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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Poly[[bis[μ-1,4-bis(3-pyridylmethyl)piperazine-κ<sup>2</sup><italic>N</italic>:<italic>N</italic>′]dichloridocadmium(II)] tetrahydrate]</title><author><name sortKey="Blake, Karyn M" sort="Blake, Karyn M" uniqKey="Blake K" first="Karyn M." last="Blake">Karyn M. Blake</name><affiliation><nlm:aff id="a">Lyman Briggs College, Department of Chemistry, Michigan State University, East Lansing, MI 48825,<country>USA</country></nlm:aff></affiliation></author><author><name sortKey="Laduca, Robert L" sort="Laduca, Robert L" uniqKey="Laduca R" first="Robert L." last="Laduca">Robert L. Laduca</name><affiliation><nlm:aff id="a">Lyman Briggs College, Department of Chemistry, Michigan State University, East Lansing, MI 48825,<country>USA</country></nlm:aff></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">PMC</idno><idno type="pmid">21583397</idno><idno type="pmc">2977128</idno><idno type="url">http://www.ncbi.nlm.nih.gov/pmc/articles/PMC2977128</idno><idno type="RBID">PMC:2977128</idno><idno type="doi">10.1107/S1600536809027767</idno><date when="2009">2009</date><idno type="wicri:Area/Pmc/Corpus">000A14</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Corpus" wicri:corpus="PMC">000A14</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en" level="a" type="main">Poly[[bis[μ-1,4-bis(3-pyridylmethyl)piperazine-κ<sup>2</sup><italic>N</italic>:<italic>N</italic>′]dichloridocadmium(II)] tetrahydrate]</title><author><name sortKey="Blake, Karyn M" sort="Blake, Karyn M" uniqKey="Blake K" first="Karyn M." last="Blake">Karyn M. Blake</name><affiliation><nlm:aff id="a">Lyman Briggs College, Department of Chemistry, Michigan State University, East Lansing, MI 48825,<country>USA</country></nlm:aff></affiliation></author><author><name sortKey="Laduca, Robert L" sort="Laduca, Robert L" uniqKey="Laduca R" first="Robert L." last="Laduca">Robert L. Laduca</name><affiliation><nlm:aff id="a">Lyman Briggs College, Department of Chemistry, Michigan State University, East Lansing, MI 48825,<country>USA</country></nlm:aff></affiliation></author></analytic><series><title level="j">Acta Crystallographica Section E: Structure Reports Online</title><idno type="eISSN">1600-5368</idno><imprint><date when="2009">2009</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en"><p>In the title compound, {[CdCl<sub>2</sub>(C<sub>16</sub>H<sub>20</sub>N<sub>4</sub>)<sub>2</sub>]·4H<sub>2</sub>O}<sub><italic>n</italic></sub>, octahedrally coordinated Cd<sup>II</sup> ions, situated on crystallographic inversion centres, bearing <italic>trans</italic>-disposed chloride ligands, are linked into (4,4)-grid coordination polymer layers by tethering 1,4-bis(3-pyridylmethyl)piperazine ligands. The layers are aligned parallel to the (<inline-formula><inline-graphic xlink:href="e-65-0m947-efi7.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula>01) crystal planes and aggregate by means of O—H⋯N, O—H⋯O and O—H⋯Cl hydrogen-bonding mechanisms imparted by cyclic water molecule tetramers.</p></div></front><back><div1 type="bibliography"><listBibl><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct></listBibl></div1></back></TEI><pmc article-type="research-article"><pmc-dir>properties open_access</pmc-dir>
<front><journal-meta><journal-id journal-id-type="nlm-ta">Acta Crystallogr Sect E Struct Rep Online</journal-id><journal-id journal-id-type="publisher-id">Acta Cryst. E</journal-id><journal-title-group><journal-title>Acta Crystallographica Section E: Structure Reports Online</journal-title></journal-title-group><issn pub-type="epub">1600-5368</issn><publisher><publisher-name>International Union of Crystallography</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="pmid">21583397</article-id><article-id pub-id-type="pmc">2977128</article-id><article-id pub-id-type="publisher-id">lh2863</article-id><article-id pub-id-type="doi">10.1107/S1600536809027767</article-id><article-id pub-id-type="coden">ACSEBH</article-id><article-id pub-id-type="pii">S1600536809027767</article-id><article-categories><subj-group subj-group-type="heading"><subject>Metal-Organic Papers</subject></subj-group></article-categories><title-group><article-title>Poly[[bis[μ-1,4-bis(3-pyridylmethyl)piperazine-κ<sup>2</sup><italic>N</italic>:<italic>N</italic>′]dichloridocadmium(II)] tetrahydrate]</article-title><alt-title><italic>[CdCl<sub>2</sub>(C<sub>16</sub>H<sub>20</sub>N<sub>4</sub>)<sub>2</sub>]·4H<sub>2</sub>O</italic></alt-title></title-group><contrib-group><contrib contrib-type="author"><name><surname>Blake</surname><given-names>Karyn M.</given-names></name><xref ref-type="aff" rid="a">a</xref></contrib><contrib contrib-type="author"><name><surname>LaDuca</surname><given-names>Robert L.</given-names></name><xref ref-type="aff" rid="a">a</xref><xref ref-type="corresp" rid="cor">*</xref></contrib><aff id="a"><label>a</label>Lyman Briggs College, Department of Chemistry, Michigan State University, East Lansing, MI 48825,<country>USA</country></aff></contrib-group><author-notes><corresp id="cor">Correspondence e-mail: <email>laduca@msu.edu</email></corresp></author-notes><pub-date pub-type="collection"><day>01</day><month>8</month><year>2009</year></pub-date><pub-date pub-type="epub"><day>18</day><month>7</month><year>2009</year></pub-date><pub-date pub-type="pmc-release"><day>18</day><month>7</month><year>2009</year></pub-date><pmc-comment> PMC Release delay is 0 months and 0 days and was based on the
<volume>65</volume><issue>Pt 8</issue><issue-id pub-id-type="publisher-id">e090800</issue-id><fpage>m947</fpage><lpage>m947</lpage><history><date date-type="received"><day>10</day><month>7</month><year>2009</year></date><date date-type="accepted"><day>14</day><month>7</month><year>2009</year></date></history><permissions><copyright-statement>© Blake and LaDuca 2009</copyright-statement><copyright-year>2009</copyright-year><license license-type="open-access" xlink:href="http://creativecommons.org/licenses/by/2.0/uk/"><license-p>This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.</license-p></license></permissions><self-uri xlink:type="simple" xlink:href="http://dx.doi.org/10.1107/S1600536809027767">A full version of this article is available from Crystallography Journals Online.</self-uri><abstract><p>In the title compound, {[CdCl<sub>2</sub>(C<sub>16</sub>H<sub>20</sub>N<sub>4</sub>)<sub>2</sub>]·4H<sub>2</sub>O}<sub><italic>n</italic></sub>, octahedrally coordinated Cd<sup>II</sup> ions, situated on crystallographic inversion centres, bearing <italic>trans</italic>-disposed chloride ligands, are linked into (4,4)-grid coordination polymer layers by tethering 1,4-bis(3-pyridylmethyl)piperazine ligands. The layers are aligned parallel to the (<inline-formula><inline-graphic xlink:href="e-65-0m947-efi7.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula>01) crystal planes and aggregate by means of O—H⋯N, O—H⋯O and O—H⋯Cl hydrogen-bonding mechanisms imparted by cyclic water molecule tetramers.</p></abstract></article-meta></front><body><sec id="sec1"><title>Related literature</title><p>For a cadmium succinate coordination polymer containing <italic>N,N′</italic>-bis(4-pyridylmethyl)piperazine, see: Martin <italic>et al.</italic> (2009<xref ref-type="bibr" rid="bb2"> ▶</xref>). For the preparation of <italic>N,N′</italic>-bis(3-pyridylmethyl)piperazine, see: Pocic <italic>et al.</italic> (2005<xref ref-type="bibr" rid="bb4"> ▶</xref>).<chem-struct id="scheme1"><graphic xlink:href="e-65-0m947-scheme1.jpg" position="float"></graphic></chem-struct></p></sec><sec sec-type="" id="sec2"><title>Experimental</title><sec id="sec2.1"><title></title><sec id="sec2.1.1"><title>Crystal data</title><p><list list-type="simple"><list-item><p>[CdCl<sub>2</sub>(C<sub>16</sub>H<sub>20</sub>N<sub>4</sub>)<sub>2</sub>]·4H<sub>2</sub>O</p></list-item><list-item><p><italic>M</italic><italic><sub>r</sub></italic> = 792.08</p></list-item><list-item><p>Monoclinic, <inline-formula><inline-graphic xlink:href="e-65-0m947-efi8.