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1<?xml version="1.0" encoding="UTF-8"?> 2<html cmlx:fileId="C:\Users\pm286\workspace\crystaleyeTestData\html\4\9\7\497722bd-a75f-4369-ac30-321fac1cfa70\suppText.html" xmlns:cmlx="http://www.xml-cml.org/schema/cmlx"> 3<head> 4<meta name="generator" content="HTML Tidy, see www.w3.org"/> 5<title>(IUCr) Crystallography Journals Online - supplementary 6material</title> 7<meta name="copyright" content="� International Union of Crystallography 2008"/> 8<style type="text/css"> 9 10 <!--/* <![CDATA[ */ 11 a {color:#000066; text-decoration: none;} 12 a:hover {color:#000000; text-decoration: underline;} 13 .bluetable {border: 2px solid #99ccff;} 14 .openurllink {position: absolute; right: 1.0em;} 15 h1, h2, h3 {margin-top: 0em; margin-bottom: 0.5em;padding: 0em;} 16 /* ]]> */--> 17</style> 18 19<script language="JavaScript" src="http://journals.iucr.org/javascript/scripts.js" type="text/javascript"> 20</script> 21 22<script src="http://www.google-analytics.com/urchin.js" type="text/javascript"> 23</script> 24 25<script type="text/javascript"> 26_uacct = "UA-187984-3"; 27urchinTracker(); 28</script> 29 30<link href="../../../../../styles/publcif.css" rel="stylesheet" type="text/css"/> 31</head> 32<body bgcolor="#FFFFFF" text="#000000"> 33<a id="top" name="top"/> 34<h1 class="suptitle">supplementary materials</h1> 35 36<br/> 37<div class="buttonlinks"><a href="./index.html" target="_parent"><img src="../../../../../graphics/htmlborder.gif" alt="HTML version" align="top" border="0"/></a><a href="./bi2319.pdf"><img src="../../../../../graphics/pdfborder.gif" alt="pdf version" align="top" border="0"/></a><a href="http://scripts.iucr.org/cgi-bin/sendcif?bi2319sup1"><img src="../../../../../graphics/cifborder.gif" alt="cif file" align="top" border="0"/></a><a href="http://scripts.iucr.org/cgi-bin/sendcif?bi2319sup1&Qmime=cif"> 38<img src="../../../../../graphics/3dviewborder.gif" alt="3d view" align="top" border="0"/></a><a href="./bi2319Isup2.hkl"><img src="../../../../../graphics/structurefactorsborder.gif" alt="structure factors" align="top" border="0"/></a><a href="./bi2319sup0.html"><img src="../../../../../graphics/supplementarymaterialsborder.gif" alt="supplementary materials" align="top" border="0"/></a><a href="./bi2319checkcif.html"><img src="../../../../../graphics/checkcifborder.gif" alt="CIF check report" align="top" border="0"/></a><a href="http://scripts.iucr.org/cgi-bin/similar?wordList=ethyl%20or%20hydroxyphenyl%20or%20oxo%20or%20(tetrahydropyrimidine%20and%20carboxylate)&from=bi2319"> 39<img src="../../../../../graphics/similarpapersborder.gif" alt="similar papers" align="top" border="0"/></a>�<a href="../../../../../../services/openaccess.html"><img src="../../../../../../logos/free.gif" alt="Open access" align="top" border="0"/></a></div> 40 41<p class="scheme"><img src="./bi2319contents.gif" alt="bi2319 scheme"/></p> 42 43<div class="bibline"> 44<p><i>Acta Cryst.</i> (2008). E<b>64</b>, 45o2488-o2489����[ <a title="Open URL link" href="http://dx.doi.org/10.1107/S1600536808039548">doi:10.1107/S1600536808039548</a> 46]</p> 47</div> 48 49<h3>Ethyl 504-(4-hydroxyphenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate 51monohydrate</h3> 52 53<h3><a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Das,%20U."> 54U. Das</a>, <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Chheda,%20S.B."> 55S. B. Chheda</a>, <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Pednekar,%20S.R."> 56S. R. Pednekar</a>, <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Karambelkar,%20N.P."> 57N. P. Karambelkar</a> and <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Guru%20Row,%20T.N."> 58T. N. . Guru Row</a></h3> 59 60<div class="abstract"><a id="abstract" name="abstract"/> 61 62<div class="heading2">Abstract <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 63</div> 64 65<!-- endheading2div --> 66<p>There are three formula units in the asymmetric unit of the 67title compound, C<span class="inf"><sub>14</sub></span>H<span class="inf"><sub>16</sub></span>N<span class="inf"><sub>2</sub></span>O<span class="inf"><sub>4</sub></span>�H<span class="inf"><sub>2</sub></span>O. Molecules are linked by N-H<img alt="..." border="0" src="/logos/entities/ctdot_rmgif.gif"/>O 68hydrogen bonds into dimers with the common <span class="it"><i>R</i></span><span class="inf"><sub>2</sub></span><span class="sup"><sup>2</sup></span>(8) graph-set motif. Between dimers, 69single N-H<img alt="..." border="0" src="/logos/entities/ctdot_rmgif.gif"/>O hydrogen bonds are formed 70between the other N-H group of each pyrimidine ring and the 71hydroxyl groups. The water molecules accept O-H<img alt="..." border="0" src="/logos/entities/ctdot_rmgif.gif"/>O hydrogen bonds 72from the hydroxyl groups and donate hydrogen bonds to the ester 73groups.</p> 74</div> 75 76<!-- endabstractdiv --> 77<div class="contentslist"> 78<ul> 79<li class="comment"><a title="Comment" href="#comment">Comment</a></li> 80 81<li class="relatedliterature"><a title="Related literature" href="#relatedliterature">Related literature</a></li> 82 83<li class="experimental"><a title="Experimental" href="#experimental">Experimental</a></li> 84 85<li class="refinement"><a title="Refinement" href="#refinement">Refinement</a></li> 86 87<li class="computingdetails"><a title="Computing details" href="#computingdetails">Computing details</a></li> 88 89<li class="figures"><a title="Figures" href="#figures">Figures</a></li> 90 91<li><a title="(I)" href="#chemicalname1">Ethyl 924-(4-hydroxyphenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate 93monohydrate</a> 94 95<ul> 96<li><a title="Crystal data" href="#crystaldata1">Crystal 97data</a></li> 98 99<li><a title="Data collection" href="#datacollection1">Data 100collection</a></li> 101 102<li><a title="Refinement data" href="#refinementdata1">Refinement 103data</a></li> 104 105<li class="specialdetails"><a title="Special details" href="#specialdetails1">Special details</a></li> 106 107<li class="licoords"><a title="Fractional atomic coordinates" href="#fractionalatomiccoordinates1">Fractional atomic 108coordinates</a></li> 109 110<li class="liadps"><a title="Atomic displacement parameters" href="#atomicdisplacement1">Atomic displacement parameters</a></li> 111 112<li class="ligeomlong"><a title="Geometric parameters" href="#geometricparameters1">Geometric parameters</a></li> 113 114<li class="lihbondslong"><a title="Hydrogen-bond geometry" href="#hydrogen-bondgeometry1">Hydrogen-bond geometry</a></li> 115 116<li class="lihbondsshort"><a title="Hydrogen-bond geometry" href="#hydrogen-bondgeometry1">Hydrogen-bond geometry</a></li> 117</ul> 118</li> 119 120<li class="acknowledgements"><a title="Acknowledgements" href="#acknowledgements">Acknowledgements</a></li> 121 122<li class="publreferences"><a title="References" href="#publreferences">References</a></li> 123</ul> 124</div> 125 126<!