β-Yb2CdSb2—A Complex Non-Centrosymmetric Zintl Polymorph

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} div.type-section h2 { font-size: 20px; line-height: 26px; font-weight: 300; } div.type-section h3 { margin-left: 15px; margin-bottom: 0px; font-weight: 300; } .journal-tabs .tab-title.active a { } </style> <link rel="stylesheet" href="https://pub.mdpi-res.com/assets/css/slick.css?f38b2db10e01b157?1732286508"> <meta name="title" content="β-Yb2CdSb2—A Complex Non-Centrosymmetric Zintl Polymorph"> <meta name="description" content="The ternary Zintl phase, Yb2CdSb2, was discovered to exist in two different polymorphic forms. In addition to the orthorhombic α-Yb2CdSb2 (space group Cmc21) known for its excellent thermoelectric properties, we present the synthesis and characterization of the crystal and electronic structure of its monoclinic variant, β-Yb2CdSb2. Structural characterization was performed with the single-crystal X-ray diffraction method. β-Yb2CdSb2 crystallizes in a monoclinic crystal system with the non-centrosymmetric space group Cm (Z = 33, a = 81.801(5) Å, b = 4.6186(3) Å, c = 12.6742(7) Å, β = 93.0610(10)°) and constitutes a new structure type. The complex crystal structure of β-Yb2CdSb2 contrasts with the previously studied β-Ca2CdPn2 (Pn = P, As, Sb) polymorphs, although it shares similar structural features. It consists of three different layers, made of corner-sharing [CdSb4] tetrahedra and stacked in the ABC sequence. The layers are interconnected via [CdSb3] trigonal planar units. Multiple Yb and Cd atomic sites exhibit partial occupancy, resulting in extensive structural disorder. Valence electron partitioning within the Zintl–Klemm formalism yields the formulation (Yb2+)1.98(Cd2+)1.01(Sb3−)2(h+)0.02, highlighting the nearly charge-balanced composition. Detailed electronic structure calculations reveal the closed band gap and presumably semimetallic nature of β-Yb2CdSb2 with the band structure features hinting at potential topological properties." > <link rel="image_src" href="https://pub.mdpi-res.com/img/journals/crystals-logo.png?a2c22e8538083c0b" > <meta name="dc.title" content="β-Yb2CdSb2—A Complex Non-Centrosymmetric Zintl Polymorph"> <meta name="dc.creator" content="Spencer R. Watts"> <meta name="dc.creator" content="Larissa Najera"> <meta name="dc.creator" content="Michael O. Ogunbunmi"> <meta name="dc.creator" content="Svilen Bobev"> <meta name="dc.creator" content="Sviatoslav Baranets"> <meta name="dc.type" content="Article"> <meta name="dc.source" content="Crystals 2024, Vol. 14, Page 920"> <meta name="dc.date" content="2024-10-25"> <meta name ="dc.identifier" content="10.3390/cryst14110920"> <meta name="dc.publisher" content="Multidisciplinary Digital Publishing Institute"> <meta name="dc.rights" content="http://creativecommons.org/licenses/by/3.0/"> <meta name="dc.format" content="application/pdf" > <meta name="dc.language" content="en" > <meta name="dc.description" content="The ternary Zintl phase, Yb2CdSb2, was discovered to exist in two different polymorphic forms. In addition to the orthorhombic α-Yb2CdSb2 (space group Cmc21) known for its excellent thermoelectric properties, we present the synthesis and characterization of the crystal and electronic structure of its monoclinic variant, β-Yb2CdSb2. Structural characterization was performed with the single-crystal X-ray diffraction method. β-Yb2CdSb2 crystallizes in a monoclinic crystal system with the non-centrosymmetric space group Cm (Z = 33, a = 81.801(5) Å, b = 4.6186(3) Å, c = 12.6742(7) Å, β = 93.0610(10)°) and constitutes a new structure type. The complex crystal structure of β-Yb2CdSb2 contrasts with the previously studied β-Ca2CdPn2 (Pn = P, As, Sb) polymorphs, although it shares similar structural features. It consists of three different layers, made of corner-sharing [CdSb4] tetrahedra and stacked in the ABC sequence. The layers are interconnected via [CdSb3] trigonal planar units. Multiple Yb and Cd atomic sites exhibit partial occupancy, resulting in extensive structural disorder. Valence electron partitioning within the Zintl–Klemm formalism yields the formulation (Yb2+)1.98(Cd2+)1.01(Sb3−)2(h+)0.02, highlighting the nearly charge-balanced composition. Detailed electronic structure calculations reveal the closed band gap and presumably semimetallic nature of β-Yb2CdSb2 with the band structure features hinting at potential topological properties." > <meta name="dc.subject" content="Zintl phases" > <meta name="dc.subject" content="single-crystal X-ray diffraction" > <meta name="dc.subject" content="charge balance" > <meta name="dc.subject" content="structural disorder" > <meta name="dc.subject" content="topological insulators" > <meta name ="prism.issn" content="2073-4352"> <meta name ="prism.publicationName" content="Crystals"> <meta name ="prism.publicationDate" content="2024-10-25"> <meta name ="prism.volume" content="14"> <meta name ="prism.number" content="11"> <meta name ="prism.section" content="Article" > <meta name ="prism.startingPage" content="920" > <meta name="citation_issn" content="2073-4352"> <meta name="citation_journal_title" content="Crystals"> <meta name="citation_publisher" content="Multidisciplinary Digital Publishing Institute"> <meta name="citation_title" content="β-Yb2CdSb2—A Complex Non-Centrosymmetric Zintl Polymorph"> <meta name="citation_publication_date" content="2024/11"> <meta name="citation_online_date" content="2024/10/25"> <meta name="citation_volume" content="14"> <meta name="citation_issue" content="11"> <meta name="citation_firstpage" content="920"> <meta name="citation_author" content="Watts, Spencer R."> <meta name="citation_author" content="Najera, Larissa"> <meta name="citation_author" content="Ogunbunmi, Michael O."> <meta name="citation_author" content="Bobev, Svilen"> <meta name="citation_author" content="Baranets, Sviatoslav"> <meta name="citation_doi" content="10.3390/cryst14110920"> <meta name="citation_id" content="mdpi-cryst14110920"> <meta name="citation_abstract_html_url" content="https://www.mdpi.com/2073-4352/14/11/920"> <meta name="citation_pdf_url" content="https://www.mdpi.com/2073-4352/14/11/920/pdf?version=1729846639"> <link rel="alternate" type="application/pdf" title="PDF Full-Text" href="https://www.mdpi.com/2073-4352/14/11/920/pdf?version=1729846639"> <meta name="fulltext_pdf" content="https://www.mdpi.com/2073-4352/14/11/920/pdf?version=1729846639"> <meta name="citation_fulltext_html_url" content="https://www.mdpi.com/2073-4352/14/11/920/htm"> <link rel="alternate" type="text/html" title="HTML Full-Text" href="https://www.mdpi.com/2073-4352/14/11/920/htm"> <meta name="fulltext_html" content="https://www.mdpi.com/2073-4352/14/11/920/htm"> <link rel="alternate" type="text/xml" title="XML Full-Text" href="https://www.mdpi.com/2073-4352/14/11/920/xml"> <meta name="fulltext_xml" content="https://www.mdpi.com/2073-4352/14/11/920/xml"> <meta name="citation_xml_url" content="https://www.mdpi.com/2073-4352/14/11/920/xml"> <meta name="twitter:card" content="summary" /> <meta name="twitter:site" content="@MDPIOpenAccess" /> <meta name="twitter:image" content="https://pub.mdpi-res.com/img/journals/crystals-logo-social.png?a2c22e8538083c0b" /> <meta property="fb:app_id" content="131189377574"/> <meta property="og:site_name" content="MDPI"/> <meta property="og:type" content="article"/> <meta property="og:url" content="https://www.mdpi.com/2073-4352/14/11/920" /> <meta property="og:title" content="β-Yb2CdSb2—A Complex Non-Centrosymmetric Zintl Polymorph" /> <meta property="og:description" content="The ternary Zintl phase, Yb2CdSb2, was discovered to exist in two different polymorphic forms. In addition to the orthorhombic α-Yb2CdSb2 (space group Cmc21) known for its excellent thermoelectric properties, we present the synthesis and characterization of the crystal and electronic structure of its monoclinic variant, β-Yb2CdSb2. Structural characterization was performed with the single-crystal X-ray diffraction method. β-Yb2CdSb2 crystallizes in a monoclinic crystal system with the non-centrosymmetric space group Cm (Z = 33, a = 81.801(5) Å, b = 4.6186(3) Å, c = 12.6742(7) Å, β = 93.0610(10)°) and constitutes a new structure type. The complex crystal structure of β-Yb2CdSb2 contrasts with the previously studied β-Ca2CdPn2 (Pn = P, As, Sb) polymorphs, although it shares similar structural features. It consists of three different layers, made of corner-sharing [CdSb4] tetrahedra and stacked in the ABC sequence. The layers are interconnected via [CdSb3] trigonal planar units. Multiple Yb and Cd atomic sites exhibit partial occupancy, resulting in extensive structural disorder. Valence electron partitioning within the Zintl–Klemm formalism yields the formulation (Yb2+)1.98(Cd2+)1.01(Sb3−)2(h+)0.02, highlighting the nearly charge-balanced composition. Detailed electronic structure calculations reveal the closed band gap and presumably semimetallic nature of β-Yb2CdSb2 with the band structure features hinting at potential topological properties." /> <meta property="og:image" content="https://pub.mdpi-res.com/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g001-550.jpg?1729846810" /> <link rel="alternate" type="application/rss+xml" title="MDPI Publishing - Latest articles" href="https://www.mdpi.com/rss"> <meta name="google-site-verification" content="PxTlsg7z2S00aHroktQd57fxygEjMiNHydKn3txhvwY"> <meta name="facebook-domain-verification" content="mcoq8dtq6sb2hf7z29j8w515jjoof7" /> <script id="Cookiebot" data-cfasync="false" src="https://consent.cookiebot.com/uc.js" data-cbid="51491ddd-fe7a-4425-ab39-69c78c55829f" type="text/javascript" async></script>  <script type="text/plain" data-cookieconsent="statistics"> (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start': new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0], j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src= 'https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f); 