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Tiêu đề Protein farnesyltransferase inhibitors interfere with farnesyl diphosphate binding by rubber transferase
Tác giả Christopher J. D. Mau, Sylvie Garneau, Andrew A. Scholte, Jennifer E. Van Fleet, John C. Vederas, Katrina Cornish
Trường học University of Alberta
Chuyên ngành Biochemistry
Thể loại báo cáo khoa học
Năm xuất bản 2003
Thành phố Edmonton
Định dạng
Số trang 7
Dung lượng 304,19 KB

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In an effort to characterize the catalytic site of rubber transferase, the effects of two types of protein farnesyltransferase inhibitors, several chaetomellic acid A analogs 2, 4–7 and a-

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Protein farnesyltransferase inhibitors interfere with farnesyl

diphosphate binding by rubber transferase

Christopher J D Mau1, Sylvie Garneau2, Andrew A Scholte2, Jennifer E Van Fleet1, John C Vederas2 and Katrina Cornish1

1

USDA, Agricultural Research Service, Western Regional Research Center, Albany, CA, USA;2Department of Chemistry, University of Alberta, Edmonton, Alberta, Canada

Rubber transferase, a cis-prenyltransferase, catalyzes the

addition of thousands of isopentenyl diphosphate (IPP)

molecules to an allylic diphosphate initiator, such as farnesyl

diphosphate (FPP, 1), in the presence of a divalent metal

cofactor In an effort to characterize the catalytic site of

rubber transferase, the effects of two types of protein

farnesyltransferase inhibitors, several chaetomellic acid A

analogs (2, 4–7) and a-hydroxyfarnesylphosphonic acid (3),

on the ability of rubber transferase to add IPP to the allylic

diphosphate initiator were determined Both types of

com-pounds inhibited the activity of rubber transferases from

Hevea brasiliensis and Parthenium argentatum, but there

were species–specific differences in the inhibition of rubber transferases by these compounds Several shorter analogs

of chaetomellic acid A did not inhibit rubber transferase activity, even though the analogs contained chemical features that are present in an elongating rubber molecule These results indicate that the initiator-binding site in rubber transferase shares similar features to FPP binding sites in other enzymes

Keywords: Hevea brasiliensis; Parthenium argentatum; chaetomellic acid A; hydroxyfarnesylphosphonic acid

Rubber transferase catalyzes the biosynthesis of natural

rubber [1] To form this polymer of cis-polyisoprene, rubber

transferase adds up to thousands of molecules of

isopente-nyl diphosphate (IPP) to a single initiating allylic

diphos-phate, usually considered to be farnesyl diphosphate (FPP,

1, Fig 1) as the in vivo substrate However, rubber

transferase can also use other allylic diphosphates as

initiators; this substrate flexibility is probably a reflection

on the manner in which the catalytic site deals with the

elongating rubber polymer In addition, a divalent metal

cofactor, such as Mg2+, is required In spite of the

dependence of modern industrial society on natural rubber,

the biochemical properties of rubber transferase are only

partially understood [1–6]

Several compounds are known to bind to FPP sites in

other enzymes that use FPP as a substrate Most of these

substances have been discovered as a result of oncogenesis

studies involving protein farnesyltransferases

Chaetomel-lic acid A (2) (Fig 1), made by Chaetomella acutiseta, is an

inhibitor of protein farnesyltransferases (PFTs), such as

those that modify Ras, and competes for the FPP binding

site of PFTs with an IC50 of 55 nM [7] Derivatives of

chaetomellic acid A have also been found to inhibit PFTs [8] a-Hydroxyfarnesylphosphonic acid (HFPA, 3) (Fig 1)

is another compound shown to inhibit PFTs [9] with an

IC50of 30 nM[7]

In an effort to characterize the FPP binding site of rubber transferase, we have tested the ability of chaetomellic acid A and several analogs, as well as HFPA, to inhibit rubber biosynthesis in vitro We have used rubber transferases from Hevea brasiliensisand Parthenium argentatum to determine

if there are similarities in enzymatic behavior that might be characteristic of rubber transferases in general, as well as species-specific differences

