# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Vimal K. Jain' _publ_contact_author_email jainvk@barc.gov.in loop_ _publ_author_name 'Vimal K.Jain' 'Kedarnath Gotluru' 'Rohit Chauhan' 'Amey Wadawale' 'Alexandra Slawin' # Attachment '- 5.3H2O.cif' data_5.3H2O. _database_code_depnum_ccdc_archive 'CCDC 864901' #TrackingRef '- 5.3H2O.cif' # start Validation Reply Form _vrf_PLAT306_5.3H2O. ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 RESPONSE: solvent water - no hydrogen atoms located. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H64 N2 P4 Pd2 Te2,Cl2,3(H2 O)' _chemical_formula_sum 'C66 H70 Cl2 N2 O3 P4 Pd2 Te2' _chemical_formula_weight 1602.02 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' 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' Te Te -0.5308 1.6751 '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 11.934(6) _cell_length_b 13.083(7) _cell_length_c 13.460(7) _cell_angle_alpha 114.084(2) _cell_angle_beta 99.385(4) _cell_angle_gamma 111.686(5) _cell_volume 1656.3(15) _cell_formula_units_Z 1 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 4185 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.6 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 794 _exptl_absorpt_coefficient_mu 1.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16863 _diffrn_reflns_av_R_equivalents 0.1030 _diffrn_reflns_av_sigmaI/netI 0.1567 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.39 _reflns_number_total 6038 _reflns_number_gt 4541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _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^)+(0.0495P)^2^+2.9187P] 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 6038 _refine_ls_number_parameters 365 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1727 _refine_ls_wR_factor_gt 0.1577 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 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 0.01969(6) 0.09638(5) -0.08143(5) 0.02541(19) Uani 1 1 d . . . Te1 Te 0.05103(5) 0.14119(4) 0.13296(4) 0.02939(18) Uani 1 1 d . . . C1 C 0.2460(8) 0.1710(8) 0.1777(7) 0.0382(19) Uani 1 1 d . . . N2 N 0.2525(7) 0.0640(7) 0.1138(6) 0.0451(18) Uani 1 1 d . . . C3 C 0.3695(10) 0.0708(9) 0.1395(9) 0.054(3) Uani 1 1 d . . . H3A H 0.3766 -0.0026 0.0938 0.065 Uiso 1 1 calc R . . C4 C 0.4811(10) 0.1802(9) 0.2299(9) 0.054(2) Uani 1 1 d . . . H4A H 0.5623 0.1816 0.2468 0.065 Uiso 1 1 calc R . . C5 C 0.4690(9) 0.2868(9) 0.2940(8) 0.048(2) Uani 1 1 d . . . H5A H 0.5434 0.3620 0.3569 0.058 Uiso 1 1 calc R . . C6 C 0.3528(8) 0.2874(8) 0.2694(7) 0.0368(19) Uani 1 1 d . . . C7 C 0.3413(9) 0.4025(8) 0.3366(7) 0.046(2) Uani 1 1 d . . . H7A H 0.4265 0.4727 0.3957 0.069 Uiso 1 1 calc R . . H7B H 0.2802 0.3836 0.3753 0.069 Uiso 1 1 calc R . . H7C H 0.3095 0.4274 0.2832 0.069 Uiso 1 1 calc R . . P1 P 0.0639(2) 0.30152(19) -0.02403(16) 0.0283(5) Uani 1 1 d . . . C8 C 0.0321(8) 0.3348(7) -0.1405(7) 0.0337(19) Uani 1 1 d . . . H8A H -0.0629 0.2901 -0.1832 0.040 Uiso 1 1 calc R . . H8B H 0.0635 0.4278 -0.1055 0.040 Uiso 1 1 calc R . . C9 C 0.0958(8) 0.2942(7) -0.2273(6) 0.0317(18) Uani 1 1 d . . . H9A H 0.1846 0.3165 -0.1839 0.038 Uiso 1 1 calc R . . H9B H 0.1034 0.3426 -0.2686 0.038 Uiso 1 1 calc R . . C10 C 0.0204(8) 0.1508(7) -0.3179(7) 0.0338(19) Uani 1 1 d . . . H10A H 0.0532 0.1351 -0.3827 0.041 Uiso 1 1 calc R . . H10B H -0.0720 0.1263 -0.3510 0.041 Uiso 1 1 calc R . . P2 P 0.0300(2) 0.04679(19) -0.26282(16) 0.0279(5) Uani 1 1 d . . . C11 C 0.2317(7) 0.4191(7) 0.0637(6) 0.0278(17) Uani 1 1 d . . . C12 C 0.3286(8) 0.3825(7) 0.0557(7) 0.0351(19) Uani 1 1 d . . . H12A H 0.3045 0.2944 0.0116 0.042 Uiso 1 1 calc R . . C13 C 0.4587(8) 0.4736(8) 0.1116(7) 0.040(2) Uani 1 1 d . . . H13A H 0.5233 0.4480 0.1045 0.048 Uiso 1 1 calc R . . C14 C 0.4944(8) 0.6004(8) 0.1769(7) 0.042(2) Uani 1 1 d . . . H14A H 0.5837 0.6627 0.2148 0.050 Uiso 1 1 calc R . . C15 C 0.4012(8) 0.6383(8) 0.1881(7) 0.042(2) Uani 1 1 d . . . H15A H 0.4271 0.7263 0.2359 0.050 Uiso 1 1 calc R . . C16 C 0.2706(8) 0.5496(8) 0.1305(7) 0.0367(19) Uani 1 1 d . . . H16A H 0.2073 0.5771 0.1361 0.044 Uiso 1 1 calc R . . C17 C -0.0359(8) 0.3409(7) 0.0577(6) 0.0308(18) Uani 1 1 d . . . C18 C -0.1674(8) 0.2902(7) -0.0036(7) 0.0356(19) Uani 1 1 d . . . H18A H -0.2016 0.2431 -0.0868 0.043 Uiso 1 1 calc R . . C19 C -0.2476(9) 0.3086(8) 0.0569(8) 0.047(2) Uani 1 1 d . . . H19A H -0.3370 0.2752 0.0152 0.057 Uiso 1 1 calc R . . C20 C -0.1976(10) 0.3765(9) 0.1794(9) 0.050(3) Uani 1 1 d . . . H20A H -0.2537 0.3874 0.2206 0.060 Uiso 1 1 calc R . . C21 C -0.0696(9) 0.4270(8) 0.2398(7) 0.043(2) Uani 1 1 d . . . H21A H -0.0361 0.4744 0.3230 0.051 Uiso 1 1 calc R . . C22 C 0.0122(9) 0.4096(8) 0.1805(7) 0.039(2) Uani 1 1 d . . . H22A H 0.1015 0.4444 0.2233 0.047 Uiso 1 1 calc R . . C23 C -0.0901(8) -0.1120(7) -0.3839(6) 0.0289(17) Uani 1 1 d . . . C24 C -0.0580(8) -0.2109(7) -0.4305(6) 0.0308(17) Uani 1 1 d . . . H24A H 0.0272 -0.1963 -0.3983 0.037 Uiso 1 1 calc R . . C25 C -0.1540(8) -0.3308(8) -0.5247(7) 0.0364(19) Uani 1 1 d . . . H25A H -0.1339 -0.3983 -0.5563 0.044 Uiso 1 1 calc R . . C26 C -0.2757(9) -0.3520(8) -0.5716(7) 0.042(2) Uani 1 1 d . . . H26A H -0.3382 -0.4326 -0.6383 0.050 Uiso 1 1 calc R . . C27 C -0.3102(9) -0.2565(8) -0.5230(7) 0.044(2) Uani 1 1 d . . . H27A H -0.3966 -0.2732 -0.5539 0.053 Uiso 1 1 calc R . . C28 C -0.2169(8) -0.1378(7) -0.4297(6) 0.0314(17) Uani 1 1 d . . . H28A H -0.2397 -0.0726 -0.3961 0.038 Uiso 1 1 calc R . . C29 C 0.1861(8) 0.0507(7) -0.2551(7) 0.0318(18) Uani 1 1 d . . . C30 C 0.2590(7) 0.0536(7) -0.1615(6) 0.0303(17) Uani 1 1 d . . . H30A H 0.2301 0.0580 -0.0989 0.036 Uiso 1 1 calc R . . C31 C 0.3743(8) 0.0501(7) -0.1594(7) 0.0379(19) Uani 1 1 d . . . H31A H 0.4256 0.0548 -0.0941 0.045 Uiso 1 1 calc R . . C32 C 0.4148(9) 0.0398(7) -0.2527(8) 0.043(2) Uani 1 1 d . . . H32A H 0.4918 0.0341 -0.2525 0.051 Uiso 1 1 calc R . . C33 C 0.3425(8) 0.0380(8) -0.3465(7) 0.042(2) Uani 1 1 d . . . H33A H 0.3722 0.0339 -0.4086 0.051 Uiso 1 1 calc R . . C34 C 0.2268(8) 0.0422(7) -0.3497(6) 0.0343(19) Uani 1 1 d . . . H34A H 0.1765 0.0394 -0.4142 0.041 Uiso 1 1 calc R . . Cl1 Cl 0.6922(2) 0.1116(2) 0.66995(18) 0.0465(6) Uani 1 1 d . . . O1 O 0.5522(7) 0.1800(7) 0.5047(6) 0.072(2) Uani 1 1 d . . . O2 O 0.2361(16) 0.6608(15) 0.5223(14) 0.086(5) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0330(4) 0.0266(3) 0.0227(3) 0.0137(3) 0.0128(3) 0.0178(3) Te1 0.0413(4) 0.0279(3) 0.0246(3) 0.0146(2) 0.0145(3) 0.0197(3) C1 0.033(5) 0.046(5) 0.037(4) 0.027(4) 0.009(4) 0.015(4) N2 0.041(5) 0.039(4) 0.055(4) 0.023(4) 0.012(4) 0.023(4) C3 0.050(7) 0.051(6) 0.069(6) 0.035(5) 0.010(5) 0.034(5) C4 0.041(6) 0.052(6) 0.068(6) 0.038(5) 0.008(5) 0.017(5) C5 0.035(6) 0.049(5) 0.051(5) 0.028(5) 0.005(4) 0.013(5) C6 0.037(5) 0.036(4) 0.039(4) 0.023(4) 0.010(4) 0.016(4) C7 0.050(6) 0.038(5) 0.030(4) 0.013(4) 0.010(4) 0.009(5) P1 0.0385(13) 0.0272(10) 0.0245(9) 0.0126(8) 0.0134(9) 0.0208(10) C8 0.036(5) 0.025(4) 0.038(4) 0.012(4) 0.019(4) 0.016(4) C9 0.035(5) 0.030(4) 0.023(3) 0.007(3) 0.011(4) 0.016(4) C10 0.048(5) 0.037(4) 0.032(4) 0.024(4) 0.018(4) 0.027(4) P2 0.0366(12) 0.0294(10) 0.0234(9) 0.0144(8) 0.0156(9) 0.0184(10) C11 0.041(5) 0.025(4) 0.020(3) 0.013(3) 0.011(3) 0.017(4) C12 0.046(6) 0.034(4) 0.031(4) 0.017(4) 0.016(4) 0.024(4) C13 0.030(5) 0.055(6) 0.040(4) 0.023(4) 0.015(4) 0.023(5) C14 0.031(5) 0.044(5) 0.039(4) 0.019(4) 0.008(4) 0.012(4) C15 0.044(6) 0.044(5) 0.036(4) 0.020(4) 0.011(4) 0.022(5) C16 0.042(6) 0.039(5) 0.033(4) 0.019(4) 0.012(4) 0.024(4) C17 0.044(5) 0.029(4) 0.034(4) 0.017(3) 0.023(4) 0.028(4) C18 0.042(5) 0.034(4) 0.043(4) 0.024(4) 0.020(4) 0.023(4) C19 0.036(6) 0.040(5) 0.061(6) 0.020(5) 0.021(5) 0.019(5) C20 0.064(7) 0.058(6) 0.069(6) 0.042(5) 0.051(6) 0.046(6) C21 0.064(7) 0.042(5) 0.041(5) 0.023(4) 0.031(5) 0.036(5) C22 0.053(6) 0.040(5) 0.040(4) 0.022(4) 0.024(4) 0.031(5) C23 0.040(5) 0.030(4) 0.032(4) 0.020(3) 0.020(4) 0.024(4) C24 0.033(5) 0.034(4) 0.026(3) 0.015(3) 0.013(3) 0.015(4) C25 0.039(5) 0.034(4) 0.031(4) 0.012(4) 0.014(4) 0.017(4) C26 0.049(6) 0.026(4) 0.032(4) 0.011(4) 0.012(4) 0.006(4) C27 0.044(6) 0.051(5) 0.043(5) 0.028(5) 0.020(5) 0.021(5) C28 0.042(5) 0.030(4) 0.023(3) 0.013(3) 0.010(4) 0.020(4) C29 0.036(5) 0.029(4) 0.035(4) 0.016(4) 0.018(4) 0.019(4) C30 0.035(5) 0.033(4) 0.029(4) 0.015(3) 0.015(4) 0.020(4) C31 0.040(5) 0.033(4) 0.047(5) 0.022(4) 0.014(4) 0.022(4) C32 0.046(6) 0.033(5) 0.061(6) 0.027(4) 0.030(5) 0.023(4) C33 0.047(6) 0.040(5) 0.049(5) 0.025(4) 0.033(5) 0.021(5) C34 0.035(5) 0.045(5) 0.027(4) 0.021(4) 0.017(4) 0.019(4) Cl1 0.0413(13) 0.0542(13) 0.0414(11) 0.0175(11) 0.0148(10) 0.0287(12) O1 0.080(6) 0.080(5) 0.069(5) 0.035(4) 0.032(4) 0.052(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 Pd1 P1 2.282(2) . ? Pd1 P2 2.294(2) . ? Pd1 Te1 2.6299(15) . ? Pd1 Te1 2.6391(17) 2 ? Te1 C1 2.148(8) . ? Te1 Pd1 2.6391(17) 2 ? C1 N2 1.350(10) . ? C1 C6 1.409(11) . ? N2 C3 1.343(11) . ? C3 C4 1.394(13) . ? C3 H3A 0.9500 . ? C4 C5 1.385(12) . ? C4 H4A 0.9500 . ? C5 C6 1.376(11) . ? C5 H5A 0.9500 . ? C6 C7 1.478(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? P1 C11 1.800(8) . ? P1 C8 1.811(8) . ? P1 C17 1.820(6) . ? C8 C9 1.519(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.531(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 P2 1.824(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? P2 C23 1.817(8) . ? P2 C29 1.830(8) . ? C11 C16 1.401(10) . ? C11 C12 1.411(10) . ? C12 C13 1.384(11) . ? C12 H12A 0.9500 . ? C13 C14 1.368(11) . ? C13 H13A 0.9500 . ? C14 C15 1.381(11) . ? C14 H14A 0.9500 . ? C15 C16 1.382(11) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.395(11) . ? C17 C22 1.402(10) . ? C18 C19 1.379(10) . ? C18 H18A 0.9500 . ? C19 C20 1.399(13) . ? C19 H19A 0.9500 . ? C20 C21 1.357(13) . ? C20 H20A 0.9500 . ? C21 C22 1.382(10) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C28 1.390(11) . ? C23 C24 1.414(9) . ? C24 C25 1.398(10) . ? C24 H24A 0.9500 . ? C25 C26 1.358(12) . ? C25 H25A 0.9500 . ? C26 C27 1.400(11) . ? C26 H26A 0.9500 . ? C27 C28 1.380(11) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.387(11) . ? C29 C34 1.413(9) . ? C30 C31 1.390(10) . ? C30 H30A 0.9500 . ? C31 C32 1.392(10) . ? C31 H31A 0.9500 . ? C32 C33 1.394(12) . ? C32 H32A 0.9500 . ? C33 C34 1.395(10) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P2 95.32(7) . . ? P1 Pd1 Te1 91.20(5) . . ? P2 Pd1 Te1 167.01(6) . . ? P1 Pd1 Te1 172.79(5) . 2 ? P2 Pd1 Te1 90.54(5) . 2 ? Te1 Pd1 Te1 83.89(2) . 2 ? C1 Te1 Pd1 95.5(2) . . ? C1 Te1 Pd1 85.7(2) . 2 ? Pd1 Te1 Pd1 96.11(2) . 