Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Elizabeth J. MacLean' 'Richard I. Robinson' 'Simon J. Teat' 'Claire Wilson' 'Simon Woodward' _publ_contact_author_name 'Dr Simon Woodward' _publ_contact_author_address ; School of Chemistry The University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email 'Dr Simon Woodward' _journal_name_full ' J. Chem. Soc., Dalton Transactions' _publ_section_title ; Sequential Oxidation of Sulfur Dioxide to Sulfate at a Palladium Centre ; data_pdtrac _database_code_CSD 186000 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H41 Cl N4 O2 Pd' _chemical_formula_weight 643.53 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 11.0537(9) _cell_length_b 22.089(2) _cell_length_c 12.7592(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.132(1) _cell_angle_gamma 90.00 _cell_volume 3066.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7775 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.6 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8119 _exptl_absorpt_correction_T_max 0.9191 _exptl_absorpt_process_details 'XPREP' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.5 _diffrn_reflns_number 26915 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 28.79 _reflns_number_total 7342 _reflns_number_gt 6181 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2000)' _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^)+(0.0276P)^2^+2.4234P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed, MeCN from delta-F' _refine_ls_hydrogen_treatment 'riding model, MeCN rigid rotating group' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7156 _refine_ls_number_parameters 354 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0681 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Pd Pd 0.453938(13) 0.069372(6) 0.420707(12) 0.02226(5) Uani 1 1 d . . . Cl1 Cl 0.45635(5) 0.22395(2) 0.91041(4) 0.02927(11) Uani 1 1 d . . . N1 N 0.54856(14) 0.13039(7) 0.50699(12) 0.0213(3) Uani 1 1 d . . . C2 C 0.52752(17) 0.14033(8) 0.60599(15) 0.0214(4) Uani 1 1 d . . . C3 C 0.59772(17) 0.18316(9) 0.66980(15) 0.0221(4) Uani 1 1 d . . . H3A H 0.5823 0.1913 0.7393 0.026 Uiso 1 1 calc R . . C4 C 0.69144(17) 0.21421(8) 0.63093(15) 0.0218(4) Uani 1 1 d . . . C5 C 0.70901(17) 0.20223(9) 0.52646(15) 0.0227(4) Uani 1 1 d . . . H5A H 0.7710 0.2231 0.4979 0.027 Uiso 1 1 calc R . . C6 C 0.63571(17) 0.16000(8) 0.46538(15) 0.0213(4) Uani 1 1 d . . . C7 C 0.77722(18) 0.25976(9) 0.69735(15) 0.0241(4) Uani 1 1 d . . . C8 C 0.9066(2) 0.23171(12) 0.7176(2) 0.0392(5) Uani 1 1 d . . . H8A H 0.9054 0.1938 0.7574 0.059 Uiso 1 1 calc R . . H8B H 0.9645 0.2600 0.7590 0.059 Uiso 1 1 calc R . . H8C H 0.9324 0.2234 0.6494 0.059 Uiso 1 1 calc R . . C9 C 0.7795(2) 0.31915(10) 0.63504(17) 0.0327(5) Uani 1 1 d . . . H9A H 0.6972 0.3371 0.6222 0.049 Uiso 1 1 calc R . . H9B H 0.8053 0.3108 0.5668 0.049 Uiso 1 1 calc R . . H9C H 0.8376 0.3474 0.6764 0.049 Uiso 1 1 calc R . . C10" C 0.3328(2) 0.06561(10) 0.94207(17) 0.0320(5) Uani 1 1 d . . . H10A H 0.3736 0.0262 0.9427 0.048 Uiso 1 1 calc R . . H10B H 0.2970 0.0700 1.0067 0.048 Uiso 1 1 calc R . . H10C H 0.3929 0.0979 0.9395 0.048 Uiso 1 1 calc R . . C10 C 0.7385(2) 0.27395(10) 0.80393(16) 0.0299(4) Uani 1 1 d . . . H10D H 0.6559 0.2916 0.7912 0.045 Uiso 1 1 calc R . . H10E H 0.7966 0.3028 0.8437 0.045 Uiso 1 1 calc R . . H10F H 0.7382 0.2365 0.8452 0.045 Uiso 1 1 calc R . . C10' C 0.9307(2) 0.16609(12) 0.17433(18) 0.0358(5) Uani 1 1 d . . . H10G H 0.9483 0.1227 0.1827 0.054 Uiso 1 1 calc R . . H10H H 0.9422 0.1854 0.2446 0.054 Uiso 1 1 calc R . . H10I H 0.9866 0.1845 0.1317 0.054 Uiso 1 1 calc R . . N1' N 0.55531(15) 0.09855(7) 0.31434(13) 0.0233(3) Uani 1 1 d . . . C2' C 0.63958(17) 0.14192(9) 0.35382(15) 0.0223(4) Uani 1 1 d . . . C3' C 0.71830(18) 0.16632(9) 0.29231(15) 0.0240(4) Uani 1 1 d . . . H3'A H 0.7777 0.1955 0.3220 0.029 Uiso 1 1 calc R . . C4' C 0.71073(18) 0.14803(9) 0.18575(15) 0.0245(4) Uani 1 1 d . . . C5' C 0.62137(19) 0.10541(9) 0.14708(16) 0.0270(4) Uani 1 1 d . . . H5'A H 0.6111 0.0929 0.0748 0.032 Uiso 1 1 calc R . . C6' C 0.54740(19) 0.08115(9) 0.21317(16) 0.0264(4) Uani 1 1 d . . . H6'A H 0.4889 0.0511 0.1857 0.032 Uiso 1 1 calc R . . C7' C 0.7975(2) 0.17501(10) 0.11794(16) 0.0277(4) Uani 1 1 d . . . C8' C 0.7690(2) 0.24308(10) 0.10454(18) 0.0355(5) Uani 1 1 d . . . H8'A H 0.7787 0.2623 0.1748 0.053 Uiso 1 1 calc R . . H8'B H 0.6844 0.2485 0.0672 0.053 Uiso 1 1 calc R . . H8'C H 0.8259 0.2618 0.0632 0.053 Uiso 1 1 calc R . . C9' C 0.7811(2) 0.14526(11) 0.00743(16) 0.0346(5) Uani 1 1 d . . . H9'A H 0.7993 0.1019 0.0154 0.052 Uiso 1 1 calc R . . H9'B H 0.8372 0.1641 -0.0344 0.052 Uiso 1 1 calc R . . H9'C H 0.6961 0.1508 -0.0292 0.052 Uiso 1 1 calc R . . N1" N 0.38031(15) 0.06136(7) 0.55319(13) 0.0227(3) Uani 1 1 d . . . C2" C 0.42719(17) 0.10157(8) 0.63242(15) 0.0216(4) Uani 1 1 d . . . C3" C 0.38100(17) 0.10425(9) 0.72588(16) 0.0234(4) Uani 1 1 d . . . H3"A H 0.4137 0.1326 0.7794 0.028 Uiso 1 1 calc R . . C4" C 0.28534(18) 0.06506(9) 0.74227(16) 0.0244(4) Uani 1 1 d . . . C5" C 0.24270(18) 0.02398(9) 0.66147(17) 0.0268(4) Uani 1 1 d . . . H5"A H 0.1799 -0.0039 0.6702 0.032 Uiso 1 1 calc R . . C6" C 0.29103(18) 0.02350(9) 0.56867(17) 0.0256(4) Uani 1 1 d . . . H6"A H 0.2598 -0.0046 0.5143 0.031 Uiso 1 1 calc R . . C7" C 0.23010(19) 0.06993(9) 0.84342(17) 0.0271(4) Uani 1 1 d . . . C8" C 0.1352(2) 0.01976(11) 0.84942(19) 0.0377(5) Uani 1 1 d . . . H8"A H 0.1755 -0.0198 0.8509 0.057 Uiso 1 1 calc R . . H8"B H 0.0696 0.0222 0.7870 0.057 Uiso 1 1 calc R . . H8"C H 0.1001 0.0249 0.9142 0.057 Uiso 1 1 calc R . . C9" C 0.1655(2) 0.13182(10) 0.84188(19) 0.0349(5) Uani 1 1 d . . . H9"A H 0.1006 0.1344 0.7789 0.052 Uiso 1 1 calc R . . H9"B H 0.2255 0.1642 0.8395 0.052 Uiso 1 1 calc R . . H9"C H 0.1292 0.1362 0.9062 0.052 Uiso 1 1 calc R . . O1 O 0.36682(16) 0.00061(7) 0.33001(14) 0.0377(4) Uani 1 1 d . . . O2 O 0.2023(2) 0.05394(10) 0.28765(19) 0.0667(6) Uani 1 1 d . . . C1A C 0.2681(3) 0.00847(10) 0.28404(19) 0.0401(6) Uani 1 1 d . . . C2A C 0.2126(3) -0.04480(14) 0.2124(3) 0.0569(8) Uani 1 1 d . . . H2A1 H 0.2782 -0.0656 0.1839 0.085 Uiso 1 1 calc R . . H2A2 H 0.1517 -0.0292 0.1534 0.085 Uiso 1 1 calc R . . H2A3 H 0.1729 -0.0733 0.2545 0.085 Uiso 1 1 calc R . . N1S N -0.0939(3) 0.07627(13) 0.5460(3) 0.0771(9) Uani 1 1 d . . . C2S C -0.0170(2) 0.09853(12) 0.5124(2) 0.0450(6) Uani 1 1 d . . . C3S C 0.0801(3) 0.12902(12) 0.4705(2) 0.0473(6) Uani 1 1 d . . . H3S1 H 0.0504 0.1684 0.4412 0.071 Uiso 1 1 calc R . . H3S2 H 0.1050 0.1043 0.4142 0.071 Uiso 1 1 calc R . . H3S3 H 0.1507 0.1351 0.5278 0.071 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 0.02094(8) 0.02117(8) 0.02456(8) -0.00536(6) 0.00366(5) -0.00174(6) Cl1 0.0305(2) 0.0281(2) 0.0308(2) -0.00367(19) 0.0096(2) -0.00339(19) N1 0.0219(8) 0.0192(7) 0.0223(8) -0.0023(6) 0.0030(6) 0.0008(6) C2 0.0201(9) 0.0203(9) 0.0241(9) 0.0006(7) 0.0047(7) 0.0020(7) C3 0.0225(9) 0.0223(9) 0.0218(9) -0.0019(7) 0.0049(7) -0.0007(7) C4 0.0210(9) 0.0204(9) 0.0236(9) -0.0001(7) 0.0029(7) 0.0008(7) C5 0.0222(9) 0.0222(9) 0.0241(9) 0.0002(7) 0.0051(7) -0.0029(7) C6 0.0200(9) 0.0212(9) 0.0230(9) -0.0015(7) 0.0042(7) 0.0013(7) C7 0.0229(9) 0.0263(10) 0.0232(9) -0.0034(8) 0.0039(7) -0.0056(8) C8 0.0260(11) 0.0444(14) 0.0444(13) -0.0113(11) -0.0014(10) -0.0011(10) C9 0.0415(12) 0.0284(11) 0.0299(11) -0.0034(9) 0.0110(9) -0.0135(9) C10" 0.0347(11) 0.0325(11) 0.0291(10) 0.0022(9) 0.0065(9) 0.0011(9) C10 0.0318(11) 0.0339(11) 0.0237(10) -0.0052(8) 0.0039(8) -0.0101(9) C10' 0.0303(11) 0.0469(14) 0.0314(11) -0.0008(10) 0.0089(9) -0.0012(10) N1' 0.0211(8) 0.0239(8) 0.0244(8) -0.0033(6) 0.0028(6) 0.0024(6) C2' 0.0220(9) 0.0221(9) 0.0217(9) -0.0031(7) 0.0008(7) 0.0021(7) C3' 0.0240(9) 0.0247(9) 0.0226(9) -0.0020(7) 0.0018(7) 0.0002(7) C4' 0.0257(10) 0.0255(10) 0.0221(9) 0.0008(8) 0.0033(7) 0.0046(8) C5' 0.0292(10) 0.0295(10) 0.0213(9) -0.0046(8) 0.0017(8) 0.0029(8) C6' 0.0247(10) 0.0261(10) 0.0273(10) -0.0060(8) 0.0012(8) 0.0001(8) C7' 0.0333(11) 0.0294(11) 0.0211(9) -0.0007(8) 0.0064(8) -0.0007(8) C8' 0.0478(14) 0.0293(11) 0.0299(11) 0.0006(9) 0.0080(10) -0.0038(10) C9' 0.0471(13) 0.0355(12) 0.0230(10) -0.0012(9) 0.0111(9) -0.0023(10) N1" 0.0222(8) 0.0187(8) 0.0271(8) -0.0026(6) 0.0037(6) -0.0002(6) C2" 0.0207(9) 0.0166(9) 0.0266(10) -0.0009(7) 0.0019(7) 0.0005(7) C3" 0.0229(9) 0.0203(9) 0.0266(10) -0.0011(7) 0.0038(7) 0.0002(7) C4" 0.0228(9) 0.0224(9) 0.0283(10) 0.0046(8) 0.0049(8) 0.0035(7) C5" 0.0241(10) 0.0214(9) 0.0343(11) 0.0031(8) 0.0036(8) -0.0032(7) C6" 0.0240(9) 0.0201(9) 0.0315(10) -0.0020(8) 0.0013(8) -0.0017(7) C7" 0.0265(10) 0.0259(10) 0.0301(10) 0.0017(8) 0.0084(8) -0.0027(8) C8" 0.0365(12) 0.0421(13) 0.0373(12) 0.0022(10) 0.0140(10) -0.0109(10) C9" 0.0341(11) 0.0359(12) 0.0371(12) 0.0026(10) 0.0128(9) 0.0078(9) O1 0.0482(10) 0.0229(8) 0.0459(10) -0.0162(7) 0.0190(8) -0.0079(7) O2 0.0608(13) 0.0514(12) 0.0778(15) -0.0158(11) -0.0160(11) 0.0146(10) C1A 0.0672(18) 0.0240(11) 0.0348(12) -0.0025(9) 0.0247(12) 0.0000(11) C2A 0.0464(16) 0.0599(18) 0.0612(18) -0.0247(15) 0.0006(13) -0.0061(14) N1S 0.0611(17) 0.0661(19) 0.105(2) -0.0123(17) 0.0158(17) -0.0284(15) C2S 0.0429(14) 0.0366(13) 0.0517(15) -0.0080(11) -0.0026(12) -0.0037(11) C3S 0.0542(16) 0.0358(13) 0.0527(16) 0.0126(11) 0.0121(12) 0.0118(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N1 