#_______________________________________________________________________ # # 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 = Pd3(C2H3O2)3(C13H8N)2Cl # = Tris(\m~2~-acetato)- # bis(benzo[h<\i>]quinolato)- # (\m~2~-chloro)tripalladium(II) at 193(2) K # # This compound crystallizes as orange plates # (from dichloromethane / diethyl ether) in the # triclinic space group P-1 (No. 2) with 2 # formula units per unit cell. # # Version date: July 3, 2008 #_______________________________________________________________________ data_tr033 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tris(\m~2~-acetato)-bis(benzo[h<\i>]quinolato)-(\m~2~-chloro)- tripalladium(II) ; _chemical_name_common 'DCP2' _chemical_formula_iupac '[Pd3 (C2 H3 O2)3 (C13 H8 N)2 Cl]' _chemical_formula_moiety 'C32 H25 Cl N2 O6 Pd3' _chemical_formula_structural ; ((Pd (C2 H3 O2)2 (C13 H8 N)) (Pd (C2 H3 O2) (C13 H8 N) Cl)) Pd ; _chemical_formula_analytical ? _chemical_formula_sum 'C32 H25 Cl N2 O6 Pd3' _chemical_formula_weight 888.19 _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 'Triclinic' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0632(2) _cell_length_b 11.2475(2) _cell_length_c 13.9230(2) _cell_angle_alpha 96.989(1) _cell_angle_beta 95.423(1) _cell_angle_gamma 108.992(1) _cell_volume 1463.85(5) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 13725 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 30.02 _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 2.015 _exptl_crystal_density_method 'not measured' _exptl_crystal_density_meas ? _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 1.964 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.7571 _exptl_absorpt_correction_T_max 0.9434 _exptl_absorpt_process_details 'SADABS (Bruker AXS, 2004)' _exptl_special_details ; The compound was crystallized from a dichloromethane / diethyl ether solution as orange plates. A crystal 0.030 mm x 0.095 mm x 0.150 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 2580 frames were collected at 193(2) K to \q~max~ = 30.0\% with an oscillation range of 0.5\%/frame, and an exposure time of 30 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 0.7571 and 0.9434, respectively. A total of 36302 reflections were collected, 8529 were unique (R~int~ = 0.029), and 7147 had I > 2\s(I). A lack of systematic absences were consistent with the compound having crystallized in the triclinic space group P1 or P-1. The latter centrosymmetric space group P-1 (No. 2) was selected based on an observed mean |E^2^-1| value of 0.924 (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 'Mo K\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, 2580 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 36302 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 30.00 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _reflns_number_total 8529 _reflns_number_gt 7147 _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 tris (\m~2~-acetato)-bis(benzo[h<\i>]quinolato)-(\m~2~-chloro)- tripalladium(II). All of the nonhydrogen atoms were refined with anisotropic displacement coefficients. 