# Electronic Supplementary Material (ESI) for Organic Chemistry Frontiers. # This journal is © the Partner Organisations 2015 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_TZ888_2_0m_a _database_code_depnum_ccdc_archive 'CCDC 1423805' _audit_update_record ; 2015-09-11 deposited with the CCDC. 2015-10-15 downloaded from the CCDC. ; _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 'C26 H23 F6 N2 O P2 Rh' _chemical_formula_weight 658.31 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 '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/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.6439(13) _cell_length_b 11.6245(14) _cell_length_c 21.782(3) _cell_angle_alpha 90 _cell_angle_beta 100.416(2) _cell_angle_gamma 90 _cell_volume 2650.7(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 'clear light yellow' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.650 _exptl_crystal_F_000 1320 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.389 _exptl_crystal_size_mid 0.319 _exptl_crystal_size_min 0.112 _exptl_absorpt_coefficient_mu 0.831 _shelx_estimated_absorpt_T_min 0.738 _shelx_estimated_absorpt_T_max 0.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_T_max 0.91 _exptl_absorpt_process_details 'SADABS V2014/5 (Bruker AXS Inc.)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker ApexII Triumph monochromator sealed tube' _diffrn_measurement_method 'Photon 50 CMOS detector' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30389 _diffrn_reflns_av_unetI/netI 0.0442 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.903 _diffrn_reflns_theta_max 24.997 _diffrn_reflns_theta_full 24.997 _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 4661 _reflns_number_gt 3905 _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^)+(0.0524P)^2^+5.0183P] 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 4661 _refine_ls_number_parameters 346 _refine_ls_number_restraints 334 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0948 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _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 Rh1 Rh 0.42179(3) 0.38207(2) 0.32221(2) 0.01866(11) Uani 1 1 d . U . . . P1 P 0.27115(9) 0.42056(8) 0.37710(4) 0.0188(2) Uani 1 1 d . U . . . N1 N 0.2739(3) 0.3091(2) 0.26109(13) 0.0183(6) Uani 1 1 d . U . . . N2 N 0.5289(3) 0.3087(3) 0.25654(14) 0.0216(6) Uani 1 1 d D U . . . H2 H 0.589(3) 0.264(3) 0.2764(18) 0.026 Uiso 1 1 d D U . . . C20 C 0.5469(4) 0.4588(4) 0.37535(18) 0.0275(8) Uani 1 1 d . U . . . O1 O 0.6214(3) 0.5127(3) 0.40771(14) 0.0460(8) Uani 1 1 d . U . . . C1 C 0.4446(4) 0.2236(3) 0.21676(17) 0.0239(8) Uani 1 1 d . U . . . H1A H 0.4642 0.1454 0.2339 0.029 Uiso 1 1 calc R U . . . H1B H 0.4643 0.2251 0.1741 0.029 Uiso 1 1 calc R U . . . C2 C 0.3043(4) 0.2470(3) 0.21316(16) 0.0209(7) Uani 1 1 d . U . . . C3 C 0.2110(4) 0.2037(3) 0.16679(17) 0.0255(8) Uani 1 1 d . U . . . H3 H 0.2337 0.1634 0.1324 0.031 Uiso 1 1 calc R U . . . C4 C 0.0836(4) 0.2196(3) 0.17084(17) 0.0271(8) Uani 1 1 d . U . . . H4 H 0.0180 0.1891 0.1397 0.033 Uiso 1 1 calc R U . . . C5 C 0.0534(4) 0.2804(3) 0.22080(17) 0.0250(8) Uani 1 1 d . U . . . H5 H -0.0333 0.2906 0.2247 0.030 Uiso 1 1 calc R U . . . C6 C 0.1502(3) 0.3264(3) 0.26506(16) 0.0198(7) Uani 1 1 d . U . . . C7 C 0.1257(3) 0.4037(3) 0.31696(16) 0.0219(8) Uani 1 1 d . U . . . H7A H 0.0564 0.3707 0.3363 