data_130910_s2_lss _audit_creation_date 2013-09-10 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H30 O3' _chemical_formula_sum 'C24 H30 O3' _chemical_formula_weight 366.48 _chemical_absolute_configuration ? _chemical_melting_point ? _chemical_oxdiff_formula C12H20N2O3 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.2379(5) _cell_length_b 12.6069(8) _cell_length_c 12.8921(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1989.01(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1680 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.9883 _cell_measurement_theta_min 3.1539 _exptl_absorpt_coefficient_mu 0.079 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.96824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_unetI/netI 0.0636 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 5761 _diffrn_reflns_point_group_measured_fraction_full 0.943 _diffrn_reflns_point_group_measured_fraction_max 0.934 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 3.160 _diffrn_ambient_temperature 293.15 _diffrn_detector_area_resol_mean 16.0874 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -3.00 30.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 19.1580 88.0000 134.0000 33 #__ type_ start__ end____ width___ exp.time_ 2 omega -50.00 34.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 19.1580 -57.0000 -180.0000 84 #__ type_ start__ end____ width___ exp.time_ 3 omega 56.00 89.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 19.1580 77.0000 -60.0000 33 ; _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0122935000 _diffrn_orient_matrix_UB_12 -0.0499709000 _diffrn_orient_matrix_UB_13 -0.0224667000 _diffrn_orient_matrix_UB_21 0.0507363000 _diffrn_orient_matrix_UB_22 0.0007104000 _diffrn_orient_matrix_UB_23 -0.0265589000 _diffrn_orient_matrix_UB_31 0.0251619000 _diffrn_orient_matrix_UB_32 -0.0258570000 _diffrn_orient_matrix_UB_33 0.0426183000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.645 _reflns_Friedel_fraction_full 0.870 _reflns_Friedel_fraction_max 0.848 _reflns_number_gt 2673 _reflns_number_total 3794 _reflns_odcompleteness_completeness 99.70 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL-2012, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELXS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.167 _refine_diff_density_min -0.160 _refine_diff_density_rms 0.036 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack -3(2) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 246 _refine_ls_number_reflns 3794 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0522 _refine_ls_restrained_S_all 1.019 _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^)+(0.0463P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1013 _refine_ls_wR_factor_ref 0.1191 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C7(H7), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16), C18(H18) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C8(H8A,H8B), C12(H12A,H12B), C13(H13A,H13B), C17(H17A,H17B), C20(H20A,H20B), C21(H21A,H21B) 2.c Aromatic/amide H refined with riding coordinates: C5(H5) 2.d Idealised Me refined as rotating group: C23(H23A,H23B,H23C), C24(H24A,H24B,H24C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 O1 O 0.79634(18) 0.6978(2) 0.61614(19) 0.0547(7) Uani 1 1 d . . . . . O2 O 0.0469(2) 0.3161(3) 0.3376(2) 0.1128(14) Uani 1 1 d . . . . . O3 O 0.8218(2) 0.7388(3) 0.7821(2) 0.0799(9) Uani 1 1 d . . . . . C1 C 0.3649(2) 0.4005(2) 0.4252(2) 0.0342(7) Uani 1 1 d . . . . . C2 C 0.2720(3) 0.3912(3) 0.5050(2) 0.0429(8) Uani 1 1 d . . . . . H2A H 0.3020 0.3644 0.5695 0.051 Uiso 1 1 calc R U . . . H2B H 0.2430 0.4615 0.5185 0.051 Uiso 1 1 calc R U . . . C3 C 0.1793(3) 0.3197(3) 0.4717(3) 0.0598(11) Uani 1 1 d . . . . . H3A H 0.2041 0.2467 0.4731 0.072 Uiso 1 1 calc R U . . . H3B H 0.1198 0.3264 0.5211 0.072 Uiso 1 1 calc R U . . . C4 C 0.1375(3) 0.3445(3) 0.3661(3) 0.0614(11) Uani 1 1 d . . . . . C5 C 0.2102(3) 0.4030(3) 0.2982(3) 0.0476(9) Uani 1 1 d . . . . . H5 H 0.1826 0.4249 0.2345 0.057 Uiso 1 1 calc R U . . . C6 C 0.3144(3) 0.4281(2) 0.3201(2) 0.0375(8) Uani 1 1 d . . . . . C7 C 0.3782(3) 0.4880(3) 0.2433(2) 0.0458(9) Uani 1 1 d . . . . . H7 H 0.3341 0.5327 0.1973 0.055 Uiso 1 1 calc R U . . . C8 C 0.4832(3) 0.4459(4) 0.1941(3) 0.0604(11) Uani 1 1 d . . . . . H8A H 0.5090 0.3766 0.2160 0.072 Uiso 1 1 calc R U . . . H8B H 0.4966 0.4626 0.1218 0.072 Uiso 1 1 calc R U . . . C9 C 0.4890(3) 0.5342(3) 0.2706(2) 0.0475(9) Uani 1 1 d . . . . . H9 H 0.5043 0.6043 0.2412 0.057 Uiso 1 1 calc R U . . . C10 C 0.5340(2) 0.5153(3) 0.3790(2) 0.0375(8) Uani 1 1 d . . . . . H10 H 0.5839 0.4545 0.3773 0.045 Uiso 1 1 calc R U . . . C11 C 0.4416(2) 0.4927(3) 0.4576(2) 0.0353(7) Uani 1 1 d . . . . . H11 H 0.3959 0.5565 0.4582 0.042 Uiso 1 1 calc R U . . . C12 C 0.4862(3) 0.4814(3) 0.5681(2) 0.0432(8) Uani 1 1 d . . . . . H12A H 0.5321 0.4188 0.5717 0.052 Uiso 1 1 calc R U . . . H12B H 0.4255 0.4712 0.6155 0.052 Uiso 1 1 calc R U . . . C13 C 0.5526(3) 0.5784(3) 0.6030(2) 0.0438(9) Uani 1 1 d . . . . . H13A H 0.5057 0.6403 0.6054 0.053 Uiso 1 1 calc R U . . . H13B H 0.5813 0.5663 0.6721 0.053 Uiso 1 1 calc R U . . . C14 C 0.6466(3) 0.5981(3) 0.5279(2) 0.0395(8) Uani 1 1 d . . . . . C15 C 0.5958(2) 0.6127(3) 0.4190(2) 0.0410(8) Uani 1 1 d . . . . . H15 H 0.5385 0.6659 0.4295 0.049 Uiso 1 1 calc R U . . . C16 C 0.6816(3) 0.6702(3) 0.3547(3) 0.0616(11) Uani 1 1 d . . . . . H16 H 0.6570 0.7098 0.2936 0.074 Uiso 1 1 calc R U . . . C17 C 0.7997(3) 0.6427(4) 0.3622(3) 0.0793(15) Uani 1 1 d . . . . . H17A H 0.8472 0.6651 0.3061 0.095 Uiso 1 1 calc R U . . . H17B H 0.8187 0.5750 0.3931 0.095 Uiso 1 1 calc R U . . . C18 C 0.7542(3) 0.7270(4) 0.4324(3) 0.0660(12) Uani 1 1 d . . . . . H18 H 0.7740 0.8006 0.4169 0.079 Uiso 1 1 calc R U . . . C19 C 0.7094(3) 0.7044(3) 0.5380(3) 0.0484(9) Uani 1 1 d . . . . . C20 C 0.6407(3) 0.7981(3) 0.5773(3) 0.0580(10) Uani 1 1 d . . . . . H20A H 0.6657 0.8643 0.5472 0.070 Uiso 1 1 calc R U . . . H20B H 0.5641 0.7883 0.5605 0.070 Uiso 1 1 calc R U . . . C21 C 0.6581(3) 0.7975(3) 0.6935(3) 0.0604(11) Uani 1 1 d . . . . . H21A H 0.6608 0.8691 0.7208 0.072 Uiso 1 1 calc R U . . . H21B H 0.6004 0.7586 0.7284 0.072 Uiso 1 1 calc R U . . . C22 C 0.7665(3) 0.7426(3) 0.7063(3) 0.0563(10) Uani 1 1 d . . . . . C23 