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E<b>64</b>, 44o10����[ <a title="Open URL link" href="http://dx.doi.org/10.1107/S1600536807061521">doi:10.1107/S1600536807061521</a> 45]</p> 46</div> 47 48<h3>3-Benzyl-1-butylimidazo[1,2-<span class="it"><i>a</i></span>]benzothieno[3,2-<span class="it"><i>d</i></span>]pyrimidine-2,5(1<span class="it"><i>H</i></span>,3<span class="it"><i>H</i></span>)-dione</h3> 49 50<h3><a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Cao,%20M.-H."> 51M.-H. Cao</a>, <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Zhu,%20J."> 52J. Zhu</a> and <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Ni,%20D.-J."> 53D.-J. Ni</a></h3> 54 55<div class="abstract"><a id="abstract" name="abstract"/> 56 57<div class="heading2">Abstract <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 58</div> 59 60<!-- endheading2div --> 61<p>In the crystal structure of the title compound, C<span class="inf"><sub>23</sub></span>H<span class="inf"><sub>21</sub></span>N<span class="inf"><sub>3</sub></span>O<span class="inf"><sub>2</sub></span>S, all ring atoms of the 62imidazo[1,2-<span class="it"><i>a</i></span>]benzothieno[3,2-<span class="it"><i>d</i></span>]pyrimidine system are essentially 63coplanar and the phenyl ring is twisted with respect to it 64[dihedral angle = 72.60�(9)�]. The crystal packing is 65mainly governed by C-H<img alt="..." border="0" src="/logos/entities/ctdot_rmgif.gif"/><img alt="[pi]" border="0" src="/logos/entities/pi_rmgif.gif"/> hydrogen bonds and 66intermolecular <img alt="[pi]" border="0" src="/logos/entities/pi_rmgif.gif"/>-<img alt="[pi]" border="0" src="/logos/entities/pi_rmgif.gif"/> interactions, with 67interplanar distances of 3.54�(1) and 683.56�(1)��, and with distances between adjacent ring 69centroids of 3.72�(1) and 3.80�(1) �. The three 70terminal C atoms of the butyl group are disordered over two 71positions; the site occupancy factors are <span class="it"><i>ca</i></span> 0.6 and 0.4.</p> 72</div> 73 74<!-- endabstractdiv --> 75<div class="contentslist"> 76<ul> 77<li class="comment"><a title="Comment" href="#comment">Comment</a></li> 78 79<li class="relatedliterature"><a title="Related literature" href="#relatedliterature">Related literature</a></li> 80 81<li class="experimental"><a title="Experimental" href="#experimental">Experimental</a></li> 82 83<li class="refinement"><a title="Refinement" href="#refinement">Refinement</a></li> 84 85<li class="computingdetails"><a title="Computing details" href="#computingdetails">Computing details</a></li> 86 87<li class="figures"><a title="Figures" href="#figures">Figures</a></li> 88 89<li><a title="(I)" href="#chemicalname1">3-Benzyl-1-butylimidazo[1,2-<i>a</i>]benzothieno[3,2-<i> 90d</i>]pyrimidine- 2,5(1<i>H</i>,3<i>H</i>)-dione</a> 91 92<ul> 93<li><a title="Crystal data" href="#crystaldata1">Crystal 94data</a></li> 95 96<li><a title="Data collection" href="#datacollection1">Data 97collection</a></li> 98 99<li><a title="Refinement data" href="#refinementdata1">Refinement 100data</a></li> 101 102<li class="specialdetails"><a title="Special details" href="#specialdetails1">Special details</a></li> 103 104<li class="licoords"><a title="Fractional atomic coordinates" href="#fractionalatomiccoordinates1">Fractional atomic 105coordinates</a></li> 106 107<li class="liadps"><a title="Atomic displacement parameters" href="#atomicdisplacement1">Atomic displacement parameters</a></li> 108 109<li class="ligeomlong"><a title="Geometric parameters" href="#geometricparameters1">Geometric parameters</a></li> 110 111<li class="lihbondslong"><a title="Hydrogen-bond geometry" href="#hydrogen-bondgeometry1">Hydrogen-bond geometry</a></li> 112 113<li class="lihbondsshort"><a title="Hydrogen-bond geometry" href="#hydrogen-bondgeometry1">Hydrogen-bond geometry</a></li> 114</ul> 115</li> 116 117<li class="acknowledgements"><a title="Acknowledgements" href="#acknowledgements">Acknowledgements</a></li> 118 119<li class="publreferences"><a title="References" href="#publreferences">References</a></li> 120</ul> 121</div> 122 123<!-- endcontentslistdiv --> 124<div class="comment"><a id="comment" name="comment"/> 125 126<div class="heading2">Comment <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 127</div> 128 129<!-- endheading2div --> 130<p>In the field of bioactive molecules, thienopyrimidine have 131received a great deal of attention (Walter, 1999<i>a</i>,b). 132Recently, There have being focused on the synthesis of the fused 133heterocycle systems containing thienopyrimidine <i>via</i> 134aza-Wittig reaction at room temperature(Ding <i>et al.</i>, 2004). 135Herein, we present X-ray crystallographic analysis of the compound 136(I) in this paper, (Fig. 1), which may be used as a new precursor 137for obtaining bioactive molecules.</p> 138 139<p>In the molecule, the bond lengths and angles are unexceptional 140(Cao <i>et al.</i>, 2006; Xu <i>et al.</i>, 2005). The four fused 141rings are close to coplanarity, with maximum deviations 1420.060�(2)� and -0.033�(3)� for O3 and C11, 143respectively, which forms a dihedral angle of 72.60�(9)� 144with the adjacent C18-C23 phenyl ring.</p> 145 146<p>Intermolecular C-H���<span style="font-family:Times">?</span> hydrogen bonds (Table 2) 147seem to be effective in stabilizing the crystal structure. Further 148stability the crystal structure is provided by offset <span style="font-family:Times">?</span>-<span style="font-family:Times">?</span> stacking interactions 149(Janiak, 2000) involving the thiophene (A), the imidazoe (B) and 150the C1-C6 benzene (C) rings. The A:<i>C</i> interplanar distance is 1513.54�(1) � with distances between adjacent ring centroids 152of 3.72�(1)� (symmetry code relating the adjacent rings: 1531 - <i>x</i>, 2 - <i>y</i>, -<i>z</i>). A further interaction 154occurs between B adjacent C rings (symmetry code: 1 - <i>x</i>, 1 - 155<i>y</i>, -<i>z</i>), with an interplanar distance of 1563.56�(1)� and a centroid-to-centroid distance of 1573.80�(1)� (Fig. 2).</p> 158</div> 159 160<!-- endcommentdiv --> 161<div class="relatedliterature"><a id="relatedliterature" name="relatedliterature"/> 162 163<div class="heading2">Related literature <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 164</div> 165 166<!