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. During refinement, a residual peak was observed between the oxygen atoms of one of the bridging acetato ligands (O5, O6), so attempts were made to treat that bridging site as compositionally disordered (i.e. partially occupied by an acetate and by a chloride). However, even with restraints, this model yielded Pd-Cl distances that were too long and a miniscule Cl site occupancy factor of 0.036(4). Therefore, the residual peak was left unassigned and the refinement was completed with all atoms fully occupied. The refinement converged to R(F) = 0.0369, wR(F^2^) = 0.0792, and S = 1.091 for 7147 reflections with I > 2\s(I), and R(F) = 0.0479, wR(F^2^) = 0.0834, and S = 1.091 for 8529 unique reflections and 400 parameters. The maximum |\D/\s| in the final cycle of least-squares was less than 0.001, and the residual peaks on the final difference-Fourier map ranged from -1.375 to 1.876 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^)+(0.0279P)^2^+3.3960P] 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 8529 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.876 _refine_diff_density_min -1.375 _refine_diff_density_rms 0.112 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 0.31583(3) 0.72867(2) 0.391327(18) 0.02369(6) Uani 1 1 d . . . Pd2 Pd 0.29317(3) 0.55473(2) 0.212309(19) 0.02652(7) Uani 1 1 d . . . Pd3 Pd 0.41931(3) 0.86353(3) 0.12754(2) 0.03027(7) Uani 1 1 d . . . Cl1 Cl 0.46513(12) 0.67651(9) 0.13473(8) 0.0423(2) Uani 1 1 d . . . N1 N 0.4441(3) 0.9061(3) 0.3814(2) 0.0254(6) Uani 1 1 d . . . C2 C 0.5846(4) 0.9492(3) 0.3865(3) 0.0321(8) Uani 1 1 d . . . H2 H 0.6358 0.8927 0.3947 0.039 Uiso 1 1 calc R . . C3 C 0.6583(4) 1.0757(4) 0.3802(3) 0.0371(9) Uani 1 1 d . . . H3 H 0.7588 1.1044 0.3844 0.045 Uiso 1 1 calc R . . C4 C 0.5871(5) 1.1591(4) 0.3680(3) 0.0386(9) Uani 1 1 d . . . H4 H 0.6378 1.2452 0.3636 0.046 Uiso 1 1 calc R . . C4A C 0.4391(4) 1.1164(3) 0.3622(2) 0.0324(8) Uani 1 1 d . . . C5 C 0.3494(5) 1.1915(4) 0.3499(3) 0.0445(10) Uani 1 1 d . . . H5 H 0.3911 1.2784 0.3433 0.053 Uiso 1 1 calc R . . C6 C 0.2091(6) 1.1427(4) 0.3475(3) 0.0498(11) Uani 1 1 d . . . H6 H 0.1539 1.1959 0.3391 0.060 Uiso 1 1 calc R . . C6A C 0.1387(5) 1.0123(4) 0.3574(3) 0.0391(9) Uani 1 1 d . . . C7 C -0.0078(5) 0.9548(5) 0.3557(4) 