Crystal structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II)
Identifieur interne : 000050 ( Pmc/Corpus ); précédent : 000049; suivant : 000051Crystal structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II)
Auteurs : Marwa Mghandef ; Habib BoughzalaSource :
- Acta Crystallographica Section E: Crystallographic Communications [ 2056-9890 ] ; 2015.
Abstract
In the structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II), the essentially planar cations are connected through N—H⋯Cl hydrogen bonds to the tetrahedral anion.
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DOI: 10.1107/S2056989015007707
PubMed: 25995878
PubMed Central: 4420110
Links to Exploration step
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Crystal structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II)</title><author><name sortKey="Mghandef, Marwa" sort="Mghandef, Marwa" uniqKey="Mghandef M" first="Marwa" last="Mghandef">Marwa Mghandef</name><affiliation><nlm:aff id="a">Laboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Université de Tunis El Manar, 2092 Manar II Tunis,<country>Tunisia</country></nlm:aff></affiliation></author><author><name sortKey="Boughzala, Habib" sort="Boughzala, Habib" uniqKey="Boughzala H" first="Habib" last="Boughzala">Habib Boughzala</name><affiliation><nlm:aff id="a">Laboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Université de Tunis El Manar, 2092 Manar II Tunis,<country>Tunisia</country></nlm:aff></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">PMC</idno><idno type="pmid">25995878</idno><idno type="pmc">4420110</idno><idno type="url">http://www.ncbi.nlm.nih.gov/pmc/articles/PMC4420110</idno><idno type="RBID">PMC:4420110</idno><idno type="doi">10.1107/S2056989015007707</idno><date when="2015">2015</date><idno type="wicri:Area/Pmc/Corpus">000050</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Corpus" wicri:corpus="PMC">000050</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en" level="a" type="main">Crystal structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II)</title><author><name sortKey="Mghandef, Marwa" sort="Mghandef, Marwa" uniqKey="Mghandef M" first="Marwa" last="Mghandef">Marwa Mghandef</name><affiliation><nlm:aff id="a">Laboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Université de Tunis El Manar, 2092 Manar II Tunis,<country>Tunisia</country></nlm:aff></affiliation></author><author><name sortKey="Boughzala, Habib" sort="Boughzala, Habib" uniqKey="Boughzala H" first="Habib" last="Boughzala">Habib Boughzala</name><affiliation><nlm:aff id="a">Laboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Université de Tunis El Manar, 2092 Manar II Tunis,<country>Tunisia</country></nlm:aff></affiliation></author></analytic><series><title level="j">Acta Crystallographica Section E: Crystallographic Communications</title><idno type="eISSN">2056-9890</idno><imprint><date when="2015">2015</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en"><p>In the structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II), the essentially planar cations are connected through N—H⋯Cl hydrogen bonds to the tetrahedral anion.</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><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 E Crystallogr Commun</journal-id><journal-id journal-id-type="iso-abbrev">Acta Crystallogr E Crystallogr Commun</journal-id><journal-id journal-id-type="publisher-id">Acta Cryst. E</journal-id><journal-title-group><journal-title>Acta Crystallographica Section E: Crystallographic Communications</journal-title></journal-title-group><issn pub-type="epub">2056-9890</issn><publisher><publisher-name>International Union of Crystallography</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="pmid">25995878</article-id><article-id pub-id-type="pmc">4420110</article-id><article-id pub-id-type="publisher-id">wm5146</article-id><article-id pub-id-type="doi">10.1107/S2056989015007707</article-id><article-id pub-id-type="coden">ACSECI</article-id><article-id pub-id-type="pii">S2056989015007707</article-id><article-categories><subj-group subj-group-type="heading"><subject>Research Communications</subject></subj-group></article-categories><title-group><article-title>Crystal structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II)</article-title><alt-title><italic>(C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[CoCl<sub>4</sub>]</italic></alt-title></title-group><contrib-group><contrib contrib-type="author"><name><surname>Mghandef</surname><given-names>Marwa</given-names></name><xref ref-type="aff" rid="a">a</xref></contrib><contrib contrib-type="author"><name><surname>Boughzala</surname><given-names>Habib</given-names></name><xref ref-type="aff" rid="a">a</xref><xref ref-type="corresp" rid="cor">*</xref></contrib><aff id="a"><label>a</label>Laboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Université de Tunis El Manar, 2092 Manar II Tunis,<country>Tunisia</country></aff></contrib-group><author-notes><corresp id="cor">Correspondence e-mail: <email>habib.boughzala@ipein.rnu.tn</email></corresp></author-notes><pub-date pub-type="collection"><day>01</day><month>5</month><year>2015</year></pub-date><pub-date pub-type="epub"><day>25</day><month>4</month><year>2015</year></pub-date><pub-date pub-type="pmc-release"><day>25</day><month>4</month><year>2015</year></pub-date><pmc-comment> PMC Release delay is 0 months and 0 days and was based on the
<volume>71</volume><issue>Pt 5</issue><issue-id pub-id-type="publisher-id">e150500</issue-id><fpage>555</fpage><lpage>557</lpage><history><date date-type="received"><day>11</day><month>4</month><year>2015</year></date><date date-type="accepted"><day>19</day><month>4</month><year>2015</year></date></history><permissions><copyright-statement>© Mghandef and Boughzala 2015</copyright-statement><copyright-year>2015</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/S2056989015007707">A full version of this article is available from Crystallography Journals Online.</self-uri><abstract abstract-type="toc"><p>In the structure of bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II), the essentially planar cations are connected through N—H⋯Cl hydrogen bonds to the tetrahedral anion.