# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1258 data_global _audit_creation_method 'manual editing of cif files' # SUBMISSION DETAILS _publ_contact_author_name 'Dr L\'aszl\'o P\'ark'anyi' _publ_contact_author_address ; Institute of Chemistry Chemical Research Center of the Hungarian Academy of Sciences H-1525-Budapest, P.O.Box 17, Hungary ; _publ_contact_author_email parka@cric.chemres.hu _publ_contact_author_fax '(36-1)-325-7554' _publ_contact_author_phone '(36-1)-325-7547' _publ_contact_letter ; Please consider this CIF submission for publication in J.Chem.Soc. Dalton Transactions. ; _publ_requested_journal 'J.Chem.Soc. Dalton Transactions' # TITLE AND AUTHOR LIST _publ_section_title ; Arylsulfonylnitrene and arylsulfonyl azide complexes of palladium ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'I. Foch' ; Institute of Chemistry Chemical Research Center of the Hungarian Academy of Sciences H-1525-Budapest, P.O.Box 17, Hungary ; 'L. P\'ark\'anyi' . ; Institute of Chemistry, Chemical Research Center of the Hungarian Academy of Sciences, H-1525 Budapest, P.O.Box 17, Hungary ; 'G. Besenyei' ; Institute of Chemistry, Chemical Research Center of the Hungarian Academy of Sciences, H-1525 Budapest, P.O.Box 17, Hungary ; 'L.I. Sim\'andi' ; Institute of Chemistry, Chemical Research Center of the Hungarian Academy of Sciences, H-1525 Budapest, P.O.Box 17, Hungary ; 'Alajos K\'alm\'an' . ; Institute of Chemistry, Chemical Research Center of the Hungarian Academy of Sciences, H-1525 Budapest, P.O.Box 17, Hungary ; # end of global data (Submission details) ============================= # Marked as 3d in paper data_pdono2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H49 Cl5 N2 O4 P4 Pd2 S' _chemical_formula_weight 1371.97 _chemical_melting_point ? _chemical_compound_source 'G.Besenyei (KKKI)' 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' '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' '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.827(1) _cell_length_b 19.622(1) _cell_length_c 23.149(6) _cell_angle_alpha 90.000 _cell_angle_beta 98.74(2) _cell_angle_gamma 90.000 _cell_volume 5758.7(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 15.49 _cell_measurement_theta_max 15.92 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.582 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 1.051 _exptl_absorpt_correction_type 'Empirical (Psi-scan)' _exptl_absorpt_correction_T_min 0.8451 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MOka _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'enraf nonius cad4' _diffrn_measurement_method omega-theta-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3 _diffrn_reflns_number 16992 _diffrn_reflns_av_R_equivalents 0.0182 _diffrn_reflns_av_sigmaI/netI 0.1228 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 29.46 _reflns_number_total 15932 _reflns_number_gt 7997 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms,1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15932 _refine_ls_number_parameters 755 _refine_ls_number_restraints 82 _refine_ls_R_factor_all 0.1618 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1201 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 1.036 _refine_ls_shift/su_mean 0.041 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.03309(2) 0.203351(15) 0.229403(14) 0.03148(8) Uani 1 d . . . Pd2 Pd -0.06091(2) 0.054012(15) 0.259153(15) 0.03273(8) Uani 1 d . . . Cl1 Cl 0.11376(9) 0.30267(5) 0.26734(6) 0.0515(3) Uani 1 d . . . Cl2 Cl -0.09829(10) -0.02401(6) 0.32766(6) 0.0568(3) Uani 1 d . . . S1 S -0.08829(8) 0.10826(5) 0.13035(5) 0.0371(2) Uani 1 d . . . P1 P -0.13272(8) 0.25237(5) 0.22692(5) 0.0328(2) Uani 1 d . . . P2 P 0.19633(8) 0.14861(5) 0.24007(5) 0.0325(2) Uani 1 d . . . P3 P -0.21566(8) 0.11212(5) 0.26897(5) 0.0348(2) Uani 1 d . . . P4 P 0.10071(8) 0.00361(5) 0.25414(5) 0.0334(2) Uani 1 d . . . O1 O -0.1527(3) 0.04757(17) 0.12415(14) 0.0551(9) Uani 1 d . . . O2 O -0.1395(2) 0.16904(16) 0.10457(13) 0.0495(8) Uani 1 d . . . O3 O -0.039(3) 0.227(3) 0.0148(15) 0.193(19) Uani 0.38(6) d PD . . O3' O -0.004(3) 0.2396(15) 0.0073(7) 0.078(13) Uani 0.36(7) d PDU . . O3" O 0.026(4) 0.2567(16) 0.0155(14) 0.069(9) Uani 0.26(3) d PDU . . O4 O 0.0629(4) 0.2383(2) 0.1021(2) 0.0900(14) Uani 1 d . . . N1 N -0.0317(2) 0.11645(16) 0.19361(14) 0.0319(7) Uani 1 d . . . N2 N 0.0341(5) 0.2126(3) 0.0539(3) 0.0749(15) Uani 1 d D . . C1 C -0.2407(3) 0.1899(2) 0.22489(19) 0.0361(9) Uani 1 d . . . H1A H -0.3005 0.2130 0.2371 0.047 Uiso 1 calc R . . H1B H -0.2616 0.1762 0.1845 0.047 Uiso 1 calc R . . C2 C 0.1894(3) 0.05877(19) 0.21913(19) 0.0348(9) Uani 1 d . . . H2A H 0.2600 0.0399 0.2274 0.045 Uiso 1 calc R . . H2B H 0.1677 0.0563 0.1772 0.045 Uiso 1 calc R . . C3 C 0.0097(3) 0.0909(2) 0.08427(18) 0.0399(10) Uani 1 d . . . C4 C 0.0510(4) 0.1385(2) 0.0499(2) 0.0494(12) Uani 1 d . . . C5 C 0.1202(4) 0.1202(3) 0.0114(2) 0.0623(14) Uani 1 d . . . H5 H 0.1442 0.1529 -0.0125 0.081 Uiso 1 calc R . . C6 C 0.1523(4) 0.0541(3) 0.0088(3) 0.0691(16) Uani 1 d . . . H6 H 0.1996 0.0418 -0.0160 0.090 Uiso 1 calc R . . C7 C 0.1148(4) 0.0069(3) 0.0427(2) 0.0633(15) Uani 1 d . . . H7 H 0.1379 -0.0379 0.0417 0.082 Uiso 1 calc R . . C8 C 0.0416(4) 0.0243(2) 0.0795(2) 0.0495(12) Uani 1 d . . . H8 H 0.0142 -0.0096 0.1009 0.064 Uiso 1 calc R . . C1P C -0.1763(4) 0.3052(2) 0.1637(2) 0.0436(11) Uani 1 d . . . C2P C -0.1011(4) 0.3405(3) 0.1393(2) 0.0606(14) Uani 1 d . . . H2P H -0.0303 0.3358 0.1552 0.079 Uiso 1 calc R . . C3P C -0.1289(6) 0.3825(3) 0.0920(3) 0.083(2) Uani 1 d . . . H3P H -0.0771 0.4061 0.0761 0.108 Uiso 1 calc R . . C4P C -0.2317(7) 0.3895(3) 0.0685(2) 0.084(2) Uani 1 d . . . H4P H -0.2506 0.4184 0.0368 0.109 Uiso 1 calc R . . C5P C -0.3082(5) 0.3537(3) 0.0915(3) 0.0753(18) Uani 1 d . . . H5P H -0.3787 0.3579 0.0750 0.098 Uiso 1 calc R . . C6P C -0.2802(4) 0.3120(3) 0.1388(2) 0.0601(14) Uani 1 d . . . H6P H -0.3321 0.2880 0.1543 0.078 Uiso 1 calc R . . C7P C -0.1467(3) 0.3067(2) 0.2895(2) 0.0377(10) Uani 1 d . . . C8P C -0.2090(4) 0.3646(2) 0.2836(2) 0.0499(12) Uani 1 d . . . H8P H -0.2449 0.3769 0.2472 0.065 Uiso 1 calc R . . C9P C -0.2177(5) 0.4041(3) 0.3318(3) 0.0706(17) Uani 1 d . . . H9P H -0.2592 0.4432 0.3278 0.092 Uiso 1 calc R . . C10P C -0.1657(5) 0.3862(4) 0.3853(3) 0.083(2) Uani 1 d . . . H10P H -0.1723 0.4128 0.4178 0.108 Uiso 1 calc R . . C11P C -0.1040(5) 0.3295(3) 0.3913(3) 0.0740(17) Uani 1 d . . . H11P H -0.0694 0.3173 0.4281 0.096 Uiso 1 calc R . . C12P C -0.0921(4) 0.2900(3) 0.3437(2) 0.0551(13) Uani 1 d . . . H12P H -0.0477 0.2522 0.3480 0.072 Uiso 1 calc R . . C13P C 0.2710(3) 0.1473(2) 0.31341(19) 0.0390(10) Uani 1 d . . . C14P C 0.2290(4) 0.1749(2) 0.3602(2) 0.0507(12) Uani 1 d . . . H14P H 0.1634 0.1961 0.3540 0.066 Uiso 1 calc R . . C15P C 0.2861(5) 0.1706(3) 0.4163(2) 0.0699(16) Uani 1 d . . . H15P H 0.2583 0.1895 0.4475 0.091 Uiso 1 calc R . . C16P C 0.3817(5) 0.1390(3) 0.4263(3) 0.0717(17) Uani 1 d . . . H16P H 0.4190 0.1369 0.4639 0.093 Uiso 1 calc R . . C17P C 0.4232(4) 0.1102(3) 0.3803(3) 0.0683(16) Uani 1 d . . . H17P H 0.4875 0.0874 0.3870 0.089 Uiso 1 calc R . . C18P C 0.3687(3) 0.1153(3) 0.3241(2) 0.0524(12) Uani 1 d . . . H18P H 0.3978 0.0971 0.2930 0.068 Uiso 1 calc R . . C19P C 0.2880(3) 0.1840(2) 0.1948(2) 0.0402(10) Uani 1 d . . . C20P C 0.2964(4) 0.1584(3) 0.1403(2) 0.0687(16) Uani 1 d . . . H20P H 0.2587 0.1195 0.1271 0.089 Uiso 1 calc R . . C21P C 0.3594(5) 0.1892(4) 0.1052(3) 0.096(2) Uani 1 d . . . H21P H 0.3642 0.1715 0.0684 0.125 Uiso 1 calc R . . C22P C 0.4151(5) 0.2461(4) 0.1249(3) 0.087(2) Uani 1 d . . . H22P H 0.4578 0.2671 0.1011 0.113 Uiso 1 calc R . . C23P C 0.4095(5) 0.2724(3) 0.1779(3) 0.091(2) Uani 1 d . . . H23P H 0.4482 0.3110 0.1907 0.118 Uiso 1 calc R . . C24P C 0.3454(4) 0.2413(3) 0.2130(3) 0.0696(17) Uani 1 d . . . H24P H 0.3412 0.2595 0.2497 0.091 Uiso 1 calc R . . C25P C -0.3383(3) 0.0646(2) 0.2480(2) 0.0408(10) Uani 1 d . . . C26P C -0.3918(4) 0.0679(3) 0.1921(3) 0.0672(16) Uani 1 d . . . H26P H -0.3686 0.0971 0.1651 0.087 Uiso 1 calc R . . C27P C -0.4805(5) 0.0278(3) 0.1756(3) 0.0802(19) Uani 1 d . . . H27P H -0.5163 0.0304 0.1376 0.104 Uiso 1 calc R . . C28P C -0.5154(4) -0.0150(3) 0.2143(3) 0.0703(17) Uani 1 d . . . H28P H -0.5740 -0.0425 0.2028 0.091 Uiso 1 calc R . . C29P C -0.4641(4) -0.0176(3) 0.2702(3) 0.0724(18) Uani 1 d . . . H29P H -0.4895 -0.0458 0.2972 0.094 Uiso 1 calc R . . C30P C -0.3744(4) 0.0212(2) 0.2875(2) 0.0545(13) Uani 1 d . . . H30P H -0.3387 0.0179 0.3255 0.071 Uiso 1 calc R . . C31P C -0.2216(3) 0.1396(2) 0.34391(19) 0.0416(10) Uani 1 d . . . C32P C -0.3112(4) 0.1711(2) 0.3584(2) 0.0532(12) Uani 1 d . . . H32P H -0.3694 0.1780 0.3298 0.069 Uiso 1 calc R . . C33P C -0.3146(5) 0.1924(3) 0.4152(2) 0.0644(15) Uani 1 d . . . H33P H -0.3749 0.2131 0.4248 0.084 Uiso 1 calc R . . C34P C -0.2290(6) 0.1826(3) 0.4566(3) 0.0801(19) Uani 1 d . . . H34P H -0.2308 0.1968 0.4948 0.104 Uiso 1 calc R . . C35P C -0.1396(6) 0.1521(3) 0.4428(3) 0.0818(19) Uani 1 d . . . H35P H -0.0817 0.1459 0.4717 0.106 Uiso 1 calc R . . C36P C -0.1349(4) 0.1309(3) 0.3872(2) 0.0619(14) Uani 1 d . . . H36P H -0.0739 0.1105 0.3783 0.080 Uiso 1 calc R . . C37P C 0.0858(3) -0.0712(2) 0.20710(19) 0.0382(10) Uani 1 d . . . C38P C 0.1621(4) -0.0948(2) 0.1767(2) 0.0521(12) Uani 1 d . . . H38P H 0.2263 -0.0721 0.1798 0.068 Uiso 1 calc R . . C39P C 0.1450(5) -0.1523(3) 0.1414(2) 0.0658(15) Uani 1 d . . . H39P H 0.1983 -0.1687 0.1220 0.086 Uiso 1 calc R . . C40P C 0.0502(5) -0.1843(3) 0.1355(3) 0.0787(19) Uani 1 d . . . H40P H 0.0377 -0.2221 0.1111 0.102 Uiso 1 calc R . . C41P C -0.0264(5) -0.1614(3) 0.1650(3) 0.081(2) Uani 1 d . . . H41P H -0.0910 -0.1838 0.1607 0.106 Uiso 1 calc R . . C42P C -0.0099(4) -0.1052(2) 0.2014(3) 0.0605(14) Uani 1 d . . . H42P H -0.0627 -0.0903 0.2218 0.079 Uiso 1 calc R . . C43P C 0.1790(3) -0.0263(2) 0.32190(19) 0.0395(10) Uani 1 d . . . C44P C 0.1645(4) 0.0018(3) 0.3746(2) 0.0565(13) Uani 1 d . . . H44P H 0.1139 0.0355 0.3757 0.073 Uiso 1 calc R . . C45P C 0.2244(5) -0.0197(3) 0.4254(2) 0.0738(17) Uani 1 d . . . H45P H 0.2156 0.0005 0.4606 0.096 Uiso 1 calc R . . C46P C 0.2973(5) -0.0708(3) 0.4249(3) 0.0756(18) Uani 1 d . . . H46P H 0.3369 -0.0855 0.4596 0.098 Uiso 1 calc R . . C47P C 0.3112(4) -0.0996(3) 0.3734(3) 0.0705(16) Uani 1 d . . . H47P H 0.3601 -0.1345 0.3728 0.092 Uiso 1 calc R . . C48P C 0.2531(4) -0.0772(3) 0.3222(2) 0.0574(14) Uani 1 d . . . H48P H 0.2640 -0.0968 0.2870 0.075 Uiso 1 calc R . . C1S C -0.3414(4) 0.1221(3) 0.0133(2) 0.117(3) Uani 1 d D . . H1S H -0.2717 0.1157 0.0345 0.163 Uiso 1 d R . . Cl1S Cl -0.4115(10) 0.0472(4) 0.0044(10) 0.158(7) Uani 0.34(2) d PDU . . Cl2S Cl -0.3591(9) 0.0755(12) -0.0503(7) 0.233(12) Uani 0.406(14) d PDU . . Cl3S Cl -0.3316(10) 0.1284(9) -0.0598(3) 0.157(7) Uani 0.320(18) d PDU . . Cl4S Cl -0.3295(9) 0.175(2) -0.0448(13) 0.38(3) Uani 0.29(2) d PDU . . Cl5S Cl -0.3490(19) 0.2054(6) -0.0101(13) 0.46(2) Uani 0.413(18) d PDU . . Cl6S Cl -0.3889(12) 0.2009(7) 0.0288(9) 0.117(8) Uani 0.25(2) d PDU . . Cl7S Cl -0.4225(10) 0.1669(12) 0.0523(3) 0.142(7) Uani 0.37(2) d PDU . . Cl8S Cl -0.4379(12) 0.131(3) 0.0568(6) 0.26(3) Uiso 0.181(16) d PD . . Cl9S Cl -0.4318(10) 0.0657(11) 0.0334(8) 0.265(13) Uani 0.43(2) d PDU . . 