Chloroselenate(IV): Darstellung, Struktur und Eigenschaften von [As(C6H5)4]2Se2Cl10 und [As(C6H5)4]Se2Cl9

Krebs, Bernt; Rieskamp, N.; Schäffer, Andreas

doi:10.1002/zaac.19865320117

Cited by 24 publications

(8 citation statements)

References 31 publications

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“…Compound B (refinement in C2/c)' 2.590(8) Cl(1)-Te-Cl(l a) 2.372 (7) Cl(1)-Te-Cl(2) 2.573 (12) Cl(1)-Te-Cl(2a) 2.461 (12) Cl(1 a)-Te-Cl(2) 2.50 (9) Cl(1 a)-Te-Cl(2a) 1.869 (15) Cl (2)-Te-Cl(2a) 1.581 (15) 0-Te-Cl(1) 0.387 (16) 0-Te-Cl(1 a) 3.520 (3) 0-Te-Cl(2) 3.531 (3) 0-Te-Cl(2a) 3.062 (9) Te-0-Cl(2b) 2.967 (17) 0-Te-O(a) 3.084 (14) C1 ( (13) Cl(2)-Te-Cl(2A) 3.508 (14) 0-Te-Cl(1) 3.554 (10) 0-Te-Cl(1 A) 3.508 (9) 0-Te-Cl(2) 3.526 (13) 0-Te-Cl(2A) 3.032 (9) Te-0-Cl(2Ac) 2.955 (19) Cl ( For personal use only. (4) Cl ( (C) (A) in &Hallo2"-, &Hal;-.…”

Section: Crystal Structuresmentioning

confidence: 99%

Crystal structures of (n-Pr₄N)₂SnCl₆, (n-Pr₄N)[TeCl₄(OH)], (n-Pr₄N)₂[Te₂Cl₁₀] (nominal), and (n-Pr₄N)₂[Se₂O₂Cl₆], with observations on Z₂L₁₀²ⁿ⁻ and Z₂L₈²⁻ dimers in general

James¹,

Knop²,

Cameron³

1992

Can. J. Chem.

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This paper is dedicated to Professor Kurt Dehnicke on the occasion of his 60th birthday MARGARET ANN JAMES, OSVALD KNOP, and T. STANLEY CAMERON. Can. J. Chem. 70, 1795Chem. 70, (1992. anion. The actual composition of the centrosymmetric p2-dimer in C is Te2Cls(Cl, OH)!-, the replacement of C1 by OH being at the axial ligand positions of the TeC1,-halves of the dimer. In the centrosymmetric p 2 -~e 2 0 2~1 2 -dimer in D the Se-0 bonds are perpendicular to the Se(Cl),Se bridge plane and trans to the presumed lone-electron pairs on the Se atoms. It is shown that the Z-Hal bonds in the known centrosymmetric homoligand p2-&~al,,2"-(Z = Se, Te) and p,-&~al:-(Z = As, Sb, Bi) as well as in the p 2 -~e 2~2~a 1 2 -dimers exhibit a uniform stereochemistry, in which the d(Z-Hal) bond lengths in pairs of opposing bonds trans to each other are consistently related by the trans effect (TE). Empirical quantification of Te for the Se and Te dimers is exploited to authenticate the composition of the dimer in situations where the nature of the ligand is in doubt (in the present case on partial hydrolysis). The asymmetry of the Z(Hal),Z double bridge is examined in relation to the overall stereochemistry of the dimer. Also examined are circumstances that may lead to the occurrence, in a crystal, of a &~al,,2"-dimer on the one hand and of a discrete ZHa1,"-monomer on the other, in situations which otherwise are chemically closely similar. TLS analysis of the thermal motion is used to judge the strength of association of the two monomer halves in a k-dimer, with results that are important when correcting bond lengths for the effects of thermal motion. A variety of general observations on p,-dimers in crystals is proffered for good measure. On exploite une quantification empirique du TE pour les dimkres du Se et du Te pour authentifier la composition de dimkres dans des situations oh la nature du ligand n'est pas certaine (dans le cas examine ici, il s'agit du produit d'hydrolyse partielle). On a examine I'asymCtrie du double pont Z(Hal)2Z en rapport avec la stCrCochimie globale du dimkre. On a aussi examine les circonstances qui peuvent conduire, dans un cristal, & la presence d'une part d'un dimkre ~,~a l , , 2 " -et d'un monomkre ZHa1,"-individuel, dans des conditions chimiques qui sont par ailleurs chimiquement semblables. On a utilisC l'analyse TLS du mouvement thermique pour juger de la force de l'association de deux parties de monomeres dans un dimkre-p,; les resultats sont importants pour coniger les longueurs de liaison pour les effets des mouvements thermiques. On prksente aussi un nombre d'observations gCnCrales sur dimeres-p2 dans les cristaux.[Traduit par la redaction]In the course of investigating the actual geometry of tallographic studies showed three of them (see title) to conoctahedral 12-and 14-valence-electron ML,"-anions in tain uncommon Se(1V)-and Te(1V)-derived anions and thus crystals (cf. ref. 1) we obtained, serendipitously, several tetrato merit closer investigation. The crystal structures of these n-propy...

