Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Zuideveld, Martin A.' ; Institute of Molecular Chemistry Universiteit van Amsterdam Nieuwew Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Swennenhuis, Bert H.G.' ; Institute of Molecular Chemistry Universiteit van Amsterdam Nieuwew Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Boele, Maarten D.K.' ; Institute of Molecular Chemistry Universiteit van Amsterdam Nieuwew Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Guari, Yannick' ; Institute of Molecular Chemistry Universiteit van Amsterdam Nieuwew Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'van Strijdonck, Gino P.F.' ; Institute of Molecular Chemistry Universiteit van Amsterdam Nieuwew Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Reek, Joost N.H.' ; Institute of Molecular Chemistry Universiteit van Amsterdam Nieuwew Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Kamer, Paul C.J.' ; Institute of Molecular Chemistry Universiteit van Amsterdam Nieuwew Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Goubitz, Kees' ; Dept. Crystallography Universiteit van Amsterdam Nieuwew Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Fraanje, Jan' ; Dept. Crystallography Universiteit van Amsterdam Nieuwew Achtergracht 166 1018 WV Amsterdam The Netherlands ; 'Lutz, Martin' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Spek, Anthony L.' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'van Leeuwen, Piet W.N.M.' ; Institute of Molecular Chemistry Universiteit van Amsterdam Nieuwew Achtergracht 166 1018 WV Amsterdam The Netherlands ; _publ_contact_author_name 'Prof Piet W. N. M. van Leeuwen' _publ_contact_author_address ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email 'pwnm@science.uva.nl ' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The Coordination Behaviour of Large Natural Bite Angle Diphosphine Ligands towards Methyl and 4-Cyanophenylpalladium(II) Complexes ; data_s2031a _database_code_CSD 133392 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H36 Br N O P2 Pd, 0.58(C H2 Cl2)' _chemical_formula_sum 'C46.58 H37.16 Br Cl1.16 N O P2 Pd' _chemical_formula_weight 916.27 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' 'Br' 'Br' -0.2901 2.4595 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.8648(2) _cell_length_b 10.0742(1) _cell_length_c 22.7549(2) _cell_angle_alpha 90.00 _cell_angle_beta 119.142(1) _cell_angle_gamma 90.00 _cell_volume 4377.76(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'red-brown' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1849 _exptl_absorpt_coefficient_mu 1.515 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78748 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10040 _reflns_number_gt 9150 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'COLLECT data collection software, Nonius B.V., 1998.' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'DIRDIF-97 (Beurskens et al., 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+9.0473P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constraint _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10040 _refine_ls_number_parameters 525 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.234232(10) 0.15253(2) 0.407781(10) 0.01552(8) Uani 1 1 d . . . Br2 Br 0.153891(15) 0.16477(3) 0.281733(14) 0.02135(9) Uani 1 1 d . . . P3 P 0.32586(4) 0.22644(8) 0.39352(4) 0.01863(15) Uani 1 1 d . . . P4 P 0.14283(4) 0.19485(7) 0.42928(3) 0.01615(14) Uani 1 1 d . . . C5 C 0.29637(15) 0.3887(3) 0.35143(14) 0.0208(6) Uani 1 1 d . . . C6 C 0.32529(16) 0.4398(3) 0.31322(15) 0.0262(6) Uani 1 1 d . . . H6 H 0.3608 0.3913 0.3100 0.031 Uiso 1 1 calc R . . C7 C 0.30285(18) 0.5601(4) 0.28006(16) 0.0306(7) Uani 1 1 d . . . H7 H 0.3235 0.5940 0.2548 0.037 Uiso 1 1 calc R . . C8 C 0.25051(18) 0.6310(3) 0.28353(17) 0.0296(7) Uani 1 1 d . . . H8 H 0.2346 0.7120 0.2595 0.036 Uiso 1 1 calc R . . C9 C 0.22061(16) 0.5855(3) 0.32176(15) 0.0233(6) Uani 1 1 d . . . C10 C 0.24466(15) 0.4646(3) 0.35538(14) 0.0198(5) Uani 1 1 d . . . O11 O 0.21778(10) 0.4183(2) 0.39580(10) 0.0191(4) Uani 1 1 d . . . C12 C 0.14845(14) 0.4490(3) 0.37627(14) 0.0197(5) Uani 1 1 d . . . C13 C 0.12074(16) 0.5699(3) 0.34443(15) 0.0231(6) Uani 1 1 d . . . C14 C 0.05180(18) 0.5997(3) 0.32830(17) 0.0289(7) Uani 1 1 d . . . H14 H 0.0316 0.6812 0.3064 0.035 Uiso 1 1 calc R . . C15 C 0.01245(17) 0.5134(3) 0.34351(17) 0.0297(7) Uani 1 1 d . . . H15 H -0.0338 0.5366 0.3332 0.036 Uiso 1 1 calc R . . C16 C 0.04078(16) 0.3921(3) 0.37405(15) 0.0243(6) Uani 1 1 d . . . H16 H 0.0133 0.3325 0.3838 0.029 Uiso 1 1 calc R . . C17 C 0.10913(15) 0.3570(3) 0.39051(14) 0.0190(5) Uani 1 1 d . . . C18 C 0.16671(18) 0.6659(3) 0.33095(16) 0.0257(6) Uani 1 1 d . . . C19 C 0.1222(2) 0.7535(3) 0.26922(18) 0.0346(8) Uani 1 1 d . . . H19A H 0.0979 0.6973 0.2292 0.052 Uiso 1 1 calc R . . H19B H 0.1527 0.8162 0.2628 0.052 Uiso 1 1 calc R . . H19C H 0.0877 0.8026 0.2764 0.052 Uiso 1 1 calc R . . C20 C 0.2063(2) 0.7567(4) 0.39335(19) 0.0383(8) Uani 1 1 d . . . H20A H 0.1724 0.8090 0.4001 0.057 Uiso 1 1 calc R . . H20B H 0.2374 0.8165 0.3862 0.057 Uiso 1 1 calc R . . H20C H 0.2341 0.7019 0.4332 0.057 Uiso 1 1 calc R . . C21 C 0.35459(16) 0.1328(3) 0.34263(15) 0.0224(6) Uani 1 1 d . . . C22 C 0.41694(17) 0.1635(4) 0.34240(18) 0.0303(7) Uani 1 1 d . . . H22 H 0.4462 0.2324 0.3706 0.036 Uiso 1 1 calc R . . C23 C 0.43632(19) 0.0938(4) 0.30127(19) 0.0358(8) Uani 1 1 d . . . H23 H 0.4781 0.1168 0.3006 0.043 Uiso 1 1 calc R . . C24 C 0.3947(2) -0.0093(4) 0.26117(19) 0.0369(8) Uani 1 1 d . . . H24 H 0.4078 -0.0566 0.2328 0.044 Uiso 1 1 calc R . . C25 C 0.33425(19) -0.0428(4) 0.26277(18) 0.0351(8) Uani 1 1 d . . . H25 H 0.3063 -0.1145 0.2361 0.042 Uiso 1 1 calc R . . C26 C 0.31371(17) 0.0277(3) 0.30315(17) 0.0278(6) Uani 1 1 d . . . H26 H 0.2719 0.0041 0.3037 0.033 Uiso 1 1 calc R . . C27 C 0.40735(15) 0.2641(4) 0.46975(15) 0.0274(7) Uani 1 1 d . . . C28 C 0.4229(2) 0.3916(4) 0.49703(19) 0.0432(9) Uani 1 1 d . . . H28 H 0.3940 0.4644 0.4727 0.052 Uiso 1 1 calc R . . C29 C 0.4809(3) 0.4116(6) 0.5602(2) 0.0644(15) Uani 1 1 d . . . H29 H 0.4911 0.4980 0.5794 0.077 Uiso 1 1 calc R . . C30 C 0.5241(2) 0.3059(6) 0.5953(2) 0.0642(15) Uani 1 1 d . . . H30 H 0.5640 0.3205 0.6380 0.077 Uiso 1 1 calc R . . C31 C 0.5092(2) 0.1801(6) 0.5684(2) 0.0521(12) Uani 1 1 d . . . H31 H 0.5391 0.1083 0.5925 0.063 Uiso 1 1 calc R . . C32 C 0.45048(18) 0.1572(4) 0.50599(18) 0.0366(8) Uani 1 1 d . . . H32 H 0.4397 0.0698 0.4881 0.044 Uiso 1 1 calc R . . C33 C 0.06481(14) 0.0895(3) 0.39812(14) 0.0189(5) Uani 1 1 d . . . C34 C 0.02431(16) 0.0854(3) 0.43036(16) 0.0266(6) Uani 1 1 d . . . H34 H 0.0376 0.1367 0.4698 0.032 Uiso 1 1 calc R . . C35 C -0.03555(17) 0.0061(4) 0.40474(17) 0.0314(7) Uani 1 1 d . . . H35 H -0.0628 0.0034 0.4269 0.038 Uiso 1 1 calc R . . C36 C -0.05557(16) -0.0687(3) 0.34704(17) 0.0280(6) Uani 1 1 d . . . H36 H -0.0963 -0.1226 0.3298 0.034 Uiso 1 1 calc R . . C37 C -0.01582(16) -0.0647(3) 0.31463(15) 0.0232(6) Uani 1 1 d . . . H37 H -0.0296 -0.1154 0.2750 0.028 Uiso 1 1 calc R . . C38 C 0.04439(15) 0.0137(3) 0.34009(15) 0.0204(5) Uani 1 1 d . . . H38 H 0.0716 0.0156 0.3179 0.024 Uiso 1 1 calc R . . C39 C 0.16613(15) 0.2190(3) 0.51694(14) 0.0213(6) Uani 1 1 d . . . C40 C 0.1678(2) 0.3427(4) 0.54446(18) 0.0334(8) Uani 1 1 d . . . H40 H 0.1542 0.4198 0.5170 0.040 Uiso 1 1 calc R . . C41 C 0.1897(2) 0.3525(5) 0.6134(2) 0.0472(11) Uani 1 1 d . . . H41 H 0.1903 0.4369 0.6323 0.057 Uiso 1 1 calc R . . C42 C 0.2101(2) 0.2429(5) 0.65384(18) 0.0439(10) Uani 1 1 d . . . H42 H 0.2257 0.2513 0.7006 0.053 Uiso 1 1 calc R . . C43 C 0.20798(17) 0.1197(4) 0.62638(17) 0.0349(8) Uani 1 1 d . . . H43 H 0.2212 0.0430 0.6542 0.042 Uiso 1 1 calc R . . C44 C 0.18667(16) 0.1074(4) 0.55833(16) 0.0270(6) Uani 1 1 d . . . H44 H 0.1861 0.0225 0.5399 0.032 Uiso 1 1 calc R . . C45 C 0.29927(15) 0.1299(3) 0.50694(14) 0.0206(6) Uani 1 1 d . . . C46 C 0.32294(15) 0.2380(3) 0.55087(15) 0.0240(6) Uani 1 1 d . . . H46 H 0.3095 0.3253 0.5335 0.029 Uiso 1 1 calc R . . C47 C 0.36592(16) 0.2198(4) 0.61961(15) 0.0277(7) Uani 1 1 d . . . H47 H 0.3817 0.2940 0.6491 0.033 Uiso 1 1 calc R . . C48 C 0.38567(16) 0.0915(4) 0.64499(15) 0.0285(7) Uani 1 1 d . . . C49 C 0.36317(17) -0.0168(4) 0.60178(16) 0.0305(7) Uani 1 1 d . . . H49 H 0.3768 -0.1040 0.6191 0.037 Uiso 1 1 calc R . . C50 C 0.32047(16) 0.0032(3) 0.53288(16) 0.0268(6) Uani 1 1 d . . . H50 H 0.3057 -0.0709 0.5033 0.032 Uiso 1 1 calc R . . C51 C 0.42886(18) 0.0710(4) 0.71689(17) 0.0365(8) Uani 1 1 d . . . N52 N 0.46312(18) 0.0567(4) 0.77352(15) 0.0502(10) Uani 1 1 d . . . C53 C 0.1046(3) 0.7721(8) -0.0014(4) 0.044(2) Uani 0.46 1 d PD . . H53A H 0.1059 0.8124 -0.0405 0.053 Uiso 0.46 1 calc PR . . H53B H 0.0876 0.6798 -0.0140 0.053 Uiso 0.46 1 calc PR . . Cl54 Cl 0.04456(18) 0.8573(2) 0.01158(19) 0.0694(9) Uani 0.46 1 d PD . . Cl55 Cl 0.1890(2) 0.7660(3) 0.06453(16) 0.0842(11) Uani 0.46 1 d PD . . C56 C 0.3894(15) 0.907(3) 0.077(2) 0.070(13) Uani 0.12 1 d PD . . H56A H 0.4302 0.9063 0.1226 0.084 Uiso 0.12 1 calc PR . . H56B H 0.3858 0.9982 0.0586 0.084 Uiso 0.12 1 calc PR . . Cl57 Cl 0.4063(4) 0.7997(8) 0.0276(5) 0.0475(19) Uani 0.12 1 d PD . . Cl58 Cl 0.3154(5) 0.8769(11) 0.0827(5) 0.056(2) Uani 0.12 1 d PD . . 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 0.01290(11) 0.01898(13) 0.01304(11) 0.00082(7) 0.00503(9) -0.00031(7) Br2 0.01759(14) 0.02797(17) 0.01524(14) 0.00135(10) 0.00544(11) -0.00243(10) P3 0.0136(3) 0.0249(4) 0.0160(3) 0.0007(3) 0.0061(3) -0.0013(3) P4 0.0146(3) 0.0189(3) 0.0144(3) 0.0007(3) 0.0067(3) 0.0000(3) C5 0.0180(13) 0.0244(15) 0.0166(12) -0.0015(11) 0.0057(11) -0.0062(11) C6 0.0216(14) 0.0341(17) 0.0223(14) -0.0008(12) 0.0100(12) -0.0071(12) C7 0.0331(17) 0.0337(18) 0.0265(15) 0.0022(13) 0.0157(14) -0.0107(14) C8 0.0335(17) 0.0252(15) 0.0255(15) 0.0037(12) 0.0106(14) -0.0069(13) C9 0.0270(14) 0.0197(14) 0.0198(13) -0.0016(11) 0.0086(12) -0.0046(11) C10 0.0203(13) 0.0207(14) 0.0161(12) -0.0015(10) 0.0070(10) -0.0067(11) O11 0.0182(9) 0.0202(10) 0.0185(9) 0.0018(8) 0.0086(8) -0.0004(8) C12 0.0191(13) 0.0215(14) 0.0154(12) -0.0018(10) 0.0059(10) 0.0010(11) C13 0.0287(15) 0.0178(14) 0.0200(13) -0.0011(11) 0.0096(12) 0.0011(11) C14 0.0312(16) 0.0218(15) 0.0283(15) 0.0028(12) 0.0104(13) 0.0084(12) C15 0.0232(15) 0.0310(17) 0.0309(16) 0.0022(13) 0.0100(13) 0.0094(13) C16 0.0207(14) 0.0270(16) 0.0235(14) 0.0012(12) 0.0094(12) 0.0019(12) C17 0.0203(13) 0.0193(13) 0.0156(12) 0.0004(10) 0.0073(11) 0.0016(10) C18 0.0333(17) 0.0162(14) 0.0247(15) 0.0004(11) 0.0118(13) -0.0011(11) C19 0.044(2) 0.0227(16) 0.0354(18) 0.0087(14) 0.0181(16) 0.0051(14) C20 0.052(2) 0.0253(17) 0.0361(19) -0.0110(14) 0.0202(17) -0.0116(16) C21 0.0199(13) 0.0287(15) 0.0205(13) 0.0032(11) 0.0112(11) 0.0029(11) C22 0.0221(15) 0.039(2) 0.0311(17) 0.0012(13) 0.0142(14) -0.0003(13) C23 0.0292(16) 0.047(2) 0.0394(19) 0.0070(16) 0.0234(15) 0.0070(15) C24 0.0411(19) 0.043(2) 0.0362(18) 0.0038(16) 0.0263(16) 0.0131(16) C25 0.0371(18) 0.0353(19) 0.0353(18) -0.0056(15) 0.0196(15) 0.0024(15) C26 0.0257(15) 0.0297(17) 0.0301(16) -0.0004(13) 0.0154(13) 0.0014(12) C27 0.0169(13) 0.0435(19) 0.0190(13) 0.0022(13) 0.0065(11) -0.0072(13) C28 0.040(2) 0.045(2) 0.0281(18) -0.0005(16) 0.0041(16) -0.0202(17) C29 0.065(3) 0.067(3) 0.033(2) -0.004(2) 0.001(2) -0.040(3) C30 0.039(2) 0.094(4) 0.030(2) 0.006(2) -0.0056(18) -0.034(3) C31 0.0246(18) 0.087(4) 0.031(2) 0.018(2) 0.0027(16) 0.002(2) C32 0.0210(16) 0.057(2) 0.0258(17) 0.0058(15) 0.0066(14) 0.0047(15) C33 0.0161(12) 0.0195(13) 0.0197(13) 0.0020(10) 0.0076(10) -0.0008(10) C34 0.0242(14) 0.0351(17) 0.0234(14) -0.0042(12) 0.0139(12) -0.0050(13) C35 0.0266(15) 0.0423(19) 0.0320(17) -0.0028(14) 0.0195(14) -0.0075(14) C36 0.0222(14) 0.0290(16) 0.0308(16) 0.0004(13) 0.0114(13) -0.0064(12) C37 0.0240(14) 0.0193(14) 0.0246(14) -0.0019(11) 0.0104(12) -0.0026(11) C38 0.0199(13) 0.0192(14) 0.0234(14) 0.0005(11) 0.0116(11) 0.0009(10) C39 0.0174(13) 0.0302(16) 0.0167(13) -0.0011(11) 0.0086(11) -0.0010(11) C40 0.0351(18) 0.037(2) 0.0243(16) -0.0049(13) 0.0115(15) 0.0056(14) C41 0.049(2) 0.059(3) 0.0285(19) -0.0156(17) 0.0155(18) 0.0076(19) C42 0.0341(18) 0.079(3) 0.0182(15) -0.0030(17) 0.0125(14) 0.0032(19) C43 0.0240(16) 0.058(2) 0.0212(15) 0.0081(15) 0.0102(13) -0.0024(15) C44 0.0215(14) 0.0362(18) 0.0223(14) 0.0040(13) 0.0100(12) -0.0024(13) C45 0.0146(12) 0.0317(15) 0.0147(12) 0.0018(11) 0.0067(10) -0.0023(11) C46 0.0196(13) 0.0300(16) 0.0207(14) -0.0001(12) 0.0085(11) -0.0015(12) C47 0.0207(14) 0.0411(19) 0.0191(14) -0.0059(13) 0.0079(12) -0.0021(13) C48 0.0187(14) 0.047(2) 0.0178(14) 0.0021(13) 0.0073(11) 0.0040(13) C49 0.0272(15) 0.0369(18) 0.0241(15) 0.0083(13) 0.0098(13) 0.0076(13) C50 0.0236(14) 0.0309(16) 0.0217(14) -0.0022(12) 0.0077(12) 0.0014(12) C51 0.0251(16) 0.060(2) 0.0234(16) 0.0029(16) 0.0113(13) 0.0112(16) N52 0.0389(17) 0.087(3) 0.0209(14) 0.0066(16) 0.0117(13) 0.0197(18) C53 0.079(6) 0.026(4) 0.040(4) 0.001(3) 0.039(5) 0.005(4) Cl54 0.106(2) 0.0365(12) 0.128(3) 0.0104(13) 0.106(2) -0.0036(12) Cl55 0.109(3) 0.0281(12) 0.0675(18) -0.0086(11) 0.0058(17) 0.0170(14) C56 0.09(3) 0.04(2) 0.07(3) 0.00(2) 0.03(3) 0.02(2) Cl57 0.041(4) 0.035(4) 0.065(5) -0.003(4) 0.026(4) 0.001(3) Cl58 0.056(5) 0.060(6) 0.046(5) -0.010(4) 0.019(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C45 2.010(3) . ? Pd1 P3 2.3037(7) . ? Pd1 P4 2.3167(7) . ? Pd1 Br2 2.5339(3) . ? P3 C27 1.822(3) . ? P3 C21 1.826(3) . ? P3 C5 1.845(3) . ? P4 C39 1.819(3) . ? P4 C17 1.832(3) . ? P4 C33 1.833(3) . ? C5 C6 1.399(4) . ? C5 C10 1.404(4) . ? C6 C7 1.385(5) . ? C6 H6 0.9500 . ? C7 C8 1.383(5) . ? C7 H7 0.9500 . ? C8 C9 1.396(4) . ? C8 H8 0.9500 . ? C9 C10 1.397(4) . ? C9 C18 1.526(5) . ? C10 O11 1.391(3) . ? O11 C12 1.391(3) . ? C12 C13 1.395(4) . ? C12 C17 1.405(4) . ? C13 C14 1.399(4) . ? C13 C18 1.530(4) . ? C14 C15 1.381(5) . ? C14 H14 0.9500 . ? C15 C16 1.393(5) . ? C15 H15 0.9500 . ? C16 C17 1.398(4) . ? C16 H16 0.9500 . ? C18 C19 1.538(5) . ? C18 C20 1.551(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.395(5) . ? C21 C22 1.400(4) . ? C22 C23 1.391(5) . ? C22 H22 0.9500 . ? C23 C24 1.390(6) . ? C23 H23 0.9500 . ? C24 C25 1.383(5) . ? C24 H24 0.9500 . ? C25 C26 1.397(5) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.394(6) . ? C27 C32 1.404(5) . ? C28 C29 1.393(5) . ? C28 H28 0.9500 . ? C29 C30 1.388(8) . ? C29 H29 0.9500 . ? C30 C31 1.376(8) . ? C30 H30 0.9500 . ? C31 C32 1.393(5) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.397(4) . ? C33 C34 1.399(4) . ? C34 C35 1.395(4) . ? C34 H34 0.9500 . ? C35 C36 1.387(5) . ? C35 H35 0.9500 . ? C36 C37 1.387(4) . ? C36 H36 0.9500 . ? C37 C38 1.396(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.388(5) . ? C39 C44 1.393(5) . ? C40 C41 1.403(5) . ? C40 H40 0.9500 . ? C41 C42 1.366(7) . ? C41 H41 0.9500 . ? C42 C43 1.380(6) . ? C42 H42 0.9500 . ? C43 C44 1.388(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C50 1.388(5) . ? C45 C46 1.396(4) . ? C46 C47 1.390(4) . ? C46 H46 0.9500 . ? C47 C48 1.395(5) . ? C47 H47 0.9500 . ? C48 C49 1.388(5) . ? C48 C51 1.451(4) . ? C49 C50 1.394(4) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 N52 1.141(5) . ? C53 Cl54 1.711(6) . ? C53 Cl55 1.722(7) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C56 Cl58 1.718(10) . ? C56 Cl57 1.720(10) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? 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 C45 Pd1 P3 90.37(8) . . ? C45 Pd1 P4 89.73(8) . . ? P3 Pd1 P4 150.35(3) . . ? C45 Pd1 Br2 176.12(9) . . ? P3 Pd1 Br2 89.76(2) . . ? P4 Pd1 Br2 92.076(19) . . ? C27 P3 C21 103.45(15) . . ? C27 P3 C5 104.01(15) . . ? C21 P3 C5 105.64(14) . . ? C27 P3 Pd1 116.60(10) . . ? C21 P3 Pd1 120.92(11) . . ? C5 P3 Pd1 104.56(9) . . ? C39 P4 C17 103.96(14) . . ? C39 P4 C33 102.26(13) . . ? C17 P4 C33 104.47(13) . . ? C39 P4 Pd1 116.51(9) . . ? C17 P4 Pd1 104.38(10) . . ? C33 P4 Pd1 123.20(10) . . ? C6 C5 C10 117.5(3) . . ? C6 C5 P3 119.9(2) . . ? C10 C5 P3 122.6(2) . . ? C7 C6 C5 120.9(3) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C8 C7 C6 120.3(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 121.2(3) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C10 117.5(3) . . ? C8 C9 C18 122.6(3) . . ? C10 C9 C18 119.8(3) . . ? O11 C10 C9 119.1(3) . . ? O11 C10 C5 118.2(3) . . ? C9 C10 C5 122.7(3) . . ? C12 O11 C10 117.4(2) . . ? O11 C12 C13 119.3(3) . . ? O11 C12 C17 118.3(3) . . ? C13 C12 C17 122.4(3) . . ? C12 C13 C14 117.6(3) . . ? C12 C13 C18 119.6(3) . . ? C14 C13 C18 122.7(3) . . ? C15 C14 C13 121.5(3) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 119.8(3) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C17 120.9(3) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 117.7(3) . . ? C16 C17 P4 118.8(2) . . ? C12 C17 P4 123.5(2) . . ? C9 C18 C13 108.6(2) . . ? C9 C18 C19 111.5(3) . . ? C13 C18 C19 111.1(3) . . ? C9 C18 C20 108.3(3) . . ? C13 C18 C20 108.5(3) . . ? C19 C18 C20 108.7(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 119.0(3) . . ? C26 C21 P3 119.3(2) . . ? C22 C21 P3 121.7(3) . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.2(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 119.6(3) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 120.8(3) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C21 C26 C25 119.9(3) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C32 119.8(3) . . ? C28 C27 P3 121.9(3) . . ? C32 C27 P3 117.7(3) . . ? C29 C28 C27 119.6(4) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C30 C29 C28 120.3(5) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 120.2(4) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C30 C31 C32 120.4(4) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C27 119.6(4) . . ? C31 C32 H32 120.2 . . ? C27 C32 H32 120.2 . . ? C38 C33 C34 119.1(3) . . ? C38 C33 P4 119.4(2) . . ? C34 C33 P4 121.4(2) . . ? C35 C34 C33 120.1(3) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 120.4(3) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C37 119.8(3) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C38 120.3(3) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C33 120.3(3) . . ? C37 C38 H38 119.9 . . ? C33 C38 H38 119.9 . . ? C40 C39 C44 119.4(3) . . ? C40 C39 P4 123.1(2) . . ? C44 C39 P4 117.4(2) . . ? C39 C40 C41 119.2(3) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C42 C41 C40 121.2(4) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C41 C42 C43 119.6(3) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C42 C43 C44 120.3(4) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 120.3(3) . . ? C43 C44 H44 119.8 . . ? C39 C44 H44 119.8 . . ? C50 C45 C46 118.8(3) . . ? C50 C45 Pd1 119.3(2) . . ? C46 C45 Pd1 121.9(2) . . ? C47 C46 C45 121.0(3) . . ? C47 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? C46 C47 C48 119.4(3) . . ? C46 C47 H47 120.3 . . ? C48 C47 H47 120.3 . . ? C49 C48 C47 120.2(3) . . ? C49 C48 C51 119.9(3) . . ? C47 C48 C51 119.9(3) . . ? C48 C49 C50 119.7(3) . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C45 C50 C49 120.9(3) . . ? C45 C50 H50 119.6 . . ? C49 C50 H50 119.6 . . ? N52 C51 C48 179.0(5) . . ? Cl54 C53 Cl55 117.0(5) . . ? Cl54 C53 H53A 108.0 . . ? Cl55 C53 H53A 108.0 . . ? Cl54 C53 H53B 108.0 . . ? Cl55 C53 H53B 108.0 . . ? H53A C53 H53B 107.3 . . ? Cl58 C56 Cl57 116.5(10) . . ? Cl58 C56 H56A 108.2 . . ? Cl57 C56 H56A 108.2 . . ? Cl58 C56 H56B 108.2 . . ? Cl57 C56 H56B 108.2 . . ? H56A C56 H56B 107.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C45 Pd1 P3 C27 -11.07(17) . . . . ? P4 Pd1 P3 C27 79.03(15) . . . . ? Br2 Pd1 P3 C27 172.81(14) . . . . ? C45 Pd1 P3 C21 116.03(15) . . . . ? P4 Pd1 P3 C21 -153.88(12) . . . . ? Br2 Pd1 P3 C21 -60.09(12) . . . . ? C45 Pd1 P3 C5 -125.26(13) . . . . ? P4 Pd1 P3 C5 -35.17(11) . . . . ? Br2 Pd1 P3 C5 58.61(10) . . . . ? C45 Pd1 P4 C39 10.01(15) . . . . ? P3 Pd1 P4 C39 -80.25(13) . . . . ? Br2 Pd1 P4 C39 -173.42(12) . . . . ? C45 Pd1 P4 C17 123.98(13) . . . . ? P3 Pd1 P4 C17 33.72(11) . . . . ? Br2 Pd1 P4 C17 -59.45(10) . . . . ? C45 Pd1 P4 C33 -117.59(14) . . . . ? P3 Pd1 P4 C33 152.14(11) . . . . ? Br2 Pd1 P4 C33 58.97(11) . . . . ? C27 P3 C5 C6 80.8(3) . . . . ? C21 P3 C5 C6 -27.8(3) . . . . ? Pd1 P3 C5 C6 -156.4(2) . . . . ? C27 P3 C5 C10 -99.9(2) . . . . ? C21 P3 C5 C10 151.6(2) . . . . ? Pd1 P3 C5 C10 22.9(3) . . . . ? C10 C5 C6 C7 -0.7(4) . . . . ? P3 C5 C6 C7 178.6(2) . . . . ? C5 C6 C7 C8 -0.9(5) . . . . ? C6 C7 C8 C9 1.9(5) . . . . ? C7 C8 C9 C10 -1.1(5) . . . . ? C7 C8 C9 C18 175.4(3) . . . . ? C8 C9 C10 O11 177.8(3) . . . . ? C18 C9 C10 O11 1.3(4) . . . . ? C8 C9 C10 C5 -0.6(4) . . . . ? C18 C9 C10 C5 -177.2(3) . . . . ? C6 C5 C10 O11 -177.0(2) . . . . ? P3 C5 C10 O11 3.7(4) . . . . ? C6 C5 C10 C9 1.5(4) . . . . ? P3 C5 C10 C9 -177.9(2) . . . . ? C9 C10 O11 C12 32.6(4) . . . . ? C5 C10 O11 C12 -148.9(3) . . . . ? C10 O11 C12 C13 -33.6(4) . . . . ? C10 O11 C12 C17 147.4(3) . . . . ? O11 C12 C13 C14 -177.2(3) . . . . ? C17 C12 C13 C14 1.8(4) . . . . ? O11 C12 C13 C18 0.6(4) . . . . ? C17 C12 C13 C18 179.5(3) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? C18 C13 C14 C15 -177.4(3) . . . . ? C13 C14 C15 C16 -1.7(5) . . . . ? C14 C15 C16 C17 0.9(5) . . . . ? C15 C16 C17 C12 1.1(4) . . . . ? C15 C16 C17 P4 -179.0(2) . . . . ? O11 C12 C17 C16 176.5(2) . . . . ? C13 C12 C17 C16 -2.5(4) . . . . ? O11 C12 C17 P4 -3.5(4) . . . . ? C13 C12 C17 P4 177.5(2) . . . . ? C39 P4 C17 C16 -78.9(3) . . . . ? C33 P4 C17 C16 28.0(3) . . . . ? Pd1 P4 C17 C16 158.5(2) . . . . ? C39 P4 C17 C12 101.1(3) . . . . ? C33 P4 C17 C12 -152.1(2) . . . . ? Pd1 P4 C17 C12 -21.5(3) . . . . ? C8 C9 C18 C13 153.4(3) . . . . ? C10 C9 C18 C13 -30.3(4) . . . . ? C8 C9 C18 C19 30.6(4) . . . . ? C10 C9 C18 C19 -153.0(3) . . . . ? C8 C9 C18 C20 -89.0(4) . . . . ? C10 C9 C18 C20 87.4(3) . . . . ? C12 C13 C18 C9 29.3(4) . . . . ? C14 C13 C18 C9 -153.1(3) . . . . ? C12 C13 C18 C19 152.3(3) . . . . ? C14 C13 C18 C19 -30.1(4) . . . . ? C12 C13 C18 C20 -88.2(3) . . . . ? C14 C13 C18 C20 89.4(4) . . . . ? C27 P3 C21 C26 143.4(3) . . . . ? C5 P3 C21 C26 -107.6(3) . . . . ? Pd1 P3 C21 C26 10.6(3) . . . . ? C27 P3 C21 C22 -36.3(3) . . . . ? C5 P3 C21 C22 72.7(3) . . . . ? Pd1 P3 C21 C22 -169.1(2) . . . . ? C26 C21 C22 C23 2.7(5) . . . . ? P3 C21 C22 C23 -177.6(3) . . . . ? C21 C22 C23 C24 -1.6(5) . . . . ? C22 C23 C24 C25 -0.4(6) . . . . ? C23 C24 C25 C26 1.4(6) . . . . ? C22 C21 C26 C25 -1.7(5) . . . . ? P3 C21 C26 C25 178.5(3) . . . . ? C24 C25 C26 C21 -0.3(5) . . . . ? C21 P3 C27 C28 131.9(3) . . . . ? C5 P3 C27 C28 21.7(3) . . . . ? Pd1 P3 C27 C28 -92.8(3) . . . . ? C21 P3 C27 C32 -56.8(3) . . . . ? C5 P3 C27 C32 -167.0(3) . . . . ? Pd1 P3 C27 C32 78.5(3) . . . . ? C32 C27 C28 C29 -0.2(6) . . . . ? P3 C27 C28 C29 171.0(4) . . . . ? C27 C28 C29 C30 1.4(7) . . . . ? C28 C29 C30 C31 -1.0(8) . . . . ? C29 C30 C31 C32 -0.5(8) . . . . ? C30 C31 C32 C27 1.6(6) . . . . ? C28 C27 C32 C31 -1.3(5) . . . . ? P3 C27 C32 C31 -172.8(3) . . . . ? C39 P4 C33 C38 -159.1(2) . . . . ? C17 P4 C33 C38 92.8(2) . . . . ? Pd1 P4 C33 C38 -25.6(3) . . . . ? C39 P4 C33 C34 22.3(3) . . . . ? C17 P4 C33 C34 -85.8(3) . . . . ? Pd1 P4 C33 C34 155.8(2) . . . . ? C38 C33 C34 C35 0.2(5) . . . . ? P4 C33 C34 C35 178.8(3) . . . . ? C33 C34 C35 C36 -0.3(5) . . . . ? C34 C35 C36 C37 0.0(5) . . . . ? C35 C36 C37 C38 0.4(5) . . . . ? C36 C37 C38 C33 -0.5(5) . . . . ? C34 C33 C38 C37 0.2(4) . . . . ? P4 C33 C38 C37 -178.4(2) . . . . ? C17 P4 C39 C40 -10.2(3) . . . . ? C33 P4 C39 C40 -118.7(3) . . . . ? Pd1 P4 C39 C40 104.0(3) . . . . ? C17 P4 C39 C44 173.2(2) . . . . ? C33 P4 C39 C44 64.7(3) . . . . ? Pd1 P4 C39 C44 -72.5(2) . . . . ? C44 C39 C40 C41 -0.4(5) . . . . ? P4 C39 C40 C41 -176.9(3) . . . . ? C39 C40 C41 C42 0.8(6) . . . . ? C40 C41 C42 C43 -1.3(7) . . . . ? C41 C42 C43 C44 1.4(6) . . . . ? C42 C43 C44 C39 -1.1(5) . . . . ? C40 C39 C44 C43 0.6(5) . . . . ? P4 C39 C44 C43 177.3(2) . . . . ? P3 Pd1 C45 C50 -104.7(2) . . . . ? P4 Pd1 C45 C50 105.0(2) . . . . ? P3 Pd1 C45 C46 76.4(2) . . . . ? P4 Pd1 C45 C46 -73.9(2) . . . . ? C50 C45 C46 C47 -1.2(4) . . . . ? Pd1 C45 C46 C47 177.7(2) . . . . ? C45 C46 C47 C48 0.0(5) . . . . ? C46 C47 C48 C49 0.7(5) . . . . ? C46 C47 C48 C51 -178.2(3) . . . . ? C47 C48 C49 C50 -0.3(5) . . . . ? C51 C48 C49 C50 178.7(3) . . . . ? C46 C45 C50 C49 1.7(5) . . . . ? Pd1 C45 C50 C49 -177.3(2) . . . . ? C48 C49 C50 C45 -0.