# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prasenjit Ghosh' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Bombay Powai Mumbai Maharastra 400076 INDIA ; _publ_contact_author_email PGHOSH@CHEM.IITB.AC.IN loop_ _publ_author_name 'Prasenjit Ghosh' 'Raymond J. Butcher' 'Alex John' 'Mobin M. Shaikh' #=== data_pg067 _database_code_depnum_ccdc_archive 'CCDC 626720' #TrackingRef 'combined_cif_25Apr10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H58 Cl4 N10 Pd2, C2 H3 N' _chemical_formula_sum 'C44 H61 Cl4 N11 Pd2' _chemical_formula_weight 1098.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8252(1) _cell_length_b 12.8252(1) _cell_length_c 17.6659(2) _cell_angle_alpha 98.513(9) _cell_angle_beta 111.107(8) _cell_angle_gamma 107.462(8) _cell_volume 2476.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 7983 _cell_measurement_theta_min 2.9141 _cell_measurement_theta_max 32.2149 _exptl_crystal_description prism _exptl_crystal_colour yellow-orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.81964 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcaliber CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25515 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.1060 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 32.36 _reflns_number_total 13369 _reflns_number_gt 6764 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXLTL (Sheldrick, 2008)' _computing_publication_material SHELXLTL _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^)+(0.0806P)^2^] 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 13369 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1627 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _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 0.74263(4) 0.73351(3) 0.27344(2) 0.02194(10) Uani 1 1 d . . . Pd2 Pd 0.27020(4) 0.21044(3) 0.22816(2) 0.02084(10) Uani 1 1 d . . . Cl1 Cl 0.79619(13) 0.58420(11) 0.23850(7) 0.0311(3) Uani 1 1 d . . . Cl2 Cl 0.68543(14) 0.87785(11) 0.31286(8) 0.0341(3) Uani 1 1 d . . . Cl3 Cl 0.27901(13) 0.19444(11) 0.09987(7) 0.0298(3) Uani 1 1 d . . . Cl4 Cl 0.26992(13) 0.23700(12) 0.35850(8) 0.0327(3) Uani 1 1 d . . . N1 N 0.6083(4) 0.6887(3) 0.1554(2) 0.0243(9) Uani 1 1 d . . . N2 N 0.5030(4) 0.5957(3) 0.1218(2) 0.0243(9) Uani 1 1 d . . . N3 N 0.3071(4) 0.5737(3) 0.1828(2) 0.0251(9) Uani 1 1 d . . . N4 N 0.0872(4) 0.3202(3) 0.2044(3) 0.0256(9) Uani 1 1 d . . . N5 N 0.1082(4) 0.2261(3) 0.1816(2) 0.0232(9) Uani 1 1 d . . . N6 N 0.4155(4) 0.1708(3) 0.2746(2) 0.0242(9) Uani 1 1 d . . . N7 N 0.5319(4) 0.2353(3) 0.2933(2) 0.0230(9) Uani 1 1 d . . . N8 N 0.7100(4) 0.4646(4) 0.4466(2) 0.0276(10) Uani 1 1 d . . . N9 N 0.8793(4) 0.7698(4) 0.4604(2) 0.0266(10) Uani 1 1 d . . . N10 N 0.8857(4) 0.7898(3) 0.3883(2) 0.0222(9) Uani 1 1 d . . . C1 C 0.7098(6) 0.8496(5) 0.1130(4) 0.0444(16) Uani 1 1 d . . . H1A H 0.7159 0.9119 0.1559 0.067 Uiso 1 1 calc R . . H1B H 0.6980 0.8711 0.0604 0.067 Uiso 1 1 calc R . . H1C H 0.7845 0.8350 0.1334 0.067 Uiso 1 1 calc R . . C2 C 0.6038(5) 0.7431(4) 0.0963(3) 0.0299(12) Uani 1 1 d . . . C3 C 0.4958(6) 0.6838(5) 0.0246(3) 0.0347(14) Uani 1 1 d . . . H3 H 0.4708 0.7039 -0.0268 0.042 Uiso 1 1 calc R . . C4 C 0.4313(5) 0.5899(4) 0.0414(3) 0.0272(11) Uani 1 1 d . . . C5 C 0.3102(6) 0.4976(5) -0.0109(3) 0.0399(15) Uani 1 1 d . . . H5A H 0.3175 0.4233 -0.0144 0.060 Uiso 1 1 calc R . . H5B H 0.2780 0.5062 -0.0680 0.060 Uiso 1 1 calc R . . H5C H 0.2554 0.5023 0.0151 0.060 Uiso 1 1 calc R . . C6 C 0.4733(5) 0.5221(4) 0.1719(3) 0.0274(11) Uani 1 1 d . . . H6A H 0.5467 0.5107 0.2069 0.033 Uiso 1 1 calc R . . H6B H 0.4120 0.4467 0.1335 0.033 Uiso 1 1 calc R . . C7 C 0.4246(5) 0.5711(4) 0.2295(3) 0.0257(11) Uani 1 1 d . . . H7A H 0.4184 0.5243 0.2688 0.031 Uiso 1 1 calc R . . H7B H 0.4825 0.6496 0.2640 0.031 Uiso 1 1 calc R . . C8 C 0.2896(5) 0.6713(4) 0.2234(3) 0.0282(12) Uani 1 1 d . . . H8A H 0.3628 0.7411 0.2414 0.034 Uiso 1 1 calc R . . H8B H 0.2792 0.6590 0.2747 0.034 Uiso 1 1 calc R . . C9 C 0.1812(5) 0.6887(4) 0.1651(3) 0.0270(11) Uani 1 1 d . . . C10 C 0.1751(5) 0.7095(4) 0.0895(3) 0.0300(12) Uani 1 1 d . . . H10 H 0.2368 0.7079 0.0723 0.036 Uiso 1 1 calc R . . C11 C 0.0782(6) 0.7330(5) 0.0383(3) 0.0393(15) Uani 1 1 d . . . H11 H 0.0758 0.7497 -0.0127 0.047 Uiso 1 1 calc R . . C12 C -0.0142(6) 0.7321(5) 0.0612(3) 0.0370(14) Uani 1 1 d . . . H12 H -0.0804 0.7474 0.0260 0.044 Uiso 1 1 calc R . . C13 C -0.0094(6) 0.7090(5) 0.1349(4) 0.0385(14) Uani 1 1 d . . . H13 H -0.0730 0.7079 0.1508 0.046 Uiso 1 1 calc R . . C14 C 0.0860(5) 0.6874(4) 0.1864(3) 0.0311(12) Uani 1 1 d . . . H14 H 0.0874 0.6713 0.2374 0.037 Uiso 1 1 calc R . . C15 C 0.2070(5) 0.4655(4) 0.1600(3) 0.0239(10) Uani 1 1 d . . . H15A H 0.2231 0.4040 0.1311 0.029 Uiso 1 1 calc R . . H15B H 0.1323 0.4689 0.1190 0.029 Uiso 1 1 calc R . . C16 C 0.1846(5) 0.4340(4) 0.2342(3) 0.0265(11) Uani 1 1 d . . . H16A H 0.2597 0.4339 0.2772 0.032 Uiso 1 1 calc R . . H16B H 0.1615 0.4913 0.2609 0.032 Uiso 1 1 calc R . . C17 C -0.0859(7) 0.3788(5) 0.1959(4) 0.0459(16) Uani 1 1 d . . . H17A H -0.0424 0.4263 0.2550 0.069 Uiso 1 1 calc R . . H17B H -0.1715 0.3396 0.1826 0.069 Uiso 1 1 calc R . . H17C H -0.0789 0.4272 0.1585 0.069 Uiso 1 1 calc R . . C18 C -0.0322(6) 0.2918(5) 0.1829(3) 0.0313(13) Uani 1 1 d . . . C19 C -0.0889(5) 0.1757(5) 0.1477(3) 0.0299(12) Uani 1 1 d . . . H19 H -0.1725 0.1309 0.1277 0.036 Uiso 1 1 calc R . . C20 C 0.0016(5) 0.1371(4) 0.1475(3) 0.0265(11) Uani 1 1 d . . . C21 C -0.0070(6) 0.0184(5) 0.1166(4) 0.0351(13) Uani 1 1 d . . . H21A H 0.0535 0.0207 0.0946 0.053 Uiso 1 1 calc R . . H21B H -0.0880 -0.0276 0.0714 0.053 Uiso 1 1 calc R . . H21C H 0.0080 -0.0158 0.1635 0.053 Uiso 1 1 calc R . . C22 C 0.2977(6) -0.0234(5) 0.2711(4) 0.0426(15) Uani 1 1 d . . . H22A H 0.2606 0.0038 0.3055 0.064 Uiso 1 1 calc R . . H22B H 0.3144 -0.0892 0.2860 0.064 Uiso 1 1 calc R . . H22C H 0.2422 -0.0460 0.2110 0.064 Uiso 1 1 calc R . . C23 C 0.4137(5) 0.0702(4) 0.2880(3) 0.0275(12) Uani 1 1 d . . . C24 C 0.5322(6) 0.0739(5) 0.3162(3) 0.0313(13) Uani 1 1 d . . . H24 H 0.5569 0.0137 0.3300 0.038 Uiso 1 1 calc R . . C25 C 0.6062(6) 0.1789(5) 0.3206(3) 0.0312(12) Uani 1 1 d . . . C26 C 0.7377(6) 0.2283(6) 0.3442(4) 0.0453(16) Uani 1 1 d . . . H26A H 0.7506 0.2348 0.2934 0.068 Uiso 1 1 calc R . . H26B H 0.7756 0.1785 0.3698 0.068 Uiso 1 1 calc R . . H26C H 0.7740 0.3041 0.3849 0.068 Uiso 1 1 calc R . . C27 C 0.5673(5) 0.3555(4) 0.2958(3) 0.0272(11) Uani 1 1 d . . . H27A H 0.5032 0.3648 0.2486 0.033 Uiso 1 1 calc R . . H27B H 0.6426 0.3807 0.2879 0.033 Uiso 1 1 calc R . . C28 C 0.5878(5) 0.4302(4) 0.3798(3) 0.0267(11) Uani 1 1 d . . . H28A H 0.5726 0.4996 0.3704 0.032 Uiso 1 1 calc R . . H28B H 0.5285 0.3880 0.3990 0.032 Uiso 1 1 calc R . . C29 C 0.7126(6) 0.4778(5) 0.5313(3) 0.0348(14) Uani 1 1 d . . . H29A H 0.6657 0.5242 0.5386 0.042 Uiso 1 1 calc R . . H29B H 0.7971 0.5184 0.5748 0.042 Uiso 1 1 calc R . . C30 C 0.6593(5) 0.3622(4) 0.5431(3) 0.0292(12) Uani 1 1 d . . . C31 C 0.5481(6) 0.3268(5) 0.5460(3) 0.0377(14) Uani 1 1 d . . . H31 H 0.5059 0.3766 0.5428 0.045 Uiso 1 1 calc R . . C32 C 0.4974(7) 0.2185(5) 0.5536(4) 0.0457(16) Uani 1 1 d . . . H32 H 0.4206 0.1945 0.5548 0.055 Uiso 1 1 calc R . . C33 C 0.5586(7) 0.1469(5) 0.5592(3) 0.049(2) Uani 1 1 d . . . H33 H 0.5243 0.0732 0.5645 0.059 Uiso 1 1 calc R . . C34 C 0.6691(8) 0.1816(6) 0.5574(4) 0.054(2) Uani 1 1 d . . . H34 H 0.7113 0.1315 0.5621 0.064 Uiso 1 1 calc R . . C35 C 0.7211(7) 0.2879(5) 0.5487(3) 