# Electronic Supplementary Material (ESI) for Metallomics # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Metallomics _journal_coden_cambridge 1400 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'E. Ramachandran' _publ_contact_author_email ramschemist@gmail.com loop_ _publ_author_name K.Natarajan E.Ramachandran data_dst_m _database_code_depnum_ccdc_archive 'CCDC 769765' #TrackingRef 'new.cif.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H30 Cl2 N3 Ni1 O2 P1 S1' _chemical_formula_weight 645.19 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' P P 0.1023 0.0942 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.333(3) _cell_length_b 10.316(3) _cell_length_c 15.611(4) _cell_angle_alpha 93.677(5) _cell_angle_beta 90.998(5) _cell_angle_gamma 95.767(5) _cell_volume 1491.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3622 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7566 _exptl_absorpt_correction_T_max 0.8274 _exptl_absorpt_process_details 'SADABS, (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15489 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5832 _reflns_number_gt 3622 _reflns_threshold_expression >2\s(I) _computing_data_collection 'SMART (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction SAINT _computing_structure_solution 'WinGX-Version 1.70.01(Farrugia, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997) and CAMERON (Watkin et al., 1993)' _computing_publication_material 'PLATON (Spek, 2003)' _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^ > 2\s(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^)+(0.0844P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5832 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.892 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.30437(5) 0.46590(4) 0.33803(3) 0.03945(16) Uani 1 1 d . . . S1 S 0.14424(10) 0.30455(10) 0.30488(6) 0.0494(3) Uani 1 1 d . . . P1 P 0.38042(9) 0.47488(9) 0.20426(6) 0.0380(2) Uani 1 1 d . . . Cl2 Cl 0.55929(14) 0.93232(12) 0.68218(8) 0.0776(4) Uani 1 1 d . . . N3 N 0.2342(3) 0.4671(3) 0.45060(18) 0.0397(7) Uani 1 1 d . . . O1 O 0.4461(3) 0.6014(2) 0.36467(15) 0.0511(7) Uani 1 1 d . . . N2 N 0.1205(3) 0.3753(3) 0.4664(2) 0.0482(8) Uani 1 1 d . . . C1 C 0.5635(4) 0.4310(4) 0.1878(2) 0.0416(9) Uani 1 1 d . . . C7 C 0.2713(4) 0.3775(4) 0.1196(2) 0.0401(8) Uani 1 1 d . . . N1 N -0.0355(3) 0.2008(3) 0.4192(2) 0.0632(10) Uani 1 1 d . . . H01A H -0.0713 0.1985 0.4696 0.076 Uiso 1 1 calc R . . H01B H -0.0688 0.1447 0.3788 0.076 Uiso 1 1 calc R . . C22 C 0.4689(4) 0.6717(4) 0.4374(2) 0.0449(9) Uani 1 1 d . . . C20 C 0.2778(4) 0.5475(4) 0.5145(2) 0.0451(9) Uani 1 1 d . . . H20 H 0.2314 0.5375 0.5663 0.054 Uiso 1 1 calc R . . C8 C 0.2083(4) 0.4361(4) 0.0532(2) 0.0492(9) Uani 1 1 d . . . H8 H 0.2229 0.5261 0.0500 0.059 Uiso 1 1 calc R . . C24 C 0.6103(4) 0.8571(4) 0.5160(3) 0.0521(10) Uani 1 1 d . . . C26 C 0.4220(4) 0.7315(4) 0.5871(2) 0.0513(10) Uani 1 1 d . . . H26 H 0.3696 0.7173 0.6363 0.062 Uiso 1 1 calc R . . C21 C 0.3899(4) 0.6492(3) 0.5125(2) 0.0417(9) Uani 1 1 d . . . C18 C 0.4886(4) 0.6914(4) 0.1155(2) 0.0499(10) Uani 1 1 d . . . H18 H 0.5591 0.6403 0.0954 0.060 Uiso 1 1 calc R . . C19 C 0.0715(4) 0.2911(4) 0.4039(2) 0.0470(9) Uani 1 1 d . . . C23 C 0.5801(4) 0.7760(4) 0.4424(3) 0.0518(10) Uani 1 1 d . . . H23 H 0.6352 0.7907 0.3943 0.062 Uiso 1 1 calc R . . C12 C 0.2496(4) 0.2430(4) 0.1222(2) 0.0498(10) Uani 1 1 d . . . H12 H 0.2933 0.2018 0.1655 0.060 Uiso 1 1 calc R . . C13 C 0.3850(4) 0.6408(3) 0.1719(2) 0.0399(8) Uani 1 1 d . . . C2 C 0.6742(4) 0.4931(4) 0.2403(2) 0.0524(10) Uani 1 1 d . . . H2 H 0.6542 0.5539 0.2839 0.063 Uiso 1 1 calc R . . C6 C 0.5957(4) 0.3439(4) 0.1223(3) 0.0576(11) Uani 1 1 d . . . H6 H 0.5227 0.3034 0.0857 0.069 Uiso 1 1 calc R . . C25 C 0.5291(4) 0.8319(4) 0.5880(3) 0.0542(10) Uani 1 1 d . . . C15 C 0.2813(5) 0.8437(4) 0.1743(3) 0.0661(12) Uani 1 1 d . . . H15 H 0.2110 0.8954 0.1940 0.079 Uiso 1 1 calc R . . C11 C 0.1621(5) 0.1694(4) 0.0600(3) 0.0594(11) Uani 1 1 d . . . H11 H 0.1466 0.0793 0.0625 0.071 Uiso 1 1 calc R . . C4 C 0.8437(4) 0.3755(5) 0.1644(3) 0.0683(13) Uani 1 1 d . . . H4 H 0.9377 0.3548 0.1577 0.082 Uiso 1 1 calc R . . C16 C 0.3831(5) 0.8923(4) 0.1183(3) 0.0684(12) Uani 1 1 d . . . H16 H 0.3814 0.9762 0.1001 0.082 Uiso 1 1 calc R . . C3 C 0.8137(4) 0.4652(5) 0.2280(3) 0.0622(12) Uani 1 1 d . . . H3 H 0.8879 0.5074 0.2631 0.075 Uiso 1 1 calc R . . C5 C 0.7370(4) 0.3160(5) 0.1106(3) 0.0703(13) Uani 1 1 d . . . H5 H 0.7586 0.2571 0.0663 0.084 Uiso 1 1 calc R . . C14 C 0.2831(4) 0.7201(4) 0.2012(2) 0.0540(10) Uani 1 1 d . . . H14 H 0.2149 0.6892 0.2397 0.065 Uiso 1 1 calc R . . C10 C 0.0990(4) 0.2280(5) -0.0045(3) 0.0654(12) Uani 1 1 d . . . H10 H 0.0398 0.1783 -0.0454 0.079 Uiso 1 1 calc R . . C17 C 0.4862(5) 0.8159(4) 0.0899(3) 0.0636(12) Uani 1 1 d . . . H17 H 0.5556 0.8487 0.0528 0.076 Uiso 1 1 calc R . . C9 C 0.1230(4) 0.3601(5) -0.0089(3) 0.0618(11) Uani 1 1 d . . . H9 H 0.0819 0.3997 -0.0538 0.074 Uiso 1 1 calc R . . C27 C 0.7269(5) 0.9682(4) 0.5180(3) 0.0770(14) Uani 1 1 d . . . H27B H 0.6855 1.0492 0.5280 0.115 Uiso 1 1 calc R . . H27A H 0.7747 0.9677 0.4640 0.115 Uiso 1 1 calc R . . H27C H 0.7953 0.9590 0.5633 0.115 Uiso 1 1 calc R . . Cl1 Cl 0.97515(13) 0.28652(12) 0.62611(7) 0.0750(4) Uani 1 1 d . . . O2 O 0.9236(6) 0.9661(4) 0.3142(3) 0.1263(16) Uani 1 1 d . . . H2A H 0.9502 0.9020 0.3360 0.189 Uiso 1 1 calc R . . C29 C 0.8357(10) 0.9252(7) 0.2412(4) 0.147(3) Uani 1 1 d . . . H29A H 0.8795 0.8579 0.2077 0.176 Uiso 1 1 calc R . . H29B H 0.7427 0.8874 0.2595 0.176 Uiso 1 1 calc R . . C28 C 0.8162(9) 1.0244(8) 0.1914(5) 0.157(3) Uani 1 1 d . . . H28B H 0.7660 1.0881 0.2229 0.235 Uiso 1 1 calc R . . H28A H 0.7606 0.9915 0.1409 0.235 Uiso 1 1 calc R . . H28C H 0.9081 1.0643 0.1750 0.235 Uiso 1 1 calc R . . H2N H 0.106(4) 0.371(4) 0.518(3) 0.055(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0321(3) 0.0489(3) 0.0364(3) 0.0038(2) 0.00312(19) -0.0017(2) S1 0.0415(6) 0.0587(6) 0.0454(6) 0.0008(5) 0.0031(4) -0.0067(4) P1 0.0299(5) 0.0471(6) 0.0368(5) 0.0032(4) 0.0032(4) 0.0022(4) Cl2 0.0877(9) 0.0705(8) 0.0691(8) -0.0190(6) -0.0108(6) -0.0020(6) N3 0.0362(17) 0.0436(17) 0.0387(17) 0.0037(14) 0.0019(13) -0.0001(13) O1 0.0427(15) 0.0654(18) 0.0409(15) -0.0002(13) 0.0071(11) -0.0143(13) N2 0.043(2) 0.058(2) 0.041(2) 0.0062(17) 0.0114(16) -0.0106(15) C1 0.0317(19) 0.055(2) 0.039(2) 0.0086(17) 0.0038(15) 0.0060(17) C7 0.0292(19) 0.049(2) 0.042(2) 0.0013(17) 0.0040(15) 0.0056(16) N1 0.053(2) 0.069(2) 0.063(2) 0.0064(18) 0.0090(17) -0.0200(18) C22 0.038(2) 0.051(2) 0.045(2) 0.0043(19) -0.0022(17) 0.0020(17) C20 0.044(2) 0.054(2) 0.038(2) 0.0071(18) 0.0069(17) 0.0049(18) C8 0.044(2) 0.060(2) 0.043(2) 0.0011(19) -0.0011(18) 0.0036(19) C24 0.042(2) 0.048(2) 0.065(3) 0.003(2) -0.0081(19) -0.0014(18) C26 0.052(2) 0.059(3) 0.043(2) 0.0058(19) 0.0024(18) 0.001(2) C21 0.037(2) 0.045(2) 0.043(2) 0.0025(17) -0.0021(16) 0.0024(16) C18 0.053(2) 0.052(2) 0.044(2) 0.0020(18) 0.0081(18) 0.0039(19) C19 0.040(2) 0.049(2) 0.052(2) 0.0050(19) 0.0029(18) 0.0023(18) C23 0.043(2) 