ALBERT

Notes: Summary Nine healthy young volunteers received diets furnishing from 5 to 10 eggs (1.03–2.06g egg cholesterol) per day through two consecutive periods of 3 weeks. The amounts of proteins and fat per 100 calories were the same in all the diets. Immediately before, and 3 and 6 weeks after beginning of the egg regimen, samples of duodenal bile were collected, after injection of cholecystokinin, and analyzed with respect to pH, dry matter, cholesterol, lipid-soluble phosphorus, glycocholic acid, glycochenodeoxycholic acid, glycodeoxycholid acid, taurocholic acid and taurochenodeoxycholic plus taurodeoxycholic acids. Simultaneously with the collection of bile, blood samples were taken for determination of serum total cholesterol. The main results were as follows: Serum total cholesterol increased during the egg regimen. In the bile no great changes occurred in the distribution of the different bile acids in the total bile acids. The predominant change of the ratios between total bile acids and cholesterol and between lipid-soluble phosphorus and cholesterol was a slight to moderate increase. Thus, the results did not provide evidence for a lessening of the solubility of cholesterol in the bile in spite of the fact that serum cholesterol increased.

Notes: Summary With the further purpose of studying the influence of diet and pharmaca on human bile, the composition of duodenal bile from 42 healthy young volunteers (group V, 7 men, 35 women) was compared with the composition of bladder bile from 27 peptic ulcer patients without diseases of the biliary tract and liver (group A, 17 men, 10 women), and with the composition of bladder bile from 26 patients having uncomplicated gallstone disease and functioning gall bladder (group B, 4 men, 22 women). Generally, the duodenal biles had lower concentrations of the components determined (dry matter, cholesterol, lipid-soluble phosphorus and bile acids) than had the bladder biles, especially those in group A. The mean value of the molar ratio between glycine-conjugation and taurine-conjugation was somewhat lower in group V than in groups A and B. The mean value of the ratio between total bile acids and lipid-soluble phosphorus was almost the same in groups V and A, and higher than in group B. Comparison of the individual values of the ratio between lipid-soluble phosphorus and cholesterol with yet unpublished studies of the solubility of cholesterol in aqueous solutions of lecithins and bile salts suggests that roughly half of the biles in all three groups would be supersaturated with respect to cholesterol if the solubility of cholesterol in bile depends only on the components determined in the present study. The fatty acid composition of bile lecithin was determined in 23 cases from group V, 16 cases from group A and 13 cases from group B. The distribution of the fatty acids was almost the same in groups A and B as in 17 cases in group V, in which less than 10% lysolecithin was formed during collection of the bile samples.

Notes: Summary Seven healthy young volunteers received daily doses of cholestyramine (ca. 0.4 g „Cuemid“ per kg body weight) through two consecutive periods of 3 weeks. Duodenal bile was collected, after injection of cholecystokinin, twice before and 3 and 6 weeks after beginning of the treatment. The bile samples were analyzed with respect to pH, dry matter, cholesterol, lipid-soluble phosphorus, glycocholic acid, glycochenodeoxycholic acid, glycodeoxycholic acid, taurocholic acid and taurochenodeoxycholic plus taurodeoxycholic acids. Simultaneously with the collection of bile, blood samples were taken for determination of serum total cholesterol. Compared with the respective mean values before beginning of the treatment, the predominant changes were as follows: Serum total cholesterol decreased. In the bile, the molar ratio between dihydroxycholanoic acids, and trihydroxycholanoic acids decreased markedly, and the molar ratio between glycine-conjugation and taurine-conjugation increased. These changes were due to drastic increase of the molar percentage of glycocholic acid and more or less pronounced decreases of the molar percentages of the other bile acids in the total bile acids. The mean values of the molar ratios between total bile acids and cholesterol and between lipid-soluble phosphorus and cholesterol were slightly to moderately decreased. Thus, the results have not provided evidence for an increased solubility of cholesterol in the bile as a consequence of cholestyramine treatment, but rather point in the opposite direction, although further data are necessary before a decisive conclusion can be reached.

Notes: Summary Recently,Weihofen andPringle compared, by means of „Z-scores“, the heights and weights of 36 children with cystic fibrosis with the heights and weights of 30 „normal“ children, finding that indeed the sick children were both significantly shorter and significantly lighter than healthy ones. However, it would be expected that this be the case, and for that reason, we ask and answer, by means of multivariate statistical theory, whether the height-weight growth in normal children has been not just retarded, but distorted. That is, if growth has been retarded, as could be the case with any ill child regardless of the illness, he could possibly recover what he has lost more readily if his growth is uniformly retarded, as a prematurely born infant can reach full height-weight proportions. Of course, we define mathematically exactly what we mean by the term „distortion“. Next, we correct several calculation errors ofWeihofen andPringle and point out the necessity of publishing the raw data. That is, we wrote Mrs.Weihofen for the original data for normal children and were told that she „must have discarded“ it. Since not all data is available, it cannot be reviewed for accuracy, and we must make an approximation, which we explain, in order to apply our multivariate statistical procedure. However, we do not feel that the approximation will seriously affect the results, and, in any case, it affords an opportunity to demonstrate the method.

Notes: Zusammenfassung Eine Analyse des Zuckerverbrauchs in der BRD und der CSSR zeigt, daß der Unterschied im Verbrauch von etwa 6 kg je Kopf und Jahr auf den Verbrauch in Haushalten — Zuckereinkauf — zurückzuführen ist. Das geht aus Versorgungsangaben und Daten der Wirtschaftsrechnungen hervor. An zuckerreichen Erzeugnissen wird in der BRD nur ein höherer Verbrauch an Schokolade und Süßwaren festgestellt. Der ernährungsphysiologische Aspekt ist für die Beurteilung des Verbrauchs konsequent zu verfolgen. Ein hoher Zuckerverbrauch hat eine negative Auswirkung auf die gegenwärtig erwünschte Ernährung. Sie zeigt sich besonders in dem als Folge eines höheren Zuckerverbrauchs bedingten reduzierten Verbrauch an biologisch wertvolleren Lebensmitteln. Die Preise von Zucker und zuckerreichen Erzeugnissen sind in der BRD niedriger und können nicht eine Hemmung der Steigerung des Zuckerverbrauchs bedeuten, ebenso wie die relativ, im Vergleich mit anderen Positionen des Nahrungsmittelverbrauchs, langsame Erhöhung des Zuckerpreises. Demgegenüber kann die Preisentwicklung in der CSSR als einer der Faktoren des steigenden Zuckerverbrauchs bezeichnet werden. Beschriebene Unterschiede im Verbrauch finden einen Rückschlag im Nährwertgehalt des Lebensmittelverbrauchs, in seiner Zusammensetzung sowie in den Nahrungsmittelausgaben. Die Erzeugungsverhältnisse zeigen in der BRD einen dem Verbrauch in etwa angepaßten Zuckerrübenanbau, in der CSSR aber eine weniger intensive Übererzeugung, welche fast zur Hälfte für die Ausfuhr bestimmt ist. In beiden Ländern erhöht sich die Zuckererzeugung, in der CSSR ein wenig schneller, ebenfalls die Erzeugung an zuckerreichen Erzeugnissen. Was den Zuckergehalt in den Erzeugnissen betrifft, scheint dieser in der BRD außer in Getränken prinzipiell höher zu sein. An weiteren, den Zuckerverbrauch beeinflussenden Faktoren sind bisher weniger bekannte oder beachtete Ernährungsgewohnheiten zu erwähnen, die aber von der Volkswirtschaft unmittelbar oder mittelbar beeinflußt werden. In der ernährungsphysiologischen Beurteilung positive Tätigkeiten von Gesellschaften und Institutionen in bezug auf Aufklärung, wirtschaftspolitische Maßnahmen, können in dem Zusammenhang ebenfalls genannt werden. Die Situation des Zuckerverbrauchs in beiden Ländern läßt sich dahingehend charakterisieren, daß die Trends des Verbrauchs und der Erzeugung steigend sind, die jedoch zugleich eine Tendenz zu einer gewissen Verschlechterung der gesamten Ernährungssituation bedeuten. Unsere Analyse sucht Begründungen für die Unterschiede der Verbrauchshöhen beider Länder. In der BRD wurden keine Ursachen außer dem des Verbraucherverhalten gefunden. In der CSSR lassen sich dagegen einige Momente in der Wirtschaftspolitik zeigen, die für die Steigerung des Zuckerverbrauchs eine günstige Ausgangsposition bildeten. Trotz der Unterschiede sind in beiden Ländern Überlegungen zur weiteren Entwicklung aktuell, wozu diese Studie Unterlagen bringen kann. In der BRD kann die volle Aufmerksamkeit der industriellen Verarbeitung gewidmet werden, wo Möglichkeiten zur Beschränkung des Zuckeranteils zu suchen sind. In der CSSR liegt der Schwerpunkt in den Privathaushalten, also im Wirken auf die Verbraucher und in der Getränkeherstellung.