0.0414(15) Uani 1 1 d . . . H35 H 0.7974 0.3103 0.5466 0.050 Uiso 1 1 calc R . . C36 C 0.7994(5) 0.5630(4) 0.4418(3) 0.0254(11) Uani 1 1 d . . . H36A H 0.7996 0.5443 0.3854 0.030 Uiso 1 1 calc R . . H36B H 0.8806 0.5755 0.4848 0.030 Uiso 1 1 calc R . . C37 C 0.7785(5) 0.6749(4) 0.4557(3) 0.0256(11) Uani 1 1 d . . . H37A H 0.7030 0.6672 0.4085 0.031 Uiso 1 1 calc R . . H37B H 0.7689 0.6902 0.5089 0.031 Uiso 1 1 calc R . . C38 C 1.0075(6) 0.8279(6) 0.6158(3) 0.0378(14) Uani 1 1 d . . . H38A H 0.9371 0.8305 0.6247 0.057 Uiso 1 1 calc R . . H38B H 1.0802 0.8930 0.6571 0.057 Uiso 1 1 calc R . . H38C H 1.0175 0.7567 0.6230 0.057 Uiso 1 1 calc R . . C39 C 0.9889(5) 0.8334(4) 0.5279(3) 0.0276(12) Uani 1 1 d . . . C40 C 1.0630(5) 0.8954(5) 0.4987(3) 0.0306(12) Uani 1 1 d . . . H40 H 1.1441 0.9483 0.5312 0.037 Uiso 1 1 calc R . . C41 C 0.9967(5) 0.8662(4) 0.4119(3) 0.0277(11) Uani 1 1 d . . . C42 C 1.0308(6) 0.9085(5) 0.3478(4) 0.0398(14) Uani 1 1 d . . . H42A H 1.0401 0.8482 0.3128 0.060 Uiso 1 1 calc R . . H42B H 1.1075 0.9750 0.3760 0.060 Uiso 1 1 calc R . . H42C H 0.9675 0.9304 0.3118 0.060 Uiso 1 1 calc R . . C111 C 0.4170(8) 0.9616(6) 0.0935(5) 0.067(2) Uani 1 1 d . . . H11A H 0.3528 0.9881 0.0936 0.101 Uiso 1 1 calc R . . H11B H 0.4392 0.9272 0.1399 0.101 Uiso 1 1 calc R . . H11C H 0.3879 0.9047 0.0394 0.101 Uiso 1 1 calc R . . N111 N 0.6031(7) 1.1323(6) 0.1125(4) 0.0668(19) Uani 1 1 d . . . C222 C 0.5226(8) 1.0582(7) 0.1051(4) 0.0549(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0210(2) 0.01903(19) 0.02314(18) 0.00465(14) 0.00895(15) 0.00553(17) Pd2 0.0216(2) 0.01671(18) 0.02307(18) 0.00499(14) 0.00962(15) 0.00615(16) Cl1 0.0391(9) 0.0271(6) 0.0304(6) 0.0066(5) 0.0154(6) 0.0172(6) Cl2 0.0323(9) 0.0245(6) 0.0383(7) -0.0002(5) 0.0098(6) 0.0123(6) Cl3 0.0327(8) 0.0305(7) 0.0243(6) 0.0059(5) 0.0125(5) 0.0102(6) Cl4 0.0342(9) 0.0402(7) 0.0285(6) 0.0081(6) 0.0177(6) 0.0160(7) N1 0.020(3) 0.019(2) 0.026(2) 0.0039(17) 0.0061(17) 0.0013(19) N2 0.028(3) 0.020(2) 0.024(2) 0.0049(17) 0.0120(18) 0.008(2) N3 0.024(3) 0.018(2) 0.0210(19) 0.0022(16) 0.0021(17) 0.0040(19) N4 0.025(3) 0.021(2) 0.032(2) 0.0069(18) 0.0153(19) 0.007(2) N5 0.024(3) 0.017(2) 0.028(2) 0.0063(17) 0.0104(17) 0.0081(19) N6 0.027(3) 0.017(2) 0.028(2) 0.0066(17) 0.0115(18) 0.0091(19) N7 0.022(3) 0.022(2) 0.027(2) 0.0057(17) 0.0114(17) 0.010(2) N8 0.027(3) 0.027(2) 0.025(2) 0.0075(18) 0.0104(18) 0.006(2) N9 0.024(3) 0.025(2) 0.024(2) 0.0058(17) 0.0110(18) 0.001(2) N10 0.018(3) 0.025(2) 0.0235(19) 0.0063(17) 0.0101(16) 0.0078(19) C1 0.037(4) 0.043(4) 0.049(3) 0.019(3) 0.019(3) 0.007(3) C2 0.032(4) 0.026(3) 0.030(3) 0.009(2) 0.014(2) 0.007(3) C3 0.046(4) 0.035(3) 0.021(2) 0.011(2) 0.011(2) 0.018(3) C4 0.025(3) 0.028(3) 0.021(2) -0.001(2) 0.005(2) 0.008(2) C5 0.044(4) 0.029(3) 0.028(3) 0.000(2) 0.006(2) 0.003(3) C6 0.027(3) 0.019(2) 0.030(2) 0.009(2) 0.008(2) 0.006(2) C7 0.021(3) 0.024(3) 0.025(2) 0.007(2) 0.006(2) 0.002(2) C8 0.034(4) 0.016(2) 0.028(2) 0.005(2) 0.010(2) 0.005(2) C9 0.031(3) 0.015(2) 0.027(2) 0.006(2) 0.007(2) 0.006(2) C10 0.028(3) 0.030(3) 0.033(3) 0.010(2) 0.014(2) 0.010(3) C11 0.051(5) 0.029(3) 0.032(3) 0.010(2) 0.010(3) 0.016(3) C12 0.032(4) 0.026(3) 0.036(3) 0.001(2) 0.000(2) 0.010(3) C13 0.029(4) 0.023(3) 0.049(3) 0.003(3) 0.010(3) 0.003(3) C14 0.032(4) 0.021(3) 0.032(3) 0.007(2) 0.012(2) 0.003(2) C15 0.021(3) 0.023(2) 0.026(2) 0.010(2) 0.008(2) 0.007(2) C16 0.021(3) 0.022(2) 0.031(3) 0.010(2) 0.008(2) 0.005(2) C17 0.044(5) 0.035(3) 0.077(4) 0.022(3) 0.037(4) 0.023(3) C18 0.040(4) 0.031(3) 0.034(3) 0.015(2) 0.022(3) 0.017(3) C19 0.020(3) 0.027(3) 0.035(3) 0.008(2) 0.011(2) 0.001(2) C20 0.023(3) 0.019(2) 0.028(2) 0.007(2) 0.007(2) 0.000(2) C21 0.025(4) 0.026(3) 0.048(3) 0.007(2) 0.017(3) 0.002(3) C22 0.047(5) 0.025(3) 0.056(4) 0.016(3) 0.024(3) 0.011(3) C23 0.043(4) 0.019(2) 0.021(2) 0.005(2) 0.016(2) 0.011(3) C24 0.041(4) 0.031(3) 0.040(3) 0.018(2) 0.024(3) 0.026(3) C25 0.035(4) 0.040(3) 0.031(3) 0.014(2) 0.018(2) 0.023(3) C26 0.034(4) 0.064(4) 0.061(4) 0.029(3) 0.028(3) 0.034(4) C27 0.018(3) 0.027(3) 0.032(3) 0.014(2) 0.007(2) 0.005(2) C28 0.025(3) 0.017(2) 0.038(3) 0.006(2) 0.013(2) 0.009(2) C29 0.048(4) 0.030(3) 0.033(3) 0.014(2) 0.023(3) 0.014(3) C30 0.038(4) 0.027(3) 0.021(2) 0.009(2) 0.013(2) 0.009(3) C31 0.047(4) 0.034(3) 0.029(3) 0.011(2) 0.013(3) 0.015(3) C32 0.042(4) 0.039(4) 0.040(3) 0.013(3) 0.014(3) -0.002(3) C33 0.086(6) 0.028(3) 0.028(3) 0.014(2) 0.024(3) 0.011(4) C34 0.096(7) 0.044(4) 0.041(3) 0.021(3) 0.037(4) 0.040(4) C35 0.058(5) 0.045(3) 0.037(3) 0.019(3) 0.024(3) 0.032(3) C36 0.026(3) 0.023(2) 0.026(2) 0.008(2) 0.011(2) 0.006(2) C37 0.020(3) 0.025(3) 0.030(2) 0.007(2) 0.011(2) 0.006(2) C38 0.026(4) 0.053(4) 0.028(3) 0.003(3) 0.008(2) 0.015(3) C39 0.030(3) 0.027(3) 0.019(2) -0.002(2) 0.008(2) 0.009(3) C40 0.020(3) 0.025(3) 0.032(3) -0.003(2) 0.001(2) 0.007(2) C41 0.026(3) 0.018(2) 0.031(3) 0.004(2) 0.009(2) 0.003(2) C42 0.034(4) 0.039(3) 0.041(3) 0.018(3) 0.018(3) 0.002(3) C111 0.075(7) 0.055(5) 0.056(4) -0.005(4) 0.042(4) -0.003(4) N111 0.057(5) 0.078(5) 0.066(4) 0.027(4) 0.032(4) 0.017(4) C222 0.057(6) 0.060(5) 0.043(4) 0.010(3) 0.025(4) 0.013(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 N10 2.023(4) . ? Pd1 N1 2.027(4) . ? Pd1 Cl2 2.2915(13) . ? Pd1 Cl1 2.2945(12) . ? Pd2 N6 1.999(4) . ? Pd2 N5 2.025(4) . ? Pd2 Cl4 2.2788(12) . ? Pd2 Cl3 2.2916(12) . ? N1 C2 1.332(6) . ? N1 N2 1.359(6) . ? N2 C4 1.361(6) . ? N2 C6 1.447(6) . ? N3 C7 1.447(6) . ? N3 C15 1.459(7) . ? N3 C8 1.466(6) . ? N4 N5 1.349(5) . ? N4 C18 1.351(7) . ? N4 C16 1.474(7) . ? N5 C20 1.342(7) . ? N6 C23 1.340(6) . ? N6 N7 1.358(6) . ? N7 C25 1.359(6) . ? N7 C27 1.459(6) . ? N8 C28 1.464(7) . ? N8 C36 1.466(7) . ? N8 C29 1.468(6) . ? N9 N10 1.362(5) . ? N9 C39 1.371(7) . ? N9 C37 1.452(7) . ? N10 C41 1.333(7) . ? C1 C2 1.511(8) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.385(8) . ? C3 C4 1.381(8) . ? C3 H3 0.9500 . ? C4 C5 1.486(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.526(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.505(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.379(7) . ? C9 C14 1.398(8) . ? C10 C11 1.396(8) . ? C10 H10 0.9500 . ? C11 C12 1.381(9) . ? C11 H11 0.9500 . ? C12 C13 1.360(8) . ? C12 H12 0.9500 . ? C13 C14 1.370(8) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.523(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.509(8) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.372(7) . ? C19 C20 1.392(8) . ? C19 H19 0.9500 . ? C20 C21 1.497(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.500(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.402(8) . ? C24 C25 1.367(8) . ? C24 H24 0.9500 . ? C25 C26 1.482(9) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.528(7) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.515(7) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.383(8) . ? C30 C35 1.404(8) . ? C31 C32 1.394(8) . ? C31 H31 0.9500 . ? C32 C33 1.368(10) . ? C32 H32 0.9500 . ? C33 C34 1.367(10) . ? C33 H33 0.9500 . ? C34 C35 1.385(9) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.539(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.498(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.350(8) . ? C40 C41 1.384(7) . ? C40 H40 0.9500 . ? C41 C42 1.471(7) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C111 C222 1.460(11) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? N111 C222 1.123(10) . ? 