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1<?xml version="1.0" encoding="UTF-8"?> 2<html cmlx:fileId="C:\Users\pm286\workspace\crystaleyeTestData\html\4\6\3\4630266e-8fea-4d71-a2c6-ba1256c7825f\suppText.html" xmlns:cmlx="http://www.xml-cml.org/schema/cmlx"> 3<head> 4<meta name="generator" content="HTML Tidy, see www.w3.org"/> 5<title>(IUCr) Crystallography Journals Online - supplementary 6material</title> 7<meta name="copyright" content="� International Union of Crystallography 2008"/> 8<style type="text/css"> 9 10 <!--/* <![CDATA[ */ 11 a {color:#000066; text-decoration: none;} 12 a:hover {color:#000000; text-decoration: underline;} 13 .bluetable {border: 2px solid #99ccff;} 14 .openurllink {position: absolute; right: 1.0em;} 15 h1, h2, h3 {margin-top: 0em; margin-bottom: 0.5em;padding: 0em;} 16 /* ]]> */--> 17</style> 18 19<script language="JavaScript" src="http://journals.iucr.org/javascript/scripts.js" type="text/javascript"> 20</script> 21 22<script src="http://www.google-analytics.com/urchin.js" type="text/javascript"> 23</script> 24 25<script type="text/javascript"> 26_uacct = "UA-187984-3"; 27urchinTracker(); 28</script> 29 30<link href="../../../../../styles/publcif.css" rel="stylesheet" type="text/css"/> 31</head> 32<body bgcolor="#FFFFFF" text="#000000"> 33<a id="top" name="top"/> 34<h1 class="suptitle">supplementary materials</h1> 35 36<br/> 37<div class="buttonlinks"><a href="./index.html" target="_parent"><img src="../../../../../graphics/htmlborder.gif" alt="HTML version" align="top" border="0"/></a><a href="./at2651.pdf"><img src="../../../../../graphics/pdfborder.gif" alt="pdf version" align="top" border="0"/></a><a href="http://scripts.iucr.org/cgi-bin/sendcif?at2651sup1"><img src="../../../../../graphics/cifborder.gif" alt="cif file" align="top" border="0"/></a><a href="http://scripts.iucr.org/cgi-bin/sendcif?at2651sup1&Qmime=cif"> 38<img src="../../../../../graphics/3dviewborder.gif" alt="3d view" align="top" border="0"/></a><a href="./at2651Isup2.hkl"><img src="../../../../../graphics/structurefactorsborder.gif" alt="structure factors" align="top" border="0"/></a><a href="./at2651sup0.html"><img src="../../../../../graphics/supplementarymaterialsborder.gif" alt="supplementary materials" align="top" border="0"/></a><a href="./at2651checkcif.html"><img src="../../../../../graphics/checkcifborder.gif" alt="CIF check report" align="top" border="0"/></a><a href="http://scripts.iucr.org/cgi-bin/similar?wordList=methylphenyl%20or%20iminiomethyl%20or%20phenolato%20or%20thiocyanato%20or%20zinc&from=at2651"> 39<img src="../../../../../graphics/similarpapersborder.gif" alt="similar papers" align="top" border="0"/></a>�<a href="../../../../../../services/openaccess.html"><img src="../../../../../../logos/free.gif" alt="Open access" align="top" border="0"/></a></div> 40 41<p class="scheme"><img src="./at2651contents.gif" alt="at2651 scheme"/></p> 42 43<div class="bibline"> 44<p><i>Acta Cryst.</i> (2008). E<b>64</b>, 45m1495����[ <a title="Open URL link" href="http://dx.doi.org/10.1107/S1600536808035368">doi:10.1107/S1600536808035368</a> 46]</p> 47</div> 48 49<h3>Bis{2-methoxy-6-[(4-methylphenyl)iminiomethyl]phenolato-<img alt="[kappa]" border="0" src="/logos/entities/kappa_rmgif.gif"/><span class="it"><i>O</i></span><span class="sup"><sup>1</sup></span>}bis(thiocyanato-<img alt="[kappa]" border="0" src="/logos/entities/kappa_rmgif.gif"/><span class="it"><i>N</i></span>)zinc(II)</h3> 50 51<h3><a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Li,%20H.-Q."> 52H.-Q. Li</a>, <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Xian,%20H.-D."> 53H.-D. Xian</a>, <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Liu,%20J.-F."> 54J.-F. Liu</a> and <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Zhao,%20G.-L."> 55G.-L. Zhao</a></h3> 56 57<div class="abstract"><a id="abstract" name="abstract"/> 58 59<div class="heading2">Abstract <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 60</div> 61 62<!-- endheading2div --> 63<p>The Schiff base 2-[(4-methylphenyl)iminomethyl]-6-methoxyphenol 64(H<span class="it"><i>L</i></span>) forms a complex with a Zn<span class="sup"><sup>2+</sup></span> atom and two independent 65thiocyanate ions, [Zn(NCS)<span class="inf"><sub>2</sub></span>(C<span class="inf"><sub>15</sub></span>H<span class="inf"><sub>15</sub></span>NO<span class="inf"><sub>2</sub></span>)<span class="inf"><sub>2</sub></span>], in which two phenolate O atoms 66the two independent Schiff base ligands are coordinated to thee 67Zn<span class="sup"><sup>2+</sup></span> atom. The protonated imine 68N atoms are involved in an intramolecular hydrogen bond with the 69phenoxide group. The Zn atom is also coordinated by two N atoms of 70two thiocyanate ligands. The coordination environment of the Zn 71atom is distorted-tetrahedral.</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">Bis{6-methoxy-6-[(4-methylphenyl)iminiomethyl]phenolato- 90<span style="font-family:Times">?</span><i>O</i><sup>1</sup>}bis(thiocyanato-<span style="font-family:Times">?</span><i>N</i>)zinc(II)</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="publreferences"><a title="References" href="#publreferences">References</a></li> 118</ul> 119</div> 120 121<!-- endcontentslistdiv --> 122<div class="comment"><a id="comment" name="comment"/> 123 124<div class="heading2">Comment <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 125</div> 126 127<!-- endheading2div --> 128<p>The Schiff base ligands, the products of condensation of 129<i>o</i>-vanillin with amines, viewed several different kind of 130coordination modes with the centre metals (Sen <i>et al.</i>, 1312006). And, in early articles, researchers have reported three 132coordination modes of the Schiff base ligand, HL, derived from 133condensation of <i>o</i>-vanillin and <i>p</i>-toluidine. The first 134mode was that two O atoms of the Schiff base ligand were 135coordinated to the centre metal (Zhou & Zhao, 2007; Yu <i>et 136al.</i>, 2007; Zhao <i>et al.</i>, 2007). The second one was that 137the ligands coordinate to centre metal through hydroxy O atom and 138the azomethine N atom (Iyere <i>et al.</i>, 2004). The third one 139was that the centre metal only coordinated to the phenol O atoms 140(Zhou <i>et al.</i>, 2007). In fact, there was still another 141coordination mode of the Schiff base ligand. It was that all the 142three donor atoms were coordinated to centre metal, but without its 143X-ray crystallographic conformations (Maurya <i>et al.