# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1844 data_4a _publ_contact_author_name 'Prof. Bernhard Lippert' _publ_contact_author_address ; Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_email 'lippert@pop.uni-dortmund.de' _publ_contact_author_fax 'Int. code + (231) 755-3797' _publ_contact_author_phone '231 755-3840' _publ_contact_letter ? _publ_requested_journal 'Dalton Transactions' _publ_title ; Ready formation of water-stable Pt(II)-(-NH2)-Pd(II) species through combination of trans-[(NH3)2 Pt(II)L2] (L = N,N'-hterocycle) and [enPd(H2O)2]2+ ; _publ_author_address ; Alexandra Fichtel, Eva Freisinger, Bettina Beck, Bernhard Lippert' Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H36 N14 O15 Pd3 Pt' _chemical_formula_weight 1154.86 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 8.274(2) _cell_length_b 13.653(3) _cell_length_c 27.992(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.56(3) _cell_angle_gamma 90.00 _cell_volume 3159.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 136(2) _cell_measurement_reflns_used 3631 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 21.72 _exptl_crystal_description stick _exptl_crystal_colour red-brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.428 _exptl_crystal_density_method ? _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 6.182 _exptl_absorpt_correction_type SCALEPACK _exptl_absorpt_correction_T_min 0.2052 _exptl_absorpt_correction_T_max 0.6967 _exptl_special_details ; ? ; _diffrn_ambient_temperature 136(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 'Enraf-Nonius-KappaCCD' _diffrn_measurement_method ; 360 frames via \w-rotation (\D\w\=1\%) and two times 70s per frame ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3631 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 21.72 _reflns_number_total 3631 _reflns_number_observed 2810 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, Netherlands)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 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^)+(0.0228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ; refU, except H2, H2', H8a, H8b, H8a', H8b', H1wa, H1wb, H2wa, H2wb, H3wa, H3wb refall' ; _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00007(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3628 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_obs 0.0248 _refine_ls_wR_factor_all 0.0490 _refine_ls_wR_factor_obs 0.0458 _refine_ls_goodness_of_fit_all 0.920 _refine_ls_goodness_of_fit_obs 1.013 _refine_ls_restrained_S_all 0.937 _refine_ls_restrained_S_obs 1.013 _refine_ls_shift/esd_max 0.007 _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 Pt1 Pt 0.87259(3) 0.82675(2) 0.608965(10) 0.01873(10) Uani 1 d . . Pd1 Pd 0.71610(6) 0.67597(4) 0.59603(2) 0.01860(15) Uani 1 d . . Pd2 Pd 0.77363(5) 0.73983(4) 0.49678(2) 0.0188(2) Uani 1 d . . Pd3 Pd 0.75230(6) 0.68860(4) 0.70404(2) 0.0189(2) Uani 1 d . . N11' N 0.9342(6) 0.8171(4) 0.5393(2) 0.0198(15) Uani 1 d . . N11 N 0.8014(7) 0.8258(4) 0.6777(2) 0.0203(15) Uani 1 d . . N21 N 0.6297(6) 0.6550(4) 0.4523(2) 0.0246(15) Uani 1 d . . H21A H 0.6251(6) 0.5937(4) 0.4639(2) 0.026(5) Uiso 1 calc R . H21B H 0.5286(6) 0.6796(4) 0.4504(2) 0.026(5) Uiso 1 calc R . C21 C 0.6984(7) 0.6538(5) 0.4038(2) 0.024(2) Uani 1 d . . H21C H 0.6737(7) 0.7145(5) 0.3871(2) 0.026(5) Uiso 1 calc R . H21D H 0.6532(7) 0.5998(5) 0.3850(2) 0.026(5) Uiso 1 calc R . C22 C 0.8779(8) 0.6416(5) 0.4114(3) 0.027(2) Uani 1 d . . H22A H 0.9023(8) 0.5767(5) 0.4237(3) 0.026(5) Uiso 1 calc R . H22B H 0.9299(8) 0.6492(5) 0.3812(3) 0.026(5) Uiso 1 calc R . N22 N 0.9396(6) 0.7173(4) 0.4461(2) 0.0235(15) Uani 1 d . . H22C H 0.9578(6) 0.7737(4) 0.4306(2) 0.026(5) Uiso 1 calc R . H22D H 1.0337(6) 0.6971(4) 0.4602(2) 0.026(5) Uiso 1 calc R . N31 N 0.7070(6) 0.5578(4) 0.7377(2) 0.0237(14) Uiso 1 d . . H31A H 0.6284(6) 0.5246(4) 0.7214(2) 0.026(5) Uiso 1 calc R . H31B H 0.7969(6) 0.5205(4) 0.7393(2) 0.026(5) Uiso 1 calc R . C31 C 0.6563(8) 0.5809(5) 0.7859(3) 0.029(2) Uani 1 d . . H31C H 0.7499(8) 0.5969(5) 0.8065(3) 0.026(5) Uiso 1 calc R . H31D H 0.6024(8) 0.5249(5) 0.7993(3) 0.026(5) Uiso 1 calc R . C32 C 0.5418(8) 0.6676(5) 0.7824(3) 0.029(2) Uani 1 d . . H32A H 0.4444(8) 0.6507(5) 0.7637(3) 0.026(5) Uiso 1 calc R . H32B H 0.5115(8) 0.6878(5) 0.8140(3) 0.026(5) Uiso 1 calc R . N32 N 0.6320(6) 0.7477(4) 0.7586(2) 0.0267(15) Uiso 1 d . . H32C H 0.7025(6) 0.7761(4) 0.7798(2) 0.026(5) Uiso 1 calc R . H32D H 0.5624(6) 0.7938(4) 0.7474(2) 0.026(5) Uiso 1 calc R . N1 N 0.6741(6) 0.9015(4) 0.5846(2) 0.0175(13) Uiso 1 d . . N2 N 0.5932(6) 0.7575(4) 0.5448(2) 0.0209(14) Uiso 1 d . . C2 C 0.5621(7) 0.8549(5) 0.5567(2) 0.021(2) Uiso 1 d . . C3 C 0.4203(7) 0.9046(5) 0.5407(2) 0.024(2) Uiso 1 d . . H3 H 0.3413(7) 0.8722(5) 0.5221(2) 0.026(7) Uiso 1 calc R . C4 C 0.3999(8) 1.0001(5) 0.5527(3) 0.026(2) Uiso 1 d . . H4 H 0.3080(8) 1.0336(5) 0.5415(3) 0.026(7) Uiso 1 calc R . C5 C 0.5160(8) 1.0481(6) 0.5816(3) 0.030(2) Uani 1 d . . H5 H 0.5026(8) 1.1132(6) 0.5902(3) 0.026(7) Uiso 1 calc R . C6 C 0.6519(8) 0.9960(5) 0.5970(2) 0.023(2) Uani 1 d . . H6 H 0.7303(8) 1.0269(5) 0.6165(2) 0.026(7) Uiso 1 calc R . N1' N 1.0586(5) 0.7417(4) 0.6326(2) 0.0180(13) Uiso 1 d . . C2' C 1.0280(7) 0.6483(5) 0.6468(2) 0.020(2) Uiso 1 d . . N2' N 0.8659(7) 0.6211(4) 0.6485(2) 0.024(2) Uiso 1 d . . C3' C 1.1550(7) 0.5856(5) 0.6615(2) 0.026(2) Uiso 1 d . . H3' H 1.1338(7) 0.5220(5) 0.6713(2) 0.026(7) Uiso 1 calc R . C4' C 1.3099(8) 0.6195(6) 0.6613(3) 0.029(2) Uiso 1 d . . H4' H 1.3949(8) 0.5778(6) 0.6701(3) 0.026(7) Uiso 1 calc R . C5' C 1.3429(8) 0.7157(6) 0.6479(3) 0.031(2) Uani 1 d . . H5' H 1.4483(8) 0.7394(6) 0.6485(3) 0.026(7) Uiso 1 calc R . C6' C 1.2148(7) 0.7736(5) 0.6340(2) 0.026(2) Uani 1 d . . H6' H 1.2351(7) 0.8379(5) 0.6251(2) 0.026(7) Uiso 1 calc R . N10 N 1.0535(6) 1.0420(5) 0.5986(3) 0.027(2) Uani 1 d . . O11 O 1.0365(5) 0.9704(3) 0.6270(2) 0.0261(12) Uani 1 d . . O12 O 1.1301(5) 1.1148(4) 0.6139(2) 0.0309(13) Uani 1 d . . O13 O 0.9918(5) 1.0397(4) 0.5568(2) 0.0315(13) Uani 1 d . . N20 N 0.7395(7) 0.8892(5) 0.0204(2) 0.035(2) Uani 1 d . . O21 O 0.8632(5) 0.9446(4) 0.0156(2) 0.0348(14) Uani 1 d . . O22 O 0.7535(5) 0.7994(4) 0.0168(2) 0.0350(14) Uani 1 d . . O23 O 0.6080(7) 0.9260(4) 0.0267(3) 0.080(2) Uani 1 d . . N30 N 0.2425(7) 0.1574(5) 0.1293(3) 0.029(2) Uani 1 d . . O31 O 0.2782(5) 0.0988(4) 0.1625(2) 0.0333(13) Uani 1 d . . O32 O 0.2216(5) 0.1266(4) 0.0867(2) 0.0333(13) Uani 1 d . . O33 O 0.2284(7) 0.2463(4) 0.1367(2) 0.058(2) Uani 1 d . . N40 N 0.8557(8) 0.1426(5) 0.2288(3) 0.043(2) Uani 1 d . . O41 O 0.7178(6) 0.1581(4) 0.2123(2) 0.050(2) Uani 1 d . . O42 O 0.9012(7) 0.0614(5) 0.2395(3) 0.084(2) Uani 1 d . . O43 O 0.9728(15) 0.2016(9) 0.2281(5) 0.048(4) Uiso 0.50 d P . O43A O 0.9218(16) 0.2211(10) 0.2451(5) 0.062(4) Uiso 0.50 d P . O1W O 0.5810(6) 0.5475(4) 0.5889(2) 0.0272(14) Uani 1 d . . O2W O -0.0007(6) 0.5511(4) 0.2294(2) 0.047(2) Uani 1 d . . O3W O 0.8895(7) 0.3866(5) 0.1863(2) 0.050(2) Uani 1 d . . H2 H 0.5061(66) 0.7320(47) 0.5372(21) 0.027(6) Uiso 1 d . . H2' H 0.8419(73) 0.5774(50) 0.6561(24) 0.027(6) Uiso 1 d . . H11A H 0.8712(79) 0.8407(49) 0.6988(25) 0.027(6) Uiso 1 d . . H11B H 0.7086(75) 0.8516(46) 0.6821(23) 0.027(6) Uiso 1 d . . H11C H 0.9406(72) 0.8749(49) 0.5231(24) 0.027(6) Uiso 1 d . . H11D H 1.0157(73) 0.7913(49) 0.5359(24) 0.027(6) Uiso 1 d . . H1WA H 0.5075(74) 0.5549(52) 0.5704(25) 0.027(6) Uiso 1 d . . H1WB H 0.6313(78) 0.5002(50) 0.5845(26) 0.027(6) Uiso 1 d . . H2WA H -0.0758(77) 0.5681(51) 0.2473(25) 0.027(6) Uiso 1 d . . H2WB H -0.0322(74) 0.4982(50) 0.2137(25) 0.027(6) Uiso 1 d . . H3WA H 0.8111(80) 0.3904(53) 0.1688(26) 0.027(6) Uiso 1 d . . H3WB H 0.9112(80) 0.3358(52) 0.2000(26) 0.027(6) Uiso 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 Pt1 0.0178(2) 0.0164(2) 0.0221(2) 0.0004(2) 0.00247(11) 0.00015(13) Pd1 0.0165(3) 0.0168(3) 0.0226(4) 0.0004(3) 0.0020(2) 0.0003(2) Pd2 0.0165(3) 0.0174(3) 0.0224(4) 0.0005(3) 0.0017(2) -0.0001(2) Pd3 0.0195(3) 0.0165(3) 0.0208(4) 0.0004(3) 0.0029(2) 0.0006(2) N11' 0.016(3) 0.017(4) 0.027(4) 0.002(3) -0.001(3) 0.003(3) N11 0.011(3) 0.019(4) 0.031(4) 0.000(3) 0.000(3) -0.002(3) N21 0.026(3) 0.018(4) 0.030(4) 0.002(3) 0.000(3) -0.005(3) C21 0.025(4) 0.028(5) 0.019(5) -0.002(4) 0.001(3) -0.005(3) C22 0.032(4) 0.021(5) 0.027(5) -0.005(4) 0.001(4) -0.001(3) N22 0.022(3) 0.021(4) 0.027(4) 0.007(3) 0.002(3) 0.001(3) C31 0.033(4) 0.028(5) 0.026(5) 0.004(4) 0.004(4) -0.002(4) C32 0.026(4) 0.034(5) 0.027(5) -0.005(4) 0.007(3) 0.002(4) C5 0.035(4) 0.026(5) 0.030(5) 0.002(4) 0.015(4) 0.012(4) C6 0.037(4) 0.017(5) 0.015(5) -0.001(4) 0.005(3) 0.000(4) C5' 0.014(4) 0.043(5) 0.037(5) -0.002(4) 0.004(3) 0.002(3) C6' 0.024(4) 0.026(5) 0.029(5) 0.001(4) 0.004(3) -0.001(4) N10 0.019(3) 0.024(4) 0.037(5) 0.001(4) 0.006(3) 0.005(3) O11 0.033(3) 0.017(3) 0.028(3) 0.003(3) 0.001(2) -0.007(2) O12 0.037(3) 0.018(3) 0.038(4) -0.001(3) 0.003(3) -0.008(3) O13 0.034(3) 0.028(3) 0.033(4) 0.002(3) 0.001(3) -0.001(2) N20 0.027(4) 0.041(5) 0.038(5) -0.012(4) -0.003(3) 0.007(4) O21 0.028(3) 0.030(3) 0.046(4) 