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E<b>65</b>, 47m125����[ <a title="Open URL link" href="http://dx.doi.org/10.1107/S1600536808042621">doi:10.1107/S1600536808042621</a> 48]</p> 49</div> 50 51<h3>Pentacarbonyl-2<img alt="[kappa]" border="0" src="/logos/entities/kappa_rmgif.gif"/><span class="sup"><sup>5</sup></span><span class="it"><i>C</i></span>-chlorido-1<img alt="[kappa]" border="0" src="/logos/entities/kappa_rmgif.gif"/><span class="it"><i>Cl</i></span>-bis[1(<img alt="[eta]" border="0" src="/logos/entities/eta_rmgif.gif"/><span class="sup"><sup>5</sup></span>)-cyclopentadienyl](<img alt="[mu]" border="0" src="/logos/entities/mu_rmgif.gif"/>-1-oxidoethylene-1:2<img alt="[kappa]" border="0" src="/logos/entities/kappa_rmgif.gif"/><span class="sup"><sup>2</sup></span><span class="it"><i>O</i></span>:<span class="it"><i>C</i></span>)chromium(0)zirconium(IV)</h3> 52 53<h3><a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Esterhuysen,%20C."> 54C. Esterhuysen</a>, <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Retief,%20L."> 55L. Retief</a>, <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Kruger,%20G.J."> 56G. J. Kruger</a>, <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Cronje,%20S."> 57S. Cronje</a> and <a href="http://scripts.iucr.org/cgi-bin/citedin?search_on=name&author_name=Raubenheimer,%20H.G."> 58H. G. Raubenheimer</a></h3> 59 60<div class="abstract"><a id="abstract" name="abstract"/> 61 62<div class="heading2">Abstract <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 63</div> 64 65<!-- endheading2div --> 66<p>The title compound, [CrZr(C<span class="inf"><sub>5</sub></span>H<span class="inf"><sub>5</sub></span>)<span class="inf"><sub>2</sub></span>(C<span class="inf"><sub>2</sub></span>H<span class="inf"><sub>3</sub></span>O)Cl(CO)<span class="inf"><sub>5</sub></span>], consists of two metal centres, 67with a (pentacarbonylchromium)oxymethylcarbene group coordinating 68as a monodentate ligand to the zirconocene chloride. <img alt="[pi]" border="0" src="/logos/entities/pi_rmgif.gif"/>-Delocalization through the 69Zr-O-C=Cr unit is indicated by a short Zr-O distance 70[2.041�(3)��] and a nearly linear Zr-O-C angle 71[170.5�(3)�]. Molecules are aligned with their molecular 72planes (through Zr, Cl, carbene and Cr) parallel to the <span class="it"><i>ab</i></span> plane. C-H<img alt="..." border="0" src="/logos/entities/ctdot_rmgif.gif"/>Cl interactions result in 73zigzag chains of molecules propagating parallel to the <span class="it"><i>b</i></span> axis.</p> 74</div> 75 76<!-- endabstractdiv --> 77<div class="contentslist"> 78<ul> 79<li class="comment"><a title="Comment" href="#comment">Comment</a></li> 80 81<li class="relatedliterature"><a title="Related literature" href="#relatedliterature">Related literature</a></li> 82 83<li class="experimental"><a title="Experimental" href="#experimental">Experimental</a></li> 84 85<li class="refinement"><a title="Refinement" href="#refinement">Refinement</a></li> 86 87<li class="computingdetails"><a title="Computing details" href="#computingdetails">Computing details</a></li> 88 89<li class="figures"><a title="Figures" href="#figures">Figures</a></li> 90 91<li><a title="(I)" href="#chemicalname1">Pentacarbonyl-2<span style="font-family:Times">?</span><sup>5</sup>C-chlorido-1<span style="font-family:Times">?</span>Cl-bis[1(<span style="font-family:Times">?</span><sup>5</sup>)-cyclopentadienyl](�-1- 92oxidoethylene-1:2<span style="font-family:Times">?</span><sup>2</sup>O:C)chromiumzirconium</a> 93 94 95<ul> 96<li><a title="Crystal data" href="#crystaldata1">Crystal 97data</a></li> 98 99<li><a title="Data collection" href="#datacollection1">Data 100collection</a></li> 101 102<li><a title="Refinement data" href="#refinementdata1">Refinement 103data</a></li> 104 105<li class="specialdetails"><a title="Special details" href="#specialdetails1">Special details</a></li> 106 107<li class="licoords"><a title="Fractional atomic coordinates" href="#fractionalatomiccoordinates1">Fractional atomic 108coordinates</a></li> 109 110<li class="liadps"><a title="Atomic displacement parameters" href="#atomicdisplacement1">Atomic displacement parameters</a></li> 111 112<li class="ligeomlong"><a title="Geometric parameters" href="#geometricparameters1">Geometric parameters</a></li> 113 114<li class="lihbondslong"><a title="Hydrogen-bond geometry" href="#hydrogen-bondgeometry1">Hydrogen-bond geometry</a></li> 115 116<li class="ligeomshort"><a title="Geometric parameters" href="#geometricparameters1">Geometric parameters</a></li> 117 118<li class="lihbondsshort"><a title="Hydrogen-bond geometry" href="#hydrogen-bondgeometry1">Hydrogen-bond geometry</a></li> 119</ul> 120</li> 121 122<li class="acknowledgements"><a title="Acknowledgements" href="#acknowledgements">Acknowledgements</a></li> 123 124<li class="publreferences"><a title="References" href="#publreferences">References</a></li> 125</ul> 126</div> 127 128<!-- endcontentslistdiv --> 129<div class="comment"><a id="comment" name="comment"/> 130 131<div class="heading2">Comment <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 132</div> 133 134<!-- endheading2div --> 135<p>Since Cp<sub>2</sub>TiCl<sub>2</sub> was shown to polymerize 136ethylene when activated by methylaluminoxane, MAO (Sinn <i>et 137al.</i>, 1980), derivatives of this compound have been synthesized 138where a Cl ligand was replaced by a monodentate anionic 139Fischer-type carbene ligand (Barluenga and Fa�an�s, 1402000). We have shown that zirconocene equivalents of this family of 141homogeneous catalysts, 142Cp<sub>2</sub>Zr(Cl)OC(<i>R</i>)<i>M</i>(CO)<sub>5</sub> (where 143<i>M</i> = W or Cr), catalyze the oligomerization of 1-pentene, as 144well as the copolymerization of ethene and 1-pentene, in the 145presence of MAO (Luruli <i>et al.</i>, 2004; Luruli <i>et al.</i>, 1462006). Herein we report the crystal structure of the title 147zirconocene complex, (I).</p> 148 149<p>In the molecular structure the Zr-O and O-C distances are 150similar to those found in the equivalent tungsten pentacarbonyl 151complex (Esterhuysen, Nel & Cronje, 2008). The Zr-O-C angle, on 152the other hand, is less linear than the previously published 153tungsten structure [177.4�(7)�], but similar to the 154hafnocene complex 155W(CO)<sub>5</sub>C(C<sub>6</sub>H<sub>5</sub>)OHf(C<sub>5</sub>H<sub> 1565</sub>)<sub>2</sub>Cl (Esterhuysen, Neveling <i>et al.