# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Datong Song' _publ_contact_author_email DSONG@CHEM.UTORONTO.CA _publ_section_title ; Novel Dinuclear and Trinuclear Palladium beta-Diiminate Complexes Containing Amido-Chloro Double-Bridges ; loop_ _publ_author_name 'Datong Song.' 'Alen Hadzovic' 'John Janetzko' # Attachment 'CIFs.txt' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 680460' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H63 Cl3 N6 Pd3, C H2 Cl2' _chemical_formula_sum 'C55 H65 Cl5 N6 Pd3' _chemical_formula_weight 1306.58 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9402(3) _cell_length_b 15.3099(7) _cell_length_c 15.5713(5) _cell_angle_alpha 85.923(2) _cell_angle_beta 78.728(2) _cell_angle_gamma 88.962(2) _cell_volume 2784.49(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 29972 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.56 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.822 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29972 _diffrn_reflns_av_R_equivalents 0.0919 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.56 _reflns_number_total 12695 _reflns_number_gt 8374 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+3.9226P] 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 12695 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1021 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1845 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.59607(4) 0.86776(3) 0.27902(3) 0.03815(13) Uani 1 1 d . . . Pd2 Pd 0.59475(4) 0.67259(3) 0.26717(3) 0.04253(14) Uani 1 1 d . . . Pd3 Pd 0.51179(4) 0.84529(3) 0.09068(3) 0.04760(15) Uani 1 1 d . . . Cl1 Cl 0.46730(13) 0.76507(11) 0.35920(10) 0.0504(4) Uani 1 1 d . . . Cl1S Cl 0.9724(2) 0.1643(2) 0.06994(15) 0.0943(7) Uani 1 1 d . . . Cl2 Cl 0.31835(14) 0.85129(13) 0.15181(11) 0.0575(4) Uani 1 1 d . . . Cl2S Cl 1.0388(3) 0.3261(2) 0.13373(18) 0.1201(10) Uani 1 1 d . . . Cl3 Cl 0.70033(14) 0.82237(13) 0.02373(12) 0.0615(5) Uani 1 1 d . . . N1 N 0.4741(4) 0.9617(3) 0.2750(3) 0.0402(11) Uani 1 1 d . . . N2 N 0.7041(4) 0.9482(3) 0.1937(3) 0.0410(11) Uani 1 1 d . . . N3 N 0.7152(4) 0.7664(3) 0.2804(3) 0.0400(11) Uani 1 1 d . . . H3N H 0.7722 0.7718 0.2302 0.048 Uiso 1 1 calc R . . N4 N 0.7081(4) 0.6044(3) 0.1847(3) 0.0448(12) Uani 1 1 d . . . N5 N 0.4695(4) 0.5891(4) 0.2586(3) 0.0481(12) Uani 1 1 d . . . N6 N 0.4750(5) 0.7171(4) 0.0599(4) 0.0565(14) Uani 1 1 d . . . H6NA H 0.5372 0.6815 0.0630 0.068 Uiso 1 1 calc R . . H6NB H 0.4145 0.6950 0.1011 0.068 Uiso 1 1 calc R . . C1 C 0.3727(5) 1.0614(4) 0.1852(4) 0.0480(15) Uani 1 1 d . . . H1A H 0.3230 1.0711 0.2417 0.072 Uiso 1 1 calc R . . H1B H 0.3272 1.0393 0.1454 0.072 Uiso 1 1 calc R . . H1C H 0.4086 1.1167 0.1595 0.072 Uiso 1 1 calc R . . C1S C 1.0504(9) 0.2086(7) 0.1330(6) 0.093(3) Uani 1 1 d . . . H1SA H 1.1315 0.1927 0.1126 0.111 Uiso 1 1 calc R . . H1SB H 1.0267 0.1829 0.1939 0.111 Uiso 1 1 calc R . . C2 C 0.4635(5) 0.9956(4) 0.1989(4) 0.0403(13) Uani 1 1 d . . . C3 C 0.5463(5) 0.9741(4) 0.1195(4) 0.0445(14) Uani 1 1 d . . . H3A H 0.5320 1.0150 0.0697 0.053 Uiso 1 1 calc R . . C4 C 0.6671(5) 0.9828(4) 0.1259(4) 0.0425(13) Uani 1 1 d . . . C5 C 0.7407(6) 1.0356(5) 0.0526(4) 0.0600(18) Uani 1 1 d . . . H5A H 0.8207 1.0300 0.0588 0.090 Uiso 1 1 calc R . . H5B H 0.7174 1.0973 0.0545 0.090 Uiso 1 1 calc R . . H5C H 0.7324 1.0142 -0.0037 0.090 Uiso 1 1 calc R . . C6 C 0.3939(5) 0.9815(4) 0.3522(4) 0.0479(15) Uani 1 1 d . . . C7 C 0.4256(6) 1.0343(5) 0.4107(4) 0.0589(18) Uani 1 1 d . . . H7A H 0.5016 1.0554 0.4017 0.071 Uiso 1 1 calc R . . C8 C 0.3445(9) 1.0570(6) 0.4840(5) 0.077(2) Uani 1 1 d . . . H8A H 0.3653 1.0946 0.5242 0.092 Uiso 1 1 calc R . . C9 C 0.2368(8) 1.0255(6) 0.4974(5) 0.078(3) Uani 1 1 d . . . H9A H 0.1817 1.0429 0.5460 0.094 Uiso 1 1 calc R . . C10 C 0.2064(7) 0.9692(7) 0.4422(6) 0.084(3) Uani 1 1 d . . . H10B H 0.1317 0.9451 0.4540 0.101 Uiso 1 1 calc R . . C11 C 0.2848(6) 0.9469(5) 0.3686(5) 0.0607(18) Uani 1 1 d . . . H11A H 0.2636 0.9081 0.3297 0.073 Uiso 1 1 calc R . . C12 C 0.8220(5) 0.9566(4) 0.2015(4) 0.0429(14) Uani 1 1 d . . . C13 C 0.9078(5) 0.9159(5) 0.1437(4) 0.0513(16) Uani 1 1 d . . . H13A H 0.8899 0.8842 0.0979 0.062 Uiso 1 1 calc R . . C14 C 1.0201(6) 