Changeset 3073 for Tutorials/TOF Single Crystal Refinement/TOF single crystal refinement in GSAS.htm
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TabularUnified Tutorials/TOF Single Crystal Refinement/TOF single crystal refinement in GSAS.htm ¶
r2390 r3073 24 24 <o:DocumentProperties> 25 25 <o:Author>vondreele</o:Author> 26 <o:LastAuthor> Von Dreele</o:LastAuthor>27 <o:Revision>1 2</o:Revision>28 <o:TotalTime>10 31</o:TotalTime>26 <o:LastAuthor>vondreele</o:LastAuthor> 27 <o:Revision>14</o:Revision> 28 <o:TotalTime>1085</o:TotalTime> 29 29 <o:Created>2015-02-17T16:18:00Z</o:Created> 30 <o:LastSaved>201 6-07-28T18:57:00Z</o:LastSaved>30 <o:LastSaved>2017-09-13T16:56:00Z</o:LastSaved> 31 31 <o:Pages>1</o:Pages> 32 <o:Words> 2061</o:Words>33 <o:Characters>1 1753</o:Characters>32 <o:Words>1889</o:Words> 33 <o:Characters>10773</o:Characters> 34 34 <o:Company>Argonne National Laboratory</o:Company> 35 <o:Lines> 97</o:Lines>36 <o:Paragraphs>2 7</o:Paragraphs>37 <o:CharactersWithSpaces>1 3787</o:CharactersWithSpaces>35 <o:Lines>89</o:Lines> 36 <o:Paragraphs>25</o:Paragraphs> 37 <o:CharactersWithSpaces>12637</o:CharactersWithSpaces> 38 38 <o:Version>16.00</o:Version> 39 39 </o:DocumentProperties> … … 48 48 <!--[if gte mso 9]><xml> 49 49 <w:WordDocument> 50 <w:View>Print</w:View> 51 <w:Zoom>124</w:Zoom> 50 52 <w:SpellingState>Clean</w:SpellingState> 51 53 <w:GrammarState>Clean</w:GrammarState> … … 650 652 {font-family:"Cambria Math"; 651 653 panose-1:2 4 5 3 5 4 6 3 2 4; 652 mso-font-charset: 1;654 mso-font-charset:0; 653 655 mso-generic-font-family:roman; 654 656 mso-font-pitch:variable; 655 mso-font-signature: 0 0 0 0 00;}657 mso-font-signature:-536870145 1107305727 0 0 415 0;} 656 658 @font-face 657 659 {font-family:Calibri; … … 660 662 mso-generic-font-family:swiss; 661 663 mso-font-pitch:variable; 662 mso-font-signature:-5368 70145 1073786111 1 0 4150;}664 mso-font-signature:-536859905 -1073732485 9 0 511 0;} 663 665 @font-face 664 666 {font-family:Cambria; … … 1115 1117 font-family:"Calibri",sans-serif; 1116 1118 mso-fareast-font-family:"Times New Roman"; 1117 mso-fareast-theme-font:minor-fareast; 1118 mso-bidi-font-family:Calibri;} 1119 mso-fareast-theme-font:minor-fareast;} 1119 1120 span.SpellE 1120 1121 {mso-style-name:""; … … 1229 1230 1230 1231 <p class=MsoNormal>In these exercises you will use GSAS-II to refine the 1231 structure of sapphire (really corundum, Al<sub>2</sub>O<sub>3</sub>) from single1232 crystal diffraction data collected at the SNS on the TOPAZ instrument at room 1233 temperature. The data consists of a suite of exposures with the crystal in 31 1234 different orientations all within a single data file. Note that menu entries1232 structure of sapphire (really corundum, Al<sub>2</sub>O<sub>3</sub>) from 1233 single crystal diffraction data collected at the SNS on the TOPAZ instrument at 1234 room temperature. The data consists of a suite of exposures with the crystal in 1235 31 different orientations all within a single data file. Note that menu entries 1235 1236 and user input are shown in bold face below as <b style='mso-bidi-font-weight: 1236 1237 normal'><span style='font-family:"Calibri",sans-serif;mso-ascii-theme-font: 1237 minor-latin;mso-hansi-theme-font:minor-latin;mso-bidi-font-family:Calibri; 1238 mso-bidi-theme-font:minor-latin'>Help/About GSAS-II</span></b>, which lists 1239 first the name of the menu (here <b style='mso-bidi-font-weight:normal'><span 1240 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1241 mso-hansi-theme-font:minor-latin;mso-bidi-font-family:Calibri;mso-bidi-theme-font: 1238 minor-latin;mso-hansi-theme-font:minor-latin;mso-bidi-theme-font:minor-latin'>Help/About 1239 GSAS-II</span></b>, which lists first the name of the menu (here <b 1240 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1241 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin;mso-bidi-theme-font: 1242 1242 minor-latin'>Help</span></b>) and second the name of the entry in the menu 1243 1243 (here <b style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1244 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin;mso-bidi- font-family:1245 Calibri;mso-bidi-theme-font:minor-latin'>About GSAS-II</span></b>). If you have 1246 not done so already, startGSAS-II.</p>1244 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin;mso-bidi-theme-font: 1245 minor-latin'>About GSAS-II</span></b>). If you have not done so already, start 1246 GSAS-II.</p> 1247 1247 1248 1248 <h2>Step 1. Setup the phase information for sapphire</h2> … … 1252 1252 style='font:7.0pt "Times New Roman"'> </span></span></span><![endif]>Use 1253 1253 the <b style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1254 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin;mso-bidi-font-family: 1255 Calibri;mso-bidi-theme-font:minor-latin'>Data/Add phase</span></b> menu item 1256 add a new phase into the current GSAS-II project. A popup window will appear 1257 asking for a phase name; I entered <b style='mso-bidi-font-weight:normal'><span 1258 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1259 mso-hansi-theme-font:minor-latin'>sapphire</span></b>; press <b 1260 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1254 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin;mso-bidi-theme-font: 1255 minor-latin'>Data/Add new phase</span></b> menu item add a new phase into the 1256 current GSAS-II project. A popup window will appear asking for a phase name; I 1257 entered <b style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1258 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>sapphire</span></b>; 1259 press <b style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1261 1260 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>OK</span></b> 1262 1261 when done. Select <b style='mso-bidi-font-weight:normal'><span … … 1285 1284 <v:path o:extrusionok="f" gradientshapeok="t" o:connecttype="rect"/> 1286 1285 <o:lock v:ext="edit" aspectratio="t"/> 1287 </v:shapetype><v:shape id="Picture_x0020_ 1" o:spid="_x0000_i1050" type="#_x0000_t75"1288 style='width: 640.5pt;height:375pt;visibility:visible;mso-wrap-style:square'>1286 </v:shapetype><v:shape id="Picture_x0020_27" o:spid="_x0000_i1050" type="#_x0000_t75" 1287 style='width:468pt;height:209.25pt;visibility:visible;mso-wrap-style:square'> 1289 1288 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image001.png" 1290 1289 o:title=""/> 1291 </v:shape><![endif]--><![if !vml]><img width= 854 height=5001292 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 51.gif"1293 v:shapes="Picture_x0020_ 1"><![endif]></span></p>1290 </v:shape><![endif]--><![if !vml]><img width=624 height=279 1291 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image002.gif" 