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 ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 B18 Cl18 O2 P2 Pd2, 2(C4 H8 O)' _chemical_formula_sum 'C44 H56 B18 Cl18 O2 P2 Pd2' _chemical_formula_weight 1612.20 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' 'B' 'B' 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' 'P' 'P' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 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 triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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' _cell_length_a 13.050(3) _cell_length_b 12.040(2) _cell_length_c 13.060(3) _cell_angle_alpha 107.57(3) _cell_angle_beta 91.15(3) _cell_angle_gamma 123.19(3) _cell_volume 1592.3(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3713 _cell_measurement_theta_min 0.077 _cell_measurement_theta_max 0.627 _exptl_crystal_description 'nano prism' _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_F_000 279 _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 _shelx_estimated_absorpt_T_min 0.0 _shelx_estimated_absorpt_T_max 0.0 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 23883 _diffrn_reflns_av_unetI/netI 0.1456 _diffrn_reflns_av_R_equivalents 0.2173 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 0.077 _diffrn_reflns_theta_max 0.627 _diffrn_reflns_theta_full 0.627 _diffrn_measured_fraction_theta_max 0.809 _diffrn_measured_fraction_theta_full 0.809 _diffrn_reflns_Laue_measured_fraction_max 0.809 _diffrn_reflns_Laue_measured_fraction_full 0.809 _diffrn_reflns_point_group_measured_fraction_max 0.809 _diffrn_reflns_point_group_measured_fraction_full 0.809 _reflns_number_total 3713 _reflns_number_gt 2839 _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 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 1362(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3713 _refine_ls_number_parameters 398 _refine_ls_number_restraints 557 _refine_ls_R_factor_all 0.2155 _refine_ls_R_factor_gt 0.1822 _refine_ls_wR_factor_ref 0.4004 _refine_ls_wR_factor_gt 0.3798 _refine_ls_goodness_of_fit_ref 1.929 _refine_ls_restrained_S_all 1.803 _refine_ls_shift/su_max 0.028 _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 0.3851(2) 0.7719(3) 0.5036(4) 0.0658(13) Uani 1 1 d . . . . . Cl1 Cl 0.2239(6) 0.5185(6) 0.4640(9) 0.078(2) Uani 1 1 d . . . . . P1 P 0.4101(5) 0.8215(6) 0.6747(8) 0.057(2) Uani 1 1 d . . . . . O1 O 0.3616(14) 0.7198(15) 0.3406(19) 0.088(3) Uani 1 1 d . . . . . C1 C 0.5244(13) 0.9739(15) 0.5312(19) 0.080(5) Uani 1 1 d . . . . . H1A H 0.550898 1.031577 0.609455 0.096 Uiso 1 1 calc R U . . . H1B H 0.596014 0.979420 0.506351 0.096 Uiso 1 1 calc R U . . . B1 B 0.2363(13) 0.5131(15) 0.5903(19) 0.060(3) Uani 1 1 d . . . . . Cl2 Cl 0.5134(5) 0.6006(6) 0.6657(8) 0.078(3) Uani 1 1 d . . . . . C2 C 0.3243(9) 0.6574(11) 0.6956(14) 0.047(3) Uani 1 1 d . . . . . B2 B 0.3670(11) 0.5527(13) 0.6755(17) 0.053(3) Uani 1 1 d . . . . . Cl3 Cl 0.4013(5) 0.7405(6) 0.9254(8) 0.066(2) Uani 1 1 d . . . . . B3 B 0.3188(11) 0.6151(13) 0.7983(16) 0.047(3) Uani 1 1 d . . . . . Cl4 Cl 0.0963(5) 0.6361(6) 0.7121(8) 0.076(3) Uani 1 1 d . . . . . B4 B 0.1852(11) 0.5718(13) 0.7011(16) 0.050(3) Uani 1 1 d . . . . . Cl5 Cl -0.0370(6) 0.2905(7) 0.5469(9) 0.090(3) Uani 1 1 d . . . . . B5 B 0.1079(12) 0.3827(14) 0.6230(19) 0.062(3) Uani 1 1 d . . . . . Cl6 Cl 0.2565(7) 0.2653(7) 0.5127(10) 0.093(3) Uani 1 1 d . . . . . B6 B 0.2402(12) 0.3754(13) 0.6124(19) 0.062(3) Uani 1 1 d . . . . . Cl7 Cl 0.3833(6) 0.4340(7) 0.8469(9) 