XRPD Analysis of Bihovsky Samples – Batch 2
`
`(13-134-1x; 13-137-1x; 13-143-1x; 13-144-1x)
`
`Dr. William E. Mayo
`2715 North Ocean Blvd. – Unit 2B
`Fort Lauderdale, FL 33308
`412-596-6113
`billm02127@gmail.com
`January 15, 2022
`
`Page 1 of 44
`
`EISAI EXHIBIT 1053
`Eisai v. Crystal Pharm.
`PGR2021-00047
`
`
`
`(13-134-1x; 13-137-1x; 13-143-1x; 13-144-1x)
`
`Dr. William E. Mayo
`2715 North Ocean Blvd. – Unit 2B
`Fort Lauderdale, FL 33308
`412-596-6113
`billm02127@gmail.com
`January 15, 2022
`
`Page 1 of 44
`
`EISAI EXHIBIT 1053
`Eisai v. Crystal Pharm.
`PGR2021-00047
`
`
`
`Photographs of As-Received Samples
`
`Page 2 of 44
`
`
`
`Shipping container (small ice box – ice packs not shown) and the four
`Figure 1
`samples. (Received by Dr. Steven Miller on 1/4/22). After receipt, the samples
`were stored in a lab freezer at -20° C.
`
`Page 3 of 44
`
`
`
`Close up photo of the four samples showing the sample identifications
`Figure 2
`13-134-1x; 13-137-1x; 13-143-1x; and 13-144-1x.
`
`Page 4 of 44
`
`
`
`Triplicate XRPD Diffraction Scans of As-Received Samples
`
`Page 5 of 44
`
`
`
`Summary of Test Conditions:
`
`Instrument:
`
`Panalytical X’Pert with X’Celerator line detector
`S/N – DY1368 (Located at H&M Analytical Services)
`Bragg Brentano para-focusing geometry
`Type:
`45KV/40 mA
`Power:
`2° - 40°
`Scan range:
`0.0131° (nominal)
`Step size:
`100 secs/step (nominal)
`Count time:
`DS – 1/4°; ASS – 1/2°; RS – 9.1
`Slits:
`0.04 Rad
`Soller Slits:
`Sample Spinner: 4 secs/rev
`Filter:
`Nickel
`Mask:
`10 mm
`Sample holder:
`Standard (16 mm Φ x 2mm deep; back loaded)
`
`Page 6 of 44
`
`
`
`Figure 3
`
`Triplicate scans of sample 13-134-1x showing good reproducibility
`
`Sample 13-134-1x
`
`Scan #3
`
`Scan #2
`
`Scan #1
`
`Intensity (Arbitrary Units)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Page 7 of 44
`
`
`
`Figure 4
`
`Triplicate scans of sample 13-137-1x showing good reproducibility
`
`Sample 13-137-1x
`
`Scan #3
`
`Scan #2
`
`Scan #1
`
`Intensity (Arbitrary Units)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Page 8 of 44
`
`
`
`Figure 5
`
`Triplicate scans of sample 13-143-1x showing good reproducibility
`
`Sample 13-143-1x
`
`Scan #3
`
`Scan #2
`
`Scan #1
`
`Intensity (Arbitrary Units)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Page 9 of 44
`
`
`
`Figure 6
`
`Triplicate scans of sample 13-144-1x showing good reproducibility
`
`Sample 13-144-1x
`
`Scan #3
`
`Scan #2
`
`Scan #1
`
`Intensity (Arbitrary Units)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Page 10 of 44
`
`
`
`Comparison of XRPD Pattern from 13-134-1x
`with Fig. 5 of the ‘779 Patent
`
`Page 11 of 44
`
`
`
`Figure 7
`
`Comparison of a typical synthesized sample (13-134-1x) with Figure 5 of the '779 Patent
`
`Fig. 5 from '779 Patent
`
`Intensity (Arbitrary Units)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`13-134-1x
`
`Page 12 of 44
`
`
`
`Analysis of XRPD Diffraction Scans of As-Received
`Samples to Determine Peak Positions
`
`Page 13 of 44
`
`
`
`[Full-13-134-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 8
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-134-1x
`
`Page 14 of 44
`
`
`
`[Full-13-137-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 9
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-137-1x
`
`Page 15 of 44
`
`
`
`[Full-13-143-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 10
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-143-1x
`
`Page 16 of 44
`
`
`
`[Full-13-144-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 11
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-144-1x
`
`Page 17 of 44
`
`
`
`[Full-2-13-134-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 12
