gsa data repository 2018006 - geological society of americaµm, respectively. a common-pb correction...

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GSA Data Repository 2018006 New U/Pb Dates Reveal a Paleogene Origin of the Modern SE Asia Biodiversity 'Hotspot' Linnemann, U. 1,* , Su, T. 2, , Kunzmann, L. 1 , Spicer, R.A. 3,4 , Ding, W.-N 2,5 , Spicer, T.E.V. 4 , Zieger, J. 1 , Hofmann, M. 1 , Moraweck, K. 1 , Gärtner, A. 1 , Gerdes, A. 6 , Marko, L. 6 , Zhang, S.- T. 7 , Li, S.-F. 2 , Tang, H. 2,4 , Huang, J. 2,4 , Mulch, A. 6,8 , Mosbrugger, V. 9 , Zhou, Z.-K. 2 Methods (U-Th-Pb isotopes, Hf isotopes, geochemistry, plant fossils) Zircon concentrates were separated from 1 kg samples at the Senckenberg Naturhistorische Sammlungen Dresden (Museum für Mineralogie und Geologie) by crushing (jaw crusher), sieving, heavy mineral separation by heavy liquid (LST), and by making use of a magnetic separator. Final selection of the zircon grains for U-Pb dating was achieved by hand-picking under a binocular microscope. Zircon grains of all grain sizes and morphological types were selected, mounted in resin blocks and polished to half their thickness. Concerning stratigraphic ages, the stratigraphic time scale of Ogg et al. (2016) has been used. Zircons were analyzed for U, Th, and Pb isotopes by LA-SF ICP-MS techniques at the Museum für Mineralogie und Geologie (GeoPlasma Lab, Senckenberg Naturhistorische Sammlungen Dresden), using a Thermo-Scientific Element 2 XR sector field ICP-MS coupled to a New Wave UP-193 Excimer Laser System. A teardrop-shaped, low volume laser cell was used to enable sequential sampling of heterogeneous grains (e.g., growth zones) during time resolved data acquisition. Each analysis consisted of approximately 15 s background acquisition followed by 30 s data acquisition, using a laser spot-size of 25 and 35

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Page 1: GSA Data Repository 2018006 - Geological Society of Americaµm, respectively. A common-Pb correction based on the interference- and background-corrected 204Pb signal and a model Pb

GSA Data Repository 2018006 New U/Pb Dates Reveal a Paleogene Origin of the Modern SE Asia Biodiversity

'Hotspot'

Linnemann, U.1,*, Su, T.2,, Kunzmann, L.1, Spicer, R.A.3,4, Ding, W.-N2,5, Spicer, T.E.V. 4,

Zieger, J.1, Hofmann, M.1, Moraweck, K. 1, Gärtner, A.1, Gerdes, A.6, Marko, L.6, Zhang, S.-

T.7, Li, S.-F.2, Tang, H.2,4, Huang, J.2,4, Mulch, A.6,8, Mosbrugger, V.9, Zhou, Z.-K.2

Methods (U-Th-Pb isotopes, Hf isotopes, geochemistry, plant fossils)

Zircon concentrates were separated from 1 kg samples at the Senckenberg

Naturhistorische Sammlungen Dresden (Museum für Mineralogie und Geologie) by crushing

(jaw crusher), sieving, heavy mineral separation by heavy liquid (LST), and by making use of

a magnetic separator. Final selection of the zircon grains for U-Pb dating was achieved by

hand-picking under a binocular microscope. Zircon grains of all grain sizes and

morphological types were selected, mounted in resin blocks and polished to half their

thickness. Concerning stratigraphic ages, the stratigraphic time scale of Ogg et al. (2016) has

been used.

