Phasenbeziehungen im System Se-SeCl4 und die Kristallstruktur einer metastabilen Modifikation von SeCl4 / Phase Relations in the System Se-SeCl4 and the Crystal Structure of a Metastable Modification of SeCl4

Born, P. J.; Kniep, Rüdiger; Mootz, D.

doi:10.1515/znb-1981-1206

Cited by 30 publications

(5 citation statements)

References 5 publications

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“…13 Few colorless crystals identified as β-SeCl 4 were also isolated from the decanted solution after several days, which could be formed only in a reaction of SeO 3 with CCl 4 . 14 The possible subproducts of this reaction are phosgene and CO 2 . However, all our attempts to confirm their presence in the reaction mixture were futile.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…However, it is not possible to eliminate the solvating dioxane molecules even under vacuum; thus, unsolvated Se 3 O 7 should be prepared as reported previously . Few colorless crystals identified as β-SeCl 4 were also isolated from the decanted solution after several days, which could be formed only in a reaction of SeO 3 with CCl 4 . The possible subproducts of this reaction are phosgene and CO 2 .…”

Section: Resultsmentioning

confidence: 99%

“…Exposing 1 to temperatures over 15 °C or any attempt to recrystallize it led to its decomposition. Raman spectrum: ν̃(int) 109 (33), 128 (46), 135 (39), 177 (59), 204 (43), 278 (33), 331 (31), 393 (15), 408 (25), 473 (31), 594 (6), 716 (5), 826 (53), 849 (10), 876 (6), 926 (100), 987 (34), 994 (80), 1012 (34), 1039 (5), 1089 (6), 1129 (15), 1221 (10), 1298 (6), 1308 (16), 1338 (5), 1376 (5), 1446 (16), 1460 (12), 2670 (2), 2723 (3), 2744 (3), 2782 (3), 2867 (7), 2875 (8), 2900 (10), 2919 (11), 2933 (15), 2948 (12), 2986 (22), 2996 (14), 3013 (17) cm −1 .…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

“…Compound 2 is isolated by filtration and drying in vacuum in 80% yield. Raman spectrum: ν̃(int) 113 (22), 147 (29), 181 (58), 212 (10), 234 (9), 258 (5), 281 (14), 323 (33), 337 (28), 394b (9), 426 (3), 447 (14), 460 (5), 484 (17), 548b (11), 568sh (5), 819 (50), 824 (69), 847 (10), 852 (8), 921 (75), 958 (36), 987 (100), 1011 (30), 1038 (3), 1086 (3), 1125 (13), 1218 (10), 1225 (6), 1295sh (4), 1301sh (5), 1308 (17), 1335 (3), 1374 (5), 1383 (5), 1399 (2), 1443 (19), 1460 (13), 2732 (5), 2737 (6), 2791 (5), 2869 (21), 2895 (20), 2911 (21), 2925 (22), 2971 (21), 2985 (29), 2991sh (26) cm −1 .…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

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Taming the Oxidative Power of SeO₃ in 1,4-Dioxane, Isolation of Two New Isomers of Mixed-Valence Selenium Oxides, and Two Unprecedented Cyclic Esters of Selenic Acid

et al. 2014

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The reaction of (SeO3)4 with 1,4-dioxane (diox, dioxane) with or without diluting solvent led to the isolation of the unprecedented esters of selenic acid-1,2-ethyl selenate (CH2O)2SeO2 and the glyoxal diselenate O2Se[(OCHO)2]SeO2. It was possible to isolate an unknown dimeric form of Se2O5 (Se4O10·(diox)2) and a geometrical isomer of the mixed-valence oxide trans-Se3O7, both stabilized by dioxane. The dioxane adduct of monomeric selenium trioxide SeO3·diox was obtained from the reaction of (SeO3)4 with dioxane in liquid SO2. The reaction mechanism for the formation of these compounds was elucidated, and the molecular structure of the unstable form of the selenium trioxide was determined, consisting in a trimeric arrangement (SeO3)3.