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-134-1x (duplicate)
`
`Page 18 of 44
`
`
`
`[full-2-13-137-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 13
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-137-1x (duplicate)
`
`Page 19 of 44
`
`
`
`[Full-2-13-143-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 14
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-143-1x (duplicate)
`
`Page 20 of 44
`
`
`
`[Full-2-13-144-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 15
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-144-1x (duplicate)
`
`Page 21 of 44
`
`
`
`[Full-3-13-134-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 16
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-134-1x (triplicate)
`
`Page 22 of 44
`
`
`
`[Full-3-13-137-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 17
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-137-1x (triplicate)
`
`Page 23 of 44
`
`
`
`[Full-3-13-143-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 18
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-143-1x (triplicate)
`
`Page 24 of 44
`
`
`
`[Full-3-13-144-1x.dif]
`
`7.8
`
`11.4
`
`15.6
`
`12.5
`
`21.3
`
`27.3
`
`19.4
`
`22.3 24.0
`
`Claim 1
`
`Claim 1
`
`Claim 3
`
`Intensity(Counts)
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Figure 19
`
`Comparison of the peaks in the '779 claims with the XRPD pattern from sample 13-144-1x (triplicate)
`
`Page 25 of 44
`
`
`
`Numerical Analysis of Peak Position Agreement Between
`The Present Synthesized Samples and the ‘779 Patent
`
`Page 26 of 44
`
`
`
`Methodology:
`
`Program:
`Peak Picker:
`
`Filter:
`Threshold:
`
`Intensity Cutoff:
`
`Angle to find BG:
`Point for SG Average:
`
`Jade Plus (v. 9.5.0)
`Automated (Centroid method)
`2nd Derivative Savitzky-Golay method)
`Variable (39) with parabolic fit
`1.0
`0.1
`1.0
`7
`
`Page 27 of 44
`
`
`
`Summary of Peak Matching Analysis for Triplicate Samples of 13-134-1x
`
`Table I
`
`Claim 1 Peak Positions
`
`Claim 2 Peak Positions
`
`Claim 3 Peak Positions
`
`7.8°
`
`15.6°
`
`11.4°
`
`12.5°
`
`21.3°
`
`27.3°
`
`24.0°
`
`19.4°
`
`22.3°
`
`Sample 13-134-1x
`(scan #1)
`
`Sample 13-134-1x
`(scan #2)
`
`Sample 13-134-1x
`(scan #3)
`
`7.949°
`
`15.650°
`
`11.582°
`
`12.660°
`
`21.213°
`
`27.269°
`
`23.977°
`
`19.510°
`
`22.290°
`
`(+0.149°)
`
`(+0.050°)
`
`(+0.182°)
`
`(+0.160°)
`
`(-0.087°)
`
`(-0.031°)
`
`(-0.023°)
`
`(+0.110°)
`
`(-0.010°)
`
`7.973°
`
`15.687°
`
`11.598°
`
`12.685°
`
`21.156°
`
`27.256°
`
`24.045°
`
`19.547°
`
`22.309°
`
`(+0.173°)
`
`(+0.087°)
`
`(+0.198°)
`
`(+0.185°)
`
`(-0.144°)
`
`(-0.044°)
`
`(+0.045°)
`
`(+0.147°)
`
`(+0.009°)
`
`7.973°
`
`15.689°
`
`11.594°
`
`12.677°
`
`21.191°
`
`27.283°
`
`24.032°
`
`19.542°
`
`22.299°
`
`(+0.173°)
`
`(+0.089°)
`
`(+0.194°)
`
`(+0.177°)
`
`(-0.109°)
`
`(-0.017°)
`
`(+0.032°)
`
`(+0.142°)
`
`(-0.001°)
`
`Note: Experimental peak positions obtained by standard centroid method
`
`Page 28 of 44
`
`
`
`Summary of Peak Matching Analysis for Triplicate Samples of 13-137-1x
`
`Table II
`
`Claim 1 Peak Positions
`
`Claim 2 Peak Positions
`
`Claim 3 Peak Positions
`
`7.8°
`
`15.6°
`
`11.4°
`
`12.5°
`
`21.3°
`
`27.3°
`
`24.0°
`
`19.4°
`
`22.3°
`
`Sample 13-137-1x
`(scan #1)
`
`Sample 13-137-1x
`(scan #2)
`
`Sample 13-137-1x
`(scan #3)
`
`7.952°
`
`15.658°
`
`11.576°
`
`12.655°
`
`21.150°
`
`27.217°
`
`24.000°
`
`19.525°
`
`22.296°
`
`(+0.152°)
`
`(+0.058°)
`
`(+0.176°)
`
`(+0.155°)
`
`(-0.150°)
`
`(-0.083°)
`
`( 0.000°)
`
`(+0.125°)
`
`(-0.004°)
`
`7.961°
`
`15.673°
`
`11.585°
`
`12.671°
`
`21.192°
`
`27.230°
`
`24.013°
`
`19.541°
`
`22.313°
`
`(+0.161°)
`
`(+0.073°)
`