Zircons were analyzed for U, Th, and Pb isotopes by LA-SF ICP-MS techniques at the

Museum für Mineralogie und Geologie (GeoPlasma Lab, Senckenberg Naturhistorische

Sammlungen Dresden), using a Thermo-Scientific Element 2 XR sector field ICP-MS

coupled to a New Wave UP-193 Excimer Laser System. A teardrop-shaped, low volume laser

cell was used to enable sequential sampling of heterogeneous grains (e.g., growth zones)

during time resolved data acquisition. Each analysis consisted of approximately 15 s

background acquisition followed by 30 s data acquisition, using a laser spot-size of 25 and 35

Page 2: GSA Data Repository 2018006 - Geological Society of Americaµm, respectively. A common-Pb correction based on the interference- and background-corrected 204Pb signal and a model Pb

µm, respectively. A common-Pb correction based on the interference- and background-

corrected 204Pb signal and a model Pb composition (Stacey and Kramers, 1975) was carried

out if necessary. The necessity of the correction was judged on whether the corrected

207Pb/206Pb lies outside of the internal error of the measured ratios. Discordant analyses were

interpreted with care. Raw data were corrected for background signal, common Pb, laser

induced elemental fractionation, instrumental mass discrimination, and time-dependant

elemental fractionation of Pb/Th and Pb/U using an Excel® spreadsheet program developed

by Axel Gerdes (Institute of Geosciences, Johann Wolfgang Goethe-University Frankfurt,

Frankfurt am Main, Germany). Reported uncertainties were propagated by quadratic addition

of the external reproducibility obtained from the standard zircon GJ-1 (~0.6% and 0.5-1% for

the 207Pb/206Pb and 206Pb/238U, respectively) during individual analytical sessions and the

within-run precision of each analysis. According to the recommendation of Horstwood et al.

(2016) a secondary zircon standard (Plesovice zircon) was analysed. Sequences started with

the analysis of five GJ1, one Plesovice and 10 unknowns followed by a repetition of a

succession of three measurements of the GJ1 standard, one measurement of the Plesovice

standard and 10 unknowns. U-Pb ages were in the recommended range of Slama et al. (2008).

Concordia diagrams (2 error ellipses) and Concordia ages (95% confidence level) were

produced using Isoplot/Ex 2.49 (Ludwig 2001). The 207Pb/206Pb age was taken for

interpretation for all zircons >1.0 Ga, and the 206Pb/238U ages for younger grains. For further

details on analytical protocol and data processing see Gerdes and Zeh (2006). Th/U ratios are

obtained from the LA-ICP-MS measurements of investigated zircon grains. U and Pb content

and Th/U ratio were calculated relative to the GJ-1 zircon standard and are accurate to

approximately 10%. Analytical results of U-Th-Pb isotopes and calculated U-Pb ages are

given in Table DR 1.

SEM and cathodoluminescence images (CL) were obtained using an EVO 50 scanning

electron microscope (Zeiss) at Senckenberg Naturhistorische Sammlungen Dresden.

Page 3: GSA Data Repository 2018006 - Geological Society of Americaµm, respectively. A common-Pb correction based on the interference- and background-corrected 204Pb signal and a model Pb

Hafnium isotope measurements were performed with a Thermo-Finnigan NEPTUNE

multi collector ICP-MS at Goethe Universität Frankfurt coupled to a RESOlution M50 193nm

ArF Excimer (Resonetics) laser system following Gerdes and Zeh (Gerdes and Zeh, 2006).

Spots of 40 µm in diameter were drilled with a repetition rate of 5.5 Hz and an energy density

of 6 J/cm2 during 50s of data acquisition. The instrumental mass bias for Hf isotopes was

corrected using an exponential law and a 179Hf/177Hf value of 0.7325. In case of Yb isotopes

the mass bias was corrected using the Hf mass bias of the individual integration step

multiplied by a daily βHf/βYb offset factor (Gerdes and Zeh, 2009). All data were adjusted

relative to the JMC475 of 176Hf/177Hf ratio = 0.282160 and quoted uncertainties are quadratic

additions of the within-run precision of each analysis and the reproducibility of the JMC475

(2SD = 0.0028%, n = 8). The accuracy and external reproducibility of the method was

verified by repeated analyses of reference zircon GJ-1 and Plesovice (Table DR 2). Results

are in excellent agreement with previously published results (Gerdes and Zeh, 2006; Sláma et

al., 2008) and with the LA-MC-ICPMS long-term average of GJ-1 (0.282010 ±0.000025; n >

800) and Plesovice (0.282483 ±0.000025, n > 300) reference zircon.

