1 Transcriptomic and Proteomic Insight into the Mechanism of Cyclooctasulfur- versus

2 -Oxidation by the Chemolithoautotroph Sulfurimonas denitrificans

3

4 Florian Götz1,2,#, Petra Pjevac3,#, Stephanie Markert2,5, Jesse McNichol1,6, Dörte Becher7,

5 Thomas Schweder2,5, Marc Mussmann3,4, Stefan M. Sievert1,*

6

7 1Biology Department, Woods Hole Oceanographic Institution, Woods Hole, MA 02543, USA

8 2Department of Pharmaceutical Biotechnology, Institute of Pharmacy, University of Greifswald, 9 D-17487 Greifswald, Germany

10 3Division of Microbial Ecology, Department of Microbiology and Science, Research 11 Network ‘Chemistry Meets Microbiology’, University of Vienna, Althanstr- 14, 1090, Vienna, 12 Austria

13 4Department of Molecular Ecology, Max Planck Institute for Marine Microbiology, Celsiusstr. 1, 14 28359 Bremen, Germany

15 5Institute of Marine Biotechnology, Walther-Rathenau-Strasse 49, D-17489 Greifswald, 16 Germany.

17 6Present Address: Department of Biological Sciences, University of Southern California, Los 18 Angeles, CA 90089

19 7Institute of Microbiology, University of Greifswald, D-17487 Greifswald, Germany

20 #Contributed equally to this work

21 *corresponding author; email: [email protected]

22

23 Running title: S8 in Sulfurimonas denitrificans

1 24 Originality-Significance Statement: To the best of our knowledge, this is the first proteomic

25 and transcriptomic study of a chemolithoautotrophic campylobacterium, using Sulfurimonas

26 denitrificans as a model organism. To date, Sulfurimonas denitrificans is the only neutrophilic

27 with the demonstrated capability of cylcooctasulfur (S8) oxidation. However, the

28 mechanism by which this is accomplished is not known. Our results provide insight into the

29 active metabolism of S. denitrificans, revealing for the first time a differential regulation of the

30 -oxidation multienzyme complex (SOX) in response to the provided sulfur substrates.

31 Based on these findings, a model for the oxidation of S8 is proposed that might also apply to

32 other sulfur-oxidizing Campylobacteria that have been identified as key players in the oxidation

33 of zero-valence sulfur, a central intermediate in the sulfur cycle.

2 34 Abstract

35 Chemoautotrophic belonging to the genus Sulfurimonas (class Campylobacteria)

36 were previously identified as key players in the turnover of zero-valence sulfur, a central

37 intermediate in the marine sulfur cycle. S. denitrificans was further shown to be able to oxidize

38 cyclooctasulfur (S8). However, at present the mechanism of activation and metabolism of

39 cyclooctasulfur is not known. Here, we assessed the transcriptome and proteome of S.

40 denitrificans grown with either thiosulfate or S8 as the electron donor. While the overall

41 expression profiles under the two growth conditions were rather similar, distinct differences were

42 observed that could be attributed to the utilization of S8. This included a higher abundance of

43 expressed related to surface attachment in the presence of S8, and the differential

44 regulation of the sulfur-oxidation multienzyme complex (SOX), which in S. denitrificans is

45 encoded in two clusters: soxABXY1Z1 and soxCDY2Z2. While the proteins of both clusters

46 were present with thiosulfate, only proteins of the soxCDY2Z2 were detected at significant levels

47 with S8. Based on these findings a model for the oxidation of S8 is proposed. Our results have

48 implications for interpreting metatranscriptomic and -proteomic data and for the observed high

49 level of diversification of soxY2Z2 among sulfur-oxidizing Campylobacteria.

50

51

3 52 Introduction

53 Sulfur occurs in many oxidation states and is of central importance in biogeochemical

54 cycles (Sievert et al., 2007). As an essential component of biomass, sulfur is assimilated into

55 organic compounds and is also involved in energy yielding processes either as electron acceptor

56 or donor in chemolithautotrophic, photolithoautotrophic, and heterotrophic

57 (Kletzin et al., 2004; Friedrich et al., 2005; Robertson and Kuenen, 2006; Sievert et al., 2007;

58 Finster, 2008; Dahl et al., 2008; Sievert and Vetriani, 2012). In various environments, elemental

59 sulfur accumulates in amounts visible to the naked eye, including marine sediments, microbial

60 mats, hydrothermal vents, glacial shields, minimum zones and volcanic soils (Ruby et

61 al., 1981; Woodruff and Shanks, 1988; Raiswell, 1992; Taylor and Wirsen, 1997; Alonso-

62 Azcárate et al., 2001; Engel et al., 2004; Zopfi et al., 2004; Lavik et al., 2009; Cosmidis and

63 Templeton, 2016; Lau et al., 2017). In these cases, sulfur occurs mostly in the form of zero-

0 64 valence sulfur (S ) with cyclooctasulfur (S8) as the most stable and common form (Steudel and

65 Eckert, 2003).

2- 0 66 During microbial sulfide (S ) oxidation, S in the form of S8, polymeric sulfur (Sµ) or

67 sulfur chains is often produced and deposited as an intermediate oxidation product (Friedrich et

68 al., 2001; Prange et al., 2002; Dahl and Prange, 2006; Sievert et al., 2007; 2008). In various S0-

69 rich natural and engineered environments, members of the genus Sulfurimonas and other sulfur-

70 oxidizing Campylobacteria, such as Sulfurovum and Sulfuricurvum, are highly abundant

71 (Macalady et al., 2008; Legatzki et al., 2011; Hubert et al., 2012; Meyer et al., 2013; Pjevac et

72 al., 2014; Gulmann et al., 2015; Zhang et al., 2015; Li et al., 2016; McNichol et al., 2016). It has

0 73 been proposed that especially Sulfurimonas and Sulfurovum species occupy the niche for S /S8

74 oxidation in marine sediments and at hydrothermal vents (Pjevac et al., 2014; Meier et al., 2017).

4 75 Considering the extremely low solubility and reactivity of S8 (Kamyshny, 2009; Franz et al.,

76 2007; Pjevac et al., 2014), neutrophilic S8-oxidizing microorganisms most likely need a specific

77 activation or solubilization mechanism to make S8 available for their energy metabolism, as has

78 been shown for acidophilic sulfur-oxidizing bacteria (Rohwerder and Sand, 2003; Mangold et

79 al., 2011; Chen et al., 2012). To date, Sulfurimonas denitrificans, the type strain of the genus

80 Sulfurimonas, is the only neutrophilic microorganism with the demonstrated capability of S8

81 oxidation (Pjevac et al., 2014).

82 S. denitrificans, a member of the globally distributed genus Sulfurimonas (Han and

83 Perner, 2015), was initially isolated from coastal marine sediments with thiosulfate and nitrate as

0 84 substrates, but subsequent studies showed that it can also use H2S, S , S8, and (H2) as

85 electron donors (Timmer-Ten Hoor, 1975; Sievert et al., 2008; Pjevac et al., 2014). S.

86 denitrificans is thought to use the sulfur-oxidation multienzyme complex (SOX) for the

87 oxidation of reduced sulfur compounds (Friedrich et al., 2005, 2001; Sievert et al., 2008), which

88 was previously shown for the campylobacterium Sulfurovum sp. NBC37-1 (Yamamoto et al.,

89 2010). While genes of the SOX system in the model organism Paracoccus pantotrophus

90 (Friedrich et al., 2001; 2005) are found in one operon (soxABCDXYZ), S. denitrificans and other

91 Campylobacteria possess two operons of the sulfur oxidation system (SOX) (Sievert et al., 2008;

92 Yamamoto and Takai, 2011). One operon encodes the soxABX cluster and one of the two soxYZ

93 copies (Y1Z1), while the other operon encodes the soxCD genes and a second, highly divergent

94 soxYZ copy (Y2Z2) (Sievert et al., 2008; Meier et al., 2017). These two clusters were previously

95 hypothesized to be differentially regulated, for example in response to the availability of

96 different sulfur compounds (Sievert et al., 2008; Meier et al., 2017; Pjevac et al., 2018). Notably,

97 the differential expression of sox genes present in separate clusters has previously been reported

5 98 for the gammaproteobacterium Allochromatium vinosum (Hensen et al., 2006; Weissgerber et

99 al., 2013).

100 In the currently accepted model of the SOX multi- system, SoxYZ is the sulfur

101 carrier, and binds various reduced sulfur compounds covalently to a cysteine residue on SoxY,

102 which is coordinated by SoxAX (Quentmeier and Friedrich, 2001; Dahl and Prange, 2006;

2- 103 Grabarczyk and Berks, 2017). SoxB then hydrolyzes sulfate (SO4 ) to generate a cysteine-

104 persulfide left on SoxY. The sulfur dehydrogenase (Sox[CD]2) catalyzes the oxidation of the

105 outer sulfone sulfur of the cystein-persulfide on SoxY, which is subsequently hydrolyzed to

106 sulfate by SoxB (Friedrich et al., 2001, 2005). In a fully operational SOX pathway, sulfur is

107 oxidized to sulfate without a visible accumulation of sulfur intermediates in cells (Dahl and

0 108 Prange, 2006). In contrast, in a truncated SOX system lacking Sox(CD)2, S , Sµ or polysulfides

- 109 (Sn ) are formed as products of thiosulfate oxidation by the activity of SoxXYZAB (Friedrich et

110 al., 2005; Hensen et al., 2006). While work on acidophilic S0 oxidizers such as Acidithiobacillus

111 ferrooxidans or A. caldus has shown that the S8 ring is activated by reactive thiols and involves

112 outer membrane proteins (Rohwerder and Sand, 2003; Mangold et al., 2011; Chen et al., 2012),

113 the mechanism involved in the activation of insoluble and inert sulfur forms, like Sµ and S8, by

114 neutrophilic sulfur oxidizers such as S. denitrificans is at present unknown.

