# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Partha Mukherjee' _publ_contact_author_name 'Partha Mukherjee' _publ_contact_author_address ; Bangalore Karnataka India 560012 ; _publ_contact_author_email psm@ipc.iisc.ernet.in # Attachment '- bs-123.cif' data_complex-1 _database_code_depnum_ccdc_archive 'CCDC 790087' #TrackingRef '- bs-123.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H66 P4 Pd2' _chemical_formula_sum 'C60 H66 P4 Pd2' _chemical_formula_weight 1123.81 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' 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 P21/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 9.935(2) _cell_length_b 20.917(4) _cell_length_c 12.996(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.57(3) _cell_angle_gamma 90.00 _cell_volume 2636.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 28.0 _exptl_crystal_description 'needle shape' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.7629 _exptl_absorpt_correction_T_max 0.9058 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 0.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12406 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6618 _reflns_number_gt 5210 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker kappa apex ccd' _computing_cell_refinement 'Bruker kappa apex ccd' _computing_data_reduction 'Bruker saint' _computing_structure_solution shelxs-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ortep-III _computing_publication_material WinGX1.80.05 _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^ > 2\s(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^)+(0.0748P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6618 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1042 _refine_ls_wR_factor_gt 0.0977 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _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 C10A C 0.4483(6) 0.0449(2) 0.8009(4) 0.0263(11) Uani 0.54 1 d P . . C10B C 0.5417(8) 0.0632(3) 0.7844(5) 0.0297(15) Uani 0.46 1 d P . . Pd1 Pd 0.504940(19) 0.118033(8) 0.447342(14) 0.01547(8) Uani 1 1 d . . . P1 P 0.61641(7) 0.16694(3) 0.32916(5) 0.01760(15) Uani 1 1 d . . . P2 P 0.39329(7) 0.08570(3) 0.57714(5) 0.02032(16) Uani 1 1 d . . . C1 C 0.7739(3) 0.13170(13) 0.3011(2) 0.0237(6) Uani 1 1 d . . . C2 C 0.9006(3) 0.13501(17) 0.3900(3) 0.0307(7) Uani 1 1 d . . . C3 