The initial 176Hf/177Hf values are expressed as εHf(t), which is calculated using a

decay constant value of 1.867×10−11 year−1, CHUR (Bouvier et al., 2008)

(176Hf/177HfCHUR,today = 0.282785 and 176Lu/177Hf CHUR,today = 0.0336) and U-Pb ages obtained

for the respective domains (Supplementary Table 1). For the calculation of Hf two stage

model ages (TDM) in 106 years the measured 176Lu/177Lu of each spot (first stage = age of

zircon), a value of 0.0113 for the average continental crust, and a juvenile crust 176Lu/177LuNC

= 0.0384 and 176Hf/177Hf NC = 0.283165 (average MORB (Chauvel et al., 2008)) were used.

Hf isotpe data ages are given in Table DR 2.

Geochemical data (major and trace elements, REE) were analyzed the ACTLABS

(Canada) using ICP and ICP-MS (for details see www.actlabs.com, option 4Litho,

lithogeochemistry). Results are given in Table DR 3.

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Plant fossils were collected during several field trips from 2014 to 2016. Plant fossils

occur both above and below the ash layers in lacustrine, primarily organic-rich clays and silts

and among them one layer, 14 m above the dated horizons and within the near-surface

oxidized zone of the section, contains the most abundant plant fossils (Fig. 3, Table 1, Fig.

DR 2). Specimens in forms of seeds, fruits and leaves from this one metre thick layer were

collected for this study (n=1667). Fossils were identified at the genus level by comparison

with specimens of living species from the Herbarium of the Kunming Institute of Botany,

Kunming (KUN) and online databases. All specimens are deposited in the laboratory of the

Palaeoecology Research Group, Xishuangbanna Tropical Botanical Garden, CAS.

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Figure DR 1. Sedimentary log of the Lühe section showing the positions of the ash beds and

fossil assemblages.

Page 6: GSA Data Repository 2018006 - Geological Society of Americaµm, respectively. A common-Pb correction based on the interference- and background-corrected 204Pb signal and a model Pb

Figure DR 2. Illustrations of plant fossils from the Lühe section. a) Tsuga sp. (LH3-0251); b)

Calocedrus sp. (LH3-0270); c) Metasequoia sp. (LH3-0004); d) Carpinus sp.(LH1-0097); e)

Alnus sp. (LH1-0557); f) Mahonia sp. (LH2-0017); g) Picea sp. (LH4-0015); h) Quercus sp.

(LH1-0243); i) Ilex sp. (LH2-0060); j) Machilus sp. (LH1-0588); k) Populus sp. (LH3-540); l)

Palaeocarya sp. (LH1-0493); m) Fraxinus sp. (LH1-0578); n) Acer sp. (LH3-0217); o)

Dipteronia sp. (LH1-0425); p) Ailanthus sp. (LH1-0237). Scale bars = 1 cm.

Page 7: GSA Data Repository 2018006 - Geological Society of Americaµm, respectively. A common-Pb correction based on the interference- and background-corrected 204Pb signal and a model Pb

Figure DR 3. Images of thin sections of ash bed sample LS1: (a): Image done with reflected

light. Note the dominance of feldspar clasts (white) mixed with magnetite fragments (black).

(b): Image done under transmitted light and crossed Nicols. Note the graded bedding of the

laminae in the ash bed and the angular shape of mineral and lithic fragments. (c): Hornblende

xenocryst under transmitted light and crossed Nicols.

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Figure DR 4. Examplary images of zircon grains of ash bed sample LS1 analysed for U-Pb

isotopes by LA SF ICP MS. (a): REM 3D images (back scatter) of five grains. (b): CL

(cathodoluminescence) images of the same grains and location of laserspots including the

238U-206Pb age.

Page 9: GSA Data Repository 2018006 - Geological Society of Americaµm, respectively. A common-Pb correction based on the interference- and background-corrected 204Pb signal and a model Pb

Figure DR 5. Images of (sub)rounded zircons from LS2.

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Figure DR 6. Concordia diagrams showing the concordia ages of magmatic zircon crystals

from ash bed LS1 (a) (33 ± 1 Ma), LS2 (b) (32 ± 1 Ma), and LS 3 (c) (32 ± 1 Ma).

