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. 2023 Mar 17;48:109065. doi: 10.1016/j.dib.2023.109065

Carbon, nitrogen and sulphur isotope data of archaeological fish and mammal bone collagen from Lithuania

Harry K Robson a,, Kurt J Gron b, Darren R Gröcke c, Giedrė Piličiauskienė d, Gytis Piličiauskas e
PMCID: PMC10060587  PMID: 37006399

Abstract

Until relatively recently, stable sulphur isotope analysis of bone collagen was seldom undertaken in bioarchaeological research. With increasing frequency, its application has proven useful in reconstructing palaeodiets and palaeoecologies, as well as identifying potential migration and mobility patterns. Here, sulphur (δ34S) isotope analysis, together with carbon (δ13C) and nitrogen (δ15N), was performed on six fish and 34 mammal bone collagen samples from 14 prehistoric sites in Lithuania dating from the Late Mesolithic (ca. 7000–5000 cal BC) to the Late Bronze Age (ca. 1100–500 cal BC). We present the first δ34S data from Lithuania, including coupled δ13C and δ15N data, offering a crucial dataset for future research to explore spatial and temporal variability in the region and beyond.

Keywords: Stable isotope analysis, Bone collagen, Palaeodiet, Palaeoeconomy, Mesolithic, Subneolithic, Neolithic, Bronze age


Specifications Table

Subject Social Sciences - Archaeology
Specific subject area Archaeology
Bioarchaeology
Stable isotope analysis
Bone collagen
Carbon
Nitrogen
Sulphur
Palaeodiet
Palaeoeconomy
Type of data Table
Figure
How data were acquired Carbon, nitrogen and sulphur stable isotope measurements were obtained by Isotope Ratio Mass Spectrometry (IRMS). A Costech Elemental Analyser (ECS 4010) connected to a Thermo Scientific Delta V Advantage IRMS system was used to generate the δ13C and δ15N data. However, δ34S data was generated using an IsoLink connected to a Thermo Scientific Delta V Plus IRMS.
Data format Raw
Description of data collection The bone samples were demineralised, and the collagen was extracted following a standard modified Longin method [1,2,3,4].
Data source location Institution: Durham University
City: Durham
Country: United Kingdom
Latitude and longitude for collected samples/data: Daktariškė 5 (55°47′54.82′'N, 22°23′15.68′'E), Donkalnis (55°48′26.95"N, 22°25′19.77"E), Kretuonas 1B (55°15′38.92"N, 26°5′58.18"E), Plinkaigalis (55°24′38.27"N, 23°38′48.67"E), Spiginas (55°46′3.93"N, 22°25′2.24"E), Šventoji 1 (56°1′1.92′'N, 21°5′21.85′'E), Šventoji 2 (56°0′53.75′'N, 21°5′10.22′'E), Šventoji 3 (56°0′57.18′'N, 21°5′13.20′'E), Šventoji 4 (56°0′53.23′'N, 21°5′5.87′'E), Šventoji 23 (56°0′1.68"N, 21°5′23.53"E), Šventoji 26 (56°0′8.08′'N, 21°5′27.29′'E), Šventoji 43 (55°58′50.43"N, 21°5′20.5"E), Turlojiškė (54°21′45.78"N, 23°18′3.47"E) and Žemaitiškė 2 (55°15′36.81′'N, 26°6′29.66′'E)
Data accessibility This dataset is deposited in IsoArcH [5] (www.isoarch.eu) with the following Digital Object Identifier (DOI): https://doi.isoarch.eu/doi/2022.003
Data identification number: 10.48530/isoarch.2022.003
Data is available under the Creative Commons BY-NC-SA 4.0 license.

Value of the Data

  • These data represent the first δ34S values derived from prehistoric material from Lithuania, and can be utilised for future research to examine temporal and spatial variability in the region.

  • These isotopic data will be useful to archaeologists, especially bioarchaeologists, examining palaeodiets and palaeoecologies dating to the Late Mesolithic, Subneolithic, Neolithic and Bronze Age throughout Europe.

  • These data supplement the limited number of δ13C and δ15N data obtained previously from prehistoric fish bone collagen [see 6].

  • These data can be compared with other data from prehistoric sites in Lithuania and beyond.