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 N10 Pd1 N1 174.74(17) . . ? N10 Pd1 Cl2 90.14(12) . . ? N1 Pd1 Cl2 88.88(12) . . ? N10 Pd1 Cl1 89.04(12) . . ? N1 Pd1 Cl1 92.20(12) . . ? Cl2 Pd1 Cl1 176.95(5) . . ? N6 Pd2 N5 171.00(16) . . ? N6 Pd2 Cl4 88.65(12) . . ? N5 Pd2 Cl4 88.90(12) . . ? N6 Pd2 Cl3 90.90(12) . . ? N5 Pd2 Cl3 92.04(11) . . ? Cl4 Pd2 Cl3 176.61(5) . . ? C2 N1 N2 106.5(4) . . ? C2 N1 Pd1 128.0(4) . . ? N2 N1 Pd1 125.5(3) . . ? N1 N2 C4 111.3(4) . . ? N1 N2 C6 121.2(4) . . ? C4 N2 C6 127.4(5) . . ? C7 N3 C15 113.4(4) . . ? C7 N3 C8 113.0(4) . . ? C15 N3 C8 112.8(4) . . ? N5 N4 C18 109.9(4) . . ? N5 N4 C16 119.9(4) . . ? C18 N4 C16 129.4(4) . . ? C20 N5 N4 107.1(4) . . ? C20 N5 Pd2 123.6(3) . . ? N4 N5 Pd2 125.7(3) . . ? C23 N6 N7 106.9(4) . . ? C23 N6 Pd2 125.3(4) . . ? N7 N6 Pd2 127.7(3) . . ? N6 N7 C25 111.4(4) . . ? N6 N7 C27 120.5(4) . . ? C25 N7 C27 127.3(5) . . ? C28 N8 C36 113.4(4) . . ? C28 N8 C29 112.5(4) . . ? C36 N8 C29 113.0(4) . . ? N10 N9 C39 108.9(4) . . ? N10 N9 C37 120.4(4) . . ? C39 N9 C37 129.1(4) . . ? C41 N10 N9 106.4(4) . . ? C41 N10 Pd1 128.1(3) . . ? N9 N10 Pd1 124.7(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.5(5) . . ? N1 C2 C1 119.9(5) . . ? C3 C2 C1 130.5(5) . . ? C4 C3 C2 107.4(4) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? N2 C4 C3 105.3(5) . . ? N2 C4 C5 123.2(5) . . ? C3 C4 C5 131.5(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 C7 112.4(4) . . ? N2 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? N2 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? N3 C7 C6 112.7(4) . . ? N3 C7 H7A 109.1 . . ? C6 C7 H7A 109.1 . . ? N3 C7 H7B 109.1 . . ? C6 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N3 C8 C9 112.2(4) . . ? N3 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? N3 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C10 C9 C14 118.0(5) . . ? C10 C9 C8 120.3(5) . . ? C14 C9 C8 121.7(4) . . ? C9 C10 C11 120.1(6) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.6(5) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C13 C12 C11 119.2(5) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 120.8(6) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C9 121.2(5) . . ? C13 C14 H14 119.4 . . ? C9 C14 H14 119.4 . . ? N3 C15 C16 114.9(4) . . ? N3 C15 H15A 108.5 . . ? C16 C15 H15A 108.5 . . ? N3 C15 H15B 108.5 . . ? C16 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? N4 C16 C15 110.0(4) . . ? N4 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? N4 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 C19 107.9(5) . . ? N4 C18 C17 122.9(5) . . ? C19 C18 C17 129.2(6) . . ? C18 C19 C20 105.7(5) . . ? C18 C19 H19 127.2 . . ? C20 C19 H19 127.2 . . ? N5 C20 C19 109.4(4) . . ? N5 C20 C21 120.9(5) . . ? C19 C20 C21 129.6(5) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N6 C23 C24 108.0(5) . . ? N6 C23 C22 121.1(5) . . ? C24 C23 C22 130.9(5) . . ? C25 C24 C23 108.3(4) . . ? C25 C24 H24 125.8 . . ? C23 C24 H24 125.8 . . ? N7 C25 C24 105.3(5) . . ? N7 C25 C26 123.1(5) . . ? C24 C25 C26 131.5(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N7 C27 C28 111.6(4) . . ? N7 C27 H27A 109.3 . . ? C28 C27 H27A 109.3 . . ? N7 C27 H27B 109.3 . . ? C28 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? N8 C28 C27 113.4(4) . . ? N8 C28 H28A 108.9 . . ? C27 C28 H28A 108.9 . . ? N8 C28 H28B 108.9 . . ? C27 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? N8 C29 C30 110.4(4) . . ? N8 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? N8 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C31 C30 C35 119.0(5) . . ? C31 C30 C29 120.9(5) . . ? C35 C30 C29 120.0(6) . . ? C30 C31 C32 120.6(6) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C33 C32 C31 119.9(7) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C34 C33 C32 120.0(6) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 121.5(6) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C34 C35 C30 119.0(7) . . ? C34 C35 H35 120.5 . . ? C30 C35 H35 120.5 . . ? N8 C36 C37 115.0(4) . . ? N8 C36 H36A 108.5 . . ? C37 C36 H36A 108.5 . . ? N8 C36 H36B 108.5 . . ? C37 C36 H36B 108.5 . . ? H36A C36 H36B 107.5 . . ? N9 C37 C36 110.8(4) . . ? N9 C37 H37A 109.5 . . ? C36 C37 H37A 109.5 . . ? N9 C37 H37B 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? 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 . . ? C40 C39 N9 108.1(4) . . ? C40 C39 C38 131.5(5) . . ? N9 C39 C38 120.3(5) . . ? C39 C40 C41 106.0(5) . . ? C39 C40 H40 127.0 . . ? C41 C40 H40 127.0 . . ? N10 C41 C40 110.5(5) . . ? N10 C41 C42 119.6(5) . . ? C40 C41 C42 129.9(6) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C222 C111 H11A 109.5 . . ? C222 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C222 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? N111 C222 C111 178.8(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 N10 Pd1 N1 C2 -6(2) . . . . ? Cl2 Pd1 N1 C2 72.9(4) . . . . ? Cl1 Pd1 N1 C2 -110.0(4) . . . . ? N10 Pd1 N1 N2 174.4(16) . . . . ? Cl2 Pd1 N1 N2 -106.3(4) . . . . ? Cl1 Pd1 N1 N2 70.9(4) . . . . ? C2 N1 N2 C4 0.3(6) . . . . ? Pd1 N1 N2 C4 179.6(3) . . . . ? C2 N1 N2 C6 -174.9(4) . . . . ? Pd1 N1 N2 C6 4.5(6) . . . . ? C18 N4 N5 C20 -1.7(5) . . . . ? C16 N4 N5 C20 -172.4(4) . . . . ? C18 N4 N5 Pd2 -160.6(3) . . . . ? C16 N4 N5 Pd2 28.7(5) . . . . ? N6 Pd2 N5 C20 -18.3(12) . . . . ? Cl4 Pd2 N5 C20 -92.5(4) . . . . ? Cl3 Pd2 N5 C20 90.8(4) . . . . ? N6 Pd2 N5 N4 137.4(9) . . . . ? Cl4 Pd2 N5 N4 63.1(3) . . . . ? Cl3 Pd2 N5 N4 -113.6(3) . . . . ? N5 Pd2 N6 C23 4.0(12) . . . . ? Cl4 Pd2 N6 C23 78.2(4) . . . . ? Cl3 Pd2 N6 C23 -105.1(4) . . . . ? N5 Pd2 N6 N7 179(31) . . . . ? Cl4 Pd2 N6 N7 -106.5(4) . . . . ? Cl3 Pd2 N6 N7 70.1(4) . . . . ? C23 N6 N7 C25 -1.6(5) . . . . ? Pd2 N6 N7 C25 -177.5(3) . . . . ? C23 N6 N7 C27 -172.0(4) . . . . ? Pd2 N6 N7 C27 12.0(6) . . . . ? C39 N9 N10 C41 -1.3(5) . . . . ? C37 N9 N10 C41 -168.2(4) . . . . ? C39 N9 N10 Pd1 -171.6(3) . . . . ? C37 N9 N10 Pd1 21.5(6) . . . . ? N1 Pd1 N10 C41 -10(2) . . . . ? Cl2 Pd1 N10 C41 -89.4(4) . . . . ? Cl1 Pd1 N10 C41 93.6(4) . . . . ? N1 Pd1 N10 N9 157.9(17) . . . . ? Cl2 Pd1 N10 N9 78.7(4) . . . . ? Cl1 Pd1 N10 N9 -98.3(4) . . . . ? N2 N1 C2 C3 -0.7(6) . . . . ? Pd1 N1 C2 C3 -180.0(4) . . . . ? N2 N1 C2 C1 -178.3(5) . . . . ? Pd1 N1 C2 C1 2.4(8) . . . . ? N1 C2 C3 C4 0.8(6) . . . . ? C1 C2 C3 C4 178.1(6) . . . . ? N1 N2 C4 C3 0.2(6) . . . . ? C6 N2 C4 C3 175.0(5) . . . . ? N1 N2 C4 C5 -179.7(5) . . . . ? C6 N2 C4 C5 -4.9(8) . . . . ? C2 C3 C4 N2 -0.6(6) . . . . ? C2 C3 C4 C5 179.2(6) . . . . ? N1 N2 C6 C7 79.8(6) . . . . ? C4 N2 C6 C7 -94.5(6) . . . . ? C15 N3 C7 C6 83.6(5) . . . . ? C8 N3 C7 C6 -146.5(4) . . . . ? N2 C6 C7 N3 67.9(6) . . . . ? C7 N3 C8 C9 166.5(4) . . . . ? C15 N3 C8 C9 -63.3(5) . . . . ? N3 C8 C9 C10 -59.9(6) . . . . ? N3 C8 C9 C14 121.9(5) . . . . ? C14 C9 C10 C11 2.5(8) . . . . ? C8 C9 C10 C11 -175.8(5) . . . . ? C9 C10 C11 C12 -2.0(8) . . . . ? C10 C11 C12 C13 0.6(9) . . . . ? C11 C12 C13 C14 0.4(8) . . . . ? C12 C13 C14 C9 0.1(8) . . . . ? C10 C9 C14 C13 -1.6(8) . . . . ? C8 C9 C14 C13 176.7(5) . . . . ? C7 N3 C15 C16 69.6(6) . . . . ? C8 N3 C15 C16 -60.4(5) . . . . ? N5 N4 C16 C15 72.6(5) . . . . ? C18 N4 C16 C15 -96.0(6) . . . . ? N3 C15 C16 N4 -176.3(4) . . . . ? N5 N4 C18 C19 2.0(5) . . . . ? C16 N4 C18 C19 171.5(4) . . . . ? N5 N4 C18 C17 -176.8(5) . . . . ? C16 N4 C18 C17 -7.3(8) . . . . ? N4 C18 C19 C20 -1.4(5) . . . . ? C17 C18 C19 C20 177.2(5) . . . . ? N4 N5 C20 C19 0.8(5) . . . . ? Pd2 N5 C20 C19 160.3(3) . . . . ? N4 