Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name C.Carmen W.Oberhauser _publ_contact_author_name 'Werner Oberhauser' _publ_contact_author_email werner.oberhauser@iccom.cnr.it data_xylophos _database_code_depnum_ccdc_archive 'CCDC 660552' _audit_creation_date 2007-04-14T17:26:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C36 H40 Cl2 O7 P2 Pd' _chemical_formula_weight 823.92 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.395(5) _cell_length_b 17.986(5) _cell_length_c 20.001(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 4099(2) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.936 _exptl_absorpt_correction_type empirical #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.1303 _diffrn_reflns_av_unetI/netI 0.0769 _diffrn_reflns_number 59870 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.42 _diffrn_reflns_theta_max 64.83 _diffrn_reflns_theta_full 64.83 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 6800 _reflns_number_gt 5206 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Oxford Diffraction software' _computing_cell_refinement 'Oxford Diffraction software' _computing_structure_solution "SIR-97, WinGX v1.70.01'(Farrugia, 1997)" _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0511P)^2^+0.0000P] 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_number_reflns 6800 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(8) _refine_diff_density_max 1.045 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.58995(4) 0.04691(2) 0.659079(18) 0.02879(11) Uani 1 1 d . . . Cl1 Cl 0.58410(15) 0.08656(8) 0.77076(6) 0.0453(4) Uani 1 1 d . . . Cl2 Cl 0.76013(13) -0.02548(7) 0.67668(7) 0.0405(4) Uani 1 1 d . . . P1 P 0.58040(14) 0.00244(7) 0.55308(6) 0.0284(3) Uani 1 1 d . . . P2 P 0.44448(12) 0.12798(7) 0.63849(7) 0.0318(4) Uani 1 1 d . . . O1 O 0.4512(4) -0.1269(2) 0.60405(19) 0.0441(10) Uani 1 1 d . . . O2 O 0.6154(4) -0.0123(2) 0.4047(2) 0.0512(12) Uani 1 1 d . . . O3 O 0.2119(4) 0.1959(2) 0.6092(2) 0.0515(12) Uani 1 1 d . . . O4 O 0.6352(4) 0.2339(2) 0.6232(2) 0.0457(11) Uani 1 1 d . . . O5 O 0.2493(4) 0.0350(2) 0.39507(18) 0.0431(10) Uani 1 1 d . . . O6 O 0.2747(3) -0.0595(2) 0.46865(18) 0.0432(10) Uani 1 1 d . . . O7 O 0.4055(4) 0.10023(17) 0.43996(16) 0.0349(9) Uani 1 1 d . . . C1 C 0.6200(5) -0.0953(3) 0.5455(3) 0.0365(15) Uani 1 1 d . . . C2 C 0.7295(6) -0.1146(3) 0.5162(3) 0.0417(15) Uani 1 1 d . . . H2 H 0.7802 -0.0779 0.5008 0.05 Uiso 1 1 calc R . . C3 C 0.7589(7) -0.1881(4) 0.5110(3) 0.0561(19) Uani 