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  • 1980-1984  (3,596)
  • 1965-1969  (4,232)
  • 1890-1899  (8,112)
  • 1810-1819
  • Inorganic Chemistry  (15,815)
  • Insulin
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Keywords
  • 1
    Electronic Resource
    Electronic Resource
    Vanadate stimulates the pumped movements of Na in skeletal muscle (1984)
    Springer
    Pflügers Archiv 400 (1984), S. 413-417 
    Details
    ISSN: 1432-2013
    Keywords: Sodium pump ; Na-K ATPase ; Na fluxes ; Vanadate ; Insulin ; Skeletal muscle ; Ouabain
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract We have measured the effects of concentrations of vanadate ranging between 0.01 and 10 mM on the22Na efflux of frog sartorius muscles. The addition of vanadate had no effects when concentrations lower than 0.5 mM were used; higher concentrations increased Na efflux. The increase was abolished by the addition of ouabain (10−5M). In muscles pretreated with ouabain vanadate did not modify Na efflux. The stimulatory effects of vanadate on Na efflux were also observed in Na-free solutions indicating that the effux of vanadate was not caused mainly either by an increase in the exchange of Na for Na or by an increase in Na entry into the muscle. We also examined the effects of vanadate on muscles immersed in solutions containing 20 mM K+; both vanadate and increased K+ produced stimulations of Na efflux that were additive. Similarly when the effects of vanadate and insulin were measured on the Na efflux of the same muscle, additive effects were found. As the ouabain-sensitive Na efflux in frog muscle is generally agreed to be due to the activity of the Na-K ATPase, our findings suggest that the net effect of vanadate in intact muscle cells is an increase in the activity of the Na pump. Since vanadate affects many enzymes it is quite possible that the stimulatory action is not due to a direct effect on the Na-K ATPase but may be mediated through an intermediary step. Regardless of the specific mechanism, it is evident that, our results as well as other findings in the literature, strongly indicate that Na pumping by intact cells can be increased by vanadate administration. Hence it is not justified to attribute the physiological modifications caused by vanadate administration to blockade of the Na-K ATPase unless the attribution is justified by specific experimental evidence.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00587542
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  • 2
    Electronic Resource
    Electronic Resource
    Factors governing the human immune response to injected insulin (1984)
    Springer
    Diabetologia 26 (1984), S. 266-271 
    Details
    ISSN: 1432-0428
    Keywords: Insulin ; insulin antibody ; immunogenicity ; immune response genes ; haemocyanin ; HLA ; DR7 ; C2 ; C4 ; factor B ; Gm ; C-peptide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Seventy-nine patients were observed prospectively during their initial period of treatment with conventional bovine insulins. Insulin antibody levels 6 months after starting insulin therapy did not correlate with age, gender or β cell function at onset of treatment. Patients who required soluble insulin in addition to isophane insulin developed higher levels of insulin antibody. Patients bearing the HLA-B8, DR3 and C4AQO alleles had lower levels of insulin antibody, whereas those bearing DR7 produced significantly higher levels. Other alleles at the C4A, C4B, C2, factor B or Gm loci did not appear to have a significant effect on insulin antibody production. The hyporesponsiveness of B8/DR3/C4AQO-positive individuals probably reflects a non-specific abnormality of immunity whereas the enhanced responsiveness of those positive for DR7 suggests the presence of a specific immune response gene for insulin
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00283648
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  • 3
    Electronic Resource
    Electronic Resource
    Evidence for post-transcriptional regulation by insulin of 3-hydroxy-3-methylglutaryl coenzyme A reductase and sterol synthesis in human mononuclear leucocytes (1984)
    Springer
    Diabetologia 26 (1984), S. 366-369 
    Details
    ISSN: 1432-0428
    Keywords: Insulin ; 3-hydroxy-3-methylglutaryl coenzyme A ; sterol synthesis ; human mononuclear leucocytes ; post-transcriptional regulation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Incubation of freshly isolated human mononuclear leucocytes in lipid-depleted serum for 4 h resulted in a two-fold increase in 3-hydroxy-3-methylglutaryl coenzyme A (HMG-CoA) reductase activity. Insulin, when added to the incubation medium at concentrations of 10 and 100 nmol/l at zero time, caused additional increases in the enzyme activity of 30% and 37%, respectively. The hormone action was not immediate because no effect was observed when insulin was added at 4 h and activity examined thereafter. Under these conditions sterol synthesis from 14C-acetate and tritiated water was strictly proportional to the activity of HMG-CoA reductase. Cycloheximide (20 μg/ml), a translational inhibitor of protein synthesis, prevented the insulin-mediated increase in the enzyme activity and the incorporation of 14C-acetate into sterols. Cordycepin (50 μg/ml) inhibited messenger RNA synthesis by 〉 50%, but had no inhibitory effect on the induction of HMG-CoA reductase and sterol synthesis. Low density lipoprotein (80 μg protein/ml) and complete serum blocked the induction of the enzyme and sterol synthesis from 14C-acetate caused by lipid-depleted serum. The insulin-effect, however, remained unchanged. The results suggest that insulin may regulate the de novo synthesis of HMG-CoA reductase and accordingly sterol synthesis at a post-transcriptional level.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00266038
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  • 4
    Electronic Resource
    Electronic Resource
    Effect of contact material on vibration-induced insulin aggregation (1984)
    Springer
    Diabetologia 27 (1984), S. 373-378 
    Details
    ISSN: 1432-0428
    Keywords: Insulin ; administration and dosage ; therapeutic use ; insulin infusion devices
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The tendency of insulin to form insoluble aggregates is a major obstacle to the development of implantable insulin infusion systems for treatment of insulin-deficient diabetic patients. A test system was developed to examine the kinetics of insulin aggregation under controlled conditions of temperature, vibration and contact material in an effort to provide design criteria for minimising aggregation. The contact materials tested were all potentially suitable for pump reservoirs on engineering criteria and included metals (stainless steel, titanium and a titanium alloy) and various plastics (polypropylene, polytetrafluoroethylene, Polyvinylchloride, polyamide, cellulose butyrate and silicone elastomer). The rate of insulin aggregation was markedly affected by the nature of the contact material. Hydrophilic materials, particularly polyamide and cellulose butyrate (2% of total insulin aggregated after 96 h vibration), appeared more compatible with insulin stability than did hydrophobic ones, such as polypropylene (16% aggregation) and Polyvinylchloride (37% aggregation). A specially formulated ‘pump’ insulin preparation, stabilised by addition of polyethylenepolypropyleneglycol, was significantly superior (three to five times more stable) to a regular neutral insulin formulation under most, but not all, conditions. Standard clinical syringes (polypropylene) performed poorly with both insulin formulations but especially with the neutral regular insulin (100% aggregation after 96 h vibration). In addition to physical aggregates, significant amounts (5%–30%) of the insulin remaining in solution were no longer detectable by immuno- or receptorassay in all materials tested. Appropriate combinations of insulin formulations and materials can minimise insulin aggregation and denaturation, but since the mechanisms involved are as yet poorly understood, realistic testing of proposed reservoir components and insulin formulations must be a prerequisite in insulin infusion pump planning and design. These testing procedures should be designed to test for denaturation in solution as well as for precipitation of insulin.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00304853
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  • 5
    Electronic Resource
    Electronic Resource
    Effect of co-ingestion of fat on the metabolic responses to slowly and rapidly absorbed carbohydrates (1984)
    Springer
    Diabetologia 26 (1984), S. 50-54 
    Details
    ISSN: 1432-0428
    Keywords: Insulin ; gastric inhibitory polypeptide ; insulin sensitivity ; glucose tolerance ; diabetes ; diet ; fat ; rate of carbohydrate digestion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The present study examined the acute effects of coingestion of fat (37.5 g) on the post-prandial metabolic responses to 75 g of carbohydrate which was either slowly absorbed (lentils) or rapidly absorbed (potatoes). Co-ingestion of fat resulted in a significant flattening of the post-prandial glucose curves, the effect being more pronounced for the rapidly absorbed potatoes. This was probably due to delayed gastric emptying. However, the post-prandial insulin responses to either carbohydrate were not significantly reduced by fat, suggesting that the insulin response to a given glucose concentration was potentiated in the presence of fat. The gastric inhibitory polypeptide (GIP) responses to both carbohydrates were greatly increased in the presence of fat. To investigate further the possible roles of GIP in the entero-insular axis, a 5-g bolus of glucose was injected intravenously 1 h after lentils ± fat. This was sufficient to raise the glucose levels above the threshold reported for GIP to potentiate insulin secretion. However, despite the large differences in circulating GIP levels, the insulin response to glucose was not affected by the presence of fat. These results suggest that (1) the rate of absorption of carbohydrate is a major determinant of post-prandial metabolic responses even in the presence of fat, (2) fat-stimulated GIP secretion does not potentiate glucose-induced insulin secretion, and (3) the potentiation of the insulin response to glucose when carbohydrate is co-ingested with fat is consistent with the well-documented insulin resistance associated with high fat diets.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00252263