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height: 16px; border-radius: 50%;"><span class="sciprofiles-link__name">Sviatoslav Baranets</span></div></div></div><div class="profile-card__buttons" style="margin-bottom: 10px;"><a href="https://sciprofiles.com/profile/1006490?utm_source=mdpi.com&utm_medium=website&utm_campaign=avatar_name" class="button button--color-inversed" target="_blank"> SciProfiles </a><a href="https://scilit.net/scholars?q=Sviatoslav%20Baranets" class="button button--color-inversed" target="_blank"> Scilit </a><a href="https://www.preprints.org/search?search1=Sviatoslav%20Baranets&field1=authors" class="button button--color-inversed" target="_blank"> Preprints.org </a><a href="https://scholar.google.com/scholar?q=Sviatoslav%20Baranets" class="button button--color-inversed" target="_blank" rels="noopener noreferrer"> Google Scholar </a></div></div><sup> 1,2,*</sup><span style="display: inline; margin-left: 5px;"></span><a class="toEncode emailCaptcha visibility-hidden" data-author-id="13313780" href="/cdn-cgi/l/email-protection#81aee2efe5ace2e6e8aeedaee4ece0e8edacf1f3eef5e4e2f5e8eeefa2b1b1b0b0b6b2b0b3b1b0b0b3b0e5b0b7b1b6b1b1b2b2b0e7b1b1b1b7b4e5b0b7b0b6b1b7"><sup><i class="fa fa-envelope-o"></i></sup></a><a href="https://orcid.org/0000-0003-3449-3344" target="_blank" rel="noopener noreferrer"><img src="https://pub.mdpi-res.com/img/design/orcid.png?0465bc3812adeb52?1732286508" title="ORCID" style="position: relative; width: 13px; margin-left: 3px; max-width: 13px !important; height: auto; top: -5px;"></a></span> </div> <div class="nrm"></div> <span style="display:block; height:6px;"></span> <div></div> <div style="margin: 5px 0 15px 0;" class="hypothesis_container"> <div class="art-affiliations"> <div class="affiliation "> <div class="affiliation-item"><sup>1</sup></div> <div class="affiliation-name ">Department of Chemistry, Louisiana State University, Baton Rouge, LA 70803, USA</div> </div> <div class="affiliation "> <div class="affiliation-item"><sup>2</sup></div> <div class="affiliation-name ">Department of Chemistry and Biochemistry, University of Delaware, Newark, DE 19716, USA</div> </div> <div class="affiliation "> <div class="affiliation-item"><sup>3</sup></div> <div class="affiliation-name ">Department of Physics and Computer Science, Xavier University of Louisiana, New Orleans, LA 70125, USA</div> </div> <div class="affiliation"> <div class="affiliation-item"><sup>*</sup></div> <div class="affiliation-name ">Authors to whom correspondence should be addressed. </div> </div> </div> </div> <div class="bib-identity" style="margin-bottom: 10px;"> <em>Crystals</em> <b>2024</b>, <em>14</em>(11), 920; <a href="https://doi.org/10.3390/cryst14110920">https://doi.org/10.3390/cryst14110920</a> </div> <div class="pubhistory" style="font-weight: bold; padding-bottom: 10px;"> <span style="display: inline-block">Submission received: 1 October 2024</span> / <span style="display: inline-block">Revised: 15 October 2024</span> / <span style="display: inline-block">Accepted: 21 October 2024</span> / <span style="display: inline-block">Published: 25 October 2024</span> </div> <div class="belongsTo" style="margin-bottom: 10px;"> (This article belongs to the Special Issue <a href=" /journal/crystals/special_issues/JF6HN92P83 ">Crystalline Materials: Polymorphism</a>)<br/> </div> <div class="highlight-box1"> <div class="download"> <a class="button button--color-inversed button--drop-down" data-dropdown="drop-download-1506415" aria-controls="drop-supplementary-1506415" aria-expanded="false"> Download <i class="material-icons">keyboard_arrow_down</i> </a> <div id="drop-download-1506415" class="f-dropdown label__btn__dropdown label__btn__dropdown--button" data-dropdown-content aria-hidden="true" tabindex="-1"> <a class="UD_ArticlePDF" href="/2073-4352/14/11/920/pdf?version=1729846639" data-name="β-Yb2CdSb2—A Complex Non-Centrosymmetric Zintl Polymorph" data-journal="crystals">Download PDF</a> <br/> <a id="js-pdf-with-cover-access-captcha" href="#" data-target="/2073-4352/14/11/920/pdf-with-cover" class="accessCaptcha">Download PDF with Cover</a> <br/> <a id="js-xml-access-captcha" href="#" data-target="/2073-4352/14/11/920/xml" class="accessCaptcha">Download XML</a> <br/> <a href="/2073-4352/14/11/920/epub" id="epub_link">Download Epub</a> <br/> <a href="javascript:void(0);" data-reveal-id="supplementaryModal">Download Supplementary Material</a> <br/> </div> <div class="js-browse-figures" style="display: inline-block;"> <a href="#" class="button button--color-inversed margin-bottom-10 openpopupgallery UI_BrowseArticleFigures" data-target='article-popup' data-counterslink = "https://www.mdpi.com/2073-4352/14/11/920/browse" >Browse Figures</a> </div> <div id="article-popup" class="popupgallery" style="display: inline; line-height: 200%"> <a href="https://pub.mdpi-res.com/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g001.png?1729846809" title=" <strong>Figure 1</strong><br/> <p>Ternary Yb−Cd−Sb compositional diagram. The newly identified Yb<sub>2</sub>CdSb<sub>2</sub> polymorph is identified as a red star. Known binary and ternary phases are indicated as well. Note that Yb<sub>14</sub>CdSb<sub>11</sub> and Yb<sub>10.5</sub>Cd<sub>0.5</sub>Sb<sub>9</sub> have not yet been reported.</p> "> </a> <a href="https://pub.mdpi-res.com/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g002.png?1729846812" title=" <strong>Figure 2</strong><br/> <p>Crystal structures of β-Yb<sub>2</sub>CdSb<sub>2</sub> (<b>a</b>), β-Ca<sub>2</sub>CdSb<sub>2</sub> (<b>b</b>), β-Ca<sub>2</sub>CdAs<sub>2</sub> (<b>c</b>), and α-Yb<sub>2</sub>CdSb<sub>2</sub> (<b>d</b>) viewed along the <span class="html-italic">b</span>-axis. The unit cell of β-Yb<sub>2</sub>CdSb<sub>2</sub> is doubled along the <span class="html-italic">c</span>-axis for clarity. The Ca and Yb atoms are drawn as dark gray, Cd atoms are green, and <span class="html-italic">Pn</span> = Sb/As atoms are blue-gray. [Cd<span class="html-italic">Pn</span><sub>4</sub>] tetrahedral units are drawn in dark green. The unit cells are outlined. Interatomic Cd–Sb contacts exceeding 3.10 Å are not displayed.</p> "> </a> <a href="https://pub.mdpi-res.com/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g003.png?1729846815" title=" <strong>Figure 3</strong><br/> <p>The representation of the β-Yb<sub>2</sub>CdSb<sub>2</sub> structure with the labeled ABC layers. The unit cell of β-Yb<sub>2</sub>CdSb<sub>2</sub> is doubled along the <span class="html-italic">c</span>-axis. Cd atoms with less than 50% occupancy are avoided for clarity (<b>a</b>). Close-up view of the A layer in β-Yb<sub>2</sub>CdSb<sub>2</sub> (<b>b</b>), <sub>∞</sub><sup>2</sup>[CdSb<sub>2</sub>]<sup>4–</sup> layer in β-Ca<sub>2</sub>CdSb<sub>2</sub> (<b>c</b>), and [Cd<sub>3</sub>Sb<sub>10</sub>] units composing B/C layers (<b>d</b>). Typical six-coordinated octahedral coordination environment of [YbSb<sub>6</sub>] units (<b>e</b>) and five-coordinated square pyramidal [YbSb<sub>5</sub>] units (<b>f</b>). Completeness of the spheres visualizes SOFs. Similar structural units in β-Yb<sub>2</sub>CdSb<sub>2</sub> and β-Ca<sub>2</sub>CdSb<sub>2</sub> are highlighted by red tetrahedra. The color code is the same as in <a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>.</p> "> </a> <a href="https://pub.mdpi-res.com/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g004.png?1729846819" title=" <strong>Figure 4</strong><br/> <p>Calculated (<b>a</b>) band structure, (<b>b</b>) total (DOS) density of states, and partial (PDOS) density of states for (<b>d</b>) Yb, (<b>e</b>) Cd, and (<b>f</b>) Sb for Yb<sub>2</sub>CdSb<sub>2</sub>. An enlarged view of the band structure at the Fermi level is provided in (<b>c</b>). The Fermi level is the energy reference at 0 eV. The second dashed line at 0.08 eV indicates a 2-electron shift per unit cell.</p> "> </a> </div> <a class="button button--color-inversed" href="/2073-4352/14/11/920/notes">Versions Notes</a> </div> </div> <div class="responsive-moving-container small hidden" data-id="article-counters" style="margin-top: 15px;"></div> <div class="html-dynamic"> <section> <div class="art-abstract art-abstract-new in-tab hypothesis_container"> <p> <div><section class="html-abstract" id="html-abstract"> <h2 id="html-abstract-title">Abstract</h2><b>:</b> <div class="html-p">The ternary Zintl phase, Yb<sub>2</sub>CdSb<sub>2</sub>, was discovered to exist in two different polymorphic forms. In addition to the orthorhombic α-Yb<sub>2</sub>CdSb<sub>2</sub> (space group <span class="html-italic">Cmc</span>2<sub>1</sub>) known for its excellent thermoelectric properties, we present the synthesis and characterization of the crystal and electronic structure of its monoclinic variant, β-Yb<sub>2</sub>CdSb<sub>2</sub>. Structural characterization was performed with the single-crystal X-ray diffraction method. β-Yb<sub>2</sub>CdSb<sub>2</sub> crystallizes in a monoclinic crystal system with the non-centrosymmetric space group <span class="html-italic">Cm</span> (<span class="html-italic">Z</span> = 33, <span class="html-italic">a</span> = 81.801(5) Å, <span class="html-italic">b</span> = 4.6186(3) Å, <span class="html-italic">c</span> = 12.6742(7) Å, <span class="html-italic">β</span> = 93.0610(10)°) and constitutes a new structure type. The complex crystal structure of β-Yb<sub>2</sub>CdSb<sub>2</sub> contrasts with the previously studied β-Ca<sub>2</sub>Cd<span class="html-italic">Pn</span><sub>2</sub> (<span class="html-italic">Pn</span> = P, As, Sb) polymorphs, although it shares similar structural features. It consists of three different layers, made of corner-sharing [CdSb<sub>4</sub>] tetrahedra and stacked in the ABC sequence. The layers are interconnected via [CdSb<sub>3</sub>] trigonal planar units. Multiple Yb and Cd atomic sites exhibit partial occupancy, resulting in extensive structural disorder. Valence electron partitioning within the Zintl–Klemm formalism yields the formulation (Yb<sup>2+</sup>)<sub>1.98</sub>(Cd<sup>2+</sup>)<sub>1.01</sub>(Sb<sup>3−</sup>)<sub>2</sub>(<span class="html-italic">h</span><sup>+</sup>)<sub>0.02</sub>, highlighting the nearly charge-balanced composition. Detailed electronic structure calculations reveal the closed band gap and presumably semimetallic nature of β-Yb<sub>2</sub>CdSb<sub>2</sub> with the band structure features hinting at potential topological properties.