0.006(3) -0.001(3) -0.009(3) O22 0.025(3) 0.024(4) 0.055(4) 0.005(3) -0.004(2) 0.002(2) O23 0.036(4) 0.050(4) 0.153(8) -0.043(4) 0.006(4) 0.002(3) N30 0.027(3) 0.033(5) 0.028(5) -0.009(4) 0.001(3) -0.007(3) O31 0.046(3) 0.030(3) 0.024(4) 0.007(3) 0.003(3) 0.002(3) O32 0.038(3) 0.037(3) 0.024(4) -0.002(3) 0.001(3) -0.008(2) O33 0.092(4) 0.023(4) 0.058(5) -0.012(3) -0.016(3) 0.016(3) N40 0.051(5) 0.028(5) 0.049(5) 0.002(4) -0.009(4) -0.006(4) O41 0.029(3) 0.060(4) 0.060(4) 0.008(3) -0.009(3) 0.009(3) O42 0.079(5) 0.051(5) 0.124(7) 0.031(5) 0.016(4) 0.031(4) O1W 0.020(3) 0.024(3) 0.037(4) 0.005(3) -0.002(2) 0.001(2) O2W 0.036(4) 0.028(4) 0.076(6) -0.008(3) -0.003(3) -0.003(3) O3W 0.052(4) 0.037(4) 0.061(5) 0.009(4) -0.015(3) -0.008(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 Pt1 N1' 2.016(5) . ? Pt1 N1 2.026(5) . ? Pt1 N11 2.038(6) . ? Pt1 N11' 2.041(6) . ? Pt1 O11 2.425(5) . ? Pt1 Pd1 2.4503(7) . ? Pd1 N2' 2.024(6) . ? Pd1 N2 2.049(6) . ? Pd1 O1W 2.084(5) . ? Pd1 Pd2 2.9706(10) . ? Pd1 Pd3 3.0298(10) . ? Pd2 N11' 2.039(6) . ? Pd2 N22 2.041(5) . ? Pd2 N21 2.043(5) . ? Pd2 N2 2.067(5) . ? Pd3 N32 2.028(5) . ? Pd3 N11 2.060(6) . ? Pd3 N31 2.061(5) . ? Pd3 N2' 2.068(6) . ? N21 C21 1.495(8) . ? C21 C22 1.500(9) . ? C22 N22 1.493(8) . ? N31 C31 1.465(8) . ? C31 C32 1.517(9) . ? C32 N32 1.498(8) . ? N1 C2 1.345(8) . ? N1 C6 1.350(8) . ? N2 C2 1.398(9) . ? C2 C3 1.410(9) . ? C3 C4 1.359(9) . ? C4 C5 1.391(9) . ? C5 C6 1.383(9) . ? N1' C6' 1.362(7) . ? N1' C2' 1.363(8) . ? C2' N2' 1.395(8) . ? C2' C3' 1.403(9) . ? C3' C4' 1.363(9) . ? C4' C5' 1.396(10) . ? C5' C6' 1.366(9) . ? N10 O12 1.244(7) . ? N10 O13 1.256(7) . ? N10 O11 1.272(7) . ? N20 O23 1.219(7) . ? N20 O22 1.237(7) . ? N20 O21 1.284(7) . ? N30 O33 1.237(8) . ? N30 O31 1.251(7) . ? N30 O32 1.270(7) . ? N40 O42 1.204(8) . ? N40 O41 1.230(7) . ? N40 O43 1.262(13) . ? N40 O43A 1.278(14) . ? O43 O43A 0.70(2) . ? 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' Pt1 N1 175.1(2) . . ? N1' Pt1 N11 86.3(2) . . ? N1 Pt1 N11 93.3(2) . . ? N1' Pt1 N11' 93.3(2) . . ? N1 Pt1 N11' 86.8(2) . . ? N11 Pt1 N11' 175.3(2) . . ? N1' Pt1 O11 89.2(2) . . ? N1 Pt1 O11 95.7(2) . . ? N11 Pt1 O11 89.5(2) . . ? N11' Pt1 O11 95.2(2) . . ? N1' Pt1 Pd1 87.44(15) . . ? N1 Pt1 Pd1 87.62(15) . . ? N11 Pt1 Pd1 87.8(2) . . ? N11' Pt1 Pd1 87.6(2) . . ? O11 Pt1 Pd1 175.77(12) . . ? N2' Pd1 N2 168.0(2) . . ? N2' Pd1 O1W 93.8(2) . . ? N2 Pd1 O1W 98.2(2) . . ? N2' Pd1 Pt1 84.3(2) . . ? N2 Pd1 Pt1 83.6(2) . . ? O1W Pd1 Pt1 177.0(2) . . ? N2' Pd1 Pd2 132.0(2) . . ? N2 Pd1 Pd2 44.05(15) . . ? O1W Pd1 Pd2 105.4(2) . . ? Pt1 Pd1 Pd2 77.64(2) . . ? N2' Pd1 Pd3 42.8(2) . . ? N2 Pd1 Pd3 133.7(2) . . ? O1W Pd1 Pd3 99.9(2) . . ? Pt1 Pd1 Pd3 77.10(2) . . ? Pd2 Pd1 Pd3 154.66(2) . . ? N11' Pd2 N22 92.5(2) . . ? N11' Pd2 N21 174.9(2) . . ? N22 Pd2 N21 83.3(2) . . ? N11' Pd2 N2 91.7(2) . . ? N22 Pd2 N2 175.8(2) . . ? N21 Pd2 N2 92.5(2) . . ? N11' Pd2 Pd1 74.5(2) . . ? N22 Pd2 Pd1 138.3(2) . . ? N21 Pd2 Pd1 106.8(2) . . ? N2 Pd2 Pd1 43.6(2) . . ? N32 Pd3 N11 91.1(2) . . ? N32 Pd3 N31 84.0(2) . . ? N11 Pd3 N31 173.8(2) . . ? N32 Pd3 N2' 176.6(2) . . ? N11 Pd3 N2' 91.9(2) . . ? N31 Pd3 N2' 93.2(2) . . ? N32 Pd3 Pd1 138.1(2) . . ? N11 Pd3 Pd1 73.0(2) . . ? N31 Pd3 Pd1 113.2(2) . . ? N2' Pd3 Pd1 41.7(2) . . ? Pd2 N11' Pt1 114.1(3) . . ? Pt1 N11 Pd3 114.4(3) . . ? C21 N21 Pd2 108.9(4) . . ? N21 C21 C22 106.7(6) . . ? N22 C22 C21 108.9(5) . . ? C22 N22 Pd2 109.6(4) . . ? C31 N31 Pd3 107.4(4) . . ? N31 C31 C32 108.3(6) . . ? N32 C32 C31 106.0(5) . . ? C32 N32 Pd3 108.4(4) . . ? C2 N1 C6 120.2(6) . . ? C2 N1 Pt1 118.9(4) . . ? C6 N1 Pt1 120.8(4) . . ? C2 N2 Pd1 116.2(4) . . ? C2 N2 Pd2 114.3(4) . . ? Pd1 N2 Pd2 92.4(2) . . ? N1 C2 N2 117.3(6) . . ? N1 C2 C3 119.9(6) . . ? N2 C2 C3 122.8(6) . . ? C4 C3 C2 119.6(7) . . ? C3 C4 C5 120.3(7) . . ? C6 C5 C4 118.0(7) . . ? N1 C6 C5 121.9(7) . . ? C6' N1' C2' 118.6(5) . . ? C6' N1' Pt1 122.3(5) . . ? C2' N1' Pt1 119.0(4) . . ? N1' C2' N2' 116.8(6) . . ? N1' C2' C3' 120.7(6) . . ? N2' C2' C3' 122.4(6) . . ? C2' N2' Pd1 115.7(5) . . ? C2' N2' Pd3 112.2(5) . . ? Pd1 N2' Pd3 95.5(3) . . ? C4' C3' C2' 118.9(7) . . ? C3' C4' C5' 121.1(7) . . ? C6' C5' C4' 117.5(6) . . ? N1' C6' C5' 123.1(7) . . ? O12 N10 O13 121.3(6) . . ? O12 N10 O11 117.9(7) . . ? O13 N10 O11 120.8(6) . . ? N10 O11 Pt1 124.6(4) . . ? O23 N20 O22 120.6(6) . . ? O23 N20 O21 119.6(7) . . ? O22 N20 O21 119.8(6) . . ? O33 N30 O31 121.6(7) . . ? O33 N30 O32 118.2(7) . . ? O31 N30 O32 120.2(6) . . ? O42 N40 O41 121.7(7) . . ? O42 N40 O43 111.1(9) . . ? O41 N40 O43 125.7(9) . . ? O42 N40 O43A 124.0(9) . . ? O41 N40 O43A 111.4(9) . . ? O43 N40 O43A 32.2(7) . . ? O43A O43 N40 75.2(18) . . ? O43 O43A N40 72.7(18) . . ? 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' Pt1 Pd1 N2' 26.5(2) . . . . ? N1 Pt1 Pd1 N2' -153.3(2) . . . . ? N11 Pt1 Pd1 N2' -59.9(2) . . . . ? N11' Pt1 Pd1 N2' 119.8(2) . . . . ? O11 Pt1 Pd1 N2' -10.3(14) . . . . ? N1' Pt1 Pd1 N2 -153.1(2) . . . . ? N1 Pt1 Pd1 N2 27.2(2) . . . . ? N11 Pt1 Pd1 N2 120.5(2) . . . . ? N11' Pt1 Pd1 N2 -59.7(2) . . . . ? O11 Pt1 Pd1 N2 170.2(14) . . . . ? N1' Pt1 Pd1 O1W 78.9(25) . . . . ? N1 Pt1 Pd1 O1W -100.8(25) . . . . ? N11 Pt1 Pd1 O1W -7.5(25) . . . . ? N11' Pt1 Pd1 O1W 172.3(25) . . . . ? O11 Pt1 Pd1 O1W 42.2(29) . . . . ? N1' Pt1 Pd1 Pd2 -108.80(15) . . . . ? N1 Pt1 Pd1 Pd2 71.47(15) . . . . ? N11 Pt1 Pd1 Pd2 164.8(2) . . . . ? N11' Pt1 Pd1 Pd2 -15.4(2) . . . . ? O11 Pt1 Pd1 Pd2 -145.5(14) . . . . ? N1' Pt1 Pd1 Pd3 69.28(15) . . . . ? N1 Pt1 Pd1 Pd3 -110.45(15) . . . . ? N11 Pt1 Pd1 Pd3 -17.1(2) . . . . ? N11' Pt1 Pd1 Pd3 162.6(2) . . . . ? O11 Pt1 Pd1 Pd3 32.5(14) . . . . ? N2' Pd1 Pd2 N11' -54.5(3) . . . . ? N2 Pd1 Pd2 N11' 109.7(3) . . . . ? O1W Pd1 Pd2 N11' -164.4(2) . . . . ? Pt1 Pd1 Pd2 N11' 16.0(2) . . . . ? Pd3 Pd1 Pd2 N11' 11.6(2) . . . . ? N2' Pd1 Pd2 N22 21.4(3) . . . . ? N2 Pd1 Pd2 N22 -174.4(3) . . . . ? O1W Pd1 Pd2 N22 -88.5(3) . . . . ? Pt1 Pd1 Pd2 N22 91.9(2) . . . . ? Pd3 Pd1 Pd2 N22 87.5(2) . . . . ? N2' Pd1 Pd2 N21 120.4(3) . . . . ? N2 Pd1 Pd2 N21 -75.4(3) . . . . ? O1W Pd1 Pd2 N21 10.5(2) . . . . ? Pt1 Pd1 Pd2 N21 -169.1(2) . . . . ? Pd3 Pd1 Pd2 N21 -173.5(2) . . . . ? N2' Pd1 Pd2 N2 -164.2(3) . . . . ? N2 Pd1 Pd2 N2 0.000(3) . . . . ? O1W Pd1 Pd2 N2 85.9(3) . . . . ? Pt1 Pd1 Pd2 N2 -93.6(2) . . . . ? Pd3 Pd1 Pd2 N2 -98.0(2) . . . . ? N2' Pd1 Pd3 N32 -174.9(3) . . . . ? N2 Pd1 Pd3 N32 21.6(3) . . . . ? O1W Pd1 Pd3 N32 -90.0(3) . . . . ? Pt1 Pd1 Pd3 N32 89.5(2) . . . . ? Pd2 Pd1 Pd3 N32 93.9(2) . . . . ? N2' Pd1 Pd3 N11 113.3(3) . . . . ? N2 Pd1 Pd3 N11 -50.2(3) . . . . ? O1W Pd1 Pd3 N11 -161.8(2) . . . . ? Pt1 Pd1 Pd3 N11 17.7(2) . . . . ? Pd2 Pd1 Pd3 N11 22.1(2) . . . . ? N2' Pd1 Pd3 N31 -66.9(3) . . . . ? N2 Pd1 Pd3 N31 129.6(3) . . . . ? O1W Pd1 Pd3 N31 18.0(2) . . . . ? Pt1 Pd1 Pd3 N31 -162.5(2) . . . . ? Pd2 Pd1 Pd3 N31 -158.1(2) . . . . ? N2' Pd1 Pd3 N2' 0.000(4) . . . . ? N2 Pd1 Pd3 N2' -163.5(3) . . . . ? O1W Pd1 Pd3 N2' 84.9(3) . . . . ? Pt1 Pd1 Pd3 N2' -95.6(2) . . . . ? Pd2 Pd1 Pd3 N2' -91.2(2) . . . . ? N22 Pd2 N11' Pt1 -160.5(3) . . . . ? N21 Pd2 N11' Pt1 -126.9(25) . . . . ? N2 Pd2 N11' Pt1 19.7(3) . . . . ? Pd1 Pd2 N11' Pt1 -20.8(2) . . . . ? N1' Pt1 N11' Pd2 111.8(3) . . . . ? N1 Pt1 N11' Pd2 -63.3(3) . . . . ? N11 Pt1 N11' Pd2 27.7(29) . . . . ? O11 Pt1 N11' Pd2 -158.7(3) . . . . ? Pd1 Pt1 N11' Pd2 24.5(3) . . . . ? N1' Pt1 N11 Pd3 -60.0(3) . . . . ? N1 Pt1 N11 Pd3 115.1(3) . . . . ? N11' Pt1 N11 Pd3 24.4(29) . . . . ? O11 Pt1 N11 Pd3 -149.2(3) . . . . ? Pd1 Pt1 N11 Pd3 27.6(2) . . . . ? N32 Pd3 N11 Pt1 -163.7(3) . . . . ? N31 Pd3 N11 Pt1 158.8(18) . . . . ? N2' Pd3 N11 Pt1 14.6(3) . . . . ? Pd1 Pd3 N11 Pt1 -23.0(2) . . . . ? N11' Pd2 N21 C21 -52.6(28) . . . . ? N22 Pd2 N21 C21 -18.7(4) . . . . ? N2 Pd2 N21 C21 160.9(4) . . . . ? Pd1 Pd2 N21 C21 -157.3(4) . . . . ? Pd2 N21 C21 C22 42.9(6) . . . . ? N21 C21 C22 N22 -51.9(7) . . . . ? C21 C22 N22 Pd2 36.1(6) . . . . ? N11' Pd2 N22 C22 167.7(4) . . . . ? N21 Pd2 N22 C22 -9.5(4) . . . . ? N2 Pd2 N22 C22 -15.5(33) . . . . ? Pd1 Pd2 N22 C22 98.4(4) . . . . ? N32 Pd3 N31 C31 -14.5(4) . . . . ? N11 Pd3 N31 C31 23.2(21) . . . . ? N2' Pd3 N31 C31 167.4(4) . . . . ? Pd1 Pd3 N31 C31 -154.8(4) . . . . ? Pd3 N31 C31 C32 42.0(6) . . . . ? N31 C31 C32 N32 -56.2(7) . . . . ? C31 C32 N32 Pd3 42.2(6) . . . . ? N11 Pd3 N32 C32 167.9(4) . . . . ? N31 Pd3 N32 C32 -15.9(4) . . . . ? N2' Pd3 N32 C32 18.0(41) . . . . ? Pd1 Pd3 N32 C32 102.6(4) . . . . ? N1' Pt1 N1 C2 -25.4(27) . . . . ? N11 Pt1 N1 C2 -109.9(5) . . . . ? N11' Pt1 N1 C2 65.4(5) . . . . ? O11 Pt1 N1 C2 160.3(5) . . . . ? Pd1 Pt1 N1 C2 -22.3(5) . . . . ? N1' Pt1 N1 C6 153.0(23) . . . . ? N11 Pt1 N1 C6 68.5(5) . . . . ? N11' Pt1 N1 C6 -116.1(5) . . . . ? O11 Pt1 N1 C6 -21.3(5) . . . . ? Pd1 Pt1 N1 C6 156.2(5) . . . . ? N2' Pd1 N2 C2 -42.1(13) . . . . ? O1W Pd1 N2 C2 137.7(5) . . . . ? Pt1 Pd1 N2 C2 -39.9(4) . . . . ? Pd2 Pd1 N2 C2 -118.7(5) . . . . ? Pd3 Pd1 N2 C2 25.4(6) . . . . ? N2' Pd1 N2 Pd2 76.7(11) . . . . ? O1W Pd1 N2 Pd2 -103.6(2) . . . . ? Pt1 Pd1 N2 Pd2 78.8(2) . . . . ? Pd2 Pd1 N2 Pd2 0.000(2) . . . . ? Pd3 Pd1 N2 Pd2 144.10(10) . . . . ? N11' Pd2 