# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1922 data_global _audit_creation_method SHELXL-97 # SUBMISSION DETAILS _publ_contact_author ; Dr Guy C. Lloyd-Jones School of Chemistry University of Bristol Bristol BS8 1TS UK ; _publ_contact_author_email Guy.Lloyd-Jones@bristol.ac.uk _publ_contact_author_fax '+44(0)117 929 8611' _publ_contact_author_phone '+44(0)117 928 8165' _publ_contact_letter ; Please consider this CIF submission for publication in J. Chem. Soc., Dalton Trans. ; _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' # TITLE AND AUTHOR LIST _publ_section_title ; Ligand Exchange and Stereodynamics in the Cationic Pd(II)-pi-allyl complex of 2,2'-Bis-Pyridyl-1,1'-Binaphthalene, a Novel Atropisomeric N,N-Ligand ; loop_ _publ_author_name _publ_author_address 'Jonathan P. H. Charmant' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'Ian A. Fallis' ; School of Chemistry, University of Wales at Cardiff PO Box 912 Cardiff CF10 3TB UK ; 'Neil J. Hunt' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'Guy C. Lloyd-Jones' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'Martin Murray' ; School of Chemistry University of Bristol Bristol BS8 1TS UK ; 'Thorsten Nowak' ; AstraZeneca Pharmaceuticals Mereside Alderley Park Macclesfield Cheshire SK10 4TG UK ; #===END (global) data_24 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H20 Cl2 N2 Zn' _chemical_formula_weight 544.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 18.6724(17) _cell_length_b 9.0454(9) _cell_length_c 15.9192(20) _cell_angle_alpha 90.00 _cell_angle_beta 110.510(9) _cell_angle_gamma 90.00 _cell_volume 2518.30(53) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 319 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.209 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.747 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details ; G. M. Sheldrick. SADABS: A program for absorption correction with the Siemens SMART system; University of G\"ottingen: Germany, 1996. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'frame exposures each covering 0.3 deg in \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 25226 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.43 _reflns_number_total 5741 _reflns_number_gt 4882 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V4' _computing_cell_refinement 'Bruker SMART V4' _computing_data_reduction 'Bruker SAINT V4' _computing_structure_solution 'Bruker SHELXTL V5' _computing_structure_refinement 'Bruker SHELXTL V5' _computing_molecular_graphics 'Bruker SHELXTL V5' _computing_publication_material 'Bruker SHELXTL V5' _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^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5741 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.003 _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 Zn Zn 0.715982(9) 0.540291(17) 0.285632(11) 0.02176(6) Uani 1 1 d . . . Cl1 Cl 0.80135(2) 0.68430(4) 0.25325(2) 0.02880(9) Uani 1 1 d . . . Cl2 Cl 0.60720(2) 0.48774(4) 0.17368(3) 0.03424(10) Uani 1 1 d . . . N1 N 0.77210(7) 0.34336(12) 0.32549(8) 0.0230(2) Uani 1 1 d . . . C2 C 0.82705(9) 0.30741(16) 0.29229(10) 0.0290(3) Uani 1 1 d . . . H2 H 0.8451 0.3803 0.2637 0.035 Uiso 1 1 calc R . . C3 C 0.85769(9) 0.16689(17) 0.29894(11) 0.0327(3) Uani 1 1 d . . . H3 H 0.8966 0.1464 0.2769 0.039 Uiso 1 1 calc R . . C4 C 0.82916(9) 0.05758(16) 0.33910(11) 0.0324(3) Uani 1 1 d . . . H4 H 0.8476 -0.0386 0.3431 0.039 Uiso 1 1 calc R . . C5 C 0.77277(9) 0.09335(16) 0.37321(10) 0.0284(3) Uani 1 1 d . . . H5 H 0.7527 0.0207 0.3999 0.034 Uiso 1 1 calc R . . C6 C 0.74604(8) 0.23811(15) 0.36766(9) 0.0218(3) Uani 1 1 d . . . C7 C 0.69060(8) 0.28159(14) 0.41187(9) 0.0218(3) Uani 1 1 d . . . C8 C 0.71364(7) 0.37402(14) 0.48600(9) 0.0199(3) Uani 1 1 d . . . C9 C 0.66380(8) 0.39995(15) 0.53527(9) 0.0223(3) Uani 1 1 d . . . C10 C 0.68588(9) 0.48673(16) 0.61470(10) 0.0274(3) Uani 1 1 d . . . H10 H 0.7341 0.5299 0.6357 0.033 Uiso 1 1 calc R . . C11 C 0.63677(10) 0.50767(18) 0.66096(11) 0.0349(4) Uani 1 1 d . . . H11 H 0.6518 0.5655 0.7125 0.042 Uiso 1 1 calc R . . C12 C 0.56353(10) 0.44154(19) 0.63029(11) 0.0370(4) Uani 1 1 d . . . H12 H 0.5307 0.4552 0.6621 0.044 Uiso 1 1 calc R . . C13 C 0.54078(9) 0.35799(18) 0.55446(11) 0.0331(4) Uani 1 1 d . . . H13 H 0.4922 0.3160 0.5347 0.040 