Polysulfonylamine, Clxxv [1]. Intermolekulare Wechselwirkungen In Kristallinen Di(Organosulfonyl)Aminen. Teil 3 [2]. Supramolekulare Strukturen Von Di(Benzolsulfonyl)Amin, (Benzolsulfonyl)(Methansulfonyl)Amin Und Di(Ethansulfonyl)Amin

Na[Ag{N(SO 2 ϪC 6 H 4 Ϫ4-F) 2 } 2 ] (monoclinic, C2/c, ZЈ ϭ 1/2) is the first heterobimetallic representative in a well-documented class of layered inorgano-organic solids where the inorganic component is comprised of metal cations and coordinating N(SO 2 ) 2 groups and the outer regions are formed by the aromatic rings of the di(arenesulfonyl)amide entities, which adopt a folded conformation approximating to mirror symmetry. The inversion-symmetric bis(amido)argentate unit of the novel compound displays an exactly linear NϪAgϪN core and short AgϪN bonds of 217.55(17) pm (at Ϫ140°C); the coordination number of the silver 1 Einleitung Metall(I)-di(arensulfonyl)amide des allgemeinen Typs MN(SO 2 ϪAr) 2 иn H 2 O (Ar ϭ Phenyl oder substituiertes Phenyl, n Ն 0) kristallisieren vorzugsweise in lamellaren Schichtverbänden [3]. Innerhalb der Schichten bilden Nund/oder O-koordinierte Kationen zusammen mit N(SO 2 ) 2 -Gruppen und eventuell vorhandenen Wassermolekülen eine polare anorganische Lamelle, aus welcher die lipophilen Arylgruppen beidseitig herausragen. Da die N(SO 2 C) 2 -Gerüste in der Regel gefaltete Konformationen [4a] mit synperiplanarer Torsion τ(CϪS···SЈϪCЈ) und annähernder Spiegelsymmetrie aufweisen, befinden sich die Arylringe eines jeden Anions in paarig-gestapelter Anordnung auf der 1265 ion is extended to 2 ϩ 6 by four internal and two external Ag···O secondary interactions. The polar lamella is constructed from rows of Na ϩ ions located on twofold axes, alternating with bis(amido)argentate strands reinforced by Ag···O interactions and weak CϪH···O hydrogen bonds; Na ϩ is embedded in an O 6 environment. Adjacent layers are cross-linked via short CϪH···FϪC contacts suggestive of weak hydrogen bonding enhanced by cooperativity.

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Strukturen ionischer Di(arensulfonyl)amide. 8. Natrium‐bis[di(4‐fluorbenzolsulfonyl)amido‐N]argentat: Ein Heterobimetallkomplex mit lamellarer Schichtstruktur und kurzen Zwischenschichtkontakten C–H···F–C

Zerbe

Jones

Blaschette

2007

Zeitschrift anorg allge chemie

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Polysulfonylamine. CLXXXIII. Neues aus der Festkörperchemie der Di(arensulfonyl)amine: Silber(I)‐di(4‐iod‐ benzolsulfonyl)amid, eine Schichtverbindung mit strukturdirigierenden Ag–I–C‐Motiven, und Di(4‐fluorbenzolsulfonyl)amin‐Monohydrat, eine Säulenstruktur mit intracolumnaren Wasserketten und intercolumnaren Wasserstoffbrücken C–H···F–C