Notes: Zusammenfassung Die Versuche ergaben, daß die Verfütterung erhitzter Öle an Wistar-Ratten keinen Einfluß auf die Fortpflanzung der Versuchstiere und die Aufzucht von deren Jungen hat. Junge Weibchen zeigten sich signifikant paarungsfreudiger als ältere.

Notes: Summary The solubility of cholesterol in aqueous solutions of bile salts and lecithin with N/10 phosphate buffer, pH 7.3 has been examined. For the sodium salts of the six bile acids used in the study, the capacity for dissolving cholesterol was found to decrease in the following order: Glycodeoxycholate, Taurodeoxycholate, Glycochenodeoxycholate, Taurochenodeoxycholate, Glycocholate, Taurocholate. The differences with respect to cholesterol dissolving capacity were greatest when no lecithin was present, and decreased as the amount of lecithin increased. Graphical representations (molar ratio bile salt to cholesterol as abscissa, molar ratio lecithin to cholesterol as ordinate) of the limits for solubility of cholesterol in 100 millimolar solutions of each of the six bile salts to which purified egg lecithin is added in amounts varying from zero to approximately 80 millimoles per 100 millimoles bile salt, had the shape of curved lines tending to converge against a point, approximately 3.5, on the vertical axis but without reaching it. (Fig. 1). The starting points of the curves on the horizontal axis (millimoles bile salt required to dissolve 1 millimole of cholesterol in the absence of lecithin) were: for Glycodeoxycholate 19, for Taurodeoxycholate 30, for Glycochenodeoxycholate 34, for Taurochenodeoxycholate 47, for Glycocholate 52, for Taurocholate 62. The graphical representation, as above, of the limit for solubility of cholesterol in a 100 millimolar solution of a mixture of the six bile salts in relative amounts as in human bile, to which lecithin from human bile is added was practically identical to the corresponding curve for a 100 millimolar solution of glycochenodeoxycholate with additions of purified egg lecithin (Fig. 2.). The starting point on the horizontal axis for the curve representing mixed bile salts could be calculated — with fair approximation — from the cholesterol dissolving capacities of the individual bile salts in the mixture. The graphical representations of the limits for solubility of cholesterol in 50 millimolar, 100 millimolar and 200 millimolar aqueous solutions of sodium taurodeoxycholate to which purified egg lecithin was added in varying amounts did not show any certain differences from each other. Two purified egg lecithins of greatly different fatty acid pattern (Table 1) isolated from eggs of hens fed linoleic acid deficient diets and linoleic acid rich diets respectively, did not show any certain difference from each other with respect to cholesterol dissolving capacity when added in varying amounts to a 100 millimolar solution of sodium taurodeoxycholate.

Notes: Zusammenfassung Durch eine quantitative radiale Immunodiffusion und Elektrophorese in albuminhaltigem Agar-Agarose-Gel wurden die Verschiebungen in den Serum-Lipoproteinen in der Fetalperiode der Neugeborenen verfolgt. Bei der Geburt konnte ein Übergewicht (relativ) von einer Fraktion mit Mobilität wie Prä-Beta-Lipoprotein und ein niedriges Alpha- und Beta-Lipoprotein nachgewiesen werden. Letztes stieg in der ersten Woche nach der Geburt fast linear mit dem Alter in Tagen, erreichte aber nicht den Serum-Lipoproteinwert der Mutter. Beim Vergleich der Konzentration von Serum-Beta-Lipoprotein bei Neugeborenen mit Geburtsgewicht und Kost, konnte der niedrigste tägliche Zuwachs bei Neugeborenen mit Geburtsgewicht unter 2500 g gefunden werden. Bei Kindern (Geburtsgewicht über 2500g) mit Muttermilch unter Zugabe von „half skimmed milk“ (E) ernährt, ergab sich der höchste tägliche Zuwachs von Beta-Lipoprotein. Die Ergebnisse wurden auf Grundlage der vorliegenden Literatur über die Physiologie der Lipid Metabolisme der Geburtsperiode besprochen.

Notes: Zusammenfassung In Rattenversuchen wurden die biologischen Funktionen der noch nicht identifizierten Nahrungsfaktoren weiter präzisiert. Die von der Darm-Mikroflora synthetisierten Faktoren üben im höheren Tierorganismus ausschließlich Wachstumsfunktionen aus, wogegen die nur in höheren Pflanzen enthaltenen Faktoren außerdem auch für die Fortpflanzung sowie für die Entwicklung und Funktionstüchtigkeit mehrerer Organe notwendig sind.

Notes: Zusammenfassung Die Fettsäureverteilung und der Gesamtgehalt an Fettsäuren und E-Vitamin im Serum wurde in den Tagen nach der Geburt der Neugeborenen verfolgt und mit den Werten der Mutter und teils mit den Werten der der Kinder angebotenen Nahrung verglichen. Beim Vergleich der polyungesättigten Fettsäuren mit dem E-Vitamingehalt in der Babykost konnte festgestellt werden, daß mit der Ernährung durch eine europäische Kost kein Risiko für einen relativen E-Vitaminmangel vorliegt und damit normalerweise kein nahrungsbestimmtes Risiko für eine peroxidative Hemolyse vorhanden ist. Andererseits sind Befunde über einen niedrigen E-Vitamingehalt bei Geburt von Kindern mit Geburtsgewicht unter 2500 g, jedoch ein normaler Gehalt bei Kindern mit Geburtsgewicht über 2500 g festgestellt worden. Das erste Verhältnis muß durch einen herabgesetzten Transport des E-Vitamines durch die Placenta erklärt werden. Der Fettsäuregehalt im Serum in der Geburtsperiode konnte beträchtliche Änderungen aufweisen. So ist der Gesamtgehalt an Fettsäuren im Geburtsaugenblick mehr wie zweimal so niedrig wie der der Mutter. Der Arachidonsäuregehalt ist höher, während der Linolsäuregehalt niedriger ist als der der Mutter. Innerhalb der ersten Tage nach der Geburt sank der Linolsäuregehalt relativ im Serum, während der Gehalt an Palmitinsäure stieg. In den folgenden vier Tagen stieg die Linolsäuremenge, während die Palmitinsäuremenge sank. Die Ölsäure stieg relativ während der ganzen Periode hindurch, während Stearinsäure und Arachidonsäure absanken. Obenerwähnte Änderungen in der Fettsäureverteilung wurden durch eine Regressionsanalyse statistisch behandelt und in Beziehung zu Kost, und Geburtsgewicht gesetzt. Zum Schluß wurden die Ergebnisse auf Grundlage der vorliegenden Literatur über die Physiologie der Geburtsperiode besprochen.

Notes: Zusammenfassung Für die etwa 5500 einbezogenen Haushalte wird der Verbrauch an Lebensmitteln, die Zufuhr an Calorien und Nährstoffen sowie die Höhe der Bedarfsdeckung an wichtigen Nährstoffen nach Bundesland, Betriebsgröße, AK-Besatz, Erzeugungsrichtung dargestellt. Im Mittel wird die wünschenswerte Höhe der Nährstoffzufuhr nach allen Kriterien erreicht. Einzelwerte geben jedoch unzureichende Zufuhren, im wesentlichen an Protein, Calcium, Thiamin, andererseits aber auch überreichliche Zufuhren, vornehmlich an Reinfett, Protein tierischer Herkunft, Niacin zu erkennen.

Notes: Summary Groups of young female hamsters were reared for 56 to 64 days on the following diets: 1. A basal diet having rice starch as the carbohydrate component and containing no added fat. 2. The basal diet modified by incorporation of 10% hydrogenated palm oil at the expense of the same weight of rice starch. 3. The basal diet modified by incorporation of 10% of a mixture of 4 parts of hydrogenated palm oil and 6 parts of sunflower seed oil at the expense of the same weight of rice starch. At the end of the feeding period the molar ratio between lipid-soluble phosphorus and cholesterol in the bladder bile was lowest with diet no. 1, slightly but not significantly higher with diet no. 2, and considerably and significantly higher with diet no. 3. The gain in weight of the animals was almost the same with diet no. 2 as with diet no. 3, and significantly greater than with diet no. 1.