N2 C2 55.1(5) . . . . ? N22 Pd2 N2 C2 -121.8(30) . . . . ? N21 Pd2 N2 C2 -127.7(5) . . . . ? Pd1 Pd2 N2 C2 120.3(5) . . . . ? N11' Pd2 N2 Pd1 -65.2(2) . . . . ? N22 Pd2 N2 Pd1 118.0(30) . . . . ? N21 Pd2 N2 Pd1 112.0(2) . . . . ? Pd1 Pd2 N2 Pd1 0.000(2) . . . . ? C6 N1 C2 N2 179.4(6) . . . . ? Pt1 N1 C2 N2 -2.2(8) . . . . ? C6 N1 C2 C3 -0.6(10) . . . . ? Pt1 N1 C2 C3 177.8(5) . . . . ? Pd1 N2 C2 N1 34.2(7) . . . . ? Pd2 N2 C2 N1 -71.7(7) . . . . ? Pd1 N2 C2 C3 -145.8(5) . . . . ? Pd2 N2 C2 C3 108.3(6) . . . . ? N1 C2 C3 C4 1.6(10) . . . . ? N2 C2 C3 C4 -178.3(6) . . . . ? C2 C3 C4 C5 -1.7(11) . . . . ? C3 C4 C5 C6 0.7(10) . . . . ? C2 N1 C6 C5 -0.4(10) . . . . ? Pt1 N1 C6 C5 -178.8(5) . . . . ? C4 C5 C6 N1 0.3(10) . . . . ? N1 Pt1 N1' C6' 162.7(22) . . . . ? N11 Pt1 N1' C6' -112.5(5) . . . . ? N11' Pt1 N1' C6' 72.1(5) . . . . ? O11 Pt1 N1' C6' -23.0(5) . . . . ? Pd1 Pt1 N1' C6' 159.6(5) . . . . ? N1 Pt1 N1' C2' -15.9(27) . . . . ? N11 Pt1 N1' C2' 68.9(5) . . . . ? N11' Pt1 N1' C2' -106.5(5) . . . . ? O11 Pt1 N1' C2' 158.4(5) . . . . ? Pd1 Pt1 N1' C2' -19.1(5) . . . . ? C6' N1' C2' N2' 174.9(6) . . . . ? Pt1 N1' C2' N2' -6.5(8) . . . . ? C6' N1' C2' C3' -1.4(10) . . . . ? Pt1 N1' C2' C3' 177.3(5) . . . . ? N1' C2' N2' Pd1 37.5(8) . . . . ? C3' C2' N2' Pd1 -146.4(6) . . . . ? N1' C2' N2' Pd3 -70.7(7) . . . . ? C3' C2' N2' Pd3 105.4(7) . . . . ? N2 Pd1 N2' C2' -38.7(14) . . . . ? O1W Pd1 N2' C2' 141.6(5) . . . . ? Pt1 Pd1 N2' C2' -40.8(5) . . . . ? Pd2 Pd1 N2' C2' 26.9(6) . . . . ? Pd3 Pd1 N2' C2' -117.9(6) . . . . ? N2 Pd1 N2' Pd3 79.2(11) . . . . ? O1W Pd1 N2' Pd3 -100.5(2) . . . . ? Pt1 Pd1 N2' Pd3 77.1(2) . . . . ? Pd2 Pd1 N2' Pd3 144.83(11) . . . . ? Pd3 Pd1 N2' Pd3 0.000(3) . . . . ? N32 Pd3 N2' C2' -150.8(37) . . . . ? N11 Pd3 N2' C2' 59.3(5) . . . . ? N31 Pd3 N2' C2' -117.1(5) . . . . ? Pd1 Pd3 N2' C2' 120.7(6) . . . . ? N32 Pd3 N2' Pd1 88.5(40) . . . . ? N11 Pd3 N2' Pd1 -61.5(2) . . . . ? N31 Pd3 N2' Pd1 122.2(2) . . . . ? Pd1 Pd3 N2' Pd1 0.000(3) . . . . ? N1' C2' C3' C4' -0.3(10) . . . . ? N2' C2' C3' C4' -176.3(7) . . . . ? C2' C3' C4' C5' 1.8(11) . . . . ? C3' C4' C5' C6' -1.7(11) . . . . ? C2' N1' C6' C5' 1.5(10) . . . . ? Pt1 N1' C6' C5' -177.1(5) . . . . ? C4' C5' C6' N1' 0.0(11) . . . . ? O12 N10 O11 Pt1 174.0(4) . . . . ? O13 N10 O11 Pt1 -4.5(8) . . . . ? N1' Pt1 O11 N10 132.1(5) . . . . ? N1 Pt1 O11 N10 -48.4(5) . . . . ? N11 Pt1 O11 N10 -141.6(5) . . . . ? N11' Pt1 O11 N10 38.9(5) . . . . ? Pd1 Pt1 O11 N10 168.8(11) . . . . ? O42 N40 O43 O43A -120.7(18) . . . . ? O41 N40 O43 O43A 72.6(21) . . . . ? O43A N40 O43 O43A 0.0 . . . . ? N40 O43 O43A N40 0.0 . . . . ? O42 N40 O43A O43 75.2(20) . . . . ? O41 N40 O43A O43 -123.7(18) . . . . ? O43 N40 O43A O43 0.0 . . . . ? _refine_diff_density_max 0.780 _refine_diff_density_min -1.020 _refine_diff_density_rms 0.113 #===END data_2 _publ_contact_author_name 'Prof. Bernhard Lippert' _publ_contact_author_address ; Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_email 'lippert@pop.uni-dortmund.de' _publ_contact_author_fax 'Int. code + (231) 755-3797' _publ_contact_author_phone '231 755-3840' _publ_contact_letter ? _publ_requested_journal 'Dalton Transactions' _publ_title ; Ready formation of water-stable Pt(II)-(-NH2)-Pd(II) species through combination of trans-[(NH3)2 Pt(II)L2] (L = N,N'-hterocycle) and [enPd(H2O)2]2+ ; _publ_author_address ; Alexandra Fichtel, Eva Freisinger, Bettina Beck, Bernhard Lippert' Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C5 H15 Br N5 O Pd Pt0.50' _chemical_formula_weight 445.07 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.0470(10) _cell_length_b 9.580(2) _cell_length_c 13.568(3) _cell_angle_alpha 105.65(3) _cell_angle_beta 98.84(3) _cell_angle_gamma 98.60(3) _cell_volume 611.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2464 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 27.10 _exptl_crystal_description stick _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.417 _exptl_crystal_density_method ? _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 10.452 _exptl_absorpt_correction_type SCALEPACK _exptl_absorpt_correction_T_min 0.0674 _exptl_absorpt_correction_T_max 0.6799 _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 'Enraf-Nonius-KappaCCD' _diffrn_measurement_method ; 360 frames via \w-rotation (\D\w\=1\%) and two times 60s per frame ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2464 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.10 _reflns_number_total 2464 _reflns_number_observed 2070 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, Netherlands)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 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^)+(0.0587P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'refU' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0069(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2455 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_obs 0.0325 _refine_ls_wR_factor_all 0.0944 _refine_ls_wR_factor_obs 0.0827 _refine_ls_goodness_of_fit_all 1.018 _refine_ls_goodness_of_fit_obs 1.069 _refine_ls_restrained_S_all 1.116 _refine_ls_restrained_S_obs 1.069 _refine_ls_shift/esd_max -0.029 _refine_ls_shift/esd_mean 0.004 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 Pt1 Pt 0.5000 0.0000 0.0000 0.03600(14) Uani 1 d S . N11 N 0.2518(11) 0.1513(6) 0.0209(4) 0.0406(11) Uani 1 d . . H11A H 0.3398(11) 0.2343(6) 0.0117(4) 0.045(13) Uiso 1 calc R . H11B H 0.1012(11) 0.1157(6) -0.0303(4) 0.045(13) Uiso 1 calc R . Pd1 Pd 0.12825(9) 0.20894(5) 0.15775(3) 0.0404(2) Uani 1 d . . N21 N -0.0053(14) 0.2819(8) 0.2968(5) 0.061(2) Uani 1 d . . H21A H -0.1208(14) 0.2072(8) 0.3058(5) 0.090(11) Uiso 1 calc R . H21B H 0.1386(14) 0.3121(8) 0.3510(5) 0.090(11) Uiso 1 calc R . N22 N 0.0130(11) 0.3924(6) 0.1325(5) 0.0508(13) Uani 1 d . . H22A H 0.1363(11) 0.4367(6) 0.1034(5) 0.090(11) Uiso 1 calc R . H22B H -0.1503(11) 0.3668(6) 0.0881(5) 0.090(11) Uiso 1 calc R . C21 C -0.1468(17) 0.4063(9) 0.2934(6) 0.059(2) Uani 1 d . . H21C H -0.1376(17) 0.4685(9) 0.3638(6) 0.090(11) Uiso 1 calc R . H21D H -0.3378(17) 0.3683(9) 0.2598(6) 0.090(11) Uiso 1 calc R . C22 C -0.0061(18) 0.4952(9) 0.2324(6) 0.063(2) Uani 1 d . . H22C H -0.1104(18) 0.5681(9) 0.2197(6) 0.090(11) Uiso 1 calc R . H22D H 0.1754(18) 0.5468(9) 0.2718(6) 0.090(11) Uiso 1 calc R . N1 N 0.4329(10) -0.0352(6) 0.1344(4) 0.0412(11) Uani 1 d . . N2 N 0.2697(12) 0.0395(6) 0.1916(4) 0.0465(13) Uani 1 d . . C3 C 0.2684(17) -0.0089(9) 0.2763(6) 0.060(2) Uani 1 d . . H3 H 0.1735(17) 0.0242(9) 0.3288(6) 0.058(12) Uiso 1 calc R . C4 C 0.4230(17) -0.1109(9) 0.2741(6) 0.059(2) Uani 1 d . . H4 H 0.4545(17) -0.1613(9) 0.3232(6) 0.058(12) Uiso 1 calc R . C5 C 0.5248(16) -0.1262(8) 0.1856(5) 0.054(2) Uani 1 d . . H5 H 0.6407(16) -0.1899(8) 0.1638(5) 0.058(12) Uiso 1 calc R . O1W O 0.0135(18) 0.8529(10) 0.4953(7) 0.120(3) Uani 1 d . . Br1 Br 0.5000 -0.5000 0.0000 0.0544(3) Uani 1 d S . Br2 Br 0.4745(3) 0.6350(2) 0.48973(13) 0.0667(4) Uani 0.50 d P . 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 Pt1 0.0365(2) 0.0351(2) 0.0370(2) 0.01322(14) 0.00761(12) 0.00467(12) N11 0.041(3) 0.041(3) 0.041(3) 0.014(2) 0.005(2) 0.012(2) Pd1 0.0379(3) 0.0441(3) 0.0411(3) 0.0141(2) 0.0103(2) 0.0089(2) N21 0.059(4) 0.076(4) 0.053(4) 0.020(3) 0.020(3) 0.021(3) N22 0.041(3) 0.057(3) 0.060(4) 0.021(3) 0.014(2) 0.014(2) C21 0.057(5) 0.056(4) 0.058(5) 0.005(4) 0.007(3) 0.016(3) C22 0.073(5) 0.057(4) 0.059(5) 0.007(4) 0.024(4) 0.018(4) N1 0.040(3) 0.040(3) 0.045(3) 0.014(2) 0.011(2) 0.008(2) N2 0.054(3) 0.048(3) 0.049(3) 0.024(3) 0.020(2) 0.016(2) C3 0.079(5) 0.071(5) 0.046(4) 0.033(4) 0.026(4) 0.024(4) C4 0.083(6) 0.062(4) 0.044(4) 0.027(3) 0.019(4) 0.026(4) C5 0.073(5) 0.051(4) 0.047(4) 0.025(3) 0.009(3) 0.021(3) O1W 0.113(6) 0.118(7) 0.141(8) 0.050(6) 0.042(5) 0.025(5) Br1 0.0496(6) 0.0475(5) 0.0758(7) 0.0307(5) 0.0161(5) 0.0133(4) Br2 0.0567(9) 0.0767(10) 0.0644(10) 0.0203(8) 0.0086(7) 0.0119(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 Pt1 N1 2.010(5) 2_655 ? Pt1 N1 2.010(5) . ? Pt1 N11 2.044(5) . ? Pt1 N11 2.044(5) 2_655 ? N11 Pd1 2.011(5) . ? N11 H11A 0.90 . ? N11 H11B 0.90 . ? Pd1 N2 2.001(5) . ? Pd1 N22 2.028(5) . ? Pd1 N21 2.079(6) . ? N21 C21 1.486(9) . ? N21 H21A 0.90 . ? N21 H21B 0.90 . ? N22 C22 1.472(9) . ? N22 H22A 0.90 . ? N22 H22B 0.90 . ? C21 C22 1.515(12) . ? C21 H21C 0.97 . ? C21 H21D 0.97 . ? C22 H22C 0.97 . ? C22 H22D 0.97 . ? N1 C5 1.344(8) . ? N1 N2 1.366(7) . ? N2 C3 1.351(8) . ? C3 C4 1.336(10) . ? C3 H3 0.93 . ? C4 C5 1.358(10) . ? C4 H4 0.93 . ? C5 H5 0.93 . ? Br2 Br2 2.721(4) 2_666 ? 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 Pt1 N1 180.0 2_655 . ? N1 Pt1 N11 92.0(2) 2_655 . ? N1 Pt1 N11 88.0(2) . . ? N1 Pt1 N11 88.0(2) 2_655 2_655 ? N1 Pt1 N11 92.0(2) . 2_655 ? N11 Pt1 N11 180.0 . 