2 ? N2 C1 C6 124.5(8) . . ? N2 C1 Te1 112.5(6) . . ? C6 C1 Te1 122.9(6) . . ? C3 N2 C1 117.1(8) . . ? N2 C3 C4 123.2(9) . . ? N2 C3 H3A 118.4 . . ? C4 C3 H3A 118.4 . . ? C5 C4 C3 117.5(9) . . ? C5 C4 H4A 121.3 . . ? C3 C4 H4A 121.3 . . ? C6 C5 C4 122.1(9) . . ? C6 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? C5 C6 C1 115.6(8) . . ? C5 C6 C7 121.8(8) . . ? C1 C6 C7 122.6(8) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C11 P1 C8 102.2(3) . . ? C11 P1 C17 109.0(3) . . ? C8 P1 C17 105.6(3) . . ? C11 P1 Pd1 114.1(2) . . ? C8 P1 Pd1 116.0(2) . . ? C17 P1 Pd1 109.3(2) . . ? C9 C8 P1 113.7(5) . . ? C9 C8 H8A 108.8 . . ? P1 C8 H8A 108.8 . . ? C9 C8 H8B 108.8 . . ? P1 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C8 C9 C10 113.0(6) . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C9 C10 P2 115.3(6) . . ? C9 C10 H10A 108.4 . . ? P2 C10 H10A 108.4 . . ? C9 C10 H10B 108.4 . . ? P2 C10 H10B 108.4 . . ? H10A C10 H10B 107.5 . . ? C23 P2 C10 103.1(4) . . ? C23 P2 C29 104.8(3) . . ? C10 P2 C29 106.9(4) . . ? C23 P2 Pd1 116.5(2) . . ? C10 P2 Pd1 117.8(2) . . ? C29 P2 Pd1 106.7(3) . . ? C16 C11 C12 118.3(7) . . ? C16 C11 P1 121.6(6) . . ? C12 C11 P1 119.7(5) . . ? C13 C12 C11 120.6(7) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C14 C13 C12 120.1(7) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C14 C15 120.3(8) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C14 C15 C16 120.7(8) . . ? C14 C15 H15A 119.6 . . ? C16 C15 H15A 119.6 . . ? C15 C16 C11 119.9(7) . . ? C15 C16 H16A 120.0 . . ? C11 C16 H16A 120.0 . . ? C18 C17 C22 119.0(7) . . ? C18 C17 P1 118.7(6) . . ? C22 C17 P1 122.0(6) . . ? C19 C18 C17 119.8(8) . . ? C19 C18 H18A 120.1 . . ? C17 C18 H18A 120.1 . . ? C18 C19 C20 120.1(9) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C21 C20 C19 120.5(7) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C22 120.1(8) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C21 C22 C17 120.4(9) . . ? C21 C22 H22A 119.8 . . ? C17 C22 H22A 119.8 . . ? C28 C23 C24 119.3(7) . . ? C28 C23 P2 119.4(5) . . ? C24 C23 P2 121.3(6) . . ? C25 C24 C23 118.8(8) . . ? C25 C24 H24A 120.6 . . ? C23 C24 H24A 120.6 . . ? C26 C25 C24 120.9(8) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C25 C26 C27 120.9(8) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C28 C27 C26 119.0(9) . . ? C28 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? C27 C28 C23 121.1(7) . . ? C27 C28 H28A 119.5 . . ? C23 C28 H28A 119.5 . . ? C30 C29 C34 120.7(7) . . ? C30 C29 P2 120.4(5) . . ? C34 C29 P2 118.8(6) . . ? C29 C30 C31 119.9(7) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C30 C31 C32 120.1(8) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C33 120.2(8) . . ? C31 C32 H32A 119.9 . . ? C33 C32 H32A 119.9 . . ? C34 C33 C32 120.5(7) . . ? C34 C33 H33A 119.7 . . ? C32 C33 H33A 119.7 . . ? C33 C34 C29 118.6(8) . . ? C33 C34 H34A 120.7 . . ? C29 C34 H34A 120.7 . . ? 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 P1 Pd1 Te1 C1 -99.0(2) . . . . ? P2 Pd1 Te1 C1 21.2(3) . . . . ? Te1 Pd1 Te1 C1 86.3(2) 2 . . . ? P1 Pd1 Te1 Pd1 174.71(6) . . . 2 ? P2 Pd1 Te1 Pd1 -65.1(3) . . . 2 ? Te1 Pd1 Te1 Pd1 0.0 2 . . 2 ? Pd1 Te1 C1 N2 -65.4(6) . . . . ? Pd1 Te1 C1 N2 30.3(6) 2 . . . ? Pd1 Te1 C1 C6 118.7(6) . . . . ? Pd1 Te1 C1 C6 -145.6(7) 2 . . . ? C6 C1 N2 C3 -0.7(13) . . . . ? Te1 C1 N2 C3 -176.5(7) . . . . ? C1 N2 C3 C4 2.0(14) . . . . ? N2 C3 C4 C5 -1.1(15) . . . . ? C3 C4 C5 C6 -1.2(14) . . . . ? C4 C5 C6 C1 2.3(13) . . . . ? C4 C5 C6 C7 -178.6(8) . . . . ? N2 C1 C6 C5 -1.4(12) . . . . ? Te1 C1 C6 C5 174.0(6) . . . . ? N2 C1 C6 C7 179.5(8) . . . . ? Te1 C1 C6 C7 -5.0(11) . . . . ? P2 Pd1 P1 C11 -96.9(2) . . . . ? Te1 Pd1 P1 C11 71.9(2) . . . . ? Te1 Pd1 P1 C11 118.8(5) 2 . . . ? P2 Pd1 P1 C8 21.5(3) . . . . ? Te1 Pd1 P1 C8 -169.7(3) . . . . ? Te1 Pd1 P1 C8 -122.8(5) 2 . . . ? P2 Pd1 P1 C17 140.8(3) . . . . ? Te1 Pd1 P1 C17 -50.4(3) . . . . ? Te1 Pd1 P1 C17 -3.5(6) 2 . . . ? C11 P1 C8 C9 72.3(6) . . . . ? C17 P1 C8 C9 -173.7(5) . . . . ? Pd1 P1 C8 C9 -52.5(6) . . . . ? P1 C8 C9 C10 80.0(8) . . . . ? C8 C9 C10 P2 -73.0(8) . . . . ? C9 C10 P2 C23 170.5(5) . . . . ? C9 C10 P2 C29 -79.4(6) . . . . ? C9 C10 P2 Pd1 40.7(7) . . . . ? P1 Pd1 P2 C23 -140.1(3) . . . . ? Te1 Pd1 P2 C23 100.1(4) . . . . ? Te1 Pd1 P2 C23 35.7(3) 2 . . . ? P1 Pd1 P2 C10 -16.7(3) . . . . ? Te1 Pd1 P2 C10 -136.5(4) . . . . ? Te1 Pd1 P2 C10 159.1(3) 2 . . . ? P1 Pd1 P2 C29 103.4(3) . . . . ? Te1 Pd1 P2 C29 -16.4(4) . . . . ? Te1 Pd1 P2 C29 -80.8(3) 2 . . . ? C8 P1 C11 C16 70.3(6) . . . . ? C17 P1 C11 C16 -41.1(7) . . . . ? Pd1 P1 C11 C16 -163.6(5) . . . . ? C8 P1 C11 C12 -102.4(6) . . . . ? C17 P1 C11 C12 146.2(6) . . . . ? Pd1 P1 C11 C12 23.7(6) . . . . ? C16 C11 C12 C13 -0.7(11) . . . . ? P1 C11 C12 C13 172.3(6) . . . . ? C11 C12 C13 C14 1.1(12) . . . . ? C12 C13 C14 C15 0.3(13) . . . . ? C13 C14 C15 C16 -2.2(13) . . . . ? C14 C15 C16 C11 2.7(12) . . . . ? C12 C11 C16 C15 -1.2(11) . . . . ? P1 C11 C16 C15 -174.0(6) . . . . ? C11 P1 C17 C18 159.7(6) . . . . ? C8 P1 C17 C18 50.5(7) . . . . ? Pd1 P1 C17 C18 -75.0(6) . . . . ? C11 P1 C17 C22 -26.9(7) . . . . ? C8 P1 C17 C22 -136.0(7) . . . . ? Pd1 P1 C17 C22 98.5(6) . . . . ? C22 C17 C18 C19 0.3(11) . . . . ? P1 C17 C18 C19 173.9(6) . . . . ? C17 C18 C19 C20 -0.8(12) . . . . ? C18 C19 C20 C21 1.3(14) . . . . ? C19 C20 C21 C22 -1.2(13) . . . . ? C20 C21 C22 C17 0.7(12) . . . . ? C18 C17 C22 C21 -0.2(12) . . . . ? P1 C17 C22 C21 -173.6(6) . . . . ? C10 P2 C23 C28 -54.6(6) . . . . ? C29 P2 C23 C28 -166.3(6) . . . . ? Pd1 P2 C23 C28 76.0(6) . . . . ? C10 P2 C23 C24 127.1(6) . . . . ? C29 P2 C23 C24 15.4(7) . . . . ? Pd1 P2 C23 C24 -102.2(6) . . . . ? C28 C23 C24 C25 2.6(10) . . . . ? P2 C23 C24 C25 -179.1(6) . . . . ? C23 C24 C25 C26 0.5(11) . . . . ? C24 C25 C26 C27 -3.4(12) . . . . ? C25 C26 C27 C28 3.1(12) . . . . ? C26 C27 C28 C23 0.1(12) . . . . ? C24 C23 C28 C27 -2.9(11) . . . . ? P2 C23 C28 C27 178.8(6) . . . . ? C23 P2 C29 C30 -110.8(6) . . . . ? C10 P2 C29 C30 140.2(6) . . . . ? Pd1 P2 C29 C30 13.3(7) . . . . ? C23 P2 C29 C34 65.1(7) . . . . ? C10 P2 C29 C34 -43.8(7) . . . . ? Pd1 P2 C29 C34 -170.8(5) . . . . ? C34 C29 C30 C31 1.0(12) . . . . ? P2 C29 C30 C31 176.8(6) . . . . ? C29 C30 C31 C32 -1.9(11) . . . . ? C30 C31 C32 C33 2.5(12) . . . . ? C31 C32 C33 C34 -2.1(13) . . . . ? C32 C33 C34 C29 1.2(12) . . . . ? C30 C29 C34 C33 -0.6(12) . . . . ? P2 C29 C34 C33 -176.5(6) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.324 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.183 # Attachment '- ligand.cif' data_ligand _database_code_depnum_ccdc_archive 'CCDC 864902' #TrackingRef '- ligand.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H12 N2 Te2' _chemical_formula_sum 'C12 H12 N2 Te2' _chemical_formula_weight 439.44 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' Te Te -0.5308 1.6751 '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 6.804(2) _cell_length_b 7.5995(14) _cell_length_c 7.7209(4) _cell_angle_alpha 63.64(3) _cell_angle_beta 66.90(3) _cell_angle_gamma 86.84(4) _cell_volume 325.58(12) _cell_formula_units_Z 1 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 1309 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 28.1 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 202 _exptl_absorpt_coefficient_mu 4.455 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type CCD _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1998 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.34 _reflns_number_total 1126 _reflns_number_gt 1085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _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. The largest peak is located 1.27A from Te1.Isor restatints were used for C1 and C4. ; _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^)+(0.0437P)^2^+9.4033P] 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 1126 _refine_ls_number_parameters 73 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0339 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.0977 _refine_ls_goodness_of_fit_ref 1.275 _refine_ls_restrained_S_all 1.268 _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 Te1 Te 0.16837(11) 0.41316(10) 0.03901(11) 0.0167(3) Uani 1 1 d . . . C1 C -0.0240(18) 0.3199(16) 0.3681(17) 0.015(2) Uani 1 1 d U . . N2 N -0.2216(14) 0.3736(14) 0.4155(15) 0.0156(19) Uani 1 1 d . . . C3 C -0.3508(18) 0.3168(17) 0.6214(19) 0.019(2) Uani 1 1 d . . . H3A H -0.4934 0.3494 0.6573 0.023 Uiso 1 1 calc R . . C4 C -0.2816(18) 0.2109(16) 0.7848(18) 0.016(2) Uani 1 1 d U . . H4A H -0.3745 0.1699 0.9294 0.019 Uiso 1 1 calc R . . C5 C -0.0718(19) 0.1697(17) 0.7243(17) 0.018(2) Uani 1 1 d . . . H5A H -0.0172 0.1070 0.8299 0.022 Uiso 1 1 calc R . . C6 C 0.0613(17) 0.2154(16) 0.5180(17) 0.016(2) Uani 1 1 d . . . C7 C 0.2855(18) 0.1613(19) 0.4525(19) 0.022(2) Uani 1 1 d . . . H7A H 0.3166 0.0893 0.5780 0.033 Uiso 1 1 calc R . . H7B H 0.3902 0.2825 0.3528 0.033 Uiso 1 1 calc R . . H7C H 0.2957 0.0771 0.3841 0.033 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 Te1 0.0139(4) 0.0217(5) 0.0132(4) -0.0085(3) -0.0040(3) 0.0049(3) C1 0.015(2) 0.015(2) 0.015(2) -0.0073(13) -0.0057(13) 0.0017(10) N2 0.009(4) 0.018(5) 0.020(5) -0.016(4) 0.001(4) 0.000(4) C3 0.013(5) 0.016(6) 0.026(6) -0.011(5) -0.003(5) 0.000(4) C4 0.016(2) 0.016(2) 0.016(2) -0.0074(13) -0.0062(13) 0.0020(10) C5 0.024(6) 0.019(6) 0.008(5) 0.001(4) -0.010(5) -0.001(5) C6 0.013(5) 0.017(5) 0.014(5) -0.011(4) 0.003(4) -0.011(4) C7 0.011(5) 0.028(6) 0.024(6) -0.009(5) -0.008(5) 0.002(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 Te1 C1 2.136(11) . ? Te1 Te1 2.7199(17) 2_565 ? C1 N2 1.340(14) . ? C1 C6 1.403(16) . ? N2 C3 1.350(15) . ? C3 C4 1.409(16) . ? C3 H3A 0.9500 . ? C4 C5 1.383(16) . ? C4 H4A 0.9500 . ? C5 C6 1.375(16) . ? C5 H5A 0.9500 . ? C6 C7 1.503(16) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Te1 Te1 87.7(3) . 2_565 ? N2 C1 C6 124.2(10) . . ? N2 C1 Te1 115.7(8) . . ? C6 C1 Te1 120.1(8) . . ? C1 N2 C3 118.2(10) . . ? N2 C3 C4 122.3(10) . . ? N2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C5 C4 C3 116.7(10) . . ? C5 C4 H4A 121.6 . . ? C3 C4 H4A 121.6 . . ? C6 C5 C4 122.8(10) . . ? C6 C5 H5A 118.6 . . ? C4 C5 H5A 118.6 . . ? C5 C6 C1 115.6(10) . . ? C5 C6 C7 123.2(11) . . ? C1 C6 C7 121.2(10) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 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 Te1 Te1 C1 N2 0.0(8) 2_565 . . . ? Te1 Te1 C1 C6 -177.8(8) 2_565 . . . ? C6 C1 N2 C3 -2.9(16) . . . . ? Te1 C1 N2 C3 179.3(7) . . . . ? C1 N2 C3 C4 2.6(16) . . . . ? N2 C3 C4 C5 1.0(16) . . . . ? C3 C4 C5 C6 -4.5(17) . . . . ? C4 C5 C6 C1 4.2(17) . . . . ? C4 C5 C6 C7 -176.6(11) . . . . ? N2 C1 C6 C5 -0.4(16) . . . . ? Te1 C1 C6 C5 177.2(8) . . . . ? N2 C1 C6 C7 -179.6(10) . . . . ? Te1 C1 C6 C7 -1.9(14) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.553 _refine_diff_density_min -1.711 _refine_diff_density_rms 0.431 data_rc-1 _database_code_depnum_ccdc_archive 'CCDC 864904' #TrackingRef 'new-rc-1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H21 Cl3 N P Pd Te' _chemical_formula_weight 694.74 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' P P 0.1023 0.0942 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 17.000(14) _cell_length_b 10.775(4) _cell_length_c 15.631(15) _cell_angle_alpha 90.00 _cell_angle_beta 115.51(6) _cell_angle_gamma 90.00 _cell_volume 2584(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 12.4 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.786 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 2.209 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.786 _exptl_absorpt_correction_T_max 0.905 _exptl_special_details ; The crystal loaded was a thin square plate with dimensions of much lesser than 0.15 mm x 0.15 mm x 0.5 mm, almost two dimensional, isolated with difficulty from a NMR tube. This may have lead to a low Ratio Observed / Unique Reflections ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.11 _diffrn_reflns_number 7091 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.4716 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 27.53 _reflns_number_total 5940 _reflns_number_gt 1494 _reflns_threshold_expression >2sigma(I) _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction CrystalStructure _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows' _computing_publication_material 'WinGX 1.7.01' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. SIMU restraints were applied to carbon atoms of phenyl and pyridine rings to improve the quality of ellipsoid.i.e a total of 23 atom sites were restrained leading to 132 least square restraints. ; _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^)+(0.0068P)^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 5940 _refine_ls_number_parameters 240 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.3597 _refine_ls_R_factor_gt 0.0720 _refine_ls_wR_factor_ref 0.1452 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.893 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0787(8) 0.2226(15) 0.5359(10) 0.040(4) Uani 1 1 d U . . C2 C 0.0182(9) 0.2958(14) 0.4650(11) 0.051 Uani 1 1 d U . . C3 C -0.0691(9) 0.2718(15) 0.4408(11) 0.052 Uani 1 1 d U . . H3 H -0.1131 0.3165 0.3932 0.063 Uiso 1 1 calc R . . C4 C -0.0880(10) 0.1800(17) 0.4897(12) 0.062(5) Uani 1 1 d U . . H4 H -0.1464 0.1632 0.4736 0.074 Uiso 1 1 calc R . . C5 C -0.0266(10) 0.1115(16) 0.5605(12) 0.057(5) Uani 1 1 d U . . H5 H -0.0430 0.0505 0.5918 0.068 Uiso 1 1 calc R . . C6 C 0.0457(10) 0.3921(16) 0.4158(11) 0.074(6) Uani 1 1 d . . . H6A H 0.1006 0.4264 0.4590 0.112 Uiso 1 1 calc R . . H6B H 0.0027 0.4568 0.3936 0.112 Uiso 1 1 calc R . . H6C H 0.0516 0.3556 0.3628 0.112 Uiso 1 1 calc R . . C7 C 0.3531(9) -0.1131(13) 0.8079(10) 0.036(4) Uani 1 1 d U . . C8 C 0.3017(10) -0.2065(16) 0.7570(12) 0.062(5) Uani 1 1 d U . . H8 H 0.2416 -0.1960 0.7265 0.074 Uiso 1 1 calc R . . C9 C 0.3384(12) -0.3178(17) 0.7501(13) 0.067(5) Uani 1 1 d U . . H9 H 0.3019 -0.3803 0.7130 0.080 Uiso 1 1 calc R . . C10 C 0.4222(13) -0.3397(18) 0.7933(14) 0.077(6) Uani 1 1 d U . . H10 H 0.4443 -0.4174 0.7894 0.092 Uiso 1 1 calc R . . C11 C 0.4754(11) -0.249(2) 0.8429(12) 0.077(5) Uani 1 1 d U . . H11 H 0.5352 -0.2628 0.8714 0.092 Uiso 1 1 calc R . . C12 C 0.4431(11) -0.1340(16) 0.8528(13) 0.074(6) Uani 1 1 d U . . H12 H 0.4808 -0.0718 0.8887 0.089 Uiso 1 1 calc R . . C13 C 0.3933(10) 0.1445(16) 0.8186(11) 0.049(4) Uani 1 1 d U . . C14 C 0.4168(11) 0.1371(18) 0.7462(14) 0.077 Uani 1 1 d U . . H14 H 0.3890 0.0820 0.6964 0.093 Uiso 1 1 calc R . . C15 C 0.4834(10) 0.2136(17) 0.7478(13) 0.075 Uani 1 1 d U . . H15 H 0.5039 0.2027 0.7020 0.091 Uiso 1 1 calc R . . C16 C 0.5192(13) 0.303(2) 0.8138(14) 0.089 Uani 1 1 d U . . H16 H 0.5621 0.3544 0.8112 0.106 Uiso 1 1 calc R . . C17 C 0.4933(14) 0.3185(19) 0.8835(16) 0.113(8) Uani 1 1 d U . . H17 H 0.5186 0.3792 0.9296 0.136 Uiso 1 1 calc R . . C18 C 0.4255(12) 0.239(2) 0.8852(12) 0.079(5) Uani 1 1 d U . . H18 H 0.4039 0.2507 0.9301 0.095 Uiso 1 1 calc R . . C19 C 0.3040(9) 0.0545(15) 0.9249(10) 0.044 Uani 1 1 d U . . C20 C 0.2655(11) 0.1568(16) 0.9438(13) 0.072(5) Uani 1 1 d U . . H20 H 0.2430 0.2196 0.8989 0.086 Uiso 1 1 calc R . . C21 C 0.2604(13) 0.166(2) 1.0276(14) 0.107 Uani 1 1 d U . . H21 H 0.2283 0.2311 1.0354 0.128 Uiso 1 1 calc R . . C22 C 0.2981(12) 0.088(2) 1.0988(12) 0.089(6) Uani 1 1 d U . . H22 H 0.2957 0.1008 1.1565 0.106 Uiso 1 1 calc R . . C23 C 0.3402(12) -0.0100(17) 1.0851(11) 0.069(5) Uani 1 1 d U . . H23 H 0.3661 -0.0680 1.1333 0.083 Uiso 1 1 calc R . . C24 C 0.3450(9) -0.0252(16) 0.9987(11) 0.060(5) Uani 1 1 d U . . H24 H 0.3769 -0.0910 0.9914 0.072 Uiso 1 1 calc R . . N1 N 0.0577(7) 0.1339(12) 0.5840(8) 0.043(3) Uani 1 1 d . . . P1 P 0.3078(2) 0.0391(4) 0.8131(3) 0.0364(11) Uani 1 1 d . . . Cl1 Cl 0.1131(2) -0.0719(4) 0.7553(3) 0.0554(12) Uani 1 1 d . . . Cl2 Cl 0.2290(3) 0.0788(5) 0.4966(3) 0.0796(16) Uani 1 1 d . . . Cl3 Cl 0.1842(3) 0.4069(5) 0.7007(4) 0.0768(15) Uani 1 1 d . . . Pd1 Pd 0.17570(7) 0.07569(12) 0.69551(9) 0.0378(3) Uani 1 1 d . . . Te1 Te 0.21598(6) 0.24233(12) 0.60647(7) 0.0442(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(8) 0.054(12) 0.030(8) -0.008(9) 0.011(7) 0.010(9) C2 0.031 0.045 0.051 -0.006 -0.007 -0.004 C3 0.043 0.048 0.050 -0.012 0.006 -0.025 C4 0.030(9) 0.076(13) 0.068(12) -0.019(10) 0.010(9) -0.015(9) C5 0.025(9) 0.076(14) 0.074(13) -0.008(11) 0.026(9) -0.022(10) C6 0.068(13) 0.079(15) 0.072(14) 0.044(12) 0.027(11) 0.017(11) C7 0.039(9) 0.024(9) 0.037(9) -0.011(7) 0.008(8) -0.009(7) C8 0.050(11) 0.060(13) 0.077(12) -0.001(10) 0.028(10) 0.006(10) C9 0.061(12) 0.057(12) 0.085(13) -0.033(11) 0.035(11) 0.000(11) C10 0.075(13) 0.054(13) 0.110(16) -0.020(12) 0.048(13) 0.018(11) C11 0.073(12) 0.046(11) 0.090(13) -0.020(13) 0.015(10) 0.016(12) C12 0.054(11) 0.040(11) 0.094(14) -0.025(11) -0.001(10) -0.016(10) C13 0.046(10) 0.048(11) 0.048(10) 0.014(9) 0.015(9) 0.019(9) C14 0.068 0.078 0.085 0.029 0.031 0.007 C15 0.050 0.077 0.083 0.017 0.014 0.012 C16 0.090 0.081 0.072 0.016 0.013 0.010 C17 0.120(17) 0.068(15) 0.103(15) -0.023(13) 0.003(14) -0.017(13) C18 0.095(14) 0.057(13) 0.081(12) 0.001(13) 0.033(11) 0.003(13) C19 0.030 0.044 0.044 -0.016 0.002 -0.009 C20 0.094(13) 0.061(12) 0.083(13) 0.024(11) 0.060(11) 0.017(11) C21 0.124 0.146 0.090 0.026 0.085 0.056 C22 0.128(15) 0.113(16) 0.051(11) 0.026(12) 0.062(10) 0.053(13) C23 0.106(14) 0.069(13) 0.036(10) 0.008(10) 0.033(10) 0.008(11) C24 0.057(10) 0.085(13) 0.054(11) -0.021(10) 0.040(9) 0.001(10) N1 0.035(8) 0.051(10) 0.037(8) 0.005(7) 0.009(7) 0.001(7) P1 0.037(2) 0.037(3) 0.040(3) 0.001(2) 0.021(2) 0.000(2) Cl1 0.056(3) 0.047(3) 0.080(3) 0.006(3) 0.044(2) -0.005(2) Cl2 0.082(3) 0.099(4) 0.072(3) -0.014(3) 0.047(3) 0.007(3) Cl3 0.086(4) 0.069(4) 0.081(4) -0.019(3) 0.041(3) -0.011(3) Pd1 0.0339(7) 0.0420(8) 0.0394(8) 0.0026(8) 0.0175(6) -0.0015(8) Te1 0.0376(6) 0.0516(8) 0.0448(6) 0.0076(8) 0.0190(5) -0.0006(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. SIMU restraints were used for sets of aromatic carbon atoms in each of aromatic rings SIMU C7 C8 C9 C10 C11 C12; C13 C14 C15 C16 C17 C18; C19 C20 C21 C22 C23 C24; C1 C2 C3 C4 C5 ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.355(17) . ? C1 C2 1.388(18) . ? C1 Te1 2.120(13) . ? C2 C3 1.389(17) . ? C2 C6 1.482(19) . ? C3 C4 1.370(19) . ? C3 H3 0.9300 . ? C4 C5 1.37(2) . ? C4 H4 0.9300 . ? C5 N1 1.339(16) . ? C5 H5 0.9300 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.346(18) . ? C7 C12 1.400(18) . ? C7 P1 1.829(15) . ? C8 C9 1.38(2) . ? C8 H8 0.9300 . ? C9 C10 1.31(2) . ? C9 H9 0.9300 . ? C10 C11 1.33(2) . ? C10 H10 0.9300 . ? C11 C12 1.39(2) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.35(2) . ? C13 C18 1.39(2) . ? C13 P1 1.817(17) . ? C14 C15 1.39(2) . ? C14 H14 0.9300 . ? C15 C16 1.35(2) . ? C15 H15 0.9300 . ? C16 C17 1.35(3) . ? C16 H16 0.9300 . ? C17 C18 1.45(2) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.365(19) . ? C19 C20 1.377(19) . ? C19 P1 1.783(16) . ? C20 C21 1.35(2) . ? C20 H20 0.9300 . ? C21 C22 1.32(2) . ? C21 H21 0.9300 . ? C22 C23 1.35(2) . ? C22 H22 0.9300 . ? C23 C24 1.397(18) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? N1 Pd1 2.108(11) . ? P1 Pd1 2.241(5) . ? Cl1 Pd1 2.322(4) . ? Cl2 Te1 2.536(5) . ? Cl3 Te1 2.508(5) . ? Pd1 Te1 2.540(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 124.2(13) . . ? N1 C1 Te1 106.0(10) . . ? C2 C1 Te1 129.0(12) . . ? C3 C2 C1 116.7(16) . . ? C3 C2 C6 121.9(15) . . ? C1 C2 C6 121.4(14) . . ? C4 C3 C2 117.6(16) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C5 C4 C3 124.1(15) . . ? C5 C4 H4 117.9 . . ? C3 C4 H4 117.9 . . ? N1 C5 C4 118.6(16) . . ? N1 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C12 117.8(15) . . ? C8 C7 P1 121.3(12) . . ? C12 C7 P1 120.8(12) . . ? C7 C8 C9 119.8(16) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 123.1(18) . . ? C10 C9 H9 118.4 . . ? C8 C9 H9 118.4 . . ? C9 C10 C11 118.9(18) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C10 C11 C12 121.2(17) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 119.0(15) . . ? C11 C12 H12 120.5 . . ? C7 C12 H12 120.5 . . ? C14 C13 C18 120.4(18) . . ? C14 C13 P1 116.2(15) . . ? C18 C13 P1 122.8(14) . . ? C13 C14 C15 118.7(19) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 122(2) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C17 121(2) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 119(2) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C13 C18 C17 118.7(19) . . ? C13 C18 H18 120.6 . . ? C17 C18 H18 120.6 . . ? C24 C19 C20 116.0(15) . . ? C24 C19 P1 123.3(13) . . ? C20 C19 P1 120.3(13) . . ? C21 C20 C19 120.0(18) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 124(2) . . ? C22 C21 H21 117.9 . . ? C20 C21 H21 117.9 . . ? C21 C22 C23 117.7(17) . . ? C21 C22 H22 121.2 . . ? C23 C22 H22 121.2 . . ? C22 C23 C24 120.1(17) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C19 C24 C23 121.5(16) . . ? C19 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C5 N1 C1 118.8(14) . . ? C5 N1 Pd1 134.2(12) . . ? C1 N1 Pd1 106.5(9) . . ? C19 P1 C13 105.2(7) . . ? C19 P1 C7 108.7(7) . . ? C13 P1 C7 102.6(7) . . ? C19 P1 Pd1 109.9(5) . . ? C13 P1 Pd1 115.3(5) . . ? C7 P1 Pd1 114.4(5) . . ? N1 Pd1 P1 172.4(4) . . ? N1 Pd1 Cl1 95.7(4) . . ? P1 Pd1 Cl1 91.17(15) . . ? N1 Pd1 Te1 73.8(4) . . ? P1 Pd1 Te1 99.35(12) . . ? Cl1 Pd1 Te1 169.48(12) . . ? C1 Te1 Cl3 84.8(4) . . ? C1 Te1 Cl2 88.6(4) . . ? Cl3 Te1 Cl2 173.04(16) . . ? C1 Te1 Pd1 73.6(5) . . ? Cl3 Te1 Pd1 90.07(13) . . ? Cl2 Te1 Pd1 90.14(14) . . ? 