Ci a ion: Es eban, J.J.; Cue as, J.;
Tubía, J.M. Pe i-Gondwanan
P o enance and Geodynamic
E olu ion o The Guadaiza Nappe
(Alpuja ide Complex, Be ic
Co dille as, Spain): Insigh s on The
Paleo e hyan Paleogeog aphy.
Mine als 2022,12, 325. h ps://
doi.o g/10.3390/min12030325
Academic Edi o s: Vic o ia B.
E sho a, A em V. Moisee , And ey
Khudoley and Manuel F ancisco
Pe ei a
Recei ed: 20 Janua y 2022
Accep ed: 3 Ma ch 2022
Published: 5 Ma ch 2022
Publishe ’s No e: MDPI s ays neu al
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published maps and ins i u ional a il-
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Copy igh : © 2022 by he au ho s.
Licensee MDPI, Basel, Swi ze land.
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mine als
A icle
Pe i-Gondwanan P o enance and Geodynamic E olu ion o The
Guadaiza Nappe (Alpuja ide Complex, Be ic Co dille as, Spain):
Insigh s on The Paleo e hyan Paleogeog aphy
JoséJulián Es eban *, Julia Cue as and JoséMa ía Tubía
Depa men o Geology, Facul y o Science and Technology, Uni e si y o he Basque Coun y (UPV/EHU),
Ap o. 644, 48080 Bilbao, Spain; [email p o ec ed] (J.C.); [email p o ec ed] (J.M.T.)
*Co espondence: [email p o ec ed]; Tel.: +34-946-01-24-53
Abs ac :
Based on he LA-ICP-MS U-Pb zi con ages o ou me amo phic samples, we discuss
he geoch onology and p o enance o he Guadaiza nappe, an alloch honous uni ha unde lies
he Ronda pe ido i es (Be ic Co dille as, Spain). The Guadaiza nappe is composed o T iassic
ma bles o e lying a me apeli ic sequence wi h schis s and migma i es. Zi cons om a qua zi e
in e laye ed wi h he ma bles yield a maximum deposi ional age o ca. 289 Ma ha suppo s
he T iassic age. The idiomo phic mo phology o hese Paleozoic zi con c ys als and he lack o
la e-Va iscan me amo phism (ca. 300 Ma) suppo s a p oximal sou ce a ea, and sugges s ha he
ma bles we e disco dan ly deposi ed o e he me apeli ic sequence, along he no he n ma gin o he
Albo an mic opla e. The zi con pa e ns om he me apeli ic sequence mainly yield Paleop o e ozoic
(ca. 1.6–2.5 Ga), Tonian–S enian (ca. 1000 Ma), Ediaca an–C yogenian (ca. 600 Ma) and Paleozoic
(ca. 500 Ma) age clus e s. These esul s sugges p o enance om a eas wi hin he iangle bound by
he Wes A ican C a on, he Me asaha an C a on and he Hun Supe e ane du ing he Paleo e hys
opening (Silu ian–De onian). A Silu ian–Ca boni e ous deposi ion age o he schis p o oli hs is
cons ained by he younges de i al zi con popula ion (ca. 443 Ma) and he Va iscan age o hei
migma iza ion by an addi ional peak o a ound 299 Ma in he migma i es.
Keywo ds: pe i-Gondwana; Be ic Co dille as; Guadaiza nappe; de i al zi con; LA-ICP-MS
1. In oduc ion
In he las decade, he echnological imp o emen o he geoch onological echniques
(LA-ICP-MS, SHRIMP, SIMS, among o he s) and he acili ies o acqui e indi idual zi con
da a om sedimen a y and me amo phic ocks, as he U-Pb age de e mina ion can supply
he maximum deposi ional age o he ec ono he mal e en s, means hey ha e become he
pe ec geological ool o deciphe he paleogeog aphic and geodynamic e olu ion o an-
cien e anes. Some o hese e anes, such as he Be ic Co dille as, Kabylian, Pelo i anian
and Calab ian bel s sca e ed a ound he Albo an Sea (wes e n Medi e anean), o m he
so-called Albo an mic opla e [
1
], AlKaPeCa mic opla e [
2
], Mesomedi e anean e ain [
3
]
o Albo an Domain [
4
] ha d i ed away om no he n Gondwana du ing he Paleo e hys
ape u e (Silu ian–De onian). Howe e , al hough i has been concluded ha i con o ms
o a pe i-Gondwanan e ane, e.g., [
5
–
10
], he sca ci y o geoch onological de i al zi con
age da a, he a iable imp in o he Alpine ec onics ha e ased he es iges o p e ious
o ogenic e en s, and, in o he cases, he ac ha he me amo phic ocks ha o m he base-
men ha e been da ed as undi e en ia ed Paleozoic, makes i s paleogeog aphic loca ion
s ill con o e sial. On his ma e , some au ho s ha e sugges ed ha du ing Camb ian
and O do ician imes he Albo an mic opla e should be loca ed in a cen al posi ion o he
Gala ian Supe e ane ( o me ly e e ed o as he Hun Supe e ane, [
5
,
11
,
12
]), lying in
be ween he Aqui aine and he in a-Alpine e anes [
11
,
13
]. Ins ead, o he au ho s ha e
Mine als 2022,12, 325. h ps://doi.o g/10.3390/min12030325 h ps://www.mdpi.com/jou nal/mine als
Mine als 2022,12, 325 2 o 16
sugges ed a wes e nmos s a ing localiza ion o he Albo an mic opla e, in di ec ela-
ionship wi h he Ossa-Mo ena (SW Ibe ian Massi ) and Mo occan Mese a e anes [
14
,
15
].
The e o e, he acquisi ion o new geoch onological da a will help in p o iding a be e
unde s anding o he ec onic e olu ion o he Alpine o ogenic segmen s ha su ound he
Albo an Sea.