-- endcontentslistdiv --> 127<div class="comment"><a id="comment" name="comment"/> 128 129<div class="heading2">Comment <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 130</div> 131 132<!-- endheading2div --> 133<p>Heterocyclic compounds containing the pyrimidine subunit have 134been found to have strong bioactivity especially as calcium 135antagonists. In addition, some of these compounds have also been 136found to exhibit antihypertensive, antiviral, anti-tumor, 137antibacterial and anti-inflammatory activity. They can also be 138potentially used in prevention of coronary artery spasm (Kappe, 1392000). The title compound has been synthesized using a Biginelli 140reaction (Biginelli, 1891), a century-old multi-component reaction 141(MCR) used to design alkaloids with dihydropyrimidine cores (List, 1422006; Mabry & Ganem, 2006).</p> 143 144<p>The compound crystallizes in space group 145<i>P</i>2<sub>1</sub>/<i>c</i> with an unusual <i>Z</i> value of 14612. A search of the Cambridge Structural Database (CSD) yielded 147only 275 structures having <i>Z</i> = 12, which is less than 0.5% 148of the 75,822 <i>P</i>2<sub>1</sub>/<i>c</i> structures. In each 149molecule in the asymmetric unit (Fig. 1), the tetrahydropyrimidine 150ring adopts a twist boat conformation [C29-N2-C30-C24 = 151-13.09�, C8-N4-C23-C32 = -14.55�, C38-N6-C33-C37 = 15214.90�, C29-N1-C9-C24 = -21.8�, C8-N3-C34-C32 = 153-31.09�, C38-N5-C52-C37 = 28.07�]. The C-N bond lengths 154in the tetrahydropyrimidine ring (1.327�(3) to 1.473�(3) 155�) are in accordance with those in similar structures. The 156mean plane of the pyrimidine ring is nearly perpendicular to the 157phenyl ring [C37-C52-N5 = 110.05�, C14-C34-N3 = 110.25�, 158C18-C9-N1 = 110.38�].</p> 159 160<p>The structure contains extensive intermolecular 161N-H���O hydrogen bonding (see Table). Atom N2 acts 162as a hydrogen-bond donor to O2 to form a centrosymmetric dimer 163centered at (1/2,1/2,1/2) with the common 164<i>R</i><sub>2</sub><sup>2</sup>(8) graph-set motif. Atom N6 acts 165as a hydrogen-bond donor to O6 and N4 acts as a donor to O10 to 166form another dimeric <i>R</i><sub>2</sub><sup>2</sup>(8) motif. 167However, such <i>R</i><sub>2</sub><sup>2</sup>(8) motifs are not 168generated <i>via</i> N1, N3 and N5. Instead, these N atoms form 169single N-H���O hydrogen bonds to hydroxyl groups: N1 170to O5, N3 to O9 and N5 to O1.</p> 171</div> 172 173<!-- endcommentdiv --> 174<div class="relatedliterature"><a id="relatedliterature" name="relatedliterature"/> 175 176<div class="heading2">Related literature <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 177</div> 178 179<!-- endheading2div --> 180<p>For background literature concerning pyrimidine compounds and 181for synthesis details, see: Kappe (2000); Biginelli (1891); List 182(2006); Mabry & Ganem (2006).</p> 183</div> 184 185<!-- endrelatedliteraturediv --> 186<div class="experimental"><a id="experimental" name="experimental"/> 187 188<div class="heading2">Experimental <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 189</div> 190 191<!-- endheading2div --> 192<p>4-Hydroxybenzaldehyde (0.01 mol), ethyl acetoacetate (0.01 mol), 193urea (0.02 mol) and <i>p</i>-TSA (0.002 mol) were ground for 4-5 194min using a mortar and pestle. The initial syrupy reaction mixture 195solidified within 15 min. The solid was filtered, washed and 196recrystallized from a water-acetic acid mixture (yield 95%, m.p. 197509-511 K).</p> 198 199<p><sup>1</sup>H NMR (DMSO):<span style="font-family:Times">?</span> 6.66 (<i>d</i>, 2H), 7.02 200(<i>d</i>, 2H), 1.07 (<i>t</i>, 2H), 3.98 (<i>q</i>, 2 H), 2.23 201(<i>s</i>, 3 H), 5.08 (<i>s</i>, 1 H), 7.58 (<i>s</i>, 1H), 9.08 202(<i>s</i>, 1H), 9.30 (<i>s</i>, 1H).</p> 203</div> 204 205<!-- endexperimentaldiv --> 206<div class="refinement"><a id="refinement" name="refinement"/> 207 208<div class="heading2">Refinement <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 209</div> 210 211<!-- endheading2div --> 212<p>H atoms bound to C atoms were placed geometrically and allowed 213to ride during subsequent refinement with C-H = 2140.93�(3)-0.98�(3) � and <i>U</i><sub>iso</sub>(H) = 2151.2 or 1.5 <i>U</i><sub>eq</sub>(C). H atoms of the hydroxyl groups 216were placed geometrically with C-H = 0.82 � and allowed to 217rotate around the C-O bond with <i>U</i><sub>iso</sub>(H) = 1.5 218<i>U</i><sub>eq</sub>(O). H atoms of the water molecules were 219located in difference Fourier maps and refined freely with 220isotropic displacement parameters.</p> 221</div> 222 223<!-- endrefinementdiv --> 224<div class="computingdetails"><a id="computingdetails" name="computingdetails"/> 225 226<div class="heading2">Computing details <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 227</div> 228 229<!-- endheading2div --> 230<p>Data collection: <i>SMART</i> (Bruker, 2004); cell refinement: 231<i>SAINT</i> (Bruker, 2004); data reduction: <i>SAINT</i> (Bruker, 2322004); program(s) used to solve structure: <i>SHELXS97</i> 233(Sheldrick, 2008); program(s) used to refine structure: 234<i>SHELXL97</i> (Sheldrick, 2008); molecular graphics: <i>ORTEP-3 235for Windows</i> (Farrugia, 1999) and <i>CAMERON</i> (Watkin <i>et 236al.</i>, 1993); software used to prepare material for publication: 237<i>PLATON</i> (Spek, 2003).</p> 238</div> 239 240<!-- endcomputingdetailsdiv --> 241<div class="schemes"><a href="./bi2319scheme1.gif"/></div> 242 243<!-- endschemesdiv --> 244<div class="figures"><a id="figures" name="figures"/> 245 246<div class="heading2">Figures <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 247</div> 248 249<!-- endheading2div --> 250<table style="table-layout:fixed" width="100%" class="nodecs"> 251<colgroup span="2"> 252<col width="110"/> 253<col/></colgroup> 254 255<tr> 256<td class="nodecs" align="center" width="110"><a href="./bi2319fig1.html"><img width="100" src="./bi2319fig1thm.gif" alt="[Figure 1]" align="middle"/></a> </td> 257<td class="nodecs" valign="middle">Fig. 1. The asymmetric unit of 258the title compound with displacement ellipsoids drawn at the 50% 259probability level. H atoms are omitted. </td> 260</tr> 261 262<tr> 263<td class="nodecs" align="center" width="110"><a href="./bi2319fig2.html"><img width="100" src="./bi2319fig2thm.gif" alt="[Figure 2]" align="middle"/></a> </td> 264<td class="nodecs" valign="middle">Fig. 2. Partial packing diagram 265showing the <i>R</i><sub>2</sub><sup>2</sup>(8) motifs formed by 266N-H���O hydrogen bonds. </td> 267</tr> 268</table> 269</div> 270 271<!