</i>, 2008), 157where the Hf-O-C angle deviates slightly more from linearity 158[171.4�(3)�]. These results are indicative of <span style="font-family:Times">?</span> delocalization through the 159Zr-O-C = W unit.</p> 160 161<p>Molecules are linked by C-H���Cl interactions 162into zigzag chains along the <i>b</i> axis. All molecules in a 163chain point in the same direction, with their molecular planes 164parallel. Neighbouring chains in the a-direction have the same 165orientation, thus forming a layer parallel to the <i>ab</i>-plane. 166Molecules in neighbouring layers in the c-direction have 167alternating orientations.</p> 168</div> 169 170<!-- endcommentdiv --> 171<div class="relatedliterature"><a id="relatedliterature" name="relatedliterature"/> 172 173<div class="heading2">Related literature <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 174</div> 175 176<!-- endheading2div --> 177<p>For related literature regarding catalytic data of the title 178compound, see: Sinn <i>et al.</i> (1980); Luruli <i>et al.</i> 179(2004, 2006). For other cases of anionic Fischer-type carbenes 180being used as monodentate ligands, see: Barluenga & 181Fa�an�s (2000). For comparable structures, see: 182Esterhuysen, Nel & Cronje (2008); Esterhuysen, Neveling <i>et 183al.</i> (2008).</p> 184</div> 185 186<!-- endrelatedliteraturediv --> 187<div class="experimental"><a id="experimental" name="experimental"/> 188 189<div class="heading2">Experimental <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 190</div> 191 192<!-- endheading2div --> 193<p>A solution of LiCH<sub>3</sub> (11 ml, 1.5<i>M</i> in 194diethylether, 16.5 mmol) in 10 ml diethylether was added to a well 195stirred suspension of Cr(CO)<sub>6</sub> (3.30 g, 15.0 mmol) in 100 196ml of diethylether over the period of 1.5 h. The mixture was 197stripped of solvent <i>in vacuo</i>. The residue was dried for 3 h, 198extracted with cold (273 K), degassed water (1 � 40 ml, 2 199� 20 ml) and the formed solution filtered. The aqueous 200solution was treated with a solution of [NEt<sub>4</sub>]Cl (2.49 201g, 15 mmol) in cold, degassed water (4 ml) and the formed 202precipitate was isolated and dried overnight <i>in vacuo</i>. The 203precipitate was dissolved in warm CH<sub>2</sub>Cl<sub>2</sub> (5 204ml) layered with penatne and cooled to 258 K to yield yellow 205crystals of (CO)<sub>5</sub>Cr{=C(Me)O}[NEt<sub>4</sub>]. A 206solution of 0.61 g (2.0 mmol) of the product in 30 ml of 207CH<sub>2</sub>Cl<sub>2</sub> was added to a solution of 208Cp<sub>2</sub>ZrCl<sub>2</sub> (0.58 g, 2.0 mmol) in 70 ml of 209diethylether at 233 K over a period of 40 min. AgBF<sub>4</sub> 210(0.39 g, 2.0 mmol) was then added to the mixture and stirred for an 211hour at 233 K. After reaching room temperature the solvent was 212removed in vacuo and the residue extracted in 5 portions of 10 ml 213of toluene. The extract was filtered, and the filtrate dried over 214anhydrous MgSO<sub>4</sub>. The solution was layered with pentane 215and kept at 258 K to yield orange crystals suitable for X-ray 216diffraction analysis.</p> 217</div> 218 219<!-- endexperimentaldiv --> 220<div class="refinement"><a id="refinement" name="refinement"/> 221 222<div class="heading2">Refinement <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 223</div> 224 225<!-- endheading2div --> 226<p>H atoms were positioned geometrically, with C-H = 0.95 � 227and 0.98 �, and constrained to ride on their parent atoms, 228with <i>U</i><sub>iso</sub>(H) = 1.2 or 2291.5<i>U</i><sub>eq</sub>(C). Large anisotropy on atoms C16 and C17 230suggests the presence of disorder in the C13-C17 Cp ring, however 231this could not be modeled. Highest peak: 1.03 � from Zr1; 232deepest hole: 1.04 � from Zr1.</p> 233</div> 234 235<!-- endrefinementdiv --> 236<div class="computingdetails"><a id="computingdetails" name="computingdetails"/> 237 238<div class="heading2">Computing details <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 239</div> 240 241<!-- endheading2div --> 242<p>Data collection: PWPC (Gomm, 1998); cell refinement: PWPC (Gomm, 2431998); data reduction: <i>Xtal3</i>.4 (Hall <i>et al.</i>, 1995); 244program(s) used to solve structure: <i>SHELXS97</i> (Sheldrick, 2452008); program(s) used to refine structure: <i>SHELXL97</i> 246(Sheldrick, 2008); molecular graphics: <i>X-SEED</i> (Barbour, 2472001; Atwood & Barbour, 2003); software used to prepare 248material for publication: publCIF (Westrip, 2009).</p> 249</div> 250 251<!-- endcomputingdetailsdiv --> 252<div class="schemes"><a href="./at2691scheme1.gif"/></div> 253 254<!-- endschemesdiv --> 255<div class="figures"><a id="figures" name="figures"/> 256 257<div class="heading2">Figures <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 258</div> 259 260<!-- endheading2div --> 261<table style="table-layout:fixed" width="100%" class="nodecs"> 262<colgroup span="2"> 263<col width="110"/> 264<col/></colgroup> 265 266<tr> 267<td class="nodecs" align="center" width="110"><a href="./at2691fig1.html"><img width="100" src="./at2691fig1thm.gif" alt="[Figure 1]" align="middle"/></a> </td> 268<td class="nodecs" valign="middle">Fig. 1. The molecular structure 269of (I) showing the atomic labelling scheme and displacement 270ellipsoids drawn at the 50% probability level. </td> 271</tr> 272 273<tr> 274<td class="nodecs" align="center" width="110"><a href="./at2691fig2.html"><img width="100" src="./at2691fig2thm.gif" alt="[Figure 2]" align="middle"/></a> </td> 275<td class="nodecs" valign="middle">Fig. 2. A portion of the packing 276diagram showing zigzag chains of molecules forming a layer 277perpendicular to the <i>c</i> axis. </td> 278</tr> 279</table> 280</div> 281 282<!-- endfiguresdiv --> 283<div class="datablock1"> 284<div class="heading2"><a id="chemicalname1" name="chemicalname1"/>Pentacarbonyl-2<span style="font-family:Times">?</span><sup>5</sup>C-chlorido-1<span style="font-family:Times">?</span>Cl-bis[1(<span style="font-family:Times">?</span><sup>5</sup>)-cyclopentadienyl](�-1- 285oxidoethylene-1:2<span style="font-family:Times">?</span><sup>2</sup>O:C)chromiumzirconium 286<span class="toplink"><a class="buttons" href="#top">top</a></span> 287<!