1 1 d . . . H3 H 0.8297 -0.2011 0.491 0.067 Uiso 1 1 calc R . . C4 C 0.6870(7) -0.2425(4) 0.5344(3) 0.0577(19) Uani 1 1 d . . . H4 H 0.7085 -0.2921 0.53 0.069 Uiso 1 1 calc R . . C5 C 0.5843(7) -0.2244(3) 0.5641(3) 0.0543(17) Uani 1 1 d . . . H5 H 0.5357 -0.2621 0.5797 0.065 Uiso 1 1 calc R . . C6 C 0.5492(6) -0.1498(3) 0.5721(3) 0.0435(17) Uani 1 1 d . . . C7 C 0.3671(6) -0.1795(4) 0.6244(3) 0.060(2) Uani 1 1 d . . . H7A H 0.3369 -0.205 0.5859 0.09 Uiso 1 1 calc R . . H7B H 0.3041 -0.1547 0.6471 0.09 Uiso 1 1 calc R . . H7C H 0.4029 -0.2148 0.6541 0.09 Uiso 1 1 calc R . . C8 C 0.6827(5) 0.0511(3) 0.5002(3) 0.0332(13) Uani 1 1 d . . . C9 C 0.7595(6) 0.1005(3) 0.5300(3) 0.0434(16) Uani 1 1 d . . . H9 H 0.7545 0.11 0.5756 0.052 Uiso 1 1 calc R . . C10 C 0.8442(6) 0.1359(4) 0.4913(4) 0.0581(19) Uani 1 1 d . . . H10 H 0.898 0.1678 0.5114 0.07 Uiso 1 1 calc R . . C11 C 0.8487(7) 0.1237(4) 0.4229(4) 0.066(2) Uani 1 1 d . . . H11 H 0.9023 0.1504 0.3973 0.079 Uiso 1 1 calc R . . C12 C 0.7778(6) 0.0746(4) 0.3925(4) 0.0539(19) Uani 1 1 d . . . H12 H 0.7862 0.0642 0.3472 0.065 Uiso 1 1 calc R . . C13 C 0.6902(5) 0.0390(3) 0.4307(3) 0.0423(15) Uani 1 1 d . . . C14 C 0.6246(6) -0.0300(5) 0.3352(3) 0.085(3) Uani 1 1 d . . . H14A H 0.6098 0.0138 0.3091 0.128 Uiso 1 1 calc R . . H14B H 0.5681 -0.0675 0.324 0.128 Uiso 1 1 calc R . . H14C H 0.7022 -0.0481 0.3258 0.128 Uiso 1 1 calc R . . C15 C 0.3017(5) 0.0931(3) 0.6577(3) 0.0366(13) Uani 1 1 d . . . C16 C 0.2930(6) 0.0213(4) 0.6893(3) 0.0515(18) Uani 1 1 d . . . H16 H 0.3608 -0.0042 0.7012 0.062 Uiso 1 1 calc R . . C17 C 0.1840(7) -0.0098(4) 0.7021(4) 0.065(2) Uani 1 1 d . . . H17 H 0.1778 -0.0549 0.7245 0.078 Uiso 1 1 calc R . . C18 C 0.0841(7) 0.0278(4) 0.6806(3) 0.065(2) Uani 1 1 d . . . H18 H 0.011 0.0059 0.6871 0.078 Uiso 1 1 calc R . . C19 C 0.0897(6) 0.0958(4) 0.6502(3) 0.0611(17) Uani 1 1 d . . . H19 H 0.021 0.1199 0.6375 0.073 Uiso 1 1 calc R . . C20 C 0.1967(6) 0.1289(4) 0.6382(3) 0.0456(16) Uani 1 1 d . . . C21 C 0.1114(7) 0.2362(5) 0.5897(5) 0.095(3) Uani 1 1 d . . . H21A H 0.0888 0.2216 0.5453 0.143 Uiso 1 1 calc R . . H21B H 0.1287 0.2884 0.5902 0.143 Uiso 1 1 calc R . . H21C H 0.0484 0.226 0.6202 0.143 Uiso 1 1 calc R . . C22 C 0.4586(5) 0.2168(3) 0.6809(3) 0.0342(14) Uani 1 1 d . . . C23 C 0.3746(5) 0.2404(3) 0.7271(3) 0.0401(15) Uani 1 1 d . . . H23 H 0.313 0.209 0.7387 0.048 Uiso 1 1 calc R . . C24 C 0.3826(6) 0.3099(3) 0.7552(3) 0.0455(17) Uani 1 1 d . . . H24 H 0.3249 0.326 0.7848 0.055 Uiso 1 1 calc