88

SHORT

COMMUNICATION

Table I. Crystal data.

C6H3F3: The systematic absences hkl with (h + k) odd and

hOl with l odd indicate space groups Cc (No. 9) or C2/c

C6F6
Laue Class: 2/m
Space Group : P2j/n
a=17.02+0.05 A
b = 9-51 _+0"01
c = 5"84+0"04
,8=91.8+0.3

F.W. = 186.1
F(000) = 540 e
Z =6
D~, = 1"96 g cm -3
Din= 1"88 g c m -3

1,3,5-C6HaF3
Laue Class: 2/m
F.W. = 132.1
Space Group: Cc or C2/c
F(000) = 264 e
a = 9"14+0.04/~,
Z =4
b = 11"90+0.2
D,, = 1"56 g cm -3
c = 6.27 + 0.02
Dm= 1"50 g cm -3
fl = 124.7 + 0.2
(Alternate cell : a = 7"96, b = 11"90, c = 6-27/~,
.8= 98.4 ~, space group lc or 12/c)

(No. 15). Inspection of the Weissenberg photographs

indicates a wide distribution of intensities, suggesting the
centrosymmetric space group C2/c; in this case the four
molecules in the cell must lie on twofold axes parallel to b.
However, the length of the b axis, 11.9/~,, seems inappropriate for such an arrangement. Accordingly, it is quite
possible either that the structure is disordered or that the
intensity distribution reflects only the hypersymmetry of the
molecule, and that the space group is the non-centric Cc.
We are grateful to Dr Sten Samson and Mr Ernest Moore
for assistance in maintenance and operation of the coldroom facilities and to Dr Gary Cristoph for advice and
help in the data refinement.

Discussion

References

C6F6: Our results are in satisfactory agreement with those

of Boden et al. (1973), who report unit-cell dimensions,
measured at 120K, that average about 2 % smaller than
our values. They find that, of the six molecules in the unit
cell, two lie on centers of symmetry while the other four lie
in general positions. Recent infrared (Bertolucci, 1972) and
N M R (Albert et al., 1972) studies are in agreement with the
lack of site symmetry for at least some of the molecules.

ABRAMOWITZ, S. & LEVIN, I. W. (1970). Spectrochim. Acta,

26 A, 2261-2268.
ALBERT, S., GUTOWSKY, H. S. & RIPMEESTER,J. A. (1972).
J. Chem. Phys. 56, 2844-2850.
BERTOLVCCI, M. D. (1972). P h . D . Thesis, California
Institute of Technology.
BODEN, A., DAVIS, P. P., STAM, C. H. & WESSELINK, G. A.
(1973). Mol. Phys. 25, 81-86.

Crystal Data
J. Appl. Cryst. (1974). 7, 88

Crystal data for some mescaline salts, By S. R. ERNST* and F. W. CACLE JR, Department of Chemistry, University of
Utah, Salt Lake City, Utah 84112, U.S.A.
(Received 1 August 1973; accepted 16 August 1973)
Unit-cell parameters and indexed powder patterns are reported for mescaline sulfate dihydrate, hydrochloride, hydrobromide and hydroiodide. Mescaline (3,4,5-trimethoxyphenethylamihe) is a hallucinogenic
substance naturally occurring in the peyote cactus, Lophophora williamsii.

The salts used in this study were prepared from a sample of

mescaline sulfate dihydrate [(CI~HITNOa)2.H2SO4.2H20]
obtained from L. Light and Co. Single crystals of the sulfate
were obtained by recrystailization from water. The hydrohalides (CIIH~7NOa. HX) were prepared from aqueous
solutions of the sulfate by reaction with the appropriate
barium halide (Heffter, 1898). The hydrochloride was
prepared by slow evaporation of water from an aqueous
solution. The hydrobromide grew as large prisms on slow
evaporation of an aqueous n-butanol solution. The hydroiodide grew as needles from an aqueous solution and as
prisms from an ethanol-di-n-butyl ether solution.

