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Scientific Reports Volume 11, Article Number: 22730 (2021) Cite this article

Ammonoids are extinct shelled cephalopods and dominate in many Late Paleozoic and Mesozoic marine ecosystems. The stable isotope data from the ammonite shell constitutes the main tool for understanding its paleohabitat. However, in most of the world's sedimentary sequences, the aragonite shells of ammonites dissolve during the fossilization process, so they cannot be used for geochemical research. We overcome this burial bias by analyzing the better-preserved calcite element in the ammonite jaw (aptychi). We studied mold and aptychi from two consecutive members of a navicular evolutionary lineage from the Late Cretaceous Cretaceous in Poland, which we interpreted as temporal subspecies. In order to reconstruct their habitat depth preference, we analyzed the powerful combination of stable isotope data from aptychi and symbiotic benthic and planktonic foraminifera with predation markers preserved on scaphoid specimens. On this basis, we conclude that the populations of the older subspecies lead the benthic life, while the populations of the younger subspecies lead the benthic life. The change in habitat depth preference may be the response of the local population to the shallower sea. Previous studies have largely assumed a stable depth preference for chrysanthemum species, genera and even higher clades. Our research questioned this generalization by pointing out that ammonites may be more flexible than expected in their depth-related behavior.

Ammonoids belong to the most diverse, richest and best-studied clade in the history of life1,2,3. These extinct cephalopods with outer cavity shells dominate many marine ecosystems in the Late Paleozoic and Mesozoic. They follow the pelagic life pattern 4, inhabiting bodies of water close to the seabed as benthic organisms, or as plankton or plankton at higher places. Ammonoid depth preferences can be reconstructed based on a variety of methods, including the comparative morphology of conch shells, the mechanical properties of shell materials, and phase inference4,5,6,7,8. The use of stable isotope thermometry of aragonite ammonite shells has yielded particularly promising results for deep inferences9,10,11,12. However, this method excludes from the study those specimens derived from carbonates, in which the stone shells of these specimens were dissolved during the fossilization process, leaving only natural molds (steinkerns). This is the case with the Cretaceous facies, which dominated the Cretaceous Sea in northern Europe during the 13th, 14th, and 15th of the Late Cretaceous.

However, the absence of primitive shells does not mean that the chalk ammonia-like biota in Europe16,17 is completely out of reach in terms of isotopic paleotemperature measurement. The chalk locally produces aptychi, the calcite covering of the lower ammonite jaws18,19. According to Kruta et al.20, aptychi is secreted in equilibrium with the surrounding seawater and is therefore a potential archive of isotope data of paleontological significance.

Following the groundbreaking study by Kruta et al. 20, we used aptychi's stable isotope thermometry to reconstruct the habitat depth preference of the Compositae Scaphitidae from the Chalk Sea in northern Europe. Our target is Hoploscaphites constrictus (Figure 1), a species commonly found in Maastricht in Europe 21,22. More specifically, we studied two consecutive members of Hoploscaphites constrictus evolutionary lineage 21 (we interpret them as two temporal subspecies or temporal subspecies), based on the late Maastricht overland exposed in Chełm Three-spaced specimens and samples from the Light Cretaceous, Poland 23,24. In order to reconstruct the preferred position of these inulins in the water body, we compared the temperature calculated based on the oxygen isotope composition of aptychi with the temperature of symbiotic foraminifera with known bathymetric preferences; we also studied the carbon isotope for more clues11 .

Researched the scaphitid ammonoid. (a) Side view of Hoploscaphites constrictus lvivensis (positive model of subspecies, ZPAL Am. 12/1051). (b) A pair of internal mold preservation aptychi in H. c. mold (there is a discernible growth increase on the back of the original aptychi). Livingcis, ZPAL Am. 12/796 (see Machalski, 202122 for explanation of this specimen and aptychi terminology). (c) Single aptychus, ZPAL Am. 24/104, ventral view. (d, e). Speculative life recovery of animals in side view (d) and front view (e). Specimen from Chełm (ac).