C 0.4253(3) 0.2930(3) 0.4193(3) 0.0477(9) Uani 1 1 d . . . . . H23A H 0.3771 0.2401 0.3914 0.072 Uiso 1 1 calc R U . . . H23B H 0.4481 0.2722 0.4875 0.072 Uiso 1 1 calc R U . . . H23C H 0.4881 0.2999 0.3752 0.072 Uiso 1 1 calc R U . . . C24 C 0.7267(3) 0.5031(3) 0.5403(3) 0.0536(10) Uani 1 1 d . . . . . H24A H 0.7162 0.4540 0.4843 0.080 Uiso 1 1 calc R U . . . H24B H 0.7128 0.4679 0.6051 0.080 Uiso 1 1 calc R U . . . H24C H 0.8006 0.5286 0.5394 0.080 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 O1 0.0441(13) 0.0643(17) 0.0557(15) -0.0089(14) -0.0091(12) -0.0049(13) O2 0.0645(18) 0.181(4) 0.093(2) 0.033(2) -0.0294(18) -0.063(2) O3 0.0808(19) 0.091(2) 0.0675(18) -0.0193(19) -0.0297(16) 0.0069(18) C1 0.0353(15) 0.0334(17) 0.0338(16) 0.0019(15) -0.0015(14) 0.0006(15) C2 0.0389(18) 0.047(2) 0.0423(18) 0.0028(18) -0.0015(15) -0.0073(18) C3 0.049(2) 0.074(3) 0.057(2) 0.010(2) -0.0038(19) -0.019(2) C4 0.047(2) 0.073(3) 0.065(3) 0.002(2) -0.009(2) -0.015(2) C5 0.0445(19) 0.051(2) 0.048(2) 0.0033(19) -0.0133(16) -0.0039(19) C6 0.0417(18) 0.0319(17) 0.0389(18) -0.0017(15) -0.0028(15) 0.0035(16) C7 0.0437(18) 0.057(2) 0.0369(17) 0.0060(18) -0.0047(16) 0.0007(19) C8 0.053(2) 0.094(3) 0.0335(18) -0.009(2) 0.0036(17) -0.002(2) C9 0.048(2) 0.061(2) 0.0329(17) 0.0094(18) -0.0018(16) -0.0134(19) C10 0.0353(16) 0.0423(18) 0.0349(16) 0.0027(16) -0.0001(14) -0.0031(17) C11 0.0360(16) 0.0335(18) 0.0364(16) -0.0009(15) 0.0015(14) -0.0002(15) C12 0.0482(19) 0.047(2) 0.0338(16) 0.0000(17) -0.0006(15) -0.0106(18) C13 0.0495(19) 0.045(2) 0.0369(18) -0.0017(17) -0.0044(15) -0.0109(18) C14 0.0405(18) 0.0398(19) 0.0383(17) 0.0019(16) -0.0033(15) -0.0068(17) C15 0.0406(17) 0.044(2) 0.0382(17) 0.0033(18) 0.0014(15) -0.0075(18) C16 0.067(2) 0.076(3) 0.042(2) 0.011(2) -0.0001(19) -0.031(2) C17 0.060(3) 0.117(4) 0.061(3) 0.006(3) 0.014(2) -0.029(3) C18 0.066(2) 0.073(3) 0.058(2) 0.004(2) 0.000(2) -0.030(2) C19 0.0436(19) 0.052(2) 0.050(2) 0.001(2) -0.0063(17) -0.0117(19) C20 0.061(2) 0.039(2) 0.074(3) 0.004(2) -0.014(2) -0.009(2) C21 0.058(2) 0.050(2) 0.073(3) -0.013(2) -0.006(2) -0.003(2) C22 0.057(2) 0.050(2) 0.062(2) -0.008(2) -0.009(2) -0.012(2) C23 0.050(2) 0.040(2) 0.053(2) -0.0026(19) -0.0097(17) 0.0079(18) C24 0.055(2) 0.051(2) 0.055(2) -0.002(2) -0.0126(18) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C19 1.468(4) . ? O1 C22 1.342(4) . ? O2 C4 1.223(4) . ? O3 C22 1.191(4) . ? C1 C2 1.538(4) . ? C1 C6 1.530(4) . ? C1 C11 1.553(4) . ? C1 C23 1.545(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C3 1.511(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.487(5) . ? C4 C5 1.450(5) . ? C5 H5 0.9300 . ? C5 C6 1.343(4) . ? C6 C7 1.469(4) . ? C7 H7 0.9800 . ? C7 C8 1.529(5) . ? C7 C9 1.517(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C9 1.489(5) . ? C9 H9 0.9800 . ? C9 C10 1.522(4) . ? C10 H10 0.9800 . ? C10 C11 1.545(4) . ? C10 C15 1.531(4) . ? C11 H11 0.9800 . ? C11 C12 1.532(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C13 1.535(4) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C13 C14 1.525(4) . ? C14 C15 1.546(4) . ? C14 C19 1.551(5) . ? C14 C24 1.556(5) . ? C15 H15 0.9800 . ? C15 C16 1.521(4) . ? C16 H16 0.9800 . ? C16 C17 1.490(6) . ? C16 C18 1.519(5) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C18 1.502(6) . ? C18 H18 0.9800 . ? C18 C19 1.495(5) . ? C19 C20 1.536(5) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 C21 1.513(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 C22 1.505(5) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 C22 O1 C19 111.9(3) . . ? C2 C1 C11 108.9(2) . . ? C2 C1 C23 108.6(3) . . ? C6 C1 C2 108.2(2) . . ? C6 C1 C11 108.2(2) . . ? C6 C1 C23 110.5(3) . . ? C23 C1 C11 112.4(2) . . ? C1 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C3 C2 C1 114.2(3) . . ? C3 C2 H2A 108.7 . . ? C3 C2 H2B 108.7 . . ? C2 C3 H3A 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C4 C3 C2 113.1(3) . . ? C4 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? O2 C4 C3 121.7(4) . . ? O2 C4 C5 121.6(4) . . ? C5 C4 C3 116.7(3) . . ? C4 C5 H5 117.4 . . ? C6 C5 C4 125.1(3) . . ? C6 C5 H5 117.4 . . ? C5 C6 C1 121.0(3) . . ? C5 C6 C7 119.0(3) . . ? C7 C6 C1 119.9(3) . . ? C6 C7 H7 114.3 . . ? C6 C7 C8 123.2(3) . . ? C6 C7 C9 121.1(3) . . ? C8 C7 H7 114.3 . . ? C9 C7 H7 114.3 . . ? C9 C7 C8 58.5(2) . . ? C7 C8 H8A 117.7 . . ? C7 C8 H8B 117.7 . . ? H8A C8 H8B 114.9 . . ? C9 C8 C7 60.3(2) . . ? C9 C8 H8A 117.7 . . ? C9 C8 H8B 117.7 . . ? C7 C9 H9 115.3 . . ? C7 C9 C10 118.5(3) . . ? C8 C9 C7 61.1(2) . . ? C8 C9 H9 115.3 . . ? C8 C9 C10 120.5(3) . . ? C10 C9 H9 115.3 . . ? C9 C10 H10 109.1 . . ? C9 C10 C11 111.5(2) . . ? C9 C10 C15 111.3(3) . . ? C11 C10 H10 109.1 . . ? C15 C10 H10 109.1 . . ? C15 C10 C11 106.8(2) . . ? C1 C11 H11 105.8 . . ? C10 C11 C1 113.9(2) . . ? C10 C11 H11 105.8 . . ? C12 C11 C1 113.3(3) . . ? C12 C11 C10 111.5(2) . . ? C12 C11 H11 105.8 . . ? C11 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? C11 C12 C13 112.8(3) . . ? H12A C12 H12B 107.8 . . ? C13 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? C12 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? H13A C13 H13B 108.2 . . ? C14 C13 C12 110.1(3) . . ? C14 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? C13 C14 C15 107.0(3) . . ? C13 C14 C19 117.5(3) . . ? C13 C14 C24 106.5(3) . . ? C15 C14 C19 100.0(3) . . ? C15 C14 C24 116.0(3) . . ? C19 C14 C24 110.2(3) . . ? C10 C15 C14 114.1(3) . . ? C10 C15 H15 104.0 . . ? C14 C15 H15 104.0 . . ? C16 C15 C10 122.7(3) . . ? C16 C15 C14 105.9(3) . . ? C16 C15 H15 104.0 . . ? C15 C16 H16 118.0 . . ? C17 C16 C15 121.5(4) . . ? C17 C16 H16 118.0 . . ? C17 C16 C18 59.9(3) . . ? C18 C16 C15 105.6(3) . . ? C18 C16 H16 118.0 . . ? C16 C17 H17A 117.7 . . ? C16 C17 H17B 117.7 . . ? C16 C17 C18 61.0(3) . . ? H17A C17 H17B 114.8 . . ? C18 C17 H17A 117.7 . . ? C18 C17 H17B 117.7 . . ? C16 C18 H18 117.1 . . ? C17 C18 C16 59.1(3) . . ? C17 C18 H18 117.1 . . ? C19 C18 C16 107.2(3) . . ? C19 C18 C17 123.4(4) . . ? C19 C18 H18 117.1 . . ? O1 C19 C14 111.6(3) . . ? O1 C19 C18 111.7(3) . . ? O1 C19 C20 102.3(3) . . ? C18 C19 C14 105.6(3) . . ? C18 C19 C20 110.8(3) . . ? C20 C19 C14 114.9(3) . . ? C19 C20 H20A 110.9 . . ? C19 C20 H20B 110.9 . . ? H20A C20 H20B 108.9 . . ? C21 C20 C19 104.2(3) . . ? C21 