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 0.02769(15) 0.02352(14) 0.04369(19) -0.00022(14) 0.00685(13) -0.00139(12) Pd2 0.03011(16) 0.02430(15) 0.04486(19) 0.00378(14) 0.00917(13) 0.00046(13) Cl1 0.0436(6) 0.0306(5) 0.0799(9) -0.0091(6) 0.0081(6) -0.0096(5) Cl2 0.0580(8) 0.0465(7) 0.0694(8) 0.0223(6) 0.0211(6) -0.0015(6) S1 0.0331(5) 0.0379(6) 0.0391(6) -0.0025(5) 0.0022(5) -0.0026(4) P1 0.0301(5) 0.0247(5) 0.0443(6) 0.0029(5) 0.0077(5) 0.0029(4) P2 0.0275(5) 0.0292(5) 0.0415(6) -0.0022(5) 0.0079(5) -0.0015(4) P3 0.0280(5) 0.0309(5) 0.0471(7) 0.0035(5) 0.0108(5) -0.0002(4) P4 0.0312(5) 0.0252(5) 0.0437(6) -0.0010(5) 0.0051(5) 0.0030(4) O1 0.0493(19) 0.054(2) 0.061(2) -0.0130(17) 0.0051(16) -0.0194(16) O2 0.0493(19) 0.0513(19) 0.0450(18) 0.0053(15) -0.0025(15) 0.0139(16) O3 0.37(5) 0.13(3) 0.096(15) 0.086(18) 0.12(3) 0.09(3) O3' 0.17(3) 0.027(15) 0.053(9) 0.029(10) 0.054(12) 0.002(14) O3" 0.109(18) 0.024(13) 0.076(15) 0.016(10) 0.015(12) -0.022(11) O4 0.090(3) 0.059(3) 0.125(4) -0.021(3) 0.029(3) -0.013(2) N1 0.0340(18) 0.0268(16) 0.0351(19) -0.0007(14) 0.0063(15) -0.0047(14) N2 0.101(4) 0.067(4) 0.066(4) 0.004(3) 0.043(3) 0.000(3) C1 0.028(2) 0.031(2) 0.049(3) 0.0004(19) 0.0072(19) 0.0003(16) C2 0.032(2) 0.029(2) 0.044(2) -0.0030(18) 0.0060(18) 0.0028(17) C3 0.050(3) 0.037(2) 0.032(2) -0.0070(19) 0.005(2) 0.003(2) C4 0.057(3) 0.046(3) 0.046(3) -0.003(2) 0.009(2) 0.005(2) C5 0.069(4) 0.073(4) 0.050(3) 0.000(3) 0.024(3) -0.004(3) C6 0.065(4) 0.083(4) 0.065(4) -0.010(3) 0.028(3) 0.007(3) C7 0.070(4) 0.060(3) 0.059(3) -0.016(3) 0.007(3) 0.019(3) C8 0.063(3) 0.043(3) 0.041(3) -0.004(2) 0.002(2) 0.003(2) C1P 0.055(3) 0.030(2) 0.047(3) 0.002(2) 0.011(2) 0.009(2) C2P 0.072(4) 0.053(3) 0.059(3) 0.013(3) 0.018(3) 0.007(3) C3P 0.116(6) 0.081(4) 0.057(4) 0.031(3) 0.028(4) 0.008(4) C4P 0.146(7) 0.064(4) 0.039(3) 0.016(3) 0.012(4) 0.036(4) C5P 0.090(5) 0.068(4) 0.062(4) 0.007(3) -0.007(3) 0.023(4) C6P 0.061(3) 0.055(3) 0.061(3) 0.011(3) 0.003(3) 0.015(3) C7P 0.031(2) 0.031(2) 0.053(3) -0.0044(19) 0.014(2) -0.0009(17) C8P 0.042(3) 0.041(3) 0.070(3) -0.006(2) 0.018(2) 0.002(2) C9P 0.063(4) 0.056(3) 0.097(5) -0.031(3) 0.029(4) 0.002(3) C10P 0.082(5) 0.089(5) 0.086(5) -0.051(4) 0.035(4) -0.015(4) C11P 0.083(4) 0.084(4) 0.055(4) -0.016(3) 0.010(3) -0.014(4) C12P 0.060(3) 0.053(3) 0.052(3) -0.004(2) 0.006(3) 0.001(3) C13P 0.039(2) 0.035(2) 0.042(3) -0.0023(19) 0.003(2) -0.0070(19) C14P 0.058(3) 0.050(3) 0.045(3) 0.004(2) 0.010(2) -0.002(2) C15P 0.108(5) 0.055(3) 0.049(3) -0.002(3) 0.019(3) -0.012(3) C16P 0.091(5) 0.063(4) 0.055(4) 0.006(3) -0.007(3) -0.020(3) C17P 0.052(3) 0.072(4) 0.072(4) 0.017(3) -0.019(3) -0.006(3) C18P 0.037(3) 0.059(3) 0.060(3) -0.004(3) 0.005(2) 0.001(2) C19P 0.029(2) 0.042(2) 0.052(3) 0.005(2) 0.011(2) 0.0030(18) C20P 0.065(4) 0.089(4) 0.053(3) -0.006(3) 0.012(3) -0.025(3) C21P 0.089(5) 0.132(6) 0.074(4) -0.011(4) 0.037(4) -0.052(5) C22P 0.071(4) 0.101(5) 0.098(5) 0.016(4) 0.040(4) -0.029(4) C23P 0.097(5) 0.063(4) 0.125(6) -0.012(4) 0.061(5) -0.038(4) C24P 0.074(4) 0.052(3) 0.091(4) -0.021(3) 0.039(3) -0.024(3) C25P 0.032(2) 0.028(2) 0.062(3) 0.003(2) 0.008(2) -0.0009(17) C26P 0.057(3) 0.065(4) 0.074(4) 0.007(3) -0.008(3) -0.026(3) C27P 0.061(4) 0.077(4) 0.097(5) 0.006(4) -0.005(3) -0.026(3) C28P 0.036(3) 0.049(3) 0.125(6) -0.004(3) 0.005(3) -0.004(2) C29P 0.048(3) 0.044(3) 0.132(6) 0.013(3) 0.034(4) -0.007(3) C30P 0.044(3) 0.044(3) 0.077(4) 0.012(3) 0.014(3) -0.001(2) C31P 0.046(3) 0.036(2) 0.045(3) 0.004(2) 0.014(2) 0.002(2) C32P 0.055(3) 0.048(3) 0.058(3) 0.001(2) 0.016(3) 0.006(2) C33P 0.079(4) 0.058(3) 0.062(4) -0.003(3) 0.029(3) 0.012(3) C34P 0.126(6) 0.063(4) 0.055(4) -0.009(3) 0.026(4) 0.006(4) C35P 0.106(5) 0.079(4) 0.054(4) -0.005(3) -0.009(3) 0.018(4) C36P 0.062(3) 0.064(4) 0.058(3) -0.004(3) 0.005(3) 0.011(3) C37P 0.037(2) 0.024(2) 0.051(3) -0.0019(18) -0.001(2) 0.0038(17) C38P 0.054(3) 0.037(3) 0.065(3) -0.006(2) 0.006(3) 0.009(2) C39P 0.075(4) 0.051(3) 0.071(4) -0.018(3) 0.010(3) 0.021(3) C40P 0.077(4) 0.050(3) 0.104(5) -0.034(3) -0.004(4) 0.010(3) C41P 0.062(4) 0.052(3) 0.127(6) -0.033(4) 0.003(4) -0.006(3) C42P 0.053(3) 0.037(3) 0.089(4) -0.009(3) 0.003(3) -0.003(2) C43P 0.035(2) 0.036(2) 0.046(3) 0.004(2) 0.002(2) 0.0004(18) C44P 0.065(3) 0.052(3) 0.053(3) -0.005(2) 0.008(3) 0.006(3) C45P 0.099(5) 0.073(4) 0.046(3) -0.005(3) -0.002(3) 0.002(4) C46P 0.076(4) 0.078(4) 0.066(4) 0.024(3) -0.012(3) -0.001(3) C47P 0.066(4) 0.062(4) 0.079(4) 0.019(3) -0.004(3) 0.023(3) C48P 0.055(3) 0.058(3) 0.058(3) 0.003(3) 0.006(3) 0.023(3) C1S 0.073(5) 0.157(9) 0.116(7) -0.006(6) 0.001(5) -0.003(5) Cl1S 0.183(11) 0.139(9) 0.148(13) 0.034(8) 0.014(9) 0.010(7) Cl2S 0.114(7) 0.29(2) 0.27(2) -0.167(17) -0.033(9) 0.060(10) Cl3S 0.181(12) 0.143(11) 0.184(11) 0.027(8) 0.141(10) 0.053(8) Cl4S 0.40(3) 0.36(4) 0.47(4) 0.09(3) 0.34(3) -0.05(3) Cl5S 0.63(4) 0.33(2) 0.35(3) -0.006(19) -0.20(3) -0.27(3) Cl6S 0.154(10) 0.111(10) 0.081(11) -0.040(7) 0.003(7) 0.029(8) Cl7S 0.163(8) 0.200(15) 0.062(5) 0.011(6) 0.013(4) 0.083(9) Cl9S 0.314(17) 0.35(3) 0.140(10) 0.055(12) 0.074(9) -0.069(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 Pd1 N1 2.019(3) . y Pd1 Cl1 2.3160(11) . y Pd1 P1 2.3270(11) . y Pd1 P2 2.3328(11) . y Pd1 Pd2 3.2814(5) . y Pd2 N1 2.029(3) . y Pd2 Cl2 2.3064(12) . y Pd2 P4 2.3157(11) . y Pd2 P3 2.3300(11) . y S1 O1 1.444(3) . y S1 O2 1.446(3) . y S1 N1 1.541(3) . y S1 C3 1.801(4) . y P1 C1P 1.811(4) . y P1 C7P 1.830(4) . y P1 C1 1.845(4) . y P2 C13P 1.818(4) . y P2 C2 1.827(4) . y P2 C19P 1.828(4) . y P3 C31P 1.829(5) . y P3 C25P 1.830(4) . y P3 C1 1.836(4) . y P4 C37P 1.820(4) . y P4 C43P 1.826(4) . y P4 C2 1.844(4) . y O3 O3" 1.02(6) . ? O3 N2 1.235(2) . y O3' N2 1.235(2) . y O3" N2 1.235(2) . y O4 N2 1.229(6) . y N2 C4 1.475(7) . y C3 C8 1.379(6) . y C3 C4 1.383(6) . y C4 C5 1.398(7) . y C5 C6 1.363(8) . y C6 C7 1.349(8) . y C7 C8 1.401(7) . y C1P C6P 1.376(7) . ? C1P C2P 1.376(7) . ? C2P C3P 1.374(7) . ? C3P C4P 1.356(9) . ? C4P C5P 1.377(9) . ? C5P C6P 1.371(7) . ? C7P C12P 1.380(6) . ? C7P C8P 1.383(6) . ? C8P C9P 1.375(7) . ? C9P C10P 1.360(9) . ? C10P C11P 1.361(9) . ? C11P C12P 1.375(7) . ? C13P C18P 1.389(6) . ? C13P C14P 1.390(6) . ? C14P C15P 1.393(7) . ? C15P C16P 1.363(8) . ? C16P C17P 1.381(8) . ? C17P C18P 1.384(7) . ? C19P C24P 1.375(6) . ? C19P C20P 1.378(7) . ? C20P C21P 1.370(7) . ? C21P C22P 1.366(9) . ? C22P C23P 1.342(9) . ? C23P C24P 1.383(7) . ? C25P C26P 1.370(7) . ? C25P C30P 1.380(6) . ? C26P C27P 1.387(7) . ? C27P C28P 1.353(8) . ? C28P C29P 1.361(8) . ? C29P C30P 1.386(7) . ? C31P C36P 1.389(6) . ? C31P C32P 1.391(6) . ? C32P C33P 1.386(7) . ? C33P C34P 1.357(8) . ? C34P C35P 1.373(8) . ? C35P C36P 1.363(8) . ? C37P C38P 1.369(6) . ? C37P C42P 1.386(6) . ? C38P C39P 1.390(7) . ? C39P C40P 1.358(8) . ? C40P C41P 1.357(8) . ? C41P C42P 1.384(7) . ? C43P C44P 1.377(6) . ? C43P C48P 1.378(6) . ? C44P C45P 1.370(7) . ? C45P C46P 1.371(8) . ? C46P C47P 1.354(8) . ? C47P C48P 1.373(7) . ? C1S Cl9S 1.719(2) . ? C1S Cl7S 1.719(2) . ? C1S Cl3S 1.718(2) . ? C1S Cl6S 1.719(2) . ? C1S Cl2S 1.719(2) . ? C1S Cl4S 1.720(2) . ? C1S Cl8S 1.720(4) . ? C1S Cl1S 1.720(2) . ? C1S Cl5S 1.720(2) . ? #Cl1S Cl9S 0.839(19) . ? #Cl1S Cl2S 1.62(3) . ? #Cl1S Cl8S 2.10(5) . ? #Cl2S Cl3S 1.13(2) . ? #Cl2S Cl4S 1.99(4) . ? #Cl2S Cl9S 2.28(3) . ? #Cl3S Cl4S 0.97(4) . ? #Cl3S Cl5S 1.93(4) . ? #Cl4S Cl5S 1.06(6) . ? #Cl4S Cl6S 2.03(5) . ? #Cl5S Cl6S 1.10(4) . ? #Cl5S Cl7S 1.99(4) . ? #Cl6S Cl7S 1.000(19) . ? #Cl6S Cl8S 1.68(6) . ? #Cl7S Cl8S 0.74(6) . ? #Cl7S Cl9S 2.03(3) . ? #Cl8S Cl9S 1.40(6) . ? 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 Cl1 177.11(10) . . y N1 Pd1 P1 91.22(9) . . y Cl1 Pd1 P1 90.89(4) . . y N1 Pd1 P2 87.79(9) . . y Cl1 Pd1 P2 90.30(4) . . y P1 Pd1 P2 174.42(4) . . y N1 Pd1 Pd2 35.94(9) . . y Cl1 Pd1 Pd2 146.01(4) . . y P1 Pd1 Pd2 90.61(3) . . y P2 Pd1 Pd2 85.36(3) . . y N1 Pd2 Cl2 175.09(10) . . y N1 Pd2 P4 87.25(10) . . y Cl2 Pd2 P4 91.84(4) . . y N1 Pd2 P3 91.97(10) . . y Cl2 Pd2 P3 89.34(4) . . y P4 Pd2 P3 175.08(4) . . y N1 Pd2 Pd1 35.73(9) . . y Cl2 Pd2 Pd1 149.15(4) . . y P4 Pd2 Pd1 90.61(3) . . y P3 Pd2 Pd1 85.94(3) . . y O1 S1 O2 114.99(19) . . y O1 S1 N1 111.11(19) . . y O2 S1 N1 115.16(18) . . y O1 S1 C3 103.0(2) . . y O2 S1 C3 103.1(2) . . y N1 S1 C3 108.20(19) . . y C1P P1 C7P 104.5(2) . . y C1P P1 C1 102.8(2) . . y C7P P1 C1 104.14(19) . . y C1P P1 Pd1 115.15(16) . . y C7P P1 Pd1 114.88(14) . . y C1 P1 Pd1 113.91(13) . . ? C13P P2 C2 103.4(2) . . y C13P P2 C19P 104.3(2) . . y C2 P2 C19P 102.98(19) . . y C13P P2 Pd1 116.25(15) . . y C2 P2 Pd1 114.16(14) . . y C19P P2 Pd1 114.16(14) . . y C31P P3 C25P 104.2(2) . . y C31P P3 C1 104.7(2) . . y C25P P3 C1 101.83(19) . . y C31P P3 Pd2 113.30(15) . . y C25P P3 Pd2 115.82(14) . . y C1 P3 Pd2 115.57(14) . . y C37P P4 C43P 104.42(19) . . y C37P P4 C2 103.05(19) . . y C43P P4 C2 105.71(19) . . y C37P P4 Pd2 111.17(14) . . y C43P P4 Pd2 118.28(15) . . y C2 P4 Pd2 112.82(13) . . y #O3" O3 N2 65.5(16) . . ? #O3 O3" N2 65.5(15) . . ? S1 N1 Pd1 125.67(19) . . y S1 N1 Pd2 122.27(18) . . y Pd1 N1 Pd2 108.33(15) . . y #O3' N2 O3" 24.6(16) . . ? #O3' N2 O3 27(3) . . ? #O3" N2 O3 49(3) . . ? O3' N2 O4 129.9(16) . . y O3" N2 O4 110.3(19) . . y O3 N2 O4 132(2) . . y O3' N2 C4 114.3(16) . . y O3" N2 C4 130(2) . . y O3 N2 C4 106(2) . . y O4 N2 C4 115.8(5) . . y P3 C1 P1 118.1(2) . . y P2 C2 P4 117.3(2) . . y C8 C3 C4 116.7(4) . . y C8 C3 S1 118.0(4) . . y C4 C3 S1 125.1(3) . . y C3 C4 C5 121.9(5) . . y C3 C4 N2 123.9(4) . . y C5 C4 N2 114.0(5) . . y C6 C5 C4 119.8(5) . . y C7 C6 C5 119.4(5) . . y C6 C7 C8 121.1(5) . . y C3 C8 C7 120.9(5) . . y C6P C1P C2P 118.3(5) . . ? C6P C1P P1 123.7(4) . . ? C2P C1P P1 118.0(4) . . ? C3P C2P C1P 121.0(6) . . ? C4P C3P C2P 120.0(6) . . ? C3P C4P C5P 120.0(5) . . ? C6P C5P C4P 119.8(6) . . ? C5P C6P C1P 120.8(6) . . ? C12P C7P C8P 119.4(4) . . ? C12P C7P P1 118.9(3) . . ? C8P C7P P1 121.7(4) . . ? C9P C8P C7P 120.0(5) . . ? C10P C9P C8P 120.2(6) . . ? C11P C10P C9P 120.1(5) . . ? C10P C11P C12P 120.8(6) . . ? C11P C12P C7P 119.4(5) . . ? C18P C13P C14P 118.9(4) . . ? C18P C13P P2 120.3(4) . . ? C14P C13P P2 120.7(3) . . ? C15P C14P C13P 119.5(5) . . ? C16P C15P C14P 121.2(6) . . ? C15P C16P C17P 119.8(5) . . ? C16P C17P C18P 119.7(5) . . ? C17P C18P C13P 120.8(5) . . ? C24P C19P C20P 117.9(4) . . ? C24P C19P P2 119.7(4) . . ? C20P C19P P2 122.2(4) . . ? C21P C20P C19P 121.1(6) . . ? C20P C21P C22P 119.3(6) . . ? C23P C22P C21P 121.4(6) . . ? C22P C23P C24P 119.2(6) . . ? C19P C24P C23P 121.2(5) . . ? C26P C25P C30P 118.9(4) . . ? C26P C25P P3 121.0(4) . . ? C30P C25P P3 120.0(4) . . ? C25P C26P C27P 120.4(5) . . ? C28P C27P C26P 120.6(6) . . ? C27P C28P C29P 119.4(5) . . ? C28P C29P C30P 120.9(5) . . ? C25P C30P C29P 119.7(5) . . ? C36P C31P C32P 118.7(4) . . ? C36P C31P P3 120.3(4) . . ? C32P C31P P3 121.0(4) . . ? C33P C32P C31P 120.6(5) . . ? C34P C33P C32P 119.3(5) . . ? C33P C34P C35P 120.8(6) . . ? C36P C35P C34P 120.8(6) . . ? C35P C36P C31P 119.9(5) . . ? C38P C37P C42P 118.6(4) . . ? C38P C37P P4 124.2(3) . . ? C42P C37P P4 117.1(4) . . ? C37P C38P C39P 121.1(5) . . ? C40P C39P C38P 119.6(5) . . ? C41P C40P C39P 120.1(5) . . ? C40P C41P C42P 121.0(6) . . ? C41P C42P C37P 119.5(5) . . ? C44P C43P C48P 118.1(4) . . ? C44P C43P P4 120.1(4) . . ? C48P C43P P4 121.8(4) . . ? C45P C44P C43P 120.2(5) . . ? C46P C45P C44P 