data_WQQ116a_0m_a _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H20 F3 N5 O4 S' _chemical_formula_weight 531.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8433(14) _cell_length_b 16.994(2) _cell_length_c 12.4738(14) _cell_angle_alpha 90 _cell_angle_beta 102.967(3) _cell_angle_gamma 90 _cell_volume 2446.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_F_000 1096 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.419 _exptl_crystal_size_mid 0.245 _exptl_crystal_size_min 0.192 _exptl_absorpt_coefficient_mu 0.197 _shelx_estimated_absorpt_T_min 0.922 _shelx_estimated_absorpt_T_max 0.963 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6223 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker D8 Quest ECO PHOTON 50' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22502 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.060 _diffrn_reflns_theta_max 25.458 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 4505 _reflns_number_gt 3547 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+2.0677P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4505 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 0.912 _refine_ls_restrained_S_all 0.912 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 S001 S 0.46045(4) 0.86097(3) 0.72300(4) 0.02834(15) Uani 1 1 d . . . . . O1 O 0.59417(11) 0.49674(8) 0.66743(12) 0.0274(3) Uani 1 1 d . . . . . O2 O 0.57547(14) 0.86860(10) 0.70764(18) 0.0529(5) Uani 1 1 d . . . . . O3 O 0.43595(14) 0.78425(10) 0.75904(16) 0.0501(5) Uani 1 1 d . . . . . N5 N 0.60965(16) 0.65146(11) 0.78208(15) 0.0282(4) Uani 1 1 d . . . . . N4 N 0.73923(17) 0.74300(10) 0.74743(15) 0.0284(4) Uani 1 1 d . . . . . N2 N 0.36567(16) 0.66629(11) 1.11179(15) 0.0330(4) Uani 1 1 d . . . . . N3 N 0.78720(14) 0.61266(10) 0.75193(14) 0.0266(4) Uani 1 1 d . . . . . H3 H 0.8483 0.6262 0.7270 0.032 Uiso 1 1 calc R U . . . O4 O 0.42192(18) 0.92549(12) 0.77822(16) 0.0587(5) Uani 1 1 d . . . . . N1 N 1.00386(15) 0.35810(10) 0.32240(16) 0.0334(4) Uani 1 1 d . . . . . F3 F 0.3904(2) 0.93744(11) 0.54067(15) 0.0919(7) Uani 1 1 d . . . . . C13 C 0.51418(16) 0.44058(11) 0.62537(15) 0.0223(4) Uani 1 1 d . . . . . C8 C 0.52522(17) 0.38501(11) 0.54506(15) 0.0235(4) Uani 1 1 d . . . . . C23 C 0.71182(16) 0.66827(11) 0.75934(15) 0.0227(4) Uani 1 1 d . . . . . C14 C 0.40490(17) 0.49583(12) 0.75319(16) 0.0263(4) Uani 1 1 d . . . . . C3 C 0.80567(17) 0.36597(11) 0.40940(16) 0.0253(4) Uani 1 1 d . . . . . C16 C 0.38733(17) 0.57980(11) 0.92565(16) 0.0249(4) Uani 1 1 d . . . . . C7 C 0.62477(18) 0.37979(11) 0.49780(16) 0.0254(4) Uani 1 1 d . . . . . C12 C 0.41247(17) 0.44305(11) 0.66527(16) 0.0245(4) Uani 1 1 d . . . . . C2 C 0.80319(17) 0.32840(12) 0.30946(17) 0.0281(4) Uani 1 1 d . . . . . H00K H 0.7340 0.3046 0.2692 0.034 Uiso 1 1 calc R U . . . C15 C 0.39767(17) 0.53530(12) 0.83100(17) 0.0267(4) Uani 1 1 d . . . . . C21 C 0.71569(17) 0.47874(12) 0.68827(18) 0.0296(5) Uani 1 1 d . . . . . H00H H 0.7457 0.4889 0.6216 0.035 Uiso 1 1 calc R U . . . H00J H 0.7288 0.4226 0.7084 0.035 Uiso 1 1 calc R U . . . C17 C 0.28046(19) 0.58736(12) 0.95431(17) 0.0292(5) Uani 1 1 d . . . . . H00N H 0.2130 0.5632 0.9112 0.035 Uiso 1 1 calc R U . . . C6 C 0.70516(18) 0.37181(11) 0.45513(17) 0.0269(4) Uani 1 1 d . . . . . C18 C 0.27482(19) 0.63077(13) 1.04667(18) 0.0327(5) Uani 1 1 d . . . . . H00P H 0.2016 0.6357 1.0651 0.039 Uiso 1 1 calc R U . . . C1 C 0.90330(18) 0.32643(13) 0.27021(18) 0.0313(5) Uani 1 1 d . . . . . H00Q H 0.9005 0.3010 0.2019 0.038 Uiso 1 1 calc R U . . . C22 C 0.77734(19) 0.53053(12) 0.78171(18) 0.0312(5) Uani 1 1 d . . . . . H00M H 0.7353 0.5279 0.8418 0.037 Uiso 1 1 calc R U . . . H00R H 0.8561 0.5092 0.8105 0.037 Uiso 1 1 calc R U . . . C9 C 0.43253(18) 0.33327(12) 0.50666(16) 0.0279(4) Uani 1 1 d . . . . . H00S H 0.4394 0.2946 0.4535 0.033 Uiso 1 1 calc R U . . . F1 F 0.3972(3) 0.81306(13) 0.52128(16) 0.1278(11) Uani 1 1 d . . . . . C11 C 0.32114(18) 0.39215(12) 0.62365(17) 0.0290(5) Uani 1 1 d . . . . . H00U H 0.2517 0.3950 0.6495 0.035 Uiso 1 1 calc R U . . . C20 C 0.48235(18) 0.61589(13) 0.99319(17) 0.0300(5) Uani 1 1 d . . . . . H00V H 0.5569 0.6117 0.9773 0.036 Uiso 1 1 calc R U . . . C10 C 0.33177(18) 0.33735(13) 0.54435(17) 0.0310(5) Uani 1 1 d . . . . . H00W