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.181 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.114 # Compound 1a data_s1867b _database_code_CSD 133393 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H32 Br N O P2 Pd' _chemical_formula_sum 'C43 H32 Br N O P2 Pd' _chemical_formula_weight 826.95 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' 'Br' 'Br' -0.2901 2.4595 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.308(2) _cell_length_b 10.5695(19) _cell_length_c 16.309(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.245(9) _cell_angle_gamma 90.00 _cell_volume 3500.6(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 1.799 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 0.87 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4T' _diffrn_measurement_method 'omega/2theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6387 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6143 _reflns_number_gt 4053 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Locally modified CAD4-Version 5 Software' _computing_cell_refinement 'SET4 (de Boer & Duisenberg, 1984)' _computing_data_reduction 'HELENA (Spek, 1997)' _computing_structure_solution 'DIFABS-97 (Beurskens et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material 'manually editing of SHELXL results' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+4.8964P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constraint _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6143 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1006 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.25321(2) 0.53542(5) 0.69142(3) 0.01599(12) Uani 1 1 d . . . Br1 Br 0.30382(3) 0.72261(6) 0.75699(4) 0.02817(18) Uani 1 1 d . . . P1 P 0.35190(7) 0.51153(15) 0.61089(10) 0.0183(4) Uani 1 1 d . . . P2 P 0.18302(7) 0.40082(15) 0.62344(9) 0.0164(4) Uani 1 1 d . . . O1 O 0.31215(18) 0.2536(4) 0.6157(2) 0.0245(10) Uani 1 1 d . . . N1 N 0.0138(3) 0.6642(6) 1.0219(4) 0.0520(19) Uani 1 1 d . . . C1 C 0.3299(3) 0.2835(6) 0.5346(4) 0.0214(14) Uani 1 1 d . . . C2 C 0.3520(3) 0.4049(6) 0.5221(4) 0.0182(14) Uani 1 1 d . . . C3 C 0.3723(3) 0.4390(6) 0.4438(4) 0.0233(15) Uani 1 1 d . . . H3 H 0.3875 0.5226 0.4337 0.028 Uiso 1 1 calc R . . C4 C 0.3703(3) 0.3521(7) 0.3811(4) 0.0297(17) Uani 1 1 d . . . H4 H 0.3840 0.3765 0.3277 0.036 Uiso 1 1 calc R . . C5 C 0.3487(3) 0.2288(6) 0.3944(4) 0.0303(16) Uani 1 1 d . . . H5 H 0.3482 0.1690 0.3510 0.036 Uiso 1 1 calc R . . C6 C 0.3277(3) 0.1946(6) 0.4726(4) 0.0286(16) Uani 1 1 d . . . H6 H 0.3120 0.1114 0.4831 0.034 Uiso 1 1 calc R . . C7 C 0.2579(3) 0.1742(6) 0.6239(4) 0.0226(14) Uani 1 1 d . . . C8 C 0.1943(3) 0.2290(5) 0.6261(3) 0.0157(13) Uani 1 1 d . . . C9 C 0.1405(3) 0.1466(6) 0.6283(3) 0.0205(14) Uani 1 1 d . . . H9 H 0.0970 0.1798 0.6281 0.025 Uiso 1 1 calc R . . C10 C 0.1502(3) 0.0167(6) 0.6308(3) 0.0273(16) Uani 1 1 d . . . H10 H 0.1132 -0.0383 0.6304 0.033 Uiso 1 1 calc R . . C11 C 0.2125(3) -0.0336(7) 0.6339(4) 0.0294(15) Uani 1 1 d . . . H11 H 0.2184 -0.1225 0.6382 0.035 Uiso 1 1 calc R . . C12 C 0.2671(3) 0.0459(6) 0.6306(4) 0.0276(15) Uani 1 1 d . . . H12 H 0.3103 0.0117 0.6330 0.033 Uiso 1 1 calc R . . C13 C 0.3822(3) 0.6578(6) 0.5658(4) 0.0199(14) Uani 1 1 d . . . C14 C 0.3389(3) 0.7360(6) 0.5242(4) 0.0342(17) Uani 1 1 d . . . H14 H 0.2935 0.7147 0.5228 0.041 Uiso 1 1 calc R . . C15 C 0.3598(4) 0.8436(6) 0.4849(4) 0.0353(18) Uani 1 1 d . . . H15 H 0.3294 0.8934 0.4543 0.042 Uiso 1 1 calc R . . C16 C 0.4244(4) 0.8788(6) 0.4898(4) 0.0325(17) Uani 1 1 d . . . H16 H 0.4388 0.9553 0.4651 0.039 Uiso 1 1 calc R . . C17 C 0.4683(4) 0.8033(7) 0.5306(4) 0.0373(18) Uani 1 1 d . . . H17 H 0.5134 0.8269 0.5332 0.045 Uiso 1 1 calc R . . C18 C 0.4477(3) 0.6929(6) 0.5682(4) 0.0268(16) Uani 1 1 d . . . H18 H 0.4789 0.6409 0.5958 0.032 Uiso 1 1 calc R . . C19 C 0.4227(3) 0.4552(6) 0.6707(4) 0.0204(13) Uani 1 1 d . . . C20 C 0.4370(3) 0.5084(7) 0.7458(4) 0.040(2) Uani 1 1 d . . . H20 H 0.4071 0.5675 0.7690 0.049 Uiso 1 1 calc R . . C21 C 0.4939(4) 0.4776(8) 0.7883(4) 0.050(2) Uani 1 1 d . . . H21 H 0.5029 0.5162 0.8398 0.060 Uiso 1 1 calc R . . C22 C 0.5372(3) 0.3924(7) 0.7566(4) 0.0335(18) Uani 1 1 d . . . H22 H 0.5763 0.3714 0.7859 0.040 Uiso 1 1 calc R . . C23 C 0.5242(3) 0.3371(7) 0.6826(4) 0.0355(18) Uani 1 1 d . . . H23 H 0.5539 0.2764 0.6607 0.043 Uiso 1 1 calc R . . C24 C 0.4673(3) 0.3700(6) 0.6389(4) 0.0347(18) Uani 1 1 d . . . H24 H 0.4592 0.3331 0.5867 0.042 Uiso 1 1 calc R . . C25 C 0.1851(3) 0.4425(6) 0.5152(3) 0.0172(14) Uani 1 1 d . . . C26 C 0.1836(3) 0.3538(6) 0.4521(4) 0.0230(15) Uani 1 1 d . . . H26 H 0.1779 0.2666 0.4642 0.028 Uiso 1 1 calc R . . C27 C 0.1905(3) 0.3933(7) 0.3713(4) 0.0282(16) Uani 1 1 d . . . H27 H 0.1898 0.3327 0.3283 0.034 Uiso 1 1 calc R . . C28 C 0.1983(3) 0.5194(8) 0.3532(4) 0.0338(17) Uani 1 1 d . . . H28 H 0.2047 0.5456 0.2981 0.041 Uiso 1 1 calc R . . C29 C 0.1970(3) 0.6075(7) 0.4153(4) 0.0301(17) Uani 1 1 d . . . H29 H 0.2004 0.6949 0.4025 0.036 Uiso 1 1 calc R . . C30 C 0.1908(3) 0.5702(6) 0.4958(4) 0.0260(16) Uani 1 1 d . . . H30 H 0.1903 0.6318 0.5382 0.031 Uiso 1 1 calc R . . C31 C 0.0970(3) 0.4234(6) 0.6520(4) 0.0210(15) Uani 1 1 d . . . C32 C 0.0746(3) 0.3772(6) 0.7269(4) 0.0204(14) Uani 1 1 d . . . H32 H 0.1019 0.3221 0.7581 0.024 Uiso 1 1 calc R . . C33 C 0.0134(3) 0.4101(6) 0.7564(4) 0.0279(16) Uani 1 1 d . . . H33 H -0.0011 0.3787 0.8078 0.033 Uiso 1 1 calc R . . C34 C -0.0268(3) 0.4888(6) 0.7109(4) 0.0261(16) Uani 1 1 d . . . H34 H -0.0684 0.5138 0.7318 0.031 Uiso 1 1 calc R . . C35 C -0.0064(3) 0.5313(7) 0.6349(4) 0.0296(15) Uani 1 1 d . . . H35 H -0.0347 0.5830 0.6027 0.036 Uiso 1 1 calc R . . C36 C 0.0557(3) 0.4983(6) 0.6053(4) 0.0226(15) Uani 1 1 d . . . H36 H 0.0695 0.5274 0.5530 0.027 Uiso 1 1 calc R . . C37 C 0.1826(3) 0.5633(5) 0.7761(4) 0.0180(14) Uani 1 1 d . . . C38 C 0.1877(3) 0.4968(5) 0.8496(4) 0.0201(14) Uani 1 1 d . . . H38 H 0.2217 0.4360 0.8566 0.024 Uiso 1 1 calc R . . C39 C 0.1430(3) 0.5189(6) 0.9136(4) 0.0274(15) Uani 1 1 d . . . H39 H 0.1463 0.4718 0.9630 0.033 Uiso 1 1 calc R . . C40 C 0.0940(3) 0.6099(6) 0.9043(4) 0.0255(15) Uani 1 1 d . . . C41 C 0.0887(3) 0.6759(6) 0.8308(4) 0.0240(15) Uani 1 1 d . . . H41 H 0.0546 0.7365 0.8234 0.029 Uiso 1 1 calc R . . C42 C 0.1335(3) 0.6529(6) 0.7678(4) 0.0214(14) Uani 1 1 d . . . H42 H 0.1302 0.6998 0.7183 0.026 Uiso 1 1 calc R . . C43 C 0.0495(4) 0.6388(7) 0.9714(4) 0.0339(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0162(2) 0.0172(2) 0.0146(2) -0.0015(2) 0.00036(17) 0.0000(2) Br1 0.0248(3) 0.0256(4) 0.0341(4) -0.0100(3) -0.0008(3) -0.0023(3) P1 0.0178(8) 0.0171(9) 0.0201(8) 0.0002(7) 0.0017(6) 0.0004(7) P2 0.0167(8) 0.0184(9) 0.0143(8) 0.0009(7) 0.0009(7) -0.0001(7) O1 0.023(2) 0.023(2) 0.028(3) -0.003(2) 0.0016(19) -0.002(2) N1 0.070(5) 0.049(5) 0.037(4) -0.004(4) 0.028(4) 0.015(4) C1 0.016(3) 0.026(4) 0.023(3) -0.001(3) 0.001(3) 0.002(3) C2 0.012(3) 0.020(3) 0.023(3) -0.003(3) 0.002(3) 0.005(3) C3 0.023(3) 0.024(4) 0.023(3) 0.005(3) 0.002(3) -0.003(3) C4 0.031(4) 0.042(5) 0.017(3) -0.007(3) 0.006(3) 0.001(3) C5 0.028(4) 0.029(4) 0.034(4) -0.012(3) 0.002(3) -0.006(3) C6 0.027(4) 0.021(4) 0.038(4) -0.007(3) 0.005(3) -0.004(3) C7 0.025(3) 0.024(4) 0.018(3) 0.000(3) 0.001(3) -0.006(3) C8 0.021(3) 0.016(3) 0.010(3) 0.004(3) -0.002(2) -0.001(3) C9 0.026(3) 0.026(4) 0.010(3) -0.001(3) 0.002(3) 0.001(3) C10 0.041(4) 0.024(4) 0.017(3) -0.003(3) 0.004(3) -0.016(3) C11 0.046(4) 0.019(3) 0.024(3) 0.002(3) 0.000(3) -0.006(4) C12 0.035(4) 0.020(4) 0.028(4) 0.001(3) 0.000(3) 0.005(3) C13 0.028(3) 0.015(3) 0.017(3) -0.002(3) 0.004(3) 0.004(3) C14 0.037(4) 0.025(4) 0.041(4) 0.006(4) 0.000(3) -0.002(3) C15 0.051(5) 0.022(4) 0.033(4) 0.003(3) -0.009(4) 0.007(4) C16 0.052(5) 0.021(4) 0.025(4) 0.004(3) 0.008(3) -0.004(4) C17 0.044(4) 0.036(5) 0.032(4) -0.001(4) 0.011(4) -0.009(4) C18 0.030(4) 0.016(4) 0.034(4) 0.003(3) -0.001(3) -0.005(3) C19 0.019(3) 0.016(3) 0.026(3) 0.004(3) -0.003(3) 0.002(3) C20 0.038(4) 0.054(5) 0.029(4) -0.010(4) -0.010(3) 0.021(4) C21 0.050(5) 0.083(6) 0.017(4) -0.010(4) -0.008(3) 0.035(5) C22 0.029(4) 0.045(5) 0.026(4) 0.009(4) -0.006(3) 0.007(4) C23 0.027(4) 0.035(4) 0.044(5) -0.008(4) -0.001(3) 0.012(3) C24 0.036(4) 0.031(4) 0.037(4) -0.011(4) -0.008(3) 0.012(3) C25 0.016(3) 0.022(4) 0.014(3) -0.002(3) -0.004(2) 0.002(3) C26 0.027(4) 0.023(4) 0.019(3) -0.003(3) 0.001(3) -0.001(3) C27 0.035(4) 0.034(4) 0.015(4) -0.002(3) -0.005(3) -0.001(3) C28 0.030(4) 0.054(5) 0.017(3) 0.007(4) 0.000(3) 0.001(4) C29 0.032(4) 0.030(4) 0.028(4) 0.012(3) -0.002(3) -0.006(3) C30 0.028(4) 0.025(4) 0.024(4) 0.001(3) -0.001(3) 0.004(3) C31 0.019(3) 0.024(4) 0.021(3) -0.009(3) 0.001(3) -0.008(3) C32 0.022(3) 0.021(3) 0.019(3) -0.003(3) -0.005(3) -0.003(3) C33 0.028(4) 0.033(4) 0.022(4) -0.002(3) 0.009(3) -0.005(3) C34 0.022(3) 0.030(4) 0.027(4) -0.006(3) 0.005(3) -0.003(3) C35 0.026(3) 0.037(4) 0.026(3) 0.004(4) -0.004(3) 0.008(4) C36 0.022(3) 0.029(4) 0.016(3) 0.005(3) 0.001(3) 0.001(3) C37 0.017(3) 0.018(4) 0.019(3) -0.001(3) 0.001(3) -0.002(3) C38 0.024(3) 0.016(4) 0.021(3) -0.001(3) -0.008(3) 0.004(3) C39 0.042(4) 0.029(4) 0.011(3) 0.005(3) 0.004(3) 0.001(3) C40 0.027(4) 0.022(4) 0.027(4) -0.004(3) 0.005(3) -0.003(3) C41 0.025(3) 0.020(4) 0.026(4) -0.003(3) 0.002(3) 0.002(3) C42 0.027(3) 0.019(3) 0.018(3) 0.006(3) 0.001(3) -0.001(3) C43 0.044(4) 0.025(4) 0.032(4) -0.002(3) -0.001(4) 0.002(3) _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 C37 2.016(6) . ? Pd1 P2 2.2959(17) . ? Pd1 P1 2.4142(16) . ? Pd1 Br1 2.4709(9) . ? P1 C13 1.820(6) . ? P1 C19 1.834(6) . ? P1 C2 1.835(6) . ? P2 C25 1.820(6) . ? P2 C31 1.825(6) . ? P2 C8 1.831(6) . ? O1 C7 1.392(7) . ? O1 C1 1.410(7) . ? N1 C43 1.134(8) . ? C1 C2 1.374(8) . ? C1 C6 1.381(8) . ? C2 C3 1.391(8) . ? C3 C4 1.376(8) . ? C3 H3 0.9500 . ? C4 C5 1.392(9) . ? C4 H4 0.9500 . ? C5 C6 1.394(9) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.373(9) . ? C7 C8 1.416(8) . ? C8 C9 1.399(8) . ? C9 C10 1.388(9) . ? C9 H9 0.9500 . ? C10 C11 1.373(9) . ? C10 H10 0.9500 . ? C11 C12 1.392(9) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.382(8) . ? C13 C14 1.383(9) . ? C14 C15 1.374(9) . ? C14 H14 0.9500 . ? C15 C16 1.367(9) . ? C15 H15 0.9500 . ? C16 C17 1.366(9) . ? C16 H16 0.9500 . ? C17 C18 1.383(9) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.378(8) . ? C19 C24 1.380(8) . ? C20 C21 1.384(9) . ? C20 H20 0.9500 . ? C21 C22 1.362(9) . ? C21 H21 0.9500 . ? C22 C23 1.366(9) . ? C22 H22 0.9500 . ? C23 C24 1.400(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.391(8) . ? C25 C26 1.392(8) . ? C26 C27 1.390(8) . ? C26 H26 0.9500 . ? C27 C28 1.374(9) . ? C27 H27 0.9500 . ? C28 C29 1.376(9) . ? C28 H28 0.9500 . ? C29 C30 1.377(8) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.380(8) . ? C31 C32 1.393(8) . ? C32 C33 1.380(8) . ? C32 H32 0.9500 . ? C33 C34 1.378(9) . ? C33 H33 0.9500 . ? C34 C35 1.384(8) . ? C34 H34 0.9500 . ? C35 C36 1.396(8) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.381(8) . ? C37 C38 1.393(8) . ? C38 C39 1.404(8) . ? C38 H38 0.9500 . ? C39 C40 1.392(9) . ? C39 H39 0.9500 . ? C40 C41 1.391(8) . ? C40 C43 1.454(9) . ? C41 C42 1.396(8) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C37 Pd1 P2 88.82(17) . . ? C37 Pd1 P1 169.18(17) . . ? P2 Pd1 P1 100.82(6) . . ? C37 Pd1 Br1 83.24(16) . . ? P2 Pd1 Br1 164.03(5) . . ? P1 Pd1 Br1 88.53(4) . . ? C13 P1 C19 103.0(3) . . ? C13 P1 C2 101.6(3) . . ? C19 P1 C2 102.6(3) . . ? C13 P1 Pd1 114.4(2) . . ? C19 P1 Pd1 113.3(2) . . ? C2 P1 Pd1 119.79(19) . . ? C25 P2 C31 104.0(3) . . ? C25 P2 C8 105.0(3) . . ? C31 P2 C8 104.1(3) . . ? C25 P2 Pd1 107.54(19) . . ? C31 P2 Pd1 112.8(2) . . ? C8 P2 Pd1 121.71(19) . . ? C7 O1 C1 115.6(5) . . ? C2 C1 C6 122.5(6) . . ? C2 C1 O1 115.7(5) . . ? C6 C1 O1 121.8(6) . . ? C1 C2 C3 118.4(6) . . ? C1 C2 P1 117.1(5) . . ? C3 C2 P1 124.5(5) . . ? C4 C3 C2 120.1(6) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 121.1(6) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 119.0(6) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C1 C6 C5 118.9(6) . . ? C1 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C12 C7 O1 119.7(6) . . ? C12 C7 C8 121.7(6) . . ? O1 C7 C8 118.6(5) . . ? C9 C8 C7 117.3(5) . . ? C9 C8 P2 121.4(4) . . ? C7 C8 P2 121.3(4) . . ? C10 C9 C8 120.3(6) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 121.0(6) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.9(6) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 119.4(6) . . ? C7 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C18 C13 C14 117.6(6) . . ? C18 C13 P1 122.9(5) . . ? C14 C13 P1 119.4(5) . . ? C15 C14 C13 121.8(7) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C16 C15 C14 119.7(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 119.6(7) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 120.7(7) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C13 C18 C17 120.4(6) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C24 117.8(6) . . ? C20 C19 P1 120.1(5) . . ? C24 C19 P1 121.7(5) . . ? C19 C20 C21 121.4(6) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C22 C21 C20 120.3(7) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 119.7(6) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C22 C23 C24 120.0(6) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 120.8(6) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C30 C25 C26 119.1(6) . . ? C30 C25 P2 117.2(5) . . ? C26 C25 P2 123.6(5) . . ? C27 C26 C25 119.8(6) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.5(6) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 119.7(6) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C28 C29 C30 120.7(7) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 120.2(6) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C36 C31 C32 119.0(6) . . ? C36 C31 P2 120.9(5) . . ? C32 C31 P2 119.7(5) . . ? C33 C32 C31 121.0(6) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C32 119.8(6) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.0(6) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 120.1(6) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 120.0(6) . . ? C31 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C42 C37 C38 118.7(5) . . ? C42 C37 Pd1 123.3(4) . . ? C38 C37 Pd1 117.7(4) . . ? C37 C38 C39 120.7(5) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C40 C39 C38 119.9(6) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C41 119.5(6) . . ? C39 C40 C43 120.6(6) . . ? C41 C40 C43 119.8(6) . . ? C40 C41 C42 119.8(6) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C37 C42 C41 121.4(6) . . ? C37 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? N1 C43 C40 177.6(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C37 Pd1 P1 C13 -86.2(9) . . . . ? P2 Pd1 P1 C13 121.2(2) . . . . ? Br1 Pd1 P1 C13 -45.7(2) . . . . ? C37 Pd1 P1 C19 31.5(10) . . . . ? P2 Pd1 P1 C19 -121.1(2) . . . . ? Br1 Pd1 P1 C19 72.0(2) . . . . ? C37 Pd1 P1 C2 152.8(9) . . . . ? P2 Pd1 P1 C2 0.2(2) . . . . ? Br1 Pd1 P1 C2 -166.8(2) . . . . ? C37 Pd1 P2 C25 133.4(3) . . . . ? P1 Pd1 P2 C25 -51.6(2) . . . . ? Br1 Pd1 P2 C25 73.4(3) . . . . ? C37 Pd1 P2 C31 19.2(3) . . . . ? P1 Pd1 P2 C31 -165.7(2) . . . . ? Br1 Pd1 P2 C31 -40.8(3) . . . . ? C37 Pd1 P2 C8 -105.6(3) . . . . ? P1 Pd1 P2 C8 69.4(2) . . . . ? Br1 Pd1 P2 C8 -165.6(2) . . . . ? C7 O1 C1 C2 142.9(5) . . . . ? C7 O1 C1 C6 -39.5(8) . . . . ? C6 C1 C2 C3 0.4(9) . . . . ? O1 C1 C2 C3 178.0(5) . . . . ? C6 C1 C2 P1 180.0(5) . . . . ? O1 C1 C2 P1 -2.4(7) . . . . ? C13 P1 C2 C1 -178.7(5) . . . . ? C19 P1 C2 C1 74.9(5) . . . . ? Pd1 P1 C2 C1 -51.5(5) . . . . ? C13 P1 C2 C3 0.8(6) . . . . ? C19 P1 C2 C3 -105.5(5) . . . . ? Pd1 P1 C2 C3 128.0(5) . . . . ? C1 C2 C3 C4 -0.3(9) . . . . ? P1 C2 C3 C4 -179.9(5) . . . . ? C2 C3 C4 C5 -0.5(10) . . . . ? C3 C4 C5 C6 1.1(10) . . . . ? C2 C1 C6 C5 0.2(9) . . . . ? O1 C1 C6 C5 -177.2(5) . . . . ? C4 C5 C6 C1 -1.0(9) . . . . ? C1 O1 C7 C12 93.4(7) . . . . ? C1 O1 C7 C8 -87.3(6) . . . . ? C12 C7 C8 C9 -5.3(9) . . . . ? O1 C7 C8 C9 175.4(5) . . . . ? C12 C7 C8 P2 176.2(5) . . . . ? O1 C7 C8 P2 -3.0(8) . . . . ? C25 P2 C8 C9 -94.3(5) . . . . ? C31 P2 C8 C9 14.7(5) . . . . ? Pd1 P2 C8 C9 143.5(4) . . . . ? C25 P2 C8 C7 84.1(5) . . . . ? C31 P2 C8 C7 -166.9(5) . . . . ? Pd1 P2 C8 C7 -38.1(5) . . . . ? C7 C8 C9 C10 2.0(8) . . . . ? P2 C8 C9 C10 -179.6(4) . . . . ? C8 C9 C10 C11 2.1(9) . . . . ? C9 C10 C11 C12 -3.0(9) . . . . ? O1 C7 C12 C11 -176.2(5) . . . . ? C8 C7 C12 C11 4.6(10) . . . . ? C10 C11 C12 C7 -0.4(9) . . . . ? C19 P1 C13 C18 10.8(6) . . . . ? C2 P1 C13 C18 -95.1(6) . . . . ? Pd1 P1 C13 C18 134.3(5) . . . . ? C19 P1 C13 C14 -171.9(5) . . . . ? C2 P1 C13 C14 82.2(5) . . . . ? Pd1 P1 C13 C14 -48.4(6) . . . . ? C18 C13 C14 C15 1.4(10) . . . . ? P1 C13 C14 C15 -176.1(5) . . . . ? C13 C14 C15 C16 -3.3(11) . . . . ? C14 C15 C16 C17 3.1(10) . . . . ? C15 C16 C17 C18 -1.2(10) . . . . ? C14 C13 C18 C17 0.6(9) . . . . ? P1 C13 C18 C17 178.0(5) . . . . ? C16 C17 C18 C13 -0.7(10) . . . . ? C13 P1 C19 C20 78.3(6) . . . . ? C2 P1 C19 C20 -176.4(5) . . . . ? Pd1 P1 C19 C20 -45.9(6) . . . . ? C13 P1 C19 C24 -94.2(6) . . . . ? C2 P1 C19 C24 11.1(6) . . . . ? Pd1 P1 C19 C24 141.6(5) . . . . ? C24 C19 C20 C21 -0.1(11) . . . . ? P1 C19 C20 C21 -172.9(6) . . . . ? C19 C20 C21 C22 -0.6(13) . . . . ? C20 C21 C22 C23 0.0(12) . . . . ? C21 C22 C23 C24 1.2(11) . . . . ? C20 C19 C24 C23 1.3(10) . . . . ? P1 C19 C24 C23 174.0(5) . . . . ? C22 C23 C24 C19 -1.9(11) . . . . ? C31 P2 C25 C30 83.3(5) . . . . ? C8 P2 C25 C30 -167.6(5) . . . . ? Pd1 P2 C25 C30 -36.6(5) . . . . ? C31 P2 C25 C26 -98.9(5) . . . . ? C8 P2 C25 C26 10.2(6) . . . . ? Pd1 P2 C25 C26 141.2(5) . . . . ? C30 C25 C26 C27 2.6(9) . . . . ? P2 C25 C26 C27 -175.1(5) . . . . ? C25 C26 C27 C28 -0.4(10) . . . . ? C26 C27 C28 C29 -2.4(10) . . . . ? C27 C28 C29 C30 2.9(10) . . . . ? C28 C29 C30 C25 -0.6(10) . . . . ? C26 C25 C30 C29 -2.1(9) . . . . ? P2 C25 C30 C29 175.7(5) . . . . ? C25 P2 C31 C36 -20.0(6) . . . . ? C8 P2 C31 C36 -129.8(5) . . . . ? Pd1 P2 C31 C36 96.3(5) . . . . ? C25 P2 C31 C32 167.7(5) . . . . ? C8 P2 C31 C32 57.9(5) . . . . ? Pd1 P2 C31 C32 -76.1(5) . . . . ? C36 C31 C32 C33 -3.2(9) . . . . ? P2 C31 C32 C33 169.3(5) . . . . ? C31 C32 C33 C34 0.8(10) . . . . ? C32 C33 C34 C35 2.0(10) . . . . ? C33 C34 C35 C36 -2.3(10) . . . . ? C32 C31 C36 C35 2.8(9) . . . . ? P2 C31 C36 C35 -169.5(5) . . . . ? C34 C35 C36 C31 -0.2(10) . . . . ? P2 Pd1 C37 C42 -86.1(5) . . . . ? P1 Pd1 C37 C42 120.8(8) . . . . ? Br1 Pd1 C37 C42 80.0(5) . . . . ? P2 Pd1 C37 C38 100.2(4) . . . . ? P1 Pd1 C37 C38 -52.9(12) . . . . ? Br1 Pd1 C37 C38 -93.7(4) . . . . ? C42 C37 C38 C39 1.1(9) . . . . ? Pd1 C37 C38 C39 175.2(5) . . . . ? C37 C38 C39 C40 -1.4(9) . . . . ? C38 C39 C40 C41 1.7(9) . . . . ? C38 C39 C40 C43 -176.8(6) . . . . ? C39 C40 C41 C42 -1.7(9) . . . . ? C43 C40 C41 C42 176.7(6) . . . . ? C38 C37 C42 C41 -1.2(9) . . . . ? Pd1 C37 C42 C41 -174.9(5) . . . . ? C40 C41 C42 C37 1.5(9) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.484 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.120 #===END # Compound 4b data_s2100a _database_code_CSD 133394 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H36 N O P2 Pd, C F3 O3 S, C H2 Cl2' _chemical_formula_sum 'C48 H38 Cl2 F3 N O4 P2 Pd S' _chemical_formula_weight 1021.09 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' 'F' 'F' 0.0171 0.0103 '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' 'Pd' 'Pd' -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 13.2554(10) _cell_length_b 22.3413(10) _cell_length_c 15.0667(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.984(10) _cell_angle_gamma 90.00 _cell_volume 4459.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82840 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.00 _reflns_number_total 82840 _reflns_number_gt 67110 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'DIRAX' _computing_data_reduction 'EVAL14' _computing_structure_solution 'DIRDIF-97 (Beurskens et al., 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0961P)^2^+25.6260P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constraint _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 82840 _refine_ls_number_parameters 555 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.2163 _refine_ls_wR_factor_gt 0.1941 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.122 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.184790(11) 0.154612(8) 0.251963(11) 0.02790(6) Uani 1 1 d . . . P2 P 0.15848(4) 0.15605(3) 0.10088(4) 0.02852(14) Uani 1 1 d . . . P3 P 0.16656(5) 0.15462(3) 0.40199(4) 0.03276(15) Uani 1 1 d . . . C4 C 0.04569(17) 0.10975(11) 0.09215(15) 0.0286(5) Uani 1 1 d . . . C5 C 0.0036(2) 0.09247(12) 0.00919(17) 0.0387(6) Uani 1 1 d . . . H5 H 0.0338 0.1057 -0.0436 0.046 Uiso 1 1 calc R . . C6 C -0.0801(2) 0.05699(13) 0.0035(2) 0.0466(7) Uani 1 1 d . . . H6 H -0.1091 0.0462 -0.0528 0.056 Uiso 1 1 calc R . . C7 C -0.1224(2) 0.03673(12) 0.0811(2) 0.0450(7) Uani 1 1 d . . . H7 H -0.1799 0.0114 0.0765 0.054 Uiso 1 1 calc R . . C8 C -0.08470(18) 0.05173(11) 0.16393(17) 0.0355(6) Uani 1 1 d . . . C9 C -0.00045(17) 0.08854(11) 0.16765(16) 0.0316(6) Uani 1 1 d . . . O10 O 0.04385(10) 0.10658(7) 0.24929(10) 0.0323(4) Uani 1 1 d . . . C11 C 0.00336(18) 0.08931(11) 0.32999(16) 0.0331(6) Uani 1 1 d . . . C12 C -0.08223(18) 0.05295(12) 0.33079(18) 0.0383(7) Uani 1 1 d . . . C13 C -0.1190(2) 0.04003(12) 0.41339(19) 0.0436(7) Uani 1 1 d . . . H13 H -0.1771 0.0153 0.4167 0.052 Uiso 1 1 calc R . . C14 C -0.0751(2) 0.06147(13) 0.4907(2) 0.0481(8) Uani 1 1 d . . . H14 H -0.1036 0.0524 0.5461 0.058 Uiso 1 1 calc R . . C15 C 0.01096(19) 0.09629(12) 0.48774(18) 0.0400(6) Uani 1 1 d . . . H15 H 0.0427 0.1103 0.5413 0.048 Uiso 1 1 calc R . . C16 C 0.05088(18) 0.11071(11) 0.40700(16) 0.0334(6) Uani 1 1 d . . . C17 C -0.13176(16) 0.02665(11) 0.24665(19) 0.0422(6) Uani 1 1 d . . . C18 C -0.24603(17) 0.04127(13) 0.2436(2) 0.0572(8) Uani 1 1 d . . . H18A H -0.2769 0.0249 0.2966 0.086 Uiso 1 1 calc R . . H18B H -0.2780 0.0234 0.1904 0.086 Uiso 1 1 calc R . . H18C H -0.2554 0.0848 0.2420 0.086 Uiso 1 1 calc R . . C19 C -0.1170(2) -0.04170(11) 0.2481(2) 0.0569(8) Uani 1 1 d . . . H19A H -0.1470 -0.0583 0.3013 0.085 Uiso 1 1 calc R . . H19B H -0.0447 -0.0510 0.2490 0.085 Uiso 1 1 calc R . . H19C H -0.1499 -0.0593 0.1950 0.085 Uiso 1 1 calc R . . C20 C 0.12688(18) 0.22847(11) 0.05246(15) 0.0339(6) Uani 1 1 d . . . C21 C 0.0343(2) 0.24222(12) 0.01362(16) 0.0389(6) Uani 1 1 d . . . H21 H -0.0175 0.2128 0.0101 0.047 Uiso 1 1 calc R . . C22 C 0.0168(3) 0.29944(15) -0.02064(19) 0.0574(8) Uani 1 1 d . . . H22 H -0.0471 0.3086 -0.0478 0.069 Uiso 1 1 calc R . . C23 C 0.0899(3) 0.34243(13) -0.01572(19) 0.0539(8) Uani 1 1 d . . . H23 H 0.0771 0.3814 -0.0388 0.065 Uiso 1 1 calc R . . C24 C 0.1820(3) 0.32865(13) 0.0230(2) 0.0583(8) Uani 1 1 d . . . H24 H 0.2329 0.3585 0.0268 0.070 Uiso 1 1 calc R . . C25 C 0.2022(2) 0.27226(13) 0.05668(19) 0.0516(7) Uani 1 1 d . . . H25 H 0.2669 0.2633 0.0825 0.062 Uiso 1 1 calc R . . C26 C 0.24779(18) 0.12295(12) 0.02645(16) 0.0330(6) Uani 1 1 d . . . C27 C 0.2622(2) 0.14558(13) -0.05772(17) 0.0425(7) Uani 1 1 d . . . H27 H 0.2242 0.1790 -0.0791 0.051 Uiso 1 1 calc R . . C28 C 0.3330(2) 0.11865(15) -0.11018(19) 0.0530(8) Uani 1 1 d . . . H28 H 0.3438 0.1341 -0.1678 0.064 Uiso 1 1 calc R . . C29 C 0.3864(2) 0.07123(15) -0.08126(19) 0.0536(8) Uani 1 1 d . . . H29 H 0.4345 0.0538 -0.1188 0.064 Uiso 1 1 calc R . . C30 C 0.3733(2) 0.04727(15) 0.0017(2) 0.0522(8) Uani 1 1 d . . . H30 H 0.4110 0.0133 0.0213 0.063 Uiso 1 1 calc R . . C31 C 0.30260(19) 0.07418(13) 0.05675(17) 0.0428(7) Uani 1 1 d . . . H31 H 0.2927 0.0588 0.1146 0.051 Uiso 1 1 calc R . . C32 C 0.1433(2) 0.22607(12) 0.45379(16) 0.0404(6) Uani 1 1 d . . . C33 C 0.0503(2) 0.24419(13) 0.48115(17) 0.0448(7) Uani 1 1 d . . . H33 H -0.0053 0.2175 0.4748 0.054 Uiso 1 1 calc R . . C34 C 0.0355(3) 0.30016(13) 0.51772(18) 0.0526(8) Uani 1 1 d . . . H34 H -0.0294 0.3119 0.5361 0.063 Uiso 1 1 calc R . . C35 C 0.1158(3) 0.33818(14) 0.5270(2) 0.0670(10) Uani 1 1 d . . . H35 H 0.1063 0.3764 0.5531 0.080 Uiso 1 1 calc R . . C36 C 0.2079(3) 0.32293(17) 0.5001(3) 0.0871(13) Uani 1 1 d . . . H36 H 0.2627 0.3503 0.5057 0.105 Uiso 1 1 calc R . . C37 C 0.2221(3) 0.26502(15) 0.4630(2) 0.0731(11) Uani 1 1 d . . . H37 H 0.2871 0.2534 0.4446 0.088 Uiso 1 1 calc R . . C38 C 0.25634(19) 0.11587(13) 0.47426(16) 0.0402(7) Uani 1 1 d . . . C39 C 0.3020(2) 0.06481(13) 0.44048(19) 0.0450(7) Uani 1 1 d . . . H39 H 0.2876 0.0530 0.3808 0.054 Uiso 1 1 calc R . . C40 C 0.3683(2) 0.03111(16) 0.4936(2) 0.0597(9) Uani 1 1 d . . . H40 H 0.3974 -0.0043 0.4708 0.072 Uiso 1 1 calc R . . C41 C 0.3914(2) 0.04866(19) 0.5777(2) 0.0676(10) Uani 1 1 d . . . H41 H 0.4380 0.0260 0.6133 0.081 Uiso 1 1 calc R . . C42 C 0.3481(3) 0.09880(19) 0.6120(2) 0.0671(10) Uani 1 1 d . . . H42 H 0.3643 0.1106 0.6713 0.081 Uiso 1 1 calc R . . C43 C 0.2800(2) 0.13280(15) 0.56003(18) 0.0526(8) Uani 1 1 d . . . H43 H 0.2502 0.1676 0.5841 0.063 Uiso 1 1 calc R . . C44 C 0.31640(15) 0.19528(10) 0.25398(14) 0.0296(5) Uani 1 1 d . . . C45 C 0.32345(18) 0.25742(11) 0.25859(18) 0.0435(6) Uani 1 1 d . . . H45 H 0.2638 0.2804 0.2646 0.052 Uiso 1 1 calc R . . C46 C 0.41498(18) 0.28639(11) 0.25461(18) 0.0427(6) Uani 1 1 d . . . H46 H 0.4179 0.3289 0.2566 0.051 Uiso 1 1 calc R . . C47 C 0.50154(17) 0.25370(11) 0.24781(16) 0.0377(6) Uani 1 1 d . . . C48 C 0.49776(16) 0.19108(12) 0.24599(16) 0.0399(6) Uani 1 1 d . . . H48 H 0.5583 0.1685 0.2427 0.048 Uiso 1 1 calc R . . C49 C 0.40511(16) 0.16196(10) 0.24908(15) 0.0321(5) Uani 1 1 d . . . H49 H 0.4023 0.1195 0.2479 0.039 Uiso 1 1 calc R . . C50 C 0.59564(19) 0.28397(12) 0.24077(19) 0.0467(7) Uani 1 1 d . . . N51 N 0.66999(16) 0.30995(11) 0.23554(18) 0.0612(7) Uani 1 1 d . . . S52 S 0.28170(5) 0.45258(3) 0.24575(5) 0.05014(18) Uani 1 1 d D . . O53 O 0.3436(2) 0.41761(13) 0.3029(2) 0.1158(11) Uani 1 1 d DU . . O54 O 0.2812(3) 0.43549(14) 0.15580(16) 0.1355(16) Uani 1 1 d DU . . O55 O 0.28466(16) 0.51597(9) 0.26120(13) 0.0644(6) Uani 1 1 d DU . . C56 C 0.1579(2) 0.43118(14) 0.2757(2) 0.0711(10) Uani 1 1 d D . . F57 F 0.13858(16) 0.37359(9) 0.26051(15) 0.0922(7) Uani 1 1 d DU . . F58 F 0.08855(17) 0.46312(13) 0.2380(3) 0.1643(15) Uani 1 1 d DU . . F59 F 0.1472(2) 0.44001(11) 0.36281(19) 0.1348(13) Uani 1 1 d DU . . Cl61 Cl 0.48200(6) 0.23822(5) 0.74984(6) 0.0813(3) Uani 1 1 d DU . . Cl62 Cl 0.31531(8) 0.29819(4) 0.83591(7) 0.0864(3) Uani 1 1 d DU . . C61 C 0.3606(3) 0.2730(2) 0.7289(3) 0.0992(13) Uiso 1 1 d D . . H61A H 0.3127 0.2439 0.7013 0.119 Uiso 1 1 calc R . . H61B H 0.3671 0.3074 0.6882 0.119 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02421(8) 0.03307(10) 0.02683(11) -0.00294(8) 0.00687(7) -0.00340(7) P2 0.0275(3) 0.0321(4) 0.0263(4) -0.0044(3) 0.0046(2) -0.0010(2) P3 0.0333(3) 0.0388(4) 0.0268(4) -0.0026(3) 0.0105(2) -0.0028(3) C4 0.0269(12) 0.0249(14) 0.0340(16) -0.0069(10) 0.0023(9) 0.0004(10) C5 0.0409(15) 0.0401(16) 0.0352(17) -0.0098(11) 0.0013(11) 0.0055(12) C6 0.0417(16) 0.0438(18) 0.053(2) -0.0158(13) -0.0111(13) 0.0029(13) C7 0.0297(14) 0.0325(16) 0.073(2) -0.0119(13) 0.0013(13) -0.0009(12) C8 0.0238(13) 0.0316(15) 0.0512(18) -0.0065(11) 0.0027(10) 0.0038(11) C9 0.0237(13) 0.0305(14) 0.0408(17) -0.0064(10) 0.0034(10) 0.0051(10) O10 0.0264(7) 0.0398(9) 0.0312(10) -0.0043(7) 0.0074(7) -0.0061(6) C11 0.0289(13) 0.0323(15) 0.0393(17) 0.0036(11) 0.0161(10) -0.0006(11) C12 0.0281(14) 0.0319(16) 0.0557(19) 0.0059(12) 0.0116(11) 0.0015(11) C13 0.0353(15) 0.0391(17) 0.058(2) 0.0107(13) 0.0177(13) 0.0000(12) C14 0.0416(16) 0.0448(18) 0.060(2) 0.0202(14) 0.0277(14) 0.0112(13) C15 0.0387(15) 0.0404(17) 0.0420(18) 0.0059(12) 