Wölper¹,

Kandula²,

Graumann³

et al. 2008

Zeitschrift anorg allge chemie

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Polysulfonylamines. CLXXXIII. Novel Solid‐State Aspects of Di(arenesulfonyl)amines: Silver(I) Di(4‐iodobenzenesulfonyl)amide, a Layer Compound Displaying Structure‐Directing Ag–I–C Motifs, and Di(4‐fluorobenzenesulfonyl)amine Monohydrate, a Column Structure Exhibiting Intracolumnar Water Chains and Intercolumnar C–H···F–C Hydrogen Bonds Low‐temperature X‐ray structures are reported for (4‐I–C6H4SO2)2NAg (1, triclinic, $P{\bar 1}$, Z′ = 1) and (4‐F–C6H4SO2)2NH·H2O (2, orthorhombic, Pna21, Z′ = 2). Whereas metal di(arenesulfonyl)amides usually display folded anions (C–S···S′–C′ synperiplanar) and crystallize in lamellar layers, compound 1 has an extended anion (C–S···S′–C′ antiperiplanar) and forms non‐lamellar striated layers in which the ions are connected by Ag–N/Ag–O bonds in one dimension and by Ag–I–C interactions, C–I···O halogen bonds and weak π/π ring interactions in the other dimension. The silver ion adopts a trigonal‐bipyramidal pentacoordination comprising two long axial Ag–O bonds (259 and 261 pm), one short Ag–N bond (228 pm) and two structure‐determining Ag–I bonds (289 and 294 pm, Ag–I–C 107 and 109°). An analysis of Ag···I–C contacts < 340 pm extracted from the Cambridge Structural Database (25 structures, 63 contacts) reveals that the Ag–I–C angles lie between 90 and 110° for contacts < 300 pm, whereas for longer interactions, the directionality rapidly becomes weaker; this result is in keeping with the electrophile/nucleophile model for interactions involving halogen atoms bonded to carbon. In the structure of compound 2, a dimer of two independent water molecules is repeated via glide planes to give a chain in which water 1 acts as a difunctional hydrogen bond donor and water 2 as a difunctional acceptor. The extended disulfonylamine molecules are connected to water 1 by N–H···O(w), to water 2 by O(w)–H···O=S bonds. The resulting supramolecular polymer is a square column that is reinforced by C–H···O=S hydrogen bonds and π/π interactions and bears four one‐dimensional sets of fluorine atoms at the vertices. Dense packing of these columns causes all the fluorine atoms to segregate into parallel tunnels and to form short C–H···F–C intercolumnar contacts strongly suggestive of weak hydrogen bonding (H···F 240–250 pm, C···F 328–346 pm, C–H···F 137–148°).

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Polysulfonylamine. CLXXXIV. Kristallstrukturen molekularer Triphenylphosphangold(I)‐di(4‐X‐benzolsulfonyl)‐amide: Isomorphie und dichte Packung (X = Me, F, Cl, NO₂) vs. struktursteuernde Halogenbrücken C–X···Au/O (X = Br, I)

Wölper

Piñol

Durán

et al. 2008

Zeitschrift anorg allge chemie

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Polysulfonylamines. CLXXXIV. Crystal Structures of Molecular Triphenylphosphanegold(I) Di(4‐X‐benzenesulfonyl)amides: Isomorphism and Close Packing (X = Me, F, Cl, NO2) vs. Structure‐Determining C–X···Au/O Halogen Bonds (X = Br, I)In order to study the structure‐determining influence that halogen bonding can exert during the course of crystallization, solid‐state structures are compared for two previously reported and four new molecular gold(I) complexes of the type Ph3P–Au–N(SO2–C6H4–4‐X)2, each featuring linear P,N coordination at gold and two phenyl rings with varying p‐substituents X = Me, F, Cl, NO2, Br or I. The compounds were synthesized by reactions of Ph3PAuX (X = Cl or I) with the corresponding silver di(arenesulfonyl)amides, crystallized from dichloromethane, and characterized by low‐temperature X‐ray diffraction. The Me, F, Cl and NO2 congeners are isomorphic and crystallize without solvent inclusion in the chiral orthorhombic space group P212121 (Z′ = 1). These structures are governed by isotropic close packing via three‐dimensional 21 symmetry, incidentally supported by an invariant set of C–H···O=S hydrogen bonds, CH/π interactions and π/π stackings of aromatic rings; in particular, the hard halogen atoms of the fluoro and the chloro homologues are not involved in X···Au, X···O or X···X interactions. The higher homologues, with soft halogen atoms, were obtained as a dichloromethane hemisolvate for X = Br and a corresponding monosolvate for X = I, each triclinic in the centrosymmetric space group $P{\bar 1}$ (Z′ = 1). Here, the primary structural effect is implemented by infinite chains in which translation‐related molecules are connected for the bromo compound by a bifurcated Au···Br(2)···O=S interaction, for the iodo congener by an equivalent Au···I(2)···O=S interaction and a short halogen bond C–I(1)···O=S. The latter bond is stronger than a similar C–Br···O=S interaction and induces a conformational adjustment of the (CSO2)2N group from the normal twofold symmetry in the bromo compound to an energetically unfavourable asymmetric form in the iodo homologue. In both cases, pairs of antiparallel molecular catemers are associated into strands via sixfold phenyl embraces, the strands are stacked to form layers, the solvent molecules are intercalated between adjacent layers, and the crystal packings are reinforced by a number of C–H···O=S hydrogen bonds and interactions of aromatic rings.

