 -2 11.00 1.67 0 -10 2 14.40 2.04 0 -10 3 -0.66 1.00 0 -10 4 20.65 2.11 0 -10 4 14.90 1.83 0 -10 5 22.18 2.07 0 -10 5 21.28 1.96 0 -9 0 0.59 1.43 0 -9 0 -0.81 1.65 0 -9 -1 23.98 2.95 0 -9 1 27.10 3.32 0 -9 -1 29.28 3.44 0 -9 1 28.09 3.41 0 -9 2 19.92 2.94 0 -9 -2 24.47 3.01 0 -9 -3 23.11 2.96 0 -9 3 21.92 3.12 0 -9 4 63.24 5.09 0 -9 4 77.48 5.43 0 -9 -4 72.17 4.85 0 -9 5 0.43 1.52 0 -9 6 12.17 2.31 0 -9 7 17.05 2.28 0 -9 7 14.20 2.25 0 -9 8 6.50 1.57 0 -8 0 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220.53 11.39 0 -7 1 233.72 13.63 0 -7 -1 216.78 11.32 0 -7 1 215.33 11.13 0 -7 -1 191.17 10.28 0 -7 -1 220.93 11.16 0 -7 2 18.85 2.87 0 -7 2 19.63 4.07 0 -7 2 25.48 3.56 0 -7 -2 17.71 3.01 0 -7 2 20.79 3.54 0 -7 -2 18.40 2.87 0 -7 -3 168.60 9.20 0 -7 3 196.72 10.50 0 -7 3 158.42 9.05 0 -7 3 191.71 10.42 0 -7 3 172.76 11.69 0 -7 3 159.46 9.12 0 -7 3 166.88 9.97 0 -7 -3 182.05 9.86 0 -7 -3 194.53 11.87 0 -7 -4 530.12 24.11 0 -7 -4 528.07 21.85 0 -7 4 514.30 21.59 0 -7 4 494.01 22.34 0 -7 4 491.76 21.35 0 -7 -4 518.59 20.90 0 -7 4 488.60 23.96 0 -7 5 20.27 3.46 0 -7 5 21.73 3.60 0 -7 5 13.31 3.49 0 -7 5 14.74 2.94 0 -7 5 17.62 3.16 0 -7 -5 16.11 2.90 0 -7 5 19.80 3.51 0 -7 -5 12.95 3.41 0 -7 6 60.99 5.84 0 -7 6 50.57 5.94 0 -7 6 67.08 5.87 0 -7 -6 56.19 6.25 0 -7 -6 60.68 4.96 0 -7 6 72.13 6.14 0 -7 6 58.07 5.37 0 -7 6 56.17 5.30 0 -7 -7 13.81 2.39 0 -7 7 14.90 3.08 0 -7 7 11.33 2.90 0 -7 7 11.33 3.08 0 -7 7 12.36 3.12 0 -7 8 15.21 3.20 0 -7 8 21.68 3.47 0 -7 8 15.16 3.31 0 -7 8 17.71 3.39 0 -7 9 179.97 9.99 0 -7 9 178.07 9.85 0 -7 9 175.91 9.89 0 -7 9 171.64 9.72 0 -7 10 129.87 7.61 0 -7 10 120.00 7.62 0 -7 11 19.49 2.82 0 -6 0 34.78 3.74 0 -6 0 33.65 3.63 0 -6 0 37.49 4.72 0 -6 0 28.39 3.29 0 -6 1 50.92 4.18 0 -6 -1 57.68 4.48 0 -6 -1 60.44 4.78 0 -6 1 57.65 4.85 0 -6 1 65.47 5.04 0 -6 -1 57.01 4.76 0 -6 1 77.32 6.76 0 -6 -1 72.01 6.44 0 -6 2 857.63 33.73 0 -6 2 912.43 34.68 0 -6 2 902.33 34.70 0 -6 -2 911.52 34.42 0 -6 2 997.69 37.53 0 -6 -2 912.18 34.08 0 -6 2 943.19 34.83 0 -6 -3 5.42 1.91 0 -6 3 6.46 2.28 0 -6 -3 9.30 2.10 0 -6 3 5.45 2.16 0 -6 3 10.00 3.12 0 -6 3 10.12 2.38 0 -6 -3 7.83 2.83 0 -6 4 5.49 2.72 0 -6 4 5.58 2.17 0 -6 -4 3.09 1.60 0 -6 4 4.65 1.99 0 -6 -4 4.10 1.57 0 -6 -4 3.14 2.46 0 -6 4 4.42 2.27 0 -6 5 105.80 8.54 0 -6 5 105.55 7.42 0 -6 5 116.03 7.62 0 -6 5 105.58 7.29 0 -6 -5 134.27 8.99 0 -6 5 111.40 7.78 0 -6 -5 105.01 6.91 0 -6 -6 650.00 26.23 0 -6 6 706.86 27.72 0 -6 6 673.71 27.22 0 -6 6 725.25 27.63 0 -6 -6 663.21 28.51 0 -6 7 311.60 17.34 0 -6 7 373.94 17.10 0 -6 -7 372.76 15.90 0 -6 7 359.78 17.16 0 -6 7 362.02 17.49 0 -6 7 378.09 17.17 0 -6 -8 30.11 4.51 0 -6 8 24.07 3.95 0 -6 8 24.97 3.89 0 -6 -8 27.96 3.19 0 -6 9 36.94 4.63 0 -6 9 46.02 4.98 0 -6 -9 37.20 5.06 0 -6 9 40.73 4.76 0 -6 -10 157.09 9.88 0 -6 10 153.20 9.16 0 -6 10 144.45 9.12 0 -6 -11 67.05 6.05 0 -6 11 71.30 5.93 0 -6 11 70.19 5.72 0 -6 12 65.77 5.13 0 -6 -12 66.31 5.51 0 -6 12 61.31 5.26 0 -6 13 3.00 1.78 0 -6 -13 3.78 2.08 0 -6 -14 40.97 3.16 0 -6 14 45.15 3.23 0 -5 0 -0.52 1.19 0 -5 0 0.63 1.93 0 -5 0 0.27 1.29 0 -5 -1 5.56 2.41 0 -5 1 4.94 2.38 0 -5 1 5.26 1.67 0 -5 -1 4.49 1.56 0 -5 2 130.27 8.25 0 -5 -2 115.09 6.63 0 -5 2 109.75 6.61 0 -5 2 107.35 6.59 0 -5 2 121.33 6.82 0 -5 3 707.42 27.49 0 -5 -3 781.86 29.17 0 -5 3 727.96 27.28 0 -5 -3 708.21 27.16 0 -5 3 685.16 27.29 0 -5 3 698.08 29.26 0 -5 4 169.54 9.03 0 -5 4 167.18 8.92 0 -5 -4 183.59 10.14 0 -5 4 180.89 10.46 0 -5 4 161.78 9.02 0 -5 4 163.91 8.91 0 -5 -4 163.21 8.63 0 -5 5 60.29 5.03 0 -5 5 67.56 5.17 0 -5 -5 63.80 5.59 0 -5 5 59.99 4.89 0 -5 -5 54.15 4.45 0 -5 5 45.71 5.22 0 -5 -6 77.73 5.64 0 -5 6 84.00 6.32 0 -5 -6 84.88 6.68 0 -5 -6 97.93 6.17 0 -5 6 79.84 6.77 0 -5 6 88.68 6.39 0 -5 6 90.69 6.27 0 -5 6 88.73 6.29 0 -5 7 475.05 20.75 0 -5 7 505.03 20.45 0 -5 -7 493.53 19.77 0 -5 -7 495.05 19.59 0 -5 7 471.85 20.43 0 -5 -8 381.42 15.68 0 -5 8 367.12 16.62 0 -5 8 290.65 16.10 0 -5 8 365.58 16.12 0 -5 -8 361.10 15.18 0 -5 8 303.50 15.68 0 -5 9 658.67 26.94 0 -5 9 597.76 26.34 0 -5 9 