Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Liu, Shiuh-Tzung' 'Hsin-Pei, Chen' 'Yi-Hung, Liu' 'Shie-ming, Peng' _publ_contact_author_name 'Prof Shiuh-Tzung Liu' _publ_contact_author_address ; Department of Chemistry National Taiwan University 1, Sec. 4, Roosevelt Rd. Taipei 106 TAIWAN ; _publ_contact_author_email 'STLIU@CCMS.NTU.EDU.TW' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; New Bulky Phosphino-Pyridine Ligands. P~N~C Tridentates in Palladium Complexes. ; data_ic8696 _database_code_CSD 199587 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C30 H38 B F4 N2 P Pd' _chemical_formula_weight 650.80 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' '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' _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 9.4710(2) _cell_length_b 12.1480(3) _cell_length_c 14.1510(4) _cell_angle_alpha 104.0900(10) _cell_angle_beta 94.3890(10) _cell_angle_gamma 103.3000(10) _cell_volume 1521.56(7) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 78403 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method ? _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.709 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.904 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Nonius KappaCCD' _diffrn_measurement_method '\f-\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21100 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5334 _reflns_number_observed 4716 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Denzo-SMN & Scalepack' _computing_data_reduction 'Denzo-SMN & Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELX _computing_publication_material SHELX _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+0.5615P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0501(39) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5323 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_obs 0.0498 _refine_ls_wR_factor_all 0.1486 _refine_ls_wR_factor_obs 0.1355 _refine_ls_goodness_of_fit_all 1.108 _refine_ls_goodness_of_fit_obs 1.082 _refine_ls_restrained_S_all 1.112 _refine_ls_restrained_S_obs 1.082 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd -0.18608(3) 0.40987(2) 0.71008(2) 0.0494(2) Uani 1 d . . P1 P 0.03476(11) 0.37235(9) 0.65469(8) 0.0469(3) Uani 1 d . . N1 N -0.0500(3) 0.5518(3) 0.8033(2) 0.0462(7) Uani 1 d . . N2 N -0.3521(4) 0.2748(4) 0.6316(3) 0.0637(9) Uani 1 d . . C1 C -0.4569(5) 0.2046(4) 0.5962(4) 0.0645(11) Uani 1 d . . C2 C -0.5929(6) 0.1174(5) 0.5532(4) 0.083(2) Uani 1 d . . H2A H -0.5936(6) 0.0470(5) 0.5728(4) 0.125 Uiso 1 calc R . H2B H -0.6019(6) 0.1004(5) 0.4828(4) 0.125 Uiso 1 calc R . H2C H -0.6736(6) 0.1470(5) 0.5756(4) 0.125 Uiso 1 calc R . C3 C 0.0959(4) 0.5876(3) 0.7974(3) 0.0466(8) Uani 1 d . . C4 C 0.1863(4) 0.6817(3) 0.8673(3) 0.0511(9) Uani 1 d . . H4A H 0.2856(4) 0.7036(3) 0.8622(3) 0.061 Uiso 1 calc R . C5 C 0.1318(4) 0.7448(3) 0.9458(3) 0.0514(9) Uani 1 d . . C6 C -0.0193(5) 0.7090(4) 0.9476(3) 0.0549(9) Uani 1 d . . H6A H -0.0608(5) 0.7506(4) 0.9973(3) 0.066 Uiso 1 calc R . C7 C -0.1068(4) 0.6143(3) 0.8779(3) 0.0517(9) Uani 1 d . . C8 C -0.2687(4) 0.5643(4) 0.8789(3) 0.0573(10) Uani 1 d . . C9 C -0.3370(5) 0.4868(4) 0.7753(4) 0.0620(11) Uani 1 d . . H9A H -0.3689(5) 0.5342(4) 0.7361(4) 0.074 Uiso 1 calc R . H9B H -0.4219(5) 0.4267(4) 0.7795(4) 0.074 Uiso 1 calc R . C10 C -0.3479(6) 0.6633(5) 0.9080(4) 0.0788(15) Uani 1 d . . H10A H -0.4500(6) 0.6293(5) 0.9080(4) 0.118 Uiso 1 calc R . H10B H -0.3376(6) 0.7094(5) 0.8614(4) 0.118 Uiso 1 calc R . H10C H -0.3052(6) 0.7125(5) 0.9725(4) 0.118 Uiso 1 calc R . C11 C -0.2801(6) 0.4920(5) 0.9542(4) 0.0774(14) Uani 1 d . . H11A H -0.3814(6) 0.4586(5) 0.9571(4) 0.116 Uiso 1 calc R . H11B H -0.2338(6) 0.5419(5) 1.0178(4) 0.116 Uiso 1 calc R . H11C H -0.2320(6) 0.4302(5) 0.9349(4) 0.116 Uiso 1 calc R . C12 C 0.2276(5) 0.8506(4) 1.0245(3) 0.0614(11) Uani 1 d . . C13 C 0.3894(6) 0.8514(5) 1.0303(5) 0.090(2) Uani 1 d . . H13A H 0.4210(6) 0.8514(5) 0.9674(5) 0.135 Uiso 1 calc R . H13B H 0.4029(6) 0.7829(5) 1.0483(5) 0.135 Uiso 1 calc R . H13C H 0.4461(6) 0.9206(5) 1.0789(5) 0.135 Uiso 1 calc R . C14 C 0.2131(8) 0.9601(5) 0.9955(7) 0.123(3) Uani 1 d . . H14A H 0.2419(8) 0.9569(5) 0.9315(7) 0.185 Uiso 1 calc R . H14B H 0.2751(8) 1.0282(5) 1.0426(7) 0.185 Uiso 1 calc R . H14C H 0.1131(8) 0.9646(5) 0.9941(7) 0.185 Uiso 1 calc R . C15 C 0.1837(11) 0.8508(8) 1.1248(5) 0.155(4) Uani 1 d . . H15A H 0.1942(11) 0.7803(8) 1.1405(5) 0.232 Uiso 1 calc R . H15B H 0.0834(11) 0.8543(8) 1.1246(5) 0.232 Uiso 1 calc R . H15C H 0.2454(11) 0.9179(8) 1.1731(5) 0.232 Uiso 1 calc R . C19 C 0.1493(4) 0.5246(3) 0.7078(3) 0.0519(9) Uani 1 d . . H19A H 0.2495(4) 0.5225(3) 0.7253(3) 0.062 Uiso 1 calc R . H19B H 0.1489(4) 0.5678(3) 0.6585(3) 0.062 Uiso 1 calc R . C20 C 0.0576(5) 0.3336(3) 0.5250(3) 0.0522(9) Uani 1 d . . C21 C -0.0702(5) 0.2834(4) 0.4591(3) 0.0603(11) Uani 1 d . . H21A H -0.1598(5) 0.2794(4) 0.4827(3) 0.072 Uiso 1 calc R . C22 C -0.0693(6) 0.2384(4) 0.3586(3) 0.0697(13) Uani 1 d . . H22A H -0.1563(6) 0.2038(4) 0.3156(3) 0.084 Uiso 1 calc R . C23 C 0.0641(7) 0.2468(4) 0.3252(4) 0.0758(14) Uani 1 d . . H23A H 0.0673(7) 0.2162(4) 0.2587(4) 0.091 Uiso 1 calc R . C24 C 0.1939(7) 0.3000(5) 0.3887(4) 0.0723(13) Uani 1 d . . H24A H 0.2823(7) 0.3055(5) 0.3634(4) 0.087 Uiso 1 calc R . C25 C 0.1960(5) 0.3453(4) 0.4890(3) 0.0593(10) Uani 1 d . . C26 C 0.3395(5) 0.4054(5) 0.5522(4) 0.0747(13) Uani 1 d . . H26A H 0.3236(5) 0.4319(5) 0.6192(4) 0.112 Uiso 1 calc R . H26B H 0.3871(5) 0.4715(5) 0.5303(4) 0.112 Uiso 1 calc R . H26C H 0.4001(5) 0.3515(5) 0.5478(4) 0.112 Uiso 1 calc R . C30 C 0.1205(4) 0.2766(3) 0.7074(3) 0.0485(8) Uani 1 d . . C31 C 0.2501(5) 0.3216(4) 0.7750(3) 0.0599(10) Uani 1 d . . H31A H 0.2922(5) 0.4022(4) 0.7947(3) 0.072 Uiso 1 calc R . C32 C 0.3160(5) 0.2476(5) 0.8128(4) 0.0739(13) Uani 1 d . . H32A H 0.4022(5) 0.2786(5) 0.8569(4) 0.089 Uiso 1 calc R . C33 C 0.2541(7) 0.1288(5) 0.7851(4) 0.0796(15) Uani 1 d . . H33A H 0.3002(7) 0.0788(5) 0.8084(4) 0.096 Uiso 1 calc R . C34 C 0.1262(6) 0.0846(4) 0.7239(4) 0.0740(13) Uani 1 d . . H34A H 0.0830(6) 0.0044(4) 0.7092(4) 0.089 Uiso 1 calc R . C35 C 0.0549(5) 0.1543(4) 0.6811(3) 0.0553(9) Uani 1 d . . C36 C -0.0871(6) 0.0979(4) 0.6136(4) 0.0761(14) Uani 1 d . . H36A H -0.1213(6) 0.1567(4) 0.5908(4) 0.114 Uiso 1 calc R . H36B H -0.1586(6) 0.0611(4) 0.6485(4) 0.114 Uiso 1 calc R . H36C H -0.0723(6) 0.0399(4) 0.5584(4) 0.114 Uiso 1 calc R . B1 B 0.4877(7) 0.8418(6) 0.7037(5) 0.076(2) Uani 1 d . . F1 F 0.4403(13) 0.8914(11) 0.6417(9) 0.307(6) Uani 1 d . . F2 F 0.4176(7) 0.8771(6) 0.7771(4) 0.177(3) Uani 1 d . . F3 F 0.6297(6) 0.8811(6) 0.7167(6) 0.216(4) Uani 1 d . . F4 F 0.4402(7) 0.7364(6) 0.6546(7) 0.234(4) Uani 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 Pd1 0.0398(2) 0.0509(2) 0.0548(3) 0.0096(2) 0.00883(14) 0.01093(14) P1 0.0421(5) 0.0462(5) 0.0533(6) 