-- endfiguresdiv --> 272<div class="datablock1"> 273<div class="heading2"><a id="chemicalname1" name="chemicalname1"/>Ethyl 2744-(4-hydroxyphenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyrimidine-5-carboxylate 275monohydrate <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 276</div> 277 278<!-- endheading2div --> 279<div class="tablewrapcrystaldatalong"><a id="crystaldata1" name="crystaldata1"/><span class="heading3">Crystal data</span> 280<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 281<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 282<colgroup span="2"> 283<col width="50%"/> 284<col width="50%"/></colgroup> 285 286<tr> 287<td width="50%" class="tabledata"> 288C<sub>14</sub>H<sub>16</sub>N<sub>2</sub>O<sub>4</sub>�H<sub>2</sub>O</td> 289<td width="50%" class="tabledata"><i>F</i><sub>000</sub> = 2901872</td> 291</tr> 292 293<tr> 294<td width="50%" class="tabledata"><i>M</i><i><sub>r</sub></i> = 295294.30</td> 296<td width="50%" class="tabledata"><i>D</i><sub>x</sub> = 1.364 Mg 297m<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 298</tr> 299 300<tr> 301<td width="50%" class="tabledata">Monoclinic, 302<i>P</i>2<sub>1</sub>/<i>c</i></td> 303<td width="50%" class="tabledata">Mo <i>K</i><span style="font-family:Times">?</span> radiation<br/> 304<span style="font-family:Times">?</span> = 0.71073 �</td> 305</tr> 306 307<tr> 308<td width="50%" class="tabledata">Hall symbol: -P 2ybc</td> 309<td width="50%" class="tabledata">Cell parameters from 1328 310reflections</td> 311</tr> 312 313<tr> 314<td width="50%" class="tabledata"><i>a</i> = 11.1583 (15) 315�</td> 316<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 1.8-26.0�</td> 317</tr> 318 319<tr> 320<td width="50%" class="tabledata"><i>b</i> = 17.773 (2) �</td> 321<td width="50%" class="tabledata">� = 0.10 mm<span style="font-family:Times"><sup>?</sup></span><sup>1</sup></td> 322</tr> 323 324<tr> 325<td width="50%" class="tabledata"><i>c</i> = 21.686 (3) �</td> 326<td width="50%" class="tabledata"><i>T</i> = 292 (2) K</td> 327</tr> 328 329<tr> 330<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 91.448 (2)�</td> 331<td width="50%" class="tabledata">Lath, colourless</td> 332</tr> 333 334<tr> 335<td width="50%" class="tabledata"><i>V</i> = 4299.3 (10) 336�<sup>3</sup></td> 337<td width="50%" class="tabledata">0.50 � 0.20 � 0.10 338mm</td> 339</tr> 340 341<tr> 342<td width="50%" class="tabledata"><i>Z</i> = 12</td> 343<td width="50%" class="tabledata"/> 344</tr> 345</table> 346 347<!-- endtabledatatable --> 348</div> 349 350<!-- endtablewrapcrystaldatalongdiv --> 351<div class="tablewrapdatacollectionlong"><a id="datacollection1" name="datacollection1"/><span class="heading3">Data 352collection</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 353<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 354<colgroup span="2"> 355<col width="50%"/> 356<col width="50%"/></colgroup> 357 358<tr> 359<td width="50%" class="tabledata">Bruker SMART APEX CCD<br/> 360diffractometer</td> 361<td width="50%" class="tabledata">8419 independent reflections</td> 362</tr> 363 364<tr> 365<td width="50%" class="tabledata">Radiation source: fine-focus 366sealed tube</td> 367<td width="50%" class="tabledata">3947 reflections with <i>I</i> 368> 2<span style="font-family:Times">?</span>(<i>I</i>)</td> 369</tr> 370 371<tr> 372<td width="50%" class="tabledata">Monochromator: graphite</td> 373<td width="50%" class="tabledata"><i>R</i><sub>int</sub> = 3740.083</td> 375</tr> 376 377<tr> 378<td width="50%" class="tabledata"><i>T</i> = 292(2) K</td> 379<td width="50%" class="tabledata"><span style="font-family:Times">?</span><sub>max</sub> = 38026.0�</td> 381</tr> 382 383<tr> 384<td width="50%" class="tabledata"><span style="font-family:Times">?</span> and <span style="font-family:Times">?</span> scans</td> 385<td width="50%" class="tabledata"><span style="font-family:Times">?</span><sub>min</sub> = 3861.8�</td> 387</tr> 388 389<tr> 390<td width="50%" class="tabledata">Absorption correction: 391multi-scan<br/> 392(SADABS; Sheldrick, 1996)</td> 393<td width="50%" class="tabledata"><i>h</i> = <span style="font-family:Times">?</span>13?13</td> 394</tr> 395 396<tr> 397<td width="50%" class="tabledata"><i>T</i><sub>min</sub> = 0.906, 398<i>T</i><sub>max</sub> = 0.990</td> 399<td width="50%" class="tabledata"><i>k</i> = <span style="font-family:Times">?</span>20?21</td> 400</tr> 401 402<tr> 403<td width="50%" class="tabledata">33204 measured reflections</td> 404<td width="50%" class="tabledata"><i>l</i> = <span style="font-family:Times">?</span>26?26</td> 405</tr> 406</table> 407 408<!-- endtabledatatable --> 409</div> 410 411<!-- endtablewrapdatacollectionlongdiv --> 412<div class="tablewraprefinementdatalong"><a id="refinementdata1" name="refinementdata1"/><span class="heading3">Refinement</span> 413<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 414<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 415<colgroup span="2"> 416<col width="50%"/> 417<col width="50%"/></colgroup> 418 419<tr> 420<td width="50%" class="tabledata">Refinement on 421<i>F</i><sup>2</sup></td> 422<td width="50%" class="tabledata">Secondary atom site location: 423difference Fourier map</td> 424</tr> 425 426<tr> 427<td width="50%" class="tabledata">Least-squares matrix: full</td> 428<td width="50%" class="tabledata">Hydrogen site location: inferred 429from neighbouring sites</td> 430</tr> 431 432<tr> 433<td width="50%" class="tabledata"><i>R</i>[<i>F</i><sup>2</sup> 434> 2<span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>)] = 4350.054</td> 436<td width="50%" class="tabledata">H atoms treated by a mixture 437of<br/> 438 independent and constrained refinement</td> 439</tr> 440 441<tr> 442<td width="50%" class="tabledata"><i>wR</i>(<i>F</i><sup>2</sup>) = 4430.138</td> 444<td width="50%" class="tabledata">� <i>w</i> = 1/[<span style="font-family:Times">?</span><sup>2</sup>(<i>F</i><sub>o</sub><sup> 4452</sup>) + (0.0537<i>P</i>)<sup>2</sup> + 0.2183<i>P</i>]<br/> 446where <i>P</i> = (<i>F</i><sub>o</sub><sup>2</sup> + 4472<i>F</i><sub>c</sub><sup>2</sup>)/3</td> 448</tr> 449 450<tr> 451<td width="50%" class="tabledata"><i>S</i> = 0.90</td> 452<td width="50%" class="tabledata">(?/<span style="font-family:Times">?</span>)<sub>max</sub> = 0.048</td> 453</tr> 454 455<tr> 456<td width="50%" class="tabledata">8419 reflections</td> 457<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>max</sub> = 0.19 e 458�<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 459</tr> 460 461<tr> 462<td width="50%" class="tabledata">601 parameters</td> 463<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>min</sub> = <span style="font-family:Times">?