1292 v:shapes="Picture_x0020_27"><![endif]></span></p> 1294 1293 1295 1294 <p class=MsoListParagraph><o:p> </o:p></p> … … 1310 1309 1311 1310 <p class=MsoListParagraph><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1312 id="Picture_x0020_2 9" o:spid="_x0000_i1049" type="#_x0000_t75" style='width:487.5pt;1313 height: 375pt;visibility:visible;mso-wrap-style:square'>1311 id="Picture_x0020_28" o:spid="_x0000_i1049" type="#_x0000_t75" style='width:468pt; 1312 height:265.5pt;visibility:visible;mso-wrap-style:square'> 1314 1313 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image003.png" 1315 1314 o:title=""/> 1316 </v:shape><![endif]--><![if !vml]><img width=6 50 height=5001317 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 52.gif"1318 v:shapes="Picture_x0020_2 9"><![endif]></span></p>1315 </v:shape><![endif]--><![if !vml]><img width=624 height=354 1316 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image004.gif" 1317 v:shapes="Picture_x0020_28"><![endif]></span></p> 1319 1318 1320 1319 <p class=MsoListParagraph><o:p> </o:p></p> … … 1325 1324 <b style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1326 1325 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>4.7613</span></b> 1327 for <span class=GramE>a </span> and<b style='mso-bidi-font-weight:normal'><span1326 for <span class=GramE>a and</span> <b style='mso-bidi-font-weight:normal'><span 1328 1327 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1329 1328 mso-hansi-theme-font:minor-latin'>12.9846</span></b> for c; a new cell volume … … 1337 1336 tab; it will be empty. Do <b style='mso-bidi-font-weight:normal'><span 1338 1337 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1339 mso-hansi-theme-font:minor-latin'>Edit /Append atom</span></b> from the <b1338 mso-hansi-theme-font:minor-latin'>Edit Atoms/Append atom</span></b> from the <b 1340 1339 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1341 1340 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>Phase Data … … 1343 1342 1344 1343 <p class=MsoListParagraph><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1345 id="Picture_x0020_ 31" o:spid="_x0000_i1048" type="#_x0000_t75" style='width:525pt;1346 height: 225pt;visibility:visible;mso-wrap-style:square'>1344 id="Picture_x0020_29" o:spid="_x0000_i1048" type="#_x0000_t75" style='width:468pt; 1345 height:153.75pt;visibility:visible;mso-wrap-style:square'> 1347 1346 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image005.png" 1348 1347 o:title=""/> 1349 </v:shape><![endif]--><![if !vml]><img width= 700 height=3001350 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 53.gif"1351 v:shapes="Picture_x0020_ 31"><![endif]></span></p>1348 </v:shape><![endif]--><![if !vml]><img width=624 height=205 1349 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image006.gif" 1350 v:shapes="Picture_x0020_29"><![endif]></span></p> 1352 1351 1353 1352 <p class=MsoListParagraph style='text-indent:-.25in;mso-list:l0 level1 lfo2'><![if !supportLists]><span … … 1362 1361 1363 1362 <p class=MsoListParagraph><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1364 id="Picture_x0020_3 2" o:spid="_x0000_i1047" type="#_x0000_t75" style='width:525pt;1365 height: 225pt;visibility:visible;mso-wrap-style:square'>1363 id="Picture_x0020_30" o:spid="_x0000_i1047" type="#_x0000_t75" style='width:468pt; 1364 height:153.75pt;visibility:visible;mso-wrap-style:square'> 1366 1365 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image007.png" 1367 1366 o:title=""/> 1368 </v:shape><![endif]--><![if !vml]><img width= 700 height=3001369 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 54.gif"1370 v:shapes="Picture_x0020_3 2"><![endif]></span></p>1367 </v:shape><![endif]--><![if !vml]><img width=624 height=205 1368 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image008.gif" 1369 v:shapes="Picture_x0020_30"><![endif]></span></p> 1371 1370 1372 1371 <p class=MsoListParagraph style='text-indent:-.25in;mso-list:l0 level1 lfo2'><![if !supportLists]><span 1373 1372 style='mso-fareast-font-family:"Times New Roman"'><span style='mso-list:Ignore'>6.<span 1374 1373 style='font:7.0pt "Times New Roman"'> </span></span></span><![endif]>Change 1375 the Al(z) to <b style='mso-bidi-font-weight:normal'><span style='font-family: 1374 the <span class=GramE>Al(</span>z) to <b style='mso-bidi-font-weight:normal'><span 1375 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1376 mso-hansi-theme-font:minor-latin'>0. 352</span></b>, the O(x) to <b 1377 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1378 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>-0.306</span></b> 1379 and the O(z) to <b style='mso-bidi-font-weight:normal'><span style='font-family: 1376 1380 "Calibri",sans-serif;mso-ascii-theme-font:minor-latin;mso-hansi-theme-font: 1377 minor-latin'>0. 352</span></b>, the O(x) to <b style='mso-bidi-font-weight: 1378 normal'><span style='font-family:"Calibri",sans-serif;mso-ascii-theme-font: 1379 minor-latin;mso-hansi-theme-font:minor-latin'>-0.306</span></b> and the O(z) to 1380 <b style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1381 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>Œ</span></b> 1382 (it will be changed to 0.2500). Site symmetries and multiplicities will 1383 automatically change for these positions.</p> 1381 minor-latin'>Œ</span></b> (it will be changed to 0.2500). Also set both <span 1382 class=SpellE>Uiso</span> to <b style='mso-bidi-font-weight:normal'><span 1383 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1384 mso-hansi-theme-font:minor-latin;mso-bidi-theme-font:minor-latin'>0.005</span></b>. 1385 Site symmetries and multiplicities will automatically change for these 1386 positions.</p> 1384 1387 1385 1388 <p class=MsoListParagraph><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1386 id="Picture_x0020_3 4" o:spid="_x0000_i1046" type="#_x0000_t75" style='width:525pt;1387 height: 225pt;visibility:visible;mso-wrap-style:square'>1389 id="Picture_x0020_31" o:spid="_x0000_i1046" type="#_x0000_t75" style='width:468pt; 1390 height:153.75pt;visibility:visible;mso-wrap-style:square'> 1388 1391 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image009.png" 1389 1392 o:title=""/> 1390 </v:shape><![endif]--><![if !vml]><img width= 700 height=3001391 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 55.gif"1392 v:shapes="Picture_x0020_3 4"><![endif]></span></p>1393 </v:shape><![endif]--><![if !vml]><img width=624 height=205 1394 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image010.gif" 1395 v:shapes="Picture_x0020_31"><![endif]></span></p> 1393 1396 1394 1397 <p class=MsoListParagraph><o:p> </o:p></p> … … 1438 1441 1439 1442 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1440 