0.0112(4) 0.0114(4) 0.0138(4) N1 0.043(2) 0.046(2) 0.052(2) 0.0142(14) 0.0114(14) 0.0135(13) N2 0.049(2) 0.068(2) 0.067(2) 0.005(2) 0.009(2) 0.014(2) C1 0.051(2) 0.069(3) 0.065(3) 0.004(2) 0.010(2) 0.012(2) C2 0.058(3) 0.085(4) 0.084(4) -0.001(3) 0.011(3) 0.000(3) C3 0.044(2) 0.045(2) 0.056(2) 0.019(2) 0.012(2) 0.015(2) C4 0.042(2) 0.047(2) 0.063(2) 0.017(2) 0.008(2) 0.007(2) C5 0.054(2) 0.048(2) 0.055(2) 0.018(2) 0.009(2) 0.012(2) C6 0.056(2) 0.051(2) 0.055(2) 0.009(2) 0.015(2) 0.014(2) C7 0.049(2) 0.049(2) 0.060(2) 0.015(2) 0.014(2) 0.014(2) C8 0.045(2) 0.061(2) 0.065(3) 0.012(2) 0.017(2) 0.014(2) C9 0.047(2) 0.066(3) 0.069(3) 0.006(2) 0.011(2) 0.016(2) C10 0.062(3) 0.072(3) 0.101(4) 0.006(3) 0.028(3) 0.027(2) C11 0.072(3) 0.076(3) 0.079(3) 0.019(3) 0.028(3) 0.004(3) C12 0.061(3) 0.055(2) 0.059(3) 0.007(2) 0.006(2) 0.007(2) C13 0.066(3) 0.081(3) 0.100(4) -0.003(3) -0.018(3) 0.014(3) C14 0.104(5) 0.051(3) 0.193(8) 0.018(4) -0.038(5) 0.013(3) C15 0.153(8) 0.158(8) 0.068(4) -0.028(4) 0.025(4) -0.067(6) C19 0.046(2) 0.046(2) 0.066(3) 0.014(2) 0.020(2) 0.013(2) C20 0.061(2) 0.048(2) 0.051(2) 0.014(2) 0.012(2) 0.020(2) C21 0.067(3) 0.057(2) 0.061(3) 0.018(2) 0.009(2) 0.024(2) C22 0.093(4) 0.063(3) 0.053(3) 0.015(2) 0.000(2) 0.026(3) C23 0.118(5) 0.066(3) 0.054(3) 0.021(2) 0.020(3) 0.037(3) C24 0.096(4) 0.072(3) 0.067(3) 0.027(2) 0.041(3) 0.037(3) C25 0.069(3) 0.058(2) 0.065(3) 0.027(2) 0.022(2) 0.027(2) C26 0.058(3) 0.087(3) 0.085(3) 0.023(3) 0.030(2) 0.023(2) C30 0.048(2) 0.048(2) 0.052(2) 0.014(2) 0.013(2) 0.013(2) C31 0.057(2) 0.061(2) 0.061(3) 0.017(2) 0.006(2) 0.012(2) C32 0.061(3) 0.092(4) 0.074(3) 0.034(3) 0.000(2) 0.021(3) C33 0.085(4) 0.088(4) 0.087(4) 0.043(3) 0.017(3) 0.042(3) C34 0.088(4) 0.053(3) 0.088(4) 0.027(2) 0.022(3) 0.020(2) C35 0.059(2) 0.050(2) 0.059(2) 0.017(2) 0.014(2) 0.015(2) C36 0.072(3) 0.048(2) 0.096(4) 0.010(2) 0.003(3) 0.004(2) B1 0.073(4) 0.077(4) 0.075(4) 0.013(3) 0.021(3) 0.018(3) F1 0.355(14) 0.389(15) 0.306(11) 0.251(12) 0.125(11) 0.156(12) F2 0.169(5) 0.190(5) 0.121(4) -0.016(4) 0.067(4) -0.004(4) F3 0.096(3) 0.170(5) 0.282(8) -0.090(5) 0.041(4) -0.010(3) F4 0.124(4) 0.129(5) 0.352(10) -0.085(6) 0.043(5) -0.001(3) _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 N1 1.996(3) . ? Pd1 N2 2.014(4) . ? Pd1 C9 2.041(4) . ? Pd1 P1 2.3900(10) . ? P1 C20 1.822(4) . ? P1 C30 1.826(4) . ? P1 C19 1.854(4) . ? N1 C3 1.366(5) . ? N1 C7 1.366(5) . ? N2 C1 1.136(6) . ? C1 C2 1.445(7) . ? C3 C4 1.373(6) . ? C3 C19 1.500(5) . ? C4 C5 1.394(6) . ? C5 C6 1.401(6) . ? C5 C12 1.526(6) . ? C6 C7 1.367(6) . ? C7 C8 1.517(5) . ? C8 C11 1.533(7) . ? C8 C9 1.535(6) . ? C8 C10 1.549(6) . ? C12 C15 1.509(8) . ? C12 C14 1.515(7) . ? C12 C13 1.526(7) . ? C20 C21 1.385(6) . ? C20 C25 1.432(6) . ? C21 C22 1.395(7) . ? C22 C23 1.373(8) . ? C23 C24 1.385(8) . ? C24 C25 1.389(7) . ? C25 C26 1.490(7) . ? C30 C31 1.406(6) . ? C30 C35 1.415(6) . ? C31 C32 1.387(6) . ? C32 C33 1.372(8) . ? C33 C34 1.349(8) . ? C34 C35 1.410(6) . ? C35 C36 1.500(6) . ? B1 F4 1.256(8) . ? B1 F1 1.287(10) . ? B1 F3 1.302(8) . ? B1 F2 1.313(8) . ? 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 N1 Pd1 N2 169.22(13) . . ? N1 Pd1 C9 80.9(2) . . ? N2 Pd1 C9 88.6(2) . . ? N1 Pd1 P1 83.71(9) . . ? N2 Pd1 P1 106.89(11) . . ? C9 Pd1 P1 164.12(13) . . ? C20 P1 C30 104.5(2) . . ? C20 P1 C19 106.1(2) . . ? C30 P1 C19 107.1(2) . . ? C20 P1 Pd1 122.91(14) . . ? C30 P1 Pd1 118.45(13) . . ? C19 P1 Pd1 95.71(12) . . ? C3 N1 C7 118.9(3) . . ? C3 N1 Pd1 123.6(3) . . ? C7 N1 Pd1 117.5(3) . . ? C1 N2 Pd1 170.8(4) . . ? N2 C1 C2 178.1(5) . . ? N1 C3 C4 121.1(4) . . ? N1 C3 C19 116.7(3) . . ? C4 C3 C19 122.1(3) . . ? C3 C4 C5 121.1(4) . . ? C4 C5 C6 116.5(4) . . ? C4 C5 C12 123.0(4) . . ? C6 C5 C12 120.5(4) . . ? C7 C6 C5 121.3(4) . . ? N1 C7 C6 121.0(4) . . ? N1 C7 C8 114.2(4) . . ? C6 C7 C8 124.7(4) . . ? C7 C8 C11 106.8(4) . . ? C7 C8 C9 108.4(4) . . ? C11 C8 C9 111.1(4) . . ? C7 C8 C10 111.2(4) . . ? C11 C8 C10 110.2(4) . . ? C9 C8 C10 109.0(4) . . ? C8 C9 Pd1 109.6(3) . . ? C15 C12 C14 111.9(7) . . ? C15 C12 C5 110.9(4) . . ? C14 C12 C5 107.6(4) . . ? C15 C12 C13 107.3(6) . . ? C14 C12 C13 107.0(5) . . ? C5 C12 C13 112.1(4) . . ? C3 C19 P1 112.4(3) . . ? C21 C20 C25 119.3(4) . . ? C21 C20 P1 115.9(3) . . ? C25 C20 P1 124.7(3) . . ? C20 C21 C22 122.3(5) . . ? C23 C22 C21 117.9(5) . . ? C22 C23 C24 121.3(5) . . ? C23 C24 C25 122.0(5) . . ? C24 C25 C20 117.2(5) . . ? C24 C25 C26 119.0(4) . . ? C20 C25 C26 123.8(4) . . ? C31 C30 C35 118.8(4) . . ? C31 C30 P1 121.5(3) . . ? C35 C30 P1 119.7(3) . . ? C32 C31 C30 120.9(4) . . ? C33 C32 C31 120.1(5) . . ? C34 C33 C32 119.8(5) . . ? C33 C34 C35 123.1(5) . . ? C34 C35 C30 117.2(4) . . ? C34 C35 C36 119.7(4) . . ? C30 C35 C36 123.1(4) . . ? F4 B1 F1 99.1(9) . . ? F4 B1 F3 114.7(6) . . ? F1 B1 F3 105.3(8) . . ? F4 B1 F2 116.1(7) . . ? F1 B1 F2 99.8(7) . . ? F3 B1 F2 117.7(6) . . ? _refine_diff_density_max 0.818 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.174 data_ic8560 _database_code_CSD 199588 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C29 H39 Cl N P Pd' _chemical_formula_weight 574.43 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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' '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 9.79400(10) _cell_length_b 12.24100(10) _cell_length_c 13.1120(2) _cell_angle_alpha 75.4280(10) _cell_angle_beta 72.4730(10) _cell_angle_gamma 72.8460(10) _cell_volume 1409.27(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 49546 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method ? _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.863 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Nonius KappaCCD' _diffrn_measurement_method '\f-\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9383 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4972 _reflns_number_observed 4432 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Denzo-SMN & Scalepack' _computing_data_reduction 'Denzo-SMN & Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELX _computing_publication_material SHELX _refine_special_details ; Refinement on F^2^ for ALL reflections except for 14 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+0.3825P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0426(26) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4958 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_obs 0.0408 _refine_ls_wR_factor_all 0.1297 _refine_ls_wR_factor_obs 0.1127 _refine_ls_goodness_of_fit_all 1.226 _refine_ls_goodness_of_fit_obs 1.139 _refine_ls_restrained_S_all 1.233 _refine_ls_restrained_S_obs 1.139 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.42487(3) 0.40251(2) 0.11397(2) 0.0379(2) Uani 1 d . . Cl1 Cl 0.41735(12) 0.45864(9) -0.07313(7) 0.0503(3) Uani 1 d . . P1 P 0.42531(10) 0.35798(7) 0.28943(7) 0.0354(2) Uani 1 d . . N1 N 0.1343(3) 0.5687(3) 0.2793(3) 