-- endtoplinkspan --> 288</div> 289 290<!-- endheading2div --> 291<div class="tablewrapcrystaldatalong"><a id="crystaldata1" name="crystaldata1"/><span class="heading3">Crystal data</span> 292<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 293<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 294<colgroup span="2"> 295<col width="50%"/> 296<col width="50%"/></colgroup> 297 298<tr> 299<td width="50%" class="tabledata"> 300[CrZr(C<sub>5</sub>H<sub>5</sub>)<sub>2</sub>(C<sub>2</sub>H<sub>3</sub>O)Cl(CO)<sub> 3015</sub>]</td> 302<td width="50%" class="tabledata"><i>F</i>(000) = 976</td> 303</tr> 304 305<tr> 306<td width="50%" class="tabledata"><i>M</i><i><sub>r</sub></i> = 307491.94</td> 308<td width="50%" class="tabledata"><i>D</i><sub>x</sub> = 1.686 Mg 309m<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 310</tr> 311 312<tr> 313<td width="50%" class="tabledata">Monoclinic, 314<i>P</i>2<sub>1</sub>/<i>c</i></td> 315<td width="50%" class="tabledata">Mo <i>K</i><span style="font-family:Times">?</span> radiation, <span style="font-family:Times">?</span> = 0.71073 �</td> 316</tr> 317 318<tr> 319<td width="50%" class="tabledata">Hall symbol: -P 2ybc</td> 320<td width="50%" class="tabledata">Cell parameters from 48 321reflections</td> 322</tr> 323 324<tr> 325<td width="50%" class="tabledata"><i>a</i> = 12.7395 (7) 326�</td> 327<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 2-17�</td> 328</tr> 329 330<tr> 331<td width="50%" class="tabledata"><i>b</i> = 12.1117 (6) 332�</td> 333<td width="50%" class="tabledata">� = 1.27 mm<span style="font-family:Times"><sup>?</sup></span><sup>1</sup></td> 334</tr> 335 336<tr> 337<td width="50%" class="tabledata"><i>c</i> = 12.7859 (7) 338�</td> 339<td width="50%" class="tabledata"><i>T</i> = 173 K</td> 340</tr> 341 342<tr> 343<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 100.826 (5)�</td> 344<td width="50%" class="tabledata">Plate, orange</td> 345</tr> 346 347<tr> 348<td width="50%" class="tabledata"><i>V</i> = 1937.71 (18) 349�<sup>3</sup></td> 350<td width="50%" class="tabledata">0.30 � 0.28 � 0.08 351mm</td> 352</tr> 353 354<tr> 355<td width="50%" class="tabledata"><i>Z</i> = 4</td> 356<td width="50%" class="tabledata"/> 357</tr> 358</table> 359 360<!-- endtabledatatable --> 361</div> 362 363<!-- endtablewrapcrystaldatalongdiv --> 364<div class="tablewrapdatacollectionlong"><a id="datacollection1" name="datacollection1"/><span class="heading3">Data 365collection</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 366<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 367<colgroup span="2"> 368<col width="50%"/> 369<col width="50%"/></colgroup> 370 371<tr> 372<td width="50%" class="tabledata">Philips PW1100<br/> 373diffractometer</td> 374<td width="50%" class="tabledata">2332 reflections with <i>I</i> 375> 2<span style="font-family:Times">?</span>(<i>I</i>)</td> 376</tr> 377 378<tr> 379<td width="50%" class="tabledata">Radiation source: fine-focus 380sealed tube</td> 381<td width="50%" class="tabledata"><i>R</i><sub>int</sub> = 3820.000</td> 383</tr> 384 385<tr> 386<td width="50%" class="tabledata">graphite</td> 387<td width="50%" class="tabledata"><span style="font-family:Times">?</span><sub>max</sub> = 25.0�, 388<span style="font-family:Times">?</span><sub>min</sub> = 3892.3�</td> 390</tr> 391 392<tr> 393<td width="50%" class="tabledata"><span style="font-family:Times">?</span>-2<span style="font-family:Times">?</span> scans</td> 394<td width="50%" class="tabledata"><i>h</i> = <span style="font-family:Times">?</span>15<span style="font-family:Times">?</span>14</td> 395</tr> 396 397<tr> 398<td width="50%" class="tabledata">Absorption correction: <span style="font-family:Times">?</span> scan<br/> 399(North <i>et al.</i>, 1968)</td> 400<td width="50%" class="tabledata"><i>k</i> = 0<span style="font-family:Times">?</span>14</td> 401</tr> 402 403<tr> 404<td width="50%" class="tabledata"><i>T</i><sub>min</sub> = 0.68, 405<i>T</i><sub>max</sub> = 0.88</td> 406<td width="50%" class="tabledata"><i>l</i> = 0<span style="font-family:Times">?</span>15</td> 407</tr> 408 409<tr> 410<td width="50%" class="tabledata">3423 measured reflections</td> 411<td width="50%" class="tabledata">3 standard reflections every 50 412reflections</td> 413</tr> 414 415<tr> 416<td width="50%" class="tabledata">3423 independent reflections</td> 417<td width="50%" class="tabledata">intensity decay: none</td> 418</tr> 419</table> 420 421<!-- endtabledatatable --> 422</div> 423 424<!-- endtablewrapdatacollectionlongdiv --> 425<div class="tablewraprefinementdatalong"><a id="refinementdata1" name="refinementdata1"/><span class="heading3">Refinement</span> 426<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 427<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 428<colgroup span="2"> 429<col width="50%"/> 430<col width="50%"/></colgroup> 431 432<tr> 433<td width="50%" class="tabledata">Refinement on 434<i>F</i><sup>2</sup></td> 435<td width="50%" class="tabledata">Primary atom site location: 436structure-invariant direct methods</td> 437</tr> 438 439<tr> 440<td width="50%" class="tabledata">Least-squares matrix: full</td> 441<td width="50%" class="tabledata">Secondary atom site location: 442difference Fourier map</td> 443</tr> 444 445<tr> 446<td width="50%" class="tabledata"><i>R</i>[<i>F</i><sup>2</sup> 447> 2<span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>)] = 4480.039</td> 449<td width="50%" class="tabledata">Hydrogen site location: inferred 450from neighbouring sites</td> 451</tr> 452 453<tr> 454<td width="50%" class="tabledata"><i>wR</i>(<i>F</i><sup>2</sup>) = 4550.109</td> 456<td width="50%" class="tabledata">H-atom parameters 457constrained</td> 458</tr> 459 460<tr> 461<td width="50%" class="tabledata"><i>S</i> = 1.06</td> 462<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> 4632</sup>) + (0.053<i>P</i>)<sup>2</sup>]<br/> 464where <i>P</i> = (<i>F</i><sub>o</sub><sup>2</sup> + 4652<i>F</i><sub>c</sub><sup>2</sup>)/3</td> 466</tr> 467 468<tr> 469<td width="50%" class="tabledata">3423 reflections</td> 470<td width="50%" class="tabledata">(?/<span style="font-family:Times">?