id="Picture_x0020_3 5" o:spid="_x0000_i1045" type="#_x0000_t75" style='width:240pt;1441 height:2 32.5pt;visibility:visible;mso-wrap-style:square'>1443 id="Picture_x0020_32" o:spid="_x0000_i1045" type="#_x0000_t75" style='width:233.25pt; 1444 height:228.75pt;visibility:visible;mso-wrap-style:square'> 1442 1445 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image011.png" 1443 1446 o:title=""/> 1444 </v:shape><![endif]--><![if !vml]><img width=3 20 height=3101445 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 56.gif"1446 v:shapes="Picture_x0020_3 5"><![endif]></span></p>1447 </v:shape><![endif]--><![if !vml]><img width=311 height=305 1448 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image012.gif" 1449 v:shapes="Picture_x0020_32"><![endif]></span></p> 1447 1450 1448 1451 <p class=MsoNormal>This makes the connection between the data you just read and … … 1458 1461 1459 1462 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1460 id="Picture_x0020_3 6" o:spid="_x0000_i1044" type="#_x0000_t75" style='width:300pt;1461 height:1 87.5pt;visibility:visible;mso-wrap-style:square'>1463 id="Picture_x0020_33" o:spid="_x0000_i1044" type="#_x0000_t75" style='width:468pt; 1464 height:153.75pt;visibility:visible;mso-wrap-style:square'> 1462 1465 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image013.png" 1463 1466 o:title=""/> 1464 </v:shape><![endif]--><![if !vml]><img width= 400 height=2501465 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 57.gif"1466 v:shapes="Picture_x0020_3 6"><![endif]></span></p>1467 1468 <p class=MsoNormal>The plot window shows a not very interesting 2D view of the l=01469 l ayer of reciprocal space for the last data set. If you select the 1<sup>st</sup>1467 </v:shape><![endif]--><![if !vml]><img width=624 height=205 1468 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image014.gif" 1469 v:shapes="Picture_x0020_33"><![endif]></span></p> 1470 1471 <p class=MsoNormal>The plot window shows a not very interesting 2D view of the 1472 l=0 layer of reciprocal space for the last data set. If you select the 1<sup>st</sup> 1470 1473 HKLF entry (<b style='mso-bidi-font-weight:normal'><span style='font-family: 1471 1474 "Calibri",sans-serif;mso-ascii-theme-font:minor-latin;mso-hansi-theme-font: … … 1474 1477 1475 1478 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1476 id="Picture_x0020_ 10" o:spid="_x0000_i1043" type="#_x0000_t75" style='width:525pt;1477 height:4 50pt;visibility:visible;mso-wrap-style:square'>1479 id="Picture_x0020_34" o:spid="_x0000_i1043" type="#_x0000_t75" style='width:468pt; 1480 height:401.25pt;visibility:visible;mso-wrap-style:square'> 1478 1481 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image015.png" 1479 1482 o:title=""/> 1480 </v:shape><![endif]--><![if !vml]><img width= 700 height=6001481 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 58.gif"1482 v:shapes="Picture_x0020_ 10"><![endif]></span></p>1483 </v:shape><![endif]--><![if !vml]><img width=624 height=535 1484 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image016.gif" 1485 v:shapes="Picture_x0020_34"><![endif]></span></p> 1483 1486 1484 1487 <p class=MsoNormal>Green circles are drawn representing the magnitude of 4 … … 1499 1502 1500 1503 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1501 id=" _x0000_i1042" type="#_x0000_t75" style='width:363pt;height:311.25pt;1502 visibility:visible;mso-wrap-style:square'>1504 id="Picture_x0020_35" o:spid="_x0000_i1042" type="#_x0000_t75" style='width:468pt; 1505 height:406.5pt;visibility:visible;mso-wrap-style:square'> 1503 1506 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image017.png" 1504 o:title="" croptop="11818f" cropbottom="16324f" cropleft="40001f" 1505 cropright="10518f"/> 1506 </v:shape><![endif]--><![if !vml]><img width=484 height=415 1507 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image059.jpg" 1508 v:shapes="_x0000_i1042"><![endif]></span></p> 1507 o:title=""/> 1508 </v:shape><![endif]--><![if !vml]><img width=624 height=542 1509 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image018.gif" 1510 v:shapes="Picture_x0020_35"><![endif]></span></p> 1509 1511 1510 1512 <p class=MsoNormal>Here the plot has the correct representation for reciprocal 1511 space as sampled by this crystal orientation on TOPAZ. The <b style='mso-bidi-font-weight: 1512 normal'><span style='font-family:"Calibri",sans-serif;mso-ascii-theme-font: 1513 minor-latin;mso-hansi-theme-font:minor-latin'>save as/key</span></b> commands give 1514 you control on the appearance of the plot; the plot responds to zoom/rotate 1515 commands from the mouse. Left mouse button to rotate, right mouse button to 1516 translate, center wheel to rotate about view direction and the wheel to zoom in 1517 or out. One cursor is the view point and the other is the 000 reciprocal space 1518 origin. </p> 1513 space as sampled by this crystal orientation on TOPAZ; the two branches come 1514 from the two detectors on this instrument. The <b style='mso-bidi-font-weight: 1515 normal'><span style='font-family:"Calibri",sans-serif;mso-ascii-theme-font: 1516 minor-latin;mso-hansi-theme-font:minor-latin'>save as/key</span></b> commands 1517 give you control on the appearance of the plot; the plot responds to 1518 zoom/rotate commands from the mouse. Left mouse button to rotate, right mouse 1519 button to translate, center wheel to rotate about view direction and the wheel 1520 to zoom in or out. One cursor is the view point and the other is the 000 1521 reciprocal space origin. </p> 1519 1522 1520 1523 <p class=MsoNormal>If you want to see the entire data set plotted together do <b … … 1532 1535 1533 1536 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1534 id=" _x0000_i1041" type="#_x0000_t75" style='width:365.25pt;height:310.5pt;1535 visibility:visible;mso-wrap-style:square'>1537 id="Picture_x0020_36" o:spid="_x0000_i1041" type="#_x0000_t75" style='width:468pt; 1538 height:402.75pt;visibility:visible;mso-wrap-style:square'> 1536 1539 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image019.png" 1537 o:title="" croptop="12098f" cropbottom="16193f" cropleft="40187f" 1538 cropright="10237f"/> 1539 </v:shape><![endif]--><![if !vml]><img width=487 height=414 1540 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image060.jpg" 1541 v:shapes="_x0000_i1041"><![endif]></span></p> 1540 o:title=""/> 1541 </v:shape><![endif]--><![if !vml]><img width=624 height=537 1542 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image020.gif" 1543 v:shapes="Picture_x0020_36"><![endif]></span></p> 1542 1544 1543 1545 <p class=MsoNormal>Ive rotated the drawing around to show an obvious gap in … … 1552 1554 normal'><span style='font-family:"Calibri",sans-serif;mso-ascii-theme-font: 1553 1555 minor-latin;mso-hansi-theme-font:minor-latin'>Calculate/Refine</span></b> from 1554 the main GSAS-II data tree window menu. This will do an F refinement by 1555 default. A progress bar will appear to show you the residuals as the histograms 1556 are processed. When it finishes and you have accepted the result a plot will 1557 show the l=0 layer for the 1<sup>st</sup> data set.