ChemInform Abstract: Synthesis and Crystal Structure of Trichlorosulfonium Nonachlorodititanate(IV), (SCl3)(Ti2Cl9).

Troyanov, S. I.; Рыбаков, В. Б.; Timoshchenko, N. I.; Fokina, Z. A.

doi:10.1002/chin.199042034

Cited by 5 publications

(8 citation statements)

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“…The structural results were very similar to each other (with R 1 = 0.054 and 0.065, respectively) and to the data published recently in [15]. Thus, until now only one polymorph has been detected for Ta 2 Cl 10 .…”

Section: Resultssupporting

confidence: 77%

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Reactions of Chalcogen Oxide Chlorides EOCl2 (E = S, Se) with Group 5 Metal Chlorides

Calderazzo

D'Attoma

Pampaloni

et al. 2001

Z. anorg. allg. Chem.

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The tantalum derivative TaCl 5 (SOCl 2 ), thermally unstable above 290 K, was prepared from Ta 2 Cl 10 and SOCl 2 and studied by X-ray crystallography at 180 K. Tantalum atom is octahedrally coordinated by five chlorides at Ta±Cl distances comprised between 2.32 and 2.36 A Ê and by the oxygen atom of SOCl 2 at the Ta±O distance of 2.34 A Ê . No evidence for the existence of an analogous compound of niobium(V) has been obtained. The halides of Group 5, M 2 Cl 10 , M = Nb, Ta, react with SeOCl 2 to give the solid adducts MCl 5 (SeOCl 2 ) stable at room temperature. The reaction of NbCl 5 (SeOCl 2 ) with SOCl 2 affords [SeCl 3 ][NbCl 6 ] which contains trigonal-pyramidal (SeCl 3 ) + cations with Se±Cl distances of 2.13±2.16 A Ê and octahedral [NbCl 6 ] ± anions (Nb±Cl: 2.27±2.45 A Ê ). A distorted octahedral coordination around the selenium atom is achieved by additional interactions [Se´´´Cl, 2.81±2.98 A Ê ] between selenium and the [NbCl 6 ] ± anion.

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Section: Resultssupporting

confidence: 77%

“…242 K. At variance to niobium, the crystals decompose at room temperature during the isolation procedure (see Experimental) losing SOCl 2 to give Ta 2 Cl 10 . Moreover, addition of heptane to a solution of Ta 2 Cl 10 in SOCl 2 at room temperature gave crystalline Ta 2 Cl 10 .…”

Section: Resultsmentioning

confidence: 99%

Reactions of Chalcogen Oxide Chlorides EOCl2 (E = S, Se) with Group 5 Metal Chlorides

Calderazzo

D'Attoma

Pampaloni

et al. 2001

Z. anorg. allg. Chem.

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“…The structure reveals interactions of the sulfur atom and the chlorine atoms of the anion. Similar interactions were found in [(SCl 3 ) 2 ][OsCl 6 ] ( 106 d ), [SCl 3 ][RuCl 3 (SCl 2 ) 2 ] ( 107 ), and [SCl 3 ][IrCl 4 (SCl 2 ) 2 ] ( 108 ) and the chlorine atoms of the two anions in [SCl 3 ][Ti 2 Cl 9 ] ( 109 ) . Thermal decomposition of [SCl 3 ][AuCl 4 ] ( 3 ) revealed a stepwise degradation which is initiated by the loss of a chlorine molecule at 133 °C to yield [AuCl 3 (SCl 2 )] ( 4 ) (see section 2.1 ) followed by SCl 2 release at 151 °C and the precipitation of AuCl 3 which can be further decomposed to elemental gold by heating the sample up to 333 °C .…”

Section: Sulfur(iv) Compoundssupporting

confidence: 59%

Reactivity of Binary and Ternary Sulfur Halides towards Transition‐Metal Compounds

Dirican

Pfister

Wozniak

et al. 2020

Chemistry A European J

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Binary sulfur fluorides exhibit an interesting reactivity towards transition metal complexes. They open up routes for the generation of sulfur‐containing building blocks. Often ligands with particular properties can be constructed. This includes their ability to transfer sulfur atoms or polysulfide units as well as fluorination reactions. This Minireview provides an insight into the reactivity of the binary and ternary sulfur halides S2Cl2, SCl2, SF4, SF6 and SF5Cl towards transition‐metal compounds.