-- endheading2div --> 167<p>Related preparation and biological activity is described by 168Walter (1999<i>a</i>,<i>b</i>). For related literature, see: Ding 169<i>et al.</i> (2004); Janiak (2000). For the crystal structures of 170other fused pyrimidinone derivatives, see: Cao <i>et al.</i> 171(2006); Xu <i>et al.</i> (2005).</p> 172</div> 173 174<!-- endrelatedliteraturediv --> 175<div class="experimental"><a id="experimental" name="experimental"/> 176 177<div class="heading2">Experimental <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 178</div> 179 180<!-- endheading2div --> 181<p>To a solution of the ethyl 1823-((butylimino)methyleneamino)benzothiophene-2-carboxylate (3 mmol) 183in dichloromethane (5 ml) was added ethyl 1842-amino-3-phenylpropanoate (3 mmol). After stirring the reaction 185mixture for 2 h, the solvent was removed and anhydrous ethanol (10 186ml) with several drops of EtONa in EtOH was added. The mixture was 187stirred for 5 h at room temperature. The solution was concentrated 188under reduced pressure and the residue was recrystallized from 189ethanol to give the title compound in a yield of 86%. Crystals 190suitable for single-crystal X-ray diffraction were obtained by 191recrystallization from a mixed solvent of ethanol and 192dichloromethane (1:3 <i>v</i>/<i>v</i>) at room temperature.</p> 193</div> 194 195<!-- endexperimentaldiv --> 196<div class="refinement"><a id="refinement" name="refinement"/> 197 198<div class="heading2">Refinement <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 199</div> 200 201<!-- endheading2div --> 202<p>All H-atoms were positioned geometrically and refined using a 203riding model with C-H = 0.93 �, 204<i>U</i><sub>iso</sub>=1.2<i>U</i><sub>eq</sub> (C) for 205C<i>sp</i><sup>2</sup>, C-H = 0.97 �, <i>U</i><sub>iso</sub> = 2061.2<i>U</i><sub>eq</sub> (C) for CH<sub>2</sub>, C-H = 0.96 �, 207<i>U</i><sub>iso</sub> = 1.5<i>U</i><sub>eq</sub> (C) for 208CH<sub>3</sub>. C14, C15, C16 and attached hydrogen atoms are 209disordered over two sites, with refined occupancies of 2100.387�(9) and 0.613�(9).</p> 211</div> 212 213<!-- endrefinementdiv --> 214<div class="computingdetails"><a id="computingdetails" name="computingdetails"/> 215 216<div class="heading2">Computing details <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 217</div> 218 219<!-- endheading2div --> 220<p>Data collection: <i>SMART</i> (Bruker, 2001); cell refinement: 221<i>SAINT-Plus</i> (Bruker, 2001); data reduction: 222<i>SAINT-Plus</i>; program(s) used to solve structure: 223<i>SHELXS97</i> (Sheldrick, 1997); program(s) used to refine 224structure: <i>SHELXL97</i> (Sheldrick, 1997); molecular graphics: 225<i>PLATON</i> (Spek, 2003); software used to prepare material for 226publication: <i>SHELXTL</i> (Sheldrick, 2001).</p> 227</div> 228 229<!-- endcomputingdetailsdiv --> 230<div class="schemes"><a href="./at2501scheme1.gif"/></div> 231 232<!-- endschemesdiv --> 233<div class="figures"><a id="figures" name="figures"/> 234 235<div class="heading2">Figures <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 236</div> 237 238<!-- endheading2div --> 239<table style="table-layout:fixed" width="100%" class="nodecs"> 240<colgroup span="2"> 241<col width="110"/> 242<col/></colgroup> 243 244<tr> 245<td class="nodecs" align="center" width="110"><a href="./at2501fig1.html"><img width="100" src="./at2501fig1thm.gif" alt="[Figure 1]" align="middle"/></a> </td> 246<td class="nodecs" valign="middle">Fig. 1. The molecular structure 247of the title compound, showing the atom-labeling scheme. 248Displacement ellipsoids are drawn at the 50% probability level. 249Only the major disorder component is shown. </td> 250</tr> 251 252<tr> 253<td class="nodecs" align="center" width="110"><a href="./at2501fig2.html"><img width="100" src="./at2501fig2thm.gif" alt="[Figure 2]" align="middle"/></a> </td> 254<td class="nodecs" valign="middle">Fig. 2. The packing of the title 255compound. </td> 256</tr> 257</table> 258</div> 259 260<!-- endfiguresdiv --> 261<div class="datablock1"> 262<div class="heading2"><a id="chemicalname1" name="chemicalname1"/>3-Benzyl-1-butylimidazo[1,2-<i>a</i>]benzothieno[3,2-<i> 263d</i>]pyrimidine- 2,5(1<i>H</i>,3<i>H</i>)-dione <span class="toplink"><a class="buttons" href="#top">top</a></span> 264<!-- endtoplinkspan --> 265</div> 266 267<!-- endheading2div --> 268<div class="tablewrapcrystaldatalong"><a id="crystaldata1" name="crystaldata1"/><span class="heading3">Crystal data</span> 269<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 270<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 271<colgroup span="2"> 272<col width="50%"/> 273<col width="50%"/></colgroup> 274 275<tr> 276<td width="50%" class="tabledata"> 277C<sub>23</sub>H<sub>21</sub>N<sub>3</sub>O<sub>2</sub>S</td> 278<td width="50%" class="tabledata"><i>F</i><sub>000</sub> = 848</td> 279</tr> 280 281<tr> 282<td width="50%" class="tabledata"><i>M</i><i><sub>r</sub></i> = 283403.49</td> 284<td width="50%" class="tabledata"><i>D</i><sub>x</sub> = 1.324 Mg 285m<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 286</tr> 287 288<tr> 289<td width="50%" class="tabledata">Monoclinic, 290<i>P</i>2<sub>1</sub>/<i>n</i></td> 291<td width="50%" class="tabledata">Mo <i>K</i><span style="font-family:Times">?</span> radiation<br/> 292<span style="font-family:Times">?</span> = 0.71073 �</td> 293</tr> 294 295<tr> 296<td width="50%" class="tabledata">Hall symbol: -P 2yn</td> 297<td width="50%" class="tabledata">Cell parameters from 3589 298reflections</td> 299</tr> 300 301<tr> 302<td width="50%" class="tabledata"><i>a</i> = 13.1732 (16) 303�</td> 304<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 2.3-23.5�</td> 305</tr> 306 307<tr> 308<td width="50%" class="tabledata"><i>b</i> = 8.4957 (11) 309�</td> 310<td width="50%" class="tabledata">� = 0.18 mm<span style="font-family:Times"><sup>?</sup></span><sup>1</sup></td> 311</tr> 312 313<tr> 314<td width="50%" class="tabledata"><i>c</i> = 18.584 (2) �</td> 315<td width="50%" class="tabledata"><i>T</i> = 298 (2) K</td> 316</tr> 317 318<tr> 319<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 103.345 (2)�</td> 320<td width="50%" class="tabledata">Prism, colourless</td> 321</tr> 322 323<tr> 324<td width="50%" class="tabledata"><i>V</i> = 2023.7 (4) 325�<sup>3</sup></td> 326<td width="50%" class="tabledata">0.26 � 0.16 � 0.10 327mm</td> 328</tr> 329 330<tr> 331<td width="50%" class="tabledata"><i>Z</i> = 4</td> 332<td width="50%" class="tabledata"/> 333</tr> 334</table> 335 336<!