{"title":"Hydrothermal synthesis and structural determination of a three-dimensional microporous iron(III)phosphate: [H3N(CH2)4NH3]3[Fe8(HPO4)12(PO4)2(H2O)6]","authors":"M.B. Korzenski, G.L. Schimek, J.W. Kolis","doi":"10.1016/S0992-4361(98)80193-8","DOIUrl":"10.1016/S0992-4361(98)80193-8","url":null,"abstract":"<div><p>A new microporous iron (III) phosphate, [H<sub>3</sub>N(CH<sub>2</sub>)<sub>4</sub>NH<sub>3</sub>]<sub>3</sub>[Fe<sub>8</sub>(HPO<sub>4</sub>)<sub>12</sub>(PO<sub>4</sub>)<sub>2</sub>(H<sub>2</sub>O)<sub>6</sub>], has been prepared using low temperature hydrothermal methods and characterized by single-crystal X-ray diffraction, EDAX, infrared spectroscopy, thermogravimetric analysis and bond valence sums. The title compound crystallizes as light pink hexagonal-shaped tabs in the centrosymmetric hexagonal space group 3¯ (No.147) with <em>a</em> = <em>b</em> = 13.495(2) Å, <em>c</em> = 9.396(2) Å, V = 1481.9(4) Å<sup>3</sup> and Z = 4 with R/R<sub>w</sub> = 0.044/0.048. The compound exhibits a complicated three-dimensional microporous structure with quaternary ammonium ions acting as a template for the framework. It is similar to previously reported [HN(CH<sub>2</sub>CH<sub>2</sub>)<sub>3</sub>NH]<sub>3</sub>[Fe<sub>8</sub>(HPO<sub>4</sub>)<sub>12</sub>(PO<sub>4</sub>)<sub>2</sub>(H<sub>2</sub>O)<sub>6</sub>].</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 2","pages":"Pages 143-160"},"PeriodicalIF":0.0,"publicationDate":"1998-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(98)80193-8","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81398099","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Polychalcogenoaurates(I) with pseudo-onedimensional structures: Preparation and crystal structure of Cs2Au2Se3","authors":"K.O. Klepp, C. Weithaler","doi":"10.1016/S0992-4361(98)80189-6","DOIUrl":"10.1016/S0992-4361(98)80189-6","url":null,"abstract":"<div><p>Cs<sub>2</sub>Au<sub>2</sub>Se<sub>3</sub> was obtained as red platelike crystals by reacting a stoichiometric mixture of Cs<sub>2</sub>Se, Au and Se at 670K. It crystallizes in space group C2/c, Z = 4 with a = 9.769(5) Å, b = 13.44(1) Å, c = 7.178(3) Å, β = 90.69(1)°. The crystal structure was determined from single crystal data and refined to a conventional R of 0.042 for 674 Fo's and 34 variables. The characteristic structural feature of this new selenoaurate is the formation of infinite helical anionic chains, <sub>∞</sub><sup>1</sup>-[AuSeAuSe<sub>2</sub>]<sup>2−</sup> which run parallel to [001] and are separated by the alkali cations. The average Au-Se bond length is 2.402 Å, the bond length in the Se<sub>2</sub>-unit is 2.436 Å. Au…Au contacts of 3.200 Å, are formed within the anionic chains. The cesium atoms are coordinated to seven Se in an irregular configuration.</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 2","pages":"Pages 101-110"},"PeriodicalIF":0.0,"publicationDate":"1998-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(98)80189-6","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81478259","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Synthesis and crystal structure of two fluorophosphated compounds with different infinite sheets: Sr2Ga(HPO4)(PO4)F2 and Sr2Fe2(HPO4)(PO4)2F2","authors":"J.