2_655 ? Pd1 N11 Pt1 118.5(2) . . ? Pd1 N11 H11A 107.7(2) . . ? Pt1 N11 H11A 107.68(15) . . ? Pd1 N11 H11B 107.68(15) . . ? Pt1 N11 H11B 107.68(15) . . ? H11A N11 H11B 107.1 . . ? N2 Pd1 N11 88.4(2) . . ? N2 Pd1 N22 175.1(2) . . ? N11 Pd1 N22 93.0(2) . . ? N2 Pd1 N21 95.6(2) . . ? N11 Pd1 N21 176.0(2) . . ? N22 Pd1 N21 83.0(2) . . ? C21 N21 Pd1 109.4(5) . . ? C21 N21 H21A 109.8(4) . . ? Pd1 N21 H21A 109.8(2) . . ? C21 N21 H21B 109.8(4) . . ? Pd1 N21 H21B 109.8(2) . . ? H21A N21 H21B 108.2 . . ? C22 N22 Pd1 109.5(5) . . ? C22 N22 H22A 109.8(4) . . ? Pd1 N22 H22A 109.8(2) . . ? C22 N22 H22B 109.8(4) . . ? Pd1 N22 H22B 109.8(2) . . ? H22A N22 H22B 108.2 . . ? N21 C21 C22 108.2(6) . . ? N21 C21 H21C 110.1(4) . . ? C22 C21 H21C 110.1(4) . . ? N21 C21 H21D 110.1(4) . . ? C22 C21 H21D 110.1(5) . . ? H21C C21 H21D 108.4 . . ? N22 C22 C21 108.2(6) . . ? N22 C22 H22C 110.1(4) . . ? C21 C22 H22C 110.1(4) . . ? N22 C22 H22D 110.1(4) . . ? C21 C22 H22D 110.1(5) . . ? H22C C22 H22D 108.4 . . ? C5 N1 N2 107.2(5) . . ? C5 N1 Pt1 131.2(5) . . ? N2 N1 Pt1 121.6(4) . . ? C3 N2 N1 106.7(5) . . ? C3 N2 Pd1 130.6(5) . . ? N1 N2 Pd1 121.9(4) . . ? C4 C3 N2 110.4(6) . . ? C4 C3 H3 124.8(4) . . ? N2 C3 H3 124.8(4) . . ? C3 C4 C5 106.0(6) . . ? C3 C4 H4 127.0(4) . . ? C5 C4 H4 127.0(4) . . ? N1 C5 C4 109.7(6) . . ? N1 C5 H5 125.2(4) . . ? C4 C5 H5 125.2(4) . . ? 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 Pt1 N11 Pd1 -171.2(3) 2_655 . . . ? N1 Pt1 N11 Pd1 8.8(3) . . . . ? N11 Pt1 N11 Pd1 -103.7(1000) 2_655 . . . ? Pt1 N11 Pd1 N2 -11.8(3) . . . . ? Pt1 N11 Pd1 N22 163.5(3) . . . . ? Pt1 N11 Pd1 N21 159.9(32) . . . . ? N2 Pd1 N21 C21 -175.7(5) . . . . ? N11 Pd1 N21 C21 12.7(36) . . . . ? N22 Pd1 N21 C21 9.1(5) . . . . ? N2 Pd1 N22 C22 -54.9(26) . . . . ? N11 Pd1 N22 C22 -160.8(5) . . . . ? N21 Pd1 N22 C22 18.9(5) . . . . ? Pd1 N21 C21 C22 -34.4(7) . . . . ? Pd1 N22 C22 C21 -43.0(7) . . . . ? N21 C21 C22 N22 51.1(8) . . . . ? N1 Pt1 N1 C5 -40.4(10) 2_655 . . . ? N11 Pt1 N1 C5 180.0(6) . . . . ? N11 Pt1 N1 C5 0.0(6) 2_655 . . . ? N1 Pt1 N1 N2 139.4(5) 2_655 . . . ? N11 Pt1 N1 N2 -0.2(5) . . . . ? N11 Pt1 N1 N2 179.8(5) 2_655 . . . ? C5 N1 N2 C3 0.1(7) . . . . ? Pt1 N1 N2 C3 -179.7(5) . . . . ? C5 N1 N2 Pd1 171.0(5) . . . . ? Pt1 N1 N2 Pd1 -8.9(7) . . . . ? N11 Pd1 N2 C3 -179.3(7) . . . . ? N22 Pd1 N2 C3 74.6(26) . . . . ? N21 Pd1 N2 C3 1.3(7) . . . . ? N11 Pd1 N2 N1 12.2(5) . . . . ? N22 Pd1 N2 N1 -93.9(24) . . . . ? N21 Pd1 N2 N1 -167.2(5) . . . . ? N1 N2 C3 C4 -0.3(9) . . . . ? Pd1 N2 C3 C4 -170.1(6) . . . . ? N2 C3 C4 C5 0.3(10) . . . . ? N2 N1 C5 C4 0.1(8) . . . . ? Pt1 N1 C5 C4 179.9(5) . . . . ? C3 C4 C5 N1 -0.2(10) . . . . ? _refine_diff_density_max 1.336 _refine_diff_density_min -1.339 _refine_diff_density_rms 0.156 #===END data_4b _publ_contact_author_name 'Prof. Bernhard Lippert' _publ_contact_author_address ; Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_email 'lippert@pop.uni-dortmund.de' _publ_contact_author_fax 'Int. code + (231) 755-3797' _publ_contact_author_phone '231 755-3840' _publ_contact_letter ? _publ_requested_journal 'Dalton Transactions' _publ_title ; Ready formation of water-stable Pt(II)-(-NH2)-Pd(II) species through combination of trans-[(NH3)2 Pt(II)L2] (L = N,N'-hterocycle) and [enPd(H2O)2]2+ ; _publ_author_address ; Alexandra Fichtel, Eva Freisinger, Bettina Beck, Bernhard Lippert' Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ; 'trans-[(NH3)2Pt{(2-ampy-N2)Pd(en)}2PdCl](NO3)3 * 1.3H2O' ; _chemical_formula_analytical ? _chemical_formula_sum 'C14 H32.60 Cl N13 O10.30 Pd3 Pt' _chemical_formula_weight 1097.67 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.046(2) _cell_length_b 12.056(2) _cell_length_c 12.971(3) _cell_angle_alpha 101.93(3) _cell_angle_beta 102.74(3) _cell_angle_gamma 112.30(3) _cell_volume 1475.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4835 _cell_measurement_theta_min 4.54 _cell_measurement_theta_max 24.98 _exptl_crystal_description stick _exptl_crystal_colour brown _exptl_crystal_size_max 0.88 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.470 _exptl_crystal_density_method ? _exptl_crystal_F_000 1046 _exptl_absorpt_coefficient_mu 6.685 _exptl_absorpt_correction_type SCALEPACK _exptl_absorpt_correction_T_min 0.0670 _exptl_absorpt_correction_T_max 0.4770 _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 'Enraf-Nonius-KappaCCD' _diffrn_measurement_method ; 360 frames via \w-rotation (\D\w\=1\%) and two times 20s per frame ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4835 _diffrn_reflns_av_R_equivalents 0.066 _diffrn_reflns_av_sigmaI/netI 0.1165 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.54 _diffrn_reflns_theta_max 24.98 _reflns_number_total 4835 _reflns_number_observed 2893 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, Netherlands)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 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^)+(0.0208P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ; refU, except H11a to H11d, H2 and H2' noref ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4833 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_obs 0.0369 _refine_ls_wR_factor_all 0.0667 _refine_ls_wR_factor_obs 0.0597 _refine_ls_goodness_of_fit_all 0.847 _refine_ls_goodness_of_fit_obs 1.021 _refine_ls_restrained_S_all 0.860 _refine_ls_restrained_S_obs 1.021 _refine_ls_shift/esd_max -0.001 _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 Pt1 Pt 0.65839(4) 0.21581(4) 0.35802(3) 0.03261(13) Uani 1 d . . Pd1 Pd 0.48775(7) 0.25699(6) 0.23272(5) 0.0340(2) Uani 1 d . . Pd3 Pd 0.31336(7) 0.05978(6) 0.30237(5) 0.0347(2) Uani 1 d . . Pd2 Pd 0.76449(8) 0.45479(6) 0.24504(5) 0.0380(2) Uani 1 d . . Cl1 Cl 0.3180(3) 0.2877(3) 0.1158(2) 0.0728(9) Uani 1 d . . N11 N 0.5019(7) 0.1028(6) 0.4056(5) 0.040(2) Uani 1 d . . H11A H 0.5091(7) 0.0309(6) 0.4055(5) 0.048 Uiso 1 calc R . H11B H 0.5114(7) 0.1433(6) 0.4757(5) 0.048 Uiso 1 calc R . N11' N 0.8088(7) 0.3272(6) 0.3057(5) 0.044(2) Uani 1 d . . H11C H 0.8888(7) 0.3692(6) 0.3635(5) 0.053 Uiso 1 calc R . H11D H 0.8221(7) 0.2768(6) 0.2522(5) 0.053 Uiso 1 calc R . N21 N 0.2235(7) 0.0545(6) 0.4248(5) 0.039(2) Uani 1 d . . H21A H 0.2010(7) -0.0204(6) 0.4373(5) 0.049(10) Uiso 1 calc R . H21B H 0.2828(7) 0.1166(6) 0.4888(5) 0.049(10) Uiso 1 calc R . C21 C 0.0972(10) 0.0718(9) 0.3860(8) 0.049(3) Uani 1 d . . H21C H 0.1221(10) 0.1605(9) 0.3957(8) 0.056(10) Uiso 1 calc R . H21D H 0.0365(10) 0.0438(9) 0.4287(8) 0.056(10) Uiso 1 calc R . C22 C 0.0247(10) -0.0059(9) 0.2638(7) 0.053(3) Uani 1 d . . H22A H -0.0104(10) -0.0954(9) 0.2554(7) 0.056(10) Uiso 1 calc R . H22B H -0.0529(10) 0.0104(9) 0.2334(7) 0.056(10) Uiso 1 calc R . N22 N 0.1253(7) 0.0291(7) 0.2029(5) 0.050(2) Uani 1 d . . H22C H 0.1316(7) 0.0996(7) 0.1864(5) 0.049(10) Uiso 1 calc R . H22D H 0.0969(7) -0.0337(7) 0.1387(5) 0.049(10) Uiso 1 calc R . N31 N 0.8983(8) 0.4726(7) 0.1562(6) 0.047(2) Uani 1 d . . H31A H 0.9857(8) 0.5262(7) 0.2009(6) 0.049(10) Uiso 1 calc R . H31B H 0.8953(8) 0.3969(7) 0.1260(6) 0.049(10) Uiso 1 calc R . C31 C 0.8547(11) 0.5216(9) 0.0690(8) 0.059(3) Uani 1 d . . H31C H 0.7699(11) 0.4563(9) 0.0117(8) 0.056(10) Uiso 1 calc R . H31D H 0.9258(11) 0.5493(9) 0.0347(8) 0.056(10) Uiso 1 calc R . C32 C 0.8315(12) 0.6301(10) 0.1219(9) 0.072(3) Uani 1 d . . H32A H 0.7965(12) 0.6624(10) 0.0656(9) 0.056(10) Uiso 1 calc R . H32B H 0.9179(12) 0.6979(10) 0.1753(9) 0.056(10) Uiso 1 calc R . N32 N 0.7280(9) 0.5842(7) 0.1799(6) 0.063(3) Uani 1 d . . H32C H 0.6412(9) 0.5481(7) 0.1312(6) 0.049(10) Uiso 1 calc R . H32D H 0.7374(9) 0.6495(7) 0.2347(6) 0.049(10) Uiso 1 calc R . N10 N 0.9526(11) 0.2468(9) 0.5379(7) 0.052(2) Uani 1 d . . O11 O 0.8273(7) 0.1669(6) 0.4833(5) 0.046(2) Uani 1 d . . O12 O 0.9982(8) 0.3525(8) 0.5269(6) 0.081(2) Uani 1 d . . O13 O 1.0256(8) 0.2174(7) 0.6023(6) 0.077(2) Uani 1 d . . N1 N 0.6961(7) 0.3752(6) 0.4717(5) 0.033(2) Uani 1 d . . C2 C 0.6628(9) 0.4616(8) 0.4387(7) 0.038(2) Uani 1 d . . N2 N 0.6184(7) 0.4443(6) 0.3253(5) 0.036(2) Uani 1 d . . H2 H 0.5714 0.5042 0.3060 0.043 Uiso 1 d . . C3 C 0.6751(10) 0.5684(9) 0.5154(7) 0.044(3) Uani 1 d . . H3 H 0.6533(10) 0.6277(9) 0.4907(7) 0.033(8) Uiso 1 calc R . C4 C 0.7193(11) 0.5852(9) 0.6264(8) 0.054(3) Uani 1 d . . H4 H 0.7262(11) 0.6554(9) 0.6780(8) 0.033(8) Uiso 1 calc R . C5 C 0.7542(10) 0.4968(9) 0.6626(7) 0.056(3) Uani 1 d . . H5 H 0.7858(10) 0.5073(9) 0.7383(7) 0.033(8) Uiso 1 calc R . C6 C 0.7405(9) 0.3945(9) 0.5838(7) 0.046(3) Uani 1 d . . H6 H 0.7625(9) 0.3347(9) 0.6076(7) 0.033(8) Uiso 1 calc R . N1' N 0.5985(7) 0.0561(6) 0.2313(5) 0.032(2) Uani 1 d . . C2' C 0.4708(9) 0.0055(8) 0.1549(7) 0.032(2) Uani 1 d . . N2' N 0.3875(7) 0.0642(6) 0.1669(5) 0.036(2) Uani 1 d . . H2' H 0.3116 0.0338 0.1215 0.043 Uiso 1 d . . C3' C 0.4289(10) -0.1031(8) 0.0647(7) 0.039(2) Uani 1 d . . H3' H 0.3414(10) -0.1388(8) 0.0113(7) 0.033(8) Uiso 1 calc R . C4' C 0.5177(10) -0.1567(8) 0.0551(7) 0.044(3) Uani 1 d . . H4' H 0.4894(10) -0.2293(8) -0.0043(7) 0.033(8) Uiso 1 calc R . C5' C 0.6465(10) -0.1040(8) 0.1321(7) 0.045(3) Uani 1 d . . H5' H 0.7081(10) -0.1383(8) 0.1254(7) 0.033(8) Uiso 1 calc R . C6' C 0.6832(10) 0.0015(8) 0.2204(7) 0.042(2) Uani 1 d . . H6' H 0.7699(10) 0.0366(8) 0.2747(7) 0.033(8) Uiso 1 calc R . N20 N 0.9323(9) 0.1827(9) 0.0734(7) 0.053(2) Uani 1 d . . O21 O 0.9703(8) 0.2288(7) 0.1755(6) 0.083(3) Uani 1 d . . O22 O 0.9046(8) 0.0703(7) 0.0314(6) 0.078(3) Uani 1 d . . O23 O 0.9142(9) 0.2436(7) 0.0105(7) 0.093(3) Uani 1 d . . N30 N 0.5228(11) 0.7391(8) 0.3013(7) 0.058(3) Uani 1 d . . O31 O 0.4946(8) 0.8204(7) 0.3495(6) 0.079(3) Uani 1 d . . O32 O 0.6248(10) 0.7302(8) 0.3464(6) 0.092(3) Uani 1 d . . O33 O 0.4465(9) 0.6653(8) 0.2079(7) 0.112(3) Uani 1 d . . O1W O 0.1825(8) 0.7188(7) 0.2051(6) 0.090(3) Uani 1 d . . O2W O 0.4667(29) 0.5184(25) 0.0555(21) 0.100(9) Uiso 0.30 d P . 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 Pt1 0.0376(3) 0.0334(2) 0.0285(2) 0.0088(2) 0.0105(2) 0.0184(2) Pd1 0.0406(5) 0.0392(4) 0.0285(4) 0.0109(3) 0.0123(3) 0.0236(4) Pd3 0.0384(5) 0.0377(4) 0.0310(4) 0.0095(3) 0.0143(4) 0.0193(4) Pd2 0.0474(5) 0.0340(4) 0.0333(4) 0.0115(3) 0.0137(4) 0.0184(4) Cl1 0.089(3) 0.091(2) 0.053(2) 0.018(2) 0.021(2) 0.058(2) N11 0.051(6) 0.042(5) 0.024(4) 0.000(3) 0.007(4) 0.027(4) N11' 0.043(5) 0.049(5) 0.039(4) 0.005(4) 0.009(4) 0.027(4) N21 0.038(5) 0.041(5) 0.038(4) 0.014(4) 0.014(4) 0.015(4) C21 0.045(7) 0.057(7) 0.065(7) 0.030(6) 0.027(6) 0.032(6) C22 0.038(7) 0.069(7) 0.055(6) 0.016(6) 0.013(5) 0.030(6) N22 0.052(6) 0.062(6) 0.031(4) 0.001(4) 0.016(4) 0.026(5) N31 0.057(6) 0.039(5) 0.053(5) 0.024(4) 0.026(4) 0.019(5) C31 0.076(9) 0.058(7) 0.055(6) 0.022(6) 0.035(6) 0.032(7) C32 0.101(11) 0.060(8) 0.074(8) 0.043(7) 0.040(8) 0.037(8) N32 0.104(8) 0.060(6) 0.052(5) 0.029(5) 0.038(5) 0.052(6) N10 0.067(8) 0.047(6) 0.057(6) 0.027(5) 0.025(6) 0.033(6) O11 0.022(4) 0.042(4) 0.061(4) 0.024(3) -0.008(4) 0.009(4) O12 0.063(6) 0.064(5) 0.081(5) 0.032(5) -0.018(4) 0.011(5) O13 0.085(7) 0.084(6) 0.060(5) 0.023(4) -0.002(4) 0.048(5) N1 0.033(5) 0.038(4) 0.024(4) 0.003(3) 0.005(3) 0.016(4) C2 0.037(6) 0.037(6) 0.044(6) 0.011(5) 0.016(5) 0.020(5) N2 0.052(5) 0.039(4) 0.029(4) 0.009(3) 0.013(4) 0.033(4) C3 0.052(7) 0.044(6) 0.035(5) 0.006(5) 0.011(5) 0.023(5) C4 0.074(9) 0.034(6) 0.051(7) 0.008(5) 0.033(6) 0.018(6) C5 0.073(9) 0.045(7) 0.031(5) 0.004(5) 0.014(5) 0.015(6) C6 0.051(7) 0.050(6) 0.037(5) 0.006(5) 0.010(5) 0.029(6) N1' 0.037(5) 0.033(4) 0.033(4) 0.008(3) 0.016(4) 0.022(4) C2' 0.032(6) 0.031(5) 0.036(5) 0.015(4) 0.011(5) 0.015(5) N2' 0.039(5) 0.032(4) 0.035(4) 0.009(3) 0.008(4) 0.018(4) C3' 0.036(7) 0.043(6) 0.027(5) 0.008(5) 0.013(4) 0.006(5) C4' 0.051(8) 0.037(6) 0.041(5) 0.002(5) 0.024(5) 0.018(6) C5' 0.038(7) 0.042(6) 0.053(6) -0.003(5) 0.020(5) 0.022(6) C6' 0.037(7) 0.039(6) 0.042(5) 0.008(5) 0.009(5) 0.012(5) N20 0.050(6) 0.065(7) 0.048(6) 0.027(6) 0.014(5) 0.025(6) O21 0.095(7) 0.086(6) 0.053(5) 0.000(4) 0.026(4) 0.036(5) O22 0.107(7) 0.066(5) 0.051(4) 0.000(4) 0.006(4) 0.048(5) O23 0.092(7) 0.078(6) 0.099(6) 0.047(5) 0.005(5) 0.032(5) N30 0.082(9) 0.051(6) 0.039(6) 0.016(5) 0.026(6) 0.022(6) O31 0.117(7) 0.092(6) 0.088(6) 0.059(5) 0.070(5) 0.071(6) O32 0.105(8) 0.106(7) 0.072(6) 0.023(5) 0.009(6) 0.070(7) O33 0.108(8) 0.099(7) 0.066(5) 0.002(5) 0.016(5) 0.002(6) O1W 0.076(6) 0.102(6) 0.094(6) 0.054(5) 0.028(5) 0.031(5) _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 Pt1 N1 1.998(6) . ? Pt1 N1' 2.023(6) . ? Pt1 N11' 2.050(7) . ? Pt1 N11 2.063(7) . ? Pt1 Pd1 2.4765(11) . ? Pt1 O11 2.523(6) . ? Pd1 N2' 2.041(6) . ? Pd1 N2 2.066(7) . ? Pd1 Cl1 2.336(3) . ? Pd1 Pd3 2.8913(14) . ? Pd1 Pd2 3.025(2) . ? Pd3 N11 2.016(7) . ? Pd3 N22 2.038(7) . ? Pd3 N21 2.049(6) . ? Pd3 N2' 2.098(6) . ? Pd2 N11' 2.032(7) . ? Pd2 N31 2.043(7) . ? Pd2 N32 2.046(7) . ? Pd2 N2 2.084(6) . ? N11 H11A 0.90 . ? N11 H11B 0.90 . ? N11' H11C 0.90 . ? N11' H11D 0.90 . ? N21 C21 1.483(10) . ? N21 H21A 0.90 . ? N21 H21B 0.90 . ? C21 C22 1.512(11) . ? C21 H21C 0.97 . ? C21 H21D 0.97 . ? C22 N22 1.485(10) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? N22 H22C 0.90 . ? N22 H22D 0.90 . ? N31 C31 1.454(11) . ? N31 H31A 0.90 . ? N31 H31B 0.90 . ? C31 C32 1.487(12) . ? C31 H31C 0.97 . ? C31 H31D 0.97 . ? C32 N32 1.500(11) . ? C32 H32A 0.97 . ? C32 H32B 0.97 . ? N32 H32C 0.90 . ? N32 H32D 0.90 . ? N10 O13 1.231(9) . ? N10 O12 1.232(9) . ? N10 O11 1.272(9) . ? N1 C2 1.345(10) . ? N1 C6 1.367(9) . ? C2 N2 1.388(10) . ? C2 C3 1.394(11) . ? N2 H2 1.075(6) . ? C3 C4 1.359(11) . ? C3 H3 0.93 . ? C4 C5 1.395(12) . ? C4 H4 0.93 . ? C5 C6 1.363(11) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? N1' C6' 1.346(10) . ? N1' C2' 1.351(10) . ? C2' N2' 1.372(10) . ? C2' C3' 1.402(10) . ? N2' H2' 0.803(7) . ? C3' C4' 1.376(11) . ? C3' H3' 0.93 . ? C4' C5' 1.361(11) . ? C4' H4' 0.93 . ? C5' C6' 1.377(10) . ? C5' H5' 0.93 . ? C6' H6' 0.93 . ? N20 O21 1.229(9) . ? N20 O23 1.238(10) . ? N20 O22 1.239(9) . ? N30 O32 1.205(10) . ? N30 O33 1.227(10) . ? N30 O31 1.230(10) . ? O2W O2W 1.81(5) 2_665 ? 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 Pt1 N1' 172.5(3) . . ? N1 Pt1 N11' 86.8(3) . . ? N1' Pt1 N11' 94.5(3) . . ? N1 Pt1 N11 93.8(3) . . ? N1' Pt1 N11 84.6(2) . . ? N11' Pt1 N11 178.0(3) . . ? N1 Pt1 Pd1 86.2(2) . . ? N1' Pt1 Pd1 86.5(2) . . ? N11' Pt1 Pd1 88.7(2) . . ? N11 Pt1 Pd1 89.5(2) . . ? N1 Pt1 O11 95.1(2) . . ? N1' Pt1 O11 92.2(2) . . ? N11' Pt1 O11 92.5(2) . . ? N11 Pt1 O11 89.3(2) . . ? Pd1 Pt1 O11 178.28(15) . . ? N2' Pd1 N2 167.1(3) . . ? N2' Pd1 Cl1 94.5(2) . . ? N2 Pd1 Cl1 98.2(2) . . ? N2' Pd1 Pt1 83.4(2) . . ? N2 Pd1 Pt1 83.8(2) . . ? Cl1 Pd1 Pt1 177.16(9) . . ? N2' Pd1 Pd3 46.5(2) . . ? N2 Pd1 Pd3 128.5(2) . . ? Cl1 Pd1 Pd3 99.76(9) . . ? Pt1 Pd1 Pd3 77.40(4) . . ? N2' Pd1 Pd2 133.5(2) . . ? N2 Pd1 Pd2 43.4(2) . . ? Cl1 Pd1 Pd2 106.44(9) . . ? Pt1 Pd1 Pd2 76.40(4) . . ? Pd3 Pd1 Pd2 153.40(3) . . ? N11 Pd3 N22 176.0(3) . . ? N11 Pd3 N21 94.4(3) . . ? N22 Pd3 N21 84.5(3) . . ? N11 Pd3 N2' 91.1(3) . . ? N22 Pd3 N2' 89.9(3) . . ? N21 Pd3 N2' 174.4(3) . . ? N11 Pd3 Pd1 79.5(2) . . ? N22 Pd3 Pd1 98.5(2) . . ? N21 Pd3 Pd1 135.4(2) . . ? N2' Pd3 Pd1 44.9(2) . . ? N11' Pd2 N31 93.1(3) . . ? N11' Pd2 N32 176.9(3) . . ? N31 Pd2 N32 83.8(3) . . ? N11' Pd2 N2 92.4(3) . . ? N31 Pd2 N2 174.2(3) . . ? N32 Pd2 N2 90.7(3) . . ? N11' Pd2 Pd1 75.0(2) . . ? N31 Pd2 Pd1 137.4(2) . . ? N32 Pd2 Pd1 107.5(3) . . ? N2 Pd2 Pd1 43.0(2) . . ? Pd3 N11 Pt1 111.5(3) . . ? Pd3 N11 H11A 109.3(2) . . ? Pt1 N11 H11A 109.3(2) . . ? Pd3 N11 H11B 109.3(2) . . ? Pt1 N11 H11B 109.3(2) . . ? H11A N11 H11B 108.0 . . ? Pd2 N11' Pt1 114.3(3) . . ? Pd2 N11' H11C 108.7(2) . . ? Pt1 N11' H11C 108.7(2) . . ? Pd2 N11' H11D 108.7(2) . . ? Pt1 N11' H11D 108.7(2) . . ? H11C N11' H11D 107.6 . . ? C21 N21 Pd3 107.6(5) . . ? C21 N21 H21A 110.2(5) . . ? Pd3 N21 H21A 110.2(2) . . ? C21 N21 H21B 110.2(4) . . ? Pd3 N21 H21B 110.2(2) . . ? H21A N21 H21B 108.5 . . ? N21 C21 C22 107.7(7) . . ? N21 C21 H21C 110.2(4) . . ? C22 C21 H21C 110.2(5) . . ? N21 C21 H21D 110.2(4) . . ? C22 C21 H21D 110.2(5) . . ? H21C C21 H21D 108.5 . . ? N22 C22 C21 108.8(7) . . ? N22 C22 H22A 109.9(5) . . ? C21 C22 H22A 109.9(5) . . ? N22 C22 H22B 109.9(5) . . ? C21 C22 H22B 109.9(5) . . ? H22A C22 H22B 108.3 . . ? C22 N22 Pd3 108.3(5) . . ? C22 N22 H22C 110.0(5) . . ? Pd3 N22 H22C 110.0(2) . . ? C22 N22 H22D 110.0(4) . . ? Pd3 N22 H22D 110.0(2) . . ? H22C N22 H22D 108.4 . . ? C31 N31 Pd2 106.9(6) . . ? C31 N31 H31A 110.3(5) . . ? Pd2 N31 H31A 110.3(2) . . ? C31 N31 H31B 110.3(5) . . ? Pd2 N31 H31B 110.3(2) . . ? H31A N31 H31B 108.6 . . ? N31 C31 C32 107.5(8) . . ? N31 C31 H31C 110.2(5) . . ? C32 C31 H31C 110.2(6) . . ? N31 C31 H31D 110.2(5) . . ? C32 C31 H31D 110.2(6) . . ? H31C C31 H31D 108.5 . . ? C31 C32 N32 108.0(8) . . ? C31 C32 H32A 110.1(6) . . ? N32 C32 H32A 110.1(5) . . ? C31 C32 H32B 110.1(6) . . ? N32 C32 H32B 110.1(6) . . ? H32A C32 H32B 108.4 . . ? C32 N32 Pd2 107.7(6) . . ? C32 N32 H32C 110.2(6) . . ? Pd2 N32 H32C 110.2(2) . . ? C32 N32 H32D 110.2(5) . . ? Pd2 N32 H32D 110.2(2) . . ? H32C N32 H32D 108.5 . . ? O13 N10 O12 121.1(10) . . ? O13 N10 O11 119.1(9) . . ? O12 N10 O11 119.8(9) . . ? N10 O11 Pt1 123.4(6) . . ? C2 N1 C6 117.6(7) . . ? C2 N1 Pt1 119.7(5) . . ? C6 N1 Pt1 122.3(6) . . ? N1 C2 N2 118.5(7) . . ? N1 C2 C3 121.7(8) . . ? N2 C2 C3 119.8(8) . . ? C2 N2 Pd1 112.0(5) . . ? C2 N2 Pd2 116.0(5) . . ? Pd1 N2 Pd2 93.6(2) . . ? C2 N2 H2 112.9(6) . . ? Pd1 N2 H2 110.7(5) . . ? Pd2 N2 H2 110.1(5) . . ? C4 C3 C2 119.6(9) . . ? C4 C3 H3 120.2(6) . . ? C2 C3 H3 120.2(6) . . ? C3 C4 C5 119.7(8) . . ? C3 C4 H4 120.1(6) . . ? C5 C4 H4 120.1(5) . . ? C6 C5 C4 118.0(9) . . ? C6 C5 H5 121.0(6) . . ? C4 C5 H5 121.0(5) . . ? C5 C6 N1 123.4(9) . . ? C5 C6 H6 118.3(6) . . ? N1 C6 H6 118.3(5) . . ? C6' N1' C2' 119.9(7) . . ? C6' N1' Pt1 121.9(6) . . ? C2' N1' Pt1 118.3(5) . . ? N1' C2' N2' 118.7(7) . . ? N1' C2' C3' 119.1(8) . . ? N2' C2' C3' 122.2(8) . . ? C2' N2' Pd1 115.6(6) . . ? C2' N2' Pd3 117.3(5) . . ? Pd1 N2' Pd3 88.6(2) . . ? C2' N2' H2' 118.4(7) . . ? Pd1 N2' H2' 116.9(6) . . ? Pd3 N2' H2' 93.9(5) . . ? C4' C3' C2' 119.9(9) . . ? C4' C3' H3' 120.1(5) . . ? C2' C3' H3' 120.1(5) . . ? C5' C4' C3' 120.4(8) . . ? C5' C4' H4' 119.8(5) . . ? C3' C4' H4' 119.8(6) . . ? C4' C5' C6' 118.0(9) . . ? C4' C5' H5' 121.0(5) . . ? C6' C5' H5' 121.0(6) . . ? N1' C6' C5' 122.7(9) . . ? N1' C6' H6' 118.6(5) . . ? C5' C6' H6' 118.6(6) . . ? O21 N20 O23 121.9(10) . . ? O21 N20 O22 119.5(9) . . ? O23 N20 O22 118.5(9) . . ? O32 N30 O33 119.5(10) . . ? O32 N30 O31 120.1(9) . . ? O33 N30 O31 120.4(12) . . ? 