0.092(3) Uani 1 1 d . . . . . B7 B 0.2935(11) 0.4489(14) 0.7589(18) 0.054(3) Uani 1 1 d . . . . . Cl8 Cl 0.0861(6) 0.4573(7) 0.8782(9) 0.080(3) Uani 1 1 d . . . . . B8 B 0.1644(11) 0.4603(13) 0.7716(17) 0.050(3) Uani 1 1 d . . . . . Cl9 Cl 0.0678(5) 0.1517(6) 0.6992(9) 0.086(3) Uani 1 1 d . . . . . B9 B 0.1503(12) 0.3171(14) 0.6919(19) 0.061(4) Uani 1 1 d . . . . . C3 C 0.3482(10) 0.9156(11) 0.7345(12) 0.050(3) Uani 1 1 d D . . . . C4 C 0.3000(11) 0.9502(13) 0.6697(15) 0.061(4) Uani 1 1 d D . . . . H4 H 0.298562 0.921283 0.594847 0.073 Uiso 1 1 calc R U . . . C5 C 0.2533(13) 1.0255(16) 0.7093(17) 0.067(5) Uani 1 1 d D . . . . H5 H 0.215405 1.043984 0.662098 0.080 Uiso 1 1 calc R U . . . C6 C 0.2624(13) 1.0732(15) 0.8173(13) 0.064(4) Uani 1 1 d D . . . . H6 H 0.238357 1.133812 0.847038 0.077 Uiso 1 1 calc R U . . . C7 C 0.3049(12) 1.0357(13) 0.8825(15) 0.062(4) Uani 1 1 d D . . . . H7 H 0.304477 1.063356 0.957045 0.075 Uiso 1 1 calc R U . . . C8 C 0.3490(12) 0.9577(14) 0.8418(17) 0.063(4) Uani 1 1 d D . . . . H8 H 0.380314 0.932693 0.888553 0.075 Uiso 1 1 calc R U . . . C9 C 0.5655(10) 0.9193(11) 0.7451(12) 0.052(3) Uani 1 1 d D . . . . C10 C 0.6172(10) 1.0170(14) 0.8546(16) 0.068(4) Uani 1 1 d D . . . . H10 H 0.564626 1.025017 0.898582 0.081 Uiso 1 1 calc R U . . . C11 C 0.7387(11) 1.0970(16) 0.8956(17) 0.081(5) Uani 1 1 d D . . . . H11 H 0.771054 1.160994 0.968601 0.097 Uiso 1 1 calc R U . . . C12 C 0.8150(13) 1.0891(15) 0.8366(15) 0.091(6) Uani 1 1 d D . . . . H12 H 0.901192 1.147235 0.867104 0.109 Uiso 1 1 calc R U . . . C13 C 0.7701(11) 0.9989(16) 0.7341(19) 0.087(5) Uani 1 1 d D . . . . H13 H 0.826519 0.995528 0.693142 0.104 Uiso 1 1 calc R U . . . C14 C 0.6490(10) 0.9124(13) 0.6856(15) 0.074(5) Uani 1 1 d D . . . . H14 H 0.620865 0.848300 0.612894 0.088 Uiso 1 1 calc R U . . . C15 C 0.420(2) 0.670(2) 0.275(3) 0.096(5) Uani 1 1 d . . . . . H15A H 0.510286 0.736699 0.301074 0.115 Uiso 1 1 calc R U . . . H15B H 0.394638 0.578390 0.276345 0.115 Uiso 1 1 calc R U . . . C16 C 0.386(2) 0.655(3) 0.172(3) 0.136(8) Uani 1 1 d . . . . . H16A H 0.382342 0.576094 0.118193 0.163 Uiso 1 1 calc R U . . . H16B H 0.443613 0.741776 0.158795 0.163 Uiso 1 1 calc R U . . . C17 C 0.260(2) 0.625(2) 0.166(3) 0.110(6) Uani 1 1 d . . . . . H17A H 0.247774 0.670524 0.122343 0.132 Uiso 1 1 calc R U . . . H17B H 0.195404 0.522588 0.133099 0.132 Uiso 1 1 calc R U . . . C18 C 0.2532(16) 0.6790(17) 0.274(2) 0.090(5) Uani 1 1 d . . . . . H18A H 0.178667 0.606562 0.289784 0.108 Uiso 1 1 calc R U . . . H18B H 0.250362 0.760598 0.285299 0.108 Uiso 1 1 calc R U . . . O20 O 0.880(3) 0.791(4) 0.965(4) 0.175(11) Uani 1 1 d D U . A 1 C20 C 0.955(3) 0.771(5) 0.904(4) 0.199(16) Uani 1 1 d D U . A 1 H20A H 1.043082 0.842523 0.941944 0.239 Uiso 1 1 calc R U . A 1 H20B H 0.935510 0.676824 0.889267 0.239 Uiso 1 1 calc R U . A 1 C21 C 0.930(4) 0.785(6) 0.812(4) 0.210(18) Uani 1 1 d D U . A 1 H21A H 0.991296 0.881997 0.816517 0.252 Uiso 1 1 calc R U . A 1 H21B H 0.936146 0.720656 0.749908 0.252 Uiso 1 1 calc R U . A 1 C22 C 0.824(4) 0.756(5) 0.797(4) 0.200(16) Uani 1 1 d D U . A 1 H22A H 0.765294 0.657361 0.746522 0.240 Uiso 1 1 calc R U . A 1 H22B H 0.822368 0.817485 0.764690 0.240 Uiso 1 1 calc R U . A 1 C23 C 0.792(3) 0.774(4) 0.893(3) 0.170(13) Uani 1 1 d D U . A 1 H23A H 0.709226 0.691356 0.887542 0.204 Uiso 1 1 calc R U . A 1 H23B H 0.791334 0.858044 0.917167 0.204 Uiso 1 1 calc R U . A 1 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 0.0512(15) 0.0368(13) 0.102(4) 0.0277(17) 0.0209(17) 0.0204(11) Cl1 