Solvothermal synthesis of [Ni(C4H13N3)2]2Sb4S8: the first compound with a cyclic [Sb4S8]4− anion

Bensch, Wolfgang; Näther, Christian; Stähler, Ralph

doi:10.1039/b009583o

Cited by 83 publications

(41 citation statements)

References 23 publications

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“…1 a- (Table 1) with NϪNiϪN angles ranging from 80.2(1) and 104.6(1)°. Angles and distances are comparable with those reported in the literature [7,8,10]. We note that dien complexes of transition metal ions have been known for a long time [11] and the geometric isomers of the cations were intensively studied [12].…”

Section: Resultssupporting

confidence: 75%

Solvothermal Synthesis and Crystal Structure of the New Layered Thioantimonate(III) [Ni(C4H13N3)2]9Sb22S42 · 0.5H2O: Interconnection of the SbS3, SbS4, and SbS5 Primary Building Units Yielding the Very Large Sb30S30 HeteroringDedicated to Professor Welf Bronger on the Occasion of his 70th Birthday

Stähler

Bensch

2002

Z. anorg. allg. Chem.

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The novel thioantimonate(III) [Ni(dien) 2 ] 9 Sb 22 S 42 ·0.5H 2 O was synthesised under solvothermal conditions by reacting elemental Ni, Sb and S in an aqueous solution of diethylenetriamine (dien) (80%). The compound crystallises in the triclinic space group P1, a ϭ 8.997(2) Å , b ϭ 15.293(3) Å , c ϭ 34.434(7) Å , α ϭ 85.51(3)°, β ϭ 84.16(3)°, γ ϭ 83.54(3)°, V ϭ 4672.7 (16) Å 3 , Z ϭ 1. The layered 2 ϱ [Sb 22 S 42 18Ϫ ] anion in [Ni(dien) 2 ] 9 Sb 22 S 42 · 0.5H 2 O is composed of nine SbS 3 trigonal pyramids, one SbS 4 and one SbS 5 unit. The interconnection of these units by sharing common S atoms yields Sb-S heterorings of different sizes. Besides the Solvothermale Synthese und Kristallstruktur des neuen schichtartigen Thioantimonats(III) [Ni(C 4 H 13 N 3 ) 2 ] 9 Sb 22 S 42 · 0,5H 2 O: Verknüpfung der primären SbS 3 -, SbS 4 -und SbS 5 -Baueinheiten zu einem sehr großen Sb 30 S 30 -Heteroring Inhaltsübersicht. Das neue Thioantimonat(III) [Ni(dien) 2 ] 9 Sb 22 S 42 · 0.5H 2 O wurde unter solvothermalen Bedingungen aus elementarem Ni, Sb und S in einer 80%igen Diethylentriamin (dien) Lösung hergestellt. Die Verbindung kristallisiert in der triklinen Raumgruppe P1 mit a ϭ 8,997(2) Å , b ϭ 15,293(3) Å , c ϭ 34,434(7) Å , α ϭ 85,51(3)°, β ϭ 84,16(3)°, γ ϭ 83,54(3)°, V ϭ 4672,7 (16) Å 3 , Z ϭ 1. Das 2 ϱ [Sb 22 S 42 18Ϫ ] Anion in [Ni(dien) 2 ] 9 Sb 22 S 42 · 0.5H 2 O wird aus neun SbS 3 trigonalen Pyramiden, einer SbS 4 -und einer SbS 5 -Einheit aufgebaut. Die Verknüpfung dieser Einheiten über gemeinsame Schwefelatome führt zur Ausbildung von Sb-S-Hetero-

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Section: Resultssupporting

confidence: 75%

Solvothermal Synthesis and Crystal Structure of the New Layered Thioantimonate(III) [Ni(C4H13N3)2]9Sb22S42 · 0.5H2O: Interconnection of the SbS3, SbS4, and SbS5 Primary Building Units Yielding the Very Large Sb30S30 HeteroringDedicated to Professor Welf Bronger on the Occasion of his 70th Birthday

Stähler

Bensch

2002

Z. anorg. allg. Chem.

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“…The SbϪS distances in the Sb 3 S 3 ring are similar to those reported for extended thioanti- 2.3310(9) Sb(1)ϪS (3) 2.4756(10) Sb (1)ϪS (4) Sb (1)ϪS (1) 2.4838(9) Sb(2)ϪS (5) 2.3333(9) Sb(2)ϪS (2) 2.4617(9) Sb (2)ϪS (1) 2.4623(9) Sb(3)ϪS (6) 2.3216(9) Sb(3)ϪS (3) 2.4702(9) Sb(3)ϪS (2) 2.4774(9) S(4)ϪSb (1)ϪS (3) 93.47 (3) S (4)ϪSb (1)ϪS (1) 98.40(3) S(3)ϪSb (1)ϪS (1) 99.56 (3) S (5)ϪSb (2)ϪS (2) 102.22(3) S(5)ϪSb (2)ϪS (1) 99.00 (3) S (2)ϪSb (2)ϪS (1) 98.00(3) S(6)ϪSb (3)ϪS (3) 104.70 (3) S (6)ϪSb (3)ϪS (2) 101.46(3) S(3)ϪSb (3)ϪS (2) 97.68 (3) Sb (2)ϪS (1)ϪSb (1) 102.03(3) Sb (2)ϪS (2)ϪSb (3) 93.44 (3) Sb (3)ϪS (3)ϪSb (1) (Table 2). [8,19,20] Cations and anions are packed in such a way that both form individual stacks parallel to the a axis ( …”

