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PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 1 / 21 OPEN ACCESS Citation: Ramírez-Cruzado Aguilar-Galindo S, Luciañez-Triviño M, Muñiz Guinea F, Cáceres Puro LM, Toscano Grande A, Díaz-Guardamino M, et al. (2025) From the jaws of the “Leviathan”: A sperm whale tooth from the Valencina Copper Age Megasite. PLoS One 20(5): e0323773. https://doi.org/10.1371/ journal.pone.0323773 Editor: Annalisa Zaccaroni, Universita di Bologna, ITALY Received: May 31, 2024 Accepted: April 15, 2025 Published: May 14, 2025 Copyright: © 2025 Ramírez-Cruzado AguilarGalindo et al . This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited. Data availability statement: All relevant data are within the manuscript. Funding: ATG-This work has been co-financed by the FEDER Program/ Junta RESEARCH ARTICLE From the jaws of the “Leviathan”: A sperm whale tooth from the Valencina Copper Age Megasite Samuel Ramírez-Cruzado Aguilar-Galindo 1,2☯*, Miriam Luciañez-Triviño1☯, Fernando Muñiz Guinea3☯, Luis Miguel Cáceres Puro4☯, Antonio Toscano Grande4, Marta Díaz-Guardamino 5, Juan Manuel Vargas Jiménez6, Thomas Xavier Schuhmacher7, Rafael María Martínez Sánchez 8, Santiago Guillamón Dávila 8, Joaquín Rodríguez Vidal 4, Leonardo García Sanjuán1☯ 1 Department of Prehistory and Archaeology, University of Seville, Seville, Spain, 2 Canary Islands Oceanographic Center (COC), Spanish Institute of Oceanography (IEO), Spanish Research Council (CSIC), Santa Cruz de Tenerife, Spain, 3 Department of Crystallography, Mineralogy and Agricultural Chemistry, Faculty of Chemistry and Geology Museum, University of Seville, Seville, Spain, 4 Department of Earth Sciences, University of Huelva, Huelva, Spain, 5 Department of Archaeology, Durham University, Durham, United Kingdom, 6 Servicio de Arqueología, Ayuntamiento de Valencina de la Concepción, Valencina de la Concepción, Seville, Spain, 7 German Archaeological Institute, Madrid, Spain, 8 Department of History, University of Córdoba, Córdoba, Spain ☯ These authors contributed equally to this work. * [email protected] Abstract During the excavations undertaken in 2018 at the Nueva Biblioteca sector of the Valencina Copper Age mega-site, in south-west Spain, an exceptional sperm-whale tooth was found inside a non-burial pit. This remarkable object is the first of its kind ever found for Late Prehistoric Iberia. Due to its rarity and importance, a multidisciplinary study was carried out, including photogrammetric 3D modelling, as well as taphonomic, paleontological, technological and contextual analysis. This led to a full characterisation of the artefact through the analysis of its bioerosion traces, anthropogenic marks, depositional context and socio-cultural background. The ensuing discussion covers the history and processes the tooth went through from the death of the animal and disposal on the seabed, through the disarticulation of the tooth to its collection in a coastal environment and its subsequent use and deposition in the pit. 'No permits were required for the described study, which complied with all relevant regulations.' Not far from the gate is a common tomb, where lie all those who met their death when fighting against Alexander and the Macedonians. Hard by they show a place where, it is said, Cadmus (he may believe the story who likes) sowed the teeth of the dragon, which he slew at the fountain, from which teeth men came up out of the earth. Pausanias, Description of Greece (Book 9.1-22), 2nd century AD
PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 2 / 21 Introduction As a raw material, ivory has a long history of use that goes back to, at least, the Upper Palaeolithic [1–5]. Since Prehistory, it has been used to craft a wide range of (largely) sumptuous and sacred objects, ranging from personal ornaments (bracelets, necklaces, combs) to art (sculptures, figurines, furniture) or musical instruments [6]. Because of its physical properties, which render it fairly resistant to diagenetic processes, as well as aesthetic appeal and exoticism, ivory is a unique indicator in the study of ancient crafts, arts, exchange and socio-cultural organisation. The large majority of the archaeological literature focuses on ivory from land mammals, mainly on proboscideans, but also on hippopotamus, deer, bear, wolf, etc. Thus, for the Iberian Peninsula, a vast bibliographic production reflects the presence of elephant ivory in Neolithic, Copper Age, Bronze Age and Iron Age contexts – for recent syntheses [6]. In recent years, this field of research has been expanded to include ivory (teeth) from marine mammals, particularly Odontocete cetaceans, but also Pinnipeds (seals, walruses, etc) and Sirenia. [7–13]. Undoubtedly, the use of such ivory may have been connected with the exploitation of marine mammals, a subject for which the available archaeological evidence is scant and difficult to interpret. In Africa, the evidence of the scavenging of whale carcasses goes back to the Lower Pleistocene [14]. In Europe, the processing and/or consumption of marine mammals, including cetaceans, is attested since the Upper Palaeolithic (Table 1) [15,16] and through the Mesolithic [17–20], Neolithic [12,21,22], Copper Age [10,11,23] and, of course, later historical periods [24–26]. Whether or not these de Andalucía-Consejería de Economía y Conocimiento/ Project (UHU-202052). Paleontología de mamíferos marinos del margen atlántico suribérico. The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript. Competing interests: The authors have declared that no competing interests exist. Table 1. Record of remarkable cetacean remains at archaeological sites in Europe belonging to Neolithic and Chalcolithic. Material Processing/ Consumption Chronology Location Publication Bowl made from a whale vertebra Processed 3100-2200 bc, Neolithic Skara Brae, Scotland National Museum Scotland Collection Whale bone carved figure Processed 3100-2200 bc, Neolithic Skara Brae, Scotland National Museum Scotland Collection Sperm whale tooth Unprocessed End of Neolithic, start of Copper Age Sardinia, Italy Melis y Zedda (2021) Cetacean rib Unprocessed Copper Age Leceia, Portugal Cardoso (1995) Cetacean rib Unprocessed Copper Age Alpena, Portugal Zbyszewski (1977) Five buttons with V-hole perforation made from sperm whale teeth Processed Copper Age Verdelha dos Ruivos, Portugal Schuhmacher et al. (2009) 17 objects (beads, buttons and a cylinder) made from sperm whale bone Processed Copper Age Praia das Maçãs, Verdelha dos Ruivos Palmela, Dolmen das Conchadas and Pedra de Ouro (Lisboa) Schuhmacher et al. (2013) Buttons with V-hole perforation made from sperm whale bone Processed Copper Age Galera da Cisterna, Portugal Zilhao (2016) One double perforated button with appendages made of sperm whale teeth Processed Copper Age Madrid Liesau (2020) Two vertebrae and a whale rib Processed Copper Age La Vital, Gandía, Spain Pascual Benito et al. (2019) https://doi.org/10.1371/journal.pone.0323773.t001
PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 3 / 21 animals were hunted in prehistory, or stranded carcasses were simply opportunistically exploited, has been and still is a matter of debate [27,28]. In this paper we present an exceptional sperm-whale tooth found at the Copper Age mega-site of Valencina de la Concepción-Castilleja de Guzmán (henceforth Valencina), located near the city of Sevilla, in south-west Spain. Following the discovery of La Pastora, a tholos-type megalithic monument, in the 1860s, and gradual, if slow, advances throughout the 20th century, research on Valencina has made substantial progress in the last two decades. In addition to its large size (c. 450 hectares), Valencina is remarkable for the scale and number of features found in it, including massive ditches up to 9–10 m across and 8–9 m deep, remarkable tholoi (such as Montelirio, Matarrubilla, Structure 10.042-10.049 and La Pastora itself) as well as tens of thousands of pits, shallow basins and shafts used for a variety of purposes [for a recent overview, see [29]. Recent research has also highlighted the amount and quality of the material culture found in some of those features, particularly (but not only) in the tholoi. Of special relevance are the objects made in elephant ivory, which not only represents the largest collection of this raw material in 3rd millennium western Europe, but also includes finely crafted and highly idiosyncratic artefacts [6,30–33]. Recent reviews of Neolithic and Copper Age Europe have discussed Valencina as a focus of early social complexity in 3rd millennium Europe - see for example [34–36]. The sperm whale tooth studied here, found in excavations undertaken in 2018 at the Nueva Biblioteca sector of Valencina, is the first of its kind ever found in the Iberian Peninsula, and only the second published for the Western Mediterranean, after the one recently discovered at the site of Monte d’Accoddi, Sardinia [22]. A multidisciplinary approach is followed, including techniques and expertise from biology, geology, archaeology and taphonomy. This leads to a full characterisation of the item through the analysis of its bioerosion traces, anthropogenic marks and