Uiso 1 1 calc R . . C14 C 0.58980(8) 0.33390(15) 0.50501(10) 0.0256(3) Uani 1 1 d . . . C15 C 0.56703(8) 0.24607(16) 0.42612(10) 0.0297(3) Uani 1 1 d . . . H15 H 0.5181 0.2061 0.4047 0.036 Uiso 1 1 calc R . . C16 C 0.61616(8) 0.21944(15) 0.38121(10) 0.0270(3) Uani 1 1 d . . . H16 H 0.6007 0.1602 0.3302 0.032 Uiso 1 1 calc R . . N21 N 0.68303(7) 0.66093(12) 0.37491(8) 0.0227(2) Uani 1 1 d . . . C22 C 0.61715(8) 0.73735(15) 0.34089(10) 0.0274(3) Uani 1 1 d . . . H22 H 0.5853 0.7174 0.2824 0.033 Uiso 1 1 calc R . . C23 C 0.59476(9) 0.84382(16) 0.38882(11) 0.0322(4) Uani 1 1 d . . . H23 H 0.5486 0.8935 0.3634 0.039 Uiso 1 1 calc R . . C24 C 0.64215(10) 0.87490(17) 0.47497(11) 0.0366(4) Uani 1 1 d . . . H24 H 0.6288 0.9471 0.5084 0.044 Uiso 1 1 calc R . . C25 C 0.70991(10) 0.79739(16) 0.51126(10) 0.0320(4) Uani 1 1 d . . . H25 H 0.7427 0.8177 0.5692 0.038 Uiso 1 1 calc R . . C26 C 0.72883(8) 0.68843(15) 0.46045(9) 0.0235(3) Uani 1 1 d . . . C27 C 0.79842(8) 0.59490(16) 0.50106(9) 0.0242(3) Uani 1 1 d . . . C28 C 0.79129(8) 0.44537(15) 0.51602(9) 0.0215(3) Uani 1 1 d . . . C29 C 0.85817(8) 0.36006(16) 0.56264(9) 0.0254(3) Uani 1 1 d . . . C30 C 0.85417(9) 0.20911(17) 0.58550(10) 0.0305(3) Uani 1 1 d . . . H30 H 0.8069 0.1623 0.5685 0.037 Uiso 1 1 calc R . . C31 C 0.91909(10) 0.1314(2) 0.63235(11) 0.0402(4) Uani 1 1 d . . . H31 H 0.9155 0.0328 0.6469 0.048 Uiso 1 1 calc R . . C32 C 0.99122(10) 0.2012(2) 0.65839(13) 0.0497(5) Uani 1 1 d . . . H32 H 1.0350 0.1482 0.6901 0.060 Uiso 1 1 calc R . . C33 C 0.99704(10) 0.3448(2) 0.63745(12) 0.0479(5) Uani 1 1 d . . . H33 H 1.0451 0.3886 0.6545 0.057 Uiso 1 1 calc R . . C34 C 0.93140(9) 0.4298(2) 0.59002(11) 0.0350(4) Uani 1 1 d . . . C35 C 0.93599(9) 0.5817(2) 0.57044(12) 0.0426(4) Uani 1 1 d . . . H35 H 0.9836 0.6269 0.5862 0.051 Uiso 1 1 calc R . . C36 C 0.87179(9) 0.66238(18) 0.52889(11) 0.0363(4) Uani 1 1 d . . . H36 H 0.8760 0.7627 0.5186 0.044 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 Zn 0.02038(9) 0.02123(9) 0.02203(9) 0.00033(6) 0.00538(7) 0.00073(6) Cl1 0.02320(18) 0.02767(18) 0.0330(2) 0.00394(14) 0.00670(15) -0.00343(14) Cl2 0.02682(19) 0.0380(2) 0.0305(2) -0.00316(16) 0.00073(16) -0.00679(15) N1 0.0251(6) 0.0219(6) 0.0221(6) -0.0005(5) 0.0082(5) 0.0012(5) C2 0.0332(8) 0.0282(7) 0.0302(8) 0.0012(6) 0.0167(7) 0.0020(6) C3 0.0348(9) 0.0337(8) 0.0346(8) -0.0026(7) 0.0186(7) 0.0070(7) C4 0.0390(9) 0.0222(7) 0.0366(9) -0.0028(6) 0.0140(7) 0.0065(6) C5 0.0344(8) 0.0208(7) 0.0303(8) -0.0002(6) 0.0118(7) -0.0006(6) C6 0.0214(7) 0.0228(7) 0.0192(7) -0.0024(5) 0.0044(6) -0.0011(5) C7 0.0229(7) 0.0183(6) 0.0237(7) 0.0033(5) 0.0076(6) 0.0008(5) C8 0.0184(7) 0.0191(6) 0.0211(7) 0.0038(5) 0.0055(5) 0.0025(5) C9 0.0211(7) 0.0213(6) 0.0246(7) 0.0077(5) 0.0082(6) 0.0055(5) C10 0.0259(8) 0.0321(8) 0.0248(7) 0.0034(6) 0.0095(6) 0.0044(6) C11 0.0391(9) 0.0416(9) 0.0271(8) 0.0064(7) 0.0155(7) 0.0125(7) C12 0.0348(9) 0.0470(10) 0.0387(9) 0.0181(8) 0.0247(8) 0.0165(7) C13 0.0243(8) 0.0376(9) 0.0415(9) 0.0172(7) 0.0166(7) 0.0063(6) C14 0.0219(7) 0.0236(7) 0.0323(8) 0.0106(6) 0.0107(6) 0.0043(6) C15 0.0191(7) 0.0272(7) 0.0400(9) 0.0056(6) 0.0070(6) -0.0036(6) C16 0.0251(7) 0.0217(7) 0.0306(8) -0.0013(6) 0.0055(6) -0.0035(6) N21 0.0218(6) 0.0218(6) 0.0257(6) 0.0015(5) 0.0098(5) -0.0007(5) C22 0.0225(7) 0.0264(7) 0.0336(8) 0.0055(6) 0.0103(6) 0.0003(6) C23 0.0319(8) 0.0264(8) 0.0457(10) 0.0101(7) 0.0231(8) 0.0060(6) C24 0.0560(11) 0.0241(7) 0.0437(10) 0.0041(7) 0.0348(9) 0.0057(7) C25 0.0478(10) 0.0248(7) 0.0275(8) 0.0002(6) 0.0184(7) -0.0022(7) C26 0.0268(7) 0.0210(7) 0.0251(7) 0.0007(5) 0.0119(6) -0.0041(5) C27 0.0241(7) 0.0280(7) 0.0200(7) -0.0019(6) 0.0071(6) -0.0035(6) C28 0.0202(7) 0.0276(7) 0.0180(6) -0.0024(5) 0.0082(6) -0.0003(5) C29 0.0209(7) 0.0360(8) 0.0200(7) -0.0013(6) 0.0080(6) 0.0030(6) C30 0.0292(8) 0.0362(8) 0.0265(8) 0.0009(6) 0.0102(7) 0.0073(6) C31 0.0412(10) 0.0451(10) 0.0352(9) 0.0059(8) 0.0145(8) 0.0182(8) C32 0.0290(9) 0.0710(13) 0.0448(11) 0.0074(10) 0.0076(8) 0.0243(9) C33 0.0210(8) 0.0729(14) 0.0454(11) 0.0026(10) 0.0061(8) 0.0056(8) C34 0.0206(8) 0.0534(10) 0.0295(8) 0.0000(7) 0.0068(6) 0.0013(7) C35 0.0219(8) 0.0557(11) 0.0458(10) -0.0011(9) 0.0066(7) -0.0132(8) C36 0.0317(9) 0.0371(9) 0.0369(9) -0.0013(7) 0.0081(7) -0.0125(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Zn N21 