N5 C20 C21 -179.0(4) . . . . ? Pd2 N5 C20 C21 -19.5(6) . . . . ? C18 C19 C20 N5 0.4(5) . . . . ? C18 C19 C20 C21 -179.9(5) . . . . ? N7 N6 C23 C24 0.6(5) . . . . ? Pd2 N6 C23 C24 176.6(3) . . . . ? N7 N6 C23 C22 -178.4(4) . . . . ? Pd2 N6 C23 C22 -2.3(6) . . . . ? N6 C23 C24 C25 0.6(6) . . . . ? C22 C23 C24 C25 179.4(5) . . . . ? N6 N7 C25 C24 1.9(5) . . . . ? C27 N7 C25 C24 171.6(4) . . . . ? N6 N7 C25 C26 179.0(5) . . . . ? C27 N7 C25 C26 -11.3(8) . . . . ? C23 C24 C25 N7 -1.5(6) . . . . ? C23 C24 C25 C26 -178.3(5) . . . . ? N6 N7 C27 C28 80.9(5) . . . . ? C25 N7 C27 C28 -87.9(6) . . . . ? C36 N8 C28 C27 81.9(5) . . . . ? C29 N8 C28 C27 -148.3(4) . . . . ? N7 C27 C28 N8 85.5(5) . . . . ? C28 N8 C29 C30 72.8(6) . . . . ? C36 N8 C29 C30 -157.2(5) . . . . ? N8 C29 C30 C31 -109.1(6) . . . . ? N8 C29 C30 C35 69.1(7) . . . . ? C35 C30 C31 C32 -0.6(8) . . . . ? C29 C30 C31 C32 177.5(5) . . . . ? C30 C31 C32 C33 0.8(9) . . . . ? C31 C32 C33 C34 0.0(9) . . . . ? C32 C33 C34 C35 -0.9(9) . . . . ? C33 C34 C35 C30 1.0(9) . . . . ? C31 C30 C35 C34 -0.3(8) . . . . ? C29 C30 C35 C34 -178.4(5) . . . . ? C28 N8 C36 C37 64.4(5) . . . . ? C29 N8 C36 C37 -65.2(5) . . . . ? N10 N9 C37 C36 82.3(5) . . . . ? C39 N9 C37 C36 -81.7(6) . . . . ? N8 C36 C37 N9 172.8(4) . . . . ? N10 N9 C39 C40 1.6(6) . . . . ? C37 N9 C39 C40 167.1(5) . . . . ? N10 N9 C39 C38 180.0(4) . . . . ? C37 N9 C39 C38 -14.6(8) . . . . ? N9 C39 C40 C41 -1.3(6) . . . . ? C38 C39 C40 C41 -179.3(5) . . . . ? N9 N10 C41 C40 0.5(5) . . . . ? Pd1 N10 C41 C40 170.3(3) . . . . ? N9 N10 C41 C42 -178.1(5) . . . . ? Pd1 N10 C41 C42 -8.3(7) . . . . ? C39 C40 C41 N10 0.5(6) . . . . ? C39 C40 C41 C42 178.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.755 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.882 _refine_diff_density_max 2.730 _refine_diff_density_min -1.463 _refine_diff_density_rms 0.156 # Attachment 'combined_cif_25Apr10.txt' data_pg079a _database_code_depnum_ccdc_archive 'CCDC 630628' #TrackingRef 'combined_cif_25Apr10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H30 Cl2 N6 Pd' _chemical_formula_weight 555.82 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 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 11.6343(2) _cell_length_b 12.5462(3) _cell_length_c 16.8066(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2453.20(9) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 23176 _cell_measurement_theta_min 2.9760 _cell_measurement_theta_max 32.0906 _exptl_crystal_description prism _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7680 _exptl_absorpt_correction_T_max 0.8411 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Saphire CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37032 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 32.22 _reflns_number_total 8066 _reflns_number_gt 7284 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXLTL (Sheldrick, 2008)' _computing_publication_material SHELXLTL _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^)+(0.0445P)^2^+1.8089P] 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 -0.02(3) _refine_ls_number_reflns 8066 _refine_ls_number_parameters 259 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.458448(18) 0.780229(17) 0.850217(13) 0.01880(5) Uani 1 1 d . . . Cl1 Cl 0.54858(8) 0.89489(6) 0.93547(5) 0.02740(15) Uani 1 1 d . . . Cl2 Cl 0.62776(6) 0.72883(7) 0.79184(5) 0.02907(16) Uani 1 1 d . . . N1 N 0.3081(2) 0.8240(2) 0.90156(16) 0.0209(5) Uani 1 1 d . . . N2 N 0.2375(2) 0.8994(2) 0.87076(16) 0.0225(5) Uani 1 1 d . . . N3 N 0.2274(2) 0.8679(2) 0.72740(17) 0.0216(5) Uani 1 1 d . . . N4 N 0.3291(2) 0.7004(2) 0.70705(16) 0.0221(5) Uani 1 1 d . . . N5 N 0.3774(2) 0.6753(2) 0.77765(16) 0.0215(5) Uani 1 1 d . . . C1 C 0.3243(3) 0.7176(3) 1.0240(2) 0.0297(6) Uani 1 1 d . . . H1A H 0.4077 0.7272 1.0200 0.044 Uiso 1 1 calc R . . H1B H 0.3038 0.6453 1.0071 0.044 Uiso 1 1 calc R . . H1C H 0.3001 0.7285 1.0793 0.044 Uiso 1 1 calc R . . C2 C 0.2653(3) 0.7966(2) 0.9718(2) 0.0219(6) Uani 1 1 d . . . C3 C 0.1628(3) 0.8521(3) 0.9849(2) 0.0267(7) Uani 1 1 d . . . H3A H 0.1140 0.8464 1.0300 0.032 Uiso 1 1 calc R . . C4 C 0.1465(3) 0.9165(3) 0.9200(2) 0.0257(6) Uani 1 1 d . . . C5 C 0.0510(4) 0.9912(3) 0.9012(2) 0.0371(8) Uani 1 1 d . . . H5A H 0.0827 1.0615 0.8882 0.056 Uiso 1 1 calc R . . H5B H 0.0001 0.9974 0.9474 0.056 Uiso 1 1 calc R . . H5C H 0.0074 0.9640 0.8557 0.056 Uiso 1 1 calc R . . C6 C 0.2567(3) 0.9408(3) 0.7896(2) 0.0237(6) Uani 1 1 d . . . H6A H 0.2108 1.0066 0.7827 0.028 Uiso 1 1 calc R . . H6B H 0.3387 0.9604 0.7841 0.028 Uiso 1 1 calc R . . C7 C 0.1089(3) 0.8595(2) 0.70350(19) 0.0223(6) Uani 1 1 d . . . C8 C 0.0364(3) 0.7834(3) 0.73815(19) 0.0256(5) Uani 1 1 d . . . C9 C 0.0759(3) 0.7022(3) 0.7981(2) 0.0319(7) Uani 1 1 d . . . H9A H 0.1564 0.7158 0.8120 0.048 Uiso 1 1 calc R . . H9B H 0.0686 0.6306 0.7754 0.048 Uiso 1 1 calc R . . H9C H 0.0283 0.7075 0.8461 0.048 Uiso 1 1 calc R . . C10 C -0.0788(3) 0.7823(3) 0.7145(2) 0.0333(7) Uani 1 1 d . . . H10A H -0.1300 0.7321 0.7376 0.040 Uiso 1 1 calc R . . C11 C -0.1195(3) 0.8532(3) 0.6581(3) 0.0383(9) Uani 1 1 d . . . H11A H -0.1978 0.8502 0.6421 0.046 Uiso 1 1 calc R . . C12 C -0.0466(4) 0.9289(3) 0.6247(2) 0.0330(7) Uani 1 1 d . . . H12A H -0.0757 0.9784 0.5869 0.040 Uiso 1 1 calc R . . C13 C 0.0683(3) 0.9323(2) 0.6464(2) 0.0249(6) Uani 1 1 d . . . C14 C 0.1468(3) 1.0140(3) 0.6103(2) 0.0320(7) Uani 1 1 d . . . H14A H 0.1062 1.0521 0.5679 0.048 Uiso 1 1 calc R . . H14B H 0.2146 0.9784 0.5880 0.048 Uiso 1 1 calc R . . H14C H 0.1710 1.0647 0.6513 0.048 Uiso 1 1 calc R . . C15 C 0.3145(3) 0.8127(2) 0.6840(2) 0.0221(6) Uani 1 1 d . . . H15A H 0.3886 0.8502 0.6918 0.026 Uiso 1 1 calc R . . H15B H 0.2956 0.8159 0.6267 0.026 Uiso 1 1 calc R . . C16 C 0.2349(4) 0.6146(3) 0.5891(2) 0.0365(8) Uani 1 1 d . . . H16A H 0.2891 0.6435 0.5500 0.055 Uiso 1 1 calc R . . H16B H 0.1665 0.6601 0.5913 0.055 Uiso 1 1 calc R . . H16C H 0.2125 0.5423 0.5734 0.055 Uiso 1 1 calc R . . C17 C 0.2908(3) 0.6115(3) 0.6693(2) 0.0262(7) Uani 1 1 d . . . C18 C 0.3157(3) 0.5267(3) 0.7177(2) 0.0299(7) Uani 1 1 d . . . H18A H 0.2993 0.4538 0.7075 0.036 Uiso 1 1 calc R . . C19 C 0.3698(3) 0.5683(3) 0.7850(2) 0.0262(6) Uani 1 1 d . . . C20 C 0.4177(4) 0.5118(3) 0.8561(3) 0.0401(9) Uani 1 1 d . . . H20A H 0.4996 0.5287 0.8614 0.060 Uiso 1 1 calc R . . H20B H 0.4082 0.4348 0.8494 0.060 Uiso 1 1 calc R . . H20C H 0.3767 0.5351 0.9039 0.060 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 0.01720(8) 0.02018(8) 0.01903(9) -0.00050(8) 0.00113(8) 0.00108(9) Cl1 0.0244(3) 0.0311(4) 0.0267(4) -0.0062(3) 0.0004(3) -0.0028(3) Cl2 0.0210(3) 0.0369(4) 0.0293(4) -0.0058(3) 0.0041(3) 0.0023(3) N1 0.0175(11) 0.0224(12) 0.0227(13) -0.0008(10) 0.0012(9) -0.0015(9) N2 0.0208(12) 0.0209(11) 0.0259(14) -0.0002(10) 0.0009(9) 0.0037(9) N3 0.0207(12) 0.0204(12) 0.0238(13) -0.0016(10) 0.0009(10) 0.0000(9) N4 0.0240(12) 0.0192(13) 0.0230(13) -0.0016(9) -0.0033(10) -0.0009(9) N5 0.0215(12) 0.0194(11) 0.0236(13) 0.0009(10) 0.0006(10) 0.0028(10) C1 0.0301(15) 0.0334(16) 0.0255(16) 0.0058(16) 0.0045(12) 0.0016(16) C2 0.0192(13) 0.0210(15) 0.0255(15) 0.0006(12) -0.0001(11) 0.0002(11) C3 0.0240(15) 0.0301(16) 0.0260(16) -0.0033(13) 0.0049(12) 0.0014(13) C4 0.0239(15) 0.0265(15) 0.0267(17) -0.0039(12) 0.0040(12) 0.0022(12) C5 0.0302(18) 0.0418(19) 0.039(2) -0.0001(15) 0.0062(17) 0.0117(17) C6 0.0274(15) 0.0181(13) 0.0256(16) 0.0009(12) 0.0027(12) -0.0022(11) C7 0.0223(14) 