-- endtabledatatable --> 337</div> 338 339<!-- endtablewrapcrystaldatalongdiv --> 340<div class="tablewrapdatacollectionlong"><a id="datacollection1" name="datacollection1"/><span class="heading3">Data 341collection</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 342<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 343<colgroup span="2"> 344<col width="50%"/> 345<col width="50%"/></colgroup> 346 347<tr> 348<td width="50%" class="tabledata">Bruker SMART 4K CCD 349area0detector<br/> 350diffractometer</td> 351<td width="50%" class="tabledata">3958 independent reflections</td> 352</tr> 353 354<tr> 355<td width="50%" class="tabledata">Radiation source: fine-focus 356sealed tube</td> 357<td width="50%" class="tabledata">2896 reflections with <i>I</i> 358> 2<span style="font-family:Times">?</span>(<i>I</i>)</td> 359</tr> 360 361<tr> 362<td width="50%" class="tabledata">Monochromator: graphite</td> 363<td width="50%" class="tabledata"><i>R</i><sub>int</sub> = 3640.129</td> 365</tr> 366 367<tr> 368<td width="50%" class="tabledata"><i>T</i> = 298(2) K</td> 369<td width="50%" class="tabledata"><span style="font-family:Times">?</span><sub>max</sub> = 37026.0�</td> 371</tr> 372 373<tr> 374<td width="50%" class="tabledata"><span style="font-family:Times">?</span> and <span style="font-family:Times">?</span> scans</td> 375<td width="50%" class="tabledata"><span style="font-family:Times">?</span><sub>min</sub> = 3761.7�</td> 377</tr> 378 379<tr> 380<td width="50%" class="tabledata">Absorption correction: 381multi-scan<br/> 382(SADABS; Sheldrick, 2003)</td> 383<td width="50%" class="tabledata"><i>h</i> = <span style="font-family:Times">?</span>16?16</td> 384</tr> 385 386<tr> 387<td width="50%" class="tabledata"><i>T</i><sub>min</sub> = 0.954, 388<i>T</i><sub>max</sub> = 0.982</td> 389<td width="50%" class="tabledata"><i>k</i> = <span style="font-family:Times">?</span>10?10</td> 390</tr> 391 392<tr> 393<td width="50%" class="tabledata">15534 measured reflections</td> 394<td width="50%" class="tabledata"><i>l</i> = <span style="font-family:Times">?</span>22?22</td> 395</tr> 396</table> 397 398<!-- endtabledatatable --> 399</div> 400 401<!-- endtablewrapdatacollectionlongdiv --> 402<div class="tablewraprefinementdatalong"><a id="refinementdata1" name="refinementdata1"/><span class="heading3">Refinement</span> 403<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 404<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 405<colgroup span="2"> 406<col width="50%"/> 407<col width="50%"/></colgroup> 408 409<tr> 410<td width="50%" class="tabledata">Refinement on 411<i>F</i><sup>2</sup></td> 412<td width="50%" class="tabledata">Secondary atom site location: 413difference Fourier map</td> 414</tr> 415 416<tr> 417<td width="50%" class="tabledata">Least-squares matrix: full</td> 418<td width="50%" class="tabledata">Hydrogen site location: inferred 419from neighbouring sites</td> 420</tr> 421 422<tr> 423<td width="50%" class="tabledata"><i>R</i>[<i>F</i><sup>2</sup> 424> 2<span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>)] = 4250.059</td> 426<td width="50%" class="tabledata">H-atom parameters 427constrained</td> 428</tr> 429 430<tr> 431<td width="50%" class="tabledata"><i>wR</i>(<i>F</i><sup>2</sup>) = 4320.170</td> 433<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> 4342</sup>) + (0.0962<i>P</i>)<sup>2</sup>]<br/> 435where <i>P</i> = (<i>F</i><sub>o</sub><sup>2</sup> + 4362<i>F</i><sub>c</sub><sup>2</sup>)/3</td> 437</tr> 438 439<tr> 440<td width="50%" class="tabledata"><i>S</i> = 1.00</td> 441<td width="50%" class="tabledata">(?/<span style="font-family:Times">?</span>)<sub>max</sub> < 4420.001</td> 443</tr> 444 445<tr> 446<td width="50%" class="tabledata">3958 reflections</td> 447<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>max</sub> = 0.26 e 448�<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 449</tr> 450 451<tr> 452<td width="50%" class="tabledata">292 parameters</td> 453<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>min</sub> = <span style="font-family:Times">?</span>0.32 e �<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 454</tr> 455 456<tr> 457<td width="50%" class="tabledata">22 restraints</td> 458<td width="50%" class="tabledata">Extinction correction: none</td> 459</tr> 460 461<tr> 462<td width="50%" class="tabledata">Primary atom site location: 463structure-invariant direct methods</td> 464<td width="50%" class="tabledata"/> 465</tr> 466</table> 467 468<!-- endtabledatatable --> 469</div> 470 471<!-- endtablewraprefinementdatalongdiv --> 472<div class="tablewrapcrystaldatashort"><a id="crystaldata1" name="crystaldata1"/><span class="heading3">Crystal data</span> 473<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 474<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 475<colgroup span="2"> 476<col width="50%"/> 477<col width="50%"/></colgroup> 478 479<tr> 480<td width="50%" class="tabledata"> 481C<sub>23</sub>H<sub>21</sub>N<sub>3</sub>O<sub>2</sub>S</td> 482<td width="50%" class="tabledata"><i>V</i> = 2023.7 (4) 483�<sup>3</sup></td> 484</tr> 485 486<tr> 487<td width="50%" class="tabledata"><i>M</i><i><sub>r</sub></i> = 488403.49</td> 489<td width="50%" class="tabledata"><i>Z</i> = 4</td> 490</tr> 491 492<tr> 493<td width="50%" class="tabledata">Monoclinic, 494<i>P</i>2<sub>1</sub>/<i>n</i></td> 495<td width="50%" class="tabledata">Mo <i>K</i><span style="font-family:Times">?</span></td> 496</tr> 497 498<tr> 499<td width="50%" class="tabledata"><i>a</i> = 13.1732 (16) 500�</td> 501<td width="50%" class="tabledata">� = 0.18 mm<span style="font-family:Times"><sup>?</sup></span><sup>1</sup></td> 502</tr> 503 504<tr> 505<td width="50%" class="tabledata"><i>b</i> = 8.4957 (11) 506�</td> 507<td width="50%" class="tabledata"><i>T</i> = 298 (2) K</td> 508</tr> 509 510<tr> 511<td width="50%" class="tabledata"><i>c</i> = 18.584 (2) �</td> 512<td width="50%" class="tabledata">0.26 � 0.16 � 0.10 513mm</td> 514</tr> 515 516<tr> 517<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 103.345 (2)�</td> 518<td width="50%" class="tabledata"/> 519</tr> 520</table> 521 522<!-- endtabledatatable --> 523</div> 524 525<!