0.054(2) 0.057(2) 0.008(2) 0.0018(18) -0.0072(19) C12 0.047(2) 0.054(3) 0.049(2) 0.0014(19) 0.0037(18) 0.0089(19) C13 0.037(2) 0.045(2) 0.0365(19) -0.0058(16) 0.0000(15) 0.0025(16) C2 0.037(2) 0.071(3) 0.048(2) 0.000(2) 0.0017(18) 0.0028(19) C6 0.038(2) 0.075(3) 0.060(3) -0.009(2) -0.0003(19) 0.013(2) C25 0.055(3) 0.051(2) 0.056(3) -0.004(2) -0.007(2) 0.005(2) C15 0.070(3) 0.057(3) 0.073(3) -0.009(2) 0.004(2) 0.021(2) C11 0.060(3) 0.051(3) 0.062(3) -0.012(2) 0.007(2) -0.005(2) C4 0.036(2) 0.104(4) 0.069(3) 0.010(3) 0.005(2) 0.022(2) C16 0.090(4) 0.049(3) 0.066(3) 0.003(2) -0.005(3) 0.007(3) C3 0.031(2) 0.095(3) 0.059(3) 0.002(2) -0.0046(19) 0.001(2) C5 0.044(3) 0.094(4) 0.072(3) -0.014(3) 0.005(2) 0.019(2) C14 0.056(3) 0.056(3) 0.051(2) 0.001(2) 0.0093(19) 0.009(2) C10 0.050(3) 0.079(3) 0.062(3) -0.020(2) -0.004(2) -0.001(2) C17 0.074(3) 0.054(3) 0.061(3) 0.009(2) 0.010(2) -0.009(2) C9 0.049(3) 0.084(3) 0.051(3) 0.002(2) -0.008(2) 0.008(2) C27 0.059(3) 0.063(3) 0.103(4) 0.004(3) -0.004(3) -0.017(2) Cl1 0.0831(8) 0.0802(8) 0.0611(7) 0.0112(6) 0.0256(6) -0.0027(6) O2 0.198(5) 0.081(3) 0.097(3) -0.010(2) -0.049(3) 0.018(3) C29 0.241(10) 0.107(6) 0.092(5) 0.025(4) -0.015(6) 0.014(6) C28 0.174(8) 0.150(7) 0.137(7) 0.006(6) -0.019(6) -0.022(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Ni1 O1 1.847(2) . ? Ni1 N3 1.886(3) . ? Ni1 S1 2.1528(11) . ? Ni1 P1 2.2220(11) . ? S1 C19 1.707(4) . ? P1 C13 1.812(4) . ? P1 C1 1.829(3) . ? P1 C7 1.836(4) . ? Cl2 C25 1.745(4) . ? N3 C20 1.289(4) . ? N3 N2 1.386(4) . ? O1 C22 1.310(4) . ? N2 C19 1.308(5) . ? N2 H2N 0.83(4) . ? C1 C6 1.375(5) . ? C1 C2 1.386(5) . ? C7 C8 1.385(5) . ? C7 C12 1.386(5) . ? N1 C19 1.332(5) . ? N1 H01A 0.8600 . ? N1 H01B 0.8600 . ? C22 C21 1.415(5) . ? C22 C23 1.416(5) . ? C20 C21 1.408(5) . ? C20 H20 0.9300 . ? C8 C9 1.391(5) . ? C8 H8 0.9300 . ? C24 C23 1.385(5) . ? C24 C25 1.390(6) . ? C24 C27 1.497(5) . ? C26 C25 1.365(5) . ? C26 C21 1.405(5) . ? C26 H26 0.9300 . ? C18 C17 1.372(5) . ? C18 C13 1.404(5) . ? C18 H18 0.9300 . ? C23 H23 0.9300 . ? C12 C11 1.393(5) . ? C12 H12 0.9300 . ? C13 C14 1.380(5) . ? C2 C3 1.376(5) . ? C2 H2 0.9300 . ? C6 C5 1.390(5) . ? C6 H6 0.9300 . ? C15 C14 1.370(5) . ? C15 C16 1.381(6) . ? C15 H15 0.9300 . ? C11 C10 1.362(6) . ? C11 H11 0.9300 . ? C4 C5 1.362(6) . ? C4 C3 1.365(6) . ? C4 H4 0.9300 . ? C16 C17 1.366(6) . ? C16 H16 0.9300 . ? C3 H3 0.9300 . ? C5 H5 0.9300 . ? C14 H14 0.9300 . ? C10 C9 1.364(6) . ? C10 H10 0.9300 . ? C17 H17 0.9300 . ? C9 H9 0.9300 . ? C27 H27B 0.9600 . ? C27 H27A 0.9600 . ? C27 H27C 0.9600 . ? O2 C29 1.409(7) . ? O2 H2A 0.8200 . ? C29 C28 1.349(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C28 H28B 0.9600 . ? C28 H28A 0.9600 . ? C28 H28C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N3 93.66(12) . . ? O1 Ni1 S1 178.14(9) . . ? N3 Ni1 S1 87.61(9) . . ? O1 Ni1 P1 85.59(8) . . ? N3 Ni1 P1 176.63(9) . . ? S1 Ni1 P1 93.23(4) . . ? C19 S1 Ni1 97.90(14) . . ? C13 P1 C1 104.62(16) . . ? C13 P1 C7 104.11(16) . . ? C1 P1 C7 104.46(16) . . ? C13 P1 Ni1 109.76(11) . . ? C1 P1 Ni1 115.19(11) . . ? C7 P1 Ni1 117.42(12) . . ? C20 N3 N2 115.9(3) . . ? C20 N3 Ni1 126.8(3) . . ? N2 N3 Ni1 117.3(2) . . ? C22 O1 Ni1 128.1(2) . . ? C19 N2 N3 118.7(3) . . ? C19 N2 H2N 127(3) . . ? N3 N2 H2N 112(3) . . ? C6 C1 C2 119.0(3) . . ? C6 C1 P1 122.2(3) . . ? C2 C1 P1 118.7(3) . . ? C8 C7 C12 118.9(3) . . ? C8 C7 P1 121.2(3) . . ? C12 C7 P1 119.8(3) . . ? C19 N1 H01A 120.0 . . ? C19 N1 H01B 120.0 . . ? H01A N1 H01B 120.0 . . ? O1 C22 C21 124.1(3) . . ? O1 C22 C23 118.7(3) . . ? C21 C22 C23 117.3(3) . . ? N3 C20 C21 125.4(3) . . ? N3 C20 H20 117.3 . . ? C21 C20 H20 117.3 . . ? C7 C8 C9 120.0(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C23 C24 C25 117.8(4) . . ? C23 C24 C27 121.1(4) . . ? C25 C24 C27 121.1(4) . . ? C25 C26 C21 120.7(4) . . ? C25 C26 H26 119.6 . . ? C21 C26 H26 119.6 . . ? C26 C21 C20 118.6(3) . . ? C26 C21 C22 119.5(3) . . ? C20 C21 C22 121.8(3) . . ? C17 C18 C13 120.2(4) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? N2 C19 N1 118.9(3) . . ? N2 C19 S1 118.5(3) . . ? N1 C19 S1 122.6(3) . . ? C24 C23 C22 122.8(4) . . ? C24 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C7 C12 C11 119.9(4) . . ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C18 118.2(3) . . ? C14 C13 P1 120.1(3) . . ? C18 C13 P1 121.6(3) . . ? C3 C2 C1 120.2(4) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C1 C6 C5 120.3(4) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C26 C25 C24 121.8(4) . . ? C26 C25 Cl2 118.0(3) . . ? C24 C25 Cl2 120.1(3) . . ? C14 C15 C16 120.5(4) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C17 C16 C15 119.4(4) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C4 C5 C6 119.7(4) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C15 C14 C13 120.8(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C11 C10 C9 119.7(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C16 C17 C18 120.8(4) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C10 C9 C8 120.7(4) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? C24 C27 H27B 109.5 . . ? C24 C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? C24 C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? C29 O2 H2A 109.5 . . ? C28 C29 O2 112.2(7) . . ? C28 C29 H29A 109.2 . . ? O2 C29 H29A 109.2 . . ? C28 C29 H29B 109.2 . . ? O2 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C29 C28 H28B 109.5 . . ? C29 C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? C29 C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ni1 S1 C19 132(3) . . . . ? N3 Ni1 S1 C19 -1.19(15) . . . . ? P1 Ni1 S1 C19 -177.92(13) . . . . ? O1 Ni1 P1 C13 -52.12(15) . . . . ? N3 Ni1 P1 C13 25.0(16) . . . . ? S1 Ni1 P1 C13 129.32(12) . . . . ? O1 Ni1 P1 C1 65.61(16) . . . . ? N3 Ni1 P1 C1 142.7(16) . . . . ? S1 Ni1 P1 C1 -112.96(14) . . . . ? O1 Ni1 P1 C7 -170.68(16) . . . . ? N3 Ni1 P1 C7 -93.6(16) . . . . ? S1 Ni1 P1 C7 10.75(13) . . . . ? O1 Ni1 N3 C20 3.6(3) . . . . ? S1 Ni1 N3 C20 -177.7(3) . . . . ? P1 Ni1 N3 C20 -73.2(17) . . . . ? O1 Ni1 N3 N2 -178.9(2) . . . . ? S1 Ni1 N3 N2 -0.2(2) . . . . ? P1 Ni1 N3 N2 104.3(16) . . . . ? N3 Ni1 O1 C22 -4.9(3) . . . . ? S1 Ni1 O1 C22 -138(2) . . . . ? P1 Ni1 O1 C22 171.8(3) . . . . ? C20 N3 N2 C19 180.0(3) . . . . ? Ni1 N3 N2 C19 2.2(4) . . . . ? C13 P1 C1 C6 -108.1(3) . . . . ? C7 P1 C1 C6 1.0(4) . . . . ? Ni1 P1 C1 C6 131.3(3) . . . . ? C13 P1 C1 C2 68.2(3) . . . . ? C7 P1 C1 C2 177.3(3) . . . . ? Ni1 P1 C1 C2 -52.4(3) . . . . ? C13 P1 C7 C8 -3.2(3) . . . . ? C1 P1 C7 C8 -112.6(3) . . . . ? Ni1 P1 C7 C8 118.4(3) . . . . ? C13 P1 C7 C12 177.7(3) . . . . ? C1 P1 C7 C12 68.2(3) . . . . ? Ni1 P1 C7 C12 -60.8(3) . . . . ? Ni1 O1 C22 C21 4.1(5) . . . . ? Ni1 O1 C22 C23 -176.8(2) . . . . ? N2 N3 C20 C21 -179.0(3) . . . . ? Ni1 N3 C20 C21 -1.5(5) . . . . ? C12 C7 C8 C9 0.9(5) . . . . ? P1 C7 C8 C9 -178.3(3) . . . . ? C25 C26 C21 C20 -179.6(3) . . . . ? C25 C26 C21 C22 -0.6(6) . . . . ? N3 C20 C21 C26 178.1(3) . . . . ? N3 C20 C21 C22 -0.9(6) . . . . ? O1 C22 C21 C26 -179.3(3) . . . . ? C23 C22 C21 C26 1.5(5) . . . . ? O1 C22 C21 