#_______________________________________________________________________ # # Requested by: Jessica Y. Wu, David C. Powers and Tobias Ritter # Harvard University # Department of Chemistry and Chemical Biology # 12 Oxford Street # Cambridge, MA 02138 # Tel: (617) 496-0750 # Fax: (617) 496-4591 # Email: ritter@chemistry.harvard.edu # # Crystallography by: Douglas M. Ho and Jessica Y. Wu # Harvard University # Department of Chemistry and Chemical Biology # 12 Oxford Street, B05-B06 # Cambridge, MA 02138 # Tel: (617) 495-0787 # Fax: (617) 496-8783 # Email: ho@chemistry.harvard.edu # # Comments: tr033 = Pd2(C2H3O2)4(C13H8N)2 . 2CH2Cl2 # = Bis(acetato)bis(\m~2~-acetato)- # bis(10-benzo[h]quinolato)- # dipalladium(III) Bis(dichloromethane) # Solvate at 193(2) K # # This compound crystallizes as dark red plates # (from dichloromethane at -40 \%C) in the # orthorhombic space group Pbca (No. 61) with 8 # formula units per unit cell. # # Version date: July 30, 2008 #_______________________________________________________________________ data_tr046 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(acetato)bis(\m~2~-acetato)-bis(10-benzo[h]quinolato)- dipalladium(III) bis(dichloromethane) solvate ; _chemical_name_common 'DCP-IV-15' _chemical_formula_iupac ; [Pd (C2 H3 O2)2 (C13 H8 N)]2 . 2(C H2 Cl2) ; _chemical_formula_moiety ; ((Pd 3+) (C2 H3 O2 1-)2 (C13 H8 N 1-))2, 2(C H2 Cl2) ; _chemical_formula_structural ; (Pd (C2 H3 O2)2 (C13 H8 N))2 2C H2 Cl2) ; _chemical_formula_analytical ? _chemical_formula_sum 'C36 H32 Cl4 N2 O8 Pd2' _chemical_formula_weight 975.24 _chemical_melting_point ? _chemical_compound_source 'chemical synthesis' 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' '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 'Orthorhombic' _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' _symmetry_Int_Tables_number 61 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 16.3668(4) _cell_length_b 17.4864(4) _cell_length_c 26.0050(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7442.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 3200 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 22.35 _exptl_crystal_description 'plate' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.125 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.010 _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 1.308 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.8536 _exptl_absorpt_correction_T_max 0.9870 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004)' _exptl_special_details ; The compound was crystallized from a dichloromethane solution at -40 \%C as dark red plates. A crystal 0.010 mm x 0.125 mm x 0.125 mm in size was selected, mounted on a nylon loop with Paratone-N oil, and transferred to a Bruker SMART APEX II diffractometer equipped with an Oxford Cryosystems 700 Series Cryostream Cooler and Mo K\a radiation (\l = 0.71073 \%A). A total of 694 frames were collected at 193(2) K to \q~max~ = 25.0\% with an oscillation range of 0.5\%/frame, and an exposure time of 90 s/frame using the APEX2 suite of software. (Bruker AXS, 2001a) Unit cell refinement on all observed reflections, and data reduction with corrections for Lp and decay were performed using SAINT. (Bruker AXS, 2006b) Scaling and a numerical absorption correction were done using SADABS. (Bruker AXS, 2004) The minimum and maximum transmission factors were 0.8536 and 0.9870, respectively. A total of 36560 reflections were collected, 6548 were unique (R~int~ = 0.102), and 4318 had I > 2\s(I). Systematic absences were consistent with the compound having crystallized in the orthorhombic space group Pbca (No. 61). The observed mean |E^2^-1| value was 0.958 (versus the expectation values of 0.968 and 0.736 for centric and noncentric data, respectively). ________________________________________________________________________ Bruker AXS (2004). SADABS. Bruker Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Bruker AXS (2006a). APEX2 v2.1-0. Bruker Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Bruker AXS (2006b). SAINT V7.34A. Bruker Analytical X-ray Systems Inc., Madison, Wisconsin, USA. ________________________________________________________________________ ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method '\w scans, 694 0.5\% rotations' _diffrn_detector_area_resol_mean 840 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 36560 _diffrn_reflns_av_R_equivalents 0.1022 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 6548 _reflns_number_gt 4318 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'APEX2 v2.1-0 (Bruker AXS, 2006a)' _computing_cell_refinement 'SAINT V7.34A (Bruker AXS, 2006b)' _computing_data_reduction ; SAINT V7.34A (Bruker AXS, 2006b), SADABS (Bruker AXS, 2004) ; _computing_structure_solution 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_structure_refinement 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_molecular_graphics 'SHELXTL v6.12 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL v6.12 (Bruker AXS, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. The structure was solved by direct methods and refined by full-matrix least-squares on F^2^ using SHELXTL. (Bruker AXS, 2001) The centrosymmetric unit was found to contain one molecule of Bis(acetato)bis(\m~2~-acetato)-bis(10-benzo[h]quinolato)- dipalladium(III) and two molecules of dichloromethane. All of the nonhydrogen atoms were refined with anisotropic displacement coefficients. All of the hydrogen atoms were assigned isotropic displacement coefficients U(H) = 1.2U(C) or 1.5U(C~methyl~), and their coordinates were allowed to ride on their respective carbons. The ligating atoms of the 10-benzo[h<\i>] quinolinato ligands exhibited signs of compositional disorder. This was treated with a two-site model [N(1), C(12)], [N(1'), C(12')] and [C(1), N(12)], [C(1'), N(12')] with refined site occupancy factors of 0.78(3) and 0.22(3), respectively. The dichloromethane molecules were disordered and were treated with three-site models, i.e., [C(1S), Cl(1), Cl(2)], [C(1S'), Cl(1'), Cl(2')], [C(1S"), Cl(1"), Cl(2")], [C(2S), Cl(3), Cl(4)], [C(2S'), Cl(3'), Cl(4')], [C(2S"), Cl(3"), Cl(4")] with fixed site occupancy factors of 0.763(4), 0.125(5), 0.112(4), 0.352(4), 0.29(4), and 0.36(3) based on population refinement tests and included in the least-squares refinement with 1,2-distance, 1,3-distance, rigid-bond, and similar U~ij~ restraints. The refinement converged to R(F) = 0.0428, wR(F^2^) = 0.0819, and S = 1.005 for 4318 reflections with I > 2\s(I), and R(F) = 0.0866, wR(F^2^) = 0.0969, and S = 1.005 for 6548 unique reflections, 582 parameters, and 444 restraints. The maximum |\D/\s| in the final cycle of least-squares was 0.002, and the residual peaks on the final difference-Fourier map ranged from -0.504 to 0.630 e\%A^-3^. Scattering factors were taken from the International Tables for Crystallography, Volume C. (Maslen et al., 1992, and Creagh & McAuley, 1992) ________________________________________________________________________ R(F ) = R1 = \S ||F~o~|-|F~c~|| / \S|F~o~|, wR(F ^2^) = wR2 = [ \S w (F~o~^2^-F~c~^2^)^2^ / \S w (F~o~^2^)^2^ ]^1/2^, and S = Goodness-of-fit on F ^2^ = [ \S w (F~o~^2^-F~c~^2^)^2^ / (n-p) ]^1/2^, where n is the number of reflections and p is the number of parameters refined. ________________________________________________________________________ Bruker AXS (2001). SHELXTL v6.12. Bruker Analytical X-ray Systems Inc., Madison, Wisconsin, USA. Creagh, D. C. & McAuley, W. J. (1992). International Tables for Crystallography: Mathematical, Physical and Chemical Tables, Vol C, edited by A. J. C. Wilson, pp. 206-222. Dordrecht, The Netherlands: Kluwer. Maslen, E. N., Fox, A. G. & O'Keefe, M. A. (1992). International Tables for Crystallography: Mathematical, Physical and Chemical Tables, Vol C, edited by A. J. C. Wilson, pp. 476-516. Dordrecht, The Netherlands: Kluwer. ________________________________________________________________________ ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+6.2541P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6548 _refine_ls_number_parameters 582 _refine_ls_number_restraints 444 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.630 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.111 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 Pd Pd 0.77382(2) 0.01123(2) 0.634193(15) 0.02457(12) Uani 1 1 d . . . Pd' Pd 0.90237(2) 0.09378(2) 0.622981(15) 0.02437(12) Uani 1 1 d . A . N1 N 0.7539(3) 0.0365(3) 0.70823(17) 0.0272(13) Uani 0.78(3) 1 d P A 1 C1 C 0.7539(3) 0.0365(3) 0.70823(17) 0.0272(13) Uani 0.22(3) 1 d P A 2 C2 C 0.7126(3) 0.0958(3) 0.7280(2) 0.0331(14) Uani 1 1 d . . . H2 H 0.6891 0.1325 0.7055 0.040 Uiso 1 1 calc R A 1 C3 C 0.7037(3) 0.1043(4) 0.7809(2) 0.0392(15) Uani 1 1 d . A . H3 H 0.6738 0.1465 0.7942 0.047 Uiso 1 1 calc R . . C4 C 0.7375(4) 0.0528(4) 0.8134(2) 0.0482(18) Uani 1 1 d . . . H4 H 0.7317 0.0593 0.8495 0.058 Uiso 1 1 calc R A . C5 C 0.7805(3) -0.0097(4) 0.7944(2) 0.0351(14) Uani 1 1 d . A . C6 C 0.8181(4) -0.0696(4) 0.8244(2) 0.0484(18) Uani 1 1 d . . . H6 H 0.8155 -0.0669 0.8609 0.058 Uiso 1 1 calc R A . C7 C 0.8567(4) -0.1293(4) 0.8024(3) 0.0465(17) Uani 1 1 d . A . H7 H 0.8804 -0.1676 0.8236 0.056 Uiso 1 1 calc R . . C8 C 0.8627(3) -0.1361(3) 0.7478(2) 0.0345(15) Uani 1 1 d . . . C9 C 0.8990(3) -0.1983(3) 0.7220(3) 0.0419(16) Uani 1 1 d . A . H9 H 0.9238 -0.2385 0.7409 0.050 Uiso 1 1 calc R . . C10 C 0.8980(4) -0.2002(4) 0.6699(3) 0.0454(16) Uani 1 1 d . . . H10 H 0.9213 -0.2431 0.6530 0.055 Uiso 1 1 calc R A . C11 C 0.8639(3) -0.1412(3) 0.6397(2) 0.0376(15) Uani 1 1 d . A . H11 H 0.8649 -0.1437 0.6032 0.045 Uiso 1 1 calc R B 1 C12 C 0.8297(3) -0.0805(3) 0.6643(2) 0.0269(14) Uani 0.78(3) 1 d P A 1 N12 N 0.8297(3) -0.0805(3) 0.6643(2) 0.0269(14) Uani 0.22(3) 1 d P A 2 C13 C 0.8282(3) -0.0786(3) 0.7173(2) 0.0293(13) Uani 1 1 d . A . C14 C 0.7875(3) -0.0159(3) 0.7410(2) 0.0299(13) Uani 1 1 d . . . N1' N 0.9724(3) 0.0363(2) 0.67329(18) 0.0262(12) Uani 0.78(3) 1 d P A 1 C1' C 0.9724(3) 0.0363(2) 0.67329(18) 0.0262(12) Uani 0.22(3) 1 d P A 2 C2' C 1.0193(3) -0.0253(3) 0.6631(2) 0.0324(14) Uani 1 1 d . . . H2' H 1.0223 -0.0455 0.6292 0.039 Uiso 1 1 calc R A 1 C3' C 1.0635(3) -0.0587(3) 0.7031(2) 0.0378(15) Uani 1 1 d . A . H3' H 1.0975 -0.1014 0.6959 0.045 Uiso 1 1 calc R . . C4' C 1.0591(3) -0.0316(3) 0.7524(2) 0.0366(15) Uani 1 1 d . . . H4' H 1.0879 -0.0566 0.7793 0.044 Uiso 1 1 calc R A . C5' C 1.0116(3) 0.0334(3) 0.7629(2) 0.0300(14) Uani 1 1 d . A . C6' C 1.0029(4) 0.0687(4) 0.8119(2) 0.0374(15) Uani 1 1 d . . . H6' H 1.0293 0.0468 0.8409 0.045 Uiso 1 1 calc R A . C7' C 0.9578(3) 0.1326(4) 0.8179(2) 0.0373(15) Uani 1 1 d . A . H7' H 0.9547 0.1555 0.8510 0.045 Uiso 1 1 calc R . . C8' C 0.9145(3) 0.1669(3) 0.7762(2) 0.0315(14) Uani 1 1 d . . . C9' C 0.8674(4) 0.2348(3) 0.7781(2) 0.0390(16) Uani 1 1 d . A . H9' H 0.8598 0.2605 0.8099 0.047 Uiso 1 1 calc R . . C10' C 0.8331(4) 0.2633(3) 0.7343(3) 0.0392(15) Uani 1 1 d . . . H10' H 0.8034 0.3100 0.7362 0.047 Uiso 1 1 calc R A . C11' C 0.8398(3) 0.2269(3) 0.6869(2) 0.0332(14) Uani 1 1 d . A . H11' H 0.8151 0.2483 0.6571 0.040 Uiso 1 1 calc R C 1 C12' C 0.8824(3) 0.1598(3) 0.68394(19) 0.0253(13) Uani 0.78(3) 1 d P A 1 N12' N 0.8824(3) 0.1598(3) 0.68394(19) 0.0253(13) Uani 0.22(3) 1 d P A 2 C13' C 0.9206(3) 0.1320(3) 0.7278(2) 0.0258(13) Uani 1 1 d . A . C14' C 0.9688(3) 0.0651(3) 0.7219(2) 0.0241(12) Uani 1 1 d . . . O1 O 0.6581(2) -0.0431(2) 0.63621(16) 0.0409(10) Uani 1 1 d . A . O2 O 0.6914(3) -0.1459(3) 0.5899(2) 0.0650(14) Uani 1 1 d . A . C15 C 0.6426(3) -0.1063(3) 0.6129(2) 0.0344(14) Uani 1 1 d . . . C16 C 0.5537(3) -0.1308(4) 0.6156(3) 0.0489(17) Uani 1 1 d . A . H16A H 0.5425 -0.1679 0.5882 0.073 Uiso 1 1 calc R . . H16B H 0.5185 -0.0859 0.6111 0.073 Uiso 1 1 calc R . . H16C H 0.5428 -0.1543 0.6491 0.073 Uiso 1 1 calc R . . O3 O 0.7123(2) 0.1089(2) 0.60674(14) 