-- endtablewrapcrystaldatashortdiv --> 526<div class="tablewrapdatacollectionshort"><a id="datacollection1" name="datacollection1"/><span class="heading3">Data 527collection</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 528<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 529<colgroup span="2"> 530<col width="50%"/> 531<col width="50%"/></colgroup> 532 533<tr> 534<td width="50%" class="tabledata">Bruker SMART 4K CCD 535area0detector<br/> 536diffractometer</td> 537<td width="50%" class="tabledata">3958 independent reflections</td> 538</tr> 539 540<tr> 541<td width="50%" class="tabledata">Absorption correction: 542multi-scan<br/> 543(SADABS; Sheldrick, 2003)</td> 544<td width="50%" class="tabledata">2896 reflections with <i>I</i> 545> 2<span style="font-family:Times">?</span>(<i>I</i>)</td> 546</tr> 547 548<tr> 549<td width="50%" class="tabledata"><i>T</i><sub>min</sub> = 0.954, 550<i>T</i><sub>max</sub> = 0.982</td> 551<td width="50%" class="tabledata"><i>R</i><sub>int</sub> = 5520.129</td> 553</tr> 554 555<tr> 556<td width="50%" class="tabledata">15534 measured reflections</td> 557<td width="50%" class="tabledata"/> 558</tr> 559</table> 560 561<!-- endtabledatatable --> 562</div> 563 564<!-- endtablewrapdatacollectionshortdiv --> 565<div class="tablewraprefinementdatashort"><a id="refinementdata1" name="refinementdata1"/><span class="heading3">Refinement</span> 566<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 567<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 568<colgroup span="2"> 569<col width="50%"/> 570<col width="50%"/></colgroup> 571 572<tr> 573<td width="50%" class="tabledata"><i>R</i>[<i>F</i><sup>2</sup> 574> 2<span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>)] = 5750.059</td> 576<td width="50%" class="tabledata">22 restraints</td> 577</tr> 578 579<tr> 580<td width="50%" class="tabledata"><i>wR</i>(<i>F</i><sup>2</sup>) = 5810.170</td> 582<td width="50%" class="tabledata">H-atom parameters 583constrained</td> 584</tr> 585 586<tr> 587<td width="50%" class="tabledata"><i>S</i> = 1.00</td> 588<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>max</sub> = 0.26 e 589�<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 590</tr> 591 592<tr> 593<td width="50%" class="tabledata">3958 reflections</td> 594<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>min</sub> = <span style="font-family:Times">?</span>0.32 e �<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 595</tr> 596 597<tr> 598<td width="50%" class="tabledata">292 parameters</td> 599<td width="50%" class="tabledata"/> 600</tr> 601</table> 602 603<!-- endtabledatatable --> 604</div> 605 606<!-- endtablewraprefinementdatashortdiv --> 607<div class="specialdetails"><a id="specialdetails1" name="specialdetails1"/><span class="heading3">Special 608details</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 609<table style="table-layout:fixed" width="100%" class="tabledata"> 610<tr> 611<td class="tabledata"> 612<p><b>Geometry</b>. All e.s.d.'s (except the e.s.d. in the 613dihedral angle between two l.s. planes) are estimated using the 614full covariance matrix. The cell e.s.d.'s are taken into 615account individually in the estimation of e.s.d.'s in 616distances, angles and torsion angles; correlations between 617e.s.d.'s in cell parameters are only used when they are defined 618by crystal symmetry. An approximate (isotropic) treatment of cell 619e.s.d.'s is used for estimating e.s.d.'s involving l.s. 620planes.</p> 621</td> 622</tr> 623 624<tr> 625<td class="tabledata"> 626<p><b>Refinement</b>. Refinement of <i>F</i><sup>2</sup> against 627ALL reflections. The weighted <i>R</i>-factor <i>wR</i> and 628goodness of fit <i>S</i> are based on <i>F</i><sup>2</sup>, 629conventional <i>R</i>-factors <i>R</i> are based on <i>F</i>, with 630<i>F</i> set to zero for negative <i>F</i><sup>2</sup>. The 631threshold expression of <i>F</i><sup>2</sup> > <span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>) is 632used only for calculating <i>R</i>-factors(gt) <i>etc</i>. and is 633not relevant to the choice of reflections for refinement. 634<i>R</i>-factors based on <i>F</i><sup>2</sup> are statistically 635about twice as large as those based on <i>F</i>, and <i>R</i>- 636factors based on ALL data will be even larger.</p> 637</td> 638</tr> 639</table> 640</div> 641 642<!-- endspecialdetailsdiv --> 643<div class="tablewrapcoords"><a id="fractionalatomiccoordinates1" name="fractionalatomiccoordinates1"/> <span class="heading3">Fractional atomic coordinates and isotropic or 644equivalent isotropic displacement parameters 645(�<sup>2</sup>)</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span> 646<!-- endtoplinkspan --> 647<table style="table-layout:fixed" width="100%" summary="" class="tabledata"> 648<tr> 649<td class="tabledata"/> 650<td class="tabledata"><i>x</i></td> 651<td class="tabledata"><i>y</i></td> 652<td class="tabledata"><i>z</i></td> 653<td class="tabledata"> 654<i>U</i><sub>iso</sub>*/<i>U</i><sub>eq</sub></td> 655<td class="tabledata">Occ. (<1)</td> 656</tr> 657 658<tr> 659<td class="tabledata">C1</td> 660<td class="tabledata">0.45304 (17)</td> 661<td class="tabledata">0.7981 (3)</td> 662<td class="tabledata">0.00701 (13)</td> 663<td class="tabledata">0.0455 (6)</td> 664<td class="tabledata"/> 665</tr> 666 667<tr> 668<td class="tabledata">C2</td> 669<td class="tabledata">0.40479 (19)</td> 670<td class="tabledata">0.8227 (3)</td> 671<td class="tabledata"><span style="font-family:Times">?</span>0.06750 (13)</td> 672<td class="tabledata">0.0541 (6)</td> 673<td class="tabledata"/> 674</tr> 675 676<tr> 677<td class="tabledata">H2</td> 678<td class="tabledata">0.4330</td> 679<td class="tabledata">0.7798</td> 680<td class="tabledata"><span style="font-family:Times">?</span>0.1046</td> 681<td class="tabledata">0.065*</td> 682<td class="tabledata"/> 683</tr> 684 685<tr> 686<td class="tabledata">C3</td> 687<td class="tabledata">0.31509 (19)</td> 688<td class="tabledata">0.9112 (3)</td> 689<td class="tabledata"><span style="font-family:Times">?</span>0.08510 (14)</td> 690<td class="tabledata">0.0613 (7)</td> 691<td class="tabledata"/> 692</tr> 693 694<tr> 695<td class="tabledata">H3</td> 696<td class="tabledata">0.2828</td> 697<td class="tabledata">0.9287</td> 698<td class="tabledata"><span style="font-family:Times">?