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Synthesis and Coordination Behaviour of (Ph3SnO)3As. The Crystal Structures of (Ph3SnO)3As and [{(Ph3SnO)3As}Fe(CO)4] (Ph3SnO)3As ( 1 ) was obtained from the reaction of Ph3SnOH with As2O3 in a dichloromethane/water mixture as solvent. Upon recrystallization from DMF 1 forms orthorhombic crystals, space group P212121, with a = 977.3(2), b = 1903.5(3) and c = 2600.9(5) pm (at 220 K). In 1 the As atom is bound to three OSnPh3 groups with As–O distances of 171.9(3)–174.9(3) pm. Reaction of 1 with Fe2(CO)9 gives [{(Ph3SnO)3As}Fe(CO)4] ( 2 ). 2 crystallizes monoclinic, space group P21/n with a = 2242.3(5), b = 1112.6(2), c = 2353.0(5) pm and β = 111,46(2)° (at 220 K). In 2 the iron atom exhibits a trigonal bipyramidal coordination with the (Ph3SnO)3As ligand in an axial position. The Fe–As bond length is 230.5(1) pm. 相似文献
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The reaction of Ph3SnCl, (R4N)2[Mo6O19] and (R4N)OH in a molar ratio of 6:1:10 leads to the formation of (R4N)[(Ph3Sn)MoO4] (R = nPr ( 1 ), nBu ( 2 )). Compounds 1· CH3CN and 2 have been charactarized by IR spectroscopy and single crystal X‐ray diffraction. 1· CH3CN forms orthorhombic crystals, space group P212121 with a = 1339.9(2), b = 1508.9(2), c = 1733.2(3) pm. 2 crystallizes in the monoclinic space group P21 with a = 1342.6(2), b = 2280.3(4), c = 1344.0(2) pm, β = 118.34(1). Both compounds 1 and 2 consist of isolated R4N+ cations and polymeric $\rm^{1}_{\infty}$ [(Ph3Sn)MoO4]– chains with an alternating arrangement of Ph3Sn+ and MoO42– groups. Treatment of (Ph3Sn)2MoO4 with bis(ethylenediamine)copper(II) succinate yields [Cu(en)2(Ph3Sn)2(MoO4)2] ( 3 ). The zinc derivative [Zn(en)2(Ph3Sn)2(MoO4)2] ( 4 ) is obtained similarly by reaction of (Ph3Sn)2MoO4 with bis(ethylenediamine)zinc(II) formiate. Compounds 3· 2DMF · EtOH and 4· 2DMF · EtOH crystallize in the monoclinic space group P21/n with a = 1998.0(2), b = 1313.3(1), c = 2181.6(2) pm, β = 90.97(1)° for 3 and a = 2015.4(1), b = 1316.7(1), c = 2157.0(1) pm, β = 90.40(1)° for 4 . Like in the cases of 1 and 2, polymeric $\rm^{1}_{\infty}$ [(Ph3Sn)MoO4]– chains are observed. The [M(en)2]2+ units (M = Cu, Zn) act as linkers between the $\rm^{1}_{\infty}$ [(Ph3Sn)MoO4]– chains to give 2D layer structures with (6, 3) net topology. 相似文献
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[{Cp(CO)3Mo}4In4(PSiMe3)4], an Organometallic In4P4-Heterocubane [{Cp(CO)3Mo}InCl2] reacts with P(SiMe3)3 in THF as solvent to form [{Cp(CO)3Mo}4In4(PSiMe3)4] 1. 1 crystallizes in the space group P1 . The lattice constants (at 208 K) are: a = 1 770.1(6), b = 1 490.3(6), c = 1 317.5(6) pm, α = 76.59(4),β = 88.54(3), γ = 88.98(3)°. According to the crystal structure analysis, 1 contains a slightly distorted In4P4-core with an alternating arrangement of In and P atoms. The In atoms are coordinated roughly tetrahedrally by three PSiMe3 groups (In–P: 256.9(3)–262.3(3) pm) and a {Cp(CO)3Mo} substituent (In? Mo: 278.0(2)–279.5(3) pm). 相似文献
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New Polynuclear Organotin(IV)–Nitrogen Compounds. Synthesis and Crystal Structures of [(PhSn)4(NPh)5Cl2] and [(MeSn)4(NHPh)4(NPh)4] The reaction of the organotin halides PhSnCl3 and MeSnCl3 with LiNHPh leads to the formation of two new nitrogen bridged organotin compounds, [(PhSn)4(NPh)5Cl2] ( 1 ) and [(MeSn)4(NHPh)4(NPh)4] ( 2 ). The crystal structures of 1 and 2 have been determined by low temperature X‐ray diffraction. 1 contains a bicyclic Sn4N5 framework, which consists of two six‐membered Sn3N3‐rings. All tin atoms are coordinated nearly tetrahedrally. Two tin atoms are bonded to a phenyl group and three nitrogen atoms, the other two tin atoms are coordinated by a phenyl group, two nitrogen atoms and a terminal chlorine atom. In 2 the tin atoms define the corners of a distorted square. Each edge of the square is bridged by a μ2‐NHPh and a μ2‐NPh group. The bridging NHPh and NPh groups are arranged at opposite sides of the Sn4 plane. The tin atoms are coordinated square pyramidally by 4 nitrogen atoms and a methyl group. 相似文献