Notes: Zusammenfassung Es werden allgemeine Faktoren für die Berechnung des Caloriengehaltes gemischter Nahrung aus dem Gehalt an Fett, Protein und Kohlenhydraten aufgestellt. Die Grundlage bilden die speziellen Faktoren nach demAtwater-System und die gegenwärtige Zusammensetzung der Nährstoffversorgung in der Bunderepublik Deutschland. Die Voraussetzungen für eine sachgemäße Anwendung dieser Faktoren werden dargestellt.

Notes: Zusammenfassung 80 männliche Sprague-Dawley-Ratten erhielten über 4 Wochen eine Diät mit 20% Rotbarschöl. In der 5. Woche wurde anstelle des Rotbarchöles eine Diät mit 10% Cocosfett und von der 6. Woche an mit 20% Cocosfett bis zur 27. Woche gegeben. Die Kontrollgruppe erhielt eine Diät mit 4% Fett (Altromin). Nach 4 Wochen Rotbarschöl entfielen in den Nierenlipiden 2,4% der Gesamtfettsäuren auf Docosahexaensäure, 8,2% auf Pentaensäuren, 9,8% auf Tetraensäuren und 8,3% auf Diensäuren. Nach Umstellung der Diät von Rotbarschöl auf Cocosfett vermehrte sich die Linolsäure von 6,7 auf 13,5% nach einer Woche Cocosfett, stieg auf 14,4% nach 11 Wochen Cocosfett und sank schließlich auf 5,8–7,8% bei Versuchsende. Die Arachidonsäure stieg von 9,3 auf 11,1% nach 1 Woche Cocosfett und erhöhte sich auf 18–20,9% am Ende der Cocosperiode. Die Halbwertszeit der Docosahexaensäure beträgt im Nierengewebe etwa 10 Wochen. Die beiden Docosapentaensäuren Ω 3 und Ω 6 fielen von 0,3 bzw. 0,8% bis zum Versuchsende auf 0,1% ab. Ihre Halbwertszeiten betrugen 22 Wochen (Ω 6) und 6 Wochen (Ω 3). Die Halbwertszeit Eicosapentaensäure Ω 6 betrug 1 1/2 Wochen und die der isomeren Ω 3-Säure 4 1/2 Wochen. Die ölsäure vermehrte sich von 23,7 auf 30,1–32,9% bei Versuchsende. Laurin- und Myristinsäure stiegen leicht an, Palmitin- und Stearinsäure verminderten sich im Laufe des Versuches.

Notes: Zusammenfassung 80 männliche Sprague-Dawley-Ratten erhielten über 4 Wochen eine Diät mit 20% Rotbarschöl. In der 5. Woche wurde anstelle des Rotbarschöles 10% Cocosfett und von der 6. Woche bis zur 27. Woche 20% Cocosfett gegeben. Die Kontrollgruppe erhielt eine Standarddiät mit 4% Fett (Altromin). Nach 4 Wochen Rotbarschöl entfielen in den Herzmuskellipiden 7,9% der Gesamtfettsäuren auf Docosahexaensäure, 3,9% auf Pentaensäuren, 7,65% auf Tetraensäuren und 6,7% auf Diensäuren. Nach Umstellung der Diät von Rotbarschöl auf Cocosfett stieg die Linolsäure von 6,4% bis auf 24,3% nach 4 Wochen Cocosfett an. Bis zur 11. Woche Cocosfett blieb der Linolsäuregehalt des Myokards bei 19% und sank bis zum Versuchsende auf 9,4–12,6% ab. Gleichzeitig vermehrte sich Arachidonsäure von 7,6 auf 14,3%. Die Halbwertszeit der Docosahexaensäure beträgt 6–7 Wochen. Die Docosapentaensäure Ω 3 stieg auf 1,6% (C 2, C 3) an und sank bis Versuchende auf 0,4% ab. Ihre Halbwertszeit betrug 7 Wochen. Die Docosapentaensäure Ω 6 stieg von 0,1% (R 4) bis auf 1,4% bei Versuchsende. Die Halbwertszeiten der Eicosapentaensäuren waren bei unserer Versuchsanordnung nicht exakt bestimmbar. Die gesättigten Fettsäuren vermehrten sich im Myokard nicht wesentlich. Entsprechend der Abnahme der Polyenfettsäuren stiegen unter Cocosfütterung Palmitoleinr und Olsäure an.

Notes: Zusammenfassung Bei männlichen Jugendlichen zwischen 6–16 Lebensjahren, die sportlich tätig waren, wurden mittels der anthropometrischen Methode, die Hautfaltengrößenbestimmung, nach der Methode der WHO (J. B.Jeliffe), der Röntgenhistometrie und mit dem Ultraschallecholotverfahren vergleichend der Fettgehalt und das Magergewicht — welches mit der Muskulatur in engem Zusammenhange steht — bestimmt. Die verschiedenen Methoden können zur gegenseitigen Kontrolle der Ergebnisse verwendet werden.

Notes: Summary Summary With the method described it is possible to record thespontaneous food-intake in man simultaneously and quantitatively. The experimental situation is suitable for longterm-studies and is relatively free of socio-cultural cues, habits, attitudes, and stereotypes. The subject cannot control his food-intake optically. Results: 1. Having adapted to the experimental setting, Ss with normal weight have a consistent food-intake. 2. Interindividual differences are recorded and analysed with regard (a) to the estimate of absolute quantity, (b) to the estimate of relative quantity. 3. The data recorded have average predictive validity-coefficients. 4. The effects of the independent variables can be accounted for quantitatively and qualitatively. 5. Individually consistent, but interindividually different types of cumulative food-intake curves are described, but cannot be fully interpreted yet.

Notes: Summary Following the oral intake of 50 gm fructose, sorbitol or xylitol, an increase in the Concentration of serum uric acid from 0.5 to 2.5 mg% was observed. Xylitol proved to be the most effective substance. Sorbitol had the least effect. Galactose and glucose had no effect even in considerably higher dosage (up to 200 gm by mouth). Saccharose, however, in very high dosage (200 gm by mouth) resulted in an increase in the concentration of serum uric acid. The increase in serum uric after fructose, sorbitol and xylitol was due to uric acid synthesis as the uric acid loss during the experiments was increased. A small measurable increase in blood lactate concentration was found only after the ingestion of fructose. Die Untersuchungen wurden mit Unterstützung der Jacques Pfrimmer-Gedächtnisstiftung durchgeführt.

Notes: Zusammenfassung In 20 Tagesnahrungen gesunder Kinder wurde der Caloriengehalt nach folgenden Methoden bestimmt und miteinander verglichen: 1. Berechnung mit Nährstofftabellen 2. Calorimetrische Bestimmungen 3. Berechnungen aus der chemischen Analyse a) nachAtwater b) nachRubner c) nach einer vereinfachten Formel, basierend auf demAtwater-System. Die Berechnung der physiologischen Verbrennungswärme ergibt nach allen Methoden ähnliche Werte, nachAtwater die höchsten, aus Nährstofftabellen die niedrigsten. Diese Unterschiede werden im Blick auf die Berechnungsgrundlagen diskutiert. Bezogen auf den Durchschnittswert für die physiologische Verbrennungswärme liegt die calorimetrisch bestimmte physikalische Verbrennungswärme etwa 3% höher, die verfügbare Verbrennungswärme etwa 5% niedriger. Mit einer vereinfachten Formel: δH′=Fett × 9,4 + (0,95 x Trockensubstanz—Fett) x 4,2 läßt sich die physiologische Verbrennungswärme einer gemischten Nahrung des europäischnordamerikanischen Grundmusters für praktische Zwecke hinreichend genau berechnen. Obwohl die Grundlagen zur Calorienberechnung überwiegend auf Untersuchungen mit Erwachsenen beruhen, stimmen die Resultate langfristiger Bilanzversuche mit Kindern (Macy) gut damit überein.

Notes: Abstract Hydrogen atoms in phenanthrene at room temperature have been located with estimated standard deviations of ±0·07 Å by neutron diffraction analysis. With carbon atoms fixed at positions determined in a previous X-ray analysis, least-squares refinement of limited neutron diffraction data led to anR index of 0·122 over 214 independent observations. An intramolecular contact of 2·03 Å is confirmed for the bay hydrogen atoms H(4) and H(5).