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 C1 C2 C3 -2(2) . . . . ? Te1 C1 C2 C3 -171.0(10) . . . . ? N1 C1 C2 C6 179.4(14) . . . . ? Te1 C1 C2 C6 11(2) . . . . ? C1 C2 C3 C4 1(2) . . . . ? C6 C2 C3 C4 179.3(15) . . . . ? C2 C3 C4 C5 0(2) . . . . ? C3 C4 C5 N1 -1(3) . . . . ? C12 C7 C8 C9 0(3) . . . . ? P1 C7 C8 C9 176.3(13) . . . . ? C7 C8 C9 C10 2(3) . . . . ? C8 C9 C10 C11 -3(3) . . . . ? C9 C10 C11 C12 3(3) . . . . ? C10 C11 C12 C7 -1(3) . . . . ? C8 C7 C12 C11 0(3) . . . . ? P1 C7 C12 C11 -176.5(14) . . . . ? C18 C13 C14 C15 10(3) . . . . ? P1 C13 C14 C15 -178.5(12) . . . . ? C13 C14 C15 C16 -7(3) . . . . ? C14 C15 C16 C17 2(3) . . . . ? C15 C16 C17 C18 -1(3) . . . . ? C14 C13 C18 C17 -8(3) . . . . ? P1 C13 C18 C17 -179.6(13) . . . . ? C16 C17 C18 C13 4(3) . . . . ? C24 C19 C20 C21 -8(2) . . . . ? P1 C19 C20 C21 177.9(15) . . . . ? C19 C20 C21 C22 7(3) . . . . ? C20 C21 C22 C23 -4(4) . . . . ? C21 C22 C23 C24 2(3) . . . . ? C20 C19 C24 C23 6(2) . . . . ? P1 C19 C24 C23 -179.8(12) . . . . ? C22 C23 C24 C19 -3(3) . . . . ? C4 C5 N1 C1 -1(2) . . . . ? C4 C5 N1 Pd1 170.4(12) . . . . ? C2 C1 N1 C5 2(2) . . . . ? Te1 C1 N1 C5 173.1(11) . . . . ? C2 C1 N1 Pd1 -171.1(12) . . . . ? Te1 C1 N1 Pd1 -0.3(10) . . . . ? C24 C19 P1 C13 -97.3(14) . . . . ? C20 C19 P1 C13 76.2(14) . . . . ? C24 C19 P1 C7 12.1(14) . . . . ? C20 C19 P1 C7 -174.4(13) . . . . ? C24 C19 P1 Pd1 138.0(12) . . . . ? C20 C19 P1 Pd1 -48.5(14) . . . . ? C14 C13 P1 C19 171.4(13) . . . . ? C18 C13 P1 C19 -17.0(15) . . . . ? C14 C13 P1 C7 57.7(14) . . . . ? C18 C13 P1 C7 -130.7(14) . . . . ? C14 C13 P1 Pd1 -67.4(14) . . . . ? C18 C13 P1 Pd1 104.3(13) . . . . ? C8 C7 P1 C19 103.9(14) . . . . ? C12 C7 P1 C19 -79.6(14) . . . . ? C8 C7 P1 C13 -145.0(14) . . . . ? C12 C7 P1 C13 31.4(15) . . . . ? C8 C7 P1 Pd1 -19.4(15) . . . . ? C12 C7 P1 Pd1 157.1(12) . . . . ? C5 N1 Pd1 P1 -144(2) . . . . ? C1 N1 Pd1 P1 27(3) . . . . ? C5 N1 Pd1 Cl1 9.1(15) . . . . ? C1 N1 Pd1 Cl1 -179.0(9) . . . . ? C5 N1 Pd1 Te1 -171.6(15) . . . . ? C1 N1 Pd1 Te1 0.2(8) . . . . ? C19 P1 Pd1 N1 100(3) . . . . ? C13 P1 Pd1 N1 -19(3) . . . . ? C7 P1 Pd1 N1 -138(3) . . . . ? C19 P1 Pd1 Cl1 -53.9(6) . . . . ? C13 P1 Pd1 Cl1 -172.6(7) . . . . ? C7 P1 Pd1 Cl1 68.7(5) . . . . ? C19 P1 Pd1 Te1 126.2(6) . . . . ? C13 P1 Pd1 Te1 7.5(7) . . . . ? C7 P1 Pd1 Te1 -111.2(5) . . . . ? N1 C1 Te1 Cl3 -91.4(9) . . . . ? C2 C1 Te1 Cl3 78.9(13) . . . . ? N1 C1 Te1 Cl2 90.8(9) . . . . ? C2 C1 Te1 Cl2 -98.9(13) . . . . ? N1 C1 Te1 Pd1 0.2(8) . . . . ? C2 C1 Te1 Pd1 170.5(14) . . . . ? N1 Pd1 Te1 C1 -0.1(5) . . . . ? P1 Pd1 Te1 C1 -176.6(4) . . . . ? Cl1 Pd1 Te1 C1 3.9(8) . . . . ? N1 Pd1 Te1 Cl3 84.4(4) . . . . ? P1 Pd1 Te1 Cl3 -92.07(17) . . . . ? Cl1 Pd1 Te1 Cl3 88.4(7) . . . . ? N1 Pd1 Te1 Cl2 -88.6(4) . . . . ? P1 Pd1 Te1 Cl2 94.89(16) . . . . ? Cl1 Pd1 Te1 Cl2 -84.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.747 _refine_diff_density_min -1.368 _refine_diff_density_rms 0.189 _iucr_refine_instructions_details ;TITL PPP-2 CELL 0.71069 17.0000 10.7753 15.6308 90.000 115.513 90.000 ZERR 4.00 0.0144 0.0039 0.0146 0.000 0.060 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H N P CL PD TE UNIT 96 84 4 4 12 4 4 MERG 2 SIMU C7 C8 C9 C10 C11 C12 SIMU C13 C14 C15 C16 C17 C18 SIMU C19 C20 C21 C22 C23 C24 SIMU C1 C2 C3 C4 C5 TWIN FMAP 2 PLAN 25 SIZE 0.15 0.15 0.50 ACTA BOND $H CONF LIST 3 L.S. 20 TEMP 25.00 WGHT 0.006800 BASF 0.00001 FVAR 0.02244 C1 1 0.078683 0.222557 0.535852 11.00000 0.03334 0.05373 = 0.02998 -0.00846 0.01109 0.00967 C2 1 0.018192 0.295767 0.464951 11.00000 10.03073 10.04460 = 10.05117 9.99428 9.99272 9.99628 C3 1 -0.069091 0.271811 0.440819 11.00000 10.04342 10.04767 = 10.05042 9.98764 10.00626 9.97500 AFIX 43 H3 2 -0.113084 0.316468 0.393235 11.00000 -1.20000 AFIX 0 C4 1 -0.088040 0.179977 0.489669 11.00000 0.02982 0.07581 = 0.06824 -0.01862 0.01006 -0.01540 AFIX 43 H4 2 -0.146395 0.163244 0.473562 11.00000 -1.20000 AFIX 0 C5 1 -0.026604 0.111458 0.560540 11.00000 0.02529 0.07590 = 0.07417 -0.00820 0.02648 -0.02183 AFIX 43 H5 2 -0.042962 0.050537 0.591846 11.00000 -1.20000 AFIX 0 C6 1 0.045703 0.392109 0.415752 11.00000 0.06842 0.07937 = 0.07189 0.04377 0.02673 0.01700 AFIX 137 H6A 2 0.100645 0.426398 0.458957 11.00000 -1.50000 H6B 2 0.002694 0.456757 0.393643 11.00000 -1.50000 H6C 2 0.051586 0.355560 0.362795 11.00000 -1.50000 AFIX 0 C7 1 0.353094 -0.113095 0.807950 11.00000 0.03890 0.02403 = 0.03695 -0.01095 0.00849 -0.00866 C8 1 0.301701 -0.206536 0.756967 11.00000 0.04991 0.05986 = 0.07661 -0.00118 0.02772 0.00589 AFIX 43 H8 2 0.241586 -0.195974 0.726478 11.00000 -1.20000 AFIX 0 C9 1 0.338411 -0.317777 0.750103 11.00000 0.06073 0.05702 = 0.08548 -0.03275 0.03494 0.00045 AFIX 43 H9 2 0.301932 -0.380298 0.713006 11.00000 -1.20000 AFIX 0 C10 1 0.422242 -0.339708 0.793329 11.00000 0.07499 0.05391 = 0.11037 -0.01989 0.04845 0.01760 AFIX 43 H10 2 0.444263 -0.417434 0.789438 11.00000 -1.20000 AFIX 0 C11 1 0.475364 -0.249075 0.842865 11.00000 0.07285 0.04606 = 0.08970 -0.02006 0.01497 0.01640 AFIX 43 H11 2 0.535202 -0.262850 0.871426 11.00000 -1.20000 AFIX 0 C12 1 0.443126 -0.133964 0.852794 11.00000 0.05440 0.03960 = 0.09425 -0.02456 -0.00109 -0.01557 AFIX 43 H12 2 0.480837 -0.071788 0.888700 11.00000 -1.20000 AFIX 0 C13 1 0.393336 0.144451 0.818563 11.00000 0.04556 0.04810 = 0.04767 0.01441 0.01475 0.01890 C14 1 0.416822 0.137092 0.746227 11.00000 10.06831 10.07775 = 10.08461 10.02891 10.03125 10.00733 AFIX 43 H14 2 0.389001 0.081990 0.696432 11.00000 -1.20000 AFIX 0 C15 1 0.483392 0.213572 0.747835 11.00000 10.05038 10.07711 = 10.08321 10.01705 10.01399 10.01154 AFIX 43 H15 2 0.503896 0.202707 0.701952 11.00000 -1.20000 AFIX 0 C16 1 0.519193 0.303026 0.813812 11.00000 10.08959 10.08123 = 10.07191 10.01558 10.01298 10.00962 AFIX 43 H16 2 0.562057 0.354427 0.811212 11.00000 -1.20000 AFIX 0 C17 1 0.493306 0.318496 0.883511 11.00000 0.12019 0.06822 = 0.10335 -0.02262 0.00284 -0.01701 AFIX 43 H17 2 0.518584 0.379236 0.929574 11.00000 -1.20000 AFIX 0 C18 1 0.425548 0.238890 0.885241 11.00000 0.09508 0.05722 = 0.08068 0.00094 0.03331 0.00286 AFIX 43 H18 2 0.403946 0.250674 0.930116 11.00000 -1.20000 AFIX 0 C19 1 0.303987 0.054474 0.924888 11.00000 10.03006 10.04385 = 10.04401 9.98388 10.00181 9.99099 C20 1 0.265504 0.156793 0.943750 11.00000 0.09399 0.06140 = 0.08280 0.02441 0.06036 0.01686 AFIX 43 H20 2 0.243025 0.219624 0.898911 11.00000 -1.20000 AFIX 0 C21 1 0.260418 0.165847 1.027602 11.00000 10.12415 10.14630 = 10.09030 10.02560 10.08517 10.05601 AFIX 43 H21 2 0.228277 0.231052 1.035442 11.00000 -1.20000 AFIX 0 C22 1 0.298085 0.088200 1.098774 11.00000 0.12752 0.11256 = 0.05097 0.02585 0.06231 0.05302 AFIX 43 H22 2 0.295672 0.100828 1.156454 11.00000 -1.20000 AFIX 0 C23 1 0.340176 -0.010028 1.085113 11.00000 0.10597 0.06904 = 0.03580 0.00838 0.03272 0.00839 AFIX 43 H23 2 0.366113 -0.067975 1.133265 11.00000 -1.20000 AFIX 0 C24 1 0.345007 -0.025169 0.998742 11.00000 0.05698 0.08499 = 0.05405 -0.02121 0.04018 0.00071 AFIX 43 H24 2 0.376916 -0.091050 0.991409 11.00000 -1.20000 AFIX 0 N1 3 0.057683 0.133894 0.583969 11.00000 0.03504 0.05136 = 0.03703 0.00471 0.00923 0.00081 P1 4 0.307808 0.039135 0.813140 11.00000 0.03653 0.03689 = 0.04034 0.00056 0.02077 -0.00024 CL1 5 0.113089 -0.071934 0.755292 11.00000 0.05595 0.04651 = 0.07958 0.00567 0.04430 -0.00472 CL2 5 0.229015 0.078767 0.496612 11.00000 0.08215 0.09864 = 0.07206 -0.01430 0.04654 0.00714 CL3 5 0.184206 0.406922 0.700653 11.00000 0.08570 0.06934 = 0.08083 -0.01936 0.04104 -0.01091 PD1 6 0.175702 0.075692 0.695506 11.00000 0.03391 0.04201 = 0.03935 0.00255 0.01754 -0.00148 TE1 7 0.215983 0.242329 0.606468 11.00000 0.03763 0.05165 = 0.04481 0.00763 0.01903 -0.00064 HKLF 4 REM PPP-2 REM R1 = 0.0720 for 1494 Fo > 4sig(Fo) and 0.3597 for all 5940 data REM 240 parameters refined using 132 restraints END WGHT 0.0052 0.0000 REM Highest difference peak 0.747, deepest hole -1.368, 1-sigma level 0.189 Q1 1 0.4205 -0.4587 0.8528 11.00000 0.05 0.75 Q2 1 0.3104 0.0372 0.8698 11.00000 0.05 0.74 Q3 1 0.4912 -0.3419 0.7908 11.00000 0.05 0.73 Q4 1 0.4849 -0.5068 0.7597 11.00000 0.05 0.71 Q5 1 0.0676 0.5673 0.4445 11.00000 0.05 0.71 Q6 1 0.5818 -0.4370 0.9520 11.00000 0.05 0.70 Q7 1 0.4693 0.3802 0.9014 11.00000 0.05 0.69 Q8 1 0.4625 -0.0603 0.8477 11.00000 0.05 0.69 Q9 1 0.2898 0.0253 0.7528 11.00000 0.05 0.68 Q10 1 0.4230 -0.5634 0.8134 11.00000 0.05 0.67 Q11 1 0.5023 0.2924 0.8605 11.00000 0.05 0.67 Q12 1 0.1919 0.3011 0.6470 11.00000 0.05 0.67 Q13 1 -0.0851 0.1188 0.4866 11.00000 0.05 0.66 Q14 1 -0.1957 0.3676 0.4086 11.00000 0.05 0.65 Q15 1 0.4424 0.2558 0.7526 11.00000 0.05 0.65 Q16 1 0.1882 0.5062 0.5772 11.00000 0.05 0.65 Q17 1 0.2696 0.3143 0.6639 11.00000 0.05 0.65 Q18 1 -0.0620 0.2664 0.3811 11.00000 0.05 0.65 Q19 1 0.3228 -0.2647 0.7653 11.00000 0.05 0.64 Q20 1 0.1832 0.3001 0.5617 11.00000 0.05 0.64 Q21 1 0.5937 -0.2737 0.9368 11.00000 0.05 0.63 Q22 1 0.2226 0.2314 0.7164 11.00000 0.05 0.63 Q23 1 0.4396 0.2250 1.0089 11.00000 0.05 0.63 Q24 1 0.2211 0.3886 0.5571 11.00000 0.05 0.63 Q25 1 0.2567 -0.5220 0.6424 11.00000 0.05 0.62 ; loop_ _restr_U_similar_atom_site_label_1 _restr_U_similar_atom_site_label_2 _restr_U_similar_atom_site_label_3 _restr_U_similar_atom_site_label_4 _restr_U_similar_atom_site_label_5 _restr_U_similar_atom_site_label_6 _restr_U_similar_weight_param C7 C8 C9 C10 C11 C12 . C13 C14 C15 C16 C17 C18 . C19 C20 C21 C22 C23 C24 . C1 C2 C3 C4 C5 . . _definition ; SIMU restraints were applied to carbon atoms of phenyl and pyridine rings to improve the quality of ellipsoid.i.e a total of 23 atom sites were restrained leading to 132 least square restraints. ; # Attachment 'new-rc-1.pdf' # 57 # 58 # 63 # 64 # 65 data_barc031 _database_code_depnum_ccdc_archive 'CCDC 864905' #TrackingRef '- new-clfixed-barc031.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C168 H162 Cl21 P12 Pd6 Te4' _chemical_formula_weight 4445.88 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' P P 0.1023 0.0942 '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' Te Te -0.5308 1.6751 '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 14.2448(4) _cell_length_b 18.8456(6) _cell_length_c 18.9875(5) _cell_angle_alpha 81.392(2) _cell_angle_beta 83.613(2) _cell_angle_gamma 69.894(3) _cell_volume 4722.