-M. Le Meins, A. Hemon-Ribaud, G. Courbion","doi":"10.1016/S0992-4361(98)80191-4","DOIUrl":"10.1016/S0992-4361(98)80191-4","url":null,"abstract":"<div><p>New compounds, Sr<sub>2</sub>Ga(HPO<sub>4</sub>)(PO<sub>4</sub>)F<sub>2</sub> and Sr<sub>2</sub>Fe<sub>2</sub>(HPO<sub>4</sub>)(PO<sub>4</sub>)<sub>2</sub>F<sub>2</sub>, have been prepared by hydrothermal synthesis (700°C, 180 MPa, 24 h) and characterized by single-crystal X-ray diffraction. Sr<sub>2</sub>Ga(HPO<sub>4</sub>)(PO<sub>4</sub>)F<sub>2</sub> crystallizes in the monoclinic space group P2<sub>1</sub>/n with a = 8.257(1) Å, b = 7.205(1) Å, c = 13.596(2) Å, β = 108.02(1)°, V = 769.2(2) Å<sup>3</sup> and Z = 4 and Sr<sub>2</sub>Fe<sub>2</sub>(HPO<sub>4</sub>)(PO<sub>4</sub>)<sub>2</sub>F<sub>2</sub> in the triclinic space group P2<sub>1</sub>/n with a = 8.072(1) Å, b = 8.794(1) Å, c = 8.885(1) Å, α = 102.46(1)°, β = 115.95(1)°, γ = 89.95(1)°, V = 550.6(1) Å<sup>3</sup> and Z = 2. Structures are both based on different sheets involving corner-linkage between octahedra and tetrahedra. The sheets are linked by Sr<sup>2+</sup> cations. Structural relationships exist between the descloizite mineral and the title compounds.</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 2","pages":"Pages 117-132"},"PeriodicalIF":0.0,"publicationDate":"1998-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(98)80191-4","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78462730","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
J.M. Bassat, C. Allançon, P. Odier, J.P. Loup, M. Deus Carvalho, A. Wattiaux
{"title":"Electronic properties of Pr4Ni3O10±δ","authors":"J.M. Bassat, C. Allançon, P. Odier, J.P. Loup, M. Deus Carvalho, A. Wattiaux","doi":"10.1016/S0992-4361(98)80195-1","DOIUrl":"10.1016/S0992-4361(98)80195-1","url":null,"abstract":"<div><p>Two synthesis methods for preparing Pr<sub>4</sub>Ni<sub>3</sub>O<sub>10±δ</sub> are compared : a modified sol — gel route and a nitrate — citrate one. It is shown that the autoignition involved in the nitrate — citrate route provides good conditions ressembling the Rapid Thermal Annealing procedure. The oxygen stoichiometry of Pr<sub>4</sub>Ni<sub>3</sub>O<sub>10±δ</sub> phases is measured according to the method of synthesis and thermal treatment. The compounds are metallic as seen by electrical resistivity measurements and thermoelectric power. We show that the adjustment of δ in this series is an important parameter of the transport properties that change from metallic for −0.1 <δ < 0.1 to insulating for Pr<sub>4</sub>Ni<sub>3</sub>O<sub>8.25</sub>. An electronic anomaly is evidenced at 160 K, which intensity is more marked for the stoichiometric Pr<sub>4</sub>Ni<sub>3</sub>O<sub>10</sub>. Our results are consistent with the existence of a charge density wave instability.</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 2","pages":"Pages 173-188"},"PeriodicalIF":0.0,"publicationDate":"1998-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(98)80195-1","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75502339","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
D. Mercurio, J.C. Champarnaud-Mesjard, I. Gouby, B. Frit
{"title":"On the crystal structure of Bi2Te2O7","authors":"D. Mercurio, J.C. Champarnaud-Mesjard, I. Gouby, B. Frit","doi":"10.1016/S0992-4361(98)80014-3","DOIUrl":"10.1016/S0992-4361(98)80014-3","url":null,"abstract":"<div><p>Bi<sub>2</sub>Te<sub>2</sub>O<sub>7</sub> is orthothobic, space group Pbcn. The lattice parameters derived from a Guinier powder pattern (Si standard) are: a= 22.794 ± 0.005, b= 5.526 ± 0.001, c= 22.065 ± 0.005Å, z= 16. The structure was solved by analysis of single crystal X-ray data and refined on the basis of neutron powder diffraction data. It is an anion-deficient 4: 1: 4 superstructure of fluorite in which the electron lone-pairs of tellurium are stereochemically active. The structural relationships with fluorite and with Bi<sub>2</sub>TeO<sub>5</sub> (and other anion-deficient fluorite-related superstructures) have been shown and discussed.