Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Robin Bedford' _publ_contact_author_address ; Chemistry Department University of Bristol Cantock's Close Clifton Bristol BS8 1TS UNITED KINGDOM ; _publ_contact_author_email R.BEDFORD@BRISTOL.AC.UK _publ_section_title ; Five-coordinate Pd(II) orthometallated triarylphosphite complexes ; loop_ _publ_author_name 'Robin Bedford' 'Michael Betham' 'Craig P. Butts' 'Simon J. Coles' 'Marica Cutajar' 'Thomas Gelbrich' ; M.Hursthouse ; 'P. Noelle Scully' 'Stephen Wimperis' data_8 _database_code_depnum_ccdc_archive 'CCDC 207765' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 F6 N2 O4 Pd2' _chemical_formula_weight 731.25 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 11.0425(2) _cell_length_b 15.4028(3) _cell_length_c 16.0274(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2726.03(10) _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 yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.782 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 1.392 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7681 _exptl_absorpt_correction_T_max 0.8733 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15811 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5039 _reflns_number_gt 4674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2^, conventional R-factors R are based on F, with F set to zero for negative F2^. The threshold expression of F2^ > 2sigma(F2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s2^(Fo2^)+(0.0352P)2^+0.0000P] where P=(Fo2^+2Fc2^)/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 _refine_ls_extinction_coef 0.0009(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc2^\l3^/sin(2\q)]-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 5039 _refine_ls_number_parameters 380 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0688 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.19090(3) 0.05260(2) 0.20412(2) 0.02608(11) Uani 1 1 d . . . Pd2 Pd 0.07147(3) 0.15301(2) 0.07510(2) 0.02468(10) Uani 1 1 d . . . N1' N 0.3248(3) 0.1382(2) 0.2286(2) 0.0303(8) Uani 1 1 d . . . N1 N 0.1933(3) 0.1540(2) -0.0174(2) 0.0263(7) Uani 1 1 d . . . O1 O -0.0598(3) 0.16634(19) 0.16563(18) 0.0312(7) Uani 1 1 d . . . O2 O 0.0457(2) 0.1157(2) 0.27622(19) 0.0324(7) Uani 1 1 d . . . O1' O 0.0664(3) -0.04210(19) 0.17293(18) 0.0319(7) Uani 1 1 d . . . O2' O 0.0049(2) 0.0216(2) 0.0530(2) 0.0318(7) Uani 1 1 d . . . F1 F -0.2473(2) 0.1204(2) 0.2750(2) 0.0612(9) Uani 1 1 d . . . F2 F -0.1881(3) 0.25189(19) 0.28504(19) 0.0577(8) Uani 1 1 d . . . F3 F -0.1352(3) 0.1591(2) 0.37568(18) 0.0587(9) Uani 1 1 d . . . F1' F -0.0700(7) -0.1374(5) 0.0069(3) 0.081(2) Uani 0.63 1 d PDU A 1 F2' F -0.1877(4) -0.0937(4) 0.1052(5) 0.0767(18) Uani 0.63 1 d PDU A 1 F3' F -0.0538(5) -0.1835(3) 0.1325(4) 0.0549(13) Uani 0.63 1 d PDU A 1 F1" F -0.0013(10) -0.1829(7) 0.0706(10) 0.105(4) Uiso 0.37 1 d PD A 2 F2" F -0.1494(14) -0.1336(11) 0.1460(8) 0.132(6) Uiso 0.37 1 d PD A 2 F3" F -0.1314(9) -0.1145(7) 0.0167(6) 0.062(3) Uiso 0.37 1 d PD A 2 C1 C -0.0438(3) 0.1473(3) 0.2411(3) 0.0258(9) Uani 1 1 d . . . C2 C -0.1542(4) 0.1701(3) 0.2956(3) 0.0340(11) Uani 1 1 d . . . C1' C 0.0078(4) -0.0371(3) 0.1057(3) 0.0291(10) Uani 1 1 d . A . C2' C -0.0728(4) -0.1145(3) 0.0868(3) 0.0403(11) Uani 1 1 d D . . C10 C 0.3211(4) -0.0024(3) 0.1395(3) 0.0322(10) Uani 1 1 d . . . C11 C 0.4291(4) 0.0470(3) 0.1382(3) 0.0359(10) Uani 1 1 d . . . C12 C 0.5290(4) 0.0201(4) 0.0924(4) 0.0492(15) Uani 1 1 d . . . H12 H 0.6007 0.0542 0.0918 0.065(17) Uiso 1 1 calc R . . C13 C 0.5238(4) -0.0563(4) 0.0477(3) 0.0473(13) Uani 1 1 d . . . H13 H 0.5920 -0.0752 0.0164 0.050(15) Uiso 1 1 calc R . . C14 C 0.4190(5) -0.1054(3) 0.0486(3) 0.0449(13) Uani 1 1 d . . . H14 H 0.4152 -0.1578 0.0174 0.031(12) Uiso 1 1 calc R . . C15 C 0.3180(4) -0.0786(3) 0.0953(3) 0.0400(12) Uani 1 1 d . . . H15 H 0.2471 -0.1135 0.0962 0.09(2) Uiso 1 1 calc R . . C16 C 0.4235(4) 0.1246(3) 0.1891(3) 0.0340(10) Uani 1 1 d . . . H16 H 0.4900 0.1635 0.1930 0.025(11) Uiso 1 1 calc R . . C17 C 0.3093(4) 0.2124(3) 0.2864(3) 0.0358(11) Uani 1 1 d . . . H17 H 0.2262 0.2361 0.2767 0.026(12) Uiso 1 1 calc R . . C18 C 0.3123(5) 0.1791(3) 0.3746(3) 0.0480(13) Uani 1 1 d . . . H18A H 0.2533 0.1320 0.3808 0.050(16) Uiso 1 1 calc R . . H18B H 0.2920 0.2263 0.4131 0.057(16) Uiso 1 1 calc R . . H18C H 0.3936 0.1572 0.3873 0.053(15) Uiso 1 1 calc R . . C19 C 0.3990(4) 0.2871(4) 0.2702(4) 0.0517(15) Uani 1 1 d . . . H19A H 0.3910 0.3069 0.2124 0.043(15) Uiso 1 1 calc R . . H19B H 0.4819 0.2666 0.2798 0.032(12) Uiso 1 1 calc R . . H19C H 0.3813 0.3353 0.3082 0.042(14) Uiso 1 1 calc R . . C20 C 0.1322(4) 0.2716(3) 0.0899(3) 0.0273(10) Uani 1 1 d . . . C21 C 0.2241(4) 0.2939(3) 0.0321(3) 0.0302(10) Uani 1 1 d . . . C22 C 0.2780(4) 0.3743(3) 0.0335(3) 0.0391(12) Uani 1 1 d . . . H22 H 0.3380 0.3886 -0.0067 0.033(12) Uiso 1 1 calc R . . C23 C 0.2453(4) 0.4346(3) 0.0934(3) 0.0397(12) Uani 1 1 d . . . H23 H 0.2821 0.4903 0.0942 0.08(2) Uiso 1 1 calc R . . C24 C 0.1580(4) 0.4130(3) 0.1525(3) 0.0372(12) Uani 1 1 d . . . H24 H 0.1361 0.4537 0.1944 0.017(10) Uiso 1 1 calc R . . C25 C 0.1018(4) 0.3306(3) 0.1501(3) 0.0332(11) Uani 1 1 d . . . H25 H 0.0424 0.3161 0.1907 0.020(11) Uiso 1 1 calc R . . C26 C 0.2539(4) 0.2245(3) -0.0250(3) 0.0332(11) Uani 1 1 d . . . H26 H 0.3154 0.2308 -0.0660 0.030(11) Uiso 1 1 calc R . . C27 C 0.2102(4) 0.0774(3) -0.0722(3) 0.0309(10) Uani 1 1 d . . . H27 H 0.2005 0.0242 -0.0372 0.026(11) Uiso 1 1 calc R . . C28 C 0.3344(4) 0.0740(3) -0.1123(3) 0.0384(12) Uani 1 1 d . . . H28A H 0.3967 0.0740 -0.0688 0.045(14) Uiso 1 1 calc R . . H28B H 0.3452 0.1249 -0.1483 0.09(2) Uiso 1 1 calc R . . H28C H 0.3414 0.0211 -0.1458 0.050(15) Uiso 1 1 calc R . . C29 C 0.1091(4) 0.0776(4) -0.1376(3) 0.0402(12) Uani 1 1 d . . . H29A H 0.0303 0.0799 -0.1095 0.016(10) Uiso 1 1 calc R . . H29B H 0.1141 0.0246 -0.1712 0.13(3) Uiso 1 1 calc R . . H29C H 0.1181 0.1284 -0.1739 0.052(16) Uiso 1 1 calc R . . 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 0.02613(17) 0.02853(19) 0.02357(18) 0.00263(15) -0.00091(13) 0.00223(14) Pd2 0.02714(17) 0.02493(18) 0.02197(18) 0.00409(14) 0.00164(13) 0.00050(13) N1' 0.0308(19) 0.031(2) 0.029(2) 0.0005(17) -0.0023(16) 0.0023(16) N1 0.0307(17) 0.0257(19) 0.0226(18) 0.0039(16) 0.0003(15) 0.0015(18) O1 0.0307(15) 0.0344(19) 0.0285(17) 0.0061(14) 0.0023(13) 0.0042(14) O2 0.0317(17) 0.0352(18) 0.0302(18) 0.0062(14) 0.0010(13) 0.0051(13) O1' 0.0346(16) 0.0290(17) 0.0322(17) 0.0053(13) -0.0040(14) 0.0015(15) O2' 0.0335(16) 0.0308(19) 0.0310(19) 0.0020(15) -0.0049(13) -0.0015(12) F1 0.0327(15) 0.074(2) 0.077(2) -0.0066(19) 0.0177(15) -0.0085(15) F2 0.072(2) 0.0387(17) 0.062(2) 0.0100(16) 0.0258(17) 0.0225(16) F3 0.0621(18) 0.084(3) 0.0299(17) 0.0130(18) 0.0190(13) 0.0198(19) F1' 0.118(5) 0.076(4) 0.048(3) -0.022(3) 0.025(3) -0.054(4) F2' 0.024(2) 0.051(3) 0.155(5) 0.002(3) -0.009(3) -0.014(2) F3' 0.070(3) 0.029(2) 0.066(3) 0.025(2) -0.029(2) -0.022(2) C1 0.032(2) 0.020(2) 0.026(2) 0.005(2) 0.0001(18) -0.0041(19) C2 0.035(2) 0.035(3) 0.031(3) 0.008(2) 0.009(2) 0.0027(19) C1' 0.032(2) 0.025(3) 0.030(3) 0.006(2) 0.0045(19) 0.0012(17) C2' 0.045(3) 0.040(3) 0.035(3) 0.001(2) -0.001(2) -0.008(2) C10 0.036(2) 0.035(3) 0.025(2) 0.005(2) -0.005(2) 0.008(2) C11 0.031(2) 0.042(3) 0.035(3) 0.000(2) 0.004(2) 0.004(2) C12 0.038(3) 0.065(4) 0.044(3) -0.007(3) 0.006(2) 0.002(2) C13 0.045(3) 0.061(4) 0.036(3) -0.006(3) 0.012(2) 0.017(3) C14 0.059(3) 0.041(3) 0.035(3) -0.004(2) -0.006(2) 0.020(3) C15 0.036(3) 0.038(3) 0.046(3) -0.001(2) -0.005(2) 0.005(2) C16 0.032(2) 0.037(3) 0.032(3) 0.001(2) 0.002(2) -0.0038(19) C17 0.034(2) 0.035(3) 0.038(3) -0.005(2) 0.000(2) 0.0013(19) C18 0.057(3) 0.046(3) 0.041(3) -0.009(3) 0.001(3) 0.004(3) C19 0.043(3) 0.040(3) 0.072(5) -0.007(3) 0.002(3) -0.003(2) C20 0.029(2) 0.024(2) 0.028(3) 0.007(2) -0.0015(18) 0.0022(17) C21 0.031(2) 0.027(3) 0.033(3) 0.005(2) 0.0059(19) 0.0036(17) C22 0.037(3) 0.032(3) 0.048(3) 0.007(2) 0.005(2) -0.0026(19) C23 0.043(3) 0.028(3) 0.048(3) 0.001(2) 0.004(2) -0.002(2) C24 0.034(3) 0.031(3) 0.046(3) -0.007(2) 0.002(2) 0.0059(19) C25 0.028(2) 0.037(3) 0.035(3) 0.002(2) 0.0027(19) 0.0007(18) C26 0.034(2) 0.034(3) 0.032(3) 0.003(2) 0.007(2) 0.008(2) C27 0.035(2) 0.032(3) 0.026(2) -0.004(2) 0.006(2) 0.0059(18) C28 0.040(3) 0.038(3) 0.036(3) -0.011(2) 0.003(2) 0.003(2) C29 0.039(3) 0.051(3) 0.031(3) -0.010(3) -0.001(2) 0.009(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 C10 1.964(5) . ? Pd1 N1' 2.020(3) . ? Pd1 O1' 2.066(3) . ? Pd1 O2 2.202(3) . ? Pd1 Pd2 2.8996(4) . ? Pd2 C20 1.960(4) . ? Pd2 N1 2.002(3) . ? Pd2 O1 2.061(3) . ? Pd2 O2' 2.182(3) . ? N1' C16 1.277(5) . ? N1' C17 1.481(6) . ? N1 C26 1.282(6) . ? N1 C27 1.482(6) . ? O1 C1 1.257(5) . ? O2 C1 1.237(5) . ? O1' C1' 1.259(5) . ? O2' C1' 1.239(5) . ? F1 C2 1.324(5) . ? F2 C2 1.326(5) . ? F3 C2 1.312(5) . ? F1' C2' 1.328(6) . ? F2' C2' 1.342(6) . ? F3' C2' 1.308(5) . ? F1" C2' 1.342(7) . ? F2" C2' 1.305(8) . ? F3" C2' 1.296(7) . ? C1 C2 1.539(6) . ? C1' C2' 1.519(6) . ? C10 C15 1.372(7) . ? C10 C11 1.415(7) . ? C11 C12 1.388(7) . ? C11 C16 1.449(6) . ? C12 C13 1.379(8) . ? C12 H12 0.9500 . ? C13 C14 1.383(8) . ? C13 H13 0.9500 . ? C14 C15 1.405(7) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.504(7) . ? C17 C19 1.540(7) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.367(6) . ? C20 C21 1.417(6) . ? C21 C22 1.375(7) . ? C21 C26 1.445(6) . ? C22 C23 1.383(7) . ? C22 H22 0.9500 . ? C23 C24 1.392(7) . ? C23 H23 0.9500 . ? C24 C25 1.414(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.515(6) . ? C27 C29 1.531(6) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 C10 Pd1 N1' 81.24(17) . . ? C10 Pd1 O1' 93.16(16) . . ? N1' Pd1 O1' 174.38(13) . . ? C10 Pd1 O2 179.35(17) . . ? N1' Pd1 O2 98.23(13) . . ? O1' Pd1 O2 87.38(12) . . ? C10 Pd1 Pd2 100.78(13) . . ? N1' Pd1 Pd2 97.09(10) . . ? O1' Pd1 Pd2 84.34(8) . . ? O2 Pd1 Pd2 78.92(8) . . ? C20 Pd2 N1 81.55(17) . . ? C20 Pd2 O1 93.58(15) . . ? N1 Pd2 O1 173.27(13) . . ? C20 Pd2 O2' 177.59(16) . . ? N1 Pd2 O2' 96.47(13) . . ? O1 Pd2 O2' 88.28(12) . . ? C20 Pd2 Pd1 104.78(12) . . ? N1 Pd2 Pd1 103.10(10) . . ? O1 Pd2 Pd1 82.58(8) . . ? O2' Pd2 Pd1 76.96(8) . . ? C16 N1' C17 122.3(4) . . ? C16 N1' Pd1 114.9(3) . . ? C17 N1' Pd1 122.7(3) . . ? C26 N1 C27 123.5(4) . . ? C26 N1 