# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Martin Broring' _publ_contact_author_email MARTIN.BROERING@CHEMIE.UNI-MARBURG.DE loop_ _publ_author_name M.Broring C.Kleeberg data_ck30ck _database_code_depnum_ccdc_archive 'CCDC 677873' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H28 N6 Pd S2' _chemical_formula_sum 'C27 H28 N6 Pd S2' _chemical_formula_weight 607.07 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' S S 0.1246 0.1234 '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_int_tables_number 14 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 10.3605(8) _cell_length_b 23.687(3) _cell_length_c 11.4803(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.311(9) _cell_angle_gamma 90.00 _cell_volume 2752.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 25.95 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.850 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.7657 _exptl_absorpt_correction_T_max 0.8562 _exptl_absorpt_process_details ; a grid of 8 x 8 x 8 = 512 sampling points was used PLATON-ABSGAUSS (1980-2003 A.L.Spek) was used for abs. correction. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'IPDS 1 (Stoe)' _diffrn_measurement_method phi-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21357 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.96 _reflns_number_total 5282 _reflns_number_gt 4332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe Expose' _computing_cell_refinement 'Stoe Cell' _computing_data_reduction 'Stoe Integrate' _computing_structure_solution 'SIR-92 (Giacovazzo, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WinGX v1.64.05' _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^)+(0.0495P)^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 5282 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 C1 C 0.2624(3) 0.42115(11) 0.2428(2) 0.0351(6) Uani 1 1 d . . . H1A H 0.2311 0.3838 0.2096 0.042 Uiso 1 1 calc R . . H1B H 0.1918 0.4383 0.2772 0.042 Uiso 1 1 calc R . . C2 C 0.2910(3) 0.45930(11) 0.1421(2) 0.0346(6) Uani 1 1 d . . . C3 C 0.3445(3) 0.42284(14) 0.0519(3) 0.0535(8) Uani 1 1 d . . . H3A H 0.3682 0.4472 -0.0094 0.080 Uiso 1 1 calc R . . H3B H 0.2764 0.3959 0.0142 0.080 Uiso 1 1 calc R . . H3C H 0.4229 0.4022 0.0933 0.080 Uiso 1 1 calc R . . C4 C 0.1662(3) 0.49034(13) 0.0782(3) 0.0485(7) Uani 1 1 d . . . H4A H 0.1361 0.5157 0.1344 0.073 Uiso 1 1 calc R . . H4B H 0.0968 0.4628 0.0473 0.073 Uiso 1 1 calc R . . H4C H 0.1860 0.5124 0.0119 0.073 Uiso 1 1 calc R . . C5 C 0.3986(2) 0.49971(10) 0.1971(2) 0.0312(5) Uani 1 1 d . . . C6 C 0.4340(3) 0.55097(11) 0.1637(2) 0.0383(6) Uani 1 1 d . . . H6 H 0.3858 0.5716 0.0976 0.046 Uiso 1 1 calc R . . C7 C 0.5858(2) 0.51301(9) 0.3402(2) 0.0267(5) Uani 1 1 d . . . C8 C 0.6977(2) 0.45937(9) 0.4999(2) 0.0256(5) Uani 1 1 d . . . C9 C 0.8197(2) 0.44744(10) 0.5886(2) 0.0280(5) Uani 1 1 d . . . C10 C 0.9374(2) 0.47701(11) 0.6185(2) 0.0321(5) Uani 1 1 d . . . H10 H 0.9475 0.5127 0.5838 0.039 Uiso 1 1 calc R . . C11 C 1.0399(3) 0.45285(12) 0.7006(2) 0.0410(6) Uani 1 1 d . . . H11 H 1.1218 0.4722 0.7227 0.049 Uiso 1 1 calc R . . C12 C 1.0244(3) 0.40093(12) 0.7506(3) 0.0427(6) Uani 1 1 d . . . H12 H 1.0965 0.3851 0.8062 0.051 Uiso 1 1 calc R . . C13 C 0.9064(3) 0.37119(11) 0.7222(2) 0.0363(6) Uani 1 1 d . . . H13 H 0.8965 0.3357 0.7578 0.044 Uiso 1 1 calc R . . C14 C 0.8031(2) 0.39525(10) 0.6395(2) 0.0297(5) Uani 1 1 d . . . C15 C 0.6670(2) 0.37697(10) 0.5834(2) 