In his wo k, we p esen new U-Pb LA-ICP-MS de i al zi con da a om ou me amo -
phic samples o he Guadaiza nappe (wes e n In e nal Zone o he Be ic Co dille as, Spain),
in o de o discuss hei geoch onology and p o enance. The p esence o wo di e en
migma iza ion e en s makes he Guadaiza nappe s and ou [
16
,
17
] as an in e es ing a ge
o sea ch o he in e ela ionship be ween old and new o ogenic e en s. Mo eo e , he
loca ion o he Guadaiza nappe in he In e nal Zones unde he ul ama ic ocks o he Be ic
and Ri o ogens adds addi ional in e es o he explana ion o he ob ained esul s in he
oldes o ogenies (Va iscan, Caledonian, e c.) o he wes e n Medi e anean.
2. Geological Se ing
The Guadaiza nappe, one o he nappes ha o ms he wes e n pa o he Alpuja ide
Complex (In e nal Zones o he Be ic Co dille a), c ops ou in wo main a eas (Figu e 1):
he Albo noque sec o and he Guadaiza ec onic window, su ounded by he la ges
wo ldwide exposu e o subcon inen al li hosphe ic man le, he Ronda pe ido i es. O he
mino ou c ops o Guadaiza nappe a e ound in he no he n pa o he s udied egion, as
small ec onic windows o along he h us con ac be ween he Ronda pe ido i es and he
T iassic limes ones (locally ma bles) o he Sie a de Las Nie es. The pe ido i es also es
o e some o he con inen al c us al sequences composed mainly o gneisses, me apeli es
and ma bles belonging o he Ojen nappe and Yunque a Uni .
Mine als 2022, 12, x 2 o 16
o he au ho s ha e sugges ed a wes e nmos s a ing localiza ion o he Albo an mic o-
pla e, in di ec ela ionship wi h he Ossa-Mo ena (SW Ibe ian Massi ) and Mo occan Me-
se a e anes [14,15]. The e o e, he acquisi ion o new geoch onological da a will help in
p o iding a be e unde s anding o he ec onic e olu ion o he Alpine o ogenic seg-
men s ha su ound he Albo an Sea.
In his wo k, we p esen new U-Pb LA-ICP-MS de i al zi con da a om ou me a-
mo phic samples o he Guadaiza nappe (wes e n In e nal Zone o he Be ic Co dille as,
Spain), in o de o discuss hei geoch onology and p o enance. The p esence o wo di -
e en migma iza ion e en s makes he Guadaiza nappe s and ou [16,17] as an in e es ing
a ge o sea ch o he in e ela ionship be ween old and new o ogenic e en s. Mo eo e ,
he loca ion o he Guadaiza nappe in he In e nal Zones unde he ul ama ic ocks o he
Be ic and Ri o ogens adds addi ional in e es o he explana ion o he ob ained esul s in
he oldes o ogenies (Va iscan, Caledonian, e c.) o he wes e n Medi e anean.
2. Geological Se ing
The Guadaiza nappe, one o he nappes ha o ms he wes e n pa o he Alpuja ide
Complex (In e nal Zones o he Be ic Co dille a), c ops ou in wo main a eas (Figu e 1):
he Albo noque sec o and he Guadaiza ec onic window, su ounded by he la ges
wo ldwide exposu e o subcon inen al li hosphe ic man le, he Ronda pe ido i es. O he
mino ou c ops o Guadaiza nappe a e ound in he no he n pa o he s udied egion,
as small ec onic windows o along he h us con ac be ween he Ronda pe ido i es and
he T iassic limes ones (locally ma bles) o he Sie a de Las Nie es. The pe ido i es also
es o e some o he con inen al c us al sequences composed mainly o gneisses, me ape-
li es and ma bles belonging o he Ojen nappe and Yunque a Uni .
Figu e 1. Geological map o he Guadaiza nappe (modi ied om Es eban e al. [16]) and analysed
sample loca ions (s a s).
The li hological sequence o he Guadaiza nappe (Figu e 1) is cha ac e ized by an
undi e en ia ed Paleozoic me apeli ic sequence wi h in e laye ed qua zi es, schis s and
mino amphiboli es [17]. This sequence is mainly cha ac e ized by abundan olded eins
o qua z (Figu e 2a) and a well-de eloped axial plane schis osi y, S2. The me amo phic
Figu e 1.
Geological map o he Guadaiza nappe (modi ied om Es eban e al. [
16
]) and analysed
sample loca ions (s a s).
The li hological sequence o he Guadaiza nappe (Figu e 1) is cha ac e ized by an
undi e en ia ed Paleozoic me apeli ic sequence wi h in e laye ed qua zi es, schis s and
mino amphiboli es [
17
]. This sequence is mainly cha ac e ized by abundan olded eins
o qua z (Figu e 2a) and a well-de eloped axial plane schis osi y, S
2
. The me amo phic
Mine als 2022,12, 325 3 o 16
condi ions o he me apeli ic sequence ange om he andalusi e zone a uppe le els o
he sillimani e zone close o he unde laying Is an migma i es [17]. This membe includes
gneisses, dia exi es, me a exi es and medium o ine-g ained leucog ani es. O e he
me apeli ic sequence, coa se-g ained laye ed ma bles comple e he li hological sequence
o he Guadaiza nappe. The T iassic age is commonly assigned o hese ma bles, based
on s a ig aphic co ela ions wi h he less me amo phic Alpuja ide uni s o he eas e n
In e nal Zone o he Be ic Co dille a [18,19].