Pd2 115.3(3) . . ? C27 N1 Pd2 121.2(3) . . ? C1 O1 Pd2 123.7(3) . . ? C1 O2 Pd1 121.1(3) . . ? C1' O1' Pd1 120.4(3) . . ? C1' O2' Pd2 123.9(3) . . ? O2 C1 O1 129.9(4) . . ? O2 C1 C2 117.7(4) . . ? O1 C1 C2 112.4(3) . . ? F3 C2 F1 107.0(4) . . ? F3 C2 F2 107.0(4) . . ? F1 C2 F2 107.4(4) . . ? F3 C2 C1 113.5(3) . . ? F1 C2 C1 110.0(4) . . ? F2 C2 C1 111.6(4) . . ? O2' C1' O1' 129.9(4) . . ? O2' C1' C2' 114.9(4) . . ? O1' C1' C2' 115.1(4) . . ? F3" C2' F2" 107.9(9) . . ? F3" C2' F3' 124.5(7) . . ? F2" C2' F3' 60.9(8) . . ? F3" C2' F1' 34.6(5) . . ? F2" C2' F1' 131.1(9) . . ? F3' C2' F1' 108.7(5) . . ? F3" C2' F2' 73.7(6) . . ? F2" C2' F2' 44.0(7) . . ? F3' C2' F2' 102.9(5) . . ? F1' C2' F2' 107.4(6) . . ? F3" C2' F1" 97.2(8) . . ? F2" C2' F1" 110.2(10) . . ? F3' C2' F1" 51.4(7) . . ? F1' C2' F1" 65.9(7) . . ? F2' C2' F1" 141.9(7) . . ? F3" C2' C1' 117.8(6) . . ? F2" C2' C1' 114.3(8) . . ? F3' C2' C1' 115.5(4) . . ? F1' C2' C1' 112.8(4) . . ? F2' C2' C1' 108.8(4) . . ? F1" C2' C1' 108.0(6) . . ? C15 C10 C11 118.2(4) . . ? C15 C10 Pd1 128.5(4) . . ? C11 C10 Pd1 113.2(3) . . ? C12 C11 C10 121.1(5) . . ? C12 C11 C16 125.4(4) . . ? C10 C11 C16 113.5(4) . . ? C13 C12 C11 119.8(5) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 119.7(4) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C15 120.6(5) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C10 C15 C14 120.5(5) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? N1' C16 C11 116.8(4) . . ? N1' C16 H16 121.6 . . ? C11 C16 H16 121.6 . . ? N1' C17 C18 108.8(4) . . ? N1' C17 C19 113.4(4) . . ? C18 C17 C19 113.5(5) . . ? N1' C17 H17 106.9 . . ? C18 C17 H17 106.9 . . ? C19 C17 H17 106.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 118.4(4) . . ? C25 C20 Pd2 128.4(3) . . ? C21 C20 Pd2 113.1(3) . . ? C22 C21 C20 121.2(4) . . ? C22 C21 C26 125.4(4) . . ? C20 C21 C26 113.4(4) . . ? C21 C22 C23 120.2(5) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 119.6(5) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C23 C24 C25 120.0(5) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C20 C25 C24 120.6(4) . . ? C20 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? N1 C26 C21 116.6(4) . . ? N1 C26 H26 121.7 . . ? C21 C26 H26 121.7 . . ? N1 C27 C28 113.1(4) . . ? N1 C27 C29 108.2(3) . . ? C28 C27 C29 111.7(4) . . ? N1 C27 H27 107.9 . . ? C28 C27 H27 107.9 . . ? C29 C27 H27 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.673 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.079 data_13a _database_code_depnum_ccdc_archive 'CCDC 223269' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H101 F6 O4 P5 Pd' _chemical_formula_weight 1537.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3703(2) _cell_length_b 18.2612(2) _cell_length_c 19.3131(2) _cell_angle_alpha 71.258(7) _cell_angle_beta 74.580(5) _cell_angle_gamma 82.499(5 _cell_volume 4620.97(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 41101 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9507 _exptl_absorpt_correction_T_max 0.9667 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36147 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0830 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 24.55 _reflns_number_total 14919 _reflns_number_gt 10072 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F2^, conventional R-factors R are based on F, with F set to zero for negative F2^. The threshold expression of F2^ > 2sigma(F2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s2^(Fo2^)+(0.0152P)2^+8.0000P] where P=(Fo2^+2Fc2^)/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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14919 _refine_ls_number_parameters 918 _refine_ls_number_restraints 115 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0608 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.82912(2) 0.36625(2) 0.820512(19) 0.04030(12) Uani 1 1 d . . . P1 P 0.70668(8) 0.37090(7) 0.92968(7) 0.0457(3) Uani 1 1 d . . . P2 P 0.94814(8) 0.36164(7) 0.88322(7) 0.0427(3) Uani 1 1 d . . . P3 P 0.75701(11) 0.24354(8) 1.15986(8) 0.0613(4) Uani 1 1 d . . . P4 P 0.73182(8) 0.37718(7) 0.74270(7) 0.0424(3) Uani 1 1 d . . . O4 O 0.6621(2) 0.31153(18) 0.7538(2) 0.0586(9) Uani 1 1 d . . . O1 O 0.6589(3) 0.2801(2) 1.1737(2) 0.0816(11) Uani 1 1 d . . . O2 O 0.8003(2) 0.39017(18) 0.66049(16) 0.0513(8) Uani 1 1 d . . . O3 O 0.6535(2) 0.44514(17) 0.72634(17) 0.0474(8) Uani 1 1 d . . . C1 C 0.7354(3) 0.4000(3) 1.0043(3) 0.0504(12) Uani 1 1 d . . . H1A H 0.7334 0.4561 0.9882 0.061 Uiso 1 1 calc R . . H1B H 0.6827 0.3844 1.0485 0.061 Uiso 1 1 calc R . . C2 C 0.8290(3) 0.3724(3) 1.0304(2) 0.0483(12) Uani 1 1 d . . . C3 C 0.9171(3) 0.3989(3) 0.9649(2) 0.0483(12) Uani 1 1 d . . . H3A H 0.9731 0.3878 0.9864 0.058 Uiso 1 1 calc R . . H3B H 0.9097 0.4548 0.9455 0.058 Uiso 1 1 calc R . . C4 C 0.6091(3) 0.4413(3) 0.9089(3) 0.0514(12) Uani 1 1 d . . . C5 C 0.4493(4) 0.4812(5) 0.8913(4) 0.0857(19) Uani 1 1 d . . . H5 H 0.3873 0.4683 0.8950 0.103 Uiso 1 1 calc R . . C6 C 0.5612(5) 0.5765(4) 0.8612(3) 0.0767(17) Uani 1 1 d . . . H6 H 0.5759 0.6283 0.8440 0.092 Uiso 1 1 calc R . . C7 C 0.4720(5) 0.5565(5) 0.8643(3) 0.085(2) Uani 1 1 d . . . H7 H 0.4264 0.5947 0.8480 0.102 Uiso 1 1 calc R . . C8 C 0.5179(4) 0.4228(3) 0.9135(3) 0.0671(15) Uani 1 1 d . . . H8 H 0.5016 0.3713 0.9314 0.081 Uiso 1 1 calc R . . C9 C 0.6302(4) 0.5199(3) 0.8834(3) 0.0623(14) Uani 1 1 d . . . H9 H 0.6910 0.5339 0.8814 0.075 Uiso 1 1 calc R . . C10 C 0.6529(3) 0.2782(3) 0.9769(3) 0.0525(12) Uani 1 1 d . . . C11 C 0.5721(4) 0.2681(3) 1.0370(3) 0.0714(16) Uani 1 1 d . . . H11 H 0.5451 0.3097 1.0547 0.086 Uiso 1 1 calc R . . C12 C 0.5319(5) 0.1977(4) 1.0702(4) 0.096(2) Uani 1 1 d . . . H12 H 0.4763 0.1921 1.1090 0.116 Uiso 1 1 calc R . . C13 C 0.5736(6) 0.1350(4) 1.0464(4) 0.102(2) Uani 1 1 d . . . H13 H 0.5467 0.0869 1.0698 0.123 Uiso 1 1 calc R . . C14 C 0.6545(5) 0.1430(4) 0.9887(4) 0.0851(19) Uani 1 1 d . . . H14 H 0.6835 0.1003 0.9735 0.102 Uiso 1 1 calc R . . C15 C 0.6926(4) 0.2146(3) 0.9530(3) 0.0608(14) Uani 1 1 d . . . H15 H 0.7459 0.2204 0.9123 0.073 Uiso 1 1 calc R . . C16 C 0.9978(3) 0.2638(3) 0.9148(3) 0.0494(12) Uani 1 1 d . . . C17 C 1.0611(4) 0.2429(3) 0.9614(3) 0.0702(16) Uani 1 1 d . . . H17 H 1.0821 0.2805 0.9760 0.084 Uiso 1 1 calc R . . C18 C 1.0938(5) 0.1662(4) 0.9867(4) 0.097(2) Uani 1 1 d . . . H18 H 1.1365 0.1527 1.0180 0.116 Uiso 1 1 calc R . . C19 C 1.0639(6) 0.1111(4) 0.9659(4) 0.108(2) Uani 1 1 d . . . H19 H 1.0864 0.0600 0.9828 0.130 Uiso 1 1 calc R . . C20 C 1.0000(5) 0.1302(3) 0.9194(4) 0.089(2) Uani 1 1 d . . . H20 H 0.9794 0.0919 0.9055 0.106 Uiso 1 1 calc R . . C22 C 1.0462(3) 0.4248(3) 0.8274(3) 0.0463(12) Uani 1 1 d . . . C21 C 0.9676(4) 0.2055(3) 0.8940(3) 0.0638(14) Uani 1 1 d . . . H21 H 0.9250 0.2183 0.8627 0.077 Uiso 1 1 calc R . . C23 C 1.1404(4) 0.4074(4) 0.8343(3) 0.0744(16) Uani 1 1 d . . . H23 H 1.1571 0.3594 0.8650 0.089 Uiso 1 1 calc R . . C24 C 1.2100(5) 0.4613(5) 0.7957(4) 0.090(2) Uani 1 1 d . . . H24 H 1.2729 0.4494 0.8017 0.108 Uiso 1 1 calc R . . C25 C 1.1882(5) 0.5308(5) 0.7494(4) 0.0859(19) Uani 1 1 d . . . H25 H 1.2362 0.5656 0.7219 0.103 Uiso 1 1 calc R . . C26 C 1.0947(5) 0.5494(4) 0.7433(3) 0.0878(19) Uani 1 1 d . . . H26 H 1.0785 0.5978 0.7131 0.105 Uiso 1 1 calc R . . C27 C 1.0234(4) 0.4956(3) 0.7827(3) 0.0713(16) Uani 1 1 d . . . H27 H 0.9600 0.5084 0.7781 0.086 Uiso 1 1 calc R . . C28 C 0.8196(5) 0.2429(3) 1.2289(3) 0.0738(17) Uani 1 1 d . . . C29 C 0.7650(6) 0.2558(4) 1.2954(4) 0.102(2) Uani 1 1 d . . . H29 H 0.6991 0.2681 1.3006 0.122 Uiso 1 1 calc R . . C30 C 0.8051(10) 0.2510(6) 1.3532(5) 0.138(4) Uani 1 1 d D . . H30 H 0.7667 0.2600 1.3970 0.166 Uiso 1 1 calc R . . C31 C 0.9017(9) 0.2332(6) 1.3469(6) 0.157(5) Uani 1 1 d D . . H31 H 0.9287 0.2284 1.3870 0.189 Uiso 1 1 calc R . . C32 C 0.9588(8) 0.2224(5) 1.2813(6) 0.137(3) Uani 1 1 d D . . H32 H 1.0250 0.2121 1.2764 0.164 Uiso 1 1 calc R . . C33 C 0.9181(6) 0.2269(4) 1.2220(4) 0.100(2) Uani 1 1 d . . . H33 H 0.9571 0.2191 1.1778 0.120 Uiso 1 1 calc R . . C34 C 0.7558(5) 0.1434(3) 1.1683(3) 0.0753(16) Uani 1 1 d . . . C35 C 0.6693(6) 0.1066(5) 1.2044(5) 0.129(3) Uani 1 1 d . . . H35 H 0.6142 0.1338 1.2229 0.155 Uiso 1 1 calc R . . C36 C 0.6667(10) 0.0285(6) 1.2122(8) 0.187(6) Uani 1 1 d . . . H36 H 0.6085 0.0045 1.2362 0.224 Uiso 1 1 calc R . . C37 C 0.7427(13) -0.0134(6) 1.1872(9) 0.196(7) Uani 1 1 d . . . H37 H 0.7381 -0.0655 1.1933 0.235 Uiso 1 1 calc R . . C38 C 0.8237(10) 0.0201(6) 1.1542(8) 0.188(5) Uani 1 1 d . . . H38 H 0.8778 -0.0091 1.1372 0.225 Uiso 1 1 calc R . . C39 C 0.8329(7) 0.1007(4) 1.1427(6) 0.142(3) Uani 1 1 d . . . H39 H 0.8918 0.1233 1.1177 0.170 Uiso 1 1 calc R . . C40 C 0.8992(3) 0.3691(3) 0.6568(3) 0.0432(11) Uani 1 1 d . . . C41 C 0.9316(3) 0.3562(2) 0.7220(2) 0.0385(10) Uani 1 1 d . . . C42 C 1.0274(3) 0.3304(3) 0.7168(3) 0.0487(12) Uani 1 1 d . . . H42 H 1.0521 0.3200 0.7591 0.058 Uiso 1 1 calc R . . C43 C 1.0881(3) 0.3193(3) 0.6517(3) 0.0560(13) Uani 1 1 d . . . C44 C 1.0505(4) 0.3350(3) 0.5892(3) 0.0620(14) Uani 1 1 d . . . H44 H 1.0911 0.3282 0.5452 0.074 Uiso 1 1 calc R . . C45 C 0.9560(3) 0.3600(3) 0.5889(3) 0.0525(13) Uani 1 1 d . . . C46 C 1.1936(4) 0.2916(5) 0.6501(3) 0.090(2) Uani 1 1 d . . . C47 C 1.2482(8) 0.2801(6) 0.5804(6) 0.188(4) Uiso 1 1 d . . . H47A H 1.2317 0.3212 0.5393 0.282 Uiso 1 1 calc R . . H47B H 1.2335 0.2314 0.5778 0.282 Uiso 1 1 calc R . . H47C H 1.3159 0.2800 0.5775 0.282 Uiso 1 1 calc R . . C48 C 1.2507(6) 0.3670(6) 0.6397(6) 0.163(4) Uani 1 1 d U . . H48A H 1.2231 0.3874 0.6812 0.244 Uiso 1 1 calc R . . H48B H 1.2452 0.4058 0.5935 0.244 Uiso 1 1 calc R . . H48C H 1.3177 0.3524 0.6382 0.244 Uiso 1 1 calc R . . C49 C 1.2093(5) 0.2419(5) 0.7220(4) 0.133(3) Uani 1 1 d . . . H49A H 1.1762 0.2646 0.7609 0.199 Uiso 1 1 calc R . . H49B H 1.2773 0.2363 0.7200 0.199 Uiso 1 1 calc R . . H49C H 1.1849 0.1920 0.7327 0.199 Uiso 1 1 calc R . . C50 C 0.9154(4) 0.3754(4) 0.5193(3) 0.0754(17) Uani 1 1 d . . . C51 C 0.9961(5) 0.3630(5) 0.4524(3) 0.129(3) Uani 1 1 d . . . H51A H 0.9697 0.3725 0.4094 0.194 Uiso 1 1 calc R . . H51B H 1.0224 0.3106 0.4657 0.194 Uiso 1 1 calc R . . H51C H 1.0462 0.3980 0.4405 0.194 Uiso 1 1 calc R . . C52 C 0.8753(5) 0.4593(4) 0.4944(3) 0.102(2) Uani 1 1 d . . . H52A H 0.8500 0.4672 0.4511 0.153 Uiso 1 1 calc R . . H52B H 0.9261 0.4940 0.4818 