They represent least-squares fits of 15 to 22 indexed reflections in each case. Estimated standard deviations are given
in parentheses after each parameter. The data were obtained at 20+ 1 C using Mo Ke radiation (2= 0.710688 A).
The space group of mescaline hydrobromide and mescaline hydroiodide is PT. This was determined by optical
examination of well-formed crystals. Further, refined structures from three-dimensional data (submitted for publication elsewhere) confirmed the centrosymmetric space
group. Neither the hydrochloride nor the sulfate crystals
were well suited to optical examination. From X-ray data
the diffraction symbol 12/mlC. c. was assigned to the hydrochloride, and the diffraction symbol TP. was assigned to
the sulfate.

Crystal geometry

Powder data

The cell parameters shown in Table 1 were obtained from

single crystals by use of a Syntex P I Autodiffractometer.

The powder patterns reported in Table 2 were obtained

with a Norelco powder camera (nominal radius 57.3 mm),
which had been modified to cast fiducial shadows on the
film. The camera had been calibrated with diamond ( a =
3.5667 A), and nickel-filtered Cu K~ radiation (2= 1.5418 A)

Origin of specimens

* Present address: Department of Crystallography, University of Pittsburgh, Pittsburgh, Pennsylvania 15213, U.S.A.

CRYSTAL

DATA

89

Table 1. Crystal data for mescaline salts

(M = CllH17NO3)

M. HC1

Formula weight
(C R = 12.000)

M. HBr

247.72

Habit
a (A)
b
c
~t (o)
fl
)'
Density (measured) g ml-~
Density (calculated) g ml -~
Z
Cell volume (.~3)

M2H2SO4.2H20

339.17

292.18

Tabular
38.763 (22)
5.145 (1)
13.022 (4)
90.00
103.50 (9)
90.00
1.30
1.30
8
2525.3

M.HI

Equant
7-4272 (8)
9.1770 (10)
11.8972 (6)
121-180 (11)
104.186 (12)
92.675 (9)
1.48
1.48
2
657.8

556"63

Acicular
7-511 (2)
9-238 (2)
10-767 (2)
74.97 (3)
72.43 (3)
87-17 (3)
1.63

Tabular
10.605 (2)
13.686 (2)
20-581 (3)

78.05 (3)
82-52 (3)
67.24 (3)
1.37
1.37

1.64
2
687.6

4
2690-7

Table 2. Powder diffraction data

hkl
002
112
003
021 }
020 .
02]211
210
023
212
21]02~
201
220
130
132
213
21~
023
2]-0
231
203
2]-1
230
224
203
233
~12
2]-2
23]134
02~
204
223 J
2]-3
31]135
2~0
241
041
2]-4
314
215
33~
2~3
315
312

dob, A d~,A I/Io

10.15 10.052
5
7.74
7.700
4
6.70
6.701 100
6.249
72
6.25
6.217
5.671 38
5.67
5.258
5"25
5"256 17
5"005
4.933
4"96
4.928 56
4"923
4.806
4.80
4.801 92
4.456
4.432
10
4"43
4"430
4"424
4-20
4"212 26
4"061
4"06
4"058 42
4.055
3"973
75
3"96
3"968
3.850
10
3"86
3"846
3"779
3"778
3"75
3.752
9
3.747
3.747
3"617
3"60
3"603 73
3"597
3.46
3.45863
3"370
3.36
3"355 32
3-292
78
3.29
3"289
3"155
3.15
3.14456
3.017
3.00
3.007 11
2"897
2-891 2"894 17
2.784
8
2.783 2"776

hkl

dobs A dca,c A
9.41
9"423
6"282
6-29
5.93
5"936
5"619
5.62
5"098
5-10
5"093
4"678
4-68
4"199
4.19
4.03
4"033
3"911
3'90
3"878
3"769
3"736
3"74
3"720
3"653
3.64
3"633
3"423
3"42
3"331
3"307
3.32
3"303
3"248
3.25
3"141
3.14
3"017
3"009
3.01
3"003
2.827 2"834
2.690 2"693
2.586 2"591
2.547 2"549
2.481 2"482
2.371 2"375
2.306 2"308
2.238 2"240
2"197
2.196 2"197
2"146 2"145
2"142
2.084 2"082
2"057
822
10,0,(; i 2"054 2"055
1"996
024
31~;
1.993 1"996
1"996
13,1,3
1"990
12,2,0 J
424
1"895 1"897

