# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1359 data_STRUCT1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H34 N2 O4 P2 Pd' _chemical_formula_weight 751.01 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' 'O' 'O' 0.0106 0.0060 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4901(19) _cell_length_b 10.4479(16) _cell_length_c 18.6230(13) _cell_angle_alpha 74.544(9) _cell_angle_beta 79.718(6) _cell_angle_gamma 80.364(9) _cell_volume 1737.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.669 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7266 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.1098 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.07 _reflns_number_total 4747 _reflns_number_gt 3509 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4747 _refine_ls_number_parameters 426 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 0.852 _refine_ls_restrained_S_all 0.852 _refine_ls_shift/su_max 0.014 _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 0.25385(4) 0.02192(3) 0.25925(2) 0.03495(12) Uani 1 1 d . . . P2 P 0.42319(13) -0.16555(11) 0.29045(6) 0.0333(3) Uani 1 1 d . . . P1 P 0.09709(13) 0.22042(11) 0.23239(6) 0.0362(3) Uani 1 1 d . . . N1 N -0.1390(6) 0.1505(6) 0.1931(3) 0.1041(19) Uani 1 1 d . . . N2 N 0.6057(6) -0.3403(5) 0.2166(3) 0.0904(17) Uani 1 1 d . . . O1 O 0.3041(4) 0.1248(4) 0.3787(2) 0.0678(11) Uani 1 1 d . . . O2 O 0.4616(4) 0.1640(3) 0.27426(19) 0.0581(10) Uani 1 1 d . . . O3 O 0.1509(4) -0.0782(3) 0.20407(18) 0.0513(9) Uani 1 1 d . . . O4 O 0.2363(5) 0.0546(5) 0.0973(2) 0.0893(15) Uani 1 1 d . . . C1 C 0.3431(5) 0.1126(4) 0.3163(3) 0.0414(12) Uani 1 1 d . . . C2 C 0.5319(7) 0.2432(6) 0.3064(4) 0.095(2) Uani 1 1 d . . . H2A H 0.6044 0.2856 0.2690 0.143 Uiso 1 1 calc R . . H2B H 0.5762 0.1864 0.3482 0.143 Uiso 1 1 calc R . . H2C H 0.4618 0.3104 0.3234 0.143 Uiso 1 1 calc R . . C3 C 0.1636(7) -0.0333(6) 0.1323(4) 0.0637(18) Uani 1 1 d . . . C4 C 0.0746(9) -0.0924(7) 0.0930(4) 0.133(3) Uani 1 1 d . . . H4A H -0.0158 -0.1089 0.1241 0.200 Uiso 1 1 calc R . . H4B H 0.1258 -0.1750 0.0836 0.200 Uiso 1 1 calc R . . H4C H 0.0571 -0.0308 0.0460 0.200 Uiso 1 1 calc R . . C5 C -0.0214(5) 0.2587(5) 0.3145(3) 0.0402(12) Uani 1 1 d . . . C6 C -0.0250(6) 0.1664(5) 0.3821(3) 0.0598(15) Uani 1 1 d . . . H6 H 0.0375 0.0869 0.3866 0.072 Uiso 1 1 calc R . . C7 C -0.1206(7) 0.1900(7) 0.4440(3) 0.0807(19) Uani 1 1 d . . . H7 H -0.1260 0.1254 0.4894 0.097 Uiso 1 1 calc R . . C8 C -0.2063(7) 0.3091(8) 0.4371(4) 0.086(2) Uani 1 1 d . . . H8 H -0.2689 0.3273 0.4787 0.103 Uiso 1 1 calc R . . C9 C -0.2015(6) 0.4025(7) 0.3699(4) 0.0810(19) Uani 1 1 d . . . H9 H -0.2595 0.4846 0.3657 0.097 Uiso 1 1 calc R . . C10 C -0.1119(5) 0.3746(5) 0.3097(3) 0.0553(14) Uani 1 1 d . . . H10 H -0.1122 0.4369 0.2635 0.066 Uiso 1 1 calc R . . C11 C 0.1991(5) 0.3595(5) 0.1886(3) 0.0441(12) Uani 1 1 d . . . C12 C 0.3066(7) 0.3455(6) 0.1317(4) 0.085(2) Uani 1 1 d . . . H12 H 0.3250 0.2655 0.1168 0.102 Uiso 1 1 calc R . . C13 C 0.3885(8) 0.4450(8) 0.0959(4) 0.113(3) Uani 1 1 d . . . H13 H 0.4610 0.4337 0.0564 0.135 Uiso 1 1 calc R . . C14 C 0.3632(9) 0.5611(8) 0.1184(5) 0.101(3) Uani 1 1 d . . . H14 H 0.4192 0.6297 0.0947 0.121 Uiso 1 1 calc R . . C15 C 0.2584(11) 0.5766(7) 0.1743(5) 0.124(3) Uani 1 1 d . . . H15 H 0.2411 0.6564 0.1895 0.149 Uiso 1 1 calc R . . C16 C 0.1754(7) 0.4760(6) 0.2099(3) 0.081(2) Uani 1 1 d . . . H16 H 0.1024 0.4881 0.2490 0.097 Uiso 1 1 calc R . . C17 C -0.0326(5) 0.2356(5) 0.1684(3) 0.0427(12) Uani 1 1 d . . . C18 C -0.2405(7) 0.1610(7) 0.1435(4) 0.092(2) Uani 1 1 d . . . H18 H -0.3145 0.1071 0.1585 0.111 Uiso 1 1 calc R . . C19 C -0.2319(7) 0.2478(7) 0.0746(4) 0.081(2) Uani 1 1 d . . . H19 H -0.2982 0.2526 0.0425 0.097 Uiso 1 1 calc R . . C20 C -0.1251(8) 0.3275(6) 0.0535(3) 0.082(2) Uani 1 1 d . . . H20 H -0.1192 0.3873 0.0064 0.098 Uiso 1 1 calc R . . C21 C -0.0270(6) 0.3223(5) 0.0990(3) 0.0632(16) Uani 1 1 d . . . H21 H 0.0449 0.3784 0.0829 0.076 Uiso 1 1 calc R . . C22 C 0.5281(5) -0.2140(5) 0.2074(3) 0.0426(12) Uani 1 1 d . . . C23 C 0.6959(7) -0.3682(7) 0.1536(4) 0.092(2) Uani 1 1 d . . . H23 H 0.7487 -0.4527 0.1579 0.110 Uiso 1 1 calc R . . C24 C 0.7101(7) -0.2783(8) 0.0866(4) 0.094(2) Uani 1 1 d . . . H24 H 0.7736 -0.2998 0.0461 0.113 Uiso 1 1 calc R . . C25 C 0.6299(7) -0.1553(7) 0.0790(3) 0.0819(19) Uani 1 1 d . . . H25 H 0.6382 -0.0928 0.0328 0.098 Uiso 1 1 calc R . . C26 C 0.5368(6) -0.1232(5) 0.1392(3) 0.0541(14) Uani 1 1 d . . . H26 H 0.4803 -0.0403 0.1335 0.065 Uiso 1 1 calc R . . C27 C 0.3407(5) -0.3115(4) 0.3472(2) 0.0380(11) Uani 1 1 d . . . C28 C 0.4191(5) -0.4159(5) 0.3897(3) 0.0494(13) Uani 1 1 d . . . H28 H 0.5161 -0.4125 0.3906 0.059 Uiso 1 1 calc R . . C29 C 0.3565(8) -0.5240(6) 0.4303(4) 0.0770(18) Uani 1 1 d . . . H29 H 0.4115 -0.5948 0.4590 0.092 Uiso 1 1 calc R . . C30 C 0.2136(8) -0.5326(6) 0.4305(3) 0.0780(19) Uani 1 1 d . . . H30 H 0.1732 -0.6098 0.4572 0.094 Uiso 1 1 calc R . . C31 C 0.1324(7) -0.4265(6) 0.3911(3) 0.0793(19) Uani 1 1 d . . . H31 H 0.0345 -0.4291 0.3924 0.095 Uiso 1 1 calc R . . C32 C 0.1946(6) -0.3153(5) 0.3494(3) 0.0579(14) Uani 1 1 d . . . H32 H 0.1387 -0.2426 0.3225 0.069 Uiso 1 1 calc R . . C33 C 0.5622(5) -0.1553(4) 0.3432(3) 0.0392(12) Uani 1 1 d . . . C34 C 0.7062(6) -0.1533(5) 0.3129(3) 0.0621(15) Uani 1 1 d . . . H34 H 0.7361 -0.1616 0.2638 0.075 Uiso 1 1 calc R . . C35 C 0.8057(7) -0.1391(6) 0.3550(5) 0.090(2) Uani 1 1 d . . . H35 H 0.9018 -0.1358 0.3337 0.108 Uiso 1 1 calc R . . C36 C 0.7645(9) -0.1300(6) 0.4273(5) 0.089(2) Uani 1 1 d . . . H36 H 0.8327 -0.1223 0.4556 0.107 Uiso 1 1 calc R . . C37 C 0.6227(8) -0.1319(5) 0.4586(3) 0.0707(18) Uani 1 1 d . . . H37 H 0.5952 -0.1250 0.5080 0.085 Uiso 1 1 calc R . . C38 C 0.5206(6) -0.1441(4) 0.4178(3) 0.0485(13) Uani 1 1 d . . . H38 H 0.4245 -0.1450 0.4395 0.058 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 0.0384(2) 0.0393(2) 0.0268(2) -0.00778(15) -0.00633(16) -0.00250(15) P2 0.0333(7) 0.0372(7) 0.0263(7) -0.0056(5) -0.0010(6) -0.0027(6) P1 0.0354(8) 0.0404(7) 0.0293(7) -0.0067(6) -0.0023(6) -0.0009(6) N1 0.079(4) 0.146(5) 0.094(4) -0.023(4) -0.019(4) -0.035(4) N2 0.081(4) 0.100(4) 0.085(4) -0.039(3) -0.002(3) 0.019(3) O1 0.063(3) 0.105(3) 