0.153 Uiso 1 1 calc R . . H52C H 0.8246 0.4691 0.5346 0.153 Uiso 1 1 calc R . . C53 C 0.8363(5) 0.3187(4) 0.5361(4) 0.108(2) Uani 1 1 d . . . H53A H 0.8112 0.3287 0.4925 0.163 Uiso 1 1 calc R . . H53B H 0.7851 0.3255 0.5775 0.163 Uiso 1 1 calc R . . H53C H 0.8633 0.2665 0.5490 0.163 Uiso 1 1 calc R . . C54 C 0.6715(3) 0.5250(3) 0.6973(2) 0.0458(11) Uani 1 1 d . . . C55 C 0.6102(3) 0.5741(3) 0.6559(3) 0.0505(12) Uani 1 1 d . . . C56 C 0.6218(4) 0.6523(3) 0.6401(3) 0.0621(14) Uani 1 1 d . . . H56 H 0.5801 0.6870 0.6143 0.075 Uiso 1 1 calc R . . C57 C 0.6915(4) 0.6833(3) 0.6599(3) 0.0641(14) Uani 1 1 d . . . C58 C 0.7539(4) 0.6317(3) 0.6954(3) 0.0612(14) Uani 1 1 d . . . H58 H 0.8036 0.6499 0.7070 0.073 Uiso 1 1 calc R . . C59 C 0.7449(3) 0.5527(3) 0.7144(3) 0.0554(13) Uani 1 1 d . . . H59 H 0.7881 0.5183 0.7387 0.066 Uiso 1 1 calc R . . C60 C 0.5341(4) 0.5437(3) 0.6301(3) 0.0622(14) Uani 1 1 d . . . C61 C 0.4819(5) 0.6104(4) 0.5801(4) 0.104(2) Uani 1 1 d . . . H61A H 0.4351 0.5897 0.5649 0.155 Uiso 1 1 calc R . . H61B H 0.5282 0.6375 0.5362 0.155 Uiso 1 1 calc R . . H61C H 0.4499 0.6454 0.6078 0.155 Uiso 1 1 calc R . . C62 C 0.4593(4) 0.5004(4) 0.6961(3) 0.0843(18) Uani 1 1 d . . . H62A H 0.4125 0.4828 0.6783 0.126 Uiso 1 1 calc R . . H62B H 0.4276 0.5340 0.7256 0.126 Uiso 1 1 calc R . . H62C H 0.4899 0.4566 0.7265 0.126 Uiso 1 1 calc R . . C63 C 0.5840(4) 0.4919(4) 0.5821(3) 0.0784(17) Uani 1 1 d . . . H63A H 0.5367 0.4735 0.5654 0.118 Uiso 1 1 calc R . . H63B H 0.6167 0.4486 0.6113 0.118 Uiso 1 1 calc R . . H63C H 0.6300 0.5208 0.5392 0.118 Uiso 1 1 calc R . . C64 C 0.6928(6) 0.7695(3) 0.6476(4) 0.088(2) Uani 1 1 d . . . C65 C 0.7873(8) 0.7918(5) 0.6534(7) 0.186(4) Uani 1 1 d U . . H65A H 0.8000 0.7619 0.7012 0.279 Uiso 1 1 calc R . . H65B H 0.7834 0.8458 0.6492 0.279 Uiso 1 1 calc R . . H65C H 0.8386 0.7817 0.6136 0.279 Uiso 1 1 calc R . . C66 C 0.6589(9) 0.8170(6) 0.5782(6) 0.184(4) Uani 1 1 d U . . H66A H 0.6613 0.8710 0.5722 0.276 Uiso 1 1 calc R . . H66B H 0.5938 0.8052 0.5834 0.276 Uiso 1 1 calc R . . H66C H 0.7002 0.8050 0.5348 0.276 Uiso 1 1 calc R . . C67 C 0.6239(8) 0.7900(4) 0.7121(5) 0.185(5) Uani 1 1 d . . . H67A H 0.6409 0.7598 0.7582 0.277 Uiso 1 1 calc R . . H67B H 0.5595 0.7794 0.7138 0.277 Uiso 1 1 calc R . . H67C H 0.6269 0.8440 0.7058 0.277 Uiso 1 1 calc R . . C68 C 0.6822(4) 0.2309(3) 0.7731(3) 0.0562(13) Uani 1 1 d . . . C69 C 0.6033(4) 0.1826(3) 0.8012(3) 0.0616(14) Uani 1 1 d . . . C70 C 0.6278(4) 0.1036(3) 0.8194(3) 0.0711(16) Uani 1 1 d . . . H70 H 0.5776 0.0698 0.8375 0.085 Uiso 1 1 calc R . . C71 C 0.7215(5) 0.0714(3) 0.8123(3) 0.0722(16) Uani 1 1 d . . . C72 C 0.7962(4) 0.1221(3) 0.7831(3) 0.0713(16) Uani 1 1 d . . . H72 H 0.8600 0.1027 0.7765 0.086 Uiso 1 1 calc R . . C73 C 0.7763(4) 0.2015(3) 0.7635(3) 0.0613(14) Uani 1 1 d . . . H73 H 0.8268 0.2349 0.7439 0.074 Uiso 1 1 calc R . . C74 C 0.7398(6) -0.0175(3) 0.8363(4) 0.093(2) Uani 1 1 d . . . C75 C 0.6929(6) -0.0507(4) 0.9214(5) 0.121(3) Uani 1 1 d . . . H75A H 0.6248 -0.0375 0.9306 0.182 Uiso 1 1 calc R . . H75B H 0.7216 -0.0292 0.9496 0.182 Uiso 1 1 calc R . . H75C H 0.7033 -0.1060 0.9366 0.182 Uiso 1 1 calc R . . C76 C 0.6902(7) -0.0520(4) 0.7946(5) 0.153(4) Uani 1 1 d . . . H76A H 0.6224 -0.0375 0.8049 0.230 Uiso 1 1 calc R . . H76B H 0.6989 -0.1074 0.8110 0.230 Uiso 1 1 calc R . . H76C H 0.7177 -0.0329 0.7414 0.230 Uiso 1 1 calc R . . C77 C 0.8475(6) -0.0406(4) 0.8244(5) 0.128(3) Uani 1 1 d . . . H77A H 0.8560 -0.0961 0.8405 0.192 Uiso 1 1 calc R . . H77B H 0.8756 -0.0194 0.8532 0.192 Uiso 1 1 calc R . . H77C H 0.8786 -0.0211 0.7719 0.192 Uiso 1 1 calc R . . C78 C 0.4982(4) 0.2141(4) 0.8097(4) 0.0818(18) Uani 1 1 d . . . C79 C 0.4843(5) 0.2641(4) 0.7294(5) 0.118(3) Uani 1 1 d . . . H79A H 0.5004 0.2325 0.6961 0.177 Uiso 1 1 calc R . . H79B H 0.5258 0.3069 0.7098 0.177 Uiso 1 1 calc R . . H79C H 0.4182 0.2832 0.7333 0.177 Uiso 1 1 calc R . . C80 C 0.4731(4) 0.2639(4) 0.8616(4) 0.112(3) Uani 1 1 d . . . H80A H 0.4068 0.2826 0.8660 0.167 Uiso 1 1 calc R . . H80B H 0.5141 0.3071 0.8415 0.167 Uiso 1 1 calc R . . H80C H 0.4824 0.2339 0.9104 0.167 Uiso 1 1 calc R . . C81 C 0.4285(4) 0.1483(4) 0.8391(5) 0.124(3) Uani 1 1 d . . . H81A H 0.4438 0.1169 0.8058 0.186 Uiso 1 1 calc R . . H81B H 0.3634 0.1696 0.8417 0.186 Uiso 1 1 calc R . . H81C H 0.4344 0.1170 0.8885 0.186 Uiso 1 1 calc R . . C82 C 0.8321(4) 0.4145(3) 1.0871(3) 0.0605(14) Uani 1 1 d . . . H82A H 0.8904 0.3985 1.1045 0.091 Uiso 1 1 calc R . . H82B H 0.7772 0.4017 1.1291 0.091 Uiso 1 1 calc R . . H82C H 0.8308 0.4694 1.0631 0.091 Uiso 1 1 calc R . . C83 C 0.8349(3) 0.2843(3) 1.0669(3) 0.0511(12) Uani 1 1 d . . . H83A H 0.9012 0.2691 1.0702 0.061 Uiso 1 1 calc R . . H83B H 0.8210 0.2602 1.0330 0.061 Uiso 1 1 calc R . . P5 P 1.19723(15) 0.32689(10) 1.08142(12) 0.1025(7) Uani 1 1 d D . . F1 F 1.0984(4) 0.3565(4) 1.0566(4) 0.138(4) Uani 0.626(11) 1 d PGDU A 1 F2 F 1.2368(4) 0.2959(6) 1.0090(4) 0.150(4) Uani 0.626(11) 1 d PGD A 1 F3 F 1.1575(4) 0.3546(6) 1.1540(4) 0.201(6) Uani 0.626(11) 1 d PGD A 1 F4 F 1.2400(6) 0.4080(3) 1.0335(5) 0.177(5) Uani 0.626(11) 1 d PGDU A 1 F5 F 1.1531(6) 0.2438(3) 1.1289(5) 0.190(5) Uani 0.626(11) 1 d PGD A 1 F6 F 1.2966(4) 0.2962(5) 1.1054(4) 0.178(5) Uani 0.626(11) 1 d PGD A 1 F1' F 1.1755(7) 0.4098(5) 1.0964(10) 0.135(7) Uani 0.374(11) 1 d PGD A 2 F2' F 1.2054(9) 0.3682(9) 0.9936(3) 0.183(9) Uani 0.374(11) 1 d PGD A 2 F3' F 1.1864(10) 0.2867(9) 1.1695(3) 0.279(14) Uani 0.374(11) 1 d PGDU A 2 F4' F 1.3088(3) 0.3368(7) 1.0693(7) 0.157(7) Uani 0.374(11) 1 d PGDU A 2 F5' F 1.0836(3) 0.3193(7) 1.0941(7) 0.148(7) Uani 0.374(11) 1 d PGD A 2 F6' F 1.2190(8) 0.2454(5) 1.0668(10) 0.162(7) Uani 0.374(11) 1 d PGDU A 2 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 0.0352(2) 0.0466(2) 0.0426(2) -0.01588(17) -0.01326(16) 0.00056(15) P1 0.0386(7) 0.0526(8) 0.0481(8) -0.0193(6) -0.0093(6) -0.0011(6) P2 0.0383(7) 0.0493(7) 0.0432(7) -0.0140(6) -0.0139(6) -0.0027(6) P3 0.0698(10) 0.0503(8) 0.0569(9) -0.0112(7) -0.0097(7) -0.0025(7) P4 0.0363(7) 0.0441(7) 0.0530(8) -0.0176(6) -0.0187(6) 0.0014(5) O4 0.049(2) 0.046(2) 0.091(3) -0.0183(19) -0.0343(19) -0.0044(16) O1 0.071(3) 0.073(3) 0.079(3) -0.012(2) 0.001(2) 0.005(2) O2 0.0400(19) 0.072(2) 0.050(2) -0.0244(18) -0.0201(16) 0.0057(16) O3 0.0400(18) 0.0435(19) 0.062(2) -0.0159(17) -0.0193(16) 0.0030(14) C1 0.051(3) 0.056(3) 0.047(3) -0.019(3) -0.012(2) -0.002(2) C2 0.058(3) 0.046(3) 0.042(3) -0.015(2) -0.012(2) 0.001(2) C3 0.048(3) 0.056(3) 0.044(3) -0.015(2) -0.016(2) -0.006(2) C4 0.043(3) 0.065(4) 0.052(3) -0.028(3) -0.012(2) 0.004(2) C5 0.051(4) 0.123(6) 0.090(5) -0.046(5) -0.021(3) 0.018(4) C6 0.087(5) 0.071(4) 0.067(4) -0.027(3) -0.014(4) 0.025(4) C7 0.080(5) 0.108(6) 0.063(4) -0.040(4) -0.013(4) 0.046(4) C8 0.052(3) 0.079(4) 0.078(4) -0.033(3) -0.019(3) 0.005(3) C9 0.058(3) 0.071(4) 0.059(3) -0.026(3) -0.012(3) 0.009(3) C10 0.046(3) 0.060(3) 0.054(3) -0.020(3) -0.013(3) -0.002(2) C11 0.071(4) 0.074(4) 0.064(4) -0.024(3) 0.001(3) -0.017(3) C12 0.087(5) 0.102(6) 0.089(5) -0.029(5) 0.014(4) -0.038(4) C13 0.120(6) 0.080(5) 0.101(6) -0.016(4) -0.011(5) -0.045(5) C14 0.104(5) 0.060(4) 0.092(5) -0.026(4) -0.015(4) -0.015(4) C15 0.060(3) 0.057(3) 0.063(3) -0.017(3) -0.012(3) -0.005(3) C16 0.047(3) 0.054(3) 0.047(3) -0.015(3) -0.013(2) 0.003(2) C17 0.072(4) 0.073(4) 0.076(4) -0.024(3) -0.040(3) 0.009(3) C18 0.106(5) 0.089(5) 0.103(5) -0.028(4) -0.062(4) 0.039(4) C19 0.146(7) 0.060(4) 0.124(6) -0.028(4) -0.063(6) 0.039(4) C20 0.107(5) 0.056(4) 0.116(6) -0.034(4) -0.045(5) 0.010(4) C22 0.044(3) 0.058(3) 0.042(3) -0.016(3) -0.013(2) -0.009(2) C21 0.064(4) 0.061(4) 0.070(4) -0.022(3) -0.023(3) 0.005(3) C23 0.052(4) 0.079(4) 0.087(4) -0.014(4) -0.013(3) -0.015(3) C24 0.059(4) 0.107(6) 0.099(5) -0.020(5) -0.012(4) -0.026(4) C25 0.075(5) 0.105(6) 0.079(5) -0.027(4) -0.005(4) -0.039(4) C26 0.106(6) 0.072(4) 0.080(5) 0.001(4) -0.030(4) -0.029(4) C27 0.064(4) 0.075(4) 0.071(4) -0.002(3) -0.029(3) -0.018(3) C28 0.111(5) 0.048(3) 0.053(4) -0.008(3) -0.006(4) -0.014(3) C29 0.148(7) 0.087(5) 0.067(5) -0.020(4) -0.017(5) -0.019(5) C30 0.237(13) 0.119(7) 0.068(5) -0.030(5) -0.034(8) -0.042(9) C31 0.293(16) 0.103(7) 0.107(8) -0.003(6) -0.110(11) -0.060(10) C32 0.175(9) 0.130(7) 0.131(8) -0.021(6) -0.097(8) -0.021(6) C33 0.114(6) 0.109(6) 0.076(5) -0.015(4) -0.037(5) -0.009(5) C34 0.086(5) 0.057(4) 0.081(4) -0.014(3) -0.022(4) -0.006(4) C35 0.118(7) 0.080(6) 0.175(9) -0.008(5) -0.043(6) -0.018(5) C36 0.199(13) 0.069(7) 0.282(15) 0.011(8) -0.095(12) -0.059(7) C37 0.28(2) 0.055(7) 0.287(17) -0.024(9) -0.143(16) -0.025(9) C38 0.229(14) 0.071(7) 0.273(15) -0.080(9) -0.056(12) 0.025(8) C39 0.137(7) 0.073(5) 0.204(10) -0.054(6) -0.011(7) 0.000(5) C40 0.036(3) 0.046(3) 0.050(3) -0.017(2) -0.013(2) -0.001(2) C41 0.037(3) 0.043(3) 0.039(3) -0.015(2) -0.012(2) -0.001(2) C42 0.042(3) 0.062(3) 0.047(3) -0.018(3) -0.020(2) 0.004(2) C43 0.041(3) 0.074(4) 0.057(3) -0.028(3) -0.014(3) 0.011(3) C44 0.055(3) 0.083(4) 0.051(3) -0.031(3) -0.009(3) 0.009(3) C45 0.048(3) 0.067(3) 0.049(3) -0.024(3) -0.016(2) 0.002(3) C46 0.060(4) 0.147(6) 0.064(4) -0.047(4) -0.018(3) 0.034(4) C48 0.103(5) 0.168(7) 0.202(7) -0.022(6) -0.045(5) -0.016(5) C49 0.061(4) 0.156(8) 0.124(7) 0.019(6) -0.018(4) 0.031(5) C50 0.066(4) 0.122(5) 0.045(3) -0.035(4) -0.019(3) 0.009(4) C51 0.097(5) 0.245(10) 0.060(4) -0.074(6) -0.027(4) 0.031(6) C52 0.089(5) 0.147(7) 0.061(4) -0.010(4) -0.036(4) 0.011(5) C53 0.108(5) 0.154(7) 0.106(5) -0.078(5) -0.049(4) -0.004(5) C54 0.046(3) 0.049(3) 0.043(3) -0.021(2) -0.006(2) 0.004(2) C55 0.047(3) 0.059(3) 0.043(3) -0.012(3) -0.014(2) 0.008(2) C56 0.070(4) 0.055(4) 0.056(3) -0.012(3) -0.021(3) 0.015(3) C57 0.084(4) 0.047(3) 0.061(4) -0.018(3) -0.018(3) 0.003(3) C58 0.073(4) 0.051(3) 0.066(4) -0.018(3) -0.023(3) -0.009(3) C59 0.054(3) 0.052(3) 0.066(3) -0.020(3) -0.023(3) 0.002(3) C60 0.050(3) 0.073(4) 0.068(4) -0.020(3) -0.029(3) 0.011(3) C61 0.095(5) 0.104(5) 0.120(6) -0.019(5) -0.065(5) 0.010(4) C62 0.047(3) 0.118(5) 0.090(5) -0.031(4) -0.022(3) -0.002(3) C63 0.073(4) 0.101(5) 0.077(4) -0.037(4) -0.032(3) -0.004(3) C64 0.136(6) 0.054(4) 0.086(5) -0.020(4) -0.054(4) 0.008(4) C65 0.181(7) 0.121(6) 0.253(8) -0.049(6) -0.043(6) -0.031(5) C66 0.275(8) 0.130(6) 0.169(7) -0.051(5) -0.083(6) -0.012(6) C67 0.280(13) 0.078(6) 0.171(9) -0.079(6) 0.049(9) -0.026(7) C68 