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula></p></list-item><list-item><p><italic>a</italic> = 10.3481 (2) Å</p></list-item><list-item><p><italic>b</italic> = 13.9791 (2) Å</p></list-item><list-item><p><italic>c</italic> = 12.7789 (2) Å</p></list-item><list-item><p>β = 92.4730 (10)°</p></list-item><list-item><p><italic>V</italic> = 1846.84 (5) Å<sup>3</sup></p></list-item><list-item><p><italic>Z</italic> = 2</p></list-item><list-item><p>Mo <italic>K</italic>α radiation</p></list-item><list-item><p>μ = 0.78 mm<sup>−1</sup></p></list-item><list-item><p><italic>T</italic> = 173 K</p></list-item><list-item><p>0.38 × 0.35 × 0.19 mm</p></list-item></list></p></sec><sec id="sec2.1.2"><title>Data collection</title><p><list list-type="simple"><list-item><p>Bruker APEXII diffractometer</p></list-item><list-item><p>Absorption correction: multi-scan (<italic>SADABS</italic>; Sheldrick, 1996<xref ref-type="bibr" rid="bb5"> ▶</xref>) <italic>T</italic><sub>min</sub> = 0.753, <italic>T</italic><sub>max</sub> = 0.868</p></list-item><list-item><p>16443 measured reflections</p></list-item><list-item><p>3391 independent reflections</p></list-item><list-item><p>3060 reflections with <italic>I</italic> > 2σ(<italic>I</italic>)</p></list-item><list-item><p><italic>R</italic><sub>int</sub> = 0.027</p></list-item></list></p></sec><sec id="sec2.1.3"><title>Refinement</title><p><list list-type="simple"><list-item><p><italic>R</italic>[<italic>F</italic><sup>2</sup> > 2σ(<italic>F</italic><sup>2</sup>)] = 0.021</p></list-item><list-item><p><italic>wR</italic>(<italic>F</italic><sup>2</sup>) = 0.055</p></list-item><list-item><p><italic>S</italic> = 1.07</p></list-item><list-item><p>3391 reflections</p></list-item><list-item><p>226 parameters</p></list-item><list-item><p>6 restraints</p></list-item><list-item><p>H atoms treated by a mixture of independent and constrained refinement</p></list-item><list-item><p>Δρ<sub>max</sub> = 0.42 e Å<sup>−3</sup></p></list-item><list-item><p>Δρ<sub>min</sub> = −0.23 e Å<sup>−3</sup></p></list-item></list></p></sec></sec><sec id="d5e555"><title></title><p>Data collection: <italic>APEX2</italic> (Bruker, 2006<xref ref-type="bibr" rid="bb1"> ▶</xref>); cell refinement: <italic>SAINT</italic> (Bruker, 2006<xref ref-type="bibr" rid="bb1"> ▶</xref>); data reduction: <italic>SAINT</italic>; program(s) used to solve structure: <italic>SHELXS97</italic> (Sheldrick, 2008<xref ref-type="bibr" rid="bb6"> ▶</xref>); program(s) used to refine structure: <italic>SHELXL97</italic> (Sheldrick, 2008<xref ref-type="bibr" rid="bb6"> ▶</xref>); molecular graphics: <italic>CrystalMaker</italic> (Palmer, 2007<xref ref-type="bibr" rid="bb3"> ▶</xref>); software used to prepare material for publication: <italic>SHELXL97</italic>.</p></sec></sec><sec sec-type="supplementary-material"><title>Supplementary Material</title><supplementary-material content-type="local-data" xlink:href="e-65-0m947-sup1.cif" position="float" xlink:type="simple"><p>Crystal structure: contains datablocks I, global. DOI: <ext-link ext-link-type="uri" xlink:type="simple" xlink:href="http://dx.doi.org/10.1107/S1600536809027767/lh2863sup1.cif">10.1107/S1600536809027767/lh2863sup1.cif</ext-link></p><media mimetype="chemical" mime-subtype="x-cif" xlink:href="e-65-0m947-sup1.cif" position="float" xlink:type="simple"></media></supplementary-material><supplementary-material content-type="local-data" xlink:href="e-65-0m947-Isup2.hkl" position="float" xlink:type="simple"><p>Structure factors: contains datablocks I. DOI: <ext-link ext-link-type="uri" xlink:type="simple" xlink:href="http://dx.doi.org/10.1107/S1600536809027767/lh2863Isup2.hkl">10.1107/S1600536809027767/lh2863Isup2.hkl</ext-link></p><media mimetype="text" mime-subtype="plain" xlink:href="e-65-0m947-Isup2.hkl" position="float" xlink:type="simple"></media></supplementary-material><supplementary-material position="float" xlink:type="simple"><p>Additional supplementary materials: <ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/sendsupfiles?lh2863&file=lh2863sup0.html&mime=text/html" xlink:type="simple"> crystallographic information</ext-link>; <ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/sendcif?lh2863sup1&Qmime=cif" xlink:type="simple">3D view</ext-link>; <ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/paper?lh2863&checkcif=yes" xlink:type="simple">checkCIF report</ext-link></p></supplementary-material></sec></body><back><fn-group><fn id="fnu1"><p>Supplementary data and figures for this paper are available from the IUCr electronic archives (Reference: <ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/sendsup?lh2863">LH2863</ext-link>).</p></fn></fn-group><ack><p>We gratefully acknowledge the American Chemical Society Petroleum Research Fund for funding this work.</p></ack><app-group><app><title>supplementary crystallographic
information</title><sec id="comment"><title>Comment </title><p>The title compound was prepared during an attempt to prepare a divalent cadmium
coordination polymer containing both succinate and
<italic>N,N'</italic>-di(3-pyridylmethyl)piperazine (3-bpmp) ligands.
A cadmium succinate coordination polymer
containing the isomeric <italic>N,N'</italic>-di(4-pyridylmethyl)piperazine (4-bpmp)
ligand manifested the unique example of a 6<sup>5</sup>8 layered topology (Martin
<italic>et al.</italic>, 2009).</p><p>The asymmetric unit of the title compound (Fig. 1) contains a Cd<sup>II</sup> ion on the
crystallographic inversion centre, one chloro ligand, one 3-bpmp ligand, and
two water molecules of crystallization. Operation of the crystallographic
symmetry generates an octahedral {CdCl<sub>2</sub>N<sub>4</sub>} coordination environment, with
<italic>trans</italic> disposed chloro ligands and four N atom donors from pyridyl
groups of four different 3-bpmp ligands.</p><p>Each Cd<sup>II</sup> ion is linked to four others through the tethering 3-bpmp ligands
to construct (4,4)-grid [CdCl<sub>2</sub>(3-bpmp)<sub>2</sub>]<sub>n</sub> coordination polymer layers
(Fig. 2) that are oriented parallel to the (1 0 1) crystal planes. The
through-ligand Cd···Cd distances measure 10.658 (3) Å. The layers stack in an
<italic>AAA</italic> pattern along the <italic>a</italic> crystal direction <italic>via</italic>hydrogen-bonding mechanisms provided by tetrameric water molecule aggregations
(Fig. 3). Within a single coordination polymer layer, a water molecule (O1W)
engages in O—H···N hydrogen-bonding with a piperazinyl N atom, and in turn
with another water molecule of crystallization (O2W). Then, this second water
molecule of crystallization provides O—H···Cl hydrogen-bonding to a chloro
ligand. The water molecules of crystallization engage in mutual O—H···O
hydrogen-bonding across the interlamellar regions to construct the cyclic
water molecule tetramers.</p></sec><sec id="experimental"><title>Experimental </title><p>Cadmium chloride dihydrate and succinic acid were obtained commercially.
<italic>N,N'</italic>-bis(3-pyridylmethyl)piperazine was prepared <italic>via</italic> a published
procedure (Pocic, <italic>et al.</italic>, 2005). A mixture of cadmium chloride
dihydrate (81 mg, 0.37 mmol), succinic acid (44 mg, 0.37 mmol),
<italic>N,N'</italic>-bis(3-pyridylmethyl)piperazine (99 mg, 0.37 mmol) and 10.0 g water
(550 mmol) was placed into a 23 ml Teflon-lined Parr Acid Digestion bomb,
which was then heated under autogenous pressure at 393 K for 48 h. The
resulting yellowish solution was allowed to stand undisturbed at 293 K for 3 d. Large straw-colored crystals of the title compound were deposited.</p></sec><sec id="refinement"><title>Refinement </title><p>All H atoms bound to C atoms were placed in calculated positions, with C—H =
0.95 Å and refined in riding mode with <italic>U</italic><sub>iso</sub> = 1.2<italic>U</italic><sub>eq</sub>(C).