660.45 27.16 0 -5 10 74.93 6.27 0 -5 10 84.52 6.77 0 -5 11 51.23 5.38 0 -5 11 50.42 5.20 0 -5 -11 54.56 6.01 0 -5 -12 38.35 5.10 0 -5 12 33.35 4.29 0 -5 12 30.40 3.97 0 -5 -13 94.28 7.06 0 -5 13 100.24 6.69 0 -5 14 10.37 2.20 0 -5 -14 6.07 2.28 0 -5 -15 1.38 1.44 0 -4 0 26.89 3.25 0 -4 1 40.14 4.20 0 -4 2 314.66 14.31 0 -4 3 31.37 3.83 0 -4 -3 39.47 3.83 0 -4 -4 38.87 3.98 0 -4 4 36.70 4.00 0 -4 4 33.56 2.16 0 -4 -5 468.75 19.71 0 -4 5 505.71 19.72 0 -4 5 455.93 18.00 0 -4 -5 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279.36 13.59 0 2 -12 232.29 15.71 0 2 -12 267.10 13.12 0 2 -12 263.93 13.84 0 2 -12 279.83 14.00 0 2 -12 274.41 14.87 0 2 -12 232.44 13.35 0 2 -12 262.29 14.21 0 2 -13 79.28 6.02 0 2 -13 75.75 6.88 0 2 -13 46.71 5.20 0 2 -13 73.06 6.29 0 2 -13 72.34 7.99 0 2 -13 79.52 5.87 0 2 -13 59.18 5.38 0 2 -13 70.72 6.25 0 2 -13 60.87 6.04 0 2 -14 10.06 2.40 0 2 -14 9.82 2.53 0 2 -14 8.83 2.99 0 2 -14 9.17 2.76 0 2 -14 6.73 2.60 0 2 -14 9.40 2.87 0 2 -14 7.89 3.49 0 2 -15 37.55 5.10 0 2 -15 36.40 3.43 0 2 -15 41.91 4.23 0 2 -15 34.92 4.08 0 2 -15 37.94 4.14 0 2 -15 30.86 3.44 0 2 -16 52.28 4.05 0 2 -16 53.65 5.28 0 2 -16 73.20 4.81 0 2 -16 64.40 4.18 0 2 -16 68.00 4.65 0 3 0 0.23 0.48 0 3 -1 1907.89 59.81 0 3 1 1707.53 58.21 0 3 -1 1990.85 61.17 0 3 -1 1677.71 58.90 0 3 2 123.54 4.84 0 3 -2 137.63 5.75 0 3 -2 141.52 5.91 0 3 -2 147.52 7.65 0 3 -3 1653.55 56.35 0 3 3 1520.92 52.57 0 3 -3 1643.12 53.41 0 3 -3 1516.42 53.05 0 3 4 377.88 14.18 0 3 -4 360.60 14.20 0 3 -4 413.24 14.95 0 3 -4 404.06 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625.71 25.89 0 3 -11 569.15 29.58 0 3 -11 598.04 26.22 0 3 -12 59.55 5.03 0 3 -12 47.42 7.13 0 3 -12 63.37 5.97 0 3 -12 64.46 6.84 0 3 -12 57.87 6.31 0 3 -12 49.86 5.70 0 3 -12 57.19 5.87 0 3 -12 65.89 6.77 0 3 -12 66.95 5.45 0 3 12 49.71 5.35 0 3 -12 44.61 5.67 0 3 -12 56.29 6.92 0 3 -12 63.59 5.80 0 3 -13 65.97 6.71 0 3 -13 44.38 5.23 0 3 -13 48.51 6.47 0 3 -13 52.44 5.11 0 3 -13 50.70 4.52 0 3 -13 55.21 4.88 0 3 -13 42.12 5.04 0 3 -13 57.13 5.36 0 3 -13 53.15 5.68 0 3 -13 58.43 6.18 0 3 -13 64.93 5.78 0 3 -14 14.40 3.61 0 3 -14 13.68 3.70 0 3 -14 12.21 2.94 0 3 -14 15.28 3.02 0 3 -14 14.99 3.32 0 3 -14 14.71 2.71 0 3 -14 16.01 3.04 0 3 -15 19.59 3.32 0 3 -15 19.73 2.96 0 3 -15 16.11 2.37 0 3 -15 23.22 3.08 0 3 -15 16.93 2.98 0 3 -15 18.43 3.28 0 3 -16 51.11 3.62 0 3 -16 61.20 4.37 0 3 -16 33.05 3.33 0 3 -16 41.40 3.24 0 3 -16 59.12 3.86 0 4 0 21.83 1.53 0 4 0 24.09 2.47 0 4 -1 35.40 2.47 0 4 -1 44.31 3.22 0 4 -2 341.19 15.30 0 4 -2 321.38 12.29 0 4 -2 306.98 12.61 0 4 -3 34.56 2.72 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98.38 8.09 0 4 -12 106.12 7.51 0 4 -12 83.59 7.94 0 4 -12 96.18 7.49 0 4 -12 73.05 7.30 0 4 -13 5.39 2.41 0 4 -13 6.27 2.93 0 4 -13 3.57 2.83 0 4 -13 9.57 3.39 0 4 -13 4.59 1.83 0 4 -13 6.15 2.59 0 4 -13 4.98 2.70 0 4 -13 5.60 2.30 0 4 -13 5.95 2.33 0 4 -14 9.94 2.25 0 4 -14 10.32 2.40 0 4 -14 7.62 2.43 0 4 -14 10.36 2.87 0 4 -14 7.39 1.82 0 4 -14 13.40 3.22 0 4 -15 31.42 3.56 0 4 -15 18.60 2.27 0 4 -15 28.54 3.24 0 4 -15 20.83 2.58 0 4 -15 27.11 2.85 0 5 0 0.14 1.04 0 5 0 -0.56 1.72 0 5 -1 6.06 2.43 0 5 1 6.63 2.18 0 5 1 3.04 1.45 0 5 -1 6.84 1.72 0 5 -2 96.27 5.09 0 5 -2 107.54 8.10 0 5 -2 107.60 5.77 0 5 -3 749.51 29.41 0 5 -3 613.15 23.79 0 5 -4 166.70 8.30 0 5 -4 168.97 11.96 0 5 4 169.25 8.35 0 5 -5 56.71 4.46 0 5 -5 53.92 7.36 0 5 -5 47.10 4.63 0 5 -6 88.91 6.58 0 5 -6 86.11 7.73 0 5 -6 85.97 6.27 0 5 -6 78.14 6.41 0 5 -6 88.31 6.16 0 5 -6 82.86 9.50 0 5 -7 532.72 20.96 0 5 -7 470.66 21.16 0 5 -7 515.85 22.49 0 5 -7 478.33 23.18 0 5 -7 483.68 20.98 0 5 -7 451.49 26.44 0 5 -7 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3 -11 44.53 5.64 2 3 -11 34.94 5.85 -2 3 11 40.22 4.43 2 3 -11 47.61 5.24 2 3 -10 122.68 7.69 2 3 -10 124.65 10.27 2 3 -10 118.78 9.09 2 3 -10 102.96 9.09 2 3 -10 116.78 7.70 2 3 -10 81.79 10.23 2 3 -10 89.66 9.70 2 3 -10 114.93 9.16 2 3 -10 110.61 10.08 -2 3 10 97.94 7.93 -2 3 10 127.97 8.05 2 3 -10 145.48 9.21 -2 3 9 152.56 10.02 2 3 -9 