0.0562(13) Uani 1 1 d . . . H7 H -0.0685 1.0037 0.3501 0.067 Uiso 1 1 calc R . . C8 C -0.0635(5) 0.8279(5) 0.3620(4) 0.0577(13) Uani 1 1 d . . . H8 H -0.1632 0.7901 0.3600 0.069 Uiso 1 1 calc R . . C9 C 0.0219(4) 0.7522(4) 0.3715(3) 0.0429(9) Uani 1 1 d . . . H9 H -0.0201 0.6643 0.3751 0.051 Uiso 1 1 calc R . . C10 C 0.1668(4) 0.8056(3) 0.3755(3) 0.0288(7) Uani 1 1 d . . . C10A C 0.2230(4) 0.9352(3) 0.3669(2) 0.0303(7) Uani 1 1 d . . . C10B C 0.3715(4) 0.9883(3) 0.3696(2) 0.0257(7) Uani 1 1 d . . . N1' N 0.3922(3) 1.0333(3) 0.1157(2) 0.0324(7) Uani 1 1 d . . . C2' C 0.2719(5) 1.0572(4) 0.1040(3) 0.0415(9) Uani 1 1 d . . . H2' H 0.1845 0.9897 0.1011 0.050 Uiso 1 1 calc R . . C3' C 0.2705(5) 1.1799(5) 0.0960(3) 0.0482(11) Uani 1 1 d . . . H3' H 0.1826 1.1942 0.0862 0.058 Uiso 1 1 calc R . . C4' C 0.3941(6) 1.2783(4) 0.1021(3) 0.0476(11) Uani 1 1 d . . . H4' H 0.3929 1.3616 0.0976 0.057 Uiso 1 1 calc R . . C4A' C 0.5235(5) 1.2565(4) 0.1152(3) 0.0416(9) Uani 1 1 d . . . C5' C 0.6621(6) 1.3507(4) 0.1237(3) 0.0498(11) Uani 1 1 d . . . H5' H 0.6704 1.4370 0.1226 0.060 Uiso 1 1 calc R . . C6' C 0.7806(6) 1.3201(4) 0.1331(3) 0.0521(12) Uani 1 1 d . . . H6' H 0.8704 1.3852 0.1381 0.063 Uiso 1 1 calc R . . C6A' C 0.7745(5) 1.1911(4) 0.1358(3) 0.0400(9) Uani 1 1 d . . . C7' C 0.8923(5) 1.1524(5) 0.1443(3) 0.0495(11) Uani 1 1 d . . . H7' H 0.9847 1.2134 0.1486 0.059 Uiso 1 1 calc R . . C8' C 0.8763(5) 1.0275(5) 0.1467(3) 0.0497(11) Uani 1 1 d . . . H8' H 0.9583 1.0030 0.1521 0.060 Uiso 1 1 calc R . . C9' C 0.7408(5) 0.9335(4) 0.1412(3) 0.0424(9) Uani 1 1 d . . . H9' H 0.7329 0.8474 0.1433 0.051 Uiso 1 1 calc R . . C10' C 0.6214(4) 0.9662(4) 0.1328(3) 0.0329(8) Uani 1 1 d . . . C10C C 0.6398(4) 1.0960(4) 0.1292(3) 0.0333(8) Uani 1 1 d . . . C10D C 0.5174(4) 1.1306(4) 0.1200(3) 0.0332(8) Uani 1 1 d . . . O1 O 0.4924(3) 0.6644(2) 0.41579(19) 0.0341(6) Uani 1 1 d . . . O2 O 0.4450(3) 0.5092(2) 0.28706(19) 0.0326(5) Uani 1 1 d . . . C11 C 0.5150(4) 0.5742(3) 0.3669(3) 0.0281(7) Uani 1 1 d . . . C12 C 0.6373(4) 0.5367(4) 0.4074(3) 0.0409(9) Uani 1 1 d . . . H12C H 0.7076 0.6102 0.4503 0.061 Uiso 1 1 calc R . . H12B H 0.6814 0.5085 0.3534 0.061 Uiso 1 1 calc R . . H12A H 0.6023 0.4672 0.4447 0.061 Uiso 1 1 calc R . . O3 O 0.1709(3) 0.5623(2) 0.41546(19) 0.0335(6) Uani 1 1 d . . . O4 O 0.1434(3) 0.4323(2) 0.27393(19) 0.0351(6) Uani 1 1 d . . . C13 C 0.1120(4) 0.4602(3) 0.3568(3) 0.0286(7) Uani 1 1 d . . . C14 C -0.0094(5) 0.3606(4) 0.3888(3) 0.0425(10) Uani 1 1 d . . . H14A H 0.0284 0.3166 0.4352 0.064 Uiso 1 1 calc R . . H14B H -0.0654 0.2988 0.3316 0.064 Uiso 1 1 calc R . . H14C H -0.0699 0.4017 0.4202 0.064 Uiso 1 1 calc R . . O5 O 0.1268(3) 0.5742(3) 0.1333(2) 0.0399(6) Uani 1 1 d . . . O6 