0.0348(10) Uani 1 1 d . A . O4 O 0.8289(2) 0.1571(2) 0.57579(14) 0.0317(9) Uani 1 1 d . . . C17 C 0.7514(4) 0.1547(3) 0.5790(2) 0.0321(13) Uani 1 1 d . A . C18 C 0.7059(4) 0.2097(4) 0.5457(2) 0.0490(18) Uani 1 1 d . . . H18A H 0.6471 0.2042 0.5517 0.074 Uiso 1 1 calc R A . H18B H 0.7181 0.1991 0.5095 0.074 Uiso 1 1 calc R . . H18C H 0.7228 0.2621 0.5541 0.074 Uiso 1 1 calc R . . O5 O 0.7967(2) -0.0187(2) 0.55965(14) 0.0340(9) Uani 1 1 d . A . O6 O 0.9270(2) 0.0186(2) 0.56103(14) 0.0335(9) Uani 1 1 d . . . C19 C 0.8673(3) -0.0131(3) 0.5398(2) 0.0303(13) Uani 1 1 d . A . C20 C 0.8785(4) -0.0473(4) 0.4878(3) 0.061(2) Uani 1 1 d . . . H20A H 0.9289 -0.0274 0.4724 0.092 Uiso 1 1 calc R A . H20B H 0.8319 -0.0340 0.4660 0.092 Uiso 1 1 calc R . . H20C H 0.8824 -0.1031 0.4909 0.092 Uiso 1 1 calc R . . O7 O 0.9990(2) 0.1582(2) 0.59152(15) 0.0406(10) Uani 1 1 d . . . O8 O 1.0600(3) 0.1993(2) 0.66331(17) 0.0495(12) Uani 1 1 d . . . C21 C 1.0563(3) 0.1940(3) 0.6166(2) 0.0310(13) Uani 1 1 d . A . C22 C 1.1177(4) 0.2328(4) 0.5831(3) 0.0518(18) Uani 1 1 d . . . H22A H 1.1092 0.2883 0.5844 0.078 Uiso 1 1 calc R A . H22B H 1.1114 0.2149 0.5476 0.078 Uiso 1 1 calc R . . H22C H 1.1729 0.2208 0.5953 0.078 Uiso 1 1 calc R . . C1S C 0.6326(11) -0.0463(5) 0.4902(3) 0.087(3) Uani 0.76 1 d PDU D 1 H1SA H 0.5817 -0.0689 0.5042 0.104 Uiso 0.76 1 calc PR D 1 H1SB H 0.6736 -0.0457 0.5182 0.104 Uiso 0.76 1 calc PR D 1 Cl1 Cl 0.6127(4) 0.0482(3) 0.4711(2) 0.1491(18) Uani 0.76 1 d PDU D 1 Cl2 Cl 0.6688(2) -0.1049(3) 0.43980(16) 0.1327(17) Uani 0.76 1 d PDU D 1 C1S' C 0.633(9) -0.039(5) 0.5012(18) 0.132(9) Uani 0.13 1 d PDU E 2 H1SC H 0.6921 -0.0321 0.5089 0.158 Uiso 0.13 1 calc PR E 2 H1SD H 0.6128 -0.0813 0.5230 0.158 Uiso 0.13 1 calc PR E 2 Cl1' Cl 0.5804(18) 0.0455(19) 0.5170(12) 0.165(8) Uani 0.13 1 d PDU E 2 Cl2' Cl 0.622(2) -0.064(2) 0.4360(12) 0.162(9) Uani 0.13 1 d PDU E 2 C1S" C 0.584(3) 0.010(3) 0.445(4) 0.129(9) Uani 0.11 1 d PDU F 3 H1SE H 0.5423 0.0467 0.4575 0.155 Uiso 0.11 1 calc PR F 3 H1SF H 0.5819 0.0093 0.4072 0.155 Uiso 0.11 1 calc PR F 3 Cl1" Cl 0.6813(19) 0.0426(18) 0.4646(11) 0.133(8) Uani 0.11 1 d PDU F 3 Cl2" Cl 0.561(2) -0.082(2) 0.4687(14) 0.174(9) Uani 0.11 1 d PDU F 3 C2S C 0.5757(16) -0.3300(17) 0.4706(10) 0.109(7) Uani 0.35 1 d PDU G 1 H2SA H 0.5449 -0.3786 0.4729 0.131 Uiso 0.35 1 calc PR G 1 H2SB H 0.6002 -0.3196 0.5047 0.131 Uiso 0.35 1 calc PR G 1 Cl3 Cl 0.6542(11) -0.3398(18) 0.4247(9) 0.107(5) Uani 0.35 1 d PDU G 1 Cl4 Cl 0.5078(12) -0.2556(13) 0.4548(8) 0.101(7) Uani 0.35 1 d PDU G 1 C2S' C 0.593(3) -0.283(3) 0.4813(13) 0.111(8) Uani 0.29 1 d PDU H 2 H2SC H 0.5745 -0.3185 0.5085 0.133 Uiso 0.29 1 calc PR H 2 H2SD H 0.6380 -0.2516 0.4953 0.133 Uiso 0.29 1 calc PR H 2 Cl3' Cl 0.6279(12) -0.3353(19) 0.4279(14) 0.123(6) Uani 0.29 1 d PDU H 2 Cl4' Cl 0.5109(16) -0.2218(13) 0.4649(11) 0.112(6) Uani 0.29 1 d PDU H 2 C2S" C 0.5945(19) -0.307(3) 0.4756(8) 0.101(7) Uani 0.36 1 d PDU I 3 H2SE H 0.5762 -0.3397 0.5043 0.121 Uiso 0.36 1 calc PR I 3 H2SF H 0.6188 -0.2597 0.4904 0.121 Uiso 0.36 1 calc PR I 3 Cl3" Cl 0.6688(12) -0.3555(17) 0.4389(7) 0.133(6) Uani 0.36 1 d PDU I 3 Cl4" Cl 0.5102(11) -0.2823(11) 0.4369(5) 0.115(5) Uani 0.36 1 d PDU I 3 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 Pd 0.0200(2) 0.0252(2) 0.0285(2) -0.00018(19) 0.00069(19) 0.00098(18) Pd' 0.0209(2) 0.0241(2) 0.0281(2) 0.00062(19) -0.00063(19) -0.00089(18) N1 0.021(3) 0.027(3) 0.033(3) 0.000(2) -0.001(2) -0.003(2) C1 0.021(3) 0.027(3) 0.033(3) 0.000(2) -0.001(2) -0.003(2) C2 0.023(3) 0.033(3) 0.043(4) 0.003(3) 0.003(3) -0.004(3) C3 0.034(3) 0.043(4) 0.040(4) -0.006(3) 0.010(3) -0.005(3) C4 0.046(4) 0.063(5) 0.035(4) -0.015(4) 0.007(3) -0.017(4) C5 0.031(3) 0.044(4) 0.031(3) 0.000(3) -0.001(3) -0.012(3) C6 0.047(4) 0.062(5) 0.037(4) 0.017(4) -0.009(3) -0.019(4) C7 0.040(4) 0.049(4) 0.050(4) 0.020(4) -0.014(3) -0.004(3) C8 0.023(3) 0.027(3) 0.054(4) 0.007(3) -0.008(3) -0.008(3) C9 0.032(3) 0.028(3) 0.065(5) 0.009(3) -0.013(3) 