Materials and methods Chemicals

Chemicals were purchased from Sigma Chemical Com-pany unless otherwise noted Farnesyl diphosphate (FPP), dimethyl allyl diphosphate (DMAPP) and [1-14C]IPP (2.04 GBqÆmmol)1) were purchased from American Radiolabe-led Chemicals, Inc (St Louis, MO, USA) a-Hydroxy-farnesylphosphonic acid (HFPA) was purchased from Calbiochem-Novabiochem Corp Washed rubber particles (WRP) from P argentatum and H brasiliensis were purified ([10,11], respectively) and stored in liquid nitrogen [12]

Synthesis of chaetomellic acid A analogs Several analogs of chaetomellic acid, purified as lithium salts, were made according to Ratemi et al [8] The structures of (Z)-2-octyl-3-methylbutenedioic acid dilithium

Correspondence to K Cornish, Western Regional Research Center,

USDA-ARS 800 Buchanan Street, Albany, CA 94710, USA.

Fax: + 1 510 559 5663, Tel.: + 1 510 559 5950,

E-mail: kcornish@pw.usda.gov

Abbreviations: DMAPP, dimethyl allyl diphosphate; FPP, farnesyl

diphosphate; IPP, isopentenyl diphosphate; HFPA,

a-hydroxyfarne-sylphosphonic acid; PFT, protein farnesyltransferase; WRP, washed

rubber particles; UDP, undecaprenyl diphosphate.

(Received 5 June 2003, revised 8 July 2003, accepted 31 July 2003)

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salt (4) (Z)-2-nerolyl-3-methylbutenedioic acid dilithium salt

(5) (Z)-2-farnesyl-3-methylbutenedioic acid dilithium salt

(6), and (Z)-2-geranyl-3-methylbutenedioic acid dilithium

salt (7) are shown in Fig 1 Concentrated stock solutions of

chaetomellic acid A analogs (4–7) were prepared in

dimethylsulfoxide at 2 mM

Reaction conditions

Rubber transferase assays were performed in multiwell

plates as described in Mau et al [13] The typical reaction

assay contained 1 mM [1-14C]IPP (7.03 MBqÆmmol)1),

1.25 mM MgSO4, 5 mM dithiothreitol and 100 mM Tris

pH 7.5 in a total volume of 50 lL Various concentrations

of initiators (FPP or DMAPP) were added, ranging from

10 pM to 1 mM, along with the stated concentrations of

chaetomellic acid A analogs (4–7) or HFPA (3) (that was

dissolved in ethanol) For rubber transferase assays (all

performed in triplicate), 0.5 mg of H brasiliensis WRP

was used; 0.25 mg of WRP was used per assay involving

P argentatum rubber transferase The reactions were

started by the addition of WRPs to the other components

and were incubated at 25°C for H brasiliensis WRP and

16°C for P argentatum WRP The assays were incubated

for 4 h and were stopped by the addition of 0.5MEDTA

pH 8 to a final concentration of 20 mM The incorporated

14C was measured by liquid scintillation counting of the

newly synthesized rubber which had been trapped on

filters and subsequently washed to remove unincorporated

[14C]IPP

Results Effects of various organic solvents and lithium salts

on rubber transferase activity Prior to the first assays involving the analogs, several organic solvents that could be used to dissolve the chaeto-mellic acid A analogs were added to the standard rubber transferase assay [13] to determine what effects the presence

of these solvents had on enzymatic activity The range of concentrations tested were typical working dilutions Dimethylsulfoxide and ethanol did not inhibit rubber transferase activity at the final concentration of 10% (v/v)

in the rubber transferase assay, so these were the chosen conditions for conducting the inhibitor studies (data not shown)

As the chaetomellic acid A analogs (4–7) were synthes-ized as lithium salts, the effect of lithium cations on rubber transferase activity was also evaluated The presence of LiCl

in the amounts of 1 lM to 1 mM did not affect rubber transferase activity (data not shown)

As a result, all subsequent assays involving analogs 4–7 were compared to internal controls containing comparable amounts of LiCl and dimethylsulfoxide Within any experiment in which the chaetomellic acid A analogs were diluted serially, the final dimethylsulfoxide concentration was kept constant at 10% Assays involving HFPA were compared to control reactions supplemented with ethanol, and serial dilutions of HFPA were made to maintain a final ethanol concentration of 10%