</span>)<sub>max</sub> < 4710.001</td> 472</tr> 473 474<tr> 475<td width="50%" class="tabledata">235 parameters</td> 476<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>max</sub> = 0.55 e 477�<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 478</tr> 479 480<tr> 481<td width="50%" class="tabledata">0 restraints</td> 482<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>min</sub> = <span style="font-family:Times">?</span>0.58 e �<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 483</tr> 484</table> 485 486<!-- endtabledatatable --> 487</div> 488 489<!-- endtablewraprefinementdatalongdiv --> 490<div class="tablewrapcrystaldatashort"><a id="crystaldata1" name="crystaldata1"/><span class="heading3">Crystal data</span> 491<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 492<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 493<colgroup span="2"> 494<col width="50%"/> 495<col width="50%"/></colgroup> 496 497<tr> 498<td width="50%" class="tabledata"> 499[CrZr(C<sub>5</sub>H<sub>5</sub>)<sub>2</sub>(C<sub>2</sub>H<sub>3</sub>O)Cl(CO)<sub> 5005</sub>]</td> 501<td width="50%" class="tabledata"><i>V</i> = 1937.71 (18) 502�<sup>3</sup></td> 503</tr> 504 505<tr> 506<td width="50%" class="tabledata"><i>M</i><i><sub>r</sub></i> = 507491.94</td> 508<td width="50%" class="tabledata"><i>Z</i> = 4</td> 509</tr> 510 511<tr> 512<td width="50%" class="tabledata">Monoclinic, 513<i>P</i>2<sub>1</sub>/<i>c</i></td> 514<td width="50%" class="tabledata">Mo <i>K</i><span style="font-family:Times">?</span> radiation</td> 515</tr> 516 517<tr> 518<td width="50%" class="tabledata"><i>a</i> = 12.7395 (7) 519�</td> 520<td width="50%" class="tabledata">� = 1.27 mm<span style="font-family:Times"><sup>?</sup></span><sup>1</sup></td> 521</tr> 522 523<tr> 524<td width="50%" class="tabledata"><i>b</i> = 12.1117 (6) 525�</td> 526<td width="50%" class="tabledata"><i>T</i> = 173 K</td> 527</tr> 528 529<tr> 530<td width="50%" class="tabledata"><i>c</i> = 12.7859 (7) 531�</td> 532<td width="50%" class="tabledata">0.30 � 0.28 � 0.08 533mm</td> 534</tr> 535 536<tr> 537<td width="50%" class="tabledata"><span style="font-family:Times">?</span> = 100.826 (5)�</td> 538<td width="50%" class="tabledata"/> 539</tr> 540</table> 541 542<!-- endtabledatatable --> 543</div> 544 545<!-- endtablewrapcrystaldatashortdiv --> 546<div class="tablewrapdatacollectionshort"><a id="datacollection1" name="datacollection1"/><span class="heading3">Data 547collection</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 548<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 549<colgroup span="2"> 550<col width="50%"/> 551<col width="50%"/></colgroup> 552 553<tr> 554<td width="50%" class="tabledata">Philips PW1100<br/> 555diffractometer</td> 556<td width="50%" class="tabledata">2332 reflections with <i>I</i> 557> 2<span style="font-family:Times">?</span>(<i>I</i>)</td> 558</tr> 559 560<tr> 561<td width="50%" class="tabledata">Absorption correction: <span style="font-family:Times">?</span> scan<br/> 562(North <i>et al.</i>, 1968)</td> 563<td width="50%" class="tabledata"><i>R</i><sub>int</sub> = 5640.000</td> 565</tr> 566 567<tr> 568<td width="50%" class="tabledata"><i>T</i><sub>min</sub> = 0.68, 569<i>T</i><sub>max</sub> = 0.88</td> 570<td width="50%" class="tabledata"><span style="font-family:Times">?</span><sub>max</sub> = 57125.0�</td> 572</tr> 573 574<tr> 575<td width="50%" class="tabledata">3423 measured reflections</td> 576<td width="50%" class="tabledata">3 standard reflections every 50 577reflections</td> 578</tr> 579 580<tr> 581<td width="50%" class="tabledata">3423 independent reflections</td> 582<td width="50%" class="tabledata">intensity decay: none</td> 583</tr> 584</table> 585 586<!-- endtabledatatable --> 587</div> 588 589<!-- endtablewrapdatacollectionshortdiv --> 590<div class="tablewraprefinementdatashort"><a id="refinementdata1" name="refinementdata1"/><span class="heading3">Refinement</span> 591<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 592<table style="table-layout:fixed" width="80%" summary="" class="tabledata"> 593<colgroup span="2"> 594<col width="50%"/> 595<col width="50%"/></colgroup> 596 597<tr> 598<td width="50%" class="tabledata"><i>R</i>[<i>F</i><sup>2</sup> 599> 2<span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>)] = 6000.039</td> 601<td width="50%" class="tabledata">0 restraints</td> 602</tr> 603 604<tr> 605<td width="50%" class="tabledata"><i>wR</i>(<i>F</i><sup>2</sup>) = 6060.109</td> 607<td width="50%" class="tabledata">H-atom parameters 608constrained</td> 609</tr> 610 611<tr> 612<td width="50%" class="tabledata"><i>S</i> = 1.06</td> 613<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>max</sub> = 0.55 e 614�<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 615</tr> 616 617<tr> 618<td width="50%" class="tabledata">3423 reflections</td> 619<td width="50%" class="tabledata">?<span style="font-family:Times">?</span><sub>min</sub> = <span style="font-family:Times">?</span>0.58 e �<span style="font-family:Times"><sup>?</sup></span><sup>3</sup></td> 620</tr> 621 622<tr> 623<td width="50%" class="tabledata">235 parameters</td> 624<td width="50%" class="tabledata"/> 625</tr> 626</table> 627 628<!-- endtabledatatable --> 629</div> 630 631<!-- endtablewraprefinementdatashortdiv --> 632<div class="specialdetails"><a id="specialdetails1" name="specialdetails1"/><span class="heading3">Special 633details</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 634<table style="table-layout:fixed" width="100%" class="tabledata"> 635<tr> 636<td class="tabledata"> 637<p><b>Geometry</b>. All e.s.d.'s (except the e.s.d. in the 638dihedral angle between two l.s. planes) are estimated using the 639full covariance matrix. The cell e.s.d.'s are taken into 640account individually in the estimation of e.s.d.'s in 641distances, angles and torsion angles; correlations between 642e.s.d.'s in cell parameters are only used when they are defined 643by crystal symmetry. An approximate (isotropic) treatment of cell 644e.s.d.'s is used for estimating e.s.d.'s involving l.s. 645planes.</p> 646</td> 647</tr> 648 649<tr> 650<td class="tabledata"> 651<p><b>Refinement</b>. Refinement of <i>F</i><sup>2</sup> against 652ALL reflections. The weighted <i>R</i>-factor <i>wR</i> and 653goodness of fit <i>S</i> are based on <i>F</i><sup>2</sup>, 654conventional <i>R</i>-factors <i>R</i> are based on <i>F</i>, with 655<i>F</i> set to zero for negative <i>F</i><sup>2</sup>. The 656threshold expression of <i>F</i><sup>2</sup> > <span style="font-family:Times">?