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Mark Niemeyer Philip P. Power 《Angewandte Chemie (International ed. in English)》1998,37(9):1277-1279
A “one-legged thallium” is observed in the arylthallium(I ) compound 2,6-Trip2C6H3Tl (Trip=2,4,6-iPr3C6H2), which was synthesized from the corresponding organolithium compound and thallium chloride. X-ray structure analysis reveals that 2,6-Trip2C6H3Tl is monomeric in the solid state and contains a singly coordinated thallium atom (see space-filling model on the right). 相似文献
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Chemistry of Dimesityl Iron. X. Mesityl Iron Complexes [FeMes(X)]2 with a Central {Fe2(μ-Mes)2} Unit (Mes = C6H2-2,4,6-(CH3)3) Dimeric complexes [{MesFe(OAryl)}2] with coordination number (CN) of 3 are obtained from Fe2Mes4 1 by partial acidolyses with 2,6-di-tert-butyl-substituted phenols (HOAryl). 1 reacts with 1,3-diketones in a molar ratio of 1:2 to [{MesFe(diketonate)}2] with CN 4. A central {Fe2(μ-Mes)2}-unit with short Fe—Fe distances of 2.56 to 2.63 Å ( 1: 2.615 Å) is found in both types of complexes. The mixed ligand complexes react with an excess of phenol or diketone to {Fe(OAryl)2} or {Fe(diketonate)2}, respectively. 1 reacts with HOAryl in the molar ratio of 1:1 to [Fe2(μ-Mes)2Mes(OAryl)]. The structures of [Fe2(μ-Mes)2(OC6H2-2,6-tBu2-4-CH3)2] ( 3 ), [Fe2(μ-Mes)2Mes(OC6H2-2,4,6-tBu3)] ( 5 ) and [Fe2(μ-Mes)2{(tBuCO)2CH}2] ( 9 ) are presented. 相似文献
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Alcoholysis of [Fe2(OtBu)6] as a Simple Route to New Iron(III)‐Alkoxo Compounds: Synthesis and Crystal Structures of [Fe2(OtAmyl)6], [Fe5OCl(OiPr)12], [Fe5O(OiPr)13], [Fe5O(OiBu)13], [Fe5O(OCH2CF3)13], [Fe5O(OnPr)13], and [Fe9O3(OnPr)21] · nPrOH New alkoxo‐iron compounds can be synthesized easily by alcoholysis of [Fe2(OtBu)6] ( 1 ). Due to different bulkyness of the alcohols used, three different structure types are formed: [Fe2(OR)6], [Fe5O(OR)13] and [Fe9O3(OR)21] · ROH. We report synthesis and crystal structures of the compounds [Fe5OCl(OiPr)12] ( 2 ), [Fe2(OtAmyl)6] ( 3 ), [Fe5O(OiPr)13] ( 4 ), [Fe5O(OiBu)13] ( 5 ), [Fe5O(OCH2CF3)13] ( 6 ), [Fe9O3(OnPr)21] · nPrOH ( 7 ) and [Fe5O(OnPr)13] ( 8 ). Crystallographic Data: 2 , tetragonal, P 4/n, a = 16.070(5) Å, c = 9.831(5) Å, V = 2539(2) Å3, Z = 2, dc = 1.360 gcm?3, R1 = 0.0636; 3 , monoclinic, P 21/c, a = 10.591(5) Å, b = 10.654(4) Å, c = 16.740(7) Å, β = 104.87(2)°, V = 1826(2) Å3, Z = 2, dc = 1.154 gcm?3, R1 = 0.0756; 4 , triclinic, , a = 20.640(3) Å, b = 21.383(3) Å, c = 21.537(3) Å, α = 82.37(1)°, β = 73.15(1)°, γ = 61.75(1)°, V = 8013(2) Å3, Z = 6, dc = 1.322 gcm?3, R1 = 0.0412; 5 , tetragonal, P 4cc, a = 13.612(5) Å, c = 36.853(5) Å, V = 6828(4) Å3, Z = 4, dc = 1.079 gcm?3, R1 = 0.0609; 6 , triclinic, , a = 12.039(2) Å, b = 12.673(3) Å, c = 19.600(4) Å, α = 93.60(1)°, β = 97.02(1)°, γ = 117.83(1)°, V = 2600(2) Å3, Z = 2, dc = 2.022 gcm?3, R1 = 0.0585; 7 , triclinic, , a = 12.989(3) Å, b = 16.750(4) Å, c = 21.644(5) Å, α = 84.69(1)°, β = 86.20(1)°, γ = 77.68(1)°, V = 4576(2) Å3, Z = 2, dc = 1.344 gcm?3, R1 = 0.0778; 8 , triclinic, , a = 12.597(5) Å, b = 12.764(5) Å, c = 16.727(7) Å, α = 91.94(1)°, β = 95.61(1)°, γ = 93.24(2)°, V = 2670(2) Å3, Z = 2, dc = 1.323 gcm?3, R1 = 0.0594. 相似文献
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Iron(II) Phosphane Complexes. Synthesis and Crystal Structures of [Fe2I4(dppe)2], [Fe2(SR)4(dppe)2], [Fe(SR′)2(dppp)] and [Fe(SR)2(PMePh2)2] (dppe = Ph2P(CH2)2PPh2; dppp = Ph2P(CH2)3PPh2; R = 2,4,6-Me3C6H2; R′ = 2,4-tBuC6H3) The title compounds were isolated and their structures determined by crystallographic methods. [Fe2I4(dppe)2] ( 1 ) and [Fe2(SR)4(dppe)2] ( 2 ) form dimeric complexes with the bidentate phosphane binding to different iron atoms. The resulting ten-membered rings of both compounds exhibit a nearly identical conformation. The central FeS2P2 units of the mononuclear complexes [Fe(SR′)2(dppp)] ( 3 ) and [Fe(SR)2(PMePh2)2] ( 4 ) show like 2 large deviations from ideal C2v symmetry with bonding angles around the central iron atom ranging from 97.2, 92.5, and 96.5° (angle P? Fe? P in 2, 3 , and 4 , respectively) to 129.0, 129.9, and 133.6° (angle S? Fe? S in 2, 3 , and 4 , respectively). 相似文献