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  • 6
    Electronic Resource
    Electronic Resource
    Long-term follow-up of children with craniopharyngioma (1984)
    Springer
    European journal of pediatrics 142 (1984), S. 179-185 
    Details
    ISSN: 1432-1076
    Keywords: Craniopharyngioma ; Growth ; Insulin ; Neurosurgery ; Radiotherapy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract Management of craniopharyngiomas is still controversial. 28 children with this tumor were studied. GH deficiency was present in 22 patients following surgery, 10 of these GH-lacking patients had normal or accelerated growth (usually associated with rapid weight gain) postoperatively. Somatomedin levels were normal in three of six normally growing patients. After craniotomy their basal and TRH-stimulated prolactin levels were in the normal range, but their insulin secretion was markedly increased. Postoperatively there was a significant correlation between peak insulin levels following arginine infusion and growth velocity in all patients. Complete tumor removal could be performed in 28% of our patients. Altogether 36% of all patients had at least one tumor recurrence. Recent literature with the addition of our series showed tumor recurrence in 22% of patients with “total” tumor excision and in 72% of patients with partial tumor removal. Radiotherapy seems to be capable of destroying craniopharyngioma tissue. The recurrence rate was only 26% in patients with subtotal excision plus radiotherapy. Unless radical tumor removal can be attempted with safety, subtotal tumor removal plus radiotherapy appears to be the treatment of choice for craniopharyngioma.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00442445
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  • 7
    Electronic Resource
    Electronic Resource
    Inotropic effect of prenalterol in amitriptyline poisoning (1984)
    Springer
    Intensive care medicine 10 (1984), S. 209-211 
    Details
    ISSN: 1432-1238
    Keywords: Amitriptyline ; Hydrocortisone ; Insulin ; Prenalterol ; Cardiac failure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract A case of severe amitriptyline poisoning with grade IV coma, seizures, bradycardia and hypotension who did not respond to dopamine was successfully treated with prenalterol, a new cardioselective β-agonist. The case is discussed with respect to plasma concentrations of dopamine, prenalterol and amitriptyline. Prenalterol, hydrocortisone and insulin may be useful as inotropic agents in tricyclic poisoning where dopamine fails to provide an adequate response.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00259441
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  • 8
    Electronic Resource
    Electronic Resource
    Energetics of active sodium-potassium transport following stimulation with insulin, adrenaline or salbutamol in rat soleus muscle (1984)
    Springer
    Pflügers Archiv 401 (1984), S. 160-166 
    Details
    ISSN: 1432-2013
    Keywords: Biological transport ; Insulin ; Energy metabolism ; Epinephrine ; Endocrinology ; Albuterol (salbutamol) ; Active sodium-potassium transport ; Muscle
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Abstract The total metabolic energy expenditure associated with active Na−K-transport over the first 20 min of stimulation with insulin, adrenaline or salbutamol (ΔHmNa−K) was determined from direct calorimetric and tracer ion flux measurements in isolated muscles at rest. The reversible work performed by the Na−K-pump during the same interval of time (WrevNa−K) was calculated as the product of the ouabain-suppressible Na−K transfers and the mean free energy increase imparted to the two ions as they are transported against their electrochemical gradients across the plasma membrane. Comparison of membrane potential and intracellular Na and K concentrations before and after the stimulations indicated that part of WrevNa−K had contributed to increase the ion electrochemical gradients in the preparation (i.e. had not been lost as heat) during the 20 min period. Accordingly, the maximum value of ΔHmNa−K was taken as the sum of the ouabain-suppressible heat production and WrevNa−K. Following stimulation with insulin, adrenaline or salbutamol this maximum corresponded to 10, 10 and 12% respectively, of basal metabolism. Under the same three conditions, the minimum “energetic efficiency” of the active Na−K-transport process, defined as the ratio between WrevNa−K and maximum ΔHmNa−K, was 35, 41 and 38%, respectively.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00583876
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  • 9
    Electronic Resource
    Electronic Resource
    Neurotensin — Was ist gesichert über seine Rolle als Hormon im Magen-Darmtrakt? (1984)
    Springer
    Journal of molecular medicine 62 (1984), S. 523-530 
    Details
    ISSN: 1432-1440
    Keywords: Neurotensin ; Gastrointestinal hormones ; Gastric secretion ; Pancreatic secretion ; Motility ; Insulin ; Glucagon
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Neurotensin is a tridecapeptide originally isolated and characterized from bovine hypothalamus and later, in identical form, from bovine and human intestine. In the rat about 85% of immunoreactive neurotensin is found in the gut and about 10% in the brain. When an antibody specific for the amino terminal region of neurotensin was used the highest concentrations were found in the mucosa of the ileum, while an antibody specific for the biologically active region, the carboxyl terminus, also detected large amounts in the mucosa of the upper gastrointestinal tract. After a meal neurotensin — as measured by carboxyl terminal antibodies — rises after 5 min, a time in which the chymus has not yet reached the ileum, the main source of whole neurotensin. It is therefore possible that the carboxyl terminal molecules of neurotensin, found in the upper gastrointestinal tract, play an important physiological role. In plasma, neurotensin is rapidly degraded into smaller amino terminal and therefore biologically inactive molecules. Increases of carboxyl terminal neurotensin have been found in plasma in only a very few studies. The nature of this immunoreactive material has not yet been established. Therefore, the physiological role of neurotensin as a circulating hormone is unknown. Potential actions of neurotensin include thermoregulation, regulation of hormone release from brain (pituitary hormones) and gut (glucagon, insulin, somatostatin, pancreatic polypeptide), increase of vascular permeability, vasodilatation, inhibition of gastric acid secretion, stimulation of pancreatic secretion and changes of gut motility from the fasting to the fed type.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01727746
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  • 10
    Electronic Resource
    Electronic Resource
    Studies on acute glucose-induced aldosterone suppression: Role of renin-angiotensin system (1984)
    Springer
    Journal of molecular medicine 62 (1984), S. 213-217 
    Details
    ISSN: 1432-1440
    Keywords: Aldosterone ; Glucose ; Insulin ; Potassium ; Renin-angiotensin system ; Cortisol ; Captopril
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Glucose loading is known to cause acute suppression of plasma aldosterone and stimulation of plasma renin activity. The relative contribution of variations in circulating angiotensin II to the regulation of aldosterone secretion following glucose loading was assessed in ten normal subjects. The effects of a standard oral glucose loading test (100 g) on plasma concentrations of glucose, insulin, potassium, aldosterone, renin activity and cortisol were studied (a) under basal conditions, and (b) after inhibition of angiotensin II with the converting enzyme inhibitor captopril (50 mg t.i.d. during 3 days). Under basal conditions the acute increase in plasma glucose and insulin after glucose loading was accompanied by a significant decrease (P〈0.01) in plasma cortisol and aldosterone and by a significant increase in plasma renin activity (P〈0.01); plasma potassium was decreased slightly but not significantly. Following captopril treatment preloading plasma renin activity was increased significantly, most probably reflecting an effective reduction of angiotensin II. Glucose loading caused a similar suppression of plasma aldosterone, as observed under basal conditions. This observation suggests that renin activation does not substantially contribute to the acute regulation of plasma aldosterone after an oral glucose load.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01721046
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  • 11
    Electronic Resource
    Electronic Resource
    Effect of continuous and oscillatory portal vein insulin infusion upon glucose-induced insulin release in rats (1984)
    Springer
    Research in experimental medicine 184 (1984), S. 67-71 
    Details
    ISSN: 1433-8580
    Keywords: Oscillations ; Insulin ; Glucose
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary The present study was designed to determine the effect of low dose continuous and oscillatory intraportal insulin infusions upon subsequent glucose-induced insulin release. In overnight-fasted and anesthetized rats with indwelling catheters in the jugular vein, carotic artery, and mesenteric vein insulin was infused intraportally for 3 h via the mesenteric vein catheter at a continuous rate of 45 µU/kg·min, or the same amount of insulin was administered at alternating high (72 µU/kg·min) and low infusion rates (18 µU/kg·min), respectively, in 2-, 4-, 8-, and 16-min cycles (oscillatory infusions). Another group received a continuous infusion of saline. Glucose (0.4 g/kg) was given i.v. 30 min after the end of the insulin or saline infusion. During the 3-h infusion of insulin or saline the peripheral glucose level remained unchanged in all groups. In response to the i.v. glucose load peripheral arterial plasma insulin levels were significantly elevated after preceding oscillatory infusions compared to the continuous insulin infusion. As compared to the group receiving saline the glucose-induced insulin response after continuous insulin infusion was significantly reduced. The plasma glucose responses were not different except for inexplicably elevated glucose levels in the 4-min cycle group. No difference was observed for plasma glucagon levels in all groups. The present data demonstrate an augmented responsiveness of theβ-cell to glucose after a preceding oscillatory infusion of insulin and an impaired responsiveness to glucose after continuous insulin infusion. This indicates that an oscillatory insulin release might be of importance for an adequate regulation ofβ-cell function.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01852224