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 Pt1 Pd1 N2' -149.8(3) . . . . ? N1' Pt1 Pd1 N2' 28.7(3) . . . . ? N11' Pt1 Pd1 N2' 123.3(2) . . . . ? N11 Pt1 Pd1 N2' -55.9(2) . . . . ? O11 Pt1 Pd1 N2' -7.8(48) . . . . ? N1 Pt1 Pd1 N2 28.8(3) . . . . ? N1' Pt1 Pd1 N2 -152.7(3) . . . . ? N11' Pt1 Pd1 N2 -58.1(2) . . . . ? N11 Pt1 Pd1 N2 122.7(2) . . . . ? O11 Pt1 Pd1 N2 170.8(48) . . . . ? N1 Pt1 Pd1 Cl1 -106.2(14) . . . . ? N1' Pt1 Pd1 Cl1 72.3(14) . . . . ? N11' Pt1 Pd1 Cl1 166.9(14) . . . . ? N11 Pt1 Pd1 Cl1 -12.4(14) . . . . ? O11 Pt1 Pd1 Cl1 35.7(52) . . . . ? N1 Pt1 Pd1 Pd3 -103.0(2) . . . . ? N1' Pt1 Pd1 Pd3 75.5(2) . . . . ? N11' Pt1 Pd1 Pd3 170.1(2) . . . . ? N11 Pt1 Pd1 Pd3 -9.1(2) . . . . ? O11 Pt1 Pd1 Pd3 39.0(48) . . . . ? N1 Pt1 Pd1 Pd2 72.3(2) . . . . ? N1' Pt1 Pd1 Pd2 -109.2(2) . . . . ? N11' Pt1 Pd1 Pd2 -14.5(2) . . . . ? N11 Pt1 Pd1 Pd2 166.2(2) . . . . ? O11 Pt1 Pd1 Pd2 -145.7(48) . . . . ? N2' Pd1 Pd3 N11 102.4(3) . . . . ? N2 Pd1 Pd3 N11 -61.8(3) . . . . ? Cl1 Pd1 Pd3 N11 -170.7(2) . . . . ? Pt1 Pd1 Pd3 N11 9.5(2) . . . . ? Pd2 Pd1 Pd3 N11 -0.7(2) . . . . ? N2' Pd1 Pd3 N22 -81.2(3) . . . . ? N2 Pd1 Pd3 N22 114.6(3) . . . . ? Cl1 Pd1 Pd3 N22 5.8(2) . . . . ? Pt1 Pd1 Pd3 N22 -174.1(2) . . . . ? Pd2 Pd1 Pd3 N22 175.8(2) . . . . ? N2' Pd1 Pd3 N21 -172.0(4) . . . . ? N2 Pd1 Pd3 N21 23.8(4) . . . . ? Cl1 Pd1 Pd3 N21 -85.1(3) . . . . ? Pt1 Pd1 Pd3 N21 95.1(3) . . . . ? Pd2 Pd1 Pd3 N21 84.9(3) . . . . ? N2' Pd1 Pd3 N2' 0.0 . . . . ? N2 Pd1 Pd3 N2' -164.2(3) . . . . ? Cl1 Pd1 Pd3 N2' 87.0(3) . . . . ? Pt1 Pd1 Pd3 N2' -92.9(3) . . . . ? Pd2 Pd1 Pd3 N2' -103.0(3) . . . . ? N2' Pd1 Pd2 N11' -51.7(3) . . . . ? N2 Pd1 Pd2 N11' 110.5(3) . . . . ? Cl1 Pd1 Pd2 N11' -164.9(2) . . . . ? Pt1 Pd1 Pd2 N11' 15.2(2) . . . . ? Pd3 Pd1 Pd2 N11' 25.4(2) . . . . ? N2' Pd1 Pd2 N31 26.3(4) . . . . ? N2 Pd1 Pd2 N31 -171.5(4) . . . . ? Cl1 Pd1 Pd2 N31 -86.9(3) . . . . ? Pt1 Pd1 Pd2 N31 93.2(3) . . . . ? Pd3 Pd1 Pd2 N31 103.4(3) . . . . ? N2' Pd1 Pd2 N32 126.3(3) . . . . ? N2 Pd1 Pd2 N32 -71.5(3) . . . . ? Cl1 Pd1 Pd2 N32 13.1(2) . . . . ? Pt1 Pd1 Pd2 N32 -166.8(2) . . . . ? Pd3 Pd1 Pd2 N32 -156.6(2) . . . . ? N2' Pd1 Pd2 N2 -162.2(4) . . . . ? N2 Pd1 Pd2 N2 0.0 . . . . ? Cl1 Pd1 Pd2 N2 84.6(3) . . . . ? Pt1 Pd1 Pd2 N2 -95.3(3) . . . . ? Pd3 Pd1 Pd2 N2 -85.1(3) . . . . ? N22 Pd3 N11 Pt1 -72.9(39) . . . . ? N21 Pd3 N11 Pt1 -147.4(3) . . . . ? N2' Pd3 N11 Pt1 31.6(3) . . . . ? Pd1 Pd3 N11 Pt1 -12.0(2) . . . . ? N1 Pt1 N11 Pd3 100.0(3) . . . . ? N1' Pt1 N11 Pd3 -72.7(3) . . . . ? N11' Pt1 N11 Pd3 -8.3(72) . . . . ? Pd1 Pt1 N11 Pd3 13.8(2) . . . . ? O11 Pt1 N11 Pd3 -164.9(3) . . . . ? N31 Pd2 N11' Pt1 -158.2(3) . . . . ? N32 Pd2 N11' Pt1 -162.3(53) . . . . ? N2 Pd2 N11' Pt1 20.0(3) . . . . ? Pd1 Pd2 N11' Pt1 -19.7(2) . . . . ? N1 Pt1 N11' Pd2 -62.8(3) . . . . ? N1' Pt1 N11' Pd2 109.8(3) . . . . ? N11 Pt1 N11' Pd2 45.6(72) . . . . ? Pd1 Pt1 N11' Pd2 23.5(3) . . . . ? O11 Pt1 N11' Pd2 -157.8(3) . . . . ? N11 Pd3 N21 C21 159.1(5) . . . . ? N22 Pd3 N21 C21 -17.0(5) . . . . ? N2' Pd3 N21 C21 -10.9(30) . . . . ? Pd1 Pd3 N21 C21 79.6(6) . . . . ? Pd3 N21 C21 C22 41.8(8) . . . . ? N21 C21 C22 N22 -53.4(10) . . . . ? C21 C22 N22 Pd3 37.8(8) . . . . ? N11 Pd3 N22 C22 -86.4(40) . . . . ? N21 Pd3 N22 C22 -11.6(6) . . . . ? N2' Pd3 N22 C22 169.0(6) . . . . ? Pd1 Pd3 N22 C22 -146.7(5) . . . . ? N11' Pd2 N31 C31 158.8(6) . . . . ? N32 Pd2 N31 C31 -21.5(6) . . . . ? N2 Pd2 N31 C31 -2.3(29) . . . . ? Pd1 Pd2 N31 C31 87.7(6) . . . . ? Pd2 N31 C31 C32 47.4(9) . . . . ? N31 C31 C32 N32 -56.2(11) . . . . ? C31 C32 N32 Pd2 36.2(10) . . . . ? N11' Pd2 N32 C32 -4.1(58) . . . . ? N31 Pd2 N32 C32 -8.2(6) . . . . ? N2 Pd2 N32 C32 173.7(6) . . . . ? Pd1 Pd2 N32 C32 -146.1(6) . . . . ? O13 N10 O11 Pt1 175.6(6) . . . . ? O12 N10 O11 Pt1 -3.2(11) . . . . ? N1 Pt1 O11 N10 -50.5(7) . . . . ? N1' Pt1 O11 N10 131.2(6) . . . . ? N11' Pt1 O11 N10 36.5(6) . . . . ? N11 Pt1 O11 N10 -144.3(6) . . . . ? Pd1 Pt1 O11 N10 167.6(44) . . . . ? N1' Pt1 N1 C2 -32.6(25) . . . . ? N11' Pt1 N1 C2 67.9(7) . . . . ? N11 Pt1 N1 C2 -110.2(7) . . . . ? Pd1 Pt1 N1 C2 -20.9(6) . . . . ? O11 Pt1 N1 C2 160.1(6) . . . . ? N1' Pt1 N1 C6 139.8(20) . . . . ? N11' Pt1 N1 C6 -119.7(7) . . . . ? N11 Pt1 N1 C6 62.2(7) . . . . ? Pd1 Pt1 N1 C6 151.5(7) . . . . ? O11 Pt1 N1 C6 -27.5(7) . . . . ? C6 N1 C2 N2 179.6(8) . . . . ? Pt1 N1 C2 N2 -7.7(11) . . . . ? C6 N1 C2 C3 1.1(13) . . . . ? Pt1 N1 C2 C3 173.9(7) . . . . ? N1 C2 N2 Pd1 40.4(9) . . . . ? C3 C2 N2 Pd1 -141.2(7) . . . . ? N1 C2 N2 Pd2 -65.4(9) . . . . ? C3 C2 N2 Pd2 113.0(8) . . . . ? N2' Pd1 N2 C2 -37.0(14) . . . . ? Cl1 Pd1 N2 C2 134.8(5) . . . . ? Pt1 Pd1 N2 C2 -43.2(5) . . . . ? Pd3 Pd1 N2 C2 25.3(6) . . . . ? Pd2 Pd1 N2 C2 -119.9(6) . . . . ? N2' Pd1 N2 Pd2 82.9(11) . . . . ? Cl1 Pd1 N2 Pd2 -105.3(2) . . . . ? Pt1 Pd1 N2 Pd2 76.8(2) . . . . ? Pd3 Pd1 N2 Pd2 145.22(12) . . . . ? Pd2 Pd1 N2 Pd2 0.0 . . . . ? N11' Pd2 N2 C2 51.7(6) . . . . ? N31 Pd2 N2 C2 -147.2(24) . . . . ? N32 Pd2 N2 C2 -128.1(6) . . . . ? Pd1 Pd2 N2 C2 116.6(6) . . . . ? N11' Pd2 N2 Pd1 -64.9(3) . . . . ? N31 Pd2 N2 Pd1 96.2(26) . . . . ? N32 Pd2 N2 Pd1 115.3(3) . . . . ? Pd1 Pd2 N2 Pd1 0.0 . . . . ? N1 C2 C3 C4 -1.3(14) . . . . ? N2 C2 C3 C4 -179.7(9) . . . . ? C2 C3 C4 C5 1.1(15) . . . . ? C3 C4 C5 C6 -0.9(16) . . . . ? C4 C5 C6 N1 0.8(15) . . . . ? C2 N1 C6 C5 -0.9(13) . . . . ? Pt1 N1 C6 C5 -173.5(7) . . . . ? N1 Pt1 N1' C6' 165.8(19) . . . . ? N11' Pt1 N1' C6' 65.8(7) . . . . ? N11 Pt1 N1' C6' -116.0(7) . . . . ? Pd1 Pt1 N1' C6' 154.1(6) . . . . ? O11 Pt1 N1' C6' -26.9(7) . . . . ? N1 Pt1 N1' C2' -12.7(25) . . . . ? N11' Pt1 N1' C2' -112.8(6) . . . . ? N11 Pt1 N1' C2' 65.4(6) . . . . ? Pd1 Pt1 N1' C2' -24.4(6) . . . . ? O11 Pt1 N1' C2' 154.6(6) . . . . ? C6' N1' C2' N2' -178.9(7) . . . . ? Pt1 N1' C2' N2' -0.3(10) . . . . ? C6' N1' C2' C3' -0.4(12) . . . . ? Pt1 N1' C2' C3' 178.2(6) . . . . ? N1' C2' N2' Pd1 34.3(10) . . . . ? C3' C2' N2' Pd1 -144.2(7) . . . . ? N1' C2' N2' Pd3 -68.3(9) . . . . ? C3' C2' N2' Pd3 113.3(8) . . . . ? N2 Pd1 N2' C2' -47.1(14) . . . . ? Cl1 Pd1 N2' C2' 141.0(5) . . . . ? Pt1 Pd1 N2' C2' -41.0(5) . . . . ? Pd3 Pd1 N2' C2' -119.8(6) . . . . ? Pd2 Pd1 N2' C2' 23.2(7) . . . . ? N2 Pd1 N2' Pd3 72.7(12) . . . . ? Cl1 Pd1 N2' Pd3 -99.2(2) . . . . ? Pt1 Pd1 N2' Pd3 78.9(2) . . . . ? Pd3 Pd1 N2' Pd3 0.0 . . . . ? Pd2 Pd1 N2' Pd3 143.01(12) . . . . ? N11 Pd3 N2' C2' 44.4(6) . . . . ? N22 Pd3 N2' C2' -139.5(6) . . . . ? N21 Pd3 N2' C2' -145.6(25) . . . . ? Pd1 Pd3 N2' C2' 118.3(7) . . . . ? N11 Pd3 N2' Pd1 -73.9(3) . . . . ? N22 Pd3 N2' Pd1 102.2(3) . . . . ? N21 Pd3 N2' Pd1 96.1(27) . . . . ? Pd1 Pd3 N2' Pd1 0.0 . . . . ? N1' C2' C3' C4' 0.1(12) . . . . ? N2' C2' C3' C4' 178.5(8) . . . . ? C2' C3' C4' C5' -0.8(14) . . . . ? C3' C4' C5' C6' 1.6(14) . . . . ? C2' N1' C6' C5' 1.4(13) . . . . ? Pt1 N1' C6' C5' -177.1(7) . . . . ? C4' C5' C6' N1' -2.0(14) . . . . ? _refine_diff_density_max 0.985 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.142 #===END data_4c _publ_contact_author_name 'Prof. Bernhard Lippert' _publ_contact_author_address ; Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_email 'lippert@pop.uni-dortmund.de' _publ_contact_author_fax 'Int. code + (231) 755-3797' _publ_contact_author_phone '231 755-3840' _publ_contact_letter ? _publ_requested_journal 'Dalton Transactions' _publ_title ; Ready formation of water-stable Pt(II)-(-NH2)-Pd(II) species through combination of trans-[(NH3)2 Pt(II)L2] (L = N,N'-hterocycle) and [enPd(H2O)2]2+ ; _publ_author_address ; Alexandra Fichtel, Eva Freisinger, Bettina Beck, Bernhard Lippert' Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H39.20 Br2 N12 O10.60 Pd3 Pt' _chemical_formula_weight 1219.48 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.641(2) _cell_length_b 11.757(2) _cell_length_c 14.136(3) _cell_angle_alpha 111.96(3) _cell_angle_beta 105.48(3) _cell_angle_gamma 100.62(3) _cell_volume 1639.