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Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: ■ Experimental Sectionmentioning

confidence: 99%

Section: ■ Experimental Sectionmentioning

confidence: 99%

See 2 more Smart Citations

Taming the Oxidative Power of SeO₃ in 1,4-Dioxane, Isolation of Two New Isomers of Mixed-Valence Selenium Oxides, and Two Unprecedented Cyclic Esters of Selenic Acid

et al. 2014

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“…The vertex‐connected [SeCl 6 ] 2– octahedra within the infinite chains 1 ∞ {[SeCl t 4/1 Cl v 2/2 ] – } (t = terminal, v = vertex‐connecting) in [PCl 4 ][SeCl 5 ] behave alike, as they share cis ‐oriented corners, while monomeric [SeCl 5 ] – anions with the expected ψ 1 ‐octahedral shape still remain unknown. Even the tetrameric SeCl 4 (= [Se 4 Cl 4 ]Cl 12 ) with a molecular heterocubane core gives only a slight idea of lone‐pair influence according to {[SeCl 3 ] + (Cl – )} 4 , . With mixed ligands such as oxygen and chlorine in complexes like [SeOCl 3 ] – condensation and lone‐pair activity are found, since dimers [Se 2 O 2 Cl 6 ] 2– with a bridging Cl – ··· Cl – edge of two square [SeOCl 4 ] 2– pyramids with trans ‐oriented oxygen (and lone‐pair) vertices dominate the structure of [As(C 6 H 5 ) 4 ] 2 [Se 2 O 2 Cl 6 ] .…”

Section: Introductionmentioning

confidence: 99%

Sm₃O₂Sm[SeO₃]₄ and Sm₃O₂Cl[SeO₃]₂: A Monoclinic Form of Samarium Oxide Oxoselenate(IV) and a Samarium Oxide Chloride Oxoselenate(IV) both with ¹_∞{[O₂Sm₃]⁵⁺} Chains

Zitzer

Greiner

et al. 2018

Zeitschrift anorg allge chemie

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Appropriate mixtures of Sm2O3 and SeO2 with various chloride fluxes yielded single crystals of Sm3O2Sm[SeO3]4 (monoclinic, P21/n; a = 1497.89(8), b = 556.61(3), c = 1639.63(9) pm, β = 91.054(3)° with Z = 8 for Sm2Se2O7) or Sm3O2Cl[SeO3]2 (orthorhombic, Pnma; a = 565.82(4), b = 1457.14(9), c = 1145.23(7) pm and Z = 4). In contrast to the known tetragonal form of Sm2Se2O7, the monoclinic one exhibits four crystallographically different Sm3+ and Se4+ cations. Nonetheless [OSm4]10+ tetrahedra are connected by trans‐oriented edges to single chains 1∞{[OSm4/2]4+} like in tetragonal Sm2O[SeO3]2. The monoclinic form, however, displays double chains 1∞{[O2Sm3]5+} of edge‐linked [OSm4]10+ tetrahedra, which are also present in the samarium(III) oxide chloride oxoselenate(IV) Sm3O2Cl[SeO3]2. Both tetragonal Sm2O[SeO3]2 and monoclinic Sm3O2Sm[SeO3]4 with the empirical formula Sm2Se2O7 as well as Sm3O2Cl[SeO3]2 contain empty channels in their crystal structures, apt to accommodate the lone‐pair electrons at the Se4+ cations. These are residing in isolated ψ1‐tetrahedral [SeO3]2― anions. Non‐selenium bonded oxide anions (and if necessary chloride anions in the case of Sm3O2Cl[SeO3]2) take care of the charge balance. The much higher density (Dx = 6.207 g·cm–3) of the tetragonal form (P42/ncm; a = 1077.03(8), c = 526.38(4) pm) indicates the new monoclinic modification of Sm2Se2O7 (Dx = 5.546 g·cm–3) as high‐temperature phase, which is confirmed by its synthesis under fast quenching conditions.

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Selenium: Inorganic ChemistryBased in part on the article Selenium: Inorganic Chemistry by Bernt Krebs, Stefan Bonmann, & Illenora Eidenschink which appeared in theEncyclopedia of Inorganic Chemistry, First Edition.

