data_scaled_a _publ_contact_author_name 'Hosea Nelson' _publ_contact_author_address ;Department of Chemistry and Biochemistry University of California, Los Angeles ; _publ_contact_author_email hosea@chem.ucla.edu loop_ _publ_author_name _publ_author_address 'Nelson, Hosea M.' ;Department of Chemistry and Biochemistry University of California, Los Angeles ; 'Asay, Matthew' ;Department of Chemistry and Biochemistry University of California, Los Angeles ; 'Jones, Chris' ;Department of Chemistry and Biochemistry University of California, Los Angeles ; 'Kim, Lee Joon' ;Department of Chemistry and Biochemistry University of California, Los Angeles ; 'Saha, Ambarneil' ;Department of Chemistry and Biochemistry University of California, Los Angeles ; 'Rodriguez, Jose' ;Department of Chemistry and Biochemistry University of California, Los Angeles ; 'Cascio, Duilio' ;Department of Chemistry and Biochemistry University of California, Los Angeles ; 'Fulton, Tyler' ;Department of Chemistry California Institute of Technology ; 'Stoltz, Brian' ;Department of Chemistry California Institute of Technology ; 'Jack F. Kleinsasser' ;Department of Chemistry University of California, Riverside ; 'Kevin R. Berkly' ;Department of Chemistry University of California, Riverside ; 'Matthew P. Conley' ;Department of Chemistry University of California, Riverside ; 'Vincent Lavallo' ;Department of Chemistry University of California, Riverside ; _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common PdPHOX _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C168 H160 N4 O8 P4 Pd4' _chemical_formula_weight 2912.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0000 0.0000 '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' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.0000 0.0000 '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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.200(2) _cell_length_b 17.040(3) _cell_length_c 19.900(4) _cell_angle_alpha 90.00(3) _cell_angle_beta 90.00(3) _cell_angle_gamma 90.00(3) _cell_volume 3458.8(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3596 _cell_measurement_theta_min 0.079 _cell_measurement_theta_max 0.564 _exptl_crystal_description 'nano crystals' _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_F_000 583 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.001 _exptl_crystal_size_mid 0.0007 _exptl_crystal_size_min 0.0005 _exptl_absorpt_coefficient_mu 0.000 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.0 _exptl_absorpt_correction_T_max 0.0 _exptl_absorpt_process_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.01969 _diffrn_radiation_type '300 KeV electrons' _diffrn_source 'electron microscope FEG' _diffrn_measurement_device_type 'Technai F-30' _diffrn_measurement_method 'continuous rotation' _diffrn_detector_area_resol_mean 32 _diffrn_reflns_number 12338 _diffrn_reflns_av_unetI/netI 0.2641 _diffrn_reflns_av_R_equivalents 0.2282 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 0.079 _diffrn_reflns_theta_max 0.564 _diffrn_reflns_theta_full 0.564 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 0.994 _reflns_number_total 3596 _reflns_number_gt 2459 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.744 _reflns_Friedel_fraction_max 0.997 _reflns_Friedel_fraction_full 0.997 _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 TVIPS _computing_cell_refinement 'XSCALE XDS' _computing_data_reduction XDSCONV _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics ShelxLe _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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Direct _atom_sites_solution_secondary Difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_extinction_coef 584(41) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details ; All f" are zero, so absolute structure could not be determined ; _refine_ls_abs_structure_Flack 0 _chemical_absolute_configuration syn _refine_ls_number_reflns 3596 _refine_ls_number_parameters 428 _refine_ls_number_restraints 429 _refine_ls_R_factor_all 0.1764 _refine_ls_R_factor_gt 0.1432 _refine_ls_wR_factor_ref 0.3504 _refine_ls_wR_factor_gt 0.3168 _refine_ls_goodness_of_fit_ref 1.301 _refine_ls_restrained_S_all 1.249 _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 Pd1 Pd 0.5843(4) 0.3887(2) 0.60337(19) 0.0437(12) Uani 1 1 d . . . . . P1 P 0.5272(9) 0.5122(5) 0.6321(5) 0.039(2) Uani 1 1 d . . . . . O1 O 0.8158(18) 0.5206(15) 0.4666(12) 0.086(6) Uani 1 1 d . . . . . N1 N 0.6676(18) 0.4490(12) 0.5175(9) 0.058(4) Uani 1 1 d . . . . . O2 O 0.4114(16) 0.2264(12) 0.5690(10) 0.071(5) Uani 1 1 d . . . . . C1 C 0.4146(15) 0.5592(9) 0.5765(9) 0.044(4) Uani 1 1 d D . . . . C2 C 0.4383(19) 0.6266(10) 0.5474(10) 0.060(5) Uani 1 1 d D . . . . H2 H 0.516809 0.652521 0.555955 0.072 Uiso 1 1 calc R U . . . C4 C 0.347(2) 0.6597(17) 0.5039(13) 0.106(9) Uani 1 1 d D . . . . H4 H 0.364863 0.708398 0.484768 0.127 Uiso 1 1 calc R U . . . C3 C 0.236(2) 0.6235(15) 0.4890(15) 0.100(8) Uani 1 1 d D . . . . H3 H 0.176039 0.646741 0.460163 0.120 Uiso 1 1 calc R U . . . C5 C 0.212(2) 0.5538(17) 0.5156(13) 0.090(7) Uani 1 1 d D . . . . H5 H 0.137353 0.525090 0.504796 0.108 Uiso 1 1 calc R U . . . C6 C 0.3036(16) 0.5270(14) 0.5602(11) 0.069(6) Uani 1 1 d D . . . . H6 H 0.284056 0.479827 0.581421 0.082 Uiso 1 1 calc R U . . . C7 C 0.4578(18) 0.5336(10) 0.7161(9) 0.052(5) Uani 1 1 d D . . . . C8 C 0.3743(18) 0.5931(11) 0.7299(9) 0.057(5) Uani 1 1 d D . . . . H8 H 0.347520 0.626476 0.695566 0.068 Uiso 1 1 calc R U . . . C9 C 0.329(2) 0.6047(13) 0.7930(10) 0.073(6) Uani 1 1 d D . . . . H9 H 0.272547 0.646024 0.802056 0.087 Uiso 1 1 calc R U . . . C10 C 0.368(2) 0.5551(12) 0.8436(11) 0.073(6) Uani 1 1 d D . . . . H10 H 0.336999 0.562546 0.887124 0.088 Uiso 1 1 calc R U . . . C11 C 0.4508(18) 0.4957(10) 0.8301(9) 0.052(5) Uani 1 1 d D . . . . H11 H 0.473474 0.460082 0.863481 0.063 Uiso 1 1 calc R U . . . C12 C 0.4998(19) 0.4884(10) 0.7689(8) 0.049(4) Uani 1 1 d D . . . . H12 H 0.565053 0.451348 0.761394 0.059 Uiso 1 1 calc R U . . . C13 C 0.6711(18) 0.5667(11) 0.6276(8) 0.056(4) Uani 1 1 d D . . . . C14 C 0.706(2) 0.6226(12) 0.6750(12) 0.074(6) Uani 1 1 d D . . . . H14 H 0.653658 0.627461 0.713050 0.089 Uiso 1 1 calc R U . . . C15 C 0.812(3) 0.6707(16) 0.6695(15) 0.106(8) Uani 1 1 d D . . . . H15 H 0.826390 0.708702 0.702160 0.127 Uiso 1 1 calc R U . . . C16 C 0.896(2) 0.6640(19) 0.6169(13) 0.125(11) Uani 1 1 d D . . . . H16 H 0.969241 0.696321 0.612859 0.150 Uiso 1 1 calc R U . . . C17 C 0.868(2) 0.6071(15) 0.5701(15) 0.097(7) Uani 1 1 d D . . . . H17 H 0.926365 0.599779 0.534610 0.116 Uiso 1 1 calc R U . . . C18 C 0.7581(18) 0.5604(13) 0.5736(11) 0.066(5) Uani 1 1 d D . . . . C19 C 0.743(2) 0.5062(15) 0.5175(11) 0.067(5) Uani 1 1 d . . . . . C20 C 0.793(2) 0.4564(16) 0.4215(12) 0.082(6) Uani 1 1 d . . . . . H20A H 0.869579 0.422791 0.419250 0.099 Uiso 1 1 calc R U . . . H20B H 0.773781 0.475672 0.376741 0.099 Uiso 1 1 calc R U . . . C21 C 0.6752(17) 0.4107(13) 0.4496(8) 0.059(4) Uani 1 1 d . . . . . H21 H 0.700284 0.355603 0.455375 0.071 Uiso 1 1 calc R U . . . C22 C 0.550(2) 0.4145(15) 0.4082(9) 0.070(5) Uani 1 1 d . . . . . C23 C 0.573(3) 0.370(2) 0.3420(11) 0.142(13) Uani 1 1 d . . . . . H23A H 0.491563 0.363780 0.318803 0.212 Uiso 1 1 calc R U . . . H23B H 0.610765 0.319906 0.351383 