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  • 12
    Electronic Resource
    Electronic Resource
    Metabolic and hormonal responses to prolonged physical exercise in dogs after a single fat-enriched meal (1984)
    Springer
    European journal of applied physiology 53 (1984), S. 267-273 
    Details
    ISSN: 1439-6327
    Keywords: Exercise ; Triglycerides ; Free fatty acids ; Glycerol ; Insulin ; Catecholamines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Metabolic and hormonal responses to prolonged treadmill exercise in dogs fed a fat-enriched meal 4 h prior to the exercise were compared to those measured 4 h after a mixed meal or in the postabsorptive state. Ingestion of the fat-enriched meal caused significant elevations in the resting values of plasma triglyceride (TG), free fatty acid (FFA), and glycerol concentrations. A reduction of the plasma TG concentration (from 1.6±0.2 to 1.1±0.10 mmol·l−1,P〈0.005) occurred only in dogs exercising after the fat-enriched meal. No significant changes in this variable were noted in dogs fed a mixed meal, whilst in the postabsorptive state exercise caused an increase in the plasma TG level (from 0.42±0.03 to 0.99±0.11 mmol·l−1,P〈0.01). The exercise-induced elevations in plasma FFA and glycerol concentrations were the highest in the dogs given the fat-enriched meal. Plasma glycerol during exercise correlated with the initial values of circulating TG (r=0.73). The plasma FFA-glycerol ratio, at the end of exercise was lowest in the dogs taking the fat-enriched meal (1.39±0.19), suggesting an increased utilization of FFA in comparison with that in the postabsorptive state (3.27±0.37) or after a mixed meal (2.88±0.55). Basal serum insulin (IRI) concentrations were similarly enhanced in dogs fed fat-enriched and mixed meals, and they were reduced to control values within 60 min of exercise. Plasma adrenaline and noradrenaline concentrations correlated with time of exercise (r=0.84 andr=0.96, respectively) and were unaffected by the nutritional modifications. It is concluded that ingestion of a single fat-enriched meal considerably modifies the exercise-induced changes in lipid metabolism. The pattern of changes in plasma TG, FFA, and glycerol concentrations indicates an enhanced hydrolysis of plasma chylomicron-TG, suggesting that this lipid source may contribute markedly to exercise metabolism.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00776601
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  • 13
    Electronic Resource
    Electronic Resource
    Further increase in high density lipoprotein in trained males after enhanced training (1984)
    Springer
    European journal of applied physiology 52 (1984), S. 426-430 
    Details
    ISSN: 1439-6327
    Keywords: Apoproteins ; Lipoproteins ; Insulin ; Blood lactate ; Physical training
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary Eight well-trained males were studied before, during and after 6 months of a progressively increased amount of endurance training in order to elucidate the effects on the apoproteins and apo-lipoproteins. Initially high HDL-cholesterol levels were revealed (1.62±0.15 mmol×l−1, mean ± SE.). After a transient but not significant, slight decline at the onset of the increased training program (1.57±0.06 mmol×l−1) HDL-cholesterol increased gradually to the end of the training period (1.92±0.12 mmol×l−1). There was an increased aerobic capacity as judged by maximal oxygen uptake and by lactate concentration during standardized submaximal work. However, at the end of the training period, a levelling off in maximal oxygen uptake was revealed, while HDL-cholesterol was still increasing. The present data demonstrate that HDL can be influenced by training at all levels of aerobic capacity.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00943374
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  • 14
    Electronic Resource
    Electronic Resource
    Effects of a rapid change in muscle glycogen availability on metabolic and hormonal responses during exercise (1984)
    Springer
    European journal of applied physiology 53 (1984), S. 57-62 
    Details
    ISSN: 1439-6327
    Keywords: Muscle glycogen ; Time sequence ; Free fatty acids ; Insulin ; Exercise in humans
    Source: Springer Online Journal Archives 1860-2000
    Topics: Medicine
    Notes: Summary To evaluate the metabolic and hormonal adaptations following a rapid change in muscle glycogen availability, 14 subjects had their muscle glycogen content increased in one leg (IG) and decreased in the other (DG). In group A (n=7), subjects exercised on a bicycle ergometer at 70% maximal oxygen uptake for 20 min using the DG leg. Without resting these same subjects exercised another 20 min using the IG leg. Subjects in group B (n=7) followed the same single-leg exercise protocol but in the reverse order. In order to get some information on the time sequence of these possible adaptations, blood samples were collected at rest and at the beginning and the end of each exercise period (min 5, 20, 25, and 40). Results indicated that 5 min after the switch from the DG leg to the IG leg. transient increases in plasma free fatty acids (1.20 to 1.39 meq·l−1) and serum insulin (10.1 to 12 mU·l−1) concentrations occured. Between minute 25 and 40 of exercise, the DG to IG switch was accompanied by a decrease in free fatty acids and glycerol concentrations as well as an increase in lactate levels. An opposite response was observed in the IG to DG condition during the same time span. Plasma norepinephrine, epinephrine, glucagon, and serum cortisol concentrations were not significantly affected by the leg change. These results suggest a rapid preferential use of muscle glycogen when available and a time lag in the response of the extramuscular substrate mobilization factors.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00964691
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  • 15
    Electronic Resource
    Electronic Resource
    Effects of prolonged maternal fast on the pancreas of 18–21-day-old foetal rats (1984)
    Springer
    Cell & tissue research 237 (1984), S. 169-179 
    Details
    ISSN: 1432-0878
    Keywords: Foetal pancreas ; β Cells ; Insulin ; Fasting mothers ; Morphometry ; Rat
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Medicine
    Notes: Summary After maternal fasting for 72 h the pancreatic β cells of 18-day-old foetal rats show a conspicuous enrichment in secretory material, with an increase of pancreatic insulin concentration and a marked development of the rough endoplasmic reticulum and the Golgi apparatus. The morphometric analysis shows that the intracytoplasmic migration of the secretory granules is inhibited, principally inside the cell web. Consequently the number of secretory granules fused with plasma membrane decreases and this is associated with a decreased foetal plasma insulin. The difference in the ultrastructural aspect of the β cells of foetuses from fasting mothers and of foetuses from fed mothers is less conspicuous at 19 days of gestation and progressively disappears at 20 and 21 days. The modifications in ultrastructural aspect and in functional state are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00229213
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  • 16
    Electronic Resource
    Electronic Resource
    Coordination Complexes of Some Group(IV) Halides with Monodentate Schiff Bases (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 187-190 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Komplexe von Halogeniden der IV. Gruppe mit einzähnigen Schiffschen BasenVerschiedene Komplexe, die bei der Reaktion von N-(phenyl)benzalaldimin und seinen Derivaten mit einer Methylgruppe in verschiedenen Positionen des Anilinringes mit Halogeniden der IV. Gruppe, MX4, (M = Si bzw. Sn und X = Cl bzw. Br) entstehen, wurden hergestellt und mittels UV-, IR- und Raman-Spektren charakterisiert.
    Notes: Coordination compounds resulting from the interaction of N-(phenyl)benzalaldimine and its derivatives containing a methyl group in different positions of the aniline ring and group(IV) halides, MX4 (where M = Si or Sn and X = Cl or Br), have been prepared and characterized by elemental analyses and electronic, infrared and Raman spectra.
    Additional Material: 4 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845080126
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  • 17
    Electronic Resource
    Electronic Resource
    Neue Beobachtungen zum chemischen Transport von GeO2. V. Zur Mineralisatorwirkung von Na-Verbindungen auf den Modifikationswechsel von GeO2 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 208-208 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845080130
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  • 18
    Electronic Resource
    Electronic Resource
    Beiträge zur Chemie des Phosphors. 134. Über die Triphosphane H(t-BuP)3H, Li(t-BuP)3Li und Me3Si(t-BuP)3SiMe3 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 38-52 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Phosphorus. 134. On the Triphosphanes H(t-BuP)3H' Li(t-BuP)3Li, and Me3Si(t-BuP)3SiMe3The reaction of 1,3-diiodo-1,2,3-tri-tert-butyltriphosphane, I(t-BuP)3I, with lithium aluminium hydride leads to 1,2,3-tri-tert-butyltriphosphane, H(t-BuP)3H (1). 1 reacts with n-butyllithium to 1,3-dilithium-1,2,3-tri-tert-butyltriphosphide, Li(t-BuP)3Li (2), which reacts further with trimethylchlorosilane yielding 1,3-bis(trimethylsilyl)-1,2,3-tri-tert-butyltriphosphane, Me3Si(t-BuP)3SiMe3 (3). The triphosphanes 1, 2 and 3 could be isolated in a pure state. In solution 1 forms the threo, threo and the threo,erythro configurated diastereomers 1a and 1b in a ratio of about 2:1. 3 predominantly exists in form of the threo,erythro configurated diastereomer 3b by steric reasons.