120.9(6) . . ? C47P C46P C45P 119.5(5) . . ? C46P C47P C48P 119.9(5) . . ? C47P C48P C43P 121.3(5) . . ? Cl9S C1S Cl7S 72.5(13) . . ? Cl9S C1S Cl3S 117.8(10) . . ? Cl7S C1S Cl3S 128.4(6) . . ? Cl9S C1S Cl6S 104.3(13) . . ? Cl7S C1S Cl6S 33.8(6) . . ? Cl3S C1S Cl6S 102.9(10) . . ? Cl9S C1S Cl2S 83.2(12) . . ? Cl7S C1S Cl2S 135.2(6) . . ? Cl3S C1S Cl2S 38.3(8) . . ? Cl6S C1S Cl2S 130.8(9) . . ? Cl9S C1S Cl4S 137.9(9) . . ? Cl7S C1S Cl4S 103.7(17) . . ? Cl3S C1S Cl4S 32.9(15) . . ? Cl6S C1S Cl4S 73(2) . . ? Cl2S C1S Cl4S 70.6(18) . . ? Cl9S C1S Cl8S 48(2) . . ? Cl7S C1S Cl8S 25(2) . . ? Cl3S C1S Cl8S 137.4(7) . . ? Cl6S C1S Cl8S 58(2) . . ? Cl2S C1S Cl8S 122.9(17) . . ? Cl4S C1S Cl8S 123.6(18) . . ? Cl9S C1S Cl1S 28.3(7) . . ? Cl7S C1S Cl1S 98.7(12) . . ? Cl3S C1S Cl1S 93.4(11) . . ? Cl6S C1S Cl1S 126.7(10) . . ? Cl2S C1S Cl1S 56.2(11) . . ? Cl4S C1S Cl1S 121.8(17) . . ? Cl8S C1S Cl1S 75(2) . . ? Cl9S C1S Cl5S 133.5(12) . . ? Cl7S C1S Cl5S 70.7(15) . . ? Cl3S C1S Cl5S 68.4(14) . . ? Cl6S C1S Cl5S 37.5(15) . . ? Cl2S C1S Cl5S 104.1(15) . . ? Cl4S C1S Cl5S 36(2) . . ? Cl8S C1S Cl5S 94(3) . . ? Cl1S C1S Cl5S 140.5(6) . . ? Cl9S Cl1S Cl2S 133.9(9) . . ? Cl9S Cl1S C1S 75.8(4) . . ? Cl2S Cl1S C1S 61.9(5) . . ? Cl9S Cl1S Cl8S 26.1(11) . . ? Cl2S Cl1S Cl8S 107.8(13) . . ? C1S Cl1S Cl8S 52.3(11) . . ? Cl3S Cl2S Cl1S 130.2(6) . . ? Cl3S Cl2S C1S 70.8(4) . . ? Cl1S Cl2S C1S 61.9(5) . . ? Cl3S Cl2S Cl4S 17.7(9) . . ? Cl1S Cl2S Cl4S 112.6(12) . . ? C1S Cl2S Cl4S 54.7(9) . . ? Cl3S Cl2S Cl9S 114.9(7) . . ? Cl1S Cl2S Cl9S 15.4(4) . . ? C1S Cl2S Cl9S 48.4(6) . . ? Cl4S Cl2S Cl9S 97.2(12) . . ? Cl4S Cl3S Cl2S 141.6(12) . . ? Cl4S Cl3S C1S 73.6(8) . . ? Cl2S Cl3S C1S 70.9(4) . . ? Cl4S Cl3S Cl5S 19.2(13) . . ? Cl2S Cl3S Cl5S 122.5(10) . . ? C1S Cl3S Cl5S 55.8(7) . . ? Cl5S Cl4S Cl3S 143.3(11) . . ? Cl5S Cl4S C1S 72.0(11) . . ? Cl3S Cl4S C1S 73.5(7) . . ? Cl5S Cl4S Cl6S 20.6(10) . . ? Cl3S Cl4S Cl6S 122.7(8) . . ? C1S Cl4S Cl6S 53.7(10) . . ? Cl5S Cl4S Cl2S 122.6(11) . . ? Cl3S Cl4S Cl2S 20.6(5) . . ? C1S Cl4S Cl2S 54.7(9) . . ? Cl6S Cl4S Cl2S 102.1(7) . . ? Cl4S Cl5S Cl6S 139.6(13) . . ? Cl4S Cl5S C1S 72.0(11) . . ? Cl6S Cl5S C1S 71.2(8) . . ? Cl4S Cl5S Cl3S 17.5(8) . . ? Cl6S Cl5S Cl3S 122.1(8) . . ? C1S Cl5S Cl3S 55.7(7) . . ? Cl4S Cl5S Cl7S 121.6(11) . . ? Cl6S Cl5S Cl7S 18.0(5) . . ? C1S Cl5S Cl7S 54.6(8) . . ? Cl3S Cl5S Cl7S 104.1(6) . . ? Cl7S Cl6S Cl5S 142.1(9) . . ? Cl7S Cl6S C1S 73.1(4) . . ? Cl5S Cl6S C1S 71.3(7) . . ? Cl7S Cl6S Cl8S 13.2(12) . . ? Cl5S Cl6S Cl8S 128.9(15) . . ? C1S Cl6S Cl8S 60.8(12) . . ? Cl7S Cl6S Cl4S 122.4(11) . . ? Cl5S Cl6S Cl4S 19.8(12) . . ? C1S Cl6S Cl4S 53.8(10) . . ? Cl8S Cl6S Cl4S 109.2(15) . . ? Cl8S Cl7S Cl6S 148.8(15) . . ? Cl8S Cl7S C1S 77.6(12) . . ? Cl6S Cl7S C1S 73.1(3) . . ? Cl8S Cl7S Cl9S 25.4(14) . . ? Cl6S Cl7S Cl9S 123.4(8) . . ? C1S Cl7S Cl9S 53.8(6) . . ? Cl8S Cl7S Cl5S 128.9(16) . . ? Cl6S Cl7S Cl5S 19.9(8) . . ? C1S Cl7S Cl5S 54.6(8) . . ? Cl9S Cl7S Cl5S 103.5(8) . . ? Cl7S Cl8S Cl9S 141.5(10) . . ? Cl7S Cl8S C1S 77.5(8) . . ? Cl9S Cl8S C1S 65.9(11) . . ? Cl7S Cl8S Cl6S 18.0(5) . . ? Cl9S Cl8S Cl6S 123.5(8) . . ? C1S Cl8S Cl6S 60.7(11) . . ? Cl7S Cl8S Cl1S 126.2(10) . . ? Cl9S Cl8S Cl1S 15.3(4) . . ? C1S Cl8S Cl1S 52.3(12) . . ? Cl6S Cl8S Cl1S 108.2(8) . . ? Cl1S Cl9S Cl8S 138.5(12) . . ? Cl1S Cl9S C1S 76.0(4) . . ? Cl8S Cl9S C1S 66.1(9) . . ? Cl1S Cl9S Cl7S 125.5(8) . . ? Cl8S Cl9S Cl7S 13.1(10) . . ? C1S Cl9S Cl7S 53.8(6) . . ? Cl1S Cl9S Cl2S 30.7(7) . . ? Cl8S Cl9S Cl2S 107.8(12) . . ? C1S Cl9S Cl2S 48.4(6) . . ? Cl7S Cl9S Cl2S 94.7(7) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 29.46 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.199 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.116 #=END # Marked as 3e in paper data_pd2naft _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C60.50 H51.50 Cl3.50 N O3.67 P4 Pd2 S' _chemical_formula_weight 1344.02 _chemical_melting_point ? _chemical_compound_source 'G.Besenyei KKKI' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 21.714(4) _cell_length_b 14.489(3) _cell_length_c 38.342(7) _cell_angle_alpha 90.000 _cell_angle_beta 90.390(10) _cell_angle_gamma 90.000 _cell_volume 12063(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.43 _cell_measurement_theta_max 12.95 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5427 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type 'semi-empirical (psi-scan)' _exptl_absorpt_correction_T_min 0.9759 _exptl_absorpt_correction_T_max 1.0000 _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 'Enraf-Nonius CAD4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -3 _diffrn_reflns_number 25644 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1835 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.81 _reflns_number_total 25644 _reflns_number_gt 10598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25644 _refine_ls_number_parameters 1407 _refine_ls_number_restraints 1703 _refine_ls_R_factor_all 0.1604 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1092 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 0.813 _refine_ls_restrained_S_all 0.795 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1_1 Pd 0.364921(17) 0.07058(3) 0.713388(10) 0.03777(10) Uani 1 d U . . Pd2_1 Pd 0.472007(17) -0.04639(3) 0.755287(10) 0.04112(11) Uani 1 d U . . Cl1_1 Cl 0.29882(6) 0.19719(9) 0.71503(4) 0.0588(4) Uani 1 d U . . Cl2_1 Cl 0.53065(6) -0.06298(11) 0.80594(4) 0.0635(4) Uani 1 d U . . S1_1 S 0.42344(6) -0.11207(10) 0.68159(4) 0.0474(3) Uani 1 d U . . P1_1 P 0.29008(6) -0.02825(9) 0.73500(3) 0.0354(3) Uani 1 d U . . P2_1 P 0.44809(6) 0.16137(10) 0.69414(4) 0.0456(4) Uani 1 d U . . P3_1 P 0.38900(6) -0.11610(9) 0.78240(3) 0.0387(3) Uani 1 d U . . P4_1 P 0.54933(6) 0.03146(11) 0.72639(4) 0.0497(4) Uani 1 d U . . O1_1 O 0.48082(19) -0.1610(3) 0.68251(12) 0.0856(14) Uani 1 d U . . O2_1 O 0.36955(17) -0.1706(3) 0.68072(9) 0.0628(11) Uani 1 d U . . N1_1 N 0.42422(17) -0.0361(3) 0.71028(10) 0.0392(10) Uani 1 d U . . C1_1 C 0.3221(2) -0.1330(3) 0.75440(12) 0.0331(11) Uani 1 d U . . H1A_1 H 0.2902 -0.1629 0.7679 0.043 Uiso 1 d R . . H1B_1 H 0.3334 -0.1748 0.7357 0.043 Uiso 1 d R . . C2_1 C 0.5203(2) 0.0967(4) 0.68905(14) 0.0485(14) Uani 1 d U . . H2A_1 H 0.5145 0.0536 0.6700 0.063 Uiso 1 d R . . H2B_1 H 0.5521 0.1398 0.6820 0.063 Uiso 1 d R . . C3_1 C 0.4203(3) -0.0528(4) 0.64160(14) 0.0671(18) Uani 1 d DU . . C4_1 C 0.3653(3) -0.0121(4) 0.63054(15) 0.085(2) Uani 1 d DU . . H4_1 H 0.3295 -0.0193 0.6449 0.110 Uiso 1 d R . . C5_1 C 0.3633(5) 0.0377(5) 0.59931(17) 0.137(4) Uani 1 d DU . . C6_1 C 0.3085(5) 0.0779(8) 0.5873(3) 0.221(6) Uani 1 d DU . . H6_1 H 0.2728 0.0707 0.6016 0.287 Uiso 1 d R . . C7_1 C 0.3062(7) 0.1273(11) 0.5559(3) 0.262(8) Uani 1 d DU . . H7_1 H 0.2678 0.1548 0.5490 0.341 Uiso 1 d R . . C8_1 C 0.3633(8) 0.1324(13) 0.5393(4) 0.232(8) Uani 1 d DU . . H8_1 H 0.3607 0.1672 0.5180 0.302 Uiso 1 d R . . C9_1 C 0.4216(8) 0.0969(10) 0.5471(3) 0.249(8) Uani 1 d DU . . H9_1 H 0.4574 0.1041 0.5328 0.323 Uiso 1 d R . . C10_1 C 0.4153(5) 0.0476(7) 0.5784(2) 0.161(5) Uani 1 d DU . . C11_1 C 0.4690(5) 0.0028(7) 0.5896(2) 0.143(4) Uani 1 d DU . . H11_1 H 0.5047 0.0100 0.5753 0.186 Uiso 1 d R . . C12_1 C 0.4729(3) -0.0470(5) 0.62079(17) 0.108(3) Uani 1 d DU . . H12_1 H 0.5112 -0.0745 0.6278 0.140 Uiso 1 d R . . C1P_1 C 0.2402(2) -0.0700(4) 0.70022(13) 0.0425(13) Uani 1 d U . . C2P_1 C 0.2157(3) -0.0063(4) 0.67765(15) 0.0642(17) Uani 1 d U . . H2P_1 H 0.2245 0.0582 0.6806 0.083 Uiso 1 d R . . C3P_1 C 0.1769(3) -0.0366(5) 0.64986(16) 0.078(2) Uani 1 d U . . H3P_1 H 0.1616 0.0067 0.6329 0.101 Uiso 1 d R . . C4P_1 C 0.1621(3) -0.1274(5) 0.64717(16) 0.0660(18) Uani 1 d U . . H4P_1 H 0.1353 -0.1480 0.6288 0.086 Uiso 1 d R . . C5P_1 C 0.1850(3) -0.1886(5) 0.67053(18) 0.077(2) Uani 1 d U . . H5P_1 H 0.1741 -0.2526 0.6685 0.100 Uiso 1 d R . . C6P_1 C 0.2234(2) -0.1611(4) 0.69714(14) 0.0538(15) Uani 1 d U . . H6P_1 H 0.2389 -0.2056 0.7135 0.070 Uiso 1 d R . . C7P_1 C 0.2356(2) 0.0122(3) 0.76727(12) 0.0373(12) Uani 1 d U . . C8P_1 C 0.1822(2) -0.0381(4) 0.77291(15) 0.0560(15) Uani 1 d U . . H8P_1 H 0.1743 -0.0925 0.7593 0.073 Uiso 1 d R . . C9P_1 C 0.1401(3) -0.0108(5) 0.79807(16) 0.0691(18) Uani 1 d U . . H9P_1 H 0.1042 -0.0475 0.8025 0.090 Uiso 1 d R . . C10P_1 C 0.1505(3) 0.0685(5) 0.81613(16) 0.0694(18) Uani 1 d U . . H10_1 H 0.1206 0.0892 0.8327 0.090 Uiso 1 d R . . C11P_1 C 0.2029(3) 0.1194(4) 0.81102(15) 0.0614(16) Uani 1 d U . . H11P_1 H 0.2103 0.1744 0.8244 0.080 Uiso 1 d R . . C12P_1 C 0.2450(2) 0.0905(3) 0.78668(13) 0.0452(13) Uani 1 d U . . H12P_1 H 0.2817 0.1262 0.7830 0.059 Uiso 1 d R . . C13P_1 C 0.4418(3) 0.2216(4) 0.65307(15) 0.0582(15) Uani 1 d U . . C14P_1 C 0.3902(4) 0.2700(6) 0.6461(2) 0.118(3) Uani 1 d U . . H14P_1 H 0.3560 0.2665 0.6617 0.153 Uiso 1 d R . . C15P_1 C 0.3859(5) 0.3264(8) 0.6163(3) 0.160(4) Uani 1 d U . . H15P_1 H 0.3501 0.3642 0.6127 0.208 Uiso 1 d R . . C16P_1 C 0.4309(5) 0.3266(7) 0.5925(3) 0.138(4) Uani 1 d U . . H16P_1 H 0.4273 0.3633 0.5718 0.180 Uiso 1 d R . . C17P_1 C 0.4807(4) 0.2781(7) 0.5987(2) 0.127(3) Uani 1 d U . . H17P_1 H 0.5129 0.2789 0.5817 0.166 Uiso 1 d R . . C18P_1 C 0.4873(3) 0.2229(6) 0.6281(2) 0.104(3) Uani 1 d U . . H18P_1 H 0.5239 0.1866 0.6312 0.136 Uiso 1 d R . . C19P_1 C 0.4688(3) 0.2540(4) 0.72321(17) 0.0567(15) Uani 1 d U . . C20P_1 C 0.5151(3) 0.3156(5) 0.7143(2) 0.089(2) Uani 1 d U . . H20P_1 H 0.5356 0.3094 0.6923 0.115 Uiso 1 d R . . C21P_1 C 0.5318(4) 0.3851(6) 0.7368(3) 0.108(3) Uani 1 d U . . H21P_1 H 0.5641 0.4268 0.7303 0.140 Uiso 1 d R . . C22P_1 C 0.5034(4) 0.3962(6) 0.7676(3) 0.104(3) Uani 1 d U . . H22P_1 H 0.5154 0.4456 0.7828 0.136 Uiso 1 d R . . C23P_1 C 0.4580(3) 0.3373(5) 0.7771(2) 0.097(3) Uani 1 d U . . H23P_1 H 0.4382 0.3454 0.7991 0.126 Uiso 1 d R . . C24P_1 C 0.4396(3) 0.2636(5) 0.75490(19) 0.078(2) Uani 1 d U . . H24P_1 H 0.4075 0.2218 0.7617 0.102 Uiso 1 d R . . C25P_1 C 0.4069(2) -0.2307(3) 0.79818(14) 0.0423(13) Uani 1 d U . . C26P_1 C 0.4025(3) -0.3073(4) 0.77676(17) 0.0712(19) Uani 1 d U . . H26P_1 H 0.3856 -0.3011 0.7537 0.093 Uiso 1 d R . . C27P_1 C 0.4216(3) -0.3934(5) 0.7886(2) 0.096(3) Uani 1 d U . . H27P_1 H 0.4183 -0.4459 0.7734 0.124 Uiso 1 d R . . C28P_1 C 0.4452(3) -0.4037(5) 0.8208(2) 0.084(2) Uani 1 d U . . H28P_1 H 0.4572 -0.4637 0.8290 0.109 Uiso 1 d R . . C29P_1 C 0.4516(3) -0.3281(5) 0.84213(17) 0.0725(19) Uani 1 d U . . H29P_1 H 0.4696 -0.3347 0.8649 0.094 Uiso 1 d R . . C30P_1 C 0.4327(3) -0.2427(4) 0.83088(15) 0.0600(16) Uani 1 d U . . H30P_1 H 0.4372 -0.1903 0.8460 0.078 Uiso 1 d R . . C31P_1 C 0.3609(2) -0.0530(4) 0.82014(12) 0.0420(13) Uani 1 d U . . C32P_1 C 0.3104(3) -0.0861(5) 0.83819(15) 0.0639(17) Uani 1 d U . . H32P_1 H 0.2910 -0.1427 0.8312 0.083 Uiso 1 d R . . C33P_1 C 0.2874(3) -0.0368(6) 0.86635(19) 0.093(2) Uani 1 d U . . H33P_1 H 0.2526 -0.0599 0.8790 0.120 Uiso 1 d R . . C34P_1 C 0.3144(4) 0.0432(7) 0.8762(2) 0.092(3) Uani 1 d U . . H34P_1 H 0.2982 0.0774 0.8955 0.120 Uiso 1 d R . . C35P_1 C 0.3644(4) 0.0765(5) 0.85895(18) 0.083(2) Uani 1 d U . . H35P_1 H 0.3834 0.1332 0.8664 0.107 Uiso 1 d R . . C36P_1 C 0.3880(3) 0.0286(4) 0.83065(14) 0.0546(15) Uani 1 d U . . H36P_1 H 0.4230 0.0523 0.8184 0.071 Uiso 1 d R . . C37P_1 C 0.5943(3) 0.1182(4) 0.74926(17) 0.0573(16) Uani 1 d U . . C38P_1 C 0.6468(3) 0.1564(5) 0.7338(2) 