0.026 Uiso 1 1 calc R U . . . H7B H 0.0973 0.4801 0.2997 0.026 Uiso 1 1 calc R U . . . C8 C 0.2501(3) 0.5598(3) 0.41179(16) 0.0212(7) Uani 1 1 d . U . . . C9 C 0.2070(4) 0.5712(4) 0.46810(18) 0.0312(9) Uani 1 1 d . U . . . H9 H 0.1878 0.5047 0.4900 0.037 Uiso 1 1 calc R U . . . C10 C 0.1919(5) 0.6796(4) 0.49212(19) 0.0371(10) Uani 1 1 d . U . . . H10 H 0.1624 0.6870 0.5306 0.045 Uiso 1 1 calc R U . . . C11 C 0.2193(4) 0.7772(4) 0.4609(2) 0.0344(10) Uani 1 1 d . U . . . H11 H 0.2096 0.8512 0.4780 0.041 Uiso 1 1 calc R U . . . C12 C 0.2612(4) 0.7664(3) 0.40450(18) 0.0299(9) Uani 1 1 d . U . . . H12 H 0.2786 0.8333 0.3824 0.036 Uiso 1 1 calc R U . . . C13 C 0.2776(4) 0.6587(3) 0.38030(17) 0.0258(8) Uani 1 1 d . U . . . H13 H 0.3078 0.6519 0.3420 0.031 Uiso 1 1 calc R U . . . C14 C 0.2671(4) 0.3148(3) 0.43853(16) 0.0212(7) Uani 1 1 d . U . . . C15 C 0.3827(4) 0.2755(4) 0.47228(17) 0.0277(8) Uani 1 1 d . U . . . H15 H 0.4607 0.3062 0.4639 0.033 Uiso 1 1 calc R U . . . C16 C 0.3852(4) 0.1922(4) 0.51799(19) 0.0351(10) Uani 1 1 d . U . . . H16 H 0.4646 0.1669 0.5413 0.042 Uiso 1 1 calc R U . . . C17 C 0.2721(4) 0.1456(4) 0.52965(19) 0.0362(10) Uani 1 1 d . U . . . H17 H 0.2736 0.0872 0.5602 0.043 Uiso 1 1 calc R U . . . C18 C 0.1573(4) 0.1847(4) 0.49662(19) 0.0367(10) Uani 1 1 d . U . . . H18 H 0.0796 0.1536 0.5050 0.044 Uiso 1 1 calc R U . . . C19 C 0.1542(4) 0.2688(4) 0.45131(17) 0.0289(9) Uani 1 1 d . U . . . H19 H 0.0745 0.2951 0.4289 0.035 Uiso 1 1 calc R U . . . C21 C 0.5848(4) 0.3965(3) 0.22225(16) 0.0197(7) Uani 1 1 d . U . . . C22 C 0.5111(4) 0.4527(3) 0.17189(17) 0.0252(8) Uani 1 1 d . U . . . H22 H 0.4228 0.4356 0.1600 0.030 Uiso 1 1 calc R U . . . C23 C 0.5679(4) 0.5337(3) 0.13932(18) 0.0307(9) Uani 1 1 d . U . . . H23 H 0.5181 0.5716 0.1046 0.037 Uiso 1 1 calc R U . . . C24 C 0.6957(4) 0.5604(3) 0.15645(19) 0.0298(9) Uani 1 1 d . U . . . H24 H 0.7344 0.6149 0.1332 0.036 Uiso 1 1 calc R U . . . C25 C 0.7669(4) 0.5069(3) 0.20795(19) 0.0286(9) Uani 1 1 d . U . . . H25 H 0.8546 0.5260 0.2205 0.034 Uiso 1 1 calc R U . . . C26 C 0.7121(4) 0.4255(3) 0.24147(18) 0.0253(8) Uani 1 1 d . U . . . H26 H 0.7612 0.3901 0.2772 0.030 Uiso 1 1 calc R U . . . P2 P 0.16328(9) 0.62625(9) 0.15430(4) 0.0240(2) Uani 1 1 d . U . . . F1 F 0.1174(3) 0.6065(2) 0.08197(11) 0.0432(7) Uani 1 1 d . U . . . F2 F 0.2013(2) 0.4944(2) 0.16359(12) 0.0391(6) Uani 1 1 d . U . . . F3 F 0.2141(3) 0.6503(3) 0.22736(12) 0.0588(8) Uani 1 1 d . U . . . F4 F 0.1281(2) 0.7611(2) 0.14535(11) 0.0371(6) Uani 1 1 d . U . . . F5 F 0.3042(2) 0.6567(2) 0.14267(15) 0.0494(7) Uani 1 1 d . U . . . F6 F 0.0254(3) 0.6017(3) 0.16739(16) 0.0582(8) Uani 1 1 d . 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 Rh1 0.01640(17) 0.02461(18) 0.01559(16) 0.00082(11) 0.00457(11) -0.00127(11) P1 0.0181(5) 0.0252(5) 0.0139(4) 0.0005(3) 0.0045(4) -0.0005(4) N1 0.0200(15) 0.0194(15) 0.0162(13) 0.0023(11) 0.0050(11) -0.0002(12) N2 0.0193(16) 0.0234(16) 0.0228(15) 0.0023(12) 0.0058(12) 0.0034(12) C20 0.024(2) 0.036(2) 0.0232(18) 0.0045(16) 0.0074(15) -0.0053(17) O1 0.0414(19) 0.059(2) 0.0344(16) -0.0041(15) -0.0026(14) -0.0235(16) C1 0.0251(19) 0.0243(19) 0.0242(18) -0.0036(15) 0.0095(15) -0.0028(15) C2 0.0229(18) 0.0198(17) 0.0212(17) 0.0018(13) 0.0075(14) -0.0001(14) C3 0.031(2) 0.028(2) 0.0181(17) -0.0012(14) 0.0070(15) -0.0002(16) C4 0.027(2) 0.030(2) 