C20 H20A 110.9 . . ? C21 C20 H20B 110.9 . . ? C20 C21 H21A 111.0 . . ? C20 C21 H21B 111.0 . . ? H21A C21 H21B 109.0 . . ? C22 C21 C20 103.6(3) . . ? C22 C21 H21A 111.0 . . ? C22 C21 H21B 111.0 . . ? O1 C22 C21 109.8(3) . . ? O3 C22 O1 122.6(4) . . ? O3 C22 C21 127.6(4) . . ? C1 C23 H23A 109.5 . . ? C1 C23 H23B 109.5 . . ? C1 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C14 C24 H24A 109.5 . . ? C14 C24 H24B 109.5 . . ? C14 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _shelx_estimated_absorpt_T_max 0.984 _shelx_estimated_absorpt_T_min 0.977 _shelx_hkl_checksum 23412 _shelx_hkl_file ; 0 0 -2 63049.2 1394.29 2 0 0 -2 62838.2 1232.61 1 0 0 2 64320.2 1396.88 2 0 0 3 24.9004 72.8007 2 0 0 -3 21.9439 42.0495 1 0 0 -3 177.653 91.0756 2 0 0 4 2575.12 289.806 2 0 0 -4 2665.15 287.831 2 0 0 -4 3173.98 224.732 1 0 0 -5-15.8422 65.4804 1 0 0 5 85.9670 126.038 2 0 0 -5 217.166 126.142 2 0 0 -6 42747.7 1197.73 1 0 0 6 43335.6 1547.19 2 0 0 -7-11.3095 72.8664 1 0 0 7 159.825 182.472 2 0 0 -8 10273.8 594.980 1 0 0 8 11313.5 837.870 2 0 0 9 109.963 191.577 2 0 0 -9 85.0359 96.2468 1 0 0 10 843.073 309.798 2 0 0 11 591.389 313.885 2 0 0 12 4032.08 639.592 2 0 0 13 404.579 250.352 2 0 0 14 322.440 293.050 2 0 0 15-187.442 308.089 2 0 0 16 231.734 280.195 2 0 1 -2 167786. 3095.32 2 0 1 2 163154. 3146.51 2 0 -1 -2 163028. 3141.96 2 0 1 -3 24170.9 828.773 2 0 1 3 24978.9 713.418 1 0 1 3 25106.2 860.082 2 0 -1 -3 25251.3 867.493 2 0 -1 3 25898.9 840.433 2 0 1 4 45559.7 1404.74 2 0 1 -4 47930.2 1386.00 2 0 -1 4 46307.0 1372.46 2 0 1 4 46589.3 1163.17 1 0 -1 -4 46174.3 1418.09 2 0 1 -5 59482.9 1714.50 2 0 -1 -5 57541.5 1730.88 2 0 1 5 56997.0 1728.91 2 0 1 5 54252.3 1395.45 1 0 -1 5 56258.8 1688.52 2 0 -1 6 5836.23 517.724 2 0 1 6 5543.22 362.862 1 0 1 -6 5345.44 358.679 1 0 1 6 4958.94 492.708 2 0 -1 7 9706.04 720.748 2 0 1 7 10291.5 766.386 2 0 1 -7 9667.46 543.173 1 0 -1 8-207.157 192.823 2 0 1 8-19.3094 184.087 2 0 1 -8-90.5789 90.6015 1 0 1 -9 99.3245 125.924 1 0 -1 9 406.063 208.172 2 0 1 9 83.0004 152.665 2 0 -1 10 665.736 275.289 2 0 1 -10 906.253 208.987 1 0 1 10 897.645 298.624 2 0 -1 11 1638.48 352.259 2 0 1 11 2674.66 517.295 2 0 1 -11 2079.39 309.246 1 0 1 12 5090.56 768.492 2 0 -1 12 5480.34 737.732 2 0 -1 13 2643.52 546.845 2 0 1 13 2902.22 605.088 2 0 -1 14-194.813 285.487 2 0 1 14-141.381 191.908 2 0 1 15 35.2253 278.726 2 0 1 16-570.684 350.033 2 0 2 0 22005.9 637.679 3 0 -2 -1 117708. 2303.61 3 0 2 1 118101. 2367.20 2 0 -2 -2 4657.12 326.899 2 0 2 2 4467.14 319.588 2 0 2 3 5309.87 390.820 2 0 2 -3 5131.14 362.937 2 0 -2 -3 5101.27 386.892 2 0 -2 -4 37675.6 1278.67 2 0 2 -4 40090.8 1248.60 2 0 2 4 36596.0 1278.58 2 0 2 5 746.059 155.381 1 0 2 5 695.393 206.306 2 0 2 -5 970.113 204.256 2 0 2 6 3569.10 329.214 1 0 2 6 3093.85 404.428 2 0 2 7 14142.6 922.491 2 0 2 7 13977.1 699.297 1 0 -2 7 14189.8 890.763 2 0 2 8 1498.66 338.987 2 0 2 8 1932.76 251.342 1 0 -2 8 2230.31 399.078 2 0 2 -9 90.8830 86.6982 1 0 -2 9-134.816 131.925 2 0 2 9 71.7118 161.477 2 0 -2 10 2358.98 445.247 2 0 2 -10 2086.05 304.269 1 0 2 10 2460.39 465.636 2 0 2 -11 13463.1 798.627 1 0 2 11 15281.9 1196.45 2 0 2 12 201.247 241.284 2 0 2 -12 66.9295 122.582 1 0 2 13 2185.26 525.596 2 0 2 14 6742.46 926.422 2 0 2 15 2162.63 569.462 2 0 2 16 2603.14 655.824 2 0 3 0 75.5027 100.364 3 0 3 1 18338.2 668.904 3 0 -3 -1 19461.2 691.149 3 0 3 2 387170. 7062.69 2 0 -3 -2 389641. 7087.97 2 0 3 3 1375.00 214.752 2 0 -3 -3 1656.68 235.365 2 0 -3 -4 2115.26 297.992 2 0 3 4 2328.97 311.853 2 0 3 -4 2182.74 281.961 2 0 3 5 2134.78 328.261 2 0 3 6 10700.8 758.418 2 0 3 6 11060.4 631.976 1 0 3 7 1243.87 288.892 2 0 3 7 1780.62 265.028 1 0 3 8 679.852 250.343 2 0 3 9 8365.42 830.900 2 0 3 10 20741.6 1375.90 2 0 3 -10 19974.3 968.544 1 0 3 11 2442.82 517.981 2 0 3 -11 1963.07 310.343 1 0 3 12 4803.39 722.824 2 0 3 -12 4746.88 490.768 1 0 3 13 371.979 183.094 2 0 3 14 450.603 309.484 2 0 3 15 5664.26 928.828 2 0 4 0 168487. 3440.78 3 0 4 1 16807.9 710.818 3 0 -4 -1 16935.2 716.513 3 0 4 2 22020.0 935.044 2 0 -4 -2 23243.9 887.912 3 0 4 3 22735.7 996.713 2 0 -4 -3 24486.7 1032.57 2 0 4 4 52870.0 1736.41 2 0 4 5 1083.45 240.692 2 0 4 6 49537.5 1841.56 2 0 4 7 12439.0 933.290 2 0 4 8 5205.25 632.439 2 0 4 9 17019.8 1196.94 2 0 4 10 3853.57 617.333 2 0 4 11-3.05165 228.200 2 0 4 12 7600.13 925.711 2 0 4 -12 6440.12 576.955 1 0 4 13 139.552 205.022 2 0 4 14 2800.00 642.688 2 0 4 15 415.146 369.751 2 0 5 0 58.4814 88.7751 3 0 5 1 2520.56 301.258 3 0 -5 -2 13710.9 721.741 3 0 5 2 12729.2 749.879 2 0 5 3-14.8390 115.119 2 0 -5 -3 20.2314 90.8202 3 0 5 4 1386.30 289.783 2 0 5 5 1645.15 316.942 2 0 5 6 686.491 237.537 2 0 5 7 116.145 155.801 2 0 5 8 2771.11 474.039 2 0 5 9 5778.58 716.377 2 0 5 10 4056.49 655.015 2 0 5 11-468.201 336.337 2 0 5 12 1177.41 408.059 2 0 5 13 881.661 362.502 2 0 5 14 320.311 270.870 2 0 5 15 185.787 260.104 2 0 6 0 1535.31 261.315 3 0 6 1 6497.24 522.673 3 0 -6 -2 24213.8 1066.32 3 0 6 2 22072.3 1098.65 2 0 6 3 3268.73 429.167 2 0 6 4 20923.5 1125.24 2 0 6 5 2055.61 372.074 2 0 6 6 786.613 278.129 2 0 6 7 859.094 311.491 2 0 6 8 18279.2 1247.51 2 0 6 9 666.593 310.884 2 0 6 10 38202.6 2047.48 2 0 6 11 1118.76 410.578 2 0 6 12 1373.78 473.457 2 0 6 13 2189.30 556.985 2 0 6 14 636.031 412.649 2 0 7 0 97.1264 129.074 3 0 7 1 43.9547 107.690 3 0 7 -1-84.8109 130.350 3 0 7 2 390.886 152.868 2 0 7 3 18326.3 1084.21 2 0 7 4 996.060 337.618 2 0 7 5 3142.80 464.633 2 0 7 6 30844.5 1578.27 2 0 7 7-151.117 260.789 2 0 7 8 5154.34 699.709 2 0 7 9 8061.97 891.219 2 0 7 10 22308.3 1549.30 2 0 7 11-42.4351 360.836 2 0 7 12 1396.18 479.142 2 0 7 13 239.250 270.195 2 0 7 14 827.356 393.364 2 0 8 0-5.93884 174.615 3 0 8 1 28365.5 1302.47 3 0 8 -1 26782.6 1291.48 3 0 8 2 1302.98 316.748 2 0 8 3 3911.40 552.640 2 0 8 4 24811.7 1357.32 2 0 8 5 507.189 239.149 2 0 8 6 8058.62 820.532 2 0 8 7-206.880 245.004 2 0 8 8 498.677 277.474 2 0 8 9 690.680 348.856 2 0 8 10 2865.26 599.653 2 0 8 11 670.697 330.258 2 0 8 12-152.384 217.178 2 0 8 13 272.162 212.187 2 0 9 0-154.434 210.510 3 0 9 1 5589.29 592.746 3 0 9 -1 5434.45 622.295 3 0 9 -2 2307.39 432.492 3 0 9 2 2546.80 465.665 2 0 9 3 5005.99 640.395 2 0 9 4 1693.33 373.801 2 0 9 5 6737.65 738.007 2 0 9 6 256.769 237.171 2 0 9 7 877.767 342.241 2 0 9 8 15962.6 1299.78 