As an independent test of paleotemperature inference, we studied the predator markers preserved on the scaphoid mold of Chełm25. The quantitative ratio between the various types of such markers in the fossil assemblage provides insights into the depth preference of ammonite prey26,27.

Habitat depth preference is an important issue in the discussion of ammonite paleontology4,5,8,10,28. Our results provide a new way of thinking about this problem by recording the depth preference changes that occur between closely related members (continuous timed subspecies) of a single lineage of these cephalopods.

Detailed data on the geological environment is provided in Supplementary Information (SI). In short, our specimens and samples come from a 40-meter thick layer of chalk 23 exposed in the quarry of the Chelm Cement Plant in Poland (Figure 2; SI-Figure 1, 2). Due to the particularity of chalk excavation in the mine (see SI), our sampling of large fossils, including scaphitid mold and aptychi, is limited to three chalk layers, AC, each 2 m thick (Figure 2, SI-Figure 1)) .

The chalk part of Chełm, quarry grade VI-II, sampling interval AC, and stratigraphic changes in the δ18O and δ13C values ​​of benthic and planktonic foraminifera and large rock samples. The red bars are the average δ13C and δ18O values ​​of Hoploscaphites constrictus aptychi, which are separated from A-CH and heterospiral; GL., Globigerinelloides; G., Gyroidinoides; C., Cibiciidoides.

During the Late Cretaceous, the Chełm site today was located in the eastern part of the Cretaceous Sea in northern Europe (Surlyk et al. 13; Thibault et al. 14; Wilmsen and Niebuhr 15). Cheheim chalk deposits in an onshore (upper platform) environment, and the classical areas of chalk deposits in Denmark and northern Germany are separated by an area dominated by spinel limestone deposits (the so-called opokas) (for example, Leszczyński 29; Jurkowska and Świerczewska-Gładysz 30). The current coordinates of the Chełm area are 51.1303° N, 23.5303° E. According to Gplates Web Service31, the paleo position 69 meters before the site is 47.77°N and 22.16°E. During Maastricht, the region witnessed a gradual cooling trend with lower and lower temperature fluctuations14.

Chełm Chalk is assigned to the lower Maastricht Belemnitella Junior and Belemnitella Junior-Spyridoceramus tegulatus areas of the standard European northern subdivision 21,23,32. Based on the correlation with the Danish Stevns-1 reference core (SI-Figure 2; Surlyk et al. 33; Thibault et al. 14), we approximate the time intervals A, B, and C to 69.0, 68.7, and 68.3 Ma, respectively. Chełm chalk matches the characteristics of "benthic barren chalk" in the Boreal Chalk Sea facies model. The planktonic foraminifera assemblage indicates that the sea level dropped during the chalk deposition to a depth of c. The interval A is 100 m, and the interval C is tens of meters (see Dubicka and Peryt 23, 24, and SI). REE data (SI) confirms the lightening upward trend of the Chełm series. The benthic foraminifer assemblage 23 and large and trace fossils (SI) prove the bottom aerobic conditions and normal water salinity during chalk deposition. We also failed to find pyrite twigs in the sediments, which may indicate temporal hypoxia during chalk deposition (see SI, compare Tagliavento et al. 34).

The materials studied have been identified and evaluated based on several lines of evidence for their applicability to this research (see SI and SI-Figure 3-11); the following is a brief summary.

Box and whisker plots of the δ18O data of Hoploscaphites constrictus target foraminifera and aptychi from Chełm interval AC, grouped by taxa. Each box represents the average value and must extend between the maximum and minimum δ18O values. H., Heterospiral; GL., Globigerinelloides; G., Gyroidinoides.