</div> </section> <div id="html-keywords"> <div class="html-gwd-group"><div id="html-keywords-title">Keywords: </div><a href="/search?q=Zintl+phases">Zintl phases</a>; <a href="/search?q=single-crystal+X-ray+diffraction">single-crystal X-ray diffraction</a>; <a href="/search?q=charge+balance">charge balance</a>; <a href="/search?q=structural+disorder">structural disorder</a>; <a href="/search?q=topological+insulators">topological insulators</a></div> <div> </div> </div> </div> </p> </div> </section> </div> <div class="hypothesis_container"> <ul class="menu html-nav" data-prev-node="#html-quick-links-title"> </ul> <div class="html-body"> <section id='sec1-crystals-14-00920' type='intro'><h2 data-nested='1'> 1. Introduction</h2><div class='html-p'>The structural complexity within the family of polar intermetallic and Zintl phases is viewed as a frequently observed phenomenon that influences their physical properties and potential applications [<a href="#B1-crystals-14-00920" class="html-bibr">1</a>,<a href="#B2-crystals-14-00920" class="html-bibr">2</a>]. Complex compounds with large unit cells containing hundreds of atoms are often characterized by extensive disorder that originates from compositional and structural inhomogeneities. Materials with such complex structural arrangements often possess low glass-like thermal conductivity, offering a promising platform for the design of novel advanced functional materials, such as thermoelectrics [<a href="#B3-crystals-14-00920" class="html-bibr">3</a>,<a href="#B4-crystals-14-00920" class="html-bibr">4</a>,<a href="#B5-crystals-14-00920" class="html-bibr">5</a>,<a href="#B6-crystals-14-00920" class="html-bibr">6</a>]. In addition, superstructures with extended periodicity or ordering can induce localization of electronic states and alter band structure. With this in mind, enhancing complexity and promoting the formation of superstructures or complex polymorphs may be viewed as an efficient way to fine-tune the transport properties of the materials.</div><div class='html-p'>Zintl compounds are known for their complex bonding interactions, involving electron transfer from electropositive elements from groups 1 and 2 or lanthanides to more electronegative elements from groups 13–15, which, in turn, can result in complex covalently bonded anionic substructures [<a href="#B2-crystals-14-00920" class="html-bibr">2</a>,<a href="#B7-crystals-14-00920" class="html-bibr">7</a>]. Pronounced compositional and structural abundance within Zintl phases is often responsible for the formation of complex structures. Complex Zintl phases usually display a range of unprecedented physical properties, although the inherent complexity poses challenges in understanding structure–property relationships [<a href="#B8-crystals-14-00920" class="html-bibr">8</a>,<a href="#B9-crystals-14-00920" class="html-bibr">9</a>,<a href="#B10-crystals-14-00920" class="html-bibr">10</a>,<a href="#B11-crystals-14-00920" class="html-bibr">11</a>,<a href="#B12-crystals-14-00920" class="html-bibr">12</a>,<a href="#B13-crystals-14-00920" class="html-bibr">13</a>,<a href="#B14-crystals-14-00920" class="html-bibr">14</a>,<a href="#B15-crystals-14-00920" class="html-bibr">15</a>,<a href="#B16-crystals-14-00920" class="html-bibr">16</a>].</div><div class='html-p'>In recent years, we pushed the frontiers of complexity within the family of Zintl phases containing pnictogens, i.e., elements from group 15, by synthesizing and structurally characterizing complex and often disordered Zintl compounds with several hundreds of atoms in the unit cell, such as Ba<sub>2</sub>Mn<sub>1−x</sub>Bi<sub>2</sub> [<a href="#B17-crystals-14-00920" class="html-bibr">17</a>], Eu<sub>8</sub>Zn<sub>2</sub>As<sub>6</sub>O [<a href="#B18-crystals-14-00920" class="html-bibr">18</a>], Ba<sub>16</sub>Sb<sub>11</sub> [<a href="#B19-crystals-14-00920" class="html-bibr">19</a>], Ca<sub>9</sub>(Zn,In)<sub>4</sub>Sb<sub>9</sub> [<a href="#B20-crystals-14-00920" class="html-bibr">20</a>], and Ca<sub>2</sub>CdSb<sub>2</sub> [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>], to name a few. The three latter compositions are particularly interesting, as they exemplify the existence of relatively rare Zintl polymorphs with enhanced structural complexity and substantially large unit cells.</div><div class='html-p'>Inspired by our recent discovery of polymorphism of the Ca<sub>2</sub>CdSb<sub>2</sub> composition, which adopts a simpler orthorhombic modification (<span class='html-italic'>V</span> ≈ 585 Å<sup>3</sup>) [<a href="#B22-crystals-14-00920" class="html-bibr">22</a>] and a more complex monoclinic modification (<span class='html-italic'>V</span> ≈ 4398 Å<sup>3</sup>) [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>], we investigated the amenability of compositionally and structurally related Yb<sub>2</sub>CdSb<sub>2</sub> Zintl antimonide to host polymorphic modifications as well. The orthorhombic α-Yb<sub>2</sub>CdSb<sub>2</sub> (space group <span class='html-italic'>Cmc</span>2<sub>1</sub>, ICSD 173171) phase was discovered in 2007 [<a href="#B22-crystals-14-00920" class="html-bibr">22</a>], and since then, materials crystallizing in its archetype have received noticeable attention due to their promising thermoelectric performance [<a href="#B23-crystals-14-00920" class="html-bibr">23</a>,<a href="#B24-crystals-14-00920" class="html-bibr">24</a>,<a href="#B25-crystals-14-00920" class="html-bibr">25</a>,<a href="#B26-crystals-14-00920" class="html-bibr">26</a>], optical properties [<a href="#B27-crystals-14-00920" class="html-bibr">27</a>,<a href="#B28-crystals-14-00920" class="html-bibr">28</a>,<a href="#B29-crystals-14-00920" class="html-bibr">29</a>], and interesting aspects of structural science [<a href="#B30-crystals-14-00920" class="html-bibr">30</a>,<a href="#B31-crystals-14-00920" class="html-bibr">31</a>,<a href="#B32-crystals-14-00920" class="html-bibr">32</a>,<a href="#B33-crystals-14-00920" class="html-bibr">33</a>]. Although several reports indicate the existence of polymorphs for the structurally related Ca<sub>2</sub>Cd<span class='html-italic'>Pn</span><sub>2</sub> (<span class='html-italic'>Pn</span> = P, As, Sb) phases [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>,<a href="#B27-crystals-14-00920" class="html-bibr">27</a>,<a href="#B32-crystals-14-00920" class="html-bibr">32</a>], the polymorphism within the Yb-bearing Yb<sub>2</sub>Cd<span class='html-italic'>Pn</span><sub>2</sub> family has not been reported to date.</div><div class='html-p'>In this manuscript, we report the discovery of a polymorph of the Yb<sub>2</sub>CdSb<sub>2</sub> phase and provide a comprehensive characterization of its complex crystal and electronic structure, highlighting bonding aspects and the role of structural disorder in charge balance and its semiconducting nature. The reported modification crystallizes in the monoclinic space group <span class='html-italic'>Cm</span>; therefore, we will notate it m-Yb<sub>2</sub>CdSb<sub>2</sub> or β-Yb<sub>2</sub>CdSb<sub>2</sub> hereafter to distinguish it from the original orthorhombic o-Yb<sub>2</sub>CdSb<sub>2</sub>, which will be notated as α-Yb<sub>2</sub>CdSb<sub>2</sub> throughout this manuscript.</div></section><section id='sec2-crystals-14-00920' type=''><h2 data-nested='1'> 2. Materials and Methods</h2><section id='sec2dot1-crystals-14-00920' type=''><h4 class='html-italic' data-nested='2'> 2.1. Synthesis</h4><div class='html-p'>The monoclinic Yb<sub>2</sub>CdSb<sub>2</sub> phase reported here was synthesized by the direct solid-state method, i.e., from melt. The reaction procedures involve loading stoichiometric amounts of the elements (Sigma-Aldrich or Alfa-Aesar with typical purity of ≥99.9 wt.%.) into a Nb tube. Handling of the starting materials was carried out in an Ar-filled glovebox. The tube was then properly shut and arc-welded using Ar plasma. The sealed Nb tube was further flame-sealed in the silica ampoule under vacuum. The ampoule was loaded into a programmable tube furnace which was heated to 1173 K at the rate of 100 K h<sup>−1</sup> and maintained at this temperature for 72 h before cooling to 873 K followed by immediate quenching in cold water. The silica ampoule was crack-opened, and the Nb tube with reacted material was returned to the glovebox. The product was a mixture of several binary phases, including the stable Yb<sub>11</sub>Sb<sub>10</sub> composition [<a href="#B34-crystals-14-00920" class="html-bibr">34</a>]. Also found were the ternary o-Yb<sub>2</sub>CdSb<sub>2</sub> phase previously reported [<a href="#B22-crystals-14-00920" class="html-bibr">22</a>], along with the monoclinic polymorph reported herein.</div><div class='html-p'><span class='html-italic'>Safety Note. Extreme caution should be taken when executing high-temperature reactions with Cd metal. Experiments must be handled with extreme care in well-ventilated areas. The high vapor pressure of Cd at reaction temperatures exceeding its boiling point can cause sealed containers to rupture, creating potentially hazardous conditions. Slow heating is recommended to minimize these risks.