0.058(3) 0.044(3) 0.077(4) -0.020(3) -0.032(3) -0.002(3) C69 0.062(4) 0.055(3) 0.076(4) -0.016(3) -0.032(3) -0.011(3) C70 0.075(4) 0.052(3) 0.094(4) -0.016(3) -0.036(4) -0.014(3) C71 0.086(4) 0.048(3) 0.092(4) -0.022(3) -0.037(4) -0.003(3) C72 0.070(4) 0.053(4) 0.099(5) -0.027(3) -0.032(3) 0.005(3) C73 0.062(4) 0.047(3) 0.083(4) -0.020(3) -0.029(3) -0.005(3) C74 0.117(6) 0.049(4) 0.127(6) -0.027(4) -0.053(5) 0.000(4) C75 0.145(7) 0.067(5) 0.129(7) 0.006(5) -0.038(6) -0.008(5) C76 0.253(11) 0.064(5) 0.190(9) -0.046(5) -0.126(8) 0.002(6) C77 0.122(7) 0.058(4) 0.181(8) -0.020(5) -0.030(6) 0.022(4) C78 0.058(4) 0.077(4) 0.121(5) -0.025(4) -0.043(4) -0.010(3) C79 0.093(5) 0.104(6) 0.177(8) -0.023(6) -0.088(6) -0.003(4) C80 0.067(4) 0.125(6) 0.160(7) -0.075(6) -0.020(5) 0.005(4) C81 0.069(5) 0.092(5) 0.206(9) -0.022(6) -0.039(5) -0.031(4) C82 0.080(4) 0.056(3) 0.054(3) -0.021(3) -0.025(3) 0.000(3) C83 0.054(3) 0.052(3) 0.050(3) -0.020(3) -0.012(2) 0.001(2) P5 0.1273(17) 0.0698(12) 0.1322(18) -0.0158(12) -0.0809(15) -0.0138(11) F1 0.139(6) 0.149(6) 0.150(7) -0.048(5) -0.086(5) 0.019(5) F2 0.144(7) 0.211(11) 0.125(8) -0.074(8) -0.039(6) -0.033(7) F3 0.218(11) 0.290(16) 0.185(10) -0.161(11) -0.126(9) 0.070(11) F4 0.206(8) 0.139(6) 0.168(7) 0.001(5) -0.051(6) -0.055(6) F5 0.219(11) 0.074(5) 0.240(12) -0.023(6) -0.004(10) -0.047(6) F6 0.135(8) 0.219(11) 0.191(9) -0.024(9) -0.118(7) 0.023(7) F1' 0.091(9) 0.131(12) 0.210(19) -0.085(13) -0.042(11) 0.002(8) F2' 0.27(2) 0.151(16) 0.091(10) 0.043(10) -0.067(12) -0.051(15) F3' 0.290(15) 0.287(16) 0.268(15) -0.076(9) -0.088(8) -0.013(8) F4' 0.146(9) 0.158(10) 0.195(10) -0.069(7) -0.065(7) -0.013(6) F5' 0.150(12) 0.206(17) 0.088(9) 0.020(10) -0.055(8) -0.112(12) F6' 0.179(10) 0.131(9) 0.187(10) -0.057(7) -0.046(7) -0.015(6) _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 C41 2.118(4) . ? Pd1 P4 2.2594(11) . ? Pd1 P2 2.3233(12) . ? Pd1 P1 2.3772(12) . ? P1 C10 1.809(5) . ? P1 C4 1.810(5) . ? P1 C1 1.842(4) . ? P2 C16 1.809(5) . ? P2 C22 1.815(5) . ? P2 C3 1.840(4) . ? P3 O1 1.474(4) . ? P3 C34 1.785(6) . ? P3 C28 1.793(6) . ? P3 C83 1.822(5) . ? P4 O3 1.574(3) . ? P4 O4 1.588(3) . ? P4 O2 1.591(3) . ? O4 C68 1.409(5) . ? O2 C40 1.412(5) . ? O3 C54 1.416(5) . ? C1 C2 1.529(6) . ? C2 C3 1.533(6) . ? C2 C83 1.536(6) . ? C2 C82 1.538(6) . ? C4 C8 1.370(6) . ? C4 C9 1.404(7) . ? C5 C7 1.356(9) . ? C5 C8 1.396(8) . ? C6 C7 1.358(8) . ? C6 C9 1.381(7) . ? C10 C15 1.384(6) . ? C10 C11 1.389(7) . ? C11 C12 1.366(8) . ? C12 C13 1.376(9) . ? C13 C14 1.366(8) . ? C14 C15 1.375(7) . ? C16 C17 1.382(6) . ? C16 C21 1.403(6) . ? C17 C18 1.390(8) . ? C18 C19 1.349(9) . ? C19 C20 1.387(8) . ? C20 C21 1.369(7) . ? C22 C27 1.360(7) . ? C22 C23 1.381(6) . ? C23 C24 1.383(8) . ? C24 C25 1.351(9) . ? C25 C26 1.369(8) . ? C26 C27 1.400(8) . ? C28 C33 1.387(8) . ? C28 C29 1.390(8) . ? C29 C30 1.360(11) . ? C30 C31 1.366(8) . ? C31 C32 1.371(8) . ? C32 C33 1.394(9) . ? C34 C39 1.347(9) . ? C34 C35 1.392(9) . ? C35 C36 1.389(12) . ? C36 C37 1.322(16) . ? C37 C38 1.294(15) . ? C38 C39 1.435(12) . ? C40 C41 1.395(6) . ? C40 C45 1.396(6) . ? C41 C42 1.384(6) . ? C42 C43 1.385(6) . ? C43 C44 1.384(6) . ? C43 C46 1.529(7) . ? C44 C45 1.375(6) . ? C45 C50 1.537(7) . ? C46 C47 1.430(11) . ? C46 C49 1.453(9) . ? C46 C48 1.624(10) . ? C50 C52 1.534(8) . ? C50 C53 1.537(8) . ? C50 C51 1.545(7) . ? C54 C59 1.381(6) . ? C54 C55 1.389(6) . ? C55 C56 1.385(7) . ? C55 C60 1.540(6) . ? C56 C57 1.400(7) . ? C57 C58 1.361(7) . ? C57 C64 1.516(7) . ? C58 C59 1.384(6) . ? C60 C62 1.501(7) . ? C60 C63 1.517(7) . ? C60 C61 1.539(7) . ? C64 C67 1.490(9) . ? C64 C65 1.509(11) . ? C64 C66 1.509(11) . ? C68 C73 1.375(6) . ? C68 C69 1.409(7) . ? C69 C70 1.392(7) . ? C69 C78 1.530(7) . ? C70 C71 1.387(7) . ? C71 C72 1.390(7) . ? C71 C74 1.545(8) . ? C72 C73 1.386(7) . ? C74 C76 1.517(9) . ? C74 C77 1.526(9) . ? C74 C75 1.550(9) . ? C78 C80 1.508(8) . ? C78 C81 1.531(8) . ? C78 C79 1.576(9) . ? P5 F4 1.575(3) . ? P5 F6' 1.580(4) . ? P5 F3 1.582(3) . ? P5 F4' 1.583(4) . ? P5 F1 1.592(3) . ? P5 F6 1.595(3) . ? P5 F3' 1.596(4) . ? P5 F2' 1.599(4) . ? P5 F5' 1.603(4) . ? P5 F1' 1.607(4) . ? P5 F5 1.611(3) . ? P5 F2 1.612(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 C41 Pd1 P4 78.88(11) . . ? C41 Pd1 P2 92.79(11) . . ? P4 Pd1 P2 170.93(5) . . ? C41 Pd1 P1 175.55(11) . . ? P4 Pd1 P1 97.91(4) . . ? P2 Pd1 P1 90.59(4) . . ? C10 P1 C4 106.7(2) . . ? C10 P1 C1 105.2(2) . . ? C4 P1 C1 99.6(2) . . ? C10 P1 Pd1 110.95(16) . . ? C4 P1 Pd1 113.00(16) . . ? C1 P1 Pd1 120.08(16) . . ? C16 P2 C22 108.9(2) . . ? C16 P2 C3 106.6(2) . . ? C22 P2 C3 97.2(2) . . ? C16 P2 Pd1 110.89(15) . . ? C22 P2 Pd1 113.65(15) . . ? C3 P2 Pd1 118.56(15) . . ? O1 P3 C34 112.4(3) . . ? O1 P3 C28 112.0(3) . . ? C34 P3 C28 103.4(3) . . ? O1 P3 C83 115.8(2) . . ? C34 P3 C83 104.1(3) . . ? C28 P3 C83 108.1(3) . . ? O3 P4 O4 94.30(16) . . ? O3 P4 O2 100.37(17) . . ? O4 P4 O2 105.83(17) . . ? O3 P4 Pd1 123.97(12) . . ? O4 P4 Pd1 122.81(14) . . ? O2 P4 Pd1 106.50(11) . . ? C68 O4 P4 127.9(3) . . ? C40 O2 P4 116.0(3) . . ? C54 O3 P4 125.6(3) . . ? C2 C1 P1 122.3(3) . . ? C1 C2 C3 110.6(4) . . ? C1 C2 C83 112.0(4) . . ? C3 C2 C83 111.2(4) . . ? C1 C2 C82 107.4(4) . . ? C3 C2 C82 105.2(4) . . ? C83 C2 C82 110.2(4) . . ? C2 C3 P2 122.1(3) . . ? C8 C4 C9 118.3(5) . . ? C8 C4 P1 124.3(4) . . ? C9 C4 P1 117.4(4) . . ? C7 C5 C8 120.7(6) . . ? C7 C6 C9 120.2(6) . . ? C5 C7 C6 120.2(6) . . ? C4 C8 C5 120.1(6) . . ? C6 C9 C4 120.5(5) . . ? C15 C10 C11 118.2(5) . . ? C15 C10 P1 119.7(4) . . ? C11 C10 P1 122.1(4) . . ? C12 C11 C10 120.6(6) . . ? C11 C12 C13 120.2(6) . . ? C14 C13 C12 120.3(6) . . ? C13 C14 C15 119.6(6) . . ? C14 C15 C10 121.1(5) . . ? C17 C16 C21 118.1(5) . . ? C17 C16 P2 123.0(4) . . ? C21 C16 P2 118.8(4) . . ? C16 C17 C18 120.6(5) . . ? C19 C18 C17 120.2(6) . . ? C18 C19 C20 120.6(6) . . ? C21 C20 C19 119.6(6) . . ? C27 C22 C23 118.9(5) . . ? C27 C22 P2 117.8(4) . . ? C23 C22 P2 123.0(4) . . ? C20 C21 C16 120.8(5) . . ? C22 C23 C24 120.2(6) . . ? C25 C24 C23 121.1(6) . . ? C24 C25 C26 119.3(6) . . ? C25 C26 C27 120.1(6) . . ? C22 C27 C26 120.4(5) . . ? C33 C28 C29 117.7(6) . . ? C33 C28 P3 124.5(5) . . ? C29 C28 P3 117.7(6) . . ? C30 C29 C28 121.9(8) . . ? C29 C30 C31 120.1(9) . . ? C30 C31 C32 119.9(10) . . ? C31 C32 C33 120.2(9) . . ? C28 C33 C32 120.1(8) . . ? C39 C34 C35 117.6(7) . . ? C39 C34 P3 124.5(6) . . ? C35 C34 P3 117.9(6) . . ? C36 C35 C34 119.0(9) . . ? C37 C36 C35 123.3(12) . . ? C38 C37 C36 118.3(11) . . ? C37 C38 C39 122.4(12) . . ? C34 C39 C38 119.5(9) . . ? C41 C40 C45 125.2(4) . . ? C41 C40 O2 117.6(4) . . ? C45 C40 O2 117.2(4) . . ? C42 C41 C40 115.2(4) . . ? C42 C41 Pd1 126.3(3) . . ? C40 C41 Pd1 118.1(3) . . ? C41 C42 C43 123.0(4) . . ? C44 C43 C42 117.9(4) . . ? C44 C43 C46 122.0(4) . . ? C42 C43 C46 120.1(4) . . ? C45 C44 C43 123.4(4) . . ? C44 C45 C40 115.3(4) . . ? C44 C45 C50 122.4(4) . . ? C40 C45 C50 122.4(4) . . ? C47 C46 C49 121.7(7) . . ? C47 C46 C43 114.8(6) . . ? C49 C46 C43 114.0(5) . . ? C47 C46 C48 94.3(7) . . ? C49 C46 C48 100.6(6) . . ? C43 C46 C48 106.5(6) . . ? C52 C50 C45 111.1(5) . . ? C52 C50 C53 110.3(5) . . ? C45 C50 C53 109.9(5) . . ? C52 C50 C51 107.1(6) . . ? C45 C50 C51 110.4(4) . . ? C53 C50 C51 107.9(5) . . ? C59 C54 C55 121.9(5) . . ? C59 C54 O3 119.8(4) . . ? C55 C54 O3 118.2(4) . . ? C56 C55 C54 115.0(4) . . ? C56 C55 C60 122.5(4) . . ? C54 C55 C60 122.5(4) . . ? C55 C56 C57 125.1(5) . . ? C58 C57 C56 116.7(5) . . ? C58 C57 C64 121.6(5) . . ? C56 C57 C64 121.6(5) . . ? C57 C58 C59 121.2(5) . . ? C54 C59 C58 120.0(5) . . ? C62 C60 C63 110.2(5) . . ? C62 C60 C61 108.0(5) . . ? C63 C60 C61 106.3(5) . . ? C62 C60 C55 111.4(4) . . ? C63 C60 C55 109.4(4) . . ? C61 C60 C55 111.4(5) . . ? C67 C64 C65 101.3(7) . . ? C67 C64 C66 106.0(7) . . ? C65 C64 C66 115.3(8) . . ? C67 C64 C57 109.2(6) . . ? C65 C64 C57 112.1(6) . . ? C66 C64 C57 112.0(6) . . ? C73 C68 C69 122.0(5) . . ? C73 C68 O4 120.3(4) . . ? C69 C68 O4 117.8(4) . . ? C70 C69 C68 115.1(5) . . ? C70 C69 C78 122.0(5) . . ? C68 C69 C78 122.9(5) . . ? C71 C70 C69 124.8(5) . . ? C70 C71 C72 117.3(5) . . ? C70 C71 C74 120.2(5) . . ? C72 C71 C74 122.5(6) . . ? C73 C72 C71 120.5(5) . . ? C68 C73 C72 120.3(5) . . ? C76 C74 C77 112.1(6) . . ? C76 C74 C71 109.3(6) . . ? C77 C74 C71 111.8(6) . . ? C76 C74 C75 107.1(7) . . ? C77 C74 C75 107.5(6) . . ? C71 C74 C75 108.9(6) . . ? C80 C78 C69 111.3(5) . . ? C80 C78 C81 109.4(6) . . ? C69 C78 C81 111.2(5) . . ? C80 C78 C79 109.3(6) . . ? C69 C78 C79 108.2(5) . . ? C81 C78 C79 107.3(5) . . ? C2 C83 P3 118.4(3) . . ? F4 P5 F6' 130.7(4) . . ? F4 P5 F3 91.92(16) . . ? F6' P5 F3 134.5(4) . . ? F4 P5 F4' 61.3(4) . . ? F6' P5 F4' 91.1(2) . . ? F3 P5 F4' 98.8(5) . . ? F4 P5 F1 89.47(16) . . ? F6' P5 F1 103.1(4) . . ? F3 P5 F1 90.26(17) . . ? F4' P5 F1 149.5(4) . . ? F4 P5 F6 90.87(16) . . ? F6' P5 F6 76.0(5) . . ? F3 P5 F6 90.61(15) . . ? F4' P5 F6 30.6(4) . . ? F1 P5 F6 179.1(2) . . ? F4 P5 F3' 126.7(4) . . ? F6' P5 F3' 90.67(19) . . ? F3 P5 F3' 45.2(4) . . ? F4' P5 F3' 91.12(19) . . ? F1 P5 F3' 115.2(4) . . ? F6 P5 F3' 65.3(4) . . ? F4 P5 F2' 53.3(4) . . ? F6' P5 F2' 90.14(19) . . ? F3 P5 F2' 133.7(4) . . ? F4' P5 F2' 90.07(19) . . ? F1 P5 F2' 63.5(4) . . ? F6 P5 F2' 116.1(4) . . ? F3' P5 F2' 178.6(3) . . ? F4 P5 F5' 117.4(4) . . ? F6' P5 F5' 90.57(19) . . ? F3 P5 F5' 80.0(4) . . ? F4' P5 F5' 178.3(3) . . ? F1 P5 F5' 29.7(4) . . ? F6 P5 F5' 150.3(4) . . ? F3' P5 F5' 88.92(19) . . ? F2' P5 F5' 89.87(18) . . ? F4 P5 F1' 49.2(4) . . ? F6' P5 F1' 179.8(3) . . ? F3 P5 F1' 45.4(4) . . ? F4' P5 F1' 88.65(18) . . ? F1 P5 F1' 77.1(4) . . ? F6 P5 F1' 103.8(4) . . ? F3' P5 F1' 89.25(19) . . ? F2' P5 F1' 89.95(19) . . ? F5' P5 F1' 89.66(19) . . ? F4 P5 F5 178.8(2) . . ? F6' P5 F5 48.5(4) . . ? F3 P5 F5 89.10(16) . . ? F4' P5 F5 119.1(4) . . ? F1 P5 F5 89.90(15) . . ? F6 P5 F5 89.75(16) . . ? F3' P5 F5 54.5(4) . . ? F2' P5 F5 125.5(4) . . ? F5' P5 F5 62.2(4) . . ? F1' P5 F5 131.6(4) . . ? F4 P5 F2 89.88(16) . . ? F6' P5 F2 43.7(4) . . ? F3 P5 F2 178.2(2) . . ? F4' P5 F2 81.8(4) . . ? F1 P5 F2 89.99(15) . . ? F6 P5 F2 89.13(16) . . ? F3' P5 F2 133.2(4) . . ? F2' P5 F2 47.9(4) . . ? F5' P5 F2 99.4(4) . . ? F1' P5 F2 136.4(4) . . ? F5 P5 F2 89.10(15) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 24.55 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.932 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.068 # Attachment '6a.cif' data_6a _database_code_depnum_ccdc_archive 'CCDC 621716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H47 O3 P4 Pd, F6 Sb, C H2 Cl2' _chemical_formula_sum 'C53 H49 Cl2 F6 O3 P3 Pd Sb' _chemical_formula_weight 1239.