</span>(<i>F</i><sup>2</sup>) is 657used only for calculating <i>R</i>-factors(gt) <i>etc</i>. and is 658not relevant to the choice of reflections for refinement. 659<i>R</i>-factors based on <i>F</i><sup>2</sup> are statistically 660about twice as large as those based on <i>F</i>, and <i>R</i>- 661factors based on ALL data will be even larger.</p> 662</td> 663</tr> 664</table> 665</div> 666 667<!-- endspecialdetailsdiv --> 668<div class="tablewrapcoords"><a id="fractionalatomiccoordinates1" name="fractionalatomiccoordinates1"/> <span class="heading3">Fractional atomic coordinates and isotropic or 669equivalent isotropic displacement parameters 670(�<sup>2</sup>)</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span> 671<!-- endtoplinkspan --> 672<table style="table-layout:fixed" width="100%" summary="" class="tabledata"> 673<tr> 674<td class="tabledata"/> 675<td class="tabledata"><i>x</i></td> 676<td class="tabledata"><i>y</i></td> 677<td class="tabledata"><i>z</i></td> 678<td class="tabledata"> 679<i>U</i><sub>iso</sub>*/<i>U</i><sub>eq</sub></td> 680<td class="tabledata"/> 681</tr> 682 683<tr> 684<td class="tabledata">Zr1</td> 685<td class="tabledata">0.67690 (3)</td> 686<td class="tabledata">0.45977 (3)</td> 687<td class="tabledata">0.79870 (3)</td> 688<td class="tabledata">0.03838 (16)</td> 689<td class="tabledata"/> 690</tr> 691 692<tr> 693<td class="tabledata">Cr2</td> 694<td class="tabledata">0.82371 (6)</td> 695<td class="tabledata">0.82936 (6)</td> 696<td class="tabledata">0.79664 (6)</td> 697<td class="tabledata">0.0441 (2)</td> 698<td class="tabledata"/> 699</tr> 700 701<tr> 702<td class="tabledata">Cl1</td> 703<td class="tabledata">0.51592 (14)</td> 704<td class="tabledata">0.56328 (16)</td> 705<td class="tabledata">0.80604 (18)</td> 706<td class="tabledata">0.1054 (7)</td> 707<td class="tabledata"/> 708</tr> 709 710<tr> 711<td class="tabledata">O1</td> 712<td class="tabledata">0.6062 (3)</td> 713<td class="tabledata">0.7896 (4)</td> 714<td class="tabledata">0.6561 (3)</td> 715<td class="tabledata">0.0785 (12)</td> 716<td class="tabledata"/> 717</tr> 718 719<tr> 720<td class="tabledata">O2</td> 721<td class="tabledata">0.7878 (4)</td> 722<td class="tabledata">1.0760 (3)</td> 723<td class="tabledata">0.7936 (4)</td> 724<td class="tabledata">0.1005 (16)</td> 725<td class="tabledata"/> 726</tr> 727 728<tr> 729<td class="tabledata">O3</td> 730<td class="tabledata">0.7167 (4)</td> 731<td class="tabledata">0.7914 (4)</td> 732<td class="tabledata">0.9852 (4)</td> 733<td class="tabledata">0.1065 (17)</td> 734<td class="tabledata"/> 735</tr> 736 737<tr> 738<td class="tabledata">O4</td> 739<td class="tabledata">0.9358 (4)</td> 740<td class="tabledata">0.8437 (4)</td> 741<td class="tabledata">0.6086 (4)</td> 742<td class="tabledata">0.0886 (14)</td> 743<td class="tabledata"/> 744</tr> 745 746<tr> 747<td class="tabledata">O5</td> 748<td class="tabledata">1.0309 (4)</td> 749<td class="tabledata">0.8682 (5)</td> 750<td class="tabledata">0.9517 (4)</td> 751<td class="tabledata">0.1162 (19)</td> 752<td class="tabledata"/> 753</tr> 754 755<tr> 756<td class="tabledata">O6</td> 757<td class="tabledata">0.7769 (3)</td> 758<td class="tabledata">0.5916 (3)</td> 759<td class="tabledata">0.8006 (3)</td> 760<td class="tabledata">0.0532 (9)</td> 761<td class="tabledata"/> 762</tr> 763 764<tr> 765<td class="tabledata">C1</td> 766<td class="tabledata">0.6880 (4)</td> 767<td class="tabledata">0.8052 (4)</td> 768<td class="tabledata">0.7069 (4)</td> 769<td class="tabledata">0.0492 (12)</td> 770<td class="tabledata"/> 771</tr> 772 773<tr> 774<td class="tabledata">C2</td> 775<td class="tabledata">0.8007 (5)</td> 776<td class="tabledata">0.9823 (5)</td> 777<td class="tabledata">0.7944 (4)</td> 778<td class="tabledata">0.0631 (15)</td> 779<td class="tabledata"/> 780</tr> 781 782<tr> 783<td class="tabledata">C3</td> 784<td class="tabledata">0.7572 (5)</td> 785<td class="tabledata">0.8072 (5)</td> 786<td class="tabledata">0.9152 (5)</td> 787<td class="tabledata">0.0627 (15)</td> 788<td class="tabledata"/> 789</tr> 790 791<tr> 792<td class="tabledata">C4</td> 793<td class="tabledata">0.8933 (4)</td> 794<td class="tabledata">0.8394 (4)</td> 795<td class="tabledata">0.6786 (5)</td> 796<td class="tabledata">0.0566 (13)</td> 797<td class="tabledata"/> 798</tr> 799 800<tr> 801<td class="tabledata">C5</td> 802<td class="tabledata">0.9534 (5)</td> 803<td class="tabledata">0.8515 (5)</td> 804<td class="tabledata">0.8931 (5)</td> 805<td class="tabledata">0.0689 (16)</td> 806<td class="tabledata"/> 807</tr> 808 809<tr> 810<td class="tabledata">C6</td> 811<td class="tabledata">0.8496 (4)</td> 812<td class="tabledata">0.6625 (4)</td> 813<td class="tabledata">0.7962 (4)</td> 814<td class="tabledata">0.0449 (11)</td> 815<td class="tabledata"/> 816</tr> 817 818<tr> 819<td class="tabledata">C7</td> 820<td class="tabledata">0.9547 (4)</td> 821<td class="tabledata">0.6101 (5)</td> 822<td class="tabledata">0.7899 (6)</td> 823<td class="tabledata">0.086 (2)</td> 824<td class="tabledata"/> 825</tr> 826 827<tr> 828<td class="tabledata">H7A</td> 829<td class="tabledata">1.0080</td> 830<td class="tabledata">0.6678</td> 831<td class="tabledata">0.7871</td> 832<td class="tabledata">0.129*</td> 833<td class="tabledata"/> 834</tr> 835 836<tr> 837<td class="tabledata">H7B</td> 838<td class="tabledata">0.9469</td> 839<td class="tabledata">0.5645</td> 840<td class="tabledata">0.7256</td> 841<td class="tabledata">0.129*</td> 842<td class="tabledata"/> 843</tr> 844 845<tr> 846<td class="tabledata">H7C</td> 847<td class="tabledata">0.9780</td> 848<td class="tabledata">0.5639</td> 849<td class="tabledata">0.8528</td> 850<td class="tabledata">0.129*</td> 851<td class="tabledata"/> 852</tr> 853 854<tr> 855<td class="tabledata">C8</td> 856<td class="tabledata">0.8066 (5)</td> 857<td class="tabledata">0.4232 (6)</td> 858<td class="tabledata">0.9667 (5)</td> 859<td class="tabledata">0.0733 (18)</td> 860<td class="tabledata"/> 861</tr> 862 863<tr> 864<td class="tabledata">H8</td> 865<td class="tabledata">0.8737</td> 866<td class="tabledata">0.4599</td> 