2.0499(12) . ? Zn N1 2.0513(11) . ? Zn Cl2 2.2341(4) . ? Zn Cl1 2.2537(4) . ? N1 C2 1.3484(18) . ? N1 C6 1.3501(17) . ? C2 C3 1.383(2) . ? C3 C4 1.382(2) . ? C4 C5 1.382(2) . ? C5 C6 1.3931(19) . ? C6 C7 1.4940(19) . ? C7 C8 1.3859(18) . ? C7 C16 1.4180(19) . ? C8 C9 1.4310(19) . ? C8 C28 1.5039(18) . ? C9 C10 1.421(2) . ? C9 C14 1.4253(19) . ? C10 C11 1.375(2) . ? C11 C12 1.414(2) . ? C12 C13 1.360(2) . ? C13 C14 1.418(2) . ? C14 C15 1.420(2) . ? C15 C16 1.368(2) . ? N21 C22 1.3480(18) . ? N21 C26 1.3534(18) . ? C22 C23 1.381(2) . ? C23 C24 1.376(2) . ? C24 C25 1.383(2) . ? C25 C26 1.397(2) . ? C26 C27 1.495(2) . ? C27 C28 1.388(2) . ? C27 C36 1.421(2) . ? C28 C29 1.4341(19) . ? C29 C30 1.422(2) . ? C29 C34 1.428(2) . ? C30 C31 1.373(2) . ? C31 C32 1.412(3) . ? C32 C33 1.355(3) . ? C33 C34 1.419(2) . ? C34 C35 1.418(2) . ? C35 C36 1.361(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N21 Zn N1 119.52(5) . . ? N21 Zn Cl2 104.86(3) . . ? N1 Zn Cl2 106.56(3) . . ? N21 Zn Cl1 105.01(3) . . ? N1 Zn Cl1 104.30(3) . . ? Cl2 Zn Cl1 117.306(15) . . ? C2 N1 C6 118.77(12) . . ? C2 N1 Zn 117.68(9) . . ? C6 N1 Zn 122.15(9) . . ? N1 C2 C3 122.88(14) . . ? C4 C3 C2 118.50(15) . . ? C3 C4 C5 118.99(14) . . ? C4 C5 C6 120.05(14) . . ? N1 C6 C5 120.71(13) . . ? N1 C6 C7 118.59(12) . . ? C5 C6 C7 120.64(13) . . ? C8 C7 C16 120.44(13) . . ? C8 C7 C6 120.02(12) . . ? C16 C7 C6 119.40(12) . . ? C7 C8 C9 119.87(12) . . ? C7 C8 C28 120.43(12) . . ? C9 C8 C28 119.69(12) . . ? C10 C9 C14 118.48(13) . . ? C10 C9 C8 122.45(13) . . ? C14 C9 C8 119.06(13) . . ? C11 C10 C9 120.82(15) . . ? C10 C11 C12 120.17(16) . . ? C13 C12 C11 120.35(15) . . ? C12 C13 C14 121.10(15) . . ? C13 C14 C15 121.72(14) . . ? C13 C14 C9 119.08(14) . . ? C15 C14 C9 119.21(13) . . ? C16 C15 C14 120.88(13) . . ? C15 C16 C7 120.42(14) . . ? C22 N21 C26 118.42(12) . . ? C22 N21 Zn 116.60(10) . . ? C26 N21 Zn 123.93(9) . . ? N21 C22 C23 123.08(14) . . ? C24 C23 C22 118.66(14) . . ? C23 C24 C25 119.17(14) . . ? C24 C25 C26 119.72(15) . . ? N21 C26 C25 120.90(13) . . ? N21 C26 C27 118.57(12) . . ? C25 C26 C27 120.47(13) . . ? C28 C27 C36 120.33(14) . . ? C28 C27 C26 120.31(12) . . ? C36 C27 C26 119.25(13) . . ? C27 C28 C29 119.65(13) . . ? C27 C28 C8 120.23(12) . . ? C29 C28 C8 120.09(12) . . ? C30 C29 C34 118.46(14) . . ? C30 C29 C28 122.34(13) . . ? C34 C29 C28 119.17(14) . . ? C31 C30 C29 120.98(16) . . ? C30 C31 C32 120.04(17) . . ? C33 C32 C31 120.46(16) . . ? C32 C33 C34 121.41(17) . . ? C35 C34 C33 122.29(16) . . ? C35 C34 C29 119.07(14) . . ? C33 C34 C29 118.63(16) . . ? C36 C35 C34 121.04(15) . . ? C35 C36 C27 120.66(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.270 _refine_diff_density_min -0.305 _refine_diff_density_rms 0.043 #===END (data for 24) data_25 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H50 F6 N4 O6 Pd2 S2' _chemical_formula_weight 1410.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 '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' 'O' 'O' 0.0106 0.0060 '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 'Triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.766(3) _cell_length_b 15.359(4) _cell_length_c 18.607(4) _cell_angle_alpha 89.95(2) _cell_angle_beta 80.42(2) _cell_angle_gamma 85.26(2) _cell_volume 3023.1(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 98 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_process_details ; G.M. Sheldrick. SADABS: A program for absorption correction with the Siemens SMART system; University of G\"ottingen: Germany, 1996. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART' _diffrn_measurement_method 'Frames, each covering 0.3 deg. in \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 25936 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10584 _reflns_number_gt 8225 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART v4' _computing_cell_refinement 'Bruker SMART v4' _computing_data_reduction 'Bruker SAINT v4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL v5' _computing_publication_material 'Bruker SHELXTL v5' _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^)+(0.0458P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00096(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10584 _refine_ls_number_parameters 794 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0783 