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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Redetermination of <italic>cyclo</italic>-tetrakis(μ-5,10,15,20-tetra-4-pyridylporphyrinato)tetrazinc(II) dimethylformamide octasolvate trihydrate at 100 K</title><author><name sortKey="Seidel, Rudiger W" sort="Seidel, Rudiger W" uniqKey="Seidel R" first="Rüdiger W." last="Seidel">Rüdiger W. Seidel</name><affiliation><nlm:aff id="a">Lehrstuhl für Analytische Chemie, Ruhr-Universität Bochum, Universitätsstrasse 150, 44780 Bochum,<country>Germany</country></nlm:aff></affiliation></author><author><name sortKey="Graf, Jurgen" sort="Graf, Jurgen" uniqKey="Graf J" first="Jürgen" last="Graf">Jürgen Graf</name><affiliation><nlm:aff id="b">Incoatec GmbH, Max-Planck-Strasse 2, 21502 Geesthacht,<country>Germany</country></nlm:aff></affiliation></author><author><name sortKey="Goddard, Richard" sort="Goddard, Richard" uniqKey="Goddard R" first="Richard" last="Goddard">Richard Goddard</name><affiliation><nlm:aff id="c">Max-Planck-Institut für Kohlenforschung, Kaiser-Wilhelm-Platz 1, 45470 Mülheim an der Ruhr,<country>Germany</country></nlm:aff></affiliation></author><author><name sortKey="Oppel, Iris M" sort="Oppel, Iris M" uniqKey="Oppel I" first="Iris M." last="Oppel">Iris M. Oppel</name><affiliation><nlm:aff id="d">Institut für Anorganische Chemie, Rheinisch-Westfälische Technische Hochschule Aachen, Landoltweg 1, 52074 Aachen,<country>Germany</country></nlm:aff></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">PMC</idno><idno type="pmid">21522892</idno><idno type="pmc">3051794</idno><idno type="url">http://www.ncbi.nlm.nih.gov/pmc/articles/PMC3051794</idno><idno type="RBID">PMC:3051794</idno><idno type="doi">10.1107/S1600536811002054</idno><date when="2011">2011</date><idno type="wicri:Area/Pmc/Corpus">000A02</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Corpus" wicri:corpus="PMC">000A02</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en" level="a" type="main">Redetermination of <italic>cyclo</italic>-tetrakis(μ-5,10,15,20-tetra-4-pyridylporphyrinato)tetrazinc(II) dimethylformamide octasolvate trihydrate at 100 K</title><author><name sortKey="Seidel, Rudiger W" sort="Seidel, Rudiger W" uniqKey="Seidel R" first="Rüdiger W." last="Seidel">Rüdiger W. Seidel</name><affiliation><nlm:aff id="a">Lehrstuhl für Analytische Chemie, Ruhr-Universität Bochum, Universitätsstrasse 150, 44780 Bochum,<country>Germany</country></nlm:aff></affiliation></author><author><name sortKey="Graf, Jurgen" sort="Graf, Jurgen" uniqKey="Graf J" first="Jürgen" last="Graf">Jürgen Graf</name><affiliation><nlm:aff id="b">Incoatec GmbH, Max-Planck-Strasse 2, 21502 Geesthacht,<country>Germany</country></nlm:aff></affiliation></author><author><name sortKey="Goddard, Richard" sort="Goddard, Richard" uniqKey="Goddard R" first="Richard" last="Goddard">Richard Goddard</name><affiliation><nlm:aff id="c">Max-Planck-Institut für Kohlenforschung, Kaiser-Wilhelm-Platz 1, 45470 Mülheim an der Ruhr,<country>Germany</country></nlm:aff></affiliation></author><author><name sortKey="Oppel, Iris M" sort="Oppel, Iris M" uniqKey="Oppel I" first="Iris M." last="Oppel">Iris M. Oppel</name><affiliation><nlm:aff id="d">Institut für Anorganische Chemie, Rheinisch-Westfälische Technische Hochschule Aachen, Landoltweg 1, 52074 Aachen,<country>Germany</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="2011">2011</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en"><p>The structure of the title compound, [Zn<sub>4</sub>(C<sub>40</sub>H<sub>24</sub>N<sub>8</sub>)<sub>4</sub>]·8C<sub>3</sub>H<sub>7</sub>NO·3H<sub>2</sub>O, has been redetermined at 100 K. The redetermination is of significantly higher precision and gives further insight into the disorder of pyridyl groups and solvent molecules. The molecules of (5,10,15,20-tetra-4-pyridylporphyrinato)zinc(II) (ZnTPyP) form homomolecular cyclic tetramers by coordination of a peripheral pyridyl group to the central Zn atom of an adjacent symmetry-related molecule. The tetramer so formed exhibits molecular <italic>S</italic><sub>4</sub> symmetry and is located about a crystallographic fourfold rotoinversion axis. Severely disordered dimethylformamide and water molecules are present in the crystal, the contributions of which were omitted from refinement. Intermolecular C—H⋯N hydrogen bonding is observed.</p></div></front><back><div1 type="bibliography"><listBibl><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><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">21522892</article-id><article-id pub-id-type="pmc">3051794</article-id><article-id pub-id-type="publisher-id">bv2170</article-id><article-id pub-id-type="doi">10.1107/S1600536811002054</article-id><article-id pub-id-type="coden">ACSEBH</article-id><article-id pub-id-type="pii">S1600536811002054</article-id><article-categories><subj-group subj-group-type="heading"><subject>Metal-Organic Papers</subject></subj-group></article-categories><title-group><article-title>Redetermination of <italic>cyclo</italic>-tetrakis(μ-5,10,15,20-tetra-4-pyridylporphyrinato)tetrazinc(II) dimethylformamide octasolvate trihydrate at 100 K</article-title><alt-title><italic>[Zn<sub>4</sub>(C<sub>40</sub>H<sub>24</sub>N<sub>8</sub>)<sub>4</sub>]·8C<sub>3</sub>H<sub>7</sub>NO·3H<sub>2</sub>O</italic></alt-title></title-group><contrib-group><contrib contrib-type="author"><name><surname>Seidel</surname><given-names>Rüdiger W.</given-names></name><xref ref-type="aff" rid="a">a</xref><xref ref-type="corresp" rid="cor">*</xref></contrib><contrib contrib-type="author"><name><surname>Graf</surname><given-names>Jürgen</given-names></name><xref ref-type="aff" rid="b">b</xref></contrib><contrib contrib-type="author"><name><surname>Goddard</surname><given-names>Richard</given-names></name><xref ref-type="aff" rid="c">c</xref></contrib><contrib contrib-type="author"><name><surname>Oppel</surname><given-names>Iris M.</given-names></name><xref ref-type="aff" rid="d">d</xref></contrib><aff id="a"><label>a</label>Lehrstuhl für Analytische Chemie, Ruhr-Universität Bochum, Universitätsstrasse 150, 44780 Bochum,<country>Germany</country></aff><aff id="b"><label>b</label>Incoatec GmbH, Max-Planck-Strasse 2, 21502 Geesthacht,<country>Germany</country></aff><aff id="c"><label>c</label>Max-Planck-Institut für Kohlenforschung, Kaiser-Wilhelm-Platz 1, 45470 Mülheim an der Ruhr,<country>Germany</country></aff><aff id="d"><label>d</label>Institut für Anorganische Chemie, Rheinisch-Westfälische Technische Hochschule Aachen, Landoltweg 1, 52074 Aachen,<country>Germany</country></aff></contrib-group><author-notes><corresp id="cor">Correspondence e-mail: <email>Ruediger.Seidel@rub.de</email></corresp></author-notes><pub-date pub-type="collection"><day>01</day><month>2</month><year>2011</year></pub-date><pub-date pub-type="epub"><day>22</day><month>1</month><year>2011</year></pub-date><pub-date pub-type="pmc-release"><day>22</day><month>1</month><year>2011</year></pub-date><pmc-comment> PMC Release delay is 0 months and 0 days and was based on the
<volume>67</volume><issue>Pt 2</issue><issue-id pub-id-type="publisher-id">e110200</issue-id><fpage>m236</fpage><lpage>m237</lpage><history><date date-type="received"><day>02</day><month>12</month><year>2010</year></date><date date-type="accepted"><day>13</day><month>1</month><year>2011</year></date></history><permissions><copyright-statement>© Seidel et al. 2011</copyright-statement><copyright-year>2011</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/S1600536811002054">A full version of this article is available from Crystallography Journals Online.</self-uri><abstract><p>The structure of the title compound, [Zn<sub>4</sub>(C<sub>40</sub>H<sub>24</sub>N<sub>8</sub>)<sub>4</sub>]·8C<sub>3</sub>H<sub>7</sub>NO·3H<sub>2</sub>O, has been redetermined at 100 K. The redetermination is of significantly higher precision and gives further insight into the disorder of pyridyl groups and solvent molecules. The molecules of (5,10,15,20-tetra-4-pyridylporphyrinato)zinc(II) (ZnTPyP) form homomolecular cyclic tetramers by coordination of a peripheral pyridyl group to the central Zn atom of an adjacent symmetry-related molecule. The tetramer so formed exhibits molecular <italic>S</italic><sub>4</sub> symmetry and is located about a crystallographic fourfold rotoinversion axis. Severely disordered dimethylformamide and water molecules are present in the crystal, the contributions of which were omitted from refinement. Intermolecular C—H⋯N hydrogen bonding is observed.</p></abstract></article-meta></front><body><sec id="sec1"><title>Related literature</title><p>For the structure at 200 K, see: Seidel <italic>et al.</italic> (2010<xref ref-type="bibr" rid="bb10"> ▶</xref>). For the 2-chlorophenol solvate of cyclic tetrameric ZnTPyP, see: Lipstman & Goldberg (2010<xref ref-type="bibr" rid="bb8"> ▶</xref>). For a review article on structural motifs in coordination polymers of the 5,10,15,20-tetra4-pyridylporphyrin ligand, see: DeVries & Choe (2009<xref ref-type="bibr" rid="bb5"> ▶</xref>). For the supramolecular chemistry of ZnTPyP in the solid-state, see: Lipstman & Goldberg (2010<xref ref-type="bibr" rid="bb8"> ▶</xref>); Seidel <italic>et al.</italic> (2010<xref ref-type="bibr" rid="bb10"> ▶</xref>) and references cited therein. For a description of the IμS microfocus X-ray source used in the present study, see: Graf (2008<xref ref-type="bibr" rid="bb7"> ▶</xref>); Schulz <italic>et al.</italic> (2009<xref ref-type="bibr" rid="bb9"> ▶</xref>). For <italic>PLATON</italic> / <italic>SQUEEZE</italic>, see: van der Sluis & Spek (1990<xref ref-type="bibr" rid="bb12"> ▶</xref>); Spek (2009<xref ref-type="bibr" rid="bb13"> ▶</xref>). For a description of the program <italic>COOT</italic>, see: Emsley <italic>et al.</italic> (2010<xref ref-type="bibr" rid="bb6"> ▶</xref>).<chem-struct id="scheme1"><graphic xlink:href="e-67-0m236-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>[Zn<sub>4</sub>(C<sub>40</sub>H<sub>24</sub>N<sub>8</sub>)<sub>4</sub>]·8C<sub>3</sub>H<sub>7</sub>NO·3H<sub>2</sub>O</p></list-item><list-item><p><italic>M</italic><italic><sub>r</sub></italic> = 3366.98</p></list-item><list-item><p>Tetragonal, <inline-formula><inline-graphic xlink:href="e-67-0m236-efi3.