The H atoms bound to water molecule O atoms were found in a difference Fourier
map, restrained with O—H = 0.89 Å, and refined with <italic>U</italic><sub>iso</sub> =
1.2<italic>U</italic><sub>eq</sub>(O).</p></sec><sec id="figures"><title>Figures</title><fig id="Fap1"><label>Fig. 1.</label><caption><p>The expanded asymmetric unit of the title compound, showing 50% probability ellipsoids and atom numbering scheme. Hydrogen atom positions are shown as grey sticks. Color codes: violet Cd, green Cl, N blue, orange O, black C. Symmetry codes: (i) x+1/2, -y+3/2, z+1/2 (ii) -x-1/2, y-1/2, -z+1/2 (iii) -x, -y+1, -z+1.</p></caption><graphic xlink:href="e-65-0m947-fig1"></graphic></fig><fig id="Fap2"><label>Fig. 2.</label><caption><p>A view of the (4,4)-grid coordination polymer layer in the title compound.</p></caption><graphic xlink:href="e-65-0m947-fig2"></graphic></fig><fig id="Fap3"><label>Fig. 3.</label><caption><p>Stacking diagram of the title compound, viewed along the b crystal direction. Water molecule tetramers can be seen in the interlamellar regions.</p></caption><graphic xlink:href="e-65-0m947-fig3"></graphic></fig></sec><sec id="tablewrapcrystaldatalong"><title>Crystal data</title><table-wrap position="anchor" id="d1e191"><table rules="all" frame="box" style="table-layout:fixed" summary=""><colgroup span="2"><col span="1"></col><col span="1"></col></colgroup><tr><td rowspan="1" colspan="1">[CdCl<sub>2</sub>(C<sub>16</sub>H<sub>20</sub>N<sub>4</sub>)<sub>2</sub>]·4H<sub>2</sub>O</td><td rowspan="1" colspan="1"><italic>F</italic>(000) = 820</td></tr><tr><td rowspan="1" colspan="1"><italic>M</italic><italic><sub>r</sub></italic> = 792.08</td><td rowspan="1" colspan="1"><italic>D</italic><sub>x</sub> = 1.424 Mg m<sup>−</sup><sup>3</sup></td></tr><tr><td rowspan="1" colspan="1">Monoclinic, <italic>P</italic>2<sub>1</sub>/<italic>n</italic></td><td rowspan="1" colspan="1">Mo <italic>K</italic>α radiation, λ = 0.71073 Å</td></tr><tr><td rowspan="1" colspan="1">Hall symbol: -P 2yn</td><td rowspan="1" colspan="1">Cell parameters from 16643 reflections</td></tr><tr><td rowspan="1" colspan="1"><italic>a</italic> = 10.3481 (2) Å</td><td rowspan="1" colspan="1">θ = 2.2–25.4°</td></tr><tr><td rowspan="1" colspan="1"><italic>b</italic> = 13.9791 (2) Å</td><td rowspan="1" colspan="1">µ = 0.78 mm<sup>−</sup><sup>1</sup></td></tr><tr><td rowspan="1" colspan="1"><italic>c</italic> = 12.7789 (2) Å</td><td rowspan="1" colspan="1"><italic>T</italic> = 173 K</td></tr><tr><td rowspan="1" colspan="1">β = 92.473 (1)°</td><td rowspan="1" colspan="1">Fragment, colourless</td></tr><tr><td rowspan="1" colspan="1"><italic>V</italic> = 1846.84 (5) Å<sup>3</sup></td><td rowspan="1" colspan="1">0.38 × 0.35 × 0.19 mm</td></tr><tr><td rowspan="1" colspan="1"><italic>Z</italic> = 2</td><td rowspan="1" colspan="1"></td></tr></table></table-wrap></sec><sec id="tablewrapdatacollectionlong"><title>Data collection</title><table-wrap position="anchor" id="d1e329"><table rules="all" frame="box" style="table-layout:fixed" summary=""><colgroup span="2"><col span="1"></col><col span="1"></col></colgroup><tr><td rowspan="1" colspan="1">Bruker APEXII diffractometer</td><td rowspan="1" colspan="1">3391 independent reflections</td></tr><tr><td rowspan="1" colspan="1">Radiation source: fine-focus sealed tube</td><td rowspan="1" colspan="1">3060 reflections with <italic>I</italic> > 2σ(<italic>I</italic>)</td></tr><tr><td rowspan="1" colspan="1">graphite</td><td rowspan="1" colspan="1"><italic>R</italic><sub>int</sub> = 0.027</td></tr><tr><td rowspan="1" colspan="1">ω and φ scans</td><td rowspan="1" colspan="1">θ<sub>max</sub> = 25.4°, θ<sub>min</sub> = 2.2°</td></tr><tr><td rowspan="1" colspan="1">Absorption correction: multi-scan (<italic>SADABS</italic>; Sheldrick, 1996)</td><td rowspan="1" colspan="1"><italic>h</italic> = −12→12</td></tr><tr><td rowspan="1" colspan="1"><italic>T</italic><sub>min</sub> = 0.753, <italic>T</italic><sub>max</sub> = 0.868</td><td rowspan="1" colspan="1"><italic>k</italic> = −15→16</td></tr><tr><td rowspan="1" colspan="1">16443 measured reflections</td><td rowspan="1" colspan="1"><italic>l</italic> = −15→15</td></tr></table></table-wrap></sec><sec id="tablewraprefinementdatalong"><title>Refinement</title><table-wrap position="anchor" id="d1e446"><table rules="all" frame="box" style="table-layout:fixed" summary=""><colgroup span="2"><col span="1"></col><col span="1"></col></colgroup><tr><td rowspan="1" colspan="1">Refinement on <italic>F</italic><sup>2</sup></td><td rowspan="1" colspan="1">Primary atom site location: structure-invariant direct methods</td></tr><tr><td rowspan="1" colspan="1">Least-squares matrix: full</td><td rowspan="1" colspan="1">Secondary atom site location: difference Fourier map</td></tr><tr><td rowspan="1" colspan="1"><italic>R</italic>[<italic>F</italic><sup>2</sup> > 2σ(<italic>F</italic><sup>2</sup>)] = 0.021</td><td rowspan="1" colspan="1">Hydrogen site location: inferred from neighbouring sites</td></tr><tr><td rowspan="1" colspan="1"><italic>wR</italic>(<italic>F</italic><sup>2</sup>) = 0.055</td><td rowspan="1" colspan="1">H atoms treated by a mixture of independent and constrained refinement</td></tr><tr><td rowspan="1" colspan="1"><italic>S</italic> = 1.07</td><td rowspan="1" colspan="1"><italic>w</italic> = 1/[σ<sup>2</sup>(<italic>F</italic><sub>o</sub><sup>2</sup>) + (0.0261<italic>P</italic>)<sup>2</sup> + 0.7641<italic>P</italic>] where <italic>P</italic> = (<italic>F</italic><sub>o</sub><sup>2</sup> + 2<italic>F</italic><sub>c</sub><sup>2</sup>)/3</td></tr><tr><td rowspan="1" colspan="1">3391 reflections</td><td rowspan="1" colspan="1">(Δ/σ)<sub>max</sub> = 0.001</td></tr><tr><td rowspan="1" colspan="1">226 parameters</td><td rowspan="1" colspan="1">Δρ<sub>max</sub> = 0.42 e Å<sup>−</sup><sup>3</sup></td></tr><tr><td rowspan="1" colspan="1">6 restraints</td><td rowspan="1" colspan="1">Δρ<sub>min</sub> = −0.23 e Å<sup>−</sup><sup>3</sup></td></tr></table></table-wrap></sec><sec id="specialdetails"><title>Special details</title><table-wrap position="anchor" id="d1e603"><table rules="all" frame="box" style="table-layout:fixed"><tr><td rowspan="1" colspan="1">Experimental. The fragment used in the single-crystal diffraction experiment was cleaved from
a very large prismatic crystal using a scalpel.</td></tr><tr><td rowspan="1" colspan="1">Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell e.s.d.'s are taken
into account individually in the estimation of e.s.d.'s in distances, angles
and torsion angles; correlations between e.s.d.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s.
planes.</td></tr><tr><td rowspan="1" colspan="1">Refinement. Refinement of <italic>F</italic><sup>2</sup> against ALL reflections. The weighted <italic>R</italic>-factor
<italic>wR</italic> and goodness of fit <italic>S</italic> are based on <italic>F</italic><sup>2</sup>, conventional
<italic>R</italic>-factors <italic>R</italic> are based on <italic>F</italic>, with <italic>F</italic> set to zero for
negative <italic>F</italic><sup>2</sup>. The threshold expression of <italic>F</italic><sup>2</sup> >
σ(<italic>F</italic><sup>2</sup>) is used only for calculating <italic>R</italic>-factors(gt) <italic>etc</italic>.
and is not relevant to the choice of reflections for refinement.
<italic>R</italic>-factors based on <italic>F</italic><sup>2</sup> are statistically about twice as large
as those based on <italic>F</italic>, and <italic>R</italic>- factors based on ALL data will be
