39 Park Drive
`UPMINSTER
`Essex RM14 3AL
`
`Tel: 017082 220742
`
`CAREER HISTORY
`
`TERRY THRELFALL
`
`School of Chemistry
`University of Southampton
`Highfield, Southampton
`SO17 1BJ, UK
`
`Tel: 01904 432576/Fax: 01904 432516
`email t. threlfall@soton.ac.uk
`
`Senior Research Fellow, Crystallography Group, School of Chemistry 2003 - date
`Research - investigating crystallisation and solid-solid transition processes, crystallizing samples
`for X-ray crystallographic studies, understanding the molecular solid state through structural
`systematics, spectral and thermal studies of polymorphs, solvates, hydrates and derivatives.
`Honorary Research Fellow, Department of Chemistry 1999 - 2003
`Research - investigating polymorphism through spectral and structural investigation of the solid
`state forms of sulphadrugs.
`Industrial Liaison Executive, Department of Chemistry.
`1991 - 1999
`Responsible for organising Short Courses for Industry; setting up Multi-university Modular MSc.;
`External Analytical Services; Skills teaching
`¯
`Involved in skills based workshops for undergraduates
`¯ Set up and tutored on "Problem Solving for Analytical Chemists" and "IR and Raman
`Spectroscopy" courses for industrial analysts.
`Joint author of ’A Question of Chemistry’. Now translated into French and Japanese.
`
`¯
`
`29 years with Rhone Poulenc Rorer Ltd., formerly May & Baker Ltd, now Sanofi-Aventis.
`Consultant 1990 - 1991
`Responsible for providing technical support and data gathering for overseas tax litigation.
`Principal Scientist 1987- 1990
`Responsible for maintaining patent monopoly worth £130 million per annum worldwide.
`©rganised schools and academic liaison activities and acted as an internal scientific consultant.
`¯ Negotiating skills, especially in Japan
`Process Research Manager 1983 - 1987
`Responsible for developing processes for whole of May and Baker Ltd. Facilities included pilot
`plant, pressure reactor and clean room. 28 scientific staff. Budget £½ m.
`¯ General management skills; also helped with management skills courses.
`¯
`Interviewing. Noted that many well qualified candidates did not interview well and that
`many well qualified appointees failed to apply their knowledge effectively.
`¯ On Career Counselling Panel
`Departmental Head, Physical Chemistry 1976 - 1983
`Providing a wide range of scientific services. Ran pigment development project. 22 staff.
`¯ Organised technicians’ development courses
`¯ Presented successful cases for expansion, new laboratory and new equipment.
`Section Head, Spectroscopy 1962 - 1976
`Responsible for providing a spectroscopic service and for pearling agent research.
`EARLIER HISTORY
`Mathematics Teacher 1962; NATO Research Student, Switzerland, 1959-1961; Part-time lecturer in
`Chemistry and Physics 1957-1959; Trainee in Electrical Engineering Industry 1955-1956.
`
`Lupin Ex. 1026 (Page 1 of 6)
`
`