0.9226(5) 0.1547(5) 0.0620(19) Uani 1 1 d . . . H14A H 1.0802 0.8962 0.1155 0.074 Uiso 1 1 calc R . . C15 C 1.0442(5) 0.9679(5) 0.2227(4) 0.0577(18) Uani 1 1 d . . . H15A H 1.1211 0.9720 0.2300 0.069 Uiso 1 1 calc R . . C16 C 0.9593(5) 1.0067(5) 0.2797(4) 0.0551(17) Uani 1 1 d . . . H16A H 0.9772 1.0383 0.3256 0.066 Uiso 1 1 calc R . . C17 C 0.8464(5) 0.9996(4) 0.2697(4) 0.0490(15) Uani 1 1 d . . . H17A H 0.7866 1.0246 0.3102 0.059 Uiso 1 1 calc R . . C18 C 0.7626(5) 0.7552(4) 0.3544(4) 0.0456(14) Uani 1 1 d . . . C19 C 0.7023(6) 0.7153(5) 0.4351(4) 0.0545(17) Uani 1 1 d . . . H19A H 0.6272 0.6938 0.4393 0.065 Uiso 1 1 calc R . . C20 C 0.7538(6) 0.7082(5) 0.5070(5) 0.0619(19) Uani 1 1 d . . . H20A H 0.7125 0.6807 0.5600 0.074 Uiso 1 1 calc R . . C21 C 0.8621(5) 0.7388(5) 0.5064(4) 0.0498(15) Uani 1 1 d . . . C22 C 0.9220(5) 0.7749(4) 0.4269(4) 0.0500(15) Uani 1 1 d . . . H22A H 0.9979 0.7945 0.4232 0.060 Uiso 1 1 calc R . . C23 C 0.8726(5) 0.7833(4) 0.3515(4) 0.0501(15) Uani 1 1 d . . . H23A H 0.9156 0.8087 0.2979 0.060 Uiso 1 1 calc R . . C24 C 0.9071(6) 0.7315(5) 0.5922(4) 0.0589(18) Uani 1 1 d . . . C25 C 1.0237(6) 0.7742(6) 0.5818(5) 0.072(2) Uani 1 1 d . . . H25A H 1.0795 0.7437 0.5393 0.108 Uiso 1 1 calc R . . H25B H 1.0478 0.7706 0.6386 0.108 Uiso 1 1 calc R . . H25C H 1.0188 0.8358 0.5609 0.108 Uiso 1 1 calc R . . C26 C 0.9121(7) 0.6350(6) 0.6252(5) 0.077(2) Uani 1 1 d . . . H26A H 0.9653 0.6033 0.5820 0.115 Uiso 1 1 calc R . . H26B H 0.8359 0.6093 0.6335 0.115 Uiso 1 1 calc R . . H26C H 0.9383 0.6308 0.6812 0.115 Uiso 1 1 calc R . . C27 C 0.8233(7) 0.7814(6) 0.6608(5) 0.077(2) Uani 1 1 d . . . H27A H 0.8201 0.8432 0.6399 0.115 Uiso 1 1 calc R . . H27B H 0.8497 0.7770 0.7167 0.115 Uiso 1 1 calc R . . H27C H 0.7470 0.7557 0.6691 0.115 Uiso 1 1 calc R . . C28 C 0.7734(6) 0.5149(5) 0.0594(5) 0.0603(18) Uani 1 1 d . . . H28A H 0.8177 0.5624 0.0236 0.090 Uiso 1 1 calc R . . H28B H 0.7397 0.4790 0.0214 0.090 Uiso 1 1 calc R . . H28C H 0.8238 0.4784 0.0899 0.090 Uiso 1 1 calc R . . C29 C 0.6788(6) 0.5534(4) 0.1265(4) 0.0491(15) Uani 1 1 d . . . C30 C 0.5670(5) 0.5295(4) 0.1265(4) 0.0498(15) Uani 1 1 d . . . H30A H 0.5548 0.5022 0.0762 0.060 Uiso 1 1 calc R . . C31 C 0.4720(6) 0.5406(4) 0.1909(4) 0.0514(16) Uani 1 1 d . . . C32 C 0.3635(6) 0.4912(5) 0.1862(5) 0.0619(19) Uani 1 1 d . . . H32A H 0.3012 0.5332 0.1830 0.093 Uiso 1 1 calc R . . H32B H 0.3426 0.4513 0.2387 0.093 Uiso 1 1 calc R . . H32C H 0.3770 0.4576 0.1339 0.093 Uiso 1 1 calc R . . C33 C 0.8274(5) 0.6155(4) 0.1864(4) 0.0498(15) Uani 1 1 d . . . C34 C 0.8734(6) 0.5711(5) 0.2531(5) 0.0605(18) Uani 1 1 d . . . H34A H 0.8265 0.5341 0.2967 0.073 Uiso 1 1 calc R . . C35 C 0.9872(7) 0.5814(6) 0.2553(6) 0.072(2) Uani 1 1 d . . . H35A H 1.0189 0.5513 0.3005 0.087 Uiso 1 1 calc R . . C36 C 1.0555(7) 0.6354(6) 0.1919(6) 0.075(2) Uani 1 1 d . . . H36A H 1.1342 0.6414 0.1932 0.090 Uiso 1 1 calc R . . C37 C 1.0098(6) 0.6807(6) 0.1270(6) 0.073(2) Uani 1 1 d . . . H37A H 1.0565 0.7179 0.0836 0.088 Uiso 1 1 calc R . . C38 C 0.8945(6) 0.6710(5) 0.1259(5) 0.0577(17) Uani 1 1 d . . . H38A H 0.8620 0.7035 0.0826 0.069 Uiso 1 1 calc R . . C39 C 0.3778(5) 0.5799(5) 0.3346(4) 0.0517(16) Uani 1 1 d . . . C40 C 0.3962(6) 0.5274(5) 0.4065(5) 0.0646(19) Uani 1 1 d . . . H40A H 0.4672 0.4981 0.4053 0.078 Uiso 1 1 calc R . . C41 C 0.3098(7) 0.5177(5) 0.4808(5) 0.072(2) Uani 1 1 d . . . H41A H 0.3214 0.4812 0.5303 0.086 Uiso 1 1 calc R . . C42 C 0.2094(7) 0.5605(7) 0.4823(6) 0.079(2) Uani 1 1 d . . . H42A H 0.1506 0.5535 0.5330 0.094 Uiso 1 1 calc R . . C43 C 0.1913(6) 0.6131(6) 0.4124(6) 0.073(2) Uani 1 1 d . . . H43A H 0.1202 0.6425 0.4142 0.087 Uiso 1 1 calc R . . C44 C 0.2766(6) 0.6239(5) 0.3384(5) 0.0626(19) Uani 1 1 d . . . H44A H 0.2648 0.6620 0.2901 0.075 Uiso 1 1 calc R . . C45 C 0.4479(6) 0.7148(4) -0.0254(4) 0.0536(16) Uani 1 1 d . . . C46 C 0.5320(6) 0.7131(5) -0.0996(4) 0.0551(16) Uani 1 1 d . . . H46A H 0.6100 0.7120 -0.0945 0.066 Uiso 1 1 calc R . . C47 C 0.5034(6) 0.7130(5) -0.1827(5) 0.0567(17) Uani 1 1 d . . . H47A H 0.5631 0.7130 -0.2330 0.068 Uiso 1 1 calc R . . C48 C 0.3927(5) 0.7130(5) -0.1939(4) 0.0523(16) Uani 1 1 d . . . C49 C 0.3087(6) 0.7151(5) -0.1185(5) 0.0573(17) Uani 1 1 d . . . H49A H 0.2307 