0.0456(7) Uani 1 d . . C1 C 0.2918(5) 0.2940(4) 0.1372(3) 0.0554(10) Uani 1 d . . H1A H 0.2718(5) 0.2960(4) 0.0693(3) 0.083 Uiso 1 calc R . H1B H 0.2009(5) 0.3186(4) 0.1887(3) 0.083 Uiso 1 calc R . H1C H 0.3399(5) 0.2163(4) 0.1645(3) 0.083 Uiso 1 calc R . C3 C 0.2568(4) 0.5904(3) 0.2862(3) 0.0418(8) Uani 1 d . . C4 C 0.2962(4) 0.6954(3) 0.2408(3) 0.0455(8) Uani 1 d . . H4A H 0.3821(4) 0.7070(3) 0.2482(3) 0.055 Uiso 1 calc R . C5 C 0.2052(4) 0.7831(3) 0.1840(3) 0.0501(9) Uani 1 d . . C6 C 0.0790(4) 0.7589(3) 0.1772(3) 0.0516(9) Uani 1 d . . H6A H 0.0158(4) 0.8153(3) 0.1394(3) 0.062 Uiso 1 calc R . C7 C 0.0450(4) 0.6526(3) 0.2254(3) 0.0475(9) Uani 1 d . . C8 C -0.0907(5) 0.6236(4) 0.2124(4) 0.0605(11) Uani 1 d . . C9 C -0.2188(6) 0.7313(6) 0.2091(7) 0.118(3) Uani 1 d . . H9A H -0.2464(6) 0.7601(6) 0.2759(7) 0.178 Uiso 1 calc R . H9B H -0.3014(6) 0.7112(6) 0.1999(7) 0.178 Uiso 1 calc R . H9C H -0.1889(6) 0.7903(6) 0.1494(7) 0.178 Uiso 1 calc R . C10 C -0.0448(8) 0.5764(9) 0.1086(6) 0.124(3) Uani 1 d . . H10A H -0.0121(8) 0.6341(9) 0.0486(6) 0.186 Uiso 1 calc R . H10B H -0.1271(8) 0.5570(9) 0.0981(6) 0.186 Uiso 1 calc R . H10C H 0.0341(8) 0.5081(9) 0.1129(6) 0.186 Uiso 1 calc R . C11 C -0.1429(7) 0.5341(5) 0.3086(6) 0.091(2) Uani 1 d . . H11A H -0.1717(7) 0.5656(5) 0.3741(6) 0.136 Uiso 1 calc R . H11B H -0.0643(7) 0.4656(5) 0.3137(6) 0.136 Uiso 1 calc R . H11C H -0.2256(7) 0.5145(5) 0.2990(6) 0.136 Uiso 1 calc R . C12 C 0.2482(6) 0.8978(4) 0.1275(5) 0.0706(13) Uani 1 d . . C13 C 0.3678(20) 0.9127(10) 0.1558(15) 0.318(12) Uani 1 d . . H13A H 0.4482(20) 0.8455(10) 0.1466(15) 0.478 Uiso 1 calc R . H13B H 0.3388(20) 0.9226(10) 0.2303(15) 0.478 Uiso 1 calc R . H13C H 0.3982(20) 0.9802(10) 0.1099(15) 0.478 Uiso 1 calc R . C14 C 0.1287(11) 0.9943(6) 0.1399(13) 0.262(10) Uani 1 d . . H14A H 0.0483(11) 0.9820(6) 0.1201(13) 0.393 Uiso 1 calc R . H14B H 0.1575(11) 1.0624(6) 0.0939(13) 0.393 Uiso 1 calc R . H14C H 0.0982(11) 1.0047(6) 0.2143(13) 0.393 Uiso 1 calc R . C15 C 0.2934(19) 0.9041(10) 0.0100(8) 0.239(9) Uani 1 d . . H15A H 0.3762(19) 0.8407(10) -0.0079(8) 0.359 Uiso 1 calc R . H15B H 0.3205(19) 0.9763(10) -0.0243(8) 0.359 Uiso 1 calc R . H15C H 0.2131(19) 0.8995(10) -0.0151(8) 0.359 Uiso 1 calc R . C19 C 0.3581(4) 0.4949(3) 0.3453(3) 0.0427(8) Uani 1 d . . H19A H 0.3065(4) 0.4781(3) 0.4210(3) 0.051 Uiso 1 calc R . H19B H 0.4425(4) 0.5226(3) 0.3425(3) 0.051 Uiso 1 calc R . C20 C 0.6115(4) 0.3023(3) 0.3135(3) 0.0426(8) Uani 1 d . . C21 C 0.6412(4) 0.2772(3) 0.4157(3) 0.0494(9) Uani 1 d . . C22 C 0.7894(5) 0.2341(4) 0.4205(4) 0.0621(11) Uani 1 d . . H22A H 0.8118(5) 0.2151(4) 0.4878(4) 0.075 Uiso 1 calc R . C23 C 0.9011(5) 0.2193(4) 0.3297(4) 0.0674(12) Uani 1 d . . H23A H 0.9979(5) 0.1911(4) 0.3359(4) 0.081 Uiso 1 calc R . C24 C 0.8722(5) 0.2453(4) 0.2304(4) 0.0666(12) Uani 1 d . . H24A H 0.9492(5) 0.2363(4) 0.1686(4) 0.080 Uiso 1 calc R . C25 C 0.7282(4) 0.2853(3) 0.2211(4) 0.0524(9) Uani 1 d . . H25A H 0.7085(4) 0.3012(3) 0.1531(4) 0.063 Uiso 1 calc R . C26 C 0.5280(5) 0.2899(5) 0.5197(4) 0.0675(12) Uani 1 d . . H26A H 0.5753(5) 0.2674(5) 0.5786(4) 0.101 Uiso 1 calc R . H26B H 0.4621(5) 0.2411(5) 0.5308(4) 0.101 Uiso 1 calc R . H26C H 0.4733(5) 0.3694(5) 0.5168(4) 0.101 Uiso 1 calc R . C30 C 0.3184(4) 0.2565(3) 0.3825(3) 0.0420(8) Uani 1 d . . C31 C 0.1821(4) 0.3002(4) 0.4491(3) 0.0504(9) Uani 1 d . . H31A H 0.1450(4) 0.3801(4) 0.4438(3) 0.061 Uiso 1 calc R . C32 C 0.1015(5) 0.2256(5) 0.5231(4) 0.0662(12) Uani 1 d . . H32A H 0.0119(5) 0.2557(5) 0.5684(4) 0.079 Uiso 1 calc R . C33 C 0.1519(6) 0.1100(5) 0.5299(4) 0.0751(14) Uani 1 d . . H33A H 0.0978(6) 0.0604(5) 0.5806(4) 0.090 Uiso 1 calc R . C34 C 0.2847(6) 0.0645(4) 0.4612(4) 0.0686(13) Uani 1 d . . H34A H 0.3174(6) -0.0157(4) 0.4658(4) 0.082 Uiso 1 calc R . C35 C 0.3704(5) 0.1363(3) 0.3853(3) 0.0515(9) Uani 1 d . . C36 C 0.5121(5) 0.0811(4) 0.3125(4) 0.0659(12) Uani 1 d . . H36C H 0.5587(5) 0.1405(4) 0.2650(4) 0.099 Uiso 1 calc R . H36D H 0.4913(5) 0.0375(4) 0.2699(4) 0.099 Uiso 1 calc R . H36A H 0.5767(5) 0.0301(4) 0.3560(4) 0.099 Uiso 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 0.0433(2) 0.0423(2) 0.0321(2) 0.00047(12) -0.01312(13) -0.01798(13) Cl1 0.0656(6) 0.0631(6) 0.0348(5) 0.0042(4) -0.0197(4) -0.0373(5) P1 0.0398(5) 0.0359(4) 0.0322(4) 0.0002(3) -0.0126(4) -0.0130(4) N1 0.047(2) 0.043(2) 0.047(2) -0.0037(13) -0.0144(14) -0.0130(13) C1 0.063(2) 0.066(3) 0.048(2) 0.002(2) -0.022(2) -0.033(2) C3 0.048(2) 0.039(2) 0.042(2) -0.0086(15) -0.015(2) -0.0096(15) C4 0.049(2) 0.038(2) 0.052(2) -0.003(2) -0.016(2) -0.014(2) C5 0.053(2) 0.042(2) 0.054(2) -0.005(2) -0.014(2) -0.012(2) C6 0.051(2) 0.045(2) 0.054(2) 0.002(2) -0.020(2) -0.007(2) C7 0.044(2) 0.052(2) 0.048(2) -0.010(2) -0.013(2) -0.011(2) C8 0.046(2) 0.069(3) 0.071(3) -0.011(2) -0.019(2) -0.016(2) C9 0.054(3) 0.095(4) 0.202(9) 0.002(5) -0.057(4) -0.011(3) C10 0.092(4) 0.221(9) 0.100(5) -0.073(6) -0.026(4) -0.057(5) C11 0.079(4) 0.094(4) 0.107(5) -0.002(3) -0.021(3) -0.048(3) C12 0.075(3) 0.042(2) 0.091(4) 0.009(2) -0.022(3) -0.023(2) C13 0.471(23) 0.171(10) 0.472(23) 0.205(13) -0.396(21) -0.244(14) C14 0.141(8) 0.048(4) 0.476(25) -0.015(8) 0.078(11) -0.029(4) C15 0.406(22) 0.172(10) 0.123(8) -0.010(7) 0.066(11) -0.192(14) C19 0.050(2) 0.041(2) 0.042(2) -0.0061(15) -0.019(2) -0.0128(15) C20 0.044(2) 0.037(2) 0.048(2) 0.0001(15) -0.018(2) -0.0125(14) C21 0.057(2) 0.045(2) 0.052(2) 0.001(2) -0.025(2) -0.016(2) C22 0.063(3) 0.056(2) 0.073(3) 0.009(2) -0.037(2) -0.019(2) C23 0.053(2) 0.060(3) 0.090(4) 0.001(2) -0.030(3) -0.013(2) C24 0.048(2) 0.062(3) 0.079(3) -0.008(2) -0.006(2) -0.009(2) C25 0.048(2) 0.053(2) 0.053(2) -0.006(2) -0.012(2) -0.012(2) C26 0.069(3) 0.088(3) 0.048(2) -0.005(2) -0.025(2) -0.016(2) C30 0.050(2) 0.045(2) 0.035(2) 0.0022(15) -0.016(2) -0.020(2) C31 0.050(2) 0.061(2) 0.044(2) -0.006(2) -0.010(2) -0.022(2) C32 0.067(3) 0.090(3) 0.046(2) -0.005(2) -0.006(2) -0.040(2) C33 0.089(4) 0.085(4) 0.055(3) 0.017(2) -0.016(3) -0.053(3) C34 0.097(4) 0.049(2) 0.066(3) 0.015(2) -0.032(3) -0.035(2) C35 0.066(2) 0.045(2) 0.049(2) 0.004(2) -0.023(2) -0.022(2) C36 0.077(3) 0.041(2) 0.082(3) -0.010(2) -0.027(3) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.033(4) . ? Pd1 P1 2.2279(9) . ? Pd1 Cl1 2.3931(9) . ? Pd1 Cl1 2.4812(10) 2_665 ? Cl1 Pd1 2.4811(10) 2_665 ? P1 C30 1.834(3) . ? P1 C20 1.843(4) . ? P1 C19 1.858(4) . ? N1 C3 1.335(5) . ? N1 C7 1.340(5) . ? C3 C4 1.388(5) . ? C3 C19 1.508(5) . ? C4 C5 1.390(5) . ? C5 C6 1.386(6) . ? C5 C12 1.527(6) . ? C6 C7 1.386(6) . ? C7 C8 1.539(6) . ? C8 C10 1.503(7) . ? C8 C11 1.516(7) . ? C8 C9 1.530(7) . ? C12 C14 1.400(10) . ? C12 C13 1.402(10) . ? C12 C15 1.457(11) . ? C20 C21 1.397(5) . ? C20 C25 1.403(5) . ? C21 C22 1.405(6) . ? C21 C26 1.486(6) . ? C22 C23 1.362(7) . ? C23 C24 1.355(7) . ? C24 C25 1.382(6) . ? C30 C31 1.394(5) . ? C30 C35 1.402(5) . ? C31 C32 1.384(6) . ? C32 C33 1.344(7) . ? C33 C34 1.390(8) . ? C34 C35 1.400(6) . ? C35 C36 1.506(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 91.10(12) . . ? C1 Pd1 Cl1 89.64(12) . . ? P1 Pd1 Cl1 177.44(3) . . ? C1 Pd1 Cl1 175.93(12) . 