Crystallographic Data. 187. Diphenylsilanediol - ACS Publications

Determination of C9 Alkylbenzenes. D. E. NICHOLSON and S. .... silanediol obtained fromethyl alcohol. Principal Lines in. djA. I/Io d, A. I/Io. 12. 10...
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Determination of CS Alkylbenzene' D. E. NICHOLSON and 5. Baytown, Tex.

H. HASTINGS,

Humble Oil 8 Refining Co.,

CS-116 Imfrumenf: Perkin-Elmer Model I 12, CrBr prism Sample Phose: Solution in corbon tetrachloride

Concn, compooent

Cell Windows; CrBr Absorbance Meosuremenf: Calculofion: 0-Propyibenzene

CeHll 10-100

1.3.5-Trimethyl-

CeHlz

10.5

20.42s

0.362

1 0.100

~ _ _ _ _ _ _ _ _ _ _ _ ~ _ _ _ ~benzene_

0-100

_

_

1.2.4-Trimethylbenzene

187.

_

CoHt2

f0.5

~

0-100

CeHlp

benzene

_

P o i n f L

0.100

benzene

1-Methyl?-ethyl-

Bare line-

0-100

19.36~ 0.321

_

iO.5

_

_

~

31.15~ 1.407

~

1 0.100

I"

_

i""el.e matri GraphicalAndy

Relative AI

Componenf/X

m.odp

20.42~

1

1.631 n.nfii

0.100

_

1

_

?

I""

_

1.203

19.36~ 0.475 n.nxo

31.15~ 0.029 n.nz4

22.77~

0.034

n nAx

~

j=O,

Diphenylsilanediol

D. J. NEAL and R. D. BLAUMANIS Research Laborotory, linde Co., Division of Union Corbrde Corp., Tonowando, N. Y.

OH

I

CnHh-Si-GH.

bH Stmcturai r ormula of Diphenylsilanediol

D

is soluble in acetone, ethyl ether, ethyl alcohol, and dimethylformamide. It is nearly insoluble in rater, xylene, toluene, n-heptane, benzene, and carbon tetrachloride. It crystallizes from ethIPHENYLSILANEDIOL

anol in lathlike crystals (Figure 1). It melts with decomposition a t 13741" C.

Indicated Crystal System. Monoclinic.

OPTICALPROPERTIES Refractive indices (daylight filter) :

a = 1.564 f 0.004; p = 1.648 =t0.004; y = 1.656 1 0.004.

Optic Axial Angle. 2V = 43". Optic Axial Plane. 100. Sign of Double Refraction. Negative. Extinction, p A a = 12"; o( A c = 110. Color. Colorless.

ACKNOWLEDGMENT

The diphenylsilanediol described was prepared by the Silicones Division of Union Carbide Corp. CONTRIBUTIONG of crysta4lopraphic data for this section should be sent t o Walter C. McCrone, 501 East 32nd St,, Chicago 16, Iii.

Drincipal Lines in X-Roy Spectrum d , A.

4.40 4.25 4.00

3.85 3.70 3.55 3.45 3.38 3.20 Figure 1. Typicol crystals of diphenylsilonedial obtained from ethyl alcohol

l/Io 8 6 5 7 4 3 6 2 3

d, A.

l/Io

d, A.

3.10 3.05 2.95 2.77 2.75 2.70 2.63 2.46 2.42

3

2.36 2.30 2.22 2.13 2.06 2.02 1.97 1.93 1.80

4 4 2

2 3 '

1 1 3

1.69

1.62 1.59 1.56

1/10 3

a

1 R 1

1 2 1

2

2 1

1

1

VOL. 32, NO. 1, JANUARY 1960

139