17%
Vol 65
C'OMMZTNICAI'IONS TO THE E D 1 I OK
cyanate and isocyanate, but it iz not known which of these was produced. Anal. Calcd. for Ge(0CN)r: Ge, 30.17 Found: Ge, 30.35. Germanium (1so)cyanate is a colorless liquid which rapidly hydrolyzes to germanium dioxide. A vapor pressure study, using the isotensiscopic method already described,s showed that thermal decomposition occurs slowly above 140'. The equilibrium vapor pressure values for the range 35 to 140" are expressed satisfactorily by the equation
p. (extrapolated), 196"; molar heat of vaporization, 12.6 kcal.; rn. p. - S o ; density 2.1' (pycnometric), 1.7694; ?'''ID 1.4793. B.
(3) Laubengayer and Carey J Phrs Chem , 30, 1045 (1936)
Two New Thionacetophenetides o-Thionacetophenetide was prepared in 26% yield by adding 18 g. of o-ethoxyphenyl isothiocyanate in ether to methylmagnesium iodide, from 32 g. of methyl iodide, 9 g. of magnesium turnings and 90 ml. of dry ether, refluxing for three hours, hydrolyzing and recrystallizing the resulting solid from 25% acetic acid, m. p. 70-71'. Anal. Calcd. for C ~ O H ~ ~ N O N,S7.17; : S,16.42. Found: N, 7.01, 7.14; S, 16.62, 17.34. m-Thionacetophenetide was prepared in a similar manner and melted a t 89-90", Anal. Found: h', 6.90, 7.09; S, 17.26, 16.53. We also prepared and analyzed p-thionacetophenetide and our melting point agrees with that of recent workers' rather than with that of Sachs and Loevy.2 (1) Warrail, T H I S J O U R N A L . 46, 2838 11921); Kiprianos. S u i t n i k and Suich, Cheni d b s . . 30, 4863 (1936). J . Gen. Chewz. (I;. S. S. R . ) , 6 , 42.-!) (1936). ( 2 ) Sachs and Loevy. Ber., 37, 876 (1904).
DEPARTMENT OF CHEMISTRY SCHOOL OF CHEMISTRY UNIVERSITY A W. LAUBENGAYERRUTGERS CORNELL UNIVERSITY LOCISE. PERLGUT ITHACA, N Y. LESLIERECGEL NEWBRUNSWICK, N. J. D. L. COTTLE RECEIVED APRIL17, 1943 RECEIVED JULY 12, 1943
COMMUNICATIONS T O T H E EDITOR LONG X-RAY DIFFRACTION SPACINGS OF THE JSERATINS
idional arcs together. This is unavoidable a t present with porcupine quill patterns, since promSi7: inent large-spacing (83 layer-line components Recently, with techniques previously employed cannot be resolved satisfactorily, except on the to determine the large fiber-axis period of collagen equator, because of lateral diffuseness and lack of (640 A.),l the following data were obtained for perfect orientation. The situation is better with porcupine quill (CY)and feather (P) keratins. feather, whose patterns show a strong, easily resolved row line indicating an important 34 A. RIERIDIONAL AND NEAR-MERIDIONAL REFLECTIONS spacing transverse to the fiber axis. Porcupine quill tip beather rachi, 1 I1 1I1 1 II I11 In meridional directions on the patterns of both (,ti ,i 198 23 c 4 94 4 materials sharpness facilitates good resolution. 49 1 19h 11 9 8 95 2 The third order of porcupine quill and the fourth 39 5 195 I O 45 9 94 1 of feather are strongest and innermost in each 7 198 ij31 15 Y45 27 4 24 5 Y 19tj 5 .53 17 94 1) case, and probably represent important structural 22 ( J 9 198 4 98 19 94 ti features in the directions of the fiber axes. 4 45 21 93 5 19 8 10 198 The evidence clearly indicates fiber-axis periods 18 06 11 197 8 Layer-line reflections 15 2 13 198 with k values of 2 and 4 of 198 and 95 A,, respectively, for porcupine quill and feather. On the eve of publication of these IJ 2 17 197 t u 13, inclusive, have 12 36 16 197 8 been observed on the conclusioiis MacArthurL reported that periods of LO 40 I9 197 h feather pattern5 either 198 or 658 A are possible for porcupine I, Bragg :pacing, 1x1 A , 11. order n o , k , 111, k time> quill, although the larger figure was favored and \pacing, 111 A ha5 been the only one anticipated previously The low values listed iii several instances re- I t is impossible to deny categorically that periods ( 2 ) 1 MacArthur, Nature, 169, $8 (1943) sult from considering meridional arid near-mer
A.)
(11
H S Bear.
IHrs lorrHNAr,
64, 727 (19421
\ 01
3) See W T Astbury, p p 88-96 in "Advances in hnzymology ' 111 Interscience Publishers Inc New York N Y 1943