867<td class="tabledata">0.9772</td> 868<td class="tabledata">0.088*</td> 869<td class="tabledata"/> 870</tr> 871 872<tr> 873<td class="tabledata">C9</td> 874<td class="tabledata">0.7144 (6)</td> 875<td class="tabledata">0.4611 (5)</td> 876<td class="tabledata">0.9977 (4)</td> 877<td class="tabledata">0.0769 (19)</td> 878<td class="tabledata"/> 879</tr> 880 881<tr> 882<td class="tabledata">H9</td> 883<td class="tabledata">0.7065</td> 884<td class="tabledata">0.5287</td> 885<td class="tabledata">1.0332</td> 886<td class="tabledata">0.092*</td> 887<td class="tabledata"/> 888</tr> 889 890<tr> 891<td class="tabledata">C10</td> 892<td class="tabledata">0.6349 (5)</td> 893<td class="tabledata">0.3814 (6)</td> 894<td class="tabledata">0.9672 (4)</td> 895<td class="tabledata">0.0758 (18)</td> 896<td class="tabledata"/> 897</tr> 898 899<tr> 900<td class="tabledata">H10</td> 901<td class="tabledata">0.5635</td> 902<td class="tabledata">0.3850</td> 903<td class="tabledata">0.9787</td> 904<td class="tabledata">0.091*</td> 905<td class="tabledata"/> 906</tr> 907 908<tr> 909<td class="tabledata">C11</td> 910<td class="tabledata">0.6779 (6)</td> 911<td class="tabledata">0.2982 (5)</td> 912<td class="tabledata">0.9184 (5)</td> 913<td class="tabledata">0.0762 (19)</td> 914<td class="tabledata"/> 915</tr> 916 917<tr> 918<td class="tabledata">H11</td> 919<td class="tabledata">0.6414</td> 920<td class="tabledata">0.2335</td> 921<td class="tabledata">0.8893</td> 922<td class="tabledata">0.091*</td> 923<td class="tabledata"/> 924</tr> 925 926<tr> 927<td class="tabledata">C12</td> 928<td class="tabledata">0.7831 (6)</td> 929<td class="tabledata">0.3228 (5)</td> 930<td class="tabledata">0.9179 (5)</td> 931<td class="tabledata">0.0711 (17)</td> 932<td class="tabledata"/> 933</tr> 934 935<tr> 936<td class="tabledata">H12</td> 937<td class="tabledata">0.8315</td> 938<td class="tabledata">0.2779</td> 939<td class="tabledata">0.8887</td> 940<td class="tabledata">0.085*</td> 941<td class="tabledata"/> 942</tr> 943 944<tr> 945<td class="tabledata">C13</td> 946<td class="tabledata">0.7269 (6)</td> 947<td class="tabledata">0.4442 (6)</td> 948<td class="tabledata">0.6179 (5)</td> 949<td class="tabledata">0.081 (2)</td> 950<td class="tabledata"/> 951</tr> 952 953<tr> 954<td class="tabledata">H13</td> 955<td class="tabledata">0.7843</td> 956<td class="tabledata">0.4867</td> 957<td class="tabledata">0.6012</td> 958<td class="tabledata">0.097*</td> 959<td class="tabledata"/> 960</tr> 961 962<tr> 963<td class="tabledata">C14</td> 964<td class="tabledata">0.6228 (6)</td> 965<td class="tabledata">0.4758 (6)</td> 966<td class="tabledata">0.6006 (5)</td> 967<td class="tabledata">0.084 (2)</td> 968<td class="tabledata"/> 969</tr> 970 971<tr> 972<td class="tabledata">H14</td> 973<td class="tabledata">0.5943</td> 974<td class="tabledata">0.5445</td> 975<td class="tabledata">0.5727</td> 976<td class="tabledata">0.100*</td> 977<td class="tabledata"/> 978</tr> 979 980<tr> 981<td class="tabledata">C15</td> 982<td class="tabledata">0.5653 (7)</td> 983<td class="tabledata">0.3857 (10)</td> 984<td class="tabledata">0.6326 (6)</td> 985<td class="tabledata">0.119 (3)</td> 986<td class="tabledata"/> 987</tr> 988 989<tr> 990<td class="tabledata">H15</td> 991<td class="tabledata">0.4901</td> 992<td class="tabledata">0.3814</td> 993<td class="tabledata">0.6282</td> 994<td class="tabledata">0.142*</td> 995<td class="tabledata"/> 996</tr> 997 998<tr> 999<td class="tabledata">C16</td> 1000<td class="tabledata">0.6386 (11)</td> 1001<td class="tabledata">0.3060 (7)</td> 1002<td class="tabledata">0.6711 (6)</td> 1003<td class="tabledata">0.124 (4)</td> 1004<td class="tabledata"/> 1005</tr> 1006 1007<tr> 1008<td class="tabledata">H16</td> 1009<td class="tabledata">0.6228</td> 1010<td class="tabledata">0.2365</td> 1011<td class="tabledata">0.6989</td> 1012<td class="tabledata">0.149*</td> 1013<td class="tabledata"/> 1014</tr> 1015 1016<tr> 1017<td class="tabledata">C17</td> 1018<td class="tabledata">0.7361 (9)</td> 1019<td class="tabledata">0.3420 (7)</td> 1020<td class="tabledata">0.6632 (5)</td> 1021<td class="tabledata">0.106 (3)</td> 1022<td class="tabledata"/> 1023</tr> 1024 1025<tr> 1026<td class="tabledata">H17</td> 1027<td class="tabledata">0.8011</td> 1028<td class="tabledata">0.3027</td> 1029<td class="tabledata">0.6854</td> 1030<td class="tabledata">0.127*</td> 1031<td class="tabledata"/> 1032</tr> 1033</table> 1034</div> 1035 1036<!-- endtablewrapcoordsdiv --> 1037<div class="tablewrapadps"><a id="atomicdisplacement1" name="atomicdisplacement1"/> <span class="heading3">Atomic 1038displacement parameters (�<sup>2</sup>)</span> 1039<!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span><!-- endtoplinkspan --> 1040<table style="table-layout:fixed" width="100%" summary="" class="tabledata"> 1041<tr> 1042<td class="tabledata"/> 1043<td class="tabledata"><i>U</i><sup>11</sup></td> 1044<td class="tabledata"><i>U</i><sup>22</sup></td> 1045<td class="tabledata"><i>U</i><sup>33</sup></td> 1046<td class="tabledata"><i>U</i><sup>12</sup></td> 1047<td class="tabledata"><i>U</i><sup>13</sup></td> 1048<td class="tabledata"><i>U</i><sup>23</sup></td> 1049</tr> 1050 1051<tr> 1052<td class="tabledata">Zr1</td> 1053<td class="tabledata">0.0412 (3)</td> 1054<td class="tabledata">0.0306 (2)</td> 1055<td class="tabledata">0.0410 (3)</td> 1056<td class="tabledata"><span style="font-family:Times">?</span>0.0002 (2)</td> 1057<td class="tabledata">0.00175 (18)</td> 1058<td class="tabledata">0.0023 (2)</td> 1059</tr> 1060 1061<tr> 1062<td class="tabledata">Cr2</td> 1063<td class="tabledata">0.0464 (5)</td> 1064<td class="tabledata">0.0299 (4)</td> 1065<td class="tabledata">0.0544 (5)</td> 1066<td class="tabledata">0.0011 (3)</td> 1067<td class="tabledata">0.0054 (4)</td> 1068<td class="tabledata">0.0004 (3)</td> 1069</tr> 1070 1071<tr> 1072<td class="tabledata">Cl1</td> 1073<td class="tabledata">0.0717 (11)</td> 1074<td class="tabledata">0.0871 (13)</td> 1075<td class="tabledata">0.1666 (19)</td> 1076<td class="tabledata">0.0361 (10)</td> 1077<td class="tabledata">0.0464 (12)</td> 1078<td class="tabledata">0.0408 (12)</td> 1079</tr> 1080 1081<tr> 1082<td class="tabledata">O1</td> 1083<td class="tabledata">0.048 (2)</td> 1084<td class="tabledata">0.097 (3)</td> 1085<td class="tabledata">0.084 (3)</td> 1086<td class="tabledata">0.002 (2)</td> 1087<td class="tabledata"><span style="font-family:Times">?