1. Objective

For more than 30 years, stable isotope analysis has been successfully employed in palaeodietary reconstructions. Its application to identify palaeomobility has, however, only recently gathered momentum. To determine the origin(s) of potential migrants and evaluate the extent of mobility amongst prehistoric communities in Lithuania, associated with the Comb Ware and Corded Ware cultures, the IZOMOB project (2020-2022) was launched. Sulphur (δ34S), strontium (87Sr/86Sr) and oxygen (δ18O) isotope analyses was undertaken on modern soil and water samples as well as a range of modern and prehistoric faunal and floral remains. This dataset is one output of that project.

2. Data Description

These data include carbon (δ13C), nitrogen (δ15N) and sulphur (δ34S) stable isotope values extracted from fish and mammal bone samples. A number of taxa were sampled, including aurochs (Bos primigenius), domestic cattle (Bos taurus), common bream (Abramis brama), domestic dog (Canis familiaris), Eurasian beaver (Castor fiber), goat (Capra sp.), harp seal (Pagophilus groenlandicus), human (Homo sapiens), northern pike (Esox lucius) and wild boar (Sus scrofa), representing a range of behavioural life histories and habitat uses. The specimens date to the Late Mesolithic (ca. 7000–5000 cal BC), Subneolithic (ca. 5000–2900 cal BC), Neolithic (ca. 2900–1800 cal BC), Early Bronze Age (ca. 1800–1100 cal BC) and Late Bronze Age (ca. 1100–500 cal BC). The samples were derived from 14 prehistoric sites (i.e., Daktariškė 5, Donkalnis, Kretuonas 1B, Plinkaigalis, Spiginas, Šventoji 1, Šventoji 2, Šventoji 3, Šventoji 4, Šventoji 23, Šventoji 26, Šventoji 43, Turlojiškė and Žemaitiškė 2) in Lithuania (Fig. 1). The localities are represented by burial grounds, fishing stations, ritual depositions and settlement sites which have differing research histories. Excavations took place during the 20th and 21st centuries [see [6], [7], [8], [9], [10], [11]]. Samples were collected by one of us (GyP) and then submitted for isotopic analysis to the Stable Isotope Biogeochemistry Laboratory (SIBL), managed and operated by another one of us (DRG) in the Department of Earth Sciences, Durham University.

Fig. 1.

Fig 1

Locations of the 14 prehistoric sites in Lithuania from where the samples were obtained.

In total, 22 animal and 18 human bone samples were prepared for analysis. Of these, 27 produced sufficient quantities of well-preserved collagen for carbon and nitrogen stable isotope analysis, yielding atomic C:N ratios within the acceptable range of between 2.9 and 3.6 according to DeNiro [4]. A total of 16 samples yielded sufficient quantities of well-preserved collagen for sulphur stable isotope analysis, producing atomic C:S and N:S ratios within the acceptable ranges of between 600 ± 300 and 200 ± 100, respectively, according to Nehlich and Richards [12]. Four samples, however, yielded only enough collagen for a single sulphur measurement, consequently carbon and nitrogen stable isotope data from a previous study was utilised [8]. These data also yielded atomic C:N ratios which were within the acceptable range, indicating a low likelihood of diagenesis [4]. Stable isotope measurements were performed in the Stable Isotope Biogeochemistry Laboratory (SIBL) at Durham University using a Thermo IsoLink coupled to a Thermo Scientific Delta V Plus Advantage isotope ratio mass spectrometer. Sulphur isotope ratios are reported in standard delta (δ) notation in per mil (‰) relative to the VCDT scale. Correction of δ34S was performed using four international standards (IAEA-S-1, IAEA-S-2, IAEA-S-3, NBS 127): this provided a linear range in δ34S between -32.5‰ and +22.6‰. Analytical uncertainty of δ34S is typically ±0.2‰ for replicate analyses of the international standards. Total sulphur is determined as part of the isotopic analysis (i.e., total peak area) using an internal standard, sulphanilamide (18.6196% sulphur). Further details on analytical procedures, standards and errors for carbon and nitrogen are reported in Walser et al. [13].