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.05163(2) 0.079973(15) 0.823731(12) 0.02470(8) Uani 1 1 d . . . C1 C 0.1936(3) 0.0320(2) 0.7353(2) 0.0469(10) Uani 1 1 d . . . H1A H 0.1567 0.0868 0.7221 0.056 Uiso 1 1 calc R . . H1B H 0.2827 0.0227 0.7321 0.056 Uiso 1 1 calc R . . C2 C 0.1193(4) -0.0328(3) 0.7585(2) 0.0651(12) Uani 1 1 d . . . H2 H 0.1585 -0.0870 0.7713 0.078 Uiso 1 1 calc R . . C3 C -0.0081(3) -0.0242(2) 0.76435(18) 0.0384(8) Uani 1 1 d . . . H3A H -0.0496 0.0293 0.7519 0.046 Uiso 1 1 calc R . . H3B H -0.0561 -0.0717 0.7809 0.046 Uiso 1 1 calc R . . N4 N -0.1223(2) 0.10180(16) 0.90119(13) 0.0262(6) Uani 1 1 d . . . C5 C -0.2264(3) 0.0727(2) 0.88040(17) 0.0310(7) Uani 1 1 d . . . H5 H -0.2247 0.0618 0.8300 0.037 Uiso 1 1 calc R . . C6 C -0.3346(3) 0.0579(2) 0.92801(19) 0.0388(8) Uani 1 1 d . . . H6 H -0.4063 0.0392 0.9107 0.047 Uiso 1 1 calc R . . C7 C -0.3365(3) 0.0708(2) 1.00123(19) 0.0439(9) Uani 1 1 d . . . H7 H -0.4076 0.0577 1.0359 0.053 Uiso 1 1 calc R . . C8 C -0.2335(3) 0.1031(2) 1.02334(18) 0.0373(8) Uani 1 1 d . . . H8 H -0.2341 0.1136 1.0737 0.045 Uiso 1 1 calc R . . C9 C -0.1289(3) 0.12054(19) 0.97313(16) 0.0268(7) Uani 1 1 d . . . C10 C -0.0266(3) 0.16612(19) 0.99790(15) 0.0255(7) Uani 1 1 d . . . C11 C 0.0426(3) 0.1256(2) 1.04906(17) 0.0332(8) Uani 1 1 d . . . H11 H 0.0268 0.0681 1.0648 0.040 Uiso 1 1 calc R . . C12 C 0.1316(3) 0.1680(2) 1.07586(17) 0.0362(8) Uani 1 1 d . . . H12 H 0.1811 0.1385 1.1076 0.043 Uiso 1 1 calc R . . C13 C 0.1512(3) 0.2559(2) 1.05683(16) 0.0279(7) Uani 1 1 d . . . C14 C 0.2388(3) 0.3032(2) 1.08755(18) 0.0375(8) Uani 1 1 d . . . H14 H 0.2883 0.2747 1.1198 0.045 Uiso 1 1 calc R . . C15 C 0.2522(3) 0.3886(2) 1.07121(18) 0.0385(8) Uani 1 1 d . . . H15 H 0.3099 0.4195 1.0926 0.046 Uiso 1 1 calc R . . C16 C 0.1812(3) 0.4311(2) 1.02293(18) 0.0350(8) Uani 1 1 d . . . H16 H 0.1908 0.4908 1.0121 0.042 Uiso 1 1 calc R . . C17 C 0.0985(3) 0.3875(2) 0.99129(17) 0.0290(7) Uani 1 1 d . . . H17 H 0.0521 0.4172 0.9582 0.035 Uiso 1 1 calc R . . C18 C 0.0806(3) 0.29795(19) 1.00700(15) 0.0233(6) Uani 1 1 d . . . C19 C -0.0054(3) 0.25040(19) 0.97528(15) 0.0229(6) Uani 1 1 d . . . C20 C -0.0662(3) 0.29017(18) 0.91462(15) 0.0224(6) Uani 1 1 d . . . C21 C -0.1947(3) 0.32546(19) 0.92571(16) 0.0239(7) Uani 1 1 d . . . C22 C -0.2758(3) 0.3224(2) 0.99421(17) 0.0298(7) Uani 1 1 d . . . H22 H -0.2438 0.2972 1.0348 0.036 Uiso 1 1 calc R . . C23 C -0.3991(3) 0.3554(2) 1.00215(19) 0.0380(8) Uani 1 1 d . . . H23 H -0.4526 0.3515 1.0479 0.046 Uiso 1 1 calc R . . C24 C -0.4478(3) 0.3949(2) 0.9436(2) 0.0407(9) Uani 1 1 d . . . H24 H -0.5338 0.4176 0.9499 0.049 Uiso 1 1 calc R . . C25 C -0.3723(3) 0.4008(2) 0.87802(19) 0.0363(8) Uani 1 1 d . . . H25 H -0.4058 0.4286 0.8390 0.044 Uiso 1 1 calc R . . C26 C -0.2443(3) 0.36627(19) 0.86675(17) 0.0274(7) Uani 1 1 d . . . C27 C -0.1648(3) 0.3720(2) 0.79849(17) 0.0329(8) Uani 1 1 d . . . H27 H -0.1974 0.3996 0.7590 0.039 Uiso 1 1 calc R . . C28 C -0.0417(3) 0.3381(2) 0.78891(17) 0.0327(8) Uani 1 1 d . . . H28 H 0.0108 0.3431 0.7430 0.039 Uiso 1 1 calc R . . C29 C 0.0082(3) 0.29601(18) 0.84635(15) 0.0238(7) Uani 1 1 d . . . C30 C 0.1428(3) 0.2630(2) 0.83820(15) 0.0272(7) Uani 1 1 d . . . C31 C 0.2382(3) 0.3194(2) 0.82442(17) 0.0349(8) Uani 1 1 d . . . H31 H 0.2196 0.3778 0.8104 0.042 Uiso 1 1 calc R . . C32 C 0.3604(3) 0.2898(3) 0.83132(19) 0.0429(9) Uani 1 1 d . . . H32 H 0.4266 0.3276 0.8223 0.052 Uiso 1 1 calc R . . C33 C 0.3846(3) 0.2053(3) 0.85133(19) 0.0424(9) Uani 1 1 d . . . H33 H 0.4662 0.1849 0.8604 0.051 Uiso 1 1 calc R . . C34 C 0.2887(3) 0.1498(2) 0.85812(18) 0.0381(8) Uani 1 1 d . . . H34 H 0.3079 0.0902 0.8688 0.046 Uiso 1 1 calc R . . N35 N 0.1695(2) 0.17635(16) 0.85036(13) 0.0281(6) Uani 1 1 d . . . Pd2 Pd 0.05312(2) -0.671675(16) 0.363134(13) 0.03255(9) Uani 1 1 d . . . C36 C 0.1748(4) -0.6100(3) 0.27874(18) 0.0523(10) Uani 1 1 d . . . H36A H 0.2183 -0.6636 0.2892 0.063 Uiso 1 1 calc R . . H36B H 0.2135 -0.5568 0.2806 0.063 Uiso 1 1 calc R . . C37 C 0.0548(5) -0.6093(3) 0.2607(2) 0.0695(14) Uani 1 1 d . . . H37 H 0.0103 -0.5561 0.2501 0.083 Uiso 1 1 calc R . . C38 C 0.0012(4) -0.6885(3) 0.25849(19) 0.0619(12) Uani 1 1 d . . . H38A H 0.0467 -0.7413 0.2692 0.074 Uiso 1 1 calc R . . H38B H -0.0809 -0.6899 0.2463 0.074 Uiso 1 1 calc R . . N39 N -0.0986(2) -0.74642(19) 