0.0170(11) 0.0065(12) C16 0.0348(13) 0.0315(15) 0.0346(16) 0.0036(11) 0.0121(10) 0.0089(11) C17 0.0269(11) 0.0349(14) 0.065(2) -0.0047(13) 0.0085(11) -0.0065(10) C18 0.0275(12) 0.0582(19) 0.087(2) -0.0036(16) 0.0114(13) -0.0095(12) C19 0.0505(15) 0.0297(14) 0.091(3) -0.0060(15) 0.0089(15) -0.0125(12) C20 0.0416(14) 0.0352(15) 0.0255(15) -0.0035(10) 0.0081(10) 0.0033(11) C21 0.0405(14) 0.0386(16) 0.0381(17) 0.0006(11) 0.0063(11) 0.0065(11) C22 0.066(2) 0.064(2) 0.043(2) 0.0074(15) 0.0142(14) 0.0125(17) C23 0.075(2) 0.0382(18) 0.049(2) 0.0014(13) 0.0105(15) 0.0117(16) C24 0.087(2) 0.0387(18) 0.049(2) -0.0038(13) 0.0010(16) -0.0207(17) C25 0.0593(18) 0.0484(19) 0.046(2) -0.0040(13) -0.0099(13) -0.0113(14) C26 0.0296(12) 0.0422(16) 0.0278(16) -0.0068(11) 0.0080(9) -0.0041(11) C27 0.0451(15) 0.0578(19) 0.0253(16) -0.0079(12) 0.0093(11) -0.0025(13) C28 0.0529(18) 0.074(2) 0.0330(18) -0.0044(14) 0.0160(13) -0.0071(16) C29 0.0422(16) 0.080(2) 0.041(2) -0.0172(16) 0.0212(13) -0.0031(15) C30 0.0389(16) 0.063(2) 0.055(2) -0.0082(15) 0.0130(12) 0.0139(14) C31 0.0384(14) 0.0591(19) 0.0315(17) -0.0034(12) 0.0093(11) 0.0041(13) C32 0.0541(16) 0.0433(17) 0.0247(15) -0.0014(11) 0.0126(11) -0.0048(13) C33 0.0573(17) 0.0465(18) 0.0306(17) -0.0005(12) 0.0037(12) 0.0040(13) C34 0.074(2) 0.0426(19) 0.0416(19) -0.0031(13) 0.0061(14) 0.0176(16) C35 0.111(3) 0.040(2) 0.051(2) -0.0123(14) 0.0258(19) -0.0002(19) C36 0.096(3) 0.060(2) 0.107(3) -0.038(2) 0.038(2) -0.027(2) C37 0.078(2) 0.058(2) 0.086(3) -0.0368(18) 0.0364(19) -0.0276(18) C38 0.0375(14) 0.063(2) 0.0209(16) 0.0058(12) 0.0067(10) -0.0065(13) C39 0.0437(15) 0.0510(18) 0.0409(18) 0.0020(13) 0.0077(12) 0.0100(13) C40 0.0478(18) 0.080(3) 0.052(2) 0.0188(17) 0.0075(14) 0.0100(16) C41 0.0431(17) 0.114(3) 0.046(2) 0.030(2) 0.0040(14) 0.0011(19) C42 0.063(2) 0.116(3) 0.0213(18) 0.0132(18) -0.0057(14) -0.024(2) C43 0.0594(19) 0.066(2) 0.0327(19) -0.0018(14) 0.0101(13) -0.0109(15) C44 0.0281(10) 0.0368(13) 0.0242(14) -0.0009(10) 0.0055(9) 0.0000(9) C45 0.0396(13) 0.0346(14) 0.056(2) -0.0048(12) 0.0036(12) 0.0046(10) C46 0.0441(14) 0.0344(14) 0.0498(18) 0.0005(12) 0.0043(12) -0.0059(10) C47 0.0365(12) 0.0494(16) 0.0275(15) -0.0008(11) 0.0041(10) -0.0121(11) C48 0.0267(11) 0.0564(17) 0.0368(16) 0.0036(12) 0.0068(10) 0.0052(10) C49 0.0390(12) 0.0284(12) 0.0292(14) -0.0001(10) 0.0054(10) -0.0048(9) C50 0.0393(14) 0.0515(17) 0.0496(19) 0.0054(13) 0.0060(12) -0.0033(12) N51 0.0383(13) 0.0589(16) 0.087(2) 0.0104(14) 0.0092(12) -0.0103(11) S52 0.0481(4) 0.0598(5) 0.0435(5) -0.0153(4) 0.0154(3) -0.0127(3) O53 0.0783(19) 0.083(2) 0.183(3) -0.0429(19) -0.0485(19) 0.0240(16) O54 0.235(4) 0.125(3) 0.0520(18) -0.0480(16) 0.076(2) -0.109(3) O55 0.0776(14) 0.0532(13) 0.0639(15) -0.0124(10) 0.0230(11) -0.0228(10) C56 0.059(2) 0.057(2) 0.098(3) 0.0072(19) 0.0199(19) -0.0101(16) F57 0.0917(14) 0.0690(14) 0.1178(19) -0.0155(12) 0.0314(12) -0.0368(11) F58 0.0509(13) 0.122(2) 0.317(5) 0.043(3) -0.038(2) 0.0010(14) F59 0.190(3) 0.0819(18) 0.140(2) -0.0270(16) 0.121(2) -0.0382(18) Cl61 0.0688(5) 0.1105(8) 0.0657(6) 0.0096(5) 0.0191(4) -0.0129(5) Cl62 0.0728(6) 0.0544(6) 0.1324(9) -0.0137(5) 0.0070(5) -0.0108(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C44 1.966(2) . ? Pd1 O10 2.1537(14) . ? Pd1 P3 2.2816(6) . ? Pd1 P2 2.2912(6) . ? P2 C26 1.816(2) . ? P2 C20 1.818(3) . ? P2 C4 1.819(2) . ? P3 C38 1.806(3) . ? P3 C32 1.808(3) . ? P3 C16 1.824(3) . ? C4 C9 1.393(3) . ? C4 C5 1.405(3) . ? C5 C6 1.363(4) . ? C5 H5 0.9500 . ? C6 C7 1.390(4) . ? C6 H6 0.9500 . ? C7 C8 1.370(4) . ? C7 H7 0.9500 . ? C8 C9 1.386(3) . ? C8 C17 1.520(4) . ? C9 O10 1.404(3) . ? O10 C11 1.400(3) . ? C11 C16 1.386(4) . ? C11 C12 1.396(3) . ? C12 C13 1.383(4) . ? C12 C17 1.525(4) . ? C13 C14 1.371(4) . ? C13 H13 0.9500 . ? C14 C15 1.382(4) . ? C14 H14 0.9500 . ? C15 C16 1.381(3) . ? C15 H15 0.9500 . ? C17 C19 1.540(3) . ? C17 C18 1.549(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.376(3) . ? C20 C25 1.398(4) . ? C21 C22 1.395(4) . ? C21 H21 0.9500 . ? C22 C23 1.364(4) . ? C22 H22 0.9500 . ? C23 C24 1.370(5) . ? C23 H23 0.9500 . ? C24 C25 1.381(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.379(4) . ? C26 C27 1.385(3) . ? C27 C28 1.385(4) . ? C27 H27 0.9500 . ? C28 C29 1.339(4) . ? C28 H28 0.9500 . ? C29 C30 1.376(4) . ? C29 H29 0.9500 . ? C30 C31 1.407(4) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.363(4) . ? C32 C33 1.374(4) . ? C33 C34 1.383(4) . ? C33 H33 0.9500 . ? C34 C35 1.365(5) . ? C34 H34 0.9500 . ? C35 C36 1.344(5) . ? C35 H35 0.9500 . ? C36 C37 1.424(5) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C43 1.372(4) . ? C38 C39 1.395(4) . ? C39 C40 1.390(4) . ? C39 H39 0.9500 . ? C40 C41 1.352(4) . ? C40 H40 0.9500 . ? C41 C42 1.368(5) . ? C41 H41 0.9500 . ? C42 C43 1.398(5) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.393(3) . ? C44 C49 1.396(3) . ? C45 C46 1.378(3) . ? C45 H45 0.9500 . ? C46 C47 1.367(3) . ? C46 H46 0.9500 . ? C47 C48 1.400(3) . ? C47 C50 1.426(3) . ? C48 C49 1.392(3) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 N51 1.149(3) . ? S52 O53 1.406(3) . ? S52 O54 1.408(2) . ? S52 O55 1.436(2) . ? S52 C56 1.782(3) . ? C56 F58 1.281(4) . ? C56 F57 1.330(3) . ? C56 F59 1.340(4) . ? Cl61 C61 1.805(4) . ? Cl62 C61 1.828(4) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? 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 C44 Pd1 O10 177.63(8) . . ? C44 Pd1 P3 96.26(7) . . ? O10 Pd1 P3 84.09(5) . . ? C44 Pd1 P2 96.50(7) . . ? O10 Pd1 P2 83.47(5) . . ? P3 Pd1 P2 165.15(2) . . ? C26 P2 C20 105.11(11) . . ? C26 P2 C4 105.99(11) . . ? C20 P2 C4 107.44(11) . . ? C26 P2 Pd1 121.86(9) . . ? C20 P2 Pd1 115.87(8) . . ? C4 P2 Pd1 99.22(8) . . ? C38 P3 C32 106.37(13) . . ? C38 P3 C16 104.75(12) . . ? C32 P3 C16 107.49(11) . . ? C38 P3 Pd1 120.47(9) . . ? C32 P3 Pd1 116.95(9) . . ? C16 P3 Pd1 99.15(8) . . ? C9 C4 C5 117.4(2) . . ? C9 C4 P2 121.15(18) . . ? C5 C4 P2 121.38(19) . . ? C6 C5 C4 120.8(3) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.2(3) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C8 C7 C6 122.8(3) . . ? C8 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C7 C8 C9 116.7(2) . . ? C7 C8 C17 120.6(2) . . ? C9 C8 C17 122.6(2) . . ? C8 C9 C4 123.0(2) . . ? C8 C9 O10 121.2(2) . . ? C4 C9 O10 115.8(2) . . ? C11 O10 C9 121.37(17) . . ? C11 O10 Pd1 118.64(14) . . ? C9 O10 Pd1 119.72(13) . . ? C16 C11 C12 122.7(2) . . ? C16 C11 O10 117.1(2) . . ? C12 C11 O10 120.3(2) . . ? C13 C12 C11 116.2(3) . . ? C13 C12 C17 120.8(2) . . ? C11 C12 C17 122.9(2) . . ? C14 C13 C12 122.6(3) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.1(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C11 118.7(3) . . ? C15 C16 P3 120.7(2) . . ? C11 C16 P3 120.61(18) . . ? C8 C17 C12 111.25(19) . . ? C8 C17 C19 108.8(2) . . ? C12 C17 C19 108.6(2) . . ? C8 C17 C18 109.1(2) . . ? C12 C17 C18 109.6(2) . . ? C19 C17 C18 109.5(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 119.2(3) . . ? C21 C20 P2 124.0(2) . . ? C25 C20 P2 116.8(2) . . ? C20 C21 C22 119.8(3) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 121.1(3) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 119.1(3) . . ? C22 C23 H23 120.5 . . ? C24 C23 H23 120.5 . . ? C23 C24 C25 121.4(3) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C24 C25 C20 119.5(3) . . ? C24 C25 H25 120.3 . . ? C20 C25 H25 120.3 . . ? C31 C26 C27 120.3(2) . . ? C31 C26 P2 117.69(19) . . ? C27 C26 P2 122.0(2) . . ? C26 C27 C28 118.8(3) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C29 C28 C27 121.3(3) . . ? C29 C28 H28 119.4 . . ? C27 C28 H28 119.4 . . ? C28 C29 C30 121.4(3) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C29 C30 C31 118.5(3) . . ? C29 C30 H30 120.8 . . ? C31 C30 H30 120.8 . . ? C26 C31 C30 119.8(3) . . ? C26 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C37 C32 C33 118.3(3) . . ? C37 C32 P3 117.8(2) . . ? C33 C32 P3 123.9(2) . . ? C32 C33 C34 121.8(3) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C35 C34 C33 118.8(3) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C36 C35 C34 121.7(3) . . ? C36 C35 H35 119.2 . . ? C34 C35 H35 119.2 . . ? C35 C36 C37 118.8(3) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C32 C37 C36 120.6(3) . . ? C32 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C43 C38 C39 118.7(3) . . ? C43 C38 P3 124.1(2) . . ? C39 C38 P3 117.2(2) . . ? C40 C39 C38 120.4(3) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C41 C40 C39 120.1(3) . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.5(3) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C43 120.3(3) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C38 C43 C42 120.0(3) . . ? C38 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C49 118.6(2) . . ? C45 C44 Pd1 121.28(16) . . ? C49 C44 Pd1 120.08(16) . . ? C46 C45 C44 121.6(2) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C47 C46 C45 119.7(2) . . ? C47 C46 H46 120.2 . . ? C45 C46 H46 120.2 . . ? C46 C47 C48 120.4(2) . . ? C46 C47 C50 119.4(2) . . ? C48 C47 C50 120.2(2) . . ? C49 C48 C47 119.8(2) . . ? C49 C48 H48 120.1 . . ? C47 C48 H48 120.1 . . ? C48 C49 C44 119.9(2) . . ? C48 C49 H49 120.1 . . ? C44 C49 H49 120.1 . . ? N51 C50 C47 178.0(3) . . ? O53 S52 O54 115.0(2) . . ? O53 S52 O55 115.90(15) . . ? O54 S52 O55 115.02(16) . . ? O53 S52 C56 102.61(19) . . ? O54 S52 C56 101.36(18) . . ? O55 S52 C56 104.12(14) . . ? F58 C56 F57 109.4(3) . . ? F58 C56 F59 104.7(3) . . ? F57 C56 F59 106.6(3) . . ? F58 C56 S52 113.0(2) . . ? F57 C56 S52 112.9(2) . . ? F59 C56 S52 109.8(2) . . ? Cl61 C61 Cl62 107.3(2) . . ? Cl61 C61 H61A 110.3 . . ? Cl62 C61 H61A 110.3 . . ? Cl61 C61 H61B 110.3 . . ? Cl62 C61 H61B 110.3 . . ? H61A C61 H61B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C44 Pd1 P2 C26 57.05(12) . . . . ? O10 Pd1 P2 C26 -120.57(11) . . . . ? P3 Pd1 P2 C26 -153.84(12) . . . . ? C44 Pd1 P2 C20 -72.92(11) . . . . ? O10 Pd1 P2 C20 109.46(10) . . . . ? P3 Pd1 P2 C20 76.19(13) . . . . ? C44 Pd1 P2 C4 172.48(10) . . . . ? O10 Pd1 P2 C4 -5.13(8) . . . . ? P3 Pd1 P2 C4 -38.41(12) . . . . ? C44 Pd1 P3 C38 -61.50(13) . . . . ? O10 Pd1 P3 C38 116.14(12) . . . . ? P2 Pd1 P3 C38 149.37(13) . . . . ? C44 Pd1 P3 C32 70.25(12) . . . . ? O10 Pd1 P3 C32 -112.11(11) . . . . ? P2 Pd1 P3 C32 -78.88(14) . . . . ? C44 Pd1 P3 C16 -174.70(10) . . . . ? O10 Pd1 P3 C16 2.94(9) . . . . ? P2 Pd1 P3 C16 36.17(13) . . . . ? C26 P2 C4 C9 130.8(2) . . . . ? C20 P2 C4 C9 -117.2(2) . . . . ? Pd1 P2 C4 C9 3.7(2) . . . . ? C26 P2 C4 C5 -47.2(2) . . . . ? C20 P2 C4 C5 64.8(2) . . . . ? Pd1 P2 C4 C5 -174.30(18) . . . . ? C9 C4 C5 C6 0.9(4) . . . . ? P2 C4 C5 C6 179.0(2) . . . . ? C4 C5 C6 C7 -1.5(4) . . . . ? C5 C6 C7 C8 1.2(4) . . . . ? C6 C7 C8 C9 -0.3(4) . . . . ? C6 C7 C8 C17 -177.9(2) . . . . ? C7 C8 C9 C4 -0.3(4) . . . . ? C17 C8 C9 C4 177.3(2) . . . . ? C7 C8 C9 O10 179.9(2) . . . . ? C17 C8 C9 O10 -2.5(3) . . . . ? C5 C4 C9 C8 0.0(3) . . . . ? P2 C4 C9 C8 -178.07(19) . . . . ? C5 C4 C9 O10 179.8(2) . . . . ? P2 C4 C9 O10 1.7(3) . . . . ? C8 C9 O10 C11 -1.5(3) . . . . ? C4 C9 O10 C11 178.6(2) . . . . ? C8 C9 O10 Pd1 172.49(17) . . . . ? C4 C9 O10 Pd1 -7.3(3) . . . . ? P3 Pd1 O10 C11 -6.18(14) . . . . ? P2 Pd1 O10 C11 -178.05(15) . . . . ? P3 Pd1 O10 C9 179.63(15) . . . . ? P2 Pd1 O10 C9 7.76(14) . . . . ? C9 O10 C11 C16 -178.3(2) . . . . ? Pd1 O10 C11 C16 7.6(3) . . . . ? C9 O10 C11 C12 0.6(3) . . . . ? Pd1 O10 C11 C12 -173.47(17) . . . . ? C16 C11 C12 C13 1.2(4) . . . . ? O10 C11 C12 C13 -177.7(2) . . . . ? C16 C11 C12 C17 -176.8(2) . . . . ? O10 C11 C12 C17 4.3(4) . . . . ? C11 C12 C13 C14 0.2(4) . . . . ? C17 C12 C13 C14 178.2(2) . . . . ? C12 C13 C14 C15 -1.6(4) . . . . ? C13 C14 C15 C16 1.7(4) . . . . ? C14 C15 C16 C11 -0.4(4) . . . . ? C14 C15 C16 P3 -178.0(2) . . . . ? C12 C11 C16 C15 -1.1(4) . . . . ? O10 C11 C16 C15 177.8(2) . . . . ? C12 C11 C16 P3 176.57(19) . . . . ? O10 C11 C16 P3 -4.5(3) . . . . ? C38 P3 C16 C15 52.3(2) . . . . ? C32 P3 C16 C15 -60.5(2) . . . . ? Pd1 P3 C16 C15 177.34(18) . . . . ? C38 P3 C16 C11 -125.3(2) . . . . ? C32 P3 C16 C11 121.9(2) . . . . ? Pd1 P3 C16 C11 -0.3(2) . . . . ? C7 C8 C17 C12 -175.9(2) . . . . ? C9 C8 C17 C12 6.5(3) . . . . ? C7 C8 C17 C19 64.5(3) . . . . ? C9 C8 C17 C19 -113.1(3) . . . . ? C7 C8 C17 C18 -54.9(3) . . . . ? C9 C8 C17 C18 127.6(2) . . . . ? C13 C12 C17 C8 174.6(2) . . . . ? C11 C12 C17 C8 -7.5(3) . . . . ? C13 C12 C17 C19 -65.7(3) . . . . ? C11 C12 C17 C19 112.2(3) . . . . ? C13 C12 C17 C18 53.9(3) . . . . ? C11 C12 C17 C18 -128.2(3) . . . . ? C26 P2 C20 C21 110.0(2) . . . . ? C4 P2 C20 C21 -2.6(2) . . . . ? Pd1 P2 C20 C21 -112.4(2) . . . . ? C26 P2 C20 C25 -70.7(2) . . . . ? C4 P2 C20 C25 176.68(19) . . . . ? Pd1 P2 C20 C25 66.9(2) . . . . ? C25 C20 C21 C22 -0.2(4) . . . . ? P2 C20 C21 C22 179.1(2) . . . . ? C20 C21 C22 C23 -0.5(4) . . . . ? C21 C22 C23 C24 0.5(4) . . . . ? C22 C23 C24 C25 0.3(5) . . . . ? C23 C24 C25 C20 -1.0(5) . . . . ? C21 C20 C25 C24 0.9(4) . . . . ? P2 C20 C25 C24 -178.4(2) . . . . ? C20 P2 C26 C31 165.3(2) . . . . ? C4 P2 C26 C31 -81.1(2) . . . . ? Pd1 P2 C26 C31 30.9(2) . . . . ? C20 P2 C26 C27 -14.1(2) . . . . ? C4 P2 C26 C27 99.5(2) . . . . ? Pd1 P2 C26 C27 -148.53(18) . . . . ? C31 C26 C27 C28 -0.5(4) . . . . ? P2 C26 C27 C28 178.8(2) . . . . ? C26 C27 C28 C29 0.6(4) . . . . ? C27 C28 C29 C30 0.0(5) . . . . ? C28 C29 C30 C31 -0.7(5) . . . . ? C27 C26 C31 C30 -0.2(4) . . . . ? P2 C26 C31 C30 -179.5(2) . . . . ? C29 C30 C31 C26 0.8(4) . . . . ? C38 P3 C32 C37 63.9(3) . . . . ? C16 P3 C32 C37 175.6(3) . . . . ? Pd1 P3 C32 C37 -74.0(3) . . . . ? C38 P3 C32 C33 -118.7(2) . . . . ? C16 P3 C32 C33 -6.9(3) . . . . ? Pd1 P3 C32 C33 103.4(2) . . . . ? C37 C32 C33 C34 -0.3(4) . . . . ? P3 C32 C33 C34 -177.7(2) . . . . ? C32 C33 C34 C35 -0.2(4) . . . . ? C33 C34 C35 C36 1.2(5) . . . . ? C34 C35 C36 C37 -1.5(6) . . . . ? C33 C32 C37 C36 -0.1(5) . . . . ? P3 C32 C37 C36 177.5(3) . . . . ? C35 C36 C37 C32 1.0(6) . . . . ? C32 P3 C38 C43 14.2(3) . . . . ? C16 P3 C38 C43 -99.5(3) . . . . ? Pd1 P3 C38 C43 150.3(2) . . . . ? C32 P3 C38 C39 -167.4(2) . . . . ? C16 P3 C38 C39 78.9(2) . . . . ? Pd1 P3 C38 C39 -31.3(2) . . . . ? C43 C38 C39 C40 1.5(4) . . . . ? P3 C38 C39 C40 -177.0(2) . . . . ? C38 C39 C40 C41 -2.0(5) . . . . ? C39 C40 C41 C42 1.5(5) . . . . ? C40 C41 C42 C43 -0.5(5) . . . . ? C39 C38 C43 C42 -0.5(4) . . . . ? P3 C38 C43 C42 177.9(2) . . . . ? C41 C42 C43 C38 0.0(5) . . . . ? P3 Pd1 C44 C45 -83.4(2) . . . . ? P2 Pd1 C44 C45 88.9(2) . . . . ? P3 Pd1 C44 C49 97.75(18) . . . . ? P2 Pd1 C44 C49 -89.85(18) . . . . ? C49 C44 C45 C46 2.8(4) . . . . ? Pd1 C44 C45 C46 -176.0(2) . . . . ? C44 C45 C46 C47 -1.4(4) . . . . ? C45 C46 C47 C48 -0.8(4) . . . . ? C45 C46 C47 C50 177.9(2) . . . . ? C46 C47 C48 C49 1.5(4) . . . . ? C50 C47 C48 C49 -177.3(2) . . . . ? C47 C48 C49 C44 0.0(4) . . . . ? C45 C44 C49 C48 -2.1(3) . . . . ? Pd1 C44 C49 C48 176.75(18) . . . . ? O53 S52 C56 F58 172.5(3) . . . . ? O54 S52 C56 F58 -68.3(3) . . . . ? O55 S52 C56 F58 51.3(3) . . . . ? O53 S52 C56 F57 -62.7(3) . . . . ? O54 S52 C56 F57 56.4(3) . . . . ? O55 S52 C56 F57 176.1(2) . . . . ? O53 S52 C56 F59 56.0(3) . . . . ? O54 S52 C56 F59 175.2(3) . . . . ? O55 S52 C56 F59 -65.2(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 5.223 _refine_diff_density_min -1.182 _refine_diff_density_rms 0.132 #===END data_s1866a _database_code_CSD 177711 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H36 Br N O P2 Pd Si, 2(C H2 Cl2)' _chemical_formula_sum 'C47 H40 Br Cl4 N O P2 Pd Si' _chemical_formula_weight 1052.94 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' 'Br' 'Br' -0.2901 2.4595 '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' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.781(3) _cell_length_b 10.5595(13) _cell_length_c 22.522(4) _cell_angle_alpha 90.00 _cell_angle_beta 119.206(13) _cell_angle_gamma 90.00 _cell_volume 4521.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.52 _cell_measurement_theta_max 14.04 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.665 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4T' _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 18205 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.1010 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 27.44 _reflns_number_total 10315 _reflns_number_gt 6496 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'locally modified CAD4 software' _computing_cell_refinement 'SET4' _computing_data_reduction 'HELENA' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10315 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1077 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1256 _refine_ls_wR_factor_gt 0.1021 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.233290(18) 0.84502(4) 0.407602(17) 0.01159(9) Uani 1 1 d . . . Br1 Br 0.15165(3) 0.83316(6) 0.28030(2) 0.02261(13) Uani 1 1 d . . . P1 P 0.32501(6) 0.78149(12) 0.39239(6) 0.0129(3) Uani 1 1 d . . . P2 P 0.14197(6) 0.80481(12) 0.42819(6) 0.0127(3) Uani 1 1 d . . . Si1 Si 0.16873(7) 0.31988(13) 0.33027(7) 0.0185(3) Uani 1 1 d . . . O1 O 0.21574(16) 0.5906(3) 0.39083(16) 0.0134(7) Uani 1 1 d . . . N1 N 0.4718(3) 0.9104(6) 0.7772(2) 0.0438(15) Uani 1 1 d . . . C1 C 0.2483(2) 0.5464(5) 0.3543(2) 0.0133(10) Uani 1 1 d . . . C2 C 0.2990(3) 0.6254(5) 0.3517(2) 0.0156(11) Uani 1 1 d . . . C3 C 0.3333(3) 0.5803(5) 0.3167(2) 0.0184(11) Uani 1 1 d . . . H3 H 0.3679 0.6316 0.3143 0.022 Uiso 1 1 calc R . . C4 C 0.3176(3) 0.4624(5) 0.2858(3) 0.0225(12) Uani 1 1 d . . . H4 H 0.3404 0.4339 0.2614 0.027 Uiso 1 1 calc R . . C5 C 0.2690(3) 0.3874(5) 0.2906(3) 0.0236(12) Uani 1 1 d . . . H5 H 0.2590 0.3063 0.2698 0.028 Uiso 1 1 calc R . . C6 C 0.2340(3) 0.4256(5) 0.3249(2) 0.0181(11) Uani 1 1 d . . . C7 C 0.1473(2) 0.5574(5) 0.3754(2) 0.0136(10) Uani 1 1 d . . . C8 C 0.1088(2) 0.6488(5) 0.3903(2) 0.0147(10) Uani 1 1 d . . . C9 C 0.0417(3) 0.6147(5) 0.3786(2) 0.0172(11) Uani 1 1 d . . . H9 H 0.0156 0.6737 0.3892 0.021 Uiso 1 1 calc R . . C10 C 0.0124(3) 0.4982(5) 0.3524(3) 0.0210(12) Uani 1 1 d . . . H10 H -0.0338 0.4782 0.3438 0.025 Uiso 1 1 calc R . . C11 C 0.0507(3) 0.4121(5) 0.3388(3) 0.0229(12) Uani 1 1 d . . . H11 H 0.0305 0.3317 0.3208 0.027 Uiso 1 1 calc R . . C12 C 0.1193(3) 0.4386(5) 0.3505(2) 0.0171(11) Uani 1 1 d . . . C13 C 0.4090(2) 0.7517(5) 0.4685(2) 0.0147(10) Uani 1 1 d . . . C14 C 0.4487(3) 0.8567(5) 0.5050(2) 0.0212(11) Uani 1 1 d . . . H14 H 0.4335 0.9395 0.4874 0.025 Uiso 1 1 calc R . . C15 C 0.5095(3) 0.8409(6) 0.5662(3) 0.0273(12) Uani 1 1 d . . . H15 H 0.5364 0.9126 0.5905 0.033 Uiso 1 1 calc R . . C16 C 0.5313(3) 0.7208(6) 0.5920(3) 0.0308(14) Uani 1 1 d . . . H16 H 0.5730 0.7100 0.6344 0.037 Uiso 1 1 calc R . . C17 C 0.4930(3) 0.6164(6) 0.5565(3) 0.0290(13) Uani 1 1 d . . . H17 H 0.5083 0.5338 0.5744 0.035 Uiso 1 1 calc R . . C18 C 0.4319(3) 0.6319(5) 0.4945(3) 0.0217(12) Uani 1 1 d . . . H18 H 0.4059 0.5598 0.4699 0.026 Uiso 1 1 calc R . . C19 C 0.3518(3) 0.8747(5) 0.3401(2) 0.0155(11) Uani 1 1 d . . . C20 C 0.4152(3) 0.8520(5) 0.3413(3) 0.0208(11) Uani 1 1 d . . . H20 H 0.4463 0.7887 0.3706 0.025 Uiso 1 1 calc R . . C21 C 0.4333(3) 0.9214(6) 0.3000(3) 0.0278(13) Uani 1 1 d . . . H21 H 0.4764 0.9045 0.3005 0.033 Uiso 1 1 calc R . . C22 C 0.3891(3) 1.0152(6) 0.2579(3) 0.0267(13) Uani 1 1 d . . . H22 H 0.4015 1.0620 0.2293 0.032 Uiso 1 1 calc R . . C23 C 0.3267(3) 1.0402(6) 0.2578(3) 0.0276(13) Uani 1 1 d . . . H23 H 0.2964 1.1049 0.2292 0.033 Uiso 1 1 calc R . . C24 C 0.3081(3) 0.9714(5) 0.2992(3) 0.0204(11) Uani 1 1 d . . . H24 H 0.2657 0.9903 0.2996 0.024 Uiso 1 1 calc R . . C25 C 0.1639(2) 0.7810(5) 0.5163(2) 0.0159(11) Uani 1 1 d . . . C26 C 0.1853(3) 0.8870(6) 0.5589(3) 0.0224(12) Uani 1 1 d . . . H26 H 0.1851 0.9683 0.5407 0.027 Uiso 1 1 calc R . . C27 C 0.2065(3) 0.8739(6) 0.6269(3) 0.0318(15) Uani 1 1 d . . . H27 H 0.2211 0.9463 0.6556 0.038 Uiso 1 1 calc R . . C28 C 0.2069(3) 0.7563(7) 0.6540(3) 0.0412(17) Uani 1 1 d . . . H28 H 0.2215 0.7483 0.7010 0.049 Uiso 1 1 calc R . . C29 C 0.1865(3) 0.6520(7) 0.6134(3) 0.0398(16) Uani 1 1 d . . . H29 H 0.1868 0.5714 0.6323 0.048 Uiso 1 1 calc R . . C30 C 0.1648(3) 0.6624(6) 0.5437(3) 0.0271(12) Uani 1 1 d . . . H30 H 0.1508 0.5893 0.5155 0.033 Uiso 1 1 calc R . . C31 C 0.0653(2) 0.9087(5) 0.3957(2) 0.0147(10) Uani 1 1 d . . . C32 C 0.0243(3) 0.9175(5) 0.4282(3) 0.0201(11) Uani 1 1 d . . . H32 H 0.0361 0.8674 0.4673 0.024 Uiso 1 1 calc R . . C33 C -0.0331(3) 0.9984(5) 0.4038(3) 0.0234(12) Uani 1 1 d . . . H33 H -0.0605 1.0034 0.4260 0.028 Uiso 1 1 calc R . . C34 C -0.0501(3) 1.0716(5) 0.3471(3) 0.0233(12) Uani 1 1 d . . . H34 H -0.0893 1.1272 0.3304 0.028 Uiso 1 1 calc R . . C35 C -0.0104(3) 1.0645(5) 0.3145(3) 0.0193(11) Uani 1 1 d . . . H35 H -0.0224 1.1149 0.2754 0.023 Uiso 1 1 calc R . . C36 C 0.0471(3) 0.9834(5) 0.3390(2) 0.0159(10) Uani 1 1 d . . . H36 H 0.0743 0.9792 0.3166 0.019 Uiso 1 1 calc R . . C37 C 0.2988(2) 0.8599(5) 0.5080(2) 0.0160(10) Uani 1 1 d . . . C38 C 0.3211(3) 0.7555(5) 0.5507(2) 0.0179(11) Uani 1 1 d . . . H38 H 0.3053 0.6739 0.5316 0.021 Uiso 1 1 calc R . . C39 C 0.3653(3) 0.7657(5) 0.6200(3) 0.0227(12) Uani 1 1 d . . . H39 H 0.3798 0.6923 0.6479 0.027 Uiso 1 1 calc R . . C40 C 0.3880(3) 0.8843(6) 0.6481(2) 0.0227(12) Uani 1 1 d . . . C41 C 0.3675(3) 0.9910(5) 0.6069(2) 0.0212(12) Uani 1 1 d . . . H41 H 0.3841 1.0723 0.6262 0.025 Uiso 1 1 calc R . . C42 C 0.3226(3) 0.9788(5) 0.5371(2) 0.0186(11) Uani 1 1 d . . . H42 H 0.3082 1.0521 0.5091 0.022 Uiso 1 1 calc R . . C43 C 0.1130(3) 0.2402(6) 0.2480(3) 0.0281(13) Uani 1 1 d . . . H43A H 0.1413 0.1784 0.2393 0.042 Uiso 1 1 calc R . . H43B H 0.0941 0.3033 0.2115 0.042 Uiso 1 1 calc R . . H43C H 0.0741 0.1966 0.2496 0.042 Uiso 1 1 calc R . . C44 C 0.2113(3) 0.2003(5) 0.3987(3) 0.0305(14) Uani 1 1 d . . . H44A H 0.2368 0.1391 0.3861 0.046 Uiso 1 1 calc R . . H44B H 0.1753 0.1561 0.4049 0.046 Uiso 1 1 calc R . . H44C H 0.2443 0.2425 0.4412 0.046 Uiso 1 1 calc R . . C45 C 0.4348(3) 0.8987(6) 0.7207(3) 0.0286(14) Uani 1 1 d . . . Cl1 Cl 0.40363(9) 0.20405(18) 0.02985(10) 0.0503(5) Uani 1 1 d . . . Cl2 Cl 0.30814(11) 0.1486(2) 0.08240(11) 0.0720(7) Uani 1 1 d . . . C46 C 0.3781(4) 0.0968(7) 0.0730(4) 0.0520(19) Uani 1 1 d . . . H46A H 0.3652 0.0155 0.0480 0.062 Uiso 1 1 calc R . . H46B H 0.4187 0.0807 0.1187 0.062 Uiso 1 1 calc R . . Cl3 Cl 0.16840(15) 0.2690(3) 0.09289(15) 0.0950(9) Uani 1 1 d . . . Cl4 Cl 0.03518(18) 0.1491(3) 0.00341(18) 0.1176(13) Uani 1 1 d . . . C47 C 0.1044(5) 0.2365(9) 0.0069(5) 0.076(3) Uani 1 1 d . . . H47A H 0.0863 0.3172 -0.0180 0.092 Uiso 1 1 calc R . . H47B H 0.1266 0.1886 -0.0154 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01157(17) 0.01117(18) 0.01156(17) -0.00034(16) 0.00529(14) 0.00019(17) Br1 0.0211(3) 0.0273(3) 0.0180(2) -0.0015(2) 0.0083(2) 0.0021(2) P1 0.0130(6) 0.0110(6) 0.0153(6) -0.0008(5) 0.0072(5) -0.0018(5) P2 0.0142(6) 0.0117(6) 0.0134(6) -0.0001(5) 0.0076(5) 0.0005(5) Si1 0.0200(7) 0.0112(8) 0.0185(7) -0.0009(6) 0.0048(6) -0.0005(6) O1 0.0153(17) 0.0116(18) 0.0154(16) -0.0017(14) 0.0090(14) 0.0002(14) N1 0.032(3) 0.076(4) 0.021(3) 0.001(3) 0.011(2) -0.016(3) C1 0.012(2) 0.013(3) 0.014(2) -0.0010(19) 0.0051(19) 0.004(2) C2 0.018(2) 0.012(3) 0.012(2) -0.0017(19) 0.0040(19) -0.001(2) C3 0.019(3) 0.019(3) 0.018(2) -0.002(2) 0.010(2) -0.003(2) C4 0.026(3) 0.022(3) 0.020(3) -0.001(2) 0.012(2) 0.010(2) C5 0.026(3) 0.019(3) 0.024(3) -0.006(2) 0.010(2) 0.003(2) C6 0.020(3) 0.015(3) 0.014(2) 0.001(2) 0.004(2) 0.004(2) C7 0.015(2) 0.014(3) 0.009(2) 0.0048(19) 0.0034(19) 0.000(2) C8 0.018(2) 0.010(2) 0.015(2) 0.004(2) 0.0074(19) 0.002(2) C9 0.015(2) 0.017(3) 0.020(3) 0.002(2) 0.009(2) 0.003(2) C10 0.016(3) 0.023(3) 0.022(3) -0.002(2) 0.008(2) -0.008(2) C11 0.019(3) 0.016(3) 0.026(3) -0.003(2) 0.005(2) -0.008(2) C12 0.019(3) 0.011(3) 0.015(2) 0.004(2) 0.003(2) -0.002(2) C13 0.011(2) 0.016(3) 0.015(2) -0.004(2) 0.005(2) 0.001(2) C14 0.022(3) 0.020(3) 0.020(2) -0.001(2) 0.009(2) 0.001(2) C15 0.022(3) 0.029(3) 0.023(3) -0.003(3) 0.006(2) -0.004(3) C16 0.017(3) 0.040(4) 0.025(3) -0.003(3) 0.001(2) 0.003(3) C17 0.023(3) 0.026(3) 0.026(3) 0.004(2) 0.003(2) 0.011(3) C18 0.019(3) 0.015(3) 0.026(3) -0.004(2) 0.007(2) 0.001(2) C19 0.020(3) 0.009(3) 0.020(2) -0.0065(19) 0.012(2) -0.009(2) C20 0.019(3) 0.022(3) 0.025(3) -0.003(2) 0.014(2) -0.003(2) C21 0.028(3) 0.033(4) 0.031(3) -0.005(3) 0.021(3) -0.007(3) C22 0.036(3) 0.029(3) 0.021(3) -0.003(2) 0.019(3) -0.011(3) C23 0.036(3) 0.022(3) 0.028(3) 0.006(2) 0.018(3) -0.002(3) C24 0.022(3) 0.017(3) 0.026(3) -0.001(2) 0.014(2) 0.000(2) C25 0.012(2) 0.025(3) 0.012(2) 0.000(2) 0.007(2) 0.001(2) C26 0.021(3) 0.029(3) 0.022(3) -0.004(2) 0.014(2) -0.001(2) C27 0.024(3) 0.054(5) 0.018(3) -0.007(3) 0.011(2) 0.004(3) C28 0.034(4) 0.071(5) 0.022(3) 0.008(3) 0.017(3) 0.003(4) C29 0.042(4) 0.047(4) 0.026(3) 0.012(3) 0.013(3) -0.003(4) C30 0.028(3) 0.031(3) 0.020(3) 0.009(3) 0.010(2) 0.001(3) C31 0.016(2) 0.009(2) 0.017(2) 0.000(2) 0.007(2) 0.001(2) C32 0.020(3) 0.021(3) 0.023(3) 0.001(2) 0.014(2) 0.003(2) C33 0.022(3) 0.027(3) 0.027(3) 0.001(2) 0.017(2) 0.006(2) C34 0.019(3) 0.017(3) 0.033(3) 0.001(2) 0.012(2) 0.006(2) C35 0.019(3) 0.014(3) 0.023(3) 0.002(2) 0.009(2) 0.002(2) C36 0.019(3) 0.013(3) 0.018(2) 0.001(2) 0.012(2) -0.001(2) C37 0.011(2) 0.018(3) 0.019(2) 0.002(2) 0.0078(19) 0.002(2) C38 0.020(3) 0.016(3) 0.016(2) 0.001(2) 0.008(2) 0.000(2) C39 0.017(3) 0.027(3) 0.023(3) 0.009(2) 0.009(2) 0.007(2) C40 0.016(3) 0.036(3) 0.015(2) -0.002(2) 0.006(2) -0.003(2) C41 0.021(3) 0.019(3) 0.018(3) -0.003(2) 0.006(2) -0.005(2) C42 0.017(3) 0.020(3) 0.015(2) -0.002(2) 0.005(2) -0.001(2) C43 0.030(3) 0.024(3) 0.022(3) -0.005(2) 0.006(2) -0.004(3) C44 0.033(3) 0.019(3) 0.029(3) 0.007(2) 0.007(3) 0.005(3) C45 0.019(3) 0.045(4) 0.021(3) 0.000(3) 0.009(2) -0.007(3) Cl1 0.0433(10) 0.0399(10) 0.0709(12) 0.0099(9) 0.0303(9) 0.0035(8) Cl2 0.0567(12) 0.1015(19) 0.0640(12) 0.0375(13) 0.0342(10) 0.0220(13) C46 0.059(5) 0.041(4) 0.055(5) 0.006(4) 0.028(4) 0.001(4) Cl3 0.100(2) 0.0799(19) 0.109(2) 0.0117(16) 0.0547(18) 0.0286(16) Cl4 0.169(3) 0.086(2) 0.180(3) -0.072(2) 0.149(3) -0.055(2) C47 0.105(8) 0.065(6) 0.090(7) -0.012(5) 0.071(6) -0.006(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 C37 2.007(5) . ? Pd1 P1 2.2861(13) . ? Pd1 P2 2.2917(13) . ? Pd1 Br1 2.5343(8) . ? P1 C13 1.824(5) . ? P1 C19 1.835(5) . ? P1 C2 1.836(5) . ? P2 C25 1.818(5) . ? P2 C31 1.827(5) . ? P2 C8 1.834(5) . ? Si1 C43 1.850(5) . ? Si1 C12 1.849(5) . ? Si1 C44 1.853(5) . ? Si1 C6 1.857(5) . ? O1 C7 1.401(6) . ? O1 C1 1.402(5) . ? N1 C45 1.133(7) . ? C1 C6 1.401(7) . ? C1 C2 1.407(7) . ? C2 C3 1.407(7) . ? C3 C4 1.386(7) . ? C3 H3 0.9500 . ? C4 C5 1.369(8) . ? C4 H4 0.9500 . ? C5 C6 1.384(7) . ? C5 H5 0.9500 . ? C7 C12 1.388(7) . ? C7 C8 1.421(7) . ? C8 C9 1.400(7) . ? C9 C10 1.379(7) . ? C9 H9 0.9500 . ? C10 C11 1.366(7) . ? C10 H10 0.9500 . ? C11 C12 1.412(7) . ? C11 H11 0.9500 . ? C13 C18 1.381(7) . ? C13 C14 1.398(7) . ? C14 C15 1.379(7) . ? C14 H14 0.9500 . ? C15 C16 1.379(8) . ? C15 H15 0.9500 . ? C16 C17 1.379(8) . ? C16 H16 0.9500 . ? C17 C18 1.390(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.389(7) . ? C19 C24 1.394(7) . ? C20 C21 1.383(7) . ? C20 H20 0.9500 . ? C21 C22 1.384(8) . ? C21 H21 0.9500 . ? C22 C23 1.382(8) . ? C22 H22 0.9500 . ? C23 C24 1.389(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.392(8) . ? C25 C26 1.397(7) . ? C26 C27 1.375(7) . ? C26 H26 0.9500 . ? C27 C28 1.381(9) . ? C27 H27 0.9500 . ? C28 C29 1.361(9) . ? C28 H28 0.9500 . ? C29 C30 1.406(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.384(7) . ? C31 C32 1.405(7) . ? C32 C33 1.388(7) . ? C32 H32 0.9500 . ? C33 C34 1.380(7) . ? C33 H33 0.9500 . ? C34 C35 1.384(7) . ? C34 H34 0.9500 . ? C35 C36 1.389(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.385(7) . ? C37 C42 1.393(7) . ? C38 C39 1.381(7) . ? C38 H38 0.9500 . ? C39 C40 1.382(8) . ? C39 H39 0.9500 . ? C40 C41 1.388(7) . ? C40 C45 1.452(7) . ? C41 C42 1.395(7) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? Cl1 C46 1.751(7) . ? Cl2 C46 1.725(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? Cl3 C47 1.782(9) . ? Cl4 C47 1.737(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? 