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Accessory Publication Pitfalls in the Photoelectron Spectroscopic Investigations of Benzyne. Photoelectron Spectrum of Cyclopentadienylideneketene. Anna Chrostowska, A,C Genevieve Pfister-Guillouzo, A Françoise Gracian A and Curt Wentrup B,C A Equipe de Chimie Physique, Institut Pluridisciplinaire de Recherche sur l'environnement et les Matériaux, UMR CRNS 5254, Université de Pau et les Pays de l Adour, 6400 Pau, France. B School of Chemistry and Molecular Biosciences, The University of Queensland, Brisbane, Qld 4072, Australia C Correspondence authors. E-mail: anna.chrostowska@univ-pau.fr; wentrup@uq.edu.au Cartesian coordinates for 12 B3LYP/6-311G(d,p) C -0.5993935778-2.4946100834 0. C 0.8738239628-2.2783916433 0. C 1.1249126654-0.9566961485 0. C -1.2201196612-1.2999408471 0. C -0.1797810135-0.2497747213 0. C -0.3904028587 1.0708142386 0. H -1.0708578046-3.4679745101 0. H 1.6056200158-3.0749148449 0. H 2.0803515544-0.4543738282 0. H -2.2793129735-1.0936465208 0. C 0.054158939 2.2801649901 0. O 0.2897681519 3.4260454689 0. - E tot = 344,3527 au 9370,39 ev - E+ Zp-c = 344,268474 au 9368,10 ev ΔSCF = 0,3207 au 8,73 ev Cartesian coordinates for 12 MP2/6-311G(d,p) C -0.5820363335-2.5075815232 0. C 0.8775357695-2.2323000199 0. C 1.074787654-0.8888514447 0. C -1.2556229717-1.3269907688 0. C -0.2575737182-0.2431870322 0. S 1

C -0.5429926365 1.0802042628 0. H -1.0185773195-3.499981566 0. H 1.646337934-2.9969235837 0. H 2.0118418678-0.3459603504 0. H -2.325292675-1.1635663506 0. C 0.1396573247 2.2114284638 0. O 0.5207025043 3.3204114628 0. SCF Done: E(RHF) = -342.222163897 hartrees Sum of electronic and zero-point Energies= -343.274766 Sum of electronic and thermal Energies= -343.268027 Sum of electronic and thermal Enthalpies= -343.267083 Sum of electronic and thermal Free Energies= -343.306159 Cartesian coordinates for 12 HF/6-311G(d,p) C -0.5820363335-2.5075815232 0. C 0.8775357695-2.2323000199 0. C 1.074787654-0.8888514447 0. C -1.2556229717-1.3269907688 0. C -0.2575737182-0.2431870322 0. C -0.5429926365 1.0802042628 0. H -1.0185773195-3.499981566 0. H 1.646337934-2.9969235837 0. H 2.0118418678-0.3459603504 0. H -2.325292675-1.1635663506 0. C 0.1396573247 2.2114284638 0. O 0.5207025043 3.3204114628 0. SCF Done: E(RHF) = -342.222163897 hartrees Sum of electronic and zero-point Energies= -343.274766 Sum of electronic and thermal Energies= -343.268027 Sum of electronic and thermal Enthalpies= -343.267083 Sum of electronic and thermal Free Energies= -343.306159 Table 1. Calculated [B3LYP/6-311G(d,p); MP2/6-311G(d,p)(ΔSCF)] and experimental ionization energies (IEs) for 12 (all values in ev). nature of MO -ε KS TD-DFT MP2(ΔSCF) Exp. A 6.61 8.73 a 8.72 a A 6.73 8.75 8.80 8.9 A 7.91 9.98 9.97 10.2 A 10.68 12.66 S 2