0.089(2) Uani 1 d U . . H38P_1 H 0.6617 0.1315 0.7122 0.116 Uiso 1 d R . . C39P_1 C 0.6778(4) 0.2278(6) 0.7491(3) 0.119(3) Uani 1 d U . . H39P_1 H 0.7129 0.2554 0.7381 0.154 Uiso 1 d R . . C40P_1 C 0.6573(4) 0.2609(6) 0.7806(3) 0.112(3) Uani 1 d U . . H40P_1 H 0.6795 0.3098 0.7920 0.145 Uiso 1 d R . . C41P_1 C 0.6058(4) 0.2259(5) 0.7963(2) 0.095(2) Uani 1 d U . . H41P_1 H 0.5910 0.2512 0.8178 0.123 Uiso 1 d R . . C42P_1 C 0.5751(3) 0.1525(5) 0.78052(18) 0.0723(19) Uani 1 d U . . H42P_1 H 0.5399 0.1257 0.7917 0.094 Uiso 1 d R . . C43P_1 C 0.6060(2) -0.0460(4) 0.70779(16) 0.0568(15) Uani 1 d U . . C44P_1 C 0.6233(3) -0.1210(5) 0.72732(16) 0.0669(18) Uani 1 d U . . H44P_1 H 0.6052 -0.1310 0.7498 0.087 Uiso 1 d R . . C45P_1 C 0.6670(3) -0.1824(5) 0.7148(2) 0.091(2) Uani 1 d U . . H45P_1 H 0.6784 -0.2357 0.7283 0.118 Uiso 1 d R . . C46P_1 C 0.6940(3) -0.1674(6) 0.6829(2) 0.083(2) Uani 1 d U . . H46P_1 H 0.7249 -0.2089 0.6745 0.108 Uiso 1 d R . . C47P_1 C 0.6765(3) -0.0932(6) 0.66331(19) 0.080(2) Uani 1 d U . . H47P_1 H 0.6946 -0.0834 0.6408 0.104 Uiso 1 d R . . C48P_1 C 0.6333(3) -0.0324(5) 0.67581(17) 0.0690(18) Uani 1 d U . . H48P_1 H 0.6219 0.0202 0.6620 0.090 Uiso 1 d R . . Pd1_2 Pd 0.759579(19) 0.16905(3) 0.590065(11) 0.04828(12) Uani 1 d U . . Pd2_2 Pd 0.83786(2) 0.28907(3) 0.534882(10) 0.04606(12) Uani 1 d U . . Cl1_2 Cl 0.66407(7) 0.15470(13) 0.61754(4) 0.0779(5) Uani 1 d U . . Cl2_2 Cl 0.83717(9) 0.42110(11) 0.50075(4) 0.0824(5) Uani 1 d U . . P1_2 P 0.80460(7) 0.25128(10) 0.63604(4) 0.0453(4) Uani 1 d U . . P2_2 P 0.71783(7) 0.09939(11) 0.54047(4) 0.0572(4) Uani 1 d U . . P3_2 P 0.87118(7) 0.37474(10) 0.58230(4) 0.0457(4) Uani 1 d U . . P4_2 P 0.80519(7) 0.19674(11) 0.48876(4) 0.0505(4) Uani 1 d U . . N1_2 N 0.83946(18) 0.1731(3) 0.56407(10) 0.0439(11) Uani 1 d U . . S1_2 S 0.89959(7) 0.12151(10) 0.57522(4) 0.0514(4) Uani 1 d U . . O1_2 O 0.95074(18) 0.1580(3) 0.55683(13) 0.0901(15) Uani 1 d U . . O2_2 O 0.9070(2) 0.1132(3) 0.61271(10) 0.0801(13) Uani 1 d U . . C1_2 C 0.8741(2) 0.3137(3) 0.62386(12) 0.0434(13) Uani 1 d U . . H1A_2 H 0.8834 0.3582 0.6421 0.056 Uiso 1 calc R . . H1B_2 H 0.9080 0.2701 0.6232 0.056 Uiso 1 calc R . . C2_2 C 0.7709(3) 0.0883(4) 0.50448(14) 0.0569(16) Uani 1 d U . . H2A_2 H 0.7494 0.0592 0.4851 0.074 Uiso 1 calc R . . H2B_2 H 0.8040 0.0472 0.5116 0.074 Uiso 1 calc R . . C3_2 C 0.8923(3) 0.0030(5) 0.56271(18) 0.0665(18) Uani 1 d U . . C4_2 C 0.8620(4) -0.0564(5) 0.5868(2) 0.101(3) Uani 1 d U . . H4_2 H 0.8468 -0.0317 0.6084 0.131 Uiso 1 d R . . C5_2 C 0.8548(4) -0.1490(6) 0.5796(2) 0.108(3) Uani 1 d U . . H5_2 H 0.8339 -0.1890 0.5956 0.140 Uiso 1 d R . . C6_2 C 0.8780(3) -0.1828(6) 0.5491(2) 0.083(2) Uani 1 d U . . C7_2 C 0.8705(4) -0.2830(6) 0.5408(2) 0.104(3) Uani 1 d U . . H7_2 H 0.8498 -0.3248 0.5562 0.135 Uiso 1 d R . . C8_2 C 0.8953(4) -0.3113(5) 0.5102(2) 0.107(3) Uani 1 d U . . H8_2 H 0.8902 -0.3744 0.5032 0.140 Uiso 1 d R . . C9_2 C 0.9282(4) -0.2515(6) 0.4887(2) 0.114(3) Uani 1 d U . . H9_2 H 0.9477 -0.2742 0.4681 0.148 Uiso 1 d R . . C10_2 C 0.9319(4) -0.1619(7) 0.4969(3) 0.116(3) Uani 1 d U . . H10_2 H 0.9530 -0.1213 0.4813 0.151 Uiso 1 d R . . C11_2 C 0.9082(3) -0.1269(5) 0.5255(2) 0.078(2) Uani 1 d U . . C12_2 C 0.9158(3) -0.0262(5) 0.5335(2) 0.089(2) Uani 1 d U . . H12_2 H 0.9368 0.0147 0.5179 0.115 Uiso 1 d R . . C1P_2 C 0.8286(3) 0.1796(4) 0.67227(13) 0.0506(14) Uani 1 d U . . C2P_2 C 0.7900(3) 0.1075(5) 0.68120(16) 0.0715(19) Uani 1 d U . . H2P_2 H 0.7527 0.0974 0.6681 0.093 Uiso 1 d R . . C3P_2 C 0.8049(4) 0.0503(5) 0.7089(2) 0.096(2) Uani 1 d U . . H3P_2 H 0.7783 -0.0002 0.7149 0.125 Uiso 1 d R . . C4P_2 C 0.8578(4) 0.0674(6) 0.72801(19) 0.098(3) Uani 1 d U . . H4P_2 H 0.8673 0.0289 0.7477 0.127 Uiso 1 d R . . C5P_2 C 0.8962(3) 0.1351(6) 0.71922(18) 0.090(2) Uani 1 d U . . H5P_2 H 0.9336 0.1443 0.7323 0.117 Uiso 1 d R . . C6P_2 C 0.8819(3) 0.1925(5) 0.69119(15) 0.0673(18) Uani 1 d U . . H6P_2 H 0.9095 0.2415 0.6850 0.087 Uiso 1 d R . . C7P_2 C 0.7593(3) 0.3413(4) 0.65712(15) 0.0583(16) Uani 1 d U . . C8P_2 C 0.7826(3) 0.3881(5) 0.68620(16) 0.078(2) Uani 1 d U . . H8P_2 H 0.8213 0.3699 0.6963 0.102 Uiso 1 d R . . C9P_2 C 0.7502(5) 0.4599(6) 0.7006(2) 0.108(3) Uani 1 d U . . H9P_2 H 0.7670 0.4922 0.7203 0.141 Uiso 1 d R . . C10P_2 C 0.6957(5) 0.4856(6) 0.6872(2) 0.113(3) Uani 1 d U . . H10P_2 H 0.6737 0.5359 0.6976 0.147 Uiso 1 d R . . C11P_2 C 0.6714(4) 0.4418(6) 0.6590(2) 0.106(3) Uani 1 d U . . H11P_2 H 0.6324 0.4610 0.6497 0.138 Uiso 1 d R . . C12P_2 C 0.70306(19) 0.3685(3) 0.64384(10) 0.077(2) Uani 1 d U . . H12P_2 H 0.6855 0.3373 0.6240 0.100 Uiso 1 d R . . C13P_2 C 0.69138(19) -0.0185(3) 0.54655(10) 0.0717(19) Uani 1 d RU . . C14P_2 C 0.72682(19) -0.0926(3) 0.53898(10) 0.104(3) Uani 1 d RU . . H14P_2 H 0.7667 -0.0834 0.5289 0.135 Uiso 1 d R . . C15P_2 C 0.7067(4) -0.1827(6) 0.5455(3) 0.129(3) Uani 1 d U . . H15P_2 H 0.7318 -0.2352 0.5401 0.168 Uiso 1 d R . . C16P_2 C 0.6495(5) -0.1945(7) 0.5596(2) 0.115(3) Uani 1 d U . . H16P_2 H 0.6354 -0.2555 0.5651 0.150 Uiso 1 d R . . C17P_2 C 0.6126(5) -0.1238(7) 0.5667(3) 0.133(4) Uani 1 d U . . H17P_2 H 0.5719 -0.1336 0.5756 0.173 Uiso 1 d R . . C18P_2 C 0.6342(4) -0.0339(6) 0.5605(2) 0.121(3) Uani 1 d U . . H18P_2 H 0.6084 0.0179 0.5659 0.157 Uiso 1 d R . . C19P_2 C 0.6529(3) 0.1596(5) 0.52201(16) 0.0640(17) Uani 1 d U . . C20P_2 C 0.6217(3) 0.1258(6) 0.4933(2) 0.102(3) Uani 1 d U . . H20P_2 H 0.6333 0.0671 0.4837 0.132 Uiso 1 d R . . C21P_2 C 0.5749(4) 0.1750(8) 0.4780(2) 0.123(3) Uani 1 d U . . H21P_2 H 0.5548 0.1510 0.4576 0.160 Uiso 1 d R . . C22P_2 C 0.5568(4) 0.2554(9) 0.4918(3) 0.134(4) Uani 1 d U . . H22P_2 H 0.5235 0.2885 0.4810 0.174 Uiso 1 d R . . C23P_2 C 0.5844(5) 0.2918(7) 0.5205(2) 0.126(3) Uani 1 d U . . H23P_2 H 0.5709 0.3494 0.5302 0.164 Uiso 1 d R . . C24P_2 C 0.6348(4) 0.2421(6) 0.53561(18) 0.088(2) Uani 1 d U . . H24P_2 H 0.6556 0.2668 0.5557 0.114 Uiso 1 d R . . C25P_2 C 0.9489(3) 0.4174(4) 0.57741(13) 0.0474(14) Uani 1 d U . . C26P_2 C 0.9601(3) 0.4904(5) 0.5552(2) 0.104(3) Uani 1 d U . . H26P_2 H 0.9258 0.5211 0.5443 0.135 Uiso 1 d R . . C27P_2 C 1.0181(4) 0.5208(6) 0.5484(2) 0.105(3) Uani 1 d U . . H27P_2 H 1.0237 0.5707 0.5322 0.136 Uiso 1 d R . . C28P_2 C 1.0666(3) 0.4831(5) 0.56398(16) 0.074(2) Uani 1 d U . . H28P_2 H 1.1075 0.5052 0.5595 0.097 Uiso 1 d R . . C29P_2 C 1.0569(3) 0.4136(5) 0.58593(18) 0.090(2) Uani 1 d U . . H29P_2 H 1.0914 0.3852 0.5974 0.117 Uiso 1 d R . . C30P_2 C 0.9986(3) 0.3799(5) 0.59241(17) 0.078(2) Uani 1 d U . . H30P_2 H 0.9935 0.3293 0.6083 0.101 Uiso 1 d R . . C31P_2 C 0.8250(3) 0.4754(4) 0.59228(14) 0.0526(15) Uani 1 d U . . C32P_2 C 0.8444(3) 0.5354(5) 0.61845(16) 0.0765(19) Uani 1 d U . . H32P_2 H 0.8833 0.5258 0.6299 0.099 Uiso 1 d R . . C33P_2 C 0.8069(4) 0.6099(5) 0.6279(2) 0.092(2) Uani 1 d U . . H33P_2 H 0.8201 0.6505 0.6463 0.119 Uiso 1 d R . . C34P_2 C 0.7531(4) 0.6251(5) 0.6111(2) 0.090(2) Uani 1 d U . . H34P_2 H 0.7278 0.6764 0.6179 0.117 Uiso 1 d R . . C35P_2 C 0.7336(3) 0.5662(5) 0.5846(2) 0.090(2) Uani 1 d U . . H35P_2 H 0.6954 0.5777 0.5726 0.117 Uiso 1 d R . . C36P_2 C 0.7694(3) 0.4915(5) 0.57550(16) 0.0680(18) Uani 1 d U . . H36P_2 H 0.7559 0.4509 0.5572 0.088 Uiso 1 d R . . C37P_2 C 0.8687(3) 0.1605(5) 0.46154(14) 0.0621(17) Uani 1 d U . . C38P_2 C 0.8792(3) 0.0707(5) 0.45086(16) 0.079(2) Uani 1 d U . . H38P_2 H 0.8525 0.0222 0.4587 0.102 Uiso 1 d R . . C39P_2 C 0.9289(4) 0.0502(6) 0.42867(18) 0.092(2) Uani 1 d U . . H39P_2 H 0.9359 -0.0124 0.4215 0.120 Uiso 1 d R . . C40P_2 C 0.9658(3) 0.1189(8) 0.4176(2) 0.098(3) Uani 1 d U . . H40P_2 H 0.9993 0.1042 0.4024 0.127 Uiso 1 d R . . C41P_2 C 0.9565(3) 0.2078(7) 0.42768(19) 0.099(3) Uani 1 d U . . H41P_2 H 0.9834 0.2559 0.4197 0.129 Uiso 1 d R . . C42P_2 C 0.9074(3) 0.2269(5) 0.44978(17) 0.079(2) Uani 1 d U . . H42P_2 H 0.9008 0.2896 0.4569 0.103 Uiso 1 d R . . C43P_2 C 0.7500(3) 0.2401(4) 0.45691(14) 0.0554(15) Uani 1 d U . . C44P_2 C 0.7176(3) 0.3203(5) 0.46299(17) 0.081(2) Uani 1 d U . . H44P_2 H 0.7237 0.3551 0.4840 0.105 Uiso 1 d R . . C45P_2 C 0.6751(3) 0.3495(6) 0.4375(2) 0.108(3) Uani 1 d U . . H45P_2 H 0.6509 0.4039 0.4417 0.141 Uiso 1 d R . . C46P_2 C 0.6680(4) 0.3028(8) 0.4066(2) 0.119(4) Uani 1 d U . . H46P_2 H 0.6399 0.3255 0.3892 0.155 Uiso 1 d R . . C47P_2 C 0.7002(4) 0.2247(7) 0.4007(2) 0.102(3) Uani 1 d U . . H47P_2 H 0.6943 0.1915 0.3793 0.132 Uiso 1 d R . . C48P_2 C 0.7418(3) 0.1914(5) 0.42558(16) 0.0744(19) Uani 1 d U . . H48P_2 H 0.7647 0.1360 0.4213 0.097 Uiso 1 d R . . C1S C 0.5169(2) -0.3441(3) 0.65007(14) 0.119(3) Uani 1 d DU . . H1S H 0.5003 -0.2877 0.6591 0.154 Uiso 1 d R . . Cl1S Cl 0.5940(2) -0.3131(10) 0.6491(5) 0.168(5) Uani 0.52(3) d PDU . . Cl2S Cl 0.4950(4) -0.4516(6) 0.6341(5) 0.206(13) Uani 0.38(7) d PDU . . Cl3S Cl 0.4949(5) -0.4540(6) 0.6365(6) 0.158(12) Uani 0.17(7) d PDU . . Cl4S Cl 0.5172(4) -0.4395(11) 0.6774(6) 0.156(7) Uani 0.365(18) d PDU . . Cl5S Cl 0.5895(5) -0.3165(13) 0.6344(6) 0.210(8) Uani 0.46(3) d PDU . . Cl6S Cl 0.5277(6) -0.3850(15) 0.6923(3) 0.179(6) Uani 0.378(18) d PDU . . Cl7S Cl 0.4932(3) -0.3286(7) 0.60722(14) 0.280(6) Uani 0.729(10) d PDU . . O1W O 0.5310(7) 0.4986(11) 0.4796(4) 0.192(9) Uiso 0.529(18) d P . . O2W O 0.2300(8) 0.3348(12) 0.5556(4) 0.265(13) Uiso 0.61(2) d P . . O3W O 0.6486(7) 0.5642(11) 0.4964(4) 0.303(12) Uiso 0.76(2) d P . . O4W O 0.2255(8) 0.2218(12) 0.6212(5) 0.197(10) Uiso 0.461(14) d P . . O5W O 0.4343(9) 0.4612(14) 0.4521(5) 0.271(11) Uiso 0.539(14) d P . . O6W O 0.1896(10) 0.1455(16) 0.5568(6) 0.241(15) Uiso 0.44(2) d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1_1 0.0365(2) 0.0317(2) 0.0451(2) 0.00063(19) 0.00103(17) 0.00082(18) Pd2_1 0.0334(2) 0.0423(2) 0.0476(2) 0.0037(2) -0.00387(18) -0.00145(19) Cl1_1 0.0553(9) 0.0408(8) 0.0804(10) 0.0053(8) 0.0091(8) 0.0120(7) Cl2_1 0.0523(8) 0.0785(11) 0.0594(9) 0.0108(8) -0.0189(7) -0.0065(8) S1_1 0.0487(8) 0.0395(8) 0.0541(9) -0.0064(7) 0.0016(7) 0.0046(7) P1_1 0.0325(7) 0.0320(7) 0.0417(8) -0.0030(6) -0.0027(6) 0.0001(6) P2_1 0.0412(8) 0.0380(8) 0.0576(9) 0.0060(7) 0.0040(7) -0.0035(7) P3_1 0.0361(7) 0.0375(8) 0.0423(8) 0.0032(6) -0.0051(6) -0.0015(6) P4_1 0.0358(8) 0.0509(9) 0.0625(10) 0.0054(8) 0.0014(7) -0.0028(7) O1_1 0.067(3) 0.079(3) 0.110(4) -0.039(3) -0.012(3) 0.035(3) O2_1 0.072(3) 0.065(3) 0.052(2) -0.004(2) -0.003(2) -0.027(2) N1_1 0.040(2) 0.034(2) 0.043(2) 0.005(2) -0.0031(19) 0.005(2) C1_1 0.035(3) 0.028(3) 0.037(3) -0.001(2) 0.002(2) -0.006(2) C2_1 0.042(3) 0.042(3) 0.061(4) -0.002(3) 0.008(3) -0.003(3) C3_1 0.096(5) 0.062(4) 0.043(3) -0.016(3) 0.014(3) -0.022(4) C4_1 0.130(7) 0.073(5) 0.051(4) 0.004(4) -0.022(4) 0.006(5) C5_1 0.277(12) 0.071(6) 0.063(5) 0.008(5) -0.054(7) -0.015(7) C6_1 0.359(16) 0.167(11) 0.134(9) 0.049(8) -0.127(10) -0.011(11) C7_1 0.44(2) 0.185(12) 0.158(14) 0.070(11) -0.139(14) -0.022(16) C8_1 0.45(3) 0.158(12) 0.086(9) 0.019(8) -0.040(14) -0.066(17) C9_1 0.45(2) 0.154(13) 0.136(11) 0.036(9) -0.061(13) -0.105(15) C10_1 0.343(15) 0.098(8) 0.044(5) 0.019(5) 0.007(8) -0.054(9) C11_1 0.238(12) 0.120(9) 0.072(7) 0.012(5) 0.064(7) -0.049(8) C12_1 0.154(7) 0.098(6) 0.073(5) -0.019(5) 0.054(5) -0.030(6) C1P_1 0.034(3) 0.044(3) 0.049(3) -0.002(3) -0.003(2) 0.005(3) C2P_1 0.079(4) 0.052(4) 0.061(4) 0.001(3) -0.021(3) 0.001(3) C3P_1 0.080(5) 0.094(6) 0.059(4) 0.010(4) -0.034(4) 0.005(4) C4P_1 0.063(4) 0.075(5) 