C 0.5142(3) 0.18125(13) 0.1963(2) 0.0249(6) Uani 1 1 d . . . C4 C 0.4875(4) 0.12165(14) 0.1282(2) 0.0303(7) Uani 1 1 d . . . C5 C 0.6704(3) 0.24711(12) 0.3768(2) 0.0257(6) Uani 1 1 d . . . C6 C 0.5564(4) 0.28462(14) 0.4114(2) 0.0305(7) Uani 1 1 d . . . C7 C 0.3374(3) 0.15800(12) 0.6330(2) 0.0237(6) Uani 1 1 d . . . C8 C 0.2471(4) 0.20110(14) 0.5518(3) 0.0294(7) Uani 1 1 d . . . C9 C 0.4994(4) 0.0428(2) 0.6901(3) 0.0631(14) Uani 1 1 d . . . C11 C 0.2400(3) 0.03609(14) 0.5365(3) 0.0308(7) Uani 1 1 d . . . C12 C 0.1382(3) 0.03800(14) 0.6084(2) 0.0257(6) Uani 1 1 d . . . C13 C 0.6738(3) 0.13207(12) 0.5616(2) 0.0209(6) Uani 1 1 d . . . C14 C 0.7747(3) 0.13967(12) 0.6316(2) 0.0197(5) Uani 1 1 d . . . C15 C 0.8978(3) 0.14732(11) 0.71259(19) 0.0178(5) Uani 1 1 d . . . C16 C 0.9580(3) 0.09295(12) 0.77505(19) 0.0176(5) Uani 1 1 d . . . C17 C 1.0829(3) 0.10175(12) 0.8525(2) 0.0204(5) Uani 1 1 d . . . C18 C 1.1440(3) 0.16394(13) 0.8665(2) 0.0234(6) Uani 1 1 d . . . C19 C 1.0851(3) 0.21437(13) 0.8067(2) 0.0250(6) Uani 1 1 d . . . C20 C 0.9629(3) 0.20562(12) 0.7291(2) 0.0226(6) Uani 1 1 d . . . C21 C 0.3311(3) 0.10455(12) 0.3362(2) 0.0211(6) Uani 1 1 d . . . C22 C 0.2268(3) 0.09504(12) 0.2710(2) 0.0196(5) Uani 1 1 d . . . C23 C 0.1035(3) 0.08356(11) 0.1921(2) 0.0184(5) Uani 1 1 d . . . C24 C 0.0408(3) 0.13243(13) 0.1277(2) 0.0214(6) Uani 1 1 d . . . C25 C -0.0817(3) 0.12323(12) 0.0512(2) 0.0248(6) Uani 1 1 d . . . C26 C -0.1440(3) 0.06433(13) 0.0385(2) 0.0221(6) Uani 1 1 d . . . C27 C -0.0836(3) 0.01129(12) 0.10127(19) 0.0193(5) Uani 1 1 d . . . C28 C 0.0415(3) 0.02042(12) 0.17911(19) 0.0182(5) Uani 1 1 d . . . C29 C 0.1009(3) -0.03195(12) 0.2386(2) 0.0186(5) Uani 1 1 d . . . C30 C -0.1427(3) -0.04938(12) 0.0879(2) 0.0192(5) Uani 1 1 d . . . H20 H 0.921(3) 0.2403(14) 0.685(2) 0.026(8) Uiso 1 1 d . . . H25 H -0.129(3) 0.1582(15) 0.008(2) 0.025(8) Uiso 1 1 d . . . H19 H 1.127(3) 0.2525(14) 0.812(2) 0.021(7) Uiso 1 1 d . . . H18 H 1.221(3) 0.1671(14) 0.919(2) 0.025(8) Uiso 1 1 d . . . H24 H 0.090(3) 0.1752(14) 0.135(2) 0.025(8) Uiso 1 1 d . . . H30 H -0.224(3) -0.0574(12) 0.037(2) 0.015(7) Uiso 1 1 d . . . H26 H -0.223(4) 0.0565(15) -0.014(3) 0.036(9) Uiso 1 1 d . . . H29 H 0.176(3) -0.0269(13) 0.286(2) 0.013(7) Uiso 1 1 d . . . H12A H 0.103(4) 0.0829(18) 0.612(3) 0.045(10) Uiso 1 1 d . . . H6A H 0.519(3) 0.2607(18) 0.467(3) 0.042(10) Uiso 