`

`EDUCATION
`B.Sc. Chemistry 1956; Ph.D. Organic Chemistry 1971; Ll.B. Law 1984.
`OTHER ACTIVITIES
`Taught German part-time for - 25 years. Active member of many societies.
`PERSONAL
`Aged 74 years, married with 2 grown-up children.
`
`1.
`
`I am a Senior Research Fellow in the Department of Chemistry at the University of
`
`Southampton. My principal fields of interest are polymorphism and other aspects of solid state
`
`crystal structure and behaviour, and in understanding crystallization and transformation
`
`processes. My current research interests are in relating molecular structure to crystal structure
`
`using structural systematics and in applying spectroscopy and microscopy to crystallization and
`
`to solid-solid transition processes.
`
`2.
`
`I received a Bachelor of Science degree in chemistry from London University in 1956,
`
`a Ph.D. in organic chemistry from London University in 1971 and a Batchelor of Law degree from
`
`the University of London in 1984.
`
`3.
`
`In 1962, I was appointed Section Head of Spectroscopy at May & Baker Ltd., which
`
`later became known as Rhone Poulenc Rorer Ltd. Over the years at May & Baker, I introduced
`
`NMR, mass spectroscopy, preparative HPLC and chemical microscopy and electron microscopy
`
`to the company. As the Section Head, I was specifically responsible for the Pearling agent
`
`research program which presented substantial crystalline challenges. In 1976, I was appointed as
`
`the Department Head of Physical Chemistry. In this capacity, I was responsible for overseeing a
`
`substantial group of scientists, technical officers, and technicians in relation to the origin of
`
`samples, identity of samples, purity of samples, hydration, solvation, polymorphism, salt
`
`formation, crystal habit and amorphicity. In 1983, I was appointed as Process Research Manager
`
`and was responsible for scaling up synthetic routes, which involved consideration of the purity,
`
`purification, crystallisation, stability and filterability of samples. In 1987, I became a Principal
`
`Scientist, in which capacity I organized schools liaison and acted as an internal scientific
`
`consultant. Over my twenty-nine years at May & Baker, I gained considerable experience of a
`
`wide variety of situations and of problems associated with the identification, purification,
`
`crystallisation and separation of compounds of all kinds, but particularly with organic
`
`pharmaceuticals.
`
`Lupin Ex. 1026 (Page 2 of 6)
`
`

`

`4.
`
`Prior to taking a position at the University of Southampton, I was the Industrial
`
`Liaison Executive in the Department of Chemistry at the University of York. Specifically, I joined
`
`the University of York faculty in 1991 and was later appointed a Research Fellow. At the
`
`University of York, I organized short courses for industry, participated in skills based workshops
`
`for undergraduates, and conducted research on polymorphism, instrumentation and molecular
`
`templates.
`I currently conduct research relating to growing crystals large enough for single crystal diffraction
`
`work and for other studies. I personally carry out 500 crystallisations per year, particularly for
`
`the preparation of polymorphs, hydrates, solvates and co-crystals.
`
`Lupin Ex. 1026 (Page 3 of 6)
`
`

`

`PUBLICATIONS BY TERRY THRELFALL
`
`BOOKS
`
`A Question of Chemistry: Creative Problems for Critical Thinkers. Garrett, J., Overton,
`T. and Threlfall, T,, Longman, Harlow, UK, 1999. Now translated into French and
`Japanese.
`
`BOOK CHAPTERS
`"Vibrational Spectroscopy of Solid-State Forms - Introduction, Principles and Overview"
`T.L, Threlfall and J.M. Chalmers in "Applications of Vibrational Spectroscopy in
`Pharmaceutical Research and Development" Ed. D.E. Pivonka, J.M. Chalmers and P.R.
`Griffiths, J. Wiley, New York and Chichester
`
`"Polymorphs, Solvates and Amorphous Compounds" in the "Wiley Handbook of
`Vibrational Spectroscopy", Ed. Griffiths, P. and Chalmers, J. Wiley, New York and
`Chichester 2001
`
`"Instrument Design Considerations" in Standards and Best Practice in Absorption
`Spectrometry. Ed. Burgess, C. and Frost, T., Blackwell Science, Oxford, UK 1999
`
`"Colour Measurement" in Practical Absorption Spectrometry Ed. Burgess, C., Russell,
`M. and Frost, T., Chapman and Hall, London, UK, 1996
`
`"Structure-Spectral Relationships" in Practical Absorption Spectrometry_ Ed. Burgess, C.,
`Russell, M. and Frost, T., Chapman and Hall, London, UK, 1996
`
`ARTICLES
`35. A Systematic Study of the Crystallisation Products of a Series of Dicarboxy#c
`Acids with Imidazole Derivatives. S. Callear, M.B. Hursthouse and T. Threlfall,
`CrystEngComm., 2010. 12, 898-908
`34. Why do organic compounds crystallise well, badly or ever so slowly? Why is
`crystallisation nevertheless such a good purification technique? M.B. Hursthouse, L.S.
`Huth and T.L. Threlfall, Org. Proc. Res. Dev., 2009, 13, 1231-40
`33. Turning DSC Charts of Polymorphs into Phase Diagrams: A Tutorial Paper. T.
`Threlfall, Org. Proc. Res. Dev., 2009, 13, 1224-1230
`32. The Elusive High-Temperature Sofd-State Structure of D, L-Norleucine. S.J.
`Coles, T. Gelbrich, U.J. Greisser, M.B. Hursthouse, M. Pitak and T. Threlfall, Cryst.
`Growth. Des., 2009,9, 4610-12
`31. Co-crystallisation of organic c~,co-dicarboxyfc acids with the cycfc amides 2-
`pyrrofdine and 2-imidazofne. S. Callear, M.B. Hursthouse and T.L. Threlfall,
`CrystEngComm., 2009, 11, 1609-14
`
`30. Packing Similarity in Polymorphs ofSulfathiazole, T. Gelbrich, D. S. Hughes,
`M.B. Hursthouse and T.L. Threlfall, CrystEngComm. 2008, 10, 1328
`
`Lupin Ex. 1026 (Page 4 of 6)
`
`