The scaphitids studied represent the late Maastricht part of the Hoploscaphites constrictus evolutionary lineage (SI-Figure 3). In terms of subdividing the pedigree into temporal subspecies based on materials from several regions in Europe (SI-Figure 3-4; Machalski21), the B from Interval A and Chełm was assigned to H. c. lvivensis, and those From C to H. c. Aff. crassus, the intermediate of shell decoration to H. c. crassus (SI-Figure 5-7). The latter subspecies was interpreted by Machalski21 as a direct descendant of H. c. Livingcis; The existence of transitional forms in Chełm provides additional arguments for this explanation.

Combination of stable isotope and paleotemperature data from Hoploscaphites constrictus and foraminifera aptychi, as well as predation marker data stored on H. constrictus mold, interval AC, Chełm profile. (a) Box plot of the temperature gradient traversed by the scaphoid under study (based on δ18O data from aptychi). Each box represents the average value and must extend between the highest and lowest temperature values. The gray shaded area represents the bottom water gradient estimated based on the δ18O data from the benthic foraminifer G. globosus. (b) Based on the average paleotemperature from the δ18O data, the position of the studied taxa in the shallow waters of the Maastricht Sea. (c) The incidence of predation marks on H. constrictus (see SI-Figure 8). H., Helix; GL., Globigerinelloides; G., Gyroidinoides; C., Cibiciidoides; H. c., Hoploscaphites constrictus.

An example of the ontogeny δ18O variation of Hoploscaphites constrictus (from left to right: ZPAL Am. 24/95 in the A zone, 39 in the B zone, 91 in the C zone), taken from their concave surface and anatomical back, showing the growth increment ( Compare Machalski, 202122); white circles indicate sampling points.

For reasons of burial geology, post-mortem transportation of scaphoid remains from remote habitats was excluded. Specifically, the in situ characteristics of the studied combination are still maintained by the appearance of aptychi in the scaphitid body cavity (SI-Figure 7), the ubiquity of double-petal aptychi (SI-Figure 6), and the carbonized residues of the original chitin mandible. Attached to aptychi (SI-Figure 6).

The inference of the habitat depth preference of Hoploscaphites constrictus changes as the seawater at the Chełm site becomes shallower. See the text for further explanation.

The original preservation of aptychi (SI-Figure 9-10) and foraminifer 35 recorded on the basis of microstructure and geochemistry makes them suitable for paleontology-oriented geochemical analysis. First, there are clear increments and growth lines (SI-Figure 9) and the original layered microstructure, with different flakes, without any signs of diagenetic secondary facies (SI-Figure 9), indicating that aptychi has no diagenetic changes) . This means that the studied aptychi has a high preservation index of 5 (excellent preservation) 20. Second, most of the aptychi that we examined with cathodoluminescence (CL) microscopes did not emit light (SI-Figure 10), indicating that there were no diagenetic changes. Third, the results of electron microprobe analysis (EMPA) showed that the content of trace elements Mn, Sr, and Ba was below the detection limit of the microprobe (SI Table 2), which is the characteristic of unchanged diagenetic samples. Fourth, the stable isotope distribution of aptychi individuals from the AC interval usually reveals the oscillation values ​​of δ18O and δ13C (SI-Figure 15-16), which may be interpreted as reflecting the original seasonal biological cycle; diagenesis tends to cause these signals Homogenization.

Among the foraminifera selected for analysis (SI-Figure 11), there are two benthic species, Gyroidinoides globosus and Cibicidoides voltzianus, and two planktonic species, the surface-dwelling Heterohelix striata and the deeper-dwelling Globigerinelloides praihillensis. Among them, G. globosus, H. striata and G. prairiehillensis precipitate oxygen, and the carbon isotopes of C. voltzianus and G. prairiehillensis are close to equilibrium with environmental water35. Therefore, these foraminifera are expected to provide reliable data for reconstructing the depth-related temperature profile of the water column, and the water column can be located by isotopic data from aptychi.