1.9280(16) . y Pd N1' 2.0119(17) . y Pd N1" 2.0087(17) . y Pd O1 2.0448(15) . y N1 C2 1.342(2) . ? N1 C6 1.348(2) . ? C2 C3 1.392(3) . ? C2 C2" 1.486(3) . ? C3 C4 1.404(3) . ? C4 C5 1.406(3) . ? C4 C7 1.532(3) . ? C5 C6 1.383(3) . ? C6 C2' 1.486(3) . ? C7 C10 1.528(3) . ? C7 C9 1.537(3) . ? C7 C8 1.539(3) . ? C10" C7" 1.542(3) . ? C10' C7' 1.533(3) . ? N1' C6' 1.335(3) . ? N1' C2' 1.369(2) . ? C2' C3' 1.380(3) . ? C3' C4' 1.407(3) . ? C4' C5' 1.391(3) . ? C4' C7' 1.522(3) . ? C5' C6' 1.382(3) . ? C7' C9' 1.537(3) . ? C7' C8' 1.540(3) . ? N1" C6" 1.335(2) . ? N1" C2" 1.377(2) . ? C2" C3" 1.379(3) . ? C3" C4" 1.410(3) . ? C4" C5" 1.392(3) . ? C4" C7" 1.526(3) . ? C5" C6" 1.382(3) . ? C7" C8" 1.537(3) . ? C7" C9" 1.541(3) . ? O1 C1A 1.157(3) . ? O2 C1A 1.246(3) . ? C1A C2A 1.549(3) . ? N1S C2S 1.130(4) . ? C2S C3S 1.447(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd N1" 80.82(7) . . y N1 Pd N1' 81.41(7) . . y N1" Pd N1' 162.18(6) . . y N1 Pd O1 175.23(7) . . y N1" Pd O1 100.99(6) . . y N1' Pd O1 96.83(6) . . y C2 N1 C6 123.05(16) . . ? C2 N1 Pd 119.04(13) . . ? C6 N1 Pd 117.89(12) . . ? N1 C2 C3 119.38(17) . . ? N1 C2 C2" 112.28(16) . . ? C3 C2 C2" 128.34(17) . . ? C2 C3 C4 119.71(17) . . ? C3 C4 C5 118.47(17) . . ? C3 C4 C7 123.29(17) . . ? C5 C4 C7 118.23(16) . . ? C6 C5 C4 119.77(17) . . ? N1 C6 C5 119.59(17) . . ? N1 C6 C2' 112.94(16) . . ? C5 C6 C2' 127.47(17) . . ? C10 C7 C4 112.59(16) . . ? C10 C7 C9 108.55(17) . . ? C4 C7 C9 109.85(16) . . ? C10 C7 C8 109.31(17) . . ? C4 C7 C8 107.16(16) . . ? C9 C7 C8 109.34(18) . . ? C6' N1' C2' 118.81(17) . . ? C6' N1' Pd 127.63(14) . . ? C2' N1' Pd 113.56(12) . . ? N1' C2' C3' 121.36(17) . . ? N1' C2' C6 114.08(16) . . ? C3' C2' C6 124.55(17) . . ? C2' C3' C4' 120.09(18) . . ? C5' C4' C3' 117.07(18) . . ? C5' C4' C7' 122.88(17) . . ? C3' C4' C7' 120.05(18) . . ? C6' C5' C4' 120.38(18) . . ? N1' C6' C5' 122.23(19) . . ? C4' C7' C10' 109.40(17) . . ? C4' C7' C9' 111.66(17) . . ? C10' C7' C9' 108.95(18) . . ? C4' C7' C8' 107.96(17) . . ? C10' C7' C8' 109.78(19) . . ? C9' C7' C8' 109.07(17) . . ? C6" N1" C2" 119.23(17) . . ? C6" N1" Pd 126.83(14) . . ? C2" N1" Pd 113.91(13) . . ? N1" C2" C3" 120.94(17) . . ? N1" C2" C2 113.87(17) . . ? C3" C2" C2 125.19(17) . . ? C2" C3" C4" 120.21(18) . . ? C5" C4" C3" 117.09(18) . . ? C5" C4" C7" 122.60(18) . . ? C3" C4" C7" 120.28(18) . . ? C6" C5" C4" 120.54(18) . . ? N1" C6" C5" 121.96(18) . . ? C4" C7" C8" 111.68(17) . . ? C4" C7" C9" 107.78(16) . . ? C8" C7" C9" 108.76(18) . . ? C4" C7" C10" 109.85(16) . . ? C8" C7" C10" 108.98(18) . . ? C9" C7" C10" 109.76(18) . . ? C1A O1 Pd 118.93(16) . . ? O1 C1A O2 127.4(2) . . ? O1 C1A C2A 115.2(2) . . ? O2 C1A C2A 117.4(3) . . ? N1S C2S C3S 178.0(3) . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.554 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.061 data_pdtrpy _database_code_CSD 186001 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28.75 H40.50 Cl5.50 N3 O Pd' _chemical_formula_weight 745.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 15.9261(13) _cell_length_b 13.1424(11) _cell_length_c 17.6773(14) _cell_angle_alpha 90.00 _cell_angle_beta 112.388(2) _cell_angle_gamma 90.00 _cell_volume 3421.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5234 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 28.85 _exptl_crystal_description block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1526 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.876 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Sadabs v2.03 (Bruker 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18584 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.86 _reflns_number_total 8213 _reflns_number_gt 6745 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT version 6.01 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _refine_special_details ; 2 partially occupied DCM sites. C2s 0.5 occupied due to symm related neighbour, C3s 0.25, Cl8 modelled over 2 sites 0.15 and 0.1 occupation. Geometry restraints applied. Largest residual electron density peak in region of DCM. ; _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^)+(0.0589P)^2^+4.3919P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed, H2O from delta-F, C3s omitted' _refine_ls_hydrogen_treatment 'riding model, H2O refined with restraints' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7861 _refine_ls_number_parameters 390 _refine_ls_number_restraints 29 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1171 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.153 _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 0.919173(14) 0.592290(16) -0.015697(12) 0.01993(8) Uani 1 1 d . . . Cl1 Cl 1.02660(5) 0.71906(6) 0.01813(5) 0.02973(17) Uani 1 1 d . . . N1 N 0.82619(16) 0.48890(18) -0.04699(14) 0.0218(5) Uani 1 1 d . . . C2 C 0.80385(19) 0.4443(2) -0.12050(17) 0.0214(5) Uani 1 1 d . . . C3 C 0.7383(2) 0.3688(2) -0.14395(17) 0.0236(6) Uani 1 1 d . . . H3A H 0.7219 0.3370 -0.1959 0.028 Uiso 1 1 calc R . . C4 C 0.69631(19) 0.3393(2) -0.09058(18) 0.0235(6) Uani 1 1 d . . . C5 C 0.7218(2) 0.3873(2) -0.01458(18) 0.0236(6) Uani 1 1 d . . . H5A H 0.6950 0.3679 0.0229 0.028 Uiso 1 1 calc R . . C6 C 0.78709(19) 0.4639(2) 0.00555(17) 0.0227(6) Uani 1 1 d . . . C7 C 0.6242(2) 0.2558(2) -0.11762(19) 0.0287(6) Uani 1 1 d . . . C8 C 0.5500(2) 0.2867(3) -0.1997(2) 0.0406(8) Uani 1 1 d . . . H8A H 0.5036 0.2334 -0.2179 0.061 Uiso 1 1 calc R . . H8B H 0.5771 0.2958 -0.2406 0.061 Uiso 1 1 calc R . . H8C H 0.5221 0.3507 -0.1929 0.061 Uiso 1 1 calc R . . C9 C 0.6695(3) 0.1578(3) -0.1306(2) 0.0414(8) Uani 1 1 d . . . H9A H 0.6242 0.1032 -0.1484 0.062 Uiso 1 1 calc R . . H9B H 0.7183 0.1382 -0.0791 0.062 Uiso 1 1 calc R . . H9C H 0.6947 0.1694 -0.1724 0.062 Uiso 1 1 calc R . . C10 C 0.5799(3) 0.2385(4) -0.0561(2) 0.0531(12) Uani 1 1 d . . . H10D H 0.5343 0.1845 -0.0760 0.080 Uiso 1 1 calc R . . H10E H 0.5506 0.3015 -0.0494 0.080 Uiso 1 1 calc R . . H10F H 0.6263 0.2184 -0.0034 0.080 Uiso 1 1 calc R . . N1' N 0.88517(17) 0.59601(18) 0.08390(15) 0.0230(5) Uani 1 1 d . . . C2' C 0.81756(19) 0.5293(2) 0.07932(17) 0.0224(5) Uani 1 1 d . . . C3' C 0.7777(2) 0.5300(2) 0.13612(18) 0.0249(6) Uani 1 1 d . . . H3'A H 0.7319 0.4816 0.1323 0.030 Uiso 1 1 calc R . . C4' C 0.8043(2) 0.6016(2) 0.19939(19) 0.0262(6) Uani 1 1 d . . . C5' C 0.8768(2) 0.6645(2) 0.20502(19) 0.0294(6) Uani 1 1 d . . . H5'A H 0.8998 0.7112 0.2492 0.035 Uiso 1 1 calc R . . C6' C 0.9158(2) 0.6601(2) 0.14739(18) 0.0271(6) Uani 1 1 d . . . H6'A H 0.9655 0.7036 0.1530 0.033 Uiso 1 1 calc R . . C7' C 0.7550(2) 0.6153(3) 0.2582(2) 0.0318(7) Uani 1 1 d . . . C8' C 0.7287(4) 0.7279(3) 0.2573(3) 0.0597(13) Uani 1 1 d . . . H8'A H 0.6969 0.7381 0.2945 0.090 Uiso 1 1 calc R . . H8'B H 0.6888 0.7475 0.2017 0.090 Uiso 1 1 calc R . . H8'C H 0.7836 0.7700 0.2751 0.090 Uiso 1 1 calc R . . C9' C 0.8170(3) 0.5822(4) 0.3436(3) 0.0619(14) Uani 1 1 d . . . H9'A H 0.8324 0.5101 0.3428 0.093 Uiso 1 1 calc R . . H9'B H 0.7860 0.5923 0.3814 0.093 Uiso 1 1 calc R . . H9'C H 0.8728 0.6230 0.3617 0.093 Uiso 1 1 calc R . . C10' C 0.6670(3) 0.5529(3) 0.2308(2) 0.0405(8) Uani 1 1 d . . . H10A H 0.6813 0.4805 0.2304 0.061 Uiso 1 1 calc R . . H10B H 0.6269 0.5740 0.1756 0.061 Uiso 1 1 calc R . . H10C H 0.6364 0.5645 0.2688 0.061 Uiso 1 1 calc R . . N1" N 0.91914(16) 0.55705(19) -0.12694(15) 0.0215(5) Uani 1 1 d . . . C2" C 0.85612(19) 0.4851(2) -0.16739(17) 0.0222(5) Uani 1 1 d . . . C3" C 0.8422(2) 0.4564(2) -0.24651(18) 0.0243(6) Uani 1 1 d . . . H3"A H 0.7981 0.4061 -0.2734 0.029 Uiso 1 1 calc R . . C4" C 0.8931(2) 0.5015(2) -0.28736(18) 0.0245(6) Uani 1 1 d . . . C5" C 0.9599(2) 0.5708(2) -0.24325(18) 0.0251(6) Uani 1 1 d . . . H5"A H 0.9980 0.6004 -0.2676 0.030 Uiso 1 1 calc R . . C6" C 0.9709(2) 0.5969(2) -0.16432(18) 0.0234(6) Uani 1 1 d . . . H6"A H 1.0167 0.6447 -0.1355 0.028 Uiso 1 1 calc R . . C7" C 0.8717(2) 0.4760(3) -0.37690(19) 0.0295(6) Uani 1 1 d . . . C8" C 0.9346(3) 0.5315(4) -0.4104(2) 0.0512(11) Uani 1 1 d . . . H8"A H 0.9285 0.6051 -0.4054 0.077 Uiso 1 1 calc R . . H8"B H 0.9179 0.5137 -0.4682 0.077 Uiso 1 1 calc R . . H8"C H 0.9976 0.5111 -0.3793 0.077 Uiso 1 1 calc R . . C9" C 0.8802(3) 0.3603(3) -0.3860(2) 0.0436(9) Uani 1 1 d . . . H9"A H 0.8400 0.3248 -0.3644 0.065 Uiso 1 1 calc R . . H9"B H 0.9431 0.3393 -0.3554 0.065 Uiso 1 1 calc R . . H9"C H 0.8630 0.3434 -0.4439 0.065 Uiso 1 1 calc R . . C10" C 0.7735(3) 0.5085(4) -0.4260(2) 0.0469(9) Uani 1 1 d . . . H10G H 0.7677 0.5821 -0.4205 0.070 Uiso 1 1 calc R . . H10H H 0.7327 0.4729 -0.4051 0.070 Uiso 1 1 calc R . . H10I H 0.7572 0.4914 -0.4838 0.070 Uiso 1 1 calc R . . Cl2 Cl 0.69148(5) 0.22662(6) -0.33422(5) 0.03245(17) Uani 1 1 d . . . O1W O 1.11004(19) 0.6900(3) -0.29238(18) 0.0505(7) Uani 1 1 d D . . H1WA H 1.1647(10) 0.692(3) -0.262(2) 0.045(12) Uiso 1 1 d D . . H1WB H 1.108(3) 0.711(4) -0.3378(15) 0.057(14) Uiso 1 1 d D . . C1S C 0.5619(3) 0.0515(4) 0.1129(3) 0.0666(13) Uani 1 1 d D . . H1SA H 0.5990 0.1142 0.1279 0.080 Uiso 1 1 calc R . . H1SB H 0.5727 0.0192 0.0668 0.080 Uiso 1 1 calc R . . Cl3 Cl 0.59729(10) -0.03083(11) 0.19556(11) 0.0866(5) Uani 1 1 d D . . Cl4 Cl 0.44848(10) 0.08376(13) 0.08124(10) 0.0818(4) Uani 1 1 d D . . C2S C 0.5300(5) 0.6113(8) -0.1042(6) 0.068(3) Uiso 0.50 1 d PD A 1 H2SA H 0.5025 0.5721 -0.1556 0.081 Uiso 0.50 1 calc PR A 1 H2SB H 0.4924 0.6729 -0.1093 0.081 Uiso 0.50 1 calc PR A 1 Cl5 Cl 0.63590(17) 0.6489(2) -0.09515(19) 0.0732(8) Uani 0.50 1 d PD A 1 Cl6 Cl 0.52471(17) 0.5383(2) -0.02489(16) 0.0622(6) Uani 0.50 1 d PD . 