One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel Aqua(2,9-dimethyl-1,10-phenanthroline)NiCl2 Complex
Identifieur interne : 000037 ( Pmc/Curation ); précédent : 000036; suivant : 000038One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel Aqua(2,9-dimethyl-1,10-phenanthroline)NiCl2 Complex
Auteurs : Assem Barakat ; Mousa Al-Noaimi ; Mohammed Suleiman ; Abdullah S. Aldwayyan ; Belkheir Hammouti ; Taibi Ben Hadda ; Salim F. Haddad ; Ahmed Boshaala ; Ismail WaradSource :
- International Journal of Molecular Sciences [ 1422-0067 ] ; 2013.
Abstract
[NiCl2(C14H12N2)(H2O)] complex has been synthesized from nickel chloride hexahydrate (NiCl2·6H2O) and 2,9-dimethyl-1,10-phenanthroline (dmphen) as
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DOI: 10.3390/ijms141223941
PubMed: 24351867
PubMed Central: 3876087
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel <italic>Aqua</italic>(2,9-dimethyl-1,10-phenanthroline)NiCl<sub>2</sub> Complex</title><author><name sortKey="Barakat, Assem" sort="Barakat, Assem" uniqKey="Barakat A" first="Assem" last="Barakat">Assem Barakat</name><affiliation><nlm:aff id="af1-ijms-14-23941">Department of Chemistry, King Saud University, P.O. Box 2455, Riyadh 11451, Saudi Arabia; E-Mail:<email>ambarakat@ksu.edu.sa</email></nlm:aff></affiliation></author><author><name sortKey="Al Noaimi, Mousa" sort="Al Noaimi, Mousa" uniqKey="Al Noaimi M" first="Mousa" last="Al-Noaimi">Mousa Al-Noaimi</name><affiliation><nlm:aff id="af2-ijms-14-23941">Department of Chemistry, Hashemite University, Zarqa 13115, Jordan; E-Mail:<email>manoaimi@hu.edu.jo</email></nlm:aff></affiliation></author><author><name sortKey="Suleiman, Mohammed" sort="Suleiman, Mohammed" uniqKey="Suleiman M" first="Mohammed" last="Suleiman">Mohammed Suleiman</name><affiliation><nlm:aff id="af3-ijms-14-23941">Department of Chemistry, Science College, AN-Najah National University, P.O. Box 7, Nablus, Palestine; E-Mail:<email>suleimanshtaya@najah.edu</email></nlm:aff></affiliation></author><author><name sortKey="Aldwayyan, Abdullah S" sort="Aldwayyan, Abdullah S" uniqKey="Aldwayyan A" first="Abdullah S." last="Aldwayyan">Abdullah S. Aldwayyan</name><affiliation><nlm:aff id="af4-ijms-14-23941">Department of Physics and Astronomy, King Saud University, P.O. Box 2455, Riyadh 11451, Saudi Arabia; E-Mail:<email>dwayyan@ksu.edu.sa</email></nlm:aff></affiliation></author><author><name sortKey="Hammouti, Belkheir" sort="Hammouti, Belkheir" uniqKey="Hammouti B" first="Belkheir" last="Hammouti">Belkheir Hammouti</name><affiliation><nlm:aff id="af5-ijms-14-23941">Laboratoire de Chimie Appliquée et Environnement, LCAE-URAC18, Faculity of Science, University Mohammed Premier, Oujda 60000, Morocco; E-Mail:<email>hammoutib@gmail.com</email></nlm:aff></affiliation></author><author><name sortKey="Ben Hadda, Taibi" sort="Ben Hadda, Taibi" uniqKey="Ben Hadda T" first="Taibi" last="Ben Hadda">Taibi Ben Hadda</name><affiliation><nlm:aff id="af6-ijms-14-23941">Lab of Chemical Material, FSO, University Mohammed Premier, Oujda 60000, Morocco; E-Mail:<email>taibi.ben.hadda@gmail.com</email></nlm:aff></affiliation></author><author><name sortKey="Haddad, Salim F" sort="Haddad, Salim F" uniqKey="Haddad S" first="Salim F." last="Haddad">Salim F. Haddad</name><affiliation><nlm:aff id="af7-ijms-14-23941">Department of Chemistry, the University of Jordan, Amman 11942, Jordan; E-Mail:<email>hadsal2003@yahoo.com</email></nlm:aff></affiliation></author><author><name sortKey="Boshaala, Ahmed" sort="Boshaala, Ahmed" uniqKey="Boshaala A" first="Ahmed" last="Boshaala">Ahmed Boshaala</name><affiliation><nlm:aff id="af8-ijms-14-23941">Department of Chemistry, Faculty of Science, Benghazi University, P.O. Box 1308, Benghazi 5341, Libya; E-Mail:<email>ahmedboshaala@yahoo.co.uk</email></nlm:aff></affiliation></author><author><name