2_665 ? P1 Pd1 Cl1 92.81(3) . 2_665 ? Cl1 Pd1 Cl1 86.40(3) . 2_665 ? Pd1 Cl1 Pd1 93.60(3) . 2_665 ? C30 P1 C20 105.0(2) . . ? C30 P1 C19 106.4(2) . . ? C20 P1 C19 102.3(2) . . ? C30 P1 Pd1 119.87(12) . . ? C20 P1 Pd1 113.51(12) . . ? C19 P1 Pd1 108.17(12) . . ? C3 N1 C7 118.3(3) . . ? N1 C3 C4 123.4(3) . . ? N1 C3 C19 118.0(3) . . ? C4 C3 C19 118.6(3) . . ? C3 C4 C5 119.0(4) . . ? C6 C5 C4 116.8(4) . . ? C6 C5 C12 122.2(4) . . ? C4 C5 C12 120.9(4) . . ? C5 C6 C7 121.4(4) . . ? N1 C7 C6 121.1(4) . . ? N1 C7 C8 117.6(4) . . ? C6 C7 C8 121.2(4) . . ? C10 C8 C11 110.5(5) . . ? C10 C8 C9 110.8(6) . . ? C11 C8 C9 107.3(5) . . ? C10 C8 C7 107.3(4) . . ? C11 C8 C7 109.8(4) . . ? C9 C8 C7 111.2(4) . . ? C14 C12 C13 111.0(10) . . ? C14 C12 C15 102.5(10) . . ? C13 C12 C15 105.5(11) . . ? C14 C12 C5 112.8(5) . . ? C13 C12 C5 113.8(5) . . ? C15 C12 C5 110.5(5) . . ? C3 C19 P1 114.2(2) . . ? C21 C20 C25 119.7(3) . . ? C21 C20 P1 124.3(3) . . ? C25 C20 P1 116.1(3) . . ? C20 C21 C22 117.3(4) . . ? C20 C21 C26 125.0(3) . . ? C22 C21 C26 117.7(4) . . ? C23 C22 C21 122.1(4) . . ? C24 C23 C22 120.5(4) . . ? C23 C24 C25 119.9(4) . . ? C24 C25 C20 120.5(4) . . ? C31 C30 C35 119.9(3) . . ? C31 C30 P1 119.2(3) . . ? C35 C30 P1 120.9(3) . . ? C32 C31 C30 120.5(4) . . ? C33 C32 C31 120.5(5) . . ? C32 C33 C34 120.0(4) . . ? C33 C34 C35 121.6(4) . . ? C34 C35 C30 117.3(4) . . ? C34 C35 C36 118.8(4) . . ? C30 C35 C36 123.9(4) . . ? _refine_diff_density_max 0.950 _refine_diff_density_min -0.749 _refine_diff_density_rms 0.260 data_ic8660 _database_code_CSD 199589 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H78 Cl2 N2 O2 P2 Pd2' _chemical_formula_weight 1204.88 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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' '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 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 12.3940(2) _cell_length_b 16.7220(3) _cell_length_c 15.0540(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.5590(10) _cell_angle_gamma 90.00 _cell_volume 2990.58(8) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 33836 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method ? _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.899 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Nonius KappaCCD' _diffrn_measurement_method '\f-\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14733 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5266 _reflns_number_observed 3984 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Denzo-SMN & Scalepack' _computing_data_reduction 'Denzo-SMN & Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELX _computing_publication_material SHELX _refine_special_details ; Refinement on F^2^ for ALL reflections except for 20 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0779P)^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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0146(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5246 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_obs 0.0436 _refine_ls_wR_factor_all 0.1381 _refine_ls_wR_factor_obs 0.1097 _refine_ls_goodness_of_fit_all 1.121 _refine_ls_goodness_of_fit_obs 1.038 _refine_ls_restrained_S_all 1.127 _refine_ls_restrained_S_obs 1.038 _refine_ls_shift/esd_max -0.008 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.52233(3) 0.10451(2) 0.54006(2) 0.0373(2) Uani 1 d . . Cl1 Cl 0.41493(10) -0.00967(7) 0.56729(7) 0.0473(3) Uani 1 d . . P1 P 0.59957(10) 0.22233(7) 0.51012(7) 0.0374(3) Uani 1 d . . O1 O 0.5100(4) 0.1549(3) 0.7106(3) 0.0846(14) Uani 1 d . . N1 N 0.3370(3) 0.3014(2) 0.3537(3) 0.0465(10) Uani 1 d . . H1A H 0.3667(3) 0.3472(2) 0.3721(3) 0.056 Uiso 1 calc R . C1 C 0.4608(5) 0.1600(3) 0.6301(4) 0.0557(14) Uani 1 d . . C2 C 0.3462(6) 0.1960(4) 0.5930(5) 0.085(2) Uani 1 d . . H2A H 0.3237(6) 0.1932(4) 0.5265(5) 0.127 Uiso 1 calc R . H2B H 0.3481(6) 0.2509(4) 0.6120(5) 0.127 Uiso 1 calc R . H2C H 0.2934(6) 0.1670(4) 0.6165(5) 0.127 Uiso 1 calc R . C3 C 0.4019(4) 0.2382(3) 0.3557(3) 0.0413(11) Uani 1 d . . C4 C 0.3582(4) 0.1635(3) 0.3263(3) 0.0480(12) Uani 1 d . . H4A H 0.4060(4) 0.1202(3) 0.3286(3) 0.058 Uiso 1 calc R . C5 C 0.2439(4) 0.1539(3) 0.2939(3) 0.0516(12) Uani 1 d . . C6 C 0.1786(5) 0.2208(3) 0.2933(4) 0.0561(13) Uani 1 d . . H6A H 0.1006(5) 0.2163(3) 0.2723(4) 0.067 Uiso 1 calc R . C7 C 0.2257(4) 0.2940(3) 0.3230(3) 0.0506(12) Uani 1 d . . C8 C 0.1581(5) 0.3700(4) 0.3226(5) 0.072(2) Uani 1 d . . C9 C 0.0308(5) 0.3529(4) 0.2930(5) 0.082(2) Uani 1 d . . H9A H 0.0091(5) 0.3305(4) 0.2318(5) 0.123 Uiso 1 calc R . H9B H -0.0097(5) 0.4018(4) 0.2934(5) 0.123 Uiso 1 calc R . H9C H 0.0135(5) 0.3156(4) 0.3356(5) 0.123 Uiso 1 calc R . C10 C 0.1908(8) 0.4051(6) 0.4177(8) 0.167(6) Uani 1 d . . H10A H 0.1483(8) 0.4531(6) 0.4180(8) 0.251 Uiso 1 calc R . H10B H 0.2697(8) 0.4176(6) 0.4358(8) 0.251 Uiso 1 calc R . H10C H 0.1754(8) 0.3673(6) 0.4605(8) 0.251 Uiso 1 calc R . C11 C 0.1798(6) 0.4262(4) 0.2484(7) 0.122(3) Uani 1 d . . H11A H 0.1569(6) 0.4004(4) 0.1890(7) 0.183 Uiso 1 calc R . H11B H 0.2586(6) 0.4387(4) 0.2637(7) 0.183 Uiso 1 calc R . H11C H 0.1375(6) 0.4746(4) 0.2461(7) 0.183 Uiso 1 calc R . C12 C 0.1860(5) 0.0733(4) 0.2643(4) 0.0628(15) Uani 1 d . . C13 C 0.2701(7) 0.0075(4) 0.2633(6) 0.110(3) Uani 1 d . . H13A H 0.3238(7) 0.0036(4) 0.3233(6) 0.165 Uiso 1 calc R . H13B H 0.3085(7) 0.0198(4) 0.2179(6) 0.165 Uiso 1 calc R . H13C H 0.2311(7) -0.0425(4) 0.2480(6) 0.165 Uiso 1 calc R . C14 C 0.1258(7) 0.0497(5) 0.3362(5) 0.113(3) Uani 1 d . . H14A H 0.1797(7) 0.0457(5) 0.3961(5) 0.170 Uiso 1 calc R . H14B H 0.0892(7) -0.0010(5) 0.3197(5) 0.170 Uiso 1 calc R . H14C H 0.0706(7) 0.0895(5) 0.3378(5) 0.170 Uiso 1 calc R . C15 C 0.1016(7) 0.0798(4) 0.1708(5) 0.111(3) Uani 1 d . . H15A H 0.0487(7) 0.1214(4) 0.1719(5) 0.166 Uiso 1 calc R . H15B H 0.0623(7) 0.0299(4) 0.1554(5) 0.166 Uiso 1 calc R . H15C H 0.1396(7) 0.0921(4) 0.1251(5) 0.166 Uiso 1 calc R . C19 C 0.5274(4) 0.2513(3) 0.3893(3) 0.0417(11) Uani 1 d . . H19A H 0.5667(4) 0.2731(3) 0.3509(3) 0.050 Uiso 1 calc R . C20 C 0.7465(4) 0.2198(3) 0.5078(3) 0.0435(11) Uani 1 d . . C21 C 0.7991(4) 0.1451(4) 0.5195(4) 0.0575(13) Uani 1 d . . H21A H 0.7590(4) 0.1008(4) 0.5300(4) 0.069 Uiso 1 calc R . C22 C 0.9082(5) 0.1346(5) 0.5162(5) 0.078(2) Uani 1 d . . H22A H 0.9405(5) 0.0839(5) 0.5237(5) 0.094 Uiso 1 calc R . C23 C 0.9685(5) 0.1996(5) 0.5018(5) 0.082(2) Uani 1 d . . H23A H 1.0418(5) 0.1933(5) 0.4984(5) 0.099 Uiso 1 calc R . C24 C 0.9199(5) 0.2739(4) 0.4924(4) 0.071(2) Uani 1 d . . H24A H 0.9626(5) 0.3177(4) 0.4847(4) 0.086 Uiso 1 calc R . C25 C 0.8093(4) 0.2867(3) 0.4937(3) 0.0546(13) Uani 1 d . . C26 C 0.7633(6) 0.3716(4) 