depositional context, followed by a discussion that places this find within the general background of the use of marine resources and ivory in Copper Age Iberia. Archaeological context The Nueva Biblioteca (‘New Library’) sector is located on the northern half of Valencina (Fig 1A–1C). Excavations undertaken during the spring and summer of 2018 as a result of the construction of a new municipal library revealed a series of features, including the pit in which the sperm-whale tooth described in this paper was found. Topographically, the Nueva Biblioteca land plot is at the foot of the western slope of a gentle hill. This hill, the highest elevation of the Valencina megasite (158 masl), and designated as La Perrera, was excavated in the 1970s and yielded very interesting results, as is discussed below. The Nueva Biblioteca excavation extended over an area of 758 m2 and revealed several interesting pieces of evidence. Prominent among those is the fact that stratigraphic deposits reaching an average depth between 1.20 and 1.5 m were found across most of the sector. This is quite remarkable, because a well-known characteristic of the Valencina megasite is that the vast majority of the stratification occurs inside negative features (such as pits, shallow basins, shafts or ditches) that were cut into the local substrate of yellow sandy silts, while very little, or none, occurs outside those. The excavators were able to tell apart up to seven stratigraphic units, with three major phases of use and construction. In the earliest of those three phases, stones were used to build a feature circular in plan and measuring 28.79 m in length by 2 m in width, which was cut at three points by as many transversal ditches. This phase also included a single secondary inhumation inside a pit, measuring 1 m in maximum diameter, and involving a skull, a long bone and several other fragments (currently under study). The second construction phase involved the abandonment of the stone structure and the cutting of four shallow basins averaging 4 m of maximum diameter. The third phase involved the accumulation of clayish deposits over the entire area and new episodes of use, including five more pits. Two radiocarbon dates obtained for this study (Table 2) suggest a long period of use (c. 400 years) for the Nueva Biblioteca sector, which is in accordance with the deposition of thick layers outside underground structures as well as the diversity of features found across the sector, within a relatively small space, including three ditches, various stone features, pits, etc. The most recent of the two dates
PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 4 / 21 Fig 1. The Nueva Biblioteca sector in which the sperm whale tooth was found. A-B, geographical context; C, Pit US-123; D, stratigraphy of Pit US-123; E, general plan of the Nueva Biblioteca with the prehistoric structures discovered in this area (24,27,28,33,50,88,95: stratigraphic units). https://doi.org/10.1371/journal.pone.0323773.g001
PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 5 / 21 (MAMS 41417) place the third phase between c. 2500 and 2400 BC, that is to say, in the period leading to the abandonments of the Valencina mega-site (c. 2300 BC). It was at around this time that pit US-123 was made, and the sperm-whale tooth was deposited in it. Pit US-123 was found on the eastern side of Trench XI and, initially, approximately only one-third of it could be excavated (Fig 1C and 1D). However, upon the discovery of the sperm-whale tooth, the trench was extended to allow a fuller excavation. At the end, although the pit could not be excavated completely, its shape and measurements were established with a reasonable degree of certainty. On its upper part it had a circular plan c. 1 m in diameter, narrowing down to the bottom to 64 cm, which resulted in a conical shape. Its bottom could not be reached, the maximum recorded depth being 89 cm. The sperm-whale tooth was found on the upper third of the pit’s infill, consisting of a dark brown clayish soil with some small sandstone. No evidence of combustion was found inside the pit. The pit contained 187 pottery fragments, weighting 3.437 kg, which in general did not show a high degree of rounding. This suggests that the pottery fragments did not experience a long period of wearing before being introduced into the pit. The fragments whose shape could be discerned (34 in total) reveal the habitual pottery repertoire at Valencina, with large ‘almond-rim’ dishes (with diameters up to 40–50 cm), saucers as well as smaller globular vessels and bowls – see a recent review [38]. It