0.068(4) 0.037(3) 0.085(7) 0.012(4) 0.010(4) 0.010(3) P1 0.031(3) 0.029(3) 0.109(7) 0.027(3) 0.022(3) 0.015(2) O1 0.086(7) 0.071(7) 0.108(8) 0.027(7) 0.031(7) 0.048(7) C1 0.065(8) 0.056(7) 0.129(18) 0.058(9) 0.039(9) 0.031(6) B1 0.043(6) 0.037(6) 0.085(8) 0.018(6) 0.026(6) 0.016(5) Cl2 0.041(3) 0.048(3) 0.157(11) 0.047(5) 0.050(4) 0.028(3) C2 0.038(5) 0.029(4) 0.076(8) 0.023(5) 0.022(5) 0.019(4) B2 0.035(5) 0.034(6) 0.093(10) 0.028(6) 0.036(6) 0.019(5) Cl3 0.056(3) 0.043(3) 0.082(7) 0.019(3) 0.014(3) 0.022(3) B3 0.038(5) 0.028(5) 0.077(8) 0.027(5) 0.025(5) 0.015(4) Cl4 0.041(3) 0.051(3) 0.145(10) 0.042(4) 0.027(4) 0.030(3) B4 0.033(5) 0.028(5) 0.092(10) 0.029(6) 0.026(6) 0.015(4) Cl5 0.050(3) 0.055(4) 0.122(11) 0.020(5) -0.005(4) 0.013(3) B5 0.037(5) 0.032(6) 0.094(9) 0.014(6) 0.012(5) 0.012(5) Cl6 0.082(4) 0.046(3) 0.126(10) 0.014(4) 0.054(5) 0.031(3) B6 0.038(6) 0.025(5) 0.102(9) 0.014(6) 0.027(6) 0.010(5) Cl7 0.059(3) 0.070(4) 0.178(11) 0.078(6) 0.027(4) 0.040(3) B7 0.033(5) 0.035(5) 0.101(9) 0.031(6) 0.031(5) 0.021(5) Cl8 0.070(4) 0.060(4) 0.120(9) 0.043(5) 0.058(5) 0.038(3) B8 0.029(5) 0.032(5) 0.088(8) 0.027(6) 0.024(5) 0.015(5) Cl9 0.055(3) 0.040(3) 0.170(12) 0.056(5) 0.040(5) 0.024(3) B9 0.038(6) 0.031(5) 0.107(12) 0.023(6) 0.027(6) 0.016(5) C3 0.048(6) 0.035(6) 0.077(11) 0.024(7) 0.019(7) 0.028(5) C4 0.072(7) 0.067(7) 0.085(12) 0.041(8) 0.042(8) 0.057(7) C5 0.091(9) 0.093(10) 0.062(12) 0.027(10) 0.013(10) 0.081(9) C6 0.084(8) 0.069(8) 0.066(12) 0.018(9) 0.022(9) 0.062(8) C7 0.080(8) 0.054(7) 0.055(12) 0.000(7) 0.005(8) 0.050(6) C8 0.079(8) 0.065(8) 0.084(11) 0.037(9) 0.031(9) 0.060(7) C9 0.034(5) 0.039(5) 0.091(10) 0.037(5) 0.027(5) 0.020(4) C10 0.040(5) 0.062(7) 0.092(11) 0.023(7) 0.018(6) 0.027(5) C11 0.045(6) 0.080(9) 0.108(14) 0.039(8) 0.014(6) 0.029(6) C12 0.035(6) 0.054(8) 0.141(15) 0.025(8) 0.025(7) 0.006(6) C13 0.039(5) 0.076(9) 0.135(15) 0.030(8) 0.032(7) 0.032(6) C14 0.038(5) 0.049(7) 0.113(13) 0.022(7) 0.033(6) 0.017(5) C15 0.117(11) 0.076(10) 0.121(15) 0.053(12) 0.062(12) 0.063(10) C16 0.127(14) 0.136(18) 0.118(15) 0.063(17) 0.062(15) 0.053(14) C17 0.154(13) 0.082(12) 0.100(12) 0.035(11) 0.038(12) 0.072(12) C18 0.084(8) 0.057(9) 0.091(12) 0.014(10) 0.015(8) 0.027(8) O20 0.20(2) 0.23(3) 0.14(3) 0.06(3) 0.048(19) 0.15(2) C20 0.17(2) 0.29(4) 0.17(4) 0.08(3) 0.06(2) 0.15(3) C21 0.21(3) 0.32(5) 0.13(4) 0.05(4) 0.05(3) 0.19(3) C22 0.24(3) 0.32(4) 0.13(3) 0.06(3) 0.07(2) 0.22(3) C23 0.19(2) 0.23(3) 0.10(3) 0.00(2) 0.028(18) 0.16(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.988(12) . ? Pd1 O1 1.99(2) . ? Pd1 P1 2.100(10) . ? Pd1 Cl1 2.445(6) . ? Cl1 B1 1.68(2) . ? P1 C9 1.732(14) . ? P1 C3 1.744(13) . ? P1 C2 1.774(11) . ? O1 C15 1.38(3) . ? O1 C18 1.39(3) . ? C1 C1 1.48(3) 2_676 ? B1 C2 1.59(2) . ? B1 B4 1.73(3) . ? B1 B5 1.73(2) . ? B1 B2 1.76(3) . ? B1 B6 1.79(2) . ? Cl2 B2 1.687(12) . ? C2 B4 1.538(15) . ? C2 B3 1.56(2) . ? C2 B2 1.595(15) . ? B2 B6 1.729(17) . ? B2 B7 1.79(2) . ? B2 B3 1.83(2) . ? Cl3 B3 1.68(2) . ? B3 B7 1.740(16) . ? B3 B8 1.767(15) . ? B3 B4 1.85(2) . ? Cl4 B4 1.699(13) . ? B4 B8 1.75(2) . ? B4 B5 1.813(19) . ? Cl5 B5 1.660(18) . ? B5 B9 1.62(3) . ? B5 B6 1.781(19) . ? B5 B8 1.81(3) . ? Cl6 B6 1.666(19) . ? B6 B9 1.59(3) . ? B6 B7 1.78(3) . ? Cl7 B7 1.738(19) . ? B7 B9 1.62(2) . ? B7 B8 1.771(16) . ? Cl8 B8 1.741(19) . ? B8 B9 1.63(2) . ? Cl9 B9 1.705(14) . ? C3 C4 1.328(15) . ? C3 C8 1.336(15) . ? C4 C5 1.340(15) . ? C5 C6 1.328(16) . ? C6 C7 1.314(16) . ? C7 C8 1.342(15) . ? C9 C14 1.377(15) . ? C9 C10 1.400(16) . ? C10 