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Figure 1.

Schematic of the Molecular Architecture of the Enzymes Investigated in This Study

The mature forms of the C. japonicus esterases consist of a single catalytic module. The C. thermocellum enzyme containing a CE2 module (CtCel5C-CE2) consists of an N-terminal GH5 cellulase module (CtCel5C), a central type I dockerin module (Doc) that facilitates the integration of the enzyme into the cellulosome, and a C-terminal CE2 module (CtCE2). The CE2 modules of all the esterases contains an N-terminal domain of ∼160 residues that displays a jelly roll fold and a C-terminal domain that exhibits an α/β-hydrolase fold. The black lines are ∼15-residue P/T linker sequences. The residues in CjCE2C that carry an asterisk are predicted catalytic residues based on sequence alignments.

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Table 1.

Catalytic Activity of CE2 Enzymes against 4-Nitrophenyl Acetate (4-NPAc)

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Table 2.

Activity of CE2 Esterases against Acetylated Polysaccharides

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Figure 2.

3-D Structures and Catalytic Constellation Geometries for Three CE2 Esterases

(A) 3-D structure of CjCE2B with the catalytic domain in green and the β-sheet domain in magenta. The catalytic Ser and His are shown in ball-and-stick representation.

(B) CjCE2A, drawn as above.

(C) CtCE2 as above and with cellopentaose in blue.

(D) The catalytic Ser-His-Asp triad of CjCE2A.

(E) The catalytic Ser-His dyad with the main-chain carbonyl interaction from Cys333 of CjCE2B.

(F) The catalytic dyad and main-chain carbonyl of CtCE2.

This figure was drawn with PyMOL (DeLano Scientific, http://pymol.sourceforge.net/).

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Figure 3.

Binding of Cellooligosaccharides through the Esterase Active Centre of CtCE2

Observed electron density (maximum-likelihood weighted 2Fobs − Fcalc contoured at 1 σ) for cellohexaose (in which cellopentaose is ordered) bound to wild-type CtCE2. Ser-612 and His-791 form the catalytic dyad, with Trp-790 causing a change in position of Asp-789 and forming the binding-platform for the second glucose. Other interactions with aromatic residues discussed in the text are shown. The figure is in divergent (“wall-eyed”) stereo and was drawn with PyMOL.

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Figure 4.

Binding of CE2 Esterases to Cellulose

(A) An AGE experiment in which the enzymes were subjected to nondenaturing gel electrophoresis in the absence (−) or presence (+) of 0.1 % (w/v) hydroxyethylcellulose. The lanes contained BSA (1), CtCE2 (2), CjCE2A (3), and CjCE2C (4). CjCE2B did not migrate on the nondenaturing gel.

(B) Shows a pull-down experiment using insoluble cellulose. The original protein samples (s) and bound protein eluted from cellulose with 10% SDS (b) were subjected to SDS-PAGE. The lanes contained CtCE2 (1), CjCE2A (2), CjCE2B (3), CjCE2C, (4), and BSA as a noninteracting control (5). Molecular weight markers are shown.

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Figure 5.

Examples of Isothermal Titration Calorimetry of Wild-Type and Mutants of CtCE2

The proteins were titrated with cellohexaose in 50 mM sodium HEPES buffer, pH 7.0, at 25 °C. The protein concentration for each titration was 100 μM.

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Table 3.

The Binding of CE2 Esterases to Cellohexaose and β-Glucan

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Table 3 Expand

Table 4.

ITC Analysis of CtCE2 Wild-Type and Mutants Binding to Cellooligosaccharides and β-Glucan

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Figure 6.

Inhibition of Wild-Type CtCE2 by Cellohexaose

CtCE2 was assayed at 37 °C using either 4-nitrophenyl acetate (A) or acetylated glucomannan (B) as the substrate in the presence of different concentrations of cellohexaose (C6). The figure displays double reciprocal plots of the data.

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Table 5.

Data Collection and Refinement Statistics

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