data_8a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H39 Cl2 N2 O P Pd' _chemical_formula_weight 603.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3128(9) _cell_length_b 11.2919(10) _cell_length_c 12.7707(11) _cell_angle_alpha 104.5880(10) _cell_angle_beta 99.9120(10) _cell_angle_gamma 97.6740(10) _cell_volume 1393.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 9026 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 21.67 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624.0 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8065 _exptl_absorpt_correction_T_max 0.8646 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 7 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10961 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 21.68 _reflns_number_total 2611 _reflns_number_gt 2452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054' _computing_cell_refinement 'Bruker SAINT v6.022' _computing_data_reduction 'Bruker SAINT v6.022' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2611 _refine_ls_number_parameters 305 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0514 _refine_ls_goodness_of_fit_ref 2.114 _refine_ls_restrained_S_all 2.114 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.72377(2) 0.71601(2) 0.670188(19) 0.01502(13) Uani 1 1 d . . . P1 P 0.71143(8) 0.91360(7) 0.76481(7) 0.0187(2) Uani 1 1 d . . . O1 O 0.89309(18) 0.77950(18) 0.61229(18) 0.0175(5) Uani 1 1 d . . . N1 N 0.8025(2) 0.5234(2) 0.5016(2) 0.0118(6) Uani 1 1 d . . . N2 N 0.7403(2) 0.4395(2) 0.6243(2) 0.0126(6) Uani 1 1 d . . . C1 C 0.7509(3) 0.5436(3) 0.5926(3) 0.0120(8) Uani 1 1 d . . . C2 C 0.8138(3) 0.3913(3) 0.4591(2) 0.0156(8) Uani 1 1 d . . . H2A H 0.9016 0.3838 0.4392 0.019 Uiso 1 1 calc R . . H2B H 0.7413 0.3470 0.3938 0.019 Uiso 1 1 calc R . . C3 C 0.8001(3) 0.3427(3) 0.5577(2) 0.0180(8) Uani 1 1 d . . . H3A H 0.7403 0.2603 0.5347 0.022 Uiso 1 1 calc R . . H3B H 0.8883 0.3366 0.5989 0.022 Uiso 1 1 calc R . . C4 C 0.8305(3) 0.6119(3) 0.4438(3) 0.0114(8) Uani 1 1 d . . . C5 C 0.8162(3) 0.5731(3) 0.3300(3) 0.0174(8) Uani 1 1 d . . . H5 H 0.7846 0.4875 0.2916 0.021 Uiso 1 1 calc R . . C6 C 0.8472(3) 0.6568(3) 0.2708(3) 0.0199(8) Uani 1 1 d . . . H6 H 0.8360 0.6294 0.1926 0.024 Uiso 1 1 calc R . . C7 C 0.8945(3) 0.7804(3) 0.3279(3) 0.0209(9) Uani 1 1 d . . . H7 H 0.9175 0.8388 0.2889 0.025 Uiso 1 1 calc R . . C8 C 0.9086(3) 0.8195(3) 0.4411(3) 0.0188(8) Uani 1 1 d . . . H8 H 0.9410 0.9052 0.4786 0.023 Uiso 1 1 calc R . . C9 C 0.8772(3) 0.7381(3) 0.5029(3) 0.0135(8) Uani 1 1 d . . . C10 C 0.7047(3) 0.4256(3) 0.7252(3) 0.0142(8) Uani 1 1 d . . . C11 C 0.5835(3) 0.3500(3) 0.7177(3) 0.0144(8) Uani 1 1 d . . . C12 C 0.5512(3) 0.3356(3) 0.8160(3) 0.0213(9) Uani 1 1 d . . . H12 H 0.4686 0.2844 0.8125 0.026 Uiso 1 1 calc R . . C13 C 0.6346(4) 0.3928(3) 0.9180(3) 0.0238(9) Uani 1 1 d . . . C14 C 0.7541(3) 0.4675(3) 0.9212(3) 0.0216(9) Uani 1 1 d . . . H14 H 0.8122 0.5083 0.9911 0.026 Uiso 1 1 calc R . . C15 C 0.7924(3) 0.4849(3) 0.8263(3) 0.0156(8) Uani 1 1 d . . . C16 C 0.4877(3) 0.2881(3) 0.6089(3) 0.0221(9) Uani 1 1 d . . . H16A H 0.4813 0.3471 0.5644 0.033 Uiso 1 1 calc R . . H16B H 0.3991 0.2610 0.6221 0.033 Uiso 1 1 calc R . . H16C H 0.5200 0.2156 0.5691 0.033 Uiso 1 1 calc R . . C17 C 0.5962(4) 0.3760(3) 1.0227(3) 0.0408(10) Uani 1 1 d . . . H17A H 0.5172 0.4132 1.0336 0.061 Uiso 1 1 calc R . . H17B H 0.6708 0.4168 1.0860 0.061 Uiso 1 1 calc R . . H17C H 0.5755 0.2869 1.0167 0.061 Uiso 1 1 calc R . . C18 C 0.9229(3) 0.5681(3) 0.8346(3) 0.0249(9) Uani 1 1 d . . . H18A H 0.9050 0.6455 0.8185 0.037 Uiso 1 1 calc R . . H18B H 0.9711 0.5255 0.7810 0.037 Uiso 1 1 calc R . . H18C H 0.9777 0.5874 0.9096 0.037 Uiso 1 1 calc R . . C19 C 0.5473(3) 0.6497(3) 0.7055(3) 0.0191(8) Uani 1 1 d . . . H19A H 0.5034 0.5720 0.6488 0.029 Uiso 1 1 calc R . . H19B H 0.4887 0.7113 0.7064 0.029 Uiso 1 1 calc R . . H19C H 0.5650 0.6340 0.7782 0.029 Uiso 1 1 calc R . . C20 C 0.6338(3) 0.9332(3) 0.8842(3) 0.0280(9) Uani 1 1 d . . . H20A H 0.6376 1.0230 0.9180 0.034 Uiso 1 1 calc R . . H20B H 0.5383 0.8923 0.8595 0.034 Uiso 1 1 calc R . . C21 C 0.7032(3) 0.8778(3) 0.9708(3) 0.0379(10) Uani 1 1 d . . . H21A H 0.6975 0.7884 0.9382 0.057 Uiso 1 1 calc R . . H21B H 0.6592 0.8907 1.0339 0.057 Uiso 1 1 calc R . . H21C H 0.7975 0.9188 0.9961 0.057 Uiso 1 1 calc R . . C22 C 0.8771(3) 1.0126(3) 0.8182(3) 0.0208(9) Uani 1 1 d . . . H22A H 0.9290 0.9772 0.8716 0.025 Uiso 1 1 calc R . . H22B H 0.9230 1.0075 0.7557 0.025 Uiso 1 1 calc R . . C23 C 0.8835(3) 1.1503(3) 0.8753(3) 0.0324(10) Uani 1 1 d . . . H23A H 0.8320 1.1874 0.8242 0.049 Uiso 1 1 calc R . . H23B H 0.9770 1.1937 0.8969 0.049 Uiso 1 1 calc R . . H23C H 0.8455 1.1580 0.9415 0.049 Uiso 1 1 calc R . . C24 C 0.6213(3) 0.9959(3) 0.6786(3) 0.0261(9) Uani 1 1 d . . . H24A H 0.5293 0.9480 0.6457 0.031 Uiso 1 1 calc R . . H24B H 0.6144 1.0782 0.7255 0.031 Uiso 1 1 calc R . . C25 C 0.6901(3) 1.0143(3) 0.5862(3) 0.0272(9) Uani 1 1 d . . . H25A H 0.7724 1.0769 0.6177 0.041 Uiso 1 1 calc R . . H25B H 0.6300 1.0426 0.5333 0.041 Uiso 1 1 calc R . . H25C H 0.7124 0.9353 0.5481 0.041 Uiso 1 1 calc R . . Cl1 Cl 0.27208(9) 0.94685(8) 0.67942(8) 0.0435(3) Uani 1 1 d . . . Cl2 Cl 0.23497(9) 0.80095(8) 0.83376(7) 0.0377(3) Uani 1 1 d . . . C31 C 0.1648(3) 0.8968(3) 0.7581(3) 0.0316(10) Uani 1 1 d . . . H31A H 0.0789 0.8500 0.7083 0.038 Uiso 1 1 calc R . . H31B H 0.1457 0.9703 0.8101 0.038 