C11 1.308(16) . ? C11 C12 1.299(16) . ? C12 C13 1.307(18) . ? C13 C14 1.320(17) . ? C15 C16 1.33(4) . ? C16 C17 1.47(3) . ? C17 C18 1.38(3) . ? O20 C20 1.35(4) . ? O20 C23 1.36(4) . ? C20 C21 1.33(4) . ? C21 C22 1.22(4) . ? C22 C23 1.33(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 O1 91.5(8) . . ? C1 Pd1 P1 89.5(7) . . ? O1 Pd1 P1 178.2(4) . . ? C1 Pd1 Cl1 175.7(5) . . ? O1 Pd1 Cl1 86.8(5) . . ? P1 Pd1 Cl1 92.1(3) . . ? B1 Cl1 Pd1 101.0(6) . . ? C9 P1 C3 108.0(7) . . ? C9 P1 C2 108.4(7) . . ? C3 P1 C2 107.0(6) . . ? C9 P1 Pd1 114.2(5) . . ? C3 P1 Pd1 111.6(6) . . ? C2 P1 Pd1 107.4(6) . . ? C15 O1 C18 108(2) . . ? C15 O1 Pd1 126.2(18) . . ? C18 O1 Pd1 122.4(14) . . ? C1 C1 Pd1 107.1(14) 2_676 . ? C2 B1 Cl1 120.3(11) . . ? C2 B1 B4 55.0(9) . . ? Cl1 B1 B4 129.5(11) . . ? C2 B1 B5 111.7(15) . . ? Cl1 B1 B5 120.1(13) . . ? B4 B1 B5 63.2(9) . . ? C2 B1 B2 56.6(9) . . ? Cl1 B1 B2 128.1(10) . . ? B4 B1 B2 93.0(14) . . ? B5 B1 B2 104.0(13) . . ? C2 B1 B6 108.4(15) . . ? Cl1 B1 B6 121.4(13) . . ? B4 B1 B6 104.0(13) . . ? B5 B1 B6 60.6(8) . . ? B2 B1 B6 58.3(9) . . ? B4 C2 B3 73.5(10) . . ? B4 C2 B1 66.8(9) . . ? B3 C2 B1 107.4(11) . . ? B4 C2 B2 107.4(8) . . ? B3 C2 B2 71.0(10) . . ? B1 C2 B2 66.9(10) . . ? B4 C2 P1 126.8(8) . . ? B3 C2 P1 134.3(11) . . ? B1 C2 P1 118.2(13) . . ? B2 C2 P1 123.5(8) . . ? C2 B2 Cl2 124.4(8) . . ? C2 B2 B6 111.5(10) . . ? Cl2 B2 B6 119.7(9) . . ? C2 B2 B1 56.5(9) . . ? Cl2 B2 B1 136.2(13) . . ? B6 B2 B1 61.9(9) . . ? C2 B2 B7 105.7(10) . . ? Cl2 B2 B7 116.8(10) . . ? B6 B2 B7 60.8(9) . . ? B1 B2 B7 101.8(9) . . ? C2 B2 B3 53.6(9) . . ? Cl2 B2 B3 127.2(12) . . ? B6 B2 B3 102.3(9) . . ? B1 B2 B3 90.1(9) . . ? B7 B2 B3 57.3(8) . . ? C2 B3 Cl3 121.1(9) . . ? C2 B3 B7 109.8(13) . . ? Cl3 B3 B7 121.3(12) . . ? C2 B3 B8 105.7(13) . . ? Cl3 B3 B8 123.3(12) . . ? B7 B3 B8 60.7(6) . . ? C2 B3 B2 55.3(9) . . ? Cl3 B3 B2 132.3(9) . . ? B7 B3 B2 60.2(8) . . ? B8 B3 B2 99.5(10) . . ? C2 B3 B4 52.7(8) . . ? Cl3 B3 B4 132.2(9) . . ? B7 B3 B4 100.9(10) . . ? B8 B3 B4 57.9(8) . . ? B2 B3 B4 86.4(11) . . ? C2 B4 Cl4 124.2(8) . . ? C2 B4 B1 58.1(9) . . ? Cl4 B4 B1 131.1(14) . . ? C2 B4 B8 107.3(10) . . ? Cl4 B4 B8 119.4(9) . . ? B1 B4 B8 101.2(10) . . ? C2 B4 B5 110.3(10) . . ? Cl4 B4 B5 117.9(9) . . ? B1 B4 B5 58.6(9) . . ? B8 B4 B5 61.0(9) . . ? C2 B4 B3 53.8(9) . . ? Cl4 B4 B3 132.8(12) . . ? B1 B4 B3 90.5(10) . . ? B8 B4 B3 58.5(8) . . ? B5 B4 B3 101.7(9) . . ? B9 B5 Cl5 122.3(9) . . ? B9 B5 B1 110.9(10) . . ? Cl5 B5 B1 121.4(15) . . ? B9 B5 B6 55.5(10) . . ? Cl5 B5 B6 135.7(14) . . ? B1 B5 B6 61.3(8) . . ? B9 B5 B8 56.4(11) . . ? Cl5 B5 B8 129.8(11) . . ? B1 B5 B8 98.7(11) . . ? B6 B5 B8 88.2(12) . . ? B9 B5 B4 109.5(14) . . ? Cl5 B5 B4 117.6(9) . . ? B1 B5 B4 58.2(8) . . ? B6 B5 B4 101.0(9) . . ? B8 B5 B4 57.9(9) . . ? B9 B6 Cl6 120.3(9) . . ? B9 B6 B2 113.2(15) . . ? Cl6 B6 B2 118.8(9) . . ? B9 B6 B5 57.1(10) . . ? Cl6 B6 B5 129.3(14) . . ? B2 B6 B5 103.2(9) . . ? B9 B6 B7 57.1(11) . . ? Cl6 B6 B7 132.1(12) . . ? B2 B6 B7 61.4(9) . . ? B5 B6 B7 91.5(12) . . ? B9 B6 B1 109.3(10) . . ? Cl6 B6 B1 120.7(15) . . ? B2 B6 B1 59.8(9) . . ? B5 B6 B1 58.0(8) . . ? B7 B6 B1 100.9(11) . . ? B9 B7 Cl7 122.4(10) . . ? B9 B7 B3 113.1(10) . . ? Cl7 B7 B3 115.8(12) . . ? B9 B7 B8 57.2(8) . . ? Cl7 B7 B8 132.1(14) . . ? B3 B7 B8 60.4(6) . . ? B9 B7 B6 55.5(11) . . ? Cl7 B7 B6 132.4(9) . . ? B3 B7 B6 103.9(11) . . ? B8 B7 B6 89.4(11) . . ? B9 B7 B2 108.5(15) . . ? Cl7 B7 B2 119.8(8) . . ? B3 B7 B2 62.5(8) . . ? B8 B7 B2 100.9(10) . . ? B6 B7 B2 57.8(9) . . ? B9 