Scolaro Luigi Monsù, Plutino Maria Rosaria, Romeo Andrea, Romeo Raffaello, Ricciardi Giampaolo, Belviso Sandra, Albinati Alberto
Dipartimento di Chimica Inorganica, Chimica Analitica e Chimica Fisica, Università di Messina, and C.I.R.C.M.S.B. Unità di Messina, Salita Sperone 31, 98166 Vill. S. Agata, Messina, Italy.
Dalton Trans. 2006 Jun 7(21):2551-9. doi: 10.1039/b516391a. Epub 2006 Feb 27.
Reactions of the cationic complex ions [PtMe(Me2SO)(PP)]+ (PP = dppf (1,1'-bis(diphenylphosphino)ferrocene) and dppe (1,2-bis(diphenylphosphino)ethane)) with 5,10,15,20-tetrakis(4-pyridyl)-21H,23H-porphyrin (TpyP) led to the formation of the symmetrical tetraplatinated porphyrin complexes, [PtMe(PP)]4TpyP.X4 (PP = dppf, X = CF3SO3-, 3, and PP = dppe, X = BF4-, 5) containing the organometallic fragment [PtMe(PP)]. The precursor sulfoxide platinum complexes [PtMe(Me2SO)(dppf)]CF3SO3, 2 and [PtMe(Me2SO)(dppe)]BF4, 4, were prepared by halide abstraction from [PtMeCl(dppf)], 1, and by controlled protonolysis of [PtMe2(dppe)] respectively, in the presence of a small amount of dimethyl sulfoxide. All these starting platinum(II) compounds, as well as the porphyrin derivatives 3 and 5, were fully characterized through elemental analysis, 1H NMR mono- and bidimensional, 31P[1H], 31P-1H HMBC, UV/Vis absorption and photophysical measurements. The X-ray crystal structure of complex 1 has been determined. In order to ascertain the electronic influence of ferrocene, the spectroscopic and redox properties of 3 were compared with those of TPyP and of the analogous 5. Cyclic voltammetry (CV), differential pulse voltammetry (DPV), 1H and 31P NMR data, and UV/Vis data, all suggest a certain degree of communication between the central porphyrin and the peripheral hetero-bimetallic fragments. In contrast, no detectable interaction among these peripheral groups seem to come into play. Unlikely from the porphyrin derivative 5, formation of well defined fluorescent mesoscopic ring structures was easily achieved by simple evaporation from diluted dichloromethane solutions of 3.
阳离子络合离子[PtMe(Me₂SO)(PP)]⁺(PP = dppf(1,1'-双(二苯基膦基)二茂铁)和dppe(1,2-双(二苯基膦基)乙烷))与5,10,15,20-四(4-吡啶基)-21H,23H-卟啉(TpyP)反应生成对称的四铂化卟啉络合物[PtMe(PP)]₄TpyP·X₄(PP = dppf,X = CF₃SO₃⁻,3;PP = dppe,X = BF₄⁻,5),其中含有有机金属片段[PtMe(PP)]。前体亚砜铂络合物[PtMe(Me₂SO)(dppf)]CF₃SO₃,2和[PtMe(Me₂SO)(dppe)]BF₄,4,分别通过从[PtMeCl(dppf)],1中进行卤化物提取以及在少量二甲亚砜存在下对[PtMe₂(dppe)]进行受控质子解来制备。所有这些起始铂(II)化合物以及卟啉衍生物3和5,都通过元素分析、¹H NMR一维和二维、³¹P[¹H]、³¹P-¹H HMBC、UV/Vis吸收和光物理测量进行了全面表征。已确定络合物1的X射线晶体结构。为了确定二茂铁的电子影响,将3的光谱和氧化还原性质与TpyP以及类似物5的进行了比较。循环伏安法(CV)、差分脉冲伏安法(DPV)、¹H和³¹P NMR数据以及UV/Vis数据均表明中心卟啉与外围异双金属片段之间存在一定程度的相互作用。相比之下,这些外围基团之间似乎没有可检测到的相互作用。与卟啉衍生物5不同,通过从3的稀释二氯甲烷溶液中简单蒸发,很容易形成定义明确的荧光介观环结构。