Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Robin B. Bedford' 'Michael E. Blake' 'Simon J. Coles' 'Michael B. Hursthouse' 'P. Noelle Scully' _publ_contact_author_name 'Dr Robin B. Bedford' _publ_contact_author_address ; School of Chemistry University of Exeter Exeter EX4 4QD UNITED KINGDOM ; _publ_contact_author_email R.BEDFORD@EX.AC.UK _publ_contact_author_phone '+44 (0)2380 596722' _publ_contact_author_fax '+44 (0)2380 596723' _publ_section_title ; The first example of a doubly orthometallated aryl bis(phosphinite) ligand ; data_1 _database_code_CSD 210006 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 Cl6 F12 O12 P4 Pd4' _chemical_formula_weight 2097.38 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' Cl Cl 0.1484 0.1585 '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' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.4010(5) _cell_length_b 14.0306(3) _cell_length_c 20.3106(3) _cell_angle_alpha 90.00 _cell_angle_beta 126.4610(10) _cell_angle_gamma 90.00 _cell_volume 7655.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 22222 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.820 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4128 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7800 _exptl_absorpt_correction_T_max 0.9257 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _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' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_decay_% negligible _diffrn_reflns_number 38540 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8745 _reflns_number_gt 7183 _reflns_threshold_expression >2\s(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 '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^)+(0.0280P)^2^+27.4581P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00047(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8745 _refine_ls_number_parameters 498 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0905 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.005 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 Cl1 Cl 0.13050(5) 0.02747(11) 0.47843(9) 0.0635(4) Uani 1 1 d . . . Cl2 Cl 0.11512(8) 0.00265(15) 0.60295(9) 0.0926(6) Uani 1 1 d . . . Cl3 Cl 0.03731(5) -0.04971(9) 0.43580(9) 0.0573(3) Uani 1 1 d . . . C36 C 0.08677(19) 0.0298(3) 0.5002(3) 0.0444(11) Uani 1 1 d . . . H36 H 0.0728 0.0957 0.4895 0.053 Uiso 1 1 calc R . . Pd1 Pd -0.063355(9) 0.476093(17) 0.333597(14) 0.01455(8) Uani 1 1 d . . . Pd2 Pd 0.121851(9) 0.426491(17) 0.357579(14) 0.01441(8) Uani 1 1 d . . . P1 P -0.05775(3) 0.62425(6) 0.36980(5) 0.01551(18) Uani 1 1 d . . . P2 P 0.17732(3) 0.52616(6) 0.44759(5) 0.01583(18) Uani 1 1 d . . . F1 F 0.05571(10) 0.13754(16) 0.16065(15) 0.0415(6) Uani 1 1 d . . . F2 F 0.06614(9) 0.11999(15) 0.27417(14) 0.0377(6) Uani 1 1 d . . . F3 F -0.00504(8) 0.16452(17) 0.16723(15) 0.0399(6) Uani 1 1 d . . . F4 F 0.25502(8) 0.35549(18) 0.35239(13) 0.0363(6) Uani 1 1 d . . . F5 F 0.20773(9) 0.2897(2) 0.23418(14) 0.0450(7) Uani 1 1 d . . . F6 F 0.22882(10) 0.4367(2) 0.24500(18) 0.0535(8) Uani 1 1 d . . . O2 O 0.15301(8) 0.59031(16) 0.48191(13) 0.0174(5) Uani 1 1 d . . . O3 O 0.05403(9) 0.32571(16) 0.17029(14) 0.0195(5) Uani 1 1 d . . . O4 O 0.07299(9) 0.30711(16) 0.29640(14) 0.0206(5) Uani 1 1 d . . . O5 O 0.13781(9) 0.44578(17) 0.20668(14) 0.0205(5) Uani 1 1 d . . . O6 O 0.16810(9) 0.36882(17) 0.32603(14) 0.0200(5) Uani 1 1 d . . . O10 O 0.00027(8) 0.63884(16) 0.44924(13) 0.0170(5) Uani 1 1 d . . . C1 C -0.09271(12) 0.6608(2) 0.4063(2) 0.0172(7) Uani 1 1 d . . . C2 C -0.14465(13) 0.6575(3) 0.3502(2) 0.0242(8) Uani 1 1 d . . . H2 H -0.1598 0.6354 0.2960 0.029 Uiso 1 1 calc R . . C3 C -0.17377(13) 0.6864(3) 0.3743(2) 0.0286(8) Uani 1 1 d . . . H3 H -0.2090 0.6854 0.3362 0.034 Uiso 1 1 calc R . . C4 C -0.15170(14) 0.7168(3) 0.4537(2) 0.0281(8) Uani 1 1 d . . . H4 H -0.1719 0.7362 0.4699 0.034 Uiso 1 1 calc R . . C5 C -0.10043(14) 0.7193(3) 0.5097(2) 0.0254(8) Uani 1 1 d . . . H5 H -0.0855 0.7399 0.5642 0.030 Uiso 1 1 calc R . . C6 C -0.07044(13) 0.6912(2) 0.4859(2) 0.0203(7) Uani 1 1 d . . . H6 H -0.0352 0.6930 0.5240 0.024 Uiso 1 1 calc R . . C7 C -0.06747(12) 0.7162(2) 0.2994(2) 0.0190(7) Uani 1 1 d . . . C8 C -0.07846(15) 0.8088(2) 0.3081(2) 0.0275(8) Uani 1 1 d . . . H8 H -0.0841 0.8224 0.3477 0.033 Uiso 1 1 calc R . . C9 C -0.08119(16) 0.8815(3) 0.2593(3) 0.0341(9) Uani 1 1 d . . . H9 H -0.0890 0.9445 0.2652 0.041 Uiso 1 1 calc R . . C10 C -0.07249(15) 0.8618(3) 0.2019(2) 0.0319(9) Uani 1 1 d . . . H10 H -0.0739 0.9116 0.1689 0.038 Uiso 1 1 calc R . . C11 C -0.06172(14) 0.7696(3) 0.1926(2) 0.0285(8) Uani 1 1 d . . . H11 H -0.0559 0.7566 0.1530 0.034 Uiso 1 1 calc R . . C12 C -0.05939(13) 0.6962(3) 0.2405(2) 0.0217(7) Uani 1 1 d . . . H12 H -0.0524 0.6330 0.2335 0.026 Uiso 1 1 calc R . . C13 C 0.02992(12) 0.5852(2) 0.43480(19) 0.0142(6) Uani 1 1 d . . . C14 C 0.07916(12) 0.6138(2) 0.47295(19) 0.0155(6) Uani 1 1 d . . . C15 C 0.10211(13) 0.6968(2) 0.5318(2) 0.0211(7) Uani 1 1 d . . . H15A H 0.1368 0.6818 0.5766 0.032 Uiso 1 1 calc R . . H15B H 0.0834 0.7087 