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7089(13) _cell_length_b 24.953(3) _cell_length_c 16.2793(19) _cell_angle_alpha 90.00 _cell_angle_beta 94.354(10) _cell_angle_gamma 90.00 _cell_volume 5147.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 11893 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2484 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6594 _exptl_absorpt_correction_T_max 0.8047 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 64191 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11807 _reflns_number_gt 9220 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+7.3653P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11807 _refine_ls_number_parameters 631 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0925 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F3 F 0.0834(2) 0.62001(12) 0.31640(16) 0.0691(8) Uani 1 1 d . . . F4 F 0.0607(3) 0.58513(12) 0.4631(2) 0.1038(13) Uani 1 1 d . . . F5 F 0.2309(2) 0.64083(17) 0.4306(3) 0.1133(16) Uani 1 1 d . . . F6 F 0.0889(2) 0.68116(14) 0.52395(16) 0.0784(10) Uani 1 1 d . . . F1 F -0.05720(19) 0.66349(11) 0.4076(2) 0.0680(8) Uani 1 1 d . . . F2 F 0.1057(3) 0.71850(11) 0.3730(2) 0.0892(11) Uani 1 1 d . . . Sb1 Sb 0.088058(17) 0.651528(10) 0.419776(14) 0.02738(7) Uani 1 1 d . . . C1 C 0.3613(2) 0.43641(11) 0.06684(18) 0.0148(6) Uani 1 1 d . . . C2 C 0.3365(2) 0.48182(12) 0.11075(19) 0.0166(6) Uani 1 1 d . . . H2 H 0.3230 0.4785 0.1671 0.020 Uiso 1 1 calc R . . C3 C 0.3310(2) 0.53200(12) 0.0737(2) 0.0212(7) Uani 1 1 d . . . H3 H 0.3137 0.5625 0.1050 0.025 Uiso 1 1 calc R . . C4 C 0.3504(2) 0.53792(12) -0.0080(2) 0.0240(7) Uani 1 1 d . . . H4 H 0.3451 0.5723 -0.0332 0.029 Uiso 1 1 calc R . . C5 C 0.3777(2) 0.49368(12) -0.0535(2) 0.0205(7) Uani 1 1 d . . . H5 H 0.3926 0.4973 -0.1095 0.025 Uiso 1 1 calc R . . C6 C 0.3824(2) 0.44428(12) -0.01500(19) 0.0165(6) Uani 1 1 d . . . C7 C 0.2588(2) 0.30357(12) -0.10826(18) 0.0173(6) Uani 1 1 d . . . C8 C 0.2157(3) 0.34389(13) -0.1577(2) 0.0223(7) Uani 1 1 d . . . H8 H 0.2579 0.3730 -0.1734 0.027 Uiso 1 1 calc R . . C9 C 0.1096(3) 0.34113(14) -0.1840(2) 0.0290(8) Uani 1 1 d . . . H9 H 0.0789 0.3683 -0.2189 0.035 Uiso 1 1 calc R . . C10 C 0.0481(3) 0.29910(15) -0.1600(2) 0.0319(9) Uani 1 1 d . . . H10 H -0.0246 0.2976 -0.1783 0.038 Uiso 1 1 calc R . . C11 C 0.0925(3) 0.25918(15) -0.1092(2) 0.0303(8) Uani 1 1 d . . . H11 H 0.0501 0.2305 -0.0921 0.036 Uiso 1 1 calc R . . C12 C 0.1994(3) 0.26125(13) -0.08345(19) 0.0229(7) Uani 1 1 d . . . H12 H 0.2308 0.2339 -0.0492 0.027 Uiso 1 1 calc R . . C13 C 0.5951(2) 0.31511(12) -0.08800(19) 0.0186(6) Uani 1 1 d . . . C14 C 0.5836(3) 0.34459(13) -0.1599(2) 0.0214(7) Uani 1 1 d . . . H14 H 0.5326 0.3724 -0.1665 0.026 Uiso 1 1 calc R . . C15 C 0.6484(3) 0.33258(14) -0.2226(2) 0.0278(8) Uani 1 1 d . . . H15 H 0.6421 0.3526 -0.2724 0.033 Uiso 1 1 calc R . . C16 C 0.7221(3) 0.29159(14) -0.2132(2) 0.0314(8) Uani 1 1 d . . . H16 H 0.7655 0.2834 -0.2566 0.038 Uiso 1 1 calc R . . C17 C 0.7321(3) 0.26312(14) -0.1413(2) 0.0320(8) Uani 1 1 d . . . H17 H 0.7830 0.2353 -0.1348 0.038 Uiso 1 1 calc R . . C18 C 0.6688(2) 0.27443(13) -0.0777(2) 0.0244(7) Uani 1 1 d . . . H18 H 0.6759 0.2545 -0.0279 0.029 Uiso 1 1 calc R . . C19 C 0.0762(2) 0.38258(11) 0.03955(18) 0.0147(6) Uani 1 1 d . . . C20 C 0.1016(2) 0.42638(12) -0.00773(19) 0.0191(6) Uani 1 1 d . . . H20 H 0.1687 0.4430 0.0016 0.023 Uiso 1 1 calc R . . C21 C 0.0292(2) 0.44603(13) -0.0687(2) 0.0220(7) Uani 1 1 d . . . H21 H 0.0466 0.4762 -0.1005 0.026 Uiso 1 1 calc R . . C22 C -0.0682(2) 0.42161(13) -0.0831(2) 0.0237(7) Uani 1 1 d . . . H22 H -0.1173 0.4349 -0.1251 0.028 Uiso 1 1 calc R . . C23 C -0.0940(2) 0.37800(13) -0.0365(2) 0.0239(7) Uani 1 1 d . . . H23 H -0.1609 0.3613 -0.0465 0.029 Uiso 1 1 calc R . . C24 C -0.0225(2) 0.35843(12) 0.0249(2) 0.0206(7) Uani 1 1 d . . . H24 H -0.0408 0.3286 0.0571 0.025 Uiso 1 1 calc R . . C25 C 0.1220(2) 0.39449(12) 0.21162(18) 0.0162(6) Uani 1 1 d . . . C26 C 0.1057(2) 0.36885(13) 0.28559(19) 0.0192(6) Uani 1 1 d . . . H26 H 0.1153 0.3312 0.2902 0.023 Uiso 1 1 calc R . . C27 C 0.0753(3) 0.39797(14) 0.3528(2) 0.0259(7) Uani 1 1 d . . . H27 H 0.0643 0.3800 0.4029 0.031 Uiso 1 1 calc R . . C28 C 0.0612(3) 0.45279(14) 0.3471(2) 0.0277(8) Uani 1 1 d . . . H28 H 0.0407 0.4726 0.3931 0.033 Uiso 1 1 calc R . . C29 C 0.0773(3) 0.47854(14) 0.2738(2) 0.0261(7) Uani 1 1 d . . . H29 H 0.0680 0.5162 0.2696 0.031 Uiso 1 1 calc R . . C30 C 0.1066(2) 0.44993(13) 0.2068(2) 0.0220(7) Uani 1 1 d . . . H30 H 0.1164 0.4681 0.1567 0.026 Uiso 1 1 calc R . . C31 C 0.1336(2) 0.28887(11) 0.13845(19) 0.0161(6) Uani 1 1 d . . . H31A H 0.0657 0.2871 0.1645 0.019 Uiso 1 1 calc R . . H31B H 0.1240 0.2707 0.0843 0.019 Uiso 1 1 calc R . . C32 C 0.2184(2) 0.25985(12) 0.19271(18) 0.0160(6) Uani 1 1 d . . . H32A H 0.2039 0.2209 0.1907 0.019 Uiso 1 1 calc R . . H32B H 0.2150 0.2718 0.2504 0.019 Uiso 1 1 calc R . . C33 C 0.3879(2) 0.21398(11) 0.10225(18) 0.0156(6) Uani 1 1 d . . . C34 C 0.3148(3) 0.17496(12) 0.0750(2) 0.0216(7) Uani 1 1 d . . . H34 H 0.2434 0.1779 0.0880 0.026 Uiso 1 1 calc R . . C35 C 0.3462(3) 0.13175(13) 0.0288(2) 0.0265(7) Uani 1 1 d . . . H35 H 0.2961 0.1055 0.0097 0.032 Uiso 1 1 calc R . . C36 C 0.4502(3) 0.12697(13) 0.0107(2) 0.0256(7) Uani 1 1 d . . . H36 H 0.4718 0.0970 -0.0200 0.031 Uiso 1 1 calc R . . C37 C 0.5232(3) 0.16571(13) 0.0370(2) 0.0235(7) Uani 1 1 d . . . H37 H 0.5947 0.1625 0.0242 0.028 Uiso 1 1 calc R . . C38 C 0.4920(2) 0.20912(12) 0.08206(19) 0.0189(6) Uani 1 1 d . . . H38 H 0.5420 0.2359 0.0994 0.023 Uiso 1 1 calc R . . C39 C 0.4361(2) 0.26807(11) 0.25701(18) 0.0167(6) Uani 1 1 d . . . H39A H 0.4132 0.2379 0.2909 0.020 Uiso 1 1 calc R . . H39B H 0.5100 0.2614 0.2444 0.020 Uiso 1 1 calc R . . C40 C 0.4296(2) 0.32065(12) 0.30491(18) 0.0182(6) Uani 1 1 d . . . H40A H 0.4807 0.3202 0.3539 0.022 Uiso 1 1 calc R . . H40B H 0.3578 0.3253 0.3236 0.022 Uiso 1 1 calc R . . C41 C 0.4409(2) 0.43733(12) 0.29204(18) 0.0173(6) Uani 1 1 d . . . C42 C 0.3503(2) 0.44435(13) 0.33414(19) 0.0204(7) Uani 1 1 d . . . H42 H 0.3022 0.4155 0.3378 0.024 Uiso 1 1 calc R . . C43 C 0.3298(3) 0.49285(14) 0.3705(2) 0.0268(7) Uani 1 1 d . . . H43 H 0.2684 0.4970 0.3998 0.032 Uiso 1 1 calc R . . C44 C 0.3982(3) 0.53521(14) 0.3645(2) 0.0327(8) Uani 1 1 d . . . H44 H 0.3839 0.5686 0.3894 0.039 Uiso 1 1 calc R . . C45 C 0.4879(3) 0.52906(14) 0.3221(2) 0.0322(8) Uani 1 1 d . . . H45 H 0.5348 0.5584 0.3176 0.039 Uiso 1 1 calc R . . C46 C 0.5095(3) 0.48057(13) 0.2862(2) 0.0234(7) Uani 1 1 d . . . H46 H 0.5713 0.4766 0.2574 0.028 Uiso 1 1 calc R . . C47 C 0.6033(2) 0.36941(12) 0.23561(19) 0.0178(6) Uani 1 1 d . . . C48 C 0.6704(2) 0.38035(13) 0.3056(2) 0.0249(7) Uani 1 1 d . . . H48 H 0.6418 0.3926 0.3545 0.030 Uiso 1 1 calc R . . C49 C 0.7780(3) 0.37342(14) 0.3040(2) 0.0311(8) Uani 1 1 d . . . H49 H 0.8234 0.3818 0.3513 0.037 Uiso 1 1 calc R . . C50 C 0.8199(3) 0.35439(16) 0.2340(3) 0.0363(9) Uani 1 1 d . . . H50 H 0.8940 0.3499 0.2332 0.044 Uiso 1 1 calc R . . C51 C 0.7547(3) 0.34177(17) 0.1652(2) 0.0359(9) Uani 1 1 d . . . H51 H 0.7836 0.3274 0.1177 0.043 Uiso 1 1 calc R . . C52 C 0.6462(3) 0.35020(14) 0.1655(2) 0.0252(7) Uani 1 1 d . . . H52 H 0.6015 0.3427 0.1175 0.030 Uiso 1 1 calc R . . O1 O 0.40854(16) 0.40039(8) -0.06356(12) 0.0177(4) Uani 1 1 d . . . O2 O 0.36770(16) 0.30350(8) -0.08494(12) 0.0174(4) Uani 1 1 d . . . O3 O 0.53796(16) 0.32623(8) -0.01945(12) 0.0184(4) Uani 1 1 d . . . P1 P 0.41786(6) 0.34390(3) -0.01566(5) 0.01371(15) Uani 1 1 d . . . P2 P 0.16916(6) 0.35937(3) 0.12300(5) 0.01314(15) Uani 1 1 d . . . P3 P 0.35150(6) 0.27188(3) 0.16111(5) 0.01338(15) Uani 1 1 d . . . P4 P 0.46048(6) 0.37592(3) 0.23567(5) 0.01482(16) Uani 1 1 d . . . Pd1 Pd 0.357838(16) 0.358232(8) 0.109628(13) 0.01143(6) Uani 1 1 d . . . C53 C 0.1701(4) 0.45386(18) 0.6554(3) 0.0523(12) Uani 1 1 d . . . H53A H 0.2039 0.4186 0.6483 0.063 Uiso 1 1 calc R . . H53B H 0.0927 0.4485 0.6513 0.063 Uiso 1 1 calc R . . Cl1 Cl 0.20358(12) 0.49682(5) 0.57738(7) 0.0642(3) Uani 1 1 d . . . Cl2 Cl 0.21056(8) 0.47963(4) 0.75370(6) 0.0440(2) Uani 1 1 d . . . 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 F3 0.086(2) 0.0742(19) 0.0436(16) -0.0264(14) -0.0159(14) 0.0241(16) F4 0.148(3) 0.0565(19) 0.114(3) 0.046(2) 0.053(3) 0.037(2) F5 0.0222(14) 0.182(4) 0.133(3) -0.086(3) -0.0170(16) 0.0304(18) F6 0.081(2) 0.117(3) 0.0361(15) -0.0321(16) -0.0047(14) 0.0321(19) F1 0.0260(13) 0.0616(17) 0.115(3) -0.0064(17) -0.0046(14) 0.0145(12) F2 0.123(3) 0.0462(16) 0.108(3) 0.0045(17) 0.072(2) -0.0197(17) Sb1 0.01922(12) 0.03835(14) 0.02460(13) -0.00250(10) 0.00185(9) 0.00248(9) C1 0.0129(14) 0.0150(14) 0.0164(15) 0.0015(12) -0.0002(11) -0.0025(11) C2 0.0141(14) 0.0165(15) 0.0188(15) 0.0006(12) -0.0007(12) 0.0002(11) C3 0.0156(15) 0.0133(15) 0.0342(19) -0.0034(14) -0.0011(13) 0.0009(12) C4 0.0214(16) 0.0147(15) 0.035(2) 0.0083(14) -0.0034(14) 0.0000(13) C5 0.0167(15) 0.0214(16) 0.0228(17) 0.0093(13) -0.0014(12) -0.0022(12) C6 0.0133(14) 0.0166(15) 0.0195(16) -0.0003(12) 0.0007(12) 0.0001(11) C7 0.0169(15) 0.0206(15) 0.0145(15) -0.0070(12) 0.0012(11) 0.0010(12) C8 0.0265(17) 0.0214(16) 0.0186(16) -0.0034(13) -0.0013(13) 0.0012(13) C9 0.0292(18) 0.0310(19) 0.0254(18) -0.0101(15) -0.0061(14) 0.0085(15) C10 0.0201(17) 0.047(2) 0.029(2) -0.0196(17) 0.0001(14) 0.0041(16) C11 0.0284(18) 0.041(2) 0.0233(18) -0.0151(16) 0.0120(14) -0.0123(16) C12 0.0283(17) 0.0247(17) 0.0162(16) -0.0037(13) 0.0053(13) -0.0025(14) C13 0.0192(15) 0.0183(15) 0.0188(16) -0.0062(13) 0.0042(12) -0.0054(12) C14 0.0217(16) 0.0210(16) 0.0220(17) -0.0045(13) 0.0047(13) -0.0037(13) C15 0.0323(19) 0.0310(19) 0.0213(18) -0.0034(15) 0.0096(14) -0.0111(15) C16 0.0285(19) 0.034(2) 0.033(2) -0.0135(17) 0.0166(15) -0.0090(16) C17 0.0275(18) 0.0256(18) 0.045(2) -0.0101(17) 0.0155(16) -0.0007(15) C18 0.0225(16) 0.0217(16) 0.0297(18) -0.0020(14) 0.0067(14) -0.0008(13) C19 0.0151(14) 0.0158(14) 0.0130(14) -0.0006(12) 0.0012(11) 0.0030(11) C20 0.0167(15) 0.0223(16) 0.0182(16) 0.0004(13) 