A 10.70 12.75 a ΔSCF value (see computational details below) Cartesian coordinates for 17 B3LYP/6-311G(d,p) C -0.6888965452-1.2460180007-1.7673680969 C -1.1661790461-0.0054186614-0.9689804146 C -0.7212817203 1.26965138-1.7308818502 C 0.8676247131-1.2281241131-1.5722796035 C 1.1049692135 0.0197001687-0.6837968282 C 0.8352423412 1.2862211063-1.5358162254 C -0.1580976992-0.0089231784 0.1665335925 C -0.3398427942-0.0306685488 1.4751521631 C 0.0155355785-0.0424266058 2.7060069523 O 0.1966731006-0.0549280479 3.8652353734 H -0.9848136913-1.181823984-2.8171352175 H -1.1237189033-2.159713887-1.3568556625 H -2.2126398983-0.023191018-0.6724808011 H -1.1793423111 2.1595448314-1.2941738156 H -1.0158615248 1.2283510048-2.7821723466 H 1.4112163152-1.1523184981-2.5170448201 H 1.2090257055-2.1337703879-1.0665566498 H 2.0451975288 0.0238695975-0.1361612177 H 1.3802475253 1.2517869073-2.4821813878 H 1.153434842 2.1853456151-1.0039983735 Neutral: SCF Done: E(RB+HF-LYP) = -424.235034688 Zero-point correction= 0.167624 (Hartree/Particle) Thermal correction to Energy= 0.176110 Thermal correction to Enthalpy= 0.177054 Thermal correction to Gibbs Free Energy= 0.133364 Sum of electronic and zero-point Energies= -424.067411 Sum of electronic and thermal Energies= -424.058925 Sum of electronic and thermal Enthalpies= -424.057981 Sum of electronic and thermal Free Energies= -424.101671 Cation: SCF Done: E(UB+HF-LYP) = -423.936996948 ΔSCF = 0.2980377 au = 8.11 ev S 3

Cartesian coordinates for 17 HF/6-311G(d,p) C -0.6890030911-1.2374343506-1.7881956119 C -1.2022165431-0.0043518728-1.0129754931 C -0.7183013778 1.2620690282-1.7526030045 C 0.8531243507-1.2227082251-1.5180103938 C 1.0485946645 0.0164688904-0.6185015328 C 0.8236704694 1.2765142528-1.4814209831 C -0.2523614046-0.009898495 0.1624171295 C -0.5231565198-0.0310385602 1.4726488142 C 0.15013882-0.0372909768 2.60385125 O 0.5332661396-0.0447203245 3.7139248577 H -0.931857124-1.1653667693-2.8533655284 H -1.1422909726-2.1531876792-1.3967082164 H -2.2644189976-0.0203436949-0.7645069859 H -1.1934890858 2.1553775205-1.3360628056 H -0.9589505707 1.2141356153-2.8196343791 H 1.4419977646-1.1409905323-2.4375112692 H 1.1642421261-2.1319476708-0.9945374906 H 1.9623217908 0.0185248504-0.0205235207 H 1.4146501078 1.236232883-2.4023162891 H 1.1125321836 2.1771017908-0.9309237772 SCF Done: E(RHF) = -421.507163263 hartrees Zero-point correction= 0.169270 (Hartree/Particle) Thermal correction to Energy= 0.177744 Thermal correction to Enthalpy= 0.178688 Thermal correction to Gibbs Free Energy= 0.135098 Sum of electronic and zero-point Energies= -422.813872 Sum of electronic and thermal Energies= -422.805399 Sum of electronic and thermal Enthalpies= -422.804454 Sum of electronic and thermal Free Energies= -422.848045 Table 2. Calculated [B3LYP/6-311G(d,p); MP2/6-311G(d,p)(ΔSCF)] and experimental ionization energies (IEs) for 17 (all values in ev). nature of MO -ε KS TD-DFT MP2(ΔSCF) Exp. 5.98 8.11 a 8.34 a 8.35 7.76 9.11 a ΔSCF value (see computational details below) S 4

