Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'R. Puddephatt' 'Michael C. Jennings' 'Chang-Qiu Zhao.' _publ_contact_author_name 'R. Puddephatt' _publ_contact_author_address ; Department of Chemistry The University of Western Ontario LONDON ONTARIO N6A 5B7 CANADA ; _publ_contact_author_email PUDD@UWO.CA _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A Hemilabile Binucleating Pincer Ligand for Self-Assembly of Coordination Oligomers and Polymers ; data_03025 _database_code_depnum_ccdc_archive 'CCDC 664675' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C124 H120 Cl6 N4 P8 Pd4, 2(C2 H4 Cl2), 2(C H2 Cl2), 6(C H Cl3)' _chemical_formula_sum 'C136 H138 Cl34 N4 P8 Pd4' _chemical_formula_weight 3707.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9810(2) _cell_length_b 12.3410(2) _cell_length_c 41.0338(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.2640(10) _cell_angle_gamma 90.00 _cell_volume 7987.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16991 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3728 _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7262 _exptl_absorpt_correction_T_max 0.8042 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58815 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13870 _reflns_number_gt 10181 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.1343P)^2^+40.3441P] 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 13870 _refine_ls_number_parameters 769 _refine_ls_number_restraints 252 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.2418 _refine_ls_wR_factor_gt 0.2240 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.35299(4) 0.49308(5) 0.672084(16) 0.0535(2) Uani 1 1 d U . . Cl1 Cl 0.48648(15) 0.4283(2) 0.69122(6) 0.0709(7) Uani 1 1 d U . . P1 P 0.29808(16) 0.4358(2) 0.71743(6) 0.0596(6) Uani 1 1 d U . . C11 C 0.1853(6) 0.4539(8) 0.7020(2) 0.059(2) Uani 1 1 d U . . H11A H 0.1629 0.3909 0.6884 0.071 Uiso 1 1 calc R . . H11B H 0.1533 0.4609 0.7206 0.071 Uiso 1 1 calc R . . C12 C 0.1765(6) 0.5555(8) 0.6815(2) 0.059(2) Uani 1 1 d U . . H12A H 0.1966 0.6186 0.6955 0.071 Uiso 1 1 calc R . . H12B H 0.1162 0.5674 0.6721 0.071 Uiso 1 1 calc R . . P2 P 0.39129(15) 0.59140(19) 0.62942(6) 0.0594(6) Uani 1 1 d U . . C21 C 0.2892(5) 0.6463(7) 0.6105(2) 0.0556(19) Uani 1 1 d U . . H21A H 0.2967 0.7185 0.6009 0.067 Uiso 1 1 calc R . . H21B H 0.2619 0.5977 0.5928 0.067 Uiso 1 1 calc R . . C22 C 0.2351(6) 0.6553(7) 0.6373(2) 0.0557(19) Uani 1 1 d U . . H22A H 0.1777 0.6809 0.6278 0.067 Uiso 1 1 calc R . . H22B H 0.2604 0.7087 0.6541 0.067 Uiso 1 1 calc R . . N1 N 0.2288(4) 0.5443(5) 0.65375(16) 0.0510(14) Uani 1 1 d U . . C2 C 0.1857(5) 0.4667(7) 0.62904(18) 0.0470(17) Uani 1 1 d U . . C3 C 0.2236(5) 0.3689(7) 0.62399(19) 0.0468(17) Uani 1 1 d U . . H3A H 0.2780 0.3527 0.6361 0.056 Uiso 1 1 calc R . . C4 C 0.1840(5) 0.2944(7) 0.60172(18) 0.0456(17) Uani 1 1 d U . . H4A H 0.2112 0.2273 0.5990 0.055 Uiso 1 1 calc R . . C5 C 0.1041(4) 0.3156(6) 0.58289(18) 0.0418(16) Uani 1 1 d U . . C6 C 0.0675(5) 0.4156(6) 0.58868(19) 0.0462(17) Uani 1 1 d U . . H6A H 0.0136 0.4334 0.5765 0.055 Uiso 1 1 calc R . . C7 C 0.1065(5) 0.4883(6) 0.61121(18) 0.0469(17) Uani 1 1 d U . . H7A H 0.0789 0.5544 0.6147 0.056 Uiso 1 1 calc R . . N8 N 0.0658(4) 0.2430(5) 0.56019(16) 0.0455(14) Uani 1 1 d U . . Pd2 Pd -0.21366(3) 0.09128(4) 0.496370(13) 0.03599(17) Uani 1 1 d U . . Cl3 Cl -0.32661(11) 0.18455(16) 0.46770(5) 0.0475(5) Uani 1 1 d U . . Cl4 Cl -0.09995(12) -0.00098(15) 0.52462(5) 0.0475(4) Uani 1 1 d U . . P3 P 0.25814(11) 0.06766(16) 0.53075(4) 0.0369(4) Uani 1 1 d U . . C31 C 0.1803(4) 0.1747(6) 0.53177(18) 0.0390(15) Uani 1 1 d U . . H31A H 0.2097 0.2412 0.5410 0.047 Uiso 1 1 calc R . . H31B H 0.1528 0.1909 0.5089 0.047 Uiso 1 1 calc R . . C32 C 0.1113(4) 0.1445(6) 0.55264(18) 0.0402(16) Uani 1 1 d U . . H32A H 0.0708 0.0926 0.5403 0.048 Uiso 1 1 calc R . . H32B H 0.1378 0.1094 0.5734 0.048 Uiso 1 1 calc R . . P4 P -0.19342(11) 0.22596(15) 0.53605(5) 0.0375(4) Uani 1 1 d U . . C41 C -0.0881(4) 0.2355(6) 0.56069(17) 0.0397(15) Uani 1 1 d U . . H41A H -0.0891 0.2921 0.5777 0.048 Uiso 1 1 calc R . . H41B H -0.0747 0.1657 0.5723 0.048 Uiso 1 1 calc R . . C42 C -0.0174(4) 0.2621(6) 0.54088(17) 0.0403(16) Uani 1 1 d U . . H42A H -0.0242 0.2168 0.5207 0.048 Uiso 1 1 calc R . . H42B H -0.0220 0.3390 0.5340 0.048 Uiso 1 1 calc R . . C1A C 0.3242(4) 0.5360(5) 0.74966(14) 0.065(2) Uani 1 1 d GU . . C1B C 0.4046(4) 0.5820(6) 0.75404(15) 0.072(2) Uani 1 1 d GU . . H1BA H 0.4455 0.5572 0.7413 0.086 Uiso 1 1 calc R . . C1C C 0.4252(4) 0.6644(6) 0.77703(16) 0.080(3) Uani 1 1 d GU . . H1CA H 0.4802 0.6959 0.7800 0.097 Uiso 1 1 calc R . . C1D C 0.3655(5) 0.7007(6) 0.79565(17) 0.106(5) Uani 1 1 d GU . . H1DA H 0.3796 0.7570 0.8114 0.127 Uiso 1 1 calc R . . C1E C 0.2851(5) 0.6546(7) 0.79128(19) 0.128(6) Uani 1 1 d GU . . H1EA H 0.2442 0.6795 0.8040 0.153 Uiso 1 1 calc R . . C1F C 0.2644(4) 0.5723(7) 0.76828(17) 0.110(5) Uani 1 1 d GU . . H1FA H 0.2095 0.5408 0.7653 0.132 Uiso 1 1 calc R . . C1G C 0.3163(5) 0.3011(5) 0.73479(18) 0.070(2) Uani 1 1 d GU . . C1H C 0.3279(6) 0.2162(6) 0.71371(17) 0.107(4) Uani 1 1 d GU . . H1HA H 0.3256 0.2294 0.6908 0.129 Uiso 1 1 calc R . . C1I C 0.3429(6) 0.1121(5) 0.7262(3) 0.144(6) Uani 1 1 d GU . . H1IA H 0.3508 0.0540 0.7118 0.173 Uiso 1 1 calc R . . C1J C 0.3463(6) 0.0928(6) 0.7598(3) 0.118(4) Uani 1 1 d GU . . H1JA H 0.3565 0.0216 0.7683 0.141 Uiso 1 1 calc R . . C1K C 0.3347(7) 0.1777(8) 0.78084(17) 0.153(7) Uani 1 1 d GU . . H1KA H 0.3370 0.1646 0.8038 0.184 Uiso 1 1 calc R . . C1L C 0.3197(7) 0.2819(6) 0.76836(16) 0.156(8) Uani 1 1 d GU . . H1LA H 0.3118 0.3399 0.7828 0.187 Uiso 1 1 calc R . . C2A C 0.4395(4) 0.5290(6) 0.59719(16) 0.067(2) Uani 1 1 d GU . . C2B C 0.5039(5) 0.4539(8) 0.6062(2) 0.177(9) Uani 1 1 d GU . . H2BA H 0.5229 0.4385 0.6289 0.212 Uiso 1 1 calc R . . C2C C 0.5404(6) 0.4012(8) 0.5820(3) 0.192(10) Uani 1 1 d GU . . H2CA H 0.5844 0.3499 0.5882 0.230 Uiso 1 1 calc R . . C2D C 0.5126(7) 0.4237(8) 0.5489(2) 0.132(5) Uani 1 1 d GU . . H2DA H 0.5375 0.3877 0.5323 0.159 Uiso 1 1 calc R . . C2E C 0.4482(6) 0.4989(9) 0.53986(16) 0.128(5) Uani 1 1 d GU . . H2EA H 0.4292 0.5142 0.5172 0.154 Uiso 1 1 calc R . . C2F C 0.4117(5) 0.5515(7) 0.56402(18) 0.100(4) Uani 1 1 d GU . . H2FA H 0.3677 0.6029 0.5579 0.120 Uiso 1 1 calc R . . C2G C 0.4532(4) 0.7098(5) 0.64630(16) 0.069(2) Uani 1 1 d GU . . C2H C 0.5037(5) 0.7630(6) 0.62675(14) 0.100(4) Uani 1 1 d GU . . H2HA H 0.5077 0.7361 0.6054 0.119 Uiso 1 1 calc R . . C2I C 0.5481(5) 0.8556(6) 0.63848(18) 0.098(4) Uani 1 1 d GU . . H2IA H 0.5826 0.8919 0.6251 0.118 Uiso 1 1 calc R . . C2J C 0.5422(5) 0.8949(5) 0.66977(19) 0.086(3) Uani 1 1 d GU . . H2JA H 0.5726 0.9582 0.6778 0.103 Uiso 1 1 calc R . . C2K C 0.4918(5) 0.8417(5) 0.68932(14) 0.081(3) Uani 1 1 d GU . . H2KA H 0.4877 0.8686 0.7107 0.098 Uiso 1 1 calc R . . C2L C 0.4473(4) 0.7491(5) 0.67759(15) 0.069(2) Uani 1 1 d GU . . H2LA H 0.4128 0.7128 0.6909 0.083 Uiso 1 1 calc R . . C3A C 0.3296(3) 0.1201(5) 0.50414(11) 0.0440(16) Uani 1 1 d GU . . C3B C 0.2961(2) 0.1621(5) 0.47335(12) 0.0533(19) Uani 1 1 d GU . . H3BA H 0.2365 0.1683 0.4670 0.064 Uiso 1 1 calc R . . C3C C 0.3500(4) 0.1950(5) 0.45180(11) 0.067(2) Uani 1 1 d GU . . H3CA H 0.3271 0.2236 0.4308 0.081 Uiso 1 1 calc R . . C3D C 0.4373(3) 0.1859(6) 0.46103(15) 0.076(3) Uani 1 1 d GU . . H3DA H 0.4741 0.2083 0.4463 0.091 Uiso 1 1 calc R . . C3E C 0.4707(2) 0.1439(7) 0.49181(16) 0.088(3) Uani 1 1 d GU . . H3EA H 0.5304 0.1377 0.4981 0.106 Uiso 1 1 calc R . . C3F C 0.4169(3) 0.1110(6) 0.51337(12) 0.070(3) Uani 1 1 d GU . . H3FA H 0.4397 0.0823 0.5344 0.084 Uiso 1 1 calc R . . C3G C 0.3168(3) 0.0730(4) 0.57271(10) 0.0435(16) Uani 1 1 d GU . . C3H C 0.3070(4) -0.0096(4) 0.59480(14) 0.065(2) Uani 1 1 d GU . . H3HA H 0.2742 -0.0718 0.5875 0.079 Uiso 1 1 calc R . . C3I C 0.3453(5) -0.0014(5) 0.62762(13) 0.096(4) Uani 1 1 d GU . . H3IA H 0.3386 -0.0579 0.6427 0.116 Uiso 1 1 calc R . . C3J C 0.3933(5) 0.0895(6) 0.63834(10) 0.092(3) Uani 1 1 d GU . . H3JA H 0.4194 0.0952 0.6608 0.111 Uiso 1 1 calc R . . C3K C 0.4030(4) 0.1722(5) 0.61624(15) 0.073(2) Uani 1 1 d GU . . H3KA H 0.4358 0.2343 0.6236 0.088 Uiso 1 1 calc R . . C3L C 0.3648(3) 0.1639(4) 0.58343(13) 0.056(2) Uani 1 1 d GU . . H3LA H 0.3714 0.2204 0.5683 0.067 Uiso 1 1 calc R . . C4A C -0.2180(3) 0.3637(3) 0.52237(13) 0.0426(16) Uani 1 1 d GU . . C4B C -0.2680(4) 0.4311(4) 0.53842(13) 0.067(3) Uani 1 1 d GU . . H4BA H -0.2903 0.4052 0.5571 0.081 Uiso 1 1 calc R . . C4C C -0.2852(4) 0.5363(4) 0.52721(17) 0.086(4) Uani 1 1 d GU . . H4CA H -0.3193 0.5823 0.5382 0.103 Uiso 1 1 calc R . . C4D C -0.2524(4) 0.5741(3) 0.49994(17) 0.079(3) Uani 1 1 d GU . . H4DA H -0.2642 0.6460 0.4923 0.095 Uiso 1 1 calc R . . C4E C -0.2024(4) 0.5067(4) 0.48389(13) 0.064(2) Uani 1 1 d GU . . H4EA H -0.1801 0.5326 0.4653 0.076 Uiso 1 1 calc R . . C4F C -0.1852(3) 0.4015(4) 0.49511(13) 0.0506(18) Uani 1 1 d GU . . H4FA H -0.1511 0.3555 0.4841 0.061 Uiso 1 1 calc R . . C4G C -0.2616(3) 0.1934(4) 