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This structure shows a dramatically different overall conformation from previous structures of EF-G, although the indi-vidual domains are highly similar.. Between the different structure

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analysis of a target for fusidic acid

Yang Chen, Ravi Kiran Koripella, Suparna Sanyal and Maria Selmer

Department of Cell and Molecular Biology, Uppsala University, Sweden

Introduction

Protein synthesis, translation of mRNA into protein, is

performed on the ribosome To synthesize a protein,

the ribosome goes through the phases of initiation,

elongation, termination, and recycling, each phase

being assisted by a number of protein translation

fac-tors [1,2] Some of these facfac-tors, in prokaryotes

initia-tion factor 2, elongainitia-tion factor Tu (EF-Tu), elongainitia-tion

factor G (EF-G), and release factor 3, are GTPases,

which drive the process forwards using GTP as the

energy source Among these, only EF-G participates

in two distinct steps of the translation cycle:

elonga-tion and ribosome recycling During elongaelonga-tion, after

formation of each new peptide bond, EF-G binds to the ribosome and, under GTP hydrolysis, catalyses translocation, the concerted movement of mRNA, together with A-site and P-site tRNAs, to expose a new A-site codon [3,4] Recycling takes place when the translating ribosome has reached a stop codon and released the nascent peptide At this point, EF-G and ribosome recycling factor bind to the post-termination complex to catalyse the disassembly of the complex [5– 7] EF-G has a low intrinsic activity in GTP hydrolysis that is stimulated by the interaction with the ribosome [8,9] The currently prevalent model states that EF-G

Keywords

antibiotic resistance; crystallography;

elongation factor G (EF-G); fusidic acid;

switch region

Correspondence

M Selmer, Department of Cell and

Molecular Biology, Uppsala University,

BMC, Box 596, 751 24 Uppsala, Sweden

Fax: +46 18 536971

Tel: +46 18 4714177

E-mail: maria.selmer@icm.uu.se

Database

The atomic coordinates and observed

structure factors are available in the Protein

Data Bank database under the accession

number 2XEX

(Received 22 April 2010, revised 28 June

2010, accepted 14 July 2010)

doi:10.1111/j.1742-4658.2010.07780.x

Fusidic acid (FA) is a bacteriostatic antibiotic that locks elongation factor G (EF-G) on the ribosome in a post-translocational state It is used clinically against Gram-positive bacteria such as pathogenic strains of Staphylo-coccus aureus, but no structural information has been available for EF-G from these species We have solved the apo crystal structure of EF-G from

S aureusto 1.9 A˚ resolution This structure shows a dramatically different overall conformation from previous structures of EF-G, although the indi-vidual domains are highly similar Between the different structures of free

or ribosome-bound EF-G, domains III–V move relative to domains I–II, resulting in a displacement of the tip of domain IV relative to domain G

In S aureus EF-G, this displacement is about 25 A˚ relative to structures of Thermus thermophilusEF-G in a direction perpendicular to that in previous observations Part of the switch I region (residues 46–56) is ordered in

a helix, and has a distinct conformation as compared with structures of EF-Tu in the GDP and GTP states Also, the switch II region shows a new conformation, which, as in other structures of free EF-G, is incompatible with FA binding We have analysed and discussed all known fusA-based fusidic acid resistance mutations in the light of the new structure of EF-G from S aureus, and a recent structure of T thermophilus EF-G in complex with the 70S ribosome with fusidic acid [Gao YG et al (2009) Science 326, 694–699] The mutations can be classified as affecting FA binding, EF-G– ribosome interactions, EF-G conformation, and EF-G stability

Abbreviations

EF-G, elongation factor G; EF-Tu, elongation factor Tu; EM, electron microscopy; FA, fusidic acid; PDB, Protein Data Bank.

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binds to the ribosome in GTP form, hydrolyses GTP,

releases inorganic phosphate and, through a

conforma-tional change, drives tRNA translocation [10] or

ribo-some recycling [7] However, there are recent

indications that EF-G may act differently in

transloca-tion and ribosome recycling [11]

The crystal structure of EF-G from Thermus

thermo-philus was first solved in 1994 in complex with GDP

[12] as well as in apo form [13] Since then, structures of

several mutants of EF-G from the same bacterium have

been solved [14–16] EF-G forms an extended structure

consisting of five domains (Fig 1A) The domain G

(domain I) and domain II form a globular structure

that is conserved in all other ribosomal GTPases The

exception is the additional subdomain G¢, which

is inserted in domain G, and exists only in release factor

3 and EF-G As in other GTPases, domain G

contains a conserved P-loop, which coordinates the

a-phosphate and b-phosphate, and two so-called switch

regions, which coordinate the c-phosphate and change

conformation between a tense GTP state and a relaxed

GDP state [17]