115 In order to investigate the mechanism of S8 oxidation in S. denitrificans, we analyzed and

116 compared its transcriptome and proteome under denitrifying conditions with either thiosulfate or

117 S8 as sole electron donors. Our results provide insight into the active metabolism of S.

118 denitrificans, revealing a differential regulation of the SOX system in response to the provided

119 sulfur substrate. Based on these findings, a model for the oxidation of cylcooctasulfur is

6 120 proposed that might also apply to other Campylobacteria that share the same genome

121 arrangement of the SOX system.

122

123 Material and Methods

124 Cultivation

125 Sulfurimonas denitrificans was grown in batch cultures at 22ºC in 2 L pyrex bottles

126 containing 1 L of artificial seawater medium (Timmer-Ten Hoor, 1975) purged with N2:CO2

127 (80:20, 1.1 atm) and sealed with butyl rubber stoppers. The bicarbonate concentration in the

128 medium was increased to 5 g L-1 to buffer the pH at approximately 7. Three replicate cultures

-1 -1 129 were supplemented with 5 g L S8 (S8-1, S8-2, S8-3), and two control cultures with 40 mmol L

130 thiosulfate (T-1, T-2) as electron donor. S8 for the experiments was freshly synthesized, as

131 described in Pjevac et al., (2014). Nitrate (20 mmol L-1) was added to all cultures as the electron

132 acceptor. In order to determine cell numbers, 4,6-Diamidino-2-phenylindole (DAPI) counts were

133 performed. Cells were harvested during exponential growth. For proteomics, 100 mL of culture

134 was harvested by centrifugation at 7,000 x g for 7 min at 20 °C in 50 mL centrifugation tubes.

135 For transcriptomics, 100 mL of culture was filtered onto 0.2 µm teflon filters and immediately

136 immersed in RNA later and stored at -20°C.

137 Protein isolation

138 For the isolation of proteins, cell pellets were resuspended in 1 mL 1x Tris-EDTA (TE)

139 buffer (pH 8; Sigma-Aldrich, St. Louis, MO, USA), containing cOmpleteTM Protease inhibitor

140 (Roche, Basel, Switzerland). To lyse cells, the suspensions were sonicated three times for 30 sec

141 at 5 x 10% amplitude using the Sonoplus HD2070 sonication probe (Bandelin, Berlin, Germany).

7 142 The obtained crude extracts were centrifuged for 10 min at 15,500 x g at 4°C. The raw protein

143 extracts (supernatants) were concentrated by means of Amicon tubes (Ultra-15 3 kDa cutoff

144 Merck Millipore, Kenilworth, NJ, USA), which were centrifuged for 30-60 min at 5,000 x g and

145 4°C as described in the manufacturer’s instructions. Protein concentrations were determined

146 using the Roti-Nanoquant protein assay (Carl Roth, Karlsruhe, Germany) as instructed by the

147 manufacturer. Subsequently, 4 x loading buffer (200 mmol L-1 Tris-HCl pH 6.8, 50 mmol L-1

148 EDTA pH 8.0, 40 % glycerol (v/v), 8 % SDS (w/v), 0.08 % bromophenol blue (v/v), 1 mmol L-1

149 dithiothreitol) was added to aliquots of ~25 µg protein, and samples were denatured for 10 min at

150 90°C. The denatured extracts and a Roti-Mark standard (Roti-Mark STANDARD, Carl Roth,

151 Karlsruhe, Germany) were transferred onto a polyacrylamide SDS mini gel (10% Mini-

152 PROTEAN, TGX Stain-free, BioRad, Hercules, CA, USA) and run approximately 20 min at 50

153 V and another 35 min at 150 V. The gel was fixed for 30 min in an ethanol: acetic acid: water

154 (40:10:50) solution. The gel was stained overnight in a Coomassie Brilliant Blue G250 (CBB)

155 staining solution (Carl Roth, Germany), followed by washing step in distilled water to remove

156 non-bound CBB before imaging of the protein bands.

157 Protein digestion

158 On a glass plate, cleaned with methanol and double distilled water (ddH2O), the entire

159 protein-containing gel lane was excised and divided into 10 equal-sized subsamples for each

160 sample. Each subsample was cut in small pieces and transferred into 2 mL Eppendorf cups. CBB

161 bound to the protein was removed by incubating the gel pieces multiple times in a wash solution

-1 162 containing 200 mmol L NH4HCO3 and 30% acetonitrile at 37°C for 30 min. De-stained gel

163 pieces were dried for 15 min in an Eppendorf Concentrator plus at 1,400 rpm, ambient

164 temperature and 20 mbar vacuum. For protein digestion, 2 µg mL-1 trypsin solution (Promega,

8 165 Madison, WI, USA) was added to dried gel pieces until covered (~50 µL) and incubated at room

166 temperature for 30 min. Additional trypsin was added to cover rehydrated gel pieces and

167 incubated at 37°C for 14-16 h. Thereafter, 50 µL ddH2O was added to the incubated gel pieces,

168 which were further sonicated for 15 min in an ultrasound bath (37 kHz, 600W \ FB15054

169 Fisherbrand) to elute the peptides. After sonication, the sample was centrifuged at 5,000 x g for

170 10 s. The peptide-containing supernatants were transferred into new tubes, and centrifuged at

171 250 x g under vacuum in an Eppendorf Concentrator to reduce the sample volume to 10 µL. The

172 10 µL peptide mixes were stored at -80 °C until measurement.

173 Mass spectrometry and proteome analysis

174 Peptide mixes were separated via chromatography on a reversed phase C18 column in a

175 nano-ACQUITY-UPLC (Waters Corporation, Milford, MA, USA) as described by Otto et al.

176 (2010). Mass spectrometry (MS) and MS/MS data were recorded with an online-coupled LTQ-

177 Orbitrap mass spectrometer (Thermo Fisher Scientific Inc., Waltham, MA, USA). MS data were

178 searched against a forward-decoy S. denitrificans protein database (Refseq Genome project:

179 NC_007575.1, NCBI [National Center for Biotechnology Information]), which also included

180 common laboratory contaminants, using Sequest (Thermo Fisher Scientific, San Jose, CA, USA;

181 v 27.11). The protein false discovery rate (FDR) was zero for all samples, with the exception of

182 one technical replicate of T-1, in which case the FDR was 0.2%. Identifications were filtered in

183 Scaffold (http://www.proteomesoftware.com) using the “Sequest” filter settings described by

184 Heinz et al., (2012). The total spectral count values of all proteins were exported for calculation

185 of the normalized spectral abundance factors (NSAF, Zybailov et al., 2006), which are given in

186 Supplementary Table 1. The average of the NSAF and the standard deviation were calculated for

187 the three biological replicates for S8 (S8 1-3). For thiosulfate, only two biological replicates were

9 188 available (T-1 and T-2). However, two technical replicates were run for sample T-1 to assess the

189 variability between runs. The NSAFs of the two technical replicates were averaged before being

190 averaged with the second biological replicate T-2 for statistical analyses. PSI-BLAST and

191 DELTA-BLAST (Boratyn et al., 2012) were used for domain analysis of hypothetical proteins.

192 We also used the tools BOCTOPUS (boctopus.bioinfo.se) and PRED-TMMB

193 (http://bioinformatics.biol.uoa.gr////PRED-TMBB) to search for beta-barrel topology. To detect

194 signal peptides, SignalP 4.0 (Petersen et al., 2011; http://www.cbs.dtu.dk/services/SignalP/) was

195 used. The mass spectrometry proteomics data are available through the ProteomeXchange

196 Consortium (http://proteomecentral.proteomexchange.org) via the PRIDE partner repository

197 (Vizcaino et al., 2016) with the dataset identifier PXD009127 (Reviewer account details:

198 Username: [email protected] Password: sj7sSWSj).

199 RNA extraction, transcriptome sequencing and analysis

200 The membrane filters with the cells were cut in pieces, put in a microcentrifuge tube

201 containing extraction buffer provided with the mirVana miRNA isolation kit (Ambion, Carlsbad,

202 CA, USA), and subjected to bead-beating. Subsequently, total RNA was extracted using the

203 mirVana miRNA isolation kit, with subsequent turbo DNAse (Ambion) treatment and

204 purification with the Qiagen RNAeasy kit (Qiagen, Hilden, Germany) according to the

205 manufacturer’s instructions. Ribosomal RNA was not depleted. Total RNA extracts were sent to

206 the Max Planck Genome Centre (Cologne, Germany) for preparation of RNAseq-libraries and

207 subsequent sequencing of paired-end (2 x 150 bp) reads in the HiSeq2000 (Illumina).

208 Sequencing statistics are provided in Supplement Table 2. Sequence reads were quality trimmed

209 at a Phred score of 28 using the bbduk function of BBMap v35.82

210 (https://sourceforge.net/projects/bbmap/), and mapped to a reference file of all open reading

10 211 frames (ORFs) deposited in NCBI for the S. denitrificans genome (NCBI project NC_007575.1)

212 using the bbmap function of BBMap v35.82. Sequences were mapped as paired reads with a

213 minimal identity of 99%. For comparison between cultures (Supplement Table 1), read counts

214 were transformed to transcripts per million (TPM) values as described in Li et al. (2010). The

215 transcriptome sequence data has been deposited in the European Nucleotide Archive (ENA)

216 under the project accession number PRJEB25508.

