Mixed‐Metal Monophosphate Tungsten Bronzes Containing Rhodium and Iridium
Solution combustion synthesis followed by annealing in air led to the MPTB‐related phosphates (Rh1/6W5/6O3)8(PO2)4, (Ir1/6W5/6O3)8(PO2)4 (a=5.258(2) Å, b=6.538(3) Å, c=17.322(8) Å), (Rh1/9W8/9O3)12(PO2)4 and (Rh2/21W19/21O3)14(PO2)4. Single‐crystals of the mixed‐metal (Rh,W)‐MPTBs at m=4 and at m=7...
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| Veröffentlicht in: | European journal of inorganic chemistry 2021-04, Vol.2021 (15), p.1459-1469 |
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| creator | Karbstein, Alexander Weber, Markus Lahr, Dominic Daniels, Jörg Assenmacher, Wilfried Mader, Werner Rosowski, Frank Schunk, Stephan A. Glaum, Robert |
| description | Solution combustion synthesis followed by annealing in air led to the MPTB‐related phosphates (Rh1/6W5/6O3)8(PO2)4, (Ir1/6W5/6O3)8(PO2)4 (a=5.258(2) Å, b=6.538(3) Å, c=17.322(8) Å), (Rh1/9W8/9O3)12(PO2)4 and (Rh2/21W19/21O3)14(PO2)4. Single‐crystals of the mixed‐metal (Rh,W)‐MPTBs at m=4 and at m=7 were grown by chemical vapor transport (CVT). Their crystal structures have been refined from X‐ray single‐crystal data {(Rh,W)‐MPTB at m=4: P212121, Z=1, a=5.2232(3) Å, b=6.4966(3) Å, c=17.3819(9) Å, R1=0.032, wR2=0.075 for 1714 unique reflections, 1524 with Fo>4σ(Fo), 66 variables, 1 constraint, composition from refinement (Rh0.15W0.85O3)8(PO2)4; (Rh,W)‐MPTB at m=7: P21/n, Z=1, a=5.2510(4) Å, b=6.4949(5) Å, c=26.685(2) Å, β=90.30(1)°, R1=0.060, wR2=0.163 for 2074 unique reflections, 1894 with Fo>4σ(Fo), 100 variables, comp. from ref. (Rh0.07W0.93O3)14(PO2)4}. These structure refinements show unexpected distribution of Rh and W over the available metal sites. Further characterization (powder reflectance and magnetic measurements) of the (Rh,W)‐MPTB at m=4 and at m=7 suggest for both phases a homogeneity range with respect to the Rh/W ratio and the presence of small amounts of W5+ besides Rh3+ and W6+. Results of the ligand field analysis for the reference material Rh(PO3)3, which is containing the octahedral chromophore [RhIIIO6], are reported (Δo=23200 cm−1, B=490 cm−1).
Incorporation of rhodium or iridium in phosphates of the MPTB structure family is possible. SXRD analysis of (Rh1/6W5/6O3)8(PO2)4 and (Rh2/21W19/21O3)14(PO2)4 reveals an unexpected distribution pattern for Rh3+ over the available metal sites. Results of further characterization by TEM, powder reflectance spectroscopy and magnetic measurements are reported. |
| doi_str_mv | 10.1002/ejic.202100047 |
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Incorporation of rhodium or iridium in phosphates of the MPTB structure family is possible. SXRD analysis of (Rh1/6W5/6O3)8(PO2)4 and (Rh2/21W19/21O3)14(PO2)4 reveals an unexpected distribution pattern for Rh3+ over the available metal sites. Results of further characterization by TEM, powder reflectance spectroscopy and magnetic measurements are reported.