2 0 9 9-156.735 243.837 2 0 9 10 6304.22 870.502 2 0 9 11-54.9899 242.744 2 0 9 12 66.2946 232.609 2 0 9 13 1206.13 469.825 2 0 10 0 79653.5 2657.24 3 0 10 -1 6947.59 725.744 3 0 10 1 6425.19 649.183 3 0 10 -2 43742.3 1914.54 3 0 10 2 41414.8 1953.56 2 0 10 3 7672.84 832.439 2 0 10 4-178.449 232.756 2 0 10 5-221.831 220.916 2 0 10 6 6989.41 842.353 2 0 10 7-19.1324 216.466 2 0 10 8 2062.92 466.850 2 0 10 9 1919.52 504.523 2 0 10 10 229.838 278.435 2 0 10 11 95.6705 284.404 2 0 10 12-93.5326 283.807 2 0 11 0 19.0917 167.856 3 0 11 1 797.625 319.965 3 0 11 -1 371.481 237.996 3 0 11 2 656.246 364.686 2 0 11 -2 272.615 234.789 3 0 11 -3 2848.66 524.156 3 0 11 3 2314.45 520.680 2 0 11 4 1436.51 417.453 2 0 11 5-130.353 230.150 2 0 11 6-103.303 283.492 2 0 11 7-20.7743 294.252 2 0 11 8 477.313 342.815 2 0 11 9 671.064 381.799 2 0 11 10 1030.59 423.954 2 0 11 11 1046.42 430.709 2 0 12 0 1796.15 423.945 3 0 12 1 933.916 325.202 3 0 12 -1 1486.79 415.086 3 0 12 -2 246.253 256.004 3 0 12 2 619.204 384.870 2 0 12 3 464.749 312.779 2 0 12 -3 1140.67 394.940 3 0 12 -4 236.062 266.465 3 0 12 4-9.97238 244.306 2 0 12 5 2509.14 550.122 2 0 12 6 1702.36 443.726 2 0 12 7 922.209 372.834 2 0 12 8 261.152 293.182 2 0 12 9 2121.17 525.452 2 0 12 10 367.641 247.961 2 0 13 0-136.588 181.763 3 0 13 -1 1992.42 453.387 3 0 13 1 2054.15 484.367 2 0 13 1 1390.64 366.799 3 0 13 2-117.094 206.922 2 0 13 -2 320.033 256.171 3 0 13 3 1188.57 420.329 2 0 13 -3 1363.93 430.220 3 0 13 -4 1069.19 406.033 3 0 13 4 1190.78 393.683 2 0 13 5-190.137 226.629 2 0 13 6 136.242 251.716 2 0 13 7 1697.58 481.225 2 0 13 8 3063.03 656.798 2 0 13 9 40.1648 235.840 2 0 14 0-115.248 289.049 3 0 14 -1 588.750 271.706 3 0 14 1 1318.46 423.468 2 0 14 2 516.916 294.967 2 0 14 -2 299.655 271.870 3 0 14 -3 1054.73 393.579 3 0 14 3 849.464 395.604 2 0 14 4 535.350 345.640 2 0 14 -4 1271.44 399.253 3 0 14 -5 1591.01 440.869 3 0 14 5 1206.37 416.443 2 0 14 6-133.948 234.256 2 0 14 7 379.331 327.597 2 0 14 8 297.774 268.920 2 0 15 0 215.454 284.639 2 0 15 -1 155.988 249.402 3 0 15 1-616.771 337.838 2 0 15 -2 100.049 242.092 3 0 15 2 687.281 381.672 2 0 15 3 53.3284 214.713 2 0 15 -3 740.150 361.019 3 0 15 -4 260.736 267.857 3 0 15 4-13.0014 232.499 2 0 15 -5 367.128 300.750 3 0 15 5-42.0950 226.198 2 0 15 -6 428.856 293.704 3 0 15 6 343.427 291.526 2 0 15 -7 849.307 389.418 3 0 15 7 1455.31 526.559 2 0 16 0 288.645 355.325 2 0 16 1 211.944 289.464 2 0 16 2 287.818 248.364 2 0 16 3 464.515 313.968 2 0 16 4 90.8683 224.964 2 0 16 5-467.518 428.754 2 0 17 1-709.636 378.298 2 0 17 2-230.345 227.598 2 1 0 2 286584. 5022.30 2 -1 0 2 283483. 5082.41 2 1 0 -2 286622. 5070.43 2 -1 0 -2 281060. 5053.18 2 -1 0 -2 282181. 5018.52 1 -1 0 -3 65336.7 1553.53 2 -1 0 -3 62515.6 1479.03 1 1 0 3 64425.7 1542.83 2 1 0 -3 63291.0 1575.75 2 -1 0 3 62403.6 1570.31 2 -1 0 4 32728.9 1138.53 2 1 0 -4 34926.3 1159.65 2 1 0 4 34738.8 1136.83 2 -1 0 -4 32967.3 1008.19 1 1 0 -4 34497.5 771.219 1 -1 0 -4 34634.8 1132.62 2 -1 0 5 38715.6 1365.99 2 -1 0 -5 38825.6 1175.52 1 1 0 -5 39925.7 1373.51 2 1 0 -5 39877.5 938.387 1 1 0 5 39911.6 1349.01 2 -1 0 -5 39235.2 1332.99 2 -1 0 6 89838.7 2467.17 2 1 0 -6 88658.0 1870.91 1 1 0 6 88510.4 2434.48 2 -1 0 -6 90561.5 2175.60 1 -1 0 7 26467.8 1254.76 2 -1 0 -7 25590.3 1012.37 1 1 0 7 26670.9 1234.63 2 -1 0 -8 8163.92 565.927 1 1 0 8 8825.99 742.791 2 -1 0 8 8789.20 753.235 2 -1 0 -9 386.090 167.118 1 1 0 9 417.041 230.352 2 -1 0 9 423.949 191.363 2 -1 0 -10 754.867 232.534 1 1 0 10 155.325 192.796 2 -1 0 10 370.933 189.285 2 -1 0 11-24.9825 196.790 2 1 0 11 46.1388 190.950 2 1 0 12 18216.0 1351.27 2 -1 0 12 18090.8 1354.72 2 -1 0 13 540.339 351.380 2 1 0 13 384.186 260.677 2 1 0 14 1402.75 459.822 2 -1 0 14 1079.99 340.136 2 1 0 15 682.927 354.103 2 -1 0 15 506.847 311.270 2 1 0 16 563.024 312.675 2 -1 1 16 2094.26 612.030 2 1 -1 15 1345.05 482.354 2 -1 1 15 1311.68 432.681 2 1 -1 14 265.308 282.926 2 -1 1 14-127.770 279.933 2 1 -1 13 780.177 342.404 2 -1 1 13 694.349 337.466 2 -1 1 12 5614.61 772.302 2 1 -1 12 4019.28 639.996 2 1 -1 11 19155.1 1295.78 2 -1 1 11 16779.8 1258.70 2 1 -1 10 2633.16 454.554 2 -1 1 10 2768.74 483.727 2 1 1 -10 2782.06 298.589 1 1 1 -9 177.194 93.6447 1 -1 1 9-15.2968 149.684 2 1 -1 9 323.691 197.944 2 -1 1 8 15790.3 1018.09 2 1 1 -8 14828.4 630.253 1 1 -1 8 15627.2 977.740 2 1 -1 7 18858.4 1004.55 2 -1 1 7 18676.2 1043.31 2 1 1 -7 16891.4 640.461 1 1 1 -6 11875.4 476.841 1 -1 1 6 11835.0 760.253 2 -1 1 6 11315.1 470.241 1 -1 -1 -6 11558.9 627.262 1 1 -1 6 12595.5 749.801 2 -1 -1 -5 113801. 2722.12 2 -1 -1 -5 113283. 2497.98 1 -1 1 5 105932. 2159.38 1 1 -1 5 109012. 2609.34 2 -1 1 5 111544. 2711.92 2 1 1 -4 110220. 2561.08 2 -1 -1 -4 112301. 2418.73 1 1 -1 4 112217. 2488.37 2 -1 1 4 108276. 2552.24 2 -1 1 4 109579. 2115.00 1 -1 -1 -4 113171. 2591.71 2 1 -1 3 125921. 2591.61 2 -1 -1 -3 127798. 2714.61 2 -1 1 3 127720. 2684.91 2 -1 -1 -3 129008. 2604.29 1 1 1 -3 126829. 2687.23 2 -1 1 2 81194.7 1742.23 2 1 -1 2 80788.6 1652.89 2 -1 -1 -2 81312.1 1776.36 2 -1 1 -2 82248.9 1659.63 2 1 1 2 82156.2 1741.72 1 1 -1 -2 78312.1 1729.80 2 1 1 2 81337.1 1785.56 2 1 1 3 130317. 2726.64 2 1 1 3 128783. 2603.78 1 -1 1 -3 127595. 2612.35 2 1 -1 -3 125001. 2680.52 2 1 1 4 108239. 2527.07 2 -1 -1 4 109349. 2545.97 2 1 1 4 108750. 2365.47 1 -1 1 -4 110629. 2470.02 2 1 -1 -4 109324. 2537.90 2 1 -1 -5 106678. 2687.89 2 -1 -1 5 112798. 2717.55 2 -1 1 -5 110966. 2644.85 2 1 1 5 107414. 2449.50 1 1 1 5 113931. 