1 1 d . . . H3A H 0.433(4) 0.1989(15) 0.204(2) 0.028(8) Uiso 1 1 d . . . H1B H 0.787(3) 0.1556(16) 0.243(3) 0.036(9) Uiso 1 1 d . . . H8A H 0.294(4) 0.2168(16) 0.496(3) 0.038(9) Uiso 1 1 d . . . H3B H 0.557(3) 0.2162(16) 0.165(3) 0.038(9) Uiso 1 1 d . . . H5B H 0.708(3) 0.2734(16) 0.316(3) 0.041(9) Uiso 1 1 d . . . H2C H 0.968(4) 0.1127(16) 0.369(3) 0.043(11) Uiso 1 1 d . . . H1A H 0.752(3) 0.0860(15) 0.282(2) 0.028(8) Uiso 1 1 d . . . H12C H 0.066(3) 0.0068(15) 0.591(2) 0.032(8) Uiso 1 1 d . . . H8B H 0.167(4) 0.1795(17) 0.523(3) 0.045(10) Uiso 1 1 d . . . H2B H 0.918(4) 0.1786(19) 0.397(3) 0.050(11) Uiso 1 1 d . . . H4A H 0.569(5) 0.1064(18) 0.119(3) 0.052(12) Uiso 1 1 d . . . H12B H 0.188(3) 0.0244(17) 0.686(3) 0.042(9) Uiso 1 1 d . . . H6C H 0.475(4) 0.2902(15) 0.357(3) 0.033(9) Uiso 1 1 d . . . H11A H 0.196(5) 0.048(2) 0.464(4) 0.079(15) Uiso 1 1 d . . . H5A H 0.746(3) 0.2394(16) 0.437(3) 0.038(9) Uiso 1 1 d . . . H6B H 0.591(4) 0.3263(18) 0.432(3) 0.042(10) Uiso 1 1 d . . . H2A H 0.882(4) 0.1149(15) 0.453(3) 0.038(10) Uiso 1 1 d . . . H4B H 0.437(4) 0.1369(17) 0.054(3) 0.040(9) Uiso 1 1 d . . . H8C H 0.221(4) 0.241(2) 0.586(3) 0.060(12) Uiso 1 1 d . . . H4C H 0.446(4) 0.0855(17) 0.163(3) 0.040(9) Uiso 1 1 d . . . H11B H 0.271(4) -0.0072(18) 0.531(3) 0.047(10) Uiso 1 1 d . . . H7A H 0.422(4) 0.1773(15) 0.665(3) 0.035(9) Uiso 1 1 d . . . H7B H 0.295(3) 0.1458(16) 0.693(3) 0.038(9) Uiso 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 C10A 0.024(4) 0.031(3) 0.023(3) 0.007(2) 0.002(2) 0.003(2) C10B 0.033(5) 0.038(3) 0.016(3) 0.000(2) -0.002(3) 0.008(3) Pd1 0.01085(15) 0.01460(10) 0.01966(11) 0.00156(6) 0.00048(8) -0.00035(6) P1 0.0153(4) 0.0158(3) 0.0206(3) 0.0012(2) 0.0016(3) -0.0014(2) P2 0.0167(4) 0.0177(3) 0.0271(3) 0.0041(2) 0.0059(3) 0.0025(2) C1 0.0209(17) 0.0244(13) 0.0255(14) 0.0026(10) 0.0044(12) 0.0011(11) C2 0.0201(19) 0.0393(17) 0.0338(16) 0.0008(13) 0.0080(13) 0.0043(13) C3 0.0201(18) 0.0250(13) 0.0279(14) 0.0065(11) 0.0012(12) -0.0017(11) C4 0.029(2) 0.0341(16) 0.0259(15) -0.0007(12) 0.0025(13) -0.0051(13) C5 0.0267(18) 0.0192(12) 0.0306(14) -0.0024(10) 0.0050(13) -0.0045(11) C6 0.036(2) 0.0230(14) 0.0322(16) -0.0022(11) 0.0058(14) 0.0038(12) C7 0.0256(18) 0.0195(11) 0.0239(13) -0.0039(10) 0.0008(12) -0.0002(11) C8 0.026(2) 0.0243(14) 0.0367(16) -0.0005(12) 0.0037(14) 0.0059(12) C9 0.036(3) 0.094(3) 