B8 Cl8 121.3(9) . . ? B9 B8 B4 112.0(15) . . ? Cl8 B8 B4 118.4(8) . . ? B9 B8 B3 111.3(9) . . ? Cl8 B8 B3 116.8(13) . . ? B4 B8 B3 63.5(8) . . ? B9 B8 B7 56.7(8) . . ? Cl8 B8 B7 130.1(13) . . ? B4 B8 B7 103.6(9) . . ? B3 B8 B7 58.9(6) . . ? B9 B8 B5 55.9(11) . . ? Cl8 B8 B5 131.8(9) . . ? B4 B8 B5 61.1(10) . . ? B3 B8 B5 105.3(11) . . ? B7 B8 B5 90.9(11) . . ? B6 B9 B5 67.3(12) . . ? B6 B9 B7 67.5(10) . . ? B5 B9 B7 103.9(10) . . ? B6 B9 B8 101.9(10) . . ? B5 B9 B8 67.7(10) . . ? B7 B9 B8 66.1(9) . . ? B6 B9 Cl9 129.8(12) . . ? B5 B9 Cl9 130.2(11) . . ? B7 B9 Cl9 125.9(13) . . ? B8 B9 Cl9 128.2(13) . . ? C4 C3 C8 118.2(12) . . ? C4 C3 P1 117.8(11) . . ? C8 C3 P1 124.0(9) . . ? C3 C4 C5 121.8(15) . . ? C6 C5 C4 118.6(14) . . ? C7 C6 C5 120.6(13) . . ? C6 C7 C8 120.1(16) . . ? C3 C8 C7 120.4(15) . . ? C14 C9 C10 116.3(12) . . ? C14 C9 P1 117.4(11) . . ? C10 C9 P1 125.9(8) . . ? C11 C10 C9 120.7(13) . . ? C12 C11 C10 121.4(17) . . ? C11 C12 C13 119.6(15) . . ? C12 C13 C14 123.5(14) . . ? C13 C14 C9 118.4(15) . . ? C16 C15 O1 109(2) . . ? C15 C16 C17 103(2) . . ? C18 C17 C16 107(2) . . ? C17 C18 O1 105.7(19) . . ? C20 O20 C23 105(5) . . ? C21 C20 O20 105(3) . . ? C22 C21 C20 109(2) . . ? C21 C22 C23 109(2) . . ? C22 C23 O20 106(3) . . ? _refine_diff_density_max 0.334 _refine_diff_density_min -0.176 _refine_diff_density_rms 0.055 _shelx_res_file ; TITL scaled_a.res in P-1 scaled_a.res created by SHELXL-2018/3 at 19:39:00 on 29-May-2019 REM Old TITL Lavallo Pd REM SHELXT solution in P-1: R1 0.293, Rweak 0.170, Alpha 0.273 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C32 B P2 Cl9 CELL 0.019687 13.0500 12.0400 13.0600 107.566 91.152 123.194 ZERR 1.000 0.0030 0.0020 0.0030 0.030 0.030 0.030 LATT 1 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 B 0.1298 0.418 0.52 3.9214 1.3767 16.6634 = 0.7666 51.7511 0 0 0 0 0.83 10.811 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 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 CL 0.3398 0.3379 0.8908 2.619 2.3878 11.0684 = 1.2376 33.5378 0 0 0 0 0.99 35.45 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 44 56 18 4 2 18 2 ACTA L.S. 50 BOND LIST 4 FMAP 2 PLAN 20 RIGU WGHT 0.100000 EXTI 1617.889038 FVAR 1.84232 PD1 7 0.385082 0.771866 0.503593 11.00000 0.05117 0.03677 = 0.10209 0.02771 0.02092 0.02037 CL1 6 0.223948 0.518453 0.463967 11.00000 0.06824 0.03713 = 0.08475 0.01236 0.01009 0.01014 P1 5 0.410133 0.821479 0.674712 11.00000 0.03142 0.02880 = 0.10893 0.02722 0.02236 0.01540 O1 4 0.361639 0.719767 0.340632 11.00000 0.08572 0.07086 = 0.10790 0.02668 0.03140 0.04793 C1 1 0.524372 0.973892 0.531195 11.00000 0.06548 0.05634 = 0.12931 0.05788 0.03888 0.03067 AFIX 23 H1A 2 0.550898 1.031577 0.609455 11.00000 -1.20000 H1B 2 0.596014 0.979420 0.506351 11.00000 -1.20000 AFIX 0 B1 3 0.236252 0.513089 0.590327 11.00000 0.04341 0.03662 = 0.08499 0.01767 0.02557 0.01607 CL2 6 0.513355 0.600624 0.665734 11.00000 0.04132 0.04830 = 0.15683 0.04716 0.05047 0.02840 C2 1 0.324280 0.657395 0.695600 11.00000 0.03774 0.02918 = 0.07575 0.02253 0.02190 0.01900 B2 3 0.366951 0.552653 0.675498 11.00000 0.03499 0.03441 = 0.09304 0.02845 0.03595 0.01856 CL3 6 0.401296 0.740499 0.925373 11.00000 0.05607 0.04299 = 0.08240 0.01877 0.01392 0.02178 B3 3 0.318827 0.615138 0.798302 11.00000 0.03805 0.02751 = 0.07692 0.02668 0.02465 0.01532 CL4 6 0.096257 0.636075 0.712128 11.00000 0.04097 0.05114 = 0.14500 0.04229 0.02676 0.02979 B4 3 0.185177 0.571823 0.701144 11.00000 0.03311 0.02802 = 0.09166 0.02873 0.02558 0.01544 CL5 6 -0.036951 