Ribosomal complexes that have been stalled by the

locking of EF-G to the ribosome with either a

nonhy-drolysable GTP analogue [18] or the antibiotic fusidic

acid (FA) and GDP [19–21] have been visualized with

cryo-electron microscopy (EM) and single-particle

reconstructions Recently, a 3.6 A˚ crystal structure of

EF-G bound to the T thermophilus ribosome showed

the FA-binding site for the first time, and revealed the detailed interactions of EF-G with the ribosome [22] (summarized in Fig 1B) As compared with this FA-stabilized, ribosome-bound conformation, crystal struc-tures of T thermophilus EF-G display different confor-mations, where domains III–V have rotated relative to domains I–II, resulting in the position of the tip of domain IV differing by 20 A˚ (Fig 2; discussed further below) It appears that ribosome binding is the main trigger of the conformational change in EF-G, as in solution it can accommodate GDP or GTP without forcing any major changes in its global conformation [15,23,24]

FA is a clinically used steroid antibiotic that locks EF-G on the ribosome after GTP hydrolysis and trans-location [25] FA binds to a pocket between domains

I, II and III of EF-G, and seems to lock EF-G in a conformation intermediate between the GTP-bound and GDP-bound forms [22] Staphylococcus aureus is one of the major clinical targets for FA treatment However, very few studies have been performed using EF-G from this species In this study, we have solved the apo crystal structure of S aureus EF-G to 1.9 A˚ resolution, allowing us to examine the generality of conclusions drawn from the T thermophilus EF-G structures and to pinpoint the role of amino acids that are mutated in isolated FA-resistant strains of

S aureus[26,27]

Results and Discussion Structure solution

S aureus EF-G was crystallized in a mixture of poly-ethylene glycol 3350 and NaCl in Tris⁄ HCl buffer at

pH 8.7 The crystals grew in space group P21 and diffracted to 1.9 A˚ resolution (Table 1) There are two molecules in the asymmetric unit, forming a noncrys-tallographic two-fold symmetry b-Sheets from domain

V of molecules A and B form an extended b-sheet, and helix AV packs in an antiparallel fashion to the equivalent helix in molecule B Residues 2–38, 64–441 and 445–692 in molecule A and residues 2–41, 46–56, 65–441 and 447–692 in molecule B were ordered and could be built into the electron density maps The ordered part includes domain III, which is disordered

in structures of wild-type T thermophilus EF-G [12,13] In molecule B, part of the switch I region could be built The entire switch I region is disordered

in all previous EF-G structures from T thermophilus [12–16], including the EF-G–70S complex structure with GDP and FA [22], and has been suggested to be ordered only in the ribosome-bound GTP state, as

Table 1 Summary of crystallographic data and refinement.

Data collection statistics

Refinement statistics

Number of atoms

Rmsd from ideality

Ramachandran statistics

a

Values in parentheses represent the highest-resolution bin.

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indicated by recent proteolytic cleavage experiments

[28] It is also disordered in structures of the

eukary-otic equivalent, eEF2 [29] In the present structure,

res-idues 46–56 form a helix that was only clearly visible

in difference Fourier maps after refinement of the rest

of the structure The density for residues 42–45 was

too weak to allow interpretation, but this region would

need to be in an extended conformation to bridge

16.5 A˚ between the a carbons of residues 41 and 46

In molecule A, the density for the entire switch I

region is too weak for interpretation, indicating higher

flexibility

Attempts to soak S aureus EF-G crystals with GDP

as well as nonhydrolysable GTP analogues resulted in

partial occupancy of GDP in the nucleotide-binding

site Therefore, we present here the apo structure of

S aureusEF-G

Overall structure and comparison with previous EF-G structures

All five domains of S aureus EF-G are ordered in our structure The overall conformation of the two EF-G molecules in the asymmetric unit is very similar (rmsd

of 0.58 A˚ for 660 Caatoms), with only a slight differ-ence in the orientation of domains III and IV Thus, when the two molecules are superimposed on the basis

of domains I and II, the maximum difference at the edge of domain III is 2.3 A˚

Comparison of S aureus EF-G with the previously solved T thermophilus EF-G structures shows that the individual domains are highly similar However, domains III, IV and V are in a different orienta-tion relative to domains I and II in comparison to previous EF-G structures (Fig 1C) Between all the

A

B

C

Fig 1 EF-G structure (A) Overall structure

and structural domains of S aureus EF-G

(PDB 2xex) The switch regions are shown

in black, with switch II facing domains II

and III, and switch I behind the G-domain.