0.004(3) C10 0.038(4) 0.035(4) 0.063(5) -0.002(3) -0.004(4) 0.006(3) C11 0.029(3) 0.032(3) 0.052(4) -0.001(3) 0.000(3) 0.000(3) C12 0.019(3) 0.022(3) 0.040(3) 0.008(3) -0.001(2) 0.000(2) N12 0.019(3) 0.022(3) 0.040(3) 0.008(3) -0.001(2) 0.000(2) C13 0.016(3) 0.030(3) 0.042(4) 0.005(3) -0.005(2) -0.006(2) C14 0.019(3) 0.031(3) 0.039(3) 0.002(3) -0.002(2) -0.007(3) N1' 0.021(3) 0.022(3) 0.036(3) 0.001(2) -0.001(2) -0.003(2) C1' 0.021(3) 0.022(3) 0.036(3) 0.001(2) -0.001(2) -0.003(2) C2' 0.022(3) 0.032(3) 0.044(4) -0.001(3) -0.003(3) 0.002(3) C3' 0.024(3) 0.026(3) 0.063(5) -0.002(3) -0.006(3) 0.002(3) C4' 0.027(3) 0.035(4) 0.047(4) 0.012(3) -0.014(3) -0.007(3) C5' 0.021(3) 0.029(3) 0.041(4) 0.000(3) -0.006(3) -0.006(3) C6' 0.036(3) 0.043(4) 0.034(4) 0.004(3) -0.011(3) -0.011(3) C7' 0.041(4) 0.049(4) 0.023(3) -0.002(3) 0.001(3) -0.015(3) C8' 0.028(3) 0.032(3) 0.035(3) -0.006(3) 0.005(3) -0.013(3) C9' 0.040(4) 0.035(4) 0.042(4) -0.016(3) 0.007(3) -0.012(3) C10' 0.034(3) 0.025(3) 0.059(4) -0.010(3) 0.002(3) -0.001(3) C11' 0.029(3) 0.024(3) 0.046(4) 0.000(3) 0.001(3) 0.001(3) C12' 0.019(3) 0.024(3) 0.033(3) 0.000(2) 0.002(2) -0.003(2) N12' 0.019(3) 0.024(3) 0.033(3) 0.000(2) 0.002(2) -0.003(2) C13' 0.020(3) 0.028(3) 0.030(3) 0.002(3) 0.003(2) -0.005(2) C14' 0.021(3) 0.020(3) 0.031(3) -0.002(2) -0.004(2) -0.008(2) O1 0.029(2) 0.042(2) 0.052(3) -0.007(2) 0.004(2) -0.0089(19) O2 0.054(3) 0.046(3) 0.096(4) -0.020(3) 0.020(3) -0.008(2) C15 0.033(3) 0.033(4) 0.037(4) 0.003(3) 0.003(3) -0.002(3) C16 0.040(4) 0.046(4) 0.060(5) -0.005(4) 0.003(3) -0.016(3) O3 0.023(2) 0.042(2) 0.040(2) 0.004(2) -0.0010(17) 0.0069(18) O4 0.028(2) 0.034(2) 0.033(2) 0.0056(18) -0.0034(18) 0.0011(19) C17 0.033(3) 0.034(3) 0.029(3) -0.001(3) -0.008(3) 0.005(3) C18 0.048(4) 0.045(4) 0.054(4) 0.007(4) -0.019(3) 0.010(3) O5 0.032(2) 0.036(2) 0.034(2) -0.0039(19) 0.0010(18) -0.0049(19) O6 0.024(2) 0.039(2) 0.037(2) -0.0121(19) 0.0039(17) -0.0036(18) C19 0.032(3) 0.026(3) 0.032(3) -0.003(3) 0.002(3) 0.005(3) C20 0.051(4) 0.076(5) 0.057(5) -0.034(4) 0.009(4) -0.019(4) O7 0.039(2) 0.045(3) 0.039(2) -0.001(2) 0.003(2) -0.015(2) O8 0.045(3) 0.057(3) 0.047(3) 0.006(2) -0.010(2) -0.017(2) C21 0.031(3) 0.023(3) 0.039(4) -0.004(3) -0.004(3) 0.001(3) C22 0.051(4) 0.047(4) 0.056(4) -0.016(4) 0.012(3) -0.018(3) C1S 0.063(6) 0.145(8) 0.052(6) 0.033(6) -0.022(6) -0.028(6) Cl1 0.160(5) 0.156(4) 0.132(4) 0.056(3) -0.038(4) -0.011(4) Cl2 0.097(3) 0.208(5) 0.092(3) -0.023(3) -0.007(2) -0.047(3) C1S' 0.109(17) 0.194(16) 0.093(14) 0.030(16) -0.029(17) -0.053(15) Cl1' 0.146(17) 0.204(18) 0.145(16) -0.004(15) -0.057(16) -0.052(14) Cl2' 0.149(19) 0.23(2) 0.106(13) 0.010(14) -0.039(15) -0.043(17) C1S" 0.112(15) 0.190(16) 0.086(17) 0.006(16) -0.023(16) -0.029(16) Cl1" 0.116(14) 0.197(18) 0.085(14) 0.013(14) -0.042(14) -0.016(14) Cl2" 0.175(18) 0.211(17) 0.138(17) 0.021(16) 0.004(17) -0.046(15) C2S 0.067(12) 0.192(17) 0.068(12) 0.048(14) -0.009(9) -0.008(12) Cl3 0.049(9) 0.200(12) 0.072(9) 0.023(8) -0.020(7) -0.003(8) Cl4 0.058(6) 0.192(19) 0.053(10) 0.013(12) -0.022(7) -0.008(11) C2S' 0.071(13) 0.193(19) 0.068(12) 0.039(13) -0.019(12) -0.022(13) Cl3' 0.098(15) 0.163(12) 0.107(10) 0.011(9) -0.022(13) -0.024(12) Cl4' 0.070(6) 0.185(16) 0.082(13) 0.017(11) -0.016(7) -0.028(10) C2S" 0.051(11) 0.188(18) 0.064(12) 0.051(13) -0.017(8) 0.006(12) Cl3" 0.090(9) 0.231(16) 0.077(10) -0.014(10) -0.015(8) 0.011(8) Cl4" 0.081(6) 0.176(13) 0.086(10) 0.050(9) -0.050(7) -0.021(7) _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 Pd N1 2.002(5) . ? Pd C12 2.006(5) . ? Pd O5 2.042(4) . ? Pd O3 2.108(4) . ? Pd O1 2.120(4) . ? Pd Pd' 2.5681(5) . ? Pd' C12' 1.988(5) . ? Pd' N1' 2.009(4) . ? Pd' O4 2.043(4) . ? Pd' O7 2.107(4) . ? Pd' O6 2.118(4) . ? N1 C2 1.340(7) . ? N1 C14 1.367(7) . ? C2 C3 1.391(8) . ? C2 H2 0.9500 . ? C3 C4 1.355(9) . ? C3 H3 0.9500 . ? C4 C5 1.391(8) . ? C4 H4 0.9500 . ? C5 C14 1.398(8) . ? C5 C6 1.444(8) . ? C6 C7 1.349(9) . ? C6 H6 0.9500 . ? C7 C8 1.427(8) . ? C7 H7 