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula></p></list-item><list-item><p><italic>a</italic> = 23.6897 (5) Å</p></list-item><list-item><p><italic>c</italic> = 14.9876 (7) Å</p></list-item><list-item><p><italic>V</italic> = 8411.1 (5) Å<sup>3</sup></p></list-item><list-item><p><italic>Z</italic> = 2</p></list-item><list-item><p>Cu <italic>K</italic>α radiation</p></list-item><list-item><p>μ = 1.24 mm<sup>−1</sup></p></list-item><list-item><p><italic>T</italic> = 100 K</p></list-item><list-item><p>0.16 × 0.04 × 0.02 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 X8 PROSPECTOR diffractometer</p></list-item><list-item><p>Absorption correction: multi-scan (<italic>SADABS</italic>; Bruker, 2008<xref ref-type="bibr" rid="bb3"> ▶</xref>) <italic>T</italic><sub>min</sub> = 0.827, <italic>T</italic><sub>max</sub> = 0.976</p></list-item><list-item><p>44415 measured reflections</p></list-item><list-item><p>7723 independent reflections</p></list-item><list-item><p>6768 reflections with <italic>I</italic> > 2σ(<italic>I</italic>)</p></list-item><list-item><p><italic>R</italic><sub>int</sub> = 0.018</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>)] = 0.042</p></list-item><list-item><p><italic>wR</italic>(<italic>F</italic><sup>2</sup>) = 0.108</p></list-item><list-item><p><italic>S</italic> = 1.04</p></list-item><list-item><p>7723 reflections</p></list-item><list-item><p>442 parameters</p></list-item><list-item><p>H-atom parameters constrained</p></list-item><list-item><p>Δρ<sub>max</sub> = 0.59 e Å<sup>−3</sup></p></list-item><list-item><p>Δρ<sub>min</sub> = −0.42 e Å<sup>−3</sup></p></list-item></list></p></sec></sec><sec id="d5e709"><title></title><p>Data collection: <italic>APEX2</italic> (Bruker, 2008<xref ref-type="bibr" rid="bb3"> ▶</xref>); cell refinement: <italic>SAINT</italic> (Bruker, 2010<xref ref-type="bibr" rid="bb4"> ▶</xref>); data reduction: <italic>SAINT</italic>; program(s) used to solve structure: <italic>SHELXS97</italic> (Sheldrick, 2008<xref ref-type="bibr" rid="bb11"> ▶</xref>); program(s) used to refine structure: <italic>SHELXL97</italic> (Sheldrick, 2008<xref ref-type="bibr" rid="bb11"> ▶</xref>); molecular graphics: <italic>DIAMOND</italic> (Brandenburg, 2010<xref ref-type="bibr" rid="bb2"> ▶</xref>); software used to prepare material for publication: <italic>enCIFer</italic> (Allen <italic>et al.</italic>, 2004<xref ref-type="bibr" rid="bb1"> ▶</xref>).</p></sec></sec><sec sec-type="supplementary-material"><title>Supplementary Material</title><supplementary-material content-type="local-data" xlink:href="e-67-0m236-sup1.cif" position="float" xlink:type="simple"><p>Crystal structure: contains datablocks global, I. DOI: <ext-link ext-link-type="uri" xlink:type="simple" xlink:href="http://dx.doi.org/10.1107/S1600536811002054/bv2170sup1.cif">10.1107/S1600536811002054/bv2170sup1.cif</ext-link></p><media mimetype="chemical" mime-subtype="x-cif" xlink:href="e-67-0m236-sup1.cif" position="float" xlink:type="simple"></media></supplementary-material><supplementary-material content-type="local-data" xlink:href="e-67-0m236-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/S1600536811002054/bv2170Isup2.hkl">10.1107/S1600536811002054/bv2170Isup2.hkl</ext-link></p><media mimetype="text" mime-subtype="plain" xlink:href="e-67-0m236-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?bv2170&file=bv2170sup0.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?bv2170sup1&Qmime=cif" xlink:type="simple">3D view</ext-link>; <ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/paper?bv2170&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?bv2170">BV2170</ext-link>).</p></fn></fn-group><ack><p>The Deutsche Forschungsgemeinschaft (DFG) is acknowledged for financial support. RWS is grateful to Professor William S. Sheldrick and Professor Christian W. Lehmann for generous support.</p></ack><app-group><app><title>supplementary crystallographic
information</title><sec id="comment"><title>Comment </title><p>5,10,15,20-Tetra(4-pyridyl)porphyrin has been widely used as ligand for the
construction of coordination polymers (DeVries & Choe, 2009). We and
others
have reported on the solid-state supramolecular chemistry of the
self-complementary [5,10,15,20-tetra(4-pyridyl)porphyrinato]zinc(II) (ZnTPyP)
building block (Lipstman & Goldberg, 2010; Seidel <italic>et al.</italic>,
2010 and
references cited therein). Recently, we reported the title structure of
[ZnTPyP]<sub>4</sub>.</p><p>The small dark red plate-shaped crystals of the title compound were subjected
to diffraction experiments using a Bruker AXS X8 PROSPECTOR diffractometer
equipped with an INCOATEC microfocus X-ray source (IµS) for Cu radiation
(Graf, 2008). Such microfocus X-ray sources use multilayer mirrors to
focus
the X-ray beam onto the crystal and, therefore, lead to a significant
reduction of the background and an increase in diffracted intensities. It has
already been demonstrated that the Mo IµS gives data of significantly higher
quality than a 2 kW Mo fine focus sealed tube, when small crystals are
examined (Schulz <italic>et al.</italic>, 2009). The data collection presented
here,
using the Cu IµS, resulted in intensity data of surprisingly good quality
and, hence, indicated a re-refinement of the crystal structure. The crystals
investigated in the original work were significantly larger than those
examined in the present study and split on cooling to 100 K. For this
reason, the data were collected at 200 K with a Cu rotating anode system at
that time. Using small crystals has the advantage that these are less likely
to split on flash cooling.</p><p>The molecular structure of [ZnTPyP]<sub>4</sub> is depicted in Fig. 1. The asymmetric
unit contains one ZnTPyP unit (Fig 2.) and the <italic>S</italic><sub>4</sub> symmetric tetramer
is generated by crystallographic fourfold rotoinversion symmetry. One
peripheral pyridyl group binds to the central Zn atom of an adjacent symmetry
related ZnTPyP unit. Zn1 is pentacoordinated and is displaced from the N<sub>4</sub>mean plane by 0.3196 (9) Å. The coordination geometry parameters about Zn1
are given in Table 1. The three remaining pyridyl groups are non-coordinating.
Even at 100 K, the pyridyl groups attached to C5 and C15 show elongated
ellipsoids, which cause a checkCIF B level alert (Spek, 2009) due to
large
<italic>U</italic><sub>eq</sub>(max)/<italic>U</italic><sub>eq</sub>(min) ratio. This reveals that the disorder is
rather of static than dynamic nature. Attempts were made to describe the
electron density of the pyridyl ring attached to C15 (Fig. 3) by a split
model. However, the refinement results could not be improved thereby. Thus,
both pyridyl rings were finally described with large displacement parameters.</p><p>In the crystal, the [ZnTPyP]<sub>4</sub> entities are stacked into columns located at
<italic>x</italic> = 1/4, <italic>y</italic> = 1/4 and <italic>x</italic> = 3/4, <italic>y</italic> = 3/4 (Fig 4). The
stacking propagates <italic>via</italic> C<sub>β</sub>—H···N<sub>py</sub> interactions (see Table 2) by
translational symmetry in the <italic>c</italic> axis direction. Within a column, the
distance between the centroids of the pyridyl rings attached to C5 and
C15<sup>iii</sup> is 4.0714 (1) Å. Adjacent columns of [ZnTPyP]<sub>4</sub> are arranged with
an offset of <italic>c</italic>/2 (<italic>ca</italic> 7.49 Å). Interstitial channels are formed
parallel to the <italic>c</italic> axis direction centred at <italic>x</italic> = 1/4, <italic>y</italic> =
3/4 and <italic>x</italic> = 3/4, <italic>y</italic> = 1/4 (Fig 5). The potential solvent
accessible void estimated with <italic>PLATON</italic> / <italic>SOLV</italic> (Spek, 2009)
is
33.2% of the unit cell volume. On cooling to 100 K, the <italic>a</italic> lattice
vector is shortened by approximately 0.27 Å in comparison to the tetragonal
unit cell at 200 K (<italic>a</italic> = 23.958 (2) Å), whereas the length of <italic>c</italic>lattice vector remains relatively unaffected (<italic>c</italic> = 15.0646 (16) Å at
200 K; Seidel <italic>et al.</italic>, 2010).</p><p>Despite intensive efforts, the disordered solvent molecules filling the voids
within the columns of [ZnTPyP]<sub>4</sub> and the interstitial channels could not be
modeled reasonably with the data collected at 100 K. Nevertheless, residual
electron density was visible in a difference Fourier synthesis calculated for
the solvent regions (Fig. 6) with phases based on the model using <italic>COOT</italic>(Emsley <italic>et al.</italic>, 2010). For the visualization of the surface of
the
(difference) electron density using a three-dimensional mesh, the electron
densities should be read into <italic>COOT</italic> in terms of structure factors. To
obtain a structure factor (.fcf) file containg the informations necessary for
the calculation of electron density maps and suitable for <italic>COOT</italic>, the
LIST 6 instruction of <italic>SHELXL-97</italic> was used. The atomic model of the
framework was read into <italic>COOT</italic> by means of the <italic>SHELXL-97</italic>. res
file. The visual inspection of the difference electron density map indicates
that four molecules of dimethylformamide (DMF) plus one water molecule are
located within the voids in the columns approximately centred at (1/4,1/4,0),
whereas another four molecules of DMF and two water molecules are clustered
around the 4<sub>2</sub> screw axes running through the interstitial channels parallel
to the <italic>c</italic> axis direction. The compound can, therefore, probably best be
described as [ZnTPyP]<sub>4</sub>. 8 DMF. 3 H<sub>2</sub>O. The compound was originally
formulated as being a pure DMF solvate (Seidel <italic>et al.</italic>, 2010). To
improve the fit of the model to the data and, hence, the precision of the main
part of the structure, the contributions of the disordered solvent molecules
were removed from the diffraction data with <italic>PLATON</italic> / <italic>SQUEEZE</italic>(van der Sluis & Spek, 1990; Spek, 2009). <italic>SQUEEZE</italic>estimated the
electron counts in the voids within the columns and interstitial channels of
[ZnTPyP]<sub>4</sub> to be 182 and 207, respectively. These values are relatively close
to those based on the proposed chemical formula (178 and 196).</p></sec><sec id="experimental"><title>Experimental </title><p>Small dark red plate-shaped crystals of the title compound were obtained
similarly as reported previously (Seidel <italic>et al.</italic>, 2010); 12 mg of
ZnTPyP
(Aldrich) and 11 mg of [Pd(NO<sub>3</sub>)<sub>2</sub>(en)] (en = 1,2-diaminoethane) were placed
in an ampoule and 4 ml of DMF were added. The ampoule was sealed and placed in
a heater. The sample was heated to 150 °C in 24 h and held for five days at
this temperature. Subsequently, the sample was cooled down to room temperature
in 100 h. Noteworthy, the crystals of the title compound were accompanied by
crystals of the triclinic phase, containing a polymeric one-dimensional ladder