We obtained a grand total of 27 δ13C and δ15N values. In addition, 20 δ34S values were obtained, making it the largest dataset of δ34S values from prehistoric sites in Lithuania. The δ13C and δ15N values are plotted against the δ34S values in Fig. 2. In Fig. 3 the dataset is compared with previously published data from Lithuania. Table 1 presents the data per sample, including sample number, site, grave number or individual, period, species or taxon, skeletal element, ontogentic age, context, excavation campaign and/or find number, %N, δ15N, %C, δ13C, %S, δ34S, C:N, C:S and N:S. Summary statistics for the various groups and species or taxon are shown in Table 2. This dataset is deposited in IsoArcH [5] (www.isoarch.eu) with the following Digital Object Identifier (DOI): https://doi.isoarch.eu/doi/2022.003; data identification number: 10.48530/isoarch.2022.003; data is available under the Creative Commons BY-NC-SA 4.0 license.

Fig. 2.

Fig 2

Carbon (δ13C), nitrogen (δ15N) and sulphur (δ34S) stable isotope data obtained on fish and mammal bone collagen.

Fig. 3.

Fig 3

Comparison of the carbon (δ13C) and nitrogen (δ15N) stable isotope data for fauna (a) and humans (b) obtained with previously published data from Lithuania [6,8,9,16]. Connecting lines, measurements made on different skeletal elements of the same individual. This variation likely reflects differences in the bone turnover rates between skeletal elements rather than inter-instrument variation between institutions [see 17].

Table 1.

Fish and mammal bone samples and stable isotope data. Note that the data has been sorted alphabetically according to the site. Although the C:S ratio for one sample (HUM-08), a human humerus from Kretuonas 1B (Grave No. 3), was unacceptable according to the criteria defined by Nehlich and Richards [12], both the C:N and N:S ratios were within the acceptable ranges defined by DeNiro [4] and Nehlich and Richards [12]. As such, it was included here. Blank, no collagen preserved or no data. *, mean of stable isotope data from NAU and UOY [see 8]. **, stable isotope data from NAU only [see 8].