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9827 _cell_measurement_theta_min 3.2867 _cell_measurement_theta_max 32.7265 _exptl_crystal_description thin-plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2206 _exptl_absorpt_coefficient_mu 1.623 _exptl_absorpt_correction_T_min 0.6164 _exptl_absorpt_correction_T_max 0.7268 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 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 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57192 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.1787 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 32.81 _reflns_number_total 31237 _reflns_number_gt 14708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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. data restr special details #TrackingRef '- new-clfixed-barc031.cif' _name 'DFIX DELU SIMU ISOR EADP' _category restr _type char _definition Total 165 restr is applied :The chloroform molcules were applied with following restraint DFIX DELU SIMU. The Cl1 was restraint by using ISOR and EADP. Electron density synthesis with coefficients Fo-Fc Highest peak 16.01 at 0.0000 0.0000 1.0000 [ 0.00 A from CL1 ] Deepest hole -6.58 at 0.1452 0.2232 0.4803 [ 0.05 A from CL2 ] Mean = 0.00, Rms deviation from mean = 0.27 e/A3 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(0.08(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0654+0.0000*P+(0.0607P)^2^+0.1401sin\q/\l] where P = 0.01559Fo^2^ + 0.98441Fc^2^ ; _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 31237 _refine_ls_number_parameters 1024 _refine_ls_number_restraints 106 _refine_ls_R_factor_all 0.1837 _refine_ls_R_factor_gt 0.0958 _refine_ls_wR_factor_ref 0.2258 _refine_ls_wR_factor_gt 0.1997 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.176 _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 Pd1 Pd 0.90361(4) 0.85400(4) 0.22489(3) 0.02498(15) Uani 1 1 d . . . Pd2 Pd 0.80766(4) 0.71291(4) 0.31053(3) 0.02648(15) Uani 1 1 d . . . Pd3 Pd 0.83190(4) 0.73367(4) 0.13174(4) 0.02831(16) Uani 1 1 d . . . Te1 Te 0.73391(4) 0.83206(3) 0.21934(3) 0.02559(13) Uani 1 1 d . . . Te2 Te 0.96491(4) 0.70715(3) 0.22430(3) 0.02800(14) Uani 1 1 d . . . Cl1 Cl 1.0000 1.0000 1.0000 0.0209(3) Uani 1 2 d S . . Cl2 Cl 0.85385(12) 0.77947(11) 0.52013(10) 0.0209(3) Uani 1 1 d . . . P1 P 1.06407(15) 0.85495(14) 0.22556(12) 0.0286(5) Uani 1 1 d . . . P2 P 0.82622(15) 0.98257(14) 0.22797(12) 0.0278(5) Uani 1 1 d . . . P3 P 0.65733(15) 0.73354(14) 0.37565(12) 0.0310(5) Uani 1 1 d . . . P4 P 0.89336(16) 0.60430(14) 0.38036(12) 0.0306(5) Uani 1 1 d . . . P5 P 0.70621(16) 0.76863(14) 0.05509(12) 0.0297(5) Uani 1 1 d . . . P6 P 0.93517(18) 0.64504(15) 0.06144(14) 0.0363(6) Uani 1 1 d . . . C1 C 1.0790(6) 0.9463(5) 0.1917(5) 0.034(2) Uani 1 1 d . . . H1A H 1.1481 0.9434 0.1986 0.040 Uiso 1 1 calc R . . H1B H 1.0701 0.9562 0.1398 0.040 Uiso 1 1 calc R . . C2 C 1.0071(6) 1.0115(5) 0.2268(5) 0.034(2) Uani 1 1 d . . . H2A H 1.0356 1.0532 0.2214 0.040 Uiso 1 1 calc R . . H2B H 0.9991 0.9950 0.2784 0.040 Uiso 1 1 calc R . . C3 C 0.9021(6) 1.0423(5) 0.1953(5) 0.034(2) Uani 1 1 d . . . H3A H 0.9108 1.0455 0.1426 0.041 Uiso 1 1 calc R . . H3B H 0.8665 1.0944 0.2081 0.041 Uiso 1 1 calc R . . C4 C 1.1597(6) 0.7901(6) 0.1725(5) 0.034(2) Uani 1 1 d . . . C5 C 1.1727(7) 0.8097(7) 0.0976(5) 0.045(3) Uani 1 1 d . . . H5 H 1.1337 0.8581 0.0757 0.054 Uiso 1 1 calc R . . C6 C 1.2412(7) 0.7589(7) 0.0569(6) 0.053(3) Uani 1 1 d . . . H6 H 1.2492 0.7717 0.0068 0.064 Uiso 1 1 calc R . . C7 C 1.2976(7) 0.6906(7) 0.0886(6) 0.051(3) Uani 1 1 d . . . H7 H 1.3479 0.6569 0.0606 0.061 Uiso 1 1 calc R . . C8 C 1.2839(7) 0.6692(6) 0.1592(7) 0.050(3) Uani 1 1 d . . . H8 H 1.3224 0.6197 0.1791 0.060 Uiso 1 1 calc R . . C9 C 1.2174(6) 0.7159(6) 0.2020(6) 0.044(2) Uani 1 1 d . . . H9 H 1.2090 0.6996 0.2514 0.052 Uiso 1 1 calc R . . C10 C 1.1113(6) 0.8359(5) 0.3145(5) 0.034(2) Uani 1 1 d . . . C11 C 1.2069(7) 0.8405(6) 0.3238(5) 0.040(2) Uani 1 1 d . . . H11 H 1.2492 0.8488 0.2833 0.048 Uiso 1 1 calc R . . C12 C 1.2378(6) 0.8332(6) 0.3909(6) 0.048(3) Uani 1 1 d . . . H12 H 1.3003 0.8383 0.3975 0.058 Uiso 1 1 calc R . . C13 C 1.1769(7) 0.8182(6) 0.4493(5) 0.044(3) Uani 1 1 d . . . H13 H 1.1986 0.8133 0.4959 0.052 Uiso 1 1 calc R . . C14 C 1.0871(7) 0.8104(6) 0.4421(5) 0.041(2) Uani 1 1 d . . . H14 H 1.0469 0.7995 0.4829 0.049 Uiso 1 1 calc R . . C15 C 1.0554(6) 0.8188(5) 0.3731(5) 0.033(2) Uani 1 1 d . . . H15 H 0.9935 0.8123 0.3672 0.039 Uiso 1 1 calc R . . C16 C 0.7820(6) 1.0092(5) 0.3159(4) 0.0259(18) Uani 1 1 d . . . C17 C 0.7979(6) 0.9559(6) 0.3747(5) 0.035(2) Uani 1 1 d . . . H17 H 0.8289 0.9035 0.3690 0.042 Uiso 1 1 calc R . . C18 C 0.7692(9) 0.9777(8) 0.4420(6) 0.058(3) Uani 1 1 d . . . H18 H 0.7834 0.9398 0.4820 0.070 Uiso 1 1 calc R . . C19 C 0.7203(8) 1.0530(8) 0.4535(6) 0.058(3) Uani 1 1 d . . . H19 H 0.6995 1.0670 0.5002 0.070 Uiso 1 1 calc R . . C20 C 0.7029(7) 1.1072(7) 0.3933(7) 0.056(3) Uani 1 1 d . . . H20 H 0.6701 1.1595 0.3986 0.067 Uiso 1 1 calc R . . C21 C 0.7335(7) 1.0847(6) 0.3264(6) 0.046(3) Uani 1 1 d . . . H21 H 0.7210 1.1222 0.2859 0.055 Uiso 1 1 calc R . . C22 C 0.7202(6) 1.0269(5) 0.1730(5) 0.033(2) Uani 1 1 d . . . C23 C 0.7343(7) 1.0419(6) 0.0996(5) 0.043(3) Uani 1 1 d . . . H23 H 0.8006 1.0285 0.0780 0.051 Uiso 1 1 calc R . . C24 C 0.6555(7) 1.0753(6) 0.0576(5) 0.044(2) Uani 1 1 d . . . H24 H 0.6667 1.0872 0.0076 0.053 Uiso 1 1 calc R . . C25 C 0.5578(7) 1.0920(7) 0.0887(6) 0.056(3) Uani 1 1 d . . . H25 H 0.5024 1.1146 0.0596 0.067 Uiso 1 1 calc R . . C26 C 0.5418(7) 1.0760(6) 0.1606(6) 0.048(3) Uani 1 1 d . . . H26 H 0.4751 1.0868 0.1809 0.057 Uiso 1 1 calc R . . C27 C 0.6203(6) 1.0445(6) 0.2042(5) 0.041(2) Uani 1 1 d . . . H27 H 0.6082 1.0346 0.2544 0.049 Uiso 1 1 calc R . . C28 C 0.6732(6) 0.6969(6) 0.4727(5) 0.045(3) Uani 1 1 d . . . H28A H 0.7088 0.7247 0.4937 0.054 Uiso 1 1 calc R . . H28B H 0.6066 0.7058 0.4985 0.054 Uiso 1 1 calc R . . C29 C 0.7329(6) 0.6116(5) 0.4810(5) 0.036(2) Uani 1 1 d . . . H29A H 0.7156 0.5874 0.4438 0.043 Uiso 1 1 calc R . . H29B H 0.7142 0.5880 0.5282 0.043 Uiso 1 1 calc R . . C30 C 0.8448(6) 0.5970(6) 0.4748(5) 0.041(2) Uani 1 1 d . . . H30A H 0.8796 0.5455 0.4987 0.049 Uiso 1 1 calc R . . H30B H 0.8594 0.6344 0.4994 0.049 Uiso 1 1 calc R . . C31 C 0.5773(6) 0.8312(6) 0.3769(5) 0.035(2) Uani 1 1 d . . . C32 C 0.5982(7) 0.8801(6) 0.4169(6) 0.047(3) Uani 1 1 d . . . H32 H 0.6533 0.8608 0.4463 0.056 Uiso 1 1 calc R . . C33 C 0.5409(8) 0.9549(8) 0.4143(7) 0.063(3) Uani 1 1 d . . . H33 H 0.5562 0.9869 0.4422 0.076 Uiso 1 1 calc R . . C34 C 0.4605(9) 0.9849(7) 0.3716(8) 0.069(4) Uani 1 1 d . . . H34 H 0.4202 1.0369 0.3710 0.083 Uiso 1 1 calc R . . C35 C 0.4387(7) 0.9388(7) 0.3297(7) 0.061(3) Uani 1 1 d . . . H35 H 0.3838 0.9595 0.3000 0.074 Uiso 1 1 calc R . . C36 C 0.4950(7) 0.8652(7) 0.3309(6) 0.047(3) Uani 1 1 d . . . H36 H 0.4805 0.8347 0.3010 0.057 Uiso 1 1 calc R . . C37 C 0.5764(6) 0.6867(6) 0.3478(5) 0.034(2) Uani 1 1 d . . . C38 C 0.4946(7) 0.6828(7) 0.3924(6) 0.059(3) Uani 1 1 d . . . H38 H 0.4812 0.7026 0.4370 0.071 Uiso 1 1 calc R . . C39 C 0.4312(10) 0.6482(9) 0.3695(8) 0.081(5) Uani 1 1 d . . . H39 H 0.3745 0.6445 0.3993 0.098 Uiso 1 1 calc R . . C40 C 0.4502(9) 0.6201(7) 0.3054(7) 0.063(4) Uani 1 1 d . . . H40 H 0.4059 0.5985 0.2899 0.076 Uiso 1 1 calc R . . C41 C 0.5343(9) 0.6232(7) 0.2629(6) 0.060(3) Uani 1 1 d . . . H41 H 0.5501 0.6013 0.2193 0.072 Uiso 1 1 calc R . . C42 C 0.5946(7) 0.6576(6) 0.2837(6) 0.049(3) Uani 1 1 d . . . H42 H 0.6505 0.6615 0.2531 0.059 Uiso 1 1 calc R . . C43 C 0.8907(7) 0.5179(5) 0.3513(5) 0.039(2) Uani 1 1 d . . . C44 C 0.8326(6) 0.5204(6) 0.2974(5) 0.039(2) Uani 1 1 d . . . H44 H 0.7958 0.5686 0.2740 0.047 Uiso 1 1 calc R . . C45 C 0.8251(8) 0.4555(7) 0.2755(6) 0.052(3) Uani 1 1 d . . . H45 H 0.7864 0.4587 0.2368 0.063 Uiso 1 1 calc R . . C46 C 0.8765(8) 0.3856(7) 0.3125(6) 0.054(3) Uani 1 1 d . . . H46 H 0.8700 0.3403 0.3005 0.065 Uiso 1 1 calc R . . C47 C 0.9366(9) 0.3811(7) 0.3663(6) 0.055(3) Uani 1 1 d . . . H47 H 0.9725 0.3331 0.3907 0.066 Uiso 1 1 calc R . . C48 C 0.9435(7) 0.4461(6) 0.3837(5) 0.044(2) Uani 1 1 d . . . H48 H 0.9867 0.4425 0.4198 0.053 Uiso 1 1 calc R . . C49 C 1.0270(6) 0.5882(5) 0.3871(5) 0.0302(19) Uani 1 1 d . . . C50 C 1.0988(7) 0.5429(6) 0.3422(5) 0.039(2) Uani 1 1 d . . . H50 H 1.0786 0.5187 0.3091 0.047 Uiso 1 1 calc R . . C51 C 1.1973(7) 0.5327(6) 0.3448(6) 0.042(2) Uani 1 1 d . . . H51 H 1.2458 0.5018 0.3136 0.051 Uiso 1 1 calc R . . C52 C 1.2269(7) 0.5681(6) 0.3938(6) 0.047(3) Uani 1 1 d . . . H52 H 1.2959 0.5602 0.3970 0.056 Uiso 1 1 calc R . . C53 C 1.1554(7) 0.6148(6) 0.4377(6) 0.047(3) Uani 1 1 d . . . H53 H 1.1754 0.6393 0.4706 0.056 Uiso 1 1 calc R . . C54 C 1.0557(7) 0.6255(6) 0.4338(5) 0.039(2) Uani 1 1 d . . . H54 H 1.0066 0.6585 0.4630 0.046 Uiso 1 1 calc R . . C55 C 0.8717(7) 0.5918(6) 0.0239(5) 0.041(2) Uani 1 1 d . . . H55A H 0.9216 0.5547 -0.0049 0.049 Uiso 1 1 calc R . . H55B H 0.8443 0.5626 0.0635 0.049 Uiso 1 1 calc R . . C56 C 0.7859(7) 0.6410(6) -0.0233(6) 0.049(3) Uani 1 1 d . . . H56A H 0.8107 0.6755 -0.0589 0.059 Uiso 1 1 calc R . . H56B H 0.7661 0.6073 -0.0495 0.059 Uiso 1 1 calc R . . C57 C 0.6926(7) 0.6890(6) 0.0189(5) 0.042(2) Uani 1 1 d . . . H57A H 0.6741 0.6551 0.0589 0.050 Uiso 1 1 calc R . . H57B H 0.6364 0.7089 -0.0129 0.050 Uiso 1 1 calc R . . C58 C 0.5795(6) 0.8183(6) 0.0892(5) 0.034(2) Uani 1 1 d . . . C59 C 0.5439(6) 0.8957(6) 0.0887(5) 0.039(2) Uani 1 1 d . . . H59 H 0.5858 0.9243 0.0684 0.047 Uiso 1 1 calc R . . C60 C 0.4502(7) 0.9331(6) 0.1164(5) 0.047(3) Uani 1 1 d . . . H60 H 0.4271 0.9869 0.1155 0.056 Uiso 1 1 calc R . . C61 C 0.3893(7) 0.8908(7) 0.1460(6) 0.048(3) Uani 1 1 d . . . H61 H 0.3238 0.9160 0.1653 0.058 Uiso 1 1 calc R . . C62 C 0.4215(7) 0.8162(7) 0.1475(6) 0.053(3) Uani 1 1 d . . . H62 H 0.3790 0.7882 0.1682 0.063 Uiso 1 1 calc R . . C63 C 0.5185(7) 0.7772(6) 0.1185(5) 0.045(3) Uani 1 1 d . . . H63 H 0.5411 0.7234 0.1192 0.054 Uiso 1 1 calc R . . C70 C 0.9920(6) 0.6899(6) -0.0153(5) 0.039(2) Uani 1 1 d U . . C71 C 1.0213(10) 0.6585(8) -0.0773(7) 0.078(4) Uani 1 1 d U . . H71 H 1.0112 0.6121 -0.0816 0.093 Uiso 1 1 calc R . . C72 C 1.0653(13) 0.6926(9) -0.1341(8) 0.110(7) Uani 1 1 d . . . H72 H 1.0870 0.6702 -0.1772 0.132 Uiso 1 1 calc R . . C73 C 1.0773(10) 0.7621(8) -0.1260(7) 0.081(5) Uani 1 1 d . . . H73 H 1.1078 0.7864 -0.1647 0.097 Uiso 1 1 calc R . . C74 C 1.0481(8) 0.7940(7) -0.0677(6) 0.054(3) Uani 1 1 d . . . H74 H 1.0548 0.8418 -0.0643 0.064 Uiso 1 1 calc R . . C75 C 1.0071(6) 0.7571(6) -0.0105(5) 0.041(2) Uani 1 1 d . . . H75 H 0.9889 0.7788 0.0332 0.049 Uiso 1 1 calc R . . C76 C 1.0386(7) 0.5691(6) 0.1042(5) 0.043(2) Uani 1 1 d . . . C77 C 1.1384(8) 0.5692(7) 0.0896(7) 0.063(3) Uani 1 1 d . . . H77 H 1.1539 0.6072 0.0565 0.076 Uiso 1 1 calc R . . C78 C 1.2118(8) 0.5114(7) 0.1257(7) 0.065(4) Uani 1 1 d . . . H78 H 1.2790 0.5107 0.1168 0.078 Uiso 1 1 calc R . . C79 C 1.1937(9) 0.4562(8) 0.1728(6) 0.064(3) Uani 1 1 d . . . H79 H 1.2469 0.4177 0.1964 0.077 Uiso 1 1 calc R . . C80 C 1.0973(11) 0.4564(8) 0.1861(6) 0.072(4) Uani 1 1 d . . . H80 H 1.0837 0.4180 0.2198 0.086 Uiso 1 1 calc R . . C81 C 1.0188(8) 0.5116(6) 0.1515(6) 0.049(3) Uani 1 1 d . . . H81 H 0.9525 0.5100 0.1600 0.059 Uiso 1 1 calc R . . C111 C 0.0696(10) 1.1314(10) 0.3626(8) 0.060(5) Uani 0.531(9) 1 d PDU A 1 H111 H 0.0841 1.1582 0.3996 0.072 Uiso 0.531(9) 1 calc PR A 1 Cl11 Cl -0.0363(8) 1.1097(9) 0.3902(6) 0.151(8) Uani 0.531(9) 1 d PDU A 1 Cl22 Cl 0.1753(7) 1.0601(8) 0.3414(6) 0.068(3) Uani 0.531(9) 1 d PDU A 1 Cl33 Cl 0.0556(7) 1.1894(5) 0.2834(4) 0.106(4) Uani 0.531(9) 1 d PDU A 1 C101 C 0.0584(12) 1.1018(11) 0.3942(12) 0.059(8) Uani 0.469(9) 1 d PD A 2 H101 H 0.0728 1.1278 0.4319 0.071 Uiso 0.469(9) 1 calc PR A 2 Cl1A Cl 0.1700(12) 1.0505(10) 0.3572(9) 0.138(8) Uani 0.469(9) 1 d PDU A 2 Cl2A Cl 0.0183(6) 1.0308(6) 0.4368(5) 0.086(3) Uani 0.469(9) 1 d PDU A 2 Cl3A Cl -0.0333(7) 1.1675(4) 0.3468(5) 0.084(4) Uani 0.469(9) 1 d PDU A 2 C222 C 0.3229(13) 1.2484(8) 0.3431(8) 0.079(7) Uani 0.636(9) 1 d PDU B 1 H222 H 0.2768 1.2273 0.3764 0.095 Uiso 0.636(9) 1 calc PR B 1 Cl44 Cl 0.4396(5) 1.1963(4) 0.3701(5) 0.129(4) Uani 0.636(9) 1 d PDU B 1 Cl55 Cl 0.3047(10) 1.2315(7) 0.2603(5) 0.163(5) Uani 0.636(9) 1 d PD B 1 Cl66 Cl 0.2780(10) 1.3446(6) 0.3498(6) 0.083(3) Uani 0.636(9) 1 d PDU B 1 C201 C 0.2489(16) 1.2544(13) 0.3281(12) 0.060(9) Uani 0.364(9) 1 d PDU B 2 H201 H 0.2181 1.2370 0.3744 0.072 Uiso 0.364(9) 1 calc PR B 2 Cl4A Cl 0.1706(9) 1.2637(6) 0.2602(6) 0.095(5) Uani 0.364(9) 1 d PDU B 2 Cl5A Cl 0.3664(12) 1.1881(9) 0.3123(10) 0.133(6) Uani 0.364(9) 1 d PDU B 2 Cl6A Cl 0.268(3) 1.3399(17) 0.3358(16) 0.195(17) Uani 0.364(9) 1 d PDU B 2 C333 C 0.6032(7) 0.4076(6) 0.3846(7) 0.074(3) Uani 1 1 d DU . . H333 H 0.6182 0.4239 0.3332 0.088 Uiso 1 1 calc R . . Cl77 Cl 0.4829(3) 0.4104(3) 0.3968(3) 0.1109(16) Uani 1 1 d DU . . Cl88 Cl 0.6817(3) 0.3165(3) 0.4079(5) 0.213(4) Uani 1 1 d DU . . Cl99 Cl 0.6291(4) 0.4648(4) 0.4370(3) 0.136(2) Uani 1 1 d DU . . C64 C 0.7308(6) 0.8311(5) -0.0196(5) 0.035(2) Uani 1 1 d . . . C65 C 0.7077(6) 0.8301(6) -0.0895(5) 0.036(2) Uani 1 1 d . . . H65 H 0.6719 0.7980 -0.0975 0.044 Uiso 1 1 calc R . . C69 C 0.7794(6) 0.8822(6) -0.0115(5) 0.042(2) Uani 1 1 d . . . H69 H 0.7941 0.8859 0.0352 0.051 Uiso 1 1 calc R . . C66 C 0.7361(7) 0.8751(6) -0.1470(5) 0.041(2) Uani 1 1 d . . . H66 H 0.7205 0.8737 -0.1940 0.049 Uiso 1 1 calc R . . C68 C 0.8067(6) 0.9270(6) -0.0675(6) 0.041(2) Uani 1 1 d . . . H68 H 0.8389 0.9616 -0.0602 0.050 Uiso 1 1 calc R . . C67 C 0.7864(6) 0.9207(6) -0.1349(5) 0.040(2) Uani 1 1 d . . . H67 H 0.8085 0.9496 -0.1745 0.048 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 0.0230(3) 0.0287(4) 0.0246(3) -0.0012(3) -0.0027(2) -0.0109(3) Pd2 0.0254(3) 0.0290(4) 0.0264(4) 0.0003(3) -0.0031(2) -0.0119(3) Pd3 0.0291(3) 0.0291(4) 0.0281(4) -0.0042(3) -0.0024(2) -0.0111(3) Te1 0.0240(3) 0.0279(3) 0.0257(3) -0.0008(2) -0.00304(19) -0.0103(2) Te2 0.0252(3) 0.0283(3) 0.0301(3) 0.0000(2) -0.0023(2) -0.0097(2) Cl1 0.0194(7) 0.0273(9) 0.0203(8) -0.0076(6) -0.0036(5) -0.0104(6) Cl2 0.0194(7) 0.0273(9) 0.0203(8) -0.0076(6) -0.0036(5) -0.0104(6) P1 0.0224(10) 0.0342(14) 0.0300(13) -0.0013(10) -0.0024(8) -0.0112(9) P2 0.0266(11) 0.0292(13) 0.0284(12) -0.0008(10) -0.0041(8) -0.0108(9) P3 0.0263(11) 0.0372(15) 0.0318(13) -0.0010(11) -0.0018(8) -0.0146(10) P4 0.0310(11) 0.0314(14) 0.0305(13) 0.0016(10) -0.0051(9) -0.0132(10) P5 0.0293(11) 0.0322(14) 0.0303(13) -0.0044(10) -0.0027(8) -0.0130(10) P6 0.0420(13) 0.0304(14) 0.0358(14) -0.0076(11) -0.0008(10) -0.0099(11) C1 0.023(4) 0.041(6) 0.039(5) 0.004(4) -0.004(3) -0.017(4) C2 0.034(5) 0.040(6) 0.038(5) -0.009(4) -0.006(4) -0.023(4) C3 0.030(4) 0.039(6) 0.038(5) -0.002(4) -0.004(4) -0.016(4) C4 0.025(4) 0.049(6) 0.032(5) -0.004(4) -0.003(3) -0.015(4) C5 0.043(5) 0.062(8) 0.030(5) 0.002(5) -0.010(4) -0.018(5) C6 0.050(6) 0.057(8) 0.045(7) -0.027(6) 0.011(5) -0.004(5) C7 0.038(6) 0.052(8) 0.062(8) -0.023(6) 0.001(5) -0.010(5) C8 0.038(5) 0.039(7) 0.076(9) -0.008(6) -0.015(5) -0.012(5) C9 0.031(5) 0.042(7) 0.058(7) -0.013(5) -0.001(4) -0.010(4) C10 0.033(5) 0.027(5) 0.043(6) -0.009(4) -0.002(4) -0.009(4) C11 0.040(5) 0.053(7) 0.037(6) -0.010(5) -0.004(4) -0.026(5) C12 0.026(5) 0.056(7) 0.061(7) 0.003(6) -0.012(4) -0.012(4) C13 0.043(5) 0.057(7) 0.031(5) -0.001(5) -0.017(4) -0.014(5) C14 0.037(5) 0.047(7) 0.038(6) -0.008(5) 0.002(4) -0.014(4) C15 0.024(4) 0.038(6) 0.034(5) 0.000(4) 0.000(3) -0.012(4) C16 0.027(4) 0.030(5) 0.026(5) -0.001(4) 0.001(3) -0.017(4) C17 0.041(5) 0.031(5) 0.032(5) -0.004(4) 0.001(4) -0.012(4) C18 0.085(8) 0.067(9) 0.037(7) 0.009(6) -0.019(6) -0.047(7) C19 0.078(8) 0.068(9) 0.039(7) -0.019(6) -0.003(5) -0.032(7) C20 0.052(6) 0.049(8) 0.068(9) -0.025(7) 0.005(5) -0.015(5) C21 0.045(6) 0.052(7) 0.040(6) -0.007(5) -0.002(4) -0.016(5) C22 0.028(4) 0.031(5) 0.045(6) -0.004(4) -0.008(4) -0.012(4) C23 0.032(5) 0.063(8) 0.035(6) 0.000(5) -0.002(4) -0.021(5) C24 0.056(6) 0.049(7) 0.028(5) -0.008(5) -0.009(4) -0.016(5) C25 0.044(6) 0.066(9) 0.061(8) -0.001(6) -0.032(5) -0.017(5) C26 0.030(5) 0.056(8) 0.055(7) -0.013(6) -0.012(4) -0.007(5) C27 0.035(5) 0.042(6) 0.042(6) -0.010(5) 0.001(4) -0.009(4) C28 0.026(4) 0.063(8) 0.046(6) 0.010(5) -0.001(4) -0.023(5) C29 0.030(4) 0.038(6) 0.044(6) 0.001(5) -0.005(4) -0.019(4) C30 0.042(5) 0.037(6) 0.044(6) 0.001(5) 0.002(4) -0.019(4) C31 0.025(4) 0.042(6) 0.038(5) 0.004(4) 0.007(3) -0.018(4) C32 0.036(5) 0.050(7) 0.063(7) -0.013(6) -0.005(5) -0.023(5) C33 0.057(7) 0.068(9) 0.070(9) -0.032(7) 0.009(6) -0.022(6) C34 0.059(8) 0.043(8) 0.094(11) -0.015(7) 0.013(7) -0.005(6) C35 0.035(6) 0.059(9) 0.075(9) 0.004(7) 0.001(5) -0.004(5) C36 0.041(6) 0.052(7) 0.051(7) -0.004(6) -0.001(4) -0.021(5) C37 0.039(5) 0.040(6) 0.029(5) 0.004(4) -0.006(4) -0.022(4) C38 0.045(6) 0.093(10) 0.054(7) -0.013(7) 0.007(5) -0.044(6) C39 0.079(9) 0.099(12) 0.088(11) 0.020(9) -0.018(8) -0.064(9) C40 0.081(8) 0.064(9) 0.062(8) 0.013(7) -0.034(7) -0.047(7) C41 0.081(8) 0.079(9) 0.044(7) 0.014(6) -0.021(6) -0.060(7) C42 0.048(6) 0.047(7) 0.055(7) 0.000(6) -0.008(5) -0.022(5) C43 0.051(6) 0.027(5) 0.040(6) -0.002(4) 0.005(4) -0.018(4) C44 0.038(5) 0.044(6) 0.036(6) -0.006(5) -0.003(4) -0.012(4) C45 0.074(7) 0.045(7) 0.048(7) -0.007(6) -0.014(5) -0.029(6) C46 0.080(8) 0.048(8) 0.041(7) -0.005(6) 0.001(5) -0.031(6) C47 0.088(8) 0.039(7) 0.042(7) -0.007(5) -0.005(6) -0.026(6) C48 0.057(6) 0.041(7) 0.033(6) 0.002(5) -0.010(4) -0.017(5) C49 0.037(5) 0.027(5) 0.027(5) 0.002(4) -0.002(3) -0.013(4) C50 0.045(5) 0.041(6) 0.036(6) -0.003(5) -0.005(4) -0.019(5) C51 0.035(5) 0.041(6) 0.050(7) -0.006(5) 0.000(4) -0.012(4) C52 0.033(5) 0.048(7) 0.060(7) 0.000(6) 0.002(4) -0.017(5) C53 0.035(5) 0.043(7) 0.067(8) -0.003(6) -0.014(5) -0.018(5) C54 0.047(5) 0.046(6) 0.032(5) 0.006(5) -0.011(4) -0.029(5) C55 0.050(6) 0.033(6) 0.041(6) -0.014(5) 0.004(4) -0.013(4) C56 0.053(6) 0.040(7) 0.056(7) -0.018(6) -0.014(5) -0.009(5) C57 0.046(5) 0.055(7) 0.034(6) -0.009(5) -0.003(4) -0.027(5) C58 0.027(4) 0.048(6) 0.029(5) -0.003(4) -0.005(3) -0.015(4) C59 0.019(4) 0.050(7) 0.054(6) 0.001(5) -0.005(4) -0.022(4) C60 0.034(5) 0.052(7) 0.055(7) -0.001(6) -0.007(4) -0.016(5) C61 0.035(5) 0.048(7) 0.061(7) -0.001(6) -0.001(4) -0.017(5) C62 0.030(5) 0.065(8) 0.064(8) 0.002(6) 0.008(4) -0.025(5) C63 0.039(5) 0.046(7) 0.052(7) 0.008(5) -0.004(4) -0.023(5) C70 0.037(5) 0.041(6) 0.037(5) -0.009(5) 0.003(4) -0.009(4) C71 0.121(11) 0.063(9) 0.061(8) -0.030(7) 0.036(8) -0.049(8) C72 0.197(17) 0.095(13) 0.068(10) -0.064(9) 0.080(11) -0.090(13) C73 0.108(11) 0.061(10) 0.062(9) -0.003(8) 0.040(8) -0.028(8) C74 0.062(7) 0.050(8) 0.054(8) -0.008(6) 0.002(5) -0.026(6) C75 0.041(5) 0.049(7) 0.034(6) -0.008(5) -0.001(4) -0.016(5) C76 0.047(6) 0.030(6) 0.045(6) -0.012(5) 0.005(4) -0.004(4) C77 0.062(7) 0.047(8) 0.082(10) -0.009(7) -0.017(6) -0.014(6) C78 0.046(6) 0.056(9) 0.087(10) -0.022(8) -0.023(6) 0.001(6) C79 0.061(8) 0.068(10) 0.048(8) -0.005(7) -0.016(6) 0.001(6) C80 0.118(11) 0.056(9) 0.021(6) -0.006(6) -0.016(6) 0.001(7) C81 0.066(7) 0.032(6) 0.040(6) -0.010(5) 0.001(5) -0.004(5) C111 0.071(11) 0.083(17) 0.047(12) -0.047(9) 0.004(10) -0.037(9) Cl11 0.137(9) 0.241(19) 0.151(11) -0.136(13) 0.085(8) -0.143(12) Cl22 0.061(5) 0.099(8) 0.051(5) -0.016(5) 0.009(4) -0.036(5) Cl33 0.153(8) 0.071(6) 0.074(5) -0.030(4) -0.021(5) 0.002(5) C101 0.059(17) 0.07(2) 0.037(16) -0.026(14) -0.010(11) 0.003(14) Cl1A 0.181(14) 0.092(10) 0.092(10) -0.054(8) -0.095(9) 0.061(9) Cl2A 0.101(6) 0.084(7) 0.092(6) -0.029(5) 0.011(5) -0.051(5) Cl3A 0.091(6) 0.047(5) 0.111(8) -0.019(5) -0.062(6) 0.004(4) C222 0.098(18) 0.051(14) 0.083(17) -0.022(12) 0.027(14) -0.023(14) Cl44 0.084(5) 0.081(5) 0.211(10) -0.041(6) 0.013(5) -0.011(4) Cl55 0.268(15) 0.157(10) 0.107(7) -0.083(7) 0.020(8) -0.108(10) Cl66 0.174(8) 0.049(5) 0.027(4) -0.001(3) -0.003(4) -0.040(5) C201 0.12(3) 0.025(15) 0.024(15) -0.001(12) 0.011(17) -0.021(18) Cl4A 0.146(11) 0.056(7) 0.069(7) -0.013(6) -0.014(6) -0.011(6) Cl5A 0.146(13) 0.097(12) 0.133(15) -0.017(10) -0.014(10) -0.008(9) Cl6A 0.41(4) 0.097(17) 0.055(14) -0.029(11) -0.025(16) -0.05(2) C333 0.050(6) 0.061(7) 0.104(11) 0.006(7) 0.000(6) -0.020(5) Cl77 0.059(2) 0.125(4) 0.154(4) 0.018(3) -0.014(2) -0.049(2) Cl88 0.082(3) 0.064(3) 0.461(13) 0.039(5) 0.001(5) -0.018(2) Cl99 0.168(4) 0.165(5) 0.117(4) -0.007(4) -0.035(3) -0.106(4) C64 0.022(4) 0.030(5) 0.046(6) -0.005(4) -0.003(3) 0.001(3) C65 0.035(5) 0.047(6) 0.031(5) -0.010(5) -0.002(4) -0.017(4) C69 0.041(5) 0.053(7) 0.043(6) -0.002(5) -0.023(4) -0.023(5) C66 0.045(5) 0.056(7) 0.026(5) -0.004(5) -0.002(4) -0.023(5) C68 0.028(5) 0.041(6) 0.057(7) 0.005(5) -0.002(4) -0.019(4) C67 0.037(5) 0.036(6) 0.046(6) 0.000(5) 0.002(4) -0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.293(2) . ? Pd1 P2 2.298(2) . ? Pd1 Te2 2.6013(9) . ? Pd1 Te1 2.6045(7) . ? Pd2 P3 2.291(2) . ? Pd2 P4 2.295(2) . ? Pd2 Te1 2.6005(8) . ? Pd2 Te2 2.6038(8) . ? Pd3 P5 2.289(2) . ? Pd3 P6 2.297(3) . ? Pd3 Te2 2.5989(8) . ? Pd3 Te1 2.6037(9) . ? P1 C4 1.811(10) . ? P1 C1 1.820(9) . ? P1 C10 1.827(10) . ? P2 C16 1.799(9) . ? P2 C22 1.814(9) . ? P2 C3 1.816(8) . ? P3 C31 1.804(10) . ? P3 C37 1.834(9) . ? P3 C28 1.878(10) . ? P4 C43 1.809(10) . ? P4 C49 1.838(8) . ? P4 C30 1.851(9) . ? P5 C64 1.788(9) . ? P5 C58 1.820(9) . ? P5 C57 1.817(10) . ? P6 C70 1.825(10) . ? P6 C55 1.820(10) . ? P6 C76 1.829(10) . ? C1 C2 1.493(13) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.559(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C9 1.422(13) . ? C4 C5 1.424(12) . ? C5 C6 1.370(14) . ? C5 H5 0.9500 . ? C6 C7 1.352(15) . ? C6 H6 0.9500 . ? C7 C8 1.355(15) . ? C7 H7 0.9500 . ? C8 C9 1.342(14) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.360(11) . ? C10 C11 1.426(11) . ? C11 C12 1.366(13) . ? C11 H11 0.9500 . ? C12 C13 1.387(13) . ? C12 H12 0.9500 . ? C13 C14 1.362(12) . ? C13 H13 0.9500 . ? C14 C15 1.402(13) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.367(12) . ? C16 C21 1.386(13) . ? C17 C18 1.376(14) . ? C17 H17 0.9500 . ? C18 C19 1.389(17) . ? C18 H18 0.9500 . ? C19 C20 1.396(16) . ? C19 H19 0.9500 . ? C20 C21 1.378(14) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.386(13) . ? C22 C27 1.425(11) . ? C23 C24 1.363(13) . ? C23 H23 0.9500 . ? C24 C25 1.398(14) . ? C24 H24 0.9500 . ? C25 C26 1.364(14) . ? C25 H25 0.9500 . ? C26 C27 1.377(13) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.532(14) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.515(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.401(14) . ? C31 C36 1.446(13) . ? C32 C33 1.361(16) . ? C32 H32 0.9500 . ? C33 C34 1.383(17) . ? C33 H33 0.9500 . ? C34 C35 1.390(17) . ? C34 H34 0.9500 . ? C35 C36 1.341(15) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.372(14) . ? C37 C38 1.379(12) . ? C38 C39 1.417(16) . ? C38 H38 0.9500 . ? C39 C40 1.363(18) . ? C39 H39 0.9500 . ? C40 C41 1.381(15) . ? C40 H40 0.9500 . ? C41 C42 1.358(13) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48 1.389(13) . ? C43 C44 1.372(13) . ? C44 C45 1.390(14) . ? C44 H44 0.9500 . ? C45 C46 1.393(15) . ? C45 H45 0.9500 . ? C46 C47 1.379(15) . ? C46 H46 0.9500 . ? C47 C48 1.355(14) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.387(13) . ? C49 C54 1.383(12) . ? C50 C51 1.354(12) . ? C50 H50 0.9500 . ? C51 C52 1.398(14) . ? C51 H51 0.9500 . ? C52 C53 1.385(14) . ? C52 H52 0.9500 . ? C53 C54 1.372(11) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.539(13) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.542(13) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C63 1.375(11) . ? C58 C59 1.368(13) . ? C59 C60 1.365(13) . ? C59 H59 0.9500 . ? C60 C61 1.391(13) . ? C60 H60 0.9500 . ? C61 C62 1.318(15) . ? C61 H61 0.9500 . ? C62 C63 1.417(13) . ? C62 H62 0.9500 . ? C63 H63 0.9500 . ? C70 C71 1.358(15) . ? C70 C75 1.372(14) . ? C71 C72 1.375(16) . ? C71 H71 0.9500 . ? C72 C73 1.408(18) . ? C72 H72 0.9500 . ? C73 C74 1.300(16) . ? C73 H73 0.9500 . ? C74 C75 1.385(13) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C81 1.387(14) . ? C76 C77 1.417(14) . ? C77 C78 1.379(15) . ? C77 H77 0.9500 . ? C78 C79 1.342(16) . ? C78 H78 0.9500 . ? C79 C80 1.368(16) . ? C79 H79 0.9500 . ? C80 C81 1.387(15) . ? C80 H80 0.9500 . ? C81 H81 0.9500 . ? C111 Cl22 1.694(12) . ? C111 Cl11 1.704(12) . ? C111 Cl33 1.709(12) . ? C111 H111 1.0000 . ? C101 Cl1A 1.690(16) . ? C101 Cl2A 1.693(17) . ? C101 Cl3A 1.693(15) . ? C101 H101 1.0000 . ? C222 Cl44 1.705(14) . ? C222 Cl55 1.714(12) . ? C222 Cl66 1.723(10) . ? C222 H222 1.0000 . ? C201 Cl5A 1.737(18) . ? C201 Cl6A 1.752(18) . ? C201 Cl4A 1.747(17) . ? C201 H201 1.0000 . ? C333 Cl88 1.719(11) . ? C333 Cl99 1.721(12) . ? C333 Cl77 1.688(9) . ? C333 H333 1.0000 . ? C64 C69 1.399(12) . ? C64 C65 1.407(13) . ? C65 C66 1.392(12) . ? C65 H65 0.9500 . ? C69 C68 1.364(12) . ? C69 H69 0.9500 . ? C66 C67 1.351(13) . ? C66 H66 0.9500 . ? C68 C67 1.373(14) . ? C68 H68 0.9500 . ? C67 H67 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P2 96.11(8) . . ? P1 Pd1 Te2 92.21(7) . . ? P2 Pd1 Te2 171.59(6) . . ? P1 Pd1 Te1 171.37(7) . . ? P2 Pd1 Te1 92.34(5) . . ? Te2 Pd1 Te1 79.39(2) . . ? P3 Pd2 P4 96.01(8) . . ? P3 Pd2 Te1 92.20(6) . . ? P4 Pd2 Te1 171.75(6) . . ? P3 Pd2 Te2 171.61(7) . . ? P4 Pd2 Te2 92.38(6) . . ? Te1 Pd2 Te2 79.41(2) . . ? P5 Pd3 P6 91.85(9) . . ? P5 Pd3 Te2 174.05(7) . . ? P6 Pd3 Te2 93.82(7) . . ? P5 Pd3 Te1 94.83(7) . . ? P6 Pd3 Te1 173.12(7) . . ? Te2 Pd3 Te1 79.44(3) . . ? Pd2 Te1 Pd3 80.17(3) . . ? Pd2 Te1 Pd1 84.69(2) . . ? Pd3 Te1 Pd1 85.54(2) . . ? Pd3 Te2 Pd2 80.20(2) . . ? Pd3 Te2 Pd1 85.71(3) . . ? Pd2 Te2 Pd1 84.68(3) . . ? C4 P1 C1 102.5(4) . . ? C4 P1 C10 105.2(4) . . ? C1 P1 C10 102.6(4) . . ? C4 P1 Pd1 116.7(3) . . ? C1 P1 Pd1 114.0(3) . . ? C10 P1 Pd1 114.1(3) . . ? C16 P2 C22 105.9(4) . . ? C16 P2 C3 102.9(4) . . ? C22 P2 C3 100.4(4) . . ? C16 P2 Pd1 114.2(3) . . ? C22 P2 Pd1 115.6(3) . . ? C3 P2 Pd1 116.2(3) . . ? C31 P3 C37 103.8(4) . . ? C31 P3 C28 103.7(5) . . ? C37 P3 C28 104.4(4) . . ? C31 P3 Pd2 116.7(3) . . ? C37 P3 Pd2 114.5(3) . . ? C28 P3 Pd2 112.4(3) . . ? C43 P4 C49 104.5(4) . . ? C43 P4 C30 102.8(4) . . ? C49 P4 C30 103.2(4) . . ? C43 P4 Pd2 113.6(3) . . ? C49 P4 Pd2 116.0(3) . . ? C30 P4 Pd2 115.2(3) . . ? C64 P5 C58 105.0(4) . . ? C64 P5 C57 106.5(5) . . ? C58 P5 C57 103.1(4) . . ? C64 P5 Pd3 110.0(3) . . ? C58 P5 Pd3 117.8(3) . . ? C57 P5 Pd3 113.6(3) . . ? C70 P6 C55 105.2(5) . . ? C70 P6 C76 106.0(4) . . ? C55 P6 C76 102.3(5) . . ? C70 P6 Pd3 111.3(3) . . ? C55 P6 Pd3 114.1(3) . . ? C76 P6 Pd3 116.9(3) . . ? C2 C1 P1 113.8(6) . . ? C2 C1 H1A 108.8 . . ? P1 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? P1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C1 C2 C3 113.2(7) . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2B 108.9 . . ? C3 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C2 C3 P2 112.4(6) . . ? C2 C3 H3A 109.1 . . ? P2 C3 H3A 109.1 . . ? C2 C3 H3B 109.1 . . ? P2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C9 C4 C5 117.5(9) . . ? C9 C4 P1 122.0(7) . . ? C5 C4 P1 120.2(8) . . ? C6 C5 C4 120.1(10) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C7 C6 C5 119.6(10) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C8 C7 C6 121.4(10) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C9 C8 C7 121.9(11) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? C8 C9 C4 119.2(10) . . ? C8 C9 H9 120.4 . . ? C4 C9 H9 120.4 . . ? C15 C10 C11 118.7(8) . . ? C15 C10 P1 120.9(7) . . ? C11 C10 P1 120.4(7) . . ? C12 C11 C10 120.1(9) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 119.2(9) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 122.2(9) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 118.3(8) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C10 C15 C14 121.4(8) . . ? C10 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C21 118.0(9) . . ? C17 C16 P2 121.1(7) . . ? C21 C16 P2 120.9(7) . . ? C16 C17 C18 120.4(10) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C19 C18 C17 122.5(11) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C18 C19 C20 117.0(11) . . ? C18 C19 H19 121.5 . . ? C20 C19 H19 121.5 . . ? C19 C20 C21 119.9(11) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C16 122.3(10) . . ? C20 C21 H21 118.9 . . ? C16 C21 H21 118.9 . . ? C23 C22 C27 118.6(8) . . ? C23 C22 P2 120.9(6) . . ? C27 C22 P2 120.5(7) . . ? C24 C23 C22 121.6(8) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 119.4(9) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C26 C25 C24 120.2(9) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C25 C26 C27 121.3(9) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C22 118.9(9) . . ? C26 C27 H27 120.6 . . ? C22 C27 H27 120.6 . . ? C29 C28 P3 110.0(7) . . ? C29 C28 H28A 109.7 . . ? P3 C28 H28A 109.7 . . ? C29 C28 H28B 109.7 . . ? P3 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C28 C29 C30 111.7(7) . . ? C28 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? C28 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 107.9 . . ? C29 C30 P4 111.6(7) . . ? C29 C30 H30A 109.3 . . ? P4 C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? P4 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C32 C31 C36 116.5(9) . . ? C32 C31 P3 121.5(7) . . ? C36 C31 P3 121.7(8) . . ? C33 C32 C31 121.2(10) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C34 C33 C32 120.7(12) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C35 C34 C33 120.0(12) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.1(11) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 121.4(11) . . ? C35 C36 H36 119.3 . . ? C31 C36 H36 119.3 . . ? C42 C37 C38 120.2(9) . . ? C42 C37 P3 121.5(7) . . ? C38 C37 P3 118.3(8) . . ? C37 C38 C39 117.8(12) . . ? C37 C38 H38 121.1 . . ? C39 C38 H38 121.1 . . ? C40 C39 C38 121.1(11) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C41 C40 C39 119.6(11) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C40 C41 C42 119.8(12) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C41 C42 C37 121.5(10) . . ? C41 C42 H42 119.3 . . ? C37 C42 H42 119.3 . . ? C48 C43 C44 116.4(9) . . ? C48 C43 P4 122.3(8) . . ? C44 C43 P4 121.2(8) . . ? C43 C44 C45 123.1(10) . . ? C43 C44 H44 118.5 . . ? C45 C44 H44 118.5 . . ? C46 C45 C44 117.4(10) . . ? C46 C45 H45 121.3 . . ? C44 C45 H45 121.3 . . ? C47 C46 C45 120.9(11) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C48 C47 C46 118.9(11) . . ? C48 C47 H47 120.5 . . ? C46 C47 H47 120.5 . . ? C47 C48 C43 123.1(10) . . ? C47 C48 H48 118.4 . . ? C43 C48 H48 118.4 . . ? C50 C49 C54 119.7(8) . . ? C50 C49 P4 120.3(7) . . ? C54 C49 P4 119.8(7) . . ? C51 C50 C49 121.0(9) . . ? C51 C50 H50 119.5 . . ? C49 C50 H50 119.5 . . ? C50 C51 C52 119.4(9) . . ? C50 C51 H51 120.3 . . ? C52 C51 H51 120.3 . . ? C53 C52 C51 119.9(9) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C54 120.2(10) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C53 C54 C49 119.8(10) . . ? C53 C54 H54 120.1 . . ? C49 C54 H54 120.1 . . ? C56 C55 P6 114.7(7) . . ? C56 C55 H55A 108.6 . . ? P6 C55 H55A 108.6 . . ? C56 C55 H55B 108.6 . . ? P6 C55 H55B 108.6 . . ? H55A C55 H55B 107.6 . . ? C57 C56 C55 113.7(9) . . ? C57 C56 H56A 108.8 . . ? C55 C56 H56A 108.8 . . ? C57 C56 H56B 108.8 . . ? C55 C56 H56B 108.8 . . ? H56A C56 H56B 107.7 . . ? C56 C57 P5 115.7(6) . . ? C56 C57 H57A 108.4 . . ? P5 C57 H57A 108.4 . . ? C56 C57 H57B 108.4 . . ? P5 C57 H57B 108.4 . . ? H57A C57 H57B 107.4 . . ? C63 C58 C59 118.7(8) . . ? C63 C58 P5 119.5(8) . . ? C59 C58 P5 121.8(6) . . ? C58 C59 C60 122.1(8) . . ? C58 C59 H59 118.9 . . ? C60 C59 H59 118.9 . . ? C59 C60 C61 118.6(10) . . ? C59 C60 H60 120.7 . . ? C61 C60 H60 120.7 . . ? C62 C61 C60 120.8(10) . . ? C62 C61 H61 119.6 . . ? C60 C61 H61 119.6 . . ? C61 C62 C63 120.8(9) . . ? C61 C62 H62 119.6 . . ? C63 C62 H62 119.6 . . ? C58 C63 C62 119.0(10) . . ? C58 C63 H63 120.5 . . ? C62 C63 H63 120.5 . . ? C71 C70 C75 118.3(10) . . ? C71 C70 P6 122.1(9) . . ? C75 C70 P6 119.6(8) . . ? C70 C71 C72 121.1(12) . . ? C70 C71 H71 119.4 . . ? C72 C71 H71 119.4 . . ? C71 C72 C73 117.7(12) . . ? C71 C72 H72 121.2 . . ? C73 C72 H72 121.2 . . ? C74 C73 C72 122.4(11) . . ? C74 C73 H73 118.8 . . ? C72 C73 H73 118.8 . . ? C73 C74 C75 118.7(12) . . ? C73 C74 H74 120.6 . . ? C75 C74 H74 120.6 . . ? C74 C75 C70 121.7(10) . . ? C74 C75 H75 119.1 . . ? C70 C75 H75 119.1 . . ? C81 C76 C77 120.0(10) . . ? C81 C76 P6 119.6(8) . . ? C77 C76 P6 120.4(8) . . ? C78 C77 C76 117.0(12) . . ? C78 C77 H77 121.5 . . ? C76 C77 H77 121.5 . . ? C79 C78 C77 123.8(12) . . ? C79 C78 H78 118.1 . . ? C77 C78 H78 118.1 . . ? C80 C79 C78 118.8(11) . . ? C80 C79 H79 120.6 . . ? C78 C79 H79 120.6 . . ? C79 C80 C81 121.4(12) . . ? C79 C80 H80 119.3 . . ? C81 C80 H80 119.3 . . ? C80 C81 C76 119.0(11) . . ? C80 C81 H81 120.5 . . ? C76 C81 H81 120.5 . . ? Cl22 C111 Cl11 118.4(11) . . ? Cl22 C111 Cl33 100.2(9) . . ? Cl11 C111 Cl33 111.2(11) . . ? Cl22 C111 H111 108.8 . . ? Cl11 C111 H111 108.8 . . ? Cl33 C111 H111 108.8 . . ? Cl1A C101 Cl2A 100.4(12) . . ? Cl1A C101 Cl3A 123.7(14) . . ? Cl2A C101 Cl3A 110.7(12) . . ? Cl1A C101 H101 107.0 . . ? Cl2A C101 H101 107.0 . . ? Cl3A C101 H101 107.0 . . ? Cl44 C222 Cl55 112.5(10) . . ? Cl44 C222 Cl66 118.9(11) . . ? Cl55 C222 Cl66 110.3(10) . . ? Cl44 C222 H222 104.5 . . ? Cl55 C222 H222 104.5 . . ? Cl66 C222 H222 104.5 . . ? Cl5A C201 Cl6A 107(2) . . ? Cl5A C201 Cl4A 111.1(14) . . ? Cl6A C201 Cl4A 112.5(18) . . ? Cl5A C201 H201 108.8 . . ? Cl6A C201 H201 108.8 . . ? Cl4A C201 H201 108.8 . . ? Cl88 C333 Cl99 106.6(7) . . ? Cl88 C333 Cl77 109.8(6) . . ? Cl99 C333 Cl77 112.5(7) . . ? Cl88 C333 H333 109.3 . . ? Cl99 C333 H333 109.3 . . ? Cl77 C333 H333 109.3 . . ? C69 C64 C65 116.1(9) . . ? C69 C64 P5 120.6(7) . . ? C65 C64 P5 123.2(7) . . ? C66 C65 C64 121.2(9) . . ? C66 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? C68 C69 C64 122.9(9) . . ? C68 C69 H69 118.5 . . ? C64 C69 H69 118.5 . . ? C67 C66 C65 118.9(9) . . ? C67 C66 H66 120.5 . . ? C65 C66 H66 120.5 . . ? C69 C68 C67 118.3(9) . . ? C69 C68 H68 120.9 . . ? C67 C68 H68 120.9 . . ? C66 C67 C68 122.4(9) . . ? C66 C67 H67 118.8 . . ? C68 C67 H67 118.