1 C3S C 0.5636(8) 0.6833(10) -0.0837(8) 0.073(6) Uiso 0.25 1 d PD B 2 Cl7 Cl 0.5703(3) 0.5772(3) -0.1374(3) 0.0514(10) Uani 0.25 1 d PD B 2 Cl8 Cl 0.6742(5) 0.7275(5) -0.0244(5) 0.064(2) Uani 0.15 1 d PD B 2 Cl8' Cl 0.6401(7) 0.7005(9) 0.0109(6) 0.056(2) Uiso 0.10 1 d PD B 3 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 0.02078(12) 0.02035(13) 0.01983(12) -0.00065(7) 0.00903(9) -0.00222(7) Cl1 0.0311(4) 0.0301(4) 0.0301(4) -0.0046(3) 0.0140(3) -0.0106(3) N1 0.0232(11) 0.0230(12) 0.0207(11) -0.0016(9) 0.0102(9) -0.0019(9) C2 0.0219(13) 0.0228(14) 0.0214(13) -0.0003(10) 0.0102(11) -0.0005(11) C3 0.0269(14) 0.0242(14) 0.0211(13) -0.0037(11) 0.0108(11) -0.0019(11) C4 0.0240(13) 0.0228(14) 0.0245(14) -0.0012(11) 0.0103(11) -0.0035(11) C5 0.0269(14) 0.0250(14) 0.0229(14) -0.0008(11) 0.0141(11) -0.0024(11) C6 0.0231(13) 0.0248(14) 0.0216(13) -0.0003(11) 0.0103(11) -0.0004(11) C7 0.0328(16) 0.0304(16) 0.0272(15) -0.0073(12) 0.0163(13) -0.0131(12) C8 0.0279(16) 0.049(2) 0.0399(19) -0.0037(16) 0.0077(14) -0.0101(15) C9 0.054(2) 0.0267(17) 0.046(2) -0.0033(15) 0.0207(17) -0.0084(15) C10 0.067(3) 0.066(3) 0.042(2) -0.0247(19) 0.038(2) -0.045(2) N1' 0.0260(12) 0.0227(12) 0.0221(12) -0.0015(9) 0.0112(10) -0.0026(9) C2' 0.0227(13) 0.0231(14) 0.0208(13) -0.0004(11) 0.0077(11) -0.0010(10) C3' 0.0277(14) 0.0249(14) 0.0239(14) -0.0017(11) 0.0117(11) -0.0035(11) C4' 0.0301(15) 0.0266(15) 0.0240(14) -0.0006(11) 0.0127(12) 0.0003(12) C5' 0.0357(16) 0.0273(16) 0.0264(15) -0.0081(12) 0.0132(13) -0.0054(12) C6' 0.0294(15) 0.0255(15) 0.0263(15) -0.0056(12) 0.0105(12) -0.0067(12) C7' 0.0368(17) 0.0357(17) 0.0295(16) -0.0072(13) 0.0202(14) -0.0021(14) C8' 0.073(3) 0.041(2) 0.090(4) -0.019(2) 0.059(3) -0.005(2) C9' 0.050(2) 0.109(4) 0.031(2) 0.004(2) 0.0198(18) 0.002(2) C10' 0.0412(19) 0.048(2) 0.041(2) -0.0047(16) 0.0263(16) -0.0018(16) N1" 0.0220(11) 0.0222(12) 0.0214(11) 0.0012(9) 0.0094(9) 0.0007(9) C2" 0.0235(13) 0.0209(13) 0.0236(13) 0.0008(11) 0.0104(11) -0.0004(10) C3" 0.0254(13) 0.0253(15) 0.0242(14) -0.0014(11) 0.0116(11) -0.0012(11) C4" 0.0263(14) 0.0263(15) 0.0235(14) 0.0003(11) 0.0123(11) 0.0028(11) C5" 0.0260(14) 0.0272(15) 0.0260(14) 0.0040(11) 0.0144(12) 0.0003(11) C6" 0.0244(14) 0.0216(14) 0.0259(14) 0.0027(11) 0.0116(11) -0.0007(10) C7" 0.0335(16) 0.0354(17) 0.0235(14) -0.0018(12) 0.0153(12) -0.0023(13) C8" 0.064(3) 0.068(3) 0.0322(18) -0.0096(18) 0.0302(18) -0.028(2) C9" 0.063(2) 0.038(2) 0.0344(18) -0.0063(15) 0.0243(17) 0.0049(17) C10" 0.045(2) 0.065(3) 0.0262(17) -0.0029(16) 0.0076(15) 0.0094(18) Cl2 0.0351(4) 0.0360(4) 0.0269(4) -0.0041(3) 0.0125(3) -0.0001(3) O1W 0.0365(14) 0.074(2) 0.0386(15) 0.0112(14) 0.0113(12) -0.0149(14) C1S 0.055(3) 0.068(3) 0.080(4) -0.023(3) 0.030(3) -0.020(2) Cl3 0.0684(8) 0.0586(8) 0.1154(13) -0.0150(8) 0.0154(8) -0.0178(6) Cl4 0.0615(8) 0.1000(12) 0.0840(10) -0.0108(8) 0.0280(7) -0.0129(7) Cl5 0.0553(13) 0.0748(17) 0.100(2) 0.0455(15) 0.0415(14) 0.0258(12) Cl6 0.0659(14) 0.0627(14) 0.0665(14) 0.0175(11) 0.0347(12) 0.0093(11) Cl7 0.054(2) 0.0301(18) 0.057(2) 0.0037(16) 0.0062(18) 0.0232(16) Cl8 0.055(4) 0.037(3) 0.071(5) 0.013(3) -0.009(4) -0.011(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 N1 1.929(2) . y Pd N1" 2.020(2) . y Pd N1' 2.030(2) . y Pd Cl1 2.2980(7) . y N1 C6 1.341(4) . ? N1 C2 1.344(4) . ? C2 C3 1.385(4) . ? C2 C2" 1.481(4) . ? C3 C4 1.403(4) . ? C4 C5 1.397(4) . ? C4 C7 1.527(4) . ? C5 C6 1.393(4) . ? C6 C2' 1.481(4) . ? C7 C10 1.522(4) . ? C7 C9 1.534(5) . ? C7 C8 1.537(5) . ? N1' C6' 1.338(4) . ? N1' C2' 1.367(4) . ? C2' C3' 1.377(4) . ? C3' C4' 1.398(4) . ? C4' C5' 1.393(4) . ? C4' C7' 1.533(4) . ? C5' C6' 1.382(4) . ? C7' C9' 1.520(6) . ? C7' C10' 1.535(5) . ? C7' C8' 1.537(5) . ? N1" C6" 1.344(4) . ? N1" C2" 1.366(4) . ? C2" C3" 1.382(4) . ? C3" C4" 1.406(4) . ? C4" C5" 1.393(4) . ? C4" C7" 1.524(4) . ? C5" C6" 1.381(4) . ? C7" C8" 1.529(5) . ? C7" C10" 1.532(5) . ? C7" C9" 1.540(5) . ? C1S Cl4 1.729(4) . ? C1S Cl3 1.730(5) . ? C2S Cl5 1.705(7) . ? C2S Cl6 1.727(7) . ? C3S Cl8' 1.668(8) . ? C3S Cl7 1.712(8) . ? C3S Cl8 1.771(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd N1" 81.01(10) . . y N1 Pd N1' 80.59(10) . . y N1" Pd N1' 161.53(10) . . y N1 Pd Cl1 178.02(8) . . y N1" Pd Cl1 98.26(7) . . y N1' Pd Cl1 100.07(7) . . y C6 N1 C2 122.7(2) . . ? C6 N1 Pd 118.82(19) . . ? C2 N1 Pd 118.43(19) . . ? N1 C2 C3 119.6(3) . . ? N1 C2 C2" 112.6(2) . . ? C3 C2 C2" 127.8(3) . . ? C2 C3 C4 119.7(3) . . ? C5 C4 C3 118.9(3) . . ? C5 C4 C7 122.3(3) . . ? C3 C4 C7 118.8(3) . . ? C6 C5 C4 119.2(3) . . ? N1 C6 C5 119.9(3) . . ? N1 C6 C2' 112.6(2) . . ? C5 C6 C2' 127.4(3) . . ? C10 C7 C4 112.4(3) . . ? C10 C7 C9 110.7(3) . . ? C4 C7 C9 108.1(3) . . ? C10 C7 C8 108.4(3) . . ? C4 C7 C8 108.7(3) . . ? C9 C7 C8 108.5(3) . . ? C6' N1' C2' 118.7(2) . . ? C6' N1' Pd 127.6(2) . . ? C2' N1' Pd 113.42(18) . . ? N1' C2' C3' 121.6(3) . . ? N1' C2' C6 114.3(2) . . ? C3' C2' C6 124.0(3) . . ? C2' C3' C4' 120.3(3) . . ? C5' C4' C3' 116.6(3) . . ? C5' C4' C7' 120.4(3) . . ? C3' C4' C7' 123.0(3) . . ? C6' C5' C4' 121.1(3) . . ? N1' C6' C5' 121.5(3) . . ? C9' C7' C4' 109.5(3) . . ? C9' C7' C10' 109.3(3) . . ? C4' C7' C10' 111.4(3) . . ? C9' C7' C8' 110.9(4) . . ? C4' C7' C8' 108.4(3) . . ? C10' C7' C8' 107.4(3) . . ? C6" N1" C2" 118.6(2) . . ? C6" N1" Pd 128.1(2) . . ? C2" N1" Pd 113.32(18) . . ? N1" C2" C3" 121.4(3) . . ? N1" C2" C2 114.5(2) . . ? C3" C2" C2 124.0(3) . . ? C2" C3" C4" 120.2(3) . . ? C5" C4" C3" 117.1(3) . . ? C5" C4" C7" 123.1(3) . . ? C3" C4" C7" 119.8(3) . . ? C6" C5" C4" 120.3(3) . . ? N1" C6" C5" 122.2(3) . . ? C4" C7" C8" 112.2(3) . . ? C4" C7" C10" 107.7(3) . . ? C8" C7" C10" 109.0(3) . . ? C4" C7" C9" 109.4(3) . . ? C8" C7" C9" 109.5(3) . . ? C10" C7" C9" 109.2(3) . . ? Cl4 C1S Cl3 113.0(3) . . ? Cl5 C2S Cl6 116.0(5) . . ? Cl8' C3S Cl7 119.4(9) . . ? Cl7 C3S Cl8 109.7(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA Cl2 0.832(10) 2.319(14) 3.137(3) 168(4) 2_754 O1W H1WB Cl1 0.836(10) 2.55(2) 3.320(3) 154(4) 4_575 _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.547 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.107 data_rir018 _database_code_CSD 186002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31.50 H39.50 Cl13.50 N3 O3 Pd S' _chemical_formula_weight 1125.20 _refine_special_details ; Asymmetric unit contains 4.5 molecules of CHCl3. Molecule C5a is half occupied and disordered across inversion centre. Molecule C4a has the Cl atoms modelled over 3 sites, 0.5:0.3:0.2. Largest residual electron density in this region but not sensible geometry for further disorder modelling. One TBu group of ligand shows disorder, modelled over 2 sites with occupancies 0.6:0.4. All partially occupied non-H atoms refined with Uiso only and geometry restraints applied. ; 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' 'Pd' 'Pd' -0.9988 1.0072 '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' _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 11.2719(10) _cell_length_b 20.494(2) _cell_length_c 20.230(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.222(2) _cell_angle_gamma 90.00 _cell_volume 4645.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4849 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.02 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.813 _exptl_absorpt_process_details 'Bruker SADABS (1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 42063 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 29.00 _reflns_number_total 11484 _reflns_number_gt 6661 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1999)' _computing_cell_refinement 'Bruker SAINT version 6.01 (Bruker, 1999)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.1130P)^2^+1.9637P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11178 _refine_ls_number_parameters 497 _refine_ls_number_restraints 284 _refine_ls_R_factor_all 0.1123 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.2084 _refine_ls_wR_factor_gt 0.1838 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.008 _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 0.70983(3) 0.054667(18) 0.55995(2) 0.03965(15) Uani 1 1 d U . . S1 S 0.70259(11) 0.16410(6) 0.55560(7) 0.0398(3) Uani 1 1 d U . . O1 O 0.7988(4) 0.1929(2) 0.6001(3) 0.0826(17) Uani 1 1 d U . . O2 O 0.7116(5) 0.18424(19) 0.4873(2) 0.0788(15) Uani 1 1 d U . . O3 O 0.5885(3) 0.18242(18) 0.5767(2) 0.0571(11) Uani 1 1 d U . . N1 N 0.7074(3) -0.04311(19) 0.5657(2) 0.0387(9) Uani 1 1 d U . . C2 C 0.6566(4) -0.0766(2) 0.5141(3) 0.0384(11) Uani 1 1 d U . . C3 C 0.6404(4) -0.1434(2) 0.5194(3) 0.0407(11) Uani 1 1 d U . . H3B H 0.6016 -0.1673 0.4830 0.049 Uiso 1 1 calc R . . C4 C 0.6820(4) -0.1756(2) 0.5790(3) 0.0407(11) Uani 1 1 d U A . C5 C 0.7350(5) -0.1381(3) 0.6311(3) 0.0438(12) Uani 1 1 d U . . H5A H 0.7627 -0.1582 0.6722 0.053 Uiso 1 1 calc R . . C6 C 0.7478(5) -0.0716(2) 0.6235(3) 0.0407(11) Uani 1 1 d U . . C7 C 0.6633(4) -0.2491(3) 0.5853(3) 0.0491(14) Uani 1 1 d DU . . C8 C 0.5316(7) -0.2628(5) 0.5898(5) 0.056(2) Uiso 0.60 1 d PDU A 1 H8A H 0.5102 -0.2481 0.6330 0.084 Uiso 0.60 1 calc PR A 