O 0.1978(3) 0.7829(3) 0.1225(2) 0.0401(6) Uani 1 1 d . . . C15 C 0.1079(5) 0.6743(4) 0.1141(3) 0.0381(9) Uani 1 1 d . . . C16 C -0.0452(5) 0.6592(5) 0.0775(4) 0.0567(13) Uani 1 1 d . . . H16A H -0.1001 0.6513 0.1324 0.085 Uiso 1 1 calc R . . H16B H -0.0868 0.5825 0.0280 0.085 Uiso 1 1 calc R . . H16C H -0.0473 0.7340 0.0488 0.085 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 0.02787(13) 0.01782(11) 0.02629(12) 0.00448(9) 0.00413(9) 0.00860(9) Pd2 0.03174(14) 0.02271(12) 0.02515(12) 0.00552(9) 0.00606(10) 0.00819(10) Pd3 0.03395(15) 0.03066(14) 0.02624(13) 0.00745(10) 0.00777(11) 0.00909(11) Cl1 0.0476(6) 0.0375(5) 0.0511(6) 0.0202(4) 0.0245(5) 0.0175(4) N1 0.0322(15) 0.0198(12) 0.0236(13) 0.0026(10) 0.0057(11) 0.0077(11) C2 0.036(2) 0.0264(17) 0.0327(18) 0.0025(14) 0.0089(15) 0.0087(15) C3 0.038(2) 0.0309(19) 0.0348(19) 0.0011(15) 0.0102(16) 0.0014(16) C4 0.054(3) 0.0230(17) 0.0327(19) 0.0036(14) 0.0085(17) 0.0040(16) C4A 0.052(2) 0.0200(15) 0.0228(16) 0.0020(12) 0.0028(15) 0.0096(15) C5 0.070(3) 0.0220(17) 0.041(2) 0.0037(15) -0.002(2) 0.0192(19) C6 0.067(3) 0.036(2) 0.055(3) 0.0072(19) -0.001(2) 0.033(2) C6A 0.045(2) 0.039(2) 0.041(2) 0.0075(17) 0.0030(18) 0.0250(18) C7 0.052(3) 0.059(3) 0.076(3) 0.023(3) 0.011(2) 0.039(3) C8 0.034(2) 0.063(3) 0.087(4) 0.030(3) 0.014(2) 0.023(2) C9 0.035(2) 0.041(2) 0.056(3) 0.0191(19) 0.0085(19) 0.0134(18) C10 0.0336(19) 0.0287(17) 0.0281(17) 0.0076(13) 0.0052(14) 0.0149(15) C10A 0.043(2) 0.0297(17) 0.0239(16) 0.0052(13) 0.0041(14) 0.0191(16) C10B 0.0399(19) 0.0193(14) 0.0184(14) 0.0012(11) 0.0026(13) 0.0118(13) N1' 0.0377(17) 0.0339(16) 0.0251(14) 0.0050(12) 0.0064(12) 0.0109(14) C2' 0.043(2) 0.046(2) 0.038(2) 0.0097(18) 0.0108(18) 0.0165(19) C3' 0.055(3) 0.052(3) 0.049(2) 0.010(2) 0.013(2) 0.031(2) C4' 0.070(3) 0.035(2) 0.043(2) 0.0062(18) 0.012(2) 0.025(2) C4A' 0.061(3) 0.034(2) 0.0280(18) 0.0030(15) 0.0071(18) 0.0137(19) C5' 0.064(3) 0.030(2) 0.048(2) 0.0052(18) 0.007(2) 0.005(2) C6' 0.057(3) 0.038(2) 0.049(3) 0.0064(19) 0.005(2) 0.000(2) C6A' 0.039(2) 0.039(2) 0.0333(19) 0.0033(16) 0.0045(16) 0.0020(17) C7' 0.034(2) 0.052(3) 0.050(3) 0.003(2) 0.0062(19) -0.0017(19) C8' 0.037(2) 0.061(3) 0.053(3) 0.011(2) 0.011(2) 0.018(2) C9' 0.044(2) 0.042(2) 0.042(2) 0.0093(18) 0.0089(18) 0.0142(19) C10' 0.038(2) 0.0352(19) 0.0240(16) 0.0057(14) 0.0061(14) 0.0101(16) C10C 0.039(2) 0.0342(19) 0.0223(16) 0.0028(14) 0.0067(14) 0.0062(16) C10D 0.042(2) 0.0316(18) 0.0233(16) 0.0026(13) 0.0055(15) 0.0092(16) O1 0.0352(14) 0.0289(13) 0.0393(14) 0.0038(11) -0.0026(11) 0.0153(11) O2 0.0374(14) 0.0254(12) 0.0371(14) 0.0038(10) 0.0051(11) 0.0142(11) C11 0.0274(17) 0.0217(15) 0.0386(19) 0.0134(13) 0.0073(14) 0.0092(13) C12 0.033(2) 0.034(2) 0.062(3) 