</p> 1556 the main GSAS-II data tree window menu. You will need to save a copy of the 1557 project first; select an appropriate directory and a name (I used sapphire). This 1558 will do an F refinement by default. A progress bar will appear to show you the 1559 residuals as the histograms are processed. When it finishes and you have 1560 accepted the result a plot will show the l=0 layer for the 1<sup>st</sup> data 1561 set.</p> 1558 1562 1559 1563 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1560 id="Picture_x0020_ 11" o:spid="_x0000_i1040" type="#_x0000_t75" style='width:525pt;1561 height:4 50pt;visibility:visible;mso-wrap-style:square'>1564 id="Picture_x0020_43" o:spid="_x0000_i1040" type="#_x0000_t75" style='width:468pt; 1565 height:401.25pt;visibility:visible;mso-wrap-style:square'> 1562 1566 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image021.png" 1563 1567 o:title=""/> 1564 </v:shape><![endif]--><![if !vml]><img width= 700 height=6001565 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 61.gif"1566 v:shapes="Picture_x0020_ 11"><![endif]></span></p>1568 </v:shape><![endif]--><![if !vml]><img width=624 height=535 1569 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image022.gif" 1570 v:shapes="Picture_x0020_43"><![endif]></span></p> 1567 1571 1568 1572 <p class=MsoNormal>Green rings are the observed magnitude, blue rings are the … … 1578 1582 1579 1583 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1580 id="Picture_x0020_ 12" o:spid="_x0000_i1039" type="#_x0000_t75" style='width:369pt;1581 height: 310.5pt;visibility:visible;mso-wrap-style:square'>1584 id="Picture_x0020_44" o:spid="_x0000_i1039" type="#_x0000_t75" style='width:468pt; 1585 height:404.25pt;visibility:visible;mso-wrap-style:square'> 1582 1586 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image023.png" 1583 o:title="" croptop="9828f" cropbottom="18427f" cropleft="38257f" cropright="12033f"/>1584 </v:shape><![endif]--><![if !vml]><img width= 492 height=4141585 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 62.jpg"1586 v:shapes="Picture_x0020_ 12"><![endif]></span></p>1587 o:title=""/> 1588 </v:shape><![endif]--><![if !vml]><img width=624 height=539 1589 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image024.gif" 1590 v:shapes="Picture_x0020_44"><![endif]></span></p> 1587 1591 1588 1592 <p class=MsoNormal>The size of the squares is proportional to the magnitude of <span … … 1605 1609 1606 1610 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1607 id="Picture_x0020_ 16" o:spid="_x0000_i1038" type="#_x0000_t75" style='width:300pt;1608 height: 303pt;visibility:visible;mso-wrap-style:square'>1611 id="Picture_x0020_39" o:spid="_x0000_i1038" type="#_x0000_t75" style='width:468pt; 1612 height:265.5pt;visibility:visible;mso-wrap-style:square'> 1609 1613 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image025.png" 1610 1614 o:title=""/> 1611 </v:shape><![endif]--><![if !vml]><img width= 400 height=4041612 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 63.gif"1613 v:shapes="Picture_x0020_ 16"><![endif]></span></p>1615 </v:shape><![endif]--><![if !vml]><img width=624 height=354 1616 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image026.gif" 1617 v:shapes="Picture_x0020_39"><![endif]></span></p> 1614 1618 1615 1619 <p class=MsoNormal>We can cut to the chase here select <b style='mso-bidi-font-weight: … … 1629 1633 tutorial, you can try the other models and see how they compare. Next do <b 1630 1634 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1631 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>Edit /Copy1635 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>Edit Phase/Copy 1632 1636 selected data</span></b>, pick <b style='mso-bidi-font-weight:normal'><span 1633 1637 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; … … 1651 1655 tab; it will be empty. Do <b style='mso-bidi-font-weight:normal'><span 1652 1656 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1653 mso-hansi-theme-font:minor-latin'>Edit /Add equivalence</span></b>; the1654 following popup will appear</p>1657 mso-hansi-theme-font:minor-latin'>Edit Constr<span class=GramE>./</span>Add 1658 equivalence</span></b>; the following popup will appear</p> 1655 1659 1656 1660 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1657 id=" _x0000_i1037" type="#_x0000_t75" style='width:468.75pt;height:300pt;1658 visibility:visible;mso-wrap-style:square'>1661 id="Picture_x0020_40" o:spid="_x0000_i1037" type="#_x0000_t75" style='width:468pt; 1662 height:299.25pt;visibility:visible;mso-wrap-style:square'> 1659 1663 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image027.png" 1660 1664 o:title=""/> 1661 </v:shape><![endif]--><![if !vml]><img width=625 height=400 1662 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image064.gif" 1663 v:shapes="_x0000_i1037"><![endif]></span></p> 1664 1665 <p class=MsoNormal>Select the line beginning with <span class=GramE><b 1666 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1667 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>0:0:Eg</span></b></span> 1665 </v:shape><![endif]--><![if !vml]><img width=624 height=399 1666 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image028.gif" 1667 v:shapes="Picture_x0020_40"><![endif]></span></p> 1668 1669 <p class=MsoNormal>Select the line beginning with <b style='mso-bidi-font-weight: 1670 normal'><span style='font-family:"Calibri",sans-serif;mso-ascii-theme-font: 1671 minor-latin;mso-hansi-theme-font:minor-latin'>0:0<span class=GramE>:Eg<span 1672 style='font-family:"Times New Roman",serif;font-weight:normal'></span></span></span></b> 1668 1673 (the Secondary type I parameter you just set to vary) and press <b 1669 1674 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; … … 1672 1677 1673 1678 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1674 id=" _x0000_i1036" type="#_x0000_t75" style='width:468.75pt;height:300pt;1675 visibility:visible;mso-wrap-style:square'>1679 id="Picture_x0020_41" o:spid="_x0000_i1036" type="#_x0000_t75" style='width:468pt; 1680 height:237.75pt;visibility:visible;mso-wrap-style:square'> 1676 1681 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image029.png" 1677 1682 o:title=""/> 1678 </v:shape><![endif]--><![if !vml]><img width=625 height=400 1679 