0.7159 -0.1237 0.069 Uiso 1 1 calc R . . C50 C 0.3355(6) 0.7163(5) -0.0370(5) 0.0567(17) Uani 1 1 d . . . H50A H 0.2755 0.7181 0.0129 0.068 Uiso 1 1 calc R . . C51 C 0.3619(6) 0.7151(5) -0.2848(5) 0.0589(17) Uani 1 1 d . . . C52 C 0.2941(7) 0.7997(6) -0.2982(6) 0.084(3) Uani 1 1 d . . . H52A H 0.2273 0.8022 -0.2505 0.126 Uiso 1 1 calc R . . H52B H 0.2688 0.8004 -0.3545 0.126 Uiso 1 1 calc R . . H52C H 0.3428 0.8505 -0.2982 0.126 Uiso 1 1 calc R . . C53 C 0.4653(7) 0.7137(7) -0.3608(5) 0.082(3) Uani 1 1 d . . . H53A H 0.5093 0.6598 -0.3543 0.124 Uiso 1 1 calc R . . H53B H 0.5137 0.7645 -0.3599 0.124 Uiso 1 1 calc R . . H53C H 0.4388 0.7158 -0.4167 0.124 Uiso 1 1 calc R . . C54 C 0.2875(8) 0.6356(6) -0.2883(5) 0.083(3) Uani 1 1 d . . . H54A H 0.3310 0.5818 -0.2801 0.125 Uiso 1 1 calc R . . H54B H 0.2643 0.6374 -0.3454 0.125 Uiso 1 1 calc R . . H54C H 0.2194 0.6367 -0.2415 0.125 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 0.0421(2) 0.0376(3) 0.0362(2) 0.00254(18) -0.01277(18) -0.00044(19) Pd2 0.0466(3) 0.0384(3) 0.0441(3) 0.0010(2) -0.0139(2) 0.0013(2) Pd3 0.0536(3) 0.0473(3) 0.0449(3) -0.0019(2) -0.0179(2) 0.0044(2) Cl1 0.0542(8) 0.0445(9) 0.0515(9) 0.0025(7) -0.0102(7) -0.0023(7) Cl1S 0.0903(15) 0.114(2) 0.0800(14) -0.0103(14) -0.0173(12) -0.0079(14) Cl2 0.0555(9) 0.0606(11) 0.0588(10) -0.0068(8) -0.0160(7) -0.0012(8) Cl2S 0.155(3) 0.124(3) 0.0827(17) -0.0061(17) -0.0241(17) -0.032(2) Cl3 0.0548(9) 0.0724(13) 0.0611(10) -0.0151(9) -0.0180(8) 0.0089(8) N1 0.049(3) 0.035(3) 0.040(3) 0.000(2) -0.018(2) 0.002(2) N2 0.047(3) 0.041(3) 0.037(2) -0.001(2) -0.012(2) -0.001(2) N3 0.062(3) 0.033(3) 0.024(2) 0.0052(19) -0.009(2) 0.007(2) N4 0.050(3) 0.041(3) 0.045(3) 0.005(2) -0.015(2) 0.003(2) N5 0.050(3) 0.044(3) 0.053(3) 0.003(3) -0.020(2) 0.001(2) N6 0.071(4) 0.038(3) 0.061(3) -0.002(3) -0.014(3) 0.001(3) C1 0.050(3) 0.045(4) 0.050(3) 0.011(3) -0.017(3) 0.003(3) C1S 0.117(7) 0.090(7) 0.065(5) -0.013(5) 0.000(5) 0.009(6) C2 0.046(3) 0.032(3) 0.047(3) -0.005(3) -0.018(3) 0.001(2) C3 0.050(3) 0.045(4) 0.044(3) -0.002(3) -0.023(3) 0.010(3) C4 0.051(3) 0.042(4) 0.035(3) 0.002(3) -0.010(2) 0.003(3) C5 0.070(4) 0.061(5) 0.050(4) 0.015(3) -0.020(3) -0.010(4) C6 0.051(3) 0.046(4) 0.047(3) 0.005(3) -0.012(3) 0.009(3) C7 0.075(4) 0.060(5) 0.042(3) -0.006(3) -0.012(3) 0.016(4) C8 0.121(7) 0.058(5) 0.057(5) -0.009(4) -0.031(5) 0.020(5) C9 0.093(6) 0.080(6) 0.050(4) 0.010(4) 0.006(4) 0.033(5) C10 0.073(5) 0.083(7) 0.081(6) 0.021(5) 0.013(4) 0.014(5) C11 0.059(4) 0.063(5) 0.056(4) 0.002(4) -0.003(3) -0.002(4) C12 0.040(3) 0.044(4) 0.045(3) 0.014(3) -0.013(3) -0.015(3) C13 0.049(3) 0.062(5) 0.042(3) 0.006(3) -0.012(3) -0.003(3) C14 0.051(4) 0.077(6) 0.055(4) 0.008(4) -0.007(3) -0.002(4) C15 0.046(3) 0.068(5) 0.059(4) 0.021(4) -0.020(3) -0.017(3) C16 0.059(4) 0.054(4) 0.054(4) 0.006(3) -0.020(3) -0.011(3) C17 0.055(4) 0.045(4) 0.046(3) 0.005(3) -0.010(3) -0.003(3) C18 0.046(3) 0.041(4) 0.049(3) 0.006(3) -0.012(3) 0.003(3) C19 0.057(4) 0.055(4) 0.056(4) 0.002(3) -0.027(3) -0.001(3) C20 0.058(4) 0.075(6) 0.050(4) 0.016(4) -0.013(3) 0.002(4) C21 0.054(4) 0.049(4) 0.046(3) 0.006(3) -0.012(3) 0.000(3) C22 0.054(4) 0.041(4) 0.059(4) -0.002(3) -0.023(3) 0.003(3) C23 0.053(4) 0.046(4) 0.049(3) 0.009(3) -0.008(3) -0.002(3) C24 0.061(4) 0.069(5) 0.050(4) 0.001(3) -0.020(3) 0.009(4) C25 0.068(5) 0.095(7) 0.058(4) -0.006(4) -0.026(4) 0.004(4) C26 0.086(5) 0.081(6) 0.068(5) 0.019(4) -0.034(4) 0.002(5) C27 0.083(5) 0.098(7) 0.052(4) -0.009(4) -0.018(4) 0.018(5) C28 0.065(4) 0.054(5) 0.062(4) -0.010(4) -0.010(3) 0.001(3) C29 0.062(4) 0.040(4) 0.045(3) 0.004(3) -0.016(3) 0.006(3) C30 0.058(4) 0.041(4) 0.054(4) -0.001(3) -0.019(3) -0.001(3) C31 0.058(4) 0.038(4) 0.061(4) 0.003(3) -0.023(3) 0.003(3) C32 0.055(4) 0.053(5) 0.082(5) -0.013(4) -0.021(4) -0.004(3) C33 0.054(4) 0.044(4) 0.054(4) -0.003(3) -0.017(3) 0.006(3) C34 0.069(4) 0.052(5) 0.065(4) 0.000(4) -0.026(4) 0.008(3) C35 0.075(5) 0.059(5) 0.094(6) 0.000(5) -0.048(5) 0.010(4) C36 0.053(4) 0.079(6) 0.098(6) -0.009(5) -0.027(4) 0.004(4) C37 0.047(4) 0.081(6) 0.091(6) -0.003(5) -0.015(4) 0.000(4) C38 0.057(4) 0.058(5) 0.058(4) 0.004(3) -0.013(3) 0.004(3) C39 0.049(3) 0.050(4) 0.058(4) -0.005(3) -0.012(3) 0.001(3) C40 0.062(4) 