CRYST AL STRUCTURE OF 110

EZCURRITE

The Crystal Structure of Ezcurrite

Euo A. DAL NEGRO, AND LUCIANO UNGARETTI, Centro di Studio del
CANNILLO,
C. N. R. per la Cristallografia strutturale, lstituto di Mineralogia dell'Universita
di Pavia., Italy

Abstract

La estructura cristalina de ezcurrita, un borato hidratado con fórmula química 2Na2O· 5B,Oa ·7H,O, se ha resuelto mediante
el uso de métodos directos. Los datos tridimensionales de Weissenberg (reflexiones de 1974) dieron un factor R final de
0,050. Los parámetros de la red son: a = 8.598, b = 9.510, c = 6.576 A, cada uno± 0.002; a = 102°45', (3 = 101°30', 'Y =
71°31', cada ± 3'. Grupo espacial Pi. La estructura cristalina de ezcurrita contiene [B,OlOH),]2- polianiones unidos entre sí
para formar cadenas a lo largo de c. El polianión está formado por dos anillos de boro-oxígeno de seis miembros, uno
formado por dos tetraedros y un triángulo, el otro por dos triángulos y un tetraedro. Por lo tanto, la fórmula estructural de
ezcurrita es [Na,B,Q7COH)al • 2H2O, Las cadenas están unidas entre sí por los Na-poliedros y por una red de enlaces de
hidrógeno.
Introducción La estructura se resolvió mediante el uso de métodos
Esta investigación de la estructura cristalina del ezcurita, 2N O
directos. La determinación del signo se llevó a cabo
·5B2O3· 7H2O, es parte de un estudio sistemático de minerales mediante la aplicación de las relaciones de Sayre a
de borato hidratados (Dal Negro et al., 1969, 1971). Ezcurrite 374 reflexiones con normalizado structure factors JEJ
fue descrito como un nuevo ministro por Muessig y Allen > 1.30. Todo el proceso se realizó utilizando un
(1957) y reestudiado por Hurlbut y Aristarain en 1967. Christ programa informático escrito por R. E. Long (1965).
(1960) propuso para ezcurrite un polianión [B5O6(OHh]2-
formado por dos tetraedros y tres triángulos. La ocurrencia y las
En el mapa F0 calculado con las fases derivadas del
propiedades químicas y físicas de este mineral fueron descritas conjunto con, el índice de consistencia más alto, fue
completamente por Hurlbut y Aristarain; No se realizó ningún posible encontrar un número de máximos
análisis químico ni determinación de los parámetros de la celda correspondientes a los átomos de sodio y oxígeno. Las
unitaria en la muestra utilizada para este trabajo. sucesivas síntesis tridimensionales de Fourier,
Experimental calculadas sobre la base de estas coordenadas, dieron las
coordenadas de todos los átomos no hidrogénicos en la
Se estudió un fragmento incoloro de ezcurrita de 0,11 X 0,26 X 0,64
unidad asimétrica. Se calculó un factor R de 0,19 a partir
mm de la mina Tincalayu, Salta, Argentina, alargado a lo largo de
[001]. Los datos cristalográficos relevantes tomados de Hurlbut y de estas coordenadas. Esto se redujo a 0,095 después de
Aristarain (1967) son: Pi; a = 8,598, b = 9,510, c = 6,576 A (cada ± tres ciclos de mínimos cuadrados llevados a cabo con el
0,002); a = 102°45', (3 = 107°30', 'Y = 71°31' (cada uno± 3'); V = programa informático ORFLS de Busing, Martin y Levy
484,7 A•; contenido celular Na,[BsO7(OH),h·4H,O; gravedad (1962), utilizando las curvas /-para átomos neutros de
específica 2.049 (calc), 2.053 (meas). Las fotografías integradas de Na, 0 y B dadas por Hanson et al. (1964) y parámetros
Weissenberg se tomaron utilizando radiación CuKa y múltiples térmicos isotrópicos. En esta etapa se alcanzó la
paquetes de película a medida que el cristal giraba alrededor de su eje
convergencia isotrópica y se introdujeron parámetros
c. Se aplicaron correcciones de polarización de Lorentz y duplicación
de puntos a1-a2 a las intensidades medidas fotométricamente, pero no térmicos anisótropos. Después de dos ciclos, el factor R
se realizó ninguna corrección para la absorción (μ = 25,5 cm-1). se redujo a 0,06. Se calculó una síntesis de Fourier de
Dentro de la esfera limitante de CuKa, se recogieron reflexiones diferencia tridimensional, dando ciertos máximos que
independientes de 1974 o aproximadamente el 90 por ciento de los podrían asignarse razonablemente a los átomos de
2198 presentes. De estos, 893 eran demasiado débiles para ser hidrógeno; Sin embargo, el número de estos picos fue
medidos con precisión y se consideraron no observados. mayor que ...
Structure Analysis
110
 CRYST AL STRUCTURE OF 111
EZCURRITE
TABLA 1.Ezcurrite. Atom.io parámetro■ con su
r ocn
desviación etandard■ entre paréntesis y equivalente
ieotrópico tnperatu.re tac tor• según Hamilton (1959),
Atom !I ll.2 !I 9iic.F>