</span>0.23 e �<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 464</tr> 465 466<tr> 467<td width="50%" class="tabledata">Primary atom site location: 468structure-invariant direct methods</td> 469<td width="50%" class="tabledata">Extinction correction: none</td> 470</tr> 471</table> 472 473<!-- endtabledatatable --> 474</div> 475 476<!-- endtablewraprefinementdatalongdiv --> 477<div class="tablewrapcrystaldatashort"><a id="crystaldata1" name="crystaldata1"/><span class="heading3">Crystal data</span> 478<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 479<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 480<colgroup span="2"> 481<col width="50%"/> 482<col width="50%"/></colgroup> 483 484<tr> 485<td width="50%" class="tabledata"> 486C<sub>14</sub>H<sub>16</sub>N<sub>2</sub>O<sub>4</sub>�H<sub>2</sub>O</td> 487<td width="50%" class="tabledata"><i>V</i> = 4299.3 (10) 488�<sup>3</sup></td> 489</tr> 490 491<tr> 492<td width="50%" class="tabledata"><i>M</i><i><sub>r</sub></i> = 493294.30</td> 494<td width="50%" class="tabledata"><i>Z</i> = 12</td> 495</tr> 496 497<tr> 498<td width="50%" class="tabledata">Monoclinic, 499<i>P</i>2<sub>1</sub>/<i>c</i></td> 500<td width="50%" class="tabledata">Mo <i>K</i><span style="font-family:Times">?</span></td> 501</tr> 502 503<tr> 504<td width="50%" class="tabledata"><i>a</i> = 11.1583 (15) 505�</td> 506<td width="50%" class="tabledata">� = 0.10 mm<span style="font-family:Times"><sup>?</sup></span><sup>1</sup></td> 507</tr> 508 509<tr> 510<td width="50%" class="tabledata"><i>b</i> = 17.773 (2) �</td> 511<td width="50%" class="tabledata"><i>T</i> = 292 (2) K</td> 512</tr> 513 514<tr> 515<td width="50%" class="tabledata"><i>c</i> = 21.686 (3) �</td> 516<td width="50%" class="tabledata">0.50 � 0.20 � 0.10 517mm</td> 518</tr> 519 520<tr> 521<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 91.448 (2)�</td> 522<td width="50%" class="tabledata"/> 523</tr> 524</table> 525 526<!-- endtabledatatable --> 527</div> 528 529<!-- endtablewrapcrystaldatashortdiv --> 530<div class="tablewrapdatacollectionshort"><a id="datacollection1" name="datacollection1"/><span class="heading3">Data 531collection</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 532<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 533<colgroup span="2"> 534<col width="50%"/> 535<col width="50%"/></colgroup> 536 537<tr> 538<td width="50%" class="tabledata">Bruker SMART APEX CCD<br/> 539diffractometer</td> 540<td width="50%" class="tabledata">8419 independent reflections</td> 541</tr> 542 543<tr> 544<td width="50%" class="tabledata">Absorption correction: 545multi-scan<br/> 546(SADABS; Sheldrick, 1996)</td> 547<td width="50%" class="tabledata">3947 reflections with <i>I</i> 548> 2<span style="font-family:Times">?</span>(<i>I</i>)</td> 549</tr> 550 551<tr> 552<td width="50%" class="tabledata"><i>T</i><sub>min</sub> = 0.906, 553<i>T</i><sub>max</sub> = 0.990</td> 554<td width="50%" class="tabledata"><i>R</i><sub>int</sub> = 5550.083</td> 556</tr> 557 558<tr> 559<td width="50%" class="tabledata">33204 measured reflections</td> 560<td width="50%" class="tabledata"/> 561</tr> 562</table> 563 564<!-- endtabledatatable --> 565</div> 566 567<!-- endtablewrapdatacollectionshortdiv --> 568<div class="tablewraprefinementdatashort"><a id="refinementdata1" name="refinementdata1"/><span class="heading3">Refinement</span> 569<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 570<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 571<colgroup span="2"> 572<col width="50%"/> 573<col width="50%"/></colgroup> 574 575<tr> 576<td width="50%" class="tabledata"><i>R</i>[<i>F</i><sup>2</sup> 577> 2<span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>)] = 5780.054</td> 579<td width="50%" class="tabledata">601 parameters</td> 580</tr> 581 582<tr> 583<td width="50%" class="tabledata"><i>wR</i>(<i>F</i><sup>2</sup>) = 5840.138</td> 585<td width="50%" class="tabledata">H atoms treated by a mixture 586of<br/> 587 independent and constrained refinement</td> 588</tr> 589 590<tr> 591<td width="50%" class="tabledata"><i>S</i> = 0.90</td> 592<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>max</sub> = 0.19 e 593�<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 594</tr> 595 596<tr> 597<td width="50%" class="tabledata">8419 reflections</td> 598<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>min</sub> = <span style="font-family:Times">?</span>0.23 e �<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 599</tr> 600</table> 601 602<!-- endtabledatatable --> 603</div> 604 605<!-- endtablewraprefinementdatashortdiv --> 606<div class="specialdetails"><a id="specialdetails1" name="specialdetails1"/><span class="heading3">Special 607details</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 608<table style="table-layout:fixed" width="100%" class="tabledata"> 609<tr> 610<td class="tabledata"> 611<p><b>Geometry</b>. Bond distances, angles <i>etc</i>. have been 612calculated using the rounded fractional coordinates. All su's 613are estimated from the variances of the (full) variance-covariance 614matrix. The cell e.s.d.'s are taken into account in the 615estimation of distances, angles and torsion angles</p> 616</td> 617</tr> 618 619<tr> 620<td class="tabledata"> 621<p><b>Refinement</b>. Refinement of <i>F</i><sup>2</sup> against 622ALL reflections. The weighted <i>R</i>-factor <i>wR</i> and 623goodness of fit <i>S</i> are based on <i>F</i><sup>2</sup>, 624conventional <i>R</i>-factors <i>R</i> are based on <i>F</i>, with 625<i>F</i> set to zero for negative <i>F</i><sup>2</sup>. The 626threshold expression of <i>F</i><sup>2</sup> > <span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>) is 627used only for calculating <i>R</i>-factors(gt) <i>etc</i>. and is 628not relevant to the choice of reflections for refinement. 629<i>R</i>-factors based on <i>F</i><sup>2</sup> are statistically 630about twice as large as those based on <i>F</i>, and <i>R</i>- 631factors based on ALL data will be even larger.</p> 632</td> 633</tr> 634</table> 635</div> 636 637<!-- endspecialdetailsdiv --> 638<div class="tablewrapcoords"><a id="fractionalatomiccoordinates1" name="fractionalatomiccoordinates1"/> <span class="heading3">Fractional atomic coordinates and isotropic or 639equivalent isotropic displacement parameters 640(�<sup>2</sup>)</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span> 641<!