Our isotope analysis is based on samples of large rocks and foraminifera from the entire section, as well as aptychi from large and continuous samples from the AC interval. We use isolated, loose aptychi found in chalk for these analyses. The oxygen (δ18O) and carbon (δ13C) isotope analysis of calcite and the calculated paleotemperature of the entire section are shown in Fig. 2, and the interval AC in Fig. 2 is shown. 3, 4a, b, and 5, as well as the SI-graph. 12-16 (see SI Table 3-13 for rough data).

In order to determine the significant difference in the δ18O and δ13C isotopic values ​​between the intervals AC, we performed the non-parametric Kruskal-Wallis test (for each foraminifer species and a large number of sampled aptychi, respectively). Only the δ18O isotope characteristics of aptychi are significantly different (Kruskal-Wallis test, Hc = 14.73, p = 0.0006), while the oxygen characteristics in the C interval specimens are heavier (Mann-Whitney pairwise comparison). The change in the δ13​​C value indicates that the difference between aptychi and C. voltzianus is negligible (Kruskal-Wallis test, Hc = 4.989, p = 0.0827; Hc = 6.433, p = 0.0404). The δ13C of the interval A of the former is slightly lighter. Those who have a heavier δ13C in interval C. We also tested the oxygen isotope changes in the interval AC (Figure 5; SI-Figure 15-16) through ontogeny through ontogeny, and found no significant difference between these intervals.

Two types of fatal injuries caused by hard-eating predators can be discerned on the mold of Hoploscaphites constrictus from Chełm (SI-Figure 8; see also Machalski and Malchyk 25). Ventral injury manifests as a half crescent or V-shaped notch in the ventral part of the shell, mainly near the bottom of the body cavity. Lateral injuries are represented by sub-circular to irregular holes on the side of the body cavity. The frequency of these two types of predation marks fluctuates between sampling intervals, and the abundance of lateral traces in interval C increases significantly (Figure 4c). The ratio of lateral to ventral trajectories in the sampling interval is equal to 1.16 in interval A, 1.39 in interval B, and rises to 8.25 in C (SI Table 1). In the sampling interval (Kruskal-Wallis test, Hc = 1.143, p = 0.56), there is no clear relationship between the type of predation marker and its frequency on the ammonite shell.

The entire Chewum section (see the section on geological environment and SI above) completely appeared narrow-salt-type micro- and macrofauna, which allowed us to exclude salinity changes as a factor controlling the results of stable oxygen isotopes; therefore, we based on ancient Temperature explains these results.

The positions of Heterohelix striata, Globigerinelloides prairiehillensis and Gyroidinoides globosus in the water body reconstructed based on oxygen-derived temperature (Figure 4a, b) are consistent with the inferred habitat depth of these foraminifera 24,35 According to surface striatum and benthic G The temperature difference between globosus, the temperature at the surface and bottom of the water column is estimated to be 4–5 °C. In all the intervals studied, the paleotemperature calculated from aptychi positions Hoploscaphites constrictus between the deep-dwelling plankton G. prairiehillensis and the benthic G. globosus, which is very close to the latter in the interval C (Figure 4a, b) ). Statistical tests show that the scaphitid aptychi in C changes significantly to higher oxygen levels, which indicates that the habitat has become colder and deeper waters, closer to the bottom than A and B. No significant changes in the thermal gradient between samples in interval A- C are recorded. Starting from interval C, no obvious dissolved inorganic carbon shifts to heavier δ13C value, which is related to the shallower seawater (δ13CDIC value tends to increase the water column upward and toward the coast 11).

It is important to note that the isotope results of a large number of samples of aptychi are average values, reflecting the net sum of movement of a specific individual in the entire water body during the sampling period. Therefore, these results indicate the most common (preferred) position of these animals in the water column. The lack of significant directional trends in the δ18O (and δ13C) isotope values ​​of continuously sampled aptychi indicates that the depth of their owner's habitat has not changed significantly since the late childhood (due to the destruction of the early stage, there is no record of the early stage). Analyze the top part of the specimen, Figures 1c and 5 and SI-Figures 6 and 9).