Na(1 0,8988( 0,3700(2 1,0373( 3) 1,81

) 2) ) 8C4./HC3)
Na(2 0,5860( 0.1519(3 0,5616(4) 2.88
)
0(1)
3)
0,1756(
)
0,2244( 3 0,2169(5) 1,17
o<s>' /Jfjjoc9)
4) )
0(2) 0,4110( 0,0118(3 0,2130(5) 1,35
4) )
o.1510(3 >.

'\;o,.,
O(J) 0,2982( -0,0867( 5 1,02
4) ) . 0(7)

'cr
0(4) 0,4508( 0,2564( 3 0,2527(5) 1,34
4) ) 03
0(5) 0,5666( 0,4476(4 0,2676(5) 1,94 '
4) )
0(6) o.3627( o.3865( 3 -0,0474(5) 1. 34
4) )
0(7) 0,0778( o.3727( 3 -o.1868( 5) 1,21
4) )
0(8) 0,2846( 0,2489( 3 -o.3991 ( 5) 1, i8
4) )
0(9) - 0,4156(4 -o.3508 ( 5) 2,00
0,2072(4) )
0(10 - o.3259(4 -0,5695(5) 1,47 Fm. 1. Projection of the unit BsO?(OH)a on the (100)
) 0.0113(4 )
) plane.
0(11 0,8265( 0.0547(5 0,4041(5) 4.07
) 5) )
0(12 0,8261( o.1440(6) 0,9732( 12) 1,28
)
B(1)
nected to form chains
7)
0,16-
along0,1463(81
c; two equivalent
1,05
chains are present in a single unit cell (Fig. 2). The
0,3333(
7) 08(61 [B5O7(OH)a]2- group is formed by two six-mem
B(21 0,2566(0,2850(6 -0,1777(8) 1, 12
bered boron-oxygen rings joined through a common
tetrahedral boron. One of the rings consists of two
structure factor calculation with isotropic tempera triangles B03 and B02(0H) in addition to the cen-
ture factors equal to 3.0 for those belonging to the
hydroxyls and 5.0 for the hydrogens belonging to
the water molecules. This reduced the R factor to
0.05 for the observed reflections. All the observed
structure-factors were weighted equally during the
refinement.
The final position parameters are listed in Table
1 and the observed and calculated structure factors
are compared in Table 2.1

Description and Discussion of the Structure

The main feature of the crystal structure of
ezcur rite is the [B5O7(OH)s]2- unit first found in
this structure (Fig. 1). These structural units are
con-

1
To obtain a copy of Table 2, order NAPS Document
01978 from Microfiche Publications, Division of Microfiche
Systems Corporation, 305 East 46th Street, New York, Fm. 2. Clinographic projection of the crystal structure
N. Y. 10017. Please remit in advance $1.50 for microfiche of ezcurrite; the polyanions link together to form chains
or $5.00 for photocopies. Check the most recent issue of along c.
this journal for the current address and prices.
 CRYST AL STRUCTURE OF
EZCURRITE
TA.BL& le ijing Mglea,plan.H and d,rviatione trOtll plA11afit:y tn •=-ew-r.ite1
Equation!{'of plane through thr•• oxygens in the form A! + Bi + C.!, • D
112
TABLE 4. Boron•Oxygen,Boron-Boron diat1111cee and Oxygen-Boron-Oxygen ,.ngles
"1tb their etandard deviations in parentheses.