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P3 Pd2 Te1 Pd3 -134.36(7) . . . . ? P4 Pd2 Te1 Pd3 40.1(5) . . . . ? Te2 Pd2 Te1 Pd3 45.57(2) . . . . ? P3 Pd2 Te1 Pd1 139.26(7) . . . . ? P4 Pd2 Te1 Pd1 -46.3(5) . . . . ? Te2 Pd2 Te1 Pd1 -40.81(2) . . . . ? P5 Pd3 Te1 Pd2 135.96(6) . . . . ? P6 Pd3 Te1 Pd2 -57.7(6) . . . . ? Te2 Pd3 Te1 Pd2 -45.68(2) . . . . ? P5 Pd3 Te1 Pd1 -138.67(6) . . . . ? P6 Pd3 Te1 Pd1 27.6(6) . . . . ? Te2 Pd3 Te1 Pd1 39.69(2) . . . . ? P1 Pd1 Te1 Pd2 54.2(4) . . . . ? P2 Pd1 Te1 Pd2 -137.61(6) . . . . ? Te2 Pd1 Te1 Pd2 40.86(2) . . . . ? P1 Pd1 Te1 Pd3 -26.4(4) . . . . ? P2 Pd1 Te1 Pd3 141.87(6) . . . . ? Te2 Pd1 Te1 Pd3 -39.66(2) . . . . ? P5 Pd3 Te2 Pd2 61.5(6) . . . . ? P6 Pd3 Te2 Pd2 -135.84(7) . . . . ? Te1 Pd3 Te2 Pd2 45.60(2) . . . . ? P5 Pd3 Te2 Pd1 -23.8(6) . . . . ? P6 Pd3 Te2 Pd1 138.82(7) . . . . ? Te1 Pd3 Te2 Pd1 -39.74(2) . . . . ? P3 Pd2 Te2 Pd3 -45.2(5) . . . . ? P4 Pd2 Te2 Pd3 133.54(7) . . . . ? Te1 Pd2 Te2 Pd3 -45.67(2) . . . . ? P3 Pd2 Te2 Pd1 41.4(5) . . . . ? P4 Pd2 Te2 Pd1 -139.91(7) . . . . ? Te1 Pd2 Te2 Pd1 40.87(2) . . . . ? P1 Pd1 Te2 Pd3 -138.28(6) . . . . ? P2 Pd1 Te2 Pd3 50.2(4) . . . . ? Te1 Pd1 Te2 Pd3 39.73(2) . . . . ? P1 Pd1 Te2 Pd2 141.18(6) . . . . ? P2 Pd1 Te2 Pd2 -30.3(4) . . . . ? Te1 Pd1 Te2 Pd2 -40.80(2) . . . . ? P2 Pd1 P1 C4 -143.4(3) . . . . ? Te2 Pd1 P1 C4 37.9(3) . . . . ? Te1 Pd1 P1 C4 24.8(6) . . . . ? P2 Pd1 P1 C1 -24.1(4) . . . . ? Te2 Pd1 P1 C1 157.2(3) . . . . ? Te1 Pd1 P1 C1 144.1(5) . . . . ? P2 Pd1 P1 C10 93.4(3) . . . . ? Te2 Pd1 P1 C10 -85.3(3) . . . . ? Te1 Pd1 P1 C10 -98.4(5) . . . . ? P1 Pd1 P2 C16 -96.3(3) . . . . ? Te2 Pd1 P2 C16 75.2(5) . . . . ? Te1 Pd1 P2 C16 85.5(3) . . . . ? P1 Pd1 P2 C22 140.6(3) . . . . ? Te2 Pd1 P2 C22 -48.0(6) . . . . ? Te1 Pd1 P2 C22 -37.7(3) . . . . ? P1 Pd1 P2 C3 23.3(3) . . . . ? Te2 Pd1 P2 C3 -165.3(5) . . . . ? Te1 Pd1 P2 C3 -155.0(3) . . . . ? P4 Pd2 P3 C31 149.4(4) . . . . ? Te1 Pd2 P3 C31 -31.4(4) . . . . ? Te2 Pd2 P3 C31 -31.9(7) . . . . ? P4 Pd2 P3 C37 -89.0(3) . . . . ? Te1 Pd2 P3 C37 90.2(3) . . . . ? Te2 Pd2 P3 C37 89.7(6) . . . . ? P4 Pd2 P3 C28 29.9(4) . . . . ? Te1 Pd2 P3 C28 -150.9(4) . . . . ? Te2 Pd2 P3 C28 -151.4(5) . . . . ? P3 Pd2 P4 C43 91.1(3) . . . . ? Te1 Pd2 P4 C43 -83.3(6) . . . . ? Te2 Pd2 P4 C43 -88.7(3) . . . . ? P3 Pd2 P4 C49 -147.7(3) . . . . ? Te1 Pd2 P4 C49 37.8(7) . . . . ? Te2 Pd2 P4 C49 32.5(3) . . . . ? P3 Pd2 P4 C30 -27.1(3) . . . . ? Te1 Pd2 P4 C30 158.5(5) . . . . ? Te2 Pd2 P4 C30 153.1(3) . . . . ? P6 Pd3 P5 C64 -79.3(3) . . . . ? Te2 Pd3 P5 C64 83.4(7) . . . . ? Te1 Pd3 P5 C64 99.1(3) . . . . ? P6 Pd3 P5 C58 160.5(4) . . . . ? Te2 Pd3 P5 C58 -36.8(8) . . . . ? Te1 Pd3 P5 C58 -21.1(4) . . . . ? P6 Pd3 P5 C57 39.9(3) . . . . ? Te2 Pd3 P5 C57 -157.5(6) . . . . ? Te1 Pd3 P5 C57 -141.7(3) . . . . ? P5 Pd3 P6 C70 78.6(3) . . . . ? Te2 Pd3 P6 C70 -99.7(3) . . . . ? Te1 Pd3 P6 C70 -87.8(7) . . . . ? P5 Pd3 P6 C55 -40.3(4) . . . . ? Te2 Pd3 P6 C55 141.5(4) . . . . ? Te1 Pd3 P6 C55 153.4(6) . . . . ? P5 Pd3 P6 C76 -159.5(4) . . . . ? Te2 Pd3 P6 C76 22.3(4) . . . . ? Te1 Pd3 P6 C76 34.2(8) . . . . ? C4 P1 C1 C2 179.6(6) . . . . ? C10 P1 C1 C2 -71.4(7) . . . . ? Pd1 P1 C1 C2 52.5(7) . . . . ? P1 C1 C2 C3 -81.7(8) . . . . ? C1 C2 C3 P2 78.0(8) . . . . ? C16 P2 C3 C2 78.1(7) . . . . ? C22 P2 C3 C2 -172.8(7) . . . . ? Pd1 P2 C3 C2 -47.4(7) . . . . ? C1 P1 C4 C9 141.6(7) . . . . ? C10 P1 C4 C9 34.6(8) . . . . ? Pd1 P1 C4 C9 -93.0(7) . . . . ? C1 P1 C4 C5 -44.6(8) . . . . ? C10 P1 C4 C5 -151.6(7) . . . . ? Pd1 P1 C4 C5 80.8(7) . . . . ? C9 C4 C5 C6 -2.3(13) . . . . ? P1 C4 C5 C6 -176.4(8) . . . . ? C4 C5 C6 C7 -1.0(16) . . . . ? C5 C6 C7 C8 3.9(17) . . . . ? C6 C7 C8 C9 -3.4(16) . . . . ? C7 C8 C9 C4 -0.1(15) . . . . ? C5 C4 C9 C8 2.8(13) . . . . ? P1 C4 C9 C8 176.8(7) . . . . ? C4 P1 C10 C15 -125.8(8) . . . . ? C1 P1 C10 C15 127.3(8) . . . . ? Pd1 P1 C10 C15 3.4(9) . . . . ? C4 P1 C10 C11 55.7(9) . . . . ? C1 P1 C10 C11 -51.2(8) . . . . ? Pd1 P1 C10 C11 -175.0(7) . . . . ? C15 C10 C11 C12 -4.6(15) . . . . ? P1 C10 C11 C12 173.9(9) . . . . ? C10 C11 C12 C13 2.5(17) . . . . ? C11 C12 C13 C14 0.2(17) . . . . ? C12 C13 C14 C15 -0.8(16) . . . . ? C11 C10 C15 C14 4.0(15) . . . . ? P1 C10 C15 C14 -174.5(8) . . . . ? C13 C14 C15 C10 -1.3(15) . . . . ? C22 P2 C16 C17 130.5(7) . . . . ? C3 P2 C16 C17 -124.6(7) . . . . ? Pd1 P2 C16 C17 2.2(7) . . . . ? C22 P2 C16 C21 -51.6(8) . . . . ? C3 P2 C16 C21 53.4(8) . . . . ? Pd1 P2 C16 C21 -179.8(6) . . . . ? C21 C16 C17 C18 -2.1(12) . . . . ? P2 C16 C17 C18 175.9(7) . . . . ? C16 C17 C18 C19 2.5(15) . . . . ? C17 C18 C19 C20 -1.5(16) . . . . ? C18 C19 C20 C21 0.4(15) . . . . ? C19 C20 C21 C16 -0.2(15) . . . . ? C17 C16 C21 C20 1.1(13) . . . . ? P2 C16 C21 C20 -177.0(7) . . . . ? C16 P2 C22 C23 156.5(8) . . . . ? C3 P2 C22 C23 49.8(9) . . . . ? Pd1 P2 C22 C23 -76.1(8) . . . . ? C16 P2 C22 C27 -25.8(9) . . . . ? C3 P2 C22 C27 -132.5(8) . . . . ? Pd1 P2 C22 C27 101.7(8) . . . . ? C27 C22 C23 C24 2.4(16) . . . . ? P2 C22 C23 C24 -179.8(9) . . . . ? C22 C23 C24 C25 -2.8(17) . . . . ? C23 C24 C25 C26 1.0(17) . . . . ? C24 C25 C26 C27 1.1(18) . . . . ? C25 C26 C27 C22 -1.4(17) . . . . ? C23 C22 C27 C26 -0.3(15) . . . . ? P2 C22 C27 C26 -178.1(8) . . . . ? C31 P3 C28 C29 175.2(5) . . . . ? C37 P3 C28 C29 66.8(6) . . . . ? Pd2 P3 C28 C29 -57.9(6) . . . . ? P3 C28 C29 C30 86.1(8) . . . . ? C28 C29 C30 P4 -81.4(9) . . . . ? C43 P4 C30 C29 -73.5(8) . . . . ? C49 P4 C30 C29 178.0(7) . . . . ? Pd2 P4 C30 C29 50.6(8) . . . . ? C37 P3 C31 C32 158.6(7) . . . . ? C28 P3 C31 C32 49.7(8) . . . . ? Pd2 P3 C31 C32 -74.4(8) . . . . ? C37 P3 C31 C36 -28.2(8) . . . . ? C28 P3 C31 C36 -137.1(7) . . . . ? Pd2 P3 C31 C36 98.8(7) . . . . ? C36 C31 C32 C33 2.6(14) . . . . ? P3 C31 C32 C33 176.1(8) . . . . ? C31 C32 C33 C34 -0.4(17) . . . . ? C32 C33 C34 C35 -1.2(18) . . . . ? C33 C34 C35 C36 0.5(18) . . . . ? C34 C35 C36 C31 1.8(16) . . . . ? C32 C31 C36 C35 -3.3(13) . . . . ? P3 C31 C36 C35 -176.8(8) . . . . ? C31 P3 C37 C42 113.9(9) . . . . ? C28 P3 C37 C42 -137.8(9) . . . . ? Pd2 P3 C37 C42 -14.5(9) . . . . ? C31 P3 C37 C38 -64.8(9) . . . . ? C28 P3 C37 C38 43.6(9) . . . . ? Pd2 P3 C37 C38 166.8(7) . . . . ? C42 C37 C38 C39 -0.2(17) . . . . ? P3 C37 C38 C39 178.5(9) . . . . ? C37 C38 C39 C40 -0.3(19) . . . . ? C38 C39 C40 C41 2(2) . . . . ? C39 C40 C41 C42 -3.3(19) . . . . ? C40 C41 C42 C37 2.9(17) . . . . ? C38 C37 C42 C41 -1.1(16) . . . . ? P3 C37 C42 C41 -179.7(9) . . . . ? C49 P4 C43 C48 48.3(8) . . . . ? C30 P4 C43 C48 -59.2(8) . . . . ? Pd2 P4 C43 C48 175.7(7) . . . . ? C49 P4 C43 C44 -134.3(8) . . . . ? C30 P4 C43 C44 118.2(8) . . . . ? Pd2 P4 C43 C44 -6.9(9) . . . . ? C48 C43 C44 C45 0.3(14) . . . . ? P4 C43 C44 C45 -177.2(7) . . . . ? C43 C44 C45 C46 2.5(15) . . . . ? C44 C45 C46 C47 -3.3(16) . . . . ? C45 C46 C47 C48 1.2(17) . . . . ? C46 C47 C48 C43 1.9(16) . . . . ? C44 C43 C48 C47 -2.6(14) . . . . ? P4 C43 C48 C47 174.9(8) . . . . ? C43 P4 C49 C50 31.1(8) . . . . ? C30 P4 C49 C50 138.3(7) . . . . ? Pd2 P4 C49 C50 -94.8(7) . . . . ? C43 P4 C49 C54 -153.4(7) . . . . ? C30 P4 C49 C54 -46.2(8) . . . . ? Pd2 P4 C49 C54 80.7(7) . . . . ? C54 C49 C50 C51 2.1(14) . . . . ? P4 C49 C50 C51 177.6(7) . . . . ? C49 C50 C51 C52 0.3(15) . . . . ? C50 C51 C52 C53 -1.8(15) . . . . ? C51 C52 C53 C54 0.8(15) . . . . ? C52 C53 C54 C49 1.6(14) . . . . ? C50 C49 C54 C53 -3.1(13) . . . . ? P4 C49 C54 C53 -178.6(7) . . . . ? C70 P6 C55 C56 -63.2(8) . . . . ? C76 P6 C55 C56 -173.8(7) . . . . ? Pd3 P6 C55 C56 59.1(8) . . . . ? P6 C55 C56 C57 -70.9(10) . . . . ? C55 C56 C57 P5 71.4(10) . . . . ? C64 P5 C57 C56 62.2(8) . . . . ? C58 P5 C57 C56 172.4(7) . . . . ? Pd3 P5 C57 C56 -59.0(8) . . . . ? C64 P5 C58 C63 146.1(8) . . . . ? C57 P5 C58 C63 34.8(9) . . . . ? Pd3 P5 C58 C63 -91.2(8) . . . . ? C64 P5 C58 C59 -35.9(9) . . . . ? C57 P5 C58 C59 -147.3(8) . . . . ? Pd3 P5 C58 C59 86.8(8) . . . . ? C63 C58 C59 C60 0.2(15) . . . . ? P5 C58 C59 C60 -177.7(8) . . . . ? C58 C59 C60 C61 -0.1(15) . . . . ? C59 C60 C61 C62 0.2(17) . . . . ? C60 C61 C62 C63 -0.5(18) . . . . ? C59 C58 C63 C62 -0.5(14) . . . . ? P5 C58 C63 C62 177.5(8) . . . . ? C61 C62 C63 C58 0.6(17) . . . . ? C55 P6 C70 C71 -29.0(11) . . . . ? C76 P6 C70 C71 78.9(11) . . . . ? Pd3 P6 C70 C71 -153.0(9) . . . . ? C55 P6 C70 C75 151.8(8) . . . . ? C76 P6 C70 C75 -100.3(8) . . . . ? Pd3 P6 C70 C75 27.8(9) . . . . ? C75 C70 C71 C72 0(2) . . . . ? P6 C70 C71 C72 -179.0(13) . . . . ? C70 C71 C72 C73 -1(3) . . . . ? C71 C72 C73 C74 0(3) . . . . ? C72 C73 C74 C75 2(2) . . . . ? C73 C74 C75 C70 -3.3(17) . . . . ? C71 C70 C75 C74 2.0(16) . . . . ? P6 C70 C75 C74 -178.7(8) . . . . ? C70 P6 C76 C81 -162.2(8) . . . . ? C55 P6 C76 C81 -52.2(9) . . . . ? Pd3 P6 C76 C81 73.1(9) . . . . ? C70 P6 C76 C77 18.2(10) . . . . ? C55 P6 C76 C77 128.2(9) . . . . ? Pd3 P6 C76 C77 -106.5(9) . . . . ? C81 C76 C77 C78 -1.7(16) . . . . ? P6 C76 C77 C78 177.9(9) . . . . ? C76 C77 C78 C79 0.3(19) . . . . ? C77 C78 C79 C80 0(2) . . . . ? C78 C79 C80 C81 0.9(19) . . . . ? C79 C80 C81 C76 -2.3(17) . . . . ? C77 C76 C81 C80 2.7(16) . . . . ? P6 C76 C81 C80 -176.9(8) . . . . ? C58 P5 C64 C69 94.2(8) . . . . ? C57 P5 C64 C69 -156.9(8) . . . . ? Pd3 P5 C64 C69 -33.5(8) . . . . ? C58 P5 C64 C65 -88.9(8) . . . . ? C57 P5 C64 C65 20.0(8) . . . . ? Pd3 P5 C64 C65 143.5(7) . . . . ? C69 C64 C65 C66 2.8(13) . . . . ? P5 C64 C65 C66 -174.2(7) . . . . ? C65 C64 C69 C68 -2.2(14) . . . . ? P5 C64 C69 C68 174.9(8) . . . . ? C64 C65 C66 C67 -0.4(15) . . . . ? C64 C69 C68 C67 -0.8(15) . . . . ? C65 C66 C67 C68 -2.9(15) . . . . ? C69 C68 C67 C66 3.5(15) . . . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 16.007 _refine_diff_density_min -6.576 _refine_diff_density_rms 0.267