</span>0.1345</td> 699<td class="tabledata">0.074*</td> 700<td class="tabledata"/> 701</tr> 702 703<tr> 704<td class="tabledata">C4</td> 705<td class="tabledata">0.27219 (19)</td> 706<td class="tabledata">0.9745 (3)</td> 707<td class="tabledata"><span style="font-family:Times">?</span>0.03029 (15)</td> 708<td class="tabledata">0.0658 (8)</td> 709<td class="tabledata"/> 710</tr> 711 712<tr> 713<td class="tabledata">H4</td> 714<td class="tabledata">0.2111</td> 715<td class="tabledata">1.0332</td> 716<td class="tabledata"><span style="font-family:Times">?</span>0.0435</td> 717<td class="tabledata">0.079*</td> 718<td class="tabledata"/> 719</tr> 720 721<tr> 722<td class="tabledata">C5</td> 723<td class="tabledata">0.31784 (19)</td> 724<td class="tabledata">0.9528 (3)</td> 725<td class="tabledata">0.04333 (15)</td> 726<td class="tabledata">0.0605 (7)</td> 727<td class="tabledata"/> 728</tr> 729 730<tr> 731<td class="tabledata">H5</td> 732<td class="tabledata">0.2883</td> 733<td class="tabledata">0.9956</td> 734<td class="tabledata">0.0798</td> 735<td class="tabledata">0.073*</td> 736<td class="tabledata"/> 737</tr> 738 739<tr> 740<td class="tabledata">C6</td> 741<td class="tabledata">0.40899 (17)</td> 742<td class="tabledata">0.8655 (3)</td> 743<td class="tabledata">0.06174 (13)</td> 744<td class="tabledata">0.0500 (6)</td> 745<td class="tabledata"/> 746</tr> 747 748<tr> 749<td class="tabledata">C7</td> 750<td class="tabledata">0.54724 (16)</td> 751<td class="tabledata">0.7149 (3)</td> 752<td class="tabledata">0.03847 (12)</td> 753<td class="tabledata">0.0441 (5)</td> 754<td class="tabledata"/> 755</tr> 756 757<tr> 758<td class="tabledata">C8</td> 759<td class="tabledata">0.57103 (17)</td> 760<td class="tabledata">0.7199 (3)</td> 761<td class="tabledata">0.11501 (12)</td> 762<td class="tabledata">0.0465 (6)</td> 763<td class="tabledata"/> 764</tr> 765 766<tr> 767<td class="tabledata">C9</td> 768<td class="tabledata">0.66293 (18)</td> 769<td class="tabledata">0.6487 (3)</td> 770<td class="tabledata">0.15852 (12)</td> 771<td class="tabledata">0.0497 (6)</td> 772<td class="tabledata"/> 773</tr> 774 775<tr> 776<td class="tabledata">C10</td> 777<td class="tabledata">0.68847 (18)</td> 778<td class="tabledata">0.5729 (3)</td> 779<td class="tabledata">0.03767 (12)</td> 780<td class="tabledata">0.0454 (5)</td> 781<td class="tabledata"/> 782</tr> 783 784<tr> 785<td class="tabledata">C11</td> 786<td class="tabledata">0.8372 (2)</td> 787<td class="tabledata">0.4266 (3)</td> 788<td class="tabledata">0.06606 (15)</td> 789<td class="tabledata">0.0563 (6)</td> 790<td class="tabledata"/> 791</tr> 792 793<tr> 794<td class="tabledata">C12</td> 795<td class="tabledata">0.81459 (18)</td> 796<td class="tabledata">0.4798 (3)</td> 797<td class="tabledata">0.13877 (14)</td> 798<td class="tabledata">0.0544 (6)</td> 799<td class="tabledata"/> 800</tr> 801 802<tr> 803<td class="tabledata">H12</td> 804<td class="tabledata">0.7970</td> 805<td class="tabledata">0.3870</td> 806<td class="tabledata">0.1648</td> 807<td class="tabledata">0.065*</td> 808<td class="tabledata"/> 809</tr> 810 811<tr> 812<td class="tabledata">C13</td> 813<td class="tabledata">0.7543 (2)</td> 814<td class="tabledata">0.4725 (3)</td> 815<td class="tabledata"><span style="font-family:Times">?</span>0.06900 (13)</td> 816<td class="tabledata">0.0638 (7)</td> 817<td class="tabledata"/> 818</tr> 819 820<tr> 821<td class="tabledata">H13A</td> 822<td class="tabledata">0.6849</td> 823<td class="tabledata">0.4359</td> 824<td class="tabledata"><span style="font-family:Times">?</span>0.0928</td> 825<td class="tabledata">0.077*</td> 826<td class="tabledata">0.613�(9)</td> 827</tr> 828 829<tr> 830<td class="tabledata">H13B</td> 831<td class="tabledata">0.8029</td> 832<td class="tabledata">0.3908</td> 833<td class="tabledata"><span style="font-family:Times">?</span>0.0754</td> 834<td class="tabledata">0.077*</td> 835<td class="tabledata">0.613�(9)</td> 836</tr> 837 838<tr> 839<td class="tabledata">H13C</td> 840<td class="tabledata">0.6838</td> 841<td class="tabledata">0.4415</td> 842<td class="tabledata"><span style="font-family:Times">?</span>0.0932</td> 843<td class="tabledata">0.077*</td> 844<td class="tabledata">0.387�(9)</td> 845</tr> 846 847<tr> 848<td class="tabledata">H13D</td> 849<td class="tabledata">0.8002</td> 850<td class="tabledata">0.3872</td> 851<td class="tabledata"><span style="font-family:Times">?</span>0.0756</td> 852<td class="tabledata">0.077*</td> 853<td class="tabledata">0.387�(9)</td> 854</tr> 855 856<tr> 857<td class="tabledata">C14</td> 858<td class="tabledata">0.8106 (7)</td> 859<td class="tabledata">0.6116 (9)</td> 860<td class="tabledata"><span style="font-family:Times">?</span>0.0933 (4)</td> 861<td class="tabledata">0.062 (2)</td> 862<td class="tabledata">0.613�(9)</td> 863</tr> 864 865<tr> 866<td class="tabledata">H14A</td> 867<td class="tabledata">0.8832</td> 868<td class="tabledata">0.6084</td> 869<td class="tabledata"><span style="font-family:Times">?</span>0.0668</td> 870<td class="tabledata">0.074*</td> 871<td class="tabledata">0.613�(9)</td> 872</tr> 873 874<tr> 875<td class="tabledata">H14B</td> 876<td class="tabledata">0.7807</td> 877<td class="tabledata">0.7079</td> 878<td class="tabledata"><span style="font-family:Times">?</span>0.0793</td> 879<td class="tabledata">0.074*</td> 880<td class="tabledata">0.613�(9)</td> 881</tr> 882 883<tr> 884<td class="tabledata">C15</td> 885<td class="tabledata">0.8060 (5)</td> 886<td class="tabledata">0.6175 (9)</td> 887<td class="tabledata"><span style="font-family:Times">?</span>0.1761 (3)</td> 888<td class="tabledata">0.087 (2)</td> 889<td class="tabledata">0.613�(9)</td> 890</tr> 891 892<tr> 893<td class="tabledata">H15A</td> 894<td class="tabledata">0.8560</td> 895<td class="tabledata">0.6945</td> 896<td class="tabledata"><span style="font-family:Times">?</span>0.1852</td> 897<td class="tabledata">0.105*</td> 898<td class="tabledata">0.613�(9)</td> 899</tr> 900 901<tr> 902<td class="tabledata">H15B</td> 903<td class="tabledata">0.8260</td> 904<td class="tabledata">0.5156</td> 905<td class="tabledata"><span style="font-family:Times">?</span>0.1920</td> 906<td class="tabledata">0.105*</td> 907<td class="tabledata">0.613�(9)</td> 908</tr> 909 910<tr> 911<td class="tabledata">C16</td> 912<td class="tabledata">0.7009 (7)</td> 913<td class="tabledata">0.6589 (14)</td> 914<td class="tabledata"><span style="font-family:Times">?