(B) Crystal structure of EF-G bound to the

T thermophilus 70S ribosome with GDP

and FA (PDB 2wri [22]) FA (left) and GDP

(right) are shown in black Numbers indicate

ribosomal contact areas: 1, decoding centre;

2, 23S RNA 2475 loop; 3, 23S RNA

5, C-terminal domain of ribosomal protein

L12; 6, 23S RNA 2660 loop (from the back);

7, ribosomal protein S12 Thickness of lines

indicates closeness to the viewer.

(C) Comparison of apo-EF-G from S aureus

(PDB 2xex, magenta) and T thermophilus

(PDB 1elo [13], grey) Superposition is

based on domains I and II.

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T thermophilusEF-G structures, wild type and various

mutants, domains III, IV and V display a movement

relative to domains I and II, resulting in a shift of the

tip of domain IV of up to 8 A˚ [14,16] The

ribosome-bound structure of EF-G as visualized by

crystallogra-phy [22] shows a larger movement in the same

direc-tion, measuring about 27 A˚ The equivalent

comparison with S aureus EF-G shows a shift of

domains III, IV and V by approximately 25 A˚ in the

perpendicular direction (Fig 2) The hinge region for

this conformational change consists of residues 400–

405, as previously observed in T thermophilus EF-G

[16] Conformational changes of EF-G in more than

one direction were suggested in early cryo-EM studies

of ribosome–EF-G complexes [20], but because of the

low resolution (17–20 A˚), the structural interpretation

is not very reliable

The P-loop (residues 12–27) has the same

conforma-tion as in the apo structure of T thermophilus EF-G

[13], and upon crystal soaking with GDP, partial

occu-pancy of the peptide-flipped structure is observed, in

agreement with structures of T thermophilus EF-G

[30] (data not shown)

The switch I region consists of residues 39–63 The

ordered part is a helix from residues 46 to 56 that

packs against helix AGso that Trp52 makes

hydropho-bic interactions with Leu31, Tyr32 and Ile37, and

Met53 interacts with Glu28 (Fig 3A) With the

exception of Ile37, all of these residues are conserved in EF-G from different species In contrast to the situation in EF-G, the switch I region is fully ordered

in structures of EF-Tu with GDP [31] and a GTP analogue [32], as well as in the structure of the EF-G homologue EF-G-2 with GTP [18] In EF-Tu, the switch I region forms a short helix followed by a b-hair-pin reaching away from the nucleotide-binding site in the GDP state, whereas in the GTP state, it forms two short helices just before the conserved Thr that coordi-nates a magnesium ion and the c phosphate The helix that we observe is longer than in any of these structures, and has a different orientation (Fig 3B) It is too far away from the nucleotide-binding site to allow the inter-action of the conserved Thr62 with magnesium and c phosphate that should occur in the GTP state Superpo-sition of the current structure with the ribosome-bound EF-G [22] shows that the observed switch I conforma-tion would be compatible with ribosome binding and located in the intersubunit space at a distance of 10 A˚ from residue 2655 of 23S RNA, 15 A˚ from ribosomal protein L14, and 10 A˚ from residue 342 of 16S RNA The switch II region of S aureus EF-G has electron density for all residues, including side chains, except for Gly84 (Fig 3C) It has a different conformation compared to the T thermophilus EF-G structures (Fig 3D) The hydrogen bond Asp87–Arg659 stabi-lizes the switch II region and the current domain

38 Å

Fig 2 Conformational space of EF-G on and off the ribosome (A) Superposition of S aureus EF-G with the ribosome-bound T thermophilus EF-G (PDB 2wri [22], dark blue) and the T thermophilus apo-EF-G structure (PDB 1elo [13], yellow), based on domains I and II The arrow indicates the direction of projection to the circle in (C) (B) As (A), view 90 away (C) Comparison of the positions of the tip of domain IV in all available EF-G structures in the PDB The structures were superimposed on the basis of domains I and II Looking from the direction of the arrow in (A) and (B), the coordinates of His572 at the tip of domain IV are roughly in one plane, and were manually covered with a col-oured dot 1, E coli EF-G + GMPPNP + 70S (PDB 2om7 [18], cryo-EM); 2, T thermophilus EF-G + 70S + FA + GDP (PDB 2wri [22]); 3,