`(+0.185°)
`
`(+0.171°)
`
`(-0.108°)
`
`(-0.070°)
`
`(+0.013°)
`
`(+0.141°)
`
`(+0.013°)
`
`7.956°
`
`15.679°
`
`11.583°
`
`12.666°
`
`21.185°
`
`27.296°
`
`24.015°
`
`19.553°
`
`22.312°
`
`(+0.156°)
`
`(+0.079°)
`
`(+0.183°)
`
`(+0.166°)
`
`(-0.115°)
`
`(-0.004°)
`
`(+0.015°)
`
`(+0.153°)
`
`(+0.012°)
`
`Note: Experimental peak positions obtained by standard centroid method
`
`Page 29 of 44
`
`
`
`Summary of Peak Matching Analysis for Triplicate Samples of 13-143-1x
`
`Table III
`
`Claim 1 Peak Positions
`
`Claim 2 Peak Positions
`
`Claim 3 Peak Positions
`
`7.8°
`
`15.6°
`
`11.4°
`
`12.5°
`
`21.3°
`
`27.3°
`
`24.0°
`
`19.4°
`
`22.3°
`
`Sample 13-143-1x
`(scan #1)
`
`Sample 13-143-1x
`(scan #2)
`
`Sample 13-143-1x
`(scan #3)
`
`7.947°
`
`15.667°
`
`11.576°
`
`12.654°
`
`21.154°
`
`27.191°
`
`24.001°
`
`19.511°
`
`22.303°
`
`(+0.147°)
`
`(+0.067°)
`
`(+0.176°)
`
`(+0.154°)
`
`(-0.146°)
`
`(-0.109°)
`
`(+0.001°)
`
`(+0.111°)
`
`(+0.003°)
`
`7.938°
`
`15.663°
`
`11.557°
`
`12.644°
`
`21.195°
`
`27.230°
`
`23.987°
`
`19.497°
`
`22.298°
`
`(+0.138°)
`
`(+0.063°)
`
`(+0.157°)
`
`(+0.144°)
`
`(-0.105°)
`
`(-0.070°)
`
`(-0.013°)
`
`(+0.097°)
`
`(-0.002°)
`
`7.967°
`
`15.674°
`
`11.592°
`
`12.694°
`
`21.219°
`
`27.217°
`
`24.017°
`
`19.551°
`
`22.315°
`
`(+0.167°)
`
`(+0.074°)
`
`(+0.192°)
`
`(+0.194°)
`
`(-0.081°)
`
`(-0.083°)
`
`(+0.017°)
`
`(+0.151°)
`
`(+0.015°)
`
`Note: Experimental peak positions obtained by standard centroid method
`
`Page 30 of 44
`
`
`
`Summary of Peak Matching Analysis for Triplicate Samples of 13-144-1x
`
`Table IV
`
`Claim 1 Peak Positions
`
`Claim 2 Peak Positions
`
`Claim 3 Peak Positions
`
`7.8°
`
`15.6°
`
`11.4°
`
`12.5°
`
`21.3°
`
`27.3°
`
`24.0°
`
`19.4°
`
`22.3°
`
`Sample 13-144-1x
`(scan #1)
`
`Sample 13-144-1x
`(scan #2)
`
`Sample 13-144-1x
`(scan #3)
`
`7.926°
`
`15.627°
`
`11.545°
`
`12.630°
`
`21.195°
`
`27.278°
`
`23.985°
`
`19.492°
`
`22.257°
`
`(+0.126°)
`
`(+0.027°)
`
`(+0.145°)
`
`(+0.130°)
`
`(-0.105°)
`
`(-0.022°)
`
`(-0.015°)
`
`(+0.092°)
`
`(-0.043°)
`
`7.949°
`
`15.650°
`
`11.567°
`
`12.653°
`
`21.184°
`
`27.217°
`
`23.989°
`
`19.529°
`
`22.301°
`
`(+0.149°)
`
`(+0.050°)
`
`(+0.167°)
`
`(+0.153°)
`
`(-0.116°)
`
`(-0.083°)
`
`(-0.011°)
`
`(+0.129°)
`
`(+0.001°)
`
`7.956°
`
`15.658°
`
`11.575°
`
`12.660°
`
`21.174°
`
`27.257°
`
`24.005°
`
`19.535°
`
`22.299°
`
`(+0.156°)
`
`(+0.058°)
`
`(+0.175°)
`
`(+0.160°)
`
`(-0.126°)
`
`(-0.043°)
`
`(+0.005°)
`
`(+0.135°)
`
`(-0.001°)
`
`Note: Experimental peak positions obtained by standard centroid method
`
`Page 31 of 44
`
`
`
`Printouts of Automated Peak Peaker Results for
`
`Triplicate Scans of Samples 13-134-1x, 13-137-1x,
`
`13-143-1x and 13-144-1x
`
`Page 32 of 44
`
`
`
`[Full-13-134-1x.difi Bihovsky 13-134-1x
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, l(p)=50000, 01/14/22 09:33a
`
`Peak Search Report
`
`PEAK: 41(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alphal)
`
`[
`
`1
`2
`3
`4
`5
`6
`7
`8
`9
`10
`11
`12
`
`d(A)
`2-Theta
`7.949 11.1128
`11.582
`7.6344
`12.660
`6.9866
`15.650
`5.6576
`19.158
`4.6289
`4.5462
`19.510
`21.213
`4.1849
`4.1319
`21.488
`3.9852
`22.290
`23.977
`3.7085
`3.2677
`27.269
`3.2493
`27.427
`
`A% FWHM
`Area
`H%
`BG Height
`48.4
`0.256
`56.7 641027
`713 27961
`0.283
`12.2
`13.0 161780
`702
`6391
`0.265
`10.0
`11.4 132801
`5601
`700
`695 49305 100.0 1324328 100.0
`0.300
`56.3
`0.409
`41.2 745255
`694 20315
`0.571
`33.3 840630
`63.5
`694 16424
`4.5
`0.175
`3580
`7.3
`59499
`694
`12.7 198429
`15.0
`0.333
`694
`6264
`54.4
`0.568
`28.7 719992
`695 14136
`0.404
`15.5 276743
`20.9
`7653
`697
`27.1
`0.468
`16.4 358953
`702
`8062
`0.424
`22.9 428580
`32.4
`703 11268
`
`1 .