`

`26.
`
`25.
`
`24.
`
`23.
`
`22.
`
`20.
`
`21.
`
`29. Delta-Sulfanilamide T. Gelbrich, A. Bingham, T. Threlfall, M. Hursthouse, Acta
`Cryst.C 2008, C64, o205-o207
`28. Polymorph VI of sulfapyridine : interpenetrating two- and three-dimensional
`hydrogen-bonded nets formed from two tautomericforms, T. Gelbrich and T. Threlfall,
`Acta Cryst. C 2007, C63, o323-o326
`27. T. Gelbrich, M.B. Hursthouse and T.L. Threlfall, Structural Systematics: Crystal
`structures of para,para-disubstitured benzenesulfonamides: Part 1, Overview and
`the isostructural dimers. Acta Cryst. B, 2007, 63B, 621-632.
`T.L. Threlfall and T. Gelbrich, The structure of methylparaben at l18K does not
`represent a new polymorph, Cryst. Growth and Design, 2007,7, 2297
`Gelbrich, T., Threlfall, T.L., Hursthouse, M.B., Anilinium chloride adduct of 4-
`bromo-N-benzenesulfonamide, Acta Cryst. C, 2006, 62, 470-472
`Gelbrich, T., Threlfall, T.L., Huth, S., Seeger, E., Structures ofracemic #thium
`tartrate hydrates, Polyhedron, 2006, 25, 937-944
`S. Karami, L. Yang, D.S. Hughes, M.B. Hursthouse, A.E. Russell, T.L. Threlfall,
`M. Claybourne, R. Roberts, Further Errors in Polymorph identification:
`Furosemide and Finasteride. Acta Cryst., 2006, B62, 689-91
`Gelbrich, T., Threlfall, T.L., Huth, S., Seeger, E., Hursthouse, M.B., Investigation
`of the relationship between racemic alka# and ammonium hydrogen tartrates and
`their chiral counterparts. Z. Anorg. Allg. Chem., 2004, 630, 1451
`Threlfall, T.L., The Structural and Thermodynamic Basis of Ostwald’s Rule. Org.
`Proc. Res. Dev., 2003, 7(6), 1017-1027
`Portieri, A., Harris, R.K., Fletton, R.A, Lancaster, R.W. and Threlfall, T.L. Effects
`of Polymorphic Differences for Sulfanilamide, as seen through 13C and 15N
`so#d-state NMR, together with shielding calculations. Org. Magn. Resonance,
`2003
`Bingham, A., Hughes, D.S., Hursthouse, M., Lancaster, R.W., Tavener,
`Threlfall, T. Over one hundred solvates of Sulfathiazole. Chem. Commun. 2001,
`603 -604
`Threlfall, T.L, Crystallisation of Polymorphs: Thermodynamic Insight into the
`Role of Solvent, Org. Process Res. Dev. 2000, 4, 384-390
`Apperley, D.C., Fletton, R.A., Harris, R.K., Lancaster, R.W., Tavener, S. and
`Threlfall, T.L., Sulfathiazole Polymorphism Studied by Magic Angle Spinning
`NMR Spectroscopy, J. Pharm. Sci., 1999, 88~ 1275-1280
`Hughes, D.S., Hursthouse, M.B., Threlfall, T. and Tavener, S. A New Polymorph
`ofSulfathiazole, Acta Cryst. 1999, C55, 1831-1833
`Hughes, D., Hursthouse, M., Lancaster, R., Tavener, S., Threlfall, T. and Turner,
`P, How Many Polymorphs has Sulphathiazole ? Proposals for reporting
`Crystallographic Data ofPolymorphs, J. Pharm. Pharmacol., 1997, 49~ ($4) p.20
`
`19.
`
`18.
`
`17.
`
`16.
`
`15.
`
`14.
`
`13.
`
`12.
`
`Threlfall, T.L. Analysis of Organic Polymorphs A Review, Analyst, 1995, 120,
`2435-2460
`Windram, V.A. and Threlfall, T.L. ChemicalMicroscopy in the Pharmaceutical
`Industry, Analytical Proceedings, 1992, 29, 108-110
`Deeley, C.M., Spragg, R.A. and Threlfall, T.L. A Comparison of Fourier
`Transform Infrared and Fourier Transform Raman Spectroscopy for Quantitative
`
`Lupin Ex. 1026 (Page 5 of 6)
`
`