Ring 1 A B C D
8(1)-0(1)
11(1)-0(2)
1.468 (6)
1.472 (6)
1 B(2)-0(J)
B(2)-0(6)
1.431 %
(6)
1.495
(6)
B(1)-0(4) 1.491 (6) 8(2)-0(8) 1.494 (6)
Ring 2
0(7)'-0(6)-0(10) 3. 6254 9.4904 -2.0046 2.1891 A.Yare.ge 1.477
Avenp 1.472

Ancl• between plan•• 11 2 82•, 26

8(3)-0(4)
8(3)-0(5)
1.322 (6)
1.383 (6)
1 8(4)-0(7)
B(4)-0(9)
1.365
(6)
%
1.345
(6)
Ring Atom Deviation tt'oa plane (l)

B(1) 0.504 (5) Average 1. Avera«• 1.

B(2) -0.668 (5) 35 36
8(3) 0.947 (5) 9 0
8(2) -0.202 (6) 8(5)-0(1) 1.336 (6)
B(4) -0.095 (6) 1
Ancl••
. .B(5)

0- 0 andB-0-B internal to the ringll.

0.037 (6)

81114 1
8(5)-0(8)
8(5)-0(10)
1. 349 (6)
1.415 (6)
Ring 2

B(1)-8(2) 2.4a3 <1> l 8(2)-8(4) 2.511 (7) 1

Ring Atome Angle■ B(1)-B(3) 2.454 (7) 8(2)-8(5) 2.512 (7)
8(2)-B(J) 8(4)-8(5)
,,,......
8(2)-0(3)-8(1) 118•.5 2.480 (7) 2.395 (6)
0(3)-8(1 )-0(4) 109•.5
8(1)-0(4)-8(3) 121•.2 2.472 Averac• 2.472
0(4)-8(3)-0(6) 123•.1
8(3)-0(6)-B(2)
0(6)-B( 2 )-0( 3)
119•.7 Betwoc riD&II 1,2 B(1)-B(5) 2.515 <8> l
112•.2

mean value 111•.4 0(1 )-8(1 )-0(2) 107•36' (22•) 0(3)-8(2)-0(6) 112•12• (2J')
0(1)-1(1 )-0( 3) 110•20• (22') O(J)-B( 2)-0( 7) 111•39• (23•)
8(2)-0(7)-8(4) 121•. 7 0(1)-1(1 )-0(4) 109•3()• (22') 0(3)-8(2)-0(8) 110• (2J')
0(7)-8( 4)-0(10) 121•.3 0(2)-8(1 )-0(3) 110•24• (22') 0(6)-8(?)-0(7) 105•40• (23•)
8(4)-0(10)-B(5) 120•.1 0(2)-8(1 )-0(4) 109•22• (22') 0(6)-8(2)-0(8) 107•36• (23')
0(10)-B(5)-0(8) 120•.o 0())-1(1)-0(4) 109•32• (22') 0(7)-8(2)-0(8) 109•31' (23')
8( 5 )-0( 8)-B( 2) 124°.,
0(4)-B(3)-C)(5) 111•411,• (25') 0(7)-8(4)-0(9) 115• 5' (24')
0(6)-B(2)-0(7) 109•.5
o< 4>-•o >-o< 6 l 123• 3' (26') 0(7)-8(4)-0(10) 121•17• (25')
mean value 119•.5 Of5 )-1())-0(6) ,,,. <25• > 0(9)-8(4)-0(10) 123•37• (2'')
!/ ,.;£,.! are the atomic coordinatea(l)referred to the cryetallographic a•
0(1)-8(5)-0(8) 121•54• (25')
axu: and D ia the dietance ot the planes from the origin(l). 0(1)-8(5)-o(lO) 113• 2/ (22')
0(8)•1(5)-o(I0) 120' 2' (24')