Mine als 2022, 12, x 3 o 16
condi ions o he me apeli ic sequence ange om he andalusi e zone a uppe le els o
he sillimani e zone close o he unde laying Is an migma i es [17]. This membe includes
gneisses, dia exi es, me a exi es and medium o ine-g ained leucog ani es. O e he me -
apeli ic sequence, coa se-g ained laye ed ma bles comple e he li hological sequence o
he Guadaiza nappe. The T iassic age is commonly assigned o hese ma bles, based on
s a ig aphic co ela ions wi h he less me amo phic Alpuja ide uni s o he eas e n In-
e nal Zone o he Be ic Co dille a [18,19].
Figu e 2. Field images o s udied sample ou c ops: (A) schis s and qua zi es o he me apeli ic se-
quence ( b-2009-7), (B) Is an migma i es ( b-07-845), (C) in e laye ed qua zi e wi hin coa se-g ained
ma bles ( b-18-06) and (D) Hoyo del Bo e myloni ic migma i e (Gu-35-2) wi h elonga ed whi e
qua z nodules and me apeli ic es i es (da k g ey) ha de ine he myloni ic olia ion (SMyl).
The Guadaiza nappe shows wo main ana ec ic e en s ecognized om ec onic a -
gumen s [17]. The oldes one is eco ded by he Is an migma i es (Figu e 2b) and is ela ed
o he p e-alpine egional me amo phism o he me apeli ic sequence. Pe o med geo-
ch onological s udies wi h he 207Pb/206Pb sequen ial e apo a ion echnique [20] and U/Pb
SHRIMP da ing o me amo phic zi cons [21] yield Va iscan and la e-Va iscan ages o 319
± 8 Ma and 299 ± 4 Ma, espec i ely. The younges e en is ep esen ed by he migma i es
concen a ed a ound a dynamo he mal au eole associa ed wi h he emplacemen o he
o e lying Ronda pe ido i es (Figu e 1). This dynamo he mal au eole, named as Hoyo del
Bo e migma i e [17], o ms a 100–200-m- hick laye pa allel o he lowe con ac o he
pe ido i e shee ha cu s obliquely all he ma e ials, including he Is an migma i es [16,22]
and de lec s he p e ious s uc u es (S1, S2) de eloped in he me apeli ic sequence o he
Guadaiza nappe. This dynamo he mal au eole is in e p e ed as a low- iscosi y shea zone
o med a empe a u es high enough, ≈725 °C, o p omo e he pa ial mel ing o he un-
de laying me apeli ic sequence du ing he ho emplacemen o he Ronda pe ido i es a
Alpine imes [23]. I shows an ana exis and s ain inc ease owa d he con ac o he pe i-
do i e slab. I s lowe po ion con ains un olia ed s oma ic migma i es ha a e p og es-
si ely ans o med in o nebuli ic migma i es ich in ounded blocks o qua z and angula
es i es om he me amo phic sequence and e en he ma bles [17]. Towa d he pe ido-
i es, he coa se-g ained and un olia ed migma i es a e p og essi ely ans o med in o
p o omyloni es ha gi e way o S/C myloni es and, inally, ul amyloni es. The age o his
second migma iza ion has been cons ained by U-Pb SHRIMP da ing on zi cons a 22 Ma
[21] and 22.3 ± 0.7 Ma [23]. O he addi ional geoch onological da a come om he g ani e
Figu e 2.
Field images o s udied sample ou c ops: (
A
) schis s and qua zi es o he me apeli ic
sequence ( b-2009-7), (
B
) Is an migma i es ( b-07-845), (
C
) in e laye ed qua zi e wi hin coa se-
g ained ma bles ( b-18-06) and (
D
) Hoyo del Bo e myloni ic migma i e (Gu-35-2) wi h elonga ed
whi e qua z nodules and me apeli ic es i es (da k g ey) ha de ine he myloni ic olia ion (SMyl).
The Guadaiza nappe shows wo main ana ec ic e en s ecognized om ec onic a -
gumen s [
17
]. The oldes one is eco ded by he Is an migma i es (Figu e 2b) and is
ela ed o he p e-alpine egional me amo phism o he me apeli ic sequence. Pe o med
geoch onological s udies wi h he
207
Pb/
206
Pb sequen ial e apo a ion echnique [
20
] and
U/Pb SHRIMP da ing o me amo phic zi cons [
21
] yield Va iscan and la e-Va iscan ages
o
319 ±8 Ma
and 299
±
4 Ma, espec i ely. The younges e en is ep esen ed by he
migma i es concen a ed a ound a dynamo he mal au eole associa ed wi h he emplace-
men o he o e lying Ronda pe ido i es (Figu e 1). This dynamo he mal au eole, named
as Hoyo del Bo e migma i e [
17
], o ms a 100–200-m- hick laye pa allel o he lowe
con ac o he pe ido i e shee ha cu s obliquely all he ma e ials, including he Is an
migma i es [
16
,
22
] and de lec s he p e ious s uc u es (S
1
, S
2
) de eloped in he me apeli ic
sequence o he Guadaiza nappe. This dynamo he mal au eole is in e p e ed as a low-
iscosi y shea zone o med a empe a u es high enough,
≈
725
◦
C, o p omo e he pa ial
mel ing o he unde laying me apeli ic sequence du ing he ho emplacemen o he Ronda
pe ido i es a Alpine imes [
23
]. I shows an ana exis and s ain inc ease owa d he con ac
o he pe ido i e slab. I s lowe po ion con ains un olia ed s oma ic migma i es ha a e
p og essi ely ans o med in o nebuli ic migma i es ich in ounded blocks o qua z and
angula es i es om he me amo phic sequence and e en he ma bles [
17
]. Towa d he
pe ido i es, he coa se-g ained and un olia ed migma i es a e p og essi ely ans o med
in o p o omyloni es ha gi e way o S/C myloni es and, inally, ul amyloni es. The age
o his second migma iza ion has been cons ained by U-Pb SHRIMP da ing on zi cons a
Mine als 2022,12, 325 4 o 16
22 Ma [
21
] and 22.3
±
0.7 Ma [
23
]. O he addi ional geoch onological da a come om he
g ani e dykes de eloped om pa ial mel s a ising om he dynamo he mal au eole. The
g ani e dykes ha in ude in o he pe ido i es also da e he ana exis and dynamo he mal
au eole a a ound 22 Ma [23,24].
