# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email ctchen@mail.nchu.edu.tw _publ_contact_author_name 'Chi-Tien Chen' loop_ _publ_author_name 'Chi-Tien Chen' 'Wei-Chi Wang' 'Kuo-Fu Peng' 'Ming-Tsz Chen' data_Compound5 _database_code_depnum_ccdc_archive 'CCDC 829869' #TrackingRef '- BenzamidineCNSPd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H26 N2 O2 Pd S' _chemical_formula_sum 'C21 H26 N2 O2 Pd S' _chemical_formula_weight 476.90 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' O O 0.0106 0.0060 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4397(11) _cell_length_b 13.6472(12) _cell_length_c 14.2697(12) _cell_angle_alpha 83.055(2) _cell_angle_beta 66.2150(10) _cell_angle_gamma 75.150(2) _cell_volume 2142.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 9145 _cell_measurement_theta_min 2.657 _cell_measurement_theta_max 26.013 _exptl_crystal_description parallelplpiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.981 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7573 _exptl_absorpt_correction_T_max 0.9083 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12004 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 26.02 _reflns_number_total 8253 _reflns_number_gt 7444 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0545P)^2^+1.1957P] 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 8253 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.764174(15) 0.536967(13) 0.513420(13) 0.03464(7) Uani 1 1 d . . . Pd2 Pd 0.708471(16) 0.991079(14) 0.035572(14) 0.03796(7) Uani 1 1 d . . . O1 O 0.75789(18) 0.50139(14) 0.38112(14) 0.0462(4) Uani 1 1 d . . . O2 O 0.86532(19) 0.61331(17) 0.28820(15) 0.0562(5) Uani 1 1 d . . . O3 O 0.75882(17) 1.12662(14) -0.00235(15) 0.0490(4) Uani 1 1 d . . . O4 O 0.58049(19) 1.21295(16) 0.10542(18) 0.0603(5) Uani 1 1 d . . . S1 S 0.64600(6) 0.70738(5) 0.51178(5) 0.04204(14) Uani 1 1 d . . . S2 S 0.69282(6) 0.99229(5) 0.21048(5) 0.04749(16) Uani 1 1 d . . . N1 N 0.93690(18) 0.44858(16) 0.64008(15) 0.0394(4) Uani 1 1 d . . . H1A H 0.9982 0.4354 0.6569 0.047 Uiso 1 1 calc R . . N2 N 0.76969(18) 0.57401(16) 0.64237(15) 0.0386(4) Uani 1 1 d . . . N3 N 0.57753(19) 0.86507(16) -0.04816(17) 0.0421(5) Uani 1 1 d . . . H3A H 0.5205 0.8501 -0.0591 0.051 Uiso 1 1 calc R . . N4 N 0.65682(19) 0.86005(16) 0.07469(17) 0.0429(5) Uani 1 1 d . . . C1 C 0.8542(2) 0.53488(19) 0.67667(18) 0.0368(5) Uani 1 1 d . . . C2 C 0.8683(2) 0.5787(2) 0.76119(19) 0.0426(5) Uani 1 1 d . . . C3 C 0.8803(3) 0.6771(2) 0.7556(3) 0.0579(7) Uani 1 1 d . . . H3B H 0.8775 0.7187 0.6996 0.069 Uiso 1 1 calc R . . C4 C 0.8967(3) 0.7136(3) 0.8355(4) 0.0800(12) Uani 1 1 d . . . H4A H 0.9048 0.7799 0.8329 0.096 Uiso 1 1 calc R . . C5 C 0.9008(4) 0.6509(4) 0.9179(3) 0.0918(15) Uani 1 1 d . . . H5A H 0.9119 0.6751 0.9708 0.110 Uiso 1 1 calc R . . C6 C 0.8887(4) 0.5536(4) 0.9227(3) 0.0864(13) Uani 1 1 d . . . H6A H 0.8910 0.5122 0.9789 0.104 Uiso 1 1 calc R . . C7 C 0.8732(3) 0.5168(3) 0.8452(2) 0.0605(8) Uani 1 1 d . . . H7A H 0.8659 0.4502 0.8485 0.073 Uiso 1 1 calc R . . C8 C 0.9350(2) 0.37696(18) 0.57730(18) 0.0379(5) Uani 1 1 d . . . C9 C 0.8622(2) 0.39883(18) 0.52124(17) 0.0369(5) Uani 1 1 d . . . C10 C 0.8632(2) 0.3186(2) 0.4681(2) 0.0455(6) Uani 1 1 d . . . H10A H 0.8151 0.3304 0.4304 0.055 Uiso 1 1 calc R . . C11 C 0.9332(3) 0.2228(2) 0.4699(2) 0.0555(7) Uani 1 1 d . . . H11A H 0.9296 0.1705 0.4358 0.067 Uiso 1 1 calc R . . C12 C 1.0084(3) 0.2045(2) 0.5221(2) 0.0565(7) Uani 1 1 d . . . H12A H 1.0580 0.1405 0.5213 0.068 Uiso 1 1 calc R . . C13 C 1.0101(3) 0.2813(2) 0.5755(2) 0.0498(6) Uani 1 1 d . . . H13A H 1.0614 0.2693 0.6104 0.060 Uiso 1 1 calc R . . C14 C 0.6659(2) 0.6547(2) 0.69968(19) 0.0450(6) Uani 1 1 d . . . H14A H 0.6807 0.6772 0.7544 0.054 Uiso 1 1 calc R . . H14B H 0.5940 0.6278 0.7304 0.054 Uiso 1 1 calc R . . C15 C 0.6454(3) 0.7439(2) 0.6299(2) 0.0473(6) Uani 1 1 d . . . H15A H 0.7078 0.7810 0.6136 0.057 Uiso 1 1 calc R . . H15B H 0.5684 0.7892 0.6662 0.057 Uiso 1 1 calc R . . C16 C 0.4867(2) 0.7056(2) 0.5406(2) 0.0527(7) Uani 1 1 d . . . C17 C 0.4922(3) 0.6587(3) 0.4471(3) 0.0682(9) Uani 1 1 d . . . H17A H 0.4125 0.6550 0.4563 0.102 Uiso 1 1 calc R . . H17B H 0.5433 0.5917 0.4384 0.102 Uiso 1 1 calc R . . H17C H 0.5242 0.6997 0.3874 0.102 Uiso 1 1 calc R . . C18 C 0.4340(3) 0.6449(4) 0.6362(3) 0.0786(11) Uani 1 1 d . . . H18A H 0.3520 0.6460 0.6480 0.118 Uiso 1 1 calc R . . H18B H 0.4358 0.6739 0.6934 0.118 Uiso 1 1 calc R . . H18C H 0.4804 0.5762 0.6281 0.118 Uiso 1 1 calc R . . C19 C 0.4155(4) 0.8155(3) 0.5484(4) 0.0851(12) Uani 1 1 d . . . H19A H 0.3326 0.8172 0.5634 0.128 Uiso 1 1 calc R . . H19B H 0.4486 0.8506 0.4846 0.128 Uiso 1 1 calc R . . H19C H 0.4206 0.8477 0.6022 0.128 Uiso 1 1 calc R . . C20 C 0.8059(2) 0.5502(2) 0.29850(19) 0.0425(6) Uani 1 1 d . . . C21 C 0.7836(3) 0.5242(3) 0.2091(2) 0.0642(8) Uani 1 1 d . . . H21A H 0.8217 0.5632 0.1498 0.096 Uiso 1 1 calc R . . H21B H 0.6983 0.5394 0.2254 0.096 Uiso 1 1 calc R . . H21C H 0.8166 0.4532 0.1952 0.096 Uiso 1 1 calc R . . C22 C 0.5916(2) 0.82781(18) 0.0382(2) 0.0412(5) Uani 1 1 d . . . C23 C 0.5254(2) 0.74675(19) 0.0921(2) 0.0450(6) Uani 1 1 d . . . C24 C 0.4297(3) 0.7682(3) 0.1853(3) 0.0618(8) Uani 1 1 d . . . H24A H 0.4079 0.8322 0.2126 0.074 Uiso 1 1 calc R . . C25 C 0.3661(4) 0.6964(3) 0.2382(3) 0.0799(11) Uani 1 1 d . . . H25A H 0.3007 0.7123 0.3001 0.096 Uiso 1 1 calc R . . C26 C 0.3993(4) 0.6025(3) 0.1995(4) 0.0912(14) Uani 1 1 d . . . H26A H 0.3576 0.5534 0.2359 0.109 Uiso 1 1 calc R . . C27 C 0.4945(4) 0.5790(3) 0.1065(4) 0.0887(13) Uani 1 1 d . . . H27A H 0.5164 0.5142 0.0808 0.106 Uiso 1 1 calc R . . C28 C 0.5584(3) 0.6522(2) 0.0505(3) 0.0665(8) Uani 1 1 d . . . H28A H 0.6212 0.6374 -0.0130 0.080 Uiso 1 1 calc R . . C29 C 0.6458(2) 0.92603(18) -0.12298(19) 0.0396(5) Uani 1 1 d . . . C30 C 0.7162(2) 0.98041(19) -0.1040(2) 0.0404(5) Uani 1 1 d . . . C31 C 0.7919(2) 1.0281(2) -0.1891(2) 0.0501(6) Uani 1 1 d . . . H31A H 0.8413 1.0634 -0.1795 0.060 Uiso 1 1 calc R . . C32 C 0.7950(3) 1.0240(3) -0.2865(2) 0.0612(8) Uani 1 1 d . . . H32A H 0.8487 1.0534 -0.3418 0.073 Uiso 1 1 calc R . . C33 C 0.7178(3) 0.9762(2) -0.3012(2) 0.0595(7) Uani 1 1 d . . . H33A H 0.7166 0.9762 -0.3659 0.071 Uiso 1 1 calc R . . C34 C 0.6426(3) 0.9282(2) -0.2198(2) 0.0511(6) Uani 1 1 d . . . H34A H 0.5895 0.8972 -0.2295 0.061 Uiso 1 1 calc R . . C35 C 0.6868(3) 0.8042(2) 0.1592(2) 0.0513(6) Uani 1 1 d . . . H35A H 0.7732 0.7767 0.1351 0.062 Uiso 1 1 calc R . . H35B H 0.6473 0.7480 0.1815 0.062 Uiso 1 1 calc R . . C36 C 0.6474(3) 0.8724(2) 0.2485(2) 0.0558(7) Uani 1 1 d . . . H36A H 0.6816 0.8375 0.2970 0.067 Uiso 1 1 calc R . . H36B H 0.5602 0.8859 0.2830 0.067 Uiso 1 1 calc R . . C37 C 0.8466(3) 0.9677(2) 0.2118(3) 0.0575(7) Uani 1 1 d . . . C38 C 0.9318(3) 0.8773(3) 0.1472(4) 0.0854(12) Uani 1 1 d . . . H38A H 1.0099 0.8671 0.1497 0.128 Uiso 1 1 calc R . . H38B H 0.9386 0.8899 0.0776 0.128 Uiso 1 1 calc R . . H38C H 0.9006 0.8178 0.1735 0.128 Uiso 1 1 calc R . . C39 C 0.8868(4) 1.0656(3) 0.1689(4) 0.0858(12) Uani 1 1 d . . . H39A H 0.9664 1.0597 0.1666 0.129 Uiso 1 1 calc R . . H39B H 0.8318 1.1207 0.2120 0.129 Uiso 1 1 calc R . . H39C H 0.8875 1.0782 0.1010 0.129 Uiso 1 1 calc R . . C40 C 0.8351(4) 0.9510(3) 0.3219(3) 0.0803(11) Uani 1 1 d . . . H40A H 0.9136 0.9382 0.3242 0.120 Uiso 1 1 calc R . . H40B H 0.7998 0.8940 0.3510 0.120 Uiso 1 1 calc R . . H40C H 0.7846 1.0105 0.3604 0.120 Uiso 1 1 calc R . . C41 C 0.6860(3) 1.2064(2) 0.0449(2) 0.0494(6) Uani 1 1 d . . . C42 C 0.7401(4) 1.2985(3) 0.0212(4) 0.0858(13) Uani 1 1 d . . . H42C H 0.6807 1.3552 0.0590 0.129 Uiso 1 1 calc R . . H42D H 0.7655 1.3143 -0.0509 0.129 Uiso 1 1 calc R . . H42A H 0.8083 1.2845 0.0402 0.129 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 0.03562(11) 0.03880(11) 0.03169(10) -0.00042(7) -0.01562(8) -0.00807(8) Pd2 0.03559(11) 0.03740(11) 0.04511(12) 0.00256(8) -0.01900(8) -0.01144(8) O1 0.0554(11) 0.0498(10) 0.0411(9) -0.0024(8) -0.0263(8) -0.0117(8) O2 0.0562(12) 0.0693(13) 0.0485(11) 0.0036(9) -0.0227(9) -0.0216(10) O3 0.0498(10) 0.0423(10) 0.0595(11) 0.0040(8) -0.0223(9) -0.0186(8) O4 0.0486(11) 0.0569(12) 0.0786(15) -0.0082(11) -0.0252(11) -0.0135(9) S1 0.0453(3) 0.0399(3) 0.0437(3) 0.0010(2) -0.0214(3) -0.0083(3) S2 0.0459(3) 0.0515(4) 0.0486(4) -0.0006(3) -0.0244(3) -0.0074(3) N1 0.0378(10) 0.0450(11) 0.0395(10) -0.0005(9) -0.0196(9) -0.0092(9) N2 0.0373(10) 0.0435(11) 0.0353(10) -0.0026(8) -0.0154(8) -0.0069(8) N3 0.0378(10) 0.0440(11) 0.0491(12) 0.0000(9) -0.0185(9) -0.0147(9) N4 0.0443(11) 0.0386(11) 0.0495(12) 0.0051(9) -0.0216(10) -0.0126(9) C1 0.0365(12) 0.0434(13) 0.0309(11) 0.0025(9) -0.0126(9) -0.0123(10) C2 0.0377(12) 