176.63 9.70 2 3 -9 168.37 12.06 2 3 -9 167.24 11.08 2 3 -9 152.54 10.91 2 3 -9 183.70 10.38 2 3 -9 177.20 9.85 2 3 -9 147.51 13.04 2 3 -9 145.20 11.47 2 3 -9 141.21 11.80 2 3 -9 175.90 10.67 2 3 -8 11.40 3.19 2 3 -8 9.36 2.84 2 3 -8 13.11 3.41 2 3 -8 9.67 3.21 2 3 -8 11.23 2.71 2 3 -8 6.84 3.15 2 3 -8 13.98 4.42 2 3 -8 11.12 2.70 2 3 -8 10.89 2.71 2 3 -8 13.08 4.35 2 3 -8 12.60 3.52 -2 3 8 9.15 2.63 2 3 -8 9.33 3.56 2 3 -7 57.98 5.14 -2 3 7 65.21 5.69 2 3 -7 68.89 5.54 2 3 -7 57.88 5.73 2 3 -7 58.12 5.76 2 3 -7 68.71 5.84 2 3 -7 66.65 7.39 2 3 -7 56.05 5.90 2 3 -7 48.13 6.23 2 3 -7 53.62 5.94 2 3 -7 56.83 5.52 2 3 -7 58.58 5.75 2 3 -6 125.03 8.63 2 3 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5.69 3.24 2 7 -9 4.68 2.58 2 7 -9 1.84 2.06 2 7 -9 4.12 2.24 2 7 -8 172.47 11.58 2 7 -8 187.91 10.54 2 7 -8 176.53 11.06 2 7 -8 182.62 10.54 2 7 -8 153.10 8.92 2 7 -7 97.63 8.86 2 7 -7 101.23 7.86 2 7 -7 98.02 7.91 2 7 -7 96.11 8.52 2 7 -7 92.47 6.83 2 7 -6 26.10 4.63 2 7 -6 25.36 3.99 2 7 -6 25.97 4.55 2 7 -5 23.57 4.10 2 7 -5 21.48 4.60 2 7 -4 28.17 4.48 2 7 -4 16.26 4.01 2 7 -4 23.71 3.49 2 7 -4 23.49 5.64 2 7 -3 74.40 8.87 2 7 -3 62.20 5.63 2 7 -3 53.12 6.57 2 7 -2 122.51 8.64 2 7 -2 137.28 11.64 2 7 -1 20.91 4.53 2 7 -1 29.49 4.31 2 7 -1 35.41 6.07 2 7 0 160.10 10.60 2 7 0 127.07 10.17 2 7 1 55.65 6.11 2 7 1 46.41 5.83 2 7 2 10.74 3.25 2 7 2 10.77 3.33 2 7 3 67.63 7.21 2 7 4 217.82 13.92 -2 7 -5 36.27 4.70 -2 7 -6 -0.71 2.19 -2 7 -7 1.37 2.51 -2 7 -7 0.46 2.12 -2 7 -7 -0.87 2.74 -2 7 -8 76.29 6.84 -2 7 -8 74.21 6.13 -2 7 -8 73.16 6.91 -2 7 -9 85.49 6.60 -2 7 -9 73.45 6.29 -2 7 -9 76.11 5.80 -2 7 -10 1.98 1.70 -2 7 -10 2.96 1.97 -2 7 -10 1.93 1.90 -2 7 -10 1.66 1.87 -2 7 -11 32.51 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4 7 165.60 12.31 -3 4 -7 233.01 13.14 -3 4 -8 231.89 12.58 -3 4 -8 272.17 14.99 -3 4 -8 201.55 11.85 3 4 8 269.95 14.40 -3 4 -8 275.89 14.01 3 4 8 202.95 13.66 -3 4 -8 250.43 13.97 -3 4 -9 22.48 3.78 -3 4 -9 24.71 4.76 3 4 9 25.20 4.35 -3 4 -9 27.22 4.36 -3 4 -9 26.31 4.45 -3 4 -10 128.26 8.43 -3 4 -10 141.01 9.59 -3 4 -10 132.43 8.87 -3 4 -10 142.83 9.22 -3 4 -11 33.48 3.97 -3 4 -11 32.27 4.37 -3 4 -11 32.51 4.14 -3 4 -11 32.08 4.18 -3 4 -12 69.78 5.11 -3 4 -12 77.71 5.80 -3 4 -12 71.16 5.35 -3 4 -12 77.91 5.55 -3 4 -13 2.29 1.17 -3 4 -13 6.06 1.74 -3 4 -13 6.56 1.67 -3 4 -13 3.65 1.55 3 4 13 3.44 1.33 3 5 -13 59.47 3.77 3 5 -12 0.91 1.38 3 5 -12 1.58 1.88 3 5 -12 1.18 1.42 3 5 -12 1.67 1.73 3 5 -11 153.17 8.21 3 5 -11 126.31 6.73 3 5 -11 139.48 9.13 3 5 -11 145.49 8.25 3 5 -11 154.48 8.77 3 5 -10 8.72 2.71 3 5 -10 7.10 1.97 3 5 -10 4.01 3.28 3 5 -10 7.75 2.82 3 5 -10 10.65 2.09 3 5 -10 5.23 2.85 3 5 -9 35.24 3.95 3 5 -9 26.99 5.41 3 5 -9 30.77 4.75 3 5 -9 28.10 4.58 3 5 -9 29.54 3.63 3 5 -9 29.83 4.95 3 5 -9 38.84 4.79 3 5 -8 17.48 4.08 3 5 -8 12.56 2.89 3 5 -8 12.98 4.65 3 5 -8 12.73 3.86 3 5 -8 10.99 3.33 3 5 -8 14.19 2.90 3 5 -8 14.44 4.17 3 5 -7 175.54 10.28 3 5 -7 154.41 11.23 3 5 -7 178.89 11.49 3 5 -7 165.15 9.99 3 5 -7 175.58 11.33 3 5 -6 363.62 17.30 3 5 -6 346.25 18.25 3 5 -6 385.53 17.47 3 5 -6 358.18 18.12 3 5 -6 353.03 21.29 3 5 -6 385.24 18.76 3 5 -5 113.78 8.45 3 5 -5 119.87 8.50 3 5 -5 121.51 9.27 3 5 -5 128.18 11.26 3 5 -5 96.69 9.52 3 5 -5 119.97 9.36 3 5 -4 72.64 6.89 3 5 -4 67.77 6.94 3 5 -4 78.83 6.82 3 5 -4 75.66 8.58 3 5 -4 68.47 7.85 3 5 -3 30.91 4.79 -3 5 3 37.37 4.17 3 5 -3 36.11 5.06 3 5 -3 41.91 5.23 -3 5 2 626.88 23.19 3 5 -2 587.62 25.38 3 5 -2 501.14 23.87 3 5 -2 503.24 22.57 3 5 -2 504.33 25.80 -3 5 1 748.76 28.01 3 5 -1 686.13 30.20 3 5 -1 667.88 28.33 3 5 -1 675.38 31.26 -3 5 0 95.26 6.54 3 5 0 92.48 8.09 3 5 0 89.51 7.08 3 5 0 89.22 8.58 3 5 1 71.08 7.06 3 5 1 60.60 6.11 3 5 1 57.63 7.10 3 5 2 18.61 4.46 -3 5 -2 31.30 3.82 3 5 3 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2.23 4 3 -6 4.89 3.02 4 3 -6 0.30 1.73 -4 3 6 2.68 2.02 4 3 -6 2.30 3.02 4 3 -6 0.58 1.81 -4 3 5 264.69 14.03 4 3 -5 260.66 13.19 4 3 -5 246.54 13.99 4 3 -5 238.70 13.81 4 3 -5 243.86 15.36 4 3 -5 244.48 