even larger.</td></tr></table></table-wrap></sec><sec id="tablewrapcoords"><title>Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å<sup>2</sup>)</title><table-wrap position="anchor" id="d1e708"><table rules="all" frame="box" style="table-layout:fixed" summary=""><tr><td rowspan="1" colspan="1"></td><td rowspan="1" colspan="1"><italic>x</italic></td><td rowspan="1" colspan="1"><italic>y</italic></td><td rowspan="1" colspan="1"><italic>z</italic></td><td rowspan="1" colspan="1"><italic>U</italic><sub>iso</sub>*/<italic>U</italic><sub>eq</sub></td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">Cd1</td><td rowspan="1" colspan="1">0.0000</td><td rowspan="1" colspan="1">0.5000</td><td rowspan="1" colspan="1">0.5000</td><td rowspan="1" colspan="1">0.01972 (7)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">Cl1</td><td rowspan="1" colspan="1">−0.00576 (4)</td><td rowspan="1" colspan="1">0.56521 (3)</td><td rowspan="1" colspan="1">0.69090 (3)</td><td rowspan="1" colspan="1">0.02753 (11)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">O1W</td><td rowspan="1" colspan="1">0.31111 (17)</td><td rowspan="1" colspan="1">1.01315 (12)</td><td rowspan="1" colspan="1">0.44201 (15)</td><td rowspan="1" colspan="1">0.0498 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H1WA</td><td rowspan="1" colspan="1">0.267 (2)</td><td rowspan="1" colspan="1">0.9840 (17)</td><td rowspan="1" colspan="1">0.3915 (18)</td><td rowspan="1" colspan="1">0.060*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H1WB</td><td rowspan="1" colspan="1">0.375 (2)</td><td rowspan="1" colspan="1">1.0362 (19)</td><td rowspan="1" colspan="1">0.4063 (19)</td><td rowspan="1" colspan="1">0.060*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">O2W</td><td rowspan="1" colspan="1">0.4410 (2)</td><td rowspan="1" colspan="1">0.92673 (13)</td><td rowspan="1" colspan="1">0.61847 (14)</td><td rowspan="1" colspan="1">0.0623 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H2WA</td><td rowspan="1" colspan="1">0.385 (3)</td><td rowspan="1" colspan="1">0.958 (2)</td><td rowspan="1" colspan="1">0.5722 (19)</td><td rowspan="1" colspan="1">0.075*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H2WB</td><td rowspan="1" colspan="1">0.443 (3)</td><td rowspan="1" colspan="1">0.9689 (18)</td><td rowspan="1" colspan="1">0.6730 (17)</td><td rowspan="1" colspan="1">0.075*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N1</td><td rowspan="1" colspan="1">0.16425 (14)</td><td rowspan="1" colspan="1">0.61714 (10)</td><td rowspan="1" colspan="1">0.46966 (11)</td><td rowspan="1" colspan="1">0.0256 (3)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N2</td><td rowspan="1" colspan="1">0.14429 (14)</td><td rowspan="1" colspan="1">0.90557 (10)</td><td rowspan="1" colspan="1">0.29043 (11)</td><td rowspan="1" colspan="1">0.0242 (3)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N3</td><td rowspan="1" colspan="1">−0.05153 (14)</td><td rowspan="1" colspan="1">1.05084 (11)</td><td rowspan="1" colspan="1">0.26799 (11)</td><td rowspan="1" colspan="1">0.0267 (3)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N4</td><td rowspan="1" colspan="1">−0.35028 (14)</td><td rowspan="1" colspan="1">1.12026 (10)</td><td rowspan="1" colspan="1">0.05522 (11)</td><td rowspan="1" colspan="1">0.0235 (3)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C1</td><td rowspan="1" colspan="1">0.14831 (17)</td><td rowspan="1" colspan="1">0.67064 (12)</td><td rowspan="1" colspan="1">0.38328 (14)</td><td rowspan="1" colspan="1">0.0254 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H1</td><td rowspan="1" colspan="1">0.0828</td><td rowspan="1" colspan="1">0.6526</td><td rowspan="1" colspan="1">0.3328</td><td rowspan="1" colspan="1">0.031*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C2</td><td rowspan="1" colspan="1">0.22184 (17)</td><td rowspan="1" colspan="1">0.75090 (12)</td><td rowspan="1" colspan="1">0.36317 (14)</td><td rowspan="1" colspan="1">0.0246 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C3</td><td rowspan="1" colspan="1">0.31970 (18)</td><td rowspan="1" colspan="1">0.77468 (13)</td><td rowspan="1" colspan="1">0.43639 (15)</td><td rowspan="1" colspan="1">0.0301 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H3</td><td rowspan="1" colspan="1">0.3738</td><td rowspan="1" colspan="1">0.8283</td><td rowspan="1" colspan="1">0.4251</td><td rowspan="1" colspan="1">0.036*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C4</td><td rowspan="1" colspan="1">0.33772 (19)</td><td rowspan="1" colspan="1">0.71988 (13)</td><td rowspan="1" colspan="1">0.52574 (16)</td><td rowspan="1" colspan="1">0.0336 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H4</td><td rowspan="1" colspan="1">0.4041</td><td rowspan="1" colspan="1">0.7354</td><td rowspan="1" colspan="1">0.5766</td><td rowspan="1" colspan="1">0.040*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C5</td><td rowspan="1" colspan="1">0.25809 (18)</td><td rowspan="1" colspan="1">0.64246 (13)</td><td rowspan="1" colspan="1">0.53994 (15)</td><td rowspan="1" colspan="1">0.0308 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H5</td><td rowspan="1" colspan="1">0.2701</td><td rowspan="1" colspan="1">0.6055</td><td rowspan="1" colspan="1">0.6020</td><td rowspan="1" colspan="1">0.037*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C6</td><td rowspan="1" colspan="1">0.19428 (18)</td><td rowspan="1" colspan="1">0.80989 (13)</td><td rowspan="1" colspan="1">0.26599 (14)</td><td rowspan="1" colspan="1">0.0281 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H6A</td><td rowspan="1" colspan="1">0.2748</td><td rowspan="1" colspan="1">0.8168</td><td rowspan="1" colspan="1">0.2276</td><td rowspan="1" colspan="1">0.034*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H6B</td><td rowspan="1" colspan="1">0.1301</td><td rowspan="1" colspan="1">0.7760</td><td rowspan="1" colspan="1">0.2197</td><td rowspan="1" colspan="1">0.034*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C7</td><td rowspan="1" colspan="1">0.02170 (18)</td><td rowspan="1" colspan="1">0.90049 (13)</td><td rowspan="1" colspan="1">0.34449 (15)</td><td rowspan="1" colspan="1">0.0290 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H7A</td><td rowspan="1" colspan="1">0.0356</td><td rowspan="1" colspan="1">0.8657</td><td rowspan="1" colspan="1">0.4115</td><td rowspan="1" colspan="1">0.035*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H7B</td><td rowspan="1" colspan="1">−0.0430</td><td rowspan="1" colspan="1">0.8647</td><td rowspan="1" colspan="1">0.3006</td><td rowspan="1" colspan="1">0.035*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C8</td><td rowspan="1" colspan="1">−0.0291 (2)</td><td rowspan="1" colspan="1">0.99965 (13)</td><td rowspan="1" colspan="1">0.36577 (16)</td><td rowspan="1" colspan="1">0.0309 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H8A</td><td rowspan="1" colspan="1">−0.1109</td><td rowspan="1" colspan="1">0.9950</td><td rowspan="1" colspan="1">0.4028</td><td rowspan="1" colspan="1">0.037*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H8B</td><td rowspan="1" colspan="1">0.0344</td><td rowspan="1" colspan="1">1.0350</td><td rowspan="1" colspan="1">0.4112</td><td rowspan="1" colspan="1">0.037*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C9</td><td rowspan="1" colspan="1">0.06858 (18)</td><td rowspan="1" colspan="1">1.05772 (13)</td><td rowspan="1" colspan="1">0.21285 (15)</td><td rowspan="1" colspan="1">0.0307 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H9A</td><td rowspan="1" colspan="1">0.1326</td><td rowspan="1" colspan="1">1.0953</td><td rowspan="1" colspan="1">0.2555</td><td rowspan="1" colspan="1">0.037*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H9B</td><td rowspan="1" colspan="1">0.0521</td><td rowspan="1" colspan="1">1.0916</td><td rowspan="1" colspan="1">0.1456</td><td rowspan="1" colspan="1">0.037*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C10</td><td rowspan="1" colspan="1">0.12320 (18)</td><td rowspan="1" colspan="1">0.95935 (14)</td><td rowspan="1" colspan="1">0.19196 (14)</td><td rowspan="1" colspan="1">0.0297 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H10A</td><td rowspan="1" colspan="1">0.0624</td><td rowspan="1" colspan="1">0.9237</td><td rowspan="1" colspan="1">0.1444</td><td rowspan="1" colspan="1">0.036*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H10B</td><td rowspan="1" colspan="1">0.2062</td><td rowspan="1" colspan="1">0.9659</td><td rowspan="1" colspan="1">0.1569</td><td rowspan="1" colspan="1">0.036*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C11</td><td rowspan="1" colspan="1">−0.11128 (18)</td><td rowspan="1" colspan="1">1.14457 (13)</td><td rowspan="1" colspan="1">0.28181 (15)</td><td rowspan="1" colspan="1">0.0312 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H11A</td><td rowspan="1" colspan="1">−0.0434</td><td rowspan="1" colspan="1">1.1930</td><td rowspan="1" colspan="1">0.2976</td><td rowspan="1" colspan="1">0.037*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H11B</td><td rowspan="1" colspan="1">−0.1691</td><td rowspan="1" colspan="1">1.1423</td><td rowspan="1" colspan="1">0.3415</td><td rowspan="1" colspan="1">0.037*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C12</td><td rowspan="1" colspan="1">−0.27629 (17)</td><td rowspan="1" colspan="1">1.10601 (12)</td><td rowspan="1" colspan="1">0.14168 (14)</td><td rowspan="1" colspan="1">0.0247 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H12</td><td rowspan="1" colspan="1">−0.2843</td><td rowspan="1" colspan="1">1.0468</td><td rowspan="1" colspan="1">0.1772</td><td rowspan="1" colspan="1">0.030*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C13</td><td rowspan="1" colspan="1">−0.18808 (16)</td><td rowspan="1" colspan="1">1.17228 (12)</td><td rowspan="1" colspan="1">0.18317 (14)</td><td rowspan="1" colspan="1">0.0243 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C14</td><td rowspan="1" colspan="1">−0.17827 (18)</td><td rowspan="1" colspan="1">1.25856 (13)</td><td rowspan="1" colspan="1">0.13158 (15)</td><td rowspan="1" colspan="1">0.0298 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H14</td><td rowspan="1" colspan="1">−0.1203</td><td rowspan="1" colspan="1">1.3064</td><td rowspan="1" colspan="1">0.1578</td><td rowspan="1" colspan="1">0.036*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C15</td><td rowspan="1" colspan="1">−0.25411 (18)</td><td rowspan="1" colspan="1">1.27477 (13)</td><td rowspan="1" colspan="1">0.04085 (15)</td><td rowspan="1" colspan="1">0.0311 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H15</td><td rowspan="1" colspan="1">−0.2482</td><td rowspan="1" colspan="1">1.3335</td><td rowspan="1" colspan="1">0.0040</td><td rowspan="1" colspan="1">0.037*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C16</td><td rowspan="1" colspan="1">−0.33791 (17)</td><td rowspan="1" colspan="1">1.20436 (12)</td><td rowspan="1" colspan="1">0.00536 (14)</td><td rowspan="1" colspan="1">0.0261 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H16</td><td rowspan="1" colspan="1">−0.3892</td><td rowspan="1" colspan="1">1.2156</td><td rowspan="1" colspan="1">−0.0569</td><td rowspan="1" colspan="1">0.031*</td><td rowspan="1" colspan="1"></td></tr></table></table-wrap></sec><sec id="tablewrapadps"><title>Atomic displacement parameters (Å<sup>2</sup>)</title><table-wrap position="anchor" id="d1e1362"><table rules="all" frame="box" style="table-layout:fixed" summary=""><tr><td rowspan="1" colspan="1"></td><td rowspan="1" colspan="1"><italic>U</italic><sup>11</sup></td><td rowspan="1" colspan="1"><italic>U</italic><sup>22</sup></td><td rowspan="1" colspan="1"><italic>U</italic><sup>33</sup></td><td rowspan="1" colspan="1"><italic>U</italic><sup>12</sup></td><td rowspan="1" colspan="1"><italic>U</italic><sup>13</sup></td><td rowspan="1" colspan="1"><italic>U</italic><sup>23</sup></td></tr><tr><td rowspan="1" colspan="1">Cd1</td><td rowspan="1" colspan="1">0.02129 (11)</td><td rowspan="1" colspan="1">0.01716 (10)</td><td rowspan="1" colspan="1">0.02035 (10)</td><td rowspan="1" colspan="1">0.00052 (6)</td><td rowspan="1" colspan="1">−0.00332 (7)</td><td rowspan="1" colspan="1">0.00085 (6)</td></tr><tr><td rowspan="1" colspan="1">Cl1</td><td rowspan="1" colspan="1">0.0316 (2)</td><td rowspan="1" colspan="1">0.0285 (2)</td><td rowspan="1" colspan="1">0.0221 (2)</td><td rowspan="1" colspan="1">0.00443 (18)</td><td rowspan="1" colspan="1">−0.00335 (17)</td><td rowspan="1" colspan="1">−0.00290 (17)</td></tr><tr><td rowspan="1" colspan="1">O1W</td><td rowspan="1" colspan="1">0.0434 (10)</td><td rowspan="1" colspan="1">0.0459 (10)</td><td rowspan="1" colspan="1">0.0592 (11)</td><td rowspan="1" colspan="1">0.0018 (7)</td><td rowspan="1" colspan="1">−0.0069 (8)</td><td rowspan="1" colspan="1">−0.0213 (8)</td></tr><tr><td rowspan="1" colspan="1">O2W</td><td rowspan="1" colspan="1">0.0815 (14)</td><td rowspan="1" colspan="1">0.0578 (11)</td><td rowspan="1" colspan="1">0.0473 (10)</td><td rowspan="1" colspan="1">−0.0181 (10)</td><td rowspan="1" colspan="1">−0.0018 (9)</td><td rowspan="1" colspan="1">−0.0145 (8)</td></tr><tr><td rowspan="1" colspan="1">N1</td><td rowspan="1" colspan="1">0.0276 (8)</td><td rowspan="1" colspan="1">0.0227 (8)</td><td rowspan="1" colspan="1">0.0264 (8)</td><td rowspan="1" colspan="1">−0.0006 (6)</td><td rowspan="1" colspan="1">−0.0017 (6)</td><td rowspan="1" colspan="1">−0.0003 (6)</td></tr><tr><td rowspan="1" colspan="1">N2</td><td rowspan="1" colspan="1">0.0242 (7)</td><td rowspan="1" colspan="1">0.0247 (8)</td><td rowspan="1" colspan="1">0.0240 (7)</td><td rowspan="1" colspan="1">−0.0006 (6)</td><td rowspan="1" colspan="1">0.0033 (6)</td><td rowspan="1" colspan="1">0.0054 (6)</td></tr><tr><td rowspan="1" colspan="1">N3</td><td rowspan="1" colspan="1">0.0272 (8)</td><td rowspan="1" colspan="1">0.0269 (8)</td><td rowspan="1" colspan="1">0.0258 (8)</td><td rowspan="1" colspan="1">0.0029 (6)</td><td rowspan="1" colspan="1">−0.0011 (6)</td><td rowspan="1" colspan="1">0.0039 (6)</td></tr><tr><td rowspan="1" colspan="1">N4</td><td rowspan="1" colspan="1">0.0234 (7)</td><td rowspan="1" colspan="1">0.0221 (8)</td><td rowspan="1" colspan="1">0.0247 (7)</td><td rowspan="1" colspan="1">−0.0007 (6)</td><td rowspan="1" colspan="1">−0.0030 (6)</td><td rowspan="1" colspan="1">−0.0004 (6)</td></tr><tr><td rowspan="1" colspan="1">C1</td><td rowspan="1" colspan="1">0.0250 (9)</td><td rowspan="1" colspan="1">0.0246 (9)</td><td rowspan="1" colspan="1">0.0266 (9)</td><td rowspan="1" colspan="1">−0.0002 (7)</td><td rowspan="1" colspan="1">0.0008 (7)</td><td rowspan="1" colspan="1">−0.0025 (7)</td></tr><tr><td rowspan="1" colspan="1">C2</td><td rowspan="1" colspan="1">0.0247 (9)</td><td rowspan="1" colspan="1">0.0209 (9)</td><td rowspan="1" colspan="1">0.0288 (9)</td><td rowspan="1" colspan="1">0.0033 (7)</td><td rowspan="1" colspan="1">0.0070 (7)</td><td rowspan="1" colspan="1">−0.0010 (7)</td></tr><tr><td rowspan="1" colspan="1">C3</td><td rowspan="1" colspan="1">0.0267 (9)</td><td rowspan="1" colspan="1">0.0208 (9)</td><td rowspan="1" colspan="1">0.0426 (11)</td><td rowspan="1" colspan="1">−0.0027 (7)</td><td rowspan="1" colspan="1">0.0014 (8)</td><td rowspan="1" colspan="1">−0.0005 (8)</td></tr><tr><td rowspan="1" colspan="1">C4</td><td rowspan="1" colspan="1">0.0301 (10)</td><td rowspan="1" colspan="1">0.0288 (10)</td><td rowspan="1" colspan="1">0.0410 (11)</td><td rowspan="1" colspan="1">−0.0017 (8)</td><td rowspan="1" colspan="1">−0.0089 (9)</td><td rowspan="1" colspan="1">−0.0015 (8)</td></tr><tr><td rowspan="1" colspan="1">C5</td><td rowspan="1" colspan="1">0.0326 (10)</td><td rowspan="1" colspan="1">0.0276 (10)</td><td rowspan="1" colspan="1">0.0317 (10)</td><td rowspan="1" colspan="1">0.0009 (8)</td><td rowspan="1" colspan="1">−0.0044 (8)</td><td rowspan="1" colspan="1">0.0027 (8)</td></tr><tr><td rowspan="1" colspan="1">C6</td><td rowspan="1" colspan="1">0.0310 (10)</td><td rowspan="1" colspan="1">0.0261 (10)</td><td rowspan="1" colspan="1">0.0275 (9)</td><td rowspan="1" colspan="1">−0.0018 (8)</td><td rowspan="1" colspan="1">0.0059 (8)</td><td rowspan="1" colspan="1">0.0015 (7)</td></tr><tr><td rowspan="1" colspan="1">C7</td><td rowspan="1" colspan="1">0.0278 (9)</td><td rowspan="1" colspan="1">0.0306 (10)</td><td rowspan="1" colspan="1">0.0291 (10)</td><td rowspan="1" colspan="1">−0.0011 (8)</td><td rowspan="1" colspan="1">0.0055 (8)</td><td rowspan="1" colspan="1">0.0082 (8)</td></tr><tr><td rowspan="1" colspan="1">C8</td><td rowspan="1" colspan="1">0.0288 (10)</td><td rowspan="1" colspan="1">0.0368 (11)</td><td rowspan="1" colspan="1">0.0274 (10)</td><td rowspan="1" colspan="1">0.0037 (8)</td><td rowspan="1" colspan="1">0.0052 (8)</td><td rowspan="1" colspan="1">0.0048 (8)</td></tr><tr><td rowspan="1" colspan="1">C9</td><td rowspan="1" colspan="1">0.0308 (10)</td><td rowspan="1" colspan="1">0.0305 (10)</td><td rowspan="1" colspan="1">0.0308 (10)</td><td rowspan="1" colspan="1">−0.0018 (8)</td><td rowspan="1" colspan="1">0.0000 (8)</td><td rowspan="1" colspan="1">0.0093 (8)</td></tr><tr><td rowspan="1" colspan="1">C10</td><td rowspan="1" colspan="1">0.0300 (10)</td><td rowspan="1" colspan="1">0.0325 (10)</td><td rowspan="1" colspan="1">0.0269 (9)</td><td rowspan="1" colspan="1">−0.0008 (8)</td><td rowspan="1" colspan="1">0.0046 (8)</td><td rowspan="1" colspan="1">0.0074 (8)</td></tr><tr><td rowspan="1" colspan="1">C11</td><td rowspan="1" colspan="1">0.0312 (10)</td><td rowspan="1" colspan="1">0.0292 (10)</td><td rowspan="1" colspan="1">0.0324 (10)</td><td rowspan="1" colspan="1">0.0011 (8)</td><td rowspan="1" colspan="1">−0.0085 (8)</td><td rowspan="1" colspan="1">−0.0051 (8)</td></tr><tr><td rowspan="1" colspan="1">C12</td><td rowspan="1" colspan="1">0.0267 (9)</td><td rowspan="1" colspan="1">0.0190 (9)</td><td rowspan="1" colspan="1">0.0283 (9)</td><td rowspan="1" colspan="1">0.0002 (7)</td><td rowspan="1" colspan="1">−0.0011 (7)</td><td rowspan="1" colspan="1">0.0015 (7)</td></tr><tr><td rowspan="1" colspan="1">C13</td><td rowspan="1" colspan="1">0.0215 (9)</td><td rowspan="1" colspan="1">0.0230 (9)</td><td rowspan="1" colspan="1">0.0282 (9)</td><td rowspan="1" colspan="1">0.0011 (7)</td><td rowspan="1" colspan="1">−0.0016 (7)</td><td rowspan="1" colspan="1">−0.0033 (7)</td></tr><tr><td rowspan="1" colspan="1">C14</td><td rowspan="1" colspan="1">0.0272 (9)</td><td rowspan="1" colspan="1">0.0223 (9)</td><td rowspan="1" colspan="1">0.0396 (11)</td><td rowspan="1" colspan="1">−0.0049 (7)</td><td rowspan="1" colspan="1">−0.0021 (8)</td><td rowspan="1" colspan="1">−0.0041 (8)</td></tr><tr><td rowspan="1" colspan="1">C15</td><td rowspan="1" colspan="1">0.0370 (11)</td><td rowspan="1" colspan="1">0.0212 (9)</td><td rowspan="1" colspan="1">0.0349 (10)</td><td rowspan="1" colspan="1">−0.0023 (8)</td><td rowspan="1" colspan="1">0.0002 (8)</td><td rowspan="1" colspan="1">0.0047 (8)</td></tr><tr><td rowspan="1" colspan="1">C16</td><td rowspan="1" colspan="1">0.0293 (9)</td><td rowspan="1" colspan="1">0.0239 (9)</td><td rowspan="1" colspan="1">0.0251 (9)</td><td rowspan="1" colspan="1">0.0016 (7)</td><td rowspan="1" colspan="1">−0.0010 (7)</td><td rowspan="1" colspan="1">0.0021 (7)</td></tr></table></table-wrap></sec><sec id="tablewrapgeomlong"><title>Geometric parameters (Å, °)</title><table-wrap position="anchor" id="d1e1847"><table rules="all" frame="box" style="table-layout:fixed" summary=""><colgroup span="4"><col span="1"></col><col span="1"></col><col span="1"></col><col span="1"></col></colgroup><tr><td rowspan="1" colspan="1">Cd1—N4<sup>i</sup></td><td rowspan="1" colspan="1">2.3728 (14)</td><td rowspan="1" colspan="1">C4—C5</td><td rowspan="1" colspan="1">1.377 (3)</td></tr><tr><td rowspan="1" colspan="1">Cd1—N4<sup>ii</sup></td><td rowspan="1" colspan="1">2.3728 (14)</td><td rowspan="1" colspan="1">C4—H4</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">Cd1—N1</td><td rowspan="1" colspan="1">2.4036 (15)</td><td rowspan="1" colspan="1">C5—H5</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">Cd1—N1<sup>iii</sup></td><td rowspan="1" colspan="1">2.4036 (15)</td><td rowspan="1" colspan="1">C6—H6A</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">Cd1—Cl1</td><td rowspan="1" colspan="1">2.6074 (4)</td><td rowspan="1" colspan="1">C6—H6B</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">Cd1—Cl1<sup>iii</sup></td><td rowspan="1" colspan="1">2.6074 (4)</td><td rowspan="1" colspan="1">C7—C8</td><td rowspan="1" colspan="1">1.511 (3)</td></tr><tr><td rowspan="1" colspan="1">O1W—H1WA</td><td rowspan="1" colspan="1">0.874 (16)</td><td rowspan="1" colspan="1">C7—H7A</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">O1W—H1WB</td><td rowspan="1" colspan="1">0.884 (16)</td><td rowspan="1" colspan="1">C7—H7B</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">O2W—H2WA</td><td rowspan="1" colspan="1">0.921 (17)</td><td rowspan="1" colspan="1">C8—H8A</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">O2W—H2WB</td><td rowspan="1" colspan="1">0.912 (17)</td><td rowspan="1" colspan="1">C8—H8B</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">N1—C1</td><td rowspan="1" colspan="1">1.338 (2)</td><td rowspan="1" colspan="1">C9—C10</td><td rowspan="1" colspan="1">1.515 (3)</td></tr><tr><td rowspan="1" colspan="1">N1—C5</td><td rowspan="1" colspan="1">1.342 (2)</td><td rowspan="1" colspan="1">C9—H9A</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">N2—C7</td><td rowspan="1" colspan="1">1.472 (2)</td><td rowspan="1" colspan="1">C9—H9B</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">N2—C6</td><td rowspan="1" colspan="1">1.472 (2)</td><td rowspan="1" colspan="1">C10—H10A</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">N2—C10</td><td rowspan="1" colspan="1">1.474 (2)</td><td rowspan="1" colspan="1">C10—H10B</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">N3—C8</td><td rowspan="1" colspan="1">1.450 (2)</td><td rowspan="1" colspan="1">C11—C13</td><td rowspan="1" colspan="1">1.511 (2)</td></tr><tr><td rowspan="1" colspan="1">N3—C9</td><td rowspan="1" colspan="1">1.458 (2)</td><td rowspan="1" colspan="1">C11—H11A</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">N3—C11</td><td rowspan="1" colspan="1">1.463 (2)</td><td rowspan="1" colspan="1">C11—H11B</td><td rowspan="1" colspan="1">0.9900</td></tr><tr><td rowspan="1" colspan="1">N4—C12</td><td rowspan="1" colspan="1">1.332 (2)</td><td rowspan="1" colspan="1">C12—C13</td><td rowspan="1" colspan="1">1.390 (2)</td></tr><tr><td rowspan="1" colspan="1">N4—C16</td><td rowspan="1" colspan="1">1.346 (2)</td><td rowspan="1" colspan="1">C12—H12</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">N4—Cd1<sup>iv</sup></td><td rowspan="1" colspan="1">2.3728 (14)</td><td rowspan="1" colspan="1">C13—C14</td><td rowspan="1" colspan="1">1.380 (3)</td></tr><tr><td rowspan="1" colspan="1">C1—C2</td><td rowspan="1" colspan="1">1.386 (2)</td><td rowspan="1" colspan="1">C14—C15</td><td rowspan="1" colspan="1">1.390 (3)</td></tr><tr><td rowspan="1" colspan="1">C1—H1</td><td rowspan="1" colspan="1">0.9500</td><td rowspan="1" colspan="1">C14—H14</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C2—C3</td><td rowspan="1" colspan="1">1.389 (3)</td><td rowspan="1" colspan="1">C15—C16</td><td rowspan="1" colspan="1">1.376 (3)</td></tr><tr><td rowspan="1" colspan="1">C2—C6</td><td rowspan="1" colspan="1">1.508 (2)</td><td rowspan="1" colspan="1">C15—H15</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C3—C4</td><td rowspan="1" colspan="1">1.381 (3)</td><td rowspan="1" colspan="1">C16—H16</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C3—H3</td><td rowspan="1" colspan="1">0.9500</td><td rowspan="1" colspan="1"></td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1"></td><td rowspan="1" colspan="1"></td><td rowspan="1" colspan="1"></td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N4<sup>i</sup>—Cd1—N4<sup>ii</sup></td><td rowspan="1" colspan="1">180.0</td><td rowspan="1" colspan="1">C2—C6—H6B</td><td rowspan="1" colspan="1">109.2</td></tr><tr><td rowspan="1" colspan="1">N4<sup>i</sup>—Cd1—N1</td><td rowspan="1" colspan="1">94.21 (5)</td><td rowspan="1" colspan="1">H6A—C6—H6B</td><td rowspan="1" colspan="1">107.9</td></tr><tr><td rowspan="1" colspan="1">N4<sup>ii</sup>—Cd1—N1</td><td rowspan="1" colspan="1">85.79 (5)</td><td rowspan="1" colspan="1">N2—C7—C8</td><td rowspan="1" colspan="1">110.71 (15)</td></tr><tr><td rowspan="1" colspan="1">N4<sup>i</sup>—Cd1—N1<sup>iii</sup></td><td rowspan="1" colspan="1">85.79 (5)</td><td rowspan="1" colspan="1">N2—C7—H7A</td><td rowspan="1" colspan="1">109.5</td></tr><tr><td rowspan="1" colspan="1">N4<sup>ii</sup>—Cd1—N1<sup>iii</sup></td><td rowspan="1" colspan="1">94.21 (5)</td><td rowspan="1" colspan="1">C8—C7—H7A</td><td rowspan="1" colspan="1">109.5</td></tr><tr><td rowspan="1" colspan="1">N1—Cd1—N1<sup>iii</sup></td><td rowspan="1" colspan="1">180.00 (5)</td><td rowspan="1" colspan="1">N2—C7—H7B</td><td rowspan="1" colspan="1">109.5</td></tr><tr><td rowspan="1" colspan="1">N4<sup>i</sup>—Cd1—Cl1</td><td rowspan="1" colspan="1">90.60 (4)</td><td rowspan="1" colspan="1">C8—C7—H7B</td><td rowspan="1" colspan="1">109.5</td></tr><tr><td rowspan="1" colspan="1">N4<sup>ii</sup>—Cd1—Cl1</td><td rowspan="1" colspan="1">89.40 (4)</td><td rowspan="1" colspan="1">H7A—C7—H7B</td><td rowspan="1" colspan="1">108.1</td></tr><tr><td rowspan="1" colspan="1">N1—Cd1—Cl1</td><td rowspan="1" colspan="1">87.57 (4)</td><td rowspan="1" colspan="1">N3—C8—C7</td><td rowspan="1" colspan="1">109.98 (16)</td></tr><tr><td rowspan="1" colspan="1">N1<sup>iii</sup>—Cd1—Cl1</td><td rowspan="1" colspan="1">92.43 (4)</td><td rowspan="1" colspan="1">N3—C8—H8A</td><td rowspan="1" colspan="1">109.7</td></tr><tr><td rowspan="1" colspan="1">N4<sup>i</sup>—Cd1—Cl1<sup>iii</sup></td><td rowspan="1" colspan="1">89.40 (4)</td><td rowspan="1" colspan="1">C7—C8—H8A</td><td rowspan="1" colspan="1">109.7</td></tr><tr><td rowspan="1" colspan="1">N4<sup>ii</sup>—Cd1—Cl1<sup>iii</sup></td><td rowspan="1" colspan="1">90.60 (4)</td><td rowspan="1" colspan="1">N3—C8—H8B</td><td rowspan="1" colspan="1">109.7</td></tr><tr><td rowspan="1" colspan="1">N1—Cd1—Cl1<sup>iii</sup></td><td rowspan="1" colspan="1">92.43 (4)</td><td