_UDK 903.23'I6(498)''634'':902.65_
Documenta PraehistoricaXXXIV (2007)
Phase and chemical composition analysis of pigments
used in Cucuteni Neolithic painted ceramics
Bogdan Constantinescu1, Roxana Bugoi1, Emmanuel Pantos2, Dragomir Popovici3
1 'Horia Hulubei' National Institute of Nuclear Physics and Engineering, Bucharest, Romania
bconst@nipne.ro
2 CCLRC, Daresbury Laboratory, Warrington, UK
3 National Museum of Romania's History, Bucharest, Romania
ABSTRACT - Two analytical methods - 241Am-based X-Ray Fluorescence (XRF) and Synchrotron Ra-
diation X-ray Diffraction (SR-XRD) - were used to investigate the elemental and mineralogical com-
position of pigments which decorate some Cucuteni Neolithic ceramic sherds. Local hematite and lo-
cal calcite were the main components for red and white pigments, respectively. For black pigments,
iron oxides (e.g. magnetite) were used. They were often mixed with manganese oxides (e.g. jacob-
site), which originated from Iacobeni manganese minerals deposits on the Bistrita River. Taking into
account the results of the experiments, several conclusions regarding manufacturing procedures em-
ployed, and potential trade routes during the Neolithic were drawn.
IZVLEČEK - Za določanje elementarne in mineraloške sestave pigmentov, s katerimi so okrašene ne-
katere keramične posode kulture Cucuteni, sta bili uporabljeni dve analitski metodi - 241Am X-Ray
Fluorescence (XRF) in Synchrotron Radiation X-ray Diffraction (SR-XRD). Lokalni hematit in kalcit
sta bila glavni komponenti rdečih oziroma belih pigmentov. Za črne pigmente so uporabljali železo-
ve okside (magnetit). Pogosto so jih zmešali z manganovimi oksidi (jakobsitom), ki izvirajo iz Iaco-
beni manganovih mineralnih depozitov reke Bistrita. Če upoštevamo rezultate poizkusov, lahko po-
tegnemo več zaključkov o uporabljenih proizvodnih postopkih in o možnih trgovskih poteh v času
neolitika.
KEY WORDS - Cucuteni-Tripolye; ceramics; pigments; XRF; SR-XRD
Cucuteni ceramics
The history of the V-IVth millennia BCE is marked
by the flourishing of some great Eneolithical civiliza-
tions in the South-Eastern part of Europe: Vinca, Gu-
melnita and Cucuteni-Tripolye, representing moments
of high cultural evolution. Spread over a vast terri-
tory, with a total area of more than 300 000 km2 in
Romania, the Republic of Moldova and Ukraine, the
Cucuteni (in Romania, Tripolye in Ukraine) culture
is one of the last brilliant cultural expressions of the
Copper Age. Cucuteni-Tripolye culture had a long
evolution, being divided by specialists into three
main phases: Cucuteni A, Cucuteni A-B and Cucu-
teni B. The skilful and ingenious use of all the natu-
ral resources allowed the Cucutenian communities
to build solid and lasting houses, with resistant wo-
oden structures covered with clay mixed with straw
and hay. The craftsmen manufactured tools in either
carved or polished stone (flint, opal, jasper, etc.),
bone, horn or metal (copper), thus showing a high
level of knowledge.
The 'Queen' of prehistoric pottery, the Cucutenian
ceramics (Figs. 1, 2, 3) represent the most eloquent
proof not only of a perfect mastery of pottery (pro-
duction and temperature control and clay model-
ling), but also of an extremely well-developed aesthe-
tic sense that gave birth to genuine and unrivalled
prehistoric masterpieces. The decorations on this pot-
tery is proof of a remarkable aesthetic sense and, at
the same time, of a very complex spiritual life. The
prehistoric craftsmen created characteristic decora-
tions for each of the three evolutional stages of the
Copyright by Department of Archaeology, Faculty of arts, University of Ljubljana.
281
culture, with the use of incised lines, flutings and co-
lours (white, black and red), using the spiral as an
essential decorative element on the external (and
sometimes, internal) surface of the pots. It is almost
certain that the colours had magical significance: red
= life (blood), white = the good (light), and black =
the evil (darkness).