0.0177(18) 0.0036(18) 0.0170(17) O3 0.0385(15) 0.0222(12) 0.0365(14) 0.0063(10) 0.0095(11) 0.0045(10) O4 0.0371(15) 0.0268(12) 0.0360(14) 0.0046(10) 0.0092(11) 0.0027(11) C13 0.0247(17) 0.0248(16) 0.0366(18) 0.0094(13) 0.0031(14) 0.0076(13) C14 0.040(2) 0.0307(19) 0.051(2) 0.0073(17) 0.0196(19) 0.0017(17) O5 0.0370(15) 0.0334(14) 0.0450(16) 0.0083(12) -0.0061(12) 0.0091(12) O6 0.0367(15) 0.0324(14) 0.0501(17) 0.0135(12) 0.0100(13) 0.0069(12) C15 0.044(2) 0.037(2) 0.0327(19) 0.0113(16) 0.0061(16) 0.0101(17) C16 0.043(3) 0.048(3) 0.076(3) 0.018(2) -0.004(2) 0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C10 1.969(3) . ? Pd1 N1 2.022(3) . ? Pd1 O3 2.052(2) . ? Pd1 O1 2.140(3) . ? Pd1 Pd2 2.9168(4) . ? Pd2 O5 2.003(3) . ? Pd2 O2 2.005(3) . ? Pd2 O4 2.021(3) . ? Pd2 Cl1 2.2822(10) . ? Pd3 C10' 1.974(4) . ? Pd3 N1' 2.039(3) . ? Pd3 O6 2.106(3) . ? Pd3 Cl1 2.3068(10) . ? N1 C2 1.328(5) . ? N1 C10B 1.368(4) . ? C2 C3 1.392(5) . ? C2 H2 0.9500 . ? C3 C4 1.369(6) . ? C3 H3 0.9500 . ? C4 C4A 1.398(6) . ? C4 H4 0.9500 . ? C4A C10B 1.401(5) . ? C4A C5 1.436(6) . ? C5 C6 1.334(7) . ? C5 H5 0.9500 . ? C6 C6A 1.436(6) . ? C6 H6 0.9500 . ? C6A C7 1.400(7) . ? C6A C10A 1.405(5) . ? C7 C8 1.370(7) . ? C7 H7 0.9500 . ? C8 C9 1.401(6) . ? C8 H8 0.9500 . ? C9 C10 1.377(6) . ? C9 H9 0.9500 . ? C10 C10A 1.406(5) . ? C10A C10B 1.412(5) . ? N1' C2' 1.322(5) . ? N1' C10D 1.364(5) . ? C2' C3' 1.404(6) . ? C2' H2' 0.9500 . ? C3' C4' 1.356(7) . ? C3' H3' 0.9500 . ? C4' C4A' 1.401(7) . ? C4' H4' 0.9500 . ? C4A' C10D 1.408(5) . ? C4A' C5' 1.434(6) . ? C5' C6' 1.343(7) . ? C5' H5' 0.9500 . ? C6' C6A' 1.437(6) . ? C6' H6' 0.9500 . ? C6A' C7' 1.389(7) . ? C6A' C10C 1.414(5) . ? C7' C8' 1.366(7) . ? C7' H7' 0.9500 . ? C8' C9' 1.416(6) . ? C8' H8' 0.9500 . ? C9' C10' 1.366(6) . ? C9' H9' 0.9500 . ? C10' C10C 1.418(5) . ? C10C C10D 1.407(6) . ? O1 C11 1.247(4) . ? O2 C11 1.260(4) . ? C11 C12 1.507(5) . ? C12 H12C 0.9800 . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? O3 C13 1.254(4) . ? O4 C13 1.256(4) . ? C13 C14 1.509(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O5 C15 1.256(5) . ? O6 C15 1.246(5) . ? C15 C16 1.524(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 C10 Pd1 N1 82.71(14) . . ? C10 Pd1 O3 91.09(13) . . ? N1 Pd1 O3 171.31(11) . . ? C10 Pd1 O1 174.02(13) . . ? N1 Pd1 O1 92.10(11) . . ? O3 Pd1 O1 93.74(11) . . ? C10 Pd1 Pd2 108.68(10) . . ? N1 Pd1 Pd2 109.92(8) . . ? O3 Pd1 Pd2 77.80(7) . . ? O1 Pd1 Pd2 75.84(7) . . ? O5 Pd2 O2 172.05(11) . . ? O5 Pd2 O4 84.22(12) . . ? O2 Pd2 O4 90.26(11) . . ? O5 Pd2 Cl1 97.12(9) . . ? O2 Pd2 Cl1 87.86(8) . . ? O4 Pd2 Cl1 174.57(8) . . ? O5 Pd2 Pd1 100.16(8) . . ? O2 Pd2 Pd1 84.80(7) . . ? O4 Pd2 Pd1 83.07(7) . . ? Cl1 Pd2 Pd1 