In summary, the paleotemperatures obtained from aptychi (Figures 3 and 4a, b) indicate that H. c. lvivensis from intervals A and B shares the same ecological area with the deep-water planktonic foraminifer G. prairiehillensis, while H. c. Aff. Crassus from interval C is very close to benthic G. globosus in its habitat. On this basis, it can be inferred that H. c.'s main lifestyle is nektic. lvivensis and a benthic organism (bottom layer) used in H. c. Afu. Crassou (Figure 6). This habitat transition must occur at some time between the deposition of interval B and C, that is, between 68.7 and 68.3 Ma. These inferences can be verified by predation-labeled data. Following Klompmaker et al.36, we interpreted the ventral injury as caused by predatory fish or colloidal cephalopods. These animals can live with benthic or benthic animals, so their tracks are ambiguous for sounding. After Fraaye37, Machalski and Malchyk25 interpreted the lateral markings as traces left by predatory swimming crabs. Here, we prefer another explanation-lateral damage is caused by the predation of mouth-pods, which use their raptor appendages to smash ammonite shells26 (see discussion in SI). These crustaceans are entirely benthic animals26,38. Therefore, their trace abundance on H. c. is mainly increased. Afu. Crassula from interval C (Figure 4c, SI Table 1) confirmed the subspecies' bottom life pattern inferred from isotope thermometry (Figure 6).

Nautilus is the only analogue of the recently extinct exovolute cephalopod, and its depth preference varies from population to population and is controlled by a variety of factors, including feeding preference, temperature, and buoyancy regulation requirements39. Nautilus is an active scavenger that moves hundreds of meters up and down along the slope of the reef. Its maximum depth range (over 700 m) is related to the strength of the shell that prevents it from implosion under water pressure40. In contrast, boattail fish are considered to be slow, mainly bottom swimmers or occasional passive floats, feed on zooplankton, and are confined to shallow seas due to their thin shells41, 42. More specifically, Tsujita and Westermann 43 calculated the maximum habitat depths of Campania and Maastricht scaphitids from Canada based on the strength of the diaphragm, indicating that most of these species cannot venture below 100 m depth . For their Hoploscaphites sp. α, which is most similar to H. constrictus in shape and size, and these authors estimate that the maximum habitat depth is c. 70 meters. By analogy, we have proposed roughly similar depth limits for the European boats. According to our estimates, the depth of Chełm’s basin ranges from 100 meters in A layer to tens of meters in C (see SI discussion). Therefore, we suggest that during the deposition of the chalk layers A and B (69.0 and 68.7 Ma), the seafloor should be located near the maximum habitat depth of Hoploscaphites constrictus (Figure 6). Most individuals spend most of their time high above the water column, living in the zooplankton "cloud" and feeding on the zooplankton "cloud"44. The predation of H. c. by orropods proves that some individuals occasionally descend to the bottom. lvivensis comes from the A and B layers. The situation was different during the deposition of the shallowest chalk layer C (68.3 Ma). At this time, H. constrictus aff. The Krasu population follows the bottom life style and conducts large-scale exploration of the seabed. It is speculated that they mainly feed on bottom zooplankton here, that is, mobile benthic organisms, which regularly move up into the water column45. At the same time, scaphocerans are more often prey of benthic mouth-pods that are active on the seafloor (Figure 6).

Inferred lifestyle changes and another member of the evolutionary lineage H. c. Af. Crassou. Therefore, it is easy to explain this shift from the perspective of evolutionary processes. However, our preferred hypothesis is that it reflects an opportunistic and reversible response of the local population to the new demands of the local environment. According to Walter's law of phases, we expect that each of our samples AC will have its counterpart in different areas of sounding in other parts of the chalk basin. We assume that the scaphitid populations from these regions and their Chełm equivalents lead different lifestyles. However, based on the data at hand, it is impossible to test this hypothesis. The Chełm part is the only part in Europe that allows full sampling of this part of the evolutionary lineage of H. constrictus. Outside the Chełm quarry, H. c. lvivensis was only found in the surrounding area of ​​Lviv in western Ukraine21. However, the outcrops that produced these materials do not exist today, and there are only inadequately localized mold specimens and some aptychi in the museum collection, which is not suitable for research like the present.​​​​​