In the following lines, the previous results obtained
on Cucuteni ceramics by using X-Ray Fluorescence
(XRF), X-Ray Diffraction (XRD), and other specific
mineralogical methods will be reviewed. By means
of the XRF and powder diffraction analysis of a num-
ber of Cucuteni sherds from the Poduri settlement
(Bacau district - 50 km East of the Bistrita River)
were analyzed by Niculescu and Coltos (Niculescu,
Coltos and Popovici 1982.205-206). They pointed
out that the chromatophorous minerals of the white,
red and dark brown pigments were calcium silicate,
hematite, and jacobsite respectively, confirming the
results obtained for other Cucuteni-Tripolye settle-
ments by Stos-Gale and Rook (1981.155- 161).
In a synthetic study of Cucuteni-Tripolye culture,
Ellis (1980.211-230) made a technological characte-
rization of the Cucutenian pottery. The X-ray diffra-
ction and microscopic analyses were aimed at deter-
mining the mineralogical components of the ceramic
composition, and the pigments used in the painting
of the pottery. The results showed that the sources of
clay were local; the black pigment came from manga-
nese ores in the region, the red pigment from the
alteration of the iron minerals, and the white from
marls and kaolins. In late Cucuteni culture was fired
Fig. 2. Cucuteni A pottery, excavated from Poduri
site.
Fig. 1. Cucuteni A pottery, excavated from Poduri
site.
in kilns with a controlled atmosphere, the tempera-
tures in the kilns reaching 1000-1100 °C.
A comprehensive study of Cucuteni ceramics from
Northern Moldova (including pigments issue) has
been made by Gä|ä in (Marinescu-Balcu and Bolo-
mey 2000.111-131).
Summarizing the results from all the above referen-
ces, it can be stated that the pigments used for the
Cucuteni ceramics painting were mineral pigments
including clay minerals, quartz, and feldspars, with-
out iron and manganese oxides for the white chro-
Fig. 3. Cucuteni A pottery (Romanian National Hi-
story Museum).
mes, with iron oxides for the red chromes, and with
manganese oxides for the brownish-black chromes.
These pigments were prepared starting from diffe-
rent coloured clays as raw materials by powdering,
dispersion in water, separation of the fine fraction
by decantation, and drying. In general, the pigment
particle dimensions were of 5-15 ^m, based on the
width at half intensity of the quartz line at 4.26 A
(Sherrer's law). The raw materials were cements
and concretions with manganese oxides (birnesite
and manganite - very often found in Iacobeni depo-
sits) for the brownish-black chromes, iron and man-
ganese concretions, cambic horizons or lehms (goe-
thite - a-FOOH brown-red-brown-yellow colour and
lepidocrocite) for the red chromes, and a loam with-
out iron and manganese oxides for the white chro-
me. Through firing, the iron oxides, goethite and le-
pidocrocite, were transformed into hematite (Fe2O3 -
reddish-grey-white colour) for the red chromes, the
manganese oxides, birnesite and manganite, into
bixbyite, and more rarely into jacobsite, depending
on the iron and manganese content, and rarely into
haussmanite. The firing of the clay minerals caused
the predominant components to transform into oxi-
des in the process of crystallization, and at a tempe-
rature of over 900 °C, y AhO3 appeared. The fine-
ness of the pigment particles and their mineralogi-
cal composition indicate that the raw material for
the pigments came from the proximity of the settle-
ment, or from the region. The experimental prepara-
tion of pigments with brownish black and red chrome
from cemented sand, iron and manganese concre-
tions, and reddish clays, and the similar composition,
chromes and fineness thus obtained proved that
these were the sources for pigments.
White pigment was prepared from loam deprived of
chromophorous oxides; analyses of white and of its
sources were identical when the former had not un-
dergone firing.
The firm adhesion of the pigments to the vessel walls
was explained by their smectite content, a clay mi-
neral that gives the required adhesion. Neither the
clay, nor the pigments had calcareous concretions or
noticeable amounts of carbonates dispersed in the fa-
bric, and their source appeared to be a layer leached
of carbonates. The grain conglomerate structure of
the medium and course fabric, the large amounts of
iron and manganese concretions and broken sherds
in the ceramic mass, and the presence of remains
from pigment preparation, indicated their employ-
ment as an admixture in the fabric of vessels with
thicker walls.
