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. 2016 Jun 17;291(33):17077–17092. doi: 10.1074/jbc.M116.735530

TABLE 3.

EPR spectroscopic properties of NeHAO, KsHOX, and KsHDH

EPR species are numbered according to Ref. 15 with our refinement.

Protein EPR species (iron/monomer)a gxyz values Comment/Assignment
NeHAOb
    1 (1) 1.20; 2.26; 3.03 Uncoupled heme 1
    2 (3) 1.35; 2.19; 3.11 (3.09)c Uncoupled hemes 7 and 8; includes the easily reducible heme 2
    3 (2) 1.27; 2.28; 3.06 Coupled hemes 3 and 5
    4 (2) 8 Coupled hemes 6 and 4 (P460); only observed in parallel mode EPR

KsHOX
    1 (1) 1.452; 2.305; 2.955 Heme 1; g values become 1.452, 2.260, and 2.980 after NH2OH incubation
    2a (1) 1.41; 2.145; 3.1412 Reduced after NH2OH incubation; heme 2
    2b (2) 1.41, 2.217, 2.955 Uncoupled hemes 7 and 8; g values become 1.37, 2.217, and 2.980 after NH2OH incubation
    3 (2) 1.40; 2.18; 3.247 Coupled hemes 3 and 5 (Euler angles: 45, −180, and 135°); after NH2OH incubation, each heme reduces by 60%, gz changes to 3.265, and the exchange splitting increases from 0.031 to 0.035 cm−1
    4 (2) NDd
    5 (minor) 6.07; 5.81; 1.98 High spin heme, but amount is preparation-dependent (0.03–0.14/monomer; the higher value shown in Figs. 8 (A and B) and 9A

KsHDH
    1 (1) 1.6; 2.05; 3.14 Uncoupled heme (heme 1) with broad resonances that sharpen and shift (gx,y,z = 1.51, 2.256, 3.10) upon reduction by hydrazine
    2a (1) (3.8%) (6.7%) (6.1%) 1.772; 2.06; 2.579 Heme 2; N2H4-reducible; same heme in slightly different environments
    2b (2) 1.772; 2.06; 2.543
1.772; 2.06; 2.497
1.5; 2.3; 3.0 Coupled hemes 7 and 8 (Euler angles: 45, 180, and 87°); no reduction by hydrazine, but gz changes to 3.05; the exchange splitting is 0.035 cm−1
    3 (2) 1.5; 2.3; 3.0 Coupled hemes 3 and 5 (Euler angles: 45, −180, and 135°); reduction by hydrazine (70%), and gz changes to 3.04; the exchange splitting is 0.074 cm−1 and 0.087 cm−1 after reduction
    4 (2) ND
    5 (minor) 6.0; 6.0; 2.0 Minor high spin heme (<0.02/monomer)
    6 (minor) 2.009 Possible tyrosine radical coupled to heme 4

a In column 1, numbers in parentheses indicate the integral number of spins, and percentage values represent the percentage of the total of integrated spins.

b Data from Hendrich et al. (15).

c In parentheses, gz after 1-electron reduction.

d ND, not determined. Signal accounting for hemes 6 and 4, which only would be observed in parallel mode EPR.