</span>0.2207 (5)</td> 915<td class="tabledata">0.154 (4)</td> 916<td class="tabledata">0.613�(9)</td> 917</tr> 918 919<tr> 920<td class="tabledata">H16A</td> 921<td class="tabledata">0.6520</td> 922<td class="tabledata">0.5788</td> 923<td class="tabledata"><span style="font-family:Times">?</span>0.2150</td> 924<td class="tabledata">0.230*</td> 925<td class="tabledata">0.613�(9)</td> 926</tr> 927 928<tr> 929<td class="tabledata">H16B</td> 930<td class="tabledata">0.7031</td> 931<td class="tabledata">0.6667</td> 932<td class="tabledata"><span style="font-family:Times">?</span>0.2719</td> 933<td class="tabledata">0.230*</td> 934<td class="tabledata">0.613�(9)</td> 935</tr> 936 937<tr> 938<td class="tabledata">H16C</td> 939<td class="tabledata">0.6797</td> 940<td class="tabledata">0.7580</td> 941<td class="tabledata"><span style="font-family:Times">?</span>0.2042</td> 942<td class="tabledata">0.230*</td> 943<td class="tabledata">0.613�(9)</td> 944</tr> 945 946<tr> 947<td class="tabledata">C14'</td> 948<td class="tabledata">0.7768 (13)</td> 949<td class="tabledata">0.6158 (15)</td> 950<td class="tabledata"><span style="font-family:Times">?</span>0.1097 (5)</td> 951<td class="tabledata">0.076 (4)</td> 952<td class="tabledata">0.387�(9)</td> 953</tr> 954 955<tr> 956<td class="tabledata">H14C</td> 957<td class="tabledata">0.8496</td> 958<td class="tabledata">0.6457</td> 959<td class="tabledata"><span style="font-family:Times">?</span>0.0940</td> 960<td class="tabledata">0.091*</td> 961<td class="tabledata">0.387�(9)</td> 962</tr> 963 964<tr> 965<td class="tabledata">H14D</td> 966<td class="tabledata">0.7337</td> 967<td class="tabledata">0.7037</td> 968<td class="tabledata"><span style="font-family:Times">?</span>0.1018</td> 969<td class="tabledata">0.091*</td> 970<td class="tabledata">0.387�(9)</td> 971</tr> 972 973<tr> 974<td class="tabledata">C15'</td> 975<td class="tabledata">0.7494 (10)</td> 976<td class="tabledata">0.5634 (13)</td> 977<td class="tabledata"><span style="font-family:Times">?</span>0.1926 (4)</td> 978<td class="tabledata">0.101 (4)</td> 979<td class="tabledata">0.387�(9)</td> 980</tr> 981 982<tr> 983<td class="tabledata">H15C</td> 984<td class="tabledata">0.7920</td> 985<td class="tabledata">0.4746</td> 986<td class="tabledata"><span style="font-family:Times">?</span>0.2002</td> 987<td class="tabledata">0.121*</td> 988<td class="tabledata">0.387�(9)</td> 989</tr> 990 991<tr> 992<td class="tabledata">H15D</td> 993<td class="tabledata">0.6765</td> 994<td class="tabledata">0.5343</td> 995<td class="tabledata"><span style="font-family:Times">?</span>0.2083</td> 996<td class="tabledata">0.121*</td> 997<td class="tabledata">0.387�(9)</td> 998</tr> 999 1000<tr> 1001<td class="tabledata">C16'</td> 1002<td class="tabledata">0.7727 (11)</td> 1003<td class="tabledata">0.7057 (14)</td> 1004<td class="tabledata"><span style="font-family:Times">?</span>0.2344 (5)</td> 1005<td class="tabledata">0.117 (4)</td> 1006<td class="tabledata">0.387�(9)</td> 1007</tr> 1008 1009<tr> 1010<td class="tabledata">H16D</td> 1011<td class="tabledata">0.7340</td> 1012<td class="tabledata">0.7943</td> 1013<td class="tabledata"><span style="font-family:Times">?</span>0.2230</td> 1014<td class="tabledata">0.175*</td> 1015<td class="tabledata">0.387�(9)</td> 1016</tr> 1017 1018<tr> 1019<td class="tabledata">H16E</td> 1020<td class="tabledata">0.7528</td> 1021<td class="tabledata">0.6849</td> 1022<td class="tabledata"><span style="font-family:Times">?</span>0.2866</td> 1023<td class="tabledata">0.175*</td> 1024<td class="tabledata">0.387�(9)</td> 1025</tr> 1026 1027<tr> 1028<td class="tabledata">H16F</td> 1029<td class="tabledata">0.8460</td> 1030<td class="tabledata">0.7285</td> 1031<td class="tabledata"><span style="font-family:Times">?</span>0.2204</td> 1032<td class="tabledata">0.175*</td> 1033<td class="tabledata">0.387�(9)</td> 1034</tr> 1035 1036<tr> 1037<td class="tabledata">C17</td> 1038<td class="tabledata">0.90741 (18)</td> 1039<td class="tabledata">0.5630 (3)</td> 1040<td class="tabledata">0.18900 (13)</td> 1041<td class="tabledata">0.0555 (7)</td> 1042<td class="tabledata"/> 1043</tr> 1044 1045<tr> 1046<td class="tabledata">H17A</td> 1047<td class="tabledata">0.8906</td> 1048<td class="tabledata">0.5818</td> 1049<td class="tabledata">0.2364</td> 1050<td class="tabledata">0.067*</td> 1051<td class="tabledata"/> 1052</tr> 1053 1054<tr> 1055<td class="tabledata">H17B</td> 1056<td class="tabledata">0.9667</td> 1057<td class="tabledata">0.4920</td> 1058<td class="tabledata">0.1975</td> 1059<td class="tabledata">0.067*</td> 1060<td class="tabledata"/> 1061</tr> 1062 1063<tr> 1064<td class="tabledata">C18</td> 1065<td class="tabledata">0.93996 (16)</td> 1066<td class="tabledata">0.7166 (3)</td> 1067<td class="tabledata">0.16112 (12)</td> 1068<td class="tabledata">0.0475 (6)</td> 1069<td class="tabledata"/> 1070</tr> 1071 1072<tr> 1073<td class="tabledata">C19</td> 1074<td class="tabledata">0.99200 (17)</td> 1075<td class="tabledata">0.7229 (3)</td> 1076<td class="tabledata">0.10411 (13)</td> 1077<td class="tabledata">0.0509 (6)</td> 1078<td class="tabledata"/> 1079</tr> 1080 1081<tr> 1082<td class="tabledata">H19</td> 1083<td class="tabledata">1.0040</td> 1084<td class="tabledata">0.6301</td> 1085<td class="tabledata">0.0808</td> 1086<td class="tabledata">0.061*</td> 1087<td class="tabledata"/> 1088</tr> 1089 1090<tr> 1091<td class="tabledata">C20</td> 1092<td class="tabledata">1.02611 (18)</td> 1093<td class="tabledata">0.8632 (3)</td> 1094<td class="tabledata">0.08140 (14)</td> 1095<td class="tabledata">0.0543 (6)</td> 1096<td class="tabledata"/> 1097</tr> 1098 1099<tr> 1100<td class="tabledata">H20</td> 1101<td class="tabledata">1.0604</td> 1102<td class="tabledata">0.8644</td> 1103<td class="tabledata">0.0429</td> 1104<td class="tabledata">0.065*</td> 1105<td class="tabledata"/> 1106</tr> 1107 1108<tr> 1109<td class="tabledata">C21</td> 1110<td class="tabledata">1.00975 (19)</td> 1111<td class="tabledata">1.0019 (3)</td> 1112<td class="tabledata">0.11538 (14)</td> 1113<td class="tabledata">0.0593 (7)</td> 1114<td class="tabledata"/> 1115</tr> 1116 1117<tr> 1118<td class="tabledata">H21</td> 1119<td class="tabledata">1.0336</td> 1120<td