Fig 1 Structures of various chemicals tested for effects on rubber transferase activity in vitro Farnesyl diphosphate 1 is the presumed initi-ator in vivo Chaetomellic acid A (SG-2–29, 2) and a-hydroxyfarnesylphosphonic acid (HFPA, 3) are known inhibitors of protein farnesyltransferases, which covalently modify proteins with a FPP molecule (Z)-2-octyl-3-methylbutenedioic acid dilithium salt (SG-2–96, 4) (Z)-2-nerolyl-3-methyl-butenedioic acid dilithium salt (SG-1–27, 5) (Z)-2-farnesyl-3-methylbutenedioic acid dilithium salt (SG-1–29, 6), and (Z)-2-geranyl-3-methylbutenedioic acid dilithium salt (SG-1–30, 7) are analogs of chaetomellic acid A.

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Chaetomellic acid A analogs inhibit rubber transferase

Hevea brasiliensis Incubating H brasiliensis WRP with

20 lM chaetomellic acid A (2) and varying amounts of

DMAPP or FPP initiator in a rubber transferase enzymatic

assay demonstrated that chaetomellic acid A (2) was

inhi-bitory when present at 20-fold molar excess of DMAPP or

200-fold molar excess FPP (Fig 2) The related compound

4 inhibited H brasiliensis rubber transferase by 40% when

included at 180 lMin the presence of 10 nMFPP (data not

shown)

Compounds 5, 6 and 7 (Fig 1) were tested for inhibitory

effects on H brasiliensis rubber transferase in vitro

Com-pound 5 was made to resemble the first cis-elongation

product formed when using DMAPP as an initiator, while

compounds 6 and 7 were synthesized to resemble FPP and

geranyl diphosphate, respectively Compound 6 inhibited

activity by 25% when present in the assay at 180 lM in

1800-fold molar excess of FPP Compounds 5 and 7 were

not inhibitory when included in the assay at 180 lMin over

a million-fold molar excess of initiator

Parthenium argentatum All five chaetomellic acid A

ana-logs (2, 4, 5, 6 and 7) were tested using the rubber transferase

from guayule, P argentatum, a species phylogenetically

distant from H brasiliensis Compounds 2 and 6 reduced

rubber transferase activity by 27% (when added at 180 lM

in a 18,000-fold molar excess) and by 48% (when present

at 180 lM in a 180-fold molar excess), respectively

Compounds 4, 5 and 7 did not inhibit rubber transferase

activity under the conditions tested (supplemented in the

assay at 180 lMin over a million-fold molar excess)

Because compounds 2 and 6 were more inhibitory than 4

and 7, respectively, the long hydrophobic tails on these

molecules might have some important role in determining efficacy of inhibition To examine this possibility, palmitic acid and stearic acid were tested to see if either had any effect on rubber transferase activity When present at

180 lM, neither palmitate nor stearate inhibited IPP incor-poration into DMAPP- or FPP-initiated newly synthesized rubber by H brasiliensis or P argentatum (data not shown)

a-Hydroxyfarnesylphosphonic acid also inhibits rubber transferases As chaetomellic acid A had been described initially as an inhibitor of protein farnesyltransferase, another type of PFT inhibitor was also tested to determine

if it also could inhibit rubber transferase activity HFPA inhibited FPP utilization by H brasiliensis and P argent-atumWRP by 36–37% when present at 20 lMat 2000-fold molar excess

Determination of kinetic constants for chaetomellic acid

A analogs and HFPA Double reciprocal plots (1/v vs 1/[FPP]) of kinetic experiments indicated that compounds 2 and 3 were competitive inhibitors of H brasiliensis rubber transferase (Fig 3A,B), whereas compound 6 was a noncompetitive inhibitor (Fig 3C) In contrast, all three compounds behaved as competitive inhibitors of the

P argentatumrubber transferase (Fig 4A–C)

The apparent Kis for the chaetomellic acid A analogs and HFPA were determined from plots (not shown) of the slope

of the each reciprocal plot vs the concentration of the inhibitory compound [14] (Table 1)

