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. Author manuscript; available in PMC: 2012 Aug 3.

Published in final edited form as: J Am Chem Soc. 2011 Jul 11;133(30):11655–11664. doi: 10.1021/ja2036018

(A) Comparaion of 35 GHz ReMims pulsed ¹⁵N ENDOR spectra of intermediates trapped during turnover of the α-70^Ala/α-195^Gln MoFe protein with ¹⁵N₂H₄, ¹⁵N₂H₄, and ¹⁵NH=N-CH₃ (denoted ¹⁵MD). (B) 2D Field-Frequency plot of 35 GHz pulsed ¹⁵N ENDOR spectra of l(¹⁵N₂H₄) intermediate. Conditions: microwave frequency, 34.82 GHz; ReMims sequence, π/2 = 30 ns, τ₁ = 200 ns; RF 40 μs; repetition time, 10 ms; 500–950 scans; temperature, 2 K. Spectral baselines were corrected by simple subtraction if needed. Simulation (red) parameters: g = [2.09, 2.015, 1.98], hyperfine tensor A = [1.0, 2.8, 1.5] MHz, Euler angles ϕ = 50°, θ= 60°, ψ = 55° with respect to g-frame.

(A) Comparaion of 35 GHz ReMims pulsed ¹⁵N ENDOR spectra of intermediates trapped during turnover of the α-70^Ala/α-195^Gln MoFe protein with ¹⁵N₂H₄, ¹⁵N₂H₄, and ¹⁵NH=N-CH₃ (denoted ¹⁵MD). (B) 2D Field-Frequency plot of 35 GHz pulsed ¹⁵N ENDOR spectra of l(¹⁵N₂H₄) intermediate. Conditions: microwave frequency, 34.82 GHz; ReMims sequence, π/2 = 30 ns, τ₁ = 200 ns; RF 40 μs; repetition time, 10 ms; 500–950 scans; temperature, 2 K. Spectral baselines were corrected by simple subtraction if needed. Simulation (red) parameters: g = [2.09, 2.015, 1.98], hyperfine tensor A = [1.0, 2.8, 1.5] MHz, Euler angles ϕ = 50°, θ= 60°, ψ = 55° with respect to g-frame.