CIRCULAR-DICHROISM, CRYSTAL-STRUCTURE, AND ABSOLUTE-CONFIGURATION OF THE SIDEROPHORE FERRIC N,N',N'-TRIACETYLFUSARININE, FEC39H57N6O15
CIRCULAR-DICHROISM, CRYSTAL-STRUCTURE, AND ABSOLUTE-CONFIGURATION OF THE SIDEROPHORE FERRIC N,N',N'-TRIACETYLFUSARININE, FEC39H57N6O15
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DOI：
10.1021/ja00538a012
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发表时间：
1980-01-01
影响因子：
15
通讯作者：
VANDERHELM, D
中科院分区：
文献类型：
--
作者：
HOSSAIN, MB;ENGWILMOT, DL;VANDERHELM, D
从一株不明青霉菌的缺铁培养物中分离得到铁载体N，N”，N”-三乙酰fusarinine (FeC39H57N6O15)，并通过阴离子交换、吸附和凝胶过滤层析进行纯化。该螯合物在正交空间群P212121中结晶为苯溶剂化物（每不对称单元有6-7个苯分子），每单元胞有4个苯分子，尺寸为a = 21.82 (3), b = 23.89 (3), c = 14.14(1)。在-135(2)度。C.强度数据（5669）在CAD-4型自动衍射仪上采集，使用Mo K.hivin. alpha。-135(2)度的辐射。该结构通过Patterson合成和连续差分傅立叶合成进行求解，并通过最小二乘法进行细化。所有数据的最终R值为0.141,4566份观测数据的最终R值为0.108。在扭曲的八面体中，Fe3+离子由3个羟基的氧原子配位。分子相对平坦，总厚度约为4.5 μ g；3个苯溶剂分子夹在大环之间。在由乙醇/苯得到的晶体中，分子具有。lambda。-顺式绝对构型，由固态上的反常色散和圆二色性确定；然而，在溶液中，在与氯仿形态不同的晶体中，分子主要以。delta的形式存在。-顺式非对映异构体，由圆二色性决定。
The siderophore ferric N,N'',N"-triacetylfusarinine (FeC39H57N6O15) was isolated from Fe-deficient cultures of an unidentified Penicillium sp. and purified by anion exchange, adsorption and gel-filtration chromatographies. The chelate was crystallized as the benzene solvate (6-7 molecules of benzene per asymmetric unit) in the orthorhombic space group P212121 with 4 molecules per unit cell of the dimensions a = 21.82 (3), b = 23.89 (3) and c = 14.14 (1) .ANG. at -135 (2).degree. C. The intensity data (5669) were collected on a CAD-4 automatic diffractometer, using Mo K.hivin..alpha. radiation at -135 (2).degree. C. The structure was solved by a Patterson synthesis and successive difference Fourier syntheses, and refined by least-squares methods. The final R values were 0.141 for all data and 0.108 for 4566 observed data. The Fe3+ ion is coordinated by the oxygen atoms of the 3 hydroxamate groups in a distorted octahedron. The molecule is relatively flat with a total thickness of about 4.5 .ANG.; 3 of the benzene solvent molecules are tucked between the macrocyclic rings. In the crystals obtained from ethanol/benzene, the molecules assume the .LAMBDA.-cis absolute configuration, as determined from anomalous dispersion and circular dichroism on the solid state; however, in solution, and in the morphologically different crystals from chloroform, the molecule exists predominantly as the .DELTA.-cis diastereoisomer, as determined by circular dichroism.