-- endtoplinkspan --> 642<table style="table-layout:fixed" width="100%" summary="" class="tabledata"> 643<tr> 644<td class="tabledata"/> 645<td class="tabledata"><i>x</i></td> 646<td class="tabledata"><i>y</i></td> 647<td class="tabledata"><i>z</i></td> 648<td class="tabledata"> 649<i>U</i><sub>iso</sub>*/<i>U</i><sub>eq</sub></td> 650<td class="tabledata"/> 651</tr> 652 653<tr> 654<td class="tabledata">O1</td> 655<td class="tabledata">0.33773 (18)</td> 656<td class="tabledata">0.41538 (12)</td> 657<td class="tabledata">0.11596 (8)</td> 658<td class="tabledata">0.0621 (8)</td> 659<td class="tabledata"/> 660</tr> 661 662<tr> 663<td class="tabledata">O2</td> 664<td class="tabledata">0.57587 (15)</td> 665<td class="tabledata">0.42885 (10)</td> 666<td class="tabledata">0.45666 (8)</td> 667<td class="tabledata">0.0497 (7)</td> 668<td class="tabledata"/> 669</tr> 670 671<tr> 672<td class="tabledata">O3</td> 673<td class="tabledata">0.02224 (16)</td> 674<td class="tabledata">0.37128 (12)</td> 675<td class="tabledata">0.41500 (9)</td> 676<td class="tabledata">0.0719 (9)</td> 677<td class="tabledata"/> 678</tr> 679 680<tr> 681<td class="tabledata">O4</td> 682<td class="tabledata">0.11134 (15)</td> 683<td class="tabledata">0.28500 (11)</td> 684<td class="tabledata">0.35739 (8)</td> 685<td class="tabledata">0.0557 (7)</td> 686<td class="tabledata"/> 687</tr> 688 689<tr> 690<td class="tabledata">N1</td> 691<td class="tabledata">0.45115 (16)</td> 692<td class="tabledata">0.35440 (12)</td> 693<td class="tabledata">0.39975 (9)</td> 694<td class="tabledata">0.0422 (8)</td> 695<td class="tabledata"/> 696</tr> 697 698<tr> 699<td class="tabledata">N2</td> 700<td class="tabledata">0.37628 (18)</td> 701<td class="tabledata">0.45170 (12)</td> 702<td class="tabledata">0.45626 (9)</td> 703<td class="tabledata">0.0458 (8)</td> 704<td class="tabledata"/> 705</tr> 706 707<tr> 708<td class="tabledata">C9</td> 709<td class="tabledata">0.3345 (2)</td> 710<td class="tabledata">0.33601 (14)</td> 711<td class="tabledata">0.37022 (11)</td> 712<td class="tabledata">0.0389 (9)</td> 713<td class="tabledata"/> 714</tr> 715 716<tr> 717<td class="tabledata">C18</td> 718<td class="tabledata">0.3331 (2)</td> 719<td class="tabledata">0.35869 (14)</td> 720<td class="tabledata">0.30237 (11)</td> 721<td class="tabledata">0.0367 (9)</td> 722<td class="tabledata"/> 723</tr> 724 725<tr> 726<td class="tabledata">C24</td> 727<td class="tabledata">0.2357 (2)</td> 728<td class="tabledata">0.37138 (15)</td> 729<td class="tabledata">0.40681 (11)</td> 730<td class="tabledata">0.0391 (9)</td> 731<td class="tabledata"/> 732</tr> 733 734<tr> 735<td class="tabledata">C27</td> 736<td class="tabledata">0.2886 (2)</td> 737<td class="tabledata">0.42710 (15)</td> 738<td class="tabledata">0.28185 (12)</td> 739<td class="tabledata">0.0425 (10)</td> 740<td class="tabledata"/> 741</tr> 742 743<tr> 744<td class="tabledata">C29</td> 745<td class="tabledata">0.4734 (2)</td> 746<td class="tabledata">0.41183 (15)</td> 747<td class="tabledata">0.43768 (11)</td> 748<td class="tabledata">0.0400 (10)</td> 749<td class="tabledata"/> 750</tr> 751 752<tr> 753<td class="tabledata">C30</td> 754<td class="tabledata">0.2591 (2)</td> 755<td class="tabledata">0.42843 (15)</td> 756<td class="tabledata">0.44647 (11)</td> 757<td class="tabledata">0.0407 (10)</td> 758<td class="tabledata"/> 759</tr> 760 761<tr> 762<td class="tabledata">C35</td> 763<td class="tabledata">0.3341 (2)</td> 764<td class="tabledata">0.39763 (17)</td> 765<td class="tabledata">0.17742 (12)</td> 766<td class="tabledata">0.0452 (10)</td> 767<td class="tabledata"/> 768</tr> 769 770<tr> 771<td class="tabledata">C36</td> 772<td class="tabledata">0.2889 (2)</td> 773<td class="tabledata">0.44681 (15)</td> 774<td class="tabledata">0.22048 (12)</td> 775<td class="tabledata">0.0447 (10)</td> 776<td class="tabledata"/> 777</tr> 778 779<tr> 780<td class="tabledata">C41</td> 781<td class="tabledata">0.1130 (2)</td> 782<td class="tabledata">0.34506 (17)</td> 783<td class="tabledata">0.39467 (12)</td> 784<td class="tabledata">0.0469 (10)</td> 785<td class="tabledata"/> 786</tr> 787 788<tr> 789<td class="tabledata">C43</td> 790<td class="tabledata">0.3778 (2)</td> 791<td class="tabledata">0.31030 (15)</td> 792<td class="tabledata">0.25840 (12)</td> 793<td class="tabledata">0.0461 (10)</td> 794<td class="tabledata"/> 795</tr> 796 797<tr> 798<td class="tabledata">C51</td> 799<td class="tabledata">0.3789 (2)</td> 800<td class="tabledata">0.32967 (16)</td> 801<td class="tabledata">0.19670 (12)</td> 802<td class="tabledata">0.0511 (11)</td> 803<td class="tabledata"/> 804</tr> 805 806<tr> 807<td class="tabledata">C58</td> 808<td class="tabledata"><span style="font-family:Times">?</span>0.0060 (2)</td> 809<td class="tabledata">0.25637 (19)</td> 810<td class="tabledata">0.33819 (14)</td> 811<td class="tabledata">0.0726 (13)</td> 812<td class="tabledata"/> 813</tr> 814 815<tr> 816<td class="tabledata">C59</td> 817<td class="tabledata">0.1717 (2)</td> 818<td class="tabledata">0.47050 (15)</td> 819<td class="tabledata">0.48439 (12)</td> 820<td class="tabledata">0.0564 (11)</td> 821<td class="tabledata"/> 822</tr> 823 824<tr> 825<td class="tabledata">C63</td> 826<td class="tabledata">0.0100 (3)</td> 827<td class="tabledata">0.19780 (19)</td> 828<td class="tabledata">0.29252 (17)</td> 829<td class="tabledata">0.0982 (16)</td> 830<td class="tabledata"/> 831</tr> 832 833<tr> 834<td class="tabledata">O5</td> 835<td class="tabledata">0.66400 (17)</td> 836<td class="tabledata">0.25970 (11)</td> 837<td class="tabledata">0.36851 (8)</td> 838<td class="tabledata">0.0604 (8)</td> 839<td class="tabledata"/> 840</tr> 841 842<tr> 843<td class="tabledata">O6</td> 844<td class="tabledata">0.43755 (14)</td> 845<td class="tabledata">0.22711 (11)</td> 846<td class="tabledata">0.03821 (8)</td> 847<td class="tabledata">0.0521 (7)</td> 848<td class="tabledata"/> 849</tr> 850 851<tr> 852<td class="tabledata">O7</td> 853<td class="tabledata">0.99348 (15)</td> 854<td class="tabledata">0.17389 (11)</td> 855<td class="tabledata">0.07701 (9)</td> 856<td class="tabledata">0.0656 (8)</td> 857<td class="tabledata"/> 858</tr> 859 860<tr> 861<td class="tabledata">O8</td> 862<td class="tabledata">0.90818 (14)</td> 863<td class="tabledata">0.09252 (10)</td> 864<td class="tabledata">0.14113 (8)</td> 865<td class="tabledata">0.0464 (7)</td> 866<td class="tabledata"/> 867</tr> 868 869<tr> 870<td class="tabledata">N3</td> 871<td class="tabledata">0.56592 (16)</td> 872<td class="tabledata">0.15289 (12)</td> 873<td class="tabledata">0.09325 (9)</td> 874<td class="tabledata">0.0402 (8)</td> 875<td class="tabledata"/> 876</tr> 877 878<tr> 879<td class="tabledata">N4</td> 880<td class="tabledata">0.63647 (17)</td> 881<td class="tabledata">0.25030 (12)</td> 882<td class="tabledata">0.03655 (9)</td> 883<td class="tabledata">0.0458 (8)</td> 884<td class="tabledata"/> 885</tr> 886 887<tr> 888<td class="tabledata">C8</td> 889<td class="tabledata">0.5406 (2)</td> 890<td class="tabledata">0.21040 (15)</td> 891<td class="tabledata">0.05610 (11)</td> 892<td class="tabledata">0.0392 (10)</td> 893<td class="tabledata"/> 894</tr> 895 