</span></div></section><section id='sec2dot2-crystals-14-00920' type=''><h4 class='html-italic' data-nested='2'> 2.2. Structural Characterization</h4><div class='html-p'>Single-crystal X-ray diffraction (SCXRD) data for m-Yb<sub>2</sub>CdSb<sub>2</sub> were collected at 200 K using a Bruker APEX II diffractometer equipped with Mo Kα radiation (<span class='html-italic'>λ</span> = 0.71073 Å) and a CCD detector. An inert atmosphere and low temperature were maintained by continuously flowing a nitrogen stream over the MiTeGen plastic loop holding the mounted crystal. The unit cell refinements, data reduction, and integration were completed with the SAINT program, whereas the SADABS program package was used for absorption corrections [<a href="#B35-crystals-14-00920" class="html-bibr">35</a>,<a href="#B36-crystals-14-00920" class="html-bibr">36</a>]. The structure was solved by the Intrinsic Phasing method using the SHELXT (version 2018/2) program and consequently refined with full-matrix least-squares methods on <span class='html-italic'>F</span><sup>2</sup> using SHELXL (version 2018/3) utilizing Olex2 software (version 1.5) as the GUI [<a href="#B37-crystals-14-00920" class="html-bibr">37</a>,<a href="#B38-crystals-14-00920" class="html-bibr">38</a>,<a href="#B39-crystals-14-00920" class="html-bibr">39</a>,<a href="#B40-crystals-14-00920" class="html-bibr">40</a>]. The STRUCTURE TIDY program was used to standardize coordinates [<a href="#B41-crystals-14-00920" class="html-bibr">41</a>]. Selected crystallographic data, atomic coordinates, displacement parameters, site occupancy factors (SOFs), and selected bond distances are presented in <a href="#crystals-14-00920-t001" class="html-table">Table 1</a>, <a href="#app1-crystals-14-00920" class="html-app">Tables S1 and S2</a>, respectively.</div></section><section id='sec2dot3-crystals-14-00920' type=''><h4 class='html-italic' data-nested='2'> 2.3. Electronic Structure Calculations</h4><div class='html-p'>To better understand the properties and the potential of Yb<sub>2</sub>CdSb<sub>2</sub> for applications, structural optimization and electronic structure calculations were performed with density functional theory (DFT) using Vienna Ab Initio Simulation Package (VASP) software (version 6.4.3.) [<a href="#B42-crystals-14-00920" class="html-bibr">42</a>]. The generalized gradient approximation (GGA) of PBEsol [<a href="#B43-crystals-14-00920" class="html-bibr">43</a>] was used for the exchange correlation functional, with both core and valence electrons treated using the projector-augmented wave (PAW) method [<a href="#B44-crystals-14-00920" class="html-bibr">44</a>]. <span class='html-italic'>k</span>-point mesh and <span class='html-italic'>k</span>-path for band structure were automatically generated using VASPKIT [<a href="#B45-crystals-14-00920" class="html-bibr">45</a>], with a Monkhorst-Pack mesh of 1 × 7 × 3 points in the Brillouin zone for self-consistency field calculations. The Fermi level was selected to be used as an energy reference (<span class='html-italic'>E</span><sub>F</sub> = 0 eV).</div></section></section><section id='sec3-crystals-14-00920' type='results'><h2 data-nested='1'> 3. Results and Discussions</h2><section id='sec3dot1-crystals-14-00920' type=''><h4 class='html-italic' data-nested='2'> 3.1. Synthesis</h4><div class='html-p'>In this section, we discuss additional details on aspects of the sample synthesis procedures presented in the experimental section. After the initial discovery of the m-Yb<sub>2</sub>CdSb<sub>2</sub> polymorphic phase through a direct solid-state reaction, we explored several approaches to access the phase via a high-temperature flux technique. From previous synthesis experiences, where a polymorphic Ca<sub>2</sub>CdSb<sub>2</sub> phase was identified from a Cd-flux method [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>], we attempted to synthesize the title m-Yb<sub>2</sub>CdSb<sub>2</sub> polymorph similarly by loading starting elements Yb:Cd:Sb at a 9:60:9.2 ratio and treating the mixture with the thermal treatment described in our previous report [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>]. However, the observed products were predominantly needle-shaped crystals of the previously reported o-Yb<sub>2</sub>CdSb<sub>2</sub> phase. Only a few of the checked crystals were indexed with lattice parameters that are shown in <a href="#crystals-14-00920-t001" class="html-table">Table 1</a>, i.e., m-Yb<sub>2</sub>CdSb<sub>2</sub>, although the quality was usually poor. Understandably, the powder patterns of both phases are very complex and hardly distinguishable, making it difficult to exhaustively confirm the presence of the monoclinic phase; however, weak superstructure peaks can presumably be identified from the high-resolution synchrotron data. Attempts to produce the title phase via Pb- or Sn-flux reactions also failed, yielding mainly the Yb<sub>11</sub>Sb<sub>10</sub> phase [<a href="#B34-crystals-14-00920" class="html-bibr">34</a>].</div><div class='html-p'>Whereas the solid-state direct reaction synthetic route appears to be the best means of preparing the m-Yb<sub>2</sub>CdSb<sub>2</sub> phase, this approach has its own challenges, specifically, the predominant occurrence of the o-Yb<sub>2</sub>CdSb<sub>2</sub> phase. Also, the crystals obtained from this method are mostly of micron sizes that are mainly suitable for SCXRD data collection but not for transport and magnetic property measurements. It is therefore noted that further optimization of kinetic parameters of the synthesis is expected to grow larger crystals, and perhaps a better understanding of the homogeneity temperature range of this phase may be unraveled via the time-dependent in situ approach [<a href="#B46-crystals-14-00920" class="html-bibr">46</a>], which can provide useful information on the reaction pathways.</div><div class='html-p'>The compositional space within the Yb–Cd–Sb ternary system is not well populated, with only two reported compositions, o-Yb<sub>2</sub>CdSb<sub>2</sub> [<a href="#B22-crystals-14-00920" class="html-bibr">22</a>] and YbCd<sub>2</sub>Sb<sub>2</sub> [<a href="#B47-crystals-14-00920" class="html-bibr">47</a>,<a href="#B48-crystals-14-00920" class="html-bibr">48</a>], being known for a long time. Recently, we identified two (yet to be reported) other ternary compounds, Yb<sub>14</sub>CdSb<sub>11</sub> and Yb<sub>10</sub>CdSb<sub>9</sub> (note the real structure of the latter is heavily disordered and its composition is non-stoichiometric), significantly advancing the compositional landscape of this ternary system (<a href="#crystals-14-00920-f001" class="html-fig">Figure 1</a>).</div></section><section id='sec3dot2-crystals-14-00920' type=''><h4 class='html-italic' data-nested='2'> 3.2. Crystal Structure and Structural Relationships</h4><div class='html-p'>Ternary Zintl pnictides with <span class='html-italic'>A</span><sub>2</sub><span class='html-italic'>MPn</span><sub>2</sub> composition (<span class='html-italic'>A</span> = Ca, Sr, Ba, Eu, Yb; <span class='html-italic'>M</span> = Mn, Zn, Cd; <span class='html-italic'>Pn</span> = P, As, Sb, Bi) represent a promising but still relatively underexplored class of functional materials with the potential for advancing various technologies [<a href="#B49-crystals-14-00920" class="html-bibr">49</a>,<a href="#B50-crystals-14-00920" class="html-bibr">50</a>,<a href="#B51-crystals-14-00920" class="html-bibr">51</a>]. This family of compounds offers a rich chemical diversity and complexity with more than a dozen structure types [<a href="#B17-crystals-14-00920" class="html-bibr">17</a>,<a href="#B21-crystals-14-00920" class="html-bibr">21</a>,<a href="#B22-crystals-14-00920" class="html-bibr">22</a>,<a href="#B27-crystals-14-00920" class="html-bibr">27</a>,<a href="#B32-crystals-14-00920" class="html-bibr">32</a>,<a href="#B52-crystals-14-00920" class="html-bibr">52</a>,<a href="#B53-crystals-14-00920" class="html-bibr">53</a>,<a href="#B54-crystals-14-00920" class="html-bibr">54</a>], including superstructure polymorphs of Ca<sub>2</sub>CdP<sub>2</sub> [<a href="#B27-crystals-14-00920" class="html-bibr">27</a>], Ca<sub>2</sub>CdAs<sub>2</sub> [<a href="#B32-crystals-14-00920" class="html-bibr">32</a>], and Ca<sub>2</sub>CdSb<sub>2</sub> [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>] phases. These β-Ca<sub>2</sub>CdP<sub>2</sub> and β-Ca<sub>2</sub>CdAs<sub>2</sub> polymorphs are isostructural and crystallize in the monoclinic space group <span class='html-italic'>Cm</span> with unit cell parameters <span class='html-italic'>a</span> ≈ 21.0/21.5 Å, <span class='html-italic'>b</span> ≈ 4.2/4.3 Å, <span class='html-italic'>c</span> ≈ 14.0/14.4 Å, and <span class='html-italic'>β</span> ≈ 109.1/110.0°, respectively. The monoclinic structure of the β-Ca<sub>2</sub>CdSb<sub>2</sub> is more complex (<span class='html-italic'>a</span> ≈ 37.3 Å, <span class='html-italic'>b</span> ≈ 4.6 Å, <span class='html-italic'>c</span> ≈ 25.7 Å, and <span class='html-italic'>β</span> ≈ 96.0°) and heavily disordered with multiple partially occupied Cd atoms.</div><div class='html-p'>As reported in this work, the title m-Yb<sub>2</sub>CdSb<sub>2</sub> (β-Yb<sub>2</sub>CdSb<sub>2</sub>) phase also crystallizes in the non-centrosymmetric monoclinic space group <span class='html-italic'>Cm</span> (No. 8) akin to all three listed Ca-bearing polymorphs. Still, its structure is notably different, being the largest (<span class='html-italic'>a</span> ≈ 81.8 Å, <span class='html-italic'>b</span> ≈ 4.6 Å, <span class='html-italic'>c</span> ≈ 12.7 Å, <span class='html-italic'>β</span> ≈ 93.0°) and the most complex with the enormous <span class='html-italic'>a</span> lattice parameter (<a href="#crystals-14-00920-t001" class="html-table">Table 1</a>). Its asymmetric unit contains 33 crystallographically independent Yb atomic sites, 23 Cd sites, and 33 Sb sites, all occupying special positions (Wyckoff 2<span class='html-italic'>a</span>) with the site symmetry <span class='html-italic'>m</span> (<a href="#app1-crystals-14-00920" class="html-app">Table S1</a>). Similarly to the structure of β-Ca<sub>2</sub>CdSb<sub>2</sub>, multiple Cd atoms in β-Yb<sub>2</sub>CdSb<sub>2</sub> are disordered with the site occupancy factors (SOFs) varying from 10% to 60% (<a href="#app1-crystals-14-00920" class="html-app">Table S1</a>). The disorder in β-Yb<sub>2</sub>CdSb<sub>2</sub> is further exacerbated by the partial occupancy of two Yb atomic sites and the split of one Cd atomic position (<a href="#app1-crystals-14-00920" class="html-app">Table S1</a>). The latter type of disorder, however, was previously observed for the Lu-doped version of the β-Ca<sub>2</sub>CdSb<sub>2</sub> phase and was considered an efficient mechanism to increase the dimensionality of the polyanionic substructure and, therefore, enhance transport properties [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>].