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 0.01445(19) 0.0139(2) 0.0165(2) 0.00301(14) 0.00421(13) 0.00306(12) P1 0.0173(5) 0.0163(6) 0.0210(6) 0.0017(5) 0.0059(4) 0.0029(4) O1 0.0153(13) 0.0188(13) 0.0159(16) 0.0005(12) 0.0058(11) -0.0006(10) N1 0.0135(15) 0.0098(18) 0.0142(18) 0.0038(15) 0.0063(14) 0.0042(12) N2 0.0158(16) 0.0134(17) 0.0103(17) 0.0032(14) 0.0064(13) 0.0042(13) C1 0.0058(18) 0.015(2) 0.014(2) 0.0042(18) -0.0012(17) 0.0013(15) C2 0.0156(19) 0.013(2) 0.020(2) 0.0037(17) 0.0058(16) 0.0049(15) C3 0.018(2) 0.015(2) 0.023(2) 0.0035(18) 0.0083(17) 0.0052(16) C4 0.0073(19) 0.016(2) 0.013(2) 0.006(2) 0.0047(16) 0.0040(16) C5 0.014(2) 0.014(2) 0.024(3) 0.004(2) 0.0058(17) 0.0035(15) C6 0.022(2) 0.026(3) 0.014(2) 0.005(2) 0.0070(17) 0.0064(18) C7 0.022(2) 0.024(3) 0.025(3) 0.014(2) 0.0135(18) 0.0084(18) C8 0.017(2) 0.011(2) 0.027(3) 0.002(2) 0.0081(17) 0.0008(15) C9 0.0053(18) 0.016(2) 0.021(3) 0.005(2) 0.0060(17) 0.0034(16) C10 0.017(2) 0.013(2) 0.017(3) 0.0064(18) 0.006(2) 0.0098(18) C11 0.017(2) 0.010(2) 0.019(2) 0.0052(18) 0.0070(19) 0.0090(17) C12 0.022(2) 0.013(2) 0.034(3) 0.010(2) 0.013(2) 0.0055(16) C13 0.037(3) 0.019(2) 0.022(3) 0.009(2) 0.016(2) 0.0138(19) C14 0.032(3) 0.019(2) 0.012(2) 0.0010(18) 0.0003(19) 0.0117(19) C15 0.017(2) 0.012(2) 0.018(2) 0.0021(18) 0.003(2) 0.0084(17) C16 0.019(2) 0.019(2) 0.029(2) 0.0058(18) 0.0059(18) 0.0054(16) C17 0.062(3) 0.041(3) 0.032(3) 0.020(2) 0.023(2) 0.018(2) C18 0.024(2) 0.027(2) 0.019(2) 0.0008(17) 0.0006(17) 0.0075(18) C19 0.017(2) 0.018(2) 0.022(2) 0.0048(17) 0.0060(16) 0.0031(16) C20 0.023(2) 0.023(2) 0.032(2) -0.0037(19) 0.0116(18) -0.0047(17) C21 0.046(3) 0.039(3) 0.022(2) -0.001(2) 0.016(2) -0.009(2) C22 0.020(2) 0.023(2) 0.019(2) 0.0029(18) 0.0081(16) 0.0024(16) C23 0.029(2) 0.028(2) 0.033(2) -0.004(2) 0.0150(19) -0.0054(17) C24 0.023(2) 0.020(2) 0.032(2) 0.0009(18) 0.0052(18) 0.0056(16) C25 0.033(2) 0.020(2) 0.029(2) 0.0107(18) 0.0018(19) 0.0073(17) Cl1 0.0458(7) 0.0371(6) 0.0562(7) 0.0182(5) 0.0211(5) 0.0142(5) Cl2 0.0434(6) 0.0397(6) 0.0255(6) 0.0043(5) 0.0056(5) 0.0040(5) C31 0.018(2) 0.042(2) 0.028(2) -0.0048(19) 0.0009(18) 0.0129(17) _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 2.030(3) . yes Pd1 C19 2.041(3) . yes Pd1 O1 2.1182(19) . yes Pd1 P1 2.2858(9) . yes P1 C20 1.820(3) . ? P1 C24 1.826(3) . ? P1 C22 1.827(3) . ? O1 C9 1.329(4) . ? N1 C1 1.340(3) . ? N1 C4 1.413(4) . ? N1 C2 1.481(3) . ? N2 C1 1.334(3) . ? N2 C10 1.438(4) . ? N2 C3 1.480(3) . ? C2 C3 1.515(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.383(4) . ? C4 C9 1.408(4) . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 C7 1.378(4) . ? C6 H6 0.9500 . ? C7 C8 1.377(4) . ? C7 H7 0.9500 . ? C8 C9 1.395(4) . ? C8 H8 0.9500 . ? C10 C11 1.390(4) . ? C10 C15 1.390(4) . ? C11 C12 1.395(4) . ? C11 C16 1.500(4) . ? C12 C13 1.377(4) . ? C12 H12 0.9500 . ? C13 C14 1.385(4) . ? C13 C17 1.507(4) . ? C14 C15 1.389(4) . ? C14 H14 0.9500 . ? C15 C18 1.507(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.524(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.529(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.520(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? Cl1 C31 1.747(3) . ? Cl2 C31 1.768(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 C19 93.37(12) . . yes C1 Pd1 O1 84.61(10) . . yes C19 Pd1 O1 172.65(10) . . yes C1 Pd1 P1 175.26(8) . . yes C19 Pd1 P1 90.02(9) . . yes O1 Pd1 P1 92.44(6) . . yes C20 P1 C24 104.05(15) . . ? C20 P1 C22 104.50(15) . . ? C24 P1 C22 103.70(14) . . ? C20 P1 Pd1 118.05(11) . . ? C24 P1 Pd1 113.40(11) . . ? C22 P1 Pd1 111.75(10) . . ? C9 O1 Pd1 112.98(17) . . ? C1 N1 C4 125.4(3) . . ? C1 N1 C2 112.2(2) . . ? C4 N1 C2 122.1(3) . . ? C1 N2 C10 126.3(3) . . ? C1 N2 C3 112.5(2) . . ? C10 N2 C3 119.9(2) . . ? N2 C1 N1 108.3(3) . . ? N2 C1 Pd1 130.0(2) . . ? N1 C1 Pd1 121.3(2) . . ? N1 C2 C3 101.8(2) . . ? N1 C2 H2A 111.4 . . ? C3 C2 H2A 111.4 . . ? N1 C2 H2B 111.4 . . ? C3 C2 H2B 111.4 . . ? H2A C2 H2B 109.3 . . ? N2 C3 C2 101.8(2) . . ? N2 C3 H3A 111.4 . . ? C2 C3 H3A 111.4 . . ? N2 C3 H3B 111.4 . . ? C2 C3 H3B 111.4 . . ? H3A C3 H3B 109.3 . . ? C5 C4 C9 120.7(3) . . ? C5 C4 N1 119.6(3) . . ? C9 C4 N1 119.7(3) . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 118.7(3) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C7 C8 120.2(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 122.6(3) . . ? C7 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? O1 C9 C8 120.7(3) . . ? O1 C9 C4 122.7(3) . . ? C8 C9 C4 116.6(3) . . ? C11 C10 C15 122.0(3) . . ? C11 C10 N2 118.2(3) . . ? C15 C10 N2 119.8(3) . . ? C10 C11 C12 117.7(3) . . ? C10 C11 C16 122.0(3) . . ? C12 C11 C16 120.3(3) . . ? C13 C12 C11 122.4(3) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 117.8(3) . . ? C12 C13 C17 121.0(3) . . ? C14 C13 C17 121.2(3) . . ? C13 C14 C15 122.5(3) . . ? C13 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? C14 C15 C10 117.6(3) . . ? C14 C15 C18 120.3(3) . . ? C10 C15 C18 122.0(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Pd1 C19 H19A 109.5 . . ? Pd1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Pd1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 P1 111.8(2) . . ? C21 C20 H20A 109.3 . . ? P1 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? P1 C20 H20B 109.3 . . ? H20A C20 H20B 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 P1 117.5(2) . . ? C23 C22 H22A 107.9 . . ? P1 C22 H22A 107.9 . . ? C23 C22 H22B 107.9 . . ? P1 C22 H22B 107.9 . . ? H22A C22 H22B 107.