# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_DK_JS_III_132 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H16 O2' _chemical_formula_sum 'C16 H16 O2' _chemical_formula_weight 240.29 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 monoclinic _space_group_IT_number 7 _space_group_name_H-M_alt 'P c' _space_group_name_Hall 'P -2yc' _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, -y, z+1/2' _cell_length_a 6.4499(11) _cell_length_b 13.834(2) _cell_length_c 7.0464(12) _cell_angle_alpha 90 _cell_angle_beta 90.240(3) _cell_angle_gamma 90 _cell_volume 628.74(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7645 _cell_measurement_theta_min 5.890 _cell_measurement_theta_max 53.552 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.269 _exptl_crystal_F_000 256 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.556 _exptl_crystal_size_mid 0.328 _exptl_crystal_size_min 0.173 _exptl_absorpt_coefficient_mu 0.082 _shelx_estimated_absorpt_T_min 0.956 _shelx_estimated_absorpt_T_max 0.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6820 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details ; SADABS-2012/1, G. Sheldrick, Goettingen ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'INCOATEC Mo Microsource' _diffrn_measurement_device_type 'Bruker SMart APEXII' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19964 _diffrn_reflns_av_unetI/netI 0.0203 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.945 _diffrn_reflns_theta_max 27.150 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 2806 _reflns_number_gt 2724 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.987 _reflns_Friedel_fraction_max 0.999 _reflns_Friedel_fraction_full 0.998 _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 'APEX 2013.4-1' _computing_cell_refinement 'APEX 2013.4-1' _computing_data_reduction 'SAINT V8.30C' _computing_structure_solution 'SHELXT-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'XP (Sheldrick)' _computing_publication_material 'XP (Sheldrick)' _refine_special_details ; The hydrogen atom H1 at O2 was found via difference fourier analysis and was refined with a distance restraint set to 0.84 A. The isotropic vibrational parameter of H1 was constrained to 150% of its adjacent carbon atom. ; _iucr_refine_instructions_details ; see below ; _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^)+(0.0431P)^2^+0.1389P] 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_abs_structure_details ; Flack x determined using 1314 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.1(3) _chemical_absolute_configuration ? _refine_ls_number_reflns 2806 _refine_ls_number_parameters 167 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 O1 O 0.7913(2) 0.56932(11) 0.9656(2) 0.0223(3) Uani 1 1 d . . . . . O2 O 0.5416(2) 0.59901(10) 0.6800(2) 0.0185(3) Uani 1 1 d D . . . . H1 H 0.657(4) 0.5761(19) 0.696(4) 0.028 Uiso 1 1 d D U . . . C1 C 0.7888(3) 0.71050(14) 1.2806(3) 0.0155(4) Uani 1 1 d . . . . . C2 C 0.7935(3) 0.81015(15) 1.2601(3) 0.0190(4) Uani 1 1 d . . . . . H2 H 0.6832 0.8423 1.1965 0.023 Uiso 1 1 calc R U . . . C3 C 0.9598(4) 0.86328(15) 1.3325(3) 0.0232(4) Uani 1 1 d . . . . . H3 H 0.9618 0.9316 1.3190 0.028 Uiso 1 1 calc R U . . . C4 C 1.1220(3) 0.81669(17) 1.4241(3) 0.0231(4) Uani 1 1 d . . . . . H4 H 1.2341 0.8530 1.4753 0.028 Uiso 1 1 calc R U . . . C5 C 1.1198(3) 0.71673(16) 1.4408(3) 0.0210(4) Uani 1 1 d . . . . . H5 H 1.2323 0.6845 1.5008 0.025 Uiso 1 1 calc R U . . . C6 C 0.9541(3) 0.66372(14) 1.3702(3) 0.0178(4) Uani 1 1 d . . . . . H6 H 