0.4791(5) 0.085(2) Uani 1 d . . H26A H 0.6868(6) 0.3720(4) 0.4817(5) 0.128 Uiso 1 calc R . H26B H 0.7661(6) 0.3907(4) 0.4197(5) 0.128 Uiso 1 calc R . H26C H 0.8081(6) 0.4057(4) 0.5269(5) 0.128 Uiso 1 calc R . C30 C 0.5891(4) 0.3078(3) 0.5832(3) 0.0422(11) Uani 1 d . . C31 C 0.5109(4) 0.3682(3) 0.5483(3) 0.0516(13) Uani 1 d . . H31A H 0.4668(4) 0.3653(3) 0.4871(3) 0.062 Uiso 1 calc R . C32 C 0.4972(5) 0.4317(3) 0.6016(4) 0.0615(14) Uani 1 d . . H32A H 0.4437(5) 0.4709(3) 0.5768(4) 0.074 Uiso 1 calc R . C33 C 0.5634(5) 0.4371(4) 0.6925(4) 0.065(2) Uani 1 d . . H33A H 0.5549(5) 0.4799(4) 0.7294(4) 0.078 Uiso 1 calc R . C34 C 0.6413(5) 0.3792(4) 0.7274(4) 0.061(2) Uani 1 d . . H34A H 0.6864(5) 0.3843(4) 0.7882(4) 0.073 Uiso 1 calc R . C35 C 0.6568(4) 0.3121(3) 0.6762(3) 0.0473(12) Uani 1 d . . C36 C 0.7428(5) 0.2513(4) 0.7196(3) 0.068(2) Uani 1 d . . H36A H 0.7428(5) 0.2098(4) 0.6756(3) 0.102 Uiso 1 calc R . H36B H 0.7256(5) 0.2288(4) 0.7726(3) 0.102 Uiso 1 calc R . H36C H 0.8157(5) 0.2761(4) 0.7387(3) 0.102 Uiso 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 0.0485(3) 0.0328(2) 0.0311(2) -0.00061(14) 0.0119(2) -0.0031(2) Cl1 0.0656(8) 0.0378(7) 0.0457(6) -0.0021(5) 0.0277(6) -0.0075(6) P1 0.0439(7) 0.0351(7) 0.0316(6) 0.0001(5) 0.0081(5) -0.0037(5) O1 0.118(4) 0.092(4) 0.051(2) -0.025(2) 0.035(2) -0.025(3) N1 0.055(3) 0.036(2) 0.044(2) -0.004(2) 0.008(2) -0.003(2) C1 0.080(4) 0.042(3) 0.053(3) -0.012(2) 0.033(3) -0.020(3) C2 0.092(5) 0.067(4) 0.114(5) -0.001(4) 0.060(4) 0.011(4) C3 0.050(3) 0.040(3) 0.032(2) 0.000(2) 0.010(2) 0.003(2) C4 0.051(3) 0.044(3) 0.045(3) -0.001(2) 0.007(2) 0.002(2) C5 0.049(3) 0.048(3) 0.051(3) 0.000(2) 0.003(2) -0.001(2) C6 0.047(3) 0.053(4) 0.061(3) 0.002(3) 0.004(2) 0.000(3) C7 0.046(3) 0.048(3) 0.052(3) -0.004(2) 0.005(2) 0.001(2) C8 0.056(4) 0.053(4) 0.096(5) -0.010(3) 0.005(3) 0.010(3) C9 0.063(4) 0.075(5) 0.107(5) 0.008(4) 0.021(3) 0.021(3) C10 0.104(7) 0.175(11) 0.182(10) -0.122(9) -0.023(6) 0.058(7) C11 0.080(5) 0.051(4) 0.238(11) 0.041(6) 0.051(6) 0.016(4) C12 0.060(3) 0.046(3) 0.069(4) -0.003(3) -0.003(3) -0.008(3) C13 0.097(6) 0.048(4) 0.161(7) -0.026(5) -0.002(5) -0.007(4) C14 0.146(8) 0.087(6) 0.102(6) -0.001(5) 0.028(5) -0.051(5) C15 0.134(7) 0.067(5) 0.086(5) -0.002(4) -0.043(5) -0.014(5) C19 0.043(3) 0.052(3) 0.029(2) 0.003(2) 0.008(2) -0.006(2) C20 0.046(3) 0.049(3) 0.034(2) 0.001(2) 0.009(2) -0.004(2) C21 0.048(3) 0.056(4) 0.064(3) 0.001(3) 0.010(2) 0.000(3) C22 0.054(4) 0.086(5) 0.094(5) 0.007(4) 0.020(3) 0.012(3) C23 0.048(4) 0.110(6) 0.091(5) 0.007(4) 0.024(3) 0.005(4) C24 0.059(4) 0.091(5) 0.067(4) -0.004(3) 0.023(3) -0.028(4) C25 0.056(3) 0.062(4) 0.047(3) -0.001(2) 0.016(2) -0.018(3) C26 0.096(5) 0.057(4) 0.116(6) 0.001(4) 0.053(4) -0.026(4) C30 0.054(3) 0.039(3) 0.033(2) -0.001(2) 0.011(2) -0.007(2) C31 0.062(3) 0.046(3) 0.045(3) -0.006(2) 0.011(2) -0.001(2) C32 0.076(4) 0.045(3) 0.063(3) -0.005(3) 0.020(3) 0.001(3) C33 0.086(4) 0.057(4) 0.059(3) -0.020(3) 0.030(3) -0.015(3) C34 0.078(4) 0.067(4) 0.037(3) -0.016(3) 0.018(3) -0.029(3) C35 0.059(3) 0.049(3) 0.034(2) -0.002(2) 0.012(2) -0.010(2) C36 0.076(4) 0.080(4) 0.037(3) 0.003(3) -0.002(3) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 1.968(5) . ? Pd1 P1 2.2907(12) . ? Pd1 Cl1 2.4282(12) . ? Pd1 Cl1 2.5392(11) 3_656 ? Cl1 Pd1 2.5393(11) 3_656 ? P1 C30 1.831(5) . ? P1 C20 1.832(5) . ? P1 C19 1.848(4) . ? O1 C1 1.194(6) . ? N1 C3 1.324(6) . ? N1 C7 1.330(6) . ? C1 C2 1.496(9) . ? C3 C4 1.384(7) . ? C3 C19 1.508(6) . ? C4 C5 1.370(7) . ? C5 C6 1.379(7) . ? C5 C12 1.532(8) . ? C6 C7 1.375(7) . ? C7 C8 1.521(8) . ? C8 C10 1.493(11) . ? C8 C11 1.542(10) . ? C8 C9 1.540(8) . ? C12 C15 1.499(8) . ? C12 C13 1.518(9) . ? C12 C14 1.532(9) . ? C20 C21 1.397(7) . ? C20 C25 1.412(7) . ? C21 C22 1.378(7) . ? C22 C23 1.372(10) . ? C23 C24 1.370(10) . ? C24 C25 1.393(8) . ? C25 C26 1.522(9) . ? C30 C31 1.394(7) . ? C30 C35 1.414(6) . ? C31 C32 1.370(7) . ? C32 C33 1.384(8) . ? C33 C34 1.363(8) . ? C34 C35 1.406(7) . ? C35 C36 1.483(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 89.78(15) . . ? C1 Pd1 Cl1 85.14(15) . . ? P1 Pd1 Cl1 171.67(4) . . ? C1 Pd1 Cl1 169.21(15) . 3_656 ? P1 Pd1 Cl1 101.01(4) . 3_656 ? Cl1 Pd1 Cl1 84.16(4) . 3_656 ? Pd1 Cl1 Pd1 95.84(4) . 3_656 ? C30 P1 C20 105.7(2) . . ? C30 P1 C19 106.8(2) . . ? C20 P1 C19 101.1(2) . . ? C30 P1 Pd1 116.62(15) . . ? C20 P1 Pd1 117.2(2) . . ? C19 P1 Pd1 107.9(2) . . ? C3 N1 C7 119.8(4) . . ? O1 C1 C2 124.3(5) . . ? O1 C1 Pd1 118.7(5) . . ? C2 C1 Pd1 116.4(4) . . ? N1 C3 C4 122.3(4) . . ? N1 C3 C19 117.0(4) . . ? C4 C3 C19 120.7(4) . . ? C5 C4 C3 119.4(5) . . ? C4 C5 C6 116.9(5) . . ? C4 C5 C12 123.9(5) . . ? C6 C5 C12 119.1(5) . . ? C7 C6 C5 121.7(5) . . ? N1 C7 C6 119.9(5) . . ? N1 C7 C8 116.0(5) . . ? C6 C7 C8 124.1(5) . . ? C10 C8 C7 109.1(6) . . ? C10 C8 C11 113.5(8) . . ? C7 C8 C11 107.6(6) . . ? C10 C8 C9 109.0(6) . . ? C7 C8 C9 111.3(5) . . ? C11 C8 C9 106.3(5) . . ? C15 C12 C13 109.9(6) . . ? C15 C12 C5 110.7(5) . . ? C13 C12 C5 112.0(5) . . ? C15 C12 C14 109.4(6) . . ? C13 C12 C14 107.1(6) . . ? C5 C12 C14 107.6(5) . . ? C3 C19 P1 117.1(3) . . ? C21 C20 C25 118.0(5) . . ? C21 C20 P1 116.7(4) . . ? C25 C20 P1 125.3(4) . . ? C22 C21 C20 122.4(6) . . ? C23 C22 C21 119.4(7) . . ? C22 C23 C24 119.4(6) . . ? C23 C24 C25 123.0(6) . . ? C24 C25 C20 117.8(5) . . ? C24 C25 C26 118.1(5) . . ? C20 C25 C26 124.1(5) . . ? C31 C30 C35 119.3(4) . . ? C31 C30 P1 120.0(3) . . ? C35 C30 P1 120.7(4) . . ? C32 C31 C30 122.0(5) . . ? C31 C32 C33 119.4(6) . . ? C34 C33 C32 119.4(5) . . ? C33 C34 C35 123.3(5) . . ? C34 C35 C30 116.6(5) . . ? C34 C35 C36 119.9(5) . . ? C30 C35 C36 123.5(5) . . ? _refine_diff_density_max 0.663 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.241 data_ic8246 _database_code_CSD 199590 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C66 H94 Cl2 N2 P2 Pd2' _chemical_formula_weight 1261.07 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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' '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 11.54900(10) _cell_length_b 16.13000(10) _cell_length_c 17.9020(2) _cell_angle_alpha 94.5540(10) _cell_angle_beta 101.6010(10) _cell_angle_gamma 91.3250(10) _cell_volume 3253.83(5) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method ? _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.870 _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Nonius KappaCCD' _diffrn_measurement_method '\f-\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21494 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11445 _reflns_number_observed 9591 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'Denzo-SMN & Scalepack' _computing_data_reduction 'Denzo-SMN & Scalepack' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELX _computing_publication_material SHELX _refine_special_details ; Refinement on F^2^ for ALL reflections except