Notes: Abstract Crystals of ethidium bromide (2,7-diamino-9-phenyl-10-ethylphenanthridinium bromide) monohydrate are monoclinic,a = 9·577,b = 10·698,c = 20·242 Å, β = 106·34 °,Z = 4, space groupP21/c. The structure was determined with CuKα. diffractometer data by direct methods, and was refined by full-matrix least-squares methods toR = 0·058 for 2151 observed reflexions. The phenanthridinium ring is slightly non-planar; the phenyl ring makes an angle of 97 ° with the mean plane of the phenanthridine ring, and the ethyl group is rotated about the N-C bond 84 ° out of the mean plane. One of the amino nitrogen atoms has a pyramidal and the other a planar configuration. Only three of the six active hydrogen atoms participate in a hydrogen-bonding scheme, which involves the pyramidal nitrogen atom, the water molecule and the bromide ion. The phenanthridine rings of two molecules related by a centre of symmetry are separated by 3·50 Å.

Notes: Abstract The crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)gold(III) bis(1,2-dicyanoethene-1,2-dithiolato)aurate(III), Au[S2CN(C4H9)2]2Au[S2C2(CN)2]2, has been determined from a single-crystal X-ray diffraction study. The monoclinic cell, space groupP21,/c, witha = 9·930(3),b = 12·517(3),c = 15·632(3) Å and β = 110·46(3) °, contains two formula units. Three-dimensional intensity data, up to θ = 35 ° were collected on an automatic diffractometer. Atomic parameters were refined by full-matrix least-squares methods to a conventionalR value of 0·04 for 1874 independent non-zero reflections. The structure consists of bis(di-n-butyldithiocarbamato)gold(III) cations and bis(l,2-dicyanoethene-l,2-dithiolato)aurate(III) anions. In both ions, the gold atom is in planar coordination with four sulphur atoms, the Au-S bond lengths being 2·333(4) and 2·337(4) Å in the cation and 2·312(4) and 2·306(5) Å in the anion.

Notes: Abstract Crystals of morpholine biguanide hydrochloride, C6H13N5O. HC1, belong to the orthorhombic space groupPbca;a = 19·02 Å,b = 9·92 Å,c = 10·34 Å andZ = 8. The structure has been solved by three-dimensional Patterson and heavy-atom Fourier syntheses. The hydrogen positions have been located from a three-dimensional difference Fourier synthesis. The positional coordinates of all the atoms and their temperature factors (anisotropic for non-hydrogen atoms and isotropic for hydrogen atoms) have been refined by three-dimensional least-squares methods. The finalR value is 0·087. The morpholine ring has been found to assume a chair configuration. The contribution of various valence bond structures to the normal state of the morpholine biguanide hydrochloride molecule has been studied with reference to the characters of the C-N bonds in the biguanide part of the molecule. Both the guanidine groups are planar. Of six available hydrogen atoms, only four take part in forming hydrogen bonds of the type N-H···Cl−. The molecules in the crystal are linked by a three-dimensional network of hydrogen bonds.

Notes: Abstract The crystal and molecular structure of bis(N,N-diethyldithiocarbamato)palladium(II), Pd(S2CN(C2H5)2)2, has been determined by a three-dimensional X-ray analysis. The compound crystallizes in the tetragonal space groupP42/n with unit cell dimensionsa = 16·439(8) Å andc = 6·247(3) Å. The crystals are isomorphous with bis(N,N-diethyldithiocarbamato)platinum(II). Intensities were obtained with an automatic diffractometer. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·038 for 600 non-zero observed reflections. The palladium is in planar coordination with four sulphur atoms, the two non-equivalent Pd-S bond lengths being 2·317(3) and 2·315(3) Å.

Notes: Abstract The crystal structure of a cyclobutane derivative, 4,8-dibromo-3,7-diketo-3,4,4a,4b,7,8,8a,8b-octahydrodibenzo-[a,g]-biphenylene (C20H14O2Br2), has been determined from 1614 intensities collected with a four-circle diffractometer and refined by three-dimensional least-squares techniques. The crystals are monoclinic, space groupP21/c, with four molecules in a unit cell of dimensionsa = 10·863 ± 0·006,b = 21·060 ± 0·011,c = 7·772 ± 0·005 Å and β = 105·33 ± 0·04 °. The cyclobutane ring was found to have a bent configuration with a dihedral angle of 157 °.

Notes: Summary The crystal structure of tetrakis(N,N′-diallylthiourea)nickel(II) iodide [Ni(C7H12N2S)4I2] has been determined by a three-dimensional X-ray analysis. FinalR, after anisotropic least-squares refinement, is 8·8%. The crystals are tetragonal (P4/n):a = 11·24(1),c = 15·43(1) Å,Z = 2. Ni(II) is on a 4-fold axis; the coordination around it is flattened pyramidal and involves four sulphur atoms from four diallylthiourea molecules (Ni-S = 2·221 Å). Ni(II) is out of the plane through the sulphur atoms by 0·40 Å. Two I- ions lie on opposite sides with respect to the nickel atom along the 4-fold axis, at distances Ni...I(1) = 3·74 Å, Ni...I(2) = 6·64 Å. The orientation of the allylthiourea molecules is determined mainly by a hydrogen bond formed by one nitrogen (N(1)) with the iodine which is nearer to the nickel.

Notes: Abstract The results of a unified normal coordinate treatment for vinyl fluoride and the seven deuterated species are presented. Our calculation confirms the out-of-plane assignment of Scherer and Potts. For the in-plane vibrations, we have used a modified valence-force type of potential function and, on the basis of the results, we are presenting a satisfactory assignment for most of the fundamentals. Investigation of the liquid spectra is recommended to resolve the ambiguity of the remaining few undecided in-plane fundamentals.

Notes: Abstract Rubidium and ammonium hydrogen glutarates (M + −CO2.C3H6.CO2H) each crystallize with four molecules in orthorhombic unit cells of almost identical dimensions: (M = Rb)a = 18·55,b = 7·57,c = 5·29 Å; (M = NH4)a= 18·59,b= 7·56,c= 5· 27 Å. They have very similar structures, but they are not isomorphous: space groupsCmma (Rb) andPmaa (NH4). The crystal structures have been determined by three-dimensional X-ray analysis and refined with moderate precision. Both have infinite chains of glutarate residues, linked end-to-end by very short, symmetrical hydrogen bonds, with O···H···O = 2·40(2) (Rb) and O···H···O = 2·460(6) Å (NH4). In the Rb salt, the glutarate residue has strict, crystallographicm symmetry. The difference in the NH4 salt arises from small movements of the carbon and (especially) the oxygen atoms out of this symmetry plane. These are due to N-H···O bonding: two equivalent cations in the Rb salt, each making contact with eight oxygen atoms, become differentiated in the NH4 salt by linkage to different sets of four oxygens.

Notes: Abstract Crystals of 1-aminocyclooctanecarboxylic acid hydrobromide are orthorhombic, witha= 26·026,b=7·087,c= 6·149,Z= 4 and space groupP212121.The structure was solved in projections by direct methods and later refined with three-dimensional data using a full-matrix least-squares treatment. All hydrogen atoms were located from a difference Fourier and the finalRfactor for the 1128 observed reflections was 8·62 %. The molecules are held together by a series of hydrogen bonds in a three-dimensional network. A detailed discussion of the intramolecular and the intermolecular features of the structure is presented. The cyclooctane ring is found to exist in theboat-chair conformation.

Notes: Abstract The crystal structures of two isomeric complex compounds of formula [Cu(Cl)2(NH2NHCONH2)] have been determined by X-ray diffraction methods. The orthorhombic isomer has space groupPna21 and unit cell constants:a = 6·91(1),b = 8·30(1),c = 10·24(1) Å;Z = 4. The monoclinic isomer has space groupP21/c and unit cell constants:a = 6·91(1),b = 8·30(1),c = 11·32(1) Å, β = 117·1(2)°;Z = 4. In both complexes coordination around copper is octahedral, with chains of coordination polyhedra along [100]. In the monoclinic compound, the two semicarbazide molecules, which are present in two adjacent octahedra along the chain, have the oxygen and nitrogen atoms in thetrans configuration, one with respect to the other, and are correlated by a centre of symmetry. In the orthorhombic compound, the two semicarbazide molecules are in thecis configuration and there is no centre of symmetry. In both compounds packing is determined by the NH···Cl and NH···O hydrogen bonds which join the chains together.