0.0274(5) Uani 1 1 d . . . C16 C 0.6621(2) 0.29164(10) 0.6807(2) 0.0313(5) Uani 1 1 d . . . C17 C 0.7390(3) 0.23182(11) 0.8516(2) 0.0403(6) Uani 1 1 d . . . H17 H 0.7632 0.2129 0.9259 0.048 Uiso 1 1 calc R . . C18 C 0.7681(2) 0.21334(10) 0.7490(2) 0.0304(5) Uani 1 1 d . . . C19 C 0.8397(3) 0.16010(12) 0.7274(3) 0.0467(7) Uani 1 1 d . . . C20 C 0.8983(4) 0.13066(15) 0.8443(3) 0.0664(10) Uani 1 1 d . . . H20A H 0.9594 0.1563 0.8958 0.100 Uiso 1 1 calc R . . H20B H 0.9460 0.0968 0.8283 0.100 Uiso 1 1 calc R . . H20C H 0.8271 0.1199 0.8841 0.100 Uiso 1 1 calc R . . C21 C 0.9472(5) 0.1750(2) 0.6617(5) 0.116(2) Uani 1 1 d . . . H21A H 1.0109 0.2005 0.7110 0.175 Uiso 1 1 calc R . . H21B H 0.9078 0.1937 0.5864 0.175 Uiso 1 1 calc R . . H21C H 0.9924 0.1405 0.6453 0.175 Uiso 1 1 calc R . . C22 C 0.7389(5) 0.12009(16) 0.6524(4) 0.0900(15) Uani 1 1 d . . . H22A H 0.7838 0.0857 0.6348 0.135 Uiso 1 1 calc R . . H22B H 0.6974 0.1387 0.5776 0.135 Uiso 1 1 calc R . . H22C H 0.6711 0.1103 0.6968 0.135 Uiso 1 1 calc R . . C23 C 0.3772(3) 0.28953(11) 0.4069(3) 0.0548(8) Uani 1 1 d . . . H23 H 0.4381 0.2852 0.3563 0.066 Uiso 1 1 calc R . . C24 C 0.3281(4) 0.24204(13) 0.4499(4) 0.0769(12) Uani 1 1 d . . . H24 H 0.3535 0.2056 0.4284 0.092 Uiso 1 1 calc R . . C25 C 0.2416(4) 0.24792(15) 0.5248(4) 0.0783(12) Uani 1 1 d . . . H25 H 0.2079 0.2157 0.5577 0.094 Uiso 1 1 calc R . . C26 C 0.2052(4) 0.30114(14) 0.5510(3) 0.0634(9) Uani 1 1 d . . . H26 H 0.1448 0.3064 0.6017 0.076 Uiso 1 1 calc R . . C27 C 0.2568(3) 0.34704(12) 0.5033(3) 0.0401(6) Uani 1 1 d . . . H27 H 0.2299 0.3838 0.5211 0.048 Uiso 1 1 calc R . . N1 N 0.48424(19) 0.47921(8) 0.29811(17) 0.0271(4) Uani 1 1 d . . . N2 N 0.6889(2) 0.50496(8) 0.43197(17) 0.0279(4) Uani 1 1 d . . . N3 N 0.6092(2) 0.41694(8) 0.49965(18) 0.0268(4) Uani 1 1 d . . . N4 N 0.6020(2) 0.33259(9) 0.60048(19) 0.0339(5) Uani 1 1 d . . . N5 N 0.7216(2) 0.24778(8) 0.65053(17) 0.0302(4) Uani 1 1 d . . . N6 N 0.3433(2) 0.34171(8) 0.4327(2) 0.0332(5) Uani 1 1 d . . . S2 S 0.65235(9) 0.29406(3) 0.82998(7) 0.04787(19) Uani 1 1 d . . . S1 S 0.57728(7) 0.57424(3) 0.25566(6) 0.03709(16) Uani 1 1 d . . . Pd1 Pd 0.426917(17) 0.411139(7) 0.372317(16) 0.02609(7) 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 C1 0.0253(13) 0.0354(13) 0.0421(14) 0.0011(11) 0.0014(12) -0.0002(10) C2 0.0254(13) 0.0437(14) 0.0323(13) -0.0001(11) 0.0010(11) 0.0063(11) C3 0.0455(19) 0.070(2) 0.0426(17) -0.0203(15) 0.0032(15) 0.0002(15) C4 0.0326(16) 0.0604(19) 0.0479(17) 0.0116(14) -0.0017(14) 0.0056(13) C5 0.0265(13) 0.0385(13) 0.0293(13) 0.0032(10) 0.0078(11) 0.0082(10) C6 0.0359(15) 0.0429(14) 0.0353(14) 0.0125(11) 0.0062(12) 0.0065(12) C7 0.0278(13) 0.0246(11) 0.0296(12) 0.0002(9) 0.0101(11) 0.0007(9) C8 0.0219(12) 0.0298(12) 0.0248(11) -0.0041(9) 0.0045(10) -0.0017(9) C9 0.0281(13) 0.0337(12) 0.0233(11) -0.0023(9) 0.0078(10) 0.0000(10) C10 0.0281(14) 0.0407(13) 0.0281(13) -0.0048(10) 0.0070(11) -0.0064(10) C11 0.0259(14) 0.0576(17) 0.0377(15) -0.0069(12) 0.0028(12) -0.0080(12) C12 0.0293(15) 0.0581(18) 0.0371(14) 0.0002(12) -0.0013(12) 0.0046(12) C13 0.0320(14) 0.0418(14) 0.0332(14) 0.0043(10) 0.0029(12) 0.0027(11) C14 0.0296(14) 0.0332(12) 0.0274(12) -0.0010(9) 0.0084(11) -0.0003(10) C15 0.0244(13) 0.0293(12) 0.0282(12) 0.0012(9) 0.0051(10) 0.0037(9) C16 0.0269(13) 0.0315(12) 0.0337(13) 0.0053(10) 0.0025(11) -0.0022(10) C17 0.0520(17) 0.0387(14) 0.0290(13) 0.0087(11) 0.0060(13) -0.0027(12) C18 0.0272(13) 0.0353(13) 