0.050(2) -0.044(2) -0.009(2) -0.009(2) O2 0.061(3) 0.060(2) 0.060(2) -0.0180(19) -0.008(2) -0.022(2) O3 0.072(3) 0.045(2) 0.041(2) -0.0111(16) -0.0147(19) -0.0093(18) O4 0.105(4) 0.106(4) 0.036(2) -0.009(2) 0.000(2) 0.024(3) C1 0.040(3) 0.043(3) 0.040(3) -0.007(2) -0.015(3) 0.003(2) C2 0.083(5) 0.099(5) 0.132(6) -0.055(5) -0.025(5) -0.038(4) C3 0.077(5) 0.071(4) 0.046(4) -0.027(3) -0.029(4) 0.027(3) C4 0.161(8) 0.170(7) 0.109(6) -0.089(6) -0.086(6) 0.030(6) C5 0.034(3) 0.056(3) 0.032(3) -0.015(2) 0.002(2) -0.008(2) C6 0.054(4) 0.073(4) 0.049(4) -0.019(3) 0.005(3) -0.003(3) C7 0.075(5) 0.119(6) 0.040(4) -0.019(4) 0.010(3) -0.011(4) C8 0.070(5) 0.125(6) 0.072(5) -0.060(5) 0.023(4) -0.015(5) C9 0.054(4) 0.090(5) 0.099(6) -0.045(5) 0.008(4) 0.007(4) C10 0.044(4) 0.060(3) 0.054(4) -0.011(3) -0.003(3) 0.009(3) C11 0.040(3) 0.046(3) 0.039(3) 0.001(2) -0.007(3) -0.003(2) C12 0.080(5) 0.049(4) 0.094(5) 0.012(4) 0.027(4) -0.010(4) C13 0.086(6) 0.094(6) 0.108(6) 0.027(5) 0.037(5) -0.010(5) C14 0.101(7) 0.109(7) 0.090(6) 0.018(5) -0.026(5) -0.062(6) C15 0.210(11) 0.092(6) 0.091(6) -0.024(5) -0.018(7) -0.079(7) C16 0.125(6) 0.063(4) 0.055(4) -0.019(3) 0.025(4) -0.049(4) C17 0.042(3) 0.047(3) 0.037(3) -0.009(2) -0.005(2) -0.004(2) C18 0.067(5) 0.147(6) 0.074(5) -0.019(5) -0.028(4) -0.038(4) C19 0.068(5) 0.116(6) 0.064(5) -0.035(4) -0.033(4) 0.018(4) C20 0.098(6) 0.095(5) 0.049(4) -0.001(3) -0.040(4) 0.002(4) C21 0.082(4) 0.060(4) 0.047(4) 0.002(3) -0.021(3) -0.019(3) C22 0.040(3) 0.061(3) 0.029(3) -0.020(2) 0.000(2) -0.002(3) C23 0.073(5) 0.114(6) 0.087(6) -0.052(5) -0.001(4) 0.027(4) C24 0.068(5) 0.154(8) 0.063(5) -0.055(5) 0.029(4) -0.016(5) C25 0.075(5) 0.132(6) 0.038(4) -0.022(4) 0.012(3) -0.032(5) C26 0.051(4) 0.076(4) 0.033(3) -0.012(3) 0.002(3) -0.013(3) C27 0.041(3) 0.042(3) 0.029(3) -0.010(2) 0.004(2) -0.007(2) C28 0.041(3) 0.036(3) 0.063(4) -0.002(3) -0.006(3) 0.002(3) C29 0.083(5) 0.052(4) 0.085(5) -0.012(3) -0.006(4) 0.008(4) C30 0.110(6) 0.050(4) 0.068(4) 0.003(3) 0.000(4) -0.033(4) C31 0.071(5) 0.088(5) 0.077(5) 0.006(4) -0.013(4) -0.045(4) C32 0.050(4) 0.065(4) 0.052(4) 0.003(3) -0.011(3) -0.012(3) C33 0.042(3) 0.032(3) 0.037(3) 0.004(2) -0.009(2) -0.003(2) C34 0.052(4) 0.071(4) 0.061(4) -0.003(3) -0.014(3) -0.013(3) C35 0.048(4) 0.097(5) 0.118(6) 0.003(5) -0.035(5) -0.014(4) C36 0.103(6) 0.067(4) 0.106(6) 0.009(4) -0.072(6) -0.024(4) C37 0.115(6) 0.060(4) 0.044(4) 0.001(3) -0.041(4) -0.020(4) C38 0.063(4) 0.046(3) 0.034(3) 0.000(2) -0.009(3) -0.010(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 1.967(5) . ? Pd1 O3 2.092(3) . ? Pd1 P2 2.3302(12) . ? Pd1 P1 2.3333(13) . ? P2 C33 1.812(5) . ? P2 C27 1.817(5) . ? P2 C22 1.827(4) . ? P1 C11 1.809(5) . ? P1 C17 1.821(5) . ? P1 C5 1.822(4) . ? N1 C17 1.392(7) . ? N1 C18 1.422(7) . ? N2 C22 1.382(6) . ? N2 C23 1.392(7) . ? O1 C1 1.189(5) . ? O2 C1 1.353(6) . ? O2 C2 1.442(5) . ? O3 C3 1.283(6) . ? O4 C3 1.215(7) . ? C3 C4 1.507(8) . ? C5 C10 1.355(6) . ? C5 C6 1.366(6) . ? C6 C7 1.384(7) . ? C7 C8 1.356(8) . ? C8 C9 1.366(8) . ? C9 C10 1.347(7) . ? C11 C16 1.350(6) . ? C11 C12 1.353(7) . ? C12 C13 1.359(8) . ? C13 C14 1.357(9) . ? C14 C15 1.329(9) . ? C15 C16 1.373(9) . ? C17 C21 1.364(6) . ? C18 C19 1.356(8) . ? C19 C20 1.357(8) . ? C20 C21 1.353(7) . ? C22 C26 1.366(6) . ? C23 C24 1.347(9) . ? C24 C25 1.366(8) . ? C25 C26 1.378(7) . ? C27 C28 1.359(6) . ? C27 C32 1.387(6) . ? C28 C29 1.346(7) . ? C29 C30 1.373(8) . ? C30 C31 1.358(8) . ? C31 C32 1.374(7) . ? C33 C34 1.384(7) . ? C33 C38 1.405(6) . ? C34 C35 1.379(7) . ? C35 C36 1.356(9) . ? C36 C37 1.368(9) . ? C37 C38 1.374(7) . ? 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 O3 176.78(19) . . ? C1 Pd1 P2 88.94(13) . . ? O3 Pd1 P2 91.18(9) . . ? C1 Pd1 P1 85.82(13) . . ? O3 Pd1 P1 94.11(9) . . ? P2 Pd1 P1 174.66(4) . . ? C33 P2 C27 103.4(2) . . ? C33 P2 C22 102.6(2) . . ? C27 P2 C22 106.5(2) . . ? C33 P2 Pd1 118.28(14) . . ? C27 P2 Pd1 112.55(15) . . ? C22 P2 Pd1 112.35(16) . . ? C11 P1 C17 103.8(2) . . ? C11 P1 C5 108.2(2) . . ? C17 P1 C5 101.2(2) . . ? C11 P1 Pd1 109.97(15) . . ? C17 P1 Pd1 118.62(15) . . ? C5 P1 Pd1 114.05(16) . . ? C17 N1 C18 116.9(6) . . ? C22 N2 C23 116.5(5) . . ? C1 O2 C2 116.9(4) . . ? C3 O3 Pd1 114.7(4) . . ? O1 C1 O2 121.6(4) . . ? O1 C1 Pd1 127.9(4) . . ? O2 C1 Pd1 110.5(3) . . ? O4 C3 O3 124.0(6) . . ? O4 C3 C4 120.8(6) . . ? O3 C3 C4 115.2(7) . . ? C10 C5 C6 118.4(5) . . ? C10 C5 P1 121.7(4) . . ? C6 C5 P1 119.8(4) . . ? C5 C6 C7 120.8(5) . . ? C8 C7 C6 118.7(6) . . ? C7 C8 C9 120.7(6) . . ? C10 C9 C8 119.3(6) . . ? C9 C10 C5 122.0(6) . . ? C16 C11 C12 118.0(5) . . ? C16 C11 P1 123.8(4) . . ? C12 C11 P1 118.1(4) . . ? C11 C12 C13 121.8(6) . . ? C12 C13 C14 119.2(7) . . ? C15 C14 C13 119.9(8) . . ? C14 C15 C16 120.6(7) . . ? C11 C16 C15 120.4(6) . . ? C21 C17 N1 120.4(5) . . ? C21 C17 P1 123.2(4) . . ? N1 C17 P1 116.4(4) . . ? C19 C18 N1 121.4(6) . . ? C18 C19 C20 119.0(6) . . ? C21 C20 C19 121.8(6) . . ? C20 C21 C17 120.5(6) . . ? C26 C22 N2 121.4(5) . . ? C26 C22 P2 120.0(4) . . ? N2 C22 P2 118.4(4) . . ? C24 C23 N2 122.9(6) . . ? C23 C24 C25 119.1(6) . . ? C24 C25 C26 120.4(6) . . ? C22 C26 C25 119.6(5) . . ? C28 C27 C32 119.2(5) . . ? C28 C27 P2 121.0(4) . . ? C32 C27 P2 119.8(4) . . ? C29 C28 C27 120.0(5) . . ? C28 C29 C30 121.8(6) . . ? C31 C30 C29 118.8(6) . . ? C30 C31 C32 120.1(6) . . ? C31 C32 C27 120.0(5) . . ? C34 C33 C38 118.4(5) . . ? C34 C33 P2 123.3(4) . . ? C38 C33 P2 118.2(4) . . ? C35 C34 C33 120.4(6) . . ? C36 C35 C34 120.5(7) . . ? C35 C36 C37 120.2(6) . . ? C36 C37 C38 120.7(6) . . ? C37 C38 C33 119.