0.5540 0.032 Uiso 1 1 calc R . . H15C H 0.1011 0.7537 0.5028 0.032 Uiso 1 1 calc R . . C16 C 0.10404(12) 0.5625(2) 0.44859(19) 0.0154(6) Uani 1 1 d . . . C17 C 0.08318(12) 0.4875(2) 0.39208(19) 0.0150(6) Uani 1 1 d . . . C18 C 0.03425(12) 0.4606(2) 0.35855(19) 0.0164(6) Uani 1 1 d . . . H18 H 0.0195 0.4090 0.3209 0.020 Uiso 1 1 calc R . . C19 C 0.00695(12) 0.5089(2) 0.37990(19) 0.0149(6) Uani 1 1 d . . . C20 C 0.05898(12) 0.2807(2) 0.2273(2) 0.0178(7) Uani 1 1 d . . . C21 C 0.04439(13) 0.1737(2) 0.2076(2) 0.0223(7) Uani 1 1 d . . . C22 C 0.16893(12) 0.3987(2) 0.2687(2) 0.0164(7) Uani 1 1 d . . . C23 C 0.21570(14) 0.3704(3) 0.2755(2) 0.0265(8) Uani 1 1 d . . . C24 C 0.24542(14) 0.4925(3) 0.6147(2) 0.0246(8) Uani 1 1 d . . . H24 H 0.2280 0.5404 0.6213 0.030 Uiso 1 1 calc R . . C25 C 0.28619(15) 0.4487(3) 0.6823(2) 0.0333(9) Uani 1 1 d . . . H25 H 0.2968 0.4669 0.7355 0.040 Uiso 1 1 calc R . . C26 C 0.31187(14) 0.3786(3) 0.6737(2) 0.0326(9) Uani 1 1 d . . . H26 H 0.3404 0.3497 0.7207 0.039 Uiso 1 1 calc R . . C27 C 0.29587(15) 0.3509(3) 0.5962(2) 0.0340(9) Uani 1 1 d . . . H27 H 0.3132 0.3021 0.5902 0.041 Uiso 1 1 calc R . . C28 C 0.25470(14) 0.3936(3) 0.5273(2) 0.0264(8) Uani 1 1 d . . . H28 H 0.2435 0.3736 0.4742 0.032 Uiso 1 1 calc R . . C29 C 0.22977(12) 0.4666(2) 0.5365(2) 0.0184(7) Uani 1 1 d . . . C30 C 0.20427(12) 0.6138(2) 0.4191(2) 0.0185(7) Uani 1 1 d . . . C31 C 0.24026(15) 0.5856(3) 0.4084(2) 0.0286(8) Uani 1 1 d . . . H31 H 0.2513 0.5213 0.4179 0.034 Uiso 1 1 calc R . . C32 C 0.25965(17) 0.6518(3) 0.3838(3) 0.0367(10) Uani 1 1 d . . . H32 H 0.2843 0.6330 0.3770 0.044 Uiso 1 1 calc R . . C33 C 0.24343(16) 0.7449(3) 0.3692(2) 0.0330(9) Uani 1 1 d . . . H33 H 0.2565 0.7897 0.3516 0.040 Uiso 1 1 calc R . . C34 C 0.20810(15) 0.7734(3) 0.3802(2) 0.0298(8) Uani 1 1 d . . . H34 H 0.1973 0.8378 0.3707 0.036 Uiso 1 1 calc R . . C35 C 0.18823(13) 0.7075(3) 0.4050(2) 0.0235(7) Uani 1 1 d . . . H35 H 0.1638 0.7269 0.4122 0.028 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 Cl1 0.0516(8) 0.0785(10) 0.0610(8) -0.0282(7) 0.0338(7) -0.0120(7) Cl2 0.1160(15) 0.1118(14) 0.0397(8) 0.0159(8) 0.0406(9) 0.0443(12) Cl3 0.0552(8) 0.0424(7) 0.0722(9) 0.0005(6) 0.0368(7) 0.0021(6) C36 0.052(3) 0.043(3) 0.036(2) -0.002(2) 0.025(2) 0.011(2) Pd1 0.01197(13) 0.01464(14) 0.01733(14) -0.00157(9) 0.00887(11) -0.00125(9) Pd2 0.01392(13) 0.01482(13) 0.01690(14) -0.00114(9) 0.01047(11) 0.00000(9) P1 0.0127(4) 0.0155(4) 0.0184(4) -0.0013(3) 0.0093(3) -0.0002(3) P2 0.0131(4) 0.0171(4) 0.0185(4) -0.0013(3) 