0.069(3) 0.062(2) 0.031(2) 0.038(2) C11 0.029(2) 0.0266(14) 0.0417(18) -0.0094(12) 0.0181(15) -0.0094(12) C12 0.0189(18) 0.0307(15) 0.0279(15) 0.0001(11) 0.0061(12) -0.0038(12) C13 0.0223(17) 0.0177(11) 0.0226(13) 0.0019(9) 0.0049(11) 0.0012(10) C14 0.0149(15) 0.0209(11) 0.0217(12) 0.0002(10) 0.0008(11) 0.0023(10) C15 0.0119(15) 0.0240(12) 0.0161(11) -0.0014(9) 0.0003(10) 0.0026(10) C16 0.0161(15) 0.0209(11) 0.0153(11) -0.0017(9) 0.0019(10) 0.0023(10) C17 0.0168(16) 0.0226(11) 0.0203(12) -0.0036(9) 0.0009(11) -0.0001(10) C18 0.0170(17) 0.0265(13) 0.0230(13) -0.0050(10) -0.0037(11) -0.0019(11) C19 0.0251(18) 0.0212(12) 0.0267(14) -0.0040(10) 0.0012(12) -0.0031(11) C20 0.0226(17) 0.0205(12) 0.0235(13) 0.0003(10) 0.0025(11) 0.0016(10) C21 0.0178(16) 0.0187(11) 0.0266(13) 0.0004(10) 0.0044(12) -0.0010(10) C22 0.0168(16) 0.0174(11) 0.0237(13) 0.0000(9) 0.0022(11) -0.0006(10) C23 0.0115(15) 0.0231(12) 0.0206(12) -0.0008(9) 0.0035(10) 0.0000(9) C24 0.0166(16) 0.0215(12) 0.0259(13) 0.0024(10) 0.0044(11) 0.0020(10) C25 0.0248(19) 0.0248(13) 0.0240(14) 0.0038(10) 0.0035(12) 0.0057(11) C26 0.0143(17) 0.0271(13) 0.0230(13) 0.0007(10) -0.0004(11) 0.0041(10) C27 0.0175(16) 0.0227(12) 0.0167(11) -0.0001(9) 0.0015(10) 0.0021(10) C28 0.0142(15) 0.0220(11) 0.0186(11) -0.0005(9) 0.0041(10) 0.0022(10) C29 0.0138(16) 0.0245(12) 0.0165(12) -0.0042(9) 0.0013(10) -0.0003(10) C30 0.0119(15) 0.0250(12) 0.0176(12) -0.0015(9) -0.0035(10) 0.0007(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C10A C10B 1.067(9) . ? C10A C9 1.628(6) . ? C10B C9 1.279(7) . ? Pd1 C13 2.005(3) . ? Pd1 C21 2.016(3) . ? Pd1 P2 2.3126(9) . ? Pd1 P1 2.3178(8) . ? P1 C5 1.827(3) . ? P1 C3 1.827(3) . ? P1 C1 1.837(3) . ? P2 C7 1.816(3) . ? P2 C11 1.823(3) . ? P2 C9 1.842(3) . ? C1 C2 1.514(4) . ? C1 H1B 0.94(3) . ? C1 H1A 1.00(3) . ? C2 H2C 0.91(4) . ? C2 H2B 0.93(4) . ? C2 H2A 0.98(4) . ? C3 C4 1.518(4) . ? C3 H3A 0.91(3) . ? C3 H3B 0.97(3) . ? C4 H4A 0.91(4) . ? C4 H4B 1.04(4) . ? C4 H4C 1.02(4) . ? C5 C6 1.524(4) . ? C5 H5B 1.09(4) . ? C5 H5A 0.97(3) . ? C6 H6A 1.01(3) . ? C6 H6C 0.96(3) . ? C6 H6B 0.95(4) . ? C7 C8 1.523(4) . ? C7 H7A 0.95(4) . ? C7 H7B 1.00(4) . ? C8 H8A 1.00(3) . ? C8 H8B 0.92(4) . ? C8 H8C 1.01(4) . ? C11 C12 1.520(4) . ? C11 H11A 0.98(5) . ? C11 H11B 0.97(4) . ? C12 H12A 1.01(4) . ? C12 H12C 0.96(3) . ? C12 H12B 1.06(4) . ? C13 C14 1.209(4) . ? C14 