    Notes: Die Umsetzung von 1,3-Diiod-1,2,3-tri-tert-butyltriphosphan, I(t-BuP)3I, mit Lithiumaluminiumhydrid führt zu 1,2,3-Tri-tert-butyltriphosphan, H(t-BuP)3H (1). 1 reagiert mit n-Butyllithium zu 1,3-Dilithium-1,2,3-tri-tert-butyltriphosphid, Li(t-BuP)3Li (2), das mit Trimethylchlorsilan weiter zu 1,3-Bis(trimethylsilyl)-1,2,3-tri-tert-butyltriphosphan, Me3Si(t-BuP)3SiMe3 (3), umgesetzt werden kann. Die Triphosphane 1, 2 und 3 konnten in reiner Form isoliert werden. In Lösung bildet 1 die threo, threo- und threo,erythro-konfigurierten Diastereomere 1 a und 1 b im Verhältnis von etwa 2:1. 3 liegt aus sterischen Gründen hauptsächlich in Form des threo, erythro-konfigurierten Diastereomers 3 b vor.
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    URL: http://dx.doi.org/10.1002/zaac.19845090204
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    Oxydationsprodukte intermetallischer Phasen. III. Tieftemperaturformen von K2Sn2O3 und Rb2Sn2O3 und eine Notiz über K2Ge2O3 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 145-152 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Oxidation Products of Intermetallic Compounds. III. Low Temperature Forms of K2Sn2O3 and Rb2Sn2O3 and a Notice about K2Ge2O3By controlled oxidation of KSn (at 320°C) and RbSn (at 410°C) with O2 the hitherto unknown low temperature forms of K2Sn2O3 (a = 8.4100(8) Å) and Rb2Sn2O3 (a = 8.6368(8) Å) are obtained, which are isotopic with cubic K2Pb2O3. Oxidation at higher temperatures (at 510-5207°C) leads to the well-known HT-forms. The Madelung Part of Lattic Energie, MAPLE, is calculated for both compounds.K2Pb2O3, Rb2Pb2O3, Cs2Pb2O3, and Cs2Sn2O3 have been prepared too by oxidation of KPb, RbPb, CsPb, and CsSn.Oxidation of KGe (at 400°C) leads to the first oxogermanate(II), K2Ge2O3 (cubic a = 8.339(1) Å, isotypic with K2Pb2O3) together with K6Ge2O7.
    Notes: Aus KSn bzw. RbSn entstehen durch direkte Oxydation K2Sn2O3 bzw. Rb2Sn2O3 bei 320°C bzw. 410°C die bislang unbekannten „Tieftemperaturformen“ (a = 8,4100(8)Å bzw. a = 8,6368(8)Å), isotyp mit kubischem K2Pb2O3. Bei höherer Temperatur (510 bzw. 520°C) entstehen die bekannten Hochtemperaturformen.Der Madelunganteil der Gitterenergie, MAPLE, wird berechnet und diskutiert.Ebenso erhält man durch direkte Oxydation von KPb, RbPb, CsPb und CsSn die Oxide K2Pb2O3, Rb2Pb2O3, Cs2Pb2O3 und Cs2Sn2O3. Durch Oxydation von KGe wurde bei 400°C erstmals K2Ge2O3 (kubisch a = 8,339(1) Å; isotyp mit K2Pb2O3) neben K6Ge2O7 erhalten.
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    URL: http://dx.doi.org/10.1002/zaac.19845090215
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  • 20
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    The Reaction of SnCl2 with Br2 and I2 in Weak Donor Solvents (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 174-182 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die Reaktion des SnCl2 mit Br2 und I2 in schwachen Donor-LösungsmittelnEs wurden die Verbindungen SnCl2Br2(MeCN)2, “Sn3Cl8Br4(THF)6” und “Sn3Cl10Br2(OEt)6” durch Reaktion zwischen SnCl2 und Br2 in Acetonitril (MeCN), Tetrahydrofuran (THF) und Diethylether (OEt2) gewonnen. Die zwei letzten Verbindungen sind feste Lösungen von SnCl4L2 und SnCl2Br2L2 (L = THF, OEt2) jeweils im Verhältnis 1:2 und 2:1. Die Verbindungen wurden mit Hilfe von IR-, Raman- und Mößbauer-Spektroskopie charakterisiert. Es wurde C1-Symmetrie für SnCl2Br2(MeCN)2 und C2v mit den Liganden in trans-Position für SnCl2Br2L2 (L = THF, OEt2) gefunden. Das bisher nicht bekannte Mößbauer-Spektrum des SnBr4(THF)2 wurde gemessen und ebenfalls die Reaktion zwischen SnCl2 und I2 in denselben Lösungsmitteln studiert. Die Bildung des SnCl4L2 (L = MeCN, THF, OEt2) SnI4 und einer kleinen Menge des SnI3Cl wurde beobachtet und Raman-spektroskopisch identifiziert.
    Notes: The compounds SnCl2Br2(MeCN)2, “Sn3Cl8Br4(THF)6”, and “Sn3Cl10Br2(OEt2)6” were obtained by reaction between SnCl2 and Br2 in acetonitrile (MeCN), tetrahydrofuran (THF) and diethyl ether (OEt2). The two last are solid solutions of SnCl4L2 and SnCl2Br2L2 (L = THF, OEt2) in the proportions 1:2 and 2:1, respectively. The compounds are characterized by IR, Raman, and Mössbauer spectroscopy, a C1 symmetry being found for SnCl2Br2 (MeCN)2 together with a C2v symmetry, with the ligands in trans positions, for SnCl2Br2L2 (L = THF, OEt2). The Mössbauer spectrum of SnBr4(THF)2 was also obtained, which has not previously been reported. The reaction between SnCl2 and I2 has also been studied in the same solvents, and the formation of SnCl4L2 (L = MeCN, THF, OEt2), SnI4, and a small amount of SnI3Cl was observed, which have been identified by Raman spectroscopy.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845090219
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  • 21
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    Cobalt(II) Complexes of 4,6-Dimethylpyrimidine-2(1H)-one (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 192-200 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Einige Cobalt(II)-Komplexe von 4,6-Dimethylpyrimidin-2(1H)-on (HL) wurden dargestellt und mittels IR- und Elektronenspektren magnetochemisch und konduktometrisch untersucht. Der Ligand wird über das nicht protonierte N-Ringatom angelagert und in einem Fall auch über das O-Atom der Carbonylgruppe. Die “blauen” Komplexe [CoX2 · 2HL] (X2 = Cl2, CBr, Br2, (NCS)2) und [CoX2 · 2HL] · 2HL (X = Cl, Br) haben eine verzerrte C2v-Anordnung [CoX2N2]; die Thiocyanate sind über die N-Atome an das Metall gebunden. Die „grünen“ Komplexe CoX2 · 2HL (X = Cl(4H2O), Br) besitzen eine quadratisch-pyramidale Anordnung [CoX2N2O]. Die „rosa“ Komplexe CoX2 · 4HL · nH2O (X = ClO4, n = 2, X = BF4, n = 8, CF3CO2, n = 4) und die „cremefarbigen“ CoX2 · 4HL · 6H2O (X = J, ClO4) zeigen oktaedrische Anordnung; nur CF3CO2- ist koordiniert. Die „veilchenfarbenen“ Komplexe CoAcL · 2HL · 2H2O und Co3Ac4L2 · 2HL · 2H2O haben eine mehrkernige Struktur; das Acetation betätigt sich als zweizähniger Ligand.
    Abstract: CoII-Komplexe von 4,6-Dimethylpyrimidin-2(1H)-on
    Notes: Some cobalt(II) complexes of 4,6-dimethylpyrimidine-2(1H)-one (HL) have been prepared and studied by infrared and electronic spectra and by magneto-chemical and conductometric measurements. The ligand is coordinated through the unprotonated ring-nitrogen atom and in one case also through the carbonylic oxygen atom. The “blue” complexes [CoX2 · 2HL] (X2 = Cl2, ClBr, Br2, (NCS)2) and [CoX2 · 2HL] · 2HL (X = Cl, Br) have a distorted C2v [CoX2N2] coordination; the thiocyanate ion is N-bonded to the metal. The “green” complexes CoX2 · 2HL (X = Cl(4H2O), Br) have a square-pyramidal [CoX2N2O] coordination. The “pink” CoX2 · 4HL · nH2O (X = ClO4, n = 2; X = BF4, n = 8; X = F3Ac, n = 4) and “cream” CoX2 · 4HL · 6 H2O (X = I, ClO4) complexes have an octahedral coordination; only the F3Ac- ion is coordinated. The “cyclamen” CoAcL · 2HL · 2 H2O and Co3Ac4L2 · 2HL · 2H2O complexes have a polynuclear constitution; the Ac- ion behaves as bidentate ligand.