E coli EF-G + GDP + 70S + FA (PDB 1jqm [21], cryo-EM); 4, T thermophilus EF-G T84A + GMPPNP (PDB 2bv3 [15]); 5, T thermophilus EF-G + GDP (dimer, PDB 1ktv); 6, T thermophilus EF-G apo (PDb 1elo [13]); 7, T thermophilus EF-G T84A + GDP, FA-resistant (PDB 2bm0 [14]); 8, T thermophilus EF-G G16V + GDP, FA-hypersensitive (PDB 2bm1 [14]); 9, T thermophilus EF-G H573A + GDP (PDB 1fnm [16]); 10,

S aureus EF-G (PDB 2xex).

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C

B

D

E

map is contoured at 1r (B) Comparison of switch I in EF-G and EF-Tu The structures were superimposed on the basis of the equivalent parts of domains G and II The switch I region of S aureus apo-EF-G (PDB 2xex, magenta), EF-Tu in complex with GDP (PDB 1tui, yellow

region of S aureus EF-G contoured at 3r Omitted residues are shown in yellow stick representation (D) Comparison of the switch II region

thermo-philus EF-G wild type (PDB 1elo, yellow [13]); T thermothermo-philus EF-G H573A (PDB 1fnm, orange [16]); T thermothermo-philus EF-G T84A (PDB 2bm0, light blue [14]); T thermophilus EF-G G16V (PDB 2bm1, red [14]); T thermophilus EF-G T84A with GDPNP (PDB 2bv3, green [15]);

T thermophilus EF-G–GDP–FA complex with the ribosome (PDB 2wri, dark blue [22]) Residues 20–200 are shown, but only the switch II region and the side chain of Phe88 are coloured (E) Domain III and the FA-binding site Switch II regions of S aureus EF-G (magenta) and

residues 407–474), showing how the FA-binding site in the S aureus EF-G structure is blocked by the switch II region.

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arrangement, with a larger contact area between

domains II and V than that in any other structure of

EF-G The switch II region and the conserved Phe88

(Phe90 in T thermophilus) displays many different

ori-entations in the available crystal structures, and none

of the isolated EF-G structures displays a switch II

conformation identical to that of EF-G in complex

with the 70S ribosome and FA [22] (Fig 3D) Whereas

Phe88 in the ribosome-bound structure is exposed at

the surface of EF-G and forms part of the FA-binding

site, it points to the opposite direction in our structure,

interacting with Glu93 in helix BGand Tyr126 in helix

CG in the core of the domain, and blocking the

FA-binding site (Fig 3E) Despite its many different

con-formations, the switch II region also blocks the

FA-binding site in all structures of free T thermophilus EF-G (not shown) However, we do not believe that the alternative switch II conformations observed in structures of wild-type and mutant T thermophilus EF-G are responsible for FA sensitivity and resistance, respectively [14] Rather, the switch II region only adopts its FA-stabilized conformation when bound to the ribosome in the presence of the drug, and several

FA resistance mutations in the switch II region influ-ence direct contacts with FA (discussed further below)

Conformational space of EF-G The present structure of S aureus EF-G shows that EF-G, when not bound to the ribosome, can acquire

Fig 4 FA resistance mutations (A) All known FA resistance mutation sites (Table 2) mapped on the S aureus EF-G structure The mutation sites are displayed as side chains and located in domain III, domain V and the interface of domains G, III and V (B) Mutation sites in domain

are facing the ribosome, and the four-stranded b-sheet is facing the other domains of EF-G (D) Linker region between domains I–II and domains III–V The four sites of FA resistance mutations in this region are shown with side chains.