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New Organometallic Indium Nitrogen Compounds. Synthesis and Crystal Structures of [{Cp(CO)3Mo}2InN(SiMe3)2] and [{Cp(CO)3Mo}In{N(SiMe3)2}2] The reaction of [{Cp(CO)3Mo}2InCl] with LiN · (SiMe3)2 leads to the formation of [{Cp(CO)3Mo}2InN · (SiMe3)2] ( 1 ). 1 is monomeric and it contains an indium atom which is coordinated in a trigonal planar manner by two {Cp(CO)3Mo} fragments and a N(SiMe3)2 group. The corresponding bis-amide [{Cp(CO)3Mo}In{N(SiMe3)2}2] ( 2 ) is prepared by the reaction of [{Cp(CO)3Mo}InCl2] with two equivalents of LiN(SiMe3)2. In analogy to 1, 2 is monomeric and it contains an indium atom in a trigonal planar coordination. 相似文献
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Coordinatively Unsaturated Diruthenium Complexes: Synthesis and X‐ray Crystal Structures of [Ru2(CO)n(μ‐H)(μ‐PtBu2)(μ‐Ph2PCH2PPh2)] (n = 4; 5) and [Ru2(CO)4(μ‐CH2)(μ‐H)(μ‐PtBu2)(μ‐Ph2PCH2PPh2)] The reaction of [Ru2(μ‐CO)(CO)5(μ‐H)(μ‐PtBu2)(tBu2PH)] ( 2 ) with dppm yields the dinuclear species [Ru2(μ‐CO)(CO)4(μ‐H)(μ‐PtBu2)(μ‐dppm)] ( 3 ) (dppm = Ph2PCH2PPh2). Under thermal or photolytic conditions 3 loses very easily one carbonyl ligand and affords the corresponding electronically and coordinatively unsaturated complex [Ru2(CO)4(μ‐H)(μ‐PtBu2)(μ‐dppm)] ( 4 ). 4 is also obtainable by an one‐pot synthesis from [Ru3(CO)12], an excess of tBu2PH and stoichiometric amounts of dppm via the formation of [Ru2(CO)4(μ‐H)(μ‐PtBu2)(tBu2PH)2] ( 1 ). 4 exhibits a Ru–Ru double bond which could be confirmed by addition of methylene to the dimetallacyclopropane [Ru2(CO)4(μ‐CH2)(μ‐H)(μ‐PtBu2)(μ‐dppm)] ( 5 ). The molecular structures of 3 , 4 and 5 were determined by X‐ray crystal structure analyses. 相似文献
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Coordinatively Unsaturated Diiron Complexes: Synthesis and Crystal Structures of [Fe2(CO)4(μ‐H)(μ‐PtBu2)(μ‐Ph2PCH2PPh2)] and [Fe2(CO)4(μ‐CH2)(μ‐H)(μ‐PtBu2)(μ‐Ph2PCH2PPh2)] [Fe2(μ‐CO)(CO)6(μ‐H)(μ‐PtBu2)] ( 1 ) reacts spontaneously with dppm (dppm = Ph2PCH2PPh2) to give [Fe2(μ‐CO)(CO)4(μ‐H)(μ‐PtBu2)(μ‐dppm)] ( 2 c ). By thermolysis or photolysis, 2 c loses very easily one carbonyl ligand and yields the corresponding electronically and coordinatively unsaturated complex [Fe2(CO)4(μ‐H)(μ‐PtBu2)(μ‐dppm)] ( 3 ). 3 exhibits a Fe–Fe double bond which could be confirmed by the addition of methylene to the corresponding dimetallacyclopropane [Fe2(CO)4(μ‐CH2)(μ‐H)(μ‐PtBu2)(μ‐dppm)] ( 4 ). The reaction of 1 with dppe (Ph2PC2H4PPh2) affords [Fe2(μ‐CO)(CO)4(μ‐H)(μ‐PtBu2)(μ‐dppe)] ( 5 ). In contrast to the thermolysis of 2 c , yielding 3 , the heating of 5 in toluene leads rapidly to complete decomposition. The reaction of 1 with PPh3 yields [Fe2(CO)6(H)(μ‐PtBu2)(PPh3)] ( 6 a ), while with tBu2PH the compound [Fe2(μ‐CO)(CO)5(μ‐H)(μ‐PtBu2)(tBu2PH)] ( 6 b ) is formed. The thermolysis of 6 b affords [Fe2(CO)5(μ‐PtBu2)2] and the degradation products [Fe(CO)3(tBu2PH)2] and [Fe(CO)4(tBu2PH)]. The molecular structures of 3 , 4 and 6 b were determined by X‐ray crystal structure analyses. 相似文献