0.0228(18) -0.0034(15) 0.0004(15) -0.0010(16) C5 0.0180(18) 0.032(2) 0.0245(18) 0.0027(15) 0.0035(14) -0.0004(15) C6 0.0188(17) 0.0244(18) 0.0168(16) 0.0045(13) 0.0047(13) 0.0009(14) C7 0.0172(18) 0.031(2) 0.0179(16) 0.0008(14) 0.0034(14) 0.0019(15) C8 0.0180(18) 0.0289(18) 0.0168(16) -0.0008(14) 0.0030(14) -0.0004(15) C9 0.044(3) 0.032(2) 0.0205(18) 0.0019(15) 0.0126(17) 0.0015(18) C10 0.053(3) 0.036(2) 0.026(2) -0.0060(16) 0.0188(19) 0.0021(19) C11 0.040(3) 0.029(2) 0.035(2) -0.0066(16) 0.0091(19) 0.0012(18) C12 0.035(2) 0.027(2) 0.028(2) 0.0024(15) 0.0085(17) -0.0045(17) C13 0.027(2) 0.0298(19) 0.0223(18) 0.0015(15) 0.0088(16) -0.0014(16) C14 0.0218(18) 0.0271(19) 0.0157(16) -0.0029(14) 0.0061(13) -0.0019(14) C15 0.0229(19) 0.039(2) 0.0213(18) 0.0072(16) 0.0034(15) -0.0024(16) C16 0.033(2) 0.044(2) 0.026(2) 0.0125(18) 0.0001(17) -0.0006(18) C17 0.043(2) 0.042(2) 0.0219(19) 0.0103(17) 0.0015(17) -0.0107(19) C18 0.035(2) 0.049(3) 0.027(2) 0.0075(18) 0.0063(17) -0.0158(19) C19 0.023(2) 0.041(2) 0.0216(18) 0.0063(16) 0.0014(15) -0.0051(17) C21 0.0216(18) 0.0235(18) 0.0161(16) -0.0020(13) 0.0095(14) -0.0007(14) C22 0.0203(19) 0.032(2) 0.0242(18) 0.0025(15) 0.0055(15) 0.0044(15) C23 0.038(2) 0.030(2) 0.0263(19) 0.0066(16) 0.0127(17) 0.0063(17) C24 0.038(2) 0.023(2) 0.033(2) -0.0005(16) 0.0197(17) -0.0026(16) C25 0.025(2) 0.029(2) 0.034(2) -0.0062(16) 0.0121(16) -0.0070(16) C26 0.0248(19) 0.0260(19) 0.0255(18) -0.0048(15) 0.0055(15) -0.0001(15) P2 0.0210(5) 0.0292(5) 0.0222(5) 0.0015(4) 0.0046(4) 0.0011(4) F1 0.0582(18) 0.0428(15) 0.0258(13) -0.0031(10) -0.0001(12) 0.0030(12) F2 0.0426(15) 0.0322(13) 0.0417(14) 0.0095(10) 0.0056(12) 0.0011(11) F3 0.084(2) 0.0581(17) 0.0273(13) -0.0008(12) -0.0083(14) 0.0038(16) F4 0.0365(14) 0.0341(13) 0.0377(13) -0.0033(10) -0.0012(11) 0.0077(10) F5 0.0267(13) 0.0462(15) 0.078(2) 0.0082(14) 0.0156(13) 0.0007(12) F6 0.0390(16) 0.0672(19) 0.077(2) 0.0002(16) 0.0342(15) -0.0070(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 Rh1 C20 1.831(4) . ? Rh1 N1 2.053(3) . ? Rh1 N2 2.160(3) . ? Rh1 P1 2.2120(9) . ? P1 C8 1.817(4) . ? P1 C14 1.823(4) . ? P1 C7 1.849(4) . ? N1 C6 1.350(5) . ? N1 C2 1.356(5) . ? N2 C21 1.454(5) . ? N2 C1 1.501(5) . ? N2 H2 0.87(3) . ? C20 O1 1.147(5) . ? C1 C2 1.506(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.377(5) . ? C3 C4 1.387(5) . ? C3 H3 0.9500 . ? C4 C5 1.384(5) . ? C4 H4 0.9500 . ? C5 C6 1.384(5) . ? C5 H5 0.9500 . ? C6 C7 1.503(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.392(5) . ? C8 C13 1.397(5) . ? C9 C10 1.385(6) . ? C9 H9 0.9500 . ? C10 C11 1.380(6) . ? C10 H10 0.9500 . ? C11 C12 1.386(6) . ? C11 H11 0.9500 . ? C12 C13 1.382(6) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.389(5) . ? C14 C15 1.391(5) . ? C15 C16 1.386(5) . ? C15 H15 0.9500 . ? C16 C17 1.385(6) . ? C16 H16 0.9500 . ? C17 C18 1.378(6) . ? C17 H17 0.9500 . ? C18 C19 1.386(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C21 C26 1.386(5) . ? C21 C22 1.390(5) . ? C22 C23 1.382(5) . ? C22 H22 0.9500 . ? C23 C24 1.380(6) . ? C23 H23 0.9500 . ? C24 C25 1.383(6) . ? C24 H24 0.9500 . ? C25 C26 1.386(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? P2 F6 1.571(3) . ? P2 F1 1.580(3) . ? P2 F2 1.589(3) . ? P2 F5 1.605(3) . ? P2 F3 1.610(3) . ? P2 F4 1.615(3) . ? 