Discussion Rubber transferases exhibit a considerable degree of toler-ance and can bind to a variety of different sizes of allylic diphosphate initiator molecules, at least up to solanesyl (C45) diphosphate (M H Chapman and K Cornish, unpublished data) Furthermore, the affinity of rubber transferase for the initiator increases with the size of the initiator, up to FPP (C15) in P argentatum and geranylger-anyl diphosphate (C20) in H brasiliensis As a result, a model was proposed for the rubber transferase active site, envisioning the presence of non–specific hydrophobic interactions, which increased the affinity for longer allylic diphosphate substrates [15] Nevertheless, it was uncertain if the chaetomellic acid analogs with the diacid groups could occupy the initiator-binding site with enough affinity to inhibit rubber biosynthesis

As seen in Fig 2, chaetomellic acid A (2) was able to interfere with IPP incorporation in the rubber transferase assay Almost 10-times more DMAPP than FPP was needed to overcome the same degree of inhibition by chaetomellic acid A (2) (Fig 2) The ability of DMAPP or FPP to displace chaetomellic acid A from the initiator-binding site in H brasiliensis rubber transferase paralleled the ninefold lower affinity of the enzyme for DMAPP vs FPP (Km,DMAPPof 13.2 and Km,FPPof 1.5 lM[1]) The length of the hydrophobic carbon tail also affected the inhibitory activity of the chaetomellic acid A analogs Compound 6, which has a farnesyl tail, was weakly inhibitory at 180 lM, in both species, whereas 7, which has a shorter geranyl tail, was not inhibitory at all

Fig 2 Chaetomellic acid A inhibits H brasiliensis rubber transferase.

Assays were performed using H brasiliensis WRP, 1 m M [14C]IPP, an

allylic diphosphate initiator, and either chaetomellic acid A (SG-2–29)

or its analog SG-2–96 DMAPP was varied in the presence of 20 l M

SG-2–29 (d) or 20 l M SG-2–96 (s), while various concentrations of

FPP were tested in combination with 20 l M SG-2–29 (.) The amount

of [ 14 C]IPP incorporated in these reactions was compared to control

reactions containing dimethylsulfoxide and LiCl instead of the

chaetomellic acid A analogs.

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Chaetomellic acid A (2) with a 14-carbon aliphatic chain strongly inhibited H brasiliensis rubber transferase at

20 lMwhile 4, with a similar structure but having a shorter 8-carbon tail, required 180 lMbefore it became inhibitory

On the other hand, P argentatum rubber transferase activity was only weakly inhibited by 180 lMchaetomellic acid A (2) and not at all by 180 lMcompound 4 In both cases, lengthening the hydrophobic surface of the analog added additional interactions, which increased the binding affinity of the inhibitor for the initiator-binding site The difference in the inhibition of H brasiliensis and P argent-atumrubber transferases by chaetomellic acid A indicated that there may be differences in the catalytic site geometry between the two species

However, a hydrophobic aliphatic tail simply attached to

a negative charge is not the sole cause of the observed inhibitory activity, because neither palmitic nor stearic acid was inhibitory in either species (data not shown) High affinity binding of substrates in the catalytic site appears to require two negatively charged oxygen atoms at one end of the molecule

These criteria are met by a-hydroxyfarnesylphosphonic acid (3), which did inhibit rubber transferase activity in both species That two types of protein farnesyltransferase inhibitors could also interfere with rubber transferase, a cis-prenyltransferase, indicates that the initiator binding site

of rubber transferase shares similarities with the FPP binding site of the protein farnesyltransferases

For P argentatum rubber transferase, compounds 2, 3 and 6 all appear to inhibit FPP binding (and subsequent IPP incorporation) competitively (Figs 4A–C) In contrast, although 2 and 3 both competitively inhibited the H bra-siliensis rubber transferase (Figs 3A,B), 6 acted in a noncompetitive manner (Fig 3C)

The calculated Kis show that the active sites of

H brasiliensisand P argentatum rubber transferases have

a higher affinity for 2 than for 6 (Table 1) While the allylic compound 6 more closely resembles the FPP initiator, compound 2 with its more flexible aliphatic backbone probably makes more extensive contact with the nonspecific hydrophobic surface lining the catalytic cavity [15] Alternatively, the difference in length of the inhibitors allows 2 to interact with the polyisoprene molecules within the rubber particle In both cases, the additional interactions result in tighter binding of 2 when compared to that of 6