Sample no. Site, grave no./individual Period Species or taxon Skeletal element, ontogenetic age, context, excavation campaign, find no. %N δ15N (‰) %C δ13C (‰) %S δ34S (‰) Atomic C:N Atomic C:S Atomic N:S
AN-01 Daktariškė 5 Subneolithic Esox lucius Cleithrum, sin., 60-70 cm in length, 2016 year, No. 2557 0.3 -0.1
AN-02 Daktariškė 5 Subneolithic-Early Bronze Age Canis familiaris Radius, sin. 14.29 9.89 40.08 -21.84 0.31 -0.39 3.27 350.64 107.22
AN-03 Daktariškė 5 Subneolithic-Early Bronze Age Capra sp. Mandible, sin., adult 13.60 3.84 38.29 -22.59 0.26 8.61 3.28 395.47 120.42
AN-04 Daktariškė 5 Subneolithic-Early Bronze Age Bos taurus Femur, sin. 14.67 4.61 41.69 -23.35 0.27 5.53 3.31 407.42 122.93
AN-05 Daktariškė 5 Subneolithic-Early Bronze Age Bos primigenius Metacarpus, sin., 2016 year, No. 1797 14.90 5.26 41.91 -22.44 0.25 7.72 3.28 443.83 135.29
AN-06 Daktariškė 5 Subneolithic Sus scrofa Mandible, 10 months-year, 2016 year, No. 569 10.58 3.49 32.32 -23.49 0.18 6.94 3.56 482.36 135.36
AN-07 Daktariškė 5 Subneolithic-Early Bronze Age Castor fiber Fibula, dex., young, 2016 year, No. 1172 13.79 3.69 38.31 -22.02 3.24
HUM-04 Donkalnis, Grave No. 1 Subneolithic Homo sapiens Femur diaphysis, 20-25 year-old female 13.84 11.84 37.99 -24.26 0.20 3.17 3.20 502.10 156.81
HUM-05 Donkalnis, Grave No. 6 Subneolithic Homo sapiens Fibula diaphysis, 35-40 year-old female 15.48 11.63 42.13 -22.32 0.21 3.37 3.17 545.11 171.69
HUM-06 Donkalnis, Grave No. 7 Late Subneolithic Homo sapiens Fibula diaphysis, >45 year-old male 9.65 10.61 28.29 -21.74 3.42
HUM-07 Donkalnis, 5th individual Late Mesolithic Homo sapiens J245D, ∼7 year-old individual 0.21 4.18
AN-08 Kretuonas 1B Subneolithic-Neolithic Esox lucius Precaudal vertebra, 80-100 cm in length
AN-09 Kretuonas 1B Subneolithic-Neolithic Bos primigenius 2nd phalanx
AN-10 Kretuonas 1B Subneolithic-Neolithic Sus scrofa Astragalus, sin. 8.48 4.84 25.10 -23.31 3.45
AN-11 Kretuonas 1B Subneolithic-Neolithic Castor fiber Tibia, dex., young 12.41 3.29 36.85 -22.72 3.46
AN-12 Kretuonas 1B Subneolithic-Neolithic Cyprinidae, cf. Abramis brama 1 x precaudal vertebra; 3 x caudal vertebrae
HUM-08* Kretuonas 1B, Grave No. 3 Subneolithic Homo sapiens Humerus diaphysis, 50-55 year-old male 13.90 11.80 38.70 -22.80 0.11 5.97 3.20 945.43 291.18
HUM-17 Plinkaigalis, Grave No. 241 Neolithic Homo sapiens Femoral distal epiphysis, 50-55 year-old female 10.36 8.85 29.24 -21.55 0.22 7.39 3.29 360.77 109.64
HUM-18 Plinkaigalis, Grave No. 242 Neolithic Homo sapiens Upper dex. molar (M2), root, >40 year-old female
HUM-01 Spiginas, Grave No. 1 Subneolithic Homo sapiens Femur diaphysis, 35-45 year-old male 10.21 11.83 29.52 -23.07 0.18 3.79 3.37 429.74 127.39
HUM-02 Spiginas, Grave No. 3 Late Mesolithic Homo sapiens Fibula diaphysis, indeterminate female 14.84 12.10 41.96 -23.13 0.24 3.33 3.30 469.20 142.24
HUM-03 Spiginas, Grave No. 4 Late Mesolithic Homo sapiens 30-35 year-old female 15.02 12.92 41.78 -22.59 0.22 -2.53 3.24 509.59 157.15
AN-16 Šventoji 1 Subneolithic-Neolithic Canis familiaris Mandible, 1968 year 12.62 14.46 35.89 -16.38 3.32
AN-18 Šventoji 2 Subneolithic-Neolithic Sus scrofa Femur, sin., adult 14.03 4.47 40.43 -21.47 3.36
AN-19 Šventoji 2 Subneolithic-Neolithic Castor fiber Femur, sin., young 14.37 4.02 41.32 -22.56 3.35
AN-20 Šventoji 3 Subneolithic-Neolithic Pagophilus groenlandicus Os temporale, sin., adult, 1972 year 14.46 9.51 40.80 -23.33 3.29
AN-14 Šventoji 4 Subneolithic Esox lucius Dentary, sin., 90-100 cm in length, 2014 year, No. 1514 (1038)
AN-15 Šventoji 4 Subneolithic Abramis brama Preopercular, subopercular, opercular, 2014 year, No's. 1218-1227 12.50 7.92 36.83 -23.94 3.44
AN-17 Šventoji 4 Subneolithic-Neolithic Bos primigenius Maxilla, 2003 year 13.68 5.01 38.21 -22.66 3.26
HUM-09 Šventoji 23, single bone No. 1 Subneolithic Homo sapiens 13-18 year-old individual
HUM-10 Šventoji 23, single bone No. 2 Subneolithic Homo sapiens 20-30 year-old individual
HUM-12 Šventoji 26, single bone No. 1 Subneolithic Homo sapiens Femur diaphysis
HUM-11 Šventoji 43, single bone No. 2 Subneolithic Homo sapiens Lower dex. molar
AN-21 Turlojiškė Late Bronze Age Esox lucius Dentary, dex., 70-80 cm in length, 1998 year 14.28 12.56 40.38 -16.70 3.30
AN-22 Turlojiškė Late Bronze Age Capra sp. Humerus, dex., >11-13 months, 1998 year, IV, I trench, C-11 13.39 5.42 36.31 -21.18 0.29 0.80 3.16 339.97 107.52
HUM-13 Turlojiškė, Grave No. 3 Late Bronze Age Homo sapiens Ulna diaphysis, 25-30 year-old male 14.08 9.17 39.03 -18.36 0.25 6.51 3.23 410.15 126.83
HUM-14** Turlojiškė, Grave No. 4 Late Bronze Age Homo sapiens 20-25 year-old male 15.40 9.40 43.40 -16.90 0.25 6.99 3.30 466.07 141.81
HUM-15 Turlojiškė, Grave No. 5 Late Bronze Age Homo sapiens "IIv, 6 perk.", 1999 year 14.09 8.88 40.00 -17.88 0.28 2.92 3.31 377.44 114.00
HUM-16 Turlojiškė, Grave No. 6 Late Bronze Age Homo sapiens "II v, 7 perk.", 1999 year 13.05 9.00 37.55 -18.92 0.28 2.98 3.36 356.75 106.30
AN-13 Žemaitiškė 2 Early Bronze Age Bos taurus M2 12.99 4.97 36.44 -23.60 0.29 8.26 3.27 340.39 104.03

