# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_6MPdCl _database_code_depnum_ccdc_archive 'CCDC 784539' #TrackingRef '6MPdCl.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H37 Cl N2 Pd, 0.5(C H2 Cl2)' _chemical_formula_sum 'C31.50 H38 Cl2 N2 Pd' _chemical_formula_weight 621.94 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.6985(17) _cell_length_b 16.7201(13) _cell_length_c 17.7371(14) _cell_angle_alpha 90.00 _cell_angle_beta 112.570(2) _cell_angle_gamma 90.00 _cell_volume 5942.2(8) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 999 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2568 _exptl_absorpt_coefficient_mu 0.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.820 _exptl_absorpt_correction_T_max 0.883 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998a)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 SMART 1K CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 59982 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.00 _reflns_number_total 14317 _reflns_number_gt 11534 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Bruker, 1998b)' _computing_cell_refinement 'SAINTPlus (Bruker, 1998a)' _computing_data_reduction 'SAINTPlus (Bruker, 1998a)' _computing_structure_solution 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_structure_refinement 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_molecular_graphics 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _computing_publication_material 'SHELXTL ver. 5.1 (Sheldrick, 1998b)' _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^)+(0.0911P)^2^+15.8664P] 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 14317 _refine_ls_number_parameters 679 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.002 _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 0.560243(13) 0.675225(15) 0.663012(15) 0.02141(8) Uani 1 1 d . . . Pd2 Pd 0.877663(13) 0.954956(15) 0.675877(16) 0.02377(8) Uani 1 1 d . . . Cl1 Cl 0.48747(4) 0.57835(4) 0.68436(5) 0.02341(16) Uani 1 1 d . . . Cl2 Cl 0.95442(4) 0.87588(5) 0.64029(5) 0.02451(17) Uani 1 1 d . . . N1 N 0.50188(16) 0.81626(18) 0.71899(18) 0.0273(6) Uani 1 1 d . . . N2 N 0.58525(15) 0.74908(18) 0.82070(18) 0.0260(6) Uani 1 1 d . . . N3 N 0.95329(15) 1.11245(18) 0.70833(18) 0.0256(6) Uani 1 1 d . . . N4 N 0.97640(16) 1.03128(18) 0.81986(19) 0.0278(6) Uani 1 1 d . . . C1 C 0.54703(17) 0.7566(2) 0.7410(2) 0.0230(6) Uani 1 1 d . A . C2 C 0.4913(2) 0.8748(3) 0.7748(2) 0.0415(10) Uani 0.60 1 d PD A 1 H2A H 0.4433 0.8886 0.7558 0.050 Uiso 0.60 1 calc PR A 1 H2B H 0.5166 0.9243 0.7760 0.050 Uiso 0.60 1 calc PR A 1 C3 C 0.5145(3) 0.8388(4) 0.8588(3) 0.0394(16) Uani 0.60 1 d PD A 1 H3A H 0.4829 0.7964 0.8595 0.047 Uiso 0.60 1 calc PR A 1 H3B H 0.5145 0.8806 0.8983 0.047 Uiso 0.60 1 calc PR A 1 C4 C 0.5836(2) 0.8036(3) 0.8850(2) 0.0397(10) Uani 0.60 1 d PD A 1 H4A H 0.6168 0.8469 0.8938 0.048 Uiso 0.60 1 calc PR A 1 H4B H 0.5947 0.7741 0.9369 0.048 Uiso 0.60 1 calc PR A 1 C2A C 0.4913(2) 0.8748(3) 0.7748(2) 0.0415(10) Uani 0.40 1 d PD A 2 H2C H 0.4515 0.8593 0.7860 0.050 Uiso 0.40 1 calc PR A 2 H2D H 0.4828 0.9282 0.7487 0.050 Uiso 0.40 1 calc PR A 2 C3A C 0.5514(4) 0.8789(7) 0.8541(4) 0.041(2) Uani 0.40 1 d PD A 2 H3C H 0.5846 0.9152 0.8464 0.050 Uiso 0.40 1 calc PR A 2 H3D H 0.5375 0.9032 0.8960 0.050 Uiso 0.40 1 calc PR A 2 C4A C 0.5836(2) 0.8036(3) 0.8850(2) 0.0397(10) Uani 0.40 1 d PD A 2 H4C H 0.5598 0.7770 0.9159 0.048 Uiso 0.40 1 calc PR A 2 H4D H 0.6299 0.8141 0.9235 0.048 Uiso 0.40 1 calc PR A 2 C5 C 0.46492(19) 0.8315(2) 0.6336(2) 0.0272(7) Uani 1 1 d . A . C6 C 0.40054(19) 0.7986(2) 0.5954(2) 0.0297(7) Uani 1 1 d . . . C7 C 0.36615(19) 0.8147(2) 0.5123(2) 0.0304(8) Uani 1 1 d . A . H7A H 0.3226 0.7933 0.4852 0.036 Uiso 1 1 calc R . . C8 C 0.39351(19) 0.8607(2) 0.4683(2) 0.0309(8) Uani 1 1 d . . . C9 C 0.45615(19) 0.8954(2) 0.5100(2) 0.0308(8) Uani 1 1 d . A . H9A H 0.4746 0.9289 0.4808 0.037 Uiso 1 1 calc R . . C10 C 0.49205(18) 0.8824(2) 0.5923(2) 0.0294(7) Uani 1 1 d . . . C11 C 0.3698(2) 0.7487(3) 0.6419(3) 0.0375(9) Uani 1 1 d . A . H11A H 0.3995 0.7040 0.6679 0.056 Uiso 1 1 calc R . . H11B H 0.3267 0.7280 0.6044 0.056 Uiso 1 1 calc R . . H11C H 0.3631 0.7816 0.6839 0.056 Uiso 1 1 calc R . . C12 C 0.3575(2) 0.8738(3) 0.3776(3) 0.0410(10) Uani 1 1 d . A . H12A H 0.3179 0.8395 0.3570 0.062 Uiso 1 1 calc R . . H12B H 0.3874 0.8604 0.3497 0.062 Uiso 1 1 calc R . . H12C H 0.3440 0.9299 0.3673 0.062 Uiso 1 1 calc R . . C13 C 0.5580(2) 0.9237(2) 0.6351(3) 0.0369(9) Uani 1 1 d . A . H13A H 0.5872 0.8894 0.6791 0.055 Uiso 1 1 calc R . . H13B H 0.5507 0.9744 0.6581 0.055 Uiso 1 1 calc R . . H13C H 0.5789 0.9341 0.5960 0.055 Uiso 1 1 calc R . . C14 C 0.63573(18) 0.6872(2) 0.8463(2) 0.0257(7) Uani 1 1 d . A . C15 C 0.69654(18) 0.6995(2) 0.8391(2) 0.0293(7) Uani 1 1 d . . . C16 C 0.7434(2) 0.6381(3) 0.8631(3) 0.0413(10) Uani 1 1 d . A . H16A H 0.7849 0.6455 0.8578 0.050 Uiso 1 1 calc R . . C17 C 0.7315(2) 0.5666(3) 0.8945(2) 0.0414(10) Uani 1 1 d . . . C18 C 0.6722(2) 0.5579(3) 0.9038(2) 0.0386(9) Uani 1 1 d . A . H18A H 0.6640 0.5098 0.9269 0.046 Uiso 1 1 calc R . . C19 C 0.6234(2) 0.6172(2) 0.8806(2) 0.0315(8) Uani 1 1 d . . . C20 C 0.7142(2) 0.7785(3) 0.8105(3) 0.0412(10) Uani 1 1 d . A . H20A H 0.7557 0.7992 0.8520 0.062 Uiso 1 1 calc R . . H20B H 0.6781 0.8170 0.8020 0.062 Uiso 1 1 calc R . . H20C H 0.7204 0.7705 0.7591 0.062 Uiso 1 1 calc R . . C21 C 0.7854(3) 0.5020(4) 0.9213(3) 0.0674(18) Uani 1 1 d . A . H21A H 0.8037 0.4950 0.8792 0.101 Uiso 1 1 calc R . . H21B H 0.7658 0.4514 0.9293 0.101 Uiso 1 1 calc R . . H21C H 0.8211 0.5180 0.9727 0.101 Uiso 1 1 calc R . . C22 C 0.5595(2) 0.6062(3) 0.8943(3) 0.0439(10) Uani 1 1 d . A . H22A H 0.5214 0.6110 0.8421 0.066 Uiso 1 1 calc R . . H22B H 0.5564 0.6473 0.9320 0.066 Uiso 1 1 calc R . . H22C H 0.5592 0.5531 0.9176 0.066 Uiso 1 1 calc R . . C23 C 0.6099(2) 0.7432(2) 0.6024(3) 0.0343(8) Uani 1 1 d . . . H23A H 0.5826 0.7605 0.5461 0.041 Uiso 1 1 calc R . . H23B H 0.6412 0.7848 0.6353 0.041 Uiso 1 1 calc R . . C24 C 0.6345(2) 0.6646(2) 0.6117(2) 0.0309(8) Uani 1 1 d . . . H24A H 0.6820 0.6538 0.6481 0.037 Uiso 1 1 calc R . . C25 C 0.59063(19) 0.6008(2) 0.5796(2) 0.0298(8) Uani 1 1 d . . . H25A H 0.5612 0.6087 0.5209 0.036 Uiso 1 1 calc R . . C26 C 0.61050(19) 0.5166(2) 0.5997(2) 0.0290(7) Uani 1 1 d . . . C27 C 0.6568(2) 0.4951(3) 0.6776(3) 0.0393(9) Uani 1 1 d . . . H27A H 0.6749 0.5345 0.7189 0.047 Uiso 1 1 calc R . . C28 C 0.6758(2) 0.4157(3) 0.6933(3) 0.0470(11) Uani 1 1 d . . . H28A H 0.7067 0.4011 0.7460 0.056 Uiso 1 1 calc R . . C29 C 0.6508(3) 0.3576(3) 0.6343(3) 0.0470(11) Uani 1 1 d . . . H29A H 0.6654 0.3038 0.6456 0.056 Uiso 1 1 calc R . . C30 C 0.6043(2) 0.3786(3) 0.5587(3) 0.0438(10) Uani 1 1 d . . . H30A H 0.5855 0.3387 0.5182 0.053 Uiso 1 1 calc R . . C31 C 0.5849(2) 0.4571(2) 0.5416(3) 0.0364(9) Uani 1 1 d . . . H31A H 0.5534 0.4708 0.4889 0.044 Uiso 1 1 calc R . . C32 C 0.94233(17) 1.0437(2) 0.7393(2) 0.0242(7) Uani 1 1 d . . . C33 C 0.9988(2) 1.1760(2) 0.7567(2) 0.0335(8) Uani 1 1 d . . . H33A H 0.9805 1.2290 0.7343 0.040 Uiso 1 1 calc R . . H33B H 1.0428 1.1701 0.7526 0.040 Uiso 1 1 calc R . . C34 C 1.0074(3) 1.1715(3) 0.8453(3) 0.0449(11) Uani 1 1 d . . . H34A H 1.0433 1.2084 0.8783 0.054 Uiso 1 1 calc R . . H34B H 0.9655 1.1879 0.8508 0.054 Uiso 1 1 calc R . . C35 C 1.0247(2) 1.0879(3) 0.8756(3) 0.0435(11) Uani 1 1 d . . . H35A H 1.0703 1.0748 0.8791 0.052 Uiso 1 1 calc R . . H35B H 1.0242 1.0830 0.9310 0.052 Uiso 1 1 calc R . . C36 C 0.92155(18) 1.1312(2) 0.6227(2) 0.0263(7) Uani 1 1 d . . . C37 C 0.86405(19) 1.1789(2) 0.5959(2) 0.0302(8) Uani 1 1 d . . . C38 C 0.8379(2) 1.2033(2) 0.5156(3) 0.0362(9) Uani 1 1 d . . . H38A H 0.7990 1.2357 0.4970 0.043 Uiso 1 1 calc R . . C39 C 0.8669(2) 1.1817(3) 0.4610(3) 0.0388(9) Uani 1 1 d . . . C40 C 0.9237(2) 1.1344(2) 0.4883(2) 0.0364(9) Uani 1 1 d . . . H40A H 0.9434 1.1191 0.4510 0.044 Uiso 1 1 calc R . . C41 C 0.9527(2) 1.1086(2) 0.5698(2) 0.0309(8) Uani 1 1 d . . . C42 C 0.8333(2) 1.2060(3) 0.6554(3) 0.0358(9) Uani 1 1 d . . . H42A H 0.7954 1.2414 0.6273 0.054 Uiso 1 1 calc R . . H42B H 0.8667 1.2349 0.7009 0.054 Uiso 1 1 calc R . . H42C H 0.8178 1.1592 0.6765 0.054 Uiso 1 1 calc R . . C43 C 0.8380(3) 1.2105(3) 0.3737(3) 0.0573(14) Uani 1 1 d . . . H43A H 0.7908 1.1956 0.3487 0.086 Uiso 1 1 calc R . . H43B H 0.8623 1.1857 0.3432 0.086 Uiso 1 1 calc R . . H43C H 0.8423 1.2688 0.3726 0.086 Uiso 1 1 calc R . . C44 C 1.0163(2) 1.0615(3) 0.5991(3) 0.0382(9) Uani 1 1 d . . . H44A H 1.0491 1.0874 0.6474 0.057 Uiso 1 1 calc R . . H44B H 1.0339 1.0591 0.5558 0.057 Uiso 1 1 calc R . . H44C H 1.0076 1.0071 0.6131 0.057 Uiso 1 1 calc R . . C45 C 0.96200(18) 0.9606(2) 0.8567(2) 0.0257(7) Uani 1 1 d . . . C46 C 1.00290(18) 0.8934(2) 0.8688(2) 0.0275(7) Uani 1 1 d . . . C47 C 0.9859(2) 0.8251(2) 0.9013(2) 0.0295(8) Uani 1 1 d . . . H47A H 1.0131 0.7788 0.9098 0.035 Uiso 1 1 calc R . . C48 C 0.9301(2) 0.8228(2) 0.9215(2) 0.0307(8) Uani 1 1 d . . . C49 C 0.8934(2) 0.8927(3) 0.9140(2) 0.0329(8) Uani 1 1 d . . . H49A H 0.8562 0.8924 0.9298 0.039 Uiso 1 1 calc R . . C50 C 0.9097(2) 0.9629(2) 0.8839(2) 0.0309(8) Uani 1 1 d . . . C51 C 1.0641(2) 0.8946(3) 0.8484(3) 0.0386(9) Uani 1 1 d . . . H51A H 1.0896 0.8452 0.8680 0.058 Uiso 1 1 calc R . . H51B H 1.0920 0.9407 0.8749 0.058 Uiso 1 1 calc R . . H51C H 1.0508 0.8987 0.7891 0.058 Uiso 1 1 calc R . . C52 C 0.9101(2) 0.7467(3) 0.9515(3) 0.0404(9) Uani 1 1 d . . . H52A H 0.9491 0.7232 0.9946 0.061 Uiso 1 1 calc R . . H52B H 0.8922 0.7088 0.9061 0.061 Uiso 1 1 calc R . . H52C H 0.8758 0.7585 0.9731 0.061 Uiso 1 1 calc R . . C53 C 0.8742(3) 1.0401(3) 0.8855(3) 0.0450(11) Uani 1 1 d . . . H53A H 0.8307 1.0282 0.8878 0.068 Uiso 1 1 calc R . . H53B H 0.8677 1.0710 0.8361 0.068 Uiso 1 1 calc R . . H53C H 0.9011 1.0712 0.9338 0.068 Uiso 1 1 calc R . . C54 C 0.7870(2) 1.0035(3) 0.6717(3) 0.0383(9) Uani 1 1 d . . . H54A H 0.7889 1.0348 0.7200 0.046 Uiso 1 1 calc R . . H54B H 0.7577 1.0276 0.6192 0.046 Uiso 1 1 calc R . . C55 C 0.78358(19) 0.9196(2) 0.6779(3) 0.0339(8) Uani 1 1 d . . . H55A H 0.7812 0.8947 0.7280 0.041 Uiso 1 1 calc R . . C56 C 0.79053(19) 0.8715(2) 0.6170(2) 0.0320(8) Uani 1 1 d . . . H56A H 0.7610 0.8897 0.5610 0.038 Uiso 1 1 calc R . . C57 C 0.79652(17) 0.7840(2) 0.6225(2) 0.0278(7) Uani 1 1 d . . . C58 C 0.82289(19) 0.7431(2) 0.6972(2) 0.0320(8) Uani 1 1 d . . . H58A H 0.8406 0.7723 0.7468 0.038 Uiso 1 1 calc R . . C59 C 0.8233(2) 0.6606(3) 0.6989(3) 0.0374(9) Uani 1 1 d . . . H59A H 0.8402 0.6338 0.7500 0.045 Uiso 1 1 calc R . . C60 C 0.7996(2) 0.6158(3) 0.6276(3) 0.0397(9) Uani 1 1 d . . . H60A H 0.7999 0.5590 0.6297 0.048 Uiso 1 1 calc R . . C61 C 0.7752(2) 0.6557(3) 0.5528(3) 0.0400(9) Uani 1 1 d . . . H61A H 0.7600 0.6263 0.5032 0.048 Uiso 1 1 calc R . . C62 C 0.7734(2) 0.7386(3) 0.5512(2) 0.0351(8) Uani 1 1 d . . . H62A H 0.7559 0.7652 0.5000 0.042 Uiso 1 1 calc R . . C63 C 0.67953(16) 0.0354(3) 0.9312(2) 0.0471(11) Uani 1 1 d D . . H63A H 0.6421 0.0739 0.9161 0.057 Uiso 1 1 calc R . . H63B H 0.6687 -0.0103 0.9595 0.057 Uiso 1 1 calc R . . Cl3 Cl 0.75357(6) 0.08222(8) 0.99797(8) 0.0522(3) Uani 1 1 d D . . Cl4 Cl 0.68886(8) 0.00091(12) 0.84177(10) 0.0784(5) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02441(14) 0.01958(13) 0.01856(13) -0.00102(9) 0.00638(10) 0.00110(9) Pd2 0.02448(14) 0.02134(14) 0.02251(14) -0.00147(9) 0.00571(10) -0.00194(9) Cl1 0.0230(4) 0.0154(3) 0.0289(4) -0.0008(3) 0.0067(3) -0.0059(3) Cl2 0.0298(4) 0.0148(3) 0.0352(4) -0.0093(3) 0.0195(3) -0.0005(3) N1 0.0299(15) 0.0243(15) 0.0240(15) -0.0033(11) 0.0062(12) 0.0036(12) N2 0.0295(15) 0.0240(14) 0.0217(14) -0.0030(11) 0.0069(12) 0.0003(12) N3 0.0270(14) 0.0219(14) 0.0249(14) -0.0029(11) 0.0067(12) -0.0037(11) N4 0.0301(16) 0.0240(14) 0.0247(14) -0.0024(12) 0.0054(12) -0.0029(12) C1 0.0235(15) 0.0215(15) 0.0229(15) 0.0008(12) 0.0076(13) -0.0022(12) C2 0.046(2) 0.036(2) 0.036(2) -0.0070(17) 0.0088(18) 0.0171(18) C3 0.038(4) 0.053(4) 0.029(3) -0.016(3) 0.014(3) 0.007(3) C4 0.047(2) 0.042(2) 0.0247(18) -0.0093(17) 0.0079(17) 0.0068(19) C2A 0.046(2) 0.036(2) 0.036(2) -0.0070(17) 0.0088(18) 0.0171(18) C3A 0.052(7) 0.037(6) 0.032(5) -0.010(4) 0.014(5) 0.007(5) C4A 0.047(2) 0.042(2) 0.0247(18) -0.0093(17) 0.0079(17) 0.0068(19) C5 0.0313(18) 0.0211(16) 0.0255(17) -0.0018(13) 0.0067(14) 0.0068(13) C6 0.0296(18) 0.0249(17) 0.0326(19) -0.0031(14) 0.0098(15) 0.0027(14) C7 0.0253(17) 0.0305(18) 0.0317(19) -0.0033(15) 0.0068(15) 0.0049(14) C8 0.0318(18) 0.0239(17) 0.0313(19) 0.0006(14) 0.0058(15) 0.0101(14) C9 0.0292(18) 0.0244(17) 0.0349(19) 0.0060(15) 0.0078(15) 0.0064(14) C10 0.0247(17) 0.0248(17) 0.0334(19) 0.0002(14) 0.0051(14) 0.0046(14) C11 0.033(2) 0.040(2) 0.038(2) 0.0014(17) 0.0125(17) 0.0001(17) C12 0.037(2) 0.043(2) 0.034(2) 0.0040(18) 0.0035(17) 0.0034(18) C13 0.038(2) 0.0273(19) 0.035(2) 0.0016(16) 0.0025(17) -0.0028(16) C14 0.0288(17) 0.0252(17) 0.0191(15) -0.0034(13) 0.0048(13) 0.0009(13) C15 0.0267(17) 0.0326(19) 0.0230(16) -0.0031(14) 0.0032(14) 0.0000(15) C16 0.030(2) 0.057(3) 0.032(2) -0.0106(19) 0.0053(16) 0.0073(19) C17 0.044(2) 0.043(2) 0.0234(18) -0.0023(16) -0.0019(17) 0.0155(19) C18 0.054(3) 0.0300(19) 0.0224(18) 0.0044(15) 0.0040(17) 0.0064(18) C19 0.043(2) 0.0294(18) 0.0198(16) -0.0001(14) 0.0092(15) -0.0011(16) C20 0.032(2) 0.041(2) 0.046(2) 0.0011(19) 0.0107(18) -0.0085(17) C21 0.075(4) 0.068(4) 0.043(3) 0.001(3) 0.005(3) 0.043(3) C22 0.055(3) 0.043(2) 0.037(2) 0.0048(18) 0.022(2) -0.009(2) C23 0.049(2) 0.0299(19) 0.034(2) -0.0002(15) 0.0268(18) -0.0018(17) C24 0.037(2) 0.0325(19) 0.0274(18) -0.0024(14) 