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Pd1 P2 C33 -3.5(2) . . . . ? O3 Pd1 P2 C33 179.7(2) . . . . ? P1 Pd1 P2 C33 7.2(6) . . . . ? C1 Pd1 P2 C27 117.1(2) . . . . ? O3 Pd1 P2 C27 -59.67(18) . . . . ? P1 Pd1 P2 C27 127.8(5) . . . . ? C1 Pd1 P2 C22 -122.7(2) . . . . ? O3 Pd1 P2 C22 60.50(19) . . . . ? P1 Pd1 P2 C22 -112.0(6) . . . . ? C1 Pd1 P1 C11 56.0(2) . . . . ? O3 Pd1 P1 C11 -127.24(19) . . . . ? P2 Pd1 P1 C11 45.2(6) . . . . ? C1 Pd1 P1 C17 175.1(2) . . . . ? O3 Pd1 P1 C17 -8.1(2) . . . . ? P2 Pd1 P1 C17 164.4(5) . . . . ? C1 Pd1 P1 C5 -65.8(2) . . . . ? O3 Pd1 P1 C5 110.98(19) . . . . ? P2 Pd1 P1 C5 -76.5(6) . . . . ? C1 Pd1 O3 C3 157(3) . . . . ? P2 Pd1 O3 C3 -111.4(3) . . . . ? P1 Pd1 O3 C3 67.9(3) . . . . ? C2 O2 C1 O1 -4.8(7) . . . . ? C2 O2 C1 Pd1 175.0(3) . . . . ? O3 Pd1 C1 O1 -7(3) . . . . ? P2 Pd1 C1 O1 -98.9(4) . . . . ? P1 Pd1 C1 O1 82.1(4) . . . . ? O3 Pd1 C1 O2 174(3) . . . . ? P2 Pd1 C1 O2 81.4(3) . . . . ? P1 Pd1 C1 O2 -97.6(3) . . . . ? Pd1 O3 C3 O4 4.4(7) . . . . ? Pd1 O3 C3 C4 -172.5(4) . . . . ? C11 P1 C5 C10 52.6(4) . . . . ? C17 P1 C5 C10 -56.1(4) . . . . ? Pd1 P1 C5 C10 175.3(3) . . . . ? C11 P1 C5 C6 -130.5(4) . . . . ? C17 P1 C5 C6 120.8(4) . . . . ? Pd1 P1 C5 C6 -7.8(5) . . . . ? C10 C5 C6 C7 1.1(8) . . . . ? P1 C5 C6 C7 -175.9(4) . . . . ? C5 C6 C7 C8 -3.0(9) . . . . ? C6 C7 C8 C9 1.9(10) . . . . ? C7 C8 C9 C10 0.9(10) . . . . ? C8 C9 C10 C5 -2.9(9) . . . . ? C6 C5 C10 C9 1.9(8) . . . . ? P1 C5 C10 C9 178.9(4) . . . . ? C17 P1 C11 C16 100.0(5) . . . . ? C5 P1 C11 C16 -7.0(5) . . . . ? Pd1 P1 C11 C16 -132.2(5) . . . . ? C17 P1 C11 C12 -80.9(5) . . . . ? C5 P1 C11 C12 172.1(4) . . . . ? Pd1 P1 C11 C12 47.0(5) . . . . ? C16 C11 C12 C13 -0.7(9) . . . . ? P1 C11 C12 C13 -179.9(5) . . . . ? C11 C12 C13 C14 1.0(11) . . . . ? C12 C13 C14 C15 -0.7(13) . . . . ? C13 C14 C15 C16 0.2(13) . . . . ? C12 C11 C16 C15 0.3(10) . . . . ? P1 C11 C16 C15 179.4(6) . . . . ? C14 C15 C16 C11 0.0(12) . . . . ? C18 N1 C17 C21 -1.2(8) . . . . ? C18 N1 C17 P1 -179.7(4) . . . . ? C11 P1 C17 C21 9.5(5) . . . . ? C5 P1 C17 C21 121.6(4) . . . . ? Pd1 P1 C17 C21 -112.8(4) . . . . ? C11 P1 C17 N1 -172.0(4) . . . . ? C5 P1 C17 N1 -59.9(4) . . . . ? Pd1 P1 C17 N1 65.7(4) . . . . ? C17 N1 C18 C19 1.5(10) . . . . ? N1 C18 C19 C20 -1.0(10) . . . . ? C18 C19 C20 C21 0.2(10) . . . . ? C19 C20 C21 C17 0.1(9) . . . . ? N1 C17 C21 C20 0.4(8) . . . . ? P1 C17 C21 C20 178.9(4) . . . . ? C23 N2 C22 C26 1.9(8) . . . . ? C23 N2 C22 P2 -173.5(4) . . . . ? C33 P2 C22 C26 -107.5(4) . . . . ? C27 P2 C22 C26 144.2(4) . . . . ? Pd1 P2 C22 C26 20.5(5) . . . . ? C33 P2 C22 N2 67.9(4) . . . . ? C27 P2 C22 N2 -40.4(4) . . . . ? Pd1 P2 C22 N2 -164.0(4) . . . . ? C22 N2 C23 C24 0.7(10) . . . . ? N2 C23 C24 C25 -1.9(11) . . . . ? C23 C24 C25 C26 0.6(10) . . . . ? N2 C22 C26 C25 -3.2(8) . . . . ? P2 C22 C26 C25 172.2(4) . . . . ? C24 C25 C26 C22 1.9(9) . . . . ? C33 P2 C27 C28 -30.9(4) . . . . ? C22 P2 C27 C28 76.8(4) . . . . ? Pd1 P2 C27 C28 -159.7(3) . . . . ? C33 P2 C27 C32 147.1(4) . . . . ? C22 P2 C27 C32 -105.2(4) . . . . ? Pd1 P2 C27 C32 18.3(4) . . . . ? C32 C27 C28 C29 3.1(7) . . . . ? P2 C27 C28 C29 -178.9(4) . . . . ? C27 C28 C29 C30 -0.1(9) . . . . ? C28 C29 C30 C31 -2.9(9) . . . . ? C29 C30 C31 C32 2.8(9) . . . . ? C30 C31 C32 C27 0.2(9) . . . . ? C28 C27 C32 C31 -3.2(7) . . . . ? P2 C27 C32 C31 178.8(4) . . . . ? C27 P2 C33 C34 124.5(4) . . . . ? C22 P2 C33 C34 13.9(5) . . . . ? Pd1 P2 C33 C34 -110.3(4) . . . . ? C27 P2 C33 C38 -57.8(4) . . . . ? C22 P2 C33 C38 -168.4(3) . . . . ? Pd1 P2 C33 C38 67.4(4) . . . . ? C38 C33 C34 C35 -0.7(7) . . . . ? P2 C33 C34 C35 177.0(4) . . . . ? C33 C34 C35 C36 1.5(9) . . . . ? C34 C35 C36 C37 -1.4(10) . . . . ? C35 C36 C37 C38 0.5(9) . . . . ? C36 C37 C38 C33 0.3(8) . . . . ? C34 C33 C38 C37 -0.2(7) . . . . ? P2 C33 C38 C37 -178.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.768 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.768 _refine_diff_density_max 0.552 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.070 data_struct5 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H30 Cl N2 O2 P2 Pd' _chemical_formula_weight 726.41 _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' 'O' 'O' 0.0106 0.0060 '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.084(9) _cell_length_b 15.609(8) _cell_length_c 24.354(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.630(10) _cell_angle_gamma 90.00 _cell_volume 6434(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 0.795 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12339 _diffrn_reflns_av_R_equivalents 0.0547 _diffrn_reflns_av_sigmaI/netI 0.1041 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4659 _reflns_number_gt 3200 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4659 _refine_ls_number_parameters 398 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0947 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.862 _refine_ls_shift/su_max 0.000 _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 0.026576(19) 0.74397(2) 0.008627(13) 0.02387(12) Uani 1 1 d . . . Cl1 Cl -0.07480(7) 0.85124(8) -0.02506(5) 0.0352(3) Uani 1 1 d . . . P1 P 0.04333(7) 0.74685(8) -0.08176(5) 0.0260(3) Uani 1 1 d . . . P2 P 0.02261(6) 0.74316(8) 0.10316(4) 0.0214(3) Uani 1 1 d . . . N1 N 0.0998(4) 0.8600(3) -0.1416(2) 0.0730(17) Uani 1 1 d . . . N2 N -0.1361(3) 0.6987(3) 0.05703(18) 0.0537(13) Uani 1 1 d . . . O1 O 0.1757(2) 0.6589(2) 0.05238(13) 0.0377(8) Uani 1 1 d . . . O2 O 0.0695(2) 0.5759(2) 0.02105(13) 0.0388(9) Uani 1 1 d . . . C1 C 0.0824(3) 0.8514(3) -0.09295(19) 0.0318(12) Uani 1 1 d . . . C2 C 0.1328(5) 0.9355(5) -0.1472(3) 0.096(3) Uani 1 1 d . . . H2 H 0.1459 0.9430 -0.1806 0.116 Uiso 1 1 calc R . . C3 C 0.1486(4) 1.0012(4) -0.1087(3) 0.0548(17) Uani 1 1 d . . . H3 H 0.1706 1.0521 -0.1156 0.066 Uiso 1 1 calc R . . C4 C 0.1310(3) 0.9898(4) -0.0597(2) 0.0438(14) Uani 1 1 d U . . H4 H 0.1417 1.0326 -0.0314 0.053 Uiso 1 1 calc R . . C5 C 0.0971(3) 0.9141(3) -0.0524(2) 0.0379(13) Uani 1 1 d . . . H5 H 0.0840 0.9059 -0.0191 0.045 Uiso 1 1 calc R . . C6 C 0.1137(3) 0.6729(3) -0.09443(17) 0.0261(11) Uani 1 1 d . . . C7 C 0.0904(3) 0.5919(3) -0.11552(19) 0.0377(13) Uani 1 1 d . . . H7 H 0.0377 0.5760 -0.1257 0.045 Uiso 1 1 calc R . . C8 C 0.1451(3) 0.5335(3) -0.1217(2) 0.0422(14) Uani 1 1 d . . . H8 H 0.1292 0.4785 -0.1355 0.051 Uiso 1 1 calc R . . C9 C 0.2223(3) 0.5573(3) -0.1075(2) 0.0404(13) Uani 1 1 d . . . H9 H 0.2589 0.5188 -0.1122 0.048 Uiso 1 1 calc R . . C10 C 0.2459(3) 0.6385(3) -0.0862(2) 0.0382(12) Uani 1 1 d . . . H10 H 0.2986 0.6542 -0.0763 0.046 Uiso 1 1 calc R . . C11 C 0.1923(3) 0.6965(3) -0.07942(19) 0.0317(11) Uani 1 1 d . . . H11 H 0.2087 0.7511 -0.0649 0.038 Uiso 1 1 calc R . . C12 C -0.0469(3) 0.7257(3) -0.14261(18) 0.0324(12) Uani 1 1 d . . . C13 C -0.1093(3) 0.6868(3) -0.1327(2) 0.0387(13) Uani 1 1 d . . . H13 H -0.1062 0.6767 -0.0943 0.046 Uiso 1 1 calc R . . C14 