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a conformation that is distinctly different from what

has previously been observed for T thermophilus

EF-G The fact that the two molecules in the

asym-metric unit show identical conformations, despite

being involved in different crystal contacts, suggests

that this is not a crystallographic artefact

In the many different crystal structures of T

thermo-philus EF-G, only smaller conformational differences

have been observed [12–16] An explanation for this

could be that the interdomain movements of T

ther-mophilus EF-G are limited by crystal contacts between

domains G¢ and IV, which form an extended b-sheet

between the two domains [15,33] By crystallizing

EF-G from another species, S aureus, we have

obtained a new crystal packing arrangement that

avoids this problem

Furthermore, the only existing data on the

confor-mation of EF-G in solution come from small-angle

scattering measurements on T thermophilus EF-G

[23] These measurements resulted in radii of

gyra-tion in the range 30.2–32.9 A˚ for EF-G bound to

different nucleotides, and the difference between the

different states was judged to be nonsignificant as

compared with the experimental errors The

calcu-lated radius of gyration from the S aureus EF-G

crystal structure is 30.6 A˚, whereas the corresponding

value for T thermophilus EF-G [Protein Data Bank

(PDB) 1fnm] [16] is 30.5 A˚, agreeing equally well

with those measurements In conclusion, EF-G may

display larger interdomain flexibility in solution than

previously thought Our new conformation is

signifi-cant, as it demonstrates the size of the

conforma-tional space of EF-G when not bound to the

ribosome

The active conformation of EF-G is the one that

occurs on the ribosome So far, only

post-transloca-tional states, where domain IV of EF-G has entered

the A-site, have been visualized on the ribosome

[18–22] The ribosome-bound EF-G conformations in

the presence of GMPPNP or GDP and FA differ by

approximately 6 A˚ in position of the tip of domain

IV when the G-domains are superimposed (Fig 2C,

points 1 and 2) However, there is, at present, no

structural information regarding the initial binding of

EF-G to a presumably ratcheted ribosome where

the 30S A-site is still occupied by the peptidyl

tRNA Most likely, ribosome binding induces a

somewhat stable but transient conformation of EF-G

that is compatible with a tRNA in the 30S A-site,

and we can only speculate that this conformation of

EF-G may be more similar to either of the

confor-mations observed in the crystal structures of free

EF-G

FA resistance mutations

FA binds to EF-G on the ribosome and prevents its dissociation after GTP hydrolysis and translocation In the recent crystal structure of a 70S–EF-G complex [22] (Fig 1B), it is shown that FA allows the switch I region to change from a GTP to a GDP conformation, whereas the switch II region is prevented from adopt-ing its GDP conformation This, in turn, stops the glo-bal conformational change of EF-G to the GDP state that would leave the ribosome In other words, FA locks EF-G in a conformation between its GTP and GDP forms that cannot dissociate from the ribosome

FA resistance mutations belong to three classes: fusA mutants, with mutations in the EF-G gene; fusB, fusC and fusD mutants, which express a resistance pro-tein that somehow protects the cell from FA inhibi-tion; and fusE mutants, with mutations in ribosomal protein L6 [27]

There are, in total, 42 positions in EF-G where point mutations of the fusA class have been reported

to cause FA resistance [27,34,35] (Fig 4A) The previ-ous analysis of these [16] was performed without accu-rate knowledge of the FA-binding site [22], and, in addition, new mutations have recently been identified [27] On the basis of analysis of the S aureus EF-G structure together with the recent T thermophilus EF-G–70S complex structure with FA [22], we can now classify the mutations into four groups, A–D (Table 2) These perturb four critical parameters for locking

EF-G to the ribosome: drug binding (A), ribosome–EF-EF-G interactions (B), EF-G conformation (C), and EF-G stability (D) Several mutations seem to affect more than one of these parameters; for example, EF-G con-formation and stability are intimately linked to FA binding as well as ribosome binding

Group A mutations involve residues in direct con-tact with FA as well as residues that shape the drug-binding pocket These resistance mutations will directly alter drug–EF-G interactions, probably lowering the affinity of FA for the ribosome-bound EF-G The switch II loop directly contributes to the FA-binding site, where both Thr82 and Phe88 are in direct contact with FA in the ribosome complex structure [22] Muta-tion of the corresponding residues in T thermophilus (Thr84 and Phe90) also leads to resistance [36]

One edge of the FA-binding pocket is formed by domain III [22] A cluster of mutation sites is located

in this area, where the C-terminal end of helix AIII

packs against the central part of helix BIII (Fig 4B) Asp434 and Thr436 in helix AIII both form hydrogen bonds with His457 in helix BIII Thus, the mutations P435Q, T436I, H457Y and P435Q will change this

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5G

5G

CG

CG

CG

CG

DG

CG

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AIII

Leu Arg Gln

AIII

AIII

AIII

BIII

AIII

AIII

BIII

AIII

Ser Cys Val

BIII

BIII

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BIII

BIII

BIII

BIII

Ser His Leu Cys

BIII

AIII

AV

AV

2V

3V

BV

BV

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