14.19 4 3 -5 213.35 14.83 4 3 -5 244.72 12.70 4 3 -5 249.27 13.94 4 3 -4 84.84 7.11 -4 3 4 74.98 6.70 4 3 -4 75.69 6.55 4 3 -4 72.28 7.08 4 3 -4 90.25 7.91 4 3 -4 73.06 6.78 4 3 -4 75.76 7.90 4 3 -4 70.64 8.12 4 3 -4 74.88 6.32 4 3 -4 83.56 7.38 4 3 -3 511.64 23.06 -4 3 3 482.48 22.29 4 3 -3 525.94 22.45 4 3 -3 501.06 22.01 4 3 -3 515.24 23.92 4 3 -3 555.59 23.24 4 3 -3 484.33 22.20 4 3 -3 478.20 23.01 4 3 -2 241.11 13.34 -4 3 2 246.16 12.89 4 3 -2 217.98 12.27 4 3 -2 233.61 12.87 4 3 -2 227.17 13.60 4 3 -2 204.94 14.32 4 3 -2 221.73 12.67 -4 3 1 147.43 9.08 4 3 -1 145.69 9.64 4 3 -1 129.39 8.71 4 3 -1 134.03 8.96 4 3 -1 134.86 9.86 4 3 -1 122.75 10.71 4 3 -1 129.38 9.21 -4 3 0 64.61 5.63 4 3 0 58.59 6.00 -4 3 0 62.33 5.43 4 3 0 51.96 5.34 -4 3 0 55.59 5.44 4 3 0 55.52 5.47 4 3 0 48.00 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8.78 4 4 -4 116.94 8.49 4 4 -4 127.03 9.19 4 4 -4 124.98 10.68 4 4 -4 111.86 10.24 4 4 -4 111.05 7.56 4 4 -4 115.83 9.01 4 4 -3 168.80 10.95 4 4 -3 165.00 9.84 4 4 -3 151.43 10.73 -4 4 2 630.60 26.31 4 4 -2 698.94 28.50 4 4 -2 648.84 28.45 4 4 -2 634.82 26.68 4 4 -1 85.35 7.38 -4 4 1 83.34 6.51 4 4 -1 85.26 7.74 4 4 -1 82.04 7.72 4 4 -1 69.09 8.35 4 4 -1 71.81 6.61 4 4 0 206.75 12.74 -4 4 0 239.52 12.25 4 4 0 217.38 13.56 4 4 0 212.95 13.24 4 4 0 215.95 14.54 4 4 0 223.18 12.89 -4 4 -1 315.04 15.24 4 4 1 320.54 17.24 4 4 1 297.10 17.77 4 4 1 324.62 16.71 4 4 2 316.28 15.49 -4 4 -2 345.52 15.80 4 4 2 321.35 17.64 4 4 2 284.29 17.51 4 4 2 364.39 17.80 -4 4 -3 334.66 15.20 4 4 3 307.40 15.09 4 4 3 335.81 17.56 4 4 3 313.21 16.95 -4 4 -4 33.10 4.09 4 4 4 31.95 4.18 4 4 4 27.89 4.64 4 4 4 35.39 5.37 4 4 5 118.39 8.07 -4 4 -5 103.85 7.12 4 4 5 106.18 9.01 -4 4 -6 0.40 1.80 4 4 6 0.23 1.84 -4 4 -7 218.25 11.73 -4 4 -7 229.17 11.46 -4 4 -8 8.45 2.48 -4 4 -8 9.99 2.45 4 4 8 9.66 3.08 -4 4 -9 5.80 2.26 -4 4 -9 4.58 1.93 4 4 9 3.17 2.22 -4 4 -10 25.31 3.15 -4 4 -10 23.47 2.87 4 4 10 24.55 3.26 -4 4 -11 16.17 2.15 -4 4 -11 14.05 1.92 4 4 11 9.12 1.80 4 5 -10 57.32 4.07 4 5 -10 57.59 3.56 4 5 -10 37.26 3.67 4 5 -10 45.40 3.41 4 5 -10 50.06 3.96 4 5 -9 42.32 3.60 4 5 -9 35.79 4.37 4 5 -9 36.98 3.50 4 5 -9 37.96 3.35 4 5 -9 45.40 4.36 4 5 -9 45.12 4.11 4 5 -8 9.82 2.28 4 5 -8 8.08 2.93 4 5 -8 12.32 2.60 4 5 -8 10.98 2.32 4 5 -8 11.41 2.99 4 5 -7 16.65 3.01 4 5 -7 11.44 3.77 4 5 -7 13.51 2.91 4 5 -7 10.71 2.81 4 5 -7 15.67 2.91 4 5 -7 16.26 3.68 4 5 -6 128.26 8.01 4 5 -6 92.20 7.31 4 5 -6 111.20 7.74 4 5 -6 111.80 7.65 4 5 -6 110.13 8.49 4 5 -5 161.99 9.71 4 5 -5 132.69 9.30 4 5 -5 140.68 9.26 4 5 -5 149.02 9.45 4 5 -5 152.11 10.41 4 5 -4 14.85 4.01 4 5 -4 18.08 3.76 4 5 -4 11.00 3.29 4 5 -4 11.16 3.33 4 5 -3 9.03 3.38 4 5 -3 14.95 3.68 4 5 -3 13.14 3.53 4 5 -3 10.68 2.44 4 5 -2 74.96 6.89 4 5 -2 78.06 7.04 4 5 -2 66.19 5.68 4 5 -1 293.03 15.36 4 5 -1 265.60 13.88 4 5 0 185.43 11.71 4 5 0 171.00 10.62 4 5 1 144.54 10.17 4 5 1 127.36 9.13 4 5 2 36.54 4.99 4 5 3 -1.41 2.63 4 5 4 110.90 8.76 4 5 5 281.29 15.37 4 5 6 77.96 7.06 4 5 7 15.19 3.36 -4 5 -8 2.05 1.47 -4 5 -9 78.33 4.74 -4 5 -9 68.68 4.40 4 5 10 26.16 2.90 4 6 -9 13.12 2.31 4 6 -9 14.52 1.86 4 6 -9 17.13 2.30 4 6 -9 14.17 2.03 4 6 -8 5.45 1.87 4 6 -8 3.59 1.39 4 6 -8 4.37 2.23 4 6 -8 3.41 1.59 4 6 -8 7.43 2.27 4 6 -7 40.33 3.62 4 6 -7 40.22 4.97 4 6 -7 37.85 3.79 4 6 -7 39.13 3.83 4 6 -7 38.18 3.32 4 6 -7 43.40 4.54 4 6 -7 46.26 4.30 4 6 -6 97.29 6.02 4 6 -6 79.06 5.98 4 6 -6 90.12 5.75 4 6 -6 87.51 6.88 4 6 -6 91.58 6.59 4 6 -5 3.43 2.50 4 6 -5 1.60 1.89 4 6 -5 2.48 2.23 4 6 -5 0.39 2.06 4 6 -5 3.53 2.04 4 6 -5 3.40 2.74 4 6 -4 3.19 2.31 4 6 -4 1.50 2.27 4 6 -4 2.29 2.02 4 6 -4 3.90 2.85 4 6 -3 63.60 5.68 4 6 -3 55.88 5.69 4 6 -3 59.65 5.50 4 6 -2 24.01 3.94 4 6 -2 18.72 3.54 4 6 -1 21.11 3.80 4 6 -1 23.28 4.00 4 6 -1 15.53 2.59 4 6 0 3.43 2.63 4 6 0 2.45 2.42 4 6 0 3.30 1.89 4 6 1 50.27 5.61 4 6 1 55.67 5.14 4 6 2 99.02 7.83 4 6 2 99.01 7.23 4 6 3 22.49 4.17 4 6 3 27.21 3.93 4 6 4 10.00 2.95 4 6 5 9.75 2.98 4 6 6 22.73 3.58 4 6 7 19.87 3.24 4 6 8 5.66 1.92 4 6 9 4.06 1.48 4 7 -7 4.16 1.39 4 7 -7 4.12 1.84 4 7 -6 78.88 4.46 4 7 -6 67.30 4.74 4 7 -6 84.35 5.09 4 7 -5 9.99 2.33 4 7 -5 7.94 1.80 4 7 -5 5.27 1.90 4 7 -5 9.64 2.23 4 7 -4 73.35 4.95 4 7 -4 75.96 5.41 4 7 -4 68.90 4.49 4 7 -4 81.25 5.76 4 7 -3 7.36 2.56 4 7 -3 6.87 2.14 4 7 -3 5.35 2.24 4 7 -3 6.39 1.81 4 7 -2 141.66 7.93 4 7 -2 114.70 7.67 4 7 -2 123.33 7.27 4 7 -2 128.54 8.24 4 7 -1 1.65 2.19 4 7 -1 2.19 1.98 4 7 -1 -0.17 1.66 4 7 0 100.04 6.87 4 7 0 85.17 6.24 4 7 1 117.52 7.59 4 7 1 106.16 7.19 4 7 2 49.97 4.88 4 7 2 42.18 4.38 4 7 2 34.37 3.33 4 7 3 8.72 2.47 4 7 3 7.23 1.89 4 7 4 74.42 5.64 4 7 4 61.67 4.75 4 7 5 46.00 4.41 4 7 5 43.24 3.83 4 7 6 10.81 2.23 4 7 6 15.45 2.52 4 7 6 12.66 2.10 4 8 -3 10.60 2.16 4 8 -3 12.63 2.05 4 8 -2 6.50 1.84 4 8 -2 6.80 1.75 4 8 -2 8.93 2.27 4 8 -1 10.27 2.17 4 8 -1 7.56 1.71 4 8 -1 7.55 1.93 4 8 -1 6.77 2.21 4 8 0 18.92 2.45 4 8 0 18.74 2.61 4 8 0 26.35 3.13 4 8 1 8.92 2.23 4 8 1 8.96 1.96 4 8 2 0.66 1.46 4 8 2 3.24 1.59 4 8 3 10.86 2.18 4 8 3 12.99 2.09 -5 -6 5 20.93 2.06 -5 -6 4 30.20 2.73 -5 -6 3 5.23 1.61 -5 -6 3 3.73 1.11 -5 -6 2 10.31 1.99 -5 -6 2 10.36 1.70 -5 -6 1 17.55 2.44 -5 -6 1 13.30 1.95 -5 -6 0 19.36 2.31 -5 -6 -1 15.82 2.15 -5 -6 -1 13.24 1.70 -5 -6 -2 27.70 2.62 -5 -6 -2 22.21 2.23 -5 -6 -3 9.70 1.51 -5 -6 -4 2.32 0.95 -5 -5 7 29.54 2.50 -5 -5 6 134.11 6.87 -5 -5 5 43.93 3.75 -5 -5 4 49.05 4.16 -5 -5 4 33.75 2.88 -5 -5 3 14.83 2.12 -5 -5 3 15.03 2.64 -5 -5 2 76.48 5.57 -5 -5 2 65.52 4.71 -5 -5 1 25.23 3.30 -5 -5 1 19.58 2.72 -5 -5 0 67.34 5.11 -5 -5 0 58.34 4.44 -5 -5 -1 82.80 5.53 -5 -5 -1 73.19 4.92 -5 -5 -2 75.28 5.17 -5 -5 -2 66.84 4.66 -5 -5 -3 3.57 1.50 -5 -5 -4 21.02 2.57 -5 -5 -5 16.16 2.24 -5 -5 -6 1.32 0.99 -5 -5 -6 1.76 1.08 -5 -4 8 27.85 2.33 -5 -4 7 8.62 1.89 -5 -4 6 134.29 7.52 5 -4 -6 139.92 6.91 -5 -4 5 26.96 3.37 5 -4 -5 24.91 2.60 -5 -4 4 14.88 2.08 -5 -4 4 17.46 3.05 -5 -4 3 11.37 2.72 -5 -4 3 9.44 1.94 -5 -4 2 87.21 6.43 -5 -4 2 78.35 5.48 -5 -4 1 8.18 2.68 -5 -4 1 7.09 2.14 -5 -4 0 241.57 11.90 -5 -4 0 200.88 9.90 -5 -4 -1 11.00 2.75 -5 -4 -1 10.96 2.20 -5 -4 -2 87.57 5.83 -5 -4 -3 86.75 5.83 -5 -4 -4 29.66 2.93 -5 -4 -4 41.85 3.84 -5 -4 -5 51.56 3.94 -5 -4 -5 65.68 4.74 -5 -4 -6 144.67 7.57 -5 -4 -6 185.98 8.56 -5 -4 -7 106.81 5.80 -5 -4 -7 130.69 6.48 -5 -4 -8 9.26 1.57 -5 -3 8 20.87 2.13 5 -3 -8 26.83 3.31 5 -3 -8 27.86 2.73 -5 -3 7 3.42 1.46 5 -3 -7 4.17 1.99 5 -3 -7 5.17 1.74 -5 -3 6 18.45 2.78 5 -3 -6 27.34 3.82 5 -3 -6 26.74 3.08 -5 -3 5 57.40 5.06 -5 -3 5 68.76 5.37 5 -3 -5 74.37 6.25 5 -3 -5 70.55 5.15 -5 -3 4 188.19 10.70 -5 -3 4 224.59 11.05 5 -3 -4 210.75 10.45 -5 -3 3 141.46 8.69 -5 -3 3 156.40 8.57 5 -3 -3 137.15 7.83 -5 -3 2 31.81 3.48 -5 -3 2 34.91 4.27 -5 -3 2 28.79 3.71 5 -3 -2 35.45 4.26 5 -3 -2 36.66 3.60 -5 -3 1 14.60 3.11 5 -3 -1 11.48 2.76 -5 -3 1 15.36 2.83 5 -3 -1 12.60 2.24 -5 -3 0 24.59 3.42 -5 -3 0 30.45 4.01 5 -3 0 25.67 3.71 -5 -3 0 21.67 2.78 -5 -3 -1 5.63 2.46 5 -3 1 4.04 2.16 -5 -3 -1 6.69 2.20 -5 -3 -1 4.32 1.81 5 -3 2 105.53 7.41 -5 -3 -2 103.88 6.86 5 -3 3 77.02 6.27 -5 -3 -3 87.97 6.07 -5 -3 -4 46.85 4.46 5 -3 4 37.21 4.27 -5 -3 -4 32.62 3.43 -5 -3 -4 42.89 4.15 5 -3 5 39.71 4.16 -5 -3 -5 32.34 3.50 -5 -3 -5 41.10 4.13 -5 -3 -6 89.37 5.91 5 -3 6 78.01 5.53 -5 -3 -6 64.58 4.85 -5 -3 -6 79.05 5.37 -5 -3 -6 63.20 4.56 5 -3 7 59.88 4.47 -5 -3 -7 58.46 4.31 -5 -3 -7 49.54 3.83 -5 -3 -8 39.85 3.47 -5 -3 -8 33.25 3.02 -5 -3 -9 26.64 2.33 5 -2 -10 4.01 1.68 5 -2 -9 40.07 4.29 5 -2 -9 41.69 3.40 5 -2 -8 25.09 3.77 5 -2 -7 9.83 2.90 5 -2 -7 7.12 2.15 -5 -2 6 1.57 1.42 5 -2 -6 1.81 2.35 5 -2 -6 2.60 1.85 -5 -2 5 8.90 2.16 5 -2 -5 12.90 2.63 -5 -2 4 136.68 8.49 5 -2 -4 185.95 9.59 -5 -2 3 36.96 4.20 5 -2 -3 39.59 4.71 5 -2 -3 49.28 4.58 -5 -2 2 290.08 14.71 -5 -2 2 314.30 15.42 5 -2 -2 333.62 16.18 5 -2 -2 337.04 15.10 -5 -2 1 61.19 5.56 -5 -2 1 74.36 6.12 5 -2 -1 74.17 6.51 5 -2 -1 75.10 5.70 -5 -2 0 15.32 3.14 5 -2 0 18.78 3.50 -5 -2 0 17.58 3.15 5 -2 0 17.11 2.85 -5 -2 -1 36.75 4.32 -5 -2 -1 37.80 4.21 5 -2 1 32.98 4.38 5 -2 1 32.04 3.67 -5 -2 -2 92.64 6.66 -5 -2 -2 81.40 5.95 5 -2 2 95.77 7.54 5 -2 2 82.63 5.67 -5 -2 -3 234.46 12.05 5 -2 3 248.14 13.64 -5 -2 -3 263.16 12.77 -5 -2 -4 29.34 3.71 5 -2 4 26.28 4.14 -5 -2 -4 29.81 3.86 -5 -2 -5 76.71 5.94 5 -2 5 66.10 6.24 -5 -2 -5 70.15 5.66 -5 -2 -6 86.77 6.33 5 -2 6 89.32 6.98 -5 -2 -6 90.75 6.38 -5 -2 -7 9.59 2.39 -5 -2 -7 8.99 2.33 5 -2 7 5.92 2.23 -5 -2 -7 6.18 1.68 -5 -2 -8 114.68 6.44 5 -2 8 112.83 6.78 -5 -2 -8 97.61 6.29 -5 -2 -9 16.80 2.35 -5 -2 -9 14.44 2.29 5 -2 9 16.97 2.36 -5 -2 -9 16.48 2.14 -5 -2 -9 11.68 1.72 -5 -2 -10 6.43 1.32 5 -1 -10 2.80 1.89 5 -1 -10 2.26 1.25 5 -1 -9 30.39 4.11 5 -1 -9 27.36 2.72 5 -1 -9 33.70 3.18 5 -1 -8 6.16 2.61 5 -1 -8 5.09 1.71 5 -1 -8 4.65 1.91 5 -1 -7 98.37 7.75 5 -1 -7 82.17 5.56 5 -1 -7 88.08 6.18 5 -1 -6 64.08 6.37 5 -1 -6 36.66 3.81 5 -1 -5 121.18 7.27 5 -1 -4 156.10 8.71 5 -1 -4 168.64 9.75 5 -1 -3 1194.78 44.73 5 -1 -3 1105.64 43.19 5 -1 -2 15.99 3.36 -5 -1 2 15.75 3.50 5 -1 -2 13.72 2.97 -5 -1 1 71.73 5.61 -5 -1 1 78.06 6.68 5 -1 -1 83.30 7.14 5 -1 -1 80.89 6.42 -5 -1 0 153.96 8.87 -5 -1 0 154.63 9.74 5 -1 0 154.51 10.36 5 -1 0 155.74 9.51 -5 -1 -1 70.48 6.15 5 -1 1 85.50 7.35 5 -1 1 72.63 6.06 -5 -1 -2 230.01 11.96 5 -1 2 212.09 12.91 5 -1 2 198.80 11.12 -5 -1 -3 87.84 6.19 5 -1 3 95.41 8.10 5 -1 3 83.72 6.24 -5 -1 -3 105.29 7.30 -5 -1 -4 82.24 5.98 5 -1 4 83.63 7.34 -5 -1 -4 87.58 6.55 -5 -1 -5 18.33 3.14 -5 -1 -5 20.46 3.57 5 -1 5 23.37 4.24 -5 -1 -6 135.77 8.37 5 -1 6 128.03 9.32 -5 -1 -6 150.59 8.79 -5 -1 -7 67.58 5.37 5 -1 7 66.55 6.14 -5 -1 -7 61.19 5.38 -5 -1 -8 14.92 2.61 -5 -1 -8 14.07 2.78 5 -1 8 13.73 2.92 -5 -1 -8 10.51 2.00 -5 -1 -9 30.68 3.09 5 -1 9 26.26 3.26 -5 -1 -9 23.48 3.12 -5 -1 -10 17.34 2.10 -5 -1 -10 10.74 2.05 5 -1 10 17.51 2.30 5 0 -11 46.73 4.06 5 0 -10 23.80 2.40 5 0 -10 18.82 3.26 5 0 -10 21.25 2.34 5 0 -10 20.51 2.21 5 0 -9 5.24 1.67 5 0 -9 6.51 2.64 5 0 -9 3.51 1.68 5 0 -9 4.55 1.56 5 0 -8 25.75 3.04 5 0 -8 32.33 4.52 5 0 -8 22.27 3.07 5 0 -8 25.24 3.11 5 0 -7 7.81 2.13 5 0 -7 7.44 3.01 5 0 -7 10.83 2.49 5 0 -7 10.51 2.41 5 0 -6 85.38 5.93 5 0 -6 92.57 6.43 5 0 -6 89.12 6.41 5 0 -5 58.64 4.82 5 0 -5 64.77 5.48 5 0 -5 55.71 5.27 5 0 -4 9.88 2.28 5 0 -4 7.48 2.42 5 0 -3 54.35 4.61 5 0 -3 62.57 6.21 5 0 -3 62.51 5.48 5 0 -2 16.68 3.60 5 0 -2 13.04 3.01 5 0 -2 15.65 3.39 5 0 -1 14.70 3.55 -5 0 1 12.98 3.31 5 0 -1 12.93 2.89 5 0 -1 12.41 3.14 5 0 0 8.71 3.08 -5 0 0 15.97 3.50 5 0 0 10.40 2.55 5 0 0 9.35 2.92 -5 0 -1 93.13 7.21 5 0 1 76.50 7.33 5 0 1 81.23 6.84 -5 0 -2 55.09 5.59 5 0 2 57.37 6.34 5 0 2 61.90 5.82 -5 0 -3 123.96 8.39 5 0 3 131.09 9.65 5 0 3 112.40 8.03 -5 0 -4 19.87 3.06 5 0 4 26.27 4.50 -5 0 -4 26.66 3.94 5 0 4 24.33 3.72 -5 0 -5 8.15 2.26 -5 0 -5 10.06 2.96 5 0 5 12.29 3.45 5 0 5 4.97 2.19 -5 0 -6 25.67 3.53 5 0 6 26.35 4.46 -5 0 -6 26.79 3.84 -5 0 -7 37.26 3.98 5 0 7 29.07 4.43 -5 0 -7 33.10 4.16 -5 0 -8 65.00 4.98 5 0 8 55.54 5.39 -5 0 -8 54.40 4.95 -5 0 -9 50.04 4.10 5 0 9 51.22 4.73 -5 0 -9 58.75 4.73 -5 0 -10 16.24 2.10 5 0 10 15.66 2.40 -5 0 -10 16.66 2.51 5 1 -10 1.83 1.22 5 1 -10 0.68 1.72 5 1 -10 1.96 1.30 5 1 -10 2.01 0.91 5 1 -9 29.96 3.14 5 1 -9 31.15 4.11 5 1 -9 26.19 3.03 5 1 -9 26.94 2.81 5 1 -8 6.22 1.97 5 1 -8 2.90 2.39 5 1 -8 4.83 2.65 5 1 -8 6.22 2.19 5 1 -8 3.31 1.68 5 1 -7 84.57 5.96 5 1 -7 99.22 7.77 5 1 -7 82.62 6.25 5 1 -7 90.85 6.09 5 1 -6 43.72 4.32 5 1 -6 47.67 5.64 5 1 -6 40.42 4.53 5 1 -6 42.40 4.36 5 1 -5 130.64 8.04 5 1 -5 134.66 8.61 5 1 -5 126.36 8.23 5 1 -4 159.66 9.18 5 1 -4 160.30 9.82 5 1 -4 159.70 9.71 5 1 -3 1103.81 41.72 5 1 -3 1166.29 43.84 5 1 -3 1103.33 42.81 5 1 -3 1106.87 42.85 5 1 -2 15.56 2.95 5 1 -2 12.45 3.38 5 1 -2 12.32 3.22 5 1 -2 9.61 2.96 5 1 -1 72.49 5.68 -5 1 1 82.41 6.85 5 1 -1 86.04 7.25 5 1 -1 76.89 6.68 -5 1 0 162.39 9.99 5 1 0 150.42 10.34 5 1 0 141.96 9.54 5 1 0 169.96 10.48 -5 1 -1 82.23 6.68 5 1 1 78.41 7.17 5 1 1 61.73 6.02 5 1 1 76.94 6.79 -5 1 -2 196.93 11.33 5 1 2 203.13 12.41 5 1 2 183.65 11.03 5 1 2 228.03 12.48 5 1 3 95.47 8.03 5 1 3 84.75 6.81 5 1 3 96.41 7.61 -5 1 -3 108.72 7.62 5 1 4 