structure of ZnTPyP, as observed previously (Seidel <italic>et al.</italic>,
2010).</p></sec><sec id="refinement"><title>Refinement </title><p>For the final refinement, the contributions of severely disordered DMF and water
molecules of crystallization were removed from the diffraction data with
<italic>PLATON</italic> / <italic>SQUEEZE</italic> (van der Sluis & Spek, 1990; Spek,
2009), see
comment. H atoms were placed at geometrically calculated positions and refined
with constrained C—H bond length of 0.95 Å and <italic>U</italic><sub>iso</sub>(H) = 1.2
<italic>U</italic><sub>eq</sub>(C) allowing them to ride on the parent C atom.</p></sec><sec id="figures"><title>Figures</title><fig id="Fap1"><label>Fig. 1.</label><caption><p>Molecular structure of the title compound. H atoms are omitted for clarity.</p></caption><graphic xlink:href="e-67-0m236-fig1"></graphic></fig><fig id="Fap2"><label>Fig. 2.</label><caption><p>Displacement ellipsoid plot of one repeat unit of cyclic [ZnTPyP]4 drawn at 50% probability. H atoms are omitted for clarity. Symmetry code: (i) y, -x + 1/2, -z + 1/2.</p></caption><graphic xlink:href="e-67-0m236-fig2"></graphic></fig><fig id="Fap3"><label>Fig. 3.</label><caption><p>Contour plot of the Fo electron density map in the plane of the pyridyl group attached to C15, calculated with phases from Fc. Contours are drawn at 0.50 e Å-3 starting at 6.00 e Å-3. The contour plot was generated with PLATON (Spek, 2009).</p></caption><graphic xlink:href="e-67-0m236-fig3"></graphic></fig><fig id="Fap4"><label>Fig. 4.</label><caption><p>Stacking of the [ZnTPyP]4 entities viewed along the a axis direction. H atoms are omitted for clarity. Cβ—H···Npy interactions are represented by dashed lines.</p></caption><graphic xlink:href="e-67-0m236-fig4"></graphic></fig><fig id="Fap5"><label>Fig. 5.</label><caption><p>Packing diagram of the title compound projected along the c axis direction. H atoms are omitted for clarity.</p></caption><graphic xlink:href="e-67-0m236-fig5"></graphic></fig><fig id="Fap6"><label>Fig. 6.</label><caption><p>The tetragonal unit cell of the title compound viewed approximately along the c axis direction showing the Fo-Fc map of the disordered solvent regions (contoured at 3.0σ level). The figure was created with COOT (Emsley et al., 2010) using Fo including the contributions of the disordered solvent with phases from Fc based on the model.</p></caption><graphic xlink:href="e-67-0m236-fig6"></graphic></fig></sec><sec id="tablewrapcrystaldatalong"><title>Crystal data</title><table-wrap position="anchor" id="d1e401"><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">[Zn<sub>4</sub>(C<sub>40</sub>H<sub>24</sub>N<sub>8</sub>)<sub>4</sub>]·8C<sub>3</sub>H<sub>7</sub>NO·3H<sub>2</sub>O</td><td rowspan="1" colspan="1"><italic>D</italic><sub>x</sub> = 1.329 Mg m<sup>−</sup><sup>3</sup></td></tr><tr><td rowspan="1" colspan="1"><italic>M</italic><italic><sub>r</sub></italic> = 3366.98</td><td rowspan="1" colspan="1">Cu <italic>K</italic>α radiation, λ = 1.54178 Å</td></tr><tr><td rowspan="1" colspan="1">Tetragonal, <italic>P</italic>4<sub>2</sub>/<italic>n</italic></td><td rowspan="1" colspan="1">Cell parameters from 130 reflections</td></tr><tr><td rowspan="1" colspan="1">Hall symbol: -P 4bc</td><td rowspan="1" colspan="1">θ = 3.5–31.5°</td></tr><tr><td rowspan="1" colspan="1"><italic>a</italic> = 23.6897 (5) Å</td><td rowspan="1" colspan="1">µ = 1.24 mm<sup>−</sup><sup>1</sup></td></tr><tr><td rowspan="1" colspan="1"><italic>c</italic> = 14.9876 (7) Å</td><td rowspan="1" colspan="1"><italic>T</italic> = 100 K</td></tr><tr><td rowspan="1" colspan="1"><italic>V</italic> = 8411.1 (5) Å<sup>3</sup></td><td rowspan="1" colspan="1">Plate, dark red</td></tr><tr><td rowspan="1" colspan="1"><italic>Z</italic> = 2</td><td rowspan="1" colspan="1">0.16 × 0.04 × 0.02 mm</td></tr><tr><td rowspan="1" colspan="1"><italic>F</italic>(000) = 3500</td><td rowspan="1" colspan="1"></td></tr></table></table-wrap></sec><sec id="tablewrapdatacollectionlong"><title>Data collection</title><table-wrap position="anchor" id="d1e536"><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 X8 PROSPECTOR goniometer diffractometer</td><td rowspan="1" colspan="1">7723 independent reflections</td></tr><tr><td rowspan="1" colspan="1">Radiation source: Incoatec IµS microfocus X-ray source</td><td rowspan="1" colspan="1">6768 reflections with <italic>I</italic> > 2σ(<italic>I</italic>)</td></tr><tr><td rowspan="1" colspan="1">Incoatec Quazar Multilayer Mirror</td><td rowspan="1" colspan="1"><italic>R</italic><sub>int</sub> = 0.018</td></tr><tr><td rowspan="1" colspan="1">Detector resolution: 8.33 pixels mm<sup>-1</sup></td><td rowspan="1" colspan="1">θ<sub>max</sub> = 69.2°, θ<sub>min</sub> = 2.6°</td></tr><tr><td rowspan="1" colspan="1">ω scans</td><td rowspan="1" colspan="1"><italic>h</italic> = −28→25</td></tr><tr><td rowspan="1" colspan="1">Absorption correction: multi-scan (<italic>SADABS</italic>; Bruker, 2008)</td><td rowspan="1" colspan="1"><italic>k</italic> = −24→28</td></tr><tr><td rowspan="1" colspan="1"><italic>T</italic><sub>min</sub> = 0.827, <italic>T</italic><sub>max</sub> = 0.976</td><td rowspan="1" colspan="1"><italic>l</italic> = −17→14</td></tr><tr><td rowspan="1" colspan="1">44415 measured reflections</td><td rowspan="1" colspan="1"></td></tr></table></table-wrap></sec><sec id="tablewraprefinementdatalong"><title>Refinement</title><table-wrap position="anchor" id="d1e656"><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>)] = 0.042</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>) = 0.108</td><td rowspan="1" colspan="1">H-atom parameters constrained</td></tr><tr><td rowspan="1" colspan="1"><italic>S</italic> = 1.04</td><td rowspan="1" colspan="1"><italic>w</italic> = 1/[σ<sup>2</sup>(<italic>F</italic><sub>o</sub><sup>2</sup>) + (0.0472<italic>P</italic>)<sup>2</sup> + 5.0454<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">7723 reflections</td><td rowspan="1" colspan="1">(Δ/σ)<sub>max</sub> < 0.001</td></tr><tr><td rowspan="1" colspan="1">442 parameters</td><td rowspan="1" colspan="1">Δρ<sub>max</sub> = 0.59 e Å<sup>−</sup><sup>3</sup></td></tr><tr><td rowspan="1" colspan="1">0 restraints</td><td rowspan="1" colspan="1">Δρ<sub>min</sub> = −0.42 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="d1e813"><table rules="all" frame="box" style="table-layout:fixed"><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="d1e912"><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">Zn1</td><td rowspan="1" colspan="1">0.350673 (11)</td><td rowspan="1" colspan="1">0.520064 (11)</td><td rowspan="1" colspan="1">0.185590 (16)</td><td rowspan="1" colspan="1">0.03823 (9)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N21</td><td rowspan="1" colspan="1">0.38601 (8)</td><td rowspan="1" colspan="1">0.54998 (7)</td><td rowspan="1" colspan="1">0.06850 (10)</td><td rowspan="1" colspan="1">0.0433 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N22</td><td rowspan="1" colspan="1">0.27781 (7)</td><td rowspan="1" colspan="1">0.50134 (7)</td><td rowspan="1" colspan="1">0.11541 (10)</td><td rowspan="1" colspan="1">0.0404 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N23</td><td rowspan="1" colspan="1">0.41242 (7)</td><td rowspan="1" colspan="1">0.56428 (7)</td><td rowspan="1" colspan="1">0.25451 (10)</td><td rowspan="1" colspan="1">0.0404 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N24</td><td rowspan="1" colspan="1">0.30440 (7)</td><td rowspan="1" colspan="1">0.51392 (7)</td><td rowspan="1" colspan="1">0.30222 (10)</td><td rowspan="1" colspan="1">0.0377 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C1</td><td rowspan="1" colspan="1">0.46288 (9)</td><td rowspan="1" colspan="1">0.58336 (8)</td><td rowspan="1" colspan="1">0.22081 (13)</td><td rowspan="1" colspan="1">0.0420 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C2</td><td rowspan="1" colspan="1">0.50033 (10)</td><td rowspan="1" colspan="1">0.59793 (10)</td><td rowspan="1" colspan="1">0.29314 (14)</td><td rowspan="1" colspan="1">0.0532 (6)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H2</td><td rowspan="1" colspan="1">0.5379</td><td rowspan="1" colspan="1">0.6115</td><td rowspan="1" colspan="1">0.2880</td><td rowspan="1" colspan="1">0.064*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C3</td><td rowspan="1" colspan="1">0.47175 (10)</td><td rowspan="1" colspan="1">0.58861 (10)</td><td rowspan="1" colspan="1">0.36945 (15)</td><td rowspan="1" colspan="1">0.0534 (6)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H3</td><td rowspan="1" colspan="1">0.4853</td><td rowspan="1" colspan="1">0.5949</td><td rowspan="1" colspan="1">0.4283</td><td rowspan="1" colspan="1">0.064*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C4</td><td rowspan="1" colspan="1">0.41675 (9)</td><td rowspan="1" colspan="1">0.56739 (9)</td><td rowspan="1" colspan="1">0.34544 (13)</td><td rowspan="1" colspan="1">0.0428 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C5</td><td rowspan="1" colspan="1">0.37497 (9)</td><td rowspan="1" colspan="1">0.55138 (9)</td><td rowspan="1" colspan="1">0.40720 (13)</td><td rowspan="1" colspan="1">0.0442 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C6</td><td rowspan="1" colspan="1">0.32280 (9)</td><td rowspan="1" colspan="1">0.52641 (9)</td><td rowspan="1" colspan="1">0.38657 (12)</td><td rowspan="1" colspan="1">0.0411 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C7</td><td rowspan="1" colspan="1">0.28126 (9)</td><td rowspan="1" colspan="1">0.50864 (9)</td><td rowspan="1" colspan="1">0.45108 (13)</td><td rowspan="1" colspan="1">0.0451 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H7</td><td rowspan="1" colspan="1">0.2835</td><td rowspan="1" colspan="1">0.5130</td><td rowspan="1" colspan="1">0.5140</td><td rowspan="1" colspan="1">0.054*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C8</td><td rowspan="1" colspan="1">0.23852 (9)</td><td rowspan="1" colspan="1">0.48459 (9)</td><td rowspan="1" colspan="1">0.40491 (13)</td><td rowspan="1" colspan="1">0.0422 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H8</td><td rowspan="1" colspan="1">0.2052</td><td rowspan="1" colspan="1">0.4684</td><td rowspan="1" colspan="1">0.4292</td><td rowspan="1" colspan="1">0.051*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C9</td><td rowspan="1" colspan="1">0.25323 (8)</td><td rowspan="1" colspan="1">0.48825 (8)</td><td rowspan="1" colspan="1">0.31165 (12)</td><td rowspan="1" colspan="1">0.0362 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C10</td><td rowspan="1" colspan="1">0.21846 (8)</td><td rowspan="1" colspan="1">0.46994 (8)</td><td