217 Statistical analysis

218 To test for statistically significant differences between the two different growth

219 conditions, the NSAFs and TPMs of all biological replicates of each growth condition were used

220 as the input parameters to calculate P-values based on the Welch’s t-Test. Due to the small

221 number of biological replicates available for the thiosulfate treatment (n=2), the Welch’s rather

222 than the Student’s t-Test was selected as a more stringent manner to statistically evaluate

223 differences in gene transcription and protein expression between the two conditions. Transcripts

224 and proteins with a P-value smaller than 0.05 were considered to be statistically significantly

225 different between the two conditions.

226

227 Results

228 Growth characteristics

229 The growth rate of thiosulfate-grown cultures was 1.8-times higher compared to cultures

-1 -1 230 grown on cyclooctasulfur (2.7 day vs. 1.5 day ), corresponding to a doubling time of ~6 h and

231 ~11 h for thiosulfate- and S8-grown cultures, respectively (Supplement Figure S1). Thiosulfate-

232 grown cultures also had a significantly shorter lag phase, which might be related to the easier

11 233 accessibility to thiosulfate than to S8. One of the three S8-grown cultures had a significantly

234 extended lag phase, but once growth started, the growth rate was similar to the other two

235 cultures.

236 The transcriptome and proteome of thiosulfate- versus S8-grown cells are largely similar

237 Transcriptomic and proteomic data were obtained from either thiosulfate- or S8-grown

238 cultures sampled in early exponential phase. Overall, reads mapping to 97.7 % of the genes in

239 the genome (2,114 and 2,104 out of 2,164) were detected in the transcriptome of cultures grown

240 with thiosulfate or S8, respectively. In the proteome, 38.8% and 37% of proteins encoded in the

241 genome (822 and 784 out of 2,119 protein coding genes) were identified in thiosulfate- and S8-

242 grown cultures, respectively (Table 1). 122 and 84 proteins were detected exclusively in

243 thiosulfate- and S8-grown cultures, respectively, while 176 and 200 proteins were identified in

244 only one of the analyzed replicates of thiosulfate- and in S8-grown cultures, respectively (Table

245 1).

246 In general, a classification into clusters of orthologous genes (COG) showed similar

247 profiles of transcribed protein coding genes and identified comparable sets of proteins between

248 thiosulfate- and S8-grown cultures (Figure 1). Genes of the translational apparatus (including

249 tRNA ligases and ribosomal subunits) accounted for up to one third of the classifiable transcripts

250 and proteins under both conditions, followed by transcribed genes and proteins of the energy

251 metabolism (Figure 1). The most apparent difference among functional genes is the increased

252 transcription level of genes that encode proteins of the flagellar apparatus in S8-grown cultures

253 (Figure 1).

12 254 Since transcriptome sequencing was performed without rRNA depletion to minimize

255 sample processing biases, the majority of the transcriptomic reads (88.2-94.0%) mapped onto

256 rRNA-encoding genes from one of the four rRNA operons encoded by S. denitrificans

257 (Supplement Table 1). No differences were observed for ribosomal RNA in thiosulfate- and S8-

258 grown cultures. In addition, proteins of the small and large ribosomal subunits showed little

259 variance in their abundance, which is expected since all subunits and the ribosomal RNA form

260 functioning ribosomes. However, we found significant differences in the transcription of genes

261 encoding ribosomal small and large subunit proteins, which were transcribed at a significantly

262 higher level in thiosulfate-grown cultures. We also evaluated the expression of an alternative

263 indicator for growth - the translation elongation factor TU (EF-TU; WP_011371980.1) (Pedersen

264 et al., 1978), which also had a higher expression level in the transcriptome and higher levels of

265 abundance in the proteome in thiosulfate-grown cultures (Supplement Table 1).

266 Although the differences in transcriptomic and proteomic profiles between cells grown

267 with the two different electron donors were subtle (Supplement Figure S2), a small number of

268 proteins showed statistically significant differences in relative abundance (Supplement Table 1).

269 One of these proteins (WP_011373531.1) was present at significantly higher levels (2.9 x

270 increase) in S8-grown cultures, compared to thiosulfate-grown cultures. This hypothetical protein

271 was also differentially regulated in the transcriptome, but in the opposite manner - it was

272 transcribed at higher levels under the thiosulfate condition compared to the S8 condition. Based

273 on analyses using BOCTOPUS, PRED-TMMB and SignalP 4.0, WP_011373531.1 contains a

274 beta-barrel structure and a predicted signal peptide. It also contains a phenylalanine at the C-

275 terminal position, as well as hydrophobic amino acids at positions -3, -5, -7, and -9 relative to the

276 C-terminus, which have previously been reported to be important for the assembly into the outer

13 277 membrane (Struyvé et al., 1991; Tommassen, 2010). These indications suggest that it is an outer

278 membrane protein. Protein domain analysis (DELTA-BLAST and PSI-BLAST, NCBI) of this

279 hypothetical protein further showed that the first 177 amino acids of WP_011373531.1 have

280 similarity to the conserved domain of the outer membrane protein family OprD and the major

281 outer membrane protein of Campylobacter (Campylo_MOMP), suggesting an involvement in

282 transport and/or adhesion (Yoshihara et al., 1998; Zhang et al., 2000). However, based on the

283 low overall similarity, a functional classification cannot be inferred at present. A protein

284 BLAST-based comparison of alignment length and amino acid sequence identity revealed the

285 presence of homologs of this putative outer membrane protein (>70% alignment fraction, >30%

286 amino acid identity) in various campylobacterial species (e.g., Sulfurimonas, Sulfurovum,

287 Sulfuricurvum, Nitratiruptor) that are also implicated in elemental sulfur utilization (Campbell et

288 al., 2006; Sievert et al., 2008; Sievert and Vetriani, 2012).

289

290 Flagella-related proteins and transcripts are differentially abundant

291 Significant differences in gene transcription levels were observed for a large number of

292 genes involved in flagella biosynthesis and motility (Figure 2). Flagella-related genes were

293 generally upregulated in cultures grown with S8 as electron donor. In contrast, the differences in

294 the expression of proteins of the flagellar apparatus were not as pronounced between the growth

295 conditions, but the flagellar hook protein FlgE and flagellin were found in considerably higher

296 relative abundance in the proteome of S8-grown cultures (Supplement Table 1).

297

298 Genes and proteins of central biochemical pathways

14 299 Growing with nitrate as the electron acceptor with thiosulfate or cyclooctasulfur as the

300 sole electron donor, S. denitrificans gains energy through coupled to sulfur

301 oxidation. The generated energy mainly fuels through the reductive tricarboxylic

302 acid (rTCA) cycle. Accordingly, all transcripts and proteins of the rTCA cycle were identified. In

303 the genome, two copies of succinate dehydrogenase/fumarate reductase have been identified, one

304 being membrane-bound and one being cytoplasmic (Sievert et al., 2008). It has previously been

305 proposed that the membrane-bound form might play a direct role in the rTCA cycle by

306 transferring electrons derived from the oxidation of hydrogen or sulfur via the quinone pool

307 (Sievert et al., 2008). In line with this hypothesis, the putatively membrane-bound succinate

308 dehydrogenase/fumarate reductase (SDH; EC 1.3.5.1; WP_011372658.1-WP_011372660.1) was

309 found in the transcriptomes and proteomes under both growth conditions, while the cytoplasmic

310 succinate dehydrogenase/fumarate reductase (WP_011371673.1-WP_011371674.1) only

311 displayed a low transcription level and was not identified in the proteome (Supplement Table 1).

312 For the reduction of nitrate, we could confirm that all transcripts and all proteins involved

313 in the canonical dissimilatory denitrification pathway were present (Figure 3), including the

314 nitric oxide reductase cNOR, which had previously been questioned to be functional due to the

315 absence of norD and norQ in the genome (Sievert et al., 2008). In contrast, neither the transcripts

316 nor the proteins of the proposed alternative non-electrogenic quinone-oxidizing nitric oxide

317 reductase (gNOR, WP_011371739.1-WP_011371741.1; Sievert et al., 2008) could be detected

318 (Supplement Table 1). The comparatively low abundance of the nitrous oxide reductase (NorB,

319 NorC) in the proteome compared to the other of the denitrification pathway is most

320 likely due to the fact that NorB is an integral membrane protein and NorC is anchored in the

321 membrane. Membrane associated proteins are not extracted with the same efficiency as soluble

15 322 proteins by the used extraction procedure, resulting in their lower representation in the proteome.

323 The same bias applies for the membrane bound components of the nitrate reductase complex

324 (NapFGH).

325 With respect to sulfur compound metabolism, transcripts and proteins of the periplasmic

326 SOX (sulfur oxidation) multienzyme complex were detected, confirming the use of the SOX

327 system for sulfur oxidation in S. denitrificans, as has previously been shown for the

328 campylobacterium Sulfurovum sp. NCB37-1 (Yamamoto et al., 2010). The transcripts of both

329 sox operons, i.e., soxABXY1Z1 and soxCDY2Z2, showed a trend of increased transcription levels in

330 thiosulfate grown-cultures. However, the transcripts of soxABXY1Z1 were more strongly

331 upregulated with thiosulfate, as the transcription ratios for soxABXY1Z1 between S8 and

332 thiosulfate ranged from 0.3-0.6, while those of soxCDY2Z2 ranged from 0.65-0.8 (Figure 4). In

333 the proteomes of S8-grown cultures, SOX proteins of the soxABXY1Z1 operon were hardly

334 detected, while they were present in significantly higher abundance with thiosulfate (Figure 4).