for 61 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+1.8004P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0081(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11384 _refine_ls_number_parameters 668 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_obs 0.0437 _refine_ls_wR_factor_all 0.1399 _refine_ls_wR_factor_obs 0.1219 _refine_ls_goodness_of_fit_all 1.186 _refine_ls_goodness_of_fit_obs 1.145 _refine_ls_restrained_S_all 1.198 _refine_ls_restrained_S_obs 1.145 _refine_ls_shift/esd_max 0.084 _refine_ls_shift/esd_mean 0.008 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.74632(2) 0.29020(2) 0.10136(2) 0.03882(12) Uani 1 d . . Cl1 Cl 0.90818(9) 0.39009(6) 0.16381(7) 0.0604(3) Uani 1 d . . P1 P 0.82950(8) 0.17180(5) 0.14189(5) 0.0360(2) Uani 1 d . . N1 N 1.1549(3) 0.1435(2) 0.2515(2) 0.0480(8) Uani 1 d . . H1A H 1.1694(3) 0.1084(2) 0.2161(2) 0.058 Uiso 1 calc R . C1 C 0.5989(4) 0.2234(3) 0.0444(3) 0.0684(14) Uani 1 d . . H1B H 0.5427(4) 0.2604(3) 0.0194(3) 0.103 Uiso 1 calc R . H1C H 0.5646(4) 0.1946(3) 0.0801(3) 0.103 Uiso 1 calc R . H1D H 0.6199(4) 0.1838(3) 0.0070(3) 0.103 Uiso 1 calc R . C3 C 1.0656(3) 0.1943(2) 0.2362(2) 0.0410(8) Uani 1 d . . C4 C 1.0396(3) 0.2524(2) 0.2914(2) 0.0427(8) Uani 1 d . . H4A H 0.9779(3) 0.2881(2) 0.2786(2) 0.051 Uiso 1 calc R . C5 C 1.1058(3) 0.2573(2) 0.3657(2) 0.0465(9) Uani 1 d . . C6 C 1.1981(4) 0.2033(3) 0.3793(3) 0.0579(11) Uani 1 d . . H6A H 1.2451(4) 0.2047(3) 0.4281(3) 0.069 Uiso 1 calc R . C7 C 1.2220(4) 0.1472(3) 0.3220(3) 0.0568(11) Uani 1 d . . C8 C 1.3218(4) 0.0872(4) 0.3350(3) 0.0722(14) Uani 1 d . . C9 C 1.4108(9) 0.1090(9) 0.2917(8) 0.260(9) Uani 1 d . . H9A H 1.4385(9) 0.1657(9) 0.3064(8) 0.391 Uiso 1 calc R . H9B H 1.3765(9) 0.1028(9) 0.2380(8) 0.391 Uiso 1 calc R . H9C H 1.4759(9) 0.0729(9) 0.3022(8) 0.391 Uiso 1 calc R . C10 C 1.3880(10) 0.0921(7) 0.4178(6) 0.215(7) Uani 1 d . . H10A H 1.4180(10) 0.1481(7) 0.4337(6) 0.322 Uiso 1 calc R . H10B H 1.4526(10) 0.0552(7) 0.4222(6) 0.322 Uiso 1 calc R . H10C H 1.3351(10) 0.0761(7) 0.4497(6) 0.322 Uiso 1 calc R . C11 C 1.2787(9) 0.0028(5) 0.3142(9) 0.257(9) Uani 1 d . . H11A H 1.2205(9) -0.0104(5) 0.3433(9) 0.385 Uiso 1 calc R . H11B H 1.3431(9) -0.0338(5) 0.3246(9) 0.385 Uiso 1 calc R . H11C H 1.2434(9) -0.0038(5) 0.2606(9) 0.385 Uiso 1 calc R . C12 C 1.0810(4) 0.3191(3) 0.4289(2) 0.0574(11) Uani 1 d . . C13 C 0.9752(5) 0.3718(4) 0.4018(3) 0.081(2) Uani 1 d . . H13A H 0.9058(5) 0.3362(4) 0.3837(3) 0.122 Uiso 1 calc R . H13B H 0.9902(5) 0.4031(4) 0.3611(3) 0.122 Uiso 1 calc R . H13C H 0.9629(5) 0.4094(4) 0.4436(3) 0.122 Uiso 1 calc R . C14 C 1.0557(7) 0.2718(4) 0.4953(3) 0.096(2) Uani 1 d . . H14A H 0.9886(7) 0.2340(4) 0.4772(3) 0.145 Uiso 1 calc R . H14B H 1.0391(7) 0.3107(4) 0.5349(3) 0.145 Uiso 1 calc R . H14C H 1.1235(7) 0.2411(4) 0.5155(3) 0.145 Uiso 1 calc R . C15 C 1.1870(5) 0.3795(4) 0.4565(4) 0.093(2) Uani 1 d . . H15A H 1.1711(5) 0.4184(4) 0.4963(4) 0.139 Uiso 1 calc R . H15B H 1.2012(5) 0.4092(4) 0.4146(4) 0.139 Uiso 1 calc R . H15C H 1.2555(5) 0.3492(4) 0.4760(4) 0.139 Uiso 1 calc R . C19 C 0.9953(3) 0.1859(2) 0.1554(2) 0.0416(8) Uani 1 d . . H19A H 1.0320(3) 0.1877(2) 0.1138(2) 0.050 Uiso 1 calc R . C20 C 0.8175(3) 0.1349(2) 0.2352(2) 0.0398(8) Uani 1 d . . C21 C 0.8765(4) 0.0632(2) 0.2602(2) 0.0496(9) Uani 1 d . . C22 C 0.8743(5) 0.0422(3) 0.3336(3) 0.0666(13) Uani 1 d . . H22A H 0.9131(5) -0.0049(3) 0.3501(3) 0.080 Uiso 1 calc R . C23 C 0.8183(5) 0.0870(4) 0.3830(3) 0.0761(15) Uani 1 d . . C24 C 0.7590(5) 0.1549(3) 0.3572(3) 0.0658(12) Uani 1 d . . H24A H 0.7184(5) 0.1850(3) 0.3896(3) 0.079 Uiso 1 calc R . C25 C 0.7567(4) 0.1809(3) 0.2844(2) 0.0507(9) Uani 1 d . . C26 C 0.9405(4) 0.0057(2) 0.2122(3) 0.0566(11) Uani 1 d . . H26A H 0.9362(4) 0.0263(2) 0.1629(3) 0.085 Uiso 1 calc R . H26B H 0.9039(4) -0.0492(2) 0.2060(3) 0.085 Uiso 1 calc R . H26C H 1.0218(4) 0.0036(2) 0.2375(3) 0.085 Uiso 1 calc R . C27 C 0.8207(8) 0.0615(5) 0.4636(4) 0.124(3) Uani 1 d . . H27A H 0.8666(8) 0.0129(5) 0.4716(4) 0.186 Uiso 1 calc R . H27B H 0.7414(8) 0.0494(5) 0.4695(4) 0.186 Uiso 1 calc R . H27C H 0.8558(8) 0.1062(5) 0.5005(4) 0.186 Uiso 1 calc R . C28 C 0.6874(4) 0.2563(3) 0.2641(3) 0.0647(12) Uani 1 d . . H28A H 0.6922(4) 0.2685(3) 0.2132(3) 0.097 Uiso 1 calc R . H28B H 0.7195(4) 0.3029(3) 0.2995(3) 0.097 Uiso 1 calc R . H28C H 0.6062(4) 0.2458(3) 0.2666(3) 0.097 Uiso 1 calc R . C30 C 0.7831(3) 0.0809(2) 0.0715(2) 0.0389(8) Uani 1 d . . C31 C 0.6927(3) 0.0239(2) 0.0795(2) 0.0430(8) Uani 1 d . . C32 C 0.6699(3) -0.0481(2) 0.0293(2) 0.0482(9) Uani 1 d . . H32A H 0.6109(3) -0.0859(2) 0.0349(2) 0.058 Uiso 1 calc R . C33 C 0.7313(4) -0.0653(3) -0.0284(3) 0.0544(10) Uani 1 d . . C34 C 0.8097(4) -0.0044(3) -0.0404(2) 0.0540(10) Uani 1 d . . H34A H 0.8472(4) -0.0131(3) -0.0816(2) 0.065 Uiso 1 calc R . C35 C 0.8353(3) 0.0698(2) 0.0068(2) 0.0436(8) Uani 1 d . . C36 C 0.6132(4) 0.0352(3) 0.1367(3) 0.0533(10) Uani 1 d . . H36A H 0.6357(4) 0.0863(3) 0.1683(3) 0.080 Uiso 1 calc R . H36B H 0.6209(4) -0.0106(3) 0.1682(3) 0.080 Uiso 1 calc R . H36C H 0.5326(4) 0.0372(3) 0.1100(3) 0.080 Uiso 1 calc R . C37 C 0.7123(5) -0.1484(3) -0.0757(3) 0.077(2) Uani 1 d . . H37A H 0.6549(5) -0.1820(3) -0.0583(3) 0.116 Uiso 1 calc R . H37B H 0.7857(5) -0.1763(3) -0.0701(3) 0.116 Uiso 1 calc R . H37C H 0.6841(5) -0.1396(3) -0.1285(3) 0.116 Uiso 1 calc R . C38 C 0.9125(4) 0.1346(3) -0.0176(3) 0.0583(11) Uani 1 d . . H38A H 0.9237(4) 0.1823(3) 0.0191(3) 0.088 Uiso 1 calc R . H38B H 0.8752(4) 0.1507(3) -0.0669(3) 0.088 Uiso 1 calc R . H38C H 0.9879(4) 0.1120(3) -0.0205(3) 0.088 Uiso 1 calc R . Pd1A Pd 0.79368(3) 0.51372(2) 0.12413(2) 0.04348(12) Uani 1 d . . Cl1A Cl 0.65940(9) 0.41065(6) 0.04730(6) 0.0554(3) Uani 1 d . . P1A P 0.90280(9) 0.61444(5) 0.20568(5) 0.0399(2) Uani 1 d . . N1A N 1.1733(3) 0.5950(2) 0.3688(2) 0.0477(8) Uani 1 d . . H1AA H 1.1408(3) 0.6251(2) 0.4001(2) 0.057 Uiso 1 calc R . C1A C 0.6789(5) 0.6000(3) 0.0800(3) 0.078(2) Uani 1 d . . H1AB H 0.6176(5) 0.5732(3) 0.0407(3) 0.117 Uiso 1 calc R . H1AC H 0.7206(5) 0.6413(3) 0.0588(3) 0.117 Uiso 1 calc R . H1AD H 0.6443(5) 0.6261(3) 0.1199(3) 0.117 Uiso 1 calc R . C3A C 1.1078(3) 0.5557(2) 0.3055(2) 0.0409(8) Uani 1 d . . C4A C 1.1565(3) 0.5058(2) 0.2545(2) 0.0460(9) Uani 1 d . . H4AA H 1.1080(3) 0.4790(2) 0.2110(2) 0.055 Uiso 1 calc R . C5A C 1.2777(4) 0.4956(3) 0.2680(2) 0.0509(9) Uani 1 d . . C6A C 1.3441(4) 0.5382(3) 0.3339(3) 0.0561(10) Uani 1 d . . H6AA H 1.4258(4) 0.5338(3) 0.3451(3) 0.067 Uiso 1 calc R . C7A C 1.2900(3) 0.5868(3) 0.3827(2) 0.0509(9) Uani 1 d . . C8A C 1.3579(4) 0.6350(3) 0.4565(3) 0.0637(12) Uani 1 d . . C9A C 1.3145(6) 0.6034(5) 0.5245(3) 0.106(2) Uani 1 d . . H9AA H 1.2306(6) 0.6093(5) 0.5176(3) 0.159 Uiso 1 calc R . H9AB H 1.3534(6) 0.6353(5) 0.5706(3) 0.159 Uiso 1 calc R . H9AC H 1.3323(6) 0.5459(5) 0.5281(3) 0.159 Uiso 1 calc R . C10A C 1.4900(4) 0.6244(4) 0.4696(4) 0.093(2) Uani 