0.56651(10) 0.0398(15) Uani 1 1 d GU . . C4H C -0.2459(3) 0.2380(4) 0.59802(12) 0.057(2) Uani 1 1 d GU . . H4HA H -0.2003 0.2874 0.6037 0.068 Uiso 1 1 calc R . . C4I C -0.2969(4) 0.2102(5) 0.62115(9) 0.062(2) Uani 1 1 d GU . . H4IA H -0.2862 0.2407 0.6427 0.074 Uiso 1 1 calc R . . C4J C -0.3636(3) 0.1380(5) 0.61279(11) 0.055(2) Uani 1 1 d GU . . H4JA H -0.3985 0.1190 0.6286 0.066 Uiso 1 1 calc R . . C4K C -0.3793(3) 0.0934(4) 0.58128(13) 0.055(2) Uani 1 1 d GU . . H4KA H -0.4249 0.0440 0.5756 0.066 Uiso 1 1 calc R . . C4L C -0.3283(3) 0.1212(4) 0.55814(9) 0.0479(18) Uani 1 1 d GU . . H4LA H -0.3391 0.0907 0.5366 0.058 Uiso 1 1 calc R . . Cl99 Cl 0.00720(17) 0.7247(2) 0.65494(6) 0.0765(7) Uani 1 1 d . . . Cl51 Cl 0.2364(6) 0.8535(4) 0.71104(17) 0.202(3) Uani 1 1 d DU . . C52A C 0.146(2) 0.934(5) 0.700(2) 0.34(4) Uani 0.60 1 d PDU A 1 H52A H 0.0963 0.8853 0.6981 0.403 Uiso 0.60 1 calc PR A 1 H52B H 0.1429 0.9840 0.7184 0.403 Uiso 0.60 1 calc PR A 1 C53A C 0.136(4) 1.002(5) 0.668(2) 0.58(10) Uani 0.60 1 d PDU A 1 H53A H 0.1264 0.9485 0.6501 0.696 Uiso 0.60 1 calc PR A 1 H53B H 0.1921 1.0337 0.6679 0.696 Uiso 0.60 1 calc PR A 1 Cl54 Cl 0.065(5) 1.104(5) 0.6564(18) 0.92(8) Uani 0.60 1 d PDU A 1 C52B C 0.157(3) 0.934(6) 0.6892(9) 0.23(3) Uani 0.40 1 d PDU A 2 H52C H 0.1018 0.8991 0.6901 0.281 Uiso 0.40 1 calc PR A 2 H52D H 0.1572 1.0047 0.7007 0.281 Uiso 0.40 1 calc PR A 2 C53B C 0.164(3) 0.956(3) 0.6528(9) 0.127(8) Uani 0.40 1 d PDU A 2 H53C H 0.1330 0.9013 0.6378 0.152 Uiso 0.40 1 calc PR A 2 H53D H 0.2230 0.9618 0.6490 0.152 Uiso 0.40 1 calc PR A 2 Cl55 Cl 0.113(3) 1.078(3) 0.6498(15) 0.50(4) Uani 0.40 1 d PDU A 2 C61 C -0.0006(6) -0.2194(9) 0.5709(2) 0.086(3) Uani 1 1 d DU . . H61A H -0.0336 -0.1519 0.5656 0.103 Uiso 1 1 calc R . . H61B H -0.0009 -0.2375 0.5943 0.103 Uiso 1 1 calc R . . Cl62 Cl -0.0485(2) -0.3293(3) 0.54460(10) 0.1188(13) Uani 1 1 d DU . . Cl63 Cl 0.10603(19) -0.2000(3) 0.56387(7) 0.0907(9) Uani 1 1 d DU . . C71 C -0.1309(10) 0.5124(14) 0.6518(3) 0.174(5) Uani 1 1 d DU . . H71A H -0.0984 0.5766 0.6619 0.209 Uiso 1 1 calc R . . Cl72 Cl -0.2163(6) 0.4806(7) 0.6727(2) 0.255(4) Uani 1 1 d DU . . Cl73 Cl -0.1621(5) 0.5289(5) 0.60871(15) 0.209(3) Uani 1 1 d DU . . Cl74 Cl -0.0678(5) 0.3953(5) 0.65543(13) 0.178(2) Uani 1 1 d DU . . C81 C -0.0110(9) 0.6992(11) 0.7349(3) 0.139(4) Uani 1 1 d DU . . H81A H 0.0030 0.7207 0.7129 0.167 Uiso 1 1 calc R . . Cl82 Cl 0.0555(6) 0.7621(7) 0.76518(18) 0.250(4) Uani 1 1 d DU . . Cl83 Cl 0.0009(4) 0.5580(4) 0.74021(12) 0.1517(17) Uani 1 1 d DU . . Cl84 Cl -0.1135(5) 0.7365(7) 0.7375(2) 0.234(3) Uani 1 1 d DU . . C91 C -0.1413(8) 0.9132(13) 0.6445(3) 0.181(5) Uani 1 1 d DU . . H91A H -0.0943 0.8590 0.6490 0.217 Uiso 1 1 calc R . . Cl92 Cl -0.1584(3) 0.9479(3) 0.60371(7) 0.1109(12) Uani 1 1 d DU . . Cl93 Cl -0.1202(7) 1.0229(11) 0.67032(16) 0.391(7) Uani 1 1 d DU . . Cl94 Cl -0.2351(5) 0.8561(14) 0.6508(3) 0.422(8) Uani 1 1 d DU . . 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 0.0543(4) 0.0503(4) 0.0508(4) 0.0029(3) -0.0072(3) 0.0034(3) Cl1 0.0575(13) 0.0691(15) 0.0779(16) 0.0095(12) -0.0137(11) 0.0091(11) P1 0.0659(14) 0.0629(14) 0.0459(12) 0.0053(10) -0.0031(10) -0.0039(12) C11 0.060(4) 0.070(5) 0.048(5) -0.004(4) 0.007(3) -0.003(4) C12 0.068(5) 0.068(5) 0.038(4) -0.006(4) 0.001(3) 0.013(4) P2 0.0522(13) 0.0513(13) 0.0703(15) 0.0116(11) -0.0030(11) 0.0006(10) C21 0.060(5) 0.043(4) 0.059(5) 0.005(4) -0.003(3) 0.007(4) C22 0.059(5) 0.043(4) 0.060(5) 0.000(4) -0.002(4) 0.010(4) N1 0.057(4) 0.045(3) 0.048(3) -0.002(3) 0.000(3) 0.008(3) C2 0.053(4) 0.048(4) 0.038(4) -0.003(3) 0.001(3) 0.003(3) C3 0.044(4) 0.053(4) 0.043(4) 0.003(3) 0.004(3) 0.009(3) C4 0.039(4) 0.052(4) 0.045(4) -0.004(3) 0.005(3) 0.010(3) C5 0.038(4) 0.048(4) 0.041(4) -0.003(3) 0.008(3) 0.007(3) C6 0.041(4) 0.049(4) 0.047(4) 0.001(3) 0.001(3) 0.012(3) C7 0.052(4) 0.047(4) 0.041(4) 0.001(3) 0.004(3) 0.014(3) N8 0.032(3) 0.053(4) 0.051(4) -0.009(3) 0.004(2) 0.009(3) Pd2 0.0311(3) 0.0396(3) 0.0390(3) 0.0044(2) 0.0110(2) 0.0025(2) Cl3 0.0363(9) 0.0539(11) 0.0528(11) 0.0114(9) 0.0088(8) 0.0082(8) Cl4 0.0417(10) 0.0445(10) 0.0535(11) -0.0006(8) -0.0003(8) 0.0085(8) P3 0.0303(9) 0.0434(10) 0.0388(10) 0.0018(8) 0.0105(7) 0.0012(8) C31 0.034(3) 0.042(4) 0.041(4) -0.006(3) 0.008(3) -0.001(3) C32 0.037(4) 0.042(4) 0.044(4) -0.002(3) 0.014(3) 0.003(3) P4 0.0338(9) 0.0393(10) 0.0421(10) 0.0046(8) 0.0143(8) 0.0024(8) C41 0.038(3) 0.044(4) 0.038(4) -0.002(3) 0.010(3) 0.002(3) C42 0.035(3) 0.050(4) 0.037(4) -0.005(3) 0.008(3) 0.001(3) C1A 0.080(6) 0.075(5) 0.038(4) 0.008(4) 0.002(4) -0.025(5) C1B 0.085(6) 0.081(7) 0.047(5) 0.002(4) 0.003(4) -0.015(5) C1C 0.096(7) 0.087(7) 0.058(6) -0.007(5) 0.012(5) -0.033(6) C1D 0.131(9) 0.139(11) 0.054(6) -0.036(6) 0.035(6) -0.071(8) C1E 0.138(10) 0.175(14) 0.084(8) -0.064(9) 0.062(8) -0.090(11) C1F 0.127(9) 0.156(12) 0.057(6) -0.044(7) 0.047(6) -0.086(9) C1G 0.052(5) 0.069(5) 0.083(6) 0.017(4) -0.002(5) -0.015(4) C1H 0.144(12) 0.069(6) 0.129(9) 0.027(5) 0.085(9) 0.012(7) C1I 0.173(16) 0.076(7) 0.213(13) 0.049(8) 0.121(14) 0.022(9) C1J 0.062(7) 0.093(7) 0.192(12) 0.073(7) 0.001(8) -0.006(6) C1K 0.212(19) 0.098(8) 0.117(9) 0.050(6) -0.074(10) -0.056(11) C1L 0.29(2) 0.081(7) 0.068(6) 0.022(5) -0.048(10) -0.049(11) C2A 0.058(5) 0.057(5) 0.089(5) 0.028(4) 0.024(4) 0.005(4) C2B 0.153(13) 0.228(17) 0.187(11) 0.157(12) 0.141(11) 0.145(13) C2C 0.207(18) 0.172(16) 0.240(14) 0.137(15) 0.169(15) 0.131(15) C2D 0.121(11) 0.094(10) 0.211(12) 0.018(10) 0.113(11) 0.010(7) C2E 0.105(10) 0.172(16) 0.117(8) -0.013(9) 0.046(8) 0.019(9) C2F 0.073(7) 0.136(11) 0.087(6) -0.017(7) 0.006(6) 0.024(7) C2G 0.063(5) 0.066(5) 0.075(6) 0.012(4) 0.003(4) -0.007(4) C2H 0.107(9) 0.122(10) 0.072(7) 0.002(6) 0.022(6) -0.046(7) C2I 0.123(10) 0.081(8) 0.092(7) 0.014(6) 0.022(7) -0.034(7) C2J 0.079(7) 0.066(7) 0.108(7) 0.010(5) 0.002(6) -0.013(5) C2K 0.087(7) 0.070(6) 0.084(7) 0.003(5) 0.004(5) 0.000(5) C2L 0.069(6) 0.067(6) 0.071(5) 0.007(4) 0.010(5) -0.007(5) C3A 0.043(4) 0.045(4) 0.049(4) -0.003(3) 0.020(3) -0.003(3) C3B 0.049(4) 0.057(5) 0.058(5) 0.008(4) 0.023(3) -0.001(4) C3C 0.084(5) 0.063(6) 0.064(5) 0.008(5) 0.037(4) 0.000(5) C3D 0.066(5) 0.082(7) 0.092(6) -0.007(5) 0.048(5) -0.021(5) C3E 0.050(5) 0.133(10) 0.091(7) 0.003(7) 0.038(4) -0.011(6) C3F 0.040(4) 0.105(8) 0.069(6) 0.006(5) 0.021(4) 0.004(5) C3G 0.033(4) 0.057(4) 0.043(3) -0.004(3) 0.010(3) 0.005(3) C3H 0.078(6) 0.067(5) 0.049(4) 0.002(4) 0.003(4) 0.012(5) C3I 0.127(10) 0.106(8) 0.049(5) 0.013(5) -0.007(6) 0.011(7) C3J 0.094(8) 0.125(9) 0.050(5) -0.014(5) -0.016(5) 0.028(6) C3K 0.043(5) 0.098(7) 0.073(6) -0.031(5) -0.004(4) 0.008(5) C3L 0.037(4) 0.073(5) 0.060(4) -0.014(4) 0.010(3) -0.001(4) C4A 0.040(4) 0.039(3) 0.051(4) 0.008(3) 0.013(3) 0.000(3) C4B 0.078(6) 0.045(4) 0.090(7) 0.016(4) 0.049(5) 0.010(4) C4C 0.103(8) 0.050(5) 0.119(9) 0.020(6) 0.065(7) 0.020(5) C4D 0.083(7) 0.045(5) 0.117(9) 0.029(5) 0.040(6) 0.008(5) C4E 0.067(6) 0.053(5) 0.078(6) 0.023(4) 0.030(5) -0.005(4) C4F 0.044(4) 0.052(4) 0.058(5) 0.008(4) 0.016(4) 0.001(4) C4G 0.039(3) 0.039(4) 0.046(4) 0.008(3) 0.019(3) 0.006(3) C4H 0.062(5) 0.064(5) 0.050(4) -0.003(4) 0.026(4) -0.015(4) C4I 0.075(6) 0.073(6) 0.044(4) -0.004(4) 0.029(4) -0.008(4) C4J 0.055(5) 0.057(5) 0.062(5) 0.015(4) 0.035(4) 0.005(4) C4K 0.040(4) 0.068(6) 0.061(5) 0.005(4) 0.023(4) -0.006(4) C4L 0.040(4) 0.061(5) 0.046(4) -0.002(4) 0.017(3) -0.002(3) Cl99 0.0824(17) 0.0841(18) 0.0645(14) 0.0074(13) 0.0165(12) 0.0308(14) Cl51 0.321(9) 0.102(3) 0.191(5) -0.051(4) 0.060(6) -0.014(4) C52A 0.10(2) 0.39(8) 0.50(11) 0.06(8) -0.01(5) -0.11(2) C53A 0.35(9) 0.36(8) 0.90(19) 0.37(12) -0.28(10) -0.25(5) Cl54 1.31(16) 0.73(8) 0.93(11) 0.62(9) 0.84(12) 0.58(10) C52B 0.26(6) 0.32(7) 0.09(2) 0.03(4) -0.07(3) -0.12(4) C53B 0.15(3) 0.12(2) 0.136(15) -0.070(15) 0.101(18) -0.071(16) Cl55 0.62(6) 0.33(3) 0.70(7) 0.37(5) 0.58(6) 0.24(4) C61 0.080(6) 0.119(8) 0.064(6) 0.032(5) 0.028(5) 0.057(5) Cl62 0.095(2) 0.123(3) 0.130(3) 0.062(2) -0.005(2) -0.017(2) Cl63 0.0870(19) 0.116(2) 0.0758(17) 0.0022(16) 0.0335(15) -0.0087(17) C71 0.24(2) 0.159(14) 0.135(9) -0.049(11) 0.077(12) -0.079(9) Cl72 0.285(9) 0.252(8) 0.268(8) -0.105(7) 0.168(8) -0.081(7) Cl73 0.312(9) 0.166(5) 0.143(4) -0.022(4) 0.020(5) -0.084(5) Cl74 0.238(6) 0.182(5) 0.124(3) -0.027(3) 0.054(4) -0.073(4) C81 0.209(11) 0.130(8) 0.088(9) -0.029(8) 0.055(9) 0.023(11) Cl82 0.320(9) 0.233(7) 0.173(6) 0.009(5) -0.029(6) -0.085(7) Cl83 0.189(5) 0.138(3) 0.139(4) -0.006(3) 0.060(3) 0.032(3) Cl84 0.239(6) 0.214(7) 0.252(8) -0.037(6) 0.051(6) 0.098(6) C91 0.156(10) 0.320(17) 0.081(7) 0.065(9) 0.061(8) 0.159(9) Cl92 0.146(3) 0.116(3) 0.0699(17) 0.0157(17) 0.0131(18) 0.060(2) Cl93 0.384(10) 0.612(16) 0.142(5) -0.168(8) -0.065(6) 0.367(10) Cl94 0.174(6) 0.80(2) 0.325(10) 0.370(12) 0.145(6) 0.145(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.103(7) . ? Pd1 P2 2.293(3) . ? Pd1 P1 2.293(3) . ? Pd1 Cl1 2.295(2) . ? P1 C1A 1.810(5) . ? P1 C1G 1.813(6) . ? P1 C11 1.826(9) . ? C11 C12 1.503(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N1 