335 In contrast, the sulfur dehydrogenase proteins, i.e., SoxCD, were significantly more abundant in

336 the proteome of S8- grown cultures, although still present with thiosulfate (Figure 4). Regardless

337 of the supplied electron donor, the SoxY and SoxZ proteins of the soxCDY2Z2 operon were not

338 only the two most abundant proteins of the SOX multienzyme system, but of both proteomes

339 under both growth conditions overall (Figure 4, Supplement Table 1), suggesting that they play

340 an important role under both conditions. In addition, a protein encoded by gene

341 WP_011373670.1 that is located next to soxCDY2Z2 is present in the transcriptome and proteome

342 under both growth conditions (Figure 4, Supplement Table 1). The 340 amino acids-long protein

343 has a signal peptide indicating a periplasmic location, and based on BLAST search it further

344 contains a metallo-hydrolase-like_MBL-fold with all the conserved residues of the active site

16 345 and three putative metal binding sites, suggesting it has a hydrolytic function. Transcript reads

346 and protein abundance of the sulfide:quinone oxidoreductase (SQR), a sulfide-oxidizng enzyme,

347 and the putative membrane-bound polysulfide reductase, a polysuldide-reducing complex, which

348 might be involved in the reduction of polysulfide, were low, and no significant differences

349 between growth conditions was observed (Figure 4).

350

351 Transcribed and translated genes involved in alternative energy metabolism

352 The S. denitrificans genome reflects the potential to use alternative energy sources to

353 generate energy for carbon fixation (Sievert et al., 2008). We were able to detect the

354 transcription of genes that are involved in the metabolism of compounds which were not

355 provided in the medium. The assessment of transcriptomic data revealed that genes of a cbb3-

356 type cytochrome c oxidase (fixNOQP cluster involved in aerobic respiration) as well as genes

357 encoding a membrane-bound [Ni,Fe]-uptake (hydABC cluster involved in hydrogen

358 oxidation) were transcribed in all cultures (Supplement Figure S3). In addition, FixO and HydB

359 were identified at low relative abundance in the proteomes under both cultivation conditions

360 (Supplement Table 1), whereas the proposed cytoplasmic hydrogenase putatively involved in

361 direct electron transfer as part of the rTCA cycle (WP_011373066.1; WP041672536.1; Sievert et

362 al., 2008) was not expressed under either cultivation condition (Supplement Table 1). Genes

363 encoding the membrane-bound formate dehydrogenase complex were transcribed at higher

364 relative levels in the S8-grown cultures (Supplement Figure S3), but no proteins of the complex

365 were identified (Supplement Table 1).

366

17 367 Discussion

368 In this study, we performed proteomic and transcriptomic analyses to investigate the

369 metabolism of Sulfurimonas denitrificans with either S8 or thiosulfate as the sole electron donor.

370 Transcriptomic and proteomic approaches complement each other to assess microbial activity

371 and metabolic regulation, as the half-life for mRNA is in the range of minutes (Selinger et al.,

372 2003), whereas that of proteins is in the range of hours (Maier et al., 2011). However, a protein

373 concentration of roughly 100 fmol per protein is necessary for successful detection (Silva et al.,

374 2006), which is much higher than the mRNA abundance required if a sufficient sequencing depth

375 is attained. Furthermore, isolation and detection of membrane-bound proteins remains a

376 challenge in proteomics. Thus, the combined application of proteomic and transcriptomic

377 profiling provides a comprehensive assessment of the microbial response to different

378 physiological conditions. In some instances, we did observe that there was not a strict correlation

379 between transcribed genes and detected proteins, which could be explained either by

380 posttranscriptional regulation (Picard, 2009; van Assche et al., 2015), the initiation of

381 transcription before proteins reached levels high enough for their detection, or the longer lifetime

382 of proteins compared to transcripts.

383 In the present study, the detection of 42% of the predicted proteins encoded in the

384 genome is comparable to was found for the gram-positive bacterium Bacillus subtilis, but lower

385 than for example the 70% reported for the thaumarchaeon “Candidatus Nitrosopelagicus brevis”

386 (Hahne et al., 2010, Santoro et al., 2015). The number of transcribed genes and identified

387 proteins was similar under both growth conditions. This similarity of the transcriptomic and

388 proteomic profiles was mirrored in the broad COG categories (Figure 1), and differences

389 between the growth conditions were restricted to individual mRNA and protein categories.

18 390 Ribosomal RNA levels as well as protein levels of ribosomal subunits did not vary

391 significantly between the two growth conditions, despite higher growth rates with thiosulfate.

392 Similar observations have been made previously and it was concluded that rRNA levels in

393 combination with the growth rates are not always a good indicator for microbial activity

394 (Blazewicz et al., 2013). However, in cultures grown with thiosulfate, transcription of ribosomal

395 subunit genes was significantly higher in relation to rRNA gene transcription levels, which,

396 together with elevated transcript and protein levels of the elongation factor TU, likely reflects the

397 higher growth rates and higher overall activity in cultures grown with thiosulfate. One of the

398 most abundant proteins of the proteome was identified as a hypothetical protein

399 (WP_011373531.1), which is likely to play an important role for Sulfurimonas species and other

400 Campylobacteria as apparent homologs are present in genomes of various Campylobacteria. In

401 S8-grown cultures, this protein showed an almost threefold increase in relative abundance.

402 Possibly, this protein could be involved in the activation of S8, similar to the outer membrane

403 protein identified in A. caldus (Ramírez et al., 2004; Mangold et al., 2011; Chen et al., 2012),

404 although no similarity was observed between these proteins. On the other hand, transcripts

405 showed an opposite trend with the level of WP_011373531.1 gene expression being higher under

406 the thiosulfate condition, making a specific role in S8 metabolism less certain. However, the

407 relative abundance of the transcripts is influenced by the absolute number of identified

408 transcripts and translation could further be prevented by posttranscriptional regulation, making

409 the proteomic data overall a better indicator for the involvement of the protein under different

410 growth conditions. Thus, although we are presently not able to assign a function to this protein,

411 our results indicate that it may play a fundamental role in the cells’ metabolism, including the

412 possibility of its involvement in S8 metabolism. To resolve the role of this protein in S.

19 413 denitrificans, and potentially other Campylobacteria, more work is needed. Such experiments,

414 however, were beyond the scope of this study, since they would rely on heterologous gene

415 expression assays or a genetic system for S. denitrificans, which is currently not available.

416

417 The expression of genes and proteins involved in energy metabolism

418 Chemoautotrophic bacteria gain energy through redox reactions. In our experiments, S.

419 denitrificans coupled the reduction of nitrate with the oxidation of thiosulfate or cyclooctasulfur

420 to gain energy for growth. All proteins of the canonical denitrification pathway were identified,

421 but no protein of the proposed alternative non-electrogenic gNOR system (Sievert et al., 2008).

422 To the best of our knowledge, we provide the first validation of a functional cNOR system that

423 lacks the components encoded by norD and norQ, which are absent from the genome of S.

424 denitrificans and other Campylobacteria (Sievert et al., 2008).

425 Besides the utilization of nitrate, S. denitrificans can utilize oxygen using a cbb3-type

426 cytochrome c oxidase (Sievert et al., 2008). All genes were transcribed under both conditions

427 (Supplementary Figure S3), which could be either an indicator for the presence of small amounts

428 of oxygen in our batch culture system, for example by leakage through the butyl stoppers, or for

429 constitutive transcription. In addition, genes for the membrane bound [Ni,Fe]-uptake

430 hydrogenase and genes for the formate dehydrogenase were transcribed (Supplement Figure S3),

431 although no hydrogen or formate was provided in the cultivation medium. Notably, even though

432 low level of transcripts for hydrogenase could be detected in the absence of hydrogen, the

433 transcripts for the hydrogenase are highly upregulated in the presence of hydrogen (unpublished

434 data).

20 435 The simultaneous transcription (at a low level) of genes for the utilization of alternative

436 substrates could be a mechanism to react quickly when either oxygen or hydrogen become

437 available in the environment. This high level of metabolic flexibility is a possible explanation for

438 the environmental success of Sulfurimonas species, which have been described as r-strategist

439 (Rogge et al., 2017) and primary colonizers (López-García et al., 2003).

440

441 Flagella likely facilitate attachment to S8

442 Cyclooctasulfur is a solid substrate, which likely requires the attachment of cells to make

443 it accessible (Mangold et al., 2011; Pjevac et al., 2014). Proteins of the flagellar apparatus have

444 been shown to play a critical role in attachment and formation, including in

445 Campylobacteria (e.g., O’Toole and Kolter, 1998; Pratt and Kolter, 1998; Otteman and

446 Lowenthal, 2002; Joshua at al., 2006; Haiko and Westerlund-Wikström, 2013). Previously,

447 Mangold and colleagues identified a flagellar basal-body rod protein (FlgC) to be up-regulated in

448 S0-grown vs. tetrathionate-grown cultures of A. caldus, facilitating attachment to the solid

449 substrate (Mangold et al., 2011). Interestingly, the only COG category that showed differences

450 between the two growth conditions encompassed genes of the flagellar apparatus. Specifically,

451 transcriptomic data showed a significantly higher expression of genes involved in flagella

452 biosynthesis and flagella motility in S8-grown cultures (Figure 2). Thus, we propose that the

453 increased transcription of flagella-related genes as well as the higher relative abundance of FlgE

454 (flagellar hook protein) and flagellin in S8-grown cultures is indicative of attachment and biofilm

455 formation cyclooctasulfur particles. On the other hand, genes related to chemotaxis showed a

456 trend of higher expression in thiosulfate-grown cultures, indicating that chemotaxis is more

457 important in sensing gradients of the soluble substrate thiosulfate. In this context, it is important

21 458 to note that while the original strain used in our experiments has been described as non-motile, S.

459 denitrificans has regained motility during cultivation in our laboratory (unpublished data). We

460 attribute this to the spontaneous excision of the transposon that was shown to interrupt a flagellin

461 biosynthesis operon, as its genome otherwise contains all genes required for a fully functional

462 flagellar apparatus (Sievert et al., 2008).