</span>0.005 (2)</td> 1088<td class="tabledata">0.002 (2)</td> 1089</tr> 1090 1091<tr> 1092<td class="tabledata">O2</td> 1093<td class="tabledata">0.121 (4)</td> 1094<td class="tabledata">0.035 (2)</td> 1095<td class="tabledata">0.140 (4)</td> 1096<td class="tabledata">0.013 (2)</td> 1097<td class="tabledata">0.013 (3)</td> 1098<td class="tabledata"><span style="font-family:Times">?</span>0.005 (2)</td> 1099</tr> 1100 1101<tr> 1102<td class="tabledata">O3</td> 1103<td class="tabledata">0.134 (5)</td> 1104<td class="tabledata">0.122 (4)</td> 1105<td class="tabledata">0.076 (3)</td> 1106<td class="tabledata">0.023 (4)</td> 1107<td class="tabledata">0.053 (3)</td> 1108<td class="tabledata">0.009 (3)</td> 1109</tr> 1110 1111<tr> 1112<td class="tabledata">O4</td> 1113<td class="tabledata">0.086 (3)</td> 1114<td class="tabledata">0.096 (3)</td> 1115<td class="tabledata">0.094 (3)</td> 1116<td class="tabledata"><span style="font-family:Times">?</span>0.016 (3)</td> 1117<td class="tabledata">0.042 (3)</td> 1118<td class="tabledata"><span style="font-family:Times">?</span>0.007 (3)</td> 1119</tr> 1120 1121<tr> 1122<td class="tabledata">O5</td> 1123<td class="tabledata">0.077 (3)</td> 1124<td class="tabledata">0.118 (4)</td> 1125<td class="tabledata">0.132 (4)</td> 1126<td class="tabledata"><span style="font-family:Times">?</span>0.015 (3)</td> 1127<td class="tabledata"><span style="font-family:Times">?</span>0.033 (3)</td> 1128<td class="tabledata"><span style="font-family:Times">?</span>0.002 (4)</td> 1129</tr> 1130 1131<tr> 1132<td class="tabledata">O6</td> 1133<td class="tabledata">0.052 (2)</td> 1134<td class="tabledata">0.0333 (18)</td> 1135<td class="tabledata">0.073 (2)</td> 1136<td class="tabledata"><span style="font-family:Times">?</span>0.0062 (16)</td> 1137<td class="tabledata">0.0079 (17)</td> 1138<td class="tabledata"><span style="font-family:Times">?</span>0.0001 (16)</td> 1139</tr> 1140 1141<tr> 1142<td class="tabledata">C1</td> 1143<td class="tabledata">0.058 (3)</td> 1144<td class="tabledata">0.039 (3)</td> 1145<td class="tabledata">0.054 (3)</td> 1146<td class="tabledata">0.008 (2)</td> 1147<td class="tabledata">0.018 (3)</td> 1148<td class="tabledata">0.005 (2)</td> 1149</tr> 1150 1151<tr> 1152<td class="tabledata">C2</td> 1153<td class="tabledata">0.074 (4)</td> 1154<td class="tabledata">0.041 (3)</td> 1155<td class="tabledata">0.071 (4)</td> 1156<td class="tabledata">0.004 (3)</td> 1157<td class="tabledata">0.007 (3)</td> 1158<td class="tabledata"><span style="font-family:Times">?</span>0.003 (3)</td> 1159</tr> 1160 1161<tr> 1162<td class="tabledata">C3</td> 1163<td class="tabledata">0.076 (4)</td> 1164<td class="tabledata">0.055 (3)</td> 1165<td class="tabledata">0.057 (3)</td> 1166<td class="tabledata">0.008 (3)</td> 1167<td class="tabledata">0.010 (3)</td> 1168<td class="tabledata"><span style="font-family:Times">?</span>0.005 (3)</td> 1169</tr> 1170 1171<tr> 1172<td class="tabledata">C4</td> 1173<td class="tabledata">0.054 (3)</td> 1174<td class="tabledata">0.045 (3)</td> 1175<td class="tabledata">0.071 (4)</td> 1176<td class="tabledata"><span style="font-family:Times">?</span>0.008 (3)</td> 1177<td class="tabledata">0.014 (3)</td> 1178<td class="tabledata">0.000 (3)</td> 1179</tr> 1180 1181<tr> 1182<td class="tabledata">C5</td> 1183<td class="tabledata">0.061 (4)</td> 1184<td class="tabledata">0.052 (3)</td> 1185<td class="tabledata">0.088 (4)</td> 1186<td class="tabledata"><span style="font-family:Times">?</span>0.007 (3)</td> 1187<td class="tabledata"><span style="font-family:Times">?</span>0.002 (3)</td> 1188<td class="tabledata"><span style="font-family:Times">?</span>0.003 (3)</td> 1189</tr> 1190 1191<tr> 1192<td class="tabledata">C6</td> 1193<td class="tabledata">0.044 (3)</td> 1194<td class="tabledata">0.036 (3)</td> 1195<td class="tabledata">0.052 (3)</td> 1196<td class="tabledata">0.000 (2)</td> 1197<td class="tabledata">0.003 (2)</td> 1198<td class="tabledata">0.002 (2)</td> 1199</tr> 1200 1201<tr> 1202<td class="tabledata">C7</td> 1203<td class="tabledata">0.048 (3)</td> 1204<td class="tabledata">0.049 (3)</td> 1205<td class="tabledata">0.160 (7)</td> 1206<td class="tabledata">0.008 (3)</td> 1207<td class="tabledata">0.016 (4)</td> 1208<td class="tabledata">0.004 (4)</td> 1209</tr> 1210 1211<tr> 1212<td class="tabledata">C8</td> 1213<td class="tabledata">0.073 (4)</td> 1214<td class="tabledata">0.076 (4)</td> 1215<td class="tabledata">0.058 (4)</td> 1216<td class="tabledata"><span style="font-family:Times">?</span>0.007 (4)</td> 1217<td class="tabledata"><span style="font-family:Times">?</span>0.020 (3)</td> 1218<td class="tabledata">0.016 (3)</td> 1219</tr> 1220 1221<tr> 1222<td class="tabledata">C9</td> 1223<td class="tabledata">0.115 (6)</td> 1224<td class="tabledata">0.071 (4)</td> 1225<td class="tabledata">0.041 (3)</td> 1226<td class="tabledata">0.015 (4)</td> 1227<td class="tabledata">0.004 (3)</td> 1228<td class="tabledata"><span style="font-family:Times">?</span>0.011 (3)</td> 1229</tr> 1230 1231<tr> 1232<td class="tabledata">C10</td> 1233<td class="tabledata">0.083 (5)</td> 1234<td class="tabledata">0.099 (5)</td> 1235<td class="tabledata">0.047 (3)</td> 1236<td class="tabledata"><span style="font-family:Times">?</span>0.006 (4)</td> 1237<td class="tabledata">0.019 (3)</td> 1238<td class="tabledata">0.015 (3)</td> 1239</tr> 1240 1241<tr> 1242<td class="tabledata">C11</td> 1243<td class="tabledata">0.124 (6)</td> 1244<td class="tabledata">0.049 (3)</td> 1245<td class="tabledata">0.050 (4)</td> 1246<td class="tabledata"><span style="font-family:Times">?</span>0.013 (4)</td> 1247<td class="tabledata">0.002 (4)</td> 1248<td class="tabledata">0.014 (3)</td> 1249</tr> 1250 1251<tr> 1252<td class="tabledata">C12</td> 1253<td class="tabledata">0.084 (5)</td> 1254<td class="tabledata">0.065 (4)</td> 1255<td class="tabledata">0.061 (4)</td> 1256<td class="tabledata">0.026 (4)</td> 1257<td class="tabledata">0.005 (3)</td> 1258<td class="tabledata">0.020 (3)</td> 1259</tr> 1260 1261<tr> 1262<td class="tabledata">C13</td> 1263<td class="tabledata">0.104 (6)</td> 1264<td class="tabledata">0.093 (5)</td> 1265<td class="tabledata">0.048 (3)</td> 1266<td class="tabledata"><span style="font-family:Times">?