0.056(5) 0.076(5) 0.001(4) -0.016(4) 0.005(4) C41 0.083(5) 0.055(5) 0.071(5) 0.005(4) -0.004(4) -0.002(4) C42 0.066(5) 0.088(7) 0.077(6) -0.014(5) 0.005(4) -0.018(5) C43 0.051(4) 0.081(6) 0.089(6) -0.020(5) -0.018(4) 0.003(4) C44 0.050(4) 0.064(5) 0.077(5) -0.020(4) -0.014(3) -0.003(3) C45 0.068(4) 0.042(4) 0.053(4) -0.002(3) -0.018(3) 0.007(3) C46 0.056(4) 0.048(4) 0.061(4) -0.003(3) -0.011(3) -0.002(3) C47 0.061(4) 0.050(4) 0.057(4) -0.007(3) -0.005(3) -0.004(3) C48 0.054(4) 0.046(4) 0.057(4) -0.007(3) -0.011(3) -0.004(3) C49 0.057(4) 0.050(4) 0.068(4) -0.010(4) -0.017(3) -0.002(3) C50 0.056(4) 0.056(5) 0.058(4) -0.008(3) -0.009(3) 0.000(3) C51 0.077(5) 0.045(4) 0.055(4) -0.002(3) -0.016(3) 0.006(3) C52 0.084(5) 0.084(7) 0.087(6) 0.014(5) -0.032(5) 0.011(5) C53 0.090(6) 0.088(7) 0.064(5) -0.002(5) -0.004(4) 0.004(5) C54 0.102(6) 0.080(7) 0.069(5) -0.005(5) -0.017(5) -0.019(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 Pd1 N2 2.025(5) . ? Pd1 N1 2.034(5) . ? Pd1 N3 2.087(5) . ? Pd1 Cl1 2.3351(19) . ? Pd2 N4 2.008(5) . ? Pd2 N5 2.016(5) . ? Pd2 N3 2.100(5) . ? Pd2 Cl1 2.3941(18) . ? Pd3 C3 2.119(6) . ? Pd3 N6 2.127(6) . ? Pd3 Cl3 2.3204(18) . ? Pd3 Cl2 2.3226(18) . ? Cl1S C1S 1.664(10) . ? Cl2S C1S 1.804(11) . ? N1 C2 1.288(7) . ? N1 C6 1.430(7) . ? N2 C4 1.297(7) . ? N2 C12 1.445(7) . ? N3 C18 1.379(7) . ? N4 C29 1.337(8) . ? N4 C33 1.443(8) . ? N5 C31 1.327(8) . ? N5 C39 1.447(8) . ? N6 C45 1.430(8) . ? C1 C2 1.502(8) . ? C2 C3 1.477(8) . ? C3 C4 1.474(8) . ? C4 C5 1.494(9) . ? C6 C7 1.370(9) . ? C6 C11 1.385(9) . ? C7 C8 1.405(10) . ? C8 C9 1.355(13) . ? C9 C10 1.361(13) . ? C10 C11 1.390(10) . ? C12 C17 1.371(9) . ? C12 C13 1.393(9) . ? C13 C14 1.392(9) . ? C14 C15 1.384(10) . ? C15 C16 1.367(9) . ? C16 C17 1.394(9) . ? C18 C23 1.381(9) . ? C18 C19 1.421(9) . ? C19 C20 1.375(9) . ? C20 C21 1.382(9) . ? C21 C22 1.385(9) . ? C21 C24 1.530(9) . ? C22 C23 1.411(9) . ? C24 C25 1.523(11) . ? C24 C26 1.534(11) . ? C24 C27 1.549(10) . ? C28 C29 1.522(9) . ? C29 C30 1.391(9) . ? C30 C31 1.376(9) . ? C31 C32 1.529(9) . ? C33 C38 1.366(10) . ? C33 C34 1.398(9) . ? C34 C35 1.378(10) . ? C35 C36 1.384(12) . ? C36 C37 1.379(12) . ? C37 C38 1.390(10) . ? C39 C44 1.366(9) . ? C39 C40 1.383(10) . ? C40 C41 1.392(10) . ? C41 C42 1.353(11) . ? C42 C43 1.358(12) . ? C43 C44 1.383(11) . ? C45 C46 1.376(9) . ? C45 C50 1.388(9) . ? C46 C47 1.401(9) . ? C47 C48 1.366(9) . ? C48 C49 1.388(9) . ? C48 C51 1.530(10) . ? C49 C50 1.370(10) . ? C51 C54 1.530(11) . ? C51 C53 1.534(10) . ? C51 C52 1.539(11) . ? 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 N2 Pd1 N1 87.2(2) . . ? N2 Pd1 N3 94.40(19) . . ? N1 Pd1 N3 176.70(19) . . ? N2 Pd1 Cl1 171.55(14) . . ? N1 Pd1 Cl1 93.64(15) . . ? N3 Pd1 Cl1 84.33(15) . . ? N4 Pd2 N5 90.8(2) . . ? N4 Pd2 N3 93.58(19) . . ? N5 Pd2 N3 175.50(19) . . ? N4 Pd2 Cl1 175.10(16) . . ? N5 Pd2 Cl1 92.99(15) . . ? N3 Pd2 Cl1 82.61(13) . . ? C3 Pd3 N6 178.8(2) . . ? C3 Pd3 Cl3 92.30(17) . . ? N6 Pd3 Cl3 88.15(17) . . ? C3 Pd3 Cl2 94.85(17) . . ? N6 Pd3 Cl2 84.69(17) . . ? Cl3 Pd3 Cl2 172.81(7) . . ? Pd1 Cl1 Pd2 78.96(5) . . ? C2 N1 C6 120.8(5) . . ? C2 N1 Pd1 117.4(4) . . ? C6 N1 Pd1 121.3(4) . . ? C4 N2 C12 121.3(5) . . ? C4 N2 Pd1 117.0(4) . . ? C12 N2 Pd1 121.1(4) . . ? C18 N3 Pd1 116.2(4) . . ? C18 N3 Pd2 116.1(4) . . ? Pd1 N3 Pd2 91.81(19) . . ? C29 N4 C33 119.3(5) . . ? C29 N4 Pd2 123.4(4) . . ? C33 N4 Pd2 117.2(4) . . ? C31 N5 C39 120.8(6) . . ? C31 N5 Pd2 123.5(5) . . ? C39 N5 Pd2 115.7(4) . . ? C45 N6 Pd3 113.0(4) . . ? Cl1S C1S Cl2S 114.2(6) . . ? N1 C2 C3 120.4(5) . . ? N1 C2 C1 123.4(5) . . ? C3 C2 C1 116.2(5) . . ? C4 C3 C2 114.8(5) . . ? C4 C3 Pd3 110.7(4) . . ? C2 C3 Pd3 107.8(4) . . ? N2 C4 C3 120.5(5) . . ? N2 C4 C5 123.2(6) . . ? C3 C4 C5 116.3(5) . . ? C7 C6 C11 119.8(6) . . ? C7 C6 N1 119.8(6) . . ? C11 C6 N1 120.4(6) . . ? C6 C7 C8 119.3(7) . . ? C9 C8 C7 120.2(8) . . ? C8 C9 C10 120.8(8) . . ? C9 C10 C11 119.9(9) . . ? C6 C11 C10 119.8(8) . . ? C17 C12 C13 121.1(5) . . ? C17 C12 N2 118.9(5) . . ? C13 C12 N2 119.9(5) . . ? C14 C13 C12 118.6(6) . . ? C15 C14 C13 119.8(7) . . ? C16 C15 C14 121.2(6) . . ? C15 C16 C17 119.4(6) . . ? C12 C17 C16 119.8(6) . . ? N3 C18 C23 119.6(6) . . ? N3 C18 C19 122.5(6) . . ? C23 C18 