1 H8B H 0.5165 -0.3097 0.5850 0.084 Uiso 0.60 1 calc PR A 1 H8C H 0.4833 -0.2393 0.5542 0.084 Uiso 0.60 1 calc PR A 1 C9 C 0.7077(10) -0.2831(6) 0.5254(5) 0.071(3) Uiso 0.60 1 d PDU A 1 H9A H 0.7952 -0.2842 0.5308 0.106 Uiso 0.60 1 calc PR A 1 H9B H 0.6798 -0.2592 0.4847 0.106 Uiso 0.60 1 calc PR A 1 H9C H 0.6768 -0.3278 0.5222 0.106 Uiso 0.60 1 calc PR A 1 C10 C 0.7362(8) -0.2762(5) 0.6489(4) 0.053(2) Uiso 0.60 1 d PDU A 1 H10G H 0.7532 -0.2408 0.6810 0.079 Uiso 0.60 1 calc PR A 1 H10H H 0.8114 -0.2947 0.6372 0.079 Uiso 0.60 1 calc PR A 1 H10I H 0.6900 -0.3102 0.6685 0.079 Uiso 0.60 1 calc PR A 1 C8A C 0.6144(14) -0.2811(9) 0.5179(6) 0.075(5) Uiso 0.40 1 d PDU A 2 H8AA H 0.6762 -0.2802 0.4874 0.112 Uiso 0.40 1 calc PR A 2 H8AB H 0.5443 -0.2569 0.4984 0.112 Uiso 0.40 1 calc PR A 2 H8AC H 0.5918 -0.3265 0.5256 0.112 Uiso 0.40 1 calc PR A 2 C9A C 0.7790(12) -0.2825(11) 0.6114(10) 0.109(8) Uiso 0.40 1 d PDU A 2 H9AA H 0.8123 -0.2614 0.6528 0.164 Uiso 0.40 1 calc PR A 2 H9AB H 0.8362 -0.2791 0.5784 0.164 Uiso 0.40 1 calc PR A 2 H9AC H 0.7635 -0.3286 0.6200 0.164 Uiso 0.40 1 calc PR A 2 C10A C 0.5643(13) -0.2583(11) 0.6312(8) 0.092(6) Uiso 0.40 1 d PDU A 2 H10J H 0.5892 -0.2383 0.6745 0.138 Uiso 0.40 1 calc PR A 2 H10K H 0.5498 -0.3049 0.6371 0.138 Uiso 0.40 1 calc PR A 2 H10L H 0.4909 -0.2373 0.6112 0.138 Uiso 0.40 1 calc PR A 2 N1' N 0.7934(4) 0.0400(2) 0.6549(2) 0.0487(11) Uani 1 1 d U . . C2' C 0.8036(5) -0.0246(3) 0.6732(3) 0.0445(12) Uani 1 1 d U . . C3' C 0.8632(5) -0.0427(3) 0.7330(3) 0.0526(14) Uani 1 1 d U . . H3'A H 0.8683 -0.0876 0.7446 0.063 Uiso 1 1 calc R . . C4' C 0.9162(6) 0.0034(3) 0.7772(3) 0.0590(15) Uani 1 1 d U . . C5' C 0.9033(7) 0.0676(4) 0.7580(3) 0.0694(18) Uani 1 1 d U . . H5'A H 0.9371 0.1010 0.7866 0.083 Uiso 1 1 calc R . . C6' C 0.8426(6) 0.0838(3) 0.6986(3) 0.0560(14) Uani 1 1 d U . . H6'A H 0.8348 0.1287 0.6874 0.067 Uiso 1 1 calc R . . C7' C 0.9834(7) -0.0181(4) 0.8441(3) 0.0741(19) Uani 1 1 d U . . C8' C 0.8904(8) -0.0402(5) 0.8895(4) 0.097(3) Uani 1 1 d U . . H8'A H 0.8438 -0.0765 0.8685 0.146 Uiso 1 1 calc R . . H8'B H 0.8371 -0.0038 0.8968 0.146 Uiso 1 1 calc R . . H8'C H 0.9311 -0.0546 0.9323 0.146 Uiso 1 1 calc R . . C9' C 1.0687(7) -0.0742(4) 0.8327(4) 0.082(2) Uani 1 1 d U . . H9'A H 1.0233 -0.1107 0.8115 0.124 Uiso 1 1 calc R . . H9'B H 1.1096 -0.0883 0.8755 0.124 Uiso 1 1 calc R . . H9'C H 1.1277 -0.0593 0.8039 0.124 Uiso 1 1 calc R . . C10' C 1.0583(9) 0.0388(4) 0.8786(4) 0.109(3) Uani 1 1 d U . . H10D H 1.1177 0.0534 0.8498 0.163 Uiso 1 1 calc R . . H10E H 1.0990 0.0235 0.9211 0.163 Uiso 1 1 calc R . . H10F H 1.0054 0.0752 0.8866 0.163 Uiso 1 1 calc R . . N1" N 0.6319(3) 0.0301(2) 0.4656(2) 0.0404(9) Uani 1 1 d U . . C2" C 0.6213(4) -0.0352(2) 0.4556(3) 0.0381(11) Uani 1 1 d U . . C3" C 0.5850(4) -0.0609(3) 0.3932(3) 0.0423(11) Uani 1 1 d U . . H3"A H 0.5767 -0.1068 0.3882 0.051 Uiso 1 1 calc R . . C4" C 0.5603(4) -0.0208(3) 0.3373(3) 0.0443(12) Uani 1 1 d U . . C5" C 0.5678(5) 0.0461(3) 0.3503(3) 0.0497(13) Uani 1 1 d U . . H5"A H 0.5487 0.0759 0.3148 0.060 Uiso 1 1 calc R . . C6" C 0.6015(4) 0.0696(2) 0.4121(3) 0.0436(12) Uani 1 1 d U . . H6"A H 0.6042 0.1155 0.4185 0.052 Uiso 1 1 calc R . . C7" C 0.5369(5) -0.0483(3) 0.2675(3) 0.0537(14) Uani 1 1 d U . . C8" C 0.6515(7) -0.0370(5) 0.2330(4) 0.088(2) Uani 1 1 d U . . H8"A H 0.7182 -0.0606 0.2573 0.132 Uiso 1 1 calc R . . H8"B H 0.6697 0.0097 0.2328 0.132 Uiso 1 1 calc R . . H8"C H 0.6389 -0.0530 0.1872 0.132 Uiso 1 1 calc R . . C9" C 0.4354(6) -0.0112(3) 0.2276(3) 0.0616(16) Uani 1 1 d U . . H9"A H 0.3615 -0.0175 0.2482 0.092 Uiso 1 1 calc R . . H9"B H 0.4248 -0.0278 0.1819 0.092 Uiso 1 1 calc R . . H9"C H 0.4550 0.0353 0.2272 0.092 Uiso 1 1 calc R . . C10" C 0.5072(8) -0.1198(3) 0.2674(4) 0.080(2) Uani 1 1 d U . . H10A H 0.5722 -0.1438 0.2928 0.120 Uiso 1 1 calc R . . H10B H 0.4971 -0.1360 0.2215 0.120 Uiso 1 1 calc R . . H10C H 0.4330 -0.1264 0.2877 0.120 Uiso 1 1 calc R . . C1A C 0.5873(5) 0.2041(3) 0.1738(3) 0.0721(18) Uani 1 1 d DU . . H1AA H 0.6032 0.2449 0.1491 0.087 Uiso 1 1 calc R . . Cl1 Cl 0.6236(4) 0.13711(16) 0.1286(2) 0.1964(19) Uani 1 1 d DU . . Cl2 Cl 0.6723(3) 0.2040(2) 0.24922(14) 0.1711(17) Uani 1 1 d DU . . Cl3 Cl 0.4379(2) 0.20057(12) 0.18544(15) 0.1121(9) Uani 1 1 d DU . . C2A C 1.0821(5) -0.1078(3) 0.5766(3) 0.0567(15) Uani 1 1 d U . . H2AA H 1.1583 -0.1215 0.5596 0.068 Uiso 1 1 calc R . . Cl4 Cl 0.96197(15) -0.12960(10) 0.51821(10) 0.0757(5) Uani 1 1 d U . . Cl5 Cl 1.08290(18) -0.02282(10) 0.58731(13) 0.0920(7) Uani 1 1 d U . . Cl6 Cl 1.0697(2) -0.14690(13) 0.65160(11) 0.1071(8) Uani 1 1 d U . . C3A C 1.0514(5) 0.2182(4) 0.6504(3) 0.0677(17) Uani 1 1 d U . . H3AA H 0.9792 0.2143 0.6173 0.081 Uiso 1 1 calc R . . Cl7 Cl 1.1252(2) 0.14333(14) 0.65621(13) 0.1152(9) Uani 1 1 d U . . Cl8 Cl 1.1460(2) 0.27788(17) 0.62326(17) 0.1391(11) Uani 1 1 d U . . Cl9 Cl 1.0069(2) 0.24070(12) 0.72700(10) 0.0978(7) Uani 1 1 d U . . C4A C 0.7970(4) 0.1813(3) 0.9515(2) 0.0672(18) Uiso 1 1 d DU . . H4A H 0.7549 0.2183 0.9712 0.081 Uiso 1 1 calc R B 1 Cl10 Cl 0.7699(4) 0.1851(2) 0.86620(18) 0.0743(11) Uiso 0.50 1 d PDU C 1 Cl11 Cl 0.9502(4) 0.1867(2) 0.9778(3) 0.0894(13) Uiso 0.50 1 d PDU C 1 Cl12 Cl 0.7439(5) 0.1078(2) 0.9803(3) 0.1030(16) Uiso 0.50 1 d PDU C 1 Cl1A Cl 0.7087(6) 0.1102(3) 0.9546(4) 0.081(2) Uiso 0.30 1 d PDU C 2 Cl2A Cl 0.8159(9) 0.1990(5) 0.8697(3) 0.110(3) Uiso 0.30 1 d PDU C 2 Cl3A Cl 0.9294(5) 0.1724(3) 1.0016(3) 0.0628(15) Uiso 0.30 1 d PDU C 2 Cl1B Cl 0.7067(10) 0.1358(6) 0.8936(6) 0.115(4) Uiso 0.20 1 d PDU C 3 Cl2B Cl 0.9227(11) 0.2033(9) 0.9115(8) 0.168(7) Uiso 0.20 1 d PDU C 3 Cl3B Cl 0.8451(18) 0.1339(9) 1.0196(7) 0.205(9) Uiso 0.20 1 d PDU C 3 C5A C 0.4866(16) 0.4498(8) 0.5132(8) 0.083(4) Uani 0.50 1 d PU D -1 H5AA H 0.5301 0.4072 0.5146 0.100 Uiso 0.50 1 calc PR D -1 Cl13 Cl 0.4308(8) 0.4662(4) 0.4318(3) 0.126(2) Uani 0.50 1 d PU D -1 Cl14 Cl 0.3682(7) 0.4429(3) 0.5587(3) 0.132(2) Uani 0.50 1 d PU D -1 Cl15 Cl 0.5870(10) 0.5110(4) 0.5386(5) 0.167(4) Uani 0.50 1 d PU D -1 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 0.0351(2) 0.0289(2) 0.0561(3) 0.00745(18) 0.01030(16) 0.00343(16) S1 0.0330(6) 0.0302(6) 0.0561(8) 0.0049(5) 0.0052(5) 0.0019(5) O1 0.052(3) 0.041(2) 0.143(4) 0.021(3) -0.041(3) -0.0092(19) O2 0.148(5) 0.031(2) 0.064(3) 0.0044(19) 0.040(3) -0.011(3) O3 0.042(2) 0.034(2) 0.098(3) -0.009(2) 0.022(2) -0.0012(16) N1 0.033(2) 0.031(2) 0.054(2) 0.0103(17) 0.0132(18) 0.0065(16) C2 0.027(2) 0.035(2) 0.054(3) 0.012(2) 0.009(2) 0.0042(19) C3 0.032(2) 0.033(2) 0.058(3) 0.010(2) 0.012(2) 0.0017(19) C4 0.036(3) 0.030(2) 0.059(3) 0.014(2) 0.013(2) 0.007(2) C5 0.043(3) 0.039(3) 0.052(3) 0.012(2) 0.014(2) 0.011(2) C6 0.041(3) 0.035(2) 0.048(3) 0.009(2) 0.014(2) 0.009(2) C7 0.049(3) 0.030(3) 0.068(4) 0.018(2) 0.008(3) 0.003(2) N1' 0.051(3) 0.041(2) 0.055(3) 0.0022(19) 0.012(2) 0.005(2) C2' 0.040(3) 0.040(3) 0.054(3) 0.002(2) 0.012(2) 0.010(2) C3' 0.061(4) 0.048(3) 0.051(3) 0.002(2) 0.017(2) 0.020(3) C4' 0.065(4) 0.062(4) 0.051(3) -0.008(3) 0.007(3) 0.021(3) C5' 0.087(5) 0.066(4) 0.055(4) -0.011(3) 0.006(3) 0.012(4) C6' 0.063(4) 0.044(3) 0.061(3) -0.004(3) 0.007(3) 0.007(3) C7' 0.091(5) 0.080(5) 0.051(4) -0.008(3) 0.004(3) 0.036(4) C8' 0.117(6) 0.120(7) 0.058(4) 0.013(4) 0.022(4) 0.056(5) C9' 0.078(5) 0.102(6) 0.066(4) -0.005(4) 0.002(4) 0.041(4) C10' 0.130(7) 0.105(6) 0.081(6) -0.024(5) -0.036(5) 0.031(5) N1" 0.029(2) 0.033(2) 0.060(3) 0.0111(18) 0.0057(18) -0.0009(16) C2" 0.024(2) 0.032(2) 0.059(3) 0.013(2) 0.007(2) 0.0000(18) C3" 0.035(3) 0.038(3) 0.055(3) 0.013(2) 0.008(2) 0.002(2) C4" 0.033(3) 0.045(3) 0.056(3) 0.014(2) 0.011(2) 0.004(2) C5" 0.040(3) 0.045(3) 0.065(3) 0.020(2) 0.007(2) 0.002(2) C6" 0.035(3) 0.030(3) 0.066(3) 0.017(2) 0.008(2) 0.002(2) C7" 0.050(3) 0.055(3) 0.057(3) 0.013(3) 0.010(3) 0.008(3) C8" 0.067(4) 0.122(7) 0.081(5) 0.021(5) 0.034(4) 0.034(4) C9" 0.058(4) 0.071(4) 0.056(4) 0.006(3) 0.007(3) 0.015(3) C10" 0.122(7) 0.062(4) 0.054(4) 0.006(3) -0.002(4) 0.005(4) C1A 0.080(4) 0.068(4) 0.069(4) 0.007(3) 0.013(3) 0.024(4) Cl1 0.275(5) 0.095(2) 0.240(4) -0.005(2) 0.124(4) 0.079(3) Cl2 0.1003(19) 0.306(5) 0.0987(18) 0.088(2) -0.0292(15) -0.040(2) Cl3 0.0743(13) 0.0972(17) 0.164(2) -0.0323(16) 0.0109(14) 0.0028(12) C2A 0.044(3) 0.064(4) 0.064(4) 0.006(3) 0.014(3) 0.015(3) Cl4 0.0550(10) 0.0936(13) 0.0791(12) -0.0121(10) 0.0095(8) 0.0082(9) Cl5 0.0715(12) 0.0664(12) 0.143(2) -0.0079(12) 0.0315(12) -0.0025(9) Cl6 0.1114(17) 0.135(2) 0.0765(13) 0.0405(13) 0.0193(12) 0.0600(15) C3A 0.041(3) 0.093(5) 0.066(4) -0.008(4) -0.009(3) -0.002(3) Cl7 0.0911(16) 0.133(2) 0.1172(19) -0.0051(16) -0.0087(14) 0.0504(15) Cl8 0.0789(16) 0.178(3) 0.163(3) 0.038(2) 0.0244(16) -0.0304(17) Cl9 0.1230(18) 0.0979(16) 0.0717(12) -0.0241(11) 0.0069(12) -0.0191(13) C5A 0.107(11) 0.068(9) 0.071(8) -0.006(7) -0.007(7) 0.020(7) Cl13 0.185(7) 0.112(5) 0.074(3) 0.029(3) -0.019(4) -0.024(5) Cl14 0.195(6) 0.114(4) 0.095(3) -0.016(3) 0.055(4) 0.002(4) Cl15 0.204(8) 0.115(5) 0.178(9) -0.071(6) 0.002(7) -0.028(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N1 2.008(4) . y Pd N1' 2.069(5) . y Pd N1" 2.075(5) . y Pd S1 2.2457(13) . y S1 O3 1.448(4) . y S1 O2 1.456(5) . y S1 O1 1.457(4) . y N1 C2 1.327(7) . ? N1 C6 1.343(6) . ? C2 C3 1.385(7) . ? C2 C2" 1.476(7) . ? C3 C4 1.411(7) . ? C4 C5 1.387(8) . ? C4 C7 1.529(7) . ? C5 C6 