H 0.2695 0.3025 0.5159 0.037 Uiso 1 1 calc R U . . . C4 C 0.91080(19) 0.39825(13) 0.46499(19) 0.0343(5) Uani 1 1 d . . . . . H00X H 0.9170 0.4236 0.5339 0.041 Uiso 1 1 calc R U . . . C19 C 0.4675(2) 0.65789(13) 1.08369(18) 0.0344(5) Uani 1 1 d . . . . . H00Y H 0.5336 0.6823 1.1287 0.041 Uiso 1 1 calc R U . . . C5 C 1.00535(19) 0.39278(13) 0.4184(2) 0.0381(5) Uani 1 1 d . . . . . H00Z H 1.0763 0.4152 0.4573 0.046 Uiso 1 1 calc R U . . . F2 F 0.26201(19) 0.86462(16) 0.5852(3) 0.1354(12) Uani 1 1 d . . . . . C24 C 0.3729(3) 0.86917(16) 0.5856(2) 0.0624(9) Uani 1 1 d . . . . . H4 H 0.801(2) 0.7544(13) 0.7251(18) 0.027(6) Uiso 1 1 d . . . . . H4A H 0.682(2) 0.7795(15) 0.7417(19) 0.036(6) Uiso 1 1 d . . . . . H5A H 0.558(2) 0.6909(15) 0.7805(18) 0.032(6) Uiso 1 1 d . . . . . H5 H 0.583(2) 0.6057(16) 0.7690(19) 0.034(6) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S001 0.0200(3) 0.0301(3) 0.0347(3) 0.0013(2) 0.0057(2) -0.00102(19) O1 0.0237(7) 0.0218(7) 0.0367(8) -0.0053(6) 0.0070(6) -0.0010(5) O2 0.0250(9) 0.0449(10) 0.0917(15) 0.0258(10) 0.0191(9) 0.0023(7) O3 0.0307(9) 0.0440(10) 0.0747(13) 0.0194(9) 0.0098(8) -0.0064(7) N5 0.0290(10) 0.0215(9) 0.0378(10) -0.0007(7) 0.0153(8) -0.0026(8) N4 0.0278(10) 0.0244(9) 0.0356(10) 0.0033(7) 0.0128(8) -0.0025(8) N2 0.0401(11) 0.0316(10) 0.0295(10) -0.0039(8) 0.0124(8) 0.0056(8) N3 0.0239(9) 0.0259(9) 0.0310(9) -0.0023(7) 0.0083(7) -0.0019(7) O4 0.0754(14) 0.0555(12) 0.0481(11) -0.0069(9) 0.0199(10) 0.0189(10) N1 0.0254(9) 0.0295(9) 0.0468(11) -0.0004(8) 0.0112(8) 0.0012(7) F3 0.160(2) 0.0599(12) 0.0480(10) 0.0150(9) 0.0072(11) 0.0530(13) C13 0.0252(10) 0.0210(9) 0.0205(9) 0.0017(7) 0.0044(8) -0.0010(8) C8 0.0275(10) 0.0229(10) 0.0202(9) 0.0019(7) 0.0056(8) 0.0038(8) C23 0.0253(10) 0.0246(10) 0.0183(9) -0.0014(7) 0.0052(8) -0.0026(8) C14 0.0253(10) 0.0270(10) 0.0278(11) 0.0010(8) 0.0087(8) 0.0000(8) C3 0.0261(10) 0.0229(10) 0.0266(10) 0.0007(8) 0.0056(8) 0.0021(8) C16 0.0308(11) 0.0216(9) 0.0237(10) 0.0024(8) 0.0093(8) 0.0023(8) C7 0.0320(11) 0.0206(10) 0.0234(10) -0.0027(8) 0.0057(9) 0.0004(8) C12 0.0285(10) 0.0240(10) 0.0217(10) 0.0002(8) 0.0072(8) 0.0009(8) C2 0.0240(10) 0.0305(11) 0.0290(11) -0.0037(9) 0.0043(8) -0.0013(8) C15 0.0276(11) 0.0270(10) 0.0269(11) 0.0009(9) 0.0087(8) -0.0011(8) C21 0.0260(10) 0.0254(10) 0.0358(12) -0.0049(9) 0.0038(9) 0.0024(8) C17 0.0318(11) 0.0285(11) 0.0296(11) 0.0003(9) 0.0119(9) -0.0036(8) C6 0.0299(11) 0.0251(10) 0.0254(10) -0.0021(8) 0.0055(9) 0.0009(8) C18 0.0343(12) 0.0332(12) 0.0353(12) 0.0001(9) 0.0176(10) 0.0015(9) C1 0.0306(11) 0.0344(12) 0.0304(11) -0.0034(9) 0.0101(9) 0.0025(9) C22 0.0325(11) 0.0246(10) 0.0330(12) -0.0029(9) 0.0002(9) 0.0029(9) C9 0.0336(11) 0.0274(10) 0.0217(10) -0.0037(8) 0.0040(8) 0.0002(9) F1 0.231(3) 0.0698(13) 0.0504(11) -0.0262(10) -0.0364(14) 0.0689(16) C11 0.0281(11) 0.0319(11) 0.0281(11) -0.0006(9) 0.0088(9) -0.0034(9) C20 0.0282(11) 0.0347(11) 0.0285(11) -0.0024(9) 0.0089(9) 0.0029(9) C10 0.0306(11) 0.0316(11) 0.0299(11) -0.0037(9) 0.0048(9) -0.0066(9) C4 0.0325(12) 0.0346(12) 0.0343(12) -0.0083(10) 0.0041(9) -0.0018(9) C19 0.0346(12) 0.0362(12) 0.0327(12) -0.0067(9) 0.0080(10) 0.0000(9) C5 0.0254(11) 0.0360(12) 0.0500(14) -0.0071(11) 0.0023(10) -0.0033(9) F2 0.0519(13) 0.136(2) 0.175(3) -0.0077(19) -0.0656(15) 0.0138(13) C24 0.078(2) 0.0421(16) 0.0515(17) -0.0078(13) -0.0188(15) 0.0248(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 S001 O4 1.4234(18) . ? S001 O2 1.4235(16) . ? S001 O3 1.4298(17) . ? S001 C24 1.798(3) . ? O1 C13 1.364(2) . ? O1 C21 1.437(2) . ? N5 C23 1.334(3) . ? N4 C23 1.327(3) . ? N2 C19 1.337(3) . ? N2 C18 1.338(3) . ? N3 C23 1.317(3) . ? N3 C22 1.456(3) . ? N1 C5 1.331(3) . ? N1 C1 1.336(3) . ? F3 C24 1.325(4) . ? C13 C12 1.404(3) . ? C13 C8 1.404(3) . ? C8 C9 1.404(3) . ? C8 C7 1.434(3) . ? C14 C15 1.199(3) . ? C14 C12 1.435(3) . ? C3 C4 1.394(3) . ? C3 C2 1.395(3) . ? C3 C6 1.434(3) . ? C16 C20 1.388(3) . ? C16 C17 1.396(3) . ? C16 C15 1.430(3) . ? C7 C6 1.198(3) . ? C12 C11 1.391(3) . ? C2 C1 1.381(3) . ? C21 C22 1.511(3) . ? C17 C18 1.382(3) . ? C9 C10 1.379(3) . ? F1 C24 1.319(3) . ? C11 C10 1.385(3) . ? C20 C19 1.380(3) . ? C4 C5 1.375(3) . ? F2 C24 1.315(4) . ? 