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Section: Crystal Structuresmentioning

confidence: 99%

Crystal structures of (n-Pr₄N)₂SnCl₆, (n-Pr₄N)[TeCl₄(OH)], (n-Pr₄N)₂[Te₂Cl₁₀] (nominal), and (n-Pr₄N)₂[Se₂O₂Cl₆], with observations on Z₂L₁₀²ⁿ⁻ and Z₂L₈²⁻ dimers in general

James¹,

Knop²,

Cameron³

1992

Can. J. Chem.

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“…It is rather expectable, considering that these elements in oxidation state 4 + form almost exclusively mononuclear halide complexes (excluding Te [30,31] ). Attempting to overcome this threshold, we focused on Se IV which readily forms polynuclear anionic halides [35][36][37][38][39] and oxyhalides. [40][41][42] Our attempt was successful: bubbling Cl 2 through HCl solution of SeO 2 and TMA chloride (see Supporting Information for experimental procedure), we isolated single crystals of 1 suitable for X-ray diffractometry (see Supporting Information).…”

mentioning

confidence: 99%

Oxochloroselenate(IV) with Incorporated {Cl₂}: The Case of Strong Cl⋅⋅⋅Cl Halogen Bonding

Usoltsev

Korobeynikov

Kolesov

et al. 2021

Chemistry A European J

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Reaction of SeO 2 , tetramethylammonium (TMA) chloride, aqueous HCl and Cl 2 yields oxochloroselenate with incorporated Cl 2 units, TMA 3 {[Se 2 O 2 Cl 7 ](Cl 2 )}. The main feature of this compound is the strong (up to 3.5 kcal mol À 1 , according to DFT calculations) Cl•••Cl bonding, which is also detected by Raman spectroscopy.Ability of halide complexes (hetero-or, more commonly, homoleptic) to form inclusion compounds with di-or polyhalogens was noticed decades ago. [1][2][3] Surprisingly, this feature was not systematically studied for years (probably with the only exception -in 1960s and 1970s, Jacobson et al. presented [4][5][6][7] numerous examples of bromoantimonates with {Br 2 } or (Br 3 ) À units incorporated in solid state, as followed from XRD data). After a long pause, this area experiences revival nowadays (it can be related to, on one hand, development of chemistry of polyhalogens [8][9][10] itself [11][12][13][14][15][16][17][18][19][20] and, on another, increasing attention on halogen bonding [21,22] ). In last years, it was shown that formation of "polyhalogenhalometalates" is possible for numerous elements, such as Bi, [23][24][25] Cu, [26] Sn, [27] Pt, [28] Zn, [29] Te [30][31][32] etc. Most of these compounds contain polyiodides (these compounds are of interest due to their lower optical band gaps, [23,24] assuming their potential applicability in photovoltaics) or, less commonly, -bromides; meanwhile, complexes with "trapped" {Cl 2 } are yet very rare. The earlier single report describing Cat 2 {[MCl 6 ](Cl 2 )] (M=Sn IV and Pd IV[2] remained generally overlooked; very recently, we showed [33] that such complexes can be also prepared for Te IV[33] and Pb IV , [34] demonstrating unusually high thermal stability in the case of cat = TMA + .Despite it can be seen now that dichloro-chlorometalates can be prepared for, at least, four elements (Sn, [2,34] Te, [33] Pb [34] and Pd [2] ), their structural chemistry is yet not rich: all known structures are based on [M IV Cl 6 ] 2À building blocks which are