Page 11: GSA Data Repository 2018006 - Geological Society of Americaµm, respectively. A common-Pb correction based on the interference- and background-corrected 204Pb signal and a model Pb

Figure DR 7. Concordia diagrams showing the concordia age of magmatic zircon crystals

from ash bed LS2 (a) (32 ± 1 Ma) and ages of older detrital zircon grains in ash bed sample

LS2 (b).

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Figure DR 8. Hf isotope evolution diagram of zircon from the studied magmatic zircon grains

of ash beds LS1, LS2, and LS3 (n=13). Data point to the recycling of a Mesoproterozoic crust

(c. 1.3 to 1.45 Ga) during magma generation. For details and references of depleted mantle

evolution see (Dhuime et al., 2011; Gerdes and Zeh, 2006). Data were calculated using the

decay constant of 1.867 x 10-11 (Scherer et al., 2001) and the CHUR parameters (Bouvier et

al., 2008).

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Figure DR 9. Geochemical data of samples LS1-3 in different discrimination plots. Top:

SiO2-Na2O+K2O (TAS) diagram (Cox et al., 1979) (TAS=Alkalis-Silica). Bottom: Log

(Nb/Y)-Log (Zr/TiO2) diagram (Winchester and Floyd, 1977).

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Figure DR 10. Geochemical data of samples LS1-3 in different discrimination plots. Top:

A/CNK-A/NK diagram (Maniar and Piccoli, 1989) [A/NK = molar Al2O3/(Na2O+K2O)

versus A/CNK = molar Al2O3/(CaO + Na2O+K2O)]. Bottom: AFM diagram (Irvine and

Baragar, 1971; Kuno, 1968) (AFM: A-Alkalis, F-Iron, M-Magnesium).

Page 15: GSA Data Repository 2018006 - Geological Society of Americaµm, respectively. A common-Pb correction based on the interference- and background-corrected 204Pb signal and a model Pb

Figure DR 11. Geochemical data of samples LS1-3 in different discrimination plots. Top:

SiO2-Na2O+K2O diagram (Peacock, 1931). Bottom: Log Y - Log Nb diagram (Pearce et al.,

1984) (WPG-within-plate granite, VAG + syn COLG-volcanic arc and syn-collision granites,

ORG - oceanic ridge granite).

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Figure DR 12. Geochemical data of samples LS1-3 in different discrimination plots. Top:

Rare Earth Elements normalized against the C1 condrite (normalizing factors from

(McDonough and Sun, 1995). Bottom: Spider diagram showing a plot of different trace and

Rare Earth Elements against the C1 condrite (normalizing factors from (McDonough and Sun,

1995).

Page 17: GSA Data Repository 2018006 - Geological Society of Americaµm, respectively. A common-Pb correction based on the interference- and background-corrected 204Pb signal and a model Pb

Supplementary Table DR1: LA-SF-ICP-MS U-Pb-Th data of magmatic zircon from tuff samples LS1, LS2, and LS3, Luhe site, Yunnan, China, Xiaolongtan Formation, Lühe Basin, coordinates: 25.141627 °N, 101.373840 °E, 1890 m amsl. Recommended ages in the range of concordance of 90-110%

207Pba Ub Pbb Thb 206Pbc 206Pbc 2 207Pbc

2 207Pbc 2 rhod 206Pb 2 207Pb 2

Number (cps) (ppm) (ppm) U 204Pb 238U % 235U % 206Pb % 238U (Ma) 235U (Ma) conc %