C -0.1764(3) 0.6624(3) -0.1785(2) 0.0420(13) Uani 1 1 d . . . H14 H -0.2178 0.6360 -0.1708 0.050 Uiso 1 1 calc R . . C15 C -0.1819(3) 0.6770(4) -0.2347(2) 0.0501(15) Uani 1 1 d . . . H15 H -0.2264 0.6594 -0.2656 0.060 Uiso 1 1 calc R . . C16 C -0.1218(4) 0.7175(5) -0.2454(2) 0.071(2) Uani 1 1 d . . . H16 H -0.1266 0.7296 -0.2839 0.086 Uiso 1 1 calc R . . C17 C -0.0535(3) 0.7410(4) -0.19972(19) 0.0580(18) Uani 1 1 d . . . H17 H -0.0122 0.7670 -0.2078 0.070 Uiso 1 1 calc R . . C18 C -0.0744(3) 0.7265(3) 0.10720(17) 0.0231(10) Uani 1 1 d . . . C19 C -0.0863(3) 0.7367(3) 0.15922(18) 0.0319(12) Uani 1 1 d . . . H19 H -0.0448 0.7542 0.1925 0.038 Uiso 1 1 calc R . . C20 C -0.1589(3) 0.7214(4) 0.1625(2) 0.0463(14) Uani 1 1 d . . . H20 H -0.1663 0.7296 0.1980 0.056 Uiso 1 1 calc R . . C21 C -0.2210(3) 0.6942(3) 0.1149(2) 0.0378(13) Uani 1 1 d . . . H21 H -0.2698 0.6833 0.1182 0.045 Uiso 1 1 calc R . . C22 C -0.2107(3) 0.6831(3) 0.0614(2) 0.0340(12) Uani 1 1 d . . . H22 H -0.2528 0.6654 0.0287 0.041 Uiso 1 1 calc R . . C23 C 0.0847(3) 0.6665(3) 0.15620(17) 0.0256(11) Uani 1 1 d . . . C24 C 0.0539(3) 0.5968(3) 0.1749(2) 0.0386(13) Uani 1 1 d . . . H24 H -0.0005 0.5883 0.1608 0.046 Uiso 1 1 calc R . . C25 C 0.1024(3) 0.5390(3) 0.2145(2) 0.0518(16) Uani 1 1 d . . . H25 H 0.0811 0.4910 0.2261 0.062 Uiso 1 1 calc R . . C26 C 0.1824(3) 0.5536(4) 0.2362(2) 0.0499(15) Uani 1 1 d . . . H26 H 0.2153 0.5159 0.2636 0.060 Uiso 1 1 calc R . . C27 C 0.2140(3) 0.6225(3) 0.2182(2) 0.0434(14) Uani 1 1 d . . . H27 H 0.2683 0.6317 0.2331 0.052 Uiso 1 1 calc R . . C28 C 0.1652(3) 0.6784(3) 0.1777(2) 0.0381(13) Uani 1 1 d . . . H28 H 0.1869 0.7249 0.1649 0.046 Uiso 1 1 calc R . . C29 C 0.0554(3) 0.8455(3) 0.14129(18) 0.0266(11) Uani 1 1 d . . . C30 C 0.0714(3) 0.8475(3) 0.19937(17) 0.0392(14) Uani 1 1 d . . . H30 H 0.0684 0.7982 0.2200 0.047 Uiso 1 1 calc R . . C31 C 0.0917(4) 0.9227(4) 0.2266(2) 0.070(2) Uani 1 1 d . . . H31 H 0.1022 0.9249 0.2668 0.084 Uiso 1 1 calc R . . C32 C 0.0980(3) 0.9961(3) 0.1988(2) 0.0515(16) Uani 1 1 d . . . H32 H 0.1127 1.0470 0.2197 0.062 Uiso 1 1 calc R . . C33 C 0.0825(3) 0.9943(3) 0.1402(2) 0.0391(14) Uani 1 1 d . . . H33 H 0.0866 1.0437 0.1202 0.047 Uiso 1 1 calc R . . C34 C 0.0606(3) 0.9177(3) 0.11100(19) 0.0314(12) Uani 1 1 d . . . H34 H 0.0494 0.9151 0.0707 0.038 Uiso 1 1 calc R . . C35 C 0.1060(3) 0.6518(3) 0.03199(17) 0.0249(10) Uani 1 1 d . . . C36 C 0.1215(4) 0.5015(3) 0.0355(2) 0.0595(17) Uani 1 1 d . . . H36A H 0.0910 0.4505 0.0216 0.089 Uiso 1 1 calc R . . H36B H 0.1475 0.4981 0.0773 0.089 Uiso 1 1 calc R . . H36C H 0.1604 0.5069 0.0172 0.089 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 0.0219(2) 0.0306(2) 0.0212(2) 0.00575(16) 0.01023(13) 0.00354(18) Cl1 0.0327(7) 0.0424(8) 0.0335(7) 0.0100(5) 0.0152(5) 0.0106(6) P1 0.0283(7) 0.0300(7) 0.0243(6) 0.0073(5) 0.0150(5) 0.0083(6) P2 0.0187(6) 0.0260(7) 0.0190(6) 0.0033(5) 0.0059(4) -0.0006(5) N1 0.141(5) 0.040(3) 0.069(3) 0.005(3) 0.076(4) -0.004(3) N2 0.047(3) 0.051(3) 0.057(3) 0.008(2) 0.012(2) 0.001(2) O1 0.028(2) 0.037(2) 0.045(2) 0.0032(15) 0.0095(16) 0.0020(16) O2 0.040(2) 0.024(2) 0.047(2) 0.0049(15) 0.0086(16) -0.0023(16) C1 0.037(3) 0.037(3) 0.029(3) 0.010(2) 0.022(2) 0.011(2) C2 0.202(9) 0.053(5) 0.085(5) 0.015(4) 0.112(6) -0.002(5) C3 0.083(5) 0.029(3) 0.072(4) 0.014(3) 0.051(4) 0.006(3) C4 0.043(4) 0.046(4) 0.050(4) -0.005(3) 0.026(3) 0.001(3) C5 0.038(3) 0.052(4) 0.031(3) 0.001(2) 0.022(2) -0.007(3) C6 0.032(3) 0.027(3) 0.025(3) 0.0049(19) 0.016(2) 0.009(2) C7 0.027(3) 0.043(3) 0.045(3) -0.004(2) 0.015(2) -0.004(2) C8 0.036(3) 0.033(3) 0.060(4) -0.015(2) 0.020(3) 0.003(2) C9 0.034(3) 0.036(3) 0.054(3) -0.001(2) 0.018(3) 0.011(2) C10 0.024(3) 0.046(3) 0.046(3) 0.001(2) 0.014(2) -0.001(2) C11 0.029(3) 0.027(3) 0.042(3) 0.000(2) 0.017(2) 0.004(2) C12 0.032(3) 0.048(3) 0.022(3) 0.012(2) 0.015(2) 0.016(2) C13 0.058(4) 0.039(3) 0.025(3) 0.001(2) 0.022(3) 0.004(3) C14 0.050(4) 0.040(3) 0.040(3) -0.002(2) 0.020(3) -0.002(3) C15 0.039(4) 0.062(4) 0.038(3) 0.006(3) 0.000(3) 0.017(3) C16 0.049(4) 0.134(7) 0.031(3) 0.024(3) 0.012(3) 0.013(4) C17 0.032(3) 0.118(6) 0.028(3) 0.018(3) 0.015(2) 0.008(3) C18 0.024(3) 0.023(3) 0.020(2) 0.0038(17) 0.0064(19) 0.0009(19) C19 0.024(3) 0.047(3) 0.026(3) -0.003(2) 0.011(2) -0.006(2) C20 0.046(4) 0.065(4) 0.038(3) 0.000(3) 0.027(3) 0.000(3) C21 0.025(3) 0.043(3) 0.051(3) 0.007(2) 0.022(3) 0.002(2) C22 0.020(3) 0.036(3) 0.043(3) 0.003(2) 0.007(2) -0.006(2) C23 0.029(3) 0.026(3) 0.024(3) 0.0041(19) 0.012(2) 0.000(2) C24 0.027(3) 0.036(3) 0.050(3) 0.009(2) 0.009(2) -0.002(2) C25 0.046(4) 0.039(4) 0.065(4) 0.028(3) 0.013(3) 0.006(3) C26 0.049(4) 0.051(4) 0.042(3) 0.017(3) 0.007(3) 0.021(3) C27 0.029(3) 0.049(4) 0.047(3) 0.015(3) 0.006(2) 0.010(3) C28 0.030(3) 0.044(3) 0.039(3) 0.014(2) 0.010(2) 0.001(2) C29 0.025(3) 0.025(3) 0.030(3) 0.004(2) 0.009(2) -0.001(2) C30 0.067(4) 0.021(3) 0.015(3) 0.0061(19) -0.003(2) -0.021(2) C31 0.106(6) 0.050(4) 0.030(3) -0.001(3) -0.006(3) -0.021(4) C32 0.062(4) 0.031(3) 0.047(4) -0.006(2) 0.001(3) -0.019(3) C33 0.037(3) 0.027(3) 0.050(4) 0.012(2) 0.011(3) -0.003(2) C34 0.028(3) 0.038(3) 0.029(3) 0.005(2) 0.010(2) 0.000(2) C35 0.026(3) 0.030(3) 0.021(2) 0.0052(19) 0.012(2) -0.001(2) C36 0.064(4) 0.028(3) 0.081(4) 0.003(3) 0.019(3) 0.009(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 C35 1.970(5) . ? Pd1 P1 2.3257(11) . ? Pd1 P2 2.3285(11) . ? Pd1 Cl1 2.4035(15) . ? P1 C12 1.806(5) . ? P1 C6 1.824(5) . ? P1 C1 1.837(5) . ? P2 C18 1.811(5) . ? P2 C23 1.828(4) . ? P2 C29 1.837(5) . ? N1 C1 1.335(6) . ? N1 C2 1.350(8) . ? N2 C18 1.401(6) . ? N2 C22 1.412(6) . ? O1 C35 1.185(5) . ? O2 C35 1.338(5) . ? O2 C36 1.458(6) . ? C1 C5 1.349(6) . ? C2 C3 1.350(8) . ? C3 C4 1.350(7) . ? C4 C5 1.372(7) . ? C6 C7 1.373(6) . ? C6 C11 1.387(6) . ? C7 C8 1.392(7) . ? C8 C9 1.366(7) . ? C9 C10 1.379(7) . ? C10 C11 1.379(6) . ? C12 C17 1.374(6) . ? C12 C13 1.376(7) . ? C13 C14 1.382(7) . ? C14 C15 1.356(7) . ? C15 C16 1.359(8) . ? C16 C17 1.390(8) . ? C18 C19 1.367(6) . ? C19 C20 1.364(7) . ? C20 C21 1.367(7) . ? C21 C22 1.390(6) . ? C23 C24 1.371(6) . ? C23 C28 1.375(6) . ? C24 C25 1.384(6) . ? C25 C26 1.373(7) . ? C26 C27 1.362(7) . ? C27 C28 1.379(6) . ? C29 C30 1.341(6) . ? C29 C34 1.369(6) . ? C30 C31 1.335(7) . ? C31 C32 1.356(7) . ? C32 C33 1.353(7) . ? C33 C34 1.376(7) . ? 