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 O4 S001 O2 114.54(12) . . ? O4 S001 O3 116.14(12) . . ? O2 S001 O3 113.15(10) . . ? O4 S001 C24 102.86(12) . . ? O2 S001 C24 103.24(15) . . ? O3 S001 C24 104.84(13) . . ? C13 O1 C21 120.10(15) . . ? C19 N2 C18 116.27(18) . . ? C23 N3 C22 125.13(17) . . ? C5 N1 C1 116.56(18) . . ? O1 C13 C12 114.83(16) . . ? O1 C13 C8 125.26(17) . . ? C12 C13 C8 119.86(17) . . ? C9 C8 C13 118.28(18) . . ? C9 C8 C7 118.22(18) . . ? C13 C8 C7 123.47(18) . . ? N3 C23 N4 119.46(18) . . ? N3 C23 N5 121.50(18) . . ? N4 C23 N5 119.01(18) . . ? C15 C14 C12 175.3(2) . . ? C4 C3 C2 117.51(18) . . ? C4 C3 C6 120.21(19) . . ? C2 C3 C6 122.28(18) . . ? C20 C16 C17 117.52(18) . . ? C20 C16 C15 121.78(18) . . ? C17 C16 C15 120.69(19) . . ? C6 C7 C8 176.3(2) . . ? C11 C12 C13 120.42(18) . . ? C11 C12 C14 119.81(18) . . ? C13 C12 C14 119.70(17) . . ? C1 C2 C3 118.70(19) . . ? C14 C15 C16 177.8(2) . . ? O1 C21 C22 107.84(16) . . ? C18 C17 C16 118.6(2) . . ? C7 C6 C3 176.1(2) . . ? N2 C18 C17 124.3(2) . . ? N1 C1 C2 124.1(2) . . ? N3 C22 C21 114.46(17) . . ? C10 C9 C8 121.49(19) . . ? C10 C11 C12 119.81(19) . . ? C19 C20 C16 119.36(19) . . ? C9 C10 C11 120.11(19) . . ? C5 C4 C3 118.9(2) . . ? N2 C19 C20 123.9(2) . . ? N1 C5 C4 124.2(2) . . ? F2 C24 F1 108.0(3) . . ? F2 C24 F3 107.5(2) . . ? F1 C24 F3 107.4(3) . . ? F2 C24 S001 111.2(3) . . ? F1 C24 S001 111.48(19) . . ? F3 C24 S001 111.1(2) . . ? _refine_diff_density_max 0.410 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.047 _shelx_res_file ; WQQ116a_0m_a.res created by SHELXL-2014/7 TITL WQQ116a_0m in P2(1)/n CELL 0.71073 11.8433 16.9936 12.4738 90.000 102.967 90.000 ZERR 4.00 0.00140 0.00220 0.00140 0.0000 0.0034 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O F S UNIT 96 80 20 16 12 4 L.S. 10 BOND FMAP 2 PLAN 20 OMIT 0 2 0 OMIT 1 1 0 ACTA SIZE 0.192 0.245 0.419 TEMP -123.140 WGHT 0.066200 2.067700 FVAR 0.56031 S001 6 0.460451 0.860968 0.723004 11.00000 0.01998 0.03011 = 0.03470 0.00128 0.00566 -0.00102 O1 4 0.594171 0.496744 0.667432 11.00000 0.02369 0.02179 = 0.03673 -0.00532 0.00704 -0.00103 O2 4 0.575469 0.868596 0.707642 11.00000 0.02505 0.04491 = 0.09168 0.02581 0.01915 0.00234 O3 4 0.435953 0.784251 0.759042 11.00000 0.03068 0.04399 = 0.07472 0.01941 0.00981 -0.00640 N5 3 0.609646 0.651456 0.782076 11.00000 0.02895 0.02151 = 0.03777 -0.00072 0.01528 -0.00261 N4 3 0.739234 0.743001 0.747431 11.00000 0.02784 0.02437 = 0.03564 0.00327 0.01279 -0.00249 N2 3 0.365673 0.666288 1.111791 11.00000 0.04011 0.03163 = 0.02949 -0.00385 0.01244 0.00561 N3 3 0.787195 0.612663 0.751928 11.00000 0.02389 0.02593 = 0.03101 -0.00225 0.00828 -0.00185 AFIX 43 H3 2 0.848303 0.626233 0.727018 11.00000 -1.20000 AFIX 0 O4 4 0.421917 0.925494 0.778217 11.00000 0.07544 0.05549 = 0.04809 -0.00694 0.01986 0.01890 N1 3 1.003858 0.358104 0.322399 11.00000 0.02536 0.02954 = 0.04680 -0.00041 0.01118 0.00121 F3 5 0.390389 0.937442 0.540668 11.00000 0.16009 0.05991 = 0.04800 0.01497 0.00724 0.05303 C13 1 0.514184 0.440578 0.625370 11.00000 0.02521 0.02098 = 0.02051 0.00171 0.00443 -0.00103 C8 1 0.525215 0.385009 0.545060 11.00000 0.02750 0.02294 = 0.02020 0.00193 0.00556 0.00382 C23 1 0.711816 0.668270 0.759338 11.00000 0.02526 0.02461 = 0.01829 -0.00138 0.00524 -0.00262 C14 1 0.404900 0.495828 0.753188 11.00000 0.02534 0.02699 = 0.02777 0.00102 0.00870 0.00003 C3 1 0.805673 0.365969 0.409399 11.00000 0.02611 0.02286 = 0.02663 0.00065 0.00558 0.00212 C16 1 0.387332 0.579805 0.925649 11.00000 0.03085 0.02158 = 0.02368 0.00237 0.00933 0.00226 C7 1 0.624771 0.379793 0.497796 11.00000 0.03200 0.02061 = 0.02337 -0.00266 0.00565 0.00037 C12 1 0.412467 0.443050 0.665273 11.00000 0.02846 0.02404 = 0.02171 0.00019 0.00719 0.00091 C2 1 0.803187 0.328399 0.309458 11.00000 0.02402 0.03055 = 0.02901 -0.00367 0.00426 -0.00133 AFIX 43 H00K 2 0.733979 0.304632 0.269188 11.00000 -1.20000 AFIX 0 C15 1 0.397674 0.535298 0.830999 11.00000 0.02757 0.02698 = 0.02687 0.00086 0.00865 -0.00106 C21 1 0.715694 0.478740 0.688266 11.00000 0.02599 0.02539 = 0.03581 -0.00491 0.00376 0.00245 AFIX 23 H00H 2 0.745660 0.488895 0.621582 11.00000 -1.20000 H00J 2 0.728761 0.422596 0.708440 11.00000 -1.20000 AFIX 0 C17 1 0.280463 0.587363 0.954312 11.00000 0.03177 0.02851 = 0.02956 0.00030 0.01191 -0.00364 AFIX 43 H00N 2 