LS 1 a1 283 1016 6 1.16 598 0.00517 3.5 0.03411 14.1 0.04784 13.7 0.25 33 1 34 5 36 a2 186 785 5 1.03 397 0.00547 2.4 0.03582 13.4 0.04753 13.2 0.18 35 1 36 5 46 a3 163 701 5 1.43 358 0.00514 4.8 0.03309 18.2 0.04668 17.6 0.27 33 2 33 6 101 a4 210 906 6 1.24 451 0.00530 1.9 0.03414 14.0 0.04675 13.8 0.14 34 1 34 5 94 a5 145 508 4 1.39 312 0.00521 3.1 0.03383 8.0 0.04714 7.4 0.38 33 1 34 3 60 a6 181 784 5 1.00 393 0.00520 2.9 0.03349 12.6 0.04674 12.3 0.23 33 1 33 4 94 a7 204 859 5 1.15 443 0.00516 3.2 0.03322 11.5 0.04667 11.1 0.27 33 1 33 4 103 a8 190 868 5 1.09 410 0.00535 3.7 0.03459 16.4 0.04685 16.0 0.23 34 1 35 6 82 a9 250 1068 7 1.20 543 0.00510 3.6 0.03286 11.2 0.04673 10.6 0.32 33 1 33 4 93 a10 255 1111 7 1.11 554 0.00517 2.4 0.03323 14.4 0.04663 14.2 0.17 33 1 33 5 109

LS 2 a1 282 1054 8 2.61 593 0.00521 5.1 0.03387 12.5 0.04719 11.4 0.41 33 2 34 4 57 a2 51 199 1 1.54 105 0.00511 10.3 0.03399 25.3 0.04824 23.1 0.41 33 3 34 8 30 a3 770 148 13 0.61 712 0.08293 2.6 0.84149 4.8 0.07359 4.1 0.54 514 13 620 23 50 a4 79 331 2 1.82 154 0.00513 5.3 0.03697 25.4 0.05224 24.8 0.21 33 2 37 9 11 a5 193 476 4 2.09 235 0.00514 4.3 0.05304 37.0 0.07485 36.8 0.11 33 1 52 19 3 a7 204 1026 7 1.85 442 0.00507 3.6 0.03315 14.6 0.04737 14.2 0.25 33 1 33 5 48 a9 2439 500 41 0.86 757 0.07331 2.4 0.70762 5.0 0.07000 4.3 0.48 456 11 543 21 49 a10 2075 343 31 0.03 3459 0.09714 2.2 0.80745 5.0 0.06028 4.5 0.44 598 13 601 23 97 a11 63200 1720 218 1.69 25 0.02441 38.9 2.57576 38.9 0.76518 1.0 1.00 155 60 1294 334 3 a12 5791 2203 77 0.36 426 0.03138 2.1 0.46273 9.5 0.10694 9.3 0.22 199 4 386 31 11 a13 1393 476 30 1.18 1493 0.05174 2.8 0.37883 7.0 0.05311 6.5 0.40 325 9 326 20 98 a14 384 1568 9 1.07 817 0.00495 2.5 0.03185 11.5 0.04670 11.2 0.22 32 1 32 4 94

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a15 889 3778 23 1.58 1912 0.00510 2.4 0.03285 5.3 0.04674 4.7 0.45 33 1 33 2 91 a16 349 1166 7 1.38 593 0.00492 7.3 0.04018 10.3 0.05919 7.3 0.71 32 2 40 4 6 a17 443 177 12 2.77 821 0.04337 3.8 0.32458 9.1 0.05428 8.2 0.42 274 10 285 23 72 a18 355 163 12 2.83 602 0.04631 3.3 0.33301 21.7 0.05215 21.4 0.15 292 9 292 57 100 a19 2047 588 48 1.17 3682 0.06968 2.5 0.53612 5.4 0.05580 4.7 0.47 434 11 436 19 98 a20 2081 342 32 0.03 3427 0.09965 2.2 0.83924 4.5 0.06108 3.9 0.50 612 13 619 21 95 a21 549 390 11 0.48 1115 0.02848 3.0 0.19655 9.4 0.05005 8.9 0.32 181 5 182 16 92 a22 151 765 5 1.16 310 0.00519 4.2 0.03494 9.2 0.04884 8.1 0.46 33 1 35 3 24 a23 157 691 4 1.23 338 0.00514 5.4 0.03308 11.0 0.04667 9.6 0.49 33 2 33 4 103 a24 215 1122 8 2.43 460 0.00496 4.3 0.03233 12.5 0.04723 11.7 0.34 32 1 32 4 53 a25 271 832 8 4.25 583 0.00499 5.4 0.03221 12.5 0.04683 11.2 0.43 32 2 32 4 79