0.0266(12) 0.0092(10) 0.0015(10) -0.0009(10) C19 0.0516(18) 0.0458(16) 0.0439(16) 0.0178(13) 0.0131(14) 0.0200(13) C20 0.075(3) 0.055(2) 0.063(2) 0.0271(16) 0.0022(19) 0.0193(18) C21 0.101(4) 0.123(4) 0.152(5) 0.082(4) 0.090(4) 0.079(3) C22 0.121(4) 0.051(2) 0.081(3) -0.0243(19) -0.015(3) 0.025(2) C23 0.0529(19) 0.0309(14) 0.087(2) -0.0009(14) 0.0288(18) -0.0025(13) C24 0.082(3) 0.0294(16) 0.127(4) 0.0022(18) 0.040(3) -0.0046(16) C25 0.086(3) 0.0438(19) 0.114(3) 0.019(2) 0.043(3) -0.0114(18) C26 0.068(2) 0.056(2) 0.074(2) 0.0105(17) 0.033(2) -0.0086(17) C27 0.0344(15) 0.0389(14) 0.0458(15) 0.0038(12) 0.0059(13) -0.0037(11) N1 0.0239(10) 0.0290(10) 0.0287(10) 0.0005(8) 0.0063(9) 0.0028(8) N2 0.0268(11) 0.0276(10) 0.0292(10) 0.0006(8) 0.0059(9) -0.0023(8) N3 0.0226(10) 0.0259(10) 0.0313(10) 0.0038(8) 0.0042(9) 0.0005(7) N4 0.0270(11) 0.0305(10) 0.0409(12) 0.0067(9) -0.0003(10) 0.0004(9) N5 0.0280(11) 0.0345(11) 0.0257(10) 0.0076(8) 0.0007(9) 0.0029(8) N6 0.0256(11) 0.0269(10) 0.0444(12) 0.0027(9) 0.0014(10) -0.0015(8) S2 0.0703(5) 0.0388(4) 0.0393(4) -0.0006(3) 0.0225(4) 0.0039(3) S1 0.0392(4) 0.0327(3) 0.0391(4) 0.0098(3) 0.0078(3) -0.0013(3) Pd1 0.02077(11) 0.02374(10) 0.03260(11) 0.00024(7) 0.00308(8) 0.00038(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.545(4) . ? C1 Pd1 2.022(3) . ? C2 C5 1.502(4) . ? C2 C4 1.532(4) . ? C2 C3 1.540(4) . ? C5 C6 1.348(4) . ? C5 N1 1.389(3) . ? C6 S1 1.719(3) . ? C7 N1 1.329(3) . ? C7 N2 1.344(3) . ? C7 S1 1.737(2) . ? C8 N2 1.324(3) . ? C8 N3 1.361(3) . ? C8 C9 1.471(3) . ? C9 C10 1.385(3) . ? C9 C14 1.394(3) . ? C10 C11 1.384(4) . ? C11 C12 1.381(4) . ? C12 C13 1.388(4) . ? C13 C14 1.392(4) . ? C14 C15 1.484(3) . ? C15 N4 1.285(3) . ? C15 N3 1.391(3) . ? C16 N5 1.292(3) . ? C16 N4 1.390(3) . ? C16 S2 1.740(2) . ? C17 C18 1.349(4) . ? C17 S2 1.716(3) . ? C18 N5 1.394(3) . ? C18 C19 1.510(4) . ? C19 C21 1.513(5) . ? C19 C20 1.519(4) . ? C19 C22 1.532(5) . ? C23 N6 1.335(3) . ? C23 C24 1.369(4) . ? C24 C25 1.375(5) . ? C25 C26 1.368(5) . ? C26 C27 1.375(4) . ? C27 N6 1.337(3) . ? N1 Pd1 1.9734(19) . ? N3 Pd1 2.132(2) . ? N6 Pd1 2.047(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 Pd1 110.65(17) . . ? C5 C2 C4 111.7(2) . . ? C5 C2 C3 107.4(2) . . ? C4 C2 C3 109.5(2) . . ? C5 C2 C1 107.6(2) . . ? C4 C2 C1 111.2(2) . . ? C3 C2 C1 109.2(2) . . ? C6 C5 N1 112.8(2) . . ? C6 C5 C2 132.6(2) . . ? N1 C5 C2 114.4(2) . . ? C5 C6 S1 111.5(2) . . ? N1 C7 N2 129.4(2) . . ? N1 C7 S1 110.96(18) . . ? N2 C7 S1 119.60(17) . . ? N2 C8 N3 129.7(2) . . ? N2 C8 C9 120.4(2) . . ? N3 C8 C9 109.8(2) . . ? C10 C9 C14 121.7(2) . . ? C10 C9 C8 130.9(2) . . ? C14 C9 C8 107.2(2) . . ? C11 C10 C9 117.8(2) . . ? C12 C11 C10 120.7(3) . . ? C11 C12 C13 121.9(3) . . ? C12 C13 C14 117.6(2) . . ? C13 C14 C9 120.2(2) . . ? C13 C14 C15 134.2(2) . . ? C9 C14 C15 105.5(2) . . ? N4 C15 N3 120.0(2) . . ? N4 C15 C14 130.7(2) . . ? N3 C15 C14 109.3(2) . . ? N5 C16 N4 123.7(2) . . ? N5 C16 S2 114.94(18) . . ? N4 C16 S2 121.19(18) . . ? C18 C17 S2 111.12(19) . . ? C17 C18 N5 114.5(2) . . ? C17 C18 C19 128.6(2) . . ? N5 C18 C19 116.9(2) . . ? C18 C19 C21 109.0(3) . . ? C18 C19 C20 110.8(3) . . ? C21 C19 C20 110.5(3) . . ? C18 C19 C22 108.0(3) . . ? C21 C19 C22 110.5(4) . . ? C20 C19 C22 108.0(3) . . ? N6 C23 C24 123.0(3) . . ? C23 C24 C25 118.9(3) . . ? C26 C25 C24 118.6(3) . . ? C25 C26 C27 119.5(3) . . ? N6 C27 C26 122.3(3) . . ? C7 N1 C5 114.1(2) . . ? C7 N1 Pd1 128.55(17) . . ? C5 