</description><identifier>ISSN: 1434-1948</identifier><identifier>EISSN: 1099-0682</identifier><identifier>DOI: 10.1002/ejic.202100047</identifier><language>eng</language><publisher>Weinheim: Wiley Subscription Services, Inc</publisher><subject>Chromophores ; Combustion synthesis ; Crystal structure ; Crystals ; Equilibrium relations ; Homogeneity ; Inorganic chemistry ; Iridium ; Magnetic measurement ; MPTB ; Phosphates ; Rhodium ; Solid-state chemistry ; Solid-state structure ; Tungsten bronze ; Uniqueness</subject><ispartof>European journal of inorganic chemistry, 2021-04, Vol.2021 (15), p.1459-1469</ispartof><rights>2021 The Authors. European Journal of Inorganic Chemistry published by Wiley-VCH GmbH</rights><rights>2021. This article is published under http://creativecommons.org/licenses/by-nc/4.0/ (the “License”). Notwithstanding the ProQuest Terms and Conditions, you may use this content in accordance with the terms of the License.</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c3577-cc873816e1a236d8f918cb661855d306c56e41d49876f406976fc41b8fa626d43</citedby><cites>FETCH-LOGICAL-c3577-cc873816e1a236d8f918cb661855d306c56e41d49876f406976fc41b8fa626d43</cites><orcidid>0000-0002-1253-4566 ; 0000-0002-4958-5092 ; 0000-0001-5805-1466 ; 0000-0002-5044-1766</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://onlinelibrary.wiley.com/doi/pdf/10.1002%2Fejic.202100047$$EPDF$$P50$$Gwiley$$Hfree_for_read</linktopdf><linktohtml>$$Uhttps://onlinelibrary.wiley.com/doi/full/10.1002%2Fejic.202100047$$EHTML$$P50$$Gwiley$$Hfree_for_read</linktohtml><link.rule.ids>314,780,784,1417,27923,27924,45573,45574</link.rule.ids></links><search><creatorcontrib>Karbstein, Alexander</creatorcontrib><creatorcontrib>Weber, Markus</creatorcontrib><creatorcontrib>Lahr, Dominic</creatorcontrib><creatorcontrib>Daniels, Jörg</creatorcontrib><creatorcontrib>Assenmacher, Wilfried</creatorcontrib><creatorcontrib>Mader, Werner</creatorcontrib><creatorcontrib>Rosowski, Frank</creatorcontrib><creatorcontrib>Schunk, Stephan A.</creatorcontrib><creatorcontrib>Glaum, Robert</creatorcontrib><title>Mixed‐Metal Monophosphate Tungsten Bronzes Containing Rhodium and Iridium</title><title>European journal of inorganic chemistry</title><description>Solution combustion synthesis followed by annealing in air led to the MPTB‐related phosphates (Rh1/6W5/6O3)8(PO2)4, (Ir1/6W5/6O3)8(PO2)4 (a=5.258(2) Å, b=6.538(3) Å, c=17.322(8) Å), (Rh1/9W8/9O3)12(PO2)4 and (Rh2/21W19/21O3)14(PO2)4. Single‐crystals of the mixed‐metal (Rh,W)‐MPTBs at m=4 and at m=7 were grown by chemical vapor transport (CVT). Their crystal structures have been refined from X‐ray single‐crystal data {(Rh,W)‐MPTB at m=4: P212121, Z=1, a=5.2232(3) Å, b=6.4966(3) Å, c=17.3819(9) Å, R1=0.032, wR2=0.075 for 1714 unique reflections, 1524 with Fo>4σ(Fo), 66 variables, 1 constraint, composition from refinement (Rh0.15W0.85O3)8(PO2)4; (Rh,W)‐MPTB at m=7: P21/n, Z=1, a=5.2510(4) Å, b=6.4949(5) Å, c=26.685(2) Å, β=90.30(1)°, R1=0.060, wR2=0.163 for 2074 unique reflections, 1894 with Fo>4σ(Fo), 100 variables, comp. from ref. (Rh0.07W0.93O3)14(PO2)4}. These structure refinements show unexpected distribution of Rh and W over the available metal sites. Further characterization (powder reflectance and magnetic measurements) of the (Rh,W)‐MPTB at m=4 and at m=7 suggest for both phases a homogeneity range with respect to the Rh/W ratio and the presence of small amounts of W5+ besides Rh3+ and W6+. Results of the ligand field analysis for the reference material Rh(PO3)3, which is containing the octahedral chromophore [RhIIIO6], are reported (Δo=23200 cm−1, B=490 cm−1).