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 C37 Pd1 P1 89.95(14) . . ? C37 Pd1 P2 89.80(14) . . ? P1 Pd1 P2 152.15(5) . . ? C37 Pd1 Br1 178.19(15) . . ? P1 Pd1 Br1 89.89(4) . . ? P2 Pd1 Br1 91.18(4) . . ? C13 P1 C19 102.0(2) . . ? C13 P1 C2 103.8(2) . . ? C19 P1 C2 106.2(2) . . ? C13 P1 Pd1 117.33(16) . . ? C19 P1 Pd1 120.91(17) . . ? C2 P1 Pd1 105.00(17) . . ? C25 P2 C31 102.8(2) . . ? C25 P2 C8 102.6(2) . . ? C31 P2 C8 106.1(2) . . ? C25 P2 Pd1 117.03(16) . . ? C31 P2 Pd1 121.49(17) . . ? C8 P2 Pd1 104.79(16) . . ? C43 Si1 C12 112.3(2) . . ? C43 Si1 C44 109.9(3) . . ? C12 Si1 C44 111.8(2) . . ? C43 Si1 C6 110.9(2) . . ? C12 Si1 C6 99.5(2) . . ? C44 Si1 C6 112.1(3) . . ? C7 O1 C1 123.6(4) . . ? C6 C1 O1 121.4(4) . . ? C6 C1 C2 121.2(4) . . ? O1 C1 C2 117.3(4) . . ? C3 C2 C1 117.7(4) . . ? C3 C2 P1 117.6(4) . . ? C1 C2 P1 124.6(4) . . ? C4 C3 C2 121.2(5) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 119.3(5) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 122.4(5) . . ? C4 C5 H5 118.8 . . ? C6 C5 H5 118.8 . . ? C5 C6 C1 118.2(5) . . ? C5 C6 Si1 120.6(4) . . ? C1 C6 Si1 121.2(4) . . ? C12 C7 O1 122.1(4) . . ? C12 C7 C8 121.1(5) . . ? O1 C7 C8 116.8(4) . . ? C9 C8 C7 117.5(5) . . ? C9 C8 P2 117.1(4) . . ? C7 C8 P2 125.2(4) . . ? C10 C9 C8 122.2(5) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C11 C10 C9 118.9(5) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 122.1(5) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C7 C12 C11 118.1(5) . . ? C7 C12 Si1 121.2(4) . . ? C11 C12 Si1 120.6(4) . . ? C18 C13 C14 119.0(5) . . ? C18 C13 P1 123.1(4) . . ? C14 C13 P1 117.7(4) . . ? C15 C14 C13 120.5(5) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 119.9(5) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.3(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C18 120.0(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C13 C18 C17 120.3(5) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C24 119.4(5) . . ? C20 C19 P1 121.3(4) . . ? C24 C19 P1 119.3(4) . . ? C21 C20 C19 120.1(5) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.6(5) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.5(5) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 120.5(5) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 119.9(5) . . ? C23 C24 H24 120.1 . . ? C19 C24 H24 120.1 . . ? C30 C25 C26 119.2(5) . . ? C30 C25 P2 123.2(4) . . ? C26 C25 P2 117.4(4) . . ? C27 C26 C25 120.2(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.6(6) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C29 C28 C27 120.1(5) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.6(6) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C25 C30 C29 119.3(6) . . ? C25 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C36 C31 C32 118.2(5) . . ? C36 C31 P2 120.4(4) . . ? C32 C31 P2 121.4(4) . . ? C33 C32 C31 120.9(5) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C32 119.6(5) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 120.4(5) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 119.8(5) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C31 C36 C35 121.0(5) . . ? C31 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C38 C37 C42 117.9(5) . . ? C38 C37 Pd1 122.3(4) . . ? C42 C37 Pd1 119.8(4) . . ? C39 C38 C37 122.5(5) . . ? C39 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? C38 C39 C40 119.0(5) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C39 C40 C41 120.2(5) . . ? C39 C40 C45 120.6(5) . . ? C41 C40 C45 119.2(5) . . ? C40 C41 C42 119.9(5) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C37 C42 C41 120.6(5) . . ? C37 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? Si1 C43 H43A 109.5 . . ? Si1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si1 C44 H44A 109.5 . . ? Si1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N1 C45 C40 179.4(6) . . ? Cl2 C46 Cl1 113.7(4) . . ? Cl2 C46 H46A 108.8 . . ? Cl1 C46 H46A 108.8 . . ? Cl2 C46 H46B 108.8 . . ? Cl1 C46 H46B 108.8 . . ? H46A C46 H46B 107.7 . . ? Cl4 C47 Cl3 110.7(5) . . ? Cl4 C47 H47A 109.5 . . ? Cl3 C47 H47A 109.5 . . ? Cl4 C47 H47B 109.5 . . ? Cl3 C47 H47B 109.5 . . ? H47A C47 H47B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C37 Pd1 P1 C13 7.3(2) . . . . ? P2 Pd1 P1 C13 -82.2(2) . . . . ? Br1 Pd1 P1 C13 -174.53(19) . . . . ? C37 Pd1 P1 C19 -118.4(2) . . . . ? P2 Pd1 P1 C19 152.11(19) . . . . ? Br1 Pd1 P1 C19 59.79(18) . . . . ? C37 Pd1 P1 C2 121.9(2) . . . . ? P2 Pd1 P1 C2 32.4(2) . . . . ? Br1 Pd1 P1 C2 -59.94(16) . . . . ? C37 Pd1 P2 C25 -8.2(2) . . . . ? P1 Pd1 P2 C25 81.4(2) . . . . ? Br1 Pd1 P2 C25 173.4(2) . . . . ? C37 Pd1 P2 C31 119.1(2) . . . . ? P1 Pd1 P2 C31 -151.42(19) . . . . ? Br1 Pd1 P2 C31 -59.42(19) . . . . ? C37 Pd1 P2 C8 -121.0(2) . . . . ? P1 Pd1 P2 C8 -31.51(19) . . . . ? Br1 Pd1 P2 C8 60.49(15) . . . . ? C7 O1 C1 C6 -32.8(6) . . . . ? C7 O1 C1 C2 150.8(4) . . . . ? C6 C1 C2 C3 1.9(7) . . . . ? O1 C1 C2 C3 178.3(4) . . . . ? C6 C1 C2 P1 -176.6(4) . . . . ? O1 C1 C2 P1 -0.2(6) . . . . ? C13 P1 C2 C3 -76.1(4) . . . . ? C19 P1 C2 C3 31.0(4) . . . . ? Pd1 P1 C2 C3 160.1(3) . . . . ? C13 P1 C2 C1 102.4(4) . . . . ? C19 P1 C2 C1 -150.5(4) . . . . ? Pd1 P1 C2 C1 -21.4(4) . . . . ? C1 C2 C3 C4 0.2(7) . . . . ? P1 C2 C3 C4 178.8(4) . . . . ? C2 C3 C4 C5 -1.5(8) . . . . ? C3 C4 C5 C6 0.8(8) . . . . ? C4 C5 C6 C1 1.2(8) . . . . ? C4 C5 C6 Si1 -179.8(4) . . . . ? O1 C1 C6 C5 -178.8(4) . . . . ? C2 C1 C6 C5 -2.6(7) . . . . ? O1 C1 C6 Si1 2.2(6) . . . . ? C2 C1 C6 Si1 178.4(4) . . . . ? C43 Si1 C6 C5 -41.5(5) . . . . ? C12 Si1 C6 C5 -159.9(4) . . . . ? C44 Si1 C6 C5 81.8(5) . . . . ? C43 Si1 C6 C1 137.5(4) . . . . ? C12 Si1 C6 C1 19.1(4) . . . . ? C44 Si1 C6 C1 -99.3(4) . . . . ? C1 O1 C7 C12 34.3(6) . . . . ? C1 O1 C7 C8 -149.3(4) . . . . ? C12 C7 C8 C9 -0.2(7) . . . . ? O1 C7 C8 C9 -176.6(4) . . . . ? C12 C7 C8 P2 176.0(4) . . . . ? O1 C7 C8 P2 -0.5(6) . . . . ? C25 P2 C8 C9 74.2(4) . . . . ? C31 P2 C8 C9 -33.4(4) . . . . ? Pd1 P2 C8 C9 -163.1(3) . . . . ? C25 P2 C8 C7 -101.9(4) . . . . ? C31 P2 C8 C7 150.5(4) . . . . ? Pd1 P2 C8 C7 20.8(4) . . . . ? C7 C8 C9 C10 -1.4(7) . . . . ? P2 C8 C9 C10 -177.9(4) . . . . ? C8 C9 C10 C11 1.6(8) . . . . ? C9 C10 C11 C12 -0.2(8) . . . . ? O1 C7 C12 C11 177.8(4) . . . . ? C8 C7 C12 C11 1.5(7) . . . . ? O1 C7 C12 Si1 -4.4(6) . . . . ? C8 C7 C12 Si1 179.3(3) . . . . ? C10 C11 C12 C7 -1.3(8) . . . . ? C10 C11 C12 Si1 -179.2(4) . . . . ? C43 Si1 C12 C7 -135.5(4) . . . . ? C44 Si1 C12 C7 100.5(4) . . . . ? C6 Si1 C12 C7 -18.1(4) . . . . ? C43 Si1 C12 C11 42.3(5) . . . . ? C44 Si1 C12 C11 -81.8(5) . . . . ? C6 Si1 C12 C11 159.7(4) . . . . ? C19 P1 C13 C18 -126.5(4) . . . . ? C2 P1 C13 C18 -16.3(5) . . . . ? Pd1 P1 C13 C18 99.0(4) . . . . ? C19 P1 C13 C14 59.2(4) . . . . ? C2 P1 C13 C14 169.4(4) . . . . ? Pd1 P1 C13 C14 -75.3(4) . . . . ? C18 C13 C14 C15 -0.4(8) . . . . ? P1 C13 C14 C15 174.2(4) . . . . ? C13 C14 C15 C16 -0.4(8) . . . . ? C14 C15 C16 C17 0.7(9) . . . . ? C15 C16 C17 C18 -0.1(9) . . . . ? C14 C13 C18 C17 0.9(8) . . . . ? P1 C13 C18 C17 -173.3(4) . . . . ? C16 C17 C18 C13 -0.7(9) . . . . ? C13 P1 C19 C20 34.5(5) . . . . ? C2 P1 C19 C20 -73.9(4) . . . . ? Pd1 P1 C19 C20 166.9(3) . . . . ? C13 P1 C19 C24 -144.5(4) . . . . ? C2 P1 C19 C24 107.2(4) . . . . ? Pd1 P1 C19 C24 -12.0(5) . . . . ? C24 C19 C20 C21 -2.8(8) . . . . ? P1 C19 C20 C21 178.3(4) . . . . ? C19 C20 C21 C22 1.0(8) . . . . ? C20 C21 C22 C23 0.6(8) . . . . ? C21 C22 C23 C24 -0.5(8) . . . . ? C22 C23 C24 C19 -1.3(8) . . . . ? C20 C19 C24 C23 2.9(8) . . . . ? P1 C19 C24 C23 -178.1(4) . . . . ? C31 P2 C25 C30 120.0(4) . . . . ? C8 P2 C25 C30 9.9(5) . . . . ? Pd1 P2 C25 C30 -104.2(4) . . . . ? C31 P2 C25 C26 -64.3(4) . . . . ? C8 P2 C25 C26 -174.3(4) . . . . ? Pd1 P2 C25 C26 71.6(4) . . . . ? C30 C25 C26 C27 -0.2(8) . . . . ? P2 C25 C26 C27 -176.2(4) . . . . ? C25 C26 C27 C28 -0.2(8) . . . . ? C26 C27 C28 C29 0.3(9) . . . . ? C27 C28 C29 C30 0.0(10) . . . . ? C26 C25 C30 C29 0.5(8) . . . . ? P2 C25 C30 C29 176.2(4) . . . . ? C28 C29 C30 C25 -0.4(9) . . . . ? C25 P2 C31 C36 157.6(4) . . . . ? C8 P2 C31 C36 -94.9(4) . . . . ? Pd1 P2 C31 C36 24.3(5) . . . . ? C25 P2 C31 C32 -20.8(5) . . . . ? C8 P2 C31 C32 86.6(4) . . . . ? Pd1 P2 C31 C32 -154.1(4) . . . . ? C36 C31 C32 C33 0.4(8) . . . . ? P2 C31 C32 C33 178.8(4) . . . . ? C31 C32 C33 C34 -0.2(8) . . . . ? C32 C33 C34 C35 0.1(8) . . . . ? C33 C34 C35 C36 -0.2(8) . . . . ? C32 C31 C36 C35 -0.4(7) . . . . ? P2 C31 C36 C35 -178.9(4) . . . . ? C34 C35 C36 C31 0.3(8) . . . . ? P1 Pd1 C37 C38 -78.7(4) . . . . ? P2 Pd1 C37 C38 73.4(4) . . . . ? P1 Pd1 C37 C42 102.1(4) . . . . ? P2 Pd1 C37 C42 -105.7(4) . . . . ? C42 C37 C38 C39 0.2(7) . . . . ? Pd1 C37 C38 C39 -179.0(4) . . . . ? C37 C38 C39 C40 0.3(8) . . . . ? C38 C39 C40 C41 -1.1(8) . . . . ? C38 C39 C40 C45 -179.7(5) . . . . ? C39 C40 C41 C42 1.4(8) . . . . ? C45 C40 C41 C42 179.9(5) . . . . ? C38 C37 C42 C41 0.1(7) . . . . ? Pd1 C37 C42 C41 179.2(4) . . . . ? C40 C41 C42 C37 -0.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.821 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.130 #===END # Compound 1d data_s2099a _database_code_CSD 177712 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H34 Br N O P2 Pd S, C H2 Cl2' _chemical_formula_sum 'C46 H36 Br Cl2 N O P2 Pd S' _chemical_formula_weight 969.97 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' 'Br' 'Br' -0.2901 2.4595 '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' 'Pd' 'Pd' -0.9988 1.0072 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P nma' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 18.47910(10) _cell_length_b 15.15340(10) _cell_length_c 14.92570(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4179.51(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 1.691 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.77 _exptl_absorpt_correction_T_max 0.86 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75073 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4971 _reflns_number_gt 4527 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'DENZO 1.11.0' _computing_data_reduction 'DENZO 1.11.0' _computing_structure_solution 'DIRDIF-97 (Beurskens et al., 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+4.2377P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constraint _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4971 _refine_ls_number_parameters 272 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.663915(10) 0.7500 0.725310(12) 0.01411(6) Uani 1 2 d S . . Br2 Br 0.741295(16) 0.7500 0.867416(18) 0.02213(8) Uani 1 2 d S . . P3 P 0.68815(3) 0.60313(3) 0.71160(3) 0.01508(10) Uani 1 1 d . . . C4 C 0.78785(10) 0.59949(13) 0.71128(12) 0.0177(4) Uani 1 1 d . . . C5 C 0.82266(11) 0.52050(14) 0.73385(13) 0.0228(4) Uani 1 1 d . . . H5 H 0.7940 0.4713 0.7511 0.027 Uiso 1 1 calc R . . C6 C 0.89775(11) 0.51120(15) 0.73198(14) 0.0251(4) Uani 1 1 d . . . C7 C 0.93293(13) 0.42628(15) 0.76110(18) 0.0363(5) Uani 1 1 d . . . H7A H 0.9348 0.4240 0.8267 0.055 Uiso 1 1 calc R . . H7B H 0.9822 0.4234 0.7370 0.055 Uiso 1 1 calc R . . H7C H 0.9047 0.3762 0.7386 0.055 Uiso 1 1 calc R . . C8 C 0.93853(11) 0.58324(14) 0.70491(13) 0.0238(4) Uani 1 1 d . . . H8 H 0.9898 0.5787 0.7032 0.029 Uiso 1 1 calc R . . C9 C 0.90548(10) 0.66204(14) 0.68019(13) 0.0199(4) Uani 1 1 d . . . C10 C 0.83062(10) 0.67090(13) 0.68399(12) 0.0174(4) Uani 1 1 d . . . O11 O 0.79867(10) 0.7500 0.65614(12) 0.0171(4) Uani 1 2 d S . . S12 S 0.95871(4) 0.7500 0.63871(5) 0.02361(15) Uani 1 2 d S . . C13 C 0.65463(10) 0.53073(13) 0.80048(13) 0.0202(4) Uani 1 1 d . . . C14 C 0.65332(13) 0.43900(15) 0.79126(16) 0.0308(5) Uani 1 1 d . . . H14 H 0.6719 0.4122 0.7385 0.037 Uiso 1 1 calc R . . C15 C 0.62471(17) 0.38689(18) 0.85960(18) 0.0461(7) Uani 1 1 d . . . H15 H 0.6241 0.3245 0.8533 0.055 Uiso 1 1 calc R . . C16 C 0.59736(15) 0.42499(19) 0.93603(17) 0.0440(7) Uani 1 1 d . . . H16 H 0.5786 0.3888 0.9825 0.053 Uiso 1 1 calc R . . C17 C 0.59711(12) 0.51557(17) 0.94550(15) 0.0331(5) Uani 1 1 d . . . H17 H 0.5777 0.5417 0.9981 0.040 Uiso 1 1 calc R . . C18 C 0.62539(11) 0.56861(15) 0.87778(13) 0.0246(4) Uani 1 1 d . . . H18 H 0.6248 0.6310 0.8842 0.030 Uiso 1 1 calc R . . C19 C 0.66641(10) 0.54123(12) 0.61044(12) 0.0176(4) Uani 1 1 d . . . C20 C 0.59646(11) 0.50875(14) 0.59968(14) 0.0234(4) Uani 1 1 d . . . H20 H 0.5603 0.5225 0.6427 0.028 Uiso 1 1 calc R . . C21 C 0.57927(12) 0.45647(14) 0.52659(14) 0.0260(4) Uani 1 1 d . . . H21 H 0.5319 0.4328 0.5208 0.031 Uiso 1 1 calc R . . C22 C 0.63080(13) 0.43858(15) 0.46208(14) 0.0305(5) Uani 1 1 d . . . H22 H 0.6190 0.4027 0.4119 0.037 Uiso 1 1 calc R . . C23 C 0.69939(13) 0.47297(19) 0.47082(15) 0.0379(6) Uani 1 1 d . . . H23 H 0.7346 0.4617 0.4259 0.045 Uiso 1 1 calc R . . C24 C 0.71757(12) 0.52401(16) 0.54486(14) 0.0283(5) Uani 1 1 d . . . H24 H 0.7651 0.5471 0.5505 0.034 Uiso 1 1 calc R . . C25 C 0.60374(14) 0.7500 0.61343(18) 0.0168(5) Uani 1 2 d S . . C26 C 0.63537(16) 0.7500 0.52824(19) 0.0234(6) Uani 1 2 d S . . H26 H 0.6866 0.7500 0.5231 0.028 Uiso 1 2 calc SR . . C27 C 0.59337(18) 0.7500 0.4511(2) 0.0263(6) Uani 1 2 d S . . H27 H 0.6157 0.7500 0.3938 0.032 Uiso 1 2 calc SR . . C28 C 0.51792(17) 0.7500 0.4586(2) 0.0252(6) Uani 1 2 d S . . C29 C 0.48568(16) 0.7500 0.5424(2) 0.0247(6) Uani 1 2 d S . . H29 H 0.4344 0.7500 0.5475 0.030 Uiso 1 2 calc SR . . C30 C 0.52845(15) 0.7500 0.61916(19) 0.0202(5) Uani 1 2 d S . . H30 H 0.5060 0.7500 0.6764 0.024 Uiso 1 2 calc SR . . C31 C 0.4737(2) 0.7500 0.3788(2) 0.0338(8) Uani 1 2 d S . . N32 N 0.4382(2) 0.7500 0.3157(2) 0.0488(9) Uani 1 2 d S . . C33 C 0.3015(3) 0.2500 0.9092(4) 0.156(4) Uani 1 2 d SDU . . H33A H 0.2802 0.1973 0.9381 0.187 Uiso 0.50 1 calc PR . . H33B H 0.2802 0.3027 0.9381 0.187 Uiso 0.50 1 calc PR . . Cl34 Cl 0.27736(8) 0.2500 0.79743(9) 0.0675(3) Uani 1 2 d SD . . Cl35 Cl 0.39505(9) 0.2500 0.92874(9) 0.0805(4) Uani 1 2 d SD . . 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 0.01321(11) 0.01549(10) 0.01362(10) 0.000 -0.00098(7) 0.000 Br2 0.02465(15) 0.02430(15) 0.01744(13) 0.000 -0.00402(10) 0.000 P3 0.0138(2) 0.0157(2) 0.0157(2) -0.00027(17) -0.00087(16) -0.00032(17) C4 0.0142(9) 0.0219(9) 0.0171(8) -0.0021(7) -0.0022(7) 0.0025(7) C5 0.0211(10) 0.0215(10) 0.0257(10) -0.0015(8) -0.0046(8) 0.0021(8) C6 0.0211(10) 0.0263(11) 0.0280(10) -0.0056(8) -0.0068(8) 0.0074(8) C7 0.0277(12) 0.0268(12) 0.0545(15) -0.0019(10) -0.0099(11) 0.0097(10) C8 0.0154(9) 0.0314(11) 0.0246(10) -0.0053(8) -0.0024(7) 0.0067(8) C9 0.0155(9) 0.0264(10) 0.0177(9) -0.0029(7) 0.0000(7) 0.0009(8) C10 0.0152(9) 0.0221(9) 0.0149(8) -0.0021(7) -0.0017(7) 0.0028(7) O11 0.0135(9) 0.0193(9) 0.0186(9) 0.000 -0.0006(7) 0.000 S12 0.0134(3) 0.0330(4) 0.0244(3) 0.000 0.0038(3) 0.000 C13 0.0184(9) 0.0227(10) 0.0194(9) 0.0047(8) -0.0024(7) -0.0031(8) C14 0.0383(13) 0.0244(11) 0.0297(11) 0.0041(9) -0.0035(9) -0.0023(9) C15 0.0658(19) 0.0274(12) 0.0452(15) 0.0143(11) -0.0044(13) -0.0110(12) C16 0.0524(16) 0.0504(16) 0.0292(12) 0.0187(11) -0.0036(11) -0.0172(13) C17 0.0301(12) 0.0482(14) 0.0211(10) 0.0062(10) 0.0009(8) -0.0097(10) C18 0.0200(10) 0.0324(11) 0.0214(9) 0.0010(8) -0.0009(8) -0.0047(8) C19 0.0190(9) 0.0167(9) 0.0172(8) -0.0008(7) -0.0019(7) -0.0005(7) C20 0.0194(10) 0.0274(10) 0.0234(10) -0.0035(8) 0.0015(8) -0.0028(8) C21 0.0247(11) 0.0266(11) 0.0268(10) -0.0027(8) -0.0031(8) -0.0068(8) C22 0.0368(13) 0.0325(11) 0.0221(10) -0.0093(9) -0.0035(9) -0.0042(10) C23 0.0293(12) 0.0600(17) 0.0245(11) -0.0154(11) 0.0065(9) -0.0036(11) C24 0.0206(10) 0.0425(13) 0.0219(10) -0.0062(9) 0.0034(8) -0.0064(9) C25 0.0174(13) 0.0158(12) 0.0172(12) 0.000 -0.0028(10) 0.000 C26 0.0228(14) 0.0260(14) 0.0213(14) 0.000 -0.0006(11) 0.000 C27 0.0372(17) 0.0249(15) 0.0168(13) 0.000 -0.0021(12) 0.000 C28 0.0335(16) 0.0160(13) 0.0261(15) 0.000 -0.0152(12) 0.000 C29 0.0194(14) 0.0216(14) 0.0332(16) 0.000 -0.0079(12) 0.000 C30 0.0185(13) 0.0198(13) 0.0222(13) 0.000 -0.0019(10) 0.000 C31 0.0439(19) 0.0210(15) 0.0364(18) 0.000 -0.0185(15) 0.000 N32 0.064(2) 0.0405(18) 0.0423(18) 0.000 -0.0311(17) 0.000 C33 0.103(6) 0.320(14) 0.044(3) 0.000 0.007(4) 0.000 Cl34 0.0680(8) 0.0630(7) 0.0715(8) 0.000 0.0034(6) 0.000 Cl35 0.0935(10) 0.0977(11) 0.0504(7) 0.000 0.0008(7) 0.000 _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 C25 2.006(3) . ? Pd1 P3 2.2794(5) 8_575 ? Pd1 P3 2.2794(5) . ? Pd1 Br2 2.5580(3) . ? P3 C19 1.8223(19) . ? P3 C13 1.829(2) . ? P3 C4 1.8433(19) . ? C4 C5 1.400(3) . ? C4 C10 1.401(3) . ? C5 C6 1.395(3) . ? C5 H5 0.9500 . ? C6 C8 1.387(3) . ? C6 C7 1.506(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.391(3) . ? C8 H8 0.9500 . ? C9 C10 1.391(3) . ? C9 S12 1.769(2) . ? C10 O11 1.399(2) . ? O11 C10 1.399(2) 8_575 ? S12 C9 1.769(2) 8_575 ? C13 C14 1.397(3) . ? C13 C18 1.397(3) . ? C14 C15 1.394(3) . ? C14 H14 0.9500 . ? C15 C16 1.375(4) . ? C15 H15 0.9500 . ? C16 C17 1.380(4) . ? C16 H16 0.9500 . ? C17 C18 1.393(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.386(3) . ? C19 C20 1.393(3) . ? C20 C21 1.385(3) . ? C20 H20 0.9500 . ? C21 C22 1.381(3) . ? C21 H21 0.9500 . ? C22 C23 1.377(3) . ? C22 H22 0.9500 . ? C23 C24 1.390(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.394(4) . ? C25 C26 1.399(4) . ? C26 C27 1.388(4) . ? C26 H26 0.9500 . ? C27 C28 1.399(5) . ? C27 H27 0.9500 . ? C28 C29 1.386(4) . ? C28 C31 1.445(4) . ? C29 C30 1.392(4) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 N32 1.147(4) . ? C33 Cl34 1.726(5) . ? C33 Cl35 1.753(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 C25 Pd1 P3 91.96(2) . 8_575 ? C25 Pd1 P3 91.96(2) . . ? P3 Pd1 P3 155.05(3) 8_575 . ? C25 Pd1 Br2 179.67(8) . . ? P3 Pd1 Br2 87.971(13) 8_575 . ? P3 Pd1 Br2 87.973(13) . . ? C19 P3 C13 102.57(9) . . ? C19 P3 C4 101.70(8) . . ? C13 P3 C4 108.80(9) . . ? C19 P3 Pd1 122.25(6) . . ? C13 P3 Pd1 116.99(7) . . ? C4 P3 Pd1 103.05(6) . . ? C5 C4 C10 118.12(17) . . ? C5 C4 P3 118.95(15) . . ? C10 C4 P3 122.80(14) . . ? C6 C5 C4 122.6(2) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C8 C6 C5 117.83(19) . . ? C8 C6 C7 121.48(19) . . ? C5 C6 C7 120.7(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 C9 120.96(18) . . ? C6 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 120.58(19) . . ? C10 C9 S12 119.64(16) . . ? C8 C9 S12 119.71(15) . . ? C9 C10 O11 119.36(18) . . ? C9 C10 C4 119.89(18) . . ? O11 C10 C4 120.67(16) . . ? C10 O11 C10 117.9(2) . 8_575 ? C9 S12 C9 97.82(13) . 8_575 ? C14 C13 C18 118.9(2) . . ? C14 C13 P3 122.08(17) . . ? C18 C13 P3 118.90(16) . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 120.6(2) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C17 120.3(2) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 119.9(2) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C13 120.5(2) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C24 C19 C20 119.04(18) . . ? C24 C19 P3 122.13(15) . . ? C20 C19 P3 118.82(15) . . ? C21 C20 C19 120.39(19) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C20 120.2(2) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C23 C22 C21 119.6(2) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 120.6(2) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C19 C24 C23 120.1(2) . . ? C19 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C30 C25 C26 118.2(3) . . ? C30 C25 Pd1 120.1(2) . . ? C26 C25 Pd1 121.6(2) . . ? C27 C26 C25 121.3(3) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C28 119.4(3) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C29 C28 C27 120.0(3) . . ? C29 C28 C31 120.1(3) . . ? C27 C28 C31 119.9(3) . . ? C28 C29 C30 119.9(3) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C29 C30 C25 121.1(3) . . ? C29 C30 H30 119.5 . . ? C25 C30 H30 119.5 . . ? N32 C31 C28 179.6(4) . . ? Cl34 C33 Cl35 114.6(4) . . ? Cl34 C33 H33A 108.6 . . ? Cl35 C33 H33A 108.6 . . ? Cl34 C33 H33B 108.6 . . ? Cl35 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C25 Pd1 P3 C19 10.88(11) . . . . ? P3 Pd1 P3 C19 -88.01(9) 8_575 . . . ? Br2 Pd1 P3 C19 -168.80(7) . . . . ? C25 Pd1 P3 C13 -116.72(10) . . . . ? P3 Pd1 P3 C13 144.39(8) 8_575 . . . ? Br2 Pd1 P3 C13 63.60(7) . . . . ? C25 Pd1 P3 C4 123.98(10) . . . . ? P3 Pd1 P3 C4 25.09(9) 8_575 . . . ? Br2 Pd1 P3 C4 -55.70(6) . . . . ? C19 P3 C4 C5 -73.90(16) . . . . ? C13 P3 C4 C5 33.87(18) . . . . ? Pd1 P3 C4 C5 158.70(14) . . . . ? C19 P3 C4 C10 102.00(16) . . . . ? C13 P3 C4 C10 -150.23(16) . . . . ? Pd1 P3 C4 C10 -25.40(16) . . . . ? C10 C4 C5 C6 1.4(3) . . . . ? P3 C4 C5 C6 177.52(16) . . . . ? C4 C5 C6 C8 -1.2(3) . . . . ? C4 C5 C6 C7 177.0(2) . . . . ? C5 C6 C8 C9 -0.2(3) . . . . ? C7 C6 C8 C9 -178.5(2) . . . . ? C6 C8 C9 C10 1.4(3) . . . . ? C6 C8 C9 S12 -175.67(16) . . . . ? C8 C9 C10 O11 -178.07(18) . . . . ? S12 C9 C10 O11 -1.0(3) . . . . ? C8 C9 C10 C4 -1.2(3) . . . . ? S12 C9 C10 C4 175.87(14) . . . . ? C5 C4 C10 C9 -0.2(3) . . . . ? P3 C4 C10 C9 -176.11(14) . . . . ? C5 C4 C10 O11 176.64(17) . . . . ? P3 C4 C10 O11 0.7(3) . . . . ? C9 C10 O11 C10 -44.0(3) . . . 8_575 ? C4 C10 O11 C10 139.15(15) . . . 8_575 ? C10 C9 S12 C9 34.7(2) . . . 8_575 ? C8 C9 S12 C9 -148.15(12) . . . 8_575 ? C19 P3 C13 C14 30.4(2) . . . . ? C4 P3 C13 C14 -76.75(19) . . . . ? Pd1 P3 C13 C14 167.08(16) . . . . ? C19 P3 C13 C18 -145.62(16) . . . . ? C4 P3 C13 C18 107.21(16) . . . . ? Pd1 P3 C13 C18 -8.97(18) . . . . ? C18 C13 C14 C15 -1.5(3) . . . . ? P3 C13 C14 C15 -177.57(19) . . . . ? C13 C14 C15 C16 0.3(4) . . . . ? C14 C15 C16 C17 0.8(4) . . . . ? C15 C16 C17 C18 -0.7(4) . . . . ? C16 C17 C18 C13 -0.5(3) . . . . ? C14 C13 C18 C17 1.6(3) . . . . ? P3 C13 C18 C17 177.81(16) . . . . ? C13 P3 C19 C24 -128.50(18) . . . . ? C4 P3 C19 C24 -16.0(2) . . . . ? Pd1 P3 C19 C24 97.82(18) . . . . ? C13 P3 C19 C20 50.20(18) . . . . ? C4 P3 C19 C20 162.74(16) . . . . ? Pd1 P3 C19 C20 -83.48(17) . . . . ? C24 C19 C20 C21 3.1(3) . . . . ? P3 C19 C20 C21 -175.68(16) . . . . ? C19 C20 C21 C22 -2.2(3) . . . . ? C20 C21 C22 C23 0.0(4) . . . . ? C21 C22 C23 C24 1.3(4) . . . . ? C20 C19 C24 C23 -1.7(3) . . . . ? P3 C19 C24 C23 176.97(19) . . . . ? C22 C23 C24 C19 -0.4(4) . . . . ? P3 Pd1 C25 C30 -102.321(13) 8_575 . . . ? P3 Pd1 C25 C30 102.321(13) . . . . ? P3 Pd1 C25 C26 77.679(13) 8_575 . . . ? P3 Pd1 C25 C26 -77.679(13) . . . . ? C30 C25 C26 C27 0.0 . . . . ? Pd1 C25 C26 C27 180.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C26 C27 C28 C31 180.0 . . . . ? C27 C28 C29 C30 0.0 . . . . ? C31 C28 C29 C30 180.0 . . . . ? C28 C29 C30 C25 0.0 . . . . ? C26 C25 C30 C29 0.0 . . . . ? Pd1 C25 C30 C29 180.0 . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.607 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.120 #===END # Compound 2b data_Compound_2b _database_code_CSD 177713 # 2. EXPERIMENTAL DATA #--------------------- _publ_section_exptl_prep #<< material & crystal preparation text ; ? ; _publ_section_exptl_refinement #<< crystallographic methods #used ; ? ; _chemical_formula_sum 'C40 H35 Cl O P2 Pd . C4 H10 O' _chemical_formula_moiety 'C40 H35 Cl O P2 Pd' _chemical_formula_weight 735.5 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.7823(9) _cell_length_b 17.9540(10) _cell_length_c 16.961(2) _cell_angle_alpha 90.00000 _cell_angle_beta 93.290(5) _cell_angle_gamma 90.00000 _cell_volume 3886.0(6) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 40.11 _cell_measurement_theta_max 40.89 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 5.65 _exptl_crystal_description cube _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour yellow #<< use NfA code _diffrn_measurement_device_type CAD4 _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type PSI-scans _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 1.00 _exptl_absorpt_correction_T_max 3.04 _diffrn_reflns_number 7967 _reflns_number_total 7967 _reflns_Friedel_coverage ? _reflns_number_gt 6830 _reflns_threshold_expression 'Iobs > 2.50 sig(Iobs)' _diffrn_reflns_theta_max 74.77 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 #<< do not append units _diffrn_standards_decay_% 5 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .061 _refine_ls_wR_factor_ref .064 _refine_ls_goodness_of_fit_ref .928 _refine_ls_number_reflns 6807 _refine_ls_number_parameters 567 _refine_ls_weighting_scheme '1/[10.