463

464

465 The mechanism of thiosulfate- and S8-oxidation

466 With the exception of the potential involvement of the hypothetical protein in the

467 activation and transport of S8 into the cell, we were not able to identify a possible mechanism for

468 the activation of cyclooctasulfur, as has for example been proposed for acidophilic sulfur-

469 oxidizing bacteria (Rohwerder and Sand, 2003; Mangold et al., 2011; Chen et al., 2012).

470 However, our data confirm the previously hypothesized differential regulation of the two SOX

471 gene clusters present in S. denitrificans in response to the available sulfur substrate (Sievert et

472 al., 2008; Meier et al., 2017; Pjevac et al., 2018), allowing us to propose a possible oxidation

473 pathway. In thiosulfate-grown cultures, the first gene cluster encoding soxABXY1Z1 was highly

474 transcribed and the corresponding proteins were found in significantly higher abundance

475 compared to growth with S8, confirming their involvement in thiosulfate oxidation as previously

476 proposed (Friedrich et al., 2001; 2005). The differential abundance of the SoxABXY1Z1-proteins

477 is in contrast to the phototrophic sulfur-oxidizing gammaproteobacterium A. vinosum, for which

478 no differences were observed in response to different sulfur compounds (Weissgerber et al.,

479 2014). Under both growth conditions, soxY2Z2 was highly transcribed and the corresponding

480 proteins were highly abundant in S. denitrificans, suggesting that it plays an important role in the

22 481 oxidation of both thiosulfate and S8 (Figure 4). In contrast, SoxCD proteins were significantly

482 more abundant in S8-grown cultures. Although the soxABXY1Z1-operon was present in the

483 transcriptome, it was nearly undetectable in the proteome, suggesting that it might be under post-

484 transcriptional control and not translated into functional proteins when S. denitrificans is grown

485 with S8 (Picard, 2009; van Assche et al., 2015) or translated at low levels preventing the

486 detection of the proteins by our methods. Thus, we propose that the oxidation of S8 is mediated

487 mainly by soxCDY2Z2, and we interpret the low abundance of transcripts and in particular of

488 proteins of the soxABXY1Z1 operon in S8-grown cultures as another reflection of baseline activity

489 and for metabolic flexibility, allowing S. denitrificans to quickly respond to the availability of

490 thiosulfate. This interpretation is in line with qPCR data that showed the presence of soxB

491 transcripts in low abundance in hydrogen-grown S. denitrificans cultures lacking reduced sulfur

492 compounds, and their increased abundance in the presence of thiosulfate, while soxD transcripts

493 remained more or less unchanged, pointing to its constitutive expression (unpublished data).

494

495 An alternative model for sulfur oxidation in S. denitrificans

496 Based on our observations on the differential abundance of the SOX proteins during

497 growth on thiosulfate versus S8 and previous results (Friedrich et al., 2001; 2005; Sauvé et al.,

498 2007; Grabarczyk and Berks, 2017), we propose a sulfur oxidation model for the oxidation of S8

499 by S. denitrificans that does not involve the SoxABXY1Z1 protein complex (Figure 5). At

500 present, we are not able to resolve how the sulfonate group bound to SoxY2Z2 is being

501 hydrolyzed to form sulfate. One option could be that SoxB, which might be present in low

502 abundance, could perform that function. However, another possibility might be that the putative

503 periplasmic metallo-hydrolase encoded by WP_011373670.1 could perform this function. This

23 504 scenario appears intriguing as this gene is located next to soxCDY2Z2 and homologs of this gene

505 are found in other sulfur-oxidizing Campylobacteria with conserved synteny. The protein’s

506 catalytic domain has similarities to SoxH of Parococcus pantotrophus. However, while soxH

507 expression is specifically induced by thiosulfate, it is not required for sulfur oxidation in P.

508 pantotrophus and its function is currently unknown (Rother et al., 2001), although it has been

509 described as a putative thiol hydrolase (Friedrich et al., 2001). Lastly, it might be possible that

510 SoxCDY2Z2 can catalyze the reaction by itself, although there is at present no evidence to

511 support this hypothesis. Future experiments need to be carried out to differentiate between these

512 options. Thiosulfate oxidation by S. denitrificans proceeds mainly as proposed in the current

513 sulfur oxidation model (Friedrich et al., 2001; 2005; Grabarczyk and Berks, 2017). First,

514 thiosulfate is activated via SoxXA and bound to a cysteine residue of SoxY in the SoxYZ1

515 complex, followed by the hydrolysis of the outer sulfonate group of the bound thiosulfate by

516 SoxB (Friedrich et al, 2001). However, we hypothesize that subsequently the sulfone group is

517 being transferred to SoxY2Z2, where it is oxidized and hydrolyzed to sulfate as described above,

518 in line with the high abundance of SoxCD and in particular SoxY2Z2 under both growth

519 conditions. We postulate SoxY2Z2 to interact specifically with SoxCD based on the operon

520 structure and the observed expression pattern. This way, we propose that SoxCDY2Z2 is always

521 present, whereas SoxABXY1Z1 is only needed in the presence of thiosulfate. Biochemical and

522 genetic studies will be required to validate this proposed model for the oxidation of S8 and

523 thiosulfate in S. denitrificans and other Campylobacteria with the same genetic arrangement of

524 the SOX system.

525 In addition to the described function in S. denitrificans, the soxY2Z2 genes of the

526 soxCDY2Z2 operon show a much higher level of diversification between different Sulfurimonas

24 527 and Sulfurovum species (up to 79% nucleotide sequence dissimilarity) than soxY1Z1 of the

528 soxABXY1Z1 operon (Meier et al., 2017). Moreover, the sequence similarity between the two

529 SoxYZ copies in S. denitrificans and other Campylobacteria is very low. The amino acid

530 sequence identity is 33% for the two SoxY proteins, and 28% (over a 61% alignment fraction)

531 for the two SoxZ proteins of S. denitrificans. In fact, no significant identity, except for the export

532 signal sequence, is detectable on the nucleotide level for either gene. This highly divergent

533 intragenomic duplication, and the intergenomic diversification of the SoxY2Z2 proteins, is

534 present in all currently available Sulfurimonas and Sulfurovum genomes (Meier et al., 2017).

535 Furthermore, a significantly higher expression level of SoxY2Z2 proteins when compared to

536 SoxY1Z1 proteins has been found in the metaproteomes of Campylobacteria-dominated

537 forming on black-smoker chimneys (Pjevac et al., 2018). The diversification of the SoxY2Z2

538 proteins could lead to different substrate preferences with respect to the chain length of the

539 bound polysulfide or to differences in overall substrate-binding affinities, and may therefore be

540 involved in niche partitioning between co-occurring Sulfurimonas and Sulfurovum species,

541 whereas the SoxY1Z1 proteins are specific for thiosulfate, explaining their lower diversity and

542 lower abundance in environmental samples, where thiosulfate is usually present in lower

543 concentrations than elemental sulfur or polysulfide (Zopfi et al., 2004). Potentially, the ratio of

544 the SoxCD to SoxAB proteins (SoxCD/SoxAB: S8:19; TS:0.9) and SoxY2Z2 to SoxY1Z1 proteins

545 (SoxY2Z2/ SoxY1Z1: S8:89; TS:9) , and to a lesser extent that of the transcripts (soxCD/soxAB:

546 S8:2.7; TS:1.5 and soxY2Z2/soxY1Z1: S8:3.3; TS:1.9), could be used as an indicator for the type of

547 sulfur compound being utilized by Sulfurimonas and possibly other sulfur-oxidizing

548 Campylobacteria in the environment.

549

25 550

551 Conclusions

552 We have applied transcriptomics and proteomics as two powerful approaches to elucidate

553 the biochemical pathways involved in the oxidation of two different sulfur compounds by the

554 campylobacterium S. denitrificans. We were able to show that the SOX system in S. denitrificans

555 is differentially regulated in response to the available sulfur substrate. Based on the available

556 data, we propose a model for the oxidation of cyclooctasulfur in S. denitrificans. We further

557 identified a hypothetical protein that may play a central role in the metabolism of reduced sulfur

558 compounds. In the future, genetic and biochemical studies are needed to elucidate its function,

559 including its potential involvement in the activation of S8, and to validate our proposed model for

560 sulfur oxidation in S. denitrificans, which is likely to also operate in other sulfur-oxidizing

561 Campylobacteria. The data presented here will aid in the interpretation of environmental

562 metatranscriptomic and –proteomic data and help to provide a biochemical basis for the observed

563 niche partitioning of different sulfur-oxidizing Campylobacteria.

564

565 Acknowledgements

566 We thank Dali Smolsky for helping with culturing and cell counts, Jörg Wulf for RNA

567 extraction, Jana Matulla for instructions on protein isolation, Sebastian Grund for mass

568 spectrometry measurements and Fabian Götz for helping with statistical analysis. We also would

569 like to thank two anonymous reviewers for their insightful and constructive comments that

570 improved the manuscript. Funding was provided by NSF OCE-1136727 and The Investment in

26 571 Science Fund at WHOI (SMS). Florian Götz was partly supported by a scholarship of the

572 Institute of Marine Biotechnology e.V. (IMaB).

573

574 References

575 Alonso-Azcárate, J., Bottrell, S.H., and Tritlla, J. (2001) Sulfur redox reactions and formation of

576 native sulfur veins during low grade metamorphism of gypsum evaporites, Cameros

577 Basin (NE Spain). Chem. Geol. 174: 389–402.

578 Blazewicz, S.J., Barnard, R.L., Daly, R.A., and Firestone, M.K. (2013) Evaluating rRNA as an

579 indicator of microbial activity in environmental communities: limitations and uses. ISME

580 J. 7: 2061–2068.

581 Boratyn, G.M., Schäffer, A.A., Agarwala, R., Altschul, S.F., Lipman, D.J., and Madden, T.L.

582 (2012) Domain enhanced lookup time accelerated BLAST. Biol. Direct 7: 12.