Table 2.

Summary statistics for the various groups and species (or taxon). Note that the human data has been disaggregated according to site. Standard deviations have only been calculated for N > 2. Blank, no data.

Group N Mean δ13C (‰) Max δ13C (‰) Min δ13C (‰) Range δ13C (‰) N Mean δ15N (‰) Max δ15N (‰) Min δ15N (‰) Range δ15N (‰) N Mean δ34S (‰) Max δ34S (‰) Min δ34S (‰) Range δ34S (‰)
Homo sapiens 12 -21.13 -16.90 -24.26 7.36 12 10.67 12.92 8.85 4.07 12 4.01 7.39 -2.53 9.92
Donkalnis 3 -22.77 -21.74 -24.26 2.52 3 11.36 11.84 10.61 1.23 3 3.57 4.18 3.17 1.01
Kretuonas 1B 1 -22.80 1 11.80 1 6.00
Plinkaigalis 1 -21.55 1 8.85 1 7.39
Spiginas 3 -22.93 -22.59 -23.07 0.48 3 12.28 12.92 11.83 1.09 3 1.53 3.79 -2.53 6.32
Turlojiškė 4 -18.02 -16.90 -18.92 2.02 4 9.11 9.40 8.88 0.52 4 4.85 6.99 2.92 4.07
Semi-aquatic herbivores 3 -22.07 -22.72 -22.02 -0.70 3 5.85 4.02 3.29 0.73
Castor fiber 3 -22.22 -22.72 -22.02 -0.70 3 6.50 4.02 3.29 0.73
Terrestrial herbivores 6 -21.98 -21.18 -23.60 2.42 6 6.09 5.42 3.84 1.58 5 6.31 8.61 0.80 7.81
Bos primigenius 2 -22.28 -22.44 -22.66 0.22 2 5.88 5.26 5.01 0.25 1 7.72
Bos taurus 2 -22.99 -23.35 -23.60 0.25 2 4.31 4.97 4.61 0.37 2 7.11 8.26 5.53 2.73
Capra sp. 2 -21.98 -21.18 -22.59 1.41 2 6.09 5.42 3.84 1.58 2 6.31 8.61 0.80 7.81
Marine carnivores 1 -23.33 1 9.51
Pagophilus groenlandicus 1 -23.33 1 9.51
Freshwater fish 2 -21.00 -16.70 -23.94 7.24 2 8.28 12.56 7.92 4.64 1 -0.13
Abramis brama 1 -23.94 1 7.92
Esox lucius 1 -16.70 1 12.56 1 -0.13
Omnivores 5 -22.29 -16.38 -23.49 7.11 5 5.83 14.46 3.49 10.97 2 5.68 6.94 -0.39 7.33
Canis familiaris 2 -22.74 -16.38 -21.84 5.46 2 5.42 14.46 9.89 4.57 1 -0.39
Sus scrofa 3 -22.01 -21.47 -23.49 2.02 3 6.42 4.84 3.49 1.35 1 6.94

The humans (n = 12) had a broad range of δ13C (-24.3‰ to -16.9‰), δ15N (+8.9‰ to +12.9‰) and δ34S (-2.5‰ to +7.4‰) values. There were two groups with one indicating the consumption of freshwater derived protein and the other demonstrating the consumption of C4 foodstuffs, including millet [see 8], agreeing with their chronological affiliation (i.e., hunter-gatherer-fishers in the former and agriculturalists in the latter). Since all human δ34S values were below +10.0‰, which is considered a minimum for the impacts of the sea spray affect [see 18], they indicate inland residency. This is perhaps not unexpected since the site closest to the coast yielding δ34S values was 86 km away (i.e., Donkalnis), while the impacts of the sea spray affect are known up to ca. 30 km inland [18].