Notes: Abstract The crystal and molecular structures of two polymorphs ofo-bromophenylazocarbamide (C7H6N3OBr) have been determined and refined by Fourier methods, using three-dimensional X-ray data collected at room temperature by photographic techniques. The unit cell parameters are, for the monoclinic modificationa = 25·20(1),b = 5·03(1),c = 14·01(1) Å, β = 105·5(1·0)°,Z = 8, space groupC2/c; for the orthorhombic modification,a= 14·02(1),b = 5·04(1),c = 24·32(3) Å,Z = 8, space groupPca21. In both polymorphs a rather large thermal effect is present, being greater for the orthorhombic phase. Corresponding bond distances and angles are equal in both structures to within 1σ. The double bond is virtually localized in theazo group, so that there is no conjugation between the bromophenyl and the carbamidic groups. NH···O hydrogen bonds link the molecules in ribbons, which are parallel in the monoclinic modification and mutually tilted (76·7 °) in the orthorhombic structure.

Notes: Abstract 1-aminocyclohexane carboxylic acid hydrochloride crystallizes in the monoclinic space groupP21 with unit cell dimensionsa = 9·36,b = 6·40,c = 7·40 Å and β = 96·0 °. The structure has been solved bybeta synthesis and refined three-dimensionally to anR factor of 10·9% with 817 observed reflexions. The conformation of the cyclohexane ring is a slightly distorted chair.

Notes: Abstract The infrared spectra oftrans-dichlorodiiodoethylene as a solid and in solution were recorded in the region 4000–25 cm−1. Raman spectra of the compound were obtained and semiquantitative polarization data were calculated. The mutual exclusion between the infrared and Raman frequencies are in agreement with the expectedC 2h (2/m) symmetry for this molecule. The fundamentals have been assigned and a normal coordinate analysis carried out. Thermodynamic functions and the root mean square amplitudes of vibration have been obtained.

Notes: Abstract The infrared spectra of both CH3OPSClF and CD3OPSClF in the vapor phase have been recorded from 4000 to 33 cm−1. The Raman spectra of the liquids have been recorded and a temperature study of the CD3OPSClF spectrum has been completed. Two isomeric configurations are indicated from the low-temperature Raman spectra. The doublet due to the P=S stretching vibration has a separation of only 15 cm−1. From the variation in the relative intensity of the doublet, an energy difference of −450 cal/mol was obtained for the two isomers. The fundamental vibrations are assigned on the basis of the band positions and isotopic shift factors. The assignments are compared to those previously given for the CH3OPSCl2 and CH3OPSF2 molecules.

Notes: Abstract The crystal and molecular structure ofcis-dicarbonyltetraphosphinechromium(O), [(CO)2(PH3)4Cr] has been determined by X-ray diffraction methods. The compound crystallizes in the monoclinic system: space groupC2/c,a = 6·968(6),b = 11·98(1),c = 12·87(1) Å, β = 99·80(8) °,V= 1059(3) Å3,Z=4,D m = 1·534(5),D x = 1·531(5) gcm−3, diffraction symmetry 2/m. The structure was solved by conventional methods, and refined by least-squares techniques to an agreement factorR = 0·078. The chromium atoms lie on rotation diads, and thus the molecules must have at least the symmetry 2(C 2); they were found to have, within the limits of accuracy, the even higher symmetrymm2 (C 2v ). There are two distinct independent Cr-P distances in the molecule, the Cr-P bonds where phosphorus istrans to carbonyl [2·338(4) Å] being significantly longer than those where phosphorus istrans to phosphine [2·282(4) Å]. This difference may be attributed to a difference in the back-bonding capabilities of the two types of ligands.

Notes: Abstract The crystal and molecular structure of diiodo-N,N,N′,N′-tetramethylthiuramdisulphidemercury(II), HgI2(S2CN(CH3)2)2, has been determined by a three-dimensional X-ray analysis. The compound crystallizes in the monoclinic space groupP21/c with the unit cell dimensionsa = 7·957 ± 4,b = 22·639 ± 7,c = 9·956 ± 6 Å and β = 112·14 ± 5 °;Z = 4. Intensities were obtained with an automatic diffractometer. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·044 for 1294 non-zero observed reflexions. The mercury is in distorted tetrahedral coordination with two iodine and two sulphur atoms. The Hg-I distances are 2.654 ± 2 and 2·661 ± 2 Å; the Hg-S distances are 2·651 ± 7 and 2·882 ± 7 Å. The thiuramdisulphide ligand consists of two planar units S2CNC2, nearly perpendicular to each other. Bond distances of the ligand are compared with distances in tetraalkylthiuram disulphide molecules and agree with infrared observations.

Notes: Summary The crystal and molecular structure of the N′,N′-(2-chlorobenziliden)histamine has been determined and refined by Fourier and least-squares methods using three-dimensional X-ray data collected at room temperature by photographic techniques. Crystal data is as follows:a = 8·76(2),b = 13·82(1),c = 9·88(2) Å, β = 110·3(1) °,Z = 4. Space group:P21/c. The structure of the molecule is of the same tetrahydroimidazo[4,5-c]pyridine type found in spinaceamine. The benzene ring is rotated with respect to the other part of the molecule, which is formed by a non-planar tetrahydropyridine ring condensed with a planar imidazole ring. The bond distances and angles in these two rings are consistent with the observed distribution of the hydrogen atoms. Packing is mainly determined by a N-H ... N hydrogen bond, which joins the molecules in zig-zag chains running along [001].

Notes: Abstract Dichloro-N-2-methylthiophenyl-2′-pyridylmethyleneiminecopper(II) is monoclinic:P21/c;a = 8·49(1),b = 10·80(1),c = 15·67(1) Å, β = 92·0(3)·,Z = 4. The crystal structure has been determined at room temperature from three-dimensional X-ray photographic data and refined by differential methods with anisotropic thermal parameters to a finalR value of 8·1%. Cu(II) coordinates to two chlorine atoms (Cu-Cl = 2·255,2·443 Å) and to one sulphur (Cu-S = 2·341 Å) and to two nitrogen atoms (Cu-N = 2·011, 2·014 Å) from methylthiophenylpyridylmethyleneimine; this represents a distorted tetragonal pyramid with the organic molecule behaving as a tridentate ligand. Packing is determined by normal van der Waals contacts.

Notes: Abstract The crystal structure of dioxotetrapyridinerhenium(V) chloride dihydrate has been determined by single crystal X-ray diffraction methods. The crystals are monoclinic with unit cell dimensionsa = 13·592(2),b = 11·973(2),c = 15·55(1) Å, β = 116·2(1)°, and the space group isCc with 4 formula weights per unit cell. A total of 1279 independent reflexions were examined and the structure was refined by full-matrix least squares to anR value of 0·11. The structure was refined both with rigid pyridine groups and independent atoms. The molecular cation has a near linear arrangement of the O-Re-O group, with an average Re-O distance of 1·76(3) Å. The average Re-N distance is 2·15(4) Å. The molecular cations are packed in layers along the ¯101 direction with pyridine groups interleaved. The chloride ion and water molecules lie between these layers, and the structure is held together by electrostatic forces between the cations and the chloride ions, and by hydrogen bonds between the water molecules and chloride ions or oxygen atoms. The cation is substantially distorted from 4/mmm (D 4h) as a result of crystal packing.

Notes: Abstract The crystal structure of the nickel(II) chelate of the monothio derivative of 2,2,6,6-tetramethyl-heptane-3, 5-dione has been studied at room temperature by X-ray diffraction methods. The space group isP21/c and the crystal data area = 19·96(2),b = 10·25(1),c = 12·45(1) Å, β = 102·17(5) °Z = 4,D m = 1·22,D c = 1·23 g cm−3. Full-matrix least-squares refinement of atomic and anisotropic thermal parameters, using 2109 non-zero intensities obtained by counter methods, terminated with a conventionalR of 0·105. The nickel was found to be surrounded by acis arrangement of two oxygen and two sulphur atoms which is almost planar, but slightly distorted towards a tetrahedron. All the evidence obtained supports extensive delocalization in the chelate rings, and the entire molecule has pseudomm symmetry. Thecis, rather thantrans relationship of the ligand atoms may indicate weak S-S interaction.