0.0101(3) -0.0010(3) F1 0.0682(18) 0.0231(12) 0.0548(15) -0.0141(11) 0.0484(14) -0.0060(11) F2 0.0507(15) 0.0159(11) 0.0366(13) 0.0055(9) 0.0206(12) 0.0024(10) F3 0.0227(12) 0.0268(12) 0.0561(15) -0.0068(11) 0.0157(11) -0.0102(10) F4 0.0186(11) 0.0606(16) 0.0246(11) 0.0018(10) 0.0101(9) 0.0162(11) F5 0.0338(13) 0.0641(17) 0.0364(13) -0.0117(12) 0.0204(11) 0.0187(12) F6 0.0343(14) 0.076(2) 0.0711(18) 0.0364(15) 0.0427(14) 0.0187(14) O2 0.0126(11) 0.0190(12) 0.0220(12) -0.0054(9) 0.0110(10) -0.0028(9) O3 0.0194(12) 0.0170(12) 0.0208(12) 0.0000(10) 0.0113(10) 0.0011(10) O4 0.0226(13) 0.0197(12) 0.0246(13) -0.0047(10) 0.0167(11) -0.0044(10) O5 0.0161(12) 0.0247(13) 0.0233(12) 0.0064(10) 0.0131(10) 0.0052(10) O6 0.0214(12) 0.0217(12) 0.0232(12) 0.0014(10) 0.0166(10) 0.0056(10) O10 0.0126(11) 0.0200(12) 0.0184(11) -0.0057(9) 0.0093(9) 0.0000(9) C1 0.0174(16) 0.0140(15) 0.0248(17) 0.0015(13) 0.0150(14) 0.0030(13) C2 0.0158(17) 0.0225(18) 0.0288(19) -0.0045(15) 0.0102(15) 0.0006(14) C3 0.0144(17) 0.0250(19) 0.046(2) 0.0023(17) 0.0176(17) 0.0032(15) C4 0.031(2) 0.0267(19) 0.041(2) 0.0072(17) 0.0291(19) 0.0086(16) C5 0.031(2) 0.0273(19) 0.0266(19) 0.0049(15) 0.0218(17) 0.0051(16) C6 0.0177(17) 0.0224(18) 0.0217(17) 0.0023(14) 0.0123(14) 0.0019(14) C7 0.0152(16) 0.0199(17) 0.0193(16) -0.0007(13) 0.0088(13) -0.0020(13) C8 0.037(2) 0.0174(18) 0.033(2) -0.0012(15) 0.0239(18) -0.0012(16) C9 0.044(2) 0.0180(18) 0.045(2) 0.0000(17) 0.030(2) -0.0026(17) C10 0.035(2) 0.027(2) 0.032(2) 0.0084(16) 0.0183(18) -0.0018(17) C11 0.0243(19) 0.039(2) 0.0208(18) 0.0019(16) 0.0128(16) -0.0045(17) C12 0.0184(17) 0.0227(18) 0.0216(17) -0.0007(14) 0.0105(14) -0.0018(14) C13 0.0140(15) 0.0138(15) 0.0175(15) 0.0018(12) 0.0108(13) 0.0038(12) C14 0.0128(15) 0.0176(16) 0.0158(15) -0.0006(13) 0.0084(13) -0.0005(13) C15 0.0183(17) 0.0224(18) 0.0234(17) -0.0052(14) 0.0129(14) -0.0035(14) C16 0.0107(15) 0.0184(16) 0.0172(16) -0.0017(13) 0.0084(13) -0.0032(12) C17 0.0149(15) 0.0138(15) 0.0180(16) 0.0022(12) 0.0106(13) 0.0015(12) C18 0.0148(16) 0.0157(16) 0.0155(15) -0.0015(12) 0.0073(13) -0.0006(13) C19 0.0132(15) 0.0138(15) 0.0175(16) 0.0025(12) 0.0091(13) 0.0021(12) C20 0.0112(15) 0.0211(17) 0.0204(17) -0.0005(14) 0.0090(13) 0.0023(13) C21 0.0232(18) 0.0188(17) 0.0236(18) -0.0015(14) 0.0131(15) -0.0005(15) C22 0.0135(15) 0.0195(17) 0.0207(16) -0.0014(13) 0.0126(14) 0.0013(13) C23 0.0228(19) 0.040(2) 0.0204(18) 0.0046(16) 0.0146(15) 0.0123(17) C24 0.0258(19) 0.0241(18) 0.0251(19) -0.0009(15) 0.0158(16) 0.0004(15) C25 0.029(2) 0.044(2) 