0.213047 0.563180 0.911242 11.00000 -1.20000 AFIX 0 C6 1 0.705161 0.371807 0.455127 11.00000 0.02985 0.02509 = 0.02545 -0.00207 0.00554 0.00089 C18 1 0.274820 0.630771 1.046673 11.00000 0.03429 0.03321 = 0.03526 0.00011 0.01765 0.00153 AFIX 43 H00P 2 0.201563 0.635713 1.065135 11.00000 -1.20000 AFIX 0 C1 1 0.903297 0.326432 0.270209 11.00000 0.03064 0.03444 = 0.03037 -0.00337 0.01014 0.00252 AFIX 43 H00Q 2 0.900465 0.300975 0.201851 11.00000 -1.20000 AFIX 0 C22 1 0.777339 0.530532 0.781710 11.00000 0.03249 0.02459 = 0.03302 -0.00287 0.00019 0.00291 AFIX 23 H00M 2 0.735293 0.527882 0.841837 11.00000 -1.20000 H00R 2 0.856132 0.509250 0.810479 11.00000 -1.20000 AFIX 0 C9 1 0.432532 0.333268 0.506662 11.00000 0.03357 0.02737 = 0.02168 -0.00371 0.00396 0.00025 AFIX 43 H00S 2 0.439392 0.294577 0.453518 11.00000 -1.20000 AFIX 0 F1 5 0.397204 0.813057 0.521277 11.00000 0.23098 0.06980 = 0.05044 -0.02622 -0.03637 0.06890 C11 1 0.321142 0.392153 0.623647 11.00000 0.02815 0.03193 = 0.02813 -0.00056 0.00877 -0.00338 AFIX 43 H00U 2 0.251691 0.394990 0.649547 11.00000 -1.20000 AFIX 0 C20 1 0.482348 0.615891 0.993189 11.00000 0.02816 0.03467 = 0.02848 -0.00243 0.00894 0.00285 AFIX 43 H00V 2 0.556883 0.611713 0.977257 11.00000 -1.20000 AFIX 0 C10 1 0.331770 0.337347 0.544353 11.00000 0.03059 0.03164 = 0.02987 -0.00373 0.00479 -0.00655 AFIX 43 H00W 2 0.269545 0.302499 0.515871 11.00000 -1.20000 AFIX 0 C4 1 0.910797 0.398248 0.464993 11.00000 0.03245 0.03461 = 0.03434 -0.00829 0.00412 -0.00182 AFIX 43 H00X 2 0.917015 0.423617 0.533940 11.00000 -1.20000 AFIX 0 C19 1 0.467497 0.657890 1.083687 11.00000 0.03457 0.03616 = 0.03267 -0.00669 0.00798 -0.00003 AFIX 43 H00Y 2 0.533568 0.682295 1.128711 11.00000 -1.20000 AFIX 0 C5 1 1.005348 0.392778 0.418426 11.00000 0.02543 0.03603 = 0.05000 -0.00711 0.00231 -0.00335 AFIX 43 H00Z 2 1.076267 0.415177 0.457272 11.00000 -1.20000 AFIX 0 F2 5 0.262011 0.864624 0.585195 11.00000 0.05187 0.13633 = 0.17495 -0.00772 -0.06559 0.01378 C24 1 0.372934 0.869168 0.585607 11.00000 0.07777 0.04214 = 0.05154 -0.00779 -0.01882 0.02483 H4 2 0.801184 0.754384 0.725131 11.00000 0.02695 H4A 2 0.681969 0.779538 0.741727 11.00000 0.03594 H5A 2 0.557739 0.690888 0.780497 11.00000 0.03194 H5 2 0.583329 0.605712 0.768951 11.00000 0.03364 HKLF 4 REM WQQ116a_0m in P2(1)/n REM R1 = 0.0413 for 3547 Fo > 4sig(Fo) and 0.0584 for all 4505 data REM 350 parameters refined using 0 restraints END WGHT 0.0469 1.6947 REM Highest difference peak 0.410, deepest hole -0.346, 1-sigma level 0.047 Q1 1 0.4609 0.8457 0.5173 11.00000 0.05 0.41 Q2 1 0.3006 0.8704 0.5341 11.00000 0.05 0.36 Q3 1 0.2572 0.8716 0.6245 11.00000 0.05 0.33 Q4 1 0.3614 0.8103 0.5229 11.00000 0.05 0.31 Q5 1 0.4378 0.7670 0.6953 11.00000 0.05 0.30 Q6 1 0.4779 0.9286 0.7593 11.00000 0.05 0.30 Q7 1 0.4050 0.8651 0.6468 11.00000 0.05 0.28 Q8 1 0.4349 0.9715 0.5818 11.00000 0.05 0.28 Q9 1 0.5062 0.4276 0.5603 11.00000 0.05 0.25 Q10 1 0.4764 0.8049 0.7795 11.00000 0.05 0.24 Q11 1 0.3774 0.9059 0.7258 11.00000 0.05 0.22 Q12 1 0.6284 0.3651 0.4355 11.00000 0.05 0.21 Q13 1 0.5401 0.8439 0.6627 11.00000 0.05 0.19 Q14 1 0.3883 0.5442 0.7584 11.00000 0.05 0.19 Q15 1 0.4815 0.6079 1.0590 11.00000 0.05 0.19 Q16 1 0.4842 0.3587 0.5341 11.00000 0.05 0.18 Q17 1 0.8498 0.4009 0.4163 11.00000 0.05 0.18 Q18 1 0.4143 0.9330 0.8038 11.00000 0.05 0.18 Q19 1 0.3255 0.6028 0.9207 11.00000 0.05 0.18 Q20 1 0.3800 0.8161 0.7236 11.00000 0.05 0.18 ; _shelx_res_checksum 13366 _shelx_hkl_file ; -2 0 0 828.52 20.50 -2 0 0 825.22 20.50 2 0 0 864.21 20.50 2 0 0 834.52 20.50 -2 0 0 878.51 20.80 -3 0 0 -5.20 1.40 3 0 0 -2.10 1.60 -3 0 0 -2.50 1.30 -3 0 0 -3.30 2.20 3 0 0 -4.70 1.40 4 0 0 188.48 6.10 4 0 0 186.48 6.00 -4 0 0 204.68 6.10 5 0 0 -1.70 2.30 5 0 0 0.10 2.10 6 0 0 3684.83 88.39 7 0 0 -0.60 2.60 8 0 0 6.80 4.20 -9 0 0 -4.20 4.40 9 0 0 5.90 3.50 -10 0 0 503.25 18.20 10 0 0 545.05 16.70 -11 0 0 -2.90 5.60 -12 0 0 39.90 7.50 -13 0 0 5.60 5.80 -13 0 0 0.60 7.30 -1 -1 0 0.00 0.50 -1 -1 0 0.50 0.30 -1 1 0 -1.20 0.50 2 -1 0 765.32 18.30 2 -1 0 735.03 18.10 -2 -1 0 720.33 17.80 -2 -1 0 739.23 18.40 -2 1 0 715.93 18.30 -2 1 0 753.32 18.10 2 1 0 734.73 18.40 2 1 0 729.93 17.90 -2 1 0 746.43 18.20 3 -1 0 616.84 15.80 3 -1 0 618.74 16.00 -3 -1 0 635.94 15.60 -3 -1 0 