Incorporation of rhodium or iridium in phosphates of the MPTB structure family is possible. SXRD analysis of (Rh1/6W5/6O3)8(PO2)4 and (Rh2/21W19/21O3)14(PO2)4 reveals an unexpected distribution pattern for Rh3+ over the available metal sites. Results of further characterization by TEM, powder reflectance spectroscopy and magnetic measurements are reported.</description><subject>Chromophores</subject><subject>Combustion synthesis</subject><subject>Crystal structure</subject><subject>Crystals</subject><subject>Equilibrium relations</subject><subject>Homogeneity</subject><subject>Inorganic chemistry</subject><subject>Iridium</subject><subject>Magnetic measurement</subject><subject>MPTB</subject><subject>Phosphates</subject><subject>Rhodium</subject><subject>Solid-state chemistry</subject><subject>Solid-state structure</subject><subject>Tungsten bronze</subject><subject>Uniqueness</subject><issn>1434-1948</issn><issn>1099-0682</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2021</creationdate><recordtype>article</recordtype><sourceid>24P</sourceid><sourceid>WIN</sourceid><recordid>eNqFkL9OwzAYxC0EEqWwMkdiTrHjP7FHiAoEWiGhMluu47SuWjvYiaBMPALPyJOQqghGprtP-t190gFwjuAIQZhdmpXVowxm_QFJfgAGCAqRQsazw94TTFIkCD8GJzGuegRDzAbgYWrfTPX18Tk1rVonU-98s_SxWarWJLPOLWJrXHIdvHs3MSm8a5V11i2Sp6WvbLdJlKuSMtidPwVHtVpHc_ajQ_B8M54Vd-nk8bYsriapxjTPU615jjliBqkMs4rXAnE9ZwxxSisMmabMEFQRwXNWE8hEL5qgOa8Vy1hF8BBc7Hub4F86E1u58l1w_UuZUYQppUyInhrtKR18jMHUsgl2o8JWIih3g8ndYPJ3sD4g9oFXuzbbf2g5vi-Lv-w3ll9vJw</recordid><startdate>20210422</startdate><enddate>20210422</enddate><creator>Karbstein, Alexander</creator><creator>Weber, Markus</creator><creator>Lahr, Dominic</creator><creator>Daniels, Jörg</creator><creator>Assenmacher, Wilfried</creator><creator>Mader, Werner</creator><creator>Rosowski, Frank</creator><creator>Schunk, Stephan A.</creator><creator>Glaum, Robert</creator><general>Wiley Subscription Services, Inc</general><scope>24P</scope><scope>WIN</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7SR</scope><scope>7U5</scope><scope>8BQ</scope><scope>8FD</scope><scope>JG9</scope><scope>L7M</scope><orcidid>https://orcid.org/0000-0002-1253-4566</orcidid><orcidid>https://orcid.org/0000-0002-4958-5092</orcidid><orcidid>https://orcid.org/0000-0001-5805-1466</orcidid><orcidid>https://orcid.org/0000-0002-5044-1766</orcidid></search><sort><creationdate>20210422</creationdate><title>Mixed‐Metal Monophosphate Tungsten Bronzes Containing Rhodium and Iridium</title><author>Karbstein, Alexander ; Weber, Markus ; Lahr, Dominic ; Daniels, Jörg ; Assenmacher, Wilfried ; Mader, Werner ; Rosowski, Frank ; Schunk, Stephan A. ; Glaum, Robert</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c3577-cc873816e1a236d8f918cb661855d306c56e41d49876f406976fc41b8fa626d43</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2021</creationdate><topic>Chromophores</topic><topic>Combustion synthesis</topic><topic>Crystal structure</topic><topic>Crystals</topic><topic>Equilibrium relations</topic><topic>Homogeneity</topic><topic>Inorganic chemistry</topic><topic>Iridium</topic><topic>Magnetic measurement</topic><topic>MPTB</topic><topic>Phosphates</topic><topic>Rhodium</topic><topic>Solid-state chemistry</topic><topic>Solid-state structure</topic><topic>Tungsten bronze</topic><topic>Uniqueness</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Karbstein, Alexander</creatorcontrib><creatorcontrib>Weber, Markus</creatorcontrib><creatorcontrib>Lahr, Dominic</creatorcontrib><creatorcontrib>Daniels, Jörg</creatorcontrib><creatorcontrib>Assenmacher, Wilfried</creatorcontrib><creatorcontrib>Mader, Werner</creatorcontrib><creatorcontrib>Rosowski, Frank</creatorcontrib><creatorcontrib>Schunk, Stephan A.