N1 Pd1 116.64(16) . . ? C8 N2 C7 121.4(2) . . ? C8 N3 C15 108.1(2) . . ? C8 N3 Pd1 123.19(16) . . ? C15 N3 Pd1 128.19(15) . . ? C15 N4 C16 119.8(2) . . ? C16 N5 C18 110.8(2) . . ? C23 N6 C27 117.6(2) . . ? C23 N6 Pd1 121.21(19) . . ? C27 N6 Pd1 121.09(17) . . ? C17 S2 C16 88.59(12) . . ? C6 S1 C7 90.58(12) . . ? N1 Pd1 C1 82.58(9) . . ? N1 Pd1 N6 172.11(8) . . ? C1 Pd1 N6 89.55(9) . . ? N1 Pd1 N3 86.52(8) . . ? C1 Pd1 N3 168.78(9) . . ? N6 Pd1 N3 101.32(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 Pd1 C1 C2 C5 -29.9(2) . . . . ? Pd1 C1 C2 C4 -152.5(2) . . . . ? Pd1 C1 C2 C3 86.4(2) . . . . ? C4 C2 C5 C6 -34.1(4) . . . . ? C3 C2 C5 C6 86.1(3) . . . . ? C1 C2 C5 C6 -156.4(3) . . . . ? C4 C2 C5 N1 150.8(2) . . . . ? C3 C2 C5 N1 -89.0(3) . . . . ? C1 C2 C5 N1 28.5(3) . . . . ? N1 C5 C6 S1 1.3(3) . . . . ? C2 C5 C6 S1 -173.8(2) . . . . ? N2 C8 C9 C10 0.3(4) . . . . ? N3 C8 C9 C10 177.9(2) . . . . ? N2 C8 C9 C14 -175.8(2) . . . . ? N3 C8 C9 C14 1.8(2) . . . . ? C14 C9 C10 C11 0.5(3) . . . . ? C8 C9 C10 C11 -175.1(2) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? C10 C11 C12 C13 -0.6(4) . . . . ? C11 C12 C13 C14 0.7(4) . . . . ? C12 C13 C14 C9 -0.2(4) . . . . ? C12 C13 C14 C15 177.6(2) . . . . ? C10 C9 C14 C13 -0.4(3) . . . . ? C8 C9 C14 C13 176.1(2) . . . . ? C10 C9 C14 C15 -178.7(2) . . . . ? C8 C9 C14 C15 -2.2(2) . . . . ? C13 C14 C15 N4 3.5(4) . . . . ? C9 C14 C15 N4 -178.6(2) . . . . ? C13 C14 C15 N3 -176.0(2) . . . . ? C9 C14 C15 N3 2.0(2) . . . . ? S2 C17 C18 N5 -0.5(3) . . . . ? S2 C17 C18 C19 -178.4(2) . . . . ? C17 C18 C19 C21 -130.6(4) . . . . ? N5 C18 C19 C21 51.5(4) . . . . ? C17 C18 C19 C20 -8.7(4) . . . . ? N5 C18 C19 C20 173.3(3) . . . . ? C17 C18 C19 C22 109.3(4) . . . . ? N5 C18 C19 C22 -68.6(3) . . . . ? N6 C23 C24 C25 -1.1(6) . . . . ? C23 C24 C25 C26 1.7(7) . . . . ? C24 C25 C26 C27 -0.7(6) . . . . ? C25 C26 C27 N6 -0.9(5) . . . . ? N2 C7 N1 C5 -176.6(2) . . . . ? S1 C7 N1 C5 1.3(2) . . . . ? N2 C7 N1 Pd1 13.3(3) . . . . ? S1 C7 N1 Pd1 -168.82(11) . . . . ? C6 C5 N1 C7 -1.8(3) . . . . ? C2 C5 N1 C7 174.34(19) . . . . ? C6 C5 N1 Pd1 169.64(17) . . . . ? C2 C5 N1 Pd1 -14.3(2) . . . . ? N3 C8 N2 C7 -5.8(4) . . . . ? C9 C8 N2 C7 171.2(2) . . . . ? N1 C7 N2 C8 -3.5(4) . . . . ? S1 C7 N2 C8 178.70(17) . . . . ? N2 C8 N3 C15 176.7(2) . . . . ? C9 C8 N3 C15 -0.5(2) . . . . ? N2 C8 N3 Pd1 4.4(3) . . . . ? C9 C8 N3 Pd1 -172.84(14) . . . . ? N4 C15 N3 C8 179.6(2) . . . . ? C14 C15 N3 C8 -0.9(2) . . . . ? N4 C15 N3 Pd1 -8.6(3) . . . . ? C14 C15 N3 Pd1 170.94(14) . . . . ? N3 C15 N4 C16 177.3(2) . . . . ? C14 C15 N4 C16 -2.1(4) . . . . ? N5 C16 N4 C15 -93.7(3) . . . . ? S2 C16 N4 C15 90.6(3) . . . . ? N4 C16 N5 C18 -177.9(2) . . . . ? S2 C16 N5 C18 -2.0(3) . . . . ? C17 C18 N5 C16 1.6(3) . . . . ? C19 C18 N5 C16 179.8(2) . . . . ? C24 C23 N6 C27 -0.5(5) . . . . ? C24 C23 N6 Pd1 176.9(3) . . . . ? C26 C27 N6 C23 1.4(4) . . . . ? C26 C27 N6 Pd1 -176.0(3) . . . . ? C18 C17 S2 C16 -0.5(2) . . . . ? N5 C16 S2 C17 1.5(2) . . . . ? N4 C16 S2 C17 177.5(2) . . . . ? C5 C6 S1 C7 -0.5(2) . . . . ? N1 C7 S1 C6 -0.48(18) . . . . ? N2 C7 S1 C6 177.67(19) . . . . ? C7 N1 Pd1 C1 166.9(2) . . . . ? C5 N1 Pd1 C1 -3.06(17) . . . . ? C7 N1 Pd1 N6 163.6(5) . . . . ? C5 N1 Pd1 N6 -6.3(7) . . . . ? C7 N1 Pd1 N3 -10.47(19) . . . . ? C5 N1 Pd1 N3 179.59(16) . . . . ? C2 C1 Pd1 N1 18.73(17) . . . . ? C2 C1 Pd1 N6 -161.71(18) . . . . ? C2 C1 Pd1 N3 32.5(6) . . . . ? C23 N6 Pd1 N1 104.7(6) . . . . ? C27 N6 Pd1 N1 -78.0(6) . . . . ? C23 N6 Pd1 C1 101.4(2) . . . . ? C27 N6 Pd1 C1 -81.2(2) . . . . ? C23 N6 Pd1 N3 -81.3(2) . . . . ? C27 N6 Pd1 N3 96.0(2) . . . . ? C8 N3 Pd1 N1 2.67(17) . . . . ? C15 N3 Pd1 N1 -168.01(19) . . . . ? C8 N3 Pd1 C1 -11.0(5) . . . . ? C15 N3 Pd1 C1 178.4(4) . . . . ? C8 N3 Pd1 N6 -176.51(17) . . . . ? C15 N3 Pd1 N6 12.