2716.21 2 1 1 6 12472.0 786.592 2 -1 1 -6 10523.6 586.039 1 1 1 6 12567.2 634.132 1 -1 -1 6 12397.1 775.947 2 -1 1 -7 17079.8 837.034 1 1 1 7 18066.9 1021.82 2 -1 -1 7 17081.2 984.362 2 -1 -1 8 14211.0 960.663 2 1 1 8 15497.4 1006.91 2 -1 1 -8 14318.4 772.284 1 -1 -1 9-75.1592 136.728 2 -1 1 -9 140.713 124.934 1 1 1 9 81.3670 178.513 2 -1 1 -10 2998.90 388.114 1 -1 -1 10 3247.87 539.608 2 1 1 10 2519.04 466.315 2 -1 -1 11 15804.3 1232.65 2 -1 1 -11 16866.8 956.085 1 1 1 11 18088.1 1298.87 2 -1 -1 12 5013.86 732.039 2 -1 1 -12 4742.76 524.640 1 1 1 12 4351.25 676.514 2 1 1 13 902.597 355.713 2 1 1 14 350.455 289.422 2 1 1 15 1149.93 395.706 2 1 1 16 1868.71 506.381 2 -1 2 15 2866.28 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935.672 2 -1 6 8 8853.14 861.336 2 -1 6 7 4533.32 592.849 2 -1 6 6 5553.78 604.826 2 -1 6 5 6238.65 613.023 2 -1 6 4 29987.9 1347.02 2 -1 6 3 856.500 230.687 2 -1 6 2 8786.95 645.015 2 -1 6 1 367.318 121.012 3 -1 6 0 51897.2 1541.83 3 1 6 0 50389.4 1715.27 3 1 6 1 286.548 159.984 3 1 6 2 8699.21 658.715 3 1 -6 -2 9554.84 596.455 3 1 -6 -3 904.135 201.634 3 1 6 3 725.877 243.006 2 1 6 4 31899.3 1436.41 2 1 6 5 6034.20 623.354 2 1 6 6 5327.51 617.798 2 1 6 7 5133.95 651.770 2 1 6 8 9140.89 913.633 2 1 6 9 9760.18 955.463 2 1 6 10 2890.34 574.964 2 1 6 11 3677.51 645.783 2 1 6 12 625.116 314.185 2 1 6 13 3735.89 723.643 2 1 6 14 675.684 405.335 2 -1 7 14 225.002 259.776 2 -1 7 13 511.510 289.139 2 -1 7 12 1344.23 444.495 2 -1 7 11 2013.02 504.435 2 -1 7 10 3866.38 678.430 2 -1 7 9 10462.0 1001.64 2 -1 7 8 8203.94 844.241 2 -1 7 7 1765.61 409.597 2 -1 7 6 4925.71 600.267 2 -1 7 5 566.922 247.721 2 -1 7 4 2817.09 399.284 2 -1 7 3 17191.8 983.475 2 -1 7 2 24449.4 1183.39 2 1 7 -1 2905.35 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11012.3 797.538 2 2 5 5 24691.1 1280.60 2 2 5 6 2644.89 423.095 2 2 5 7 4628.61 587.934 2 2 5 8 427.808 280.113 2 2 5 9 2809.80 527.881 2 2 5 10 5774.36 777.505 2 2 5 11 3149.49 628.275 2 2 5 12 1984.39 524.617 2 2 5 13-82.1607 308.514 2 -2 5 -13 312.613 191.966 1 2 5 14 1960.13 585.793 2 2 5 15 1098.46 484.530 2 -2 6 14 2403.45 614.248 2 -2 6 13 1549.11 499.238 2 -2 6 12 533.702 286.397 2 -2 6 11 1003.12 345.822 2 -2 6 10 325.532 184.491 2 -2 6 9 12969.0 1064.34 2 -2 6 8 5559.31 650.021 2 -2 6 7 6737.16 692.841 2 -2 6 6 2278.12 392.623 2 -2 6 5 1034.83 266.939 2 -2 6 4 10282.8 736.627 2 -2 6 3 8423.66 621.695 2 -2 6 2 21084.3 955.405 2 -2 6 1 5367.52 449.511 2 2 6 -1 5023.57 551.594 3 -2 6 1 3853.16 332.400 3 2 6 0 42346.6 1605.27 3 -2 6 0 41069.8 1242.13 3 2 6 1 4847.51 504.053 3 2 -6 -2 22022.5 863.436 3 2 6 2 21553.6 1108.41 3 2 6 3 8459.35 754.540 2 2 -6 -3 8056.45 543.382 3 2 6 4 10135.0 820.259 2 2 -6 -4 10597.3 658.238 3 2 6 5 514.317 233.833 2 2 6 6 1727.25 375.620 2 2 6 7 5984.91 705.653 2 2 6 8 4635.79 646.253 2 2 6 9 13248.5 1121.22 2 2 6 10 424.408 231.131 2 2 6 11 452.478 329.430 2 2 6 12 484.809 248.883 2 2 6 13 1866.51 504.291 2 2 6 14 1816.95 526.440 2 -2 7 14 1206.81 493.111 2 -2 7 13 958.861 391.660 2 -2 7 12 2666.96 562.635 2 -2 7 11 113.234 255.963 2 -2 7 10 195.596 237.412 2 -2 7 9 1114.07 345.385 2 -2 7 8 328.060 183.842 2 -2 7 7 782.282 269.633 2 -2 7 6 6719.64 695.346 2 -2 7 5 3702.95 484.528 2 -2 7 4 2150.57 373.917 2 -2 7 3 18124.0 995.796 2 -2 7 2 42991.1 1541.38 2 2 7 -1 16343.1 1040.76 3 -2 7 1 17131.6 785.488 3 -2 7 1 17121.7 902.881 2 2 7 0 5403.20 582.659 3 -2 7 0 5506.98 447.885 3 2 7 1 16046.0 1010.47 3 2 7 2 42964.9 1734.03 3 2 7 3 15639.9 1063.36 2 2 -7 -3 18169.3 876.508 3 2 7 4 1451.78 366.999 2 2 7 5 3144.78 512.566 2 2 7 6 7375.89 783.578 2 2 7 7 688.284 241.142 2 2 7 8 9.09427 240.796 2 2 7 9 565.044 302.691 2 2 7 10 225.279 263.512 2 2 7 11 544.590 281.639 2 2 7 12 2553.30 607.226 2 2 7 13 620.866 343.147 2 2 7 14 685.435 351.049 2 -2 8 13 107.360 266.195 2 -2 8 12 2102.57 533.430 2 -2 8 11 1292.45 407.267 2 -2 8 10 7441.58 911.597 2 -2 8 9 1675.68 436.010 2 -2 8 8 4692.22 662.222 2 -2 8 7 4638.86 626.271 2 -2 8 6 681.593 303.930 2 -2 8 5 4008.89 541.809 2 -2 8 4 7282.97 681.097 2 -2 8 3 5306.84 555.256 2 -2 8 2 15094.2 923.664 2 -2 8 1 4043.34 457.309 2 2 8 -1 4538.42 573.349 3 -2 8 1 4552.92 432.057 3 2 8 0 204.896 225.680 3 -2 8 0 55.6735 113.700 3 -2 8 -1 5157.19 486.925 3 2 8 1 4084.37 540.567 3 2 8 2 14320.2 990.553 3 2 8 3 5213.94 667.105 2 2 8 4 6404.45 734.397 2 2 8 5 3821.52 562.589 2 2 8 6 644.535 285.737 2 2 8 7 5802.57 749.377 2 2 8 8 5668.88 767.392 2 2 8 9 989.348 388.558 2 2 8 10 6184.59 862.780 2 2 8 11 568.305 345.072 2 2 8 12 755.823 322.994 2 2 8 13 42.1446 264.279 2 -2 9 13 258.355 298.854 2 -2 9 12 1311.93 465.771 2 -2 9 11 2224.58 556.413 2 -2 9 10 1989.54 496.117 2 -2 9 9 12125.8 1135.81 2 -2 9 8 6246.99 792.039 2 -2 9 7 835.871 284.912 2 -2 9 6 310.230 293.774 2 -2 9 5 3979.86 561.186 2 -2 9 4 1697.52 323.729 2 -2 9 3 3525.13 492.269 2 2 9 -2 7851.24 801.968 3 -2 9 2 7370.37 688.909 2 -2 9 1 190.891 159.181 2 -2 9 1 288.755 160.508 3 2 9 -1 10.4062 198.335 3 2 9 0 15897.5 1124.29 3 -2 9 0 16540.6 930.403 3 -2 9 -1-11.1068 169.011 3 2 9 1 592.633 251.947 3 2 9 2 7737.07 776.231 3 2 9 3 4317.53 624.665 2 2 9 4 2870.00 546.373 2 2 9 5 3787.33 600.107 2 2 9 6 57.9101 266.370 2 2 9 7 726.251 345.912 2 2 9 8 6880.82 904.637 2 2 9 9 11200.2 1164.43 2 2 9 10 2067.44 568.266 2 2 9 11 1087.72 438.901 2 2 9 12 3897.51 774.246 2 2 9 13 347.534 309.616 2 -2 10 12 532.737 357.858 2 -2 10 11 210.837 419.909 2 -2 10 10 471.431 286.535 2 -2 10 9 445.472 264.102 2 -2 10 8 52.3641 175.705 2 -2 10 7 3550.43 588.051 2 -2 10 6 1966.86 421.808 2 -2 10 5 3224.22 527.920 2 -2 10 4 7483.20 768.668 2 -2 10 3-90.5293 153.932 2 -2 10 2 1625.95 375.160 2 2 10 -2 2210.99 493.768 3 -2 10 1 1650.81 305.153 3 -2 10 1 2034.49 389.521 2 2 10 -1 1967.76 434.599 3 2 10 0 1155.32 329.780 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769.822 2 2 11 6 4279.62 716.629 2 2 11 7 1888.06 502.495 2 2 11 8 2482.71 586.453 2 2 11 9 2648.50 622.818 2 2 11 10 557.915 395.169 2 2 11 11 89.3105 299.788 2 -2 12 11 656.444 397.601 2 -2 12 10 823.506 385.671 2 -2 12 9 1732.27 500.681 2 -2 12 8 2885.70 606.364 2 -2 12 7 1964.61 499.184 2 -2 12 6 1686.64 431.701 2 -2 12 5 930.431 365.158 2 -2 12 4 2798.80 511.914 2 2 12 -4 2200.47 570.523 3 -2 12 3 3405.93 581.706 2 2 12 -3 3599.71 654.880 3 -2 12 2 6368.26 767.741 2 2 12 -2 7423.52 911.004 3 -2 12 1 1687.60 394.369 2 2 12 -1 1840.61 455.132 3 -2 12 0 706.790 262.293 3 2 12 0 555.201 292.332 3 -2 12 0 512.414 264.504 2 -2 12 -1 1242.36 295.809 3 2 12 1 1410.82 380.712 3 -2 12 -2 6636.91 728.847 3 2 12 2 8053.53 954.511 2 -2 12 -3 3630.61 559.195 3 2 12 3 4046.62 709.440 2 2 12 4 2397.12 527.006 2 2 12 5 438.995 272.599 2 2 12 6 1834.89 503.115 2 2 12 7 939.340 360.253 2 2 12 8 2954.93 666.615 2 2 12 9 1870.72 533.283 2 2 12 10 586.253 312.884 2 -2 13 10 306.299 238.863 2 -2 13 9 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34448.2 1374.19 3 3 -4 -2 17457.4 550.887 3 3 -4 -2 17538.7 726.347 2 3 4 2 15922.9 892.934 3 3 -4 -3 39264.5 1269.63 2 3 4 3 40281.4 1535.84 2 -3 4 -3 38518.3 1065.75 2 3 -4 -4 4025.50 394.637 2 3 4 4 3591.74 463.955 2 -3 4 -4 4272.01 339.170 2 -3 4 -5 38319.8 1276.23 2 3 4 5 39476.1 1612.70 2 3 4 6 5966.78 635.111 2 3 4 7 33.1811 156.167 2 3 4 8 14482.2 1071.64 2 3 4 9 543.035 266.944 2 3 4 10 14334.5 1173.45 2 3 4 11 1609.99 449.783 2 -3 4 -11 859.775 279.030 1 -3 4 -12 1021.36 320.927 1 3 4 12 815.714 348.508 2 3 4 13 448.145 309.769 2 -3 4 -13 819.132 319.069 1 3 4 14-187.977 248.159 2 3 4 15 293.970 299.627 2 -3 5 15 328.138 297.494 2 -3 5 14 486.447 291.064 2 -3 5 13 690.925 365.412 2 -3 5 12 397.620 272.468 2 -3 5 11 1970.20 500.061 2 -3 5 10 1471.73 374.735 2 -3 5 9 760.224 289.534 2 -3 5 8 3599.81 522.459 2 -3 5 7 6716.01 673.242 2 -3 5 6 12080.8 856.756 2 -3 5 5 1652.59 296.246 2 -3 5 4 12665.0 754.274 2 -3 5 3 18663.7 866.555 2 -3 5 2 75607.6 1930.63 2 -3 5 1 139956. 