3. Sample Loca ion and Desc ip ion
Fou samples om he Guadaiza nappe (Figu e 1) we e selec ed o his s udy. The
samples we e collec ed om he p e iously desc ibed membe s o he Guadaiza nappe:
(1) a
schis om he me apeli ic sequence (sample b-2009-7; Figu e 2a), (2) a migma i e
om he Is an migma i es (sample b-07-845; Figu e 2b), (3) a qua zi e in e laye ed wi h he
coa se-g ained T iassic ma bles (sample b-18-06; Figu e 2c) and (4) a myloni ic migma i e
om he Hoyo del Bo e migma i e (sample Gu-35-2; Figu e 2d).
The sample b-2009-7, a ine-g ained da k schis loca ed a he uppe le els o he
me apeli ic sequence o he Guadaiza nappe (Figu e 1), comes om a s ongly de o med
zone wi h a pene a i e S
2
-schis osi y. S
2
is pa allel o he axial plane o igh olds ha de-
o m eins o whi e qua z and an olde S
1
-schis osi y (Figu e 2a), de ined by qua z, bio i e
and g aphi e. Idioblas ic po phy oblas s o andalusi e andomly g ow on S2(Figu e 3a).
Mine als 2022, 12, x 4 o 16
dykes de eloped om pa ial mel s a ising om he dynamo he mal au eole. The g ani e
dykes ha in ude in o he pe ido i es also da e he ana exis and dynamo he mal au eole
a a ound 22 Ma [23,24].
3. Sample Loca ion and Desc ip ion
Fou samples om he Guadaiza nappe (Figu e 1) we e selec ed o his s udy. The
samples we e collec ed om he p e iously desc ibed membe s o he Guadaiza nappe:
(1) a schis om he me apeli ic sequence (sample b-2009-7; Figu e 2a), (2) a migma i e
om he Is an migma i es (sample b-07-845; Figu e 2b), (3) a qua zi e in e laye ed wi h
he coa se-g ained T iassic ma bles (sample b-18-06; Figu e 2c) and (4) a myloni ic mig-
ma i e om he Hoyo del Bo e migma i e (sample Gu-35-2; Figu e 2d).
The sample b-2009-7, a ine-g ained da k schis loca ed a he uppe le els o he
me apeli ic sequence o he Guadaiza nappe (Figu e 1), comes om a s ongly de o med
zone wi h a pene a i e S2-schis osi y. S2 is pa allel o he axial plane o igh olds ha
de o m eins o whi e qua z and an olde S1-schis osi y (Figu e 2a), de ined by qua z,
bio i e and g aphi e. Idioblas ic po phy oblas s o andalusi e andomly g ow on S2 (Figu e
3a).
Figu e 3. Tex u al pho omic og aphs o he analysed samples. (A) De ail o ela ions in schis s be-
ween he S2 pa allel o he axial plane o mic o olds ha de o m an olde S1-schis osi y. The schis-
osi y is de ined by qua z bio i e and g aphi e. Idioblas ic po phy oblas o andalusi e (And)
g ow h on S2. Plane-pola ized ligh (sample b-2009-7). (B) Polymine alic sillimani e (Sil) lakes and
pa allel a angemen o qua z and plagioclase in he sample b-07-845 om he Is an migma i es.
C ossed pola s. (C) Mic oscopic ab ic o sample b-18-06, a qua zi e in e laye ed wi h ma bles,
showing a pene a i e schis osi y, S2, ma ked by he p e e ed o ien a ion o ec ys allized g ains o
qua z and musco i e. C ossed pola s. (D) Idioblas ic po phy oblas o plagioclase wi h inclusions
o ga ne and bio i e. Co die i e (C d) po phy oblas s and mosaic ex u es in ec ys allized qua z
indica e a high empe a u e de o ma ion o sample Gu-35-2 (Hoyo del Bo e migma i e). C ossed
pola s.
Tb-07-845 is a sample om he Is an migma i es ha co esponds o he deepes and
mos me amo phic zone o he Guadaiza nappe and only c ops ou in he eas e n pa o
he s udied zone (Figu e 1). Despi e i s small a eal ex en , he Is an migma i es display
Figu e 3.
Tex u al pho omic og aphs o he analysed samples. (
A
) De ail o ela ions in schis s
be ween he S
2
pa allel o he axial plane o mic o olds ha de o m an olde S
1
-schis osi y. The schis-
osi y is de ined by qua z bio i e and g aphi e. Idioblas ic po phy oblas o andalusi e (And) g ow h
on S
2
. Plane-pola ized ligh (sample b-2009-7). (
B
) Polymine alic sillimani e (Sil) lakes and pa allel
a angemen o qua z and plagioclase in he sample b-07-845 om he Is an migma i es. C ossed
pola s. (
C
) Mic oscopic ab ic o sample b-18-06, a qua zi e in e laye ed wi h ma bles, showing a
pene a i e schis osi y, S
2
, ma ked by he p e e ed o ien a ion o ec ys allized g ains o qua z and
musco i e. C ossed pola s. (
D
) Idioblas ic po phy oblas o plagioclase wi h inclusions o ga ne and
bio i e. Co die i e (C d) po phy oblas s and mosaic ex u es in ec ys allized qua z indica e a high
empe a u e de o ma ion o sample Gu-35-2 (Hoyo del Bo e migma i e). C ossed pola s.