R . . C25 C 0.4759(6) 0.3562(3) 0.7399(3) 0.0488(18) Uani 1 1 d . . . H25 H 0.4797 0.4034 0.7588 0.059 Uiso 1 1 calc R . . C26 C 0.5643(6) 0.3326(3) 0.6964(3) 0.0517(18) Uani 1 1 d . . . H26 H 0.6277 0.3634 0.6869 0.062 Uiso 1 1 calc R . . C27 C 0.5559(5) 0.2621(3) 0.6674(3) 0.0415(15) Uani 1 1 d . . . C28 C 0.7325(7) 0.2819(4) 0.6040(4) 0.080(3) Uani 1 1 d . . . H28A H 0.7756 0.2591 0.5682 0.12 Uiso 1 1 calc R . . H28B H 0.7834 0.2891 0.6417 0.12 Uiso 1 1 calc R . . H28C H 0.7025 0.329 0.5894 0.12 Uiso 1 1 calc R . . C29 C 0.4271(5) 0.0086(3) 0.5221(2) 0.0286(13) Uani 1 1 d . . . H29 H 0.3775 -0.0113 0.5579 0.034 Uiso 1 1 calc R . . C30 C 0.3852(5) 0.0888(3) 0.5100(2) 0.0306(14) Uani 1 1 d . . . H30 H 0.3002 0.0901 0.5174 0.037 Uiso 1 1 calc R . . C31 C 0.4381(5) 0.1517(3) 0.5485(3) 0.0374(15) Uani 1 1 d . . . H31A H 0.3913 0.1962 0.5423 0.045 Uiso 1 1 calc R . . H31B H 0.5166 0.1616 0.532 0.045 Uiso 1 1 calc R . . C32 C 0.3891(5) -0.0308(3) 0.4586(2) 0.0337(14) Uani 1 1 d . . . H32 H 0.4453 -0.0684 0.4434 0.04 Uiso 1 1 calc R . . C33 C 0.3715(5) 0.0342(3) 0.4069(3) 0.0385(15) Uani 1 1 d . . . H33 H 0.4163 0.026 0.3657 0.046 Uiso 1 1 calc R . . C34 C 0.2026(6) -0.0366(4) 0.4145(3) 0.0470(16) Uani 1 1 d . . . C35 C 0.2139(6) -0.0895(3) 0.3562(3) 0.0513(18) Uani 1 1 d . . . H35A H 0.2946 -0.0924 0.3427 0.077 Uiso 1 1 calc R . . H35B H 0.1673 -0.0717 0.3195 0.077 Uiso 1 1 calc R . . H35C H 0.187 -0.1379 0.3693 0.077 Uiso 1 1 calc R . . C36 C 0.0787(6) -0.0270(4) 0.4385(3) 0.069(2) Uani 1 1 d . . . H36A H 0.0756 0.0126 0.4706 0.104 Uiso 1 1 calc R . . H36B H 0.0522 -0.0723 0.4589 0.104 Uiso 1 1 calc R . . H36C H 0.029 -0.0151 0.4012 0.104 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 0.0293(2) 0.0322(2) 0.02491(19) 0.00197(18) -0.0015(2) -0.00092(19) Cl1 0.0491(9) 0.0602(9) 0.0267(7) -0.0030(6) -0.0036(8) 0.0063(9) Cl2 0.0325(8) 0.0469(9) 0.0420(9) 0.0014(6) -0.0065(6) 0.0060(6) P1 0.0312(8) 0.0291(7) 0.0248(7) 0.0007(5) -0.0006(7) 0.0008(7) P2 0.0318(9) 0.0345(8) 0.0293(8) -0.0037(6) -0.0008(6) 0.0009(6) O1 0.053(3) 0.038(2) 0.041(2) 0.0079(18) 0.004(2) 0.000(2) O2 0.056(3) 0.064(3) 0.033(2) -0.008(2) 0.010(2) 0.001(2) O3 0.040(3) 0.065(3) 0.050(3) -0.002(2) -0.007(2) 0.011(2) O4 0.043(3) 0.043(2) 0.051(3) -0.006(2) 0.008(2) -0.005(2) O5 0.044(3) 0.038(2) 0.047(2) 0.0013(18) -0.012(2) 0.001(2) O6 0.041(2) 0.055(3) 0.034(2) -0.0010(19) -0.0065(19) -0.010(2) O7 0.045(2) 0.0311(19) 0.028(2) 0.0024(15) -0.004(2) 0.002(2) C1 0.043(4) 0.031(3) 