0.41218(14) 0.0352(7) Uani 1 1 d . . . C40 C -0.2146(3) -0.7250(3) 0.39670(19) 0.0481(10) Uani 1 1 d . . . H40 H -0.2353 -0.6670 0.3824 0.058 Uiso 1 1 calc R . . C41 C -0.3047(4) -0.7845(3) 0.4009(2) 0.0623(12) Uani 1 1 d . . . H41 H -0.3869 -0.7668 0.3913 0.075 Uiso 1 1 calc R . . C42 C -0.2751(4) -0.8694(3) 0.4191(2) 0.0564(11) Uani 1 1 d . . . H42 H -0.3338 -0.9122 0.4184 0.068 Uiso 1 1 calc R . . C43 C -0.1572(3) -0.8917(2) 0.43877(19) 0.0424(9) Uani 1 1 d . . . H43 H -0.1354 -0.9493 0.4538 0.051 Uiso 1 1 calc R . . C44 C -0.0718(3) -0.8279(2) 0.43598(16) 0.0309(7) Uani 1 1 d . . . C45 C 0.0522(3) -0.84569(19) 0.46059(16) 0.0258(7) Uani 1 1 d . . . C46 C 0.1472(3) -0.9026(2) 0.41934(17) 0.0332(8) Uani 1 1 d . . . H46 H 0.1303 -0.9313 0.3772 0.040 Uiso 1 1 calc R . . C47 C 0.2626(3) -0.9165(2) 0.43961(19) 0.0382(8) Uani 1 1 d . . . H47 H 0.3269 -0.9534 0.4106 0.046 Uiso 1 1 calc R . . C48 C 0.2879(3) -0.8768(2) 0.50359(18) 0.0318(7) Uani 1 1 d . . . C49 C 0.4077(3) -0.8894(3) 0.5251(2) 0.0506(10) Uani 1 1 d . . . H49 H 0.4724 -0.9264 0.4966 0.061 Uiso 1 1 calc R . . C50 C 0.4322(4) -0.8494(3) 0.5858(2) 0.0602(12) Uani 1 1 d . . . H50 H 0.5139 -0.8581 0.5989 0.072 Uiso 1 1 calc R . . C51 C 0.3376(3) -0.7956(3) 0.6290(2) 0.0501(10) Uani 1 1 d . . . H51 H 0.3548 -0.7691 0.6720 0.060 Uiso 1 1 calc R . . C52 C 0.2209(3) -0.7810(2) 0.60986(17) 0.0344(8) Uani 1 1 d . . . H52 H 0.1576 -0.7440 0.6395 0.041 Uiso 1 1 calc R . . C53 C 0.1929(3) -0.82024(19) 0.54634(16) 0.0257(7) Uani 1 1 d . . . C54 C 0.0738(3) -0.80431(18) 0.52287(15) 0.0229(6) Uani 1 1 d . . . C55 C -0.0269(3) -0.73914(19) 0.56130(15) 0.0234(6) Uani 1 1 d . . . C56 C -0.1372(3) -0.76864(19) 0.60567(15) 0.0232(6) Uani 1 1 d . . . C57 C -0.1467(3) -0.85776(19) 0.62373(16) 0.0256(7) Uani 1 1 d . . . H57 H -0.0806 -0.9000 0.6038 0.031 Uiso 1 1 calc R . . C58 C -0.2497(3) -0.8838(2) 0.66939(16) 0.0292(7) Uani 1 1 d . . . H58 H -0.2542 -0.9437 0.6814 0.035 Uiso 1 1 calc R . . C59 C -0.3492(3) -0.8217(2) 0.69862(17) 0.0317(8) Uani 1 1 d . . . H59 H -0.4202 -0.8401 0.7306 0.038 Uiso 1 1 calc R . . C60 C -0.3445(3) -0.7358(2) 0.68157(17) 0.0312(7) Uani 1 1 d . . . H60 H -0.4130 -0.6950 0.7009 0.037 Uiso 1 1 calc R . . C61 C -0.2377(3) -0.7064(2) 0.63492(15) 0.0259(7) Uani 1 1 d . . . C62 C -0.2274(3) -0.6172(2) 0.62002(16) 0.0299(7) Uani 1 1 d . . . H62 H -0.2968 -0.5758 0.6366 0.036 Uiso 1 1 calc R . . C63 C -0.1185(3) -0.5895(2) 0.58198(16) 0.0294(7) Uani 1 1 d . . . H63 H -0.1108 -0.5287 0.5754 0.035 Uiso 1 1 calc R . . C64 C -0.0167(3) -0.65037(19) 0.55223(15) 0.0254(7) Uani 1 1 d . . . C65 C 0.1070(3) -0.61875(19) 0.51836(16) 0.0280(7) Uani 1 1 d . . . C66 C 0.1713(3) -0.5718(2) 0.56130(18) 0.0392(8) Uani 1 1 d . . . H66 H 0.1308 -0.5518 0.6084 0.047 Uiso 1 1 calc R . . C67 C 0.2943(3) -0.5538(3) 0.53590(19) 0.0484(10) Uani 1 1 d . . . H67 H 0.3388 -0.5202 0.5644 0.058 Uiso 1 1 calc R . . C68 C 0.3506(3) -0.5856(2) 0.4684(2) 0.0444(9) Uani 1 1 d . . . H68 H 0.4371 -0.5783 0.4510 0.053 Uiso 1 1 calc R . . C69 C 0.2809(3) -0.6280(2) 0.42648(18) 0.0348(8) Uani 1 1 d . . . H69 H 0.3207 -0.6481 0.3793 0.042 Uiso 1 1 calc R . . N70 N 0.1577(2) -0.64288(16) 0.44875(13) 0.0279(6) Uani 1 1 d . . . C71 C 0.4979(4) -0.8250(3) 0.2351(3) 0.0653(13) Uani 1 1 d . . . F71A F 0.4364(3) -0.7808(2) 0.2904(2) 0.1245(15) Uani 1 1 d . . . F71B F 0.4761(3) -0.78340(19) 0.1733(2) 0.1215(14) Uani 1 1 d . . . F71C F 0.6206(2) -0.82283(16) 0.23590(16) 0.0758(8) Uani 1 1 d . . . S72 S 0.45467(8) -0.93555(6) 0.23142(5) 0.0382(2) Uani 1 1 d . . . O72A O 0.4901(3) -0.9712(2) 0.29780(15) 0.0678(9) Uani 1 1 d . . . O72B O 0.5328(2) -0.97105(18) 0.16744(14) 0.0585(8) Uani 1 1 d . . . O72C O 0.3213(2) -0.92572(18) 0.23048(15) 0.0538(7) Uani 1 1 d . . . C73 C 0.3653(4) 0.5761(2) 0.8053(2) 0.0465(9) Uani 1 1 d . . . F73A F 0.4800(2) 0.59793(16) 0.81534(14) 0.0719(7) Uani 1 1 d . . . F73B F 0.2903(2) 0.64951(15) 0.81386(12) 0.0660(7) Uani 1 1 d . . . F73C F 0.3256(2) 0.52275(15) 0.85865(11) 0.0622(7) Uani 1 1 d . . . S74 S 0.37425(9) 0.52588(6) 0.71676(5) 0.0434(2) Uani 1 1 d . . . O74A O 0.4171(3) 0.59182(19) 0.66668(14) 0.0616(8) Uani 1 1 d . . . O74B O 0.2440(2) 0.5078(2) 0.71603(15) 0.0624(8) Uani 1 1 d . . . O74C O 0.4587(3) 0.45044(18) 0.71961(15) 0.0637(8) 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 0.02722(13) 