0.0171(18) -0.0015(17) 0.0077(16) -0.0004(18) C26 0.0209(19) 0.042(2) 0.027(2) 0.0097(18) 0.0100(16) 0.0024(17) C27 0.027(2) 0.035(2) 0.037(2) 0.0078(18) 0.0178(18) 0.0114(17) C28 0.0260(19) 0.028(2) 0.0253(19) 0.0011(15) 0.0153(16) 0.0052(16) C29 0.0149(16) 0.0188(17) 0.0202(17) -0.0006(13) 0.0097(14) -0.0029(13) C30 0.0128(16) 0.0221(17) 0.0192(16) -0.0019(13) 0.0087(13) -0.0040(13) C31 0.031(2) 0.0255(19) 0.041(2) -0.0041(16) 0.0284(19) -0.0041(16) C32 0.041(2) 0.039(2) 0.051(3) -0.007(2) 0.039(2) -0.0091(19) C33 0.039(2) 0.032(2) 0.036(2) -0.0037(17) 0.0271(19) -0.0163(18) C34 0.029(2) 0.026(2) 0.030(2) 0.0047(16) 0.0150(17) -0.0023(16) C35 0.0145(17) 0.0264(19) 0.0271(18) 0.0009(15) 0.0110(15) -0.0031(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C36 1.760(5) . ? Cl2 C36 1.746(5) . ? Cl3 C36 1.765(5) . ? Pd1 C19 1.996(3) . ? Pd1 O3 2.141(2) 2 ? Pd1 O5 2.149(2) 2 ? Pd1 P1 2.1756(9) . ? Pd1 Pd2 3.2190(3) 2 ? Pd2 C17 1.992(3) . ? Pd2 O4 2.145(2) . ? Pd2 O6 2.151(2) . ? Pd2 P2 2.1690(9) . ? Pd2 Pd1 3.2190(3) 2 ? P1 O10 1.638(2) . ? P1 C1 1.790(3) . ? P1 C7 1.806(3) . ? P2 O2 1.621(2) . ? P2 C29 1.808(3) . ? P2 C30 1.810(3) . ? F1 C21 1.320(4) . ? F2 C21 1.325(4) . ? F3 C21 1.344(4) . ? F4 C23 1.330(4) . ? F5 C23 1.338(5) . ? F6 C23 1.328(5) . ? O2 C16 1.403(4) . ? O3 C20 1.241(4) . ? O3 Pd1 2.141(2) 2 ? O4 C20 1.243(4) . ? O5 C22 1.244(4) . ? O5 Pd1 2.149(2) 2 ? O6 C22 1.252(4) . ? O10 C13 1.406(4) . ? C1 C6 1.386(5) . ? C1 C2 1.400(5) . ? C2 C3 1.384(5) . ? C3 C4 1.383(6) . ? C4 C5 1.383(5) . ? C5 C6 1.402(5) . ? C7 C8 1.389(5) . ? C7 C12 1.402(5) . ? C8 C9 1.387(5) . ? C9 C10 1.386(6) . ? C10 C11 1.385(6) . ? C11 C12 1.387(5) . ? C13 C14 1.397(4) . ? C13 C19 1.401(4) . ? C14 C16 1.394(4) . ? C14 C15 1.510(4) . ? C16 C17 1.400(4) . ? C17 C18 1.398(5) . ? C18 C19 1.396(4) . ? C20 C21 1.555(5) . ? C22 C23 1.537(5) . ? C24 C25 1.377(5) . ? C24 C29 1.393(5) . ? C25 C26 1.383(6) . ? C26 C27 1.383(6) . ? C27 C28 1.387(5) . ? C28 C29 1.400(5) . ? C30 C35 1.384(5) . ? C30 C31 1.401(5) . ? C31 C32 1.385(5) . ? C32 C33 1.376(6) . ? C33 C34 1.383(6) . ? C34 C35 1.395(5) . ? 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 Cl2 C36 Cl1 110.8(3) . . ? Cl2 C36 Cl3 110.6(3) . . ? Cl1 C36 Cl3 110.7(2) . . ? C19 Pd1 O3 95.06(11) . 2 ? C19 Pd1 O5 175.02(11) . 2 ? O3 Pd1 O5 87.23(9) 2 2 ? C19 Pd1 P1 77.28(9) . . ? O3 Pd1 P1 165.66(7) 2 . ? O5 Pd1 P1 99.53(7) 2 . ? C19 Pd1 Pd2 108.59(9) . 2 ? O3 Pd1 Pd2 74.92(6) 2 2 ? O5 Pd1 Pd2 76.26(6) 2 2 ? P1 Pd1 Pd2 118.87(2) . 