C15 1.439(4) . ? C15 C20 1.375(4) . ? C15 C16 1.449(3) . ? C16 C29 1.399(4) 3_656 ? C16 C17 1.430(4) . ? C17 C30 1.397(4) 3_656 ? C17 C18 1.430(4) . ? C18 C19 1.364(4) . ? C18 H18 0.91(3) . ? C19 C20 1.412(4) . ? C19 H19 0.89(3) . ? C20 H20 0.96(3) . ? C21 C22 1.204(4) . ? C22 C23 1.437(4) . ? C23 C24 1.380(4) . ? C23 C28 1.451(3) . ? C24 C25 1.407(4) . ? C24 H24 1.01(3) . ? C25 C26 1.372(4) . ? C25 H25 0.98(3) . ? C26 C27 1.429(4) . ? C26 H26 0.93(3) . ? C27 C30 1.393(4) . ? C27 C28 1.434(4) . ? C28 C29 1.395(4) . ? C29 C16 1.399(4) 3_656 ? C29 H29 0.87(3) . ? C30 C17 1.397(4) 3_656 ? C30 H30 0.95(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 C10B C10A C9 51.7(4) . . ? C10A C10B C9 87.4(6) . . ? C13 Pd1 C21 178.02(11) . . ? C13 Pd1 P2 87.70(8) . . ? C21 Pd1 P2 90.56(8) . . ? C13 Pd1 P1 88.99(8) . . ? C21 Pd1 P1 92.59(8) . . ? P2 Pd1 P1 170.63(2) . . ? C5 P1 C3 103.39(13) . . ? C5 P1 C1 103.64(13) . . ? C3 P1 C1 101.53(14) . . ? C5 P1 Pd1 109.14(10) . . ? C3 P1 Pd1 116.83(10) . . ? C1 P1 Pd1 120.34(9) . . ? C7 P2 C11 106.32(15) . . ? C7 P2 C9 104.97(18) . . ? C11 P2 C9 104.53(19) . . ? C7 P2 Pd1 106.57(10) . . ? C11 P2 Pd1 117.25(11) . . ? C9 P2 Pd1 116.19(11) . . ? C2 C1 P1 115.6(2) . . ? C2 C1 H1B 111(2) . . ? P1 C1 H1B 103(2) . . ? C2 C1 H1A 109.3(17) . . ? P1 C1 H1A 106.4(17) . . ? H1B C1 H1A 112(3) . . ? C1 C2 H2C 107(2) . . ? C1 C2 H2B 103(2) . . ? H2C C2 H2B 113(3) . . ? C1 C2 H2A 110(2) . . ? H2C C2 H2A 108(3) . . ? H2B C2 H2A 114(3) . . ? C4 C3 P1 114.0(2) . . ? C4 C3 H3A 110(2) . . ? P1 C3 H3A 106.7(19) . . ? C4 C3 H3B 114.4(19) . . ? P1 C3 H3B 108.1(19) . . ? H3A C3 H3B 102(3) . . ? C3 C4 H4A 109(2) . . ? C3 C4 H4B 106(2) . . ? H4A C4 H4B 104(3) . . ? C3 C4 H4C 112.8(19) . . ? H4A C4 H4C 106(3) . . ? H4B C4 H4C 119(3) . . ? C6 C5 P1 113.0(2) . . ? C6 C5 H5B 110.2(18) . . ? P1 C5 H5B 109.7(18) . . ? C6 C5 H5A 110(2) . . ? P1 C5 H5A 104(2) . . ? H5B C5 H5A 110(3) . . ? C5 C6 H6A 112(2) . . ? C5 C6 H6C 114(2) . . ? H6A C6 H6C 102(3) . . ? C5 C6 H6B 108(2) . . ? H6A C6 H6B 115(3) . . ? H6C C6 H6B 107(3) . . ? C8 C7 P2 113.6(2) . . ? C8 C7 H7A 113(2) . . ? P2 C7 H7A 102(2) . . ? C8 C7 H7B 114(2) . . ? P2 C7 H7B 108.4(19) . . ? H7A C7 H7B 104(3) . . ? C7 C8 H8A 114(2) . . ? C7 C8 H8B 109(2) . . ? H8A C8 H8B 111(3) . . ? C7 C8 H8C 111(2) . . ? H8A C8 H8C 104(3) . . ? H8B C8 H8C 108(3) . . ? C10B C9 C10A 