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image065.gif" 1680 v:shapes="_x0000_i1036"><![endif]></span></p> 1681 1682 <p class=MsoNormal>Pick either <span class=GramE><b style='mso-bidi-font-weight: 1683 normal'><span style='font-family:"Calibri",sans-serif;mso-ascii-theme-font: 1684 minor-latin;mso-hansi-theme-font:minor-latin'>0:all</span></b></span><b 1685 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1686 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>:Eg</span></b> 1683 </v:shape><![endif]--><![if !vml]><img width=624 height=317 1684 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image030.gif" 1685 v:shapes="Picture_x0020_41"><![endif]></span></p> 1686 1687 <p class=MsoNormal>Pick either <b style='mso-bidi-font-weight:normal'><span 1688 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1689 mso-hansi-theme-font:minor-latin'>0<span class=GramE>:all:Eg</span></span></b> 1687 1690 or <b style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1688 1691 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>0:all=<span … … 1694 1697 1695 1698 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1696 id="Picture_x0020_ 20" o:spid="_x0000_i1035" type="#_x0000_t75" style='width:481.5pt;1699 id="Picture_x0020_42" o:spid="_x0000_i1035" type="#_x0000_t75" style='width:468pt; 1697 1700 height:184.5pt;visibility:visible;mso-wrap-style:square'> 1698 1701 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image031.png" 1699 1702 o:title=""/> 1700 </v:shape><![endif]--><![if !vml]><img width=6 42height=2461701 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 66.gif"1702 v:shapes="Picture_x0020_ 20"><![endif]></span></p>1703 </v:shape><![endif]--><![if !vml]><img width=624 height=246 1704 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image032.gif" 1705 v:shapes="Picture_x0020_42"><![endif]></span></p> 1703 1706 1704 1707 <p class=MsoNormal>Now do <b style='mso-bidi-font-weight:normal'><span 1705 1708 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1706 mso-hansi-theme-font:minor-latin'>Calculate/Refine</span></b> from the main GSAS-II1707 data tree menu. You may have to repeat this twice to get convergence (<span1708 class=SpellE>Rw</span> ~ 14%); note the console output value of Delta1709 indicates closeness to convergence. Select one of the HKLF data sets and view 1710 the 3DStructure Factors plot for it alone</p>1709 mso-hansi-theme-font:minor-latin'>Calculate/Refine</span></b> from the main 1710 GSAS-II data tree menu. You may have to repeat this twice to get convergence (<span 1711 class=SpellE>Rw</span> ~6.8%); note the console output value of Delta indicates 1712 closeness to convergence. Select one of the HKLF data sets and view the 3D 1713 Structure Factors plot for it alone</p> 1711 1714 1712 1715 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1713 id="Picture_x0020_ 17" o:spid="_x0000_i1034" type="#_x0000_t75" style='width:362.25pt;1714 height: 311.25pt;visibility:visible;mso-wrap-style:square'>1716 id="Picture_x0020_45" o:spid="_x0000_i1034" type="#_x0000_t75" style='width:468pt; 1717 height:403.5pt;visibility:visible;mso-wrap-style:square'> 1715 1718 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image033.png" 1716 o:title="" croptop="15476f" cropbottom="12688f" cropleft="40744f" 1717 cropright="9798f"/> 1718 </v:shape><![endif]--><![if !vml]><img width=483 height=415 1719 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image067.jpg" 1720 v:shapes="Picture_x0020_17"><![endif]></span></p> 1721 1722 <p class=MsoNormal>The <span class=SpellE>wDF</span> is positive close to 0,0,0 1723 then negative for an inner shell around the positive core and finally positive 1724 for the outer shell. This is a thermal parameter/extinction effect. So both 1725 have to be now refined. However, as a matter of course we may expect that the 1726 extinction corrections are less accurate when <span class=SpellE>Fo</span><< 1727 Fc. In addition some reflections were poorly measured. We want to reject 1728 reflections where <span class=SpellE>Fo</span>/Fc < 0.5 and Fo2/s(Fo2) < 1729 3. These can be applied on the <b style='mso-bidi-font-weight:normal'><span 1730 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1731 mso-hansi-theme-font:minor-latin'>Controls</span></b> page. After setting these 1732 my Controls were</p> 1719 o:title=""/> 1720 </v:shape><![endif]--><![if !vml]><img width=624 height=538 1721 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image034.gif" 1722 v:shapes="Picture_x0020_45"><![endif]></span></p> 1723 1724 <p class=MsoNormal>The <span class=SpellE>wDF</span> is positive close to 0<span 1725 class=GramE>,0,0</span> then negative for an inner shell around the positive 1726 core and finally positive for the outer shell. This is a thermal 1727 parameter/extinction effect. So both have to be now refined. However, as a 1728 matter of course we may expect that the extinction corrections are less 1729 accurate when <span class=SpellE>Fo</span><< Fc. In addition some 1730 reflections were poorly measured. We want to reject reflections where <b 1731 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1732 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin;mso-bidi-theme-font: 1733 minor-latin'>Min extinct.</span></b> = <b style='mso-bidi-font-weight:normal'><span 1734 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1735 mso-hansi-theme-font:minor-latin;mso-bidi-theme-font:minor-latin'>0.5</span></b> 1736 and <b style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1737 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin;mso-bidi-theme-font: 1738 minor-latin'>Min <span class=SpellE>obs</span>/sig</span></b> = <b 1739 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1740 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin;mso-bidi-theme-font: 1741 minor-latin'>3</span></b>. These can be applied on the <b style='mso-bidi-font-weight: 1742 normal'><span style='font-family:"Calibri",sans-serif;mso-ascii-theme-font: 1743 minor-latin;mso-hansi-theme-font:minor-latin'>Controls</span></b> page. After 1744 setting these my Controls were</p> 1733 1745 1734 1746 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1735 id="Picture_x0020_ 18" o:spid="_x0000_i1033" type="#_x0000_t75" style='width:366pt;1736 height:21 2.25pt;visibility:visible;mso-wrap-style:square'>1747 id="Picture_x0020_46" o:spid="_x0000_i1033" type="#_x0000_t75" style='width:468pt; 1748 height:215.25pt;visibility:visible;mso-wrap-style:square'> 1737 1749 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image035.png" 1738 1750 o:title=""/> 1739 </v:shape><![endif]--><![if !vml]><img width= 488 height=2831740 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 