0.0218(14) 0.0229(15) -0.0040(11) 0.0001(12) 0.0014(11) C8 0.0247(13) 0.0226(12) 0.0295(14) -0.0010(12) 0.0033(13) 0.0016(16) C9 0.0321(16) 0.0240(16) 0.0396(19) 0.0045(13) 0.0040(14) -0.0035(12) C10 0.0268(14) 0.0288(15) 0.044(2) -0.0026(18) 0.0018(13) -0.0035(15) C11 0.0227(15) 0.0398(19) 0.052(2) -0.0077(18) -0.0058(17) 0.0026(14) C12 0.0331(17) 0.0315(16) 0.0344(18) -0.0031(13) -0.0089(16) 0.0113(16) C13 0.0280(15) 0.0211(12) 0.0256(15) -0.0011(13) 0.0000(13) 0.0012(10) C14 0.0402(19) 0.0265(16) 0.0292(18) 0.0072(13) -0.0045(15) 0.0006(14) C15 0.0225(14) 0.0230(14) 0.0207(15) 0.0018(11) 0.0012(11) 0.0016(11) C16 0.040(2) 0.0371(19) 0.0320(19) -0.0028(16) -0.0111(16) -0.0038(16) C17 0.0241(15) 0.0246(14) 0.0300(18) -0.0038(12) -0.0010(12) -0.0011(12) C18 0.0356(18) 0.0193(14) 0.035(2) -0.0051(13) 0.0040(15) -0.0010(12) C19 0.0303(16) 0.0212(14) 0.0271(17) -0.0002(12) 0.0010(13) 0.0016(12) C20 0.052(2) 0.0266(16) 0.042(2) 0.0055(17) -0.0015(19) 0.0092(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.026(3) . ? Pd1 N5 2.027(3) . ? Pd1 Cl1 2.2852(8) . ? Pd1 Cl2 2.2932(8) . ? Pd1 H6B 2.8777 . ? Pd1 H15A 2.9194 . ? N1 C2 1.327(4) . ? N1 N2 1.356(4) . ? N2 C4 1.361(4) . ? N2 C6 1.476(4) . ? N3 C15 1.427(4) . ? N3 C6 1.430(4) . ? N3 C7 1.440(4) . ? N4 N5 1.351(4) . ? N4 C17 1.359(4) . ? N4 C15 1.471(4) . ? N5 C19 1.350(4) . ? C1 C2 1.490(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.399(4) . ? C3 C4 1.369(5) . ? C3 H3A 0.9500 . ? C4 C5 1.488(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.401(4) . ? C7 C13 1.407(5) . ? C8 C10 1.399(5) . ? C8 C9 1.504(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.384(6) . ? C10 H10A 0.9500 . ? C11 C12 1.392(6) . ? C11 H11A 0.9500 . ? C12 C13 1.386(5) . ? C12 H12A 0.9500 . ? C13 C14 1.500(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.498(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.370(5) . ? C18 C19 1.396(5) . ? C18 H18A 0.9500 . ? C19 C20 1.497(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 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 N1 Pd1 N5 91.78(11) . . ? N1 Pd1 Cl1 87.61(8) . . ? N5 Pd1 Cl1 178.11(8) . . ? N1 Pd1 Cl2 179.37(8) . . ? N5 Pd1 Cl2 87.67(8) . . ? Cl1 Pd1 Cl2 92.93(3) . . ? N1 Pd1 H6B 62.2 . . ? N5 Pd1 H6B 93.0 . . ? Cl1 Pd1 H6B 88.3 . . ? Cl2 Pd1 H6B 118.1 . . ? N1 Pd1 H15A 93.8 . . ? N5 Pd1 H15A 61.1 . . ? Cl1 Pd1 H15A 120.7 . . ? Cl2 Pd1 H15A 86.2 . . ? H6B Pd1 H15A 43.7 . . ? C2 N1 N2 107.1(3) . . ? C2 N1 Pd1 129.2(2) . . ? N2 N1 Pd1 123.4(2) . . ? N1 N2 C4 110.4(3) . . ? N1 N2 C6 120.4(3) . . ? C4 N2 C6 128.7(3) . . ? C15 N3 C6 121.0(3) . . ? C15 N3 C7 120.1(3) . . ? C6 N3 C7 118.6(3) . . ? N5 N4 C17 110.8(3) . . ? N5 N4 C15 120.2(3) . . ? C17 N4 C15 128.8(3) . . ? C19 N5 N4 106.6(3) . . ? C19 N5 Pd1 128.4(2) . . ? N4 N5 Pd1 124.77(19) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.3(3) . . ? N1 C2 C1 121.6(3) . . ? C3 C2 C1 129.2(3) . . ? C4 C3 C2 106.7(3) . . ? C4 C3 H3A 126.6 . . ? C2 C3 H3A 126.6 . . ? N2 C4 C3 106.5(3) . . ? N2 C4 C5 123.4(3) . . ? C3 C4 C5 130.1(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 N2 114.5(3) . . ? N3 C6 H6A 108.6 . . ? N2 C6 H6A 108.6 . . ? N3 C6 H6B 108.6 . . ? N2 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C13 121.6(3) . . ? C8 C7 N3 120.7(3) . . ? C13 C7 N3 117.6(3) . . ? C10 C8 C7 117.7(3) . . ? C10 C8 C9 118.4(3) . . ? C7 C8 C9 123.8(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C8 121.1(3) . . ? C11 C10 H10A 119.4 . . ? C8 C10 H10A 119.4 . . ? C10 C11 C12 120.4(3) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C7 118.9(3) . . ? C12 C13 C14 120.1(3) . . ? C7 C13 C14 121.0(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 N4 114.3(3) . . ? N3 C15 H15A 108.7 . . ? N4 C15 H15A 108.7 . . ? N3 C15 H15B 108.7 . . ? N4 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 C18 106.9(3) . . ? N4 C17 C16 122.8(3) . . ? C18 C17 C16 130.3(3) . . ? C17 C18 C19 106.6(3) . . ? C17 C18 H18A 126.7 . . ? C19 C18 H18A 126.7 . . ? N5 C19 C18 109.1(3) . . ? N5 C19 C20 121.2(3) . . ? C18 C19 C20 129.6(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? 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 N5 Pd1 N1 C2 102.9(3) . . . . ? Cl1 Pd1 N1 C2 -75.3(3) . . . . ? Cl2 Pd1 N1 C2 74(8) . . . . ? H6B Pd1 N1 C2 -164.6 . . . . ? H15A Pd1 N1 C2 164.0 . . . . ? N5 Pd1 N1 N2 -84.8(2) . . . . ? Cl1 Pd1 N1 N2 97.0(2) . . . . ? Cl2 Pd1 N1 N2 -114(8) . . . . ? H6B Pd1 N1 N2 7.7 . . . . ? H15A Pd1 N1 N2 -23.7 . . . . ? C2 N1 N2 C4 -2.8(3) . . . . ? Pd1 N1 N2 C4 -176.5(2) . . . . ? C2 N1 N2 C6 -175.2(3) . . . . ? Pd1 N1 N2 C6 11.0(4) . . . . ? C17 N4 N5 C19 0.0(4) . . . . ? C15 N4 N5 C19 174.7(3) . . . . ? C17 N4 N5 Pd1 174.5(2) . . . . ? C15 N4 N5 Pd1 -10.8(4) . . . . ? N1 Pd1 N5 C19 -101.4(3) . . . . ? Cl1 Pd1 N5 C19 -30(3) . . . . ? Cl2 Pd1 N5 C19 78.3(3) . . . . ? H6B Pd1 N5 C19 -163.7 . . . . ? H15A Pd1 N5 C19 165.2 . . . . ? N1 Pd1 N5 N4 85.4(2) . . . . ? Cl1 Pd1 N5 N4 156(2) . . . . ? Cl2 Pd1 N5 N4 -94.9(2) . . . . ? H6B Pd1 N5 N4 23.1 . . . . ? H15A Pd1 N5 N4 -8.0 . . . . ? N2 N1 C2 C3 2.5(3) . . . . ? Pd1 N1 C2 C3 175.7(2) . . . . ? N2 N1 C2 C1 -177.7(3) . . . . ? Pd1 N1 C2 C1 -4.4(4) . . . . ? N1 C2 C3 C4 -1.3(4) . . . . ? C1 C2 C3 C4 178.9(3) . . . . ? N1 N2 C4 C3 2.0(4) . . . . ? C6 N2 C4 C3 173.6(3) . . . . ? N1 N2 C4 C5 -177.3(3) . . . . ? C6 N2 C4 C5 -5.6(5) . . . . ? C2 C3 C4 N2 -0.4(4) . . . . ? C2 C3 C4 C5 178.7(4) . . . . ? C15 N3 C6 N2 -104.5(3) . . . . ? C7 N3 C6 N2 82.0(4) . . . . ? N1 N2 C6 N3 72.7(4) . . . . ? C4 N2 C6 N3 -98.2(4) . . . . ? C15 N3 C7 C8 94.1(4) . . . . ? C6 N3 C7 C8 -92.3(4) . . . . ? C15 N3 C7 C13 -87.9(4) . . . . ? C6 N3 C7 C13 85.7(4) . . . . ? C13 C7 C8 C10 -0.5(5) . . . . ? N3 C7 C8 C10 177.5(3) . . . . ? C13 C7 C8 C9 178.6(3) . . . . ? N3 C7 C8 C9 -3.4(5) . . . . ? C7 C8 C10 C11 0.8(5) . . . . ? C9 C8 C10 C11 -178.4(3) . . . . ? C8 C10 C11 C12 -1.3(6) . . . . ? C10 C11 C12 C13 1.5(6) . . . . ? C11 C12 C13 C7 -1.1(5) . . . . ? C11 C12 C13 C14 180.0(4) . . . . ? C8 C7 C13 C12 0.6(5) . . . . ? N3 C7 C13 C12 -177.4(3) . . . . ? C8 C7 C13 C14 179.5(3) . . . . ? N3 C7 C13 C14 1.5(5) . . . . ? C6 N3 C15 N4 103.4(3) . . . . ? C7 N3 C15 N4 -83.2(4) . . . . ? N5 N4 C15 N3 -71.7(4) . . . . ? C17 N4 C15 N3 101.9(4) . . . . ? N5 N4 C17 C18 0.0(4) . . . . ? C15 N4 C17 C18 -174.1(3) . . . . ? N5 N4 C17 C16 -179.0(3) . . . . ? C15 N4 C17 C16 6.9(5) . . . . ? N4 C17 C18 C19 -0.1(4) . . . . ? C16 C17 C18 C19 178.9(4) . . . . ? N4 N5 C19 C18 -0.1(4) . . . . ? Pd1 N5 C19 C18 -174.3(2) . . . . ? N4 N5 C19 C20 178.6(3) . . . . ? Pd1 N5 C19 C20 4.4(5) . . . . ? C17 C18 C19 N5 0.1(4) . . . . ? C17 C18 C19 C20 -178.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.623 _refine_diff_density_min -1.078 _refine_diff_density_rms 0.109 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.046 0.250 0.000 171 43 ' ' 2 -0.091 0.750 0.500 171 43 ' ' _platon_squeeze_details ; ; #=== data_pg099 _database_code_depnum_ccdc_archive 'CCDC 636906' #TrackingRef 'combined_cif_25Apr10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H29 Cl2 N5 Pd, 2(C2 H3 N)' _chemical_formula_sum 'C25 H35 Cl2 N7 Pd' _chemical_formula_weight 610.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.688(4) _cell_length_b 12.313(2) _cell_length_c 12.6717(12) _cell_angle_alpha 110.583(14) _cell_angle_beta 105.572(19) _cell_angle_gamma 101.64(2) _cell_volume 1420.