rowspan="1" colspan="1">0.24113 (12)</td><td rowspan="1" colspan="1">0.0360 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C11</td><td rowspan="1" colspan="1">0.22974 (8)</td><td rowspan="1" colspan="1">0.47834 (8)</td><td rowspan="1" colspan="1">0.14991 (12)</td><td rowspan="1" colspan="1">0.0376 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C12</td><td rowspan="1" colspan="1">0.19052 (9)</td><td rowspan="1" colspan="1">0.46543 (9)</td><td rowspan="1" colspan="1">0.07858 (13)</td><td rowspan="1" colspan="1">0.0460 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H12</td><td rowspan="1" colspan="1">0.1543</td><td rowspan="1" colspan="1">0.4486</td><td rowspan="1" colspan="1">0.0845</td><td rowspan="1" colspan="1">0.055*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C13</td><td rowspan="1" colspan="1">0.21544 (10)</td><td rowspan="1" colspan="1">0.48202 (10)</td><td rowspan="1" colspan="1">0.00230 (14)</td><td rowspan="1" colspan="1">0.0526 (6)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H13</td><td rowspan="1" colspan="1">0.1998</td><td rowspan="1" colspan="1">0.4794</td><td rowspan="1" colspan="1">−0.0559</td><td rowspan="1" colspan="1">0.063*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C14</td><td rowspan="1" colspan="1">0.26979 (9)</td><td rowspan="1" colspan="1">0.50435 (10)</td><td rowspan="1" colspan="1">0.02480 (13)</td><td rowspan="1" colspan="1">0.0477 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C15</td><td rowspan="1" colspan="1">0.30923 (11)</td><td rowspan="1" colspan="1">0.52569 (10)</td><td rowspan="1" colspan="1">−0.03612 (14)</td><td rowspan="1" colspan="1">0.0545 (6)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C16</td><td rowspan="1" colspan="1">0.36281 (10)</td><td rowspan="1" colspan="1">0.54737 (10)</td><td rowspan="1" colspan="1">−0.01508 (13)</td><td rowspan="1" colspan="1">0.0515 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C17</td><td rowspan="1" colspan="1">0.40164 (12)</td><td rowspan="1" colspan="1">0.57099 (11)</td><td rowspan="1" colspan="1">−0.07905 (15)</td><td rowspan="1" colspan="1">0.0636 (7)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H17</td><td rowspan="1" colspan="1">0.3959</td><td rowspan="1" colspan="1">0.5743</td><td rowspan="1" colspan="1">−0.1416</td><td rowspan="1" colspan="1">0.076*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C18</td><td rowspan="1" colspan="1">0.44735 (11)</td><td rowspan="1" colspan="1">0.58736 (10)</td><td rowspan="1" colspan="1">−0.03328 (15)</td><td rowspan="1" colspan="1">0.0581 (6)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H18</td><td rowspan="1" colspan="1">0.4801</td><td rowspan="1" colspan="1">0.6046</td><td rowspan="1" colspan="1">−0.0575</td><td rowspan="1" colspan="1">0.070*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C19</td><td rowspan="1" colspan="1">0.43790 (9)</td><td rowspan="1" colspan="1">0.57411 (9)</td><td rowspan="1" colspan="1">0.05937 (13)</td><td rowspan="1" colspan="1">0.0455 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C20</td><td rowspan="1" colspan="1">0.47569 (9)</td><td rowspan="1" colspan="1">0.58754 (8)</td><td rowspan="1" colspan="1">0.12914 (13)</td><td rowspan="1" colspan="1">0.0429 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N51</td><td rowspan="1" colspan="1">0.40921 (10)</td><td rowspan="1" colspan="1">0.58630 (15)</td><td rowspan="1" colspan="1">0.68340 (15)</td><td rowspan="1" colspan="1">0.0812 (8)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C52</td><td rowspan="1" colspan="1">0.38597 (16)</td><td rowspan="1" colspan="1">0.62318 (17)</td><td rowspan="1" colspan="1">0.6300 (2)</td><td rowspan="1" colspan="1">0.0945 (11)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H52</td><td rowspan="1" colspan="1">0.3762</td><td rowspan="1" colspan="1">0.6589</td><td rowspan="1" colspan="1">0.6542</td><td rowspan="1" colspan="1">0.113*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C53</td><td rowspan="1" colspan="1">0.37466 (15)</td><td rowspan="1" colspan="1">0.61389 (13)</td><td rowspan="1" colspan="1">0.54115 (18)</td><td rowspan="1" colspan="1">0.0816 (9)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H53</td><td rowspan="1" colspan="1">0.3581</td><td rowspan="1" colspan="1">0.6429</td><td rowspan="1" colspan="1">0.5060</td><td rowspan="1" colspan="1">0.098*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C54</td><td rowspan="1" colspan="1">0.38735 (9)</td><td rowspan="1" colspan="1">0.56279 (11)</td><td rowspan="1" colspan="1">0.50349 (14)</td><td rowspan="1" colspan="1">0.0513 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C55</td><td rowspan="1" colspan="1">0.41194 (13)</td><td rowspan="1" colspan="1">0.52451 (15)</td><td rowspan="1" colspan="1">0.55825 (18)</td><td rowspan="1" colspan="1">0.0792 (8)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H55</td><td rowspan="1" colspan="1">0.4222</td><td rowspan="1" colspan="1">0.4884</td><td rowspan="1" colspan="1">0.5360</td><td rowspan="1" colspan="1">0.095*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C56</td><td rowspan="1" colspan="1">0.42214 (14)</td><td rowspan="1" colspan="1">0.53814 (18)</td><td rowspan="1" colspan="1">0.6469 (2)</td><td rowspan="1" colspan="1">0.0885 (10)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H56</td><td rowspan="1" colspan="1">0.4397</td><td rowspan="1" colspan="1">0.5105</td><td rowspan="1" colspan="1">0.6834</td><td rowspan="1" colspan="1">0.106*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N101</td><td rowspan="1" colspan="1">0.06117 (6)</td><td rowspan="1" colspan="1">0.38923 (7)</td><td rowspan="1" colspan="1">0.30189 (10)</td><td rowspan="1" colspan="1">0.0355 (3)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C102</td><td rowspan="1" colspan="1">0.06574 (8)</td><td rowspan="1" colspan="1">0.44515 (8)</td><td rowspan="1" colspan="1">0.29549 (13)</td><td rowspan="1" colspan="1">0.0403 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H102</td><td rowspan="1" colspan="1">0.0327</td><td rowspan="1" colspan="1">0.4673</td><td rowspan="1" colspan="1">0.3038</td><td rowspan="1" colspan="1">0.048*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C103</td><td rowspan="1" colspan="1">0.11567 (8)</td><td rowspan="1" colspan="1">0.47254 (8)</td><td rowspan="1" colspan="1">0.27747 (13)</td><td rowspan="1" colspan="1">0.0406 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H103</td><td rowspan="1" colspan="1">0.1167</td><td rowspan="1" colspan="1">0.5126</td><td rowspan="1" colspan="1">0.2740</td><td rowspan="1" colspan="1">0.049*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C104</td><td rowspan="1" colspan="1">0.16441 (8)</td><td rowspan="1" colspan="1">0.44146 (8)</td><td rowspan="1" colspan="1">0.26451 (11)</td><td rowspan="1" colspan="1">0.0339 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C105</td><td rowspan="1" colspan="1">0.16034 (9)</td><td rowspan="1" colspan="1">0.38345 (9)</td><td rowspan="1" colspan="1">0.27246 (17)</td><td rowspan="1" colspan="1">0.0506 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H105</td><td rowspan="1" colspan="1">0.1928</td><td rowspan="1" colspan="1">0.3604</td><td rowspan="1" colspan="1">0.2652</td><td rowspan="1" colspan="1">0.061*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C106</td><td rowspan="1" colspan="1">0.10845 (9)</td><td rowspan="1" colspan="1">0.35925 (9)</td><td rowspan="1" colspan="1">0.29112 (16)</td><td rowspan="1" colspan="1">0.0490 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H106</td><td rowspan="1" colspan="1">0.1064</td><td rowspan="1" colspan="1">0.3194</td><td rowspan="1" colspan="1">0.2965</td><td rowspan="1" colspan="1">0.059*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N151</td><td rowspan="1" colspan="1">0.2660 (2)</td><td rowspan="1" colspan="1">0.5329 (2)</td><td rowspan="1" colspan="1">−0.3142 (2)</td><td rowspan="1" colspan="1">0.1294 (17)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C152</td><td rowspan="1" colspan="1">0.2458 (3)</td><td rowspan="1" colspan="1">0.5685 (2)</td><td rowspan="1" colspan="1">−0.2569 (3)</td><td rowspan="1" colspan="1">0.155 (2)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H152</td><td rowspan="1" colspan="1">0.2211</td><td rowspan="1" colspan="1">0.5972</td><td rowspan="1" colspan="1">−0.2780</td><td rowspan="1" colspan="1">0.185*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C153</td><td rowspan="1" colspan="1">0.2581 (2)</td><td rowspan="1" colspan="1">0.56707 (18)</td><td rowspan="1" colspan="1">−0.1666 (2)</td><td rowspan="1" colspan="1">0.1290 (18)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H153</td><td rowspan="1" colspan="1">0.2421</td><td rowspan="1" colspan="1">0.5945</td><td rowspan="1" colspan="1">−0.1278</td><td rowspan="1" colspan="1">0.155*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C154</td><td rowspan="1" colspan="1">0.29319 (12)</td><td rowspan="1" colspan="1">0.52625 (14)</td><td rowspan="1" colspan="1">−0.13291 (16)</td><td rowspan="1" colspan="1">0.0729 (8)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C155</td><td rowspan="1" colspan="1">0.31337 (15)</td><td rowspan="1" colspan="1">0.4886 (2)</td><td rowspan="1" colspan="1">−0.19209 (18)</td><td rowspan="1" colspan="1">0.1009 (13)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H155</td><td rowspan="1" colspan="1">0.3375</td><td rowspan="1" colspan="1">0.4591</td><td rowspan="1" colspan="1">−0.1726</td><td rowspan="1" colspan="1">0.121*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C156</td><td rowspan="1" colspan="1">0.29872 (18)</td><td rowspan="1" colspan="1">0.4931 (2)</td><td rowspan="1" colspan="1">−0.2832 (2)</td><td rowspan="1" colspan="1">0.1174 (17)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H156</td><td rowspan="1" colspan="1">0.3133</td><td rowspan="1" colspan="1">0.4659</td><td rowspan="1" colspan="1">−0.3237</td><td rowspan="1" colspan="1">0.141*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N201</td><td rowspan="1" colspan="1">0.63736 (10)</td><td rowspan="1" colspan="1">0.65387 (10)</td><td rowspan="1" colspan="1">0.05085 (15)</td><td rowspan="1" colspan="1">0.0695 (6)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C202</td><td rowspan="1" colspan="1">0.60235 (13)</td><td rowspan="1" colspan="1">0.68222 (12)</td><td rowspan="1" colspan="1">0.1038 (2)</td><td rowspan="1" colspan="1">0.0742 (8)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H202</td><td rowspan="1" colspan="1">0.6140</td><td rowspan="1" colspan="1">0.7184</td><td rowspan="1" colspan="1">0.1241</td><td