0.035(3) -0.002(3) -0.009(3) 0.004(3) C2 0.044(4) 0.041(4) 0.040(4) -0.003(3) 0.005(3) 0.001(3) C3 0.070(5) 0.054(4) 0.044(4) -0.006(3) 0.005(4) 0.010(4) C4 0.079(6) 0.035(4) 0.059(5) 0.002(3) 0.001(4) 0.021(4) C5 0.070(5) 0.037(4) 0.056(4) 0.000(3) -0.009(4) -0.002(4) C6 0.067(5) 0.037(4) 0.026(3) 0.000(3) -0.005(3) 0.003(3) C7 0.058(5) 0.059(4) 0.062(5) -0.005(4) -0.004(4) -0.018(4) C8 0.032(3) 0.034(3) 0.034(3) 0.005(3) 0.006(3) 0.010(3) C9 0.046(4) 0.041(4) 0.043(4) 0.007(3) 0.001(3) -0.009(3) C10 0.045(4) 0.054(4) 0.075(5) 0.006(4) 0.015(4) -0.009(3) C11 0.061(5) 0.060(5) 0.076(6) 0.012(4) 0.042(4) 0.000(4) C12 0.055(5) 0.059(5) 0.048(4) 0.004(3) 0.022(4) -0.003(4) C13 0.037(4) 0.051(4) 0.039(4) 0.004(3) 0.006(3) 0.011(3) C14 0.064(5) 0.145(7) 0.046(4) -0.023(5) 0.008(4) -0.012(5) C15 0.029(3) 0.048(3) 0.033(3) -0.013(3) -0.001(3) -0.004(3) C16 0.051(4) 0.064(4) 0.040(4) -0.012(3) 0.018(3) -0.012(3) C17 0.062(5) 0.074(5) 0.060(5) 0.002(4) 0.011(4) -0.035(4) C18 0.027(4) 0.104(6) 0.064(5) -0.004(4) -0.002(4) -0.017(4) C19 0.042(4) 0.073(5) 0.068(5) 0.008(4) 0.003(5) -0.008(4) C20 0.045(4) 0.056(4) 0.035(4) -0.005(3) -0.002(3) 0.000(3) C21 0.050(6) 0.104(6) 0.131(8) 0.029(6) -0.014(5) 0.009(5) C22 0.039(4) 0.037(3) 0.026(3) 0.001(2) -0.005(3) -0.001(3) C23 0.040(4) 0.051(4) 0.029(3) 0.003(3) 0.001(3) 0.003(3) C24 0.050(5) 0.051(4) 0.035(4) -0.016(3) 0.001(3) 0.012(3) C25 0.069(5) 0.043(4) 0.034(4) -0.013(3) 0.000(3) 0.003(4) C26 0.062(5) 0.047(4) 0.046(4) 0.000(3) -0.015(4) -0.017(3) C27 0.054(4) 0.033(3) 0.037(4) -0.001(3) 0.000(3) 0.003(3) C28 0.074(6) 0.066(5) 0.100(6) -0.011(4) 0.029(5) -0.030(5) C29 0.031(3) 0.030(3) 0.025(3) 0.002(2) -0.004(3) -0.002(3) C30 0.034(4) 0.036(3) 0.022(3) -0.002(2) 0.010(2) 0.001(3) C31 0.037(4) 0.041(3) 0.034(3) -0.004(3) 0.007(3) -0.001(3) C32 0.027(4) 0.043(3) 0.030(3) 0.000(2) 0.000(2) 0.007(3) C33 0.053(4) 0.029(3) 0.034(3) 0.002(3) -0.003(3) 0.002(3) C34 0.047(4) 0.051(4) 0.043(4) 0.000(3) -0.014(3) -0.006(3) C35 0.080(5) 0.041(3) 0.033(4) -0.002(3) -0.012(3) -0.014(3) C36 0.041(4) 0.099(6) 0.067(5) 0.000(4) -0.002(4) -0.008(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 P2 2.2457(16) . ? Pd1 P1 2.2687(14) . ? Pd1 Cl1 2.3458(14) . ? Pd1 Cl2 2.3621(16) . ? P1 C8 1.802(5) . ? P1 C1 1.822(5) . ? P1 C29 1.856(6) . ? P2 C15 1.786(5) . ? P2 C22 1.816(5) . ? P2 C31 1.851(5) . ? O1 C6 1.351(7) . ? O1 C7 1.407(7) . ? O2 C13 1.359(7) . ? O2 C14 1.429(7) . ? O3 C20 1.348(7) . ? O3 C21 1.410(8) . ? O4 C27 1.363(7) . ? O4 C28 1.456(7) . ? O5 C33 1.412(7) . ? O5 C34 1.447(7) . ? O6 C32 1.416(6) . ? O6 C34 1.420(7) . ? O7 C33 1.414(6) . ? O7 C30 1.434(6) . ? C1 C6 1.376(8) . ? C1 C2 1.422(8) . ? C2 C3 1.367(8) . ? C2 H2 0.93 . ? C3 C4 1.360(9) . ? C3 H3 0.93 . ? C4 C5 1.352(9) . ? C4 H4 0.93 . ? C5 C6 1.408(8) . ? C5 H5 0.93 . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 C9 1.382(7) . ? C8 C13 1.408(8) . ? C9 C10 1.392(8) . ? C9 H9 0.93 . ? C10 C11 1.387(10) . ? C10 H10 0.93 . ? C11 C12 1.343(9) . ? C11 H11 0.93 . ? C12 C13 1.411(8) . ? C12 H12 0.93 . ? C14 H14A 0.96 . ? C14 H14B 0.96 . ? C14 H14C 0.96 . ? C15 C20 1.414(8) . ? C15 C16 1.440(8) . ? C16 C17 1.386(8) . ? C16 H16 0.93 . ? C17 C18 1.392(10) . ? C17 H17 0.93 . ? C18 C19 1.369(9) . ? C18 H18 0.93 . ? C19 C20 1.377(8) . ? C19 H19 0.93 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 C23 1.396(7) . ? C22 C27 1.402(7) . ? C23 C24 1.374(8) . ? C23 H23 0.93 . ? C24 C25 1.384(8) . ? C24 H24 0.93 . ? C25 C26 1.397(9) . ? C25 H25 0.93 . ? C26 C27 1.398(7) . ? C26 H26 0.93 . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 C32 1.517(7) . ? C29 C30 1.540(7) . ? C29 H29 0.98 . ? C30 C31 1.495(7) . ? C30 H30 0.98 . ? C31 H31A 0.97 . ? C31 H31B 0.97 . ? C32 C33 1.572(7) . ? C32 H32 0.98 . ? C33 H33 0.98 . ? C34 C36 1.501(9) . ? C34 C35 1.511(8) . ? C35 H35A 0.96 . ? C35 H35B 0.96 . ? C35 H35C 0.96 . ? C36 H36A 0.96 . ? C36 H36B 0.96 . ? C36 H36C 0.96 . ? 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 P2 Pd1 P1 91.27(5) . . ? P2 Pd1 Cl1 87.49(5) . . ? P1 Pd1 Cl1 174.71(6) . . ? P2 Pd1 Cl2 172.38(5) . . ? P1 Pd1 Cl2 89.10(5) . . ? Cl1 Pd1 Cl2 92.81(5) . . ? C8 P1 C1 105.1(3) . . ? C8 P1 C29 112.6(2) . . ? C1 P1 C29 105.2(2) . . ? C8 P1 Pd1 110.28(19) . . ? C1 P1 Pd1 113.96(18) . . ? C29 P1 Pd1 109.65(17) . . ? C15 P2 C22 106.8(3) . . ? C15 P2 C31 104.8(3) . . ? C22 P2 C31 104.8(2) . . ? C15 P2 Pd1 113.9(2) . . ? C22 P2 Pd1 114.83(19) . . ? C31 P2 Pd1 110.90(19) . . ? C6 O1 C7 119.7(5) . . ? C13 O2 C14 118.5(5) . . ? C20 O3 C21 118.3(5) . . ? C27 O4 C28 117.1(5) . . ? C33 O5 C34 107.9(4) . . ? C32 O6 C34 108.6(4) . . ? C33 O7 C30 107.0(4) . . ? C6 C1 C2 120.0(5) . . ? C6 C1 P1 120.7(5) . . ? C2 C1 P1 119.2(4) . . ? C3 C2 C1 118.8(6) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C4 C3 C2 121.5(7) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 119.9(6) . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C4 C5 C6 121.7(7) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? O1 C6 C1 116.8(5) . . ? O1 C6 C5 125.4(6) . . ? C1 C6 C5 117.9(6) . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 119.1(5) . . ? C9 C8 P1 117.9(4) . . ? C13 C8 P1 122.9(5) . . ? C8 C9 C10 119.6(6) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C11 C10 C9 120.1(7) . . ? C11 C10 H10 120 . . ? C9 C10 H10 120 . . ? C12 C11 C10 121.9(6) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C11 C12 C13 118.7(7) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? O2 C13 C8 116.5(5) . . ? O2 C13 C12 123.0(6) . . ? C8 C13 C12 120.4(6) . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 118.1(5) . . ? C20 C15 P2 123.4(4) . . ? C16 C15 P2 118.2(4) . . ? C17 C16 C15 120.3(6) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 118.7(7) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? C19 C18 C17 122.2(7) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 120.3(7) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? O3 C20 C19 125.0(6) . . ? O3 C20 C15 114.7(5) . . ? C19 C20 C15 120.3(6) . . ? O3 C21 H21A 109.5 . . ? O3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 119.6(5) . . ? C23 C22 P2 121.0(4) . . ? C27 C22 P2 119.4(4) . . ? C24 C23 C22 120.1(6) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.5(6) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C26 120.6(5) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C27 119.0(6) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? O4 C27 C26 124.2(5) . . ? O4 C27 C22 115.7(5) . . ? C26 C27 C22 120.1(6) . . ? O4 C28 H28A 109.5 . . ? O4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C29 C30 102.5(4) . . ? C32 C29 P1 121.4(4) . . ? C30 C29 P1 113.6(4) . . ? C32 C29 H29 106.1 . . ? C30 C29 H29 106.1 . . ? P1 C29 H29 106.1 . . ? O7 C30 C31 109.3(4) . . ? O7 C30 C29 103.7(4) . . ? C31 C30 C29 120.1(5) . . ? O7 C30 H30 107.7 . . ? C31 C30 H30 107.7 . . ? C29 C30 H30 107.7 . . ? C30 C31 P2 110.1(4) . . ? C30 C31 H31A 109.6 . . ? P2 C31 H31A 109.6 . . ? C30 C31 H31B 109.6 . . ? P2 C31 H31B 109.6 . . ? H31A C31 H31B 108.2 . . ? O6 C32 C29 108.3(4) . . ? O6 C32 C33 104.3(4) . . ? C29 C32 C33 103.9(4) . . ? O6 C32 H32 113.2 . . ? C29 C32 H32 113.2 . . ? C33 C32 H32 113.2 . . ? O5 C33 O7 109.8(4) . . ? O5 C33 C32 104.1(5) . . ? O7 C33 C32 106.4(4) . . ? O5 C33 H33 112 . . ? O7 C33 H33 112 . . ? C32 C33 H33 112 . . ? O6 C34 O5 104.5(5) . . ? O6 C34 C36 109.6(5) . . ? O5 C34 C36 109.2(6) . . ? O6 C34 C35 110.9(5) . . ? O5 C34 C35 108.7(5) . . ? C36 C34 C35 113.5(5) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ?