# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email chhbsia@chem.iitb.ac.in _publ_contact_author_name 'Prof Harkesh B. Singh' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_address ; Department of Chemistry, Indian Institute of Technology, Bombay, Powai, Mumbai 400076,India ; _publ_section_title ; Contrasting coordination behaviour of 22-membered chalcogenaaza (Se, Te) macrocylces towards Pd(II) and Pt(II): Isolation and structural characterization of the first metallamacrocyle with a C-Pt-Se linkage ; loop_ _publ_author_name 'Harkesh B. Singh' 'Ray J. Butcher' 'Snigdha Panda' data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 221526' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H39 Cl2 N4 O2 Pt Se2' _chemical_formula_weight 935.58 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9635(19) _cell_length_b 10.210(2) _cell_length_c 17.427(3) _cell_angle_alpha 94.196(3) _cell_angle_beta 105.466(3) _cell_angle_gamma 106.808(4) _cell_volume 1613.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max .15 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .48 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.925 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 910 _exptl_absorpt_coefficient_mu 6.806 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.599187 _exptl_absorpt_correction_T_max 0.928074 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16279 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 29.02 _reflns_number_total 7802 _reflns_number_gt 6649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+6.7165P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7802 _refine_ls_number_parameters 467 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.430 _refine_ls_shift/su_mean 0.012 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 Pt Pt 1.073604(19) -1.11041(2) -0.295521(10) 0.02030(5) Uani 1 1 d . . . Se1 Se 1.42816(5) -0.82680(5) -0.01104(3) 0.02559(10) Uani 1 1 d . . . Se2 Se 0.98802(6) -1.14600(5) -0.44125(3) 0.02845(11) Uani 1 1 d . . . Cl1 Cl 1.32722(13) -1.02166(15) -0.29624(8) 0.0341(3) Uani 1 1 d . . . Cl2 Cl 0.93661(15) -0.57770(14) -0.22877(8) 0.0344(3) Uani 1 1 d . . . O1WA O 0.645(4) -0.770(2) -0.3273(16) 0.057(13) Uani 0.169(16) 1 d PD A 1 H1WA H 0.698(7) -0.738(16) -0.357(5) 0.085 Uiso 0.169(16) 1 d PD A 1 H1WB H 0.64(2) -0.699(11) -0.302(14) 0.085 Uiso 0.169(16) 1 d PD A 1 O1WB O 0.5768(9) -0.6867(13) -0.3162(8) 0.129(5) Uani 0.831(16) 1 d PD A 2 H1WC H 0.663(4) -0.691(10) -0.297(10) 0.194 Uiso 0.831(16) 1 d PD A 2 H1WD H 0.531(13) -0.759(9) -0.351(7) 0.194 Uiso 0.831(16) 1 d PD A 2 O2WA O 0.438(4) -0.951(3) -0.4770(16) 0.38(2) Uani 0.61(3) 1 d PD B 1 H2WA H 0.528(6) -0.95(2) -0.461(12) 0.570 Uiso 0.61(3) 1 d PD B 1 H2WB H 0.421(17) -0.92(5) -0.435(11) 0.570 Uiso 0.61(3) 1 d PD B 1 O2WB O 0.430(2) -0.886(2) -0.4392(13) 0.102(10) Uani 0.39(3) 1 d PD B 2 H2WC H 0.40(3) -0.90(2) -0.491(2) 0.153 Uiso 0.39(3) 1 d PD B 2 H2WD H 0.38(2) -0.964(13) -0.429(11) 0.153 Uiso 0.39(3) 1 d PD B 2 N1A N 1.1677(4) -1.0864(3) -0.1651(2) 0.0154(7) Uani 1 1 d . . . H1AA H 1.2630 -1.0257 -0.1533 0.036(16) Uiso 1 1 calc R . . N2A N 1.0938(4) -1.3041(4) -0.2909(2) 0.0233(8) Uani 1 1 d . . . H2AB H 1.0093 -1.3572 -0.2806 0.044(18) Uiso 1 1 calc R . . N1B N 1.2247(5) -0.6984(5) -0.1804(2) 0.0285(9) Uani 1 1 d . . . H1B H 1.1485 -0.6621 -0.1911 0.045(19) Uiso 1 1 d R . . N2B N 1.0383(5) -0.9236(4) -0.2985(2) 0.0260(9) Uani 1 1 d . . . H2BB H 1.0708 -0.8930 -0.2431 0.16(5) Uiso 1 1 calc R . . C1A C 1.3023(5) -0.9754(5) 0.0236(3) 0.0232(9) Uani 1 1 d . . . C2A C 1.3555(6) -1.0081(6) 0.0991(3) 0.0320(12) Uani 1 1 d . . . H2AA H 1.4531 -0.9586 0.1318 0.041(17) Uiso 1 1 calc R . . C3A C 1.2678(7) -1.1117(6) 0.1271(3) 0.0365(13) Uani 1 1 d . . . H3AA H 1.3058 -1.1359 0.1781 0.035(16) Uiso 1 1 calc R . . C4A C 1.1260(6) -1.1798(6) 0.0815(3) 0.0326(11) Uani 1 1 d . . . H4AA H 1.0639 -1.2484 0.1018 0.07(2) Uiso 1 1 calc R . . C5A C 1.0730(6) -1.1488(5) 0.0057(3) 0.0281(10) Uani 1 1 d . . . H5AA H 0.9745 -1.1974 -0.0259 0.07(2) Uiso 1 1 calc R . . C6A C 1.1601(5) -1.0487(5) -0.0250(3) 0.0218(9) Uani 1 1 d . . . C7A C 1.1011(5) -1.0284(5) -0.1108(3) 0.0224(9) Uani 1 1 d . . . H7AA H 0.9932 -1.0736 -0.1298 0.030(15) Uiso 1 1 calc R . . H7AB H 1.1213 -0.9280 -0.1126 0.034(16) Uiso 1 1 calc R . . C8A C 1.1840(5) -1.2236(5) -0.1496(3) 0.0250(10) Uani 1 1 d . . . H8AA H 1.0921 -1.2837 -0.1422 0.012(11) Uiso 1 1 calc R . . H8AB H 1.2647 -1.2102 -0.0991 0.043(18) Uiso 1 1 calc R . . C9A C 1.2168(5) -1.2935(6) -0.2176(3) 0.0270(10) Uani 1 1 d . . . H9AA H 1.3119 -1.2380 -0.2236 0.030(15) Uiso 1 1 calc R . . H9AB H 1.2214 -1.3867 -0.2081 0.005(10) Uiso 1 1 calc R . . C10A C 1.0984(6) -1.3805(6) -0.3654(3) 0.0334(12) Uani 1 1 d . . . H10A H 1.1337 -1.4599 -0.3526 0.022(13) Uiso 1 1 calc R . . H10B H 1.1667 -1.3185 -0.3895 0.035(16) Uiso 1 1 calc R . . C11A C 0.9461(6) -1.4314(6) -0.4237(3) 0.0311(11) Uani 1 1 d . . . C12A C 0.8646(7) -1.5698(7) -0.4394(3) 0.0409(14) Uani 1 1 d . . . H12A H 0.9079 -1.6339 -0.4149 0.05(2) Uiso 1 1 calc R . . C13A C 0.7206(8) -1.6183(8) -0.4901(4) 0.0529(18) Uani 1 1 d . . . H13A H 0.6660 -1.7143 -0.5005 0.15(5) Uiso 1 1 calc R . . C14A C 0.6586(8) -1.5235(8) -0.5251(4) 0.0547(19) Uani 1 1 d . . . H14A H 0.5598 -1.5548 -0.5591 0.07(2) Uiso 1 1 calc R . . C15A C 0.7381(7) -1.3852(7) -0.5112(3) 0.0425(15) Uani 1 1 d . . . H15A H 0.6949 -1.3217 -0.5367 0.025(14) Uiso 1 1 calc R . . C16A C 0.8808(6) -1.3381(6) -0.4604(3) 0.0289(11) Uani 1 1 d . . . C1B C 1.3451(5) -0.6876(5) 0.0153(3) 0.0246(10) Uani 1 1 d . . . C2B C 1.3169(5) -0.6761(5) 0.0885(3) 0.0273(10) Uani 1 1 d . . . H2BA H 1.3394 -0.7362 0.1255 0.011(11) Uiso 1 1 calc R . . C3B C 1.2563(6) -0.5780(6) 0.1080(3) 0.0329(12) Uani 1 1 d . . . H3BA H 1.2379 -0.5698 0.1586 0.05(2) Uiso 1 1 calc R . . C4B C 1.2225(6) -0.4922(6) 0.0544(4) 0.0372(13) Uani 1 1 d . . . H4BA H 1.1774 -0.4265 0.0668 0.019(13) Uiso 1 1 calc R . . C5B C 1.2541(6) -0.5017(6) -0.0170(3) 0.0364(13) Uani 1 1 d . . . H5BA H 1.2323 -0.4405 -0.0534 0.06(2) Uiso 1 1 calc R . . C6B C 1.3168(5) -0.5976(5) -0.0378(3) 0.0273(11) Uani 1 1 d . . . C7B C 1.3490(6) -0.6040(6) -0.1172(3) 0.0297(11) Uani 1 1 d . . . H7BA H 1.3725 -0.5102 -0.1322 0.016(12) Uiso 1 1 calc R . . H7BB H 1.4359 -0.6351 -0.1118 0.007(11) Uiso 1 1 calc R . . C8B C 1.2647(6) -0.7190(6) -0.2527(3) 0.0325(12) Uani 1 1 d . . . H8BA H 1.3393 -0.7673 -0.2429 0.043(18) Uiso 1 1 calc R . . H8BB H 1.3088 -0.6279 -0.2672 0.034(16) Uiso 1 1 calc R . . C9B C 1.1332(6) -0.8030(5) -0.3212(3) 0.0293(11) Uani 1 1 d . . . H9BA H 1.0746 -0.7428 -0.3423 0.026(14) Uiso 1 1 calc R . . H9BB H 1.1671 -0.8357 -0.3653 0.019(13) Uiso 1 1 calc R . . C10B C 0.8980(7) -0.9326(6) -0.3107(4) 0.0418(14) Uani 1 1 d . . . H10C H 0.8626 -0.8575 -0.3238 0.07(2) Uiso 1 1 calc R . . C11B C 0.8024(5) -1.0658(5) -0.3027(3) 0.0271(10) Uani 1 1 d . . . C12B C 0.6552(6) -1.0887(6) -0.3075(3) 0.0362(12) Uani 1 1 d . . . H12B H 0.6144 -1.0153 -0.3132 0.05(2) Uiso 1 1 calc R . . C13B C 0.5706(6) -1.2191(6) -0.3038(3) 0.0329(12) Uani 1 1 d . . . H13B H 0.4699 -1.2368 -0.3074 0.027(14) Uiso 1 1 calc R . . C14B C 0.6310(6) -1.3237(6) -0.2950(3) 0.0327(12) Uani 1 1 d . . . H14B H 0.5723 -1.4132 -0.2912 0.033(16) Uiso 1 1 calc R . . C15B C 0.7771(5) -1.3007(6) -0.2916(3) 0.0278(10) Uani 1 1 d . . . H15B H 0.8173 -1.3746 -0.2862 0.07(3) Uiso 1 1 calc R . . C16B C 0.8627(5) -1.1720(5) -0.2960(2) 0.0221(9) 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 Pt 0.01993(8) 0.02735(9) 0.01473(8) 0.00531(6) 0.00111(6) 0.01257(7) Se1 0.0204(2) 0.0323(3) 0.0217(2) 0.00332(19) 0.00114(17) 0.00990(19) Se2 0.0398(3) 0.0341(3) 0.0156(2) 0.00863(18) 0.00555(19) 0.0196(2) Cl1 0.0257(5) 0.0409(7) 0.0423(7) 0.0142(6) 0.0130(5) 0.0164(5) Cl2 0.0463(7) 0.0391(7) 0.0275(6) 0.0131(5) 0.0133(5) 0.0243(6) O1WA 0.08(3) 0.017(13) 0.043(15) 0.004(10) 0.004(15) -0.009(14) O1WB 0.051(5) 0.146(10) 0.206(12) 0.076(9) 0.055(6) 0.029(5) O2WA 0.87(8) 0.25(3) 0.26(2) 0.21(2) 0.38(3) 0.31(3) O2WB 0.096(16) 0.106(17) 0.088(15) 0.053(12) 0.008(11) 0.018(12) N1A 0.0176(16) 0.0068(15) 0.0174(16) 0.0037(13) -0.0039(13) 0.0053(13) N2A 0.0257(19) 0.028(2) 0.0182(17) 0.0003(15) 0.0035(15) 0.0159(17) N1B 0.025(2) 0.034(2) 0.0232(19) 0.0030(17) 0.0014(16) 0.0098(18) N2B 0.028(2) 0.030(2) 0.0230(19) 0.0084(16) 0.0049(16) 0.0166(17) C1A 0.029(2) 0.022(2) 0.020(2) 0.0061(17) 0.0040(18) 0.0122(19) C2A 0.039(3) 0.037(3) 0.018(2) 0.003(2) -0.004(2) 0.021(2) C3A 0.059(3) 0.036(3) 0.022(2) 0.011(2) 0.010(2) 0.027(3) C4A 0.050(3) 0.030(3) 0.029(2) 0.011(2) 0.020(2) 0.020(2) C5A 0.033(3) 0.028(3) 0.027(2) 0.002(2) 0.012(2) 0.013(2) C6A 0.024(2) 0.025(2) 0.018(2) 0.0033(17) 0.0030(17) 0.0136(18) C7A 0.023(2) 0.026(2) 0.018(2) 0.0019(17) -0.0006(17) 0.0132(18) C8A 0.031(2) 0.029(2) 0.018(2) 0.0066(18) -0.0006(18) 0.020(2) C9A 0.026(2) 0.038(3) 0.021(2) 0.0072(19) 0.0003(18) 0.021(2) C10A 0.047(3) 0.040(3) 0.020(2) 0.006(2) 0.008(2) 0.026(3) C11A 0.041(3) 0.036(3) 0.017(2) 0.0035(19) 0.008(2) 0.014(2) C12A 0.057(4) 0.043(3) 0.020(2) 0.002(2) 0.008(2) 0.016(3) C13A 0.057(4) 0.052(4) 0.035(3) -0.008(3) 0.009(3) 0.004(3) C14A 0.044(4) 0.073(5) 0.028(3) -0.018(3) -0.005(3) 0.010(3) C15A 0.043(3) 0.062(4) 0.020(2) -0.006(2) -0.004(2) 0.029(3) C16A 0.036(3) 0.035(3) 0.0128(19) 0.0010(18) 0.0042(18) 0.012(2) C1B 0.022(2) 0.025(2) 0.020(2) 0.0017(18) -0.0020(17) 0.0053(19) C2B 0.025(2) 0.030(3) 0.023(2) 0.0062(19) 0.0008(18) 0.009(2) C3B 0.036(3) 0.029(3) 0.030(3) 0.000(2) 0.006(2) 0.009(2) C4B 0.037(3) 0.028(3) 0.041(3) 0.000(2) 0.002(2) 0.014(2) C5B 0.040(3) 0.028(3) 0.034(3) 0.008(2) 0.001(2) 0.009(2) C6B 0.024(2) 0.027(3) 0.021(2) 0.0045(19) -0.0035(18) 0.0026(19) C7B 0.032(3) 0.030(3) 0.021(2) 0.0095(19) 0.0001(19) 0.006(2) C8B 0.031(3) 0.036(3) 0.029(2) 0.004(2) 0.006(2) 0.011(2) C9B 0.034(3) 0.029(3) 0.023(2) 0.009(2) 0.004(2) 0.011(2) C10B 0.043(3) 0.034(3) 0.058(4) 0.009(3) 0.020(3) 0.023(3) C11B 0.025(2) 0.031(3) 0.024(2) 0.0006(19) 0.0019(18) 0.014(2) C12B 0.031(3) 0.046(3) 0.038(3) 0.003(2) 0.007(2) 0.025(2) C13B 0.020(2) 0.050(3) 0.026(2) 0.000(2) 0.0020(19) 0.014(2) C14B 0.027(2) 0.041(3) 0.025(2) 0.002(2) 0.007(2) 0.006(2) C15B 0.025(2) 0.034(3) 0.024(2) 0.004(2) 0.0034(18) 0.013(2) C16B 0.023(2) 0.031(3) 0.0112(18) 0.0014(17) 0.0005(16) 0.0119(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt C16B 2.009(5) . ? Pt N2B 2.038(4) . ? Pt N2A 2.050(4) . ? Pt N1A 2.180(3) . ? Pt Se2 2.4165(7) . ? Pt Cl1 2.4292(13) . ? Se1 C1A 1.917(5) . ? Se1 C1B 1.924(5) . ? Se2 C16A 1.897(6) . ? O1WA H1WA 0.85(2) . ? O1WA H1WB 0.85(2) . ? O1WA H1WC 0.88(13) . ? O1WA H1WD 1.15(13) . ? O1WB H1WB 0.7(2) . ? O1WB H1WC 0.85(2) . ? O1WB H1WD 0.85(2) . ? O2WA H2WA 0.85(2) . ? O2WA H2WB 0.85(2) . ? O2WA H2WC 0.8(2) . ? O2WA H2WD 1.11(19) . ? O2WB H2WB 0.4(5) . ? O2WB H2WC 0.85(2) . ? O2WB H2WD 0.85(2) . ? N1A C7A 1.472(6) . ? N1A C8A 1.492(6) . ? N1A H1AA 0.9300 . ? N2A C10A 1.484(6) . ? N2A C9A 1.487(6) . ? N2A H2AB 0.9300 . ? N1B C8B 1.438(7) . ? N1B C7B 1.450(6) . ? N1B H1B 0.9200 . ? N2B C10B 1.332(7) . ? N2B C9B 1.471(7) . ? N2B H2BB 0.9300 . ? C1A C2A 1.386(6) . ? C1A C6A 1.392(6) . ? C2A C3A 1.374(8) . ? C2A H2AA 0.9500 . ? C3A C4A 1.365(8) . ? C3A H3AA 0.9500 . ? C4A C5A 1.382(7) . ? C4A H4AA 0.9500 . ? C5A C6A 1.378(7) . ? C5A H5AA 0.9500 . ? C6A C7A 1.506(6) . ? C7A H7AA 0.9900 . ? C7A H7AB 0.9900 . ? C8A C9A 1.497(7) . ? C8A H8AA 0.9900 . ? C8A H8AB 0.9900 . ? C9A H9AA 0.9900 . ? C9A H9AB 0.9900 . ? C10A C11A 1.500(8) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11A C12A 1.376(8) . ? C11A C16A 1.402(8) . ? C12A C13A 1.390(9) . ? C12A H12A 0.9500 . ? C13A C14A 1.386(11) . ? C13A H13A 0.9500 . ? C14A C15A 1.372(10) . ? C14A H14A 0.9500 . ? C15A C16A 1.382(8) . ? C15A H15A 0.9500 . ? C1B C2B 1.382(7) . ? C1B C6B 1.384(7) . ? C2B C3B 1.376(8) . ? C2B H2BA 0.9500 . ? C3B C4B 1.370(8) . ? C3B H3BA 0.9500 . ? C4B C5B 1.366(8) . ? C4B H4BA 0.9500 . ? C5B C6B 1.379(8) . ? C5B H5BA 0.9500 . ? C6B C7B 1.502(7) . ? C7B H7BA 0.9900 . ? C7B H7BB 0.9900 . ? C8B C9B 1.498(7) . ? C8B H8BA 0.9900 . ? C8B H8BB 0.9900 . ? C9B H9BA 0.9900 . ? C9B H9BB 0.9900 . ? C10B C11B 1.458(8) . ? C10B H10C 0.9500 . ? C11B C16B 1.381(7) . ? C11B C12B 1.395(7) . ? C12B C13B 1.371(8) . ? C12B H12B 0.9500 . ? C13B C14B 1.369(8) . ? C13B H13B 0.9500 . ? C14B C15B 1.389(7) . ? C14B H14B 0.9500 . ? C15B C16B 1.364(7) . ? C15B H15B 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 C16B Pt N2B 81.52(19) . . ? C16B Pt N2A 94.13(18) . . ? N2B Pt N2A 175.59(17) . . ? C16B Pt N1A 95.80(15) . . ? N2B Pt N1A 97.27(15) . . ? N2A Pt N1A 82.35(14) . . ? C16B Pt Se2 88.54(12) . . ? N2B Pt Se2 86.80(12) . . ? N2A Pt Se2 93.88(11) . . ? N1A Pt Se2 174.42(10) . . ? C16B Pt Cl1 176.39(15) . . ? N2B Pt Cl1 94.89(12) . . ? N2A Pt Cl1 89.46(12) . . ? N1A Pt Cl1 85.03(10) . . ? Se2 Pt Cl1 90.85(4) . . ? C1A Se1 C1B 96.4(2) . . ? C16A Se2 Pt 98.81(14) . . ? H1WA O1WA H1WB 105(4) . . ? H1WA O1WA H1WC 97(10) . . ? H1WB O1WA H1WC 15(10) . . ? H1WA O1WA H1WD 110(10) . . ? H1WB O1WA H1WD 68(10) . . ? H1WC O1WA H1WD 82(4) . . ? H1WB O1WB H1WC 8(10) . . ? H1WB O1WB H1WD 99(10) . . ? H1WC O1WB H1WD 105(3) . . ? H2WA O2WA H2WB 105(3) . . ? H2WA O2WA H2WC 131(10) . . ? H2WB O2WA H2WC 77(10) . . ? H2WA O2WA H2WD 115(10) . . ? H2WB O2WA H2WD 26(10) . . ? H2WC O2WA H2WD 88(10) . . ? H2WB O2WB H2WC 105(10) . . ? H2WB O2WB H2WD 19(10) . . ? H2WC O2WB H2WD 104(3) . . ? C7A N1A C8A 113.8(4) . . ? C7A N1A Pt 120.1(3) . . ? C8A N1A Pt 105.3(3) . . ? C7A N1A H1AA 105.5 . . ? C8A N1A H1AA 105.5 . . ? Pt N1A H1AA 105.5 . . ? C10A N2A C9A 114.6(4) . . ? C10A N2A Pt 117.5(3) . . ? C9A N2A Pt 107.5(3) . . ? C10A N2A H2AB 105.4 . . ? C9A N2A H2AB 105.4 . . ? Pt N2A H2AB 105.4 . . ? C8B N1B C7B 110.4(4) . . ? C8B N1B H1B 109.4 . . ? C7B N1B H1B 109.4 . . ? C10B N2B C9B 117.5(4) . . ? C10B N2B Pt 113.4(4) . . ? C9B N2B Pt 124.0(3) . . ? C10B N2B H2BB 97.5 . . ? C9B N2B H2BB 97.5 . . ? Pt N2B H2BB 97.5 . . ? C2A C1A C6A 120.2(5) . . ? C2A C1A Se1 118.4(4) . . ? C6A C1A Se1 121.4(3) . . ? C3A C2A C1A 120.3(5) . . ? C3A C2A H2AA 119.9 . . ? C1A C2A H2AA 119.9 . . ? C4A C3A C2A 119.9(5) . . ? C4A C3A H3AA 120.0 . . ? C2A C3A H3AA 120.0 . . ? C3A C4A C5A 119.9(5) . . ? C3A C4A H4AA 120.0 . . ? C5A C4A H4AA 120.0 . . ? C6A C5A C4A 121.3(5) . . ? C6A C5A H5AA 119.3 . . ? C4A C5A H5AA 119.3 . . ? C5A C6A C1A 118.2(4) . . ? C5A C6A C7A 119.0(4) . . ? C1A C6A C7A 122.8(4) . . ? N1A C7A C6A 111.9(4) . . ? N1A C7A H7AA 109.2 . . ? C6A C7A H7AA 109.2 . . ? N1A C7A H7AB 109.2 . . ? C6A C7A H7AB 109.2 . . ? H7AA C7A H7AB 107.9 . . ? N1A C8A C9A 111.5(4) . . ? N1A C8A H8AA 109.3 . . ? C9A C8A H8AA 109.3 . . ? N1A C8A H8AB 109.3 . . ? C9A C8A H8AB 109.3 . . ? H8AA C8A H8AB 108.0 . . ? N2A C9A C8A 105.6(4) . . ? N2A C9A H9AA 110.6 . . ? C8A C9A H9AA 110.6 . . ? N2A C9A H9AB 110.6 . . ? C8A C9A H9AB 110.6 . . ? H9AA C9A H9AB 108.8 . . ? N2A C10A C11A 108.3(4) . . ? N2A C10A H10A 110.0 . . ? C11A C10A H10A 110.0 . . ? N2A C10A H10B 110.0 . . ? C11A C10A H10B 110.0 . . ? H10A C10A H10B 108.4 . . ? C12A C11A C16A 118.4(5) . . ? C12A C11A C10A 120.8(5) . . ? C16A C11A C10A 120.7(5) . . ? C11A C12A C13A 121.8(6) . . ? C11A C12A H12A 119.1 . . ? C13A C12A H12A 119.1 . . ? C14A C13A C12A 118.5(7) . . ? C14A C13A H13A 120.7 . . ? C12A C13A H13A 120.7 . . ? C15A C14A C13A 120.9(6) . . ? C15A C14A H14A 119.5 . . ? C13A C14A H14A 119.6 . . ? C14A C15A C16A 120.1(6) . . ? C14A C15A H15A 120.0 . . ? C16A C15A H15A 120.0 . . ? C15A C16A C11A 120.3(5) . . ? C15A C16A Se2 119.4(4) . . ? C11A C16A Se2 120.3(4) . . ? C2B C1B C6B 120.2(5) . . ? C2B C1B Se1 119.5(4) . . ? C6B C1B Se1 120.4(4) . . ? C3B C2B C1B 120.2(5) . . ? C3B C2B H2BA 119.9 . . ? C1B C2B H2BA 119.9 . . ? C4B C3B C2B 119.9(5) . . ? C4B C3B H3BA 120.0 . . ? C2B C3B H3BA 120.0 . . ? C5B C4B C3B 119.6(6) . . ? C5B C4B H4BA 120.2 . . ? C3B C4B H4BA 120.2 . . ? C4B C5B C6B 121.9(5) . . ? C4B C5B H5BA 119.1 . . ? C6B C5B H5BA 119.1 . . ? C5B C6B C1B 118.2(5) . . ? C5B C6B C7B 119.8(5) . . ? C1B C6B C7B 122.0(5) . . ? N1B C7B C6B 111.3(4) . . ? N1B C7B H7BA 109.4 . . ? C6B C7B H7BA 109.4 . . ? N1B C7B H7BB 109.4 . . ? C6B C7B H7BB 109.4 . . ? H7BA C7B H7BB 108.0 . . ? N1B C8B C9B 111.0(4) . . ? N1B C8B H8BA 109.4 . . ? C9B C8B H8BA 109.4 . . ? N1B C8B H8BB 109.4 . . ? C9B C8B H8BB 109.4 . . ? H8BA C8B H8BB 108.0 . . ? N2B C9B C8B 113.4(4) . . ? N2B C9B H9BA 108.9 . . ? C8B C9B H9BA 108.9 . . ? N2B C9B H9BB 108.9 . . ? C8B C9B H9BB 108.9 . . ? H9BA C9B H9BB 107.7 . . ? N2B C10B C11B 115.3(5) . . ? N2B C10B H10C 122.4 . . ? C11B C10B H10C 122.4 . . ? C16B C11B C12B 121.4(5) . . ? C16B C11B C10B 116.1(5) . . ? C12B C11B C10B 122.4(5) . . ? C13B C12B C11B 118.8(5) . . ? C13B C12B H12B 120.6 . . ? C11B C12B H12B 120.6 . . ? C14B C13B C12B 120.0(5) . . ? C14B C13B H13B 120.0 . . ? C12B C13B H13B 120.0 . . ? C13B C14B C15B 120.9(5) . . ? C13B C14B H14B 119.5 . . ? C15B C14B H14B 119.5 . . ? C16B C15B C14B 119.9(5) . . ? C16B C15B H15B 120.0 . . ? C14B C15B H15B 120.0 . . ? C15B C16B C11B 119.0(5) . . ? C15B C16B Pt 128.5(4) . . ? C11B C16B Pt 112.4(4) . . ? 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 C16B Pt Se2 C16A -60.2(2) . . . . ? N2B Pt Se2 C16A -141.8(2) . . . . ? N2A Pt Se2 C16A 33.9(2) . . . . ? N1A Pt Se2 C16A 81.1(10) . . . . ? Cl1 Pt Se2 C16A 123.39(17) . . . . ? C16B Pt N1A C7A -39.1(3) . . . . ? N2B Pt N1A C7A 43.1(3) . . . . ? N2A Pt N1A C7A -132.5(3) . . . . ? Se2 Pt N1A C7A 179.8(8) . . . . ? Cl1 Pt N1A C7A 137.4(3) . . . . ? C16B Pt N1A C8A 90.8(3) . . . . ? N2B Pt N1A C8A 173.0(3) . . . . ? N2A Pt N1A C8A -2.6(3) . . . . ? Se2 Pt N1A C8A -50.3(11) . . . . ? Cl1 Pt N1A C8A -92.7(3) . . . . ? C16B Pt N2A C10A 106.5(4) . . . . ? N2B Pt N2A C10A 116(2) . . . . ? N1A Pt N2A C10A -158.2(4) . . . . ? Se2 Pt N2A C10A 17.7(4) . . . . ? Cl1 Pt N2A C10A -73.1(4) . . . . ? C16B Pt N2A C9A -122.4(3) . . . . ? N2B Pt N2A C9A -112(2) . . . . ? N1A Pt N2A C9A -27.1(3) . . . . ? Se2 Pt N2A C9A 148.8(3) . . . . ? Cl1 Pt N2A C9A 58.0(3) . . . . ? C16B Pt N2B C10B -8.9(4) . . . . ? N2A Pt N2B C10B -19(2) . . . . ? N1A Pt N2B C10B -103.7(4) . . . . ? Se2 Pt N2B C10B 80.1(4) . . . . ? Cl1 Pt N2B C10B 170.6(4) . . . . ? C16B Pt N2B C9B -163.0(4) . . . . ? N2A Pt N2B C9B -173.0(19) . . . . ? N1A Pt N2B C9B 102.2(4) . . . . ? Se2 Pt N2B C9B -74.0(4) . . . . ? Cl1 Pt N2B C9B 16.6(4) . . . . ? C1B Se1 C1A C2A -99.0(4) . . . . ? C1B Se1 C1A C6A 80.4(4) . . . . ? C6A C1A C2A C3A -0.9(8) . . . . ? Se1 C1A C2A C3A 178.5(4) . . . . ? C1A C2A C3A C4A -2.2(8) . . . . ? C2A C3A C4A C5A 3.0(8) . . . . ? C3A C4A C5A C6A -0.7(8) . . . . ? C4A C5A C6A C1A -2.3(7) . . . . ? C4A C5A C6A C7A 174.5(5) . . . . ? C2A C1A C6A C5A 3.1(7) . . . . ? Se1 C1A C6A C5A -176.3(4) . . . . ? C2A C1A C6A C7A -173.5(5) . . . . ? Se1 C1A C6A C7A 7.0(7) . . . . ? C8A N1A C7A C6A 41.6(5) . . . . ? Pt N1A C7A C6A 167.6(3) . . . . ? C5A C6A C7A N1A -104.9(5) . . . . ? C1A C6A C7A N1A 71.7(6) . . . . ? C7A N1A C8A C9A 166.1(4) . . . . ? Pt N1A C8A C9A 32.5(4) . . . . ? C10A N2A C9A C8A -175.6(4) . . . . ? Pt N2A C9A C8A 51.7(4) . . . . ? N1A C8A C9A N2A -56.9(5) . . . . ? C9A N2A C10A C11A 158.0(4) . . . . ? Pt N2A C10A C11A -74.3(5) . . . . ? N2A C10A C11A C12A -107.5(6) . . . . ? N2A C10A C11A C16A 69.3(6) . . . . ? C16A C11A C12A C13A -0.1(9) . . . . ? C10A C11A C12A C13A 176.8(6) . . . . ? C11A C12A C13A C14A -0.3(10) . . . . ? C12A C13A C14A C15A 1.2(10) . . . . ? C13A C14A C15A C16A -1.5(10) . . . . ? C14A C15A C16A C11A 1.1(9) . . . . ? C14A C15A C16A Se2 -179.4(5) . . . . ? C12A C11A C16A C15A -0.2(8) . . . . ? C10A C11A C16A C15A -177.1(5) . . . . ? C12A C11A C16A Se2 -179.8(4) . . . . ? C10A C11A C16A Se2 3.3(7) . . . . ? Pt Se2 C16A C15A 129.8(4) . . . . ? Pt Se2 C16A C11A -50.6(4) . . . . ? C1A Se1 C1B C2B 45.1(4) . . . . ? C1A Se1 C1B C6B -136.4(4) . . . . ? C6B C1B C2B C3B 2.0(7) . . . . ? Se1 C1B C2B C3B -179.4(4) . . . . ? C1B C2B C3B C4B 0.6(8) . . . . ? C2B C3B C4B C5B -2.3(8) . . . . ? C3B C4B C5B C6B 1.3(8) . . . . ? C4B C5B C6B C1B 1.3(8) . . . . ? C4B C5B C6B C7B 179.8(5) . . . . ? C2B C1B C6B C5B -2.9(7) . . . . ? Se1 C1B C6B C5B 178.5(4) . . . . ? C2B C1B C6B C7B 178.6(4) . . . . ? Se1 C1B C6B C7B 0.0(6) . . . . ? C8B N1B C7B C6B -171.5(4) . . . . ? C5B C6B C7B N1B -89.7(6) . . . . ? C1B C6B C7B N1B 88.8(6) . . . . ? C7B N1B C8B C9B -173.5(4) . . . . ? C10B N2B C9B C8B 122.7(6) . . . . ? Pt N2B C9B C8B -84.2(5) . . . . ? N1B C8B C9B N2B -44.2(6) . . . . ? C9B N2B C10B C11B 168.2(5) . . . . ? Pt N2B C10B C11B 12.4(7) . . . . ? N2B C10B C11B C16B -9.7(8) . . . . ? N2B C10B C11B C12B 174.9(5) . . . . ? C16B C11B C12B C13B 1.2(8) . . . . ? C10B C11B C12B C13B 176.4(5) . . . . ? C11B C12B C13B C14B 0.5(8) . . . . ? C12B C13B C14B C15B -1.5(8) . . . . ? C13B C14B C15B C16B 0.8(8) . . . . ? C14B C15B C16B C11B 0.9(7) . . . . ? C14B C15B C16B Pt -178.2(4) . . . . ? C12B C11B C16B C15B -2.0(7) . . . . ? C10B C11B C16B C15B -177.4(5) . . . . ? C12B C11B C16B Pt 177.3(4) . . . . ? C10B C11B C16B Pt 1.9(6) . . . . ? N2B Pt C16B C15B -177.3(4) . . . . ? N2A Pt C16B C15B 2.0(4) . . . . ? N1A Pt C16B C15B -80.7(4) . . . . ? Se2 Pt C16B C15B 95.8(4) . . . . ? Cl1 Pt C16B C15B 176.0(17) . . . . ? N2B Pt C16B C11B 3.5(3) . . . . ? N2A Pt C16B C11B -177.2(3) . . . . ? N1A Pt C16B C11B 100.1(3) . . . . ? Se2 Pt C16B C11B -83.4(3) . . . . ? Cl1 Pt C16B C11B -3(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1WA H1WB Cl2 0.85(2) 2.8(2) 2.96(3) 96(14) . O1WB H1WD O2WB 0.85(2) 1.79(4) 2.62(3) 168(15) . O2WA H2WA O2WA 0.85(2) 1.61(16) 2.07(7) 111(14) 2_634 O2WA H2WB O1WA 0.85(2) 2.50(17) 2.95(4) 114(14) . O2WB H2WD Cl1 0.85(2) 2.59(16) 3.20(2) 129(17) 1_455 N2A H2AB Cl2 0.93 2.47 3.201(4) 135.3 1_545 N1B H1B Cl2 0.92 2.45 3.373(5) 175.8 . N2B H2BB N1B 0.93 2.13 2.788(6) 127.1 . _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 1.985 _refine_diff_density_min -2.270 _refine_diff_density_rms 0.165 #===END data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 221527' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H36 F12 N4 P2 Pd Se2' _chemical_formula_weight 1030.91 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' F F 0.0171 0.0103 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9501(14) _cell_length_b 10.5010(15) _cell_length_c 10.6403(16) _cell_angle_alpha 103.622(2) _cell_angle_beta 117.296(2) _cell_angle_gamma 103.042(3) _cell_volume 885.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description chunk _exptl_crystal_colour 'very pale y' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.933 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 2.765 _exptl_absorpt_correction_type Sadabs _exptl_absorpt_correction_T_min 0.6350 _exptl_absorpt_correction_T_max 0.8927 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5787 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.33 _reflns_number_total 4045 _reflns_number_gt 3317 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.6220P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0009(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4045 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.5000 0.5000 0.5000 0.01625(10) Uani 1 2 d S . . Se Se 0.74026(4) 0.88294(4) 0.96277(4) 0.02432(11) Uani 1 1 d . . . P P 0.81953(11) 0.56927(9) 1.20694(10) 0.0233(2) Uani 1 1 d . . . F1 F 0.7639(4) 0.4033(3) 1.1621(3) 0.0682(9) Uani 1 1 d . . . F2 F 0.6953(3) 0.5705(3) 1.2637(3) 0.0478(6) Uani 1 1 d . . . F3 F 0.8754(3) 0.7357(2) 1.2567(3) 0.0556(7) Uani 1 1 d . . . F4 F 0.9443(3) 0.5695(3) 1.1531(3) 0.0564(8) Uani 1 1 d . . . F5 F 0.6828(3) 0.5466(3) 1.0394(3) 0.0457(6) Uani 1 1 d . . . F6 F 0.9600(3) 0.5938(3) 1.3753(3) 0.0479(6) Uani 1 1 d . . . N1A N 0.6399(3) 0.5253(3) 0.7264(3) 0.0215(6) Uani 1 1 d . . . H1AA H 0.5921 0.5599 0.7767 0.016(9) Uiso 1 1 calc R . . N1B N 0.4515(3) 0.6806(3) 0.5447(3) 0.0183(5) Uani 1 1 d . . . H1BA H 0.5521 0.7564 0.5973 0.032(11) Uiso 1 1 calc R . . C1A C 0.8121(4) 0.8674(3) 0.8211(4) 0.0200(7) Uani 1 1 d . . . C2A C 0.8288(4) 0.9752(4) 0.7676(4) 0.0245(7) Uani 1 1 d . . . H2AA H 0.8123 1.0575 0.8064 0.018(9) Uiso 1 1 calc R . . C3A C 0.8692(4) 0.9633(4) 0.6588(4) 0.0292(8) Uani 1 1 d . . . H3AA H 0.8780 1.0361 0.6208 0.042(12) Uiso 1 1 calc R . . C4A C 0.8968(4) 0.8450(4) 0.6054(4) 0.0319(8) Uani 1 1 d . . . H4AA H 0.9235 0.8359 0.5295 0.026(10) Uiso 1 1 calc R . . C5A C 0.8857(4) 0.7394(4) 0.6617(4) 0.0279(8) Uani 1 1 d . . . H5AA H 0.9090 0.6604 0.6268 0.040(12) Uiso 1 1 calc R . . C6A C 0.8408(4) 0.7473(3) 0.7686(4) 0.0218(7) Uani 1 1 d . . . C7A C 0.8173(4) 0.6240(3) 0.8162(4) 0.0246(7) Uani 1 1 d . . . H7AA H 0.8822 0.5707 0.7999 0.028(10) Uiso 1 1 calc R . . H7AB H 0.8587 0.6604 0.9272 0.023(9) Uiso 1 1 calc R . . C8A C 0.6208(4) 0.3773(3) 0.7208(4) 0.0239(7) Uani 1 1 d . . . H8AA H 0.7002 0.3814 0.8228 0.033(10) Uiso 1 1 calc R . . H8AB H 0.5087 0.3240 0.6927 0.022(9) Uiso 1 1 calc R . . C1B C 0.5693(4) 0.9474(3) 0.8586(4) 0.0216(7) Uani 1 1 d . . . C2B C 0.5969(4) 1.0884(4) 0.9274(4) 0.0256(7) Uani 1 1 d . . . H2BA H 0.6996 1.1503 1.0186 0.024(9) Uiso 1 1 calc R . . C3B C 0.4755(4) 1.1392(4) 0.8638(4) 0.0264(8) Uani 1 1 d . . . H3BA H 0.4950 1.2360 0.9108 0.023(9) Uiso 1 1 calc R . . C4B C 0.3252(5) 1.0485(4) 0.7312(4) 0.0299(8) Uani 1 1 d . . . H4BA H 0.2409 1.0826 0.6879 0.048(13) Uiso 1 1 calc R . . C5B C 0.2982(4) 0.9074(4) 0.6616(4) 0.0270(8) Uani 1 1 d . . . H5BA H 0.1956 0.8462 0.5699 0.039(11) Uiso 1 1 calc R . . C6B C 0.4190(4) 0.8546(3) 0.7242(4) 0.0198(7) Uani 1 1 d . . . C7B C 0.3847(4) 0.7007(3) 0.6461(4) 0.0206(7) Uani 1 1 d . . . H7BA H 0.4342 0.6627 0.7253 0.031(10) Uiso 1 1 calc R . . H7BB H 0.2647 0.6458 0.5833 0.021(9) Uiso 1 1 calc R . . C8B C 0.3487(4) 0.6953(4) 0.3974(4) 0.0242(7) Uani 1 1 d . . . H8BA H 0.3767 0.7972 0.4148 0.029(10) Uiso 1 1 calc R . . H8BB H 0.2312 0.6519 0.3601 0.011(8) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01603(18) 0.01512(18) 0.01702(18) 0.00589(13) 0.00829(14) 0.00690(13) Se 0.02326(19) 0.0308(2) 0.02083(19) 0.01028(15) 0.01205(15) 0.01301(15) P 0.0231(4) 0.0202(4) 0.0227(4) 0.0058(3) 0.0103(4) 0.0090(4) F1 0.097(2) 0.0221(13) 0.0626(19) 0.0070(12) 0.0344(17) 0.0161(14) F2 0.0397(14) 0.0677(17) 0.0478(15) 0.0278(13) 0.0307(12) 0.0187(12) F3 0.0742(19) 0.0236(13) 0.0699(19) 0.0171(12) 0.0422(16) 0.0143(12) F4 0.0426(15) 0.105(2) 0.0460(15) 0.0347(15) 0.0315(13) 0.0461(15) F5 0.0328(13) 0.0748(18) 0.0286(12) 0.0221(12) 0.0127(10) 0.0260(12) F6 0.0381(14) 0.0652(17) 0.0272(12) 0.0184(12) 0.0081(10) 0.0194(12) N1A 0.0236(14) 0.0214(14) 0.0210(14) 0.0090(11) 0.0118(12) 0.0110(12) N1B 0.0171(13) 0.0167(13) 0.0207(14) 0.0063(11) 0.0099(11) 0.0080(11) C1A 0.0153(15) 0.0223(16) 0.0179(15) 0.0059(13) 0.0077(13) 0.0051(13) C2A 0.0215(17) 0.0218(17) 0.0230(17) 0.0062(14) 0.0090(14) 0.0059(14) C3A 0.0233(18) 0.033(2) 0.0266(19) 0.0139(16) 0.0117(15) 0.0058(15) C4A 0.0255(19) 0.040(2) 0.0275(19) 0.0099(17) 0.0167(16) 0.0069(16) C5A 0.0223(17) 0.0266(18) 0.0263(18) 0.0021(15) 0.0115(15) 0.0077(14) C6A 0.0150(15) 0.0211(16) 0.0189(16) 0.0030(13) 0.0055(13) 0.0035(13) C7A 0.0209(17) 0.0211(17) 0.0254(18) 0.0072(14) 0.0075(14) 0.0108(14) C8A 0.0295(19) 0.0214(17) 0.0230(17) 0.0118(14) 0.0140(15) 0.0105(14) C1B 0.0229(17) 0.0263(17) 0.0240(17) 0.0120(14) 0.0160(14) 0.0136(14) C2B 0.0260(18) 0.0248(17) 0.0250(18) 0.0070(14) 0.0160(15) 0.0064(14) C3B 0.037(2) 0.0195(17) 0.0316(19) 0.0093(15) 0.0241(17) 0.0129(15) C4B 0.036(2) 0.032(2) 0.033(2) 0.0169(16) 0.0207(17) 0.0232(17) C5B 0.0258(18) 0.0280(18) 0.0252(18) 0.0080(15) 0.0117(15) 0.0140(15) C6B 0.0207(16) 0.0206(16) 0.0236(16) 0.0090(13) 0.0148(14) 0.0102(13) C7B 0.0165(15) 0.0206(16) 0.0252(17) 0.0076(13) 0.0121(14) 0.0075(13) C8B 0.0262(18) 0.0198(16) 0.0235(17) 0.0086(13) 0.0104(14) 0.0104(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N1B 2.063(2) . ? Pd N1B 2.063(2) 2_666 ? Pd N1A 2.066(3) 2_666 ? Pd N1A 2.066(3) . ? Se C1B 1.929(3) . ? Se C1A 1.933(3) . ? P F3 1.581(2) . ? P F1 1.582(3) . ? P F5 1.586(2) . ? P F4 1.587(3) . ? P F6 1.598(2) . ? P F2 1.606(2) . ? N1A C7A 1.505(4) . ? N1A C8A 1.505(4) . ? N1B C8B 1.497(4) . ? N1B C7B 1.505(4) . ? C1A C2A 1.392(5) . ? C1A C6A 1.400(4) . ? C2A C3A 1.378(5) . ? C3A C4A 1.381(5) . ? C4A C5A 1.385(5) . ? C5A C6A 1.393(5) . ? C6A C7A 1.506(5) . ? C8A C8B 1.503(5) 2_666 ? C1B C2B 1.388(5) . ? C1B C6B 1.398(5) . ? C2B C3B 1.383(5) . ? C3B C4B 1.387(5) . ? C4B C5B 1.391(5) . ? C5B C6B 1.391(4) . ? C6B C7B 1.509(4) . ? C8B C8A 1.503(5) 2_666 ? 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 N1B Pd N1B 180.000(1) . 2_666 ? N1B Pd N1A 83.73(10) . 2_666 ? N1B Pd N1A 96.27(10) 2_666 2_666 ? N1B Pd N1A 96.27(10) . . ? N1B Pd N1A 83.73(10) 2_666 . ? N1A Pd N1A 180.000(1) 2_666 . ? C1B Se C1A 96.78(14) . . ? F3 P F1 178.19(17) . . ? F3 P F5 90.04(15) . . ? F1 P F5 91.25(15) . . ? F3 P F4 90.40(16) . . ? F1 P F4 90.88(17) . . ? F5 P F4 89.43(13) . . ? F3 P F6 89.40(15) . . ? F1 P F6 89.32(15) . . ? F5 P F6 178.87(15) . . ? F4 P F6 89.59(14) . . ? F3 P F2 89.16(15) . . ? F1 P F2 89.54(16) . . ? F5 P F2 91.22(13) . . ? F4 P F2 179.22(17) . . ? F6 P F2 89.76(14) . . ? C7A N1A C8A 111.9(2) . . ? C7A N1A Pd 116.7(2) . . ? C8A N1A Pd 105.12(19) . . ? C8B N1B C7B 111.9(2) . . ? C8B N1B Pd 109.97(19) . . ? C7B N1B Pd 117.22(19) . . ? C2A C1A C6A 120.6(3) . . ? C2A C1A Se 118.8(2) . . ? C6A C1A Se 120.5(2) . . ? C3A C2A C1A 120.4(3) . . ? C2A C3A C4A 119.6(3) . . ? C3A C4A C5A 120.3(3) . . ? C4A C5A C6A 121.1(3) . . ? C5A C6A C1A 117.9(3) . . ? C5A C6A C7A 118.8(3) . . ? C1A C6A C7A 123.2(3) . . ? N1A C7A C6A 111.7(3) . . ? C8B C8A N1A 108.1(3) 2_666 . ? C2B C1B C6B 120.7(3) . . ? C2B C1B Se 117.4(3) . . ? C6B C1B Se 121.8(2) . . ? C3B C2B C1B 120.3(3) . . ? C2B C3B C4B 119.8(3) . . ? C3B C4B C5B 119.8(3) . . ? C4B C5B C6B 121.1(3) . . ? C5B C6B C1B 118.3(3) . . ? C5B C6B C7B 119.6(3) . . ? C1B C6B C7B 122.1(3) . . ? N1B C7B C6B 112.5(3) . . ? N1B C8B C8A 109.4(3) . 2_666 ? 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 N1B Pd N1A C7A -82.5(2) . . . . ? N1B Pd N1A C7A 97.5(2) 2_666 . . . ? N1A Pd N1A C7A 120(100) 2_666 . . . ? N1B Pd N1A C8A 152.9(2) . . . . ? N1B Pd N1A C8A -27.1(2) 2_666 . . . ? N1A Pd N1A C8A -4(100) 2_666 . . . ? N1B Pd N1B C8B -77(100) 2_666 . . . ? N1A Pd N1B C8B -0.6(2) 2_666 . . . ? N1A Pd N1B C8B 179.4(2) . . . . ? N1B Pd N1B C7B 52(100) 2_666 . . . ? N1A Pd N1B C7B 128.7(2) 2_666 . . . ? N1A Pd N1B C7B -51.3(2) . . . . ? C1B Se C1A C2A 43.2(3) . . . . ? C1B Se C1A C6A -134.4(3) . . . . ? C6A C1A C2A C3A 1.9(5) . . . . ? Se C1A C2A C3A -175.7(3) . . . . ? C1A C2A C3A C4A -1.5(5) . . . . ? C2A C3A C4A C5A -0.7(5) . . . . ? C3A C4A C5A C6A 2.4(5) . . . . ? C4A C5A C6A C1A -1.9(5) . . . . ? C4A C5A C6A C7A 175.1(3) . . . . ? C2A C1A C6A C5A -0.2(5) . . . . ? Se C1A C6A C5A 177.4(2) . . . . ? C2A C1A C6A C7A -177.1(3) . . . . ? Se C1A C6A C7A 0.5(4) . . . . ? C8A N1A C7A C6A 155.7(3) . . . . ? Pd N1A C7A C6A 34.6(3) . . . . ? C5A C6A C7A N1A -96.5(4) . . . . ? C1A C6A C7A N1A 80.4(4) . . . . ? C7A N1A C8A C8B -78.3(3) . . . 2_666 ? Pd N1A C8A C8B 49.2(3) . . . 2_666 ? C1A Se C1B C2B -108.0(3) . . . . ? C1A Se C1B C6B 76.1(3) . . . . ? C6B C1B C2B C3B 0.0(5) . . . . ? Se C1B C2B C3B -176.0(3) . . . . ? C1B C2B C3B C4B 0.4(5) . . . . ? C2B C3B C4B C5B -0.9(6) . . . . ? C3B C4B C5B C6B 1.0(6) . . . . ? C4B C5B C6B C1B -0.5(5) . . . . ? C4B C5B C6B C7B 179.6(3) . . . . ? C2B C1B C6B C5B 0.0(5) . . . . ? Se C1B C6B C5B 175.9(3) . . . . ? C2B C1B C6B C7B 179.9(3) . . . . ? Se C1B C6B C7B -4.2(4) . . . . ? C8B N1B C7B C6B -75.6(3) . . . . ? Pd N1B C7B C6B 156.1(2) . . . . ? C5B C6B C7B N1B 97.7(4) . . . . ? C1B C6B C7B N1B -82.2(4) . . . . ? C7B N1B C8B C8A -158.8(3) . . . 2_666 ? Pd N1B C8B C8A -26.7(3) . . . 2_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1AA F5 0.93 2.56 3.102(4) 117.2 . _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.756 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.095 #===END data_compound_7 _database_code_depnum_ccdc_archive 'CCDC 221528' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H50 Cl2 N4 O7 Pd Te2' _chemical_formula_weight 1035.26 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.072(6) _cell_length_b 13.264(6) _cell_length_c 14.527(7) _cell_angle_alpha 104.235(8) _cell_angle_beta 107.668(9) _cell_angle_gamma 110.244(8) _cell_volume 1912.6(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description chunk _exptl_crystal_colour orange-yell _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 2.169 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.646333 _exptl_absorpt_correction_T_max 0.928075 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13450 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8797 _reflns_number_gt 7420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0613P)^2^+49.8723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8797 _refine_ls_number_parameters 441 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0938 _refine_ls_R_factor_gt 0.0782 _refine_ls_wR_factor_ref 0.2003 _refine_ls_wR_factor_gt 0.1844 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.273 _refine_ls_shift/su_mean 0.010 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 0.20842(3) 0.28054(3) 0.12594(3) 0.02350(8) Uani 1 1 d . A . Te2A Te 0.06975(4) 0.34248(4) 0.30931(4) 0.01957(11) Uani 0.8235(13) 1 d P A 1 Te2B Te 0.0961(2) 0.3857(2) 0.33674(19) 0.0224(5) Uani 0.1765(13) 1 d P A 2 Pd Pd 0.26518(4) 0.46208(4) 0.28014(3) 0.02429(10) Uani 1 1 d . . . Cl1 Cl 0.1937(3) 0.7894(3) 0.2802(3) 0.1036(9) Uani 1 1 d . . . Cl2 Cl 0.3959(3) 0.4624(3) 0.5247(3) 0.0813(9) Uani 1 1 d . . . O1W O 0.23400(6) 0.20744(4) 0.4770(2) 0.067(2) Uani 1 1 d D . . H1W1 H 0.28551(11) 0.28026(3) 0.5078(4) 0.100 Uiso 1 1 d D . . H1W2 H 0.28124(13) 0.17525(9) 0.4972(4) 0.100 Uiso 1 1 d D . . O2W O -0.06477(6) 0.05495(7) 0.43316(6) 0.0776(15) Uani 1 1 d D . . H2W1 H -0.04968(11) 0.00310(9) 0.39933(8) 0.116 Uiso 1 1 d D . . H2W2 H 0.00021(13) 0.09071(14) 0.49305(7) 0.116 Uiso 1 1 d D . . O3W O 0.68219(7) 1.02555(6) 0.34629(5) 0.0403(12) Uani 1 1 d D . . H3W1 H 0.73074(9) 1.00272(10) 0.38222(7) 0.060 Uiso 1 1 d D . . H3W2 H 0.63963(18) 0.97062(12) 0.28558(6) 0.060 Uiso 1 1 d D . . O4W O 0.45387(5) 0.96819(14) 0.35269(6) 0.118(4) Uani 1 1 d D . . H4W1 H 0.38277(4) 0.9389(3) 0.29800(10) 0.177 Uiso 1 1 d D . . H4W2 H 0.51275(6) 1.0005(3) 0.33421(14) 0.177 Uiso 1 1 d D . . O5W O -0.00385(4) -0.13618(11) 0.31822(7) 0.147(6) Uani 1 1 d D . . H5W1 H -0.08223(4) -0.17134(15) 0.27151(11) 0.221 Uiso 1 1 d D . . H5W2 H 0.03748(7) -0.1620(2) 0.28897(18) 0.221 Uiso 1 1 d D . . O6W O 0.29462(5) -0.00198(5) 0.47529(10) 0.185(8) Uani 1 1 d D . . H6W1 H 0.24874(7) -0.07550(5) 0.44234(18) 0.277 Uiso 1 1 d D . . H6W2 H 0.36381(8) 0.01283(15) 0.46598(15) 0.277 Uiso 1 1 d D . . O7WA O 0.615(2) 0.865(2) 0.2091(15) 0.111(10) Uani 0.463(16) 1 d P B 1 O7WB O 0.7096(16) 0.8001(11) 0.2117(13) 0.080(5) Uani 0.537(16) 1 d P B 2 N1A N 0.4415(5) 0.5644(4) 0.2772(4) 0.0231(11) Uani 1 1 d . A . H1AA H 0.5038 0.5656 0.3313 0.028 Uiso 1 1 d R . . N2A N 0.2887(5) 0.6252(5) 0.3728(4) 0.0346(13) Uani 1 1 d . A . H2AB H 0.2396 0.6454 0.3279 0.042 Uiso 1 1 d R . . N1B N 0.2318(5) 0.1711(5) 0.2544(5) 0.0333(12) Uani 1 1 d . A . H1B H 0.2104 0.1972 0.3065 0.040 Uiso 1 1 d R . . N2B N -0.0255(5) 0.0804(5) 0.2245(5) 0.0374(14) Uani 1 1 d . . . H2B H -0.0223 0.0524 0.2752 0.045 Uiso 1 1 d R . . C1A C 0.2499(3) 0.3892(2) 0.0402(2) 0.0283(13) Uani 1 1 d G . . C2A C 0.1530(3) 0.3547(3) -0.0589(3) 0.0282(14) Uani 1 1 d G A . H2AA H 0.0755 0.2865 -0.0859 0.034 Uiso 1 1 calc R . . C3A C 0.1720(4) 0.4221(4) -0.1176(3) 0.0337(15) Uani 1 1 d G A . H3AA H 0.1072 0.3990 -0.1839 0.040 Uiso 1 1 calc R . . C4A C 0.2878(5) 0.5241(4) -0.0772(3) 0.0328(15) Uani 1 1 d G A . H4AA H 0.3005 0.5693 -0.1165 0.039 Uiso 1 1 calc R . . C5A C 0.3847(4) 0.5587(3) 0.0218(4) 0.0304(13) Uani 1 1 d G A . H5AA H 0.4622 0.6269 0.0489 0.036 Uiso 1 1 calc R . . C6A C 0.3657(3) 0.4912(3) 0.0805(3) 0.0288(13) Uani 1 1 d G A . C7A C 0.4750(5) 0.5314(5) 0.1875(5) 0.0249(13) Uani 1 1 d . . . H7AA H 0.4994 0.4693 0.1891 0.030 Uiso 1 1 calc R A . H7AB H 0.5504 0.5982 0.1967 0.030 Uiso 1 1 calc R . . C8A C 0.4577(6) 0.6870(5) 0.3123(5) 0.0298(14) Uani 1 1 d . . . H8AA H 0.4004 0.6966 0.2555 0.036 Uiso 1 1 calc R A . H8AB H 0.5470 0.7422 0.3327 0.036 Uiso 1 1 calc R . . C9A C 0.4235(6) 0.7089(6) 0.4050(5) 0.0343(15) Uani 1 1 d . A . H9AA H 0.4819 0.7004 0.4620 0.041 Uiso 1 1 calc R . . H9AB H 0.4337 0.7879 0.4299 0.041 Uiso 1 1 calc R . . C10A C 0.2492(6) 0.6371(7) 0.4607(5) 0.0364(16) Uani 1 1 d . . . H10A H 0.2934 0.7187 0.5080 0.044 Uiso 1 1 calc R A . H10B H 0.2768 0.5938 0.4997 0.044 Uiso 1 1 calc R . . C11A C 0.1011(3) 0.5923(3) 0.4226(3) 0.0407(15) Uani 1 1 d G A . C12A C 0.0557(4) 0.6715(3) 0.4547(4) 0.0504(18) Uani 1 1 d G . . H12A H 0.1146 0.7492 0.4978 0.060 Uiso 1 1 calc R A . C13A C -0.0776(5) 0.6346(5) 0.4222(4) 0.0608(17) Uani 1 1 d G A . H13A H -0.1079 0.6876 0.4436 0.073 Uiso 1 1 calc R . . C14A C -0.1655(3) 0.5185(5) 0.3577(4) 0.0513(18) Uani 1 1 d G . . H14A H -0.2547 0.4938 0.3359 0.062 Uiso 1 1 calc R A . C15A C -0.1201(3) 0.4393(4) 0.3256(4) 0.0433(16) Uani 1 1 d G A . H15A H -0.1790 0.3616 0.2824 0.052 Uiso 1 1 calc R . . C16A C 0.0132(3) 0.4762(3) 0.3581(3) 0.0320(14) Uani 1 1 d G . . C1B C 0.3654(2) 0.2388(3) 0.1333(3) 0.0273(13) Uani 1 1 d G . . C2B C 0.4055(4) 0.2342(4) 0.0529(3) 0.0278(13) Uani 1 1 d G A . H2BA H 0.3688 0.2555 -0.0006 0.033 Uiso 1 1 calc R . . C3B C 0.5003(5) 0.1977(5) 0.0523(4) 0.0347(15) Uani 1 1 d G A . H3BA H 0.5271 0.1946 -0.0015 0.042 Uiso 1 1 calc R . . C4B C 0.5551(4) 0.1658(5) 0.1322(4) 0.0379(17) Uani 1 1 d G A . H4BA H 0.6185 0.1414 0.1318 0.045 Uiso 1 1 calc R . . C5B C 0.5150(4) 0.1704(5) 0.2126(4) 0.0349(16) Uani 1 1 d G A . H5BA H 0.5517 0.1491 0.2661 0.042 Uiso 1 1 calc R . . C6B C 0.4202(4) 0.2069(4) 0.2132(3) 0.0275(13) Uani 1 1 d G A . C7B C 0.3726(6) 0.2083(6) 0.2997(5) 0.0346(14) Uani 1 1 d . . . H7BA H 0.3910 0.1561 0.3313 0.042 Uiso 1 1 calc R A . H7BB H 0.4182 0.2865 0.3541 0.042 Uiso 1 1 calc R . . C8B C 0.1501(6) 0.0425(5) 0.1994(6) 0.0368(15) Uani 1 1 d . . . H8BA H 0.1622 0.0058 0.2492 0.044 Uiso 1 1 calc R A . H8BB H 0.1762 0.0119 0.1464 0.044 Uiso 1 1 calc R . . C9B C 0.0075(6) 0.0154(6) 0.1482(6) 0.0361(15) Uani 1 1 d . A . H9BA H -0.0082 0.0372 0.0882 0.043 Uiso 1 1 calc R . . H9BB H -0.0476 -0.0678 0.1235 0.043 Uiso 1 1 calc R . . C10B C -0.1568(7) 0.0722(7) 0.1752(6) 0.0403(18) Uani 1 1 d . . . H10C H -0.1835 0.0980 0.2295 0.048 Uiso 1 1 calc R . . H10D H -0.2191 -0.0086 0.1303 0.048 Uiso 1 1 calc R . . C11B C -0.1580(3) 0.1469(3) 0.1103(3) 0.0325(15) Uani 1 1 d G A . C12B C -0.2474(3) 0.0948(3) 0.0054(3) 0.0383(18) Uani 1 1 d G . . H12B H -0.3038 0.0151 -0.0247 0.046 Uiso 1 1 calc R . . C13B C -0.2526(4) 0.1617(4) -0.0545(3) 0.0402(18) Uani 1 1 d G . . H13B H -0.3124 0.1268 -0.1246 0.048 Uiso 1 1 calc R . . C14B C -0.1683(5) 0.2807(4) -0.0094(4) 0.0369(16) Uani 1 1 d G . . H14B H -0.1718 0.3255 -0.0495 0.044 Uiso 1 1 calc R . . C15B C -0.0789(4) 0.3328(3) 0.0955(4) 0.0321(15) Uani 1 1 d G A . H15B H -0.0225 0.4125 0.1256 0.039 Uiso 1 1 calc R . . C16B C -0.0737(3) 0.2659(3) 0.1553(3) 0.0301(14) Uani 1 1 d G . . 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 0.02667(13) 0.03369(15) 0.03435(15) 0.02673(12) 0.02239(11) 0.02209(11) Te2A 0.02526(17) 0.02380(18) 0.02431(18) 0.01547(14) 0.01737(13) 0.01666(14) Te2B 0.0256(9) 0.0324(10) 0.0267(9) 0.0248(7) 0.0136(7) 0.0204(7) Pd 0.03010(16) 0.03769(18) 0.03157(17) 0.02676(14) 0.02272(13) 0.02616(14) Cl1 0.0969(14) 0.186(2) 0.1135(16) 0.1135(14) 0.0684(12) 0.0970(14) Cl2 0.0838(13) 0.0917(14) 0.0791(17) 0.0322(12) 0.0205(13) 0.0644(11) O1W 0.063(3) 0.063(3) 0.104(4) 0.038(3) 0.058(3) 0.036(3) O2W 0.110(2) 0.174(4) 0.065(2) 0.089(2) 0.0773(18) 0.126(2) O3W 0.049(2) 0.058(2) 0.046(2) 0.0378(17) 0.0370(16) 0.0318(19) O4W 0.145(6) 0.105(4) 0.137(6) 0.085(4) 0.030(5) 0.092(4) O5W 0.177(11) 0.111(6) 0.083(5) 0.065(5) 0.035(6) -0.012(8) O6W 0.125(8) 0.167(14) 0.173(12) -0.025(10) 0.083(8) 0.019(9) O7WA 0.111(13) 0.135(18) 0.067(9) 0.046(10) 0.055(9) 0.015(13) O7WB 0.125(9) 0.047(6) 0.100(9) 0.033(6) 0.072(7) 0.050(6) N1A 0.0259(18) 0.0261(19) 0.032(2) 0.0203(16) 0.0180(16) 0.0167(15) N2A 0.050(2) 0.057(3) 0.031(2) 0.0320(18) 0.0281(18) 0.040(2) N1B 0.047(2) 0.043(2) 0.051(2) 0.0367(18) 0.0387(18) 0.0368(17) N2B 0.039(2) 0.045(2) 0.056(3) 0.038(2) 0.032(2) 0.027(2) C1A 0.033(2) 0.043(3) 0.035(2) 0.029(2) 0.0246(19) 0.027(2) C2A 0.029(2) 0.032(3) 0.034(3) 0.022(2) 0.017(2) 0.015(2) C3A 0.047(3) 0.040(3) 0.038(3) 0.029(2) 0.024(2) 0.029(2) C4A 0.045(3) 0.039(3) 0.039(3) 0.031(2) 0.027(2) 0.027(2) C5A 0.037(2) 0.040(2) 0.045(3) 0.034(2) 0.030(2) 0.027(2) C6A 0.034(2) 0.045(3) 0.041(2) 0.034(2) 0.0312(18) 0.0290(19) C7A 0.026(2) 0.034(2) 0.032(2) 0.0213(19) 0.0194(18) 0.0186(19) C8A 0.039(2) 0.034(2) 0.036(3) 0.023(2) 0.022(2) 0.027(2) C9A 0.046(3) 0.046(3) 0.038(3) 0.029(2) 0.023(2) 0.036(2) C10A 0.042(3) 0.059(3) 0.037(3) 0.032(2) 0.028(2) 0.036(2) C11A 0.056(2) 0.079(3) 0.042(3) 0.046(2) 0.040(2) 0.057(2) C12A 0.076(3) 0.079(4) 0.058(3) 0.051(3) 0.056(2) 0.062(3) C13A 0.093(3) 0.126(4) 0.063(3) 0.074(3) 0.068(2) 0.101(3) C14A 0.060(3) 0.094(4) 0.057(3) 0.057(3) 0.043(2) 0.061(3) C15A 0.050(3) 0.082(4) 0.048(3) 0.048(2) 0.038(2) 0.053(2) C16A 0.045(2) 0.052(3) 0.034(2) 0.031(2) 0.0312(19) 0.036(2) C1B 0.027(2) 0.037(2) 0.040(3) 0.025(2) 0.0240(19) 