The interpretation of the double reciprocal plots must be qualified because the rubber transferase active site is localized on the surface of a rubber particle [15] This proximity to the membrane monolayer covering the rubber particle would preclude access to the active site from certain directions during the in vitro reactions In addition, experi-mental manipulations of washed rubber particles can be challenging

The binding of competitive inhibitors and substrates are mutually exclusive, which is not the case for noncompetitive inhibitors Non-competitive inhibition results when binding

of an inhibitor at a second site prevents catalysis at the normal active site, without causing any changes in the binding kinetics at the active site The P argentatum rubber transferase can only bind 6 in a manner which affects the apparent binding at the initiator substrate site On the other

Fig 3 Chaetomellic acid A and SG-1–29 are inhibitors of H

brasil-iensis rubber transferase Double reciprocal plots of 1/v vs 1/[FPP]

were created using kinetic data from H brasiliensis rubber transferase

assays Rubber transferase assays were conducted in the presence of

H brasiliensis WRP, 1 m M [14C]IPP, and the indicated amounts of

FPP v is measured in units of lmol [14C]IPP incorporated per g dry

weight rubber per 4 h (A) Chaetomellic acid A (SG-2–29) was

inclu-ded at concentrations of 10 (.), 20 (s) or 50 (d) l M during the assay

while FPP was varied from 10 n M to 100 n M (B) HFPA was present at

10 (.), 20 (s), or 40 (d) l M while FPP was varied from 10 n M to

50 n M (c) SG-1–29 was added at final concentrations of 50 (.), 100

(s), or 200 (d) l M while FPP was varied from 10 n M to 100 n M

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hand, the noncompetitive inhibition by 6 of H brasiliensis rubber transferase may be caused by interference resulting from the additional binding of compound 6 at the IPP binding site, which is in the proximity of the allylic diphosphate binding site Competition between IPP and allylic diphosphate for the IPP binding sites has been observed at high substrate concentrations [1,16], and 6 was present at a range of 2500 to 10 000-fold molar excess to FPP in the assay (30- to 130-times the Kmfor FPP [17]) These results suggest that the spatial orientation between the IPP and initiator binding sites differs between the two rubber transferases, as well as the ability to bind 6 at other surfaces within the active site

The different behavior between the two rubber trans-ferases towards 6 should also be considered in light of the cooperative effects between IPP and FPP if one assumes that 6 is perceived as FPP by both enzymes In the range of concentrations of 6 incubated in the assays, the two rubber transferases exhibit different degrees of negative coopera-tivity, with the P argentatum enzyme showing the strongest effect [17] Under these conditions, binding of the first initiator molecule decreases the ability of a free FPP to displace the bound FPP (or elongating polymer) The ability

of the FPP-like compound 6 to bind noncompetitively at an additional location within the H brasiliensis active site may explain some of differences in the degree of negative cooperativity between the two enzymes Furthermore, the development of the P argentatum rubber transferase with a low Kmfor FPP (about 150-fold lower in concentration than the corresponding constant for H brasiliensis [17]) may also explain the difference in degree of negative cooperativity, because compound 6 can bind competitively into the initiator site of the P argentatum enzyme, unlike the noncompetitive binding in the vicinity of the weaker affinity initiator binding site of the H brasiliensis protein More experimentation to elucidate the mechanism of the negative cooperativity can be performed, but the basis for this behavior will probably only become apparent after the crystal structures of the rubber transferases have been determined

The differing behavior of the various compounds tested, both in the amount of compound needed to create an observable effect and the different types of inhibition effected, supports earlier kinetic data on cosubstrate effects among the species [16,17] Differences in binding constants, competitive effects, and in substrate activation exist between species [1,15–17] Thus, although the rubber transferases

Fig 4 SG-1–29 and HFPA are competitive inhibitors of P argentatum

rubber transferase Double reciprocal plots of 1/v vs 1/[FPP] were

created using kinetics data from P argentatum rubber transferase

assays Rubber transferase assays were conducted in the presence of

P argentatum WRP, 1 m M [ 14 C]IPP, and the indicated amounts of

FPP v is measured in vitro of lmol [ 14 C]IPP incorporated per g dry

weight rubber per 4 h (A) Chaetomellic acid A (SG-2–29) was added

at 50 (.), 100 (s), or 200 (d) l M while FPP was varied from 1.3 n M to

50 n M (B) Assays contained HFPA at concentrations of 100 (.), 200

(s), or 500 (d) l M while FPP was varied from 5 n M to 100 n M (C)

SG-1–29 was present at final concentrations of 50 (.), 100 (s), or 200

(d) l M while FPP was varied from 5 n M to 100 n M

Table 1 Kinetic constants determined for the interaction between cha-etomellic acid A analogs or a-hydroxyfarnesylphosphonic acid with

H brasiliensis and P argentatum rubber transferases.