1 d . . H10D H 1.5198(4) 0.6438(4) 0.4275(4) 0.140 Uiso 1 calc R . H10E H 1.5063(4) 0.5667(4) 0.4736(4) 0.140 Uiso 1 calc R . H10F H 1.5278(4) 0.6561(4) 0.5162(4) 0.140 Uiso 1 calc R . C11A C 1.3326(7) 0.7269(4) 0.4530(5) 0.133(3) Uani 1 d . . H11D H 1.2487(7) 0.7337(4) 0.4448(5) 0.200 Uiso 1 calc R . H11E H 1.3627(7) 0.7479(4) 0.4117(5) 0.200 Uiso 1 calc R . H11F H 1.3703(7) 0.7570(4) 0.5004(5) 0.200 Uiso 1 calc R . C12A C 1.3350(4) 0.4397(3) 0.2135(3) 0.0680(13) Uani 1 d . . C13A C 1.2492(7) 0.4002(7) 0.1471(5) 0.171(5) Uani 1 d . . H13D H 1.2072(7) 0.4424(7) 0.1192(5) 0.257 Uiso 1 calc R . H13E H 1.1941(7) 0.3647(7) 0.1646(5) 0.257 Uiso 1 calc R . H13F H 1.2905(7) 0.3676(7) 0.1144(5) 0.257 Uiso 1 calc R . C14A C 1.3968(14) 0.3750(8) 0.2553(6) 0.263(9) Uani 1 d . . H14D H 1.4530(14) 0.3999(8) 0.2987(6) 0.395 Uiso 1 calc R . H14E H 1.4375(14) 0.3422(8) 0.2224(6) 0.395 Uiso 1 calc R . H14F H 1.3408(14) 0.3400(8) 0.2725(6) 0.395 Uiso 1 calc R . C15A C 1.4176(10) 0.4902(7) 0.1809(7) 0.216(7) Uani 1 d . . H15D H 1.3753(10) 0.5327(7) 0.1535(7) 0.324 Uiso 1 calc R . H15E H 1.4529(10) 0.4551(7) 0.1465(7) 0.324 Uiso 1 calc R . H15F H 1.4783(10) 0.5157(7) 0.2214(7) 0.324 Uiso 1 calc R . C19A C 0.9765(3) 0.5668(2) 0.2946(2) 0.0428(8) Uani 1 d . . H19B H 0.9339(3) 0.5507(2) 0.3302(2) 0.051 Uiso 1 calc R . C20A C 1.0318(4) 0.6718(2) 0.1862(2) 0.0456(9) Uani 1 d . . C21A C 1.0959(4) 0.7323(2) 0.2417(2) 0.0517(10) Uani 1 d . . C22A C 1.2041(5) 0.7625(3) 0.2309(3) 0.0712(14) Uani 1 d . . H22B H 1.2463(5) 0.8024(3) 0.2672(3) 0.085 Uiso 1 calc R . C23A C 1.2519(5) 0.7364(4) 0.1692(3) 0.083(2) Uani 1 d . . C24A C 1.1865(5) 0.6824(3) 0.1144(3) 0.0724(14) Uani 1 d . . H24B H 1.2159(5) 0.6670(3) 0.0709(3) 0.087 Uiso 1 calc R . C25A C 1.0768(4) 0.6489(3) 0.1204(2) 0.0554(10) Uani 1 d . . C26A C 1.0563(4) 0.7678(3) 0.3127(3) 0.0597(11) Uani 1 d . . H26D H 0.9808(4) 0.7429(3) 0.3146(3) 0.090 Uiso 1 calc R . H26E H 1.0498(4) 0.8270(3) 0.3114(3) 0.090 Uiso 1 calc R . H26F H 1.1132(4) 0.7562(3) 0.3572(3) 0.090 Uiso 1 calc R . C27A C 1.3741(6) 0.7695(6) 0.1617(5) 0.148(4) Uani 1 d . . H27D H 1.4071(6) 0.8069(6) 0.2056(5) 0.221 Uiso 1 calc R . H27E H 1.3666(6) 0.7985(6) 0.1163(5) 0.221 Uiso 1 calc R . H27F H 1.4252(6) 0.7238(6) 0.1585(5) 0.221 Uiso 1 calc R . C28A C 1.0145(6) 0.5899(3) 0.0554(3) 0.086(2) Uani 1 d . . H28D H 0.9404(6) 0.5710(3) 0.0659(3) 0.129 Uiso 1 calc R . H28E H 1.0627(6) 0.5431(3) 0.0495(3) 0.129 Uiso 1 calc R . H28F H 1.0003(6) 0.6178(3) 0.0092(3) 0.129 Uiso 1 calc R . C30A C 0.8054(3) 0.6920(2) 0.2369(2) 0.0460(9) Uani 1 d . . C31A C 0.7934(4) 0.7698(2) 0.2059(3) 0.0552(10) Uani 1 d . . C32A C 0.7264(4) 0.8296(3) 0.2361(3) 0.0683(13) Uani 1 d . . H32B H 0.7190(4) 0.8809(3) 0.2156(3) 0.082 Uiso 1 calc R . C33A C 0.6711(4) 0.8151(3) 0.2950(3) 0.0711(14) Uani 1 d . . C34A C 0.6741(4) 0.7370(3) 0.3195(3) 0.0696(13) Uani 1 d . . H34B H 0.6321(4) 0.7258(3) 0.3570(3) 0.083 Uiso 1 calc R . C35A C 0.7375(4) 0.6728(3) 0.2907(3) 0.0532(10) Uani 1 d . . C36A C 0.8458(5) 0.7925(3) 0.1391(3) 0.0677(13) Uani 1 d . . H36D H 0.8899(5) 0.7470(3) 0.1231(3) 0.102 Uiso 1 calc R . H36E H 0.8975(5) 0.8410(3) 0.1542(3) 0.102 Uiso 1 calc R . H36F H 0.7834(5) 0.8039(3) 0.0974(3) 0.102 Uiso 1 calc R . C37A C 0.6037(6) 0.8835(4) 0.3304(5) 0.115(2) Uani 1 d . . H37D H 0.6110(6) 0.9339(4) 0.3064(5) 0.172 Uiso 1 calc R . H37E H 0.6363(6) 0.8929(4) 0.3842(5) 0.172 Uiso 1 calc R . H37F H 0.5217(6) 0.8663(4) 0.3228(5) 0.172 Uiso 1 calc R . C38A C 0.7221(4) 0.5864(3) 0.3148(3) 0.0651(12) Uani 1 d . . H38D H 0.6722(4) 0.5879(3) 0.3518(3) 0.098 Uiso 1 calc R . H38E H 0.7979(4) 0.5665(3) 0.3371(3) 0.098 Uiso 1 calc R . H38F H 0.6863(4) 0.5498(3) 0.2709(3) 0.098 Uiso 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 0.0358(2) 0.0331(2) 0.0450(2) -0.00077(12) 0.00392(12) -0.00068(11) Cl1 0.0509(6) 0.0331(5) 0.0830(8) 0.0004(5) -0.0176(5) -0.0018(4) P1 0.0347(5) 0.0326(4) 0.0397(5) -0.0022(4) 0.0075(4) 0.0000(3) N1 0.040(2) 0.045(2) 0.058(2) 0.0007(15) 0.011(2) 0.0027(14) C1 0.048(2) 0.059(3) 0.086(3) 0.016(2) -0.018(2) -0.013(2) C3 0.033(2) 0.042(2) 0.049(2) 0.005(2) 0.008(2) -0.0005(15) C4 0.033(2) 0.044(2) 0.048(2) 0.003(2) 0.003(2) 0.0003(15) C5 0.043(2) 0.050(2) 0.045(2) 0.005(2) 0.008(2) -0.007(2) C6 0.049(2) 0.068(3) 0.051(2) 0.013(2) -0.005(2) -0.001(2) C7 0.043(2) 0.058(2) 0.067(3) 0.018(2) 0.001(2) 0.003(2) C8 0.050(3) 0.085(4) 0.081(3) 0.022(3) 0.004(2) 0.020(2) C9 0.146(9) 0.377(19) 0.347(18) 0.254(16) 0.155(11) 0.189(12) C10 0.200(11) 0.231(12) 0.168(10) -0.010(9) -0.072(8) 0.147(10) C11 0.121(7) 0.077(5) 0.501(25) -0.024(9) -0.094(11) 0.058(5) C12 0.058(3) 0.064(3) 0.046(2) -0.005(2) 0.007(2) -0.011(2) C13 0.088(4) 0.091(4) 0.062(3) -0.018(3) 0.014(3) 0.020(3) C14 0.134(6) 0.102(5) 0.059(3) 0.006(3) 0.038(4) -0.007(4) C15 0.085(4) 0.091(4) 0.093(4) -0.030(3) 0.016(3) -0.028(3) C19 0.033(2) 0.048(2) 0.043(2) -0.003(2) 0.010(2) -0.0003(15) C20 0.040(2) 0.038(2) 0.040(2) 0.0002(15) 0.006(2) -0.0057(15) C21 0.051(2) 0.040(2) 0.055(2) 0.005(2) 0.006(2) -0.008(2) C22 0.079(3) 0.056(3) 0.061(3) 0.017(2) 0.001(2) -0.008(2) C23 0.102(4) 0.079(3) 0.049(3) 0.010(2) 0.021(3) -0.017(3) C24 0.076(3) 0.074(3) 0.051(3) 0.000(2) 0.025(2) -0.005(3) C25 0.046(2) 0.058(2) 0.047(2) -0.006(2) 0.014(2) -0.006(2) C26 0.058(2) 0.037(2) 0.073(3) 0.008(2) 0.007(2) 0.004(2) C27 0.190(8) 0.124(6) 0.065(4) 0.037(4) 0.035(5) -0.011(6) C28 0.070(3) 0.069(3) 0.059(3) -0.007(2) 0.026(2) 0.015(2) C30 0.041(2) 0.033(2) 0.040(2) -0.0033(14) 0.005(2) 0.0032(14) C31 0.036(2) 0.046(2) 0.044(2) -0.001(2) 0.003(2) 0.001(2) C32 0.043(2) 0.040(2) 0.057(2) -0.009(2) 0.004(2) -0.005(2) C33 0.053(2) 0.045(2) 0.059(3) -0.014(2) 0.002(2) 0.000(2) C34 0.056(2) 0.058(2) 0.046(2) -0.009(2) 0.013(2) 0.004(2) C35 0.044(2) 0.044(2) 0.042(2) 0.000(2) 0.007(2) 0.002(2) C36 0.048(2) 0.050(2) 0.061(3) -0.005(2) 0.015(2) -0.007(2) C37 0.075(3) 0.064(3) 0.087(4) -0.035(3) 0.021(3) -0.010(2) C38 0.068(3) 0.061(3) 0.050(2) 0.004(2) 0.019(2) -0.004(2) Pd1A 0.0486(2) 0.0319(2) 0.0449(2) -0.00033(12) -0.00093(13) 0.00215(12) Cl1A 0.0538(6) 0.0378(5) 0.0640(6) 0.0003(4) -0.0117(5) 0.0016(4) P1A 0.0467(5) 0.0305(4) 0.0404(5) -0.0010(4) 0.0052(4) 0.0024(4) N1A 0.045(2) 0.047(2) 0.048(2) -0.0079(14) 0.0080(15) 0.0030(14) C1A 0.087(4) 0.056(3) 0.074(3) 0.001(2) -0.026(3) 0.023(3) C3A 0.040(2) 0.037(2) 0.044(2) 0.0018(15) 0.005(2) 0.0022(15) C4A 0.047(2) 0.040(2) 0.047(2) -0.006(2) 0.004(2) -0.003(2) C5A 0.047(2) 0.050(2) 0.054(2) -0.006(2) 0.012(2) 0.003(2) C6A 0.039(2) 0.065(3) 0.060(3) -0.008(2) 0.006(2) 0.000(2) C7A 0.042(2) 0.054(2) 0.053(2) -0.005(2) 0.005(2) -0.002(2) C8A 0.046(2) 0.078(3) 0.059(3) -0.020(2) 0.002(2) -0.004(2) C9A 0.085(4) 0.169(7) 0.056(3) -0.034(4) 0.015(3) -0.025(4) C10A 0.052(3) 0.132(5) 0.081(4) -0.035(4) -0.005(3) -0.005(3) C11A 0.149(7) 0.079(4) 0.130(6) -0.043(4) -0.051(5) 0.008(4) C12A 0.055(3) 0.077(3) 0.070(3) -0.023(2) 