1.523(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? P2 C2A 1.807(6) . ? P2 C21 1.821(8) . ? P2 C2G 1.837(5) . ? C21 C22 1.509(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N1 1.536(11) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N1 C2 1.481(10) . ? C2 C3 1.381(11) . ? C2 C7 1.382(11) . ? C3 C4 1.376(11) . ? C3 H3A 0.9500 . ? C4 C5 1.407(10) . ? C4 H4A 0.9500 . ? C5 N8 1.365(10) . ? C5 C6 1.402(10) . ? C6 C7 1.364(11) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? N8 C42 1.454(9) . ? N8 C32 1.474(9) . ? Pd2 Cl4 2.2945(18) . ? Pd2 Cl3 2.2985(18) . ? Pd2 P3 2.310(2) 3_556 ? Pd2 P4 2.313(2) . ? P3 C31 1.819(7) . ? P3 C3A 1.821(4) . ? P3 C3G 1.824(4) . ? P3 Pd2 2.310(2) 3_556 ? C31 C32 1.547(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? P4 C4A 1.813(4) . ? P4 C41 1.822(7) . ? P4 C4G 1.830(3) . ? C41 C42 1.530(9) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C1A C1B 1.3900 . ? C1A C1F 1.3900 . ? C1B C1C 1.3900 . ? C1B H1BA 0.9500 . ? C1C C1D 1.3900 . ? C1C H1CA 0.9500 . ? C1D C1E 1.3900 . ? C1D H1DA 0.9500 . ? C1E C1F 1.3900 . ? C1E H1EA 0.9500 . ? C1F H1FA 0.9500 . ? C1G C1H 1.3900 . ? C1G C1L 1.3900 . ? C1H C1I 1.3900 . ? C1H H1HA 0.9500 . ? C1I C1J 1.3900 . ? C1I H1IA 0.9500 . ? C1J C1K 1.3900 . ? C1J H1JA 0.9500 . ? C1K C1L 1.3900 . ? C1K H1KA 0.9500 . ? C1L H1LA 0.9500 . ? C2A C2B 1.3900 . ? C2A C2F 1.3900 . ? C2B C2C 1.3900 . ? C2B H2BA 0.9500 . ? C2C C2D 1.3900 . ? C2C H2CA 0.9500 . ? C2D C2E 1.3900 . ? C2D H2DA 0.9500 . ? C2E C2F 1.3900 . ? C2E H2EA 0.9500 . ? C2F H2FA 0.9500 . ? C2G C2H 1.3900 . ? C2G C2L 1.3900 . ? C2H C2I 1.3900 . ? C2H H2HA 0.9500 . ? C2I C2J 1.3900 . ? C2I H2IA 0.9500 . ? C2J C2K 1.3900 . ? C2J H2JA 0.9500 . ? C2K C2L 1.3900 . ? C2K H2KA 0.9500 . ? C2L H2LA 0.9500 . ? C3A C3B 1.3900 . ? C3A C3F 1.3900 . ? C3B C3C 1.3900 . ? C3B H3BA 0.9500 . ? C3C C3D 1.3900 . ? C3C H3CA 0.9500 . ? C3D C3E 1.3900 . ? C3D H3DA 0.9500 . ? C3E C3F 1.3900 . ? C3E H3EA 0.9500 . ? C3F H3FA 0.9500 . ? C3G C3H 1.3900 . ? C3G C3L 1.3900 . ? C3H C3I 1.3900 . ? C3H H3HA 0.9500 . ? C3I C3J 1.3900 . ? C3I H3IA 0.9500 . ? C3J C3K 1.3900 . ? C3J H3JA 0.9500 . ? C3K C3L 1.3900 . ? C3K H3KA 0.9500 . ? C3L H3LA 0.9500 . ? C4A C4B 1.3900 . ? C4A C4F 1.3900 . ? C4B C4C 1.3900 . ? C4B H4BA 0.9500 . ? C4C C4D 1.3900 . ? C4C H4CA 0.9500 . ? C4D C4E 1.3900 . ? C4D H4DA 0.9500 . ? C4E C4F 1.3900 . ? C4E H4EA 0.9500 . ? C4F H4FA 0.9500 . ? C4G C4H 1.3900 . ? C4G C4L 1.3900 . ? C4H C4I 1.3900 . ? C4H H4HA 0.9500 . ? C4I C4J 1.3900 . ? C4I H4IA 0.9500 . ? C4J C4K 1.3900 . ? C4J H4JA 0.9500 . ? C4K C4L 1.3900 . ? C4K H4KA 0.9500 . ? C4L H4LA 0.9500 . ? Cl51 C52B 1.74(2) . ? Cl51 C52A 1.75(2) . ? C52A C53A 1.52(2) . ? C52A H52A 0.9900 . ? C52A H52B 0.9900 . ? C53A Cl54 1.72(2) . ? C53A H53A 0.9900 . ? C53A H53B 0.9900 . ? C52B C53B 1.54(2) . ? C52B H52C 0.9900 . ? C52B H52D 0.9900 . ? C53B Cl55 1.704(19) . ? C53B H53C 0.9900 . ? C53B H53D 0.9900 . ? C61 Cl63 1.789(9) . ? C61 Cl62 1.822(11) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C71 Cl74 1.755(15) . ? C71 Cl72 1.768(14) . ? C71 Cl73 1.771(14) . ? C71 H71A 1.0000 . ? C81 Cl82 1.688(13) . ? C81 Cl84 1.721(14) . ? C81 Cl83 1.763(13) . ? C81 H81A 1.0000 . ? C91 Cl92 1.707(11) . ? C91 Cl94 1.714(14) . ? C91 Cl93 1.718(15) . ? C91 H91A 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 P2 85.4(2) . . ? N1 Pd1 P1 85.4(2) . . ? P2 Pd1 P1 165.21(10) . . ? N1 Pd1 Cl1 177.1(2) . . ? P2 Pd1 Cl1 95.62(9) . . ? P1 Pd1 Cl1 94.07(10) . . ? C1A P1 C1G 109.6(4) . . ? C1A P1 C11 105.6(4) . . ? C1G P1 C11 109.7(4) . . ? C1A P1 Pd1 108.0(2) . . ? C1G P1 Pd1 122.9(3) . . ? C11 P1 Pd1 99.6(3) . . ? C12 C11 P1 107.1(6) . . ? C12 C11 H11A 110.3 . . ? P1 C11 H11A 110.3 . . ? C12 C11 H11B 110.3 . . ? P1 C11 H11B 110.3 . . ? H11A C11 H11B 108.5 . . ? C11 C12 N1 109.2(7) . . ? C11 C12 H12A 109.8 . . ? N1 C12 H12A 109.8 . . ? C11 C12 H12B 109.8 . . ? N1 C12 H12B 109.8 . . ? H12A C12 H12B 108.3 . . ? C2A P2 C21 107.8(4) . . ? C2A P2 C2G 110.3(4) . . ? C21 P2 C2G 104.9(4) . . ? C2A P2 Pd1 122.1(3) . . ? C21 P2 Pd1 101.0(3) . . ? C2G P2 Pd1 109.1(2) . . ? C22 C21 P2 107.3(6) . . ? C22 C21 H21A 110.3 . . ? P2 C21 H21A 110.3 . . ? C22 C21 H21B 110.3 . . ? P2 C21 H21B 110.3 . . ? H21A C21 H21B 108.5 . . ? C21 C22 N1 109.8(7) . . ? C21 C22 H22A 109.7 . . ? N1 C22 H22A 109.7 . . ? C21 C22 H22B 109.7 . . ? N1 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C2 N1 C12 108.7(7) . . ? C2 N1 C22 109.4(6) . . ? C12 N1 C22 109.2(6) . . ? C2 N1 Pd1 111.0(5) . . ? C12 N1 Pd1 111.1(5) . . ? C22 N1 Pd1 107.5(5) . . ? C3 C2 C7 118.4(7) . . ? C3 C2 N1 120.1(7) . . ? C7 C2 N1 121.5(7) . . ? C4 C3 C2 121.2(7) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 121.3(7) . . ? C3 C4 H4A 119.3 . . ? C5 C4 H4A 119.3 . . ? N8 C5 C6 122.7(7) . . ? N8 C5 C4 121.3(7) . . ? C6 C5 C4 115.9(7) . . ? C7 C6 C5 122.4(7) . . ? C7 C6 H6A 118.8 . . ? C5 C6 H6A 118.8 . . ? C6 C7 C2 120.8(7) . . ? C6 C7 H7A 119.6 . . ? C2 C7 H7A 119.6 . . ? C5 N8 C42 122.4(6) . . ? C5 N8 C32 120.2(6) . . ? C42 N8 C32 117.3(6) . . ? Cl4 Pd2 Cl3 179.36(8) . . ? Cl4 Pd2 P3 88.81(7) . 3_556 ? Cl3 Pd2 P3 91.33(7) . 3_556 ? Cl4 Pd2 P4 89.50(7) . . ? Cl3 Pd2 P4 90.56(7) . . ? P3 Pd2 P4 161.21(7) 3_556 . ? C31 P3 C3A 104.6(3) . . ? C31 P3 C3G 101.6(3) . . ? C3A P3 C3G 106.1(2) . . ? C31 P3 Pd2 118.0(2) . 3_556 ? C3A P3 Pd2 100.8(2) . 3_556 ? C3G P3 Pd2 123.85(19) . 3_556 ? C32 C31 P3 112.9(5) . . ? C32 C31 H31A 109.0 . . ? P3 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? P3 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? N8 C32 C31 109.7(6) . . ? N8 C32 H32A 109.7 . . ? C31 C32 H32A 109.7 . . ? N8 C32 H32B 109.7 . . ? C31 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C4A P4 C41 104.2(3) . . ? C4A P4 C4G 107.1(2) . . ? C41 P4 C4G 103.5(3) . . ? C4A P4 Pd2 117.2(2) . . ? C41 P4 Pd2 116.7(2) . . ? C4G P4 Pd2 106.98(17) . . ? C42 C41 P4 114.5(5) . . ? C42 C41 H41A 108.6 . . ? P4 C41 H41A 108.6 . . ? C42 C41 H41B 108.6 . . ? P4 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? N8 C42 C41 111.4(6) . . ? N8 C42 H42A 109.4 . . ? C41 C42 H42A 109.4 . . ? N8 C42 H42B 109.4 . . ? C41 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? C1B C1A C1F 120.0 . . ? C1B C1A P1 118.3(4) . . ? C1F C1A P1 121.6(4) . . ? C1C C1B C1A 120.0 . . ? C1C C1B H1BA 120.0 . . ? C1A C1B H1BA 120.0 . . ? C1B C1C C1D 120.0 . . ? C1B C1C H1CA 120.0 . . ? C1D C1C H1CA 120.0 . . ? C1E C1D C1C 120.0 . . ? C1E C1D H1DA 120.0 . . ? C1C C1D H1DA 120.0 . . ? C1D C1E C1F 120.0 . . ? C1D C1E H1EA 120.0 . . ? C1F C1E H1EA 120.0 . . ? C1E C1F C1A 120.0 . . ? C1E C1F H1FA 120.0 . . ? C1A C1F H1FA 120.0 . . ? C1H C1G C1L 120.0 . . ? C1H C1G P1 118.4(5) . . ? C1L C1G P1 121.6(5) . . ? C1G C1H C1I 120.0 . . ? C1G C1H H1HA 120.0 . . ? C1I C1H H1HA 120.0 . . ? C1J C1I C1H 120.0 . . ? C1J C1I H1IA 120.0 . . ? C1H C1I H1IA 120.0 . . ? C1I C1J C1K 120.0 . . ? C1I C1J H1JA 120.0 . . ? C1K C1J H1JA 120.0 . . ? C1L C1K C1J 120.0 . . ? C1L C1K H1KA 120.0 . . ? C1J C1K H1KA 120.0 . . ? C1K C1L C1G 120.0 . . ? C1K C1L H1LA 120.0 . . ? C1G C1L H1LA 120.0 . . ? C2B C2A C2F 120.0 . . ? C2B C2A P2 118.3(4) . . ? C2F C2A P2 121.6(4) . . ? C2A C2B C2C 120.0 . . ? C2A C2B H2BA 120.0 . . ? C2C C2B H2BA 120.0 . . ? C2D C2C C2B 120.0 . . ? C2D C2C H2CA 120.0 . . ? C2B C2C H2CA 120.0 . . ? C2C C2D C2E 120.0 . . ? C2C C2D H2DA 120.0 . . ? C2E C2D H2DA 120.0 . . ? C2F C2E C2D 120.0 . . ? C2F C2E H2EA 120.0 . . ? C2D C2E H2EA 120.0 . . ? C2E C2F C2A 120.0 . . ? C2E C2F H2FA 120.0 . . ? C2A C2F H2FA 120.0 . . ? C2H C2G C2L 120.0 . . ? C2H C2G P2 119.0(4) . . ? C2L C2G P2 120.9(4) . . ? C2G C2H C2I 120.0 . . ? C2G C2H H2HA 120.0 . . ? C2I C2H H2HA 120.0 . . ? C2H C2I C2J 120.0 . . ? C2H C2I H2IA 120.0 . . ? C2J C2I H2IA 120.0 . . ? C2K C2J C2I 120.0 . . ? C2K C2J H2JA 120.0 . . ? C2I C2J H2JA 120.0 . . ? C2J C2K C2L 120.0 . . ? C2J C2K H2KA 120.0 . . ? C2L C2K H2KA 120.0 . . ? C2K C2L C2G 120.0 . . ? C2K C2L H2LA 120.0 . . ? C2G C2L H2LA 120.0 . . ? C3B C3A C3F 120.0 . . ? C3B C3A P3 119.4(3) . . ? C3F C3A P3 120.4(3) . . ? C3A C3B C3C 120.0 . . ? C3A C3B H3BA 120.0 . . ? C3C C3B H3BA 120.0 . . ? C3D C3C C3B 120.0 . . ? C3D C3C H3CA 120.0 . . ? C3B C3C H3CA 120.0 . . ? C3E C3D C3C 120.0 . . ? C3E C3D H3DA 120.0 . . ? C3C C3D H3DA 120.0 . . ? C3D C3E C3F 120.0 . . ? C3D C3E H3EA 120.0 . . ? C3F C3E H3EA 120.0 . . ? C3E C3F C3A 120.0 . . ? C3E C3F H3FA 120.0 . . ? C3A C3F H3FA 120.0 . . ? C3H C3G C3L 120.0 . . ? C3H C3G P3 119.6(3) . . ? C3L C3G P3 120.1(3) . . ? C3I C3H C3G 120.0 . . ? C3I C3H H3HA 120.0 . . ? C3G C3H H3HA 120.0 . . ? C3H C3I C3J 120.0 . . ? C3H C3I H3IA 120.0 . . ? C3J C3I H3IA 120.0 . . ? C3K C3J C3I 120.0 . . ? C3K C3J H3JA 120.0 . . ? C3I C3J H3JA 120.0 . . ? C3L C3K C3J 120.0 . . ? C3L C3K H3KA 120.0 . . ? C3J C3K H3KA 120.0 . . ? C3K C3L C3G 120.0 . . ? C3K C3L H3LA 120.0 . . ? C3G C3L H3LA 120.0 . . ? C4B C4A C4F 120.0 . . ? C4B C4A P4 121.8(3) . . ? C4F C4A P4 118.2(3) . . ? C4C C4B C4A 120.0 . . ? C4C C4B H4BA 120.0 . . ? C4A C4B H4BA 120.0 . . ? C4B