sortKey="Warad, Ismail" sort="Warad, Ismail" uniqKey="Warad I" first="Ismail" last="Warad">Ismail Warad</name><affiliation><nlm:aff id="af3-ijms-14-23941">Department of Chemistry, Science College, AN-Najah National University, P.O. Box 7, Nablus, Palestine; E-Mail:<email>suleimanshtaya@najah.edu</email></nlm:aff></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">PMC</idno><idno type="pmid">24351867</idno><idno type="pmc">3876087</idno><idno type="url">http://www.ncbi.nlm.nih.gov/pmc/articles/PMC3876087</idno><idno type="RBID">PMC:3876087</idno><idno type="doi">10.3390/ijms141223941</idno><date when="2013">2013</date><idno type="wicri:Area/Pmc/Corpus">000037</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Corpus" wicri:corpus="PMC">000037</idno><idno type="wicri:Area/Pmc/Curation">000037</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Curation">000037</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en" level="a" type="main">One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel <italic>Aqua</italic>(2,9-dimethyl-1,10-phenanthroline)NiCl<sub>2</sub> Complex</title><author><name sortKey="Barakat, Assem" sort="Barakat, Assem" uniqKey="Barakat A" first="Assem" last="Barakat">Assem Barakat</name><affiliation><nlm:aff id="af1-ijms-14-23941">Department of Chemistry, King Saud University, P.O. Box 2455, Riyadh 11451, Saudi Arabia; E-Mail:<email>ambarakat@ksu.edu.sa</email></nlm:aff></affiliation></author><author><name sortKey="Al Noaimi, Mousa" sort="Al Noaimi, Mousa" uniqKey="Al Noaimi M" first="Mousa" last="Al-Noaimi">Mousa Al-Noaimi</name><affiliation><nlm:aff id="af2-ijms-14-23941">Department of Chemistry, Hashemite University, Zarqa 13115, Jordan; E-Mail:<email>manoaimi@hu.edu.jo</email></nlm:aff></affiliation></author><author><name sortKey="Suleiman, Mohammed" sort="Suleiman, Mohammed" uniqKey="Suleiman M" first="Mohammed" last="Suleiman">Mohammed Suleiman</name><affiliation><nlm:aff id="af3-ijms-14-23941">Department of Chemistry, Science College, AN-Najah National University, P.O. Box 7, Nablus, Palestine; E-Mail:<email>suleimanshtaya@najah.edu</email></nlm:aff></affiliation></author><author><name sortKey="Aldwayyan, Abdullah S" sort="Aldwayyan, Abdullah S" uniqKey="Aldwayyan A" first="Abdullah S." last="Aldwayyan">Abdullah S. Aldwayyan</name><affiliation><nlm:aff id="af4-ijms-14-23941">Department of Physics and Astronomy, King Saud University, P.O. Box 2455, Riyadh 11451, Saudi Arabia; E-Mail:<email>dwayyan@ksu.edu.sa</email></nlm:aff></affiliation></author><author><name sortKey="Hammouti, Belkheir" sort="Hammouti, Belkheir" uniqKey="Hammouti B" first="Belkheir" last="Hammouti">Belkheir Hammouti</name><affiliation><nlm:aff id="af5-ijms-14-23941">Laboratoire de Chimie Appliquée et Environnement, LCAE-URAC18, Faculity of Science, University Mohammed Premier, Oujda 60000, Morocco; E-Mail:<email>hammoutib@gmail.com</email></nlm:aff></affiliation></author><author><name sortKey="Ben Hadda, Taibi" sort="Ben Hadda, Taibi" uniqKey="Ben Hadda T" first="Taibi" last="Ben Hadda">Taibi Ben Hadda</name><affiliation><nlm:aff id="af6-ijms-14-23941">Lab of Chemical Material, FSO, University Mohammed Premier, Oujda 60000, Morocco; E-Mail:<email>taibi.ben.hadda@gmail.com</email></nlm:aff></affiliation></author><author><name sortKey="Haddad, Salim F" sort="Haddad, Salim F" uniqKey="Haddad S" first="Salim F." last="Haddad">Salim F. Haddad</name><affiliation><nlm:aff id="af7-ijms-14-23941">Department of Chemistry, the University of Jordan, Amman 11942, Jordan; E-Mail:<email>hadsal2003@yahoo.com</email></nlm:aff></affiliation></author><author><name sortKey="Boshaala, Ahmed" sort="Boshaala, Ahmed" uniqKey="Boshaala A" first="Ahmed" last="Boshaala">Ahmed Boshaala</name><affiliation><nlm:aff id="af8-ijms-14-23941">Department of Chemistry, Faculty of Science, Benghazi University, P.O. Box 