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Synthesis and characterization of a range of antimony(I/III) N,N′-bis(2,6-diisopropylphenyl)formamidinate complexes
Acta Crystallographica Section C ( IF 0.7 ) Pub Date : 2021-08-25 , DOI: 10.1107/s2053229621008512 Areej Al-Dabbagh 1 , Zhifang Guo 1 , Peter Junk 1 , Jun Wang 1
Acta Crystallographica Section C ( IF 0.7 ) Pub Date : 2021-08-25 , DOI: 10.1107/s2053229621008512 Areej Al-Dabbagh 1 , Zhifang Guo 1 , Peter Junk 1 , Jun Wang 1
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Formamidinatoantimony(I/III) complexes have been successfully synthesized as monomers or dimers in the solid state featuring a variety of coordination geometries and have also been comprehensively characterized. The antimony(I) formamidinate complex bis[μ-N,N′-bis(2,6-diisopropylphenyl)formamidinato]diantimony(I)(2 Sb—Sb) tetrahydrofuran heptasolvate, [Sb2(C25H35N2)2]·7C4H8O or [Sb2(DippForm)2]·7THF, (1), was obtained by a metathesis reaction between sodium bis(trimethylsilyl)amide [NaN(SiMe3)2] and N,N′-bis(2,6-diisopropylphenyl)formamidine (DippFormH), followed by SbCl3. A range of trivalent haloformamidinatoantimony(III) complexes, namely, bis[N,N′-bis(2,6-diisopropylphenyl)formamidinato]chloridoantimony(III), [Sb(C25H35N2)2Cl] or [Sb(DippForm)2Cl], (2), bis[N,N′-bis(2,6-diisopropylphenyl)formamidinato]bromidoantimony(III), [SbBr(C25H35N2)2] or [SbBr(DippForm)2], (3), bis[N,N′-bis(2,6-diisopropylphenyl)formamidinato]iodidoantimony(III), [Sb(C25H35N2)2I] or [Sb(DippForm)2I], (4), [N,N′-bis(2,6-diisopropylphenyl)formamidinato]dibromidoantimony(III), [SbBr2(C25H35N2)] or [SbBr2(DippForm)], (5), and [N,N′-bis(2,6-diisopropylphenyl)formamidinato]diiodidoantimony(III), [Sb(C25H35N2)I2] or [Sb(DippForm)I2], (6), were also synthesized by adding DippFormH and MN(SiMe3)2 (M = Li or Na) to the corresponding antimony halides SbX3 (X = Cl, Br or I) in differing ratios. The complexes were all stable to rearrangement.
中文翻译：
一系列锑 (I/III) N,N'-双(2,6-二异丙基苯基)甲脒配合物的合成和表征
甲脒锑 (I/III) 配合物已成功合成为固态单体或二聚体，具有多种配位几何结构，并已得到全面表征。锑(I)甲脒配合物双[μ- N , N'-双(2,6-二异丙基苯基)甲脒]二锑(I)(2 Sb - Sb )四氢呋喃七溶剂化物，[Sb 2 (C 25 H 35 N 2 ) 2 ]·7C 4 H 8 O 或 [Sb 2 (DippForm) 2 ]·7THF, ( 1)，通过双(三甲基甲硅烷基)酰胺钠[NaN(SiMe 3 ) 2 ]和N , N '-双(2,6-二异丙基苯基)甲脒(DippFormH)和SbCl 3之间的复分解反应获得。一系列三价卤代甲脒锑(III) 络合物，即双 [ N , N '-双 (2,6-二异丙基苯基) 甲脒] 氯化锑 (III)、[Sb(C 25 H 35 N 2 ) 2 Cl] 或 [Sb (DippForm) 2 Cl], ( 2 ), 双[ N , N '-双(2,6-二异丙基苯基)甲脒]溴代锑(III), [SbBr(C 25H 35 N 2 ) 2 ]或[SbBr(DippForm) 2 ], ( 3 ), 双[ N , N '-双(2,6-二异丙基苯基)甲脒]碘代锑(III), [Sb(C 25 H 35 N) 2 ) 2 I] 或 [Sb(DippForm) 2 I], ( 4 ), [ N , N'-双(2,6-二异丙基苯基)甲脒]二溴代锑(III), [SbBr 2 (C 25 H 35 N 2) )] 或 [SbBr 2 (DippForm)]、( 5 ) 和 [ N ,N′-双(2,6-二异丙基苯基)甲脒基]二碘代锑(III)，[Sb(C 25 H 35 N 2 )I 2 ]或[Sb(DippForm)I 2 ]，( 6 )，也通过加入DippFormH 和 M N(SiMe 3 ) 2 ( M = Li 或 Na) 与相应的卤化锑 Sb X 3 ( X = Cl、Br 或 I) 以不同的比率。复合物对重排均稳定。
更新日期：2021-09-06
中文翻译：
一系列锑 (I/III) N,N'-双(2,6-二异丙基苯基)甲脒配合物的合成和表征
甲脒锑 (I/III) 配合物已成功合成为固态单体或二聚体，具有多种配位几何结构，并已得到全面表征。锑(I)甲脒配合物双[μ- N , N'-双(2,6-二异丙基苯基)甲脒]二锑(I)(2 Sb - Sb )四氢呋喃七溶剂化物，[Sb 2 (C 25 H 35 N 2 ) 2 ]·7C 4 H 8 O 或 [Sb 2 (DippForm) 2 ]·7THF, ( 1)，通过双(三甲基甲硅烷基)酰胺钠[NaN(SiMe 3 ) 2 ]和N , N '-双(2,6-二异丙基苯基)甲脒(DippFormH)和SbCl 3之间的复分解反应获得。一系列三价卤代甲脒锑(III) 络合物，即双 [ N , N '-双 (2,6-二异丙基苯基) 甲脒] 氯化锑 (III)、[Sb(C 25 H 35 N 2 ) 2 Cl] 或 [Sb (DippForm) 2 Cl], ( 2 ), 双[ N , N '-双(2,6-二异丙基苯基)甲脒]溴代锑(III), [SbBr(C 25H 35 N 2 ) 2 ]或[SbBr(DippForm) 2 ], ( 3 ), 双[ N , N '-双(2,6-二异丙基苯基)甲脒]碘代锑(III), [Sb(C 25 H 35 N) 2 ) 2 I] 或 [Sb(DippForm) 2 I], ( 4 ), [ N , N'-双(2,6-二异丙基苯基)甲脒]二溴代锑(III), [SbBr 2 (C 25 H 35 N 2) )] 或 [SbBr 2 (DippForm)]、( 5 ) 和 [ N ,N′-双(2,6-二异丙基苯基)甲脒基]二碘代锑(III)，[Sb(C 25 H 35 N 2 )I 2 ]或[Sb(DippForm)I 2 ]，( 6 )，也通过加入DippFormH 和 M N(SiMe 3 ) 2 ( M = Li 或 Na) 与相应的卤化锑 Sb X 3 ( X = Cl、Br 或 I) 以不同的比率。复合物对重排均稳定。
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