`
`°
`
`i
`
`7. 49°
`
`11.1582
`
`5
`
`10
`
`15
`
`19.18°
`
`1
`
`i10°
`
`22.x90°
`
`9
`
`27.427°
`
`23
`
`77°
`
`27'
`
`'
`
`211
`
`8
`
`21.2
`
`°
`
`J
`
`.
`
`,
`25
`20
`Two-Theta (deg)
`
`r
`
`i
`
`1
`
`1
`
`1
`30
`
`1
`
`1
`
`1
`
`1
`
`1
`
`1
`
`I
`
`1
`
`9
`35
`
`Page 33 of 44
`
`
`
`Full-2-13-134-1x.difj Duplicate scan Bihovsky 13-134-1x
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, I(p)=50000, 01/14/22 12:55p
`PEAK: 45(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`
`Peak Search Report
`
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alphal)
`A% FWHM
`H%
`Area
`BG Height
`56.6
`0.251
`77.3 853769
`884 37895
`13.9
`0.256
`18.7 210232
`916
`9172
`0.273
`13.2 158375
`10.5
`928
`6484
`0.343
`952 49048 100.0 1508669 100.0
`0.496
`64.1
`44.4 967620
`961 21792
`68.4
`0.442
`53.1 1031562
`961 26051
`0.183
`3.8
`6.7
`57236
`960
`3286
`17.4
`0.373
`16.0 262418
`7858
`959
`0.542
`55.6
`35.2 838168
`958 17273
`0.458
`18.2 366342
`24.3
`954
`8934
`0.553
`17.4 447780
`29.7
`947
`8510
`0.427
`30.9 579905
`38.4
`946 15142
`
`d(A)
`2-Theta
`7.973 11.0805
`11.598
`7.6237
`6.9728
`12.685
`15.687
`5.6446
`4.6232
`19.182
`19.547
`4.5377
`4.1961
`21.156
`4.1277
`21.511
`3.9819
`22.309
`3.6980
`24.045
`3.2692
`27.256
`3.2447
`27.466
`
`#
`1
`2
`3
`4
`5
`; 6
`7
`8
`9
`10
`11
`12
`
`19. 47°
`
`19.1 F °
`
`22.309°
`
`271166°
`
`4.
`
`45°
`
`7
`
`.
`
`21151
`
`21.1
`
`6°
`
`15.C87°
`
`7. 73°
`
`11,598
`
`12
`
`85°
`
`.
`
`.
`10
`
`15
`
`,
`
`,
`
`1
`
`1
`
`i
`
`,
`1
`25
`20
`Two-Theta (deg)
`
`1
`
`1-
`
`1
`
`1
`
`1
`30
`
`1
`
`1
`
`1
`
`1
`
`1
`
`1
`
`1
`
`1
`
`1
`35
`
`Page 34 of 44
`
`
`
`Peak Search Report
`
`[Full-3-13-134-1x.dif] Triplicate scan Bihovsky 13-134-1x
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, l(p)=50000, 01/14/22 01:13p
`PEAK: 45(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alpha1)
`A% FWHM
`Area
`H%
`BG Height
`d(A)
`2-Theta
`#
`0.268
`45.4
`52.9 626282
`787 26041
`7.973 11.0799
`1
`0.262
`10.0
`11.9 137323
`5852
`781
`7.6267
`11.594
`2
`0.272
`8.6
`9.9 1 1 8437
`4868
`783
`6.9771
`12.677
`3
`0.313
`775 49225 100.0 1379425 100.0
`5.6438
`15.689
`4
`0.483
`61.5
`39.9 848601
`768 19627
`4.6185
`19.202
`5
`0.369
`34.0
`28.8 468926
`768 14177
`4.5389
`19.542
`6
`0.228
`5.0
`69522
`6.5
`3180
`767
`4.1893
`21.191
`7
`0.434
`15.6
`11.2 214595
`5515
`766
`4.1294
`21.502
`8
`0.587
`54.9
`29.3 757868
`766 14419
`3.9835
`22.299
`9
`0.444
`21.6
`15.2 297351
`7479
`766
`3.7001
`24.032
`10
`0.443
`24.7
`16.4 340519
`8079
`768
`3.2662
`27.283
`11
`0.521
`33.5
`20.1 462000
`9898
`769
`3.2442
`27.471
`12
`
`7.