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    URL: http://dx.doi.org/10.1002/zaac.19845090221
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  • 22
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    Raman-spektroskopische Untersuchungen an koordinationspolymeren Metall-tricyanmethaniden M[C(CN)3]2 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 31-36 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Raman Spectroscopic Investigations of Coordination Polymeric Metal TricyanmethanidesThe Raman spectra of 3d-metal tricyanmethanides M{C(CN)3}2 as well as of [Ni{C(CN)3}2py2] are investigated. The observed Raman lines are assigned, characteristic variations of position and intensity of these lines are discussed.
    Notes: Es werden die Ramanspektren der koordinationspolymeren 3d-Metalltricyanmethanide M{C(CN)3}2 (M = Mn, Fe, Co, Ni, Zn) sowie von [Ni{C(CN)3}2py2] untersucht. Die beobachteten Ramanlinien werden zugeordnet, charakteristische Variationen der Lage und Intensität dieser Linien werden diskutiert.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19845100306
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  • 23
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    Zur Chemie und Strukturchemie der Phosphide und Polyphosphide. 34 [1] Dampfdruckuntersuchungen am System Europium-Phosphor (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 51-60 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemistry and Structural Chemistry of Phosphides and Polyphosphides. 34. Vapor Pressure Measurements in the Europium-Phosphorus SystemThe vapor pressure of the europium phosphides EuP7, α-EuP3, ß-EuP3, EuP2 and Eu3P4 were measured using the Knudsen-Effusion technique. These compounds were vaporized incongruently according to the general reaction a EuPm, (s) = a EuPn, (s) + P4, (g) where a (m - n) = 4. The following enthalpies and entropies of reaction were calculated (δH)kJ · mol-1/δS (J · K-1 mol-1)/ T(K). [δH/δS/T]: EuP7 → ß-EuP3 [191/215/698]; α-EuP3 → EuP2 [212/162/847]; ß-EuP3 → EuP2 [261/212/847]; EuP2 → Eu3P4 [209/144/868]; Eu3P4 → EuP [240/131/1110]. The temperature and pressure ranges over which these phosphides exist were determined from the above values. Standard enthalpies of formation relative to EuP(s) were calculated by combining different reaction enthalpies. The results demonstrate the relatively high stability of ß-EuP3, EuP7 and the instability of EuP2.
    Notes: Für die Europiumphosphide EuP7, α-EuP3, ß-EuP3, EuP2 und Eu3P4 wurden die Dampfdrucke der inkongruenten Verdampfungsreaktionen a EuPm, (f) = a EuPn, (f) + P4, (g) mit a(m - n) = 4 mit der Knudsen-Methode gemessen. Zur Abspaltung von einem Mol P4,(g) wurden bei den mittleren Temperaturen T(K) die folgenden Reaktionsenthalpien δH(kJ · mol-1) und Reaktionsentropien δS(J · K-1 · mol-1) erhalten: [δH/δS/T]: EuP7 β ß-EuP3 [191/215/698]; α-EuP3 → EuP2 [212/162/847]; ß-EuP3 → EuP2 [261/212/847]; EuP2 → Eu3P4 (209/144/868); Eu3P4 → EuP [240/131/1110]. Hierdurch wurden die Existenzfelder der verschiedenen Europiumphosphide in Abhängigkeit von Druck und Temperatur festgelegt. Durch Kombination der verschiedenen Reaktionsenthalpien werden die Standardbildungsenthalpien der Phosphide relativ zu EuP berechnet. Sie zeigen die hohe Stabilität von ß-EuP3 und EuP7 sowie die Instabilität von EuP2.
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    URL: http://dx.doi.org/10.1002/zaac.19845100309
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    Synthese und Kristallstruktur von (PPh4)2[Mo2Cl10] (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 86-92 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Crystal Structure of (PPh4)2[Mo2Cl10]The title compound is obtained in the reaction of [MoCl4(Ph—C≡C—Ph)]2 with tetraphenylphosphonium chloride in dichloro methane, forming brown crystals. It is characterized by the i.r. spectrum and a crystal structure analysis by the aid of X-ray diffraction data. The complex crystallizes triclinic in the space group P1 with one formula unit per unit cell. The cell dimensions are a = 1122 pm, b = 1137 pm, c = 1283 pm; α = 63.4°, β = 69.1°, γ = 86.5°. The crystal structure determination (2959 observed, independent reflexions, R = 4.5%) shows the constants of the unit cell to consist of on centrosymmetric anion, two cations and one disordered molecule of dichloro methane. The distance Mo—Mo in the anion is 380 pm, which excludes direct magnetic interaction between the molybdenum atoms.
    Notes: Die Titelverbindung entsteht in Form brauner Kristalle durch Umsetzung von [MoCl4(Ph—C≡C—Ph)]2 mit Tetraphenylphosphoniumchlorid in Dichlormethan; sie wird durch das IR-Spektrum und durch eine Kristallstrukturbestimmung charakterisiert. Der Komplex kristallisiert triklin in der Raumgruppe P1 mit einer Formeleinheit pro Elementarzelle. Die Zellparameter betragen a = 1122 pm, b = 1137 pm, c = 1283 pm, α = 63,4°, β = 69,1°, γ = 86,5°. Die röntgenographische Kristallstrukturbestimmung (2959 beobachtete, unabhängige Reflexe, R = 4,5%) zeigt, daß die Struktur aus zentrosymmetrischen, dimeren Anionen, isolierten Kationen, und einem fehlgeordneten Molekül Dichlormethan pro Elementarzelle besteht. Der Mo—Mo-Abstand im Anion beträgt 380 pm, was eine direkte magnetische Wechselwirkung zwischen den Mo-Atomen ausschließt.
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    URL: http://dx.doi.org/10.1002/zaac.19845080113
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    Synthese und Röntgenstrukturanalyse von Tris(diethyldithiocarbamato) dimethylphenylphosphantechnetium(III), einem Technetium-Komplex mit der Koordinationszahl 7 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 117-122 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Crystal and Molecular Structure of Tris(diethyldithiocarbamato)dimethylphenylphosphinetechnetium (III)The title compound Tc(S2CNEt2)3(Me2PhP) I has been prepared by the reaction of TcCl3(Me2PhP)3 with NaS2CNEt2. The crystal structure of I has been determined by single-crystal X-ray diffraction methods at room temperature. Crystals are rhombic, space group P212121, with a = 8.708(1), b = 12.012(1), c = 29.626(3) Å and Z = 4. The compound consists of discrete I molecules. The technetium atom has a seven-coordinated environment which is best described as a distorted pentagonal bipyramid. The Tc - P distance (2.330(3) Å) is remarkably short compared with other technetium complexes with mono-dentate phosphine ligands.
    Notes: Die Titelverbindung Tc(S2CNEt2)3(Me2PhP) I wurde durch Reaktion von TcCl3(Me2PhP)3 mit NaS2CNEt2 dargestellt und ihre Kristall- und Molekülstruktur durch Röntgenstrukturanalyse ermittelt. Die Kristalle sind rhombisch, Raumgruppe P212121, mit a = 8,708(1), b = 12,012(1), c = 29,626(3) Å und Z = 4. Die Verbindung besteht aus diskreten monomeren Molekülen. Das Technetiumatom hat siebenfache Koordination, die am besten als geringfügig verzerrte pentagonale Bipyramide beschrieben werden kann. Die Tc - P-Bindungslänge (2,330(3) Å) ist bemerkenswert kurz im Vergleich zu anderen Technetiumkomplexverbindungen mit einzähnigen Phosphanen.
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    Ein Beitrag zur Struktur geschmolzener Mischungen aus Alkalimetall- und Erdalkalimetallhalogeniden, dargestellt an ihren thermodynamischen Eigenschaften (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 152-162 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermodynamics and Structure of Molten Mixtures Alkali Halide-Alkaline Earth HalideThermodynamic quantities ai, fi, GE, and SE were calculated on the basis of vapour pressures of molten mixtures of the type alkali halide-alkaline earth halide. Negative deviations from ideality were found in all systems. The influence of cations or anions on the properties of mixtures is discussed. There is a good correlation between GE and the change of polarization energy δEp. Strong ionic interactions were found in molten mixtures, especially in the system RbBr - CaBr2. The existence of stable complex ions in melts could not be shown by Raman spectroscopy.