</i>, 1994). 144Here we decribe the synthesis and crystal structure of a new 145zinc(II) complex (Fig. 1), Zn(HL)<sub>2</sub>(NCS)<sub>2</sub>, 146involing the Schiff base HL, with the third coordination mode.</p> 147 148<p>As shown in Fig. 1, the tridentate ligands coordinate to the Zn 149atom through two phenolic hydroxy O atoms and two isothiocyanate N 150atoms, forming a distorted tetrahedral geometry around the metal 151ion. The isothiocyanate group was not used as a bridged ligand, in 152the same way to the other Zn complexes with the ligand of 153isothiocyanate (Li, 2007; Zhang & Wang, 2007; Groeneveld <i>et 154al.</i>, 1982).</p> 155</div> 156 157<!-- endcommentdiv --> 158<div class="relatedliterature"><a id="relatedliterature" name="relatedliterature"/> 159 160<div class="heading2">Related literature <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 161</div> 162 163<!-- endheading2div --> 164<p>For related literature, see: Groeneveld <i>et al.</i> (1982); 165Iyere <i>et al.</i> (2004); Li (2007); Maurya <i>et al.</i> (1994); 166Sen <i>et al.</i> (2006); Yu <i>et al.</i> (2007); Zhang & Wang 167(2007); Zhao <i>et al.</i> (2007); Zhou & Zhao (2007); Zhou 168<i>et al.</i> (2007). It would be much more useful to readers if 169the "Related literature" section had some kind of simple 170sub-division, so that, instead of just "For related 171literature, see���" it said, for example, 172"For general background, see���. For related 173structures, see���.? etc. Please revise this section 174as indicated.</p> 175</div> 176 177<!-- endrelatedliteraturediv --> 178<div class="experimental"><a id="experimental" name="experimental"/> 179 180<div class="heading2">Experimental <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 181</div> 182 183<!-- endheading2div --> 184<p>The Schiff base was prepared by refluxing <i>o</i>-vanillin (10 185mmol, 1.5251 g) and <i>p</i>-toluidine (10 mmol, 1.0700 g) in 186ethanol. The colour of the mixture changed from light yellow to 187orange. Then, for the preparation of the complex, the zinc sulfate 188heptahydrate (1 mmol, 0.2876 g) and potassium thiocyanate (0.1945 189g, 2 mmol) in methanol (10 ml) was added to a methanol (30 ml) 190solution of the Schiff base ligand (2 mmol, 0.4826 g). Red crystals 191were obtained after 10 days.</p> 192</div> 193 194<!-- endexperimentaldiv --> 195<div class="refinement"><a id="refinement" name="refinement"/> 196 197<div class="heading2">Refinement <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 198</div> 199 200<!-- endheading2div --> 201<p>The H atoms bonded to C and N atoms were positioned 202geometrically and refined using a riding model [aromatic C-H = 0.93 203�, methylic C-H = 0.96 �, N-H = 0.86 �, 204<i>U</i><sub>iso</sub>(H) = 1.2 or 2051.5<i>U</i><sub>eq</sub>(C,N)].</p> 206</div> 207 208<!-- endrefinementdiv --> 209<div class="computingdetails"><a id="computingdetails" name="computingdetails"/> 210 211<div class="heading2">Computing details <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 212</div> 213 214<!-- endheading2div --> 215<p>Data collection: <i>APEX2</i> (Bruker, 2004); cell refinement: 216<i>SAINT</i> (Bruker, 2004); data reduction: <i>SAINT</i> (Bruker, 2172004); program(s) used to solve structure: <i>SHELXTL</i> 218(Sheldrick, 2008); program(s) used to refine structure: 219<i>SHELXTL</i> (Sheldrick, 2008); molecular graphics: 220<i>SHELXTL</i> (Sheldrick, 2008); software used to prepare material 221for publication: <i>SHELXTL</i> (Sheldrick, 2008).</p> 222</div> 223 224<!-- endcomputingdetailsdiv --> 225<div class="schemes"><a href="./at2651scheme1.gif"/></div> 226 227<!-- endschemesdiv --> 228<div class="figures"><a id="figures" name="figures"/> 229 230<div class="heading2">Figures <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 231</div> 232 233<!-- endheading2div --> 234<table style="table-layout:fixed" width="100%" class="nodecs"> 235<colgroup span="2"> 236<col width="110"/> 237<col/></colgroup> 238 239<tr> 240<td class="nodecs" align="center" width="110"><a href="./at2651fig1.html"><img width="100" src="./at2651fig1thm.gif" alt="[Figure 1]" align="middle"/></a> </td> 241<td class="nodecs" valign="middle">Fig. 1. The molecular structure 242of the title complex, showing the atom-labelling scheme. 243Displacement ellipsoids are drawn at the 30% probability level. 244</td> 245</tr> 246</table> 247</div> 248 249<!-- endfiguresdiv --> 250<div class="datablock1"> 251<div class="heading2"><a id="chemicalname1" name="chemicalname1"/>Bis{6-methoxy-6-[(4-methylphenyl)iminiomethyl]phenolato- 252<span style="font-family:Times">?</span><i>O</i><sup>1</sup>}bis(thiocyanato-<span style="font-family:Times">?</span><i>N</i>)zinc(II) <span class="toplink"><a class="buttons" href="#top">top</a></span> 253<!-- endtoplinkspan --> 254</div> 255 256<!-- endheading2div --> 257<div class="tablewrapcrystaldatalong"><a id="crystaldata1" name="crystaldata1"/><span class="heading3">Crystal data</span> 258<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 259<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 260<colgroup span="2"> 261<col width="50%"/> 262<col width="50%"/></colgroup> 263 264<tr> 265<td width="50%" class="tabledata"> 266[Zn(NCS)<sub>2</sub>(C<sub>15</sub>H<sub>15</sub>NO<sub>2</sub>)<sub> 2672</sub>]</td> 268<td width="50%" class="tabledata"><i>Z</i> = 2</td> 269</tr> 270 271<tr> 272<td width="50%" class="tabledata"><i>M</i><i><sub>r</sub></i> = 273664.13</td> 274<td width="50%" class="tabledata"><i>F</i><sub>000</sub> = 688</td> 275</tr> 276 277<tr> 278<td width="50%" class="tabledata">Triclinic, <i>P</i><span style="text-decoration:overline">1</span></td> 279<td width="50%" class="tabledata"><i>D</i><sub>x</sub> = 1.370 Mg 280m<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 281</tr> 282 283<tr> 284<td width="50%" class="tabledata">Hall symbol: -P 1</td> 285<td width="50%" class="tabledata">Mo <i>K</i><span style="font-family:Times">?</span> radiation<br/> 286<span style="font-family:Times">?</span> = 0.71073 �</td> 287</tr> 288 289<tr> 290<td width="50%" class="tabledata"><i>a</i> = 9.3830 (2) �</td> 291<td width="50%" class="tabledata">Cell parameters from 5295 292reflections</td> 293</tr> 294 295<tr> 296<td width="50%" class="tabledata"><i>b</i> = 11.7146 (2) 297�</td> 298<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 1.4-25.0�</td> 299</tr> 300 301<tr> 302<td width="50%" class="tabledata"><i>c</i> = 15.7328 (3) 303�</td> 304<td width="50%" class="tabledata">� = 0.93 mm<span style="font-family:Times"><sup>?