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 P1 112.2(2) . . ? C25 C24 H24A 109.2 . . ? P1 C24 H24A 109.2 . . ? C25 C24 H24B 109.2 . . ? P1 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Cl1 C31 Cl2 111.80(17) . . ? Cl1 C31 H31A 109.3 . . ? Cl2 C31 H31A 109.3 . . ? Cl1 C31 H31B 109.3 . . ? Cl2 C31 H31B 109.3 . . ? H31A C31 H31B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.795 _diffrn_reflns_theta_full 21.68 _diffrn_measured_fraction_theta_full 0.795 _refine_diff_density_max 0.281 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.050 #===END data_8d _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H59 N2 O P Pd' _chemical_formula_weight 853.37 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' '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 15.1511(9) _cell_length_b 17.8042(11) _cell_length_c 21.5514(13) _cell_angle_alpha 100.3810(10) _cell_angle_beta 102.6620(10) _cell_angle_gamma 105.9370(10) _cell_volume 5272.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18959 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.64 _exptl_crystal_description Fragment _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8788 _exptl_absorpt_correction_T_max 0.9716 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000' _diffrn_measurement_method '\w scans at 5 \f settings' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79175 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.1128 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 28.52 _reflns_number_total 24246 _reflns_number_gt 14224 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v5.054' _computing_cell_refinement 'Bruker SAINT v6.45' _computing_data_reduction 'Bruker SAINT v6.45' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 Sigma _refine_ls_weighting_details 'w=1/s^2^(Fo^2^)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 24246 _refine_ls_number_parameters 1009 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.120811(15) 0.614332(15) 0.789323(12) 0.01795(6) Uani 1 1 d . . . P1A P 0.07453(5) 0.57220(5) 0.87546(4) 0.01911(18) Uani 1 1 d . . . O1A O 0.22815(12) 0.55737(12) 0.79569(9) 0.0192(5) Uani 1 1 d . . . N1A N 0.18802(15) 0.73113(15) 0.70793(12) 0.0201(6) Uani 1 1 d . . . N2A N 0.20801(15) 0.61438(14) 0.68132(12) 0.0195(6) Uani 1 1 d . . . C1A C 0.17171(18) 0.65828(18) 0.71997(14) 0.0182(7) Uani 1 1 d . . . C2A C 0.2515(2) 0.74345(19) 0.66485(16) 0.0282(8) Uani 1 1 d . . . H2AA H 0.3179 0.7768 0.6904 0.034 Uiso 1 1 calc R . . H2AB H 0.2280 0.7691 0.6305 0.034 Uiso 1 1 calc R . . C3A C 0.2450(2) 0.65789(18) 0.63546(16) 0.0276(8) Uani 1 1 d . . . H3AA H 0.2004 0.6366 0.5905 0.033 Uiso 1 1 calc R . . H3AB H 0.3086 0.6542 0.6341 0.033 Uiso 1 1 calc R . . C4A C 0.1692(2) 0.79860(18) 0.74296(16) 0.0212(7) Uani 1 1 d . . . C5A C 0.0927(2) 0.82173(18) 0.71058(15) 0.0212(7) Uani 1 1 d . . . C6A C 0.0741(2) 0.88587(19) 0.74592(17) 0.0272(8) Uani 1 1 d . . . H6AA H 0.0225 0.9021 0.7258 0.033 Uiso 1 1 calc R . . C7A C 0.1278(2) 0.9264(2) 0.80888(17) 0.0315(8) Uani 1 1 d . . . H7AA H 0.1136 0.9704 0.8319 0.038 Uiso 1 1 calc R . . C8A C 0.2028(2) 0.90342(19) 0.83914(17) 0.0305(8) Uani 1 1 d . . . H8AA H 0.2393 0.9313 0.8832 0.037 Uiso 1 1 calc R . . C9A C 0.2255(2) 0.84079(18) 0.80649(15) 0.0214(7) Uani 1 1 d . . . C10A C 0.0329(2) 0.77911(19) 0.64095(15) 0.0259(8) Uani 1 1 d . . . H10A H 0.0457 0.7272 0.6279 0.031 Uiso 1 1 calc R . . C11A C 0.0595(2) 0.8306(2) 0.59391(16) 0.0332(8) Uani 1 1 d . . . H11A H 0.1279 0.8429 0.5977 0.050 Uiso 1 1 calc R . . H11B H 0.0456 0.8811 0.6053 0.050 Uiso 1 1 calc R . . H11C H 0.0221 0.8008 0.5487 0.050 Uiso 1 1 calc R . . C12A C -0.0752(2) 0.7598(2) 0.63381(17) 0.0372(9) Uani 1 1 d . . . H12A H -0.0933 0.7261 0.6632 0.056 Uiso 1 1 calc R . . H12B H -0.1117 0.7308 0.5882 0.056 Uiso 1 1 calc R . . H12C H -0.0891 0.8102 0.6455 0.056 Uiso 1 1 calc R . . C13A C 0.31435(19) 0.82318(19) 0.84054(16) 0.0265(8) Uani 1 1 d . . . H13A H 0.3157 0.7720 0.8133 0.032 Uiso 1 1 calc R . . C14A C 0.4045(2) 0.8916(2) 0.84467(19) 0.0421(10) Uani 1 1 d . . . H14A H 0.4038 0.8985 0.8005 0.063 Uiso 1 1 calc R . . H14B H 0.4614 0.8781 0.8633 0.063 Uiso 1 1 calc R . . H14C H 0.4058 0.9419 0.8728 0.063 Uiso 1 1 calc R . . C15A C 0.3129(2) 0.8121(2) 0.90900(16) 0.0395(9) Uani 1 1 d . . . H15A H 0.2551 0.7681 0.9055 0.059 Uiso 1 1 calc R . . H15B H 0.3131 0.8622 0.9368 0.059 Uiso 1 1 calc R . . H15C H 0.3696 0.7989 0.9286 0.059 Uiso 1 1 calc R . . C16A C 0.20934(18) 0.53522(18) 0.68014(15) 0.0193(7) Uani 1 1 d . . . C17A C 0.1992(2) 0.48410(19) 0.62013(16) 0.0258(8) Uani 1 1 d . . . H17A H 0.1842 0.5009 0.5808 0.031 Uiso 1 1 calc R . . C18A C 0.2107(2) 0.40986(19) 0.61689(16) 0.0253(7) Uani 1 1 d . . . C19A C 0.23782(19) 0.38932(18) 0.67609(15) 0.0238(7) Uani 1 1 d . . . H19A H 0.2502 0.3396 0.6744 0.029 Uiso 1 1 calc R . . C20A C 0.24773(18) 0.43707(17) 0.73703(15) 0.0173(7) Uani 1 1 d . . . C21A C 0.22691(18) 0.51136(18) 0.73983(14) 0.0181(7) Uani 1 1 d . . . C22A C 0.1957(3) 0.3525(2) 0.55191(16) 0.0439(10) Uani 1 1 d . . . H22A H 0.1767 0.3768 0.5160 0.066 Uiso 1 1 calc R . . H22B H 0.1453 0.3017 0.5468 0.066 Uiso 1 1 calc R . . H22C H 0.2554 0.3416 0.5507 0.066 Uiso 1 1 calc R . . C23A C 0.28089(19) 0.41134(17) 0.79995(15) 0.0195(7) Uani 1 1 d . . . C24A C 0.3122(2) 0.33592(19) 0.78623(16) 0.0301(8) Uani 1 1 d . . . H24A H 0.2574 0.2902 0.7557 0.036 Uiso 1 1 calc R . . H24B