0.02263(14) 0.02402(14) 0.00061(10) -0.00318(10) -0.00298(9) C1 0.044(2) 0.036(2) 0.054(2) -0.0147(18) 0.0116(18) -0.0008(17) C2 0.075(3) 0.054(3) 0.062(3) -0.030(2) 0.001(2) -0.001(2) C3 0.047(2) 0.0265(19) 0.040(2) -0.0107(15) -0.0004(17) -0.0063(15) N4 0.0317(14) 0.0208(14) 0.0268(14) 0.0020(11) -0.0047(11) -0.0060(11) C5 0.0349(18) 0.0311(18) 0.0289(17) -0.0020(14) -0.0069(14) -0.0102(14) C6 0.0348(19) 0.039(2) 0.043(2) -0.0040(16) -0.0034(16) -0.0163(15) C7 0.046(2) 0.043(2) 0.040(2) 0.0005(17) 0.0076(17) -0.0188(17) C8 0.048(2) 0.035(2) 0.0261(18) -0.0005(15) 0.0051(16) -0.0153(16) C9 0.0377(18) 0.0174(16) 0.0252(17) 0.0022(13) -0.0051(14) -0.0030(13) C10 0.0297(16) 0.0254(17) 0.0204(15) 0.0005(13) -0.0004(13) -0.0030(13) C11 0.045(2) 0.0276(18) 0.0271(17) 0.0085(14) -0.0075(15) -0.0034(15) C12 0.0406(19) 0.041(2) 0.0283(18) 0.0040(15) -0.0135(15) 0.0043(16) C13 0.0260(16) 0.0349(19) 0.0229(16) -0.0042(14) -0.0047(13) -0.0011(13) C14 0.0307(18) 0.052(2) 0.0312(19) -0.0052(16) -0.0107(15) -0.0005(16) C15 0.0302(18) 0.048(2) 0.039(2) -0.0135(17) -0.0071(15) -0.0127(16) C16 0.0345(18) 0.0319(19) 0.0385(19) -0.0080(15) -0.0026(15) -0.0099(15) C17 0.0296(16) 0.0274(18) 0.0293(17) -0.0016(14) -0.0040(14) -0.0003(13) C18 0.0233(15) 0.0249(17) 0.0206(15) -0.0027(13) -0.0002(12) -0.0020(12) C19 0.0234(15) 0.0259(17) 0.0183(15) 0.0010(12) -0.0014(12) 0.0008(12) C20 0.0284(16) 0.0164(15) 0.0238(16) -0.0001(12) -0.0072(13) -0.0051(12) C21 0.0277(16) 0.0212(16) 0.0251(16) -0.0013(13) -0.0099(13) -0.0052(12) C22 0.0299(17) 0.0319(18) 0.0277(17) -0.0009(14) -0.0047(14) -0.0033(14) C23 0.0286(18) 0.046(2) 0.038(2) -0.0055(17) -0.0024(15) -0.0007(15) C24 0.0282(18) 0.043(2) 0.052(2) -0.0075(18) -0.0128(17) 0.0032(15) C25 0.0369(19) 0.0310(19) 0.046(2) 0.0010(16) -0.0223(17) -0.0009(15) C26 0.0318(17) 0.0216(17) 0.0311(17) -0.0011(13) -0.0117(14) -0.0036(13) C27 0.047(2) 0.0266(18) 0.0296(18) 0.0053(14) -0.0175(15) -0.0051(15) C28 0.047(2) 0.0276(18) 0.0228(17) 0.0045(14) -0.0017(15) -0.0071(15) C29 0.0302(16) 0.0190(16) 0.0222(16) -0.0011(12) -0.0025(13) -0.0056(12) C30 0.0348(17) 0.0270(18) 0.0197(16) -0.0015(13) -0.0007(13) -0.0098(14) C31 0.0375(19) 0.0325(19) 0.0329(18) -0.0025(15) 0.0042(15) -0.0126(15) C32 0.0345(19) 0.054(3) 0.040(2) -0.0114(18) 0.0036(16) -0.0200(17) C33 0.0232(17) 0.064(3) 0.039(2) -0.0101(19) -0.0024(15) -0.0047(17) C34 0.0361(19) 0.040(2) 0.037(2) -0.0041(16) -0.0058(16) 0.0015(16) N35 0.0251(13) 0.0293(15) 0.0294(14) -0.0026(12) -0.0036(11) -0.0012(11) Pd2 0.04390(16) 0.03063(16) 0.02119(14) 0.00087(11) -0.00241(11) 0.00209(11) C36 0.075(3) 0.052(3) 0.028(2) 0.0181(18) -0.004(2) -0.007(2) C37 0.097(4) 0.081(4) 0.026(2) 0.021(2) -0.003(2) 0.002(3) C38 0.082(3) 0.081(3) 0.027(2) 0.009(2) -0.020(2) -0.010(3) N39 0.0360(15) 0.0425(18) 0.0263(15) -0.0014(13) -0.0056(12) 0.0033(13) C40 0.042(2) 0.063(3) 0.039(2) 0.0001(19) -0.0138(17) 0.0115(19) C41 0.033(2) 0.102(4) 0.053(3) -0.004(3) -0.0131(19) -0.001(2) C42 0.042(2) 0.080(3) 0.049(2) -0.008(2) -0.0012(19) -0.022(2) C43 0.042(2) 0.047(2) 0.038(2) -0.0055(17) -0.0007(17) -0.0099(17) C44 0.0327(17) 0.037(2) 0.0220(16) -0.0059(14) -0.0018(14) -0.0005(14) C45 0.0313(16) 0.0204(16) 0.0242(16) 0.0031(13) 0.0010(13) -0.0048(13) C46 0.0400(19) 0.0288(18) 0.0275(17) -0.0074(14) 0.0026(15) 0.0002(15) C47 0.040(2) 0.0264(18) 0.042(2) -0.0083(15) 0.0067(16) 0.0067(15) C48 0.0270(17) 0.0287(18) 0.0381(19) 0.0006(15) -0.0018(14) 0.0000(13) C49 0.036(2) 0.051(2) 0.060(3) -0.003(2) -0.0028(19) 0.0097(17) C50 0.034(2) 0.077(3) 0.073(3) -0.005(2) -0.023(2) 0.007(2) C51 0.047(2) 0.066(3) 0.041(2) -0.0053(19) -0.0178(18) -0.002(2) C52 0.0335(18) 0.040(2) 0.0297(18) 0.0049(15) -0.0061(15) -0.0002(15) C53 0.0306(16) 0.0205(16) 0.0238(16) 0.0058(13) 0.0008(13) -0.0004(13) C54 0.0273(16) 0.0201(16) 0.0191(15) 0.0043(12) 0.0018(12) -0.0007(12) C55 0.0283(16) 0.0255(17) 0.0158(15) 0.0005(12) -0.0033(12) 0.0003(13) C56 0.0274(16) 0.0253(17) 0.0167(15) -0.0002(12) -0.0052(12) 0.0015(12) C57 0.0243(15) 0.0253(17) 0.0259(16) -0.0009(13) -0.0017(13) 0.0012(13) C58 0.0325(17) 0.0258(17) 0.0290(17) -0.0004(14) -0.0034(14) -0.0039(13) C59 0.0271(17) 0.036(2) 0.0300(18) -0.0013(15) 0.0028(14) -0.0048(14) C60 0.0242(16) 0.0343(19) 0.0332(18) -0.0056(15) -0.0012(14) 0.0022(13) C61 0.0276(16) 0.0299(18) 