</div><div class='html-p'>The crystal structure of β-Yb<sub>2</sub>CdSb<sub>2</sub> has no precedent and should be considered a novel structure type. Given the extensive disorder, assigning a proper Wyckoff sequence is complicated, although we tend to formally consider it as <span class='html-italic'>a</span><sup>88</sup> by neglecting the split on the Cd site. Formally, the Pearson symbol can be assigned as <span class='html-italic'>mS</span>176, yet given the vacant Cd and Yb sites, it could also be viewed as <span class='html-italic'>mS</span>165.</div><div class='html-p'>The disordered anionic substructure of β-Yb<sub>2</sub>CdSb<sub>2</sub> shown in <a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>a is much more complex than that of ordered α-Yb<sub>2</sub>CdSb<sub>2</sub> (<a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>d) and β-Ca<sub>2</sub>Cd<span class='html-italic'>Pn</span><sub>2</sub> (<span class='html-italic'>Pn</span> = P, As) (<a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>c), but comparable to the β-Ca<sub>2</sub>CdSb<sub>2</sub> (<a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>b) and its Lu-doped variant [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>]. All listed structure types lack inversion symmetry and crystallize in the non-centrosymmetric space group <span class='html-italic'>Cmc</span>2<sub>1</sub> for α-Yb<sub>2</sub>CdSb<sub>2</sub> or <span class='html-italic'>Cm</span> for the rest of the compounds, which allows the identification of structural relationships across the series. α-Yb<sub>2</sub>CdSb<sub>2</sub> and β-Ca<sub>2</sub>CdSb<sub>2</sub> contain layers composed of the corner-sharing [CdSb<sub>4</sub>] tetrahedra, which are stacked in the AAAA sequence, although with the 1/2-translation displacement along the shortest <span class='html-italic'>a</span>- or <span class='html-italic'>b</span>-axis, respectively. However, careful analysis of the β-Yb<sub>2</sub>CdSb<sub>2</sub> structure reveals the presence of several different layers so that the stacking sequence can be denoted as ABC (<a href="#crystals-14-00920-f003" class="html-fig">Figure 3</a>a). Similarly to the β-Ca<sub>2</sub>CdSb<sub>2</sub>, adjacent slabs of [ABC] layers are displaced by a translation halfway along the shortest <span class='html-italic'>b</span>-axis, which corresponds to the viewing direction in <a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>a and <a href="#crystals-14-00920-f003" class="html-fig">Figure 3</a>a.</div><div class='html-p'>To better understand the compositional and structural configurations of each layer, we should consider the structural model with the partially reduced disorder. The crystal structure of the title β-Yb<sub>2</sub>CdSb<sub>2</sub> phase contains eight partially occupied or split Cd atomic sites. All of them, but Cd22 with the SOF of ca. 58%, are coordinated by three Sb atoms in a trigonal planar arrangement, with the Cd atoms noticeably protruding from the plane. However, the coordination of these Cd sites cannot be extended to the tetrahedra through the fourth Cd−Sb contacts, as these distances exceed 3.12 Å, which is noticeably larger than the combined values of the covalent radii of Cd and Sb (2.83 Å) [<a href="#B55-crystals-14-00920" class="html-bibr">55</a>]. A reasonable structural model with well-separated layers (<a href="#crystals-14-00920-f003" class="html-fig">Figure 3</a>a) can be obtained if we omit the Cd1, Cd2, Cd3, Cd4B, Cd5, Cd7, Cd8, and Cd9 atomic positions, i.e., those with SOFs ≤ 50% (<a href="#app1-crystals-14-00920" class="html-app">Table S1</a>).</div><div class='html-p'>Layer A, depicted in <a href="#crystals-14-00920-f003" class="html-fig">Figure 3</a>b, can be described as consisting of seven unique Cd-centered (Cd10−Cd12, Cd19−Cd22) [CdSb<sub>4</sub>] tetrahedra, which are corner-shared. Note that all Cd sites except Cd22 are fully occupied. Layer A features partially similar structural arrangements observed in α-Yb<sub>2</sub>CdSb<sub>2</sub> (<a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>d) and β-Ca<sub>2</sub>CdSb<sub>2</sub> (<a href="#crystals-14-00920-f003" class="html-fig">Figure 3</a>c), although they are not entirely identical. These complex infinite layers are located within the <span class='html-italic'>bc</span>-plane.</div><div class='html-p'>Layers B and C can be viewed as 1D [Cd<sub>3</sub>Sb<sub>10</sub>] units composed of three [CdSb<sub>4</sub>] tetrahedra interconnected via the same Sb atom. These three-fold units propagate along the <span class='html-italic'>b</span>-axis by sharing corners of all three [CdSb<sub>4</sub>] tetrahedra (<a href="#crystals-14-00920-f003" class="html-fig">Figure 3</a>d). We have recently reported similar structural fragments in β-Ca<sub>2</sub>CdAs<sub>2</sub> (<a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>c) [<a href="#B32-crystals-14-00920" class="html-bibr">32</a>], Ca<sub>8</sub>LaMn<sub>4+<span class='html-italic'>x</span></sub>Sb<sub>9</sub> [<a href="#B56-crystals-14-00920" class="html-bibr">56</a>], and Ca<sub>9</sub>(Zn,In)<sub>4</sub>Sb<sub>9</sub> [<a href="#B20-crystals-14-00920" class="html-bibr">20</a>]. Although the [Cd<sub>3</sub>Sb<sub>10</sub>] units composing B and C slabs are nearly identical in the structure of β-Yb<sub>2</sub>CdSb<sub>2</sub> (<a href="#crystals-14-00920-f003" class="html-fig">Figure 3</a>a), they consist of different sets of atoms: Cd16−Cd18-centered tetrahedra for B and Cd13−Cd15-centered tetrahedra for C. These units are slightly displaced along the <span class='html-italic'>c</span>-axis and tilted differently for B and C with respect to the <span class='html-italic'>b</span>-axis. Interatomic Cd−Sb contacts within all three described layers (<a href="#app1-crystals-14-00920" class="html-app">Table S2</a>) range from 2.75 Å to 3.09 Å and are consistent with the previously observed values for α-Yb<sub>2</sub>CdSb<sub>2</sub>, β-Ca<sub>2</sub>CdSb<sub>2,</sub> and similar materials [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>,<a href="#B22-crystals-14-00920" class="html-bibr">22</a>].</div><div class='html-p'>Trigonal planar [CdSb<sub>3</sub>] units composed of the partially occupied Cd atoms form 1D corner-sharing ribbons along the <span class='html-italic'>b</span>-axis. Some of the interatomic contacts within these units are somewhat shortened, falling below the sum of covalent radii of Sb and Cd (2.83 Å, <a href="#app1-crystals-14-00920" class="html-app">Table S2</a>), which can be attributed to the partial SOFs of the Cd atoms. With some flexibility for allowed interatomic Cd–Sb contacts, we can consider these ribbons as linking fragments for the described layers, as can be seen in <a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>a. Such structural features can contribute to the increased dimensionality of the anionic substructure and improve charge-carrier transport properties, as was recently shown for the β-Ca<sub>2</sub>CdSb<sub>2</sub> and its Lu-doped variant [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>].</div><div class='html-p'>The coordination environments of the Yb<sup>2+</sup> cations in the β-Yb<sub>2</sub>CdSb<sub>2</sub> structure are very similar to those observed in α-Yb<sub>2</sub>CdSb<sub>2</sub> and β-Ca<sub>2</sub>CdSb<sub>2</sub>. Among all 33 Yb atomic sites, 16 are coordinated in a slightly distorted octahedral fashion with CN = 6 (<a href="#crystals-14-00920-f003" class="html-fig">Figure 3</a>e), and 17 are in a distorted square pyramidal fashion with CN = 5 (<a href="#crystals-14-00920-f003" class="html-fig">Figure 3</a>f). The observed interatomic Yb−Sb distances range from 3.08 to 3.58 Å, although considering longer contacts up to 3.79 Å, some of the [YbSb<sub>5</sub>] square pyramids can be transformed into the heavily distorted [YbSb<sub>6</sub>] octahedra.</div><div class='html-p'>Two Yb sites, Yb17 with square-pyramidal coordination and Yb22 with octahedral coordination, were refined as partially occupied with SOFs of ca. 80% and 86%, respectively. The Fourier difference map indicates negligible residual electron density peaks close to multiple Yb atoms, which were considered artifacts of the absorption correction. The presence of the multiple underoccupied Yb and Cd atomic sites in the structure of β-Yb<sub>2</sub>CdSb<sub>2</sub> (<a href="#app1-crystals-14-00920" class="html-app">Table S1</a>) is explained by the charge balance and electron count considerations. Indeed, since all atomic sites have the same site symmetry (Wyckoff 2<span class='html-italic'>a</span>), and given <span class='html-italic'>Z</span> = 33, it is required to have 33 Yb sites, 33 Sb sites, and 16.5 Cd sites to maintain the charge-balanced Yb<sub>2</sub>CdSb<sub>2</sub> composition. Instead, the crystal structure of the title compound features 22 Cd sites, 8 of which are partially occupied (<a href="#app1-crystals-14-00920" class="html-app">Table S1</a>). A hypothetical structural model in which all atomic sites are fully occupied is improbable as it would have a pronouncedly electron-rich composition (i.e., Yb<sub>66</sub>Cd<sub>44</sub>Sb<sub>66</sub>(<span class='html-italic'>e</span><sup>−</sup>)<sub>22</sub> = Yb<sub>2</sub>Cd<sub>1.33(3)</sub>Sb<sub>2</sub>(<span class='html-italic'>e</span><sup>−</sup>)<sub>0.66</sub>, where <span class='html-italic'>e</span><sup>−</sup> denotes the electrons). The reported refined formula with underoccupied Cd and Yb atoms is nearly charge-balanced and can be described according to the fully ionic approximation as (Yb<sup>2+</sup>)<sub>1.98</sub>(Cd<sup>2+</sup>)<sub>1.01</sub>(Sb<sup>3−</sup>)<sub>2</sub>(<span class='html-italic'>h</span><sup>+</sup>)<sub>0.02</sub>, where <span class='html-italic'>h</span><sup>+</sup> denotes holes.