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 C35 Pd1 P1 87.85(12) . . ? C35 Pd1 P2 89.07(12) . . ? P1 Pd1 P2 174.59(4) . . ? C35 Pd1 Cl1 176.49(13) . . ? P1 Pd1 Cl1 90.09(4) . . ? P2 Pd1 Cl1 93.20(4) . . ? C12 P1 C6 103.2(2) . . ? C12 P1 C1 108.9(2) . . ? C6 P1 C1 102.1(2) . . ? C12 P1 Pd1 113.08(16) . . ? C6 P1 Pd1 118.65(14) . . ? C1 P1 Pd1 110.05(16) . . ? C18 P2 C23 103.5(2) . . ? C18 P2 C29 104.1(2) . . ? C23 P2 C29 101.7(2) . . ? C18 P2 Pd1 115.00(14) . . ? C23 P2 Pd1 118.50(15) . . ? C29 P2 Pd1 112.21(15) . . ? C1 N1 C2 115.4(5) . . ? C18 N2 C22 118.4(4) . . ? C35 O2 C36 115.2(4) . . ? N1 C1 C5 122.0(5) . . ? N1 C1 P1 116.4(4) . . ? C5 C1 P1 121.5(4) . . ? N1 C2 C3 125.8(6) . . ? C2 C3 C4 117.1(6) . . ? C3 C4 C5 118.9(5) . . ? C1 C5 C4 120.7(5) . . ? C7 C6 C11 119.6(4) . . ? C7 C6 P1 120.4(4) . . ? C11 C6 P1 119.9(4) . . ? C6 C7 C8 120.5(5) . . ? C9 C8 C7 119.7(5) . . ? C8 C9 C10 119.9(5) . . ? C9 C10 C11 120.8(5) . . ? C10 C11 C6 119.5(5) . . ? C17 C12 C13 118.1(5) . . ? C17 C12 P1 122.0(4) . . ? C13 C12 P1 119.7(3) . . ? C12 C13 C14 121.4(5) . . ? C15 C14 C13 120.0(5) . . ? C14 C15 C16 119.6(5) . . ? C15 C16 C17 120.9(5) . . ? C12 C17 C16 120.0(5) . . ? C19 C18 N2 120.5(4) . . ? C19 C18 P2 120.4(3) . . ? N2 C18 P2 119.0(3) . . ? C20 C19 C18 120.2(4) . . ? C19 C20 C21 121.6(5) . . ? C20 C21 C22 119.5(5) . . ? C21 C22 N2 119.8(4) . . ? C24 C23 C28 118.7(4) . . ? C24 C23 P2 122.3(4) . . ? C28 C23 P2 119.0(3) . . ? C23 C24 C25 121.1(5) . . ? C26 C25 C24 119.0(5) . . ? C27 C26 C25 120.8(5) . . ? C26 C27 C28 119.6(5) . . ? C23 C28 C27 120.8(5) . . ? C30 C29 C34 121.3(4) . . ? C30 C29 P2 117.7(3) . . ? C34 C29 P2 121.0(3) . . ? C31 C30 C29 117.6(4) . . ? C30 C31 C32 123.5(5) . . ? C33 C32 C31 119.1(5) . . ? C32 C33 C34 118.6(4) . . ? C29 C34 C33 119.9(4) . . ? O1 C35 O2 122.9(4) . . ? O1 C35 Pd1 127.8(4) . . ? O2 C35 Pd1 109.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C35 Pd1 P1 C12 121.1(2) . . . . ? P2 Pd1 P1 C12 176.5(5) . . . . ? Cl1 Pd1 P1 C12 -56.10(18) . . . . ? C35 Pd1 P1 C6 0.0(2) . . . . ? P2 Pd1 P1 C6 55.5(5) . . . . ? Cl1 Pd1 P1 C6 -177.11(18) . . . . ? C35 Pd1 P1 C1 -116.9(2) . . . . ? P2 Pd1 P1 C1 -61.5(5) . . . . ? Cl1 Pd1 P1 C1 65.94(17) . . . . ? C35 Pd1 P2 C18 -124.1(2) . . . . ? P1 Pd1 P2 C18 -179(32) . . . . ? Cl1 Pd1 P2 C18 53.21(16) . . . . ? C35 Pd1 P2 C23 -1.0(2) . . . . ? P1 Pd1 P2 C23 -56.4(5) . . . . ? Cl1 Pd1 P2 C23 176.27(17) . . . . ? C35 Pd1 P2 C29 117.1(2) . . . . ? P1 Pd1 P2 C29 61.8(5) . . . . ? Cl1 Pd1 P2 C29 -65.57(16) . . . . ? C2 N1 C1 C5 0.0(9) . . . . ? C2 N1 C1 P1 -176.2(5) . . . . ? C12 P1 C1 N1 -59.8(5) . . . . ? C6 P1 C1 N1 48.9(5) . . . . ? Pd1 P1 C1 N1 175.8(4) . . . . ? C12 P1 C1 C5 124.1(4) . . . . ? C6 P1 C1 C5 -127.3(4) . . . . ? Pd1 P1 C1 C5 -0.4(5) . . . . ? C1 N1 C2 C3 -0.5(12) . . . . ? N1 C2 C3 C4 1.2(12) . . . . ? C2 C3 C4 C5 -1.4(9) . . . . ? N1 C1 C5 C4 -0.2(8) . . . . ? P1 C1 C5 C4 175.8(4) . . . . ? C3 C4 C5 C1 0.9(8) . . . . ? C12 P1 C6 C7 -38.3(4) . . . . ? C1 P1 C6 C7 -151.3(4) . . . . ? Pd1 P1 C6 C7 87.6(4) . . . . ? C12 P1 C6 C11 145.6(4) . . . . ? C1 P1 C6 C11 32.6(4) . . . . ? Pd1 P1 C6 C11 -88.5(4) . . . . ? C11 C6 C7 C8 0.2(7) . . . . ? P1 C6 C7 C8 -175.9(4) . . . . ? C6 C7 C8 C9 -1.0(8) . . . . ? C7 C8 C9 C10 1.1(8) . . . . ? C8 C9 C10 C11 -0.5(8) . . . . ? C9 C10 C11 C6 -0.2(7) . . . . ? C7 C6 C11 C10 0.4(7) . . . . ? P1 C6 C11 C10 176.5(3) . . . . ? C6 P1 C12 C17 -63.7(5) . . . . ? C1 P1 C12 C17 44.2(5) . . . . ? Pd1 P1 C12 C17 166.9(4) . . . . ? C6 P1 C12 C13 110.9(4) . . . . ? C1 P1 C12 C13 -141.2(4) . . . . ? Pd1 P1 C12 C13 -18.5(5) . . . . ? C17 C12 C13 C14 0.9(8) . . . . ? P1 C12 C13 C14 -173.9(4) . . . . ? C12 C13 C14 C15 -0.2(8) . . . . ? C13 C14 C15 C16 -1.6(8) . . . . ? C14 C15 C16 C17 2.7(10) . . . . ? C13 C12 C17 C16 0.2(8) . . . . ? P1 C12 C17 C16 174.9(5) . . . . ? C15 C16 C17 C12 -2.1(10) . . . . ? C22 N2 C18 C19 1.0(7) . . . . ? C22 N2 C18 P2 177.8(4) . . . . ? C23 P2 C18 C19 58.5(4) . . . . ? C29 P2 C18 C19 -47.5(4) . . . . ? Pd1 P2 C18 C19 -170.7(3) . . . . ? C23 P2 C18 N2 -118.3(4) . . . . ? C29 P2 C18 N2 135.7(4) . . . . ? Pd1 P2 C18 N2 12.5(4) . . . . ? N2 C18 C19 C20 -1.1(7) . . . . ? P2 C18 C19 C20 -177.9(4) . . . . ? C18 C19 C20 C21 1.1(8) . . . . ? C19 C20 C21 C22 -1.0(8) . . . . ? C20 C21 C22 N2 0.9(7) . . . . ? C18 N2 C22 C21 -0.9(7) . . . . ? C18 P2 C23 C24 20.1(4) . . . . ? C29 P2 C23 C24 128.0(4) . . . . ? Pd1 P2 C23 C24 -108.5(4) . . . . ? C18 P2 C23 C28 -160.5(4) . . . . ? C29 P2 C23 C28 -52.6(4) . . . . ? Pd1 P2 C23 C28 70.9(4) . . . . ? C28 C23 C24 C25 -0.4(7) . . . . ? P2 C23 C24 C25 179.0(4) . . . . ? C23 C24 C25 C26 1.8(8) . . . . ? C24 C25 C26 C27 -1.7(9) . . . . ? C25 C26 C27 C28 0.2(9) . . . . ? C24 C23 C28 C27 -1.1(7) . . . . ? P2 C23 C28 C27 179.4(4) . . . . ? C26 C27 C28 C23 1.3(8) . . . . ? C18 P2 C29 C30 68.5(4) . . . . ? C23 P2 C29 C30 -38.8(4) . . . . ? Pd1 P2 C29 C30 -166.5(3) . . . . ? C18 P2 C29 C34 -109.3(4) . . . . ? C23 P2 C29 C34 143.4(4) . . . . ? Pd1 P2 C29 C34 15.7(4) . . . . ? C34 C29 C30 C31 0.8(8) . . . . ? P2 C29 C30 C31 -177.0(5) . . . . ? C29 C30 C31 C32 -0.9(10) . . . . ? C30 C31 C32 C33 0.4(11) . . . . ? C31 C32 C33 C34 0.3(9) . . . . ? C30 C29 C34 C33 -0.1(7) . . . . ? P2 C29 C34 C33 177.6(4) . . . . ? C32 C33 C34 C29 -0.4(7) . . . . ? C36 O2 C35 O1 -0.5(6) . . . . ? C36 O2 C35 Pd1 179.1(3) . . . . ? P1 Pd1 C35 O1 85.9(4) . . . . ? P2 Pd1 C35 O1 -89.6(4) . . . . ? Cl1 Pd1 C35 O1 140.1(19) . . . . ? P1 Pd1 C35 O2 -93.7(3) . . . . ? P2 Pd1 C35 O2 90.8(3) . . . . ? Cl1 Pd1 C35 O2 -39(2) . . . . ? _diffrn_measured_fraction_theta_max 0.815 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.815 _refine_diff_density_max 0.939 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.096 data_struct8 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H37 F3 N2 O2 P2 Pd' _chemical_formula_weight 827.08 _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' 'O' 'O' 0.0106 0.0060 '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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.557(4) _cell_length_b 20.895(2) _cell_length_c 15.5579(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.767(10) _cell_angle_gamma 90.00 _cell_volume 3752.