0.0199(15) -0.0012(13) -0.0043(13) 0.0012(13) C62 0.0358(18) 0.0262(18) 0.0244(16) -0.0031(13) -0.0011(14) 0.0094(14) C63 0.0435(19) 0.0218(17) 0.0211(16) 0.0006(13) -0.0031(14) 0.0030(14) C64 0.0346(17) 0.0239(17) 0.0171(15) 0.0020(12) -0.0034(13) -0.0001(13) C65 0.0368(18) 0.0209(17) 0.0249(16) 0.0044(13) -0.0020(14) -0.0013(13) C66 0.049(2) 0.040(2) 0.0283(18) -0.0006(15) -0.0009(16) -0.0135(17) C67 0.052(2) 0.059(3) 0.036(2) 0.0003(18) -0.0035(18) -0.025(2) C68 0.037(2) 0.052(2) 0.044(2) 0.0053(18) 0.0002(17) -0.0136(17) C69 0.0377(19) 0.0316(19) 0.0310(18) 0.0035(15) 0.0047(15) -0.0008(15) N70 0.0359(15) 0.0220(14) 0.0229(13) 0.0021(11) 0.0021(11) 0.0005(11) C71 0.049(2) 0.040(2) 0.117(4) -0.007(3) -0.043(3) -0.0005(19) F71A 0.084(2) 0.081(2) 0.210(4) -0.103(3) -0.046(2) 0.0239(17) F71B 0.118(2) 0.070(2) 0.207(4) 0.075(2) -0.103(3) -0.0340(18) F71C 0.0558(15) 0.0555(16) 0.129(2) 0.0091(15) -0.0463(15) -0.0196(12) S72 0.0383(5) 0.0333(5) 0.0402(5) -0.0053(4) 0.0037(4) -0.0073(4) O72A 0.0553(17) 0.090(2) 0.0506(17) 0.0339(16) 0.0053(14) 0.0119(16) O72B 0.0553(16) 0.0653(19) 0.0498(16) -0.0203(14) 0.0042(14) -0.0017(14) O72C 0.0402(14) 0.0580(18) 0.0650(18) -0.0042(14) -0.0101(13) -0.0117(12) C73 0.061(3) 0.038(2) 0.042(2) 0.0054(18) -0.0121(19) -0.0031(19) F73A 0.0779(17) 0.0680(17) 0.0808(18) 0.0053(14) -0.0357(14) -0.0258(14) F73B 0.0889(17) 0.0449(14) 0.0585(15) -0.0137(11) -0.0048(13) 0.0119(13) F73C 0.1023(19) 0.0550(15) 0.0312(11) 0.0068(10) -0.0060(12) -0.0275(13) S74 0.0538(6) 0.0441(6) 0.0286(5) 0.0007(4) -0.0028(4) 0.0098(4) O74A 0.0745(19) 0.0666(19) 0.0374(15) 0.0222(14) 0.0032(14) 0.0063(15) O74B 0.0516(16) 0.082(2) 0.0570(18) -0.0134(15) -0.0188(14) -0.0046(15) O74C 0.0744(19) 0.0536(18) 0.0564(17) -0.0045(14) -0.0090(15) 0.0302(15) _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 C2 2.123(4) . ? Pd1 N35 2.137(3) . ? Pd1 C1 2.137(3) . ? Pd1 C3 2.146(3) . ? Pd1 N4 2.167(2) . ? C1 C2 1.354(5) . ? C2 C3 1.353(5) . ? N4 C5 1.355(4) . ? N4 C9 1.359(4) . ? C5 C6 1.376(4) . ? C6 C7 1.373(5) . ? C7 C8 1.374(5) . ? C8 C9 1.383(4) . ? C9 C10 1.487(4) . ? C10 C19 1.386(4) . ? C10 C11 1.417(4) . ? C11 C12 1.361(5) . ? C12 C13 1.420(5) . ? C13 C18 1.416(4) . ? C13 C14 1.427(4) . ? C14 C15 1.360(5) . ? C15 C16 1.400(5) . ? C16 C17 1.364(4) . ? C17 C18 1.428(4) . ? C18 C19 1.426(4) . ? C19 C20 1.501(4) . ? C20 C29 1.392(4) . ? C20 C21 1.425(4) . ? C21 C26 1.421(4) . ? C21 C22 1.423(4) . ? C22 C23 1.366(4) . ? C23 C24 1.401(5) . ? C24 C25 1.357(5) . ? C25 C26 1.417(4) . ? C26 C27 1.415(4) . ? C27 C28 1.366(4) . ? C28 C29 1.408(4) . ? C29 C30 1.478(4) . ? C30 N35 1.365(4) . ? C30 C31 1.389(4) . ? C31 C32 1.383(5) . ? C32 C33 1.366(5) . ? C33 C34 1.382(5) . ? C34 N35 1.345(4) . ? Pd2 C37 2.131(4) . ? Pd2 C38 2.135(4) . ? Pd2 C36 2.144(4) . ? Pd2 N39 2.152(3) . ? Pd2 N70 2.164(3) . ? C36 C37 1.387(6) . ? C37 C38 1.393(6) . ? N39 C40 1.342(4) . ? N39 C44 1.352(4) . ? C40 C41 1.380(6) . ? C41 C42 1.372(6) . ? C42 C43 1.395(5) . ? C43 C44 1.392(5) . ? C44 C45 1.487(4) . ? C45 C54 1.384(4) . ? C45 C46 1.411(4) . ? C46 C47 1.357(5) . ? C47 C48 1.415(5) . ? C48 C49 1.411(5) . ? C48 C53 1.420(4) . ? C49 C50 1.359(6) . ? C50 C51 1.399(5) . ? C51 C52 1.364(5) . ? C52 C53 1.414(4) . ? C53 C54 1.425(4) . ? C54 C55 1.501(4) . ? C55 C64 1.385(4) . ? C55 C56 1.435(4) . ? C56 C57 1.417(4) . ? C56 C61 1.419(4) . ? C57 C58 1.368(4) . ? C58 C59 1.411(4) . ? C59 C60 1.360(4) . ? C60 C61 1.425(4) . ? C61 C62 1.409(4) . ? C62 C63 1.364(4) . ? C63 C64 1.419(4) . ? C64 C65 1.495(4) . ? C65 N70 1.358(4) . ? C65 C66 1.380(5) . ? C66 C67 1.381(5) . ? C67 C68 1.372(5) . ? C68 C69 1.368(5) . ? C69 N70 1.361(4) . ? C71 F71A 1.288(5) . ? C71 F71C 1.326(4) . ? C71 F71B 1.359(6) . ? C71 S72 1.802(4) . ? S72 O72B 1.419(3) . ? S72 O72C 1.434(3) . ? S72 O72A 1.446(3) . ? C73 F73B 1.324(4) . ? C73 F73C 1.325(4) . ? C73 F73A 1.348(4) . ? C73 S74 1.804(4) . ? S74 O74C 1.419(3) . ? S74 O74A 1.428(3) . ? S74 O74B 1.454(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 C2 Pd1 N35 123.92(14) . . ? C2 Pd1 C1 37.06(14) . . ? N35 Pd1 C1 91.01(12) . . ? C2 Pd1 C3 36.97(14) . . ? N35 Pd1 C3 158.50(11) . . ? C1 Pd1 C3 67.58(13) . . ? C2 Pd1 N4 128.39(14) . . ? N35 Pd1 N4 105.12(9) . . ? C1 Pd1 N4 163.82(12) . . ? C3 Pd1 N4 96.26(11) . . ? C2 C1 Pd1 70.9(2) . . ? C3 C2 C1 123.2(4) . . ? C3 C2 Pd1 