0.059(4) -0.022(4) -0.009(3) -0.009(4) C5P_1 0.083(5) 0.058(4) 0.090(5) -0.002(4) -0.025(4) -0.012(4) C6P_1 0.058(4) 0.045(3) 0.058(4) -0.002(3) -0.024(3) -0.006(3) C7P_1 0.034(3) 0.038(3) 0.039(3) -0.004(2) 0.000(2) -0.001(2) C8P_1 0.045(3) 0.058(4) 0.065(4) -0.019(3) 0.004(3) -0.006(3) C9P_1 0.047(4) 0.087(5) 0.074(4) -0.021(4) 0.018(3) -0.013(3) C10P_1 0.054(4) 0.090(5) 0.065(4) -0.026(4) 0.017(3) -0.003(4) C11P_1 0.062(4) 0.058(4) 0.065(4) -0.017(3) 0.012(3) 0.004(3) C12P_1 0.042(3) 0.038(3) 0.056(3) -0.001(3) -0.001(3) -0.007(3) C13P_1 0.060(4) 0.057(4) 0.058(4) 0.013(3) 0.005(3) -0.003(3) C14P_1 0.102(6) 0.146(8) 0.104(6) 0.069(6) 0.034(5) 0.049(6) C15P_1 0.149(9) 0.203(10) 0.130(8) 0.102(8) 0.020(7) 0.068(8) C16P_1 0.142(9) 0.161(9) 0.113(7) 0.082(7) 0.028(7) 0.037(7) C17P_1 0.121(7) 0.150(8) 0.112(7) 0.085(6) 0.054(6) 0.026(6) C18P_1 0.084(5) 0.128(7) 0.102(6) 0.056(5) 0.032(5) 0.032(5) C19P_1 0.049(3) 0.047(4) 0.075(4) 0.003(3) -0.001(3) -0.001(3) C20P_1 0.094(5) 0.058(5) 0.115(6) -0.002(4) -0.002(5) -0.026(4) C21P_1 0.097(6) 0.068(5) 0.158(9) -0.014(6) -0.015(6) -0.032(5) C22P_1 0.073(6) 0.086(6) 0.153(8) -0.058(6) -0.030(6) 0.000(5) C23P_1 0.058(4) 0.097(6) 0.135(7) -0.056(5) -0.003(4) 0.006(4) C24P_1 0.050(4) 0.081(5) 0.103(6) -0.024(4) -0.005(4) -0.014(4) C25P_1 0.034(3) 0.040(3) 0.053(3) 0.003(3) 0.002(2) -0.004(2) C26P_1 0.085(5) 0.051(4) 0.077(4) -0.005(3) -0.031(4) 0.021(4) C27P_1 0.103(6) 0.046(4) 0.137(7) -0.007(4) -0.047(5) 0.015(4) C28P_1 0.080(5) 0.059(5) 0.111(6) 0.023(5) -0.022(5) 0.001(4) C29P_1 0.078(5) 0.073(5) 0.066(4) 0.023(4) -0.019(4) 0.001(4) C30P_1 0.071(4) 0.052(4) 0.057(4) 0.010(3) -0.017(3) -0.004(3) C31P_1 0.037(3) 0.051(4) 0.038(3) 0.003(3) -0.005(2) 0.013(3) C32P_1 0.059(4) 0.080(5) 0.052(4) 0.001(3) 0.002(3) 0.011(3) C33P_1 0.079(5) 0.128(7) 0.070(5) 0.002(5) 0.018(4) 0.021(5) C34P_1 0.088(6) 0.116(7) 0.072(5) -0.018(5) -0.007(4) 0.061(6) C35P_1 0.103(6) 0.072(5) 0.073(5) -0.025(4) -0.035(4) 0.032(5) C36P_1 0.061(4) 0.048(4) 0.054(4) -0.005(3) -0.014(3) 0.014(3) C37P_1 0.046(3) 0.046(4) 0.079(4) -0.002(3) -0.011(3) -0.004(3) C38P_1 0.052(4) 0.089(5) 0.127(6) -0.006(5) 0.013(4) -0.026(4) C39P_1 0.082(6) 0.099(7) 0.175(9) -0.010(7) 0.000(6) -0.048(5) C40P_1 0.074(6) 0.086(6) 0.174(9) -0.006(6) -0.070(6) -0.019(5) C41P_1 0.091(6) 0.092(6) 0.101(6) -0.003(5) -0.028(5) 0.001(5) C42P_1 0.063(4) 0.066(5) 0.087(5) -0.004(4) -0.018(4) -0.010(4) C43P_1 0.033(3) 0.062(4) 0.075(4) 0.005(3) 0.002(3) 0.002(3) C44P_1 0.056(4) 0.085(5) 0.059(4) 0.006(4) -0.001(3) 0.018(4) C45P_1 0.082(5) 0.084(5) 0.106(6) 0.006(5) -0.020(5) 0.036(4) C46P_1 0.055(4) 0.100(6) 0.093(6) -0.022(5) 0.002(4) 0.016(4) C47P_1 0.047(4) 0.109(6) 0.084(5) -0.004(5) 0.016(4) 0.006(4) C48P_1 0.043(3) 0.088(5) 0.076(4) 0.012(4) 0.015(3) 0.004(3) Pd1_2 0.0479(3) 0.0556(3) 0.0414(2) 0.0079(2) 0.00114(19) -0.0075(2) Pd2_2 0.0572(3) 0.0457(3) 0.0353(2) 0.0041(2) 0.00347(19) -0.0049(2) Cl1_2 0.0582(10) 0.1099(14) 0.0658(10) 0.0167(10) 0.0114(8) -0.0211(10) Cl2_2 0.1297(16) 0.0631(11) 0.0544(10) 0.0189(8) 0.0040(10) -0.0135(11) P1_2 0.0477(9) 0.0509(9) 0.0374(8) 0.0065(7) 0.0044(6) -0.0011(7) P2_2 0.0587(10) 0.0612(11) 0.0515(9) 0.0052(8) -0.0046(8) -0.0147(8) P3_2 0.0533(9) 0.0450(9) 0.0388(8) 0.0038(7) 0.0004(7) -0.0051(7) P4_2 0.0568(9) 0.0566(10) 0.0381(8) 0.0022(7) -0.0033(7) -0.0010(8) N1_2 0.051(3) 0.044(3) 0.036(2) 0.008(2) 0.000(2) 0.002(2) S1_2 0.0497(9) 0.0482(9) 0.0562(9) -0.0017(7) -0.0030(7) 0.0025(7) O1_2 0.051(3) 0.080(3) 0.140(4) 0.013(3) 0.025(3) 0.003(2) O2_2 0.103(3) 0.086(3) 0.051(3) -0.003(2) -0.023(2) 0.035(3) C1_2 0.051(3) 0.043(3) 0.036(3) 0.002(2) -0.001(2) -0.004(3) C2_2 0.074(4) 0.045(4) 0.052(4) -0.003(3) -0.009(3) -0.006(3) C3_2 0.055(4) 0.084(5) 0.061(4) -0.005(4) -0.015(3) 0.021(4) C4_2 0.133(7) 0.062(5) 0.106(6) 0.011(5) -0.014(5) -0.004(5) C5_2 0.108(6) 0.109(7) 0.106(7) 0.027(6) 0.022(5) 0.003(6) C6_2 0.073(5) 0.107(7) 0.069(5) -0.017(5) 0.006(4) 0.029(5) C7_2 0.111(6) 0.078(6) 0.122(7) 0.017(5) 0.014(6) -0.019(5) C8_2 0.157(8) 0.055(5) 0.111(7) -0.013(5) 0.010(6) 0.004(5) C9_2 0.152(8) 0.073(6) 0.116(7) 0.007(6) 0.017(6) 0.036(6) C10_2 0.130(7) 0.100(7) 0.120(7) 0.008(6) 0.019(6) 0.025(6) C11_2 0.082(5) 0.071(5) 0.080(5) 0.004(4) -0.009(4) 0.007(4) C12_2 0.090(5) 0.080(5) 0.095(6) -0.022(4) -0.041(4) 0.032(4) C1P_2 0.058(4) 0.056(4) 0.038(3) 0.014(3) 0.011(3) 0.011(3) C2P_2 0.070(4) 0.082(5) 0.063(4) 0.030(4) 0.005(3) 0.013(4) C3P_2 0.096(6) 0.090(6) 0.102(6) 0.046(5) 0.022(5) -0.001(5) C4P_2 0.087(6) 0.132(7) 0.075(5) 0.056(5) 0.015(4) 0.035(5) C5P_2 0.070(5) 0.136(7) 0.064(5) 0.024(5) -0.007(4) 0.025(5) C6P_2 0.060(4) 0.094(5) 0.048(4) 0.014(4) -0.004(3) 0.003(4) C7P_2 0.058(4) 0.068(4) 0.050(4) 0.014(3) 0.010(3) 0.015(3) C8P_2 0.092(5) 0.090(5) 0.053(4) -0.002(4) 0.008(4) 0.024(4) C9P_2 0.149(8) 0.103(7) 0.074(5) -0.025(5) 0.029(5) 0.041(6) C10P_2 0.139(8) 0.115(7) 0.087(6) 0.009(6) 0.054(6) 0.050(7) C11P_2 0.093(6) 0.115(7) 0.110(7) 0.006(6) 0.019(5) 0.046(5) C12P_2 0.060(4) 0.090(5) 0.081(5) 0.009(4) 0.008(4) 0.021(4) C13P_2 0.082(5) 0.072(5) 0.062(4) 0.013(4) -0.012(4) -0.020(4) C14P_2 0.078(5) 0.073(6) 0.160(8) 0.045(5) -0.017(5) -0.006(4) C15P_2 0.103(7) 0.082(6) 0.201(10) 0.041(6) -0.004(7) 0.005(6) C16P_2 0.149(9) 0.080(6) 0.118(7) 0.029(6) -0.023(7) -0.037(6) C17P_2 0.143(9) 0.083(7) 0.174(9) 0.001(7) 0.039(7) -0.047(7) C18P_2 0.122(7) 0.085(6) 0.156(8) -0.011(6) 0.038(6) -0.038(5) C19P_2 0.060(4) 0.070(5) 0.062(4) 0.016(4) -0.004(3) -0.003(4) C20P_2 0.085(5) 0.116(7) 0.103(6) 0.006(5) -0.031(5) -0.003(5) C21P_2 0.094(6) 0.165(9) 0.109(7) 0.031(7) -0.052(5) 0.011(7) C22P_2 0.104(7) 0.183(11) 0.114(8) 0.058(8) 0.000(6) 0.063(7) C23P_2 0.146(8) 0.162(9) 0.071(6) 0.022(6) 0.026(6) 0.064(7) C24P_2 0.099(6) 0.111(6) 0.054(4) 0.026(4) 0.010(4) 0.017(5) C25P_2 0.058(4) 0.051(4) 0.034(3) 0.007(3) 0.007(3) -0.007(3) C26P_2 0.066(5) 0.103(6) 0.142(7) 0.069(5) 0.009(5) -0.017(4) C27P_2 0.082(6) 0.122(7) 0.111(6) 0.051(5) 0.003(5) -0.029(5) C28P_2 0.073(5) 0.105(6) 0.046(4) 0.006(4) 0.002(3) -0.038(4) C29P_2 0.063(5) 0.119(6) 0.088(5) 0.035(5) -0.023(4) -0.016(4) C30P_2 0.061(4) 0.093(5) 0.078(5) 0.033(4) -0.016(4) -0.029(4) C31P_2 0.072(4) 0.046(4) 0.040(3) 0.006(3) 0.008(3) -0.009(3) C32P_2 0.107(5) 0.065(5) 0.058(4) -0.005(4) -0.005(4) 0.006(4) C33P_2 0.133(7) 0.055(5) 0.086(6) -0.017(4) 0.007(5) 0.009(5) C34P_2 0.108(6) 0.069(5) 0.094(6) 0.005(5) 0.032(5) 0.028(5) C35P_2 0.084(5) 0.081(6) 0.105(6) 0.011(5) 0.010(5) 0.025(5) C36P_2 0.074(5) 0.070(5) 0.059(4) 0.004(3) -0.002(4) 0.008(4) C37P_2 0.058(4) 0.091(5) 0.038(3) -0.002(3) -0.001(3) 0.002(4) C38P_2 0.087(5) 0.091(5) 0.058(4) -0.003(4) 0.008(4) 0.026(4) C39P_2 0.108(6) 0.109(7) 0.060(5) -0.001(5) -0.001(4) 0.041(6) C40P_2 0.061(5) 0.166(9) 0.066(5) -0.013(6) -0.002(4) 0.034(6) C41P_2 0.074(5) 0.151(8) 0.074(5) -0.015(6) 0.015(4) -0.015(6) C42P_2 0.067(4) 0.101(6) 0.070(5) -0.008(4) 0.010(4) -0.005(4) C43P_2 0.065(4) 0.065(4) 0.036(3) 0.009(3) -0.002(3) -0.002(3) C44P_2 0.076(5) 0.105(6) 0.063(4) 0.015(4) 0.003(4) 0.023(4) C45P_2 0.082(5) 0.139(8) 0.104(6) 0.039(6) -0.003(5) 0.039(5) C46P_2 0.091(6) 0.198(11) 0.069(6) 0.059(7) -0.009(5) -0.010(7) C47P_2 0.083(6) 0.155(9) 0.066(5) 0.007(6) -0.017(4) -0.024(6) C48P_2 0.069(4) 0.096(5) 0.058(4) 0.003(4) -0.012(3) -0.014(4) C1S 0.090(6) 0.080(6) 0.186(10) -0.020(7) 0.016(6) 0.034(5) Cl1S 0.106(5) 0.165(7) 0.234(13) -0.002(7) -0.042(6) -0.027(5) Cl2S 0.137(14) 0.18(2) 0.304(18) -0.13(2) 0.041(13) -0.020(10) Cl3S 0.085(16) 0.088(19) 0.30(2) -0.01(2) 0.100(18) -0.017(13) Cl4S 0.076(6) 0.096(9) 0.299(17) 0.060(10) 0.063(7) 0.013(5) Cl5S 0.223(12) 0.214(10) 0.193(13) -0.009(8) 0.088(10) -0.140(10) Cl6S 0.253(13) 0.130(12) 0.154(8) 0.057(7) -0.017(8) 0.022(8) Cl7S 0.187(6) 0.393(13) 0.259(7) -0.068(7) -0.075(5) 0.023(6) _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_1 N1_1 2.016(4) . ? Pd1_1 P1_1 2.3231(14) . ? Pd1_1 Cl1_1 2.3304(14) . ? Pd1_1 P2_1 2.3567(14) . ? Pd1_1 Pd2_1 3.2877(7) . ? Pd2_1 N1_1 2.013(4) . ? Pd2_1 P4_1 2.3118(15) . ? Pd2_1 P3_1 2.3184(14) . ? Pd2_1 Cl2_1 2.3275(14) . ? S1_1 O1_1 1.434(4) . ? S1_1 O2_1 1.445(4) . ? S1_1 N1_1 1.556(4) . ? S1_1 C3_1 1.759(6) . ? P1_1 C7P_1 1.815(5) . ? P1_1 C1P_1 1.816(5) . ? P1_1 C1_1 1.826(4) . ? P2_1 C19P_1 1.800(6) . ? P2_1 C13P_1 1.805(6) . ? P2_1 C2_1 1.839(5) . ? P3_1 C25P_1 1.808(5) . ? P3_1 C1_1 1.817(4) . ? P3_1 C31P_1 1.821(5) . ? P4_1 C37P_1 1.814(6) . ? P4_1 C43P_1 1.816(6) . ? P4_1 C2_1 1.824(5) . ? C3_1 C4_1 1.396(3) . ? C3_1 C12_1 1.399(3) . ? C4_1 C5_1 1.398(3) . ? C5_1 C10_1 1.397(3) . ? C5_1 C6_1 1.399(3) . ? C6_1 C7_1 1.401(3) . ? C7_1 C8_1 1.400(3) . ? C8_1 C9_1 1.398(3) . ? C9_1 C10_1 1.404(3) . ? C10_1 C11_1 1.399(3) . ? C11_1 C12_1 1.398(3) . ? C1P_1 C2P_1 1.370(7) . ? C1P_1 C6P_1 1.374(7) . ? C2P_1 C3P_1 1.424(8) . ? C3P_1 C4P_1 1.358(8) . ? C4P_1 C5P_1 1.353(8) . ? C5P_1 C6P_1 1.372(7) . ? C7P_1 C12P_1 1.372(6) . ? C7P_1 C8P_1 1.387(7) . ? C8P_1 C9P_1 1.391(7) . ? C9P_1 C10P_1 1.359(8) . ? C10P_1 C11P_1 1.371(8) . ? C11P_1 C12P_1 1.376(7) . ? C13P_1 C14P_1 1.346(8) . ? C13P_1 C18P_1 1.379(8) . ? C14P_1 C15P_1 1.406(10) . ? C15P_1 C16P_1 1.342(11) . ? C16P_1 C17P_1 1.308(10) . ? C17P_1 C18P_1 1.391(9) . ? C19P_1 C24P_1 1.382(8) . ? C19P_1 C20P_1 1.390(8) . ? C20P_1 C21P_1 1.374(9) . ? C21P_1 C22P_1 1.345(10) . ? C22P_1 C23P_1 1.354(10) . ? C23P_1 C24P_1 1.422(9) . ? C25P_1 C30P_1 1.381(7) . ? C25P_1 C26P_1 1.384(7) . ? C26P_1 C27P_1 1.390(8) . ? C27P_1 C28P_1 1.343(9) . ? C28P_1 C29P_1 1.373(9) . ? C29P_1 C30P_1 1.372(8) . ? C31P_1 C36P_1 1.379(7) . ? C31P_1 C32P_1 1.387(7) . ? C32P_1 C33P_1 1.390(9) . ? C33P_1 C34P_1 1.352(10) . ? C34P_1 C35P_1 1.363(10) . ? C35P_1 C36P_1 1.389(8) . ? C37P_1 C42P_1 1.366(8) . ? C37P_1 C38P_1 1.402(8) . ? C38P_1 C39P_1 1.365(10) . ? C39P_1 C40P_1 1.374(11) . ? C40P_1 C41P_1 1.372(11) . ? C41P_1 C42P_1 1.391(9) . ? C43P_1 C44P_1 1.370(8) . ? C43P_1 C48P_1 1.380(7) . ? C44P_1 C45P_1 1.389(8) . ? C45P_1 C46P_1 1.376(9) . ? C46P_1 C47P_1 1.363(9) . ? C47P_1 C48P_1 1.376(8) . ? Pd1_2 N1_2 2.007(4) . ? Pd1_2 P2_2 2.3309(16) . ? Pd1_2 P1_2 2.3364(15) . ? Pd1_2 Cl1_2 2.3416(16) . ? Pd1_2 Pd2_2 3.2309(7) . ? Pd2_2 N1_2 2.019(4) . ? Pd2_2 P3_2 2.3134(15) . ? Pd2_2 Cl2_2 2.3178(16) . ? Pd2_2 P4_2 2.3243(15) . ? P1_2 C1P_2 1.809(5) . ? P1_2 C1_2 1.824(5) . ? P1_2 C7P_2 1.826(6) . ? P2_2 C19P_2 1.798(6) . ? P2_2 C2_2 1.811(6) . ? P2_2 C13P_2 1.818(4) . ? P3_2 C25P_2 1.809(6) . ? P3_2 C31P_2 1.812(6) . ? P3_2 C1_2 1.823(5) . ? P4_2 C37P_2 1.813(6) . ? P4_2 C43P_2 1.818(6) . ? P4_2 C2_2 1.842(5) . ? N1_2 S1_2 1.562(4) . ? S1_2 O1_2 1.422(4) . ? S1_2 O2_2 1.450(4) . ? S1_2 C3_2 1.790(7) . ? C3_2 C12_2 1.304(8) . ? C3_2 C4_2 1.427(9) . ? C4_2 C5_2 1.379(10) . ? C5_2 C6_2 1.369(9) . ? C6_2 C11_2 1.384(10) . ? C6_2 C7_2 1.495(10) . ? C7_2 C8_2 1.357(10) . ? C8_2 C9_2 1.393(11) . ? C9_2 C10_2 1.338(11) . ? C10_2 C11_2 1.314(10) . ? C11_2 C12_2 1.501(9) . ? C1P_2 C6P_2 1.374(7) . ? C1P_2 C2P_2 1.383(8) . ? C2P_2 C3P_2 1.385(8) . ? C3P_2 C4P_2 1.380(10) . ? C4P_2 C5P_2 1.333(10) . ? C5P_2 C6P_2 1.393(8) . ? C7P_2 C12P_2 1.378(7) . ? C7P_2 C8P_2 1.396(8) . ? C8P_2 C9P_2 1.373(9) . ? C9P_2 C10P_2 1.340(11) . ? C10P_2 C11P_2 1.355(11) . ? C11P_2 C12P_2 1.394(9) . ? C13P_2 C14P_2 1.3539 . ? C13P_2 C18P_2 1.374(8) . ? C14P_2 C15P_2 1.398(9) . ? C15P_2 C16P_2 1.369(11) . ? C16P_2 C17P_2 1.330(11) . ? C17P_2 C18P_2 1.404(10) . ? C19P_2 C24P_2 1.363(9) . ? C19P_2 C20P_2 1.381(9) . ? C20P_2 C21P_2 1.368(10) . ? C21P_2 C22P_2 1.338(12) . ? C22P_2 C23P_2 1.357(13) . ? C23P_2 C24P_2 1.430(10) . ? C25P_2 C30P_2 1.334(7) . ? C25P_2 C26P_2 1.380(8) . ? C26P_2 C27P_2 1.361(9) . ? C27P_2 C28P_2 1.326(9) . ? C28P_2 C29P_2 1.331(8) . ? C29P_2 C30P_2 1.380(8) . ? C31P_2 C36P_2 1.384(8) . ? C31P_2 C32P_2 1.391(8) . ? C32P_2 C33P_2 1.401(9) . ? C33P_2 C34P_2 1.349(10) . ? C34P_2 C35P_2 1.392(10) . ? C35P_2 C36P_2 1.378(8) . ? C37P_2 C42P_2 1.356(8) . ? C37P_2 C38P_2 1.383(8) . ? C38P_2 C39P_2 1.411(9) . ? C39P_2 C40P_2 1.347(10) . ? C40P_2 C41P_2 1.361(10) . ? C41P_2 C42P_2 1.395(9) . ? C43P_2 C44P_2 1.379(8) . ? C43P_2 C48P_2 1.403(8) . ? C44P_2 C45P_2 1.404(9) . ? C45P_2 C46P_2 1.374(11) . ? C46P_2 C47P_2 1.351(11) . ? C47P_2 C48P_2 1.395(9) . ? C1S Cl7S 1.733(3) . ? C1S Cl4S 1.734(3) . ? C1S Cl1S 1.735(3) . ? C1S Cl5S 1.736(3) . ? C1S Cl6S 1.738(3) . ? C1S Cl2S 1.739(3) . ? C1S Cl3S 1.741(3) . ? Cl1S Cl5S 0.57(3) . ? Cl1S Cl6S 2.436(17) . ? Cl2S Cl4S 1.74(3) . ? Cl2S Cl7S 2.059(17) . ? Cl3S Cl4S 1.65(3) . ? Cl3S Cl7S 2.134(19) . ? Cl3S Cl6S 2.46(2) . ? Cl4S Cl6S 0.999(14) . ? Cl5S Cl7S 2.338(19) . ? 