Regarding the technological aspects of ceramics pro-
duction, the pottery was fired in an oxidizing atmo-
sphere, in kilns with a combustion chamber and fi-
ring chamber separated by a perforated grate. All
Cucuteni ceramics in the settlement were invariably
fired according to an imported program. When the
temperature rose too quickly to the nominal firing
temperature during the initial stage, fissures and fir-
ing cracks appeared in the ceramic mass. The conti-
nuous firing stage was thoroughly maintained at a
nominal temperature of 800-900 °C, which could
be assessed by the uniform and complete firing of
most vessels. A slow cooling stage followed, lasting
at least half a day, with draught reduced to a mini-
mum, allowing the complete transformation of ß
quartz into a quartz. The hue of the brownish-black
pigment, whose colour was rendered especially by
manganese hydroxides (possibly birnesite and man-
ganite), became more intense by firing, due to the
formation of bixbyite in most of the cases, of jacob-
site more rarely, and of hausmanite accidentally, ac-
cording to the content of iron and manganese oxides
and the firing temperature. Lepidocrocite and goe-
thite in the red pigments always turned into hema-
tite. Clay minerals in the white pigment were dehy-
droxylated, and the formation of y AhO3 occurred
exclusively in the fragments fired at a temperature
above 900 °C.
Experimental
For this study, two analytical methods were used:
241Am based XRF and powder SR-XRD. The analyzed
ceramics sherds were selected from the collection of
the National Museum of Romanian History in Bucha-
rest.
XRF is an analytical method used for the determina-
tion of elemental composition. It consists of the de-
tection of the characteristic X-ray emitted by the ana-
lyzed object as a consequence of its bombardment
with photons of suitable energy (tens of keV at most).
The analytical method is sensitive (minimum detec-
tion limits in the order of parts per million - ppm),
fast, and, most important when dealing with archa-
eological artefacts, non-destructive.
For the XRF measurements performed in this study,
a spectrometer consisting of a 30 mCi 241Am annu-
lar gamma-source and a Si(Li) detector (180 eV
FWHM at 5.9 keV resolution) was used. The elemen-
tal intensities data were normalized to their total
background spectrum counts - the sum of all charac-
teristic X-rays intensities for the excitation source -
respectively, and subtracted from their correspon-
ding normalized paste composition. Due to the pig-
ments layers strong non-homogeneity and to avoid
difficult calibration procedures, only the ratios of
the main characteristic elements were used.
XRD is capable of providing qualitative and someti-
mes quantitative information on regarding the pha-
ses (e.g. compounds) composition. The analytical
method is based on the fact that the wavelengths of
X-rays are of the same order of magnitude as the di-
stances between atoms or ions in a molecule or cry-
stal (~1 A = 10-1° m). Therefore, a crystal - or a cry-
stalline powder - diffracts an X-ray beam passing
through it, producing beams at specific angles de-
pending on the X-ray wavelength, the crystal orien-
tation, and the structure of the crystal. By analyzing
the resulting diffraction pattern, information on the
phases present in the analyzed sample are obtained.
However, XRD is a destructive method, a certain
amount of sample (e.g. crystalline powder) being ne-
cessary for the analysis, the measurements taking
place in transmission mode.
Using conventional XRD in pottery analysis, major
phases can be identified. However, in the case of ar-
chaeological objects, when the amount of sample to
be analyzed has to be as small as possible, it is neces-
sary to use the best experimental facilities. The ad-
vent of synchrotron radiation sources promoted the
method of Synchrotron Radiation-X Ray Diffraction
(SR-XRD), which became a powerful tool for detailed
structural determination and mineral phase studies
(Uda 2000.758-761). Its success is due to the fact
that minute amounts of sample can be analyzed in a
very short time (Tang 2001.1015-1024).
In particular, this experiment was focused on finding
the composition of the pigments used to decorate
some Cucuteni ceramics sherds. As special case is the
one of the black pigments, the main candidates be-
long to three categories: graphite, manganese mine-
rals and/or iron compounds. From previous analy-
ses reported in Dumitrescu (1985) it is known that
for Gumelnita (3500-2500 BC) culture, graphite, and
for Petresti (3500-2500 BC) culture magnetite were
used.
