Spezielle Alkylammoniumhexachlorometallate. I. Kristallisationsverhalten und Kristallstruktur von Diethylentriammoniumhexachlororhodat, [H3N(CH2)2NH2(CH2)2NH3][RhCl6]

Frank, Walter; Reiß, Guido J.; Kleinwächter, Ingo

doi:10.1002/zaac.19966220428

Cited by 13 publications

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“…1 crystallizes in the triclinic space group P1 h. Figure 1 shows the ionic components with their direct environments, Figure 2 a packing diagram. Bond lengths and angles of the [RhCl 6 ] 3anion 9 and of the 1,6-diammoniohexane cation 10 are as expected (Table 3). Starting from the energy-favored, zigzag chain-like all-trans conformation, the bow-shaped conformer of the diam- monio cation present in 1 is achieved mainly by rotating half the cation 94.9(3)°around the C3-C4 axis.…”

Section: Resultssupporting

confidence: 74%

Alkylammonium Hexachlorometalates. 5.¹ Bis(1,6-diammoniohexane) Tetraaquahydrogen(1+) Hexachlororhodate(III) Dichloride, [H₃N(CH₂)₆NH₃]₂[H₉O₄][RhCl₆]Cl₂: Chain-like [H₉O₄]⁺ Ions Enclosed in the Cavities of a Complex Organic−Inorganic Framework

Frank

Reiß

1997

Inorg. Chem.

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[H3N(CH2)6NH3]2[H9O4][RhCl6]Cl2, obtained from 1,6-diaminohexane and rhodium trichloride in 12 M hydrochloric acid, has been shown by X-ray crystallography to contain chain-like [H9O4]+ ions in the cavities of a complex organic−inorganic framework built up by 1,6-diammoniohexane, hexachlororhodate(3−), and chloride ions. In view of crystal engineering the diammoniohexane ions act as “intelligent” building blocks, because their conformational flexibility enables them to take part in the formation of cavities with exactly the right lengths for the inclusion of the [H9O4]+.

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Section: Resultssupporting

confidence: 74%

Alkylammonium Hexachlorometalates. 5.¹ Bis(1,6-diammoniohexane) Tetraaquahydrogen(1+) Hexachlororhodate(III) Dichloride, [H₃N(CH₂)₆NH₃]₂[H₉O₄][RhCl₆]Cl₂: Chain-like [H₉O₄]⁺ Ions Enclosed in the Cavities of a Complex Organic−Inorganic Framework

Frank

Reiß

1997

Inorg. Chem.

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“…For chloride complexes of some metals with DienH 3 3 + , in which the cation appeared to be strongly fixed in the lattice by hydrogen bonds, the structures were determined from the diffraction experiments performed at room temperature [29][30][31][32][33][34][35]. …”

Section: Resultsmentioning

confidence: 99%

Structure of diethylenetriammonium tetrabromoaurates(III)

2014

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In HAuBr 4 interaction with diethylenetriamine in HBr, new complexes (DienH 3 ) 2 [AuBr 4 ] 3 Br 3 ⋅4H 2 O (I) and (DienH 3 )[AuBr 4 ] 3 ⋅H 2 O (II) (where DienH 3 3 + is protonated diethylenetriamine) are obtained, which are characterized by elemental analysis, single crystal X-ray diffraction, thermogravimetry, and IR spectroscopy. For I, the crystals are triclinic, crystallize in the space group Р-1, a = 7.9717(3) Å, b = 11.0178(4) Å, c = 12.6765(5) Å, α = 75.960(1)°, β = 75.031(1)°, γ = 75.681(1)°, V = 1023.02(7) Å 3 , Z = 2. For II, the crystals are orthorhombic, crystallize in the space group Pnma, unit cell parameters are as follows: a = 4.2981(8) Å, b = 15.394(3) Å, c = 13.402(3) Å, V = 886.7(3) Å 3 , Z = 4. In the literature, there are few works dealing with the study of crystal structures containing complex tetrabromoaurate anions [AuBr 4 ] -, as opposed to the complexes with [AuCl 4 ] -. The crystal structures of K[AuBr 4 ] [1], M[AuBr 4 ]⋅2H 2 O (M = Na [2], K [3]), and mixed M 2 [AuBr 2 ][AuBr 4 ] (M = Rb [4], Cs [5]) complexes were determined. There are data on the structure of complexes, in which different class protonated organic compounds appear as simple cations: (C 10 H 13 N 4 O 5 )[AuBr 4 ]⋅2H 2 O [6], ((C 9 H 6 NCOOH) 2 H)[AuBr 4 ]⋅H 2 O [7], (C 20 H 15 N 2 ) 2 [AuBr 2 ][AuBr 4 ] [8], (C 5 NH 6 )[AuBr 4 ] [9], (C 6 H 10 N 2 )[AuBr 4 ]Br⋅H 2 O [10]. In all studied complexes, the [AuBr 4 ] -anion has a square-planar configuration. In some structures, weak contacts of the gold atom with the bromine atoms of the neighboring complex ions or with the cation atoms were noticed, so that the coordination environment of Au(III) can be described as being 4+1 or 4+2. The same coordination environment of Au(III) was found in the structures of double complex salts (DCSs) with doubly or triply charged complex cations of another metal: [Co(NH 3 ) 6 ][AuBr 4 ]Br 2 [11], [Co(En) 3 ][AuBr 4 ] 2 Br [12], [M(NH 3 ) 5 Br][AuBr 4 ] 2 ⋅H 2 O (M = Ir, Rh) [13]. Completing the square coordination of the gold atom to a tetragonal pyramid or elongated square pyramid has been also found in DCSs containing [AuCl 4 ] -in their composition [11, 14, 15]. It should be noted that substituting chloride by bromide in [AuCl 4 ] -and varying the nature of ligands of the inner coordination sphere of multicharged cations makes it possible to obtain DCSs with different metal ratios. For example, with doubly charged complex cations Ir and Rh, DCSs of the [M(NH 3 ) 5 Cl][AuCl 4 ]Cl⋅nH 2 O (n = 0-2) [16, 17] and [M(NH 3 ) 5 Br][AuBr 4 ] 2 ⋅H 2 O [13] composition were obtained. For triplycharged complex cations Co(III), substituting chloride by bromide in the anion did not influence on the stoichiometry and structural features of the DCSs obtained, while substituting the ammonia in the Co(III) cation by ethylenediamine with the same anion gave the DCSs of different stoichiometry [11,12,14].