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 C20 Rh1 N1 175.19(15) . . ? C20 Rh1 N2 101.55(15) . . ? N1 Rh1 N2 80.91(12) . . ? C20 Rh1 P1 94.32(12) . . ? N1 Rh1 P1 83.59(8) . . ? N2 Rh1 P1 163.53(9) . . ? C8 P1 C14 105.92(16) . . ? C8 P1 C7 103.80(17) . . ? C14 P1 C7 108.70(17) . . ? C8 P1 Rh1 124.11(12) . . ? C14 P1 Rh1 112.08(12) . . ? C7 P1 Rh1 101.05(12) . . ? C6 N1 C2 120.0(3) . . ? C6 N1 Rh1 122.6(2) . . ? C2 N1 Rh1 117.2(2) . . ? C21 N2 C1 115.0(3) . . ? C21 N2 Rh1 112.1(2) . . ? C1 N2 Rh1 108.1(2) . . ? C21 N2 H2 110(3) . . ? C1 N2 H2 102(3) . . ? Rh1 N2 H2 109(3) . . ? O1 C20 Rh1 176.0(4) . . ? N2 C1 C2 113.2(3) . . ? N2 C1 H1A 108.9 . . ? C2 C1 H1A 108.9 . . ? N2 C1 H1B 108.9 . . ? C2 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? N1 C2 C3 121.2(3) . . ? N1 C2 C1 115.4(3) . . ? C3 C2 C1 123.3(3) . . ? C2 C3 C4 119.2(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 119.1(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 119.7(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? N1 C6 C5 120.6(3) . . ? N1 C6 C7 116.2(3) . . ? C5 C6 C7 123.1(3) . . ? C6 C7 P1 111.0(3) . . ? C6 C7 H7A 109.4 . . ? P1 C7 H7A 109.4 . . ? C6 C7 H7B 109.4 . . ? P1 C7 H7B 109.4 . . ? H7A C7 H7B 108.0 . . ? C9 C8 C13 119.1(4) . . ? C9 C8 P1 122.4(3) . . ? C13 C8 P1 118.5(3) . . ? C10 C9 C8 119.9(4) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C11 C10 C9 120.8(4) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.5(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 120.4(3) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? C19 C14 C15 118.8(3) . . ? C19 C14 P1 122.9(3) . . ? C15 C14 P1 118.2(3) . . ? C16 C15 C14 120.6(4) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 120.0(4) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 119.6(4) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 120.6(4) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C18 C19 C14 120.3(4) . . ? C18 C19 H19 119.8 . . ? C14 C19 H19 119.8 . . ? C26 C21 C22 120.3(3) . . ? C26 C21 N2 118.9(3) . . ? C22 C21 N2 120.7(3) . . ? C23 C22 C21 119.2(4) . . ? C23 C22 H22 120.4 . . ? C21 C22 H22 120.4 . . ? C24 C23 C22 121.1(4) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 119.1(4) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 120.9(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 C25 119.3(4) . . ? C21 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? F6 P2 F1 91.39(17) . . ? F6 P2 F2 91.51(16) . . ? F1 P2 F2 90.70(14) . . ? F6 P2 F5 177.39(18) . . ? F1 P2 F5 90.22(16) . . ? F2 P2 F5 90.53(14) . . ? F6 P2 F3 90.58(18) . . ? F1 P2 F3 177.64(18) . . ? F2 P2 F3 90.56(15) . . ? F5 P2 F3 87.77(18) . . ? F6 P2 F4 89.67(15) . . ? F1 P2 F4 89.87(14) . . ? F2 P2 F4 178.68(15) . . ? F5 P2 F4 88.28(14) . . ? F3 P2 F4 88.83(15) . . ? _refine_diff_density_max 1.316 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.104 _shelx_res_file ; TZ888_2_0m_a.res created by SHELXL-2014/7 TITL TZ888_2_0m_a.res in P2(1)/c CELL 0.71073 10.6439 11.6245 21.7819 90.000 100.416 90.000 ZERR 4.000 0.0013 0.0014 0.0025 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O F P Rh UNIT 104 92 8 4 24 8 4 REM Old TITL TZ888_2_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.093, Rweak 0.002, Alpha 0.030, Orientation as input REM Formula found by SHELXT: C26 N O2 F6 P2 Rh L.S. 10 BOND $H FMAP 2 ACTA OMIT 0 1 1 OMIT 1 0 0 OMIT -2 50 PLAN 10 SIZE 0.112 0.319 0.389 DFIX 0.9 0.03 N2 H2 RIGU TEMP -123.140 WGHT 0.052400 5.018300 FVAR 0.28576 RH1 7 0.421785 0.382074 0.322214 11.00000 0.01640 0.02461 = 0.01559 0.00082 0.00457 -0.00127 P1 6 0.271154 0.420558 0.377100 11.00000 0.01806 0.02520 = 0.01389 0.00049 0.00452 -0.00050 N1 3 0.273874 0.309105 0.261087 11.00000 0.02002 0.01943 = 0.01620 0.00227 0.00502 -0.00018 N2 3 0.528942 0.308668 0.256545 11.00000 0.01926 0.02340 = 0.02282 0.00227 0.00584 0.00340 H2 2 0.588666 0.264021 0.276439 11.00000 -1.20000 C20 1 0.546902 0.458786 0.375347 11.00000 0.02415 0.03637 = 0.02316 0.00449 0.00740 -0.00529 O1 4 0.621406 0.512662 0.407710 11.00000 0.04144 0.05859 = 0.03444 -0.00412 -0.00264 -0.02346 C1 1 0.444631 0.223589 0.216761 11.00000 0.02506 0.02428 = 0.02418 -0.00362 0.00952 -0.00279 AFIX 23 H1A 2 0.464178 0.145414 0.233879 11.00000 -1.20000 H1B 2 0.464334 0.225138 0.174056 11.00000 -1.20000 AFIX 0 C2 1 0.304307 0.247004 0.213165 11.00000 0.02294 0.01981 = 0.02117 0.00183 0.00748 -0.00009 C3 1 0.211041 0.203713 0.166793 11.00000 0.03102 0.02823 = 0.01807 -0.00117 0.00701 -0.00019 AFIX 43 H3 2 0.233690 0.163438 0.132438 11.00000 -1.20000 AFIX 0 C4 1 0.083618 0.219611 0.170839 11.00000 0.02654 0.03040 = 0.02284 -0.00343 0.00040 -0.00099 AFIX 43 H4 2 0.017954 0.189125 0.139709 11.00000 -1.20000 AFIX 0 C5 1 0.053415 0.280442 0.220803 11.00000 0.01801 0.03235 = 0.02453 0.00272 0.00349 -0.00040 AFIX 43 H5 2 -0.033340 0.290621 0.224725 11.00000 -1.20000 AFIX 0 C6 1 0.150184 0.326410 0.265056 11.00000 0.01876 0.02445 = 0.01683 0.00452 0.00466 0.00094 C7 1 0.125662 0.403685 0.316959 11.00000 0.01724 0.03078 = 0.01787 0.00078 0.00339 0.00194 AFIX 23 H7A 2 0.056376 0.370735 0.336288 11.00000 -1.20000 H7B 2 0.097330 0.480081 0.299688 11.00000 -1.20000 AFIX 0 C8 1 0.250094 0.559815 0.411788 11.00000 0.01796 0.02888 = 0.01678 -0.00085 0.00303 -0.00038 C9 1 0.206954 0.571226 0.468097 11.00000 0.04377 0.03194 = 0.02052 0.00191 0.01261 0.00150 AFIX 43 H9 2 0.187832 0.504725 0.490034 11.00000 -1.20000 AFIX 0 C10 1 0.191927 0.679650 0.492122 11.00000 0.05348 0.03567 = 0.02643 -0.00603 0.01877 0.00206 AFIX 43 H10 2 0.162381 0.686969 0.530564 11.00000 -1.20000 AFIX 0 C11 1 0.219344 0.777199 0.460908 11.00000 0.04021 0.02940 = 0.03454 -0.00663 0.00914 0.00120 AFIX 43 H11 2 0.209611 0.851196 0.477960 11.00000 -1.20000 AFIX 0 C12 1 0.261183 0.766423 0.404500 11.00000 0.03500 0.02737 = 0.02831 0.00242 0.00854 -0.00447 AFIX 43 H12 2 0.278619 0.833294 0.382411 11.00000 -1.20000 AFIX 0 C13 1 0.277606 0.658720 0.380303 11.00000 0.02699 0.02984 = 0.02226 0.00145 0.00882 -0.00145 AFIX 43 H13 2 0.307806 0.651902 0.342004 11.00000 -1.20000 AFIX 0 C14 1 0.267128 0.314835 0.438526 11.00000 0.02177 0.02715 = 0.01565 -0.00289 0.00614 -0.00193 C15 1 0.382729 0.275548 0.472283 11.00000 0.02291 0.03885 = 0.02126 0.00719 0.00341 -0.00239 AFIX 43 H15 2 0.460669 0.306152 0.463927 11.00000 -1.20000 AFIX 0 C16 1 0.385249 0.192173 0.517992 11.00000 0.03259 0.04435 = 0.02624 0.01248 0.00005 -0.00060 AFIX 43 H16 2 0.464605 0.166943 0.541323 11.00000 -1.20000 AFIX 0 C17 1 0.272087 0.145646 0.529652 11.00000 0.04331 0.04160 = 0.02190 0.01026 0.00149 -0.01069 AFIX 43 H17 2 0.273610 0.087172 0.560246 11.00000 -1.20000 AFIX 0 C18 1 0.157295 0.184664 0.496620 11.00000 0.03494 0.04898 = 0.02652 0.00747 0.00631 -0.01580 AFIX 43 H18 2 0.079570 0.153598 0.504982 11.00000 -1.20000 AFIX 0 C19 1 0.154203 0.268813 