`

`11.
`
`10.
`
`9.
`
`Measurements An Application in Polymorphism. Spectrochim. Acta, 1991~ 47A,
`1217-1223
`Threlfall, T.L. Developments in UV-Visible Spectroscopy, Eur. Spectrosc. News,
`1988, 78, 8,10,12
`Brown, O.R., Middleton, P.H. and Thrrelfall, T.L. Cathodic Elimination reactions
`ofAcycHc VicinalDibromides, J. Chem. Soc., Perkin Trans. II, 1983, 955-963
`Caton, M.L.P., Darnborough, G, Parker, T., Peart, B.J., Podmore, M.L. and
`Threlfall, T.L. Prostaglandins. 7. Synthesis of (+/-)-l l-Deoxy-lO-
`hydroxyprostaglandins. (+/-)-11-Deoxy-10-oxoprostaglandins, J. Chem,. Soc.,
`Perkin Trans. I 1983, 319-323
`Grinter, R. and Threlfall, T.L. New Empirical Relationships in Electronic
`Spectroscopy: Woodward’s, Zechmeister ’ s and Jones’ Rules Revisited, UV
`Spectrom. Group Bull., 1981, 9, 106-124
`Grinter, R and Threlfall, T.L.,The effect of Substituents upon the Ultraviolet
`Spectra of Conjugated Dienes. The Applicability of Woodward’s Rules,
`Tetrahedron, 1979, 35,1543-1549
`Threlfall,T.L. and Peart, B.J. Spectroscopy in Drug Development. Rev. Prog.
`Appl. Chem., 1975, 59, 531-543
`Ninet,L., Benazet, F.,Charpentie, Y., Dubost, M., Florent, J., Mancy, D.,
`Preud’Homme, J., Threlfall, T.L., Vuiillemin, B., Wright, D.E., Abraham, A.,
`Cartier, M., De Chezelles, N., Godard, C. and Theilleux, J. Clorobiocin, A New
`Chlorinated Antibiotic Produced by Several Streptomyces Spp., C.r. Hebh.
`Seances Acad. Sci. Set C., Sci. Chim.,1972, 275,455-458
`Clark, D.W.H. and Threlfall, T.L. Pigments Based on Titanium Dioxide,
`Zirconium Dioxide, or Alkaline Earth Metal Titanates, Brit. Patent GB 1238440
`(1971)
`Clark, D.W.H. and Threlfall, T.L., Nacreous Pigments, South African Patent ZA
`6805748 (1969)
`Corbett, K., Edwards, S.A., Lee, G.E. and Threlfall, T.L., Metabolism of 5-
`chloro-2-cyclohexyk-l-oxo-6-sulphamoyHsoindoHne (M&B 8430) Nature, 1965,
`208, 286-287
`Lunt, E. and Threlfall, T.L, Chem. Ind., 1964, 43, 1805-1806
`
`Lupin Ex. 1026 (Page 6 of 6)
`
`