40.9(4) . . ? C10B C9 P2 127.8(4) . . ? C10A C9 P2 117.2(3) . . ? C12 C11 P2 115.6(2) . . ? C12 C11 H11A 112(3) . . ? P2 C11 H11A 108(3) . . ? C12 C11 H11B 110(2) . . ? P2 C11 H11B 107(2) . . ? H11A C11 H11B 104(3) . . ? C11 C12 H12A 110(2) . . ? C11 C12 H12C 113.5(19) . . ? H12A C12 H12C 113(3) . . ? C11 C12 H12B 110.0(18) . . ? H12A C12 H12B 107(3) . . ? H12C C12 H12B 103(3) . . ? C14 C13 Pd1 178.7(2) . . ? C13 C14 C15 177.8(3) . . ? C20 C15 C14 120.6(2) . . ? C20 C15 C16 119.1(2) . . ? C14 C15 C16 120.3(2) . . ? C29 C16 C17 118.8(2) 3_656 . ? C29 C16 C15 122.3(2) 3_656 . ? C17 C16 C15 118.9(2) . . ? C30 C17 C16 119.2(2) 3_656 . ? C30 C17 C18 121.7(3) 3_656 . ? C16 C17 C18 119.1(2) . . ? C19 C18 C17 120.9(3) . . ? C19 C18 H18 123.9(19) . . ? C17 C18 H18 115.2(19) . . ? C18 C19 C20 120.2(3) . . ? C18 C19 H19 120.7(19) . . ? C20 C19 H19 119.0(18) . . ? C15 C20 C19 121.9(2) . . ? C15 C20 H20 116.8(18) . . ? C19 C20 H20 121.4(18) . . ? C22 C21 Pd1 178.3(2) . . ? C21 C22 C23 179.1(3) . . ? C24 C23 C22 120.7(2) . . ? C24 C23 C28 118.7(2) . . ? C22 C23 C28 120.6(2) . . ? C23 C24 C25 122.2(3) . . ? C23 C24 H24 116.7(17) . . ? C25 C24 H24 121.0(17) . . ? C26 C25 C24 120.4(2) . . ? C26 C25 H25 116.9(18) . . ? C24 C25 H25 122.7(18) . . ? C25 C26 C27 120.4(3) . . ? C25 C26 H26 122(2) . . ? C27 C26 H26 117(2) . . ? C30 C27 C26 121.5(2) . . ? C30 C27 C28 119.1(2) . . ? C26 C27 C28 119.4(2) . . ? C29 C28 C27 118.9(2) . . ? C29 C28 C23 122.2(2) . . ? C27 C28 C23 118.9(2) . . ? C28 C29 C16 122.1(3) . 3_656 ? C28 C29 H29 119.6(18) . . ? C16 C29 H29 118.3(18) 3_656 . ? C27 C30 C17 121.9(2) . 3_656 ? C27 C30 H30 121.6(16) . . ? C17 C30 H30 116.5(16) 3_656 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Pd1 P1 C5 -56.89(13) . . . . ? C21 Pd1 P1 C5 121.91(13) . . . . ? P2 Pd1 P1 C5 12.4(2) . . . . ? C13 Pd1 P1 C3 -173.65(13) . . . . ? C21 Pd1 P1 C3 5.16(13) . . . . ? P2 Pd1 P1 C3 -104.37(18) . . . . ? C13 Pd1 P1 C1 62.60(13) . . . . ? C21 Pd1 P1 C1 -118.59(13) . . . . ? P2 Pd1 P1 C1 131.88(17) . . . . ? C13 Pd1 P2 C7 82.38(12) . . . . ? C21 Pd1 P2 C7 -96.68(12) . . . . ? P1 Pd1 P2 C7 13.0(2) . . . . ? C13 Pd1 P2 C11 -158.74(14) . . . . ? C21 Pd1 P2 C11 22.20(14) . . . . ? P1 Pd1 P2 C11 131.88(19) . . . . ? C13 Pd1 P2 C9 -34.1(2) . . . . ? C21 Pd1 P2 C9 146.8(2) . . . . ? P1 Pd1 P2 C9 -103.5(2) . . . . ? C5 P1 C1 C2 52.2(3) . . . . ? C3 P1 C1 C2 