1308, Benghazi 5341, Libya; E-Mail:<email>ahmedboshaala@yahoo.co.uk</email></nlm:aff></affiliation></author><author><name sortKey="Warad, Ismail" sort="Warad, Ismail" uniqKey="Warad I" first="Ismail" last="Warad">Ismail Warad</name><affiliation><nlm:aff id="af3-ijms-14-23941">Department of Chemistry, Science College, AN-Najah National University, P.O. Box 7, Nablus, Palestine; E-Mail:<email>suleimanshtaya@najah.edu</email></nlm:aff></affiliation></author></analytic><series><title level="j">International Journal of Molecular Sciences</title><idno type="eISSN">1422-0067</idno><imprint><date when="2013">2013</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en"><p>[NiCl<sub>2</sub>(C<sub>14</sub>H<sub>12</sub>N<sub>2</sub>)(H<sub>2</sub>O)] complex has been synthesized from nickel chloride hexahydrate (NiCl<sub>2</sub>·6H<sub>2</sub>O) and 2,9-dimethyl-1,10-phenanthroline (dmphen) as <italic>N</italic>,<italic>N</italic>-bidentate ligand. The synthesized complex was characterized by elemental analysis, infrared (IR) spectroscopy, ultraviolet-visible (UV-vis) spectroscopy and differential thermal/thermogravimetric analysis (TG/DTA). The complex was further confirmed by single crystal X-ray diffraction (XRD) as triclinic with space group P-1. The desired complex, subjected to thermal decomposition at low temperature of 400 ºC in an open atmosphere, revealed a novel and facile synthesis of pure NiO nanoparticles with uniform spherical particle; the structure of the NiO nanoparticles product was elucidated on the basis of Fourier transform infrared (FT-IR), UV-vis spectroscopy, TG/DTA, XRD, scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDXS) and transmission electron microscopy (TEM).</p></div></front><back><div1 type="bibliography"><listBibl><biblStruct><analytic><author><name sortKey="Wei, W" uniqKey="Wei W">W. Wei</name></author><author><name sortKey="Jiang, X" uniqKey="Jiang X">X. Jiang</name></author><author><name sortKey="Lu, L" uniqKey="Lu L">L. Lu</name></author><author><name sortKey="Yang, X" uniqKey="Yang X">X. 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<front><journal-meta><journal-id journal-id-type="nlm-ta">Int J Mol Sci</journal-id><journal-id journal-id-type="iso-abbrev">Int J Mol Sci</journal-id><journal-id journal-id-type="publisher-id">ijms</journal-id><journal-title-group><journal-title>International Journal of Molecular Sciences</journal-title></journal-title-group><issn pub-type="epub">1422-0067</issn><publisher><publisher-name>Molecular Diversity Preservation International (MDPI)</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="pmid">24351867</article-id><article-id pub-id-type="pmc">3876087</article-id><article-id pub-id-type="doi">10.3390/ijms141223941</article-id><article-id pub-id-type="publisher-id">ijms-14-23941</article-id><article-categories><subj-group subj-group-type="heading"><subject>Article</subject></subj-group></article-categories><title-group><article-title>One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel <italic>Aqua</italic>(2,9-dimethyl-1,10-phenanthroline)NiCl<sub>2</sub> Complex</article-title></title-group><contrib-group><contrib contrib-type="author"><name><surname>Barakat</surname><given-names>Assem</given-names></name><xref ref-type="aff" rid="af1-ijms-14-23941">1</xref></contrib><contrib contrib-type="author"><name><surname>Al-Noaimi</surname><given-names>Mousa</given-names></name><xref ref-type="aff" rid="af2-ijms-14-23941">2</xref></contrib><contrib contrib-type="author"><name><surname>Suleiman</surname><given-names>Mohammed</given-names></name><xref ref-type="aff" rid="af3-ijms-14-23941">3</xref></contrib><contrib contrib-type="author"><name><surname>Aldwayyan</surname><given-names>Abdullah S.