    Notes: Aus den Dampfdrücken der geschmolzenen Mischungen vom Typ Alkalimetallhalogenid-Erdalkalimetallhalogenid wurden die thermodynamischen Daten ai, fi, GE sowie Orientierungswerte für SE berechnet. In allen Systemen treten z. T. beträchtliche negative Abweichungen von der Idealität auf. An ausgewählten Beispielen wird der Einfluß der Kationen bzw. Anionen auf die Mischungseigenschaften diskutiert. Für die GE-Werte ergibt sich eine gute Korrelation mit der Änderung der Polarisationsenergie δEp. Ramanspektroskopische Untersuchungen konnten die Existenz stabiler komplexer Ionen nicht belegen, weisen aber besonders bei den Mischungen RbBr - CaBr2 auf starke interionische Wechselwirkungen hin.
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    URL: http://dx.doi.org/10.1002/zaac.19845100321
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    Solid-State Equilibria in the MoO3 - TeO2 - Al2O3 System (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 189-193 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Die binären und ternären Gleichgewichte im System MoO3 - TeO2 - Al2O3 wurden rötgenographisch untersucht. Bei 750°C in Luft wurden in diesem System die im Abstract angegebenen koexistierenden Bereiche gefunden. Eine Bildung ternärer Verbindungen konnten im untersuchten Temperaturbereich (450 - 750°C) nicht beobachtet werden.
    Notes: The binary and ternary equilibrium reactions of Al2O3 with TeO2 and MoO3 were studied by X-ray diffraction methods and the following compatibility ranges were determined in the TeO2 - MoO3 - Al2O3 system at 750°C in air: TeO2, Te2MoO7, Al2TeO6; Te2MoO7, MoO3, Al2TeO6; MoO3, Al2(MoO4)3, Al2TeO6; Al2(MoO4)3, Al2O3, Al2TeO6. Ternary compound formation was not observed in the temperature range investigated (450 - 750°C).Phasengleichgewichte im System MoO3 - TeO2 - Al2O3.
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    URL: http://dx.doi.org/10.1002/zaac.19845100326
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    NMR-spektroskopische Untersuchungen an 15N-markierten N-Phosphorylphosphazenen und Imidodiphosphorsäure-DerivatenProfessor Hans-Albert Lehmann zum 65. Geburtstage am 1. Mai 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 7-18 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: N.M.R. Spectroscopic Studies of 15N Labelled N-Phosphorylphosphazenes and Imidodiphosphoric Acid Derivatives15N labelled compounds were prepared and investigated by means of 31P- and 15N-NMR spectroscopy. The chemical shift values δP and δN, and the coupling constants 1JPN and 2JPP are discussed and interpreted qualitatively by semiempirical quantumchemical calculations (CNDO/2) using POPLE'S ΔE-model.
    Notes: 15N-markierte Verbindungen der Substitutionsreihen wurden synthetisiert und mit Hilfe der 31P- und 15N-NMR-Spektroskopie untersucht. Die chemischen Verschiebungen δP und δN sowie die Kopplungskonstanten 1JPN und 2JPP werden diskutiert und qualitativ mit Hilfe halbempirischer quantenchemischer Rechnungen (CNDO/2) im Rahmen des POPLE-schen ΔE-Modells interpretiert.
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    URL: http://dx.doi.org/10.1002/zaac.19845110402
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    Zur Umsetzung des Zweikomponentensystems Triethylphosphit/Tetrachlorkohlenstoff mit wasserstoffhaltigen Nucleophilen 1. Die Reaktion mit SäureamidenProfessor Hans-Albert Lehmann zum 65. Geburtstage am 1. Mai 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 51-56 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reaction of the Two-component System Triethylphosphite/Carbon Tetrachloride with Nucleophiles Containing Hydrogen. 1. Reaction with Acyl AmidesAcyl amides react with the two-component system triethylphosphite/carbon tetrachloride yielding N-acyl phosphazenes, (EtO)3P=N—Ac. In this way (EtO)3P=N—P(O)(OEt)2, (EtO)3P=N—CN, (EtO)3P=N—C(O)Ph, and (EtO)3P=N—SO2Ph were prepared. Ethyl esters of phosphoric acid and trichloromethane phosphonic acid were obtained as by-products.
    Notes: Säureamide reagieren mit dem Zweikomponentensystem Triethylphosphat/Tetrachlorkohlenstoff zu N-Acylphosphazenen, (EtO)3P=N—Ac. Auf diese Weise wurden aus entsprechenden Amiden (EtO)3P=N—P(O)(OEt)2, (EtO)3P=N—CN, (EtO)3P=N—C(O)Ph und (EtO)3P=N—SO2Ph dargestellt. Als Nebenprodukte werden Phosphorsäureethylester und Trichlormethanphosphonsäureester erhalten.
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    Diskrete polynukleare Metall-Komplexe aus Polysulfid-Lösungen: [Cu6S17]2-, ein ungewöhnlicher binärer CuI-Komplex mit verschiedenen bemerkenswerten strukturellen Eigenschaften (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 84-88 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Discrete Polynuclear Metal Complexes from Polysulfide Solutions: [Cu6S17]2-, a Novel Binary Polynuclear CuI Complex with Several Remarkable Structural FeaturesThe complex [Cu6S17]2-, obtained from Cu(acac)2 and an ethanolic polysulfide solution, contains an unusual arrangement of the metal atoms and novel types of ligand coordination, particularly of polysulfido (S42- and S52-) ions. The relevance of the synthesis with respect to the “dilemma of transporting metals together with sulfur” for the process of metal sulfide rock formation is evidenced. (PPh4)2[Cu6S17] crystallizes in the space group C2/c with Z = 4 (for further details see Inhaltsübersicht).
    Notes: Der Komplex [Cu6S17]2-, der als Tetraphenylphosphonium-Salz (1) aus Cu(acac)2 und einer ethanolischen Polysulfidlösung erhalten wurde, zeigt eine ungewöhnliche Anordnung der Metall-Atome und eine neuartige Koordination von Polysulfidoliganden (S42- und S52-). Auf die Relevanz der Synthese bezüglich der Problematik der Entstehung von Metall-Sulfid-Mineralien wird hingewiesen. 1 kristallisiert monoklin in der Raumgruppe C2/c mit Z = 4 (Gitterdimensionen a = 20,270(7), b = 11,605(5), c = 26,331(9) Å, β = 109,68(4)°).
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    Bildung siliciumorganischer Verbindungen. 97. Über den Einfluß der Si-Substituenten (Me, Cl) auf Bildung und Reaktion von Yliden (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 108-131 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation of Organosilicon Compounds. 97. About the Influence of the Si-Substituents (Me, Cl) upon the Formation and the Reactions of Ylides1,3-disilapropanes with different grade of chlorination or methylation at the silicon atoms and containing a CCl2 group cleave the Si—P bond of Me3SiPMe2. By subsequent rearrangement ylides with = PMe2Cl group are formed. The reactivity of the CCl2 group depends on the grade of Si-chlorination resp. Si-methylation. Si-methylation decreases the reactivity of the CCl2 group. The reaction of 1,3-disilapropanes and Me3SiPMe2 (molar ratio 1:1) runs in a sequence shown in “Inhaltsübersicht”. Ylid C is able either to react with the initial compound A forming B, or in competition decomposes forming D. Reacting Si-perchlorinated carbosilanes, the decomposition forming D is not to be observed. In Si-methylated ylides like (Me3Si)2C=PMe2—PMe2 and (Me3Si)2C=PMe2—P(Me)SiMe3 the ylid carbon atom is able to abstract a proton of the P—CH3 group resp. P—H groups of the trivalent phosphorus forming (Me3Si)2C(H)PMe2. The rearrangement is proved by deuterated derivatives. The different behaviour is due to the increased basicity of the ylid-C atom in Si-methylated phosphorus ylides. Quite the same behaviour show the phosphorus ylides of 1,3,5-trisilacyclohexane.
    Notes: Die am Si-Atom unterschiedlich chlorierten und methylierten 1,3-Disilapropane mit der CCl2-Gruppe ermöglichen die Spaltung von Me3Si—PMe2 unter Bildung der P-halogenierten Phosphorylide, wobei mit steigendem Methylierungsgrad die Reaktivität abnimmt. Die Umsetzungen verlaufen in folgender Reaktionsfolge: Das Ylid C kann mit der nicht umgesetzten Ausgangsverbindung A zu B zurückreagieren oder es zersetzt sich in einer Konkurrenzreaktion zu D. Bei Si-chlorierten Yliden wird die Bildung von D nicht beobachtet. In Si-methylierten Yliden wie (Me3Si)2C=PMe2—PMe2 und (Me3Si)2C=PMe2—P(Me)SiMe3 vermag das Ylid-C-Atom ein H-Atom aus der P—CH3-Gruppe oder der PH-Gruppe des dreibindigen Phosphors zu abstrahieren unter Bildung von (Me3Si)2C(H)PMe2. Die Umlagerung wird anhand deuterierter Derivate belegt. Das unterschiedliche Verhalten wird auf die erhöhte Basizität des Ylid-C-Atoms in den Si-methylierten Phosphoryliden zurückgeführt. Ganz entsprechend verhalten sich die Phosphorylide 1,3,5-Trisilacyclohexans.