C20 -0.4(6) . . . . ? C23 C22 C21 C20 -179.5(3) . . . . ? N3 N2 C19 N1 178.4(3) . . . . ? N3 N2 C19 S1 -3.5(5) . . . . ? Ni1 S1 C19 N2 2.8(3) . . . . ? Ni1 S1 C19 N1 -179.2(3) . . . . ? C25 C24 C23 C22 1.4(6) . . . . ? C27 C24 C23 C22 -178.6(4) . . . . ? O1 C22 C23 C24 178.8(3) . . . . ? C21 C22 C23 C24 -2.0(6) . . . . ? C8 C7 C12 C11 -1.8(5) . . . . ? P1 C7 C12 C11 177.4(3) . . . . ? C17 C18 C13 C14 -0.8(5) . . . . ? C17 C18 C13 P1 177.8(3) . . . . ? C1 P1 C13 C14 -158.6(3) . . . . ? C7 P1 C13 C14 92.1(3) . . . . ? Ni1 P1 C13 C14 -34.4(3) . . . . ? C1 P1 C13 C18 22.8(3) . . . . ? C7 P1 C13 C18 -86.5(3) . . . . ? Ni1 P1 C13 C18 147.0(3) . . . . ? C6 C1 C2 C3 -1.7(6) . . . . ? P1 C1 C2 C3 -178.1(3) . . . . ? C2 C1 C6 C5 1.8(6) . . . . ? P1 C1 C6 C5 178.2(3) . . . . ? C21 C26 C25 C24 0.0(6) . . . . ? C21 C26 C25 Cl2 178.4(3) . . . . ? C23 C24 C25 C26 -0.4(6) . . . . ? C27 C24 C25 C26 179.7(4) . . . . ? C23 C24 C25 Cl2 -178.8(3) . . . . ? C27 C24 C25 Cl2 1.3(5) . . . . ? C7 C12 C11 C10 1.0(6) . . . . ? C14 C15 C16 C17 -0.1(7) . . . . ? C5 C4 C3 C2 2.2(7) . . . . ? C1 C2 C3 C4 -0.3(7) . . . . ? C3 C4 C5 C6 -2.0(7) . . . . ? C1 C6 C5 C4 0.0(7) . . . . ? C16 C15 C14 C13 -1.1(7) . . . . ? C18 C13 C14 C15 1.5(6) . . . . ? P1 C13 C14 C15 -177.1(3) . . . . ? C12 C11 C10 C9 0.8(6) . . . . ? C15 C16 C17 C18 0.8(7) . . . . ? C13 C18 C17 C16 -0.4(6) . . . . ? C11 C10 C9 C8 -1.7(6) . . . . ? C7 C8 C9 C10 0.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.794 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.085 data_r14010 _database_code_depnum_ccdc_archive 'CCDC 790190' #TrackingRef 'r14010.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H23 Cl N3 O P Pd S' _chemical_formula_sum 'C27 H23 Cl N3 O P Pd S' _chemical_formula_weight 610.36 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.7387(5) _cell_length_b 24.7405(18) _cell_length_c 27.364(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5239.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9986 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 22.33 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7503 _exptl_absorpt_correction_T_max 0.9601 _exptl_absorpt_process_details 'sadabs v2008/1' _exptl_special_details ; All H atoms were added in their calculated positions and were treated using appropriate riding models. ; _diffrn_ambient_temperature 296(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 101325 _diffrn_reflns_av_R_equivalents 0.0995 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.38 _reflns_number_total 4806 _reflns_number_gt 3544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0260P)^2^+3.9050P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4806 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.52199(3) 0.097948(10) 0.543362(9) 0.03103(8) Uani 1 1 d . . . Cl1 Cl 0.7304(2) 0.08805(6) 0.28417(4) 0.0886(4) Uani 1 1 d . . . S1 S 0.30344(12) 0.07649(4) 0.59323(3) 0.0429(2) Uani 1 1 d . . . P1 P 0.66065(11) 0.14461(3) 0.60362(3) 0.0299(2) Uani 1 1 d . . . O1 O 0.7170(3) 0.11215(10) 0.49658(8) 0.0448(6) Uani 1 1 d . . . N1 N 0.3782(3) 0.06040(10) 0.49181(10) 0.0350(7) Uani 1 1 d . . . N2 N 0.2204(4) 0.03657(11) 0.50375(11) 0.0415(7) Uani 1 1 d . . . N3 N 0.0295(4) 0.02133(12) 0.56566(12) 0.0524(8) Uani 1 1 d . . . H3A H -0.0382 0.0048 0.5457 0.063 Uiso 1 1 calc R . . H3B H 0.0011 0.0246 0.5959 0.063 Uiso 1 1 calc R . . C1 C 0.7134(5) 0.10245(13) 0.44961(12) 0.0399(8) Uani 1 1 d . . . C2 C 0.8610(5) 0.11728(15) 0.42242(13) 0.0463(9) Uani 1 1 d . . . H2 H 0.9552 0.1313 0.4393 0.056 Uiso 1 1 calc R . . C3 C 0.8741(5) 0.11233(14) 0.37236(14) 0.0491(10) Uani 1 1 d . . . C4 C 0.7291(6) 0.09164(15) 0.34805(13) 0.0531(10) Uani 1 1 d . . . C5 C 0.5876(6) 0.07448(15) 0.37257(14) 0.0496(10) Uani 1 1 d . . . H5 H 0.4958 0.0599 0.3550 0.059 Uiso 1 1 calc R . . C6 C 0.5749(5) 0.07810(13) 0.42420(13) 0.0391(9) Uani 1 1 d . . . C7 C 0.4208(5) 0.05766(13) 0.44608(13) 0.0402(9) Uani 1 1 d . . . H7 H 0.3427 0.0406 0.4253 0.048 Uiso 1 1 calc R . . C8 C 0.1808(4) 0.04212(13) 0.54949(14) 0.0393(8) Uani 1 1 d . . . C9 C 1.0365(6) 0.12848(18) 0.34606(15) 0.0685(13) Uani 1 1 d . . . H9A H 1.1249 0.1369 0.3695 0.103 Uiso 1 1 calc R . . H9B H 1.0140 0.1597 0.3262 0.103 Uiso 1 1 calc R . . H9C H 1.0745 0.0992 0.3257 0.103 Uiso 1 1 calc R . . C10 C 0.5157(4) 0.18346(12) 0.64231(12) 0.0339(8) Uani 1 1 d . . . C11 C 0.3886(5) 0.21429(15) 0.62072(14) 0.0474(9) Uani 1 1 d . . . H11 H 0.3772 0.2140 0.5869 0.057 Uiso 1 1 calc R . . C12 C 0.2775(5) 0.24565(17) 0.64844(16) 0.0578(11) Uani 1 1 d . . . H12 H 0.1940 0.2668 0.6332 0.069 Uiso 1 1 calc R . . C13 C 0.2910(5) 0.24537(18) 0.69838(17) 0.0626(12) Uani 1 1 d . . . H13 H 0.2176 0.2666 0.7172 0.075 Uiso 1 1 calc R . . C14 C 0.4132(6) 0.21362(19) 0.72035(15) 0.0689(13) Uani 1 1 d . . . H14 H 0.4199 0.2126 0.7543 0.083 Uiso 1 1 calc R . . C15 C 0.5270(5) 0.18306(16) 0.69290(13) 0.0522(10) Uani 1 1 d . . . H15 H 0.6109 0.1623 0.7083 0.063 Uiso 1 1 calc R . . C16 C 0.7811(4) 0.10213(13) 0.64579(11) 0.0328(7) Uani 1 1 d . . . C17 C 0.7104(5) 0.05255(14) 0.65924(13) 0.0442(9) Uani 1 1 d . . . H17 H 0.6053 0.0416 0.6461 0.053 Uiso 1 1 calc R . . C18 C 0.7956(6) 0.01983(16) 0.69194(15) 0.0580(11) Uani 1 1 d . . . H18 H 0.7470 -0.0130 0.7011 0.070 Uiso 1 1 calc R . . C19 C 0.9508(6) 0.03515(18) 0.71100(15) 0.0640(12) Uani 1 1 d . . . H19 H 1.0076 0.0127 0.7330 0.077 Uiso 1 1 calc R . . C20 C 1.0238(5) 0.08369(18) 0.69785(14) 0.0582(11) Uani 1 1 d . . . H20 H 1.1304 0.0938 0.7107 0.070 Uiso 1 1 calc R . . C21 C 0.9384(5) 0.11772(15) 0.66540(13) 0.0440(9) Uani 1 1 d . . . H21 H 0.9868 0.1508 0.6569 0.053 Uiso 1 1 calc R . . C22 C 0.8155(4) 0.19299(12) 0.57969(11) 0.0306(8) Uani 1 1 d . . . C23 C 0.7961(5) 0.24829(14) 0.58456(13) 0.0454(9) Uani 1 1 d . . . H23 H 0.7055 0.2622 0.6030 0.054 Uiso 1 1 calc R . . C24 C 0.9117(6) 0.28308(16) 0.56187(16) 0.0617(12) Uani 1 1 d . . . H24 H 0.8985 0.3203 0.5652 0.074 Uiso 1 1 calc R . . C25 C 1.0455(6) 0.26274(19) 0.53448(15) 0.0617(12) Uani 1 1 d . . . H25 H 1.1218 0.2861 0.5188 0.074 Uiso 1 1 calc R . . C26 C 1.0664(5) 0.20807(18) 0.53028(13) 0.0523(10) Uani 1 1 d . . . H26 H 1.1581 0.1943 0.5122 0.063 Uiso 1 1 calc R . . C27 C 0.9522(4) 0.17305(15) 0.55267(12) 0.0406(9) Uani 1 1 d . . . H27 H 0.9674 0.1359 0.5496 0.049 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 0.03270(15) 0.02761(13) 0.03278(14) -0.00159(11) -0.00387(12) -0.00381(12) Cl1 0.1207(11) 0.1068(11) 0.0383(6) -0.0179(6) 0.0093(7) -0.0150(8) S1 0.0380(5) 0.0473(5) 0.0434(5) -0.0068(4) 0.0020(4) -0.0120(4) P1 0.0316(5) 0.0277(4) 0.0303(5) 0.0010(4) -0.0030(4) -0.0037(4) O1 0.0441(15) 0.0567(16) 0.0336(14) -0.0068(11) -0.0005(11) -0.0137(12) N1 0.0360(17) 0.0301(16) 0.0389(17) -0.0014(12) -0.0047(13) -0.0032(13) N2 0.0382(18) 0.0374(17) 0.0490(19) -0.0068(14) -0.0028(15) -0.0105(14) N3 0.0439(19) 0.057(2) 0.057(2) -0.0120(16) 0.0029(16) -0.0196(17) C1 0.045(2) 0.0342(19) 0.041(2) -0.0029(17) 0.0002(17) -0.0007(17) C2 0.047(2) 0.046(2) 0.046(2) -0.0062(17) 0.0033(19) -0.0013(18) C3 0.065(3) 0.035(2) 0.047(2) -0.0030(17) 0.013(2) 