</given-names></name><xref ref-type="aff" rid="af4-ijms-14-23941">4</xref></contrib><contrib contrib-type="author"><name><surname>Hammouti</surname><given-names>Belkheir</given-names></name><xref ref-type="aff" rid="af5-ijms-14-23941">5</xref></contrib><contrib contrib-type="author"><name><surname>Ben Hadda</surname><given-names>Taibi</given-names></name><xref ref-type="aff" rid="af6-ijms-14-23941">6</xref></contrib><contrib contrib-type="author"><name><surname>Haddad</surname><given-names>Salim F.</given-names></name><xref ref-type="aff" rid="af7-ijms-14-23941">7</xref></contrib><contrib contrib-type="author"><name><surname>Boshaala</surname><given-names>Ahmed</given-names></name><xref ref-type="aff" rid="af8-ijms-14-23941">8</xref></contrib><contrib contrib-type="author"><name><surname>Warad</surname><given-names>Ismail</given-names></name><xref ref-type="aff" rid="af3-ijms-14-23941">3</xref><xref rid="c1-ijms-14-23941" ref-type="corresp">*</xref></contrib></contrib-group><aff id="af1-ijms-14-23941"><label>1</label>Department of Chemistry, King Saud University, P.O. Box 2455, Riyadh 11451, Saudi Arabia; E-Mail:<email>ambarakat@ksu.edu.sa</email></aff><aff id="af2-ijms-14-23941"><label>2</label>Department of Chemistry, Hashemite University, Zarqa 13115, Jordan; E-Mail:<email>manoaimi@hu.edu.jo</email></aff><aff id="af3-ijms-14-23941"><label>3</label>Department of Chemistry, Science College, AN-Najah National University, P.O. Box 7, Nablus, Palestine; E-Mail:<email>suleimanshtaya@najah.edu</email></aff><aff id="af4-ijms-14-23941"><label>4</label>Department of Physics and Astronomy, King Saud University, P.O. Box 2455, Riyadh 11451, Saudi Arabia; E-Mail:<email>dwayyan@ksu.edu.sa</email></aff><aff id="af5-ijms-14-23941"><label>5</label>Laboratoire de Chimie Appliquée et Environnement, LCAE-URAC18, Faculity of Science, University Mohammed Premier, Oujda 60000, Morocco; E-Mail:<email>hammoutib@gmail.com</email></aff><aff id="af6-ijms-14-23941"><label>6</label>Lab of Chemical Material, FSO, University Mohammed Premier, Oujda 60000, Morocco; E-Mail:<email>taibi.ben.hadda@gmail.com</email></aff><aff id="af7-ijms-14-23941"><label>7</label>Department of Chemistry, the University of Jordan, Amman 11942, Jordan; E-Mail:<email>hadsal2003@yahoo.com</email></aff><aff id="af8-ijms-14-23941"><label>8</label>Department of Chemistry, Faculty of Science, Benghazi University, P.O. Box 1308, Benghazi 5341, Libya; E-Mail:<email>ahmedboshaala@yahoo.co.uk</email></aff><author-notes><corresp id="c1-ijms-14-23941"><label>*</label>Author to whom correspondence should be addressed; E-Mail: <email>warad@najah.edu</email>; Tel.: +972-9234-5113; Fax: +972-9234-5982.</corresp></author-notes><pub-date pub-type="collection"><month>12</month><year>2013</year></pub-date><pub-date pub-type="epub"><day>09</day><month>12</month><year>2013</year></pub-date><volume>14</volume><issue>12</issue><fpage>23941</fpage><lpage>23954</lpage><history><date date-type="received"><day>23</day><month>10</month><year>2013</year></date><date date-type="rev-recd"><day>13</day><month>11</month><year>2013</year></date><date date-type="accepted"><day>25</day><month>11</month><year>2013</year></date></history><permissions><copyright-statement>© 2013 by the authors; licensee MDPI, Basel, Switzerland</copyright-statement><copyright-year>2013</copyright-year><license license-type="open-access" xlink:href="http://creativecommons.org/licenses/by/3.0/"><license-p>This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution license (<ext-link ext-link-type="uri" xlink:href="http://creativecommons.org/licenses/by/3.0/">http://creativecommons.org/licenses/by/3.0/</ext-link>).