tral tetrahedron, while the other is formed by one TABLE 5. Oxygen-Oxygon distances within the S-0 Polyhedra in Ei:cu.rrite.
tetrahedron B03(0H) and one triangle B02(0H) Tetrahedron around B(1) Tetrahedron around 8( 2)
in addition to the central tetrahedron.
According to the fourth rule of Christ (1960), the 0(1 )-0(2) 2.313 <4> 1 o(J)-0(6) 2.429 <4> !
borate chain in ezcurrite may be considered as 0(1)-0(3)
0(1)-0(4)
2.402 (4)
2.-417 (4)
0(3)-0(7)
0(3)-0(8)
2.417
2.)96 (4)
the first polymerization product of the still unknown 0(2)-0(3)
0(2)-0(4)
2.406 (4)
2.418 (4)
0(6)-0(7)
0(6)-0(8)
2.379 (4)
2.412 (4)
iso lated unit [B506(0H)5]2-, whereas the well- 0(3)-0(4) 2.409 (4) 0(7)-0(8) 2.437 (4)

known [B508(0H)]2- sheets found in Averq■ 2.404 Average 2.411

Kz[B50s(0H)] ·2Hi0
(Marezio, 1969) in veatchite (Clark and Christ,
1971) and in gowerite (Konnert et al., 1972) rep Triangle arc,w,d B( 4)
Triangle around B(3)
resent the second step in the polymerization process.
The ezcurrite polyanion and the [B508(0H)
J 2
-
0(4)-0(5) 2.311 0(7)-0(9)
unit are similar, both being built of the same two the 0(4)-0(6) 1
C4> 0(7)-0(10)
0(5)-0(6) 2.36 0(9)-0(10)
six-membered rings. In ezcurrite, the mean planes pla 8 (4)
2.374
of the two boron-oxygen rings are almost perpendic ne Average
(4)

ular, with an angle between the planes of 82.3 °. 2.353

Within the two six-membered rings, the internal B-B
distances are nearly equal (2.472 A is the mean Trian
value for the ring 1 and 2.473 A for the ring 2). gle
aroun
The first ring formed by 0(7), 0(8), 0(10) is 0(1 )-0(8)
0(1)-0(10)
2.401 (4):.
2.295 (4)
d
5)
practically planar with a mean value for the 0(8)-0(10) 2.394 (4)

internal angle of 119.5°, the greatest distance from 2,363

 CRYST AL STRUCTURE OF 113
2.3oj (4) A EZCURRITE
2.383 (4)
2.374 _(4)

2.353
 CRYST AL STRUCTURE OF 114
EZCURRITE
being -0.20 A (Table 3). In comparison, the sec
TABLE 6. Sodiua coordinatee in Ezc\U't'ite.
ond ring built up by O(3), 0 (4), 0 (6) is less
planar; the mean value for the internal angle is Oxygen atM Ooord.inates of oxygen atrm:/ Na(1 )-0 di■tance(l)

117.4° and the greatest deviation from the plane is

0(1) 1. 1755 0,224 1.2169 2,436 (3)
+0.95 A. The polyanions link together to form 0(6) 0,6373
4
0.613 1.0474 2,681 (4)
chains with an angle B(5)-O(1)-B(l) of 127.5° o(t) 1,0778
5
0.372 0.8132 2,438 (4)
7
and a separation B(5)-B(l) of 2.515 A. The B-O 0(7') 0.9222 o.627
3
1,1868 2.489 (4)
o.7928
distances in the ezcurrite polyanion (Table 4) are 0(9) 0,415
6
o.6492 2.,2, (4)
0(10) 0.9887 o.325 1,4305 2,557 (4)
in good agreement with those found in the 0(12) 0.8261
9
0.144 0,9732 2.355 (6)
literature for other borates. The mean B-O bond 0

length is Na(2)-0 di ..
once(1)
1.475 A for the tetrahedral boron and 1.362 A for 0(2) 0.4110 0.011 0.2130 2,676 (4)
triangular coordination. However, appreciable devia 0(2') 0.5890
8
- o.7870 2,373 (4)
0.01
tions from the average indicate that the B-O poly 0(4) 0,4508
18
0.256 0,2527 2.284 (4)
hedra are somewhat distorted. The O-B-O angles 0(8) 0.2845
4
0,248 0,6009 2,533 (4)
9
fall within the expected range (Table 4), as do the 0(11) 0.8265 0,054
7
0.4041 2.420 (5)

0-0 distances (Table 5). 0(12) 0.8261 0,144

0
0.9732 2,868 (6)