0.212 Uiso 1 1 calc R U . . . H23C H 0.632544 0.400043 0.314334 0.212 Uiso 1 1 calc R U . . . C24 C 0.4379(17) 0.3780(13) 0.4460(11) 0.069(5) Uani 1 1 d . . . . . H24A H 0.356405 0.396108 0.427512 0.104 Uiso 1 1 calc R U . . . H24B H 0.443105 0.392754 0.492495 0.104 Uiso 1 1 calc R U . . . H24C H 0.442748 0.321954 0.442191 0.104 Uiso 1 1 calc R U . . . C25 C 0.516(3) 0.5061(15) 0.3979(14) 0.100(7) Uani 1 1 d . . . . . H25A H 0.439376 0.511027 0.369864 0.150 Uiso 1 1 calc R U . . . H25B H 0.588408 0.531995 0.376818 0.150 Uiso 1 1 calc R U . . . H25C H 0.498650 0.529844 0.440739 0.150 Uiso 1 1 calc R U . . . C26 C 0.6837(15) 0.1529(14) 0.3602(8) 0.062(5) Uani 1 1 d D . . . . H26 H 0.737802 0.188947 0.381684 0.075 Uiso 1 1 calc R U . . . C27 C 0.7203(17) 0.1242(12) 0.3004(10) 0.066(6) Uani 1 1 d D . . . . H27 H 0.799566 0.139488 0.281349 0.079 Uiso 1 1 calc R U . . . C28 C 0.6421(19) 0.0734(14) 0.2683(12) 0.084(7) Uani 1 1 d D . . . . H28 H 0.663627 0.054746 0.225783 0.100 Uiso 1 1 calc R U . . . C29 C 0.530(2) 0.0500(18) 0.2998(11) 0.101(10) Uani 1 1 d D . . . . H29 H 0.477817 0.012351 0.278980 0.121 Uiso 1 1 calc R U . . . C30 C 0.491(2) 0.0793(13) 0.3606(10) 0.071(6) Uani 1 1 d D . . . . H30 H 0.412364 0.063874 0.380555 0.085 Uiso 1 1 calc R U . . . C31 C 0.5709(15) 0.1313(11) 0.3901(9) 0.053(5) Uani 1 1 d D . . . . C32 C 0.5250(18) 0.1644(12) 0.4550(9) 0.055(5) Uani 1 1 d . . . . . H32 H 0.435910 0.159783 0.464208 0.067 Uiso 1 1 calc R U . . . C33 C 0.594(2) 0.1983(11) 0.4993(9) 0.051(5) Uani 1 1 d . . . . . H33 H 0.683551 0.204776 0.492106 0.062 Uiso 1 1 calc R U . . . C34 C 0.5325(17) 0.2285(12) 0.5642(9) 0.050(4) Uani 1 1 d . . . . . C35 C 0.6098(17) 0.2724(11) 0.6075(9) 0.049(4) Uani 1 1 d . . . . . H35 H 0.695034 0.285740 0.595546 0.059 Uiso 1 1 calc R U . . . C36 C 0.5580(18) 0.2966(11) 0.6697(9) 0.052(4) Uani 1 1 d . . . . . H36 H 0.469972 0.310679 0.671010 0.062 Uiso 1 1 calc R U . . . C37 C 0.6346(19) 0.3013(13) 0.7344(9) 0.065(5) Uani 1 1 d D . . . . C38 C 0.565(2) 0.2977(11) 0.7919(9) 0.067(5) Uani 1 1 d D . . . . H38 H 0.474715 0.292071 0.791394 0.081 Uiso 1 1 calc R U . . . C39 C 0.634(3) 0.3026(14) 0.8522(11) 0.093(7) Uani 1 1 d D . . . . H39 H 0.587347 0.301625 0.892357 0.111 Uiso 1 1 calc R U . . . C40 C 0.765(3) 0.3086(16) 0.8543(12) 0.102(8) Uani 1 1 d D . . . . H40 H 0.809110 0.306954 0.895255 0.122 Uiso 1 1 calc R U . . . C41 C 0.834(3) 0.3173(19) 0.7958(13) 0.115(9) Uani 1 1 d D . . . . H41 H 0.923123 0.328110 0.796424 0.138 Uiso 1 1 calc R U . . . C42 C 0.766(2) 0.309(2) 0.7351(11) 0.107(10) Uani 1 1 d D . . . . H42 H 0.812571 0.309690 0.694765 0.129 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 Pd1 0.050(2) 0.046(2) 0.035(2) 0.001(2) 0.0045(18) 0.0016(19) P1 0.050(5) 0.036(5) 0.032(5) 0.005(4) -0.006(4) 0.012(4) O1 0.066(10) 0.114(15) 0.078(12) 0.017(10) 0.030(10) 0.003(10) N1 0.063(10) 0.077(11) 0.033(7) 0.011(7) 0.005(7) 0.010(8) O2 0.051(6) 0.091(13) 0.071(12) -0.026(12) 0.014(8) -0.002(9) C1 0.045(7) 0.034(9) 0.052(10) 0.009(8) -0.003(8) 0.005(7) C2 0.083(11) 0.028(9) 0.069(13) 0.008(9) -0.003(10) -0.002(8) C4 0.109(15) 0.12(2) 0.087(17) 0.064(17) -0.019(14) -0.015(14) C3 0.080(13) 0.122(19) 0.10(2) 0.026(16) -0.016(13) 0.019(13) C5 0.059(11) 0.115(17) 0.095(18) 0.012(16) -0.023(11) 0.005(12) C6 0.046(8) 0.087(14) 0.072(14) 0.012(13) -0.006(9) -0.011(9) C7 0.073(12) 0.050(11) 0.034(8) -0.006(8) 0.003(8) 0.013(8) C8 0.080(13) 0.046(11) 0.045(9) 0.003(9) 0.020(9) 0.015(8) C9 0.103(15) 0.051(12) 0.063(10) -0.004(10) 0.039(11) 0.012(11) C10 0.092(14) 0.082(14) 0.045(11) -0.007(10) 0.019(11) 0.008(10) C11 0.083(13) 0.034(10) 0.040(8) 0.001(9) -0.002(9) -0.013(8) C12 