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4217 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 23.28 _exptl_crystal_description stick _exptl_crystal_colour brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.470 _exptl_crystal_density_method ? _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 8.374 _exptl_absorpt_correction_type SCALEPACK _exptl_absorpt_correction_T_min 0.1431 _exptl_absorpt_correction_T_max 0.4090 _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 'Enraf-Nonius-KappaCCD' _diffrn_measurement_method ; 360 frames via \w-rotation (\D\w\=1\%) and two times 80s per frame ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4217 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 23.28 _reflns_number_total 4217 _reflns_number_observed 2844 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, Netherlands)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 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^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ; refU, except H11a to H11d roref, H2 and H2' refall ; _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00005(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4211 _refine_ls_number_parameters 402 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_obs 0.0412 _refine_ls_wR_factor_all 0.1024 _refine_ls_wR_factor_obs 0.0835 _refine_ls_goodness_of_fit_all 0.973 _refine_ls_goodness_of_fit_obs 1.098 _refine_ls_restrained_S_all 1.081 _refine_ls_restrained_S_obs 1.096 _refine_ls_shift/esd_max 0.062 _refine_ls_shift/esd_mean 0.006 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 Pt1 Pt 0.11147(4) 0.36978(5) 0.25787(4) 0.0381(2) Uani 1 d . . Pd1 Pd 0.27189(8) 0.52839(9) 0.24341(7) 0.0383(3) Uani 1 d . . Pd2 Pd 0.18174(9) 0.69574(9) 0.39955(8) 0.0441(3) Uani 1 d . . Pd3 Pd 0.27481(9) 0.26871(9) 0.09191(8) 0.0449(3) Uani 1 d . . Br1 Br 0.43584(12) 0.70331(13) 0.24984(11) 0.0564(4) Uani 1 d . . Br2 Br -0.06536(12) 0.18349(13) 0.27029(11) 0.0581(4) Uani 1 d . . N11 N 0.1196(8) 0.2261(8) 0.1259(8) 0.045(3) Uani 1 d . . H11A H 0.1151(8) 0.1555(8) 0.1376(8) 0.059 Uiso 1 calc R . H11B H 0.0518(8) 0.2058(8) 0.0667(8) 0.059 Uiso 1 calc R . N11' N 0.1071(8) 0.5192(9) 0.3900(8) 0.044(3) Uani 1 d . . H11C H 0.0269(8) 0.5085(9) 0.3853(8) 0.057 Uiso 1 calc R . H11D H 0.1501(8) 0.5165(9) 0.4519(8) 0.057 Uiso 1 calc R . N21 N 0.2651(10) 0.8770(10) 0.4167(9) 0.063(3) Uani 1 d . . H21A H 0.3120(10) 0.8716(10) 0.3748(9) 0.088(19) Uiso 1 calc R . H21B H 0.2061(10) 0.9116(10) 0.3959(9) 0.088(19) Uiso 1 calc R . N22 N 0.2389(10) 0.7898(10) 0.5674(8) 0.057(3) Uani 1 d . . H22A H 0.1730(10) 0.7744(10) 0.5878(8) 0.088(19) Uiso 1 calc R . H22B H 0.2973(10) 0.7607(10) 0.5983(8) 0.088(19) Uiso 1 calc R . C21 C 0.3452(18) 0.9577(17) 0.5339(14) 0.109(6) Uani 1 d . . H21C H 0.4266(18) 0.9442(17) 0.5471(14) 0.100(20) Uiso 1 calc R . H21D H 0.3584(18) 1.0482(17) 0.5510(14) 0.100(20) Uiso 1 calc R . C22 C 0.2916(19) 0.9288(17) 0.6037(15) 0.129(9) Uani 1 d . . H22C H 0.2255(19) 0.9680(17) 0.6081(15) 0.100(20) Uiso 1 calc R . H22D H 0.3554(19) 0.9672(17) 0.6768(15) 0.100(20) Uiso 1 calc R . N31 N 0.1850(10) 0.1368(11) -0.0672(9) 0.068(3) Uani 1 d . . H31A H 0.1775(10) 0.0564(11) -0.0736(9) 0.088(19) Uiso 1 calc R . H31B H 0.1076(10) 0.1417(11) -0.0934(9) 0.088(19) Uiso 1 calc R . N32 N 0.4270(10) 0.3015(13) 0.0444(10) 0.075(4) Uani 1 d . . H32A H 0.4449(10) 0.3802(13) 0.0462(10) 0.088(19) Uiso 1 calc R . H32B H 0.4952(10) 0.2979(13) 0.0902(10) 0.088(19) Uiso 1 calc R . C31 C 0.2589(15) 0.1652(16) -0.1277(13) 0.091(5) Uani 1 d . . H31C H 0.2324(15) 0.0906(16) -0.1983(13) 0.100(20) Uiso 1 calc R . H31D H 0.2428(15) 0.2369(16) -0.1412(13) 0.100(20) Uiso 1 calc R . C32 C 0.3916(15) 0.1975(16) -0.0713(12) 0.083(5) Uani 1 d . . H32C H 0.4382(15) 0.2289(16) -0.1090(12) 0.100(20) Uiso 1 calc R . H32D H 0.4116(15) 0.1216(16) -0.0694(12) 0.100(20) Uiso 1 calc R . N1 N -0.0186(9) 0.4149(10) 0.1638(8) 0.042(3) Uani 1 d . . C2 C 0.0135(12) 0.5296(13) 0.1641(10) 0.044(3) Uani 1 d . . N2 N 0.1334(10) 0.6151(11) 0.2310(9) 0.044(3) Uani 1 d . . C3 C -0.0705(12) 0.5624(13) 0.0929(10) 0.057(4) Uani 1 d . . H3 H -0.0461(12) 0.6416(13) 0.0917(10) 0.038(11) Uiso 1 calc R . C4 C -0.1880(13) 0.4757(16) 0.0261(11) 0.063(4) Uani 1 d . . H4 H -0.2454(13) 0.4963(16) -0.0194(11) 0.038(11) Uiso 1 calc R . C5 C -0.2203(12) 0.3560(15) 0.0272(11) 0.064(4) Uani 1 d . . H5 H -0.2997(12) 0.2959(15) -0.0170(11) 0.038(11) Uiso 1 calc R . C6 C -0.1333(11) 0.3285(12) 0.0945(10) 0.048(3) Uani 1 d . . H6 H -0.1538(11) 0.2472(12) 0.0925(10) 0.038(11) Uiso 1 calc R . N1' N 0.2619(8) 0.3408(9) 0.3496(8) 0.043(3) Uani 1 d . . C2' C 0.3716(11) 0.3655(11) 0.3329(10) 0.046(3) Uani 1 d . . N2' N 0.3742(9) 0.4070(10) 0.2514(8) 0.039(3) Uani 1 d . . C3' C 0.4750(11) 0.3507(11) 0.3971(10) 0.047(3) Uani 1 d . . H3' H 0.5499(11) 0.3633(11) 0.3847(10) 0.038(11) Uiso 1 calc R . C4' C 0.4670(13) 0.3176(13) 0.4791(11) 0.056(4) Uani 1 d . . H4' H 0.5381(13) 0.3118(13) 0.5240(11) 0.038(11) Uiso 1 calc R . C5' C 0.3579(13) 0.2932(12) 0.4959(11) 0.061(4) Uani 1 d . . H5' H 0.3526(13) 0.2688(12) 0.5505(11) 0.038(11) Uiso 1 calc R . C6' C 0.2551(12) 0.3055(11) 0.4302(10) 0.047(3) Uani 1 d . . H6' H 0.1794(12) 0.2894(11) 0.4407(10) 0.038(11) Uiso 1 calc R . N10 N 0.1495(9) 0.9237(11) 0.1616(9) 0.035(3) Uani 1 d . . O11 O 0.1257(13) 0.9501(11) 0.1000(12) 0.111(5) Uani 1 d . . O12 O 0.0904(13) 0.8590(14) 0.1794(12) 0.126(5) Uiso 1 d . . O13 O 0.2549(18) 0.9616(18) 0.2213(15) 0.187(7) Uiso 1 d . . N20 N 0.7508(10) 0.4799(13) 0.3162(9) 0.054(3) Uani 1 d D . O21 O 0.7541(19) 0.4123(16) 0.3610(16) 0.075(5) Uani 0.60 d PD 1 O22 O 0.8519(15) 0.5582(16) 0.3559(18) 0.099(7) Uani 0.60 d PD 1 O23 O 0.6583(16) 0.4835(21) 0.2571(14) 0.087(6) Uani 0.60 d PD 1 O22A O 0.7913(35) 0.5544(27) 0.2857(31) 0.114(12) Uiso 0.40 d PD 2 O23A O 0.6508(22) 0.3987(30) 0.2686(30) 0.131(15) Uiso 0.40 d PD 2 O21A O 0.8314(29) 0.4807(40) 0.3889(21) 0.094(12) Uiso 0.40 d PD 2 H2 H 0.1686(81) 0.6752(85) 0.2223(73) 0.008(29) Uiso 1 d . . H2' H 0.4576(118) 0.4436(125) 0.2683(106) 0.081(49) Uiso 1 d . . O1W O 0.0649(11) 0.0051(11) 0.3953(11) 0.116(4) Uani 1 d . . O2W O 0.5992(11) 0.1571(13) 0.1396(12) 0.144(5) Uani 1 d . . O3W O 0.3561(14) -0.0163(14) 0.0444(14) 0.153(5) Uani 1 d . . O4W O 0.8902(17) 0.8169(13) 0.3969(14) 0.179(7) Uani 1 d . . O5W O 0.5856(18) 0.5532(19) 0.1016(18) 0.121(7) Uani 0.60 d P . 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 Pt1 0.0335(3) 0.0424(3) 0.0385(3) 0.0181(3) 0.0122(2) 0.0139(2) Pd1 0.0339(5) 0.0429(6) 0.0360(6) 0.0171(5) 0.0113(4) 0.0112(5) Pd2 0.0443(6) 0.0433(6) 0.0415(6) 0.0138(5) 0.0178(5) 0.0150(5) Pd3 0.0438(6) 0.0468(7) 0.0456(7) 0.0181(5) 0.0208(5) 0.0168(5) Br1 0.0473(8) 0.0613(10) 0.0511(9) 0.0271(8) 0.0114(7) 0.0020(7) Br2 0.0567(9) 0.0550(9) 0.0598(10) 0.0215(8) 0.0275(8) 0.0113(7) N11 0.051(6) 0.033(6) 0.054(7) 0.019(6) 0.028(6) 0.007(5) N11' 0.036(6) 0.054(7) 0.051(7) 0.029(6) 0.018(5) 0.023(5) N21 0.068(8) 0.053(8) 0.065(9) 0.028(7) 0.019(7) 0.016(7) N22 0.060(7) 0.053(8) 0.049(7) 0.013(6) 0.024(6) 0.018(6) C21 0.116(15) 0.074(13) 0.070(14) -0.006(11) 0.010(12) 0.000(12) C22 0.165(19) 0.072(14) 0.081(14) -0.035(11) 0.088(14) -0.028(13) N31 0.071(8) 0.063(8) 0.061(8) 0.008(7) 0.039(7) 0.019(7) N32 0.058(7) 0.113(11) 0.073(9) 0.052(9) 0.036(7) 0.029(7) C31 0.093(13) 0.073(12) 0.055(11) -0.010(9) 0.029(10) -0.003(10) C32 0.080(12) 0.098(13) 0.053(11) 0.017(10) 0.028(9) 0.021(10) N1 0.044(7) 0.039(7) 0.043(7) 0.019(6) 0.010(5) 0.019(6) C2 0.048(9) 0.058(10) 0.040(8) 0.026(7) 0.022(7) 0.027(8) N2 0.038(7) 0.048(8) 0.051(8) 0.028(7) 0.011(6) 0.016(6) C3 0.070(10) 0.057(10) 0.050(9) 0.029(8) 0.020(8) 0.030(9) C4 0.043(9) 0.100(13) 0.049(10) 0.036(10) 0.014(8) 0.029(9) C5 0.037(8) 0.086(12) 0.052(10) 0.022(9) 0.007(7) 0.019(8) C6 0.048(8) 0.046(9) 0.043(8) 0.018(7) 0.006(7) 0.017(7) N1' 0.037(6) 0.042(6) 0.046(7) 0.017(6) 0.011(5) 0.016(5) C2' 0.032(7) 0.040(8) 0.048(9) 0.005(7) 0.014(7) 0.007(6) N2' 0.035(6) 0.051(7) 0.046(7) 0.029(6) 0.024(5) 0.022(6) C3' 0.044(8) 0.060(9) 0.038(8) 0.018(7) 0.014(7) 0.027(7) C4' 0.050(9) 0.073(10) 0.053(10) 0.035(8) 0.012(7) 0.034(8) C5' 0.069(10) 0.058(10) 0.054(10) 0.030(8) 0.004(8) 0.032(8) C6' 0.050(8) 0.054(9) 0.036(8) 0.016(7) 0.025(7) 0.009(7) N10 0.027(6) 0.055(8) 0.034(7) 0.032(6) 0.011(5) 0.013(5) O11 0.129(11) 0.076(9) 0.115(12) 0.034(9) 0.029(9) 0.048(8) N20 0.045(8) 0.066(10) 0.048(9) 0.020(8) 0.026(7) 0.007(7) O21 0.067(13) 0.084(15) 0.065(13) 0.030(12) 0.019(10) 0.022(12) O22 0.081(16) 0.108(18) 0.083(16) 0.020(14) 0.008(12) 0.055(15) O23 0.050(11) 0.117(17) 0.078(14) 0.044(12) -0.006(9) 0.040(11) O1W 0.109(9) 0.110(10) 0.159(12) 0.079(9) 0.060(9) 0.044(8) O2W 0.090(9) 0.124(11) 0.176(14) 0.043(10) 0.028(9) 0.024(8) O3W 0.154(12) 0.133(12) 0.211(16) 0.087(12) 0.102(12) 0.057(10) O4W 0.242(18) 0.106(12) 0.185(16) 0.045(11) 0.126(14) 0.023(12) O5W 0.106(15) 0.095(16) 0.137(19) 0.023(14) 0.062(14) 0.014(13) _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 Pt1 N1 2.023(9) . ? Pt1 N11 2.035(9) . ? Pt1 N1' 2.050(9) . ? Pt1 N11' 2.051(9) . ? Pt1 Pd1 2.4924(13) . ? Pt1 Br2 2.808(2) . ? Pd1 N2' 2.035(9) . ? Pd1 N2 2.063(9) . ? Pd1 Br1 2.490(2) . ? Pd1 Pd2 2.932(2) . ? Pd1 Pd3 3.016(2) . ? Pd2 N11' 2.036(9) . ? Pd2 N22 2.053(10) . ? Pd2 N21 2.065(10) . ? Pd2 N2 2.072(11) . ? Pd3 N11 2.014(9) . ? Pd3 N31 2.024(10) . ? Pd3 N2' 2.058(10) . ? Pd3 N32 2.078(10) . ? N21 C21 1.48(2) . ? N22 C22 1.47(2) . ? C21 C22 1.41(2) . ? N31 C31 1.44(2) . ? N32 C32 1.52(2) . ? C31 C32 1.44(2) . ? N1 C2 1.329(14) . ? N1 C6 1.353(14) . ? C2 N2 1.39(2) . ? C2 C3 1.42(2) . ? C3 C4 1.37(2) . ? C4 C5 1.39(2) . ? C5 C6 1.37(2) . ? N1' C2' 1.358(14) . ? N1' C6' 1.365(14) . ? C2' C3' 1.384(15) . ? C2' N2' 1.42(2) . ? C3' C4' 1.37(2) . ? C4' C5' 1.35(2) . ? C5' C6' 1.37(2) . ? N10 O11 1.018(13) . ? N10 O12 1.08(2) . ? N10 O13 1.18(2) . ? N20 O21 1.187(8) . ? N20 O22 1.187(8) . ? N20 O21A 1.187(8) . ? N20 O23A 1.188(8) . ? N20 O22A 1.189(8) . ? N20 O23 1.193(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 N1 Pt1 N11 93.2(4) . . ? N1 Pt1 N1' 171.8(4) . . ? N11 Pt1 N1' 86.0(4) . . ? N1 Pt1 N11' 86.4(4) . . ? N11 Pt1 N11' 178.0(4) . . ? N1' Pt1 N11' 94.2(4) . . ? N1 Pt1 Pd1 86.4(3) . . ? N11 Pt1 Pd1 