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    Polymorphie von SrTa2O6 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 176-184 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polymorphism of SrTa2O6Orthorhombic SrTa2O6 is a new low temperature modification related to orthorhombic CaTa2O6. SrTa2O6(orh.) was obtained when the wellknown modification SrTa2O6(TTB) which is related to the tetragonal tungsten bronzes was heated in the presence of a transporting agent (chlorine) or a mineralizer (melt of B2O3) at temperatures below 1150°C. It could be prepared by the reaction of a 1:1 mixture of Sr(NO3)2 or SrCO3 with Ta2O5 in a sealed quartz glass tube as well. SrTa2O6(orh.) also occurred as an intermediate phase of the reaction of the corresponding 1:2 mixture at temperatures below 900°C (e. g. 840°C). Indexing of Guinier powder patterns led to the following unit cell: a = 11.006 Å, b = 7.638 Å, c = 5.622 Å. At temperatures above 1220°C SrTa2O6(orh.) changes (in air) to SrTa2O6(TTB). A reversal of this transition could not be achieved without the presence of a mineralizer or a transporting agent. CaxSr1-xTa2O6 solid solutions of the low temperature form could not definitely be established. However, at 1300°C solid TTB solutions of CaxSr1-xTa2O6 were formed. For x 〉 0.05 the TTB unit cells are orthorhombically distorted. For x ≥ 0.85 the x-ray powder patterns of the solid solutions looked like the one of CaTa2O6(orh.) and no TTB-structure was observed at 1300°C.
    Notes: Von SrTa2O6 wurde eine neue, mit orthorhombischem CaTa2O6 strukturverwandte Tieftemperatur-Modifikation erhalten. SrTa2O6(orh.) ließ sich bei Temperaturen unter 1150°C sowohl aus der bisher bekannten, den tetragonalen Wolframbronzen verwandten Modifikation SrTa2O6(TWB) in Gegenwart eines Transportmittels (Chlor) bzw. eines Mineralisators (B2O3-Schmelze), wie auch durch Umsetzen von Gemengen (1:1) aus SrCO3 oder Sr(NO3)2 und Ta2O5 in geschlossenen Quarzglasampullen erhalten. Auch als Zwischenprodukt der Umsetzung entsprechender 1:2-Gemenge bei Temperaturen unter 900°C (z. B. 840°C) tritt diese Modifikation auf. Die Gitterkonstanten von SrTa2O6(orh.) sind aufgrund von Pulverdaten: a = 11,006 Å, b = 7,638 Å, c = 5,622 Å. Beim Erhitzen auf etwa 1 220°C (an der Luft) wandelt sich SrTa2O6(orh.) in SrTa2O6(TWB) um. Eine Rückumwandlung von SrTa2O6(TWB) in SrTa2O6(orh.) ohne Mineralisator- oder Transportmittelzusatz war nicht zu erreichen. Mischkristalle CaxSr1-xTa2O6 der Tieftemperaturform ließen sich nicht sicher nachweisen. Die bei Mischkristallen mit 0,05 〈 x ≤ 0,20 (1300°C) vorliegende TWB-Struktur ist orthorhombisch verzerrt. CaTa2O6(orh.) zeigte dagegen ab x ≥ 0,85 (1300°C) keine Entmischung.
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    Darstellung, Isolierung und Charakterisierung gemischter Thiocyanato(1,3-diaminopropan)chrom(III)-Komplexe (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 167-173 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation, Isolation, and Characterization of Mixed Thiocyanato(1.3-diaminopropane) -chromium(III) ComplexesThe complexes [Cr(NCS)4dap]- and trans-[Cr(NCS)2(dap)2]+ (dap = 1.3-diaminopropane) are prepared for the first time, isolated as salts and characterized by CHN analysis, chromium contents, the electrophoretic behaviour in dimethylformamide, and by UV, VIS, and IR spectra.
    Notes: Die Komplexe [Cr(NCS)4dap]- und trans-[Cr(NCS)2(dap)2]+ (dap = 1,3-Diaminopropan) werden erstmals dargestellt, als Salze isoliert und durch CHN-Analyse, Chrombestimmung, elektrophoretisches Verhalten in Dimethylformamid sowie Spektren im UV, VIS und IR charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19845090218
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    Sulphur-Nitrogen Chelating Agents. IV. Some Solid State Copper(II) Complexes of Thia-aminopyridines An I.R. and Reflectance Spectral Analysis (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 201-208 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Schwefel-Stickstoff-Chelatbildner. IV. Einige Kupfer(II)-Komplexe von Thioaminopyridinen. IR- und ReflexionsspektroskopieEine Reihe von CuII-Komplexen sind dargestellt und charakterisiert worden. Die angenommenen Strukturen beruhen auf ihren IR -und VIS-Spektren. Die Thioaminopyridine können in verschiedener Weise koordiniert sein. Im Gegensatz zu unseren Befunden an aliphatischen Thioaminen ergab sich kein Zusammenhang zwischen der Struktur der CuLX2-Verbindungen und der Art des X--Anions. Ein Hinweis auf die Struktur der CuL2+-Komplexe in wäßriger Lösung kann aus festem CuLX2 nicht erhalten werden.
    Notes: A series of solid state CuII complexes with thia-aminopyridines . S(CH2)mNH2 have been prepared and characterized. The postulated structures of these CuLX2 (X = OAc-, NO3-, ClO4- or Cl-) compounds were based on their I.R. and electronic spectra. It was found that the thiaaminopyridines may coordinate in quite different ways. In contrast with what was found for the aliphatic thiadiamines, no relation was stated between the structure of the CuLX2 compounds and the nature of the X- anion.Moreover the solid state compounds do not give a clear indication for the structure of the CuL2+ species in aqueous solution.
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    URL: http://dx.doi.org/10.1002/zaac.19845090222
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  • 35
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    Thermochemical Properties and Vapor Growth of Hg1-xCdx Te on CdTe (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 199-207 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Thermochemische Eigenschaften und Aufwachsen von Hg1-xCdxTe auf CdTeNach thermodynamischen Rechnungen enthält die Gasphase des epitaktischen Hg1-xCdxTe - HgI2 - CdTe Systems vorwiegend Hg(g) und HgI2(g) durch die andere Moleküle vom Ausgangsstoff zum CdTe Substrat wandern. Transportversuche im Temperaturgradienten 590° → 535°C zeigten, daß man dünne Schichten von Hg1-xCdxTe auf CdTe von einem ternären Ausgangsmaterial in Gegenwart von HgI2 erhält.
    Notes: Based on a thermodynamic analysis, the vapor phase of the Hg1-xCdxTe - HgI2 - CdTe epitaxy system consists predominantly of Hg(g) and HgI2(g) through which nutrient species migrate from the source to the CdTe substrate. Growth experiments in the 590° → 535°C temperature gradient showed that Hg1-xCdxTe layers can be grown on CdTe substrates using a preannealed, ternary source material in the presence of HgI2.
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    URL: http://dx.doi.org/10.1002/zaac.19845100328
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    Chemischer Transport der Nickelsulfide und einige Zusammenhänge beim Transport komplexer Bodenkörper am Beispiel der Sulfide von Fe, Co, NiProfessor Hans Albert Lehmann zum 65. Geburtstage am 1. Mai 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 19-32 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemical Transport Reactions of Ni-Sulfides and Some Relationships in C.T.R. of Complex Solids in the Case of Sulfides of Fe, Co, NiCrystals of α-Ni3S2, NiS, and NiS2 as well as solid solutions Fe1-yNiySx were grown by C.T.R. The coexistence equilibrium pressure of the solution equilibrium pressure p(S2), the activity of the metal component, the stability of gaseous metal halides concerning decomposition as well as their stability related on the transport agent have to be taken into account to choose a suitable transport agent, which have a sometimes opposite influence on the transport behaviour. Halogenes, hydrogen halides, and GeI2 were used as transport medium.
    Notes: Durch chemische Transportreaktionen wurden Kristalle der Phasen α-Ni3S2, NiS und NiS2 sowie Mischkristalle Fe1-yNiySx erhalten. Bei der Auswahl des Transportmittels sind der Koexistenzzersetzungsdruck bzw. Löslichkeitsdruck p(S2) und die Metallaktivität im Bodenkörper, die Stabilität der gasförmigen Metallhalogenide bezüglich Zerfall und ihre Stabilität relativ zum Transportmittel zu beachten, die z. T. gegenläufigen Einfluß haben. Geeignete Transportmittel sind Halogene, Halogenwasserstoffe und GeI2.