H 0.3640 0.3470 0.7646 0.036 Uiso 1 1 calc R . . C25A C 0.20014(19) 0.39090(19) 0.83313(15) 0.0238(7) Uani 1 1 d . . . H25A H 0.1802 0.4389 0.8444 0.029 Uiso 1 1 calc R . . H25B H 0.1441 0.3469 0.8021 0.029 Uiso 1 1 calc R . . C26A C 0.36714(19) 0.47860(18) 0.84984(15) 0.0259(8) Uani 1 1 d . . . H26A H 0.4209 0.4908 0.8301 0.031 Uiso 1 1 calc R . . H26B H 0.3498 0.5282 0.8600 0.031 Uiso 1 1 calc R . . C27A C 0.3476(2) 0.3124(2) 0.84969(17) 0.0333(9) Uani 1 1 d . . . H27A H 0.3682 0.2641 0.8390 0.040 Uiso 1 1 calc R . . C28A C 0.2638(2) 0.29090(19) 0.88012(17) 0.0326(9) Uani 1 1 d . . . H28A H 0.2095 0.2455 0.8488 0.039 Uiso 1 1 calc R . . H28B H 0.2842 0.2742 0.9208 0.039 Uiso 1 1 calc R . . C29A C 0.2333(2) 0.36466(19) 0.89563(16) 0.0279(8) Uani 1 1 d . . . H29A H 0.1792 0.3513 0.9157 0.033 Uiso 1 1 calc R . . C30A C 0.3170(2) 0.4348(2) 0.94460(16) 0.0320(8) Uani 1 1 d . . . H30A H 0.3380 0.4194 0.9859 0.038 Uiso 1 1 calc R . . H30B H 0.2967 0.4827 0.9552 0.038 Uiso 1 1 calc R . . C31A C 0.3995(2) 0.4548(2) 0.91375(17) 0.0320(8) Uani 1 1 d . . . H31A H 0.4548 0.5004 0.9453 0.038 Uiso 1 1 calc R . . C32A C 0.4303(2) 0.3806(2) 0.89789(17) 0.0367(9) Uani 1 1 d . . . H32A H 0.4514 0.3643 0.9387 0.044 Uiso 1 1 calc R . . H32B H 0.4847 0.3935 0.8788 0.044 Uiso 1 1 calc R . . C33A C 0.01062(19) 0.65998(19) 0.77197(15) 0.0254(8) Uani 1 1 d . . . H33A H 0.0118 0.6842 0.7346 0.038 Uiso 1 1 calc R . . H33B H 0.0175 0.7013 0.8111 0.038 Uiso 1 1 calc R . . H33C H -0.0504 0.6164 0.7618 0.038 Uiso 1 1 calc R . . C34A C -0.00364(19) 0.61785(18) 0.91002(14) 0.0197(7) Uani 1 1 d . . . C35A C -0.09289(19) 0.57202(19) 0.91354(15) 0.0248(7) Uani 1 1 d . . . H35A H -0.1163 0.5152 0.8952 0.030 Uiso 1 1 calc R . . C36A C -0.1471(2) 0.6093(2) 0.94363(16) 0.0301(8) Uani 1 1 d . . . H36A H -0.2071 0.5777 0.9464 0.036 Uiso 1 1 calc R . . C37A C -0.1152(2) 0.6914(2) 0.96951(16) 0.0327(9) Uani 1 1 d . . . H37A H -0.1533 0.7168 0.9894 0.039 Uiso 1 1 calc R . . C38A C -0.0256(2) 0.7375(2) 0.96630(16) 0.0312(8) Uani 1 1 d . . . H38A H -0.0019 0.7943 0.9849 0.037 Uiso 1 1 calc R . . C39A C 0.0275(2) 0.7000(2) 0.93606(15) 0.0266(8) Uani 1 1 d . . . H39A H 0.0874 0.7317 0.9331 0.032 Uiso 1 1 calc R . . C40A C 0.00965(19) 0.46502(18) 0.85512(15) 0.0199(7) Uani 1 1 d . . . C41A C -0.0574(2) 0.4313(2) 0.79378(16) 0.0294(8) Uani 1 1 d . . . H41A H -0.0657 0.4643 0.7643 0.035 Uiso 1 1 calc R . . C42A C -0.1121(2) 0.3506(2) 0.77506(17) 0.0344(9) Uani 1 1 d . . . H42A H -0.1581 0.3285 0.7331 0.041 Uiso 1 1 calc R . . C43A C -0.1003(2) 0.3023(2) 0.81704(17) 0.0316(8) Uani 1 1 d . . . H43A H -0.1379 0.2468 0.8041 0.038 Uiso 1 1 calc R . . C44A C -0.0337(2) 0.3344(2) 0.87801(17) 0.0287(8) Uani 1 1 d . . . H44A H -0.0254 0.3010 0.9071 0.034 Uiso 1 1 calc R . . C45A C 0.0210(2) 0.41536(18) 0.89673(15) 0.0218(7) Uani 1 1 d . . . H45A H 0.0670 0.4372 0.9387 0.026 Uiso 1 1 calc R . . C46A C 0.17432(19) 0.59722(17) 0.94925(14) 0.0187(7) Uani 1 1 d . . . C47A C 0.1609(2) 0.59681(18) 1.01090(15) 0.0220(7) Uani 1 1 d . . . H47A H 0.0978 0.5775 1.0147 0.026 Uiso 1 1 calc R . . C48A C 0.2375(2) 0.62384(19) 1.06665(16) 0.0270(8) Uani 1 1 d . . . H48A H 0.2271 0.6237 1.1085 0.032 Uiso 1 1 calc R . . C49A C 0.3303(2) 0.65142(19) 1.06135(16) 0.0284(8) Uani 1 1 d . . . H49A H 0.3836 0.6705 1.0995 0.034 Uiso 1 1 calc R . . C50A C 0.3437(2) 0.65068(19) 1.00045(15) 0.0262(8) Uani 1 1 d . . . H50A H 0.4070 0.6688 0.9969 0.031 Uiso 1 1 calc R . . C51A C 0.2682(2) 0.62448(18) 0.94440(15) 0.0229(7) Uani 1 1 d . . . H51A H 0.2793 0.6248 0.9027 0.028 Uiso 1 1 calc R . . Pd2 Pd 0.673991(16) 0.865510(15) 0.701541(13) 0.02302(7) Uani 1 1 d . . . P1B P 0.60134(5) 0.91268(5) 0.61902(4) 0.0240(2) Uani 1 1 d . . . O1B O 0.81421(13) 0.92816(12) 0.69815(10) 0.0230(5) Uani 1 1 d . . . N1B N 0.71726(16) 0.74003(16) 0.77271(13) 0.0271(7) Uani 1 1 d . . . N2B N 0.83153(16) 0.85469(15) 0.80248(12) 0.0231(6) Uani 1 1 d . . . C1B C 0.7415(2) 0.81612(19) 0.76625(16) 0.0254(8) Uani 1 1 d . . . C2B C 0.80150(19) 0.72237(19) 0.80849(17) 0.0298(8) Uani 1 1 d . . . H2BA H 0.8280 0.6930 0.7778 0.036 Uiso 1 1 calc R . . H2BB H 0.7855 0.6907 0.8402 0.036 Uiso 1 1 calc R . . C3B C 0.8691(2) 0.80587(19) 0.84290(17) 0.0316(8) Uani 1 1 d . . . H3BA H 0.8669 0.8221 0.8888 0.038 Uiso 1 1 calc R . . H3BB H 0.9357 0.8102 0.8429 0.038 Uiso 1 1 calc R . . C4B C 0.6282(2) 0.67553(19) 0.73913(17) 0.0255(8) Uani 1 1 d . . . C5B C 0.5613(2) 0.65719(19) 0.77515(17) 0.0291(8) Uani 1 1 d . . . C6B C 0.4751(2) 0.5967(2) 0.7423(2) 0.0375(9) Uani 1 1 d . . . H6BA H 0.4269 0.5844 0.7641 0.045 Uiso 1 1 calc R . . C7B C 0.4580(2) 0.5541(2) 0.6784(2) 0.0405(10) Uani 1 1 d . . . H7BA H 0.3988 0.5120 0.6571 0.049 Uiso 1 1 calc R . . C8B C 0.5263(2) 0.5720(2) 0.64483(19) 0.0378(9) Uani 1 1 d . . . H8BA H 0.5137 0.5420 0.6008 0.045 Uiso 1 1 calc R . . C9B C 0.6130(2) 0.6334(2) 0.67522(18) 0.0292(8) Uani 1 1 d . . . C10B C 0.5801(2) 0.7006(2) 0.84637(16) 0.0301(8) Uani 1 1 d . . . H10B H 0.6326 0.7532 0.8562 0.036 Uiso 1 1 calc R . . C11B C 0.6133(2) 0.6523(2) 0.89320(18) 0.0448(10) Uani 1 1 d . . . H11D H 0.6693 0.6400 0.8844 0.067 Uiso 1 1 calc R . . H11E H 0.5615 0.6018 0.8864 0.067 Uiso 1 1 calc R . . H11F H 0.6304 0.6842 0.9388 0.067 Uiso 1 1 calc R . . C12B C 0.4926(2) 0.7189(2) 0.85902(19) 0.0442(10) Uani 1 1 d . . . H12D H 0.4716 0.7499 0.8290 0.066 Uiso 1 1 calc R . . H12E H 0.5087 0.7505 0.9046 0.066 Uiso 1 1 calc R . . H12F H 0.4410 0.6681 0.8517 