0.9530 0.5954 1.3829 0.021 Uiso 1 1 calc R U . . . C7 C 0.6049(3) 0.65320(14) 1.2080(3) 0.0167(4) Uani 1 1 d . . . . . H7A H 0.4800 0.6948 1.2094 0.020 Uiso 1 1 calc R U . . . H7B H 0.5797 0.5979 1.2940 0.020 Uiso 1 1 calc R U . . . C8 C 0.6388(3) 0.61579(13) 1.0085(3) 0.0156(4) Uani 1 1 d . . . . . C9 C 0.4731(3) 0.63770(13) 0.8565(3) 0.0155(4) Uani 1 1 d . . . . . C10 C 0.2720(3) 0.58650(14) 0.9115(3) 0.0187(4) Uani 1 1 d . . . . . H10A H 0.1648 0.6002 0.8162 0.028 Uiso 1 1 calc R U . . . H10B H 0.2261 0.6098 1.0357 0.028 Uiso 1 1 calc R U . . . H10C H 0.2961 0.5166 0.9176 0.028 Uiso 1 1 calc R U . . . C11 C 0.4563(3) 0.74759(12) 0.8419(3) 0.0162(4) Uani 1 1 d . . . . . C12 C 0.2944(3) 0.79927(15) 0.9238(3) 0.0197(4) Uani 1 1 d . . . . . H12 H 0.1855 0.7658 0.9859 0.024 Uiso 1 1 calc R U . . . C13 C 0.2914(4) 0.89975(16) 0.9152(3) 0.0257(5) Uani 1 1 d . . . . . H13 H 0.1810 0.9345 0.9724 0.031 Uiso 1 1 calc R U . . . C14 C 0.4478(4) 0.94916(15) 0.8240(3) 0.0281(5) Uani 1 1 d . . . . . H14 H 0.4452 1.0178 0.8181 0.034 Uiso 1 1 calc R U . . . C15 C 0.6089(4) 0.89818(16) 0.7411(3) 0.0261(5) Uani 1 1 d . . . . . H15 H 0.7166 0.9320 0.6778 0.031 Uiso 1 1 calc R U . . . C16 C 0.6133(3) 0.79826(15) 0.7503(3) 0.0201(4) Uani 1 1 d . . . . . H16 H 0.7245 0.7639 0.6935 0.024 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 0.0159(6) 0.0268(8) 0.0243(7) -0.0058(6) -0.0024(5) 0.0033(6) O2 0.0190(7) 0.0205(7) 0.0161(7) -0.0040(5) -0.0012(5) 0.0009(5) C1 0.0155(8) 0.0201(9) 0.0109(8) -0.0014(7) 0.0001(7) 0.0000(8) C2 0.0199(9) 0.0217(10) 0.0154(10) -0.0007(7) -0.0011(7) 0.0015(8) C3 0.0296(10) 0.0196(9) 0.0204(10) -0.0017(8) 0.0022(8) -0.0049(9) C4 0.0212(10) 0.0318(12) 0.0163(10) -0.0035(8) -0.0007(8) -0.0090(9) C5 0.0182(9) 0.0307(11) 0.0143(9) -0.0002(8) -0.0017(7) 0.0010(8) C6 0.0194(9) 0.0201(9) 0.0140(9) 0.0006(8) 0.0011(7) 0.0006(8) C7 0.0154(9) 0.0194(9) 0.0153(10) 0.0007(7) -0.0017(7) 0.0001(7) C8 0.0141(8) 0.0136(8) 0.0190(9) 0.0005(7) -0.0003(7) -0.0028(7) C9 0.0150(8) 0.0171(8) 0.0144(9) -0.0012(7) 0.0004(7) -0.0004(7) C10 0.0147(9) 0.0203(9) 0.0212(10) -0.0009(8) -0.0024(7) -0.0036(7) C11 0.0189(8) 0.0172(9) 0.0123(8) -0.0004(8) -0.0045(6) 0.0000(8) C12 0.0225(9) 0.0209(10) 0.0156(9) 0.0017(8) -0.0004(8) 0.0026(8) C13 0.0357(11) 0.0230(11) 0.0183(10) -0.0009(8) 0.0003(9) 0.0098(9) C14 0.0479(14) 0.0164(9) 0.0198(11) 0.0000(8) -0.0009(9) 0.0019(10) C15 0.0370(13) 0.0225(11) 0.0190(10) -0.0005(8) 0.0031(9) -0.0081(9) C16 0.0225(10) 0.0217(10) 0.0160(9) -0.0027(8) -0.0004(8) -0.0005(8) _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 C8 1.215(2) . ? O2 C9 1.426(2) . ? O2 H1 0.81(2) . ? C1 C2 1.387(3) . ? C1 C6 1.396(3) . ? C1 C7 1.514(3) . ? C2 C3 1.395(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C5 1.388(3) . ? C4 H4 0.9500 . ? C5 C6 1.386(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.515(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.540(3) . ? C9 C11 1.527(2) . ? C9 C10 1.529(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.392(3) . ? C11 C12 1.393(3) . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 C14 1.380(3) . ? C13 H13 0.9500 . ? C14 C15 1.387(3) . ? C14 H14 0.9500 . ? C15 C16 1.384(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 O2 H1 108(2) . . ? C2 C1 C6 119.41(18) . . ? C2 C1 C7 120.19(17) . . ? C6 C1 C7 120.39(17) . . ? C1 C2 C3 120.19(19) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 120.20(18) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 119.65(19) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.32(19) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 120.20(17) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C1 C7 C8 112.11(15) . . ? C1 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? C1 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? O1 C8 C7 122.17(17) . . ? O1 C8 C9 119.41(18) . . ? C7 C8 C9 118.42(15) . . ? O2 C9 C11 109.70(15) . . ? O2 C9 C10 108.27(15) . . ? C11 C9 C10 114.72(16) . . ? O2 C9 C8 108.41(15) . . ? C11 C9 C8 106.94(15) . . ? C10 C9 C8 108.63(16) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 118.79(16) . . ? C16 C11 C9 118.74(18) . . ? C12 C11 C9 122.41(18) . . ? C13 C12 C11 120.3(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 120.3(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 119.65(19) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 120.2(2) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C11 120.63(19) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.5(3) . . . . ? C7 C1 C2 C3 177.86(19) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? C2 C3 C4 C5 1.0(3) . . . . ? C3 C4 C5 C6 -1.5(3) . . . . ? C4 C5 C6 C1 0.5(3) . . . . ? C2 C1 C6 C5 1.0(3) . . . . ? C7 C1 C6 C5 -178.34(17) . . . . ? C2 C1 C7 C8 93.6(2) . . . . ? C6 C1 C7 C8 -87.0(2) . . . . ? C1 C7 C8 O1 52.9(2) . . . . ? C1 C7 C8 C9 -127.25(18) . . . . ? O1 C8 C9 O2 -2.4(2) . . . . ? C7 C8 C9 O2 177.74(15) . . . . ? O1 C8 C9 C11 -120.58(19) . . . . ? C7 C8 C9 C11 59.5(2) . . . . ? O1 C8 C9 C10 115.08(19) . . . . ? C7 C8 C9 C10 -64.8(2) . . . . ? O2 C9 C11 C16 -42.8(2) . . . . ? C10 C9 C11 C16 -164.86(18) . . . . ? C8 C9 C11 C16 74.6(2) . . . . ? O2 C9 C11 C12 140.05(19) . . . . ? C10 C9 C11 C12 17.9(3) . . . . ? C8 C9 C11 C12 -102.6(2) . . . . ? C16 C11 C12 C13 -0.5(3) . . . . ? C9 C11 C12 C13 176.66(18) . . . . ? C11 C12 C13 C14 0.6(3) . . . . ? C12 C13 C14 C15 -0.2(3) . . . . ? C13 C14 C15 C16 -0.2(3) . . . . ? C14 C15 C16 C11 0.2(3) . . . . ? C12 C11 C16 C15 0.1(3) . . . . ? C9 C11 C16 C15 -177.16(19) . . . . ? _refine_diff_density_max 0.254 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.036 _shelxl_version_number 2013-4 _shelx_res_file ; REM Solution 1 R1 0.082 Rweak 0.018, Alpha = 0.0084 in Pc TITL pc in Pc CELL 0.71073 6.4499 13.8343 7.0464 90.000 90.240 90.000 ZERR 2.00 0.0011 0.0022 0.0012 0.000 0.003 0.000 LATT -1 SYMM X, -Y, 1/2+Z SFAC C H O UNIT 32 32 4 TEMP -173.150 SIZE 0.173 0.328 0.556 L.S. 10 BOND $H ACTA CONF LIST 4 FMAP 2 DFIX 0.84 O2 H1 PLAN 20 WGHT 0.043100 0.138900 FVAR 1.31632 O1 3 0.791333 0.569320 0.965554 11.00000 0.01592 0.02681 = 0.02426 -0.00576 -0.00235 0.00330 O2 3 0.541617 0.599007 0.680022 11.00000 0.01903 0.02047 = 0.01614 -0.00397 -0.00125 0.00091 H1 2 0.656724 0.576119 0.695815 11.00000 -1.50000 C1 1 0.788836 0.710496 1.280552 11.00000 0.01555 0.02009 = 0.01086 -0.00141 0.00013 -0.00004 C2 1 0.793541 0.810149 1.260061 11.00000 0.01986 0.02166 = 0.01539 -0.00070 -0.00108 0.00152 AFIX 43 H2 2 0.683231 0.842341 1.196497 11.00000 -1.20000 AFIX 0 C3 1 0.959797 0.863279 1.332517 11.00000 0.02965 0.01959 = 0.02039 -0.00167 0.00218 -0.00489 AFIX 43 H3 2 0.961840 0.931597 1.319025 11.00000 -1.20000 AFIX 0 C4 1 1.121992 0.816692 1.424123 11.00000 0.02120 0.03184 = 0.01633 -0.00353 -0.00070 -0.00896 AFIX 43 H4 2 1.234091 0.852985 1.475257 11.00000 -1.20000 AFIX 0 C5 1 1.119773 0.716726 1.440758 11.00000 0.01818 0.03065 = 0.01427 -0.00020 -0.00168 0.00098 AFIX 43 H5 2 1.232329 0.684465 1.500774 11.00000 -1.20000 AFIX 0 C6 1 0.954089 0.663723 1.370213 11.00000 0.01938 0.02013 = 0.01396 0.00063 0.00106 0.00062 AFIX 43 H6 2 