583 Campbell, B.J., Engel, A.S., Porter, M.L., and Takai, K. (2006) The versatile ϵ-:

584 key players in sulphidic habitats. Nat. Rev. Microbiol. 4: 458–468.

585 Chen, L., Ren, Y., Lin, Jianqun, Liu, X., Pang, X., and Lin, Jianqiang (2012) Acidithiobacillus

586 caldus sulfur oxidation model based on transcriptome analysis between the wild type and

587 sulfur oxygenase reductase defective mutant. PLOS ONE 7: e39470.

588 Cosmidis, J. and Templeton, A.S. (2016) Self-assembly of biomorphic carbon/sulfur

589 microstructures in sulfidic environments. Nat. Commun. 7: ncomms12812.

590 Dahl, C., Friedrich, C., and Kletzin, A. (2008) Sulfur oxidation in prokaryotes. In, Encyclopedia

591 of Life Sciences. John Wiley & Sons, Ltd.

27 592 Dahl, C. and Prange, A. (2006) Bacterial sulfur globules: Occurrence, structure and metabolism.

593 In, Shively, D.J.M. (ed), Inclusions in Prokaryotes. Springer Berlin Heidelberg, pp. 21–

594 51.

595 Engel, A.S., Porter, M.L., Stern, L.A., Quinlan, S., and Bennett, P.C. (2004) Bacterial diversity

596 and ecosystem function of filamentous microbial mats from aphotic (cave) sulfidic

597 springs dominated by chemolithoautotrophic “.” FEMS Microbiol.

598 Ecol. 51: 31–53.

599 Franz, B., Lichtenberg, H., Hormes, J., Modrow, H., Dahl, C., and Prange, A. (2007) Utilization

600 of solid ‘elemental’ sulfur by the phototrophic purple sulfur bacterium Allochromatium

601 vinosum: a sulfur K-edge X-ray absorption spectroscopy study. Microbiology 153: 1268–

602 1274.

603 Finster, K. (2008) Microbiological disproportionation of inorganic sulfur compounds. Journal of

604 Sulfur Chemistry 29:281-292

605 Friedrich, C.G., Bardischewsky, F., Rother, D., Quentmeier, A., and Fischer, J. (2005)

606 Prokaryotic sulfur oxidation. Curr. Opin. Microbiol. 8: 253–259.

607 Friedrich, C.G., Rother, D., Bardischewsky, F., Quentmeier, A., and Fischer, J. (2001) Oxidation

608 of reduced inorganic sulfur compounds by bacteria: Emergence of a common

609 mechanism? Appl. Environ. Microbiol. 67: 2873–2882.

610 Grabarczyk, D.B. and Berks, B.C. (2017) Intermediates in the Sox sulfur oxidation pathway are

611 bound to a sulfane conjugate of the carrier protein SoxYZ. PLOS ONE 12: e0173395.

612 Gulmann, L.K., Beaulieu, S.E., Shank, T.M., Ding, K., Seyfried, W.E.J., and Sievert, S.M.

613 (2015) Bacterial diversity and successional patterns during biofilm formation on freshly

614 exposed basalt surfaces at diffuse-flow deep-sea vents. Front. Microbiol. 6: 901.

28 615 Hahne, H., Mäder, U., Otto, A., Bonn, F., Steil, L., Bremer, E., et al. (2010) A comprehensive

616 proteomics and transcriptomics analysis of Bacillus subtilis salt stress adaptation. J.

617 Bacteriol. 192: 870–882.

618 Haiko, J. and Westerlund-Wikström, B. (2013) The Role of the Bacterial in Adhesion

619 and Virulence. Biology 2: 1242–1267.

620 Han, Y. and Perner, M. (2015) The globally widespread genus Sulfurimonas: versatile energy

621 and adaptations to redox clines. Front. Microbiol. 6: 989

622 Heinz, E., Williams, T.A., Nakjang, S., Noël, C.J., Swan, D.C., Goldberg, A.V., et al. (2012) The

623 genome of the obligate intracellular parasite Trachipleistophora hominis: new insights

624 into microsporidian genome dynamics and reductive evolution. PLoS Pathog. 8:

625 e1002979.

626 Hensen, D., Sperling, D., Trüper, H.G., Brune, D.C., and Dahl, C. (2006) Thiosulphate oxidation

627 in the phototrophic sulphur bacterium Allochromatium vinosum. Mol. Microbiol. 62:

628 794–810.

629 Hubert, C.R.J., Oldenburg, T.B.P., Fustic, M., Gray, N.D., Larter, S.R., Penn, K., et al. (2012)

630 Massive dominance of Epsilonproteobacteria in formation waters from a Canadian oil

631 sands reservoir containing severely biodegraded oil. Environ. Microbiol. 14: 387–404.

632 Joshua, G.W.P., Guthrie-Irons, C., Karlyshev, A.V., and Wren, B.W. (2006) Biofilm formation

633 in Campylobacter jejuni. Microbiology 152: 387–396.

634 Kamyshny, A. (2009) Solubility of cyclooctasulfur in pure water and sea water at different

635 temperatures. Geochim. Cosmochim. Acta 73: 6022–6028.

29 636 Kletzin, A., Urich, T., Müller, F., Bandeiras, T.M., and Gomes, C.M. (2004) Dissimilatory

637 oxidation and reduction of elemental sulfur in thermophilic archaea. J. Bioenerg.

638 Biomembr. 36: 77–91.

639 Lau, G.E., Cosmidis, J., Grasby, S.E., Trivedi, C.B., Spear, J.R., and Templeton, A.S. (2017)

640 Low-temperature formation and stabilization of rare allotropes of cyclooctasulfur (β-S8

641 and γ-S8) in the presence of organic carbon at a sulfur-rich glacial site in the Canadian

642 High Arctic. Geochim. Cosmochim. Acta 200: 218–231.

643 Lavik, G., Stührmann, T., Brüchert, V., Plas, A.V. der, Mohrholz, V., Lam, P., et al. (2009)

644 Detoxification of sulphidic African shelf waters by blooming chemolithotrophs. Nature

645 457: 581.

646 Legatzki, A., Ortiz, M., Neilson, J.W., Dominguez, S., Andersen, G.L., Toomey, R.S., et al.

647 (2011) Bacterial and archaeal community structure of two adjacent calcite speleothems in

648 Kartchner Caverns, Arizona, USA. Geomicrobiol. J. 28: 99–117.

649 Li, B., Ruotti, V., Stewart, R.M., Thomson, J.A., and Dewey, C.N. (2010) RNA-Seq gene

650 expression estimation with read mapping uncertainty. Bioinformatics 26: 493–500.

651 Li, R., Morrison, L., Collins, G., Li, A., and Zhan, X. (2016) Simultaneous nitrate and phosphate

652 removal from wastewater lacking organic matter through microbial oxidation of

653 pyrrhotite coupled to nitrate reduction. Water Res. 96: 32–41.

654 López-García, P., Duperron, S., Philippot, P., Foriel, J., Susini, J., and Moreira, D. (2003)

655 Bacterial diversity in hydrothermal sediment and epsilonproteobacterial dominance in

656 experimental microcolonizers at the Mid-Atlantic Ridge. Environ. Microbiol. 5: 961–976.

657 Macalady, J., Dattagupta, S., Schaperdoth, I., Jones, D., Druschel, G., and Eastman, D. (2008)

658 Niche differentiation among sulfur-oxidizing bacterial populations.

30 659 Maier, T., Schmidt, A., Güell, M., Kühner, S., Gavin, A.-C., Aebersold, R., and Serrano, L.

660 (2011) Quantification of mRNA and protein and integration with protein turnover in a

661 bacterium. Mol. Syst. Biol. 7: 511.

662 Mangold, S., Valdés, J., Holmes, D., and Dopson, M. (2011) Sulfur Metabolism in the extreme

663 acidophile Acidithiobacillus caldus. Front. Microbiol. 2: 17.

664 McNichol, J., Sylva, S.P., Thomas, F., Taylor, C.D., Sievert, S.M., and Seewald, J.S. (2016)

665 Assessing microbial processes in deep-sea hydrothermal systems via incubations at in

666 situ temperature and pressure. Deep Sea Res. Part Oceanogr. Res. Pap.

667 Meier, D.V., Pjevac, P., Bach, W., Hourdez, S., Girguis, P.R., Vidoudez, C., et al. (2017) Niche

668 partitioning of diverse sulfur-oxidizing bacteria at hydrothermal vents. ISME J. 11: 1545-

669 1558.

670 Meyer, J.L., Akerman, N.H., Proskurowski, G., and Huber, J.A. (2013) Microbiological

671 characterization of post-eruption “snowblower” vents at , Juan de Fuca

672 Ridge. Front. Microbiol. 4 doi: 10.3389/fmicb.2013.00153

673 O’Toole, G.A. and Kolter, R. (1998) Flagellar and twitching motility are necessary for

674 Pseudomonas aeruginosa biofilm development. Mol. Microbiol. 30: 295–304.

675 Ottemann, K.M. and Lowenthal, A.C. (2002) Helicobacter pylori uses motility for initial

676 colonization and to attain robust infection. Infect. Immun. 70: 1984–1990.

677 Otto, A., Bernhardt, J., Meyer, H., Schaffer, M., Herbst, F.-A., Siebourg, J., et al. (2010)

678 Systems-wide temporal proteomic profiling in glucose-starved Bacillus subtilis. Nat.

679 Commun. 1: 137.

31 680 Pedersen, S., Bloch, P.L., Reeh, S., and Neidhardt, F.C. (1978) Patterns of protein synthesis in E.

681 coli: a catalog of the amount of 140 individual proteins at different growth rates. Cell 14:

682 179–190.