0.0010(12) 0.0012(12) C21 0.0213(16) 0.0220(16) 0.0230(17) 0.0054(14) 0.0033(13) 0.0021(13) C22 0.0196(16) 0.0294(18) 0.0212(17) 0.0022(14) -0.0042(13) 0.0074(13) C23 0.0146(15) 0.0279(17) 0.0284(18) -0.0024(15) -0.0036(13) -0.0013(13) C24 0.0179(15) 0.0202(16) 0.0235(17) 0.0028(13) 0.0014(12) -0.0013(12) C25 0.0102(13) 0.0211(15) 0.0174(15) -0.0022(12) 0.0013(11) 0.0003(11) C26 0.0154(14) 0.0226(16) 0.0200(16) 0.0014(13) 0.0029(12) -0.0017(12) C27 0.0217(17) 0.0356(19) 0.0210(17) 0.0007(15) 0.0049(13) -0.0006(14) C28 0.0240(17) 0.035(2) 0.0242(18) -0.0094(15) 0.0043(14) 0.0045(15) C29 0.0254(17) 0.0241(17) 0.0287(19) -0.0034(15) 0.0014(14) 0.0068(14) C30 0.0181(15) 0.0231(16) 0.0247(17) 0.0022(14) 0.0018(13) 0.0028(13) C31 0.0152(14) 0.0138(14) 0.0192(16) 0.0014(12) 0.0016(12) -0.0018(11) C32 0.0158(14) 0.0161(15) 0.0165(15) 0.0021(12) 0.0040(11) -0.0007(12) C33 0.0207(15) 0.0128(14) 0.0131(14) 0.0022(12) -0.0006(11) 0.0005(12) C34 0.0238(16) 0.0189(16) 0.0219(17) 0.0020(14) 0.0006(13) -0.0029(13) C35 0.039(2) 0.0157(16) 0.0244(18) -0.0009(14) -0.0011(15) -0.0041(14) C36 0.042(2) 0.0179(16) 0.0166(16) -0.0009(13) 0.0007(14) 0.0085(15) C37 0.0266(17) 0.0250(17) 0.0195(17) 0.0029(14) 0.0051(13) 0.0098(14) C38 0.0208(15) 0.0182(15) 0.0177(16) 0.0017(13) 0.0012(12) -0.0003(12) C39 0.0194(15) 0.0144(14) 0.0163(15) 0.0021(12) 0.0002(12) 0.0021(12) C40 0.0228(16) 0.0191(15) 0.0130(15) 0.0015(12) 0.0027(12) -0.0006(12) C41 0.0199(15) 0.0169(15) 0.0142(15) -0.0047(12) -0.0045(12) -0.0004(12) C42 0.0204(16) 0.0220(16) 0.0185(16) -0.0017(13) 0.0001(12) -0.0006(13) C43 0.0247(17) 0.0317(19) 0.0238(17) -0.0056(15) 0.0001(13) 0.0051(14) C44 0.036(2) 0.0250(18) 0.036(2) -0.0120(16) -0.0055(16) 0.0035(16) C45 0.0316(19) 0.0208(17) 0.043(2) -0.0063(16) -0.0029(16) -0.0064(15) C46 0.0224(16) 0.0218(16) 0.0256(18) -0.0003(14) -0.0005(13) -0.0026(13) C47 0.0176(15) 0.0177(15) 0.0177(15) 0.0045(12) -0.0009(12) -0.0013(12) C48 0.0219(16) 0.0269(17) 0.0252(18) -0.0013(14) -0.0027(13) 0.0027(14) C49 0.0220(17) 0.034(2) 0.035(2) 0.0023(16) -0.0114(15) -0.0008(15) C50 0.0162(17) 0.050(2) 0.042(2) 0.0073(19) -0.0011(15) -0.0019(16) C51 0.0184(17) 0.060(3) 0.030(2) 0.0028(18) 0.0069(15) 0.0044(17) C52 0.0178(16) 0.039(2) 0.0184(16) 0.0037(15) 0.0002(13) -0.0016(14) O1 0.0229(11) 0.0161(10) 0.0143(11) 0.0030(9) 0.0032(8) -0.0002(9) O2 0.0178(10) 0.0185(10) 0.0156(11) -0.0047(9) -0.0002(8) 0.0015(8) O3 0.0173(10) 0.0246(11) 0.0135(10) -0.0020(9) 0.0025(8) 0.0028(9) P1 0.0141(4) 0.0151(4) 0.0121(4) -0.0005(3) 0.0021(3) 0.0001(3) P2 0.0123(3) 0.0143(4) 0.0129(4) 0.0015(3) 0.0015(3) 0.0005(3) P3 0.0144(4) 0.0118(4) 0.0140(4) 0.0015(3) 0.0019(3) 0.0008(3) P4 0.0148(4) 0.0154(4) 0.0141(4) -0.0005(3) 0.0001(3) -0.0005(3) Pd1 0.01193(11) 0.01097(11) 0.01149(11) 0.00068(8) 0.00150(8) 0.00014(8) C53 0.056(3) 0.043(2) 0.060(3) -0.004(2) 0.012(2) -0.001(2) Cl1 0.1029(10) 0.0510(7) 0.0391(6) 0.0025(5) 0.0084(6) 0.0122(7) Cl2 0.0427(5) 0.0477(6) 0.0411(6) 0.0094(5) -0.0003(4) -0.0083(5) _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 F3 Sb1 1.854(2) . ? F4 Sb1 1.844(3) . ? F5 Sb1 1.830(3) . ? F6 Sb1 1.849(3) . ? F1 Sb1 1.866(2) . ? F2 Sb1 1.857(3) . ? C1 C2 1.389(4) . ? C1 C6 1.393(4) . ? C1 Pd1 2.073(3) . ? C2 C3 1.389(4) . ? C2 H2 0.9500 . ? C3 C4 1.380(5) . ? C3 H3 0.9500 . ? C4 C5 1.388(5) . ? C4 H4 0.9500 . ? C5 C6 1.382(4) . ? C5 H5 0.9500 . ? C6 O1 1.405(4) . ? C7 C8 1.376(4) . ? C7 C12 1.377(4) . ? C7 O2 1.406(3) . ? C8 C9 1.386(5) . ? C8 H8 0.9500 . ? C9 C10 1.382(5) . ? C9 H9 0.9500 . ? C10 C11 1.387(5) . ? C10 H10 0.9500 . ? C11 C12 1.392(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.381(4) . ? C13 C18 1.382(4) . ? C13 O3 1.405(3) . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C15 C16 1.388(5) . ? C15 H15 0.9500 . ? C16 C17 1.367(5) . ? C16 H16 0.9500 . ? C17 C18 1.388(5) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.389(4) . ? C19 C24 1.396(4) . ? C19 P2 1.826(3) . ? C20 C21 1.390(4) . ? C20 H20 0.9500 . ? C21 C22 1.383(4) . ? C21 H21 0.9500 . ? C22 C23 1.380(5) . ? C22 H22 0.9500 . ? C23 C24 1.388(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.393(4) . ? C25 C30 1.399(4) . ? C25 P2 1.827(3) . ? C26 C27 1.392(5) . ? C26 H26 0.9500 . ? C27 C28 1.382(5) . ? C27 H27 0.9500 . ? C28 C29 1.385(5) . ? C28 H28 0.9500 . ? C29 C30 1.378(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.524(4) . ? C31 P2 1.839(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 P3 1.829(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C38 1.393(4) . ? C33 C34 1.395(4) . ? C33 P3 1.813(3) . ? C34 C35 1.390(5) . ? C34 H34 0.9500 . ? C35 C36 1.382(5) . ? C35 H35 0.9500 . ? C36 C37 1.385(5) . ? C36 H36 0.9500 . ? C37 C38 1.383(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.532(4) . ? C39 P3 1.830(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 P4 1.842(3) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.395(4) . ? C41 C46 1.395(4) . ? C41 P4 1.813(3) . ? C42 C43 1.381(4) . ? C42 H42 0.9500 . ? C43 C44 1.377(5) . ? C43 H43 0.9500 . ? C44 C45 1.385(5) . ? C44 H44 0.9500 . ? C45 C46 1.380(5) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.387(5) . ? C47 C48 1.397(4) . ? C47 P4 1.822(3) . ? C48 C49 1.381(5) . ? C48 H48 0.9500 . ? C49 C50 1.377(5) . ? C49 H49 0.9500 . ? C50 C51 1.378(5) . ? C50 H50 0.9500 . ? C51 C52 1.395(5) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? O1 P1 1.611(2) . ? O2 P1 1.608(2) . ? O3 P1 1.594(2) . ? P1 Pd1 2.2597(8) . ? P2 Pd1 2.4243(8) . ? P3 Pd1 2.3156(8) . ? P4 Pd1 2.3876(8) . ? C53 Cl1 1.739(5) . ? C53 Cl2 1.764(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? 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 F5 Sb1 F4 92.7(2) . . ? F5 Sb1 F6 91.93(15) . . ? F4 Sb1 F6 89.82(17) . . ? F5 Sb1 F3 89.34(14) . . ? F4 Sb1 F3 88.39(16) . . ? F6 Sb1 F3 177.86(16) . . ? F5 Sb1 F2 91.20(19) . . ? F4 Sb1 F2 175.91(18) . . ? F6 Sb1 F2 91.37(16) . . ? F3 Sb1 F2 90.33(15) . . ? F5 Sb1 F1 179.01(19) . . ? F4 Sb1 F1 88.30(16) . . ? F6 Sb1 F1 88.26(14) . . ? F3 Sb1 F1 90.51(14) . . ? F2 Sb1 F1 87.82(15) . . ? C2 C1 C6 116.4(3) . . ? C2 C1 Pd1 125.7(2) . . ? C6 C1 Pd1 117.7(2) . . ? C1 C2 C3 121.2(3) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C4 C3 C2 120.5(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 118.2(3) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C5 C6 C1 123.7(3) . . ? C5 C6 O1 116.4(3) . . ? C1 C6 O1 119.9(3) . . ? C8 C7 C12 122.0(3) . . ? C8 C7 O2 119.9(3) . . ? C12 C7 O2 118.1(3) . . ? C7 C8 C9 118.7(3) . . ? C7 C8 H8 120.7 . . ? C9 C8 H8 120.7 . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.0(3) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 119.8(3) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 119.0(3) . . ? C7 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C18 121.4(3) . . ? C14 C13 O3 122.7(3) . . ? C18 C13 O3 115.8(3) . . ? C13 C14 C15 118.4(3) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 119.7(3) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.8(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C13 C18 C17 119.0(3) . . ? C13 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C20 C19 C24 119.3(3) . . ? C20 C19 P2 119.8(2) . . ? C24 C19 P2 120.8(2) . . ? C19 C20 C21 120.3(3) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 120.0(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.1(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.2(3) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C23 C24 C19 120.1(3) . . ? C23 C24 H24 119.9 . . ? C19 C24 H24 119.9 . . ? C26 C25 C30 118.2(3) . . ? C26 C25 P2 122.8(2) . . ? C30 C25 P2 118.9(2) . . ? C27 C26 C25 120.5(3) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C26 120.4(3) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 119.3(3) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 120.5(3) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C25 120.9(3) . . ? C29 C30 H30 119.6 . . ? C25 C30 H30 119.6 . . ? C32 C31 P2 111.3(2) . . ? C32 C31 H31A 109.4 . . ? P2 C31 H31A 109.4 . . ? C32 C31 H31B 109.4 . . ? P2 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 P3 112.8(2) . . ? C31 C32 H32A 109.0 . . ? P3 C32 H32A 109.0 . . ? C31 C32 H32B 109.0 . . ? P3 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C38 C33 C34 119.1(3) . . ? C38 C33 P3 118.6(2) . . ? C34 C33 P3 122.3(2) . . ? C35 C34 C33 120.1(3) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 120.1(3) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.2(3) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C36 119.9(3) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C33 120.6(3) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? C40 C39 P3 109.8(2) . . ? C40 C39 H39A 109.7 . . ? P3 C39 H39A 109.7 . . ? C40 C39 H39B 109.7 . . ? P3 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? C39 C40 P4 107.9(2) . . ? C39 C40 H40A 110.1 . . ? P4 C40 H40A 110.1 . . ? C39 C40 H40B 110.1 . . ? P4 C40 H40B 110.1 . . ? H40A C40 H40B 108.4 . . ? C42 C41 C46 118.7(3) . . ? C42 C41 P4 120.4(2) . . ? C46 C41 P4 120.6(2) . . ? C43 C42 C41 120.7(3) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 120.1(3) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 119.9(3) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.3(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 120.3(3) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? C52 C47 C48 119.0(3) . . ? C52 C47 P4 119.0(2) . . ? C48 C47 P4 121.9(2) . . ? C49 C48 C47 120.3(3) . . ? C49 C48 H48 119.9 . . ? C47 C48 H48 119.9 . . ? C50 C49 C48 120.3(3) . . ? C50 C49 H49 119.9 . . ? C48 C49 H49 119.9 . . ? C49 C50 C51 120.4(3) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C50 C51 C52 119.7(3) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C47 C52 C51 120.4(3) . . ? C47 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C6 O1 P1 114.94(18) . . ? C7 O2 P1 121.19(18) . . ? C13 O3 P1 129.79(19) . . ? O3 P1 O2 97.43(11) . . ? O3 P1 O1 104.99(11) . . ? O2 P1 O1 101.44(11) . . ? O3 P1 Pd1 117.94(8) . . ? O2 P1 Pd1 126.11(8) . . ? O1 P1 Pd1 106.31(8) . . ? C19 P2 C25 101.70(13) . . ? C19 P2 C31 104.66(13) . . ? C25 P2 C31 104.60(14) . . ? C19 P2 Pd1 121.71(10) . . ? C25 P2 Pd1 117.53(9) . . ? C31 P2 Pd1 104.86(9) . . ? C33 P3 C32 107.23(14) . . ? C33 P3 C39 104.63(13) . . ? C32 P3 C39 104.32(14) . . ? C33 P3 Pd1 122.21(10) . . ? C32 P3 Pd1 108.23(10) . . ? C39 P3 Pd1 108.84(10) . . ? C41 P4 C47 104.53(14) . . ? C41 P4 C40 106.21(14) . . ? C47 P4 C40 101.08(14) . . ? C41 P4 Pd1 120.27(10) . . ? C47 P4 Pd1 117.53(10) . . ? C40 P4 Pd1 105.04(10) . . ? C1 Pd1 P1 80.12(8) . . ? C1 Pd1 P3 178.18(8) . . ? P1 Pd1 P3 101.70(3) . . ? C1 Pd1 P4 95.19(8) . . ? P1 Pd1 P4 127.24(3) . . ? P3 Pd1 P4 83.84(3) . . ? C1 Pd1 P2 93.77(8) . . ? P1 Pd1 P2 119.14(3) . . ? P3 Pd1 P2 85.21(3) . . ? P4 Pd1 P2 113.59(3) . . ? Cl1 C53 Cl2 111.5(2) . . ? Cl1 C53 H53A 109.3 . . ? Cl2 C53 H53A 109.3 . . ? Cl1 C53 H53B 109.3 . . ? Cl2 C53 H53B 109.3 . . ? H53A C53 H53B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.236 _refine_diff_density_min -1.361 _refine_diff_density_rms 0.108 # Attachment '04src10901.cif' data_04src1090 _database_code_depnum_ccdc_archive 'CCDC 624071' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H55 Cl2 F6 O3 P5 Pd' _chemical_formula_weight 1270.