Thioantimonate(III) anions acting as bridging ligands in neutral transition metal complexes: solvothermal synthesis and characterisation of the two novel compounds [Co(C6H18N4)]2Sb4S8 and [Co(C6H18N4)]2Sb2S5 containing [Sb4S8]4– and [Sb2S5]4– anions

Stähler, Ralph; Bensch, Wolfgang

doi:10.1039/b102273n

Cited by 70 publications

(40 citation statements)

References 25 publications

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“…Such an elongation of a bond can be explained with the so-called trans-effect. The Co(1)-S(1) bond at 2.3701(8) Å is in the range of data published in literature [54,55]. The angles around the Co (1) 2+ cation suggest an appreciable distortion ( Table 2).…”

Section: Resultssupporting

confidence: 63%

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The Effect of Temperature onto the Crystal Structure of Thioantimonates: Solvothermal Syntheses and Crystal Structures of [Co(dien)₂][Co(tren)SbS₄]₂·0.5H₂O and {[Co(tren)]₂[CoSb₂S₆]}·H₂O

Lichte

Lühmann

Näther

et al. 2009

Zeitschrift anorg allge chemie

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HAL is a multi-disciplinary open access archive for the deposit and dissemination of scientific research documents, whether they are published or not. The documents may come from teaching and research institutions in France or abroad, or from public or private research centers. L'archive ouverte pluridisciplinaire HAL, est destinée au dépôt et à la diffusion de documents scientifiques de niveau recherche, publiés ou non, émanant des établissements d'enseignement et de recherche français ou étrangers, des laboratoires publics ou privés. IntroductionIn the past few years we and other groups demonstrated that a large variety of amines are suitable structure directing molecules for the preparation of thioantimonates under solvothermal conditions . A challenge in the field of thioantimonate chemistry is the integration of transition metal ions into the thioantimonate networks. Using mono-, bi-or tridentate amine molecules like methylamine, ethylenediamine or diethylenetriamine (dien) mainly transition metal complexes are formed which are separated from the anionic network [25][26][27][28][29][30][31][32][33][34][35][36][37][38] Results and DiscussionThe two new compounds were obtained in a mixture of dien and tren applying the ratio dien:tren = 2.4:0.6 mL in 1 mL water. Phase pure [Co(dien) 2 ][Co(tren)SbS 4 ] 2 ⋅0.5 H 2 O is formed exclusively at 110 °C whereas mixtures of both compounds were observed at 120 and 130 °C. A series of experiments was performed at 120 and 130 °C varying the reaction time between 3 and 6 d. But in all products a mixture of the two title compounds was obtained. Variation of the ratio of the amines (T = 120 and 130 °C, dien:tren = 2.7:0.3, 2.6:0.4 and 2.5:0.5 with 1 mL H 2 O) and also the absolute amount of the amine in 1 mL water (dien:tren: 1.3:0. 3-anion (Fig. 1). Like in the pseudo-polymorph the Co(1)-N bond in trans position to the Co(1)-S(1) bond is longer (2.247(3) Å) than the remaining Co(1)-N bonds (2.072(3) -2.083(2) Å; Table 1). Such an elongation of a bond can be explained with the so-called trans-effect. The Co(1)-S(1) bond at 2.3701(8) Å is in the range of data published in literature [54,55]. The angles around the Co(1) 2+ cation suggest an appreciable distortion ( Table 2). The Sb-S bond lengths and S-Sb-S angles are typical for a moderately distorted [Sb(V)S 4 ] 3-tetrahedron. The arrangement of the cations and anions in the unit cell is very similar to that observed for the pseudo-polymorphic compound. The shortest O⋅⋅⋅O, O⋅⋅⋅S and O⋅⋅⋅N separations are 3.054, 3.471 and 3.722 Å respectively which are all significantly longer than in [Co(dien) 2 ][Co(tren)SbS 4 ] 2 ⋅4H 2 O and too long for significant H-bonding interactions. Nevertheless, the S atoms join neighbored cations and anions to form layers in he (001) plane (see Table 3). (Fig. 3). Alternatively one may describe the structure as two independent [Co(tren)SbS 3 ] -complexes which are connected by a Co 2+ cation. The Co(1) 2+ and Co(3) 2+ cations are each coordinated by four N atoms of the tren ligand and b...