683 Petersen, T.N., Brunak, S., von Heijne, G., and Nielsen, H. (2011) SignalP 4.0: discriminating

684 signal peptides from transmembrane regions. Nat. Methods 8: 785–786.

685 Picard, F., Dressaire, C., Girbal, L., and Cocaign-Bousquet, M. (2009) Examination of post-

686 transcriptional regulations in prokaryotes by integrative biology. C. R. Biol. 332: 958–

687 973. doi:10.1016/j.crvi.2009.09.005

688 Pjevac, P., Kamyshny, A., Dyksma, S., and Mußmann, M. (2014) Microbial consumption of

689 zero-valence sulfur in marine benthic habitats. Environ. Microbiol. 16: 3416–3430.

690 Pjevac, P., Meier, D. V., Markert, S., Hentschker, C., Schweder, T., Becher, D., et al. (2018)

691 Metaproteogenomic profiling of microbial communities colonizing actively venting

692 hydrothermal chimneys. Front. Microbiol. 9: 680. doi: 10.3389/fmicb.2018.00680

693 Prange, A., Chauvistré, R., Modrow, H., Hormes, J., Trüper, H.G., and Dahl, C. (2002)

694 Quantitative of sulfur in bacterial sulfur globules: X-ray absorption

695 spectroscopy reveals at least three different species of sulfur. Microbiology 148: 267–

696 276.

697 Pratt, L.A. and Kolter, R. (1998) Genetic analysis of Escherichia coli biofilm formation: roles of

698 flagella, motility, chemotaxis and type I pili. Mol. Microbiol. 30: 285–293.

699 Quentmeier, A. and Friedrich, C.G. (2001) The cysteine residue of the SoxY protein as the active

700 site of protein-bound sulfur oxidation of Paracoccus pantotrophus GB17. FEBS Lett.

701 503: 168–172.

32 702 Raiswell, R. (1992) Evolution of the global biogeochemical sulphur cycle, scope 39 edited by P.

703 Brimblecombe and A. Y. Lein. John Wiley and Sons, Chichester, 1989. No. of pages:

704 241. Price: £56.95 (hardback). Geol. J. 27: 192–193.

705 Ramírez, P., Guiliani, N., Valenzuela, L., Beard, S., and Jerez, C.A. (2004) Differential protein

706 expression during growth of Acidithiobacillus ferrooxidans on ferrous iron, sulfur

707 compounds, or metal sulfides. Appl. Environ. Microbiol. 70: 4491–4498.

708 Robertson, L.A. and Kuenen, J.G. (2006) The colorless sulfur bacteria. In, Dworkin, M., Falkow,

709 S., Rosenberg, E., Schleifer, K.-H., and Stackebrandt, E. (eds), The Prokaryotes. Springer

710 New York, pp. 985–1011.

711 Rogge, A., Vogts, A., Voss, M., Jürgens, K., Jost, G., and Labrenz, M. (2017) Success of

712 chemolithoautotrophic SUP05 and Sulfurimonas GD17 cells in pelagic redox

713 zones is facilitated by their lifestyles as K- and r-strategists. Environ. Microbiol. 19:

714 2495–2506.

715 Rohwerder, T. and Sand, W. (2003) The sulfane sulfur of persulfides is the actual substrate of the

716 sulfur-oxidizing enzymes from Acidithiobacillus and Acidiphilium spp. Microbiology

717 149: 1699–1710.

718 Ruby, E.G., Wirsen, C.O., and Jannasch, H.W. (1981) Chemolithotrophic sulfur-oxidizing

719 bacteria from the Galapagos Rift hydrothermal vents. Appl. Environ. Microbiol. 42: 317–

720 324.

721 Santoro, A.E., Dupont, C.L., Richter, R.A., Craig, M.T., Carini, P, McIlvin, M.R., Yang, Y.,

722 Orsi, W.D., Moran, D. M., and Saito, M.A. (2015) Genomic and proteomic

723 characterization of “Candidatus Nitrosopelagicus brevis”: An ammonia-oxidizing

724 archaeon from the open ocean. Proc. Natl. Acad. Sci. USA 112: 1173-1178

33 725 Sauvé, V., Bruno, S., Berks, B.C., and Hemmings, A.M. (2007) The SoxYZ complex carries

726 sulfur cycle intermediates on a peptide swinging arm. J. Biol. Chem. 282: 23194–23204.

727 Selinger, D.W., Saxena, R.M., Cheung, K.J., Church, G.M., and Rosenow, C. (2003) Global

728 RNA half-life analysis in Escherichia coli reveals positional patterns of transcript

729 degradation. Genome Res. 13: 216–223.

730 Sievert, S.M., Kiene, R.P., and Schulz-Vogt, H. (2007) The sulfur cycle. Oceanography 20: 117–

731 123.

732 Sievert, S.M. and Vetriani, C. (2012) Chemoautotrophy at deep-sea vents: Past, present, and

733 future. Oceanography 25: 218–233.

734 Sievert, S.M., Scott, K.M., Klotz, M.G., Chain, P.S.G., Hauser, L.J., Hemp, J., et al. (2008)

735 Genome of the epsilonproteobacterial chemolithoautotroph Sulfurimonas denitrificans.

736 Appl. Environ. Microbiol. 74: 1145–1156.

737 Silva, J.C., Gorenstein, M.V., Li, G.-Z., Vissers, J.P.C., and Geromanos, S.J. (2006) Absolute

738 quantification of proteins by LCMSE a virtue of parallel ms acquisition. Mol. Cell.

739 Proteomics 5: 144–156.

740 Steudel, R. and Eckert, B. (2003) Elemental sulfur and sulfur-rich compounds. 2. Springer,

741 Berlin [u.a.].

742 Struyvé, M., Moons, M., and Tommassen, J. (1991) Carboxy-terminal phenylalanine is essential

743 for the correct assembly of a bacterial outer membrane protein. J. Mol. Biol. 218: 141–

744 148.

745 Taylor, C.D. and Wirsen, C.O. (1997) Microbiology and ecology of filamentous sulfur

746 formation. Science 277: 1483–1485.

34 747 Timmer-Ten Hoor, A. (1975) A new type of thiosulphate oxidizing, nitrate reducing

748 microorganism: Thiomicrospira denitrificans sp. Nov. Neth. J. Sea Res. 9: 344–350.

749 Tommassen, J. (2010) Assembly of outer-membrane proteins in bacteria and mitochondria.

750 Microbiology 156: 2587–2596.

751 Van Assche, E., Van Puyvelde, S., Vanderleyden, J., and Steenackers, H.P. (2015) RNA-binding

752 proteins involved in post-transcriptional regulation in bacteria. Front. Microbiol. 6:141.

753 Vizcaíno, J.A., Csordas, A., del-Toro, N., Dianes, J.A., Griss, J., Lavidas, I., et al. (2016) 2016

754 update of the PRIDE database and its related tools. Nucleic Acids Res. 44: 447-456.

755 Weissgerber, T., Dobler, N., Polen, T., Latus, J., Stockdreher, Y., and Dahl, C. (2013) Genome-

756 wide transcriptional profiling of the purple sulfur bacterium Allochromatium vinosum

757 DSM 180T during growth on different reduced sulfur compounds. J. Bacteriol. 195:

758 4231–4245.

759 Weissgerber, T., Sylvester, M., Kröninger, L., and Dahl, C. (2014) A Comparative Quantitative

760 Proteomic Study Identifies New Proteins Relevant for Sulfur Oxidation in the Purple

761 Sulfur Bacterium Allochromatium vinosum. Appl. Environ. Microbiol. 80: 2279–2292.

762 Woodruff, L.G. and Shanks, W.C. (1988) Sulfur isotope study of chimney minerals and vent

763 fluids from 21°N, East Pacific Rise: Hydrothermal sulfur sources and disequilibrium

764 sulfate reduction. J. Geophys. Res. Solid Earth 93: 4562–4572.

765 Yoshihara, E., Yoneyama, H., Ono, T., and Nakae, T. (1998) Identification of the Catalytic Triad

766 of the Protein D2 Protease in Pseudomonas aeruginosa. Biochem. Biophys. Res.

767 Commun. 247: 142–145.

35 768 Yamamoto, M., Nakagawa, S., Shimamura S., Takai, K., and Horikoshi K. (2010) Molecular

769 characterization of inorganic sulfur-compound metabolism in the deep-sea

770 epsilonproteobacterium Sulfurovum sp. NCBC37-1. Env. Microbio. 12: 1144-1153.

771 Yamamoto, M., and Takai, K. (2011) Sulfur metabolism in epsilon- and gamma-Proteobacteria

772 in deep-sea hydrothermal fields. Front. Microbiol. 2: 192

773 Zhang, Q, Meitzler J.C., Huang, S., and Morishita, T. (2000) Sequence polymorphism, predicted

774 secondary structures, and surface-exposed conformational epitopes of Campylobacter

775 major outer membrane protein. Appl. Environ. Microbiol. 68: 5679–5689.

776 Zhang, L., Zhang, C., Hu, C., Liu, H., and Qu, J. (2015) Denitrification of groundwater using a

777 sulfur-oxidizing autotrophic denitrifying anaerobic fluidized-bed MBR: performance and

778 bacterial community structure. Appl. Microbiol. Biotechnol. 99: 2815–2827.

779 Zopfi, J., Ferdelman, T.G., and Fossing, H. (2004) Distribution and fate of sulfur intermediates—

780 sulfite, tetrathionate, thiosulfate, and elemental sulfur—in marine sediments. Geol. Soc.

781 Am. Spec. Pap. 379: 97–116.

782 Zybailov, B., Mosley, A.L., Sardiu, M.E., Coleman, M.K., Florens, L., and Washburn, M.P.

783 (2006) Statistical analysis of membrane proteome expression changes in Saccharomyces

784 cerevisiae. J. Proteome Res. 5: 2339–2347.