159.3(2) . . . . ? Pd1 P1 C1 C2 -70.0(2) . . . . ? C5 P1 C3 C4 165.0(2) . . . . ? C1 P1 C3 C4 57.7(3) . . . . ? Pd1 P1 C3 C4 -75.2(3) . . . . ? C3 P1 C5 C6 77.6(2) . . . . ? C1 P1 C5 C6 -176.7(2) . . . . ? Pd1 P1 C5 C6 -47.4(2) . . . . ? C11 P2 C7 C8 -69.7(3) . . . . ? C9 P2 C7 C8 179.9(3) . . . . ? Pd1 P2 C7 C8 56.1(2) . . . . ? C10A C10B C9 P2 89.3(6) . . . . ? C10B C10A C9 P2 -117.4(6) . . . . ? C7 P2 C9 C10B -9.2(6) . . . . ? C11 P2 C9 C10B -120.9(6) . . . . ? Pd1 P2 C9 C10B 108.2(5) . . . . ? C7 P2 C9 C10A 38.2(4) . . . . ? C11 P2 C9 C10A -73.5(4) . . . . ? Pd1 P2 C9 C10A 155.6(3) . . . . ? C7 P2 C11 C12 -36.9(3) . . . . ? C9 P2 C11 C12 73.8(3) . . . . ? Pd1 P2 C11 C12 -156.0(2) . . . . ? C21 Pd1 C13 C14 54(13) . . . . ? P2 Pd1 C13 C14 26(12) . . . . ? P1 Pd1 C13 C14 -163(12) . . . . ? Pd1 C13 C14 C15 105(13) . . . . ? C13 C14 C15 C20 108(8) . . . . ? C13 C14 C15 C16 -69(8) . . . . ? C20 C15 C16 C29 -178.8(2) . . . 3_656 ? C14 C15 C16 C29 -1.3(4) . . . 3_656 ? C20 C15 C16 C17 0.4(4) . . . . ? C14 C15 C16 C17 177.9(2) . . . . ? C29 C16 C17 C30 0.1(4) 3_656 . . 3_656 ? C15 C16 C17 C30 -179.1(2) . . . 3_656 ? C29 C16 C17 C18 179.7(2) 3_656 . . . ? C15 C16 C17 C18 0.5(4) . . . . ? C30 C17 C18 C19 179.1(3) 3_656 . . . ? C16 C17 C18 C19 -0.5(4) . . . . ? C17 C18 C19 C20 -0.5(4) . . . . ? C14 C15 C20 C19 -178.9(2) . . . . ? C16 C15 C20 C19 -1.4(4) . . . . ? C18 C19 C20 C15 1.4(4) . . . . ? C13 Pd1 C21 C22 -71(10) . . . . ? P2 Pd1 C21 C22 -43(9) . . . . ? P1 Pd1 C21 C22 146(9) . . . . ? Pd1 C21 C22 C23 -112(18) . . . . ? C21 C22 C23 C24 -84(17) . . . . ? C21 C22 C23 C28 96(17) . . . . ? C22 C23 C24 C25 -178.6(2) . . . . ? C28 C23 C24 C25 0.9(4) . . . . ? C23 C24 C25 C26 0.4(4) . . . . ? C24 C25 C26 C27 -1.4(4) . . . . ? C25 C26 C27 C30 -178.2(3) . . . . ? C25 C26 C27 C28 1.2(4) . . . . ? C30 C27 C28 C29 0.5(4) . . . . ? C26 C27 C28 C29 -178.9(2) . . . . ? C30 C27 C28 C23 179.4(2) . . . . ? C26 C27 C28 C23 0.0(4) . . . . ? C24 C23 C28 C29 177.9(3) . . . . ? C22 C23 C28 C29 -2.7(4) . . . . ? C24 C23 C28 C27 -1.0(4) . . . . ? C22 C23 C28 C27 178.4(2) . . . . ? C27 C28 C29 C16 -0.2(4) . . . 3_656 ? C23 C28 C29 C16 -179.1(2) . . . 3_656 ? C26 C27 C30 C17 178.7(3) . . . 3_656 ? C28 C27 C30 C17 -0.6(4) . . . 3_656 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.829 _refine_diff_density_min -1.604 _refine_diff_density_rms 0.120