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Section: Resultssupporting

confidence: 63%

“…The Co (2) 2+ cation is octahedrally surrounded by two tridentate dien ligands in the s-fac-configuration. The Co(2)-N bond lengths between 2.153(4) and 2.192(5) Å are in the range found in other Co amine compound [54][55][56]. The angles around Co (2) 2+ (Table 2) Table 1).…”

Section: Resultsmentioning

confidence: 83%

The Effect of Temperature onto the Crystal Structure of Thioantimonates: Solvothermal Syntheses and Crystal Structures of [Co(dien)₂][Co(tren)SbS₄]₂·0.5H₂O and {[Co(tren)]₂[CoSb₂S₆]}·H₂O

Lichte

Lühmann

Näther

et al. 2009

Zeitschrift anorg allge chemie

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“…2+ ·H 2 O (in 2), correspondingly the dimensions of pores in compounds are 1 (8.1 ϫ 14.7 Å) Ͼ 3 (8.8 ϫ 10.1 Å) Ͼ 2 (7.9 ϫ 8.4 Å), the cations and the water molecules are 85.05(8) S10d-Sb2-S4c 67.30(7) S12d-Sb2-S4c 111.29 (8) S10d-Sb2-S7c 107.10(7) S12d-Sb2-S7c 72.57 (8) S10d-Sb2-59.91(8) S12d …”

Section: Resultsmentioning

confidence: 99%

“…[21][22][23][24][25][26][27][28][29][30][31][32] The solvothermal method was proven to be [ 16 heterorings resulted in an unprecedented framework of the five-atom thick Sb x S y n-layer. In 2, a new member of Sb n S n (n = 2, 3,4,8,16,30,31,32) heterocycles Sb 15 S 15 heteroring has been obtained as the first example. In compound 3, the most particular feature is that when the secondary Sb-S bonds are considered the Sb2 atom becomes sevenfold coordinated.…”

Section: Introductionmentioning

confidence: 98%

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Solvothermal Synthesis, Crystal Structure, and Thermal Stability of Three‐Layered Thioantimonate(III) Complexes: [Ni(C₃H₁₀N₂)₃]Sb₄S₇, [C₄H₁₄N₂]Sb₈S₁₃·H₂O, and [C₆H₁₈N₂]Sb₁₀S₁₆·H₂O

et al. 2007

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Three new thioantimonate(III) complexes [Ni(1,2‐PDA)3]Sb4S7 (1) (1,2‐PDA = 1,2‐propanediamine), [dmenH22+]Sb8S13·H2O (2) (dmen = N,N‐dimethylethylenediamine), and [deenH22+]Sb10S16·H2O (3) (deen = N,N‐diethylethylenediamine), prepared under solvothermal conditions, have been characterized by single‐crystal X‐ray diffraction, elemental analysis, and DTA‐TG measurements. In compound 1, a rectangle‐like Sb16S16 heteroring whose dimensions are about 8.1 × 14.7 Å is observed, this is the largest reported pore in layered thioantimonates to date. Further condensation of the Sb16S16 heterorings resulted in an unprecedented framework of the five‐atom thick SbxSyn– layer. In 2, a new member of SbnSn (n = 2, 3, 4, 8, 16, 30, 31, 32) heterocycles Sb15S15 heteroring has been obtained as the first example. In compound 3, the most particular feature is that when the secondary Sb–S bonds are considered the Sb2 atom becomes sevenfold coordinated.(© Wiley‐VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2007)

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A Strategy for the Preparation of Thioantimonates Based on the Concept of Weak Acids and Corresponding Strong Bases

Anderer

Alarcón

Näther

et al. 2014

Chemistry A European J

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By following a new synthetic approach, which is based on the in situ formation of a basic medium by the reaction between the strong base Sb(V)S4 (3-) and the weak acid H2 O, it was possible to prepare three layered thioantimonate(III) compounds of composition [TM(2,2'-bipyridine)3 ][Sb6 S10 ] (TM=Ni, Fe) and [Ni(4,4'-dimethyl-2,2'-bipyridine)3 ][Sb6 S10 ] under hydrothermal conditions featuring two different thioantimonate(III) network topologies. The antimony source, Na3 SbS4 ⋅ 9 H2 O, undergoes several decomposition reactions and produces the Sb(III) S3 species, which condenses to generate the layered anion. The application of transition-metal complexes avoids crystallization of dense phases. The reactions are very fast compared to conventional hydrothermal/solvothermal syntheses and are much less sensitive to changes of the reaction parameters.