Notes: Abstract The crystal structure of di-μ-chloro(dicyandiamide)cadmium(II) has been determined and refined by Fourier and least-squares methods toR = 0·037 using three-dimensional X-ray data collected at room-temperature on a single-crystal automated diffractometer. Crystal data are as follows:a = 10·796(7),b = 8·933(5),c = 6·847(3) Å,β = 99·9(1) °,Z = 4; space groupP21/n. The cadmium atom is surrounded by four chlorine (Cu-Cl = 2·572, 2·607, 2·630, 2·647 Å) and two nitrogen atoms (Cd-N (nitrilic) = 2·358 Å; Cd-N (guanidic) = 2·430 Å) so that the whole polyhedron appears as a slightly distorted octahedron. The chlorine atoms form bridges between adjacent metal atoms so that the coordination octahedra are linked in chains running along [001]. These chains are joined together by dicyandiamide bridges.

Notes: Abstract The crystal structure of Lu(fod)3. H2O has been solved by three-dimensional X-ray methods at room temperature. The space group isPĪ and the cell dimensions area = 16·392,b = 22·492,c = 13·366 Å, α = 91·83 °, β = 119·93 °, γ = 90·00 °. There are four formula-units per unit cell;D m = 1·66,D c = 1·667 g cm−3. Least-squares refinement of atomic and individual isotropic thermal parameters terminated withR = 0·128. This relatively highR factor is due to crystal decomposition, to the prohibitively large asymmetric unit which necessitated refinement in parts and also to the high vapour pressure of the compound and consequently large thermal vibrations in the structure. These factors caused large uncertainties especially in the positions of the atoms at the ends of the long side chains, but the more important geometry of the coordination polyhedra at the cores of the roughly spherical molecules have been firmly established. Except for orientation differences, the two crystallographically independent formula-units are very similar and both are dimerized through water molecules with hydrogen bonds across centres of symmetry. In each case the coordination of lutetium is seven-fold, with the geometry of a monocapped trigonal prism.

Notes: Abstract The crystal structure of triptycene has been solved by packing considerations. 1585 reflexions were used in the refinement. In this refinement, the molecule was constrained to obey its free-state symmetry ¯6m2(D 3h) and to have atomic anisotropic temperature factors in agreement with a rigid-body model of molecular motion. In this way the reliability of the average molecular geometry is optimized.

Notes: Abstract Dinitro(2,9-dimethyl-1,10-phenanthroline)-palladium(II) crystallizes in the orthorhombic system, space groupP21 nb, with cell dimensionsa = 6·790,b = 19·807,c = 10·625 Å andZ = 4. The structure was determined from three-dimensional Fourier syntheses and refined by full-matrix least squares, the finalR for 1155 measured reflexions being 0·07.

Notes: Abstract The strongly temperature-dependent1H-nmr spectrum of prop-1-en-1,2-diol-3-one (triosereductone), C3H4O3, can be explained on the basis of valency tautomerism. Intramolecular hydrogen bonding is responsible for this effect.

Notes: Abstract The crystal structure of tris(N,N-di-n-butyldiselenocarbamato)nickel(IV) bromide, Ni(Se2CN-(C4H9)2)3Br, has been determined by three-dimensional X-ray methods. The Laue symmetry is 6/mmm, but the structure could be solved only in space groupP¯31c. The crystals were, therefore, regarded as being microtwinned on (001). The unit cell dimensions area =b = 14·69(3) andc = 10·91(3) Å. From integrated Weissenberg photographs, 307 non-zero symmetry-independent reflexions were measured photometrically. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·10. The quadrivalent nickel atom is octahedrally coordinated by six selenium atoms. The Ni-Se distance is 2·391(5) Å; the Se-Se distance within one diselenocarbamate ligand is 3·00(1) Å; Se-Se distances between different ligands are 3·51(1), 3·52(1) and 3·55(1) Å.

Notes: Abstract Analysis of X-ray counter data for the dihydrogen hexafluorosilicate monohydrates ofp-bromoaniline, BrC6H4NH2.1/2H2SiF6.H2O, andp-toluidine, CH3C6H4NH2.1/2H2SiF6.H2O, has shown that the two compounds are isostructural and that the orthorhombic crystals belong to the space groupPbca, witha = 7·80,b = 24·45,c = 9·48 Å anda = 7·89,b = 23·87,c = 9·53 Å, respectively, there being eight molecules in each unitcell. Structure analysis was initiated by the heavy atom method, and subsequent difference syntheses, carried out on thep-bromoaniline compound, then on thep-toluidine analogue, revealed the entire structure apart from the hydrogen atoms. From a difference synthesis on data for thep-toluidine compound refined by full-matrix least-squares procedures, the hydrogen atom sites were located, a reliability index,R = 0·052, being attained. The structures are sheet-like with bi-polar grouping of amino groups on either side of sheets of SiF 6 2− groups and are cross-linked by ionic forces and hydrogen bonds. The SiF 6 2− ion is octahedral, with an average Si-F distance of 1·69 ± 0·02 Å.

Notes: Abstract The crystal and molecular structure of (2,2′-bipyridine) pyridine tricarbonyl molybdenum (III), [(C10H8N2)(C5H5N)(CO)3Mo], has been determined from three-dimensional data collected photographically. The space group isPnam; the unit cell has the dimensionsa = 14·755 ±1,b = 8·344 ± 1,c = 13·733 ± 1 Å (at 20 °C) and contains four molecules. The structure has been refined to a residual (R) of 0·073 using least-squares methods on 1394 independent non-zero reflexions. The molecule has been found to be octahedral in arrangement, with bipyridine and pyridine forming one triangle and the three carbonyl groups forming the opposite triangle of the octahedron. The best fit plane through the pyridine and lower carbonyl groups make an angle of 78 ° with the equatorial plane. There is evidence of significant distortion from the ideal octahedral angles of 90 °. Within the molecule, no interatomic distance or bond angle departs significantly from accepted values.

Notes: Abstract The crystal structure of Dy(thd)3H2O has been solved by three-dimensional X-ray methods at room temperature. The space group isP¯1 and the cell dimensions area = 14·21(1),b = 14·88(2),c = 11·60(2) Å, α = 99·76(3), β = 109·91(1), γ = 114·08(1) °.Z = 2,D m = l·24 andD x = 1·238 gcm−3, respectively. Full-matrix least-squares refinement of atomic and individual isotropic thermal parameters, using 3015 intensities obtained by counter methods, terminated with a conventionalR of 0·058. The oxygen polyhedron around dysprosium has pure seven-coordination geometry, the seventh ligand being the water molecule. The water is hydrogen bonded to two oxygen atoms of a centre of symmetry related formula unit so that two formula units are in fact held together by hydrogen bonds in a dimer.

Notes: Abstract Irradiation of uracil in ice produces a small quantity of thecis-anti cyclobutyl type photodimer. The molecule contains a pseudo two-fold axis and a cyclobutyl ring which is puckered, with dihedral angles near 150°. Torsion angles about the C(5)-C(6′) and C(5′)-C(6) bonds are 21°. Each uracil residue has seven atoms which are coplanar to within 0-07 Å, while C(6) and C(6′) are 0·38 Å and 0·35 Å out of the planes of their respective residues. Each molecule participates in eight NH...O bonds which range from 2·83 to 2·97 Å. The material crystallizes in the triclinic space group P¯1 with unit cell parametersa = 8·594 Å,b = 7·478 Å,c = 6·915 Å, α = 96·9 °, β = 95·4 ° and γ = 85·5 °. The structure was solved by means of the symbolic addition procedure for phase determination.

Notes: Abstract This is the first reported structure analysis of a cyclobutyl type photodimer obtained from the irradiation of thymine, uracil or its derivatives which contains water in the crystal lattice. Thecis-syn 6-methyluracil photodimer. H2O gives anomalous nmr and ir spectral data which may correlate with the crystal structure. The material crystallizes in space groupP21/a with unit cell parametersa = 15·58 Å,b = 11·33 Å,c = 7·28 Å and β = 107·2 °. Channels are formed in the crystal lattice which contain the H2O molecules. Each H2O molecule participates in hydrogen bonding to three different dimer molecules. The puckered cyclobutyl ring is significantly flatter than in the anhydrouscis-syn uracil photodimer and differences in the configurations of the uracil residues occur. The structure was solved by means of the symbolic addition procedure.