1.379(7) . ? C6 C2' 1.482(8) . ? C7 C9A 1.517(9) . ? C7 C8 1.524(7) . ? C7 C9 1.528(8) . ? C7 C10A 1.539(9) . ? C7 C10 1.552(7) . ? C7 C8A 1.558(8) . ? N1' C6' 1.336(8) . ? N1' C2' 1.376(7) . ? C2' C3' 1.370(8) . ? C3' C4' 1.391(9) . ? C4' C5' 1.375(9) . ? C4' C7' 1.541(9) . ? C5' C6' 1.358(9) . ? C7' C9' 1.531(9) . ? C7' C8' 1.535(11) . ? C7' C10' 1.560(12) . ? N1" C2" 1.357(7) . ? N1" C6" 1.366(6) . ? C2" C3" 1.388(8) . ? C3" C4" 1.400(7) . ? C4" C5" 1.397(8) . ? C4" C7" 1.518(8) . ? C5" C6" 1.356(8) . ? C7" C10" 1.503(9) . ? C7" C9" 1.528(8) . ? C7" C8" 1.550(9) . ? C1A Cl2 1.711(5) . ? C1A Cl1 1.724(5) . ? C1A Cl3 1.727(5) . ? C2A Cl6 1.734(6) . ? C2A Cl4 1.755(7) . ? C2A Cl5 1.755(7) . ? C3A Cl9 1.741(7) . ? C3A Cl7 1.743(8) . ? C3A Cl8 1.750(8) . ? C4A Cl3A 1.720(6) . ? C4A Cl10 1.721(5) . ? C4A Cl3B 1.724(7) . ? C4A Cl2A 1.729(6) . ? C4A Cl1B 1.738(7) . ? C4A Cl12 1.745(6) . ? C4A Cl11 1.755(5) . ? C4A Cl2B 1.765(7) . ? C4A Cl1A 1.770(6) . ? C5A Cl14 1.707(19) . ? C5A Cl15 1.730(18) . ? C5A Cl13 1.732(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 N1 Pd N1' 78.97(18) . . y N1 Pd N1" 78.69(17) . . y N1' Pd N1" 157.53(18) . . y N1 Pd S1 176.84(11) . . y N1' Pd S1 101.10(13) . . y N1" Pd S1 101.34(12) . . y O3 S1 O2 111.2(3) . . y O3 S1 O1 109.8(3) . . y O2 S1 O1 110.4(3) . . y O3 S1 Pd 106.08(16) . . y O2 S1 Pd 108.32(18) . . y O1 S1 Pd 111.04(17) . . y C2 N1 C6 122.5(4) . . ? C2 N1 Pd 118.6(3) . . ? C6 N1 Pd 118.7(4) . . ? N1 C2 C3 120.0(5) . . ? N1 C2 C2" 112.9(4) . . ? C3 C2 C2" 127.1(5) . . ? C2 C3 C4 119.6(5) . . ? C5 C4 C3 117.8(5) . . ? C5 C4 C7 122.4(4) . . ? C3 C4 C7 119.7(5) . . ? C6 C5 C4 120.3(5) . . ? N1 C6 C5 119.8(5) . . ? N1 C6 C2' 112.8(4) . . ? C5 C6 C2' 127.5(5) . . ? C8 C7 C9 111.7(6) . . ? C9A C7 C4 110.7(10) . . ? C8 C7 C4 109.2(5) . . ? C9 C7 C4 108.9(6) . . ? C9A C7 C10A 112.8(9) . . ? C4 C7 C10A 106.5(9) . . ? C8 C7 C10 108.4(5) . . ? C9 C7 C10 107.7(6) . . ? C4 C7 C10 110.8(5) . . ? C9A C7 C8A 109.0(9) . . ? C4 C7 C8A 112.5(8) . . ? C10A C7 C8A 105.4(8) . . ? C6' N1' C2' 116.9(5) . . ? C6' N1' Pd 129.1(4) . . ? C2' N1' Pd 113.9(4) . . ? C3' C2' N1' 121.0(5) . . ? C3' C2' C6 123.7(5) . . ? N1' C2' C6 115.3(5) . . ? C2' C3' C4' 121.3(6) . . ? C5' C4' C3' 116.3(6) . . ? C5' C4' C7' 123.3(6) . . ? C3' C4' C7' 120.4(6) . . ? C6' C5' C4' 120.7(6) . . ? N1' C6' C5' 123.7(6) . . ? C9' C7' C8' 110.4(7) . . ? C9' C7' C4' 109.9(5) . . ? C8' C7' C4' 107.9(6) . . ? C9' C7' C10' 108.0(7) . . ? C8' C7' C10' 108.9(7) . . ? C4' C7' C10' 111.7(7) . . ? C2" N1" C6" 117.1(5) . . ? C2" N1" Pd 113.5(3) . . ? C6" N1" Pd 129.0(4) . . ? N1" C2" C3" 121.5(5) . . ? N1" C2" C2 115.8(5) . . ? C3" C2" C2 122.6(5) . . ? C2" C3" C4" 121.6(5) . . ? C5" C4" C3" 115.0(5) . . ? C5" C4" C7" 122.7(5) . . ? C3" C4" C7" 122.1(5) . . ? C6" C5" C4" 121.8(5) . . ? C5" C6" N1" 122.8(5) . . ? C10" C7" C4" 112.3(5) . . ? C10" C7" C9" 109.3(6) . . ? C4" C7" C9" 110.5(5) . . ? C10" C7" C8" 109.9(6) . . ? C4" C7" C8" 107.1(5) . . ? C9" C7" C8" 107.5(5) . . ? Cl2 C1A Cl1 109.3(4) . . ? Cl2 C1A Cl3 109.8(3) . . ? Cl1 C1A Cl3 109.2(4) . . ? Cl6 C2A Cl4 110.0(4) . . ? Cl6 C2A Cl5 110.5(4) . . ? Cl4 C2A Cl5 109.2(3) . . ? Cl9 C3A Cl7 110.8(4) . . ? Cl9 C3A Cl8 109.8(4) . . ? Cl7 C3A Cl8 109.5(4) . . ? Cl3A C4A Cl2A 113.4(5) . . ? Cl3B C4A Cl1B 110.3(7) . . ? Cl10 C4A Cl12 110.1(4) . . ? Cl10 C4A Cl11 111.3(4) . . ? Cl12 C4A Cl11 108.4(4) . . ? Cl3B C4A Cl2B 108.2(7) . . ? Cl1B C4A Cl2B 105.6(7) . . ? Cl3A C4A Cl1A 110.2(4) . . ? Cl2A C4A Cl1A 109.6(5) . . ? Cl14 C5A Cl15 115.1(9) . . ? Cl14 C5A Cl13 107.7(10) . . ? Cl15 C5A Cl13 107.4(11) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.553 _refine_diff_density_min -1.050 _refine_diff_density_rms 0.108 data_trpdso _database_code_CSD 186003 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cl2 N2 Pd' _chemical_formula_weight 445.69 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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 7.3555(9) _cell_length_b 19.140(2) _cell_length_c 12.969(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.666(2) _cell_angle_gamma 90.00 _cell_volume 1813.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5806 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 28.42 _exptl_crystal_description column _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 1.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.446 _exptl_absorpt_correction_T_max 0.908 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11373 _diffrn_reflns_av_R_equivalents 0.043 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.82 _reflns_number_total 4193 _reflns_number_gt 3524 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.0814P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4193 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 0.73985(3) -0.080780(12) 0.627577(17) 0.01944(11) Uani 1 1 d . . . Cl1 Cl 0.69363(14) -0.07698(4) 0.79802(6) 0.0311(2) Uani 1 1 d . . . Cl2 Cl 0.78604(13) -0.19858(5) 0.64065(6) 0.0325(2) Uani 1 1 d . . . N1 N 0.7168(3) 0.02308(14) 0.6045(2) 0.0203(5) Uani 1 1 d . . . C2 C 0.7383(4) 0.04589(15) 0.5081(2) 0.0191(6) Uani 1 1 d . . . C3 C 0.7393(4) 0.11686(16) 0.4852(2) 0.0217(6) Uani 1 1 d . . . H3A H 0.7552 0.1316 0.4169 0.026 Uiso 1 1 calc R . . C4 C 0.7173(4) 0.16650(17) 0.5609(2) 0.0230(7) Uani 1 1 d . . . C5 C 0.6913(5) 0.14090(17) 0.6586(3) 0.0263(7) Uani 1 1 d . . . H5A H 0.6721 0.1727 0.7126 0.032 Uiso 1 1 calc R . . C6 C 0.6931(5) 0.07068(18) 0.6779(3) 0.0258(7) Uani 1 1 d . . . H6A H 0.6769 0.0549 0.7457 0.031 Uiso 1 1 calc R . . C7 C 0.7220(5) 0.24506(17) 0.5432(2) 0.0249(7) Uani 1 1 d . . . C8 C 0.7255(5) 0.26291(18) 0.4279(3) 0.0304(8) Uani 1 1 d . . . H8A H 0.8334 0.2415 0.4031 0.046 Uiso 1 1 calc R . . H8B H 0.7310 0.3137 0.4196 0.046 Uiso 1 1 calc R . . H8C H 0.6145 0.2449 0.3876 0.046 Uiso 1 1 calc R . . C9 C 0.5532(5) 0.27927(18) 0.5803(3) 0.0328(8) Uani 1 1 d . . . H9A H 0.4424 0.2600 0.5414 0.049 Uiso 1 1 calc R . . H9B H 0.5575 0.3298 0.5689 0.049 Uiso 1 1 calc R . . H9C H 0.5516 0.2699 0.6545 0.049 Uiso 1 1 calc R . . C10 C 0.8956(5) 0.27497(18) 0.6043(3) 0.0381(9) Uani 1 1 d . . . H10A H 1.0036 0.2532 0.5801 0.057 Uiso 1 1 calc R . . H10B H 0.8943 0.2652 0.6784 0.057 Uiso 1 1 calc R . . H10C H 0.8999 0.3256 0.5934 0.057 Uiso 1 1 calc R . . N1' N 0.7688(4) -0.07528(12) 0.4747(2) 0.0189(5) Uani 1 1 d . . . C2' C 0.7606(4) -0.01004(16) 0.4332(2) 0.0193(6) Uani 1 1 d . . . C3' C 0.7697(4) 0.00022(16) 0.3285(2) 0.0204(6) Uani 1 1 d . . . H3'A H 0.7662 0.0464 0.3016 0.024 Uiso 1 1 calc R . . C4' C 0.7840(4) -0.05583(17) 0.2618(2) 0.0200(6) Uani 1 1 d . . . C5' C 0.7909(5) -0.12241(17) 0.3072(3) 0.0244(7) Uani 1 1 d . . . H5'A H 0.8014 -0.1626 0.2654 0.029 Uiso 1 1 calc R . . C6' C 0.7826(5) -0.12963(17) 0.4115(3) 0.0244(7) Uani 1 1 d . . . H6'A H 0.7868 -0.1753 0.4402 0.029 Uiso 1 1 calc R . . C7' C 0.7810(4) -0.04853(17) 0.1454(2) 0.0215(6) Uani 1 1 d . . . C8' C 0.9363(5) -0.0903(2) 0.1064(3) 0.0349(9) Uani 1 1 d . . . H8'A H 1.0542 -0.0722 0.1384 0.052 Uiso 1 1 calc R . . H8'B H 0.9296 -0.0859 0.0307 0.052 Uiso 1 1 calc R . . H8'C H 0.9248 -0.1396 0.1250 0.052 Uiso 1 1 calc R . . C9' C 0.7959(5) 0.02769(18) 0.1126(2) 0.0297(7) Uani 1 1 d . . . H9'A H 0.9116 0.0473 0.1451 0.044 Uiso 1 1 calc R . . H9'B H 0.6934 0.0543 0.1347 0.044 Uiso 1 1 calc R . . H9'C H 0.7922 0.0303 0.0369 0.044 Uiso 1 1 calc R . . C10' C 0.5983(5) -0.07772(18) 0.0939(3) 0.0315(8) Uani 1 1 d . . . H10D H 0.4971 -0.0514 0.1180 0.047 Uiso 1 1 calc R . . H10E H 0.5880 -0.1271 0.1125 0.047 Uiso 1 1 calc R . . H10F H 0.5933 -0.0733 0.0183 0.047 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 0.02583(16) 0.02307(16) 0.00978(15) 0.00263(8) 0.00356(10) 0.00123(9) Cl1 0.0488(5) 0.0342(5) 0.0120(4) 0.0043(3) 0.0114(4) 0.0010(4) Cl2 0.0538(5) 0.0252(4) 0.0187(4) 0.0057(3) 0.0044(4) 0.0061(4) N1 0.0256(13) 0.0252(14) 0.0107(12) 0.0003(10) 0.0040(10) 0.0011(11) C2 0.0222(15) 0.0233(16) 0.0121(14) -0.0002(11) 0.0028(11) -0.0001(11) C3 0.0293(16) 0.0233(16) 0.0128(14) 0.0014(12) 0.0041(12) -0.0004(12) C4 0.0254(16) 0.0273(17) 0.0157(15) 0.0012(12) 0.0004(12) 0.0015(13) C5 0.0382(19) 0.0256(17) 0.0154(15) -0.0053(12) 0.0048(14) 0.0029(14) C6 0.0345(19) 0.0331(19) 0.0111(15) -0.0022(12) 0.0077(13) 0.0007(13) C7 0.0340(17) 0.0235(16) 0.0174(15) -0.0006(12) 0.0041(12) 0.0032(13) C8 0.045(2) 0.0236(17) 0.0246(17) 0.0025(14) 0.0124(15) 0.0042(15) C9 0.048(2) 0.0277(18) 0.0233(17) 0.0021(13) 0.0070(15) 0.0097(15) C10 0.044(2) 0.0247(19) 0.043(2) -0.0046(16) -0.0058(17) 0.0014(15) N1' 0.0242(13) 0.0202(13) 0.0122(13) 0.0024(9) 0.0018(10) 0.0012(10) C2' 0.0211(15) 0.0229(15) 0.0140(14) 0.0020(11) 0.0027(11) 0.0001(12) C3' 0.0266(16) 0.0239(16) 0.0111(14) 0.0015(12) 0.0040(11) 0.0012(12) C4' 0.0234(16) 0.0241(15) 0.0131(14) -0.0004(12) 0.0049(11) 0.0000(12) C5' 0.0341(18) 0.0222(16) 0.0176(15) -0.0010(12) 0.0055(13) 0.0043(13) C6' 0.0334(18) 0.0252(16) 0.0150(15) -0.0004(12) 0.0045(12) 0.0025(13) C7' 0.0293(17) 0.0242(17) 0.0124(14) 0.0013(11) 0.0083(12) 0.0002(12) C8' 0.042(2) 0.044(2) 0.0214(18) 0.0012(15) 0.0144(16) 0.0107(16) C9' 0.045(2) 0.0315(18) 0.0128(15) 0.0052(13) 0.0065(14) -0.0057(15) C10' 0.042(2) 0.039(2) 0.0137(16) -0.0002(13) 0.0047(14) -0.0104(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.015(3) . y Pd1 N1' 2.022(3) . y Pd1 Cl1 2.2763(9) . y Pd1 