Stable isotope data from ammonite shells constitute the main tool for understanding its paleohabitat (for example, Moryia10). However, in most of the world's sedimentary sequences, the aragonite shells of ammonites dissolve during the fossilization process, so they cannot be used for geochemical research. Following Kruta et al.20, we overcome this burial bias by analyzing the more easily preserved calcite elements in the jaws (aptychi) of the Late Cretaceous navicular animal Hoploscaphites constrictus from the white chalk sequence deposited in the Cretaceous Sea in northern Europe. .

To study the depth preference of H. constrictus, we applied a unique and powerful combination of stable isotope data from aptychi and symbiotic foraminifera, as well as the established depth preference, and analyzed the predation markers preserved on the scaphoid specimens . On this basis, we inferred the change in habitat depth preference between two consecutive time subspecies of the Hoploscaphites constrictus lineage. This change may have occurred in response to the shallower seawater recorded in the succession studied (Figure 6).

Our results have important implications for understanding pyrethroid paleontology. As pointed out by Moryia28, basic knowledge about the depth of the habitat of Chrysanthemums is essential for understanding their paleoecology and mechanisms of evolution and extinction. Many previous studies have either explicitly or implicitly assumed that the habitat depth preference of certain Compositae species, genera and even higher clades (for example, Westermann5 and Moriya28) is stable, although the latter author mentioned the reversal of depth preference in a pedigree Single case, Perisphinctoidea. As far as scaphoids are concerned, these cephalopods are generally considered to be bottom animals8,41. Our research questions this generalization, suggesting that ammonites may be more flexible than previously expected in terms of their depth-related behavior. Encourage future research, preferably based on closely spaced and well-constrained samples, to explore this important issue in more detail.

A total of 187 Hoploscaphites molds, 130 aptychi and 34 large rock samples were collected and analyzed, as well as many other large fossils from Chełm. The material was collected by sampling the entire section, working level II-VI as the reference layer, and collected from detailed samples of three chalk layers AC, each 2 m thick (Figure 2). Due to the way the chalk is excavated here, only these intervals can collect large enough fossil samples for this study. The large-scale fossil material is located at the Institute of Paleontology of the Polish Academy of Sciences (PAS) in Warsaw (abbreviated as ZPAL Am. 12 and 24). The microfossil samples are stored in the Geological Institute of the University of Warsaw. The ammonia-like sample from Chełm described by Machalski21 was also studied for comparison.

Use standard mechanical methods to prepare samples in the field and in the laboratory: hammers, chisels, needles, and vibration tools (Paleotools, ME-9100).

For the carbon and oxygen isotope analysis of the foraminifera test, 34 bulk samples weighing approximately 0.2 kg were processed. The sample is mechanically decomposed in tap water, cleaned in an ultrasonic bath and washed through a 125 micron screen. Repeat this process until the foraminifera test is completely free of fillers. From each sample residue, hand-selected adult, large-sized foraminifera specimens were placed in a microcentrifuge tube. Each taxa (selected according to specific ecological preferences and very weak life effects, see the chapter on foraminifer selection in the supplementary information) was selected to obtain a single material of foraminifera weighing more than 2 µg.

A total of 43 samples were selected for the analysis of the bulk carbon and oxygen isotope of Sclerotium (15 in the A interval, 16 in the B interval, and 12 in the C interval, all isolated samples). These samples were crushed and homogenized in an agate mortar. In addition, 10 aptychi were continuously sampled to detect individual genetic variation in their stable isotope content (2 samples from A, 6 from B, and 2 from C; a total of 87 measurements). The carbonate samples were taken from the spots on the aptychi surface along the growth axis. In addition, the chalk matrix directly adjacent to the continuously sampled aptychi was analyzed based on 8 samples.