0.0168(16) 0.0009(15) C25 0.0352(19) 0.0332(19) 0.0198(16) -0.0024(14) 0.0094(14) 0.0047(15) C26 0.0286(18) 0.0309(19) 0.0275(17) -0.0042(14) 0.0109(14) 0.0037(14) C27 0.043(2) 0.036(2) 0.031(2) -0.0021(16) 0.0044(17) 0.0040(18) C28 0.045(3) 0.040(2) 0.049(3) 0.008(2) 0.011(2) 0.010(2) C29 0.053(3) 0.029(2) 0.065(3) 0.001(2) 0.029(2) 0.0076(19) C30 0.048(3) 0.032(2) 0.054(3) -0.0139(19) 0.022(2) 0.0017(18) C31 0.036(2) 0.034(2) 0.036(2) -0.0094(16) 0.0111(17) 0.0030(16) C32 0.0223(16) 0.0221(16) 0.0278(17) -0.0041(13) 0.0091(13) 0.0014(12) C33 0.037(2) 0.0252(18) 0.0308(19) -0.0029(14) 0.0053(16) -0.0098(15) C34 0.061(3) 0.030(2) 0.035(2) -0.0054(17) 0.009(2) -0.0114(19) C35 0.048(2) 0.033(2) 0.032(2) -0.0020(17) -0.0041(18) -0.0112(18) C36 0.0273(17) 0.0225(16) 0.0258(17) 0.0010(13) 0.0065(14) -0.0048(13) C37 0.0292(18) 0.0234(17) 0.035(2) -0.0014(14) 0.0086(15) -0.0036(14) C38 0.0312(19) 0.0277(19) 0.039(2) 0.0028(16) 0.0009(16) -0.0044(15) C39 0.045(2) 0.034(2) 0.0279(19) 0.0002(16) 0.0043(17) -0.0147(18) C40 0.047(2) 0.034(2) 0.0294(19) -0.0079(16) 0.0165(17) -0.0129(18) C41 0.038(2) 0.0231(17) 0.0306(18) -0.0065(14) 0.0117(16) -0.0081(15) C42 0.0302(19) 0.032(2) 0.046(2) 0.0012(17) 0.0149(17) 0.0026(16) C43 0.069(3) 0.058(3) 0.030(2) 0.005(2) 0.004(2) -0.022(3) C44 0.040(2) 0.035(2) 0.042(2) -0.0049(17) 0.0183(19) -0.0005(17) C45 0.0266(17) 0.0249(17) 0.0199(15) -0.0014(13) 0.0027(13) -0.0020(13) C46 0.0291(17) 0.0270(17) 0.0227(16) 0.0001(13) 0.0059(14) 0.0005(14) C47 0.0336(19) 0.0259(18) 0.0253(17) -0.0002(13) 0.0072(15) 0.0015(14) C48 0.0345(19) 0.0333(19) 0.0191(16) -0.0011(14) 0.0046(14) -0.0067(15) C49 0.0302(18) 0.042(2) 0.0250(17) -0.0005(15) 0.0091(15) -0.0034(16) C50 0.0328(19) 0.0320(19) 0.0257(17) -0.0010(14) 0.0088(15) 0.0040(15) C51 0.034(2) 0.036(2) 0.045(2) 0.0047(18) 0.0142(18) 0.0039(17) C52 0.048(2) 0.035(2) 0.035(2) 0.0033(17) 0.0121(18) -0.0095(18) C53 0.050(3) 0.042(2) 0.047(3) -0.0008(19) 0.023(2) 0.011(2) C54 0.0271(19) 0.032(2) 0.051(2) -0.0039(18) 0.0089(17) 0.0022(15) C55 0.0237(17) 0.032(2) 0.042(2) 0.0015(16) 0.0079(16) -0.0020(15) C56 0.0270(18) 0.0314(19) 0.0287(18) 0.0016(15) 0.0008(14) -0.0062(15) C57 0.0221(16) 0.0323(19) 0.0265(17) -0.0016(14) 0.0065(13) -0.0060(14) C58 0.0275(18) 0.035(2) 0.0278(18) -0.0018(15) 0.0041(14) -0.0008(15) C59 0.032(2) 0.036(2) 0.041(2) 0.0043(17) 0.0118(17) 0.0031(16) C60 0.035(2) 0.032(2) 0.055(3) -0.0038(18) 0.021(2) -0.0036(17) C61 0.041(2) 0.041(2) 0.042(2) -0.0145(19) 0.0201(19) -0.0121(18) C62 0.036(2) 0.040(2) 0.0293(19) -0.0021(16) 0.0124(16) -0.0111(17) C63 0.037(2) 0.042(2) 0.056(3) -0.002(2) 0.011(2) 0.0019(19) Cl3 0.0417(6) 0.0546(7) 0.0517(7) -0.0062(5) 0.0086(5) -0.0015(5) Cl4 0.0559(8) 0.1006(13) 0.0719(10) -0.0380(9) 0.0172(7) -0.0006(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.038(3) . ? Pd1 C23 2.120(4) . ? Pd1 C24 2.141(4) . ? Pd1 C25 2.218(4) . ? Pd1 Cl1 2.3916(8) . ? Pd2 C32 2.055(3) . ? Pd2 C54 2.103(4) . ? Pd2 C55 2.139(4) . ? Pd2 C56 2.257(4) . ? Pd2 Cl2 2.3932(8) . ? N1 C1 1.346(4) . ? N1 C5 1.438(5) . ? N1 C2 1.472(5) . ? N2 C1 1.342(4) . ? N2 C14 1.447(5) . ? N2 C4 1.472(5) . ? N3 C32 1.333(5) . ? N3 C36 1.441(5) . ? N3 C33 1.480(5) . ? N4 C32 1.350(5) . ? N4 C45 1.441(5) . ? N4 C35 1.475(5) . ? C2 C3 1.503(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.507(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C3A H3C 0.9900 . ? C3A H3D 0.9900 . ? C5 C10 1.392(6) . ? C5 C6 1.409(5) . ? C6 C7 1.400(5) . ? C6 C11 1.498(6) . ? C7 C8 1.381(6) . ? C7 H7A 0.9500 . ? C8 C9 1.399(6) . ? C8 C12 1.511(5) . ? C9 C10 1.382(5) . ? C9 H9A 0.9500 . ? C10 C13 1.505(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.389(5) . ? C14 C19 1.391(5) . ? C15 C16 1.392(6) . ? C15 C20 1.517(6) . ? C16 C17 1.384(7) . ? C16 H16A 0.9500 . ? C17 C18 1.367(7) . ? C17 C21 1.527(6) . ? C18 C19 1.393(6) . ? C18 H18A 0.9500 . ? C19 C22 1.508(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.403(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.397(6) . ? C24 H24A 1.0000 . ? C25 C26 1.476(5) . ? C25 H25A 1.0000 . ? C26 C31 1.386(5) . ? C26 C27 1.408(5) . ? C27 C28 1.386(6) . ? C27 H27A 0.9500 . ? C28 C29 1.377(7) . ? C28 H28A 0.9500 . ? C29 C30 1.380(7) . ? C29 H29A 0.9500 . ? C30 C31 1.375(6) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? C33 C34 1.511(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.493(6) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.401(5) . ? C36 C41 1.402(5) . ? C37 C38 1.377(6) . ? C37 C42 1.519(6) . ? C38 C39 1.389(7) . ? C38 H38A 0.9500 . ? C39 C40 1.386(7) . ? C39 C43 1.509(6) . ? C40 C41 1.405(6) . ? C40 H40A 0.9500 . ? C41 C44 1.499(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C50 1.395(5) . ? C45 C46 1.396(5) . ? C46 C47 1.391(5) . ? C46 C51 1.505(6) . ? C47 C48 1.388(6) . ? C47 H47A 0.9500 . ? C48 C49 1.391(6) . ? C48 C52 1.507(5) . ? C49 C50 1.389(6) . ? C49 H49A 0.9500 . ? C50 C53 1.509(6) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.411(6) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.400(6) . ? C55 H55A 1.0000 . ? C56 C57 1.470(5) . ? C56 H56A 1.0000 . ? C57 C62 1.393(5) . ? C57 C58 1.402(5) . ? C58 C59 1.380(6) . ? C58 H58A 0.9500 . ? C59 C60 1.387(6) . ? C59 H59A 0.9500 . ? C60 C61 1.396(7) . ? C60 H60A 0.9500 . ? C61 C62 1.386(6) . ? C61 H61A 0.9500 . ? C62 H62A 0.9500 . ? C63 Cl3 1.771(3) . ? C63 Cl4 1.771(3) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 C23 102.56(14) . . ? C1 Pd1 C24 131.99(14) . . ? C23 Pd1 C24 38.45(15) . . ? C1 Pd1 C25 169.32(14) . . ? C23 Pd1 C25 67.89(15) . . ? C24 Pd1 C25 37.34(15) . . ? C1 Pd1 Cl1 94.09(10) . . ? C23 Pd1 Cl1 159.74(12) . . ? C24 Pd1 Cl1 131.44(11) . . ? C25 Pd1 Cl1 96.26(11) . . ? C32 Pd2 C54 100.00(15) . . ? C32 Pd2 C55 130.25(15) . . ? C54 Pd2 C55 38.85(16) . . ? C32 Pd2 C56 166.91(14) . . ? C54 Pd2 C56 67.42(16) . . ? C55 Pd2 C56 37.02(15) . . ? C32 Pd2 Cl2 98.34(10) . . ? C54 Pd2 Cl2 160.09(12) . . ? C55 Pd2 Cl2 128.10(11) . . ? C56 Pd2 Cl2 94.63(11) . . ? C1 N1 C5 119.1(3) . . ? C1 N1 C2 125.5(3) . . ? C5 N1 C2 115.0(3) . . ? C1 N2 C14 119.1(3) . . ? C1 N2 C4 124.6(3) . . ? C14 N2 C4 116.1(3) . . ? C32 N3 C36 122.2(3) . . ? C32 N3 C33 124.4(3) . . ? C36 N3 C33 113.4(3) . . ? C32 N4 C45 118.7(3) . . ? C32 N4 C35 124.8(3) . . ? C45 N4 C35 116.4(3) . . ? N2 C1 N1 117.5(3) . . ? N2 C1 Pd1 117.4(2) . . ? N1 C1 Pd1 125.0(2) . . ? N1 C2 C3 108.7(4) . . ? N1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? N1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 C3 C4 112.2(4) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N2 C4 C3 108.7(4) . . ? N2 C4 H4A 110.0 . . ? C3 C4 H4A 110.0 . . ? N2 C4 H4B 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.3 . . ? H3C C3A H3D 107.4 . . ? C10 C5 C6 121.7(3) . . ? C10 C5 N1 119.0(3) . . ? C6 C5 N1 119.1(3) . . ? C7 C6 C5 117.5(4) . . ? C7 C6 C11 121.1(4) . . ? C5 C6 C11 121.4(4) . . ? C8 C7 C6 122.0(4) . . ? C8 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? C7 C8 C9 118.3(4) . . ? C7 C8 C12 121.5(4) . . ? C9 C8 C12 120.2(4) . . ? C10 C9 C8 122.1(4) . . ? C10 C9 H9A 118.9 . . ? C8 C9 H9A 118.9 . . ? C9 C10 C5 118.1(3) . . ? C9 C10 C13 120.1(4) . . ? C5 C10 C13 121.8(3) . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 120.9(4) . . ? C15 C14 N2 119.8(3) . . ? C19 C14 N2 119.3(3) . . ? C14 C15 C16 118.1(4) . . ? C14 C15 C20 122.1(4) . . ? C16 C15 C20 119.7(4) . . ? C17 C16 C15 122.2(4) . . ? C17 C16 H16A 118.9 . . ? C15 C16 H16A 118.9 . . ? C18 C17 C16 118.0(4) . . ? C18 C17 C21 122.0(5) . . ? C16 C17 C21 119.9(5) . . ? C17 C18 C19 122.2(4) . . ? C17 C18 H18A 118.9 . . ? C19 C18 H18A 118.9 . . ? C14 C19 C18 118.5(4) . . ? C14 C19 C22 121.1(4) . . ? C18 C19 C22 120.5(4) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 H21A 109.5 . . ? C17 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C17 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 Pd1 71.6(2) . . ? C24 C23 H23A 116.4 . . ? Pd1 C23 H23A 116.4 . . ? C24 C23 H23B 116.4 . . ? Pd1 C23 H23B 116.4 . . ? H23A C23 H23B 113.4 . . ? C25 C24 C23 119.9(4) . . ? C25 C24 Pd1 74.3(2) . . ? C23 C24 Pd1 70.0(2) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? Pd1 C24 H24A 119.8 . . ? C24 C25 C26 122.7(4) . . ? C24 C25 Pd1 68.3(2) . . ? C26 C25 Pd1 120.6(3) . . ? C24 C25 H25A 112.8 . . ? C26 C25 H25A 112.8 . . ? Pd1 C25 H25A 112.8 . . ? C31 C26 C27 118.6(4) . . ? C31 C26 C25 120.6(3) . . ? C27 C26 C25 120.8(3) . . ? C28 C27 C26 119.1(4) . . ? C28 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? C29 C28 C27 121.6(4) . . ? C29 C28 H28A 119.2 . . ? C27 C28 H28A 119.2 . . ? C28 C29 C30 119.1(4) . . ? C28 C29 H29A 120.4 . . ? C30 C29 H29A 120.4 . . ? C31 C30 C29 120.3(4) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C30 C31 C26 121.3(4) . . ? C30 C31 H31A 119.3 . . ? C26 C31 H31A 119.3 . . ? N3 C32 N4 117.2(3) . . ? N3 C32 Pd2 126.1(3) . . ? N4 C32 Pd2 116.7(3) . . ? N3 C33 C34 110.8(3) . . ? N3 C33 H33A 109.5 . . ? C34 C33 H33A 109.5 . . ? N3 C33 H33B 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 108.1 . . ? C35 C34 C33 109.6(4) . . ? C35 C34 H34A 109.8 . . ? C33 C34 H34A 109.8 . . ? C35 C34 H34B 109.8 . . ? C33 C34 H34B 109.8 . . ? H34A C34 H34B 108.2 . . ? N4 C35 C34 110.1(3) . . ? N4 C35 H35A 109.6 . . ? C34 C35 H35A 109.6 . . ? N4 C35 H35B 109.6 . . ? C34 C35 H35B 109.6 . . ? H35A C35 H35B 108.2 . . ? C37 C36 C41 121.5(3) . . ? C37 C36 N3 119.0(3) . . ? C41 C36 N3 119.2(3) . . ? C38 C37 C36 118.6(4) . . ? C38 C37 C42 121.0(4) . . ? C36 C37 C42 120.4(4) . . ? C37 C38 C39 121.8(4) . . ? C37 C38 H38A 119.1 . . ? C39 C38 H38A 119.1 . . ? C40 C39 C38 119.0(4) . . ? C40 C39 C43 120.2(5) . . ? C38 C39 C43 120.8(5) . . ? C39 C40 C41 121.5(4) . . ? C39 C40 H40A 119.3 . . ? C41 C40 H40A 119.3 . . ? C36 C41 C40 117.7(4) . . ? C36 C41 C44 121.8(4) . . ? C40 C41 C44 120.5(4) . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C39 C43 H43A 109.5 . . ? C39 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C39 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C50 C45 C46 121.5(3) . . ? C50 C45 N4 118.8(3) . . ? C46 C45 N4 119.6(3) . . ? C47 C46 C45 118.0(4) . . ? C47 C46 C51 120.6(3) . . ? C45 C46 C51 121.4(3) . . ? C48 C47 C46 121.7(4) . . ? C48 C47 H47A 119.1 . . ? C46 C47 H47A 119.1 . . ? C47 C48 C49 118.4(4) . . ? C47 C48 C52 120.9(4) . . ? C49 C48 C52 120.7(4) . . ? C50 C49 C48 121.7(4) . . ? C50 C49 H49A 119.1 . . ? C48 C49 H49A 119.1 . . ? C49 C50 C45 118.1(4) . . ? C49 C50 C53 120.6(4) . . ? C45 C50 C53 121.3(4) . . ? C46 C51 H51A 109.5 . . ? C46 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C46 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C48 C52 H52A 109.5 . . ? C48 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C48 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 Pd2 71.9(2) . . ? C55 C54 H54A 116.4 . . ? Pd2 C54 H54A 116.4 . . ? C55 C54 H54B 116.4 . . ? Pd2 C54 H54B 116.4 . . ? H54A C54 H54B 113.4 . . ? C56 C55 C54 119.1(4) . . ? C56 C55 Pd2 76.1(2) . . ? C54 C55 Pd2 69.2(2) . . ? C56 C55 H55A 120.3 . . ? C54 C55 H55A 120.3 . . ? Pd2 C55 H55A 120.3 . . ? C55 C56 C57 123.6(4) . . ? C55 C56 Pd2 66.9(2) . . ? C57 C56 Pd2 123.2(3) . . ? C55 C56 H56A 112.0 . . ? C57 C56 H56A 112.0 . . ? Pd2 C56 H56A 112.0 . . ? C62 C57 C58 117.7(4) . . ? C62 C57 C56 119.4(3) . . ? C58 C57 C56 122.9(3) . . ? C59 C58 C57 120.3(4) . . ? C59 C58 H58A 119.8 . . ? C57 C58 H58A 119.8 . . ? C58 C59 C60 121.6(4) . . ? C58 C59 H59A 119.2 . . ? C60 C59 H59A 119.2 . . ? C59 C60 C61 118.7(4) . . ? C59 C60 H60A 120.6 . . ? C61 C60 H60A 120.6 . . ? C62 C61 C60 119.7(4) . . ? C62 C61 H61A 120.2 . . ? C60 C61 H61A 120.2 . . ? C61 C62 C57 121.9(4) . . ? C61 C62 H62A 119.0 . . ? C57 C62 H62A 119.0 . . ? Cl3 C63 Cl4 110.88(18) . . ? Cl3 C63 H63A 109.5 . . ? Cl4 C63 H63A 109.5 . . ? Cl3 C63 H63B 109.5 . . ? Cl4 C63 H63B 109.5 . . ? H63A C63 H63B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 N2 C1 N1 -178.1(3) . . . . ? C4 N2 C1 N1 -3.1(5) . . . . ? C14 N2 C1 Pd1 3.4(4) . . . . ? C4 N2 C1 Pd1 178.3(3) . . . . ? C5 N1 C1 N2 173.6(3) . . . . ? C2 N1 C1 N2 0.7(5) . . . . ? C5 N1 C1 Pd1 -8.0(5) . . . . ? C2 N1 C1 Pd1 179.2(3) . . . . ? C23 Pd1 C1 N2 -107.1(3) . . . . ? C24 Pd1 C1 N2 -78.6(3) . . . . ? C25 Pd1 C1 N2 -81.2(8) . . . . ? Cl1 Pd1 C1 N2 84.5(3) . . . . ? C23 Pd1 C1 N1 74.5(3) . . . . ? C24 Pd1 C1 N1 103.0(3) . . . . ? C25 Pd1 C1 N1 100.4(8) . . . . ? Cl1 Pd1 C1 N1 -93.9(3) . . . . ? C1 N1 C2 C3 -24.5(6) . . . . ? C5 N1 C2 C3 162.4(4) . . . . ? N1 C2 C3 C4 49.7(6) . . . . ? C1 N2 C4 C3 28.8(6) . . . . ? C14 N2 C4 C3 -156.1(4) . . . . ? C2 C3 C4 N2 -51.8(7) . . . . ? C1 N1 C5 C10 -87.1(4) . . . . ? C2 N1 C5 C10 86.4(4) . . . . ? C1 N1 C5 C6 96.8(4) . . . . ? C2 N1 C5 C6 -89.6(4) . . . . ? C10 C5 C6 C7 4.1(5) . . . . ? N1 C5 C6 C7 -179.9(3) . . . . ? C10 C5 C6 C11 -175.6(4) . . . . ? N1 C5 C6 C11 0.4(5) . . . . ? C5 C6 C7 C8 0.1(5) . . . . ? C11 C6 C7 C8 179.8(4) . . . . ? C6 C7 C8 C9 -3.4(6) . . . . ? C6 C7 C8 C12 176.5(4) . . . . ? C7 C8 C9 C10 2.5(6) . . . . ? C12 C8 C9 C10 -177.3(4) . . . . ? C8 C9 C10 C5 1.5(6) . . . . ? C8 C9 C10 C13 -177.5(4) . . . . ? C6 C5 C10 C9 -4.9(5) . . . . ? N1 C5 C10 C9 179.1(3) . . . . ? C6 C5 C10 C13 174.1(4) . . . . ? N1 C5 C10 C13 -1.9(5) . . . . ? C1 N2 C14 C15 80.3(4) . . . . ? C4 N2 C14 C15 -95.1(4) . . . . ? C1 N2 C14 C19 -101.9(4) . . . . ? C4 N2 C14 C19 82.8(4) . . . . ? C19 C14 C15 C16 3.2(5) . . . . ? N2 C14 C15 C16 -179.0(3) . . . . ? C19 C14 C15 C20 -173.3(4) . . . . ? N2 C14 C15 C20 4.5(5) . . . . ? C14 C15 C16 C17 -0.8(6) . . . . ? C20 C15 C16 C17 175.8(4) . . . . ? C15 C16 C17 C18 -1.7(6) . . . . ? C15 C16 C17 C21 -178.9(4) . . . . ? C16 C17 C18 C19 1.9(6) . . . . ? C21 C17 C18 C19 179.0(4) . . . . ? C15 C14 C19 C18 -3.1(5) . . . . ? N2 C14 C19 C18 179.1(3) . . . . ? C15 C14 C19 C22 175.5(4) . . . . ? N2 C14 C19 C22 -2.3(5) . . . . ? C17 C18 C19 C14 0.4(6) . . . . ? C17 C18 C19 C22 -178.1(4) . . . . ? C1 Pd1 C23 C24 145.2(2) . . . . ? C25 Pd1 C23 C24 -29.7(2) . . . . ? Cl1 Pd1 C23 C24 -70.2(4) . . . . ? Pd1 C23 C24 C25 57.2(3) . . . . ? C1 Pd1 C24 C25 -179.2(2) . . . . ? C23 Pd1 C24 C25 -130.7(4) . . . . ? Cl1 Pd1 C24 C25 23.5(3) . . . . ? C1 Pd1 C24 C23 -48.5(3) . . . . ? C25 Pd1 C24 C23 130.7(4) . . . . ? Cl1 Pd1 C24 C23 154.2(2) . . . . ? C23 C24 C25 C26 -168.4(3) . . . . ? Pd1 C24 C25 C26 -113.3(3) . . . . ? C23 C24 C25 Pd1 -55.2(3) . . . . ? C1 Pd1 C25 C24 3.1(8) . . . . ? C23 Pd1 C25 C24 30.6(2) . . . . ? Cl1 Pd1 C25 C24 -162.5(2) . . . . ? C1 Pd1 C25 C26 119.3(7) . . . . ? C23 Pd1 C25 C26 146.7(3) . . . . ? C24 Pd1 C25 C26 116.1(4) . . . . ? Cl1 Pd1 C25 C26 -46.4(3) . . . . ? C24 C25 C26 C31 -144.7(4) . . . . ? Pd1 C25 C26 C31 132.8(3) . . . . ? C24 C25 C26 C27 33.9(6) . . . . ? Pd1 C25 C26 C27 -48.6(5) . . . . ? C31 C26 C27 C28 0.6(7) . . . . ? C25 C26 C27 C28 -178.0(4) . . . . ? C26 C27 C28 C29 0.6(8) . . . . ? C27 C28 C29 C30 -2.0(8) . . . . ? C28 C29 C30 C31 2.2(7) . . . . ? C29 C30 C31 C26 -1.1(7) . . . . ? C27 C26 C31 C30 -0.4(6) . . . . ? C25 C26 C31 C30 178.3(4) . . . . ? C36 N3 C32 N4 177.9(3) . . . . ? C33 N3 C32 N4 -1.4(5) . . . . ? C36 N3 C32 Pd2 -2.7(5) . . . . ? C33 N3 C32 Pd2 178.0(3) . . . . ? C45 N4 C32 N3 175.2(3) . . . . ? C35 N4 C32 N3 -0.3(6) . . . . ? C45 N4 C32 Pd2 -4.3(4) . . . . ? C35 N4 C32 Pd2 -179.7(3) . . . . ? C54 Pd2 C32 N3 -80.1(3) . . . . ? C55 Pd2 C32 N3 -107.6(3) . . . . ? C56 Pd2 C32 N3 -95.6(7) . . . . ? Cl2 Pd2 C32 N3 92.2(3) . . . . ? C54 Pd2 C32 N4 99.4(3) . . . . ? C55 Pd2 C32 N4 71.8(3) . . . . ? C56 Pd2 C32 N4 83.8(7) . . . . ? Cl2 Pd2 C32 N4 -88.4(3) . . . . ? C32 N3 C33 C34 -24.6(5) . . . . ? C36 N3 C33 C34 156.0(4) . . . . ? N3 C33 C34 C35 50.3(5) . . . . ? C32 N4 C35 C34 28.0(6) . . . . ? C45 N4 C35 C34 -147.5(4) . . . . ? C33 C34 C35 N4 -51.5(6) . . . . ? C32 N3 C36 C37 97.4(4) . . . . ? C33 N3 C36 C37 -83.2(4) . . . . ? C32 N3 C36 C41 -89.2(4) . . . . ? C33 N3 C36 C41 90.1(4) . . . . ? C41 C36 C37 C38 0.4(5) . . . . ? N3 C36 C37 C38 173.6(3) . . . . ? C41 C36 C37 C42 -177.0(3) . . . . ? N3 C36 C37 C42 -3.8(5) . . . . ? C36 C37 C38 C39 0.1(6) . . . . ? C42 C37 C38 C39 177.4(4) . . . . ? C37 C38 C39 C40 0.0(6) . . . . ? C37 C38 C39 C43 -178.8(4) . . . . ? C38 C39 C40 C41 -0.6(6) . . . . ? C43 C39 C40 C41 178.2(4) . . . . ? C37 C36 C41 C40 -1.0(5) . . . . ? N3 C36 C41 C40 -174.1(3) . . . . ? C37 C36 C41 C44 176.6(4) . . . . ? N3 C36 C41 C44 3.4(5) . . . . ? C39 C40 C41 C36 1.1(6) . . . . ? C39 C40 C41 C44 -176.5(4) . . . . ? C32 N4 C45 C50 -85.8(4) . . . . ? C35 N4 C45 C50 90.0(4) . . . . ? C32 N4 C45 C46 98.1(4) . . . . ? C35 N4 C45 C46 -86.1(4) . . . . ? C50 C45 C46 C47 6.6(5) . . . . ? N4 C45 C46 C47 -177.3(3) . . . . ? C50 C45 C46 C51 -172.6(4) . . . . ? N4 C45 C46 C51 3.4(5) . . . . ? C45 C46 C47 C48 -0.1(5) . . . . ? C51 C46 C47 C48 179.2(4) . . . . ? C46 C47 C48 C49 -4.4(6) . . . . ? C46 C47 C48 C52 176.0(4) . . . . ? C47 C48 C49 C50 2.6(6) . . . . ? C52 C48 C49 C50 -177.8(4) . . . . ? C48 C49 C50 C45 3.7(6) . . . . ? C48 C49 C50 C53 -172.8(4) . . . . ? C46 C45 C50 C49 -8.4(5) . . . . ? N4 C45 C50 C49 175.5(3) . . . . ? C46 C45 C50 C53 168.1(4) . . . . ? N4 C45 C50 C53 -8.0(5) . . . . ? C32 Pd2 C54 C55 -145.8(3) . . . . ? C56 Pd2 C54 C55 30.4(2) . . . . ? Cl2 Pd2 C54 C55 57.3(5) . . . . ? Pd2 C54 C55 C56 -59.6(3) . . . . ? C32 Pd2 C55 C56 175.5(2) . . . . ? C54 Pd2 C55 C56 129.0(4) . . . . ? Cl2 Pd2 C55 C56 -29.6(3) . . . . ? C32 Pd2 C55 C54 46.5(3) . . . . ? C56 Pd2 C55 C54 -129.0(4) . . . . ? Cl2 Pd2 C55 C54 -158.6(2) . . . . ? C54 C55 C56 C57 171.8(4) . . . . ? Pd2 C55 C56 C57 115.6(3) . . . . ? C54 C55 C56 Pd2 56.2(3) . . . . ? C32 Pd2 C56 C55 -15.2(7) . . . . ? C54 Pd2 C56 C55 -31.9(3) . . . . ? Cl2 Pd2 C56 C55 157.0(2) . . . . ? C32 Pd2 C56 C57 -131.3(6) . . . . ? C54 Pd2 C56 C57 -147.9(4) . . . . ? C55 Pd2 C56 C57 -116.0(4) . . . . ? Cl2 Pd2 C56 C57 41.0(3) . . . . ? C55 C56 C57 C62 150.9(4) . . . . ? Pd2 C56 C57 C62 -126.5(3) . . . . ? C55 C56 C57 C58 -27.1(6) . . . . ? Pd2 C56 C57 C58 55.5(5) . . . . ? C62 C57 C58 C59 -2.3(6) . . . . ? C56 C57 C58 C59 175.7(4) . . . . ? C57 C58 C59 C60 1.8(6) . . . . ? C58 C59 C60 C61 0.4(6) . . . . ? C59 C60 C61 C62 -1.8(6) . . . . ? C60 C61 C62 C57 1.3(6) . . . . ? C58 C57 C62 C61 0.8(6) . . . . ? C56 C57 C62 C61 -177.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.383 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.136 data_KEPd6 _database_code_depnum_ccdc_archive 'CCDC 784540' #TrackingRef 'KEPd6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H49 Cl N2 Pd, C4 H10 O' _chemical_formula_sum 'C41 H59 Cl N2 O Pd' _chemical_formula_weight 737.75 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.3349(8) _cell_length_b 15.0596(8) _cell_length_c 17.9807(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3881.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7617 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.79 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_T_max 0.944 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 SMART APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 43509 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.00 _reflns_number_total 9340 _reflns_number_gt 7374 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_data_reduction 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_structure_solution 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_publication_material 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0559P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 9340 _refine_ls_number_parameters 398 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1022 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.049880(19) 0.064513(18) 0.898380(15) 0.02427(8) Uani 1 1 d . . . Cl1 Cl -0.07742(6) 0.13779(7) 0.95129(5) 0.0290(2) Uani 1 1 d . . . N1 N 0.1370(2) 0.08829(19) 1.05053(17) 0.0225(7) Uani 1 1 d . . . N2 N 0.1864(2) 0.1843(2) 0.96043(17) 0.0232(7) Uani 1 1 d . . . C1 C 0.1371(2) 0.1120(2) 0.9789(2) 0.0202(7) Uani 1 1 d . A . C2 C 0.1849(3) 0.1376(2) 1.1105(2) 0.0311(9) Uani 0.70 1 d PD A 1 H2A H 0.2464 0.1101 1.1203 0.037 Uiso 0.70 1 calc PR A 1 H2B H 0.1475 0.1341 1.1567 0.037 Uiso 0.70 1 calc PR A 1 C3 C 0.1982(4) 0.2335(3) 1.0890(2) 0.0323(13) Uani 0.70 1 d PD A 1 H3A H 0.1376 0.2649 1.0923 0.039 Uiso 0.70 1 calc PR A 1 H3B H 0.2417 0.2621 1.1245 0.039 Uiso 0.70 1 calc PR A 1 C4 C 0.2360(3) 0.2421(3) 1.0117(2) 0.0418(11) Uani 0.70 1 d PD A 1 H4A H 0.2300 0.3045 0.9949 0.050 Uiso 0.70 1 calc PR A 1 H4B H 0.3031 0.2265 1.0116 0.050 Uiso 0.70 1 calc PR A 1 C2A C 0.1849(3) 0.1376(2) 1.1105(2) 0.0311(9) Uani 0.30 1 d P A 2 H2C H 0.2117 0.0943 1.1459 0.037 Uiso 0.30 1 calc PR A 2 H2D H 0.1381 0.1733 1.1377 0.037 Uiso 0.30 1 calc PR A 2 C3A C 0.2614(5) 0.1983(7) 1.0842(4) 0.027(3) Uani 0.30 1 d PD A 2 H3C H 0.3196 0.1638 1.0777 0.032 Uiso 0.30 1 calc PRD A 2 H3D H 0.2730 0.2445 1.1223 0.032 Uiso 0.30 1 calc PR A 2 C4A C 0.2360(3) 0.2421(3) 1.0117(2) 0.0418(11) Uani 0.30 1 d P A 2 H4C H 0.1967 0.2947 1.0222 0.050 Uiso 0.30 1 calc PR A 2 H4D H 0.2938 0.2633 0.9873 0.050 Uiso 0.30 1 calc PR A 2 C5 C 0.0990(3) 0.0036(2) 1.0742(2) 0.0221(8) Uani 1 1 d . A . C6 C 0.0171(3) 0.0021(3) 1.1165(2) 0.0271(9) Uani 1 1 d . . . C7 C -0.0132(3) -0.0809(3) 1.1418(2) 0.0315(9) Uani 1 1 d . A . H7A H -0.0683 -0.0842 1.1711 0.038 Uiso 1 1 calc R . . C8 C 0.0343(3) -0.1575(3) 1.1256(2) 0.0339(10) Uani 1 1 d . . . H8A H 0.0108 -0.2131 1.1422 0.041 Uiso 1 1 calc R A . C9 C 0.1164(3) -0.1541(2) 1.0851(2) 0.0280(9) Uani 1 1 d . A . H9A H 0.1498 -0.2073 1.0751 0.034 Uiso 1 1 calc R . . C10 C 0.1502(3) -0.0736(3) 1.05892(19) 0.0265(8) Uani 1 1 d . . . C11 C -0.0375(3) 0.0844(2) 1.1380(2) 0.0295(9) Uani 1 1 d . A . H11A H -0.0148 0.1349 1.1067 0.035 Uiso 1 1 calc R . . C12 C -0.0215(3) 0.1086(3) 1.2198(2) 0.0384(10) Uani 1 1 d . . . H12A H 0.0456 0.1147 1.2291 0.058 Uiso 1 1 calc R A . H12B H -0.0470 0.0617 1.2516 0.058 Uiso 1 1 calc R . . H12C H -0.0528 0.1649 1.2309 0.058 Uiso 1 1 calc R . . C13 C -0.1427(3) 0.0742(3) 1.1250(2) 0.0362(10) Uani 1 1 d . . . H13A H -0.1538 0.0534 1.0741 0.054 Uiso 1 1 calc R A . H13B H -0.1734 0.1317 1.1322 0.054 Uiso 1 1 calc R . . H13C H -0.1682 0.0310 1.1603 0.054 Uiso 1 1 calc R . . C14 C 0.2445(3) -0.0722(3) 1.0204(2) 0.0341(9) Uani 1 1 d . A . H14A H 0.2479 -0.0171 0.9895 0.041 Uiso 1 1 calc R . . C15 C 0.2615(4) -0.1508(3) 0.9696(3) 0.0539(14) Uani 1 1 d . . . H15A H 0.3224 -0.1443 0.9454 0.081 Uiso 1 1 calc R A . H15B H 0.2125 -0.1532 0.9316 0.081 Uiso 1 1 calc R . . H15C H 0.2607 -0.2057 0.9988 0.081 Uiso 1 1 calc R . . C16 C 0.3223(3) -0.0680(4) 1.0778(3) 0.0566(14) Uani 1 1 d . . . H16A H 0.3822 -0.0593 1.0526 0.085 Uiso 1 1 calc R A . H16B H 0.3240 -0.1237 1.1060 0.085 Uiso 1 1 calc R . . H16C H 0.3109 -0.0184 1.1119 0.085 Uiso 1 1 calc R . . C17 C 0.2002(3) 0.2073(2) 0.8826(2) 0.0269(8) Uani 1 1 d . A . C18 C 0.1403(3) 0.2710(3) 0.8494(2) 0.0333(10) Uani 1 1 d . . . C19 C 0.1577(3) 0.2920(3) 0.7754(2) 0.0387(11) Uani 1 1 d . A . H19A H 0.1185 0.3338 0.7512 0.046 Uiso 1 1 calc R . . C20 C 0.2303(4) 0.2539(3) 0.7360(3) 0.0482(13) Uani 1 1 d . . . H20A H 0.2397 0.2688 0.6852 0.058 Uiso 1 1 calc R A . C21 C 0.2887(3) 0.1944(3) 0.7706(2) 0.0389(11) Uani 1 1 d . A . H21A H 0.3387 0.1689 0.7433 0.047 Uiso 1 1 calc R . . C22 C 0.2763(3) 0.1707(3) 0.8449(2) 0.0301(9) Uani 1 1 d . . . C23 C 0.0651(3) 0.3183(3) 0.8918(3) 0.0387(10) Uani 1 1 d . A . H23A H 0.0529 0.2841 0.9385 0.046 Uiso 1 1 calc R . . C24 C -0.0269(3) 0.3250(4) 0.8489(3) 0.0570(15) Uani 1 1 d . . . H24A H -0.0139 0.3267 0.7954 0.086 Uiso 1 1 calc R A . H24B H -0.0597 0.3793 0.8636 0.086 Uiso 1 1 calc R . . H24C H -0.0658 0.2733 0.8602 0.086 Uiso 1 1 calc R . . C25 C 0.0989(4) 0.4118(3) 0.9140(3) 0.0563(14) Uani 1 1 d . . . H25A H 0.1521 0.4066 0.9480 0.085 Uiso 1 1 calc R A . H25B H 0.0481 0.4438 0.9389 0.085 Uiso 1 1 calc R . . H25C H 0.1179 0.4444 0.8694 0.085 Uiso 1 1 calc R . . C26 C 0.3496(3) 0.1126(3) 0.8831(3) 0.0408(11) Uani 1 1 d . A . H26A H 0.3218 0.0884 0.9299 0.049 Uiso 1 1 calc R . . C27 C 0.3842(4) 0.0353(3) 0.8368(3) 0.0580(15) Uani 1 1 d . . . H27A H 0.3308 0.0007 0.8190 0.087 Uiso 1 1 calc R A . H27B H 0.4244 -0.0027 0.8674 0.087 Uiso 1 1 calc R . . H27C H 0.4197 0.0577 0.7942 0.087 Uiso 1 1 calc R . . C28 C 0.4356(3) 0.1687(3) 0.9041(3) 0.0513(12) Uani 1 1 d . . . H28A H 0.4806 0.1314 0.9307 0.077 Uiso 1 1 calc R A . H28B H 0.4163 0.2180 0.9361 0.077 Uiso 1 1 calc R . . H28C H 0.4646 0.1921 0.8588 0.077 Uiso 1 1 calc R . . C29 C 0.1297(3) -0.0252(3) 0.8342(3) 0.0508(14) Uani 1 1 d . . . H29A H 0.1967 -0.0110 0.8284 0.061 Uiso 1 1 calc R . . H29B H 0.1174 -0.0891 0.8424 0.061 Uiso 1 1 calc R . . C30 C 0.0681(3) 0.0193(3) 0.7868(2) 0.0495(13) Uani 1 1 d . . . H30A H 0.0926 0.0605 0.7478 0.059 Uiso 1 1 calc R . . C31 C -0.0282(3) 0.0147(3) 0.8014(3) 0.0380(11) Uani 1 1 d . . . H31A H -0.0501 -0.0478 0.8085 0.046 Uiso 1 1 calc R . . C32 C -0.0977(5) 0.0695(4) 0.7654(4) 0.0753(7) Uani 1 1 d . . . C33 C -0.0773(5) 0.1332(4) 0.7101(4) 0.0753(7) Uani 1 1 d . . . H33A H -0.0143 0.1417 0.6951 0.090 Uiso 1 1 calc R . . C34 C -0.1462(5) 0.1835(4) 0.6773(4) 0.0753(7) Uani 1 1 d . . . H34A H -0.1317 0.2226 0.6375 0.090 Uiso 1 1 calc R . . C35 C -0.2376(5) 0.1762(4) 0.7032(4) 0.0753(7) Uani 1 1 d . . . H35A H -0.2845 0.2142 0.6837 0.090 Uiso 1 1 calc R . . C36 C -0.2604(5) 0.1147(4) 0.7564(4) 0.0753(7) Uani 1 1 d . . . H36A H -0.3235 0.1084 0.7718 0.090 Uiso 1 1 calc R . . C37 C -0.1916(4) 0.0615(5) 0.7881(4) 0.0753(7) Uani 1 1 d . . . H37A H -0.2081 0.0196 0.8253 0.090 Uiso 1 1 calc R . . O1 O 0.2100(3) 0.3659(2) 0.5691(2) 0.0655(12) Uani 1 1 d . . . C38 C 0.3640(4) 0.4204(4) 0.5795(3) 0.0753(7) Uani 1 1 d . . . H38A H 0.4082 0.4633 0.5587 0.113 Uiso 1 1 calc R . . H38B H 0.3899 0.3604 0.5753 0.113 Uiso 1 1 calc R . . H38C H 0.3527 0.4343 0.6320 0.113 Uiso 1 1 calc R . . C39 C 0.2747(5) 0.4252(4) 0.5379(3) 0.0710(18) Uani 1 1 d . . . H39A H 0.2498 0.4865 0.5401 0.085 Uiso 1 1 calc R . . H39B H 0.2855 0.4099 0.4851 0.085 Uiso 1 1 calc R . . C40 C 0.1224(4) 0.3700(4) 0.5312(3) 0.0610(16) Uani 1 1 d . . . H40A H 0.1309 0.3540 0.4782 0.073 Uiso 1 1 calc R . . H40B H 0.0970 0.4310 0.5337 0.073 Uiso 1 1 calc R . . C41 C 0.0550(4) 0.3051(4) 0.5681(3) 0.0667(16) Uani 1 1 d . . . H41A H -0.0065 0.3101 0.5447 0.100 Uiso 1 1 calc R . . H41B H 0.0498 0.3192 0.6212 0.100 Uiso 1 1 calc R . . H41D H 0.0784 0.2444 0.5622 0.100 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 0.02552(13) 0.02310(12) 0.02419(12) -0.00438(13) -0.00332(13) 0.00054(12) Cl1 0.0239(5) 0.0331(5) 0.0300(5) -0.0012(4) -0.0001(4) 0.0039(4) N1 0.0241(16) 0.0196(16) 0.0239(16) -0.0007(12) -0.0015(13) -0.0026(12) N2 0.0313(17) 0.0183(15) 0.0199(16) -0.0020(13) 0.0002(13) -0.0028(13) C1 0.0202(18) 0.0171(17) 0.0232(19) -0.0007(14) 0.0020(14) 0.0038(14) C2 0.041(2) 0.029(2) 0.023(2) -0.0022(18) -0.0093(17) -0.0067(16) C3 0.036(3) 0.034(3) 0.028(3) -0.007(3) 0.000(3) -0.005(3) C4 0.062(3) 0.032(2) 0.031(2) 0.000(2) -0.013(2) -0.020(2) C2A 0.041(2) 0.029(2) 0.023(2) -0.0022(18) -0.0093(17) -0.0067(16) C3A 0.034(7) 0.025(6) 0.021(7) -0.002(5) 0.005(5) -0.016(6) C4A 0.062(3) 0.032(2) 0.031(2) 0.000(2) -0.013(2) -0.020(2) C5 0.026(2) 0.0223(19) 0.0181(17) 