is worth noting a fragment decorated with strokes of black paint on reddish coating, of a kind well known in Valencina [39], which also shows two perforations. A fragment of an ‘almond-rim’ plate also showed three perforations, plus a fourth, unfinished one, which were placed apparently randomly. The concentration of four perforations on a single pottery fragment is a very rare occurrence at Valencina and seems to suggest some kind of ‘drilling’ practice, rather than the need to repair the vessel. Indeed, the presence of two fragments with perforations in a single pit is also quite infrequent at the site. In general, it is intriguing that this ‘abundance’ of perforations on pottery should occur in a pit containing a sperm whale tooth that shows obvious signs of perforation (see discussion below). Pit SU-123 also contained seven fragments of macro-lithic tools, possible grinding stones of the kind well recorded at the site [40] as well as one small, knapped blade, probably in quartzite. The dearth of knapped lithics in this pit is also quite remarkable, considering how frequent these items are across the site. Finally, Pit SU-123 also contained 87 animal skeletal remains. They are in a very good state of preservation, showing excellent chemical integrity, as is usual in the bone remains found in the Nueva Biblioteca sector. The zooarchaeological analysis revealed a total of 26 taxonomically identifiable remains (Table 3). With regard to the taxa identified, these were composed entirely of domestic mammals related to livestock activity, including domestic cattle (Bos taurus), goats (Capra hircus), sheep (Ovis aries), indeterminate goats (Caprinae) and swine (Sus scrofa). The latter taxon predominates in the total determined assemblage, as appears to be the case in the Table 2. Radiocarbon dates for the Nueva Biblioteca sector of Valencina. LAB. ID SAMPLE CONTEXT AGE BP AGE CAL BC 2σẟ13C AMS [‰] C:N C % MAMS-41416 Sus (mandible) UD 21 – Central strip 4049 ± 42 2848-2468 -37.6 3.5 4.2 MAMS-41417 Medium-sized land mammal (rib) UD 21 – Central strip 3986 ± 24 2572-2463 -20.9 3.3 24.9 All calibrations with Oxcal 4.4 based on the IntCal20 Northern Hemisphere radiocarbon age calibration curve [37]. https://doi.org/10.1371/journal.pone.0323773.t002 Table 3. Number of identified remains per taxon (NISP) and unidentified remains per group (NR) and weight of remains (WR). UD 123 Bos taurus Capra hircus Ovis aries Caprinae Sus scrofa LSM MSM TOTAL NISP/NR 4 9 1 1 11 19 42 87 WR (g) 485,99 52,1 7,16 3,75 92,03 102,4 95,35 838,78 LSM, Macromammals; MSM, Mesomammals. https://doi.org/10.1371/journal.pone.0323773.t003
PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 6 / 21 entire Nueva Biblioteca zooarchaeological assemblage. No marine mammals were identified. All of the remains were completely devoid of cutting or splitting marks linked to quartering. However, in at least three of them, fractures made in fresh bone were observed. More than 50% of the identified remains of land mammals (23, Table 3) showed signs of thermoalteration, ranging from relatively low temperatures, with yellowish or brownish colourations, to relatively high temperatures with completely calcinated bones. The latter is mainly observed among the pig remains, and also exists in one of the undetermined caprine remains. The soil forming the infill of pit US-123 was very homogeneous, and no strata, nor specific features, were observed in it. Therefore, this infill is interpreted as anthropogenic in nature and resulting from a single event, in which a series of items (pottery, lithic tools, animal remains and the sperm-whale tooth) were deliberately buried as a structured deposition (or offering) as a result of a single event, probably ceremonial in character. Material The specimen studied here is currently kept in the Valencina Municipal Museum and tagged as [Nv. Biblio. 2018/13-S. XI-UD.123-nº 1]. It corresponds to an incomplete isolated sperm whale tooth (preserving approximately its upper half) in a good state of preservation (Fig 2). Fig 2. The tooth of sperm whale studied. A: lingual view, B: mesial view, C: labial view, D: distal view, E: root section detail, F: occlusal view; G: reconstruction with a complete tooth. Shaded area = missing part of the tooth. A high resolution 3D model of the tooth can be viewed and downloaded here: https://skfb.ly/ovWY6. https://doi.org/10.1371/journal.pone.0323773.g002
PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 7 / 21 Methods Since the tooth is the first osseous remain of a marine mammal ever found at Valencina, and because of its special character, it has been studied using various methods in order to obtain as much information as possible about its origin, transformation and cultural significance. A 3D model of the tooth was made in line with recent advances in the field of 3D imaging and digital technologies for the study of archaeological artefact, which have led to the development of digital archaeology, favouring noninvasive studies, avoiding excessive manipulation and providing information enabling the visualization and examination of very subtle details that may be invisible to the naked eye [41–44]. Photographs were taken with a Nikon d3400 camera equipped with a Nikkor af-p 18–55 mm lens. The photogrammetric processing was carried out using Agisoft Metashape software available at the computer services of Durham University. Post-processing phase involved the analysis, treatment, fit to the plane, orientation and scale assignment to the textured photogrammetric models. The image analysis was carried out using Agisoft PhotoScan. Applying various algorithms and false colour analysis in MeshLab and CloudCompare, it was possible to emphasise the morphology of the intended tooth surface, facilitating its visualisation, analysis and interpretation (the resulting 3D model can be viewed and downloaded here: https://skfb.ly/ovWY6). This work made it easy to interpret and visualize the tooth without having to handle it, thus minimizing the risk of damaging it, as well as to be able to present the tooth to the media or exhibit the 3D replica in the museum instead of the real one. To identify possible traces of anthropic manipulation, the tooth was examined with a ShuttlePix P-400R digital microscope (up to 400X) from the University of Seville´s CITIUS microanalysis service. The description of the technical surface traces and the general vocabulary for the technology were based on Averbouh and Provenzano [45] and the Multilingual Lexicon of Bone Industries [46]. Anatomical tooth terminology based on Bianucci & Landini [47], Toscano [48] and Lambert & Bianucci [49]. Bioerosion traces were observed by using the digital microscope ShuttlePix P-400R (up to 400X) and taking photographs with the PowerShot SX50 HS camera, which made it possible to identify different ichnogenus caused by the action of marine organisms, which respond to different behaviours. Moulds were also made of some of the traces. The whole process was carried out at the Valencina de la Concepcion Museum. Results Description The fusiform morphology of the tooth as well as its large size and massive and robust root allow it to be attributed to the superfamily Physeteroidea. The absence of a rough enamel crown, constriction or occlusion facets or wear by opposing teeth places it within the family Physeteridae and subfamily Physeterinae [50,51] differentiating it from the so-called macroraptorial sperm whales. The tooth was compared with specimens described in the literature and with material from various collections and online 3D models, showing great similarity with teeth belonging to present-day sperm whale Physeter macrocephalus. The tooth is robust, unicuspid, conical, gently curved lingually and distally, with an oval cross-section, more compressed labio-lingually. It would have had a symphyseal mandibular position, probably right (the labial side is usually more curved or convex than the lingual side, resulting in a gentle inward curvature of the mouth). Approximately the upper half of the tooth is preserved, measuring 13.2 cm with a weight of 414 g. Lambert [51] indicate that the largest Physeter tooth measured was 25 cm. This suggests a tooth that would be close to that size in its entirety. In addition, the tooth shows features like wear on the labial side, and a smoothed fracture with loss of material on the lingual side (see Fig 2A–2C) that indicate that it was produced during the animal’s life, either during feeding or by collision with the teeth of a rival (clashes between males), so it belonged to an adult specimen that may have died naturally. The crown is smoother on the surface than the root. The enamel appears to be absent, showing a thin, polished cementum layer that allows the dentine to show towards the apex. The tip shows wear on the labial side, while on the
PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 8 / 21 lingual side there is a fracture with loss of material forming a slight hollow with rounded edges. Its passage to the root is not perceptible. Neither is the banding of the gingival or alveolar margin or any constriction visible. The root of the P. macrocephalus tooth is massive, fusiform, and widens until it reaches a more dilated shape in the middle part, before flattening and compressing in its lower half, which projects distally. In the tooth under study, the lower fracture of the preserved part shows a stable to slightly increasing diameter which places us in the middle part of the tooth. The size of the preserved part and its total estimate would indicate a large adult specimen. The root has a thick layer of cementum, with an outer ornamentation of folds and parallel grooves in a baso-apical orientation that deepen towards the base, and which are related to the anchorage of the tooth to the alveolus. This striation crosses transversely with a certain undulation corresponding to growth layers. The lower part, which is absent in the specimen studied here, has been separated by a net and level fracture in a cross section that shows no signs of environmental wear, preserving well-defined angles. This basal fracture allows the different tooth layers to be observed in section. The tooth grows as a superposition of cones that are added towards the base. In cross-section, this structure of overlapping layers looks as concentric rings that are clearly visible. Although the conical opening of the pulp cavity is not preserved, as the base of the root is not present, a small pulp canal or root canal through which the vessels and nerves of the tooth run is still preserved in its centre. Surrounding it are concentric layers or rings of dentine, which make up the bulk of the tooth material (maximum dentine thickness: 30 mm). Towards the outside, a layer of cement appears (maximum cement thickness: 6 mm), with a mineralisation that is more granular in appearance than the dentine, and which in the specimen is shown subdivided into 2, where the outermost and thinnest layer is detaching from the tooth. These detachment or fragmentation layers usually form at the separation between the different cementum accretion lamellae. The dentine is compact and white in colour, almost like a fresh tooth. It shows alteration on the exterior surface, where traces of sediments and concretions can be found. Alterations produced by microorganisms, as well as loss of raw material and some generalised cracks in the cementum are also visible. However, the tooth is not complete, and an important part of the proximal end is missing. Its maximum diameter (approx. 8 cm) would point to a medium-sized tooth, about 20 cm long. The estimated size, together with the lack of pulp cavity in the preserved part, lead to think that about 60% of the tooth is preserved (Fig 2G) The morphological study of the tooth has allowed us to identify it as belonging to a Sperm whale (Physeteroidea), a superfamily of odontocete (toothed) cetaceans known since the Upper Oligocene (around 25 million years BP) [52–54]. While they diversified enormously during the Middle and Upper Miocene [47,48], they are currently represented by only three species, belonging to two families: the Physeteridae family, with Physeter macrocephalus Linnaeus, 1758, being this the only member of the genus and whose adult males can reach up to 20.5 meters and weigh up to 57 tonnes; and the Kogiidae family, with two smaller species Kogia breviceps Blainville, 1838 (some individuals can reach up to 3,5 m and 400 kg of weight) and Kogia sima Owen, 1866 (the smallest species with a length of 2,7 m and 280 kg of weight). Sperm whales are oceanic animals, frequenting both the depths of the continental slope and coastal waters. They have a global distribution and are frequent in the Atlantic and Mediterranean waters of the Iberian Peninsula. Today, they come to the Strait of Gibraltar to feed on squid, mostly in spring and early summer, and are considered a semi-resident species [55,56]. Although present-day sperm whales, Physeter macrocephalus, have a cosmopolitan distribution, there are few mentions of fossil remains from after the Neogene. According to the Paleobiology Database portal, there are Holocene archaeological records from Spain, Portugal, Morocco and Italy [10,21,57]. Invertebrate bioerosion traces Four types of bioerosion traces were identified that are related to the boring activity of different groups of marine invertebrate organisms, corresponding to the ichnogenus: Entobia Bronn, 1838; Maeandropolydora Voigt, 1965; Radulichnus Voigt, 1977 and Rogerella De Saint-Seine, 1951 (Fig 3). For each ichnogenus, the main parameters of distribution in the
PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 9 / 21 Fig 3. A; location of invertebrate (rectangles) and vertebrate (circles) ichnogenus. Lingual view of the tooth. Bioerosion is not delimited to the marked areas, they represent examples of some of its locations, black a1 Meandropolydora, black a2 Rogerella, red a3 Linichnus, blue a4 Entobia, green a5 Radulichnus. https://doi.org/10.1371/journal.pone.0323773.g003
PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 16 / 21 gold foil from Structure 10.029 of the PP4-Montelirio sector or the three large copper axes of Structure UE-56 at Calle Trabajadores) were sometimes buried in simple pits without human remains, as a form of structured deposition with a high symbolical character. Two attempts to radiocarbon-date the sperm whale tooth failed on account of low collagen. The reasons behind the (apparently high) variability in the amount of collagen in human and animal bones of Copper Age chronology at the Valencina mega-site are basically unknown, although presumably they are connected to spatial variations in taphonomic and pedological conditions. A good example of the limitations imposed by this factor is Structure 10.049, the grave of ‘The Ivory Lady’ [91]. Five dates originally obtained from samples from the various ivory artefacts found in this tomb revealed very low collagen levels and yielded inconsistent ages that were deemed invalid [92]. A further seven samples of human bone and ivory submitted later, produced little or no collagen and failed the Oxford and SUERC (Scottish Universities Environmental Research Centre) quality-control procedures [84]. Finally, three more samples on human bone submitted to SUERC in 2022 also failed because of low collagen. In total, 15 samples from Structure 10.049 have been submitted for radiocarbon dating between 2012 and 2022, all of which failed due to low collagen. In this respect, four samples of approximately 1 g were extracted from the tooth core and sent to SUERC radiocarbon dating facility, and other two to BETA Analytic Laboratory. Unfortunately, all samples failed to provide sufficient quality collagen to proceed with an AMS measurement. Despite the lack of direct radiocarbon dating, the assemblage of materials found in connection with the tooth, including the fragments of almond-rim plates coupled with the most recent of the two dates (MAMS 41417) obtained as part of this study, leaves no doubt as to its usage in the final centuries of the Copper Age. The fact that the tooth is not complete and shows fractures caused by anthropic action might suggest that some of it was used as raw material, in order to manufacture sumptuary objects, such as ornaments, etc. Although, no ivory artefact has yet been diagnosed as coming from a sperm whale tooth, recent finds of ivory of marine origin in European archaeological contexts have brought a new focus to the study of the use of marine resources by prehistoric societies [10–12,16]. Indeed, the discovery of another sperm whale tooth, very similar to the one described in this paper, in Monte d’Accoddi [22] may help to understand the use and symbolism of the Valencina tooth. Both were found with no association to other remains of sperm whale or other marine animals, and both were found in what are clearly special places for their respective contexts: a votive offering (Pit US-123) at Valencina and a massive ritual monument at Monte d’Accoddi. Additionally, both teeth show marks of anthropic manipulation, which would indicate an intention to extract raw material, perhaps to manufacture objects, or to dress them to make them more suited for their intended use. In summary, it seems likely that this piece arrived to Valencina as an exotic product, as did other raw materials of great value (such as flint, ivory, rock crystal, cinnabar, ostrich eggshell and amber), and that it was collected on a marine shore rather than extracted from a hunted whale. Conclusions The sperm whale tooth studied in this paper is the only of its kind ever found in Copper Age Iberia. In fact, the only example of a similar chronology and morphology in Europe was recently found in Sardinia. This tooth, belonging to an adult sperm whale specimen, was likely found in a coastal area after it had spent some time in subaquatic conditions, as attested by the bioerosion traces left by marine organisms. Once the tooth was exposed on the surface, it was covered again by sediment and a second wearing process started, this time due to the action of roots and the creation of a cemented crust covering the tooth. After its collection, it was manipulated, perhaps with the aim of using some parts of it as a raw material to manufacture other objects (such as personal ornaments) or to transform it into a symbolically-charged artefact. Finally, the tooth was deposited in a pit. The discovery of this piece underlines the presence of the sea in the worldview of the communities that lived or frequented Valencina in the 3rd millennium BC. This is further suggested by the careful selection of rocks naturally ‘decorated’ with sedimentary structures of currents, bioerosion and marine organic remains, to manufacture some of the capstones
