Mylan Exhibit 1029
`Mylan Exhibit 1029
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`Mylan (IPR2020-00040) EX. 1029 p. 001
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`Mylan (IPR2020-00040) Ex. 1029 p. 001
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`Mylan Exhibit 1029
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`Mylan (IPR2020-00040) EX. 1029 p. 001
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`Mylan (IPR2020-00040) Ex. 1029 p. 001
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`UNITED STATES PATENT AND TRADEMARK OFFICE
`__________________
`
`BEFORE THE PATENT TRIAL AND APPEAL BOARD
`__________________
`
`MYLAN PHARMACEUTICALS INC.,
`Petitioner,
`
`v.
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`MERCK SHARP & DOHME CORP.,
`Patent Owner.
`__________________
`
`Case No. IPR2020-00040
`U.S. Patent No. 7,326,708
`__________________
`
`SECOND DECLARATION OF ADAM J. MATZGER
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`1
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`Merck Exhibit 2269, Page 1
`Mylan Pharmaceuticals Inc. v. Merck Sharp & Dohme Corp.
`IPR2020-00040
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`Mylan (IPR2020-00040) Ex. 1029 p. 002
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`I, Adam J. Matzger, declare as follows:
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`1.
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`I have been informed by counsel for Patent Owner Merck that
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`Petitioner Mylan has made a number of objections to my lab notebooks and the
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`data I generated (EX2228, EX2229, and EX2231), which as I described in my
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`Declaration (EX2103) demonstrate the existence of non-1:1 sitagliptin phosphate
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`salts. I have therefore been asked by counsel to provide certain additional
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`information about those experiments and the data I submitted as a part of my
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`Declaration.
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`2.
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`EX2228 is a true and accurate copy of one of my lab notebooks. I
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`personally performed the experiments described in EX2228, and I
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`contemporaneously recorded them in that lab notebook as I performed the
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`experiments.
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`3.
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`EX2229 is a true and accurate copy of another one of my lab
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`notebooks. I personally performed the experiments described in EX2229, and I
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`contemporaneously recorded them in that lab notebook as I performed the
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`experiments.
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`4.
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`EX2231 is a true, accurate, and complete collection of the data
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`generated in connection with my work on this case. It is a ZIP archive containing
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`various electronic data files, which I have organized by the type of experiment into
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`top-level folders: Elemental Analysis, Optical Microscopy, PXRD, Raman, Single
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`2
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`Merck Exhibit 2269, Page 2
`Mylan Pharmaceuticals Inc. v. Merck Sharp & Dohme Corp.
`IPR2020-00040
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`Mylan (IPR2020-00040) Ex. 1029 p. 003
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`Crystal, and TGA. Within each of those folders, I have applied a consistent file
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`naming convention. The file names in EX2231 correspond to the file names
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`referenced in my Declaration. File names beginning with “AJM” additionally
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`correspond to particular entries in my lab notebooks, and the file names indicate
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`the particular lab notebook and page number corresponding to the data in the file.
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`For example, Figure 6 in my Declaration is a PXRD pattern of the sitagliptin free
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`base supplied from Merck. The caption to Figure 6 identifies the file name as
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`AJM-III-25.1, and the corresponding files (AJM-III-25_1.ras, AJM-III-
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`25_1_Theta_2-Theta.asc, AJM-III-25_1_Theta_2-Theta.raw) are in the PXRD
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`folder of EX2231. The “III” in “AJM-III-25.1” indicates that the relevant entry is
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`in lab notebook 3 (EX2228); the “25” indicates that the relevant entry is on page
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`25 of the lab notebook; and the “1” indicates that it is the first piece of data
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`generated on that page.
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`5.
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`In my Declaration, I described several different experimental
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`techniques that I used to characterize the materials I generated through my salt
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`experiments: (1) X-ray powder diffraction (PXRD or XRPD), (2) single crystal X-
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`ray powder diffraction, (3) thermogravimetric analysis (TGA), (4) Raman
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`spectroscopy, and (5) elemental analysis. I describe each in turn.
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`6.
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`X-ray diffraction: X-ray diffraction is a well-known, routine
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`analytical technique (it is, for example, referred to in the specification of the ’708
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`3
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`Merck Exhibit 2269, Page 3
`Mylan Pharmaceuticals Inc. v. Merck Sharp & Dohme Corp.
`IPR2020-00040
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`Mylan (IPR2020-00040) Ex. 1029 p. 004
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`patent) that is used to identify crystalline forms and determine the crystal structure
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`of a material. It can be performed on both a powder sample (X-ray powder
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`diffraction – PXRD) of a crystalline substance or a single crystal (single crystal X-
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`ray powder diffraction). X-ray diffraction works by irradiating a material with X-
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`rays of a particular wavelength and then measuring the intensities and scattering
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`angles of the X-rays that are diffracted. Because the distances between the atoms
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`in a crystal are of a length similar to the X-ray wavelength, the presence of a
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`crystal structure in the sample will produce an observable pattern. This pattern is
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`unique to the crystal structure and thus can be used to identify the particular
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`crystalline form of a material.
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`7.
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`I describe the protocol I used for PXRD in paragraph 142 of my
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`declaration. I performed the various PXRD experiments detailed in EX2228 in
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`connection with my work on this case. The data generated in connection with
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`these experiments are in the “PXRD” folder of EX2231.
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`8.