</sup></span><sup>1</sup></td> 305</tr> 306 307<tr> 308<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 107.7830 (10)�</td> 309<td width="50%" class="tabledata"><i>T</i> = 296 (2) K</td> 310</tr> 311 312<tr> 313<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 99.4450 (10)�</td> 314<td width="50%" class="tabledata">Block, red</td> 315</tr> 316 317<tr> 318<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 94.1730 (10)�</td> 319<td width="50%" class="tabledata">0.23 � 0.18 � 0.07 320mm</td> 321</tr> 322 323<tr> 324<td width="50%" class="tabledata"><i>V</i> = 1610.41 (5) 325�<sup>3</sup></td> 326<td width="50%" class="tabledata"/> 327</tr> 328</table> 329 330<!-- endtabledatatable --> 331</div> 332 333<!-- endtablewrapcrystaldatalongdiv --> 334<div class="tablewrapdatacollectionlong"><a id="datacollection1" name="datacollection1"/><span class="heading3">Data 335collection</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 336<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 337<colgroup span="2"> 338<col width="50%"/> 339<col width="50%"/></colgroup> 340 341<tr> 342<td width="50%" class="tabledata">Bruker APEXII area-detector<br/> 343diffractometer</td> 344<td width="50%" class="tabledata">5672 independent reflections</td> 345</tr> 346 347<tr> 348<td width="50%" class="tabledata">Radiation source: fine-focus 349sealed tube</td> 350<td width="50%" class="tabledata">3679 reflections with <i>I</i> 351> 2<span style="font-family:Times">?</span>(<i>I</i>)</td> 352</tr> 353 354<tr> 355<td width="50%" class="tabledata">Monochromator: graphite</td> 356<td width="50%" class="tabledata"><i>R</i><sub>int</sub> = 3570.034</td> 358</tr> 359 360<tr> 361<td width="50%" class="tabledata"><i>T</i> = 296(2) K</td> 362<td width="50%" class="tabledata"><span style="font-family:Times">?</span><sub>max</sub> = 36325.0�</td> 364</tr> 365 366<tr> 367<td width="50%" class="tabledata"><span style="font-family:Times">?</span> scans</td> 368<td width="50%" class="tabledata"><span style="font-family:Times">?</span><sub>min</sub> = 3691.4�</td> 370</tr> 371 372<tr> 373<td width="50%" class="tabledata">Absorption correction: 374multi-scan<br/> 375(SADABS; Sheldrick, 1996)</td> 376<td width="50%" class="tabledata"><i>h</i> = <span style="font-family:Times">?</span>11?11</td> 377</tr> 378 379<tr> 380<td width="50%" class="tabledata"><i>T</i><sub>min</sub> = 0.817, 381<i>T</i><sub>max</sub> = 0.940</td> 382<td width="50%" class="tabledata"><i>k</i> = <span style="font-family:Times">?</span>13?13</td> 383</tr> 384 385<tr> 386<td width="50%" class="tabledata">20903 measured reflections</td> 387<td width="50%" class="tabledata"><i>l</i> = <span style="font-family:Times">?</span>16?18</td> 388</tr> 389</table> 390 391<!-- endtabledatatable --> 392</div> 393 394<!-- endtablewrapdatacollectionlongdiv --> 395<div class="tablewraprefinementdatalong"><a id="refinementdata1" name="refinementdata1"/><span class="heading3">Refinement</span> 396<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 397<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 398<colgroup span="2"> 399<col width="50%"/> 400<col width="50%"/></colgroup> 401 402<tr> 403<td width="50%" class="tabledata">Refinement on 404<i>F</i><sup>2</sup></td> 405<td width="50%" class="tabledata">Secondary atom site location: 406difference Fourier map</td> 407</tr> 408 409<tr> 410<td width="50%" class="tabledata">Least-squares matrix: full</td> 411<td width="50%" class="tabledata">Hydrogen site location: inferred 412from neighbouring sites</td> 413</tr> 414 415<tr> 416<td width="50%" class="tabledata"><i>R</i>[<i>F</i><sup>2</sup> 417> 2<span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>)] = 4180.040</td> 419<td width="50%" class="tabledata">H-atom parameters 420constrained</td> 421</tr> 422 423<tr> 424<td width="50%" class="tabledata"><i>wR</i>(<i>F</i><sup>2</sup>) = 4250.106</td> 426<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> 4272</sup>) + (0.0521<i>P</i>)<sup>2</sup>]<br/> 428where <i>P</i> = (<i>F</i><sub>o</sub><sup>2</sup> + 4292<i>F</i><sub>c</sub><sup>2</sup>)/3</td> 430</tr> 431 432<tr> 433<td width="50%" class="tabledata"><i>S</i> = 1.02</td> 434<td width="50%" class="tabledata">(?/<span style="font-family:Times">?</span>)<sub>max</sub> < 4350.001</td> 436</tr> 437 438<tr> 439<td width="50%" class="tabledata">5672 reflections</td> 440<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>max</sub> = 0.30 e 441�<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 442</tr> 443 444<tr> 445<td width="50%" class="tabledata">388 parameters</td> 446<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>min</sub> = <span style="font-family:Times">?</span>0.24 e �<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 447</tr> 448 449<tr> 450<td width="50%" class="tabledata">Primary atom site location: 451structure-invariant direct methods</td> 452<td width="50%" class="tabledata">Extinction correction: none</td> 453</tr> 454</table> 455 456<!-- endtabledatatable --> 457</div> 458 459<!-- endtablewraprefinementdatalongdiv --> 460<div class="tablewrapcrystaldatashort"><a id="crystaldata1" name="crystaldata1"/><span class="heading3">Crystal data</span> 461<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 462<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 463<colgroup span="2"> 464<col width="50%"/> 465<col width="50%"/></colgroup> 466 467<tr> 468<td width="50%" class="tabledata"> 469[Zn(NCS)<sub>2</sub>(C<sub>15</sub>H<sub>15</sub>NO<sub>2</sub>)<sub> 4702</sub>]</td> 471<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 94.1730 (10)�</td> 472</tr> 473 474<tr> 475<td width="50%" class="tabledata"><i>M</i><i><sub>r</sub></i> = 476664.13</td> 477<td width="50%" class="tabledata"><i>V</i> = 1610.41 (5) 478�<sup>3</sup></td> 479</tr> 480 481<tr> 482<td width="50%" class="tabledata">Triclinic, <i>P</i><span style="text-decoration:overline">1</span></td> 483<td width="50%" class="tabledata"><i>Z</i> = 2</td> 484</tr> 485 486<tr> 487<td width="50%" class="tabledata"><i>a</i> = 9.3830 (2) �</td> 488<td width="50%" class="tabledata">Mo <i>K</i><span style="font-family:Times">?