C4C C4D 120.0 . . ? C4B C4C H4CA 120.0 . . ? C4D C4C H4CA 120.0 . . ? C4E C4D C4C 120.0 . . ? C4E C4D H4DA 120.0 . . ? C4C C4D H4DA 120.0 . . ? C4D C4E C4F 120.0 . . ? C4D C4E H4EA 120.0 . . ? C4F C4E H4EA 120.0 . . ? C4E C4F C4A 120.0 . . ? C4E C4F H4FA 120.0 . . ? C4A C4F H4FA 120.0 . . ? C4H C4G C4L 120.0 . . ? C4H C4G P4 120.7(3) . . ? C4L C4G P4 119.3(3) . . ? C4G C4H C4I 120.0 . . ? C4G C4H H4HA 120.0 . . ? C4I C4H H4HA 120.0 . . ? C4H C4I C4J 120.0 . . ? C4H C4I H4IA 120.0 . . ? C4J C4I H4IA 120.0 . . ? C4I C4J C4K 120.0 . . ? C4I C4J H4JA 120.0 . . ? C4K C4J H4JA 120.0 . . ? C4L C4K C4J 120.0 . . ? C4L C4K H4KA 120.0 . . ? C4J C4K H4KA 120.0 . . ? C4K C4L C4G 120.0 . . ? C4K C4L H4LA 120.0 . . ? C4G C4L H4LA 120.0 . . ? C52B Cl51 C52A 16(3) . . ? C53A C52A Cl51 121(4) . . ? C53A C52A H52A 107.2 . . ? Cl51 C52A H52A 107.2 . . ? C53A C52A H52B 107.2 . . ? Cl51 C52A H52B 107.2 . . ? H52A C52A H52B 106.8 . . ? C52A C53A Cl54 129(5) . . ? C52A C53A H53A 105.1 . . ? Cl54 C53A H53A 105.1 . . ? C52A C53A H53B 105.1 . . ? Cl54 C53A H53B 105.1 . . ? H53A C53A H53B 105.9 . . ? C53B C52B Cl51 116(3) . . ? C53B C52B H52C 108.2 . . ? Cl51 C52B H52C 108.2 . . ? C53B C52B H52D 108.2 . . ? Cl51 C52B H52D 108.2 . . ? H52C C52B H52D 107.3 . . ? C52B C53B Cl55 97(3) . . ? C52B C53B H53C 112.4 . . ? Cl55 C53B H53C 112.4 . . ? C52B C53B H53D 112.4 . . ? Cl55 C53B H53D 112.4 . . ? H53C C53B H53D 109.9 . . ? Cl63 C61 Cl62 109.0(5) . . ? Cl63 C61 H61A 109.9 . . ? Cl62 C61 H61A 109.9 . . ? Cl63 C61 H61B 109.9 . . ? Cl62 C61 H61B 109.9 . . ? H61A C61 H61B 108.3 . . ? Cl74 C71 Cl72 104.7(9) . . ? Cl74 C71 Cl73 104.2(9) . . ? Cl72 C71 Cl73 113.3(10) . . ? Cl74 C71 H71A 111.4 . . ? Cl72 C71 H71A 111.4 . . ? Cl73 C71 H71A 111.4 . . ? Cl82 C81 Cl84 108.9(8) . . ? Cl82 C81 Cl83 108.7(9) . . ? Cl84 C81 Cl83 109.9(9) . . ? Cl82 C81 H81A 109.7 . . ? Cl84 C81 H81A 109.7 . . ? Cl83 C81 H81A 109.7 . . ? Cl92 C91 Cl94 104.2(8) . . ? Cl92 C91 Cl93 113.0(9) . . ? Cl94 C91 Cl93 108.6(10) . . ? Cl92 C91 H91A 110.2 . . ? Cl94 C91 H91A 110.2 . . ? Cl93 C91 H91A 110.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 P1 C1A -100.6(3) . . . . ? P2 Pd1 P1 C1A -48.5(5) . . . . ? Cl1 Pd1 P1 C1A 82.3(3) . . . . ? N1 Pd1 P1 C1G 130.4(4) . . . . ? P2 Pd1 P1 C1G -177.6(4) . . . . ? Cl1 Pd1 P1 C1G -46.7(3) . . . . ? N1 Pd1 P1 C11 9.4(4) . . . . ? P2 Pd1 P1 C11 61.4(5) . . . . ? Cl1 Pd1 P1 C11 -167.7(3) . . . . ? C1A P1 C11 C12 74.2(6) . . . . ? C1G P1 C11 C12 -167.8(6) . . . . ? Pd1 P1 C11 C12 -37.6(6) . . . . ? P1 C11 C12 N1 58.0(8) . . . . ? N1 Pd1 P2 C2A -118.1(4) . . . . ? P1 Pd1 P2 C2A -170.2(4) . . . . ? Cl1 Pd1 P2 C2A 59.1(3) . . . . ? N1 Pd1 P2 C21 1.2(4) . . . . ? P1 Pd1 P2 C21 -50.9(5) . . . . ? Cl1 Pd1 P2 C21 178.4(3) . . . . ? N1 Pd1 P2 C2G 111.3(3) . . . . ? P1 Pd1 P2 C2G 59.2(5) . . . . ? Cl1 Pd1 P2 C2G -71.5(3) . . . . ? C2A P2 C21 C22 156.9(6) . . . . ? C2G P2 C21 C22 -85.5(6) . . . . ? Pd1 P2 C21 C22 27.8(6) . . . . ? P2 C21 C22 N1 -56.1(8) . . . . ? C11 C12 N1 C2 72.4(8) . . . . ? C11 C12 N1 C22 -168.3(7) . . . . ? C11 C12 N1 Pd1 -49.9(8) . . . . ? C21 C22 N1 C2 -63.1(8) . . . . ? C21 C22 N1 C12 178.1(7) . . . . ? C21 C22 N1 Pd1 57.5(7) . . . . ? P2 Pd1 N1 C2 90.0(5) . . . . ? P1 Pd1 N1 C2 -101.7(5) . . . . ? Cl1 Pd1 N1 C2 -21(4) . . . . ? P2 Pd1 N1 C12 -149.0(6) . . . . ? P1 Pd1 N1 C12 19.3(5) . . . . ? Cl1 Pd1 N1 C12 100(4) . . . . ? P2 Pd1 N1 C22 -29.6(5) . . . . ? P1 Pd1 N1 C22 138.7(5) . . . . ? Cl1 Pd1 N1 C22 -141(4) . . . . ? C12 N1 C2 C3 -114.3(8) . . . . ? C22 N1 C2 C3 126.5(8) . . . . ? Pd1 N1 C2 C3 8.1(9) . . . . ? C12 N1 C2 C7 63.9(9) . . . . ? C22 N1 C2 C7 -55.3(10) . . . . ? Pd1 N1 C2 C7 -173.7(6) . . . . ? C7 C2 C3 C4 0.2(12) . . . . ? N1 C2 C3 C4 178.5(7) . . . . ? C2 C3 C4 C5 1.0(12) . . . . ? C3 C4 C5 N8 178.3(7) . . . . ? C3 C4 C5 C6 -1.0(11) . . . . ? N8 C5 C6 C7 -179.4(7) . . . . ? C4 C5 C6 C7 -0.1(12) . . . . ? C5 C6 C7 C2 1.3(13) . . . . ? C3 C2 C7 C6 -1.4(12) . . . . ? N1 C2 C7 C6 -179.6(7) . . . . ? C6 C5 N8 C42 -1.9(11) . . . . ? C4 C5 N8 C42 178.8(7) . . . . ? C6 C5 N8 C32 173.4(7) . . . . ? C4 C5 N8 C32 -5.8(11) . . . . ? C3A P3 C31 C32 178.4(5) . . . . ? C3G P3 C31 C32 -71.4(5) . . . . ? Pd2 P3 C31 C32 67.5(6) 3_556 . . . ? C5 N8 C32 C31 -73.5(8) . . . . ? C42 N8 C32 C31 102.1(7) . . . . ? P3 C31 C32 N8 164.1(5) . . . . ? Cl4 Pd2 P4 C4A 146.3(2) . . . . ? Cl3 Pd2 P4 C4A -33.1(2) . . . . ? P3 Pd2 P4 C4A -128.9(3) 3_556 . . . ? Cl4 Pd2 P4 C41 21.7(3) . . . . ? Cl3 Pd2 P4 C41 -157.6(3) . . . . ? P3 Pd2 P4 C41 106.6(3) 3_556 . . . ? Cl4 Pd2 P4 C4G -93.5(2) . . . . ? Cl3 Pd2 P4 C4G 87.1(2) . . . . ? P3 Pd2 P4 C4G -8.7(3) 3_556 . . . ? C4A P4 C41 C42 -68.3(6) . . . . ? C4G P4 C41 C42 179.8(5) . . . . ? Pd2 P4 C41 C42 62.6(6) . . . . ? C5 N8 C42 C41 -80.6(9) . . . . ? C32 N8 C42 C41 103.9(7) . . . . ? P4 C41 C42 N8 -166.2(5) . . . . ? C1G P1 C1A C1B 95.4(5) . . . . ? C11 P1 C1A C1B -146.6(5) . . . . ? Pd1 P1 C1A C1B -40.8(5) . . . . ? C1G P1 C1A C1F -88.9(5) . . . . ? C11 P1 C1A C1F 29.1(5) . . . . ? Pd1 P1 C1A C1F 134.9(4) . . . . ? C1F C1A C1B C1C 0.0 . . . . ? P1 C1A C1B C1C 175.7(5) . . . . ? C1A C1B C1C C1D 0.0 . . . . ? C1B C1C C1D C1E 0.0 . . . . ? C1C C1D C1E C1F 0.0 . . . . ? C1D C1E C1F C1A 0.0 . . . . ? C1B C1A C1F C1E 0.0 . . . . ? P1 C1A C1F C1E -175.6(5) . . . . ? C1A P1 C1G C1H -158.7(5) . . . . ? C11 P1 C1G C1H 85.8(6) . . . . ? Pd1 P1 C1G C1H -30.3(6) . . . . ? C1A P1 C1G C1L 20.6(6) . . . . ? C11 P1 C1G C1L -94.8(6) . . . . ? Pd1 P1 C1G C1L 149.0(4) . . . . ? C1L C1G C1H C1I 0.0 . . . . ? P1 C1G C1H C1I 179.4(5) . . . . ? C1G C1H C1I C1J 0.0 . . . . ? C1H C1I C1J C1K 0.0 . . . . ? C1I C1J C1K C1L 0.0 . . . . ? C1J C1K C1L C1G 0.0 . . . . ? C1H C1G C1L C1K 0.0 . . . . ? P1 C1G C1L C1K -179.3(6) . . . . ? C21 P2 C2A C2B -160.6(6) . . . . ? C2G P2 C2A C2B 85.5(6) . . . . ? Pd1 P2 C2A C2B -44.6(6) . . . . ? C21 P2 C2A C2F 17.0(7) . . . . ? C2G P2 C2A C2F -96.9(6) . . . . ? Pd1 P2 C2A C2F 133.0(5) . . . . ? C2F C2A C2B C2C 0.0 . . . . ? P2 C2A C2B C2C 177.6(6) . . . . ? C2A C2B C2C C2D 0.0 . . . . ? C2B C2C C2D C2E 0.0 . . . . ? C2C C2D C2E C2F 0.0 . . . . ? C2D C2E C2F C2A 0.0 . . . . ? C2B C2A C2F C2E 0.0 . . . . ? P2 C2A C2F C2E -177.5(6) . . . . ? C2A P2 C2G C2H 24.7(5) . . . . ? C21 P2 C2G C2H -91.2(5) . . . . ? Pd1 P2 C2G C2H 161.3(3) . . . . ? C2A P2 C2G C2L -158.2(4) . . . . ? C21 P2 C2G C2L 85.9(5) . . . . ? Pd1 P2 C2G C2L -21.5(5) . . . . ? C2L C2G C2H C2I 0.0 . . . . ? P2 C2G C2H C2I 177.1(5) . . . . ? C2G C2H C2I C2J 0.0 . . . . ? C2H C2I C2J C2K 0.0 . . . . ? C2I C2J C2K C2L 0.0 . . . . ? C2J C2K C2L C2G 0.0 . . . . ? C2H C2G C2L C2K 0.0 . . . . ? P2 C2G C2L C2K -177.1(5) . . . . ? C31 P3 C3A C3B -50.3(4) . . . . ? C3G P3 C3A C3B -157.3(3) . . . . ? Pd2 P3 C3A C3B 72.5(3) 3_556 . . . ? C31 P3 C3A C3F 134.5(4) . . . . ? C3G P3 C3A C3F 27.5(4) . . . . ? Pd2 P3 C3A C3F -102.7(3) 3_556 . . . ? C3F C3A C3B C3C 0.0 . . . . ? P3 C3A C3B C3C -175.2(4) . . . . ? C3A C3B C3C C3D 0.0 . . . . ? C3B C3C C3D C3E 0.0 . . . . ? C3C C3D C3E C3F 0.0 . . . . ? C3D C3E C3F C3A 0.0 . . . . ? C3B C3A C3F C3E 0.0 . . . . ? P3 C3A C3F C3E 175.2(4) . . . . ? C31 P3 C3G C3H 108.4(4) . . . . ? C3A P3 C3G C3H -142.4(3) . . . . ? Pd2 P3 C3G C3H -27.1(4) 3_556 . . . ? C31 P3 C3G C3L -65.6(4) . . . . ? C3A P3 C3G C3L 43.5(4) . . . . ? Pd2 P3 C3G C3L 158.8(3) 3_556 . . . ? C3L C3G C3H C3I 0.0 . . . . ? P3 C3G C3H C3I -174.1(4) . . . . ? C3G C3H C3I C3J 0.0 . . . . ? C3H C3I C3J C3K 0.0 . . . . ? C3I C3J C3K C3L 0.0 . . . . ? C3J C3K C3L C3G 0.0 . . . . ? C3H C3G C3L C3K 0.0 . . . . ? P3 C3G C3L C3K 174.1(4) . . . . ? C41 P4 C4A C4B -98.3(4) . . . . ? C4G P4 C4A C4B 11.0(4) . . . . ? Pd2 P4 C4A C4B 131.1(3) . . . . ? C41 P4 C4A C4F 81.6(4) . . . . ? C4G P4 C4A C4F -169.2(3) . . . . ? Pd2 P4 C4A C4F -49.1(4) . . . . ? C4F C4A C4B C4C 0.0 . . . . ? P4 C4A C4B C4C 179.9(5) . . . . ? C4A C4B C4C C4D 0.0 . . . . ? C4B C4C C4D C4E 0.0 . . . . ? C4C C4D C4E C4F 0.0 . . . . ? C4D C4E C4F C4A 0.0 . . . . ? C4B C4A C4F C4E 0.0 . . . . ? P4 C4A C4F C4E -179.9(4) . . . . ? C4A P4 C4G C4H -73.4(4) . . . . ? C41 P4 C4G C4H 36.4(4) . . . . ? Pd2 P4 C4G C4H 160.2(3) . . . . ? C4A P4 C4G C4L 108.3(4) . . . . ? C41 P4 C4G C4L -141.9(4) . . . . ? Pd2 P4 C4G C4L -18.1(3) . . . . ? C4L C4G C4H C4I 0.0 . . . . ? P4 C4G C4H C4I -178.3(4) . . . . ? C4G C4H C4I C4J 0.0 . . . . ? C4H C4I C4J C4K 0.0 . . . . ? C4I C4J C4K C4L 0.0 . . . . ? C4J C4K C4L C4G 0.0 . . . . ? C4H C4G C4L C4K 0.0 . . . . ? P4 C4G C4L C4K 178.3(4) . . . . ? C52B Cl51 C52A C53A -15(13) . . . . ? Cl51 C52A C53A Cl54 -166(6) . . . . ? C52A Cl51 C52B C53B -179(22) . . . . ? Cl51 C52B C53B Cl55 -152(5) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.498 _refine_diff_density_min -1.905 _refine_diff_density_rms 0.135 # Attachment 'complex3a.cif' data_02145 _database_code_depnum_ccdc_archive 'CCDC 664676' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H60 Cl2 N2 P4 Pd2, 2(C F3 O3 S)' _chemical_formula_sum 'C64 H60 Cl2 F6 N2 O6 P4 Pd2 S2' _chemical_formula_weight 1538.84 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.9519(5) _cell_length_b 