`
`73°
`
`11.594
`
`J
`
`5
`
`10
`
`19.202°
`
`[
`1542°
`
`1
`
`2. 99°
`
`27.
`27*
`
`71°
`3°
`
`24.032°
`
`21:52
`21.11:1°
`
`V
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Page 35 of 44
`
`
`
`Peak Search Report
`
`[Full-13-137-1x.dif] Bihovsky 13-137-1x
`SCAN: 2.9913/39.9922/0.01313/97.92(sec), Cu, l(p)=50000, 01/14/22 09:33a
`PEAK: 41(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alphal)
`A% FWHM
`Area
`H%
`BG Height
`d(A)
`#
`2-Theta
`0.261
`39.9
`44.0 504069
`7.952 11.1086 1006 21531
`1
`0.261
`9.0
`10.0 114096
`4882
`7.6379 1004
`11.576
`2
`0.270
`8.4
`9.0 106831
`4412
`6.9894 1005
`12.655
`3
`0.288
`5.6551 1011 48989 100.0 1264831 100.0
`15.658
`4
`0.386
`48.5
`36.2 613423
`4.6264 1013 17758
`19.169
`5
`0.648
`52.6
`23.4 664982
`4.5427 1012 11446
`19.525
`6
`0.154
`3.0
`37967
`4.9
`2423
`4.1972 1007
`21.150
`7
`0.374
`13.3
`10.2 168182
`5021
`4.1302 1005
`21.497
`8
`0.577
`52.6
`26.3 665526
`3.9840 1002 12875
`22.296
`9
`0.395
`18.8
`13.7 238197
`6726
`994
`3.7050
`24.000
`10
`0.443
`18.8
`11.3 237428
`5544
`979
`3.2739
`27.217
`11
`0.434
`26.8
`17.8 339073
`8719
`978
`3.2486
`27.433
`12
`
`15.658°
`
`19.109°
`
`
`
`pI
`
`7. 52°
`
`2.
`
`96°
`
`1
`
`525°
`
`24.
`
`00°
`
`21.k39
`
`21.1
`
`0°
`
`27.333°
`
`7.
`
`7°
`
`it
`
`11.76`
`
`, \I
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`40
`
`Page 36 of 44
`
`
`
`Peak Search Report
`
`[full-2-13-137-1x.clif] Duplicate scan Bihovsky 13-137-1x
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, I(p)=50000, 01/14/22 01:00p
`PEAK: 43(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alphal)
`A% FWHM
`Area
`H%
`BG Height
`d(A)
`2-Theta
`#
`0.244
`45.4
`53.9 582025
`708 26581
`7.961 11.0961
`1
`0.246
`10.1
`11.9 129556
`5867
`718
`7.6325
`11.585
`2
`0.271
`9.6
`10.3 123165
`5065
`718
`6.9805
`12.671
`3
`0.290
`717 49283 100.0 1282099 100.0
`5.6497
`15.673
`4
`63.1
`0.474
`38.6 809014
`720 19032
`4.6232
`19.182
`5
`0.468
`49.4
`30.6 632959
`721 15085
`4.5390
`19.541
`6
`0.208
`5.1
`65562
`6.7
`3314
`724
`4.1891
`21.192
`7
`0.386
`15.0
`11.3 192133
`5549
`724
`4.1336
`21.480
`8
`0.573
`53.2
`26.9 682166
`726 13277
`3.9810
`22.313
`9
`0.415
`20.8
`14.6 267314
`7195
`730
`3.7029
`24.013
`10
`0.478
`22.0
`12.6 281741
`6195
`737
`3.2723
`27.230
`11
`0.449
`31.7
`19.3 406437
`9509
`737
`3.2446
`27.467
`12
`
`15.¢73°
`1
`
`- 1---
`
`r
`
`7. 61°
`
`11.585
`
`il
`
`L-,...)
`
`10
`
`19.162°
`i
`1
`
`1
`
`41°
`
`22. 13°
`
`27.67°
`
`24.013°
`
`7.
`
`21348
`
`. 21.1
`
`15
`
`,,
`
`.
`.