C19 117.8(6) . . ? C20 C19 C18 119.4(6) . . ? C19 C20 C21 123.7(7) . . ? C20 C21 C22 116.6(6) . . ? C20 C21 C24 118.7(6) . . ? C22 C21 C24 124.7(6) . . ? C21 C22 C23 121.5(6) . . ? C18 C23 C22 120.8(6) . . ? C25 C24 C21 112.0(6) . . ? C25 C24 C26 110.7(6) . . ? C21 C24 C26 109.8(6) . . ? C25 C24 C27 107.1(7) . . ? C21 C24 C27 107.9(5) . . ? C26 C24 C27 109.3(7) . . ? N4 C29 C30 123.8(6) . . ? N4 C29 C28 118.4(6) . . ? C30 C29 C28 117.8(6) . . ? C31 C30 C29 127.6(6) . . ? N5 C31 C30 124.3(6) . . ? N5 C31 C32 117.7(6) . . ? C30 C31 C32 118.0(6) . . ? C38 C33 C34 119.7(6) . . ? C38 C33 N4 121.1(6) . . ? C34 C33 N4 119.1(6) . . ? C35 C34 C33 119.5(8) . . ? C34 C35 C36 120.3(7) . . ? C37 C36 C35 120.3(7) . . ? C36 C37 C38 119.1(8) . . ? C33 C38 C37 121.0(7) . . ? C44 C39 C40 119.5(7) . . ? C44 C39 N5 122.1(7) . . ? C40 C39 N5 118.3(6) . . ? C39 C40 C41 119.6(7) . . ? C42 C41 C40 119.8(8) . . ? C41 C42 C43 121.0(8) . . ? C42 C43 C44 119.8(7) . . ? C39 C44 C43 120.2(8) . . ? C46 C45 C50 117.2(6) . . ? C46 C45 N6 121.5(6) . . ? C50 C45 N6 121.3(6) . . ? C45 C46 C47 120.5(6) . . ? C48 C47 C46 122.2(6) . . ? C47 C48 C49 116.7(6) . . ? C47 C48 C51 122.1(6) . . ? C49 C48 C51 121.2(6) . . ? C50 C49 C48 121.7(6) . . ? C49 C50 C45 121.7(6) . . ? C48 C51 C54 108.5(6) . . ? C48 C51 C53 114.3(6) . . ? C54 C51 C53 108.3(6) . . ? C48 C51 C52 108.2(6) . . ? C54 C51 C52 109.6(7) . . ? C53 C51 C52 107.9(7) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.176 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.128 #===END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 680461' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H54 Cl N5 Pd2' _chemical_formula_weight 973.23 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5418(4) _cell_length_b 13.5019(4) _cell_length_c 15.5413(5) _cell_angle_alpha 106.2391(18) _cell_angle_beta 105.9472(18) _cell_angle_gamma 97.1865(16) _cell_volume 2370.66(13) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23738 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23738 _diffrn_reflns_av_R_equivalents 0.0792 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9277 _reflns_number_gt 6665 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0990P)^2^+0.0037P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9277 _refine_ls_number_parameters 536 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1756 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.002 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 1.21251(3) 0.44827(3) 0.88796(3) 0.0518(7) Uani 1 1 d . . . Pd2 Pd 1.01174(3) 0.52580(3) 0.77573(3) 0.0546(7) Uani 1 1 d . . . Cl1 Cl 1.09585(15) 0.38462(13) 0.73064(12) 0.0780(8) Uani 1 1 d . . . N1 N 1.3107(4) 0.5105(3) 1.0240(3) 0.0518(11) Uani 1 1 d . . . N2 N 1.2508(4) 0.3053(3) 0.8810(3) 0.0540(12) Uani 1 1 d . . . N3 N 0.9393(4) 0.6439(3) 0.8265(3) 0.0575(12) Uani 1 1 d . . . N4 N 0.8645(4) 0.4490(4) 0.6727(3) 0.0655(13) Uani 1 1 d . . . N5 N 1.1699(4) 0.5894(3) 0.8791(3) 0.0534(11) Uani 1 1 d . . . H1 H 1.148(4) 0.618(3) 0.931(3) 0.036(11) Uiso 1 1 d . . . C1 C 1.4826(5) 0.5345(5) 1.1599(4) 0.0660(15) Uani 1 1 d . . . H1A H 1.4435 0.5709 1.1997 0.099 Uiso 1 1 calc R . . H1B H 1.5388 0.5849 1.1539 0.099 Uiso 1 1 calc R . . H1C H 1.5190 0.4871 1.1876 0.099 Uiso 1 1 calc R . . C1S C 0.8269(11) 0.7370(11) 0.5666(8) 0.149(4) Uani 1 1 d . . . H1SA H 0.8925 0.7854 0.6088 0.179 Uiso 1 1 calc R . . C2 C 1.3985(4) 0.4723(4) 1.0632(4) 0.0558(13) Uani 1 1 d . . . C2S C 0.7513(10) 0.7036(10) 0.5979(8) 0.134(4) Uani 1 1 d . . . H2SA H 0.7613 0.7294 0.6624 0.161 Uiso 1 1 calc R . . C3 C 1.4170(4) 0.3718(4) 1.0180(4) 0.0520(13) Uani 1 1 d . . . H3A H 1.4874 0.3584 1.0446 0.062 Uiso 1 1 calc R . . C3S C 0.6541(9) 0.6291(9) 0.5373(9) 0.129(3) Uani 1 1 d . . . H3SA H 0.5961 0.6079 0.5592 0.155 Uiso 1 1 calc R . . C4 C 1.3437(5) 0.2926(4) 0.9402(4) 0.0577(14) Uani 1 1 d . . . C4S C 0.6461(10) 0.5873(9) 0.4431(8) 0.129(3) Uani 1 1 d . . . H4SA H 0.5889 0.5287 0.4030 0.155 Uiso 1 1 calc R . . C5 C 1.3707(5) 0.1855(4) 0.9228(5) 0.0713(16) Uani 1 1 d . . . H5A H 1.3087 0.1362 0.9231 0.107 Uiso 1 1 calc R . . H5B H 1.4385 0.1886 0.9717 0.107 Uiso 1 1 calc R . . H5C H 1.3822 0.1630 0.8623 0.107 Uiso 1 1 calc R . . C5S C 0.7178(10) 