</span></td> 489</tr> 490 491<tr> 492<td width="50%" class="tabledata"><i>b</i> = 11.7146 (2) 493�</td> 494<td width="50%" class="tabledata">� = 0.93 mm<span style="font-family:Times"><sup>?</sup></span><sup>1</sup></td> 495</tr> 496 497<tr> 498<td width="50%" class="tabledata"><i>c</i> = 15.7328 (3) 499�</td> 500<td width="50%" class="tabledata"><i>T</i> = 296 (2) K</td> 501</tr> 502 503<tr> 504<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 107.7830 (10)�</td> 505<td width="50%" class="tabledata">0.23 � 0.18 � 0.07 506mm</td> 507</tr> 508 509<tr> 510<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 99.4450 (10)�</td> 511<td width="50%" class="tabledata"/> 512</tr> 513</table> 514 515<!-- endtabledatatable --> 516</div> 517 518<!-- endtablewrapcrystaldatashortdiv --> 519<div class="tablewrapdatacollectionshort"><a id="datacollection1" name="datacollection1"/><span class="heading3">Data 520collection</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 521<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 522<colgroup span="2"> 523<col width="50%"/> 524<col width="50%"/></colgroup> 525 526<tr> 527<td width="50%" class="tabledata">Bruker APEXII area-detector<br/> 528diffractometer</td> 529<td width="50%" class="tabledata">5672 independent reflections</td> 530</tr> 531 532<tr> 533<td width="50%" class="tabledata">Absorption correction: 534multi-scan<br/> 535(SADABS; Sheldrick, 1996)</td> 536<td width="50%" class="tabledata">3679 reflections with <i>I</i> 537> 2<span style="font-family:Times">?</span>(<i>I</i>)</td> 538</tr> 539 540<tr> 541<td width="50%" class="tabledata"><i>T</i><sub>min</sub> = 0.817, 542<i>T</i><sub>max</sub> = 0.940</td> 543<td width="50%" class="tabledata"><i>R</i><sub>int</sub> = 5440.034</td> 545</tr> 546 547<tr> 548<td width="50%" class="tabledata">20903 measured reflections</td> 549<td width="50%" class="tabledata"/> 550</tr> 551</table> 552 553<!-- endtabledatatable --> 554</div> 555 556<!-- endtablewrapdatacollectionshortdiv --> 557<div class="tablewraprefinementdatashort"><a id="refinementdata1" name="refinementdata1"/><span class="heading3">Refinement</span> 558<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 559<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 560<colgroup span="2"> 561<col width="50%"/> 562<col width="50%"/></colgroup> 563 564<tr> 565<td width="50%" class="tabledata"><i>R</i>[<i>F</i><sup>2</sup> 566> 2<span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>)] = 5670.040</td> 568<td width="50%" class="tabledata">388 parameters</td> 569</tr> 570 571<tr> 572<td width="50%" class="tabledata"><i>wR</i>(<i>F</i><sup>2</sup>) = 5730.106</td> 574<td width="50%" class="tabledata">H-atom parameters 575constrained</td> 576</tr> 577 578<tr> 579<td width="50%" class="tabledata"><i>S</i> = 1.02</td> 580<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>max</sub> = 0.30 e 581�<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 582</tr> 583 584<tr> 585<td width="50%" class="tabledata">5672 reflections</td> 586<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>min</sub> = <span style="font-family:Times">?</span>0.24 e �<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 587</tr> 588</table> 589 590<!-- endtabledatatable --> 591</div> 592 593<!-- endtablewraprefinementdatashortdiv --> 594<div class="specialdetails"><a id="specialdetails1" name="specialdetails1"/><span class="heading3">Special 595details</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 596<table style="table-layout:fixed" width="100%" class="tabledata"> 597<tr> 598<td class="tabledata"> 599<p><b>Geometry</b>. All e.s.d.'s (except the e.s.d. in the 600dihedral angle between two l.s. planes) are estimated using the 601full covariance matrix. The cell e.s.d.'s are taken into 602account individually in the estimation of e.s.d.'s in 603distances, angles and torsion angles; correlations between 604e.s.d.'s in cell parameters are only used when they are defined 605by crystal symmetry. An approximate (isotropic) treatment of cell 606e.s.d.'s is used for estimating e.s.d.'s involving l.s. 607planes.</p> 608</td> 609</tr> 610 611<tr> 612<td class="tabledata"> 613<p><b>Refinement</b>. Refinement of <i>F</i><sup>2</sup> against 614ALL reflections. The weighted <i>R</i>-factor <i>wR</i> and 615goodness of fit <i>S</i> are based on <i>F</i><sup>2</sup>, 616conventional <i>R</i>-factors <i>R</i> are based on <i>F</i>, with 617<i>F</i> set to zero for negative <i>F</i><sup>2</sup>. The 618threshold expression of <i>F</i><sup>2</sup> > <span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>) is 619used only for calculating <i>R</i>-factors(gt) <i>etc</i>. and is 620not relevant to the choice of reflections for refinement. 621<i>R</i>-factors based on <i>F</i><sup>2</sup> are statistically 622about twice as large as those based on <i>F</i>, and <i>R</i>- 623factors based on ALL data will be even larger.</p> 624</td> 625</tr> 626</table> 627</div> 628 629<!-- endspecialdetailsdiv --> 630<div class="tablewrapcoords"><a id="fractionalatomiccoordinates1" name="fractionalatomiccoordinates1"/> <span class="heading3">Fractional atomic coordinates and isotropic or 631equivalent isotropic displacement parameters 632(�<sup>2</sup>)</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span> 633<!-- endtoplinkspan --> 634<table style="table-layout:fixed" width="100%" summary="" class="tabledata"> 635<tr> 636<td class="tabledata"/> 637<td class="tabledata"><i>x</i></td> 638<td class="tabledata"><i>y</i></td> 639<td class="tabledata"><i>z</i></td> 640<td class="tabledata"> 641<i>U</i><sub>iso</sub>*/<i>U</i><sub>eq</sub></td> 642<td class="tabledata"/> 643</tr> 644 645<tr> 646<td class="tabledata">Zn1</td> 647<td class="tabledata"><span style="font-family:Times">?</span>0.34621 (3)</td> 648<td class="tabledata"><span style="font-family:Times">?</span>0.06960 (3)</td> 649<td class="tabledata">0.25870 (2)</td> 650<td class="tabledata">0.06223 (15)</td> 651<td class="tabledata"/> 652</tr> 653 654<tr> 655<td class="tabledata">S1</td> 656<td class="tabledata"><span style="font-family:Times">?</span>0.56733 (13)</td> 657<td class="tabledata"><span style="font-family:Times">?</span>0.44672 (8)</td> 658<td class="tabledata">0.24413 (7)</td> 659<td class="tabledata">0.1062 (4)</td> 660<td class="tabledata"/> 661</tr> 662 663<tr> 664<td class="tabledata">O1</td> 665<td class="tabledata"><span style="font-family:Times">?