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 6690 _cell_measurement_theta_min 2.9374 _cell_measurement_theta_max 32.4264 _exptl_crystal_description prism _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93033 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Saphire CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23299 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.1725 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 32.37 _reflns_number_total 9378 _reflns_number_gt 4981 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXLTL (Sheldrick, 2008)' _computing_publication_material SHELXLTL _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^)+(0.0189P)^2^] 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 9378 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 0.823 _refine_ls_restrained_S_all 0.823 _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 0.75996(2) 0.146687(17) 0.100680(16) 0.01860(6) Uani 1 1 d . . . Cl1 Cl 0.79768(6) -0.03208(5) 0.00636(5) 0.02594(14) Uani 1 1 d . . . Cl2 Cl 0.62512(6) 0.13173(5) -0.08067(5) 0.02378(14) Uani 1 1 d . . . N1 N 0.88481(19) 0.16171(15) 0.26243(15) 0.0145(4) Uani 1 1 d . . . N2 N 0.83464(19) 0.12273(16) 0.33600(16) 0.0179(4) Uani 1 1 d . . . N3 N 0.62309(18) 0.16965(16) 0.33380(15) 0.0171(4) Uani 1 1 d . . . N4 N 0.62411(19) 0.30781(16) 0.23528(16) 0.0182(4) Uani 1 1 d . . . N5 N 0.72194(18) 0.30516(16) 0.18370(15) 0.0158(4) Uani 1 1 d . . . N6 N 0.9041(3) 0.6701(2) 0.9926(2) 0.0521(7) Uani 1 1 d . . . N7 N 1.2565(2) 0.1924(2) 0.7380(2) 0.0371(6) Uani 1 1 d . . . C1 C 1.1108(2) 0.2442(2) 0.2537(2) 0.0294(6) Uani 1 1 d . . . H1A H 1.0706 0.2923 0.2156 0.044 Uiso 1 1 calc R . . H1B H 1.1178 0.1734 0.1917 0.044 Uiso 1 1 calc R . . H1C H 1.2026 0.2957 0.3148 0.044 Uiso 1 1 calc R . . C2 C 1.0214(2) 0.2007(2) 0.3130(2) 0.0209(5) Uani 1 1 d . . . C3 C 1.0600(2) 0.1881(2) 0.4218(2) 0.0238(5) Uani 1 1 d . . . H3A H 1.1511 0.2088 0.4760 0.029 Uiso 1 1 calc R . . C4 C 0.9399(2) 0.1396(2) 0.4347(2) 0.0200(5) Uani 1 1 d . . . C5 C 0.9160(3) 0.1094(2) 0.5342(2) 0.0277(6) Uani 1 1 d . . . H5A H 0.8614 0.1566 0.5683 0.042 Uiso 1 1 calc R . . H5B H 1.0047 0.1306 0.5980 0.042 Uiso 1 1 calc R . . H5C H 0.8665 0.0215 0.5011 0.042 Uiso 1 1 calc R . . C6 C 0.6858(2) 0.0767(2) 0.30628(19) 0.0181(5) Uani 1 1 d . . . H6A H 0.6407 0.0214 0.2185 0.022 Uiso 1 1 calc R . . H6B H 0.6686 0.0273 0.3511 0.022 Uiso 1 1 calc R . . C7 C 0.5474(2) 0.19608(19) 0.23979(19) 0.0183(5) Uani 1 1 d . . . H7A H 0.4619 0.2062 0.2517 0.022 Uiso 1 1 calc R . . H7B H 0.5207 0.1251 0.1607 0.022 Uiso 1 1 calc R . . C8 C 0.5233(3) 0.4547(2) 0.3464(2) 0.0390(7) Uani 1 1 d . . . H8A H 0.5347 0.4248 0.4094 0.058 Uiso 1 1 calc R . . H8B H 0.4280 0.4163 0.2885 0.058 Uiso 1 1 calc R . . H8C H 0.5453 0.5441 0.3839 0.058 Uiso 1 1 calc R . . C9 C 0.6179(2) 0.4224(2) 0.2814(2) 0.0239(5) Uani 1 1 d . . . C10 C 0.7116(3) 0.4944(2) 0.2567(2) 0.0253(6) Uani 1 1 d . . . H10A H 0.7303 0.5796 0.2777 0.030 Uiso 1 1 calc R . . C11 C 0.7742(2) 0.4188(2) 0.1948(2) 0.0213(5) Uani 1 1 d . . . C12 C 0.8793(2) 0.4471(2) 0.1435(2) 0.0290(6) Uani 1 1 d . . . H12A H 0.9473 0.4066 0.1604 0.044 Uiso 1 1 calc R . . H12B H 0.9253 0.5361 0.1805 0.044 Uiso 1 1 calc R . . H12C H 0.8347 0.4174 0.0555 0.044 Uiso 1 1 calc R . . C13 C 0.6258(2) 0.2287(2) 0.45521(19) 0.0170(5) Uani 1 1 d . . . C14 C 0.5181(2) 0.17493(19) 0.48362(19) 0.0178(5) Uani 1 1 d . . . C15 C 0.4003(2) 0.0632(2) 0.3905(2) 0.0258(6) Uani 1 1 d . . . H15A H 0.3385 0.0377 0.4285 0.039 Uiso 1 1 calc R . . H15B H 0.4352 -0.0034 0.3560 0.039 Uiso 1 1 calc R . . H15C H 0.3500 0.0819 0.3258 0.039 Uiso 1 1 calc R . . C16 C 0.5223(2) 0.2281(2) 0.6018(2) 0.0210(5) Uani 1 1 d . . . H16A H 0.4499 0.1923 0.6217 0.025 Uiso 1 1 calc R . . C17 C 0.6296(2) 0.3321(2) 0.69145(19) 0.0189(5) Uani 1 1 d . . . C18 C 0.6311(3) 0.3871(2) 0.81903(19) 0.0277(6) Uani 1 1 d . . . H18A H 0.7118 0.4611 0.8693 0.041 Uiso 1 1 calc R . . H18B H 0.6351 0.3272 0.8532 0.041 Uiso 1 1 calc R . . H18C H 0.5474 0.4086 0.8173 0.041 Uiso 1 1 calc R . . C19 C 0.7329(2) 0.3847(2) 0.6604(2) 0.0215(5) Uani 1 1 d . . . H19A H 0.8057 0.4567 0.7209 0.026 Uiso 1 1 calc R . . C20 C 0.7337(2) 0.3350(2) 0.5423(2) 0.0178(5) Uani 1 1 d . . . C21 C 0.8500(2) 0.3987(2) 0.5166(2) 0.0257(6) Uani 1 1 d . . . H21A H 0.8390 0.3523 0.4322 0.039 Uiso 1 1 calc R . . H21B H 0.9377 0.4033 0.5710 0.039 Uiso 1 1 calc R . . H21C H 0.8490 0.4818 0.5300 0.039 Uiso 1 1 calc R . . C22 C 1.0653(3) 0.8807(2) 1.1644(2) 0.0355(7) Uani 1 1 d . . . H22A H 1.1390 0.8691 1.2203 0.053 Uiso 1 1 calc R . . H22B H 1.0132 0.9216 1.2086 0.053 Uiso 1 1 calc R . . H22C H 1.1052 0.9314 1.1293 0.053 Uiso 1 1 calc R . . C23 C 0.9740(3) 0.7620(3) 1.0681(3) 0.0330(6) Uani 1 1 d . . . C24 C 1.3908(3) 0.2994(2) 0.9709(2) 0.0323(6) Uani 1 1 d . . . H24A H 1.3878 0.3834 1.0033 0.048 Uiso 1 1 calc R . . H24B H 1.4866 0.3018 0.9883 0.048 Uiso 1 1 calc R . . H24C H 1.3486 0.2537 1.0092 0.048 Uiso 1 1 calc R . . C25 C 1.3152(3) 0.2388(2) 0.8400(2) 0.0265(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02009(11) 0.01975(10) 0.01718(10) 0.00778(8) 0.00809(8) 0.00766(8) Cl1 0.0323(4) 0.0243(3) 0.0247(3) 0.0090(3) 0.0139(3) 0.0146(3) Cl2 0.0272(4) 0.0236(3) 0.0175(3) 0.0081(3) 0.0046(3) 0.0086(3) N1 0.0151(11) 0.0127(10) 0.0186(10) 0.0072(8) 0.0098(9) 0.0051(8) N2 0.0192(11) 0.0194(10) 0.0197(10) 0.0113(9) 0.0098(9) 0.0068(9) N3 0.0197(11) 0.0180(10) 0.0143(10) 0.0060(8) 0.0069(8) 0.0083(9) N4 0.0176(11) 0.0228(11) 0.0202(11) 0.0110(9) 0.0110(9) 0.0102(9) N5 0.0116(10) 0.0217(11) 0.0147(10) 0.0085(9) 0.0042(8) 0.0065(9) N6 0.0408(17) 0.0392(16) 0.0616(18) 0.0065(14) 0.0234(14) 0.0050(13) N7 0.0295(14) 0.0370(14) 0.0354(14) 0.0120(12) 0.0054(12) 0.0075(11) C1 0.0203(14) 0.0385(16) 0.0340(15) 0.0185(13) 0.0133(12) 0.0090(12) C2 0.0179(13) 0.0209(13) 0.0240(13) 0.0077(11) 0.0096(11) 0.0079(11) C3 0.0157(13) 0.0289(14) 0.0218(13) 0.0094(11) 0.0018(11) 0.0070(11) C4 0.0222(14) 0.0221(13) 0.0174(12) 0.0084(11) 0.0059(11) 0.0129(11) C5 0.0293(15) 0.0374(16) 0.0253(14) 0.0203(13) 0.0101(12) 0.0161(13) C6 0.0190(13) 0.0204(12) 0.0168(12) 0.0076(10) 0.0086(10) 0.0082(11) C7 0.0155(13) 0.0206(13) 0.0196(12) 0.0089(11) 0.0072(10) 0.0057(10) C8 0.060(2) 0.0384(17) 0.0428(17) 0.0223(14) 0.0353(16) 0.0344(16) C9 0.0268(15) 0.0241(14) 0.0263(14) 0.0125(12) 0.0107(12) 0.0151(12) C10 0.0327(15) 0.0185(13) 0.0228(14) 0.0084(11) 0.0065(12) 0.0108(12) C11 0.0207(14) 0.0192(13) 0.0195(13) 0.0094(11) 0.0017(11) 0.0033(11) C12 0.0255(15) 0.0268(14) 0.0315(15) 0.0146(12) 0.0075(12) 0.0026(12) C13 0.0181(13) 0.0190(12) 0.0181(12) 0.0103(11) 0.0080(10) 0.0084(10) C14 0.0185(13) 0.0143(12) 0.0181(12) 0.0060(10) 0.0050(10) 0.0042(10) C15 0.0258(15) 0.0219(13) 0.0266(14) 0.0067(11) 0.0137(12) 0.0029(11) C16 0.0247(14) 0.0184(13) 0.0225(13) 0.0095(11) 0.0130(11) 0.0055(11) C17 0.0252(14) 0.0174(12) 0.0170(12) 0.0080(10) 0.0085(11) 0.0103(11) C18 0.0351(16) 0.0240(14) 0.0211(13) 0.0086(11) 0.0116(12) 0.0044(12) C19 0.0192(13) 0.0180(13) 0.0210(13) 0.0056(11) 0.0027(11) 0.0049(11) C20 0.0159(13) 0.0189(12) 0.0208(13) 0.0101(11) 0.0075(10) 0.0065(10) C21 0.0219(14) 0.0230(14) 0.0278(14) 0.0084(11) 0.0093(11) 0.0031(11) C22 0.0329(17) 0.0373(17) 0.0287(15) 0.0130(14) 0.0078(13) 0.0034(14) C23 0.0293(16) 0.0370(18) 0.0395(17) 0.0199(15) 0.0182(14) 0.0108(14) C24 0.0295(16) 0.0380(16) 0.0280(15) 0.0105(13) 0.0114(13) 0.0140(13) C25 0.0222(15) 0.0213(14) 0.0396(17) 0.0140(13) 0.0157(13) 0.0066(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.0448(18) . ? Pd1 N5 2.0459(18) . ? Pd1 Cl1 