Cl2 2.2834(9) . y N1 C6 1.344(4) . ? N1 C2 1.350(4) . ? C2 C3 1.390(4) . ? C2 C2' 1.467(4) . ? C3 C4 1.388(4) . ? C4 C5 1.392(4) . ? C4 C7 1.522(4) . ? C5 C6 1.367(5) . ? C7 C9 1.530(5) . ? C7 C10 1.534(5) . ? C7 C8 1.536(4) . ? N1' C6' 1.335(4) . ? N1' C2' 1.358(4) . ? C2' C3' 1.382(4) . ? C3' C4' 1.390(4) . ? C4' C5' 1.402(5) . ? C4' C7' 1.514(4) . ? C5' C6' 1.368(5) . ? C7' C9' 1.527(4) . ? C7' C8' 1.528(4) . ? C7' C10' 1.534(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N1' 79.59(10) . . y N1 Pd1 Cl1 95.36(8) . . y N1' Pd1 Cl1 174.56(7) . . y N1 Pd1 Cl2 174.02(7) . . y N1' Pd1 Cl2 95.31(7) . . y Cl1 Pd1 Cl2 89.84(3) . . y C6 N1 C2 118.4(3) . . ? C6 N1 Pd1 125.4(2) . . ? C2 N1 Pd1 116.1(2) . . ? N1 C2 C3 121.1(3) . . ? N1 C2 C2' 114.3(3) . . ? C3 C2 C2' 124.6(3) . . ? C4 C3 C2 120.9(3) . . ? C3 C4 C5 116.2(3) . . ? C3 C4 C7 124.2(3) . . ? C5 C4 C7 119.5(3) . . ? C6 C5 C4 120.9(3) . . ? N1 C6 C5 122.4(3) . . ? C4 C7 C9 110.0(3) . . ? C4 C7 C10 108.8(3) . . ? C9 C7 C10 109.6(3) . . ? C4 C7 C8 111.7(3) . . ? C9 C7 C8 108.5(3) . . ? C10 C7 C8 108.2(3) . . ? C6' N1' C2' 118.5(3) . . ? C6' N1' Pd1 125.8(2) . . ? C2' N1' Pd1 115.5(2) . . ? N1' C2' C3' 121.0(3) . . ? N1' C2' C2 114.3(3) . . ? C3' C2' C2 124.7(3) . . ? C2' C3' C4' 121.2(3) . . ? C3' C4' C5' 116.2(3) . . ? C3' C4' C7' 123.8(3) . . ? C5' C4' C7' 119.9(3) . . ? C6' C5' C4' 120.2(3) . . ? N1' C6' C5' 122.9(3) . . ? C4' C7' C9' 111.9(3) . . ? C4' C7' C8' 110.9(3) . . ? C9' C7' C8' 109.1(3) . . ? C4' C7' C10' 108.1(3) . . ? C9' C7' C10' 108.3(3) . . ? C8' C7' C10' 108.4(3) . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.154 _refine_diff_density_min -2.037 _refine_diff_density_rms 0.156 data_trpypd _database_code_CSD 186004 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H39 Cl4 N3 O4 Pd S' _chemical_formula_weight 773.89 _refine_special_details ; Disorder in one tBu group modelled over 2 sites with occupancies 0.55:0.45, in DCM, Cl atoms modelled over 2 sites with occupancies 0.60:0.40. Hydrogen atoms on the C omitted. Geometry restraints applied in both cases and partially occupied sites refined with isotropic adps. Residual electron density 1.665eA-3 near to S atom but no obvious disorder model. ; 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.1352(5) _cell_length_b 13.5105(6) _cell_length_c 24.505(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3355.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7502 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 26.92 _exptl_crystal_description wedge _exptl_crystal_colour Orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.878 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker (2001) SADABS v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 21680 _diffrn_reflns_av_R_equivalents 0.037 _diffrn_reflns_av_sigmaI/netI 0.0441 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 29.02 _reflns_number_total 7743 _reflns_number_gt 6856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SAINT version 6.01 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0723P)^2^+7.1250P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 7743 _refine_ls_number_parameters 364 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0643 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1386 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.074 _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 0.19897(4) 0.70321(3) 0.215269(15) 0.02233(10) Uani 1 1 d . . . S2 S 0.25463(15) 0.52871(11) 0.13534(6) 0.0336(3) Uani 1 1 d . . . O1 O 0.1556(4) 0.6044(3) 0.15717(16) 0.0334(9) Uani 1 1 d . . . O2 O 0.3589(5) 0.5173(4) 0.17552(18) 0.0409(11) Uani 1 1 d . . . O3 O 0.3049(6) 0.5716(3) 0.08411(18) 0.0465(11) Uani 1 1 d . . . O4 O 0.1847(6) 0.4391(3) 0.1251(2) 0.0522(12) Uani 1 1 d . . . N1 N 0.2198(4) 0.7949(3) 0.27442(15) 0.0229(8) Uani 1 1 d . . . C2 C 0.1230(5) 0.8010(4) 0.3120(2) 0.0241(10) Uani 1 1 d . . . C3 C 0.1356(6) 0.8648(4) 0.3553(2) 0.0283(11) Uani 1 1 d . . . H3A H 0.0651 0.8714 0.3805 0.034 Uiso 1 1 calc R . . C4 C 0.2495(5) 0.9197(4) 0.3627(2) 0.0240(10) Uani 1 1 d . . . C5 C 0.3495(5) 0.9110(4) 0.3224(2) 0.0254(11) Uani 1 1 d . . . H5A H 0.4290 0.9477 0.3260 0.031 Uiso 1 1 calc R . . C6 C 0.3314(5) 0.8493(4) 0.2781(2) 0.0218(10) Uani 1 1 d . . . C7 C 0.2685(6) 0.9874(4) 0.4112(2) 0.0303(12) Uani 1 1 d . . . C8 C 0.3895(9) 0.9505(8) 0.4432(3) 0.066(2) Uani 1 1 d . . . H8A H 0.3733 0.8829 0.4561 0.099 Uiso 1 1 calc R . . H8B H 0.4052 0.9940 0.4745 0.099 Uiso 1 1 calc R . . H8C H 0.4670 0.9509 0.4193 0.099 Uiso 1 1 calc R . . C9 C 0.2934(12) 1.0911(5) 0.3915(3) 0.073(3) Uani 1 1 d . . . H9A H 0.2158 1.1151 0.3716 0.109 Uiso 1 1 calc R . . H9B H 0.3701 1.0915 0.3671 0.109 Uiso 1 1 calc R . . H9C H 0.3105 1.1343 0.4228 0.109 Uiso 1 1 calc R . . C10 C 0.1517(8) 0.9875(7) 0.4492(3) 0.056(2) Uani 1 1 d . . . H10J H 0.0735 1.0111 0.4297 0.084 Uiso 1 1 calc R . . H10K H 0.1697 1.0314 0.4802 0.084 Uiso 1 1 calc R . . H10L H 0.1360 0.9202 0.4626 0.084 Uiso 1 1 calc R . . N1' N 0.3723(4) 0.7668(3) 0.19348(18) 0.0263(10) Uani 1 1 d . . . C2' C 0.4206(5) 0.8326(4) 0.2315(2) 0.0245(11) Uani 1 1 d . . . C3' C 0.5408(5) 0.8793(4) 0.2255(2) 0.0258(11) Uani 1 1 d . . . H3'A H 0.5734 0.9214 0.2534 0.031 Uiso 1 1 calc R . . C4' C 0.6150(5) 0.8639(4) 0.1774(2) 0.0292(12) Uani 1 1 d . . . C5' C 0.5625(5) 0.8015(5) 0.1389(2) 0.0329(11) Uani 1 1 d . . . H5'A H 0.6082 0.7913 0.1055 0.039 Uiso 1 1 calc R . . C6' C 0.4435(6) 0.7530(4) 0.1479(2) 0.0303(12) Uani 1 1 d . . . H6'A H 0.4115 0.7087 0.1209 0.036 Uiso 1 1 calc R . . C7' C 0.7496(6) 0.9119(5) 0.1716(3) 0.0354(13) Uani 1 1 d . . . C8' C 0.8140(8) 0.8867(7) 0.1181(3) 0.062(2) Uani 1 1 d . . . H8'A H 0.8224 0.8147 0.1149 0.093 Uiso 1 1 calc R . . H8'B H 0.9017 0.9171 0.1166 0.093 Uiso 1 1 calc R . . H8'C H 0.7597 0.9119 0.0881 0.093 Uiso 1 1 calc R . . C9' C 0.7367(7) 1.0243(5) 0.1755(3) 0.0395(14) Uani 1 1 d . . . H9'A H 0.6802 1.0484 0.1459 0.059 Uiso 1 1 calc R . . H9'B H 0.8242 1.0547 0.1725 0.059 Uiso 1 1 calc R . . H9'C H 0.6974 1.0421 0.2107 0.059 Uiso 1 1 calc R . . C10' C 0.8377(7) 0.8756(6) 0.2179(4) 0.059(2) Uani 1 1 d . . . H10G H 0.8462 0.8034 0.2158 0.089 Uiso 1 1 calc R . . H10H H 0.7984 0.8939 0.2530 0.089 Uiso 1 1 calc R . . H10I H 0.9251 0.9060 0.2146 0.089 Uiso 1 1 calc R . . N1" N 0.0315(5) 0.6724(3) 0.25643(18) 0.0244(9) Uani 1 1 d . . . C2" C 0.0152(5) 0.7307(4) 0.3015(2) 0.0247(11) Uani 1 1 d . . . C3" C -0.0956(5) 0.7225(4) 0.3347(2) 0.0255(11) Uani 1 1 d . . . H3"A H -0.1072 0.7659 0.3648 0.031 Uiso 1 1 calc R . . C4" C -0.1895(6) 0.6500(4) 0.3234(2) 0.0287(11) Uani 1 1 d . A . C5" C -0.1690(5) 0.5907(4) 0.2778(3) 0.0326(13) Uani 1 1 d . . . H5"A H -0.2310 0.5405 0.2689 0.039 Uiso 1 1 calc R . . C6" C -0.0592(6) 0.6043(4) 0.2455(2) 0.0296(12) Uani 1 1 d . . . H6"A H -0.0481 0.5635 0.2143 0.036 Uiso 1 1 calc R . . C7" C -0.3106(6) 0.6406(4) 0.3601(2) 0.0357(12) Uani 1 1 d D . . C8" C -0.3361(11) 0.5337(6) 0.3769(4) 0.036(2) Uiso 0.55 1 d PD A 1 H8"A H -0.3750 0.4976 0.3462 0.054 Uiso 0.55 1 calc PR A 1 H8"B H -0.3971 0.5324 0.4079 0.054 Uiso 0.55 1 calc PR A 1 H8"C H -0.2526 0.5024 0.3874 0.054 Uiso 0.55 1 calc PR A 1 C9" C -0.3080(15) 0.7057(9) 0.4107(4) 0.058(3) Uiso 0.55 1 d PD A 1 H9"A H -0.3563 0.7671 0.4034 0.088 Uiso 0.55 1 calc PR A 1 H9"B H -0.2164 0.7214 0.4200 0.088 Uiso 0.55 1 calc PR A 1 H9"C H -0.3496 0.6707 0.4411 0.088 Uiso 0.55 1 calc PR A 1 C10" C -0.4270(14) 0.6749(10) 0.3245(6) 0.067(4) Uiso 0.55 1 d PD A 1 H10A H -0.4161 0.6494 0.2874 0.100 Uiso 0.55 1 calc PR A 1 H10B H -0.4294 0.7474 0.3236 0.100 Uiso 0.55 1 calc PR A 1 H10C H -0.5098 0.6499 0.3400 0.100 Uiso 0.55 1 calc PR A 1 C8A C -0.3816(14) 0.5427(8) 0.3523(6) 0.042(3) Uiso 0.45 1 d PD A 2 H8AA H -0.4145 0.5383 0.3147 0.063 Uiso 0.45 1 calc PR A 2 H8AB H -0.4559 0.5384 0.3778 0.063 Uiso 0.45 1 calc PR A 2 H8AC H -0.3202 0.4880 0.3592 0.063 Uiso 0.45 1 calc PR A 2 C9A C -0.2594(17) 0.6422(12) 0.4193(5) 0.057(4) Uiso 0.45 1 d PD A 2 H9AA H -0.1774 0.6040 0.4216 0.085 Uiso 0.45 1 calc PR A 2 H9AB H -0.3256 0.6129 0.4435 0.085 Uiso 0.45 1 calc PR A 2 H9AC H -0.2425 0.7108 0.4304 0.085 Uiso 0.45 1 calc PR A 2 C10A C -0.4016(14) 0.7276(9) 0.3522(7) 0.050(4) Uiso 0.45 1 d PD A 2 H10D H -0.4373 0.7264 0.3150 0.076 Uiso 0.45 1 calc PR A 2 H10E H -0.3524 0.7892 0.3578 0.076 Uiso 0.45 1 calc PR A 2 H10F H -0.4742 0.7239 0.3785 0.076 Uiso 0.45 1 calc PR A 2 C1S C 0.0922(9) 0.7286(6) 0.0489(4) 0.062(2) Uiso 1 1 d . . . H1SA H 0.0528 0.6928 0.0801 0.074 Uiso 1 1 calc R . . H1SB H 0.1591 0.6849 0.0320 0.074 Uiso 1 1 calc R . . Cl1 Cl 0.1684(2) 0.83549(18) 0.07242(11) 0.0713(6) Uani 1 1 d . . . Cl2 Cl -0.0303(2) 0.7547(2) 0.00132(9) 0.0739(7) Uani 1 1 d . . . C2S C 0.7070(5) 0.9094(6) 0.5040(3) 0.061(2) Uiso 1 1 d D . . Cl3 Cl 0.5935(5) 0.8483(4) 0.54836(19) 0.0724(13) Uiso 0.60 1 d PD B 1 Cl4 Cl 0.8669(4) 0.8679(4) 0.52161(19) 0.0787(11) Uiso 0.60 1 d PD B 1 Cl3A Cl 0.6222(7) 0.8202(5) 0.5410(3) 0.074(2) Uiso 0.40 1 d PD B 2 Cl4A Cl 0.8713(6) 0.9310(6) 0.5245(3) 0.0783(17) Uiso 0.40 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01934(16) 0.02362(16) 0.02404(16) -0.00305(16) -0.00081(16) 0.00083(16) S2 0.0327(7) 0.0305(7) 0.0376(8) -0.0063(6) -0.0029(6) 0.0054(6) O1 0.029(2) 0.041(2) 0.031(2) -0.0114(18) -0.0072(16) 0.0100(18) O2 0.038(2) 0.049(3) 0.036(2) 0.004(2) -0.0082(19) 