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“…Indeed, some mononuclear transition metal chalcohalogenides (TMCH) are discussed as volatile precursors for CVD processes; [1] a plenty of cluster complexes with different functionalities (catalysts in hydrorefining of crude oil, X-ray contrast agents, optical limiters) are derived from TMCH compounds of heavy 5-7 group transition metals. [2,3] Unlike transition metals of 5-7 groups, the number of chalcohalide compounds of transition metals of group 4 (Ti, Zr, Hf) is rather limited: to the best of our knowledge, ionic complex [SCl 3 ][Ti 2 Cl 9 ] [4] and Ti 4 Se 9 I 6 [5] are the only ternary TMCH for titanium for to-date. It is also necessary to mention a series of Ti, Zr, Hf molecular complexes [MX 4 {o-C 6 H 4 (CH 2 EMe) 2 }] (M=Ti, Zr; X=Cl, I; E=S, Se) and [MX 4 (Et 2 Se) 2 ] (M=Zr, X=Cl or I; M=Hf, X=I), which were synthesized in [6] as CVD precursors for preparing of the metal dichalcogenides.…”

Section: Introductionmentioning

confidence: 99%

New O‐centered titanium chalcohalide: synthesis and structure of Ti₄O(Se₂)₄Br₆

Poltarak

Комаров

Gayfulin

et al. 2021

Zeitschrift anorg allge chemie

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Dedicated to Prof. Hansgeorg Schnöckel on the occasion of his 80th birthdayNew O-centered tetranuclear titanium complex Ti 4 O(Se 2 ) 4 Br 6 has been prepared from TiSe 1.73 , Se, SeO 2 and Br 2 at moderate temperature by ampule synthesis. Its X-ray crystal structure (monoclinic space group P2 1 /c, a = 9.4850( 2), b = 11.4667(2), c = 19.1413(5)Å, β = 92.0080(10)°, Z = 4, V = 2080.56(8)Å 3 ) includes molecular complex Ti 4 O(Se 2 ) 4 Br 6 based on fragment {Ti 4 (μ 4 -O)} coordinated by diselenide (Se 2 ) 2À and bromide bridging ligands. Ti 4 O(Se 2 ) 4 Br 6 is a new member of family of O-centered tetranuclear complexes with the fragment {M 4 (μ 4 -O)(Q 2 ) 4 } (M = Ti, Nb, Ta; Q=S, Se, Te); here we discuss its synthetic features, crystal and electronic structure. Experimental SectionMaterials and methods: Titanium powder (À 60 + 100 mesh, 99.5 % (metals basis)) was purchased from Alfa Aesar, selenium granules (99.997 %) and SeO 2 (99 %) was purchased from "LenPromKhim" Company (Russia), and liquid bromine (99 %) was obtained from Scientific and production association "Iodobrom" (Russia). Glass tubes from Simax Company were used for preparation of ampoules. X-ray powder diffraction (XRPD) patterns for solids were collected with a Philips PW 1830/1710 automated diffractometer (Cu Kα radiation, graphite monochromator, silicon plate as an external standard). Raman spectra were recorded with a labRAM HR Evolution spectrometer (Horiba Scientific) in the region 10-350 cm À 1 from a single crystal picked up from product Ti 4 OSe 8 Br 6 . Energy-dispersive spectroscopy (EDS) was performed with a Hitachi TM3000 device.Synthesis of the starting materials: TiSe 2 was obtained from the elements. Titanium powder (4.67 g, 97.6 mmol) and selenium granules (16.4 g, 208 mmol) in evacuated and sealed quartz ampule heated up to 750°C during 15 hours, and kept at this temperature for 15 h. Then ampule was opened and excess of selenium was removed by heating in dynamic vacuum at 350°C.

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ChemInform Abstract: Synthesis and Crystal Structure of Trichlorosulfonium Nonachlorodititanate(IV), (SCl3)(Ti2Cl9).

Abstract: ChemInform Abstract Prolonged treatment of TiCl4 (II) with a large excess of SCl2 (I) yields the novel ionic title compound (III). Single crystals of this compound are submitted to an X-ray analysis. Compound (III) is found to be rhombohedral; Z=18.

Cited by 5 publications

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Reactions of Chalcogen Oxide Chlorides EOCl2 (E = S, Se) with Group 5 Metal Chlorides

Reactions of Chalcogen Oxide Chlorides EOCl2 (E = S, Se) with Group 5 Metal Chlorides

Reactivity of Binary and Ternary Sulfur Halides towards Transition‐Metal Compounds

New O‐centered titanium chalcohalide: synthesis and structure of Ti₄O(Se₂)₄Br₆

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ChemInform Abstract: Synthesis and Crystal Structure of Trichlorosulfonium Nonachlorodititanate(IV), (SCl3)(Ti2Cl9).

Abstract: ChemInform Abstract Prolonged treatment of TiCl4 (II) with a large excess of SCl2 (I) yields the novel ionic title compound (III). Single crystals of this compound are submitted to an X-ray analysis. Compound (III) is found to be rhombohedral; Z=18.

Cited by 5 publications

References 0 publications

Reactions of Chalcogen Oxide Chlorides EOCl2 (E = S, Se) with Group 5 Metal Chlorides

Reactions of Chalcogen Oxide Chlorides EOCl2 (E = S, Se) with Group 5 Metal Chlorides

Reactivity of Binary and Ternary Sulfur Halides towards Transition‐Metal Compounds

New O‐centered titanium chalcohalide: synthesis and structure of Ti4O(Se2)4Br6

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New O‐centered titanium chalcohalide: synthesis and structure of Ti₄O(Se₂)₄Br₆