0.078(12) 0.025(9) 0.046(8) 0.005(8) 0.001(8) -0.001(8) C13 0.061(9) 0.054(10) 0.053(10) 0.008(9) -0.010(7) -0.006(8) C14 0.084(12) 0.057(13) 0.081(14) -0.015(11) 0.016(11) -0.018(10) C15 0.118(17) 0.094(17) 0.105(18) 0.016(15) -0.011(13) -0.054(14) C16 0.076(15) 0.17(3) 0.13(2) 0.013(18) -0.010(13) -0.076(17) C17 0.062(11) 0.109(18) 0.118(19) 0.027(14) -0.001(12) -0.027(11) C18 0.052(9) 0.075(13) 0.071(11) 0.007(10) 0.008(8) -0.015(9) C19 0.055(11) 0.091(13) 0.056(11) 0.013(8) 0.010(9) 0.003(9) C20 0.082(12) 0.100(15) 0.065(13) 0.034(10) 0.037(11) 0.004(12) C21 0.059(8) 0.085(13) 0.034(8) 0.014(8) 0.025(7) 0.013(8) C22 0.092(10) 0.099(13) 0.019(8) -0.011(10) 0.004(7) 0.006(10) C23 0.15(2) 0.23(3) 0.043(12) -0.060(18) -0.001(13) 0.06(3) C24 0.070(10) 0.078(14) 0.060(12) 0.002(12) -0.011(9) 0.014(10) C25 0.109(17) 0.113(14) 0.077(17) 0.026(15) -0.011(16) 0.017(14) C26 0.032(7) 0.107(16) 0.049(10) -0.013(10) -0.004(7) 0.006(9) C27 0.042(9) 0.091(16) 0.064(11) -0.013(12) 0.017(8) -0.005(9) C28 0.064(11) 0.113(19) 0.074(14) -0.030(13) 0.014(9) -0.013(12) C29 0.071(12) 0.15(2) 0.079(14) -0.059(15) 0.017(11) -0.044(14) C30 0.074(11) 0.083(14) 0.056(11) -0.019(10) 0.007(9) -0.024(11) C31 0.050(8) 0.062(12) 0.046(9) -0.012(8) 0.003(7) 0.002(8) C32 0.046(9) 0.070(13) 0.050(9) -0.020(9) 0.012(8) -0.011(9) C33 0.053(9) 0.060(12) 0.042(9) -0.011(9) -0.003(7) 0.011(9) C34 0.050(7) 0.069(11) 0.030(8) -0.002(8) 0.006(7) -0.007(8) C35 0.051(9) 0.063(9) 0.033(8) 0.001(8) 0.009(7) -0.014(8) C36 0.055(10) 0.063(10) 0.037(7) 0.004(8) 0.010(7) -0.020(9) C37 0.100(10) 0.058(13) 0.036(7) -0.004(10) -0.007(7) -0.010(11) C38 0.117(14) 0.045(11) 0.039(8) 0.000(10) 0.006(8) 0.011(12) C39 0.176(18) 0.062(15) 0.040(10) 0.014(13) -0.013(12) 0.005(18) C40 0.176(18) 0.073(16) 0.057(11) 0.009(15) -0.050(14) 0.005(19) C41 0.128(17) 0.13(2) 0.084(13) 0.028(19) -0.048(12) -0.02(2) C42 0.090(11) 0.17(3) 0.056(11) 0.023(19) -0.014(10) -0.010(16) _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 Pd1 C35 2.000(18) . ? Pd1 C36 2.068(17) . ? Pd1 N1 2.167(19) . ? Pd1 P1 2.258(10) . ? P1 C13 1.74(2) . ? P1 C1 1.78(2) . ? P1 C7 1.85(2) . ? O1 C19 1.28(3) . ? O1 C20 1.43(3) . ? N1 C19 1.24(3) . ? N1 C21 1.50(3) . ? O2 C34 1.24(2) . ? C1 C6 1.30(2) . ? C1 C2 1.308(19) . ? C2 C4 1.39(2) . ? C4 C3 1.32(3) . ? C3 C5 1.32(3) . ? C5 C6 1.37(2) . ? C7 C8 1.35(2) . ? C7 C12 1.37(2) . ? C8 C9 1.35(2) . ? C9 C10 1.37(2) . ? C10 C11 1.35(2) . ? C11 C12 1.32(2) . ? C13 C14 1.39(2) . ? C13 C18 1.40(2) . ? C14 C15 1.36(2) . ? C15 C16 1.36(3) . ? C16 C17 1.37(3) . ? C17 C18 1.38(2) . ? C18 C19 1.46(3) . ? C20 C21 1.54(3) . ? C21 C22 1.52(3) . ? C22 C24 1.50(3) . ? C22 C23 1.54(3) . ? C22 C25 1.61(3) . ? C26 C27 1.34(2) . ? C26 C31 1.35(2) . ? C27 C28 1.34(2) . ? C28 C29 1.36(2) . ? C29 C30 1.37(2) . ? C30 C31 1.34(2) . ? C31 C32 1.49(2) . ? C32 C33 1.27(2) . ? C33 C34 1.53(3) . ? C34 C35 1.39(2) . ? C35 C36 1.41(2) . ? C36 C37 1.51(3) . ? C37 C38 1.35(2) . ? C37 C42 1.35(2) . ? C38 C39 1.39(3) . ? C39 C40 1.34(3) . ? C40 C41 1.37(3) . ? C41 C42 1.40(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 C35 Pd1 C36 40.4(7) . . ? C35 Pd1 N1 116.8(8) . . ? C36 Pd1 N1 156.0(8) . . ? C35 Pd1 P1 161.2(6) . . ? C36 Pd1 P1 120.8(6) . . ? N1 Pd1 P1 81.9(6) . . ? C13 P1 C1 105.7(9) . . ? C13 P1 C7 105.3(9) . . ? C1 P1 C7 103.0(9) . . ? C13 P1 Pd1 105.5(7) . . ? C1 P1 Pd1 115.3(7) . . ? C7 P1 Pd1 120.8(7) . . ? C19 O1 C20 105(2) . . ? C19 N1 C21 108.0(18) . . ? C19 N1 Pd1 128.0(17) . . ? C21 N1 Pd1 121.6(15) . . ? C6 C1 C2 114.9(19) . . ? C6 C1 P1 121.7(14) . . ? C2 C1 P1 123.3(14) . . ? C1 C2 C4 120.6(19) . . ? C3 C4 C2 121(2) . . ? C5 C3 C4 119(3) . . ? C3 C5 C6 