</span>0.3477 (3)</td> 666<td class="tabledata">0.1704 (2)</td> 667<td class="tabledata">0.25578 (15)</td> 668<td class="tabledata">0.0886 (7)</td> 669<td class="tabledata"/> 670</tr> 671 672<tr> 673<td class="tabledata">N1</td> 674<td class="tabledata"><span style="font-family:Times">?</span>0.4233 (3)</td> 675<td class="tabledata"><span style="font-family:Times">?</span>0.2404 (3)</td> 676<td class="tabledata">0.2301 (2)</td> 677<td class="tabledata">0.0835 (8)</td> 678<td class="tabledata"/> 679</tr> 680 681<tr> 682<td class="tabledata">C1</td> 683<td class="tabledata"><span style="font-family:Times">?</span>1.0051 (5)</td> 684<td class="tabledata"><span style="font-family:Times">?</span>0.6559 (3)</td> 685<td class="tabledata"><span style="font-family:Times">?</span>0.1553 (2)</td> 686<td class="tabledata">0.1179 (15)</td> 687<td class="tabledata"/> 688</tr> 689 690<tr> 691<td class="tabledata">H1B</td> 692<td class="tabledata"><span style="font-family:Times">?</span>1.1012</td> 693<td class="tabledata"><span style="font-family:Times">?</span>0.6514</td> 694<td class="tabledata"><span style="font-family:Times">?</span>0.1852</td> 695<td class="tabledata">0.177*</td> 696<td class="tabledata"/> 697</tr> 698 699<tr> 700<td class="tabledata">H1C</td> 701<td class="tabledata"><span style="font-family:Times">?</span>1.0118</td> 702<td class="tabledata"><span style="font-family:Times">?</span>0.6975</td> 703<td class="tabledata"><span style="font-family:Times">?</span>0.1118</td> 704<td class="tabledata">0.177*</td> 705<td class="tabledata"/> 706</tr> 707 708<tr> 709<td class="tabledata">H1D</td> 710<td class="tabledata"><span style="font-family:Times">?</span>0.9522</td> 711<td class="tabledata"><span style="font-family:Times">?</span>0.6990</td> 712<td class="tabledata"><span style="font-family:Times">?</span>0.1996</td> 713<td class="tabledata">0.177*</td> 714<td class="tabledata"/> 715</tr> 716 717<tr> 718<td class="tabledata">S2</td> 719<td class="tabledata">0.05039 (9)</td> 720<td class="tabledata">0.03726 (9)</td> 721<td class="tabledata">0.14475 (6)</td> 722<td class="tabledata">0.0846 (3)</td> 723<td class="tabledata"/> 724</tr> 725 726<tr> 727<td class="tabledata">O2</td> 728<td class="tabledata"><span style="font-family:Times">?</span>0.5052 (2)</td> 729<td class="tabledata"><span style="font-family:Times">?</span>0.04420 (18)</td> 730<td class="tabledata">0.16903 (13)</td> 731<td class="tabledata">0.0691 (6)</td> 732<td class="tabledata"/> 733</tr> 734 735<tr> 736<td class="tabledata">N2</td> 737<td class="tabledata"><span style="font-family:Times">?</span>0.1629 (3)</td> 738<td class="tabledata"><span style="font-family:Times">?</span>0.0426 (3)</td> 739<td class="tabledata">0.22310 (19)</td> 740<td class="tabledata">0.0825 (8)</td> 741<td class="tabledata"/> 742</tr> 743 744<tr> 745<td class="tabledata">C2</td> 746<td class="tabledata"><span style="font-family:Times">?</span>0.9261 (5)</td> 747<td class="tabledata"><span style="font-family:Times">?</span>0.5293 (3)</td> 748<td class="tabledata"><span style="font-family:Times">?</span>0.1067 (2)</td> 749<td class="tabledata">0.0859 (11)</td> 750<td class="tabledata"/> 751</tr> 752 753<tr> 754<td class="tabledata">N3</td> 755<td class="tabledata"><span style="font-family:Times">?</span>0.7024 (2)</td> 756<td class="tabledata"><span style="font-family:Times">?</span>0.1806 (2)</td> 757<td class="tabledata">0.03326 (16)</td> 758<td class="tabledata">0.0646 (7)</td> 759<td class="tabledata"/> 760</tr> 761 762<tr> 763<td class="tabledata">H3A</td> 764<td class="tabledata"><span style="font-family:Times">?</span>0.6358</td> 765<td class="tabledata"><span style="font-family:Times">?</span>0.1743</td> 766<td class="tabledata">0.0797</td> 767<td class="tabledata">0.077*</td> 768<td class="tabledata"/> 769</tr> 770 771<tr> 772<td class="tabledata">O3</td> 773<td class="tabledata"><span style="font-family:Times">?</span>0.1914 (2)</td> 774<td class="tabledata"><span style="font-family:Times">?</span>0.1235 (2)</td> 775<td class="tabledata">0.39664 (15)</td> 776<td class="tabledata">0.0845 (7)</td> 777<td class="tabledata"/> 778</tr> 779 780<tr> 781<td class="tabledata">C3</td> 782<td class="tabledata"><span style="font-family:Times">?</span>0.7856 (5)</td> 783<td class="tabledata"><span style="font-family:Times">?</span>0.5117 (4)</td> 784<td class="tabledata"><span style="font-family:Times">?</span>0.0581 (3)</td> 785<td class="tabledata">0.0969 (12)</td> 786<td class="tabledata"/> 787</tr> 788 789<tr> 790<td class="tabledata">H3B</td> 791<td class="tabledata"><span style="font-family:Times">?</span>0.7386</td> 792<td class="tabledata"><span style="font-family:Times">?</span>0.5786</td> 793<td class="tabledata"><span style="font-family:Times">?</span>0.0571</td> 794<td class="tabledata">0.116*</td> 795<td class="tabledata"/> 796</tr> 797 798<tr> 799<td class="tabledata">O4</td> 800<td class="tabledata"><span style="font-family:Times">?</span>0.3720 (2)</td> 801<td class="tabledata">0.03332 (17)</td> 802<td class="tabledata">0.37738 (12)</td> 803<td class="tabledata">0.0650 (5)</td> 804<td class="tabledata"/> 805</tr> 806 807<tr> 808<td class="tabledata">N4</td> 809<td class="tabledata"><span style="font-family:Times">?</span>0.5101 (2)</td> 810<td class="tabledata">0.2110 (2)</td> 811<td class="tabledata">0.44824 (15)</td> 812<td class="tabledata">0.0573 (6)</td> 813<td class="tabledata"/> 814</tr> 815 816<tr> 817<td class="tabledata">H4A</td> 818<td class="tabledata"><span style="font-family:Times">?</span>0.4896</td> 819<td class="tabledata">0.1612</td> 820<td class="tabledata">0.4004</td> 821<td class="tabledata">0.069*</td> 822<td class="tabledata"/> 823</tr> 824 825<tr> 826<td class="tabledata">C4</td> 827<td class="tabledata"><span style="font-family:Times">?</span>0.7124 (4)</td> 828<td class="tabledata"><span style="font-family:Times">?</span>0.3966 (3)</td> 829<td class="tabledata"><span style="font-family:Times">?</span>0.0106 (2)</td> 830<td class="tabledata">0.0852 (10)</td> 831<td class="tabledata"/> 832</tr> 833 834<tr> 835<td class="tabledata">H4B</td> 836<td class="tabledata"><span style="font-family:Times">?</span>0.6186</td> 837<td class="tabledata"><span style="font-family:Times">?</span>0.3867</td> 838<td class="tabledata">0.0232</td> 839<td class="tabledata">0.102*</td> 840<td class="tabledata"/> 841</tr> 842 843<tr> 844<td class="tabledata">C5</td> 845<td class="tabledata"><span style="font-family:Times">?