+0.001*\s(Fobs)^2^+0.0001/\s(Fobs)]' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max .27 _refine_diff_density_min -2.998 _refine_diff_density_max 1.568 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 1322(71) _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack .00000 # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'xtal DIFDAT ADDREF SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 160 .017 .009 'Int. Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 140 0 0 'Int. Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 4 .047 .032 'Int. Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .283 .434 'Int. Tables Vol IV Tables 2.2B and 2.3.1' Cl ? 0 4 .348 .702 'Int. Tables Vol IV Tables 2.2B and 2.3.1' Pd ? 0 4 -.059 3.934 'Int. Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pd Pd Uani 0.27573(3) 0.63789(2) 0.32547(2) 1.000 0.0351(1) . . Cl Cl Uani 0.10362(11) 0.58546(10) 0.29232(9) 1.000 0.0505(5) . . P1 P Uani 0.34711(11) 0.54714(9) 0.24985(8) 1.000 0.0369(4) . . P2 P Uani 0.21812(11) 0.68258(9) 0.44188(8) 1.000 0.0370(4) . . O O Uani 0.2894(3) 0.5200(2) 0.4203(2) 1.000 0.0377(12) . . C1 C Uani 0.4220(5) 0.6906(4) 0.3463(4) 1.000 0.045(2) . . C2 C Uani 0.2394(5) 0.3912(4) 0.4992(4) 1.000 0.0475(19) . . C3 C Uani 0.3496(6) 0.3896(5) 0.5398(5) 1.000 0.061(3) . . C4 C Uani 0.1785(7) 0.3235(5) 0.5270(5) 1.000 0.068(3) . . C11 C Uani 0.3046(5) 0.4601(3) 0.2946(3) 1.000 0.0412(17) . . C12 C Uani 0.2943(6) 0.3948(4) 0.2507(4) 1.000 0.052(2) . . C13 C Uani 0.2606(6) 0.3290(4) 0.2838(5) 1.000 0.060(3) . . C14 C Uani 0.2403(6) 0.3268(4) 0.3634(4) 1.000 0.056(2) . . C15 C Uani 0.2505(5) 0.3896(3) 0.4100(4) 1.000 0.0439(17) . . C16 C Uani 0.2809(4) 0.4557(3) 0.3747(3) 1.000 0.0386(17) . . C21 C Uani 0.1769(4) 0.5985(3) 0.4939(3) 1.000 0.0384(17) . . C22 C Uani 0.1046(5) 0.6036(4) 0.5523(3) 1.000 0.0459(19) . . C23 C Uani 0.0698(5) 0.5406(4) 0.5903(4) 1.000 0.053(2) . . C24 C Uani 0.1107(5) 0.4722(4) 0.5740(4) 1.000 0.0491(19) . . C25 C Uani 0.1858(4) 0.4637(4) 0.5182(3) 1.000 0.0422(19) . . C26 C Uani 0.2157(4) 0.5277(3) 0.4787(3) 1.000 0.0371(17) . . C31 C Uani 0.4887(4) 0.5365(3) 0.2483(3) 1.000 0.0397(17) . . C32 C Uani 0.5445(6) 0.4830(4) 0.2912(5) 1.000 0.059(3) . . C33 C Uani 0.6531(6) 0.4787(5) 0.2881(6) 1.000 0.074(3) . . C34 C Uani 0.7065(6) 0.5259(5) 0.2432(5) 1.000 0.069(3) . . C35 C Uani 0.6520(6) 0.5805(5) 0.2008(4) 1.000 0.066(3) . . C36 C Uani 0.5445(5) 0.5865(4) 0.2037(4) 1.000 0.054(3) . . C41 C Uani 0.3077(4) 0.5434(3) 0.1444(3) 1.000 0.0400(17) . . C42 C Uani 0.2293(5) 0.5925(5) 0.1157(4) 1.000 0.053(2) . . C43 C Uani 0.1983(6) 0.5918(5) 0.0360(4) 1.000 0.067(3) . . C44 C Uani 0.2425(6) 0.5424(5) -0.0145(4) 1.000 0.066(3) . . C45 C Uani 0.3199(7) 0.4947(4) 0.0124(4) 1.000 0.061(3) . . C46 C Uani 0.3540(6) 0.4955(4) 0.0919(4) 1.000 0.052(2) . . C51 C Uani 0.3113(5) 0.7267(4) 0.5133(3) 1.000 0.0437(19) . . C52 C Uani 0.3214(6) 0.8033(4) 0.5158(5) 1.000 0.066(3) . . C53 C Uani 0.3957(7) 0.8352(5) 0.5702(6) 1.000 0.083(4) . . C54 C Uani 0.4608(7) 0.7922(6) 0.6180(5) 1.000 0.083(4) . . C55 C Uani 0.4539(7) 0.7162(6) 0.6130(5) 1.000 0.078(3) . . C56 C Uani 0.3787(6) 0.6830(5) 0.5608(4) 1.000 0.063(3) . . C61 C Uani 0.1064(4) 0.7466(3) 0.4359(3) 1.000 0.0406(17) . . C62 C Uani 0.0710(5) 0.7869(4) 0.4992(4) 1.000 0.051(2) . . C63 C Uani -0.0111(6) 0.8365(4) 0.4880(4) 1.000 0.058(2) . . C64 C Uani -0.0570(6) 0.8479(4) 0.4131(5) 1.000 0.062(3) . . C65 C Uani -0.0224(6) 0.8086(4) 0.3505(4) 1.000 0.058(2) . . C66 C Uani 0.0588(5) 0.7585(4) 0.3607(4) 1.000 0.048(2) . . O1S O Uiso -0.1099(9) 0.3812(7) 0.1778(7) 1.000 0.178(4) . . C1S C Uiso -0.0029(11) 0.4059(9) 0.1906(9) 1.000 0.156(6) . . C2S C Uiso 0.0369(12) 0.4437(8) 0.1193(8) 1.000 0.146(5) . . C3S C Uiso -0.1029(17) 0.3227(11) 0.2350(13) 1.000 0.259(11) . . C4S C Uiso -0.2029(15) 0.2796(12) 0.2309(12) 1.000 0.204(8) . . H12 H Uiso 0.31039 0.39527 0.19792 1.000 0.0630 . . H13 H Uiso 0.25162 0.28649 0.25283 1.000 0.0720 . . H14 H Uiso 0.21948 0.28222 0.38561 1.000 0.0670 . . H22 H Uiso 0.07927 0.65011 0.56600 1.000 0.0550 . . H23 H Uiso 0.01864 0.54484 0.62688 1.000 0.0640 . . H24 H Uiso 0.08792 0.43053 0.60070 1.000 0.0590 . . H32 H Uiso 0.50954 0.44963 0.32235 1.000 0.0710 . . H33 H Uiso 0.68961 0.44248 0.31764 1.000 0.0890 . . H34 H Uiso 0.77877 0.52169 0.24088 1.000 0.0830 . . H35 H Uiso 0.68798 0.61357 0.16998 1.000 0.0790 . . H36 H Uiso 0.50901 0.62419 0.17568 1.000 0.0640 . . H42 H Uiso 0.19830 0.62530 0.14982 1.000 0.0640 . . H43 H Uiso 0.14725 0.62497 0.01651 1.000 0.0800 . . H44 H Uiso 0.21945 0.54147 -0.06750 1.000 0.0790 . . H45 H Uiso 0.34970 0.46182 -0.02226 1.000 0.0730 . . H46 H Uiso 0.40786 0.46395 0.11002 1.000 0.0630 . . H52 H Uiso 0.27978 0.83329 0.48209 1.000 0.0790 . . H53 H Uiso 0.40062 0.88679 0.57371 1.000 0.1000 . . H54 H Uiso 0.50935 0.81435 0.65360 1.000 0.1000 . . H55 H Uiso 0.49919 0.68656 0.64430 1.000 0.0930 . . H56 H Uiso 0.37394 0.63137 0.55798 1.000 0.0760 . . H62 H Uiso 0.10286 0.78038 0.54941 1.000 0.0610 . . H63 H Uiso -0.03554 0.86225 0.53082 1.000 0.0700 . . H64 H Uiso -0.11119 0.88215 0.40530 1.000 0.0740 . . H65 H Uiso -0.05419 0.81585 0.30039 1.000 0.0700 . . H66 H Uiso 0.08198 0.73258 0.31755 1.000 0.0580 . . H101 H Uiso 0.41851 0.72444 0.38989 1.000 0.0680 . . H102 H Uiso 0.43927 0.71764 0.29998 1.000 0.0680 . . H103 H Uiso 0.47486 0.65373 0.35852 1.000 0.0680 . . H301 H Uiso 0.38341 0.34359 0.52767 1.000 0.0920 . . H302 H Uiso 0.34469 0.39364 0.59591 1.000 0.0920 . . H303 H Uiso 0.38974 0.43057 0.52126 1.000 0.0920 . . H401 H Uiso 0.21473 0.27871 0.51398 1.000 0.1020 . . H402 H Uiso 0.10960 0.32322 0.50129 1.000 0.1020 . . H403 H Uiso 0.17301 0.32615 0.58314 1.000 0.1020 . . H1S H Uiso 0.04129 0.36334 0.20418 1.000 0.1870 . . H2S H Uiso 0.00181 0.44019 0.23486 1.000 0.1870 . . H3S H Uiso 0.10812 0.45915 0.13045 1.000 0.2190 . . H4S H Uiso -0.00571 0.48647 0.10626 1.000 0.2190 . . H5S H Uiso 0.03376 0.40965 0.07558 1.000 0.2190 . . H6S H Uiso -0.09033 0.34357 0.28744 1.000 0.3110 . . H7S H Uiso -0.04490 0.29000 0.22453 1.000 0.3110 . . H8S H Uiso -0.19849 0.24024 0.26925 1.000 0.3060 . . H9S H Uiso -0.21461 0.25871 0.17904 1.000 0.3060 . . H10S H Uiso -0.25992 0.31212 0.24177 1.000 0.3060 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0325(2) 0.0407(2) 0.0322(2) 0.0015(2) 0.0021(1) 0.0007(2) Cl 0.0386(7) 0.0625(10) 0.0502(8) -0.0037(7) 0.0002(6) -0.0071(7) P1 0.0367(7) 0.0436(8) 0.0304(7) 0.0001(6) 0.0016(5) 0.0028(6) P2 0.0343(7) 0.0437(8) 0.0329(7) -0.0016(6) 0.0012(5) -0.0007(6) O 0.036(2) 0.042(2) 0.035(2) 0.0007(17) 0.0020(15) -0.0056(17) C1 0.032(3) 0.049(4) 0.055(4) -0.004(3) 0.007(3) -0.011(3) C2 0.045(3) 0.050(4) 0.047(3) 0.015(3) -0.001(3) -0.003(3) C3 0.051(4) 0.075(5) 0.057(4) 0.010(4) -0.005(3) 0.012(4) C4 0.073(5) 0.056(5) 0.076(6) 0.023(4) 0.014(4) -0.006(4) C11 0.042(3) 0.044(3) 0.037(3) 0.000(3) -0.002(2) 0.001(3) C12 0.065(4) 0.051(4) 0.040(3) -0.006(3) -0.001(3) -0.004(3) C13 0.069(5) 0.045(4) 0.064(5) -0.012(3) -0.004(4) -0.007(3) C14 0.062(4) 0.042(4) 0.063(4) 0.004(3) -0.001(3) -0.008(3) C15 0.042(3) 0.042(3) 0.047(3) 0.006(3) -0.003(3) -0.003(3) C16 0.031(3) 0.043(3) 0.041(3) -0.002(2) -0.004(2) -0.001(2) C21 0.035(3) 0.049(3) 0.031(3) 0.000(2) 0.000(2) -0.003(3) C22 0.044(3) 0.057(4) 0.037(3) 0.000(3) 0.004(3) 0.002(3) C23 0.048(4) 0.074(5) 0.038(3) 0.008(3) 0.009(3) -0.007(3) C24 0.042(3) 0.064(4) 0.041(3) 0.012(3) 0.001(3) -0.008(3) C25 0.035(3) 0.054(4) 0.037(3) 0.009(3) -0.003(2) -0.005(3) C26 0.030(3) 0.051(3) 0.030(3) 0.003(2) -0.001(2) -0.006(2) C31 0.040(3) 0.049(3) 0.030(3) -0.002(2) 0.000(2) 0.003(3) C32 0.051(4) 0.058(4) 0.067(5) 0.009(4) -0.003(3) 0.007(3) C33 0.050(4) 0.079(6) 0.092(6) 0.007(5) -0.007(4) 0.022(4) C34 0.040(4) 0.098(6) 0.069(5) -0.011(5) 0.003(3) 0.010(4) C35 0.051(4) 0.093(6) 0.054(4) -0.004(4) 0.012(3) -0.006(4) C36 0.046(4) 0.070(5) 0.045(4) 0.005(3) 0.006(3) 0.001(3) C41 0.036(3) 0.045(3) 0.039(3) 0.000(3) 0.002(2) 0.000(2) C42 0.045(3) 0.080(5) 0.035(3) 0.006(3) 0.001(3) 0.006(3) C43 0.050(4) 0.102(6) 0.047(4) 0.016(4) -0.006(3) 0.008(4) C44 0.065(5) 0.096(6) 0.036(3) 0.003(4) -0.005(3) -0.022(4) C45 0.079(5) 0.065(5) 0.039(4) -0.008(3) 0.011(3) -0.015(4) C46 0.061(4) 0.056(4) 0.040(3) -0.003(3) 0.004(3) 0.000(3) C51 0.041(3) 0.053(4) 0.037(3) -0.004(3) 0.002(2) -0.003(3) C52 0.055(4) 0.054(4) 0.087(6) -0.010(4) -0.010(4) -0.007(4) C53 0.072(6) 0.067(6) 0.110(8) -0.024(5) -0.007(5) -0.024(5) C54 0.075(6) 0.104(8) 0.068(5) -0.013(5) -0.012(4) -0.039(5) C55 0.067(5) 0.099(7) 0.064(5) 0.010(5) -0.023(4) -0.023(5) C56 0.065(5) 0.066(5) 0.056(4) 0.008(4) -0.016(3) -0.015(4) C61 0.037(3) 0.042(3) 0.043(3) -0.001(3) 0.004(2) -0.004(2) C62 0.049(4) 0.057(4) 0.046(4) -0.009(3) 0.004(3) 0.000(3) C63 0.056(4) 0.059(4) 0.060(4) -0.012(3) 0.012(3) 0.002(3) C64 0.052(4) 0.059(5) 0.074(5) -0.001(4) 0.007(4) 0.017(3) C65 0.053(4) 0.062(4) 0.059(4) 0.002(4) -0.005(3) 0.010(3) C66 0.051(4) 0.055(4) 0.039(3) -0.002(3) 0.005(3) 0.003(3) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd Cl 2.4290(16) . . yes Pd P1 2.2949(16) . . yes Pd P2 2.2916(15) . . yes Pd C1 2.107(7) . . yes P1 C11 1.833(6) . . yes P1 C31 1.822(5) . . yes P1 C41 1.831(5) . . yes P2 C21 1.841(6) . . yes P2 C51 1.830(6) . . yes P2 C61 1.831(5) . . yes O C16 1.390(6) . . yes O C26 1.412(6) . . yes O1S C3S 1.43(2) . . yes O1S C1S 1.442(18) . . yes C2 C4 1.532(11) . . no C2 C3 1.532(10) . . no C2 C15 1.528(10) . . no C2 C25 1.514(10) . . no C11 C12 1.391(9) . . no C11 C16 1.411(7) . . no C12 C13 1.387(10) . . no C13 C14 1.390(11) . . no C14 C15 1.379(9) . . no C15 C16 1.394(8) . . no C21 C26 1.394(8) . . no C21 C22 1.396(8) . . no C22 C23 1.388(10) . . no C23 C24 1.369(10) . . no C24 C25 1.395(8) . . no C25 C26 1.395(8) . . no C31 C36 1.396(9) . . no C31 C32 1.379(9) . . no C32 C33 1.394(11) . . no C33 C34 1.350(12) . . no C34 C35 1.381(12) . . no C35 C36 1.382(10) . . no C41 C46 1.394(9) . . no C41 C42 1.401(9) . . no C42 C43 1.387(10) . . no C43 C44 1.377(11) . . no C44 C45 1.367(11) . . no C45 C46 1.393(10) . . no C51 C52 1.382(10) . . no C51 C56 1.388(10) . . no C52 C53 1.407(12) . . no C53 C54 1.367(13) . . no C54 C55 1.370(15) . . no C55 C56 1.402(12) . . no C61 C62 1.392(9) . . no C61 C66 1.398(8) . . no C62 C63 1.381(10) . . no C63 C64 1.384(11) . . no C64 C65 1.369(11) . . no C65 C66 1.377(10) . . no C1 H101 0.9600 . . no C1 H102 0.9600 . . no C1 H103 0.9600 . . no C3 H301 0.9600 . . no C3 H303 0.9601 . . no C3 H302 0.9601 . . no C4 H403 0.9600 . . no C4 H402 0.9601 . . no C4 H401 0.9600 . . no C12 H12 0.9300 . . no C13 H13 0.9299 . . no C14 H14 0.9300 . . no C22 H22 0.9299 . . no C23 H23 0.9300 . . no C24 H24 0.9299 . . no C32 H32 0.9300 . . no C33 H33 0.9300 . . no C34 H34 0.9299 . . no C35 H35 0.9300 . . no C36 H36 0.9300 . . no C42 H42 0.9301 . . no C43 H43 0.9300 . . no C44 H44 0.9299 . . no C45 H45 0.9300 . . no C46 H46 0.9301 . . no C52 H52 0.9300 . . no C53 H53 0.9301 . . no C54 H54 0.9300 . . no C55 H55 0.9300 . . no C56 H56 0.9300 . . no C62 H62 0.9300 . . no C63 H63 0.9300 . . no C64 H64 0.9300 . . no C65 H65 0.9299 . . no C66 H66 0.9300 . . no C1S C2S 1.50(2) . . no C3S C4S 1.49(3) . . no C1S H1S 0.9701 . . no C1S H2S 0.9700 . . no C2S H3S 0.9600 . . no C2S H4S 0.9599 . . no C2S H5S 0.9601 . . no C3S H6S 0.9700 . . no C3S H7S 0.9700 . . no C4S H8S 0.9599 . . no C4S H9S 0.9600 . . no C4S H10S 0.9600 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl Pd P1 88.82(5) . . . yes Cl Pd P2 90.20(5) . . . yes Cl Pd C1 174.85(19) . . . yes P1 Pd P2 152.61(6) . . . yes P1 Pd C1 92.02(19) . . . yes P2 Pd C1 91.39(19) . . . yes Pd P1 C11 103.71(18) . . . yes Pd P1 C31 120.65(18) . . . yes Pd P1 C41 118.42(18) . . . yes C11 P1 C31 103.6(3) . . . yes C11 P1 C41 107.6(2) . . . yes C31 P1 C41 101.5(2) . . . yes Pd P2 C21 103.94(18) . . . yes Pd P2 C51 119.5(2) . . . yes Pd P2 C61 117.40(17) . . . yes C21 P2 C51 103.4(3) . . . yes C21 P2 C61 107.3(2) . . . yes C51 P2 C61 103.9(3) . . . yes C16 O C26 115.9(4) . . . yes C1S O1S C3S 95.8(13) . . . yes C3 C2 C4 108.5(6) . . . no C3 C2 C15 108.0(6) . . . no C4 C2 C15 111.6(6) . . . no C4 C2 C25 111.9(6) . . . no C3 C2 C25 109.6(6) . . . no C15 C2 C25 107.2(5) . . . no P1 C11 C16 122.1(4) . . . yes C12 C11 C16 116.7(5) . . . no P1 C11 C12 121.2(4) . . . yes C11 C12 C13 121.5(6) . . . no C12 C13 C14 119.8(7) . . . no C13 C14 C15 121.1(7) . . . no C2 C15 C14 124.9(6) . . . no C14 C15 C16 118.0(6) . . . no C2 C15 C16 116.9(5) . . . no O C16 C11 118.4(5) . . . yes C11 C16 C15 122.8(5) . . . no O C16 C15 118.9(5) . . . yes P2 C21 C22 120.4(4) . . . yes P2 C21 C26 123.0(4) . . . yes C22 C21 C26 116.6(5) . . . no C21 C22 C23 121.3(6) . . . no C22 C23 C24 120.1(6) . . . no C23 C24 C25 121.4(6) . . . no C2 C25 C26 117.8(5) . . . no C24 C25 C26 117.0(6) . . . no C2 C25 C24 125.2(6) . . . no O C26 C21 118.5(5) . . . yes C21 C26 C25 123.5(5) . . . no O C26 C25 117.9(5) . . . yes P1 C31 C32 123.3(5) . . . yes C32 C31 C36 118.0(6) . . . no P1 C31 C36 118.6(4) . . . yes C31 C32 C33 120.3(7) . . . no C32 C33 C34 121.5(8) . . . no C33 C34 C35 118.9(7) . . . no C34 C35 C36 120.7(7) . . . no C31 C36 C35 120.6(6) . . . no P1 C41 C46 122.9(4) . . . yes C42 C41 C46 119.2(5) . . . no P1 C41 C42 117.9(4) . . . yes C41 C42 C43 119.5(7) . . . no C42 C43 C44 120.5(7) . . . no C43 C44 C45 120.7(7) . . . no C44 C45 C46 119.8(7) . . . no C41 C46 C45 120.3(7) . . . no P2 C51 C52 120.5(5) . . . yes C52 C51 C56 119.4(7) . . . no P2 C51 C56 119.9(6) . . . yes C51 C52 C53 118.9(7) . . . no C52 C53 C54 121.6(8) . . . no C53 C54 C55 119.4(8) . . . no C54 C55 C56 120.1(8) . . . no C51 C56 C55 120.4(8) . . . no P2 C61 C66 116.3(4) . . . yes C62 C61 C66 118.7(5) . . . no P2 C61 C62 124.8(4) . . . yes C61 C62 C63 120.5(6) . . . no C62 C63 C64 120.0(7) . . . no C63 C64 C65 119.8(7) . . . no C64 C65 C66 120.9(7) . . . no C61 C66 C65 120.0(6) . . . no Pd C1 H102 109.48 . . . no Pd C1 H103 109.47 . . . no H101 C1 H102 109.47 . . . no H101 C1 H103 109.47 . . . no H102 C1 H103 109.47 . . . no Pd C1 H101 109.47 . . . no C2 C3 H301 109.47 . . . no C2 C3 H303 109.46 . . . no H301 C3 H302 109.47 . . . no H301 C3 H303 109.48 . . . no H302 C3 H303 109.47 . . . no C2 C3 H302 109.47 . . . no C2 C4 H401 109.47 . . . no C2 C4 H402 109.47 . . . no H401 C4 H402 109.46 . . . no H401 C4 H403 109.47 . . . no C2 C4 H403 109.47 . . . no H402 C4 H403 109.48 . . . no C13 C12 H12 119.23 . . . no C11 C12 H12 119.22 . . . no C12 C13 H13 120.10 . . . no C14 C13 H13 120.10 . . . no C13 C14 H14 119.45 . . . no C15 C14 H14 119.43 . . . no C23 C22 H22 119.37 . . . no C21 C22 H22 119.37 . . . no C24 C23 H23 119.96 . . . no C22 C23 H23 119.97 . . . no C23 C24 H24 119.30 . . . no C25 C24 H24 119.30 . . . no C31 C32 H32 119.85 . . . no C33 C32 H32 119.84 . . . no C34 C33 H33 119.23 . . . no C32 C33 H33 119.23 . . . no C33 C34 H34 120.55 . . . no C35 C34 H34 120.56 . . . no C36 C35 H35 119.67 . . . no C34 C35 H35 119.68 . . . no C31 C36 H36 119.70 . . . no C35 C36 H36 119.70 . . . no C43 C42 H42 120.28 . . . no C41 C42 H42 120.27 . . . no C44 C43 H43 119.74 . . . no C42 C43 H43 119.74 . . . no C43 C44 H44 119.63 . . . no C45 C44 H44 119.64 . . . no C44 C45 H45 120.10 . . . no C46 C45 H45 120.11 . . . no C45 C46 H46 119.87 . . . no C41 C46 H46 119.87 . . . no C51 C52 H52 120.55 . . . no C53 C52 H52 120.54 . . . no C54 C53 H53 119.20 . . . no C52 C53 H53 119.20 . . . no C53 C54 H54 120.29 . . . no C55 C54 H54 120.29 . . . no C56 C55 H55 119.93 . . . no C54 C55 H55 119.93 . . . no C51 C56 H56 119.79 . . . no C55 C56 H56 119.78 . . . no C63 C62 H62 119.76 . . . no C61 C62 H62 119.76 . . . no C62 C63 H63 119.98 . . . no C64 C63 H63 119.98 . . . no C65 C64 H64 120.10 . . . no C63 C64 H64 120.10 . . . no C64 C65 H65 119.53 . . . no C66 C65 H65 119.54 . . . no C61 C66 H66 120.00 . . . no C65 C66 H66 120.00 . . . no O1S C1S C2S 112.3(12) . . . yes O1S C3S C4S 109.2(17) . . . yes O1S C1S H1S 109.13 . . . no O1S C1S H2S 109.14 . . . no C2S C1S H1S 109.14 . . . no C2S C1S H2S 109.13 . . . no H1S C1S H2S 107.86 . . . no C1S C2S H3S 109.47 . . . no C1S C2S H4S 109.47 . . . no C1S C2S H5S 109.47 . . . no H3S C2S H4S 109.47 . . . no H3S C2S H5S 109.47 . . . no H4S C2S H5S 109.48 . . . no O1S C3S H6S 109.83 . . . no O1S C3S H7S 109.83 . . . no C4S C3S H6S 109.84 . . . no C4S C3S H7S 109.83 . . . no H6S C3S H7S 108.27 . . . no C3S C4S H8S 109.47 . . . no C3S C4S H9S 109.47 . . . no C3S C4S H10S 109.47 . . . no H8S C4S H9S 109.47 . . . no H8S C4S H10S 109.47 . . . no H9S C4S H10S 109.48 . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl Pd P1 C11 -57.9(2) . . . . no Cl Pd P1 C31 -173.1(2) . . . . no Cl Pd P1 C41 61.1(2) . . . . no P2 Pd P1 C11 30.2(2) . . . . no P2 Pd P1 C31 -85.0(2) . . . . no P2 Pd P1 C41 149.2(2) . . . . no C1 Pd P1 C11 127.1(3) . . . . no C1 Pd P1 C31 12.0(3) . . . . no C1 Pd P1 C41 -113.8(3) . . . . no Cl Pd P2 C21 59.81(18) . . . . no Cl Pd P2 C51 174.3(3) . . . . no Cl Pd P2 C61 -58.5(2) . . . . no P1 Pd P2 C21 -28.0(2) . . . . no P1 Pd P2 C51 86.5(3) . . . . no P1 Pd P2 C61 -146.3(2) . . . . no C1 Pd P2 C21 -125.1(3) . . . . no C1 Pd P2 C51 -10.6(3) . . . . no C1 Pd P2 C61 116.6(3) . . . . no P2 Pd C1 H102 -131.16 . . . . no P2 Pd C1 H103 108.84 . . . . no P1 Pd C1 H103 -43.98 . . . . no P1 Pd C1 H101 -163.98 . . . . no P1 Pd C1 H102 76.03 . . . . no P2 Pd C1 H101 -11.16 . . . . no C41 P1 C11 C16 -152.4(5) . . . . no Pd P1 C11 C16 -26.2(5) . . . . no C31 P1 C11 C16 100.6(5) . . . . no C31 P1 C41 C42 -139.5(5) . . . . no Pd P1 C41 C46 173.4(5) . . . . no C11 P1 C41 C46 -69.6(6) . . . . no Pd P1 C11 C12 153.9(5) . . . . no C31 P1 C11 C12 -79.3(6) . . . . no C41 P1 C11 C12 27.7(6) . . . . no C41 P1 C31 C36 56.0(5) . . . . no C11 P1 C41 C42 112.0(5) . . . . no C41 P1 C31 C32 -126.3(6) . . . . no Pd P1 C31 C32 100.4(5) . . . . no C11 P1 C31 C32 -14.9(6) . . . . no C31 P1 C41 C46 38.8(6) . . . . no Pd P1 C31 C36 -77.3(5) . . . . no Pd P1 C41 C42 -5.0(6) . . . . no C11 P1 C31 C36 167.5(5) . . . . no C51 P2 C21 C26 -101.8(5) . . . . no Pd P2 C21 C22 -157.1(4) . . . . no Pd P2 C51 C56 -77.5(5) . . . . no C61 P2 C21 C22 -32.0(5) . . . . no Pd P2 C21 C26 23.7(5) . . . . no C51 P2 C21 C22 77.4(5) . . . . no C21 P2 C61 C62 73.1(6) . . . . no Pd P2 C51 C52 97.0(6) . . . . no C61 P2 C21 C26 148.8(4) . . . . no C51 P2 C61 C66 139.7(5) . . . . no C21 P2 C51 C56 37.2(6) . . . . no C61 P2 C51 C56 149.2(5) . . . . no Pd P2 C61 C62 -170.4(5) . . . . no C61 P2 C51 C52 -36.3(6) . . . . no Pd P2 C61 C66 5.3(5) . . . . no C21 P2 C51 C52 -148.3(5) . . . . no C21 P2 C61 C66 -111.2(5) . . . . no C51 P2 C61 C62 -36.0(6) . . . . no C26 O C16 C11 145.3(5) . . . . no C26 O C16 C15 -35.3(7) . . . . no C16 O C26 C21 -143.4(5) . . . . no C16 O C26 C25 36.7(6) . . . . no C1S O1S C3S C4S -174.6(15) . . . . no C3S O1S C1S C2S 154.4(14) . . . . no C4 C2 C25 C24 18.8(9) . . . . no C3 C2 C15 C14 98.8(8) . . . . no C3 C2 C25 C24 -101.6(7) . . . . no C3 C2 C15 C16 -76.1(7) . . . . no C25 C2 C15 C14 -143.1(7) . . . . no C4 C2 C15 C16 164.7(6) . . . . no C4 C2 C25 C26 -163.2(6) . . . . no C15 C2 C25 C26 -40.6(7) . . . . no C25 C2 C15 C16 41.9(7) . . . . no C15 C2 C25 C24 141.4(6) . . . . no C4 C2 C15 C14 -20.3(9) . . . . no C3 C2 C25 C26 76.4(7) . . . . no P1 C11 C16 O 0.6(7) . . . . no P1 C11 C16 C15 -178.7(5) . . . . no P1 C11 C12 C13 -179.0(6) . . . . no C12 C11 C16 C15 1.2(9) . . . . no C16 C11 C12 C13 1.1(10) . . . . no C12 C11 C16 O -179.4(5) . . . . no C11 C12 C13 C14 -2.6(11) . . . . no C12 C13 C14 C15 1.7(11) . . . . no C13 C14 C15 C2 -174.3(7) . . . . no C13 C14 C15 C16 0.6(10) . . . . no C14 C15 C16 C11 -2.1(9) . . . . no C2 C15 C16 C11 173.2(5) . . . . no C14 C15 C16 O 178.6(6) . . . . no C2 C15 C16 O -6.1(8) . . . . no P2 C21 C26 C25 179.4(4) . . . . no C22 C21 C26 C25 0.2(8) . . . . no P2 C21 C22 C23 177.8(5) . . . . no C22 C21 C26 O -179.7(5) . . . . no P2 C21 C26 O -0.5(7) . . . . no C26 C21 C22 C23 -3.0(8) . . . . no C21 C22 C23 C24 3.7(9) . . . . no C22 C23 C24 C25 -1.4(10) . . . . no C23 C24 C25 C2 176.7(6) . . . . no C23 C24 C25 C26 -1.3(9) . . . . no C2 C25 C26 C21 -176.3(5) . . . . no C2 C25 C26 O 3.6(7) . . . . no C24 C25 C26 O -178.2(5) . . . . no C24 C25 C26 C21 1.9(8) . . . . no P1 C31 C32 C33 -179.1(6) . . . . no C36 C31 C32 C33 -1.4(11) . . . . no P1 C31 C36 C35 -180.0(5) . . . . no C32 C31 C36 C35 2.2(10) . . . . no C31 C32 C33 C34 -0.4(13) . . . . no C32 C33 C34 C35 1.3(14) . . . . no C33 C34 C35 C36 -0.5(13) . . . . no C34 C35 C36 C31 -1.3(11) . . . . no P1 C41 C42 C43 179.3(6) . . . . no P1 C41 C46 C45 179.4(6) . . . . no C42 C41 C46 C45 -2.3(10) . . . . no C46 C41 C42 C43 0.9(10) . . . . no C41 C42 C43 C44 1.2(12) . . . . no C42 C43 C44 C45 -2.0(13) . . . . no C43 C44 C45 C46 0.5(12) . . . . no C44 C45 C46 C41 1.6(11) . . . . no P2 C51 C56 C55 176.9(6) . . . . no P2 C51 C52 C53 -178.5(6) . . . . no C52 C51 C56 C55 2.3(10) . . . . no C56 C51 C52 C53 -3.9(11) . . . . no C51 C52 C53 C54 2.8(13) . . . . no C52 C53 C54 C55 0.0(14) . . . . no C53 C54 C55 C56 -1.7(13) . . . . no C54 C55 C56 C51 0.6(12) . . . . no P2 C61 C66 C65 -176.8(5) . . . . no P2 C61 C62 C63 177.0(5) . . . . no C66 C61 C62 C63 1.4(9) . . . . no C62 C61 C66 C65 -0.8(9) . . . . no C61 C62 C63 C64 -1.7(11) . . . . no C62 C63 C64 C65 1.5(11) . . . . no C63 C64 C65 C66 -1.0(11) . . . . no C64 C65 C66 C61 0.7(11) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter yes for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd O 2.658(4) . . no Pd C13 3.915(8) . 2_555 no Pd H42 3.0932 . . no Pd H66 3.0006 . . no Pd H13 2.9918 . 2_555 no Cl O 3.338(4) . . no Cl C16 3.486(5) . . no Cl C26 3.550(5) . . no Cl C42 3.482(7) . . no Cl C66 3.377(7) . . no Cl H2S 3.0497 . . no Cl H42 2.8555 . . no Cl H66 2.6926 . . no Cl H24 3.1431 . 3_566 no Cl H54 3.1461 . 4_464 no O Pd 2.658(4) . . no O Cl 3.338(4) . . no O C3 3.163(9) . . no O H303 2.6274 . . no O1S H44 2.6623 . 3_565 no C1 C36 3.497(10) . . no C3 O 3.163(9) . . no C4 C63 3.582(12) . 3_566 no C12 C32 3.599(11) . . no C12 C46 3.368(10) . . no C13 Pd 3.915(8) . 2_545 no C16 Cl 3.486(5) . . no C22 C62 3.432(10) . . no C23 C24 3.522(9) . 3_566 no C24 C23 3.522(9) . 3_566 no C26 Cl 3.550(5) . . no C32 C12 3.599(11) . . no C36 C1 3.497(10) . . no C36 C46 3.415(10) . . no C42 Cl 3.482(7) . . no C44 C64 3.509(11) . 4_564 no C46 C36 3.415(10) . . no C46 C12 3.368(10) . . no C52 C62 3.210(10) . . no C62 C22 3.432(10) . . no C62 C52 3.210(10) . . no C63 C4 3.582(12) . 3_566 no C64 C44 3.509(11) . 4_465 no C66 Cl 3.377(7) . . no C1 H7S 2.7042 . 2_555 no C3 H103 2.8583 . 3_666 no C3S H102 2.9029 . 2_545 no C4 H24 2.6004 . . no C4 H14 2.5921 . . no C11 H32 2.6415 . . no C14 H402 2.9519 . . no C14 H401 2.7333 . . no C16 H303 2.8145 . . no C21 H56 2.7493 . . no C22 H6S 2.8945 . 3_566 no C23 H6S 2.9379 . 3_566 no C24 H403 2.7423 . . no C24 H402 2.9451 . . no C26 H56 3.0086 . . no C26 H303 2.8856 . . no C31 H103 2.8274 . . no C31 H46 2.8261 . . no C33 H302 3.0196 . 3_666 no C35 H8S 2.9668 . 2_555 no C36 H103 3.0681 . . no C41 H36 2.9749 . . no C41 H12 2.8097 . . no C41 H3S 2.9636 . . no C42 H3S 2.8703 . . no C44 H64 2.7340 . 4_564 no C45 H64 3.0246 . 4_564 no C46 H12 2.6263 . . no C51 H101 2.5671 . . no C51 H62 2.9309 . . no C52 H101 2.9001 . . no C52 H62 2.9121 . . no C53 H5S 2.9949 . 2_555 no C56 H101 3.0635 . . no C61 H52 2.7836 . . no C61 H22 2.8423 . . no C62 H52 2.8264 . . no C62 H22 2.7042 . . no C62 H402 3.0391 . 3_566 no C63 H45 3.0853 . 2_555 no C64 H46 2.8662 . 2_555 no H1S H6S 2.2855 . . no H1S H7S 1.7636 . . no H2S H23 2.3896 . 3_566 no H2S H6S 2.3048 . . no H2S Cl 3.0497 . . no H3S C41 2.9636 . . no H3S C42 2.8703 . . no H5S C53 2.9949 . 2_545 no H6S H22 2.4843 . 3_566 no H6S H1S 2.2855 . . no H6S H2S 2.3048 . . no H6S C22 2.8945 . 3_566 no H6S C23 2.9379 . 3_566 no H7S C1 2.7042 . 2_545 no H7S H102 1.9360 . 2_545 no H7S H1S 1.7636 . . no H8S H35 2.4973 . 2_545 no H8S C35 2.9668 . 2_545 no H10S H65 2.4427 . 2_445 no H12 C46 2.6263 . . no H12 C41 2.8097 . . no H12 H46 2.3470 . . no H13 Pd 2.9918 . 2_545 no H14 C4 2.5921 . . no H14 H401 2.1825 . . no H14 H402 2.5847 . . no H22 C62 2.7042 . . no H22 C61 2.8423 . . no H22 H62 2.3770 . . no H22 H6S 2.4843 . 3_566 no H23 H2S 2.3896 . 3_566 no H24 H402 2.5856 . . no H24 H403 2.1957 . . no H24 Cl 3.1431 . 3_566 no H24 C4 2.6004 . . no H32 C11 2.6415 . . no H32 H55 2.5137 . 3_666 no H35 H8S 2.4973 . 2_555 no H36 C41 2.9749 . . no H36 H63 2.5019 . 4_564 no H42 Cl 2.8555 . . no H42 Pd 3.0932 . . no H44 O1S 2.6623 . 3_565 no H45 C63 3.0853 . 2_545 no H46 C64 2.8662 . 2_545 no H46 C31 2.8261 . . no H46 H12 2.3470 . . no H52 C61 2.7836 . . no H52 C62 2.8264 . . no H54 Cl 3.1461 . 4_565 no H55 H32 2.5137 . 3_666 no H56 C26 3.0086 . . no H56 C21 2.7493 . . no H62 H22 2.3770 . . no H62 C51 2.9309 . . no H62 C52 2.9121 . . no H63 H36 2.5019 . 4_465 no H64 C45 3.0246 . 4_465 no H64 C44 2.7340 . 4_465 no H65 H10S 2.4427 . 2_455 no H66 Pd 3.0006 . . no H66 Cl 2.6926 . . no H101 C51 2.5671 . . no H101 C56 3.0635 . . no H101 C52 2.9001 . . no H102 H7S 1.9360 . 2_555 no H102 C3S 2.9029 . 2_555 no H103 C31 2.8274 . . no H103 C3 2.8583 . 3_666 no H103 H301 2.5708 . 3_666 no H103 C36 3.0681 . . no H103 H302 2.5370 . 3_666 no H301 H103 2.5708 . 3_666 no H301 H401 2.4499 . . no H302 H403 2.5053 . . no H302 C33 3.0196 . 3_666 no H302 H103 2.5370 . 3_666 no H303 O 2.6274 . . no H303 C26 2.8856 . . no H303 C16 2.8145 . . no H401 H301 2.4499 . . no H401 C14 2.7333 . . no H401 H14 2.1825 . . no H402 C14 2.9519 . . no H402 H24 2.5856 . . no H402 C24 2.9451 . . no H402 H14 2.5847 . . no H402 C62 3.0391 . 