The SR-XRD measurements were performed at two
locations: at the Synchrotron Radiation Source (SRS),
Daresbury Laboratory (DL), UK, and at MAX-lab,
Lund, Sweden. Some of the SR-XRD data were taken
at station 14.1 of the SRS, by employing X-ray of
1.488 A wavelength, 0.2x0.2 mm beam size and a
flux of 1013 photons/s. The detection of the diffrac-
tion pattern was performed using a Quantum 4 ADSC
CCD detector, which collects two-dimensional dif-
fraction patterns of 2304x2304 pixels. The measure-
ments were performed in transmission mode with
an acquisition time of 30 seconds.
The pigment powders were gently scratched from
some tens of ceramics sherds using a diamond file.
The pigments were taken from areas of different co-
lours (white, red and brown/black), as well as from
the clay. Clay powders from all the sherds were also
measured in order to compare any contribution in
the diffraction patterns of the pigments, taking into
account the fact that the painted layers were very
thin (tens of ^m), and it was likely to have some
powder from the ceramic body in the sample extrac-
ted from the decorated surface.
At DL the powders were put in a sample cassette ha-
ving 36 holes, each of them having as a backing
Scotch tape®. The powders were pressed onto the
Scotch tape and the excess powder was removed in
order to have only a thin layer of it on the tape. The
overall acquisition time per sample was minimized
by the fact the cassette position (i.e. from a hole to
the neighboring one) was moved under computer
control from outside the station hutch. Silicon pow-
der was used as a standard mineral phase, in order
to determine the distance between sample and de-
tector and the centre of the diffraction pattern - both
required in order to reduce the data to intensity ver-
sus 20 angle graphs for further analysis.
The data reduction was performed by using the FIT-
2D package (the integration of the diffraction rings).
The mineral phase identification was carried out
with the aid of the ICDD (International Centre for
Diffraction Data) ®/JCPDS (Joint Committee for
Powder Diffraction Studies) database, as well as the
search-match procedures using the X'Pert HighScore
Plus and XPLOT software available at DL. The tape
background has been subtracted for all the spectra
using X'Pert HighScore Plus software.
The MAX II measurements were performed at beam
line 7.11 using the Huber G670 imaging-plate Guiner
camera (Stähl 2000.394-396) installed on crystal-
lgraphy beamline I711 at the MAX II synchrotron,
Lund, Sweden (Cerenius et al. 2000.203-208). The
samples - powder on Scotch tape - were exposed for
1200 s each to synchrotron radiation of 1.364 A wa-
velength.
The analysis of the experimental data began with
the identification of the relevant pigments using the
Diffrac Plus data base of mineralogical compounds
at MAX II. Further analysis consisted of the construc-
tion of the diffraction pattern using the data base in-
formation, followed by comparison with the results
obtained from measurements after background sub-
traction.
SR-XRD was used as a very accurate method to dis-
tinguish different clays and mineral pigments of va-
rious Neolithic pottery-producing centers located on
Romanian territory, most of them belonging to Cu-
cuteni-Tripolye painted Neolithic ceramics.
Ceramics sherds belonging to the following cultures:
Cri§-Starcevo (6000-4500 BC), the oldest Neolithical
culture, which covered the whole Balkan Peninsula
and Carpathian Basin, Vinca (4200-3500 BC), Tisza-
polgar (4500-3500 BC), Petregti (3500-2500 BC),
Gumelnita (3500-2500 BC), with its most spectacu-
lar archaeological site: the golden cemetery at Var-
na, were also studied. The extension of the study to
other cultures was due to the fact that the type and
quantity of clay minerals and non-plastic inclusions
in the clay can vary from region to region and the
composition can be altered by the preparation pro-
cedure and manufacturing process.
Results
Painted (red-white-brown-black) Cucuteni sherds
(Cucuteni A period) found in Moldova in sites situa-
ted in Bistrita Valley down the river (Izvoare, Calu,
Cagäria, Gheläiegti) were analyzed.
The XRF measurements revealed that for the black
(dark brown or chocolate black) colour Mn and Fe
were the main elements (see Fig. 4). For provenance
studies, the Mn/Fe ratio is significant because, due to
the very close energy values of the X-rays emitted
from both atoms, the matrix effects due to the pre-
sence of major (and lighter) elements can be assu-
med to have the same effect on the numerator and
denominator. Three groups of sherds were found:
Mn/Fe = 1/20, 1/5, 1/3 (1/20 is a normal value for
a common soil). In the area of Cucuteni culture there
are two main Mn deposits: Iacobeni, up to the Bistri-
ta River 150 km north of our analyzed sites in Mol-
dova, where the Mn/Fe ratio is under 3/10; and Kri-
voi Rog (Nikolaev) on the Dnepr River in Ukraine,
where the Mn/Fe ratio is from 8/10 up to 10/10.