896<tr> 897<td class="tabledata">C14</td> 898<td class="tabledata">0.67912 (19)</td> 899<td class="tabledata">0.17523 (14)</td> 900<td class="tabledata">0.19033 (11)</td> 901<td class="tabledata">0.0340 (9)</td> 902<td class="tabledata"/> 903</tr> 904 905<tr> 906<td class="tabledata">C17</td> 907<td class="tabledata">0.9035 (2)</td> 908<td class="tabledata">0.14900 (16)</td> 909<td class="tabledata">0.09962 (12)</td> 910<td class="tabledata">0.0424 (10)</td> 911<td class="tabledata"/> 912</tr> 913 914<tr> 915<td class="tabledata">C23</td> 916<td class="tabledata">0.7551 (2)</td> 917<td class="tabledata">0.22858 (15)</td> 918<td class="tabledata">0.04565 (11)</td> 919<td class="tabledata">0.0410 (10)</td> 920<td class="tabledata"/> 921</tr> 922 923<tr> 924<td class="tabledata">C26</td> 925<td class="tabledata">0.6355 (2)</td> 926<td class="tabledata">0.13308 (15)</td> 927<td class="tabledata">0.23857 (11)</td> 928<td class="tabledata">0.0434 (10)</td> 929<td class="tabledata"/> 930</tr> 931 932<tr> 933<td class="tabledata">C31</td> 934<td class="tabledata">0.6696 (2)</td> 935<td class="tabledata">0.23365 (16)</td> 936<td class="tabledata">0.30919 (12)</td> 937<td class="tabledata">0.0426 (10)</td> 938<td class="tabledata"/> 939</tr> 940 941<tr> 942<td class="tabledata">C32</td> 943<td class="tabledata">0.7804 (2)</td> 944<td class="tabledata">0.17388 (14)</td> 945<td class="tabledata">0.08680 (11)</td> 946<td class="tabledata">0.0366 (9)</td> 947<td class="tabledata"/> 948</tr> 949 950<tr> 951<td class="tabledata">C34</td> 952<td class="tabledata">0.6820 (2)</td> 953<td class="tabledata">0.14156 (14)</td> 954<td class="tabledata">0.12561 (10)</td> 955<td class="tabledata">0.0368 (9)</td> 956<td class="tabledata"/> 957</tr> 958 959<tr> 960<td class="tabledata">C39</td> 961<td class="tabledata">0.7103 (2)</td> 962<td class="tabledata">0.27746 (15)</td> 963<td class="tabledata">0.26171 (12)</td> 964<td class="tabledata">0.0451 (10)</td> 965<td class="tabledata"/> 966</tr> 967 968<tr> 969<td class="tabledata">C47</td> 970<td class="tabledata">1.0265 (2)</td> 971<td class="tabledata">0.06549 (16)</td> 972<td class="tabledata">0.15924 (12)</td> 973<td class="tabledata">0.0519 (10)</td> 974<td class="tabledata"/> 975</tr> 976 977<tr> 978<td class="tabledata">C48</td> 979<td class="tabledata">0.7151 (2)</td> 980<td class="tabledata">0.24819 (14)</td> 981<td class="tabledata">0.20283 (11)</td> 982<td class="tabledata">0.0416 (10)</td> 983<td class="tabledata"/> 984</tr> 985 986<tr> 987<td class="tabledata">C55</td> 988<td class="tabledata">0.8393 (2)</td> 989<td class="tabledata">0.27145 (16)</td> 990<td class="tabledata">0.00655 (11)</td> 991<td class="tabledata">0.0544 (10)</td> 992<td class="tabledata"/> 993</tr> 994 995<tr> 996<td class="tabledata">C57</td> 997<td class="tabledata">0.6307 (2)</td> 998<td class="tabledata">0.16154 (16)</td> 999<td class="tabledata">0.29722 (12)</td> 1000<td class="tabledata">0.0484 (11)</td> 1001<td class="tabledata"/> 1002</tr> 1003 1004<tr> 1005<td class="tabledata">C62</td> 1006<td class="tabledata">1.0128 (3)</td> 1007<td class="tabledata">0.01022 (16)</td> 1008<td class="tabledata">0.21043 (14)</td> 1009<td class="tabledata">0.0651 (11)</td> 1010<td class="tabledata"/> 1011</tr> 1012 1013<tr> 1014<td class="tabledata">O9</td> 1015<td class="tabledata">0.35723 (18)</td> 1016<td class="tabledata">0.05785 (11)</td> 1017<td class="tabledata">0.14122 (8)</td> 1018<td class="tabledata">0.0603 (8)</td> 1019<td class="tabledata"/> 1020</tr> 1021 1022<tr> 1023<td class="tabledata">O10</td> 1024<td class="tabledata">0.58206 (15)</td> 1025<td class="tabledata">0.11471 (10)</td> 1026<td class="tabledata">0.47033 (8)</td> 1027<td class="tabledata">0.0522 (7)</td> 1028<td class="tabledata"/> 1029</tr> 1030 1031<tr> 1032<td class="tabledata">O11</td> 1033<td class="tabledata">0.02324 (17)</td> 1034<td class="tabledata">0.06082 (12)</td> 1035<td class="tabledata">0.43805 (10)</td> 1036<td class="tabledata">0.0759 (9)</td> 1037<td class="tabledata"/> 1038</tr> 1039 1040<tr> 1041<td class="tabledata">O12</td> 1042<td class="tabledata">0.10976 (14)</td> 1043<td class="tabledata"><span style="font-family:Times">?</span>0.03730 (11)</td> 1044<td class="tabledata">0.39298 (8)</td> 1045<td class="tabledata">0.0509 (7)</td> 1046<td class="tabledata"/> 1047</tr> 1048 1049<tr> 1050<td class="tabledata">N5</td> 1051<td class="tabledata">0.45147 (17)</td> 1052<td class="tabledata">0.03034 (12)</td> 1053<td class="tabledata">0.42832 (9)</td> 1054<td class="tabledata">0.0443 (8)</td> 1055<td class="tabledata"/> 1056</tr> 1057 1058<tr> 1059<td class="tabledata">N6</td> 1060<td class="tabledata">0.38344 (17)</td> 1061<td class="tabledata">0.14147 (12)</td> 1062<td class="tabledata">0.46649 (9)</td> 1063<td class="tabledata">0.0440 (8)</td> 1064<td class="tabledata"/> 1065</tr> 1066 1067<tr> 1068<td class="tabledata">C22</td> 1069<td class="tabledata">0.3837 (2)</td> 1070<td class="tabledata"><span style="font-family:Times">?</span>0.01916 (16)</td> 1071<td class="tabledata">0.22853 (13)</td> 1072<td class="tabledata">0.0488 (11)</td> 1073<td class="tabledata"/> 1074</tr> 1075 1076<tr> 1077<td class="tabledata">C25</td> 1078<td class="tabledata">0.3366 (2)</td> 1079<td class="tabledata">0.02517 (15)</td> 1080<td class="tabledata">0.33034 (11)</td> 1081<td class="tabledata">0.0369 (9)</td> 1082<td class="tabledata"/> 1083</tr> 1084 1085<tr> 1086<td class="tabledata">C33</td> 1087<td class="tabledata">0.2636 (2)</td> 1088<td class="tabledata">0.11928 (15)</td> 1089<td class="tabledata">0.46115 (11)</td> 1090<td class="tabledata">0.0411 (10)</td> 1091<td class="tabledata"/> 1092</tr> 1093 1094<tr> 1095<td class="tabledata">C37</td> 1096<td class="tabledata">0.2370 (2)</td> 1097<td class="tabledata">0.05563 (15)</td> 1098<td class="tabledata">0.43094 (11)</td> 1099<td class="tabledata">0.0406 (9)</td> 1100<td class="tabledata"/> 1101</tr> 1102 1103<tr> 1104<td class="tabledata">C38</td> 1105<td class="tabledata">0.4785 (2)</td> 1106<td class="tabledata">0.09551 (16)</td> 1107<td class="tabledata">0.45504 (11)</td> 1108<td class="tabledata">0.0410 (10)</td> 1109<td class="tabledata"/> 1110</tr> 1111 1112<tr> 1113<td class="tabledata">C42</td> 1114<td class="tabledata">0.3491 (2)</td> 1115<td class="tabledata">0.04858 (17)</td> 1116<td class="tabledata">0.20369 (12)</td> 1117<td class="tabledata">0.0449 (10)</td> 1118<td class="tabledata"/> 1119</tr> 1120 1121<tr> 1122<td class="tabledata">C44</td> 1123<td class="tabledata">0.3102 (2)</td> 1124<td class="tabledata">0.10538 (15)</td> 1125<td class="tabledata">0.24164 (12)</td> 1126<td class="tabledata">0.0442 (10)</td> 1127<td class="tabledata"/> 1128</tr> 1129 1130<tr> 1131<td class="tabledata">C49</td> 1132<td class="tabledata">0.3046 (2)</td> 1133<td class="tabledata">0.09334 (15)</td> 1134<td class="tabledata">0.30425 (12)</td> 1135<td class="tabledata">0.0420 (10)</td> 1136<td class="tabledata"/> 1137</tr> 1138 1139<tr> 1140<td class="tabledata">C52</td> 1141<td class="tabledata">0.3344 (2)</td> 1142<td class="tabledata">0.01124 (15)</td> 1143<td class="tabledata">0.39965 (11)</td> 1144<td class="tabledata">0.0386 (9)</td> 1145<td class="tabledata"/> 1146</tr> 1147 1148<tr> 1149<td class="tabledata">C53</td> 1150<td class="tabledata">0.1136 (2)</td> 1151<td class="tabledata">0.02892 (17)</td> 1152<td class="tabledata">0.42254 (12)</td> 1153<td class="tabledata">0.0460 (10)</td> 1154<td class="tabledata"/> 1155</tr> 1156 1157<tr> 1158<td class="tabledata">C54</td> 1159<td class="tabledata">0.3758 (2)</td> 1160<td class="tabledata"><span style="font-family:Times">?