2.2810(7) . ? Pd1 Cl2 2.2824(8) . ? Pd1 H6A 2.8436 . ? Pd1 H7B 2.8463 . ? N1 C2 1.331(3) . ? N1 N2 1.366(2) . ? N2 C4 1.357(3) . ? N2 C6 1.469(3) . ? N3 C6 1.426(3) . ? N3 C7 1.429(3) . ? N3 C13 1.441(3) . ? N4 C9 1.348(3) . ? N4 N5 1.374(2) . ? N4 C7 1.481(3) . ? N5 C11 1.339(3) . ? N6 C23 1.126(3) . ? N7 C25 1.136(3) . ? C1 C2 1.492(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.402(3) . ? C3 C4 1.379(3) . ? C3 H3A 0.9500 . ? C4 C5 1.501(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.495(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.376(3) . ? C10 C11 1.396(3) . ? C10 H10A 0.9500 . ? C11 C12 1.483(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C20 1.398(3) . ? C13 C14 1.405(3) . ? C14 C16 1.391(3) . ? C14 C15 1.494(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.389(3) . ? C16 H16A 0.9500 . ? C17 C19 1.384(3) . ? C17 C18 1.511(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.407(3) . ? C19 H19A 0.9500 . ? C20 C21 1.506(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.452(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C24 C25 1.459(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 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 N1 Pd1 N5 92.23(7) . . ? N1 Pd1 Cl1 88.42(5) . . ? N5 Pd1 Cl1 178.84(6) . . ? N1 Pd1 Cl2 178.65(5) . . ? N5 Pd1 Cl2 88.01(5) . . ? Cl1 Pd1 Cl2 91.36(3) . . ? N1 Pd1 H6A 62.1 . . ? N5 Pd1 H6A 94.7 . . ? Cl1 Pd1 H6A 84.8 . . ? Cl2 Pd1 H6A 119.2 . . ? N1 Pd1 H7B 94.5 . . ? N5 Pd1 H7B 62.5 . . ? Cl1 Pd1 H7B 116.5 . . ? Cl2 Pd1 H7B 86.8 . . ? H6A Pd1 H7B 44.4 . . ? C2 N1 N2 107.42(17) . . ? C2 N1 Pd1 129.93(14) . . ? N2 N1 Pd1 122.53(14) . . ? C4 N2 N1 110.08(18) . . ? C4 N2 C6 129.15(17) . . ? N1 N2 C6 120.69(17) . . ? C6 N3 C7 120.39(17) . . ? C6 N3 C13 119.31(17) . . ? C7 N3 C13 120.04(17) . . ? C9 N4 N5 110.24(17) . . ? C9 N4 C7 128.93(18) . . ? N5 N4 C7 120.76(17) . . ? C11 N5 N4 106.98(17) . . ? C11 N5 Pd1 130.77(15) . . ? N4 N5 Pd1 122.17(13) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 109.02(19) . . ? N1 C2 C1 122.1(2) . . ? C3 C2 C1 128.8(2) . . ? C4 C3 C2 106.6(2) . . ? C4 C3 H3A 126.7 . . ? C2 C3 H3A 126.7 . . ? N2 C4 C3 106.82(18) . . ? N2 C4 C5 122.2(2) . . ? C3 C4 C5 131.0(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 N2 114.83(18) . . ? N3 C6 H6A 108.6 . . ? N2 C6 H6A 108.6 . . ? N3 C6 H6B 108.6 . . ? N2 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? N3 C7 N4 113.84(17) . . ? N3 C7 H7A 108.8 . . ? N4 C7 H7A 108.8 . . ? N3 C7 H7B 108.8 . . ? N4 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C9 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N4 C9 C10 106.84(19) . . ? N4 C9 C8 122.6(2) . . ? C10 C9 C8 130.6(2) . . ? C9 C10 C11 107.2(2) . . ? C9 C10 H10A 126.4 . . ? C11 C10 H10A 126.4 . . ? N5 C11 C10 108.7(2) . . ? N5 C11 C12 121.1(2) . . ? C10 C11 C12 130.2(2) . . ? 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 . . ? C20 C13 C14 121.22(19) . . ? C20 C13 N3 120.77(18) . . ? C14 C13 N3 118.00(19) . . ? C16 C14 C13 118.6(2) . . ? C16 C14 C15 119.70(19) . . ? C13 C14 C15 121.71(19) . . ? 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 . . ? C17 C16 C14 121.8(2) . . ? C17 C16 H16A 119.1 . . ? C14 C16 H16A 119.1 . . ? C19 C17 C16 118.4(2) . . ? C19 C17 C18 121.2(2) . . ? C16 C17 C18 120.4(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 C20 122.2(2) . . ? C17 C19 H19A 118.9 . . ? C20 C19 H19A 118.9 . . ? C13 C20 C19 117.73(19) . . ? C13 C20 C21 123.69(19) . . ? C19 C20 C21 118.6(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N6 C23 C22 179.2(3) . . ? C25 C24 H24A 109.5 . . ? C25 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C25 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N7 C25 C24 179.5(3) . . ? 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 N5 Pd1 N1 C2 -101.34(19) . . . . ? Cl1 Pd1 N1 C2 79.62(19) . . . . ? Cl2 Pd1 N1 C2 -1(2) . . . . ? H6A Pd1 N1 C2 164.5 . . . . ? H7B Pd1 N1 C2 -163.9 . . . . ? N5 Pd1 N1 N2 83.09(15) . . . . ? Cl1 Pd1 N1 N2 -95.95(14) . . . . ? Cl2 Pd1 N1 N2 -177(25) . . . . ? H6A Pd1 N1 N2 -11.1 . . . . ? H7B Pd1 N1 N2 20.5 . . . . ? C2 N1 N2 C4 1.3(2) . . . . ? Pd1 N1 N2 C4 177.78(13) . . . . ? C2 N1 N2 C6 178.48(18) . . . . ? Pd1 N1 N2 C6 -5.1(2) . . . . ? C9 N4 N5 C11 -1.8(2) . . . . ? C7 N4 N5 C11 -179.04(17) . . . . ? C9 N4 N5 Pd1 -178.80(14) . . . . ? C7 N4 N5 Pd1 4.0(2) . . . . ? N1 Pd1 N5 C11 101.39(19) . . . . ? Cl1 Pd1 N5 C11 -134(2) . . . . ? Cl2 Pd1 N5 C11 -77.28(19) . . . . ? H6A Pd1 N5 C11 163.6 . . . . ? H7B Pd1 N5 C11 -164.7 . . . . ? N1 Pd1 N5 N4 -82.40(16) . . . . ? Cl1 Pd1 N5 N4 42(2) . . . . ? Cl2 Pd1 N5 N4 98.93(15) . . . . ? H6A Pd1 N5 N4 -20.2 . . . . ? H7B Pd1 N5 N4 11.5 . . . . ? N2 N1 C2 C3 -0.8(2) . . . . ? Pd1 N1 C2 C3 -176.86(14) . . . . ? N2 N1 C2 C1 176.91(19) . . . . ? Pd1 N1 C2 C1 0.8(3) . . . . ? N1 C2 C3 C4 0.0(3) . . . . ? C1 C2 C3 C4 -177.5(2) . . . . ? N1 N2 C4 C3 -1.4(2) . . . . ? C6 N2 C4 C3 -178.2(2) . . . . ? N1 N2 C4 C5 177.71(19) . . . . ? C6 N2 C4 C5 0.9(3) . . . . ? C2 C3 C4 N2 0.8(2) . . . . ? C2 C3 C4 C5 -178.1(2) . . . . ? C7 N3 C6 N2 101.7(2) . . . . ? C13 N3 C6 N2 -84.1(2) . . . . ? C4 N2 C6 N3 98.8(2) . . . . ? N1 N2 C6 N3 -77.8(2) . . . . ? C6 N3 C7 N4 -101.6(2) . . . . ? C13 N3 C7 N4 84.2(2) . . . . ? C9 N4 C7 N3 -98.1(3) . . . . ? N5 N4 C7 N3 78.6(2) . . . . ? N5 N4 C9 C10 1.3(2) . . . . ? C7 N4 C9 C10 178.3(2) . . . . ? N5 N4 C9 C8 -178.4(2) . . . . ? C7 N4 C9 C8 -1.4(4) . . . . ? N4 C9 C10 C11 -0.3(3) . . . . ? C8 C9 C10 C11 179.3(2) . . . . ? N4 N5 C11 C10 1.6(2) . . . . ? Pd1 N5 C11 C10 178.20(15) . . . . ? N4 N5 C11 C12 -177.35(19) . . . . ? Pd1 N5 C11 C12 -0.7(3) . . . . ? C9 C10 C11 N5 -0.8(3) . . . . ? C9 C10 C11 C12 178.0(2) . . . . ? C6 N3 C13 C20 90.3(2) . . . . ? C7 N3 C13 C20 -95.5(2) . . . . ? C6 N3 C13 C14 -88.7(2) . . . . ? C7 N3 C13 C14 85.6(2) . . . . ? C20 C13 C14 C16 -1.5(3) . . . . ? N3 C13 C14 C16 177.42(19) . . . . ? C20 C13 C14 C15 178.4(2) . . . . ? N3 C13 C14 C15 -2.7(3) . . . . ? C13 C14 C16 C17 0.0(3) . . . . ? C15 C14 C16 C17 -179.9(2) . . . . ? C14 C16 C17 C19 1.3(3) . . . . ? C14 C16 C17 C18 -179.7(2) . . . . ? C16 C17 C19 C20 -1.2(3) . . . . ? C18 C17 C19 C20 179.9(2) . . . . ? C14 C13 C20 C19 1.6(3) . . . . ? N3 C13 C20 C19 -177.24(19) . . . . ? C14 C13 C20 C21 -178.4(2) . . . . ? N3 C13 C20 C21 2.7(3) . . . . ? C17 C19 C20 C13 -0.3(3) . . . . ? C17 C19 C20 C21 179.7(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C5 H5B N7 0.98 2.58 3.544(4) 169.5 . C6 H6A Cl2 0.99 2.74 3.479(3) 131.3 2_655 C18 H18A N6 0.98 2.57 3.543(4) 172.8 . C18 H18B Cl2 0.98 2.80 3.778(2) 172.3 1_556 C22 H22C Cl1 0.98 2.74 3.707(2) 169.2 2_766 _diffrn_measured_fraction_theta_max 0.922 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.435 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.090 #=== data_pg100 _database_code_depnum_ccdc_archive 'CCDC 636907' #TrackingRef 'combined_cif_25Apr10.