</p></abstract><abstract><p>The title salt, (C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[CoCl<sub>4</sub>], was synthesized by slow evaporation of an aqueous solution at room temperature. The asymmetric unit consists of two essentially planar (C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sup>+</sup> cations [maximum deviations = 0.010 (3) and 0.014 (3) Å] that are nearly perpendicular to each other [dihedral angle = 84.12 (7)°]. They are bonded through N—H⋯Cl hydrogen bonds to distorted [CoCl<sub>4</sub>]<sup>2−</sup> tetrahedra, leading to the formation of undulating layers parallel to (100). The structure is isotypic with the Zn analogue [Kefi <italic>et. al</italic> (2011). <italic>Acta Cryst.</italic> E<bold>67</bold>, m355–m356.]</p></abstract><kwd-group><kwd>crystal structure</kwd><kwd>cobalt(II) complex</kwd><kwd>2-amino-5-chloropyridine</kwd><kwd>hydrogen bonding</kwd></kwd-group></article-meta></front><body><sec id="sec1"><title>Chemical context </title><p>Organic–inorganic hybrid compounds frequently exhibit self-organized structures and can combine organic and inorganic characteristics (Parent <italic>et al.</italic>, 2007<xref ref-type="bibr" rid="bb15"> ▸</xref>; Zheng <italic>et al.</italic>, 2010<xref ref-type="bibr" rid="bb20"> ▸</xref>; Chang <italic>et al.</italic>, 2011<xref ref-type="bibr" rid="bb2"> ▸</xref>). In particular, anionic cobalt halides associated with organic counter-cations have some interesting physical properties, such as luminescence, in which we are interested. In this communication, we report the synthesis and crystal structure of the new organic–inorganic hybrid compound bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II), (C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[CoCl<sub>4</sub>].<chem-struct id="scheme1"><graphic xlink:href="e-71-00555-scheme1.jpg" position="float"></graphic></chem-struct></p></sec><sec id="sec2"><title>Structural commentary </title><p>The asymmetric unit of the title compound consists of two 2-amino-5-chloropyridinium cations (cat1 consists of ring C1–C5/N2 and cat2 consists of ring C9–C10/N3) and one isolated [CoCl<sub>4</sub>]<sup>2−</sup> anion (Fig. 1<xref ref-type="fig" rid="fig1"> ▸</xref>).</p><p>The organic cations are nearly planar exhibiting small maximum deviations of 0.010 (3) and 0.014 (3) Å for atoms N2 and C6, respectively. The two least-squares planes of the two cations are nearly perpendicular to each other [84.12 (7)°]. The bond angles C4—N2—C5 [123.6 (3)°] and C9—N3—C10 [123.3 (3)°] in the rings of cat1 and cat2, respectively, confirm the presence of pyridinium cations. Previous studies (Jin <italic>et al.</italic>, 2001<xref ref-type="bibr" rid="bb8"> ▸</xref>) showed that a pyridinium cation possesses an expanded C—N(H)—C angle in comparison with the parent pyridine (117°). This geometrical characteristic is in agreement with an imine–enamine resonance (Jin <italic>et al.</italic>, 2005<xref ref-type="bibr" rid="bb9"> ▸</xref>) and contributes to the structural stability.</p><p>In the [CoCl<sub>4</sub>]<sup>2−</sup> anion, the Co—Cl bond lengths range from 2.2645 (12) to 2.2934 (12) Å and the Cl—Co—Cl angles range from 104.84 (5) to 118.58 (5)°, revealing considerable distortions from the ideal tetrahedral geometry. These values are in agreement with those observed in similar compounds (Dhieb <italic>et al.</italic>, 2014<xref ref-type="bibr" rid="bb4"> ▸</xref>; Mghandef & Boughzala, 2014<xref ref-type="bibr" rid="bb12"> ▸</xref>; Oh <italic>et al.</italic>, 2011<xref ref-type="bibr" rid="bb14"> ▸</xref>). The different Co—Cl bond lengths in the [CoCl<sub>4</sub>]<sup>2−</sup> anion are related to the number of hydrogen bonds accepted by the Cl atoms. The Co—Cl1 and Co—Cl4 bonds are longer than the Co—Cl2 and Co—Cl3 bonds because atoms Cl1 and Cl4 are each acceptors of two hydrogen bonds from cat2 and cat1, respectively.</p></sec><sec id="sec3"><title>Supramolecular features </title><p>Each CoCl<sub>4</sub> tetrahedron is linked to four cations (two cat1 and two cat2) by hydrogen bonds (Fig. 2<xref ref-type="fig" rid="fig2"> ▸</xref> and Table 1<xref ref-type="table" rid="table1"> ▸</xref>). Atom Cl1 is doubly linked to one cat2 cation by N3—H<italic>N</italic>3⋯Cl1 and N4—H4<italic>A</italic>⋯Cl1, and atom Cl2 establishes one hydrogen bond with a symmetry-related cat2 cation <italic>via</italic> N4—H4<italic>B</italic>⋯Cl2. Atom Cl3 is linked to cation cat1 by N1—H1<italic>B</italic>⋯Cl3 and atom Cl4 again shares two hydrogen bonds (N1—H1<italic>A</italic>⋯Cl4 and N2—H<italic>N</italic>2⋯Cl4) with a second symmetry-related cat1 cation. The hydrogen-bonding environments of the two cations are similar. Both are linked to two CoCl<sub>4</sub> tetrahedra by three hydrogen bonds (Fig. 3<xref ref-type="fig" rid="fig3"> ▸</xref>)</p><p>The crystal packing can be described by an alternate stacking of cations and anions with a –cat1–[CoCl<sub>4</sub>]–cat2–[CoCl<sub>4</sub>]– sequence along [100], as shown in Fig. 4<xref ref-type="fig" rid="fig4"> ▸</xref>. Between antiparallel aligned cat2 cations, π–π interactions are also present [centroid-to-centroid separation = 3.900 (2) Å]. The stacked cations and anions are linked through N—H⋯Cl hydrogen bonds into zigzag layers parallel to (100) (Fig. 5<xref ref-type="fig" rid="fig5"> ▸</xref>).</p></sec><sec id="sec4"><title>Database survey </title><p>A systematic search procedure in the Cambridge Structural Database (Groom & Allen, 2014<xref ref-type="bibr" rid="bb6"> ▸</xref>) indicates a total of 32 hits for the 2-amino-5-chloropyridinium cation with various counter-anions. For tetrahalogenidometalate anions, the following structures have been reported: (C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[ZnCl<sub>4</sub>]·H<sub>2</sub>O (Coomer <italic>et al.</italic>, 2007<xref ref-type="bibr" rid="bb3"> ▸</xref>); (C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[ZnCl<sub>4</sub>] (Kefi <italic>et al.</italic>, 2011<italic>a</italic><xref ref-type="bibr" rid="bb10"> ▸</xref>); (C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[CdCl<sub>4</sub>]·H<sub>2</sub>O (Kefi <italic>et al.</italic>, 2011<italic>b</italic><xref ref-type="bibr" rid="bb11"> ▸</xref>); (C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[CuCl<sub>4</sub>] (Parsons <italic>et al.</italic>, 2006<xref ref-type="bibr" rid="bb16"> ▸</xref>); (C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[CuBr<sub>4</sub>] (Woodward <italic>et al.</italic>, 2002<xref ref-type="bibr" rid="bb19"> ▸</xref>). The title compound is isotypic with the Zn analogue (C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[ZnCl<sub>4</sub>] (Kefi <italic>et al.