2929.92 2 3 5 -1 138839. 3510.27 3 3 5 0 581586. 11110.1 3 -3 5 0 579038. 10152.6 3 3 5 1 134587. 3394.85 3 3 5 2 72666.4 2308.27 3 3 -5 -2 77835.3 1698.36 3 3 -5 -3 18432.2 722.531 3 3 -5 -3 19585.5 902.202 2 3 5 3 20354.0 1098.13 2 3 5 4 12760.7 894.707 2 -3 5 -4 12402.8 626.448 2 3 5 5 1814.41 354.094 2 -3 5 -5 1476.99 234.777 2 3 5 6 11646.7 920.517 2 3 5 7 6081.51 702.915 2 3 5 8 3983.29 592.706 2 3 5 9 580.803 284.887 2 3 5 10 974.202 329.159 2 3 5 11 1661.67 483.453 2 -3 5 -12 407.250 230.361 1 3 5 12 538.636 314.429 2 3 5 13 237.646 246.759 2 -3 5 -13 532.223 287.168 1 3 5 14 460.660 370.943 2 3 5 15 200.366 270.490 2 -3 6 14 824.264 430.071 2 -3 6 13-310.281 326.102 2 -3 6 12 501.017 320.475 2 -3 6 11 1434.57 439.081 2 -3 6 10 2227.65 498.110 2 -3 6 9 713.630 290.075 2 -3 6 8 1642.55 366.067 2 -3 6 7 5669.50 623.779 2 -3 6 6 1089.64 259.145 2 -3 6 5 3619.12 441.116 2 -3 6 4 32485.8 1342.46 2 -3 6 3 8314.23 597.936 2 -3 6 2 34626.2 1227.96 2 -3 6 1 16836.4 764.784 2 3 6 -1 16412.3 1020.22 3 -3 6 0 13265.4 564.145 3 -3 6 0 13716.8 661.343 2 3 6 0 12993.6 898.185 3 3 6 1 16047.2 994.787 3 3 6 2 34973.1 1551.35 3 3 6 3 9272.65 780.881 2 3 -6 -3 8703.75 514.274 3 3 -6 -4 32700.9 1151.09 3 3 6 4 32866.7 1570.23 2 3 6 5 3300.91 502.729 2 3 6 6 1139.12 321.799 2 3 6 7 6047.39 714.296 2 3 6 8 707.538 304.773 2 3 6 9 609.770 278.695 2 3 6 10 1614.59 411.532 2 3 6 11 1351.07 422.704 2 3 6 12 255.952 250.203 2 -3 6 -13-187.104 238.603 1 3 6 13-89.9916 264.227 2 3 6 14 602.183 374.378 2 -3 7 14 2172.24 585.562 2 -3 7 13 273.098 301.203 2 -3 7 12 801.210 307.186 2 -3 7 11 1598.85 450.031 2 -3 7 10 6354.85 829.849 2 -3 7 9 3812.99 601.796 2 -3 7 8 5773.16 696.798 2 -3 7 7 304.508 219.311 2 -3 7 6 3865.37 510.519 2 -3 7 5 5386.59 571.155 2 -3 7 4 7629.87 651.809 2 -3 7 3 252.508 145.305 2 -3 7 2 1540.20 276.658 2 -3 7 1 4636.16 422.418 2 3 7 -1 4791.14 582.209 3 3 7 0-22.1136 199.637 3 -3 7 0-17.1290 85.8036 3 -3 7 0 173.369 110.782 2 3 7 1 4487.36 584.961 3 -3 7 -1 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17477.7 1258.81 2 3 8 6-108.405 244.522 2 3 8 7 579.497 273.782 2 3 8 8 8978.97 988.899 2 3 8 9 4065.24 682.222 2 3 8 10 1752.99 528.909 2 3 8 11 139.146 217.647 2 3 8 12 774.110 352.861 2 3 8 13 824.607 406.411 2 -3 9 13 446.997 315.400 2 -3 9 12 1200.07 420.790 2 -3 9 11 2850.55 630.364 2 -3 9 10 6711.91 882.150 2 -3 9 9 539.107 329.357 2 -3 9 8 6925.12 813.310 2 -3 9 7 312.949 224.492 2 -3 9 6 9060.13 852.043 2 -3 9 5 142.227 175.646 2 -3 9 4 711.836 238.742 2 -3 9 3 14421.1 955.902 2 -3 9 2 2125.84 350.191 2 3 9 -2 2485.11 503.254 3 -3 9 1 3296.95 424.307 2 3 9 -1 3316.01 534.335 3 -3 9 0 6029.39 565.491 2 -3 9 0 5731.32 488.055 3 3 9 0 5159.55 655.210 3 3 9 1 2156.41 444.056 3 -3 9 -1 2853.22 352.430 3 3 9 2 2529.73 460.314 3 3 9 3 14100.8 1133.31 2 3 9 4 441.330 293.436 2 3 9 5 247.156 232.371 2 3 9 6 9179.69 963.816 2 3 9 7-117.909 222.044 2 3 9 8 7012.15 903.916 2 3 9 9 1103.43 466.406 2 3 9 10 5328.70 846.755 2 3 9 11 2030.13 551.304 2 3 9 12 711.859 394.634 2 -3 10 12 235.208 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8 9 1800.07 525.546 2 8 8 10 763.597 393.240 2 8 8 11 967.539 444.783 2 8 9 -5 772.492 374.603 3 8 9 -4-103.639 285.575 3 8 9 -3 506.520 400.109 3 8 9 -2 801.644 361.898 3 8 9 -1 433.262 319.735 3 8 9 0 2096.64 519.887 3 8 9 1 373.501 276.313 3 8 9 2 672.630 314.615 3 8 9 4 379.273 318.727 2 8 9 5 466.698 342.313 2 8 9 6 409.076 315.610 2 8 9 7 402.407 361.975 2 8 9 8 232.218 340.875 2 8 9 9 2102.54 565.315 2 8 9 10 2940.59 751.360 2 8 10 -6 573.939 394.688 3 8 10 -5 1793.45 600.570 3 8 10 -4 508.619 405.243 3 8 10 -3 666.928 359.078 3 8 10 -2 192.460 301.443 3 8 10 -1 362.837 275.300 3 8 10 0-133.616 239.019 3 8 10 1-354.811 356.196 3 8 10 4 218.344 259.494 2 8 10 5 1060.63 444.095 2 8 10 6 1061.60 456.724 2 8 10 7 1499.98 505.627 2 8 10 8 642.621 391.073 2 8 10 9 1027.09 471.660 2 8 11 -7 497.605 424.938 3 8 11 -6 1575.91 572.572 3 8 11 -5 1408.58 548.216 3 8 11 -4 801.047 430.102 3 8 11 -3-51.7681 309.265 3 8 11 -2 127.591 275.951 3 8 11 -1 536.316 368.907 3 8 11 0 555.624 352.127 3 8 11 1 237.289 288.899 3 8 11 3 649.421 344.892 2 8 11 4 808.514 451.013 2 8 11 5 1606.00 584.551 2 8 11 6 1274.70 483.651 2 8 11 7-313.428 303.101 2 8 11 8 2711.29 699.486 2 8 12 -6 235.601 371.791 3 8 12 -5 223.263 414.949 3 8 12 -4 782.178 425.063 3 8 12 -3-62.5206 316.012 3 8 12 -2-0.68891 299.432 3 8 12 -1 121.454 271.196 3 8 12 0-132.752 309.495 3 8 12 1-31.7739 275.679 3 8 12 3 22.2151 230.458 2 8 12 4 623.120 399.353 2 8 12 5-472.303 448.778 2 8 12 6 418.637 358.759 2 8 13 -3 731.510 410.193 3 8 13 -2 286.160 334.645 3 8 13 -1 409.146 410.542 3 8 13 0 484.307 372.178 3 8 13 1-310.476 350.698 3 8 13 3 647.063 458.307 2 -9 0 0-98.4932 169.905 1 9 0 -1 6185.08 582.554 3 -9 0 1 6613.18 636.402 1 -9 0 -1 6672.84 683.652 1 -9 0 -2 152.230 174.588 1 9 0 2 174.843 116.871 2 9 0 -2 88.5176 143.298 3 -9 0 2 474.162 201.419 1 9 0 3 3812.27 405.985 2 -9 0 -3 4030.13 570.177 1 9 0 -3 4769.07 538.766 3 -9 0 3 4793.91 504.091 1 -9 0 -4 925.526 330.424 1 -9 0 4 917.400 222.374 1 9 0 4 537.125 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3829.99 558.459 1 9 1 -2 2451.74 417.456 3 9 1 -1 109.704 175.854 3 -9 -1 -1 283.481 200.214 1 -9 1 1 198.493 134.158 1 -9 1 0 10656.0 821.873 1 9 1 0 9564.43 764.256 3 -9 -1 0 10596.0 830.272 1 -9 -1 1 289.040 182.897 1 9 -1 -1 398.698 156.562 3 -9 1 -1 311.822 217.104 1 9 -1 -2 2757.13 363.708 3 -9 -1 2 3687.77 458.433 1 -9 1 -2 