The results obtained strongly suggest the use of Ia-
cobeni Mn minerals.
Energy (keV)
Fig. 4. Cucuteni black pigment XRF spectrum.
Concerning the white colour, Ca is the main element,
the pigment raw material being a light clay (type
kaolin) found relatively frequently in the region.
For the red colour we found Fe and Ti, concluding
that the pigment is an iron-rich, clay-based one, with
Ti used as reinforcing agent.
The analyzed clay was found to be of local prove-
nances, with great variation in composition (e.g. a
lot of Ca for the central region of Transylvania, a lot
of Fe for Moldova and Banat, a lot of K in the North-
East Transylvania). No clue regarding possible com-
mercial exchanges was obtained from taking into ac-
count these results. When the black colour was close
to dark brown, the compositional studies revealed
Fe oxides in its content. Indications of the use of car-
bon from bones (Central Transylvania), but also
from graphite (Gumelnita culture), in which connec-
tions with the Neolithic graphite mines in North-East
Bulgaria were revealed. The most interesting case is
the site from Cri§-Starcevo situated in Oltenia (Sal-
cuta), where Mn was detected as pyrolusite. This mi-
neral was abundant in the North of Greece and lar-
gely used in the 4th-5th centuries BC to produce the
famous Attic black glass sherds. A possible commer-
cial connection South-North in the Balkan Peninsula
can thus be deduced. In order to confirm this hypo-
thesis, other Neolithic sites in the area of the Carpa-
thian Mountains- Danube ceramics have to be ana-
lyzed.
Regarding the SR-XRD data obtained at DL, UK, the
diffraction pattern analysis led to the following con-
clusions:
• In some of the sherds with black decoration that
showed the presence of Mn in XRF spectra, several
varieties of jacobsite (Fe2MnO4) from the ICDD data-
base fit the position and relative intensity of five of
the peaks reasonably well. On the basis of the XRF
data that showed a clear presence of Mn in these
two samples, it was concluded that jacobsite is pre-
sent in the black colour decoration of these samples,
but with a slightly modified chemical formula where
Fe and Mn are reduced in weight due to the presence
of other metal atoms, such as Mg, that alter the cry-
stal lattice slightly. Magnesian jacobsite showed the
best fit for the position and relative intensity of the
peaks in the data (see Fig. 5).
•	In other sherds, the brown/black colour was due
to the presence of magnetite (iron oxide Fe3O4).
•	A considerable amount of time was spent trying to
identify black pigment patterns other than jacobsite,
such as graphite, and other Fe and Mn compounds,
such as hausmannite, pyrite, pyrolusite, bixbyite, py-
roxmangite, manganite, despujolsite, and rhodonite.
Graphite is hard to resolve in the acquired diffraction
patterns, since it exhibits a strong overlap at 3.4 A
with the quartz peak, which is situated at 3.34 A;
however, since the other peaks of graphite were not
found in the black pigment diffraction patterns, the
hypothesis of using carbon based pigments can not
be supported. None of the above mentioned Fe and
Mn minerals were found in any of the black pigment
samples.
•	Although the white colour was explained by the
previous measurements on similar sherds as result-
ing either from calcite, kaolinite or from gypsum, the
present data led to the conclusion that only in one
of the sherds was some calcite found, as well as some
augite (see Fig. 6).
Fig. 5. Cucuteni black pigment SR-XRD spectrum.
•	The red colour seems to come from the higher con-
tent in hematite of the powder (see Fig. 7). Hematite
also seems to be a component of the corresponding
ceramic body, but in much smaller amounts.
•	The ceramic body samples contain silicates, diop-
side being identifying as a well matching phase in
most of the samples.