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“…Chloroselenates with Di-and Tetravalent Selenium: 77 Se-NMR-Spectra, Syntheses, and Crystal Structures of (PPh 4 ) 2 SeCl 6´2 CH 2 Cl 2 , (NMe 3 Ph) 2 SeCl 6 , (K-18-crown-6) 2 SeCl 6´2 CH 3 [12], obwohl die Se 2 Cl 9 ± -Ionen gleich aufgebaut sind. Es gibt allerdings auffa È llige Unterschiede bei den Se±Cl-Bindungsla È ngen zu den verbru È ckenden Chloratomen der beiden fla È chenverknu È pften Oktaeder.…”

unclassified

“…Es gibt allerdings auffa È llige Unterschiede bei den Se±Cl-Bindungsla È ngen zu den verbru È ckenden Chloratomen der beiden fla È chenverknu È pften Oktaeder. Im Arsonium-Salz reichen sie von 258,4 bis 272,1(5) pm (Mittelwert 265,2 pm), wa È hrend sie im (7) 4463(4) 11200(4) 8430(2) Cl (8) 7532 (4) 8345(3) 8357(2) Cl (9) 3578(5) 8305(4) 8599(2) Cl (10) 6153 (4) (2) 1334 (1) 508 (1) 1893(1) Se (3) 3716 (2) 577 (1) 3213(1) Cl (1) 1998 (4) ±2184 (2) 3018(2) Cl (2) 3375 (4) ±2135 (2) 2048(2) Cl (3) ±139 (3) 918 (2) 1998 (2) Cl (4) 1040 (3) (7) 3731(4) 4770(6) 7562(4) Cl (8) 2500(4) 3319(7) 7706(4) Cl (9) 2248(3) ±788(6) 7189(4) Cl (10) 3394(4) ±2398(5) 7656(4) Cl (11) 4391(4) ±857(7) 5235(4) Cl (12) 2967(4) ±1429 (6) …”

unclassified

“…2 getroffenen Zuordnungen stu È tzen sich auf die angegebenen Literaturdaten. Die Zuordnung d = 1411 fu È r das SeCl 6 2± -Ion folgt auch daraus, daû dieses Signal das einzige ist, wenn SeCl 4 mit u È berschu È ssigem Cl ± versetzt wurde, das Gleichgewicht somit zugunsten des SeCl 6 2± verschoben ist[12]. Auûerdem ist dieses Signal recht schmal (16 Hz), wa È hrend sonst u È berwiegend breitere Signale auftreten, die fu È r Austauschreaktionen sprechen.…”

unclassified

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Chloroselenate mit zwei- und vierwertigem Selen:77Se-NMR-Spektren, Synthese und Kristallstrukturen von (PPh4)2SeCl6 · 2 CH2Cl2, (NMe3Ph)2SeCl6, (K-18-Krone-6)2SeCl6 · 2 CH3CN, PPh4Se2Cl9, (NEt4)2Se2Cl10, (PPh4)2Se3Cl8 · CH2Cl2 und (PPh4)2Se4Cl12 · CH2Cl2

Czado

Maurer

Müller

1998

Z. anorg. allg. Chem.

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Die Titelverbindungen wurden durch Reaktionen von Selen und Selentetrachlorid mit PPh4Cl, NEt4Cl, NMe3PhCl oder (K‐18‐Krone‐6)Cl in Dichlormethan oder Acetonitril hergestellt. (PPh4)2Se3Cl8 · CH2Cl2 entstand auch aus GeSe, PPh4Cl und Chlor in Acetonitril. Die 77Se‐NMR‐Spektren der Lösungen zeigen das Vorliegen von dynamischen Gleichgewichten, bei denen je nach Zusammensetzung vor allem die Spezies SeCl2, SeCl4, Se2Cl2, SeCl62–, Se2Cl62– und/oder Se2Cl102– vorherrschen. Aus Lösungen von AsCl3 und (PPh4)2Se4 in Acetonitril wurde (PPh4)2Se2Cl6 durch Chlorierung mit Cl2 oder PPh4AsCl6 erhalten, bei Chlorierung mit SOCl2 war das Produkt (PPh4)2As2Se4Cl12. Nach den Kristallstrukturanalysen haben die Ionen SeCl62–, Se2Cl9– und Se2Cl102– die bekannten Strukturen mit oktaedrischer Koordination der Se‐Atome. Das Se3Cl82–‐Ion ist wie das Se3Br82–‐Ion aufgebaut, d. h. drei SeCl2‐Moleküle, die über zwei Cl–‐Ionen assoziiert sind. (PPh4)2Se4Cl12 · CH2Cl2 ist isotyp zum gleichartigen Bromoselenat und enthält Anionen, in denen drei SeCl2‐Moleküle an ein SeCl62–‐Ion angelagert sind, wobei eine eigenartige Se–Se‐Wechselwirkung auftritt.