rowspan="1" colspan="1">0.089*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C203</td><td rowspan="1" colspan="1">0.55016 (12)</td><td rowspan="1" colspan="1">0.66270 (10)</td><td rowspan="1" colspan="1">0.13114 (18)</td><td rowspan="1" colspan="1">0.0635 (7)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H203</td><td rowspan="1" colspan="1">0.5271</td><td rowspan="1" colspan="1">0.6852</td><td rowspan="1" colspan="1">0.1689</td><td rowspan="1" colspan="1">0.076*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C204</td><td rowspan="1" colspan="1">0.53176 (10)</td><td rowspan="1" colspan="1">0.61002 (9)</td><td rowspan="1" colspan="1">0.10312 (14)</td><td rowspan="1" colspan="1">0.0474 (5)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C205</td><td rowspan="1" colspan="1">0.56798 (10)</td><td rowspan="1" colspan="1">0.58046 (10)</td><td rowspan="1" colspan="1">0.04725 (15)</td><td rowspan="1" colspan="1">0.0548 (6)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H205</td><td rowspan="1" colspan="1">0.5577</td><td rowspan="1" colspan="1">0.5442</td><td rowspan="1" colspan="1">0.0255</td><td rowspan="1" colspan="1">0.066*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C206</td><td rowspan="1" colspan="1">0.61911 (11)</td><td rowspan="1" colspan="1">0.60416 (12)</td><td rowspan="1" colspan="1">0.02354 (17)</td><td rowspan="1" colspan="1">0.0645 (7)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H206</td><td rowspan="1" colspan="1">0.6429</td><td rowspan="1" colspan="1">0.5831</td><td rowspan="1" colspan="1">−0.0153</td><td rowspan="1" colspan="1">0.077*</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="d1e1866"><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">Zn1</td><td rowspan="1" colspan="1">0.04778 (16)</td><td rowspan="1" colspan="1">0.04374 (16)</td><td rowspan="1" colspan="1">0.02318 (14)</td><td rowspan="1" colspan="1">−0.00756 (11)</td><td rowspan="1" colspan="1">0.00168 (10)</td><td rowspan="1" colspan="1">−0.00080 (10)</td></tr><tr><td rowspan="1" colspan="1">N21</td><td rowspan="1" colspan="1">0.0579 (10)</td><td rowspan="1" colspan="1">0.0455 (9)</td><td rowspan="1" colspan="1">0.0266 (8)</td><td rowspan="1" colspan="1">−0.0116 (8)</td><td rowspan="1" colspan="1">0.0027 (7)</td><td rowspan="1" colspan="1">0.0007 (7)</td></tr><tr><td rowspan="1" colspan="1">N22</td><td rowspan="1" colspan="1">0.0485 (9)</td><td rowspan="1" colspan="1">0.0476 (9)</td><td rowspan="1" colspan="1">0.0251 (8)</td><td rowspan="1" colspan="1">−0.0020 (7)</td><td rowspan="1" colspan="1">−0.0005 (7)</td><td rowspan="1" colspan="1">0.0025 (7)</td></tr><tr><td rowspan="1" colspan="1">N23</td><td rowspan="1" colspan="1">0.0531 (10)</td><td rowspan="1" colspan="1">0.0414 (9)</td><td rowspan="1" colspan="1">0.0266 (8)</td><td rowspan="1" colspan="1">−0.0084 (7)</td><td rowspan="1" colspan="1">0.0028 (7)</td><td rowspan="1" colspan="1">−0.0033 (6)</td></tr><tr><td rowspan="1" colspan="1">N24</td><td rowspan="1" colspan="1">0.0438 (9)</td><td rowspan="1" colspan="1">0.0446 (9)</td><td rowspan="1" colspan="1">0.0247 (8)</td><td rowspan="1" colspan="1">−0.0010 (7)</td><td rowspan="1" colspan="1">0.0004 (6)</td><td rowspan="1" colspan="1">−0.0035 (6)</td></tr><tr><td rowspan="1" colspan="1">C1</td><td rowspan="1" colspan="1">0.0521 (12)</td><td rowspan="1" colspan="1">0.0395 (10)</td><td rowspan="1" colspan="1">0.0342 (10)</td><td rowspan="1" colspan="1">−0.0129 (9)</td><td rowspan="1" colspan="1">0.0034 (8)</td><td rowspan="1" colspan="1">−0.0050 (8)</td></tr><tr><td rowspan="1" colspan="1">C2</td><td rowspan="1" colspan="1">0.0581 (14)</td><td rowspan="1" colspan="1">0.0608 (14)</td><td rowspan="1" colspan="1">0.0408 (12)</td><td rowspan="1" colspan="1">−0.0204 (11)</td><td rowspan="1" colspan="1">0.0039 (10)</td><td rowspan="1" colspan="1">−0.0108 (10)</td></tr><tr><td rowspan="1" colspan="1">C3</td><td rowspan="1" colspan="1">0.0599 (14)</td><td rowspan="1" colspan="1">0.0649 (14)</td><td rowspan="1" colspan="1">0.0354 (11)</td><td rowspan="1" colspan="1">−0.0209 (11)</td><td rowspan="1" colspan="1">−0.0001 (10)</td><td rowspan="1" colspan="1">−0.0111 (10)</td></tr><tr><td rowspan="1" colspan="1">C4</td><td rowspan="1" colspan="1">0.0522 (12)</td><td rowspan="1" colspan="1">0.0473 (11)</td><td rowspan="1" colspan="1">0.0290 (10)</td><td rowspan="1" colspan="1">−0.0094 (9)</td><td rowspan="1" colspan="1">0.0010 (8)</td><td rowspan="1" colspan="1">−0.0072 (8)</td></tr><tr><td rowspan="1" colspan="1">C5</td><td rowspan="1" colspan="1">0.0520 (12)</td><td rowspan="1" colspan="1">0.0531 (12)</td><td rowspan="1" colspan="1">0.0275 (10)</td><td rowspan="1" colspan="1">−0.0066 (9)</td><td rowspan="1" colspan="1">−0.0019 (8)</td><td rowspan="1" colspan="1">−0.0055 (8)</td></tr><tr><td rowspan="1" colspan="1">C6</td><td rowspan="1" colspan="1">0.0479 (11)</td><td rowspan="1" colspan="1">0.0494 (11)</td><td rowspan="1" colspan="1">0.0259 (10)</td><td rowspan="1" colspan="1">0.0000 (9)</td><td rowspan="1" colspan="1">0.0024 (8)</td><td rowspan="1" colspan="1">−0.0038 (8)</td></tr><tr><td rowspan="1" colspan="1">C7</td><td rowspan="1" colspan="1">0.0494 (12)</td><td rowspan="1" colspan="1">0.0603 (13)</td><td rowspan="1" colspan="1">0.0256 (10)</td><td rowspan="1" colspan="1">−0.0036 (10)</td><td rowspan="1" colspan="1">0.0010 (8)</td><td rowspan="1" colspan="1">−0.0026 (9)</td></tr><tr><td rowspan="1" colspan="1">C8</td><td rowspan="1" colspan="1">0.0458 (11)</td><td rowspan="1" colspan="1">0.0528 (12)</td><td rowspan="1" colspan="1">0.0279 (10)</td><td rowspan="1" colspan="1">0.0012 (9)</td><td rowspan="1" colspan="1">0.0035 (8)</td><td rowspan="1" colspan="1">−0.0002 (8)</td></tr><tr><td rowspan="1" colspan="1">C9</td><td rowspan="1" colspan="1">0.0410 (10)</td><td rowspan="1" colspan="1">0.0403 (10)</td><td rowspan="1" colspan="1">0.0274 (9)</td><td rowspan="1" colspan="1">0.0045 (8)</td><td rowspan="1" colspan="1">0.0019 (7)</td><td rowspan="1" colspan="1">−0.0024 (7)</td></tr><tr><td rowspan="1" colspan="1">C10</td><td rowspan="1" colspan="1">0.0421 (10)</td><td rowspan="1" colspan="1">0.0373 (10)</td><td rowspan="1" colspan="1">0.0286 (9)</td><td rowspan="1" colspan="1">0.0047 (8)</td><td rowspan="1" colspan="1">0.0014 (7)</td><td rowspan="1" colspan="1">−0.0020 (7)</td></tr><tr><td rowspan="1" colspan="1">C11</td><td rowspan="1" colspan="1">0.0428 (10)</td><td rowspan="1" colspan="1">0.0414 (10)</td><td rowspan="1" colspan="1">0.0287 (10)</td><td rowspan="1" colspan="1">0.0024 (8)</td><td rowspan="1" colspan="1">−0.0018 (8)</td><td rowspan="1" colspan="1">−0.0010 (8)</td></tr><tr><td rowspan="1" colspan="1">C12</td><td rowspan="1" colspan="1">0.0457 (11)</td><td rowspan="1" colspan="1">0.0623 (13)</td><td rowspan="1" colspan="1">0.0300 (10)</td><td rowspan="1" colspan="1">−0.0037 (10)</td><td rowspan="1" colspan="1">−0.0036 (8)</td><td rowspan="1" colspan="1">−0.0017 (9)</td></tr><tr><td rowspan="1" colspan="1">C13</td><td rowspan="1" colspan="1">0.0565 (13)</td><td rowspan="1" colspan="1">0.0725 (15)</td><td rowspan="1" colspan="1">0.0289 (11)</td><td rowspan="1" colspan="1">−0.0093 (11)</td><td rowspan="1" colspan="1">−0.0068 (9)</td><td rowspan="1" colspan="1">0.0036 (10)</td></tr><tr><td rowspan="1" colspan="1">C14</td><td rowspan="1" colspan="1">0.0566 (13)</td><td rowspan="1" colspan="1">0.0600 (13)</td><td rowspan="1" colspan="1">0.0264 (10)</td><td rowspan="1" colspan="1">−0.0071 (10)</td><td rowspan="1" colspan="1">−0.0044 (9)</td><td rowspan="1" colspan="1">0.0036 (9)</td></tr><tr><td rowspan="1" colspan="1">C15</td><td rowspan="1" colspan="1">0.0687 (15)</td><td rowspan="1" colspan="1">0.0670 (15)</td><td rowspan="1" colspan="1">0.0279 (11)</td><td rowspan="1" colspan="1">−0.0171 (12)</td><td rowspan="1" colspan="1">−0.0035 (10)</td><td rowspan="1" colspan="1">0.0076 (9)</td></tr><tr><td rowspan="1" colspan="1">C16</td><td rowspan="1" colspan="1">0.0697 (15)</td><td rowspan="1" colspan="1">0.0574 (13)</td><td rowspan="1" colspan="1">0.0273 (10)</td><td rowspan="1" colspan="1">−0.0158 (11)</td><td rowspan="1" colspan="1">0.0024 (9)</td><td rowspan="1" colspan="1">0.0052 (9)</td></tr><tr><td rowspan="1" colspan="1">C17</td><td rowspan="1" colspan="1">0.0816 (18)</td><td rowspan="1" colspan="1">0.0817 (17)</td><td rowspan="1" colspan="1">0.0276 (11)</td><td rowspan="1" colspan="1">−0.0288 (14)</td><td rowspan="1" colspan="1">0.0023 (11)</td><td rowspan="1" colspan="1">0.0087 (11)</td></tr><tr><td rowspan="1" colspan="1">C18</td><td rowspan="1" colspan="1">0.0723 (16)</td><td rowspan="1" colspan="1">0.0672 (15)</td><td rowspan="1" colspan="1">0.0347 (12)</td><td rowspan="1" colspan="1">−0.0260 (12)</td><td rowspan="1" colspan="1">0.0053 (10)</td><td rowspan="1" colspan="1">0.0071 (10)</td></tr><tr><td rowspan="1" colspan="1">C19</td><td rowspan="1" colspan="1">0.0595 (13)</td><td rowspan="1" colspan="1">0.0455 (11)</td><td rowspan="1" colspan="1">0.0314 (10)</td><td rowspan="1" colspan="1">−0.0118 (9)</td><td rowspan="1" colspan="1">0.0050 (9)</td><td rowspan="1" colspan="1">0.0012 (8)</td></tr><tr><td rowspan="1" colspan="1">C20</td><td rowspan="1" colspan="1">0.0570 (12)</td><td rowspan="1" colspan="1">0.0366 (10)</td><td rowspan="1" colspan="1">0.0351 (10)</td><td rowspan="1" colspan="1">−0.0118 (9)</td><td rowspan="1" colspan="1">0.0066 (9)</td><td rowspan="1" colspan="1">−0.0009 (8)</td></tr><tr><td rowspan="1" colspan="1">N51</td><td rowspan="1" colspan="1">0.0633 (14)</td><td rowspan="1" colspan="1">0.145 (3)</td><td rowspan="1" colspan="1">0.0359 (12)</td><td rowspan="1" colspan="1">−0.0305 (15)</td><td rowspan="1" colspan="1">−0.0006 (10)</td><td rowspan="1" colspan="1">−0.0144 (14)</td></tr><tr><td rowspan="1" colspan="1">C52</td><td rowspan="1" colspan="1">0.126 (3)</td><td rowspan="1" colspan="1">0.113 (3)</td><td rowspan="1" colspan="1">0.0447 (17)</td><td rowspan="1" colspan="1">−0.011 (2)</td><td rowspan="1" colspan="1">−0.0056 (17)</td><td rowspan="1" colspan="1">−0.0286 (17)</td></tr><tr><td rowspan="1" colspan="1">C53</td><td rowspan="1" colspan="1">0.126 (3)</td><td rowspan="1" colspan="1">0.0787 (19)</td><td rowspan="1" colspan="1">0.0403 (14)</td><td rowspan="1" colspan="1">−0.0017 (18)</td><td rowspan="1" colspan="1">−0.0102 (15)</td><td rowspan="1" colspan="1">−0.0181 (13)</td></tr><tr><td rowspan="1" colspan="1">C54</td><td rowspan="1" colspan="1">0.0499 (12)</td><td rowspan="1" colspan="1">0.0755 (16)</td><td rowspan="1" colspan="1">0.0286 (11)</td><td rowspan="1" colspan="1">−0.0147 (11)</td><td rowspan="1" colspan="1">0.0009 (9)</td><td rowspan="1" colspan="1">−0.0067 (10)</td></tr><tr><td rowspan="1" colspan="1">C55</td><td rowspan="1" colspan="1">0.096 (2)</td><td