101.82(3) . . ? C10' Pd3 N1' 82.61(15) . . ? C10' Pd3 O6 170.51(14) . . ? N1' Pd3 O6 87.94(12) . . ? C10' Pd3 Cl1 93.57(12) . . ? N1' Pd3 Cl1 175.55(9) . . ? O6 Pd3 Cl1 95.91(8) . . ? Pd2 Cl1 Pd3 106.27(4) . . ? C2 N1 C10B 118.9(3) . . ? C2 N1 Pd1 128.2(2) . . ? C10B N1 Pd1 112.9(2) . . ? N1 C2 C3 121.3(4) . . ? N1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C4 C3 C2 120.5(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C4A 119.5(3) . . ? C3 C4 H4 120.2 . . ? C4A C4 H4 120.2 . . ? C4 C4A C10B 117.1(3) . . ? C4 C4A C5 126.3(4) . . ? C10B C4A C5 116.6(4) . . ? C6 C5 C4A 121.8(4) . . ? C6 C5 H5 119.1 . . ? C4A C5 H5 119.1 . . ? C5 C6 C6A 122.2(4) . . ? C5 C6 H6 118.9 . . ? C6A C6 H6 118.9 . . ? C7 C6A C10A 117.3(4) . . ? C7 C6A C6 125.3(4) . . ? C10A C6A C6 117.4(4) . . ? C8 C7 C6A 120.0(4) . . ? C8 C7 H7 120.0 . . ? C6A C7 H7 120.0 . . ? C7 C8 C9 122.1(4) . . ? C7 C8 H8 118.9 . . ? C9 C8 H8 118.9 . . ? C10 C9 C8 119.8(4) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C10A 117.8(3) . . ? C9 C10 Pd1 130.2(3) . . ? C10A C10 Pd1 112.0(3) . . ? C6A C10A C10 123.0(4) . . ? C6A C10A C10B 119.7(3) . . ? C10 C10A C10B 117.3(3) . . ? N1 C10B C4A 122.6(3) . . ? N1 C10B C10A 115.1(3) . . ? C4A C10B C10A 122.2(3) . . ? C2' N1' C10D 119.0(3) . . ? C2' N1' Pd3 128.1(3) . . ? C10D N1' Pd3 112.8(3) . . ? N1' C2' C3' 121.5(4) . . ? N1' C2' H2' 119.3 . . ? C3' C2' H2' 119.3 . . ? C4' C3' C2' 120.3(4) . . ? C4' C3' H3' 119.8 . . ? C2' C3' H3' 119.8 . . ? C3' C4' C4A' 119.7(4) . . ? C3' C4' H4' 120.2 . . ? C4A' C4' H4' 120.2 . . ? C4' C4A' C10D 117.2(4) . . ? C4' C4A' C5' 126.1(4) . . ? C10D C4A' C5' 116.8(4) . . ? C6' C5' C4A' 121.9(4) . . ? C6' C5' H5' 119.1 . . ? C4A' C5' H5' 119.1 . . ? C5' C6' C6A' 121.5(4) . . ? C5' C6' H6' 119.3 . . ? C6A' C6' H6' 119.3 . . ? C7' C6A' C10C 117.1(4) . . ? C7' C6A' C6' 124.6(4) . . ? C10C C6A' C6' 118.3(4) . . ? C8' C7' C6A' 120.6(4) . . ? C8' C7' H7' 119.7 . . ? C6A' C7' H7' 119.7 . . ? C7' C8' C9' 121.7(4) . . ? C7' C8' H8' 119.2 . . ? C9' C8' H8' 119.2 . . ? C10' C9' C8' 120.3(4) . . ? C10' C9' H9' 119.9 . . ? C8' C9' H9' 119.9 . . ? C9' C10' C10C 117.3(4) . . ? C9' C10' Pd3 131.2(3) . . ? C10C C10' Pd3 111.5(3) . . ? C10D C10C C6A' 119.2(4) . . ? C10D C10C C10' 117.7(3) . . ? C6A' C10C C10' 123.1(4) . . ? N1' C10D C10C 115.2(3) . . ? N1' C10D C4A' 122.3(4) . . ? C10C C10D C4A' 122.4(4) . . ? C11 O1 Pd1 127.8(2) . . ? C11 O2 Pd2 122.6(2) . . ? O1 C11 O2 126.8(3) . . ? O1 C11 C12 117.3(3) . . ? O2 C11 C12 115.9(3) . . ? C11 C12 H12C 109.5 . . ? C11 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? C11 C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? C13 O3 Pd1 128.4(2) . . ? C13 O4 Pd2 123.4(2) . . ? O3 C13 O4 126.7(3) . . ? O3 C13 C14 116.9(3) . . ? O4 C13 C14 116.4(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 O5 Pd2 129.0(3) . . ? C15 O6 Pd3 137.3(3) . . ? O6 C15 O5 128.1(4) . . ? O6 C15 C16 117.0(4) . . ? O5 C15 C16 115.0(4) . . ? 