0.953034 0.595362 1.382939 11.00000 -1.20000 AFIX 0 C7 1 0.604903 0.653203 1.208015 11.00000 0.01544 0.01936 = 0.01528 0.00065 -0.00169 0.00007 AFIX 23 H7A 2 0.480026 0.694802 1.209445 11.00000 -1.20000 H7B 2 0.579664 0.597890 1.294015 11.00000 -1.20000 AFIX 0 C8 1 0.638783 0.615790 1.008539 11.00000 0.01408 0.01361 = 0.01903 0.00053 -0.00029 -0.00277 C9 1 0.473054 0.637704 0.856475 11.00000 0.01495 0.01712 = 0.01442 -0.00115 0.00041 -0.00044 C10 1 0.271962 0.586499 0.911463 11.00000 0.01467 0.02026 = 0.02122 -0.00086 -0.00239 -0.00358 AFIX 137 H10A 2 0.164771 0.600245 0.816249 11.00000 -1.50000 H10B 2 0.226131 0.609807 1.035741 11.00000 -1.50000 H10C 2 0.296112 0.516630 0.917639 11.00000 -1.50000 AFIX 0 C11 1 0.456298 0.747591 0.841886 11.00000 0.01892 0.01724 = 0.01227 -0.00043 -0.00454 -0.00004 C12 1 0.294400 0.799274 0.923795 11.00000 0.02250 0.02087 = 0.01560 0.00174 -0.00043 0.00257 AFIX 43 H12 2 0.185471 0.765756 0.985865 11.00000 -1.20000 AFIX 0 C13 1 0.291378 0.899746 0.915185 11.00000 0.03566 0.02299 = 0.01835 -0.00092 0.00028 0.00983 AFIX 43 H13 2 0.181027 0.934496 0.972373 11.00000 -1.20000 AFIX 0 C14 1 0.447816 0.949164 0.824021 11.00000 0.04793 0.01640 = 0.01984 0.00000 -0.00093 0.00187 AFIX 43 H14 2 0.445211 1.017756 0.818069 11.00000 -1.20000 AFIX 0 C15 1 0.608861 0.898176 0.741133 11.00000 0.03699 0.02250 = 0.01896 -0.00051 0.00312 -0.00812 AFIX 43 H15 2 0.716561 0.931950 0.677819 11.00000 -1.20000 AFIX 0 C16 1 0.613284 0.798261 0.750296 11.00000 0.02252 0.02169 = 0.01605 -0.00274 -0.00044 -0.00055 AFIX 43 H16 2 0.724499 0.763923 0.693550 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 REM pc in Pc REM R1 = 0.0308 for 2724 Fo > 4sig(Fo) and 0.0318 for all 2806 data REM 167 parameters refined using 3 restraints END WGHT 0.0431 0.1389 REM Highest difference peak 0.254, deepest hole -0.173, 1-sigma level 0.036 Q1 1 0.4581 0.6948 0.8415 11.00000 0.05 0.25 Q2 1 0.3845 0.7665 0.9002 11.00000 0.05 0.21 Q3 1 0.3784 0.6128 0.8874 11.00000 0.05 0.20 Q4 1 0.5527 0.7701 0.8343 11.00000 0.05 0.20 Q5 1 0.8273 0.7563 1.2364 11.00000 0.05 0.18 Q6 1 0.2987 0.8475 0.8977 11.00000 0.05 0.18 Q7 1 0.7644 0.7603 1.3130 11.00000 0.05 0.18 Q8 1 0.8603 0.6876 1.3454 11.00000 0.05 0.16 Q9 1 0.3518 0.9146 0.8348 11.00000 0.05 0.16 Q10 1 0.5983 0.8464 0.7257 11.00000 0.05 0.16 Q11 1 0.5444 0.9207 0.8178 11.00000 0.05 0.14 Q12 1 0.9382 0.5431 1.3745 11.00000 0.05 0.13 Q13 1 0.9028 0.8367 1.2481 11.00000 0.05 0.13 Q14 1 1.1394 0.7626 1.3852 11.00000 0.05 0.12 Q15 1 1.0927 0.7660 1.4644 11.00000 0.05 0.12 Q16 1 0.4897 0.6205 0.7739 11.00000 0.05 0.12 Q17 1 0.5979 0.5936 1.2480 11.00000 0.05 0.12 Q18 1 0.2782 0.4609 0.8058 11.00000 0.05 0.12 Q19 1 1.0528 0.6922 1.3576 11.00000 0.05 0.12 Q20 1 0.6013 0.7238 0.7568 11.00000 0.05 0.11 ; _shelx_res_checksum 6533 _shelx_hkl_file ; 1 0 0 3029.60 85.69 1 0 0 3190.18 82.89 1 0 0 3113.19 83.49 1 0 0 3115.49 85.29 1 0 0 3204.68 84.69 1 0 0 3044.00 77.39 1 0 0 3048.79 85.59 1 0 0 3147.69 79.89 1 0 0 3210.98 82.69 2 0 0 347.87 11.40 2 0 0 349.07 10.80 2 0 0 336.87 11.20 2 0 0 329.27 10.80 2 0 0 348.47 11.20 2 0 0 352.36 11.00 2 0 0 340.67 11.50 2 0 0 355.06 11.20 2 0 0 335.57 10.60 -3 0 0 531.15 16.90 -3 0 0 527.65 16.90 -3 0 0 519.25 16.50 3 0 0 515.65 17.50 3 0 0 522.55 17.50 3 0 0 525.95 16.80 3 0 0 535.55 17.50 3 0 0 519.05 16.20 3 0 0 516.15 16.50 3 0 0 548.15 17.30 3 0 0 523.05 17.00 3 0 0 542.85 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14.60 3.80 -7 -3 0 21.40 5.00 -7 -3 0 16.20 3.90 7 -3 0 26.00 5.20 7 -3 0 13.40 4.70 -7 -3 0 24.80 4.90 7 -3 