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Chloroselenate(IV): Darstellung, Struktur und Eigenschaften von [As(C₆H₅)₄]₂Se₂Cl₁₀ und [As(C₆H₅)₄]Se₂Cl₉

Cited by 24 publications

References 31 publications

Crystal structures of (n-Pr₄N)₂SnCl₆, (n-Pr₄N)[TeCl₄(OH)], (n-Pr₄N)₂[Te₂Cl₁₀] (nominal), and (n-Pr₄N)₂[Se₂O₂Cl₆], with observations on Z₂L₁₀²ⁿ⁻ and Z₂L₈²⁻ dimers in general

Crystal structures of (n-Pr₄N)₂SnCl₆, (n-Pr₄N)[TeCl₄(OH)], (n-Pr₄N)₂[Te₂Cl₁₀] (nominal), and (n-Pr₄N)₂[Se₂O₂Cl₆], with observations on Z₂L₁₀²ⁿ⁻ and Z₂L₈²⁻ dimers in general

Oxochloroselenate(IV) with Incorporated {Cl₂}: The Case of Strong Cl⋅⋅⋅Cl Halogen Bonding

Chloroselenate mit zwei- und vierwertigem Selen:77Se-NMR-Spektren, Synthese und Kristallstrukturen von (PPh4)2SeCl6 · 2 CH2Cl2, (NMe3Ph)2SeCl6, (K-18-Krone-6)2SeCl6 · 2 CH3CN, PPh4Se2Cl9, (NEt4)2Se2Cl10, (PPh4)2Se3Cl8 · CH2Cl2 und (PPh4)2Se4Cl12 · CH2Cl2

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Chloroselenate(IV): Darstellung, Struktur und Eigenschaften von [As(C6H5)4]2Se2Cl10 und [As(C6H5)4]Se2Cl9

Cited by 24 publications

References 31 publications

Crystal structures of (n-Pr4N)2SnCl6, (n-Pr4N)[TeCl4(OH)], (n-Pr4N)2[Te2Cl10] (nominal), and (n-Pr4N)2[Se2O2Cl6], with observations on Z2L102n− and Z2L82− dimers in general

Crystal structures of (n-Pr4N)2SnCl6, (n-Pr4N)[TeCl4(OH)], (n-Pr4N)2[Te2Cl10] (nominal), and (n-Pr4N)2[Se2O2Cl6], with observations on Z2L102n− and Z2L82− dimers in general

Oxochloroselenate(IV) with Incorporated {Cl2}: The Case of Strong Cl⋅⋅⋅Cl Halogen Bonding

Chloroselenate mit zwei- und vierwertigem Selen:77Se-NMR-Spektren, Synthese und Kristallstrukturen von (PPh4)2SeCl6 · 2 CH2Cl2, (NMe3Ph)2SeCl6, (K-18-Krone-6)2SeCl6 · 2 CH3CN, PPh4Se2Cl9, (NEt4)2Se2Cl10, (PPh4)2Se3Cl8 · CH2Cl2 und (PPh4)2Se4Cl12 · CH2Cl2

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Chloroselenate(IV): Darstellung, Struktur und Eigenschaften von [As(C₆H₅)₄]₂Se₂Cl₁₀ und [As(C₆H₅)₄]Se₂Cl₉

Crystal structures of (n-Pr₄N)₂SnCl₆, (n-Pr₄N)[TeCl₄(OH)], (n-Pr₄N)₂[Te₂Cl₁₀] (nominal), and (n-Pr₄N)₂[Se₂O₂Cl₆], with observations on Z₂L₁₀²ⁿ⁻ and Z₂L₈²⁻ dimers in general

Crystal structures of (n-Pr₄N)₂SnCl₆, (n-Pr₄N)[TeCl₄(OH)], (n-Pr₄N)₂[Te₂Cl₁₀] (nominal), and (n-Pr₄N)₂[Se₂O₂Cl₆], with observations on Z₂L₁₀²ⁿ⁻ and Z₂L₈²⁻ dimers in general

Oxochloroselenate(IV) with Incorporated {Cl₂}: The Case of Strong Cl⋅⋅⋅Cl Halogen Bonding