There are two independent sodium atoms in the

ezcurrite structure (Fig.3), one being six-coordinated
and the other seven. The sodium cations bond to the
oxygen anions in two different centrosymmetrically
related borate chains. Moreover, each Na-polyhedron
shares an edge with another Na-polyhedron
and the centrosymmetric pairs so formed link to
gether through the vertex 0(12) to form Na-O
chains running along [111].
The two water molecules in the asymmetric unit
II Sodiw:a atom• at J,Z,! in Table 1,
are bonded only to the sodium atoms. In particular
the water molecule 0(11) is linked to Na(2) while
0(12) connects the two independent Na-O poly
hedra. The Na-O bond lengths range from 2.281
to 2.858 A (Table 6). It has been possible to single
out the hydrogens belonging to three hydroxyls (but

Na
l

i
I 1lft1'

01

FIG. 3. Details of the projection on the (.001) plane

showing the Na-0 chains.
 CRYST AL STRUCTURE OF 115
EZCURRITE
Fm. 4. Projection on the (001) plane showing the
hydro gen bonds.
 CRYST AL STRUCTURE OF 116
EZCURRITE )
0,088( 0,1]4(
0
4 4 1 4 8 1
'?ABLE 7. Di■tucu Nla.ted to the hydrogen bonde in Ezcurriui. 8) 6 5 ) 8) 7 9 4
0,116( 9 0,202( 6
7) 8 1 1 6) 1 1 7
Dooo.,!/ H;tdro«en tteceptor Coordinatee of receptor dietance o.152( 4 )
4
2
0 0,)10( 1
0
7
6
9
6) 6)
B 1 1 8 0( 1 8 1
0,101( 0 7 ] 10 0,1]1(1 3 1 1
(S 5 ] ) 0) 4 4
0(2) H(1} o(j) 0.10:i -0.151 o.o87 1.01 A 2.15, <4> A 7)
0(5) H(2) 0(6) o.637 0.613 o.on o.................... 2.672 (0 l 0,127(
5 9 5 0.266( 1 8 2
2 2 6 2 6 7
0(9) H(}) 0(5} -0.-434 0.448 -0.112 0.95 2.68J (4) 7) 7) ]
0.158( 1 9 ) 0,435( 1 1 7
0.111) H(-4) O(J) 0.102 -0.151 u.oe1 1.01 2.r;o (5)
3 5 4 1 7 7
6) 8)
o.c,2> H(5) o(,) o.">89 -0.012 0.787 0.9) 2.739 (6) 7 7 0
0 0,085( 1 6 1 0( 1 1 1
( 8) 1 9 2 11 4 1 0
1 o,116( 5
,
9 ) 1 5 7
t/ Dcnor a tom■ ta.kn et l•U! in To.ble 10 )
7) 2 7 1 1 3 8
0.135( 9 3 ) 1 9 2
6) 7 0
1 1 1 5 6 1
0 5 0 8 1 6
4 3 3 1
0 6 1 6 0( 1 1 9
only one hydrogen for each water molecule). On the (
2
1 2
5
9 12
) ] ]
3
)
other hand there are only two 0-0 distances less 2
8
4
4
1
1
8
1
1
8
4
8
1
1
than 3.1 A involving the two water molecules, sug 8 1
7
1
1
5 e
]
1
gesting that two hydrogens do not form hydrogen 5 1
2
4
4
7 9 5
6

bonds. Each B-O chain links to four other chains O

(l)
1
2
5
8
5
1
2
5
through the hydrogens belonging to the hydroxyl 7
7
1
1
9
1

groups. The chain (Fig. 4) formed by the polyanion 1

4
1
0
3
5

with atomic coordinates x, y, z of Table 1 is con

1 0

!/Root mean square thennal. vibrations aloD.B the ellip■oid u:ea(X) and
nected to two centrosymmetric chains through pairs angles
of centrosymmetric hydrogen bonds. Two other { 0) between the crystallographic axes and the principal axes (U ) of the
vibration ellipsoid.
chains, related by translations along a and c ( atomic
coordinates 1 + x, y, l + z and x - l, y, z - l),
are linked to the first chain through one distinct
hydrogen bond. In this way there is a thick network