Atwood

2005

Encyclopedia of Inorganic Chemistry

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Selenium is the first member of the group 16 elements O, S, Se, Te, and Po that shows some metallic character. The increasing metallic character in the series O, S, Se, Te, Po is reflected also in the lower electronegativity, in the less acid character of the oxides, and in the lower stability of the oxidation number +VI for selenium compared to sulfur. There is a large variety of compounds of SeII, SeIV, and SeVI with the electronegative elements N, O, F, Cl, and Br. Thus, there are six general types of compounds, and these will comprise the main sections in the article. They are cations, halides, oxides, haloselenates, oxohaloselenates, and the related compounds that form when both selenium and nitrogen are present in the molecule.

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Phasenbeziehungen im System Se-SeCl₄ und die Kristallstruktur einer metastabilen Modifikation von SeCl₄ / Phase Relations in the System Se-SeCl₄ and the Crystal Structure of a Metastable Modification of SeCl₄

Cited by 30 publications

References 5 publications

Taming the Oxidative Power of SeO₃ in 1,4-Dioxane, Isolation of Two New Isomers of Mixed-Valence Selenium Oxides, and Two Unprecedented Cyclic Esters of Selenic Acid

Taming the Oxidative Power of SeO₃ in 1,4-Dioxane, Isolation of Two New Isomers of Mixed-Valence Selenium Oxides, and Two Unprecedented Cyclic Esters of Selenic Acid

Sm₃O₂Sm[SeO₃]₄ and Sm₃O₂Cl[SeO₃]₂: A Monoclinic Form of Samarium Oxide Oxoselenate(IV) and a Samarium Oxide Chloride Oxoselenate(IV) both with ¹_∞{[O₂Sm₃]⁵⁺} Chains

Selenium: Inorganic ChemistryBased in part on the article Selenium: Inorganic Chemistry by Bernt Krebs, Stefan Bonmann, & Illenora Eidenschink which appeared in theEncyclopedia of Inorganic Chemistry, First Edition.

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Phasenbeziehungen im System Se-SeCl4 und die Kristallstruktur einer metastabilen Modifikation von SeCl4 / Phase Relations in the System Se-SeCl4 and the Crystal Structure of a Metastable Modification of SeCl4

Cited by 30 publications

References 5 publications

Taming the Oxidative Power of SeO3 in 1,4-Dioxane, Isolation of Two New Isomers of Mixed-Valence Selenium Oxides, and Two Unprecedented Cyclic Esters of Selenic Acid

Taming the Oxidative Power of SeO3 in 1,4-Dioxane, Isolation of Two New Isomers of Mixed-Valence Selenium Oxides, and Two Unprecedented Cyclic Esters of Selenic Acid

Sm3O2Sm[SeO3]4 and Sm3O2Cl[SeO3]2: A Monoclinic Form of Samarium Oxide Oxoselenate(IV) and a Samarium Oxide Chloride Oxoselenate(IV) both with 1∞{[O2Sm3]5+} Chains

Selenium: Inorganic ChemistryBased in part on the article Selenium: Inorganic Chemistry by Bernt Krebs, Stefan Bonmann, & Illenora Eidenschink which appeared in theEncyclopedia of Inorganic Chemistry, First Edition.

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Phasenbeziehungen im System Se-SeCl₄ und die Kristallstruktur einer metastabilen Modifikation von SeCl₄ / Phase Relations in the System Se-SeCl₄ and the Crystal Structure of a Metastable Modification of SeCl₄

Taming the Oxidative Power of SeO₃ in 1,4-Dioxane, Isolation of Two New Isomers of Mixed-Valence Selenium Oxides, and Two Unprecedented Cyclic Esters of Selenic Acid

Taming the Oxidative Power of SeO₃ in 1,4-Dioxane, Isolation of Two New Isomers of Mixed-Valence Selenium Oxides, and Two Unprecedented Cyclic Esters of Selenic Acid

Sm₃O₂Sm[SeO₃]₄ and Sm₃O₂Cl[SeO₃]₂: A Monoclinic Form of Samarium Oxide Oxoselenate(IV) and a Samarium Oxide Chloride Oxoselenate(IV) both with ¹_∞{[O₂Sm₃]⁵⁺} Chains