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_1 Pd1_1 P1_1 89.83(12) . . ? N1_1 Pd1_1 Cl1_1 177.46(11) . . ? P1_1 Pd1_1 Cl1_1 92.47(5) . . ? N1_1 Pd1_1 P2_1 85.32(12) . . ? P1_1 Pd1_1 P2_1 174.35(5) . . ? Cl1_1 Pd1_1 P2_1 92.44(5) . . ? N1_1 Pd1_1 Pd2_1 35.28(11) . . ? P1_1 Pd1_1 Pd2_1 90.12(4) . . ? Cl1_1 Pd1_1 Pd2_1 145.72(4) . . ? P2_1 Pd1_1 Pd2_1 84.25(4) . . ? N1_1 Pd2_1 P4_1 85.69(12) . . ? N1_1 Pd2_1 P3_1 91.08(12) . . ? P4_1 Pd2_1 P3_1 175.46(5) . . ? N1_1 Pd2_1 Cl2_1 177.20(12) . . ? P4_1 Pd2_1 Cl2_1 93.17(5) . . ? P3_1 Pd2_1 Cl2_1 90.20(5) . . ? N1_1 Pd2_1 Pd1_1 35.33(11) . . ? P4_1 Pd2_1 Pd1_1 91.60(4) . . ? P3_1 Pd2_1 Pd1_1 83.93(4) . . ? Cl2_1 Pd2_1 Pd1_1 147.36(4) . . ? O1_1 S1_1 O2_1 114.5(3) . . ? O1_1 S1_1 N1_1 109.1(2) . . ? O2_1 S1_1 N1_1 115.9(2) . . ? O1_1 S1_1 C3_1 106.9(3) . . ? O2_1 S1_1 C3_1 103.9(2) . . ? N1_1 S1_1 C3_1 105.7(2) . . ? C7P_1 P1_1 C1P_1 102.7(2) . . ? C7P_1 P1_1 C1_1 103.8(2) . . ? C1P_1 P1_1 C1_1 104.3(2) . . ? C7P_1 P1_1 Pd1_1 120.33(17) . . ? C1P_1 P1_1 Pd1_1 111.01(18) . . ? C1_1 P1_1 Pd1_1 113.08(15) . . ? C19P_1 P2_1 C13P_1 101.4(3) . . ? C19P_1 P2_1 C2_1 103.6(3) . . ? C13P_1 P2_1 C2_1 102.3(3) . . ? C19P_1 P2_1 Pd1_1 114.3(2) . . ? C13P_1 P2_1 Pd1_1 119.3(2) . . ? C2_1 P2_1 Pd1_1 113.88(17) . . ? C25P_1 P3_1 C1_1 104.1(2) . . ? C25P_1 P3_1 C31P_1 105.5(2) . . ? C1_1 P3_1 C31P_1 105.5(2) . . ? C25P_1 P3_1 Pd2_1 112.57(16) . . ? C1_1 P3_1 Pd2_1 114.49(16) . . ? C31P_1 P3_1 Pd2_1 113.79(19) . . ? C37P_1 P4_1 C43P_1 104.7(3) . . ? C37P_1 P4_1 C2_1 101.7(3) . . ? C43P_1 P4_1 C2_1 104.1(3) . . ? C37P_1 P4_1 Pd2_1 119.8(2) . . ? C43P_1 P4_1 Pd2_1 112.5(2) . . ? C2_1 P4_1 Pd2_1 112.40(17) . . ? S1_1 N1_1 Pd2_1 123.8(2) . . ? S1_1 N1_1 Pd1_1 125.5(2) . . ? Pd2_1 N1_1 Pd1_1 109.39(18) . . ? P3_1 C1_1 P1_1 115.4(2) . . ? P4_1 C2_1 P2_1 118.1(3) . . ? C4_1 C3_1 C12_1 120.1(6) . . ? C4_1 C3_1 S1_1 120.0(4) . . ? C12_1 C3_1 S1_1 119.9(5) . . ? C3_1 C4_1 C5_1 119.9(7) . . ? C10_1 C5_1 C4_1 121.7(8) . . ? C10_1 C5_1 C6_1 117.2(8) . . ? C4_1 C5_1 C6_1 121.1(8) . . ? C5_1 C6_1 C7_1 121.4(10) . . ? C8_1 C7_1 C6_1 113.1(14) . . ? C9_1 C8_1 C7_1 133.3(15) . . ? C8_1 C9_1 C10_1 106.1(13) . . ? C5_1 C10_1 C11_1 116.7(8) . . ? C5_1 C10_1 C9_1 128.8(10) . . ? C11_1 C10_1 C9_1 114.5(11) . . ? C12_1 C11_1 C10_1 123.2(8) . . ? C11_1 C12_1 C3_1 118.3(7) . . ? C2P_1 C1P_1 C6P_1 119.5(5) . . ? C2P_1 C1P_1 P1_1 117.8(4) . . ? C6P_1 C1P_1 P1_1 122.6(4) . . ? C1P_1 C2P_1 C3P_1 119.3(6) . . ? C4P_1 C3P_1 C2P_1 119.6(6) . . ? C5P_1 C4P_1 C3P_1 119.9(6) . . ? C4P_1 C5P_1 C6P_1 121.4(6) . . ? C5P_1 C6P_1 C1P_1 120.1(5) . . ? C12P_1 C7P_1 C8P_1 118.1(5) . . ? C12P_1 C7P_1 P1_1 122.8(4) . . ? C8P_1 C7P_1 P1_1 119.1(4) . . ? C7P_1 C8P_1 C9P_1 120.8(5) . . ? C10P_1 C9P_1 C8P_1 119.0(6) . . ? C9P_1 C10P_1 C11P_1 121.1(6) . . ? C10P_1 C11P_1 C12P_1 119.3(6) . . ? C7P_1 C12P_1 C11P_1 121.5(5) . . ? C14P_1 C13P_1 C18P_1 117.0(6) . . ? C14P_1 C13P_1 P2_1 118.9(5) . . ? C18P_1 C13P_1 P2_1 124.1(5) . . ? C13P_1 C14P_1 C15P_1 121.0(8) . . ? C16P_1 C15P_1 C14P_1 120.5(9) . . ? C17P_1 C16P_1 C15P_1 118.8(8) . . ? C16P_1 C17P_1 C18P_1 122.3(8) . . ? C13P_1 C18P_1 C17P_1 120.1(7) . . ? C24P_1 C19P_1 C20P_1 119.4(6) . . ? C24P_1 C19P_1 P2_1 120.3(5) . . ? C20P_1 C19P_1 P2_1 120.3(5) . . ? C21P_1 C20P_1 C19P_1 120.2(8) . . ? C22P_1 C21P_1 C20P_1 121.3(8) . . ? C21P_1 C22P_1 C23P_1 119.9(8) . . ? C22P_1 C23P_1 C24P_1 121.0(8) . . ? C19P_1 C24P_1 C23P_1 118.2(7) . . ? C30P_1 C25P_1 C26P_1 117.6(5) . . ? C30P_1 C25P_1 P3_1 120.3(4) . . ? C26P_1 C25P_1 P3_1 121.6(4) . . ? C25P_1 C26P_1 C27P_1 120.5(6) . . ? C28P_1 C27P_1 C26P_1 120.7(7) . . ? C27P_1 C28P_1 C29P_1 119.7(7) . . ? C30P_1 C29P_1 C28P_1 120.2(6) . . ? C29P_1 C30P_1 C25P_1 121.2(6) . . ? C36P_1 C31P_1 C32P_1 119.2(5) . . ? C36P_1 C31P_1 P3_1 121.2(4) . . ? C32P_1 C31P_1 P3_1 119.6(5) . . ? C31P_1 C32P_1 C33P_1 119.9(7) . . ? C34P_1 C33P_1 C32P_1 120.0(8) . . ? C33P_1 C34P_1 C35P_1 120.9(8) . . ? C34P_1 C35P_1 C36P_1 120.0(7) . . ? C31P_1 C36P_1 C35P_1 119.9(6) . . ? C42P_1 C37P_1 C38P_1 118.8(6) . . ? C42P_1 C37P_1 P4_1 120.6(5) . . ? C38P_1 C37P_1 P4_1 120.4(5) . . ? C39P_1 C38P_1 C37P_1 121.1(8) . . ? C38P_1 C39P_1 C40P_1 118.7(8) . . ? C41P_1 C40P_1 C39P_1 121.7(8) . . ? C40P_1 C41P_1 C42P_1 118.8(8) . . ? C37P_1 C42P_1 C41P_1 120.7(7) . . ? C44P_1 C43P_1 C48P_1 118.8(6) . . ? C44P_1 C43P_1 P4_1 117.3(5) . . ? C48P_1 C43P_1 P4_1 123.9(5) . . ? C43P_1 C44P_1 C45P_1 120.3(6) . . ? C46P_1 C45P_1 C44P_1 120.0(7) . . ? C47P_1 C46P_1 C45P_1 119.8(7) . . ? C46P_1 C47P_1 C48P_1 120.0(7) . . ? C47P_1 C48P_1 C43P_1 121.1(6) . . ? N1_2 Pd1_2 P2_2 86.58(12) . . ? N1_2 Pd1_2 P1_2 90.06(12) . . ? P2_2 Pd1_2 P1_2 174.11(6) . . ? N1_2 Pd1_2 Cl1_2 175.51(13) . . ? P2_2 Pd1_2 Cl1_2 89.30(6) . . ? P1_2 Pd1_2 Cl1_2 94.20(6) . . ? N1_2 Pd1_2 Pd2_2 36.74(11) . . ? P2_2 Pd1_2 Pd2_2 84.39(4) . . ? P1_2 Pd1_2 Pd2_2 90.02(4) . . ? Cl1_2 Pd1_2 Pd2_2 144.48(5) . . ? N1_2 Pd2_2 P3_2 90.38(12) . . ? N1_2 Pd2_2 Cl2_2 179.07(12) . . ? P3_2 Pd2_2 Cl2_2 90.09(6) . . ? N1_2 Pd2_2 P4_2 86.96(12) . . ? P3_2 Pd2_2 P4_2 177.31(5) . . ? Cl2_2 Pd2_2 P4_2 92.56(6) . . ? N1_2 Pd2_2 Pd1_2 36.50(11) . . ? P3_2 Pd2_2 Pd1_2 86.40(4) . . ? Cl2_2 Pd2_2 Pd1_2 144.34(5) . . ? P4_2 Pd2_2 Pd1_2 91.68(4) . . ? C1P_2 P1_2 C1_2 104.3(2) . . ? C1P_2 P1_2 C7P_2 102.9(2) . . ? C1_2 P1_2 C7P_2 102.0(3) . . ? C1P_2 P1_2 Pd1_2 113.8(2) . . ? C1_2 P1_2 Pd1_2 113.75(16) . . ? C7P_2 P1_2 Pd1_2 118.3(2) . . ? C19P_2 P2_2 C2_2 104.1(3) . . ? C19P_2 P2_2 C13P_2 105.0(3) . . ? C2_2 P2_2 C13P_2 102.6(2) . . ? C19P_2 P2_2 Pd1_2 114.2(2) . . ? C2_2 P2_2 Pd1_2 114.46(19) . . ? C13P_2 P2_2 Pd1_2 115.08(15) . . ? C25P_2 P3_2 C31P_2 105.4(3) . . ? C25P_2 P3_2 C1_2 103.2(2) . . ? C31P_2 P3_2 C1_2 102.8(2) . . ? C25P_2 P3_2 Pd2_2 112.90(17) . . ? C31P_2 P3_2 Pd2_2 115.3(2) . . ? C1_2 P3_2 Pd2_2 115.83(17) . . ? C37P_2 P4_2 C43P_2 102.4(3) . . ? C37P_2 P4_2 C2_2 104.6(3) . . ? C43P_2 P4_2 C2_2 104.4(3) . . ? C37P_2 P4_2 Pd2_2 112.0(2) . . ? C43P_2 P4_2 Pd2_2 120.6(2) . . ? C2_2 P4_2 Pd2_2 111.35(18) . . ? S1_2 N1_2 Pd1_2 125.0(2) . . ? S1_2 N1_2 Pd2_2 124.2(2) . . ? Pd1_2 N1_2 Pd2_2 106.75(18) . . ? O1_2 S1_2 O2_2 116.2(3) . . ? O1_2 S1_2 N1_2 109.9(2) . . ? O2_2 S1_2 N1_2 113.4(2) . . ? O1_2 S1_2 C3_2 107.0(3) . . ? O2_2 S1_2 C3_2 101.2(3) . . ? N1_2 S1_2 C3_2 108.3(2) . . ? P3_2 C1_2 P1_2 116.1(3) . . ? P2_2 C2_2 P4_2 115.7(3) . . ? C12_2 C3_2 C4_2 123.1(8) . . ? C12_2 C3_2 S1_2 120.4(6) . . ? C4_2 C3_2 S1_2 116.4(6) . . ? C5_2 C4_2 C3_2 120.6(8) . . ? C6_2 C5_2 C4_2 118.6(8) . . ? C5_2 C6_2 C11_2 121.9(8) . . ? C5_2 C6_2 C7_2 119.4(9) . . ? C11_2 C6_2 C7_2 118.7(7) . . ? C8_2 C7_2 C6_2 115.7(7) . . ? C7_2 C8_2 C9_2 122.0(8) . . ? C10_2 C9_2 C8_2 119.6(9) . . ? C11_2 C10_2 C9_2 123.1(10) . . ? C10_2 C11_2 C6_2 120.6(8) . . ? C10_2 C11_2 C12_2 120.2(9) . . ? C6_2 C11_2 C12_2 119.2(8) . . ? C3_2 C12_2 C11_2 116.6(8) . . ? C6P_2 C1P_2 C2P_2 118.8(5) . . ? C6P_2 C1P_2 P1_2 124.3(5) . . ? C2P_2 C1P_2 P1_2 116.9(5) . . ? C1P_2 C2P_2 C3P_2 120.2(6) . . ? C4P_2 C3P_2 C2P_2 119.2(7) . . ? C5P_2 C4P_2 C3P_2 121.3(7) . . ? C4P_2 C5P_2 C6P_2 119.8(7) . . ? C1P_2 C6P_2 C5P_2 120.6(6) . . ? C12P_2 C7P_2 C8P_2 118.1(5) . . ? C12P_2 C7P_2 P1_2 121.3(5) . . ? C8P_2 C7P_2 P1_2 120.5(5) . . ? C9P_2 C8P_2 C7P_2 120.3(7) . . ? C10P_2 C9P_2 C8P_2 120.6(8) . . ? C9P_2 C10P_2 C11P_2 120.8(8) . . ? C10P_2 C11P_2 C12P_2 120.0(8) . . ? C7P_2 C12P_2 C11P_2 120.1(6) . . ? C14P_2 C13P_2 C18P_2 118.1(4) . . ? C14P_2 C13P_2 P2_2 122.51(16) . . ? C18P_2 C13P_2 P2_2 119.3(5) . . ? C13P_2 C14P_2 C15P_2 121.6(5) . . ? C16P_2 C15P_2 C14P_2 118.2(8) . . ? C17P_2 C16P_2 C15P_2 122.3(9) . . ? C16P_2 C17P_2 C18P_2 118.5(9) . . ? C13P_2 C18P_2 C17P_2 121.3(8) . . ? C24P_2 C19P_2 C20P_2 118.3(7) . . ? C24P_2 C19P_2 P2_2 120.1(6) . . ? C20P_2 C19P_2 P2_2 121.5(6) . . ? C21P_2 C20P_2 C19P_2 121.0(9) . . ? C22P_2 C21P_2 C20P_2 120.3(9) . . ? C21P_2 C22P_2 C23P_2 121.9(9) . . ? C22P_2 C23P_2 C24P_2 117.7(9) . . ? C19P_2 C24P_2 C23P_2 120.6(8) . . ? C30P_2 C25P_2 C26P_2 115.7(6) . . ? C30P_2 C25P_2 P3_2 124.6(4) . . ? C26P_2 C25P_2 P3_2 119.6(5) . . ? C27P_2 C26P_2 C25P_2 122.2(7) . . ? C28P_2 C27P_2 C26P_2 120.9(7) . . ? C27P_2 C28P_2 C29P_2 117.9(7) . . ? C28P_2 C29P_2 C30P_2 122.1(7) . . ? C25P_2 C30P_2 C29P_2 121.2(6) . . ? C36P_2 C31P_2 C32P_2 119.2(6) . . ? C36P_2 C31P_2 P3_2 121.3(5) . . ? C32P_2 C31P_2 P3_2 119.4(5) . . ? C31P_2 C32P_2 C33P_2 119.7(7) . . ? C34P_2 C33P_2 C32P_2 120.3(7) . . ? C33P_2 C34P_2 C35P_2 120.5(7) . . ? C36P_2 C35P_2 C34P_2 119.7(7) . . ? C35P_2 C36P_2 C31P_2 120.5(7) . . ? C42P_2 C37P_2 C38P_2 117.8(6) . . ? C42P_2 C37P_2 P4_2 117.4(6) . . ? C38P_2 C37P_2 P4_2 124.8(6) . . ? C37P_2 C38P_2 C39P_2 120.3(7) . . ? C40P_2 C39P_2 C38P_2 119.5(8) . . ? C39P_2 C40P_2 C41P_2 121.4(8) . . ? C40P_2 C41P_2 C42P_2 118.3(8) . . ? C37P_2 C42P_2 C41P_2 122.6(8) . . ? C44P_2 C43P_2 C48P_2 120.5(6) . . ? C44P_2 C43P_2 P4_2 120.8(5) . . ? C48P_2 C43P_2 P4_2 118.7(5) . . ? C43P_2 C44P_2 C45P_2 118.0(7) . . ? C46P_2 C45P_2 C44P_2 121.4(8) . . ? C47P_2 C46P_2 C45P_2 120.1(9) . . ? C46P_2 C47P_2 C48P_2 120.7(8) . . ? C47P_2 C48P_2 C43P_2 119.2(7) . . ? Cl7S C1S Cl4S 132.5(9) . . ? Cl7S C1S Cl1S 103.2(7) . . ? Cl4S C1S Cl1S 102.7(7) . . ? Cl7S C1S Cl5S 84.7(8) . . ? Cl4S C1S Cl5S 113.2(8) . . ? Cl1S C1S Cl5S 19.0(9) . . ? Cl7S C1S Cl6S 164.6(8) . . ? Cl4S C1S Cl6S 33.4(5) . . ? Cl1S C1S Cl6S 89.1(8) . . ? Cl5S C1S Cl6S 106.5(10) . . ? Cl7S C1S Cl2S 72.7(7) . . ? Cl4S C1S Cl2S 59.9(10) . . ? Cl1S C1S Cl2S 119.2(7) . . ? Cl5S C1S Cl2S 109.4(8) . . ? Cl6S C1S Cl2S 93.3(10) . . ? Cl7S C1S Cl3S 75.8(8) . . ? Cl4S C1S Cl3S 56.8(11) . . ? Cl1S C1S Cl3S 119.6(7) . . ? Cl5S C1S Cl3S 110.8(8) . . ? Cl6S C1S Cl3S 90.2(11) . . ? Cl2S C1S Cl3S 3.2(8) . . ? Cl5S Cl1S C1S 80.6(6) . . ? Cl5S Cl1S Cl6S 122.1(14) . . ? C1S Cl1S Cl6S 45.5(4) . . ? Cl4S Cl2S C1S 59.9(5) . . ? Cl4S Cl2S Cl7S 113.3(5) . . ? C1S Cl2S Cl7S 53.5(4) . . ? Cl4S Cl3S C1S 61.4(6) . . ? Cl4S Cl3S Cl7S 113.2(5) . . ? C1S Cl3S Cl7S 51.9(4) . . ? Cl4S Cl3S Cl6S 16.7(3) . . ? C1S Cl3S Cl6S 44.9(6) . . ? Cl7S Cl3S Cl6S 96.6(4) . . ? Cl6S Cl4S Cl3S 135.0(6) . . ? Cl6S Cl4S C1S 73.5(3) . . ? Cl3S