0.6295(8) 0.4107(8) 0.128(3) Uani 1 1 d . . . H5SA H 0.7041 0.6098 0.3457 0.154 Uiso 1 1 calc R . . C6 C 1.2838(5) 0.6014(4) 1.0798(4) 0.0558(13) Uani 1 1 d . . . C6S C 0.8138(10) 0.7029(10) 0.4711(7) 0.137(4) Uani 1 1 d . . . H6SA H 0.8687 0.7292 0.4484 0.165 Uiso 1 1 calc R . . C7 C 1.3559(5) 0.7003(4) 1.1131(4) 0.0633(15) Uani 1 1 d . . . H7A H 1.4220 0.7092 1.0973 0.076 Uiso 1 1 calc R . . C8 C 1.3285(6) 0.7871(5) 1.1710(5) 0.0776(18) Uani 1 1 d . . . H8A H 1.3775 0.8532 1.1946 0.093 Uiso 1 1 calc R . . C9 C 1.2299(6) 0.7745(5) 1.1928(4) 0.0747(18) Uani 1 1 d . . . H9A H 1.2125 0.8320 1.2314 0.090 Uiso 1 1 calc R . . C10 C 1.1560(6) 0.6761(5) 1.1572(4) 0.0696(16) Uani 1 1 d . . . H10A H 1.0884 0.6681 1.1710 0.083 Uiso 1 1 calc R . . C11 C 1.1831(5) 0.5896(4) 1.1010(4) 0.0576(14) Uani 1 1 d . . . H11A H 1.1337 0.5237 1.0775 0.069 Uiso 1 1 calc R . . C12 C 1.1793(5) 0.2163(4) 0.8041(4) 0.0605(14) Uani 1 1 d . . . C13 C 1.2047(6) 0.1784(5) 0.7213(5) 0.0782(18) Uani 1 1 d . . . H13A H 1.2714 0.2111 0.7163 0.094 Uiso 1 1 calc R . . C14 C 1.1339(7) 0.0939(5) 0.6466(5) 0.087(2) Uani 1 1 d . . . H14A H 1.1532 0.0698 0.5919 0.104 Uiso 1 1 calc R . . C15 C 1.0344(7) 0.0444(5) 0.6519(5) 0.0828(19) Uani 1 1 d . . . H15A H 0.9868 -0.0133 0.6013 0.099 Uiso 1 1 calc R . . C16 C 1.0056(5) 0.0809(4) 0.7328(4) 0.0717(16) Uani 1 1 d . . . H16A H 0.9380 0.0482 0.7366 0.086 Uiso 1 1 calc R . . C17 C 1.0770(5) 0.1662(4) 0.8083(4) 0.0639(15) Uani 1 1 d . . . H17A H 1.0569 0.1905 0.8625 0.077 Uiso 1 1 calc R . . C18 C 0.7847(6) 0.7206(5) 0.8668(5) 0.0787(18) Uani 1 1 d . . . H18A H 0.8188 0.7351 0.9337 0.118 Uiso 1 1 calc R . . H18B H 0.7036 0.6999 0.8498 0.118 Uiso 1 1 calc R . . H18C H 0.8039 0.7830 0.8512 0.118 Uiso 1 1 calc R . . C19 C 0.8284(5) 0.6324(5) 0.8132(4) 0.0644(15) Uani 1 1 d . . . C20 C 0.7479(5) 0.5440(5) 0.7501(5) 0.0742(17) Uani 1 1 d . . . H20A H 0.6755 0.5380 0.7555 0.089 Uiso 1 1 calc R . . C21 C 0.7628(5) 0.4617(5) 0.6783(5) 0.0738(17) Uani 1 1 d . . . C22 C 0.6547(6) 0.3877(6) 0.6040(6) 0.100(2) Uani 1 1 d . . . H22A H 0.6609 0.3157 0.5955 0.151 Uiso 1 1 calc R . . H22B H 0.6445 0.4009 0.5450 0.151 Uiso 1 1 calc R . . H22C H 0.5907 0.3999 0.6247 0.151 Uiso 1 1 calc R . . C23 C 1.0102(5) 0.7483(4) 0.8759(4) 0.0565(13) Uani 1 1 d . . . C24 C 1.0462(5) 0.7910(5) 0.9738(4) 0.0657(15) Uani 1 1 d . . . H24A H 1.0292 0.7501 1.0095 0.079 Uiso 1 1 calc R . . C25 C 1.1077(6) 0.8948(5) 1.0189(5) 0.0742(17) Uani 1 1 d . . . H25A H 1.1317 0.9229 1.0847 0.089 Uiso 1 1 calc R . . C26 C 1.1330(6) 0.9555(5) 0.9676(5) 0.0779(18) Uani 1 1 d . . . H26A H 1.1713 1.0258 0.9980 0.093 Uiso 1 1 calc R . . C27 C 1.1019(5) 0.9127(4) 0.8706(5) 0.0721(17) Uani 1 1 d . . . H27A H 1.1226 0.9536 0.8361 0.087 Uiso 1 1 calc R . . C28 C 1.0405(5) 0.8103(4) 0.8238(4) 0.0628(14) Uani 1 1 d . . . H28A H 1.0194 0.7824 0.7581 0.075 Uiso 1 1 calc R . . C29 C 0.8694(5) 0.3749(5) 0.5889(4) 0.0695(16) Uani 1 1 d . . . C30 C 0.8611(6) 0.2692(5) 0.5787(5) 0.0802(18) Uani 1 1 d . . . H30A H 0.8521 0.2450 0.6273 0.096 Uiso 1 1 calc R . . C31 C 0.8663(7) 0.1979(6) 0.4956(5) 0.089(2) Uani 1 1 d . . . H31A H 0.8589 0.1265 0.4890 0.106 Uiso 1 1 calc R . . C32 C 0.8818(6) 0.2317(6) 0.4252(5) 0.091(2) Uani 1 1 d . . . H32A H 0.8847 0.1838 0.3702 0.110 Uiso 1 1 calc R . . C33 C 0.8933(6) 0.3377(6) 0.4353(5) 0.087(2) Uani 1 1 d . . . H33A H 0.9048 0.3613 0.3871 0.105 Uiso 1 1 calc R . . C34 C 0.8878(6) 0.4092(5) 0.5167(4) 0.0761(17) Uani 1 1 d . . . H34A H 0.8965 0.4806 0.5231 0.091 Uiso 1 1 calc R . . C35 C 1.2474(4) 0.6542(4) 0.8545(4) 0.0556(13) Uani 1 1 d . . . C36 C 1.2776(5) 0.6149(4) 0.7742(4) 0.0592(14) Uani 1 1 d . . . H36A H 1.2483 0.5445 0.7365 0.071 Uiso 1 1 calc R . . C37 C 1.3507(5) 0.6787(4) 0.7489(4) 0.0605(14) Uani 1 1 d . . . H37A H 1.3698 0.6497 0.6949 0.073 Uiso 1 1 calc R . . C38 C 1.3962(4) 0.7850(4) 0.8021(4) 0.0576(13) Uani 1 1 d . . . C39 C 1.3654(5) 0.8226(4) 0.8826(4) 0.0603(14) Uani 1 1 d . . . H39A H 1.3943 0.8931 0.9199 0.072 Uiso 1 1 calc R . . C40 C 1.2943(5) 0.7608(4) 0.9098(4) 0.0582(14) Uani 1 1 d . . . H40A H 1.2771 0.7896 0.9648 0.070 Uiso 1 1 calc R . . C41 C 1.4716(5) 0.8580(4) 0.7732(4) 0.0645(15) Uani 1 1 d . . . C42 C 1.5069(8) 0.7962(6) 0.6893(6) 0.100(2) Uani 