72.4(2) . . ? C1 C2 Pd1 72.1(2) . . ? C2 C3 Pd1 70.6(2) . . ? C5 N4 C9 117.0(3) . . ? C5 N4 Pd1 115.9(2) . . ? C9 N4 Pd1 124.8(2) . . ? N4 C5 C6 123.8(3) . . ? C7 C6 C5 118.5(3) . . ? C6 C7 C8 118.6(3) . . ? C7 C8 C9 120.8(3) . . ? N4 C9 C8 121.0(3) . . ? N4 C9 C10 119.8(3) . . ? C8 C9 C10 119.1(3) . . ? C19 C10 C11 120.1(3) . . ? C19 C10 C9 120.1(3) . . ? C11 C10 C9 119.6(3) . . ? C12 C11 C10 120.8(3) . . ? C11 C12 C13 120.6(3) . . ? C18 C13 C12 119.1(3) . . ? C18 C13 C14 119.4(3) . . ? C12 C13 C14 121.5(3) . . ? C15 C14 C13 120.7(3) . . ? C14 C15 C16 120.3(3) . . ? C17 C16 C15 120.7(3) . . ? C16 C17 C18 121.2(3) . . ? C13 C18 C19 119.5(3) . . ? C13 C18 C17 117.7(3) . . ? C19 C18 C17 122.8(3) . . ? C10 C19 C18 119.7(3) . . ? C10 C19 C20 120.6(3) . . ? C18 C19 C20 119.6(3) . . ? C29 C20 C21 119.5(3) . . ? C29 C20 C19 118.2(3) . . ? C21 C20 C19 122.2(2) . . ? C26 C21 C22 118.3(3) . . ? C26 C21 C20 119.3(3) . . ? C22 C21 C20 122.5(3) . . ? C23 C22 C21 120.6(3) . . ? C22 C23 C24 120.8(3) . . ? C25 C24 C23 120.1(3) . . ? C24 C25 C26 121.2(3) . . ? C27 C26 C25 121.6(3) . . ? C27 C26 C21 119.4(3) . . ? C25 C26 C21 119.0(3) . . ? C28 C27 C26 120.5(3) . . ? C27 C28 C29 120.7(3) . . ? C20 C29 C28 120.5(3) . . ? C20 C29 C30 117.8(3) . . ? C28 C29 C30 121.5(3) . . ? N35 C30 C31 121.1(3) . . ? N35 C30 C29 117.5(2) . . ? C31 C30 C29 121.1(3) . . ? C32 C31 C30 119.5(3) . . ? C33 C32 C31 119.0(3) . . ? C32 C33 C34 119.1(3) . . ? N35 C34 C33 123.0(3) . . ? C34 N35 C30 117.5(3) . . ? C34 N35 Pd1 117.9(2) . . ? C30 N35 Pd1 121.5(2) . . ? C37 Pd2 C38 38.11(17) . . ? C37 Pd2 C36 37.86(16) . . ? C38 Pd2 C36 67.81(16) . . ? C37 Pd2 N39 122.70(16) . . ? C38 Pd2 N39 90.42(14) . . ? C36 Pd2 N39 158.22(14) . . ? C37 Pd2 N70 128.26(16) . . ? C38 Pd2 N70 162.45(14) . . ? C36 Pd2 N70 95.17(13) . . ? N39 Pd2 N70 106.50(10) . . ? C37 C36 Pd2 70.5(2) . . ? C36 C37 C38 118.3(4) . . ? C36 C37 Pd2 71.6(2) . . ? C38 C37 Pd2 71.1(2) . . ? C37 C38 Pd2 70.8(2) . . ? C40 N39 C44 118.5(3) . . ? C40 N39 Pd2 118.1(2) . . ? C44 N39 Pd2 119.5(2) . . ? N39 C40 C41 122.2(4) . . ? C42 C41 C40 119.7(4) . . ? C41 C42 C43 118.7(4) . . ? C44 C43 C42 118.8(4) . . ? N39 C44 C43 121.8(3) . . ? N39 C44 C45 116.7(3) . . ? C43 C44 C45 121.5(3) . . ? C54 C45 C46 121.0(3) . . ? C54 C45 C44 119.3(3) . . ? C46 C45 C44 119.7(3) . . ? C47 C46 C45 120.3(3) . . ? C46 C47 C48 120.6(3) . . ? C49 C48 C47 121.5(3) . . ? C49 C48 C53 118.5(3) . . ? C47 C48 C53 119.9(3) . . ? C50 C49 C48 121.2(3) . . ? C49 C50 C51 120.3(3) . . ? C52 C51 C50 120.4(4) . . ? C51 C52 C53 120.8(3) . . ? C52 C53 C48 118.8(3) . . ? C52 C53 C54 122.6(3) . . ? C48 C53 C54 118.6(3) . . ? C45 C54 C53 119.6(3) . . ? C45 C54 C55 118.6(3) . . ? C53 C54 C55 121.6(3) . . ? C64 C55 C56 119.4(3) . . ? C64 C55 C54 120.5(3) . . ? C56 C55 C54 120.0(3) . . ? C57 C56 C61 118.8(3) . . ? C57 C56 C55 121.9(3) . . ? C61 C56 C55 119.2(3) . . ? C58 C57 C56 121.0(3) . . ? C57 C58 C59 120.0(3) . . ? C60 C59 C58 120.8(3) . . ? C59 C60 C61 120.6(3) . . ? C62 C61 C56 119.5(3) . . ? C62 C61 C60 121.6(3) . . ? C56 C61 C60 118.8(3) . . ? C63 C62 C61 120.6(3) . . ? C62 C63 C64 120.7(3) . . ? C55 C64 C63 120.2(3) . . ? C55 C64 C65 119.5(3) . . ? C63 C64 C65 119.9(3) . . ? N70 C65 C66 121.9(3) . . ? N70 C65 C64 119.5(3) . . ? C66 C65 C64 118.4(3) . . ? C65 C66 C67 120.0(3) . . ? C68 C67 C66 118.3(4) . . ? C69 C68 C67 119.4(3) . . ? N70 C69 C68 123.5(3) . . ? C65 N70 C69 116.4(3) . . ? C65 N70 Pd2 126.0(2) . . ? C69 N70 Pd2 115.7(2) . . ? F71A C71 F71C 108.4(4) . . ? F71A C71 F71B 108.5(4) . . ? F71C C71 F71B 105.8(4) . . ? F71A C71 S72 113.4(4) . . ? F71C C71 S72 111.5(3) . . ? F71B C71 S72 108.9(3) . . ? O72B S72 O72C 116.65(17) . . ? O72B S72 O72A 113.19(17) . . ? O72C S72 O72A 115.04(16) . . ? O72B S72 C71 103.6(2) . . ? O72C S72 C71 104.03(17) . . ? O72A S72 C71 101.8(2) . . ? F73B C73 F73C 108.3(3) . . ? F73B C73 F73A 105.9(3) . . ? F73C C73 F73A 107.0(3) . . ? F73B C73 S74 112.8(3) . . ? F73C C73 S74 111.8(3) . . ? F73A C73 S74 110.7(3) . . ? O74C S74 O74A 116.58(17) . . ? O74C S74 O74B 114.49(19) . . ? O74A S74 O74B 113.48(18) . . ? O74C S74 C73 103.10(18) . . ? O74A S74 C73 104.25(18) . . ? O74B S74 C73 102.61(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.097 _refine_diff_density_min -0.570 _refine_diff_density_rms 0.067 #===END (data for 25, also end of cif file)