0.451310 11.00000 0.02296 0.04112 = 0.02158 0.00631 0.00144 -0.00513 AFIX 43 H19 2 0.074480 0.295150 0.428886 11.00000 -1.20000 AFIX 0 C21 1 0.584755 0.396508 0.222253 11.00000 0.02163 0.02351 = 0.01610 -0.00199 0.00953 -0.00075 C22 1 0.511100 0.452672 0.171893 11.00000 0.02033 0.03153 = 0.02424 0.00255 0.00547 0.00442 AFIX 43 H22 2 0.422771 0.435559 0.160007 11.00000 -1.20000 AFIX 0 C23 1 0.567874 0.533697 0.139317 11.00000 0.03846 0.02989 = 0.02632 0.00662 0.01273 0.00625 AFIX 43 H23 2 0.518072 0.571587 0.104579 11.00000 -1.20000 AFIX 0 C24 1 0.695745 0.560430 0.156450 11.00000 0.03836 0.02304 = 0.03282 -0.00046 0.01970 -0.00257 AFIX 43 H24 2 0.734371 0.614914 0.133177 11.00000 -1.20000 AFIX 0 C25 1 0.766915 0.506851 0.207949 11.00000 0.02527 0.02902 = 0.03413 -0.00617 0.01209 -0.00698 AFIX 43 H25 2 0.854551 0.526042 0.220521 11.00000 -1.20000 AFIX 0 C26 1 0.712076 0.425516 0.241467 11.00000 0.02475 0.02599 = 0.02549 -0.00479 0.00550 -0.00006 AFIX 43 H26 2 0.761233 0.390059 0.277210 11.00000 -1.20000 AFIX 0 P2 6 0.163276 0.626246 0.154301 11.00000 0.02101 0.02924 = 0.02217 0.00153 0.00464 0.00110 F1 5 0.117418 0.606472 0.081966 11.00000 0.05820 0.04282 = 0.02577 -0.00312 -0.00006 0.00300 F2 5 0.201278 0.494358 0.163590 11.00000 0.04255 0.03222 = 0.04167 0.00952 0.00561 0.00106 F3 5 0.214082 0.650345 0.227364 11.00000 0.08421 0.05813 = 0.02733 -0.00076 -0.00830 0.00376 F4 5 0.128086 0.761057 0.145351 11.00000 0.03653 0.03415 = 0.03768 -0.00328 -0.00125 0.00767 F5 5 0.304183 0.656696 0.142675 11.00000 0.02673 0.04618 = 0.07763 0.00824 0.01557 0.00072 F6 5 0.025385 0.601701 0.167391 11.00000 0.03903 0.06715 = 0.07730 0.00016 0.03416 -0.00699 HKLF 4 REM TZ888_2_0m_a.res in P2(1)/c REM R1 = 0.0382 for 3905 Fo > 4sig(Fo) and 0.0510 for all 4661 data REM 346 parameters refined using 334 restraints END WGHT 0.0441 5.5073 REM Highest difference peak 1.316, deepest hole -0.757, 1-sigma level 0.104 Q1 1 0.3987 0.4644 0.3224 11.00000 0.05 1.32 Q2 1 0.4078 0.2976 0.3252 11.00000 0.05 1.14 Q3 1 0.2645 0.8825 0.4677 11.00000 0.05 0.85 Q4 1 0.2593 0.5049 0.3905 11.00000 0.05 0.58 Q5 1 0.2635 0.3394 0.3829 11.00000 0.05 0.58 Q6 1 0.2630 0.6167 0.1096 11.00000 0.05 0.54 Q7 1 0.1070 0.6966 0.1531 11.00000 0.05 0.54 Q8 1 0.2632 0.3810 0.4325 11.00000 0.05 0.48 Q9 1 0.1416 0.6056 0.2280 11.00000 0.05 0.47 Q10 1 0.2814 0.6241 0.2127 11.00000 0.05 0.44 ; _shelx_res_checksum 20373 _shelx_hkl_file ; -1 0 0 -3.90 0.60 1 0 0 -3.50 0.60 -2 0 0 2958.60 231.88 -2 0 0 2700.63 231.88 2 0 0 2716.83 231.98 2 0 0 2987.40 231.88 3 0 0 1526.85 128.39 3 0 0 1638.94 128.29 -3 0 0 1459.15 128.29 -3 0 0 1631.04 128.29 4 0 0 85.49 9.60 -4 0 0 86.49 8.80 4 0 0 89.89 9.10 -4 0 0 92.39 9.50 -5 0 0 421.66 34.60 5 0 0 420.96 34.40 -5 0 0 398.06 34.80 5 0 0 386.96 34.70 -6 0 0 1525.65 129.19 6 0 0 1596.24 128.99 -6 0 0 1526.25 128.99 6 0 0 1619.74 129.39 -7 0 0 2813.32 228.28 -7 0 0 2654.03 227.98 7 0 0 2732.13 228.28 7 0 0 2916.81 227.98 8 0 0 155.28 16.90 -8 0 0 142.99 17.30 8 0 0 163.58 18.20 -8 0 0 178.78 18.10 9 0 0 80.39 12.50 -9 0 0 97.99 13.30 9 0 0 109.19 12.60 -9 0 0 100.99 13.10 10 0 0 -8.30 7.40 -10 0 0 -6.30 9.10 -10 0 0 -8.60 8.20 10 0 0 -7.20 8.80 -11 0 0 30.90 11.60 11 0 0 21.20 10.00 11 0 0 15.20 12.20 -11 0 0 26.30 11.20 -12 0 0 74.39 14.40 12 0 0 82.19 17.30 12 0 0 119.19 15.80 -12 0 0 92.09 17.70 -13 0 0 140.99 21.80 13 