rowspan="1" colspan="1">0.100 (2)</td><td rowspan="1" colspan="1">0.0419 (15)</td><td rowspan="1" colspan="1">0.0139 (17)</td><td rowspan="1" colspan="1">−0.0143 (14)</td><td rowspan="1" colspan="1">−0.0037 (14)</td></tr><tr><td rowspan="1" colspan="1">C56</td><td rowspan="1" colspan="1">0.082 (2)</td><td rowspan="1" colspan="1">0.135 (3)</td><td rowspan="1" colspan="1">0.0486 (17)</td><td rowspan="1" colspan="1">0.002 (2)</td><td rowspan="1" colspan="1">−0.0152 (14)</td><td rowspan="1" colspan="1">0.0081 (18)</td></tr><tr><td rowspan="1" colspan="1">N101</td><td rowspan="1" colspan="1">0.0379 (8)</td><td rowspan="1" colspan="1">0.0442 (9)</td><td rowspan="1" colspan="1">0.0244 (8)</td><td rowspan="1" colspan="1">0.0040 (7)</td><td rowspan="1" colspan="1">−0.0013 (6)</td><td rowspan="1" colspan="1">−0.0035 (6)</td></tr><tr><td rowspan="1" colspan="1">C102</td><td rowspan="1" colspan="1">0.0418 (11)</td><td rowspan="1" colspan="1">0.0434 (11)</td><td rowspan="1" colspan="1">0.0358 (10)</td><td rowspan="1" colspan="1">0.0092 (8)</td><td rowspan="1" colspan="1">0.0059 (8)</td><td rowspan="1" colspan="1">−0.0024 (8)</td></tr><tr><td rowspan="1" colspan="1">C103</td><td rowspan="1" colspan="1">0.0466 (11)</td><td rowspan="1" colspan="1">0.0392 (10)</td><td rowspan="1" colspan="1">0.0360 (10)</td><td rowspan="1" colspan="1">0.0058 (8)</td><td rowspan="1" colspan="1">0.0063 (8)</td><td rowspan="1" colspan="1">0.0009 (8)</td></tr><tr><td rowspan="1" colspan="1">C104</td><td rowspan="1" colspan="1">0.0386 (10)</td><td rowspan="1" colspan="1">0.0412 (10)</td><td rowspan="1" colspan="1">0.0218 (8)</td><td rowspan="1" colspan="1">0.0052 (8)</td><td rowspan="1" colspan="1">−0.0005 (7)</td><td rowspan="1" colspan="1">−0.0033 (7)</td></tr><tr><td rowspan="1" colspan="1">C105</td><td rowspan="1" colspan="1">0.0376 (11)</td><td rowspan="1" colspan="1">0.0436 (12)</td><td rowspan="1" colspan="1">0.0707 (15)</td><td rowspan="1" colspan="1">0.0078 (9)</td><td rowspan="1" colspan="1">0.0018 (10)</td><td rowspan="1" colspan="1">−0.0042 (10)</td></tr><tr><td rowspan="1" colspan="1">C106</td><td rowspan="1" colspan="1">0.0422 (11)</td><td rowspan="1" colspan="1">0.0384 (11)</td><td rowspan="1" colspan="1">0.0665 (15)</td><td rowspan="1" colspan="1">0.0038 (9)</td><td rowspan="1" colspan="1">−0.0002 (10)</td><td rowspan="1" colspan="1">−0.0022 (10)</td></tr><tr><td rowspan="1" colspan="1">N151</td><td rowspan="1" colspan="1">0.157 (4)</td><td rowspan="1" colspan="1">0.182 (4)</td><td rowspan="1" colspan="1">0.0499 (18)</td><td rowspan="1" colspan="1">−0.092 (3)</td><td rowspan="1" colspan="1">−0.022 (2)</td><td rowspan="1" colspan="1">0.029 (2)</td></tr><tr><td rowspan="1" colspan="1">C152</td><td rowspan="1" colspan="1">0.267 (7)</td><td rowspan="1" colspan="1">0.130 (4)</td><td rowspan="1" colspan="1">0.067 (3)</td><td rowspan="1" colspan="1">−0.043 (4)</td><td rowspan="1" colspan="1">−0.074 (3)</td><td rowspan="1" colspan="1">0.028 (3)</td></tr><tr><td rowspan="1" colspan="1">C153</td><td rowspan="1" colspan="1">0.218 (5)</td><td rowspan="1" colspan="1">0.105 (3)</td><td rowspan="1" colspan="1">0.064 (2)</td><td rowspan="1" colspan="1">−0.016 (3)</td><td rowspan="1" colspan="1">−0.068 (3)</td><td rowspan="1" colspan="1">0.026 (2)</td></tr><tr><td rowspan="1" colspan="1">C154</td><td rowspan="1" colspan="1">0.0797 (18)</td><td rowspan="1" colspan="1">0.108 (2)</td><td rowspan="1" colspan="1">0.0312 (13)</td><td rowspan="1" colspan="1">−0.0441 (16)</td><td rowspan="1" colspan="1">−0.0058 (12)</td><td rowspan="1" colspan="1">0.0136 (13)</td></tr><tr><td rowspan="1" colspan="1">C155</td><td rowspan="1" colspan="1">0.088 (2)</td><td rowspan="1" colspan="1">0.180 (4)</td><td rowspan="1" colspan="1">0.0349 (15)</td><td rowspan="1" colspan="1">−0.029 (2)</td><td rowspan="1" colspan="1">0.0018 (13)</td><td rowspan="1" colspan="1">−0.0193 (18)</td></tr><tr><td rowspan="1" colspan="1">C156</td><td rowspan="1" colspan="1">0.098 (3)</td><td rowspan="1" colspan="1">0.210 (5)</td><td rowspan="1" colspan="1">0.0446 (19)</td><td rowspan="1" colspan="1">−0.059 (3)</td><td rowspan="1" colspan="1">0.0097 (17)</td><td rowspan="1" colspan="1">−0.011 (2)</td></tr><tr><td rowspan="1" colspan="1">N201</td><td rowspan="1" colspan="1">0.0714 (14)</td><td rowspan="1" colspan="1">0.0754 (15)</td><td rowspan="1" colspan="1">0.0616 (13)</td><td rowspan="1" colspan="1">−0.0299 (12)</td><td rowspan="1" colspan="1">0.0153 (11)</td><td rowspan="1" colspan="1">−0.0022 (11)</td></tr><tr><td rowspan="1" colspan="1">C202</td><td rowspan="1" colspan="1">0.0847 (19)</td><td rowspan="1" colspan="1">0.0592 (15)</td><td rowspan="1" colspan="1">0.0786 (19)</td><td rowspan="1" colspan="1">−0.0325 (14)</td><td rowspan="1" colspan="1">0.0173 (16)</td><td rowspan="1" colspan="1">−0.0085 (14)</td></tr><tr><td rowspan="1" colspan="1">C203</td><td rowspan="1" colspan="1">0.0751 (17)</td><td rowspan="1" colspan="1">0.0495 (13)</td><td rowspan="1" colspan="1">0.0658 (16)</td><td rowspan="1" colspan="1">−0.0190 (12)</td><td rowspan="1" colspan="1">0.0165 (13)</td><td rowspan="1" colspan="1">−0.0104 (11)</td></tr><tr><td rowspan="1" colspan="1">C204</td><td rowspan="1" colspan="1">0.0627 (13)</td><td rowspan="1" colspan="1">0.0454 (11)</td><td rowspan="1" colspan="1">0.0340 (11)</td><td rowspan="1" colspan="1">−0.0135 (10)</td><td rowspan="1" colspan="1">0.0057 (9)</td><td rowspan="1" colspan="1">0.0004 (8)</td></tr><tr><td rowspan="1" colspan="1">C205</td><td rowspan="1" colspan="1">0.0693 (15)</td><td rowspan="1" colspan="1">0.0540 (13)</td><td rowspan="1" colspan="1">0.0410 (12)</td><td rowspan="1" colspan="1">−0.0153 (11)</td><td rowspan="1" colspan="1">0.0148 (10)</td><td rowspan="1" colspan="1">−0.0076 (10)</td></tr><tr><td rowspan="1" colspan="1">C206</td><td rowspan="1" colspan="1">0.0700 (16)</td><td rowspan="1" colspan="1">0.0752 (17)</td><td rowspan="1" colspan="1">0.0482 (14)</td><td rowspan="1" colspan="1">−0.0173 (13)</td><td rowspan="1" colspan="1">0.0177 (12)</td><td rowspan="1" colspan="1">−0.0064 (12)</td></tr></table></table-wrap></sec><sec id="tablewrapgeomlong"><title>Geometric parameters (Å, °)</title><table-wrap position="anchor" id="d1e2828"><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">Zn1—N24</td><td rowspan="1" colspan="1">2.0684 (15)</td><td rowspan="1" colspan="1">C19—C20</td><td rowspan="1" colspan="1">1.413 (3)</td></tr><tr><td rowspan="1" colspan="1">Zn1—N21</td><td rowspan="1" colspan="1">2.0695 (16)</td><td rowspan="1" colspan="1">C20—C204</td><td rowspan="1" colspan="1">1.483 (3)</td></tr><tr><td rowspan="1" colspan="1">Zn1—N22</td><td rowspan="1" colspan="1">2.0695 (17)</td><td rowspan="1" colspan="1">N51—C56</td><td rowspan="1" colspan="1">1.302 (5)</td></tr><tr><td rowspan="1" colspan="1">Zn1—N23</td><td rowspan="1" colspan="1">2.0747 (16)</td><td rowspan="1" colspan="1">N51—C52</td><td rowspan="1" colspan="1">1.306 (5)</td></tr><tr><td rowspan="1" colspan="1">Zn1—N101<sup>i</sup></td><td rowspan="1" colspan="1">2.1385 (16)</td><td rowspan="1" colspan="1">C52—C53</td><td rowspan="1" colspan="1">1.376 (4)</td></tr><tr><td rowspan="1" colspan="1">N21—C19</td><td rowspan="1" colspan="1">1.363 (3)</td><td rowspan="1" colspan="1">C52—H52</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">N21—C16</td><td rowspan="1" colspan="1">1.369 (3)</td><td rowspan="1" colspan="1">C53—C54</td><td rowspan="1" colspan="1">1.369 (4)</td></tr><tr><td rowspan="1" colspan="1">N22—C11</td><td rowspan="1" colspan="1">1.364 (3)</td><td rowspan="1" colspan="1">C53—H53</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">N22—C14</td><td rowspan="1" colspan="1">1.373 (2)</td><td rowspan="1" colspan="1">C54—C55</td><td rowspan="1" colspan="1">1.355 (4)</td></tr><tr><td rowspan="1" colspan="1">N23—C4</td><td rowspan="1" colspan="1">1.369 (3)</td><td rowspan="1" colspan="1">C55—C56</td><td rowspan="1" colspan="1">1.389 (4)</td></tr><tr><td rowspan="1" colspan="1">N23—C1</td><td rowspan="1" colspan="1">1.374 (3)</td><td rowspan="1" colspan="1">C55—H55</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">N24—C9</td><td rowspan="1" colspan="1">1.363 (3)</td><td rowspan="1" colspan="1">C56—H56</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">N24—C6</td><td rowspan="1" colspan="1">1.370 (2)</td><td rowspan="1" colspan="1">N101—C102</td><td rowspan="1" colspan="1">1.333 (3)</td></tr><tr><td rowspan="1" colspan="1">C1—C20</td><td rowspan="1" colspan="1">1.411 (3)</td><td rowspan="1" colspan="1">N101—C106</td><td rowspan="1" colspan="1">1.336 (3)</td></tr><tr><td rowspan="1" colspan="1">C1—C2</td><td rowspan="1" colspan="1">1.443 (3)</td><td rowspan="1" colspan="1">N101—Zn1<sup>ii</sup></td><td rowspan="1" colspan="1">2.1385 (16)</td></tr><tr><td rowspan="1" colspan="1">C2—C3</td><td rowspan="1" colspan="1">1.347 (3)</td><td rowspan="1" colspan="1">C102—C103</td><td rowspan="1" colspan="1">1.376 (3)</td></tr><tr><td rowspan="1" colspan="1">C2—H2</td><td rowspan="1" colspan="1">0.9500</td><td rowspan="1" colspan="1">C102—H102</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C3—C4</td><td rowspan="1" colspan="1">1.442 (3)</td><td rowspan="1" colspan="1">C103—C104</td><td rowspan="1" colspan="1">1.383 (3)</td></tr><tr><td rowspan="1" colspan="1">C3—H3</td><td rowspan="1" colspan="1">0.9500</td><td rowspan="1" colspan="1">C103—H103</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C4—C5</td><td rowspan="1" colspan="1">1.407 (3)</td><td rowspan="1" colspan="1">C104—C105</td><td rowspan="1" colspan="1">1.383 (3)</td></tr><tr><td rowspan="1" colspan="1">C5—C6</td><td rowspan="1" colspan="1">1.404 (3)</td><td rowspan="1" colspan="1">C105—C106</td><td rowspan="1" colspan="1">1.385 (3)</td></tr><tr><td rowspan="1" colspan="1">C5—C54</td><td rowspan="1" colspan="1">1.497 (3)</td><td rowspan="1" colspan="1">C105—H105</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C6—C7</td><td rowspan="1" colspan="1">1.442 (3)</td><td rowspan="1" colspan="1">C106—H106</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C7—C8</td><td rowspan="1" colspan="1">1.352 (3)</td><td rowspan="1" colspan="1">N151—C152</td><td rowspan="1" colspan="1">1.294 (7)</td></tr><tr><td rowspan="1" colspan="1">C7—H7</td><td rowspan="1" colspan="1">0.9500</td><td rowspan="1" colspan="1">N151—C156</td><td rowspan="1" colspan="1">1.307 (6)</td></tr><tr><td rowspan="1" colspan="1">C8—C9</td><td rowspan="1" colspan="1">1.443 (3)</td><td rowspan="1" colspan="1">C152—C153</td><td rowspan="1" colspan="1">1.385 (5)</td></tr><tr><td rowspan="1" colspan="1">C8—H8</td><td rowspan="1" colspan="1">0.9500</td><td rowspan="1" colspan="1">C152—H152</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C9—C10</td><td