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method ? _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13837 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.1267 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5355 _reflns_number_observed 3800 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0181P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5355 _refine_ls_number_parameters 500 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_obs 0.0339 _refine_ls_wR_factor_all 0.0651 _refine_ls_wR_factor_obs 0.0630 _refine_ls_goodness_of_fit_all 0.834 _refine_ls_goodness_of_fit_obs 0.979 _refine_ls_restrained_S_all 0.833 _refine_ls_restrained_S_obs 0.977 _refine_ls_shift/esd_max 0.000 _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 0.93529(2) 0.356423(14) 0.80744(2) 0.03699(10) Uani 1 d . . P1 P 0.94522(8) 0.39912(5) 0.67041(5) 0.0361(3) Uani 1 d . . P2 P 0.94723(8) 0.24622(5) 0.79267(5) 0.0390(3) Uani 1 d . . F1 F 0.9583(16) 0.0287(8) 0.3688(8) 0.114(7) Uani 0.76(5) d P 1 F1' F 1.0410(99) 0.0108(13) 0.3564(20) 0.158(24) Uani 0.24(5) d PU 2 F2 F 1.1297(9) 0.0223(9) 0.4130(17) 0.141(8) Uani 0.68(3) d P 1 F2' F 1.1122(45) 0.0551(15) 0.4638(27) 0.167(16) Uani 0.32(3) d PU 2 F3 F 1.0018(12) 0.0820(5) 0.4779(4) 0.137(5) Uani 0.76(3) d P 1 F3' F 0.9354(37) 0.0667(16) 0.4207(50) 0.216(25) Uani 0.24(3) d PU 2 N1 N 1.1773(3) 0.4230(2) 0.7003(2) 0.0837(12) Uani 1 d . . N2 N 1.1711(3) 0.2517(2) 0.7591(2) 0.0706(10) Uani 1 d . . O1 O 1.1682(3) 0.1454(2) 0.3717(2) 0.1028(12) Uani 1 d . . O2 O 1.0014(3) 0.1414(2) 0.2948(2) 0.1008(11) Uani 1 d . . C1 C 0.9686(3) 0.3493(2) 0.5751(2) 0.0384(9) Uani 1 d . . C2 C 1.0505(3) 0.3641(2) 0.5188(2) 0.0594(12) Uani 1 d . . H2 H 1.0996(3) 0.3988(2) 0.5294(2) 0.071 Uiso 1 calc R . C3 C 1.0606(5) 0.3278(3) 0.4463(3) 0.090(2) Uani 1 d . . H3 H 1.1163(5) 0.3377(3) 0.4073(3) 0.109 Uiso 1 calc R . C4 C 0.9883(6) 0.2771(3) 0.4319(3) 0.096(2) Uani 1 d . . H4 H 0.9964(6) 0.2510(3) 0.3842(3) 0.116 Uiso 1 calc R . C5 C 0.9047(6) 0.2650(2) 0.4874(4) 0.104(2) Uani 1 d . . H5 H 0.8533(6) 0.2315(2) 0.4759(4) 0.124 Uiso 1 calc R . C6 C 0.8937(4) 0.3015(2) 0.5614(3) 0.0608(12) Uani 1 d . . H6 H 0.8364(4) 0.2929(2) 0.5997(3) 0.073 Uiso 1 calc R . C7 C 0.8204(3) 0.4463(2) 0.6345(2) 0.0355(9) Uani 1 d . . C8 C 0.8163(3) 0.4798(2) 0.5577(2) 0.0498(11) Uani 1 d . . H8 H 0.8792(3) 0.4786(2) 0.5226(2) 0.060 Uiso 1 calc R . C9 C 0.7197(4) 0.5147(2) 0.5334(3) 0.0634(12) Uani 1 d . . H9 H 0.7188(4) 0.5374(2) 0.4819(3) 0.076 Uiso 1 calc R . C10 C 0.6250(4) 0.5171(2) 0.5823(3) 0.0588(12) Uani 1 d . . H10 H 0.5605(4) 0.5412(2) 0.5649(3) 0.071 Uiso 1 calc R . C11 C 0.6271(3) 0.4831(2) 0.6579(2) 0.0525(11) Uani 1 d . . H11 H 0.5630(3) 0.4839(2) 0.6919(2) 0.063 Uiso 1 calc R . C12 C 0.7239(3) 0.4476(2) 0.6842(2) 0.0457(10) Uani 1 d . . H12 H 0.7241(3) 0.4246(2) 0.7354(2) 0.055 Uiso 1 calc R . C13 C 1.0690(3) 0.4529(2) 0.6762(2) 0.0405(9) Uani 1 d . . C14 C 1.0627(4) 0.5181(2) 0.6664(2) 0.0546(11) Uani 1 d . . H14 H 0.9921(4) 0.5373(2) 0.6509(2) 0.065 Uiso 1 calc R . C15 C 1.2740(4) 0.4633(3) 0.7124(3) 0.0683(14) Uani 1 d . . H15 H 1.3457(4) 0.4455(3) 0.7278(3) 0.082 Uiso 1 calc R . C16 C 1.2654(4) 0.5281(3) 0.7021(3) 0.082(2) Uani 1 d . . H16 H 1.3311(4) 0.5535(3) 0.7104(3) 0.098 Uiso 1 calc R . C17 C 1.1615(5) 0.5558(2) 0.6796(3) 0.0752(14) Uani 1 d . . H17 H 1.1566(5) 0.6000(2) 0.6730(3) 0.090 Uiso 1 calc R . C18 C 0.9679(3) 0.2047(2) 0.8963(2) 0.0392(9) Uani 1 d . . C19 C 1.0734(3) 0.1806(2) 0.9277(2) 0.0525(11) Uani 1 d . . H19 H 1.1375(3) 0.1813(2) 0.8938(2) 0.063 Uiso 1 calc R . C20 C 1.0821(4) 0.1553(2) 1.0105(3) 0.0652(13) Uani 1 d . . H20 H 1.1529(4) 0.1393(2) 1.0319(3) 0.078 Uiso 1 calc R . C21 C 0.9894(5) 0.1536(2) 1.0604(2) 0.0647(13) Uani 1 d . . H21 H 0.9965(5) 0.1368(2) 1.1158(2) 0.078 Uiso 1 calc R . C22 C 0.8852(4) 0.1768(2) 1.0287(2) 0.0571(12) Uani 1 d . . H22 H 0.8210(4) 0.1753(2) 1.0624(2) 0.069 Uiso 1 calc R . C23 C 0.8751(3) 0.2024(2) 0.9474(2) 0.0497(10) Uani 1 d . . H23 H 0.8039(3) 0.2183(2) 0.9268(2) 0.060 Uiso 1 calc R . C24 C 0.8190(3) 0.2057(2) 0.7474(2) 0.0407(9) Uani 1 d . . C25 C 0.8141(4) 0.1406(2) 0.7417(3) 0.0682(13) Uani 1 d . . H25 H 0.8793(4) 0.1164(2) 0.7572(3) 0.082 Uiso 1 calc R . C26 C 0.7139(5) 0.1105(2) 0.7132(3) 0.086(2) Uani 1 d . . H26 H 0.7121(5) 0.0661(2) 0.7090(3) 0.104 Uiso 1 calc R . C27 C 0.6163(4) 0.1453(3) 0.6908(3) 0.0799(14) Uani 1 d . . H27 H 0.5486(4) 0.1247(3) 0.6716(3) 0.096 Uiso 1 calc R . C28 C 0.6194(4) 0.2098(2) 0.6969(3) 0.0697(13) Uani 1 d . . H28 H 0.5534(4) 0.2335(2) 0.6818(3) 0.084 Uiso 1 calc R . C29 C 0.7208(3) 0.2412(2) 0.7257(2) 0.0535(11) Uani 1 d . . H29 H 0.7222(3) 0.2855(2) 0.7303(2) 0.064 Uiso 1 calc R . C30 C 1.0712(3) 0.2220(2) 0.7315(2) 0.0438(10) Uani 1 d . . C31 C 1.0695(4) 0.1812(2) 0.6637(3) 0.0717(13) Uani 1 d . . H31 H 1.0006(4) 0.1616(2) 0.6449(3) 0.086 Uiso 1 calc R . C32 C 1.2703(4) 0.2378(2) 0.7182(3) 0.0695(13) Uani 1 d . . H32 H 1.3392(4) 0.2573(2) 0.7372(3) 0.083 Uiso 1 calc R . C33 C 1.2714(4) 0.1966(3) 0.6512(3) 0.0775(15) Uani 1 d . . H33 H 1.3404(4) 0.1875(3) 0.6253(3) 0.093 Uiso 1 calc R . C34 C 1.1716(5) 0.1687(2) 0.6222(3) 0.087(2) Uani 1 d . . H34 H 1.1708(5) 0.1414(2) 0.5750(3) 0.104 Uiso 1 calc R . C35 C 0.9378(3) 0.3570(2) 0.9466(2) 0.0529(11) Uani 1 d . . H35A H 0.8633(3) 0.3611(2) 0.9722(2) 0.063 Uiso 1 calc R . H35B H 0.9885(3) 0.3261(2) 0.9758(2) 0.063 Uiso 1 calc R . C36 C 0.9897(4) 0.4142(2) 0.9209(2) 0.0462(10) Uani 1 d . . C37 C 0.9192(3) 0.4508(2) 0.8629(2) 0.0511(11) Uani 1 d . . H37A H 0.9572(3) 0.4854(2) 0.8337(2) 0.061 Uiso 1 calc R . H37B H 0.8432(3) 0.4623(2) 0.8818(2) 0.061 Uiso 1 calc R . C38 C 1.1167(4) 0.4281(3) 0.9356(2) 0.0592(12) Uani 1 d . . C39 C 1.1955(4) 0.3737(3) 0.9543(3) 0.121(2) Uani 1 d . . H39A H 1.1913(26) 0.3443(10) 0.9069(11) 0.181 Uiso 1 calc R . H39B H 1.1730(21) 0.3523(12) 1.0055(15) 0.181 Uiso 1 calc R . H39C H 1.2734(6) 0.3892(3) 0.9627(25) 0.181 Uiso 1 calc R . C40 C 1.1565(4) 0.4874(3) 0.9293(3) 0.087(2) Uani 1 d . . H40A H 1.2355(4) 0.4954(3) 0.9366(3) 0.105 Uiso 1 calc R . H40B H 1.1053(4) 0.5210(3) 0.9174(3) 0.105 Uiso 1 calc R . C41 C 1.0721(5) 0.1237(2) 0.3487(3) 0.0682(14) Uani 1 d . . C42 C 