rowspan="1" colspan="1">C7—C8—H8B</td><td rowspan="1" colspan="1">109.7</td></tr><tr><td rowspan="1" colspan="1">N1<sup>iii</sup>—Cd1—Cl1<sup>iii</sup></td><td rowspan="1" colspan="1">87.57 (4)</td><td rowspan="1" colspan="1">H8A—C8—H8B</td><td rowspan="1" colspan="1">108.2</td></tr><tr><td rowspan="1" colspan="1">Cl1—Cd1—Cl1<sup>iii</sup></td><td rowspan="1" colspan="1">180.0</td><td rowspan="1" colspan="1">N3—C9—C10</td><td rowspan="1" colspan="1">110.96 (15)</td></tr><tr><td rowspan="1" colspan="1">H1WA—O1W—H1WB</td><td rowspan="1" colspan="1">100 (2)</td><td rowspan="1" colspan="1">N3—C9—H9A</td><td rowspan="1" colspan="1">109.4</td></tr><tr><td rowspan="1" colspan="1">H2WA—O2W—H2WB</td><td rowspan="1" colspan="1">100 (2)</td><td rowspan="1" colspan="1">C10—C9—H9A</td><td rowspan="1" colspan="1">109.4</td></tr><tr><td rowspan="1" colspan="1">C1—N1—C5</td><td rowspan="1" colspan="1">117.70 (16)</td><td rowspan="1" colspan="1">N3—C9—H9B</td><td rowspan="1" colspan="1">109.4</td></tr><tr><td rowspan="1" colspan="1">C1—N1—Cd1</td><td rowspan="1" colspan="1">116.82 (11)</td><td rowspan="1" colspan="1">C10—C9—H9B</td><td rowspan="1" colspan="1">109.4</td></tr><tr><td rowspan="1" colspan="1">C5—N1—Cd1</td><td rowspan="1" colspan="1">124.63 (12)</td><td rowspan="1" colspan="1">H9A—C9—H9B</td><td rowspan="1" colspan="1">108.0</td></tr><tr><td rowspan="1" colspan="1">C7—N2—C6</td><td rowspan="1" colspan="1">111.94 (14)</td><td rowspan="1" colspan="1">N2—C10—C9</td><td rowspan="1" colspan="1">110.80 (15)</td></tr><tr><td rowspan="1" colspan="1">C7—N2—C10</td><td rowspan="1" colspan="1">109.05 (14)</td><td rowspan="1" colspan="1">N2—C10—H10A</td><td rowspan="1" colspan="1">109.5</td></tr><tr><td rowspan="1" colspan="1">C6—N2—C10</td><td rowspan="1" colspan="1">108.82 (14)</td><td rowspan="1" colspan="1">C9—C10—H10A</td><td rowspan="1" colspan="1">109.5</td></tr><tr><td rowspan="1" colspan="1">C8—N3—C9</td><td rowspan="1" colspan="1">109.92 (14)</td><td rowspan="1" colspan="1">N2—C10—H10B</td><td rowspan="1" colspan="1">109.5</td></tr><tr><td rowspan="1" colspan="1">C8—N3—C11</td><td rowspan="1" colspan="1">113.01 (15)</td><td rowspan="1" colspan="1">C9—C10—H10B</td><td rowspan="1" colspan="1">109.5</td></tr><tr><td rowspan="1" colspan="1">C9—N3—C11</td><td rowspan="1" colspan="1">111.90 (15)</td><td rowspan="1" colspan="1">H10A—C10—H10B</td><td rowspan="1" colspan="1">108.1</td></tr><tr><td rowspan="1" colspan="1">C12—N4—C16</td><td rowspan="1" colspan="1">117.41 (15)</td><td rowspan="1" colspan="1">N3—C11—C13</td><td rowspan="1" colspan="1">109.80 (14)</td></tr><tr><td rowspan="1" colspan="1">C12—N4—Cd1<sup>iv</sup></td><td rowspan="1" colspan="1">119.03 (11)</td><td rowspan="1" colspan="1">N3—C11—H11A</td><td rowspan="1" colspan="1">109.7</td></tr><tr><td rowspan="1" colspan="1">C16—N4—Cd1<sup>iv</sup></td><td rowspan="1" colspan="1">123.53 (11)</td><td rowspan="1" colspan="1">C13—C11—H11A</td><td rowspan="1" colspan="1">109.7</td></tr><tr><td rowspan="1" colspan="1">N1—C1—C2</td><td rowspan="1" colspan="1">123.82 (16)</td><td rowspan="1" colspan="1">N3—C11—H11B</td><td rowspan="1" colspan="1">109.7</td></tr><tr><td rowspan="1" colspan="1">N1—C1—H1</td><td rowspan="1" colspan="1">118.1</td><td rowspan="1" colspan="1">C13—C11—H11B</td><td rowspan="1" colspan="1">109.7</td></tr><tr><td rowspan="1" colspan="1">C2—C1—H1</td><td rowspan="1" colspan="1">118.1</td><td rowspan="1" colspan="1">H11A—C11—H11B</td><td rowspan="1" colspan="1">108.2</td></tr><tr><td rowspan="1" colspan="1">C1—C2—C3</td><td rowspan="1" colspan="1">117.32 (16)</td><td rowspan="1" colspan="1">N4—C12—C13</td><td rowspan="1" colspan="1">124.16 (16)</td></tr><tr><td rowspan="1" colspan="1">C1—C2—C6</td><td rowspan="1" colspan="1">120.65 (16)</td><td rowspan="1" colspan="1">N4—C12—H12</td><td rowspan="1" colspan="1">117.9</td></tr><tr><td rowspan="1" colspan="1">C3—C2—C6</td><td rowspan="1" colspan="1">122.03 (16)</td><td rowspan="1" colspan="1">C13—C12—H12</td><td rowspan="1" colspan="1">117.9</td></tr><tr><td rowspan="1" colspan="1">C4—C3—C2</td><td rowspan="1" colspan="1">119.52 (17)</td><td rowspan="1" colspan="1">C14—C13—C12</td><td rowspan="1" colspan="1">117.45 (16)</td></tr><tr><td rowspan="1" colspan="1">C4—C3—H3</td><td rowspan="1" colspan="1">120.2</td><td rowspan="1" colspan="1">C14—C13—C11</td><td rowspan="1" colspan="1">125.13 (16)</td></tr><tr><td rowspan="1" colspan="1">C2—C3—H3</td><td rowspan="1" colspan="1">120.2</td><td rowspan="1" colspan="1">C12—C13—C11</td><td rowspan="1" colspan="1">117.42 (16)</td></tr><tr><td rowspan="1" colspan="1">C5—C4—C3</td><td rowspan="1" colspan="1">118.99 (18)</td><td rowspan="1" colspan="1">C13—C14—C15</td><td rowspan="1" colspan="1">119.35 (16)</td></tr><tr><td rowspan="1" colspan="1">C5—C4—H4</td><td rowspan="1" colspan="1">120.5</td><td rowspan="1" colspan="1">C13—C14—H14</td><td rowspan="1" colspan="1">120.3</td></tr><tr><td rowspan="1" colspan="1">C3—C4—H4</td><td rowspan="1" colspan="1">120.5</td><td rowspan="1" colspan="1">C15—C14—H14</td><td rowspan="1" colspan="1">120.3</td></tr><tr><td rowspan="1" colspan="1">N1—C5—C4</td><td rowspan="1" colspan="1">122.63 (18)</td><td rowspan="1" colspan="1">C16—C15—C14</td><td rowspan="1" colspan="1">118.91 (17)</td></tr><tr><td rowspan="1" colspan="1">N1—C5—H5</td><td rowspan="1" colspan="1">118.7</td><td rowspan="1" colspan="1">C16—C15—H15</td><td rowspan="1" colspan="1">120.5</td></tr><tr><td rowspan="1" colspan="1">C4—C5—H5</td><td rowspan="1" colspan="1">118.7</td><td rowspan="1" colspan="1">C14—C15—H15</td><td rowspan="1" colspan="1">120.5</td></tr><tr><td rowspan="1" colspan="1">N2—C6—C2</td><td rowspan="1" colspan="1">112.20 (14)</td><td rowspan="1" colspan="1">N4—C16—C15</td><td rowspan="1" colspan="1">122.71 (16)</td></tr><tr><td rowspan="1" colspan="1">N2—C6—H6A</td><td rowspan="1" colspan="1">109.2</td><td rowspan="1" colspan="1">N4—C16—H16</td><td rowspan="1" colspan="1">118.6</td></tr><tr><td rowspan="1" colspan="1">C2—C6—H6A</td><td rowspan="1" colspan="1">109.2</td><td rowspan="1" colspan="1">C15—C16—H16</td><td rowspan="1" colspan="1">118.6</td></tr><tr><td rowspan="1" colspan="1">N2—C6—H6B</td><td rowspan="1" colspan="1">109.2</td><td rowspan="1" colspan="1"></td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1"></td><td rowspan="1" colspan="1"></td><td rowspan="1" colspan="1"></td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N4<sup>i</sup>—Cd1—N1—C1</td><td rowspan="1" colspan="1">138.25 (13)</td><td rowspan="1" colspan="1">C10—N2—C7—C8</td><td rowspan="1" colspan="1">−57.93 (19)</td></tr><tr><td rowspan="1" colspan="1">N4<sup>ii</sup>—Cd1—N1—C1</td><td rowspan="1" colspan="1">−41.75 (13)</td><td rowspan="1" colspan="1">C9—N3—C8—C7</td><td rowspan="1" colspan="1">−59.1 (2)</td></tr><tr><td rowspan="1" colspan="1">Cl1—Cd1—N1—C1</td><td rowspan="1" colspan="1">−131.32 (12)</td><td rowspan="1" colspan="1">C11—N3—C8—C7</td><td rowspan="1" colspan="1">175.07 (15)</td></tr><tr><td rowspan="1" colspan="1">Cl1<sup>iii</sup>—Cd1—N1—C1</td><td rowspan="1" colspan="1">48.68 (12)</td><td rowspan="1" colspan="1">N2—C7—C8—N3</td><td rowspan="1" colspan="1">60.0 (2)</td></tr><tr><td rowspan="1" colspan="1">N4<sup>i</sup>—Cd1—N1—C5</td><td rowspan="1" colspan="1">−52.61 (14)</td><td rowspan="1" colspan="1">C8—N3—C9—C10</td><td rowspan="1" colspan="1">58.00 (19)</td></tr><tr><td rowspan="1" colspan="1">N4<sup>ii</sup>—Cd1—N1—C5</td><td rowspan="1" colspan="1">127.39 (14)</td><td rowspan="1" colspan="1">C11—N3—C9—C10</td><td rowspan="1" colspan="1">−175.57 (14)</td></tr><tr><td rowspan="1" colspan="1">Cl1—Cd1—N1—C5</td><td rowspan="1" colspan="1">37.82 (14)</td><td rowspan="1" colspan="1">C7—N2—C10—C9</td><td rowspan="1" colspan="1">56.28 (19)</td></tr><tr><td rowspan="1" colspan="1">Cl1<sup>iii</sup>—Cd1—N1—C5</td><td rowspan="1" colspan="1">−142.18 (14)</td><td rowspan="1" colspan="1">C6—N2—C10—C9</td><td rowspan="1" colspan="1">178.64 (15)</td></tr><tr><td rowspan="1" colspan="1">C5—N1—C1—C2</td><td rowspan="1" colspan="1">−0.8 (3)</td><td rowspan="1" colspan="1">N3—C9—C10—N2</td><td rowspan="1" colspan="1">−57.0 (2)</td></tr><tr><td rowspan="1" colspan="1">Cd1—N1—C1—C2</td><td rowspan="1" colspan="1">169.09 (13)</td><td rowspan="1" colspan="1">C8—N3—C11—C13</td><td rowspan="1" colspan="1">−153.02 (16)</td></tr><tr><td rowspan="1" colspan="1">N1—C1—C2—C3</td><td rowspan="1" colspan="1">1.8 (3)</td><td rowspan="1" colspan="1">C9—N3—C11—C13</td><td