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H24 Cl2 N5 Pd' _chemical_formula_sum 'C19 H24 Cl2 N5 Pd' _chemical_formula_weight 499.73 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 c m n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x, -y-1/2, z' _cell_length_a 8.1966(2) _cell_length_b 13.6939(3) _cell_length_c 18.0046(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2020.90(8) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8677 _cell_measurement_theta_min 2.9721 _cell_measurement_theta_max 32.4887 _exptl_crystal_description prism _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1012 _exptl_absorpt_coefficient_mu 1.197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94097 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcaliber' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19997 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 32.58 _reflns_number_total 3588 _reflns_number_gt 2761 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXLTL (Sheldrick, 2008)' _computing_publication_material SHELXLTL _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^)+(0.0358P)^2^] 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 3588 _refine_ls_number_parameters 138 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.16196(2) 0.7500 0.277075(10) 0.01510(6) Uani 1 2 d S . . Cl1 Cl 0.18518(6) 0.87088(3) 0.36405(2) 0.02213(10) Uani 1 1 d . . . N1 N 0.13354(18) 0.64491(12) 0.19927(8) 0.0175(3) Uani 1 1 d . . . N2 N 0.25005(19) 0.61940(11) 0.14892(8) 0.0181(3) Uani 1 1 d . . . N3 N 0.4473(3) 0.7500 0.11809(12) 0.0229(5) Uani 1 2 d S . . C1 C -0.1465(2) 0.59542(16) 0.23436(11) 0.0247(4) Uani 1 1 d . . . H1A H -0.1177 0.5893 0.2870 0.037 Uiso 1 1 calc R . . H1B H -0.2224 0.5431 0.2207 0.037 Uiso 1 1 calc R . . H1C H -0.1984 0.6589 0.2258 0.037 Uiso 1 1 calc R . . C2 C 0.0046(2) 0.58771(14) 0.18802(10) 0.0199(4) Uani 1 1 d . . . C3 C 0.0387(2) 0.52430(14) 0.12922(10) 0.0233(4) Uani 1 1 d . . . H3A H -0.0323 0.4761 0.1093 0.028 Uiso 1 1 calc R . . C4 C 0.1938(2) 0.54497(14) 0.10583(10) 0.0213(4) Uani 1 1 d . . . C5 C 0.2921(3) 0.49896(15) 0.04545(11) 0.0291(5) Uani 1 1 d . . . H5A H 0.3943 0.4737 0.0661 0.044 Uiso 1 1 calc R . . H5B H 0.3165 0.5478 0.0073 0.044 Uiso 1 1 calc R . . H5C H 0.2300 0.4452 0.0233 0.044 Uiso 1 1 calc R . . C6 C 0.4162(2) 0.65981(14) 0.15440(10) 0.0214(4) Uani 1 1 d . . . H6A H 0.4423 0.6681 0.2077 0.026 Uiso 1 1 calc R . . H6B H 0.4930 0.6107 0.1342 0.026 Uiso 1 1 calc R . . C7 C 0.4688(3) 0.7500 0.03721(14) 0.0230(6) Uani 1 2 d S . . H7A H 0.4158 0.8066 0.0170 0.028 Uiso 0.50 1 d PR . . C8 C 0.6460(3) 0.7500 0.01281(14) 0.0171(5) Uani 1 2 d S . . C9 C 0.6805(3) 0.7500 -0.06341(15) 0.0232(6) Uani 1 2 d S . . H9A H 0.5932 0.7500 -0.0981 0.028 Uiso 1 2 calc SR . . C10 C 0.8410(3) 0.7500 -0.08906(16) 0.0270(6) Uani 1 2 d S . . H10A H 0.8628 0.7500 -0.1409 0.032 Uiso 1 2 calc SR . . C11 C 0.9704(3) 0.7500 -0.03785(16) 0.0268(6) Uani 1 2 d S . . H11A H 1.0802 0.7500 -0.0547 0.032 Uiso 1 2 calc SR . . C12 C 0.9360(3) 0.7500 0.03726(15) 0.0243(6) Uani 1 2 d S . . H12A H 1.0229 0.7500 0.0722 0.029 Uiso 1 2 calc SR . . C13 C 0.7757(3) 0.7500 0.06231(15) 0.0220(6) Uani 1 2 d S . . H13A H 0.7546 0.7500 0.1142 0.026 Uiso 1 2 calc SR . . 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 0.01452(9) 0.01769(10) 0.01308(10) 0.000 0.00066(7) 0.000 Cl1 0.0269(2) 0.0221(2) 0.0174(2) -0.00298(16) -0.00057(17) -0.00399(18) N1 0.0174(7) 0.0209(8) 0.0142(7) -0.0001(6) 0.0002(6) -0.0001(6) N2 0.0182(7) 0.0214(8) 0.0149(7) -0.0008(6) 0.0021(6) 0.0028(6) N3 0.0224(11) 0.0285(13) 0.0176(11) 0.000 0.0080(9) 0.000 C1 0.0196(9) 0.0275(10) 0.0271(11) -0.0013(8) 0.0031(8) -0.0044(8) C2 0.0211(9) 0.0204(9) 0.0182(9) 0.0010(7) -0.0018(7) 0.0003(8) C3 0.0287(10) 0.0203(9) 0.0210(9) -0.0012(7) -0.0032(8) -0.0016(8) C4 0.0303(10) 0.0193(9) 0.0143(9) 0.0000(7) -0.0009(7) 0.0037(8) C5 0.0421(12) 0.0234(10) 0.0217(10) -0.0030(8) 0.0074(9) 0.0037(9) C6 0.0161(8) 0.0268(10) 0.0212(9) 0.0006(8) 0.0014(7) 0.0049(8) C7 0.0156(12) 0.0359(16) 0.0176(13) 0.000 0.0021(10) 0.000 C8 0.0173(12) 0.0142(11) 0.0197(12) 0.000 0.0028(10) 0.000 C9 0.0226(14) 0.0264(14) 0.0205(13) 0.000 0.0003(10) 0.000 C10 0.0258(14) 0.0324(16) 0.0228(14) 0.000 0.0056(12) 0.000 C11 0.0197(13) 0.0299(16) 0.0309(16) 0.000 0.0060(11) 0.000 C12 0.0206(13) 0.0288(15) 0.0235(14) 0.000 -0.0042(11) 0.000 C13 0.0243(13) 0.0271(14) 0.0147(13) 0.000 0.0015(10) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.0217(15) . ? Pd1 N1 2.0217(15) 8_575 ? Pd1 Cl1 2.2866(5) . ? Pd1 Cl1 2.2866(5) 8_575 ? Pd1 H6A 2.8458 . ? N1 C2 1.331(2) . ? N1 N2 1.362(2) . ? N2 C4 1.361(2) . ? N2 C6 1.473(2) . ? N3 C6 1.420(2) 8_575 ? N3 C6 1.420(2) . ? N3 C7 1.467(3) . ? C1 C2 1.497(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.397(3) . ? C3 C4 1.369(3) . ? C3 H3A 0.9500 . ? C4 C5 1.493(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.517(3) . ? C7 H7A 0.9601 . ? C8 C13 1.388(4) . ? C8 C9 1.401(4) . ? C9 C10 1.395(4) . ? C9 H9A 0.9500 . ? C10 C11 1.405(4) . ? C10 H10A 0.9500 . ? C11 C12 1.381(4) . ? C11 H11A 0.9500 . ? C12 C13 1.389(4) . ? C12 H12A 0.9500 . ? C13 H13A 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 N1 Pd1 N1 90.76(9) . 8_575 ? N1 Pd1 Cl1 177.99(4) . . ? N1 Pd1 Cl1 88.21(5) 8_575 . ? N1 Pd1 Cl1 88.21(5) . 8_575 ? N1 Pd1 Cl1 177.99(4) 8_575 8_575 ? Cl1 Pd1 Cl1 92.76(2) . 8_575 ? N1 Pd1 H6A 60.6 . . ? N1 Pd1 H6A 94.0 8_575 . ? Cl1 Pd1 H6A 121.2 . . ? Cl1 Pd1 H6A 87.0 8_575 . ? C2 N1 N2 107.71(15) . . ? C2 N1 Pd1 128.02(12) . . ? N2 N1 Pd1 124.25(12) . . ? C4 N2 N1 109.50(15) . . ? C4 N2 C6 129.23(15) . . ? N1 N2 C6 120.46(14) . . ? C6 N3 C6 120.8(2) 8_575 . ? C6 N3 C7 118.58(11) 8_575 . ? C6 N3 C7 118.58(11) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C3 108.82(16) . . ? N1 C2 C1 122.05(16) . . ? C3 C2 C1 129.13(18) . . ? C4 C3 C2 106.86(17) . . ? C4 C3 H3A 126.6 . . ? C2 C3 H3A 126.6 . . ? N2 C4 C3 107.10(16) . . ? N2 C4 C5 123.25(18) . . ? C3 C4 C5 129.65(19) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 N2 117.48(17) . . ? N3 C6 H6A 107.9 . . ? N2 C6 H6A 107.9 . . ? N3 C6 H6B 107.9 . . ? N2 C6 H6B 107.9 . . ? H6A C6 H6B 107.2 . . ? N3 C7 C8 113.7(2) . . ? N3 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C13 C8 C9 118.3(2) . . ? C13 C8 C7 123.2(2) . . ? C9 C8 C7 118.5(2) . . ? C10 C9 C8 121.0(3) . . ? C10 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C9 C10 C11 119.7(3) . . ? C9 C10 H10A 120.2 . . ? C11 C10 H10A 120.2 . . ? C12 C11 C10 119.2(3) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C13 120.7(3) . . ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 . . ? C8 C13 C12 121.1(2) . . ? C8 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 N1 C2 -105.74(15) 8_575 . . . ? Cl1 Pd1 N1 C2 -46.2(14) . . . . ? Cl1 Pd1 N1 C2 72.52(16) 8_575 . . . ? H6A Pd1 N1 C2 160.1 . . . . ? N1 Pd1 N1 N2 75.62(14) 8_575 . . . ? Cl1 Pd1 N1 N2 135.1(12) . . . . ? Cl1 Pd1 N1 N2 -106.12(13) 8_575 . . . ? H6A Pd1 N1 N2 -18.5 . . . . ? C2 N1 N2 C4 -0.3(2) . . . . ? Pd1 N1 N2 C4 178.56(12) . . . . ? C2 N1 N2 C6 -170.99(16) . . . . ? Pd1 N1 N2 C6 7.9(2) . . . . ? N2 N1 C2 C3 -0.1(2) . . . . ? Pd1 N1 C2 C3 -178.93(12) . . . . ? N2 N1 C2 C1 179.52(16) . . . . ? Pd1 N1 C2 C1 0.7(3) . . . . ? N1 C2 C3 C4 0.5(2) . . . . ? C1 C2 C3 C4 -179.11(19) . . . . ? N1 N2 C4 C3 0.6(2) . . . . ? C6 N2 C4 C3 170.22(17) . . . . ? N1 N2 C4 C5 -179.41(17) . . . . ? C6 N2 C4 C5 -9.8(3) . . . . ? C2 C3 C4 N2 -0.7(2) . . . . ? C2 C3 C4 C5 179.4(2) . . . . ? C6 N3 C6 N2 86.6(3) 8_575 . . . ? C7 N3 C6 N2 -76.9(2) . . . . ? C4 N2 C6 N3 103.3(2) . . . . ? N1 N2 C6 N3 -88.1(2) . . . . ? C6 N3 C7 C8 98.02(18) 8_575 . . . ? C6 N3 C7 C8 -98.02(18) . . . . ? N3 C7 C8 C13 0.0 . . . . ? N3 C7 C8 C9 180.0 . . . . ? C13 C8 C9 C10 0.0 . . . . ? C7 C8 C9 C10 180.0 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C9 C8 C13 C12 0.0 . . . . ? C7 C8 C13 C12 180.0 . . . . ? C11 C12 C13 C8 0.0 . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.729 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.090