Tb-07-845 is a sample om he Is an migma i es ha co esponds o he deepes and
mos me amo phic zone o he Guadaiza nappe and only c ops ou in he eas e n pa o
he s udied zone (Figu e 1). Despi e i s small a eal ex en , he Is an migma i es display
Mine als 2022,12, 325 5 o 16
g ea s uc u al di e si y, as indica ed by he p esence o highly di e en ia ed dykes and
pods o pegma i e wi hin s oma ic o phlebi ic migma i e (Figu e 2b). These ocks coexis
wi h many es i ic zones whe e sillimani e, bio i e and g aphi e a e concen a ed. The
analysed sample, b-07-854, shows polymine alic sillimani e lakes ha enhance a weak
olia ion ha is de ined by he pa allel a angemen o sligh ly elonga ed g ains o qua z
and plagioclase (Figu e 3b). In e laye ed wi hin he coa se-g ained ma bles ha c own
he ock sequence o he Guadaiza nappe (Figu e 1), he sample b-18-06 co esponds o a
ine-g ained qua zi e laye abou ou me e s hick (Figu e 2c). Bo h ma bles and qua zi es
show a well-de ined olia ion, S
2
, ela ed o isoclinal olds. The mic oscopic ab ic exhibi s
a pene a i e schis osi y, S
2
, ma ked by he p e e ed o ien a ion o ec ys allized g ains o
qua z and musco i e (Figu e 3c).
Sample Gu-35-2 belongs o he Hoyo del Bo e migma i es ha co espond o he
dynamo he mal au eole o med du ing he ho h us ing o he Ronda pe ido i es o e
he Guadaiza nappe [
17
]. These migma i es a e medium- o coa se-g ained dia exi e and
nebuli e ha a e nea ly iso opic and ich in co die i e and eldspa po phy oblas s. They
a e easily ecognizable in he ield by he p esence o la ge es i ic blocks o whi e qua z,
schis and ma bles om he li hological me apeli ic sequence o he Guadaiza nappe.
Close o he o e lying Ronda pe ido i es, he Hoyo del Bo e migma i es ha e de eloped
a myloni ic olia ion, S
Myl
, ha is enhanced by he elonga ion o he es i ic blocks ([
22
],
Figu e 2d). The cha ac e is ic me amo phic associa ion o hese migma i es consis s o
K- eldspa + plagioclase + bio i e + co die i e. The po phy oblas s o K- eldspa usually
display poikili ic ex u e, de ined by inclusions o co die i e, qua z, sillimani e, bio i e o
ga ne in andom o ien a ion (Figu e 3d).
4. Analy ical Me hods
Zi con c ys als we e sepa a ed by con en ional mine al sepa a ion echniques (c ush-
ing, sie ing unde 125
µ
m, hea y liquids and magne ic sepa a ion) in he Depa men
o Geology o he Uni e si y o he Basque Coun y. Zi con c ys als we e handpicked
alea o y, moun ed in epoxy esin and polished app oxima ely o hal o hei hickness.
The in e nal s uc u e o he zi con c ys als was ecognized in backsca e ed elec on (BSE)
images, ob ained using a scanning elec on mic oscope (JEOL7000F-JSM; ope a i e con-
di ions
20 kV,
3 nA and WD 10 mm). Zi con c ys als we e analysed by LA-ICP-MS a
he Uni e si y o he Basque Coun y (SGIke -Geoch onology and Iso ope Geochemis y
Facili y) using a 193 nm RESOlu ion SE lase wi h a pulse ene gy densi y o ~6 J cm
−2
and a equency o 5 Hz coupled o a The mo Fishe iCAP Qc quad upole ICP-MS. The
analy ical spo size was 30 o 24
µ
m, depending on zi con size, and in mos o he spo s he
zi con c ys als we e comple ely pie ced h ough. Da a educ ion was ca ied ou using GJ-1
zi con s anda d o calib a ion [
25
] and Pleso ice [
26
] and 91500 zi con [
27
] as seconda y
s anda ds (Supplemen a y Ma e ial Table S1). The labo a o y s a educed he da a using
he Ioli e 3.6 so wa e package [
28
,
29
] and Vizual Age [
30
]. Ages in he ex and he igu es
a e quo ed always wi h conco dance be ween 90% and 110% and as
206
Pb/
238
U ages. Te a-
Wasse bu g diag ams and weigh ed a e age ages we e p oduced using Isoplo /Ex 3.0 [
31
],
he dis ibu ion o zi con ages and he Ke nel Densi y Es ima ion (KDE) plo s, wi h bin
wid hs o 60 and 30, espec i ely, we e calcula ed using Densi yPlo e 8.5 [32].
5. LA-ICP-MS Resul s
5.1. Sample b-2009-7 (Schis )
Two hund ed and one zi con c ys als we e analysed, o which only one hund ed and
se en y- ou , wi h Conco dia alues anging be ween 90% and 110%, we e conside ed
(Supplemen a y Ma e ial Table S1). Mos ly, analysed zi con c ys als a e xenomo phic
and display ounded mo phologies (Figu e 4). BSE images shows zi con c ys als wi h
single and composi e s uc u e (co es o e g own by ims). The co es display ounded,
e oded and eso bed mo phologies wi h mos ly s uc u eless o pa chy zonings, while he
ims display oscilla o y and homogenous zoning. Single zi con c ys als ha e oscilla o y
Mine als 2022,12, 325 6 o 16
and mainly homogenous zonings. Measu ed Th/U a ios a e be ween 1.71 and 0.01.
Mos ly, zi cons display Th/U a ios > 0.1 (n
−
163) and only 11 zi con analyses ha e
Th/U a ios < 0.1 (n −11) (Figu e 5).
Mine als 2022, 12, x 6 o 16
and eso bed mo phologies wi h mos ly s uc u eless o pa chy zonings, while he ims
display oscilla o y and homogenous zoning. Single zi con c ys als ha e oscilla o y and
mainly homogenous zonings. Measu ed Th/U a ios a e be ween 1.71 and 0.01. Mos ly,
zi cons display Th/U a ios > 0.1 (n − 163) and only 11 zi con analyses ha e Th/U a ios <
0.1 (n − 11) (Figu e 5).