12.4261(2) _cell_length_c 17.3210(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.7070(10) _cell_angle_gamma 90.00 _cell_volume 6389.41(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7455 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3112 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6425 _exptl_absorpt_correction_T_max 0.7777 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33729 _diffrn_reflns_av_R_equivalents 0.049 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.49 _reflns_number_total 7334 _reflns_number_gt 5491 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0463P)^2^+24.4245P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 7334 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1100 _refine_ls_wR_factor_gt 0.1014 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.382788(8) 0.32028(2) 0.146332(15) 0.01968(8) Uani 1 1 d . . . Cl Cl 0.45164(3) 0.32213(8) 0.13413(6) 0.0296(2) Uani 1 1 d . . . P1 P 0.37882(3) 0.13464(8) 0.15776(5) 0.0226(2) Uani 1 1 d . . . P2 P 0.37700(3) 0.50429(7) 0.15002(5) 0.02116(19) Uani 1 1 d . . . C1A C 0.42391(8) 0.06613(19) 0.23823(13) 0.0278(8) Uani 1 1 d G . . C1B C 0.45624(9) 0.12606(16) 0.29930(16) 0.0423(10) Uani 1 1 d G . . H1BA H 0.4561 0.2023 0.2956 0.051 Uiso 1 1 calc R . . C1C C 0.48871(9) 0.0744(2) 0.36582(15) 0.0607(15) Uani 1 1 d G . . H1CA H 0.5108 0.1153 0.4076 0.073 Uiso 1 1 calc R . . C1D C 0.48885(9) -0.0372(2) 0.37127(17) 0.0631(16) Uani 1 1 d G . . H1DA H 0.5110 -0.0726 0.4167 0.076 Uiso 1 1 calc R . . C1E C 0.45652(11) -0.09716(16) 0.3102(2) 0.0567(13) Uani 1 1 d G . . H1EA H 0.4566 -0.1734 0.3139 0.068 Uiso 1 1 calc R . . C1F C 0.42406(9) -0.04548(18) 0.24368(15) 0.0436(10) Uani 1 1 d G . . H1FA H 0.4020 -0.0864 0.2019 0.052 Uiso 1 1 calc R . . C1G C 0.36398(9) 0.0594(2) 0.06176(12) 0.0294(8) Uani 1 1 d G . . C1H C 0.38325(8) 0.0892(2) 0.00497(15) 0.0360(9) Uani 1 1 d G . . H1HA H 0.4064 0.1418 0.0197 0.043 Uiso 1 1 calc R . . C1I C 0.36860(11) 0.0419(2) -0.07329(14) 0.0539(13) Uani 1 1 d G . . H1IA H 0.3818 0.0623 -0.1121 0.065 Uiso 1 1 calc R . . C1J C 0.33466(11) -0.0351(2) -0.09477(13) 0.0554(14) Uani 1 1 d G . . H1JA H 0.3246 -0.0674 -0.1483 0.067 Uiso 1 1 calc R . . C1K C 0.31538(9) -0.0649(2) -0.03799(16) 0.0485(12) Uani 1 1 d G . . H1KA H 0.2922 -0.1175 -0.0527 0.058 Uiso 1 1 calc R . . C1L C 0.33004(9) -0.0177(2) 0.04028(14) 0.0374(9) Uani 1 1 d G . . H1LA H 0.3169 -0.0380 0.0791 0.045 Uiso 1 1 calc R . . C2A C 0.40692(7) 0.5541(2) 0.25495(11) 0.0250(7) Uani 1 1 d G . . C2B C 0.38678(6) 0.6210(2) 0.29548(14) 0.0314(8) Uani 1 1 d G . . H2BA H 0.3561 0.6413 0.2688 0.038 Uiso 1 1 calc R . . C2C C 0.41151(8) 0.65824(19) 0.37505(14) 0.0365(9) Uani 1 1 d G . . H2CA H 0.3977 0.7040 0.4027 0.044 Uiso 1 1 calc R . . C2D C 0.45639(8) 0.6286(2) 0.41409(11) 0.0385(10) Uani 1 1 d G . . H2DA H 0.4733 0.6540 0.4685 0.046 Uiso 1 1 calc R . . C2E C 0.47653(6) 0.5617(2) 0.37357(14) 0.0427(10) Uani 1 1 d G . . H2EA H 0.5072 0.5414 0.4003 0.051 Uiso 1 1 calc R . . C2F C 0.45180(7) 0.5245(2) 0.29399(14) 0.0328(9) Uani 1 1 d G . . H2FA H 0.4656 0.4788 0.2663 0.039 Uiso 1 1 calc R . . C2G C 0.39121(8) 0.59262(17) 0.08052(13) 0.0244(7) Uani 1 1 d G . . C2H C 0.39692(10) 0.70226(18) 0.09694(14) 0.0398(10) Uani 1 1 d G . . H2HA H 0.3928 0.7313 0.1444 0.048 Uiso 1 1 calc R . . C2I C 0.40864(11) 0.76936(14) 0.04394(17) 0.0473(11) Uani 1 1 d G . . H2IA H 0.4125 0.8443 0.0552 0.057 Uiso 1 1 calc R . . C2J C 0.41464(10) 0.72682(19) -0.02547(15) 0.0410(10) Uani 1 1 d G . . H2JA H 0.4226 0.7727 -0.0617 0.049 Uiso 1 1 calc R . . C2K C 0.40892(9) 0.6172(2) -0.04188(12) 0.0359(9) Uani 1 1 d G . . H2KA H 0.4130 0.5881 -0.0893 0.043 Uiso 1 1 calc R . . C2L C 0.39721(9) 0.55007(14) 0.01111(14) 0.0313(8) Uani 1 1 d G . . H2LA H 0.3933 0.4751 -0.0001 0.038 Uiso 1 1 calc R . . C11 C 0.33050(12) 0.1238(3) 0.1905(2) 0.0271(8) Uani 1 1 d . . . H11A H 0.3037 0.0987 0.1434 0.033 Uiso 1 1 calc R . . H11B H 0.3371 0.0709 0.2362 0.033 Uiso 1 1 calc R . . C12 C 0.32129(12) 0.2329(3) 0.2194(2) 0.0250(7) Uani 1 1 d . . . H12A H 0.3458 0.2519 0.2724 0.030 Uiso 1 1 calc R . . H12B H 0.2927 0.2307 0.2291 0.030 Uiso 1 1 calc R . . C21 C 0.31707(11) 0.5150(3) 0.1310(2) 0.0262(8) Uani 1 1 d . . . H21A H 0.3102 0.5860 0.1494 0.031 Uiso 1 1 calc R . . H21B H 0.2989 0.5066 0.0710 0.031 Uiso 1 1 calc R . . C22 C 0.30658(12) 0.4253(3) 0.1806(2) 0.0250(8) Uani 1 1 d . . . H22A H 0.3241 0.4362 0.2405 0.030 Uiso 1 1 calc R . . H22B H 0.2742 0.4271 0.1719 0.030 Uiso 1 1 calc R . . N31 N 0.31823(9) 0.3171(2) 0.15370(16) 0.0200(6) Uani 1 1 d . . . C32 C 0.28284(11) 0.2852(3) 0.0738(2) 0.0219(7) Uani 1 1 d . . . C33 C 0.23994(12) 0.2612(3) 0.0711(2) 0.0262(8) Uani 1 1 d . . . H33A H 0.2328 0.2692 0.1194 0.039 Uiso 1 1 calc R . . C34 C 0.29257(11) 0.2747(3) 0.0027(2) 0.0237(7) Uani 1 1 d . . . H34A H 0.3218 0.2923 0.0044 0.035 Uiso 1 1 calc R . . F41 F 0.22946(13) 0.8187(3) 0.04252(17) 0.0788(10) Uani 1 1 d . . . F42 F 0.23722(9) 0.9682(2) 0.10096(19) 0.0661(9) Uani 1 1 d . . . F43 F 0.19501(8) 0.8487(3) 0.12406(17) 0.0619(8) Uani 1 1 d . . . C44 C 0.23314(15) 0.8653(4) 0.1141(3) 0.0447(11) Uani 1 1 d . . . S45 S 0.28069(3) 0.81209(8) 0.20038(6) 0.0303(2) Uani 1 1 d . . . O46 O 0.28011(12) 0.8775(3) 0.2676(2) 0.0662(10) Uani 1 1 d . . . O47 O 0.26724(13) 0.7026(3) 0.2071(2) 0.0633(10) Uani 1 1 d . . . O48 O 0.31839(11) 0.8254(3) 0.1780(2) 0.0692(12) 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 Pd 0.01698(13) 0.02126(14) 0.01929(13) -0.00115(11) 0.00494(9) -0.00013(10) Cl 0.0204(4) 0.0333(5) 0.0367(5) 0.0032(4) 0.0123(3) 0.0018(4) P1 0.0246(5) 0.0216(5) 0.0223(4) 0.0011(3) 0.0096(4) -0.0014(4) P2 0.0199(4) 0.0204(4) 0.0213(4) -0.0017(3) 0.0054(3) 0.0002(3) C1A 0.0271(19) 0.032(2) 0.0284(18) 0.0086(15) 0.0147(15) 0.0041(15) C1B 0.034(2) 0.044(3) 0.042(2) 0.014(2) 0.0057(18) -0.0040(19) C1C 0.037(3) 0.073(4) 0.053(3) 0.025(3) -0.006(2) -0.008(2) C1D 0.032(3) 0.080(4) 0.074(3) 0.049(3) 0.016(2) 0.015(3) C1E 0.057(3) 0.043(3) 0.073(3) 0.026(3) 0.028(3) 0.013(2) C1F 0.051(3) 0.035(2) 0.044(2) 0.0047(19) 0.016(2) 0.006(2) C1G 0.036(2) 0.0273(19) 0.0264(17) -0.0001(15) 0.0133(16) -0.0005(16) C1H 0.046(2) 0.032(2) 0.035(2) 0.0004(17) 0.0196(19) -0.0034(18) C1I 0.089(4) 0.050(3) 0.032(2) -0.005(2) 0.034(2) -0.008(3) C1J 0.093(4) 0.044(3) 0.030(2) -0.012(2) 0.025(2) -0.011(3) C1K 0.060(3) 0.037(3) 0.046(2) -0.014(2) 0.017(2) -0.015(2) C1L 0.050(3) 0.031(2) 0.035(2) -0.0080(17) 0.0193(19) -0.0120(18) C2A 0.0229(18) 0.0270(19) 0.0239(16) -0.0003(14) 0.0071(14) -0.0040(14) C2B 0.036(2) 0.026(2) 0.0309(19) -0.0006(16) 0.0109(16) 0.0044(16) C2C 0.051(3) 0.030(2) 0.0300(19) -0.0075(16) 0.0168(18) -0.0010(18) C2D 0.043(2) 0.043(2) 0.0259(19) -0.0065(18) 0.0079(17) -0.0121(19) C2E 0.029(2) 0.059(3) 0.035(2) -0.007(2) 0.0056(17) -0.009(2) C2F 0.0219(19) 0.047(2) 0.0290(18) -0.0079(17) 0.0092(15) -0.0030(17) C2G 0.0199(17) 0.0257(19) 0.0256(17) 0.0008(14) 0.0061(14) 0.0013(14) C2H 0.054(3) 0.028(2) 0.045(2) -0.0065(18) 0.029(2) -0.0053(19) C2I 0.063(3) 0.034(2) 0.052(3) -0.001(2) 0.031(2) -0.009(2) C2J 0.038(2) 0.043(3) 0.045(2) 0.013(2) 0.0177(19) 0.0035(19) C2K 0.033(2) 0.047(3) 0.0291(19) 0.0084(18) 0.0138(17) 0.0101(18) C2L 0.035(2) 0.029(2) 0.0285(18) 0.0003(16) 0.0097(16) 0.0042(17) C11 0.0286(19) 0.030(2) 0.0246(17) 0.0042(15) 0.0116(15) -0.0022(15) C12 0.0248(18) 0.030(2) 0.0196(16) 0.0011(14) 0.0076(14) -0.0025(15) C21 0.0202(17) 0.0271(19) 0.0285(18) -0.0026(15) 0.0058(14) 0.0042(14) C22 0.0212(18) 0.0270(19) 0.0266(17) -0.0068(14) 0.0086(14) 0.0005(14) N31 0.0171(13) 0.0226(14) 0.0198(13) -0.0019(12) 0.0061(11) -0.0017(11) C32 0.0194(17) 0.0236(17) 0.0190(15) -0.0023(13) 0.0029(13) 0.0001(13) C33 0.0262(19) 0.034(2) 0.0199(16) -0.0035(15) 0.0100(14) -0.0025(15) C34 0.0163(16) 0.0298(19) 0.0230(16) 0.0001(14) 0.0051(13) -0.0022(14) F41 0.105(3) 0.091(3) 0.0352(15) -0.0041(16) 0.0197(16) -0.006(2) F42 0.0459(17) 0.0422(16) 0.090(2) 0.0270(15) 0.0019(15) -0.0018(13) F43 0.0268(13) 0.093(2) 0.0593(17) 0.0285(16) 0.0088(12) -0.0039(14) C44 0.038(2) 0.052(3) 0.042(2) 0.011(2) 0.0137(19) -0.003(2) S45 0.0274(5) 0.0331(5) 0.0313(5) 0.0053(4) 0.0119(4) 0.0070(4) O46 0.059(2) 0.091(3) 0.0415(18) -0.0143(19) 0.0102(16) 0.009(2) O47 0.064(2) 0.047(2) 0.088(3) 0.0260(19) 0.039(2) 0.0134(17) O48 0.0392(19) 0.093(3) 0.087(3) 0.048(2) 0.0372(19) 0.0195(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 Pd N31 2.114(3) . ? Pd Cl 2.2866(9) . ? Pd P2 2.2968(9) . ? Pd P1 2.3227(10) . ? P1 C1A 1.805(2) . ? P1 C1G 1.8113(19) . ? P1 C11 1.836(4) . ? P2 C2G 1.8067(19) . ? P2 C2A 1.8209(18) . ? P2 C21 1.824(4) . ? C1A C1B 1.3900 . ? C1A C1F 1.3900 . ? C1B C1C 1.3900 . ? C1B H1BA 0.9500 . ? C1C C1D 1.3900 . ? C1C H1CA 0.9500 . ? C1D C1E 1.3900 . ? C1D H1DA 0.9500 . ? C1E C1F 1.3900 . ? C1E H1EA 0.9500 . ? C1F H1FA 0.9500 . ? C1G C1H 1.3900 . ? C1G C1L 1.3900 . ? C1H C1I 1.3900 . ? C1H H1HA 0.9500 . ? C1I C1J 1.3900 . ? C1I H1IA 0.9500 . ? C1J C1K 1.3900 . ? C1J H1JA 0.9500 . ? C1K C1L 1.3900 . ? C1K