0.0224(19) C2B 0.035(2) 0.030(2) 0.045(3) 0.0257(19) 0.030(2) 0.0237(18) C3B 0.034(2) 0.040(3) 0.056(3) 0.027(2) 0.034(2) 0.024(2) C4B 0.025(2) 0.048(3) 0.064(4) 0.032(3) 0.029(2) 0.026(2) C5B 0.027(2) 0.043(3) 0.048(3) 0.025(2) 0.016(2) 0.024(2) C6B 0.032(2) 0.027(2) 0.042(3) 0.022(2) 0.023(2) 0.0214(19) C7B 0.045(3) 0.052(3) 0.042(3) 0.035(2) 0.028(2) 0.038(2) C8B 0.048(3) 0.035(2) 0.065(3) 0.038(2) 0.040(2) 0.032(2) C9B 0.043(3) 0.031(2) 0.063(3) 0.032(2) 0.039(2) 0.023(2) C10B 0.033(3) 0.044(3) 0.059(3) 0.032(3) 0.030(2) 0.016(2) C11B 0.027(2) 0.039(3) 0.051(3) 0.025(2) 0.028(2) 0.022(2) C12B 0.027(2) 0.050(3) 0.053(3) 0.023(3) 0.026(2) 0.023(2) C13B 0.036(2) 0.057(4) 0.047(3) 0.024(3) 0.025(2) 0.033(2) C14B 0.040(2) 0.059(3) 0.038(3) 0.027(2) 0.027(2) 0.036(2) C15B 0.031(2) 0.044(3) 0.038(3) 0.026(2) 0.021(2) 0.024(2) C16B 0.032(2) 0.044(3) 0.040(3) 0.026(2) 0.0275(19) 0.028(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te1 C1B 2.131(3) . ? Te1 C1A 2.155(3) . ? Te1 Pd 2.5611(11) . ? Te2A C16B 2.085(3) . ? Te2A C16A 2.152(4) . ? Te2A Pd 2.5709(12) . ? Te2B C16A 1.838(5) . ? Te2B Pd 2.422(3) . ? Te2B C16B 2.466(4) . ? Pd N1A 2.112(5) . ? Pd N2A 2.117(6) . ? O1W H1W1 0.8501(6) . ? O1W H1W2 0.8500(6) . ? O2W H2W1 0.8500(6) . ? O2W H2W2 0.8500(6) . ? O3W H3W1 0.8500(6) . ? O3W H3W2 0.8500(6) . ? O4W H4W1 0.8500(6) . ? O4W H4W2 0.8500(6) . ? O5W H5W1 0.8500(6) . ? O5W H5W2 0.8500(6) . ? O6W H6W1 0.8500(6) . ? O6W H6W2 0.8500(6) . ? O7WA H3W2 1.43(3) . ? N1A C7A 1.488(8) . ? N1A C8A 1.501(8) . ? N1A H1AA 0.8999 . ? N2A C9A 1.461(9) . ? N2A C10A 1.484(9) . ? N2A H2AB 0.9002 . ? N1B C7B 1.466(8) . ? N1B C8B 1.485(8) . ? N1B H1B 0.9000 . ? N2B C9B 1.472(10) . ? N2B C10B 1.480(10) . ? N2B H2B 0.9000 . ? C1A C2A 1.3900 . ? C1A C6A 1.3900 . ? C2A C3A 1.3900 . ? C2A H2AA 0.9300 . ? C3A C4A 1.3900 . ? C3A H3AA 0.9300 . ? C4A C5A 1.3900 . ? C4A H4AA 0.9300 . ? C5A C6A 1.3900 . ? C5A H5AA 0.9300 . ? C6A C7A 1.517(7) . ? C7A H7AA 0.9700 . ? C7A H7AB 0.9700 . ? C8A C9A 1.515(10) . ? C8A H8AA 0.9700 . ? C8A H8AB 0.9700 . ? C9A H9AA 0.9700 . ? C9A H9AB 0.9700 . ? C10A C11A 1.536(7) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C11A C12A 1.3900 . ? C11A C16A 1.3900 . ? C12A C13A 1.3900 . ? C12A H12A 0.9300 . ? C13A C14A 1.3900 . ? C13A H13A 0.9300 . ? C14A C15A 1.3900 . ? C14A H14A 0.9300 . ? C15A C16A 1.3900 . ? C15A H15A 0.9300 . ? C1B C2B 1.3900 . ? C1B C6B 1.3900 . ? C2B C3B 1.3900 . ? C2B H2BA 0.9300 . ? C3B C4B 1.3900 . ? C3B H3BA 0.9300 . ? C4B C5B 1.3900 . ? C4B H4BA 0.9300 . ? C5B C6B 1.3900 . ? C5B H5BA 0.9300 . ? C6B C7B 1.531(8) . ? C7B H7BA 0.9700 . ? C7B H7BB 0.9700 . ? C8B C9B 1.520(10) . ? C8B H8BA 0.9700 . ? C8B H8BB 0.9700 . ? C9B H9BA 0.9700 . ? C9B H9BB 0.9700 . ? C10B C11B 1.528(9) . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C11B C12B 1.3900 . ? C11B C16B 1.3900 . ? C12B C13B 1.3900 . ? C12B H12B 0.9300 . ? C13B C14B 1.3900 . ? C13B H13B 0.9300 . ? C14B C15B 1.3900 . ? C14B H14B 0.9300 . ? C15B C16B 1.3900 . ? C15B H15B 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1B Te1 C1A 94.26(14) . . ? C1B Te1 Pd 115.05(8) . . ? C1A Te1 Pd 88.69(9) . . ? C16B Te2A C16A 94.07(16) . . ? C16B Te2A Pd 98.82(12) . . ? C16A Te2A Pd 98.92(12) . . ? C16A Te2B Pd 114.66(18) . . ? C16A Te2B C16B 91.01(18) . . ? Pd Te2B C16B 93.16(14) . . ? N1A Pd N2A 84.0(2) . . ? N1A Pd Te2B 163.06(15) . . ? N2A Pd Te2B 83.00(18) . . ? N1A Pd Te1 93.98(14) . . ? N2A Pd Te1 163.81(16) . . ? Te2B Pd Te1 101.47(7) . . ? N1A Pd Te2A 172.23(14) . . ? N2A Pd Te2A 94.02(17) . . ? Te2B Pd Te2A 11.53(6) . . ? Te1 Pd Te2A 89.94(3) . . ? H1W1 O1W H1W2 104.49(9) . . ? H2W1 O2W H2W2 104.49(8) . . ? H3W1 O3W H3W2 104.49(9) . . ? H4W1 O4W H4W2 104.49(9) . . ? H5W1 O5W H5W2 104.50(9) . . ? H6W1 O6W H6W2 104.49(8) . . ? C7A N1A C8A 113.9(5) . . ? C7A N1A Pd 123.4(3) . . ? C8A N1A Pd 105.2(4) . . ? C7A N1A H1AA 104.0 . . ? C8A N1A H1AA 104.2 . . ? Pd N1A H1AA 104.2 . . ? C9A N2A C10A 112.7(5) . . ? C9A N2A Pd 105.8(4) . . ? C10A N2A Pd 121.0(5) . . ? C9A N2A H2AB 105.0 . . ? C10A N2A H2AB 105.4 . . ? Pd N2A H2AB 105.5 . . ? C7B N1B C8B 114.2(6) . . ? C7B N1B H1B 108.4 . . ? C8B N1B H1B 108.6 . . ? C9B N2B C10B 112.4(6) . . ? C9B N2B H2B 109.3 . . ? C10B N2B H2B 109.0 . . ? C2A C1A C6A 120.0 . . ? C2A C1A Te1 116.94(15) . . ? C6A C1A Te1 123.04(15) . . ? C1A C2A C3A 120.0 . . ? C1A C2A H2AA 120.0 . . ? C3A C2A H2AA 120.0 . . ? C2A C3A C4A 120.0 . . ? C2A C3A H3AA 120.0 . . ? C4A C3A H3AA 120.0 . . ? C5A C4A C3A 120.0 . . ? C5A C4A H4AA 120.0 . . ? C3A C4A H4AA 120.0 . . ? C4A C5A C6A 120.0 . . ? C4A C5A H5AA 120.0 . . ? C6A C5A H5AA 120.0 . . ? C5A C6A C1A 120.0 . . ? C5A C6A C7A 118.1(3) . . ? C1A C6A C7A 121.9(3) . . ? N1A C7A C6A 114.4(5) . . ? N1A C7A H7AA 108.7 . . ? C6A C7A H7AA 108.7 . . ? N1A C7A H7AB 108.7 . . ? C6A C7A H7AB 108.7 . . ? H7AA C7A H7AB 107.6 . . ? N1A C8A C9A 107.9(6) . . ? N1A C8A H8AA 110.1 . . ? C9A C8A H8AA 110.1 . . ? N1A C8A H8AB 110.1 . . ? C9A C8A H8AB 110.1 . . ? H8AA C8A H8AB 108.4 . . ? N2A C9A C8A 109.3(5) . . ? N2A C9A H9AA 109.8 . . ? C8A C9A H9AA 109.8 . . ? N2A C9A H9AB 109.8 . . ? C8A C9A H9AB 109.8 . . ? H9AA C9A H9AB 108.3 . . ? N2A C10A C11A 112.5(5) . . ? N2A C10A H10A 109.1 . . ? C11A C10A H10A 109.1 . . ? N2A C10A H10B 109.1 . . ? C11A C10A H10B 109.1 . . ? H10A C10A H10B 107.8 . . ? C12A C11A C16A 120.0 . . ? C12A C11A C10A 118.1(4) . . ? C16A C11A C10A 121.9(4) . . ? C13A C12A C11A 120.0 . . ? C13A C12A H12A 120.0 . . ? C11A C12A H12A 120.0 . . ? C12A C13A C14A 120.0 . . ? C12A C13A H13A 120.0 . . ? C14A C13A H13A 120.0 . . ? C15A C14A C13A 120.0 . . ? C15A C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C14A C15A C16A 120.0 . . ? C14A C15A H15A 120.0 . . ? C16A C15A H15A 120.0 . . ? C15A C16A C11A 120.0 . . ? C15A C16A Te2B 127.7(2) . . ? C11A C16A Te2B 112.1(2) . . ? C15A C16A Te2A 115.9(2) . . ? C11A C16A Te2A 124.0(2) . . ? Te2B C16A Te2A 12.07(7) . . ? C2B C1B C6B 120.0 . . ? C2B C1B Te1 119.43(18) . . ? C6B C1B Te1 120.35(18) . . ? C3B C2B C1B 120.0 . . ? C3B C2B H2BA 120.0 . . ? C1B C2B H2BA 120.0 . . ? C2B C3B C4B 120.0 . . ? C2B C3B H3BA 120.0 . . ? C4B C3B H3BA 120.0 . . ? C5B C4B C3B 120.0 . . ? C5B C4B H4BA 120.0 . . ? C3B C4B H4BA 120.0 . . ? C6B C5B C4B 120.0 . . ? C6B C5B H5BA 120.0 . . ? C4B C5B H5BA 120.0 . . ? C5B C6B C1B 120.0 . . ? C5B C6B C7B 120.2(3) . . ? C1B C6B C7B 119.8(3) . . ? N1B C7B C6B 109.3(5) . . ? N1B C7B H7BA 109.8 . . ? C6B C7B H7BA 109.8 . . ? N1B C7B H7BB 109.8 . . ? C6B C7B H7BB 109.8 . . ? H7BA C7B H7BB 108.3 . . ? N1B C8B C9B 109.2(6) . . ? N1B C8B H8BA 109.8 . . ? C9B C8B H8BA 109.8 . . ? N1B C8B H8BB 109.8 . . ? C9B C8B H8BB 109.8 . . ? H8BA C8B H8BB 108.3 . . ? N2B C9B C8B 109.9(6) . . ? N2B C9B H9BA 109.7 . . ? C8B C9B H9BA 109.7 . . ? N2B C9B H9BB 109.7 . . ? C8B C9B H9BB 109.7 . . ? H9BA C9B H9BB 108.2 . . ? N2B C10B C11B 111.4(5) . . ? N2B C10B H10C 109.4 . . ? C11B C10B H10C 109.4 . . ? N2B C10B H10D 109.4 . . ? C11B C10B H10D 109.4 . . ? H10C C10B H10D 108.0 . . ? C12B C11B C16B 120.0 . . ? C12B C11B C10B 119.0(3) . . ? C16B C11B C10B 121.0(3) . . ? C11B C12B C13B 120.0 . . ? C11B C12B H12B 120.0 . . ? C13B C12B H12B 120.0 . . ? C12B C13B C14B 120.0 . . ? C12B C13B H13B 120.0 . . ? C14B C13B H13B 120.0 . . ? C15B C14B C13B 120.0 . . ? C15B C14B H14B 120.0 . . ? C13B C14B H14B 120.0 . . ? C16B C15B C14B 120.0 . . ? C16B C15B H15B 120.0 . . ? C14B C15B H15B 120.0 . . ? C15B C16B C11B 120.0 . . ? C15B C16B Te2A 119.64(18) . . ? C11B C16B Te2A 120.21(18) . . ? C15B C16B Te2B 111.38(18) . . ? C11B C16B Te2B 128.62(18) . . ? Te2A C16B Te2B 9.07(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 C16A Te2B Pd N1A 72.1(6) . . . . ? C16B Te2B Pd N1A 164.7(5) . . . . ? C16A Te2B Pd N2A 31.8(2) . . . . ? C16B Te2B Pd N2A 124.3(2) . . . . ? C16A Te2B Pd Te1 -132.45(16) . . . . ? C16B Te2B Pd Te1 -39.89(12) . . . . ? C16A Te2B Pd Te2A -131.1(4) . . . . ? C16B Te2B Pd Te2A -38.6(3) . . . . ? C1B Te1 Pd N1A 45.69(19) . . . . ? C1A Te1 Pd N1A -48.40(17) . . . . ? C1B Te1 Pd N2A 128.1(6) . . . . ? C1A Te1 Pd N2A 34.0(6) . . . . ? C1B Te1 Pd Te2B -127.32(13) . . . . ? C1A Te1 Pd Te2B 138.58(11) . . . . ? C1B Te1 Pd Te2A -127.59(11) . . . . ? C1A Te1 Pd Te2A 138.32(9) . . . . ? C16B Te2A Pd N1A -169.8(11) . . . . ? C16A Te2A Pd N1A 94.6(11) . . . . ? C16B Te2A Pd N2A 114.85(19) . . . . ? C16A Te2A Pd N2A 19.27(19) . . . . ? C16B Te2A Pd Te2B 131.9(3) . . . . ? C16A Te2A Pd Te2B 36.3(3) . . . . ? C16B Te2A Pd Te1 -49.44(12) . . . . ? C16A Te2A Pd Te1 -145.01(11) . . . . ? N2A Pd N1A C7A -148.9(5) . . . . ? Te2B Pd N1A C7A 170.8(4) . . . . ? Te1 Pd N1A C7A 14.9(5) . . . . ? Te2A Pd N1A C7A 135.1(9) . . . . ? N2A Pd N1A C8A -15.9(4) . . . . ? Te2B Pd N1A C8A -56.2(7) . . . . ? Te1 Pd N1A C8A 147.9(4) . . . . ? Te2A Pd N1A C8A -91.9(12) . . . . ? N1A Pd N2A C9A -14.5(4) . . . . ? Te2B Pd N2A C9A 154.5(4) . . . . ? Te1 Pd N2A C9A -98.3(6) . . . . ? Te2A Pd N2A C9A 157.9(4) . . . . ? N1A Pd N2A C10A -144.3(5) . . . . ? Te2B Pd N2A C10A 24.8(4) . . . . ? Te1 Pd N2A C10A 131.9(5) . . . . ? Te2A Pd N2A C10A 28.2(5) . . . . ? C1B Te1 C1A C2A 118.55(19) . . . . ? Pd Te1 C1A C2A -126.42(18) . . . . ? C1B Te1 C1A C6A -63.0(2) . . . . ? Pd Te1 C1A C6A 52.06(18) . . . . ? C6A C1A C2A C3A 0.0 . . . . ? Te1 C1A C2A C3A 178.5(2) . . . . ? C1A C2A C3A C4A 0.0 . . . . ? C2A C3A C4A C5A 0.0 . . . . ? C3A C4A C5A C6A 0.0 . . . . ? C4A C5A C6A C1A 0.0 . . . . ? C4A C5A C6A C7A 179.1(4) . . . . ? C2A C1A C6A C5A 0.0 . . . . ? Te1 C1A C6A C5A -178.4(2) . . . . ? C2A C1A C6A C7A -179.0(4) . . . . ? Te1 C1A C6A C7A 2.5(4) . . . . ? C8A N1A C7A C6A -83.2(6) . . . . ? Pd N1A C7A C6A 46.3(7) . . . . ? C5A C6A C7A N1A 115.3(4) . . . . ? C1A C6A C7A N1A -65.6(6) . . . . ? C7A N1A C8A C9A -178.7(5) . . . . ? Pd N1A C8A C9A 43.2(5) . . . . ? C10A N2A C9A C8A 177.3(6) . . . . ? Pd N2A C9A C8A 42.9(6) . . . . ? N1A C8A C9A N2A -59.9(7) . . . . ? C9A N2A C10A C11A 154.8(6) . . . . ? Pd N2A C10A C11A -78.5(7) . . . . ? N2A C10A C11A C12A -117.8(5) . . . . ? N2A C10A C11A C16A 62.3(7) . . . . ? C16A C11A C12A C13A 0.0 . . . . ? C10A C11A C12A C13A -179.9(4) . . . . ? C11A C12A C13A C14A 0.0 . . . . ? C12A C13A C14A C15A 0.0 . . . . ? C13A C14A C15A C16A 0.0 . . . . ? C14A C15A C16A C11A 0.0 . . . . ? C14A C15A C16A Te2B 173.5(3) . . . . ? C14A C15A C16A Te2A 176.8(3) . . . . ? C12A C11A C16A C15A 0.0 . . . . ? C10A C11A C16A C15A 179.9(4) . . . . ? C12A C11A C16A Te2B -174.5(3) . . . . ? C10A C11A C16A Te2B 5.4(5) . . . . ? C12A C11A C16A Te2A -176.6(3) . . . . ? C10A C11A C16A Te2A 3.3(5) . . . . ? Pd Te2B C16A C15A 135.1(2) . . . . ? C16B Te2B C16A C15A 41.2(3) . . . . ? Pd Te2B C16A C11A -51.0(3) . . . . ? C16B Te2B C16A C11A -144.9(2) . . . . ? Pd Te2B C16A Te2A 120.7(5) . . . . ? C16B Te2B C16A Te2A 26.7(4) . . . . ? C16B Te2A C16A C15A 44.88(19) . . . . ? Pd Te2A C16A C15A 144.49(16) . . . . ? C16B Te2A C16A C11A -138.4(3) . . . . ? Pd Te2A C16A C11A -38.8(3) . . . . ? C16B Te2A C16A Te2B -147.8(4) . . . . ? Pd Te2A C16A Te2B -48.2(4) . . . . ? C1A Te1 C1B C2B -30.3(2) . . . . ? Pd Te1 C1B C2B -120.88(19) . . . . ? C1A Te1 C1B C6B 155.0(2) . . . . ? Pd Te1 C1B C6B 64.5(2) . . . . ? C6B C1B C2B C3B 0.0 . . . . ? Te1 C1B C2B C3B -174.69(19) . . . . ? C1B C2B C3B C4B 0.0 . . . . ? C2B C3B C4B C5B 0.0 . . . . ? C3B C4B C5B C6B 0.0 . . . . ? C4B C5B C6B C1B 0.0 . . . . ? C4B C5B C6B C7B 178.0(4) . . . . ? C2B C1B C6B C5B 0.0 . . . . ? Te1 C1B C6B C5B 174.64(19) . . . . ? C2B C1B C6B C7B -178.0(4) . . . . ? Te1 C1B C6B C7B -3.4(5) . . . . ? C8B N1B C7B C6B 79.9(7) . . . . ? C5B C6B C7B N1B -141.8(4) . . . . ? C1B C6B C7B N1B 36.2(6) . . . . ? C7B N1B C8B C9B -175.3(6) . . . . ? C10B N2B C9B C8B 171.2(6) . . . . ? N1B C8B C9B N2B -48.8(8) . . . . ? C9B N2B C10B C11B -73.9(7) . . . . ? N2B C10B C11B C12B 125.1(5) . . . . ? N2B C10B C11B C16B -56.7(7) . . . . ? C16B C11B C12B C13B 0.0 . . . . ? C10B C11B C12B C13B 178.3(4) . . . . ? C11B C12B C13B C14B 0.0 . . . . ? C12B C13B C14B C15B 0.0 . . . . ? C13B C14B C15B C16B 0.0 . . . . ? C14B C15B C16B C11B 0.0 . . . . ? C14B C15B C16B Te2A 175.6(3) . . . . ? C14B C15B C16B Te2B 179.7(2) . . . . ? C12B C11B C16B C15B 0.0 . . . . ? C10B C11B C16B C15B -178.2(5) . . . . ? C12B C11B C16B Te2A -175.5(3) . . . . ? C10B C11B C16B Te2A 6.2(5) . . . . ? C12B C11B C16B Te2B -179.6(3) . . . . ? C10B C11B C16B Te2B 2.1(5) . . . . ? C16A Te2A C16B C15B 57.0(2) . . . . ? Pd Te2A C16B C15B -42.68(18) . . . . ? C16A Te2A C16B C11B -127.4(2) . . . . ? Pd Te2A C16B C11B 132.87(19) . . . . ? C16A Te2A C16B Te2B 31.8(5) . . . . ? Pd Te2A C16B Te2B -67.9(4) . . . . ? C16A Te2B C16B C15B 61.4(2) . . . . ? Pd Te2B C16B C15B -53.36(17) . . . . ? C16A Te2B C16B C11B -118.9(3) . . . . ? Pd Te2B C16B C11B 126.3(2) . . . . ? C16A Te2B C16B Te2A -142.1(5) . . . . ? Pd Te2B C16B Te2A 103.2(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W1 Cl2 0.85 2.226(4) 3.031(4) 158.1(5) . O1W H1W2 O6W 0.85 2.3621(16) 3.1042(16) 146.13(16) . O2W H2W1 O5W 0.85 2.2671(16) 3.1160(17) 176.58(14) . O2W H2W2 O2W 0.85 2.654(2) 3.077(2) 112.17(14) 2_556 O3W H3W1 O2W 0.85 2.1395(16) 2.7694(18) 130.66(13) 1_665 O3W H3W1 O6W 0.85 2.184(2) 2.629(2) 112.48(12) 2_666 O3W H3W2 O7WA 0.85 1.43(3) 2.22(2) 152.3(11) . O4W H4W1 Cl1 0.85 2.338(4) 2.865(4) 120.5(2) . O4W H4W2 O3W 0.85 1.900(2) 2.6313(17) 143.4(3) . O5W H5W1 O7WB 0.85 2.251(17) 3.027(17) 151.7(4) 1_445 O5W H5W2 Cl1 0.85 2.221(4) 3.021(4) 156.8(3) 1_545 O6W H6W1 Cl1 0.85 2.314(4) 2.981(4) 135.7(2) 1_545 O6W H6W2 O4W 0.85 2.301(2) 3.0467(18) 146.62(13) 1_545 N1A H1AA Cl2 0.90 2.27 3.133(6) 161.6 2_666 N2A H2AB Cl1 0.90 2.36 3.179(8) 150.7 . N1B H1B O1W 0.90 2.37 3.140(7) 143.7 . N2B H2B O2W 0.90 2.49 3.286(7) 147.1 . _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 4.122 _refine_diff_density_min -2.942 _refine_diff_density_rms 0.277 ###END