0.066 Uiso 1 1 calc R . . C13B C 0.6873(2) 0.6507(2) 0.63783(17) 0.0319(8) Uani 1 1 d . . . H13B H 0.7428 0.6985 0.6662 0.038 Uiso 1 1 calc R . . C14B C 0.7239(2) 0.5787(2) 0.62408(19) 0.0460(10) Uani 1 1 d . . . H14D H 0.7494 0.5667 0.6657 0.069 Uiso 1 1 calc R . . H14E H 0.7747 0.5923 0.6025 0.069 Uiso 1 1 calc R . . H14F H 0.6711 0.5314 0.5953 0.069 Uiso 1 1 calc R . . C15B C 0.6484(2) 0.6712(2) 0.57424(18) 0.0432(10) Uani 1 1 d . . . H15D H 0.6255 0.7172 0.5839 0.065 Uiso 1 1 calc R . . H15E H 0.5953 0.6245 0.5448 0.065 Uiso 1 1 calc R . . H15F H 0.6993 0.6853 0.5529 0.065 Uiso 1 1 calc R . . C16B C 0.8860(2) 0.93639(18) 0.80987(16) 0.0228(7) Uani 1 1 d . . . C17B C 0.9519(2) 0.97853(19) 0.87020(15) 0.0249(7) Uani 1 1 d . . . H17B H 0.9543 0.9542 0.9060 0.030 Uiso 1 1 calc R . . C18B C 1.0135(2) 1.05453(19) 0.87929(15) 0.0246(7) Uani 1 1 d . . . C19B C 1.0091(2) 1.08639(19) 0.82473(16) 0.0247(7) Uani 1 1 d . . . H19B H 1.0522 1.1388 0.8303 0.030 Uiso 1 1 calc R . . C20B C 0.94615(19) 1.04678(18) 0.76291(15) 0.0200(7) Uani 1 1 d . . . C21B C 0.8779(2) 0.96926(18) 0.75448(15) 0.0213(7) Uani 1 1 d . . . C22B C 1.0903(2) 1.0976(2) 0.94366(16) 0.0412(9) Uani 1 1 d . . . H22D H 1.0813 1.0661 0.9760 0.062 Uiso 1 1 calc R . . H22E H 1.0859 1.1512 0.9599 0.062 Uiso 1 1 calc R . . H22F H 1.1534 1.1036 0.9368 0.062 Uiso 1 1 calc R . . C23B C 0.95409(19) 1.08297(17) 0.70405(15) 0.0205(7) Uani 1 1 d . . . C24B C 0.9792(2) 1.02779(19) 0.65291(15) 0.0256(8) Uani 1 1 d . . . H24C H 0.9290 0.9740 0.6381 0.031 Uiso 1 1 calc R . . H24D H 1.0405 1.0207 0.6734 0.031 Uiso 1 1 calc R . . C25B C 1.0331(2) 1.16626(19) 0.72430(16) 0.0333(8) Uani 1 1 d . . . H25C H 1.0183 1.2042 0.7569 0.040 Uiso 1 1 calc R . . H25D H 1.0951 1.1608 0.7455 0.040 Uiso 1 1 calc R . . C26B C 0.8601(2) 1.0951(2) 0.67042(16) 0.0283(8) Uani 1 1 d . . . H26C H 0.8076 1.0427 0.6558 0.034 Uiso 1 1 calc R . . H26D H 0.8438 1.1325 0.7025 0.034 Uiso 1 1 calc R . . C27B C 0.9879(2) 1.0614(2) 0.59325(17) 0.0347(9) Uani 1 1 d . . . H27B H 1.0040 1.0235 0.5607 0.042 Uiso 1 1 calc R . . C28B C 1.0661(2) 1.1438(2) 0.61608(17) 0.0384(10) Uani 1 1 d . . . H28C H 1.1282 1.1379 0.6365 0.046 Uiso 1 1 calc R . . H28D H 1.0720 1.1663 0.5778 0.046 Uiso 1 1 calc R . . C29B C 1.0416(2) 1.2007(2) 0.66547(17) 0.0346(9) Uani 1 1 d . . . H29B H 1.0937 1.2542 0.6806 0.042 Uiso 1 1 calc R . . C30B C 0.9470(2) 1.21196(19) 0.63294(17) 0.0355(9) Uani 1 1 d . . . H30C H 0.9525 1.2340 0.5944 0.043 Uiso 1 1 calc R . . H30D H 0.9311 1.2502 0.6646 0.043 Uiso 1 1 calc R . . C31B C 0.8691(2) 1.1295(2) 0.61132(17) 0.0321(9) Uani 1 1 d . . . H31B H 0.8067 1.1357 0.5902 0.039 Uiso 1 1 calc R . . C32B C 0.8935(2) 1.0729(2) 0.56158(16) 0.0347(9) Uani 1 1 d . . . H32C H 0.8992 1.0955 0.5234 0.042 Uiso 1 1 calc R . . H32D H 0.8417 1.0200 0.5457 0.042 Uiso 1 1 calc R . . C33B C 0.5444(2) 0.81514(19) 0.71508(17) 0.0313(8) Uani 1 1 d . . . H33D H 0.5522 0.7878 0.7505 0.047 Uiso 1 1 calc R . . H33E H 0.5016 0.7759 0.6743 0.047 Uiso 1 1 calc R . . H33F H 0.5167 0.8575 0.7270 0.047 Uiso 1 1 calc R . . C34B C 0.47237(19) 0.8668(2) 0.58163(15) 0.0249(8) Uani 1 1 d . . . C35B C 0.4092(2) 0.9105(2) 0.57722(16) 0.0296(8) Uani 1 1 d . . . H35B H 0.4322 0.9671 0.5964 0.036 Uiso 1 1 calc R . . C36B C 0.3128(2) 0.8720(2) 0.54490(17) 0.0359(9) Uani 1 1 d . . . H36B H 0.2702 0.9025 0.5426 0.043 Uiso 1 1 calc R . . C37B C 0.2777(2) 0.7900(2) 0.51599(17) 0.0348(9) Uani 1 1 d . . . H37B H 0.2116 0.7643 0.4934 0.042 Uiso 1 1 calc R . . C38B C 0.3394(2) 0.7460(2) 0.52033(16) 0.0354(9) Uani 1 1 d . . . H38B H 0.3159 0.6894 0.5009 0.042 Uiso 1 1 calc R . . C39B C 0.4359(2) 0.7837(2) 0.55300(16) 0.0321(8) Uani 1 1 d . . . H39B H 0.4778 0.7526 0.5559 0.039 Uiso 1 1 calc R . . C40B C 0.61608(19) 1.01900(19) 0.64523(16) 0.0238(7) Uani 1 1 d . . . C41B C 0.6172(2) 1.0485(2) 0.70977(18) 0.0361(9) Uani 1 1 d . . . H41B H 0.6108 1.0129 0.7377 0.043 Uiso 1 1 calc R . . C42B C 0.6276(2) 1.1289(2) 0.73405(18) 0.0406(9) Uani 1 1 d . . . H42B H 0.6282 1.1481 0.7783 0.049 Uiso 1 1 calc R . . C43B C 0.6370(2) 1.1812(2) 0.69380(19) 0.0375(9) Uani 1 1 d . . . H43B H 0.6436 1.2363 0.7102 0.045 Uiso 1 1 calc R . . C44B C 0.6368(2) 1.1532(2) 0.63010(19) 0.0344(9) Uani 1 1 d . . . H44B H 0.6436 1.1892 0.6025 0.041 Uiso 1 1 calc R . . C45B C 0.6268(2) 1.0733(2) 0.60581(18) 0.0321(9) Uani 1 1 d . . . H45B H 0.6272 1.0549 0.5617 0.038 Uiso 1 1 calc R . . C46B C 0.6436(2) 0.89735(18) 0.54638(16) 0.0243(8) Uani 1 1 d . . . C47B C 0.7236(2) 0.87163(19) 0.54981(17) 0.0262(7) Uani 1 1 d . . . H47B H 0.7580 0.8663 0.5904 0.031 Uiso 1 1 calc R . . C48B C 0.7524(2) 0.85407(19) 0.49412(17) 0.0322(8) Uani 1 1 d . . . H48B H 0.8064 0.8362 0.4967 0.039 Uiso 1 1 calc R . . C49B C 0.7042(2) 0.8620(2) 0.43472(18) 0.0395(9) Uani 1 1 d . . . H49B H 0.7252 0.8502 0.3968 0.047 Uiso 1 1 calc R . . C50B C 0.6248(2) 0.8875(2) 0.43083(18) 0.0412(10) Uani 1 1 d . . . H50B H 0.5910 0.8930 0.3901 0.049 Uiso 1 1 calc R . . C51B C 0.5952(2) 0.9048(2) 0.48636(16) 0.0335(9) Uani 1 1 d . . . H51B H 0.5407 0.9221 0.4834 0.040 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 0.01505(12) 0.02401(15) 0.02112(15) 0.01168(12) 0.00875(11) 0.00962(11) P1A 0.0160(4) 0.0256(5) 0.0207(5) 0.0109(4) 0.0078(4) 0.0095(4) O1A 0.0183(10) 0.0263(12) 0.0180(12) 0.0076(10) 0.0074(9) 0.0122(9) N1A 0.0209(13) 0.0241(15) 0.0243(15) 0.0123(12) 0.0137(12) 0.0118(12) N2A 0.0220(13) 0.0210(15) 0.0231(15) 0.0122(12) 0.0123(12) 