rowspan="1" colspan="1">1.408 (3)</td><td rowspan="1" colspan="1">C153—C154</td><td rowspan="1" colspan="1">1.372 (5)</td></tr><tr><td rowspan="1" colspan="1">C10—C11</td><td rowspan="1" colspan="1">1.407 (3)</td><td rowspan="1" colspan="1">C153—H153</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C10—C104</td><td rowspan="1" colspan="1">1.489 (3)</td><td rowspan="1" colspan="1">C154—C155</td><td rowspan="1" colspan="1">1.345 (5)</td></tr><tr><td rowspan="1" colspan="1">C11—C12</td><td rowspan="1" colspan="1">1.449 (3)</td><td rowspan="1" colspan="1">C155—C156</td><td rowspan="1" colspan="1">1.413 (5)</td></tr><tr><td rowspan="1" colspan="1">C12—C13</td><td rowspan="1" colspan="1">1.345 (3)</td><td rowspan="1" colspan="1">C155—H155</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C12—H12</td><td rowspan="1" colspan="1">0.9500</td><td rowspan="1" colspan="1">C156—H156</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C13—C14</td><td rowspan="1" colspan="1">1.432 (3)</td><td rowspan="1" colspan="1">N201—C206</td><td rowspan="1" colspan="1">1.320 (3)</td></tr><tr><td rowspan="1" colspan="1">C13—H13</td><td rowspan="1" colspan="1">0.9500</td><td rowspan="1" colspan="1">N201—C202</td><td rowspan="1" colspan="1">1.330 (4)</td></tr><tr><td rowspan="1" colspan="1">C14—C15</td><td rowspan="1" colspan="1">1.401 (3)</td><td rowspan="1" colspan="1">C202—C203</td><td rowspan="1" colspan="1">1.382 (4)</td></tr><tr><td rowspan="1" colspan="1">C15—C16</td><td rowspan="1" colspan="1">1.405 (3)</td><td rowspan="1" colspan="1">C202—H202</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C15—C154</td><td rowspan="1" colspan="1">1.500 (3)</td><td rowspan="1" colspan="1">C203—C204</td><td rowspan="1" colspan="1">1.387 (3)</td></tr><tr><td rowspan="1" colspan="1">C16—C17</td><td rowspan="1" colspan="1">1.442 (3)</td><td rowspan="1" colspan="1">C203—H203</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C17—C18</td><td rowspan="1" colspan="1">1.339 (3)</td><td rowspan="1" colspan="1">C204—C205</td><td rowspan="1" colspan="1">1.388 (3)</td></tr><tr><td rowspan="1" colspan="1">C17—H17</td><td rowspan="1" colspan="1">0.9500</td><td rowspan="1" colspan="1">C205—C206</td><td rowspan="1" colspan="1">1.382 (3)</td></tr><tr><td rowspan="1" colspan="1">C18—C19</td><td rowspan="1" colspan="1">1.441 (3)</td><td rowspan="1" colspan="1">C205—H205</td><td rowspan="1" colspan="1">0.9500</td></tr><tr><td rowspan="1" colspan="1">C18—H18</td><td rowspan="1" colspan="1">0.9500</td><td rowspan="1" colspan="1">C206—H206</td><td rowspan="1" colspan="1">0.9500</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">N24—Zn1—N21</td><td rowspan="1" colspan="1">162.77 (7)</td><td rowspan="1" colspan="1">C17—C18—H18</td><td rowspan="1" colspan="1">126.1</td></tr><tr><td rowspan="1" colspan="1">N24—Zn1—N22</td><td rowspan="1" colspan="1">88.42 (6)</td><td rowspan="1" colspan="1">C19—C18—H18</td><td rowspan="1" colspan="1">126.1</td></tr><tr><td rowspan="1" colspan="1">N21—Zn1—N22</td><td rowspan="1" colspan="1">88.84 (7)</td><td rowspan="1" colspan="1">N21—C19—C20</td><td rowspan="1" colspan="1">126.29 (18)</td></tr><tr><td rowspan="1" colspan="1">N24—Zn1—N23</td><td rowspan="1" colspan="1">89.34 (6)</td><td rowspan="1" colspan="1">N21—C19—C18</td><td rowspan="1" colspan="1">109.15 (18)</td></tr><tr><td rowspan="1" colspan="1">N21—Zn1—N23</td><td rowspan="1" colspan="1">87.94 (6)</td><td rowspan="1" colspan="1">C20—C19—C18</td><td rowspan="1" colspan="1">124.46 (19)</td></tr><tr><td rowspan="1" colspan="1">N22—Zn1—N23</td><td rowspan="1" colspan="1">161.70 (7)</td><td rowspan="1" colspan="1">C1—C20—C19</td><td rowspan="1" colspan="1">124.66 (19)</td></tr><tr><td rowspan="1" colspan="1">N24—Zn1—N101<sup>i</sup></td><td rowspan="1" colspan="1">95.10 (6)</td><td rowspan="1" colspan="1">C1—C20—C204</td><td rowspan="1" colspan="1">118.30 (18)</td></tr><tr><td rowspan="1" colspan="1">N21—Zn1—N101<sup>i</sup></td><td rowspan="1" colspan="1">102.11 (6)</td><td rowspan="1" colspan="1">C19—C20—C204</td><td rowspan="1" colspan="1">116.97 (18)</td></tr><tr><td rowspan="1" colspan="1">N22—Zn1—N101<sup>i</sup></td><td rowspan="1" colspan="1">102.00 (6)</td><td rowspan="1" colspan="1">C56—N51—C52</td><td rowspan="1" colspan="1">115.3 (3)</td></tr><tr><td rowspan="1" colspan="1">N23—Zn1—N101<sup>i</sup></td><td rowspan="1" colspan="1">96.29 (6)</td><td rowspan="1" colspan="1">N51—C52—C53</td><td rowspan="1" colspan="1">124.6 (3)</td></tr><tr><td rowspan="1" colspan="1">C19—N21—C16</td><td rowspan="1" colspan="1">106.82 (16)</td><td rowspan="1" colspan="1">N51—C52—H52</td><td rowspan="1" colspan="1">117.7</td></tr><tr><td rowspan="1" colspan="1">C19—N21—Zn1</td><td rowspan="1" colspan="1">126.42 (13)</td><td rowspan="1" colspan="1">C53—C52—H52</td><td rowspan="1" colspan="1">117.7</td></tr><tr><td rowspan="1" colspan="1">C16—N21—Zn1</td><td rowspan="1" colspan="1">126.72 (14)</td><td rowspan="1" colspan="1">C54—C53—C52</td><td rowspan="1" colspan="1">119.8 (3)</td></tr><tr><td rowspan="1" colspan="1">C11—N22—C14</td><td rowspan="1" colspan="1">106.27 (17)</td><td rowspan="1" colspan="1">C54—C53—H53</td><td rowspan="1" colspan="1">120.1</td></tr><tr><td rowspan="1" colspan="1">C11—N22—Zn1</td><td rowspan="1" colspan="1">126.10 (13)</td><td rowspan="1" colspan="1">C52—C53—H53</td><td rowspan="1" colspan="1">120.1</td></tr><tr><td rowspan="1" colspan="1">C14—N22—Zn1</td><td rowspan="1" colspan="1">127.37 (14)</td><td rowspan="1" colspan="1">C55—C54—C53</td><td rowspan="1" colspan="1">115.9 (2)</td></tr><tr><td rowspan="1" colspan="1">C4—N23—C1</td><td rowspan="1" colspan="1">106.45 (16)</td><td rowspan="1" colspan="1">C55—C54—C5</td><td rowspan="1" colspan="1">123.2 (2)</td></tr><tr><td rowspan="1" colspan="1">C4—N23—Zn1</td><td rowspan="1" colspan="1">125.15 (13)</td><td rowspan="1" colspan="1">C53—C54—C5</td><td rowspan="1" colspan="1">120.9 (2)</td></tr><tr><td rowspan="1" colspan="1">C1—N23—Zn1</td><td rowspan="1" colspan="1">126.61 (13)</td><td rowspan="1" colspan="1">C54—C55—C56</td><td rowspan="1" colspan="1">119.9 (3)</td></tr><tr><td rowspan="1" colspan="1">C9—N24—C6</td><td rowspan="1" colspan="1">106.48 (15)</td><td rowspan="1" colspan="1">C54—C55—H55</td><td rowspan="1" colspan="1">120.0</td></tr><tr><td rowspan="1" colspan="1">C9—N24—Zn1</td><td rowspan="1" colspan="1">126.17 (12)</td><td rowspan="1" colspan="1">C56—C55—H55</td><td rowspan="1" colspan="1">120.0</td></tr><tr><td rowspan="1" colspan="1">C6—N24—Zn1</td><td rowspan="1" colspan="1">126.59 (13)</td><td rowspan="1" colspan="1">N51—C56—C55</td><td rowspan="1" colspan="1">124.4 (3)</td></tr><tr><td rowspan="1" colspan="1">N23—C1—C20</td><td rowspan="1" colspan="1">124.64 (18)</td><td rowspan="1" colspan="1">N51—C56—H56</td><td rowspan="1" colspan="1">117.8</td></tr><tr><td rowspan="1" colspan="1">N23—C1—C2</td><td rowspan="1" colspan="1">109.72 (17)</td><td rowspan="1" colspan="1">C55—C56—H56</td><td rowspan="1" colspan="1">117.8</td></tr><tr><td rowspan="1" colspan="1">C20—C1—C2</td><td rowspan="1" colspan="1">125.64 (19)</td><td rowspan="1" colspan="1">C102—N101—C106</td><td rowspan="1" colspan="1">116.85 (17)</td></tr><tr><td rowspan="1" colspan="1">C3—C2—C1</td><td rowspan="1" colspan="1">106.8 (2)</td><td rowspan="1" colspan="1">C102—N101—Zn1<sup>ii</sup></td><td rowspan="1" colspan="1">120.26 (13)</td></tr><tr><td rowspan="1" colspan="1">C3—C2—H2</td><td rowspan="1" colspan="1">126.6</td><td rowspan="1" colspan="1">C106—N101—Zn1<sup>ii</sup></td><td rowspan="1" colspan="1">122.55 (14)</td></tr><tr><td rowspan="1" colspan="1">C1—C2—H2</td><td rowspan="1" colspan="1">126.6</td><td rowspan="1" colspan="1">N101—C102—C103</td><td rowspan="1" colspan="1">123.56 (18)</td></tr><tr><td rowspan="1" colspan="1">C2—C3—C4</td><td rowspan="1" colspan="1">107.42 (19)</td><td rowspan="1" colspan="1">N101—C102—H102</td><td rowspan="1" colspan="1">118.2</td></tr><tr><td rowspan="1" colspan="1">C2—C3—H3</td><td rowspan="1" colspan="1">126.3</td><td rowspan="1" colspan="1">C103—C102—H102</td><td rowspan="1" colspan="1">118.2</td></tr><tr><td rowspan="1" colspan="1">C4—C3—H3</td><td rowspan="1" colspan="1">126.3</td><td rowspan="1" colspan="1">C102—C103—C104</td><td rowspan="1" colspan="1">119.61 (18)</td></tr><tr><td rowspan="1" colspan="1">N23—C4—C5</td><td rowspan="1" colspan="1">126.00 (18)</td><td rowspan="1" colspan="1">C102—C103—H103</td><td rowspan="1" colspan="1">120.2</td></tr><tr><td rowspan="1" colspan="1">N23—C4—C3</td><td rowspan="1" colspan="1">109.56 (18)</td><td rowspan="1" colspan="1">C104—C103—H103</td><td rowspan="1" colspan="1">120.2</td></tr><tr><td rowspan="1" colspan="1">C5—C4—C3</td><td rowspan="1" colspan="1">124.42 (18)</td><td rowspan="1" colspan="1">C105—C104—C103</td><td rowspan="1" colspan="1">117.31 (18)</td></tr><tr><td rowspan="1" colspan="1">C6—C5—C4</td><td rowspan="1" colspan="1">125.98 (18)</td><td rowspan="1" colspan="1">C105—C104—C10</td><td rowspan="1" colspan="1">122.03 (17)</td></tr><tr><td rowspan="1" colspan="1">C6—C5—C54</td><td rowspan="1" colspan="1">117.43 (18)</td><td rowspan="1" colspan="1">C103—C104—C10</td><td rowspan="1" colspan="1">120.65 (17)</td></tr><tr><td rowspan="1" colspan="1">C4—C5—C54</td><td rowspan="1" colspan="1">116.59 (18)</td><td rowspan="1" colspan="1">C104—C105—C106</td><td rowspan="1" colspan="1">119.38 (19)</td></tr><tr><td rowspan="1" colspan="1">N24—C6—C5</td><td rowspan="1" colspan="1">125.05 (18)</td><td rowspan="1" colspan="1">C104—C105—H105</td><td rowspan="1" colspan="1">120.3</td></tr><tr><td rowspan="1" colspan="1">N24—C6—C7</td><td rowspan="1" colspan="1">109.78 (17)</td><td rowspan="1" colspan="1">C106—C105—H105</td><td rowspan="1" colspan="1">120.3</td></tr><tr><td rowspan="1" colspan="1">C5—C6—C7</td><td rowspan="1" colspan="1">125.15 (18)</td><td rowspan="1" colspan="1">N101—C106—C105</td><td rowspan="1" colspan="1">123.3 (2)</td></tr><tr><td rowspan="1" colspan="1">C8—C7—C6</td><td rowspan="1" colspan="1">106.91 (17)</td><td rowspan="1" colspan="1">N101—C106—H106</td><td rowspan="1" colspan="1">118.4</td></tr><tr><td rowspan="1" colspan="1">C8—C7—H7</td><td rowspan="1" colspan="1">126.5</td><td rowspan="1" colspan="1">C105—C106—H106</td><td rowspan="1" colspan="1">118.4</td></tr><tr><td rowspan="1" colspan="1">C6—C7—H7</td><td rowspan="1" colspan="1">126.5</td><td rowspan="1" colspan="1">C152—N151—C156</td><td rowspan="1" colspan="1">117.0 (4)</td></tr><tr><td rowspan="1" colspan="1">C7—C8—C9</td><td rowspan="1" colspan="1">106.83 (18)</td><td rowspan="1" colspan="1">N151—C152—C153</td><td rowspan="1" colspan="1">123.7 (5)</td></tr><tr><td