</div></section><section id='sec3dot3-crystals-14-00920' type=''><h4 class='html-italic' data-nested='2'> 3.3. Electronic Structure</h4><div class='html-p'>Given the moderate difference between the electronegativities of the constituted elements in Yb<sub>2</sub>CdSb<sub>2</sub> and the sizable charge transfer, we anticipate observing a semiconducting behavior for the title compound as was previously reported for the Ca<sub>2</sub>Cd<span class='html-italic'>Pn</span><sub>2</sub> (<span class='html-italic'>Pn</span> = P, As, Sb) family of compounds [<a href="#B21-crystals-14-00920" class="html-bibr">21</a>,<a href="#B22-crystals-14-00920" class="html-bibr">22</a>,<a href="#B27-crystals-14-00920" class="html-bibr">27</a>,<a href="#B32-crystals-14-00920" class="html-bibr">32</a>]. However, Yb-bearing compounds are expected to be more metallic in nature and possess smaller band gaps due to the more diffuse and larger orbitals of Yb. This prediction is corroborated by the electronic structure calculations provided below.</div><div class='html-p'>As discussed in the experimental section, a simplified structure of Yb<sub>2</sub>CdSb<sub>2</sub> can be generated by removing partially occupied atomic sites. To compose the structural model suitable for the electronic structure calculations, we further adjusted the structural model provided in <a href="#crystals-14-00920-f003" class="html-fig">Figure 3</a>a. In particular, split Cd4A and Cd4B atomic sites were combined into the singular Cd4 position with an SOF of 1. Some Cd sites with low SOFs, such as Cd3 (SOF 36.9%), Cd5 (SOF 32.3%), Cd7 (SOF 9.7%), Cd8 (SOF 10.4%), and Cd9 (SOF 19.7%), were also removed, while Yb17 (SOF 80.3%), Yb22 (SOF 86.2%), Cd1 (SOF 50%), Cd2 (SOF 50%), and Cd22 (SOF 58.1%) were given full occupancy. This allowed for a nearly charge-balanced composition of Yb<sub>66</sub>Cd<sub>34</sub>Sb<sub>66</sub> = Yb<sub>2</sub>Cd<sub>1.03</sub>Sb<sub>2</sub> with 17 fully occupied Cd sites but resulted in a two-electron shift in the Fermi level according to the (Yb<sup>2+</sup>)<sub>66</sub>(Cd<sup>2+</sup>)<sub>34</sub>(Sb<sup>3–</sup>)<sub>66</sub>(<span class='html-italic'>e</span><sup>−</sup>)<sub>2</sub> charge partitioning, as indicated on the density-of-states plots below (<a href="#crystals-14-00920-f004" class="html-fig">Figure 4</a>).</div><div class='html-p'><a href="#crystals-14-00920-f004" class="html-fig">Figure 4</a>a,c show the calculated band structure and the total (TDOS) and partial (PDOS) density of states within the energy range from −5 to 2 eV. The absence of a band gap opening in the β-Ca<sub>2</sub>CdSb<sub>2</sub> phase indicates a semimetallic behavior. Specifically, an overlap of the conduction and valence bands is observed, which can result in a relatively low carrier concentration and high mobility. Here, the Fermi level lies very close to the point of overlap between the valence and conduction bands as opposed to those of semiconductors, where the Fermi level lies within the band gap. The features observed also likely indicate the anisotropic nature of the electron and hole masses in the title phase, which can play critical roles in its electronic and transport properties. A closer look at <a href="#crystals-14-00920-f004" class="html-fig">Figure 4</a>a,c indicate the presence of what can be considered anti-crossing and band inversion features along the high-symmetry Г-points, which can be a signature of nontrivial topology. Although the observed features require further extensive investigation, it should be noted that the presented band structure in <a href="#crystals-14-00920-f004" class="html-fig">Figure 4</a>c has no spin–orbit coupling (SOC). We speculate that the switching on of SOC and/or the strain effect in this phase can provide other interesting features, such as opening a band gap, which is expected for a topological insulator state. Here, the crossing of the valence and conduction bands brings about discrete touch points in momentum space as one would expect for Dirac and Weyl semimetals, which are characterized by massless fermions and nontrivial Berry curvature. Detailed band structure calculations and parity analysis of occupied bands are expected to provide additional insight into the electronic and transport properties of this material.</div><div class='html-p'>The correlation between the surface state properties of topological insulators and excellent thermoelectric properties in Zintl phases has been established [<a href="#B57-crystals-14-00920" class="html-bibr">57</a>,<a href="#B58-crystals-14-00920" class="html-bibr">58</a>]. If confirmed, the presence of nontrivial band topology in the title compound can also provide a window of opportunity to explore this material for excellent thermoelectric properties. The heavy disorder and intricate atomic bonding in the title phase are particularly expected to drive the realization of ultra-low thermal conductivity. The presence of multiple bands below the Fermi level and the generic view of the band structure appear to be very similar to the previously reported β-Ca<sub>2</sub>CdP<sub>2</sub> and β-Ca<sub>2</sub>CdAs<sub>2</sub> phases [<a href="#B27-crystals-14-00920" class="html-bibr">27</a>,<a href="#B32-crystals-14-00920" class="html-bibr">32</a>], although they are direct-gap semiconductors with relatively wide band gaps.</div><div class='html-p'>The total and partial density of states (DOS) plots (<a href="#crystals-14-00920-f004" class="html-fig">Figure 4</a>) also show patterns similar to other ternary pnictides [<a href="#B22-crystals-14-00920" class="html-bibr">22</a>,<a href="#B54-crystals-14-00920" class="html-bibr">54</a>]. States between −5 and the valence band maxima (VBM) consist primarily of Sb-p states, with minimal contributions from Sb-s and Sb-d, indicating poor orbital mixing. Yb-p and Yb-d states both contribute to the range between −4 eV and the VBM, with Yb–d being the primary contributor. Cd-s orbitals contribute primarily to states below −5 eV, while Cd-p states contribute to the range between −4 eV and the VBM.</div></section></section><section id='sec4-crystals-14-00920' type='conclusions'><h2 data-nested='1'> 4. Conclusions</h2><div class='html-p'>A novel complex monoclinic β-Yb<sub>2</sub>CdSb<sub>2</sub> polymorph has been identified and studied, enriching the Yb–Cd–Sb phase diagram and highlighting the structural diversity of the <span class='html-italic'>A</span><sub>2</sub>Cd<span class='html-italic'>Pn</span><sub>2</sub> (<span class='html-italic'>A</span> = Ca, Yb; <span class='html-italic'>Pn</span> = P, As, Sb) family of non-centrosymmetric compounds. β-Yb<sub>2</sub>CdSb<sub>2</sub> has a disordered anionic substructure based on the distorted [CdSb<sub>4</sub>] tetrahedral and [CdSb<sub>3</sub>] trigonal planar units, being reminiscent of the related β-Ca<sub>2</sub>CdSb<sub>2</sub> phase, although with significant differences in stacking sequences and interlayer interactions. Detailed structural and electronic characterizations highlight the influence of disorder on the charge-balanced nature of the material, which can be notated as the (Yb<sup>2+</sup>)<sub>1.98</sub>(Cd<sup>2+</sup>)<sub>1.01</sub>(Sb<sup>3−</sup>)<sub>2</sub>(<span class='html-italic'>h</span><sup>+</sup>)<sub>0.02</sub>. Its discovery underscores the potential for tailoring thermoelectric and optical properties through polymorphism and structural disorder and helps in understanding the relationships between structural complexity and material properties. Electronic structure calculations reveal a presumably semimetallic feature of β-Yb<sub>2</sub>CdSb<sub>2</sub>. In addition, features reminiscent of nontrivial topological properties are observed, although subsequent studies are expected to provide a clearer picture of this.</div><div class='html-p'>Future investigations could focus on fine-tuning the disorder through doping or substitutions, aiming to optimize thermoelectric performance and explore the tuning of possible topological properties. It should be noted that this compound may occur as an impurity phase in the synthesis of thermoelectric materials based on the orthorhombic α-Yb<sub>2</sub>CdSb<sub>2</sub> polymorph, therefore posing a risk of misidentification and misinterpretation of the structure–property relationships. Subsequent studies will also benefit from optimizing the synthesis condition of this phase towards realizing larger single crystals and polycrystalline bulk synthesis, which will provide an opportunity for an exhaustive investigation of its thermoelectric and transport properties.</div></section> </div> <div class="html-back"> <section><section id='app1-crystals-14-00920' type=''><h2 data-nested='1'> Supplementary Materials</h2><div class='html-p'>The following supporting information can be downloaded at <a href='https://www.mdpi.com/article/10.3390/cryst14110920/s1' target='_blank' rel="noopener noreferrer">https://www.mdpi.com/article/10.3390/cryst14110920/s1</a>: Table S1: Refined atomic coordinates for β-Yb<sub>2</sub>CdSb<sub>2</sub>. Table S2: Selected bond distances for β-Yb<sub>2</sub>CdSb<sub>2</sub>. </div></section></section><section class='html-notes'><h2 >Author Contributions</h2><div class='html-p'>Validation, M.O.O.; formal analysis, S.R.W., M.O.O., and S.B. (Sviatoslav Baranets); data curation, S.R.W. and L.N.; writing—original draft preparation, visualization, S.R.W. and S.B. (Sviatoslav Baranets); writing—review and editing, M.O.O. and S.B. (Svilen Bobev); methodology, conceptualization, supervision, project administration, S.B. (Svilen Bobev) and S.B. (Sviatoslav Baranets), funding acquisition S.B. (Svilen Bobev). All authors have read and agreed to the published version of the manuscript.