0.0103(12) C1A 0.0149(15) 0.0207(18) 0.0210(18) 0.0089(15) 0.0032(13) 0.0084(13) C2A 0.0384(19) 0.030(2) 0.034(2) 0.0193(17) 0.0277(17) 0.0193(16) C3A 0.0341(18) 0.032(2) 0.030(2) 0.0186(17) 0.0205(16) 0.0169(16) C4A 0.0204(16) 0.0213(18) 0.032(2) 0.0134(16) 0.0176(15) 0.0101(14) C5A 0.0219(16) 0.0245(19) 0.0266(19) 0.0160(16) 0.0135(15) 0.0108(14) C6A 0.0275(18) 0.030(2) 0.042(2) 0.0235(18) 0.0207(17) 0.0186(16) C7A 0.0321(19) 0.032(2) 0.040(2) 0.0093(18) 0.0197(18) 0.0179(17) C8A 0.0300(19) 0.029(2) 0.033(2) 0.0048(17) 0.0093(16) 0.0107(16) C9A 0.0230(16) 0.0229(18) 0.0253(19) 0.0109(15) 0.0115(15) 0.0117(15) C10A 0.0250(17) 0.0275(19) 0.030(2) 0.0120(16) 0.0076(15) 0.0134(15) C11A 0.0307(19) 0.042(2) 0.034(2) 0.0199(18) 0.0123(17) 0.0141(17) C12A 0.0254(18) 0.050(2) 0.044(2) 0.024(2) 0.0107(17) 0.0172(17) C13A 0.0203(16) 0.0234(19) 0.036(2) 0.0093(16) 0.0046(15) 0.0097(14) C14A 0.0211(18) 0.038(2) 0.072(3) 0.022(2) 0.0140(19) 0.0120(17) C15A 0.040(2) 0.046(2) 0.039(2) 0.0195(19) 0.0086(18) 0.0211(18) C16A 0.0117(14) 0.0228(18) 0.0290(19) 0.0111(15) 0.0097(14) 0.0086(13) C17A 0.0257(17) 0.033(2) 0.0230(19) 0.0128(17) 0.0096(15) 0.0096(16) C18A 0.0301(18) 0.0232(19) 0.0250(19) 0.0057(16) 0.0146(15) 0.0077(15) C19A 0.0221(16) 0.0197(18) 0.034(2) 0.0119(16) 0.0133(15) 0.0061(14) C20A 0.0115(14) 0.0184(17) 0.0233(18) 0.0080(15) 0.0087(13) 0.0025(13) C21A 0.0102(14) 0.0239(18) 0.0201(18) 0.0070(15) 0.0062(13) 0.0030(13) C22A 0.068(3) 0.038(2) 0.033(2) 0.0090(19) 0.022(2) 0.021(2) C23A 0.0157(15) 0.0201(18) 0.0290(19) 0.0118(15) 0.0085(14) 0.0103(13) C24A 0.0345(19) 0.031(2) 0.038(2) 0.0176(17) 0.0188(17) 0.0190(16) C25A 0.0169(15) 0.0265(19) 0.031(2) 0.0134(16) 0.0096(14) 0.0065(14) C26A 0.0176(16) 0.0284(19) 0.035(2) 0.0159(17) 0.0084(15) 0.0074(14) C27A 0.040(2) 0.033(2) 0.046(2) 0.0235(19) 0.0192(18) 0.0266(17) C28A 0.0288(18) 0.031(2) 0.043(2) 0.0209(18) 0.0089(17) 0.0110(16) C29A 0.0244(17) 0.032(2) 0.039(2) 0.0223(17) 0.0162(16) 0.0134(16) C30A 0.035(2) 0.038(2) 0.030(2) 0.0200(18) 0.0062(17) 0.0174(17) C31A 0.0228(17) 0.035(2) 0.037(2) 0.0186(18) 0.0026(16) 0.0067(16) C32A 0.0249(18) 0.051(2) 0.044(2) 0.026(2) 0.0095(17) 0.0189(18) C33A 0.0166(15) 0.038(2) 0.035(2) 0.0219(17) 0.0125(15) 0.0177(15) C34A 0.0167(15) 0.0280(19) 0.0221(18) 0.0150(15) 0.0080(14) 0.0122(14) C35A 0.0209(16) 0.031(2) 0.032(2) 0.0165(16) 0.0124(15) 0.0138(15) C36A 0.0248(18) 0.043(2) 0.040(2) 0.0264(19) 0.0201(16) 0.0195(17) C37A 0.035(2) 0.051(3) 0.036(2) 0.0250(19) 0.0238(17) 0.0311(18) C38A 0.039(2) 0.033(2) 0.032(2) 0.0154(17) 0.0137(17) 0.0200(17) C39A 0.0237(17) 0.037(2) 0.033(2) 0.0209(17) 0.0160(15) 0.0180(16) C40A 0.0135(15) 0.0290(19) 0.0233(18) 0.0097(15) 0.0115(14) 0.0100(14) C41A 0.0331(19) 0.030(2) 0.025(2) 0.0093(17) 0.0098(16) 0.0082(16) C42A 0.0272(18) 0.037(2) 0.033(2) 0.0044(18) 0.0077(16) 0.0039(17) C43A 0.0308(19) 0.028(2) 0.037(2) 0.0066(18) 0.0193(17) 0.0044(16) C44A 0.0280(18) 0.032(2) 0.035(2) 0.0131(17) 0.0178(17) 0.0141(16) C45A 0.0179(16) 0.0229(19) 0.0283(19) 0.0075(16) 0.0111(14) 0.0082(14) C46A 0.0199(16) 0.0183(17) 0.0207(18) 0.0078(14) 0.0049(14) 0.0094(13) C47A 0.0197(16) 0.0266(19) 0.0262(19) 0.0132(15) 0.0117(15) 0.0094(14) C48A 0.0324(19) 0.034(2) 0.0220(19) 0.0121(16) 0.0097(16) 0.0169(16) C49A 0.0269(18) 0.030(2) 0.027(2) 0.0083(16) -0.0014(15) 0.0143(15) C50A 0.0180(16) 0.033(2) 0.030(2) 0.0117(17) 0.0050(15) 0.0109(15) C51A 0.0197(16) 0.0289(18) 0.026(2) 0.0127(16) 0.0093(15) 0.0107(14) Pd2 0.01529(13) 0.02823(16) 0.03582(17) 0.02160(13) 0.01148(12) 0.01124(11) P1B 0.0155(4) 0.0315(5) 0.0343(5) 0.0207(4) 0.0105(4) 0.0116(4) O1B 0.0151(10) 0.0267(13) 0.0307(13) 0.0154(11) 0.0083(10) 0.0055(9) N1B 0.0149(13) 0.0335(17) 0.0448(18) 0.0299(15) 0.0120(13) 0.0110(12) N2B 0.0175(13) 0.0289(16) 0.0334(16) 0.0222(13) 0.0105(12) 0.0124(12) C1B 0.0192(16) 0.031(2) 0.038(2) 0.0235(17) 0.0163(15) 0.0112(15) C2B 0.0144(15) 0.034(2) 0.051(2) 0.0286(18) 0.0104(16) 0.0120(15) C3B 0.0229(17) 0.041(2) 0.046(2) 0.0305(19) 0.0154(16) 0.0169(16) C4B 0.0152(16) 0.0243(19) 0.045(2) 0.0231(18) 0.0072(16) 0.0105(14) C5B 0.0157(16) 0.032(2) 0.051(2) 0.0281(19) 0.0122(16) 0.0114(15) C6B 0.0225(18) 0.042(2) 0.062(3) 0.032(2) 0.0217(19) 0.0113(17) C7B 0.0222(18) 0.035(2) 0.064(3) 0.024(2) 0.0105(19) 0.0028(16) C8B 0.034(2) 0.030(2) 0.053(3) 0.0181(19) 0.0152(19) 0.0093(17) C9B 0.0207(17) 0.027(2) 0.050(2) 0.0218(18) 0.0155(17) 0.0110(15) C10B 0.0232(17) 0.033(2) 0.039(2) 0.0214(18) 0.0125(16) 0.0059(15) C11B 0.031(2) 0.063(3) 0.060(3) 0.040(2) 0.0191(19) 0.0251(19) C12B 0.037(2) 0.052(3) 0.065(3) 0.035(2) 0.034(2) 0.0213(19) C13B 0.0277(18) 0.028(2) 0.048(2) 0.0174(18) 0.0205(17) 0.0087(16) C14B 0.039(2) 0.041(2) 0.073(3) 0.024(2) 0.029(2) 0.0222(19) C15B 0.044(2) 0.045(2) 0.058(3) 0.025(2) 0.031(2) 0.0205(19) C16B 0.0181(16) 0.0207(18) 0.040(2) 0.0164(16) 0.0172(16) 0.0105(14) C17B 0.0256(17) 0.037(2) 0.0228(19) 0.0146(16) 0.0125(15) 0.0182(16) C18B 0.0244(17) 0.031(2) 0.0241(19) 0.0075(16) 0.0113(15) 0.0136(15) C19B 0.0196(16) 0.0228(18) 0.035(2) 0.0085(16) 0.0125(16) 0.0083(14) C20B 0.0175(15) 0.0237(18) 0.0265(19) 0.0113(15) 0.0109(14) 0.0117(14) C21B 0.0184(16) 0.0278(19) 0.0278(19) 0.0139(16) 0.0130(15) 0.0142(14) C22B 0.051(2) 0.040(2) 0.034(2) 0.0102(19) 0.0109(19) 0.0173(19) C23B 0.0154(15) 0.0179(17) 0.0316(19) 0.0108(15) 0.0078(14) 0.0069(13) C24B 0.0257(17) 0.029(2) 0.031(2) 0.0155(16) 0.0147(15) 0.0138(15) C25B 0.0305(19) 0.029(2) 