626.54 15.70 -3 1 0 619.64 15.80 -3 1 0 625.84 16.30 3 1 0 624.64 15.60 -3 1 0 668.23 16.60 3 1 0 616.84 16.30 4 -1 0 797.42 19.90 4 -1 0 787.62 20.00 -4 -1 0 795.72 20.20 -4 -1 0 763.12 20.30 -4 1 0 805.82 20.70 -4 1 0 783.72 20.40 4 1 0 788.62 19.70 5 -1 0 65.09 4.20 5 -1 0 51.79 4.50 -5 1 0 50.49 5.50 5 1 0 53.69 4.10 6 -1 0 255.17 8.30 6 -1 0 234.28 8.60 6 1 0 251.07 8.20 -6 1 0 250.67 9.60 7 -1 0 54.49 4.80 7 -1 0 63.29 5.30 -7 1 0 48.10 6.00 7 1 0 58.49 4.70 8 -1 0 472.15 14.60 8 1 0 491.35 14.30 -8 1 0 487.15 16.00 9 -1 0 284.47 10.40 -9 1 0 268.87 12.30 10 -1 0 967.90 26.50 -10 1 0 934.01 28.30 11 -1 0 53.49 6.30 -11 -1 0 51.59 7.30 -11 -1 0 49.20 5.90 -11 1 0 48.30 7.30 -12 -1 0 15.60 5.30 -12 -1 0 8.40 7.20 -12 1 0 -3.80 6.50 -13 -1 0 -6.30 5.60 -13 -1 0 4.10 6.90 -13 1 0 2.20 7.80 0 -2 0 -0.50 0.50 1 -2 0 211.38 6.00 -1 -2 0 199.88 6.00 1 -2 0 249.58 6.30 -1 2 0 190.78 6.10 1 2 0 244.48 6.30 2 -2 0 62.29 3.30 2 -2 0 72.09 5.20 -2 -2 0 70.59 2.60 -2 -2 0 69.49 3.70 -2 -2 0 66.79 3.20 2 -2 0 67.09 3.30 -2 2 0 65.29 3.30 -2 2 0 68.39 3.40 2 2 0 67.29 3.50 -2 2 0 69.89 3.30 3 -2 0 330.17 9.00 -3 -2 0 322.17 9.10 3 -2 0 325.37 9.20 -3 -2 0 322.87 8.50 -3 2 0 323.77 9.40 -3 2 0 335.87 9.00 3 2 0 315.27 9.40 4 -2 0 347.07 9.60 -4 -2 0 355.46 9.80 -4 -2 0 337.17 9.20 4 -2 0 348.97 9.90 4 2 0 327.87 10.30 -4 2 0 337.37 10.20 5 -2 0 402.56 12.10 5 -2 0 411.46 11.60 -5 -2 0 419.56 11.90 5 2 0 412.66 12.80 -5 2 0 410.86 12.60 6 -2 0 262.17 8.90 -6 -2 0 245.08 8.80 6 -2 0 259.47 8.50 -6 2 0 250.77 10.00 7 -2 0 48.80 4.50 -7 -2 0 55.29 4.90 7 -2 0 41.60 5.30 -7 2 0 43.60 6.10 -8 -2 0 75.39 6.10 8 -2 0 59.69 6.10 8 -2 0 67.39 5.30 -8 2 0 63.29 6.70 9 -2 0 82.39 7.20 9 -2 0 78.99 7.30 -9 2 0 82.89 8.80 -10 -2 0 400.36 14.20 10 -2 0 418.46 14.60 -10 2 0 395.16 16.20 11 -2 0 137.09 9.70 -11 -2 0 151.18 9.50 -11 2 0 142.19 10.80 -12 -2 0 29.70 7.30 -12 -2 0 28.60 5.90 12 -2 0 20.60 6.00 -12 2 0 28.90 7.90 -13 -2 0 6.30 6.00 -13 -2 0 6.40 7.60 -13 2 0 9.20 7.50 0 3 0 -3.30 1.80 1 -3 0 3858.61 90.89 -1 -3 0 4000.60 91.19 -1 -3 0 3756.22 90.89 1 -3 0 3777.62 90.69 -1 3 0 3792.02 90.99 -1 3 0 3827.62 90.89 1 3 0 3801.02 90.99 2 -3 0 1775.32 43.90 -2 -3 0 1818.92 43.30 -2 -3 0 1817.32 44.00 2 -3 0 1836.42 44.10 2 -3 0 1814.02 44.00 -2 3 0 1874.01 44.00 -2 3 0 1778.02 44.10 2 3 0 1877.71 43.30 2 3 0 1783.22 44.20 2 3 0 1850.21 44.00 -3 -3 0 505.25 12.60 -3 -3 0 508.75 13.40 3 -3 0 505.95 13.40 3 -3 0 486.85 13.10 3 3 0 509.15 13.80 -3 3 0 491.35 13.60 -4 -3 0 64.39 3.20 4 -3 0 55.59 3.70 -4 -3 0 55.49 3.60 4 -3 0 59.69 4.10 4 3 0 59.29 4.40 -4 3 0 62.59 4.40 5 -3 0 354.26 10.60 -5 -3 0 355.26 10.90 5 -3 0 354.96 11.00 5 3 0 354.66 11.50 -5 3 0 369.36 11.90 6 -3 0 554.54 15.50 6 -3 0 539.45 15.90 -6 -3 0 567.04 15.80 -6 3 0 587.84 17.00 6 3 0 561.14 16.70 7 -3 0 428.96 13.60 -7 -3 0 446.56 13.30 7 -3 0 439.26 13.00 -7 3 0 436.46 14.50 8 -3 0 3.80 3.00 -8 -3 0 2.40 3.30 8 -3 0 9.30 3.90 -8 3 0 4.70 4.70 -9 -3 0 14.70 4.20 9 -3 0 9.90 4.40 -9 3 0 16.60 5.80 -10 -3 0 1395.76 36.50 10 -3 0 1362.56 35.90 10 -3 0 1394.56 37.00 -10 3 0 1384.06 38.40 11 -3 0 105.09 9.30 -11 -3 0 110.59 9.00 -11 3 0 84.89 9.00 12 -3 0 -1.00 5.70 -12 -3 0 -1.20 5.20 -12 3 0 -2.90 7.10 13 -3 0 18.90 6.80 -13 -3 0 7.90 6.00 -13 3 0 5.20 8.30 1 -4 0 131.69 4.70 1 -4 0 154.38 5.50 1 -4 0 126.99 5.10 -1 -4 0 129.29 4.20 -1 -4 0 129.89 5.00 1 4 0 115.79 5.40 -1 4 0 134.39 5.20 -1 4 0 133.19 5.40 1 4 0 135.99 4.20 -2 -4 0 756.82 18.10 2 -4 0 720.83 18.90 2 -4 0 730.63 18.90 -2 -4 0 723.03 19.00 2 4 0 744.53 19.30 -2 4 0 744.63 19.20 2 4 0 747.13 18.10 3 -4 0 44.90 3.70 -3 -4 0 46.00 3.50 3 -4 0 47.70 3.70 -3 -4 0 51.99 2.50 3 4 0 44.20 3.90 -3 4 0 48.90 4.30 4 -4 0 884.21 23.50 -4 -4 0 908.71 22.40 4 -4 0 926.31 23.30 -4 -4 0 906.41 23.50 -4 -4 0 926.91 22.30 -4 4 0 899.11 23.80 4 4 0 920.21 23.90 -5 -4 0 329.67 9.40 -5 -4 0 336.37 10.60 5 -4 0 338.67 10.30 5 -4 0 326.07 10.60 -5 4 0 325.57 11.30 5 4 0 322.67 11.30 -6 -4 0 694.53 19.10 6 -4 0 711.63 18.90 -6 -4 0 690.63 18.20 -6 4 0 689.13 20.00 -7 -4 0 15.20 3.30 7 -4 0 16.30 3.30 7 -4 0 9.80 3.50 -7 4 0 18.60 4.50 7 4 0 14.00 4.20 -8 -4 0 -2.30 3.90 8 -4 0 1.20 3.20 8 -4 0 2.90 3.70 8 4 0 2.20 4.10 -8 4 0 -2.60 4.20 -9 -4 0 96.19 7.50 9 -4 0 105.69 7.70 9 -4 0 99.19 6.80 -9 