Notes: Abstract The Raman spectrum of solid glyoxal has been recorded from 100 to 3500 cm−1. Fundamental frequencies were observed at 2882, 1729, 1364, 1078, 1050, and 551 cm−1 and assigned as the C—H stretching, C=O stretching, C—H in-plane bending, C—C stretching, C—H out-of-plane bending and COH rocking modes, respectively. The infrared spectrum of the solid has been investigated from 33 to 4000 cm−1, and the values observed for the fundamentals are compared with those previously reported from studies of the vapor. The unusual frequency shifts upon solidification are discussed. A comparison of the infrared and Raman bands in the crystal shows that the mutual exclusion principle is operative. It is concluded from this alternate forbiddance that the molecule has a centrosymmetric structure in the crystal and that each molecule occupies a C i (¯1) site. The factor group of the crystal is believed to be eitherC 2h (2/m) orD 2h (mmm) with two or four molecules per primitive unit cell.

Notes: Abstract The crystal structure of 1-(2-aminoethyl)biguanide-isothiocyanato-copper(II)thiocyanate, [Cu(aebg)(NCS)] (SCN) (aebg = NH2. CH2. CH2. N=C(NH2). NH. C(NH). NH2) has been determined and refined by Fourier methods using three-dimensional X-ray data collected on a Weissenberg automatic diffractometer. The unit cell parameters are:a = 11·41(2),b = 8·81(2),c = 7·45(2) Å; α = 87·6° (2); β = 67·2° (2); γ = 70·1° (2);Z = 2. Assuming space group P¯1, the structure was refined down toR = 8·5 %. The coordination around Cu is slightly distorted square planar and concerns three N atoms from the aebg ligand (Cu-N = 1·988(8), 2·019(7), 1·963(5) Å) and the terminal N of an isothiocyanate group (Cu-N = 1·941(5) Å). Two unsymmetrical, long interactions (Cu-N = 3·367(7) and 2·947(7) Å), with the N atoms belonging to two NCS groupstrans with respect to the coordination plane, complete the coordination to a distorted octahedron. In the aebg ligand the double bonds are localized on the C-N groups, whose nitrogen atoms coordinate to the metal.

Notes: Abstract The crystal and molecular structure of bis(N,N-di-n-butyldithiocarbamato)gold(III)dibromoargentate(I), Au(S2CN(C4H9)2)2AgBr2, has been determined by three-dimensional X-ray methods. The compound crystallizes in the monoclinic space groupC2/c with unit cell dimensions:a= 17·39(1)b = 18·65(1);c = 9·199(6) Å; β = 93·9(1)°;Z=4. Intensities were collected on an automatic diffractometer. The structural parameters were refined by least-squares methods to a conventionalR factor of 0·048 for 854 non-zero observed reflexions. The structure consists of Au(S2CN(C4H9)2)2+ and AgBr2 − ions. The gold is in planar coordination with four sulphur atoms, the two crystallographically non-equivalent Au-S bond lengths being 2·357(8) and 2·324(8) Å. The silver is linearly coordinated, the Ag-Br bond lengths being 2·450(5) Å. The ionic packing in the structure differs from that in the analogous Au(S2CN(C4H9)2)2AuBr2 complex.

Notes: Abstract 1-Aminocycloheptanecarboxylic acid hydrobromide monohydrate crystallizes in space groupP212121 with cell dimensionsa= 25·69,b= 6·85 andc= 6·61 Å. The structure was solved in thehk0 andh0l projections, and refined with the three-dimensional data to anR factor of 9·86%. The cycloheptane ring is disordered, which leads to ‘predominant’ and ‘alternative’ conformations. Both of these conformations correspond to a skew-chair form. The structure is stabilized by a three-dimensional network of hydrogen bonds.

Notes: Abstract An occupation-factor analysis using single-crystal neutron diffraction data has shown that the hydrogen atoms in the structure of the mineral monetite, CaHPO4, occupy hydrogen-bonding sites closely similar to those predicted in a previous X-ray refinement. Least-squares refinement in space groupP¯1 of the potential coordinates and isotropic temperature parameters for the three distinct proton sites led to a resultantR of 0·10 over the 371 independent neutron structure factors. Detailed analysis showed that the distribution of the hydrogen atoms was almost certainly ordered in symmetryP1 with only half of the O(6) atoms (in space groupP¯1) carrying hydrogen atoms; the short O(7)-P(1)... O(7′) hydrogen bond of 2·44 Å across what would be a symmetry centre inP¯1 is probably unsymmetrical. Minute piezo- and pyroelectric effects confirmedP1 as the space group. Further refinement of the X-ray data in space groupP1 indicated that the deviations from centrosymmetry must be small and, so far as can be detected, confined to the hydrogen atoms.

Notes: Abstract The crystal structure of C15H22O5, a root inhibitor isolated from adult leaves ofEucalyptus grandis, has been determined by direct methods with Cukα diffractometer data and refined by full-matrix least-squares calculations toR = 0·046 for 1829 statistically significant reflexions. The compound, a racemate, crystallizes in the monoclinic space groupP21/c, with unit cell dimensionsa = 11·767,b = 12·063,c = 10·906 Å, β = 103·2° andZ = 4. The molecular skeleton consists of a 2,3-dioxabicyclo[4.4.0]decene system with one hydroxyl, two carbonyl, one ethyl and five methyl side groups. The dihedral angle at the peroxide bond is 76·8° and the O-O bond distance is 1·480 Å. The molecules are linked in the c direction by hydrogen bonds between the hydroxyl group and one of the carbonyl oxygen atoms.

Notes: Abstract The crystal structure of di-μ-methoxo-bis(chloro-2-methylpyridine copper(II)), [CuCl(OCH3)-(2-mepy)]2, has been determined from three-dimensional, photographically recorded X-ray data. The unit cell is monoclinic, space groupP21/c, with dimensionsa = 8·79,b = 6·01,c = 17·59 Å, β = 104·4° and contains two centrosymmetric dimeric units [CuCl(OCH3). (2-mepy)]2, in which the copper atoms are linked by methoxide oxygen bridges, the dimers being joined into infinite chains through long copper-chlorine bonds. The environment of each copper atom may be described as a distorted tetragonal pyramid with one chlorine, one nitrogen and two oxygen atoms in the base and a chlorine atom from an adjacent dimer at the apex.

Notes: Abstract Bis[pyridine-2-(N-cyanocarboxamidato)]aquocopper(II), Cu(C5H4NCONCN)2(OH2), has been prepared and its i.r. spectrum and crystal structure have been determined. The crystals are triclinic (P¯1):a = 11·45(1),b = 10·35(1),c = 7·48(1) Å, α = 110·9(1), β = 102·2(2), γ = 108·9(1)°,Z = 2. The X-ray analysis, carried out using three-dimensional Patterson, Fourier and least-squares methods (finalR = 5·7%), showed copper(II) to be pentacoordinated, with two organic ligands chelating through their pyridine [Cu-N = 1·997(4), 1·989(4) Å] and amide nitrogen atoms [Cu-N = 1·980(7), 2·006(6) Å], and with one water molecule at a distance [Cu-OH2 = 2·335(4) Å] sensibly longer than the usual Cu-O(∼2·0 Å) coordinate bonds. The coordination polyhedron can be described either as a distorted tetrahedron formed by the nitrogen atoms with an extra position occupied by water or as a trigonal bipyramid having water and two nitrogen atoms in the equatorial plane. The packing determining interactions are the hydrogen bonds formed by water, and a long Cu...N (3·420 Å) contact between the metal and a nitrogen atom from an adjacent molecule.

Notes: Abstract p-toluidinium bifluoride crystallizes in the orthorhombic space groupPbca, witha = 7·161,b = 18·405,c = 11·824 Å andZ= 8. The structure was solved by direct methods from X-ray counter data measured with CuKα. radiation, and a finalR index of 0·052 was obtained for the 642 observed terms of the 1480 possible. Thep-toluidine molecule is fully protonated and the methyl group is either disordered, librating extensively or freely rotating. In the HF2 − ion the H atom is apparently centrally situated between the two fluorine atoms, and is obviously very delocalized; the F-H-F distance is 2·276 ± 0·005 Å. The structure consists of alternate layers ofp-toluidinium and hydrogenbifluoride ions with the latter hydrogen-bonded to the amine groupings.

Notes: Abstract Crystals of 1-chlorobenz[a]phenazine-7N-oxide, C16H9N2OCl, are orthorhombic,a =15·04,b = 3·91,c = 20·50 Å,Z = 4, space groupPna21. The crystal structure has been determined from two- and three-dimensional X-ray photographic data and refined by Fourier and least-squares methods toR = 0·095 for 715 observed reflexions. The molecule is slightly non-planar. Bond lengths and angles compare well with those of other molecules. Close molecular packing is given by layers of molecules parallel to (001) plane.