91.54 7.87 5 1 4 88.54 7.15 -5 1 -4 87.82 6.82 -5 1 -5 15.58 2.65 -5 1 -5 25.71 3.81 5 1 5 22.23 4.08 5 1 5 21.83 3.65 -5 1 -6 118.55 7.52 5 1 6 135.45 9.40 -5 1 -6 148.62 8.78 5 1 6 138.29 8.47 -5 1 -7 57.20 4.76 5 1 7 57.19 5.77 -5 1 -7 64.29 5.46 5 1 7 52.35 4.49 -5 1 -8 15.32 2.56 -5 1 -8 11.70 2.69 5 1 8 11.18 2.72 -5 1 -9 24.07 2.77 5 1 9 24.34 3.25 -5 1 -9 25.28 3.31 -5 1 -10 15.23 1.93 5 1 10 18.41 2.33 -5 1 -10 15.10 2.29 5 2 -10 5.04 1.42 5 2 -10 3.56 1.61 5 2 -9 40.47 3.44 5 2 -9 37.06 4.01 5 2 -9 28.58 2.49 5 2 -8 21.24 2.89 5 2 -8 18.74 3.36 5 2 -8 23.79 2.63 5 2 -7 6.94 2.32 5 2 -7 3.72 2.26 5 2 -7 4.90 2.25 5 2 -7 7.73 2.08 5 2 -6 1.78 1.88 5 2 -6 2.23 2.51 5 2 -6 0.61 2.28 5 2 -6 1.49 1.68 5 2 -5 10.14 2.66 5 2 -5 11.50 2.98 5 2 -5 12.32 2.71 5 2 -4 171.18 9.92 5 2 -4 179.59 10.70 5 2 -4 181.22 10.29 5 2 -3 42.30 4.61 5 2 -3 39.34 4.73 5 2 -3 41.96 4.93 5 2 -3 38.28 4.55 5 2 -2 314.84 15.21 -5 2 2 346.20 15.99 5 2 -2 311.64 15.90 5 2 -2 326.98 16.25 5 2 -2 300.15 15.62 5 2 -1 71.10 6.06 -5 2 1 75.57 6.32 5 2 -1 76.75 6.54 5 2 -1 70.33 6.55 5 2 -1 72.70 6.62 -5 2 0 27.65 3.90 5 2 0 19.48 3.33 5 2 0 17.66 3.30 5 2 0 14.78 3.61 5 2 0 18.91 3.88 -5 2 -1 45.29 4.72 5 2 1 35.89 4.21 5 2 1 37.49 4.58 5 2 1 37.89 4.97 -5 2 -2 93.85 6.93 5 2 2 85.80 7.19 5 2 2 76.48 6.95 5 2 2 93.79 7.73 5 2 3 252.42 13.78 5 2 3 225.98 13.09 5 2 3 270.87 14.22 -5 2 -3 250.55 12.91 5 2 4 30.67 4.40 5 2 4 25.24 4.00 5 2 4 25.12 4.26 -5 2 -4 30.86 3.98 5 2 5 65.55 6.15 5 2 5 57.57 5.50 -5 2 -5 79.88 6.01 5 2 5 67.14 6.25 5 2 6 76.74 6.63 -5 2 -6 99.56 6.71 5 2 6 86.42 6.74 -5 2 -7 6.78 1.83 -5 2 -7 10.25 2.67 5 2 7 9.58 2.70 5 2 7 11.01 2.53 -5 2 -8 88.83 5.46 5 2 8 96.54 6.48 -5 2 -8 104.37 6.45 5 2 8 88.35 5.61 -5 2 -9 16.87 2.05 5 2 9 13.09 2.20 -5 2 -9 16.45 2.50 5 3 -9 83.23 4.25 5 3 -9 95.00 4.95 5 3 -8 27.33 2.89 5 3 -8 25.69 3.13 5 3 -8 30.85 3.24 5 3 -7 2.80 1.70 5 3 -7 3.56 1.80 5 3 -7 2.97 1.88 5 3 -7 4.08 2.05 5 3 -7 3.52 1.32 5 3 -6 25.54 3.38 5 3 -6 18.85 3.27 5 3 -6 19.04 2.62 5 3 -6 21.00 3.05 5 3 -5 71.95 5.71 -5 3 5 60.62 4.96 5 3 -5 73.18 6.11 5 3 -5 69.59 5.19 5 3 -5 63.58 5.25 5 3 -4 220.57 11.28 -5 3 4 199.71 10.46 5 3 -4 191.15 10.45 5 3 -4 208.46 10.88 5 3 -3 149.05 9.04 -5 3 3 145.95 8.55 5 3 -3 157.41 9.81 5 3 -3 141.53 8.74 5 3 -3 141.45 8.78 5 3 -2 30.62 4.16 -5 3 2 33.66 3.87 5 3 -2 33.19 4.14 5 3 -2 31.03 4.49 5 3 -2 23.81 3.71 5 3 -2 31.89 4.11 5 3 -1 13.84 3.06 5 3 -1 14.32 3.18 5 3 -1 11.72 2.84 -5 3 1 13.10 2.86 5 3 -1 13.17 3.54 5 3 -1 12.14 3.16 -5 3 0 25.60 3.63 5 3 0 30.23 4.24 5 3 0 28.50 3.92 5 3 0 32.68 4.59 5 3 0 29.51 4.31 5 3 1 3.36 2.29 5 3 1 2.60 2.06 -5 3 -1 3.64 2.17 5 3 1 4.88 2.65 5 3 1 8.50 2.86 5 3 2 88.10 6.71 5 3 2 86.83 6.85 5 3 2 97.73 7.82 5 3 2 82.21 7.17 -5 3 -2 101.65 6.69 5 3 3 72.22 6.15 5 3 3 69.16 6.48 -5 3 -3 85.84 6.04 5 3 4 40.06 4.47 5 3 4 37.28 4.66 -5 3 -4 40.89 4.26 5 3 5 37.73 4.20 5 3 5 36.77 4.44 -5 3 -5 42.27 4.22 5 3 5 36.92 4.55 5 3 6 80.03 5.97 5 3 6 74.12 5.88 -5 3 -6 83.28 5.72 5 3 6 88.30 6.62 5 3 7 59.20 4.75 -5 3 -7 62.02 4.68 5 3 7 70.34 5.30 5 3 8 31.05 2.88 -5 3 -8 26.32 2.79 5 3 8 29.04 3.09 5 4 -8 35.47 2.96 5 4 -8 39.85 3.15 5 4 -8 40.66 3.25 5 4 -7 11.85 2.15 5 4 -7 9.93 2.14 5 4 -6 146.16 8.14 5 4 -6 144.30 7.85 5 4 -5 23.14 3.19 5 4 -5 25.45 3.53 5 4 -5 18.49 2.38 5 4 -5 24.15 3.28 5 4 -4 13.83 2.91 5 4 -4 17.46 3.12 5 4 -4 17.19 3.25 5 4 -4 11.67 2.27 5 4 -3 11.22 2.73 5 4 -3 13.57 3.03 5 4 -3 11.50 2.31 5 4 -2 89.35 6.62 5 4 -2 85.04 6.14 5 4 -2 78.84 6.34 5 4 -1 5.65 2.53 5 4 -1 9.75 2.77 5 4 -1 6.93 2.33 5 4 0 267.63 12.71 5 4 0 240.92 12.93 5 4 0 198.11 11.56 5 4 0 225.94 11.96 5 4 1 10.07 2.74 5 4 1 12.33 3.06 5 4 1 13.37 3.26 5 4 1 12.27 2.96 5 4 2 102.77 7.19 5 4 2 105.15 7.90 5 4 2 105.72 7.56 5 4 3 86.71 6.35 5 4 3 101.09 7.42 5 4 3 88.37 6.88 5 4 4 36.01 4.48 5 4 4 44.58 4.76 5 4 5 72.04 5.82 5 4 6 178.06 9.47 5 4 7 124.75 6.91 5 4 7 134.48 7.29 5 4 8 7.79 1.62 5 5 -7 31.46 2.61 5 5 -6 143.91 7.17 5 5 -6 152.60 7.29 5 5 -6 141.55 7.20 5 5 -5 51.40 4.05 5 5 -5 41.08 