0.9500 . ? C8 C13 1.401(7) . ? C8 C9 1.409(8) . ? C9 C10 1.356(8) . ? C9 H9 0.9500 . ? C10 C11 1.411(8) . ? C10 H10 0.9500 . ? C11 C12 1.360(7) . ? C11 H11 0.9500 . ? C12 C13 1.379(7) . ? C13 C14 1.422(8) . ? N1' C2' 1.349(7) . ? N1' C14' 1.361(7) . ? C2' C3' 1.394(8) . ? C2' H2' 0.9500 . ? C3' C4' 1.371(8) . ? C3' H3' 0.9500 . ? C4' C5' 1.402(8) . ? C4' H4' 0.9500 . ? C5' C14' 1.391(7) . ? C5' C6' 1.423(8) . ? C6' C7' 1.348(8) . ? C6' H6' 0.9500 . ? C7' C8' 1.429(8) . ? C7' H7' 0.9500 . ? C8' C13' 1.402(7) . ? C8' C9' 1.416(8) . ? C9' C10' 1.365(8) . ? C9' H9' 0.9500 . ? C10' C11' 1.392(8) . ? C10' H10' 0.9500 . ? C11' C12' 1.367(7) . ? C11' H11' 0.9500 . ? C12' C13' 1.387(7) . ? C13' C14' 1.421(7) . ? O1 C15 1.285(7) . ? O2 C15 1.215(7) . ? C15 C16 1.517(7) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? O3 C17 1.253(6) . ? O4 C17 1.272(6) . ? C17 C18 1.493(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O5 C19 1.269(6) . ? O6 C19 1.252(6) . ? C19 C20 1.490(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O7 C21 1.303(6) . ? O8 C21 1.219(6) . ? C21 C22 1.495(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C1S Cl1 1.756(7) . ? C1S Cl2 1.765(6) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C1S' Cl2' 1.761(7) . ? C1S' Cl1' 1.761(7) . ? C1S' H1SC 0.9900 . ? C1S' H1SD 0.9900 . ? C1S" Cl2" 1.759(7) . ? C1S" Cl1" 1.762(7) . ? C1S" H1SE 0.9900 . ? C1S" H1SF 0.9900 . ? C2S Cl4 1.760(7) . ? C2S Cl3 1.762(7) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C2S' Cl4' 1.760(7) . ? C2S' Cl3' 1.764(7) . ? C2S' H2SC 0.9900 . ? C2S' H2SD 0.9900 . ? C2S" Cl4" 1.761(7) . ? C2S" Cl3" 1.764(7) . ? C2S" H2SE 0.9900 . ? C2S" H2SF 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 N1 Pd C12 82.8(2) . . ? N1 Pd O5 177.54(17) . . ? C12 Pd O5 94.74(19) . . ? N1 Pd O3 93.96(17) . . ? C12 Pd O3 176.69(18) . . ? O5 Pd O3 88.49(15) . . ? N1 Pd O1 85.97(16) . . ? C12 Pd O1 92.24(17) . . ? O5 Pd O1 94.14(15) . . ? O3 Pd O1 86.83(15) . . ? N1 Pd Pd' 96.80(12) . . ? C12 Pd Pd' 96.93(14) . . ? O5 Pd Pd' 83.48(10) . . ? O3 Pd Pd' 84.11(10) . . ? O1 Pd Pd' 170.68(11) . . ? C12' Pd' N1' 82.25(19) . . ? C12' Pd' O4 93.89(18) . . ? N1' Pd' O4 176.13(17) . . ? C12' Pd' O7 97.03(17) . . ? N1' Pd' O7 95.29(16) . . ? O4 Pd' O7 85.35(15) . . ? C12' Pd' O6 176.55(18) . . ? N1' Pd' O6 94.36(17) . . ? O4 Pd' O6 89.50(15) . . ? O7 Pd' O6 83.89(15) . . ? C12' Pd' Pd 95.83(13) . . ? N1' Pd' Pd 96.42(12) . . ? O4 Pd' Pd 83.73(10) . . ? O7 Pd' Pd 163.64(11) . . ? O6 Pd' Pd 83.87(10) . . ? C2 N1 C14 118.9(5) . . ? C2 N1 Pd 128.4(4) . . ? C14 N1 Pd 112.7(4) . . ? N1 C2 C3 121.0(6) . . ? N1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 120.3(6) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.5(6) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C14 117.1(6) . . ? C4 C5 C6 126.4(6) . . ? C14 C5 C6 116.5(6) . . ? C7 C6 C5 122.1(6) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 C7 C8 121.3(6) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C13 C8 C9 117.0(6) . . ? C13 C8 C7 118.4(6) . . ? C9 C8 C7 124.5(6) . . ? C10 C9 C8 119.3(6) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 122.9(6) . . ? C9 C10 H10 118.5 . . ? C11 C10 H10 118.5 . . ? C12 C11 C10 118.1(6) . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? C11 C12 C13 119.8(5) . . ? C11 C12 Pd 128.9(4) . . ? C13 C12 Pd 111.3(4) . . ? C12 C13 C8 122.8(5) . . ? C12 C13 C14 117.4(5) . . ? C8 C13 C14 119.8(5) . . ? N1 C14 C5 122.3(5) . . ? N1 C14 C13 115.8(5) . . ? C5 C14 C13 121.9(5) . . ? C2' N1' C14' 120.1(5) . . ? C2' N1' Pd' 126.6(4) . . ? C14' N1' Pd' 113.3(3) . . ? N1' C2' C3' 118.9(5) . . ? N1' C2' H2' 120.6 . . ? C3' C2' H2' 120.6 . . ? C4' C3' C2' 121.7(6) . . ? C4' C3' H3' 119.1 . . ? C2' C3' H3' 119.1 . . ? C3' C4' C5' 119.4(5) . . ? C3' C4' H4' 120.3 . . ? C5' C4' H4' 120.3 . . ? C14' C5' C4' 117.0(5) . . ? C14' C5' C6' 117.6(5) . . ? C4' C5' C6' 125.5(6) . . ? C7' C6' C5' 121.3(6) . . ? C7' C6' H6' 119.4 . . ? C5' C6' H6' 119.4 . . ? C6' C7' C8' 122.1(5) . . ? C6' C7' H7' 118.9 . . ? C8' C7' H7' 118.9 . . ? C13' C8' C9' 115.8(5) . . ? C13' C8' C7' 117.6(5) . . ? C9' C8' C7' 126.5(5) . . ? C10' C9' C8' 120.0(6) . . ? C10' C9' H9' 120.0 . . ? C8' C9' H9' 120.0 . . ? C9' C10' C11' 122.6(6) . . ? C9' C10' H10' 118.7 . . ? C11' C10' H10' 118.7 . . ? C12' C11' C10' 118.9(6) . . ? C12' C11' H11' 120.6 . . ? C10' C11' H11' 120.6 . . ? C11' C12' C13' 119.0(5) . . ? C11' C12' Pd' 128.8(4) . . ? C13' C12' Pd' 112.2(4) . . ? C12' C13' C8' 123.6(5) . . ? C12' C13' C14' 116.8(5) . . ? C8' C13' C14' 119.7(5) . . ? N1' C14' C5' 122.9(5) . . ? N1' C14' C13' 115.4(5) . . ? C5' C14' C13' 121.7(5) . . ? C15 O1 Pd 123.4(4) . . ? O2 C15 O1 126.3(5) . . ? O2 C15 C16 119.4(6) . . ? O1 C15 C16 114.3(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C17 O3 Pd 117.9(3) . . ? C17 O4 Pd' 122.0(4) . . ? O3 C17 O4 124.6(5) . . ? O3 C17 C18 119.4(5) . . ? O4 C17 C18 116.0(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C19 O5 Pd 122.2(3) . . ? C19 O6 Pd' 117.5(3) . . ? O6 C19 O5 124.5(5) . . ? O6 C19 C20 118.7(5) . . ? O5 C19 C20 116.8(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C21 O7 Pd' 127.0(4) . . ? O8 C21 O7 124.9(5) . . ? O8 C21 C22 120.8(5) . . ? O7 C21 C22 114.2(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Cl1 C1S Cl2 113.5(6) . . ? Cl1 C1S H1SA 108.9 . . ? Cl2 C1S H1SA 108.9 . . ? Cl1 C1S H1SB 108.9 . . ? Cl2 C1S H1SB 108.9 . . ? H1SA C1S H1SB 107.7 . . ? Cl2' C1S' Cl1' 112.6(9) . . ? Cl2' C1S' H1SC 109.1 . . ? Cl1' C1S' H1SC 109.1 . . ? Cl2' C1S' H1SD 109.1 . . ? Cl1' C1S' H1SD 109.1 . . ? H1SC C1S' H1SD 107.8 . . ? Cl2" C1S" Cl1" 112.9(9) . . ? Cl2" C1S" H1SE 109.0 . . ? Cl1" C1S" H1SE 109.0 . . ? Cl2" C1S" H1SF 109.0 . . ? Cl1" C1S" H1SF 109.0 . . ? H1SE C1S" H1SF 107.8 . . ? Cl4 C2S Cl3 112.0(8) . . ? Cl4 C2S H2SA 109.2 . . ? Cl3 C2S H2SA 109.2 . . ? Cl4 C2S H2SB 109.2 . . ? Cl3 C2S H2SB 109.2 . . ? H2SA C2S H2SB 107.9 . . ? Cl4' C2S' Cl3' 111.9(8) . . ? Cl4' C2S' H2SC 109.2 . . ? Cl3' C2S' H2SC 109.2 . . ? Cl4' C2S' H2SD 109.2 . . ? Cl3' C2S' H2SD 109.2 . . ? H2SC C2S' H2SD 107.9 . . ? Cl4" C2S" Cl3" 110.4(8) . . ? Cl4" C2S" H2SE 109.6 . . ? Cl3" C2S" H2SE 109.6 . . ? Cl4" C2S" H2SF 109.6 . . ? Cl3" C2S" H2SF 109.6 . . ? H2SE C2S" H2SF 108.1 . . ? 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 N1 Pd Pd' C12' -19.07(19) . . . . ? C12 Pd Pd' C12' -102.6(2) . . . . ? O5 Pd Pd' C12' 163.39(18) . . . . ? O3 Pd Pd' C12' 74.23(18) . . . . ? N1 Pd Pd' N1' 63.75(19) . . . . ? C12 Pd Pd' N1' -19.8(2) . . . . ? O5 Pd Pd' N1' -113.79(17) . . . . ? O3 Pd Pd' N1' 157.05(17) . . . . ? N1 Pd Pd' O4 -112.36(17) . . . . ? C12 Pd Pd' O4 164.11(19) . . . . ? O5 Pd Pd' O4 70.10(15) . . . . ? O3 Pd Pd' O4 -19.05(15) . . . . ? N1 Pd Pd' O7 -160.8(4) . . . . ? C12 Pd Pd' O7 115.7(4) . . . . ? O5 Pd Pd' O7 21.7(4) . . . . ? O3 Pd Pd' O7 -67.5(4) . . . . ? N1 Pd Pd' O6 157.47(17) . . . . ? C12 Pd Pd' O6 73.94(19) . . . . ? O5 Pd Pd' O6 -20.07(15) . . . . ? O3 Pd Pd' O6 -109.22(14) . . . . ? C12 Pd N1 C2 -177.6(5) . . . . ? O3 Pd N1 C2 1.7(5) . . . . ? O1 Pd N1 C2 -84.9(5) . . . . ? Pd' Pd N1 C2 86.2(4) . . . . ? C12 Pd N1 C14 1.6(4) . . . . ? O3 Pd N1 C14 -179.1(3) . . . . ? O1 Pd N1 C14 94.4(4) . . . . ? Pd' Pd N1 C14 -94.6(3) . . . . ? C14 N1 C2 C3 0.0(8) . . . . ? Pd N1 C2 C3 179.2(4) . . . . ? N1 C2 C3 C4 0.5(8) . . . . ? C2 C3 C4 C5 -0.8(9) . . . . ? C3 C4 C5 C14 0.5(8) . . . . ? C3 C4 C5 C6 -178.7(6) . . . . ? C4 C5 C6 C7 178.0(6) . . . . ? C14 C5 C6 C7 -1.2(9) . . . . ? C5 C6 C7 C8 0.3(9) . . . . ? C6 C7 C8 C13 0.7(9) . . . . ? C6 C7 C8 C9 -177.2(6) . . . . ? C13 C8 C9 C10 -0.8(8) . . . . ? C7 C8 C9 C10 177.1(6) . . . . ? C8 C9 C10 C11 1.7(9) . . . . ? C9 C10 C11 C12 -1.0(9) . . . . ? C10 C11 C12 C13 -0.7(8) . . . . ? C10 C11 C12 Pd -178.4(4) . . . . ? N1 Pd C12 C11 176.1(5) . . . . ? O5 Pd C12 C11 -3.9(5) . . . . ? O1 Pd C12 C11 90.5(5) . . . . ? Pd' Pd C12 C11 -87.9(5) . . . . ? N1 Pd C12 C13 -1.7(4) . . . . ? O5 Pd C12 C13 