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.294(2) _cell_length_b 15.290(3) _cell_length_c 18.798(5) _cell_angle_alpha 105.391(15) _cell_angle_beta 93.38(2) _cell_angle_gamma 94.90(2) _cell_volume 2832.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12663 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Slab _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.628 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8846 _exptl_absorpt_correction_T_max 0.9753 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58599 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12985 _reflns_number_gt 10693 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+5.4247P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12985 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1191 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8304(3) 0.20482(19) 0.63383(15) 0.0235(6) Uani 1 1 d . . . C2 C 0.7095(3) 0.1809(2) 0.65738(17) 0.0264(6) Uani 1 1 d . . . H2 H 0.6991 0.1958 0.7090 0.032 Uiso 1 1 calc R . . C3 C 0.6039(3) 0.1360(2) 0.60801(17) 0.0286(6) Uani 1 1 d . . . H3 H 0.5243 0.1192 0.6264 0.034 Uiso 1 1 calc R . . C4 C 0.6132(3) 0.1155(2) 0.53219(18) 0.0309(7) Uani 1 1 d . . . H4 H 0.5399 0.0862 0.4987 0.037 Uiso 1 1 calc R . . C5 C 0.7304(3) 0.1381(2) 0.50592(17) 0.0311(7) Uani 1 1 d . . . H5 H 0.7392 0.1250 0.4542 0.037 Uiso 1 1 calc R . . C6 C 0.8348(3) 0.1804(2) 0.55678(16) 0.0268(6) Uani 1 1 d . . . C7 C 0.9941(3) 0.4071(2) 0.57041(17) 0.0265(6) Uani 1 1 d . . . C8 C 0.9888(4) 0.4736(2) 0.63577(19) 0.0353(7) Uani 1 1 d . . . H8 H 1.0480 0.4779 0.6776 0.042 Uiso 1 1 calc R . . C9 C 0.8947(4) 0.5342(2) 0.6390(2) 0.0474(10) Uani 1 1 d . . . H9 H 0.8886 0.5805 0.6834 0.057 Uiso 1 1 calc R . . C10 C 0.8101(4) 0.5269(3) 0.5776(3) 0.0518(11) Uani 1 1 d . . . H10 H 0.7470 0.5692 0.5797 0.062 Uiso 1 1 calc R . . C11 C 0.8160(4) 0.4594(3) 0.5135(3) 0.0508(10) Uani 1 1 d . . . H11 H 0.7563 0.4548 0.4719 0.061 Uiso 1 1 calc R . . C12 C 0.9082(4) 0.3982(3) 0.5092(2) 0.0376(8) Uani 1 1 d . . . H12 H 0.9124 0.3511 0.4651 0.045 Uiso 1 1 calc R . . C13 C 1.2461(3) 0.1907(2) 0.49266(16) 0.0273(6) Uani 1 1 d . . . C14 C 1.2396(4) 0.1019(2) 0.44997(19) 0.0357(8) Uani 1 1 d . . . H14 H 1.1949 0.0535 0.4648 0.043 Uiso 1 1 calc R . . C15 C 1.3011(4) 0.0852(3) 0.38393(19) 0.0434(9) Uani 1 1 d . . . H15 H 1.2985 0.0244 0.3535 0.052 Uiso 1 1 calc R . . C16 C 1.3648(4) 0.1549(3) 0.3626(2) 0.0430(9) Uani 1 1 d . . . H16 H 1.4045 0.1426 0.3172 0.052 Uiso 1 1 calc R . . C17 C 1.3715(4) 0.2433(3) 0.40714(19) 0.0392(8) Uani 1 1 d . . . H17 H 1.4172 0.2914 0.3925 0.047 Uiso 1 1 calc R . . C18 C 1.3120(3) 0.2621(2) 0.47321(18) 0.0325(7) Uani 1 1 d . . . H18 H 1.3166 0.3227 0.5042 0.039 Uiso 1 1 calc R . . C19 C 0.7841(3) 0.3479(2) 0.82407(16) 0.0264(6) Uani 1 1 d . . . C20 C 0.7790(4) 0.4127(2) 0.78418(19) 0.0361(8) Uani 1 1 d . . . H20 H 0.8379 0.4135 0.7472 0.043 Uiso 1 1 calc R . . C21 C 0.6888(4) 0.4760(2) 0.7982(2) 0.0431(9) Uani 1 1 d . . . H21 H 0.6861 0.5201 0.7710 0.052 Uiso 1 1 calc R . . C22 C 0.6029(4) 0.4751(2) 0.8513(2) 0.0400(9) Uani 1 1 d . . . H22 H 0.5414 0.5189 0.8610 0.048 Uiso 1 1 calc R . . C23 C 0.6059(3) 0.4109(2) 0.89060(19) 0.0353(8) Uani 1 1 d . . . H23 H 0.5460 0.4102 0.9271 0.042 Uiso 1 1 calc R . . C24 C 0.6962(3) 0.3470(2) 0.87707(18) 0.0302(7) Uani 1 1 d . . . H24 H 0.6976 0.3027 0.9042 0.036 Uiso 1 1 calc R . . C25 C 0.8770(3) 0.1755(2) 0.83914(16) 0.0249(6) Uani 1 1 d . . . C26 C 0.8489(3) 0.1761(2) 0.91133(17) 0.0304(7) Uani 1 1 d . . . H26 H 0.8521 0.2325 0.9484 0.037 Uiso 1 1 calc R . . C27 C 0.8164(3) 0.0950(2) 0.92903(19) 0.0367(8) Uani 1 1 d . . . H27 H 0.7953 0.0960 0.9778 0.044 Uiso 1 1 calc R . . C28 C 0.8146(4) 0.0123(2) 0.8758(2) 0.0385(8) Uani 1 1 d . . . H28 H 0.7931 -0.0432 0.8882 0.046 Uiso 1 1 calc R . . C29 C 0.8443(4) 0.0106(2) 0.8045(2) 0.0356(7) Uani 1 1 d . . . H29 H 0.8437 -0.0461 0.7681 0.043 Uiso 1 1 calc R . . C30 C 0.8750(3) 0.0917(2) 0.78609(17) 0.0282(6) Uani 1 1 d . . . H30 H 0.8947 0.0902 0.7371 0.034 Uiso 1 1 calc R . . C31 C 1.0284(3) 0.35499(19) 0.89277(15) 0.0241(6) Uani 1 1 d . . . H31A H 1.0306 0.4176 0.8871 0.029 Uiso 1 1 calc R . . H31B H 0.9836 0.3551 0.9380 0.029 Uiso 1 1 calc R . . C32 C 1.1707(3) 0.33800(19) 0.90857(15) 0.0235(6) Uani 1 1 d . . . C33 C 1.2570(3) 0.35783(19) 0.84950(15) 0.0245(6) Uani 1 1 d . . . H33A H 1.3479 0.3496 0.8647 0.029 Uiso 1 1 calc R . . H33B H 1.2556 0.4233 0.8521 0.029 Uiso 1 1 calc R . . C34 C 1.3315(3) 0.3610(2) 0.70798(16) 0.0255(6) Uani 1 1 d . . . C35 C 1.3116(3) 0.4524(2) 0.71597(17) 0.0293(7) Uani 1 1 d . . . H35 H 1.2466 0.4790 0.7461 0.035 Uiso 1 1 calc R . . C36 C 1.3863(4) 0.5040(2) 0.68013(19) 0.0364(8) Uani 1 1 d . . . H36 H 1.3714 0.5656 0.6850 0.044 Uiso 1 1 calc R . . C37 C 1.4828(4) 0.4665(3) 0.6372(2) 0.0406(8) Uani 1 1 d . . . H37 H 1.5339 0.5024 0.6128 0.049 Uiso 1 1 calc R . . C38 C 1.5046(4) 0.3769(3) 0.6300(2) 0.0398(8) Uani 1 1 d . . . H38 H 1.5719 0.3514 0.6013 0.048 Uiso 1 1 calc R . . C39 C 1.4285(3) 0.3239(2) 0.66463(18) 0.0317(7) Uani 1 1 d . . . H39 H 1.4428 0.2619 0.6586 0.038 Uiso 1 1 calc R . . C40 C 1.2922(3) 0.1862(2) 0.74170(16) 0.0258(6) Uani 1 1 d . . . C41 C 1.4185(3) 0.1837(2) 0.77183(17) 0.0298(7) Uani 1 1 d . . . H41 H 1.4712 0.2389 0.7960 0.036 Uiso 1 1 calc R . . C42 C 1.4676(3) 0.1003(2) 0.76660(19) 0.0349(7) Uani 1 1 d . . . H42 H 1.5537 0.0987 0.7872 0.042 Uiso 1 1 calc R . . C43 C 1.3912(4) 0.0200(2) 0.73153(19) 0.0373(8) Uani 1 1 d . . . H43 H 1.4249 -0.0368 0.7281 0.045 Uiso 1 1 calc R . . C44 C 1.2663(4) 0.0216(2) 0.70142(19) 0.0355(8) Uani 1 1 d . . . H44 H 1.2141 -0.0338 0.6773 0.043 Uiso 1 1 calc R . . C45 C 1.2171(3) 0.1046(2) 0.70648(17) 0.0292(7) Uani 1 1 d . . . H45 H 1.1310 0.1055 0.6856 0.035 Uiso 1 1 calc R . . C46 C 1.2220(3) 0.4085(2) 0.98181(16) 0.0302(7) Uani 1 1 d . . . H46A H 1.3148 0.4032 0.9928 0.045 Uiso 1 1 calc R . . H46B H 1.1722 0.3973 1.0219 0.045 Uiso 1 1 calc R . . H46C H 1.2117 0.4701 0.9774 0.045 Uiso 1 1 calc R . . C47 C 1.1777(3) 0.24080(19) 0.91648(16) 0.0237(6) Uani 1 1 d . . . H47A H 1.1539 0.1969 0.8673 0.028 Uiso 1 1 calc R . . H47B H 1.1115 0.2290 0.9499 0.028 Uiso 1 1 calc R . . C48 C 1.3232(3) 0.0935(2) 0.92541(16) 0.0270(6) Uani 1 1 d . . . C49 C 1.2060(3) 0.0377(2) 0.90425(18) 0.0305(7) Uani 1 1 d . . . H49 H 1.1257 0.0642 0.9047 0.037 Uiso 1 1 calc R . . C50 C 1.2054(4) -0.0565(2) 0.88241(19) 0.0359(7) Uani 1 1 d . . . H50 H 1.1248 -0.0941 0.8682 0.043 Uiso 1 1 calc R . . C51 C 1.3217(4) -0.0956(2) 0.88127(19) 0.0358(8) Uani 1 1 d . . . H51 H 1.3210 -0.1601 0.8658 0.043 Uiso 1 1 calc R . . C52 C 1.4386(4) -0.0413(2) 0.90262(19) 0.0363(8) Uani 1 1 d . . . H52 H 1.5184 -0.0683 0.9025 0.044 Uiso 1 1 calc R . . C53 C 1.4400(3) 0.0527(2) 0.92432(18) 0.0329(7) Uani 1 1 d . . . H53 H 1.5210 0.0899 0.9386 0.039 Uiso 1 1 calc R . . C54 C 1.3268(4) 0.2399(2) 1.05332(18) 0.0357(8) Uani 1 1 d . . . C55 C 1.2147(5) 0.2248(3) 1.0865(2) 0.0517(10) Uani 1 1 d . . . H55 H 1.1343 0.2039 1.0569 0.062 Uiso 1 1 calc R . . C56 C 1.2176(6) 0.2399(3) 1.1631(2) 0.0654(14) Uani 1 1 d . . . H56 H 1.1391 0.2295 1.1851 0.078 Uiso 1 1 calc R . . C57 C 1.3308(7) 0.2690(3) 1.2064(2) 0.0728(18) Uani 1 1 d . . . H57 H 1.3318 0.2787 1.2585 0.087 Uiso 1 1 calc R . . C58 C 1.4444(7) 0.2845(3) 1.1746(3) 0.0755(18) Uani 1 1 d . . . H58 H 1.5241 0.3050 1.2050 0.091 Uiso 1 1 calc R . . C59 C 1.4437(5) 0.2703(3) 1.0977(2) 0.0510(11) Uani 1 1 d . . . H59 H 1.5224 0.2814 1.0760 0.061 Uiso 1 1 calc R . . C60 C 0.1371(5) 0.7535(4) 0.7040(2) 0.0590(12) Uani 1 1 d . . . H60A H 0.1535 0.7884 0.7568 0.071 Uiso 1 1 calc R . . H60B H 0.1101 0.6891 0.7022 0.071 Uiso 1 1 calc R . . O1 O 0.9525(2) 0.19928(16) 0.52574(11) 0.0315(5) Uani 1 1 d . . . O2 O 1.0942(2) 0.34854(14) 0.56472(11) 0.0265(4) Uani 1 1 d . . . O3 O 1.1925(2) 0.20645(14) 0.56173(11) 0.0285(5) Uani 1 1 d . . . F1 F 0.2365(8) 0.7254(3) 0.9321(3) 0.191(3) Uani 1 1 d . . . F2 F 0.2551(5) 0.5866(3) 0.8996(2) 0.1409(19) Uani 1 1 d . . . F3 F 0.2384(3) 0.65504(18) 0.81110(14) 0.0736(9) Uani 1 1 d . . . F4 F 0.0884(4) 0.5449(3) 0.82215(19) 0.1144(14) Uani 1 1 d . . . F5 F 0.0878(6) 0.7284(4) 0.8702(4) 0.096(3) Uani 0.634(9) 1 d P . . F5' F 0.0023(7) 0.6454(7) 0.8106(5) 0.071(4) Uani 0.366(9) 1 d P . . F6 F 0.0510(5) 0.6278(2) 0.93320(18) 0.1323(19) Uani 1 1 d . . . P1 P 1.06696(8) 0.25455(5) 0.58559(4) 0.02385(16) Uani 1 1 d . . . P2 P 0.92248(8) 0.28038(5) 0.81410(4) 0.02161(15) Uani 1 1 d . . . P3 P 1.22298(8) 0.29387(5) 0.75177(4) 0.02215(16) Uani 1 1 d . . . P4 P 1.33907(8) 0.21852(5) 0.95275(4) 0.02863(18) Uani 1 1 d . . . P5 P 0.1423(2) 0.64132(8) 0.87198(7) 0.0802(5) Uani 1 1 d . . . Pd1 Pd 1.00666(2) 0.259916(14) 0.698281(11) 0.02113(7) Uani 1 1 d . . . Cl1 Cl 0.28211(11) 0.75891(7) 0.66091(6) 0.0505(2) Uani 1 1 d . . . Cl2 Cl 0.00886(11) 0.79689(8) 0.66276(6) 0.0554(3) Uani 1 1 d . . . 