</span>0.021 (4)</td> 1267<td class="tabledata">0.019 (4)</td> 1268<td class="tabledata"><span style="font-family:Times">?</span>0.003 (3)</td> 1269</tr> 1270 1271<tr> 1272<td class="tabledata">C14</td> 1273<td class="tabledata">0.100 (5)</td> 1274<td class="tabledata">0.094 (5)</td> 1275<td class="tabledata">0.048 (3)</td> 1276<td class="tabledata"><span style="font-family:Times">?</span>0.010 (5)</td> 1277<td class="tabledata"><span style="font-family:Times">?</span>0.007 (3)</td> 1278<td class="tabledata">0.023 (3)</td> 1279</tr> 1280 1281<tr> 1282<td class="tabledata">C15</td> 1283<td class="tabledata">0.104 (6)</td> 1284<td class="tabledata">0.185 (10)</td> 1285<td class="tabledata">0.053 (4)</td> 1286<td class="tabledata"><span style="font-family:Times">?</span>0.072 (7)</td> 1287<td class="tabledata"><span style="font-family:Times">?</span>0.021 (4)</td> 1288<td class="tabledata"><span style="font-family:Times">?</span>0.008 (5)</td> 1289</tr> 1290 1291<tr> 1292<td class="tabledata">C16</td> 1293<td class="tabledata">0.232 (12)</td> 1294<td class="tabledata">0.088 (6)</td> 1295<td class="tabledata">0.047 (4)</td> 1296<td class="tabledata"><span style="font-family:Times">?</span>0.088 (8)</td> 1297<td class="tabledata">0.009 (6)</td> 1298<td class="tabledata"><span style="font-family:Times">?</span>0.022 (4)</td> 1299</tr> 1300 1301<tr> 1302<td class="tabledata">C17</td> 1303<td class="tabledata">0.188 (10)</td> 1304<td class="tabledata">0.076 (5)</td> 1305<td class="tabledata">0.058 (4)</td> 1306<td class="tabledata">0.042 (6)</td> 1307<td class="tabledata">0.032 (5)</td> 1308<td class="tabledata"><span style="font-family:Times">?</span>0.012 (4)</td> 1309</tr> 1310</table> 1311</div> 1312 1313<!-- endtablewrapadpsdiv --> 1314<div class="tablewrapgeomlong"><a id="geometricparameters1" name="geometricparameters1"/> <span class="heading3">Geometric 1315parameters (�, �)</span><!-- endheading3span --> <span class="toplink"><a class="buttons" href="#top">top</a></span> 1316<!-- endtoplinkspan --><!-- startgeom --> 1317<table style="table-layout:fixed" width="100%" summary="" class="tabledata"> 1318<colgroup span="4"> 1319<col width="30%"/> 1320<col width="20%"/> 1321<col width="30%"/> 1322<col width="20%"/></colgroup> 1323 1324<tr> 1325<td width="30%" class="tabledata">Zr1-O6</td> 1326<td width="20%" class="tabledata">2.041�(3)</td> 1327<td width="30%" class="tabledata">C6-C7</td> 1328<td width="20%" class="tabledata">1.498�(7)</td> 1329</tr> 1330 1331<tr> 1332<td width="30%" class="tabledata">Zr1-Cl1</td> 1333<td width="20%" class="tabledata">2.4205�(16)</td> 1334<td width="30%" class="tabledata">C7-H7A</td> 1335<td width="20%" class="tabledata">0.9800</td> 1336</tr> 1337 1338<tr> 1339<td width="30%" class="tabledata">Zr1-C16</td> 1340<td width="20%" class="tabledata">2.463�(7)</td> 1341<td width="30%" class="tabledata">C7-H7B</td> 1342<td width="20%" class="tabledata">0.9800</td> 1343</tr> 1344 1345<tr> 1346<td width="30%" class="tabledata">Zr1-C17</td> 1347<td width="20%" class="tabledata">2.470�(6)</td> 1348<td width="30%" class="tabledata">C7-H7C</td> 1349<td width="20%" class="tabledata">0.9800</td> 1350</tr> 1351 1352<tr> 1353<td width="30%" class="tabledata">Zr1-C12</td> 1354<td width="20%" class="tabledata">2.476�(5)</td> 1355<td width="30%" class="tabledata">C8-C12</td> 1356<td width="20%" class="tabledata">1.373�(8)</td> 1357</tr> 1358 1359<tr> 1360<td width="30%" class="tabledata">Zr1-C11</td> 1361<td width="20%" class="tabledata">2.483�(5)</td> 1362<td width="30%" class="tabledata">C8-C9</td> 1363<td width="20%" class="tabledata">1.387�(9)</td> 1364</tr> 1365 1366<tr> 1367<td width="30%" class="tabledata">Zr1-C15</td> 1368<td width="20%" class="tabledata">2.490�(6)</td> 1369<td width="30%" class="tabledata">C8-H8</td> 1370<td width="20%" class="tabledata">0.9500</td> 1371</tr> 1372 1373<tr> 1374<td width="30%" class="tabledata">Zr1-C8</td> 1375<td width="20%" class="tabledata">2.492�(5)</td> 1376<td width="30%" class="tabledata">C9-C10</td> 1377<td width="20%" class="tabledata">1.400�(9)</td> 1378</tr> 1379 1380<tr> 1381<td width="30%" class="tabledata">Zr1-C9</td> 1382<td width="20%" class="tabledata">2.500�(5)</td> 1383<td width="30%" class="tabledata">C9-H9</td> 1384<td width="20%" class="tabledata">0.9500</td> 1385</tr> 1386 1387<tr> 1388<td width="30%" class="tabledata">Zr1-C10</td> 1389<td width="20%" class="tabledata">2.503�(5)</td> 1390<td width="30%" class="tabledata">C10-C11</td> 1391<td width="20%" class="tabledata">1.354�(9)</td> 1392</tr> 1393 1394<tr> 1395<td width="30%" class="tabledata">Zr1-C14</td> 1396<td width="20%" class="tabledata">2.504�(6)</td> 1397<td width="30%" class="tabledata">C10-H10</td> 1398<td width="20%" class="tabledata">0.9500</td> 1399</tr> 1400 1401<tr> 1402<td width="30%" class="tabledata">Zr1-C13</td> 1403<td width="20%" class="tabledata">2.517�(6)</td> 1404<td width="30%" class="tabledata">C11-C12</td> 1405<td width="20%" class="tabledata">1.374�(9)</td> 1406</tr> 1407 1408<tr> 1409<td width="30%" class="tabledata">Cr2-C2</td> 1410<td width="20%" class="tabledata">1.875�(6)</td> 1411<td width="30%" class="tabledata">C11-H11</td> 1412<td width="20%" class="tabledata">0.9500</td> 1413</tr> 1414 1415<tr> 1416<td width="30%" class="tabledata">Cr2-C5</td> 1417<td width="20%" class="tabledata">1.885�(6)</td> 1418<td width="30%" class="tabledata">C12-H12</td> 1419<td width="20%" class="tabledata">0.9500</td> 1420</tr> 1421 1422<tr> 1423<td width="30%" class="tabledata">Cr2-C3</td> 1424<td width="20%" class="tabledata">1.889�(6)</td> 1425<td width="30%" class="tabledata">C13-C14</td> 1426<td width="20%" class="tabledata">1.358�(9)</td> 1427</tr> 1428 1429<tr> 1430<td width="30%" class="tabledata">Cr2-C4</td> 1431<td width="20%" class="tabledata">1.892�(6)</td> 1432<td width="30%" class="tabledata">C13-C17</td> 1433<td width="20%" class="tabledata">1.362�(9)</td> 1434</tr> 1435 1436<tr> 1437<td width="30%" class="tabledata">Cr2-C1</td> 1438<td width="20%" class="tabledata">1.910�(6)</td> 1439<td width="30%" class="tabledata">C13-H13</td> 1440<td width="20%" cl…
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