400
600
40~
202
110 }
602
111
511
112
112 /
511 J"
10,0,0
71][
710
j
312
10,0,2
711
512 }
313
113
204
12,0,0
911 }
204
712
913
14,0,0
713
220
420
913
15,1,]115
023
13,1,2
16,0,~
10,2,]17,1,T

M.HI

M.HBr

M.HCI

M2. H2SO4.2H20

g~
15
91
14
53
30
80
20
37
71
24
42
100
92
61
31
25
24
7
13
11
8
10
17
10
8

15
10
10
17
10

hkl

dob~A d,a, A HA

hkl

dobs A de.it A I/Io

OT1
010
100
1TO
111
101
011

8.82
7.68
7.07
5.81
5"38
5"03
4"86

001
010
011
100
01"1"
111
1T0
110
1]-1
012
102
Tll
021
lit
121
1]-2
1~0
120
122
200
1~1
013
2T1
003
T22
llY
123
2"I"2
030
221
1T3
132
21T
]-31
220
~21
03i"
133
T23
~12
033
]-32
113
~22
0~3
2~3
040

9"92
8"88
7"69
7-12

8.790
7
7.678 30
7.041 15
5.834 95
5"373 11
4"990
9
4"855 33
4"741
110102 } 4"71
65
4"720
4"513 10
02]4"52
121
4-00
3"983 29
122 }
3"809
3"801 65
013
3"81
1!3
3"798
120
3"70
3"714 17
1~2 }
3"652
023
3.64
3"630 35
200
3.52
3"520100
123
3"44
3"456 24
012
3"34
3"346 89
003
3"22
3"220 20
T21
3"109
3-11
120
3-108 11
1~3
3"038
1]-3
3"02
3"023 34
213
3"018
033
2"930
221
2"922 2"920 29
~12
2"919
11~
2-872 2"883 21
131
2"821 2"824 17
132 }
2"752
2T2
2.752 2"746 15
]-13
2"648 2"652 23
13~
2.547 2"551 29
30~
2.433 2"434
7
1]-4 }
2"364
312
2"358 2"360 16
220
2"360
025 /
2-304
2]-3
2"300 2"294 11
04~
2-197
9
225
2"199 2"196
215
2.158 2"158
7
310
2"120 2"123 23
105
2"032 2"034
5

9-921
4
8"918 4
7"685 4
7-157
4
5"920
5"88
100
5"872
5-66
5-669 16
5"49
5"498 16
5"11
5"088 4
4"89
4"902 36
4"807
4"78
52
4"772
4"52
4"524 16
4"17
4"171 10
4"02
4"019 13
3"90 3"878 41
3"84 3"839 41
3"732 39
3.72
3"718
3"58
3"578 69
3"50
3"51018
3"398
3"38
3"37565
3"30 3 " 3 0 7 1 5
3"129
3"12 3"128 27
3"114
3"05
3"054 16
2"973
2"962 2"962 28
2"953
2"833
2"826 2"823 12
2"764
2-7562"749
5
2"674
2"673
16
2"666
2"586
2"579
16
2"584
2"569
2"562 2"562 16
2"561
2"439 2"445
9
2"386
2"386 2"380 10
2"236
2"2342"229
5

90

CRYSTAL

was used for all patterns. The reported intensity values were
measured with a Joyce Loebl Microdensitometer MK III
CS.

Comparison with other results

The interplanar spacings reported for the sulfate are in
general agreement with the two unindexed powder patterns
published by the Joint Committee on Powder Diffraction
Standards.

DATA
Equipment used in this work was provided by the University of Utah Research Fund and by the National
Science Foundation Science Development Grant G U 3866.
One of us (S.R.E.) would in addition like to thank the
National Science Foundation for a Graduate Traineeship,
1966-1969.