0.039(2) 0.0148(17) 0.0107(17) 0.0038(16) C26B 0.0221(17) 0.034(2) 0.043(2) 0.0236(18) 0.0179(16) 0.0159(15) C27B 0.047(2) 0.041(2) 0.039(2) 0.0232(19) 0.0310(18) 0.0275(19) C28B 0.0277(18) 0.056(3) 0.053(2) 0.045(2) 0.0232(18) 0.0191(18) C29B 0.0246(18) 0.034(2) 0.045(2) 0.0233(19) 0.0089(17) 0.0018(16) C30B 0.038(2) 0.029(2) 0.047(2) 0.0234(19) 0.0162(18) 0.0113(17) C31B 0.0209(17) 0.039(2) 0.045(2) 0.0289(19) 0.0105(16) 0.0109(16) C32B 0.0324(19) 0.036(2) 0.033(2) 0.0230(18) 0.0058(17) 0.0000(17) C33B 0.0237(17) 0.040(2) 0.048(2) 0.0311(19) 0.0172(16) 0.0207(16) C34B 0.0159(16) 0.037(2) 0.0281(19) 0.0183(17) 0.0104(14) 0.0084(15) C35B 0.0221(17) 0.038(2) 0.040(2) 0.0262(18) 0.0120(16) 0.0136(16) C36B 0.0191(17) 0.059(3) 0.045(2) 0.034(2) 0.0140(17) 0.0193(18) C37B 0.0159(17) 0.056(3) 0.035(2) 0.029(2) 0.0067(16) 0.0055(17) C38B 0.0304(19) 0.043(2) 0.034(2) 0.0173(18) 0.0104(17) 0.0077(17) C39B 0.0211(17) 0.039(2) 0.044(2) 0.0247(19) 0.0123(16) 0.0106(16) C40B 0.0132(15) 0.0292(19) 0.037(2) 0.0193(17) 0.0102(15) 0.0091(14) C41B 0.034(2) 0.038(2) 0.046(2) 0.024(2) 0.0125(18) 0.0156(17) C42B 0.045(2) 0.038(2) 0.042(2) 0.012(2) 0.0150(19) 0.0156(19) C43B 0.032(2) 0.029(2) 0.055(3) 0.013(2) 0.0105(19) 0.0160(17) C44B 0.0220(18) 0.036(2) 0.054(3) 0.026(2) 0.0099(18) 0.0146(17) C45B 0.0212(17) 0.044(2) 0.043(2) 0.025(2) 0.0150(17) 0.0164(17) C46B 0.0175(16) 0.0236(19) 0.035(2) 0.0124(16) 0.0109(15) 0.0064(14) C47B 0.0195(15) 0.0252(18) 0.036(2) 0.0120(16) 0.0083(15) 0.0077(13) C48B 0.0254(18) 0.036(2) 0.047(2) 0.0172(19) 0.0198(17) 0.0170(16) C49B 0.043(2) 0.051(2) 0.045(2) 0.025(2) 0.0284(19) 0.0247(19) C50B 0.041(2) 0.065(3) 0.037(2) 0.030(2) 0.0198(19) 0.030(2) C51B 0.0276(18) 0.050(2) 0.039(2) 0.0263(19) 0.0175(17) 0.0224(17) _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 C1A 2.009(3) . yes Pd1 C33A 2.042(3) . yes Pd1 O1A 2.1332(18) . yes Pd1 P1A 2.2987(8) . yes P1A C46A 1.826(3) . ? P1A C34A 1.821(3) . ? P1A C40A 1.811(3) . ? O1A C21A 1.322(3) . ? N1A C1A 1.336(3) . ? N1A C4A 1.432(4) . ? N1A C2A 1.478(3) . ? N2A C1A 1.345(3) . ? N2A C16A 1.411(3) . ? N2A C3A 1.473(3) . ? C2A C3A 1.508(4) . ? C4A C9A 1.390(4) . ? C4A C5A 1.417(4) . ? C5A C6A 1.386(4) . ? C5A C10A 1.505(4) . ? C6A C7A 1.366(4) . ? C7A C8A 1.384(4) . ? C8A C9A 1.375(4) . ? C9A C13A 1.526(4) . ? C10A C11A 1.530(4) . ? C10A C12A 1.545(4) . ? C13A C15A 1.527(4) . ? C13A C14A 1.533(4) . ? C16A C17A 1.392(4) . ? C16A C21A 1.419(4) . ? C17A C18A 1.371(4) . ? C18A C19A 1.397(4) . ? C18A C22A 1.508(4) . ? C19A C20A 1.383(4) . ? C20A C21A 1.436(4) . ? C20A C23A 1.534(4) . ? C23A C24A 1.544(4) . ? C23A C25A 1.540(4) . ? C23A C26A 1.536(4) . ? C24A C27A 1.530(4) . ? C25A C29A 1.531(4) . ? C26A C31A 1.532(4) . ? C27A C32A 1.504(4) . ? C27A C28A 1.541(4) . ? C28A C29A 1.514(4) . ? C29A C30A 1.533(4) . ? C30A C31A 1.529(4) . ? C31A C32A 1.524(4) . ? C34A C39A 1.373(4) . ? C34A C35A 1.400(4) . ? C35A C36A 1.384(4) . ? C36A C37A 1.371(4) . ? C37A C38A 1.404(4) . ? C38A C39A 1.374(4) . ? C40A C45A 1.385(4) . ? C40A C41A 1.389(4) . ? C41A C42A 1.380(4) . ? C42A C43A 1.373(4) . ? C43A C44A 1.379(4) . ? C44A C45A 1.384(4) . ? C46A C47A 1.389(4) . ? C46A C51A 1.405(4) . ? C47A C48A 1.377(4) . ? C48A C49A 1.394(4) . ? C49A C50A 1.370(4) . ? C50A C51A 1.372(4) . ? Pd2 C1B 2.018(3) . yes Pd2 C33B 2.031(3) . yes Pd2 O1B 2.1352(18) . yes Pd2 P1B 2.2952(8) . yes P1B C40B 1.811(3) . ? P1B C34B 1.825(3) . ? P1B C46B 1.821(3) . ? O1B C21B 1.311(3) . ? N1B C1B 1.344(4) . ? N1B C4B 1.444(4) . ? N1B C2B 1.483(3) . ? N2B C1B 1.330(3) . ? N2B C16B 1.422(4) . ? N2B C3B 1.472(3) . ? C2B C3B 1.497(4) . ? C4B C5B 1.411(4) . ? C4B C9B 1.381(4) . ? C5B C6B 1.383(4) . ? C5B C10B 1.515(5) . ? C6B C7B 1.378(5) . ? C7B C8B 1.388(4) . ? C8B C9B 1.387(4) . ? C9B C13B 1.520(4) . ? C10B C12B 1.517(4) . ? C10B C11B 1.530(4) . ? C13B C15B 1.518(4) . ? C13B C14B 1.536(4) . ? C16B C17B 1.385(4) . ? C16B C21B 1.417(4) . ? C17B C18B 1.368(4) . ? C18B C19B 1.391(4) . ? C18B C22B 1.511(4) . ? C19B C20B 1.385(4) . ? C20B C21B 1.432(4) . ? C20B C23B 1.535(4) . ? C23B C24B 1.524(4) . ? C23B C26B 1.541(4) . ? C23B C25B 1.544(4) . ? C24B C27B 1.529(4) . ? C25B C29B 1.519(4) . ? C26B C31B 1.526(4) . ? C27B C32B 1.529(4) . ? C27B C28B 1.526(4) . ? C28B C29B 1.512(5) . ? C29B C30B 1.534(4) . ? C30B C31B 1.525(4) . ? C31B C32B 1.514(5) . ? C34B C39B 1.394(4) . ? C34B C35B 1.389(4) . ? C35B C36B 1.386(4) . ? C36B C37B 1.379(5) . ? C37B C38B 1.375(4) . ? C38B C39B 1.387(4) . ? C40B C41B 1.390(4) . ? C40B C45B 1.397(4) . ? C41B C42B 1.385(4) . ? C42B C43B 1.383(5) . ? C43B C44B 1.373(5) . ? C44B C45B 1.378(4) . ? C46B C51B 1.388(4) . ? C46B C47B 1.402(4) . ? C47B C48B 1.377(4) . ? C48B C49B 1.380(4) . ? C49B C50B 1.389(4) . ? C50B C51B 1.381(4) . ? 