</span>0.7802 (3)</td> 846<td class="tabledata"><span style="font-family:Times">?</span>0.2975 (3)</td> 847<td class="tabledata"><span style="font-family:Times">?</span>0.0143 (2)</td> 848<td class="tabledata">0.0650 (8)</td> 849<td class="tabledata"/> 850</tr> 851 852<tr> 853<td class="tabledata">C6</td> 854<td class="tabledata"><span style="font-family:Times">?</span>0.9205 (4)</td> 855<td class="tabledata"><span style="font-family:Times">?</span>0.3138 (3)</td> 856<td class="tabledata"><span style="font-family:Times">?</span>0.0617 (2)</td> 857<td class="tabledata">0.0771 (9)</td> 858<td class="tabledata"/> 859</tr> 860 861<tr> 862<td class="tabledata">H6A</td> 863<td class="tabledata"><span style="font-family:Times">?</span>0.9679</td> 864<td class="tabledata"><span style="font-family:Times">?</span>0.2472</td> 865<td class="tabledata"><span style="font-family:Times">?</span>0.0631</td> 866<td class="tabledata">0.093*</td> 867<td class="tabledata"/> 868</tr> 869 870<tr> 871<td class="tabledata">C7</td> 872<td class="tabledata"><span style="font-family:Times">?</span>0.9912 (4)</td> 873<td class="tabledata"><span style="font-family:Times">?</span>0.4295 (4)</td> 874<td class="tabledata"><span style="font-family:Times">?</span>0.1073 (2)</td> 875<td class="tabledata">0.0851 (10)</td> 876<td class="tabledata"/> 877</tr> 878 879<tr> 880<td class="tabledata">H7A</td> 881<td class="tabledata"><span style="font-family:Times">?</span>1.0862</td> 882<td class="tabledata"><span style="font-family:Times">?</span>0.4393</td> 883<td class="tabledata"><span style="font-family:Times">?</span>0.1395</td> 884<td class="tabledata">0.102*</td> 885<td class="tabledata"/> 886</tr> 887 888<tr> 889<td class="tabledata">C8</td> 890<td class="tabledata"><span style="font-family:Times">?</span>0.7217 (3)</td> 891<td class="tabledata"><span style="font-family:Times">?</span>0.0826 (3)</td> 892<td class="tabledata">0.0137 (2)</td> 893<td class="tabledata">0.0647 (8)</td> 894<td class="tabledata"/> 895</tr> 896 897<tr> 898<td class="tabledata">H8A</td> 899<td class="tabledata"><span style="font-family:Times">?</span>0.7944</td> 900<td class="tabledata"><span style="font-family:Times">?</span>0.0879</td> 901<td class="tabledata"><span style="font-family:Times">?</span>0.0357</td> 902<td class="tabledata">0.078*</td> 903<td class="tabledata"/> 904</tr> 905 906<tr> 907<td class="tabledata">C9</td> 908<td class="tabledata"><span style="font-family:Times">?</span>0.6408 (3)</td> 909<td class="tabledata">0.0308 (3)</td> 910<td class="tabledata">0.06162 (19)</td> 911<td class="tabledata">0.0576 (8)</td> 912<td class="tabledata"/> 913</tr> 914 915<tr> 916<td class="tabledata">C10</td> 917<td class="tabledata"><span style="font-family:Times">?</span>0.5307 (3)</td> 918<td class="tabledata">0.0460 (3)</td> 919<td class="tabledata">0.13859 (19)</td> 920<td class="tabledata">0.0560 (7)</td> 921<td class="tabledata"/> 922</tr> 923 924<tr> 925<td class="tabledata">C11</td> 926<td class="tabledata"><span style="font-family:Times">?</span>0.4505 (3)</td> 927<td class="tabledata">0.1624 (3)</td> 928<td class="tabledata">0.18105 (19)</td> 929<td class="tabledata">0.0637 (8)</td> 930<td class="tabledata"/> 931</tr> 932 933<tr> 934<td class="tabledata">C12</td> 935<td class="tabledata"><span style="font-family:Times">?</span>0.4809 (4)</td> 936<td class="tabledata">0.2564 (3)</td> 937<td class="tabledata">0.1503 (2)</td> 938<td class="tabledata">0.0739 (9)</td> 939<td class="tabledata"/> 940</tr> 941 942<tr> 943<td class="tabledata">H12A</td> 944<td class="tabledata"><span style="font-family:Times">?</span>0.4268</td> 945<td class="tabledata">0.3322</td> 946<td class="tabledata">0.1794</td> 947<td class="tabledata">0.089*</td> 948<td class="tabledata"/> 949</tr> 950 951<tr> 952<td class="tabledata">C13</td> 953<td class="tabledata"><span style="font-family:Times">?</span>0.5930 (4)</td> 954<td class="tabledata">0.2400 (3)</td> 955<td class="tabledata">0.0753 (2)</td> 956<td class="tabledata">0.0845 (10)</td> 957<td class="tabledata"/> 958</tr> 959 960<tr> 961<td class="tabledata">H13A</td> 962<td class="tabledata"><span style="font-family:Times">?</span>0.6141</td> 963<td class="tabledata">0.3051</td> 964<td class="tabledata">0.0555</td> 965<td class="tabledata">0.101*</td> 966<td class="tabledata"/> 967</tr> 968 969<tr> 970<td class="tabledata">C14</td> 971<td class="tabledata"><span style="font-family:Times">?</span>0.6699 (4)</td> 972<td class="tabledata">0.1308 (3)</td> 973<td class="tabledata">0.0321 (2)</td> 974<td class="tabledata">0.0747 (9)</td> 975<td class="tabledata"/> 976</tr> 977 978<tr> 979<td class="tabledata">H14A</td> 980<td class="tabledata"><span style="font-family:Times">?</span>0.7435</td> 981<td class="tabledata">0.1206</td> 982<td class="tabledata"><span style="font-family:Times">?</span>0.0180</td> 983<td class="tabledata">0.090*</td> 984<td class="tabledata"/> 985</tr> 986 987<tr> 988<td class="tabledata">C15</td> 989<td class="tabledata"><span style="font-family:Times">?</span>0.2359 (5)</td> 990<td class="tabledata">0.2698 (3)</td> 991<td class="tabledata">0.2892 (3)</td> 992<td class="tabledata">0.1144 (14)</td> 993<td class="tabledata"/> 994</tr> 995 996<tr> 997<td class="tabledata">H15A</td> 998<td class="tabledata"><span style="font-family:Times">?</span>0.1725</td> 999<td class="tabledata">0.2635</td> 1000<td class="tabledata">0.3416</td> 1001<td class="tabledata">0.172*</td> 1002<td class="tabledata"/> 1003</tr> 1004 1005<tr> 1006<td class="tabledata">H15B</td> 1007<td class="tabledata"><span style="font-family:Times">?</span>0.2783</td> 1008<td class="tabledata">0.3437</td> 1009<td class="tabledata">0.3059</td> 1010<td class="tabledata">0.172*</td> 1011<td class="tabledata"/> 1012</tr> 1013 1014<tr> 1015<td class="tabledata">H15C</td> 1016<td class="tabledata"><span style="font-family:Times">?</span>0.1810</td> 1017<td class="tabledata">0.2697</td> 1018<td class="tabledata">0.2428</td> 1019<td class="tabledata">0.172*</td> 1020<td class="tabledata"/> 1021</tr> 1022 1023<tr> 1024<td class="tabledata">C16</td> 1025<td class="tabledata"><span style="font-family:Times">?</span>0.9135 (4)</td> 1026<td class="tabledata">0.5296 (3)</td> 1027<td class="tabledata">0.3767 (3)</td> 1028<td class="tabledata">0.1022 (12)</td> 1029<td class="tabledata"/> 1030</tr> 1031 1032<tr> 1033<td class="tabledata">H16A</td> 1034<td class="tabledata"><span style="font-family:Times">?