116(2) . . ? C1 C6 C5 128(2) . . ? C8 C7 C12 117.5(17) . . ? C8 C7 P1 124.9(13) . . ? C12 C7 P1 117.5(12) . . ? C9 C8 C7 120.8(18) . . ? C8 C9 C10 119.7(18) . . ? C11 C10 C9 120(2) . . ? C12 C11 C10 119.5(18) . . ? C11 C12 C7 122.3(17) . . ? C14 C13 C18 114.4(18) . . ? C14 C13 P1 123.3(14) . . ? C18 C13 P1 122.3(14) . . ? C15 C14 C13 124(2) . . ? C14 C15 C16 121(2) . . ? C15 C16 C17 117(2) . . ? C16 C17 C18 123(2) . . ? C17 C18 C13 121(2) . . ? C17 C18 C19 115(2) . . ? C13 C18 C19 124.7(17) . . ? N1 C19 O1 121(2) . . ? N1 C19 C18 124.3(19) . . ? O1 C19 C18 115(2) . . ? O1 C20 C21 106.7(18) . . ? N1 C21 C22 115.2(15) . . ? N1 C21 C20 98.5(18) . . ? C22 C21 C20 116.0(17) . . ? C24 C22 C21 110.5(15) . . ? C24 C22 C23 110(2) . . ? C21 C22 C23 108.2(19) . . ? C24 C22 C25 107.5(19) . . ? C21 C22 C25 107(2) . . ? C23 C22 C25 113(2) . . ? C27 C26 C31 122(2) . . ? C26 C27 C28 119.6(18) . . ? C27 C28 C29 118(2) . . ? C28 C29 C30 123(2) . . ? C31 C30 C29 116.7(19) . . ? C30 C31 C26 120.6(17) . . ? C30 C31 C32 116.0(16) . . ? C26 C31 C32 123.4(17) . . ? C33 C32 C31 127.0(16) . . ? C32 C33 C34 120.8(17) . . ? O2 C34 C35 122.3(19) . . ? O2 C34 C33 117.8(18) . . ? C35 C34 C33 118.3(15) . . ? C34 C35 C36 119.4(15) . . ? C34 C35 Pd1 115.8(13) . . ? C36 C35 Pd1 72.4(10) . . ? C35 C36 C37 124.9(16) . . ? C35 C36 Pd1 67.2(10) . . ? C37 C36 Pd1 115.9(12) . . ? C38 C37 C42 121(2) . . ? C38 C37 C36 116.9(17) . . ? C42 C37 C36 122.0(17) . . ? C37 C38 C39 118(2) . . ? C40 C39 C38 122(2) . . ? C39 C40 C41 119(3) . . ? C40 C41 C42 118(2) . . ? C37 C42 C41 121(2) . . ? _refine_diff_density_max 0.279 _refine_diff_density_min -0.176 _refine_diff_density_rms 0.049 _shelx_res_file ; TITL scaled_a.res in P2(1)2(1)2(1) scaled_a.res created by SHELXL-2018/3 at 18:24:19 on 28-May-2019 REM Old TITL PdPHOX SG16 REM SHELXT solution in P2(1)2(1)2(1): R1 0.317, Rweak 0.141, Alpha 0.009 REM 0.401 for 21 systematic absences, Orientation as input REM Flack x = -0.050 ( 0.070 ) from 720 Parsons' quotients REM Formula found by SHELXT: C41 O N3 P2 CELL 0.019687 10.2000 17.0400 19.9000 90.000 90.000 90.000 ZERR 1.000 0.0020 0.0030 0.0040 0.030 0.030 0.030 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C 0.1361 0.3731 0.5482 3.2814 1.2266 13.0456 = 0.5971 41.0202 0 0 0 0 0.68 12.011 SFAC H 0.0367 0.5608 0.1269 3.7913 0.236 13.5557 = 0.129 37.7229 0 0 0 0 0.23 1.008 SFAC O 0.1433 0.3055 0.5103 2.2683 0.937 8.2625 = 0.3923 25.6645 0 0 0 0 0.68 15.999 SFAC N 0.1372 0.3287 0.5344 2.6733 1.0862 10.3165 = 0.4547 32.7631 0 0 0 0 0.68 14.007 SFAC P 0.354 0.3941 0.9397 3.181 2.6203 15.6579 = 1.5707 49.5239 0 0 0 0 1.05 30.974 SFAC Pd 0.7832 0.3094 2.1753 2.5857 3.2003 = 9.8481 1.4127 37.4035 0 0 0 0 1.39 106.42 UNIT 168 160 8 4 4 4 ACTA L.S. 50 BOND LIST 4 FMAP 2 PLAN 20 RIGU FREE PD1 H35 FREE PD1 H36 FLAT C34 H35 C35 H36 C36 WGHT 0.100000 EXTI 595.182800 FVAR 1.33293 PD1 6 0.584261 0.388662 0.603370 11.00000 0.05040 0.04584 = 0.03491 0.00088 0.00454 0.00165 P1 5 0.527156 0.512178 0.632134 11.00000 0.05047 0.03591 = 0.03202 0.00482 -0.00647 0.01153 O1 3 0.815767 0.520552 0.466551 11.00000 0.06642 0.11362 = 0.07773 0.01698 0.02989 0.00284 N1 4 0.667620 0.448968 0.517540 11.00000 0.06295 0.07690 = 0.03345 0.01079 0.00469 0.00951 O2 3 0.411355 0.226377 0.569010 11.00000 0.05064 0.09109 = 0.07072 -0.02575 0.01434 -0.00182 REM PHENYL SAME C1 > C6 SAME C1 C6 < C2 C1 1 0.414632 0.559202 0.576517 11.00000 0.04473 0.03449 = 0.05158 0.00873 -0.00253 0.00507 C2 1 0.438344 0.626572 0.547422 11.00000 0.08265 0.02764 = 0.06875 0.00803 -0.00335 -0.00185 AFIX 43 H2 2 0.516809 0.652521 0.555955 11.00000 -1.20000 AFIX 0 C4 1 0.347347 0.659710 0.503881 11.00000 0.10893 