</div></section><section class='html-notes'><h2>Funding</h2><div class='html-p'>This research was funded by the United States Department of Energy, Office of Science, Basic Energy Sciences, under Award #DE-SC0008885. S. Baranets acknowledges financial support from the College of Science and Department of Chemistry at Louisiana State University (start-up funding).</div></section><section class='html-notes'><h2 >Data Availability Statement</h2><div class='html-p'>The corresponding crystallographic information files (CIFs) have been deposited with the Cambridge Crystallographic Database Centre (CCDC) and can be obtained free of charge via <a href='https://www.ccdc.cam.ac.uk/structures/' target='_blank' rel="noopener noreferrer">https://www.ccdc.cam.ac.uk/structures/</a> or by emailing <a href="/cdn-cgi/l/email-protection#f793968396a885928682928483b794949394d994969ad99694d9829c"><span class="__cf_email__" data-cfemail="d1b5b0a5b08ea3b4a0a4b4a2a591b2b2b5b2ffb2b0bcffb0b2ffa4ba">[email protected]</span></a> with the following depository number: 2387090.</div></section><section id='html-ack' class='html-ack'><h2 >Acknowledgments</h2><div class='html-p'>S. Bobev acknowledges financial support from the United States Department of Energy, Office of Science, Basic Energy Sciences, under Award #DE-SC0008885. S. Baranets acknowledges financial support from the College of Science and Department of Chemistry at Louisiana State University (start-up funding). Julien Makongo is acknowledged for his preliminary work in the Yb–Cd–Sb system.</div></section><section class='html-notes'><h2 >Conflicts of Interest</h2><div class='html-p'>The authors declare no conflicts of interest.</div></section><section id='html-references_list'><h2>References</h2><ol class='html-xx'><li id='B1-crystals-14-00920' class='html-x' data-content='1.'>Ovchinnikov, A.; Smetana, V.; Mudring, A.-V. Metallic alloys at the edge of complexity: Structural aspects, chemical bonding and physical properties. <span class='html-italic'>J. Phys. Condens. Matter</span> <b>2020</b>, <span class='html-italic'>32</span>, 243002. 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The newly identified Yb<sub>2</sub>CdSb<sub>2</sub> polymorph is identified as a red star. Known binary and ternary phases are indicated as well. Note that Yb<sub>14</sub>CdSb<sub>11</sub> and Yb<sub>10.5</sub>Cd<sub>0.5</sub>Sb<sub>9</sub> have not yet been reported.  </div> </div> <div class="html-fig_show mfp-hide" id="fig_body_display_crystals-14-00920-f001"> <div class="html-caption"> <b>Figure 1.</b> Ternary Yb−Cd−Sb compositional diagram. The newly identified Yb<sub>2</sub>CdSb<sub>2</sub> polymorph is identified as a red star. Known binary and ternary phases are indicated as well. Note that Yb<sub>14</sub>CdSb<sub>11</sub> and Yb<sub>10.5</sub>Cd<sub>0.5</sub>Sb<sub>9</sub> have not yet been reported.</div> <div class="html-img"><img data-large="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g001.png" data-original="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g001.png" alt="Crystals 14 00920 g001" data-lsrc="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g001.png" /></div> </div> <div class="html-fig-wrap" id="crystals-14-00920-f002"> <div class='html-fig_img'> <div class="html-figpopup html-figpopup-link" data-counterslinkmanual = "https://www.mdpi.com/2073-4352/14/11/920/display" href="#fig_body_display_crystals-14-00920-f002"> <img data-large="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g002.png" data-original="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g002.png" alt="Crystals 14 00920 g002" data-lsrc="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g002-550.jpg" /> <a class="html-expand html-figpopup" data-counterslinkmanual = "https://www.mdpi.com/2073-4352/14/11/920/display" href="#fig_body_display_crystals-14-00920-f002"></a> </div> </div> <div class="html-fig_description"> <b>Figure 2.</b> Crystal structures of β-Yb<sub>2</sub>CdSb<sub>2</sub> (<b>a</b>), β-Ca<sub>2</sub>CdSb<sub>2</sub> (<b>b</b>), β-Ca<sub>2</sub>CdAs<sub>2</sub> (<b>c</b>), and α-Yb<sub>2</sub>CdSb<sub>2</sub> (<b>d</b>) viewed along the <span class='html-italic'>b</span>-axis. The unit cell of β-Yb<sub>2</sub>CdSb<sub>2</sub> is doubled along the <span class='html-italic'>c</span>-axis for clarity. The Ca and Yb atoms are drawn as dark gray, Cd atoms are green, and <span class='html-italic'>Pn</span> = Sb/As atoms are blue-gray. [Cd<span class='html-italic'>Pn</span><sub>4</sub>] tetrahedral units are drawn in dark green. The unit cells are outlined. Interatomic Cd–Sb contacts exceeding 3.10 Å are not displayed.  </div> </div> <div class="html-fig_show mfp-hide" id="fig_body_display_crystals-14-00920-f002"> <div class="html-caption"> <b>Figure 2.</b> Crystal structures of β-Yb<sub>2</sub>CdSb<sub>2</sub> (<b>a</b>), β-Ca<sub>2</sub>CdSb<sub>2</sub> (<b>b</b>), β-Ca<sub>2</sub>CdAs<sub>2</sub> (<b>c</b>), and α-Yb<sub>2</sub>CdSb<sub>2</sub> (<b>d</b>) viewed along the <span class='html-italic'>b</span>-axis. The unit cell of β-Yb<sub>2</sub>CdSb<sub>2</sub> is doubled along the <span class='html-italic'>c</span>-axis for clarity. The Ca and Yb atoms are drawn as dark gray, Cd atoms are green, and <span class='html-italic'>Pn</span> = Sb/As atoms are blue-gray. [Cd<span class='html-italic'>Pn</span><sub>4</sub>] tetrahedral units are drawn in dark green. The unit cells are outlined. Interatomic Cd–Sb contacts exceeding 3.10 Å are not displayed.</div> <div class="html-img"><img data-large="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g002.png" data-original="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g002.png" alt="Crystals 14 00920 g002" data-lsrc="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g002.png" /></div> </div> <div class="html-fig-wrap" id="crystals-14-00920-f003"> <div class='html-fig_img'> <div class="html-figpopup html-figpopup-link" data-counterslinkmanual = "https://www.mdpi.com/2073-4352/14/11/920/display" href="#fig_body_display_crystals-14-00920-f003"> <img data-large="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g003.png" data-original="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g003.png" alt="Crystals 14 00920 g003" data-lsrc="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g003-550.jpg" /> <a class="html-expand html-figpopup" data-counterslinkmanual = "https://www.mdpi.com/2073-4352/14/11/920/display" href="#fig_body_display_crystals-14-00920-f003"></a> </div> </div> <div class="html-fig_description"> <b>Figure 3.</b> The representation of the β-Yb<sub>2</sub>CdSb<sub>2</sub> structure with the labeled ABC layers. The unit cell of β-Yb<sub>2</sub>CdSb<sub>2</sub> is doubled along the <span class='html-italic'>c</span>-axis. Cd atoms with less than 50% occupancy are avoided for clarity (<b>a</b>). Close-up view of the A layer in β-Yb<sub>2</sub>CdSb<sub>2</sub> (<b>b</b>), <sub>∞</sub><sup>2</sup>[CdSb<sub>2</sub>]<sup>4–</sup> layer in β-Ca<sub>2</sub>CdSb<sub>2</sub> (<b>c</b>), and [Cd<sub>3</sub>Sb<sub>10</sub>] units composing B/C layers (<b>d</b>). Typical six-coordinated octahedral coordination environment of [YbSb<sub>6</sub>] units (<b>e</b>) and five-coordinated square pyramidal [YbSb<sub>5</sub>] units (<b>f</b>). Completeness of the spheres visualizes SOFs. Similar structural units in β-Yb<sub>2</sub>CdSb<sub>2</sub> and β-Ca<sub>2</sub>CdSb<sub>2</sub> are highlighted by red tetrahedra. The color code is the same as in <a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>.  </div> </div> <div class="html-fig_show mfp-hide" id="fig_body_display_crystals-14-00920-f003"> <div class="html-caption"> <b>Figure 3.</b> The representation of the β-Yb<sub>2</sub>CdSb<sub>2</sub> structure with the labeled ABC layers. The unit cell of β-Yb<sub>2</sub>CdSb<sub>2</sub> is doubled along the <span class='html-italic'>c</span>-axis. Cd atoms with less than 50% occupancy are avoided for clarity (<b>a</b>). Close-up view of the A layer in β-Yb<sub>2</sub>CdSb<sub>2</sub> (<b>b</b>), <sub>∞</sub><sup>2</sup>[CdSb<sub>2</sub>]<sup>4–</sup> layer in β-Ca<sub>2</sub>CdSb<sub>2</sub> (<b>c</b>), and [Cd<sub>3</sub>Sb<sub>10</sub>] units composing B/C layers (<b>d</b>). Typical six-coordinated octahedral coordination environment of [YbSb<sub>6</sub>] units (<b>e</b>) and five-coordinated square pyramidal [YbSb<sub>5</sub>] units (<b>f</b>). Completeness of the spheres visualizes SOFs. Similar structural units in β-Yb<sub>2</sub>CdSb<sub>2</sub> and β-Ca<sub>2</sub>CdSb<sub>2</sub> are highlighted by red tetrahedra. The color code is the same as in <a href="#crystals-14-00920-f002" class="html-fig">Figure 2</a>.</div> <div class="html-img"><img data-large="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g003.png" data-original="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g003.png" alt="Crystals 14 00920 g003" data-lsrc="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g003.png" /></div> </div> <div class="html-fig-wrap" id="crystals-14-00920-f004"> <div class='html-fig_img'> <div class="html-figpopup html-figpopup-link" data-counterslinkmanual = "https://www.mdpi.com/2073-4352/14/11/920/display" href="#fig_body_display_crystals-14-00920-f004"> <img data-large="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g004.png" data-original="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g004.png" alt="Crystals 14 00920 g004" data-lsrc="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g004-550.jpg" /> <a class="html-expand html-figpopup" data-counterslinkmanual = "https://www.mdpi.com/2073-4352/14/11/920/display" href="#fig_body_display_crystals-14-00920-f004"></a> </div> </div> <div class="html-fig_description"> <b>Figure 4.