</span>0.9594</td> 1035<td class="tabledata">0.5009</td> 1036<td class="tabledata">0.3135</td> 1037<td class="tabledata">0.153*</td> 1038<td class="tabledata"/> 1039</tr> 1040 1041<tr> 1042<td class="tabledata">H16B</td> 1043<td class="tabledata"><span style="font-family:Times">?</span>0.8613</td> 1044<td class="tabledata">0.6089</td> 1045<td class="tabledata">0.3911</td> 1046<td class="tabledata">0.153*</td> 1047<td class="tabledata"/> 1048</tr> 1049 1050<tr> 1051<td class="tabledata">H16C</td> 1052<td class="tabledata"><span style="font-family:Times">?</span>0.9865</td> 1053<td class="tabledata">0.5333</td> 1054<td class="tabledata">0.4133</td> 1055<td class="tabledata">0.153*</td> 1056<td class="tabledata"/> 1057</tr> 1058 1059<tr> 1060<td class="tabledata">C17</td> 1061<td class="tabledata"><span style="font-family:Times">?</span>0.8083 (3)</td> 1062<td class="tabledata">0.4442 (3)</td> 1063<td class="tabledata">0.3958 (2)</td> 1064<td class="tabledata">0.0697 (9)</td> 1065<td class="tabledata"/> 1066</tr> 1067 1068<tr> 1069<td class="tabledata">C18</td> 1070<td class="tabledata"><span style="font-family:Times">?</span>0.7874 (3)</td> 1071<td class="tabledata">0.3444 (3)</td> 1072<td class="tabledata">0.3287 (2)</td> 1073<td class="tabledata">0.0785 (10)</td> 1074<td class="tabledata"/> 1075</tr> 1076 1077<tr> 1078<td class="tabledata">H18A</td> 1079<td class="tabledata"><span style="font-family:Times">?</span>0.8404</td> 1080<td class="tabledata">0.3271</td> 1081<td class="tabledata">0.2698</td> 1082<td class="tabledata">0.094*</td> 1083<td class="tabledata"/> 1084</tr> 1085 1086<tr> 1087<td class="tabledata">C19</td> 1088<td class="tabledata"><span style="font-family:Times">?</span>0.6886 (3)</td> 1089<td class="tabledata">0.2687 (3)</td> 1090<td class="tabledata">0.3468 (2)</td> 1091<td class="tabledata">0.0693 (9)</td> 1092<td class="tabledata"/> 1093</tr> 1094 1095<tr> 1096<td class="tabledata">H19A</td> 1097<td class="tabledata"><span style="font-family:Times">?</span>0.6755</td> 1098<td class="tabledata">0.2015</td> 1099<td class="tabledata">0.3002</td> 1100<td class="tabledata">0.083*</td> 1101<td class="tabledata"/> 1102</tr> 1103 1104<tr> 1105<td class="tabledata">C20</td> 1106<td class="tabledata"><span style="font-family:Times">?</span>0.6098 (3)</td> 1107<td class="tabledata">0.2925 (3)</td> 1108<td class="tabledata">0.4334 (2)</td> 1109<td class="tabledata">0.0553 (7)</td> 1110<td class="tabledata"/> 1111</tr> 1112 1113<tr> 1114<td class="tabledata">C21</td> 1115<td class="tabledata"><span style="font-family:Times">?</span>0.6300 (3)</td> 1116<td class="tabledata">0.3916 (3)</td> 1117<td class="tabledata">0.5016 (2)</td> 1118<td class="tabledata">0.0731 (9)</td> 1119<td class="tabledata"/> 1120</tr> 1121 1122<tr> 1123<td class="tabledata">H21A</td> 1124<td class="tabledata"><span style="font-family:Times">?</span>0.5774</td> 1125<td class="tabledata">0.4087</td> 1126<td class="tabledata">0.5605</td> 1127<td class="tabledata">0.088*</td> 1128<td class="tabledata"/> 1129</tr> 1130 1131<tr> 1132<td class="tabledata">C22</td> 1133<td class="tabledata"><span style="font-family:Times">?</span>0.7291 (4)</td> 1134<td class="tabledata">0.4658 (3)</td> 1135<td class="tabledata">0.4820 (2)</td> 1136<td class="tabledata">0.0789 (10)</td> 1137<td class="tabledata"/> 1138</tr> 1139 1140<tr> 1141<td class="tabledata">H22A</td> 1142<td class="tabledata"><span style="font-family:Times">?</span>0.7428</td> 1143<td class="tabledata">0.5327</td> 1144<td class="tabledata">0.5287</td> 1145<td class="tabledata">0.095*</td> 1146<td class="tabledata"/> 1147</tr> 1148 1149<tr> 1150<td class="tabledata">C23</td> 1151<td class="tabledata"><span style="font-family:Times">?</span>0.4469 (3)</td> 1152<td class="tabledata">0.2038 (3)</td> 1153<td class="tabledata">0.52612 (19)</td> 1154<td class="tabledata">0.0588 (8)</td> 1155<td class="tabledata"/> 1156</tr> 1157 1158<tr> 1159<td class="tabledata">H23A</td> 1160<td class="tabledata"><span style="font-family:Times">?</span>0.4672</td> 1161<td class="tabledata">0.2573</td> 1162<td class="tabledata">0.5786</td> 1163<td class="tabledata">0.071*</td> 1164<td class="tabledata"/> 1165</tr> 1166 1167<tr> 1168<td class="tabledata">C24</td> 1169<td class="tabledata"><span style="font-family:Times">?</span>0.3500 (3)</td> 1170<td class="tabledata">0.1207 (3)</td> 1171<td class="tabledata">0.53644 (19)</td> 1172<td class="tabledata">0.0538 (7)</td> 1173<td class="tabledata"/> 1174</tr> 1175 1176<tr> 1177<td class="tabledata">C25</td> 1178<td class="tabledata"><span style="font-family:Times">?</span>0.2911 (3)</td> 1179<td class="tabledata">0.1204 (3)</td> 1180<td class="tabledata">0.6247 (2)</td> 1181<td class="tabledata">0.0752 (9)</td> 1182<td class="tabledata"/> 1183</tr> 1184 1185<tr> 1186<td class="tabledata">H25A</td> 1187<td class="tabledata"><span style="font-family:Times">?</span>0.3154</td> 1188<td class="tabledata">0.1754</td> 1189<td class="tabledata">0.6751</td> 1190<td class="tabledata">0.090*</td> 1191<td class="tabledata"/> 1192</tr> 1193 1194<tr> 1195<td class="tabledata">C26</td> 1196<td class="tabledata"><span style="font-family:Times">?</span>0.1992 (3)</td> 1197<td class="tabledata">0.0401 (3)</td> 1198<td class="tabledata">0.6363 (2)</td> 1199<td class="tabledata">0.0848 (10)</td> 1200<td class="tabledata"/> 1201</tr> 1202 1203<tr> 1204<td class="tabledata">H26A</td> 1205<td class="tabledata"><span style="font-family:Times">?</span>0.1606</td> 1206<td class="tabledata">0.0404</td> 1207<td class="tabledata">0.6947</td> 1208<td class="tabledata">0.102*</td> 1209<td class="tabledata"/> 1210</tr> 1211 1212<tr> 1213<td class="tabledata">C27</td> 1214<td class="tabledata"><span style="font-family:Times">?</span>0.1621 (3)</td> 1215<td class="tabledata"><span style="font-family:Times">?</span>0.0424 (3)</td> 1216<td class="tabledata">0.5618 (2)</td> 1217<td class="tabledata">0.0712 (9)</td> 1218<td class="tabledata"/> 1219</tr> 1220 1221<tr> 1222<td class="tabledata">H27A</td> 1223<td class="tabledata"><span style="font-family:Times">?</span>0.0974</td> 1224<td class="tabledata"><span style="font-family:Times">?</span>0.0959</td> 1225<td class="tabledata">0.5712</td> 1226<td class="tabledata">0.085*</td> 1227<td class="tabledata"/> 1228</tr> 1229 1230<tr> 1231<td class="tabledata">C28</td> 1232<td class="tabledata"><span style="font-family:Times">?