0.0532(15) 0.0382(12) -0.0064(11) -0.0165(10) -0.0073(11) C3 0.0516(16) 0.0623(18) 0.0674(19) -0.0109(14) -0.0289(14) -0.0118(13) C4 0.060(2) 0.083(3) 0.106(3) -0.050(2) -0.035(2) -0.0028(18) C5 0.068(2) 0.142(4) 0.071(2) -0.056(3) -0.040(2) 0.014(2) C6 0.087(3) 0.124(4) 0.0426(17) -0.021(2) -0.0333(18) 0.007(2) C7 0.0632(18) 0.078(2) 0.0359(14) -0.0003(13) -0.0219(13) -0.0051(15) C8 0.0359(11) 0.0408(12) 0.0337(11) 0.0016(9) -0.0105(9) -0.0095(10) C9 0.0366(11) 0.0395(12) 0.0325(11) 0.0025(9) -0.0118(9) -0.0092(9) C10 0.0485(14) 0.0473(14) 0.0456(14) -0.0040(11) -0.0224(12) -0.0109(11) C11 0.0681(19) 0.0432(14) 0.0586(17) -0.0079(12) -0.0283(15) -0.0092(13) C12 0.0642(18) 0.0429(15) 0.0622(18) -0.0023(13) -0.0307(15) -0.0010(13) C13 0.0517(15) 0.0471(14) 0.0515(15) 0.0005(12) -0.0266(13) -0.0026(12) C14 0.0423(13) 0.0533(15) 0.0402(13) -0.0097(11) -0.0184(11) -0.0042(11) C15 0.0497(15) 0.0425(14) 0.0548(15) -0.0094(12) -0.0254(13) -0.0067(11) C16 0.0403(14) 0.0634(18) 0.0576(16) -0.0099(13) -0.0242(12) -0.0044(12) C17 0.0570(18) 0.092(2) 0.070(2) -0.0171(18) -0.0387(17) -0.0095(17) C18 0.0567(19) 0.124(3) 0.069(2) 0.008(2) -0.0283(17) -0.042(2) C19 0.067(2) 0.084(3) 0.102(3) -0.029(2) -0.045(2) 0.0200(19) C20 0.0425(13) 0.0458(13) 0.0383(13) -0.0061(10) -0.0200(11) 0.0008(11) C21 0.085(2) 0.076(2) 0.0404(15) -0.0036(14) -0.0311(15) -0.0205(18) C22 0.0348(12) 0.0367(12) 0.0516(14) -0.0022(10) -0.0162(11) -0.0076(10) C23 0.0424(13) 0.0395(13) 0.0590(16) 0.0066(11) -0.0244(12) -0.0152(10) C24 0.0505(16) 0.0611(18) 0.0677(19) 0.0057(15) -0.0145(15) -0.0195(14) C25 0.069(2) 0.089(3) 0.083(3) 0.026(2) -0.0249(19) -0.040(2) C26 0.088(3) 0.080(3) 0.121(4) 0.044(3) -0.051(3) -0.050(2) C27 0.105(3) 0.0412(17) 0.140(4) 0.011(2) -0.066(3) -0.0255(19) C28 0.066(2) 0.0446(16) 0.092(2) -0.0078(15) -0.0336(18) -0.0119(14) C29 0.0343(12) 0.0386(12) 0.0433(13) -0.0052(10) -0.0132(10) -0.0049(9) C30 0.0342(12) 0.0408(13) 0.0467(13) 0.0016(10) -0.0172(10) -0.0078(10) C31 0.0432(14) 0.0547(16) 0.0544(16) 0.0059(12) -0.0185(12) -0.0188(12) C32 0.0566(17) 0.071(2) 0.0493(16) 0.0056(14) -0.0110(13) -0.0224(15) C33 0.0695(19) 0.0645(19) 0.0430(15) -0.0040(13) -0.0190(14) -0.0158(15) C34 0.0536(16) 0.0519(15) 0.0498(15) -0.0096(12) -0.0194(13) -0.0124(12) C35 0.0528(15) 0.0473(15) 0.0620(17) 0.0132(12) -0.0312(14) -0.0168(12) C36 0.0573(17) 0.0662(19) 0.0519(16) 0.0146(14) -0.0270(14) -0.0253(14) C37 0.0531(16) 0.0586(17) 0.074(2) -0.0006(14) -0.0400(15) -0.0103(13) C38 0.0439(17) 0.101(3) 0.113(3) -0.027(2) -0.0309(19) -0.0058(18) C39 0.086(3) 0.088(3) 0.120(3) 0.026(2) -0.072(3) -0.042(2) C40 0.089(3) 0.081(2) 0.089(3) -0.001(2) -0.064(2) 0.000(2) C41 0.0526(16) 0.0427(14) 0.0654(17) 0.0052(12) -0.0331(14) -0.0179(12) C42 0.076(2) 0.0470(18) 0.136(4) 0.001(2) -0.036(2) -0.0268(17) _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 C9 1.983(2) . ? Pd1 N2 1.998(2) . ? Pd1 O1 2.0412(17) . ? Pd1 S1 2.4151(7) . ? Pd2 C30 1.976(3) . ? Pd2 N4 1.995(2) . ? Pd2 O3 2.0457(18) . ? Pd2 S2 2.4256(7) . ? O1 C20 1.279(3) . ? O2 C20 1.232(3) . ? O3 C41 1.281(3) . ? O4 C41 1.233(4) . ? S1 C15 1.811(3) . ? S1 C16 1.860(3) . ? S2 C36 1.817(3) . ? S2 C37 1.863(3) . ? N1 C1 1.346(3) . ? N1 C8 1.414(3) . ? N1 H1A 0.8600 . ? N2 C1 1.301(3) . ? N2 C14 1.479(3) . ? N3 C22 1.337(3) . ? N3 C29 1.403(3) . ? N3 H3A 0.8600 . ? N4 C22 1.304(3) . ? N4 C35 1.472(3) . ? C1 C2 1.498(3) . ? C2 C3 1.377(4) . ? C2 C7 1.394(4) . ? C3 C4 1.403(5) . ? C3 H3B 0.9300 . ? C4 C5 1.378(7) . ? C4 H4A 0.9300 . ? C5 C6 1.364(7) . ? C5 H5A 0.9300 . ? C6 C7 1.367(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.392(3) . ? C8 C13 1.393(4) . ? C9 C10 1.400(4) . ? C10 C11 1.375(4) . ? C10 H10A 0.9300 . ? C11 C12 1.375(4) . ? C11 H11A 0.9300 . ? C12 C13 1.377(4) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.514(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C18 1.503(5) . ? C16 C17 1.519(4) . ? C16 C19 1.525(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.509(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.498(3) . ? C23 C28 1.379(4) . ? C23 C24 1.382(4) . ? C24 C25 1.375(5) . ? C24 H24A 0.9300 . ? C25 C26 1.354(6) . ? C25 H25A 0.9300 . ? C26 C27 1.381(7) . ? C26 H26A 0.9300 . ? C27 C28 1.404(5) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C29 C34 1.394(4) . ? C29 C30 1.401(3) . ? C30 C31 1.410(4) . ? C31 C32 1.382(4) . ? C31 H31A 0.9300 . ? C32 C33 1.382(5) . ? C32 H32A 0.9300 . ? C33 C34 1.381(4) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.511(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C40 1.513(5) . ? C37 C39 1.519(5) . ? C37 C38 1.520(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.515(4) . ? C42 H42C 0.9600 . ? C42 H42D 0.9600 . ? C42 H42A 0.9600 . ? 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 C9 Pd1 N2 90.64(9) . . ? C9 Pd1 O1 90.18(9) . . ? N2 Pd1 O1 179.14(8) . . ? C9 Pd1 S1 176.99(7) . . ? N2 Pd1 S1 86.36(6) . . ? O1 Pd1 S1 92.83(6) . . ? C30 Pd2 N4 89.62(10) . . ? C30 Pd2 O3 90.99(9) . . ? N4 Pd2 O3 178.98(9) . . ? C30 Pd2 S2 175.51(8) . . ? N4 Pd2 S2 85.90(7) . . ? O3 Pd2 S2 93.48(6) . . ? C20 O1 Pd1 119.05(17) . . ? C41 O3 Pd2 119.11(17) . . ? C15 S1 C16 105.23(13) . . ? C15 S1 Pd1 95.41(9) . . ? C16 S1 Pd1 110.39(10) . . ? C36 S2 C37 105.17(15) . . ? C36 S2 Pd2 95.38(10) . . ? C37 S2 Pd2 109.62(11) . . ? C1 N1 C8 127.8(2) . . ? C1 N1 H1A 116.1 . . ? C8 N1 H1A 116.1 . . ? C1 N2 C14 120.2(2) . . ? C1 N2 Pd1 126.17(17) . . ? C14 N2 Pd1 113.63(15) . . ? C22 N3 C29 126.9(2) . . ? C22 N3 H3A 116.5 . . ? C29 N3 H3A 116.5 . . ? C22 N4 C35 120.2(2) . . ? C22 N4 Pd2 125.11(18) . . ? C35 N4 Pd2 114.32(17) . . ? N2 C1 N1 122.5(2) . . ? N2 C1 C2 124.2(2) . . ? N1 C1 C2 113.2(2) . . ? C3 C2 C7 120.0(3) . . ? C3 C2 C1 121.4(3) . . ? C7 C2 C1 118.6(3) . . ? C2 C3 C4 119.1(3) . . ? C2 C3 H3B 120.4 . . ? C4 C3 H3B 120.4 . . ? C5 C4 C3 119.7(4) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C6 C5 C4 120.6(3) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C5 C6 C7 120.3(4) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C6 C7 C2 120.2(4) . . ? C6 C7 H7A 119.9 . . ? C2 C7 H7A 119.9 . . ? C9 C8 C13 121.3(2) . . ? C9 C8 N1 122.9(2) . . ? C13 C8 N1 115.8(2) . . ? C8 C9 C10 116.7(2) . . ? C8 C9 Pd1 122.25(18) . . ? C10 C9 Pd1 121.09(19) . . ? C11 C10 C9 122.2(3) . . ? C11 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? C12 C11 C10 119.9(3) . . ? C12 C11 H11A 120.1 . . ? C10 C11 H11A 120.1 . . ? C11 C12 C13 119.8(3) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C12 C13 C8 120.0(3) . . ? C12 C13 H13A 120.0 . . ? C8 C13 H13A 120.0 . . ? N2 C14 C15 111.0(2) . . ? N2 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N2 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 S1 113.33(18) . . ? C14 C15 H15A 108.9 . . ? S1 C15 H15A 108.9 . . ? C14 C15 H15B 108.9 . . ? S1 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C18 C16 C17 111.1(3) . . ? C18 C16 C19 111.8(3) . . ? C17 C16 C19 109.4(3) . . ? C18 C16 S1 112.3(2) . . ? C17 C16 S1 104.5(2) . . ? C19 C16 S1 107.4(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2 C20 O1 125.9(2) . . ? O2 C20 C21 120.5(3) . . ? O1 C20 C21 113.6(3) . . ? 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 . . ? N4 C22 N3 122.9(2) . . ? N4 C22 C23 121.7(2) . . ? N3 C22 C23 115.3(2) . . ? C28 C23 C24 120.1(3) . . ? C28 C23 C22 121.3(3) . . ? C24 C23 C22 118.7(3) . . ? C25 C24 C23 121.1(4) . . ? C25 C24 H24A 119.5 . . ? C23 C24 H24A 119.5 . . ? C26 C25 C24 119.5(4) . . ? C26 C25 H25A 120.2 . . ? C24 C25 H25A 120.2 . . ? C25 C26 C27 120.6(3) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C26 C27 C28 120.4(4) . . ? C26 C27 H27A 119.8 . . ? C28 C27 H27A 119.8 . . ? C23 C28 C27 118.2(4) . . ? C23 C28 H28A 120.9 . . ? C27 C28 H28A 120.9 . . ? C34 C29 C30 120.9(2) . . ? C34 C29 N3 116.2(2) . . ? C30 C29 N3 122.9(2) . . ? C29 C30 C31 116.8(2) . . ? C29 C30 Pd2 121.69(19) . . ? C31 C30 Pd2 121.5(2) . . ? C32 C31 C30 122.0(3) . . ? C32 C31 H31A 119.0 . . ? C30 C31 H31A 119.0 . . ? C31 C32 C33 119.6(3) . . ? C31 C32 H32A 120.2 . . ? C33 C32 H32A 120.2 . . ? C34 C33 C32 120.0(3) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C29 120.3(3) . . ? C33 C34 H34A 119.9 . . ? C29 C34 H34A 119.9 . . ? N4 C35 C36 111.1(2) . . ? N4 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? N4 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 S2 113.0(2) . . ? C35 C36 H36A 109.0 . . ? S2 C36 H36A 109.0 . . ? C35 C36 H36B 109.0 . . ? S2 C36 H36B 109.0 . . ? H36A C36 H36B 107.8 . . ? C40 C37 C39 110.2(3) . . ? C40 C37 C38 110.9(3) . . ? C39 C37 C38 111.7(4) . . ? C40 C37 S2 108.2(2) . . ? C39 C37 S2 103.6(2) . . ? C38 C37 S2 111.9(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O4 C41 O3 126.1(3) . . ? O4 C41 C42 119.8(3) . . ? O3 C41 C42 114.1(3) . . ? C41 C42 H42C 109.5 . . ? C41 C42 H42D 109.5 . . ? H42C C42 H42D 109.5 . . ? C41 C42 H42A 109.5 . . ? H42C C42 H42A 109.5 . . ? H42D C42 H42A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.317 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.093 #==>END data_Compound5a _database_code_depnum_ccdc_archive 'CCDC 829870' #TrackingRef '- BenzamidineCNSPd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H52 N4 O4 Pd2 S2' _chemical_formula_sum 'C42 H52 N4 O4 Pd2 S2' _chemical_formula_weight 953.