1 1 d . . . H42A H 1.5450 0.7436 0.7062 0.150 Uiso 1 1 calc R . . H42B H 1.5570 0.8441 0.6750 0.150 Uiso 1 1 calc R . . H42C H 1.4404 0.7624 0.6348 0.150 Uiso 1 1 calc R . . C43 C 1.4044(6) 0.9379(5) 0.7413(5) 0.087(2) Uani 1 1 d . . . H43A H 1.3845 0.9795 0.7932 0.130 Uiso 1 1 calc R . . H43B H 1.3365 0.9000 0.6893 0.130 Uiso 1 1 calc R . . H43C H 1.4508 0.9835 0.7217 0.130 Uiso 1 1 calc R . . C44 C 1.5794(6) 0.9181(5) 0.8552(5) 0.0802(18) Uani 1 1 d . . . H44A H 1.5601 0.9638 0.9055 0.120 Uiso 1 1 calc R . . H44B H 1.6281 0.9596 0.8341 0.120 Uiso 1 1 calc R . . H44C H 1.6182 0.8688 0.8779 0.120 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 0.0487(7) 0.0509(7) 0.0535(7) 0.0155(3) 0.0143(3) 0.0122(2) Pd2 0.0498(7) 0.0537(7) 0.0584(7) 0.0195(3) 0.0135(3) 0.0112(2) Cl1 0.0779(12) 0.0759(11) 0.0742(12) 0.0230(8) 0.0148(8) 0.0220(8) N1 0.050(2) 0.053(2) 0.051(2) 0.0147(18) 0.0162(19) 0.0117(18) N2 0.055(3) 0.049(2) 0.056(2) 0.0156(18) 0.017(2) 0.0117(18) N3 0.054(3) 0.061(2) 0.062(3) 0.027(2) 0.018(2) 0.017(2) N4 0.054(3) 0.066(3) 0.067(3) 0.022(2) 0.009(2) 0.004(2) N5 0.048(2) 0.054(2) 0.056(3) 0.0175(19) 0.015(2) 0.0113(18) C1 0.056(3) 0.075(3) 0.064(3) 0.022(3) 0.015(3) 0.017(3) C1S 0.140(10) 0.213(12) 0.100(7) 0.076(8) 0.030(7) 0.022(9) C2 0.046(3) 0.069(3) 0.057(3) 0.027(2) 0.017(2) 0.014(2) C2S 0.099(7) 0.192(11) 0.117(8) 0.067(8) 0.028(6) 0.033(7) C3 0.036(2) 0.055(3) 0.069(3) 0.023(2) 0.017(2) 0.015(2) C3S 0.099(7) 0.153(9) 0.154(10) 0.061(8) 0.055(7) 0.034(7) C4 0.056(3) 0.056(3) 0.070(3) 0.025(3) 0.028(3) 0.016(2) C4S 0.120(8) 0.127(7) 0.125(8) 0.009(6) 0.051(7) 0.024(6) C5 0.062(4) 0.060(3) 0.090(4) 0.025(3) 0.022(3) 0.013(3) C5S 0.116(8) 0.133(8) 0.115(7) 0.010(6) 0.045(7) 0.005(6) C6 0.058(3) 0.060(3) 0.048(3) 0.017(2) 0.016(2) 0.015(2) C6S 0.128(9) 0.181(10) 0.103(7) 0.051(7) 0.043(6) 0.016(8) C7 0.059(3) 0.056(3) 0.067(3) 0.014(2) 0.018(3) 0.006(2) C8 0.092(5) 0.057(3) 0.074(4) 0.015(3) 0.023(4) 0.008(3) C9 0.099(5) 0.074(4) 0.060(3) 0.023(3) 0.030(3) 0.038(4) C10 0.083(4) 0.075(4) 0.074(4) 0.037(3) 0.040(3) 0.037(3) C11 0.059(3) 0.059(3) 0.059(3) 0.025(2) 0.019(2) 0.015(2) C12 0.068(4) 0.054(3) 0.061(3) 0.020(2) 0.020(3) 0.018(2) C13 0.089(5) 0.065(3) 0.077(4) 0.012(3) 0.036(4) 0.008(3) C14 0.116(6) 0.070(4) 0.066(4) 0.007(3) 0.036(4) 0.015(4) C15 0.100(5) 0.061(3) 0.067(4) 0.010(3) 0.009(4) 0.013(3) C16 0.063(4) 0.059(3) 0.081(4) 0.017(3) 0.011(3) 0.011(3) C17 0.063(3) 0.057(3) 0.073(4) 0.019(3) 0.025(3) 0.019(3) C18 0.061(4) 0.089(4) 0.099(5) 0.042(4) 0.031(3) 0.027(3) C19 0.054(3) 0.074(3) 0.080(4) 0.039(3) 0.027(3) 0.021(3) C20 0.051(3) 0.088(4) 0.091(4) 0.041(4) 0.022(3) 0.016(3) C21 0.054(3) 0.074(4) 0.085(4) 0.031(3) 0.010(3) 0.001(3) C22 0.062(4) 0.102(5) 0.114(6) 0.028(5) 0.009(4) 0.001(4) C23 0.054(3) 0.057(3) 0.061(3) 0.019(2) 0.020(2) 0.023(2) C24 0.066(4) 0.072(3) 0.070(4) 0.026(3) 0.028(3) 0.030(3) C25 0.074(4) 0.074(4) 0.066(4) 0.009(3) 0.020(3) 0.026(3) C26 0.071(4) 0.055(3) 0.094(5) 0.013(3) 0.017(3) 0.015(3) C27 0.064(4) 0.058(3) 0.094(5) 0.030(3) 0.018(3) 0.017(3) C28 0.060(3) 0.066(3) 0.064(3) 0.027(3) 0.018(3) 0.014(3) C29 0.055(3) 0.075(4) 0.065(4) 0.021(3) 0.007(3) 0.001(3) C30 0.086(5) 0.076(4) 0.066(4) 0.016(3) 0.021(3) -0.001(3) C31 0.093(5) 0.074(4) 0.077(4) 0.013(3) 0.016(4) -0.003(4) C32 0.082(5) 0.104(5) 0.062(4) 0.012(4) 0.007(3) -0.002(4) C33 0.071(4) 0.116(6) 0.063(4) 0.034(4) 0.007(3) 0.004(4) C34 0.069(4) 0.082(4) 0.067(4) 0.029(3) 0.007(3) 0.002(3) C35 0.049(3) 0.058(3) 0.058(3) 0.017(2) 0.016(2) 0.016(2) C36 0.061(3) 0.051(3) 0.062(3) 0.014(2) 0.016(3) 0.015(2) C37 0.070(4) 0.055(3) 0.054(3) 0.012(2) 0.023(3) 0.014(2) C38 0.050(3) 0.060(3) 0.062(3) 0.021(2) 0.015(2) 0.016(2) C39 0.054(3) 0.050(3) 0.072(3) 0.012(2) 0.019(3) 0.012(2) C40 0.056(3) 0.056(3) 0.060(3) 0.014(2) 0.019(2) 0.015(2) C41 0.062(3) 0.056(3) 0.071(4) 0.017(3) 0.020(3) 0.009(2) C42 0.118(6) 0.083(4) 0.100(5) 0.014(4) 0.064(5) -0.001(4) C43 0.083(5) 0.067(4) 0.107(5) 0.042(4) 0.019(4) 0.005(3) C44 0.066(4) 0.083(4) 0.089(5) 0.033(4) 0.020(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.002(4) . ? Pd1 N2 2.028(4) . ? Pd1 N5 2.072(4) . ? Pd1 Cl1 2.3241(17) . ? Pd1 Pd2 3.1218(5) . ? Pd2 N4 2.004(5) . ? Pd2 N3 2.011(4) . ? Pd2 