0.016(2) 0.011(2) C13A 0.100(5) 0.228(10) 0.160(8) -0.135(8) 0.024(5) 0.023(6) C14A 0.422(21) 0.262(13) 0.120(7) 0.007(8) 0.060(10) 0.284(16) C15A 0.208(11) 0.219(12) 0.251(13) -0.125(10) 0.184(11) -0.080(9) C19A 0.040(2) 0.048(2) 0.040(2) 0.008(2) 0.006(2) 0.001(2) C20A 0.056(2) 0.037(2) 0.044(2) 0.002(2) 0.011(2) 0.000(2) C21A 0.064(3) 0.042(2) 0.048(2) 0.003(2) 0.010(2) -0.008(2) C22A 0.068(3) 0.080(3) 0.061(3) 0.004(2) 0.007(2) -0.026(3) C23A 0.072(3) 0.110(4) 0.068(3) 0.019(3) 0.018(3) -0.022(3) C24A 0.081(3) 0.085(3) 0.060(3) 0.013(3) 0.033(3) 0.002(3) C25A 0.075(3) 0.044(2) 0.050(2) 0.003(2) 0.019(2) 0.001(2) C26A 0.071(3) 0.044(2) 0.058(3) -0.013(2) 0.006(2) -0.010(2) C27A 0.090(5) 0.237(11) 0.119(6) 0.005(7) 0.042(5) -0.070(6) C28A 0.122(5) 0.079(4) 0.059(3) -0.021(3) 0.038(3) -0.019(3) C30A 0.043(2) 0.041(2) 0.050(2) -0.006(2) 0.004(2) 0.004(2) C31A 0.056(2) 0.039(2) 0.067(3) -0.002(2) 0.003(2) 0.008(2) C32A 0.066(3) 0.045(2) 0.090(4) -0.003(2) 0.008(3) 0.014(2) C33A 0.058(3) 0.057(3) 0.096(4) -0.011(3) 0.014(3) 0.015(2) C34A 0.052(3) 0.082(3) 0.076(3) -0.010(3) 0.021(2) 0.008(2) C35A 0.044(2) 0.054(2) 0.060(3) 0.000(2) 0.007(2) 0.005(2) C36A 0.094(4) 0.042(2) 0.069(3) 0.012(2) 0.016(3) 0.016(2) C37A 0.107(5) 0.093(4) 0.150(7) -0.025(4) 0.048(5) 0.042(4) C38A 0.052(3) 0.071(3) 0.076(3) 0.010(2) 0.020(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.034(4) . ? Pd1 P1 2.2630(9) . ? Pd1 Cl1A 2.3911(10) . ? Pd1 Cl1 2.4647(10) . ? Cl1 Pd1A 2.4897(10) . ? P1 C20 1.846(4) . ? P1 C30 1.851(3) . ? P1 C19 1.887(4) . ? N1 C3 1.331(5) . ? N1 C7 1.338(5) . ? C3 C4 1.390(5) . ? C3 C19 1.504(5) . ? C4 C5 1.390(5) . ? C5 C6 1.388(6) . ? C5 C12 1.523(6) . ? C6 C7 1.387(7) . ? C7 C8 1.516(6) . ? C8 C11 1.432(10) . ? C8 C9 1.459(11) . ? C8 C10 1.519(10) . ? C12 C15 1.523(7) . ? C12 C13 1.526(7) . ? C12 C14 1.534(7) . ? C20 C25 1.411(5) . ? C20 C21 1.414(5) . ? C21 C22 1.387(6) . ? C21 C26 1.518(6) . ? C22 C23 1.370(7) . ? C23 C24 1.367(8) . ? C23 C27 1.526(7) . ? C24 C25 1.397(6) . ? C25 C28 1.500(6) . ? C30 C31 1.410(5) . ? C30 C35 1.411(5) . ? C31 C32 1.397(5) . ? C31 C36 1.510(5) . ? C32 C33 1.380(6) . ? C33 C34 1.379(6) . ? C33 C37 1.514(6) . ? C34 C35 1.398(5) . ? C35 C38 1.505(6) . ? Pd1A C1A 2.039(4) . ? Pd1A P1A 2.2689(10) . ? Pd1A Cl1A 2.3916(10) . ? P1A C30A 1.831(4) . ? P1A C20A 1.842(4) . ? P1A C19A 1.878(4) . ? N1A C7A 1.332(5) . ? N1A C3A 1.332(5) . ? C3A C4A 1.383(5) . ? C3A C19A 1.506(5) . ? C4A C5A 1.387(5) . ? C5A C6A 1.390(6) . ? C5A C12A 1.533(6) . ? C6A C7A 1.379(6) . ? C7A C8A 1.535(6) . ? C8A C10A 1.512(7) . ? C8A C9A 1.525(8) . ? C8A C11A 1.522(8) . ? C12A C14A 1.451(10) . ? C12A C13A 1.476(9) . ? C12A C15A 1.476(10) . ? C20A C25A 1.407(6) . ? C20A C21A 1.416(5) . ? C21A C22A 1.385(6) . ? C21A C26A 1.511(6) . ? C22A C23A 1.372(8) . ? C23A C24A 1.351(8) . ? C23A C27A 1.533(8) . ? C24A C25A 1.393(7) . ? C25A C28A 1.494(6) . ? C30A C35A 1.406(6) . ? C30A C31A 1.411(6) . ? C31A C32A 1.393(6) . ? C31A C36A 1.511(7) . ? C32A C33A 1.370(8) . ? C33A C34A 1.365(7) . ? C33A C37A 1.533(7) . ? C34A C35A 1.406(6) . ? C35A C38A 1.509(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 90.21(13) . . ? C1 Pd1 Cl1A 87.74(13) . . ? P1 Pd1 Cl1A 174.93(4) . . ? C1 Pd1 Cl1 171.17(13) . . ? P1 Pd1 Cl1 98.61(3) . . ? Cl1A Pd1 Cl1 83.51(3) . . ? Pd1 Cl1 Pd1A 93.63(3) . . ? C20 P1 C30 105.1(2) . . ? C20 P1 C19 100.3(2) . . ? C30 P1 C19 107.3(2) . . ? C20 P1 Pd1 121.88(12) . . ? C30 P1 Pd1 112.39(12) . . ? C19 P1 Pd1 108.53(12) . . ? C3 N1 C7 119.7(4) . . ? N1 C3 C4 122.1(3) . . ? N1 C3 C19 116.1(3) . . ? C4 C3 C19 121.8(3) . . ? C5 C4 C3 120.0(3) . . ? C6 C5 C4 116.2(4) . . ? C6 C5 C12 121.3(4) . . ? C4 C5 C12 122.5(4) . . ? C5 C6 C7 121.8(4) . . ? N1 C7 C6 120.2(4) . . ? N1 C7 C8 116.7(4) . . ? C6 C7 C8 123.1(4) . . ? C11 C8 C9 110.7(10) . . ? C11 C8 C7 111.3(5) . . ? C9 C8 C7 109.6(5) . . ? C11 C8 C10 107.3(8) . . ? C9 C8 C10 104.8(8) . . ? C7 C8 C10 112.9(5) . . ? C15 C12 C5 109.7(4) . . ? C15 C12 C13 106.4(5) . . ? C5 C12 C13 112.7(4) . . ? C15 C12 C14 110.3(5) . . ? C5 C12 C14 109.5(4) . . ? C13 C12 C14 108.2(5) . . ? C3 C19 P1 117.3(3) . . ? C25 C20 C21 119.3(4) . . ? C25 C20 P1 120.5(3) . . ? C21 C20 P1 120.0(3) . . ? C22 C21 C20 118.0(4) . . ? C22 C21 C26 116.9(4) . . ? C20 C21 C26 125.0(4) . . ? C23 C22 C21 123.7(5) . . ? C24 C23 C22 117.5(4) . . ? C24 C23 C27 121.3(6) . . ? C22 C23 C27 121.2(6) . . ? C23 C24 C25 122.8(5) . . ? C24 C25 C20 118.6(4) . . ? C24 C25 C28 116.7(4) . . ? C20 C25 C28 124.7(4) . . ? C31 C30 C35 119.0(3) . . ? C31 C30 P1 121.3(3) . . ? C35 C30 P1 119.6(3) . . ? C32 C31 C30 118.7(3) . . ? C32 C31 C36 115.8(3) . . ? C30 C31 C36 125.5(3) . . ? C33 C32 C31 122.6(4) . . ? C34 C33 C32 117.4(4) . . ? C34 C33 C37 122.2(4) . . ? C32 C33 C37 120.4(4) . . ? C33 C34 C35 122.8(4) . . ? C34 C35 C30 118.5(4) . . ? C34 C35 C38 117.2(4) . . ? C30 C35 C38 124.3(3) . . ? C1A Pd1A P1A 90.28(14) . . ? C1A Pd1A Cl1A 86.92(15) . . ? P1A Pd1A Cl1A 172.71(4) . . ? C1A Pd1A Cl1 169.88(15) . . ? P1A Pd1A Cl1 99.75(3) . . ? Cl1A Pd1A Cl1 82.96(3) . . ? Pd1 Cl1A Pd1A 98.10(4) . . ? C30A P1A C20A 107.0(2) . . ? C30A P1A C19A 105.8(2) . . ? C20A P1A C19A 99.1(2) . . ? C30A P1A Pd1A 109.82(13) . . ? C20A P1A Pd1A 124.66(13) . . ? C19A P1A Pd1A 108.72(12) . . ? C7A N1A C3A 118.7(3) . . ? N1A C3A C4A 122.3(3) . . ? N1A C3A C19A 115.6(3) . . ? C4A C3A C19A 122.0(3) . . ? C3A C4A C5A 120.0(3) . . ? C6A C5A C4A 116.5(4) . . ? C6A C5A C12A 121.9(4) . . ? C4A C5A C12A 121.6(4) . . ? C7A C6A C5A 120.7(4) . . ? N1A C7A C6A 121.7(4) . . ? N1A C7A C8A 114.9(4) . . ? C6A C7A C8A 123.3(4) . . ? C10A C8A C9A 107.7(5) . . ? C10A C8A C11A 109.4(5) . . ? C9A C8A C11A 108.8(6) . . ? C10A C8A C7A 113.2(4) . . ? C9A C8A C7A 108.9(4) . . ? C11A C8A C7A 108.9(4) . . ? C14A C12A C13A 108.6(8) . . ? C14A C12A C15A 110.6(9) . . ? C13A C12A C15A 105.4(8) . . ? C14A C12A C5A 109.1(5) . . ? C13A C12A C5A 113.4(4) . . ? C15A C12A C5A 109.7(5) . . ? C3A C19A P1A 117.1(3) . . ? C25A C20A C21A 118.8(4) . . ? C25A C20A P1A 120.4(3) . . ? C21A C20A P1A 120.4(3) . . ? C22A C21A C20A 118.3(4) . . ? C22A C21A C26A 116.3(4) . . ? C20A C21A C26A 125.5(4) . . ? C23A C22A C21A 123.1(5) . . ? C24A C23A C22A 117.9(5) . . ? C24A C23A C27A 121.1(6) . . ? C22A C23A C27A 120.9(6) . . ? C23A C24A C25A 122.8(5) . . ? C24A C25A C20A 118.9(4) . . ? C24A C25A C28A 116.9(4) . . ? C20A C25A C28A 124.2(4) . . ? C35A C30A C31A 119.1(4) . . ? C35A C30A P1A 119.6(3) . . ? C31A C30A P1A 121.3(3) . . ? C32A C31A C30A 119.3(4) . . ? C32A C31A C36A 116.7(4) . . ? C30A C31A C36A 124.0(4) . . ? C33A C32A C31A 122.0(5) . . ? C34A C33A C32A 118.1(4) . . ? C34A C33A C37A 120.8(6) . . ? C32A C33A C37A 121.1(5) . . ? C33A C34A C35A 123.2(5) . . ? C30A C35A C34A 117.7(4) . . ? C30A C35A C38A 123.8(4) . . ? C34A C35A C38A 118.4(4) . . ? _refine_diff_density_max 0.806 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.159