0.0018(14) -0.0072(14) -0.0045(15) C6 0.0270(19) 0.0251(18) 0.029(2) 0.0042(16) -0.0027(15) 0.0003(15) C7 0.032(2) 0.032(2) 0.031(2) 0.0105(18) 0.0006(16) -0.0063(16) C8 0.045(3) 0.027(2) 0.030(2) 0.0087(16) -0.0058(18) -0.0078(19) C9 0.036(2) 0.0203(18) 0.028(2) 0.0039(15) -0.0062(16) -0.0003(15) C10 0.0318(19) 0.027(2) 0.0208(18) 0.0028(17) -0.0025(14) -0.0006(17) C11 0.033(2) 0.029(2) 0.0266(18) 0.0081(15) 0.0007(16) 0.0051(17) C12 0.045(3) 0.040(2) 0.030(2) 0.0005(19) 0.0022(18) 0.0107(19) C13 0.033(2) 0.038(2) 0.038(2) 0.012(2) 0.0070(17) 0.0027(19) C14 0.038(2) 0.022(2) 0.043(2) 0.005(2) 0.0115(18) 0.0055(19) C15 0.058(3) 0.048(3) 0.056(3) -0.005(3) 0.013(3) 0.017(2) C16 0.030(2) 0.050(3) 0.089(4) -0.006(3) 0.003(2) 0.000(2) C17 0.037(2) 0.0236(19) 0.021(2) 0.0023(15) -0.0020(15) -0.0088(15) C18 0.032(2) 0.027(2) 0.041(2) 0.0065(18) -0.0103(18) -0.0094(17) C19 0.051(3) 0.036(2) 0.030(2) 0.0112(19) -0.012(2) -0.014(2) C20 0.074(4) 0.049(3) 0.022(2) 0.007(2) -0.006(2) -0.024(3) C21 0.053(3) 0.035(2) 0.028(2) 0.0002(19) 0.013(2) -0.014(2) C22 0.044(2) 0.021(2) 0.025(2) 0.0007(16) 0.0060(17) -0.0050(17) C23 0.042(3) 0.033(2) 0.042(2) 0.009(2) -0.005(2) 0.0040(17) C24 0.047(3) 0.055(3) 0.069(4) 0.030(3) -0.014(2) 0.002(2) C25 0.056(3) 0.037(3) 0.076(4) 0.001(2) 0.013(3) 0.000(2) C26 0.049(3) 0.031(2) 0.042(3) 0.0058(19) 0.017(2) 0.0028(19) C27 0.041(3) 0.052(3) 0.080(4) -0.022(3) 0.011(3) 0.004(2) C28 0.058(3) 0.040(2) 0.055(3) 0.000(2) -0.021(3) 0.011(2) C29 0.043(3) 0.047(3) 0.062(3) -0.037(3) -0.006(2) 0.006(2) C30 0.058(4) 0.064(3) 0.026(2) -0.020(2) 0.008(2) -0.014(2) C31 0.044(3) 0.032(2) 0.038(2) -0.0103(19) -0.0046(19) -0.0100(18) C32 0.0916(17) 0.0557(14) 0.0786(17) 0.0045(13) -0.0425(15) -0.0132(13) C33 0.0916(17) 0.0557(14) 0.0786(17) 0.0045(13) -0.0425(15) -0.0132(13) C34 0.0916(17) 0.0557(14) 0.0786(17) 0.0045(13) -0.0425(15) -0.0132(13) C35 0.0916(17) 0.0557(14) 0.0786(17) 0.0045(13) -0.0425(15) -0.0132(13) C36 0.0916(17) 0.0557(14) 0.0786(17) 0.0045(13) -0.0425(15) -0.0132(13) C37 0.0916(17) 0.0557(14) 0.0786(17) 0.0045(13) -0.0425(15) -0.0132(13) O1 0.093(3) 0.038(2) 0.066(2) 0.0107(18) -0.045(2) -0.0027(19) C38 0.0916(17) 0.0557(14) 0.0786(17) 0.0045(13) -0.0425(15) -0.0132(13) C39 0.129(5) 0.029(3) 0.055(3) 0.011(3) -0.028(3) -0.002(3) C40 0.082(4) 0.061(4) 0.040(3) -0.007(3) -0.021(3) 0.039(3) C41 0.068(4) 0.068(4) 0.064(3) -0.019(3) -0.026(3) 0.033(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.042(4) . ? Pd1 C29 2.113(4) . ? Pd1 C30 2.134(4) . ? Pd1 C31 2.204(4) . ? Pd1 Cl1 2.3351(9) . ? N1 C1 1.337(5) . ? N1 C5 1.450(5) . ? N1 C2 1.478(5) . ? N2 C1 1.340(5) . ? N2 C4 1.454(5) . ? N2 C17 1.456(5) . ? C2 C3 1.508(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.499(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C3A H3C 0.9900 . ? C3A H3D 0.9900 . ? C5 C6 1.399(5) . ? C5 C10 1.402(5) . ? C6 C7 1.399(5) . ? C6 C11 1.515(5) . ? C7 C8 1.371(6) . ? C7 H7A 0.9500 . ? C8 C9 1.385(6) . ? C8 H8A 0.9500 . ? C9 C10 1.388(5) . ? C9 H9A 0.9500 . ? C10 C14 1.519(5) . ? C11 C12 1.532(6) . ? C11 C13 1.535(6) . ? C11 H11A 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.515(6) . ? C14 C16 1.521(6) . ? C14 H14A 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C22 1.398(6) . ? C17 C18 1.418(6) . ? C18 C19 1.390(6) . ? C18 C23 1.501(6) . ? C19 C20 1.383(7) . ? C19 H19A 0.9500 . ? C20 C21 1.375(7) . ? C20 H20A 0.9500 . ? C21 C22 1.394(5) . ? C21 H21A 0.9500 . ? C22 C26 1.530(6) . ? C23 C24 1.530(6) . ? C23 C25 1.541(6) . ? C23 H23A 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.514(6) . ? C26 C28 1.541(6) . ? C26 H26A 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.397(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.407(7) . ? C30 H30A 1.0000 . ? C31 C32 1.446(7) . ? C31 H31A 1.0000 . ? C32 C37 1.412(9) . ? C32 C33 1.414(9) . ? C33 C34 1.377(8) . ? C33 H33A 0.9500 . ? C34 C35 1.395(9) . ? C34 H34A 0.9500 . ? C35 C36 1.372(9) . ? C35 H35A 0.9500 . ? C36 C37 1.392(8) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? O1 C39 1.404(7) . ? O1 C40 1.430(6) . ? C38 C39 1.483(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.527(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41D 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 C29 106.22(17) . . ? C1 Pd1 C30 134.64(16) . . ? C29 Pd1 C30 38.42(19) . . ? C1 Pd1 C31 172.34(16) . . ? C29 Pd1 C31 67.98(17) . . ? C30 Pd1 C31 37.82(18) . . ? C1 Pd1 Cl1 91.40(10) . . ? C29 Pd1 Cl1 161.37(13) . . ? C30 Pd1 Cl1 129.01(15) . . ? C31 Pd1 Cl1 94.96(12) . . ? C1 N1 C5 121.2(3) . . ? C1 N1 C2 124.6(3) . . ? C5 N1 C2 113.7(3) . . ? C1 N2 C4 126.0(3) . . ? C1 N2 C17 120.2(3) . . ? C4 N2 C17 113.6(3) . . ? N1 C1 N2 117.1(3) . . ? N1 C1 Pd1 126.1(3) . . ? N2 C1 Pd1 115.6(3) . . ? N1 C2 C3 110.7(3) . . ? N1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C4 C3 C2 111.4(3) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? N2 C4 C3 111.1(4) . . ? N2 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N2 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? H3C C3A H3D 108.0 . . ? C6 C5 C10 122.1(3) . . ? C6 C5 N1 119.3(3) . . ? C10 C5 N1 118.4(3) . . ? C5 C6 C7 116.8(3) . . ? C5 C6 C11 124.0(3) . . ? C7 C6 C11 119.1(3) . . ? C8 C7 C6 121.9(4) . . ? C8 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8A 119.9 . . ? C9 C8 H8A 119.9 . . ? C8 C9 C10 120.5(4) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C9 C10 C5 118.4(3) . . ? C9 C10 C14 118.5(4) . . ? C5 C10 C14 122.9(4) . . ? C6 C11 C12 111.3(3) . . ? C6 C11 C13 112.8(3) . . ? C12 C11 C13 108.5(3) . . ? C6 C11 H11A 108.0 . . ? C12 C11 H11A 108.0 . . ? C13 C11 H11A 108.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C10 114.1(4) . . ? C15 C14 C16 108.9(4) . . ? C10 C14 C16 110.1(3) . . ? C15 C14 H14A 107.9 . . ? C10 C14 H14A 107.9 . . ? C16 C14 H14A 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C22 C17 C18 122.4(4) . . ? C22 C17 N2 118.6(3) . . ? C18 C17 N2 118.9(4) . . ? C19 C18 C17 116.6(4) . . ? C19 C18 C23 120.5(4) . . ? C17 C18 C23 122.9(4) . . ? C20 C19 C18 122.1(4) . . ? C20 C19 H19A 119.0 . . ? C18 C19 H19A 119.0 . . ? C21 C20 C19 119.7(4) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C20 C21 C22 121.5(4) . . ? C20 C21 H21A 119.2 . . ? C22 C21 H21A 119.2 . . ? C21 C22 C17 117.6(4) . . ? C21 C22 C26 119.2(4) . . ? C17 C22 C26 123.0(3) . . ? C18 C23 C24 113.2(4) . . ? C18 C23 C25 109.8(4) . . ? C24 C23 C25 109.9(4) . . ? C18 C23 H23A 107.9 . . ? C24 C23 H23A 107.9 . . ? C25 C23 H23A 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C22 114.8(4) . . ? C27 C26 C28 107.1(4) . . ? C22 C26 C28 110.2(3) . . ? C27 C26 H26A 108.2 . . ? C22 C26 H26A 108.2 . . ? C28 C26 H26A 108.2 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 Pd1 71.6(3) . . ? C30 C29 H29A 116.4 . . ? Pd1 C29 H29A 116.4 . . ? C30 C29 H29B 116.4 . . ? Pd1 C29 H29B 116.4 . . ? H29A C29 H29B 113.4 . . ? C29 C30 C31 118.9(5) . . ? C29 C30 Pd1 70.0(3) . . ? C31 C30 Pd1 73.8(3) . . ? C29 C30 H30A 120.3 . . ? C31 C30 H30A 120.3 . . ? Pd1 C30 H30A 120.3 . . ? C30 C31 C32 124.4(5) . . ? C30 C31 Pd1 68.4(2) . . ? C32 C31 Pd1 120.6(3) . . ? C30 C31 H31A 112.2 . . ? C32 C31 H31A 112.2 . . ? Pd1 C31 H31A 112.2 . . ? C37 C32 C33 117.3(6) . . ? C37 C32 C31 118.7(6) . . ? C33 C32 C31 124.0(6) . . ? C34 C33 C32 121.7(7) . . ? C34 C33 H33A 119.1 . . ? C32 C33 H33A 119.1 . . ? C33 C34 C35 119.2(6) . . ? C33 C34 H34A 120.4 . . ? C35 C34 H34A 120.4 . . ? C36 C35 C34 120.7(6) . . ? C36 C35 H35A 119.7 . . ? C34 C35 H35A 119.6 . . ? C35 C36 C37 120.3(7) . . ? C35 C36 H36A 119.9 . . ? C37 C36 H36A 119.9 . . ? C36 C37 C32 120.6(7) . . ? C36 C37 H37A 119.7 . . ? C32 C37 H37A 119.7 . . ? C39 O1 C40 111.3(4) . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O1 C39 C38 109.7(4) . . ? O1 C39 H39A 109.7 . . ? C38 C39 H39A 109.7 . . ? O1 C39 H39B 109.7 . . ? C38 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? O1 C40 C41 108.7(4) . . ? O1 C40 H40A 109.9 . . ? C41 C40 H40A 109.9 . . ? O1 C40 H40B 109.9 . . ? C41 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41D 109.5 . . ? H41A C41 H41D 109.5 . . ? H41B C41 H41D 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 N2 -169.7(3) . . . . ? C2 N1 C1 N2 1.9(5) . . . . ? C5 N1 C1 Pd1 23.3(5) . . . . ? C2 N1 C1 Pd1 -165.1(3) . . . . ? C4 N2 C1 N1 -3.3(5) . . . . ? C17 N2 C1 N1 171.7(3) . . . . ? C4 N2 C1 Pd1 165.0(3) . . . . ? C17 N2 C1 Pd1 -20.0(4) . . . . ? C29 Pd1 C1 N1 -104.3(3) . . . . ? C30 Pd1 C1 N1 -135.0(3) . . . . ? Cl1 Pd1 C1 N1 69.6(3) . . . . ? C29 Pd1 C1 N2 88.6(3) . . . . ? C30 Pd1 C1 N2 57.9(4) . . . . ? Cl1 Pd1 C1 N2 -97.5(3) . . . . ? C1 N1 C2 C3 24.0(5) . . . . ? C5 N1 C2 C3 -163.9(3) . . . . ? N1 C2 C3 C4 -46.9(5) . . . . ? C1 N2 C4 C3 -21.6(6) . . . . ? C17 N2 C4 C3 163.2(4) . . . . ? C2 C3 C4 N2 45.8(6) . . . . ? C1 N1 C5 C6 -111.7(4) . . . . ? C2 N1 C5 C6 75.8(4) . . . . ? C1 N1 C5 C10 73.5(4) . . . . ? C2 N1 C5 C10 -99.0(4) . . . . ? C10 C5 C6 C7 -1.5(5) . . . . ? N1 C5 C6 C7 -176.1(3) . . . . ? C10 C5 C6 C11 176.4(3) . . . . ? N1 C5 C6 C11 1.9(5) . . . . ? C5 C6 C7 C8 -0.5(6) . . . . ? C11 C6 C7 C8 -178.6(4) . . . . ? C6 C7 C8 C9 2.1(6) . . . . ? C7 C8 C9 C10 -1.6(6) . . . . ? C8 C9 C10 C5 -0.3(5) . . . . ? C8 C9 C10 C14 174.9(4) . . . . ? C6 C5 C10 C9 1.9(5) . . . . ? N1 C5 C10 C9 176.5(3) . . . . ? C6 C5 C10 C14 -173.2(3) . . . . ? N1 C5 C10 C14 1.5(5) . . . . ? C5 C6 C11 C12 -104.2(4) . . . . ? C7 C6 C11 C12 73.7(5) . . . . ? C5 C6 C11 C13 133.6(4) . . . . ? C7 C6 C11 C13 -48.5(5) . . . . ? C9 C10 C14 C15 39.8(5) . . . . ? C5 C10 C14 C15 -145.1(4) . . . . ? C9 C10 C14 C16 -82.9(5) . . . . ? C5 C10 C14 C16 92.1(5) . . . . ? C1 N2 C17 C22 -87.7(4) . . . . ? C4 N2 C17 C22 87.8(4) . . . . ? C1 N2 C17 C18 97.0(4) . . . . ? C4 N2 C17 C18 -87.4(4) . . . . ? C22 C17 C18 C19 3.6(6) . . . . ? N2 C17 C18 C19 178.7(3) . . . . ? C22 C17 C18 C23 -172.9(4) . . . . ? N2 C17 C18 C23 2.2(5) . . . . ? C17 C18 C19 C20 -0.8(6) . . . . ? C23 C18 C19 C20 175.8(4) . . . . ? C18 C19 C20 C21 -1.2(7) . . . . ? C19 C20 C21 C22 0.5(7) . . . . ? C20 C21 C22 C17 2.1(6) . . . . ? C20 C21 C22 C26 -173.1(4) . . . . ? C18 C17 C22 C21 -4.2(6) . . . . ? N2 C17 C22 C21 -179.3(3) . . . . ? C18 C17 C22 C26 170.8(4) . . . . ? N2 C17 C22 C26 -4.3(6) . . . . ? C19 C18 C23 C24 46.7(5) . . . . ? C17 C18 C23 C24 -136.9(4) . . . . ? C19 C18 C23 C25 -76.6(5) . . . . ? C17 C18 C23 C25 99.8(5) . . . . ? C21 C22 C26 C27 -43.5(6) . . . . ? C17 C22 C26 C27 141.6(4) . . . . ? C21 C22 C26 C28 77.6(5) . . . . ? C17 C22 C26 C28 -97.4(5) . . . . ? C1 Pd1 C29 C30 -144.2(3) . . . . ? C31 Pd1 C29 C30 30.5(3) . . . . ? Cl1 Pd1 C29 C30 55.3(7) . . . . ? Pd1 C29 C30 C31 -57.3(4) . . . . ? C1 Pd1 C30 C29 52.2(4) . . . . ? C31 Pd1 C30 C29 -129.8(5) . . . . ? Cl1 Pd1 C30 C29 -160.3(3) . . . . ? C1 Pd1 C30 C31 -178.0(2) . . . . ? C29 Pd1 C30 C31 129.8(5) . . . . ? Cl1 Pd1 C30 C31 -30.4(4) . . . . ? C29 C30 C31 C32 168.6(5) . . . . ? Pd1 C30 C31 C32 113.1(5) . . . . ? C29 C30 C31 Pd1 55.5(4) . . . . ? C29 Pd1 C31 C30 -31.0(3) . . . . ? Cl1 Pd1 C31 C30 156.7(3) . . . . ? C29 Pd1 C31 C32 -149.1(5) . . . . ? C30 Pd1 C31 C32 -118.2(6) . . . . ? Cl1 Pd1 C31 C32 38.6(4) . . . . ? C30 C31 C32 C37 -176.5(5) . . . . ? Pd1 C31 C32 C37 -93.0(6) . . . . ? C30 C31 C32 C33 1.3(9) . . . . ? Pd1 C31 C32 C33 84.8(7) . . . . ? C37 C32 C33 C34 -2.5(9) . . . . ? C31 C32 C33 C34 179.7(5) . . . . ? C32 C33 C34 C35 5.0(9) . . . . ? C33 C34 C35 C36 -5.3(9) . . . . ? C34 C35 C36 C37 3.2(10) . . . . ? C35 C36 C37 C32 -0.6(10) . . . . ? C33 C32 C37 C36 0.2(9) . . . . ? C31 C32 C37 C36 178.2(5) . . . . ? C40 O1 C39 C38 178.9(5) . . . . ? C39 O1 C40 C41 -179.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.375 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.083 data_Pd5M _database_code_depnum_ccdc_archive 'CCDC 784541' #TrackingRef 'Pd5M.