Compound

H brasiliensis P argentatum

K i (l M )

Type of competitor K i (l M )

Type of competitor SG-2–29 (2) 42 competitive 8.8 competitive HFPA (3) 64 competitive 420 competitive SG-1–29 (6) 140 noncompetitive 25 competitive

Trang 6

from different species share many commonalities, they are

not identical These differences may have resulted from

evolutionary divergence alone or in combination with the

development of a different cellular environment for the

rubber transferase in each species; H brasiliensis rubber

transferase is found on rubber particles in a free-flowing

latex in laticifers, while P argentatum rubber transferase

is located on intracellular rubber particles in the bark

parenchyma

The discovery that compounds known to bind to other

FPP binding sites can interact with the initiator binding site

of rubber transferases opens a new approach to modeling

the catalytic site of this enzyme in the absence of crystal

structures We have already used other biochemical and

physical studies to elucidate some features of the catalytic

site [1,18]

Recently, two crystal structures of undecaprenyl

diphosphate (UDP) synthase, a cis-prenyltransferase that

catalyzes the formation of a 55-carbon carrier for glycosyl

residues in peptidoglycan synthesis in bacteria, have been

published [19,20] Information from these structures may be

helpful in our efforts to model the rubber transferase active

site because both enzymes are cis-prenyltransferases with

proposed catalytic sites near the cytosolic surface of the

membrane The active site contains a cleft flanked by

hydrophobic amino acids that surrounds the aliphatic

backbone of the substrate [20] The chain length is

apparently regulated by the size of the active site, and

site-directed mutants, in which bulky, hydrophobic residues at

the distal end of the catalytic site have been converted to

alanine, can produce longer polyprenyl molecules Similar

mutagenesis of the avian FPP synthase catalytic site also

extends the size of the product formed [21] These structures

suggest that the rubber transferase has a hydrophobic

channel to direct the elongating biopolymer, in this case to

the rubber particle interior [1,15,18] Unlike the UDP

synthase and the FPP synthase, rubber transferase appears

to lack the bulky hydrophobic residues at the distal end of

the active site The normal mechanism for releasing the

rubber molecule from the enzyme has not been determined

Thus, the results presented here further support the

proposed model for the rubber transferase active site in

which the presence of non–specific hydrophobic interactions

increase the affinity for longer allylic diphosphate substrates

[1,15] These results also indicate that structural differences

do exist between the rubber transferases from evolutionarily

divergent species

Acknowledgements

We thank Dr R Krishnakumar at the Rubber Research Institute of

India for supplying the H brasiliensis latex as a source for WRP and

Dr Francis Nakayama at the US Water Conservation Laboratory in

Phoenix, AZ for maintaining and harvesting P argentatum plants for

isolation of the P argentatum WRP used in experiments described here.

We also acknowledge the help of Ms Mary H Chapman and Dr Javier

Castillo´n for isolating the H brasiliensis and P argentatum WRP used

in our experiments Ms Saima Kint and Dr Thomas McKeon kindly

provided palmitic and stearic acids for control experiments Part of this

work has been supported by the Natural Sciences and Engineering

Research Council of Canada and the Alberta Heritage Foundation for

Medical Research.

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19 Fujihashi, M., Zhang, Y.-W., Higuchi, Y., Li, X.-Y., Koyama, T.

& Miki, K (2001) Crystal structure of cis-prenyl chain elongating enzyme, undecaprenyl diphosphate synthase Proc Natl Acad Sci USA 98, 4337–4342.

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21 Tarshis, L.C., Proteau, P.J., Kellogg, B.A., Sacchettini, J.C & Poulter, C.D (1996) Regulation of product chain length by iso-prenyl diphosphate synthases Proc Natl Acad Sci USA 93, 15018–15023.

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