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“…For related literature, see: Frank & Bujak (2002); Frank & Graf (2004); , 1997; Frank, Reiss & Kleinwä chter (1996); Gillard et al (1996); Reiss (1996).…”

Section: Related Literaturementioning

confidence: 99%

The inorganic–organic hybrid material triethylenetetrammonium hexachloridorhodate(III) chloride

Hahn¹,

Frank²

2007

Acta Cryst E

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Single crystals of the new title compound [systematic name: 1,4,7,10-tetrazoniadecane hexachloridorhodate(III) chloride], [H3N(CH2)2NH2(CH2)2NH2(CH2)2NH3][RhCl6]Cl, were obtained from the corresponding amine and rhodium trichloride in hydrochloric acid solution by slow crystallization under diffusion-controlled conditions at room temperature. Its solid-state structure is defined by a three-dimensional framework of numerous electrostatic-supported N—H⋯Cl hydrogen bonds between the ionic components of the compound. Within this framework, layered arrangements of the complex ions on one hand and of the protonated amines and chloride ions on the other hand, can be recognized. The octahedral hexachloridorhodate(III) anion resides on a symmetry site, while the triethylenetetrammonium cation and the chloride ion both reside on twofold axes.

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Spezielle Alkylammoniumhexachlorometallate. I. Kristallisationsverhalten und Kristallstruktur von Diethylentriammoniumhexachlororhodat, [H₃N(CH₂)₂NH₂(CH₂)₂NH₃][RhCl₆]

Cited by 13 publications

References 2 publications

Alkylammonium Hexachlorometalates. 5.¹ Bis(1,6-diammoniohexane) Tetraaquahydrogen(1+) Hexachlororhodate(III) Dichloride, [H₃N(CH₂)₆NH₃]₂[H₉O₄][RhCl₆]Cl₂: Chain-like [H₉O₄]⁺ Ions Enclosed in the Cavities of a Complex Organic−Inorganic Framework

Alkylammonium Hexachlorometalates. 5.¹ Bis(1,6-diammoniohexane) Tetraaquahydrogen(1+) Hexachlororhodate(III) Dichloride, [H₃N(CH₂)₆NH₃]₂[H₉O₄][RhCl₆]Cl₂: Chain-like [H₉O₄]⁺ Ions Enclosed in the Cavities of a Complex Organic−Inorganic Framework

Structure of diethylenetriammonium tetrabromoaurates(III)

The inorganic–organic hybrid material triethylenetetrammonium hexachloridorhodate(III) chloride

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Spezielle Alkylammoniumhexachlorometallate. I. Kristallisationsverhalten und Kristallstruktur von Diethylentriammoniumhexachlororhodat, [H3N(CH2)2NH2(CH2)2NH3][RhCl6]

Cited by 13 publications

References 2 publications

Alkylammonium Hexachlorometalates. 5.1 Bis(1,6-diammoniohexane) Tetraaquahydrogen(1+) Hexachlororhodate(III) Dichloride, [H3N(CH2)6NH3]2[H9O4][RhCl6]Cl2: Chain-like [H9O4]+ Ions Enclosed in the Cavities of a Complex Organic−Inorganic Framework

Alkylammonium Hexachlorometalates. 5.1 Bis(1,6-diammoniohexane) Tetraaquahydrogen(1+) Hexachlororhodate(III) Dichloride, [H3N(CH2)6NH3]2[H9O4][RhCl6]Cl2: Chain-like [H9O4]+ Ions Enclosed in the Cavities of a Complex Organic−Inorganic Framework

Structure of diethylenetriammonium tetrabromoaurates(III)

The inorganic–organic hybrid material triethylenetetrammonium hexachloridorhodate(III) chloride

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Spezielle Alkylammoniumhexachlorometallate. I. Kristallisationsverhalten und Kristallstruktur von Diethylentriammoniumhexachlororhodat, [H₃N(CH₂)₂NH₂(CH₂)₂NH₃][RhCl₆]

Alkylammonium Hexachlorometalates. 5.¹ Bis(1,6-diammoniohexane) Tetraaquahydrogen(1+) Hexachlororhodate(III) Dichloride, [H₃N(CH₂)₆NH₃]₂[H₉O₄][RhCl₆]Cl₂: Chain-like [H₉O₄]⁺ Ions Enclosed in the Cavities of a Complex Organic−Inorganic Framework

Alkylammonium Hexachlorometalates. 5.¹ Bis(1,6-diammoniohexane) Tetraaquahydrogen(1+) Hexachlororhodate(III) Dichloride, [H₃N(CH₂)₆NH₃]₂[H₉O₄][RhCl₆]Cl₂: Chain-like [H₉O₄]⁺ Ions Enclosed in the Cavities of a Complex Organic−Inorganic Framework