TABLE 8. Analysis of the anisotropic thermal parameters

in ezcurrite•

Atom Atom

T< 0.127( 1 8 129 0( 0,092( 1 9 1

o( 4) 2 1 120 4) 7) ? 6
1 0.162(1 1 ] o. 120( 0 1 ]
I 2) 4 2 7) 6 8 1
C.162(1 2 o.167( 0 1
1) 1
5) 9
0.115( 5 1 1 0,102( 1 7 5
4) 8 1 2 8) 3 2 5
o.183( 4 9 0.12>( 4
N 4) 1 6 1 0( 7) 1 1 1
a( 0.250( 0 5 4 5) 4 1 0
2) 2 2 0,220( 3 8 ]
3) 1 7 1 5) 6 1 1
0.090( 3 0 ? 0 8 1
0 0,093( 9
1])
9 1 1 8) 1 6 5
o.120( 5 4 0 0,110( 2 5 2
11) 7 9 7) ]
B 0.1]] 8 1 4 0( o.174( 1 1 1
( (11) 6 ) 8 6) 4 2 0
1 6 5) 2 3 1
) 0.088(1 0,062(1
J) 1 7 4 1) 8 ] 1
0,122(1 1 0 1 8 7
9 0.125( J
1) 6) O
o.141 ( 1 1 9 o.162( 1 7 4
5 2 1 2 5 2
11) 6)
0 6 7
B 0.114(1 1 6 77 0( 0,078( 1 6 1
( 1) ] 67 7) 9) 2 8 2
2 0,125(1 , 4 0,127( 1 7 0
) 1) 5 9 6) 1 2 ]
0,142(1 ; o,151 ( 1 6
0) 4 5
6)
6 5 1 1 1 7
0,114( 5 1 5 0,087( 3 5 2
9) 4 8) 7 1
B 0.117(1 1 9 9 O( 0,1 ]]( 1 7 1
( 1) 5 6 1 S: 7) 0 4 4
J 0,128(1 9 4 4
0,'25(
) 0) 5)
7 1 1 2 ' 1
0,070(1 4 ] 1 0,10]( 9 9 2
5 1 5
7) 7)
7 1 1 1 1 8
0,10) 6 0 5 o.12]( 1 6 8
(11) 2 4 5 4
7)
B 0,144(1 1 8 1 0( 0.17]( 1 8 1
( 0) ] 2 1 9) 6) 6 2
4 5 J 3 0
 CRYST AL STRUCTURE OF 117
EZCURRITE
of hydrogen bonds which provides the connections
among the polyanions and, through the water mol
ecules, among polyanions and Na-polyhedra. The 0-
0 distances involved in hydrogen-bonding and the
0-H bond lengths are listed in Table 7.
Analysis of the anisotropic thermal parameters
(Table 8) reveals that the thermal anisotropy of the
atoms in ezcurrite is not large except for Na(2)
and the water molecules. Taking into account the
great anisotropy of Na( 2) with respect to Na (1 ),
the strong thermal motion of the 0(12) water mol
ecule can probably be explained as interaction be
tween 0(12) and Na(2), the major axis of the
ellipsoid of thermal vibration for both atoms being
localized along the bond direction.
Considering electrostatic balance, values ranging
from 1.90 to 2.10 valence units are found for each
oxygen atom on the basis of the correlations be tween
bond length and bond strength given by Zachariasen
(1963) for B-0 and 0-H ... 0 bonds.
Strengths of 1/7 = 0.142 and 1/6 = 0.166 valence
units have been assigned to each oxygen atom co
ordinated to Na(l) and Na(2), respectively. One
proton for each water molecule does not appear to
form any hydrogen bonds, and for this reason a
1.0 valence was assigned to it.

Acknowledgments

We are much indebted to Messrs. R. D. Erd, U. S. Geological

Survey, and A. Valenti, mineral-collector, Los Angeles,
California, who made possible this investigation by sending us
some fine specimens. We also want to thank Dr. J. R. Clark,
U. S. Geological Survey, for helpful dis cussions and
suggestions on borate crystal chemistry.

References

BUSING, W. R., K. 0. MARTIN, AND H. A. LEVY (1962)

0RFLS, a Fortran crystallographic least-squares program.
U.S. Nat. Tech. Inform. Serv. ORNL-TM-305.
CHRIST, C. L. (1960) Crystal chemistry and systematic
classification of hydrated borate minerals. Amer. Min eral.
45, 334--340.
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