3.72 5 5 -5 43.45 3.85 5 5 -4 41.73 3.96 5 5 -4 40.54 4.06 5 5 -4 41.79 4.02 5 5 -3 10.32 2.46 5 5 -3 14.10 2.72 5 5 -3 12.83 2.67 5 5 -3 12.71 2.67 5 5 -3 7.34 1.55 5 5 -2 75.43 5.51 5 5 -2 73.01 5.63 5 5 -2 60.28 5.31 5 5 -2 58.41 4.35 5 5 -2 72.09 5.55 5 5 -1 17.66 3.14 5 5 -1 21.10 3.21 5 5 -1 21.37 3.38 5 5 -1 18.37 3.31 5 5 -1 18.72 2.67 5 5 0 57.51 5.03 5 5 0 52.29 5.06 5 5 0 53.34 4.43 5 5 0 56.19 5.07 5 5 1 78.45 5.92 5 5 1 74.35 5.48 5 5 1 78.70 5.88 5 5 2 79.35 5.76 5 5 2 73.55 5.55 5 5 2 69.66 5.46 5 5 3 2.56 1.70 5 5 3 3.16 1.94 5 5 4 15.50 2.44 5 5 4 21.89 3.26 5 5 4 24.50 3.18 5 5 5 13.85 2.56 5 5 5 18.80 2.73 5 5 6 2.86 1.60 5 5 6 0.72 1.35 5 6 -4 30.06 2.65 5 6 -4 22.98 2.33 5 6 -4 24.62 2.55 5 6 -3 5.56 1.72 5 6 -3 7.61 1.75 5 6 -3 6.20 1.62 5 6 -3 4.74 1.69 5 6 -2 11.85 2.15 5 6 -2 11.41 2.08 5 6 -2 9.00 2.01 5 6 -1 10.50 2.22 5 6 -1 15.61 2.44 5 6 -1 11.78 2.18 5 6 -1 12.74 2.40 5 6 0 20.07 2.67 5 6 0 20.22 2.76 5 6 0 19.27 2.82 5 6 0 20.09 2.82 5 6 1 14.00 2.37 5 6 1 14.69 2.33 5 6 1 15.06 2.51 5 6 1 10.22 1.65 5 6 2 23.90 2.76 5 6 2 29.39 3.20 5 6 2 23.99 2.40 5 6 2 23.98 2.76 5 6 3 10.46 1.82 5 6 3 13.10 2.20 5 6 3 10.35 1.71 5 6 4 3.30 1.44 -6 -2 5 23.12 2.07 -6 -2 4 111.79 5.43 6 -2 -4 107.22 6.09 -6 -2 3 24.02 2.47 6 -2 -3 25.83 3.03 6 -2 -3 18.62 1.94 -6 -2 2 60.25 4.14 -6 -2 1 23.25 2.60 -6 -2 0 16.58 2.38 6 -2 1 23.23 2.76 -6 -2 -1 24.37 2.70 6 -2 2 28.66 2.96 -6 -2 -2 28.17 2.81 6 -2 3 17.16 2.21 -6 -2 -3 15.45 2.14 -6 -2 -4 34.42 2.82 -6 -1 6 7.71 1.43 6 -1 -6 10.02 2.01 6 -1 -6 7.78 1.31 -6 -1 5 58.91 3.95 6 -1 -5 59.90 4.53 6 -1 -5 50.40 3.52 -6 -1 4 37.08 3.28 6 -1 -4 33.61 3.67 6 -1 -4 29.24 2.68 -6 -1 3 19.22 2.63 6 -1 -3 18.83 2.28 -6 -1 2 30.29 3.17 6 -1 -2 23.80 2.55 -6 -1 1 49.67 4.09 6 -1 -1 37.90 3.23 6 -1 0 13.69 2.59 -6 -1 0 14.99 2.42 6 -1 0 11.54 1.85 -6 -1 -1 13.99 2.46 6 -1 1 11.75 2.40 6 -1 2 21.88 2.95 -6 -1 -2 26.65 3.00 6 -1 3 165.78 8.76 -6 -1 -3 179.92 8.61 6 -1 4 66.18 4.71 -6 -1 -4 75.00 4.70 6 -1 5 11.63 1.87 -6 -1 -5 13.84 2.08 -6 0 6 9.00 1.59 6 0 -6 7.28 1.88 6 0 -6 6.15 1.28 -6 0 5 93.82 5.52 6 0 -5 105.72 6.46 -6 0 4 120.70 6.73 6 0 -4 126.00 7.55 -6 0 3 12.74 2.38 6 0 -3 12.31 2.09 -6 0 2 81.52 5.43 6 0 -2 72.11 4.90 -6 0 1 52.88 4.30 6 0 -1 38.49 3.58 6 0 0 12.06 2.48 -6 0 0 15.35 2.53 6 0 0 15.51 2.33 6 0 1 32.57 3.62 6 0 1 23.16 2.71 -6 0 -1 33.93 3.43 6 0 2 20.95 2.97 6 0 2 17.43 2.29 6 0 3 80.55 5.78 -6 0 -3 100.35 5.89 -6 0 -4 9.43 2.04 6 0 4 5.58 1.78 -6 0 -5 1.72 1.46 6 0 5 3.45 1.41 -6 0 -6 0.26 1.02 -6 1 6 10.17 1.55 6 1 -6 4.86 1.13 -6 1 5 51.66 3.58 6 1 -5 50.88 4.14 6 1 -5 46.35 3.36 -6 1 4 35.48 3.22 6 1 -4 39.90 3.93 6 1 -4 38.04 3.17 -6 1 3 22.66 2.77 -6 1 2 24.98 3.02 -6 1 1 41.87 3.86 6 1 -1 39.19 3.66 6 1 0 14.16 2.59 -6 1 0 11.79 2.38 6 1 0 12.59 2.37 6 1 1 12.07 2.41 -6 1 -1 12.42 2.36 6 1 1 12.13 2.24 6 1 2 20.37 2.89 -6 1 -2 23.11 2.96 6 1 2 20.71 2.59 6 1 3 155.12 8.19 6 1 3 134.05 7.18 6 1 4 66.20 4.67 -6 1 -4 71.31 4.63 6 1 5 11.77 1.92 -6 1 -5 13.46 2.08 -6 1 -6 69.77 4.06 -6 2 5 27.25 2.19 6 2 -5 29.55 2.31 -6 2 4 108.78 5.33 6 2 -4 93.98 5.75 6 2 -4 101.96 5.37 -6 2 3 28.96 2.65 6 2 -3 27.16 3.06 6 2 -3 24.09 2.46 6 2 -3 24.73 2.62 -6 2 2 59.26 4.08 6 2 -2 62.25 4.27 6 2 -1 24.42 2.79 -6 2 1 22.96 2.63 -6 2 0 15.13 2.32 6 2 1 19.84 2.63 -6 2 -1 23.45 2.68 6 2 1 22.59 2.74 6 2 2 26.42 2.87 -6 2 -2 29.92 2.89 6 2 2 22.81 2.67 6 2 3 15.25 2.14 -6 2 -3 18.86 2.29 6 2 3 16.76 2.18 -6 2 -4 40.90 3.14 6 3 -3 48.88 3.17 6 3 -2 4.85 1.39 6 3 -2 4.91 1.33 6 3 -1 10.94 1.79 6 3 -1 9.93 1.75 6 3 0 45.65 3.52 6 3 1 6.27 1.63 6 3 3 12.61 1.75 0 0 0 0.00 0.00 TITL exp_489 in P2(1) REM P2(1) (#4 in standard setting) CELL 1.54184 5.144874 8.471721 13.863552 90.0000 91.1747 90.0000 ZERR 11.00 0.000088 0.000194 0.000212 0.0000 0.0014 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H O F UNIT 11.00 11.00 11.00 11.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 1290 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.268 _oxdiff_exptl_absorpt_empirical_full_min 0.650