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c 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 12.7571(10) _cell_length_b 16.4673(13) _cell_length_c 25.1706(19) _cell_angle_alpha 90.00 _cell_angle_beta 98.628(2) _cell_angle_gamma 90.00 _cell_volume 5227.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 14675 _cell_measurement_theta_min 2.281 _cell_measurement_theta_max 25.9845 _exptl_crystal_description parallelplpiped _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.804 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8889 _exptl_absorpt_correction_T_max 0.9312 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 10255 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.01 _reflns_number_total 10255 _reflns_number_gt 8578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0511P)^2^+3.6570P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10255 _refine_ls_number_parameters 493 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1058 _refine_ls_wR_factor_gt 0.1015 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.275662(18) 1.089634(17) -0.277698(10) 0.03555(8) Uani 1 1 d U . . Pd2 Pd 0.205558(18) 0.933863(17) -0.255383(10) 0.03549(8) Uani 1 1 d . . . S1 S 0.21739(7) 1.15298(6) -0.20507(4) 0.0462(2) Uani 1 1 d U . . S2 S 0.33460(8) 0.89732(6) -0.18488(4) 0.0492(2) Uani 1 1 d . . . O1 O 0.42857(19) 1.06767(18) -0.24159(11) 0.0545(7) Uani 1 1 d . . . O2 O 0.5024(3) 1.1660(2) -0.28210(16) 0.0842(10) Uani 1 1 d . . . O3 O 0.09529(19) 0.97116(17) -0.20918(10) 0.0495(6) Uani 1 1 d . . . O4 O -0.0152(3) 0.8683(2) -0.22968(16) 0.0835(10) Uani 1 1 d . . . N1 N 0.1000(2) 0.95985(18) -0.32339(10) 0.0368(6) Uani 1 1 d . . . N2 N 0.1229(2) 1.09822(18) -0.31149(11) 0.0385(6) Uani 1 1 d . . . N3 N 0.3095(2) 1.03108(18) -0.34530(10) 0.0380(6) Uani 1 1 d . . . N4 N 0.3143(2) 0.90739(19) -0.30210(11) 0.0408(6) Uani 1 1 d . . . C1 C 0.0647(2) 1.0361(2) -0.33195(13) 0.0368(7) Uani 1 1 d . . . C2 C -0.0443(3) 1.0511(2) -0.36276(13) 0.0408(8) Uani 1 1 d . . . C3 C -0.0596(3) 1.1018(3) -0.40678(15) 0.0539(9) Uani 1 1 d . . . H3A H -0.0019 1.1285 -0.4174 0.065 Uiso 1 1 calc R . . C4 C -0.1603(4) 1.1134(3) -0.43553(17) 0.0641(12) Uani 1 1 d . . . H4A H -0.1701 1.1474 -0.4654 0.077 Uiso 1 1 calc R . . C5 C -0.2458(3) 1.0740(3) -0.41931(19) 0.0663(13) Uani 1 1 d . . . H5A H -0.3133 1.0813 -0.4384 0.080 Uiso 1 1 calc R . . C6 C -0.2314(3) 1.0244(3) -0.3754(2) 0.0639(12) Uani 1 1 d . . . H6A H -0.2895 0.9989 -0.3644 0.077 Uiso 1 1 calc R . . C7 C -0.1302(3) 1.0117(3) -0.34699(16) 0.0505(9) Uani 1 1 d . . . H7A H -0.1206 0.9769 -0.3176 0.061 Uiso 1 1 calc R . . C8 C 0.0719(3) 0.8935(2) -0.35918(14) 0.0416(8) Uani 1 1 d . . . C9 C 0.0807(3) 0.8153(2) -0.33900(16) 0.0513(9) Uani 1 1 d . . . H9A H 0.0993 0.8076 -0.3022 0.062 Uiso 1 1 calc R . . C10 C 0.0625(4) 0.7480(3) -0.3721(2) 0.0703(12) Uani 1 1 d . . . H10A H 0.0697 0.6961 -0.3574 0.084 Uiso 1 1 calc R . . C11 C 0.0341(4) 0.7575(3) -0.4262(2) 0.0760(14) Uani 1 1 d . . . H11A H 0.0227 0.7124 -0.4486 0.091 Uiso 1 1 calc R . . C12 C 0.0225(3) 0.8345(4) -0.44724(17) 0.0683(13) Uani 1 1 d . . . H12A H 0.0006 0.8409 -0.4839 0.082 Uiso 1 1 calc R . . C13 C 0.0427(3) 0.9033(3) -0.41496(15) 0.0527(9) Uani 1 1 d . . . H13A H 0.0371 0.9549 -0.4301 0.063 Uiso 1 1 calc R . . C14 C 0.0773(3) 1.1769(2) -0.29909(15) 0.0497(9) Uani 1 1 d . . . H14A H 0.0035 1.1800 -0.3154 0.060 Uiso 1 1 calc R . . H14B H 0.1156 1.2210 -0.3130 0.060 Uiso 1 1 calc R . . C15 C 0.0862(3) 1.1834(3) -0.23879(18) 0.0540(10) Uani 1 1 d . . . H15B H 0.071(3) 1.235(3) -0.2308(17) 0.065 Uiso 1 1 d . . . H15A H 0.043(4) 1.148(3) -0.2276(18) 0.065 Uiso 1 1 d . . . C16 C 0.2865(3) 1.2502(3) -0.18532(18) 0.0599(11) Uani 1 1 d . . . C17 C 0.3947(3) 1.2241(3) -0.1558(2) 0.0755(14) Uani 1 1 d . . . H17A H 0.4360 1.2713 -0.1443 0.113 Uiso 1 1 calc R . . H17B H 0.4309 1.1925 -0.1795 0.113 Uiso 1 1 calc R . . H17C H 0.3853 1.1920 -0.1250 0.113 Uiso 1 1 calc R . . C18 C 0.2245(4) 1.2929(4) -0.1463(2) 0.0877(17) Uani 1 1 d . . . H18A H 0.2583 1.3436 -0.1354 0.132 Uiso 1 1 calc R . . H18B H 0.2228 1.2592 -0.1153 0.132 Uiso 1 1 calc R . . H18C H 0.1534 1.3030 -0.1636 0.132 Uiso 1 1 calc R . . C19 C 0.2967(4) 1.3026(3) -0.2341(2) 0.0779(14) Uani 1 1 d . . . H19A H 0.3330 1.3520 -0.2226 0.117 Uiso 1 1 calc R . . H19B H 0.2274 1.3151 -0.2528 0.117 Uiso 1 1 calc R . . H19C H 0.3361 1.2736 -0.2577 0.117 Uiso 1 1 calc R . . C20 C 0.5037(3) 1.1050(3) -0.25559(18) 0.0573(10) Uani 1 1 d . . . C21 C 0.6137(4) 1.0677(5) -0.2336(4) 0.130(3) Uani 1 1 d . . . H21A H 0.6685 1.0994 -0.2458 0.195 Uiso 1 1 calc R . . H21B H 0.6169 1.0130 -0.2465 0.195 Uiso 1 1 calc R . . H21C H 0.6235 1.0676 -0.1951 0.195 Uiso 1 1 calc R . . C22 C 0.3353(2) 0.9525(2) -0.34268(13) 0.0368(7) Uani 1 1 d . . . C23 C 0.3879(3) 0.9142(2) -0.38625(14) 0.0413(8) Uani 1 1 d . . . C24 C 0.4752(3) 0.9507(3) -0.40383(15) 0.0483(9) Uani 1 1 d . . . H24A H 0.5036 0.9982 -0.3877 0.058 Uiso 1 1 calc R . . C25 C 0.5195(3) 0.9159(3) -0.44568(16) 0.0597(11) Uani 1 1 d . . . H25A H 0.5784 0.9398 -0.4570 0.072 Uiso 1 1 calc R . . C26 C 0.4773(3) 0.8468(3) -0.47034(17) 0.0636(12) Uani 1 1 d . . . H26A H 0.5071 0.8242 -0.4985 0.076 Uiso 1 1 calc R . . C27 C 0.3900(3) 0.8102(3) -0.45330(16) 0.0616(11) Uani 1 1 d . . . H27A H 0.3609 0.7635 -0.4703 0.074 Uiso 1 1 calc R . . C28 C 0.3459(3) 0.8434(3) -0.41092(15) 0.0504(9) Uani 1 1 d . . . H28A H 0.2884 0.8183 -0.3991 0.060 Uiso 1 1 calc R . . C29 C 0.2939(3) 1.0772(2) -0.39342(14) 0.0420(8) Uani 1 1 d . . . C30 C 0.3245(3) 1.1583(3) -0.39117(17) 0.0581(10) Uani 1 1 d . . . H30A H 0.3581 1.1802 -0.3590 0.070 Uiso 1 1 calc R . . C31 C 0.3052(4) 1.2066(3) -0.4363(2) 0.0761(14) Uani 1 1 d . . . H31A H 0.3264 1.2606 -0.4341 0.091 Uiso 1 1 calc R . . C32 C 0.2554(4) 1.1766(3) -0.48421(18) 0.0741(14) Uani 1 1 d . . . H32A H 0.2419 1.2101 -0.5142 0.089 Uiso 1 1 calc R . . C33 C 0.2257(4) 1.0966(3) -0.48730(16) 0.0649(12) Uani 1 1 d . . . H33A H 0.1931 1.0756 -0.5199 0.078 Uiso 1 1 calc R . . C34 C 0.2437(3) 1.0464(3) -0.44251(15) 0.0510(9) Uani 1 1 d . . . H34A H 0.2224 0.9924 -0.4452 0.061 Uiso 1 1 calc R . . C35 C 0.3798(3) 0.8372(3) -0.28201(15) 0.0507(9) Uani 1 1 d . . . H35A H 0.4339 0.8276 -0.3046 0.061 Uiso 1 1 calc R . . H35B H 0.3361 0.7889 -0.2825 0.061 Uiso 1 1 calc R . . C36 C 0.4310(3) 0.8558(3) -0.22503(16) 0.0566(10) Uani 1 1 d . . . H36A H 0.4879 0.8946 -0.2258 0.068 Uiso 1 1 calc R . . H36B H 0.4616 0.8065 -0.2082 0.068 Uiso 1 1 calc R . . C37 C 0.2913(3) 0.8077(3) -0.14803(17) 0.0605(11) Uani 1 1 d . . . C38 C 0.2375(4) 0.7439(3) -0.1850(2) 0.0785(14) Uani 1 1 d . . . H38A H 0.2170 0.6994 -0.1641 0.118 Uiso 1 1 calc R . . H38B H 0.2854 0.7248 -0.2082 0.118 Uiso 1 1 calc R . . H38C H 0.1757 0.7666 -0.2062 0.118 Uiso 1 1 calc R . . C39 C 0.3904(4) 0.7731(4) -0.1128(2) 0.0882(17) Uani 1 1 d . . . H39A H 0.3708 0.7269 -0.0933 0.132 Uiso 1 1 calc R . . H39B H 0.4209 0.8139 -0.0880 0.132 Uiso 1 1 calc R . . H39C H 0.4413 0.7569 -0.1353 0.132 Uiso 1 1 calc R . . C40 C 0.2161(5) 0.8434(4) -0.1120(2) 0.099(2) Uani 1 1 d . . . H40A H 0.1902 0.8007 -0.0914 0.149 Uiso 1 1 calc R . . H40B H 0.1574 0.8693 -0.1338 0.149 Uiso 1 1 calc R . . H40C H 0.2535 0.8826 -0.0880 0.149 Uiso 1 1 calc R . . C41 C 0.0090(4) 0.9343(3) -0.20964(17) 0.0600(10) Uani 1 1 d . . . C42 C -0.0727(5) 0.9816(5) -0.1824(3) 0.115(2) Uani 1 1 d . . . H42A H -0.1366 0.9503 -0.1842 0.172 Uiso 1 1 calc R . . H42B H -0.0883 1.0324 -0.2006 0.172 Uiso 1 1 calc R . . H42C H -0.0442 0.9917 -0.1455 0.172 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 0.03154(13) 0.03352(14) 0.04119(14) -0.00383(10) 0.00417(10) -0.00095(10) Pd2 0.03373(13) 0.03535(14) 0.03775(14) 0.00253(10) 0.00650(10) 0.00047(10) S1 0.0448(5) 0.0461(5) 0.0481(5) -0.0083(4) 0.0078(4) -0.0025(4) S2 0.0489(5) 0.0503(6) 0.0465(5) 0.0059(4) 0.0007(4) 0.0031(4) O1 0.0388(13) 0.0593(18) 0.0623(16) -0.0015(14) -0.0022(12) 0.0006(13) O2 0.0594(18) 0.082(3) 0.109(3) 0.021(2) 0.0052(18) -0.0183(18) O3 0.0489(14) 0.0514(16) 0.0506(14) -0.0065(12) 0.0148(11) 0.0004(12) O4 0.075(2) 0.079(3) 0.103(3) -0.015(2) 