N5 2.075(4) . ? Pd2 Cl1 2.3237(16) . ? N1 C2 1.341(6) . ? N1 C6 1.428(6) . ? N2 C4 1.334(7) . ? N2 C12 1.419(7) . ? N3 C19 1.330(7) . ? N3 C23 1.440(7) . ? N4 C21 1.331(8) . ? N4 C29 1.424(8) . ? N5 C35 1.426(6) . ? C1 C2 1.509(8) . ? C1S C2S 1.268(14) . ? C1S C6S 1.381(14) . ? C2 C3 1.423(7) . ? C2S C3S 1.384(15) . ? C3 C4 1.368(8) . ? C3S C4S 1.385(14) . ? C4 C5 1.495(7) . ? C4S C5S 1.291(13) . ? C5S C6S 1.368(14) . ? C6 C7 1.387(7) . ? C6 C11 1.392(7) . ? C7 C8 1.408(8) . ? C8 C9 1.373(9) . ? C9 C10 1.389(9) . ? C10 C11 1.391(8) . ? C12 C13 1.385(8) . ? C12 C17 1.400(8) . ? C13 C14 1.371(9) . ? C14 C15 1.374(10) . ? C15 C16 1.379(9) . ? C16 C17 1.383(8) . ? C18 C19 1.508(8) . ? C19 C20 1.381(9) . ? C20 C21 1.409(9) . ? C21 C22 1.525(9) . ? C23 C24 1.386(8) . ? C23 C28 1.403(7) . ? C24 C25 1.390(9) . ? C25 C26 1.361(9) . ? C26 C27 1.375(9) . ? C27 C28 1.378(8) . ? C29 C30 1.379(9) . ? C29 C34 1.390(8) . ? C30 C31 1.401(9) . ? C31 C32 1.348(10) . ? C32 C33 1.380(10) . ? C33 C34 1.385(10) . ? C35 C36 1.387(7) . ? C35 C40 1.406(7) . ? C36 C37 1.388(7) . ? C37 C38 1.394(7) . ? C38 C39 1.389(7) . ? C38 C41 1.522(7) . ? C39 C40 1.373(7) . ? C41 C44 1.521(9) . ? C41 C42 1.546(9) . ? C41 C43 1.554(8) . ? 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 Pd1 N2 91.25(16) . . ? N1 Pd1 N5 94.48(17) . . ? N2 Pd1 N5 173.66(17) . . ? N1 Pd1 Cl1 176.96(12) . . ? N2 Pd1 Cl1 91.78(13) . . ? N5 Pd1 Cl1 82.50(13) . . ? N1 Pd1 Pd2 129.33(11) . . ? N2 Pd1 Pd2 134.87(13) . . ? N5 Pd1 Pd2 41.19(12) . . ? Cl1 Pd1 Pd2 47.80(4) . . ? N4 Pd2 N3 90.64(19) . . ? N4 Pd2 N5 173.58(17) . . ? N3 Pd2 N5 95.51(18) . . ? N4 Pd2 Cl1 91.24(15) . . ? N3 Pd2 Cl1 174.17(12) . . ? N5 Pd2 Cl1 82.46(13) . . ? N4 Pd2 Pd1 132.69(13) . . ? N3 Pd2 Pd1 127.93(13) . . ? N5 Pd2 Pd1 41.14(11) . . ? Cl1 Pd2 Pd1 47.81(4) . . ? Pd2 Cl1 Pd1 84.39(6) . . ? C2 N1 C6 119.9(4) . . ? C2 N1 Pd1 123.8(3) . . ? C6 N1 Pd1 116.3(3) . . ? C4 N2 C12 119.1(4) . . ? C4 N2 Pd1 123.3(3) . . ? C12 N2 Pd1 117.4(3) . . ? C19 N3 C23 117.8(4) . . ? C19 N3 Pd2 123.8(4) . . ? C23 N3 Pd2 118.3(3) . . ? C21 N4 C29 118.2(5) . . ? C21 N4 Pd2 124.1(4) . . ? C29 N4 Pd2 117.7(4) . . ? C35 N5 Pd1 114.9(3) . . ? C35 N5 Pd2 114.4(3) . . ? Pd1 N5 Pd2 97.67(17) . . ? C2S C1S C6S 121.4(13) . . ? N1 C2 C3 122.7(5) . . ? N1 C2 C1 120.9(5) . . ? C3 C2 C1 116.3(4) . . ? C1S C2S C3S 120.8(12) . . ? C4 C3 C2 127.8(5) . . ? C2S C3S C4S 117.8(10) . . ? N2 C4 C3 124.3(4) . . ? N2 C4 C5 119.1(5) . . ? C3 C4 C5 116.6(5) . . ? C5S C4S C3S 120.1(11) . . ? C4S C5S C6S 120.8(11) . . ? C7 C6 C11 119.7(5) . . ? C7 C6 N1 121.4(5) . . ? C11 C6 N1 118.9(5) . . ? C5S C6S C1S 118.1(11) . . ? C6 C7 C8 119.6(5) . . ? C9 C8 C7 120.3(6) . . ? C8 C9 C10 120.2(5) . . ? C9 C10 C11 119.9(6) . . ? C10 C11 C6 120.3(5) . . ? C13 C12 C17 117.5(5) . . ? C13 C12 N2 122.0(5) . . ? C17 C12 N2 120.5(5) . . ? C14 C13 C12 121.6(6) . . ? C13 C14 C15 120.4(6) . . ? C14 C15 C16 119.6(6) . . ? C15 C16 C17 120.1(6) . . ? C16 C17 C12 120.8(5) . . ? N3 C19 C20 123.7(5) . . ? N3 C19 C18 119.7(6) . . ? C20 C19 C18 116.5(5) . . ? C19 C20 C21 127.4(5) . . ? N4 C21 C20 123.0(6) . . ? N4 C21 C22 120.6(6) . . ? C20 C21 C22 116.3(6) . . ? C24 C23 C28 118.8(5) . . ? C24 C23 N3 121.7(5) . . ? C28 C23 N3 119.5(5) . . ? C23 C24 C25 120.2(5) . . ? C26 C25 C24 120.5(6) . . ? C25 C26 C27 119.9(6) . . ? C26 C27 C28 121.0(6) . . ? C27 C28 C23 119.5(6) . . ? C30 C29 C34 118.3(6) . . ? C30 C29 N4 121.5(5) . . ? C34 C29 N4 120.1(6) . . ? C29 C30 C31 120.4(6) . . ? C32 C31 C30 120.7(7) . . ? C31 C32 C33 119.6(7) . . ? C32 C33 C34 120.5(6) . . ? C33 C34 C29 120.4(6) . . ? C36 C35 C40 117.5(5) . . ? C36 C35 N5 121.2(5) . . ? C40 C35 N5 121.3(4) . . ? C35 C36 C37 121.3(5) . . ? C36 C37 C38 121.8(5) . . ? C39 C38 C37 115.9(5) . . ? C39 C38 C41 121.2(5) . . ? C37 C38 C41 122.8(5) . . ? C40 C39 C38 123.4(5) . . ? C39 C40 C35 120.1(5) . . ? C44 C41 C38 111.0(5) . . ? C44 C41 C42 107.9(6) . . ? C38 C41 C42 111.8(5) . . ? C44 C41 C43 109.4(5) . . ? C38 C41 C43 108.8(5) . . ? C42 C41 C43 107.9(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.064 _refine_diff_density_min -0.039 _refine_diff_density_rms 0.005 _vrf_PLAT601_compound4 ; RESPONSE: caused by diffused water molecules. SWAT command was used. ;