Section: Resultsmentioning

confidence: 99%

[Ni(C₄H₁₃N₃)₂]₃(Sb₃S₆)₂: The First Structure Containing Isolated Heterocyclic [Sb₃S₆]³⁻ Anions

et al. 2004

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“…Despite several efforts undertaken by different groups we are far from a deeper understanding of the reaction mechanisms occurring under solvothermal conditions [26]. The following example should illustrate the main problems of the solvothermal approach: syntheses performed with Sb, S, Ni and diethylenetriamine as structure director leads to a couple of compounds like [Ni(dien) 2 ] 2 Sb 4 S 8 [27], [Ni(dien) 2 ] 2 Sb 4 S 9 [28] or [Ni(dien) 2 ] 3 (Sb 3 S 6 ) 2 [29] under almost identical conditions.…”

Section: Introductionmentioning

confidence: 99%

Solvothermal Syntheses of Two New Thiostannates and an In‐Situ Energy Dispersive X‐ray Scattering Study of Their Formation

2009

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Two new thiostannates (DBNH) 2 Sn 3 S 6 (1) and (DBNH) 2 Cu 6 Sn 2 S 8 (2) were synthesized under solvothermal conditions applying Cu, Sn, S and DBN (DBN = 1,5-diazabicyclo[4.3.0]non-7-ene). Compound 1 is a rare example of a mixed-valent thiostannate. The Sn(II) species appears in the rare trigonal-pyramidal environment whereas Sn(IV) is in a tetrahedral coordination. The chain-anion is composed of alternating Sn 3 S 4 semi-cubes and Sn 2 S 2 rings. The structure of 2 consists of undulated anionic layers and amine molecules between the layers. The layers may be viewed as a heteroatom 6 3 graphene layer constructed by condensed CuS 3 triangles and SnS 4 tetrahedra. The two thiostannates coexist which was investigated with in-situ energy dispersive X-ray scattering under real solvothermal conditions. Prior to the formation of 1 and 2 a crystalline intermediate appears which disappears after 60 min.Then reflections of 2 start to grow and reflections of 1 occur some time later. The appearance of a thiostannate(IV) followed by the crystallization of a mixed-valent thiostannate(II,IV) suggests complex redox reactions occurring under the solvothermal conditions. Syntheses without Cu in the reaction slurry lead to the formation of 1 within a very short time. The results of the in-situ studies clearly indicate that the presence of Cu species in solution retards the nucleation and crystallization of 1. The crystalline intermediate was quenched with ex-situ experiments. All syntheses performed with this intermediate do not lead to the crystallization of 1 or 2, i.e., there is no direct relation between these three crystalline compounds. The spectroscopic and thermal properties of 1 and 2 are also discussed.

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Solvothermal synthesis of [Ni(C4H13N3)2]2Sb4S8: the first compound with a cyclic [Sb4S8]4− anion

Cited by 83 publications

References 23 publications

Solvothermal Synthesis and Crystal Structure of the New Layered Thioantimonate(III) [Ni(C4H13N3)2]9Sb22S42 · 0.5H2O: Interconnection of the SbS3, SbS4, and SbS5 Primary Building Units Yielding the Very Large Sb30S30 HeteroringDedicated to Professor Welf Bronger on the Occasion of his 70th Birthday

Solvothermal Synthesis and Crystal Structure of the New Layered Thioantimonate(III) [Ni(C4H13N3)2]9Sb22S42 · 0.5H2O: Interconnection of the SbS3, SbS4, and SbS5 Primary Building Units Yielding the Very Large Sb30S30 HeteroringDedicated to Professor Welf Bronger on the Occasion of his 70th Birthday

[Ni(C₄H₁₃N₃)₂]₃(Sb₃S₆)₂: The First Structure Containing Isolated Heterocyclic [Sb₃S₆]³⁻ Anions

Solvothermal Syntheses of Two New Thiostannates and an In‐Situ Energy Dispersive X‐ray Scattering Study of Their Formation

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Solvothermal synthesis of [Ni(C4H13N3)2]2Sb4S8: the first compound with a cyclic [Sb4S8]4− anion

Cited by 83 publications

References 23 publications

Solvothermal Synthesis and Crystal Structure of the New Layered Thioantimonate(III) [Ni(C4H13N3)2]9Sb22S42 · 0.5H2O: Interconnection of the SbS3, SbS4, and SbS5 Primary Building Units Yielding the Very Large Sb30S30 HeteroringDedicated to Professor Welf Bronger on the Occasion of his 70th Birthday

Solvothermal Synthesis and Crystal Structure of the New Layered Thioantimonate(III) [Ni(C4H13N3)2]9Sb22S42 · 0.5H2O: Interconnection of the SbS3, SbS4, and SbS5 Primary Building Units Yielding the Very Large Sb30S30 HeteroringDedicated to Professor Welf Bronger on the Occasion of his 70th Birthday

[Ni(C4H13N3)2]3(Sb3S6)2: The First Structure Containing Isolated Heterocyclic [Sb3S6]3− Anions

Solvothermal Syntheses of Two New Thiostannates and an In‐Situ Energy Dispersive X‐ray Scattering Study of Their Formation

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[Ni(C₄H₁₃N₃)₂]₃(Sb₃S₆)₂: The First Structure Containing Isolated Heterocyclic [Sb₃S₆]³⁻ Anions