68.gif"1741 v:shapes="Picture_x0020_ 18"><![endif]></span></p>1751 </v:shape><![endif]--><![if !vml]><img width=624 height=287 1752 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image036.gif" 1753 v:shapes="Picture_x0020_46"><![endif]></span></p> 1742 1754 1743 1755 <p class=MsoNormal>Finally we can add the atom parameters for sapphire. Select … … 1748 1760 1749 1761 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1750 id="Picture_x0020_ 21" o:spid="_x0000_i1032" type="#_x0000_t75" style='width:525pt;1751 height: 225pt;visibility:visible;mso-wrap-style:square'>1752 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 09.png"1753 o:title=""/> 1754 </v:shape><![endif]--><![if !vml]><img width= 700 height=3001755 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 55.gif"1756 v:shapes="Picture_x0020_ 21"><![endif]></span></p>1762 id="Picture_x0020_47" o:spid="_x0000_i1032" type="#_x0000_t75" style='width:468pt; 1763 height:117.75pt;visibility:visible;mso-wrap-style:square'> 1764 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image037.png" 1765 o:title=""/> 1766 </v:shape><![endif]--><![if !vml]><img width=624 height=157 1767 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image038.gif" 1768 v:shapes="Picture_x0020_47"><![endif]></span></p> 1757 1769 1758 1770 <p class=MsoNormal>Double (right) click the <b style='mso-bidi-font-weight: … … 1762 1774 1763 1775 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1764 id="Picture_x0020_ 22" o:spid="_x0000_i1031" type="#_x0000_t75" style='width:259.5pt;1765 height: 252pt;visibility:visible;mso-wrap-style:square'>1766 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image03 7.png"1767 o:title=""/> 1768 </v:shape><![endif]--><![if !vml]><img width= 346 height=3361769 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 69.gif"1770 v:shapes="Picture_x0020_ 22"><![endif]></span></p>1776 id="Picture_x0020_48" o:spid="_x0000_i1031" type="#_x0000_t75" style='width:171.75pt; 1777 height:150pt;visibility:visible;mso-wrap-style:square'> 1778 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image039.png" 1779 o:title=""/> 1780 </v:shape><![endif]--><![if !vml]><img width=229 height=200 1781 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image040.gif" 1782 v:shapes="Picture_x0020_48"><![endif]></span></p> 1771 1783 1772 1784 <p class=MsoNormal>Choose both <b style='mso-bidi-font-weight:normal'><span … … 1780 1792 1781 1793 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1782 id="Picture_x0020_ 23" o:spid="_x0000_i1030" type="#_x0000_t75" style='width:525pt;1783 height: 225pt;visibility:visible;mso-wrap-style:square'>1784 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 39.png"1785 o:title=""/> 1786 </v:shape><![endif]--><![if !vml]><img width= 700 height=3001787 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 70.gif"1788 v:shapes="Picture_x0020_ 23"><![endif]></span></p>1794 id="Picture_x0020_49" o:spid="_x0000_i1030" type="#_x0000_t75" style='width:468pt; 1795 height:117.75pt;visibility:visible;mso-wrap-style:square'> 1796 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image041.png" 1797 o:title=""/> 1798 </v:shape><![endif]--><![if !vml]><img width=624 height=157 1799 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image042.gif" 1800 v:shapes="Picture_x0020_49"><![endif]></span></p> 1789 1801 1790 1802 <p class=MsoNormal>Showing the refine flags for both atoms. GSAS-II will sort … … 1793 1805 <p class=MsoNormal>Now do <b style='mso-bidi-font-weight:normal'><span 1794 1806 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 1795 mso-hansi-theme-font:minor-latin'>Calculate/Refine</span></b> (twice to get 1796 convergence). My <span class=SpellE>Rw</span> = 5.91%, GOF = 2.4; find these on 1797 the <bstyle='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif;1807 mso-hansi-theme-font:minor-latin'>Calculate/Refine</span></b> (twice to get convergence). 1808 My <span class=SpellE>Rw</span> = 4.705%, GOF = 1.91; find these on the <b 1809 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1798 1810 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>Covariance</span></b> 1799 1811 data window. Now get a new 3D plot of all the reflections; select any HKLF … … 1805 1817 1806 1818 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1807 id="Picture_x0020_24" o:spid="_x0000_i1029" type="#_x0000_t75" style='width:363pt; 1808 height:312.75pt;visibility:visible;mso-wrap-style:square'> 1809 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image041.png" 1810 o:title="" croptop="10627f" cropbottom="17360f" cropleft="40646f" 1811 cropright="9847f"/> 1812 </v:shape><![endif]--><![if !vml]><img width=484 height=417 1813 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image071.jpg" 1814 v:shapes="Picture_x0020_24"><![endif]></span></p> 1819 id="Picture_x0020_50" o:spid="_x0000_i1029" type="#_x0000_t75" style='width:468pt; 1820 height:405pt;visibility:visible;mso-wrap-style:square'> 1821 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image043.png" 1822 o:title=""/> 1823 </v:shape><![endif]--><![if !vml]><img width=624 height=540 1824 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image044.gif" 1825 v:shapes="Picture_x0020_50"><![endif]></span></p> 1815 1826 1816 1827 <p class=MsoNormal>Its pretty obvious that there is one really bad reflection … … 1827 1838 <p class=MsoNormal>Phase:<span style='mso-spacerun:yes'> </span><span 1828 1839 class=GramE>sapphire<span style='mso-spacerun:yes'> </span>in</span> 1829 histogram:<span style='mso-spacerun:yes'> </span>HKLF sapphire_sphere.hkl_22<span 1830 style='mso-spacerun:yes'> </span></p> 1831 1832 <p class=MsoNormal>------------------------------------------------------------------------------------------------------</p> 1840 histogram:<span style='mso-spacerun:yes'> </span>HKLF sapphire_sphere.hkl_22<o:p></o:p></p> 1841 1842 <p class=MsoNormal>=====================================================================<o:p></o:p></p> 1833 1843 1834 1844 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Final refinement RF, 1835 RF^2 = 4.64%, 8.41% on 134 reflections (3 user rejected, 9 <span class=SpellE>sp.gp.extinct</span>)<span 1836 style='mso-spacerun:yes'> </span></p> 1845 RF^2 = 4.66%, 8.45% on 134 reflections (3 user rejected, 9 <span class=SpellE>sp.gp.extinct</span>)<o:p></o:p></p> 1837 1846 1838 1847 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>HKLF histogram weight 1839 factor <span class=GramE>=<span style='mso-spacerun:yes'> </span>1.000</span><span 1840 style='mso-spacerun:yes'> 1841 </span></p> 1848 factor <span class=GramE>=<span style='mso-spacerun:yes'> </span>1.000</span><o:p></o:p></p> 1842 1849 1843 1850 