4 0 108.79 9.70 10 -4 0 11.10 5.40 -10 -4 0 -3.80 4.30 10 -4 0 6.90 4.00 -10 4 0 4.60 5.90 -11 -4 0 1.20 4.90 11 -4 0 4.30 4.50 -11 -4 0 4.10 4.50 11 -4 0 0.80 5.40 -11 4 0 4.50 7.00 -12 -4 0 181.68 10.40 12 -4 0 199.08 12.10 -12 -4 0 197.38 11.00 -12 4 0 181.98 13.80 -13 -4 0 -0.50 5.70 13 -4 0 -1.20 6.60 -13 -4 0 0.70 6.10 -13 4 0 9.40 8.40 0 5 0 2.20 1.60 0 5 0 1.40 2.20 1 -5 0 677.23 17.90 -1 -5 0 691.03 17.90 -1 -5 0 648.14 16.90 1 -5 0 668.03 17.40 1 5 0 686.93 18.00 -1 5 0 671.13 17.90 1 5 0 697.93 16.90 -2 -5 0 1210.68 29.60 2 -5 0 1207.48 30.60 -2 -5 0 1212.68 30.70 2 -5 0 1243.18 30.60 2 5 0 1281.97 29.70 2 5 0 1228.18 31.00 -2 5 0 1195.38 30.80 3 -5 0 -1.10 2.20 -3 -5 0 3.90 2.50 3 -5 0 2.40 2.40 -3 -5 0 1.80 1.40 3 5 0 5.20 1.50 3 5 0 -0.20 2.60 -3 5 0 5.60 3.00 -4 -5 0 22.70 3.20 4 -5 0 17.00 3.20 -4 -5 0 19.30 2.10 4 -5 0 16.10 3.30 4 5 0 17.40 3.70 -4 5 0 22.30 3.80 -5 -5 0 258.37 7.50 5 -5 0 260.07 9.30 -5 -5 0 256.77 7.70 -5 -5 0 255.87 8.90 5 -5 0 252.37 8.90 -5 5 0 253.27 10.10 5 5 0 253.37 9.60 6 -5 0 159.98 7.40 -6 -5 0 165.88 6.00 -6 -5 0 156.88 7.40 6 -5 0 158.08 7.00 -6 5 0 159.88 8.20 6 5 0 157.88 7.80 -7 -5 0 172.38 7.80 -7 -5 0 161.78 6.50 7 -5 0 159.68 8.30 7 -5 0 157.38 7.30 -7 5 0 169.98 9.10 7 5 0 159.28 8.40 8 -5 0 808.32 23.20 -8 -5 0 783.62 23.10 -8 -5 0 818.92 21.70 -8 5 0 846.22 24.30 8 5 0 846.82 24.50 -9 -5 0 15.30 4.60 9 -5 0 18.50 5.00 9 -5 0 18.30 4.10 -9 -5 0 17.60 3.70 -9 5 0 17.40 6.00 10 -5 0 479.25 15.30 -10 -5 0 475.05 16.10 -10 -5 0 437.66 16.20 10 -5 0 489.25 17.00 -10 5 0 497.95 18.40 -11 -5 0 15.40 4.60 11 -5 0 18.70 5.10 11 -5 0 22.10 6.40 -11 -5 0 6.50 5.30 -11 5 0 16.50 7.40 12 -5 0 5.90 6.40 12 -5 0 11.10 5.30 -12 -5 0 11.90 5.60 -12 -5 0 12.70 5.10 -12 5 0 16.10 7.40 -13 -5 0 18.00 6.70 13 -5 0 16.30 7.60 -13 -5 0 18.40 6.20 -13 5 0 12.20 8.40 0 -6 0 2714.63 66.39 0 -6 0 2678.73 65.69 0 6 0 2844.22 66.69 1 -6 0 199.48 6.90 1 -6 0 193.58 7.30 -1 -6 0 199.88 6.20 -1 -6 0 202.88 7.60 1 6 0 194.88 7.40 -1 6 0 200.78 7.70 1 6 0 210.58 6.90 2 -6 0 28.90 3.30 -2 -6 0 25.00 3.10 2 -6 0 22.80 2.90 -2 -6 0 23.70 2.10 2 6 0 23.20 2.10 -2 6 0 26.30 3.60 2 6 0 20.40 3.30 -3 -6 0 459.85 12.00 3 -6 0 463.65 13.60 -3 -6 0 463.45 13.70 3 -6 0 443.76 13.30 3 6 0 458.25 14.10 -3 6 0 458.45 13.80 3 6 0 482.45 12.10 -4 -6 0 191.58 7.90 -4 -6 0 198.28 6.00 4 -6 0 176.88 7.80 4 -6 0 182.08 8.00 -4 6 0 197.58 8.80 4 6 0 180.18 8.10 -5 -6 0 77.99 5.90 5 -6 0 71.19 5.60 5 -6 0 72.89 6.60 -5 -6 0 70.09 3.80 -5 6 0 71.79 6.10 5 6 0 69.49 7.00 6 -6 0 11.70 4.00 6 -6 0 4.70 3.00 -6 -6 0 5.90 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7 0 40.70 4.40 -2 7 0 53.39 5.20 3 -7 0 841.42 22.90 -3 -7 0 882.11 23.30 3 -7 0 856.61 23.00 -3 -7 0 869.71 21.50 3 7 0 885.61 21.60 -3 7 0 866.71 23.70 3 7 0 835.32 23.40 -4 -7 0 42.10 3.20 4 -7 0 39.70 5.80 4 -7 0 36.50 4.10 -4 -7 0 48.50 5.10 4 7 0 44.80 3.30 -4 7 0 49.90 5.40 5 -7 0 1244.48 32.00 5 -7 0 1248.38 31.50 -5 -7 0 1250.87 29.90 -5 -7 0 1207.78 31.80 5 7 0 1241.08 32.40 -5 7 0 1106.89 33.60 6 -7 0 218.08 9.40 -6 -7 0 227.58 7.40 -6 7 0 242.18 10.50 6 7 0 237.48 10.00 -7 -7 0 44.60 5.10 7 -7 0 37.50 4.60 7 -7 0 35.20 4.90 -7 -7 0 43.30 4.00 7 7 0 34.80 5.50 -7 7 0 42.90 6.00 -8 -7 0 0.30 2.60 -8 -7 0 3.30 4.30 8 -7 0 1.30 3.60 8 -7 0 -5.80 4.20 -8 7 0 -9.10 5.00 8 7 0 -4.10 4.50 9 -7 0 14.50 4.40 9 -7 0 22.40 5.50 -9 -7 0 19.10 5.10 -9 -7 0 20.80 3.60 9 7 0 33.70 6.80 -9 7 0 12.70 6.00 -10 -7 0 61.39 6.20 10 -7 0 57.99 6.00 10 -7 0 45.00 6.80 -10 -7 0 47.90 6.40 10 7 0 49.40 7.90 -10 7 0 44.20 7.70 -11 -7 0 60.49 7.10 11 -7 0 44.10 7.60 11 -7 0 60.29 6.60 -11 7 0 54.29 8.80 -12 -7 0 11.40 4.80 12 -7 0 23.10 6.00 -12 -7 0 14.90 6.50 12 -7 0 20.80 7.30 -12 7 0 9.10 8.10 13 -7 0 21.20 6.80 13 -7 0 27.10 8.10 -13 -7 0 37.80 7.70 -13 -7 0 32.80 5.80 -13 7 0 30.20 9.60 0 -8 0 2702.23 65.79 0 -8 0 2656.83 64.79 0 8 0 2682.53 65.89 1 -8 0 5.80 3.80 -1 -8 0 3.40 2.30 -1 -8 0 0.50 3.60 1 -8 0 0.40 2.90 -1 8 0 -1.50 4.10 1 8 0 -0.10 3.60 -2 -8 0 99.49 4.70 2 -8 0 92.09 6.10 2 -8 0 103.19 7.10 -2 -8 0 101.09 6.50 -2 8 0 89.29 7.50 2 8 0 102.59 6.50 3 -8 0 5.50 3.50 3 -8 0 9.40 3.30 -3 -8 0 8.80 3.50 -3 -8 0 6.80 2.10 -3 8 0 13.30 4.50 -4 -8 0 1261.57 35.90 4 -8 0 1350.66 34.40 -4 -8 0 1374.26 32.50 4 -8 0 1324.87 