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H33 Cl N2 Pd' _chemical_formula_sum 'C30 H33 Cl N2 Pd' _chemical_formula_weight 563.43 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' 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' N N 0.0061 0.0033 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2603(4) _cell_length_b 10.4211(5) _cell_length_c 16.2545(7) _cell_angle_alpha 95.6490(10) _cell_angle_beta 90.1730(10) _cell_angle_gamma 103.6930(10) _cell_volume 1352.34(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9925 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 32.63 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_T_max 0.923 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 SMART APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15097 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6493 _reflns_number_gt 6045 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_data_reduction 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_structure_solution 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_publication_material 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0297P)^2^+0.5995P] 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 6493 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0232 _refine_ls_R_factor_gt 0.0207 _refine_ls_wR_factor_ref 0.0538 _refine_ls_wR_factor_gt 0.0521 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.003 _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 0.751273(9) 0.070256(7) 0.810731(5) 0.01264(2) Uani 1 1 d . . . Cl1 Cl 0.92668(3) -0.07309(3) 0.771907(17) 0.02073(6) Uani 1 1 d . . . N1 N 0.82984(11) 0.25214(9) 0.67102(6) 0.0168(2) Uani 1 1 d . . . C1 C 0.75301(12) 0.13330(10) 0.69682(6) 0.0144(2) Uani 1 1 d . . . N2 N 0.68542(11) 0.05911(9) 0.62606(5) 0.01601(19) Uani 1 1 d . . . C2 C 0.81119(16) 0.25126(12) 0.58613(7) 0.0240(3) Uani 1 1 d . . . H2A H 0.8547 0.3226 0.5541 0.029 Uiso 1 1 calc R . . C3 C 0.72004(16) 0.13063(12) 0.55789(7) 0.0237(3) Uani 1 1 d . . . H3A H 0.6858 0.1000 0.5021 0.028 Uiso 1 1 calc R . . C4 C 0.91317(13) 0.36763(10) 0.72460(6) 0.0158(2) Uani 1 1 d . . . C5 C 1.07568(13) 0.37751(10) 0.75211(7) 0.0162(2) Uani 1 1 d . . . C6 C 1.15457(14) 0.49213(11) 0.80181(7) 0.0195(2) Uani 1 1 d . . . H6A H 1.2651 0.5007 0.8220 0.023 Uiso 1 1 calc R . . C7 C 1.07518(15) 0.59462(11) 0.82272(7) 0.0211(2) Uani 1 1 d . . . C8 C 0.91392(15) 0.58118(11) 0.79248(8) 0.0226(3) Uani 1 1 d . . . H8A H 0.8599 0.6513 0.8055 0.027 Uiso 1 1 calc R . . C9 C 0.82956(14) 0.46807(11) 0.74375(7) 0.0198(2) Uani 1 1 d . . . C10 C 1.16477(14) 0.26991(11) 0.72685(8) 0.0214(2) Uani 1 1 d . . . H10A H 1.1043 0.1865 0.7468 0.032 Uiso 1 1 calc R . . H10B H 1.2782 0.2950 0.7509 0.032 Uiso 1 1 calc R . . H10C H 1.1698 0.2582 0.6664 0.032 Uiso 1 1 calc R . . C11 C 1.16147(18) 0.71819(13) 0.87638(9) 0.0336(3) Uani 1 1 d . . . H11A H 1.2383 0.6959 0.9156 0.050 Uiso 1 1 calc R . . H11B H 1.0782 0.7556 0.9068 0.050 Uiso 1 1 calc R . . H11C H 1.2240 0.7835 0.8416 0.050 Uiso 1 1 calc R . . C12 C 0.65282(15) 0.45446(13) 0.71353(10) 0.0321(3) Uani 1 1 d . . . H12A H 0.6157 0.5343 0.7336 0.048 Uiso 1 1 calc R . . H12B H 0.5799 0.3767 0.7345 0.048 Uiso 1 1 calc R . . H12C H 0.6481 0.4436 0.6529 0.048 Uiso 1 1 calc R . . C13 C 0.58137(13) -0.07398(10) 0.62082(6) 0.0159(2) Uani 1 1 d . . . C14 C 0.41991(14) -0.09242(11) 0.65043(7) 0.0174(2) Uani 1 1 d . . . C15 C 0.31782(14) -0.22108(11) 0.64101(7) 0.0199(2) Uani 1 1 d . . . H15A H 0.2084 -0.2366 0.6620 0.024 Uiso 1 1 calc R . . C16 C 0.37298(15) -0.32645(11) 0.60164(7) 0.0218(3) Uani 1 1 d . . . C17 C 0.53455(16) -0.30324(11) 0.57306(7) 0.0234(3) Uani 1 1 d . . . H17A H 0.5725 -0.3755 0.5463 0.028 Uiso 1 1 calc R . . C18 C 0.64280(14) -0.17784(11) 0.58222(7) 0.0205(2) Uani 1 1 d . . . C19 C 0.35212(15) 0.02118(12) 0.68725(8) 0.0256(3) Uani 1 1 d . . . H19A H 0.3791 0.0940 0.6520 0.038 Uiso 1 1 calc R . . H19B H 0.4021 0.0519 0.7426 0.038 Uiso 1 1 calc R . . H19C H 0.2308 -0.0082 0.6912 0.038 Uiso 1 1 calc R . . C20 C 0.25810(18) -0.46318(12) 0.58788(8) 0.0307(3) Uani 1 1 d . . . H20A H 0.1547 -0.4640 0.6175 0.046 Uiso 1 1 calc R . . H20B H 0.3127 -0.5280 0.6086 0.046 Uiso 1 1 calc R . . H20C H 0.2323 -0.4864 0.5286 0.046 Uiso 1 1 calc R . . C21 C 0.81875(16) -0.15658(13) 0.55205(9) 0.0302(3) Uani 1 1 d . . . H21A H 0.8417 -0.2425 0.5330 0.045 Uiso 1 1 calc R . . H21B H 0.8970 -0.1127 0.5973 0.045 Uiso 1 1 calc R . . H21C H 0.8318 -0.1007 0.5063 0.045 Uiso 1 1 calc R . . C22 C 0.61557(15) 0.19143(12) 0.87841(7) 0.0224(2) Uani 1 1 d . . . H22A H 0.6819 0.2705 0.9124 0.027 Uiso 1 1 calc R . . H22B H 0.5183 0.2084 0.8494 0.027 Uiso 1 1 calc R . . C23 C 0.59024(14) 0.06889(12) 0.91312(7) 0.0214(2) Uani 1 1 d . . . H23A H 0.4774 0.0066 0.9104 0.026 Uiso 1 1 calc R . . C24 C 0.72940(14) 0.02946(11) 0.94182(7) 0.0187(2) Uani 1 1 d . . . H24A H 0.8040 0.1004 0.9798 0.022 Uiso 1 1 calc R . . C25 C 0.72418(13) -0.10545(11) 0.96425(7) 0.0184(2) Uani 1 1 d . . . C26 C 0.62689(15) -0.21874(12) 0.91974(7) 0.0230(3) Uani 1 1 d . . . H26A H 0.5609 -0.2100 0.8736 0.028 Uiso 1 1 calc R . . C27 C 0.62526(16) -0.34418(13) 0.94208(8) 0.0287(3) Uani 1 1 d . . . H27A H 0.5564 -0.4205 0.9120 0.034 Uiso 1 1 calc R . . C28 C 0.72381(17) -0.35833(13) 1.00809(9) 0.0309(3) Uani 1 1 d . . . H28A H 0.7241 -0.4443 1.0227 0.037 Uiso 1 1 calc R . . C29 C 0.82193(15) -0.24672(13) 1.05274(8) 0.0273(3) Uani 1 1 d . . . H29A H 0.8896 -0.2562 1.0981 0.033 Uiso 1 1 calc R . . C30 C 0.82154(14) -0.12054(12) 1.03126(7) 0.0221(3) Uani 1 1 d . . . H30A H 0.8880 -0.0443 1.0625 0.026 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 0.01437(3) 0.01260(3) 0.01149(3) 0.00172(3) 0.00132(3) 0.00411(3) Cl1 0.02297(11) 0.01881(11) 0.02372(12) 0.00503(9) 0.00596(10) 0.01034(9) N1 0.0192(4) 0.0137(4) 0.0165(4) 0.0033(3) -0.0021(3) 0.0010(3) C1 0.0135(4) 0.0136(4) 0.0157(5) 0.0007(4) 0.0007(4) 0.0029(4) N2 0.0179(4) 0.0155(4) 0.0131(4) 0.0019(3) 0.0004(3) 0.0007(3) C2 0.0301(6) 0.0223(5) 0.0169(5) 0.0086(4) -0.0022(4) -0.0017(5) C3 0.0285(6) 0.0251(5) 0.0143(5) 0.0059(4) -0.0018(4) -0.0016(5) C4 0.0180(5) 0.0125(4) 0.0159(5) 0.0035(4) -0.0008(4) 0.0009(4) C5 0.0177(5) 0.0136(4) 0.0178(5) 0.0039(4) 0.0012(4) 0.0037(4) C6 0.0178(5) 0.0174(5) 0.0228(5) 0.0025(4) -0.0034(4) 0.0034(4) C7 0.0249(5) 0.0146(5) 0.0227(5) -0.0001(4) -0.0025(4) 0.0032(4) C8 0.0236(5) 0.0157(5) 0.0301(6) 0.0023(4) 0.0004(5) 0.0077(4) C9 0.0165(5) 0.0164(5) 0.0270(5) 0.0058(4) -0.0016(4) 0.0039(4) C10 0.0195(5) 0.0163(5) 0.0293(6) 0.0021(4) 0.0020(4) 0.0062(4) C11 0.0355(7) 0.0229(6) 0.0398(7) -0.0092(5) -0.0113(6) 0.0068(5) C12 0.0206(5) 0.0248(6) 0.0519(8) 0.0048(5) -0.0087(6) 0.0074(4) C13 0.0185(5) 0.0148(4) 0.0123(4) 0.0009(4) -0.0012(4) 0.0003(4) C14 0.0191(5) 0.0172(5) 0.0151(5) 0.0007(4) -0.0006(4) 0.0031(4) C15 0.0202(5) 0.0208(5) 0.0168(5) 0.0035(4) 0.0018(4) 0.0002(4) C16 0.0306(6) 0.0159(5) 0.0167(5) 0.0032(4) -0.0007(4) 0.0004(4) C17 0.0307(6) 0.0181(5) 0.0207(5) -0.0025(4) 0.0010(5) 0.0065(4) C18 0.0220(5) 0.0218(5) 0.0169(5) -0.0010(4) 0.0020(4) 0.0048(4) C19 0.0192(5) 0.0233(5) 0.0332(6) -0.0056(5) 0.0024(5) 0.0063(4) C20 0.0402(7) 0.0178(5) 0.0292(6) 0.0027(5) 0.0016(6) -0.0033(5) C21 0.0249(6) 0.0314(6) 0.0318(6) -0.0075(5) 0.0073(5) 0.0059(5) C22 0.0279(5) 0.0262(5) 0.0174(5) -0.0001(4) 0.0033(4) 0.0157(4) C23 0.0237(5) 0.0281(5) 0.0148(5) 0.0014(4) 0.0065(4) 0.0109(4) C24 0.0223(5) 0.0220(5) 0.0122(4) 0.0012(4) 0.0021(4) 0.0060(4) C25 0.0170(5) 0.0242(5) 0.0156(5) 0.0064(4) 0.0054(4) 0.0064(4) C26 0.0201(5) 0.0278(6) 0.0202(5) 0.0048(4) 0.0014(4) 0.0029(4) C27 0.0279(6) 0.0242(6) 0.0308(6) 0.0051(5) 0.0030(5) -0.0012(5) C28 0.0319(6) 0.0264(6) 0.0373(7) 0.0162(5) 0.0073(5) 0.0074(5) C29 0.0237(5) 0.0348(6) 0.0263(6) 0.0143(5) 0.0012(5) 0.0083(5) C30 0.0201(5) 0.0285(5) 0.0180(5) 0.0061(4) 0.0027(4) 0.0053(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.0237(11) . ? Pd1 C22 2.1131(12) . ? Pd1 C23 2.1328(11) . ? Pd1 C24 2.2131(11) . ? Pd1 Cl1 2.3609(3) . ? N1 C1 1.3580(13) . ? N1 C2 1.3869(14) . ? N1 C4 1.4418(13) . ? C1 N2 1.3598(13) . ? N2 C3 1.3887(14) . ? N2 C13 1.4427(13) . ? C2 C3 1.3394(16) . ? C2 H2A 0.9500 . ? C3 H3A 0.9500 . ? C4 C9 1.3960(16) . ? C4 C5 1.3908(15) . ? C5 C6 1.3937(14) . ? C5 C10 1.5065(16) . ? C6 C7 1.3956(17) . ? C6 H6A 0.9500 . ? C7 C8 1.3891(17) . ? C7 C11 1.5060(16) . ? C8 C9 1.3880(15) . ? C8 H8A 0.9500 . ? C9 C12 1.5089(17) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.3958(15) . ? C13 C18 1.3967(16) . ? C14 C15 1.3985(15) . ? C14 C19 1.4998(16) . ? C15 C16 1.3867(17) . ? C15 H15A 0.9500 . ? C16 C17 1.3888(17) . ? C16 C20 1.5088(16) . ? C17 C18 1.3919(16) . ? C17 H17A 0.9500 . ? C18 C21 1.5084(17) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.4174(17) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.4021(17) . ? C23 H23A 1.0000 . ? C24 C25 1.4777(16) . ? C24 H24A 1.0000 . ? C25 C26 1.3937(16) . ? C25 C30 1.3950(16) . ? C26 C27 1.3879(18) . ? C26 H26A 0.9500 . ? C27 C28 1.3852(19) . ? C27 H27A 0.9500 . ? C28 C29 1.3857(18) . ? C28 H28A 0.9500 . ? C29 C30 1.3941(18) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 C22 102.16(4) . . ? C1 Pd1 C23 134.42(4) . . ? C22 Pd1 C23 39.00(5) . . ? C1 Pd1 C24 170.25(4) . . ? C22 Pd1 C24 68.16(4) . . ? C23 Pd1 C24 37.59(4) . . ? C1 Pd1 Cl1 92.83(3) . . ? C22 Pd1 Cl1 164.22(3) . . ? C23 Pd1 Cl1 129.28(3) . . ? C24 Pd1 Cl1 96.73(3) . . ? C1 N1 C2 111.37(9) . . ? C1 N1 C4 124.97(9) . . ? C2 N1 C4 123.58(9) . . ? N2 C1 N1 103.78(9) . . ? N2 C1 Pd1 126.41(7) . . ? N1 C1 Pd1 129.63(7) . . ? C1 N2 C3 111.38(9) . . ? C1 N2 C13 125.63(9) . . ? C3 N2 C13 122.87(9) . . ? C3 C2 N1 106.86(10) . . ? C3 C2 H2A 126.6 . . ? N1 C2 H2A 126.6 . . ? C2 C3 N2 106.60(10) . . ? C2 C3 H3A 126.7 . . ? N2 C3 H3A 126.7 . . ? C9 C4 C5 122.58(9) . . ? C9 C4 N1 118.36(10) . . ? C5 C4 N1 118.99(10) . . ? C6 C5 C4 117.62(10) . . ? C6 C5 C10 121.28(10) . . ? C4 C5 C10 121.07(9) . . ? C7 C6 C5 121.62(11) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C6 C7 C8 118.63(10) . . ? C6 C7 C11 121.25(11) . . ? C8 C7 C11 120.12(11) . . ? C9 C8 C7 121.79(11) . . ? C9 C8 H8A 119.1 . . ? C7 C8 H8A 119.1 . . ? C8 C9 C4 117.76(10) . . ? C8 C9 C12 120.73(11) . . ? C4 C9 C12 121.51(10) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 122.70(10) . . ? C14 C13 N2 118.47(10) . . ? C18 C13 N2 118.73(10) . . ? C13 C14 C15 117.73(10) . . ? C13 C14 C19 122.16(9) . . ? C15 C14 C19 120.04(10) . . ? C16 C15 C14 121.35(11) . . ? C16 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C15 C16 C17 118.84(10) . . ? C15 C16 C20 120.66(11) . . ? C17 C16 C20 120.48(11) . . ? C16 C17 C18 122.30(11) . . ? C16 C17 H17A 118.8 . . ? C18 C17 H17A 118.8 . . ? C17 C18 C13 117.05(11) . . ? C17 C18 C21 120.96(11) . . ? C13 C18 C21 121.99(10) . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 Pd1 71.25(7) . . ? C23 C22 H22A 116.5 . . ? Pd1 C22 H22A 116.5 . . ? C23 C22 H22B 116.5 . . ? Pd1 C22 H22B 116.5 . . ? H22A C22 H22B 113.5 . . ? C24 C23 C22 118.70(10) . . ? C24 C23 Pd1 74.32(7) . . ? C22 C23 Pd1 69.75(6) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? Pd1 C23 H23A 120.4 . . ? C23 C24 C25 123.87(10) . . ? C23 C24 Pd1 68.10(6) . . ? C25 C24 Pd1 119.87(7) . . ? C23 C24 H24A 112.6 . . ? C25 C24 H24A 112.6 . . ? Pd1 C24 H24A 112.6 . . ? C26 C25 C30 118.72(11) . . ? C26 C25 C24 122.09(10) . . ? C30 C25 C24 119.19(10) . . ? C27 C26 C25 120.74(11) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 120.15(11) . . ? C26 C27 H27A 119.9 . . ? C28 C27 H27A 119.9 . . ? C27 C28 C29 119.82(12) . . ? C27 C28 H28A 120.1 . . ? C29 C28 H28A 120.1 . . ? C28 C29 C30 120.10(12) . . ? C28 C29 H29A 119.9 . . ? C30 C29 H29A 119.9 . . ? C29 C30 C25 120.45(11) . . ? C29 C30 H30A 119.8 . . ? C25 C30 H30A 119.8 . . ? 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 C2 N1 C1 N2 -0.39(13) . . . . ? C4 N1 C1 N2 176.56(10) . . . . ? C2 N1 C1 Pd1 174.91(9) . . . . ? C4 N1 C1 Pd1 -8.13(16) . . . . ? C22 Pd1 C1 N2 -118.26(10) . . . . ? C23 Pd1 C1 N2 -92.68(11) . . . . ? Cl1 Pd1 C1 N2 66.70(9) . . . . ? C22 Pd1 C1 N1 67.41(11) . . . . ? C23 Pd1 C1 N1 92.99(11) . . . . ? Cl1 Pd1 C1 N1 -107.63(10) . . . . ? N1 C1 N2 C3 0.09(13) . . . . ? Pd1 C1 N2 C3 -175.41(8) . . . . ? N1 C1 N2 C13 -176.08(10) . . . . ? Pd1 C1 N2 C13 8.41(16) . . . . ? C1 N1 C2 C3 0.55(14) . . . . ? C4 N1 C2 C3 -176.45(11) . . . . ? N1 C2 C3 N2 -0.46(14) . . . . ? C1 N2 C3 C2 0.24(14) . . . . ? C13 N2 C3 C2 176.54(11) . . . . ? C1 N1 C4 C9 -100.97(13) . . . . ? C2 N1 C4 C9 75.62(14) . . . . ? C1 N1 C4 C5 81.88(14) . . . . ? C2 N1 C4 C5 -101.53(13) . . . . ? C9 C4 C5 C6 1.11(16) . . . . ? N1 C4 C5 C6 178.13(10) . . . . ? C9 C4 C5 C10 -177.05(10) . . . . ? N1 C4 C5 C10 -0.03(15) . . . . ? C4 C5 C6 C7 -0.79(17) . . . . ? C10 C5 C6 C7 177.36(11) . . . . ? C5 C6 C7 C8 -0.36(18) . . . . ? C5 C6 C7 C11 -179.93(11) . . . . ? C6 C7 C8 C9 1.29(18) . . . . ? C11 C7 C8 C9 -179.14(12) . . . . ? C7 C8 C9 C4 -0.99(18) . . . . ? C7 C8 C9 C12 178.39(12) . . . . ? C5 C4 C9 C8 -0.24(17) . . . . ? N1 C4 C9 C8 -177.28(10) . . . . ? C5 C4 C9 C12 -179.62(11) . . . . ? N1 C4 C9 C12 3.34(16) . . . . ? C1 N2 C13 C14 70.80(15) . . . . ? C3 N2 C13 C14 -104.96(13) . . . . ? C1 N2 C13 C18 -112.75(12) . . . . ? C3 N2 C13 C18 71.49(15) . . . . ? C18 C13 C14 C15 0.47(16) . . . . ? N2 C13 C14 C15 176.77(10) . . . . ? C18 C13 C14 C19 -176.32(11) . . . . ? N2 C13 C14 C19 -0.03(16) . . . . ? C13 C14 C15 C16 -1.71(17) . . . . ? C19 C14 C15 C16 175.16(11) . . . . ? C14 C15 C16 C17 1.63(17) . . . . ? C14 C15 C16 C20 -176.65(11) . . . . ? C15 C16 C17 C18 -0.29(18) . . . . ? C20 C16 C17 C18 178.00(12) . . . . ? C16 C17 C18 C13 -0.89(18) . . . . ? C16 C17 C18 C21 178.71(12) . . . . ? C14 C13 C18 C17 0.79(17) . . . . ? N2 C13 C18 C17 -175.50(10) . . . . ? C14 C13 C18 C21 -178.80(11) . . . . ? N2 C13 C18 C21 4.91(17) . . . . ? C1 Pd1 C22 C23 150.66(7) . . . . ? C24 Pd1 C22 C23 -30.50(6) . . . . ? Cl1 Pd1 C22 C23 -47.87(15) . . . . ? Pd1 C22 C23 C24 57.96(9) . . . . ? C1 Pd1 C23 C24 -171.56(6) . . . . ? C22 Pd1 C23 C24 -129.44(10) . . . . ? Cl1 Pd1 C23 C24 35.47(8) . . . . ? C1 Pd1 C23 C22 -42.12(9) . . . . ? C24 Pd1 C23 C22 129.44(10) . . . . ? Cl1 Pd1 C23 C22 164.90(5) . . . . ? C22 C23 C24 C25 -167.83(10) . . . . ? Pd1 C23 C24 C25 -112.13(10) . . . . ? C22 C23 C24 Pd1 -55.70(9) . . . . ? C22 Pd1 C24 C23 31.58(7) . . . . ? Cl1 Pd1 C24 C23 -153.11(6) . . . . ? C22 Pd1 C24 C25 149.08(10) . . . . ? C23 Pd1 C24 C25 117.50(11) . . . . ? Cl1 Pd1 C24 C25 -35.61(9) . . . . ? C23 C24 C25 C26 38.02(17) . . . . ? Pd1 C24 C25 C26 -44.36(14) . . . . ? C23 C24 C25 C30 -143.04(11) . . . . ? Pd1 C24 C25 C30 134.58(9) . . . . ? C30 C25 C26 C27 0.71(17) . . . . ? C24 C25 C26 C27 179.66(11) . . . . ? C25 C26 C27 C28 -1.48(19) . . . . ? C26 C27 C28 C29 1.1(2) . . . . ? C27 C28 C29 C30 0.0(2) . . . . ? C28 C29 C30 C25 -0.73(19) . . . . ? C26 C25 C30 C29 0.39(17) . . . . ? C24 C25 C30 C29 -178.59(11) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.547 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.058 data_KE248 _database_code_depnum_ccdc_archive 'CCDC 784542' #TrackingRef 'kE248.