0.12104 = 0.08727 0.06356 -0.01878 -0.01528 AFIX 43 H4 2 0.364863 0.708398 0.484768 11.00000 -1.20000 AFIX 0 C3 1 0.236312 0.623485 0.489026 11.00000 0.08021 0.12192 = 0.09706 0.02618 -0.01619 0.01861 AFIX 43 H3 2 0.176039 0.646741 0.460163 11.00000 -1.20000 AFIX 0 C5 1 0.211896 0.553850 0.515648 11.00000 0.05949 0.11498 = 0.09460 0.01195 -0.02346 0.00532 AFIX 43 H5 2 0.137353 0.525090 0.504796 11.00000 -1.20000 AFIX 0 C6 1 0.303573 0.527011 0.560170 11.00000 0.04631 0.08717 = 0.07216 0.01250 -0.00625 -0.01127 AFIX 43 H6 2 0.284056 0.479827 0.581421 11.00000 -1.20000 AFIX 0 REM PHENYL SAME C7 > C12 SAME C7 C12 < C8 C7 1 0.457764 0.533646 0.716076 11.00000 0.07274 0.04955 = 0.03423 -0.00583 0.00287 0.01257 C8 1 0.374321 0.593111 0.729904 11.00000 0.08038 0.04576 = 0.04492 0.00270 0.01957 0.01538 AFIX 43 H8 2 0.347520 0.626476 0.695566 11.00000 -1.20000 AFIX 0 C9 1 0.329372 0.604678 0.792988 11.00000 0.10342 0.05126 = 0.06309 -0.00395 0.03927 0.01169 AFIX 43 H9 2 0.272547 0.646024 0.802056 11.00000 -1.20000 AFIX 0 C10 1 0.367963 0.555124 0.843629 11.00000 0.09223 0.08209 = 0.04483 -0.00707 0.01933 0.00823 AFIX 43 H10 2 0.336999 0.562546 0.887124 11.00000 -1.20000 AFIX 0 C11 1 0.450833 0.495734 0.830053 11.00000 0.08344 0.03419 = 0.03967 0.00055 -0.00190 -0.01261 AFIX 43 H11 2 0.473474 0.460082 0.863481 11.00000 -1.20000 AFIX 0 C12 1 0.499792 0.488440 0.768896 11.00000 0.07787 0.02488 = 0.04562 0.00484 0.00123 -0.00057 AFIX 43 H12 2 0.565053 0.451348 0.761394 11.00000 -1.20000 AFIX 0 REM PHENYL SAME C13 > C18 SAME C13 C18 < C14 C13 1 0.671100 0.566706 0.627647 11.00000 0.06091 0.05350 = 0.05273 0.00812 -0.00982 -0.00580 C14 1 0.706010 0.622585 0.675016 11.00000 0.08412 0.05677 = 0.08080 -0.01460 0.01556 -0.01832 AFIX 43 H14 2 0.653658 0.627461 0.713050 11.00000 -1.20000 AFIX 0 C15 1 0.811626 0.670659 0.669516 11.00000 0.11786 0.09448 = 0.10463 0.01619 -0.01124 -0.05397 AFIX 43 H15 2 0.826390 0.708702 0.702160 11.00000 -1.20000 AFIX 0 C16 1 0.896223 0.663980 0.616913 11.00000 0.07640 0.16916 = 0.12986 0.01323 -0.00989 -0.07601 AFIX 43 H16 2 0.969241 0.696321 0.612859 11.00000 -1.20000 AFIX 0 C17 1 0.868393 0.607118 0.570129 11.00000 0.06214 0.10918 = 0.11832 0.02677 -0.00089 -0.02748 AFIX 43 H17 2 0.926365 0.599779 0.534610 11.00000 -1.20000 AFIX 0 C18 1 0.758099 0.560415 0.573575 11.00000 0.05165 0.07520 = 0.07132 0.00651 0.00787 -0.01484 C19 1 0.742711 0.506218 0.517471 11.00000 0.05508 0.09141 = 0.05559 0.01317 0.00969 0.00314 C20 1 0.792919 0.456371 0.421536 11.00000 0.08236 0.09971 = 0.06457 0.03357 0.03655 0.00408 AFIX 23 H20A 2 0.869579 0.422791 0.419250 11.00000 -1.20000 H20B 2 0.773781 0.475672 0.376741 11.00000 -1.20000 AFIX 0 C21 1 0.675165 0.410703 0.449600 11.00000 0.05860 0.08454 = 0.03374 0.01373 0.02492 0.01322 AFIX 13 H21 2 0.700284 0.355603 0.455375 11.00000 -1.20000 AFIX 0 C22 1 0.549730 0.414479 0.408193 11.00000 0.09233 0.09923 = 0.01941 -0.01083 0.00375 0.00618 C23 1 0.573365 0.370423 0.341973 11.00000 0.15438 0.22762 = 0.04287 -0.05979 -0.00103 0.05567 AFIX 137 H23A 2 0.491563 0.363780 0.318803 11.00000 -1.50000 H23B 2 0.610765 0.319906 0.351383 11.00000 -1.50000 H23C 2 0.632544 0.400043 0.314334 11.00000 -1.50000 AFIX 0 C24 1 0.437926 0.378041 0.446004 11.00000 0.06963 0.07753 = 0.05988 0.00169 -0.01120 0.01405 AFIX 137 H24A 2 0.356405 0.396108 0.427512 11.00000 -1.50000 H24B 2 0.443105 0.392754 0.492495 11.00000 -1.50000 H24C 2 0.442748 0.321954 0.442191 11.00000 -1.50000 AFIX 0 C25 1 0.515585 0.506109 0.397857 11.00000 0.10937 0.11270 = 0.07730 0.02619 -0.01051 0.01731 AFIX 137 H25A 2 0.439376 0.511027 0.369864 11.00000 -1.50000 H25B 2 0.588408 0.531995 0.376818 11.00000 -1.50000 H25C 2 0.498650 0.529844 0.440739 11.00000 -1.50000 AFIX 0 REM PHENYL FLAT C26 > C31 SAME C26 > C31 SAME C26 C31 < C27 C26 1 0.683659 0.152936 0.360165 11.00000 0.03170 0.10696 = 0.04863 -0.01270 -0.00433 0.00557 AFIX 43 H26 2 0.737802 0.188947 0.381684 11.00000 -1.20000 AFIX 0 C27 1 0.720317 0.124246 0.300420 11.00000 0.04194 0.09054 = 0.06448 -0.01293 0.01673 -0.00488 AFIX 43 H27 2 0.799566 0.139488 0.281349 11.00000 -1.20000 AFIX 0 C28 1 0.642115 0.073443 0.268281 11.00000 0.06387 0.11279 = 0.07440 -0.03009 0.01393 -0.01312 AFIX 43 H28 2 0.663627 0.054746 0.225783 11.00000 -1.20000 AFIX 0 C29 1 0.529977 0.049960 0.299769 11.00000 0.07095 0.15321 = 0.07944 -0.05904 0.01694 -0.04377 AFIX 43 H29 2 0.477817 0.012351 0.278980 11.00000 -1.20000 AFIX 0 C30 1 0.490730 0.079289 0.360646 11.00000 0.07353 0.08268 = 0.05592 -0.01918 0.00669 -0.02361 AFIX 43 H30 2 0.412364 0.063874 0.380555 11.00000 -1.20000 AFIX 0 C31 1 0.570911 0.131319 0.390096 11.00000 0.05019 0.06193 = 0.04557 -0.01214 0.00261 0.00183 C32 1 0.524981 0.164419 0.455046 11.00000 0.04565 0.07044 = 0.05026 -0.02026 0.01245 -0.01072 AFIX 43 H32 2 0.435910 0.159783 0.464208 11.00000 -1.20000 AFIX 0 C33 1 0.594111 0.198273 0.499275 11.00000 0.05256 0.06006 = 0.04163 -0.01111 -0.00278 0.01095 AFIX 43 H33 2 0.683551 0.204776 0.492106 11.00000 -1.20000 AFIX 0 C34 1 0.532466 0.228523 0.564181 11.00000 0.05032 0.06881 = 0.02970 -0.00193 0.00586 -0.00736 C35 1 0.609753 0.272405 0.607502 11.00000 0.05071 0.06326 = 0.03303 0.00126 0.00929 -0.01396 AFIX 43 H35 2 0.695034 0.285740 0.595546 11.00000 -1.20000 AFIX 0 C36 1 0.558015 0.296575 0.669699 11.00000 0.05512 0.06270 = 0.03727 0.00438 0.01047 -0.02044 AFIX 43 H36 2 0.469972 0.310679 0.671010 11.00000 -1.20000 AFIX 0 REM PHENYL SAME C37 > C42 SAME C37 C42 < C38 C37 1 0.634609 0.301325 0.734387 11.00000 0.10047 0.05814 = 0.03594 -0.00429 -0.00741 -0.00984 C38 1 0.565403 0.297679 0.791938 11.00000 0.11726 0.04533 = 0.03867 0.00007 0.00627 0.01097 AFIX 43 H38 2 0.474715 0.292071 0.791394 11.00000 -1.20000 AFIX 0 C39 1 0.633918 0.302572 0.852188 11.00000 0.17589 0.06246 = 0.04020 0.01396 -0.01340 0.00478 AFIX 43 H39 2 0.587347 0.301625 0.892357 11.00000 -1.20000 AFIX 0 C40 1 0.765276 0.308628 0.854301 11.00000 0.17641 0.07277 = 0.05697 0.00851 -0.04957 0.00470 AFIX 43 H40 2 0.809110 0.306954 0.895255 11.00000 -1.20000 AFIX 0 C41 1 0.833775 0.317256 0.795830 11.00000 0.12818 0.13203 = 0.08436 0.02801 -0.04845 -0.02059 AFIX 43 H41 2 0.923123 0.328110 0.796424 11.00000 -1.20000 AFIX 0 C42 1 0.766369 0.309381 0.735053 11.00000 0.08992 0.17495 = 0.05647 0.02253 -0.01440 -0.00995 AFIX 43 H42 2 0.812571 0.309690 0.694765 11.00000 -1.20000 AFIX 0 HKLF 4 REM scaled_a.res in P2(1)2(1)2(1) REM wR2 = 0.3504, GooF = S = 1.301, Restrained GooF = 1.249 for all data REM R1 = 0.1432 for 2459 Fo > 4sig(Fo) and 0.1764 for all 3596 data REM 428 parameters refined using 429 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.279, deepest hole -0.176, 1-sigma level 0.049 Q1 1 0.5830 0.4423 0.6047 11.00000 0.05 0.28 Q2 1 0.5445 0.6561 0.6634 11.00000 0.05 0.19 Q3 1 0.3969 0.6485 0.8548 11.00000 0.05 0.17 Q4 1 0.5874 0.4063 0.3654 11.00000 0.05 0.16 Q5 1 0.7523 0.1995 0.5080 11.00000 0.05 0.15 Q6 1 0.4899 0.2338 0.6762 11.00000 0.05 0.15 Q7 1 0.6036 0.3998 0.8487 11.00000 0.05 0.15 Q8 1 0.3947 0.5321 0.4758 11.00000 0.05 0.14 Q9 1 0.6577 0.6576 0.6635 11.00000 0.05 0.13 Q10 1 0.8057 0.0676 0.2459 11.00000 0.05 0.13 Q11 1 0.9752 0.2226 0.7871 11.00000 0.05 0.13 Q12 1 0.2480 0.6749 0.5059 11.00000 0.05 0.13 Q13 1 0.1211 0.4537 0.4840 11.00000 0.05 0.13 Q14 1 0.3039 0.6776 0.8295 11.00000 0.05 0.13 Q15 1 0.6165 0.4709 