H1KA 0.9500 . ? C1L H1LA 0.9500 . ? C2A C2B 1.3900 . ? C2A C2F 1.3900 . ? C2B C2C 1.3900 . ? C2B H2BA 0.9500 . ? C2C C2D 1.3900 . ? C2C H2CA 0.9500 . ? C2D C2E 1.3900 . ? C2D H2DA 0.9500 . ? C2E C2F 1.3900 . ? C2E H2EA 0.9500 . ? C2F H2FA 0.9500 . ? C2G C2H 1.3900 . ? C2G C2L 1.3900 . ? C2H C2I 1.3900 . ? C2H H2HA 0.9500 . ? C2I C2J 1.3900 . ? C2I H2IA 0.9500 . ? C2J C2K 1.3900 . ? C2J H2JA 0.9500 . ? C2K C2L 1.3900 . ? C2K H2KA 0.9500 . ? C2L H2LA 0.9500 . ? C11 C12 1.511(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N31 1.523(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C21 C22 1.519(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 N31 1.514(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N31 C32 1.482(4) . ? C32 C34 1.382(5) . ? C32 C33 1.386(5) . ? C33 C34 1.389(5) 7 ? C33 H33A 0.9500 . ? C34 C33 1.389(5) 7 ? C34 H34A 0.9500 . ? F41 C44 1.334(5) . ? F42 C44 1.313(5) . ? F43 C44 1.308(5) . ? C44 S45 1.816(4) . ? S45 O48 1.405(3) . ? S45 O46 1.426(4) . ? S45 O47 1.445(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N31 Pd Cl 178.23(7) . . ? N31 Pd P2 85.77(8) . . ? Cl Pd P2 94.75(3) . . ? N31 Pd P1 83.76(8) . . ? Cl Pd P1 95.89(3) . . ? P2 Pd P1 168.19(3) . . ? C1A P1 C1G 109.18(13) . . ? C1A P1 C11 104.43(15) . . ? C1G P1 C11 106.32(15) . . ? C1A P1 Pd 118.76(9) . . ? C1G P1 Pd 116.01(9) . . ? C11 P1 Pd 100.24(12) . . ? C2G P2 C2A 106.84(12) . . ? C2G P2 C21 109.91(15) . . ? C2A P2 C21 106.53(14) . . ? C2G P2 Pd 122.92(8) . . ? C2A P2 Pd 110.40(9) . . ? C21 P2 Pd 99.09(12) . . ? C1B C1A C1F 120.0 . . ? C1B C1A P1 119.42(15) . . ? C1F C1A P1 120.31(15) . . ? C1A C1B C1C 120.0 . . ? C1A C1B H1BA 120.0 . . ? C1C C1B H1BA 120.0 . . ? C1B C1C C1D 120.0 . . ? C1B C1C H1CA 120.0 . . ? C1D C1C H1CA 120.0 . . ? C1E C1D C1C 120.0 . . ? C1E C1D H1DA 120.0 . . ? C1C C1D H1DA 120.0 . . ? C1F C1E C1D 120.0 . . ? C1F C1E H1EA 120.0 . . ? C1D C1E H1EA 120.0 . . ? C1E C1F C1A 120.0 . . ? C1E C1F H1FA 120.0 . . ? C1A C1F H1FA 120.0 . . ? C1H C1G C1L 120.0 . . ? C1H C1G P1 118.55(14) . . ? C1L C1G P1 120.98(14) . . ? C1I C1H C1G 120.0 . . ? C1I C1H H1HA 120.0 . . ? C1G C1H H1HA 120.0 . . ? C1H C1I C1J 120.0 . . ? C1H C1I H1IA 120.0 . . ? C1J C1I H1IA 120.0 . . ? C1K C1J C1I 120.0 . . ? C1K C1J H1JA 120.0 . . ? C1I C1J H1JA 120.0 . . ? C1J C1K C1L 120.0 . . ? C1J C1K H1KA 120.0 . . ? C1L C1K H1KA 120.0 . . ? C1K C1L C1G 120.0 . . ? C1K C1L H1LA 120.0 . . ? C1G C1L H1LA 120.0 . . ? C2B C2A C2F 120.0 . . ? C2B C2A P2 122.49(13) . . ? C2F C2A P2 117.50(13) . . ? C2C C2B C2A 120.0 . . ? C2C C2B H2BA 120.0 . . ? C2A C2B H2BA 120.0 . . ? C2B C2C C2D 120.0 . . ? C2B C2C H2CA 120.0 . . ? C2D C2C H2CA 120.0 . . ? C2E C2D C2C 120.0 . . ? C2E C2D H2DA 120.0 . . ? C2C C2D H2DA 120.0 . . ? C2F C2E C2D 120.0 . . ? C2F C2E H2EA 120.0 . . ? C2D C2E H2EA 120.0 . . ? C2E C2F C2A 120.0 . . ? C2E C2F H2FA 120.0 . . ? C2A C2F H2FA 120.0 . . ? C2H C2G C2L 120.0 . . ? C2H C2G P2 120.37(13) . . ? C2L C2G P2 119.62(13) . . ? C2I C2H C2G 120.0 . . ? C2I C2H H2HA 120.0 . . ? C2G C2H H2HA 120.0 . . ? C2H C2I C2J 120.0 . . ? C2H C2I H2IA 120.0 . . ? C2J C2I H2IA 120.0 . . ? C2I C2J C2K 120.0 . . ? C2I C2J H2JA 120.0 . . ? C2K C2J H2JA 120.0 . . ? C2L C2K C2J 120.0 . . ? C2L C2K H2KA 120.0 . . ? C2J C2K H2KA 120.0 . . ? C2K C2L C2G 120.0 . . ? C2K C2L H2LA 120.0 . . ? C2G C2L H2LA 120.0 . . ? C12 C11 P1 109.0(2) . . ? C12 C11 H11A 109.9 . . ? P1 C11 H11A 109.9 . . ? C12 C11 H11B 109.9 . . ? P1 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C11 C12 N31 109.6(3) . . ? C11 C12 H12A 109.8 . . ? N31 C12 H12A 109.8 . . ? C11 C12 H12B 109.8 . . ? N31 C12 H12B 109.8 . . ? H12A C12 H12B 108.2 . . ? C22 C21 P2 106.3(2) . . ? C22 C21 H21A 110.5 . . ? P2 C21 H21A 110.5 . . ? C22 C21 H21B 110.5 . . ? P2 C21 H21B 110.5 . . ? H21A C21 H21B 108.7 . . ? N31 C22 C21 110.3(3) . . ? N31 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? N31 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C32 N31 C22 109.6(3) . . ? C32 N31 C12 109.2(3) . . ? C22 N31 C12 109.6(3) . . ? C32 N31 Pd 111.9(2) . . ? C22 N31 Pd 111.0(2) . . ? C12 N31 Pd 105.28(19) . . ? C34 C32 C33 119.7(3) . . ? C34 C32 N31 120.8(3) . . ? C33 C32 N31 119.5(3) . . ? C32 C33 C34 119.5(3) . 7 ? C32 C33 H33A 120.2 . . ? C34 C33 H33A 120.2 7 . ? C32 C34 C33 120.8(3) . 7 ? C32 C34 H34A 119.6 . . ? C33 C34 H34A 119.6 7 . ? F43 C44 F42 109.5(4) . . ? F43 C44 F41 106.7(4) . . ? F42 C44 F41 103.9(4) . . ? F43 C44 S45 111.8(3) . . ? F42 C44 S45 113.0(3) . . ? F41 C44 S45 111.5(3) . . ? O48 S45 O46 115.4(3) . . ? O48 S45 O47 116.4(2) . . ? O46 S45 O47 112.2(2) . . ? O48 S45 C44 105.8(2) . . ? O46 S45 C44 101.8(2) . . ? O47 S45 C44 103.1(2) . . ? 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 N31 Pd P1 C1A -126.23(13) . . . . ? Cl Pd P1 C1A 55.52(11) . . . . ? P2 Pd P1 C1A -98.54(18) . . . . ? N31 Pd P1 C1G 100.55(12) . . . . ? Cl Pd P1 C1G -77.71(10) . . . . ? P2 Pd P1 C1G 128.23(17) . . . . ? N31 Pd P1 C11 -13.40(14) . . . . ? Cl Pd P1 C11 168.35(12) . . . . ? P2 Pd P1 C11 14.3(2) . . . . ? N31 Pd P2 C2G -134.13(13) . . . . ? Cl Pd P2 C2G 44.16(11) . . . . ? P1 Pd P2 C2G -161.73(16) . . . . ? N31 Pd P2 C2A 98.35(11) . . . . ? Cl Pd P2 C2A -83.36(9) . . . . ? P1 Pd P2 C2A 70.75(18) . . . . ? N31 Pd P2 C21 -13.17(13) . . . . ? Cl Pd P2 C21 165.12(12) . . . . ? P1 Pd P2 C21 -40.8(2) . . . . ? C1G P1 C1A C1B 146.04(16) . . . . ? C11 P1 C1A C1B -100.58(19) . . . . ? Pd P1 C1A C1B 9.94(19) . . . . ? C1G P1 C1A C1F -39.91(19) . . . . ? C11 P1 C1A C1F 73.5(2) . . . . ? Pd P1 C1A C1F -176.01(13) . . . . ? C1F C1A C1B C1C 0.0 . . . . ? P1 C1A C1B C1C 174.1(2) . . . . ? C1A C1B C1C C1D 0.0 . . . . ? C1B C1C C1D C1E 0.0 . . . . ? C1C C1D C1E C1F 0.0 . . . . ? C1D C1E C1F C1A 0.0 . . . . ? C1B C1A C1F C1E 0.0 . . . . ? P1 C1A C1F C1E -174.0(2) . . . . ? C1A P1 C1G C1H -95.46(18) . . . . ? C11 P1 C1G C1H 152.41(18) . . . . ? Pd P1 C1G C1H 41.98(18) . . . . ? C1A P1 C1G C1L 92.38(18) . . . . ? C11 P1 C1G C1L -19.8(2) . . . . ? Pd P1 C1G C1L -130.19(14) . . . . ? C1L C1G C1H C1I 0.0 . . . . ? P1 C1G C1H C1I -172.2(2) . . . . ? C1G C1H C1I C1J 0.0 . . . . ? C1H C1I C1J C1K 0.0 . . . . ? C1I C1J C1K C1L 0.0 . . . . ? C1J C1K C1L C1G 0.0 . . . . ? C1H C1G C1L C1K 0.0 . . . . ? P1 C1G C1L C1K 172.1(2) . . . . ? C2G P2 C2A C2B 96.76(17) . . . . ? C21 P2 C2A C2B -20.7(2) . . . . ? Pd P2 C2A C2B -127.31(14) . . . . ? C2G P2 C2A C2F -82.10(16) . . . . ? C21 P2 C2A C2F 160.45(17) . . . . ? Pd P2 C2A C2F 53.82(15) . . . . ? C2F C2A C2B C2C 0.0 . . . . ? P2 C2A C2B C2C -178.8(2) . . . . ? C2A C2B C2C C2D 0.0 . . . . ? C2B C2C C2D C2E 0.0 . . . . ? C2C C2D C2E C2F 0.0 . . . . ? C2D C2E C2F C2A 0.0 . . . . ? C2B C2A C2F C2E 0.0 . . . . ? P2 C2A C2F C2E 178.89(19) . . . . ? C2A P2 C2G C2H -36.38(17) . . . . ? C21 P2 C2G C2H 78.82(19) . . . . ? Pd P2 C2G C2H -165.41(12) . . . . ? C2A P2 C2G C2L 142.48(15) . . . . ? C21 P2 C2G C2L -102.31(18) . . . . ? Pd P2 C2G C2L 13.45(19) . . . . ? C2L C2G C2H C2I 0.0 . . . . ? P2 C2G C2H C2I 178.86(19) . . . . ? C2G C2H C2I C2J 0.0 . . . . ? C2H C2I C2J C2K 0.0 . . . . ? C2I C2J C2K C2L 0.0 . . . . ? C2J C2K C2L C2G 0.0 . . . . ? C2H C2G C2L C2K 0.0 . . . . ? P2 C2G C2L C2K -178.87(19) . . . . ? C1A P1 C11 C12 108.0(2) . . . . ? C1G P1 C11 C12 -136.6(2) . . . . ? Pd P1 C11 C12 -15.4(2) . . . . ? P1 C11 C12 N31 50.9(3) . . . . ? C2G P2 C21 C22 170.4(2) . . . . ? C2A P2 C21 C22 -74.2(2) . . . . ? Pd P2 C21 C22 40.4(2) . . . . ? P2 C21 C22 N31 -58.7(3) . . . . ? C21 C22 N31 C32 -77.1(3) . . . . ? C21 C22 N31 C12 162.9(3) . . . . ? C21 C22 N31 Pd 47.0(3) . . . . ? C11 C12 N31 C32 56.9(3) . . . . ? C11 C12 N31 C22 177.0(3) . . . . ? C11 C12 N31 Pd -63.5(3) . . . . ? Cl Pd N31 C32 1(3) . . . . ? P2 Pd N31 C32 107.6(2) . . . . ? P1 Pd N31 C32 -77.9(2) . . . . ? Cl Pd N31 C22 -122(3) . . . . ? P2 Pd N31 C22 -15.30(19) . . . . ? P1 Pd N31 C22 159.2(2) . . . . ? Cl Pd N31 C12 119(3) . . . . ? P2 Pd N31 C12 -133.88(19) . . . . ? P1 Pd N31 C12 40.65(18) . . . . ? C22 N31 C32 C34 115.4(3) . . . . ? C12 N31 C32 C34 -124.4(3) . . . . ? Pd N31 C32 C34 -8.3(4) . . . . ? C22 N31 C32 C33 -67.3(4) . . . . ? C12 N31 C32 C33 52.9(4) . . . . ? Pd N31 C32 C33 169.1(3) . . . . ? C34 C32 C33 C34 1.0(6) . . . 7 ? N31 C32 C33 C34 -176.3(3) . . . 7 ? C33 C32 C34 C33 -1.0(6) . . . 7 ? N31 C32 C34 C33 176.3(3) . . . 7 ? F43 C44 S45 O48 174.2(4) . . . . ? F42 C44 S45 O48 -61.7(4) . . . . ? F41 C44 S45 O48 54.9(4) . . . . ? F43 C44 S45 O46 -64.8(4) . . . . ? F42 C44 S45 O46 59.2(4) . . . . ? F41 C44 S45 O46 175.9(3) . . . . ? F43 C44 S45 O47 51.5(4) . . . . ? F42 C44 S45 O47 175.6(3) . . . . ? F41 C44 S45 O47 -67.