3_566 no H403 H302 2.5053 . . no H403 C24 2.7423 . . no H403 H24 2.1957 . . no _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1672 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _reflns_number_observed ? _reflns_d_resolution_high .799 _reflns_d_resolution_low 12.288 _diffrn_reflns_av_sigmaI/netI 0 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_reduction_process 'perpendicular monochr Lp' _diffrn_ambient_temperature 293 _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_radiation_detector ? _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 39 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .067 _refine_ls_wR_factor_all .066 _refine_ls_goodness_of_fit_all .881 _refine_ls_shift/su_mean .005 #===END # Compound 4b data_Compound_5a _database_code_CSD 177714 # 2. EXPERIMENTAL DATA #--------------------- _publ_section_exptl_prep #<< material & crystal preparation text ; ? ; _publ_section_exptl_refinement #<< crystallographic methods used ; ? ; _chemical_formula_sum '[C39 H34 P2 Pd O S]^+^ [C F3 O3 S]^-^' _chemical_formula_moiety ? _chemical_formula_weight 850.1 _chemical_melting_point ? _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p_1_21/n_1 _symmetry_space_group_name_Hall -p_2yn loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 10.8261(6) _cell_length_b 26.801(2) _cell_length_c 13.8267(8) _cell_angle_alpha 90.00000 _cell_angle_beta 109.637(9) _cell_angle_gamma 90.00000 _cell_volume 3778.5(5) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'cu K\a' _diffrn_radiation_wavelength 1.5418 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 40.12 _cell_measurement_theta_max 41.92 _cell_measurement_temperature 293 _exptl_absorpt_coefficient_mu 5.86 _exptl_crystal_description cube _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless #<< use NfA code _diffrn_measurement_device_type CAD4 _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type PSI-scans _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 1.003 _exptl_absorpt_correction_T_max 1.243 _diffrn_reflns_number 7751 _reflns_number_total 7751 _reflns_Friedel_coverage ? _reflns_number_gt 6499 _reflns_threshold_expression 'Iobs > 2.50 sig(Iobs)' _diffrn_reflns_theta_max 74.74 _diffrn_reflns_theta_full ? _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0 #<< do not append % _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt .075 _refine_ls_wR_factor_ref .086 _refine_ls_goodness_of_fit_ref .958 _refine_ls_number_reflns 6480 _refine_ls_number_parameters 566 _refine_ls_weighting_scheme '1/[20.+0.001*\s(Fobs)^2^+0.001/\s(Fobs)]' _refine_ls_hydrogen_treatment ? _refine_ls_shift/su_max .159 _refine_diff_density_min -1.766 _refine_diff_density_max 2.738 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_coef 903(78) _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack .00000 # 3. Information for the "methods" section #----------------------------------------- _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'xtal SORTRF' _computing_structure_solution xtal _computing_structure_refinement 'xtal CRYLSQ' _computing_molecular_graphics xtal _computing_publication_material 'xtal BONDLA CIFIO' # 4. Supplementary data for validation and tables #------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0 160 .017 .009 'Int. Tables Vol IV Tables 2.2B and 2.3.1' H ? 0 136 0 0 'Int. Tables Vol IV Tables 2.2B and 2.3.1' O ? 0 16 .047 .032 'Int. Tables Vol IV Tables 2.2B and 2.3.1' N ? 0 4 .029 .018 'Int. Tables Vol IV Tables 2.2B and 2.3.1' P ? 0 8 .283 .434 'Int. Tables Vol IV Tables 2.2B and 2.3.1' S ? 0 4 .319 .557 'Int. Tables Vol IV Tables 2.2B and 2.3.1' F ? 0 12 .069 .053 'Int. Tables Vol IV Tables 2.2B and 2.3.1' Pd ? 0 4 -.059 3.934 'Int. Tables Vol IV Tables 2.2B and 2.3.1' loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Pd Pd Uani 0.18957(5) 0.17629(2) 0.25768(4) 1.000 0.0268(2) . . P1 P Uani 0.33601(18) 0.14197(8) 0.17322(15) 1.000 0.0295(5) . . P2 P Uani 0.05305(18) 0.11279(7) 0.25327(13) 1.000 0.0265(5) . . O1 O Uani 0.0948(5) 0.0804(2) 0.0702(4) 1.000 0.0320(17) . . N N Uani 0.2994(7) 0.2419(3) 0.2867(6) 1.000 0.040(2) . . C1 C Uani 0.0752(10) 0.2130(4) 0.3294(7) 1.000 0.044(3) . . C2 C Uani 0.3549(10) 0.2776(4) 0.3063(8) 1.000 0.048(3) . . C3 C Uani 0.4325(15) 0.3242(5) 0.3328(14) 1.000 0.082(6) . . C11 C Uani 0.2768(7) 0.1200(3) 0.0388(6) 1.000 0.032(3) . . C12 C Uani 0.3404(9) 0.1296(4) -0.0305(7) 1.000 0.047(3) . . C13 C Uani 0.2987(10) 0.1095(4) -0.1291(7) 1.000 0.049(3) . . C14 C Uani 0.1905(9) 0.0789(4) -0.1587(6) 1.000 0.046(3) . . C15 C Uani 0.1234(8) 0.0683(3) -0.0920(6) 1.000 0.037(3) . . C16 C Uani 0.1675(7) 0.0891(3) 0.0059(5) 1.000 0.030(2) . . C21 C Uani 0.1118(7) 0.0516(3) 0.2344(5) 1.000 0.028(2) . . C22 C Uani 0.1474(8) 0.0141(3) 0.3084(6) 1.000 0.036(3) . . C23 C Uani 0.2090(9) -0.0292(3) 0.2929(7) 1.000 0.042(3) . . C24 C Uani 0.2326(9) -0.0364(3) 0.2018(7) 1.000 0.043(3) . . C25 C Uani 0.1940(8) -0.0009(3) 0.1248(7) 1.000 0.039(3) . . C26 C Uani 0.1365(7) 0.0428(3) 0.1425(6) 1.000 0.030(2) . . C31 C Uani 0.4347(7) 0.0895(3) 0.2400(6) 1.000 0.034(2) . . C32 C Uani 0.4994(9) 0.0585(4) 0.1936(8) 1.000 0.051(3) . . C33 C Uani 0.5751(11) 0.0185(4) 0.2495(11) 1.000 0.068(4) . . C34 C Uani 0.5878(11) 0.0112(4) 0.3511(11) 1.000 0.066(4) . . C35 C Uani 0.5254(11) 0.0427(4) 0.3974(9) 1.000 0.060(4) . . C36 C Uani 0.4472(9) 0.0816(4) 0.3428(7) 1.000 0.043(3) . . C41 C Uani 0.4571(8) 0.1883(3) 0.1705(7) 1.000 0.038(3) . . C42 C Uani 0.4178(12) 0.2295(4) 0.1034(9) 1.000 0.057(4) . . C43 C Uani 0.5066(17) 0.2665(5) 0.1026(13) 1.000 0.081(6) . . C44 C Uani 0.6324(17) 0.2651(5) 0.1707(14) 1.000 0.093(7) . . C45 C Uani 0.6706(12) 0.2263(5) 0.2386(14) 1.000 0.083(6) . . C46 C Uani 0.5838(10) 0.1872(4) 0.2373(9) 1.000 0.057(4) . . C51 C Uani -0.1042(8) 0.1189(4) 0.1502(6) 1.000 0.037(3) . . C52 C Uani -0.1363(10) 0.1643(5) 0.0999(8) 1.000 0.055(4) . . C53 C Uani -0.2512(12) 0.1691(7) 0.0137(9) 1.000 0.079(5) . . C54 C Uani -0.3293(11) 0.1283(8) -0.0202(8) 1.000 0.088(7) . . C55 C Uani -0.3021(10) 0.0830(6) 0.0305(9) 1.000 0.075(5) . . C56 C Uani -0.1866(9) 0.0781(5) 0.1171(7) 1.000 0.051(4) . . C61 C Uani 0.0194(7) 0.1045(3) 0.3729(6) 1.000 0.031(2) . . C62 C Uani 0.1267(8) 0.1069(3) 0.4641(6) 1.000 0.037(3) . . C63 C Uani 0.1075(9) 0.1013(4) 0.5580(7) 1.000 0.046(3) . . C64 C Uani -0.0169(11) 0.0941(4) 0.5611(7) 1.000 0.057(4) . . C65 C Uani -0.1222(10) 0.0924(5) 0.4722(7) 1.000 0.059(4) . . C66 C Uani -0.1044(9) 0.0967(4) 0.3769(6) 1.000 0.044(3) . . S S Uiso 0.5135(3) 0.14672(12) 0.6475(2) 1.000 0.0675(8) . . F1 F Uiso 0.5756(8) 0.2352(3) 0.5926(6) 1.000 0.088(2) . . F2 F Uiso 0.5351(14) 0.1812(6) 0.4725(11) 1.000 0.189(5) . . F3 F Uiso 0.3859(19) 0.2018(8) 0.5134(17) 1.000 0.287(10) . . O2 O Uiso 0.6338(16) 0.1468(6) 0.7295(13) 1.000 0.176(6) . . O3 O Uiso 0.437(2) 0.1686(8) 0.6998(16) 1.000 0.222(8) . . O4 O Uiso 0.4603(10) 0.1039(4) 0.5916(8) 1.000 0.094(3) . . C4 C Uiso 0.5170(18) 0.1926(4) 0.5583(9) 1.000 0.130(7) . . H12 H Uiso 0.41374 0.15023 -0.01068 1.000 0.0560 . . H13 H Uiso 0.34341 0.11667 -0.17429 1.000 0.0590 . . H14 H Uiso 0.16217 0.06519 -0.22430 1.000 0.0550 . . H15 H Uiso 0.05012 0.04765 -0.11216 1.000 0.0440 . . H22 H Uiso 0.12965 0.01810 0.36925 1.000 0.0430 . . H23 H Uiso 0.23437 -0.05338 0.34405 1.000 0.0500 . . H24 H Uiso 0.27467 -0.06527 0.19213 1.000 0.0510 . . H25 H Uiso 0.20642 -0.00626 0.06225 1.000 0.0460 . . H32 H Uiso 0.49327 0.06389 0.12569 1.000 0.0620 . . H33 H Uiso 0.61668 -0.00307 0.21759 1.000 0.0810 . . H34 H Uiso 0.63849 -0.01498 0.38791 1.000 0.0790 . . H35 H Uiso 0.53526 0.03811 0.46627 1.000 0.0720 . . H36 H Uiso 0.40347 0.10224 0.37469 1.000 0.0520 . . H42 H Uiso 0.33150 0.23178 0.05938 1.000 0.0680 . . H43 H Uiso 0.48079 0.29250 0.05554 1.000 0.0970 . . H44 H Uiso 0.69135 0.29035 0.17074 1.000 0.1110 . . H45 H Uiso 0.75508 0.22583 0.28617 1.000 0.1000 . . H46 H Uiso 0.61231 0.16039 0.28197 1.000 0.0680 . . H52 H Uiso -0.08175 0.19173 0.12314 1.000 0.0660 . . H53 H Uiso -0.27347 0.19963 -0.01960 1.000 0.0950 . . H54 H Uiso -0.40281 0.13104 -0.07900 1.000 0.1050 . . H55 H Uiso -0.35886 0.05612 0.00805 1.000 0.0900 . . H56 H Uiso -0.16617 0.04778 0.15149 1.000 0.0610 . . H62 H Uiso 0.21060 0.11223 0.46189 1.000 0.0450 . . H63 H Uiso 0.17874 0.10242 0.61869 1.000 0.0550 . . H64 H Uiso -0.02949 0.09037 0.62401 1.000 0.0690 . . H65 H Uiso -0.20619 0.08836 0.47512 1.000 0.0710 . . H66 H Uiso -0.17588 0.09430 0.31657 1.000 0.0520 . . H101 H Uiso 0.12161 0.21459 0.40194 1.000 0.0670 . . H102 H Uiso -0.00558 0.19518 0.31706 1.000 0.0670 . . H103 H Uiso 0.05668 0.24621 0.30236 1.000 0.0670 . . H301 H Uiso 0.52410 0.31648 0.35113 1.000 0.1220 . . H302 H Uiso 0.41657 0.34007 0.38973 1.000 0.1220 . . H303 H Uiso 0.40713 0.34626 0.27472 1.000 0.1220 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0283(3) 0.0298(3) 0.0261(3) 0.0004(2) 0.0140(2) -0.0004(2) P1 0.0266(9) 0.0371(10) 0.0297(9) 0.0009(8) 0.0158(8) -0.0013(8) P2 0.0252(9) 0.0366(10) 0.0212(8) 0.0003(7) 0.0123(7) -0.0015(8) O1 0.032(3) 0.042(3) 0.028(3) 0.003(2) 0.018(2) 0.003(2) N 0.044(4) 0.035(4) 0.046(4) -0.001(3) 0.020(3) -0.005(3) C1 0.052(6) 0.047(5) 0.044(5) 0.000(4) 0.029(4) 0.007(4) C2 0.051(6) 0.040(5) 0.057(6) -0.004(4) 0.024(5) -0.006(4) C3 0.078(9) 0.051(7) 0.124(13) -0.020(8) 0.045(9) -0.033(7) C11 0.028(4) 0.048(5) 0.024(4) 0.005(3) 0.013(3) 0.002(3) C12 0.040(5) 0.067(7) 0.041(5) 0.000(4) 0.024(4) -0.007(4) C13 0.051(5) 0.075(7) 0.030(4) 0.006(4) 0.024(4) -0.002(5) C14 0.049(5) 0.068(6) 0.022(4) 0.006(4) 0.015(4) 0.006(5) C15 0.035(4) 0.050(5) 0.027(4) 0.000(4) 0.012(3) -0.001(4) C16 0.031(4) 0.041(4) 0.023(4) 0.004(3) 0.014(3) 0.003(3) C21 0.026(4) 0.035(4) 0.025(4) 0.000(3) 0.012(3) -0.005(3) C22 0.041(5) 0.040(5) 0.031(4) 0.002(3) 0.018(4) -0.005(4) C23 0.047(5) 0.039(5) 0.042(5) 0.009(4) 0.019(4) -0.001(4) C24 0.047(5) 0.037(5) 0.053(5) 0.001(4) 0.028(4) 0.001(4) C25 0.041(5) 0.041(5) 0.041(5) -0.003(4) 0.023(4) 0.001(4) C26 0.031(4) 0.033(4) 0.029(4) 0.000(3) 0.015(3) -0.005(3) C31 0.026(4) 0.039(4) 0.036(4) -0.002(3) 0.011(3) -0.003(3) C32 0.044(5) 0.056(6) 0.057(6) 0.001(5) 0.021(5) 0.014(4) C33 0.053(6) 0.049(6) 0.103(10) -0.004(6) 0.028(7) 0.017(5) C34 0.045(6) 0.050(6) 0.096(9) 0.023(6) 0.014(6) 0.006(5) C35 0.055(6) 0.060(7) 0.056(6) 0.023(5) 0.008(5) -0.002(5) C36 0.038(5) 0.050(5) 0.040(5) 0.006(4) 0.011(4) -0.004(4) C41 0.037(4) 0.038(5) 0.048(5) -0.002(4) 0.027(4) -0.007(3) C42 0.072(7) 0.048(6) 0.064(7) 0.005(5) 0.040(6) -0.009(5) C43 0.102(11) 0.056(8) 0.112(12) 0.009(7) 0.073(10) -0.017(7) C44 0.105(12) 0.059(8) 0.148(15) -0.017(9) 0.088(12) -0.035(8) C45 0.044(7) 0.077(9) 0.137(13) -0.027(9) 0.042(8) -0.020(6) C46 0.038(5) 0.053(6) 0.085(8) -0.007(6) 0.029(5) -0.005(4) C51 0.028(4) 0.062(6) 0.026(4) -0.001(4) 0.015(3) 0.006(4) C52 0.043(5) 0.080(8) 0.043(5) 0.020(5) 0.015(4) 0.011(5) C53 0.046(6) 0.147(14) 0.045(6) 0.031(7) 0.017(5) 0.026(8) C54 0.032(6) 0.203(18) 0.027(5) 0.003(8) 0.008(4) 0.024(9) C55 0.033(5) 0.148(13) 0.047(6) -0.046(8) 0.018(5) -0.010(7) C56 0.032(5) 0.082(8) 0.040(5) -0.021(5) 0.014(4) -0.004(5) C61 0.032(4) 0.039(4) 0.024(4) 0.000(3) 0.014(3) -0.001(3) C62 0.038(4) 0.049(5) 0.031(4) 0.001(4) 0.020(4) -0.005(4) C63 0.049(5) 0.063(6) 0.028(4) 0.003(4) 0.015(4) -0.005(5) C64 0.068(7) 0.079(8) 0.036(5) 0.002(5) 0.032(5) -0.015(6) C65 0.049(6) 0.099(9) 0.040(5) -0.001(5) 0.029(5) -0.017(6) C66 0.039(5) 0.069(6) 0.029(4) -0.002(4) 0.020(4) -0.011(4) # 5. Molecular Geometry #---------------------- loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd P1 2.443(2) . . yes Pd P2 2.241(2) . . yes Pd N 2.085(8) . . yes Pd C1 2.076(11) . . yes S O3 1.40(2) . . yes S O4 1.395(11) . . yes S O2 1.410(18) . . yes S C4 1.751(12) . . yes P1 C11 1.847(8) . . yes P1 C31 1.819(8) . . yes P1 C41 1.815(9) . . yes P2 C61 1.823(8) . . yes P2 C21 1.809(8) . . yes P2 C51 1.824(9) . . yes F1 C4 1.315(15) . . yes F2 C4 1.30(2) . . yes F3 C4 1.37(3) . . yes O1 C26 1.384(10) . . yes O1 C16 1.391(9) . . yes N C2 1.114(14) . . yes C2 C3 1.481(18) . . no C11 C12 1.379(13) . . no C11 C16 1.390(11) . . no C12 C13 1.392(13) . . no C13 C14 1.375(15) . . no C14 C15 1.382(13) . . no C15 C16 1.392(10) . . no C21 C22 1.393(11) . . no C21 C26 1.404(10) . . no C22 C23 1.390(12) . . no C23 C24 1.380(13) . . no C24 C25 1.384(12) . . no C25 C26 1.386(12) . . no C31 C32 1.376(13) . . no C31 C36 1.398(12) . . no C32 C33 1.412(16) . . no C33 C34 1.38(2) . . no C34 C35 1.367(17) . . no C35 C36 1.394(15) . . no C41 C42 1.413(14) . . no C41 C46 1.373(15) . . no C42 C43 1.38(2) . . no C43 C44 1.37(3) . . no C44 C45 1.37(2) . . no C45 C46 1.404(18) . . no C51 C52 1.387(16) . . no C51 C56 1.388(16) . . no C52 C53 1.410(17) . . no C53 C54 1.37(3) . . no C54 C55 1.38(2) . . no C55 C56 1.417(15) . . no C61 C66 1.376(13) . . no C61 C62 1.400(11) . . no C62 C63 1.390(12) . . no C63 C64 1.375(16) . . no C64 C65 1.368(14) . . no C65 C66 1.399(13) . . no C1 H101 0.9600 . . no C1 H102 0.9601 . . no C1 H103 0.9601 . . no C3 H302 0.9599 . . no C3 H303 0.9600 . . no C3 H301 0.9600 . . no C12 H12 0.9300 . . no C13 H13 0.9300 . . no C14 H14 0.9300 . . no C15 H15 0.9299 . . no C22 H22 0.9300 . . no C23 H23 0.9301 . . no C24 H24 0.9300 . . no C25 H25 0.9300 . . no C32 H32 0.9301 . . no C33 H33 0.9300 . . no C34 H34 0.9299 . . no C35 H35 0.9300 . . no C36 H36 0.9300 . . no C42 H42 0.9300 . . no C43 H43 0.9300 . . no C44 H44 0.9301 . . no C45 H45 0.9300 . . no C46 H46 0.9300 . . no C52 H52 0.9300 . . no C53 H53 0.9301 . . no C54 H54 0.9300 . . no C55 H55 0.9299 . . no C56 H56 0.9299 . . no C62 H62 0.9301 . . no C63 H63 0.9300 . . no C64 H64 0.9300 . . no C65 H65 0.9300 . . no C66 H66 0.9300 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd P2 103.24(7) . . . yes P1 Pd N 89.4(2) . . . yes P1 Pd C1 173.7(3) . . . yes P2 Pd N 166.9(2) . . . yes P2 Pd C1 83.1(3) . . . yes N Pd C1 84.3(4) . . . yes O2 S C4 109.4(9) . . . yes O2 S O3 97.5(11) . . . yes O2 S O4 123.0(8) . . . yes O4 S C4 106.9(6) . . . yes O3 S O4 115.2(10) . . . yes O3 S C4 103.1(10) . . . yes Pd P1 C11 122.7(3) . . . yes C11 P1 C31 102.1(4) . . . yes Pd P1 C31 114.4(3) . . . yes Pd P1 C41 110.0(3) . . . yes C11 P1 C41 101.9(4) . . . yes C31 P1 C41 103.5(4) . . . yes Pd P2 C51 112.8(3) . . . yes Pd P2 C21 115.6(3) . . . yes C51 P2 C61 107.5(4) . . . yes C21 P2 C61 102.0(3) . . . yes Pd P2 C61 113.5(3) . . . yes C21 P2 C51 104.5(4) . . . yes C16 O1 C26 117.8(6) . . . yes Pd N C2 176.0(8) . . . yes N C2 C3 178.2(13) . . . yes C12 C11 C16 116.9(7) . . . no P1 C11 C12 123.7(7) . . . yes P1 C11 C16 119.3(6) . . . yes C11 C12 C13 122.3(9) . . . no C12 C13 C14 119.1(9) . . . no C13 C14 C15 120.7(8) . . . no C14 C15 C16 118.8(8) . . . no C11 C16 C15 122.2(7) . . . no O1 C16 C11 119.5(6) . . . yes O1 C16 C15 118.1(7) . . . yes P2 C21 C22 124.9(6) . . . yes C22 C21 C26 117.0(7) . . . no P2 C21 C26 117.8(6) . . . yes C21 C22 C23 121.2(8) . . . no C22 C23 C24 120.2(8) . . . no C23 C24 C25 120.4(8) . . . no C24 C25 C26 118.9(8) . . . no O1 C26 C25 123.0(7) . . . yes O1 C26 C21 114.6(7) . . . yes C21 C26 C25 122.4(8) . . . no P1 C31 C36 118.2(7) . . . yes P1 C31 C32 122.3(7) . . . yes C32 C31 C36 119.5(8) . . . no C31 C32 C33 119.7(10) . . . no C32 C33 C34 120.4(11) . . . no C33 C34 C35 119.6(11) . . . no C34 C35 C36 120.9(11) . . . no C31 C36 C35 119.8(9) . . . no P1 C41 C42 119.2(8) . . . yes C42 C41 C46 118.1(9) . . . no P1 C41 C46 122.5(7) . . . yes C41 C42 C43 120.6(12) . . . no C42 C43 C44 120.5(13) . . . no C43 C44 C45 119.6(15) . . . no C44 C45 C46 120.8(15) . . . no C41 C46 C45 120.4(11) . . . no P2 C51 C56 121.0(8) . . . yes P2 C51 C52 118.8(8) . . . yes C52 C51 C56 120.1(9) . . . no C51 C52 C53 120.3(12) . . . no C52 C53 C54 119.1(15) . . . no C53 C54 C55 121.8(11) . . . no C54 C55 C56 119.1(13) . . . no C51 C56 C55 119.5(12) . . . no P2 C61 C62 117.0(6) . . . yes C62 C61 C66 119.7(7) . . . no P2 C61 C66 123.3(6) . . . yes C61 C62 C63 119.8(8) . . . no C62 C63 C64 120.0(9) . . . no C63 C64 C65 120.4(9) . . . no C64 C65 C66 120.4(10) . . . no C61 C66 C65 119.7(8) . . . no H101 C1 H103 109.46 . . . no Pd C1 H101 109.47 . . . no Pd C1 H102 109.47 . . . no Pd C1 H103 109.47 . . . no H101 C1 H102 109.48 . . . no H102 C1 H103 109.48 . . . no H302 C3 H303 109.47 . . . no C2 C3 H301 109.47 . . . no C2 C3 H302 109.47 . . . no H301 C3 H303 109.47 . . . no H301 C3 H302 109.47 . . . no C2 C3 H303 109.47 . . . no C11 C12 H12 118.84 . . . no C13 C12 H12 118.83 . . . no C12 C13 H13 120.47 . . . no C14 C13 H13 120.47 . . . no C15 C14 H14 119.65 . . . no C13 C14 H14 119.66 . . . no C14 C15 H15 120.61 . . . no C16 C15 H15 120.61 . . . no C23 C22 H22 119.42 . . . no C21 C22 H22 119.41 . . . no C24 C23 H23 119.90 . . . no C22 C23 H23 119.91 . . . no C23 C24 H24 119.82 . . . no C25 C24 H24 119.82 . . . no C26 C25 H25 120.57 . . . no C24 C25 H25 120.58 . . . no C33 C32 H32 120.14 . . . no C31 C32 H32 120.13 . . . no C32 C33 H33 119.79 . . . no C34 C33 H33 119.78 . . . no C33 C34 H34 120.21 . . . no C35 C34 H34 120.21 . . . no C36 C35 H35 119.55 . . . no C34 C35 H35 119.53 . . . no C31 C36 H36 120.08 . . . no C35 C36 H36 120.08 . . . no C41 C42 H42 119.72 . . . no C43 C42 H42 119.70 . . . no C44 C43 H43 119.76 . . . no C42 C43 H43 119.76 . . . no C43 C44 H44 120.22 . . . no C45 C44 H44 120.22 . . . no C46 C45 H45 119.60 . . . no C44 C45 H45 119.61 . . . no C41 C46 H46 119.81 . . . no C45 C46 H46 119.80 . . . no C51 C52 H52 119.83 . . . no C53 C52 H52 119.82 . . . no C54 C53 H53 120.47 . . . no C52 C53 H53 120.47 . . . no C53 C54 H54 119.09 . . . no C55 C54 H54 119.09 . . . no C54 C55 H55 120.43 . . . no C56 C55 H55 120.44 . . . no C55 C56 H56 120.25 . . . no C51 C56 H56 120.25 . . . no C61 C62 H62 120.10 . . . no C63 C62 H62 120.09 . . . no C62 C63 H63 120.02 . . . no C64 C63 H63 120.01 . . . no C65 C64 H64 119.81 . . . no C63 C64 H64 119.81 . . . no C64 C65 H65 119.78 . . . no C66 C65 H65 119.78 . . . no C65 C66 H66 120.17 . . . no C61 C66 H66 120.17 . . . no S C4 F1 118.5(9) . . . yes S C4 F2 121.5(10) . . . yes S C4 F3 100.5(14) . . . yes F1 C4 F2 109.3(14) . . . yes F1 C4 F3 108.0(13) . . . yes F2 C4 F3 94.6(14) . . . yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pd P1 C11 61.1(3) . . . . no P2 Pd P1 C31 -63.3(3) . . . . no P2 Pd P1 C41 -179.3(3) . . . . no N Pd P1 C11 -122.4(4) . . . . no N Pd P1 C31 113.2(4) . . . . no N Pd P1 C41 -2.8(4) . . . . no P1 Pd P2 C21 20.0(3) . . . . no P1 Pd P2 C51 -100.1(3) . . . . no P1 Pd P2 C61 137.3(3) . . . . no C1 Pd P2 C21 -160.8(4) . . . . no C1 Pd P2 C51 79.1(4) . . . . no C1 Pd P2 C61 -43.5(4) . . . . no P2 Pd C1 H101 103.04 . . . . no P2 Pd C1 H102 -16.96 . . . . no P2 Pd C1 H103 -136.97 . . . . no N Pd C1 H101 -73.27 . . . . no N Pd C1 H102 166.73 . . . . no N Pd C1 H103 46.72 . . . . no O2 S C4 F3 -155.2(13) . . . . no O3 S C4 F3 -52.2(14) . . . . no O4 S C4 F3 69.6(13) . . . . no O2 S C4 F1 -37.9(17) . . . . no O3 S C4 F1 65.0(17) . . . . no O4 S C4 F1 -173.2(13) . . . . no O2 S C4 F2 102.8(17) . . . . no O3 S C4 F2 -154.2(17) . . . . no O4 S C4 F2 -32.4(18) . . . . no C11 P1 C41 C42 59.1(9) . . . . no C41 P1 C31 C32 -75.5(8) . . . . no Pd P1 C31 C36 -16.9(8) . . . . no C11 P1 C31 C36 -151.6(7) . . . . no C41 P1 C31 C36 102.8(8) . . . . no C31 P1 C11 C12 -92.5(8) . . . . no C41 P1 C11 C12 14.4(9) . . . . no Pd P1 C41 C42 -72.4(8) . . . . no C31 P1 C41 C42 164.9(8) . . . . no Pd P1 C41 C46 102.0(8) . . . . no C11 P1 C41 C46 -126.4(9) . . . . no C31 P1 C41 C46 -20.6(9) . . . . no C41 P1 C11 C16 -170.3(7) . . . . no Pd P1 C31 C32 164.8(7) . . . . no C11 P1 C31 C32 30.1(8) . . . . no Pd P1 C11 C12 137.7(7) . . . . no Pd P1 C11 C16 -47.0(8) . . . . no C31 P1 C11 C16 82.8(7) . . . . no C21 P2 C51 C56 35.9(8) . . . . no Pd P2 C21 C22 110.9(7) . . . . no C51 P2 C21 C22 -124.6(7) . . . . no C51 P2 C61 C66 9.1(9) . . . . no C21 P2 C61 C62 80.2(7) . . . . no Pd P2 C51 C56 162.2(7) . . . . no Pd P2 C61 C62 -44.8(7) . . . . no C61 P2 C51 C56 -71.9(8) . . . . no C61 P2 C21 C26 174.3(6) . . . . no C21 P2 C61 C66 -100.5(8) . . . . no Pd P2 C21 C26 -62.1(7) . . . . no C21 P2 C51 C52 -139.3(8) . . . . no C51 P2 C61 C62 -170.2(7) . . . . no Pd P2 C61 C66 134.5(7) . . . . no C51 P2 C21 C26 62.4(7) . . . . no C61 P2 C51 C52 112.8(8) . . . . no C61 P2 C21 C22 -12.7(8) . . . . no Pd P2 C51 C52 -13.1(9) . . . . no C26 O1 C16 C11 -84.9(9) . . . . no C16 O1 C26 C21 147.4(7) . . . . no C16 O1 C26 C25 -34.8(11) . . . . no C26 O1 C16 C15 98.3(8) . . . . no P1 C11 C16 C15 -175.2(6) . . . . no C12 C11 C16 O1 -176.3(8) . . . . no C16 C11 C12 C13 -0.2(14) . . . . no P1 C11 C12 C13 175.2(8) . . . . no P1 C11 C16 O1 8.2(10) . . . . no C12 C11 C16 C15 0.3(12) . . . . no C11 C12 C13 C14 -0.1(16) . . . . no C12 C13 C14 C15 0.3(16) . . . . no C13 C14 C15 C16 -0.1(14) . . . . no C14 C15 C16 C11 -0.2(13) . . . . no C14 C15 C16 O1 176.4(8) . . . . no C22 C21 C26 C25 -0.2(12) . . . . no P2 C21 C22 C23 -170.7(7) . . . . no P2 C21 C26 C25 173.4(7) . . . . no C26 C21 C22 C23 2.3(12) . . . . no C22 C21 C26 O1 177.7(7) . . . . no P2 C21 C26 O1 -8.8(9) . . . . no C21 C22 C23 C24 -1.9(14) . . . . no C22 C23 C24 C25 -0.7(14) . . . . no C23 C24 C25 C26 2.7(14) . . . . no C24 C25 C26 C21 -2.3(13) . . . . no C24 C25 C26 O1 180.0(8) . . . . no C32 C31 C36 C35 0.4(14) . . . . no P1 C31 C32 C33 179.7(8) . . . . no P1 C31 C36 C35 -178.0(8) . . . . no C36 C31 C32 C33 1.4(15) . . . . no C31 C32 C33 C34 -1.9(17) . . . . no C32 C33 C34 C35 0.7(18) . . . . no C33 C34 C35 C36 1.1(18) . . . . no C34 C35 C36 C31 -1.7(17) . . . . no C42 C41 C46 C45 0.4(17) . . . . no P1 C41 C46 C45 -174.1(10) . . . . no P1 C41 C42 C43 177.3(11) . . . . no C46 C41 C42 C43 2.6(17) . . . . no C41 C42 C43 C44 -3(2) . . . . no C42 C43 C44 C45 1(3) . . . . no C43 C44 C45 C46 2(2) . . . . no C44 C45 C46 C41 -3(2) . . . . no C52 C51 C56 C55 1.2(15) . . . . no P2 C51 C52 C53 174.0(9) . . . . no C56 C51 C52 C53 -1.3(16) . . . . no P2 C51 C56 C55 -174.0(8) . . . . no C51 C52 C53 C54 -0.8(18) . . . . no C52 C53 C54 C55 3(2) . . . . no C53 C54 C55 C56 -3.1(19) . . . . no C54 C55 C56 C51 0.9(16) . . . . no C62 C61 C66 C65 1.5(15) . . . . no C66 C61 C62 C63 0.1(13) . . . . no P2 C61 C66 C65 -177.8(9) . . . . no P2 C61 C62 C63 179.5(7) . . . . no C61 C62 C63 C64 -0.9(14) . . . . no C62 C63 C64 C65 0.0(16) . . . . no C63 C64 C65 C66 1.6(18) . . . . no C64 C65 C66 C61 -2.4(18) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag #<< enter yes for value to be published ? ? ? ? ? ? ? ? ? ? ? #-------------------------------------------------------------------------- # Special items requested by author for inclusion in paper #-------------------------------------------------------------------------- loop_ _publ_manuscript_incl_extra_item _publ_manuscript_incl_extra_defn ? ? #-------------------------------------------------------------------------- # Items which are non-mandatory for Acta C submissions #-------------------------------------------------------------------------- loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pd F2 3.920(15) . . no Pd F3 3.53(2) . . no Pd O1 3.548(5) . . no Pd F1 3.235(8) . 4_454 no Pd H52 2.9304 . . no Pd H62 3.2465 . . no Pd H36 3.0660 . . no P1 C26 3.361(8) . . no F1 Pd 3.235(8) . 4_555 no F1 N 3.013(11) . 4_555 no F1 O3 3.02(2) . . no F1 O2 2.965(18) . . no F2 Pd 3.920(15) . . no F2 C36 3.178(19) . . no F2 O4 2.925(19) . . no F3 O3 2.60(3) . . no F3 O4 2.85(2) . . no F3 N 3.14(2) . . no F3 Pd 3.53(2) . . no F1 H52 2.7201 . 4_555 no F2 H36 2.6538 . . no F3 H101 2.7777 . . no O1 Pd 3.548(5) . . no O1 C56 3.322(12) . . no O1 C51 2.921(11) . . no O2 C54 3.38(2) . 1_656 no O2 F1 2.965(18) . . no O2 C3 3.16(3) . 4_555 no O2 C24 3.290(18) . 3_656 no O2 C2 3.04(2) . 4_555 no O3 F3 2.60(3) . . no O3 F1 3.02(2) . . no O4 C35 3.416(16) . . no O4 F3 2.85(2) . . no O4 C34 3.270(15) . 3_656 no O4 F2 2.925(19) . . no O2 H54 2.8376 . 1_656 no O2 H303 2.8175 . 4_555 no O2 H24 2.4918 . 3_656 no O3 H103 2.7691 . 4_555 no O3 H13 2.6796 . 1_556 no O3 H44 2.7796 . 4_455 no O4 H35 2.7777 . . no O4 H36 2.8522 . . no O4 H62 2.7047 . . no O4 H34 2.6659 . 3_656 no N C42 3.219(15) . . no N F1 3.013(11) . 4_454 no N F3 3.14(2) . . no C1 C52 3.483(15) . . no C1 C62 3.342(13) . . no C2 C41 3.446(14) . . no C2 O2 3.04(2) . 4_454 no C2 C42 3.359(16) . . no C3 O2 3.16(3) . 4_454 no C3 C15 3.494(17) . 4_555 no C12 C54 3.531(16) . 1_655 no C12 C32 3.551(14) . . no C12 C42 3.202(15) . . no C15 C25 3.387(12) . . no C15 C3 3.494(17) . 4_454 no C21 C36 3.524(13) . . no C22 C62 3.346(11) . . no C24 O2 3.290(18) . 3_656 no C25 C31 3.522(12) . . no C25 C55 3.537(16) . 3_555 no C25 C15 3.387(12) . . no C25 C32 3.501(14) . . no C26 C31 3.299(11) . . no C26 C56 3.525(13) . . no C26 P1 3.361(8) . . no C31 C26 3.299(11) . . no C31 C25 3.522(12) . . no C32 C46 3.567(15) . . no C32 C12 3.551(14) . . no C32 C25 3.501(14) . . no C34 O4 3.270(15) . 3_656 no C35 O4 3.416(16) . . no C36 F2 3.178(19) . . no C36 C21 3.524(13) . . no C41 C2 3.446(14) . . no C42 C12 3.202(15) . . no C42 C2 3.359(16) . . no C42 N 3.219(15) . . no C46 C32 3.567(15) . . no C51 O1 2.921(11) . . no C52 C1 3.483(15) . . no C54 C12 3.531(16) . 1_455 no C54 O2 3.38(2) . 1_454 no C55 C25 3.537(16) . 3_555 no C56 O1 3.322(12) . . no C56 C66 3.434(12) . . no C56 C26 3.525(13) . . no C62 C22 3.346(11) . . no C62 C1 3.342(13) . . no C66 C56 3.434(12) . . no C1 H52 2.8440 . . no C11 H42 3.0485 . . no C11 H32 2.7027 . . no C12 H32 2.8464 . . no C12 H42 3.0222 . . no C12 H54 3.0713 . 1_655 no C15 H25 2.8392 . . no C16 H25 2.6638 . . no C21 H56 2.8394 . . no C23 H64 3.0471 . 3_556 no C24 H15 2.9061 . 3_555 no C25 H15 2.8766 . 3_555 no C26 H15 3.0927 . 3_555 no C31 H46 2.6256 . . no C32 H46 3.0725 . . no C35 H65 2.9996 . 1_655 no C35 H35 3.0834 . 3_656 no C36 H46 3.0614 . . no C41 H12 2.5974 . . no C42 H12 2.6376 . . no C51 H102 2.9978 . . no C51 H66 2.7438 . . no C52 H102 2.9744 . . no C53 H302 2.8965 . 4_454 no C54 H12 2.8892 . 1_455 no C55 H32 2.9769 . 1_455 no C55 H25 2.8001 . 3_555 no C56 H66 2.7556 . . no C56 H25 3.0895 . 3_555 no C61 H22 2.6134 . . no C61 H102 2.5368 . . no C62 H101 3.0067 . . no C62 H22 2.7227 . . no C63 H14 3.0249 . 1_556 no C64 H14 3.0491 . 1_556 no C64 H43 3.0401 . 4_455 no C66 H102 3.0644 . . no H12 C42 2.6376 . . no H12 C54 2.8892 . 1_655 no H12 C41 2.5974 . . no H12 H54 2.5223 . 1_655 no H13 O3 2.6796 . 