</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 1","pages":"Pages 49-65"},"PeriodicalIF":0.0,"publicationDate":"1998-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(98)80014-3","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74122376","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"XRD study of the goethite-hematite transformation: Application to the identification of heated prehistoric pigments","authors":"M.P. Pomiès , G. Morin, C. Vignaud","doi":"10.1016/S0992-4361(98)80011-8","DOIUrl":"10.1016/S0992-4361(98)80011-8","url":null,"abstract":"<div><p>When heated, yellow goethite dehydrates and transforms to red hematite. Both iron oxides were used by the Palaeolithic artists as pigments, one question being whether those people took advantage of the phase transformation. To answer this question, the dehydration of synthetic goethite was studied by XRD coupled to Rietveld refinement. It was shown that no hydroxylated hematite is formed during the early stages of dehydration, the presence of hydroxyl ions in materials treated at high temperatures being explained by trapped water inside porous microstructure (TEM). Archaeological samples from the south of France were investigated. Some of them exhibit distinctive features of heating which, supports the idea that Palaeolithic people used both natural and ex-goethite hematite.</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 1","pages":"Pages 9-25"},"PeriodicalIF":0.0,"publicationDate":"1998-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(98)80011-8","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72927115","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
F. Bosselet , B.F. Mentzen , J.C. Viala , M.A. Etoh , J. Bouix
{"title":"Synthesis, and structure of T2-Al2MgC2","authors":"F. Bosselet , B.F. Mentzen , J.C. Viala , M.A. Etoh , J. Bouix","doi":"10.1016/S0992-4361(98)80017-9","DOIUrl":"10.1016/S0992-4361(98)80017-9","url":null,"abstract":"<div><p>The T<sub>1</sub> and T<sub>2</sub> crystalline varieties of the ternary carbide Al<sub>2</sub>MgC<sub>2</sub> were synthesized by reacting graphite particles with Mg-Al melts at 930–1020 K. Below 1000 K, the T<sub>1</sub> variety was predominant but little amounts of T<sub>2</sub> were also present. At 1000 K and above, only the T<sub>2</sub> variety was obtained. Assuming a hexagonal close packing of the metal atoms, the crystal structure of T<sub>2</sub>-Al<sub>2</sub>MgC<sub>2</sub> was determined by Rietveld refinemenent from X-ray powder diffraction data.</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 1","pages":"Pages 91-99"},"PeriodicalIF":0.0,"publicationDate":"1998-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(98)80017-9","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72615125","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"The crystal structure of a complex barium, aluminium, copper(II) fluoride: Ba4Cu2Al3F21","authors":"N. Dupont, M. Samouël, P. Gredin, A. de Kozak","doi":"10.1016/S0992-4361(98)80013-1","DOIUrl":"10.1016/S0992-4361(98)80013-1","url":null,"abstract":"<div><p>Ba<sub>4</sub>Cu<sub>2</sub>Al<sub>3</sub>F<sub>21</sub> is orthorhombic : a = 5.299(1) Å, b = 7.318(1) Å, c = 41.529(7) Å, Z = 4. The crystal structure was solved in the space group P2<sub>1</sub>2<sub>1</sub>2<sub>1</sub> (n<sup>o</sup>19) from X-ray single crystal data using 5682 unique reflections (3698 with F<sub>O</sub>/σ(F) > 4). It consists in a succession along <em>c</em> of 8 layers of 2 different types of sheets. The first layer, formulated [Cu<sub>2</sub>AlF<sub>11</sub>]<sup>4−</sup> in which copper-fluorine octahedra are linked by edges to form infinite distorted chains connected together by aluminium-fluorine octahedra, is followed by two [Al<sub>2</sub>F<sub>10</sub>]<sup>4−</sup> layers of infinite cischains of aluminium-fluorine octahedra linked by two vertices and another [Cu<sub>2</sub>AlF<sub>11</sub>]<sup>4−</sup> layer. These 4 layers are doubled along c by one of the screw-axes 2<sub>1</sub>. The barium ions, 12-coordinated, are inserted between the sheets.