class="tabledata">1.0966</td> 1121<td class="tabledata">0.1004</td> 1122<td class="tabledata">0.071*</td> 1123<td class="tabledata"/> 1124</tr> 1125 1126<tr> 1127<td class="tabledata">C22</td> 1128<td class="tabledata">0.9581 (2)</td> 1129<td class="tabledata">0.9992 (3)</td> 1130<td class="tabledata">0.17149 (15)</td> 1131<td class="tabledata">0.0643 (7)</td> 1132<td class="tabledata"/> 1133</tr> 1134 1135<tr> 1136<td class="tabledata">H22</td> 1137<td class="tabledata">0.9465</td> 1138<td class="tabledata">1.0925</td> 1139<td class="tabledata">0.1945</td> 1140<td class="tabledata">0.077*</td> 1141<td class="tabledata"/> 1142</tr> 1143 1144<tr> 1145<td class="tabledata">C23</td> 1146<td class="tabledata">0.92311 (19)</td> 1147<td class="tabledata">0.8578 (3)</td> 1148<td class="tabledata">0.19387 (13)</td> 1149<td class="tabledata">0.0575 (7)</td> 1150<td class="tabledata"/> 1151</tr> 1152 1153<tr> 1154<td class="tabledata">H23</td> 1155<td class="tabledata">0.8876</td> 1156<td class="tabledata">0.8575</td> 1157<td class="tabledata">0.2317</td> 1158<td class="tabledata">0.069*</td> 1159<td class="tabledata"/> 1160</tr> 1161 1162<tr> 1163<td class="tabledata">N1</td> 1164<td class="tabledata">0.60676 (14)</td> 1165<td class="tabledata">0.6380 (2)</td> 1166<td class="tabledata"><span style="font-family:Times">?</span>0.00223 (10)</td> 1167<td class="tabledata">0.0468 (5)</td> 1168<td class="tabledata"/> 1169</tr> 1170 1171<tr> 1172<td class="tabledata">N2</td> 1173<td class="tabledata">0.75950 (15)</td> 1174<td class="tabledata">0.4872 (2)</td> 1175<td class="tabledata">0.01036 (11)</td> 1176<td class="tabledata">0.0521 (5)</td> 1177<td class="tabledata"/> 1178</tr> 1179 1180<tr> 1181<td class="tabledata">N3</td> 1182<td class="tabledata">0.72009 (13)</td> 1183<td class="tabledata">0.5741 (2)</td> 1184<td class="tabledata">0.11365 (9)</td> 1185<td class="tabledata">0.0476 (5)</td> 1186<td class="tabledata"/> 1187</tr> 1188 1189<tr> 1190<td class="tabledata">O1</td> 1191<td class="tabledata">0.69271 (13)</td> 1192<td class="tabledata">0.6488 (2)</td> 1193<td class="tabledata">0.22618 (9)</td> 1194<td class="tabledata">0.0653 (5)</td> 1195<td class="tabledata"/> 1196</tr> 1197 1198<tr> 1199<td class="tabledata">O2</td> 1200<td class="tabledata">0.91073 (15)</td> 1201<td class="tabledata">0.3495 (2)</td> 1202<td class="tabledata">0.05804 (11)</td> 1203<td class="tabledata">0.0710 (6)</td> 1204<td class="tabledata"/> 1205</tr> 1206 1207<tr> 1208<td class="tabledata">S1</td> 1209<td class="tabledata">0.48079 (5)</td> 1210<td class="tabledata">0.82378 (9)</td> 1211<td class="tabledata">0.15079 (3)</td> 1212<td class="tabledata">0.0585 (3)</td> 1213<td class="tabledata"/> 1214</tr> 1215</table> 1216</div> 1217 1218<!-- endtablewrapcoordsdiv --> 1219<div class="tablewrapadps"><a id="atomicdisplacement1" name="atomicdisplacement1"/> <span class="heading3">Atomic 1220displacement parameters (�<sup>2</sup>)</span> 1221<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 1222<table style="table-layout:fixed" width="100%" summary="" class="tabledata"> 1223<tr> 1224<td class="tabledata"/> 1225<td class="tabledata"><i>U</i><sup>11</sup></td> 1226<td class="tabledata"><i>U</i><sup>22</sup></td> 1227<td class="tabledata"><i>U</i><sup>33</sup></td> 1228<td class="tabledata"><i>U</i><sup>12</sup></td> 1229<td class="tabledata"><i>U</i><sup>13</sup></td> 1230<td class="tabledata"><i>U</i><sup>23</sup></td> 1231</tr> 1232 1233<tr> 1234<td class="tabledata">C1</td> 1235<td class="tabledata">0.0434 (12)</td> 1236<td class="tabledata">0.0490 (14)</td> 1237<td class="tabledata">0.0430 (12)</td> 1238<td class="tabledata"><span style="font-family:Times">?</span>0.0121 (10)</td> 1239<td class="tabledata">0.0076 (10)</td> 1240<td class="tabledata"><span style="font-family:Times">?</span>0.0026 (10)</td> 1241</tr> 1242 1243<tr> 1244<td class="tabledata">C2</td> 1245<td class="tabledata">0.0530 (14)</td> 1246<td class="tabledata">0.0616 (16)</td> 1247<td class="tabledata">0.0450 (13)</td> 1248<td class="tabledata"><span style="font-family:Times">?</span>0.0097 (12)</td> 1249<td class="tabledata">0.0054 (11)</td> 1250<td class="tabledata"><span style="font-family:Times">?</span>0.0037 (11)</td> 1251</tr> 1252 1253<tr> 1254<td class="tabledata">C3</td> 1255<td class="tabledata">0.0555 (15)</td> 1256<td class="tabledata">0.0682 (18)</td> 1257<td class="tabledata">0.0539 (14)</td> 1258<td class="tabledata"><span style="font-family:Times">?</span>0.0071 (13)</td> 1259<td class="tabledata"><span style="font-family:Times">?</span>0.0001 (12)</td> 1260<td class="tabledata">0.0033 (13)</td> 1261</tr> 1262 1263<tr> 1264<td class="tabledata">C4</td> 1265<td class="tabledata">0.0513 (15)</td> 1266<td class="tabledata">0.0627 (18)</td> 1267<td class="tabledata">0.0779 (19)</td> 1268<td class="tabledata">0.0005 (13)</td> 1269<td class="tabledata">0.0037 (14)</td> 1270<td class="tabledata"><span style="font-family:Times">?</span>0.0013 (15)</td> 1271</tr> 1272 1273<tr> 1274<td class="tabledata">C5</td> 1275<td class="tabledata">0.0517 (14)</td> 1276<td class="tabledata">0.0638 (17)</td> 1277<td class="tabledata">0.0666 (16)</td> 1278<td class="tabledata"><span style="font-family:Times">?</span>0.0008 (12)</td> 1279<td class="tabledata">0.0149 (12)</td> 1280<td class="tabledata"><span style="font-family:Times">?</span>0.0094 (13)</td> 1281</tr> 1282 1283<tr> 1284<td class="tabledata">C6</td> 1285<td class="tabledata">0.0454 (13)</td> 1286<td class="tabledata">0.0577 (15)</td> 1287<td class="tabledata">0.0463 (13)</td> 1288<td class="tabledata"><span style="font-family:Times">?</span>0.0114 (11)</td> 1289<td class="tabledata">0.0093 (11)</td> 1290<td class="tabledata"><span style="font-family:Times">?</span>0.0051 (11)</td> 1291</tr> 1292 1293<tr> 1294<td class="tabledata">C7</td> 1295<td class="tabledata">0.0422 (12)</td> 1296<td class="tabledata">0.0504 (14)</td> 1297<td class="tabledata">0.0396 (11)</td> 1298<td class="tabledata"><span style="font-family:Times">?</span>0.0098 (10)</td> 1299<td class="tabledata">0.0092 (10)</td> 1300<td class="tabledata"><span style="font-family:Times">?</span>0.0035 (10)</td> 1301</tr> 1302 1303<tr> 1304<td class="tabledata">C8</td> 1305<td class="tabledata">0.0448 (12)</td> 1306<td class="tabledata">0.0572 (15)</td> 1307<td class="tabledata">0.0391 (12)</td> 1308<td class="tabledata"><span style="font-family:Times">?