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.427 _refine_diff_density_min -0.503 _refine_diff_density_rms 0.078 _exptl_crystal_recrystallization_method 'Cryst. of (4-tBuBTI)Pd from sol. in pyridine layered by n-hexane.' # Attachment 'nh4ck_compl_neu.cif' data_nh4ck _database_code_depnum_ccdc_archive 'CCDC 677874' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H23 N5 Pd S2' _chemical_formula_sum 'C22 H23 N5 Pd S2' _chemical_formula_weight 527.97 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' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 '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/n' _symmetry_int_tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.0131(16) _cell_length_b 15.444(6) _cell_length_c 25.514(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.23(2) _cell_angle_gamma 90.00 _cell_volume 2368.8(13) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5918 _cell_measurement_theta_min 11.54 _cell_measurement_theta_max 25.03 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.283 _exptl_crystal_size_mid 0.129 _exptl_crystal_size_min 0.048 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.978 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The Dataset was obtained from a crystal comprising of two domains. Both domains could be indexed individually and were integrated generating a combined dataset (HKLF5). The BASF refined to 0.53545. Since a disordered hexane could not be described reasonable, this molecule was omitted, and a "detwinned" HKLF4 file was produced using the LIST 6 command. The resulting reflection file was treated with the SQUEEZE program, in order to generate a solvent free dataset. ; _diffrn_ambient_temperature 153(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 'IPDS-2 (Stoe)' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4079 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI 0.0612 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.96 _reflns_number_total 4079 _reflns_number_gt 3005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE WinXpose (X-Area, Ver. 1.38)' _computing_cell_refinement 'STOE Wincell (X-Area, Ver. 1.38)' _computing_data_reduction 'STOE WinIntegrate (X-Area, Ver. 1.38)' _computing_structure_solution 'SIR-92 (Giacovazzo, 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'WinGX v1.70.01' _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^)+(0.0474P)^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 4079 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _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 C1 C -0.0901(8) 0.7197(3) 0.28282(17) 0.0298(10) Uani 1 1 d . . . H1A H -0.2274 0.7414 0.2652 0.036 Uiso 1 1 calc R . . H1B H -0.0824 0.6563 0.2772 0.036 Uiso 1 1 calc R . . C2 C -0.0985(8) 0.7393(3) 0.34298(17) 0.0256(10) Uani 1 1 d . . . C3 C -0.3361(9) 0.7364(4) 0.3625(2) 0.0370(12) Uani 1 1 d . . . H3A H -0.4253 0.7808 0.3444 0.056 Uiso 1 1 calc R . . H3B H -0.3354 0.7474 0.4003 0.056 Uiso 1 1 calc R . . H3C H -0.4003 0.6792 0.3553 0.056 Uiso 1 1 calc R . . C4 C 0.0422(9) 0.6711(3) 0.37275(18) 0.0332(12) Uani 1 1 