0.0032(19) C4 0.079(3) 0.043(2) 0.037(2) -0.0090(18) 0.004(2) -0.001(2) C5 0.064(3) 0.042(2) 0.043(2) -0.0132(18) -0.008(2) -0.004(2) C6 0.048(2) 0.0302(18) 0.039(2) -0.0060(15) 0.0000(17) -0.0001(16) C7 0.045(2) 0.0316(18) 0.044(2) -0.0064(16) -0.0090(17) -0.0037(16) C8 0.035(2) 0.0309(18) 0.053(2) -0.0002(17) -0.0038(18) -0.0034(15) C9 0.076(3) 0.068(3) 0.061(3) -0.010(2) 0.026(2) -0.006(3) C10 0.032(2) 0.0311(17) 0.0382(19) -0.0048(14) -0.0017(16) -0.0039(15) C11 0.044(2) 0.051(2) 0.048(2) -0.0059(19) -0.0072(18) 0.0017(19) C12 0.042(2) 0.055(3) 0.076(3) -0.009(2) -0.004(2) 0.013(2) C13 0.054(3) 0.064(3) 0.070(3) -0.015(2) 0.016(2) 0.007(2) C14 0.077(3) 0.089(3) 0.041(2) -0.008(2) 0.011(2) 0.013(3) C15 0.053(2) 0.060(2) 0.044(2) -0.0026(19) 0.002(2) 0.011(2) C16 0.0346(19) 0.0340(19) 0.0296(17) -0.0017(15) 0.0008(14) 0.0025(16) C17 0.048(2) 0.040(2) 0.045(2) 0.0059(17) -0.0046(18) 0.0012(18) C18 0.070(3) 0.044(2) 0.060(3) 0.017(2) -0.004(2) 0.003(2) C19 0.071(3) 0.070(3) 0.051(3) 0.021(2) -0.012(2) 0.024(3) C20 0.042(2) 0.085(3) 0.047(2) 0.004(2) -0.012(2) 0.009(2) C21 0.044(2) 0.049(2) 0.039(2) 0.0025(17) -0.0051(17) -0.0006(18) C22 0.0318(19) 0.0294(18) 0.0305(18) 0.0052(14) -0.0106(15) -0.0071(15) C23 0.043(2) 0.036(2) 0.057(2) 0.0030(18) -0.0048(19) -0.0024(18) C24 0.068(3) 0.037(2) 0.079(3) 0.016(2) -0.016(3) -0.016(2) C25 0.056(3) 0.075(3) 0.054(3) 0.023(2) -0.007(2) -0.031(2) C26 0.042(2) 0.073(3) 0.042(2) 0.001(2) 0.0014(17) -0.014(2) C27 0.037(2) 0.043(2) 0.041(2) -0.0005(16) -0.0055(17) -0.0091(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 O1 2.010(2) . ? Pd1 N1 2.023(3) . ? Pd1 S1 2.2371(9) . ? Pd1 P1 2.2810(9) . ? Cl1 C4 1.750(4) . ? S1 C8 1.748(3) . ? P1 C22 1.816(3) . ? P1 C10 1.817(3) . ? P1 C16 1.818(3) . ? O1 C1 1.308(4) . ? N1 C7 1.296(4) . ? N1 N2 1.394(4) . ? N2 C8 1.296(4) . ? N3 C8 1.353(4) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? C1 C2 1.411(5) . ? C1 C6 1.413(5) . ? C2 C3 1.379(5) . ? C2 H2 0.9300 . ? C3 C4 1.401(6) . ? C3 C9 1.503(5) . ? C4 C5 1.353(5) . ? C5 C6 1.419(5) . ? C5 H5 0.9300 . ? C6 C7 1.427(5) . ? C7 H7 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.378(5) . ? C10 C15 1.387(5) . ? C11 C12 1.385(5) . ? C11 H11 0.9300 . ? C12 C13 1.371(6) . ? C12 H12 0.9300 . ? C13 C14 1.369(6) . ? C13 H13 0.9300 . ? C14 C15 1.382(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C21 1.385(5) . ? C16 C17 1.393(5) . ? C17 C18 1.375(5) . ? C17 H17 0.9300 . ? C18 C19 1.363(6) . ? C18 H18 0.9300 . ? C19 C20 1.375(6) . ? C19 H19 0.9300 . ? C20 C21 1.391(5) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.382(5) . ? C22 C23 1.383(5) . ? C23 C24 1.388(5) . ? C23 H23 0.9300 . ? C24 C25 1.374(6) . ? C24 H24 0.9300 . ? C25 C26 1.367(6) . ? C25 H25 0.9300 . ? C26 C27 1.381(5) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? 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 O1 Pd1 N1 92.83(10) . . ? O1 Pd1 S1 176.09(7) . . ? N1 Pd1 S1 84.29(8) . . ? O1 Pd1 P1 91.07(7) . . ? N1 Pd1 P1 174.50(8) . . ? S1 Pd1 P1 92.00(3) . . ? C8 S1 Pd1 96.22(13) . . ? C22 P1 C10 105.58(15) . . ? C22 P1 C16 105.75(15) . . ? C10 P1 C16 104.62(15) . . ? C22 P1 Pd1 112.55(10) . . ? C10 P1 Pd1 113.48(11) . . ? C16 P1 Pd1 114.04(11) . . ? C1 O1 Pd1 125.3(2) . . ? C7 N1 N2 115.3(3) . . ? C7 N1 Pd1 123.9(2) . . ? N2 N1 Pd1 120.8(2) . . ? C8 N2 N1 112.9(3) . . ? C8 N3 H3A 120.0 . . ? C8 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? O1 C1 C2 116.9(3) . . ? O1 C1 C6 125.3(3) . . ? C2 C1 C6 117.7(3) . . ? C3 C2 C1 124.1(4) . . ? C3 C2 H2 118.0 . . ? C1 C2 H2 118.0 . . ? C2 C3 C4 116.4(4) . . ? C2 C3 C9 120.9(4) . . ? C4 C3 C9 122.6(4) . . ? C5 C4 C3 121.8(4) . . ? C5 C4 Cl1 118.9(3) . . ? C3 C4 Cl1 119.2(3) . . ? C4 C5 C6 122.0(4) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C1 C6 C5 117.7(3) . . ? C1 C6 C7 125.4(3) . . ? C5 C6 C7 116.9(3) . . ? N1 C7 C6 126.8(3) . . ? N1 C7 H7 116.6 . . ? C6 C7 H7 116.6 . . ? N2 C8 N3 118.7(3) . . ? N2 C8 S1 125.7(3) . . ? N3 C8 S1 115.5(3) . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 118.5(3) . . ? C11 C10 P1 118.9(3) . . ? C15 C10 P1 122.6(3) . . ? C10 C11 C12 121.3(4) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 119.7(4) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 119.6(4) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C13 C14 C15 121.0(4) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C10 119.9(4) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? C21 C16 C17 119.2(3) . . ? C21 C16 P1 122.4(3) . . ? C17 C16 P1 118.4(3) . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 120.5(4) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C18 C19 C20 120.3(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 120.0(4) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C16 C21 C20 119.8(4) . . ? C16 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C27 C22 C23 119.2(3) . . ? C27 C22 P1 117.6(2) . . ? C23 C22 P1 123.1(3) . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.2(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C24 119.8(4) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.5(4) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C22 120.2(4) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 S1 C8 1.70(14) . . . . ? P1 Pd1 S1 C8 177.64(12) . . . . ? O1 Pd1 P1 C22 23.38(14) . . . . ? S1 Pd1 P1 C22 -159.04(12) . . . . ? O1 Pd1 P1 C10 143.23(14) . . . . ? S1 Pd1 P1 C10 -39.20(12) . . . . ? O1 Pd1 P1 C16 -97.09(14) . . . . ? S1 Pd1 P1 C16 80.48(12) . . . . ? N1 Pd1 O1 C1 6.5(3) . . . . ? P1 Pd1 O1 C1 -169.6(3) . . . . ? O1 Pd1 N1 C7 -6.2(3) . . . . ? S1 Pd1 N1 C7 176.5(3) . . . . ? O1 Pd1 N1 N2 175.7(2) . . . . ? S1 Pd1 N1 N2 -1.7(2) . . . . ? C7 N1 N2 C8 -177.6(3) . . . . ? Pd1 N1 N2 C8 0.7(4) . . . . ? Pd1 O1 C1 C2 177.4(2) . . . . ? Pd1 O1 C1 C6 -3.0(5) . . . . ? O1 C1 C2 C3 -176.5(3) . . . . ? C6 C1 C2 C3 3.9(6) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? C1 C2 C3 C9 -179.3(4) . . . . ? C2 C3 C4 C5 -3.7(6) . . . . ? C9 C3 C4 C5 176.2(4) . . . . ? C2 C3 C4 Cl1 176.0(3) . . . . ? C9 C3 C4 Cl1 -4.0(5) . . . . ? C3 C4 C5 C6 2.2(6) . . . . ? Cl1 C4 C5 C6 -177.6(3) . . . . ? O1 C1 C6 C5 175.2(3) . . . . ? C2 C1 C6 C5 -5.3(5) . . . . ? O1 C1 C6 C7 -3.5(6) . . . . ? C2 C1 C6 C7 176.0(3) . . . . ? C4 C5 C6 C1 2.5(6) . . . . ? C4 C5 C6 C7 -178.7(3) . . . . ? N2 N1 C7 C6 -179.3(3) . . . . ? Pd1 N1 C7 C6 2.4(5) . . . . ? C1 C6 C7 N1 3.8(6) . . . . ? C5 C6 C7 N1 -174.9(3) . . . . ? N1 N2 C8 N3 179.2(3) . . . . ? N1 N2 C8 S1 1.3(4) . . . . ? Pd1 S1 C8 N2 -2.3(3) . . . . ? Pd1 S1 C8 N3 179.8(2) . . . . ? C22 P1 C10 C11 77.8(3) . . . . ? C16 P1 C10 C11 -170.8(3) . . . . ? Pd1 P1 C10 C11 -45.9(3) . . . . ? C22 P1 C10 C15 -102.7(3) . . . . ? C16 P1 C10 C15 8.7(3) . . . . ? Pd1 P1 C10 C15 133.6(3) . . . . ? C15 C10 C11 C12 2.0(5) . . . . ? P1 C10 C11 C12 -178.4(3) . . . . ? C10 C11 C12 C13 -1.4(6) . . . . ? C11 C12 C13 C14 -0.7(7) . . . . ? C12 C13 C14 C15 2.0(7) . . . . ? C13 C14 C15 C10 -1.3(7) . . . . ? C11 C10 C15 C14 -0.7(6) . . . . ? P1 C10 C15 C14 179.8(3) . . . . ? C22 P1 C16 C21 18.8(3) . . . . ? C10 P1 C16 C21 -92.4(3) . . . . ? Pd1 P1 C16 C21 143.0(3) . . . . ? C22 P1 C16 C17 -162.2(3) . . . . ? C10 P1 C16 C17 86.6(3) . . . . ? Pd1 P1 C16 C17 -38.0(3) . . . . ? C21 C16 C17 C18 0.5(5) . . . . ? P1 C16 C17 C18 -178.5(3) . . . . ? C16 C17 C18 C19 -0.9(6) . . . . ? C17 C18 C19 C20 0.2(7) . . . . ? C18 C19 C20 C21 0.8(7) . . . . ? C17 C16 C21 C20 0.4(5) . . . . ? P1 C16 C21 C20 179.4(3) . . . . ? C19 C20 C21 C16 -1.1(6) . . . . ? C10 P1 C22 C27 173.7(2) . . . . ? C16 P1 C22 C27 63.2(3) . . . . ? Pd1 P1 C22 C27 -62.0(3) . . . . ? C10 P1 C22 C23 -10.7(3) . . . . ? C16 P1 C22 C23 -121.3(3) . . . . ? Pd1 P1 C22 C23 113.6(3) . . . . ? C27 C22 C23 C24 0.9(5) . . . . ? P1 C22 C23 C24 -174.6(3) . . . . ? C22 C23 C24 C25 0.1(6) . . . . ? C23 C24 C25 C26 -1.1(6) . . . . ? C24 C25 C26 C27 1.1(6) . . . . ? C25 C26 C27 C22 -0.1(5) . . . . ? C23 C22 C27 C26 -0.9(5) . . . . ? P1 C22 C27 C26 174.