0 26.70 5.80 -7 -3 0 20.80 4.80 -7 -3 0 20.40 4.70 7 -3 0 15.90 4.30 -7 -3 0 25.20 4.50 -7 3 0 15.50 4.50 7 3 0 15.70 4.10 7 3 0 18.30 4.60 -7 3 0 23.40 4.60 7 3 0 20.30 4.20 -7 3 0 17.40 4.10 7 3 0 25.60 4.50 -7 3 0 16.30 3.90 -8 -3 0 18.90 4.30 8 -3 0 24.00 5.90 -8 -3 0 22.00 5.50 -8 -3 0 32.00 5.70 8 -3 0 19.10 5.80 8 -3 0 36.30 7.80 -8 3 0 25.30 6.00 -8 3 0 31.50 5.80 8 3 0 23.40 5.10 -8 3 0 29.10 5.40 -8 3 0 29.20 6.50 8 3 0 20.70 5.00 0 -4 0 2829.22 82.09 0 -4 0 3112.99 79.59 0 -4 0 2996.90 76.69 0 -4 0 3121.39 79.59 0 4 0 2910.01 82.09 0 4 0 3033.10 82.59 0 4 0 3004.10 81.59 0 4 0 3094.89 80.59 0 4 0 2918.31 82.49 0 4 0 2940.21 74.89 1 -4 0 444.16 13.70 1 -4 0 460.45 12.70 1 -4 0 459.65 13.40 1 -4 0 424.56 14.10 -1 -4 0 467.45 13.00 -1 -4 0 438.66 12.70 1 -4 0 468.95 13.70 1 -4 0 423.06 14.00 -1 -4 0 464.25 13.60 -1 -4 0 462.45 12.70 1 -4 0 435.16 12.70 1 4 0 459.15 13.50 1 4 0 438.86 14.00 1 4 0 460.55 12.80 1 4 0 469.95 13.90 -1 4 0 434.06 13.10 -1 4 0 448.06 14.20 -1 4 0 423.66 13.80 1 4 0 453.55 13.20 -1 4 0 448.66 12.80 -2 -4 0 460.05 14.30 -2 -4 0 458.05 13.50 2 -4 0 461.45 15.40 -2 -4 0 473.55 14.80 2 -4 0 477.05 15.30 2 -4 0 452.05 15.20 2 -4 0 472.05 15.70 -2 -4 0 473.65 14.20 -2 4 0 461.85 15.40 2 4 0 464.55 14.30 -2 4 0 465.95 13.90 2 4 0 471.25 13.50 -2 4 0 486.75 13.80 2 4 0 475.95 15.20 2 4 0 460.85 14.60 -2 4 0 490.35 15.30 2 4 0 459.35 13.60 3 -4 0 1867.51 52.29 3 -4 0 1868.81 52.59 3 -4 0 1806.12 54.89 -3 -4 0 1914.51 53.09 3 -4 0 1954.00 54.19 3 -4 0 1946.31 54.19 3 -4 0 1934.01 55.49 -3 -4 0 1946.81 52.79 -3 -4 0 1898.01 51.59 -3 -4 0 1913.01 52.99 3 -4 0 1897.81 54.79 3 4 0 1906.41 53.19 3 4 0 1893.71 54.89 -3 4 0 1883.01 54.99 -3 4 0 1881.81 49.50 -3 4 0 1903.21 52.19 3 4 0 1766.02 52.49 -3 4 0 1878.21 54.79 -3 4 0 1907.31 52.19 3 4 0 1873.11 50.89 3 4 0 1851.41 53.99 -3 4 0 1903.71 54.39 3 4 0 1913.51 53.49 4 -4 0 23.60 3.40 -4 -4 0 27.90 3.90 -4 -4 0 21.80 2.30 -4 -4 0 21.20 3.20 4 -4 0 18.40 3.40 -4 -4 0 29.90 2.50 4 -4 0 20.90 3.50 -4 -4 0 22.20 3.20 4 -4 0 21.10 3.50 4 -4 0 15.70 2.70 4 -4 0 18.50 3.60 4 -4 0 20.00 1.70 -4 4 0 17.90 2.90 -4 4 0 30.60 3.90 4 4 0 22.40 2.40 4 4 0 25.70 3.70 4 4 0 22.00 2.70 -4 4 0 25.50 2.90 -4 4 0 29.80 3.30 -4 4 0 23.90 1.70 4 4 0 24.20 2.70 4 4 0 29.60 3.80 4 4 0 25.00 3.50 4 4 0 28.80 4.00 -4 4 0 18.50 2.80 -5 -4 0 13.90 2.40 -5 -4 0 17.50 2.40 5 -4 0 9.30 2.80 -5 -4 0 18.20 2.80 -5 -4 0 21.10 3.90 -5 -4 0 15.80 3.20 5 -4 0 10.10 3.20 5 -4 0 10.30 2.80 5 -4 0 9.10 2.90 5 -4 0 14.20 3.20 -5 -4 0 14.80 2.90 5 4 0 15.00 3.40 5 4 0 14.70 3.30 -5 4 0 8.70 2.30 5 4 0 9.90 2.30 5 4 0 11.30 2.60 -5 4 0 15.10 3.00 -5 4 0 11.20 2.50 -5 4 0 12.40 2.90 5 4 0 12.20 2.30 -5 4 0 8.40 2.00 5 4 0 14.50 3.10 5 4 0 14.10 2.30 6 -4 0 14.40 3.70 -6 -4 0 20.80 3.10 6 -4 0 11.30 3.30 -6 -4 0 19.40 3.30 6 -4 0 18.90 4.60 -6 -4 0 14.10 3.50 -6 -4 0 15.20 3.30 -6 -4 0 18.50 4.20 -6 -4 0 17.10 2.80 6 -4 0 15.40 3.40 6 -4 0 15.30 4.40 -6 4 0 19.40 3.90 6 4 0 17.10 3.90 6 4 0 18.70 3.50 -6 4 0 19.30 3.30 6 4 0 27.20 5.10 -6 4 0 22.60 4.10 -6 4 0 12.50 3.30 6 4 0 14.50 3.30 7 -4 0 18.40 5.30 -7 -4 0 27.70 4.90 -7 -4 0 19.50 3.90 -7 -4 0 19.70 4.70 7 -4 0 16.90 4.40 7 -4 0 19.00 5.10 7 4 0 26.00 4.70 7 4 0 19.90 4.90 -7 4 0 18.90 4.40 -7 4 0 15.10 4.60 -7 4 0 12.10 3.50 7 4 0 22.60 4.40 -7 4 0 17.30 4.00 7 4 0 33.30 6.00 -8 -4 0 4.10 2.50 8 -4 0 4.10 3.20 8 -4 0 0.40 2.90 -8 -4 0 7.80 3.60 8 -4 0 3.00 3.40 -8 -4 0 4.20 2.90 -8 4 0 8.10 4.40 8 4 0 5.40 3.80 -8 4 0 3.10 2.70 8 4 0 8.30 3.50 -8 4 0 7.80 3.60 -8 4 0 5.00 2.90 8 4 0 6.90 3.40 0 -5 0 