0.0372(19) -0.0253(19) N1 0.0347(13) 0.0381(15) 0.0370(14) -0.0014(12) 0.0038(11) -0.0031(12) N2 0.0352(13) 0.0365(15) 0.0426(15) -0.0032(12) 0.0020(11) 0.0036(12) N3 0.0399(14) 0.0370(15) 0.0387(14) -0.0011(12) 0.0117(11) 0.0003(12) N4 0.0376(14) 0.0428(16) 0.0440(15) 0.0060(13) 0.0127(12) 0.0121(13) C1 0.0330(15) 0.0403(18) 0.0369(16) -0.0011(14) 0.0043(13) 0.0015(14) C2 0.0356(16) 0.042(2) 0.0437(18) -0.0043(15) 0.0010(14) 0.0042(14) C3 0.054(2) 0.059(3) 0.047(2) 0.0027(18) 0.0007(17) 0.0051(19) C4 0.069(3) 0.065(3) 0.052(2) 0.000(2) -0.014(2) 0.018(2) C5 0.047(2) 0.067(3) 0.075(3) -0.019(2) -0.020(2) 0.012(2) C6 0.0340(18) 0.063(3) 0.091(3) -0.014(3) -0.0021(19) -0.0012(18) C7 0.0410(18) 0.050(2) 0.059(2) -0.0034(18) 0.0010(16) 0.0018(17) C8 0.0327(15) 0.048(2) 0.0454(18) -0.0088(16) 0.0084(14) -0.0017(15) C9 0.058(2) 0.045(2) 0.051(2) -0.0056(17) 0.0106(17) -0.0078(18) C10 0.082(3) 0.049(3) 0.084(3) -0.013(2) 0.027(3) -0.013(2) C11 0.084(3) 0.072(3) 0.075(3) -0.034(3) 0.020(3) -0.016(3) C12 0.062(3) 0.094(4) 0.048(2) -0.022(2) 0.0050(19) -0.001(3) C13 0.050(2) 0.063(3) 0.045(2) -0.0072(18) 0.0059(16) 0.0030(19) C14 0.0436(19) 0.041(2) 0.062(2) -0.0053(18) -0.0021(16) 0.0046(16) C15 0.041(2) 0.051(2) 0.070(3) -0.014(2) 0.0070(18) 0.0061(18) C16 0.046(2) 0.058(3) 0.075(3) -0.029(2) 0.0073(19) -0.0068(19) C17 0.057(2) 0.081(4) 0.083(3) -0.026(3) -0.007(2) -0.011(2) C18 0.076(3) 0.082(4) 0.107(4) -0.057(3) 0.020(3) -0.011(3) C19 0.079(3) 0.055(3) 0.099(4) 0.003(3) 0.012(3) -0.012(2) C20 0.060(2) 0.046(2) 0.065(2) -0.002(2) 0.006(2) -0.005(2) C21 0.045(3) 0.129(6) 0.210(8) 0.050(6) 0.001(4) 0.007(3) C22 0.0294(14) 0.0405(19) 0.0407(17) -0.0022(14) 0.0057(13) -0.0009(13) C23 0.0357(16) 0.046(2) 0.0421(18) 0.0007(15) 0.0050(14) 0.0071(15) C24 0.0385(17) 0.055(2) 0.052(2) -0.0033(17) 0.0094(15) 0.0013(16) C25 0.043(2) 0.085(3) 0.054(2) 0.006(2) 0.0188(18) 0.008(2) C26 0.060(2) 0.084(3) 0.048(2) -0.009(2) 0.0115(18) 0.019(2) C27 0.059(2) 0.066(3) 0.056(2) -0.020(2) -0.0015(19) 0.009(2) C28 0.0452(19) 0.051(2) 0.056(2) -0.0059(18) 0.0100(16) 0.0014(17) C29 0.0368(16) 0.045(2) 0.0450(18) 0.0033(15) 0.0094(14) 0.0043(15) C30 0.067(3) 0.047(2) 0.058(2) 0.0052(19) 0.0003(19) -0.010(2) C31 0.096(4) 0.056(3) 0.076(3) 0.022(2) 0.011(3) -0.011(3) C32 0.091(3) 0.077(4) 0.054(3) 0.023(2) 0.012(2) 0.015(3) C33 0.068(3) 0.081(3) 0.043(2) 0.000(2) 0.0026(19) 0.023(2) C34 0.051(2) 0.052(2) 0.049(2) -0.0020(17) 0.0055(16) 0.0092(18) C35 0.051(2) 0.047(2) 0.057(2) 0.0062(18) 0.0197(17) 0.0135(17) C36 0.0429(19) 0.061(3) 0.066(2) 0.018(2) 0.0062(17) 0.0111(18) C37 0.059(2) 0.066(3) 0.056(2) 0.022(2) 0.0104(19) 0.009(2) C38 0.085(3) 0.073(3) 0.076(3) 0.031(3) 0.006(3) -0.011(3) C39 0.091(4) 0.096(4) 0.072(3) 0.040(3) -0.006(3) 0.012(3) C40 0.120(5) 0.110(5) 0.078(3) 0.032(3) 0.048(3) 0.035(4) C41 0.063(3) 0.064(3) 0.055(2) -0.003(2) 0.0161(19) -0.004(2) C42 0.084(4) 0.123(6) 0.152(6) -0.036(5) 0.066(4) -0.005(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 N2 2.011(3) . ? Pd1 O1 2.057(2) . ? Pd1 N3 2.057(3) . ? Pd1 S1 2.3217(9) . ? Pd1 Pd2 2.8011(4) . ? Pd2 N4 1.997(3) . ? Pd2 O3 2.049(2) . ? Pd2 N1 2.058(3) . ? Pd2 S2 2.3119(9) . ? S1 C15 1.829(4) . ? S1 C16 1.858(4) . ? S2 C36 1.837(4) . ? S2 C37 1.870(4) . ? O1 C20 1.234(5) . ? O2 C20 1.205(5) . ? O3 C41 1.255(5) . ? O4 C41 1.219(6) . ? N1 C1 1.339(4) . ? N1 C8 1.427(4) . ? N2 C1 1.323(4) . ? N2 C14 1.473(5) . ? N3 C22 1.334(4) . ? N3 C29 1.418(4) . ? N4 C22 1.322(4) . ? N4 C35 1.471(5) . ? C1 C2 1.508(4) . ? C2 C3 1.378(5) . ? C2 C7 1.381(5) . ? C3 C4 1.390(6) . ? C3 H3A 0.9300 . ? C4 C5 1.382(7) . ? C4 H4A 0.9300 . ? C5 C6 1.364(7) . ? C5 H5A 0.9300 . ? C6 C7 1.395(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.384(6) . ? C8 C13 1.407(5) . ? C9 C10 1.384(6) . ? C9 H9A 0.9300 . ? C10 C11 1.365(7) . ? C10 H10A 0.9300 . ? C11 C12 1.373(8) . ? C11 H11A 0.9300 . ? C12 C13 1.395(6) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.509(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15B 0.89(5) . ? C15 H15A 0.88(5) . ? C16 C19 1.522(7) . ? C16 C18 1.523(6) . ? C16 C17 1.529(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.555(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.507(5) . ? C23 C28 1.390(5) . ? C23 C24 1.394(5) . ? C24 C25 1.392(5) . ? C24 H24A 0.9300 . ? C25 C26 1.367(7) . ? C25 H25A 0.9300 . ? C26 C27 1.390(6) . ? C26 H26A 0.9300 . ? C27 C28 1.390(5) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C29 C30 1.390(6) . ? C29 C34 1.399(5) . ? C30 C31 1.377(6) . ? C30 H30A 0.9300 . ? C31 C32 1.369(7) . ? C31 H31A 0.9300 . ? C32 C33 1.370(7) . ? C32 H32A 0.9300 . ? C33 C34 1.389(6) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.515(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.499(7) . ? C37 C40 1.534(7) . ? C37 C39 1.540(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.542(7) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 O1 173.71(12) . . ? N2 Pd1 N3 89.62(11) . . ? O1 Pd1 N3 88.87(11) . . ? N2 Pd1 S1 84.09(8) . . ? O1 Pd1 S1 97.21(8) . . ? N3 Pd1 S1 173.51(8) . . ? N2 Pd1 Pd2 80.27(8) . . ? O1 Pd1 Pd2 93.47(8) . . ? N3 Pd1 Pd2 81.35(8) . . ? S1 Pd1 Pd2 95.97(3) . . ? N4 Pd2 O3 175.13(12) . . ? N4 Pd2 N1 88.95(11) . . ? O3 Pd2 N1 89.44(10) . . ? N4 Pd2 S2 85.27(9) . . ? O3 Pd2 S2 96.47(8) . . ? N1 Pd2 S2 173.92(8) . . ? N4 Pd2 Pd1 79.10(9) . . ? O3 Pd2 Pd1 96.10(8) . . ? N1 Pd2 Pd1 80.31(8) . . ? S2 Pd2 Pd1 100.39(3) . . ? C15 S1 C16 104.6(2) . . ? C15 S1 Pd1 97.84(14) . . ? C16 S1 Pd1 113.73(14) . . ? C36 S2 C37 104.5(2) . . ? C36 S2 Pd2 97.64(13) . . ? C37 S2 Pd2 110.90(14) . . ? C20 O1 Pd1 120.8(3) . . ? C41 O3 Pd2 121.7(3) . . ? C1 N1 C8 124.7(3) . . ? C1 N1 Pd2 119.4(2) . . ? C8 N1 Pd2 115.9(2) . . ? C1 N2 C14 123.2(3) . . ? C1 N2 Pd1 124.2(2) . . ? C14 N2 Pd1 111.2(2) . . ? C22 N3 C29 124.3(3) . . ? C22 N3 Pd1 119.6(2) . . ? C29 N3 Pd1 115.8(2) . . ? C22 N4 C35 122.5(3) . . ? C22 N4 Pd2 124.8(2) . . ? C35 N4 Pd2 112.2(2) . . ? N2 C1 N1 120.5(3) . . ? N2 C1 C2 119.6(3) . . ? N1 C1 C2 119.8(3) . . ? C3 C2 C7 119.6(3) . . ? C3 C2 C1 121.4(3) . . ? C7 C2 C1 119.0(3) . . ? C2 C3 C4 120.7(4) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C6 C5 C4 120.3(4) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C5 C6 C7 120.5(4) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C2 C7 C6 119.7(4) . . ? C2 C7 H7A 120.2 . . ? C6 C7 H7A 120.2 . . ? C9 C8 C13 117.9(4) . . ? C9 C8 N1 118.8(3) . . ? C13 C8 N1 123.1(4) . . ? C8 C9 C10 121.8(4) . . ? C8 C9 H9A 119.1 . . ? C10 C9 H9A 119.1 . . ? C11 C10 C9 120.3(5) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 119.1(4) . . ? C10 C11 H11A 120.4 . . ? C12 C11 H11A 120.4 . . ? C11 C12 C13 121.7(4) . . ? C11 C12 H12A 119.1 . . ? C13 C12 H12A 119.1 . . ? C12 C13 C8 119.1(4) . . ? C12 C13 H13A 120.4 . . ? C8 C13 H13A 120.4 . . ? N2 C14 C15 107.6(3) . . ? N2 C14 H14A 110.2 . . ? C15 C14 H14A 110.2 . . ? N2 C14 H14B 110.2 . . ? C15 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? C14 C15 S1 111.9(3) . . ? C14 C15 H15B 108(3) . . ? S1 C15 H15B 112(3) . . ? C14 C15 H15A 109(3) . . ? S1 C15 H15A 104(3) . . ? H15B C15 H15A 113(4) . . ? C19 C16 C18 111.9(5) . . ? C19 C16 C17 111.8(4) . . ? C18 C16 C17 109.6(4) . . ? C19 C16 S1 111.5(3) . . ? C18 C16 S1 107.4(3) . . ? C17 C16 S1 104.2(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O2 C20 O1 128.9(4) . . ? O2 C20 C21 117.6(5) . . ? O1 C20 C21 113.5(4) . . ? 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 . . ? N4 C22 N3 120.4(3) . . ? N4 C22 C23 119.4(3) . . ? N3 C22 C23 120.2(3) . . ? C28 C23 C24 119.5(3) . . ? C28 C23 C22 119.5(3) . . ? C24 C23 C22 121.0(3) . . ? C25 C24 C23 119.8(4) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C26 C25 C24 120.7(4) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 119.9(4) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C28 C27 C26 120.1(4) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C23 120.0(4) . . ? C27 C28 H28A 120.0 . . ? C23 C28 H28A 120.0 . . ? C30 C29 C34 118.2(4) . . ? C30 C29 N3 118.5(3) . . ? C34 C29 N3 123.2(3) . . ? C31 C30 C29 120.4(4) . . ? C31 C30 H30A 119.8 . . ? C29 C30 H30A 119.8 . . ? C32 C31 C30 121.4(5) . . ? C32 C31 H31A 119.3 . . ? C30 C31 H31A 119.3 . . ? C31 C32 C33 118.9(4) . . ? C31 C32 H32A 120.5 . . ? C33 C32 H32A 120.5 . . ? C32 C33 C34 121.1(4) . . ? C32 C33 H33A 119.5 . . ? C34 C33 H33A 119.5 . . ? C33 C34 C29 119.9(4) . . ? C33 C34 H34A 120.0 . . ? C29 C34 H34A 120.0 . . ? N4 C35 C36 108.0(3) . . ? N4 C35 H35A 110.1 . . ? C36 C35 H35A 110.1 . . ? N4 C35 H35B 110.1 . . ? C36 C35 H35B 110.1 . . ? H35A C35 H35B 108.4 . . ? C35 C36 S2 111.5(3) . . ? C35 C36 H36A 109.3 . . ? S2 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? S2 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C38 C37 C40 111.6(4) . . ? C38 C37 C39 110.9(4) . . ? C40 C37 C39 109.5(4) . . ? C38 C37 S2 112.8(3) . . ? C40 C37 S2 104.4(4) . . ? C39 C37 S2 107.4(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O4 C41 O3 127.1(4) . . ? O4 C41 C42 119.2(4) . . ? O3 C41 C42 113.7(4) . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.171 _refine_diff_density_min -0.976 _refine_diff_density_rms 0.076 # 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 -0.009 0.000 0.000 658 53 ' ' 2 -0.005 0.500 0.500 658 53 ' ' _platon_squeeze_details ; ; #==>END data_Compound6 _database_code_depnum_ccdc_archive 'CCDC 829871' #TrackingRef '- BenzamidineCNSPd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H20 N2 O2 Pd S' _chemical_formula_sum 'C22 H20 N2 O2 Pd S' _chemical_formula_weight 482.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.165(5) _cell_length_b 20.675(4) _cell_length_c 11.302(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.472(4) _cell_angle_gamma 90.00 _cell_volume 4388.0(16) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6838 _cell_measurement_theta_min 2.183 _cell_measurement_theta_max 26.005 _exptl_crystal_description parallelplpiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7626 _exptl_absorpt_correction_T_max 0.9105 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12136 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 26.20 _reflns_number_total 4315 _reflns_number_gt 3456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1100P)^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 4315 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1326 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.004 _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 Pd Pd 0.738432(13) 1.139336(15) 2.11122(2) 0.04882(15) Uani 1 1 d . . . S S 0.78907(6) 1.04947(6) 2.04803(11) 0.0675(3) Uani 1 1 d . . . O1 O 0.80956(17) 1.13724(15) 2.3107(3) 0.0643(8) Uani 1 1 d . . . O2 O 0.90372(17) 1.14718(17) 2.2763(4) 0.0765(10) Uani 1 1 d . . . N1 N 0.63556(15) 1.24452(16) 1.8977(3) 0.0517(7) Uani 1 1 d . . . H1A H 0.6240 1.2773 1.8450 0.062 Uiso 1 1 calc R . . N2 N 0.66444(17) 1.13543(14) 1.9187(3) 0.0460(7) Uani 1 1 d . . . C1 C 0.63879(17) 1.18743(19) 1.8447(3) 0.0459(7) Uani 1 1 d . . . C2 C 0.61442(18) 1.1863(2) 1.6977(3) 0.0527(8) Uani 1 1 d . . . C3 C 0.6610(2) 1.1648(2) 1.6529(4) 0.0580(9) Uani 1 1 d . . . H3A H 0.7069 1.1527 1.7139 0.070 Uiso 1 1 calc R . . C4 C 0.6401(3) 1.1609(3) 1.5176(5) 0.0770(13) Uani 1 1 d . . . H4A H 0.6717 1.1460 1.4875 0.092 Uiso 1 1 calc R . . C5 C 0.5724(3) 1.1791(4) 1.4284(4) 0.0939(18) Uani 1 1 d . . . H5A H 0.5580 1.1761 1.3375 0.113 Uiso 1 1 calc R . . C6 C 0.5251(2) 1.2020(3) 1.4717(4) 0.0868(16) Uani 1 1 d . . . H6A H 0.4794 1.2144 1.4103 0.104 Uiso 1 1 calc R . . C7 C 0.5466(2) 1.2061(2) 1.6075(4) 0.0665(11) Uani 1 1 d . . . H7A H 0.5156 1.2220 1.6378 0.080 Uiso 1 1 calc R . . C8 C 0.64902(17) 1.25738(18) 2.0314(3) 0.0483(8) Uani 1 1 d . . . C9 C 0.68991(16) 1.21615(19) 2.1366(3) 0.0482(8) Uani 1 1 d . . . C10 C 0.69481(19) 1.2319(2) 2.2620(4) 0.0575(9) Uani 1 1 d . . . H10A H 0.7196 1.2043 2.3337 0.069 Uiso 1 1 calc R . . C11 C 0.6638(2) 1.2874(2) 2.2817(4) 0.0653(11) Uani 1 1 d . . . H11A H 0.6687 1.2968 2.3660 0.078 Uiso 1 1 calc R . . C12 C 0.6257(2) 1.3284(3) 2.1766(4) 0.0690(11) Uani 1 1 d . . . H12A H 0.6052 1.3657 2.1898 0.083 Uiso 1 1 calc R . . C13 C 0.6179(2) 1.3135(2) 2.0497(4) 0.0595(9) Uani 1 1 d . . . H13A H 0.5922 1.3409 1.9780 0.071 Uiso 1 1 calc R . . C14 C 0.65236(19) 1.0722(2) 1.8590(4) 0.0527(8) Uani 1 1 d . . . C15 C 0.5867(2) 1.0534(2) 1.7563(4) 0.0610(9) Uani 1 1 d . . . H15A H 0.5485 1.0820 1.7252 0.073 Uiso 1 1 calc R . . C16 C 0.5779(3) 0.9926(2) 1.7001(5) 0.0736(12) Uani 1 1 d . . . H16A H 0.5337 0.9808 1.6316 0.088 Uiso 1 1 calc R . . C17 C 0.6331(3) 0.9491(2) 1.7435(5) 0.0787(13) Uani 1 1 d . . . H17A H 0.6268 0.9086 1.7038 0.094 Uiso 1 1 calc R . . C18 C 0.6983(3) 0.9665(2) 1.8472(4) 0.0722(12) Uani 1 1 d . . . H18A H 0.7363 0.9376 1.8770 0.087 Uiso 1 1 calc R . . C19 C 0.7075(2) 1.0272(2) 1.9077(4) 0.0567(9) Uani 1 1 d . . . C20 C 0.7991(4) 0.9837(3) 2.1623(5) 0.108(2) Uani 1 1 d . . . H20A H 0.8192 0.9467 2.1404 0.162 Uiso 1 1 calc R . . H20B H 0.7534 0.9725 2.1547 0.162 Uiso 1 1 calc R . . H20C H 0.8301 0.9971 2.2520 0.162 Uiso 1 1 calc R . . C21 C 0.8757(2) 1.1379(2) 2.3499(4) 0.0651(12) Uani 1 1 d . . . C22 C 0.9209(3) 1.1249(5) 2.4990(5) 0.125(3) Uani 1 1 d . . . H22A H 0.9704 1.1257 2.5207 0.187 Uiso 1 1 calc R . . H22B H 0.9091 1.0832 2.5205 0.187 Uiso 1 1 calc R . . H22C H 0.9117 1.1576 2.5493 0.187 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 Pd 0.0362(2) 0.0695(2) 0.0387(2) 0.00607(10) 0.01558(15) 0.00267(10) S 0.0492(5) 0.0858(8) 0.0671(6) 0.0084(5) 0.0266(5) 0.0164(5) O1 0.0483(16) 0.097(2) 0.0418(15) 0.0060(12) 0.0162(13) -0.0013(13) O2 0.0482(17) 0.112(3) 0.067(2) 0.0190(16) 0.0248(16) 0.0001(15) N1 0.0451(15) 0.071(2) 0.0372(14) 0.0093(13) 0.0174(13) 0.0053(14) N2 0.0348(15) 0.0639(19) 0.0381(15) 0.0012(12) 0.0158(13) -0.0003(12) C1 0.0310(15) 0.066(2) 0.0386(16) 0.0014(15) 0.0145(13) 0.0038(14) C2 0.0414(18) 0.072(2) 0.0390(17) -0.0023(16) 0.0139(15) 0.0009(16) C3 0.0418(19) 0.090(3) 0.0410(18) 0.0054(18) 0.0184(16) 0.0026(18) C4 0.072(3) 0.113(4) 0.056(2) -0.001(2) 0.038(2) 0.017(3) C5 0.082(3) 0.152(5) 0.035(2) -0.004(3) 0.017(2) 0.018(3) C6 0.054(2) 0.138(5) 0.044(2) -0.001(2) 0.0027(19) 0.027(3) C7 0.0438(19) 0.101(3) 0.0449(18) -0.004(2) 0.0119(16) 0.015(2) C8 0.0384(17) 0.063(2) 0.0454(17) -0.0063(15) 0.0207(15) -0.0100(15) C9 0.0327(16) 0.069(2) 0.0429(17) -0.0007(15) 0.0173(14) -0.0073(14) C10 0.0457(19) 0.083(3) 0.0424(18) 0.0001(17) 0.0194(16) -0.0058(18) C11 0.052(2) 0.097(3) 0.0469(19) -0.012(2) 0.0233(18) -0.005(2) C12 0.053(2) 0.084(3) 0.069(3) -0.021(2) 0.027(2) -0.008(2) C13 0.050(2) 0.072(2) 0.054(2) -0.0041(18) 0.0211(18) -0.0029(18) C14 0.0490(19) 0.067(2) 0.0498(18) 0.0016(16) 0.0292(17) -0.0012(16) C15 0.050(2) 0.076(3) 0.059(2) -0.0014(19) 0.0270(18) -0.0051(18) C16 0.076(3) 0.081(3) 0.066(3) -0.011(2) 0.034(2) -0.013(2) C17 0.096(4) 0.074(3) 0.078(3) -0.016(2) 0.050(3) -0.009(3) C18 0.091(3) 0.070(3) 0.070(3) 0.003(2) 0.050(3) 0.009(2) C19 0.058(2) 0.065(2) 0.059(2) 0.0090(17) 0.0374(19) 0.0088(18) C20 0.124(5) 0.097(4) 0.074(3) 0.031(3) 0.021(3) 0.034(4) C21 0.039(2) 0.098(3) 0.046(2) 0.0208(19) 0.0102(18) 0.0015(18) C22 0.064(3) 0.228(8) 0.055(3) 0.033(4) 0.004(3) -0.016(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 Pd C9 1.983(4) . ? Pd N2 2.013(3) . ? Pd O1 2.054(3) . ? Pd S 2.4119(12) . ? S C19 1.784(4) . ? S C20 1.819(6) . ? O1 C21 1.258(5) . ? O2 C21 1.240(6) . ? N1 C1 1.340(5) . ? N1 C8 1.427(4) . ? N1 H1A 0.8600 . ? N2 C1 1.316(5) . ? N2 C14 1.439(5) . ? C1 C2 1.496(4) . ? C2 C3 1.373(5) . ? C2 C7 1.385(5) . ? C3 C4 1.385(6) . ? C3 H3A 0.9300 . ? C4 C5 1.371(7) . ? C4 H4A 0.9300 . ? C5 C6 1.383(7) . ? C5 H5A 0.9300 . ? C6 C7 1.388(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.393(5) . ? C8 C13 1.396(6) . ? C9 C10 1.411(5) . ? C10 C11 1.390(6) . ? C10 H10A 0.9300 . ? C11 C12 1.377(7) . ? C11 H11A 0.9300 . ? C12 C13 1.401(6) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C19 1.393(5) . ? C14 C15 1.394(5) . ? C15 C16 1.381(6) . ? C15 H15A 0.9300 . ? C16 C17 1.374(7) . ? C16 H16A 0.9300 . ? C17 C18 1.384(7) . ? C17 H17A 0.9300 . ? C18 C19 1.399(6) . ? C18 H18A 0.9300 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.529(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 C9 Pd N2 89.55(13) . . ? C9 Pd O1 91.39(13) . . ? N2 Pd O1 175.30(12) . . ? C9 Pd S 172.10(10) . . ? N2 Pd S 83.07(9) . . ? O1 Pd S 96.20(10) . . ? C19 S C20 100.7(3) . . ? C19 S Pd 94.74(13) . . ? C20 S Pd 106.8(2) . . ? C21 O1 Pd 121.3(3) . . ? C1 N1 C8 127.7(3) . . ? C1 N1 H1A 116.2 . . ? C8 N1 H1A 116.2 . . ? C1 N2 C14 120.8(3) . . ? C1 N2 Pd 122.8(2) . . ? C14 N2 Pd 115.1(2) . . ? N2 C1 N1 121.8(3) . . ? N2 C1 C2 121.5(3) . . ? N1 C1 C2 116.6(3) . . ? C3 C2 C7 120.1(3) . . ? C3 C2 C1 118.4(3) . . ? C7 C2 C1 121.5(3) . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5A 119.5 . . ? C6 C5 H5A 119.5 . . ? C7 C6 C5 119.3(4) . . ? C7 C6 H6A 120.3 . . ? C5 C6 H6A 120.3 . . ? C2 C7 C6 119.7(4) . . ? C2 C7 H7A 120.1 . . ? C6 C7 H7A 120.1 . . ? C9 C8 C13 122.2(3) . . ? C9 C8 N1 122.1(3) . . ? C13 C8 N1 115.7(3) . . ? C8 C9 C10 116.4(3) . . ? C8 C9 Pd 121.7(2) . . ? C10 C9 Pd 121.8(3) . . ? C11 C10 C9 122.0(4) . . ? C11 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? C12 C11 C10 120.1(4) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12A 120.2 . . ? C13 C12 H12A 120.2 . . ? C8 C13 C12 119.6(4) . . ? C8 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C19 C14 C15 118.3(4) . . ? C19 C14 N2 119.1(3) . . ? C15 C14 N2 122.5(4) . . ? C16 C15 C14 120.6(4) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C17 C16 C15 121.2(5) . . ? C17 C16 H16A 119.4 . . ? C15 C16 H16A 119.4 . . ? C16 C17 C18 119.0(5) . . ? C16 C17 H17A 120.5 . . ? C18 C17 H17A 120.5 . . ? C19 C18 C17 120.4(4) . . ? C19 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C14 C19 C18 120.3(4) . . ? C14 C19 S 118.0(3) . . ? C18 C19 S 121.7(3) . . ? S C20 H20A 109.5 . . ? S C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? S C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O2 C21 O1 124.3(4) . . ? O2 C21 C22 121.1(4) . . ? O1 C21 C22 114.6(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 26.20 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.046 _refine_diff_density_min -0.900 _refine_diff_density_rms 0.090 # 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 0.000 0.000 -0.009 169 31 ' ' 2 0.500 0.500 -0.058 169 31 ' ' 3 0.500 0.292 0.250 8 0 ' ' 4 0.000 0.792 0.250 8 0 ' ' 5 0.000 0.208 0.750 8 0 ' ' 6 0.500 0.708 0.750 8 0 ' ' _platon_squeeze_details ; ; #==>END data_Compound7 _database_code_depnum_ccdc_archive 'CCDC 829872' #TrackingRef '- BenzamidineCNSPd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H17 Cl N2 Pd S' _chemical_formula_sum 'C16 H17 Cl N2 Pd S' _chemical_formula_weight 411.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.6575(6) _cell_length_b 13.7665(12) _cell_length_c 15.5516(13) _cell_angle_alpha 90.00 _cell_angle_beta 103.395(2) _cell_angle_gamma 90.00 _cell_volume 1594.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 7113 _cell_measurement_theta_min 2.6925 _cell_measurement_theta_max 25.9875 _exptl_crystal_description parallelplpiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.713 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.456 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6692 _exptl_absorpt_correction_T_max 0.8681 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8708 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3134 _reflns_number_gt 2945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0496P)^2^+0.7892P] 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 3134 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0819 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 Pd Pd 0.06722(2) 0.668244(14) 0.085055(11) 0.04021(10) Uani 1 1 d . . . Cl Cl 0.34778(10) 0.64507(7) 0.18268(5) 0.0605(2) Uani 1 1 d . . . S S -0.02474(11) 0.51542(6) 0.13391(6) 0.0625(2) Uani 1 1 d . . . N1 N -0.1203(3) 0.78300(17) -0.09561(13) 0.0422(5) Uani 1 1 d . . . H1A H -0.1474 0.7967 -0.1511 0.051 Uiso 1 1 calc R . . N2 N -0.1836(3) 0.67645(17) 0.00794(15) 0.0437(5) Uani 1 1 d . . . C1 C -0.2300(3) 0.71947(18) -0.06812(15) 0.0379(5) Uani 1 1 d . . . C2 C -0.4029(3) 0.70329(18) -0.13468(16) 0.0376(5) Uani 1 1 d . . . C3 C -0.5655(4) 0.7374(3) -0.1227(2) 0.0570(7) Uani 1 1 d . . . H3A H -0.5715 0.7683 -0.0703 0.068 Uiso 1 1 calc R . . C4 C -0.7194(4) 0.7253(3) -0.1891(2) 0.0636(8) Uani 1 1 d . . . H4A H -0.8289 0.7477 -0.1808 0.076 Uiso 1 1 calc R . . C5 C -0.7124(4) 0.6806(2) -0.2669(2) 0.0538(7) Uani 1 1 d . . . H5A H -0.8163 0.6735 -0.3113 0.065 Uiso 1 1 calc R . . C6 C -0.5515(4) 0.6462(2) -0.2792(2) 0.0554(7) Uani 1 1 d . . . H6A H -0.5461 0.6158 -0.3320 0.066 Uiso 1 1 calc R . . C7 C -0.3967(4) 0.6571(2) -0.21256(19) 0.0480(6) Uani 1 1 d . . . H7A H -0.2881 0.6330 -0.2206 0.058 Uiso 1 1 calc R . . C8 C 0.0342(3) 0.82998(18) -0.04452(17) 0.0396(5) Uani 1 1 d . . . C9 C 0.1309(3) 0.7940(2) 0.03658(16) 0.0405(5) Uani 1 1 d . . . C10 C 0.2747(4) 0.8519(2) 0.08092(18) 0.0504(6) Uani 1 1 d . . . H10A H 0.3405 0.8318 0.1360 0.061 Uiso 1 1 calc R . . C11 C 0.3221(4) 0.9369(2) 0.04648(19) 0.0558(7) Uani 1 1 d . . . H11A H 0.4188 0.9728 0.0781 0.067 Uiso 1 1 calc R . . C12 C 0.2266(4) 0.9696(2) -0.0353(2) 0.0539(7) Uani 1 1 d . . . H12A H 0.2593 1.0268 -0.0592 0.065 Uiso 1 1 calc R . . C13 C 0.0820(3) 0.9156(2) -0.08080(18) 0.0476(6) Uani 1 1 d . . . H13A H 0.0166 0.9366 -0.1357 0.057 Uiso 1 1 calc R . . C14 C -0.3155(4) 0.6177(3) 0.0408(2) 0.0587(8) Uani 1 1 d . . . H14A H -0.4270 0.6150 -0.0040 0.070 Uiso 1 1 calc R . . H14B H -0.3400 0.6484 0.0929 0.070 Uiso 1 1 calc R . . C15 C -0.2475(5) 0.5163(3) 0.0635(2) 0.0632(8) Uani 1 1 d . . . H15A H -0.2466 0.4813 0.0094 0.076 Uiso 1 1 calc R . . H15B H -0.3285 0.4827 0.0930 0.076 Uiso 1 1 calc R . . C16 C -0.0675(7) 0.5481(4) 0.2386(2) 0.0961(15) Uani 1 1 d . . . H16A H -0.1063 0.4918 0.2655 0.144 Uiso 1 1 calc R . . H16B H -0.1596 0.5968 0.2301 0.144 Uiso 1 1 calc R . . H16C H 0.0404 0.5732 0.2764 0.144 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 Pd 0.02846(13) 0.05616(15) 0.03124(13) 0.00088(7) -0.00284(9) -0.00341(7) Cl 0.0358(3) 0.0850(5) 0.0504(4) 0.0080(4) -0.0112(3) 0.0017(3) S 0.0551(4) 0.0539(4) 0.0691(5) 0.0077(3) -0.0047(4) -0.0048(3) N1 0.0304(10) 0.0591(13) 0.0307(10) 0.0038(9) -0.0056(8) -0.0079(9) N2 0.0305(11) 0.0641(14) 0.0339(11) 0.0032(9) 0.0020(9) -0.0079(9) C1 0.0244(10) 0.0522(13) 0.0339(12) -0.0035(10) 0.0000(9) -0.0015(9) C2 0.0263(11) 0.0465(12) 0.0354(12) -0.0003(10) -0.0019(9) -0.0022(9) C3 0.0354(13) 0.0781(19) 0.0537(17) -0.0171(15) 0.0027(11) 0.0064(13) C4 0.0275(12) 0.083(2) 0.074(2) -0.0132(17) -0.0026(13) 0.0090(13) C5 0.0324(14) 0.0623(16) 0.0547(17) 0.0007(13) -0.0147(12) -0.0067(11) C6 0.0468(16) 0.0678(17) 0.0441(15) -0.0124(13) -0.0048(12) -0.0070(13) C7 0.0313(13) 0.0639(16) 0.0449(15) -0.0112(12) 0.0011(11) 0.0009(11) C8 0.0263(12) 0.0548(15) 0.0352(13) -0.0052(9) 0.0020(10) -0.0043(9) C9 0.0270(11) 0.0603(14) 0.0322(11) -0.0024(10) 0.0030(9) -0.0063(10) C10 0.0333(13) 0.0781(18) 0.0346(13) -0.0008(12) -0.0029(10) -0.0127(12) C11 0.0381(14) 0.0750(19) 0.0496(16) -0.0068(14) 0.0003(12) -0.0210(13) C12 0.0432(14) 0.0621(16) 0.0534(16) 0.0018(13) 0.0048(12) -0.0154(13) C13 0.0382(13) 0.0588(15) 0.0412(13) 0.0029(11) -0.0002(11) -0.0050(11) C14 0.0360(13) 0.086(2) 0.0495(16) 0.0140(15) 0.0012(12) -0.0142(14) C15 0.0596(19) 0.073(2) 0.0499(17) -0.0007(14) -0.0013(14) -0.0261(15) C16 0.126(4) 0.105(3) 0.0479(19) 0.014(2) 0.002(2) -0.047(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C9 1.993(3) . ? Pd N2 2.018(2) . ? Pd Cl 2.3476(7) . ? Pd S 2.3974(8) . ? S C16 1.792(4) . ? S C15 1.801(3) . ? N1 C1 1.349(3) . ? N1 C8 1.419(3) . ? N1 H1A 0.8600 . ? N2 C1 1.297(3) . ? N2 C14 1.474(3) . ? C1 C2 1.497(3) . ? C2 C7 1.378(4) . ? C2 C3 1.383(4) . ? C3 C4 1.386(4) . ? C3 H3A 0.9300 . ? C4 C5 1.369(5) . ? C4 H4A 0.9300 . ? C5 C6 1.374(5) . ? C5 H5A 0.9300 . ? C6 C7 1.390(4) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.392(4) . ? C8 C9 1.397(4) . ? C9 C10 1.404(4) . ? C10 C11 1.370(4) . ? C10 H10A 0.9300 . ? C11 C12 1.388(4) . ? C11 H11A 0.9300 . ? C12 C13 1.384(4) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.504(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 C9 Pd N2 90.53(9) . . ? C9 Pd Cl 95.46(7) . . ? N2 Pd Cl 173.88(7) . . ? C9 Pd S 176.01(7) . . ? N2 Pd S 85.89(7) . . ? Cl Pd S 88.15(3) . . ? C16 S C15 101.8(2) . . ? C16 S Pd 101.34(14) . . ? C15 S Pd 96.20(11) . . ? C1 N1 C8 128.1(2) . . ? C1 N1 H1A 115.9 . . ? C8 N1 H1A 115.9 . . ? C1 N2 C14 120.1(2) . . ? C1 N2 Pd 126.11(17) . . ? C14 N2 Pd 113.41(17) . . ? N2 C1 N1 121.8(2) . . ? N2 C1 C2 125.1(2) . . ? N1 C1 C2 113.2(2) . . ? C7 C2 C3 119.4(2) . . ? C7 C2 C1 118.1(2) . . ? C3 C2 C1 122.4(2) . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 120.8(3) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 119.9(3) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C5 C6 C7 119.7(3) . . ? C5 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C2 C7 C6 120.6(3) . . ? C2 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C13 C8 C9 122.2(2) . . ? C13 C8 N1 115.0(2) . . ? C9 C8 N1 122.9(2) . . ? C8 C9 C10 115.7(2) . . ? C8 C9 Pd 121.63(18) . . ? C10 C9 Pd 122.7(2) . . ? C11 C10 C9 122.8(3) . . ? C11 C10 H10A 118.6 . . ? C9 C10 H10A 118.6 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 118.9(3) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? C12 C13 C8 120.1(3) . . ? C12 C13 H13A 119.9 . . ? C8 C13 H13A 119.9 . . ? N2 C14 C15 111.3(3) . . ? N2 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N2 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 S 112.1(2) . . ? C14 C15 H15A 109.2 . . ? S C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? S C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? S C16 H16A 109.5 . . ? S C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.549 _refine_diff_density_min -1.114 _refine_diff_density_rms 0.094 #==>END data_Compound8 _database_code_depnum_ccdc_archive 'CCDC 829873' #TrackingRef '- BenzamidineCNSPd.