</license-p></license></permissions><abstract><p>[NiCl<sub>2</sub>(C<sub>14</sub>H<sub>12</sub>N<sub>2</sub>)(H<sub>2</sub>O)] complex has been synthesized from nickel chloride hexahydrate (NiCl<sub>2</sub>·6H<sub>2</sub>O) and 2,9-dimethyl-1,10-phenanthroline (dmphen) as <italic>N</italic>,<italic>N</italic>-bidentate ligand. The synthesized complex was characterized by elemental analysis, infrared (IR) spectroscopy, ultraviolet-visible (UV-vis) spectroscopy and differential thermal/thermogravimetric analysis (TG/DTA). The complex was further confirmed by single crystal X-ray diffraction (XRD) as triclinic with space group P-1. The desired complex, subjected to thermal decomposition at low temperature of 400 ºC in an open atmosphere, revealed a novel and facile synthesis of pure NiO nanoparticles with uniform spherical particle; the structure of the NiO nanoparticles product was elucidated on the basis of Fourier transform infrared (FT-IR), UV-vis spectroscopy, TG/DTA, XRD, scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDXS) and transmission electron microscopy (TEM).</p></abstract><kwd-group><kwd>nickel(II) complex</kwd><kwd>thermal decomposition</kwd><kwd>2,9-dimethyl-1,10-phenanthroline</kwd><kwd>nanoparticles</kwd></kwd-group></article-meta></front><floats-group><fig id="f1-ijms-14-23941" position="float"><label>Figure 1.</label><caption><p>TG/DTA thermal curves of the desired complex.</p></caption><graphic xlink:href="ijms-14-23941f1"></graphic></fig><fig id="f2-ijms-14-23941" position="float"><label>Figure 2.</label><caption><p>IR-KBr disk spectra (<bold>a</bold>) desired complex; and (<bold>b</bold>) NiO nanoparticles.</p></caption><graphic xlink:href="ijms-14-23941f2"></graphic></fig><fig id="f3-ijms-14-23941" position="float"><label>Figure 3.</label><caption><p>UV-vis spectrum of the desired complex (<bold>a</bold>) and NiO nanoparticles dissolved in water at room temperature (<bold>b</bold>).</p></caption><graphic xlink:href="ijms-14-23941f3"></graphic></fig><fig id="f4-ijms-14-23941" position="float"><label>Figure 4.</label><caption><p>UV-vis band gap energy.</p></caption><graphic xlink:href="ijms-14-23941f4"></graphic></fig><fig id="f5-ijms-14-23941" position="float"><label>Figure 5.</label><caption><p>EDX spectra (<bold>a</bold>) NiCl<sub>2</sub>(2,9-dimethyl-1,10-phenanthroline)·H<sub>2</sub>O complex; and (<bold>b</bold>) NiO nanoparticles.</p></caption><graphic xlink:href="ijms-14-23941f5"></graphic></fig><fig id="f6-ijms-14-23941" position="float"><label>Figure 6.</label><caption><p>ORTEP (Oak Ridge Thermal Ellipsoid Plot) plot of two molecular units per asymmetric unit in P-1 showing atom labelling. Thermal ellipsoids are drawn at the 50% probability level.</p></caption><graphic xlink:href="ijms-14-23941f6"></graphic></fig><fig id="f7-ijms-14-23941" position="float"><label>Figure 7.</label><caption><p>XRD patterns of NiO nanoparticles via complex thermal decomposed at 400 ºC.</p></caption><graphic xlink:href="ijms-14-23941f7"></graphic></fig><fig id="f8-ijms-14-23941" position="float"><label>Figure 8.</label><caption><p>SEM micrographs (<bold>a</bold>) NiCl<sub>2</sub>(2,9-dimethyl-1,10-phenanthroline)·H<sub>2</sub>O complex and (<bold>b</bold>) NiO nanoparticles.</p></caption><graphic xlink:href="ijms-14-23941f8"></graphic></fig><fig id="f9-ijms-14-23941" position="float"><label>Figure 9.</label><caption><p>TEM micrographs (<bold>a</bold>) NiCl<sub>2</sub>(2,9-dimethyl-1,10-phenanthroline)·H<sub>2</sub>O complex and (<bold>b</bold>) NiO nanoparticles.</p></caption><graphic xlink:href="ijms-14-23941f9"></graphic></fig><fig id="f10-ijms-14-23941" position="float"><label>Scheme 1.</label><caption><p>Synthesis of the complex and NiO nanoparticles.</p></caption><graphic xlink:href="ijms-14-23941f10"></graphic></fig><table-wrap id="t1-ijms-14-23941" position="float"><label>Table 1.</label><caption><p>Selected bond distances (Å) and angles (º) of the complex.