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 . . ? 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 C10 Pd1 Pd2 O5 -0.41(14) . . . . ? N1 Pd1 Pd2 O5 -89.27(12) . . . . ? O3 Pd1 Pd2 O5 86.58(11) . . . . ? O1 Pd1 Pd2 O5 -176.33(11) . . . . ? C10 Pd1 Pd2 O2 -174.14(13) . . . . ? N1 Pd1 Pd2 O2 97.00(12) . . . . ? O3 Pd1 Pd2 O2 -87.15(11) . . . . ? O1 Pd1 Pd2 O2 9.94(11) . . . . ? C10 Pd1 Pd2 O4 -83.24(14) . . . . ? N1 Pd1 Pd2 O4 -172.09(12) . . . . ? O3 Pd1 Pd2 O4 3.75(11) . . . . ? O1 Pd1 Pd2 O4 100.84(11) . . . . ? C10 Pd1 Pd2 Cl1 99.15(11) . . . . ? N1 Pd1 Pd2 Cl1 10.29(9) . . . . ? O3 Pd1 Pd2 Cl1 -173.86(8) . . . . ? O1 Pd1 Pd2 Cl1 -76.77(8) . . . . ? O5 Pd2 Cl1 Pd3 48.73(9) . . . . ? O2 Pd2 Cl1 Pd3 -137.49(8) . . . . ? Pd1 Pd2 Cl1 Pd3 -53.26(4) . . . . ? C10' Pd3 Cl1 Pd2 149.55(11) . . . . ? O6 Pd3 Cl1 Pd2 -29.84(9) . . . . ? C10 Pd1 N1 C2 179.0(3) . . . . ? O1 Pd1 N1 C2 2.0(3) . . . . ? Pd2 Pd1 N1 C2 -73.7(3) . . . . ? C10 Pd1 N1 C10B 0.2(2) . . . . ? O1 Pd1 N1 C10B -176.8(2) . . . . ? Pd2 Pd1 N1 C10B 107.5(2) . . . . ? C10B N1 C2 C3 0.0(5) . . . . ? Pd1 N1 C2 C3 -178.7(3) . . . . ? N1 C2 C3 C4 -0.3(6) . . . . ? C2 C3 C4 C4A 0.2(6) . . . . ? C3 C4 C4A C10B 0.2(5) . . . . ? C3 C4 C4A C5 179.7(4) . . . . ? C4 C4A C5 C6 -178.3(4) . . . . ? C10B C4A C5 C6 1.2(6) . . . . ? C4A C5 C6 C6A 0.2(7) . . . . ? C5 C6 C6A C7 180.0(5) . . . . ? C5 C6 C6A C10A -1.8(7) . . . . ? C10A C6A C7 C8 -0.7(7) . . . . ? C6 C6A C7 C8 177.5(5) . . . . ? C6A C7 C8 C9 0.8(9) . . . . ? C7 C8 C9 C10 0.6(8) . . . . ? C8 C9 C10 C10A -1.8(6) . . . . ? C8 C9 C10 Pd1 178.4(4) . . . . ? N1 Pd1 C10 C9 179.3(4) . . . . ? O3 Pd1 C10 C9 -6.8(4) . . . . ? Pd2 Pd1 C10 C9 70.7(4) . . . . ? N1 Pd1 C10 C10A -0.5(2) . . . . ? O3 Pd1 C10 C10A 173.4(3) . . . . ? Pd2 Pd1 C10 C10A -109.1(2) . . . . ? C7 C6A C10A C10 -0.6(6) . . . . ? C6 C6A C10A C10 -179.0(4) . . . . ? C7 C6A C10A C10B -179.6(4) . . . . ? C6 C6A C10A C10B 2.0(6) . . . . ? C9 C10 C10A C6A 1.9(6) . . . . ? Pd1 C10 C10A C6A -178.3(3) . . . . ? C9 C10 C10A C10B -179.1(3) . . . . ? Pd1 C10 C10A C10B 0.7(4) . . . . ? C2 N1 C10B C4A 0.4(5) . . . . ? Pd1 N1 C10B C4A 179.3(2) . . . . ? C2 N1 C10B C10A -178.8(3) . . . . ? Pd1 N1 C10B C10A 0.2(4) . . . . ? C4 C4A C10B N1 -0.5(5) . . . . ? C5 C4A C10B N1 179.9(3) . . . . ? C4 C4A C10B C10A 178.6(3) . . . . ? C5 C4A C10B C10A -1.0(5) . . . . ? C6A C10A C10B N1 178.5(3) . . . . ? C10 C10A C10B N1 -0.6(4) . . . . ? C6A C10A C10B C4A -0.7(5) . . . . ? C10 C10A C10B C4A -179.8(3) . . . . ? C10' Pd3 