Figu e 4. Backsca e ed elec on images and op ical pho omic og aphs o analysed zi cons om b-
2009-7 sample (schis ). Ellipses ma k analy ical spo loca ions and he ex shows spo names (i alics)
and 208Pb/236U age in Ma (bold).
Figu e 5. U s Th composi ional diag am o analysed zi cons.
Al hough age dis ibu ion pa e ns o he analysed zi cons a e sca e ed om 256 o
2704 Ma (Figu e 6a), abou 79% o hem yield P ecamb ian ages ha mos ly g oup a ound
Neop o e ozoic (50%; ca. 551–998 Ma) and Paleop o e ozoic (20%; ca. 1.6–2.5 Ga) peaks,
wi h mino Mesop o e ozoic (6%; ca. 1.0–1.1 Ga) and A chean (3%; ca. 2.5–2.7 Ga) popu-
la ions. The emaining 21% analyses co espond o Paleozoic ages. Th ee main popula-
ions can be peaked om KDE plo s a ~ 500 Ma, ~ 600 Ma and ~ 1 Ga (Figu e 6a). The
calcula ed weigh ed a e age 206Pb/238U ages o he popula ions esul in mean alues o
494 3 Ma (n − 8), 599 3 Ma (n − 13) and 1010 5 Ma (n − 6). A weigh ed mean age o
443 4 Ma a ising om he younges ou zi con c ys als can be conside ed as he
Figu e 4.
Backsca e ed elec on images and op ical pho omic og aphs o analysed zi cons om
b-2009-7 sample (schis ). Ellipses ma k analy ical spo loca ions and he ex shows spo names
(i alics) and 208Pb/236U age in Ma (bold).
Mine als 2022, 12, x 6 o 16
and eso bed mo phologies wi h mos ly s uc u eless o pa chy zonings, while he ims
display oscilla o y and homogenous zoning. Single zi con c ys als ha e oscilla o y and
mainly homogenous zonings. Measu ed Th/U a ios a e be ween 1.71 and 0.01. Mos ly,
zi cons display Th/U a ios > 0.1 (n − 163) and only 11 zi con analyses ha e Th/U a ios <
0.1 (n − 11) (Figu e 5).
Figu e 4. Backsca e ed elec on images and op ical pho omic og aphs o analysed zi cons om b-
2009-7 sample (schis ). Ellipses ma k analy ical spo loca ions and he ex shows spo names (i alics)
and 208Pb/236U age in Ma (bold).
Figu e 5. U s Th composi ional diag am o analysed zi cons.
Al hough age dis ibu ion pa e ns o he analysed zi cons a e sca e ed om 256 o
2704 Ma (Figu e 6a), abou 79% o hem yield P ecamb ian ages ha mos ly g oup a ound
Neop o e ozoic (50%; ca. 551–998 Ma) and Paleop o e ozoic (20%; ca. 1.6–2.5 Ga) peaks,
wi h mino Mesop o e ozoic (6%; ca. 1.0–1.1 Ga) and A chean (3%; ca. 2.5–2.7 Ga) popu-
la ions. The emaining 21% analyses co espond o Paleozoic ages. Th ee main popula-
ions can be peaked om KDE plo s a ~ 500 Ma, ~ 600 Ma and ~ 1 Ga (Figu e 6a). The
calcula ed weigh ed a e age 206Pb/238U ages o he popula ions esul in mean alues o
494 3 Ma (n − 8), 599 3 Ma (n − 13) and 1010 5 Ma (n − 6). A weigh ed mean age o
443 4 Ma a ising om he younges ou zi con c ys als can be conside ed as he
Figu e 5. U s. Th composi ional diag am o analysed zi cons.
Al hough age dis ibu ion pa e ns o he analysed zi cons a e sca e ed om 256
o 2704 Ma (Figu e 6a), abou 79% o hem yield P ecamb ian ages ha mos ly g oup
a ound Neop o e ozoic (50%; ca. 551–998 Ma) and Paleop o e ozoic (20%; ca. 1.6–2.5 Ga)
peaks, wi h mino Mesop o e ozoic (6%; ca. 1.0–1.1 Ga) and A chean (3%; ca.
2.5–2.7 Ga
)
popula ions. The emaining 21% analyses co espond o Paleozoic ages. Th ee main
popula ions can be peaked om KDE plo s a ~500 Ma, ~600 Ma and ~1 Ga (Figu e 6a).
The calcula ed weigh ed a e age
206
Pb/
238
U ages o he popula ions esul in mean alues
o 494
±
3 Ma (n
−
8), 599
±
3 Ma (n
−
13) and 1010
±
5 Ma (n
−
6). A weigh ed mean
age o 443
±
4 Ma a ising om he younges ou zi con c ys als can be conside ed as he
Mine als 2022,12, 325 7 o 16
younges zi con popula ion. Th/U analyses wi h alues < 0.1 a e mainly concen a ed
a ound he zi con age popula ion o ~600 Ma (Figu e 7).
Mine als 2022, 12, x 7 o 16
younges zi con popula ion. Th/U analyses wi h alues <0.1 a e mainly concen a ed
a ound he zi con age popula ion o ~ 600 Ma (Figu e 7).
Figu e 6. Te a-Wasse bu g, Ke nel Densi y Es ima ion (KDE) plo s and his og ams o age dis ibu-
ions o analysed zi cons o Guadaiza’s samples. (A) b-2009-1, (B) b-07-845 and (C) Gu-35-2.
Figu e 6.
Te a-Wasse bu g, Ke nel Densi y Es ima ion (KDE) plo s and his og ams o age dis ibu-
ions o analysed zi cons o Guadaiza’s samples. (A) b-2009-1, (B) b-07-845 and (C) Gu-35-2.