rowspan="1" colspan="1">C7—C8—H8</td><td rowspan="1" colspan="1">126.6</td><td rowspan="1" colspan="1">N151—C152—H152</td><td rowspan="1" colspan="1">118.2</td></tr><tr><td rowspan="1" colspan="1">C9—C8—H8</td><td rowspan="1" colspan="1">126.6</td><td rowspan="1" colspan="1">C153—C152—H152</td><td rowspan="1" colspan="1">118.2</td></tr><tr><td rowspan="1" colspan="1">N24—C9—C10</td><td rowspan="1" colspan="1">125.42 (17)</td><td rowspan="1" colspan="1">C154—C153—C152</td><td rowspan="1" colspan="1">120.3 (5)</td></tr><tr><td rowspan="1" colspan="1">N24—C9—C8</td><td rowspan="1" colspan="1">110.00 (16)</td><td rowspan="1" colspan="1">C154—C153—H153</td><td rowspan="1" colspan="1">119.9</td></tr><tr><td rowspan="1" colspan="1">C10—C9—C8</td><td rowspan="1" colspan="1">124.54 (18)</td><td rowspan="1" colspan="1">C152—C153—H153</td><td rowspan="1" colspan="1">119.9</td></tr><tr><td rowspan="1" colspan="1">C11—C10—C9</td><td rowspan="1" colspan="1">125.06 (18)</td><td rowspan="1" colspan="1">C155—C154—C153</td><td rowspan="1" colspan="1">116.1 (3)</td></tr><tr><td rowspan="1" colspan="1">C11—C10—C104</td><td rowspan="1" colspan="1">117.12 (16)</td><td rowspan="1" colspan="1">C155—C154—C15</td><td rowspan="1" colspan="1">122.8 (3)</td></tr><tr><td rowspan="1" colspan="1">C9—C10—C104</td><td rowspan="1" colspan="1">117.77 (16)</td><td rowspan="1" colspan="1">C153—C154—C15</td><td rowspan="1" colspan="1">121.1 (3)</td></tr><tr><td rowspan="1" colspan="1">N22—C11—C10</td><td rowspan="1" colspan="1">125.68 (17)</td><td rowspan="1" colspan="1">C154—C155—C156</td><td rowspan="1" colspan="1">120.0 (4)</td></tr><tr><td rowspan="1" colspan="1">N22—C11—C12</td><td rowspan="1" colspan="1">109.87 (17)</td><td rowspan="1" colspan="1">C154—C155—H155</td><td rowspan="1" colspan="1">120.0</td></tr><tr><td rowspan="1" colspan="1">C10—C11—C12</td><td rowspan="1" colspan="1">124.42 (18)</td><td rowspan="1" colspan="1">C156—C155—H155</td><td rowspan="1" colspan="1">120.0</td></tr><tr><td rowspan="1" colspan="1">C13—C12—C11</td><td rowspan="1" colspan="1">106.50 (19)</td><td rowspan="1" colspan="1">N151—C156—C155</td><td rowspan="1" colspan="1">122.9 (5)</td></tr><tr><td rowspan="1" colspan="1">C13—C12—H12</td><td rowspan="1" colspan="1">126.7</td><td rowspan="1" colspan="1">N151—C156—H156</td><td rowspan="1" colspan="1">118.6</td></tr><tr><td rowspan="1" colspan="1">C11—C12—H12</td><td rowspan="1" colspan="1">126.7</td><td rowspan="1" colspan="1">C155—C156—H156</td><td rowspan="1" colspan="1">118.6</td></tr><tr><td rowspan="1" colspan="1">C12—C13—C14</td><td rowspan="1" colspan="1">107.59 (19)</td><td rowspan="1" colspan="1">C206—N201—C202</td><td rowspan="1" colspan="1">115.6 (2)</td></tr><tr><td rowspan="1" colspan="1">C12—C13—H13</td><td rowspan="1" colspan="1">126.2</td><td rowspan="1" colspan="1">N201—C202—C203</td><td rowspan="1" colspan="1">124.5 (2)</td></tr><tr><td rowspan="1" colspan="1">C14—C13—H13</td><td rowspan="1" colspan="1">126.2</td><td rowspan="1" colspan="1">N201—C202—H202</td><td rowspan="1" colspan="1">117.8</td></tr><tr><td rowspan="1" colspan="1">N22—C14—C15</td><td rowspan="1" colspan="1">124.8 (2)</td><td rowspan="1" colspan="1">C203—C202—H202</td><td rowspan="1" colspan="1">117.8</td></tr><tr><td rowspan="1" colspan="1">N22—C14—C13</td><td rowspan="1" colspan="1">109.76 (18)</td><td rowspan="1" colspan="1">C202—C203—C204</td><td rowspan="1" colspan="1">119.5 (2)</td></tr><tr><td rowspan="1" colspan="1">C15—C14—C13</td><td rowspan="1" colspan="1">125.41 (19)</td><td rowspan="1" colspan="1">C202—C203—H203</td><td rowspan="1" colspan="1">120.3</td></tr><tr><td rowspan="1" colspan="1">C14—C15—C16</td><td rowspan="1" colspan="1">126.03 (19)</td><td rowspan="1" colspan="1">C204—C203—H203</td><td rowspan="1" colspan="1">120.3</td></tr><tr><td rowspan="1" colspan="1">C14—C15—C154</td><td rowspan="1" colspan="1">117.7 (2)</td><td rowspan="1" colspan="1">C203—C204—C205</td><td rowspan="1" colspan="1">116.2 (2)</td></tr><tr><td rowspan="1" colspan="1">C16—C15—C154</td><td rowspan="1" colspan="1">116.28 (19)</td><td rowspan="1" colspan="1">C203—C204—C20</td><td rowspan="1" colspan="1">121.7 (2)</td></tr><tr><td rowspan="1" colspan="1">N21—C16—C15</td><td rowspan="1" colspan="1">125.76 (19)</td><td rowspan="1" colspan="1">C205—C204—C20</td><td rowspan="1" colspan="1">122.07 (19)</td></tr><tr><td rowspan="1" colspan="1">N21—C16—C17</td><td rowspan="1" colspan="1">109.5 (2)</td><td rowspan="1" colspan="1">C206—C205—C204</td><td rowspan="1" colspan="1">119.5 (2)</td></tr><tr><td rowspan="1" colspan="1">C15—C16—C17</td><td rowspan="1" colspan="1">124.7 (2)</td><td rowspan="1" colspan="1">C206—C205—H205</td><td rowspan="1" colspan="1">120.3</td></tr><tr><td rowspan="1" colspan="1">C18—C17—C16</td><td rowspan="1" colspan="1">106.7 (2)</td><td rowspan="1" colspan="1">C204—C205—H205</td><td rowspan="1" colspan="1">120.3</td></tr><tr><td rowspan="1" colspan="1">C18—C17—H17</td><td rowspan="1" colspan="1">126.6</td><td rowspan="1" colspan="1">N201—C206—C205</td><td rowspan="1" colspan="1">124.8 (2)</td></tr><tr><td rowspan="1" colspan="1">C16—C17—H17</td><td rowspan="1" colspan="1">126.6</td><td rowspan="1" colspan="1">N201—C206—H206</td><td rowspan="1" colspan="1">117.6</td></tr><tr><td rowspan="1" colspan="1">C17—C18—C19</td><td rowspan="1" colspan="1">107.8 (2)</td><td rowspan="1" colspan="1">C205—C206—H206</td><td rowspan="1" colspan="1">117.6</td></tr></table></table-wrap><p>Symmetry codes: (i) <italic>y</italic>, −<italic>x</italic>+1/2, −<italic>z</italic>+1/2; (ii) −<italic>y</italic>+1/2, <italic>x</italic>, −<italic>z</italic>+1/2.</p></sec><sec id="tablewraphbondslong"><title>Hydrogen-bond geometry (Å, °)</title><table-wrap position="anchor" id="d1e3951"><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">C7—H7···N151<sup>iii</sup></td><td rowspan="1" colspan="1">0.95</td><td rowspan="1" colspan="1">2.65</td><td rowspan="1" colspan="1">3.583 (4)</td><td rowspan="1" colspan="1">167.</td></tr><tr><td rowspan="1" colspan="1">C17—H17···N51<sup>iv</sup></td><td rowspan="1" colspan="1">0.95</td><td rowspan="1" colspan="1">2.66</td><td rowspan="1" colspan="1">3.583 (3)</td><td rowspan="1" colspan="1">165.</td></tr></table></table-wrap><p>Symmetry codes: (iii) <italic>x</italic>, <italic>y</italic>, <italic>z</italic>+1; (iv) <italic>x</italic>, <italic>y</italic>, <italic>z</italic>−1.</p></sec></app></app-group><ref-list><title>References</title><ref id="bb1"><mixed-citation publication-type="other">Allen, F. 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(2009). <italic>Acta Cryst.</italic> D<bold>65</bold>, 148–155.</mixed-citation></ref></ref-list></back><floats-group><table-wrap-group id="table1" position="float"><label>Table 1</label><caption><title>Selected geometric parameters (Å, °)</title></caption><table-wrap id="d32e574" position="float"><table frame="hsides" rules="groups"><tbody valign="top"><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">Zn1—N24</td><td style="" rowspan="1" colspan="1" align="char" valign="top">2.0684 (15)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">Zn1—N21</td><td style="" rowspan="1" colspan="1" align="char" valign="top">2.0695 (16)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">Zn1—N22</td><td style="" rowspan="1" colspan="1" align="char" valign="top">2.0695 (17)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">Zn1—N23</td><td style="" rowspan="1" colspan="1" align="char" valign="top">2.0747 (16)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">Zn1—N101<sup>i</sup></td><td style="" rowspan="1" colspan="1" align="char" valign="top">2.1385 (16)</td></tr></tbody></table></table-wrap><table-wrap id="d32e604" position="float"><table frame="hsides" rules="groups"><tbody valign="top"><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">N24—Zn1—N21</td><td style="" rowspan="1" colspan="1" align="char" valign="top">162.77 (7)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">N24—Zn1—N22</td><td style="" rowspan="1" colspan="1" align="char" valign="top">88.42 (6)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">N21—Zn1—N22</td><td style="" rowspan="1" colspan="1" align="char" valign="top">88.84 (7)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">N24—Zn1—N23</td><td style="" rowspan="1" colspan="1" align="char" valign="top">89.34 (6)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">N21—Zn1—N23</td><td style="" rowspan="1" colspan="1" align="char" valign="top">87.94 (6)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">N22—Zn1—N23</td><td style="" rowspan="1" colspan="1" align="char" valign="top">161.70 (7)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">N24—Zn1—N101<sup>i</sup></td><td style="" rowspan="1" colspan="1" align="char" valign="top">95.10 (6)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">N21—Zn1—N101<sup>i</sup></td><td style="" rowspan="1" colspan="1" align="char" valign="top">102.11 (6)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">N22—Zn1—N101<sup>i</sup></td><td style="" rowspan="1" colspan="1" align="char" valign="top">102.00 (6)</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">N23—Zn1—N101<sup>i</sup></td><td style="" rowspan="1" colspan="1" align="char" valign="top">96.29 (6)</td></tr></tbody></table><table-wrap-foot><p>Symmetry code: (i) <inline-formula><inline-graphic xlink:href="e-67-0m236-efi4.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula>.</p></table-wrap-foot></table-wrap></table-wrap-group><table-wrap id="table2" position="float"><label>Table 2</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">C7—H7⋯N151<sup>ii</sup></td><td style="" rowspan="1" colspan="1" align="left" valign="top">0.95</td><td style="" rowspan="1" colspan="1" align="left" valign="top">2.65</td><td style="" rowspan="1" colspan="1" align="left" valign="top">3.583 (4)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">167</td></tr><tr><td style="" rowspan="1" colspan="1" align="left" valign="top">C17—H17⋯N51<sup>iii</sup></td><td style="" rowspan="1" colspan="1" align="left" valign="top">0.95</td><td style="" rowspan="1" colspan="1" align="left" valign="top">2.66</td><td style="" rowspan="1" colspan="1" align="left" valign="top">3.583 (3)</td><td style="" rowspan="1" colspan="1" align="left" valign="top">165</td></tr></tbody></table><table-wrap-foot><p>Symmetry codes: (ii) <inline-formula><inline-graphic xlink:href="e-67-0m236-efi5.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula>; (iii) <inline-formula><inline-graphic xlink:href="e-67-0m236-efi6.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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