`25
`20
`Two-Theta (deg)
`
`f
`
`I
`
`i
`
`l
`
`,
`
`i
`
`30
`
`I
`
`I
`
`I
`
`I
`
`T
`35
`
`Page 37 of 44
`
`
`
`[Full-3-13-137-1x.dif] Triplicate Scan Bihovsky 13-137-1x
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, l(p)=50000, 01/14/22 01:17p
`
`Peak Search Report
`
`PEAK: 45(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alphal)
`
`#
`1
`2
`3
`4
`5
`6
`7
`8
`9
`10
`11
`12
`
`d(A)
`2-Theta
`7.956 11.1034
`11.583
`7.6334
`12.666
`6.9830
`15.679
`5.6473
`19.181
`4.6235
`4.5364
`19.553
`21.185
`4.1904
`21.499
`4.1299
`3.9813
`22.312
`3.7026
`24.015
`3.2646
`27.296
`27.464
`3.2450
`
`A% FWHM
`Area
`H%
`BG Height
`42.3
`0.245
`51.8 559923
`706 25559
`10.3
`0.256
`12.0 136011
`697
`5919
`8.7
`0.267
`9.8 115492
`691
`4823
`671 49329 100.0 1323644 100.0
`0.299
`0.412
`38.6 702169
`53.0
`649 19041
`44.9
`0.453
`29.7 594650
`646 14662
`65937
`5.0
`0.211
`637
`3286
`6.7
`12.6 210442
`15.9
`0.379
`636
`6200
`0.572
`29.2 738291
`55.8
`632 14414
`0.423
`15.5 289955
`21.9
`7642
`625
`0.457
`16.4 346858
`26.2
`8084
`617
`0.476
`21.3 449401
`34.0
`617 10527
`
`15.979°
`
`7. 56°
`
`1
`
`11.583
`
`19.181°
`
`1
`p53°
`
`1
`
`22.
`
`12°
`
`27.464°
`
`24 15°
`
`27.
`
`6°
`
`11
`
`11
`
`
`
`21 41
`
`t
`
`21.T
`
`°
`
`.r,.
`.,i
`
`,
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`I
`
`[
`
`1
`
`1
`
`1
`
`1
`
`1
`
`1
`30
`
`'
`35
`
`1
`
`1
`
`[
`
`i
`
`Page 38 of 44
`
`
`
`[Full-13-143-1x.dif] Bihovsky 13-143-1x
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, l(p)=50000, 01/14/22 09:34a
`
`- 1 Peak Search Report]
`
`PEAK: 41(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alphal)
`
`#
`1
`2
`3
`4
`5
`6
`7
`8 4
`9
`10
`11
`
`A% FWHM
`Area
`H%
`BG Height
`d(A)
`2-Theta
`67.7
`0.242
`89.4 938991
`7.947 11.1166 1586 43310
`15.4
`0.261
`18.8 213358
`11.576
`7.6380 1591
`9111
`15.0
`0.273
`17.6 208567
`12.654
`6.9897 1586
`8541
`5.6519 1566 48434 100.0 1386716 100.0
`0.320
`15.667
`70.4
`0.544
`4.6273 1541 19997
`41.3 975580
`19.165
`39.2 898613
`64.8
`0.528
`19.511
`4.5461 1539 19007
`3544
`7.3
`54773
`3.9
`0.151
`21.154
`4.1965 1532
`19.2
`0.357
`4.1339 1531
`8331
`17.2 266715
`21.478
`33.0 790050
`57.0
`0.551
`22.303
`3.9828 1528 15991
`19.1 329974
`23.8
`0.399
`9232
`3.7048 1525
`24.001
`0.507
`6456
`13.3 311769
`22.5
`27.191
`3.2770 1524
`
`---I
`
`7. 47°
`
`15.G7°
`
`it
`
`19.15°
`
`22.103°
`
`L 24.601°
`
`21A7
`
`1
`
`21.1
`
`4°
`
`11. 76
`
`5
`
`0
`
`•
`
`15
`
`7
`
`1
`
`1
`
`1
`
`1
`
`25
`20
`Two-Theta (deg)
`
`1
`
`i
`
`1
`
`I
`
`T
`
`30
`
`i
`
`i
`
`1
`
`i
`
`l
`
`35
`
`Page 39 of 44
`
`
`
`[Full-2-13-143-1x.dit] Duplicate scan Bihovsky 13-143-1x
`
`Peak Search Report
`
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, I(p)=50000, 01/14/22 01:05p
`
`PEAK: 43(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alphal)
`A% FWHM
`H%
`Area
`BG Height
`d(A)
`2-Theta
`0.247
`67.6 736525
`56.7
`7.938 11.1282
`897 33224
`13.5 150602
`11.6
`0.253
`7.6509
`900
`6633
`11.557
`0.270
`13.4 159517
`12.3
`12.644
`6.9953
`888
`6595
`0.295
`864 49136 100.0 1298705 100.0
`15.663
`5.6531
`0.464
`40.2 819765
`63.1
`4.6235
`850 19734
`19.181
`0.639
`30.9 869532
`67.0
`850 15180
`4.5492
`19.497
`6.6
`0.191
`9.7
`86296
`848
`4754
`21.195
`4.1885
`20.0
`0.436
`13.5 259872
`848
`6657
`21.438
`4.1416
`0.593
`30.1 786122
`60.5
`849 14803
`22.298
`3.9837
`0.445
`27.0
`17.9 351058
`851
`8797
`23.987
`3.7070
`0.402
`16.4 308248
`23.7
`8045
`3.2723
`863
`27.230
`36.3
`0.484
`22.1 471299
`864 10877
`3.2520
`27.403
`
`#
`1
`----
`2
`3
`4
`5
`6
`7
`8
`9
`10
`11
`12
`
`-
`
`-- 1
`
`7. 38°
`
`19.1€31°
`
`9 '
`
`2.498°
`
`11.5571
`
`i
`
`21
`3
`21.11 °
`
`23.