The semi-aquatic herbivores (n = 3), namely the Eurasian beaver, had a narrow range of δ13C (-22.7‰ to -22.0‰) and δ15N (+3.3‰ to +4.0‰) values, agreeing with their habitat use.

Similarly, the terrestrial herbivores (n = 6), including aurochs, domestic cattle and goat, had a narrow range of δ13C (-23.6‰ to -21.2‰) and δ15N (+3.8‰ to +5.4‰) values, though variable δ34S (n = 5; +0.8‰ to +8.6‰) values. Despite this, taken together these data indicate that they were living in somewhat similar environments unaffected by the canopy effect [19] and/or a contribution of sea spray. Similarly, the site nearest the coast yielding δ34S values was some 84 km away (i.e. Daktariškė 5).

The one marine carnivore in the dataset, a harp seal from Šventoji 3, had a δ13C value of -23.3‰ and a δ15N value of +9.5‰. These data indicate residency in a 13C-enriched environment such as the Šventoji Palaeolake directly in front of the site or the nearby Baltic Sea [see 14,15].

Several common bream remains from Šventoji 4 were combined to ensure that enough collagen could be extracted for stable isotope analysis. The δ13C (-23.9‰) and δ15N (+7.9‰) values indicate residency in a similar environment to the harp seal from Šventoji 3. In contrast, a northern pike dentary from the wetland site of Turlojiškė had a δ13C value of -16.7‰ and a δ15N value of +12.6‰, which despite being notably higher than the common bream, indicated freshwater residency [see 20]. Only one fish bone, a northern pike cleithrum from Daktariškė 5, yielded sufficient quantities of collagen for a single sulphur measurement (-0.1‰), which likewise demonstrated residency in a freshwater environment.

While the two dog bones had divergent δ13C (-21.8‰ and -16.4‰) and δ15N values (+9.9‰ and +14.5‰), it is possible that both either consumed resources from a freshwater environment or perhaps from a fresh water in the case of the former, and an intermediary waterbody enriched in 13C, such as the Baltic Sea [14,15], in the latter. The one sulphur measurement (-0.4‰) obtained from a dog from Daktariškė 5 demonstrated inland residency.

The wild boars (n = 3) had a narrow range of δ13C (-23.5‰ to -21.5‰) and δ15N (+3.5‰ to +4.8‰) values. Despite being derived from three different sites (i.e., Daktariškė 5, Kretuonas 1B and Šventoji 2), these data indicate little omnivory. The single sulphur measurement (+6.9‰) demonstrated inland residency.

3. Experimental Design, Materials and Methods

A range of species (or taxa) from each assemblage were selected for analysis. This ensured that the same individual was not sampled more than once. With regards to the human bone samples, all individuals were derived from different burials or in the case of the loose human bones from Šventoji 23 were clearly separated by ontogenetic age (Table 1).

The specimens were cleaned of obvious surface contamination using a diamond-tipped dental burr. Then, the samples were demineralised, and the collagen was extracted following a standard modified Longin method [1], [2], [3], [4]. Stable isotope measurements were performed in the Stable Isotope Biogeochemistry Laboratory (SIBL) at Durham University — the analytical methods are described in more detail in Gröcke et al. [21].

Ethics Statements

This study does not involve any modern human or animal subject.

CRediT authorship contribution statement

Harry K. Robson: Conceptualization, Formal analysis, Investigation, Data curation, Writing – original draft, Writing – review & editing, Visualization, Project administration. Kurt J. Gron: Formal analysis, Investigation, Writing – review & editing. Darren R. Gröcke: Formal analysis, Investigation, Writing – review & editing. Giedrė Piličiauskienė: Resources, Writing – review & editing. Gytis Piličiauskas: Conceptualization, Resources, Writing – review & editing, Visualization.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships which have or could be perceived to have influenced the data reported in this article.

Acknowledgment

We thank the Leverhulme Trust (Grant RPG-2016-081) for support during aspects of this research.

Data availability

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