LS 3 a1 389 913 6 1.71 824 0.00487 2.6 0.03216 5.8 0.04786 5.2 0.45 31 1 32 2 34 a2 519 1207 7 1.46 1126 0.00496 3.2 0.03193 8.6 0.04672 8.0 0.37 32 1 32 3 91 a3 534 1274 8 1.73 1167 0.00501 3.0 0.03238 13.8 0.04687 13.5 0.22 32 1 32 4 76 a4 546 1301 8 1.34 1189 0.00520 2.7 0.03352 6.7 0.04674 6.1 0.41 33 1 33 2 93 a5 826 1392 9 1.42 714 0.00550 2.6 0.04908 14.0 0.06470 13.8 0.18 35 1 49 7 5 a6 521 1291 8 1.53 1138 0.00493 2.7 0.03169 7.8 0.04662 7.3 0.35 32 1 32 2 107 a7 216 551 3 1.22 468 0.00509 3.2 0.03279 13.2 0.04675 12.8 0.24 33 1 33 4 90 a8 440 1104 7 1.11 960 0.00517 2.3 0.03327 6.7 0.04664 6.3 0.34 33 1 33 2 109 a9 408 994 6 1.16 839 0.00520 2.2 0.03348 9.6 0.04667 9.4 0.23 33 1 33 3 104 a10 345 823 5 1.00 749 0.00515 2.8 0.03309 8.9 0.04664 8.4 0.32 33 1 33 3 108

a within-run background-corrected mean 207Pb signal in counts per second b U and Pb content and Th/U ratio were calculated relative to GJ-1 and are accurate to approximately 10%. c corrected for background, mass bias, laser induced U-Pb fractionation and common Pb (if detectable, see analytical method) using Stacey & Kramers (1975) model Pb composition. 207Pb/235U calculated using 207Pb/206Pb/(238U/206Pb × 1/137.88). Errors are propagated by quadratic addition of within-run errors (2SE) and the reproducibility of GJ-1 (2SD). d Rho is the error correlation defined as err206Pb/238U/err207Pb/235

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Supplementary Table DR2: LA-MC-ICP-MS Lu-Hf data of detrital zircon from samples LS1, LS2, and LS3, n = 13, tuff layers, Luhe site, Yunnan, China, Xiaolongtan Formation, Lühe Basin, coordinates: 25.141627 °N, 101.373840 °E, 1890 m amsl.

176Yb/177Hf a ±2 176Lu/177Hf a ±2 178Hf/177Hf 180Hf/177Hf SigHf b 176Hf/177Hf ±2c 176Hf/177Hf(t)

d Hf(t) d ±2c TDM e age f ±2

(V) (Ga) (Ma)

LS1 – a6 0.0189 18 0.00066 5 1.46720 1.88495 4 0.282470 39 0.282470 -10.4 1.4 1.34 33 1 LS1 – a7 0.0185 17 0.00067 5 1.46717 1.88609 5 0.282435 47 0.282434 -11.7 1.6 1.41 33 1 LS1 – a8 0.0180 15 0.00066 4 1.46714 1.88654 6 0.282435 30 0.282434 -11.7 1.1 1.41 33 1 LS1 – a9 0.0227 26 0.00075 7 1.46722 1.88604 5 0.282482 33 0.282482 -10.0 1.2 1.32 33 1 LS1 – a10 0.0392 52 0.00123 14 1.46715 1.88596 6 0.282477 30 0.282476 -10.2 1.0 1.33 33 1 LS2 – a14 0.0250 20 0.00085 5 1.46718 1.88634 7 0.282484 28 0.282483 -10.0 1.0 1.32 32 1 LS2 – a15 0.0757 64 0.00231 15 1.46721 1.88567 5 0.282414 36 0.282413 -12.4 1.3 1.45 33 1 LS2 – a23 0.0610 78 0.00194 23 1.46740 1.87635 3 0.282403 123 0.282402 -12.8 4.3 1.47 33 1 LS3 – a6 0.0194 17 0.00070 5 1.46718 1.88571 6 0.282475 27 0.282475 -10.3 0.9 1.33 32 1 LS3 – a7 0.0193 20 0.00066 6 1.46724 1.88583 7 0.282481 24 0.282481 -10.0 0.8 1.32 33 1 LS3 – a8 0.0165 14 0.00059 4 1.46722 1.88629 7 0.282468 27 0.282467 -10.5 1.0 1.35 33 1 LS3 – a9 0.0287 27 0.00096 7 1.46716 1.88579 7 0.282467 20 0.282466 -10.6 0.7 1.35 33 1 LS3 – a10 0.0135 12 0.00049 3 1.46723 1.88621 7 0.282470 27 0.282470 -10.4 1.0 1.34 33 1