rowspan="1" colspan="1">82.25 (18)</td></tr><tr><td rowspan="1" colspan="1">N1—C1—C2—C6</td><td rowspan="1" colspan="1">−177.44 (16)</td><td rowspan="1" colspan="1">C16—N4—C12—C13</td><td rowspan="1" colspan="1">0.1 (3)</td></tr><tr><td rowspan="1" colspan="1">C1—C2—C3—C4</td><td rowspan="1" colspan="1">−1.5 (3)</td><td rowspan="1" colspan="1">Cd1<sup>iv</sup>—N4—C12—C13</td><td rowspan="1" colspan="1">−178.06 (13)</td></tr><tr><td rowspan="1" colspan="1">C6—C2—C3—C4</td><td rowspan="1" colspan="1">177.80 (17)</td><td rowspan="1" colspan="1">N4—C12—C13—C14</td><td rowspan="1" colspan="1">0.7 (3)</td></tr><tr><td rowspan="1" colspan="1">C2—C3—C4—C5</td><td rowspan="1" colspan="1">0.2 (3)</td><td rowspan="1" colspan="1">N4—C12—C13—C11</td><td rowspan="1" colspan="1">−179.79 (16)</td></tr><tr><td rowspan="1" colspan="1">C1—N1—C5—C4</td><td rowspan="1" colspan="1">−0.6 (3)</td><td rowspan="1" colspan="1">N3—C11—C13—C14</td><td rowspan="1" colspan="1">−129.54 (18)</td></tr><tr><td rowspan="1" colspan="1">Cd1—N1—C5—C4</td><td rowspan="1" colspan="1">−169.62 (14)</td><td rowspan="1" colspan="1">N3—C11—C13—C12</td><td rowspan="1" colspan="1">51.0 (2)</td></tr><tr><td rowspan="1" colspan="1">C3—C4—C5—N1</td><td rowspan="1" colspan="1">0.9 (3)</td><td rowspan="1" colspan="1">C12—C13—C14—C15</td><td rowspan="1" colspan="1">−1.0 (3)</td></tr><tr><td rowspan="1" colspan="1">C7—N2—C6—C2</td><td rowspan="1" colspan="1">−60.88 (19)</td><td rowspan="1" colspan="1">C11—C13—C14—C15</td><td rowspan="1" colspan="1">179.54 (18)</td></tr><tr><td rowspan="1" colspan="1">C10—N2—C6—C2</td><td rowspan="1" colspan="1">178.52 (15)</td><td rowspan="1" colspan="1">C13—C14—C15—C16</td><td rowspan="1" colspan="1">0.5 (3)</td></tr><tr><td rowspan="1" colspan="1">C1—C2—C6—N2</td><td rowspan="1" colspan="1">112.33 (18)</td><td rowspan="1" colspan="1">C12—N4—C16—C15</td><td rowspan="1" colspan="1">−0.7 (3)</td></tr><tr><td rowspan="1" colspan="1">C3—C2—C6—N2</td><td rowspan="1" colspan="1">−66.9 (2)</td><td rowspan="1" colspan="1">Cd1<sup>iv</sup>—N4—C16—C15</td><td rowspan="1" colspan="1">177.39 (14)</td></tr><tr><td rowspan="1" colspan="1">C6—N2—C7—C8</td><td rowspan="1" colspan="1">−178.39 (15)</td><td rowspan="1" colspan="1">C14—C15—C16—N4</td><td rowspan="1" colspan="1">0.4 (3)</td></tr></table></table-wrap><p>Symmetry codes: (i) <italic>x</italic>+1/2, −<italic>y</italic>+3/2, <italic>z</italic>+1/2; (ii) −<italic>x</italic>−1/2, <italic>y</italic>−1/2, −<italic>z</italic>+1/2; (iii) −<italic>x</italic>, −<italic>y</italic>+1, −<italic>z</italic>+1; (iv) −<italic>x</italic>−1/2, <italic>y</italic>+1/2, −<italic>z</italic>+1/2.</p></sec><sec id="tablewraphbondslong"><title>Hydrogen-bond geometry (Å, °)</title><table-wrap position="anchor" id="d1e2935"><table rules="all" frame="box" style="table-layout:fixed" summary=""><colgroup span="5"><col span="1"></col><col span="1"></col><col span="1"></col><col span="1"></col><col span="1"></col></colgroup><tr><td rowspan="1" colspan="1"><italic>D</italic>—H···<italic>A</italic></td><td rowspan="1" colspan="1"><italic>D</italic>—H</td><td rowspan="1" colspan="1">H···<italic>A</italic></td><td rowspan="1" colspan="1"><italic>D</italic>···<italic>A</italic></td><td rowspan="1" colspan="1"><italic>D</italic>—H···<italic>A</italic></td></tr><tr><td rowspan="1" colspan="1">O1W—H1WA···N2</td><td rowspan="1" colspan="1">0.87 (2)</td><td rowspan="1" colspan="1">2.08 (2)</td><td rowspan="1" colspan="1">2.950 (2)</td><td rowspan="1" colspan="1">171 (2)</td></tr><tr><td rowspan="1" colspan="1">O1W—H1WB···O2W<sup>v</sup></td><td rowspan="1" colspan="1">0.88 (2)</td><td rowspan="1" colspan="1">2.01 (2)</td><td rowspan="1" colspan="1">2.838 (3)</td><td rowspan="1" colspan="1">156 (2)</td></tr><tr><td rowspan="1" colspan="1">O2W—H2WA···O1W</td><td rowspan="1" colspan="1">0.92 (2)</td><td rowspan="1" colspan="1">1.96 (2)</td><td rowspan="1" colspan="1">2.844 (3)</td><td rowspan="1" colspan="1">161 (3)</td></tr><tr><td rowspan="1" colspan="1">O2W—H2WB···Cl1<sup>vi</sup></td><td rowspan="1" colspan="1">0.91 (2)</td><td rowspan="1" colspan="1">2.27 (2)</td><td rowspan="1" colspan="1">3.1607 (17)</td><td rowspan="1" colspan="1">165 (3)</td></tr></table></table-wrap><p>Symmetry codes: (v) −<italic>x</italic>+1, −<italic>y</italic>+2, −<italic>z</italic>+1; (vi) −<italic>x</italic>+1/2, <italic>y</italic>+1/2, −<italic>z</italic>+3/2.</p></sec></app></app-group><ref-list><title>References</title><ref id="bb1"><mixed-citation publication-type="other">Bruker (2006). <italic>APEX2</italic> and <italic>SAINT</italic> Bruker AXS Inc., Madison, Wisconsin, USA.</mixed-citation></ref><ref id="bb2"><mixed-citation publication-type="other">Martin, D., Supkowski, R. M. & LaDuca, R. L. (2009). <italic>Dalton Trans.</italic> pp. 514–520.</mixed-citation></ref><ref id="bb3"><mixed-citation publication-type="other">Palmer, D. (2007). <italic>CrystalMaker</italic> CrystalMaker Software, Bicester, Oxfordshire, England.</mixed-citation></ref><ref id="bb4"><mixed-citation publication-type="other">Pocic, D., Planeix, J.-M., Kyritsakas, N., Jouaiti, A., Abdelaziz, H. & Wais, M. (2005). <italic>CrystEngComm</italic>, <bold>7</bold>, 624–628.</mixed-citation></ref><ref id="bb5"><mixed-citation publication-type="other">Sheldrick, G. M. (1996). <italic>SADABS</italic>, University of Göttingen, Germany.</mixed-citation></ref><ref id="bb6"><mixed-citation publication-type="other">Sheldrick, G. M. (2008). <italic>Acta Cryst.</italic> A<bold>64</bold>, 112–122.</mixed-citation></ref></ref-list></back><floats-group><table-wrap id="table1" position="float"><label>Table 1</label><caption><title>Hydrogen-bond geometry (Å, °)</title></caption><table frame="hsides" rules="groups"><thead valign="bottom"><tr><th style="border-bottom:1px solid black;" rowspan="1" colspan="1" align="left" valign="bottom"><italic>D</italic>—H⋯<italic>A</italic></th><th style="border-bottom:1px solid black;" rowspan="1" colspan="1" align="left" valign="bottom"><italic>D</italic>—H</th><th style="border-bottom:1px solid black;" rowspan="1" colspan="1" align="left" valign="bottom">H⋯<italic>A</italic></th><th style="border-bottom:1px solid black;" rowspan="1" colspan="1" align="left" valign="bottom"><italic>D</italic>⋯<italic>A</italic></th><th style="border-bottom:1px solid black;" rowspan="1" colspan="1" align="left" valign="bottom"><italic>D</italic>—H⋯<italic>A</italic></th></tr></thead><tbody valign="top"><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">O1<italic>W</italic>—H1<italic>WA</italic>⋯N2</td><td style="" rowspan="1" colspan="1" align="left" valign="top">0.874 (16)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">2.084 (17)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">2.950 (2)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">171 (2)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">O1<italic>W</italic>—H1<italic>WB</italic>⋯O2<italic>W</italic><sup>i</sup></td><td style="" rowspan="1" colspan="1" align="left" valign="top">0.884 (16)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">2.007 (18)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">2.838 (3)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">156 (2)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">O2<italic>W</italic>—H2<italic>WA</italic>⋯O1<italic>W</italic></td><td style="" rowspan="1" colspan="1" align="left" valign="top">0.921 (17)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">1.958 (19)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">2.844 (3)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">161 (3)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">O2<italic>W</italic>—H2<italic>WB</italic>⋯Cl1<sup>ii</sup></td><td style="" rowspan="1" colspan="1" align="left" valign="top">0.912 (17)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">2.272 (18)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">3.1607 (17)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">165 (3)</td></tr></tbody></table><table-wrap-foot><p>Symmetry codes: (i) <inline-formula><inline-graphic xlink:href="e-65-0m947-efi9.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula>; (ii) <inline-formula><inline-graphic xlink:href="e-65-0m947-efi10.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula>.</p></table-wrap-foot></table-wrap></floats-group></pmc></record>Pour manipuler ce document sous Unix (Dilib)
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