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C19 H23 Cl N2 Pd S), C H2 Cl2 ' _chemical_formula_sum 'C77 H94 Cl6 N8 Pd4 S4' _chemical_formula_weight 1898.18 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' 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 9.7871(7) _cell_length_b 11.3669(8) _cell_length_c 19.8986(14) _cell_angle_alpha 102.6320(10) _cell_angle_beta 96.5380(10) _cell_angle_gamma 106.8330(10) _cell_volume 2030.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7920 _cell_measurement_theta_min 2.2685 _cell_measurement_theta_max 26.0285 _exptl_crystal_description parallelplpiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 962 _exptl_absorpt_coefficient_mu 1.219 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8464 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11427 _diffrn_reflns_av_R_equivalents 0.0145 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.03 _reflns_number_total 7789 _reflns_number_gt 6838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0600P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7789 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.83255(2) 0.229972(18) 0.304394(9) 0.03704(7) Uani 1 1 d . . . Pd2 Pd 0.69221(2) -0.421103(18) 0.760282(10) 0.03800(7) Uani 1 1 d . . . Cl1 Cl 0.85463(11) 0.17607(9) 0.41021(4) 0.0666(2) Uani 1 1 d . . . Cl2 Cl 0.61607(12) -0.54282(8) 0.83666(5) 0.0742(3) Uani 1 1 d . . . Cl3 Cl 1.0047(9) -0.3714(11) 1.0445(5) 0.198(5) Uani 0.50 1 d P . . Cl4 Cl 1.0145(9) -0.3690(11) 1.0137(8) 0.229(7) Uani 0.50 1 d P . . S1 S 0.90309(8) 0.05555(7) 0.24171(4) 0.04621(16) Uani 1 1 d . . . S2 S 0.68057(9) -0.60930(7) 0.67102(4) 0.05236(18) Uani 1 1 d . . . N1 N 0.6496(2) 0.3814(2) 0.23413(12) 0.0457(5) Uani 1 1 d . . . H1A H 0.5700 0.3910 0.2172 0.055 Uiso 1 1 calc R . . N2 N 0.8057(2) 0.26703(19) 0.21042(10) 0.0357(4) Uani 1 1 d . . . N3 N 0.6837(3) -0.1444(2) 0.74229(13) 0.0523(6) Uani 1 1 d . . . H3A H 0.6534 -0.0830 0.7361 0.063 Uiso 1 1 calc R . . N4 N 0.7154(3) -0.3309(2) 0.68341(12) 0.0484(6) Uani 1 1 d . . . C1 C 0.7110(3) 0.3177(2) 0.18896(13) 0.0371(5) Uani 1 1 d . . . C2 C 0.6643(3) 0.3116(3) 0.11415(13) 0.0404(6) Uani 1 1 d . . . C3 C 0.6071(4) 0.1962(3) 0.06391(16) 0.0593(8) Uani 1 1 d . . . H3B H 0.5977 0.1206 0.0766 0.071 Uiso 1 1 calc R . . C4 C 0.5639(5) 0.1931(4) -0.00504(17) 0.0737(11) Uani 1 1 d . . . H4A H 0.5255 0.1152 -0.0387 0.088 Uiso 1 1 calc R . . C5 C 0.5772(4) 0.3040(4) -0.02442(18) 0.0719(10) Uani 1 1 d . . . H5A H 0.5481 0.3011 -0.0711 0.086 Uiso 1 1 calc R . . C6 C 0.6329(5) 0.4177(4) 0.0245(2) 0.0738(10) Uani 1 1 d . . . H6A H 0.6422 0.4928 0.0114 0.089 Uiso 1 1 calc R . . C7 C 0.6759(4) 0.4224(3) 0.09412(18) 0.0612(8) Uani 1 1 d . . . H7A H 0.7129 0.5007 0.1275 0.073 Uiso 1 1 calc R . . C8 C 0.7025(3) 0.4350(2) 0.30730(13) 0.0407(6) Uani 1 1 d . . . C9 C 0.7868(3) 0.3865(3) 0.34714(13) 0.0402(6) Uani 1 1 d . . . C10 C 0.8444(3) 0.4570(3) 0.41683(14) 0.0484(6) Uani 1 1 d . . . H10A H 0.9036 0.4286 0.4449 0.058 Uiso 1 1 calc R . . C11 C 0.8160(4) 0.5674(3) 0.44512(16) 0.0597(8) Uani 1 1 d . . . H11A H 0.8575 0.6130 0.4914 0.072 Uiso 1 1 calc R . . C12 C 0.7265(4) 0.6108(3) 0.40548(17) 0.0612(8) Uani 1 1 d . . . H12A H 0.7048 0.6837 0.4252 0.073 Uiso 1 1 calc R . . C13 C 0.6691(3) 0.5445(3) 0.33589(17) 0.0530(7) Uani 1 1 d . . . H13A H 0.6087 0.5729 0.3084 0.064 Uiso 1 1 calc R . . C14 C 0.9008(3) 0.2271(3) 0.16502(14) 0.0419(6) Uani 1 1 d . . . H14A H 1.0012 0.2777 0.1854 0.050 Uiso 1 1 calc R . . H14B H 0.8777 0.2417 0.1195 0.050 Uiso 1 1 calc R . . C15 C 0.8826(3) 0.0869(3) 0.15598(14) 0.0472(6) Uani 1 1 d . . . H15A H 0.9551 0.0649 0.1311 0.057 Uiso 1 1 calc R . . H15B H 0.7872 0.0351 0.1286 0.057 Uiso 1 1 calc R . . C16 C 0.7578(5) -0.0980(3) 0.2285(2) 0.0699(10) Uani 1 1 d . . . C17 C 0.7820(9) -0.1351(5) 0.2964(3) 0.141(3) Uani 1 1 d . . . H17A H 0.7095 -0.2147 0.2936 0.212 Uiso 1 1 calc R . . H17B H 0.7750 -0.0703 0.3346 0.212 Uiso 1 1 calc R . . H17C H 0.8768 -0.1439 0.3041 0.212 Uiso 1 1 calc R . . C18 C 0.6089(4) -0.0795(4) 0.2147(3) 0.0879(13) Uani 1 1 d . . . H18A H 0.5334 -0.1591 0.2082 0.132 Uiso 1 1 calc R . . H18B H 0.5999 -0.0501 0.1732 0.132 Uiso 1 1 calc R . . H18C H 0.6003 -0.0176 0.2540 0.132 Uiso 1 1 calc R . . C19 C 0.7739(6) -0.1956(4) 0.1681(3) 0.0942(14) Uani 1 1 d . . . H19A H 0.6985 -0.2753 0.1616 0.141 Uiso 1 1 calc R . . H19B H 0.8671 -0.2066 0.1780 0.141 Uiso 1 1 calc R . . H19C H 0.7664 -0.1673 0.1262 0.141 Uiso 1 1 calc R . . C20 C 0.6924(3) -0.2244(3) 0.68352(14) 0.0416(6) Uani 1 1 d . . . C21 C 0.6722(3) -0.1788(3) 0.61951(14) 0.0452(6) Uani 1 1 d . . . C22 C 0.5344(4) -0.1939(4) 0.58663(18) 0.0651(9) Uani 1 1 d . . . H22A H 0.4542 -0.2332 0.6042 0.078 Uiso 1 1 calc R . . C23 C 0.5150(5) -0.1511(4) 0.5278(2) 0.0807(11) Uani 1 1 d . . . H23A H 0.4216 -0.1606 0.5062 0.097 Uiso 1 1 calc R . . C24 C 0.6323(5) -0.0944(4) 0.50077(18) 0.0730(11) Uani 1 1 d . . . H24A H 0.6184 -0.0670 0.4606 0.088 Uiso 1 1 calc R . . C25 C 0.7678(4) -0.0789(3) 0.53288(17) 0.0658(10) Uani 1 1 d . . . H25A H 0.8471 -0.0395 0.5149 0.079 Uiso 1 1 calc R . . C26 C 0.7906(4) -0.1207(3) 0.59230(17) 0.0555(7) Uani 1 1 d . . . H26A H 0.8845 -0.1099 0.6138 0.067 Uiso 1 1 calc R . . C27 C 0.7173(3) -0.1468(3) 0.81248(14) 0.0452(6) Uani 1 1 d . . . C28 C 0.7225(3) -0.2571(3) 0.83115(14) 0.0419(6) Uani 1 1 d . . . C29 C 0.7647(4) -0.2431(3) 0.90286(15) 0.0550(7) Uani 1 1 d . . . H29A H 0.7699 -0.3141 0.9177 0.066 Uiso 1 1 calc R . . C30 C 0.7992(4) -0.1273(4) 0.95261(17) 0.0673(9) Uani 1 1 d . . . H30A H 0.8290 -0.1212 0.9997 0.081 Uiso 1 1 calc R . . C31 C 0.7893(4) -0.0216(4) 0.93218(18) 0.0697(10) Uani 1 1 d . . . H31A H 0.8102 0.0557 0.9656 0.084 Uiso 1 1 calc R . . C32 C 0.7489(4) -0.0301(3) 0.86316(18) 0.0633(9) Uani 1 1 d . . . H32A H 0.7422 0.0414 0.8494 0.076 Uiso 1 1 calc R . . C33 C 0.7171(8) -0.4110(4) 0.6154(2) 0.112(2) Uani 1 1 d . . . H33A H 0.6194 -0.4414 0.5878 0.134 Uiso 1 1 calc R . . H33B H 0.7791 -0.3574 0.5916 0.134 Uiso 1 1 calc R . . C34 C 0.7626(9) -0.5146(4) 0.6146(2) 0.120(2) Uani 1 1 d . . . H34A H 0.8674 -0.4854 0.6293 0.144 Uiso 1 1 calc R . . H34B H 0.7392 -0.5682 0.5669 0.144 Uiso 1 1 calc R . . C35 C 0.8201(3) -0.6813(3) 0.69440(18) 0.0522(7) Uani 1 1 d . . . C36 C 0.7458(5) -0.7862(4) 0.7264(3) 0.0844(12) Uani 1 1 d . . . H36A H 0.8133 -0.8278 0.7394 0.127 Uiso 1 1 calc R . . H36B H 0.6640 -0.8471 0.6929 0.127 Uiso 1 1 calc R . . H36C H 0.7131 -0.7502 0.7673 0.127 Uiso 1 1 calc R . . C37 C 0.9489(4) -0.5833(4) 0.7476(2) 0.0768(10) Uani 1 1 d . . . H37A H 1.0201 -0.6226 0.7587 0.115 Uiso 1 1 calc R . . H37B H 0.9165 -0.5513 0.7895 0.115 Uiso 1 1 calc R . . H37C H 0.9915 -0.5141 0.7281 0.115 Uiso 1 1 calc R . . C38 C 0.8686(5) -0.7373(4) 0.6274(2) 0.0832(12) Uani 1 1 d . . . H38A H 0.9414 -0.7746 0.6392 0.125 Uiso 1 1 calc R . . H38B H 0.9082 -0.6709 0.6056 0.125 Uiso 1 1 calc R . . H38C H 0.7865 -0.8016 0.5956 0.125 Uiso 1 1 calc R . . C39 C 0.9690(15) -0.509(2) 0.9584(11) 0.115(5) Uani 0.50 1 d P . . H39A H 0.913(17) -0.512(18) 0.953(9) 0.138 Uiso 0.50 1 d P . . H39B H 1.011(18) -0.494(19) 0.945(9) 0.138 Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03487(12) 0.04007(12) 0.03602(11) 0.00919(8) 0.00584(8) 0.01291(8) Pd2 0.03814(12) 0.04055(12) 0.03945(12) 0.01438(9) 0.01087(8) 0.01480(9) Cl1 0.0846(6) 0.0826(6) 0.0497(4) 0.0311(4) 0.0162(4) 0.0413(5) Cl2 0.1029(7) 0.0618(5) 0.0603(5) 0.0321(4) 0.0291(5) 0.0134(5) Cl3 0.150(5) 0.211(9) 0.181(5) 0.042(5) 0.032(4) -0.011(5) Cl4 0.129(4) 0.258(11) 0.412(17) 0.245(13) 0.101(7) 0.096(5) S1 0.0426(4) 0.0427(4) 0.0523(4) 0.0086(3) 0.0012(3) 0.0182(3) S2 0.0647(5) 0.0434(4) 0.0516(4) 0.0118(3) 0.0093(3) 0.0227(3) N1 0.0381(12) 0.0552(14) 0.0430(12) 0.0044(10) 0.0026(9) 0.0223(10) N2 0.0337(10) 0.0369(11) 0.0349(10) 0.0070(8) 0.0077(8) 0.0103(8) N3 0.0674(16) 0.0504(14) 0.0515(13) 0.0169(11) 0.0155(12) 0.0336(12) N4 0.0658(16) 0.0434(13) 0.0450(12) 0.0155(10) 0.0207(11) 0.0247(11) C1 0.0303(12) 0.0368(12) 0.0407(13) 0.0072(10) 0.0041(10) 0.0086(10) C2 0.0372(13) 0.0441(14) 0.0403(13) 0.0109(11) 0.0051(11) 0.0146(11) C3 0.072(2) 0.0437(16) 0.0485(16) 0.0107(13) -0.0041(15) 0.0045(14) C4 0.091(3) 0.067(2) 0.0425(16) 0.0072(15) -0.0085(17) 0.0079(19) C5 0.076(2) 0.091(3) 0.0466(17) 0.0292(18) 0.0017(16) 0.019(2) C6 0.086(3) 0.073(2) 0.071(2) 0.040(2) 0.005(2) 0.026(2) C7 0.076(2) 0.0483(17) 0.0598(19) 0.0162(14) 0.0005(16) 0.0234(16) C8 0.0337(12) 0.0444(14) 0.0403(13) 0.0031(11) 0.0108(10) 0.0118(11) C9 0.0357(13) 0.0448(14) 0.0375(13) 0.0055(11) 0.0112(10) 0.0114(11) C10 0.0495(16) 0.0580(17) 0.0363(13) 0.0099(12) 0.0142(12) 0.0151(13) C11 