</span>0.03085 (15)</td> 1161<td class="tabledata">0.29138 (13)</td> 1162<td class="tabledata">0.0449 (10)</td> 1163<td class="tabledata"/> 1164</tr> 1165 1166<tr> 1167<td class="tabledata">C56</td> 1168<td class="tabledata">0.1815 (2)</td> 1169<td class="tabledata">0.17336 (15)</td> 1170<td class="tabledata">0.49137 (12)</td> 1171<td class="tabledata">0.0544 (11)</td> 1172<td class="tabledata"/> 1173</tr> 1174 1175<tr> 1176<td class="tabledata">C60</td> 1177<td class="tabledata"><span style="font-family:Times">?</span>0.0077 (2)</td> 1178<td class="tabledata"><span style="font-family:Times">?</span>0.06677 (15)</td> 1179<td class="tabledata">0.37706 (13)</td> 1180<td class="tabledata">0.0553 (11)</td> 1181<td class="tabledata"/> 1182</tr> 1183 1184<tr> 1185<td class="tabledata">C61</td> 1186<td class="tabledata">0.0072 (3)</td> 1187<td class="tabledata"><span style="font-family:Times">?</span>0.13722 (16)</td> 1188<td class="tabledata">0.34069 (14)</td> 1189<td class="tabledata">0.0699 (14)</td> 1190<td class="tabledata"/> 1191</tr> 1192 1193<tr> 1194<td class="tabledata">O13</td> 1195<td class="tabledata">0.7780 (2)</td> 1196<td class="tabledata">0.38763 (15)</td> 1197<td class="tabledata">0.38773 (12)</td> 1198<td class="tabledata">0.0812 (10)</td> 1199<td class="tabledata"/> 1200</tr> 1201 1202<tr> 1203<td class="tabledata">O14</td> 1204<td class="tabledata">0.2287 (2)</td> 1205<td class="tabledata">0.54269 (15)</td> 1206<td class="tabledata">0.08331 (12)</td> 1207<td class="tabledata">0.0840 (11)</td> 1208<td class="tabledata"/> 1209</tr> 1210 1211<tr> 1212<td class="tabledata">O15</td> 1213<td class="tabledata">0.2419 (2)</td> 1214<td class="tabledata">0.17780 (15)</td> 1215<td class="tabledata">0.10108 (11)</td> 1216<td class="tabledata">0.0879 (10)</td> 1217<td class="tabledata"/> 1218</tr> 1219 1220<tr> 1221<td class="tabledata">H1</td> 1222<td class="tabledata">0.30135</td> 1223<td class="tabledata">0.45482</td> 1224<td class="tabledata">0.10960</td> 1225<td class="tabledata">0.0932*</td> 1226<td class="tabledata"/> 1227</tr> 1228 1229<tr> 1230<td class="tabledata">H2</td> 1231<td class="tabledata">0.38863</td> 1232<td class="tabledata">0.49366</td> 1233<td class="tabledata">0.47513</td> 1234<td class="tabledata">0.0549*</td> 1235<td class="tabledata"/> 1236</tr> 1237 1238<tr> 1239<td class="tabledata">H9</td> 1240<td class="tabledata">0.32437</td> 1241<td class="tabledata">0.28129</td> 1242<td class="tabledata">0.37210</td> 1243<td class="tabledata">0.0467*</td> 1244<td class="tabledata"/> 1245</tr> 1246 1247<tr> 1248<td class="tabledata">H11</td> 1249<td class="tabledata">0.51035</td> 1250<td class="tabledata">0.32531</td> 1251<td class="tabledata">0.39174</td> 1252<td class="tabledata">0.0506*</td> 1253<td class="tabledata"/> 1254</tr> 1255 1256<tr> 1257<td class="tabledata">H27</td> 1258<td class="tabledata">0.25777</td> 1259<td class="tabledata">0.46068</td> 1260<td class="tabledata">0.31026</td> 1261<td class="tabledata">0.0509*</td> 1262<td class="tabledata"/> 1263</tr> 1264 1265<tr> 1266<td class="tabledata">H36</td> 1267<td class="tabledata">0.25859</td> 1268<td class="tabledata">0.49325</td> 1269<td class="tabledata">0.20793</td> 1270<td class="tabledata">0.0537*</td> 1271<td class="tabledata"/> 1272</tr> 1273 1274<tr> 1275<td class="tabledata">H43</td> 1276<td class="tabledata">0.40775</td> 1277<td class="tabledata">0.26369</td> 1278<td class="tabledata">0.27072</td> 1279<td class="tabledata">0.0553*</td> 1280<td class="tabledata"/> 1281</tr> 1282 1283<tr> 1284<td class="tabledata">H51</td> 1285<td class="tabledata">0.41020</td> 1286<td class="tabledata">0.29641</td> 1287<td class="tabledata">0.16817</td> 1288<td class="tabledata">0.0612*</td> 1289<td class="tabledata"/> 1290</tr> 1291 1292<tr> 1293<td class="tabledata">H58A</td> 1294<td class="tabledata"><span style="font-family:Times">?</span>0.04686</td> 1295<td class="tabledata">0.23614</td> 1296<td class="tabledata">0.37349</td> 1297<td class="tabledata">0.0871*</td> 1298<td class="tabledata"/> 1299</tr> 1300 1301<tr> 1302<td class="tabledata">H58B</td> 1303<td class="tabledata"><span style="font-family:Times">?</span>0.05442</td> 1304<td class="tabledata">0.29676</td> 1305<td class="tabledata">0.32070</td> 1306<td class="tabledata">0.0871*</td> 1307<td class="tabledata"/> 1308</tr> 1309 1310<tr> 1311<td class="tabledata">H59A</td> 1312<td class="tabledata">0.09680</td> 1313<td class="tabledata">0.47487</td> 1314<td class="tabledata">0.46189</td> 1315<td class="tabledata">0.0845*</td> 1316<td class="tabledata"/> 1317</tr> 1318 1319<tr> 1320<td class="tabledata">H59B</td> 1321<td class="tabledata">0.20257</td> 1322<td class="tabledata">0.51979</td> 1323<td class="tabledata">0.49344</td> 1324<td class="tabledata">0.0845*</td> 1325<td class="tabledata"/> 1326</tr> 1327 1328<tr> 1329<td class="tabledata">H59C</td> 1330<td class="tabledata">0.15941</td> 1331<td class="tabledata">0.44387</td> 1332<td class="tabledata">0.52223</td> 1333<td class="tabledata">0.0845*</td> 1334<td class="tabledata"/> 1335</tr> 1336 1337<tr> 1338<td class="tabledata">H63A</td> 1339<td class="tabledata">0.05611</td> 1340<td class="tabledata">0.21716</td> 1341<td class="tabledata">0.25926</td> 1342<td class="tabledata">0.1474*</td> 1343<td class="tabledata"/> 1344</tr> 1345 1346<tr> 1347<td class="tabledata">H63B</td> 1348<td class="tabledata"><span style="font-family:Times">?