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.025 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.097 # Attachment 'complex9.cif' data_02135 _database_code_depnum_ccdc_archive 'CCDC 664677' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H60 Ag2 F6 N2 O4 P4' _chemical_formula_sum 'C66 H60 Ag2 F6 N2 O4 P4' _chemical_formula_weight 1398.78 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' 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' Ag Ag -0.8971 1.1015 '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 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3770(2) _cell_length_b 11.8752(2) _cell_length_c 21.1926(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.2250(10) _cell_angle_gamma 90.00 _cell_volume 3065.41(9) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7063 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7507 _exptl_absorpt_correction_T_max 0.8385 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scans, and \w scans with \k offsets' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32166 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6271 _reflns_number_gt 4672 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1997-2001)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 2001)' _computing_publication_material SHELXTL/PC _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^)+(0.0404P)^2^+1.4576P] 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 6271 _refine_ls_number_parameters 358 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0912 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.048 _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 Ag Ag 0.810095(19) 0.235070(18) 0.353495(11) 0.03253(9) Uani 1 1 d . . . P1 P 0.64784(6) 0.11979(6) 0.35885(4) 0.03014(19) Uani 1 1 d . . . P2 P 0.92340(6) 0.19389(6) 0.27463(4) 0.02976(19) Uani 1 1 d . . . C1 C 0.9195(3) 0.0417(2) 0.26169(14) 0.0338(7) Uani 1 1 d . . . H1A H 0.8441 0.0189 0.2420 0.041 Uiso 1 1 calc R . . H1B H 0.9691 0.0217 0.2315 0.041 Uiso 1 1 calc R . . C2 C 0.9546(2) -0.0221(2) 0.32451(14) 0.0336(7) Uani 1 1 d . . . H2A H 0.9553 -0.1038 0.3151 0.040 Uiso 1 1 calc R . . H2B H 1.0305 0.0003 0.3434 0.040 Uiso 1 1 calc R . . N3 N 0.88360(19) -0.00246(19) 0.37180(11) 0.0292(6) Uani 1 1 d . . . C4 C 0.7820(2) -0.0688(2) 0.35831(14) 0.0346(7) Uani 1 1 d . . . H4A H 0.7976 -0.1469 0.3737 0.041 Uiso 1 1 calc R . . H4B H 0.7560 -0.0718 0.3114 0.041 Uiso 1 1 calc R . . C5 C 0.6920(2) -0.0195(2) 0.39032(14) 0.0338(7) Uani 1 1 d . . . H5A H 0.7191 -0.0136 0.4370 0.041 Uiso 1 1 calc R . . H5B H 0.6281 -0.0710 0.3837 0.041 Uiso 1 1 calc R . . C11 C 0.9409(2) -0.0040(2) 0.43680(13) 0.0279(7) Uani 1 1 d . . . C12 C 0.9250(2) -0.0846(2) 0.48144(14) 0.0342(7) Uani 1 1 d . . . H12A H 0.8731 -0.1432 0.4694 0.051 Uiso 1 1 calc R . . C13 C 1.0161(3) 0.0808(2) 0.45628(14) 0.0355(7) Uani 1 1 d . . . H13A H 1.0276 0.1376 0.4266 0.053 Uiso 1 1 calc R . . C1A C 1.06985(12) 0.22838(16) 0.28917(9) 0.0316(7) Uani 1 1 d G . . C1B C 1.14215(17) 0.18213(16) 0.25303(9) 0.0412(8) Uani 1 1 d G . . H1BA H 1.1161 0.1302 0.2197 0.049 Uiso 1 1 calc R . . C1C C 1.25252(15) 0.21182(19) 0.26571(10) 0.0531(10) Uani 1 1 d G . . H1CA H 1.3019 0.1802 0.2410 0.064 Uiso 1 1 calc R . . C1D C 1.29058(12) 0.2877(2) 0.31453(11) 0.0530(10) Uani 1 1 d G . . H1DA H 1.3660 0.3080 0.3232 0.064 Uiso 1 1 calc R . . C1E C 1.21828(17) 0.33399(17) 0.35066(9) 0.0497(9) Uani 1 1 d G . . H1EA H 1.2443 0.3859 0.3840 0.060 Uiso 1 1 calc R . . C1F C 1.10792(15) 0.30431(16) 0.33798(9) 0.0379(8) Uani 1 1 d G . . H1FA H 1.0585 0.3359 0.3627 0.046 Uiso 1 1 calc R . . C1G C 0.86647(17) 0.25196(16) 0.19617(8) 0.0339(7) Uani 1 1 d G . . C1H C 0.87620(19) 0.20010(15) 0.13865(10) 0.0480(9) Uani 1 1 d G . . H1HA H 0.9151 0.1311 0.1389 0.058 Uiso 1 1 calc R . . C1I C 0.8291(2) 0.2492(2) 0.08075(8) 0.0628(12) Uani 1 1 d G . . H1IA H 0.8357 0.2138 0.0414 0.075 Uiso 1 1 calc R . . C1J C 0.7722(2) 0.3503(2) 0.08039(9) 0.0638(12) Uani 1 1 d G . . H1JA H 0.7400 0.3838 0.0408 0.077 Uiso 1 1 calc R . . C1K C 0.76247(18) 0.40211(16) 0.13792(11) 0.0535(10) Uani 1 1 d G . . H1KA H 0.7236 0.4711 0.1377 0.064 Uiso 1 1 calc R . . C1L C 0.80961(17) 0.35296(16) 0.19581(9) 0.0408(8) Uani 1 1 d G . . H1LA H 0.8030 0.3884 0.2351 0.049 Uiso 1 1 calc R . . C2A C 0.55324(15) 0.16428(16) 0.41108(9) 0.0318(7) Uani 1 1 d G . . C2B C 0.57107(16) 0.26920(15) 0.44014(10) 0.0358(7) Uani 1 1 d G . . H2BA H 0.6303 0.3148 0.4322 0.043 Uiso 1 1 calc R . . C2C C 0.5023(2) 0.30734(15) 0.48077(10) 0.0573(10) Uani 1 1 d G . . H2CA H 0.5145 0.3790 0.5006 0.069 Uiso 1 1 calc R . . C2D C 0.41562(18) 0.2406(2) 0.49233(10) 0.0545(10) Uani 1 1 d G . . H2DA H 0.3686 0.2666 0.5201 0.065 Uiso 1 1 calc R . . C2E C 0.39779(16) 0.13565(19) 0.46327(11) 0.0569(10) Uani 1 1 d G . . H2EA H 0.3386 0.0900 0.4712 0.068 Uiso 1 1 calc R . . C2F C 0.46660(17) 0.09751(14) 0.42264(10) 0.0482(9) Uani 1 1 d G . . H2FA H 0.4544 0.0258 0.4028 0.058 Uiso 1 1 calc R . . C2G C 0.56535(16) 0.08804(17) 0.27980(7) 0.0322(7) Uani 1 1 d G . . C2H C 0.58167(18) 0.15778(16) 0.22966(10) 0.0509(10) Uani 1 1 d G . . H2HA H 0.6312 0.2194 0.2376 0.061 Uiso 1 1 calc R . . C2I C 0.5255(2) 0.1374(2) 0.16789(8) 0.0690(12) Uani 1 1 d G . . H2IA H 0.5367 0.1851 0.1336 0.083 Uiso 1 1 calc R . . C2J C 0.4530(2) 0.0473(2) 0.15627(8) 0.0591(11) Uani 1 1 d G . . H2JA H 0.4146 0.0334 0.1141 0.071 Uiso 1 1 calc R . . C2K C 0.43667(17) -0.02241(17) 0.20641(11) 0.0553(10) Uani 1 1 d G . . H2KA H 0.3871 -0.0840 0.1985 0.066 Uiso 1 1 calc R . . C2L C 0.49284(18) -0.00206(16) 0.26817(9) 0.0462(9) Uani 1 1 d G . . H2LA H 0.4817 -0.0497 0.3024 0.055 Uiso 1 1 calc R . . O21 O 0.8177(2) 0.37870(19) 0.42468(11) 0.0538(7) Uani 1 1 d . . . O22 O 0.9005(3) 0.4864(2) 0.36172(14) 0.0785(9) Uani 1 1 d . . . C23 C 0.8570(3) 0.4667(3) 0.40832(17) 0.0423(8) Uani 1 1 d . A . C24 C 0.8528(4) 0.5670(3) 0.4541(2) 0.0603(11) Uani 1 1 d D . . F25A F 0.8156(10) 0.5426(4) 0.5052(3) 0.137(3) Uani 0.80 1 d PDU A 1 F26A F 0.9497(3) 0.6171(4) 0.4710(3) 0.1031(16) Uani 0.80 1 d PDU A 1 F27A F 0.7880(3) 0.6480(3) 0.4255(3) 0.0784(13) Uani 0.80 1 d PDU A 1 F25B F 0.859(5) 0.6637(16) 0.4276(16) 0.28(2) Uani 0.20 1 d PDU A 2 F26B F 0.7551(11) 0.563(3) 0.4727(10) 0.157(17) Uani 0.20 1 d PDU A 2 F27B F 0.8980(16) 0.547(2) 0.5123(7) 0.117(12) Uani 0.20 1 d PDU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.03344(14) 0.03226(13) 0.03211(14) -0.00321(10) 0.00647(10) -0.00215(10) P1 0.0294(4) 0.0319(4) 0.0291(4) -0.0016(3) 0.0049(3) -0.0031(3) P2 0.0332(4) 0.0288(4) 0.0273(4) -0.0011(3) 0.0054(3) 0.0008(3) C1 0.0399(18) 0.0320(15) 0.0305(16) -0.0064(13) 0.0084(14) 0.0008(13) C2 0.0366(18) 0.0297(16) 0.0352(17) 0.0004(13) 0.0083(14) 0.0072(13) N3 0.0299(13) 0.0335(13) 0.0232(13) 0.0001(10) 0.0023(11) 0.0023(10) C4 0.0396(19) 0.0317(16) 0.0301(17) 0.0004(13) -0.0002(14) -0.0012(13) C5 0.0326(17) 0.0369(16) 0.0306(17) 0.0033(13) 0.0020(14) -0.0029(13) C11 0.0278(16) 0.0263(14) 0.0288(16) 0.0016(12) 0.0027(13) 0.0041(12) C12 0.0361(18) 0.0268(14) 0.0358(17) 0.0036(13) -0.0045(14) -0.0032(13) C13 0.0412(18) 0.0301(15) 0.0338(17) 0.0087(13) 0.0031(14) -0.0020(13) C1A 0.0326(17) 0.0326(15) 0.0291(16) 0.0075(13) 0.0044(13) 0.0025(13) C1B 0.041(2) 0.0446(18) 0.0391(19) 0.0049(15) 0.0103(16) 0.0079(15) C1C 0.038(2) 0.064(2) 0.060(2) 0.020(2) 0.0181(18) 0.0141(17) C1D 0.033(2) 0.066(2) 0.056(2) 0.017(2) -0.0030(18) -0.0050(17) C1E 0.045(2) 0.053(2) 0.046(2) 0.0042(17) -0.0055(18) -0.0055(17) C1F 0.0375(18) 0.0403(17) 0.0344(18) 0.0021(14) 0.0020(15) 0.0039(14) C1G 0.0264(16) 0.0406(18) 0.0339(17) 0.0068(13) 0.0031(13) -0.0043(13) C1H 0.060(2) 0.051(2) 0.0313(18) 0.0027(16) 0.0040(17) 0.0030(17) C1I 0.084(3) 0.070(3) 0.0303(19) -0.0001(17) 0.001(2) -0.007(2) C1J 0.061(3) 0.069(3) 0.052(2) 0.022(2) -0.016(2) -0.003(2) C1K 0.038(2) 0.058(2) 0.062(3) 0.0223(19) 0.0035(18) 0.0063(17) C1L 0.0326(18) 0.0449(18) 0.045(2) 0.0083(15) 0.0079(15) 0.0022(14) C2A 0.0299(17) 0.0400(17) 0.0261(16) 0.0029(13) 0.0064(13) 0.0025(13) C2B 0.0363(18) 0.0363(17) 0.0374(18) -0.0044(14) 0.0137(14) -0.0041(13) C2C 0.070(3) 0.053(2) 0.054(2) -0.0083(19) 0.025(2) 0.003(2) C2D 0.055(2) 0.075(3) 0.039(2) 0.0042(18) 0.0233(18) 0.016(2) C2E 0.049(2) 0.075(3) 0.052(2) 0.000(2) 0.0221(19) -0.010(2) C2F 0.046(2) 0.056(2) 0.047(2) -0.0084(17) 0.0195(17) -0.0130(17) C2G 0.0305(17) 0.0350(16) 0.0301(16) -0.0053(13) 0.0026(13) 0.0018(13) C2H 0.059(2) 0.054(2) 0.0364(19) 0.0050(16) -0.0012(18) -0.0114(18) C2I 0.085(3) 0.082(3) 0.035(2) 0.013(2) -0.002(2) -0.008(2) C2J 0.059(3) 0.074(3) 0.038(2) -0.0108(19) -0.0101(19) 0.007(2) C2K 0.050(2) 0.060(2) 0.050(2) -0.0157(19) -0.0050(19) -0.0105(18) C2L 0.046(2) 0.053(2) 0.0376(19) -0.0016(16) 0.0016(17) -0.0112(17) O21 0.0746(18) 0.0416(14) 0.0513(15) -0.0168(11) 0.0278(13) -0.0215(12) O22 0.132(3) 0.0494(16) 0.0653(19) 0.0062(14) 0.0483(19) -0.0044(17) C23 0.048(2) 0.0358(18) 0.042(2) -0.0045(15) 0.0039(17) 0.0025(15) C24 0.064(3) 0.046(2) 0.068(3) -0.018(2) 0.006(2) 0.007(2) F25A 0.287(9) 0.064(3) 0.088(5) -0.027(3) 0.110(5) -0.016(5) F26A 0.070(3) 0.076(3) 0.153(4) -0.058(3) -0.009(3) -0.0128(19) F27A 0.070(2) 0.040(2) 0.120(3) -0.016(2) 0.005(2) 0.0180(18) F25B 0.54(7) 0.041(12) 0.27(4) -0.020(16) 0.10(5) -0.11(3) F26B 0.117(15) 0.22(3) 0.11(2) -0.11(2) -0.042(15) 0.102(19) F27B 0.066(11) 0.19(2) 0.079(14) -0.103(16) -0.034(12) 0.042(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 Ag O21 2.268(2) . ? Ag P2 2.4149(9) . ? Ag P1 