GJ1, n=4 0.0075 6. 0.00028 2 1.46724 1.88648 12 0.282026 19 0.282022 -13.5 0.7 1.98 606 6

Quoted uncertainties (absolute) relate to the last quoted figure. The effect of the inter-element fractionation on the Lu/Hf was estimated to be about 6 % or less based on analyses of the GJ-1 zircon. Accuracy and reproducibilty was checked by repeated analyses (n = 4) of reference zircon GJ-1). (a) 176Yb/177Hf = (176Yb/173Yb)true x (173Yb/177Hf)meas x (M173(Yb)/M177(Hf))

(Hf), (Hf) = ln(179Hf/177Hf true / 179Hf/177Hfmeasured )/ ln (M179(Hf)/M177(Hf) ), M=mass of respective

isotope. The 176Lu/177Hf were calculated in a similar way by using the 175Lu/177Hf and (Yb). (b) Mean Hf signal in volt. (c) Uncertainties are quadratic additions of the within-run precision and the daily reproducibility of the 40ppb-JMC475 solution. Uncertainties for the JMC475 quoted at 2SD (2 standard deviation). (d) Initial 176Hf/177Hf and Hf calculated using the apparent Pb-Pb age determined by LA-ICP-MS dating (see column f), and the CHUR parameters: 176Lu/177Hf = 0.0336, and 176Hf/177Hf = 0.282785 (Bouvier et al., 2008). (e) Two stage model age in billion years using the measured 176Lu/177Hf of each spot (first stage = age of zircon), a value of 0.0113 for the average continental crust (second stage), and the depleted mantle (DM) 176Lu/177Hf and 176Hf/177Hf of 0.0384 and 0.283165, respectively (Chauvel et al., 2008) (f) U-Pb and Pb-Pb ages determined by LA-SF-ICP-MS. If the zircon age is younger than 1Ga, the 206Pb-238U age is preferred. The 207Pb-206Pb is used in the case the zircon age is older than 1 Ga.

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Supplementary Table DR3: Major and trace elements including REE of volcanic ash samples LS1, LS2, and LS3, Lühe Basin, Yunnan, China, coordinates: 25.141627 °N, 101.373840 °E, 1890 m amsl. Major Elements (%) (anhydrous) LS1 LS2 LS3 SiO2 63.59 63.26 62.05 Al2O3 18.46 20.48 20.04 Fe2O3tot 2.97 2.08 6.20 FeOtot 2.67 1.87 5.97 MnO 0.009 0.009 0.012 MgO 0.66 1.0 1.17 CaO 1.86 1.22 1.04 Na2O 3.77 2.57 2.32 K2O 5.43 4.53 4.32 TiO2 0.64 0.89 0.81 P2O5 2.61 3.02 2.04 Trace Elements (ppm) Cr 150 120 110 Ni 70 70 30 Zn 50 150 70 Rb 136 137 117 Sr 6741 6450 5079 Y 45 46 44 Nb 16 22 15 Cs 2 6 7 Ba 10040 9236 6416 Ta 1 1 1 Pb 57 97 24 Th 42 49 40 U 8 10 6 Rare Earth Elements (ppm) La 226 246 453 Ce 478 513 981 Pr 51 54 91 Nd 196 195 318 Sm 29 30 44 Eu 7.5 7.1 10.1 Gd 21 21 29 Tb 2.3 2.5 3.1 Dy 11 12 13 Ho 1.6 1.8 1.8 Er 3.8 4.4 4.2 Tm 0.44 0.53 0.48 Yb 2.2 2.9 2.6 Lu 0.26 0.35 0.33

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