N1' C2' 177.5(3) . . . . ? O6 Pd3 N1' C2' -3.5(3) . . . . ? C10' Pd3 N1' C10D -1.9(2) . . . . ? O6 Pd3 N1' C10D 177.1(2) . . . . ? C10D N1' C2' C3' 0.1(6) . . . . ? Pd3 N1' C2' C3' -179.3(3) . . . . ? N1' C2' C3' C4' -1.4(7) . . . . ? C2' C3' C4' C4A' 0.9(7) . . . . ? C3' C4' C4A' C10D 0.8(6) . . . . ? C3' C4' C4A' C5' -179.5(4) . . . . ? C4' C4A' C5' C6' -177.9(4) . . . . ? C10D C4A' C5' C6' 1.8(6) . . . . ? C4A' C5' C6' C6A' -0.4(7) . . . . ? C5' C6' C6A' C7' 179.3(4) . . . . ? C5' C6' C6A' C10C -0.7(7) . . . . ? C10C C6A' C7' C8' -0.3(6) . . . . ? C6' C6A' C7' C8' 179.7(4) . . . . ? C6A' C7' C8' C9' -0.4(7) . . . . ? C7' C8' C9' C10' 0.3(7) . . . . ? C8' C9' C10' C10C 0.5(6) . . . . ? C8' C9' C10' Pd3 -177.9(3) . . . . ? N1' Pd3 C10' C9' -179.6(4) . . . . ? Cl1 Pd3 C10' C9' -1.9(4) . . . . ? N1' Pd3 C10' C10C 1.9(2) . . . . ? Cl1 Pd3 C10' C10C 179.6(2) . . . . ? C7' C6A' C10C C10D -179.7(4) . . . . ? C6' C6A' C10C C10D 0.3(6) . . . . ? C7' C6A' C10C C10' 1.1(6) . . . . ? C6' C6A' C10C C10' -178.8(4) . . . . ? C9' C10' C10C C10D 179.6(3) . . . . ? Pd3 C10' C10C C10D -1.7(4) . . . . ? C9' C10' C10C C6A' -1.3(5) . . . . ? Pd3 C10' C10C C6A' 177.4(3) . . . . ? C2' N1' C10D C10C -178.0(3) . . . . ? Pd3 N1' C10D C10C 1.5(4) . . . . ? C2' N1' C10D C4A' 1.7(5) . . . . ? Pd3 N1' C10D C4A' -178.8(3) . . . . ? C6A' C10C C10D N1' -179.1(3) . . . . ? C10' C10C C10D N1' 0.1(5) . . . . ? C6A' C10C C10D C4A' 1.2(5) . . . . ? C10' C10C C10D C4A' -179.6(3) . . . . ? C4' C4A' C10D N1' -2.2(6) . . . . ? C5' C4A' C10D N1' 178.1(4) . . . . ? C4' C4A' C10D C10C 177.5(4) . . . . ? C5' C4A' C10D C10C -2.2(6) . . . . ? N1 Pd1 O1 C11 -122.4(3) . . . . ? O3 Pd1 O1 C11 64.0(3) . . . . ? Pd2 Pd1 O1 C11 -12.4(3) . . . . ? O4 Pd2 O2 C11 -95.9(3) . . . . ? Cl1 Pd2 O2 C11 89.1(3) . . . . ? Pd1 Pd2 O2 C11 -12.9(3) . . . . ? Pd1 O1 C11 O2 7.3(5) . . . . ? Pd1 O1 C11 C12 -171.8(2) . . . . ? Pd2 O2 C11 O1 8.2(5) . . . . ? Pd2 O2 C11 C12 -172.6(2) . . . . ? C10 Pd1 O3 C13 100.7(3) . . . . ? O1 Pd1 O3 C13 -82.8(3) . . . . ? Pd2 Pd1 O3 C13 -8.1(3) . . . . ? O5 Pd2 O4 C13 -102.6(3) . . . . ? O2 Pd2 O4 C13 83.1(3) . . . . ? Pd1 Pd2 O4 C13 -1.6(3) . . . . ? Pd1 O3 C13 O4 10.3(5) . . . . ? Pd1 O3 C13 C14 -169.6(3) . . . . ? Pd2 O4 C13 O3 -4.0(5) . . . . ? Pd2 O4 C13 C14 175.9(3) . . . . ? O4 Pd2 O5 C15 134.4(4) . . . . ? Cl1 Pd2 O5 C15 -50.9(4) . . . . ? Pd1 Pd2 O5 C15 52.5(4) . . . . ? N1' Pd3 O6 C15 169.7(4) . . . . ? Cl1 Pd3 O6 C15 -8.0(4) . . . . ? Pd3 O6 C15 O5 22.8(7) . . . . ? Pd3 O6 C15 C16 -158.3(3) . . . . ? Pd2 O5 C15 O6 15.7(6) . . . . ? Pd2 O5 C15 C16 -163.2(3) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.045 0 -1 0 0.045 0 0 1 0.075 0 0 -1 0.085 1 -1 0 0.020 9 0 -1 0.020 -5 2 1 0.020