0.290495 0.546876 11.00000 0.04960 0.05504 = 0.12172 0.01978 -0.00461 0.01299 B5 3 0.107949 0.382666 0.622952 11.00000 0.03684 0.03247 = 0.09402 0.01421 0.01153 0.01247 CL6 6 0.256489 0.265347 0.512655 11.00000 0.08189 0.04614 = 0.12637 0.01374 0.05409 0.03050 B6 3 0.240171 0.375429 0.612392 11.00000 0.03751 0.02506 = 0.10233 0.01385 0.02696 0.01014 CL7 6 0.383282 0.434039 0.846871 11.00000 0.05854 0.07000 = 0.17778 0.07838 0.02683 0.03986 B7 3 0.293548 0.448900 0.758950 11.00000 0.03275 0.03545 = 0.10094 0.03120 0.03146 0.02071 CL8 6 0.086131 0.457322 0.878219 11.00000 0.06972 0.05982 = 0.12023 0.04270 0.05775 0.03830 B8 3 0.164419 0.460338 0.771621 11.00000 0.02891 0.03240 = 0.08822 0.02716 0.02405 0.01482 CL9 6 0.067823 0.151696 0.699224 11.00000 0.05548 0.04040 = 0.16962 0.05645 0.04024 0.02351 B9 3 0.150346 0.317125 0.691858 11.00000 0.03767 0.03121 = 0.10685 0.02338 0.02745 0.01581 REM Ph ring SAME C3 > C8 SAME C3 C8 < C4 C3 1 0.348194 0.915587 0.734546 11.00000 0.04823 0.03504 = 0.07657 0.02408 0.01920 0.02788 C4 1 0.299978 0.950165 0.669740 11.00000 0.07158 0.06747 = 0.08482 0.04113 0.04173 0.05739 AFIX 43 H4 2 0.298562 0.921283 0.594847 11.00000 -1.20000 AFIX 0 C5 1 0.253318 1.025510 0.709278 11.00000 0.09126 0.09290 = 0.06197 0.02710 0.01280 0.08131 AFIX 43 H5 2 0.215405 1.043984 0.662098 11.00000 -1.20000 AFIX 0 C6 1 0.262370 1.073250 0.817293 11.00000 0.08385 0.06916 = 0.06560 0.01835 0.02158 0.06248 AFIX 43 H6 2 0.238357 1.133812 0.847038 11.00000 -1.20000 AFIX 0 C7 1 0.304917 1.035740 0.882519 11.00000 0.08000 0.05419 = 0.05452 -0.00019 0.00506 0.05012 AFIX 43 H7 2 0.304477 1.063356 0.957045 11.00000 -1.20000 AFIX 0 C8 1 0.349010 0.957660 0.841821 11.00000 0.07895 0.06519 = 0.08370 0.03704 0.03131 0.06004 AFIX 43 H8 2 0.380314 0.932693 0.888553 11.00000 -1.20000 AFIX 0 REM Ph ring SAME C9 > C14 SAME C9 C14 < C10 C9 1 0.565471 0.919295 0.745114 11.00000 0.03384 0.03891 = 0.09061 0.03698 0.02704 0.01961 C10 1 0.617184 1.016973 0.854590 11.00000 0.03980 0.06171 = 0.09229 0.02265 0.01817 0.02691 AFIX 43 H10 2 0.564626 1.025017 0.898582 11.00000 -1.20000 AFIX 0 C11 1 0.738651 1.097011 0.895605 11.00000 0.04523 0.07968 = 0.10760 0.03887 0.01438 0.02913 AFIX 43 H11 2 0.771054 1.160994 0.968601 11.00000 -1.20000 AFIX 0 C12 1 0.815027 1.089079 0.836595 11.00000 0.03452 0.05372 = 0.14055 0.02485 0.02504 0.00567 AFIX 43 H12 2 0.901192 1.147235 0.867104 11.00000 -1.20000 AFIX 0 C13 1 0.770119 0.998909 0.734094 11.00000 0.03893 0.07642 = 0.13532 0.03007 0.03220 0.03231 AFIX 43 H13 2 0.826519 0.995528 0.693142 11.00000 -1.20000 AFIX 0 C14 1 0.649047 0.912398 0.685577 11.00000 0.03828 0.04941 = 0.11278 0.02233 0.03315 0.01712 AFIX 43 H14 2 0.620865 0.848300 0.612894 11.00000 -1.20000 AFIX 0 C15 1 0.419593 0.669772 0.274528 11.00000 0.11721 0.07624 = 0.12145 0.05269 0.06242 0.06341 AFIX 23 H15A 2 0.510286 0.736699 0.301074 11.00000 -1.20000 H15B 2 0.394638 0.578390 0.276345 11.00000 -1.20000 AFIX 0 C16 1 0.385798 0.654809 0.171718 11.00000 0.12681 0.13638 = 0.11794 0.06340 0.06208 0.05263 AFIX 23 H16A 2 0.382342 0.576094 0.118193 11.00000 -1.20000 H16B 2 0.443613 0.741776 0.158795 11.00000 -1.20000 AFIX 0 C17 1 0.259957 0.624842 0.166346 11.00000 0.15413 0.08221 = 0.09983 0.03503 0.03844 0.07164 AFIX 23 H17A 2 0.247774 0.670524 0.122343 11.00000 -1.20000 H17B 2 0.195404 0.522588 0.133099 11.00000 -1.20000 AFIX 0 C18 1 0.253247 0.678985 0.273726 11.00000 0.08445 0.05686 = 0.09148 0.01435 0.01508 0.02678 AFIX 23 H18A 2 0.178667 0.606562 0.289784 11.00000 -1.20000 H18B 