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.403 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.071 data_r18310 _database_code_depnum_ccdc_archive 'CCDC 794256' #TrackingRef 'R18310.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H50 As2 Cl2 N6 O3 Pd2 S2' _chemical_formula_weight 1340.67 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4072(3) _cell_length_b 16.1292(6) _cell_length_c 20.8979(7) _cell_angle_alpha 80.612(2) _cell_angle_beta 88.340(2) _cell_angle_gamma 87.390(2) _cell_volume 2792.26(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4627 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 20.98 _exptl_crystal_description Plate _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas no _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 2.038 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7620 _exptl_absorpt_correction_T_max 0.8875 _exptl_absorpt_process_details 'sadabs v2008/1' _exptl_special_details ; All H atoms were added in their calculated positions and were treated using appropriate riding models. ; _diffrn_ambient_temperature 296(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 47938 _diffrn_reflns_av_R_equivalents 0.1068 _diffrn_reflns_av_sigmaI/netI 0.1256 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.41 _reflns_number_total 11265 _reflns_number_gt 5958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Shelx restraints used: DFIX 1.500 0.005 C1S O3 C1S' O3' DELU O3 > C1s' SIMU O3 > C1s' ; _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^)+(0.0640P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11265 _refine_ls_number_parameters 656 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1425 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 1.04805(7) 0.04172(4) 0.36039(3) 0.03585(17) Uani 1 1 d . . . Pd2 Pd 0.47147(7) 0.54657(4) 0.86829(3) 0.03692(17) Uani 1 1 d . . . As1 As 0.92551(9) 0.02248(5) 0.26253(4) 0.0393(2) Uani 1 1 d . . . As2 As 0.61345(9) 0.53041(5) 0.77070(4) 0.0383(2) Uani 1 1 d . . . S1 S 1.2823(2) -0.01847(14) 0.33639(10) 0.0507(6) Uani 1 1 d . . . S2 S 0.2553(2) 0.48551(15) 0.84038(10) 0.0519(6) Uani 1 1 d . . . Cl1 Cl 0.7069(3) 0.28580(18) 0.59691(14) 0.0914(9) Uani 1 1 d . . . Cl2 Cl 0.6998(4) 0.8020(2) 1.10285(16) 0.1169(12) Uani 1 1 d . . . N1 N 1.1573(7) 0.0596(4) 0.4412(3) 0.0386(15) Uani 1 1 d . . . N2 N 1.3123(7) 0.0291(4) 0.4542(3) 0.0423(16) Uani 1 1 d . . . N3 N 1.5265(7) -0.0398(4) 0.4157(3) 0.0554(19) Uani 1 1 d . . . H3A H 1.5777 -0.0345 0.4498 0.066 Uiso 1 1 calc R . . H3B H 1.5716 -0.0650 0.3864 0.066 Uiso 1 1 calc R . . N4 N 0.3411(7) 0.5646(4) 0.9470(3) 0.0373(15) Uani 1 1 d . . . N5 N 0.1905(7) 0.5326(4) 0.9574(3) 0.0422(16) Uani 1 1 d . . . N6 N 0.0001(8) 0.4619(4) 0.9166(3) 0.059(2) Uani 1 1 d . . . H6A H -0.0603 0.4659 0.9499 0.070 Uiso 1 1 calc R . . H6B H -0.0320 0.4367 0.8864 0.070 Uiso 1 1 calc R . . O1 O 0.8376(6) 0.0882(4) 0.3886(3) 0.0539(15) Uani 1 1 d . . . O2 O 0.6662(6) 0.5937(4) 0.8994(3) 0.0544(15) Uani 1 1 d . . . C1 C 0.6261(10) 0.2168(5) 0.4926(4) 0.054(2) Uani 1 1 d . . . C2 C 0.6627(9) 0.1688(5) 0.4444(4) 0.051(2) Uani 1 1 d . . . H2 H 0.5840 0.1607 0.4160 0.061 Uiso 1 1 calc R . . C3 C 0.8165(9) 0.1320(5) 0.4376(4) 0.0391(19) Uani 1 1 d . . . C4 C 0.9345(9) 0.1405(5) 0.4815(3) 0.0384(18) Uani 1 1 d . . . C5 C 0.8934(10) 0.1905(5) 0.5294(4) 0.049(2) Uani 1 1 d . . . H5 H 0.9706 0.1994 0.5582 0.059 Uiso 1 1 calc R . . C6 C 0.7467(11) 0.2256(5) 0.5349(4) 0.055(2) Uani 1 1 d . . . C7 C 0.4598(10) 0.2542(6) 0.4977(4) 0.074(3) Uani 1 1 d . . . H7A H 0.4605 0.3140 0.4841 0.111 Uiso 1 1 calc R . . H7B H 0.4219 0.2423 0.5419 0.111 Uiso 1 1 calc R . . H7C H 0.3910 0.2301 0.4704 0.111 Uiso 1 1 calc R . . C8 C 1.0914(9) 0.1032(5) 0.4834(3) 0.0386(18) Uani 1 1 d . . . H8 H 1.1534 0.1107 0.5180 0.046 Uiso 1 1 calc R . . C9 C 1.3759(8) -0.0086(5) 0.4084(4) 0.042(2) Uani 1 1 d . . . C10 C 0.7629(10) 0.1066(5) 0.2295(4) 0.045(2) Uani 1 1 d . . . C11 C 0.7738(11) 0.1515(6) 0.1669(5) 0.068(3) Uani 1 1 d . . . H11 H 0.8602 0.1418 0.1399 0.082 Uiso 1 1 calc R . . C12 C 0.6555(15) 0.2105(7) 0.1453(6) 0.095(4) Uani 1 1 d . . . H12 H 0.6619 0.2404 0.1034 0.113 Uiso 1 1 calc R . . C13 C 0.5285(14) 0.2256(6) 0.1850(6) 0.082(3) Uani 1 1 d . . . H13 H 0.4506 0.2663 0.1700 0.099 Uiso 1 1 calc R . . C14 C 0.5154(11) 0.1812(6) 0.2463(5) 0.071(3) Uani 1 1 d . . . H14 H 0.4281 0.1911 0.2727 0.085 Uiso 1 1 calc R . . C15 C 0.6322(10) 0.1214(5) 0.2689(4) 0.060(2) Uani 1 1 d . . . H15 H 0.6233 0.0911 0.3106 0.072 Uiso 1 1 calc R . . C16 C 1.0617(10) 0.0157(5) 0.1877(4) 0.048(2) Uani 1 1 d . . . C17 C 1.1920(12) 0.0646(7) 0.1772(5) 0.077(3) Uani 1 1 d . . . H17 H 1.2160 0.0992 0.2068 0.093 Uiso 1 1 calc R . . C18 C 1.2891(14) 0.0622(9) 0.1217(6) 0.118(5) Uani 1 1 d . . . H18 H 1.3776 0.0954 0.1148 0.141 Uiso 1 1 calc R . . C19 C 1.2560(15) 0.0128(9) 0.0783(5) 0.110(5) Uani 1 1 d . . . H19 H 1.3229 0.0106 0.0423 0.132 Uiso 1 1 calc R . . C20 C 1.1236(16) -0.0342(8) 0.0873(5) 0.105(4) Uani 1 1 d . . . H20 H 1.0978 -0.0663 0.0562 0.126 Uiso 1 1 calc R . . C21 C 1.0268(13) -0.0343(6) 0.1426(5) 0.076(3) Uani 1 1 d . . . H21 H 0.9390 -0.0680 0.1491 0.091 Uiso 1 1 calc R . . C22 C 0.8867(12) -0.1502(6) 0.3129(4) 0.062(3) Uani 1 1 d . . . H22 H 0.9887 -0.1465 0.3280 0.074 Uiso 1 1 calc R . . C23 C 0.8119(10) -0.0813(5) 0.2766(4) 0.045(2) Uani 1 1 d . . . C24 C 0.6627(10) -0.0877(6) 0.2536(5) 0.062(3) Uani 1 1 d . . . H24 H 0.6128 -0.0420 0.2279 0.074 Uiso 1 1 calc R . . C25 C 0.5868(13) -0.1634(8) 0.2692(6) 0.087(3) Uani 1 1 d . . . H25 H 0.4849 -0.1681 0.2544 0.104 Uiso 1 1 calc R . . C26 C 0.6610(16) -0.2304(8) 0.3060(6) 0.089(4) Uani 1 1 d . . . H26 H 0.6088 -0.2805 0.3169 0.106 Uiso 1 1 calc R . . C27 C 0.8091(17) -0.2248(7) 0.3267(5) 0.090(4) Uani 1 1 d . . . H27 H 0.8600 -0.2717 0.3507 0.107 Uiso 1 1 calc R . . C28 C 0.6649(9) 0.6379(5) 0.9466(4) 0.0426(19) Uani 1 1 d . . . C29 C 0.8078(10) 0.6779(6) 0.9556(4) 0.058(2) Uani 1 1 d . . . H29 H 0.8956 0.6694 0.9290 0.070 Uiso 1 1 calc R . . C30 C 0.8228(11) 0.7296(6) 1.0027(5) 0.060(2) Uani 1 1 d . . . C31 C 0.6918(12) 0.7380(6) 1.0423(4) 0.064(3) Uani 1 1 d . . . C32 C 0.5534(10) 0.6999(5) 1.0373(4) 0.054(2) Uani 1 1 d . . . H32 