d . . . H4A H 0.0374 0.6825 0.4105 0.050 Uiso 1 1 calc R . . H4B H 0.1965 0.6741 0.3613 0.050 Uiso 1 1 calc R . . H4C H -0.0177 0.6132 0.3654 0.050 Uiso 1 1 calc R . . C5 C 0.0073(8) 0.8265(3) 0.35193(17) 0.0292(11) Uani 1 1 d . . . C6 C -0.0109(8) 0.8872(3) 0.38982(18) 0.0308(11) Uani 1 1 d . . . H6 H -0.1157 0.8851 0.4171 0.037 Uiso 1 1 calc R . . C7 C 0.2837(8) 0.9186(3) 0.32618(16) 0.0249(10) Uani 1 1 d . . . C8 C 0.5305(8) 0.9205(3) 0.25650(17) 0.0251(10) Uani 1 1 d . . . C9 C 0.7305(8) 0.9549(3) 0.23116(18) 0.0265(10) Uani 1 1 d . . . C10 C 0.8874(8) 1.0158(3) 0.24609(18) 0.0279(11) Uani 1 1 d . . . H10 H 0.8764 1.0459 0.2784 0.033 Uiso 1 1 calc R . . C11 C 1.0621(9) 1.0321(3) 0.21251(19) 0.0321(12) Uani 1 1 d . . . H11 H 1.1714 1.0741 0.2219 0.038 Uiso 1 1 calc R . . C12 C 1.0782(8) 0.9873(3) 0.16515(19) 0.0339(12) Uani 1 1 d . . . H12 H 1.1992 0.9991 0.1429 0.041 Uiso 1 1 calc R . . C13 C 0.9208(9) 0.9258(3) 0.14984(18) 0.0323(11) Uani 1 1 d . . . H13 H 0.9309 0.8960 0.1174 0.039 Uiso 1 1 calc R . . C14 C 0.7480(8) 0.9096(3) 0.18389(17) 0.0276(10) Uani 1 1 d . . . C15 C 0.5570(8) 0.8521(3) 0.17997(17) 0.0270(11) Uani 1 1 d . . . C16 C 0.3259(8) 0.7555(3) 0.13161(17) 0.0276(11) Uani 1 1 d . . . C17 C 0.0115(8) 0.6541(3) 0.13944(17) 0.0286(11) Uani 1 1 d . . . H17 H -0.1082 0.6174 0.1486 0.034 Uiso 1 1 calc R . . C18 C 0.0425(8) 0.6880(3) 0.09131(17) 0.0274(10) Uani 1 1 d . . . C19 C -0.0890(8) 0.6674(3) 0.04138(17) 0.0288(11) Uani 1 1 d . . . C20 C -0.2702(9) 0.6015(4) 0.05222(19) 0.0399(13) Uani 1 1 d . . . H20A H -0.3714 0.6249 0.0783 0.060 Uiso 1 1 calc R . . H20B H -0.2024 0.5480 0.0657 0.060 Uiso 1 1 calc R . . H20C H -0.3537 0.5890 0.0197 0.060 Uiso 1 1 calc R . . C21 C 0.0764(9) 0.6285(4) 0.00186(18) 0.0375(13) Uani 1 1 d . . . H21A H -0.0009 0.6181 -0.0317 0.056 Uiso 1 1 calc R . . H21B H 0.1355 0.5737 0.0156 0.056 Uiso 1 1 calc R . . H21C H 0.1991 0.6692 -0.0033 0.056 Uiso 1 1 calc R . . C22 C -0.1895(10) 0.7507(4) 0.0188(2) 0.0413(14) Uani 1 1 d . . . H22A H -0.2960 0.7746 0.0434 0.062 Uiso 1 1 calc R . . H22B H -0.2661 0.7379 -0.0146 0.062 Uiso 1 1 calc R . . H22C H -0.0709 0.7929 0.0130 0.062 Uiso 1 1 calc R . . N1 N 0.1689(7) 0.8481(3) 0.31586(14) 0.0252(9) Uani 1 1 d . . . N2 N 0.4600(7) 0.9530(3) 0.30142(14) 0.0270(9) Uani 1 1 d . . . N3 N 0.4348(6) 0.8568(2) 0.22575(13) 0.0243(8) Uani 1 1 d . . . N4 N 0.5092(7) 0.8078(3) 0.13754(14) 0.0309(10) Uani 1 1 d . . . N5 N 0.2204(7) 0.7455(2) 0.08704(14) 0.0274(9) Uani 1 1 d . . . S1 S 0.1819(2) 0.96926(8) 0.38202(5) 0.0331(3) Uani 1 1 d . . . S2 S 0.2223(2) 0.68762(8) 0.18192(4) 0.0293(3) Uani 1 1 d . . . Pd1 Pd 0.17999(6) 0.77733(2) 0.250965(13) 0.02426(11) 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 C1 0.032(3) 0.030(2) 0.027(2) -0.004(2) -0.0020(18) -0.001(2) C2 0.024(2) 0.027(3) 0.025(2) -0.0001(18) 0.0007(18) 0.002(2) C3 0.031(3) 0.039(3) 0.041(3) -0.002(2) 0.004(2) 0.000(2) C4 0.036(3) 0.036(3) 0.027(3) 0.001(2) -0.002(2) 0.004(2) C5 0.030(3) 0.035(3) 0.022(2) 0.002(2) -0.0042(19) 0.005(2) C6 0.033(3) 0.033(3) 0.026(2) -0.002(2) 0.005(2) 0.000(2) C7 0.028(3) 0.028(3) 0.019(2) 0.0003(18) -0.0042(18) 0.008(2) C8 0.023(3) 0.027(3) 0.026(2) 0.0031(19) -0.0047(18) 0.008(2) C9 0.029(3) 0.026(3) 0.024(2) 0.0008(18) -0.0038(19) 0.003(2) C10 0.029(3) 0.030(3) 0.024(2) -0.0011(19) -0.005(2) -0.002(2) C11 0.032(3) 0.028(3) 0.036(3) -0.004(2) -0.005(2) -0.004(2) C12 0.027(3) 0.040(3) 0.036(3) 0.001(2) 0.010(2) 0.002(2) C13 