All calculations were performed using the Gaussian 03program package. 32 The 6-311G(d,p) basis set was used, and geometry optimizations were carried out at the HF as well as the DFT 33 level of theory with the B3LYP 34 functional and confirmed as true minima via frequency analysis, which was also used to calculate zero-point energies (ZPEs) without scaling. Ionization energies were calculated with ΔSCF-DFT, which means that separate SCF calculations were performed to optimize the orbitals of the ground state and the appropriate excited state determinants (IE=E cation -E neut.mol. ). The TDDFT 35 approach provides a first principles method for the calculation of excitation energies within a density functional context, taking into account the low lying ion calculated by the ΔSCF method. The advantages of this widely employed method of calculation of the first ionization energies (ΔSCF-DFT calculations) have been thoroughly demonstrated. 36 32 Gaussian 03: Frisch, M. J.; Trucks, G. W.; Schlegel, H. B.; Scuseria, G. E.; Robb, M. A.; Cheeseman, J. R.; Montgomery, J. A.; Vreven, Jr., T.; Kudin, K. N.; Stratman, R. E.; Burant, J. C.; Dapprich, S.; Millam, J. M.; Daniels, A. D.; Kudin, Burant, J. C.; Iyengar, S. S.; Tomasi, J.; Barone, V.; Mennucci, B.; Cossi, M.; Scalmani, G.; Rega, N.; Petersson, G. A.; Nakatsuji, H.; Hada, M.; Ehara, M. ; Toyota, K.; Fukuda, R.; Hasegawa, J.; Ishida, M.; Nakajima, T.; Honda, Y.; Kitao, O., Nakai, H.; Klene, M.; Li, X.J; Knox, E.; Hratchian, H. P.; Cross, J. B.; Bakken, V.; Adamo, C.; Jaramillo, J.; Gomperts, R.; Stratmann, R. E.; Yazyev, O.; Austin, A. J.; Cammi, R.; Pomelli, C.; Ochterski, J. W.; Ayala, P. Y.; Morokuma, K.; Voth, G. A.; Salvador, P.; Dannenberg, J. J.; Zakrzewski, V. G.; Dapprich, S.; Daniels, A. D.; Strain, M. C.; Farkas, O.; Malick, D. K.; Rabuck, A. D.; Raghavachari, K.; Foresman, J. B.; Ortiz, J. V.; Cui, Q.; Baboul, A. G.; Clifford, S.; Cioslowski, J.; Stefanov, B. B.; Liu, G.; Liashenko, A.; Piskorz, P.; Komaromi, I.; S 5

Martin, R.; Fox, D. J.; Keith, T.; Al-Laham, M. A.; Peng, C. Y.; Nanayakkara, A.; Challacombe, M.; Gill, P. M. W.; Jonhson, B.; Chen, W.; Wong, M. W.; Gonzalez, C.; Pople, J. A. Revisions E.01, Gaussian, Inc., Wallingford CT, 2004. 33 (a) Parr, R. G.; Yang, W.; Functional Theory of Atoms and Molecules, Oxford University Press, New York, 1989; (b) M. J. Frish, G. W. Trucks and J. R. Cheeseman, Systematic Model Chemistries Based on Density Functional Theory: Comparison with Traditional Models and with Experiment in: Recent Development and Applications of Modern Density Functional Theory, Theoretical and Computational Chemistry (Ed.: J. M. Semminario), 1996, vol 4, pp. 679-707, Elsevier Science B. V. Amsterdam Lausanne New York Oxford Shannon - Tokyo. 34 (a) Becke, A. D. Phys. Rev. 1988, 38, 3098-3100; (b) Becke, A. D. J. Chem. Phys. 1993, 98, 5648-5652; (c) Lee, C.; Yang, W.; Parr, R. G. Phys. Rev. 1988, B37, 785-789. 35 (a) R. E. Stratmann, G. E. Scuseria and M. J. Frisch, J. Chem. Phys., 1998, 109, 8218-8224; (b) M. E. Casida, C. Jamorski, K. C. Casida and D. R. Salahub, J. Chem. Phys., 1998, 108, 4439-4449. 36 (a) Joantéguy, S. ; Pfister-Guillouzo, G. ; Chermette, H. J. Phys. Chem. 1999, 103, 3505-3511 ; (b) Chrostowska, A. ; Miqueu, K. ; Pfister-Guillouzo, G. ; Briard, E. ; Levillain, J. ; Ripoll, J.-L. J. Mol. Spectrosc. 2001, 205, 323-330 ; (c) Bartnik, R. ; Baylère, P. ; Chrostowska, A. ; Galindo, A. ; Lesniak, S. ; Pfister-Guillouzo, G. Eur. J. Org. Chem. 2003, 2475-2479 ; (d) Lemierre, V. ; Chrostowska, A. ; Dargelos, A. ; Chermette, H. J. Phys. Chem. A, 2005, 109, 8348-8355. S 6