0.016(2) O3 0.055(3) 0.047(2) 0.038(2) 0.0003(19) 0.010(2) 0.002(3) O4 0.051(3) 0.038(2) 0.067(3) -0.011(2) 0.002(3) -0.009(2) N1 0.018(2) 0.0244(18) 0.027(2) -0.0033(18) -0.0028(14) -0.0023(18) C2 0.020(2) 0.025(2) 0.027(2) -0.002(2) -0.0022(18) 0.001(2) C3 0.028(3) 0.028(3) 0.029(3) -0.001(2) 0.003(2) -0.003(2) C4 0.024(2) 0.025(2) 0.023(2) -0.001(2) -0.001(2) -0.002(2) C5 0.019(2) 0.025(3) 0.032(3) 0.003(2) -0.003(2) -0.002(2) C6 0.019(2) 0.024(2) 0.022(2) 0.002(2) -0.0018(18) -0.0002(17) C7 0.030(3) 0.035(3) 0.025(3) -0.004(2) 0.000(2) -0.009(2) C8 0.049(5) 0.095(7) 0.054(5) -0.021(5) -0.015(4) 0.005(5) C9 0.129(9) 0.039(4) 0.050(4) -0.015(3) 0.010(6) -0.023(5) C10 0.046(4) 0.068(5) 0.054(4) -0.026(4) 0.012(3) -0.015(4) N1' 0.024(2) 0.028(2) 0.026(2) 0.0004(18) -0.0018(18) 0.0007(17) C2' 0.023(3) 0.027(2) 0.023(2) 0.0031(19) 0.0009(19) 0.004(2) C3' 0.025(3) 0.024(3) 0.028(3) 0.000(2) -0.001(2) 0.001(2) C4' 0.021(3) 0.033(3) 0.034(3) 0.003(2) 0.004(2) 0.001(2) C5' 0.026(3) 0.037(3) 0.035(3) 0.000(3) 0.007(2) -0.001(3) C6' 0.028(3) 0.033(3) 0.030(3) -0.002(2) 0.003(2) 0.001(2) C7' 0.022(3) 0.045(4) 0.040(3) 0.000(3) 0.005(2) -0.002(2) C8' 0.045(4) 0.075(5) 0.066(5) -0.017(4) 0.029(4) -0.019(4) C9' 0.035(3) 0.040(3) 0.043(3) -0.001(3) 0.005(3) -0.011(3) C10' 0.026(3) 0.062(5) 0.090(6) 0.020(5) -0.003(4) 0.000(3) N1" 0.023(2) 0.023(2) 0.027(2) -0.0019(17) -0.0029(18) 0.0008(16) C2" 0.019(2) 0.025(3) 0.030(3) 0.001(2) -0.0037(19) -0.0019(19) C3" 0.018(2) 0.029(3) 0.029(3) -0.002(2) 0.0012(19) 0.000(2) C4" 0.023(3) 0.025(2) 0.038(3) 0.005(2) -0.004(2) -0.001(2) C5" 0.027(3) 0.027(3) 0.043(3) -0.003(2) 0.000(2) -0.009(2) C6" 0.029(3) 0.026(3) 0.033(3) -0.008(2) -0.003(2) -0.002(2) C7" 0.026(3) 0.035(3) 0.047(3) 0.003(2) 0.008(3) -0.004(3) Cl1 0.0514(13) 0.0701(13) 0.0925(16) 0.0094(12) -0.0105(11) 0.0013(10) Cl2 0.0548(13) 0.125(2) 0.0418(9) 0.0067(11) -0.0055(9) 0.0077(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 1.918(4) . y Pd1 O1 2.001(4) . y Pd1 N1" 2.018(5) . y Pd1 N1' 2.027(5) . y S2 O4 1.425(5) . y S2 O2 1.453(5) . y S2 O3 1.474(5) . y S2 O1 1.530(4) . y N1 C2 1.347(6) . ? N1 C6 1.352(6) . ? C2 C3 1.373(8) . ? C2 C2" 1.470(7) . ? C3 C4 1.384(8) . ? C4 C5 1.419(8) . ? C4 C7 1.512(7) . ? C5 C6 1.382(7) . ? C6 C2' 1.475(7) . ? C7 C9 1.504(9) . ? C7 C10 1.507(9) . ? C7 C8 1.537(10) . ? N1' C6' 1.343(7) . ? N1' C2' 1.377(7) . ? C2' C3' 1.380(8) . ? C3' C4' 1.413(7) . ? C4' C5' 1.373(8) . ? C4' C7' 1.517(8) . ? C5' C6' 1.390(8) . ? C7' C8' 1.503(9) . ? C7' C10' 1.523(10) . ? C7' C9' 1.528(9) . ? N1" C6" 1.328(7) . ? N1" C2" 1.368(7) . ? C2" C3" 1.390(7) . ? C3" C4" 1.393(8) . ? C4" C5" 1.391(8) . ? C4" C7" 1.527(8) . ? C5" C6" 1.378(8) . ? C7" C10A 1.507(9) . ? C7" C8A 1.518(8) . ? C7" C9" 1.519(8) . ? C7" C8" 1.523(8) . ? C7" C10" 1.539(9) . ? C7" C9A 1.540(9) . ? C1S Cl1 1.736(9) . ? C1S Cl2 1.739(9) . ? C2S Cl3A 1.736(7) . ? C2S Cl4A 1.763(7) . ? C2S Cl4 1.769(7) . ? C2S Cl3 1.784(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 O1 173.10(17) . . y N1 Pd1 N1" 81.25(17) . . y O1 Pd1 N1" 91.90(18) . . y N1 Pd1 N1' 80.22(18) . . y O1 Pd1 N1' 106.61(18) . . y N1" Pd1 N1' 161.45(18) . . y O4 S2 O2 113.0(3) . . ? O4 S2 O3 110.9(3) . . ? O2 S2 O3 111.6(3) . . ? O4 S2 O1 107.7(3) . . ? O2 S2 O1 108.1(2) . . ? O3 S2 O1 105.2(3) . . ? S2 O1 Pd1 123.4(2) . . ? C2 N1 C6 122.0(4) . . ? C2 N1 Pd1 118.4(3) . . ? C6 N1 Pd1 119.6(3) . . ? N1 C2 C3 119.9(5) . . ? N1 C2 C2" 112.5(4) . . ? C3 C2 C2" 127.5(5) . . ? C2 C3 C4 121.0(5) . . ? C3 C4 C5 117.4(5) . . ? C3 C4 C7 122.3(5) . . ? C5 C4 C7 120.3(5) . . ? C6 C5 C4 120.1(5) . . ? N1 C6 C5 119.5(5) . . ? N1 C6 C2' 112.2(4) . . ? C5 C6 C2' 128.3(5) . . ? C9 C7 C10 109.2(7) . . ? C9 C7 C4 109.4(5) . . ? C10 C7 C4 112.8(5) . . ? C9 C7 C8 109.4(7) . . ? C10 C7 C8 108.2(6) . . ? C4 C7 C8 107.9(5) . . ? C6' N1' C2' 117.4(5) . . ? C6' N1' Pd1 128.8(4) . . ? C2' N1' Pd1 113.8(3) . . ? N1' C2' C3' 122.5(5) . . ? N1' C2' C6 113.8(5) . . ? C3' C2' C6 123.6(5) . . ? C2' C3' C4' 119.4(5) . . ? C5' C4' C3' 117.2(5) . . ? C5' C4' C7' 123.2(5) . . ? C3' C4' C7' 119.6(5) . . ? C4' C5' C6' 121.1(5) . . ? N1' C6' C5' 122.2(5) . . ? C8' C7' C4' 112.0(6) . . ? C8' C7' C10' 108.7(6) . . ? C4' C7' C10' 108.6(5) . . ? C8' C7' C9' 108.5(6) . . ? C4' C7' C9' 110.0(5) . . ? C10' C7' C9' 108.9(6) . . ? C6" N1" C2" 118.6(5) . . ? C6" N1" Pd1 128.6(4) . . ? C2" N1" Pd1 112.8(3) . . ? N1" C2" C3" 121.6(5) . . ? N1" C2" C2 115.0(5) . . ? C3" C2" C2 123.4(5) . . ? C2" C3" C4" 119.5(5) . . ? C5" C4" C3" 117.5(5) . . ? C5" C4" C7" 123.1(5) . . ? C3" C4" C7" 119.4(5) . . ? C6" C5" C4" 120.4(5) . . ? N1" C6" C5" 122.4(5) . . ? C10A C7" C8A 112.0(8) . . ? C9" C7" C8" 109.4(7) . . ? C10A C7" C4" 110.5(8) . . ? C8A C7" C4" 112.2(7) . . ? C9" C7" C4" 114.7(7) . . ? C8" C7" C4" 112.0(6) . . ? C9" C7" C10" 107.5(7) . . ? C8" C7" C10" 108.0(7) . . ? C4" C7" C10" 104.9(7) . . ? C10A C7" C9A 108.5(7) . . ? C8A C7" C9A 107.0(7) . . ? C4" C7" C9A 106.4(8) . . ? Cl1 C1S Cl2 111.8(5) . . ? Cl3A C2S Cl4A 115.7(6) . . ? Cl4 C2S Cl3 107.2(5) . . ? _diffrn_measured_fraction_theta_max 0.906 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.646 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.121 data_ejm16 _database_code_CSD 186163 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H39 N3 O6 Pd S' _chemical_formula_weight 640.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'N' 'N' 0.0061 0.0033 '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 13.790(5) _cell_length_b 19.148(6) _cell_length_c 10.992(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.117(8) _cell_angle_gamma 90.00 _cell_volume 2890.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21143 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 29.24 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type multiscans _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6942 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 13 _diffrn_reflns_number 14916 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5445 _reflns_number_gt 4545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.1080P)^2^+1.8739P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5445 _refine_ls_number_parameters 386 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1563 _refine_ls_wR_factor_gt 0.1490 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.051 _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 Pd Pd 0.18605(2) 0.689333(16) 0.57044(3) 0.02320(15) Uani 1 1 d . . . S1 S 0.20817(10) 0.57355(7) 0.60577(14) 0.0216(3) Uani 0.75 1 d P A 1 O1 O 0.1375(3) 0.5479(2) 0.6896(4) 0.0293(9) Uani 0.75 1 d P A 1 O2 O 0.1996(4) 0.5347(3) 0.4870(5) 0.0296(11) Uani 0.75 1 d P A 1 O3 O 0.3122(11) 0.5678(10) 0.6678(16) 0.030(3) Uani 0.75 1 d P A 1 S1A S 0.2207(3) 0.5341(3) 0.6257(4) 0.0260(9) Uiso 0.25 1 d P A 2 O1A O 0.1452(11) 0.5924(8) 0.6213(14) 0.041(3) Uiso 0.25 1 d P A 2 O2A O 0.2235(11) 0.5117(9) 0.4955(15) 0.026(4) Uiso 0.25 1 d P A 2 O3A O 0.300(3) 0.571(3) 0.664(4) 0.020(8) Uiso 0.25 1 d P A 2 N1 N 0.1890(2) 0.79213(19) 0.5472(3) 0.0214(7) Uani 1 1 d . A . C2 C 0.1394(3) 0.8328(2) 0.6207(4) 0.0197(8) Uani 1 1 d . . . C3 C 0.1486(3) 0.9041(2) 0.6149(4) 0.0234(9) Uani 1 1 d . A . H3 H 0.1138 0.9330 0.6662 0.028 Uiso 1 1 calc R . . C4 C 0.2094(3) 0.9348(2) 0.5333(4) 0.0228(9) Uani 1 1 d . . . C5 C 0.2577(3) 0.8900(2) 0.4570(4) 0.0215(9) Uani 1 1 d . A . H5 H 0.2979 0.9087 0.3991 0.026 Uiso 1 1 calc R . . C6 C 0.2462(3) 0.8183(2) 0.4670(4) 0.0232(9) Uani 1 1 d . . . C7 C 0.2221(3) 1.0136(2) 0.5297(4) 0.0260(9) Uani 1 1 d . A . C8 C 0.2509(4) 1.0406(3) 0.6603(5) 0.0421(13) Uani 1 1 d . . . H8A H 0.1999 1.0283 0.7132 0.063 Uiso 1 1 calc R A . H8B H 0.2584 1.0914 0.6586 0.063 Uiso 1 1 calc R . . H8C H 0.3125 1.0191 0.6920 0.063 Uiso 1 1 calc R . . C9 C 0.2980(4) 1.0364(3) 0.4443(5) 0.0386(12) Uani 1 1 d . . . H9A H 0.3614 1.0163 0.4724 0.058 Uiso 1 1 calc R A . H9B H 0.3029 1.0875 0.4444 0.058 Uiso 1 1 calc R . . H9C H 0.2784 1.0201 0.3612 0.058 Uiso 1 1 calc R . . C10 C 0.1239(4) 1.0454(2) 0.4814(5) 0.0355(11) Uani 1 1 d . . . H10A H 0.1042 1.0265 0.4001 0.053 Uiso 1 1 calc R A . H10B H 0.1302 1.0962 0.4763 0.053 Uiso 1 1 calc R . . H10C H 0.0746 1.0337 0.5371 0.053 Uiso 1 1 calc R . . N1' N 0.2753(3) 0.69687(17) 0.4277(3) 0.0223(8) Uani 1 1 d . A . C2' C 0.2970(3) 0.7645(2) 0.3995(4) 0.0215(9) Uani 1 1 d . A . C3' C 0.3671(3) 0.7805(2) 0.3210(4) 0.0225(9) Uani 1 1 d . . . H3' H 0.3785 0.8278 0.3006 0.027 Uiso 1 1 calc R A . C4' C 0.4215(3) 0.7271(2) 0.2712(4) 0.0256(9) Uani 1 1 d . A . C5' C 0.3930(3) 0.6597(3) 0.2936(4) 0.0295(10) Uani 1 1 d . . . H5' H 0.4235 0.6220 0.2559 0.035 Uiso 1 1 calc R A . C6' C 0.3204(3) 0.6458(2) 0.3703(5) 0.0295(10) Uani 1 1 d . A . C7' C 0.5112(3) 0.7456(2) 0.2059(4) 0.0286(10) Uani 1 1 d . . . C8' C 0.5530(4) 0.6826(3) 0.1436(5) 0.0410(13) Uani 1 1 d . A . H8'1 H 0.5705 0.6463 0.2046 0.062 Uiso 1 1 calc R . . H8'2 H 0.6111 0.6967 0.1047 0.062 Uiso 1 1 calc R . . H8'3 H 0.5042 0.6642 0.0816 0.062 Uiso 1 1 calc R . . C9' C 0.5867(4) 0.7755(4) 0.3038(5) 0.0453(14) Uani 1 1 d . A . H9'1 H 0.5996 0.7413 0.3695 0.068 Uiso 1 1 calc R . . H9'2 H 0.5612 0.8186 0.3373 0.068 Uiso 1 1 calc R . . H9'3 H 0.6472 0.7858 0.2670 0.068 Uiso 1 1 calc R . . C10' C 0.4892(4) 0.8025(2) 0.1086(5) 0.0329(11) Uani 1 1 d . A . H10D H 0.5505 0.8213 0.0836 0.049 