</italic>, 2011<italic>a</italic><xref ref-type="bibr" rid="bb10"> ▸</xref>).</p></sec><sec id="sec5"><title>Synthesis and crystallization </title><p>A mixture of cobalt(II) chloride and 2-amino-5-chloropyridine (molar ratio 1:1) was dissolved in an aqueous solution of hydrochloric acid with 5 ml of ethanol. The mixture was stirred and then kept at room temperature. Blue crystals of the title compound were obtained after two weeks.</p></sec><sec id="sec6"><title>Refinement </title><p>Crystal data, data collection and structure refinement details are summarized in Table 2<xref ref-type="table" rid="table2"> ▸</xref>. H atoms were placed geometrically and included as riding contributions, with N—H = 0.86 Å and C—H = 0.93 Å and with <italic>U</italic><sub>iso</sub>(H) = 1.2<italic>U</italic><sub>eq</sub>(N,C).</p></sec><sec sec-type="supplementary-material"><title>Supplementary Material</title><supplementary-material content-type="local-data"><p>Crystal structure: contains datablock(s) I, New_Global_Publ_Block. DOI: <ext-link ext-link-type="uri" xlink:href="http://dx.doi.org/10.1107/S2056989015007707/wm5146sup1.cif">10.1107/S2056989015007707/wm5146sup1.cif</ext-link></p><media mimetype="chemical" mime-subtype="x-cif" xlink:href="e-71-00555-sup1.cif" xlink:type="simple" id="d36e114" position="anchor"></media></supplementary-material><supplementary-material content-type="local-data"><p>Structure factors: contains datablock(s) I. DOI: <ext-link ext-link-type="uri" xlink:href="http://dx.doi.org/10.1107/S2056989015007707/wm5146Isup2.hkl">10.1107/S2056989015007707/wm5146Isup2.hkl</ext-link></p><media mimetype="text" mime-subtype="plain" xlink:href="e-71-00555-Isup2.hkl" xlink:type="simple" id="d36e121" position="anchor"></media></supplementary-material><supplementary-material content-type="local-data"><p>CCDC reference: <ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/cr.cgi?rm=csd&csdid=990478">990478</ext-link></p></supplementary-material><supplementary-material content-type="local-data"><p>Additional supporting information: <ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/sendsupfiles?wm5146&file=wm5146sup0.html&mime=text/html"> crystallographic information</ext-link>; <ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/sendcif?wm5146sup1&Qmime=cif">3D view</ext-link>; <ext-link ext-link-type="uri" xlink:href="http://scripts.iucr.org/cgi-bin/paper?wm5146&checkcif=yes">checkCIF report</ext-link></p></supplementary-material></sec></body><back><app-group><app><title>supplementary crystallographic
information</title><sec id="tablewrapcrystaldatalong"><title>Crystal data</title><table-wrap position="anchor" id="d1e36"><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">(C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[CoCl<sub>4</sub>]</td><td rowspan="1" colspan="1"><italic>F</italic>(000) = 916</td></tr><tr><td rowspan="1" colspan="1"><italic>M</italic><italic><sub>r</sub></italic> = 459.87</td><td rowspan="1" colspan="1"><italic>D</italic><sub>x</sub> = 1.735 Mg m<sup>−</sup><sup>3</sup></td></tr><tr><td rowspan="1" colspan="1">Monoclinic, <italic>P</italic>2<sub>1</sub>/<italic>c</italic></td><td rowspan="1" colspan="1">Mo <italic>K</italic>α radiation, λ = 0.71073 Å</td></tr><tr><td rowspan="1" colspan="1">Hall symbol: -P 2ybc</td><td rowspan="1" colspan="1">Cell parameters from 25 reflections</td></tr><tr><td rowspan="1" colspan="1"><italic>a</italic> = 13.519 (2) Å</td><td rowspan="1" colspan="1">θ = 10–15°</td></tr><tr><td rowspan="1" colspan="1"><italic>b</italic> = 14.945 (3) Å</td><td rowspan="1" colspan="1">µ = 1.88 mm<sup>−</sup><sup>1</sup></td></tr><tr><td rowspan="1" colspan="1"><italic>c</italic> = 8.725 (2) Å</td><td rowspan="1" colspan="1"><italic>T</italic> = 298 K</td></tr><tr><td rowspan="1" colspan="1">β = 92.858 (3)°</td><td rowspan="1" colspan="1">Prism, blue</td></tr><tr><td rowspan="1" colspan="1"><italic>V</italic> = 1760.6 (6) Å<sup>3</sup></td><td rowspan="1" colspan="1">0.5 × 0.3 × 0.2 mm</td></tr><tr><td rowspan="1" colspan="1"><italic>Z</italic> = 4</td><td rowspan="1" colspan="1"></td></tr></table></table-wrap></sec><sec id="tablewrapdatacollectionlong"><title>Data collection</title><table-wrap position="anchor" id="d1e170"><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">Enraf–Nonius CAD-4 diffractometer</td><td rowspan="1" colspan="1">2121 reflections with <italic>I</italic> > 2σ(<italic>I</italic>)</td></tr><tr><td rowspan="1" colspan="1">Radiation source: fine-focus sealed tube</td><td rowspan="1" colspan="1"><italic>R</italic><sub>int</sub> = 0.039</td></tr><tr><td rowspan="1" colspan="1">Graphite monochromator</td><td rowspan="1" colspan="1">θ<sub>max</sub> = 27.0°, θ<sub>min</sub> = 2.0°</td></tr><tr><td rowspan="1" colspan="1">non–profiled ω/2τ scans</td><td rowspan="1" colspan="1"><italic>h</italic> = −17→17</td></tr><tr><td rowspan="1" colspan="1">Absorption correction: ψ scan (North <italic>et al.</italic>, 1968)</td><td rowspan="1" colspan="1"><italic>k</italic> = −19→1</td></tr><tr><td rowspan="1" colspan="1"><italic>T</italic><sub>min</sub> = 0.423, <italic>T</italic><sub>max</sub> = 0.649</td><td rowspan="1" colspan="1"><italic>l</italic> = −11→5</td></tr><tr><td rowspan="1" colspan="1">6241 measured reflections</td><td rowspan="1" colspan="1">2 standard reflections every 120 min</td></tr><tr><td rowspan="1" colspan="1">3707 independent reflections</td><td rowspan="1" colspan="1"> intensity decay: 6%</td></tr></table></table-wrap></sec><sec id="tablewraprefinementdatalong"><title>Refinement</title><table-wrap position="anchor" id="d1e296"><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>)] = 0.041</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>) = 0.109</td><td rowspan="1" colspan="1">H-atom parameters not refined</td></tr><tr><td rowspan="1" colspan="1"><italic>S</italic> = 0.99</td><td rowspan="1" colspan="1"><italic>w</italic> = 1/[σ<sup>2</sup>(<italic>F</italic><sub>o</sub><sup>2</sup>) + (0.0443<italic>P</italic>)<sup>2</sup>] 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">3707 reflections</td><td rowspan="1" colspan="1">(Δ/σ)<sub>max</sub> < 0.001</td></tr><tr><td rowspan="1" colspan="1">190 parameters</td><td rowspan="1" colspan="1">Δρ<sub>max</sub> = 0.52 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> = −0.34 