Mine als 2022,12, 325 8 o 16
Mine als 2022, 12, x 8 o 16
Figu e 7. Th/U s 206Pb/238U Age (Ma) o analysed zi cons o Guadaiza nappe´s samples.
5.2. Sample b-07-845 (Is an Migma i e)
Two hund ed and o y-se en zi cons we e analysed by LA-ICP-MS and only one
hund ed and nine y- ou yielded conco dan ages be ween 156 Ma and 3009 Ma (Supple-
men a y Ma e ial Table S1). Analysed zi con c ys als a e idiomo phic and display p is-
ma ic o bipy amidal mo phologies (Figu e 8). Mos o he zi cons display a composi e
co e– im s uc u e. The composi e zi cons ha e an e oded o eso bed de i al inclusions-
ee co e o e g own by a ligh e and a concen ic poikili ic im s uc u e (Figu e 8). Single
zi con c ys als display mainly con inuous oscilla o y o homogenous zonings. Al hough
he measu ed Th/U a ios a y widely be ween 1.312 and 0.01 (Figu e 5), mos analyses (n
− 142) yield Th/U a ios >0.1 and 52 zi con analyses ha e Th/U a ios <0.1.
Age dis ibu ion pa e ns (Figu e 6b) show ha 48% o he analysed zi cons a e
Paleozoic and ha 3% ha e a Mesozoic o igin. The e a e 49% ha a e P ecamb ian in age
and mos ly yield Neop o e ozoic (30%; ca. 548–998 Ma) and Paleop o e ozoic (12%; ca.
1.7–2.5 Ga) ages, wi h he es being Mesop o e ozoic (5%; ca. 1.0–1.6 Ga) and A chean
(2%; 2.6–3.0 Ga). Fou main popula ions a e peaked a ~ 300 Ma, ~ 500 Ma, ~ 600 Ma and
~1 Ga (Figu e 6b). The calcula ed weigh ed a e age 206Pb/238U ages o he popula ions
aises alues o 299 2 Ma (n − 10), 500 4 Ma (n − 9), 595 4 Ma (n − 13) and 1003 9 Ma
(n − 6). Th/U analyses wi h alues <0.1 a e concen a ed wi hin ~ 300 and ~ 600 Ma aged
zi con popula ions (Figu e 7).
Figu e 7. Th/U s. 206Pb/238U Age (Ma) o analysed zi cons o Guadaiza nappe’s samples.
5.2. Sample b-07-845 (Is an Migma i e)
Two hund ed and o y-se en zi cons we e analysed by LA-ICP-MS and only
one hund ed and nine y- ou yielded conco dan ages be ween 156 Ma and 3009 Ma
(Supplemen a y Ma e ial Table S1). Analysed zi con c ys als a e idiomo phic and display
p isma ic o bipy amidal mo phologies (Figu e 8). Mos o he zi cons display a composi e
co e– im s uc u e. The composi e zi cons ha e an e oded o eso bed de i al inclusions-
ee co e o e g own by a ligh e and a concen ic poikili ic im s uc u e (Figu e 8). Single
zi con c ys als display mainly con inuous oscilla o y o homogenous zonings. Al hough
he measu ed Th/U a ios a y widely be ween 1.312 and 0.01 (Figu e 5), mos analyses
(n −142) yield Th/U a ios >0.1 and 52 zi con analyses ha e Th/U a ios < 0.1.
Mine als 2022, 12, x 9 o 16
Figu e 8. BSE images and op ical pho omic og aphs o analysed zi cons om b-07-845 sample
(migma i e). Ellipses ma k analy ical spo loca ions and he ex shows spo names (i alics) and
208Pb/236U age in Ma (bold).
5.3. Sample Gu-35-2 (Hoyo Del Bo e Migma i e)
One hund ed and se en y- i e zi cons we e analysed by LA-ICP-MS. As in he Is an
migma i e sample, he analysed zi con c ys als a e idiomo phic and display mainly bi-
py amidal mo phologies (Figu e 9). Single and composi e co e– im s uc u e zi cons a e
obse ed. The c ys als wi h composi e s uc u e ha e e oded and eso bed co es and
some imes a e o e g own by a ligh and hin im. Due o hei hinness hese ims could
no be da ed by LA-ICP-MS. Measu ed Th/U a ios a e in be ween 2.4 and 0.01. Mos zi -
cons display Th/U a ios >0.1 (n − 128) and only 13 zi con analyses ha e Th/U a ios < 0.1
(Figu e 5).
Age dis ibu ion pa e ns (Figu e 6c) om 192 o 3019 Ma show ha 79% o he ana-
lysed zi cons a e P ecamb ian in age and mos ly yield Neop o e ozoic (55%; ca. 543–1000
Ma) and Paleop o e ozoic (18%; ca. 1.6–2.4 Ga) ages, wi h he es being Mesop o e ozoic
(4%; ca. 1.0–1.6 Ga) and A chean (2%; ca. 2.5–3.0 Ga). The emaining analyses gi e Paleo-
zoic (19%; ca. 278–524 Ma) o Mesozoic (2%; ca. 192–206 Ma) ages. Two main popula ions
can be peaked a 585 3 Ma (n − 9) and 978 7 Ma (n − 5). Th/U analyses wi h alues <0.1
mainly come om he zi con popula ion aged a 585 3 Ma (Figu e 7).
Figu e 8. Con .
Mine als 2022,12, 325 9 o 16
Mine als 2022, 12, x 9 o 16
Figu e 8. BSE images and op ical pho omic og aphs o analysed zi cons om b-07-845 sample
(migma i e). Ellipses ma k analy ical spo loca ions and he ex shows spo names (i alics) and
208Pb/236U age in Ma (bold).