34.30 4 8 0 1339.57 35.10 -4 8 0 1310.27 35.20 5 -8 0 78.89 6.10 -5 -8 0 68.89 6.40 -5 -8 0 75.49 4.00 5 8 0 79.89 6.50 -5 8 0 76.59 6.70 6 -8 0 -1.50 3.60 6 -8 0 -4.70 3.10 -6 -8 0 6.20 3.90 -6 -8 0 -1.10 2.00 6 8 0 0.50 3.90 -6 8 0 -1.40 4.10 7 -8 0 1.50 3.60 -7 -8 0 0.30 3.90 -7 -8 0 4.90 2.40 7 -8 0 4.20 4.10 7 8 0 5.20 4.40 -7 8 0 -1.10 5.20 -8 -8 0 0.80 4.50 -8 -8 0 5.80 2.80 8 -8 0 8.30 4.10 8 -8 0 5.20 4.80 -8 8 0 8.00 5.40 8 8 0 2.20 5.40 -9 -8 0 99.99 6.10 -9 -8 0 103.69 8.90 9 -8 0 108.09 8.20 9 -8 0 99.79 8.90 9 8 0 117.89 9.70 -9 8 0 101.59 10.90 -10 -8 0 0.10 5.30 10 -8 0 -1.20 5.60 10 -8 0 4.30 4.90 -10 -8 0 -1.40 3.40 -10 8 0 -6.60 6.90 10 8 0 1.90 6.10 -11 -8 0 6.30 3.90 11 -8 0 5.60 6.00 11 -8 0 2.20 5.30 -11 -8 0 3.10 5.80 -11 8 0 13.70 7.90 11 8 0 6.30 6.90 12 -8 0 17.90 6.30 12 -8 0 31.60 7.60 -12 -8 0 37.70 7.20 -12 8 0 11.30 9.00 0 -9 0 -2.00 4.10 0 -9 0 0.50 2.60 0 9 0 -1.10 3.60 -1 -9 0 45.00 4.20 1 -9 0 38.70 5.60 -1 -9 0 40.70 5.60 1 -9 0 43.00 4.10 -1 9 0 37.50 4.80 1 9 0 33.70 4.70 -2 -9 0 0.80 2.30 2 -9 0 -0.40 3.00 2 9 0 -0.60 3.90 -2 9 0 -0.50 3.70 3 -9 0 7.20 3.40 3 -9 0 8.60 4.20 -3 -9 0 13.10 2.40 -3 -9 0 8.70 3.80 3 9 0 9.90 3.80 4 -9 0 -4.50 3.20 4 -9 0 0.30 3.30 -4 -9 0 1.10 2.00 -4 -9 0 0.90 3.40 -4 9 0 3.80 4.20 4 9 0 0.50 3.70 5 -9 0 9.20 3.60 -5 -9 0 7.90 2.20 5 -9 0 5.40 3.60 -5 -9 0 10.40 3.90 -5 9 0 2.00 4.30 5 9 0 0.60 3.90 -6 -9 0 546.35 14.40 6 -9 0 532.25 17.00 6 -9 0 551.24 16.90 -6 -9 0 537.55 17.30 -6 9 0 556.24 18.20 6 9 0 531.45 17.70 7 -9 0 9.10 4.80 7 -9 0 2.80 3.80 -7 -9 0 4.70 4.60 -7 -9 0 1.80 2.30 -7 9 0 1.60 5.00 7 9 0 0.40 5.00 8 -9 0 113.29 9.00 -8 -9 0 106.49 9.20 -8 -9 0 110.99 5.70 8 -9 0 119.49 8.30 -8 9 0 124.39 10.90 8 9 0 109.89 10.00 -9 -9 0 12.10 5.80 9 -9 0 9.50 5.80 -9 -9 0 16.70 3.40 9 -9 0 16.90 5.10 -9 9 0 16.80 7.00 9 9 0 15.60 6.40 -10 -9 0 221.58 8.60 -10 -9 0 213.38 12.10 10 -9 0 217.98 11.00 10 -9 0 203.58 12.00 -10 9 0 217.68 14.20 10 9 0 206.08 12.90 11 -9 0 -0.50 6.10 -11 -9 0 1.10 3.70 -11 -9 0 8.50 6.60 11 -9 0 6.30 5.60 -11 9 0 5.40 8.00 11 9 0 -3.70 6.70 -12 -9 0 -0.70 6.90 -12 -9 0 2.10 4.40 12 -9 0 -8.80 6.60 12 -9 0 2.70 6.10 -12 9 0 -2.40 8.40 0 -10 0 471.65 15.20 0 -10 0 471.25 13.80 0 10 0 469.65 15.40 1 -10 0 11.60 3.40 1 -10 0 4.80 4.00 -1 -10 0 8.60 3.90 -1 -10 0 2.20 2.60 -1 10 0 4.50 3.80 1 10 0 2.80 3.70 2 -10 0 33.90 4.70 -2 -10 0 32.20 3.20 -2 -10 0 33.20 4.70 2 -10 0 33.00 4.40 -2 10 0 38.30 5.20 2 10 0 35.80 4.80 -3 -10 0 100.99 5.00 3 -10 0 110.09 6.50 3 -10 0 100.29 7.60 -3 -10 0 108.99 7.10 -3 10 0 83.69 7.20 3 10 0 99.29 7.10 -4 -10 0 211.48 9.40 4 -10 0 202.28 8.80 4 -10 0 187.78 9.00 -4 -10 0 197.88 6.90 -4 10 0 194.68 9.70 4 10 0 200.78 10.00 -5 -10 0 29.60 4.70 -5 -10 0 30.80 2.90 5 -10 0 21.70 4.60 5 -10 0 23.70 4.50 5 10 0 30.30 5.10 -5 10 0 18.70 5.20 6 -10 0 12.30 4.70 -6 -10 0 18.20 2.70 -6 -10 0 18.60 4.80 6 -10 0 9.80 4.60 -6 10 0 18.90 5.50 6 10 0 12.90 4.90 7 -10 0 13.30 5.00 7 -10 0 19.60 5.60 -7 -10 0 18.00 5.00 -7 -10 0 19.00 2.80 -7 10 0 21.70 6.70 7 10 0 16.90 6.00 -8 -10 0 0.50 5.10 8 -10 0 -0.60 4.50 -8 -10 0 -2.00 2.60 8 -10 0 -0.70 5.70 -8 10 0 0.90 5.90 8 10 0 -0.60 5.70 9 -10 0 191.58 12.20 -9 -10 0 187.78 11.50 -9 -10 0 191.08 7.40 9 -10 0 194.98 10.70 9 10 0 186.08 12.10 -9 10 0 191.18 12.40 -10 -10 0 115.69 10.70 10 -10 0 107.39 9.60 10 -10 0 101.39 9.50 -10 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0 146.79 9.10 -6 -11 0 141.19 9.60 6 11 0 126.19 9.40 -6 11 0 138.69 10.00 -7 -11 0 77.19 4.90 7 -11 0 67.09 6.70 7 -11 0 59.59 6.90 -7 -11 0 54.49 6.60 -7 11 0 88.69 8.90 7 11 0 80.49 8.80 8 -11 0 267.87 12.90 -8 -11 0 272.77 13.30 -8 -11 0 270.27 8.80 8 -11 0 272.07 12.50 8 11 0 274.57 13.50 -8 11 0 266.87 14.60 -9 -11 0 80.59 8.10 -9 -11 0 94.79 5.60 9 -11 0 86.79 9.30 9 -11 0 88.49 8.60 9 11 0 90.59 9.40 -9 11 0 100.19 10.10 -10 -11 0 67.89 8.40 -10 -11 0 54.49 5.20 10 -11 0 60.89 7.20 10 -11 0 52.89 8.00 -10 11 0 44.90 9.00 10 11 0 63.99 9.60 -11 -11 0 75.59 5.90 11 -11 0 83.89 9.50 -11 -11 0 78.69 9.10 11 -11 0 83.59 8.50 -11 11 0 53.99 9.70 11 11 0 76.49 10.60 0 -12 0 4.00 4.00 0 -12 0 8.20 4.50 0 12 0 6.00 4.30 1 -12 0 61.39 5.60 1 -12 0 67.49 6.80 -1 -12 0 66.29 5.40 -1 -12 0 55.19 6.10 1 12 0 86.79 8.10 -1 12 0 64.79 7.10 2 -12 0 72.79 6.80 -2 -12 0 58.89 6.20 2 -12 0 50.49 5.10 -2 -12 0 76.69 5.40 -2 12 0 66.39 7.30 2 12 0 76.89 7.30 -3 -12 0 651.83 20.20 3 -12 0 624.84 19.60 3 -12 0 614.94 18.70 -3 -12 0 634.14 17.20 3 12 0 601.94 19.80 -3 12 0 620.94 19.80 4 -12 0 325.57 13.30 4 -12 0 312.97 12.00 -4 -12 0 311.07 13.50 -4 -12 0 330.47 10.10 -4 12 0 304.97 13.20 4 12 0 299.77 13.00 -5 -12 0 149.09 6.50 5 -12 0 168.08 9.20 5 -12 0 150.08 9.30 -5 -12 0 159.78 9.80 5 12 0 145.89 10.60 -5 12 0 160.08 11.30 6 -12 0 68.19 7.00 -6 -12 0 63.39 4.80 6 -12 0 68.99 7.10 -6 -12 0 68.79 7.50 6 12 0 67.89 7.40 -6 12 0 76.39 8.40 -7 -12 0 4.40 2.90 7 -12 0 3.30 5.30 -7 -12 0 7.10 5.40 7 -12 0 10.60 5.70 7 12 0 8.80 5.90 -7 12 0 -0.50 6.80 8 -12 0 1.80 5.70 -8 -12 0 0.70 2.80 -8 -12 0 0.10 5.70 8 -12 0 4.30 5.00 -8 12 0 -1.00 7.30 8 12 0 0.40 6.70 -9 -12 0 51.69 5.00 -9 -12 0 50.59 7.60 9 -12 0 42.00 7.50 9 -12 0 58.19 7.50 -9 12 0 44.80 9.10 9 12 0 41.10 7.90 10 -12 0 6.30 6.20 -10 -12 0 15.60 3.10 10 -12 0 19.10 7.60 -10 -12 0 7.50 6.90 -10 12 0 10.70 8.50 10 12 0 10.80 7.70 -11 -12 0 4.30 3.10 11 -12 0 3.80 8.10 11 -12 0 6.70 6.70 -11 -12 0 6.50 7.60 11 12 0 2.00 7.80 -11 12 0 -11.60 9.10 0 -13 0 3.80 4.90 0 -13 0 5.10 3.70 0 13 0 -1.60 4.90 -1 -13 0 11.00 5.30 1 -13 0 13.00 5.20 -1 -13 0 15.90 3.90 1 -13 0 12.00 4.20 -1 13 0 12.00 5.30 1 13 0 15.00 5.10 -2 -13 0 216.18 8.30 2 -13 0 197.38 9.40 2 -13 0 200.78 10.70 -2 -13 0 209.68 10.90 2 13 0 202.28 10.70 -2 13 0 198.08 10.70 -3 -13 0 218.88 11.90 3 -13 0 223.08 11.30 -3 -13 0 227.28 8.60 3 -13 0 215.48 10.00 -3 13 0 222.18 11.30 3 13 0 213.48 11.10 -4 -13 0 96.49 8.80 4 -13 0 82.49 7.60 -4 -13 0 89.99 5.90 4 -13 0 69.19 7.20 4 13 0 81.89 8.10 -4 13 0 85.99 8.90 -5 -13 0 92.99 5.70 -5 -13 0 80.99 7.90 5 -13 0 98.19 9.60 5 -13 0 100.19 8.40 -5 13 0 97.99 10.70 5 13 0 92.19 9.20 -6 -13 0 192.38 11.20 -6 -13 0 177.58 7.20 6 -13 0 187.98 11.50 6 -13 0 180.68 10.60 6 13 0 181.78 11.40 -6 13 0 164.48 11.60 7 -13 0 67.39 7.70 -7 -13 0 69.39 5.20 7 -13 0 75.19 7.60 -7 -13 0 68.19 8.30 -7 13 0 68.49 8.80 7 13 0 63.19 8.10 8 -13 0 71.99 8.30 -8 -13 0 86.19 9.00 8 -13 0 87.99 8.30 -8 -13 0 67.69 5.10 -8 13 0 74.79 9.30 8 13 0 72.99 8.90 9 -13 0 87.19 9.20 -9 -13 0 95.59 9.60 -9 -13 0 99.49 5.30 9 -13 0 126.99 10.60 9 13 0 90.39 9.80 -9 13 0 95.09 10.30 -10 -13 0 11.60 2.70 10 -13 0 11.40 8.00 10 -13 0 16.40 6.70 -10 -13 0 16.90 7.50 -10 13 0 10.60 9.10 10 13 0 18.20 8.30 0 -14 0 85.99 7.10 0 -14 0 98.89 9.40 0 14 0 86.69 9.40 1 -14 0 3.10 5.50 -1 -14 0 -0.10 3.70 1 -14 0 -0.20 4.30 -1 -14 0 -1.40 5.50 -1 14 0 2.60 4.90 1 14 0 -3.60 4.90 2 -14 0 447.86 16.40 -2 -14 0 440.06 14.10 -2 -14 0 430.16 16.40 2 -14 0 419.46 15.10 2 14 0 426.36 16.70 -2 14 0 456.95 16.40 3 -14 0 71.29 7.50 3 -14 0 66.99 6.40 -3 -14 0 60.19 7.10 -3 -14 0 64.29 5.90 3 14 0 59.09 7.20 -3 14 0 63.29 7.60 -4 -14 0 27.40 6.50 -4 -14 0 28.20 3.90 4 -14 0 22.10 5.80 4 -14 0 19.60 6.00 -4 14 0 22.70 6.20 4 14 0 20.50 6.10 5 -14 0 -2.60 5.20 -5 -14 0 0.30 3.20 5 -14 0 2.30 5.50 -5 -14 0 11.50 6.50 5 14 0 2.50 5.70 -5 14 0 -1.40 6.20 6 -14 0 17.20 6.00 -6 -14 0 9.60 6.70 -6 -14 0 11.70 3.30 6 -14 0 11.00 5.70 6 14 0 9.20 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7.00 -2 -14 -7 11.20 6.10 2 -14 7 17.10 6.90 -2 14 -7 14.20 4.50 2 14 7 10.50 6.10 -3 -14 -7 108.39 10.80 3 -14 7 83.19 9.20 -3 -14 -7 73.59 9.50 -3 14 -7 107.49 8.30 3 14 7 104.69 11.30 -4 -14 -7 11.80 6.30 4 -14 7 11.10 7.30 -4 -14 -7 20.20 8.70 4 14 7 14.90 6.60 -4 14 -7 19.20 5.00 -5 -14 -7 87.39 9.10 -5 -14 -7 87.89 10.50 5 -14 7 122.99 12.60 5 14 7 96.49 10.30 -5 14 -7 123.19 10.10 6 -14 7 23.50 8.40 -6 -14 -7 27.70 7.70 -6 -14 -7 24.40 9.50 6 14 7 31.50 7.80 -6 14 -7 24.60 5.50 -8 -15 7 -5.80 6.50 8 -15 -7 0.50 7.80 8 -15 -7 -1.60 6.40 -8 15 7 -4.30 9.00 8 15 -7 5.20 7.70 7 -15 -7 -0.20 6.40 -7 -15 7 0.60 6.40 7 -15 -7 -9.00 7.70 -7 15 7 2.20 9.50 7 15 -7 6.90 7.20 6 -15 -7 126.79 12.10 -6 -15 7 125.19 11.50 6 -15 -7 107.69 11.50 6 15 -7 109.69 10.50 -6 15 7 134.79 15.00 -5 -15 7 -0.50 6.30 5 -15 -7 1.30 6.90 5 -15 -7 4.60 7.20 5 15 -7 10.60 6.20 -5 15 7 -1.00 7.80 5 15 -7 4.20 2.00 5 15 -7 1.10 3.30 4 -15 -7 1.80 6.30 4 -15 -7 4.00 6.80 -4 -15 7 6.20 6.30 4 15 -7 2.60 3.50 4 15 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