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="d1e451"><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="d1e551"><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">Co</td><td rowspan="1" colspan="1">0.75262 (3)</td><td rowspan="1" colspan="1">0.48488 (3)</td><td rowspan="1" colspan="1">0.01742 (6)</td><td rowspan="1" colspan="1">0.03927 (16)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">Cl1</td><td rowspan="1" colspan="1">0.66040 (7)</td><td rowspan="1" colspan="1">0.47789 (7)</td><td rowspan="1" colspan="1">−0.20888 (12)</td><td rowspan="1" colspan="1">0.0475 (3)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">Cl2</td><td rowspan="1" colspan="1">0.64020 (8)</td><td rowspan="1" colspan="1">0.48540 (8)</td><td rowspan="1" colspan="1">0.20135 (13)</td><td rowspan="1" colspan="1">0.0580 (3)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">Cl3</td><td rowspan="1" colspan="1">0.85951 (8)</td><td rowspan="1" colspan="1">0.60044 (7)</td><td rowspan="1" colspan="1">0.05556 (14)</td><td rowspan="1" colspan="1">0.0580 (3)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">Cl4</td><td rowspan="1" colspan="1">0.84305 (8)</td><td rowspan="1" colspan="1">0.35504 (7)</td><td rowspan="1" colspan="1">0.03059 (15)</td><td rowspan="1" colspan="1">0.0690 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">Cl5</td><td rowspan="1" colspan="1">0.83772 (8)</td><td rowspan="1" colspan="1">0.37281 (8)</td><td rowspan="1" colspan="1">0.53616 (14)</td><td rowspan="1" colspan="1">0.0646 (3)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">Cl6</td><td rowspan="1" colspan="1">0.68358 (8)</td><td rowspan="1" colspan="1">0.75291 (9)</td><td rowspan="1" colspan="1">0.29194 (14)</td><td rowspan="1" colspan="1">0.0672 (4)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N1</td><td rowspan="1" colspan="1">0.9792 (2)</td><td rowspan="1" colspan="1">0.7278 (2)</td><td rowspan="1" colspan="1">0.7188 (4)</td><td rowspan="1" colspan="1">0.0616 (11)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H1A</td><td rowspan="1" colspan="1">1.0247</td><td rowspan="1" colspan="1">0.7306</td><td rowspan="1" colspan="1">0.7912</td><td rowspan="1" colspan="1">0.074*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H1B</td><td rowspan="1" colspan="1">0.9565</td><td rowspan="1" colspan="1">0.7762</td><td rowspan="1" colspan="1">0.6768</td><td rowspan="1" colspan="1">0.074*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N2</td><td rowspan="1" colspan="1">0.9798 (2)</td><td rowspan="1" colspan="1">0.5740 (2)</td><td rowspan="1" colspan="1">0.7372 (4)</td><td rowspan="1" colspan="1">0.0430 (8)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">HN2</td><td rowspan="1" colspan="1">1.0261</td><td rowspan="1" colspan="1">0.5790</td><td rowspan="1" colspan="1">0.8078</td><td rowspan="1" colspan="1">0.052*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N3</td><td rowspan="1" colspan="1">0.4647 (2)</td><td rowspan="1" colspan="1">0.8197 (2)</td><td rowspan="1" colspan="1">0.5514 (4)</td><td rowspan="1" colspan="1">0.0444 (8)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">HN3</td><td rowspan="1" colspan="1">0.4394</td><td rowspan="1" colspan="1">0.8686</td><td rowspan="1" colspan="1">0.5834</td><td rowspan="1" colspan="1">0.053*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">N4</td><td rowspan="1" colspan="1">0.3491 (2)</td><td rowspan="1" colspan="1">0.7428 (2)</td><td rowspan="1" colspan="1">0.6902 (4)</td><td rowspan="1" colspan="1">0.0557 (9)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H4A</td><td rowspan="1" colspan="1">0.3264</td><td rowspan="1" colspan="1">0.7931</td><td rowspan="1" colspan="1">0.7210</td><td rowspan="1" colspan="1">0.067*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H4B</td><td rowspan="1" colspan="1">0.3233</td><td rowspan="1" colspan="1">0.6935</td><td rowspan="1" colspan="1">0.7195</td><td rowspan="1" colspan="1">0.067*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C1</td><td rowspan="1" colspan="1">0.8770 (3)</td><td rowspan="1" colspan="1">0.4802 (3)</td><td rowspan="1" colspan="1">0.5868 (5)</td><td rowspan="1" colspan="1">0.0427 (9)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C2</td><td rowspan="1" colspan="1">0.8694 (3)</td><td rowspan="1" colspan="1">0.6385 (3)</td><td rowspan="1" colspan="1">0.5537 (5)</td><td rowspan="1" colspan="1">0.0498 (11)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H2</td><td rowspan="1" colspan="1">0.8425</td><td rowspan="1" colspan="1">0.6887</td><td rowspan="1" colspan="1">0.5045</td><td rowspan="1" colspan="1">0.060*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C3</td><td rowspan="1" colspan="1">0.8370 (3)</td><td rowspan="1" colspan="1">0.5557 (3)</td><td rowspan="1" colspan="1">0.5125 (5)</td><td rowspan="1" colspan="1">0.0503 (11)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H3</td><td rowspan="1" colspan="1">0.7880</td><td rowspan="1" colspan="1">0.5492</td><td rowspan="1" colspan="1">0.4346</td><td rowspan="1" colspan="1">0.060*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C4</td><td rowspan="1" colspan="1">0.9472 (3)</td><td rowspan="1" colspan="1">0.4907 (2)</td><td rowspan="1" colspan="1">0.6989 (5)</td><td rowspan="1" colspan="1">0.0458 (10)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H4</td><td rowspan="1" colspan="1">0.9736</td><td rowspan="1" colspan="1">0.4411</td><td rowspan="1" colspan="1">0.7504</td><td rowspan="1" colspan="1">0.055*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C5</td><td rowspan="1" colspan="1">0.9440 (3)</td><td rowspan="1" colspan="1">0.6484 (2)</td><td rowspan="1" colspan="1">0.6714 (5)</td><td rowspan="1" colspan="1">0.0418 (9)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C6</td><td rowspan="1" colspan="1">0.5837 (3)</td><td rowspan="1" colspan="1">0.7483 (3)</td><td rowspan="1" colspan="1">0.4092 (4)</td><td rowspan="1" colspan="1">0.0451 (10)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C7</td><td rowspan="1" colspan="1">0.5437 (3)</td><td rowspan="1" colspan="1">0.6658 (3)</td><td rowspan="1" colspan="1">0.4521 (5)</td><td rowspan="1" colspan="1">0.0550 (11)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H7</td><td rowspan="1" colspan="1">0.5707</td><td rowspan="1" colspan="1">0.6129</td><td rowspan="1" colspan="1">0.4168</td><td rowspan="1" colspan="1">0.066*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C8</td><td rowspan="1" colspan="1">0.4669 (3)</td><td rowspan="1" colspan="1">0.6625 (3)</td><td rowspan="1" colspan="1">0.5436 (5)</td><td rowspan="1" colspan="1">0.0536 (11)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H8</td><td rowspan="1" colspan="1">0.4413</td><td rowspan="1" colspan="1">0.6075</td><td rowspan="1" colspan="1">0.5720</td><td rowspan="1" colspan="1">0.064*</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C9</td><td rowspan="1" colspan="1">0.4253 (3)</td><td rowspan="1" colspan="1">0.7413 (3)</td><td rowspan="1" colspan="1">0.5959 (4)</td><td rowspan="1" colspan="1">0.0444 (10)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">C10</td><td rowspan="1" colspan="1">0.5418 (3)</td><td rowspan="1" colspan="1">0.8250 (3)</td><td rowspan="1" colspan="1">0.4591 (4)</td><td rowspan="1" colspan="1">0.0433 (9)</td><td rowspan="1" colspan="1"></td></tr><tr><td rowspan="1" colspan="1">H10</td><td rowspan="1" colspan="1">0.5659</td><td rowspan="1" colspan="1">0.8804</td><td rowspan="1" colspan="1">0.4301</td><td rowspan="1" colspan="1">0.052*</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="d1e988"><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">Co</td><td rowspan="1" colspan="1">0.0394 (3)</td><td rowspan="1" colspan="1">0.0288 (3)</td><td rowspan="1" colspan="1">0.0492 (4)</td><td rowspan="1" colspan="1">−0.0023 (2)</td><td rowspan="1" colspan="1">−0.0018 (2)</td><td rowspan="1" colspan="1">−0.0013 (3)</td></tr><tr><td rowspan="1" colspan="1">Cl1</td><td rowspan="1" colspan="1">0.0502 (5)</td><td rowspan="1" colspan="1">0.0460 (6)</td><td rowspan="1" colspan="1">0.0459 (6)</td><td rowspan="1" colspan="1">0.0005 (5)</td><td rowspan="1" colspan="1">−0.0002 (4)</td><td rowspan="1" colspan="1">0.0005 (5)</td></tr><tr><td rowspan="1" colspan="1">Cl2</td><td rowspan="1" colspan="1">0.0679 (6)</td><td rowspan="1" colspan="1">0.0542 (7)</td><td rowspan="1" colspan="1">0.0534 (7)</td><td rowspan="1" colspan="1">−0.0144 (5)</td><td rowspan="1" colspan="1">0.0158 (5)</td><td rowspan="1" colspan="1">−0.0045 (6)</td></tr><tr><td rowspan="1" colspan="1">Cl3</td><td rowspan="1" colspan="1">0.0587 (6)</td><td rowspan="1" colspan="1">0.0409 (6)</td><td rowspan="1" colspan="1">0.0740 (8)</td><td rowspan="1" colspan="1">−0.0159 (5)</td><td rowspan="1" colspan="1">−0.0008 (5)</td><td rowspan="1" colspan="1">−0.0049 (6)</td></tr><tr><td rowspan="1" colspan="1">Cl4</td><td rowspan="1" colspan="1">0.0673 (7)</td><td rowspan="1" colspan="1">0.0336 (6)</td><td rowspan="1" colspan="1">0.1025 (10)</td><td rowspan="1" colspan="1">0.0110 (5)</td><td rowspan="1" colspan="1">−0.0328 (7)</td><td rowspan="1" colspan="1">−0.0098 (6)</td></tr><tr><td rowspan="1" colspan="1">Cl5</td><td rowspan="1" colspan="1">0.0688 (7)</td><td rowspan="1" colspan="1">0.0414 (6)</td><td rowspan="1" colspan="1">0.0842 (9)</td><td rowspan="1" colspan="1">−0.0114 (5)</td><td rowspan="1" colspan="1">0.0087 (6)</td><td rowspan="1" colspan="1">−0.0175 (6)</td></tr><tr><td rowspan="1" colspan="1">Cl6</td><td rowspan="1" colspan="1">0.0545 (6)</td><td rowspan="1" colspan="1">0.0911 (10)</td><td rowspan="1" colspan="1">0.0556 (7)</td><td rowspan="1" colspan="1">0.0035 (6)</td><td rowspan="1" colspan="1">−0.0007 (5)</td><td rowspan="1" colspan="1">0.0019 (7)</td></tr><tr><td rowspan="1" colspan="1">N1</td><td rowspan="1" colspan="1">0.072 (2)</td><td rowspan="1" colspan="1">0.031 (2)</td><td rowspan="1" colspan="1">0.079 (3)</td><td rowspan="1" colspan="1">−0.0005 (17)</td><td rowspan="1" colspan="1">−0.020 (2)</td><td rowspan="1" colspan="1">0.0032 (19)</td></tr><tr><td rowspan="1" colspan="1">N2</td><td rowspan="1" colspan="1">0.0468 (17)</td><td rowspan="1" colspan="1">0.0315 (18)</td><td rowspan="1" colspan="1">0.050 (2)</td><td rowspan="1" colspan="1">0.0029 (14)</td><td rowspan="1" colspan="1">−0.0070 (15)</td><td rowspan="1" colspan="1">0.0019 (16)</td></tr><tr><td rowspan="1" colspan="1">N3</td><td rowspan="1" colspan="1">0.058 (2)</td><td rowspan="1" colspan="1">0.0224 (16)</td><td rowspan="1" colspan="1">0.052 (2)</td><td rowspan="1" colspan="1">0.0068 (15)</td><td rowspan="1" colspan="1">−0.0028 (17)</td><td rowspan="1" colspan="1">−0.0015 (16)</td></tr><tr><td rowspan="1" colspan="1">N4</td><td rowspan="1" colspan="1">0.060 (2)</td><td rowspan="1" colspan="1">0.048 (2)</td><td rowspan="1" colspan="1">0.058 (2)</td><td rowspan="1" colspan="1">−0.0021 (17)</td><td rowspan="1" colspan="1">−0.0021 (19)</td><td rowspan="1" colspan="1">0.0081 (19)</td></tr><tr><td rowspan="1" colspan="1">C1</td><td rowspan="1" colspan="1">0.046 (2)</td><td rowspan="1" colspan="1">0.035 (2)</td><td rowspan="1" colspan="1">0.048 (2)</td><td rowspan="1" colspan="1">−0.0022 (18)</td><td rowspan="1" colspan="1">0.0102 (18)</td><td rowspan="1" colspan="1">−0.008 (2)</td></tr><tr><td rowspan="1" colspan="1">C2</td><td rowspan="1" colspan="1">0.049 (2)</td><td rowspan="1" colspan="1">0.041 (2)</td><td rowspan="1" colspan="1">0.058 (3)</td><td rowspan="1" colspan="1">0.0069 (19)</td><td rowspan="1" colspan="1">−0.009 (2)</td><td rowspan="1" colspan="1">0.010 (2)</td></tr><tr><td rowspan="1" colspan="1">C3</td><td rowspan="1" colspan="1">0.044 (2)</td><td rowspan="1" colspan="1">0.050 (3)</td><td rowspan="1" colspan="1">0.055 (3)</td><td rowspan="1" colspan="1">0.0022 (19)</td><td rowspan="1" colspan="1">−0.0083 (19)</td><td rowspan="1" colspan="1">−0.002 (2)</td></tr><tr><td rowspan="1" colspan="1">C4</td><td rowspan="1" colspan="1">0.054 (2)</td><td rowspan="1" colspan="1">0.025 (2)</td><td rowspan="1" colspan="1">0.058 (3)</td><td rowspan="1" colspan="1">0.0077 (17)</td><td rowspan="1" colspan="1">0.005 (2)</td><td rowspan="1" colspan="1">0.003 (2)</td></tr><tr><td rowspan="1" colspan="1">C5</td><td rowspan="1" colspan="1">0.044 (2)</td><td rowspan="1" colspan="1">0.031 (2)</td><td rowspan="1" colspan="1">0.051 (3)</td><td rowspan="1" colspan="1">0.0023 (17)</td><td rowspan="1" colspan="1">0.0027 (18)</td><td rowspan="1" colspan="1">0.006 (2)</td></tr><tr><td rowspan="1" colspan="1">C6</td><td rowspan="1" colspan="1">0.049 (2)</td><td rowspan="1" colspan="1">0.048 (3)</td><td rowspan="1" colspan="1">0.038 (2)</td><td rowspan="1" colspan="1">0.0016 (19)</td><td rowspan="1" colspan="1">−0.0102 (18)</td><td rowspan="1" colspan="1">−0.001 (2)</td></tr><tr><td rowspan="1" colspan="1">C7</td><td rowspan="1" colspan="1">0.082 (3)</td><td rowspan="1" colspan="1">0.035 (2)</td><td rowspan="1" colspan="1">0.048 (3)</td><td rowspan="1" colspan="1">0.007 (2)</td><td rowspan="1" colspan="1">−0.002 (2)</td><td rowspan="1" colspan="1">−0.001 (2)</td></tr><tr><td rowspan="1" colspan="1">C8</td><td rowspan="1" colspan="1">0.080 (3)</td><td rowspan="1" colspan="1">0.032 (2)</td><td rowspan="1" colspan="1">0.049 (3)</td><td rowspan="1" colspan="1">−0.006 (2)</td><td rowspan="1" colspan="1">0.003 (2)</td><td rowspan="1" colspan="1">0.005 (2)</td></tr><tr><td rowspan="1" colspan="1">C9</td><td rowspan="1" colspan="1">0.050 (2)</td><td rowspan="1" colspan="1">0.037 (2)</td><td rowspan="1" colspan="1">0.045 (2)</td><td rowspan="1" colspan="1">−0.0010 (18)</td><td rowspan="1" colspan="1">−0.0099 (19)</td><td rowspan="1" colspan="1">0.006 (2)</td></tr><tr><td rowspan="1" colspan="1">C10</td><td rowspan="1" colspan="1">0.049 (2)</td><td rowspan="1" colspan="1">0.037 (2)</td><td rowspan="1" colspan="1">0.043 (2)</td><td rowspan="1" colspan="1">−0.0078 (18)</td><td rowspan="1" colspan="1">−0.0065 (19)</td><td rowspan="1" colspan="1">0.0046 (19)</td></tr></table></table-wrap></sec><sec id="tablewrapgeomlong"><title>Geometric parameters (Å, º)</title><table-wrap position="anchor" id="d1e1418"><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">Co—Cl2</td><td rowspan="1" colspan="1">2.2645 (12)</td><td rowspan="1" colspan="1">N4—H4A</td><td rowspan="1" colspan="1">0.8600</td></tr><tr><td rowspan="1" colspan="1">Co—Cl3</td><td rowspan="1" colspan="1">2.2657 (11)</td><td rowspan="1" colspan="1">N4—H4B</td><td rowspan="1" colspan="1">0.8600</td></tr><tr><td rowspan="1" colspan="1">Co—Cl1</td><td rowspan="1" colspan="1">2.2843 (12)</td><td rowspan="1" colspan="1">C1—C4</td><td rowspan="1" colspan="1">1.337 (5)</td></tr><tr><td rowspan="1" colspan="1">Co—Cl4</td><td rowspan="1" colspan="1">2.2934 (12)</td><td rowspan="1" colspan="1">C1—C3</td><td rowspan="1" colspan="1">1.397 (6)</td></tr><tr><td rowspan="1" colspan="1">Cl5—C1</td><td rowspan="1" colspan="1">1.741 (4)</td><td rowspan="1" colspan="1">C2—C3</td><td rowspan="1" colspan="1">1.355 (6)</td></tr><tr><td rowspan="1" colspan="1">Cl6—C6</td><td rowspan="1" colspan="1">1.735 (4)</td><td rowspan="1" colspan="1">C2—C5</td><td rowspan="1" colspan="1">1.410 (5)</td></tr><tr><td rowspan="1" colspan="1">N1—C5</td><td rowspan="1" colspan="1">1.337 (5)</td><td rowspan="1" colspan="1">C2—H2</td><td rowspan="1" colspan="1">0.9300</td></tr><tr><td rowspan="1" colspan="1">N1—H1A</td><td rowspan="1" colspan="1">0.8600</td><td rowspan="1" colspan="1">C3—H3</td><td rowspan="1" colspan="1">0.9300</td></tr><tr><td rowspan="1" colspan="1">N1—H1B</td><td rowspan="1" colspan="1">0.8600</td><td rowspan="1" colspan="1">C4—H4</td><td rowspan="1" colspan="1">0.9300</td></tr><tr><td rowspan="1" colspan="1">N2—C5</td><td rowspan="1" colspan="1">1.331 (4)</td><td rowspan="1" colspan="1">C6—C10</td><td rowspan="1" colspan="1">1.360 (5)</td></tr><tr><td rowspan="1" colspan="1">N2—C4</td><td rowspan="1" colspan="1">1.357 (5)</td><td rowspan="1" colspan="1">C6—C7</td><td rowspan="1" colspan="1">1.405 (6)</td></tr><tr><td rowspan="1" colspan="1">N2—HN2</td><td rowspan="1" colspan="1">0.8600</td><td rowspan="1" colspan="1">C7—C8</td><td rowspan="1" colspan="1">1.342 (6)</td></tr><tr><td rowspan="1" colspan="1">N3—C10</td><td rowspan="1" colspan="1">1.351 (5)</td><td rowspan="1" colspan="1">C7—H7</td><td rowspan="1" colspan="1">0.9300</td></tr><tr><td rowspan="1" colspan="1">N3—C9</td><td rowspan="1" colspan="1">1.352 (5)</td><td rowspan="1" colspan="1">C8—C9</td><td rowspan="1" colspan="1">1.392 (6)</td></tr><tr><td rowspan="1" colspan="1">N3—HN3</td><td rowspan="1" colspan="1">0.8600</td><td rowspan="1" colspan="1">C8—H8</td><td rowspan="1" colspan="1">0.9300</td></tr><tr><td rowspan="1" colspan="1">N4—C9</td><td rowspan="1" colspan="1">1.351 (5)</td><td rowspan="1" colspan="1">C10—H10</td><td rowspan="1" colspan="1">0.9300</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">Cl2—Co—Cl3</td><td rowspan="1" colspan="1">109.81 (5)</td><td rowspan="1" colspan="1">C2—C3—C1</td><td rowspan="1" colspan="1">120.1 (4)</td></tr><tr><td rowspan="1" colspan="1">Cl2—Co—Cl1</td><td rowspan="1" colspan="1">104.84 (5)</td><td rowspan="1" colspan="1">C2—C3—H3</td><td rowspan="1" colspan="1">119.9</td></tr><tr><td rowspan="1" colspan="1">Cl3—Co—Cl1</td><td rowspan="1" colspan="1">118.58 (5)</td><td rowspan="1" colspan="1">C1—C3—H3</td><td rowspan="1" colspan="1">119.9</td></tr><tr><td rowspan="1" colspan="1">Cl2—Co—Cl4</td><td rowspan="1" colspan="1">110.02 (5)</td><td rowspan="1" colspan="1">C1—C4—N2</td><td rowspan="1" colspan="1">119.9 (4)</td></tr><tr><td rowspan="1" colspan="1">Cl3—Co—Cl4</td><td rowspan="1" colspan="1">107.65 (5)</td><td rowspan="1" colspan="1">C1—C4—H4</td><td rowspan="1" colspan="1">120.1</td></tr><tr><td rowspan="1" colspan="1">Cl1—Co—Cl4</td><td rowspan="1" colspan="1">105.73 (4)</td><td rowspan="1" colspan="1">N2—C4—H4</td><td rowspan="1" colspan="1">120.1</td></tr><tr><td rowspan="1" colspan="1">C5—N1—H1A</td><td rowspan="1" colspan="1">120.0</td><td rowspan="1" colspan="1">N2—C5—N1</td><td rowspan="1" colspan="1">119.5 (3)</td></tr><tr><td rowspan="1" colspan="1">C5—N1—H1B</td><td rowspan="1" colspan="1">120.0</td><td rowspan="1" colspan="1">N2—C5—C2</td><td rowspan="1" colspan="1">117.2 (3)</td></tr><tr><td rowspan="1" colspan="1">H1A—N1—H1B</td><td rowspan="1" colspan="1">120.0</td><td rowspan="1" colspan="1">N1—C5—C2</td><td rowspan="1" colspan="1">123.3 (3)</td></tr><tr><td rowspan="1" colspan="1">C5—N2—C4</td><td rowspan="1" colspan="1">123.6 (3)</td><td rowspan="1" colspan="1">C10—C6—C7</td><td rowspan="1" colspan="1">118.8 (4)</td></tr><tr><td rowspan="1" colspan="1">C5—N2—HN2</td><td rowspan="1" colspan="1">118.2</td><td rowspan="1" colspan="1">C10—C6—Cl6</td><td rowspan="1" colspan="1">120.2 (3)</td></tr><tr><td rowspan="1" colspan="1">C4—N2—HN2</td><td rowspan="1" colspan="1">118.2</td><td rowspan="1" colspan="1">C7—C6—Cl6</td><td rowspan="1" colspan="1">120.9 (3)</td></tr><tr><td rowspan="1" colspan="1">C10—N3—C9</td><td rowspan="1" colspan="1">123.3 (3)</td><td rowspan="1" colspan="1">C8—C7—C6</td><td rowspan="1" colspan="1">120.7 (4)</td></tr><tr><td rowspan="1" colspan="1">C10—N3—HN3</td><td rowspan="1" colspan="1">118.4</td><td rowspan="1" colspan="1">C8—C7—H7</td><td rowspan="1" colspan="1">119.7</td></tr><tr><td rowspan="1" colspan="1">C9—N3—HN3</td><td rowspan="1" colspan="1">118.4</td><td rowspan="1" colspan="1">C6—C7—H7</td><td