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H51 Cl N2 Pd' _chemical_formula_sum 'C38 H51 Cl N2 Pd' _chemical_formula_weight 677.66 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 Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.8782(17) _cell_length_b 15.5946(10) _cell_length_c 19.7653(12) _cell_angle_alpha 90.00 _cell_angle_beta 113.9140(10) _cell_angle_gamma 90.00 _cell_volume 7855.3(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 655 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2848 _exptl_absorpt_coefficient_mu 0.565 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 SMART APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33825 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6896 _reflns_number_gt 4488 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_data_reduction 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_structure_solution 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_publication_material 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0376P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6896 _refine_ls_number_parameters 426 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.0839 _refine_ls_wR_factor_gt 0.0782 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.013 _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 0.156808(10) 0.944860(18) 0.112457(13) 0.04318(10) Uani 1 1 d . . . Cl1 Cl 0.22350(3) 0.84202(6) 0.16650(5) 0.0531(2) Uani 1 1 d . A . N1 N 0.15839(9) 1.01939(16) 0.24938(13) 0.0374(6) Uani 1 1 d . . . N2 N 0.23016(9) 1.06449(16) 0.22717(12) 0.0363(6) Uani 1 1 d . . . C1 C 0.18502(12) 1.0208(2) 0.20529(15) 0.0365(8) Uani 1 1 d . A . C2 C 0.17793(12) 1.0392(2) 0.32962(16) 0.0531(10) Uani 1 1 d . A . H2A H 0.1571 1.0060 0.3509 0.064 Uiso 1 1 calc R . . H2B H 0.1719 1.1008 0.3354 0.064 Uiso 1 1 calc R . . C3 C 0.23436(14) 1.0201(3) 0.37251(18) 0.0640(11) Uani 1 1 d . . . H3A H 0.2435 0.9658 0.3547 0.077 Uiso 1 1 calc R A . H3B H 0.2413 1.0129 0.4254 0.077 Uiso 1 1 calc R . . C4 C 0.26837(14) 1.0929(3) 0.36401(19) 0.0594(10) Uani 1 1 d . A . H4A H 0.2710 1.1389 0.3998 0.071 Uiso 1 1 calc R . . H4B H 0.3042 1.0709 0.3758 0.071 Uiso 1 1 calc R . . C5 C 0.24663(12) 1.1295(2) 0.28769(16) 0.0442(8) Uani 1 1 d . A . H5A H 0.2160 1.1656 0.2815 0.053 Uiso 1 1 calc R . . H5B H 0.2735 1.1671 0.2824 0.053 Uiso 1 1 calc R . . C6 C 0.10322(12) 0.9937(2) 0.21713(16) 0.0410(8) Uani 1 1 d . A . C7 C 0.06551(12) 1.0581(2) 0.18965(17) 0.0454(8) Uani 1 1 d . . . C8 C 0.01275(13) 1.0337(3) 0.15997(19) 0.0571(10) Uani 1 1 d . A . H8A H -0.0138 1.0761 0.1404 0.069 Uiso 1 1 calc R . . C9 C -0.00132(13) 0.9485(3) 0.15875(19) 0.0628(10) Uani 1 1 d . . . H9A H -0.0373 0.9327 0.1376 0.075 Uiso 1 1 calc R A . C10 C 0.03679(14) 0.8865(2) 0.18814(19) 0.0558(10) Uani 1 1 d . A . H10A H 0.0265 0.8283 0.1873 0.067 Uiso 1 1 calc R . . C11 C 0.08985(13) 0.9070(2) 0.21895(17) 0.0474(9) Uani 1 1 d . . . C12 C 0.07936(12) 1.1530(2) 0.19247(19) 0.0507(9) Uani 1 1 d . A . H12A H 0.1172 1.1569 0.2009 0.061 Uiso 1 1 calc R . . C13 C 0.07355(12) 1.1967(2) 0.2578(2) 0.0676(11) Uani 1 1 d . . . H13A H 0.0828 1.1561 0.2990 0.101 Uiso 1 1 calc R A . H13B H 0.0372 1.2155 0.2430 0.101 Uiso 1 1 calc RD . . H13C H 0.0970 1.2465 0.2733 0.101 Uiso 1 1 calc R . . C14 C 0.04790(14) 1.2009(2) 0.1214(2) 0.0679(11) Uani 1 1 d . . . H14A H 0.0513 1.1717 0.0797 0.102 Uiso 1 1 calc R A . H14B H 0.0612 1.2597 0.1251 0.102 Uiso 1 1 calc R . . H14C H 0.0109 1.2022 0.1136 0.102 Uiso 1 1 calc R . . C15 C 0.13048(14) 0.8383(2) 0.25684(19) 0.0536(9) Uani 1 1 d . A . H15A H 0.1659 0.8619 0.2658 0.064 Uiso 1 1 calc R . . C16 C 0.12233(16) 0.7563(2) 0.2115(2) 0.0728(12) Uani 1 1 d . . . H16A H 0.1214 0.7701 0.1626 0.109 Uiso 1 1 calc R A . H16B H 0.0891 0.7297 0.2057 0.109 Uiso 1 1 calc R . . H16C H 0.1513 0.7165 0.2370 0.109 Uiso 1 1 calc R . . C17 C 0.12936(18) 0.8169(3) 0.3319(2) 0.0828(14) Uani 1 1 d . . . H17A H 0.1350 0.8693 0.3614 0.124 Uiso 1 1 calc R A . H17B H 0.1572 0.7755 0.3581 0.124 Uiso 1 1 calc R . . H17C H 0.0952 0.7921 0.3241 0.124 Uiso 1 1 calc R . . C18 C 0.25832(12) 1.0698(2) 0.17957(16) 0.0400(8) Uani 1 1 d . A . C19 C 0.30595(13) 1.0263(2) 0.19964(18) 0.0440(8) Uani 1 1 d . . . C20 C 0.33245(15) 1.0352(2) 0.1531(2) 0.0583(10) Uani 1 1 d . A . H20A H 0.3649 1.0063 0.1656 0.070 Uiso 1 1 calc R . . C21 C 0.31316(17) 1.0843(3) 0.0903(2) 0.0646(11) Uani 1 1 d . . . H21A H 0.3317 1.0885 0.0593 0.077 Uiso 1 1 calc R A . C22 C 0.26664(16) 1.1275(2) 0.0727(2) 0.0566(10) Uani 1 1 d . A . H22A H 0.2532 1.1612 0.0290 0.068 Uiso 1 1 calc R . . C23 C 0.23847(13) 1.1235(2) 0.11710(17) 0.0441(8) Uani 1 1 d . . . C24 C 0.33168(13) 0.9757(2) 0.27052(19) 0.0507(9) Uani 1 1 d . A . H24A H 0.3046 0.9644 0.2905 0.061 Uiso 1 1 calc R . . C25 C 0.37603(13) 1.0274(3) 0.3285(2) 0.0667(11) Uani 1 1 d . . . H25A H 0.3626 1.0834 0.3352 0.100 Uiso 1 1 calc R A . H25B H 0.4044 1.0355 0.3118 0.100 Uiso 1 1 calc R . . H25C H 0.3895 0.9963 0.3756 0.100 Uiso 1 1 calc R . . C26 C 0.35375(15) 0.8888(2) 0.2598(2) 0.0711(12) Uani 1 1 d . . . H26A H 0.3255 0.8544 0.2238 0.107 Uiso 1 1 calc R A . H26B H 0.3687 0.8583 0.3072 0.107 Uiso 1 1 calc R . . H26C H 0.3812 0.8983 0.2415 0.107 Uiso 1 1 calc R . . C27 C 0.19126(13) 1.1816(2) 0.09950(17) 0.0480(9) Uani 1 1 d . A . H27A H 0.1699 1.1591 0.1258 0.058 Uiso 1 1 calc R . . C28 C 0.20980(15) 1.2727(2) 0.1279(2) 0.0645(11) Uani 1 1 d . . . H28A H 0.1794 1.3110 0.1133 0.097 Uiso 1 1 calc R A . H28B H 0.2339 1.2933 0.1067 0.097 Uiso 1 1 calc R . . H28C H 0.2279 1.2717 0.1820 0.097 Uiso 1 1 calc R . . C29 C 0.15606(17) 1.1877(3) 0.0170(2) 0.0837(14) Uani 1 1 d . . . H29A H 0.1515 1.1306 -0.0054 0.126 Uiso 1 1 calc R A . H29B H 0.1724 1.2258 -0.0071 0.126 Uiso 1 1 calc R . . H29C H 0.1218 1.2108 0.0104 0.126 Uiso 1 1 calc R . . C30 C 0.0896(4) 1.0046(6) 0.0403(5) 0.059(3) Uani 0.80 1 d P A 1 H30A H 0.0572 0.9931 0.0478 0.071 Uiso 0.80 1 calc PR A 1 H30B H 0.0933 1.0653 0.0285 0.071 Uiso 0.80 1 calc PR A 1 C31 C 0.1034(3) 0.9440(4) 0.0006(2) 0.0517(14) Uani 0.80 1 d P A 1 H31A H 0.1164 0.9655 -0.0366 0.062 Uiso 0.80 1 calc PR A 1 C32 C 0.1087(2) 0.8608(4) 0.0161(3) 0.0577(14) Uani 0.80 1 d P A 1 H32A H 0.0772 0.8384 0.0226 0.069 Uiso 0.80 1 calc PR A 1 C33 C 0.13221(16) 0.7934(2) -0.0121(2) 0.0473(13) Uani 0.80 1 d PD A 1 C34 C 0.11289(15) 0.7099(3) -0.0183(2) 0.0726(16) Uani 0.80 1 d PD A 1 H34A H 0.0847 0.6974 -0.0046 0.087 Uiso 0.80 1 calc PR A 1 C35 C 0.1351(2) 0.6446(2) -0.0449(3) 0.0781(18) Uani 0.80 1 d PD A 1 H35A H 0.1219 0.5877 -0.0491 0.094 Uiso 0.80 1 calc PR A 1 C36 C 0.1763(2) 0.6626(3) -0.0651(3) 0.0799(18) Uani 0.80 1 d PD A 1 H36A H 0.1913 0.6181 -0.0831 0.096 Uiso 0.80 1 calc PR A 1 C37 C 0.19560(16) 0.7461(3) -0.0588(2) 0.0823(17) Uani 0.80 1 d PD A 1 H37A H 0.2238 0.7586 -0.0726 0.099 Uiso 0.80 1 calc PR A 1 C38 C 0.17354(17) 0.8110(2) -0.0324(2) 0.0741(18) Uani 0.80 1 d PD A 1 H38A H 0.1868 0.8678 -0.0281 0.089 Uiso 0.80 1 calc PR A 1 C31A C 0.0827(7) 0.9356(18) 0.0187(10) 0.042(4) Uani 0.20 1 d P A 2 H31B H 0.0555 0.8958 0.0218 0.050 Uiso 0.20 1 calc PR A 2 C34A C 0.0903(4) 0.7408(8) -0.0062(7) 0.050(3) Uani 0.20 1 d PD A 2 H34B H 0.0644 0.7574 0.0111 0.061 Uiso 0.20 1 calc PR A 2 C32A C 0.1266(6) 0.8972(19) -0.0064(9) 0.042(4) Uani 0.20 1 d P A 2 H32B H 0.1357 0.9315 -0.0422 0.050 Uiso 0.20 1 calc PR A 2 C35A C 0.0954(5) 0.6548(7) -0.0217(7) 0.050(3) Uani 0.20 1 d PD A 2 H35B H 0.0730 0.6128 -0.0150 0.061 Uiso 0.20 1 calc PR A 2 C36A C 0.1334(6) 0.6304(7) -0.0471(8) 0.050(3) Uani 0.20 1 d PD A 2 H36B H 0.1369 0.5719 -0.0576 0.061 Uiso 0.20 1 calc PR A 2 C30A C 0.0817(13) 1.026(2) 0.0396(19) 0.042(4) Uani 0.20 1 d P A 2 H30C H 0.0571 1.0415 0.0623 0.050 Uiso 0.20 1 calc PR A 2 H30D H 0.0859 1.0700 0.0066 0.050 Uiso 0.20 1 calc PR A 2 C38A C 0.1612(5) 0.7780(9) -0.0414(9) 0.050(3) Uani 0.20 1 d PD A 2 H38B H 0.1836 0.8199 -0.0481 0.061 Uiso 0.20 1 calc PR A 2 C33A C 0.1232(6) 0.8024(7) -0.0161(9) 0.050(3) Uani 0.20 1 d PD A 2 C37A C 0.1663(5) 0.6920(10) -0.0569(8) 0.050(3) Uani 0.20 1 d PD A 2 H37B H 0.1921 0.6755 -0.0742 0.061 Uiso 0.20 1 calc PR A 2 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 0.04321(15) 0.05489(17) 0.02490(13) -0.00288(14) 0.00707(10) -0.00111(15) Cl1 0.0499(5) 0.0550(6) 0.0464(5) -0.0082(4) 0.0113(4) 0.0037(4) N1 0.0311(14) 0.0495(17) 0.0290(14) 0.0023(12) 0.0094(12) 0.0046(12) N2 0.0321(14) 0.0468(17) 0.0255(13) -0.0008(12) 0.0072(11) 0.0022(13) C1 0.0340(18) 0.045(2) 0.0247(16) 0.0045(14) 0.0064(15) 0.0079(15) C2 0.047(2) 0.082(3) 0.0295(17) -0.0039(18) 0.0156(16) 0.0058(19) C3 0.060(2) 0.097(3) 0.0293(19) 0.0001(19) 0.0122(18) 0.013(2) C4 0.051(2) 0.079(3) 0.041(2) -0.0106(19) 0.0108(18) 0.004(2) C5 0.0391(19) 0.056(2) 0.0353(18) -0.0117(16) 0.0132(16) -0.0034(16) C6 0.0334(18) 0.056(2) 0.0312(18) 0.0057(16) 0.0106(15) 0.0043(17) C7 0.0363(17) 0.060(2) 0.0377(17) 0.0080(19) 0.0126(15) -0.0006(19) C8 0.0365(19) 0.073(3) 0.055(2) 0.017(2) 0.0109(17) 0.0023(19) C9 0.040(2) 0.085(3) 0.055(2) 0.012(2) 0.0120(18) -0.015(2) C10 0.058(2) 0.056(3) 0.051(2) 0.0082(19) 0.019(2) -0.007(2) C11 0.051(2) 0.060(2) 0.0332(19) 0.0052(17) 0.0186(17) 0.0001(19) C12 0.0317(18) 0.060(3) 0.057(2) 0.0100(19) 0.0149(17) 0.0065(17) C13 0.051(2) 0.068(3) 0.090(3) 0.003(2) 0.034(2) 0.005(2) C14 0.054(2) 0.063(3) 0.076(3) 0.021(2) 0.016(2) 0.010(2) C15 0.058(2) 0.057(2) 0.052(2) 0.0097(19) 0.0291(19) 0.007(2) C16 0.075(3) 0.061(3) 0.096(3) -0.012(2) 0.049(3) -0.007(2) C17 0.112(4) 0.080(3) 0.071(3) 0.034(2) 0.053(3) 0.042(3) C18 0.0451(19) 0.043(2) 0.0333(17) -0.0058(15) 0.0171(15) -0.0063(16) C19 0.0426(19) 0.045(2) 0.050(2) -0.0059(16) 0.0234(17) -0.0047(16) C20 0.058(2) 0.051(3) 0.080(3) -0.010(2) 0.044(2) -0.0040(18) C21 0.088(3) 0.060(3) 0.071(3) -0.007(2) 0.058(3) -0.016(2) C22 0.082(3) 0.052(2) 0.045(2) -0.0050(18) 0.035(2) -0.010(2) C23 0.050(2) 0.050(2) 0.0336(18) -0.0091(16) 0.0180(17) -0.0131(17) C24 0.0358(19) 0.058(2) 0.059(2) 0.0036(18) 0.0194(18) 0.0075(17) C25 0.040(2) 0.080(3) 0.071(3) 0.007(2) 0.013(2) 0.0041(19) C26 0.052(2) 0.070(3) 0.099(3) 0.008(2) 0.038(2) 0.013(2) C27 0.050(2) 0.060(2) 0.0287(17) 0.0095(17) 0.0108(16) 0.0011(18) C28 0.070(3) 0.062(3) 0.058(2) 0.012(2) 0.023(2) 0.012(2) C29 0.094(3) 0.102(4) 0.043(2) 0.012(2) 0.015(2) -0.012(3) C30 0.057(5) 0.066(6) 0.033(3) -0.003(3) -0.004(3) 0.016(3) C31 0.055(4) 0.061(4) 0.022(2) 0.002(3) -0.002(2) -0.011(3) C32 0.043(3) 0.080(5) 0.035(3) -0.016(3) 0.000(2) -0.015(3) C33 0.057(3) 0.058(3) 0.026(2) -0.004(2) 0.016(2) -0.013(3) C34 0.079(4) 0.079(4) 0.055(3) 0.001(3) 0.023(3) -0.024(3) C35 0.108(5) 0.058(4) 0.062(4) -0.018(3) 0.028(4) -0.013(4) C36 0.113(5) 0.071(5) 0.055(3) -0.012(3) 0.032(3) 0.001(4) C37 0.108(5) 0.087(5) 0.062(4) -0.011(3) 0.046(3) -0.011(4) C38 0.091(4) 0.088(5) 0.049(3) -0.002(3) 0.035(3) -0.021(4) C31A 0.017(6) 0.089(13) 0.014(5) 0.015(6) 0.001(4) 0.006(8) C34A 0.048(6) 0.066(6) 0.019(4) -0.015(4) -0.005(4) 0.015(4) C32A 0.017(6) 0.089(13) 0.014(5) 0.015(6) 0.001(4) 0.006(8) C35A 0.048(6) 0.066(6) 0.019(4) -0.015(4) -0.005(4) 0.015(4) C36A 0.048(6) 0.066(6) 0.019(4) -0.015(4) -0.005(4) 0.015(4) C30A 0.017(6) 0.089(13) 0.014(5) 0.015(6) 0.001(4) 0.006(8) C38A 0.048(6) 0.066(6) 0.019(4) -0.015(4) -0.005(4) 0.015(4) C33A 0.048(6) 0.066(6) 0.019(4) -0.015(4) -0.005(4) 0.015(4) C37A 0.048(6) 0.066(6) 0.019(4) -0.015(4) -0.005(4) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C1 2.054(3) . ? Pd1 C30 2.060(7) . ? Pd1 C31 2.106(4) . ? Pd1 C31A 2.150(16) . ? Pd1 C32 2.252(4) . ? Pd1 C32A 2.275(18) . ? Pd1 C30A 2.37(3) . ? Pd1 Cl1 2.3580(9) . ? N1 C1 1.355(4) . ? N1 C6 1.462(4) . ? N1 C2 1.486(4) . ? N2 C1 1.339(4) . ? N2 C18 1.452(4) . ? N2 C5 1.491(4) . ? C2 C3 1.484(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.532(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.492(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.394(4) . ? C6 C11 1.407(5) . ? C7 C8 1.397(4) . ? C7 C12 1.525(5) . ? C8 C9 1.383(5) . ? C8 H8A 0.9500 . ? C9 C10 1.379(5) . ? C9 H9A 0.9500 . ? C10 C11 1.390(5) . ? C10 H10A 0.9500 . ? C11 C15 1.518(5) . ? C12 C14 1.517(4) . ? C12 C13 1.525(5) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.533(5) . ? C15 C16 1.524(5) . ? C15 H15A 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.398(4) . ? C18 C23 1.406(4) . ? C19 C20 1.400(5) . ? C19 C24 1.512(5) . ? C20 C21 1.369(5) . ? C20 H20A 0.9500 . ? C21 C22 1.375(5) . ? C21 H21A 0.9500 . ? C22 C23 1.395(4) . ? C22 H22A 0.9500 . ? C23 C27 1.518(5) . ? C24 C25 1.530(5) . ? C24 C26 1.539(5) . ? C24 H24A 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.528(4) . ? C27 C28 1.538(5) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.376(9) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.328(8) . ? C31 H31A 1.0000 . ? C32 C33 1.464(7) . ? C32 H32A 1.0000 . ? C33 C38 1.393(2) . ? C33 C34 1.395(2) . ? C34 C35 1.399(2) . ? C34 H34A 0.9500 . ? C35 C36 1.390(2) . ? C35 H35A 0.9500 . ? C36 C37 1.395(2) . ? C36 H36A 0.9500 . ? C37 C38 1.392(2) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C31A C30A 1.47(4) . ? C31A C32A 1.61(3) . ? C31A H31B 1.0000 . ? C34A C33A 1.395(3) . ? C34A C35A 1.396(3) . ? C34A H34B 0.9500 . ? C32A C33A 1.49(3) . ? C32A H32B 1.0000 . ? C35A C36A 1.397(3) . ? C35A H35B 0.9500 . ? C36A C37A 1.395(3) . ? C36A H36B 0.9500 . ? C30A H30C 0.9900 . ? C30A H30D 0.9900 . ? C38A C37A 1.394(3) . ? C38A C33A 1.395(3) . ? C38A H38B 0.9500 . ? C37A H37B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 C30 105.6(3) . . ? C1 Pd1 C31 142.5(2) . . ? C30 Pd1 C31 38.6(3) . . ? C1 Pd1 C31A 134.0(7) . . ? C30 Pd1 C31A 31.5(8) . . ? C31 Pd1 C31A 21.7(4) . . ? C1 Pd1 C32 166.42(19) . . ? C30 Pd1 C32 67.3(3) . . ? C31 Pd1 C32 35.3(2) . . ? C31A Pd1 C32 36.6(7) . . ? C1 Pd1 C32A 163.4(7) . . ? C30 Pd1 C32A 65.2(6) . . ? C31 Pd1 C32A 26.6(5) . . ? C31A Pd1 C32A 42.6(7) . . ? C32 Pd1 C32A 24.8(6) . . ? C1 Pd1 C30A 99.2(9) . . ? C30 Pd1 C30A 6.4(11) . . ? C31 Pd1 C30A 44.8(10) . . ? C31A Pd1 C30A 37.5(11) . . ? C32 Pd1 C30A 73.7(9) . . ? C32A Pd1 C30A 71.3(11) . . ? C1 Pd1 Cl1 92.37(8) . . ? C30 Pd1 Cl1 161.8(3) . . ? C31 Pd1 Cl1 124.3(2) . . ? C31A Pd1 Cl1 130.6(7) . . ? C32 Pd1 Cl1 94.43(14) . . ? C32A Pd1 Cl1 98.0(6) . . ? C30A Pd1 Cl1 168.1(9) . . ? C1 N1 C6 118.6(2) . . ? C1 N1 C2 128.6(2) . . ? C6 N1 C2 112.8(2) . . ? C1 N2 C18 120.3(2) . . ? C1 N2 C5 123.2(2) . . ? C18 N2 C5 114.2(2) . . ? N2 C1 N1 119.3(3) . . ? N2 C1 Pd1 123.5(2) . . ? N1 C1 Pd1 117.0(2) . . ? N1 C2 C3 114.4(3) . . ? N1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C2 C3 C4 110.4(3) . . ? C2 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? C2 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 112.2(3) . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N2 C5 C4 114.7(3) . . ? N2 C5 H5A 108.6 . . ? C4 C5 H5A 108.6 . . ? N2 C5 H5B 108.6 . . ? C4 C5 H5B 108.6 . . ? H5A C5 H5B 107.6 . . ? C7 C6 C11 122.4(3) . . ? C7 C6 N1 117.8(3) . . ? C11 C6 N1 119.6(3) . . ? C6 C7 C8 117.8(3) . . ? C6 C7 C12 123.0(3) . . ? C8 C7 C12 119.2(3) . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8A 119.6 . . ? C7 C8 H8A 119.6 . . ? C8 C9 C10 120.1(3) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C9 C10 C11 121.6(4) . . ? C9 C10 H10A 119.2 . . ? C11 C10 H10A 119.2 . . ? C10 C11 C6 117.1(3) . . ? C10 C11 C15 120.2(3) . . ? C6 C11 C15 122.6(3) . . ? C7 C12 C14 113.6(3) . . ? C7 C12 C13 110.6(3) . . ? C14 C12 C13 110.1(3) . . ? C7 C12 H12A 107.4 . . ? C14 C12 H12A 107.4 . . ? C13 C12 H12A 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 109.1(3) . . ? C11 C15 C16 113.5(3) . . ? C17 C15 C16 109.2(3) . . ? C11 C15 H15A 108.3 . . ? C17 C15 H15A 108.3 . . ? C16 C15 H15A 108.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 121.9(3) . . ? C19 C18 N2 119.3(3) . . ? C23 C18 N2 118.7(3) . . ? C18 C19 C20 117.3(3) . . ? C18 C19 C24 123.8(3) . . ? C20 C19 C24 118.8(3) . . ? C21 C20 C19 122.2(4) . . ? C21 C20 H20A 118.9 . . ? C19 C20 H20A 118.9 . . ? C22 C21 C20 119.1(4) . . ? C22 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C21 C22 C23 122.1(4) . . ? C21 C22 H22A 118.9 . . ? C23 C22 H22A 118.9 . . ? C22 C23 C18 117.2(3) . . ? C22 C23 C27 119.1(3) . . ? C18 C23 C27 123.5(3) . . ? C19 C24 C25 110.8(3) . . ? C19 C24 C26 113.4(3) . . ? C25 C24 C26 108.7(3) . . ? C19 C24 H24A 107.9 . . ? C25 C24 H24A 107.9 . . ? C26 C24 H24A 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 113.8(3) . . ? C23 C27 C28 109.6(3) . . ? C29 C27 C28 107.9(3) . . ? C23 C27 H27A 108.5 . . ? C29 C27 H27A 108.5 . . ? C28 C27 H27A 108.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 Pd1 72.5(3) . . ? C31 C30 H30A 116.3 . . ? Pd1 C30 H30A 116.3 . . ? C31 C30 H30B 116.3 . . ? Pd1 C30 H30B 116.3 . . ? H30A C30 H30B 113.3 . . ? C32 C31 C30 124.8(9) . . ? C32 C31 Pd1 78.4(3) . . ? C30 C31 Pd1 68.9(4) . . ? C32 C31 H31A 117.1 . . ? C30 C31 H31A 117.1 . . ? Pd1 C31 H31A 117.1 . . ? C31 C32 C33 129.8(8) . . ? C31 C32 Pd1 66.3(3) . . ? C33 C32 Pd1 122.3(3) . . ? C31 C32 H32A 110.4 . . ? C33 C32 H32A 110.4 . . ? Pd1 C32 H32A 110.4 . . ? C38 C33 C34 119.6(2) . . ? C38 C33 C32 121.2(4) . . ? C34 C33 C32 119.2(4) . . ? C33 C34 C35 119.9(2) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 120.3(2) . . ? C36 C35 H35A 119.9 . . ? C34 C35 H35A 119.9 . . ? C35 C36 C37 119.8(2) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? C38 C37 C36 120.0(2) . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C37 C38 C33 120.5(2) . . ? C37 C38 H38A 119.7 . . ? C33 C38 H38A 119.7 . . ? C30A C31A C32A 123(3) . . ? C30A C31A Pd1 79.3(16) . . ? C32A C31A Pd1 72.9(9) . . ? C30A C31A H31B 118.4 . . ? C32A C31A H31B 118.4 . . ? Pd1 C31A H31B 118.4 . . ? C33A C34A C35A 120.0(2) . . ? C33A C34A H34B 120.0 . . ? C35A C34A H34B 120.0 . . ? C33A C32A C31A 113(2) . . ? C33A C32A Pd1 115.8(13) . . ? C31A C32A Pd1 64.6(9) . . ? C33A C32A H32B 117.5 . . ? C31A C32A H32B 117.5 . . ? Pd1 C32A H32B 117.5 . . ? C34A C35A C36A 120.0(2) . . ? C34A C35A H35B 120.0 . . ? C36A C35A H35B 120.0 . . ? C37A C36A C35A 119.9(2) . . ? C37A C36A H36B 120.0 . . ? C35A C36A H36B 120.0 . . ? C31A C30A Pd1 63.2(14) . . ? C31A C30A H30C 117.4 . . ? Pd1 C30A H30C 117.4 . . ? C31A C30A H30D 117.4 . . ? Pd1 C30A H30D 117.4 . . ? H30C C30A H30D 114.5 . . ? C37A C38A C33A 120.1(2) . . ? C37A C38A H38B 120.0 . . ? C33A C38A H38B 120.0 . . ? C38A C33A C34A 120.0(2) . . ? C38A C33A C32A 107.5(12) . . ? C34A C33A C32A 132.6(12) . . ? C38A C37A C36A 120.0(2) . . ? C38A C37A H37B 120.0 . . ? C36A C37A H37B 120.0 . . ? 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 C18 N2 C1 N1 -177.5(3) . . . . ? C5 N2 C1 N1 -15.8(4) . . . . ? C18 N2 C1 Pd1 8.8(4) . . . . ? C5 N2 C1 Pd1 170.5(2) . . . . ? C6 N1 C1 N2 162.6(3) . . . . ? C2 N1 C1 N2 -18.8(5) . . . . ? C6 N1 C1 Pd1 -23.3(4) . . . . ? C2 N1 C1 Pd1 155.3(3) . . . . ? C30 Pd1 C1 N2 -113.2(4) . . . . ? C31 Pd1 C1 N2 -98.8(4) . . . . ? C31A Pd1 C1 N2 -129.1(9) . . . . ? C32 Pd1 C1 N2 -170.2(6) . . . . ? C32A Pd1 C1 N2 -59.1(16) . . . . ? C30A Pd1 C1 N2 -112.9(9) . . . . ? Cl1 Pd1 C1 N2 69.8(2) . . . . ? C30 Pd1 C1 N1 73.0(4) . . . . ? C31 Pd1 C1 N1 87.4(4) . . . . ? C31A Pd1 C1 N1 57.1(9) . . . . ? C32 Pd1 C1 N1 16.0(8) . . . . ? C32A Pd1 C1 N1 127.1(15) . . . . ? C30A Pd1 C1 N1 73.3(9) . . . . ? Cl1 Pd1 C1 N1 -104.0(2) . . . . ? C1 N1 C2 C3 -29.9(5) . . . . ? C6 N1 C2 C3 148.8(3) . . . . ? N1 C2 C3 C4 81.2(4) . . . . ? C2 C3 C4 C5 -37.5(4) . . . . ? C1 N2 C5 C4 78.3(4) . . . . ? C18 N2 C5 C4 -119.0(3) . . . . ? C3 C4 C5 N2 -46.7(4) . . . . ? C1 N1 C6 C7 -92.8(4) . . . . ? C2 N1 C6 C7 88.4(3) . . . . ? C1 N1 C6 C11 91.2(4) . . . . ? C2 N1 C6 C11 -87.7(4) . . . . ? C11 C6 C7 C8 -3.0(5) . . . . ? N1 C6 C7 C8 -178.9(3) . . . . ? C11 C6 C7 C12 175.4(3) . . . . ? N1 C6 C7 C12 -0.5(4) . . . . ? C6 C7 C8 C9 0.6(5) . . . . ? C12 C7 C8 C9 -177.8(3) . . . . ? C7 C8 C9 C10 1.1(6) . . . . ? C8 C9 C10 C11 -0.6(6) . . . . ? C9 C10 C11 C6 -1.7(5) . . . . ? C9 C10 C11 C15 174.6(3) . . . . ? C7 C6 C11 C10 3.5(5) . . . . ? N1 C6 C11 C10 179.4(3) . . . . ? C7 C6 C11 C15 -172.7(3) . . . . ? N1 C6 C11 C15 3.2(5) . . . . ? C6 C7 C12 C14 136.6(3) . . . . ? C8 C7 C12 C14 -45.0(4) . . . . ? C6 C7 C12 C13 -98.9(4) . . . . ? C8 C7 C12 C13 79.4(4) . . . . ? C10 C11 C15 C17 -73.9(4) . . . . ? C6 C11 C15 C17 102.1(4) . . . . ? C10 C11 C15 C16 48.1(4) . . . . ? C6 C11 C15 C16 -135.8(3) . . . . ? C1 N2 C18 C19 -110.0(3) . . . . ? C5 N2 C18 C19 86.7(3) . . . . ? C1 N2 C18 C23 74.2(4) . . . . ? C5 N2 C18 C23 -89.1(3) . . . . ? C23 C18 C19 C20 -2.6(5) . . . . ? N2 C18 C19 C20 -178.3(3) . . . . ? C23 C18 C19 C24 173.2(3) . . . . ? N2 C18 C19 C24 -2.5(5) . . . . ? C18 C19 C20 C21 0.0(5) . . . . ? C24 C19 C20 C21 -176.0(3) . . . . ? C19 C20 C21 C22 1.1(6) . . . . ? C20 C21 C22 C23 0.4(6) . . . . ? C21 C22 C23 C18 -2.8(5) . . . . ? C21 C22 C23 C27 172.3(3) . . . . ? C19 C18 C23 C22 4.0(5) . . . . ? N2 C18 C23 C22 179.6(3) . . . . ? C19 C18 C23 C27 -170.9(3) . . . . ? N2 C18 C23 C27 4.8(5) . . . . ? C18 C19 C24 C25 -100.8(4) . . . . ? C20 C19 C24 C25 74.9(4) . . . . ? C18 C19 C24 C26 136.6(3) . . . . ? C20 C19 C24 C26 -47.6(4) . . . . ? C22 C23 C27 C29 42.6(4) . . . . ? C18 C23 C27 C29 -142.6(3) . . . . ? C22 C23 C27 C28 -78.3(4) . . . . ? C18 C23 C27 C28 96.5(4) . . . . ? C1 Pd1 C30 C31 165.9(5) . . . . ? C31A Pd1 C30 C31 -36.3(9) . . . . ? C32 Pd1 C30 C31 -26.4(6) . . . . ? C32A Pd1 C30 C31 0.7(10) . . . . ? C30A Pd1 C30 C31 164(11) . . . . ? Cl1 Pd1 C30 C31 -23.6(15) . . . . ? Pd1 C30 C31 C32 58.0(7) . . . . ? C1 Pd1 C31 C32 -157.3(4) . . . . ? C30 Pd1 C31 C32 -134.7(10) . . . . ? C31A Pd1 C31 C32 -78(2) . . . . ? C32A Pd1 C31 C32 46.6(14) . . . . ? C30A Pd1 C31 C32 -137.3(14) . . . . ? Cl1 Pd1 C31 C32 36.6(7) . . . . ? C1 Pd1 C31 C30 -22.6(8) . . . . ? C31A Pd1 C31 C30 57(2) . . . . ? C32 Pd1 C31 C30 134.7(10) . . . . ? C32A Pd1 C31 C30 -179(2) . . . . ? C30A Pd1 C31 C30 -2.6(17) . . . . ? Cl1 Pd1 C31 C30 171.3(6) . . . . ? C30 C31 C32 C33 -167.1(6) . . . . ? Pd1 C31 C32 C33 -113.3(5) . . . . ? C30 C31 C32 Pd1 -53.8(7) . . . . ? C1 Pd1 C32 C31 89.8(10) . . . . ? C30 Pd1 C32 C31 28.7(6) . . . . ? C31A Pd1 C32 C31 37.3(8) . . . . ? C32A Pd1 C32 C31 -50.9(12) . . . . ? C30A Pd1 C32 C31 29.9(11) . . . . ? Cl1 Pd1 C32 C31 -150.4(6) . . . . ? C1 Pd1 C32 C33 -146.9(5) . . . . ? C30 Pd1 C32 C33 152.0(6) . . . . ? C31 Pd1 C32 C33 123.3(9) . . . . ? C31A Pd1 C32 C33 160.6(13) . . . . ? C32A Pd1 C32 C33 72.4(15) . . . . ? C30A Pd1 C32 C33 153.2(10) . . . . ? Cl1 Pd1 C32 C33 -27.1(5) . . . . ? C31 C32 C33 C38 31.1(7) . . . . ? Pd1 C32 C33 C38 -53.7(5) . . . . ? C31 C32 C33 C34 -149.2(5) . . . . ? Pd1 C32 C33 C34 126.0(4) . . . . ? C38 C33 C34 C35 -0.03(6) . . . . ? C32 C33 C34 C35 -179.7(4) . . . . ? C33 C34 C35 C36 -0.02(6) . . . . ? C34 C35 C36 C37 0.03(13) . . . . ? C35 C36 C37 C38 0.02(17) . . . . ? C36 C37 C38 C33 -0.07(17) . . . . ? C34 C33 C38 C37 0.08(13) . . . . ? C32 C33 C38 C37 179.7(4) . . . . ? C1 Pd1 C31A C30A 27(2) . . . . ? C30 Pd1 C31A C30A -4(2) . . . . ? C31 Pd1 C31A C30A -97(3) . . . . ? C32 Pd1 C31A C30A -168(2) . . . . ? C32A Pd1 C31A C30A -130(3) . . . . ? Cl1 Pd1 C31A C30A -178.4(15) . . . . ? C1 Pd1 C31A C32A 156.6(11) . . . . ? C30 Pd1 C31A C32A 126(2) . . . . ? C31 Pd1 C31A C32A 33.0(18) . . . . ? C32 Pd1 C31A C32A -38.4(10) . . . . ? C30A Pd1 C31A C32A 130(3) . . . . ? Cl1 Pd1 C31A C32A -48.6(17) . . . . ? C30A C31A C32A C33A 173(2) . . . . ? Pd1 C31A C32A C33A 108.7(13) . . . . ? C30A C31A C32A Pd1 64.3(19) . . . . ? C1 Pd1 C32A C33A 168.5(10) . . . . ? C30 Pd1 C32A C33A -132.3(13) . . . . ? C31 Pd1 C32A C33A -131(2) . . . . ? C31A Pd1 C32A C33A -105(2) . . . . ? C32 Pd1 C32A C33A -42.9(15) . . . . ? C30A Pd1 C32A C33A -134.3(16) . . . . ? Cl1 Pd1 C32A C33A 40.2(12) . . . . ? C1 Pd1 C32A C31A -87(2) . . . . ? C30 Pd1 C32A C31A -27.6(13) . . . . ? C31 Pd1 C32A C31A -26.7(12) . . . . ? C32 Pd1 C32A C31A 61.7(13) . . . . ? C30A Pd1 C32A C31A -29.6(16) . . . . ? Cl1 Pd1 C32A C31A 144.9(14) . . . . ? C33A C34A C35A C36A 0.00(6) . . . . ? C34A C35A C36A C37A -0.01(13) . . . . ? C32A C31A C30A Pd1 -61.2(16) . . . . ? C1 Pd1 C30A C31A -160.8(15) . . . . ? C30 Pd1 C30A C31A 17(9) . . . . ? C31 Pd1 C30A C31A 31.4(11) . . . . ? C32 Pd1 C30A C31A 7.3(14) . . . . ? C32A Pd1 C30A C31A 33.2(17) . . . . ? Cl1 Pd1 C30A C31A 6(6) . . . . ? C37A C38A C33A C34A 0.03(13) . . . . ? C37A C38A C33A C32A -178.7(13) . . . . ? C35A C34A C33A C38A -0.01(6) . . . . ? C35A C34A C33A C32A 178.3(17) . . . . ? C31A C32A C33A C38A 176.9(11) . . . . ? Pd1 C32A C33A C38A -111.3(10) . . . . ? C31A C32A C33A C34A -2(2) . . . . ? Pd1 C32A C33A C34A 70.2(16) . . . . ? C33A C38A C37A C36A -0.04(18) . . . . ? C35A C36A C37A C38A 0.03(17) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.545 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.059 data_KEPd7 _database_code_depnum_ccdc_archive 'CCDC 784543' #TrackingRef 'kepd7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H39 Cl N2 Pd' _chemical_formula_sum 'C32 H39 Cl N2 Pd' _chemical_formula_weight 593.50 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 orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.5263(13) _cell_length_b 9.5695(7) _cell_length_c 31.830(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5643.1(7) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 451 _cell_measurement_theta_min 3 _cell_measurement_theta_max 33 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 SMART APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 111418 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0330 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 33.24 _reflns_number_total 10768 _reflns_number_gt 8132 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_cell_refinement 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_data_reduction 'SAINTPlus, v. 6.2 (Bruker, 2001)' _computing_structure_solution 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _computing_publication_material 'SHELXTL, v. 