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`I describe the protocol I used for single crystal X-ray diffraction in
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`paragraph 147 of my declaration. I performed the various single crystal X-ray
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`diffraction experiments detailed in EX2228, including the collection of single
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`crystal data in the Rigaku XtaLAB Synergy-S X-ray diffractometer, which is in my
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`laboratory. Additionally, I directed the collection of single crystal data on an
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`additional piece of equipment, the Rigaku AFC10K Saturn 944+ CCD-based X-ray
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`4
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`Merck Exhibit 2269, Page 4
`Mylan Pharmaceuticals Inc. v. Merck Sharp & Dohme Corp.
`IPR2020-00040
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`Mylan (IPR2020-00040) Ex. 1029 p. 005
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`diffractometer. This latter diffractometer is not in my lab but located at a central
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`facility at the University of Michigan. While I am familiar with how to run this
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`diffractometer, this facility limits access to the instrument to only staff of the
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`facility. It is standard for outside users to provide samples to the staff to run on the
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`instrument. Thus, I prepared the sample for data collection, which involves
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`selecting a crystal and mounting that crystal on a loop for data collection. I then
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`passed the sample to Dr. Jeff Kampf, Director of X-ray Crystallography at the
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`University of Michigan, who placed the sample into the X-ray beam and ran the
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`nearly entirely automated process of data collection. I was not physically present
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`during this data collection both due to COVID restrictions and because it is
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`standard protocol at the University for samples to be placed in a queue and run
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`when the diffractometer becomes available. The data generated in connection with
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`both sets of experiments are in the “Single Crystal” folder of EX2231.
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`9.
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`Thermogravimetric Analysis: Thermogravimetric analysis (TGA) is
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`a routine analytical technique (it is, for example, referred to in the specification of
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`the ’708 patent) that measures the mass of a sample over time and/or as a function
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`of the temperature of the sample. TGA can perform a number of functions,
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`including showing and quantifying the loss of water over time. Thus it can be used
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`to identify the presence of hydrates in a material. I describe the protocol I used to
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`conduct TGA in paragraph 146 of my declaration. The TGA experiment I
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`5
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`Merck Exhibit 2269, Page 5
`Mylan Pharmaceuticals Inc. v. Merck Sharp & Dohme Corp.
`IPR2020-00040
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`Mylan (IPR2020-00040) Ex. 1029 p. 006
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`performed is detailed in EX2228, and the results are in the “TGA” folder of
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`EX2231.
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`10. Raman Spectroscopy: Raman spectroscopy is a routinely used
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`analytical technique that provides detailed information about the chemical
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`structure, phase and polymorphism, and crystallinity of a material. It is based on
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`the interaction of light with chemical bonds within a material. Raman involves
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`shining a high intensity light source such as a laser on a material and measuring
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`how the molecules of that material scatter light. A Raman spectrum thus features a
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`number of peaks that correspond to specific molecular bond vibrations. I describe
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`the protocol I used to conduct Raman Spectroscopy in paragraph 145 of my
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`declaration. I performed the Raman experiments detailed in EX2228 and EX2229.
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`The Raman data I generated are in the “Raman” folder of EX2231.
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`11. Elemental Analysis: Elemental analysis refers to a variety of
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`techniques that are used to determine the quantity of a particular element in a
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`material. It can be used to determine the relevant stoichiometry of compounds in a
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`material by looking at the ratio of particular elements. I do not perform elemental
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`analysis in my laboratory. Scientists routinely use commercial analytical services
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`such as Galbraith Laboratories for techniques that they do not conduct in their own
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`labs and rely upon the data generated from these services. Accordingly, I sent the
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`samples I created to Galbraith Laboratories with instructions to measure, and to
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`6
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`Merck Exhibit 2269, Page 6
`Mylan Pharmaceuticals Inc. v. Merck Sharp & Dohme Corp.
`IPR2020-00040
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`Mylan (IPR2020-00040) Ex. 1029 p. 007
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`report back to me, the content of nitrogen and phosphorus in those samples.
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`Galbraith Laboratories is a reputable third-party lab that specializes in a number of
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`analytical techniques, including elemental analysis. I selected Galbraith because of
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`its reputation and experience with analytical techniques such as elemental analysis,
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`my previous positive experiences with Galbraith, and because its protocols for
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`elemental analysis were appropriate for the smaller sample size of non-1:1
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`sitagliptin phosphate salts I grew. I also note that Dr. Chyall, Teva’s expert in the
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`Israel opposition, also selected Galbraith Laboratories to perform elemental
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`analysis. EX2232 is a true and accurate copy of the report containing the
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`elemental analysis results I received from Galbraith Laboratories.
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`*
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`*
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`*
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`I hereby declare that all statements made herein of my own knowledge true
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`and that all statements made on information and belief are believed to be true; and
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`further that these statements were made with the knowledge that willful false
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`statements and the like so made are punishable by fine or imprisonment, or both,
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`under Section 1001 of Title 18 of the United States Code.
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`7
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`Merck Exhibit 2269, Page 7
`Mylan Pharmaceuticals Inc. v. Merck Sharp & Dohme Corp.
`IPR2020-00040
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`Mylan (IPR2020-00040) Ex. 1029 p. 008
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`Merck Exhibit 2269, Page 8
`Mylan Pharmaceuticals Inc. v. Merck Sharp & Dohme Corp.
`IPR2020-00040
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`Mylan (IPR2020-00040) Ex. 1029 p. 009
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