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 C1A Pd1 C33A 91.65(11) . . yes C1A Pd1 O1A 85.47(9) . . yes C33A Pd1 O1A 173.07(11) . . yes C1A Pd1 P1A 174.92(8) . . yes C33A Pd1 P1A 90.26(9) . . yes O1A Pd1 P1A 93.14(5) . . yes C46A P1A C34A 99.76(13) . . ? C46A P1A C40A 108.53(14) . . ? C34A P1A C40A 103.10(13) . . ? C46A P1A Pd1 113.15(10) . . ? C34A P1A Pd1 117.64(10) . . ? C40A P1A Pd1 113.33(10) . . ? C21A O1A Pd1 115.76(16) . . ? C1A N1A C4A 126.4(2) . . ? C1A N1A C2A 112.0(2) . . ? C4A N1A C2A 120.0(2) . . ? C1A N2A C16A 127.0(2) . . ? C1A N2A C3A 111.5(2) . . ? C16A N2A C3A 121.4(2) . . ? N2A C1A N1A 108.5(2) . . ? N2A C1A Pd1 119.6(2) . . ? N1A C1A Pd1 131.4(2) . . ? N1A C2A C3A 101.7(2) . . ? N2A C3A C2A 102.5(2) . . ? C9A C4A C5A 121.2(3) . . ? C9A C4A N1A 120.7(3) . . ? C5A C4A N1A 118.1(3) . . ? C6A C5A C4A 117.2(3) . . ? C6A C5A C10A 120.4(3) . . ? C4A C5A C10A 122.4(3) . . ? C5A C6A C7A 121.9(3) . . ? C8A C7A C6A 119.9(3) . . ? C7A C8A C9A 121.1(3) . . ? C4A C9A C8A 118.7(3) . . ? C4A C9A C13A 122.9(3) . . ? C8A C9A C13A 118.4(3) . . ? C5A C10A C11A 110.7(3) . . ? C5A C10A C12A 111.9(3) . . ? C11A C10A C12A 108.7(2) . . ? C9A C13A C15A 111.8(3) . . ? C9A C13A C14A 109.6(3) . . ? C15A C13A C14A 110.5(3) . . ? C17A C16A N2A 118.3(3) . . ? C17A C16A C21A 121.7(3) . . ? N2A C16A C21A 119.9(3) . . ? C18A C17A C16A 121.0(3) . . ? C17A C18A C19A 117.7(3) . . ? C17A C18A C22A 121.5(3) . . ? C19A C18A C22A 120.9(3) . . ? C20A C19A C18A 123.9(3) . . ? C19A C20A C21A 118.3(3) . . ? C19A C20A C23A 120.6(3) . . ? C21A C20A C23A 121.1(3) . . ? O1A C21A C20A 121.9(3) . . ? O1A C21A C16A 121.3(3) . . ? C20A C21A C16A 116.8(3) . . ? C20A C23A C24A 112.1(2) . . ? C20A C23A C25A 111.1(2) . . ? C24A C23A C25A 107.3(2) . . ? C20A C23A C26A 111.3(2) . . ? C24A C23A C26A 106.8(2) . . ? C25A C23A C26A 108.1(2) . . ? C27A C24A C23A 111.5(3) . . ? C29A C25A C23A 110.9(2) . . ? C31A C26A C23A 112.0(2) . . ? C24A C27A C32A 111.2(3) . . ? C24A C27A C28A 108.1(2) . . ? C32A C27A C28A 109.7(3) . . ? C29A C28A C27A 108.5(2) . . ? C28A C29A C30A 110.1(2) . . ? C28A C29A C25A 110.9(3) . . ? C30A C29A C25A 108.9(2) . . ? C29A C30A C31A 108.8(3) . . ? C32A C31A C30A 109.3(3) . . ? C32A C31A C26A 108.7(3) . . ? C30A C31A C26A 110.0(2) . . ? C31A C32A C27A 109.5(3) . . ? C39A C34A C35A 118.5(3) . . ? C39A C34A P1A 118.9(2) . . ? C35A C34A P1A 122.5(2) . . ? C36A C35A C34A 120.1(3) . . ? C35A C36A C37A 120.8(3) . . ? C36A C37A C38A 119.2(3) . . ? C37A C38A C39A 119.5(3) . . ? C34A C39A C38A 121.8(3) . . ? C45A C40A C41A 118.3(3) . . ? C45A C40A P1A 124.6(2) . . ? C41A C40A P1A 117.1(2) . . ? C40A C41A C42A 120.9(3) . . ? C43A C42A C41A 120.0(3) . . ? C42A C43A C44A 120.0(3) . . ? C43A C44A C45A 119.8(3) . . ? C40A C45A C44A 120.9(3) . . ? C47A C46A C51A 118.7(3) . . ? C47A C46A P1A 122.3(2) . . ? C51A C46A P1A 118.7(2) . . ? C48A C47A C46A 121.1(3) . . ? C49A C48A C47A 119.7(3) . . ? C50A C49A C48A 119.2(3) . . ? C49A C50A C51A 121.9(3) . . ? C50A C51A C46A 119.3(3) . . ? C1B Pd2 C33B 93.19(12) . . yes C1B Pd2 O1B 85.16(9) . . yes C33B Pd2 O1B 173.34(12) . . yes C1B Pd2 P1B 173.58(9) . . yes C33B Pd2 P1B 89.45(9) . . yes O1B Pd2 P1B 92.87(6) . . yes C40B P1B C34B 102.83(14) . . ? C40B P1B C46B 107.93(14) . . ? C34B P1B C46B 100.33(14) . . ? C40B P1B Pd2 112.70(11) . . ? C34B P1B Pd2 118.59(10) . . ? C46B P1B Pd2 113.14(10) . . ? C21B O1B Pd2 117.01(17) . . ? C1B N1B C4B 127.0(2) . . ? C1B N1B C2B 111.4(2) . . ? C4B N1B C2B 120.4(2) . . ? C1B N2B C16B 126.9(2) . . ? C1B N2B C3B 112.1(2) . . ? C16B N2B C3B 120.7(2) . . ? N2B C1B N1B 107.9(2) . . ? N2B C1B Pd2 120.8(2) . . ? N1B C1B Pd2 130.0(2) . . ? N1B C2B C3B 101.3(2) . . ? N2B C3B C2B 101.9(2) . . ? C5B C4B C9B 123.1(3) . . ? C5B C4B N1B 117.1(3) . . ? C9B C4B N1B 119.8(3) . . ? C4B C5B C6B 116.9(3) . . ? C4B C5B C10B 123.1(3) . . ? C6B C5B C10B 120.1(3) . . ? C7B C6B C5B 121.1(3) . . ? C6B C7B C8B 120.7(3) . . ? C7B C8B C9B 120.3(4) . . ? C4B C9B C8B 117.9(3) . . ? C4B C9B C13B 122.8(3) . . ? C8B C9B C13B 119.3(3) . . ? C5B C10B C12B 111.7(3) . . ? C5B C10B C11B 111.6(3) . . ? C12B C10B C11B 109.7(3) . . ? C9B C13B C15B 111.7(3) . . ? C9B C13B C14B 110.6(3) . . ? C15B C13B C14B 110.6(3) . . ? C17B C16B N2B 117.9(3) . . ? C17B C16B C21B 122.3(3) . . ? N2B C16B C21B 119.5(3) . . ? C18B C17B C16B 121.4(3) . . ? C17B C18B C19B 117.0(3) . . ? C17B C18B C22B 121.1(3) . . ? C19B C18B C22B 121.5(3) . . ? C20B C19B C18B 124.4(3) . . ? C19B C20B C21B 118.5(3) . . ? C19B C20B C23B 120.4(3) . . ? C21B C20B C23B 121.0(3) . . ? O1B C21B C16B 120.9(3) . . ? O1B C21B C20B 122.7(3) . . ? C16B C21B C20B 116.3(3) . . ? C24B C23B C26B 108.1(2) . . ? C24B C23B C20B 110.4(2) . . ? C26B C23B C20B 112.1(2) . . ? C24B C23B C25B 107.1(2) . . ? C26B C23B C25B 106.8(2) . . ? C20B C23B C25B 112.2(2) . . ? C23B C24B C27B 112.3(3) . . ? C29B C25B C23B 111.7(3) . . ? C31B C26B C23B 111.1(2) . . ? C32B C27B C28B 108.1(3) . . ? C32B C27B C24B 109.4(2) . . ? C28B C27B C24B 109.0(3) . . ? C29B C28B C27B 109.9(3) . . ? C25B C29B C28B 109.6(3) . . ? C25B C29B C30B 110.2(3) . . ? C28B C29B C30B 109.5(3) . . ? C29B C30B C31B 107.8(3) . . ? C32B C31B C26B 110.1(3) . . ? C32B C31B C30B 109.2(3) . . ? C26B C31B C30B 110.5(3) . . ? C31B C32B C27B 109.9(3) . . ? C39B C34B C35B 118.2(3) . . ? C39B C34B P1B 118.1(2) . . ? C35B C34B P1B 123.6(3) . . ? C34B C35B C36B 120.3(3) . . ? C35B C36B C37B 121.1(3) . . ? C38B C37B C36B 119.1(3) . . ? C37B C38B C39B 120.3(3) . . ? C34B C39B C38B 121.0(3) . . ? C41B C40B C45B 117.9(3) . . ? C41B C40B P1B 117.0(2) . . ? C45B C40B P1B 125.1(3) . . ? C40B C41B C42B 121.1(3) . . ? C43B C42B C41B 119.9(4) . . ? C44B C43B C42B 119.7(3) . . ? C43B C44B C45B 120.6(3) . . ? C44B C45B C40B 120.8(3) . . ? C51B C46B C47B 118.7(3) . . ? C51B C46B P1B 122.2(2) . . ? C47B C46B P1B 119.0(2) . . ? C48B C47B C46B 119.8(3) . . ? C49B C48B C47B 121.1(3) . . ? C48B C49B C50B 119.5(3) . . ? C51B C50B C49B 119.7(3) . . ? C50B C51B C46B 121.2(3) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 28.52 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 1.151 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.084