1380.46 37.60 0 -5 0 1379.46 36.40 0 -5 0 1351.26 36.70 0 -5 0 1315.27 35.40 0 5 0 1325.17 38.20 0 5 0 1365.96 37.10 0 5 0 1324.27 34.80 0 5 0 1299.87 37.40 0 5 0 1324.57 37.80 0 5 0 1283.77 37.40 1 -5 0 659.03 21.90 1 -5 0 737.73 22.20 -1 -5 0 739.23 20.40 1 -5 0 710.23 21.40 1 -5 0 689.43 20.80 -1 -5 0 754.72 20.40 1 -5 0 720.03 21.40 -1 -5 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152.48 6.30 -4 -5 0 161.58 7.80 -4 -5 0 142.99 7.20 4 -5 0 143.39 8.40 4 -5 0 146.39 8.20 -4 -5 0 151.28 5.90 -4 -5 0 154.48 7.70 4 -5 0 137.59 8.20 4 -5 0 145.59 8.00 4 -5 0 159.68 8.90 -4 5 0 145.79 7.80 -4 5 0 152.88 6.90 4 5 0 153.68 6.60 4 5 0 148.19 7.70 -4 5 0 144.29 7.60 -4 5 0 148.89 6.30 4 5 0 143.79 8.00 4 5 0 156.68 6.20 4 5 0 147.39 8.10 4 5 0 160.68 6.60 -4 5 0 154.38 5.20 -4 5 0 148.09 7.90 4 5 0 141.09 7.60 -5 -5 0 15.00 3.10 -5 -5 0 15.20 2.60 -5 -5 0 12.10 2.20 5 -5 0 10.60 3.50 -5 -5 0 13.90 2.10 5 -5 0 15.90 3.70 -5 -5 0 14.20 3.10 -5 -5 0 13.20 2.70 5 -5 0 15.10 3.40 5 -5 0 13.10 3.30 5 -5 0 18.20 3.70 5 5 0 10.80 2.60 -5 5 0 17.40 3.20 5 5 0 12.10 3.00 -5 5 0 17.30 3.60 5 5 0 8.60 2.40 5 5 0 13.30 2.30 -5 5 0 13.40 2.90 -5 5 0 17.80 2.90 5 5 0 13.50 3.10 -6 -5 0 7.10 2.80 6 -5 0 5.70 2.90 6 -5 0 15.50 4.80 -6 -5 0 6.10 2.50 6 -5 0 7.80 2.80 6 -5 0 8.80 3.00 6 -5 0 9.60 3.40 -6 -5 0 4.60 2.20 6 5 0 5.10 2.20 6 5 0 9.60 3.30 -6 5 0 8.40 2.80 6 5 0 4.70 2.20 6 5 0 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131.69 6.30 -2 6 0 122.89 6.10 2 6 0 120.89 6.10 2 6 0 124.89 6.20 2 6 0 131.69 5.30 -2 6 0 129.09 5.50 2 6 0 134.89 6.20 -2 6 0 130.39 5.00 -2 6 0 123.89 6.30 -2 6 0 136.79 6.30 -3 -6 0 104.09 4.80 3 -6 0 103.39 6.00 3 -6 0 97.29 6.00 3 -6 0 95.89 6.10 -3 -6 0 96.59 5.20 3 -6 0 93.49 5.90 -3 -6 0 94.79 5.40 3 -6 0 98.79 6.10 -3 6 0 95.19 5.80 3 6 0 88.79 5.70 -3 6 0 91.89 4.20 3 6 0 102.09 4.70 -3 6 0 102.19 5.90 3 6 0 102.09 5.80 3 6 0 91.09 5.70 3 6 0 93.19 3.70 -3 6 0 105.09 5.80 -3 6 0 104.79 5.10 4 -6 0 161.58 9.20 -4 -6 0 193.88 8.10 -4 -6 0 184.28 8.50 4 -6 0 174.58 9.10 4 -6 0 152.98 9.20 4 -6 0 179.28 9.60 -4 -6 0 188.48 7.00 -4 -6 0 183.58 8.60 -4 -6 0 176.88 6.50 4 -6 0 167.98 9.30 4 6 0 175.18 9.20 4 6 0 165.48 9.00 -4 6 0 176.68 7.60 -4 6 0 177.48 8.80 -4 6 0 180.18 6.90 4 6 0 172.08 6.60 4 6 0 164.38 8.60 -4 6 0 181.28 9.20 -4 6 0 175.58 9.00 4 6 0 174.28 7.30 -5 -6 0 36.80 4.80 -5 -6 0 41.90 5.20 5 -6 0 40.50 5.80 5 -6 0 35.70 5.30 5 -6 0 43.80 6.20 5 -6 0 45.50 6.10 5 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143.69 8.20 -4 7 0 143.89 8.10 -4 7 0 146.19 8.30 4 7 0 149.59 8.60 4 7 0 143.49 8.40 5 -7 0 86.49 7.20 -5 -7 0 84.09 6.00 5 -7 0 74.69 6.60 -5 -7 0 88.59 6.10 5 -7 0 66.79 7.50 5 -7 0 71.69 7.90 5 -7 0 98.89 9.80 5 7 0 89.89 6.60 5 7 0 70.69 7.70 5 7 0 76.79 6.70 -5 7 0 72.59 6.40 -5 7 0 78.19 6.30 -5 7 0 78.79 6.30 -5 7 0 84.29 5.30 6 -7 0 4.30 2.60 6 -7 0 12.20 3.90 -6 -7 0 9.50 2.90 6 -7 0 8.70 4.10 -6 -7 0 5.20 2.20 -6 -7 0 11.60 3.20 -6 7 0 6.70 2.80 6 7 0 6.90 3.00 -6 7 0 9.40 3.30 6 7 0 9.00 3.00 6 7 0 3.40 2.40 -6 7 0 10.70 3.30 7 -7 0 186.98 14.20 7 -7 0 208.08 13.60 7 -7 0 176.88 13.30 -7 -7 0 201.58 11.90 -7 -7 0 175.88 10.70 7 7 0 193.08 12.00 -7 7 0 202.58 12.30 -7 7 0 177.58 11.60 7 7 0 218.98 13.70 7 7 0 179.48 12.80 -7 7 0 204.18 13.00 0 -8 0 193.48 7.80 0 -8 0 197.28 7.10 0 -8 0 193.38 7.30 0 8 0 187.08 7.60 0 8 0 185.38 7.50 0 8 0 182.28 8.00 0 8 0 189.98 7.50 0 8 0 186.48 7.20 0 8 0 184.48 7.30 1 -8 0 286.27 9.10 1 -8 0 282.17 10.60 -1 -8 0 278.27 8.80 1 -8 0 265.27 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10.10 -4 -8 0 224.78 9.70 4 -8 0 229.68 11.70 -4 8 0 239.28 11.40 4 8 0 213.08 11.00 -4 8 0 222.38 11.00 4 8 0 224.78 10.90 4 8 0 223.28 11.30 -4 8 0 243.18 11.20 -4 8 0 239.58 9.40 5 -8 0 78.39 8.20 5 -8 0 67.89 8.00 -5 -8 0 76.49 5.60 5 -8 0 71.79 8.50 -5 -8 0 69.29 5.60 5 -8 0 74.59 8.70 -5 8 0 66.09 4.90 -5 8 0 90.29 7.10 5 8 0 86.19 6.60 5 8 0 78.59 8.30 5 8 0 62.39 7.20 -5 8 0 70.49 6.10 -5 8 0 57.29 6.40 6 -8 0 59.59 8.20 6 -8 0 47.10 7.20 -6 -8 0 45.70 6.10 -6 -8 0 47.10 5.70 -6 -8 0 47.70 5.80 6 -8 0 50.49 8.00 -6 8 0 53.59 6.80 -6 8 0 56.29 7.20 -6 8 0 49.40 7.00 6 8 0 48.80 7.30 6 8 0 50.19 6.40 6 8 0 45.80 6.80 7 -8 0 13.10 4.80 7 -8 0 16.50 5.50 -7 -8 0 18.90 4.40 7 -8 0 13.90 4.50 -7 -8 0 22.70 4.40 -7 8 0 19.30 4.80 7 8 0 18.70 4.80 7 8 0 20.80 5.40 7 8 0 29.90 5.70 -7 8 0 21.10 4.80 -7 8 0 18.80 5.00 0 -9 0 56.19 3.40 0 -9 0 48.60 3.60 0 -9 0 54.19 3.60 0 -9 0 54.29 3.30 0 9 0 58.39 3.50 0 9 0 50.89 3.70 0 9 0 52.49 4.00 0 9 0 45.90 3.20 0 9 0 51.09 3.50 0 9 0 51.69 3.60 1 -9 0 49.60 3.80 -1 -9 0 45.50 2.70 -1 -9 0 52.19 3.70 -1 -9 0 54.29 3.40 1 -9 0 45.20 3.70 1 -9 0 50.69 2.80 1 -9 0 47.60 3.60 1 -9 0 47.10 3.60 -1 9 0 50.29 3.20 -1 9 0 51.49 3.70 -1 9 0 54.39 2.90 -1 9 0 54.99 4.20 1 9 0 39.40 2.70 1 9 0 44.50 3.40 1 9 0 51.19 3.80 -1 9 0 51.89 3.60 1 9 0 45.80 3.50 -1 9 0 53.89 3.90 1 9 0 56.99 4.10 -2 -9 0 98.19 4.00 2 -9 0 88.79 5.90 2 -9 0 99.99 6.00 -2 -9 0 96.99 5.40 -2 -9 0 100.39 5.10 2 -9 0 101.09 5.90 2 -9 0 84.79 5.70 -2 9 0 95.19 5.80 -2 9 0 89.79 5.80 2 9 0 100.79 6.00 -2 9 0 97.89 6.10 2 9 0 101.29 5.80 2 9 0 110.49 6.30 -2 9 0 85.39 4.30 2 9 0 96.89 4.90 -2 9 0 94.89 5.20 -3 -9 0 375.36 14.50 3 -9 0 384.66 15.70 3 -9 0 411.66 16.20 3 -9 0 399.46 16.00 -3 -9 0 396.26 13.80 3 -9 0 445.86 16.80 -3 9 0 424.76 16.30 -3 9 0 414.76 15.90 -3 9 0 406.26 13.70 3 9 0 391.16 15.60 3 9 0 417.16 16.20 3 9 0 370.16 15.30 -3 9 0 415.56 12.80 -3 9 0 376.26 15.60 4 -9 0 12.90 3.30 4 -9 0 6.00 2.60 -4 -9 0 6.10 2.00 -4 -9 0 6.40 2.20 4 -9 0 8.10 2.80 4 -9 0 13.30 3.30 -4 9 0 7.50 2.70 4 9 0 8.10 2.70 -4 9 0 10.80 2.90 4 9 0 5.00 2.50 4 9 0 8.20 2.60 -4 9 0 10.00 2.10 -4 9 0 6.90 2.40 5 -9 0 36.20 5.90 5 -9 0 23.80 5.10 -5 -9 0 33.30 4.60 -5 -9 0 34.90 4.60 5 -9 0 41.20 6.60 5 -9 0 33.30 5.50 -5 9 0 31.70 5.20 5 9 0 38.20 5.40 -5 9 0 29.90 4.70 5 9 0 41.30 6.30 -5 9 0 29.90 5.00 5 9 0 30.00 5.30 6 -9 0 21.90 5.70 6 -9 0 23.10 5.30 -6 -9 0 17.70 3.70 -6 -9 0 17.40 4.00 6 -9 0 10.80 3.60 6 9 0 19.40 4.80 -6 9 0 21.20 4.40 6 9 0 22.80 5.00 -6 9 0 21.50 5.10 -6 9 0 17.80 4.20 6 9 0 15.90 3.80 7 -9 0 26.90 6.80 7 -9 0 31.20 7.20 7 -9 0 24.50 5.90 -7 -9 0 30.20 5.30 -7 -9 0 32.90 5.80 -7 9 0 20.70 5.40 -7 9 0 24.10 5.10 7 9 0 27.40 5.60 7 9 0 38.50 7.20 -7 9 0 33.40 6.00 7 9 0 15.10 4.70 0 -10 0 290.07 10.60 0 -10 0 279.97 11.10 0 -10 0 288.47 10.60 0 -10 0 286.17 10.20 0 10 0 271.27 10.80 0 10 0 289.47 10.80 0 10 0 280.27 10.90 0 10 0 297.57 10.70 0 10 0 259.67 10.30 0 10 0 278.47 11.50 1 -10 0 23.40 3.30 1 -10 0 30.70 3.50 1 -10 0 20.40 2.20 -1 -10 0 17.10 2.60 1 -10 0 17.80 3.00 1 -10 0 27.70 3.50 -1 -10 0 23.60 2.00 -1 -10 0 28.70 3.10 -1 10 0 21.80 3.00 -1 10 0 22.00 2.60 -1 10 0 23.20 3.20 -1 10 0 20.40 2.80 1 10 0 24.20 3.30 1 10 0 24.70 3.30 -1 10 0 21.40 3.40 -1 10 0 24.80 2.50 1 10 0 20.40 2.80 1 10 0 17.80 2.10 1 10 0 21.00 2.90 -2 -10 0 591.94 18.60 2 -10 0 611.64 21.00 -2 -10 0 574.64 19.80 2 -10 0 609.64 20.70 2 -10 0 597.64 20.30 2 -10 0 610.84 21.40 -2 10 0 586.14 20.90 2 10 0 570.94 20.10 -2 10 0 663.93 18.70 -2 10 0 596.94 18.80 2 10 0 556.44 20.60 -2 10 0 