Notes: Abstract Crystals of the ‘title’ compound, C19H21NO5, are monoclinic, space groupP21/c,a = 7·706,b = 14·470,c = 16·836 Å, β = 106·45°,Z = 4. The structure was determined with CuKα diffractometer data by symbolic addition procedures and Fourier syntheses, and was refined by full-matrix least-squares methods toR = 0·079 for 2192 observed reflexions. All non-methyl hydrogen atom positions were determined. The non-aromatic six-membered ring has aboat conformation. The four-membered ring, which iscis-fused to the six-membered ring, is slightly folded, and the planar amino and carboxyl groups lie almost in the four-membered ring plane. This geometry, and the detailed bond distances suggest electron delocalization, which may make the compound a useful intermediate in the synthesis of a stable cyclobutadiene system.

Notes: Abstract X-ray diffraction data from single crystals of the trimethylamine complexes of the three boron halides, BCl3, BBr3, and BI3, lead to aP21/m monoclinic cell containing two molecules for each complex. The unit cell dimensions area = 6·68(1),b = 10·247(3),c = 6·502(6) Å, β =116·2(1)° (chloro);a = 6·86(1),b = 10·612(4),c = 6·737(6) Å, β = 115·8(1)° (bromo);a = 6·92(2),b = 10·86(1),c = 7·147(6) Å, β = 93·9(1)° (iodo). The structures were solved by three-dimensional sharpened Patterson functions and show only the chloro and bromo compounds to be isomorphous. Refinement of 662,718 and 954 observed reflexions for the chloro, bromo and iodo complexes, respectively, using anisotropic thermal parameters yielded conventionalR factors of 0·045, 0·087 and 0·054. The molecules are shown to possess a B—N dative bond, a staggered conformation, and effective 3m (C 3v) symmetry. Average C—N bond lengths are 1·52(1) Å for all three complexes. Boronhalogen bond lengths average 1·864(4), 2·04(2) and 2·28(2) Å, while B—N bond distances are 1·609(6), 1·60(2) and 1·58(3) Å, respectively, for the chloro through iodo compounds. Bond angles are approximately tetrahedral with the C—N—C angle decreasing by several degrees in the Cl → Br → I series.

Notes: Abstract The stability of a spatial configuration and the coordinating ability of the transition-metal ions are discussed in the MO approach, using the notions of molecular orbital stabilization energy and the bond stabilization energy.

Notes: Summary Computer Simulation of Second Order Faults Faults of the second order can be simulated in the computer with an accuracy hitherto unknown, by using Malina's (1969, 1970) program version of the Finite Element Method. The computations show that stress rearrangements occur with shear movements along the principal fault and with propagation of the fault. These stress rearrangements contribute to the development of new secondary faults. The computed second order faults can be classified according to Chinnery (1966) as shear plane typesA, B, E, andF. Moreover, the computation shows two dominant shear planes which cannot be classified according to Chinnery.

Notes: Zusammenfassung Eine pleistozäne Rutschung bei Kitzbühel/Tirol Bei einem Grabenaushub wurden in Grundmoräne zwei fossile Rutschkörper festgestellt. Ein Beispiel wird anhand von alten Bewegungsstrukturen beschrieben, die durch Oxydationsstreifen abgebildet wurden. Nach dem Geländeschnitt rissen z. T. die alten Schwächestellen infolge geringer Abweichungen der Scherfestigkeit des Materials wieder auf.

Notes: Summary The Mechanical Response of Pre-Fractured Rock in Compression This paper describes experimental procedures and results obtained from an experimental study of pre-cracked rock specimens. In these experiments specimens of Westerly granite and Cedar City tonalite were broken in special fixtures and subsequently retested in a triaxial apparatus. Confining pressures up to 7 kb were employed. The rock specimens were well fragmented during the pre-cracking process. The results indicate a number of interesting features, including the significant retention of load-carrying ability under many stress conditions and an increase in maximum deformation. A comparison is made with frictional data determined elsewhere for Westerly granite; the close agreement in maximum stress suggests the importance of friction in the specimen mechanical behavior.

Notes: Summary The Electro-Magnetic equations of Maxwell, the equation of mechanical motion and the equation of heat flow have been used to solve the one-dimensional problem of Magneto-Thermo-Elastic Disturbances in a semi-infinite bar of variable cross section.

Notes: Summary The spectra of Matsushiro micro-earthquakes were studied using a spectrum analyser and discussed in relation to their magnitude and the epicentral distance. It was found that the spectra of seismic waves by Matsushiro micro-earthquakes did not depend upon the epicentral distance since the sonagrams showed a peak around 5 cps at Matsushiro as well as Suzaka. The spectrum also failed to show any distinct peak for micro-earthquakes of magnitude lower than 1.0 due to the decrease of signal to noise ratio.

Notes: Summary In this paper, the problem on the vibrations of rectangular, elliptical and circular plates of non-isotropic material have been solved by using Galerkin's method. With the help of this method, the same problem for an isotropic circular plate has also been considered at the end.

Notes: Summary An irregular wave group (here called pseudospherical), the existence of which is connected with the velocity boundary at which the velocity decreases discontinuously, is investigated. A schlieren modelling device was chosen for a model investigation of this wave since it permits the investigation of wave fields inside the measured models. The model consisted of two layers of transparent gels, the source lay in the layer of higher velocity. The measurements have shown that an irregular wave in the layer of lower velocity exists only in a certain region along the boundary; its wave front has a spherical form and its intensity decreases rapidly with increasing distance of the source from the boundary. The wave always comes only after the regular refracted wave which conforms with the ray theory. These properties correspond to the properties of a wave first described byOtt [1]3) andBrekhovskikh [2]. In the conclusion of the present paper the possibilities of recording pseudospherical waves in seismology are outlined.

Notes: Summary An empirical investigation has been conducted on the practical methods of obtaining the spectra of micropulsation activity, and the interpretational limits which can be applied to the detailed use of spectra computed by the Power Spectral Density (PSD) method. Results indicate that sufficiently high resolution may be obtained reliably from the PSD method for it to be regarded as a useful improvement over handscaling methods. The limitation is shown to remain in the selection of events rather than in computational or instrumental properties.

Notes: Summary Continuous records of sunshine are available since 1945. These records are carefully checked and interruptions are interpolated by aid of a second station nearby. The homogenized data indicate generally more sunshine from December to May and 15% less from July to November. The fluctuations from one year to the other are rather great, only 1736 hours in 1948 but 2135 hours in 1956. The daily variation is nearly symmetric at M'Bandaka compared to Kinshasa-Binza where are much more clouds in the morning and less in the afternoon. The energetic measurements of global radiation since 1961 show a pronounced minimum in July 346 cal/cm2 d, a secondary maximum in October 416 cal/cm2 d and the principal maximum of 445 cal/cm2 d in March and April. These values are rather low due to clouds as well as to atmospheric turbidity.

Notes: Summary This paper deals with the study of the disturbances in an inhomogeneous semi-infinite viscoelastic bar of Reiss type acted upon by an impulsive force at its finite end, under the influence of a primary static magnetic field.

Notes: Summary Description is made of a compact evaporator of elementary iodine substance and its use for purposes of weather-modification is proposed.

Notes: Summary Expressions are obtained for the currents induced in a conducting sphere placed in an oscillating uniform field. The induced currents are plane circular loops around the axis of symmetry with respect to the external field. Current profiles are presented at three latitudinal planes inside the sphere for three parametric values of $$\sqrt {\omega \mu \sigma /2} $$ that are of importance in prospecting. Magnetic fields created by these currents loops at a point on the axis of the sphere are calculated. This study reveals some interesting results like the existence of zones contributing positively and negatively to the signal measured outside the sphere and behaviour of these zones with parameter.

Notes: Summary Simple delay and sum of sensors in a seismic array is an effective method for noise suppression. However, unless we have precise steering delays, much of the signal energy is lost during the beam forming process too. We have investigated possible error sources in time delay measurements, using a computerized cross-correlation procedure. Parameters perturbed are correlation window length and positioning, signal frequency content and signal to noise ratio (SNR). Our results indicate that relative low frequency waves and using the very first part of theP-signals give the most reliable and stable time delay values. High frequency bandpass filtering improves SNR, but signal correlation and the precision in beam steering corrections decrease. Significant loss of high frequency energy during beamforming seems to be unavoidable.

Notes: Summary The paper deals with the torsional oscillation in a hollow cylinder of visco-elastic material acted upon by a magnetic field. It is assumed that the medium apart from being perfectly conducting, is characterised by a visco-elasticity of general-linear type.