Reference
HEFFTER, A. (1898). Bet. dtsch, chem. Gesell. 31, 1193-1199.

J. Appl. Cryst. (1974). 7, 90

Crystal data for tris-(2,4-pentanedionato)indiumOI D, (CH3COCH" COCH3)3|n. By BRUCEW. MCCLELLAND, *

The University of Tennessee-Oak Ridge Graduate School of Biomedical Sciences and Biology Dieision, Oak Ridge National Laboratory,t Oak Ridge, Tennessee 37830, U.S.A.
(Receired 25 June 1973 ; accepted 20 August 1973)
The title compound, prepared by evaporation, is orthorhombic, Pcab, with a = 15.570 (6), b= 16-837 (7),
e = 13.715 (4) /~. It appears to be isomorphous with previously reported forms of the iron(Ill) and vanadium(IIl) compounds.

Origin of specimens
Crystals
of
tris-(2,4-pentanedionato)indium(I I I),
CIsH21In.O6, hereafter In(acac)3, were obtained by the slow
evaporation of cold (2 C) methanol solutions of commercially available material (Eastman Organic Chemicals, stated
melting point 188-190C).

Crystal geometry
Weissenberg and precession X-ray photographs indicated
those crystals examined to be orthorhombic, with systematic absences Okl for l odd, hOl for h odd, and hkO for k
odd; the space group was thus unequivocally established
to be Pcab. Unit-cell dimensions were obtained with the
method of least squares applied to angle data measured for
eight reflections in the range 35< 20< 38 (Mo K~t radiation, 2 = 0.70926 A) on a computer-controlled single-crystal
diffractometer (Busing, Ellison, Levy, King & Roseberry,
1968). The experimental density was determined by the
flotation method. The cell data are as follows:
a = 15.570 (6), b = 16.837 (7), c = 13.715 (4) .&;
U = 3595.3 .A,3; Z = 8 ;
Din= 1.52 (1), Dx= 1.523 g cm -3.

Crystal morphology
The crystals of In(acac)a grew in several habits, including
prismatic, platy, and bladed. Regardless of the habit, one
face usually was observed to be pseudo-hexagonal in shape.
For or~e prismatic and three platy-bladed crystals examined
;* Postdoctoral Investigator supported by subcontract No.
3322 from the Biology Division of Oak Ridge National
Laboratory to the University of Tennessee.
? Operated by Union Carbide Corporation for the U.S.
Atomic Energy Commission.

with X-rays, the diffraction patterns were indistinguishable

and the pseudo-hexagonal face was found to be (010).

Crystal physics
The crystals were observed to be transparent and
low in color. Over long periods of exposure to air,
they gradually decomposed into a white powder.
composition could be prevented by a thin coating
cement applied to the crystals.

pale yelhowever,
This deof epoxy

Comparison with other results

Two crystal forms of In(acac)3 have been identified previously. The/~ form (Barker, 1921) was found by Astbury (1926)
to have the following cell data :t
Orthorhombic, Pn** :
a = 13"4, b = 16.5, c = 8-26 .~ ;
U = 1826 A3; Z = 4 ;
Din= 1"51, Dx= 1"50 g cm-3
Another form studied goniometrically by Jaeger (1914)and
later classified as 7 by Barker (1921) was found to be
orthorhombic with a/b=0.5593 (where c is normal to a
crystal face that was observed to be pseudo-hexagonal in
shape). For the form of In(acac)3 reported herein a/2c=
0.5676, so that it may be the same form observed by Jaeger
(1914).
Two other tris-(2,4-pentanedionato)metal(llI) structures
which conform to space group Pea& Fe(acac)3 (Roof, 1956;
"~" The cell edges given by Astbury (1926) have been transformed to conform to the rules of Kennard, Speakman &
Donnay (1967) and converted to A with the conversion factor
I k X = 1.002063 A (International Tables .for X-ray Crystallography~ 1962). Values of U and D., were not included in Astbury's report and have been calculated from the converted
cell dimensions.