The SR-XRD data obtained in Lund, Sweden, led to
the clear identification of the black pigment compo-
sition from Cucuteni in Northern Moldavia and Ari-
u§d in South-Eastern Transylvania type pottery (6th-
4th millennia BC): pyroxmangite (rodonite), an iron
manganese silicate (Fe2+, Mn2+-CaMn4[Si5Oi5]) for
high-temperature, >600 °C, fired pottery (the advan-
ced Cucuteni ceramics types A and B), and a mixture
of goethite (aFeO-OH), haussmanite (MnMn2O4), ja-
cobsite (Fe2MnO4), bixbyite (Mn, Fe)2O3 and psilome-
lane (MnO + MnO2 + H2O in variable proportions) for
Fig. 6. Cucuteni white pigment SR-XRD spectrum. Fig. 7. Cucuteni red pigment SR-XRD spectrum.
pottery fired at low temperature (<400 °C) (the pri-
mitive pre-Cucuteni type C).
Historically, all these minerals have their origin in
the North Moldavian mineral deposits of Iacobeni,
leading to the conclusion that Neolithic trade routes
already existed, covering approximately 500 km with
the crossing of the Carpathians along the Bistrita Ri-
ver. In the same samples there was no evidence of
pyrolusite (MnÜ2) and manganite [MnO(OH)], the
main components of Ukrainian Nikopol manganese
deposit (used as black pigment source by contempo-
rary Tripolye Neolithic culture). Other important re-
sults were the identification of magnetite (iron oxide
Fe3O4) as the main component for the black pig-
ments of the Central Transylvania Petre§ti culture
(4200-3500 BC), and the identification of graphite
as black pigment for Oltenia Starcevo-Cri§ culture ce-
ramics (6th-5th millennia BC), most probably from
Northern Bulgaria graphite deposits. Finally, the
black color of some carbon-based pigments is due to
their organic origin (bone or wood) and it was quite
challenging to identify them for several Cucuteni
sherds from North-Eastern Moldavia.
We can suppose that the transportation from Iacobe-
ni downriver of the Mn and Fe containing clays used
as raw materials for pigments was done by raft (na-
vigation on rafts made of conifers logs tied together
using plant fibre ropes). In this area, rafting is a tra-
ditional means of transporting timber (wood used in
carpentry and in house building), mentioned in do-
cuments as early as the 14th century.
The white pigment composition appears as a combi-
nation of calcite (CaCO3) for Cucuteni culture and as
calcium silicates mixed with aluminum silicate-illite
{(K,H2))Al2[(H2O, OH)2]AlSi3O10} for Petre§ti culture
(Transylvania). As expected, the measurements have
shown the presence of hematite (iron oxide Fe2O3) as
the main component for red pigments for all the
sherds examined. The clay examined for all the
sherds was identified as of local provenance. It can
be stated that the pigments used for the examined
Neolithic ceramics painted sherds were mineral pig-
ments including clay minerals, quartz and feldspars,
with manganese oxides for the brownish-black chro-
mes, with iron oxides for the red chromes, and with-
out iron or manganese oxides for the white chromes.
Through firing, the manganese oxides were trans-
formed into bixbyite, and more rarely into jacobsite,
depending on the iron and manganese content, and
rarely into haussmanite at temperatures less than
400 °C, and into piroxmangite at temperatures hig-
her than 600 °C. Correspondingly, the iron oxides
were transformed into hematite for the red chromes.
Conclusions
The conclusion of this study is that the pigments used
to decorate Cucuteni Neolithic ceramics were mainly
based on iron oxides for the red hues, and calcium
silicate and calcium carbonate for the white, while
the black pigment was due to different iron and man-
ganese compounds, such as magnetite and jacobsite.
It is obvious that during this Neolithic period pottery
workshops extended greatly over the present Roma-
nian territory, local clays being mostly used. How-
ever, in the case of black pigments a type of primi-
tive trade is evident. It is worth mentioning here that
our findings are in good agreement with previous
XRD and mineralogical studies, proving the use of
the local manganese deposits from Iacobeni as black
pigments sources for the Cucuteni ceramics in this
area of Moldova.
-ACKNOWLEDGEMENTS-
EU COST G8 'Non-destructive analysis and museum
testing' action - for funding one of the authors (Ro-
xana Bugoi) Short Term Scientific Mission at DL, UK.
EU - Research Infrastructure Action under the FP6
'Structuring the European Research Area' Program-
me (through the Integrated Infrastructure Initiative
'Integrating Activity on Synchrotron and Free Elec-
tron Laser Science') - for the financial support provi-
ded for the beam-times at MAX-lab, Sweden. Dr. Yngve
Cerenius and the staff of beam-line I711, MAX-lab,
Sweden. The staff of beam-line 14.1 of SRS, DL, UK.
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