5.3. Sample Gu-35-2 (Hoyo Del Bo e Migma i e)
One hund ed and se en y- i e zi cons we e analysed by LA-ICP-MS. As in he Is an
migma i e sample, he analysed zi con c ys als a e idiomo phic and display mainly bi-
py amidal mo phologies (Figu e 9). Single and composi e co e– im s uc u e zi cons a e
obse ed. The c ys als wi h composi e s uc u e ha e e oded and eso bed co es and
some imes a e o e g own by a ligh and hin im. Due o hei hinness hese ims could
no be da ed by LA-ICP-MS. Measu ed Th/U a ios a e in be ween 2.4 and 0.01. Mos zi -
cons display Th/U a ios >0.1 (n − 128) and only 13 zi con analyses ha e Th/U a ios < 0.1
(Figu e 5).
Age dis ibu ion pa e ns (Figu e 6c) om 192 o 3019 Ma show ha 79% o he ana-
lysed zi cons a e P ecamb ian in age and mos ly yield Neop o e ozoic (55%; ca. 543–1000
Ma) and Paleop o e ozoic (18%; ca. 1.6–2.4 Ga) ages, wi h he es being Mesop o e ozoic
(4%; ca. 1.0–1.6 Ga) and A chean (2%; ca. 2.5–3.0 Ga). The emaining analyses gi e Paleo-
zoic (19%; ca. 278–524 Ma) o Mesozoic (2%; ca. 192–206 Ma) ages. Two main popula ions
can be peaked a 585 3 Ma (n − 9) and 978 7 Ma (n − 5). Th/U analyses wi h alues <0.1
mainly come om he zi con popula ion aged a 585 3 Ma (Figu e 7).
Figu e 8.
BSE images and op ical pho omic og aphs o analysed zi cons om b-07-845 sample
(migma i e). Ellipses ma k analy ical spo loca ions and he ex shows spo names (i alics) and
208Pb/236U age in Ma (bold).
Age dis ibu ion pa e ns (Figu e 6b) show ha 48% o he analysed zi cons a e
Paleozoic and ha 3% ha e a Mesozoic o igin. The e a e 49% ha a e P ecamb ian in
age and mos ly yield Neop o e ozoic (30%; ca. 548–998 Ma) and Paleop o e ozoic (12%;
ca. 1.7–2.5 Ga)
ages, wi h he es being Mesop o e ozoic (5%; ca. 1.0–1.6 Ga) and A chean
(2%; 2.6–3.0 Ga). Fou main popula ions a e peaked a ~300 Ma, ~500 Ma, ~600 Ma and
~1 Ga
(Figu e 6b). The calcula ed weigh ed a e age
206
Pb/
238
U ages o he popula ions
aises alues o 299
±
2 Ma (n
−
10), 500
±
4 Ma (n
−
9), 595
±
4 Ma (n
−
13) and
1003 ±9 Ma
(n
−
6). Th/U analyses wi h alues < 0.1 a e concen a ed wi hin ~ 300 and
~ 600 Ma aged zi con popula ions (Figu e 7).
5.3. Sample Gu-35-2 (Hoyo Del Bo e Migma i e)
One hund ed and se en y- i e zi cons we e analysed by LA-ICP-MS. As in he Is-
an migma i e sample, he analysed zi con c ys als a e idiomo phic and display mainly
bipy amidal mo phologies (Figu e 9). Single and composi e co e– im s uc u e zi cons
a e obse ed. The c ys als wi h composi e s uc u e ha e e oded and eso bed co es and
some imes a e o e g own by a ligh and hin im. Due o hei hinness hese ims could no
be da ed by LA-ICP-MS. Measu ed Th/U a ios a e in be ween 2.4 and 0.01. Mos zi cons
display Th/U a ios > 0.1 (n
−
128) and only 13 zi con analyses ha e
Th/U a ios < 0.1
(Figu e 5).
Mine als 2022, 12, x 10 o 16
Figu e 9. BSE images and op ical pho omic og aphs o analysed zi cons om Gu-35-2 sample (my-
loni ic migma i e). Ellipses ma k analy ical spo loca ions and he ex shows spo names (i alics)
and 208Pb/236U age in Ma (bold).
5.4. Sample b-18-06 (Qua zi e In e laye ed wi h Ma bles)
One hund ed and se en y- wo zi con c ys als we e analysed and only one hund ed
and hi y- ou we e conside ed (Supplemen a y Ma e ial Table S1). While zi con c ys als
mainly show idiomo phic shapes in he migma i es (Hoyo del Bo e and Is an) and xeno-
mo phic in he schis s, he zi con c ys als in he qua zi e o he Guadaiza nappe display
bo h xenomo phic and idiomo phic zi con popula ions in simila p opo ions (Figu e 10).
The xenomo phic zi con popula ion display a composi e s uc u e bu mos a e a single
s uc u e. The la e display homogenous o oscilla o y zonings, whe eas hose wi h a
composi e s uc u e display a ounded o eso bed co e wi h homogeneous o oscilla o y
zoning o e g own by a hin and ligh e im. Measu ed Th/U a ios a e in be ween 0.02–
3.9 and 0.01–0.56 o he xenomo phic and idiomo phic zi con popula ions, espec i ely
(Figu e 5).
Figu e 10. BSE images and op ical pho omic og aphs o analysed zi cons om b-18-06 sample
(qua zi e). Ellipses ma k analy ical spo loca ions and he ex shows spo names (i alics) and
208Pb/236U age in Ma (bold).
Figu e 9.
BSE images and op ical pho omic og aphs o analysed zi cons om Gu-35-2 sample
(myloni ic migma i e). Ellipses ma k analy ical spo loca ions and he ex shows spo names (i alics)
and 208Pb/236U age in Ma (bold).
Mine als 2022,12, 325 16 o 16
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