2 ? C17 Pd2 O4 96.33(11) . . ? C17 Pd2 O6 175.49(11) . . ? O4 Pd2 O6 88.15(9) . . ? C17 Pd2 P2 80.44(10) . . ? O4 Pd2 P2 165.07(7) . . ? O6 Pd2 P2 95.09(7) . . ? C17 Pd2 Pd1 106.01(9) . 2 ? O4 Pd2 Pd1 76.27(6) . 2 ? O6 Pd2 Pd1 75.56(6) . 2 ? P2 Pd2 Pd1 118.65(2) . 2 ? O10 P1 C1 103.73(14) . . ? O10 P1 C7 103.97(14) . . ? C1 P1 C7 105.57(16) . . ? O10 P1 Pd1 105.43(9) . . ? C1 P1 Pd1 117.86(11) . . ? C7 P1 Pd1 118.43(12) . . ? O2 P2 C29 105.24(14) . . ? O2 P2 C30 103.38(14) . . ? C29 P2 C30 105.21(15) . . ? O2 P2 Pd2 108.98(9) . . ? C29 P2 Pd2 112.28(11) . . ? C30 P2 Pd2 120.44(11) . . ? C16 O2 P2 112.11(19) . . ? C20 O3 Pd1 126.5(2) . 2 ? C20 O4 Pd2 122.2(2) . . ? C22 O5 Pd1 124.9(2) . 2 ? C22 O6 Pd2 124.5(2) . . ? C13 O10 P1 107.17(19) . . ? C6 C1 C2 120.4(3) . . ? C6 C1 P1 122.8(3) . . ? C2 C1 P1 116.9(3) . . ? C3 C2 C1 119.6(3) . . ? C4 C3 C2 120.2(3) . . ? C5 C4 C3 120.5(3) . . ? C4 C5 C6 119.9(3) . . ? C1 C6 C5 119.4(3) . . ? C8 C7 C12 119.6(3) . . ? C8 C7 P1 120.3(3) . . ? C12 C7 P1 119.8(3) . . ? C9 C8 C7 120.5(4) . . ? C10 C9 C8 119.8(4) . . ? C11 C10 C9 120.2(4) . . ? C10 C11 C12 120.5(3) . . ? C11 C12 C7 119.5(3) . . ? C14 C13 C19 124.6(3) . . ? C14 C13 O10 118.3(3) . . ? C19 C13 O10 117.0(3) . . ? C16 C14 C13 114.1(3) . . ? C16 C14 C15 123.3(3) . . ? C13 C14 C15 122.5(3) . . ? C14 C16 C17 124.6(3) . . ? C14 C16 O2 117.1(3) . . ? C17 C16 O2 118.3(3) . . ? C18 C17 C16 118.1(3) . . ? C18 C17 Pd2 121.8(2) . . ? C16 C17 Pd2 120.1(2) . . ? C19 C18 C17 120.5(3) . . ? C18 C19 C13 117.9(3) . . ? C18 C19 Pd1 123.0(2) . . ? C13 C19 Pd1 119.0(2) . . ? O3 C20 O4 130.8(3) . . ? O3 C20 C21 113.8(3) . . ? O4 C20 C21 115.4(3) . . ? F1 C21 F2 107.4(3) . . ? F1 C21 F3 107.3(3) . . ? F2 C21 F3 107.3(3) . . ? F1 C21 C20 112.1(3) . . ? F2 C21 C20 112.9(3) . . ? F3 C21 C20 109.5(3) . . ? O5 C22 O6 130.7(3) . . ? O5 C22 C23 114.9(3) . . ? O6 C22 C23 114.4(3) . . ? F6 C23 F4 106.8(3) . . ? F6 C23 F5 107.3(3) . . ? F4 C23 F5 107.0(3) . . ? F6 C23 C22 112.1(3) . . ? F4 C23 C22 112.8(3) . . ? F5 C23 C22 110.5(3) . . ? C25 C24 C29 120.0(4) . . ? C24 C25 C26 120.7(4) . . ? C27 C26 C25 119.7(4) . . ? C26 C27 C28 120.5(4) . . ? C27 C28 C29 119.6(3) . . ? C24 C29 C28 119.5(3) . . ? C24 C29 P2 120.2(3) . . ? C28 C29 P2 120.3(3) . . ? C35 C30 C31 119.9(3) . . ? C35 C30 P2 120.5(3) . . ? C31 C30 P2 119.6(3) . . ? C32 C31 C30 119.7(4) . . ? C33 C32 C31 120.4(4) . . ? C32 C33 C34 120.3(4) . . ? C33 C34 C35 120.1(4) . . ? C30 C35 C34 119.7(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.883 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.123