H 0.4685 0.7086 1.0654 0.065 Uiso 1 1 calc R . . C33 C 0.5355(9) 0.6469(5) 0.9900(3) 0.0424(19) Uani 1 1 d . . . C34 C 0.9786(13) 0.7704(7) 1.0086(5) 0.104(4) Uani 1 1 d . . . H34A H 0.9607 0.8303 1.0036 0.156 Uiso 1 1 calc R . . H34B H 1.0522 0.7569 0.9755 0.156 Uiso 1 1 calc R . . H34C H 1.0219 0.7501 1.0505 0.156 Uiso 1 1 calc R . . C35 C 0.3884(9) 0.6080(5) 0.9897(4) 0.046(2) Uani 1 1 d . . . H35 H 0.3175 0.6141 1.0237 0.055 Uiso 1 1 calc R . . C36 C 0.1436(9) 0.4947(5) 0.9116(4) 0.044(2) Uani 1 1 d . . . C37 C 0.7685(8) 0.6146(5) 0.7403(4) 0.0399(19) Uani 1 1 d . . . C38 C 0.7640(11) 0.6591(6) 0.6779(5) 0.069(3) Uani 1 1 d . . . H38 H 0.6873 0.6493 0.6491 0.082 Uiso 1 1 calc R . . C39 C 0.8790(13) 0.7195(6) 0.6593(5) 0.082(3) Uani 1 1 d . . . H39 H 0.8771 0.7507 0.6177 0.098 Uiso 1 1 calc R . . C40 C 0.9914(12) 0.7332(6) 0.7000(6) 0.077(3) Uani 1 1 d . . . H40 H 1.0645 0.7744 0.6867 0.092 Uiso 1 1 calc R . . C41 C 1.0001(11) 0.6864(6) 0.7620(5) 0.065(3) Uani 1 1 d . . . H41 H 1.0820 0.6936 0.7893 0.078 Uiso 1 1 calc R . . C42 C 0.8847(10) 0.6292(6) 0.7822(4) 0.059(2) Uani 1 1 d . . . H42 H 0.8850 0.6001 0.8244 0.071 Uiso 1 1 calc R . . C43 C 0.4893(6) 0.5303(4) 0.6948(2) 0.043(2) Uani 1 1 d G . . C44 C 0.3665(7) 0.5909(3) 0.6819(3) 0.060(2) Uani 1 1 d G . . H44 H 0.3391 0.6261 0.7119 0.072 Uiso 1 1 calc R . . C45 C 0.2848(6) 0.5988(4) 0.6242(3) 0.087(3) Uani 1 1 d G . . H45 H 0.2026 0.6393 0.6156 0.104 Uiso 1 1 calc R . . C46 C 0.3257(8) 0.5461(5) 0.5794(2) 0.089(4) Uani 1 1 d G . . H46 H 0.2710 0.5514 0.5408 0.107 Uiso 1 1 calc R . . C47 C 0.4485(8) 0.4855(4) 0.5923(3) 0.093(4) Uani 1 1 d G . . H47 H 0.4759 0.4502 0.5623 0.111 Uiso 1 1 calc R . . C48 C 0.5303(6) 0.4775(3) 0.6500(3) 0.064(3) Uani 1 1 d G . . H48 H 0.6124 0.4370 0.6586 0.077 Uiso 1 1 calc R . . C49 C 0.6590(11) 0.3525(5) 0.8037(4) 0.056(2) Uani 1 1 d . . . H49 H 0.5511 0.3551 0.8148 0.067 Uiso 1 1 calc R . . C50 C 0.7356(9) 0.4250(5) 0.7781(4) 0.0424(19) Uani 1 1 d . . . C51 C 0.8952(10) 0.4203(5) 0.7633(4) 0.056(2) Uani 1 1 d . . . H51 H 0.9471 0.4689 0.7460 0.068 Uiso 1 1 calc R . . C52 C 0.9801(12) 0.3436(7) 0.7737(6) 0.082(3) Uani 1 1 d . . . H52 H 1.0886 0.3408 0.7639 0.098 Uiso 1 1 calc R . . C53 C 0.9033(15) 0.2725(7) 0.7985(5) 0.087(4) Uani 1 1 d . . . H53 H 0.9597 0.2210 0.8058 0.104 Uiso 1 1 calc R . . C54 C 0.7431(14) 0.2765(6) 0.8128(5) 0.079(3) Uani 1 1 d . . . H54 H 0.6910 0.2274 0.8286 0.094 Uiso 1 1 calc R . . O3 O 0.093(3) 0.3823(19) 0.519(2) 0.197(12) Uani 0.50 1 d PDU A 1 H3 H 0.1691 0.3852 0.5419 0.295 Uiso 0.50 1 calc PR A 1 C1S C 0.099(5) 0.451(3) 0.4611(17) 0.187(16) Uani 0.50 1 d PDU A 1 H1S1 H 0.0911 0.5044 0.4753 0.280 Uiso 0.50 1 calc PR A 1 H1S2 H 0.0115 0.4461 0.4334 0.280 Uiso 0.50 1 calc PR A 1 H1S3 H 0.1974 0.4453 0.4376 0.280 Uiso 0.50 1 calc PR A 1 C1S' C 0.038(5) 0.538(3) 0.4300(17) 0.20(2) Uani 0.50 1 d PDU B -2 H1S4 H -0.0481 0.5274 0.4034 0.306 Uiso 0.50 1 calc PR B -2 H1S5 H 0.1371 0.5207 0.4114 0.306 Uiso 0.50 1 calc PR B -2 H1S6 H 0.0377 0.5968 0.4323 0.306 Uiso 0.50 1 calc PR B -2 O3' O 0.016(5) 0.489(3) 0.4972(17) 0.204(14) Uani 0.50 1 d PRD B -2 H3' H 0.0062 0.4389 0.4948 0.305 Uiso 0.50 1 calc PR 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 0.0343(3) 0.0400(4) 0.0327(3) -0.0038(3) -0.0052(2) -0.0006(3) Pd2 0.0368(3) 0.0426(4) 0.0306(3) -0.0045(3) 0.0039(2) -0.0009(3) As1 0.0423(5) 0.0403(5) 0.0352(5) -0.0049(4) -0.0080(4) -0.0005(4) As2 0.0400(5) 0.0413(5) 0.0331(4) -0.0058(4) 0.0054(3) -0.0025(4) S1 0.0412(12) 0.0692(16) 0.0420(12) -0.0128(11) -0.0056(9) 0.0109(11) S2 0.0443(12) 0.0726(16) 0.0425(12) -0.0183(11) 0.0082(10) -0.0145(11) Cl1 0.098(2) 0.100(2) 0.0850(19) -0.0490(17) 0.0169(15) 0.0144(17) Cl2 0.127(3) 0.145(3) 0.103(2) -0.082(2) 0.0027(19) -0.039(2) N1 0.034(4) 0.046(4) 0.034(4) 0.001(3) -0.006(3) -0.004(3) N2 0.034(4) 0.052(4) 0.040(4) -0.005(3) -0.008(3) 0.003(3) N3 0.040(4) 0.077(5) 0.048(4) -0.008(4) -0.012(3) 0.006(4) N4 0.037(4) 0.040(4) 0.033(4) 0.002(3) -0.002(3) -0.003(3) N5 0.041(4) 0.049(4) 0.035(4) -0.003(3) 0.004(3) -0.005(3) N6 0.045(4) 0.089(6) 0.044(4) -0.017(4) 0.003(3) -0.013(4) O1 0.029(3) 0.077(4) 0.058(4) -0.016(3) -0.010(3) 0.003(3) O2 0.036(3) 0.080(4) 0.052(4) -0.024(3) 0.005(3) -0.009(3) C1 0.057(6) 0.048(6) 0.050(5) 0.006(4) 0.008(4) 0.011(4) C2 0.040(5) 0.061(6) 0.051(5) -0.005(5) 0.000(4) -0.004(4) C3 0.044(5) 0.035(5) 0.036(5) 0.000(4) 0.005(4) 0.003(4) C4 0.037(4) 0.041(5) 0.035(4) 0.000(4) 0.006(3) -0.001(4) C5 0.051(5) 0.056(6) 0.038(5) -0.006(4) 0.000(4) 0.003(4) C6 0.064(6) 0.054(6) 0.047(5) -0.013(4) 0.012(5) -0.001(5) C7 0.066(6) 0.088(8) 0.066(7) -0.013(6) 0.010(5) 0.027(6) C8 0.049(5) 0.043(5) 0.026(4) -0.012(4) -0.008(3) -0.006(4) C9 0.027(4) 0.055(5) 0.042(5) 0.004(4) -0.002(3) -0.001(4) C10 0.054(5) 0.026(4) 0.056(5) -0.002(4) -0.024(4) -0.002(4) C11 0.067(6) 0.062(7) 0.068(7) 0.013(5) -0.013(5) 0.000(5) C12 0.104(9) 0.080(8) 0.084(9) 0.032(7) -0.026(8) 0.011(7) C13 0.091(9) 0.049(7) 0.103(10) 0.000(6) -0.036(7) 0.008(6) C14 0.059(6) 0.069(7) 0.087(8) -0.020(6) -0.023(6) 0.014(5) C15 0.058(6) 0.062(6) 0.057(6) -0.002(5) -0.014(5) 0.014(5) C16 0.057(6) 0.046(5) 0.042(5) -0.005(4) -0.002(4) -0.004(4) C17 0.081(7) 0.097(8) 0.057(7) -0.018(6) 0.004(5) -0.031(6) C18 0.097(9) 0.189(15) 0.075(9) -0.034(9) 0.035(7) -0.067(9) C19 0.107(10) 0.175(14) 0.056(7) -0.040(8) 0.042(7) -0.040(10) C20 0.145(12) 0.110(10) 0.072(8) -0.045(7) 0.041(8) -0.041(9) C21 0.109(9) 0.059(7) 0.064(7) -0.016(5) 0.025(6) -0.031(6) C22 0.086(7) 0.044(6) 0.056(6) -0.005(5) -0.015(5) -0.005(5) C23 0.053(5) 0.038(5) 0.047(5) -0.014(4) 0.002(4) -0.002(4) C24 0.053(6) 0.053(6) 0.082(7) -0.019(5) -0.001(5) -0.006(5) C25 0.061(7) 0.090(9) 0.119(10) -0.046(8) 0.010(7) -0.017(7) C26 0.105(10) 0.068(8) 0.102(10) -0.041(7) 0.051(8) -0.037(8) C27 0.143(12) 0.046(7) 0.080(8) -0.009(6) 0.004(8) -0.010(7) C28 0.048(5) 0.045(5) 0.032(4) 0.002(4) -0.003(4) -0.002(4) C29 0.057(6) 0.069(6) 0.050(6) -0.009(5) -0.002(4) -0.013(5) C30 0.065(6) 0.053(6) 0.063(6) -0.004(5) -0.003(5) -0.018(5) C31 0.085(7) 0.061(6) 0.050(6) -0.018(5) -0.006(5) -0.016(6) C32 0.062(6) 0.066(6) 0.035(5) -0.012(4) 0.002(4) -0.003(5) C33 0.048(5) 0.044(5) 0.033(4) 0.003(4) -0.005(4) -0.002(4) C34 0.109(9) 0.120(10) 0.087(9) -0.018(7) -0.017(7) -0.056(8) C35 0.047(5) 0.061(6) 0.030(4) -0.007(4) 0.007(4) 0.006(4) C36 0.043(5) 0.060(6) 0.027(4) 0.000(4) 0.005(3) -0.007(4) C37 0.035(4) 0.037(5) 0.045(5) -0.002(4) 0.016(4) -0.003(3) C38 0.074(7) 0.061(7) 0.065(7) 0.004(5) 0.005(5) 0.002(5) C39 0.089(8) 0.068(7) 0.076(8) 0.028(6) 0.015(6) -0.015(6) C40 0.071(7) 0.043(6) 0.114(10) -0.004(6) 0.013(7) -0.015(5) C41 0.063(6) 0.058(6) 0.077(7) -0.018(6) 0.017(5) -0.021(5) C42 0.061(6) 0.074(7) 0.041(5) -0.003(5) 0.001(4) -0.025(5) C43 0.034(4) 0.059(6) 0.035(5) -0.001(4) 0.003(3) -0.003(4) C44 0.057(6) 0.079(7) 0.043(5) -0.019(5) -0.002(4) 0.019(5) C45 0.074(7) 0.104(9) 0.075(8) -0.001(7) -0.022(6) 0.031(6) C46 0.090(8) 0.127(10) 0.053(6) -0.018(7) -0.030(6) 0.015(7) C47 0.106(9) 0.119(10) 0.064(7) -0.047(7) -0.036(6) 0.027(8) C48 0.083(7) 0.063(6) 