Uiso 1 1 calc R . . H10E H 0.4518 0.8401 0.1427 0.049 Uiso 1 1 calc R . . H10F H 0.4513 0.7823 0.0375 0.049 Uiso 1 1 calc R . . N1" N 0.0961(2) 0.72160(18) 0.7024(3) 0.0210(7) Uani 1 1 d . A . C2" C 0.0808(3) 0.7922(2) 0.7032(4) 0.0205(8) Uani 1 1 d . A . C3" C 0.0138(3) 0.8223(2) 0.7743(4) 0.0224(9) Uani 1 1 d . . . H3" H 0.0062 0.8716 0.7742 0.027 Uiso 1 1 calc R A . C4" C -0.0430(3) 0.7812(2) 0.8463(4) 0.0223(9) Uani 1 1 d . A . C5" C -0.0232(3) 0.7097(2) 0.8475(4) 0.0247(9) Uani 1 1 d . . . H5" H -0.0567 0.6797 0.8983 0.030 Uiso 1 1 calc R A . C6" C 0.0450(3) 0.6819(2) 0.7750(4) 0.0246(9) Uani 1 1 d . A . C7" C -0.1230(3) 0.8140(2) 0.9137(4) 0.0253(10) Uani 1 1 d . . . C8" C -0.1719(4) 0.7609(3) 0.9936(5) 0.0337(11) Uani 1 1 d . A . H8"1 H -0.1986 0.7223 0.9426 0.051 Uiso 1 1 calc R . . H8"2 H -0.2247 0.7839 1.0325 0.051 Uiso 1 1 calc R . . H8"3 H -0.1237 0.7428 1.0567 0.051 Uiso 1 1 calc R . . C9" C -0.1986(3) 0.8442(3) 0.8152(5) 0.0345(11) Uani 1 1 d . A . H9"1 H -0.1668 0.8783 0.7654 0.052 Uiso 1 1 calc R . . H9"2 H -0.2509 0.8671 0.8549 0.052 Uiso 1 1 calc R . . H9"3 H -0.2259 0.8063 0.7629 0.052 Uiso 1 1 calc R . . C10" C -0.0825(3) 0.8732(2) 0.9964(5) 0.0315(10) Uani 1 1 d . A . H10G H -0.0356 0.8542 1.0601 0.047 Uiso 1 1 calc R . . H10H H -0.1360 0.8958 1.0345 0.047 Uiso 1 1 calc R . . H10I H -0.0501 0.9075 0.9478 0.047 Uiso 1 1 calc R . . O1W O -0.0428(3) 0.4933(2) 0.6877(4) 0.0437(9) Uani 1 1 d D . . H1WA H -0.075(4) 0.487(4) 0.629(4) 0.066 Uiso 1 1 d D . . H1WB H 0.003(3) 0.512(4) 0.671(6) 0.066 Uiso 1 1 d D . . O2W O 0.4842(3) 0.4916(2) 0.6829(5) 0.0602(13) Uani 1 1 d D . . H2WA H 0.456(5) 0.519(3) 0.715(7) 0.090 Uiso 1 1 d D . . H2WB H 0.523(5) 0.509(4) 0.650(7) 0.090 Uiso 1 1 d D . . O3W O 0.3727(4) 0.4436(3) 0.4587(5) 0.0662(13) Uani 1 1 d D . . H3WA H 0.407(5) 0.449(5) 0.516(6) 0.099 Uiso 1 1 d D . . H3WB H 0.327(4) 0.465(5) 0.465(8) 0.099 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0275(2) 0.0091(2) 0.0331(2) 0.00150(12) 0.00311(14) -0.00506(12) S1 0.0209(7) 0.0074(7) 0.0377(8) 0.0024(6) 0.0089(6) 0.0029(5) O1 0.030(2) 0.012(2) 0.048(3) 0.0006(18) 0.0144(19) -0.0012(17) O2 0.036(3) 0.012(2) 0.042(3) -0.001(2) 0.006(2) -0.005(2) O3 0.019(5) 0.017(4) 0.054(5) -0.001(2) 0.006(3) 0.005(3) N1 0.0193(16) 0.0117(17) 0.034(2) 0.0018(14) 0.0063(14) -0.0001(13) C2 0.0199(18) 0.0093(18) 0.030(2) 0.0032(16) 0.0040(16) -0.0005(16) C3 0.027(2) 0.0086(19) 0.035(2) 0.0001(17) 0.0081(18) -0.0012(16) C4 0.0218(18) 0.013(2) 0.034(2) 0.0027(17) 0.0034(16) -0.0001(16) C5 0.0218(19) 0.0093(19) 0.035(2) 0.0027(16) 0.0096(17) 0.0016(16) C6 0.022(2) 0.016(2) 0.032(2) 0.0016(17) 0.0055(17) 0.0045(16) C7 0.032(2) 0.010(2) 0.037(3) -0.0009(17) 0.0087(19) -0.0028(17) C8 0.063(3) 0.020(2) 0.043(3) -0.002(2) 0.006(3) -0.019(2) C9 0.047(3) 0.014(2) 0.059(3) -0.001(2) 0.024(3) -0.006(2) C10 0.039(3) 0.014(2) 0.055(3) 0.003(2) 0.013(2) 0.002(2) N1' 0.0279(18) 0.0078(16) 0.032(2) -0.0022(14) 0.0043(15) 0.0002(14) C2' 0.0224(19) 0.012(2) 0.030(2) -0.0004(16) 0.0017(16) 0.0036(16) C3' 0.027(2) 0.013(2) 0.028(2) 0.0000(16) 0.0031(17) 0.0046(17) C4' 0.026(2) 0.018(2) 0.032(2) -0.0040(18) 0.0020(17) 0.0120(18) C5' 0.033(2) 0.021(2) 0.034(3) -0.0102(19) -0.0024(19) 0.0082(19) C6' 0.032(2) 0.016(2) 0.040(3) -0.0035(19) 0.001(2) 0.0063(18) C7' 0.031(2) 0.027(2) 0.029(2) -0.0027(19) 0.0063(18) 0.0093(19) C8' 0.050(3) 0.034(3) 0.042(3) 0.000(2) 0.024(2) 0.019(2) C9' 0.027(2) 0.065(4) 0.044(3) -0.006(3) 0.006(2) 0.000(3) C10' 0.032(2) 0.024(2) 0.044(3) 0.001(2) 0.008(2) 0.0032(19) N1" 0.0201(16) 0.0127(17) 0.030(2) -0.0010(14) 0.0035(14) -0.0070(14) C2" 0.0240(19) 0.0084(18) 0.030(2) 0.0032(16) 0.0042(17) -0.0038(16) C3" 0.022(2) 0.0109(19) 0.034(2) 0.0003(17) 0.0022(17) -0.0016(16) C4" 0.025(2) 0.014(2) 0.028(2) 0.0006(17) 0.0025(16) -0.0035(17) C5" 0.030(2) 0.012(2) 0.033(2) 0.0031(17) 0.0071(18) -0.0045(17) C6" 0.026(2) 0.015(2) 0.033(2) 0.0009(17) 0.0044(18) -0.0042(16) C7" 0.025(2) 0.017(2) 0.035(3) 0.0014(17) 0.0083(18) -0.0020(16) C8" 0.034(2) 0.024(2) 0.047(3) 0.007(2) 0.020(2) 0.004(2) C9" 0.026(2) 0.042(3) 0.037(3) 0.005(2) 0.0053(19) 0.009(2) C10" 0.034(2) 0.021(2) 0.040(3) -0.0033(19) 0.006(2) 0.0009(19) O1W 0.046(2) 0.032(2) 0.054(2) 0.0136(18) 0.0096(18) 0.0011(18) O2W 0.054(3) 0.048(3) 0.082(4) 0.014(2) 0.021(2) 0.027(2) O3W 0.066(3) 0.053(3) 0.081(4) -0.015(3) 0.017(3) 0.010(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 N1 1.986(4) . ? Pd O1A 2.033(16) . ? Pd N1' 2.083(4) . ? Pd N1" 2.085(4) . ? Pd S1 2.2667(16) . ? S1 O1 1.483(4) . ? S1 O2 1.498(5) . ? S1 O3 1.536(15) . ? S1A O3A 1.33(5) . ? S1A O2A 1.498(17) . ? S1A O1A 1.523(17) . ? N1 C6 1.331(6) . ? N1 C2 1.352(6) . ? C2 C3 1.374(6) . ? C2 C2" 1.487(6) . ? C3 C4 1.409(6) . ? C3 H3 0.9500 . ? C4 C5 1.408(6) . ? C4 C7 1.521(6) . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 C2' 1.481(6) . ? C7 C9 1.531(6) . ? C7 C10 1.535(7) . ? C7 C8 1.544(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N1' C6' 1.346(6) . ? N1' C2' 1.371(5) . ? C2' C3' 1.386(6) . ? C3' C4' 1.408(6) . ? C3' H3' 0.9500 . ? C4' C5' 1.376(7) . ? C4' C7' 1.527(6) . ? C5' C6' 1.390(7) . ? C5' H5' 0.9500 . ? C7' C8' 1.526(6) . ? C7' C10' 1.537(7) . ? C7' C9' 1.539(7) . ? C8' H8'1 0.9800 . ? C8' H8'2 0.9800 . ? C8' H8'3 0.9800 . ? C9' H9'1 0.9800 . ? C9' H9'2 0.9800 . ? C9' H9'3 0.9800 . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? N1" C6" 1.346(6) . ? N1" C2" 1.368(5) . ? C2" C3" 1.387(6) . ? C3" C4" 1.403(6) . ? C3" H3" 0.9500 . ? C4" C5" 1.395(6) . ? C4" C7" 1.517(6) . ? C5" C6" 1.391(6) . ? C5" H5" 0.9500 . ? C7" C10" 1.528(6) . ? C7" C8" 1.538(6) . ? C7" C9" 1.547(7) . ? C8" H8"1 0.9800 . ? C8" H8"2 0.9800 . ? C8" H8"3 0.9800 . ? C9" H9"1 0.9800 . ? C9" H9"2 0.9800 . ? C9" H9"3 0.9800 . ? C10" H10G 0.9800 . ? C10" H10H 0.9800 . ? C10" H10I 0.9800 . ? O1W H1WA 0.76(3) . ? O1W H1WB 0.76(3) . ? O2W H2WA 0.76(3) . ? O2W H2WB 0.76(3) . ? O3W H3WA 0.76(3) . ? O3W H3WB 0.76(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd O1A 161.8(5) . . ? N1 Pd N1' 79.29(14) . . ? O1A Pd N1' 117.8(5) . . ? N1 Pd N1" 79.40(14) . . ? O1A Pd N1" 83.3(5) . . ? N1' Pd N1" 158.68(14) . . ? N1 Pd S1 170.98(10) . . ? O1A Pd S1 25.3(4) . . ? N1' Pd S1 96.74(10) . . ? N1" Pd S1 104.47(10) . . ? O1 S1 O2 111.8(3) . . ? O1 S1 O3 109.9(7) . . ? O2 S1 O3 110.4(7) . . ? O1 S1 Pd 110.12(17) . . ? O2 S1 Pd 109.7(2) . . ? O3 S1 Pd 104.6(7) . . ? O3A S1A O2A 111(2) . . ? O3A S1A O1A 99(2) . . ? O2A S1A O1A 104.8(9) . . ? S1A O1A Pd 118.2(9) . . ? C6 N1 C2 122.7(4) . . ? C6 N1 Pd 118.5(3) . . ? C2 N1 Pd 118.5(3) . . ? N1 C2 C3 119.4(4) . . ? N1 C2 C2" 113.2(4) . . ? C3 C2 C2" 127.4(4) . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 117.7(4) . . ? C5 C4 C7 121.8(4) . . ? C3 C4 C7 120.5(4) . . ? C6 C5 C4 119.4(4) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? N1 C6 C5 120.2(4) . . ? N1 C6 C2' 113.9(4) . . ? C5 C6 C2' 125.8(4) . . ? C4 C7 C9 112.7(4) . . ? C4 C7 C10 107.6(4) . . ? C9 C7 C10 107.8(4) . . ? C4 C7 C8 109.1(4) . . ? C9 C7 C8 110.0(4) . . ? C10 C7 C8 109.5(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6' N1' C2' 117.4(4) . . ? C6' N1' Pd 129.2(3) . . ? C2' N1' Pd 113.0(3) . . ? N1' C2' C3' 121.9(4) . . ? N1' C2' C6 114.8(4) . . ? C3' C2' C6 123.1(4) . . ? C2' C3' C4' 120.4(4) . . ? C2' C3' H3' 119.8 . . ? C4' C3' H3' 119.8 . . ? C5' C4' C3' 116.1(4) . . ? C5' C4' C7' 124.0(4) . . ? C3' C4' C7' 119.7(4) . . ? C4' C5' C6' 121.4(4) . . ? C4' C5' H5' 119.3 . . ? C6' C5' H5' 119.3 . . ? N1' C6' C5' 122.2(4) . . ? C8' C7' C4' 112.4(4) . . ? C8' C7' C10' 107.9(4) . . ? C4' C7' C10' 111.9(4) . . ? C8' C7' C9' 110.5(4) . . ? C4' C7' C9' 106.5(4) . . ? C10' C7' C9' 107.6(4) . . ? C7' C8' H8'1 109.5 . . ? C7' C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? C7' C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? C7' C9' H9'1 109.5 . . ? C7' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C7' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C7' C10' H10D 109.5 . . ? C7' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C7' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C6" N1" C2" 117.7(4) . . ? C6" N1" Pd 128.4(3) . . ? C2" N1" Pd 113.5(3) . . ? N1" C2" C3" 121.6(4) . . ? N1" C2" C2 114.9(4) . . ? C3" C2" C2 123.5(4) . . ? C2" C3" C4" 121.2(4) . . ? C2" C3" H3" 119.4 . . ? C4" C3" H3" 119.4 . . ? C5" C4" C3" 115.8(4) . . ? C5" C4" C7" 123.5(4) . . ? C3" C4" C7" 120.7(4) . . ? C6" C5" C4" 120.8(4) . . ? C6" C5" H5" 119.6 . . ? C4" C5" H5" 119.6 . . ? N1" C6" C5" 122.7(4) . . ? C4" C7" C10" 110.8(4) . . ? C4" C7" C8" 112.4(4) . . ? C10" C7" C8" 107.8(4) . . ? C4" C7" C9" 106.7(4) . . ? C10" C7" C9" 109.1(4) . . ? C8" C7" C9" 110.1(4) . . ? C7" C8" H8"1 109.5 . . ? C7" C8" H8"2 109.5 . . ? H8"1 C8" H8"2 109.5 . . ? C7" C8" H8"3 109.5 . . ? H8"1 C8" H8"3 109.5 . . ? H8"2 C8" H8"3 109.5 . . ? C7" C9" H9"1 109.5 . . ? C7" C9" H9"2 109.5 . . ? H9"1 C9" H9"2 109.5 . . ? C7" C9" H9"3 109.5 . . ? H9"1 C9" H9"3 109.5 . . ? H9"2 C9" H9"3 109.5 . . ? C7" C10" H10G 109.5 . . ? C7" C10" H10H 109.5 . . ? H10G C10" H10H 109.5 . . ? C7" C10" H10I 109.5 . . ? H10G C10" H10I 109.5 . . ? H10H C10" H10I 109.5 . . ? H1WA O1W H1WB 108(6) . . ? H2WA O2W H2WB 109(6) . . ? H3WA O3W H3WB 109(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.016 _refine_diff_density_min -2.394 _refine_diff_density_rms 0.152