</b> Calculated (<b>a</b>) band structure, (<b>b</b>) total (DOS) density of states, and partial (PDOS) density of states for (<b>d</b>) Yb, (<b>e</b>) Cd, and (<b>f</b>) Sb for Yb<sub>2</sub>CdSb<sub>2</sub>. An enlarged view of the band structure at the Fermi level is provided in (<b>c</b>). The Fermi level is the energy reference at 0 eV. The second dashed line at 0.08 eV indicates a 2-electron shift per unit cell.  </div> </div> <div class="html-fig_show mfp-hide" id="fig_body_display_crystals-14-00920-f004"> <div class="html-caption"> <b>Figure 4.</b> Calculated (<b>a</b>) band structure, (<b>b</b>) total (DOS) density of states, and partial (PDOS) density of states for (<b>d</b>) Yb, (<b>e</b>) Cd, and (<b>f</b>) Sb for Yb<sub>2</sub>CdSb<sub>2</sub>. An enlarged view of the band structure at the Fermi level is provided in (<b>c</b>). The Fermi level is the energy reference at 0 eV. The second dashed line at 0.08 eV indicates a 2-electron shift per unit cell.</div> <div class="html-img"><img data-large="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g004.png" data-original="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g004.png" alt="Crystals 14 00920 g004" data-lsrc="/crystals/crystals-14-00920/article_deploy/html/images/crystals-14-00920-g004.png" /></div> </div> <div class="html-table-wrap" id="crystals-14-00920-t001"> <div class="html-table_wrap_td"> <div class="html-tablepopup html-tablepopup-link" data-counterslinkmanual = "https://www.mdpi.com/2073-4352/14/11/920/display" href='#table_body_display_crystals-14-00920-t001'> <img data-lsrc="https://pub.mdpi-res.com/img/table.png" /> <a class="html-expand html-tablepopup" data-counterslinkmanual = "https://www.mdpi.com/2073-4352/14/11/920/display" href="#table_body_display_crystals-14-00920-t001"></a> </div> </div> <div class="html-table_wrap_discription"> <b>Table 1.</b> Selected data collection and crystallographic details and structure refinement parameters for β-Yb<sub>2</sub>Cd<sub>2</sub>Sb<sub>2</sub> (monoclinic space group <span class='html-italic'>Cm</span>; <span class='html-italic'>Z</span> = 33; Mo Kα radiation (<span class='html-italic'>λ</span> = 0.71073 Å); <span class='html-italic'>T</span> = 200(2) K). </div> </div> <div class="html-table_show mfp-hide " id="table_body_display_crystals-14-00920-t001"> <div class="html-caption"><b>Table 1.</b> Selected data collection and crystallographic details and structure refinement parameters for β-Yb<sub>2</sub>Cd<sub>2</sub>Sb<sub>2</sub> (monoclinic space group <span class='html-italic'>Cm</span>; <span class='html-italic'>Z</span> = 33; Mo Kα radiation (<span class='html-italic'>λ</span> = 0.71073 Å); <span class='html-italic'>T</span> = 200(2) K).</div> <table > <tbody ><tr ><td align='center' valign='middle' style='border-top:solid thin;border-bottom:solid thin' class='html-align-center' >Empirical formula </td><td align='center' valign='middle' style='border-top:solid thin;border-bottom:solid thin' class='html-align-center' >Yb<sub>1.98(1)</sub>Cd<sub>1.01(1)</sub>Sb<sub>2</sub> </td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >Formula weight </td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >699.62 </td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' ><span class='html-italic'>a</span>/Å </td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >81.801(5) </td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' ><span class='html-italic'>b</span>/Å </td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >4.6186(3) </td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' ><span class='html-italic'>c</span>/Å </td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >12.6742(7) </td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' ><span class='html-italic'>β</span>/° </td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >93.0610(10) </td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' ><span class='html-italic'>V</span>/Å<sup>3</sup></td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >4781.6(5) </td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' ><span class='html-italic'>ρ<sub>calc</sub></span> g/cm<sup>3</sup> </td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >8.018 </td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' ><span class='html-italic'>μ</span>/mm<sup>−1</sup></td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >44.311 </td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >Collected/independent reflections</td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >29,216/10,902</td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' ><span class='html-italic'>R</span><sub>1</sub> (<span class='html-italic'>I</span> > 2σ<sub>(I)</sub>) <span class='html-italic'><sup>a</sup></span></td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >0.0333</td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >w<span class='html-italic'>R</span><sub>2</sub> (<span class='html-italic'>I</span> > 2σ<sub>(I)</sub>) <span class='html-italic'><sup>a</sup></span></td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >0.0589</td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' ><span class='html-italic'>R</span><sub>1</sub> (all data) <span class='html-italic'><sup>a</sup></span></td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >0.0395</td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >w<span class='html-italic'>R</span><sub>2</sub> (all data) <span class='html-italic'><sup>a</sup></span></td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >0.0616</td></tr><tr ><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >Δ<span class='html-italic'>ρ</span><sub>max,min</sub>/e<sup>−</sup> Å<sup>−3</sup></td><td align='center' valign='middle' style='border-bottom:solid thin' class='html-align-center' >2.35, −2.66 </td></tr></tbody> </table> <div class='html-table_foot html-p'><div class='html-p' style='text-indent:0em;'><span class='html-fn-content'><span class='html-italic'><sup>a</sup> R</span><sub>1</sub> = Σ ∣ ∣<span class='html-italic'>F</span><sub>o</sub>∣ − ∣<span class='html-italic'>F</span><sub>c</sub>∣ ∣/Σ∣<span class='html-italic'>F</span><sub>o</sub>∣. <span class='html-italic'>wR</span><sub>2</sub> = (Σ [<span class='html-italic'>w</span>(<span class='html-italic'>F</span><sub>o</sub><sup>2</sup> − <span class='html-italic'>F</span><sub>c</sub><sup>2</sup>)<sup>2</sup>]/Σ<span class='html-italic'>wF</span><sub>o</sub><sup>4</sup>)<sup>1/2</sup>, <span class='html-italic'>w</span> = 1/[σ<sup>2</sup>(<span class='html-italic'>F</span><sub>o</sub><sup>2</sup>)].</span></div><div style='clear:both;'></div></div> </div> </section><section class='html-fn_group'><table><tr id=''><td></td><td><div class='html-p'><b>Disclaimer/Publisher’s Note:</b> The statements, opinions and data contained in all publications are solely those of the individual author(s) and contributor(s) and not of MDPI and/or the editor(s). MDPI and/or the editor(s) disclaim responsibility for any injury to people or property resulting from any ideas, methods, instructions or products referred to in the content.</div></td></tr></table></section> <section id="html-copyright"><br>© 2024 by the authors. Licensee MDPI, Basel, Switzerland. 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margin-top: 15px;"> <div><b>MDPI and ACS Style</b></div> <p> Watts, S.R.; Najera, L.; Ogunbunmi, M.O.; Bobev, S.; Baranets, S. β-Yb<sub>2</sub>CdSb<sub>2</sub>—A Complex Non-Centrosymmetric Zintl Polymorph. <em>Crystals</em> <b>2024</b>, <em>14</em>, 920. https://doi.org/10.3390/cryst14110920 </p> <div style="display: block"> <b>AMA Style</b><br> <p> Watts SR, Najera L, Ogunbunmi MO, Bobev S, Baranets S. β-Yb<sub>2</sub>CdSb<sub>2</sub>—A Complex Non-Centrosymmetric Zintl Polymorph. <em>Crystals</em>. 2024; 14(11):920. https://doi.org/10.3390/cryst14110920 </p> <b>Chicago/Turabian Style</b><br> <p> Watts, Spencer R., Larissa Najera, Michael O. Ogunbunmi, Svilen Bobev, and Sviatoslav Baranets. 2024. "β-Yb<sub>2</sub>CdSb<sub>2</sub>—A Complex Non-Centrosymmetric Zintl Polymorph" <em>Crystals</em> 14, no. 11: 920. https://doi.org/10.3390/cryst14110920 </p> <b>APA Style</b><br> <p> Watts, S. R., Najera, L., Ogunbunmi, M. O., Bobev, S., & Baranets, S. (2024). β-Yb<sub>2</sub>CdSb<sub>2</sub>—A Complex Non-Centrosymmetric Zintl Polymorph. <em>Crystals</em>, <em>14</em>(11), 920. https://doi.org/10.3390/cryst14110920 </p> </div> </div> <div class="info-box no-margin"> Note that from the first issue of 2016, this journal uses article numbers instead of page numbers. 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#advanced_search").submit(function(e) { var searchArguments = false; $(this).find("input,select").not("#search,.search-button").each(function() { if (undefined === $(this).val() || "" === $(this).val()) { $(this).attr('name', null); } else { $(this).attr('name'); searchArguments = true; } }); if (!searchArguments) { window.location = $(this).attr('action'); return false; } }); $(".hide-show-desktop-option").click(function(e) { e.preventDefault(); var parentDiv = $(this).closest("div"); $.ajax({ url: $(this).attr('href'), success: function(msg) { parentDiv.removeClass().hide(); } }); }); $(".generic-toggleable-header").click(function(e) { $(this).toggleClass("active"); $(this).next(".generic-toggleable-content").toggleClass("active"); }); /* * handle whole row as a link if the row contains only one visible link */ $("table.new tr").hover(function() { if ($(this).find("td:visible a").length == 1) { $(this).addClass("single-link"); } }, function() { $(this).removeClass("single-link"); }); 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&beta;-Yb2CdSb2&mdash;A Complex Non-Centrosymmetric Zintl Polymorph

β-Yb2CdSb2—A Complex Non-Centrosymmetric Zintl Polymorph