</p></caption><table frame="hsides" rules="groups"><thead><tr><th align="center" valign="bottom" rowspan="1" colspan="1">Bond</th><th align="center" valign="bottom" rowspan="1" colspan="1">Bond distances (Å)</th></tr></thead><tbody><tr><td align="center" valign="top" rowspan="1" colspan="1">Ni(II)–O(II)</td><td align="center" valign="top" rowspan="1" colspan="1">2.014(2)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Ni(II)–N(III)</td><td align="center" valign="top" rowspan="1" colspan="1">2.044(2)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Ni(II)–N(IV)</td><td align="center" valign="top" rowspan="1" colspan="1">2.046(3)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Ni(II)–Cl(IV)</td><td align="center" valign="top" rowspan="1" colspan="1">2.337(8)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Ni(II)–Cl(III)</td><td align="center" valign="top" rowspan="1" colspan="1">2.347(2)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1"><bold>Angles</bold></td><td align="center" valign="top" rowspan="1" colspan="1"><bold>Angles value (º)</bold></td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">O(II)–Ni(II)–N(III)</td><td align="center" valign="top" rowspan="1" colspan="1">164.61(11)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">O(II)–Ni(II)–N(IV)</td><td align="center" valign="top" rowspan="1" colspan="1">113.61(11)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">N(III)–Ni(II)–N(IV)</td><td align="center" valign="top" rowspan="1" colspan="1">81.75(10)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">O(II)–Ni(II)–Cl(IV)</td><td align="center" valign="top" rowspan="1" colspan="1">87.35(6)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">N(III)–Ni(II)–Cl(IV)</td><td align="center" valign="top" rowspan="1" colspan="1">91.91(7)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">N(IV)–Ni(II)–Cl(IV)</td><td align="center" valign="top" rowspan="1" colspan="1">96.63(7)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">O(II)–Ni(II)–Cl(III)</td><td align="center" valign="top" rowspan="1" colspan="1">87.35(6)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">N(III)–Ni(II)–Cl(III)</td><td align="center" valign="top" rowspan="1" colspan="1">88.27(6)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">N(IV)–Ni(II)–Cl(III)</td><td align="center" valign="top" rowspan="1" colspan="1">102.71(7)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Cl(IV)–Ni(II)–Cl(III)</td><td align="center" valign="top" rowspan="1" colspan="1">160.48(4)</td></tr></tbody></table></table-wrap><table-wrap id="t2-ijms-14-23941" position="float"><label>Table 2.</label><caption><p>Crystal data and structure refinement for the complex.</p></caption><table frame="hsides" rules="groups"><thead><tr><th align="center" valign="bottom" rowspan="1" colspan="1">Parameters</th><th align="center" valign="bottom" rowspan="1" colspan="1">Data</th></tr></thead><tbody><tr><td align="center" valign="top" rowspan="1" colspan="1">Empirical formula</td><td align="center" valign="top" rowspan="1" colspan="1">C<sub>14</sub>H<sub>14</sub>C<sub>l2</sub>N<sub>2</sub>NiO</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Formula weight</td><td align="center" valign="top" rowspan="1" colspan="1">355.9 g/mol</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Temperature</td><td align="center" valign="top" rowspan="1" colspan="1">293.2(2) K</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Wavelength</td><td align="center" valign="top" rowspan="1" colspan="1">0.71073 Å</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Crystal system</td><td align="center" valign="top" rowspan="1" colspan="1">Triclinic</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Space group</td><td align="center" valign="top" rowspan="1" colspan="1">P-1</td></tr><tr><td align="center" valign="middle" rowspan="3" colspan="1">Unit cell dimensions</td><td align="center" valign="middle" rowspan="1" colspan="1"><italic>a</italic> = 7.5511(3) Å, α = 106.680(5)</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1"><italic>b</italic> = 