178.3(4) . . . . ? O1 Pd C12 C13 -87.3(4) . . . . ? Pd' Pd C12 C13 94.3(3) . . . . ? C11 C12 C13 C8 1.7(8) . . . . ? Pd C12 C13 C8 179.7(4) . . . . ? C11 C12 C13 C14 -176.5(5) . . . . ? Pd C12 C13 C14 1.5(6) . . . . ? C9 C8 C13 C12 -0.9(8) . . . . ? C7 C8 C13 C12 -179.0(5) . . . . ? C9 C8 C13 C14 177.2(5) . . . . ? C7 C8 C13 C14 -0.9(8) . . . . ? C2 N1 C14 C5 -0.3(8) . . . . ? Pd N1 C14 C5 -179.6(4) . . . . ? C2 N1 C14 C13 178.1(5) . . . . ? Pd N1 C14 C13 -1.2(6) . . . . ? C4 C5 C14 N1 0.0(8) . . . . ? C6 C5 C14 N1 179.3(5) . . . . ? C4 C5 C14 C13 -178.3(5) . . . . ? C6 C5 C14 C13 1.0(8) . . . . ? C12 C13 C14 N1 -0.2(7) . . . . ? C8 C13 C14 N1 -178.4(5) . . . . ? C12 C13 C14 C5 178.2(5) . . . . ? C8 C13 C14 C5 0.0(8) . . . . ? C12' Pd' N1' C2' -176.8(4) . . . . ? O7 Pd' N1' C2' -80.4(4) . . . . ? O6 Pd' N1' C2' 3.8(4) . . . . ? Pd Pd' N1' C2' 88.1(4) . . . . ? C12' Pd' N1' C14' 3.6(3) . . . . ? O7 Pd' N1' C14' 100.0(4) . . . . ? O6 Pd' N1' C14' -175.8(3) . . . . ? Pd Pd' N1' C14' -91.5(3) . . . . ? C14' N1' C2' C3' 0.3(7) . . . . ? Pd' N1' C2' C3' -179.3(4) . . . . ? N1' C2' C3' C4' 1.3(8) . . . . ? C2' C3' C4' C5' -2.7(9) . . . . ? C3' C4' C5' C14' 2.4(8) . . . . ? C3' C4' C5' C6' -178.6(5) . . . . ? C14' C5' C6' C7' -3.0(8) . . . . ? C4' C5' C6' C7' 177.9(5) . . . . ? C5' C6' C7' C8' 2.0(8) . . . . ? C6' C7' C8' C13' -0.4(8) . . . . ? C6' C7' C8' C9' -178.2(6) . . . . ? C13' C8' C9' C10' -1.6(8) . . . . ? C7' C8' C9' C10' 176.3(5) . . . . ? C8' C9' C10' C11' 2.3(9) . . . . ? C9' C10' C11' C12' 0.0(9) . . . . ? C10' C11' C12' C13' -2.7(8) . . . . ? C10' C11' C12' Pd' 179.4(4) . . . . ? N1' Pd' C12' C11' 174.8(5) . . . . ? O4 Pd' C12' C11' -5.5(5) . . . . ? O7 Pd' C12' C11' 80.3(5) . . . . ? Pd Pd' C12' C11' -89.5(5) . . . . ? N1' Pd' C12' C13' -3.2(3) . . . . ? O4 Pd' C12' C13' 176.6(3) . . . . ? O7 Pd' C12' C13' -97.6(4) . . . . ? Pd Pd' C12' C13' 92.5(3) . . . . ? C11' C12' C13' C8' 3.4(8) . . . . ? Pd' C12' C13' C8' -178.4(4) . . . . ? C11' C12' C13' C14' -175.7(5) . . . . ? Pd' C12' C13' C14' 2.5(6) . . . . ? C9' C8' C13' C12' -1.2(8) . . . . ? C7' C8' C13' C12' -179.3(5) . . . . ? C9' C8' C13' C14' 177.9(5) . . . . ? C7' C8' C13' C14' -0.1(7) . . . . ? C2' N1' C14' C5' -0.5(7) . . . . ? Pd' N1' C14' C5' 179.1(4) . . . . ? C2' N1' C14' C13' 177.1(4) . . . . ? Pd' N1' C14' C13' -3.2(5) . . . . ? C4' C5' C14' N1' -0.9(8) . . . . ? C6' C5' C14' N1' -180.0(5) . . . . ? C4' C5' C14' C13' -178.3(5) . . . . ? C6' C5' C14' C13' 2.6(7) . . . . ? C12' C13' C14' N1' 0.5(7) . . . . ? C8' C13' C14' N1' -178.7(5) . . . . ? C12' C13' C14' C5' 178.2(5) . . . . ? C8' C13' C14' C5' -1.0(7) . . . . ? N1 Pd O1 C15 -141.2(4) . . . . ? C12 Pd O1 C15 -58.6(5) . . . . ? O5 Pd O1 C15 36.3(4) . . . . ? O3 Pd O1 C15 124.6(4) . . . . ? Pd O1 C15 O2 5.0(9) . . . . ? Pd O1 C15 C16 -174.6(4) . . . . ? N1 Pd O3 C17 121.8(4) . . . . ? O5 Pd O3 C17 -58.3(4) . . . . ? O1 Pd O3 C17 -152.5(4) . . . . ? Pd' Pd O3 C17 25.3(4) . . . . ? C12' Pd' O4 C17 -74.1(4) . . . . ? O7 Pd' O4 C17 -170.8(4) . . . . ? O6 Pd' O4 C17 105.3(4) . . . . ? Pd Pd' O4 C17 21.4(4) . . . . ? Pd O3 C17 O4 -17.5(7) . . . . ? Pd O3 C17 C18 160.9(4) . . . . ? Pd' O4 C17 O3 -7.6(8) . . . . ? Pd' O4 C17 C18 174.0(4) . . . . ? C12 Pd O5 C19 -73.6(4) . . . . ? O3 Pd O5 C19 107.1(4) . . . . ? O1 Pd O5 C19 -166.2(4) . . . . ? Pd' Pd O5 C19 22.8(4) . . . . ? N1' Pd' O6 C19 122.6(4) . . . . ? O4 Pd' O6 C19 -57.2(4) . . . . ? O7 Pd' O6 C19 -142.6(4) . . . . ? Pd Pd' O6 C19 26.6(4) . . . . ? Pd' O6 C19 O5 -18.1(7) . . . . ? Pd' O6 C19 C20 162.3(5) . . . . ? Pd O5 C19 O6 -8.4(8) . . . . ? Pd O5 C19 C20 171.3(4) . . . . ? C12' Pd' O7 C21 36.8(4) . . . . ? N1' Pd' O7 C21 -46.0(4) . . . . ? O4 Pd' O7 C21 130.2(4) . . . . ? O6 Pd' O7 C21 -139.8(4) . . . . ? Pd Pd' O7 C21 178.4(3) . . . . ? Pd' O7 C21 O8 -4.6(8) . . . . ? Pd' O7 C21 C22 178.3(4) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.060 0 -1 0 0.070 0 0 1 0.005 0 0 -1 0.005 1 1 0 0.062 1 -1 0 0.068 -3 1 0 0.070 -3 -2 0 0.058