The slices of aptychi were prepared and examined at the Institute of Paleontology PAS. These slices are perpendicular to the surface of aptychus and roughly along the growth axis of aptychus. The petrographic observation was done using a Nikon Eclipse 80i transmitted light microscope equipped with a DS-5Mc cooling camera. Use image analysis software (NIS Elements D software, https://www.microscope.healthcare.nikon.com/products/software/nis-elements) to measure from digital micrographs (Nikon DSIFi2). The observation is carried out under transmitted light, so that the microstructure of each fossil and the presence of diagenetic minerals can be quickly assessed. The selected flakes were carbon-coated and analyzed using a cathodoluminescence (CL) microscope. The CL analysis was performed in the NanoFun laboratory (Institute of Paleontology, PAS), using an HC1-LM hot cathode microscope with the following parameters: electron energy 14 keV, beam density 0.1 μAmm-2. For aptychi's SEM study, selected polished slices (a by-product of cutting slices) were etched in 8% formic acid for 8-15 minutes, rinsed with Milli-Q water, and then air-dried. Next, the sample was placed on a short post with double-sided tape and sputter coated with a conductive carbon film. The analysis was performed at the PAS Paleontology Institute using a Philips XL20 scanning electron microscope. SEM imaging provides high-resolution support for transmitted light observations; for example, scanning electron microscopy studies make it possible to obtain more detailed information about the preservation of aptychi's microstructure. The instrument operates at an acceleration voltage of 25 kV, a beam current of 98-103 nA, and a spot diameter of 3.5 µm.

The content of major, minor and trace elements in aptychi was checked on an uncovered sheet previously recorded with transmitted light, and Cameca SX-100 electronic was used in the Mineral and Synthetic Material Analysis Center of the Joint Research Institute (College of Geology, University) The microprobe was carried out in Warsaw, Poland). A total of 43 measurements were taken on four aptychi. The mineral composition is measured on EMPA in Wavelength Dispersive Spectroscopy (WDS) mode, using 15 keV acceleration potential, 20 nA beam current, 1 µm beam current, 20-30 seconds peak and background count time and standard ZAF ( PAP) Amendment procedures. Use a combination of natural and synthetic standards for calibration. The peak count time of the major element is 10 seconds, and the peak count time of the minor element is 20 seconds. During these durations, the average detection limit for Mg is 423 ppm; silicon is 190 ppm; Ca is 232 ppm; aluminum is 155 ppm; 495 ppm strontium; Ba is 517 ppm; P is 229 ppm; S is 189 ppm; Fe 625 ppm; Mn is 593 ppm.

The stable isotope composition of the studied carbonates (large rocks, foraminifera and aptychi samples) were analyzed at the Warsaw Isotope Laboratory for Dating and Environmental Studies of the Polish Academy of Sciences. Using the Kiel IV online carbonate preparation device connected to the ThermoFinnigan Delta Plus mass spectrometer, the sample was dissolved in 100% phosphoric acid at 70 °C. The quality of the analysis is controlled by the NBS-19 international standard measurement. The values ​​of δ13​​C and δ18O are given relative to the V-PDB standard. The repeatability of the results based on NBS-19 verifies the reproducibility of the analysis. The observed deviation of δ13C <0.03‰ and the deviation of δ18O measurement <0.07‰. Statistical analysis is performed using Past-free software for scientific data analysis, including univariate and multivariate statistics46.