0.067(2) 0.0642(19) 0.0396(15) -0.0025(14) 0.0159(14) 0.0183(16) C12 0.067(2) 0.0560(19) 0.0584(18) -0.0026(15) 0.0220(16) 0.0256(16) C13 0.0515(17) 0.0525(17) 0.0590(17) 0.0089(14) 0.0145(14) 0.0257(14) C14 0.0390(13) 0.0436(14) 0.0452(14) 0.0096(11) 0.0144(11) 0.0159(11) C15 0.0497(16) 0.0435(15) 0.0484(15) 0.0049(12) 0.0135(12) 0.0190(12) C16 0.094(3) 0.0375(16) 0.071(2) 0.0162(15) 0.0153(19) 0.0099(16) C17 0.241(8) 0.064(3) 0.099(4) 0.047(3) 0.000(4) 0.015(4) C18 0.058(2) 0.067(2) 0.108(3) -0.002(2) 0.026(2) -0.0115(18) C19 0.113(4) 0.0408(19) 0.117(4) 0.000(2) 0.014(3) 0.025(2) C20 0.0396(13) 0.0456(14) 0.0429(13) 0.0157(11) 0.0119(11) 0.0144(11) C21 0.0519(16) 0.0412(14) 0.0457(14) 0.0162(12) 0.0094(12) 0.0163(12) C22 0.0525(18) 0.078(2) 0.071(2) 0.0329(18) 0.0079(16) 0.0214(16) C23 0.082(3) 0.094(3) 0.074(2) 0.030(2) -0.008(2) 0.042(2) C24 0.116(3) 0.070(2) 0.0502(18) 0.0271(17) 0.015(2) 0.048(2) C25 0.094(3) 0.0548(19) 0.060(2) 0.0248(16) 0.034(2) 0.0273(19) C26 0.0541(17) 0.0581(18) 0.0566(17) 0.0223(15) 0.0154(14) 0.0145(14) C27 0.0451(15) 0.0484(15) 0.0431(14) 0.0095(12) 0.0128(12) 0.0169(12) C28 0.0345(13) 0.0499(15) 0.0420(13) 0.0102(11) 0.0110(11) 0.0149(11) C29 0.0634(19) 0.0621(19) 0.0423(15) 0.0127(13) 0.0137(13) 0.0241(15) C30 0.075(2) 0.081(2) 0.0406(16) 0.0044(16) 0.0134(15) 0.0249(19) C31 0.084(3) 0.064(2) 0.0527(19) -0.0060(16) 0.0196(17) 0.0238(18) C32 0.081(2) 0.0499(18) 0.061(2) 0.0060(15) 0.0236(17) 0.0280(17) C33 0.246(7) 0.074(3) 0.062(2) 0.037(2) 0.083(3) 0.087(4) C34 0.266(8) 0.080(3) 0.072(3) 0.045(2) 0.090(4) 0.103(4) C35 0.0503(16) 0.0383(14) 0.0702(19) 0.0145(13) 0.0164(14) 0.0155(12) C36 0.079(3) 0.062(2) 0.131(4) 0.053(2) 0.029(3) 0.0268(19) C37 0.056(2) 0.063(2) 0.103(3) 0.014(2) 0.0051(19) 0.0172(17) C38 0.095(3) 0.067(2) 0.096(3) 0.009(2) 0.036(2) 0.042(2) C39 0.085(9) 0.114(9) 0.147(12) 0.067(9) 0.011(9) 0.012(9) _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 C9 1.993(3) . ? Pd1 N2 2.010(2) . ? Pd1 Cl1 2.3224(8) . ? Pd1 S1 2.4229(7) . ? Pd2 C28 1.996(3) . ? Pd2 N4 2.018(2) . ? Pd2 Cl2 2.3152(8) . ? Pd2 S2 2.4280(8) . ? Cl3 Cl4 0.635(15) . ? Cl3 C39 1.45(2) 2_747 ? Cl3 C39 1.97(3) . ? Cl4 C39 1.65(2) 2_747 ? Cl4 C39 1.63(3) . ? Cl4 H39A 1.74(18) . ? S1 C15 1.818(3) . ? S1 C16 1.848(4) . ? S2 C34 1.816(4) . ? S2 C35 1.849(3) . ? N1 C1 1.335(3) . ? N1 C8 1.420(3) . ? N1 H1A 0.8600 . ? N2 C1 1.304(3) . ? N2 C14 1.465(3) . ? N3 C20 1.343(3) . ? N3 C27 1.406(4) . ? N3 H3A 0.8600 . ? N4 C20 1.294(4) . ? N4 C33 1.462(4) . ? C1 C2 1.487(4) . ? C2 C7 1.380(4) . ? C2 C3 1.382(4) . ? C3 C4 1.379(4) . ? C3 H3B 0.9300 . ? C4 C5 1.372(5) . ? C4 H4A 0.9300 . ? C5 C6 1.355(5) . ? C5 H5A 0.9300 . ? C6 C7 1.385(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.386(4) . ? C8 C13 1.396(4) . ? C9 C10 1.399(4) . ? C10 C11 1.377(4) . ? C10 H10A 0.9300 . ? C11 C12 1.377(5) . ? C11 H11A 0.9300 . ? C12 C13 1.386(4) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C15 1.518(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C19 1.504(5) . ? C16 C17 1.514(6) . ? C16 C18 1.535(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.490(4) . ? C21 C22 1.376(4) . ? C21 C26 1.388(4) . ? C22 C23 1.377(5) . ? C22 H22A 0.9300 . ? C23 C24 1.374(6) . ? C23 H23A 0.9300 . ? C24 C25 1.349(6) . ? C24 H24A 0.9300 . ? C25 C26 1.386(4) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.397(4) . ? C27 C32 1.406(4) . ? C28 C29 1.400(4) . ? C29 C30 1.387(5) . ? C29 H29A 0.9300 . ? C30 C31 1.375(6) . ? C30 H30A 0.9300 . ? C31 C32 1.359(5) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.372(6) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.515(5) . ? C35 C37 1.522(5) . ? C35 C38 1.535(5) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 Cl3 1.45(2) 2_747 ? C39 Cl4 1.65(2) 2_747 ? C39 C39 1.64(4) 2_747 ? C39 H39A 0.53(15) . ? C39 H39B 0.53(16) . ? 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 C9 Pd1 N2 89.35(10) . . ? C9 Pd1 Cl1 92.54(8) . . ? N2 Pd1 Cl1 176.87(6) . . ? C9 Pd1 S1 172.22(8) . . ? N2 Pd1 S1 84.17(6) . . ? Cl1 Pd1 S1 94.13(3) . . ? C28 Pd2 N4 90.95(10) . . ? C28 Pd2 Cl2 93.22(8) . . ? N4 Pd2 Cl2 168.17(8) . . ? C28 Pd2 S2 173.78(8) . . ? N4 Pd2 S2 85.54(7) . . ? Cl2 Pd2 S2 91.22(3) . . ? Cl4 Cl3 C39 97(2) . 2_747 ? Cl4 Cl3 C39 49.4(17) . . ? C39 Cl3 C39 55.1(12) 2_747 . ? Cl3 Cl4 C39 60.9(17) . 2_747 ? Cl3 Cl4 C39 113.4(19) . . ? C39 Cl4 C39 60.3(13) 2_747 . ? Cl3 Cl4 H39A 111(6) . . ? C39 Cl4 H39A 69(6) 2_747 . ? C39 Cl4 H39A 18(5) . . ? C15 S1 C16 103.02(15) . . ? C15 S1 Pd1 97.30(9) . . ? C16 S1 Pd1 110.51(13) . . ? C34 S2 C35 102.4(2) . . ? C34 S2 Pd2 92.27(13) . . ? C35 S2 Pd2 113.20(11) . . ? C1 N1 C8 126.7(2) . . ? C1 N1 H1A 116.7 . . ? C8 N1 H1A 116.7 . . ? C1 N2 C14 121.4(2) . . ? C1 N2 Pd1 125.08(17) . . ? C14 N2 Pd1 113.49(16) . . ? C20 N3 C27 129.2(2) . . ? C20 N3 H3A 115.4 . . ? C27 N3 H3A 115.4 . . ? C20 N4 C33 116.7(3) . . ? C20 N4 Pd2 126.13(19) . . ? C33 N4 Pd2 114.7(2) . . ? N2 C1 N1 121.3(2) . . ? N2 C1 C2 123.8(2) . . ? N1 C1 C2 114.9(2) . . ? C7 C2 C3 118.9(3) . . ? C7 C2 C1 120.0(3) . . ? C3 C2 C1 121.1(2) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3B 120.0 . . ? C2 C3 H3B 120.0 . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4A 119.7 . . ? C3 C4 H4A 119.7 . . ? C6 C5 C4 119.9(3) . . ? C6 C5 H5A 120.1 . . ? C4 C5 H5A 120.1 . . ? C5 C6 C7 120.3(3) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C2 C7 C6 120.4(3) . . ? C2 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C9 C8 C13 122.1(3) . . ? C9 C8 N1 122.9(2) . . ? C13 C8 N1 115.0(3) . . ? C8 C9 C10 116.6(3) . . ? C8 C9 Pd1 120.89(18) . . ? C10 C9 Pd1 122.4(2) . . ? C11 C10 C9 121.9(3) . . ? C11 C10 H10A 119.0 . . ? C9 C10 H10A 119.0 . . ? C12 C11 C10 120.5(3) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 119.3(3) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C12 C13 C8 119.6(3) . . ? C12 C13 H13A 120.2 . . ? C8 C13 H13A 120.2 . . ? N2 C14 C15 110.9(2) . . ? N2 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? N2 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.0 . . ? C14 C15 S1 109.43(18) . . ? C14 C15 H15A 109.8 . . ? S1 C15 H15A 109.8 . . ? C14 C15 H15B 109.8 . . ? S1 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? C19 C16 C17 110.5(4) . . ? C19 C16 C18 110.7(4) . . ? C17 C16 C18 111.5(4) . . ? C19 C16 S1 109.8(3) . . ? C17 C16 S1 104.7(3) . . ? C18 C16 S1 109.5(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N4 C20 N3 122.4(3) . . ? N4 C20 C21 123.9(2) . . ? N3 C20 C21 113.6(2) . . ? C22 C21 C26 119.1(3) . . ? C22 C21 C20 119.8(3) . . ? C26 C21 C20 121.1(3) . . ? C21 C22 C23 120.1(3) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C22 C23 C24 120.6(4) . . ? C22 C23 H23A 119.7 . . ? C24 C23 H23A 119.7 . . ? C25 C24 C23 119.6(3) . . ? C25 C24 H24A 120.2 . . ? C23 C24 H24A 120.2 . . ? C24 C25 C26 121.1(3) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C25 C26 C21 119.5(3) . . ? C25 C26 H26A 120.2 . . ? C21 C26 H26A 120.2 . . ? C28 C27 N3 122.4(2) . . ? C28 C27 C32 121.6(3) . . ? N3 C27 C32 115.9(3) . . ? C27 C28 C29 115.8(3) . . ? C27 C28 Pd2 122.6(2) . . ? C29 C28 Pd2 121.2(2) . . ? C30 C29 C28 122.5(3) . . ? C30 C29 H29A 118.8 . . ? C28 C29 H29A 118.8 . . ? C31 C30 C29 119.9(3) . . ? C31 C30 H30A 120.1 . . ? C29 C30 H30A 120.1 . . ? C32 C31 C30 120.0(3) . . ? C32 C31 H31A 120.0 . . ? C30 C31 H31A 120.0 . . ? C31 C32 C27 120.2(3) . . ? C31 C32 H32A 119.9 . . ? C27 C32 H32A 119.9 . . ? C34 C33 N4 118.0(4) . . ? C34 C33 H33A 107.8 . . ? N4 C33 H33A 107.8 . . ? C34 C33 H33B 107.8 . . ? N4 C33 H33B 107.8 . . ? H33A C33 H33B 107.1 . . ? C33 C34 S2 113.3(4) . . ? C33 C34 H34A 108.9 . . ? S2 C34 H34A 108.9 . . ? C33 C34 H34B 108.9 . . ? S2 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C36 C35 C37 109.9(3) . . ? C36 C35 C38 110.4(3) . . ? C37 C35 C38 111.0(3) . . ? C36 C35 S2 105.6(2) . . ? C37 C35 S2 110.9(2) . . ? C38 C35 S2 109.0(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Cl3 C39 Cl4 22.5(7) 2_747 2_747 ? Cl3 C39 Cl4 137.5(13) 2_747 . ? Cl4 C39 Cl4 119.7(13) 2_747 . ? Cl3 C39 C39 78.7(15) 2_747 2_747 ? Cl4 C39 C39 59.2(12) 2_747 2_747 ? Cl4 C39 C39 60.4(15) . 2_747 ? Cl3 C39 Cl3 124.9(12) 2_747 . ? Cl4 C39 Cl3 104.6(11) 2_747 . ? Cl4 C39 Cl3 17.2(5) . . ? C39 C39 Cl3 46.2(14) 2_747 . ? Cl3 C39 H39A 115(10) 2_747 . ? Cl4 C39 H39A 110(10) 2_747 . ? Cl4 C39 H39A 94(10) . . ? C39 C39 H39A 114(10) 2_747 . ? Cl3 C39 H39A 92(10) . . ? Cl3 C39 H39B 92(10) 2_747 . ? Cl4 C39 H39B 110(10) 2_747 . ? Cl4 C39 H39B 93(10) . . ? C39 C39 H39B 112(10) 2_747 . ? Cl3 C39 H39B 107(10) . . ? H39A C39 H39B 130(10) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.528 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.062 #==>END