</span>0.0085 (11)</td> 1309<td class="tabledata">0.0132 (10)</td> 1310<td class="tabledata"><span style="font-family:Times">?</span>0.0015 (10)</td> 1311</tr> 1312 1313<tr> 1314<td class="tabledata">C9</td> 1315<td class="tabledata">0.0477 (13)</td> 1316<td class="tabledata">0.0636 (16)</td> 1317<td class="tabledata">0.0390 (12)</td> 1318<td class="tabledata"><span style="font-family:Times">?</span>0.0122 (11)</td> 1319<td class="tabledata">0.0124 (10)</td> 1320<td class="tabledata">0.0058 (11)</td> 1321</tr> 1322 1323<tr> 1324<td class="tabledata">C10</td> 1325<td class="tabledata">0.0520 (13)</td> 1326<td class="tabledata">0.0441 (13)</td> 1327<td class="tabledata">0.0422 (12)</td> 1328<td class="tabledata"><span style="font-family:Times">?</span>0.0078 (11)</td> 1329<td class="tabledata">0.0150 (11)</td> 1330<td class="tabledata"><span style="font-family:Times">?</span>0.0013 (10)</td> 1331</tr> 1332 1333<tr> 1334<td class="tabledata">C11</td> 1335<td class="tabledata">0.0602 (15)</td> 1336<td class="tabledata">0.0419 (14)</td> 1337<td class="tabledata">0.0678 (16)</td> 1338<td class="tabledata"><span style="font-family:Times">?</span>0.0027 (12)</td> 1339<td class="tabledata">0.0170 (13)</td> 1340<td class="tabledata">0.0062 (12)</td> 1341</tr> 1342 1343<tr> 1344<td class="tabledata">C12</td> 1345<td class="tabledata">0.0559 (14)</td> 1346<td class="tabledata">0.0524 (15)</td> 1347<td class="tabledata">0.0562 (14)</td> 1348<td class="tabledata"><span style="font-family:Times">?</span>0.0005 (11)</td> 1349<td class="tabledata">0.0154 (12)</td> 1350<td class="tabledata">0.0185 (12)</td> 1351</tr> 1352 1353<tr> 1354<td class="tabledata">C13</td> 1355<td class="tabledata">0.0673 (16)</td> 1356<td class="tabledata">0.0719 (19)</td> 1357<td class="tabledata">0.0535 (15)</td> 1358<td class="tabledata">0.0011 (14)</td> 1359<td class="tabledata">0.0163 (13)</td> 1360<td class="tabledata"><span style="font-family:Times">?</span>0.0162 (14)</td> 1361</tr> 1362 1363<tr> 1364<td class="tabledata">C14</td> 1365<td class="tabledata">0.079 (5)</td> 1366<td class="tabledata">0.065 (4)</td> 1367<td class="tabledata">0.041 (3)</td> 1368<td class="tabledata">0.019 (3)</td> 1369<td class="tabledata">0.013 (3)</td> 1370<td class="tabledata">0.008 (3)</td> 1371</tr> 1372 1373<tr> 1374<td class="tabledata">C15</td> 1375<td class="tabledata">0.101 (5)</td> 1376<td class="tabledata">0.110 (5)</td> 1377<td class="tabledata">0.047 (3)</td> 1378<td class="tabledata"><span style="font-family:Times">?</span>0.012 (4)</td> 1379<td class="tabledata">0.010 (3)</td> 1380<td class="tabledata">0.005 (3)</td> 1381</tr> 1382 1383<tr> 1384<td class="tabledata">C16</td> 1385<td class="tabledata">0.141 (7)</td> 1386<td class="tabledata">0.175 (8)</td> 1387<td class="tabledata">0.118 (6)</td> 1388<td class="tabledata"><span style="font-family:Times">?</span>0.013 (6)</td> 1389<td class="tabledata"><span style="font-family:Times">?</span>0.023 (5)</td> 1390<td class="tabledata">0.032 (5)</td> 1391</tr> 1392 1393<tr> 1394<td class="tabledata">C14'</td> 1395<td class="tabledata">0.096 (11)</td> 1396<td class="tabledata">0.095 (8)</td> 1397<td class="tabledata">0.037 (5)</td> 1398<td class="tabledata">0.030 (6)</td> 1399<td class="tabledata">0.014 (6)</td> 1400<td class="tabledata">0.017 (5)</td> 1401</tr> 1402 1403<tr> 1404<td class="tabledata">C15'</td> 1405<td class="tabledata">0.074 (8)</td> 1406<td class="tabledata">0.147 (12)</td> 1407<td class="tabledata">0.077 (7)</td> 1408<td class="tabledata"><span style="font-family:Times">?</span>0.010 (7)</td> 1409<td class="tabledata">0.005 (6)</td> 1410<td class="tabledata"><span style="font-family:Times">?</span>0.006 (7)</td> 1411</tr> 1412 1413<tr> 1414<td class="tabledata">C16'</td> 1415<td class="tabledata">0.137 (8)</td> 1416<td class="tabledata">0.130 (8)</td> 1417<td class="tabledata">0.089 (6)</td> 1418<td class="tabledata"><span style="font-family:Times">?</span>0.019 (6)</td> 1419<td class="tabledata">0.037 (6)</td> 1420<td class="tabledata">0.030 (6)</td> 1421</tr> 1422 1423<tr> 1424<td class="tabledata">C17</td> 1425<td class="tabledata">0.0504 (13)</td> 1426<td class="tabledata">0.0694 (18)</td> 1427<td class="tabledata">0.0454 (13)</td> 1428<td class="tabledata">0.0088 (12)</td> 1429<td class="tabledata">0.0080 (11)</td> 1430<td class="tabledata">0.0162 (12)</td> 1431</tr> 1432 1433<tr> 1434<td class="tabledata">C18</td> 1435<td class="tabledata">0.0373 (11)</td> 1436<td class="tabledata">0.0619 (16)</td> 1437<td class="tabledata">0.0397 (12)</td> 1438<td class="tabledata">0.0052 (11)</td> 1439<td class="tabledata">0.0017 (10)</td> 1440<td class="tabledata">0.0068 (11)</td> 1441</tr> 1442 1443<tr> 1444<td class="tabledata">C19</td> 1445<td class="tabledata">0.0527 (13)</td> 1446<td class="tabledata">0.0534 (15)</td> 1447<td class="tabledata">0.0484 (13)</td> 1448<td class="tabledata">0.0044 (11)</td> 1449<td class="tabledata">0.0151 (11)</td> 1450<td class="tabledata"><span style="font-family:Times">?</span>0.0039 (11)</td> 1451</tr> 1452 1453<tr> 1454<td class="tabledata">C20</td> 1455<td class="tabledata">0.0549 (14)</td> 1456<td class="tabledata">0.0576 (17)</td> 1457<td class="tabledata">0.0543 (14)</td> 1458<td class="tabledata">0.0015 (12)</td> 1459<td class="tabledata">0.0208 (12)</td> 1460<td class="tabledata">0.0027 (12)</td> 1461</tr> 1462 1463<tr> 1464<td class="tabledata">C21</td> 1465<td class="tabledata">0.0570 (14)</td> 1466<td class="tabledata">0.0509 (15)</td> 1467<td class="tabledata">0.0690 (17)</td> 1468<td class="tabledata"><span style="font-family:Times">?</span>0.0023 (12)</td> 1469<td class="tabledata">0.0125 (13)</td> 1470<td class="tabledata">0.0031 (13)</td> 1471</tr> 1472 1473<tr> 1474<td class="tabledata">C22</td> 1475<td class="tabledata">0.0655 (16)</td> 1476<td class="tabledata">0.0589 (18)</td> 1477<td class="tabledata">0.0679 (17)</td> 1478<td class="tabledata">0.0055 (14)</td> 1479<td class="tabledata">0.0138 (14)</td> 1480<td class="tabledata"><span style="font-family:Times">?</span>0.0143 (14)</td> 1481</tr> 1482 1483<tr> 1484<td class="tabledata">C23</td> 1485<td class="tabledata">0.0510 (14)</td> 1486<td class="tabledat…
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