89.3(3) . . ? N1' Pt1 Pd1 85.5(3) . . ? N11' Pt1 Pd1 88.8(3) . . ? N1 Pt1 Br2 94.8(3) . . ? N11 Pt1 Br2 88.7(3) . . ? N1' Pt1 Br2 93.4(3) . . ? N11' Pt1 Br2 93.3(3) . . ? Pd1 Pt1 Br2 177.75(4) . . ? N2' Pd1 N2 166.0(5) . . ? N2' Pd1 Br1 98.2(3) . . ? N2 Pd1 Br1 95.7(3) . . ? N2' Pd1 Pt1 83.7(3) . . ? N2 Pd1 Pt1 82.5(3) . . ? Br1 Pd1 Pt1 173.74(6) . . ? N2' Pd1 Pd2 133.3(3) . . ? N2 Pd1 Pd2 45.0(3) . . ? Br1 Pd1 Pd2 97.19(6) . . ? Pt1 Pd1 Pd2 77.31(4) . . ? N2' Pd1 Pd3 42.8(3) . . ? N2 Pd1 Pd3 130.1(3) . . ? Br1 Pd1 Pd3 109.50(6) . . ? Pt1 Pd1 Pd3 75.96(4) . . ? Pd2 Pd1 Pd3 153.27(5) . . ? N11' Pd2 N22 94.0(4) . . ? N11' Pd2 N21 177.0(4) . . ? N22 Pd2 N21 83.6(4) . . ? N11' Pd2 N2 90.8(4) . . ? N22 Pd2 N2 175.1(5) . . ? N21 Pd2 N2 91.6(5) . . ? N11' Pd2 Pd1 77.7(3) . . ? N22 Pd2 Pd1 135.6(3) . . ? N21 Pd2 Pd1 102.7(3) . . ? N2 Pd2 Pd1 44.7(3) . . ? N11 Pd3 N31 91.7(4) . . ? N11 Pd3 N2' 91.4(4) . . ? N31 Pd3 N2' 176.8(4) . . ? N11 Pd3 N32 175.5(4) . . ? N31 Pd3 N32 83.8(5) . . ? N2' Pd3 N32 93.0(4) . . ? N11 Pd3 Pd1 76.1(3) . . ? N31 Pd3 Pd1 138.2(3) . . ? N2' Pd3 Pd1 42.2(2) . . ? N32 Pd3 Pd1 107.4(4) . . ? Pd3 N11 Pt1 115.0(4) . . ? Pd2 N11' Pt1 112.9(4) . . ? C21 N21 Pd2 107.1(10) . . ? C22 N22 Pd2 108.7(10) . . ? C22 C21 N21 112.2(16) . . ? C21 C22 N22 113.4(14) . . ? C31 N31 Pd3 107.5(9) . . ? C32 N32 Pd3 107.6(9) . . ? C32 C31 N31 113.0(14) . . ? C31 C32 N32 107.9(12) . . ? C2 N1 C6 119.1(11) . . ? C2 N1 Pt1 118.6(8) . . ? C6 N1 Pt1 122.1(8) . . ? N1 C2 N2 118.9(11) . . ? N1 C2 C3 121.1(12) . . ? N2 C2 C3 119.9(12) . . ? C2 N2 Pd1 114.3(8) . . ? C2 N2 Pd2 118.8(8) . . ? Pd1 N2 Pd2 90.3(4) . . ? C4 C3 C2 119.0(14) . . ? C3 C4 C5 119.1(13) . . ? C6 C5 C4 118.9(13) . . ? N1 C6 C5 122.7(13) . . ? C2' N1' C6' 120.5(10) . . ? C2' N1' Pt1 118.2(8) . . ? C6' N1' Pt1 121.2(8) . . ? N1' C2' C3' 118.7(12) . . ? N1' C2' N2' 117.9(11) . . ? C3' C2' N2' 123.4(11) . . ? C2' N2' Pd1 113.7(7) . . ? C2' N2' Pd3 115.5(8) . . ? Pd1 N2' Pd3 94.9(4) . . ? C4' C3' C2' 119.9(12) . . ? C5' C4' C3' 121.4(12) . . ? C4' C5' C6' 118.2(13) . . ? N1' C6' C5' 121.3(12) . . ? O11 N10 O12 128.6(16) . . ? O11 N10 O13 119.5(16) . . ? O12 N10 O13 111.9(15) . . ? O21 N20 O22 107.4(16) . . ? O21A N20 O23A 123.0(35) . . ? O21A N20 O22A 110.8(32) . . ? O23A N20 O22A 124.8(28) . . ? O21 N20 O23 125.9(19) . . ? O22 N20 O23 125.5(19) . . ? 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 Pt1 Pd1 N2' -147.9(4) . . . . ? N11 Pt1 Pd1 N2' -54.6(4) . . . . ? N1' Pt1 Pd1 N2' 31.3(4) . . . . ? N11' Pt1 Pd1 N2' 125.6(4) . . . . ? Br2 Pt1 Pd1 N2' -27.6(11) . . . . ? N1 Pt1 Pd1 N2 29.6(4) . . . . ? N11 Pt1 Pd1 N2 122.9(4) . . . . ? N1' Pt1 Pd1 N2 -151.2(4) . . . . ? N11' Pt1 Pd1 N2 -56.9(4) . . . . ? Br2 Pt1 Pd1 N2 149.9(11) . . . . ? N1 Pt1 Pd1 Br1 103.8(5) . . . . ? N11 Pt1 Pd1 Br1 -162.9(5) . . . . ? N1' Pt1 Pd1 Br1 -76.9(5) . . . . ? N11' Pt1 Pd1 Br1 17.4(5) . . . . ? Br2 Pt1 Pd1 Br1 -135.9(10) . . . . ? N1 Pt1 Pd1 Pd2 75.0(3) . . . . ? N11 Pt1 Pd1 Pd2 168.3(3) . . . . ? N1' Pt1 Pd1 Pd2 -105.7(3) . . . . ? N11' Pt1 Pd1 Pd2 -11.4(2) . . . . ? Br2 Pt1 Pd1 Pd2 -164.7(10) . . . . ? N1 Pt1 Pd1 Pd3 -105.0(3) . . . . ? N11 Pt1 Pd1 Pd3 -11.8(3) . . . . ? N1' Pt1 Pd1 Pd3 74.2(3) . . . . ? N11' Pt1 Pd1 Pd3 168.5(2) . . . . ? Br2 Pt1 Pd1 Pd3 15.3(10) . . . . ? N2' Pd1 Pd2 N11' -56.7(5) . . . . ? N2 Pd1 Pd2 N11' 103.9(5) . . . . ? Br1 Pd1 Pd2 N11' -165.2(3) . . . . ? Pt1 Pd1 Pd2 N11' 11.8(3) . . . . ? Pd3 Pd1 Pd2 N11' 11.7(3) . . . . ? N2' Pd1 Pd2 N22 26.4(6) . . . . ? N2 Pd1 Pd2 N22 -173.0(6) . . . . ? Br1 Pd1 Pd2 N22 -82.1(4) . . . . ? Pt1 Pd1 Pd2 N22 94.9(4) . . . . ? Pd3 Pd1 Pd2 N22 94.8(5) . . . . ? N2' Pd1 Pd2 N21 120.3(5) . . . . ? N2 Pd1 Pd2 N21 -79.2(6) . . . . ? Br1 Pd1 Pd2 N21 11.8(3) . . . . ? Pt1 Pd1 Pd2 N21 -171.3(3) . . . . ? Pd3 Pd1 Pd2 N21 -171.4(3) . . . . ? N2' Pd1 Pd2 N2 -160.6(6) . . . . ? N2 Pd1 Pd2 N2 0.000(4) . . . . ? Br1 Pd1 Pd2 N2 90.9(5) . . . . ? Pt1 Pd1 Pd2 N2 -92.1(5) . . . . ? Pd3 Pd1 Pd2 N2 -92.2(5) . . . . ? N2' Pd1 Pd3 N11 108.2(5) . . . . ? N2 Pd1 Pd3 N11 -55.0(5) . . . . ? Br1 Pd1 Pd3 N11 -170.9(3) . . . . ? Pt1 Pd1 Pd3 N11 12.3(3) . . . . ? Pd2 Pd1 Pd3 N11 12.4(3) . . . . ? N2' Pd1 Pd3 N31 -175.2(6) . . . . ? N2 Pd1 Pd3 N31 21.6(7) . . . . ? Br1 Pd1 Pd3 N31 -94.3(5) . . . . ? Pt1 Pd1 Pd3 N31 88.9(5) . . . . ? Pd2 Pd1 Pd3 N31 89.0(5) . . . . ? N2' Pd1 Pd3 N2' 0.000(3) . . . . ? N2 Pd1 Pd3 N2' -163.2(6) . . . . ? Br1 Pd1 Pd3 N2' 80.9(4) . . . . ? Pt1 Pd1 Pd3 N2' -95.9(4) . . . . ? Pd2 Pd1 Pd3 N2' -95.8(4) . . . . ? N2' Pd1 Pd3 N32 -74.7(5) . . . . ? N2 Pd1 Pd3 N32 122.1(5) . . . . ? Br1 Pd1 Pd3 N32 6.2(3) . . . . ? Pt1 Pd1 Pd3 N32 -170.6(3) . . . . ? Pd2 Pd1 Pd3 N32 -170.5(3) . . . . ? N31 Pd3 N11 Pt1 -155.8(5) . . . . ? N2' Pd3 N11 Pt1 23.5(5) . . . . ? N32 Pd3 N11 Pt1 -157.9(51) . . . . ? Pd1 Pd3 N11 Pt1 -16.2(4) . . . . ? N1 Pt1 N11 Pd3 105.4(5) . . . . ? N1' Pt1 N11 Pd3 -66.4(5) . . . . ? N11' Pt1 N11 Pd3 27.1(106) . . . . ? Pd1 Pt1 N11 Pd3 19.1(4) . . . . ? Br2 Pt1 N11 Pd3 -159.9(4) . . . . ? N22 Pd2 N11' Pt1 -151.1(5) . . . . ? N21 Pd2 N11' Pt1 -112.6(72) . . . . ? N2 Pd2 N11' Pt1 27.8(4) . . . . ? Pd1 Pd2 N11' Pt1 -15.3(3) . . . . ? N1 Pt1 N11' Pd2 -68.8(5) . . . . ? N11 Pt1 N11' Pd2 9.6(105) . . . . ? N1' Pt1 N11' Pd2 103.0(5) . . . . ? Pd1 Pt1 N11' Pd2 17.6(4) . . . . ? Br2 Pt1 N11' Pd2 -163.4(4) . . . . ? N11' Pd2 N21 C21 -23.4(77) . . . . ? N22 Pd2 N21 C21 15.3(10) . . . . ? N2 Pd2 N21 C21 -163.8(10) . . . . ? Pd1 Pd2 N21 C21 -120.0(10) . . . . ? N11' Pd2 N22 C22 -175.7(10) . . . . ? N21 Pd2 N22 C22 6.2(10) . . . . ? N2 Pd2 N22 C22 16.6(49) . . . . ? Pd1 Pd2 N22 C22 107.8(10) . . . . ? Pd2 N21 C21 C22 -36.1(19) . . . . ? N21 C21 C22 N22 44.3(25) . . . . ? Pd2 N22 C22 C21 -28.8(21) . . . . ? N11 Pd3 N31 C31 163.6(10) . . . . ? N2' Pd3 N31 C31 -3.8(77) . . . . ? N32 Pd3 N31 C31 -16.5(10) . . . . ? Pd1 Pd3 N31 C31 92.8(10) . . . . ? N11 Pd3 N32 C32 -6.8(58) . . . . ? N31 Pd3 N32 C32 -8.9(9) . . . . ? N2' Pd3 N32 C32 171.8(9) . . . . ? Pd1 Pd3 N32 C32 -147.7(8) . . . . ? Pd3 N31 C31 C32 42.2(16) . . . . ? N31 C31 C32 N32 -50.8(18) . . . . ? Pd3 N32 C32 C31 32.9(15) . . . . ? N11 Pt1 N1 C2 -113.8(9) . . . . ? N1' Pt1 N1 C2 -30.1(31) . . . . ? N11' Pt1 N1 C2 64.2(9) . . . . ? Pd1 Pt1 N1 C2 -24.7(8) . . . . ? Br2 Pt1 N1 C2 157.2(8) . . . . ? N11 Pt1 N1 C6 60.9(9) . . . . ? N1' Pt1 N1 C6 144.7(24) . . . . ? N11' Pt1 N1 C6 -121.0(10) . . . . ? Pd1 Pt1 N1 C6 150.0(9) . . . . ? Br2 Pt1 N1 C6 -28.0(9) . . . . ? C6 N1 C2 N2 -176.6(11) . . . . ? Pt1 N1 C2 N2 -1.7(15) . . . . ? C6 N1 C2 C3 -0.1(17) . . . . ? Pt1 N1 C2 C3 174.8(9) . . . . ? N1 C2 N2 Pd1 36.7(14) . . . . ? C3 C2 N2 Pd1 -139.9(9) . . . . ? N1 C2 N2 Pd2 -68.1(13) . . . . ? C3 C2 N2 Pd2 115.3(11) . . . . ? N2' Pd1 N2 C2 -32.2(22) . . . . ? Br1 Pd1 N2 C2 143.5(8) . . . . ? Pt1 Pd1 N2 C2 -42.5(8) . . . . ? Pd2 Pd1 N2 C2 -122.0(10) . . . . ? Pd3 Pd1 N2 C2 22.0(11) . . . . ? N2' Pd1 N2 Pd2 89.8(17) . . . . ? Br1 Pd1 N2 Pd2 -94.4(3) . . . . ? Pt1 Pd1 N2 Pd2 79.5(3) . . . . ? Pd2 Pd1 N2 Pd2 0.000(4) . . . . ? Pd3 Pd1 N2 Pd2 144.0(2) . . . . ? N11' Pd2 N2 C2 46.7(9) . . . . ? N22 Pd2 N2 C2 -145.6(42) . . . . ? N21 Pd2 N2 C2 -135.3(9) . . . . ? Pd1 Pd2 N2 C2 118.2(10) . . . . ? N11' Pd2 N2 Pd1 -71.6(4) . . . . ? N22 Pd2 N2 Pd1 96.2(44) . . . . ? N21 Pd2 N2 Pd1 106.5(4) . . . . ? Pd1 Pd2 N2 Pd1 0.000(3) . . . . ? N1 C2 C3 C4 2.5(18) . . . . ? N2 C2 C3 C4 178.9(12) . . . . ? C2 C3 C4 C5 -2.1(20) . . . . ? C3 C4 C5 C6 -0.5(20) . . . . ? C2 N1 C6 C5 -2.6(18) . . . . ? Pt1 N1 C6 C5 -177.3(9) . . . . ? C4 C5 C6 N1 2.9(20) . . . . ? N1 Pt1 N1' C2' -20.3(31) . . . . ? N11 Pt1 N1' C2' 64.0(8) . . . . ? N11' Pt1 N1' C2' -114.0(8) . . . . ? Pd1 Pt1 N1' C2' -25.6(8) . . . . ? Br2 Pt1 N1' C2' 152.4(8) . . . . ? N1 Pt1 N1' C6' 155.7(24) . . . . ? N11 Pt1 N1' C6' -120.1(9) . . . . ? N11' Pt1 N1' C6' 61.9(9) . . . . ? Pd1 Pt1 N1' C6' 150.3(9) . . . . ? Br2 Pt1 N1' C6' -31.6(9) . . . . ? C6' N1' C2' C3' 1.7(17) . . . . ? Pt1 N1' C2' C3' 177.7(8) . . . . ? C6' N1' C2' N2' -177.4(10) . . . . ? Pt1 N1' C2' N2' -1.4(14) . . . . ? N1' C2' N2' Pd1 37.7(13) . . . . ? C3' C2' N2' Pd1 -141.4(10) . . . . ? N1' C2' N2' Pd3 -70.6(12) . . . . ? C3' C2' N2' Pd3 110.3(11) . . . . ? N2 Pd1 N2' C2' -54.9(20) . . . . ? Br1 Pd1 N2' C2' 129.4(8) . . . . ? Pt1 Pd1 N2' C2' -44.6(8) . . . . ? Pd2 Pd1 N2' C2' 21.4(10) . . . . ? Pd3 Pd1 N2' C2' -120.7(10) . . . . ? N2 Pd1 N2' Pd3 65.8(17) . . . . ? Br1 Pd1 N2' Pd3 -109.9(3) . . . . ? Pt1 Pd1 N2' Pd3 76.1(3) . . . . ? Pd2 Pd1 N2' Pd3 142.1(2) . . . . ? Pd3 Pd1 N2' Pd3 0.0 . . . . ? N11 Pd3 N2' C2' 52.0(8) . . . . ? N31 Pd3 N2' C2' -140.6(70) . . . . ? N32 Pd3 N2' C2' -127.9(8) . . . . ? Pd1 Pd3 N2' C2' 119.3(9) . . . . ? N11 Pd3 N2' Pd1 -67.3(4) . . . . ? N31 Pd3 N2' Pd1 100.1(71) . . . . ? N32 Pd3 N2' Pd1 112.8(5) . . . . ? Pd1 Pd3 N2' Pd1 0.000(2) . . . . ? N1' C2' C3' C4' -3.0(18) . . . . ? N2' C2' C3' C4' 176.0(12) . . . . ? C2' C3' C4' C5' 2.9(20) . . . . ? C3' C4' C5' C6' -1.5(20) . . . . ? C2' N1' C6' C5' -0.4(17) . . . . ? Pt1 N1' C6' C5' -176.2(9) . . . . ? C4' C5' C6' N1' 0.2(19) . . . . ? _refine_diff_density_max 1.600 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.148