The Mina and Everard Goodman Faculty of Life Sciences, Bar-Ilan University, Ramat-Gan 52900, Israel.
J Phys Chem B. 2011 Jan 13;115(1):143-57. doi: 10.1021/jp107553j. Epub 2010 Dec 16.
The slowly relaxing local structure (SRLS) approach, developed for NMR spin relaxation analysis in proteins, is applied herein to amide ¹⁵N relaxation in deoxy and carbonmonoxy hemoglobin. Experimental data including ¹⁵N T₁, T₂ and ¹⁵N-{¹H} NOE, acquired at 11.7 and 14.1 T, and 29 and 34 °C, are analyzed. The restricted local motion of the N-H bond is described in terms of the principal value (S(0)(2)) and orientation (β(D)) of an axial local ordering tensor, S, and the principal values (R(||)(L) and R(⊥)(L)) and orientation (β(O)) of an axial local diffusion tensor, R(L). The parameters c₀² (the potential coefficient in terms of which S(0)(2) is defined), R(||)(L), β(D), and β(O) are determined by data fitting; R(⊥)(L) is set equal to the global motional rate, R(C), found previously to be (5.2-5.8) × 10⁶ 1/s in the temperature range investigated. The principal axis of S is (nearly) parallel to the C(i-1)(α)-C(i)(α) axis; when the two axes are parallel, β(D) = -101.3° (in the frame used). The principal axis of R(L) is (nearly) parallel to the N-H bond; when the two axes are parallel, β(O) = -101.3°. For "rigid" N-H bonds located in secondary structure elements the best-fit parameters are S(0)(2) = 0.88-0.95 (corresponding to local potentials of 8.6-19.9 k(B)T), R(||)(L) = 10⁹-10¹⁰ 1/s, β(D) = -101.3° ± 2.0°, and β(O) = -101.3° ± 4°. For flexible N-H bonds located in loops the best-fit values are S(0)(2) = 0.75-0.80 (corresponding to local potentials of 4.5-5.5 k(B)T), R(||)(L) = (1.0-6.3) × 10⁸ 1/s, β(D) = -101.3° ± 4.0°, and β(O) = -101.3° ± 10°. These results are important in view of their physical clarity, inherent potential for further interpretation, consistency, and new qualitative insights provided (vide infra).
本文将用于蛋白质中 NMR 自旋弛豫分析的慢弛豫局部结构 (SRLS) 方法应用于脱氧和碳氧血红蛋白酰胺 ¹⁵N 弛豫的研究。在 11.7 和 14.1 T 以及 29 和 34°C 的条件下,获取了包括 ¹⁵N T₁、T₂ 和 ¹⁵N-{¹H} NOE 的实验数据,并对其进行了分析。通过轴向局部有序张量 S 的主值(S(0)(2))和取向(β(D))以及轴向局部扩散张量 R(L)的主值(R(||)(L)和 R(⊥)(L))和取向(β(O)),描述了 N-H 键的受限局部运动。参数 c₀²(用于定义 S(0)(2)的位势系数)、R(||)(L)、β(D)和β(O)是通过数据拟合确定的;R(⊥)(L)被设定为之前在研究温度范围内发现的(5.2-5.8)×10⁶ 1/s 的全局运动速率 R(C)。S 的主轴(几乎)与 C(i-1)(α)-C(i)(α)轴平行;当两个轴平行时,β(D) = -101.3°(在所使用的框架中)。R(L)的主轴(几乎)与 N-H 键平行;当两个轴平行时,β(O) = -101.3°。对于位于二级结构元件中的“刚性”N-H 键,最佳拟合参数为 S(0)(2) = 0.88-0.95(对应于 8.6-19.9 k(B)T 的局部位势),R(||)(L) = 10⁹-10¹⁰ 1/s,β(D) = -101.3° ± 2.0°,β(O) = -101.3° ± 4.0°。对于位于环中的柔性 N-H 键,最佳拟合值为 S(0)(2) = 0.75-0.80(对应于 4.5-5.5 k(B)T 的局部位势),R(||)(L) = (1.0-6.3)×10⁸ 1/s,β(D) = -101.3° ± 4.0°,β(O) = -101.3° ± 10°。这些结果具有物理清晰度、进一步解释的固有潜力、一致性以及提供的新的定性见解(见下文),非常重要。