</creatorcontrib><creatorcontrib>Glaum, Robert</creatorcontrib><collection>Wiley-Blackwell Open Access Titles</collection><collection>Wiley Free Content</collection><collection>CrossRef</collection><collection>Engineered Materials Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Technology Research Database</collection><collection>Materials Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><jtitle>European journal of inorganic chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Karbstein, Alexander</au><au>Weber, Markus</au><au>Lahr, Dominic</au><au>Daniels, Jörg</au><au>Assenmacher, Wilfried</au><au>Mader, Werner</au><au>Rosowski, Frank</au><au>Schunk, Stephan A.</au><au>Glaum, Robert</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Mixed‐Metal Monophosphate Tungsten Bronzes Containing Rhodium and Iridium</atitle><jtitle>European journal of inorganic chemistry</jtitle><date>2021-04-22</date><risdate>2021</risdate><volume>2021</volume><issue>15</issue><spage>1459</spage><epage>1469</epage><pages>1459-1469</pages><issn>1434-1948</issn><eissn>1099-0682</eissn><abstract>Solution combustion synthesis followed by annealing in air led to the MPTB‐related phosphates (Rh1/6W5/6O3)8(PO2)4, (Ir1/6W5/6O3)8(PO2)4 (a=5.258(2) Å, b=6.538(3) Å, c=17.322(8) Å), (Rh1/9W8/9O3)12(PO2)4 and (Rh2/21W19/21O3)14(PO2)4. Single‐crystals of the mixed‐metal (Rh,W)‐MPTBs at m=4 and at m=7 were grown by chemical vapor transport (CVT). Their crystal structures have been refined from X‐ray single‐crystal data {(Rh,W)‐MPTB at m=4: P212121, Z=1, a=5.2232(3) Å, b=6.4966(3) Å, c=17.3819(9) Å, R1=0.032, wR2=0.075 for 1714 unique reflections, 1524 with Fo>4σ(Fo), 66 variables, 1 constraint, composition from refinement (Rh0.15W0.85O3)8(PO2)4; (Rh,W)‐MPTB at m=7: P21/n, Z=1, a=5.2510(4) Å, b=6.4949(5) Å, c=26.685(2) Å, β=90.30(1)°, R1=0.060, wR2=0.163 for 2074 unique reflections, 1894 with Fo>4σ(Fo), 100 variables, comp. from ref. (Rh0.07W0.93O3)14(PO2)4}. These structure refinements show unexpected distribution of Rh and W over the available metal sites. Further characterization (powder reflectance and magnetic measurements) of the (Rh,W)‐MPTB at m=4 and at m=7 suggest for both phases a homogeneity range with respect to the Rh/W ratio and the presence of small amounts of W5+ besides Rh3+ and W6+. Results of the ligand field analysis for the reference material Rh(PO3)3, which is containing the octahedral chromophore [RhIIIO6], are reported (Δo=23200 cm−1, B=490 cm−1).
Incorporation of rhodium or iridium in phosphates of the MPTB structure family is possible. SXRD analysis of (Rh1/6W5/6O3)8(PO2)4 and (Rh2/21W19/21O3)14(PO2)4 reveals an unexpected distribution pattern for Rh3+ over the available metal sites. Results of further characterization by TEM, powder reflectance spectroscopy and magnetic measurements are reported.</abstract><cop>Weinheim</cop><pub>Wiley Subscription Services, Inc</pub><doi>10.1002/ejic.202100047</doi><tpages>11</tpages><orcidid>https://orcid.org/0000-0002-1253-4566</orcidid><orcidid>https://orcid.org/0000-0002-4958-5092</orcidid><orcidid>https://orcid.org/0000-0001-5805-1466</orcidid><orcidid>https://orcid.org/0000-0002-5044-1766</orcidid><oa>free_for_read</oa></addata></record> |
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| subjects | Chromophores Combustion synthesis Crystal structure Crystals Equilibrium relations Homogeneity Inorganic chemistry Iridium Magnetic measurement MPTB Phosphates Rhodium Solid-state chemistry Solid-state structure Tungsten bronze Uniqueness |
| title | Mixed‐Metal Monophosphate Tungsten Bronzes Containing Rhodium and Iridium |
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