{Ru(μ-1,2-(NH)2C6H4)(CO)(dppb)} | 137192-65-5

• 英文名称: {Ru(μ-1,2-(NH)2C6H4)(CO)(dppb)}
• CAS: 137192-65-5
• 化学式: C₃₅H₃₄N₂OP₂Ru
• 分子量: 661.685
• InChiKey: STFYHVGYDTTWTP-UHFFFAOYSA-N

计算性质

• 辛醇/水分配系数(LogP)：
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• 重原子数：
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• 可旋转键数：
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• 环数：
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• sp3杂化的碳原子比例：
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• 拓扑面积：
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• 氢给体数：
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• 氢受体数：
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反应信息

• 作为产物：
  描述：

  、 1,4-双(二苯基膦)丁烷 以 甲苯 为溶剂， 以80%的产率得到{Ru(μ-1,2-(NH)2C6H4)(CO)(dppb)}
  参考文献：
  名称：

  Crystal structure and reactivity of [Ru{C₆H₄(NH)₂-1,2}-(PPh₃)₃] with π-acid ligands

  摘要：

  The structure of the compound [Ru{C6H4(NH)2-1,2)(PPh3)3] 1 has been established from X-ray analysis by direct and Fourier methods and refined by full-matrix least squares to R = 0.071 for 3288 observed reflections: monoclinic, space group P2(1)/n, a = 18.70(1), b = 13.171 (6), c = 23.06(2) angstrom, beta 99.86(6)-degrees and Z = 4. This complex reacts with an excess of ethylene or styrene and with P(OMe), (molar ratio 1 : 1 ) in hot toluene to yield the complexes [Ru{C6H4(NH)2-1,2}L(PPh3)2] [L = C2H4 3, CH2CHPh 4 or P(OMe)3, 5]. With a slight excess of the diphosphines (Ph2P)2X [X = CH2 (dppm), C2H4 (dppe), 1,2-C6H4 (dppbz), cis-C2H2 (dppen) and C3H6 (dppp)], refluxed in toluene, the complexes [Ru{C6H4(NH)2-1,2}] (PPh3) (diphosphine)] 6-10 were obtained as dark purple crystalline solids. An excess of PMe3 in hot toluene solutions of compound 1 afforded brown prismatic crystals of [Ru{C6H4(NH)2-1,2)](PMe3)3] 11, whereas with PEt3 under the same conditions only partial substitution products are obtained, [Ru{C6H4(NH)2-1,2}](PEt3)(PPh3)2] 12 and [Ru{C6H4(NH)2-1,2}(PEt3)2(PPh2)] 13. When toluene solutions of [Ru{C6H4(NH)2-1,2}](CO)(PPh3)2] 2 were boiled with diphosphines the complexes [Ru{C6H4(NH)2-1,2}(CO)(diphosphine)] [dppe 14, dppbz 15, dppen 16, dppp 17 or dppb (X = C4H8) 18] were isolated. The complex [Ru{C6H4(NH)2-1,2)] (CO)2(PPh3)] 19 was also detected as a reaction product of carbonylation of toluene solutions of 1. All complexes have been characterized by elemental analysis and by IR and NMR spectroscopy.

  DOI：

  10.1039/dt9930001125

文献信息

• Binuclear complexes of ruthenium with diphosphines and bridging benzene-1,2-diamide. X-Ray crystal structure of [Ru₂{µ-1,2-(NH)₂C₆H₄}{µ-(Ph₂P)₂CH₂}(CO)₂(PPh₃)₂]·C₆H₅Me
  作者：Adela Anillo、Ricardo Obeso-Rosete、Maria Angela Pellinghelli、Antonio Tiripicchio

  DOI：10.1039/dt9910002019

  日期：——

  The binuclear complex [Ru2mu-1,2-(NH)2C6H4}(CO)4(PPh3)2] 1 reacts with the diphosphines (Ph2P)2X [X = C2H4 (dppe), cis-C2H2 (dppen), 1,2-C6H4 (dppbz), C3H6 (dppp) and C4H8 (dppb)], in boiling toluene, to give purple solutions from which the yellow compounds [Ru2mu-1,2-(NH)2C6H4}(CO)3(PPh3)(diphosphine)] [dppe, 2; dppen, 3, dppbz, 4; dppp, 5; or dppb, 6 can be obtained after purification on an Al2O3 column and crystallization from toluene-hexane solutions. The reaction of 1 with (Ph2P)2CH2 (dppm), in boiling toluene or xylene, affords [Ru2mu-1,2-(NH)2C6H4}-(mu-dppm) (CO)2(PPh3)2] 7 as the unique product. All these new complexes can be obtained in good yields by reaction of [Ru1,2-(NH)2C6H4}(PPh3)(diphosphine)] with [Ru(CO)3(PPh3)2] in boiling mesitylene. Compound 1 also reacts with [Ru1,2-(NH)2C6H4}(PPh3)3] or [RuH2(PPh3)4] in boiling xylene to give [Ru2mu-1,2-(NH)2C6H4}(CO)3(PPh3)3] 8 which easily regenerates 1 by reaction with CO. An excess of diphosphine (except for dppm) in the reaction with 1 produced the mononuclear complexes [Ru1,2-(NH)2C6H4}(CO)(diphosphine)] and [Ru(CO)2(PPh3)(diphosphine)] and for the reaction with dppb the complexes [Ru2mu-1,2-(NH)2C6H4}(CO)3(dppb-P)(dppb-PP')] 9, [Ru2mu-1,2-(NH)2C6H4}(mu-dppb)(CO)2(PPh3)2] 10, [Ru2mu-1,2-(NH)2C6H4}(CO)2(dppb)2] 11 and [Ru(CO)2-(dppb-P)(dppb-PP')] 12 were also detected or isolated. All complexes have been characterized by elemental analysis and by IR and NMR spectroscopy. The structure of the toluene solvate of 7 has been determined by X-ray diffraction methods: monoclinic, space group P2(1)/n, with a = 18.563(8), b = 21.066(9), c = 17.936(7) angstrom, beta = 110.47(2)-degrees and Z = 4. The structure was solved from diffractometer data by Patterson and Fourier methods and refined by full-matrix least squares to R = 0.0524 for 6679 observed reflections. The two Ru atoms are doubly bridged by the nitrogen atoms of the 1,2-diimine ligand with a short Ru-Ru separation, 2.562(1) angstrom, consistent with a metal-metal bond.