785

36 786 Table 1:

787 Overview of S. denitrificans protein identification counts for the two growth conditions

788 cyclooctasulfur (S8) and thiosulfate (S2O3). Exclusive identifications are proteins that were

789 detected in at least one replicate of one condition, but were absent in all replicates of the other

790 condition.

791

2- S8 grown cultures S2O3 grown cultures

Identified proteins total 784 822

Only in one replicate 200 176

Exclusive proteins 84 122

>1% NSAF 19 10

792

793

794

795

796

797

798

799

37 800 Figure 1: Distribution of COG categories in the S. denitrificans proteome (%NSAF =

801 Normalized Spectral Abundance Factor) and transcriptome (TPM = Transcripts Per Million) on

802 cyclooctasulfur (S8) or thiosulfate (S2O3).

803

804 Figure 2: The relative abundance of transcripts (TPM = Transcripts Per Million) and proteins

805 (%NSAF = Normalized Spectral Abundance Factor) related to flagellar biosynthesis and

806 motility. Light bars show the average values of S. denitrificans grown on cyclooctasulfur (S8)

807 and dark bars show the average of cultures grown on thiosulfate. Statistically-significant

808 differences are denoted with one (p<0.05) or two (p<0.01) asterisks. Genes indicated in bold

809 have also been identified in the proteomic dataset. Suden_0030: Flagellar hook capping protein =

810 WP_011371666.1; Suden_0031: Flagellar hook protein = WP_011371667.1; FlgE: Flagellar

811 hook = WP_011371668.1, Suden_0032; Suden_0172: Flagellin-like = WP_011371808.1;

812 Suden_0173: Flagellin-like = WP_011371809.1; Suden_0202: Flagellar hook-associated protein

813 2-like = WP_011371838.1; FliS: Flagellar protein = WP_041672386.1, Suden_0203; FliE:

814 Flagellar hook-basal body complex protein = WP_011371998.1, Suden_0363; FlgC: Flagellar

815 basal-body rod protein= WP_011371999.1, Suden_0364; FlgB: Flagellar basal-body rod protein

816 = WP_011372000.1, Suden_0365; FliF: Flagellar M-ring protein = WP_011372107.1,

817 Suden_0472; FliG: Flagellar motor switch protein = WP_011372108.1, Suden_0473;

818 Suden_0474: putative flagellar assembly protein = WP_011372109.1; Suden_0562: Flagellar P-

819 ring protein = WP_011372195.1; Suden_0733: Flagellar L-ring protein = WP_011372366.1;

820 FliL: Flagellar basal body-associated protein = WP_011372470.1, Suden_0840; Suden_1037:

821 putative flagellin = WP_011372667.1; FlgG: Flagellar basal-body rod = WP_011372733.1,

822 Suden_1103; Suden_1104: Flagellar basal body rod protein = WP_011372734.1.

38 823 Figure 3: Expression of S. denitrificans transcripts (upper panel; TPM = Transcripts Per

824 Million) and proteins (lower panel; %NSAF = Normalized Spectral Abundance Factor) involved

825 in denitrification. Light bars show the average values of S. denitrificans grown on

826 cyclooctasulfur (S8) and dark bars show the average of cultures grown on thiosulfate.

827 napAGHBFLD = Nitrate reductase (napA = WP_011373143.1, Suden_1514; napB =

828 WP_011373146.1, Suden_1517; napG = WP_041672542.1, Suden_1515; napH =

829 WP_041672543.1, Suden_1516; napF = WP_011373147.1, Suden_1518; napL =

830 WP_011373148.1, Suden_1519; napD = WP_011373150.1, Suden_1521); nirSF =

831 reductase (nirS = WP_011373599.1, Suden_1985; nirF = WP_011373602.1, Suden_1988);

832 norCB = nitric oxide reductase (norC = WP_011373597.1, Suden_1983; norB =

833 WP_011373598.1, Suden_1984); nosZ1,2 = nitrous oxide reductase (nosZ1 = WP_011372928.1,

834 Suden_1298; nosZ2 = WP_011373385.1, Suden_1770).

835

836 Figure 4: A) The relative abundance of expressed SOX (sulfur oxidation multienzyme complex)

837 and SQR (sulfide quinone reductase) proteins (%NSAF = Normalized Spectral Abundance

838 Factor) and transcripts (TPM = Transcripts Per Million). Light bars show the average values of

839 S. denitrificans grown on cyclooctasulfur (S8) and dark bars show the average of cultures grown

840 on thiosulfate. Statistically significant differences (p<0.05) are denoted with an asterisk. OMP

841 (outer membrane protein) = WP_011373531.1, Suden_1917; soxH-like = WP_011373670.1,

842 Suden_2056; SOX (sulfur oxidation multienzyme complex): soxZ2Y2DC: soxZ2 =

843 WP_011373671.1, Suden_2057; soxY2 = WP_011373672.1, Suden_2058; soxD =

844 WP_011373673.1, Suden_2059; soxC = WP_011373674.1, Suden_2060 ; soxXY1Z1AB: soxX =

845 WP_011371896.1, Suden_0260; soxY1 = WP_011371897.1, Suden_0261; soxZ1 =

39 846 WP_011371898.1, Suden_0262; soxA = WP_011371899.1, Suden_0263; soxB =

847 WP_011371900.1, Suden_0264) and SQR (sulfide quinone reductase = WP_011372252.1,

848 Suden_0619). B) The relative abundance of transcripts (upper panel; TPM = Transcripts Per

849 Million) and proteins (lower panel; %NSAF = Normalized Spectral Abundance Factor) of the

850 proposed polysulfide reductase (Suden_0498-Suden_0450: WP_011372132.1-

851 WP_011372134.1).

852

853 Figure 5: Model for the oxidation of elemental sulfur chains in S. denitrificans. The activation

2- 854 mechanism of cyclooctasulfur and the hydrolysis step resulting in the liberation of SO4 from the

855 outer sulfonate group (indicated with a “?”) are currently unknown. The ‘x7’ indicates that the

856 sulfur chain attached to SoxY2 might be oxidized completely (or in part) before accepting a new

857 sulfur chain. Sulfur is indicated as black dot, whereas oxygen is indicated as small white circles

858 on sulfur.

40 859 Supplementary Figure S1: Growth curves (dotted lines) of S. denitrificans cultures grown on

860 thiosulfate (upper panel) or cyclooctasulfur (lower panel), as determined via cell counts after

861 DAPI staining. Arrows indicate the time of sampling of the biological replicates.

862

863 Supplementary Figure S2: Distribution of the proteomic (left) and transcriptomic (right)

864 expression of S. denitrificans cultures grown on cyclooctasulfur (x-axis) vs. thiosulfate (y-axis).

865 Proteins and ORFs with statistically significant differences in expression are depicted in red.

866

867 Supplementary Figure S3: Gene expression (TPM = Transcripts Per Million) of the cbb3-type

868 cytochrome c oxidase (fixNOQP, fixN = WP_011371717.1, Suden_0081; fixO =

869 WP_011371718.1, Suden_0082; fixQ = WP_011371719.1, Suden_0083; fixP =

870 WP_011371720.1, Suden_0084), the membrane bound [Ni,Fe]-uptake hydrogenase (hydCBA,

871 hydC = WP_041672535.1, Suden_1434; hydB = WP_011373064.1, Suden_1435; hydA =

872 WP_011373065.1, Suden_1436) and the membrane bound formate dehydrogenase (fdhDCBAA,

873 fdhD = WP_011372449.1, Suden_0817; fdhC = WP_011372450.1, Suden_0818; fdhB =

874 WP_011372451.1, Suden_0819; fdhA = WP_011372452.1, Suden_0820; fdhA =

875 WP_041672204.1, Suden_0821; fdx = WP_011372455.1, Suden_0824). Light bars show the

876 average values of S. denitrificans grown on cyclooctasulfur (S8) and dark bars show the average

877 of cultures grown on thiosulfate.

878

879

41 880 Supplementary Table 1: Transcriptome and proteome of Sulfurimonas denitrificans

881 displayed with the locus tag, NCBI protein ID number, length of the gene in base pairs [bp], the

882 molecular weight of the protein in kilo Dalton [kDa], transcripts per million [TPM], percent

883 normalized spectral abundance factor [%NSAF] and the annotation. Both TPM and %NSAF are

884 given as an average of the biological replicates grown with cyclooctasulfur [S8] and thiosulfate

885 [S2O3]. In addition, the p-values for both the transcripts and proteins are provided, with p-values

886 <0.01 highlighted in light blue and p-values <0.05 highlighted in dark blue.

887

888 Supplementary Table 2: Transcriptomic data collected before and after quality control

889 (QC). S8-1-3 are the biological replicates of Sulfurimonas denitrificans grown with

890 cyclooctasulfur and T-1 and T-2 are the two biological replicates grown with thiosulfate.

Reads after Bases after Mapped

Library Reads total Bases total QC QC reads % mapped

S8-1 1.09E+07 1.64E+09 1.03E+07 1.09E+09 9.51E+06 93%

S8-2 7.85E+06 1.18E+09 7.09E+06 7.10E+08 6.57E+06 93%

S8-3 9.61E+06 1.44E+09 8.58E+06 7.72E+08 7.98E+06 93%

T-1 9.18E+06 1.38E+09 8.31E+06 8.38E+08 7.69E+06 92%

T-2 1.06E+07 1.58E+09 9.56E+06 9.67E+08 8.68E+06 91%

891

42

D C C D

Y Z ? 2 ?

D C ? - D C e D C C D 6 C D C D Y Z 2 Y Z x8? 2 O 2 3H2O 3H x8? D C x8? ? ? C D D C B H C D 6e-

Y Z 2