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0266P)^2^+4.2579P] 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 10768 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0694 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.002 _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 0.472372(4) 0.585939(8) 0.119648(3) 0.01139(2) Uani 1 1 d . . . Cl1 Cl 0.452063(17) 0.38480(3) 0.161212(9) 0.01843(6) Uani 1 1 d . . . N1 N 0.52951(5) 0.77243(10) 0.18733(3) 0.01408(19) Uani 1 1 d . . . N2 N 0.61714(5) 0.63651(11) 0.15492(3) 0.0148(2) Uani 1 1 d . . . C15 C 0.63406(6) 0.53281(13) 0.12329(4) 0.0142(2) Uani 1 1 d . . . C18 C 0.65967(7) 0.33215(14) 0.06170(4) 0.0187(3) Uani 1 1 d . . . C1 C 0.54782(6) 0.67717(12) 0.15826(3) 0.0125(2) Uani 1 1 d . . . C6 C 0.46051(6) 0.84051(12) 0.18252(4) 0.0142(2) Uani 1 1 d . . . C17 C 0.65700(7) 0.47331(14) 0.05134(4) 0.0185(3) Uani 1 1 d . . . H17A H 0.6634 0.5005 0.0229 0.022 Uiso 1 1 calc R . . C20 C 0.64032(6) 0.39278(13) 0.13508(4) 0.0165(2) Uani 1 1 d . . . C12 C 0.52284(7) 1.02587(13) 0.13858(4) 0.0207(3) Uani 1 1 d . . . H12A H 0.5625 1.0257 0.1589 0.031 Uiso 1 1 calc R . . H12B H 0.5123 1.1222 0.1301 0.031 Uiso 1 1 calc R . . H12C H 0.5368 0.9712 0.1138 0.031 Uiso 1 1 calc R . . C7 C 0.45668(7) 0.96213(12) 0.15832(4) 0.0156(2) Uani 1 1 d . . . C16 C 0.64521(6) 0.57607(13) 0.08170(4) 0.0159(2) Uani 1 1 d . . . C11 C 0.39970(7) 0.78630(12) 0.20305(4) 0.0161(2) Uani 1 1 d . . . C8 C 0.38945(7) 1.02471(13) 0.15247(4) 0.0182(3) Uani 1 1 d . . . H8A H 0.3860 1.1068 0.1358 0.022 Uiso 1 1 calc R . . C27 C 0.38967(7) 0.37172(13) 0.05908(4) 0.0179(2) Uani 1 1 d . . . C9 C 0.32729(7) 0.96940(13) 0.17051(4) 0.0191(3) Uani 1 1 d . . . C14 C 0.40508(7) 0.65902(13) 0.23070(4) 0.0203(3) Uani 1 1 d . . . H14A H 0.4424 0.6740 0.2521 0.030 Uiso 1 1 calc R . . H14B H 0.4178 0.5776 0.2135 0.030 Uiso 1 1 calc R . . H14C H 0.3585 0.6426 0.2445 0.030 Uiso 1 1 calc R . . C19 C 0.65266(7) 0.29413(14) 0.10359(4) 0.0186(3) Uani 1 1 d . . . H19A H 0.6564 0.1983 0.1110 0.022 Uiso 1 1 calc R . . C3 C 0.61867(7) 0.70080(15) 0.24311(4) 0.0219(3) Uani 1 1 d . . . H3A H 0.5938 0.6094 0.2412 0.026 Uiso 1 1 calc R . . H3B H 0.6287 0.7195 0.2731 0.026 Uiso 1 1 calc R . . C2 C 0.56935(7) 0.81386(14) 0.22614(4) 0.0190(3) Uani 1 1 d . . . H2A H 0.5339 0.8391 0.2481 0.023 Uiso 1 1 calc R . . H2B H 0.5985 0.8981 0.2200 0.023 Uiso 1 1 calc R . . C5 C 0.67832(7) 0.71774(16) 0.17222(4) 0.0230(3) Uani 1 1 d . . . H5A H 0.6693 0.8185 0.1675 0.028 Uiso 1 1 calc R . . H5B H 0.7229 0.6923 0.1568 0.028 Uiso 1 1 calc R . . C10 C 0.33383(7) 0.85265(13) 0.19628(4) 0.0184(3) Uani 1 1 d . . . H10A H 0.2919 0.8170 0.2097 0.022 Uiso 1 1 calc R . . C28 C 0.32355(8) 0.30133(15) 0.05983(4) 0.0249(3) Uani 1 1 d . . . H28A H 0.2811 0.3497 0.0681 0.030 Uiso 1 1 calc R . . C32 C 0.45137(8) 0.29762(14) 0.04772(4) 0.0238(3) Uani 1 1 d . . . H32A H 0.4970 0.3431 0.0478 0.029 Uiso 1 1 calc R . . C21 C 0.64512(7) 0.72814(14) 0.06982(4) 0.0218(3) Uani 1 1 d . . . H21A H 0.6065 0.7765 0.0850 0.033 Uiso 1 1 calc R . . H21B H 0.6371 0.7372 0.0395 0.033 Uiso 1 1 calc R . . H21C H 0.6917 0.7699 0.0772 0.033 Uiso 1 1 calc R . . C29 C 0.31946(9) 0.16057(16) 0.04853(5) 0.0328(4) Uani 1 1 d . . . H29A H 0.2743 0.1134 0.0489 0.039 Uiso 1 1 calc R . . C22 C 0.66948(8) 0.22190(16) 0.02830(4) 0.0262(3) Uani 1 1 d . . . H22A H 0.6317 0.2321 0.0069 0.039 Uiso 1 1 calc R . . H22B H 0.6661 0.1290 0.0411 0.039 Uiso 1 1 calc R . . H22C H 0.7170 0.2330 0.0151 0.039 Uiso 1 1 calc R . . C13 C 0.25457(8) 1.03545(16) 0.16333(5) 0.0294(3) Uani 1 1 d . . . H13A H 0.2600 1.1169 0.1449 0.044 Uiso 1 1 calc R . . H13B H 0.2342 1.0651 0.1903 0.044 Uiso 1 1 calc R . . H13C H 0.2222 0.9674 0.1501 0.044 Uiso 1 1 calc R . . C23 C 0.63305(7) 0.34741(15) 0.18000(4) 0.0228(3) Uani 1 1 d . . . H23A H 0.6693 0.3954 0.1971 0.034 Uiso 1 1 calc R . . H23B H 0.6404 0.2462 0.1819 0.034 Uiso 1 1 calc R . . H23C H 0.5847 0.3710 0.1903 0.034 Uiso 1 1 calc R . . C30 C 0.38119(10) 0.09027(15) 0.03677(4) 0.0348(4) Uani 1 1 d . . . H30A H 0.3785 -0.0054 0.0289 0.042 Uiso 1 1 calc R . . C4 C 0.69022(7) 0.69307(17) 0.21907(4) 0.0261(3) Uani 1 1 d . . . H4A H 0.7239 0.7644 0.2302 0.031 Uiso 1 1 calc R . . H4B H 0.7124 0.6000 0.2233 0.031 Uiso 1 1 calc R . . C31 C 0.44673(10) 0.15793(16) 0.03635(5) 0.0321(4) Uani 1 1 d . . . H31A H 0.4890 0.1087 0.0282 0.038 Uiso 1 1 calc R . . C26 C 0.39284(7) 0.51999(13) 0.07146(4) 0.0184(3) Uani 1 1 d . . . H26A H 0.3441 0.5624 0.0757 0.022 Uiso 1 1 calc R . . C25 C 0.44328(7) 0.61475(13) 0.05530(4) 0.0195(3) Uani 1 1 d . . . H25A H 0.4771 0.5847 0.0326 0.023 Uiso 1 1 calc R . . C24 C 0.45250(7) 0.74583(14) 0.07484(4) 0.0216(3) Uani 1 1 d . . . H24A H 0.4084 0.8024 0.0791 0.026 Uiso 1 1 calc R . . H24B H 0.4948 0.8015 0.0658 0.026 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 0.01262(3) 0.01081(3) 0.01074(3) -0.00044(3) -0.00146(3) -0.00065(3) Cl1 0.02568(13) 0.01324(11) 0.01638(12) 0.00172(10) 0.00076(10) -0.00168(10) N1 0.0154(4) 0.0147(4) 0.0121(4) -0.0026(3) -0.0023(4) 0.0004(4) N2 0.0123(4) 0.0199(4) 0.0122(4) -0.0025(4) -0.0009(3) -0.0009(4) C15 0.0113(4) 0.0192(5) 0.0121(5) -0.0010(4) -0.0001(4) 0.0017(4) C18 0.0135(5) 0.0251(6) 0.0175(5) -0.0043(5) -0.0009(4) 0.0031(5) C1 0.0141(4) 0.0128(4) 0.0105(4) 0.0004(4) -0.0002(4) -0.0014(4) C6 0.0178(5) 0.0123(4) 0.0126(5) -0.0031(4) -0.0003(4) 0.0008(4) C17 0.0162(5) 0.0273(6) 0.0120(5) -0.0002(5) 0.0010(4) 0.0015(5) C20 0.0128(5) 0.0222(6) 0.0145(5) 0.0018(4) 0.0000(4) 0.0031(4) C12 0.0236(6) 0.0155(5) 0.0230(6) 0.0023(4) 0.0030(5) -0.0041(5) C7 0.0204(5) 0.0119(4) 0.0146(5) -0.0023(4) 0.0004(4) -0.0009(4) C16 0.0131(5) 0.0218(5) 0.0127(5) 0.0018(4) 0.0009(4) 0.0005(4) C11 0.0203(5) 0.0131(5) 0.0148(5) -0.0028(4) 0.0024(4) -0.0009(4) C8 0.0239(6) 0.0140(5) 0.0167(5) -0.0009(4) -0.0006(4) 0.0021(5) C27 0.0238(6) 0.0175(5) 0.0125(5) 0.0003(4) -0.0061(4) -0.0019(5) C9 0.0212(6) 0.0169(5) 0.0192(5) -0.0043(4) -0.0004(5) 0.0037(5) C14 0.0272(6) 0.0164(5) 0.0173(5) 0.0018(4) 0.0073(5) 0.0014(5) C19 0.0154(5) 0.0212(5) 0.0193(5) 0.0007(5) 0.0001(4) 0.0032(4) C3 0.0231(6) 0.0294(6) 0.0132(5) -0.0024(5) -0.0036(4) 0.0032(5) C2 0.0212(5) 0.0217(6) 0.0141(5) -0.0047(4) -0.0038(4) -0.0020(5) C5 0.0149(5) 0.0352(7) 0.0190(6) -0.0059(5) -0.0010(4) -0.0059(5) C10 0.0177(5) 0.0180(5) 0.0194(5) -0.0030(4) 0.0045(4) -0.0003(4) C28 0.0264(6) 0.0259(6) 0.0225(6) 0.0043(5) -0.0066(5) -0.0073(5) C32 0.0283(6) 0.0224(6) 0.0206(6) -0.0015(5) -0.0032(5) 0.0020(5) C21 0.0235(6) 0.0232(6) 0.0186(6) 0.0032(5) 0.0031(5) 0.0003(5) C29 0.0448(8) 0.0274(7) 0.0262(7) 0.0058(6) -0.0114(6) -0.0169(6) C22 0.0275(6) 0.0295(7) 0.0217(6) -0.0078(5) -0.0025(5) 0.0056(6) C13 0.0249(6) 0.0294(7) 0.0340(7) -0.0018(6) -0.0018(6) 0.0104(6) C23 0.0245(6) 0.0278(6) 0.0161(5) 0.0066(5) 0.0021(5) 0.0080(5) C30 0.0671(11) 0.0165(6) 0.0208(6) -0.0001(5) -0.0135(7) -0.0039(7) C4 0.0186(6) 0.0401(8) 0.0197(6) -0.0078(6) -0.0065(5) 0.0010(6) C31 0.0496(9) 0.0242(7) 0.0224(6) -0.0049(5) -0.0058(6) 0.0078(7) C26 0.0187(5) 0.0180(5) 0.0184(5) -0.0013(4) -0.0080(4) -0.0005(4) C25 0.0251(6) 0.0198(5) 0.0136(5) 0.0028(4) -0.0078(4) -0.0025(5) C24 0.0276(6) 0.0174(5) 0.0200(5) 0.0048(5) -0.0098(5) -0.0034(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 C1 2.0559(11) . ? Pd1 C24 2.1239(13) . ? Pd1 C25 2.1358(12) . ? Pd1 C26 2.2185(12) . ? Pd1 Cl1 2.3658(3) . ? N1 C1 1.3424(15) . ? N1 C6 1.4429(15) . ? N1 C2 1.4927(15) . ? N2 C1 1.3461(15) . ? N2 C15 1.4479(15) . ? N2 C5 1.4806(16) . ? C15 C20 1.3963(17) . ? C15 C16 1.4026(16) . ? C18 C17 1.3914(19) . ? C18 C19 1.3882(18) . ? C18 C22 1.5088(19) . ? C6 C7 1.3974(17) . ? C6 C11 1.4019(17) . ? C17 C16 1.3958(17) . ? C17 H17A 0.9500 . ? C20 C19 1.3957(18) . ? C20 C23 1.5004(17) . ? C12 C7 1.5065(18) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C7 C8 1.3946(17) . ? C16 C21 1.5035(18) . ? C11 C10 1.3924(18) . ? C11 C14 1.5059(17) . ? C8 C9 1.3914(18) . ? C8 H8A 0.9500 . ? C27 C28 1.3981(19) . ? C27 C32 1.3929(19) . ? C27 C26 1.4737(18) . ? C9 C10 1.3912(18) . ? C9 C13 1.5056(19) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C19 H19A 0.9500 . ? C3 C2 1.5156(19) . ? C3 C4 1.5323(19) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C5 C4 1.5258(19) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C10 H10A 0.9500 . ? C28 C29 1.396(2) . ? C28 H28A 0.9500 . ? C32 C31 1.388(2) . ? C32 H32A 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C29 C30 1.379(3) . ? C29 H29A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C30 C31 1.376(3) . ? C30 H30A 0.9500 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C31 H31A 0.9500 . ? C26 C25 1.4000(18) . ? C26 H26A 1.0000 . ? C25 C24 1.4104(18) . ? C25 H25A 1.0000 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 C24 102.32(5) . . ? C1 Pd1 C25 133.64(5) . . ? C24 Pd1 C25 38.67(5) . . ? C1 Pd1 C26 170.29(5) . . ? C24 Pd1 C26 68.01(5) . . ? C25 Pd1 C26 37.45(5) . . ? C1 Pd1 Cl1 96.85(3) . . ? C24 Pd1 Cl1 159.08(4) . . ? C25 Pd1 Cl1 126.95(4) . . ? C26 Pd1 Cl1 92.84(3) . . ? C1 N1 C6 117.22(9) . . ? C1 N1 C2 128.74(10) . . ? C6 N1 C2 113.95(9) . . ? C1 N2 C15 117.36(9) . . ? C1 N2 C5 123.31(10) . . ? C15 N2 C5 116.92(10) . . ? C20 C15 C16 121.64(11) . . ? C20 C15 N2 119.27(10) . . ? C16 C15 N2 119.07(11) . . ? C17 C18 C19 118.60(12) . . ? C17 C18 C22 121.07(12) . . ? C19 C18 C22 120.32(12) . . ? N1 C1 N2 119.46(10) . . ? N1 C1 Pd1 121.91(8) . . ? N2 C1 Pd1 118.60(8) . . ? C7 C6 C11 121.62(11) . . ? C7 C6 N1 118.66(10) . . ? C11 C6 N1 119.69(10) . . ? C18 C17 C16 121.70(11) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C15 C20 C19 118.02(11) . . ? C15 C20 C23 121.75(11) . . ? C19 C20 C23 120.22(12) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C6 C7 C8 118.47(11) . . ? C6 C7 C12 121.73(11) . . ? C8 C7 C12 119.80(11) . . ? C15 C16 C17 117.94(11) . . ? C15 C16 C21 121.53(11) . . ? C17 C16 C21 120.53(11) . . ? C6 C11 C10 117.60(11) . . ? C6 C11 C14 121.24(11) . . ? C10 C11 C14 121.15(11) . . ? C9 C8 C7 121.38(11) . . ? C9 C8 H8A 119.3 . . ? C7 C8 H8A 119.3 . . ? C28 C27 C32 118.56(12) . . ? C28 C27 C26 119.62(12) . . ? C32 C27 C26 121.79(12) . . ? C8 C9 C10 118.47(12) . . ? C8 C9 C13 121.21(12) . . ? C10 C9 C13 120.31(12) . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C19 C18 121.86(12) . . ? C20 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? C2 C3 C4 112.21(11) . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N1 C2 C3 113.79(10) . . ? N1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? N2 C5 C4 113.14(11) . . ? N2 C5 H5A 109.0 . . ? C4 C5 H5A 109.0 . . ? N2 C5 H5B 109.0 . . ? C4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C9 C10 C11 122.27(12) . . ? C9 C10 H10A 118.9 . . ? C11 C10 H10A 118.9 . . ? C27 C28 C29 120.52(14) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C31 C32 C27 120.48(14) . . ? C31 C32 H32A 119.8 . . ? C27 C32 H32A 119.8 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C30 C29 C28 119.72(15) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C30 C31 120.33(14) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C5 C4 C3 110.83(11) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C32 C31 C30 120.36(16) . . ? C32 C31 H31A 119.8 . . ? C30 C31 H31A 119.8 . . ? C25 C26 C27 123.50(12) . . ? C25 C26 Pd1 68.07(7) . . ? C27 C26 Pd1 119.03(8) . . ? C25 C26 H26A 113.0 . . ? C27 C26 H26A 113.0 . . ? Pd1 C26 H26A 113.0 . . ? C26 C25 C24 119.66(12) . . ? C26 C25 Pd1 74.48(7) . . ? C24 C25 Pd1 70.21(7) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? Pd1 C25 H25A 119.9 . . ? C25 C24 Pd1 71.12(7) . . ? C25 C24 H24A 116.5 . . ? Pd1 C24 H24A 116.5 . . ? C25 C24 H24B 116.5 . . ? Pd1 C24 H24B 116.5 . . ? H24A C24 H24B 113.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 N2 C15 C20 -98.21(13) . . . . ? C5 N2 C15 C20 98.79(13) . . . . ? C1 N2 C15 C16 83.08(14) . . . . ? C5 N2 C15 C16 -79.91(14) . . . . ? C6 N1 C1 N2 163.50(10) . . . . ? C2 N1 C1 N2 -20.19(18) . . . . ? C6 N1 C1 Pd1 -18.53(14) . . . . ? C2 N1 C1 Pd1 157.79(9) . . . . ? C15 N2 C1 N1 179.56(10) . . . . ? C5 N2 C1 N1 -18.62(17) . . . . ? C15 N2 C1 Pd1 1.52(14) . . . . ? C5 N2 C1 Pd1 163.34(9) . . . . ? C24 Pd1 C1 N1 77.26(10) . . . . ? C25 Pd1 C1 N1 103.63(10) . . . . ? Cl1 Pd1 C1 N1 -94.34(9) . . . . ? C24 Pd1 C1 N2 -104.75(9) . . . . ? C25 Pd1 C1 N2 -78.37(11) . . . . ? Cl1 Pd1 C1 N2 83.66(9) . . . . ? C1 N1 C6 C7 -88.47(13) . . . . ? C2 N1 C6 C7 94.68(13) . . . . ? C1 N1 C6 C11 93.45(13) . . . . ? C2 N1 C6 C11 -83.41(13) . . . . ? C19 C18 C17 C16 -2.08(19) . . . . ? C22 C18 C17 C16 177.52(12) . . . . ? C16 C15 C20 C19 -4.85(17) . . . . ? N2 C15 C20 C19 176.48(10) . . . . ? C16 C15 C20 C23 176.07(11) . . . . ? N2 C15 C20 C23 -2.60(17) . . . . ? C11 C6 C7 C8 -4.30(17) . . . . ? N1 C6 C7 C8 177.66(10) . . . . ? C11 C6 C7 C12 175.91(11) . . . . ? N1 C6 C7 C12 -2.14(17) . . . . ? C20 C15 C16 C17 5.23(17) . . . . ? N2 C15 C16 C17 -176.09(10) . . . . ? C20 C15 C16 C21 -174.34(11) . . . . ? N2 C15 C16 C21 4.33(17) . . . . ? C18 C17 C16 C15 -1.68(18) . . . . ? C18 C17 C16 C21 177.90(12) . . . . ? C7 C6 C11 C10 4.19(17) . . . . ? N1 C6 C11 C10 -177.78(10) . . . . ? C7 C6 C11 C14 -177.10(11) . . . . ? N1 C6 C11 C14 0.93(17) . . . . ? C6 C7 C8 C9 0.73(18) . . . . ? C12 C7 C8 C9 -179.47(11) . . . . ? C7 C8 C9 C10 2.75(18) . . . . ? C7 C8 C9 C13 -178.62(12) . . . . ? C15 C20 C19 C18 0.90(18) . . . . ? C23 C20 C19 C18 179.99(12) . . . . ? C17 C18 C19 C20 2.49(19) . . . . ? C22 C18 C19 C20 -177.11(12) . . . . ? C1 N1 C2 C3 -25.55(17) . . . . ? C6 N1 C2 C3 150.87(11) . . . . ? C4 C3 C2 N1 79.75(14) . . . . ? C1 N2 C5 C4 81.73(15) . . . . ? C15 N2 C5 C4 -116.37(12) . . . . ? C8 C9 C10 C11 -2.84(19) . . . . ? C13 C9 C10 C11 178.51(12) . . . . ? C6 C11 C10 C9 -0.55(18) . . . . ? C14 C11 C10 C9 -179.26(12) . . . . ? C32 C27 C28 C29 -1.37(19) . . . . ? C26 C27 C28 C29 -179.50(12) . . . . ? C28 C27 C32 C31 1.69(19) . . . . ? C26 C27 C32 C31 179.77(12) . . . . ? C27 C28 C29 C30 0.4(2) . . . . ? C28 C29 C30 C31 0.4(2) . . . . ? N2 C5 C4 C3 -46.57(16) . . . . ? C2 C3 C4 C5 -38.18(16) . . . . ? C27 C32 C31 C30 -1.0(2) . . . . ? C29 C30 C31 C32 -0.1(2) . . . . ? C28 C27 C26 C25 -150.40(13) . . . . ? C32 C27 C26 C25 31.54(19) . . . . ? C28 C27 C26 Pd1 127.94(11) . . . . ? C32 C27 C26 Pd1 -50.13(15) . . . . ? C24 Pd1 C26 C25 30.97(8) . . . . ? Cl1 Pd1 C26 C25 -157.69(7) . . . . ? C24 Pd1 C26 C27 148.16(11) . . . . ? C25 Pd1 C26 C27 117.20(13) . . . . ? Cl1 Pd1 C26 C27 -40.49(10) . . . . ? C27 C26 C25 C24 -166.92(12) . . . . ? Pd1 C26 C25 C24 -55.77(11) . . . . ? C27 C26 C25 Pd1 -111.15(12) . . . . ? C1 Pd1 C25 C26 -174.21(7) . . . . ? C24 Pd1 C25 C26 -130.22(12) . . . . ? Cl1 Pd1 C25 C26 28.33(9) . . . . ? C1 Pd1 C25 C24 -43.99(11) . . . . ? C26 Pd1 C25 C24 130.22(12) . . . . ? Cl1 Pd1 C25 C24 158.55(7) . . . . ? C26 C25 C24 Pd1 57.85(11) . . . . ? C1 Pd1 C24 C25 149.03(8) . . . . ? C26 Pd1 C24 C25 -30.05(8) . . . . ? Cl1 Pd1 C24 C25 -54.95(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 33.24 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.821 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.090