PLOS One | https://doi.org/10.1371/journal.pone.0323773 May 14, 2025 17 / 21 and floor slabs used at major megalithic monuments such as La Pastora or Matarrubilla [93,94] in the use of numerous valves of Pecten maximus as offerings in several of the burials and votive pits that were made around ‘The Ivory Lady’ burial, in the PP4-Montelirio sector [95] or in the use of tens of thousands of discoidal beads to manufacture the attires worn by the individuals buried in the Montelirio tholos [96]. Acknowledgments We would like to thank Juan Carlos Castro Jiménez for his kind restoration work on the tooth. We would also like to thank the Museum and Council of Valencina de la Concepción and the Research Group RNM-293 of the University of Huelva. We would like to thank as well Manolo Toscano, Teodosio Donaire and Cristóbal for their help doing the tests that were carried out in the electron microscopy lab of the University of Huelva. Author contributions Conceptualization: Samuel Ramírez-Cruzado Aguilar-Galindo, Fernando Muñiz Guinea, Luis Miguel Cáceres Puro. Investigation: Samuel Ramírez-Cruzado Aguilar-Galindo, Fernando Muñiz Guinea, Luis Miguel Cáceres Puro, Antonio Toscano Grande, Marta Díaz-Guardamino, Juan Manuel Vargas Jiménez. Methodology: Samuel Ramírez-Cruzado Aguilar-Galindo, Miriam Luciañez-Triviño, Fernando Muñiz Guinea, Luis Miguel Cáceres Puro, Marta Díaz-Guardamino, Leonardo García Sanjuán. Resources: Juan Manuel Vargas Jiménez, Rafael María Martínez Sánchez. Supervision: Fernando Muñiz Guinea, Luis Miguel Cáceres Puro, Leonardo García Sanjuán. Validation: Miriam Luciañez-Triviño, Fernando Muñiz Guinea, Luis Miguel Cáceres Puro, Marta Díaz-Guardamino, Leonardo García Sanjuán. Writing – original draft: Samuel Ramírez-Cruzado Aguilar-Galindo, Miriam Luciañez-Triviño. Writing – review & editing: Fernando Muñiz Guinea, Luis Miguel Cáceres Puro, Antonio Toscano Grande, Marta DíazGuardamino, Juan Manuel Vargas Jiménez, Thomas Xavier Schuhmacher, Rafael María Martínez Sánchez, Santiago Guillamón Dávila, Joaquín Rodríguez Vidal, Leonardo García Sanjuán. References 1. Müller K, Reiche I. Differentiation of archaeological ivory and bone materials by micro-PIXE/PIGE with emphasis on two Upper Palaeolithic key sites: Abri Pataud and Isturitz, France. J Archaeol Sci. 2011;38:3234–43. 2. Pitulko VV, Pavlova EY, Nikolskiy PA, Ivanova VV. The oldest art of the Eurasian Arctic: personal ornaments and symbolic objects from Yana RHS, Arctic Siberia. Antiquity. 2012;86:642–59. 3. Schwab C, Vercoutere C. Les statuettes en ivoire gravettiennes d’europe occidentale. L’Anthropologie. 2018;122:469–91. 4. Wolf S, Heckel C. Ivory ornaments of the Aurignacian in western Europe: case studies from France and Germany. L’Anthropol. 2018;122:348–73. 5. Laznickova-Galetova M. Gravettian ivory ornaments in central europe, moravia (czech republic). L’Anthropol. 2021;125. 6. Luciañez-Triviño M, García Sanjuán L, Schuhmacher T. Crafting idiosyncrasies. Early social complexity, ivory and identity-making in Copper Age Iberia. CAJ. 2021;32(1):23–60. https://doi.org/10.1017/s0959774321000287 7. Corchón-Rodríguez MS, Álvarez Fernández E. Nuevas evidencias de restos de mamíferos marinos en el magdaleniense: los datos de la cueva de las caldas (Asturias, España). Munibe. 2008;59:47–66. 8. Langley MC, Street M. Long range inland-coastal networks during the Late Magdalenian: evidence for individual acquisition of marine resources at Andernach-Martinsberg, German Central Rhineland. J Hum Evol. 2013;64(5):457–65. https://doi.org/10.1016/j.jhevol.2013.01.015 PMID: 23490262 9. Álvarez-Fernández E. Marine resource exploitation during the Middle and early Upper Paleolithic in Europe: overview of the available evidence. In: White R, Bourrillon R, editors. Aurignacian genius: art, technology and society of the first modern humans in Europe. Proceedings of the International Symposium, New York University, Vol. 7. Palethnology; 2015. p. 188–205. 10. Schuhmacher T, Banerjee A, Dindorf W, Sastri C, Sauvage T. The use of sperm whale ivory in chalcolithic Portugal. Trabajos de Prehistoria. 2013;70:185–203. https://doi.org/10.3989/tp.2013.12109
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