</span>0.06690</td> 1349<td class="tabledata">0.18151</td> 1350<td class="tabledata">0.27685</td> 1351<td class="tabledata">0.1474*</td> 1352<td class="tabledata"/> 1353</tr> 1354 1355<tr> 1356<td class="tabledata">H63C</td> 1357<td class="tabledata">0.05152</td> 1358<td class="tabledata">0.15599</td> 1359<td class="tabledata">0.31123</td> 1360<td class="tabledata">0.1474*</td> 1361<td class="tabledata"/> 1362</tr> 1363 1364<tr> 1365<td class="tabledata">H3</td> 1366<td class="tabledata">0.51070</td> 1367<td class="tabledata">0.11999</td> 1368<td class="tabledata">0.09877</td> 1369<td class="tabledata">0.0483*</td> 1370<td class="tabledata"/> 1371</tr> 1372 1373<tr> 1374<td class="tabledata">H4</td> 1375<td class="tabledata">0.62266</td> 1376<td class="tabledata">0.29180</td> 1377<td class="tabledata">0.01724</td> 1378<td class="tabledata">0.0550*</td> 1379<td class="tabledata"/> 1380</tr> 1381 1382<tr> 1383<td class="tabledata">H5</td> 1384<td class="tabledata">0.70400</td> 1385<td class="tabledata">0.29823</td> 1386<td class="tabledata">0.37209</td> 1387<td class="tabledata">0.0906*</td> 1388<td class="tabledata"/> 1389</tr> 1390 1391<tr> 1392<td class="tabledata">H26</td> 1393<td class="tabledata">0.60883</td> 1394<td class="tabledata">0.08429</td> 1395<td class="tabledata">0.23100</td> 1396<td class="tabledata">0.0521*</td> 1397<td class="tabledata"/> 1398</tr> 1399 1400<tr> 1401<td class="tabledata">H34</td> 1402<td class="tabledata">0.69565</td> 1403<td class="tabledata">0.08730</td> 1404<td class="tabledata">0.12966</td> 1405<td class="tabledata">0.0441*</td> 1406<td class="tabledata"/> 1407</tr> 1408 1409<tr> 1410<td class="tabledata">H39</td> 1411<td class="tabledata">0.73457</td> 1412<td class="tabledata">0.32672</td> 1413<td class="tabledata">0.26929</td> 1414<td class="tabledata">0.0541*</td> 1415<td class="tabledata"/> 1416</tr> 1417 1418<tr> 1419<td class="tabledata">H47A</td> 1420<td class="tabledata">1.07654</td> 1421<td class="tabledata">0.10717</td> 1422<td class="tabledata">0.17294</td> 1423<td class="tabledata">0.0624*</td> 1424<td class="tabledata"/> 1425</tr> 1426 1427<tr> 1428<td class="tabledata">H47B</td> 1429<td class="tabledata">1.06404</td> 1430<td class="tabledata">0.04155</td> 1431<td class="tabledata">0.12448</td> 1432<td class="tabledata">0.0624*</td> 1433<td class="tabledata"/> 1434</tr> 1435 1436<tr> 1437<td class="tabledata">H48</td> 1438<td class="tabledata">0.74299</td> 1439<td class="tabledata">0.27808</td> 1440<td class="tabledata">0.17104</td> 1441<td class="tabledata">0.0499*</td> 1442<td class="tabledata"/> 1443</tr> 1444 1445<tr> 1446<td class="tabledata">H55A</td> 1447<td class="tabledata">0.85834</td> 1448<td class="tabledata">0.31867</td> 1449<td class="tabledata">0.02594</td> 1450<td class="tabledata">0.0813*</td> 1451<td class="tabledata"/> 1452</tr> 1453 1454<tr> 1455<td class="tabledata">H55B</td> 1456<td class="tabledata">0.80233</td> 1457<td class="tabledata">0.28044</td> 1458<td class="tabledata"><span style="font-family:Times">?</span>0.03322</td> 1459<td class="tabledata">0.0813*</td> 1460<td class="tabledata"/> 1461</tr> 1462 1463<tr> 1464<td class="tabledata">H55C</td> 1465<td class="tabledata">0.91146</td> 1466<td class="tabledata">0.24286</td> 1467<td class="tabledata">0.00175</td> 1468<td class="tabledata">0.0813*</td> 1469<td class="tabledata"/> 1470</tr> 1471 1472<tr> 1473<td class="tabledata">H57</td> 1474<td class="tabledata">0.60112</td> 1475<td class="tabledata">0.13213</td> 1476<td class="tabledata">0.32889</td> 1477<td class="tabledata">0.0581*</td> 1478<td class="tabledata"/> 1479</tr> 1480 1481<tr> 1482<td class="tabledata">H62A</td> 1483<td class="tabledata">0.96886</td> 1484<td class="tabledata">0.03302</td> 1485<td class="tabledata">0.24302</td> 1486<td class="tabledata">0.0977*</td> 1487<td class="tabledata"/> 1488</tr> 1489 1490<tr> 1491<td class="tabledata">H62B</td> 1492<td class="tabledata">1.09059</td> 1493<td class="tabledata"><span style="font-family:Times">?</span>0.00470</td> 1494<td class="tabledata">0.22590</td> 1495<td class="tabledata">0.0977*</td> 1496<td class="tabledata"/> 1497</tr> 1498 1499<tr> 1500<td class="tabledata">H62C</td> 1501<td class="tabledata">0.97019</td> 1502<td class="tabledata"><span style="font-family:Times">?</span>0.03319</td> 1503<td class="tabledata">0.19528</td> 1504<td class="tabledata">0.0977*</td> 1505<td class="tabledata"/> 1506</tr> 1507 1508<tr> 1509<td class="tabledata">H6</td> 1510<td class="tabledata">0.39839</td> 1511<td class="tabledata">0.18699</td> 1512<td class="tabledata">0.47771</td> 1513<td class="tabledata">0.0527*</td> 1514<td class="tabledata"/> 1515</tr> 1516 1517<tr> 1518<td class="tabledata">H9A</td> 1519<td class="tabledata">0.31708</td> 1520<td class="tabledata">0.09432</td> 1521<td class="tabledata">0.13021</td> 1522<td class="tabledata">0.0904*</td> 1523<td class="tabledata"/> 1524</tr> 1525 1526<tr> 1527<td class="tabledata">H22</td> 1528<td class="tabledata">0.41239</td> 1529<td class="tabledata"><span style="font-family:Times">?</span>0.05706</td> 1530<td class="tabledata">0.20328</td> 1531<td class="tabledata">0.0583*</td> 1532<td class="tabledata"/> 1533</tr> 1534 1535<tr> 1536<td class="tabledata">H44</td> 1537<td class="tabledata">0.28789</td> 1538<td class="tabledata">0.15168</td> 1539<td class="tabledata">0.22501</td> 1540<td class="tabledata">0.0530*</td> 1541<td class="tabledata"/> 1542</tr> 1543 1544<tr> 1545<td class="tabledata">H49</td> 1546<td class="tabledata">0.27868</td> 1547<td class="tabledata">0.13203</td> 1548<td class="tabledata">0.32952</td> 1549<td class="tabledata">0.0503*</td> 1550<td class="tabledata"/> 1551</tr> 1552 1553<tr> 1554<td class="tabledata">H52</td> 1555<td class="tabledata">0.31950</td> 1556<td class="tabledata"><span style="font-family:Times">?</span>0.04243</td> 1557<td class="tabledata">0.40642</td> 1558<td class="tabledata">0.0464*</td> 1559<td class="tabledata"/> 1560</tr> 1561 1562<tr> 1563<td class="tabledata">H54</td> 1564<td class="tabledata">0.39733</td> 1565<td class="tabledata"><span style="font-family:Times">?</span>0.07741</td> 1566<td class="tabledata">0.30781</td> 1567<td class="tabledata">0.0538*</td> 1568<td class="tabledata"/> 1569</tr> 1570 1571<tr> 1572<td class="tabledata">H56A</td> 1573<td class="tabledata">0.19101</td> 1574<td class="tabledata">0.16920</td> 1575<td class="tabledata">0.53535</td> 1576<td class="tabledata">0.0815*</td> 1577<td class="tabledata"/> 1578</tr> 1579 1580<tr> 1581<td class="tabledata">H56B</td> 1582<td class="tabledata">0.20054</td> 1583<td class="tabledata">0.22368</td> 1584<td class="tabledata">0.47884</td> 1585<td class="tabledata">0.0815*</td> 1586<td class="tabledata"/> 1587</tr> 1588 1589<tr> 1590<td class="tabledata">H56C</td> 1591<td class="tabledata">0.10009</td> 1592<td class="tabledata">0.16203</td> 1593<td class="tabledata">0.47936</td> 1594<td class="tabledata">0.0815*</td> 1595<td class="tabledata"/> 1596</tr> 1597 1598<tr> 1599<td class="tabledata">H60A</td> 1600<td class="tabledata"><span style="font-family:Times">?</span>0.05117</td> 1601<td class="tableda…
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