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 C1 0.0327(16) 0.0187(13) 0.0183(13) 0.0048(11) -0.0018(11) 0.0024(12) C2 0.0318(16) 0.0252(14) 0.0207(14) 0.0039(12) 0.0007(12) 0.0040(12) C3 0.0310(16) 0.0268(15) 0.0277(16) 0.0069(12) 0.0014(13) 0.0028(13) C4 0.0369(18) 0.0258(15) 0.0270(16) 0.0049(12) -0.0050(13) -0.0013(13) C5 0.0432(19) 0.0297(16) 0.0181(14) 0.0047(12) -0.0027(13) 0.0010(14) C6 0.0354(17) 0.0228(14) 0.0222(14) 0.0072(12) 0.0009(12) 0.0012(12) C7 0.0308(16) 0.0268(15) 0.0271(15) 0.0141(12) 0.0070(12) 0.0068(12) C8 0.045(2) 0.0278(16) 0.0340(18) 0.0087(14) 0.0061(15) 0.0062(14) C9 0.057(2) 0.0298(18) 0.060(3) 0.0127(17) 0.025(2) 0.0136(17) C10 0.044(2) 0.045(2) 0.084(3) 0.040(2) 0.025(2) 0.0204(18) C11 0.042(2) 0.064(3) 0.059(3) 0.038(2) 0.0017(19) 0.0135(19) C12 0.0399(19) 0.046(2) 0.0320(18) 0.0176(15) 0.0010(15) 0.0086(16) C13 0.0332(16) 0.0320(16) 0.0178(14) 0.0063(12) 0.0018(12) 0.0124(13) C14 0.048(2) 0.0284(16) 0.0311(17) 0.0067(14) -0.0006(15) 0.0121(15) C15 0.061(2) 0.0370(19) 0.0276(17) -0.0039(15) -0.0001(16) 0.0237(18) C16 0.052(2) 0.053(2) 0.0293(18) 0.0123(16) 0.0112(16) 0.0266(19) C17 0.045(2) 0.045(2) 0.0327(18) 0.0143(16) 0.0105(15) 0.0136(16) C18 0.0412(19) 0.0318(16) 0.0258(16) 0.0080(13) 0.0047(14) 0.0097(14) C19 0.0317(16) 0.0258(14) 0.0190(14) 0.0012(11) -0.0035(12) 0.0072(12) C20 0.050(2) 0.0328(17) 0.0287(17) 0.0100(14) 0.0017(15) 0.0161(15) C21 0.057(2) 0.0345(18) 0.038(2) 0.0082(15) -0.0074(17) 0.0187(17) C22 0.0365(19) 0.0326(17) 0.042(2) -0.0059(15) -0.0124(16) 0.0146(15) C23 0.0269(16) 0.0366(18) 0.0336(18) -0.0055(14) -0.0036(13) 0.0065(14) C24 0.0299(16) 0.0293(16) 0.0292(16) 0.0040(13) -0.0012(13) 0.0059(13) C25 0.0289(15) 0.0260(14) 0.0221(14) 0.0095(12) 0.0041(12) 0.0049(12) C26 0.0367(17) 0.0324(16) 0.0247(15) 0.0106(13) 0.0051(13) 0.0073(14) C27 0.0409(19) 0.046(2) 0.0317(17) 0.0234(16) 0.0072(15) 0.0066(16) C28 0.043(2) 0.0346(18) 0.045(2) 0.0237(16) 0.0034(16) 0.0032(15) C29 0.0420(19) 0.0256(16) 0.0392(19) 0.0102(14) -0.0009(15) 0.0026(14) C30 0.0331(16) 0.0267(15) 0.0248(15) 0.0068(12) 0.0008(13) 0.0046(13) C31 0.0358(16) 0.0192(13) 0.0169(13) 0.0036(11) 0.0000(12) 0.0060(12) C32 0.0363(16) 0.0187(13) 0.0153(13) 0.0045(11) -0.0005(12) 0.0036(12) C33 0.0347(16) 0.0198(13) 0.0170(13) 0.0031(11) -0.0037(12) 0.0016(12) C34 0.0301(16) 0.0267(15) 0.0196(14) 0.0079(12) -0.0026(12) 0.0012(12) C35 0.0382(18) 0.0252(15) 0.0250(15) 0.0081(12) 0.0005(13) 0.0042(13) C36 0.051(2) 0.0276(16) 0.0310(17) 0.0124(14) -0.0038(15) -0.0034(15) C37 0.044(2) 0.044(2) 0.0362(19) 0.0194(16) 0.0037(16) -0.0079(16) C38 0.0390(19) 0.049(2) 0.0328(18) 0.0131(16) 0.0089(15) 0.0020(16) C39 0.0363(18) 0.0315(16) 0.0285(16) 0.0098(13) 0.0036(13) 0.0050(14) C40 0.0370(17) 0.0228(14) 0.0195(14) 0.0078(11) 0.0028(12) 0.0064(12) C41 0.0371(17) 0.0294(16) 0.0253(15) 0.0103(13) 0.0030(13) 0.0075(13) C42 0.0376(18) 0.0425(19) 0.0333(17) 0.0199(15) 0.0089(14) 0.0181(15) C43 0.056(2) 0.0289(16) 0.0358(18) 0.0151(14) 0.0185(16) 0.0204(16) C44 0.053(2) 0.0230(15) 0.0308(17) 0.0056(13) 0.0117(15) 0.0062(15) C45 0.0361(17) 0.0266(15) 0.0249(15) 0.0058(12) 0.0047(13) 0.0051(13) C46 0.0469(19) 0.0227(14) 0.0186(14) 0.0033(12) -0.0030(13) 0.0005(13) C47 0.0326(16) 0.0193(13) 0.0183(13) 0.0048(11) -0.0024(12) 0.0028(12) C48 0.0362(17) 0.0259(15) 0.0215(14) 0.0104(12) 0.0009(12) 0.0054(13) C49 0.0329(17) 0.0262(15) 0.0344(17) 0.0107(13) 0.0037(13) 0.0060(13) C50 0.044(2) 0.0275(16) 0.0360(18) 0.0097(14) 0.0036(15) -0.0017(14) C51 0.052(2) 0.0276(16) 0.0314(17) 0.0120(14) 0.0071(15) 0.0110(15) C52 0.044(2) 0.0367(18) 0.0327(17) 0.0143(14) 0.0027(15) 0.0166(15) C53 0.0360(18) 0.0349(17) 0.0306(17) 0.0141(14) -0.0020(14) 0.0064(14) C54 0.061(2) 0.0224(15) 0.0231(15) 0.0062(12) -0.0115(15) 0.0090(15) C55 0.077(3) 0.051(2) 0.0290(19) 0.0182(17) -0.0059(19) 0.002(2) C56 0.113(4) 0.059(3) 0.032(2) 0.023(2) 0.008(2) 0.022(3) C57 0.148(6) 0.050(3) 0.0220(19) 0.0037(18) -0.011(3) 0.047(3) C58 0.118(5) 0.057(3) 0.037(2) -0.011(2) -0.041(3) 0.040(3) C59 0.067(3) 0.040(2) 0.037(2) -0.0032(16) -0.0250(19) 0.0196(19) C60 0.064(3) 0.079(3) 0.042(2) 0.031(2) 0.003(2) 0.008(2) O1 0.0373(12) 0.0379(12) 0.0165(10) 0.0053(9) 0.0018(9) -0.0047(10) O2 0.0324(11) 0.0259(10) 0.0233(10) 0.0087(8) 0.0044(9) 0.0067(9) O3 0.0400(13) 0.0270(11) 0.0212(10) 0.0081(9) 0.0057(9) 0.0108(9) F1 0.341(9) 0.078(3) 0.129(4) -0.024(3) 0.155(5) -0.038(4) F2 0.176(4) 0.146(4) 0.118(3) 0.098(3) -0.046(3) -0.046(3) F3 0.129(3) 0.0612(16) 0.0518(15) 0.0320(13) 0.0469(16) 0.0456(17) F4 0.092(3) 0.151(4) 0.067(2) -0.024(2) 0.0319(19) -0.013(2) F5 0.088(4) 0.109(5) 0.142(6) 0.087(5) 0.078(4) 0.068(4) F5' 0.052(5) 0.110(8) 0.083(6) 0.073(6) 0.025(4) 0.029(5) F6 0.260(5) 0.072(2) 0.061(2) 0.0073(16) 0.096(3) -0.023(3) P1 0.0324(4) 0.0236(4) 0.0157(3) 0.0056(3) 0.0021(3) 0.0031(3) P2 0.0308(4) 0.0201(3) 0.0146(3) 0.0050(3) 0.0013(3) 0.0060(3) P3 0.0298(4) 0.0193(3) 0.0175(3) 0.0055(3) -0.0002(3) 0.0035(3) P4 0.0350(4) 0.0252(4) 0.0254(4) 0.0092(3) -0.0081(3) 0.0017(3) P5 0.1750(17) 0.0365(6) 0.0422(6) 0.0182(5) 0.0580(9) 0.0259(8) Pd1 0.02977(13) 0.01973(11) 0.01393(11) 0.00464(8) 0.00055(8) 0.00353(8) Cl1 0.0543(6) 0.0500(5) 0.0501(6) 0.0186(5) 0.0022(4) 0.0063(4) Cl2 0.0581(6) 0.0623(6) 0.0456(5) 0.0127(5) 0.0021(5) 0.0137(5) _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 C1 C2 1.397(4) . ? C1 C6 1.401(4) . ? C1 Pd1 2.100(3) . ? C2 C3 1.389(4) . ? C3 C4 1.387(4) . ? C4 C5 1.382(5) . ? C5 C6 1.385(4) . ? C6 O1 1.415(4) . ? C7 C8 1.379(5) . ? C7 C12 1.378(5) . ? C7 O2 1.412(4) . ? C8 C9 1.390(5) . ? C9 C10 1.378(6) . ? C10 C11 1.370(6) . ? C11 C12 1.380(5) . ? C13 C14 1.376(4) . ? C13 C18 1.379(5) . ? C13 O3 1.410(4) . ? C14 C15 1.400(5) . ? C15 C16 1.366(6) . ? C16 C17 1.381(5) . ? C17 C18 1.390(5) . ? C19 C24 1.387(5) . ? C19 C20 1.395(4) . ? C19 P2 1.819(3) . ? C20 C21 1.384(5) . ? C21 C22 1.375(6) . ? C22 C23 1.378(5) . ? C23 C24 1.391(4) . ? C25 C30 1.397(4) . ? C25 C26 1.402(4) . ? C25 P2 1.819(3) . ? C26 C27 1.387(5) . ? C27 C28 1.387(5) . ? C28 C29 1.386(5) . ? C29 C30 1.390(4) . ? C31 C32 1.535(4) . ? C31 P2 1.838(3) . ? C32 C33 1.537(4) . ? C32 C46 1.538(4) . ? C32 C47 1.540(4) . ? C33 P3 1.835(3) . ? C34 C39 1.389(5) . ? C34 C35 1.400(4) . ? C34 P3 1.828(3) . ? C35 C36 1.380(5) . ? C36 C37 1.382(5) . ? C37 C38 1.380(5) . ? C38 C39 1.387(5) . ? C40 C45 1.390(4) . ? C40 C41 1.396(5) . ? C40 P3 1.817(3) . ? C41 C42 1.393(4) . ? C42 C43 1.380(5) . ? C43 C44 1.379(5) . ? C44 C45 1.388(4) . ? C47 P4 1.851(3) . ? C48 C49 1.389(5) . ? C48 C53 1.400(5) . ? C48 P4 1.833(3) . ? C49 C50 1.388(4) . ? C50 C51 1.383(5) . ? C51 C52 1.377(5) . ? C52 C53 1.384(5) . ? C54 C55 1.375(6) . ? C54 C59 1.393(5) . ? C54 P4 1.845(3) . ? C55 C56 1.395(5) . ? C56 C57 1.350(8) . ? C57 C58 1.375(8) . ? C58 C59 1.405(6) . ? C60 Cl1 1.746(5) . ? C60 Cl2 1.757(5) . ? O1 P1 1.593(2) . ? O2 P1 1.594(2) . ? O3 P1 1.571(2) . ? F1 P5 1.660(6) . ? F2 P5 1.626(5) . ? F3 P5 1.600(3) . ? F4 P5 1.558(4) . ? F5 P5 1.495(5) . ? F5 F5' 1.606(11) . ? F5' P5 1.808(8) . ? F6 P5 1.572(3) . ? P1 Pd1 2.2250(10) . ? P2 Pd1 2.3444(10) . ? P3 Pd1 2.3455(10) . ? 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 C2 C1 C6 114.3(3) . . ? C2 C1 Pd1 128.5(2) . . ? C6 C1 Pd1 117.0(2) . . ? C3 C2 C1 122.3(3) . . ? C4 C3 C2 120.9(3) . . ? C5 C4 C3 119.2(3) . . ? C4 C5 C6 118.4(3) . . ? C5 C6 C1 125.0(3) . . ? C5 C6 O1 115.1(3) . . ? C1 C6 O1 119.9(3) . . ? C8 C7 C12 122.1(3) . . ? C8 C7 O2 119.1(3) . . ? C12 C7 O2 118.7(3) . . ? C7 C8 C9 118.3(3) . . ? C10 C9 C8 119.9(4) . . ? C11 C10 C9 120.8(4) . . ? C10 C11 C12 120.4(4) . . ? C7 C12 C11 118.5(4) . . ? C14 C13 C18 122.5(3) . . ? C14 C13 O3 117.5(3) . . ? C18 C13 O3 119.8(3) . . ? C13 C14 C15 117.7(3) . . ? C16 C15 C14 120.9(3) . . ? C15 C16 C17 120.1(3) . . ? C16 C17 C18 120.4(4) . . ? C13 C18 C17 118.3(3) . . ? C24 C19 C20 119.0(3) . . ? C24 C19 P2 122.6(2) . . ? C20 C19 P2 117.6(3) . . ? C21 C20 C19 120.4(3) . . ? C22 C21 C20 120.2(3) . . ? C21 C22 C23 120.1(3) . . ? C22 C23 C24 120.3(3) . . ? C19 C24 C23 120.1(3) . . ? C30 C25 C26 118.8(3) . . ? C30 C25 P2 119.5(2) . . ? C26 C25 P2 121.7(2) . . ? C27 C26 C25 120.4(3) . . ? C28 C27 C26 120.2(3) . . ? C27 C28 C29 120.0(3) . . ? C28 C29 C30 120.1(3) . . ? C29 C30 C25 120.5(3) . . ? C32 C31 P2 121.8(2) . . ? C31 C32 C33 111.2(2) . . ? C31 C32 C46 106.3(2) . . ? C33 C32 C46 106.2(2) . . ? C31 C32 C47 110.7(2) . . ? C33 C32 C47 112.2(2) . . ? C46 C32 C47 110.0(2) . . ? C32 C33 P3 120.9(2) . . ? C39 C34 C35 119.0(3) . . ? C39 C34 P3 122.7(2) . . ? C35 C34 P3 118.2(2) . . ? C36 C35 C34 120.0(3) . . ? C35 C36 C37 120.5(3) . . ? C38 C37 C36 119.8(3) . . ? C37 C38 C39 120.2(3) . . ? C38 C39 C34 120.4(3) . . ? C45 C40 C41 118.9(3) . . ? C45 C40 P3 120.0(2) . . ? C41 C40 P3 121.0(2) . . ? C42 C41 C40 120.2(3) . . ? C43 C42 C41 119.9(3) . . ? C44 C43 C42 120.4(3) . . ? C43 C44 C45 119.8(3) . . ? C44 C45 C40 120.7(3) . . ? C32 C47 P4 115.0(2) . . ? C49 C48 C53 118.7(3) . . ? C49 C48 P4 125.1(2) . . ? C53 C48 P4 116.2(2) . . ? C50 C49 C48 120.4(3) . . ? C51 C50 C49 120.3(3) . . ? C52 C51 C50 120.0(3) . . ? C51 C52 C53 120.1(3) . . ? C52 C53 C48 120.6(3) . . ? C55 C54 C59 118.7(4) . . ? C55 C54 P4 125.5(3) . . ? C59 C54 P4 115.7(3) . . ? C54 C55 C56 120.7(4) . . ? C57 C56 C55 120.8(5) . . ? C56 C57 C58 119.7(4) . . ? C57 C58 C59 120.5(5) . . ? C54 C59 C58 119.5(5) . . ? Cl1 C60 Cl2 112.9(2) . . ? C6 O1 P1 113.61(18) . . ? C7 O2 P1 118.88(19) . . ? C13 O3 P1 128.01(19) . . ? P5 F5 F5' 71.2(4) . . ? F5 F5' P5 51.5(3) . . ? O3 P1 O1 104.91(12) . . ? O3 P1 O2 102.15(12) . . ? O1 P1 O2 103.81(12) . . ? O3 P1 Pd1 117.52(9) . . ? O1 P1 Pd1 108.97(9) . . ? O2 P1 Pd1 117.94(8) . . ? C25 P2 C19 108.64(15) . . ? C25 P2 C31 106.53(13) . . ? C19 P2 C31 96.98(13) . . ? C25 P2 Pd1 114.87(10) . . ? C19 P2 Pd1 112.90(10) . . ? C31 P2 Pd1 115.29(11) . . ? C40 P3 C34 105.78(14) . . ? C40 P3 C33 106.37(14) . . ? C34 P3 C33 100.87(14) . . ? C40 P3 Pd1 107.36(11) . . ? C34 P3 Pd1 115.26(10) . . ? C33 P3 Pd1 120.09(11) . . ? C48 P4 C54 99.76(14) . . ? C48 P4 C47 101.08(14) . . ? C54 P4 C47 104.40(16) . . ? F5 P5 F4 125.2(4) . . ? F5 P5 F6 91.5(3) . . ? F4 P5 F6 89.9(2) . . ? F5 P5 F3 89.3(2) . . ? F4 P5 F3 90.69(18) . . ? F6 P5 F3 178.5(3) . . ? F5 P5 F2 151.0(4) . . ? F4 P5 F2 83.5(3) . . ? F6 P5 F2 93.0(3) . . ? F3 P5 F2 85.7(2) . . ? F5 P5 F1 72.9(4) . . ? F4 P5 F1 161.8(3) . . ? F6 P5 F1 92.0(2) . . ? F3 P5 F1 87.0(2) . . ? F2 P5 F1 78.3(3) . . ? F5 P5 F5' 57.2(4) . . ? F4 P5 F5' 68.0(4) . . ? F6 P5 F5' 91.1(3) . . ? F3 P5 F5' 90.4(2) . . ? F2 P5 F5' 151.2(4) . . ? F1 P5 F5' 130.1(4) . . ? C1 Pd1 P1 79.41(9) . . ? C1 Pd1 P2 96.82(9) . . ? P1 Pd1 P2 171.78(3) . . ? C1 Pd1 P3 166.96(8) . . ? P1 Pd1 P3 92.72(4) . . ? P2 Pd1 P3 92.26(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.466 _refine_diff_density_min -1.123 _refine_diff_density_rms 0.088