11.5028(7) Å, β = 93.419(4)</td></tr><tr><td align="center" valign="middle" rowspan="1" colspan="1"><italic>c</italic> = 18.9030(11) Å, γ = 103.448(5)</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Volume</td><td align="center" valign="top" rowspan="1" colspan="1">1,515.54(14) Å<sup>3</sup></td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1"><italic>Z</italic> Formula units per unit cell</td><td align="center" valign="top" rowspan="1" colspan="1">4</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Density (calculated)</td><td align="center" valign="top" rowspan="1" colspan="1">1.560 mg/m<sup>3</sup></td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Absorption coefficient</td><td align="center" valign="top" rowspan="1" colspan="1">1.628 mm<sup>−1</sup></td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1"><italic>F</italic>(000)</td><td align="center" valign="top" rowspan="1" colspan="1">728 e/cell</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Crystal size</td><td align="center" valign="top" rowspan="1" colspan="1">0.50 × 0.50 × 0.25 mm<sup>3</sup></td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Theta range for data collection</td><td align="center" valign="top" rowspan="1" colspan="1">2.95º to 25.02º</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Index ranges</td><td align="center" valign="top" rowspan="1" colspan="1">−8 ≤ <italic>h</italic> ≤ 8, −12 ≤ <italic>k</italic> ≤ 13, −22 ≤ <italic>l</italic> ≤ 22</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Reflections collected</td><td align="center" valign="top" rowspan="1" colspan="1">10,281</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Independent reflections</td><td align="center" valign="top" rowspan="1" colspan="1">5,327 [<italic>R</italic><sub>(int)</sub> = 0.0283]</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Completeness to θ = 25.02º</td><td align="center" valign="top" rowspan="1" colspan="1">99.8%</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Absorption correction</td><td align="center" valign="top" rowspan="1" colspan="1">Semi-empirical from equivalents</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Max. and min. transmission</td><td align="center" valign="top" rowspan="1" colspan="1">0.6864 and 0.4966</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Refinement method</td><td align="center" valign="top" rowspan="1" colspan="1">Full-matrix least-squares on <italic>F</italic><sup>2</sup></td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Data/restraints/parameters</td><td align="center" valign="top" rowspan="1" colspan="1">5,327/8/379</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Goodness-of-fit on <italic>F</italic><sup>2</sup></td><td align="center" valign="top" rowspan="1" colspan="1">1.062</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Final <italic>R</italic> indices [<italic>I</italic> > 2σ(<italic>I</italic>)]</td><td align="center" valign="top" rowspan="1" colspan="1"><italic>R</italic>1 = 0.0369, <italic>wR</italic>2 = 0.0756</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1"><italic>R</italic> indices (all data)</td><td align="center" valign="top" rowspan="1" colspan="1"><italic>R</italic>1 = 0.0472, <italic>wR</italic>2 = 0.0816</td></tr><tr><td align="center" valign="top" rowspan="1" colspan="1">Largest difference peak and hole</td><td align="center" valign="top" rowspan="1" colspan="1">0.395 and −0.313 e Å<sup>−3</sup></td></tr></tbody></table></table-wrap></floats-group></pmc></record>Pour manipuler ce document sous Unix (Dilib)
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|texte= One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel Aqua(2,9-dimethyl-1,10-phenanthroline)NiCl2 Complex
}}
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