</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 1","pages":"Pages 39-47"},"PeriodicalIF":0.0,"publicationDate":"1998-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(98)80013-1","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85453571","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Crystal structure of Ba2La4Ti5O18, member n = 6 of the homologous series (Ba,La)nTin−1O3n of cation deficient perovskite-related compounds","authors":"N. Harre, D. Mercurio, G. Trolliard, B. Frit","doi":"10.1016/S0992-4361(98)80016-7","DOIUrl":"10.1016/S0992-4361(98)80016-7","url":null,"abstract":"<div><p>Ba<sub>2</sub>La<sub>4</sub>Ti<sub>5</sub>O<sub>18</sub> crystallizes in the trigonal system (space group R3) with the unit-cell parameters: a = 5.584 (1) Å; c = 41.176 (8) Å; Z= 3.</p><p>The structure has been solved from single crystal X-ray diffraction data to a final R<sub>1</sub> = 0.0285. Ba and La atoms are twelve-fold coordinated and Ti atoms six-fold coordinated. The structure can be described as consisting of identical perovskite-like blocks, five corner-sharing TiO<sub>6</sub> octahedra thick, separated by layers of vacant octahedra. The distortion of the cation and anion sublattices has been analysed and a Ba/La order has been evidenced.</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 1","pages":"Pages 77-90"},"PeriodicalIF":0.0,"publicationDate":"1998-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(98)80016-7","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82903006","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"An investigation of microporous cetineite-type phases A6[B12O18][CX3]2[Dx(H2O,OH,O)6−y] I. The cetineite structure field","authors":"X. Wang , F. Liebau","doi":"10.1016/S0992-4361(98)80012-X","DOIUrl":"10.1016/S0992-4361(98)80012-X","url":null,"abstract":"<div><p>Hydrothermal syntheses between 120 and 200 °C have been performed to determine the chemical variability of semiconducting microporous materials with cetineite structure. The syntheses were based on the general formula A<sub>6</sub>[B<sub>12</sub>O<sub>18</sub>][CX<sub>3</sub>]<sub>2</sub>[D<sub>x</sub>(H<sub>2</sub>O,OH,O)<sub>6−y</sub>], (0≤×≤2; 0≤y≤6), which was derived from X-ray crystal structure refinements. A = Li<sup>+</sup>, Na<sup>+</sup>, K<sup>+</sup>, Rb<sup>+</sup>, Cs<sup>+</sup>, Tl<sup>+</sup>, NH<sub>4</sub><sup>+</sup>, Ca<sup>2+</sup>, Sr<sup>2+</sup>, and Ba<sup>2+</sup> were introduced as hydroxides, in some cases as carbonates, B = C = As<sup>3+</sup>, Sb<sup>3+</sup>, and Bi<sup>3+</sup>, and X = S<sup>2−</sup>, Se<sup>2−</sup>, and Te<sup>2−</sup> as elements. Only syntheses with B = C = Sb<sup>3+</sup> and X = S<sup>2−</sup> and Se<sup>2−</sup> were successfull. Known cetineite-type phases now include the element combinations A/Sb<sup>3+</sup>/S<sup>2−</sup> with A = Na<sup>+</sup> and K<sup>+</sup>, and A/Sb<sup>3+</sup>/Se<sup>2−</sup> with A = Na<sup>+</sup>, K<sup>+</sup>, Rb<sup>+</sup>, Sr<sup>2+</sup>, Ba<sup>2+</sup>, and probably Tl<sup>+</sup>. Variable amounts of Na<sup>+</sup>, Sb<sup>3+</sup> and C<sup>4+</sup> were found to occupy the <strong>D</strong> position of the cetineite-type structure. The chemical variability can be described by the coupled substitutions A<sup>+</sup> + H<sub>2</sub>OA<sup>2+</sup> + OH<sup>−</sup> mH<sub>2</sub>O<strong>D</strong><sup>m+</sup> + mOH, and nOH<sup>−</sup>D<sup>n+</sup> + nO<sup>2−</sup>. The crystals obtained are orange to dark red, in agreement with their semiconducting properties.</p></div>","PeriodicalId":100507,"journal":{"name":"European Journal of Solid State and Inorganic Chemistry","volume":"35 1","pages":"Pages 27-37"},"PeriodicalIF":0.0,"publicationDate":"1998-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0992-4361(98)80012-X","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77150002","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}