1.0417(6) 0.0647(4) 0.4019(4) 0.084(2) 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 0.0403(2) 0.0363(2) 0.03423(14) 0.0020(2) 0.00052(11) 0.0011(2) P1 0.0363(6) 0.0360(7) 0.0360(5) 0.0047(5) 0.0017(4) -0.0006(5) P2 0.0401(6) 0.0344(6) 0.0421(5) 0.0038(5) -0.0016(5) -0.0007(5) F1 0.121(10) 0.103(9) 0.114(7) 0.021(6) -0.040(5) -0.032(6) F1' 0.250(72) 0.084(15) 0.140(19) 0.014(13) 0.021(26) 0.037(24) F2 0.078(7) 0.126(10) 0.220(16) 0.080(10) 0.013(7) 0.026(6) F2' 0.226(32) 0.106(17) 0.155(18) 0.037(14) -0.138(20) -0.009(18) F3 0.156(10) 0.187(8) 0.070(5) -0.001(4) 0.034(5) -0.055(7) F3' 0.132(29) 0.210(28) 0.316(59) -0.063(33) 0.107(34) -0.071(20) N1 0.063(3) 0.123(4) 0.065(2) -0.011(2) 0.003(2) -0.011(3) N2 0.063(3) 0.080(3) 0.069(2) 0.000(2) 0.010(2) -0.004(2) O1 0.066(3) 0.116(3) 0.127(3) 0.002(2) 0.007(2) -0.013(2) O2 0.107(3) 0.098(3) 0.093(2) 0.011(2) -0.031(2) 0.011(2) C1 0.039(2) 0.037(3) 0.039(2) 0.001(2) -0.004(2) 0.007(2) C2 0.051(3) 0.080(4) 0.049(2) -0.015(3) 0.012(2) -0.012(2) C3 0.070(4) 0.139(6) 0.064(3) -0.023(3) 0.017(3) 0.016(4) C4 0.120(6) 0.091(5) 0.076(4) -0.030(4) -0.022(4) 0.042(4) C5 0.120(6) 0.055(4) 0.131(5) -0.002(4) -0.041(4) -0.035(4) C6 0.069(3) 0.054(3) 0.059(3) -0.008(2) 0.003(2) -0.027(3) C7 0.036(2) 0.034(2) 0.037(2) -0.002(2) -0.003(2) -0.003(2) C8 0.046(3) 0.056(3) 0.047(2) 0.008(2) 0.003(2) 0.004(2) C9 0.076(4) 0.057(3) 0.056(3) 0.019(2) -0.008(3) 0.006(3) C10 0.058(3) 0.046(3) 0.071(3) 0.004(2) -0.013(2) 0.012(2) C11 0.042(3) 0.053(3) 0.063(3) -0.009(2) 0.002(2) 0.001(2) C12 0.040(3) 0.049(3) 0.047(2) 0.004(2) -0.005(2) -0.001(2) C13 0.036(2) 0.048(3) 0.038(2) 0.000(2) 0.001(2) -0.001(2) C14 0.051(3) 0.048(3) 0.064(3) 0.000(2) -0.002(2) -0.004(2) C15 0.036(3) 0.096(4) 0.072(3) -0.013(3) -0.006(2) -0.016(3) C16 0.058(4) 0.101(5) 0.085(3) -0.015(4) -0.003(3) -0.039(3) C17 0.084(4) 0.052(3) 0.089(3) -0.009(3) 0.002(3) -0.027(3) C18 0.044(3) 0.030(2) 0.043(2) 0.002(2) 0.000(2) -0.001(2) C19 0.049(3) 0.052(3) 0.056(2) 0.011(2) 0.002(2) 0.002(2) C20 0.060(3) 0.068(4) 0.065(3) 0.017(3) -0.021(2) 0.008(2) C21 0.095(4) 0.050(3) 0.048(2) 0.013(2) -0.009(3) -0.011(3) C22 0.070(3) 0.047(3) 0.055(3) 0.001(2) 0.013(2) -0.007(2) C23 0.049(3) 0.052(3) 0.048(2) 0.012(2) -0.001(2) 0.002(2) C24 0.042(3) 0.037(3) 0.043(2) 0.007(2) -0.005(2) -0.002(2) C25 0.060(3) 0.041(3) 0.101(3) 0.008(3) -0.031(2) -0.001(2) C26 0.079(4) 0.044(3) 0.132(4) 0.004(3) -0.037(3) -0.013(3) C27 0.067(4) 0.067(4) 0.103(3) 0.014(3) -0.028(3) -0.025(3) C28 0.037(3) 0.078(4) 0.092(3) 0.023(3) -0.010(2) -0.001(3) C29 0.043(3) 0.046(3) 0.071(3) 0.003(2) 0.002(2) -0.002(2) C30 0.040(3) 0.049(3) 0.042(2) 0.000(2) -0.001(2) 0.003(2) C31 0.060(3) 0.083(4) 0.072(3) -0.025(3) -0.006(3) 0.001(3) C32 0.051(3) 0.092(4) 0.067(3) 0.006(3) 0.008(2) -0.001(3) C33 0.057(4) 0.106(5) 0.071(3) 0.001(3) 0.017(3) 0.019(3) C34 0.084(4) 0.105(5) 0.074(3) -0.042(3) 0.016(3) 0.021(3) C35 0.069(3) 0.062(3) 0.029(2) 0.000(2) 0.011(2) 0.012(2) C36 0.058(3) 0.049(3) 0.032(2) -0.007(2) -0.000(2) 0.004(2) C37 0.058(3) 0.044(3) 0.051(2) -0.011(2) 0.004(2) 0.012(2) C38 0.054(3) 0.076(4) 0.048(2) -0.014(3) -0.006(2) 0.002(3) C39 0.065(4) 0.134(6) 0.160(5) 0.025(4) -0.040(4) 0.007(4) C40 0.072(4) 0.086(4) 0.102(4) -0.035(3) -0.002(3) -0.021(3) C41 0.064(4) 0.074(4) 0.068(3) 0.002(3) 0.014(3) 0.013(3) C42 0.059(5) 0.125(7) 0.066(4) 0.008(4) -0.004(4) -0.004(4) _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 C35 2.164(3) . ? Pd1 C37 2.165(3) . ? Pd1 C36 2.205(3) . ? Pd1 P2 2.3189(10) . ? Pd1 P1 2.3189(9) . ? P1 C7 1.813(4) . ? P1 C13 1.819(4) . ? P1 C1 1.843(3) . ? P2 C24 1.819(4) . ? P2 C30 1.829(4) . ? P2 C18 1.836(3) . ? F1 C42 1.308(10) . ? F1' C42 1.33(3) . ? F2 C42 1.354(12) . ? F2' C42 1.25(2) . ? F3 C42 1.339(10) . ? F3' C42 1.28(3) . ? N1 C15 1.406(5) . ? N1 C13 1.432(5) . ? N2 C30 1.361(5) . ? N2 C32 1.369(5) . ? O1 C41 1.236(5) . ? O2 C41 1.201(5) . ? C1 C6 1.332(5) . ? C1 C2 1.356(5) . ? C2 C3 1.368(6) . ? C3 C4 1.362(7) . ? C4 C5 1.350(7) . ? C5 C6 1.391(6) . ? C7 C8 1.383(4) . ? C7 C12 1.388(4) . ? C8 C9 1.372(5) . ? C9 C10 1.365(5) . ? C10 C11 1.373(5) . ? C11 C12 1.387(5) . ? C13 C14 1.373(5) . ? C14 C17 1.394(5) . ? C15 C16 1.365(6) . ? C16 C17 1.364(6) . ? C18 C23 1.367(5) . ? C18 C19 1.386(5) . ? C19 C20 1.391(5) . ? C20 C21 1.354(5) . ? C21 C22 1.368(5) . ? C22 C23 1.372(5) . ? C24 C25 1.363(5) . ? C24 C29 1.385(5) . ? C25 C26 1.373(5) . ? C26 C27 1.373(6) . ? C27 C28 1.351(6) . ? C28 C29 1.398(5) . ? C30 C31 1.357(5) . ? C31 C34 1.396(6) . ? C32 C33 1.353(6) . ? C33 C34 1.350(6) . ? C35 C36 1.403(5) . ? C36 C37 1.412(5) . ? C36 C38 1.502(5) . ? C38 C40 1.327(6) . ? C38 C39 1.477(6) . ? C41 C42 1.536(7) . ? 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 C35 Pd1 C37 66.00(14) . . ? C35 Pd1 C36 37.45(13) . . ? C37 Pd1 C36 37.70(12) . . ? C35 Pd1 P2 96.13(11) . . ? C37 Pd1 P2 162.01(10) . . ? C36 Pd1 P2 127.35(11) . . ? C35 Pd1 P1 156.74(12) . . ? C37 Pd1 P1 91.42(10) . . ? C36 Pd1 P1 120.05(11) . . ? P2 Pd1 P1 106.57(3) . . ? C7 P1 C13 107.0(2) . . ? C7 P1 C1 101.79(15) . . ? C13 P1 C1 104.1(2) . . ? C7 P1 Pd1 114.75(12) . . ? C13 P1 Pd1 105.42(11) . . ? C1 P1 Pd1 122.57(12) . . ? C24 P2 C30 108.3(2) . . ? C24 P2 C18 100.9(2) . . ? C30 P2 C18 104.7(2) . . ? C24 P2 Pd1 116.72(13) . . ? C30 P2 Pd1 112.21(13) . . ? C18 P2 Pd1 112.81(11) . . ? C15 N1 C13 116.9(4) . . ? C30 N2 C32 118.2(4) . . ? C6 C1 C2 122.4(4) . . ? C6 C1 P1 115.6(3) . . ? C2 C1 P1 121.7(3) . . ? C1 C2 C3 119.7(4) . . ? C4 C3 C2 119.4(5) . . ? C5 C4 C3 119.5(5) . . ? C4 C5 C6 121.5(5) . . ? C1 C6 C5 117.3(4) . . ? C8 C7 C12 118.5(3) . . ? C8 C7 P1 122.3(3) . . ? C12 C7 P1 119.2(3) . . ? C9 C8 C7 120.1(4) . . ? C10 C9 C8 121.9(4) . . ? C9 C10 C11 118.6(4) . . ? C10 C11 C12 120.6(4) . . ? C11 C12 C7 120.3(3) . . ? C14 C13 N1 120.2(4) . . ? C14 C13 P1 124.8(3) . . ? N1 C13 P1 114.7(3) . . ? C13 C14 C17 120.3(4) . . ? C16 C15 N1 121.7(5) . . ? C17 C16 C15 120.6(4) . . ? C16 C17 C14 120.2(5) . . ? C23 C18 C19 118.9(3) . . ? C23 C18 P2 117.1(3) . . ? C19 C18 P2 123.8(3) . . ? C18 C19 C20 119.2(4) . . ? C21 C20 C19 121.1(4) . . ? C20 C21 C22 119.4(4) . . ? C21 C22 C23 120.3(4) . . ? C18 C23 C22 121.0(4) . . ? C25 C24 C29 119.1(4) . . ? C25 C24 P2 121.4(3) . . ? C29 