rowspan="1" colspan="1">119.7</td></tr><tr><td rowspan="1" colspan="1">C9—N4—H4A</td><td rowspan="1" colspan="1">120.0</td><td rowspan="1" colspan="1">C7—C8—C9</td><td rowspan="1" colspan="1">120.1 (4)</td></tr><tr><td rowspan="1" colspan="1">C9—N4—H4B</td><td rowspan="1" colspan="1">120.0</td><td rowspan="1" colspan="1">C7—C8—H8</td><td rowspan="1" colspan="1">120.0</td></tr><tr><td rowspan="1" colspan="1">H4A—N4—H4B</td><td rowspan="1" colspan="1">120.0</td><td rowspan="1" colspan="1">C9—C8—H8</td><td rowspan="1" colspan="1">120.0</td></tr><tr><td rowspan="1" colspan="1">C4—C1—C3</td><td rowspan="1" colspan="1">119.2 (4)</td><td rowspan="1" colspan="1">N4—C9—N3</td><td rowspan="1" colspan="1">118.9 (4)</td></tr><tr><td rowspan="1" colspan="1">C4—C1—Cl5</td><td rowspan="1" colspan="1">119.4 (3)</td><td rowspan="1" colspan="1">N4—C9—C8</td><td rowspan="1" colspan="1">123.1 (4)</td></tr><tr><td rowspan="1" colspan="1">C3—C1—Cl5</td><td rowspan="1" colspan="1">121.4 (3)</td><td rowspan="1" colspan="1">N3—C9—C8</td><td rowspan="1" colspan="1">117.9 (4)</td></tr><tr><td rowspan="1" colspan="1">C3—C2—C5</td><td rowspan="1" colspan="1">119.9 (4)</td><td rowspan="1" colspan="1">N3—C10—C6</td><td rowspan="1" colspan="1">119.2 (4)</td></tr><tr><td rowspan="1" colspan="1">C3—C2—H2</td><td rowspan="1" colspan="1">120.0</td><td rowspan="1" colspan="1">N3—C10—H10</td><td rowspan="1" colspan="1">120.4</td></tr><tr><td rowspan="1" colspan="1">C5—C2—H2</td><td rowspan="1" colspan="1">120.0</td><td rowspan="1" colspan="1">C6—C10—H10</td><td rowspan="1" colspan="1">120.4</td></tr></table></table-wrap></sec><sec id="tablewraphbondslong"><title>Hydrogen-bond geometry (Å, º)</title><table-wrap position="anchor" id="d1e1802"><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">N1—H1<italic>A</italic>···Cl4<sup>i</sup></td><td rowspan="1" colspan="1">0.86</td><td rowspan="1" colspan="1">2.64</td><td rowspan="1" colspan="1">3.400 (4)</td><td rowspan="1" colspan="1">148</td></tr><tr><td rowspan="1" colspan="1">N1—H1<italic>B</italic>···Cl3<sup>ii</sup></td><td rowspan="1" colspan="1">0.86</td><td rowspan="1" colspan="1">2.47</td><td rowspan="1" colspan="1">3.317 (3)</td><td rowspan="1" colspan="1">169</td></tr><tr><td rowspan="1" colspan="1">N2—H<italic>N</italic>2···Cl4<sup>i</sup></td><td rowspan="1" colspan="1">0.86</td><td rowspan="1" colspan="1">2.42</td><td rowspan="1" colspan="1">3.238 (3)</td><td rowspan="1" colspan="1">160</td></tr><tr><td rowspan="1" colspan="1">N3—H<italic>N</italic>3···Cl1<sup>iii</sup></td><td rowspan="1" colspan="1">0.86</td><td rowspan="1" colspan="1">2.42</td><td rowspan="1" colspan="1">3.251 (3)</td><td rowspan="1" colspan="1">164</td></tr><tr><td rowspan="1" colspan="1">N4—H4<italic>A</italic>···Cl1<sup>iii</sup></td><td rowspan="1" colspan="1">0.86</td><td rowspan="1" colspan="1">2.77</td><td rowspan="1" colspan="1">3.519 (4)</td><td rowspan="1" colspan="1">147</td></tr><tr><td rowspan="1" colspan="1">N4—H4<italic>B</italic>···Cl2<sup>iv</sup></td><td rowspan="1" colspan="1">0.86</td><td rowspan="1" colspan="1">2.80</td><td rowspan="1" colspan="1">3.541 (4)</td><td rowspan="1" colspan="1">145</td></tr></table></table-wrap><p>Symmetry codes: (i) −<italic>x</italic>+2, −<italic>y</italic>+1, −<italic>z</italic>+1; (ii) <italic>x</italic>, −<italic>y</italic>+3/2, <italic>z</italic>+1/2; (iii) −<italic>x</italic>+1, <italic>y</italic>+1/2, −<italic>z</italic>+1/2; (iv) −<italic>x</italic>+1, −<italic>y</italic>+1, −<italic>z</italic>+1.</p></sec></app></app-group><ref-list><title>References</title><ref id="bb1"><mixed-citation publication-type="other">Brandenburg, K. 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Chem.</italic><bold>40</bold>, 772–778.</mixed-citation></ref></ref-list></back><floats-group><fig id="fig1" position="float"><label>Figure 1</label><caption><p>The molecular entities of (C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[CoCl<sub>4</sub>], showing the atom-numbering scheme. Displacement ellipsoids are drawn at the 50% probability level.</p></caption><graphic xlink:href="e-71-00555-fig1"></graphic></fig><fig id="fig2" position="float"><label>Figure 2</label><caption><p>The environment of the CoCl<sub>4</sub> tetrahedron.</p></caption><graphic xlink:href="e-71-00555-fig2"></graphic></fig><fig id="fig3" position="float"><label>Figure 3</label><caption><p>The environment around the cations (cat1 or cat2).</p></caption><graphic xlink:href="e-71-00555-fig3"></graphic></fig><fig id="fig4" position="float"><label>Figure 4</label><caption><p>Projection of the crystal structure along [010] showing the –cat1–[CoCl<sub>4</sub>]–cat2–[CoCl<sub>4</sub>]– sequence stacked along [100].</p></caption><graphic xlink:href="e-71-00555-fig4"></graphic></fig><fig id="fig5" position="float"><label>Figure 5</label><caption><p>Projection of the crystal structure along [001] showing the layered character of the hydrogen-bonded components.</p></caption><graphic xlink:href="e-71-00555-fig5"></graphic></fig><table-wrap id="table1" position="float"><label>Table 1</label><caption><title>Hydrogen-bond geometry (, )</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 rowspan="1" colspan="1" align="left" valign="top">N1H1<italic>A</italic>Cl4<sup>i</sup></td><td rowspan="1" colspan="1" align="left" valign="top">0.86</td><td rowspan="1" colspan="1" align="left" valign="top">2.64</td><td rowspan="1" colspan="1" align="left" valign="top">3.400(4)</td><td rowspan="1" colspan="1" align="left" valign="top">148</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">N1H1<italic>B</italic>Cl3<sup>ii</sup></td><td rowspan="1" colspan="1" align="left" valign="top">0.86</td><td rowspan="1" colspan="1" align="left" valign="top">2.47</td><td rowspan="1" colspan="1" align="left" valign="top">3.317(3)</td><td rowspan="1" colspan="1" align="left" valign="top">169</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">N2H<italic>N</italic>2Cl4<sup>i</sup></td><td rowspan="1" colspan="1" align="left" valign="top">0.86</td><td rowspan="1" colspan="1" align="left" valign="top">2.42</td><td rowspan="1" colspan="1" align="left" valign="top">3.238(3)</td><td rowspan="1" colspan="1" align="left" valign="top">160</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">N3H<italic>N</italic>3Cl1<sup>iii</sup></td><td rowspan="1" colspan="1" align="left" valign="top">0.86</td><td rowspan="1" colspan="1" align="left" valign="top">2.42</td><td rowspan="1" colspan="1" align="left" valign="top">3.251(3)</td><td rowspan="1" colspan="1" align="left" valign="top">164</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">N4H4<italic>A</italic>Cl1<sup>iii</sup></td><td rowspan="1" colspan="1" align="left" valign="top">0.86</td><td rowspan="1" colspan="1" align="left" valign="top">2.77</td><td rowspan="1" colspan="1" align="left" valign="top">3.519(4)</td><td rowspan="1" colspan="1" align="left" valign="top">147</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">N4H4<italic>B</italic>Cl2<sup>iv</sup></td><td rowspan="1" colspan="1" align="left" valign="top">0.86</td><td rowspan="1" colspan="1" align="left" valign="top">2.80</td><td rowspan="1" colspan="1" align="left" valign="top">3.541(4)</td><td rowspan="1" colspan="1" align="left" valign="top">145</td></tr></tbody></table><table-wrap-foot><p>Symmetry codes: (i) <inline-formula><inline-graphic xlink:href="e-71-00555-efi1.