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Scale <span 1844 class=GramE>factor :</span><span style='mso-spacerun:yes'> </span>66.8623, 1845 sig<span style='mso-spacerun:yes'> </span>0.8144<span 1846 style='mso-spacerun:yes'> 1847 </span></p> 1848 1849 <p class=MsoNormal><span 1850 style='mso-spacerun:yes'> </span><span 1851 style='mso-spacerun:yes'> </span></p> 1851 class=GramE>factor :</span><span style='mso-spacerun:yes'> </span>66.5252, 1852 sig<span style='mso-spacerun:yes'> </span>0.7222<o:p></o:p></p> 1853 1854 <p class=MsoNormal><o:p> </o:p></p> 1852 1855 1853 1856 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Single crystal 1854 1857 extinction: Type:<span style='mso-spacerun:yes'> </span><span class=GramE>Lorentzian<span 1855 1858 style='mso-spacerun:yes'> </span><span class=SpellE>Approx</span></span>:<span 1856 style='mso-spacerun:yes'> </span>Secondary Type I<span 1857 style='mso-spacerun:yes'> </span></p> 1859 style='mso-spacerun:yes'> </span>Secondary Type I<o:p></o:p></p> 1858 1860 1859 1861 <p class=MsoNormal><span style='mso-spacerun:yes'> </span><span 1860 class=SpellE>Eg</span>:<span style='mso-spacerun:yes'> </span>5.58e-04 1861 sig:<span style='mso-spacerun:yes'> </span>1.28e-05<span 1862 style='mso-spacerun:yes'> </span><span 1863 style='mso-spacerun:yes'> </span></p> 1864 1865 <p class=MsoNormal><span 1866 style='mso-spacerun:yes'> 1867 </span></p> 1862 class=SpellE>Eg</span>:<span style='mso-spacerun:yes'> </span>5.71e-04 1863 sig:<span style='mso-spacerun:yes'> </span>7.44e-06<o:p></o:p></p> 1864 1865 <p class=MsoNormal><o:p> </o:p></p> 1868 1866 1869 1867 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Phase:<span 1870 1868 style='mso-spacerun:yes'> </span><span class=GramE>sapphire<span 1871 1869 style='mso-spacerun:yes'> </span>in</span> histogram:<span 1872 style='mso-spacerun:yes'> </span>HKLF sapphire_sphere.hkl_23<span 1873 style='mso-spacerun:yes'> </span></p> 1874 1875 <p class=MsoNormal>------------------------------------------------------------------------------------------------------</p> 1870 style='mso-spacerun:yes'> </span>HKLF sapphire_sphere.hkl_23<o:p></o:p></p> 1871 1872 <p class=MsoNormal>=====================================================================<o:p></o:p></p> 1876 1873 1877 1874 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Final refinement RF, 1878 RF^2 = 21.69%, 38.49% on 148 reflections (5 user rejected, 6 <span 1879 class=SpellE>sp.gp.extinct</span>)<span style='mso-spacerun:yes'> </span></p> 1875 RF^2 = 6.10%, 11.18% on 147 reflections (6 user rejected, 6 <span class=SpellE>sp.gp.extinct</span>)<o:p></o:p></p> 1880 1876 1881 1877 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>HKLF histogram weight 1882 factor <span class=GramE>=<span style='mso-spacerun:yes'> </span>1.000</span><span 1883 style='mso-spacerun:yes'> </span><span 1884 style='mso-spacerun:yes'> </span></p> 1878 factor <span class=GramE>=<span style='mso-spacerun:yes'> </span>1.000</span><o:p></o:p></p> 1885 1879 1886 1880 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Scale <span 1887 class=GramE>factor :</span><span style='mso-spacerun:yes'> </span>43.2084, 1888 sig<span style='mso-spacerun:yes'> </span>0.6507<span 1889 style='mso-spacerun:yes'> 1890 </span></p> 1891 1892 <p class=MsoNormal><span 1893 style='mso-spacerun:yes'> 1894 </span></p> 1881 class=GramE>factor :</span><span style='mso-spacerun:yes'> </span>63.2155, 1882 sig<span style='mso-spacerun:yes'> </span>0.6834<o:p></o:p></p> 1883 1884 <p class=MsoNormal><o:p> </o:p></p> 1895 1885 1896 1886 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Single crystal 1897 1887 extinction: Type:<span style='mso-spacerun:yes'> </span><span class=GramE>Lorentzian<span 1898 1888 style='mso-spacerun:yes'> </span><span class=SpellE>Approx</span></span>:<span 1899 style='mso-spacerun:yes'> </span>Secondary Type I<span 1900 style='mso-spacerun:yes'> </span></p> 1889 style='mso-spacerun:yes'> </span>Secondary Type I<o:p></o:p></p> 1901 1890 1902 1891 <p class=MsoNormal><span style='mso-spacerun:yes'> </span><span 1903 class=SpellE>Eg</span>:<span style='mso-spacerun:yes'> </span>5.58e-04 1904 sig:<span style='mso-spacerun:yes'> </span>1.28e-05<span 1905 style='mso-spacerun:yes'> 1906 </span></p> 1907 1908 <p class=MsoNormal><span 1909 style='mso-spacerun:yes'> 1910 </span><span style='mso-spacerun:yes'> </span></p> 1892 class=SpellE>Eg</span>:<span style='mso-spacerun:yes'> </span>5.71e-04 1893 sig:<span style='mso-spacerun:yes'> </span>7.44e-06<o:p></o:p></p> 1894 1895 <p class=MsoNormal><o:p> </o:p></p> 1911 1896 1912 1897 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Phase:<span 1913 1898 style='mso-spacerun:yes'> </span><span class=GramE>sapphire<span 1914 1899 style='mso-spacerun:yes'> </span>in</span> histogram:<span 1915 style='mso-spacerun:yes'> </span>HKLF sapphire_sphere.hkl_24<span 1916 style='mso-spacerun:yes'> </span></p> 1917 1918 <p class=MsoNormal>------------------------------------------------------------------------------------------------------</p> 1900 style='mso-spacerun:yes'> </span>HKLF sapphire_sphere.hkl_24<o:p></o:p></p> 1901 1902 <p class=MsoNormal>=====================================================================<o:p></o:p></p> 1919 1903 1920 1904 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Final refinement RF, 1921 RF^2 = 3.86%, 6.70% on 160 reflections (11 user rejected, 1 <span class=SpellE>sp.gp.extinct</span>)<span 1922 style='mso-spacerun:yes'> </span></p> 1905 RF^2 = 3.77%, 6.60% on 160 reflections (11 user rejected, 1 <span class=SpellE>sp.gp.extinct</span>)<o:p></o:p></p> 1923 1906 1924 1907 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>HKLF histogram weight 1925 factor <span class=GramE>=<span style='mso-spacerun:yes'> </span>1.000</span><span 1926 style='mso-spacerun:yes'> 1927 </span></p> 1908 factor <span class=GramE>=<span style='mso-spacerun:yes'> </span>1.000</span><o:p></o:p></p> 1928 1909 1929 1910 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Scale <span 1930 class=GramE>factor :</span><span style='mso-spacerun:yes'> </span>66.6296, 1931 sig<span style='mso-spacerun:yes'> </span>0.7816<span 1932 style='mso-spacerun:yes'> </span><span 1933 style='mso-spacerun:yes'> </span></p> 1934 1935 <p class=MsoNormal><span 1936 style='mso-spacerun:yes'> 1937 </span></p> 1911 class=GramE>factor :</span><span style='mso-spacerun:yes'> </span>66.4019, 1912 sig<span style='mso-spacerun:yes'> </span>0.6817<o:p></o:p></p> 1913 1914 <p class=MsoNormal><o:p> </o:p></p> 1938 1915 1939 1916 <p class=MsoNormal><span style='mso-spacerun:yes'> </span>Single crystal 1940 1917 extinction: Type:<span style='mso-spacerun:yes'> </span><span class=GramE>Lorentzian<span 