`
`87°
`
`27.1103°
`
`7
`
`0°
`
`.
`
`.
`
`.
`
`.
`
`.
`
`.
`
`•
`.
`15
`
`.
`
`,
`
`T
`
`1
`25
`20
`Two-Theta (deg)
`
`1
`
`1
`
`1
`
`1
`
`1
`30
`
`IM
`
`!
`
`T
`35
`
`Page 40 of 44
`
`
`
`Full-3-13-143-1x.difj Triplicate scan Bihovsky 13-143-1x
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, l(p)=50000, 01/14/22 01:23p
`
`Peak Search Report
`
`PEAK: 43(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alphal)
`Area
`A% FWHM
`H%
`BG Height
`54.9
`0.238
`72.0 753105
`842 35376
`14.2 162223
`11.8
`0.259
`828
`7001
`14.6 193721
`14.1
`0.302
`7152
`834
`844 49156 100.0 1371258 100.0
`0.311
`0.480
`56.4
`36.6 773011
`836 17974
`0.440
`44.6
`31.6 611116
`835 15514
`5.9
`0.218
`8.0
`81279
`831
`3917
`0.343
`15.7 236974
`17.3
`7705
`831
`0.582
`29.8 764609
`55.8
`830 14665
`0.427
`16.7 314312
`22.9
`830
`8223
`0.489
`12.6 287889
`21.0
`6181
`833
`31.7
`0.478
`20.7 435289
`834 10171
`
`d(A)
`2-Theta
`7.967 11.0878
`11.592
`7.6275
`12.694
`6.9679
`5.6493
`15.674
`19.188
`4.6218
`4.5369
`19.551
`4.1838
`21.219
`21.500
`4.1297
`22.315
`3.9806
`3.7024
`24.017
`3.2739
`27.217
`3.2448
`27.466
`
`#
`1
`2
`3
`4
`5
`6
`7
`8
`9
`10
`11
`12
`
`_1
`
`19.48°
`
`1051°
`
`2.
`
`15°
`
`27.466°
`
`7. 7°
`
`21
`
`00'
`
`24.
`
`17°
`
`1.
`
`7. 67°
`
`12. 94°
`
`10
`
`15
`
`r
`
`I
`
`I
`
`i
`
`i
`
`25
`20
`Two-Theta (deg)
`
`I
`
`1
`
`1
`
`r
`
`1
`
`1
`
`1
`
`30
`
`1
`
`1
`
`1
`
`1
`
`1
`
`1
`
`1
`
`1
`
`1
`
`35
`
`Page 41 of 44
`
`
`
`Peak Search Report
`
`[Full-13-144-1x.dif] Bihovsky 13-144-1x
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, l(p)=50000, 01/14/22 09:34a
`PEAK: 45(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alphal)
`A% FWHM
`Area
`H%
`BG Height
`d(A)
`# I 2-Theta
`0.226
`39.9
`50.5 496815
`7.926 11.1450 1488 24527
`1
`0.243
`10.1
`11.8 125175
`5737
`7.6587 1475
`11.545
`2
`0.264
`10.0
`10.9 124962
`7.0031 1472
`5277
`12.630
`3
`0.286
`5.6660 1466 48534 100.0 1243972 100.0
`15.627
`4
`0.433
` 50.7
`33.5 631298
`4.6371 1466 16281
`19.124
`5
`0.417
`40.1
`27.5 498868
`4.5504 1466 13339
`19.492
`6
`0.243
`7.9
`98293
`8.8
`4249
`4.1885 1468
`21.195
`7
`0.748
`35.1
`13.0 436824
`6326
`4.1216 1468
`21.543
`8
`0.576
`53.2
`26.4 661440
`3.9909 1470 12819
`22.257
`9
`0.387
`19.6
`14.5 243403
`7025
`3.7072 1473
`23.985
`10
`0.433
`25.1
`15.6 311673
`7558
`3.2667 1479
`27.278
`11
`0.425
`26.1
`16.5 324088
`8005
`3.2458 1479
`27.457
`12
`
`15.627°
`
`7. 26°
`
`19.14°
`
`1 92°
`1.