0 0 138.39 20.70 13 0 0 181.98 24.40 -13 0 0 217.08 25.20 -14 0 0 203.18 25.40 14 0 0 98.59 29.00 14 0 0 148.89 23.70 0 -1 0 -1.40 0.40 0 1 0 -0.80 0.50 -2 -1 0 2139.99 165.28 2 -1 0 2000.80 165.28 2 -1 0 2232.78 165.28 -2 -1 0 1925.51 165.28 -2 1 0 1980.60 165.28 2 1 0 2037.90 165.18 2 1 0 1898.31 165.28 -2 1 0 1969.30 165.28 3 -1 0 1884.61 148.39 3 -1 0 1748.33 148.39 -3 -1 0 1842.02 148.49 -3 -1 0 1870.81 148.39 3 1 0 1670.53 148.39 -3 1 0 1921.61 148.39 3 1 0 1798.02 148.29 -3 1 0 1768.82 148.39 4 -1 0 98.19 9.40 4 -1 0 91.59 9.90 -4 -1 0 89.99 9.90 -4 -1 0 86.29 9.20 4 1 0 102.69 9.40 -4 1 0 95.19 9.50 -4 1 0 94.59 9.70 4 1 0 85.89 10.00 5 -1 0 440.76 35.40 -5 -1 0 414.16 35.80 5 -1 0 394.36 35.50 -5 -1 0 444.16 35.50 5 1 0 431.66 35.40 -5 1 0 399.66 35.60 -5 1 0 424.36 35.50 5 1 0 394.06 35.60 -6 -1 0 16.00 5.10 6 -1 0 20.20 5.70 6 -1 0 15.80 4.60 -6 -1 0 8.80 5.00 -6 1 0 16.00 5.10 6 1 0 8.20 5.60 6 1 0 18.10 4.80 -6 1 0 13.80 4.90 7 -1 0 188.98 18.10 -7 -1 0 156.68 17.60 7 -1 0 173.78 18.30 -7 -1 0 197.78 19.00 7 1 0 191.98 18.50 -7 1 0 198.58 18.60 -7 1 0 199.98 21.20 7 1 0 189.18 18.00 -8 -1 0 292.67 28.50 -8 -1 0 303.97 27.90 8 -1 0 286.87 28.00 8 -1 0 325.07 27.30 8 1 0 301.97 28.70 8 1 0 301.37 27.60 -8 1 0 308.47 28.20 -8 1 0 297.07 28.00 -9 -1 0 175.48 21.00 -9 -1 0 206.58 20.80 9 -1 0 170.68 19.90 9 -1 0 210.98 20.80 -9 1 0 193.98 21.00 9 1 0 191.78 20.00 9 1 0 189.18 20.60 -9 1 0 188.48 19.80 -10 -1 0 35.00 9.90 10 -1 0 46.30 11.60 10 -1 0 32.00 8.40 -10 -1 0 32.40 10.60 -10 1 0 42.00 10.20 -10 1 0 44.10 11.00 10 1 0 23.70 8.30 10 1 0 32.70 10.90 -11 -1 0 132.59 17.00 -11 -1 0 116.09 17.50 11 -1 0 146.79 17.50 11 -1 0 132.89 17.70 -11 1 0 108.99 17.10 11 1 0 143.19 16.90 11 1 0 154.38 18.70 12 -1 0 11.30 10.60 -12 -1 0 27.20 14.00 -12 -1 0 13.10 10.70 12 -1 0 15.10 14.10 -12 1 0 24.40 12.40 -12 1 0 16.10 13.90 12 1 0 10.10 13.20 13 -1 0 5.80 12.80 -13 -1 0 16.30 15.80 13 -1 0 34.50 15.60 -13 -1 0 28.40 13.60 13 1 0 11.20 13.40 -13 1 0 27.00 14.60 -13 1 0 15.50 17.40 13 1 0 20.90 17.20 14 -1 0 2.70 15.10 -14 -1 0 45.10 18.90 14 1 0 31.60 19.40 14 1 0 68.89 20.90 -14 1 0 19.50 18.00 0 -2 0 692.73 54.19 0 2 0 627.64 54.19 1 -2 0 445.26 37.00 -1 -2 0 429.36 37.10 -1 2 0 469.35 37.10 -1 2 0 440.66 37.00 1 2 0 448.96 37.00 1 2 0 468.15 37.10 2 -2 0 53.69 5.80 2 -2 0 57.29 5.50 -2 -2 0 51.49 5.50 -2 -2 0 56.09 5.90 2 2 0 51.09 5.50 -2 2 0 53.49 5.80 -2 2 0 64.89 5.80 2 2 0 50.89 5.90 3 -2 0 18.80 3.50 -3 -2 0 17.60 3.40 -3 -2 0 19.30 3.70 3 -2 0 24.10 3.40 3 2 0 26.10 3.90 3 2 0 20.70 3.30 -3 2 0 19.00 3.40 -3 2 0 25.70 3.60 4 -2 0 77.79 8.40 -4 -2 0 76.79 8.90 -4 -2 0 77.89 8.00 4 -2 0 73.99 8.60 -4 2 0 82.89 8.50 4 2 0 69.79 8.40 4 2 0 72.49 8.30 -4 2 0 85.69 8.60 5 -2 0 138.19 13.10 -5 -2 0 123.79 13.10 -5 -2 0 126.69 12.70 5 -2 0 153.68 13.10 -5 2 0 131.39 13.20 5 2 0 127.09 13.70 5 2 0 141.29 12.90 -5 2 0 124.89 12.70 -6 -2 0 28.10 6.10 6 -2 0 22.30 5.10 6 -2 0 32.10 5.80 -6 -2 0 32.70 5.70 -6 2 0 33.00 5.50 6 2 0 30.60 6.60 -6 2 0 27.10 5.60 6 2 0 20.90 5.00 7 -2 0 -2.00 5.80 -7 -2 0 1.30 4.70 -7 -2 0 5.90 6.00 7 -2 0 7.20 4.60 7 2 0 5.30 6.00 -7 2 0 8.70 5.60 -7 2 0 3.40 4.90 7 2 0 0.30 5.00 8 -2 0 -3.70 6.80 -8 -2 0 -3.80 5.30 8 -2 0 2.30 5.70 -8 -2 0 -10.10 6.10 -8 2 0 -4.20 6.30 8 2 0 -10.60 6.90 8 2 0 -8.20 5.80 -8 2 0 -3.50 6.30 9 -2 0 13.00 7.20 9 -2 0 17.30 8.80 -9 -2 0 12.00 