2 0.250362 0.760598 0.285299 11.00000 -1.20000 AFIX 0 PART 1 REM THF ISOR O20 C20 C21 C22 C23 SAME O20 > C23 SAME O20 C23 < C20 O20 4 0.880423 0.791105 0.965439 11.00000 0.19552 0.23492 = 0.13553 0.06424 0.04775 0.15058 C20 1 0.955075 0.771210 0.904264 11.00000 0.17384 0.28528 = 0.16952 0.07711 0.05601 0.15429 AFIX 23 H20A 2 1.043082 0.842523 0.941944 11.00000 -1.20000 H20B 2 0.935510 0.676824 0.889267 11.00000 -1.20000 AFIX 0 C21 1 0.930364 0.784724 0.811599 11.00000 0.21464 0.31792 = 0.13385 0.04801 0.05490 0.19323 AFIX 23 H21A 2 0.991296 0.881997 0.816517 11.00000 -1.20000 H21B 2 0.936146 0.720656 0.749908 11.00000 -1.20000 AFIX 0 C22 1 0.824424 0.755783 0.796980 11.00000 0.23610 0.32172 = 0.12709 0.06287 0.07118 0.22088 AFIX 23 H22A 2 0.765294 0.657361 0.746522 11.00000 -1.20000 H22B 2 0.822368 0.817485 0.764690 11.00000 -1.20000 AFIX 0 C23 1 0.792189 0.774109 0.893298 11.00000 0.19038 0.22827 = 0.09927 0.00045 0.02771 0.15573 AFIX 23 H23A 2 0.709226 0.691356 0.887542 11.00000 -1.20000 H23B 2 0.791334 0.858044 0.917167 11.00000 -1.20000 PART 0 AFIX 0 HKLF 4 REM scaled_a.res in P-1 REM wR2 = 0.4004, GooF = S = 1.929, Restrained GooF = 1.803 for all data REM R1 = 0.1822 for 2839 Fo > 4sig(Fo) and 0.2155 for all 3713 data REM 398 parameters refined using 557 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.334, deepest hole -0.176, 1-sigma level 0.055 Q1 1 0.3735 0.8210 0.6121 11.00000 0.05 0.33 Q2 1 0.4421 0.7761 0.5473 11.00000 0.05 0.33 Q3 1 0.3228 0.7562 0.4558 11.00000 0.05 0.30 Q4 1 0.4041 0.7154 0.3972 11.00000 0.05 0.29 Q5 1 0.4015 0.8745 0.7771 11.00000 0.05 0.26 Q6 1 0.4545 0.8561 0.7252 11.00000 0.05 0.20 Q7 1 0.0189 0.4413 0.8113 11.00000 0.05 0.20 Q8 1 0.3120 0.5241 0.8924 11.00000 0.05 0.18 Q9 1 0.0791 0.3999 0.7624 11.00000 0.05 0.18 Q10 1 0.0647 0.2004 0.8008 11.00000 0.05 0.17 Q11 1 0.3167 0.4045 0.7927 11.00000 0.05 0.17 Q12 1 0.5817 0.8759 0.6573 11.00000 0.05 0.17 Q13 1 0.5976 0.6582 0.7146 11.00000 0.05 0.16 Q14 1 0.3159 0.8604 0.5428 11.00000 0.05 0.16 Q15 1 0.2290 0.1642 0.5144 11.00000 0.05 0.16 Q16 1 0.3000 0.5325 0.5211 11.00000 0.05 0.16 Q17 1 0.3811 0.6619 0.9558 11.00000 0.05 0.16 Q18 1 0.1977 0.4408 0.4851 11.00000 0.05 0.16 Q19 1 0.0309 0.3141 0.5928 11.00000 0.05 0.15 Q20 1 0.4307 0.5216 0.9722 11.00000 0.05 0.15 ; _shelx_res_checksum 45468 _shelx_hkl_file ; 0 -2 3 60.66 32.09 0 -2 3 63.24 14.90 0 2 -3 93.36 44.10 0 2 -3 62.56 14.74 0 -2 2 2539.12 571.00 0 -2 2 1934.19 478.36 0 -2 2 2879.63 430.67 0 2 -2 2123.80 919.20 0 2 -2 2846.83 425.75 0 2 -2 2654.59 596.92 0 -2 1 2771.38 414.33 0 -2 1 3731.25 1396.18 0 -2 1 2592.91 508.15 0 -2 1 3017.41 998.59 0 2 -1 3741.75 1400.12 0 2 -1 2550.93 500.02 0 2 -1 2815.33 420.96 0 -2 0 43.04 9.42 0 -2 0 89.43 16.11 0 -2 0 47.56 12.88 0 2 0 79.52 14.51 0 2 0 43.76 12.09 0 2 0 41.10 9.10 0 -2 -1 15.98 5.21 0 2 1 16.23 5.11 0 -3 5 41.31 10.90 0 3 -5 46.30 11.83 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79.59 0 -4 4 289.86 66.00 0 -4 4 118.82 21.34 0 4 -4 294.92 67.12 0 4 -4 235.08 103.47 0 4 -4 130.90 23.03 0 4 -4 216.97 54.86 0 -4 3 4842.69 1089.13 0 -4 3 2842.89 703.34 0 -4 3 4542.20 679.72 0 -4 3 3565.92 699.40 0 4 -3 4205.61 1819.37 0 4 -3 2899.97 717.12 0 4 -3 3283.79 643.97 0 4 -3 4637.99 694.15 0 4 -3 4820.38 1083.88 0 -4 2 5542.75 1834.46 0 -4 2 6076.82 2274.05 0 -4 2 6259.87 935.60 0 4 -2 7177.76 2686.08 0 4 -2 7308.98 3162.42 0 4 -2 6319.57 944.79 0 4 -2 5594.59 1852.18 0 -4 1 316.90 54.77 0 -4 1 386.18 150.25 0 -4 1 351.28 54.56 0 -4 1 459.86 152.80 0 4 -1 365.58 142.31 0 