`
`2. 57°
`
`II
`
`11. 45
`
`27.}57°
`
`21i54
`
`23.985°
`
`21.1
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Page 42 of 44
`
`
`
`[Full-2-13-144-1x.dif] Duplicate scan Bihovsky 13-144-1x
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, I(p)=50000, 01/14/22 01:09p
`
`Peak Search Report
`
`PEAK: 39(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alphal)
`i
`A% FWHM
`Area
`H%
`BG Height
`d(A)
`# 1 2-Theta
`36.4
`0.258
`40.8 460714
`7.949 11.1127 1082 19959
`1 1
`1.8 U2b9
`8.1
`991)1 (
`4274
`2
`11.567
`7.6443 1048
`0.275
`8.6
`9.1 109239
`6.9904 1051
`4436
`12.653
`3
`5.6578 1073 48927 100.0 1265127 100.0
`0.289
`4
`15.650
`52.8
`0.430
`35.4 668097
`4.6346 1085 17342
`5
`19.134
`44.2
`0.567
`22.5 559514
`4.5418 1087 11015
`6
`19.529
`79812
`6.3
`0.241
`3486
`4.1906 1093
`7.1
`21.184
`7
`0.416
`11.6 211279
`16.7
`4.1322 1094
`5668
`21.487
`8
`61.0
`0.613
`28.7 771273
`3.9831 1096 14047
`22.301
`9
`0.444
`23.2
`15.1 293615
`7378
`3.7066 1102
`23.989
`10
`0.421
`12.3 241872
`19.1
`6029
`3.2739 1114
`27.217
`11
`29.7
`0.481
`8736
`17.9 376188
`3.2494 1114
`12
`27.426
`
`-45150°
`
`7.949°
`
`19.14°
`
`1 p29°
`
`22.
`
`01°
`
`12
`
`53°
`
`21.48
`
`,
`
`21.1!
`
`4°
`
`23.989°
`
`27.
`
`26°
`
`7.
`
`°
`
`1
`_L,___.,
`
`• .
`
`_,...
`
`.1,-
`
`' 110
`
`'
`
`'
`
`i
`
`rH
`
`I
`
`I
`
`I
`
`1
`
`15
`
`25
`20
`Two-Theta (deg)
`
`,
`
`1
`
`,___
`
`I
`
`T
`
`30
`
`I
`
`Mi
`
`l
`
`l
`
`i
`
`'
`
`35
`
`Page 43 of 44
`
`
`
`[Full-3-13-144-1x.dif] triplicate scan Bihovsky 13-144-1x
`
`Peak Search Report
`
`SCAN: 2.9913/39.9925/0.01313/97.92(sec), Cu, l(p)=50000, 01/14/22 01:27p
`
`PEAK: 45(pts)/Parabolic Filter, Threshold=1.0, Cutoff=0.1%, BG=3/1.0, Peak-Top=Centroid Fit
`
`NOTE: Intensity = Counts, 2T(0)=0.0(deg), Wavelength to Compute d-Spacing = 1.54059A (Cu/K-alpha1)
`
`#
`1
`2
`3
`4
`5
`6
`7
`8
`9
`10
`11
`12
`
`d(A)
`2-Theta
`7.956 11.1036
`11.575
`7.6390
`12.660
`6.9866
`15.658
`5.6549
`19.154
`4.6299
`19.535
`4.5405
`21.174
`4.1926
`21.572
`4.1160
`22.299
`3.9835
`24.005
`3.7042
`3.2692
`27.257
`27.431
`3.2488
`
`A% FWHM
`Area
`H%
`BG Height
`45.0
`0.257
`53.9 609668
`865 26510
`9.6
`0.259
`11.4 129776
`856
`5590
`9.4
`0.262
`11.0 127003
`855
`5400
`861 49139 100.0 1354664 100.0
`0.308
`878 17769
`36.2 750489
`55.4
`0.471
`880 13484
`27.4 675556
`49.9
`0.559
`890
`3544
`7.2
`90366
`6.7
`0.268
`892
`6819
`13.9 422450
`31.2
`0.691
`29.0 761418
`56.2
`0.596
`896 14270
`15.7 300552
`22.2
`0.436
`905
`7698
`14.8 327848
`24.2
`0.473
`917
`7278
`0.489
`9360
`19.0 410064
`30.3
`918
`
`7. 56°
`
`19.14°
`1
`p35.
`
`1
`
`99'
`
`11.575
`
`27.
`27.
`
`31°
`70
`
`24.905°
`
`
`
`21 57
`
`•
`
`21.14° I
`
`5
`
`10
`
`15
`
`25
`20
`Two-Theta (deg)
`
`30
`
`35
`
`Page 44 of 44
`
`
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