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Thioantimonate(III) anions acting as bridging ligands in neutral transition metal complexes: solvothermal synthesis and characterisation of the two novel compounds [Co(C6H18N4)]2Sb4S8 and [Co(C6H18N4)]2Sb2S5 containing [Sb4S8]4– and [Sb2S5]4– anions

Cited by 70 publications

References 25 publications

The Effect of Temperature onto the Crystal Structure of Thioantimonates: Solvothermal Syntheses and Crystal Structures of [Co(dien)₂][Co(tren)SbS₄]₂·0.5H₂O and {[Co(tren)]₂[CoSb₂S₆]}·H₂O

The Effect of Temperature onto the Crystal Structure of Thioantimonates: Solvothermal Syntheses and Crystal Structures of [Co(dien)₂][Co(tren)SbS₄]₂·0.5H₂O and {[Co(tren)]₂[CoSb₂S₆]}·H₂O

Solvothermal Synthesis, Crystal Structure, and Thermal Stability of Three‐Layered Thioantimonate(III) Complexes: [Ni(C₃H₁₀N₂)₃]Sb₄S₇, [C₄H₁₄N₂]Sb₈S₁₃·H₂O, and [C₆H₁₈N₂]Sb₁₀S₁₆·H₂O

A Strategy for the Preparation of Thioantimonates Based on the Concept of Weak Acids and Corresponding Strong Bases

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Thioantimonate(III) anions acting as bridging ligands in neutral transition metal complexes: solvothermal synthesis and characterisation of the two novel compounds [Co(C6H18N4)]2Sb4S8 and [Co(C6H18N4)]2Sb2S5 containing [Sb4S8]4– and [Sb2S5]4– anions

Cited by 70 publications

References 25 publications

The Effect of Temperature onto the Crystal Structure of Thioantimonates: Solvothermal Syntheses and Crystal Structures of [Co(dien)2][Co(tren)SbS4]2·0.5H2O and {[Co(tren)]2[CoSb2S6]}·H2O

The Effect of Temperature onto the Crystal Structure of Thioantimonates: Solvothermal Syntheses and Crystal Structures of [Co(dien)2][Co(tren)SbS4]2·0.5H2O and {[Co(tren)]2[CoSb2S6]}·H2O

Solvothermal Synthesis, Crystal Structure, and Thermal Stability of Three‐Layered Thioantimonate(III) Complexes: [Ni(C3H10N2)3]Sb4S7, [C4H14N2]Sb8S13·H2O, and [C6H18N2]Sb10S16·H2O

A Strategy for the Preparation of Thioantimonates Based on the Concept of Weak Acids and Corresponding Strong Bases

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The Effect of Temperature onto the Crystal Structure of Thioantimonates: Solvothermal Syntheses and Crystal Structures of [Co(dien)₂][Co(tren)SbS₄]₂·0.5H₂O and {[Co(tren)]₂[CoSb₂S₆]}·H₂O

The Effect of Temperature onto the Crystal Structure of Thioantimonates: Solvothermal Syntheses and Crystal Structures of [Co(dien)₂][Co(tren)SbS₄]₂·0.5H₂O and {[Co(tren)]₂[CoSb₂S₆]}·H₂O

Solvothermal Synthesis, Crystal Structure, and Thermal Stability of Three‐Layered Thioantimonate(III) Complexes: [Ni(C₃H₁₀N₂)₃]Sb₄S₇, [C₄H₁₄N₂]Sb₈S₁₃·H₂O, and [C₆H₁₈N₂]Sb₁₀S₁₆·H₂O