0.034(3) 0.036(3) 0.027(3) -0.005(2) 0.004(2) 0.000(2) C14 0.032(3) 0.024(2) 0.026(2) 0.0014(18) -0.0012(19) 0.001(2) C15 0.027(3) 0.026(3) 0.028(2) -0.0018(19) 0.0005(19) 0.004(2) C16 0.032(3) 0.030(3) 0.021(2) -0.0025(17) 0.0064(19) 0.002(2) C17 0.030(3) 0.031(3) 0.025(2) -0.0026(19) 0.0015(19) -0.006(2) C18 0.028(3) 0.033(3) 0.021(2) -0.0043(18) 0.0025(18) -0.002(2) C19 0.033(3) 0.033(3) 0.020(2) 0.0001(19) 0.0004(19) -0.006(2) C20 0.038(3) 0.052(4) 0.030(3) -0.004(2) -0.001(2) -0.005(3) C21 0.037(3) 0.053(3) 0.022(2) -0.008(2) 0.000(2) -0.002(3) C22 0.047(3) 0.044(3) 0.033(3) 0.001(2) -0.005(2) 0.008(3) N1 0.026(2) 0.027(2) 0.023(2) -0.0019(15) -0.0032(15) 0.0071(18) N2 0.028(2) 0.033(2) 0.020(2) -0.0009(16) 0.0004(16) -0.0014(19) N3 0.025(2) 0.027(2) 0.0208(19) -0.0031(15) -0.0021(15) -0.0012(17) N4 0.032(2) 0.037(2) 0.024(2) -0.0073(16) 0.0030(16) -0.0058(19) N5 0.033(2) 0.028(2) 0.0213(19) -0.0025(14) 0.0042(16) 0.0002(17) S1 0.0425(8) 0.0324(7) 0.0246(6) -0.0063(5) 0.0066(5) -0.0031(6) S2 0.0402(7) 0.0278(6) 0.0199(6) -0.0013(4) -0.0006(5) -0.0027(5) Pd1 0.0286(2) 0.02554(19) 0.01865(16) -0.00241(16) -0.00046(11) -0.00107(19) _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 C1 C2 1.566(6) . ? C1 Pd1 2.037(5) . ? C2 C5 1.505(7) . ? C2 C3 1.524(7) . ? C2 C4 1.541(7) . ? C5 C6 1.353(7) . ? C5 N1 1.393(6) . ? C6 S1 1.732(5) . ? C7 N1 1.313(6) . ? C7 N2 1.354(6) . ? C7 S1 1.748(4) . ? C8 N2 1.329(6) . ? C8 N3 1.377(6) . ? C8 C9 1.477(7) . ? C9 C10 1.380(7) . ? C9 C14 1.400(7) . ? C10 C11 1.393(7) . ? C11 C12 1.397(7) . ? C12 C13 1.391(7) . ? C13 C14 1.391(7) . ? C14 C15 1.454(7) . ? C15 N4 1.307(6) . ? C15 N3 1.395(6) . ? C16 N5 1.299(6) . ? C16 N4 1.373(6) . ? C16 S2 1.780(5) . ? C17 C18 1.351(6) . ? C17 S2 1.729(5) . ? C18 N5 1.397(6) . ? C18 C19 1.518(6) . ? C19 C20 1.521(7) . ? C19 C22 1.529(7) . ? C19 C21 1.552(7) . ? N1 Pd1 1.986(4) . ? N3 Pd1 2.076(4) . ? S2 Pd1 2.2599(13) . ? 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 C2 C1 Pd1 110.4(3) . . ? C5 C2 C3 111.8(4) . . ? C5 C2 C4 108.1(4) . . ? C3 C2 C4 109.1(4) . . ? C5 C2 C1 107.4(4) . . ? C3 C2 C1 111.4(4) . . ? C4 C2 C1 108.8(4) . . ? C6 C5 N1 112.0(5) . . ? C6 C5 C2 133.5(5) . . ? N1 C5 C2 114.4(4) . . ? C5 C6 S1 111.1(4) . . ? N1 C7 N2 130.2(4) . . ? N1 C7 S1 110.1(3) . . ? N2 C7 S1 119.8(4) . . ? N2 C8 N3 128.6(4) . . ? N2 C8 C9 121.3(4) . . ? N3 C8 C9 110.0(4) . . ? C10 C9 C14 121.0(5) . . ? C10 C9 C8 133.1(4) . . ? C14 C9 C8 105.9(4) . . ? C9 C10 C11 118.2(4) . . ? C10 C11 C12 120.7(5) . . ? C13 C12 C11 121.4(5) . . ? C12 C13 C14 117.4(4) . . ? C13 C14 C9 121.3(5) . . ? C13 C14 C15 131.8(4) . . ? C9 C14 C15 106.9(4) . . ? N4 C15 N3 127.6(4) . . ? N4 C15 C14 122.4(4) . . ? N3 C15 C14 109.9(4) . . ? N5 C16 N4 122.8(4) . . ? N5 C16 S2 112.9(4) . . ? N4 C16 S2 124.1(3) . . ? C18 C17 S2 109.9(4) . . ? C17 C18 N5 116.0(4) . . ? C17 C18 C19 127.0(4) . . ? N5 C18 C19 117.0(4) . . ? C18 C19 C20 110.5(4) . . ? C18 C19 C22 109.6(4) . . ? C20 C19 C22 110.6(4) . . ? C18 C19 C21 107.3(4) . . ? C20 C19 C21 109.3(4) . . ? C22 C19 C21 109.5(4) . . ? C7 N1 C5 115.9(4) . . ? C7 N1 Pd1 126.6(3) . . ? C5 N1 Pd1 117.1(3) . . ? C8 N2 C7 121.5(4) . . ? C8 N3 C15 107.0(4) . . ? C8 N3 Pd1 123.2(3) . . ? C15 N3 Pd1 129.4(3) . . ? C15 N4 C16 124.1(4) . . ? C16 N5 C18 111.5(4) . . ? C6 S1 C7 90.8(2) . . ? C17 S2 C16 89.3(2) . . ? C17 S2 Pd1 125.36(18) . . ? C16 S2 Pd1 104.37(15) . . ? N1 Pd1 C1 82.34(18) . . ? N1 Pd1 N3 88.36(15) . . ? C1 Pd1 N3 169.22(18) . . ? N1 Pd1 S2 173.47(11) . . ? C1 Pd1 S2 98.46(14) . . ? N3 Pd1 S2 91.40(11) . . ? 