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula>; (ii) <inline-formula><inline-graphic xlink:href="e-71-00555-efi2.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula>; (iii) <inline-formula><inline-graphic xlink:href="e-71-00555-efi3.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula>; (iv) <inline-formula><inline-graphic xlink:href="e-71-00555-efi4.jpg" mimetype="image" mime-subtype="gif"></inline-graphic></inline-formula>.</p></table-wrap-foot></table-wrap><table-wrap id="table2" position="float"><label>Table 2</label><caption><title>Experimental details</title></caption><table frame="hsides" rules="groups"><tbody valign="top"><tr><td rowspan="1" colspan="2" align="left" valign="top">Crystal data</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">Chemical formula</td><td rowspan="1" colspan="1" align="left" valign="top">(C<sub>5</sub>H<sub>6</sub>ClN<sub>2</sub>)<sub>2</sub>[CoCl<sub>4</sub>]</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top"><italic>M</italic><sub>r</sub></td><td rowspan="1" colspan="1" align="left" valign="top">459.87</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">Crystal system, space group</td><td rowspan="1" colspan="1" align="left" valign="top">Monoclinic, <italic>P</italic>2<sub>1</sub>/<italic>c</italic></td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">Temperature (K)</td><td rowspan="1" colspan="1" align="left" valign="top">298</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top"><italic>a</italic>, <italic>b</italic>, <italic>c</italic> ()</td><td rowspan="1" colspan="1" align="left" valign="top">13.519(2), 14.945(3), 8.725(2)</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top"> ()</td><td rowspan="1" colspan="1" align="left" valign="top">92.858(3)</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top"><italic>V</italic> (<sup>3</sup>)</td><td rowspan="1" colspan="1" align="left" valign="top">1760.6(6)</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top"><italic>Z</italic></td><td rowspan="1" colspan="1" align="left" valign="top">4</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">Radiation type</td><td rowspan="1" colspan="1" align="left" valign="top">Mo <italic>K</italic></td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top"> (mm<sup>1</sup>)</td><td rowspan="1" colspan="1" align="left" valign="top">1.88</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">Crystal size (mm)</td><td rowspan="1" colspan="1" align="left" valign="top">0.5 0.3 0.2</td></tr><tr><td rowspan="1" colspan="2" align="left" valign="top"> </td></tr><tr><td rowspan="1" colspan="2" align="left" valign="top">Data collection</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">Diffractometer</td><td rowspan="1" colspan="1" align="left" valign="top">EnrafNonius CAD-4</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">Absorption correction</td><td rowspan="1" colspan="1" align="left" valign="top"> scan (North <italic>et al.</italic>, 1968<xref ref-type="bibr" rid="bb13"> ▸</xref>)</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top"><italic>T</italic><sub>min</sub>, <italic>T</italic><sub>max</sub></td><td rowspan="1" colspan="1" align="left" valign="top">0.423, 0.649</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">No. of measured, independent and observed [<italic>I</italic> > 2(<italic>I</italic>)] reflections</td><td rowspan="1" colspan="1" align="left" valign="top">6241, 3707, 2121</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top"><italic>R</italic><sub>int</sub></td><td rowspan="1" colspan="1" align="left" valign="top">0.039</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">(sin /)<sub>max</sub> (<sup>1</sup>)</td><td rowspan="1" colspan="1" align="left" valign="top">0.638</td></tr><tr><td rowspan="1" colspan="2" align="left" valign="top"> </td></tr><tr><td rowspan="1" colspan="2" align="left" valign="top">Refinement</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top"><italic>R</italic>[<italic>F</italic><sup>2</sup> > 2(<italic>F</italic><sup>2</sup>)], <italic>wR</italic>(<italic>F</italic><sup>2</sup>), <italic>S</italic></td><td rowspan="1" colspan="1" align="left" valign="top">0.041, 0.109, 0.99</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">No. of reflections</td><td rowspan="1" colspan="1" align="left" valign="top">3707</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">No. of parameters</td><td rowspan="1" colspan="1" align="left" valign="top">190</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top">H-atom treatment</td><td rowspan="1" colspan="1" align="left" valign="top">H-atom parameters not refined</td></tr><tr><td rowspan="1" colspan="1" align="left" valign="top"><sub>max</sub>, <sub>min</sub> (e <sup>3</sup>)</td><td rowspan="1" colspan="1" align="left" valign="top">0.52, 0.34</td></tr></tbody></table><table-wrap-foot><p>Computer programs: <italic>CAD-4 EXPRESS</italic> (EnrafNonius, 1994<xref ref-type="bibr" rid="bb5"> ▸</xref>), <italic>XCAD4</italic> (Harms Wocadlo, 1995<xref ref-type="bibr" rid="bb7"> ▸</xref>), <italic>SHELXS97</italic> and <italic>SHELXL97</italic> (Sheldrick, 2008<xref ref-type="bibr" rid="bb17"> ▸</xref>), <italic>DIAMOND</italic> (Brandenburg, 2008<xref ref-type="bibr" rid="bb1"> ▸</xref>) and <italic>publCIF</italic> (Westrip, 2010<xref ref-type="bibr" rid="bb18"> ▸</xref>).</p></table-wrap-foot></table-wrap></floats-group></pmc></record>Pour manipuler 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