1941 1918 style='mso-spacerun:yes'> </span><span class=SpellE>Approx</span></span>:<span 1942 style='mso-spacerun:yes'> </span>Secondary Type I<span 1943 style='mso-spacerun:yes'> </span></p> 1919 style='mso-spacerun:yes'> </span>Secondary Type I<o:p></o:p></p> 1944 1920 1945 1921 <p class=MsoNormal><span style='mso-spacerun:yes'> </span><span 1946 class=SpellE>Eg</span>:<span style='mso-spacerun:yes'> </span>5.58e-04 sig:<span 1947 style='mso-spacerun:yes'> </span>1.28e-05<span 1948 style='mso-spacerun:yes'> 1949 </span></p> 1950 1951 <p class=MsoNormal><span 1952 style='mso-spacerun:yes'> 1953 </span></p> 1922 class=SpellE>Eg</span>:<span style='mso-spacerun:yes'> </span>5.71e-04 1923 sig:<span style='mso-spacerun:yes'> </span>7.44e-06<o:p></o:p></p> 1924 1925 <p class=MsoNormal><span style='mso-spacerun:yes'> </span><span 1926 style='mso-spacerun:yes'> 1927 </span><span style='mso-spacerun:yes'> </span></p> 1954 1928 1955 1929 <p class=MsoNormal>There is obviously something wrong with #23 (high residual … … 1961 1935 1962 1936 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1963 id="Picture_x0020_ 25" o:spid="_x0000_i1028" type="#_x0000_t75" style='width:365.25pt;1964 height: 315pt;visibility:visible;mso-wrap-style:square'>1965 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image04 3.png"1966 o:title="" croptop="9290f" cropbottom="18441f" cropleft="38576f" cropright="11843f"/>1967 </v:shape><![endif]--><![if !vml]><img width= 487 height=4201968 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 72.jpg"1969 v:shapes="Picture_x0020_ 25"><![endif]></span></p>1937 id="Picture_x0020_51" o:spid="_x0000_i1028" type="#_x0000_t75" style='width:468pt; 1938 height:405pt;visibility:visible;mso-wrap-style:square'> 1939 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image045.png" 1940 o:title=""/> 1941 </v:shape><![endif]--><![if !vml]><img width=624 height=540 1942 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image046.gif" 1943 v:shapes="Picture_x0020_51"><![endif]></span></p> 1970 1944 1971 1945 <p class=MsoNormal>By zooming in and rotating the plot around a bit, you can 1972 1946 identify the reflection with the cursor. It seems to be the <b 1973 1947 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1974 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'> 541</span></b>1948 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>342</span></b> 1975 1949 reflection; select the <b style='mso-bidi-font-weight:normal'><span 1976 1950 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; … … 1979 1953 TOPAZ data acquisition system). It is very near the bottom of the list (#<b 1980 1954 style='mso-bidi-font-weight:normal'><span style='font-family:"Calibri",sans-serif; 1981 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>1 53</span></b>).</p>1955 mso-ascii-theme-font:minor-latin;mso-hansi-theme-font:minor-latin'>147</span></b>).</p> 1982 1956 1983 1957 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 1984 1958 id="Picture_x0020_26" o:spid="_x0000_i1027" type="#_x0000_t75" style='width:585pt; 1985 1959 height:244.5pt;visibility:visible;mso-wrap-style:square'> 1986 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image04 5.png"1960 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image047.png" 1987 1961 o:title=""/> 1988 1962 </v:shape><![endif]--><![if !vml]><img width=780 height=326 1989 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 73.gif"1963 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image048.gif" 1990 1964 v:shapes="Picture_x0020_26"><![endif]></span></p> 1991 1965 … … 2002 1976 2003 1977 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 2004 id="Picture_x0020_ 27" o:spid="_x0000_i1026" type="#_x0000_t75" style='width:391.5pt;2005 height:2 25.75pt;visibility:visible;mso-wrap-style:square'>2006 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image04 7.png"2007 o:title=""/> 2008 </v:shape><![endif]--><![if !vml]><img width= 522 height=3012009 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 74.gif"2010 v:shapes="Picture_x0020_ 27"><![endif]></span></p>1978 id="Picture_x0020_52" o:spid="_x0000_i1026" type="#_x0000_t75" style='width:468pt; 1979 height:200.25pt;visibility:visible;mso-wrap-style:square'> 1980 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image049.png" 1981 o:title=""/> 1982 </v:shape><![endif]--><![if !vml]><img width=624 height=267 1983 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image050.gif" 1984 v:shapes="Picture_x0020_52"><![endif]></span></p> 2011 1985 2012 1986 <p class=MsoNormal>Change the value of <b style='mso-bidi-font-weight:normal'><span 2013 1987 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 2014 1988 mso-hansi-theme-font:minor-latin'>Max <span class=SpellE>delt</span>-F/sig</span></b> 2015 to 20; that will certainly eliminate the bad 541reflection & perhaps a few1989 to 20; that will certainly eliminate the bad 342 reflection & perhaps a few 2016 1990 others. Repeat <b style='mso-bidi-font-weight:normal'><span style='font-family: 2017 1991 "Calibri",sans-serif;mso-ascii-theme-font:minor-latin;mso-hansi-theme-font: … … 2020 1994 2021 1995 <p class=MsoNormal><span style='mso-no-proof:yes'><!--[if gte vml 1]><v:shape 2022 id="Picture_x0020_ 28" o:spid="_x0000_i1025" type="#_x0000_t75" style='width:363pt;2023 height: 309.75pt;visibility:visible;mso-wrap-style:square'>2024 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 49.png"2025 o:title="" croptop="8876f" cropbottom="19515f" cropleft="39851f" cropright="10631f"/>2026 </v:shape><![endif]--><![if !vml]><img width= 484 height=4132027 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image0 75.jpg"2028 v:shapes="Picture_x0020_ 28"><![endif]></span></p>1996 id="Picture_x0020_53" o:spid="_x0000_i1025" type="#_x0000_t75" style='width:468pt; 1997 height:404.25pt;visibility:visible;mso-wrap-style:square'> 1998 <v:imagedata src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image051.png" 1999 o:title=""/> 2000 </v:shape><![endif]--><![if !vml]><img width=624 height=539 2001 src="TOF%20single%20crystal%20refinement%20in%20GSAS_files/image052.gif" 2002 v:shapes="Picture_x0020_53"><![endif]></span></p> 2029 2003 2030 2004 <p class=MsoNormal>Looking the <span class=SpellE><b style='mso-bidi-font-weight: … … 2052 2026 style='font-family:"Calibri",sans-serif;mso-ascii-theme-font:minor-latin; 2053 2027 mso-hansi-theme-font:minor-latin'>Calculate/Refine</span></b> again. My final 2054 residual was <span class=SpellE>Rw</span>= 5.06%. </p>2028 residual was <span class=SpellE>Rw</span>=4.20%. </p> 2055 2029 2056 2030 <p class=MsoNormal>This completes the tutorial. You can explore the other
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