593.74 20.90 -2 10 0 602.14 21.60 2 10 0 610.34 21.00 -3 -10 0 189.58 9.00 3 -10 0 183.68 9.90 -3 -10 0 186.68 8.20 3 -10 0 192.48 10.10 3 -10 0 192.88 10.30 3 -10 0 186.88 10.10 3 10 0 175.58 9.80 -3 10 0 189.98 10.10 3 10 0 205.08 10.30 -3 10 0 191.88 9.90 -3 10 0 198.18 8.40 -3 10 0 178.58 9.70 3 10 0 180.08 9.50 -4 -10 0 531.25 19.90 -4 -10 0 550.74 18.80 4 -10 0 571.74 22.40 4 -10 0 575.24 22.10 4 -10 0 536.55 21.90 4 -10 0 598.84 22.90 -4 10 0 563.84 21.60 -4 10 0 578.34 22.10 4 10 0 575.04 21.70 -4 10 0 576.64 18.50 4 10 0 592.84 21.80 -4 10 0 517.65 21.50 4 10 0 572.34 22.20 -5 -10 0 18.60 3.30 -5 -10 0 18.40 3.80 5 -10 0 13.70 4.20 -5 -10 0 20.70 3.80 5 -10 0 22.30 5.10 5 -10 0 24.50 5.10 5 -10 0 21.50 4.80 5 10 0 16.90 4.30 5 10 0 11.40 3.80 5 10 0 14.40 3.50 -5 10 0 17.90 4.00 -5 10 0 12.40 3.60 -5 10 0 19.40 4.60 -6 -10 0 5.60 2.50 6 -10 0 1.70 2.90 -6 -10 0 2.40 2.10 6 -10 0 3.50 3.10 6 -10 0 4.70 2.90 6 10 0 1.30 2.20 -6 10 0 9.00 3.70 6 10 0 2.30 2.60 -6 10 0 1.40 2.40 -6 10 0 1.20 2.20 6 10 0 2.80 2.50 0 -11 0 16.80 2.70 0 -11 0 17.90 2.50 0 -11 0 17.30 2.60 0 -11 0 20.50 2.70 0 11 0 16.40 2.50 0 11 0 21.70 2.90 0 11 0 24.40 3.40 0 11 0 18.50 3.00 0 11 0 24.70 3.00 0 11 0 18.00 2.60 -1 -11 0 5.90 1.90 1 -11 0 8.00 2.30 -1 -11 0 3.90 1.50 1 -11 0 2.90 1.50 -1 -11 0 3.70 1.40 -1 -11 0 4.50 1.20 1 -11 0 2.60 1.40 1 11 0 4.70 1.60 1 11 0 1.00 1.10 1 11 0 5.30 1.90 -1 11 0 9.10 2.30 -1 11 0 8.00 1.60 1 11 0 2.60 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2.50 5 11 0 4.40 2.80 -5 11 0 1.80 2.10 5 11 0 4.00 2.30 -5 11 0 3.60 2.50 5 11 0 1.90 2.40 6 -11 0 101.59 11.20 -6 -11 0 113.29 9.00 -6 -11 0 111.09 8.10 6 -11 0 105.39 11.90 6 -11 0 105.79 12.10 6 11 0 87.09 10.10 -6 11 0 106.19 9.10 6 11 0 101.49 11.50 -6 11 0 107.29 11.70 6 11 0 107.39 9.00 -6 11 0 125.09 9.80 0 -12 0 11.70 2.60 0 -12 0 12.20 2.40 0 12 0 13.40 2.40 0 12 0 14.90 2.60 -1 -12 0 10.10 2.50 -1 -12 0 11.30 2.50 -1 -12 0 14.10 2.50 1 -12 0 11.90 2.60 1 -12 0 13.10 2.80 1 -12 0 14.60 2.80 -1 12 0 13.40 2.90 -1 12 0 15.70 3.00 1 12 0 16.20 3.30 1 12 0 15.70 2.90 1 12 0 13.10 2.80 -1 12 0 14.40 2.70 -1 12 0 17.40 3.50 -1 12 0 14.30 2.40 -2 -12 0 21.80 3.70 2 -12 0 15.80 3.20 2 -12 0 17.10 3.40 -2 -12 0 18.20 3.30 2 -12 0 18.80 3.80 -2 -12 0 16.50 2.70 2 -12 0 11.70 3.00 -2 12 0 13.50 2.90 -2 12 0 19.40 3.00 2 12 0 15.00 3.30 -2 12 0 16.10 3.30 2 12 0 18.80 3.40 -2 12 0 19.80 3.90 2 12 0 18.10 3.60 3 -12 0 19.00 4.00 -3 -12 0 20.50 3.10 -3 -12 0 18.80 3.30 -3 -12 0 20.10 3.80 3 -12 0 16.90 3.80 3 -12 0 20.50 4.20 3 -12 0 22.40 4.40 -3 12 0 22.60 3.30 -3 12 0 24.20 4.40 3 12 0 21.60 4.00 3 12 0 22.60 4.10 3 12 0 20.80 4.10 -3 12 0 18.90 3.80 -3 12 0 20.70 3.90 -4 -12 0 23.60 4.60 4 -12 0 22.60 4.90 4 -12 0 17.90 4.30 4 -12 0 25.50 4.90 -4 -12 0 22.30 3.60 4 -12 0 22.80 4.80 -4 -12 0 26.10 4.30 -4 12 0 24.60 4.50 -4 12 0 20.00 3.20 -4 12 0 20.80 4.50 -4 12 0 24.90 4.90 4 12 0 25.90 4.80 4 12 0 33.70 6.00 4 12 0 20.50 4.50 -5 -12 0 6.00 3.00 5 -12 0 3.40 2.60 5 -12 0 13.20 4.40 5 -12 0 10.70 3.90 -5 -12 0 10.20 2.90 -5 12 0 4.50 2.90 5 12 0 8.90 3.40 -5 12 0 13.60 4.00 5 12 0 13.50 3.90 -5 12 0 7.40 3.20 5 12 0 7.00 3.60 6 -12 0 49.80 8.00 6 -12 0 31.60 6.70 6 -12 0 20.40 5.90 -6 -12 0 32.80 5.30 -6 -12 0 30.70 5.90 6 12 0 38.40 6.80 6 12 0 30.30 6.30 -6 12 0 25.60 5.50 -6 12 0 32.10 6.70 6 12 0 37.10 6.80 -6 12 0 30.30 5.80 0 -13 0 360.56 14.00 0 -13 0 343.47 14.60 0 13 0 355.76 14.20 0 13 0 367.86 13.80 0 13 0 359.96 15.20 0 13 0 379.76 14.50 1 -13 0 2.20 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