Cl4S C1S 61.8(6) . . ? Cl6S Cl4S Cl2S 133.4(6) . . ? Cl3S Cl4S Cl2S 1.7(5) . . ? C1S Cl4S Cl2S 60.2(5) . . ? Cl1S Cl5S C1S 80.3(6) . . ? Cl1S Cl5S Cl7S 126.4(10) . . ? C1S Cl5S Cl7S 47.6(4) . . ? Cl4S Cl6S C1S 73.1(4) . . ? Cl4S Cl6S Cl1S 94.8(8) . . ? C1S Cl6S Cl1S 45.4(4) . . ? Cl4S Cl6S Cl3S 28.4(6) . . ? C1S Cl6S Cl3S 45.0(6) . . ? Cl1S Cl6S Cl3S 75.6(6) . . ? C1S Cl7S Cl2S 53.8(4) . . ? C1S Cl7S Cl3S 52.3(4) . . ? Cl2S Cl7S Cl3S 1.7(5) . . ? C1S Cl7S Cl5S 47.7(4) . . ? Cl2S Cl7S Cl5S 80.1(5) . . ? Cl3S Cl7S Cl5S 79.5(5) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 26.81 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.816 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.097 #=END # marked as 3f in paper data_pdfc _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H59 Cl2 Fe N O3 P4 Pd2 S' _chemical_formula_weight 1373.60 _chemical_melting_point ? _chemical_compound_source 'G. Besenyei KKKI' 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' '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.414(2) _cell_length_b 22.267(2) _cell_length_c 44.002(5) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 12163(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.25 _cell_measurement_theta_max 11.97 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5568 _exptl_absorpt_coefficient_mu 1.093 _exptl_absorpt_correction_type 'Empirical (Psi-scan)' _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength .71073 _diffrn_radiation_type MOk\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1 _diffrn_reflns_number 18026 _diffrn_reflns_av_R_equivalents 0.0095 _diffrn_reflns_av_sigmaI/netI 0.1173 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -61 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 29.97 _reflns_number_total 17628 _reflns_number_gt 8915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express' _computing_cell_refinement 'CAD4 Express' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17628 _refine_ls_number_parameters 696 _refine_ls_number_restraints 154 _refine_ls_R_factor_all 0.1215 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0859 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.843 _refine_ls_shift/su_max 1.749 _refine_ls_shift/su_mean 0.055 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.92519(2) 0.158999(11) 0.140752(5) 0.02885(6) Uani 1 d . . . Pd2 Pd 1.02880(2) 0.045994(11) 0.099879(6) 0.02953(6) Uani 1 d . . . Fe1 Fe 1.12706(5) 0.26548(3) 0.029182(13) 0.06119(18) Uani 1 d . . . Cl1 Cl 0.84205(8) 0.19689(5) 0.18413(2) 0.0555(3) Uani 1 d . . . Cl2 Cl 1.08080(8) -0.05463(4) 0.09770(3) 0.0545(3) Uani 1 d . . . S1 S 0.97166(7) 0.17384(3) 0.072385(17) 0.02972(17) Uani 1 d . . . P1 P 0.76074(7) 0.12080(4) 0.125236(19) 0.03229(19) Uani 1 d . . . P2 P 1.09741(7) 0.18273(4) 0.157001(18) 0.02943(18) Uani 1 d . . . P3 P 0.85699(7) 0.02211(4) 0.08214(2) 0.03228(19) Uani 1 d . . . P4 P 1.19105(7) 0.07181(4) 0.122836(19) 0.03059(18) Uani 1 d . . . O1 O 0.9557(2) 0.13757(11) 0.04577(5) 0.0479(7) Uani 1 d . . . O2 O 0.89065(19) 0.21874(10) 0.07832(6) 0.0449(6) Uani 1 d . . . N1 N 0.9916(2) 0.13383(11) 0.10107(5) 0.0274(5) Uani 1 d . . . C1 C 0.7586(3) 0.08261(15) 0.08829(7) 0.0341(7) Uani 1 d . . . H1A H 0.7684 0.1127 0.0726 0.044 Uiso 1 d R . . H1B H 0.6872 0.0658 0.0856 0.044 Uiso 1 d R . . C2 C 1.2029(3) 0.15155(13) 0.13236(7) 0.0312(7) Uani 1 d . . . H2A H 1.2712 0.1576 0.1421 0.040 Uiso 1 d R . . H2B H 1.2036 0.1740 0.1137 0.040 Uiso 1 d R . . C3 C 1.0902(3) 0.21532(16) 0.06572(7) 0.0370(8) Uani 1 d . . . C4 C 1.1084(3) 0.27591(18) 0.07503(9) 0.0545(10) Uani 1 d . . . H4 H 1.0580 0.3017 0.0852 0.071 Uiso 1 d R . . C5 C 1.2153(4) 0.2904(2) 0.06612(10) 0.0728(15) Uani 1 d . . . H5 H 1.2490 0.3289 0.0686 0.095 Uiso 1 d R . . C6 C 1.2619(4) 0.2410(3) 0.05217(10) 0.0732(15) Uani 1 d . . . H6 H 1.3331 0.2401 0.0437 0.095 Uiso 1 d R . . C7 C 1.1861(3) 0.1932(2) 0.05138(8) 0.0531(10) Uani 1 d . . . H7 H 1.1969 0.1535 0.0435 0.069 Uiso 1 d R . . C8 C 1.0181(8) 0.2477(4) -0.00347(17) 0.123(3) Uani 1 d U . . H8 H 0.9691 0.2144 -0.0027 0.160 Uiso 1 d R . . C9 C 1.0009(6) 0.3044(5) 0.00687(15) 0.115(3) Uani 1 d . . . H9 H 0.9342 0.3170 0.0159 0.150 Uiso 1 d R . . C10 C 1.0972(6) 0.3369(3) 0.00206(14) 0.0928(19) Uani 1 d . . . H10 H 1.1060 0.3785 0.0072 0.121 Uiso 1 d R . . C11 C 1.1690(5) 0.2995(4) -0.01223(12) 0.097(2) Uani 1 d . . . H11 H 1.2408 0.3105 -0.0181 0.127 Uiso 1 d R . . C12 C 1.1205(9) 0.2429(4) -0.01533(13) 0.128(3) Uani 1 d . . . H12 H 1.1538 0.2082 -0.0242 0.166 Uiso 1 d R . . C1p C 0.6516(3) 0.17530(15) 0.12247(8) 0.0370(8) Uani 1 d . . . C2p C 0.6378(3) 0.20865(18) 0.09649(9) 0.0501(10) Uani 1 d . . . H2p H 0.6813 0.1999 0.0790 0.065 Uiso 1 d R . . C3p C 0.5607(3) 0.2535(2) 0.09541(11) 0.0675(13) Uani 1 d . . . H3p H 0.5519 0.2765 0.0771 0.088 Uiso 1 d R . . C4p C 0.4972(4) 0.2659(2) 0.11995(12) 0.0683(13) Uani 1 d . . . H4p H 0.4447 0.2976 0.1194 0.089 Uiso 1 d R . . C5p C 0.5104(4) 0.2328(2) 0.14580(10) 0.0684(13) Uani 1 d . . . H5p H 0.4660 0.2404 0.1633 0.089 Uiso 1 d R . . C6p C 0.5869(3) 0.1877(2) 0.14742(9) 0.0551(11) Uani 1 d . . . H6p H 0.5959 0.1650 0.1658 0.072 Uiso 1 d R . . C7p C 0.7130(3) 0.06422(16) 0.15180(8) 0.0406(8) Uani 1 d . . . C8p C 0.6119(3) 0.0383(2) 0.14838(11) 0.0634(12) Uani 1 d . . . H8p H 0.5656 0.0520 0.1323 0.082 Uiso 1 d R . . C9p C 0.5783(4) -0.0058(2) 0.16841(15) 0.0929(18) Uani 1 d . . . H9p H 0.5101 -0.0255 0.1658 0.121 Uiso 1 d R . . C10p C 0.6448(5) -0.0239(2) 0.19167(13) 0.0899(18) Uani 1 d . . . H10p H 0.6202 -0.0527 0.2063 0.117 Uiso 1 d R . . C11p C 0.7458(5) 0.0014(2) 0.19498(10) 0.0789(15) Uani 1 d . . . H11p H 0.7932 -0.0119 0.2108 0.103 Uiso 1 d R . . C12p C 0.7788(4) 0.04540(18) 0.17508(8) 0.0532(10) Uani 1 d . . . H12p H 0.8487 0.0635 0.1769 0.069 Uiso 1 d R . . C13p C 1.1259(3) 0.26240(14) 0.15622(8) 0.0386(8) Uani 1 d . . . C14p C 1.0509(5) 0.2990(2) 0.1675(2) 0.171(4) Uani 1 d U . . H14p H 0.9866 0.2826 0.1745 0.223 Uiso 1 d R . . C15p C 1.0713(7) 0.3597(2) 0.1698(3) 0.220(5) Uani 1 d U . . H15p H 1.0274 0.3841 0.1828 0.286 Uiso 1 d R . . C16p C 1.1617(5) 0.3843(2) 0.15815(17) 0.119(3) Uani 1 d U . . H16p H 1.1704 0.4270 0.1565 0.155 Uiso 1 d R . . C17p C 1.2348(4) 0.34899(18) 0.14677(11) 0.0654(13) Uani 1 d . . . H17p H 1.3010 0.3649 0.1389 0.085 Uiso 1 d R . . C18p C 1.2179(3) 0.28804(17) 0.14553(10) 0.0579(11) Uani 1 d . . . H18p H 1.2726 0.2625 0.1371 0.075 Uiso 1 d R . . C19p C 1.1335(3) 0.16219(16) 0.19590(7) 0.0406(8) Uani 1 d . . . C20p C 1.2295(3) 0.1828(2) 0.20871(9) 0.0577(11) Uani 1 d . . . H20p H 1.2775 0.2067 0.1967 0.075 Uiso 1 d R . . C21p C 1.2537(5) 0.1681(2) 0.23847(10) 0.0780(15) Uani 1 d . . . H21p H 1.3199 0.1819 0.2474 0.101 Uiso 1 d R . . C22p C 1.1846(5) 0.1344(2) 0.25544(10) 0.0831(17) Uani 1 d . . . H22p H 1.2026 0.1255 0.2762 0.108 Uiso 1 d R . . C23p C 1.0917(5) 0.1143(2) 0.24295(10) 0.0824(16) Uani 1 d . . . H23p H 1.0434 0.0911 0.2553 0.107 Uiso 1 d R . . C24p C 1.0663(4) 0.1282(2) 0.21319(9) 0.0593(11) Uani 1 d . . . H24p H 1.0012 0.1131 0.2043 0.077 Uiso 1 d R . . C25p C 0.8490(3) 0.00578(16) 0.04178(8) 0.0401(8) Uani 1 d . . . C26p C 0.9057(3) -0.04344(19) 0.03130(9) 0.0584(11) Uani 1 d . . . H26p H 0.9497 -0.0661 0.0451 0.076 Uiso 1 d R . . C27p C 0.9031(4) -0.0588(2) 0.00090(11) 0.0724(14) Uani 1 d . . . H27p H 0.9423 -0.0933 -0.0061 0.094 Uiso 1 d R . . C28p C 0.8441(4) -0.0264(2) -0.01911(10) 0.0754(15) Uani 1 d . . . H28p H 0.8412 -0.0386 -0.0400 0.098 Uiso 1 d R . . C29p C 0.7899(5) 0.0234(2) -0.00929(10) 0.0862(17) Uani 1 d . . . H29p H 0.7496 0.0467 -0.0237 0.112 Uiso 1 d R . . C30p C 0.7914(4) 0.04009(19) 0.02125(9) 0.0592(12) Uani 1 d . . . H30p H 0.7540 0.0754 0.0279 0.077 Uiso 1 d R . . C31p C 0.7977(3) -0.04566(16) 0.09844(9) 0.0438(8) Uani 1 d U . . C32p C 0.7205(3) -0.0784(2) 0.08226(12) 0.0700(13) Uani 1 d U . . H32p H 0.6959 -0.0641 0.0629 0.091 Uiso 1 d R . . C33p C 0.6797(5) -0.1313(3) 0.09385(17) 0.102(2) Uani 1 d U . . H33p H 0.6261 -0.1532 0.0827 0.133 Uiso 1 d R . . C34p C 0.7132(6) -0.1518(2) 0.12137(18) 0.107(2) Uani 1 d U . . H34p H 0.6839 -0.1890 0.1286 0.139 Uiso 1 d R . . C35p C 0.7894(5) -0.1208(2) 0.13750(13) 0.0854(17) Uani 1 d U . . H35p H 0.8110 -0.1362 0.1570 0.111 Uiso 1 d R . . C36p C 0.8319(4) -0.06779(18) 0.12585(10) 0.0582(11) Uani 1 d U . . H36p H 0.8860 -0.0462 0.1370 0.076 Uiso 1 d R . . C37p C 1.3123(3) 0.05687(15) 0.10057(8) 0.0361(8) Uani 1 d . . . C38p C 1.3717(3) 0.10154(19) 0.08650(9) 0.0488(10) Uani 1 d . . . H38p H 1.3535 0.1429 0.0900 0.063 Uiso 1 d R . . C39p C 1.4550(3) 0.0873(2) 0.06683(10) 0.0625(12) Uani 1 d . . . H39p H 1.4969 0.1184 0.0574 0.081 Uiso 1 d R . . C40p C 1.4790(3) 0.0282(2) 0.06110(11) 0.0690(14) Uani 1 d . . . H40p H 1.5365 0.0187 0.0473 0.090 Uiso 1 d R . . C41p C 1.4240(4) -0.0165(2) 0.07537(12) 0.0771(15) Uani 1 d . . . H41p H 1.4433 -0.0573 0.0708 0.100 Uiso 1 d R . . C42p C 1.3400(3) -0.00241(19) 0.09478(11) 0.0620(12) Uani 1 d . . . H42p H 1.3015 -0.0343 0.1047 0.081 Uiso 1 d R . . C43p C 1.2117(3) 0.03467(15) 0.15910(8) 0.0399(8) Uani 1 d . . . C44p C 1.1288(4) -0.00054(19) 0.17106(10) 0.0601(11) Uani 1 d . . . H44p H 1.0643 -0.0065 0.1594 0.078 Uiso 1 d R . . C45p C 1.1394(5) -0.0266(2) 0.19929(12) 0.0842(16) Uani 1 d . . . H45p H 1.0833 -0.0507 0.2080 0.109 Uiso 1 d R . . C46p C 1.2306(6) -0.0168(2) 0.21538(11) 0.093(2) Uani 1 d . . . H46p H 1.2403 -0.0353 0.2349 0.121 Uiso 1 d R . . C47p C 1.3150(5) 0.0186(2) 0.20477(11) 0.0799(17) Uani 1 d . . . H47p H 1.3780 0.0260 0.2169 0.104 Uiso 1 d R . . C48p C 1.3056(4) 0.04462(18) 0.17575(9) 0.0551(11) Uani 1 d . . . H48p H 1.3632 0.0682 0.1674 0.072 Uiso 1 d R . . O1s O 0.9425(7) -0.1060(4) 0.2389(2) 0.259(4) Uani 1 d DU . . C1s C 0.9237(12) -0.1608(5) 0.2370(3) 0.266(9) Uani 1 d DU . . C2s C 1.0047(12) -0.2058(7) 0.2367(4) 0.348(11) Uani 1 d DU . . H2as H 0.9715 -0.2447 0.2369 0.487 Uiso 1 calc R . . H2bs H 1.0495 -0.2015 0.2544 0.487 Uiso 1 calc R . . H2cs H 1.0479 -0.2016 0.2188 0.487 Uiso 1 calc R . . C3s C 0.8121(12) -0.1756(6) 0.2371(4) 0.360(11) Uani 1 d DU . . H3as H 0.7919 -0.1898 0.2569 0.503 Uiso 1 calc R . . H3bs H 0.7986 -0.2064 0.2223 0.503 Uiso 1 calc R . . H3cs H 0.7706 -0.1405 0.2321 0.503 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02709(12) 0.03424(13) 0.02521(11) -0.00326(10) 0.00362(10) -0.00220(11) Pd2 0.02696(12) 0.02615(11) 0.03547(13) -0.00132(10) -0.00216(11) 0.00266(10) Fe1 0.0556(4) 0.0804(5) 0.0476(3) 0.0312(3) -0.0099(3) -0.0232(3) Cl1 0.0490(6) 0.0760(7) 0.0414(5) -0.0214(5) 0.0186(4) -0.0121(5) Cl2 0.0484(5) 0.0319(5) 0.0832(7) -0.0045(5) -0.0122(5) 0.0094(4) S1 0.0299(4) 0.0318(4) 0.0275(4) 0.0017(3) 0.0014(3) 0.0029(3) P1 0.0260(4) 0.0383(5) 0.0326(4) -0.0055(4) 0.0031(4) -0.0005(4) P2 0.0304(4) 0.0283(4) 0.0296(4) -0.0011(3) -0.0006(3) -0.0032(3) P3 0.0288(4) 0.0324(4) 0.0357(4) -0.0060(4) -0.0012(4) 0.0009(4) P4 0.0273(4) 0.0287(4) 0.0358(4) 0.0007(4) -0.0020(4) 0.0029(3) O1 0.0643(18) 0.0488(15) 0.0304(12) -0.0019(11) -0.0029(12) -0.0089(13) O2 0.0386(14) 0.0404(14) 0.0558(16) 0.0122(12) 0.0077(12) 0.0160(11) N1 0.0301(14) 0.0244(12) 0.0278(13) -0.0023(11) 0.0069(11) 0.0043(10) C1 0.0277(17) 0.0381(19) 0.0366(17) -0.0030(15) -0.0034(15) 0.0023(15) C2 0.0284(17) 0.0290(17) 0.0360(17) 0.0014(13) 0.0005(13) -0.0025(13) C3 0.0348(19) 0.044(2) 0.0319(17) 