3193.93 477.126 1 -9 1 -3 8363.71 824.698 1 9 1 3 8420.29 676.286 2 9 -1 -3 8783.65 667.995 3 9 1 4 2095.91 347.809 2 -9 1 -4 2288.25 450.663 1 -9 1 -5 991.213 318.850 1 9 1 5 954.915 239.285 2 9 1 6 4769.54 549.458 2 -9 1 -6 5856.82 740.194 1 -9 1 -7 977.606 347.494 1 9 1 7 931.153 309.891 2 -9 1 -8 11668.5 1121.34 1 9 1 8 10055.5 863.846 2 -9 1 -9 1282.07 447.451 1 9 1 9 838.305 280.187 2 9 1 10 732.716 211.664 2 -9 1 -10 784.981 312.377 1 9 1 11-151.352 272.015 2 -9 1 -11 150.591 252.636 1 9 1 12 2698.17 544.497 2 -9 1 -12 3034.93 678.979 1 -9 1 -13 3217.06 750.361 1 -9 -2 -8 3254.97 668.940 1 -9 -2 -7 13421.1 1187.77 1 9 -2 7 12591.9 771.305 2 9 -2 6 2535.62 310.157 2 -9 -2 -6 2168.65 492.118 1 -9 2 6 2788.43 322.625 1 -9 -2 -5 1489.36 455.771 1 -9 2 5 1082.67 224.577 1 9 -2 5 960.313 181.287 2 -9 2 4 17003.0 919.993 1 -9 -2 -4 17301.0 1241.35 1 9 -2 4 15820.3 664.635 2 -9 2 3 12745.7 841.852 1 9 2 -3 13446.8 996.183 3 -9 -2 -3 11898.4 1006.94 1 9 -2 3 11494.1 509.730 2 9 -2 2 4664.45 299.731 2 -9 2 2 5907.44 575.979 1 9 2 -2 5687.52 664.576 3 -9 -2 -2 6539.56 720.977 1 -9 2 1 513.058 196.454 1 9 -2 1 477.845 104.347 2 9 2 -1 693.431 245.620 3 -9 -2 -1 587.891 266.764 1 -9 2 0 4177.05 513.637 1 9 2 0 3927.25 536.980 3 9 -2 0 4061.07 298.319 2 -9 2 -1 737.573 257.331 1 9 -2 -1 558.472 135.250 2 -9 2 -2 5454.06 631.720 1 9 -2 -2 5707.70 465.510 3 9 -2 -2 5246.63 421.551 2 9 2 3 11542.2 866.025 2 -9 2 -3 14580.2 1076.58 1 9 -2 -3 13330.9 748.992 3 9 2 4 15351.4 1012.68 2 -9 2 -4 17561.6 1219.68 1 9 -2 -4 18382.7 952.912 3 9 2 5 929.667 269.340 2 -9 2 -5 1444.93 410.501 1 -9 2 -6 2866.00 563.231 1 9 2 6 2660.01 453.983 2 9 2 7 13047.4 1018.88 2 -9 2 -7 12488.7 1119.31 1 -9 2 -8 3326.19 652.558 1 9 2 8 3248.62 538.344 2 -9 2 -9 90.1854 229.592 1 9 2 9 461.507 267.276 2 -9 2 -10-72.8242 221.788 1 9 2 10 198.547 194.552 2 -9 2 -11 1466.70 496.553 1 9 2 11 947.159 333.807 2 9 2 12 125.693 260.305 2 -9 2 -12 802.577 369.430 1 9 2 13 586.690 281.995 2 -9 2 -13 1769.95 579.905 1 -9 3 6 2702.15 334.679 1 -9 3 5 3011.34 366.375 1 -9 3 4 24277.7 1137.85 1 9 3 -3 1111.16 340.842 3 9 3 -2 6588.27 722.952 3 9 3 -1 2308.61 449.111 3 9 3 0 13588.1 1030.29 3 9 -3 0 10938.7 366.617 2 9 3 1 2043.64 448.369 3 9 -3 -1 2671.08 228.900 2 -9 3 -2 5464.69 452.726 3 9 -3 -2 5436.10 392.471 2 9 -3 -3 657.711 161.922 3 -9 3 -3 408.881 293.048 1 9 3 4 25926.9 1436.83 2 -9 3 -4 28244.4 1574.11 1 9 -3 -4 28862.6 1094.57 3 9 3 5 2559.02 447.718 2 -9 3 -5 4219.43 639.426 1 9 3 6 2651.84 446.785 2 -9 3 -6 3470.05 564.023 1 -9 3 -7 1408.05 457.193 1 9 3 7 1622.50 435.490 2 -9 3 -8 3089.40 624.536 1 9 3 8 2342.94 474.861 2 9 3 9 441.042 262.600 2 -9 3 -9 555.360 248.235 1 9 3 10 149.161 200.901 2 -9 3 -10 213.756 288.405 1 -9 3 -11 433.110 295.738 1 9 3 11 744.982 328.757 2 -9 3 -12 2275.67 587.884 1 9 3 12 1207.73 418.136 2 -9 3 -13 1545.59 518.557 1 9 3 13 1386.89 444.428 2 9 3 14 749.362 399.909 2 9 4 -4 18353.7 1371.35 3 9 4 -3 21751.0 1443.01 3 9 4 -2 31128.3 1695.36 3 9 4 -1 11585.7 995.912 3 9 4 0-814.351 321.111 3 9 4 1 10437.7 941.737 3 9 4 4 17325.6 1217.75 2 9 4 5 12017.2 1013.54 2 9 4 6 3241.58 527.487 2 -9 4 -6 4342.30 683.488 1 -9 4 -7 691.363 319.613 1 9 4 7 1310.91 412.711 2 -9 4 -8 562.416 244.175 1 9 4 8 269.960 224.896 2 -9 4 -9 324.100 247.184 1 9 4 9 95.9529 178.406 2 -9 4 -10 1311.13 458.432 1 9 4 10 1082.46 380.968 2 9 4 11 249.085 280.564 2 -9 4 -11-151.730 305.762 1 -9 4 -12 596.769 348.231 1 9 4 12 872.718 387.401 2 -9 4 -13 987.600 453.677 1 9 4 13 484.729 326.951 2 9 4 14-64.1822 241.828 2 9 5 -4 1586.76 451.882 3 9 5 -3 1068.94 403.192 3 9 5 -2 12321.2 1118.63 3 9 5 -1-912.129 349.973 3 9 5 0 3015.23 537.036 3 9 5 1-215.962 238.888 3 9 5 4 1622.16 427.602 2 9 5 5 3938.77 593.661 2 9 5 6 4842.49 687.783 2 9 5 7 803.351 300.447 2 -9 5 -8 151.823 218.449 1 9 5 8 291.219 219.961 2 9 5 9 469.448 311.584 2 -9 5 -9 913.500 377.690 1 -9 5 -10 56.8712 239.470 1 9 5 10 653.382 360.544 2 -9 5 -11 130.160 237.527 1 9 5 11-140.048 247.938 2 -9 5 -12 459.934 321.281 1 9 5 12 25.7771 271.163 2 9 5 13 1139.77 456.467 2 9 6 -4 15788.9 1327.16 3 9 6 -3 17528.0 1415.87 3 9 6 -2 987.383 390.822 3 9 6 -1 5108.60 732.928 3 9 6 0 52.0386 260.901 3 9 6 1 5684.65 791.341 3 9 6 4 14462.5 1208.49 2 9 6 5 870.811 355.465 2 9 6 6 1236.81 421.261 2 9 6 7 987.036 377.631 2 9 6 8 1789.59 474.270 2 9 6 9 112.914 262.059 2 -9 6 -10 537.114 391.151 1 9 6 10 659.629 396.289 2 -9 6 -11 793.295 432.623 1 9 6 11-7.90273 210.308 2 -9 6 -12-104.721 251.073 1 9 6 12-416.576 325.732 2 9 7 -5 2846.95 658.039 3 9 7 -4 339.497 312.819 3 9 7 -3 377.856 365.016 3 9 7 -2 2795.83 608.582 3 9 7 -1 1777.30 448.646 3 9 7 0 1001.44 398.318 3 9 7 1 1327.38 393.889 3 9 7 4 18.3055 197.102 2 9 7 5 2669.49 586.579 2 9 7 6 256.935 217.819 2 9 7 7 428.897 214.995 2 9 7 8 218.659 198.809 2 9 7 9 1792.83 530.683 2 9 7 10 1349.97 496.790 2 9 7 11 3457.93 726.921 2 -9 7 -11 4800.29 830.755 1 9 7 12 1269.96 445.210 2 9 8 -5 1252.72 495.919 3 9 8 -4 468.890 349.692 3 9 8 -3 2503.45 607.097 3 9 8 -2 1495.62 491.241 3 9 8 -1 662.972 316.439 3 9 8 0 633.680 333.309 3 9 8 1 1159.79 428.559 3 9 8 4 294.533 307.019 2 9 8 5 1511.64 467.152 2 9 8 6 901.290 365.684 2 9 8 7 577.343 283.911 2 9 8 8 1778.86 507.635 2 9 8 9 425.711 437.302 2 9 8 10 176.658 302.856 2 9 8 11 1234.42 415.612 2 9 9 -6 3949.85 823.438 3 9 9 -5 342.070 246.321 3 9 9 -4 663.249 405.358 3 9 9 -3 69.9648 243.697 3 9 9 -2-144.240 320.126 3 9 9 -1 708.762 375.469 3 9 9 0 972.898 372.185 3 9 9 1 851.291 358.244 3 9 9 4 1026.82 405.539 2 9 9 5 486.582 366.213 2 9 9 6 2002.24 577.684 2 9 9 7 848.551 438.629 2 9 9 8 310.323 246.024 2 9 9 9 670.305 358.295 2 9 9 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415.105 2 14 8 4 207.820 413.351 2 14 8 5 1582.07 503.122 2 -15 0 0 112.632 270.686 1 -15 0 -1 450.618 380.594 1 -15 0 -2 1085.26 486.848 1 -15 0 -3 339.769 377.641 1 -15 0 -4 356.387 372.501 1 -15 1 1 338.440 280.555 1 -15 1 0 65.9609 259.441 1 -15 1 -1 172.795 270.602 1 -15 1 -2 583.354 347.447 1 -15 1 -3 167.362 235.768 1 -15 1 -4 1762.75 574.991 1 -15 2 1 431.104 290.822 1 -15 2 0 158.125 283.430 1 -15 2 -1-33.3579 199.866 1 -15 2 -2 1627.02 510.191 1 -15 2 -3 1621.06 530.861 1 -15 2 -4 1860.98 578.625 1 -15 3 1 461.787 282.099 1 -15 3 0-227.087 262.374 1 -15 3 -1-109.934 212.408 1 -15 3 -2 177.524 206.231 1 -15 3 -3 254.731 267.590 1 -15 3 -4 337.109 260.255 1 -15 4 1-413.728 298.651 1 -15 4 0-19.0821 203.757 1 -15 4 -1 408.735 331.950 1 -15 4 -2 538.759 341.494 1 -15 4 -3 1164.69 477.908 1 15 5 -4-674.216 393.579 3 15 5 -3 865.613 357.047 3 15 5 -2-855.874 409.742 3 -15 5 1-135.350 214.357 1 -15 5 0 19.9488 209.802 1 -15 5 -1 106.249 264.674 1 -15 5 -2-448.821 394.315 1 15 6 -4 1045.28 444.540 3 15 6 -3-196.648 282.447 3 15 6 -2 507.843 407.998 3 -15 6 0-297.759 264.150 1 -15 6 -1 641.746 434.330 1 -15 7 0 372.812 322.789 1 -16 0 -2 465.708 291.267 1 -16 1 0 567.912 406.202 1 -16 1 -1 673.337 443.628 1 -16 1 -2 571.742 357.814 1 -16 2 0 236.232 303.800 1 -16 2 -1 99.2221 216.420 1 -16 2 -2 227.281 295.383 1 -16 3 0 564.846 381.250 1 -16 3 -1 867.077 369.803 1 -16 4 0 385.849 317.579 1 -16 4 -1-149.949 247.033 1 ; _shelx_res_checksum 16022 _shelx_res_file ; TITL 130910_s2_lss in P212121 #19 CELL 0.71073 12.237879 12.606908 12.892075 90 90 90 ZERR 4 0.000456 0.000765 0.000822 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 96 120 12 L.S. 10 0 0 511 PLAN 5 SIZE 0.2 0.25 0.3 TEMP 20 REM reset to P212121 #19 BOND $H acta htab fmap 2 SHEL 999 0.8 REM E:/CCD%20data/1309/olex2_130910_s2_lss/130910_s2_lss.hkl WGHT 0.046300 FVAR 6.67153 O1 3 0.796343 0.697844 0.616142 11.00000 0.04406 0.06427 = 0.05567 -0.00891 -0.00912 -0.00485 O2 3 0.046856 0.316073 0.337612 11.00000 0.06454 0.18143 = 0.09255 0.03300 -0.02942 -0.06275 O3 3 0.821808 0.738794 0.782138 11.00000 0.08083 0.09133 = 0.06753 -0.01929 -0.02974 0.00690 C1 1 0.364854 0.400452 0.425159 11.00000 0.03530 0.03339 = 0.03381 0.00190 -0.00148 0.00061 C2 1 0.272002 0.391182 0.505029 11.00000 0.03885 0.04741 = 0.04233 0.00276 -0.00151 -0.00729 AFIX 23 H2A 2 0.302022 0.364390 0.569548 11.00000 -1.20000 H2B 2 0.243023 0.461456 0.518517 11.00000 -1.20000 AFIX 0 C3 1 0.179258 0.319731 0.471688 11.00000 0.04887 0.07365 = 0.05687 0.00980 -0.00378 -0.01910 AFIX 23 H3A 2 0.204126 0.246689 0.473122 11.00000 -1.20000 H3B 2 0.119835 0.326400 0.521051 11.00000 -1.20000 AFIX 0 C4 1 0.137521 0.344518 0.366128 11.00000 0.04713 0.07255 = 0.06452 0.00195 -0.00895 -0.01487 C5 1 0.210237 0.403044 0.298189 11.00000 0.04446 0.05067 = 0.04772 0.00326 -0.01331 -0.00388 AFIX 43 H5 2 0.182585 0.424921 0.234494 11.00000 -1.20000 AFIX 0 C6 1 0.314352 0.428115 0.320051 11.00000 0.04168 0.03189 = 0.03889 -0.00172 -0.00284 0.00346 C7 1 0.378181 0.487973 0.243314 11.00000 0.04365 0.05679 = 0.03689 0.00601 -0.00467 0.00068 AFIX 13 H7 2 0.334141 0.532669 0.197267 11.00000 -1.20000 AFIX 0 C8 1 0.483234 0.445867 0.194116 11.00000 0.05322 0.09438 = 0.03349 -0.00860 0.00363 -0.00190 AFIX 23 H8A 2 0.509014 0.376631 0.215986 11.00000 -1.20000 H8B 2 0.496638 0.462626 0.121793 11.00000 -1.20000 AFIX 0 C9 1 0.488965 0.534213 0.270566 11.00000 0.04817 0.06146 = 0.03289 0.00940 -0.00177 -0.01337 AFIX 13 H9 2 0.504254 0.604339 0.241150 11.00000 -1.20000 AFIX 0 C10 1 0.534023 0.515306 0.379016 11.00000 0.03528 0.04235 = 0.03489 0.00269 -0.00006 -0.00305 AFIX 13 H10 2 0.583908 0.454523 0.377258 11.00000 -1.20000 AFIX 0 C11 1 0.441634 0.492707 0.457586 11.00000 0.03603 0.03348 = 0.03642 -0.00091 0.00145 -0.00016 AFIX 13 H11 2 0.395922 0.556530 0.458203 11.00000 -1.20000 AFIX 0 C12 1 0.486162 0.481421 0.568088 11.00000 0.04822 0.04748 = 0.03384 0.00000 -0.00056 -0.01064 AFIX 23 H12A 2 0.532133 0.418849 0.571670 11.00000 -1.20000 H12B 2 0.425519 0.471206 0.615495 11.00000 -1.20000 AFIX 0 C13 1 0.552613 0.578358 0.603014 11.00000 0.04955 0.04510 = 0.03687 -0.00175 -0.00439 -0.01091 AFIX 23 H13A 2 0.505651 0.640292 0.605413 11.00000 -1.20000 H13B 2 0.581311 0.566275 0.672146 11.00000 -1.20000 AFIX 0 C14 1 0.646645 0.598072 0.527856 11.00000 0.04053 0.03982 = 0.03830 0.00187 -0.00334 -0.00682 C15 1 0.595812 0.612652 0.418963 11.00000 0.04063 0.04419 = 0.03816 0.00331 0.00137 -0.00749 AFIX 13 H15 2 0.538541 0.665896 0.429547 11.00000 -1.20000 AFIX 0 C16 1 0.681564 0.670177 0.354659 11.00000 0.06681 0.07604 = 0.04191 0.01096 -0.00009 -0.03150 AFIX 13 H16 2 0.656980 0.709849 0.293595 11.00000 -1.20000 AFIX 0 C17 1 0.799689 0.642666 0.362220 11.00000 0.05985 0.11680 = 0.06135 0.00554 0.01405 -0.02918 AFIX 23 H17A 2 0.847154 0.665128 0.306108 11.00000 -1.20000 H17B 2 0.818690 0.574954 0.393064 11.00000 -1.20000 AFIX 0 C18 1 0.754249 0.726954 0.432401 11.00000 0.06643 0.07325 = 0.05830 0.00353 0.00039 -0.03030 AFIX 13 H18 2 0.773981 0.800606 0.416897 11.00000 -1.20000 AFIX 0 C19 1 0.709408 0.704437 0.537982 11.00000 0.04356 0.05194 = 0.04977 0.00119 -0.00627 -0.01175 C20 1 0.640732 0.798131 0.577317 11.00000 0.06145 0.03852 = 0.07414 0.00435 -0.01398 -0.00948 AFIX 23 H20A 2 0.665720 0.864326 0.547179 11.00000 -1.20000 H20B 2 0.564144 0.788331 0.560472 11.00000 -1.20000 AFIX 0 C21 1 0.658124 0.797479 0.693512 11.00000 0.05847 0.05003 = 0.07264 -0.01320 -0.00578 -0.00311 AFIX 23 H21A 2 0.660750 0.869124 0.720834 11.00000 -1.20000 H21B 2 0.600404 0.758631 0.728381 11.00000 -1.20000 AFIX 0 C22 1 0.766494 0.742618 0.706263 11.00000 0.05653 0.05039 = 0.06212 -0.00780 -0.00948 -0.01193 C23 1 0.425261 0.292982 0.419269 11.00000 0.05029 0.03960 = 0.05322 -0.00262 -0.00968 0.00791 AFIX 137 H23A 2 0.377069 0.240105 0.391367 11.00000 -1.50000 H23B 2 0.448120 0.272226 0.487549 11.00000 -1.50000 H23C 2 0.488122 0.299850 0.375233 11.00000 -1.50000 AFIX 0 C24 1 0.726746 0.503055 0.540339 11.00000 0.05484 0.05095 = 0.05506 -0.00202 -0.01264 0.00299 AFIX 137 H24A 2 0.716204 0.454001 0.484269 11.00000 -1.50000 H24B 2 0.712822 0.467911 0.605063 11.00000 -1.50000 H24C 2 0.800625 0.528636 0.539386 11.00000 -1.50000 AFIX 0 HKLF 4 REM 130910_s2_lss in P212121 #19 REM R1 = 0.0522 for 2673 Fo > 4sig(Fo) and 0.0804 for all 3794 data REM 246 parameters refined using 0 restraints END WGHT 0.0463 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, -y+1, z+1/2 HTAB C21 O2_$1 REM Highest difference peak 0.167, deepest hole -0.160, 1-sigma level 0.036 Q1 1 0.1839 0.3858 0.2189 11.00000 0.05 0.17 Q2 1 0.4955 0.4971 0.4236 11.00000 0.05 0.14 Q3 1 0.5093 0.5184 0.3231 11.00000 0.05 0.14 Q4 1 0.4533 0.4959 0.5211 11.00000 0.05 0.13 Q5 1 0.8475 0.7845 0.8450 11.00000 0.05 0.12 ; _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. ; _shelxl_version_number 2013-2