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  33<h1 class="suptitle">supplementary materials</h1>
  34
  35<br/>
  36<div class="buttonlinks"><a href="./index.html" target="_parent"><img src="../../../../../graphics/htmlborder.gif" alt="HTML version" align="top" border="0"/></a><a href="./at2501.pdf"><img src="../../../../../graphics/pdfborder.gif" alt="pdf version" align="top" border="0"/></a><a href="http://scripts.iucr.org/cgi-bin/sendcif?at2501sup1"><img src="../../../../../graphics/cifborder.gif" alt="cif file" align="top" border="0"/></a><a href="http://scripts.iucr.org/cgi-bin/sendcif?at2501sup1&amp;Qmime=cif">
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  39
  40<p class="scheme"><img src="./at2501contents.gif" alt="at2501 scheme"/></p>
  41
  42<div class="bibline">
  43<p><i>Acta Cryst.</i> (2008). 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&amp;author_name=Cao,%20M.-H.">
  51M.-H. Cao</a>, <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&amp;author_name=Zhu,%20J.">
  52J. Zhu</a> and <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&amp;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&gt; 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&gt; 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> &lt;
 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&gt; 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&gt; 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> &gt; <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. (&lt;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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