0.051(6) -0.019(5) -0.022(5) 0.011(5) C49 0.067(6) 0.035(5) 0.062(6) -0.003(4) 0.004(5) 0.004(4) C50 0.050(5) 0.039(5) 0.038(5) -0.008(4) 0.001(4) 0.005(4) C51 0.057(6) 0.041(5) 0.072(6) -0.015(5) 0.005(5) 0.002(4) C52 0.060(7) 0.072(8) 0.120(10) -0.039(7) -0.014(6) 0.020(6) C53 0.104(10) 0.059(8) 0.099(9) -0.023(7) -0.021(8) 0.029(7) C54 0.112(10) 0.049(7) 0.073(7) -0.006(5) -0.006(7) 0.001(6) O3 0.13(2) 0.17(3) 0.29(4) -0.06(2) 0.00(2) -0.024(19) C1S 0.15(3) 0.26(5) 0.17(4) -0.10(2) 0.03(3) -0.06(4) C1S' 0.19(4) 0.28(5) 0.12(3) 0.08(3) -0.04(3) -0.14(4) O3' 0.10(2) 0.33(4) 0.22(2) -0.16(3) 0.028(18) -0.09(2) _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 O1 2.000(5) . ? Pd1 N1 2.013(6) . ? Pd1 S1 2.236(2) . ? Pd1 As1 2.3871(9) . ? Pd2 O2 2.004(5) . ? Pd2 N4 2.004(6) . ? Pd2 S2 2.242(2) . ? Pd2 As2 2.3784(9) . ? As1 C16 1.927(8) . ? As1 C10 1.941(7) . ? As1 C23 1.941(8) . ? As2 C43 1.924(4) . ? As2 C50 1.932(7) . ? As2 C37 1.944(7) . ? S1 C9 1.752(8) . ? S2 C36 1.760(8) . ? Cl1 C6 1.758(8) . ? Cl2 C31 1.764(9) . ? N1 C8 1.310(8) . ? N1 N2 1.390(7) . ? N2 C9 1.304(9) . ? N3 C9 1.344(8) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 C35 1.300(9) . ? N4 N5 1.387(8) . ? N5 C36 1.295(9) . ? N6 C36 1.334(9) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? O1 C3 1.338(8) . ? O2 C28 1.309(9) . ? C1 C2 1.387(11) . ? C1 C6 1.391(11) . ? C1 C7 1.505(11) . ? C2 C3 1.412(10) . ? C2 H2 0.9300 . ? C3 C4 1.397(10) . ? C4 C5 1.411(10) . ? C4 C8 1.423(10) . ? C5 C6 1.343(10) . ? C5 H5 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8 0.9300 . ? C10 C15 1.389(11) . ? C10 C11 1.391(11) . ? C11 C12 1.378(13) . ? C11 H11 0.9300 . ? C12 C13 1.369(14) . ? C12 H12 0.9300 . ? C13 C14 1.366(13) . ? C13 H13 0.9300 . ? C14 C15 1.381(11) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.370(11) . ? C16 C21 1.382(11) . ? C17 C18 1.405(13) . ? C17 H17 0.9300 . ? C18 C19 1.344(15) . ? C18 H18 0.9300 . ? C19 C20 1.367(15) . ? C19 H19 0.9300 . ? C20 C21 1.394(13) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.376(11) . ? C22 C27 1.380(13) . ? C22 H22 0.9300 . ? C23 C24 1.371(11) . ? C24 C25 1.390(13) . ? C24 H24 0.9300 . ? C25 C26 1.358(15) . ? C25 H25 0.9300 . ? C26 C27 1.342(15) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.414(10) . ? C28 C29 1.421(11) . ? C29 C30 1.401(11) . ? C29 H29 0.9300 . ? C30 C31 1.374(12) . ? C30 C34 1.510(12) . ? C31 C32 1.354(12) . ? C32 C33 1.424(11) . ? C32 H32 0.9300 . ? C33 C35 1.413(10) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35 0.9300 . ? C37 C42 1.383(10) . ? C37 C38 1.383(11) . ? C38 C39 1.407(12) . ? C38 H38 0.9300 . ? C39 C40 1.339(13) . ? C39 H39 0.9300 . ? C40 C41 1.390(13) . ? C40 H40 0.9300 . ? C41 C42 1.379(11) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 C46 1.3900 . ? C45 H45 0.9300 . ? C46 C47 1.3900 . ? C46 H46 0.9300 . ? C47 C48 1.3900 . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C54 1.375(11) . ? C49 C50 1.383(10) . ? C49 H49 0.9300 . ? C50 C51 1.370(10) . ? C51 C52 1.388(12) . ? C51 H51 0.9300 . ? C52 C53 1.362(14) . ? C52 H52 0.9300 . ? C53 C54 1.372(14) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? O3 C1S 1.499(5) . ? O3 H3 0.8200 . ? C1S H1S1 0.9600 . ? C1S H1S2 0.9600 . ? C1S H1S3 0.9600 . ? C1S' O3' 1.5071 . ? C1S' H1S4 0.9600 . ? C1S' H1S5 0.9600 . ? C1S' H1S6 0.9600 . ? O3' H3' 0.8200 . ? 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 O1 Pd1 N1 93.4(2) . . ? O1 Pd1 S1 175.17(17) . . ? N1 Pd1 S1 84.14(18) . . ? O1 Pd1 As1 87.82(15) . . ? N1 Pd1 As1 178.17(17) . . ? S1 Pd1 As1 94.69(6) . . ? O2 Pd2 N4 93.3(2) . . ? O2 Pd2 S2 175.39(17) . . ? N4 Pd2 S2 84.74(18) . . ? O2 Pd2 As2 88.80(15) . . ? N4 Pd2 As2 176.31(16) . . ? S2 Pd2 As2 93.39(6) . . ? C16 As1 C10 103.2(4) . . ? C16 As1 C23 105.2(3) . . ? C10 As1 C23 103.2(3) . . ? C16 As1 Pd1 117.7(2) . . ? C10 As1 Pd1 116.1(2) . . ? C23 As1 Pd1 110.0(2) . . ? C43 As2 C50 103.1(3) . . ? C43 As2 C37 102.5(3) . . ? C50 As2 C37 104.0(3) . . ? C43 As2 Pd2 117.00(16) . . ? C50 As2 Pd2 112.4(2) . . ? C37 As2 Pd2 116.1(2) . . ? C9 S1 Pd1 96.5(3) . . ? C36 S2 Pd2 95.9(3) . . ? C8 N1 N2 115.6(6) . . ? C8 N1 Pd1 123.0(5) . . ? N2 N1 Pd1 121.4(5) . . ? C9 N2 N1 113.0(6) . . ? C9 N3 H3A 120.0 . . ? C9 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C35 N4 N5 116.4(6) . . ? C35 N4 Pd2 123.1(5) . . ? N5 N4 Pd2 120.4(5) . . ? C36 N5 N4 114.4(6) . . ? C36 N6 H6A 120.0 . . ? C36 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C3 O1 Pd1 124.6(5) . . ? C28 O2 Pd2 123.9(5) . . ? C2 C1 C6 117.1(8) . . ? C2 C1 C7 119.2(8) . . ? C6 C1 C7 123.7(8) . . ? C1 C2 C3 121.6(8) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? O1 C3 C4 123.9(7) . . ? O1 C3 C2 116.0(7) . . ? C4 C3 C2 120.1(7) . . ? C3 C4 C5 116.6(7) . . ? C3 C4 C8 126.8(7) . . ? C5 C4 C8 116.5(7) . . ? C6 C5 C4 122.4(8) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C1 122.2(8) . . ? C5 C6 Cl1 118.8(7) . . ? C1 C6 Cl1 119.0(7) . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C4 126.5(7) . . ? N1 C8 H8 116.7 . . ? C4 C8 H8 116.7 . . ? N2 C9 N3 117.9(7) . . ? N2 C9 S1 124.9(6) . . ? N3 C9 S1 117.2(6) . . ? C15 C10 C11 119.4(8) . . ? C15 C10 As1 119.4(6) . . ? C11 C10 As1 121.2(7) . . ? C12 C11 C10 119.3(10) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C13 C12 C11 120.7(10) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C12 120.5(10) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 119.8(10) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C10 120.2(9) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? C17 C16 C21 119.2(8) . . ? C17 C16 As1 119.2(7) . . ? C21 C16 As1 121.5(7) . . ? C16 C17 C18 119.7(10) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 121.0(11) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 119.7(10) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C21 120.5(11) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C16 C21 C20 119.8(10) . . ? C16 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C27 119.5(10) . . ? C23 C22 H22 120.3 . . ? C27 C22 H22 120.3 . . ? C24 C23 C22 119.9(8) . . ? C24 C23 As1 123.2(7) . . ? C22 C23 As1 116.9(7) . . ? C23 C24 C25 119.2(9) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C26 C25 C24 120.2(11) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 120.5(11) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C22 120.7(11) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? O2 C28 C33 125.5(7) . . ? O2 C28 C29 116.6(7) . . ? C33 C28 C29 117.9(8) . . ? C30 C29 C28 123.1(8) . . ? C30 C29 H29 118.4 . . ? C28 C29 H29 118.4 . . ? C31 C30 C29 116.3(8) . . ? C31 C30 C34 123.9(9) . . ? C29 C30 C34 119.8(9) . . ? C32 C31 C30 123.5(9) . . ? C32 C31 Cl2 117.0(8) . . ? C30 C31 Cl2 119.4(8) . . ? C31 C32 C33 121.2(8) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C35 C33 C28 125.0(7) . . ? C35 C33 C32 117.2(7) . . ? C28 C33 C32 117.8(8) . . ? C30 C34 H34A 109.5 . . ? C30 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C30 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N4 C35 C33 127.3(7) . . ? N4 C35 H35 116.4 . . ? C33 C35 H35 116.4 . . ? N5 C36 N6 119.4(7) . . ? N5 C36 S2 124.3(6) . . ? N6 C36 S2 116.3(6) . . ? C42 C37 C38 120.2(8) . . ? C42 C37 As2 118.8(6) . . ? C38 C37 As2 120.9(7) . . ? C37 C38 C39 117.9(9) . . ? C37 C38 H38 121.1 . . ? C39 C38 H38 121.1 . . ? C40 C39 C38 121.5(10) . . ? C40 C39 H39 119.2 . . ? C38 C39 H39 119.2 . . ? C39 C40 C41 120.8(10) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 118.6(10) . . ? C42 C41 H41 120.7 . . ? C40 C41 H41 120.7 . . ? C41 C42 C37 120.8(8) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? C44 C43 C48 120.0 . . ? C44 C43 As2 118.1(3) . . ? C48 C43 As2 121.6(3) . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C47 C46 C45 120.0 . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C54 C49 C50 119.7(9) . . ? C54 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C51 C50 C49 119.4(7) . . ? C51 C50 As2 122.7(6) . . ? C49 C50 As2 117.7(6) . . ? C50 C51 C52 120.6(9) . . ? C50 C51 H51 119.7 . . ? C52 C51 H51 119.7 . . ? C53 C52 C51 119.5(10) . . ? C53 C52 H52 120.3 . . ? C51 C52 H52 120.3 . . ? C52 C53 C54 120.3(10) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C53 C54 C49 120.4(10) . . ? C53 C54 H54 119.8 . . ? C49 C54 H54 119.8 . . ? O3' C1S' H1S4 109.5 . . ? O3' C1S' H1S5 109.5 . . ? H1S4 C1S' H1S5 109.5 . . ? O3' C1S' H1S6 109.5 . . ? H1S4 C1S' H1S6 109.5 . . ? H1S5 C1S' H1S6 109.5 . . ? C1S' O3' H3' 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pd1 As1 C16 157.6(3) . . . . ? S1 Pd1 As1 C16 -26.6(3) . . . . ? O1 Pd1 As1 C10 34.6(3) . . . . ? S1 Pd1 As1 C10 -149.5(3) . . . . ? O1 Pd1 As1 C23 -82.1(3) . . . . ? S1 Pd1 As1 C23 93.8(3) . . . . ? O2 Pd2 As2 C43 -154.7(3) . . . . ? S2 Pd2 As2 C43 29.4(2) . . . . ? O2 Pd2 As2 C50 86.2(3) . . . . ? S2 Pd2 As2 C50 -89.7(3) . . . . ? O2 Pd2 As2 C37 -33.3(3) . . . . ? S2 Pd2 As2 C37 150.7(3) . . . . ? N1 Pd1 S1 C9 3.0(3) . . . . ? As1 Pd1 S1 C9 -178.4(3) . . . . ? N4 Pd2 S2 C36 -3.5(3) . . . . ? As2 Pd2 S2 C36 179.7(3) . . . . ? O1 Pd1 N1 C8 -10.6(6) . . . . ? S1 Pd1 N1 C8 173.6(6) . . . . ? O1 Pd1 N1 N2 172.5(5) . . . . ? S1 Pd1 N1 N2 -3.3(5) . . . . ? C8 N1 N2 C9 -175.4(7) . . . . ? Pd1 N1 N2 C9 1.7(8) . . . . ? O2 Pd2 N4 C35 10.3(6) . . . . ? S2 Pd2 N4 C35 -173.8(6) . . . . ? O2 Pd2 N4 N5 -171.7(5) . . . . ? S2 Pd2 N4 N5 4.1(5) . . . . ? C35 N4 N5 C36 175.5(7) . . . . ? Pd2 N4 N5 C36 -2.6(8) . . . . ? N1 Pd1 O1 C3 13.8(6) . . . . ? As1 Pd1 O1 C3 -164.9(6) . . . . ? N4 Pd2 O2 C28 -15.1(6) . . . . ? As2 Pd2 O2 C28 161.9(6) . . . . ? C6 C1 C2 C3 -1.4(12) . . . . ? C7 C1 C2 C3 -179.7(7) . . . . ? Pd1 O1 C3 C4 -9.8(10) . . . . ? Pd1 O1 C3 C2 171.9(5) . . . . ? C1 C2 C3 O1 -179.0(7) . . . . ? C1 C2 C3 C4 2.7(12) . . . . ? O1 C3 C4 C5 178.6(7) . . . . ? C2 C3 C4 C5 -3.2(11) . . . . ? O1 C3 C4 C8 -2.1(12) . . . . ? C2 C3 C4 C8 176.1(7) . . . . ? C3 C4 C5 C6 2.8(12) . . . . ? C8 C4 C5 C6 -176.6(8) . . . . ? C4 C5 C6 C1 -1.7(13) . . . . ? C4 C5 C6 Cl1 179.3(6) . . . . ? C2 C1 C6 C5 0.9(13) . . . . ? C7 C1 C6 C5 179.1(8) . . . . ? C2 C1 C6 Cl1 180.0(6) . . . . ? C7 C1 C6 Cl1 -1.8(12) . . . . ? N2 N1 C8 C4 -179.5(7) . . . . ? Pd1 N1 C8 C4 3.5(11) . . . . ? C3 C4 C8 N1 5.6(13) . . . . ? C5 C4 C8 N1 -175.1(7) . . . . ? N1 N2 C9 N3 179.3(6) . . . . ? N1 N2 C9 S1 1.9(10) . . . . ? Pd1 S1 C9 N2 -3.8(7) . . . . ? Pd1 S1 C9 N3 178.8(6) . . . . ? C16 As1 C10 C15 172.8(7) . . . . ? C23 As1 C10 C15 63.5(7) . . . . ? Pd1 As1 C10 C15 -56.9(7) . . . . ? C16 As1 C10 C11 -6.4(8) . . . . ? C23 As1 C10 C11 -115.7(7) . . . . ? Pd1 As1 C10 C11 123.9(6) . . . . ? C15 C10 C11 C12 0.6(14) . . . . ? As1 C10 C11 C12 179.8(8) . . . . ? C10 C11 C12 C13 0.4(16) . . . . ? C11 C12 C13 C14 -1.2(18) . . . . ? C12 C13 C14 C15 0.9(16) . . . . ? C13 C14 C15 C10 0.2(14) . . . . ? C11 C10 C15 C14 -0.9(13) . . . . ? As1 C10 C15 C14 179.9(7) . . . . ? C10 As1 C16 C17 92.8(8) . . . . ? C23 As1 C16 C17 -159.3(8) . . . . ? Pd1 As1 C16 C17 -36.4(8) . . . . ? C10 As1 C16 C21 -84.0(8) . . . . ? C23 As1 C16 C21 23.9(8) . . . . ? Pd1 As1 C16 C21 146.7(7) . . . . ? C21 C16 C17 C18 -1.0(16) . . . . ? As1 C16 C17 C18 -177.9(9) . . . . ? C16 C17 C18 C19 0(2) . . . . ? C17 C18 C19 C20 2(2) . . . . ? C18 C19 C20 C21 -3(2) . . . . ? C17 C16 C21 C20 -0.2(16) . . . . ? As1 C16 C21 C20 176.6(9) . . . . ? C19 C20 C21 C16 2.3(19) . . . . ? C27 C22 C23 C24 -1.1(13) . . . . ? C27 C22 C23 As1 177.4(7) . . . . ? C16 As1 C23 C24 -95.9(7) . . . . ? C10 As1 C23 C24 12.0(8) . . . . ? Pd1 As1 C23 C24 136.5(7) . . . . ? C16 As1 C23 C22 85.6(7) . . . . ? C10 As1 C23 C22 -166.5(7) . . . . ? Pd1 As1 C23 C22 -42.0(7) . . . . ? C22 C23 C24 C25 2.1(13) . . . . ? As1 C23 C24 C25 -176.4(7) . . . . ? C23 C24 C25 C26 -1.0(15) . . . . ? C24 C25 C26 C27 -1.2(17) . . . . ? C25 C26 C27 C22 2.2(17) . . . . ? C23 C22 C27 C26 -1.0(15) . . . . ? Pd2 O2 C28 C33 11.8(11) . . . . ? Pd2 O2 C28 C29 -170.1(5) . . . . ? O2 C28 C29 C30 177.8(8) . . . . ? C33 C28 C29 C30 -4.0(12) . . . . ? C28 C29 C30 C31 2.2(14) . . . . ? C28 C29 C30 C34 -179.4(9) . . . . ? C29 C30 C31 C32 -0.4(15) . . . . ? C34 C30 C31 C32 -178.8(9) . . . . ? C29 C30 C31 Cl2 -179.9(7) . . . . ? C34 C30 C31 Cl2 1.7(14) . . . . ? C30 C31 C32 C33 0.6(15) . . . . ? Cl2 C31 C32 C33 -179.9(6) . . . . ? O2 C28 C33 C35 1.3(13) . . . . ? C29 C28 C33 C35 -176.8(7) . . . . ? O2 C28 C33 C32 -178.0(7) . . . . ? C29 C28 C33 C32 3.9(11) . . . . ? C31 C32 C33 C35 178.2(8) . . . . ? C31 C32 C33 C28 -2.4(12) . . . . ? N5 N4 C35 C33 -180.0(7) . . . . ? Pd2 N4 C35 C33 -2.0(11) . . . . ? C28 C33 C35 N4 -6.9(13) . . . . ? C32 C33 C35 N4 172.4(7) . . . . ? N4 N5 C36 N6 -179.7(7) . . . . ? N4 N5 C36 S2 -1.5(10) . . . . ? Pd2 S2 C36 N5 4.0(7) . . . . ? Pd2 S2 C36 N6 -177.8(6) . . . . ? C43 As2 C37 C42 -177.1(6) . . . . ? C50 As2 C37 C42 -69.9(7) . . . . ? Pd2 As2 C37 C42 54.1(7) . . . . ? C43 As2 C37 C38 2.5(7) . . . . ? C50 As2 C37 C38 109.7(7) . . . . ? Pd2 As2 C37 C38 -126.3(6) . . . . ? C42 C37 C38 C39 -0.9(13) . . . . ? As2 C37 C38 C39 179.5(7) . . . . ? C37 C38 C39 C40 1.0(15) . . . . ? C38 C39 C40 C41 1.4(16) . . . . ? C39 C40 C41 C42 -4.0(15) . . . . ? C40 C41 C42 C37 4.1(14) . . . . ? C38 C37 C42 C41 -1.7(13) . . . . ? As2 C37 C42 C41 177.9(7) . . . . ? C50 As2 C43 C44 168.8(4) . . . . ? C37 As2 C43 C44 -83.3(4) . . . . ? Pd2 As2 C43 C44 44.9(3) . . . . ? C50 As2 C43 C48 -18.0(4) . . . . ? C37 As2 C43 C48 89.8(4) . . . . ? Pd2 As2 C43 C48 -141.9(3) . . . . ? C48 C43 C44 C45 0.0 . . . . ? As2 C43 C44 C45 173.2(4) . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C43 0.0 . . . . ? C44 C43 C48 C47 0.0 . . . . ? As2 C43 C48 C47 -173.0(4) . . . . ? C54 C49 C50 C51 -1.2(12) . . . . ? C54 C49 C50 As2 -177.0(7) . . . . ? C43 As2 C50 C51 106.5(7) . . . . ? C37 As2 C50 C51 -0.3(8) . . . . ? Pd2 As2 C50 C51 -126.6(6) . . . . ? C43 As2 C50 C49 -77.9(6) . . . . ? C37 As2 C50 C49 175.3(6) . . . . ? Pd2 As2 C50 C49 49.0(7) . . . . ? C49 C50 C51 C52 -0.1(13) . . . . ? As2 C50 C51 C52 175.4(7) . . . . ? C50 C51 C52 C53 0.6(15) . . . . ? C51 C52 C53 C54 0.3(17) . . . . ? C52 C53 C54 C49 -1.6(17) . . . . ? C50 C49 C54 C53 2.1(14) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.688 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.127