4 -1 338.88 52.74 0 4 -1 324.58 56.00 0 -4 0 708.59 120.86 0 -4 0 530.46 176.29 0 -4 0 886.39 344.65 0 -4 0 526.79 80.90 0 -4 0 508.35 127.42 0 4 0 508.35 127.55 0 4 0 524.82 80.64 0 4 0 690.87 117.77 0 -4 -1 115.87 20.53 0 4 1 113.64 20.02 0 -4 -2 898.86 152.93 0 4 2 938.23 159.36 0 -4 -3 227.28 40.13 0 -5 8 41.75 11.80 0 5 -8 3.57 19.95 0 5 -8 30.66 9.46 0 -5 7 16.42 24.28 0 -5 7 33.39 10.03 0 5 -7 20.74 21.11 0 5 -7 26.25 8.75 0 -5 6 528.10 119.74 0 -5 6 564.51 87.46 0 5 -6 544.04 123.22 0 5 -6 532.56 82.80 0 -5 5 235.22 54.08 0 -5 5 192.30 88.05 0 -5 5 181.54 30.84 0 5 -5 162.45 74.07 0 5 -5 189.55 31.84 0 5 -5 255.09 58.41 0 -5 4 120.72 28.51 0 -5 4 93.89 24.66 0 -5 4 117.51 54.57 0 -5 4 86.34 18.78 0 -5 4 103.40 19.90 0 5 -4 88.05 23.57 0 5 -4 141.20 64.33 0 5 -4 108.72 20.16 0 5 -4 137.00 31.97 0 5 -4 92.51 19.97 0 -5 3 233.25 87.92 0 -5 3 154.64 35.99 0 -5 3 141.59 24.96 0 -5 3 153.52 31.74 0 -5 3 159.10 53.18 0 5 -3 377.78 165.14 0 5 -3 339.34 127.55 0 5 -3 130.90 43.99 0 5 -3 146.12 30.21 0 5 -3 142.51 24.81 0 5 -3 160.08 37.08 0 -5 2 503.03 86.15 0 -5 2 639.90 212.32 0 -5 2 568.97 213.23 0 -5 2 660.69 165.33 0 -5 2 529.81 81.75 0 5 -2 569.56 189.02 0 5 -2 574.61 215.33 0 5 -2 453.11 70.27 0 5 -2 514.39 88.05 0 5 -2 709.90 177.60 0 -5 1 39.52 9.60 0 -5 1 25.77 10.55 0 -5 1 22.46 8.09 0 -5 1 22.67 8.14 0 5 -1 34.60 8.97 0 5 -1 25.46 7.05 0 5 -1 13.57 6.73 0 -5 0 176.95 31.66 0 -5 0 257.06 86.08 0 -5 0 238.89 93.30 0 -5 0 113.18 20.52 0 -5 0 163.30 42.25 0 5 0 150.97 39.35 0 5 0 111.28 20.08 0 5 0 165.47 29.52 0 -5 -1 6.37 6.32 0 -5 -1 19.07 6.84 0 -5 -1 12.58 6.54 0 5 1 19.43 6.34 0 5 1 20.88 8.51 0 5 1 7.34 6.40 0 -5 -2 7.35 5.26 0 -5 -2 12.16 6.71 0 5 2 4.20 4.49 0 -5 -3 18.04 7.29 0 5 3 24.65 7.37 0 -6 10 5.83 5.99 0 6 -10 4.20 5.50 0 -6 9 13.56 23.87 0 -6 9 61.21 16.01 0 6 -9 6.21 22.08 0 6 -9 56.27 15.14 0 -6 8 215.20 49.88 0 6 -8 211.20 49.01 0 -6 7 686.28 155.36 0 -6 7 791.91 122.10 0 6 -7 726.96 164.42 0 6 -7 822.75 126.50 0 -6 6 191.25 86.93 0 -6 6 330.35 83.00 0 -6 6 336.91 77.03 0 -6 6 407.44 64.94 0 6 -6 259.35 114.95 0 6 -6 420.04 105.30 0 6 -6 363.28 58.24 0 6 -6 340.26 77.75 0 -6 5 99.20 46.65 0 -6 5 53.41 13.90 0 -6 5 31.99 10.77 0 -6 5 37.43 9.96 0 -6 5 48.39 12.79 0 6 -5 43.01 13.48 0 6 -5 114.62 53.12 0 6 -5 42.51 10.87 0 6 -5 65.01 14.53 0 6 -5 55.83 14.48 0 -6 4 1620.57 702.03 0 -6 4 1582.52 356.46 0 -6 4 1093.72 166.45 0 -6 4 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21.98 9.98 0 9 -6 160.94 38.17 0 9 -6 55.05 20.27 0 -9 5 35.48 19.45 0 -9 5 17.05 8.21 0 -9 5 26.72 10.73 0 -9 5 31.55 9.95 0 -9 5 9.70 10.62 0 9 -5 6.40 9.19 0 9 -5 50.24 25.60 0 9 -5 14.20 6.63 0 9 -5 17.42 9.05 0 9 -5 36.94 14.28 0 -9 4 28.11 10.68 0 -9 4 19.19 11.50 0 9 -4 6.22 8.75 0 9 -4 49.55 13.12 0 9 -4 17.98 9.15 0 -9 3 25.58 9.11 0 -9 3 40.78 16.25 0 -9 3 38.24 16.63 0 -9 3 30.33 10.75 0 -9 3 33.76 11.57 0 9 -3 56.26 20.94 0 9 -3 32.84 11.72 0 9 -3 34.50 11.16 0 9 -3 26.08 8.40 0 -9 2 26.56 12.58 0 -9 2 31.44 13.10 0 -9 2 23.82 9.80 0 -9 2 24.98 9.62 0 9 -2 43.53 17.89 0 9 -2 16.64 8.25 0 9 -2 17.64 8.58 0 -9 1 10.95 7.49 0 -9 1 13.69 10.20 0 -9 1 12.03 7.73 0 9 -1 27.33 8.88 0 9 -1 9.82 7.89 0 -9 0 2.09 6.10 0 -9 0 14.95 10.43 0 -9 0 3.79 7.39 0 -9 0 0.48 5.13 0 -9 0 16.87 8.48 0 9 0 11.53 9.74 0 9 0 -0.89 5.65 0 9 0 2.24 6.63 0 9 0 -4.33 5.26 0 -9 -1 17.86 9.63 0 -9 -1 19.22 8.96 0 -9 -1 10.51 7.09 0 9 1 14.18 6.84 0 9 1 8.73 7.05 0 9 1 11.22 8.95 0 -9 -2 8.94 7.98 0 -9 -2 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_shelx_hkl_checksum 3381