2.4497(8) . ? P1 C2A 1.8263(18) . ? P1 C5 1.830(3) . ? P1 C2G 1.8396(15) . ? P2 C1G 1.8222(15) . ? P2 C1 1.827(3) . ? P2 C1A 1.8303(16) . ? C1 C2 1.527(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N3 1.464(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N3 C11 1.433(3) . ? N3 C4 1.468(4) . ? C4 C5 1.521(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C11 C13 1.383(4) . ? C11 C12 1.385(4) . ? C12 C13 1.391(4) 3_756 ? C12 H12A 0.9500 . ? C13 C12 1.391(4) 3_756 ? C13 H13A 0.9500 . ? C1A C1B 1.3900 . ? C1A C1F 1.3900 . ? C1B C1C 1.3900 . ? C1B H1BA 0.9500 . ? C1C C1D 1.3900 . ? C1C H1CA 0.9500 . ? C1D C1E 1.3900 . ? C1D H1DA 0.9500 . ? C1E C1F 1.3900 . ? C1E H1EA 0.9500 . ? C1F H1FA 0.9500 . ? C1G C1H 1.3900 . ? C1G C1L 1.3900 . ? C1H C1I 1.3900 . ? C1H H1HA 0.9500 . ? C1I C1J 1.3900 . ? C1I H1IA 0.9500 . ? C1J C1K 1.3900 . ? C1J H1JA 0.9500 . ? C1K C1L 1.3900 . ? C1K H1KA 0.9500 . ? C1L H1LA 0.9500 . ? C2A C2B 1.3900 . ? C2A C2F 1.3900 . ? C2B C2C 1.3900 . ? C2B H2BA 0.9500 . ? C2C C2D 1.3900 . ? C2C H2CA 0.9500 . ? C2D C2E 1.3900 . ? C2D H2DA 0.9500 . ? C2E C2F 1.3900 . ? C2E H2EA 0.9500 . ? C2F H2FA 0.9500 . ? C2G C2H 1.3900 . ? C2G C2L 1.3900 . ? C2H C2I 1.3900 . ? C2H H2HA 0.9500 . ? C2I C2J 1.3900 . ? C2I H2IA 0.9500 . ? C2J C2K 1.3900 . ? C2J H2JA 0.9500 . ? C2K C2L 1.3900 . ? C2K H2KA 0.9500 . ? C2L H2LA 0.9500 . ? O21 C23 1.228(4) . ? O22 C23 1.228(4) . ? C23 C24 1.543(5) . ? C24 F25A 1.283(6) . ? C24 F27B 1.284(13) . ? C24 F25B 1.287(14) . ? C24 F27A 1.328(5) . ? C24 F26A 1.330(5) . ? C24 F26B 1.337(15) . ? 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 O21 Ag P2 130.69(7) . . ? O21 Ag P1 109.10(7) . . ? P2 Ag P1 120.03(3) . . ? C2A P1 C5 102.87(12) . . ? C2A P1 C2G 107.42(10) . . ? C5 P1 C2G 103.20(11) . . ? C2A P1 Ag 119.04(7) . . ? C5 P1 Ag 109.13(10) . . ? C2G P1 Ag 113.54(7) . . ? C1G P2 C1 104.00(11) . . ? C1G P2 C1A 106.26(10) . . ? C1 P2 C1A 104.20(12) . . ? C1G P2 Ag 112.14(7) . . ? C1 P2 Ag 107.53(11) . . ? C1A P2 Ag 121.17(7) . . ? C2 C1 P2 111.37(19) . . ? C2 C1 H1A 109.4 . . ? P2 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? P2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N3 C2 C1 113.9(2) . . ? N3 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? N3 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C11 N3 C2 113.6(2) . . ? C11 N3 C4 116.2(2) . . ? C2 N3 C4 112.2(2) . . ? N3 C4 C5 112.1(2) . . ? N3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 P1 112.4(2) . . ? C4 C5 H5A 109.1 . . ? P1 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? P1 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C13 C11 C12 118.0(2) . . ? C13 C11 N3 118.0(3) . . ? C12 C11 N3 124.0(2) . . ? C11 C12 C13 120.8(3) . 3_756 ? C11 C12 H12A 119.6 . . ? C13 C12 H12A 119.6 3_756 . ? C11 C13 C12 121.2(3) . 3_756 ? C11 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 3_756 . ? C1B C1A C1F 120.0 . . ? C1B C1A P2 122.28(11) . . ? C1F C1A P2 117.72(11) . . ? C1A C1B C1C 120.0 . . ? C1A C1B H1BA 120.0 . . ? C1C C1B H1BA 120.0 . . ? C1D C1C C1B 120.0 . . ? C1D C1C H1CA 120.0 . . ? C1B C1C H1CA 120.0 . . ? C1C C1D C1E 120.0 . . ? C1C C1D H1DA 120.0 . . ? C1E C1D H1DA 120.0 . . ? C1D C1E C1F 120.0 . . ? C1D C1E H1EA 120.0 . . ? C1F C1E H1EA 120.0 . . ? C1E C1F C1A 120.0 . . ? C1E C1F H1FA 120.0 . . ? C1A C1F H1FA 120.0 . . ? C1H C1G C1L 120.0 . . ? C1H C1G P2 123.57(11) . . ? C1L C1G P2 116.43(11) . . ? C1G C1H C1I 120.0 . . ? C1G C1H H1HA 120.0 . . ? C1I C1H H1HA 120.0 . . ? C1J C1I C1H 120.0 . . ? C1J C1I H1IA 120.0 . . ? C1H C1I H1IA 120.0 . . ? C1I C1J C1K 120.0 . . ? C1I C1J H1JA 120.0 . . ? C1K C1J H1JA 120.0 . . ? C1J C1K C1L 120.0 . . ? C1J C1K H1KA 120.0 . . ? C1L C1K H1KA 120.0 . . ? C1K C1L C1G 120.0 . . ? C1K C1L H1LA 120.0 . . ? C1G C1L H1LA 120.0 . . ? C2B C2A C2F 120.0 . . ? C2B C2A P1 117.35(12) . . ? C2F C2A P1 122.65(12) . . ? C2A C2B C2C 120.0 . . ? C2A C2B H2BA 120.0 . . ? C2C C2B H2BA 120.0 . . ? C2D C2C C2B 120.0 . . ? C2D C2C H2CA 120.0 . . ? C2B C2C H2CA 120.0 . . ? C2E C2D C2C 120.0 . . ? C2E C2D H2DA 120.0 . . ? C2C C2D H2DA 120.0 . . ? C2D C2E C2F 120.0 . . ? C2D C2E H2EA 120.0 . . ? C2F C2E H2EA 120.0 . . ? C2E C2F C2A 120.0 . . ? C2E C2F H2FA 120.0 . . ? C2A C2F H2FA 120.0 . . ? C2H C2G C2L 120.0 . . ? C2H C2G P1 116.20(11) . . ? C2L C2G P1 123.76(11) . . ? C2I C2H C2G 120.0 . . ? C2I C2H H2HA 120.0 . . ? C2G C2H H2HA 120.0 . . ? C2H C2I C2J 120.0 . . ? C2H C2I H2IA 120.0 . . ? C2J C2I H2IA 120.0 . . ? C2K C2J C2I 120.0 . . ? C2K C2J H2JA 120.0 . . ? C2I C2J H2JA 120.0 . . ? C2J C2K C2L 120.0 . . ? C2J C2K H2KA 120.0 . . ? C2L C2K H2KA 120.0 . . ? C2K C2L C2G 120.0 . . ? C2K C2L H2LA 120.0 . . ? C2G C2L H2LA 120.0 . . ? C23 O21 Ag 115.1(2) . . ? O22 C23 O21 129.9(3) . . ? O22 C23 C24 115.3(3) . . ? O21 C23 C24 114.8(3) . . ? F25A C24 F27B 46.1(9) . . ? F25A C24 F25B 129(2) . . ? F27B C24 F25B 122.5(19) . . ? F25A C24 F27A 105.8(6) . . ? F27B C24 F27A 134.3(9) . . ? F25B C24 F27A 40(3) . . ? F25A C24 F26A 108.4(5) . . ? F27B C24 F26A 66.8(11) . . ? F25B C24 F26A 66(3) . . ? F27A C24 F26A 104.0(4) . . ? F25A C24 F26B 42.7(8) . . ? F27B C24 F26B 88.4(12) . . ? F25B C24 F26B 107(3) . . ? F27A C24 F26B 69.8(12) . . ? F26A C24 F26B 139.0(9) . . ? F25A C24 C23 114.4(4) . . ? F27B C24 C23 113.8(10) . . ? F25B C24 C23 113.7(16) . . ? F27A C24 C23 110.9(4) . . ? F26A C24 C23 112.6(4) . . ? F26B C24 C23 107.1(10) . . ? 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 O21 Ag P1 C2A 4.06(11) . . . . ? P2 Ag P1 C2A -171.54(8) . . . . ? O21 Ag P1 C5 -113.46(13) . . . . ? P2 Ag P1 C5 70.93(11) . . . . ? O21 Ag P1 C2G 132.04(11) . . . . ? P2 Ag P1 C2G -43.57(9) . . . . ? O21 Ag P2 C1G -93.29(11) . . . . ? P1 Ag P2 C1G 81.23(8) . . . . ? O21 Ag P2 C1 152.98(13) . . . . ? P1 Ag P2 C1 -32.49(10) . . . . ? O21 Ag P2 C1A 33.53(12) . . . . ? P1 Ag P2 C1A -151.95(8) . . . . ? C1G P2 C1 C2 -174.6(2) . . . . ? C1A P2 C1 C2 74.3(2) . . . . ? Ag P2 C1 C2 -55.5(2) . . . . ? P2 C1 C2 N3 61.5(3) . . . . ? C1 C2 N3 C11 -146.4(2) . . . . ? C1 C2 N3 C4 79.3(3) . . . . ? C11 N3 C4 C5 67.9(3) . . . . ? C2 N3 C4 C5 -159.0(2) . . . . ? N3 C4 C5 P1 64.6(3) . . . . ? C2A P1 C5 C4 -173.81(18) . . . . ? C2G P1 C5 C4 74.5(2) . . . . ? Ag P1 C5 C4 -46.5(2) . . . . ? C2 N3 C11 C13 66.6(3) . . . . ? C4 N3 C11 C13 -160.9(3) . . . . ? C2 N3 C11 C12 -114.0(3) . . . . ? C4 N3 C11 C12 18.5(4) . . . . ? C13 C11 C12 C13 -0.8(5) . . . 3_756 ? N3 C11 C12 C13 179.8(3) . . . 3_756 ? C12 C11 C13 C12 0.8(5) . . . 3_756 ? N3 C11 C13 C12 -179.8(3) . . . 3_756 ? C1G P2 C1A C1B -66.77(14) . . . . ? C1 P2 C1A C1B 42.72(16) . . . . ? Ag P2 C1A C1B 163.80(9) . . . . ? C1G P2 C1A C1F 112.73(12) . . . . ? C1 P2 C1A C1F -137.78(14) . . . . ? Ag P2 C1A C1F -16.70(13) . . . . ? C1F C1A C1B C1C 0.0 . . . . ? P2 C1A C1B C1C 179.49(15) . . . . ? C1A C1B C1C C1D 0.0 . . . . ? C1B C1C C1D C1E 0.0 . . . . ? C1C C1D C1E C1F 0.0 . . . . ? C1D C1E C1F C1A 0.0 . . . . ? C1B C1A C1F C1E 0.0 . . . . ? P2 C1A C1F C1E -179.52(14) . . . . ? C1 P2 C1G C1H -30.10(18) . . . . ? C1A P2 C1G C1H 79.53(14) . . . . ? Ag P2 C1G C1H -145.99(11) . . . . ? C1 P2 C1G C1L 149.06(15) . . . . ? C1A P2 C1G C1L -101.31(13) . . . . ? Ag P2 C1G C1L 33.17(13) . . . . ? C1L C1G C1H C1I 0.0 . . . . ? P2 C1G C1H C1I 179.13(17) . . . . ? C1G C1H C1I C1J 0.0 . . . . ? C1H C1I C1J C1K 0.0 . . . . ? C1I C1J C1K C1L 0.0 . . . . ? C1J C1K C1L C1G 0.0 . . . . ? C1H C1G C1L C1K 0.0 . . . . ? P2 C1G C1L C1K -179.19(16) . . . . ? C5 P1 C2A C2B 127.95(14) . . . . ? C2G P1 C2A C2B -123.57(12) . . . . ? Ag P1 C2A C2B 7.20(14) . . . . ? C5 P1 C2A C2F -51.58(15) . . . . ? C2G P1 C2A C2F 56.90(14) . . . . ? Ag P1 C2A C2F -172.33(10) . . . . ? C2F C2A C2B C2C 0.0 . . . . ? P1 C2A C2B C2C -179.54(15) . . . . ? C2A C2B C2C C2D 0.0 . . . . ? C2B C2C C2D C2E 0.0 . . . . ? C2C C2D C2E C2F 0.0 . . . . ? C2D C2E C2F C2A 0.0 . . . . ? C2B C2A C2F C2E 0.0 . . . . ? P1 C2A C2F C2E 179.52(16) . . . . ? C2A P1 C2G C2H 114.47(13) . . . . ? C5 P1 C2G C2H -137.28(15) . . . . ? Ag P1 C2G C2H -19.29(14) . . . . ? C2A P1 C2G C2L -67.83(15) . . . . ? C5 P1 C2G C2L 40.42(18) . . . . ? Ag P1 C2G C2L 158.41(12) . . . . ? C2L C2G C2H C2I 0.0 . . . . ? P1 C2G C2H C2I 177.79(16) . . . . ? C2G C2H C2I C2J 0.0 . . . . ? C2H C2I C2J C2K 0.0 . . . . ? C2I C2J C2K C2L 0.0 . . . . ? C2J C2K C2L C2G 0.0 . . . . ? C2H C2G C2L C2K 0.0 . . . . ? P1 C2G C2L C2K -177.62(17) . . . . ? P2 Ag O21 C23 27.9(3) . . . . ? P1 Ag O21 C23 -147.1(2) . . . . ? Ag O21 C23 O22 -6.3(5) . . . . ? Ag O21 C23 C24 174.9(2) . . . . ? O22 C23 C24 F25A -174.4(7) . . . . ? O21 C23 C24 F25A 4.5(8) . . . . ? O22 C23 C24 F27B -123.6(13) . . . . ? O21 C23 C24 F27B 55.3(14) . . . . ? O22 C23 C24 F25B 23(3) . . . . ? O21 C23 C24 F25B -158(3) . . . . ? O22 C23 C24 F27A 66.0(5) . . . . ? O21 C23 C24 F27A -115.0(4) . . . . ? O22 C23 C24 F26A -50.1(6) . . . . ? O21 C23 C24 F26A 128.9(5) . . . . ? O22 C23 C24 F26B 140.4(13) . . . . ? O21 C23 C24 F26B -40.6(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.094 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.071