</span>0.2183 (3)</td> 1233<td class="tabledata"><span style="font-family:Times">?</span>0.0470 (3)</td> 1234<td class="tabledata">0.4748 (2)</td> 1235<td class="tabledata">0.0597 (8)</td> 1236<td class="tabledata"/> 1237</tr> 1238 1239<tr> 1240<td class="tabledata">C29</td> 1241<td class="tabledata"><span style="font-family:Times">?</span>0.3157 (3)</td> 1242<td class="tabledata">0.0361 (2)</td> 1243<td class="tabledata">0.45939 (19)</td> 1244<td class="tabledata">0.0517 (7)</td> 1245<td class="tabledata"/> 1246</tr> 1247 1248<tr> 1249<td class="tabledata">C30</td> 1250<td class="tabledata"><span style="font-family:Times">?</span>0.1088 (4)</td> 1251<td class="tabledata"><span style="font-family:Times">?</span>0.2196 (3)</td> 1252<td class="tabledata">0.4021 (3)</td> 1253<td class="tabledata">0.0940 (11)</td> 1254<td class="tabledata"/> 1255</tr> 1256 1257<tr> 1258<td class="tabledata">H30A</td> 1259<td class="tabledata"><span style="font-family:Times">?</span>0.0982</td> 1260<td class="tabledata"><span style="font-family:Times">?</span>0.2661</td> 1261<td class="tabledata">0.3421</td> 1262<td class="tabledata">0.141*</td> 1263<td class="tabledata"/> 1264</tr> 1265 1266<tr> 1267<td class="tabledata">H30B</td> 1268<td class="tabledata"><span style="font-family:Times">?</span>0.1583</td> 1269<td class="tabledata"><span style="font-family:Times">?</span>0.2708</td> 1270<td class="tabledata">0.4284</td> 1271<td class="tabledata">0.141*</td> 1272<td class="tabledata"/> 1273</tr> 1274 1275<tr> 1276<td class="tabledata">H30C</td> 1277<td class="tabledata"><span style="font-family:Times">?</span>0.0142</td> 1278<td class="tabledata"><span style="font-family:Times">?</span>0.1865</td> 1279<td class="tabledata">0.4394</td> 1280<td class="tabledata">0.141*</td> 1281<td class="tabledata"/> 1282</tr> 1283 1284<tr> 1285<td class="tabledata">C31</td> 1286<td class="tabledata"><span style="font-family:Times">?</span>0.4834 (4)</td> 1287<td class="tabledata"><span style="font-family:Times">?</span>0.3275 (3)</td> 1288<td class="tabledata">0.2352 (2)</td> 1289<td class="tabledata">0.0683 (8)</td> 1290<td class="tabledata"/> 1291</tr> 1292 1293<tr> 1294<td class="tabledata">C32</td> 1295<td class="tabledata"><span style="font-family:Times">?</span>0.0746 (3)</td> 1296<td class="tabledata"><span style="font-family:Times">?</span>0.0081 (3)</td> 1297<td class="tabledata">0.1911 (2)</td> 1298<td class="tabledata">0.0637 (8)</td> 1299<td class="tabledata"/> 1300</tr> 1301</table> 1302</div> 1303 1304<!-- endtablewrapcoordsdiv --> 1305<div class="tablewrapadps"><a id="atomicdisplacement1" name="atomicdisplacement1"/> <span class="heading3">Atomic 1306displacement parameters (�<sup>2</sup>)</span> 1307<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 1308<table style="table-layout:fixed" width="100%" summary="" class="tabledata"> 1309<tr> 1310<td class="tabledata"/> 1311<td class="tabledata"><i>U</i><sup>11</sup></td> 1312<td class="tabledata"><i>U</i><sup>22</sup></td> 1313<td class="tabledata"><i>U</i><sup>33</sup></td> 1314<td class="tabledata"><i>U</i><sup>12</sup></td> 1315<td class="tabledata"><i>U</i><sup>13</sup></td> 1316<td class="tabledata"><i>U</i><sup>23</sup></td> 1317</tr> 1318 1319<tr> 1320<td class="tabledata">Zn1</td> 1321<td class="tabledata">0.0619 (2)</td> 1322<td class="tabledata">0.0679 (3)</td> 1323<td class="tabledata">0.0583 (2)</td> 1324<td class="tabledata">0.01883 (18)</td> 1325<td class="tabledata">0.00923 (17)</td> 1326<td class="tabledata">0.02127 (19)</td> 1327</tr> 1328 1329<tr> 1330<td class="tabledata">S1</td> 1331<td class="tabledata">0.1446 (10)</td> 1332<td class="tabledata">0.0636 (6)</td> 1333<td class="tabledata">0.1012 (8)</td> 1334<td class="tabledata">0.0019 (6)</td> 1335<td class="tabledata">0.0117 (7)</td> 1336<td class="tabledata">0.0221 (6)</td> 1337</tr> 1338 1339<tr> 1340<td class="tabledata">O1</td> 1341<td class="tabledata">0.1016 (17)</td> 1342<td class="tabledata">0.0752 (16)</td> 1343<td class="tabledata">0.0740 (15)</td> 1344<td class="tabledata"><span style="font-family:Times">?</span>0.0010 (14)</td> 1345<td class="tabledata"><span style="font-family:Times">?</span>0.0175 (13)</td> 1346<td class="tabledata">0.0231 (13)</td> 1347</tr> 1348 1349<tr> 1350<td class="tabledata">N1</td> 1351<td class="tabledata">0.091 (2)</td> 1352<td class="tabledata">0.068 (2)</td> 1353<td class="tabledata">0.094 (2)</td> 1354<td class="tabledata">0.0205 (17)</td> 1355<td class="tabledata">0.0160 (17)</td> 1356<td class="tabledata">0.0277 (17)</td> 1357</tr> 1358 1359<tr> 1360<td class="tabledata">C1</td> 1361<td class="tabledata">0.181 (4)</td> 1362<td class="tabledata">0.076 (3)</td> 1363<td class="tabledata">0.079 (3)</td> 1364<td class="tabledata"><span style="font-family:Times">?</span>0.021 (3)</td> 1365<td class="tabledata">0.019 (3)</td> 1366<td class="tabledata">0.013 (2)</td> 1367</tr> 1368 1369<tr> 1370<td class="tabledata">S2</td> 1371<td class="tabledata">0.0689 (5)</td> 1372<td class="tabledata">0.1181 (8)</td> 1373<td class="tabledata">0.0777 (6)</td> 1374<td class="tabledata">0.0175 (5)</td> 1375<td class="tabledata">0.0134 (4)</td> 1376<td class="tabledata">0.0466 (6)</td> 1377</tr> 1378 1379<tr> 1380<td class="tabledata">O2</td> 1381<td class="tabledata">0.0714 (13)</td> 1382<td class="tabledata">0.0656 (13)</td> 1383<td class="tabledata">0.0665 (13)</td> 1384<td class="tabledata">0.0135 (11)</td> 1385<td class="tabledata"><span style="font-family:Times">?</span>0.0055 (10)</td> 1386<td class="tabledata">0.0249 (11)</td> 1387</tr> 1388 1389<tr> 1390<td class="tabledata">N2</td> 1391<td class="tabledata">0.0642 (19)</td> 1392<td class="tabledata">0.113 (2)</td> 1393<td class="tabledata">0.080 (2)</td> 1394<td class="tabledata">0.0202 (17)</td> 1395<td class="tabledata">0.0182 (16)</td> 1396<td class="tabledata">0.0419 (18)</td> 1397</tr> 1398 1399<tr> 1400<td class="tabledata">C2</td> 1401<td class="tabledata">0.120 (3)</td> 1402<td class="tabledata">0.080 (3)</td> 1403<td class="tabledata">0.055 (2)</td> 1404<td class="tabledata">0.003 (3)</td> 1405<td class="tabledata">0.016 (2)</td> 1406<td class="tabledata">0.022 (2)</td> 1407</tr> 1408 1409<tr> 1410<td class="tabledata">N3</td> 1411<td class="tabledata">0.0606 (15)</td> 1412<td class="tabledata">0.0660 (18)</td>…
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