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 Pd1 C1 C2 C5 30.1(4) . . . . ? Pd1 C1 C2 C3 152.9(3) . . . . ? Pd1 C1 C2 C4 -86.7(4) . . . . ? C3 C2 C5 C6 33.6(7) . . . . ? C4 C2 C5 C6 -86.6(7) . . . . ? C1 C2 C5 C6 156.2(5) . . . . ? C3 C2 C5 N1 -151.3(4) . . . . ? C4 C2 C5 N1 88.5(5) . . . . ? C1 C2 C5 N1 -28.8(5) . . . . ? N1 C5 C6 S1 -2.5(5) . . . . ? C2 C5 C6 S1 172.7(4) . . . . ? N2 C8 C9 C10 5.3(8) . . . . ? N3 C8 C9 C10 -177.3(5) . . . . ? N2 C8 C9 C14 -176.8(4) . . . . ? N3 C8 C9 C14 0.6(5) . . . . ? C14 C9 C10 C11 1.0(7) . . . . ? C8 C9 C10 C11 178.6(5) . . . . ? C9 C10 C11 C12 -0.4(7) . . . . ? C10 C11 C12 C13 0.4(8) . . . . ? C11 C12 C13 C14 -0.9(8) . . . . ? C12 C13 C14 C9 1.4(7) . . . . ? C12 C13 C14 C15 178.6(5) . . . . ? C10 C9 C14 C13 -1.5(7) . . . . ? C8 C9 C14 C13 -179.7(4) . . . . ? C10 C9 C14 C15 -179.3(4) . . . . ? C8 C9 C14 C15 2.4(5) . . . . ? C13 C14 C15 N4 -5.7(8) . . . . ? C9 C14 C15 N4 171.8(5) . . . . ? C13 C14 C15 N3 177.8(5) . . . . ? C9 C14 C15 N3 -4.7(5) . . . . ? S2 C17 C18 N5 -4.4(6) . . . . ? S2 C17 C18 C19 172.8(4) . . . . ? C17 C18 C19 C20 0.5(7) . . . . ? N5 C18 C19 C20 177.8(4) . . . . ? C17 C18 C19 C22 122.7(6) . . . . ? N5 C18 C19 C22 -60.1(6) . . . . ? C17 C18 C19 C21 -118.5(6) . . . . ? N5 C18 C19 C21 58.7(6) . . . . ? N2 C7 N1 C5 174.7(4) . . . . ? S1 C7 N1 C5 -3.9(5) . . . . ? N2 C7 N1 Pd1 -12.5(7) . . . . ? S1 C7 N1 Pd1 169.0(2) . . . . ? C6 C5 N1 C7 4.3(6) . . . . ? C2 C5 N1 C7 -171.9(4) . . . . ? C6 C5 N1 Pd1 -169.3(3) . . . . ? C2 C5 N1 Pd1 14.5(5) . . . . ? N3 C8 N2 C7 6.7(7) . . . . ? C9 C8 N2 C7 -176.4(4) . . . . ? N1 C7 N2 C8 7.2(8) . . . . ? S1 C7 N2 C8 -174.3(3) . . . . ? N2 C8 N3 C15 173.6(5) . . . . ? C9 C8 N3 C15 -3.5(5) . . . . ? N2 C8 N3 Pd1 -12.7(7) . . . . ? C9 C8 N3 Pd1 170.2(3) . . . . ? N4 C15 N3 C8 -171.3(5) . . . . ? C14 C15 N3 C8 5.1(5) . . . . ? N4 C15 N3 Pd1 15.6(7) . . . . ? C14 C15 N3 Pd1 -168.1(3) . . . . ? N3 C15 N4 C16 -1.5(8) . . . . ? C14 C15 N4 C16 -177.4(4) . . . . ? N5 C16 N4 C15 146.1(5) . . . . ? S2 C16 N4 C15 -39.5(7) . . . . ? N4 C16 N5 C18 179.0(4) . . . . ? S2 C16 N5 C18 4.0(5) . . . . ? C17 C18 N5 C16 0.2(6) . . . . ? C19 C18 N5 C16 -177.3(4) . . . . ? C5 C6 S1 C7 0.3(4) . . . . ? N1 C7 S1 C6 2.0(4) . . . . ? N2 C7 S1 C6 -176.7(4) . . . . ? C18 C17 S2 C16 5.4(4) . . . . ? C18 C17 S2 Pd1 112.5(3) . . . . ? N5 C16 S2 C17 -5.5(4) . . . . ? N4 C16 S2 C17 179.5(4) . . . . ? N5 C16 S2 Pd1 -132.0(3) . . . . ? N4 C16 S2 Pd1 53.1(4) . . . . ? C7 N1 Pd1 C1 -169.7(4) . . . . ? C5 N1 Pd1 C1 3.1(3) . . . . ? C7 N1 Pd1 N3 4.8(4) . . . . ? C5 N1 Pd1 N3 177.6(3) . . . . ? C7 N1 Pd1 S2 92.8(11) . . . . ? C5 N1 Pd1 S2 -94.4(11) . . . . ? C2 C1 Pd1 N1 -18.8(3) . . . . ? C2 C1 Pd1 N3 -49.4(10) . . . . ? C2 C1 Pd1 S2 154.6(3) . . . . ? C8 N3 Pd1 N1 6.0(3) . . . . ? C15 N3 Pd1 N1 178.2(4) . . . . ? C8 N3 Pd1 C1 36.3(10) . . . . ? C15 N3 Pd1 C1 -151.5(8) . . . . ? C8 N3 Pd1 S2 -167.5(3) . . . . ? C15 N3 Pd1 S2 4.7(4) . . . . ? C17 S2 Pd1 N1 144.0(11) . . . . ? C16 S2 Pd1 N1 -116.5(11) . . . . ? C17 S2 Pd1 C1 47.4(3) . . . . ? C16 S2 Pd1 C1 146.9(2) . . . . ? C17 S2 Pd1 N3 -128.2(2) . . . . ? C16 S2 Pd1 N3 -28.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.751 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.112 _exptl_crystal_recrystallization_method 'Diffusion of n-Hexane into a sol. in CHCl3/C6F6'