0.0105(15) 0.0020(14) -0.0007(16) C4 0.051(2) 0.054(3) 0.058(3) 0.011(2) -0.003(2) -0.016(2) C5 0.066(3) 0.086(4) 0.066(3) 0.025(3) -0.017(3) -0.039(3) C6 0.040(2) 0.124(5) 0.056(3) 0.024(3) 0.001(2) -0.020(3) C7 0.039(2) 0.078(3) 0.042(2) 0.012(2) 0.0028(18) -0.001(2) C8 0.120(6) 0.164(8) 0.087(5) 0.079(5) -0.064(5) -0.061(6) C9 0.080(5) 0.175(7) 0.091(5) 0.071(5) -0.020(4) 0.017(5) C10 0.093(5) 0.097(4) 0.088(4) 0.049(4) -0.021(4) -0.017(4) C11 0.097(5) 0.136(6) 0.059(3) 0.056(4) -0.003(3) -0.021(5) C12 0.199(9) 0.130(7) 0.054(4) 0.024(4) -0.045(5) 0.002(7) C1p 0.0288(18) 0.043(2) 0.0393(19) -0.0067(16) 0.0011(15) 0.0034(15) C2p 0.038(2) 0.058(2) 0.053(2) -0.0009(19) 0.0097(18) 0.0126(19) C3p 0.054(3) 0.074(3) 0.075(3) 0.010(2) 0.007(2) 0.024(2) C4p 0.047(3) 0.068(3) 0.090(4) -0.003(3) 0.007(2) 0.021(2) C5p 0.051(3) 0.090(3) 0.065(3) -0.013(3) 0.016(2) 0.025(3) C6p 0.041(2) 0.073(3) 0.052(2) -0.002(2) 0.0103(19) 0.015(2) C7p 0.039(2) 0.042(2) 0.0407(19) -0.0035(16) 0.0081(16) -0.0052(16) C8p 0.042(2) 0.064(3) 0.085(3) 0.018(2) 0.005(2) -0.012(2) C9p 0.062(3) 0.083(4) 0.133(5) 0.035(4) 0.025(4) -0.015(3) C10p 0.106(5) 0.069(3) 0.095(4) 0.029(3) 0.025(4) -0.023(3) C11p 0.112(4) 0.071(3) 0.053(3) 0.015(2) 0.002(3) -0.010(3) C12p 0.065(3) 0.052(2) 0.043(2) 0.0024(19) -0.003(2) -0.010(2) C13p 0.042(2) 0.0287(17) 0.046(2) -0.0020(15) 0.0023(17) -0.0046(15) C14p 0.115(5) 0.033(3) 0.366(11) -0.016(5) 0.158(7) 0.000(3) C15p 0.173(7) 0.031(3) 0.455(14) -0.030(5) 0.201(9) -0.007(4) C16p 0.125(5) 0.029(2) 0.204(7) -0.014(3) 0.085(5) -0.013(3) C17p 0.064(3) 0.039(2) 0.093(3) -0.004(2) 0.015(3) -0.014(2) C18p 0.043(2) 0.039(2) 0.092(3) -0.006(2) 0.014(2) -0.0029(18) C19p 0.052(2) 0.0400(19) 0.0300(17) -0.0027(15) -0.0058(16) 0.0053(18) C20p 0.058(3) 0.070(3) 0.046(2) -0.003(2) -0.017(2) -0.007(2) C21p 0.086(4) 0.088(4) 0.059(3) -0.010(3) -0.039(3) 0.006(3) C22p 0.133(5) 0.074(3) 0.042(3) 0.005(2) -0.020(3) 0.003(4) C23p 0.104(4) 0.095(4) 0.049(3) 0.021(3) -0.002(3) -0.020(3) C24p 0.067(3) 0.070(3) 0.041(2) 0.009(2) -0.007(2) -0.015(2) C25p 0.037(2) 0.044(2) 0.0388(19) -0.0118(16) -0.0031(16) 0.0003(16) C26p 0.060(3) 0.063(3) 0.052(2) -0.018(2) -0.003(2) 0.014(2) C27p 0.078(4) 0.069(3) 0.070(3) -0.034(3) 0.008(3) 0.009(3) C28p 0.096(4) 0.088(4) 0.043(2) -0.027(3) 0.001(3) -0.011(3) C29p 0.116(5) 0.095(4) 0.048(3) -0.011(3) -0.029(3) 0.014(3) C30p 0.074(3) 0.060(3) 0.042(2) -0.015(2) -0.011(2) 0.017(2) C31p 0.040(2) 0.0361(18) 0.055(2) -0.0032(18) 0.0061(18) 0.0024(17) C32p 0.050(3) 0.062(3) 0.099(4) -0.010(3) 0.004(3) -0.019(2) C33p 0.088(4) 0.071(4) 0.147(6) -0.013(4) 0.017(4) -0.040(3) C34p 0.109(5) 0.052(3) 0.160(7) 0.013(4) 0.059(5) -0.019(3) C35p 0.087(4) 0.069(3) 0.100(4) 0.033(3) 0.030(3) 0.005(3) C36p 0.060(3) 0.051(2) 0.064(3) 0.007(2) 0.015(2) 0.004(2) C37p 0.0238(16) 0.042(2) 0.0420(19) -0.0070(16) -0.0060(15) 0.0025(14) C38p 0.036(2) 0.058(2) 0.052(2) 0.0064(19) 0.0022(18) 0.0068(19) C39p 0.040(2) 0.092(4) 0.056(3) 0.009(2) 0.011(2) -0.002(2) C40p 0.035(2) 0.103(4) 0.069(3) -0.031(3) 0.006(2) 0.008(3) C41p 0.043(3) 0.077(3) 0.112(4) -0.047(3) 0.012(3) 0.006(3) C42p 0.040(2) 0.051(2) 0.095(3) -0.021(2) 0.011(2) 0.0043(19) C43p 0.049(2) 0.0314(19) 0.0398(19) -0.0013(15) -0.0020(17) 0.0086(16) C44p 0.067(3) 0.058(3) 0.055(3) 0.012(2) -0.001(2) 0.002(2) C45p 0.109(5) 0.082(4) 0.062(3) 0.024(3) 0.006(3) -0.005(3) C46p 0.165(7) 0.064(3) 0.050(3) 0.015(3) -0.002(4) 0.008(4) C47p 0.120(5) 0.058(3) 0.062(3) -0.010(2) -0.045(3) 0.018(3) C48p 0.066(3) 0.045(2) 0.054(2) -0.0047(19) -0.027(2) 0.008(2) O1s 0.299(10) 0.184(7) 0.295(10) 0.059(7) 0.124(8) -0.014(7) C1s 0.36(2) 0.148(12) 0.294(16) 0.091(13) 0.151(17) -0.009(14) C2s 0.34(2) 0.270(18) 0.44(2) -0.020(17) 0.029(18) 0.155(16) C3s 0.49(3) 0.173(12) 0.42(2) 0.039(13) 0.09(2) -0.088(16) _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 2.010(2) . y Pd1 P1 2.3146(9) . y Pd1 P2 2.3154(9) . y Pd1 Cl1 2.3282(9) . y Pd2 N1 2.010(2) . y Pd2 P4 2.3255(9) . y Pd2 P3 2.3326(9) . y Pd2 Cl2 2.3337(9) . y Fe1 C3 2.010(3) . y Fe1 C8 2.013(6) . y Fe1 C7 2.020(4) . y Fe1 C10 2.022(5) . y Fe1 C12 2.023(6) . y Fe1 C6 2.030(5) . y Fe1 C5 2.037(4) . y Fe1 C11 2.041(5) . y Fe1 C9 2.041(6) . y Fe1 C4 2.044(4) . y S1 O1 1.436(2) . y S1 O2 1.442(2) . y S1 N1 1.565(3) . y S1 C3 1.762(3) . y P1 C7p 1.818(4) . y P1 C1p 1.823(3) . ? P1 C1 1.835(3) . y P2 C13p 1.809(3) . y P2 C19p 1.828(3) . y P2 C2 1.836(3) . y P3 C25p 1.815(3) . y P3 C31p 1.826(4) . y P3 C1 1.838(3) . y P4 C43p 1.816(4) . y P4 C37p 1.827(3) . y P4 C2 1.830(3) . y C3 C4 1.428(5) . y C3 C7 1.434(5) . y C4 C5 1.421(6) . y C5 C6 1.387(7) . y C6 C7 1.420(6) . y C8 C9 1.358(10) . y C8 C12 1.379(10) . y C9 C10 1.414(9) . y C10 C11 1.372(8) . y C11 C12 1.402(9) . y C1p C2p 1.374(5) . ? C1p C6p 1.389(5) . ? C2p C3p 1.384(5) . ? C3p C4p 1.365(6) . ? C4p C5p 1.365(6) . ? C5p C6p 1.384(6) . ? C7p C12p 1.375(5) . ? C7p C8p 1.390(5) . ? C8p C9p 1.384(6) . ? C9p C10p 1.376(7) . ? C10p C11p 1.382(7) . ? C11p C12p 1.376(6) . ? C13p C14p 1.332(6) . ? C13p C18p 1.361(5) . ? C14p C15p 1.380(7) . ? C15p C16p 1.348(8) . ? C16p C17p 1.300(6) . ? C17p C18p 1.374(5) . ? C19p C24p 1.360(5) . ? C19p C20p 1.395(5) . ? C20p C21p 1.383(6) . ? C21p C22p 1.362(7) . ? C22p C23p 1.354(7) . ? C23p C24p 1.382(6) . ? C25p C26p 1.382(5) . ? C25p C30p 1.383(5) . ? C26p C27p 1.381(6) . ? C27p C28p 1.354(7) . ? C28p C29p 1.367(7) . ? C29p C30p 1.394(5) . ? C31p C36p 1.370(5) . ? C31p C32p 1.399(5) . ? C32p C33p 1.380(7) . ? C33p C34p 1.359(9) . ? C34p C35p 1.368(8) . ? C35p C36p 1.391(6) . ? C37p C38p 1.384(5) . ? C37p C42p 1.388(5) . ? C38p C39p 1.385(5) . ? C39p C40p 1.373(6) . ? C40p C41p 1.361(7) . ? C41p C42p 1.384(6) . ? C43p C44p 1.396(5) . ? C43p C48p 1.395(5) . ? C44p C45p 1.377(6) . ? C45p C46p 1.352(8) . ? C46p C47p 1.392(8) . ? C47p C48p 1.407(6) . ? O1s1 C1s 1.245(6) . ? C1s1 C2s 1.421(6) . ? C1s1 C3s 1.424(6) . ? 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 P1 90.17(8) . . y N1 Pd1 P2 87.32(8) . . y P1 Pd1 P2 171.63(3) . . y N1 Pd1 Cl1 174.14(8) . . y P1 Pd1 Cl1 89.09(3) . . y P2 Pd1 Cl1 94.21(3) . . y N1 Pd2 P4 86.98(8) . . y N1 Pd2 P3 91.16(8) . . y P4 Pd2 P3 173.55(3) . . y N1 Pd2 Cl2 177.10(8) . . y P4 Pd2 Cl2 90.89(3) . . y P3 Pd2 Cl2 91.16(3) . . y C3 Fe1 C8 108.0(2) . . ? C3 Fe1 C7 41.69(14) . . ? C8 Fe1 C7 115.6(3) . . ? C3 Fe1 C10 150.1(3) . . ? C8 Fe1 C10 67.1(3) . . ? C7 Fe1 C10 168.0(2) . . ? C3 Fe1 C12 128.8(3) . . ? C8 Fe1 C12 39.9(3) . . ? C7 Fe1 C12 106.6(3) . . ? C10 Fe1 C12 67.5(3) . . ? C3 Fe1 C6 68.88(15) . . ? C8 Fe1 C6 149.0(4) . . ? C7 Fe1 C6 41.04(18) . . ? C10 Fe1 C6 131.0(2) . . ? C12 Fe1 C6 116.7(3) . . ? C3 Fe1 C5 68.64(16) . . ? C8 Fe1 C5 169.9(4) . . ? C7 Fe1 C5 68.67(19) . . ? C10 Fe1 C5 110.8(2) . . ? C12 Fe1 C5 149.5(4) . . ? C6 Fe1 C5 39.89(19) . . ? C3 Fe1 C11 168.0(3) . . ? C8 Fe1 C11 66.9(3) . . ? C7 Fe1 C11 129.4(3) . . ? C10 Fe1 C11 39.5(2) . . ? C12 Fe1 C11 40.4(3) . . ? C6 Fe1 C11 109.5(2) . . ? C5 Fe1 C11 118.3(2) . . ? C3 Fe1 C9 116.5(2) . . ? C8 Fe1 C9 39.1(3) . . ? C7 Fe1 C9 148.1(3) . . ? C10 Fe1 C9 40.7(2) . . ? C12 Fe1 C9 67.0(3) . . ? C6 Fe1 C9 170.4(3) . . ? C5 Fe1 C9 132.9(3) . . ? C11 Fe1 C9 67.0(3) . . ? C3 Fe1 C4 41.24(14) . . ? C8 Fe1 C4 130.6(3) . . ? C7 Fe1 C4 69.77(17) . . ? C10 Fe1 C4 118.2(3) . . ? C12 Fe1 C4 168.2(3) . . ? C6 Fe1 C4 68.41(18) . . ? C5 Fe1 C4 40.74(17) . . ? C11 Fe1 C4 150.2(3) . . ? C9 Fe1 C4 109.9(3) . . ? O1 S1 O2 116.20(16) . . y O1 S1 N1 111.06(14) . . y O2 S1 N1 111.03(14) . . y O1 S1 C3 105.90(16) . . y O2 S1 C3 104.44(16) . . y N1 S1 C3 107.51(15) . . y C7p P1 C1p 105.21(16) . . y C7p P1 C1 104.11(16) . . y C1p P1 C1 103.80(15) . . y C7p P1 Pd1 110.63(12) . . y C1p P1 Pd1 115.50(11) . . y C1 P1 Pd1 116.39(11) . . y C13p P2 C19p 102.42(16) . . y C13p P2 C2 102.73(15) . . y C19p P2 C2 106.47(16) . . y C13p P2 Pd1 113.48(12) . . y C19p P2 Pd1 117.30(13) . . y C2 P2 Pd1 112.93(11) . . y C25p P3 C31p 101.34(17) . . y C25p P3 C1 104.75(15) . . y C31p P3 C1 106.25(16) . . y C25p P3 Pd2 115.01(12) . . y C31p P3 Pd2 115.20(13) . . y C1 P3 Pd2 113.03(11) . . y C43p P4 C37p 105.81(16) . . y C43p P4 C2 103.26(15) . . y C37p P4 C2 103.50(15) . . y C43p P4 Pd2 113.03(13) . . y C37p P4 Pd2 115.84(11) . . y C2 P4 Pd2 114.12(11) . . y S1 N1 Pd2 124.69(14) . . y S1 N1 Pd1 118.50(14) . . y Pd2 N1 Pd1 112.84(11) . . y P1 C1 P3 117.42(17) . . y P4 C2 P2 116.43(17) . . y C4 C3 C7 108.6(3) . . y C4 C3 S1 125.4(3) . . y C7 C3 S1 125.9(3) . . y C4 C3 Fe1 70.7(2) . . ? C7 C3 Fe1 69.5(2) . . ? S1 C3 Fe1 127.90(18) . . ? C5 C4 C3 106.5(4) . . y C5 C4 Fe1 69.4(3) . . ? C3 C4 Fe1 68.1(2) . . ? C6 C5 C4 109.3(4) . . y C6 C5 Fe1 69.8(3) . . ? C4 C5 Fe1 69.9(2) . . ? C5 C6 C7 109.2(4) . . y C5 C6 Fe1 70.3(3) . . ? C7 C6 Fe1 69.1(2) . . ? C6 C7 C3 106.4(4) . . y C6 C7 Fe1 69.9(3) . . ? C3 C7 Fe1 68.8(2) . . ? C9 C8 C12 110.1(8) . . y C9 C8 Fe1 71.6(4) . . ? C12 C8 Fe1 70.4(4) . . ? C8 C9 C10 107.0(7) . . y C8 C9 Fe1 69.3(4) . . ? C10 C9 Fe1 68.9(3) . . ? C11 C10 C9 107.8(7) . . y C11 C10 Fe1 71.0(3) . . ? C9 C10 Fe1 70.4(3) . . ? C10 C11 C12 108.1(7) . . y C10 C11 Fe1 69.5(3) . . ? C12 C11 Fe1 69.2(3) . . ? C8 C12 C11 106.8(8) . . y C8 C12 Fe1 69.6(4) . . ? C11 C12 Fe1 70.5(4) . . ? C2p C1p C6p 118.6(3) . . y C2p C1p P1 120.5(3) . . ? C6p C1p P1 120.7(3) . . ? C1p C2p C3p 120.3(4) . . ? C4p C3p C2p 121.2(4) . . ? C3p C4p C5p 118.7(4) . . ? C4p C5p C6p 121.1(4) . . ? C5p C6p C1p 120.1(4) . . ? C12p C7p C8p 119.3(4) . . ? C12p C7p P1 119.8(3) . . ? C8p C7p P1 120.8(3) . . ? C9p C8p C7p 119.9(5) . . ? C10p C9p C8p 120.0(5) . . ? C9p C10p C11p 120.3(5) . . ? C12p C11p C10p 119.5(5) . . ? C7p C12p C11p 121.0(4) . . ? C14p C13p C18p 117.3(4) . . ? C14p C13p P2 117.1(3) . . ? C18p C13p P2 125.6(3) . . ? C13p C14p C15p 119.9(5) . . ? C16p C15p C14p 121.5(5) . . ? C17p C16p C15p 118.8(5) . . ? C16p C17p C18p 120.4(4) . . ? C13p C18p C17p 121.9(4) . . ? C24p C19p C20p 118.7(3) . . ? C24p C19p P2 120.9(3) . . ? C20p C19p P2 120.4(3) . . ? C21p C20p C19p 119.4(4) . . ? C22p C21p C20p 120.8(5) . . ? C23p C22p C21p 119.7(4) . . ? C22p C23p C24p 120.4(5) . . ? C19p C24p C23p 121.0(4) . . ? C26p C25p C30p 118.9(3) . . ? C26p C25p P3 117.2(3) . . ? C30p C25p P3 123.8(3) . . ? C25p C26p C27p 120.5(4) . . ? C28p C27p C26p 120.7(4) . . ? C27p C28p C29p 119.6(4) . . ? C28p C29p C30p 120.9(5) . . ? C25p C30p C29p 119.3(4) . . ? C36p C31p C32p 118.2(4) . . ? C36p C31p P3 121.2(3) . . ? C32p C31p P3 120.5(3) . . ? C33p C32p C31p 120.5(5) . . ? C34p C33p C32p 120.2(6) . . ? C33p C34p C35p 120.3(5) . . ? C34p C35p C36p 119.9(5) . . ? C31p C36p C35p 120.8(5) . . ? C38p C37p C42p 118.0(3) . . ? C38p C37p P4 123.2(3) . . ? C42p C37p P4 118.4(3) . . ? C39p C38p C37p 120.8(4) . . ? C40p C39p C38p 119.8(4) . . ? C41p C40p C39p 120.5(4) . . ? C40p C41p C42p 119.8(4) . . ? C41p C42p C37p 121.1(4) . . ? C44p C43p C48p 120.5(4) . . ? C44p C43p P4 118.9(3) . . ? C48p C43p P4 120.5(3) . . ? C45p C44p C43p 120.4(5) . . ? C46p C45p C44p 119.0(5) . . ? C45p C46p C47p 123.0(5) . . ? C46p C47p C48p 118.4(5) . . ? C43p C48p C47p 118.7(4) . . ? O1s1 C1s C2s 124.0(15) . . ? O1s1 C1s C3s 114.1(11) . . ? C2s1 C1s C3s 121.7(13) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.795 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.104 # end of file --- end of file --- end of file --- end of file --- end of file