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Polysulfonylamine, Clxxv [1]. Intermolekulare Wechselwirkungen In Kristallinen Di(Organosulfonyl)Aminen. Teil 3 [2]. Supramolekulare Strukturen Von Di(Benzolsulfonyl)Amin, (Benzolsulfonyl)(Methansulfonyl)Amin Und Di(Ethansulfonyl)Amin

Cited by 3 publications

References 1 publication

Strukturen ionischer Di(arensulfonyl)amide. 8. Natrium‐bis[di(4‐fluorbenzolsulfonyl)amido‐N]argentat: Ein Heterobimetallkomplex mit lamellarer Schichtstruktur und kurzen Zwischenschichtkontakten C–H···F–C

Strukturen ionischer Di(arensulfonyl)amide. 8. Natrium‐bis[di(4‐fluorbenzolsulfonyl)amido‐N]argentat: Ein Heterobimetallkomplex mit lamellarer Schichtstruktur und kurzen Zwischenschichtkontakten C–H···F–C

Polysulfonylamine. CLXXXIV. Kristallstrukturen molekularer Triphenylphosphangold(I)‐di(4‐X‐benzolsulfonyl)‐amide: Isomorphie und dichte Packung (X = Me, F, Cl, NO₂) vs. struktursteuernde Halogenbrücken C–X···Au/O (X = Br, I)

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Polysulfonylamine, Clxxv [1]. Intermolekulare Wechselwirkungen In Kristallinen Di(Organosulfonyl)Aminen. Teil 3 [2]. Supramolekulare Strukturen Von Di(Benzolsulfonyl)Amin, (Benzolsulfonyl)(Methansulfonyl)Amin Und Di(Ethansulfonyl)Amin

Cited by 3 publications

References 1 publication

Strukturen ionischer Di(arensulfonyl)amide. 8. Natrium‐bis[di(4‐fluorbenzolsulfonyl)amido‐N]argentat: Ein Heterobimetallkomplex mit lamellarer Schichtstruktur und kurzen Zwischenschichtkontakten C–H···F–C

Strukturen ionischer Di(arensulfonyl)amide. 8. Natrium‐bis[di(4‐fluorbenzolsulfonyl)amido‐N]argentat: Ein Heterobimetallkomplex mit lamellarer Schichtstruktur und kurzen Zwischenschichtkontakten C–H···F–C

Polysulfonylamine. CLXXXIV. Kristallstrukturen molekularer Triphenylphosphangold(I)‐di(4‐X‐benzolsulfonyl)‐amide: Isomorphie und dichte Packung (X = Me, F, Cl, NO2) vs. struktursteuernde Halogenbrücken C–X···Au/O (X = Br, I)

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Polysulfonylamine. CLXXXIV. Kristallstrukturen molekularer Triphenylphosphangold(I)‐di(4‐X‐benzolsulfonyl)‐amide: Isomorphie und dichte Packung (X = Me, F, Cl, NO₂) vs. struktursteuernde Halogenbrücken C–X···Au/O (X = Br, I)