1_554 no H14 H63 2.4500 . 1_554 no H14 H64 2.4969 . 1_554 no H14 C64 3.0491 . 1_554 no H14 C63 3.0249 . 1_554 no H15 C24 2.9061 . 3_555 no H15 C25 2.8766 . 3_555 no H15 C26 3.0927 . 3_555 no H22 C61 2.6134 . . no H22 C62 2.7227 . . no H23 H64 2.5992 . 3_556 no H24 O2 2.4918 . 3_656 no H25 C15 2.8392 . . no H25 C16 2.6638 . . no H25 C55 2.8001 . 3_555 no H25 H55 2.5558 . 3_555 no H25 C56 3.0895 . 3_555 no H32 C55 2.9769 . 1_655 no H32 C12 2.8464 . . no H32 C11 2.7027 . . no H34 O4 2.6659 . 3_656 no H35 O4 2.7777 . . no H35 C35 3.0834 . 3_656 no H35 H35 2.4707 . 3_656 no H36 O4 2.8522 . . no H36 Pd 3.0660 . . no H36 F2 2.6538 . . no H42 C11 3.0485 . . no H42 C12 3.0222 . . no H43 C64 3.0401 . 4_554 no H44 O3 2.7796 . 4_554 no H46 C32 3.0725 . . no H46 C36 3.0614 . . no H46 C31 2.6256 . . no H52 H102 2.5282 . . no H52 C1 2.8440 . . no H52 F1 2.7201 . 4_454 no H52 Pd 2.9304 . . no H54 O2 2.8376 . 1_454 no H54 C12 3.0713 . 1_455 no H54 H12 2.5223 . 1_455 no H55 H25 2.5558 . 3_555 no H56 C21 2.8394 . . no H62 O4 2.7047 . . no H62 Pd 3.2465 . . no H63 H14 2.4500 . 1_556 no H64 H14 2.4969 . 1_556 no H64 C23 3.0471 . 3_556 no H64 H23 2.5992 . 3_556 no H65 C35 2.9996 . 1_455 no H66 C56 2.7556 . . no H66 C51 2.7438 . . no H101 C62 3.0067 . . no H101 F3 2.7777 . . no H102 C51 2.9978 . . no H102 C52 2.9744 . . no H102 C61 2.5368 . . no H102 C66 3.0644 . . no H102 H52 2.5282 . . no H103 O3 2.7691 . 4_454 no H302 C53 2.8965 . 4_555 no H303 O2 2.8175 . 4_454 no _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens ? _geom_special_details ? _cell_special_details ; ? ; _exptl_special_details ; ? ; _diffrn_special_details ; ? ; _chemical_compound_source ? _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_analytical ? _chemical_formula_structural ? _exptl_crystal_F_000 1728 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? loop_ _diffrn_attenuator_code _diffrn_attenuator_scale ? ? _reflns_limit_h_min -13 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 33 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _reflns_number_observed ? _reflns_d_resolution_high .799 _reflns_d_resolution_low 13.365 _diffrn_reflns_av_sigmaI/netI 0 _diffrn_reflns_theta_min 3.3 _diffrn_reflns_reduction_process 'perpendicular monochr Lp' _diffrn_ambient_temperature 293 _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_radiation_detector ? _refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970' _refine_ls_matrix_type full _refine_ls_number_restraints 38 _refine_ls_number_constraints 0 _refine_ls_R_factor_all .085 _refine_ls_wR_factor_all .089 _refine_ls_goodness_of_fit_all .91 _refine_ls_shift/su_mean .009 #===END # Compound 5f data_s2201a _database_code_CSD 177715 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H47 Fe P2 Pd, C F3 O3 S' _chemical_formula_sum 'C28 H47 F3 Fe O3 P2 Pd S' _chemical_formula_weight 744.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' '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' 'Pd' 'Pd' -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.75150(10) _cell_length_b 16.9323(2) _cell_length_c 16.8170(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.8589(6) _cell_angle_gamma 90.00 _cell_volume 3218.88(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 1.218 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.82 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53974 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7369 _reflns_number_gt 6383 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'DENZO 1.11.0' _computing_data_reduction 'DENZO 1.11.0' _computing_structure_solution 'DIRDIF-97 (Beurskens et al., 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+2.0912P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7369 _refine_ls_number_parameters 540 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0249 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.402656(12) 0.620185(8) 0.292823(8) 0.01689(5) Uani 1 1 d . . . Fe1 Fe 0.23014(2) 0.529795(15) 0.152373(15) 0.01751(6) Uani 1 1 d . . . P1 P 0.51818(4) 0.59985(3) 0.20519(3) 0.01678(10) Uani 1 1 d . . . P2 P 0.23408(4) 0.62440(3) 0.33687(3) 0.01649(10) Uani 1 1 d . . . C1 C 0.5182(2) 0.67827(19) 0.38697(17) 0.0384(6) Uani 1 1 d . . . H1A H 0.585(3) 0.6911(19) 0.3762(19) 0.070(10) Uiso 1 1 d . . . H1B H 0.488(3) 0.726(2) 0.389(2) 0.078(12) Uiso 1 1 d . . . H1C H 0.522(3) 0.652(2) 0.430(3) 0.096(14) Uiso 1 1 d . . . C2 C 0.17771(16) 0.54781(11) 0.26099(11) 0.0193(4) Uani 1 1 d . . . C3 C 0.07715(17) 0.54335(13) 0.19004(12) 0.0232(4) Uani 1 1 d . . . H3 H 0.0220(19) 0.5841(13) 0.1716(13) 0.023(5) Uiso 1 1 d . . . C4 C 0.07911(19) 0.46850(13) 0.15251(13) 0.0283(5) Uani 1 1 d . . . H4 H 0.0264(19) 0.4514(13) 0.1062(14) 0.026(6) Uiso 1 1 d . . . C5 C 0.17940(19) 0.42599(12) 0.19759(13) 0.0269(4) Uani 1 1 d . . . H5 H 0.203(2) 0.3781(15) 0.1861(14) 0.033(7) Uiso 1 1 d . . . C6 C 0.24175(18) 0.47419(11) 0.26355(12) 0.0223(4) Uani 1 1 d . . . H6 H 0.314(2) 0.4614(13) 0.3044(14) 0.030(6) Uiso 1 1 d . . . C7 C 0.38570(16) 0.57053(11) 0.12654(11) 0.0190(4) Uani 1 1 d . . . C8 C 0.28840(17) 0.62520(12) 0.09836(11) 0.0200(4) Uani 1 1 d . . . H8 H 0.2852(18) 0.6762(13) 0.1144(13) 0.019(5) Uiso 1 1 d . . . C9 C 0.19534(19) 0.58707(13) 0.03983(12) 0.0250(4) Uani 1 1 d . . . H9 H 0.124(2) 0.6104(13) 0.0156(14) 0.026(6) Uiso 1 1 d . . . C10 C 0.23087(19) 0.50831(13) 0.03198(12) 0.0259(4) Uani 1 1 d . . . H10 H 0.1876(19) 0.4674(13) -0.0003(13) 0.025(6) Uiso 1 1 d . . . C11 C 0.34635(18) 0.49732(12) 0.08478(12) 0.0228(4) Uani 1 1 d . . . H11 H 0.3875(18) 0.4512(13) 0.0916(12) 0.019(5) Uiso 1 1 d . . . C12 C 0.22080(18) 0.58131(13) 0.43761(12) 0.0255(4) Uani 1 1 d . . . C13 C 0.3245(2) 0.52388(16) 0.46835(14) 0.0341(5) Uani 1 1 d . . . H13A H 0.320(2) 0.5004(15) 0.5199(15) 0.037(6) Uiso 1 1 d . . . H13B H 0.396(2) 0.5497(15) 0.4741(15) 0.037(7) Uiso 1 1 d . . . H13C H 0.318(2) 0.4802(15) 0.4305(15) 0.034(6) Uiso 1 1 d . . . C14 C 0.2311(3) 0.64562(17) 0.50341(15) 0.0410(6) Uani 1 1 d . . . H14A H 0.300(2) 0.6745(15) 0.5085(15) 0.039(7) Uiso 1 1 d . . . H14B H 0.234(3) 0.6198(17) 0.552(2) 0.057(9) Uiso 1 1 d . . . H14C H 0.164(2) 0.6778(16) 0.4918(16) 0.044(8) Uiso 1 1 d . . . C15 C 0.1041(2) 0.53621(17) 0.42545(17) 0.0389(6) Uani 1 1 d . . . H15A H 0.102(2) 0.5123(15) 0.4779(16) 0.041(7) Uiso 1 1 d . . . H15B H 0.096(2) 0.4914(16) 0.3881(16) 0.043(7) Uiso 1 1 d . . . H15C H 0.037(2) 0.5701(17) 0.4070(16) 0.048(8) Uiso 1 1 d . . . C16 C 0.14377(17) 0.71617(12) 0.30645(12) 0.0232(4) Uani 1 1 d . . . C17 C 0.1981(2) 0.78344(13) 0.36623(15) 0.0315(5) Uani 1 1 d . . . H17A H 0.280(2) 0.7877(14) 0.3723(15) 0.036(6) Uiso 1 1 d . . . H17B H 0.160(2) 0.8304(15) 0.3420(14) 0.032(6) Uiso 1 1 d . . . H17C H 0.186(2) 0.7783(16) 0.4201(17) 0.048(7) Uiso 1 1 d . . . C18 C 0.01287(19) 0.70684(15) 0.30348(16) 0.0321(5) Uani 1 1 d . . . H18A H -0.023(2) 0.6648(16) 0.2678(16) 0.040(7) Uiso 1 1 d . . . H18B H -0.025(2) 0.7548(16) 0.2810(16) 0.043(7) Uiso 1 1 d . . . H18C H 0.001(2) 0.6964(15) 0.3563(17) 0.045(7) Uiso 1 1 d . . . C19 C 0.1552(2) 0.74111(13) 0.22104(14) 0.0287(5) Uani 1 1 d . . . H19A H 0.115(2) 0.7928(15) 0.2041(14) 0.036(6) Uiso 1 1 d . . . H19B H 0.240(2) 0.7492(14) 0.2210(14) 0.035(6) Uiso 1 1 d . . . H19C H 0.122(2) 0.7049(14) 0.1780(15) 0.032(6) Uiso 1 1 d . . . C20 C 0.62247(18) 0.51379(12) 0.22606(13) 0.0256(4) Uani 1 1 d . . . C21 C 0.7306(2) 0.53320(16) 0.29864(16) 0.0359(5) Uani 1 1 d . . . H21A H 0.782(2) 0.5693(16) 0.2815(16) 0.044(7) Uiso 1 1 d . . . H21B H 0.709(2) 0.5553(15) 0.3430(16) 0.042(7) Uiso 1 1 d . . . H21C H 0.774(3) 0.4858(19) 0.3140(18) 0.060(9) Uiso 1 1 d . . . C22 C 0.5584(2) 0.44552(14) 0.25578(16) 0.0333(5) Uani 1 1 d . . . H22A H 0.540(2) 0.4603(14) 0.3066(16) 0.037(7) Uiso 1 1 d . . . H22B H 0.489(2) 0.4262(16) 0.2165(17) 0.045(7) Uiso 1 1 d . . . H22C H 0.613(2) 0.4014(15) 0.2704(15) 0.038(7) Uiso 1 1 d . . . C23 C 0.6621(2) 0.48907(16) 0.15021(17) 0.0392(6) Uani 1 1 d . . . H23A H 0.593(2) 0.4783(14) 0.1008(16) 0.036(7) Uiso 1 1 d . . . H23B H 0.710(2) 0.5269(14) 0.1378(15) 0.033(7) Uiso 1 1 d . . . H23C H 0.706(2) 0.4419(17) 0.1602(17) 0.052(8) Uiso 1 1 d . . . C24 C 0.57868(16) 0.68644(12) 0.15890(12) 0.0224(4) Uani 1 1 d . . . C25 C 0.5110(2) 0.76068(13) 0.17285(17) 0.0346(5) Uani 1 1 d . . . H25A H 0.542(2) 0.8064(15) 0.1501(15) 0.040(7) Uiso 1 1 d . . . H25B H 0.427(2) 0.7580(15) 0.1449(15) 0.044(7) Uiso 1 1 d . . . H25C H 0.521(2) 0.7689(16) 0.2316(18) 0.048(8) Uiso 1 1 d . . . C26 C 0.70923(19) 0.70069(15) 0.20413(14) 0.0295(5) Uani 1 1 d . . . H26A H 0.7220(19) 0.7050(13) 0.2636(14) 0.026(6) Uiso 1 1 d . . . H26B H 0.731(2) 0.7490(15) 0.1858(14) 0.034(6) Uiso 1 1 d . . . H26C H 0.760(2) 0.6607(15) 0.1911(15) 0.040(7) Uiso 1 1 d . . . C27 C 0.5634(2) 0.67502(16) 0.06644(14) 0.0317(5) Uani 1 1 d . . . H27A H 0.602(2) 0.6310(15) 0.0557(15) 0.035(7) Uiso 1 1 d . . . H27B H 0.594(2) 0.7203(15) 0.0450(15) 0.037(7) Uiso 1 1 d . . . H27C H 0.484(2) 0.6671(14) 0.0359(15) 0.036(7) Uiso 1 1 d . . . S1 S 0.13381(5) 0.20713(3) 0.50210(3) 0.02697(11) Uani 1 1 d . . . F1 F 0.15196(13) 0.35682(8) 0.54249(9) 0.0478(4) Uani 1 1 d . . . F2 F 0.22747(13) 0.32792(8) 0.44446(9) 0.0436(3) Uani 1 1 d . . . F3 F 0.03843(14) 0.33404(9) 0.42232(11) 0.0668(5) Uani 1 1 d . . . O1 O 0.24510(15) 0.19614(10) 0.56359(10) 0.0434(4) Uani 1 1 d . . . O2 O 0.03149(16) 0.20166(11) 0.53237(12) 0.0527(5) Uani 1 1 d . . . O3 O 0.12440(13) 0.16689(8) 0.42521(9) 0.0313(3) Uani 1 1 d . . . C28 C 0.13786(18) 0.31135(12) 0.47552(13) 0.0294(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01488(7) 0.02134(8) 0.01497(7) -0.00316(5) 0.00495(5) -0.00251(5) Fe1 0.01984(14) 0.01754(13) 0.01479(13) -0.00176(10) 0.00411(10) -0.00311(10) P1 0.0165(2) 0.0187(2) 0.0165(2) 0.00056(18) 0.00669(18) 0.00082(18) P2 0.0155(2) 0.0194(2) 0.0155(2) -0.00290(18) 0.00584(18) -0.00253(18) C1 0.0286(13) 0.0536(17) 0.0309(13) -0.0172(12) 0.0045(10) -0.0138(12) C2 0.0208(9) 0.0214(9) 0.0169(9) -0.0012(7) 0.0076(7) -0.0047(7) C3 0.0191(9) 0.0280(11) 0.0229(10) -0.0036(8) 0.0066(8) -0.0041(8) C4 0.0280(11) 0.0338(12) 0.0237(10) -0.0082(9) 0.0080(9) -0.0143(9) C5 0.0406(12) 0.0173(10) 0.0271(11) -0.0030(8) 0.0164(9) -0.0087(9) C6 0.0289(10) 0.0206(9) 0.0189(9) 0.0011(8) 0.0089(8) -0.0015(8) C7 0.0213(9) 0.0219(9) 0.0155(9) 0.0003(7) 0.0077(7) -0.0017(8) C8 0.0226(10) 0.0190(10) 0.0176(9) 0.0022(7) 0.0042(7) -0.0012(8) C9 0.0245(10) 0.0317(11) 0.0168(9) 0.0055(8) 0.0022(8) -0.0031(9) C10 0.0334(11) 0.0300(11) 0.0145(9) -0.0040(8) 0.0069(8) -0.0095(9) C11 0.0295(10) 0.0221(10) 0.0194(9) -0.0033(8) 0.0110(8) -0.0009(9) C12 0.0306(11) 0.0308(11) 0.0188(9) 0.0003(8) 0.0128(8) -0.0035(9) C13 0.0400(14) 0.0411(14) 0.0230(11) 0.0092(10) 0.0119(10) 0.0049(11) C14 0.0595(18) 0.0447(15) 0.0218(12) -0.0049(11) 0.0162(12) -0.0016(14) C15 0.0400(14) 0.0441(15) 0.0398(14) 0.0051(12) 0.0229(11) -0.0086(12) C16 0.0229(10) 0.0218(10) 0.0254(10) -0.0050(8) 0.0074(8) -0.0002(8) C17 0.0351(13) 0.0225(11) 0.0385(13) -0.0083(10) 0.0126(10) -0.0030(10) C18 0.0228(11) 0.0326(12) 0.0423(13) -0.0073(11) 0.0111(10) 0.0014(10) C19 0.0333(12) 0.0235(11) 0.0287(11) 0.0040(9) 0.0076(9) 0.0046(10) C20 0.0261(10) 0.0238(10) 0.0275(10) 0.0040(8) 0.0085(8) 0.0074(8) C21 0.0269(12) 0.0401(14) 0.0377(13) 0.0128(11) 0.0036(10) 0.0057(11) C22 0.0359(13) 0.0249(11) 0.0370(13) 0.0106(10) 0.0063(11) 0.0057(10) C23 0.0433(14) 0.0356(14) 0.0451(15) -0.0003(12) 0.0228(13) 0.0148(12) C24 0.0201(9) 0.0236(10) 0.0241(10) 0.0057(8) 0.0069(8) -0.0031(8) C25 0.0311(12) 0.0196(11) 0.0524(15) 0.0047(10) 0.0101(11) -0.0022(9) C26 0.0227(10) 0.0359(13) 0.0294(12) 0.0037(10) 0.0065(9) -0.0071(10) C27 0.0322(12) 0.0390(14) 0.0249(11) 0.0072(10) 0.0096(10) -0.0075(11) S1 0.0307(3) 0.0264(3) 0.0273(3) -0.0040(2) 0.0136(2) -0.0102(2) F1 0.0579(9) 0.0344(7) 0.0563(9) -0.0240(7) 0.0243(7) -0.0113(7) F2 0.0601(9) 0.0276(7) 0.0540(9) 0.0029(6) 0.0340(7) -0.0078(6) F3 0.0511(9) 0.0354(8) 0.0864(13) -0.0026(8) -0.0278(9) 0.0058(7) O1 0.0492(10) 0.0389(9) 0.0343(9) 0.0101(7) -0.0019(8) -0.0134(8) O2 0.0521(11) 0.0517(11) 0.0703(13) -0.0230(9) 0.0439(10) -0.0251(9) O3 0.0403(9) 0.0247(8) 0.0314(8) -0.0068(6) 0.0139(7) -0.0050(7) C28 0.0265(11) 0.0267(11) 0.0329(11) -0.0070(9) 0.0043(9) -0.0015(9) _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 C1 2.036(2) . ? Pd1 P1 2.2863(5) . ? Pd1 P2 2.2978(5) . ? Pd1 Fe1 3.0683(3) . ? Fe1 C4 2.057(2) . ? Fe1 C10 2.0594(19) . ? Fe1 C8 2.0599(19) . ? Fe1 C6 2.0642(19) . ? Fe1 C9 2.0657(19) . ? Fe1 C5 2.067(2) . ? Fe1 C11 2.0755(19) . ? Fe1 C3 2.0757(19) . ? Fe1 C2 2.1035(18) . ? Fe1 C7 2.1072(18) . ? P1 C7 1.8150(19) . ? P1 C20 1.874(2) . ? P1 C24 1.8879(19) . ? P2 C2 1.8130(19) . ? P2 C16 1.872(2) . ? P2 C12 1.8899(19) . ? C1 H1A 0.88(3) . ? C1 H1B 0.89(4) . ? C1 H1C 0.83(4) . ? C2 C3 1.434(3) . ? C2 C6 1.451(3) . ? C3 C4 1.419(3) . ? C3 H3 0.94(2) . ? C4 C5 1.412(3) . ? C4 H4 0.90(2) . ? C5 C6 1.410(3) . ? C5 H5 0.89(2) . ? C6 H6 0.96(2) . ? C7 C11 1.437(3) . ? C7 C8 1.447(3) . ? C8 C9 1.412(3) . ? C8 H8 0.91(2) . ? C9 C10 1.414(3) . ? C9 H9 0.92(2) . ? C10 C11 1.416(3) . ? C10 H10 0.94(2) . ? C11 H11 0.91(2) . ? C12 C14 1.533(3) . ? C12 C15 1.534(3) . ? C12 C13 1.534(3) . ? C13 H13A 0.97(3) . ? C13 H13B 0.93(3) . ? C13 H13C 0.97(3) . ? C14 H14A 0.93(3) . ? C14 H14B 0.92(3) . ? C14 H14C 0.93(3) . ? C15 H15A 0.98(3) . ? C15 H15B 0.97(3) . ? C15 H15C 0.95(3) . ? C16 C18 1.534(3) . ? C16 C19 1.538(3) . ? C16 C17 1.538(3) . ? C17 H17A 0.94(3) . ? C17 H17B 0.95(2) . ? C17 H17C 0.96(3) . ? C18 H18A 0.95(3) . ? C18 H18B 0.95(3) . ? C18 H18C 0.95(3) . ? C19 H19A 1.00(3) . ? C19 H19B 1.01(2) . ? C19 H19C 0.95(2) . ? C20 C23 1.531(3) . ? C20 C22 1.535(3) . ? C20 C21 1.538(3) . ? C21 H21A 0.96(3) . ? C21 H21B 0.93(3) . ? C21 H21C 0.95(3) . ? C22 H22A 0.97(3) . ? C22 H22B 0.96(3) . ? C22 H22C 0.97(3) . ? C23 H23A 1.01(3) . ? C23 H23B 0.92(2) . ? C23 H23C 0.94(3) . ? C24 C27 1.528(3) . ? C24 C26 1.534(3) . ? C24 C25 1.539(3) . ? C25 H25A 0.97(3) . ? C25 H25B 0.97(3) . ? C25 H25C 0.97(3) . ? C26 H26A 0.97(2) . ? C26 H26B 0.93(3) . ? C26 H26C 0.97(3) . ? C27 H27A 0.92(3) . ? C27 H27B 0.96(3) . ? C27 H27C 0.95(3) . ? S1 O2 1.4311(16) . ? S1 O3 1.4388(15) . ? S1 O1 1.4405(17) . ? S1 C28 1.824(2) . ? F1 C28 1.337(2) . ? F2 C28 1.327(2) . ? F3 C28 1.320(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd1 P1 100.76(8) . . ? C1 Pd1 P2 100.66(8) . . ? P1 Pd1 P2 158.213(18) . . ? C1 Pd1 Fe1 178.97(10) . . ? P1 Pd1 Fe1 79.191(13) . . ? P2 Pd1 Fe1 79.467(13) . . ? C4 Fe1 C10 98.47(8) . . ? C4 Fe1 C8 141.92(8) . . ? C10 Fe1 C8 67.29(8) . . ? C4 Fe1 C6 67.19(8) . . ? C10 Fe1 C6 142.45(8) . . ? C8 Fe1 C6 144.03(8) . . ? C4 Fe1 C9 106.45(9) . . ? C10 Fe1 C9 40.10(8) . . ? C8 Fe1 C9 40.03(8) . . ? C6 Fe1 C9 172.54(8) . . ? C4 Fe1 C5 40.05(9) . . ? C10 Fe1 C5 106.89(8) . . ? C8 Fe1 C5 173.37(8) . . ? C6 Fe1 C5 39.93(8) . . ? C9 Fe1 C5 137.02(8) . . ? C4 Fe1 C11 124.34(8) . . ? C10 Fe1 C11 40.06(8) . . ? C8 Fe1 C11 67.58(8) . . ? C6 Fe1 C11 118.99(8) . . ? C9 Fe1 C11 67.52(8) . . ? C5 Fe1 C11 105.98(8) . . ? C4 Fe1 C3 40.16(8) . . ? C10 Fe1 C3 123.79(8) . . ? C8 Fe1 C3 117.89(8) . . ? C6 Fe1 C3 67.82(8) . . ? C9 Fe1 C3 104.87(8) . . ? C5 Fe1 C3 67.71(9) . . ? C11 Fe1 C3 161.95(8) . . ? C4 Fe1 C2 67.33(8) . . ? C10 Fe1 C2 163.80(8) . . ? C8 Fe1 C2 118.73(8) . . ? C6 Fe1 C2 40.73(7) . . ? C9 Fe1 C2 134.10(8) . . ? C5 Fe1 C2 67.75(8) . . ? C11 Fe1 C2 155.06(8) . . ? C3 Fe1 C2 40.12(7) . . ? C4 Fe1 C7 164.36(8) . . ? C10 Fe1 C7 67.56(8) . . ? C8 Fe1 C7 40.61(7) . . ? C6 Fe1 C7 119.32(8) . . ? C9 Fe1 C7 67.86(8) . . ? C5 Fe1 C7 135.07(8) . . ? C11 Fe1 C7 40.19(7) . . ? C3 Fe1 C7 154.06(8) . . ? C2 Fe1 C7 127.45(7) . . ? C4 Fe1 Pd1 129.77(6) . . ? C10 Fe1 Pd1 131.73(6) . . ? C8 Fe1 Pd1 73.68(5) . . ? C6 Fe1 Pd1 70.37(6) . . ? C9 Fe1 Pd1 113.26(6) . . ? C5 Fe1 Pd1 109.72(6) . . ? C11 Fe1 Pd1 99.12(6) . . ? C3 Fe1 Pd1 98.92(5) . . ? C2 Fe1 Pd1 63.12(5) . . ? C7 Fe1 Pd1 64.37(5) . . ? C7 P1 C20 108.09(9) . . ? C7 P1 C24 104.87(8) . . ? C20 P1 C24 112.36(9) . . ? C7 P1 Pd1 88.21(6) . . ? C20 P1 Pd1 118.00(6) . . ? C24 P1 Pd1 120.38(6) . . ? C2 P2 C16 109.30(9) . . ? C2 P2 C12 104.53(9) . . ? C16 P2 C12 112.70(9) . . ? C2 P2 Pd1 86.12(6) . . ? C16 P2 Pd1 114.33(6) . . ? C12 P2 Pd1 124.52(7) . . ? Pd1 C1 H1A 114(2) . . ? Pd1 C1 H1B 106(2) . . ? H1A C1 H1B 100(3) . . ? Pd1 C1 H1C 107(3) . . ? H1A C1 H1C 117(3) . . ? H1B C1 H1C 112(3) . . ? C3 C2 C6 106.40(17) . . ? C3 C2 P2 133.08(15) . . ? C6 C2 P2 120.46(14) . . ? C3 C2 Fe1 68.90(10) . . ? C6 C2 Fe1 68.18(10) . . ? P2 C2 Fe1 125.28(9) . . ? C4 C3 C2 107.91(19) . . ? C4 C3 Fe1 69.19(11) . . ? C2 C3 Fe1 70.98(11) . . ? C4 C3 H3 127.0(13) . . ? C2 C3 H3 125.0(13) . . ? Fe1 C3 H3 123.9(13) . . ? C5 C4 C3 109.22(18) . . ? C5 C4 Fe1 70.36(12) . . ? C3 C4 Fe1 70.65(11) . . ? C5 C4 H4 125.2(14) . . ? C3 C4 H4 125.5(14) . . ? Fe1 C4 H4 123.5(14) . . ? C6 C5 C4 107.78(19) . . ? C6 C5 Fe1 69.94(11) . . ? C4 C5 Fe1 69.59(12) . . ? C6 C5 H5 124.6(15) . . ? C4 C5 H5 127.5(15) . . ? Fe1 C5 H5 123.6(15) . . ? C5 C6 C2 108.67(18) . . ? C5 C6 Fe1 70.13(11) . . ? C2 C6 Fe1 71.09(11) . . ? C5 C6 H6 126.9(14) . . ? C2 C6 H6 124.5(14) . . ? Fe1 C6 H6 125.1(13) . . ? C11 C7 C8 105.77(16) . . ? C11 C7 P1 133.58(15) . . ? C8 C7 P1 120.49(14) . . ? C11 C7 Fe1 68.72(11) . . ? C8 C7 Fe1 67.94(10) . . ? P1 C7 Fe1 123.98(9) . . ? C9 C8 C7 109.15(18) . . ? C9 C8 Fe1 70.21(11) . . ? C7 C8 Fe1 71.45(11) . . ? C9 C8 H8 123.7(13) . . ? C7 C8 H8 127.1(13) . . ? Fe1 C8 H8 124.6(13) . . ? C8 C9 C10 107.71(18) . . ? C8 C9 Fe1 69.77(11) . . ? C10 C9 Fe1 69.71(11) . . ? C8 C9 H9 123.7(14) . . ? C10 C9 H9 128.5(14) . . ? Fe1 C9 H9 122.4(14) . . ? C9 C10 C11 108.78(18) . . ? C9 C10 Fe1 70.19(11) . . ? C11 C10 Fe1 70.58(11) . . ? C9 C10 H10 128.5(13) . . ? C11 C10 H10 122.7(13) . . ? Fe1 C10 H10 123.5(13) . . ? C10 C11 C7 108.56(18) . . ? C10 C11 Fe1 69.36(11) . . ? C7 C11 Fe1 71.09(11) . . ? C10 C11 H11 125.3(13) . . ? C7 C11 H11 126.1(13) . . ? Fe1 C11 H11 124.4(13) . . ? C14 C12 C15 109.9(2) . . ? C14 C12 C13 107.9(2) . . ? C15 C12 C13 109.2(2) . . ? C14 C12 P2 111.29(16) . . ? C15 C12 P2 111.26(15) . . ? C13 C12 P2 107.10(14) . . ? C12 C13 H13A 109.3(14) . . ? C12 C13 H13B 110.5(15) . . ? H13A C13 H13B 112(2) . . ? C12 C13 H13C 110.5(14) . . ? H13A C13 H13C 105(2) . . ? H13B C13 H13C 110(2) . . ? C12 C14 H14A 109.7(16) . . ? C12 C14 H14B 106.2(18) . . ? H14A C14 H14B 110(2) . . ? C12 C14 H14C 111.6(16) . . ? H14A C14 H14C 112(2) . . ? H14B C14 H14C 107(2) . . ? C12 C15 H15A 109.1(15) . . ? C12 C15 H15B 113.3(15) . . ? H15A C15 H15B 104(2) . . ? C12 C15 H15C 111.8(16) . . ? H15A C15 H15C 109(2) . . ? H15B C15 H15C 110(2) . . ? C18 C16 C19 109.93(18) . . ? C18 C16 C17 109.35(17) . . ? C19 C16 C17 106.28(18) . . ? C18 C16 P2 114.34(15) . . ? C19 C16 P2 107.18(13) . . ? C17 C16 P2 109.44(15) . . ? C16 C17 H17A 110.9(15) . . ? C16 C17 H17B 106.1(14) . . ? H17A C17 H17B 109(2) . . ? C16 C17 H17C 114.0(16) . . ? H17A C17 H17C 109(2) . . ? H17B C17 H17C 108(2) . . ? C16 C18 H18A 111.6(15) . . ? C16 C18 H18B 106.0(15) . . ? H18A C18 H18B 108(2) . . ? C16 C18 H18C 113.2(16) . . ? H18A C18 H18C 107(2) . . ? H18B C18 H18C 111(2) . . ? C16 C19 H19A 110.5(13) . . ? C16 C19 H19B 112.2(13) . . ? H19A C19 H19B 106.0(19) . . ? C16 C19 H19C 114.4(14) . . ? H19A C19 H19C 106.4(19) . . ? H19B C19 H19C 106.8(19) . . ? C23 C20 C22 110.7(2) . . ? C23 C20 C21 110.23(19) . . ? C22 C20 C21 105.95(18) . . ? C23 C20 P1 112.88(15) . . ? C22 C20 P1 107.02(14) . . ? C21 C20 P1 109.80(15) . . ? C20 C21 H21A 110.5(15) . . ? C20 C21 H21B 111.9(16) . . ? H21A C21 H21B 109(2) . . ? C20 C21 H21C 107.5(18) . . ? H21A C21 H21C 107(2) . . ? H21B C21 H21C 112(2) . . ? C20 C22 H22A 110.0(14) . . ? C20 C22 H22B 115.8(16) . . ? H22A C22 H22B 110(2) . . ? C20 C22 H22C 108.1(15) . . ? H22A C22 H22C 106(2) . . ? H22B C22 H22C 107(2) . . ? C20 C23 H23A 112.0(14) . . ? C20 C23 H23B 110.3(15) . . ? H23A C23 H23B 110(2) . . ? C20 C23 H23C 111.1(17) . . ? H23A C23 H23C 106(2) . . ? H23B C23 H23C 107(2) . . ? C27 C24 C26 110.37(17) . . ? C27 C24 C25 109.67(19) . . ? C26 C24 C25 106.52(18) . . ? C27 C24 P1 111.62(14) . . ? C26 C24 P1 110.85(14) . . ? C25 C24 P1 107.63(14) . . ? C24 C25 H25A 109.1(14) . . ? C24 C25 H25B 112.8(15) . . ? H25A C25 H25B 106(2) . . ? C24 C25 H25C 110.1(16) . . ? H25A C25 H25C 109(2) . . ? H25B C25 H25C 109(2) . . ? C24 C26 H26A 112.0(13) . . ? C24 C26 H26B 107.5(14) . . ? H26A C26 H26B 107.1(19) . . ? C24 C26 H26C 112.0(15) . . ? H26A C26 H26C 110.8(19) . . ? H26B C26 H26C 107(2) . . ? C24 C27 H27A 112.2(16) . . ? C24 C27 H27B 109.3(14) . . ? H27A C27 H27B 109(2) . . ? C24 C27 H27C 113.2(14) . . ? H27A C27 H27C 104(2) . . ? H27B C27 H27C 109(2) . . ? O2 S1 O3 115.04(10) . . ? O2 S1 O1 114.99(12) . . ? O3 S1 O1 114.56(10) . . ? O2 S1 C28 103.33(11) . . ? O3 S1 C28 103.81(9) . . ? O1 S1 C28 102.80(10) . . ? F3 C28 F2 108.80(19) . . ? F3 C28 F1 106.64(18) . . ? F2 C28 F1 106.31(17) . . ? F3 C28 S1 111.73(15) . . ? F2 C28 S1 112.19(14) . . ? F1 C28 S1 110.88(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pd1 Fe1 C4 159.98(9) . . . . ? P2 Pd1 Fe1 C4 -24.43(9) . . . . ? P1 Pd1 Fe1 C10 -17.74(8) . . . . ? P2 Pd1 Fe1 C10 157.86(8) . . . . ? P1 Pd1 Fe1 C8 -54.59(6) . . . . ? P2 Pd1 Fe1 C8 121.01(6) . . . . ? P1 Pd1 Fe1 C6 126.34(6) . . . . ? P2 Pd1 Fe1 C6 -58.07(6) . . . . ? P1 Pd1 Fe1 C9 -60.67(7) . . . . ? P2 Pd1 Fe1 C9 114.93(7) . . . . ? P1 Pd1 Fe1 C5 119.42(7) . . . . ? P2 Pd1 Fe1 C5 -64.99(7) . . . . ? P1 Pd1 Fe1 C11 8.70(6) . . . . ? P2 Pd1 Fe1 C11 -175.71(6) . . . . ? P1 Pd1 Fe1 C3 -171.17(6) . . . . ? P2 Pd1 Fe1 C3 4.43(6) . . . . ? P1 Pd1 Fe1 C2 170.18(6) . . . . ? P2 Pd1 Fe1 C2 -14.23(6) . . . . ? P1 Pd1 Fe1 C7 -12.05(6) . . . . ? P2 Pd1 Fe1 C7 163.54(6) . . . . ? C1 Pd1 P1 C7 -168.41(12) . . . . ? P2 Pd1 P1 C7 0.89(8) . . . . ? Fe1 Pd1 P1 C7 12.63(6) . . . . ? C1 Pd1 P1 C20 82.00(13) . . . . ? P2 Pd1 P1 C20 -108.70(9) . . . . ? Fe1 Pd1 P1 C20 -96.96(8) . . . . ? C1 Pd1 P1 C24 -62.20(12) . . . . ? P2 Pd1 P1 C24 107.11(8) . . . . ? Fe1 Pd1 P1 C24 118.85(7) . . . . ? C1 Pd1 P2 C2 -164.19(12) . . . . ? P1 Pd1 P2 C2 26.50(8) . . . . ? Fe1 Pd1 P2 C2 14.77(6) . . . . ? C1 Pd1 P2 C16 86.37(12) . . . . ? P1 Pd1 P2 C16 -82.94(8) . . . . ? Fe1 Pd1 P2 C16 -94.67(7) . . . . ? C1 Pd1 P2 C12 -59.21(13) . . . . ? P1 Pd1 P2 C12 131.48(9) . . . . ? Fe1 Pd1 P2 C12 119.75(8) . . . . ? C16 P2 C2 C3 -5.5(2) . . . . ? C12 P2 C2 C3 115.39(19) . . . . ? Pd1 P2 C2 C3 -119.92(18) . . . . ? C16 P2 C2 C6 171.40(14) . . . . ? C12 P2 C2 C6 -67.73(16) . . . . ? Pd1 P2 C2 C6 56.96(14) . . . . ? C16 P2 C2 Fe1 87.84(13) . . . . ? C12 P2 C2 Fe1 -151.29(11) . . . . ? Pd1 P2 C2 Fe1 -26.60(10) . . . . ? C4 Fe1 C2 C3 -37.85(12) . . . . ? C10 Fe1 C2 C3 -7.8(3) . . . . ? C8 Fe1 C2 C3 100.22(13) . . . . ? C6 Fe1 C2 C3 -118.71(16) . . . . ? C9 Fe1 C2 C3 53.44(16) . . . . ? C5 Fe1 C2 C3 -81.34(13) . . . . ? C11 Fe1 C2 C3 -161.32(17) . . . . ? C7 Fe1 C2 C3 148.10(12) . . . . ? Pd1 Fe1 C2 C3 150.63(12) . . . . ? C4 Fe1 C2 C6 80.86(13) . . . . ? C10 Fe1 C2 C6 111.0(3) . . . . ? C8 Fe1 C2 C6 -141.07(11) . . . . ? C9 Fe1 C2 C6 172.15(12) . . . . ? C5 Fe1 C2 C6 37.37(12) . . . . ? C11 Fe1 C2 C6 -42.6(2) . . . . ? C3 Fe1 C2 C6 118.71(16) . . . . ? C7 Fe1 C2 C6 -93.19(13) . . . . ? Pd1 Fe1 C2 C6 -90.66(11) . . . . ? C4 Fe1 C2 P2 -166.45(15) . . . . ? C10 Fe1 C2 P2 -136.4(3) . . . . ? C8 Fe1 C2 P2 -28.38(15) . . . . ? C6 Fe1 C2 P2 112.69(17) . . . . ? C9 Fe1 C2 P2 -75.16(15) . . . . ? C5 Fe1 C2 P2 150.06(15) . . . . ? C11 Fe1 C2 P2 70.1(2) . . . . ? C3 Fe1 C2 P2 -128.60(18) . . . . ? C7 Fe1 C2 P2 19.50(16) . . . . ? Pd1 Fe1 C2 P2 22.03(9) . . . . ? C6 C2 C3 C4 1.5(2) . . . . ? P2 C2 C3 C4 178.71(15) . . . . ? Fe1 C2 C3 C4 59.59(13) . . . . ? C6 C2 C3 Fe1 -58.08(12) . . . . ? P2 C2 C3 Fe1 119.12(17) . . . . ? C10 Fe1 C3 C4 58.79(16) . . . . ? C8 Fe1 C3 C4 138.92(13) . . . . ? C6 Fe1 C3 C4 -80.44(13) . . . . ? C9 Fe1 C3 C4 98.03(14) . . . . ? C5 Fe1 C3 C4 -37.15(13) . . . . ? C11 Fe1 C3 C4 35.5(3) . . . . ? C2 Fe1 C3 C4 -118.61(18) . . . . ? C7 Fe1 C3 C4 167.80(16) . . . . ? Pd1 Fe1 C3 C4 -144.89(12) . . . . ? C4 Fe1 C3 C2 118.61(18) . . . . ? C10 Fe1 C3 C2 177.40(11) . . . . ? C8 Fe1 C3 C2 -102.47(12) . . . . ? C6 Fe1 C3 C2 38.17(11) . . . . ? C9 Fe1 C3 C2 -143.36(12) . . . . ? C5 Fe1 C3 C2 81.46(12) . . . . ? C11 Fe1 C3 C2 154.2(2) . . . . ? C7 Fe1 C3 C2 -73.6(2) . . . . ? Pd1 Fe1 C3 C2 -26.28(11) . . . . ? C2 C3 C4 C5 -0.7(2) . . . . ? Fe1 C3 C4 C5 60.02(14) . . . . ? C2 C3 C4 Fe1 -60.72(13) . . . . ? C10 Fe1 C4 C5 106.22(13) . . . . ? C8 Fe1 C4 C5 169.94(13) . . . . ? C6 Fe1 C4 C5 -37.58(12) . . . . ? C9 Fe1 C4 C5 146.55(12) . . . . ? C11 Fe1 C4 C5 72.88(15) . . . . ? C3 Fe1 C4 C5 -119.72(18) . . . . ? C2 Fe1 C4 C5 -81.91(13) . . . . ? C7 Fe1 C4 C5 80.3(3) . . . . ? Pd1 Fe1 C4 C5 -72.06(13) . . . . ? C10 Fe1 C4 C3 -134.06(13) . . . . ? C8 Fe1 C4 C3 -70.34(17) . . . . ? C6 Fe1 C4 C3 82.14(13) . . . . ? C9 Fe1 C4 C3 -93.73(13) . . . . ? C5 Fe1 C4 C3 119.72(18) . . . . ? C11 Fe1 C4 C3 -167.40(12) . . . . ? C2 Fe1 C4 C3 37.81(12) . . . . ? C7 Fe1 C4 C3 -160.0(3) . . . . ? Pd1 Fe1 C4 C3 47.66(15) . . . . ? C3 C4 C5 C6 -0.4(2) . . . . ? Fe1 C4 C5 C6 59.76(14) . . . . ? C3 C4 C5 Fe1 -60.20(14) . . . . ? C4 Fe1 C5 C6 -118.86(18) . . . . ? C10 Fe1 C5 C6 158.15(12) . . . . ? C9 Fe1 C5 C6 -169.70(13) . . . . ? C11 Fe1 C5 C6 116.31(13) . . . . ? C3 Fe1 C5 C6 -81.61(13) . . . . ? C2 Fe1 C5 C6 -38.10(12) . . . . ? C7 Fe1 C5 C6 83.25(15) . . . . ? Pd1 Fe1 C5 C6 10.18(13) . . . . ? C10 Fe1 C5 C4 -82.99(13) . . . . ? C6 Fe1 C5 C4 118.86(18) . . . . ? C9 Fe1 C5 C4 -50.85(18) . . . . ? C11 Fe1 C5 C4 -124.83(12) . . . . ? C3 Fe1 C5 C4 37.25(12) . . . . ? C2 Fe1 C5 C4 80.76(13) . . . . ? C7 Fe1 C5 C4 -157.89(12) . . . . ? Pd1 Fe1 C5 C4 129.04(11) . . . . ? C4 C5 C6 C2 1.4(2) . . . . ? Fe1 C5 C6 C2 60.93(13) . . . . ? C4 C5 C6 Fe1 -59.54(14) . . . . ? C3 C2 C6 C5 -1.8(2) . . . . ? P2 C2 C6 C5 -179.42(13) . . . . ? Fe1 C2 C6 C5 -60.33(13) . . . . ? C3 C2 C6 Fe1 58.53(13) . . . . ? P2 C2 C6 Fe1 -119.09(13) . . . . ? C4 Fe1 C6 C5 37.69(13) . . . . ? C10 Fe1 C6 C5 -35.8(2) . . . . ? C8 Fe1 C6 C5 -171.33(14) . . . . ? C11 Fe1 C6 C5 -80.12(14) . . . . ? C3 Fe1 C6 C5 81.31(13) . . . . ? C2 Fe1 C6 C5 118.92(17) . . . . ? C7 Fe1 C6 C5 -126.46(13) . . . . ? Pd1 Fe1 C6 C5 -169.83(13) . . . . ? C4 Fe1 C6 C2 -81.24(12) . . . . ? C10 Fe1 C6 C2 -154.68(13) . . . . ? C8 Fe1 C6 C2 69.74(17) . . . . ? C5 Fe1 C6 C2 -118.92(17) . . . . ? C11 Fe1 C6 C2 160.95(11) . . . . ? C3 Fe1 C6 C2 -37.61(11) . . . . ? C7 Fe1 C6 C2 114.62(11) . . . . ? Pd1 Fe1 C6 C2 71.25(10) . . . . ? C20 P1 C7 C11 4.6(2) . . . . ? C24 P1 C7 C11 124.70(19) . . . . ? Pd1 P1 C7 C11 -114.30(18) . . . . ? C20 P1 C7 C8 179.39(14) . . . . ? C24 P1 C7 C8 -60.56(16) . . . . ? Pd1 P1 C7 C8 60.44(14) . . . . ? C20 P1 C7 Fe1 96.78(12) . . . . ? C24 P1 C7 Fe1 -143.17(11) . . . . ? Pd1 P1 C7 Fe1 -22.16(10) . . . . ? C4 Fe1 C7 C11 -9.5(4) . . . . ? C10 Fe1 C7 C11 -37.41(12) . . . . ? C8 Fe1 C7 C11 -118.20(15) . . . . ? C6 Fe1 C7 C11 101.34(12) . . . . ? C9 Fe1 C7 C11 -80.91(12) . . . . ? C5 Fe1 C7 C11 54.37(15) . . . . ? C3 Fe1 C7 C11 -159.19(17) . . . . ? C2 Fe1 C7 C11 149.68(12) . . . . ? Pd1 Fe1 C7 C11 147.18(12) . . . . ? C4 Fe1 C7 C8 108.7(3) . . . . ? C10 Fe1 C7 C8 80.79(12) . . . . ? C6 Fe1 C7 C8 -140.46(11) . . . . ? C9 Fe1 C7 C8 37.29(11) . . . . ? C5 Fe1 C7 C8 172.57(12) . . . . ? C11 Fe1 C7 C8 118.20(15) . . . . ? C3 Fe1 C7 C8 -41.0(2) . . . . ? C2 Fe1 C7 C8 -92.11(13) . . . . ? Pd1 Fe1 C7 C8 -94.62(11) . . . . ? C4 Fe1 C7 P1 -138.6(3) . . . . ? C10 Fe1 C7 P1 -166.43(15) . . . . ? C8 Fe1 C7 P1 112.77(16) . . . . ? C6 Fe1 C7 P1 -27.68(15) . . . . ? C9 Fe1 C7 P1 150.07(14) . . . . ? C5 Fe1 C7 P1 -74.65(15) . . . . ? C11 Fe1 C7 P1 -129.02(18) . . . . ? C3 Fe1 C7 P1 71.8(2) . . . . ? C2 Fe1 C7 P1 20.66(16) . . . . ? Pd1 Fe1 C7 P1 18.15(9) . . . . ? C11 C7 C8 C9 -1.8(2) . . . . ? P1 C7 C8 C9 -177.83(13) . . . . ? Fe1 C7 C8 C9 -60.36(13) . . . . ? C11 C7 C8 Fe1 58.57(12) . . . . ? P1 C7 C8 Fe1 -117.47(12) . . . . ? C4 Fe1 C8 C9 -36.30(19) . . . . ? C10 Fe1 C8 C9 37.73(12) . . . . ? C6 Fe1 C8 C9 -169.82(14) . . . . ? C11 Fe1 C8 C9 81.27(13) . . . . ? C3 Fe1 C8 C9 -79.70(14) . . . . ? C2 Fe1 C8 C9 -125.55(12) . . . . ? C7 Fe1 C8 C9 119.24(16) . . . . ? Pd1 Fe1 C8 C9 -171.30(13) . . . . ? C4 Fe1 C8 C7 -155.53(13) . . . . ? C10 Fe1 C8 C7 -81.51(12) . . . . ? C6 Fe1 C8 C7 70.95(17) . . . . ? C9 Fe1 C8 C7 -119.24(16) . . . . ? C11 Fe1 C8 C7 -37.97(11) . . . . ? C3 Fe1 C8 C7 161.06(10) . . . . ? C2 Fe1 C8 C7 115.22(11) . . . . ? Pd1 Fe1 C8 C7 69.47(9) . . . . ? C7 C8 C9 C10 1.5(2) . . . . ? Fe1 C8 C9 C10 -59.63(13) . . . . ? C7 C8 C9 Fe1 61.13(13) . . . . ? C4 Fe1 C9 C8 157.63(12) . . . . ? C10 Fe1 C9 C8 -118.81(17) . . . . ? C5 Fe1 C9 C8 -171.02(13) . . . . ? C11 Fe1 C9 C8 -81.42(13) . . . . ? C3 Fe1 C9 C8 115.88(12) . . . . ? C2 Fe1 C9 C8 83.50(15) . . . . ? C7 Fe1 C9 C8 -37.82(12) . . . . ? Pd1 Fe1 C9 C8 9.09(13) . . . . ? C4 Fe1 C9 C10 -83.57(13) . . . . ? C8 Fe1 C9 C10 118.81(17) . . . . ? C5 Fe1 C9 C10 -52.22(18) . . . . ? C11 Fe1 C9 C10 37.39(12) . . . . ? C3 Fe1 C9 C10 -125.31(12) . . . . ? C2 Fe1 C9 C10 -157.69(12) . . . . ? C7 Fe1 C9 C10 80.99(13) . . . . ? Pd1 Fe1 C9 C10 127.90(11) . . . . ? C8 C9 C10 C11 -0.6(2) . . . . ? Fe1 C9 C10 C11 -60.28(13) . . . . ? C8 C9 C10 Fe1 59.66(13) . . . . ? C4 Fe1 C10 C9 105.52(13) . . . . ? C8 Fe1 C10 C9 -37.66(12) . . . . ? C6 Fe1 C10 C9 168.81(13) . . . . ? C5 Fe1 C10 C9 145.73(12) . . . . ? C11 Fe1 C10 C9 -119.33(17) . . . . ? C3 Fe1 C10 C9 71.62(14) . . . . ? C2 Fe1 C10 C9 77.6(3) . . . . ? C7 Fe1 C10 C9 -81.80(13) . . . . ? Pd1 Fe1 C10 C9 -76.26(13) . . . . ? C4 Fe1 C10 C11 -135.15(13) . . . . ? C8 Fe1 C10 C11 81.68(13) . . . . ? C6 Fe1 C10 C11 -71.86(18) . . . . ? C9 Fe1 C10 C11 119.33(17) . . . . ? C5 Fe1 C10 C11 -94.94(13) . . . . ? C3 Fe1 C10 C11 -169.05(12) . . . . ? C2 Fe1 C10 C11 -163.0(3) . . . . ? C7 Fe1 C10 C11 37.53(12) . . . . ? Pd1 Fe1 C10 C11 43.08(15) . . . . ? C9 C10 C11 C7 -0.5(2) . . . . ? Fe1 C10 C11 C7 -60.54(13) . . . . ? C9 C10 C11 Fe1 60.03(14) . . . . ? C8 C7 C11 C10 1.4(2) . . . . ? P1 C7 C11 C10 176.68(15) . . . . ? Fe1 C7 C11 C10 59.46(13) . . . . ? C8 C7 C11 Fe1 -58.07(12) . . . . ? P1 C7 C11 Fe1 117.22(17) . . . . ? C4 Fe1 C11 C10 57.65(15) . . . . ? C8 Fe1 C11 C10 -80.89(13) . . . . ? C6 Fe1 C11 C10 138.54(12) . . . . ? C9 Fe1 C11 C10 -37.43(12) . . . . ? C5 Fe1 C11 C10 97.41(13) . . . . ? C3 Fe1 C11 C10 30.6(3) . . . . ? C2 Fe1 C11 C10 168.87(16) . . . . ? C7 Fe1 C11 C10 -119.25(17) . . . . ? Pd1 Fe1 C11 C10 -148.92(11) . . . . ? C4 Fe1 C11 C7 176.90(11) . . . . ? C10 Fe1 C11 C7 119.25(17) . . . . ? C8 Fe1 C11 C7 38.35(11) . . . . ? C6 Fe1 C11 C7 -102.21(12) . . . . ? C9 Fe1 C11 C7 81.82(12) . . . . ? C5 Fe1 C11 C7 -143.34(11) . . . . ? C3 Fe1 C11 C7 149.9(2) . . . . ? C2 Fe1 C11 C7 -71.9(2) . . . . ? Pd1 Fe1 C11 C7 -29.67(11) . . . . ? C2 P2 C12 C14 -163.84(17) . . . . ? C16 P2 C12 C14 -45.26(19) . . . . ? Pd1 P2 C12 C14 100.80(17) . . . . ? C2 P2 C12 C15 -40.85(18) . . . . ? C16 P2 C12 C15 77.73(18) . . . . ? Pd1 P2 C12 C15 -136.21(15) . . . . ? C2 P2 C12 C13 78.40(16) . . . . ? C16 P2 C12 C13 -163.02(15) . . . . ? Pd1 P2 C12 C13 -16.96(18) . . . . ? C2 P2 C16 C18 62.05(17) . . . . ? C12 P2 C16 C18 -53.71(18) . . . . ? Pd1 P2 C16 C18 156.61(13) . . . . ? C2 P2 C16 C19 -60.05(15) . . . . ? C12 P2 C16 C19 -175.81(14) . . . . ? Pd1 P2 C16 C19 34.51(15) . . . . ? C2 P2 C16 C17 -174.91(14) . . . . ? C12 P2 C16 C17 69.33(16) . . . . ? Pd1 P2 C16 C17 -80.35(15) . . . . ? C7 P1 C20 C23 62.32(19) . . . . ? C24 P1 C20 C23 -52.91(19) . . . . ? Pd1 P1 C20 C23 160.17(15) . . . . ? C7 P1 C20 C22 -59.70(16) . . . . ? C24 P1 C20 C22 -174.93(14) . . . . ? Pd1 P1 C20 C22 38.15(17) . . . . ? C7 P1 C20 C21 -174.25(15) . . . . ? C24 P1 C20 C21 70.52(17) . . . . ? Pd1 P1 C20 C21 -76.40(16) . . . . ? C7 P1 C24 C27 -37.83(17) . . . . ? C20 P1 C24 C27 79.34(17) . . . . ? Pd1 P1 C24 C27 -134.62(14) . . . . ? C7 P1 C24 C26 -161.32(15) . . . . ? C20 P1 C24 C26 -44.15(18) . . . . ? Pd1 P1 C24 C26 101.90(14) . . . . ? C7 P1 C24 C25 82.56(16) . . . . ? C20 P1 C24 C25 -160.28(15) . . . . ? Pd1 P1 C24 C25 -14.23(17) . . . . ? O2 S1 C28 F3 -56.45(19) . . . . ? O3 S1 C28 F3 63.96(18) . . . . ? O1 S1 C28 F3 -176.39(17) . . . . ? O2 S1 C28 F2 -178.95(16) . . . . ? O3 S1 C28 F2 -58.54(17) . . . . ? O1 S1 C28 F2 61.12(17) . . . . ? O2 S1 C28 F1 62.36(17) . . . . ? O3 S1 C28 F1 -177.23(14) . . . . ? O1 S1 C28 F1 -57.58(17) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.661 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.065 #===END # Compound 6a data_Compound_6a _database_code_CSD 177716 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H31 F3 O3 P2 Pd' _chemical_formula_sum 'C39 H31 F3 O3 P2 Pd' _chemical_formula_weight 772.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9760(10) _cell_length_b 11.5160(10) _cell_length_c 15.503(5) _cell_angle_alpha 98.140(10) _cell_angle_beta 97.050(10) _cell_angle_gamma 113.890(10) _cell_volume 1738.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 40.00 _cell_measurement_theta_max 40.82 _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 5.626 _exptl_absorpt_correction_type 'Psi-scans' _exptl_absorpt_correction_T_min 0.630 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w/2\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 7 _diffrn_reflns_number 7139 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 74.73 _reflns_number_total 7139 _reflns_number_gt 6854 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction 'HELENA' _computing_structure_solution 'DIRDIF' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1266P)^2^+2.7287P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7139 _refine_ls_number_parameters 462 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0642 _refine_ls_wR_factor_ref 0.1774 _refine_ls_wR_factor_gt 0.1761 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.020 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.00938(3) 0.23265(3) 0.217574(19) 0.03601(14) Uani 1 1 d . . . P1 P 0.09588(11) 0.07434(10) 0.23399(7) 0.0362(2) Uani 1 1 d . . . P2 P 0.20145(12) 0.41119(10) 0.23603(8) 0.0379(2) Uani 1 1 d . . . F1A F -0.3945(10) -0.1321(7) 0.2707(7) 0.094(3) Uani 0.59 1 d PDU A 1 F2A F -0.4559(13) 0.0136(13) 0.3077(9) 0.153(6) Uani 0.59 1 d PDU A 1 F3A F -0.4535(10) -0.0483(13) 0.1742(6) 0.146(5) Uani 0.59 1 d PDU A 1 F1B F -0.4182(16) -0.1362(10) 0.2179(11) 0.126(6) Uani 0.41 1 d PDU A 2 F2B F -0.4279(14) -0.0227(16) 0.3325(7) 0.113(6) Uani 0.41 1 d PDU A 2 F3B F -0.4615(13) 0.0235(14) 0.2101(9) 0.099(4) Uani 0.41 1 d PDU A 2 O1 O 0.3038(3) 0.2522(3) 0.1383(2) 0.0439(7) Uani 1 1 d . . . O2 O -0.1924(3) 0.0904(3) 0.2019(2) 0.0471(7) Uani 1 1 d . . . O3 O -0.1781(6) 0.1298(7) 0.3477(3) 0.109(2) Uani 1 1 d . . . C1 C -0.0853(6) 0.3569(5) 0.2076(4) 0.0511(11) Uani 1 1 d . . . H1A H -0.1622 0.3174 0.1591 0.077 Uiso 1 1 calc R . . H1B H -0.0219 0.4378 0.1973 0.077 Uiso 1 1 calc R . . H1C H -0.1151 0.3726 0.2619 0.077 Uiso 1 1 calc R . . C2 C -0.2372(6) 0.0783(6) 0.2717(4) 0.0549(12) Uani 1 1 d . A . C3 C -0.3860(6) -0.0187(6) 0.2564(4) 0.0709(17) Uani 1 1 d D . . C11 C 0.1900(5) 0.0309(4) 0.1546(3) 0.0386(9) Uani 1 1 d . . . C12 C 0.1688(5) -0.0981(5) 0.1279(4) 0.0513(11) Uani 1 1 d . . . H12 H 0.1148 -0.1608 0.1558 0.062 Uiso 1 1 calc R . . C13 C 0.2269(6) -0.1345(6) 0.0606(4) 0.0617(14) Uani 1 1 d . . . H13 H 0.2117 -0.2208 0.0441 0.074 Uiso 1 1 calc R . . C14 C 0.3067(7) -0.0434(7) 0.0182(4) 0.0654(15) Uani 1 1 d . . . H14 H 0.3432 -0.0684 -0.0281 0.079 Uiso 1 1 calc R . . C15 C 0.3324(6) 0.0849(6) 0.0448(4) 0.0584(13) Uani 1 1 d . . . H15 H 0.3872 0.1469 0.0168 0.070 Uiso 1 1 calc R . . C16 C 0.2767(5) 0.1220(5) 0.1133(3) 0.0408(9) Uani 1 1 d . . . C21 C 0.3610(5) 0.4018(4) 0.2735(3) 0.0412(9) Uani 1 1 d . . . C22 C 0.4498(6) 0.4725(5) 0.3541(4) 0.0530(12) Uani 1 1 d . . . H22 H 0.4297 0.5291 0.3924 0.064 Uiso 1 1 calc R . . C23 C 0.5697(6) 0.4578(6) 0.3769(4) 0.0642(15) Uani 1 1 d . . . H23 H 0.6290 0.5050 0.4307 0.077 Uiso 1 1 calc R . . C24 C 0.6007(6) 0.3748(6) 0.3213(4) 0.0644(15) Uani 1 1 d . . . H24 H 0.6796 0.3647 0.3379 0.077 Uiso 1 1 calc R . . C25 C 0.5142(5) 0.3055(5) 0.2398(4) 0.0524(11) Uani 1 1 d . . . H25 H 0.5361 0.2514 0.2006 0.063 Uiso 1 1 calc R . . C26 C 0.3944(5) 0.3189(4) 0.2184(3) 0.0416(9) Uani 1 1 d . . . C31 C -0.0390(5) -0.0871(5) 0.2279(4) 0.0499(11) Uani 1 1 d . . . C32 C -0.0397(9) -0.1577(6) 0.2938(5) 0.075(2) Uani 1 1 d . . . H32 H 0.0268 -0.1217 0.3456 0.091 Uiso 1 1 calc R . . C33 C -0.1423(11) -0.2839(7) 0.2807(6) 0.099(3) Uani 1 1 d U . . H33 H -0.1441 -0.3323 0.3242 0.119 Uiso 1 1 calc R . . C34 C -0.2412(10) -0.3375(7) 0.2038(8) 0.105(3) Uani 1 1 d U . . H34 H -0.3098 -0.4209 0.1965 0.126 Uiso 1 1 calc R . . C35 C -0.2392(7) -0.2696(7) 0.1391(7) 0.087(3) Uani 1 1 d . . . H35 H -0.3045 -0.3072 0.0869 0.104 Uiso 1 1 calc R . . C36 C -0.1383(6) -0.1424(5) 0.1513(5) 0.0652(16) Uani 1 1 d . . . H36 H -0.1382 -0.0949 0.1075 0.078 Uiso 1 1 calc R . . C41 C 0.2005(5) 0.1138(4) 0.3440(3) 0.0447(10) Uani 1 1 d . . . C42 C 0.1523(8) 0.1553(7) 0.4155(4) 0.0701(16) Uani 1 1 d . . . H42 H 0.0717 0.1646 0.4062 0.084 Uiso 1 1 calc R . . C43 C 0.2263(12) 0.1827(9) 0.5011(5) 0.099(3) Uani 1 1 d . . . H43 H 0.1934 0.2077 0.5495 0.119 Uiso 1 1 calc R . . C44 C 0.3473(12) 0.1733(8) 0.5149(5) 0.096(3) Uani 1 1 d . . . H44 H 0.3961 0.1929 0.5725 0.115 Uiso 1 1 calc R . . C45 C 0.3974(8) 0.1355(7) 0.4453(5) 0.078(2) Uani 1 1 d . . . H45 H 0.4803 0.1307 0.4553 0.094 Uiso 1 1 calc R . . C46 C 0.3231(6) 0.1041(5) 0.3590(4) 0.0529(12) Uani 1 1 d . . . H46 H 0.3557 0.0765 0.3113 0.063 Uiso 1 1 calc R . . C51 C 0.2079(5) 0.5416(5) 0.3211(3) 0.0474(10) Uani 1 1 d . . . C52 C 0.1606(7) 0.5099(7) 0.3976(4) 0.0649(14) Uani 1 1 d . . . H52 H 0.1261 0.4241 0.4041 0.078 Uiso 1 1 calc R . . C53 C 0.1647(7) 0.6065(8) 0.4643(4) 0.0759(19) Uani 1 1 d . . . H53 H 0.1346 0.5849 0.5159 0.091 Uiso 1 1 calc R . . C54 C 0.2123(8) 0.7325(8) 0.4552(5) 0.082(2) Uani 1 1 d . . . H54 H 0.2125 0.7962 0.4995 0.099 Uiso 1 1 calc R . . C55 C 0.2598(9) 0.7640(7) 0.3804(6) 0.086(2) Uani 1 1 d . . . H55 H 0.2938 0.8501 0.3745 0.103 Uiso 1 1 calc R . . C56 C 0.2584(7) 0.6704(6) 0.3133(5) 0.0645(15) Uani 1 1 d . . . H56 H 0.2913 0.6938 0.2628 0.077 Uiso 1 1 calc R . . C61 C 0.2319(5) 0.4767(4) 0.1364(3) 0.0420(9) Uani 1 1 d . . . C62 C 0.1303(6) 0.4296(5) 0.0611(3) 0.0502(11) Uani 1 1 d . . . H62 H 0.0451 0.3655 0.0619 0.060 Uiso 1 1 calc R . . C63 C 0.1542(7) 0.4770(7) -0.0154(4) 0.0633(15) Uani 1 1 d . . . H63 H 0.0849 0.4447 -0.0655 0.076 Uiso 1 1 calc R . . C64 C 0.2778(7) 0.5700(7) -0.0177(4) 0.0641(15) Uani 1 1 d . . . H64 H 0.2928 0.6018 -0.0692 0.077 Uiso 1 1 calc R . . C65 C 0.3818(7) 0.6179(7) 0.0565(5) 0.0683(16) Uani 1 1 d . . . H65 H 0.4668 0.6815 0.0549 0.082 Uiso 1 1 calc R . . C66 C 0.3585(6) 0.5701(6) 0.1334(4) 0.0571(13) Uani 1 1 d . . . H66 H 0.4285 0.6013 0.1831 0.069 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.0358(2) 0.0326(2) 0.0394(2) 0.01195(13) 0.00465(13) 0.01372(14) P1 0.0404(5) 0.0307(5) 0.0386(5) 0.0116(4) 0.0077(4) 0.0152(4) P2 0.0391(5) 0.0312(5) 0.0419(5) 0.0131(4) 0.0036(4) 0.0131(4) F1A 0.092(6) 0.055(4) 0.106(6) 0.020(4) 0.011(5) 0.005(4) F2A 0.092(7) 0.153(10) 0.231(13) 0.007(9) 0.080(8) 0.067(7) F3A 0.060(5) 0.179(11) 0.134(8) 0.080(8) -0.025(5) -0.016(6) F1B 0.088(8) 0.071(7) 0.185(13) -0.030(8) 0.037(10) 0.016(6) F2B 0.070(7) 0.155(12) 0.127(9) 0.076(9) 0.055(7) 0.037(7) F3B 0.065(6) 0.099(8) 0.127(10) 0.027(7) -0.006(6) 0.037(6) O1 0.0491(17) 0.0431(17) 0.0430(16) 0.0175(13) 0.0053(13) 0.0216(14) O2 0.0381(16) 0.0427(17) 0.0527(18) 0.0093(14) 0.0071(14) 0.0106(14) O3 0.083(4) 0.144(6) 0.053(3) 0.003(3) 0.013(3) 0.009(4) C1 0.050(3) 0.044(3) 0.068(3) 0.022(2) 0.012(2) 0.026(2) C2 0.048(3) 0.060(3) 0.058(3) 0.017(2) 0.015(2) 0.021(2) C3 0.050(3) 0.066(4) 0.105(5) 0.037(4) 0.025(3) 0.025(3) C11 0.042(2) 0.039(2) 0.0358(19) 0.0061(16) 0.0050(17) 0.0192(18) C12 0.048(3) 0.041(2) 0.063(3) 0.006(2) 0.009(2) 0.019(2) C13 0.058(3) 0.054(3) 0.067(3) -0.008(3) 0.007(3) 0.028(3) C14 0.069(4) 0.083(4) 0.049(3) -0.001(3) 0.013(3) 0.042(3) C15 0.066(3) 0.072(4) 0.044(3) 0.019(2) 0.019(2) 0.032(3) C16 0.046(2) 0.046(2) 0.0344(19) 0.0125(17) 0.0034(17) 0.023(2) C21 0.040(2) 0.037(2) 0.045(2) 0.0196(18) 0.0023(18) 0.0126(18) C22 0.052(3) 0.048(3) 0.051(3) 0.013(2) -0.003(2) 0.017(2) C23 0.051(3) 0.060(3) 0.064(3) 0.014(3) -0.015(3) 0.014(3) C24 0.044(3) 0.067(4) 0.077(4) 0.022(3) -0.007(3) 0.022(3) C25 0.047(3) 0.050(3) 0.064(3) 0.021(2) 0.010(2) 0.022(2) C26 0.040(2) 0.037(2) 0.046(2) 0.0207(18) 0.0061(18) 0.0120(18) C31 0.052(3) 0.032(2) 0.065(3) 0.009(2) 0.021(2) 0.016(2) C32 0.104(5) 0.044(3) 0.071(4) 0.020(3) 0.041(4) 0.015(3) C33 0.142(7) 0.046(3) 0.100(6) 0.022(4) 0.070(6) 0.014(4) C34 0.101(6) 0.042(3) 0.148(8) -0.004(4) 0.070(6) 0.002(4) C35 0.056(4) 0.045(3) 0.139(7) -0.013(4) 0.011(4) 0.014(3) C36 0.045(3) 0.040(3) 0.100(5) -0.001(3) 0.004(3) 0.016(2) C41 0.060(3) 0.032(2) 0.038(2) 0.0129(17) 0.0068(19) 0.015(2) C42 0.092(5) 0.074(4) 0.048(3) 0.012(3) 0.018(3) 0.038(4) C43 0.154(9) 0.094(6) 0.041(3) 0.009(3) 0.022(4) 0.045(6) C44 0.142(8) 0.083(5) 0.048(4) 0.015(3) -0.017(4) 0.042(5) C45 0.087(5) 0.071(4) 0.067(4) 0.022(3) -0.019(3) 0.032(4) C46 0.060(3) 0.048(3) 0.052(3) 0.018(2) -0.001(2) 0.026(2) C51 0.046(2) 0.041(2) 0.048(2) 0.0065(19) 0.000(2) 0.016(2) C52 0.069(4) 0.067(4) 0.057(3) 0.012(3) 0.013(3) 0.027(3) C53 0.070(4) 0.099(5) 0.054(3) 0.002(3) 0.009(3) 0.036(4) C54 0.079(4) 0.079(5) 0.079(5) -0.020(4) -0.002(4) 0.041(4) C55 0.102(6) 0.054(4) 0.096(5) -0.004(4) 0.006(5) 0.038(4) C56 0.077(4) 0.042(3) 0.075(4) 0.013(3) 0.011(3) 0.027(3) C61 0.048(2) 0.034(2) 0.047(2) 0.0163(18) 0.0090(19) 0.0189(18) C62 0.055(3) 0.051(3) 0.049(3) 0.015(2) 0.005(2) 0.026(2) C63 0.078(4) 0.080(4) 0.044(3) 0.019(3) 0.007(3) 0.045(3) C64 0.088(4) 0.075(4) 0.059(3) 0.040(3) 0.028(3) 0.052(4) C65 0.068(4) 0.066(4) 0.081(4) 0.045(3) 0.025(3) 0.026(3) C66 0.054(3) 0.053(3) 0.063(3) 0.030(3) 0.010(2) 0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C1 2.092(5) . ? Pd O2 2.113(3) . ? Pd P2 2.2199(12) . ? Pd P1 2.4008(11) . ? P1 C41 1.820(5) . ? P1 C31 1.829(5) . ? P1 C11 1.841(4) . ? P2 C61 1.822(5) . ? P2 C51 1.825(5) . ? P2 C21 1.827(5) . ? F1A C3 1.324(7) . ? F2A C3 1.287(7) . ? F3A C3 1.316(7) . ? F1B C3 1.282(7) . ? F2B C3 1.317(7) . ? F3B C3 1.311(7) . ? O1 C26 1.388(6) . ? O1 C16 1.390(6) . ? O2 C2 1.246(6) . ? O3 C2 1.210(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.524(8) . ? C11 C16 1.395(6) . ? C11 C12 1.398(6) . ? C12 C13 1.388(8) . ? C12 H12 0.9300 . ? C13 C14 1.376(10) . ? C13 H13 0.9300 . ? C14 C15 1.376(9) . ? C14 H14 0.9300 . ? C15 C16 1.388(7) . ? C15 H15 0.9300 . ? C21 C26 1.380(7) . ? C21 C22 1.394(7) . ? C22 C23 1.404(8) . ? C22 H22 0.9300 . ? C23 C24 1.369(10) . ? C23 H23 0.9300 . ? C24 C25 1.393(8) . ? C24 H24 0.9300 . ? C25 C26 1.391(7) . ? C25 H25 0.9300 . ? C31 C36 1.382(9) . ? C31 C32 1.392(9) . ? C32 C33 1.399(10) . ? C32 H32 0.9300 . ? C33 C34 1.383(15) . ? C33 H33 0.9300 . ? C34 C35 1.353(15) . ? C34 H34 0.9300 . ? C35 C36 1.401(9) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C42 1.391(8) . ? C41 C46 1.389(8) . ? C42 C43 1.389(11) . ? C42 H42 0.9300 . ? C43 C44 1.369(15) . ? C43 H43 0.9300 . ? C44 C45 1.365(13) . ? C44 H44 0.9300 . ? C45 C46 1.393(8) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C56 1.387(8) . ? C51 C52 1.389(8) . ? C52 C53 1.389(9) . ? C52 H52 0.9300 . ? C53 C54 1.364(12) . ? C53 H53 0.9300 . ? C54 C55 1.365(13) . ? C54 H54 0.9300 . ? C55 C56 1.382(10) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C66 1.382(7) . ? C61 C62 1.382(7) . ? C62 C63 1.385(8) . ? C62 H62 0.9300 . ? C63 C64 1.355(10) . ? C63 H63 0.9300 . ? C64 C65 1.385(10) . ? C64 H64 0.9300 . ? C65 C66 1.392(8) . ? C65 H65 0.9300 . ? C66 H66 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pd O2 83.13(18) . . ? C1 Pd P2 84.88(15) . . ? O2 Pd P2 167.90(10) . . ? C1 Pd P1 173.66(15) . . ? O2 Pd P1 91.01(10) . . ? P2 Pd P1 100.90(4) . . ? C41 P1 C31 103.8(2) . . ? C41 P1 C11 106.3(2) . . ? C31 P1 C11 99.3(2) . . ? C41 P1 Pd 110.89(16) . . ? C31 P1 Pd 112.54(18) . . ? C11 P1 Pd 122.05(15) . . ? C61 P2 C51 106.8(2) . . ? C61 P2 C21 102.0(2) . . ? C51 P2 C21 102.6(2) . . ? C61 P2 Pd 114.83(16) . . ? C51 P2 Pd 111.50(17) . . ? C21 P2 Pd 117.83(14) . . ? C26 O1 C16 115.6(3) . . ? C2 O2 Pd 115.4(3) . . ? Pd C1 H1A 109.5 . . ? Pd C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Pd C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 C2 O2 128.8(6) . . ? O3 C2 C3 117.6(5) . . ? O2 C2 C3 113.5(5) . . ? F1B C3 F2A 123.6(12) . . ? F1B C3 F3B 107.7(7) . . ? F2A C3 F3B 72.1(8) . . ? F1B C3 F3A 67.5(8) . . ? F2A C3 F3A 107.5(6) . . ? F1B C3 F2B 107.1(7) . . ? F3B C3 F2B 104.1(6) . . ? F3A C3 F2B 131.2(9) . . ? F2A C3 F1A 105.8(6) . . ? F3B C3 F1A 137.1(9) . . ? F3A C3 F1A 103.1(6) . . ? F2B C3 F1A 77.9(8) . . ? F1B C3 C2 117.6(8) . . ? F2A C3 C2 114.8(8) . . ? F3B C3 C2 109.3(8) . . ? F3A C3 C2 114.8(6) . . ? F2B C3 C2 110.1(8) . . ? F1A C3 C2 109.9(6) . . ? C16 C11 C12 117.1(4) . . ? C16 C11 P1 122.0(3) . . ? C12 C11 P1 120.7(4) . . ? C13 C12 C11 121.3(5) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C12 120.2(5) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 119.7(5) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 120.2(5) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 O1 118.9(4) . . ? C15 C16 C11 121.4(5) . . ? O1 C16 C11 119.7(4) . . ? C26 C21 C22 118.5(4) . . ? C26 C21 P2 117.5(3) . . ? C22 C21 P2 124.0(4) . . ? C21 C22 C23 119.5(6) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 121.0(5) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 120.1(5) . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 118.6(5) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C21 C26 O1 116.3(4) . . ? C21 C26 C25 122.3(5) . . ? O1 C26 C25 121.4(5) . . ? C36 C31 C32 119.8(5) . . ? C36 C31 P1 117.3(4) . . ? C32 C31 P1 122.7(5) . . ? C31 C32 C33 118.7(8) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C34 C33 C32 120.7(8) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C35 C34 C33 120.6(7) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C34 C35 C36 119.7(8) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C31 C36 C35 120.5(7) . . ? C31 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C42 C41 C46 119.7(5) . . ? C42 C41 P1 116.8(5) . . ? C46 C41 P1 123.4(4) . . ? C43 C42 C41 119.1(8) . . ? C43 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? C44 C43 C42 120.5(8) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C45 C44 C43 121.1(7) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C44 C45 C46 119.4(8) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C41 C46 C45 120.2(6) . . ? C41 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C56 C51 C52 118.6(5) . . ? C56 C51 P2 123.2(4) . . ? C52 C51 P2 118.2(4) . . ? C53 C52 C51 120.0(7) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C54 C53 C52 120.9(7) . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C55 C54 C53 119.2(6) . . ? C55 C54 H54 120.4 . . ? C53 C54 H54 120.4 . . ? C54 C55 C56 121.2(7) . . ? C54 C55 H55 119.4 . . ? C56 C55 H55 119.4 . . ? C55 C56 C51 120.0(7) . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C66 C61 C62 118.9(5) . . ? C66 C61 P2 120.6(4) . . ? C62 C61 P2 120.4(4) . . ? C61 C62 C63 120.5(5) . . ? C61 C62 H62 119.7 . . ? C63 C62 H62 119.7 . . ? C64 C63 C62 120.5(6) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C63 C64 C65 120.1(5) . . ? C63 C64 H64 119.9 . . ? C65 C64 H64 119.9 . . ? C64 C65 C66 119.6(6) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C61 C66 C65 120.3(6) . . ? C61 C66 H66 119.8 . . ? C65 C66 H66 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Pd P1 C41 -116.5(2) . . . . ? P2 Pd P1 C41 61.38(18) . . . . ? O2 Pd P1 C31 -0.7(2) . . . . ? P2 Pd P1 C31 177.10(19) . . . . ? O2 Pd P1 C11 117.1(2) . . . . ? P2 Pd P1 C11 -65.07(18) . . . . ? C1 Pd P2 C61 -71.6(2) . . . . ? O2 Pd P2 C61 -79.3(5) . . . . ? P1 Pd P2 C61 111.10(17) . . . . ? C1 Pd P2 C51 50.0(2) . . . . ? O2 Pd P2 C51 42.3(5) . . . . ? P1 Pd P2 C51 -127.30(18) . . . . ? C1 Pd P2 C21 168.3(2) . . . . ? O2 Pd P2 C21 160.5(5) . . . . ? P1 Pd P2 C21 -9.09(18) . . . . ? C1 Pd O2 C2 -86.5(4) . . . . ? P2 Pd O2 C2 -78.7(6) . . . . ? P1 Pd O2 C2 91.1(4) . . . . ? Pd O2 C2 O3 -6.0(10) . . . . ? Pd O2 C2 C3 176.1(3) . . . . ? O3 C2 C3 F1B -118.8(11) . . . . ? O2 C2 C3 F1B 59.4(11) . . . . ? O3 C2 C3 F2A 39.4(11) . . . . ? O2 C2 C3 F2A -142.4(8) . . . . ? O3 C2 C3 F3B 118.1(9) . . . . ? O2 C2 C3 F3B -63.8(9) . . . . ? O3 C2 C3 F3A 164.7(9) . . . . ? O2 C2 C3 F3A -17.1(9) . . . . ? O3 C2 C3 F2B 4.3(11) . . . . ? O2 C2 C3 F2B -177.5(8) . . . . ? O3 C2 C3 F1A -79.7(9) . . . . ? O2 C2 C3 F1A 98.5(7) . . . . ? C41 P1 C11 C16 -93.5(4) . . . . ? C31 P1 C11 C16 159.1(4) . . . . ? Pd P1 C11 C16 34.9(4) . . . . ? C41 P1 C11 C12 91.5(4) . . . . ? C31 P1 C11 C12 -15.9(5) . . . . ? Pd P1 C11 C12 -140.0(4) . . . . ? C16 C11 C12 C13 -2.8(7) . . . . ? P1 C11 C12 C13 172.4(4) . . . . ? C11 C12 C13 C14 -0.2(9) . . . . ? C12 C13 C14 C15 2.1(9) . . . . ? C13 C14 C15 C16 -0.8(9) . . . . ? C14 C15 C16 O1 -179.6(5) . . . . ? C14 C15 C16 C11 -2.4(8) . . . . ? C26 O1 C16 C15 -106.3(5) . . . . ? C26 O1 C16 C11 76.4(5) . . . . ? C12 C11 C16 C15 4.1(7) . . . . ? P1 C11 C16 C15 -171.1(4) . . . . ? C12 C11 C16 O1 -178.7(4) . . . . ? P1 C11 C16 O1 6.1(6) . . . . ? C61 P2 C21 C26 -63.7(4) . . . . ? C51 P2 C21 C26 -174.1(4) . . . . ? Pd P2 C21 C26 63.0(4) . . . . ? C61 P2 C21 C22 116.7(4) . . . . ? C51 P2 C21 C22 6.2(5) . . . . ? Pd P2 C21 C22 -116.7(4) . . . . ? C26 C21 C22 C23 0.0(7) . . . . ? P2 C21 C22 C23 179.6(4) . . . . ? C21 C22 C23 C24 -0.1(9) . . . . ? C22 C23 C24 C25 1.3(10) . . . . ? C23 C24 C25 C26 -2.5(9) . . . . ? C22 C21 C26 O1 -179.0(4) . . . . ? P2 C21 C26 O1 1.3(5) . . . . ? C22 C21 C26 C25 -1.2(7) . . . . ? P2 C21 C26 C25 179.1(4) . . . . ? C16 O1 C26 C21 -137.6(4) . . . . ? C16 O1 C26 C25 44.5(6) . . . . ? C24 C25 C26 C21 2.4(7) . . . . ? C24 C25 C26 O1 -179.9(5) . . . . ? C41 P1 C31 C36 178.3(4) . . . . ? C11 P1 C31 C36 -72.3(4) . . . . ? Pd P1 C31 C36 58.3(4) . . . . ? C41 P1 C31 C32 -6.0(6) . . . . ? C11 P1 C31 C32 103.5(5) . . . . ? Pd P1 C31 C32 -125.9(5) . . . . ? C36 C31 C32 C33 -0.2(10) . . . . ? P1 C31 C32 C33 -175.9(6) . . . . ? C31 C32 C33 C34 0.0(12) . . . . ? C32 C33 C34 C35 1.1(13) . . . . ? C33 C34 C35 C36 -1.9(12) . . . . ? C32 C31 C36 C35 -0.5(9) . . . . ? P1 C31 C36 C35 175.3(5) . . . . ? C34 C35 C36 C31 1.6(10) . . . . ? C31 P1 C41 C42 -78.4(5) . . . . ? C11 P1 C41 C42 177.4(4) . . . . ? Pd P1 C41 C42 42.7(5) . . . . ? C31 P1 C41 C46 101.4(4) . . . . ? C11 P1 C41 C46 -2.8(5) . . . . ? Pd P1 C41 C46 -137.5(4) . . . . ? C46 C41 C42 C43 -1.8(10) . . . . ? P1 C41 C42 C43 178.0(6) . . . . ? C41 C42 C43 C44 2.2(13) . . . . ? C42 C43 C44 C45 -0.8(14) . . . . ? C43 C44 C45 C46 -1.0(13) . . . . ? C42 C41 C46 C45 0.1(8) . . . . ? P1 C41 C46 C45 -179.7(5) . . . . ? C44 C45 C46 C41 1.3(10) . . . . ? C61 P2 C51 C56 -13.4(6) . . . . ? C21 P2 C51 C56 93.4(5) . . . . ? Pd P2 C51 C56 -139.6(5) . . . . ? C61 P2 C51 C52 167.0(4) . . . . ? C21 P2 C51 C52 -86.2(5) . . . . ? Pd P2 C51 C52 40.8(5) . . . . ? C56 C51 C52 C53 -0.1(9) . . . . ? P2 C51 C52 C53 179.5(5) . . . . ? C51 C52 C53 C54 1.3(11) . . . . ? C52 C53 C54 C55 -1.8(12) . . . . ? C53 C54 C55 C56 1.1(13) . . . . ? C54 C55 C56 C51 0.1(12) . . . . ? C52 C51 C56 C55 -0.5(10) . . . . ? P2 C51 C56 C55 179.8(6) . . . . ? C51 P2 C61 C66 69.3(5) . . . . ? C21 P2 C61 C66 -37.9(5) . . . . ? Pd P2 C61 C66 -166.5(4) . . . . ? C51 P2 C61 C62 -113.5(4) . . . . ? C21 P2 C61 C62 139.3(4) . . . . ? Pd P2 C61 C62 10.7(5) . . . . ? C66 C61 C62 C63 -1.2(8) . . . . ? P2 C61 C62 C63 -178.4(4) . . . . ? C61 C62 C63 C64 0.2(9) . . . . ? C62 C63 C64 C65 0.5(10) . . . . ? C63 C64 C65 C66 -0.2(10) . . . . ? C62 C61 C66 C65 1.5(9) . . . . ? P2 C61 C66 C65 178.7(5) . . . . ? C64 C65 C66 C61 -0.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 74.73 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.125 _refine_diff_density_min -2.418 _refine_diff_density_rms 0.130 #===END