7.70 -9 -2 0 17.70 8.30 -9 2 0 6.10 8.40 9 2 0 7.50 8.70 9 2 0 -2.10 7.00 -9 2 0 8.20 7.70 10 -2 0 6.60 7.90 -10 -2 0 6.40 9.20 -10 -2 0 -3.00 8.60 10 -2 0 -12.00 9.20 10 2 0 -9.00 9.30 -10 2 0 18.60 9.80 10 2 0 6.80 7.80 -10 2 0 8.10 8.80 11 -2 0 -19.60 10.50 -11 -2 0 2.60 10.30 -11 -2 0 -18.10 9.20 -11 2 0 -6.00 10.20 -11 2 0 0.50 11.50 11 2 0 0.30 9.40 11 2 0 4.40 10.70 12 -2 0 12.10 13.90 -12 -2 0 20.30 11.30 12 -2 0 -16.20 10.40 -12 -2 0 -7.70 12.90 12 2 0 17.00 13.80 -12 2 0 27.20 13.80 12 2 0 4.70 11.20 -12 2 0 13.80 12.70 -13 -2 0 17.30 17.20 13 -2 0 33.40 16.60 13 -2 0 49.30 13.70 -13 -2 0 30.60 16.30 13 2 0 43.40 19.00 -13 2 0 57.09 15.40 13 2 0 24.80 14.50 -13 2 0 91.99 22.20 14 -2 0 4.60 15.90 -14 -2 0 16.30 18.00 14 2 0 24.60 17.00 14 2 0 20.90 19.70 -14 2 0 -6.20 18.00 0 -3 0 -2.10 1.60 0 3 0 -0.90 1.60 0 3 0 -0.20 1.60 1 -3 0 9.30 2.20 1 -3 0 9.50 2.00 -1 -3 0 4.90 2.00 -1 -3 0 10.10 2.20 -1 3 0 8.20 2.00 1 3 0 10.70 2.40 -1 3 0 9.70 2.20 1 3 0 11.40 2.10 -2 -3 0 1079.89 95.89 2 -3 0 1270.97 95.89 2 -3 0 1194.28 95.99 -2 3 0 1228.68 95.99 -2 3 0 1130.49 95.89 2 3 0 1138.29 95.99 2 3 0 1148.59 95.79 -3 -3 0 121.19 11.30 3 -3 0 128.79 11.60 -3 -3 0 104.99 11.50 3 -3 0 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163.88 14.70 -2 6 0 156.58 14.30 2 6 0 154.48 14.80 3 -6 0 38.70 5.50 -3 -6 0 43.30 5.60 3 -6 0 47.30 6.30 -3 -6 0 33.00 5.40 -3 6 0 41.30 5.60 3 6 0 48.80 5.60 -3 6 0 63.09 7.20 3 6 0 51.49 6.30 -4 -6 0 30.60 5.20 4 -6 0 31.10 5.00 4 -6 0 21.00 5.30 -4 -6 0 26.70 5.10 -4 6 0 27.40 5.00 -4 6 0 21.10 5.10 4 6 0 34.20 5.80 4 6 0 26.20 4.70 5 -6 0 59.49 7.90 -5 -6 0 49.20 7.30 5 -6 0 51.59 6.80 -5 -6 0 51.79 7.30 -5 6 0 61.99 7.20 -5 6 0 39.30 6.60 5 6 0 44.90 7.40 5 6 0 42.70 6.70 -6 -6 0 231.18 19.90 6 -6 0 195.88 19.20 6 -6 0 181.28 18.70 -6 -6 0 189.18 19.30 -6 6 0 178.28 19.20 6 6 0 215.38 20.20 -6 6 0 196.78 18.90 6 6 0 216.48 19.10 -7 -6 0 217.18 23.00 7 -6 0 220.28 23.20 7 -6 0 227.78 22.00 -7 -6 0 234.18 22.50 7 6 0 256.27 22.90 -7 6 0 243.38 22.50 7 6 0 257.27 22.30 -7 6 0 202.78 21.80 8 -6 0 2.00 7.70 8 -6 0 -1.40 6.10 -8 -6 0 0.20 7.20 -8 -6 0 4.70 7.80 8 6 0 20.30 8.70 -8 6 0 3.90 7.30 -8 6 0 -6.40 8.50 8 6 0 7.90 7.00 -9 -6 0 -7.60 9.20 -9 -6 0 -5.30 7.80 9 -6 0 -0.90 9.40 9 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17.20 10 -7 0 102.39 14.20 -10 -7 0 100.09 15.60 -10 -7 0 114.49 16.30 -10 7 0 78.59 15.30 10 7 0 79.49 14.50 10 7 0 102.89 15.60 -10 7 0 98.69 14.50 -11 -7 0 10.30 11.90 11 -7 0 -13.80 14.00 11 -7 0 17.40 11.30 -11 -7 0 7.60 13.40 11 7 0 -7.10 13.80 11 7 0 18.40 12.60 -11 7 0 32.70 12.50 12 -7 0 9.80 12.20 -12 -7 0 11.50 16.30 12 7 0 3.30 16.20 -12 7 0 -0.70 13.60 12 7 0 -4.00 18.20 0 -8 0 488.55 41.40 0 -8 0 538.05 41.50 0 8 0 444.06 41.10 0 8 0 494.75 41.50 -1 -8 0 49.80 6.50 1 -8 0 50.29 6.50 -1 -8 0 56.29 6.80 1 8 0 41.80 6.50 -1 8 0 50.39 6.50 -1 8 0 52.09 6.30 1 8 0 48.70 6.20 2 -8 0 181.18 17.50 -2 -8 0 160.38 17.30 -2 -8 0 187.98 17.60 2 -8 0 209.28 17.80 2 8 0 202.48 17.70 2 8 0 189.98 17.90 -2 8 0 236.28 18.30 -2 8 0 184.58 17.50 3 -8 0 81.29 10.30 -3 -8 0 75.29 10.00 3 -8 0 91.19 9.60 -3 -8 0 63.99 9.20 3 8 0 78.69 10.10 3 8 0 78.29 9.60 -3 8 0 73.79 9.70 -3 8 0 96.79 10.30 4 -8 0 589.04 49.80 -4 -8 0 627.74 50.19 -4 -8 0 620.14 49.90 4 -8 0 534.75 49.99 -4 8 0 536.95 49.90 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