0.8176 11.00000 0.05 0.12 Q16 1 0.6474 0.0425 0.2781 11.00000 0.05 0.12 Q17 1 0.2001 0.6772 0.5378 11.00000 0.05 0.12 Q18 1 0.6172 0.0436 0.3898 11.00000 0.05 0.12 Q19 1 0.3502 0.4553 0.6626 11.00000 0.05 0.12 Q20 1 0.9990 0.2797 0.6760 11.00000 0.05 0.12 ; _shelx_res_checksum 52510 _shelx_hkl_file ; 0 0 3 -11.60 7.28 0 0 -3 4.99 9.06 0 0 4 1862.67 492.65 0 0 -4 1829.89 484.11 0 0 5 11.69 8.88 0 0 -5 -4.14 10.37 0 0 6 245.59 67.28 0 0 -6 284.46 77.68 0 0 7 -1.82 7.36 0 0 -7 -8.71 10.10 0 0 8 210.58 58.85 0 0 -8 216.78 60.89 0 0 9 -8.07 8.53 0 0 -9 10.68 12.71 0 0 10 109.22 34.17 0 0 -10 96.41 32.00 0 0 11 2.44 11.60 0 0 -11 11.65 14.09 0 0 12 18.41 13.68 0 0 -12 8.19 13.47 0 0 13 6.10 11.11 0 0 -13 0.02 11.65 0 0 14 131.74 41.17 0 0 -14 93.77 31.31 0 0 15 4.05 12.26 0 0 -15 6.36 11.54 0 0 16 -2.36 12.62 0 0 -16 23.77 15.04 0 0 17 0.21 14.42 0 0 -17 4.53 13.37 0 0 18 171.89 54.64 0 0 -18 166.24 52.40 0 0 19 20.54 16.58 0 0 -19 1.65 11.41 0 -1 3 26.27 11.87 0 1 -3 34.09 12.67 0 1 4 152.00 42.02 0 -1 4 186.68 52.87 0 -1 -4 243.41 66.23 0 1 -4 271.08 73.83 0 1 5 2038.35 539.47 0 -1 5 2724.32 720.67 0 -1 -5 1785.00 472.55 0 1 -5 1899.56 503.12 0 1 6 61.49 20.10 0 -1 6 105.64 33.16 0 -1 -6 109.90 32.80 0 1 -6 71.24 25.94 0 1 7 565.62 152.09 0 -1 7 609.96 164.73 0 -1 -7 397.65 108.03 0 1 -7 557.91 150.31 0 1 8 592.89 160.02 0 -1 8 662.56 178.31 0 -1 -8 862.76 230.80 0 1 -8 654.03 176.21 0 1 9 157.51 46.90 0 -1 9 103.05 32.63 0 1 -9 77.93 27.31 0 1 10 814.30 219.20 0 -1 10 1399.20 373.41 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42.57 0 -3 15 94.43 33.40 0 -3 -15 91.81 31.09 0 3 -15 88.73 31.23 0 3 16 1235.63 332.66 0 -3 16 1267.56 341.20 0 -3 -16 1157.15 312.00 0 3 -16 1169.53 315.03 0 3 17 331.28 95.67 0 -3 17 328.53 94.79 0 -3 -17 276.20 81.32 0 3 -17 284.46 82.39 0 3 18 7.42 15.60 0 -3 18 14.84 17.65 0 -3 -18 4.92 13.13 0 3 -18 -10.46 14.40 0 3 19 105.66 36.18 0 -3 19 98.50 33.35 0 -3 -19 101.06 34.95 0 3 -19 71.57 27.81 0 -4 0 1520.37 406.73 0 4 0 1429.49 382.50 0 -4 1 220.50 99.55 0 4 -1 4039.80 1078.38 0 4 -1 104.81 48.49 0 4 2 451.90 122.57 0 -4 2 88.29 41.97 0 -4 -2 273.83 75.10 0 4 -2 66.42 31.89 0 4 3 246.14 68.02 0 -4 3 745.73 334.31 0 -4 -3 413.62 112.16 0 4 -3 519.92 233.55 0 -4 4 820.91 368.73 0 4 -4 723.42 325.22 0 -4 5 291.62 134.80 0 4 -5 326.33 149.43 0 4 7 14.46 8.40 0 -4 -7 19.43 10.83 0 4 8 151.76 43.26 0 -4 -8 202.51 56.65 0 4 9 1.43 9.34 0 -4 -9 26.39 13.90 0 4 10 332.11 91.37 0 -4 -10 362.39 99.47 0 4 11 79.42 26.68 0 -4 11 202.76 58.27 0 -4 -11 107.01 33.82 0 4 -11 109.30 34.39 0 4 12 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9.42 0 7 18 44.31 19.26 0 -7 18 34.75 14.96 0 -7 -18 36.93 19.05 0 7 -18 18.73 10.18 0 -8 0 194.03 54.61 0 8 0 199.54 56.59 0 8 1 130.26 38.69 0 -8 1 104.75 30.65 0 -8 -1 137.50 39.98 0 8 -1 140.72 40.62 0 8 2 200.45 57.36 0 -8 2 170.81 48.33 0 -8 -2 187.37 53.40 0 8 -2 177.42 49.82 0 8 3 53.48 20.00 0 -8 3 21.22 9.50 0 -8 3 27.17 19.68 0 -8 -3 28.06 15.63 0 8 -3 36.16 13.90 0 8 -3 19.49 14.54 0 -8 4 388.28 176.16 0 8 -4 411.14 186.15 0 8 5 620.43 169.55 0 -8 5 540.57 244.29 0 -8 -5 642.46 175.17 0 8 -5 1327.60 595.09 0 8 6 63.17 23.40 0 -8 6 71.74 39.49 0 -8 -6 80.44 26.21 0 8 -6 151.27 73.11 0 8 7 78.21 25.54 0 -8 7 306.77 142.04 0 -8 -7 89.03 29.11 0 8 -7 308.15 142.32 0 -8 8 150.55 74.02 0 8 -8 140.81 69.20 0 -8 9 54.55 36.02 0 8 -9 -2.76 23.18 0 -8 10 96.82 52.16 0 8 -10 152.00 75.32 0 8 -11 11.91 26.73 0 8 12 30.29 13.00 0 8 13 73.11 24.49 0 -8 -13 29.66 13.23 0 8 14 258.16 74.10 0 -8 -14 338.44 94.76 0 8 15 4.37 11.44 0 -8 -15 0.21 11.08 0 8 16 4.35 10.96 0 -8 -16 43.81 18.70 0 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