C24 P2 119.2(3) . . ? C24 C25 C26 120.7(4) . . ? C27 C26 C25 120.6(5) . . ? C28 C27 C26 119.5(4) . . ? C27 C28 C29 120.6(4) . . ? C24 C29 C28 119.5(4) . . ? C31 C30 N2 120.8(4) . . ? C31 C30 P2 126.6(3) . . ? N2 C30 P2 112.5(3) . . ? C30 C31 C34 119.7(4) . . ? C33 C32 N2 122.2(4) . . ? C34 C33 C32 119.5(5) . . ? C33 C34 C31 119.5(4) . . ? C36 C35 Pd1 72.9(2) . . ? C35 C36 C37 113.7(4) . . ? C35 C36 C38 123.3(4) . . ? C37 C36 C38 121.4(4) . . ? C35 C36 Pd1 69.7(2) . . ? C37 C36 Pd1 69.6(2) . . ? C38 C36 Pd1 117.8(2) . . ? C36 C37 Pd1 72.7(2) . . ? C40 C38 C39 121.4(5) . . ? C40 C38 C36 120.6(4) . . ? C39 C38 C36 118.0(4) . . ? O2 C41 O1 131.4(5) . . ? O2 C41 C42 117.2(5) . . ? O1 C41 C42 111.4(5) . . ? F2' C42 F3' 115.4(42) . . ? F2' C42 F1' 105.2(38) . . ? F3' C42 F1' 99.7(52) . . ? F1 C42 F3 103.0(11) . . ? F1 C42 F2 102.0(15) . . ? F3 C42 F2 110.6(11) . . ? F2' C42 C41 112.7(13) . . ? F3' C42 C41 110.2(19) . . ? F1 C42 C41 115.7(5) . . ? F1' C42 C41 112.9(15) . . ? F3 C42 C41 110.9(8) . . ? F2 C42 C41 113.8(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C35 Pd1 P1 C7 -72.6(3) . . . . ? C37 Pd1 P1 C7 -59.2(2) . . . . ? C36 Pd1 P1 C7 -85.0(2) . . . . ? P2 Pd1 P1 C7 120.35(13) . . . . ? C35 Pd1 P1 C13 44.8(3) . . . . ? C37 Pd1 P1 C13 58.2(2) . . . . ? C36 Pd1 P1 C13 32.4(2) . . . . ? P2 Pd1 P1 C13 -122.22(13) . . . . ? C35 Pd1 P1 C1 163.2(3) . . . . ? C37 Pd1 P1 C1 176.6(2) . . . . ? C36 Pd1 P1 C1 150.8(2) . . . . ? P2 Pd1 P1 C1 -3.80(15) . . . . ? C35 Pd1 P2 C24 110.7(2) . . . . ? C37 Pd1 P2 C24 104.1(4) . . . . ? C36 Pd1 P2 C24 133.4(2) . . . . ? P1 Pd1 P2 C24 -74.46(13) . . . . ? C35 Pd1 P2 C30 -123.5(2) . . . . ? C37 Pd1 P2 C30 -130.1(4) . . . . ? C36 Pd1 P2 C30 -100.8(2) . . . . ? P1 Pd1 P2 C30 51.36(14) . . . . ? C35 Pd1 P2 C18 -5.5(2) . . . . ? C37 Pd1 P2 C18 -12.1(4) . . . . ? C36 Pd1 P2 C18 17.2(2) . . . . ? P1 Pd1 P2 C18 169.37(13) . . . . ? C7 P1 C1 C6 -74.7(3) . . . . ? C13 P1 C1 C6 174.2(3) . . . . ? Pd1 P1 C1 C6 55.1(3) . . . . ? C7 P1 C1 C2 99.6(3) . . . . ? C13 P1 C1 C2 -11.5(3) . . . . ? Pd1 P1 C1 C2 -130.5(3) . . . . ? C6 C1 C2 C3 -2.4(6) . . . . ? P1 C1 C2 C3 -176.3(3) . . . . ? C1 C2 C3 C4 -0.2(7) . . . . ? C2 C3 C4 C5 2.7(9) . . . . ? C3 C4 C5 C6 -2.9(9) . . . . ? C2 C1 C6 C5 2.2(6) . . . . ? P1 C1 C6 C5 176.6(3) . . . . ? C4 C5 C6 C1 0.4(8) . . . . ? C13 P1 C7 C8 57.6(3) . . . . ? C1 P1 C7 C8 -51.3(3) . . . . ? Pd1 P1 C7 C8 174.2(3) . . . . ? C13 P1 C7 C12 -124.2(3) . . . . ? C1 P1 C7 C12 126.9(3) . . . . ? Pd1 P1 C7 C12 -7.6(3) . . . . ? C12 C7 C8 C9 1.7(6) . . . . ? P1 C7 C8 C9 179.9(3) . . . . ? C7 C8 C9 C10 -0.8(6) . . . . ? C8 C9 C10 C11 -0.3(6) . . . . ? C9 C10 C11 C12 0.6(6) . . . . ? C10 C11 C12 C7 0.3(6) . . . . ? C8 C7 C12 C11 -1.5(5) . . . . ? P1 C7 C12 C11 -179.7(3) . . . . ? C15 N1 C13 C14 -0.4(5) . . . . ? C15 N1 C13 P1 -175.1(3) . . . . ? C7 P1 C13 C14 8.1(3) . . . . ? C1 P1 C13 C14 115.4(3) . . . . ? Pd1 P1 C13 C14 -114.4(3) . . . . ? C7 P1 C13 N1 -177.5(2) . . . . ? C1 P1 C13 N1 -70.2(3) . . . . ? Pd1 P1 C13 N1 60.0(3) . . . . ? N1 C13 C14 C17 0.2(5) . . . . ? P1 C13 C14 C17 174.3(3) . . . . ? C13 N1 C15 C16 0.2(6) . . . . ? N1 C15 C16 C17 0.1(7) . . . . ? C15 C16 C17 C14 -0.3(7) . . . . ? C13 C14 C17 C16 0.2(6) . . . . ? C24 P2 C18 C23 -53.1(3) . . . . ? C30 P2 C18 C23 -165.5(3) . . . . ? Pd1 P2 C18 C23 72.2(3) . . . . ? C24 P2 C18 C19 132.2(3) . . . . ? C30 P2 C18 C19 19.8(4) . . . . ? Pd1 P2 C18 C19 -102.5(3) . . . . ? C23 C18 C19 C20 -0.7(6) . . . . ? P2 C18 C19 C20 174.0(3) . . . . ? C18 C19 C20 C21 0.4(6) . . . . ? C19 C20 C21 C22 0.4(7) . . . . ? C20 C21 C22 C23 -0.8(6) . . . . ? C19 C18 C23 C22 0.2(6) . . . . ? P2 C18 C23 C22 -174.8(3) . . . . ? C21 C22 C23 C18 0.5(6) . . . . ? C30 P2 C24 C25 57.0(3) . . . . ? C18 P2 C24 C25 -52.7(3) . . . . ? Pd1 P2 C24 C25 -175.3(3) . . . . ? C30 P2 C24 C29 -129.1(3) . . . . ? C18 P2 C24 C29 121.3(3) . . . . ? Pd1 P2 C24 C29 -1.3(3) . . . . ? C29 C24 C25 C26 1.3(6) . . . . ? P2 C24 C25 C26 175.2(3) . . . . ? C24 C25 C26 C27 -0.7(7) . . . . ? C25 C26 C27 C28 0.1(8) . . . . ? C26 C27 C28 C29 0.0(7) . . . . ? C25 C24 C29 C28 -1.2(6) . . . . ? P2 C24 C29 C28 -175.3(3) . . . . ? C27 C28 C29 C24 0.6(6) . . . . ? C32 N2 C30 C31 -2.0(6) . . . . ? C32 N2 C30 P2 -179.8(3) . . . . ? C24 P2 C30 C31 0.3(4) . . . . ? C18 P2 C30 C31 107.3(4) . . . . ? Pd1 P2 C30 C31 -130.0(3) . . . . ? C24 P2 C30 N2 178.0(3) . . . . ? C18 P2 C30 N2 -75.0(3) . . . . ? Pd1 P2 C30 N2 47.7(3) . . . . ? N2 C30 C31 C34 0.9(6) . . . . ? P2 C30 C31 C34 178.4(3) . . . . ? C30 N2 C32 C33 1.0(6) . . . . ? N2 C32 C33 C34 1.1(7) . . . . ? C32 C33 C34 C31 -2.2(8) . . . . ? C30 C31 C34 C33 1.2(7) . . . . ? C37 Pd1 C35 C36 -32.5(2) . . . . ? C36 Pd1 C35 C36 0.000(1) . . . . ? P2 Pd1 C35 C36 149.7(2) . . . . ? P1 Pd1 C35 C36 -17.8(4) . . . . ? Pd1 C35 C36 C37 55.3(3) . . . . ? Pd1 C35 C36 C38 -110.6(3) . . . . ? Pd1 C35 C36 Pd1 0.0 . . . . ? C35 Pd1 C36 C35 0.000(1) . . . . ? C37 Pd1 C36 C35 126.5(4) . . . . ? P2 Pd1 C36 C35 -39.2(3) . . . . ? P1 Pd1 C36 C35 172.0(2) . . . . ? C35 Pd1 C36 C37 -126.5(4) . . . . ? C37 Pd1 C36 C37 0.000(2) . . . . ? P2 Pd1 C36 C37 -165.7(2) . . . . ? P1 Pd1 C36 C37 45.4(3) . . . . ? C35 Pd1 C36 C38 117.8(4) . . . . ? C37 Pd1 C36 C38 -115.6(4) . . . . ? P2 Pd1 C36 C38 78.7(3) . . . . ? P1 Pd1 C36 C38 -70.2(3) . . . . ? C35 C36 C37 Pd1 -55.4(3) . . . . ? C38 C36 C37 Pd1 110.9(3) . . . . ? Pd1 C36 C37 Pd1 0.000(1) . . . . ? C35 Pd1 C37 C36 32.3(2) . . . . ? C36 Pd1 C37 C36 0.000(2) . . . . ? P2 Pd1 C37 C36 39.5(5) . . . . ? P1 Pd1 C37 C36 -141.9(2) . . . . ? C35 C36 C38 C40 -163.8(4) . . . . ? C37 C36 C38 C40 31.3(5) . . . . ? Pd1 C36 C38 C40 113.2(4) . . . . ? C35 C36 C38 C39 18.2(5) . . . . ? C37 C36 C38 C39 -146.7(4) . . . . ? Pd1 C36 C38 C39 -64.8(5) . . . . ? O2 C41 C42 F2' -170.7(35) . . . . ? O1 C41 C42 F2' 8.2(35) . . . . ? O2 C41 C42 F3' -40.2(39) . . . . ? O1 C41 C42 F3' 138.7(38) . . . . ? O2 C41 C42 F1 18.5(15) . . . . ? O1 C41 C42 F1 -162.6(14) . . . . ? O2 C41 C42 F1' 70.3(52) . . . . ? O1 C41 C42 F1' -110.8(52) . . . . ? O2 C41 C42 F3 -98.3(8) . . . . ? O1 C41 C42 F3 80.6(9) . . . . ? O2 C41 C42 F2 136.2(16) . . . . ? O1 C41 C42 F2 -44.9(17) . . . . ? _refine_diff_density_max 0.609 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.059