The calcite temperature is calculated using the Anderson and Arthur47 equations modified by Coplen et al. 48, assuming that the δ18O value of non-glacial seawater is −1‰, based on the ancient location and climate of the Chevrem site in the studied time interval (compare Thibault et al. 14, Page 436):

To search for pyrite twigs, approximately 15 grams of chalk samples from each of the three sampling intervals in Chełm (AC) were studied. These samples were coarsely ground and then put into a hydrochloric acid solution with a pH of 5.0 to dissolve the carbonate portion. The insoluble residue is neutralized by washing with demineralized water and ethanol. The samples were dried at room temperature for 2 days and then coarsely ground again. The powder is placed on a short rod, sputter coated with platinum and inspected in a Philips XL-20 SEM (IP PAS).

The rare earth element (REE) content of three chalk samples from the AC interval of the Chełm sequence and a comparative sample of the upper Maastricht spire-column limestone from the Wola Piasecka quarry in southeast Lublin was studied. The samples were powdered and analyzed at Bureau Veritas Acme Labs Canada Ltd. The content of major, minor and rare elements is analyzed by inductively coupled plasma mass spectrometry (ICP-MS). The precision and accuracy of the results are better than ±0.05% for major elements (mostly ±0.01%), and usually better than ±1ppm for trace elements. The REE concentration is standardized to the Postarchean Australian Shale (PAAS)49 as indicated by the subscript "N". Due to the presence of positive La anomalies and highly variable negative Ce anomalies in shallow seawater, the enrichment of HREE is calculated as YbN/NdN. Calculate CeN anomaly based on the relationship proposed by Webb and Kamber50:

All graphics in this article, including those in the supplementary materials, use CorelDraw 18 (https://www.corel.com/pl/?link=wm) and Adobe Photoshop CS3 (https://www.adobe .com/ de/creativecloud/desktop-app.html?mv=affiliate&mv2=red).

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This work was funded by the Polish National Science Center and awarded 2015/19/B/ST10/02033 to MM. Cathodoluminescence imaging was an innovation co-funded by Europe at the NanoFun Laboratory (Cathodeluminescence Laboratory, Institute of Paleontology, PAS, Warsaw) Regional Development Fund POIG.02.02.00-00-025/09 in the Economic Operation Plan. We thank M. Andziak for on-site assistance, C. Kulicki for SEM assistance, G. Dziewińska and M. Dziewiński for photography work, A. Hołda-Michalska for digital computer processing (all from the Paleontology Institute PAS), B. Waksmundzki ( University of Warsaw) for drawing inulin specimens, B. Gebus-Czupyt (Polish Academy of Sciences Dating and Environmental Research Warsaw Isotope Laboratory) for isotope analysis, JWM Jagt (Maastricht Museum of Natural History, Netherlands) provided language assistance, N. Thibault (University of Copenhagen, Denmark) provided samples from the Stevns 1 core, and M. Yacobucci (Bowling Green State University, USA) helped estimate the ancient coordinates of the Chełm site. Thanks to the staff of Cemex Polska for their help in various ways.

Institute of Paleontology, Polish Academy of Sciences, Twarda 51/55, 00-818, Warsaw, Poland

Marcin Machalski, Krzysztof Owocki and Oksana Malchyk

Faculty of Geology, University of Warsaw, Ayr. Żwirki i Wigury 93, 02-089, Warsaw, Poland

Zofia Dubicka & Weronika Wierny

Polish Institute of Geology-National Institute, Rakowiecka 4, 00-975, Warsaw, Poland

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MM, KO and ZD design research. MM and OM collected large-scale fossil materials and were responsible for field observation. KO is responsible for processing geochemical and other analytical data, as well as conducting statistical tests. ZD and WW are responsible for foraminifera data. OM participated in the analysis of predator markers. MM is responsible for all ammonoid-related data and writes the main text and Supplementary Information text. In cooperation with ZD and KO, all authors discussed the results and reviewed the manuscript.

The author declares no competing interests.

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Machalski, M., Owocki, K., Dubicka, Z. etc. Stable isotopes and predation markers provide new clues for the depth preference of pyrethroid habitats. Scientific Report 11, 22730 (2021). https://doi.org/10.1038/s41598-021-02236-9

DOI: https://doi.org/10.1038/s41598-021-02236-9

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