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    Zum chemischen Transport von Zinkoxid und zur Bestimmung seiner PhasenbreiteProfessor Hans-Albert Lehmann zum 65. Geburtstage am 1. Mai 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 57-71 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Chemical Transport of Zinc Oxide and the Estimation of its Phase WidthThe chemical transport behaviour of zinc oxide using different transport agents and the influence of the transport conditions (T, ΔT, p) on transport rate and deposition form was studied. The range of homogeneity of ZnO is very narrow. The best agents for deposition of ZnO with the upper phase boundary are Cl2 and Br2, for the deposition of the lower phase boundary HBr and NH4Br are more suitable. The deviation from stoichiometry depends on the deposition temperature and amounts to 10 till 250 ppm in the range of 1073 up to 1373 K.
    Notes: Das chemische Transportverhalten von Zinkoxid mit Cl2, Br2, HCl, HBr, NH4Cl und NH4Br und der Einfluß der Transportbedingungen (T, ΔT, p) auf die Abscheidungsgeschwindigkeit und Abscheidungsform wurde studiert. ZnO weist ein sehr schmales Homogenitätsgebiet auf. Zur Abscheidung von ZnO der oberen Phasengrenzzusammensetzung sind Cl2 und Br2 am besten geeignet. Für die Abscheidung von ZnO der unteren Phasengrenzzusammensetzung sind am besten HBr und NH4Br geeignet. Die Abweichung von der Stöchiometrie hängt von der Präparationstemperatur der Kristalle ab und liegt zwischen 10 und 250 ppm im Temperaturbereich 1073 bis 1373 K.
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    Beiträge zur Chemie der Alkylverbindungen von Übergangsmetallen. XXXVIII. Reaktion von Dibenzylmangan mit Sauerstoff (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 511 (1984), S. 89-94 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Transition Metal Alkyl Compounds. XXXVIII. Reactions of Dibenzyl Manganese with Oxygene(C6H5CH2)2Mn · C4H8O2 reacts with oxygen forming an unstable deep violet compound which changes in a stable unsoluble yellow peroxide of the formula C6H5CH2MnO—OMnCH2C6 H5. With excess oxygen a polynuclear complex of 3 valent manganese is formed with the composition Mn4O4(OH)4(OCHC6H5)2.The compounds isolated were characterized by the products of hydrolyses and thermolyses, anaerobic reaction with iodine, magnetic moments, i.r. and e.s.r. spectra.
    Notes: Dibenzylmangan-1,4-dioxan reagiert mit Sauerstoff zu einer tiefvioletten instabilen Substanz. Diese wandelt sich in ein stabiles gelbes, schwerlösliches Peroxid der Formel C6H5CH2MnO—OMnCH2C6H5 um. Mit überschüssigem Sauerstoff entsteht daraus ein Mehrkernkomplex des 3wertigen Mangans der Zusammensetzung Mn4O4(OH)4(OCHC6H5)2.Die isolierten Verbindungen wurden durch ihre Hydrolyse- und Thermolyseprodukte, anaerobe Iodierung, magnetischen Momente sowie IR- und ESR-Spektren näher charakterisiert.
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    Masthead (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845080101
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    Darstellung und Struktur von Antimon(III)-tris(thiophosphinaten) (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 19-25 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of Antimony (III) Tris (thiophosphinates)The title compounds are formed by the reaction of Sb(CH3COO)3 with thiophosphinic acids R2P(=S)OH (R = CH3 cyclo-C6H11, C6H5). The crystal and molecular structures of Sb((cyclo-C6H11)2POS)3 and Sb((C6H5)2POS)3 have been determined by single crystal X-ray methods. SbIII is pyramidally coordinated to the oxygen atoms of the R2POS ligands through short (primary) bonds with a mean length of 203 pm. The Sb—S distances of the mainly chelating ligands vary between 300 and 320 pm (secondary bonds). The lone electron pair is stereochemically active.
    Notes: Die Umsetzung von Sb(CH3COO)3 mit Thiophosphinsäuren R2P(=S)OH (R = CH3, cyclo-C6H11, C6H5) führt zu Verbindungen der Formel Sb(R2POS)3. Die Strukturen der Verbindungen mit R = cyclo-C6H11 und C6H5 wurden an Einkristallen röntgenographisch bestimmt. SbIII ist über kurze (primäre) Bindungen mit der mittleren Länge von 203 pm pyramidal an die Sauerstoffatome der R2POS-Liganden gebunden. Die Sb—S-Abstände (sekundäre Bindungen) sind ungefähr 320 pm lang. Das freie Elektronenpaar ist stereochemisch aktiv.
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    Schwingungs- und massenspektroskopische Untersuchungen an α,ω-Dihydrochlorsilanen H(SiCl2)nH mit n = 3-7 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 43-49 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: I.R. and Mass Spectroscopic Investigations on α,ω-Dihydrochloro Silanes H(SiCl2)nH with n = 3-7Mass spectra of α,ω-dihydrochlorosilanes H(SiCl2)nH were analyzed respecting to their fragmentation. This shows, that the cleavage starts with the break of SiSi bonds, by preference in the middle of the chain. This is in accordance to the results of IR spectra which show very similar frequencies like perchlorooligo silanes. Thus, the lowest force constants of SiSi bondings in α,ω-dihydrochloro silanes, can be also expected in the middle of the chain.
    Notes: Die Massenspektren der α,ω-Dihydrochlorsilane H(SiCl2)nH mit n = 3-7 werden bezüglich ihrer Fragmentierung analysiert. Es zeigt sich, daß die Spaltung mit einem Zerbrechen der SiSi-Bindung, vorzugsweise in der Mitte der Kette beginnt. Dies steht im Einklang mit den Ergebnissen der IR-Spektren, die sehr ähnliche Frequenzen zeigen, wie bei den Perchlorsilanen gefunden. Daraus kann geschlossen werden, daß auch bei den α,ω-Dihydrochlorsilanen die mittleren SiSi-Bindungen die kleinsten Kraftkonstanten zeigen.
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    URL: http://dx.doi.org/10.1002/zaac.19845080107
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    Röntgenographische Phasenbestimmungen zur thermischen Dissoziation und das Hydrolyseverhalten von Alkalihexafluorogermanaten bei höheren TemperaturenProfessor Günther Rienäcker zum 80. Geburtstage am 13. Mai 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 512 (1984), S. 48-58 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Phase Determinations by X-rays on the Thermal Dissociation and the Hydrolysis of Alkali Hexafluorogermanates at Higher TemperaturesFor a better understanding of the thermal dissociation of alcaline hexafluorosilicates investigations have been done on hexafluorogermanates. In these systems the formation of new phases has been studied by x-rays in dependence of temperature. Thermal behaviour of the substances strongly depends on the starting structure. Phase transformations taking place at lower temperatures are strongly determine the reaction at higher temperature. Therefore, we found differences to the analogous thermal reactions of hexafluorosilicates.There is a high sensitivity to hydrolysis of hexafluorogermanates above 600°C. We discuss the difference in reaction of thin powder layers and of powder samples in the volume.
    Notes: Zum besseren Verständnis des thermischen Verhaltens von Alkalihexafluorosilicaten wurden Vergleiche mit analogen Germanium-Verbindungen angestellt. Die Phasenneubildung wurde als Funktion der Temperatur röntgenographisch untersucht. Es ergab sich eine starke Abhängigkeit des thermischen Verhaltens von der Ausgangsstruktur. Phasentransformationen, die bei niederen Temperaturen ablaufen, beeinflussen bei höherer Temperatur das Reaktionsgeschehen (thermische Vorgeschichte der Substanz). Deshalb resultieren gegenüber den Hexafluorosilicaten differierende Reaktionsabläufe. Durch Heizguinieraufnahmen unter getrocknetem, strömendem Inertgas wurde die enorme Hydrolysenempfindlichkeit der Hexafluorogermanate oberhalb 600°C bewiesen.Das unterschiedliche Verhalten von dünnen Pulverschichten und kompakten Pulverproben wird diskutiert.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845120507
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    Bildung siliciumorganischer Verbindungen. 99. Zur Trennung von Carbosilan- und Silylphosphan-Gemischen mit Hilfe der HochdruckflüssigkeitschromatographieProfessor Günther Rienäcker zum 80. Geburtstage am 13. Mai 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 512 (1984), S. 93-102 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation of Organosilicon Compounds. 99. Separation of Carbosilane and Silylphosphane Mixtures by Means of HPLCTest mixtures of Si-methylated carbosilanes were separated by means of reversedphase HPLC (nucleosil 5-C18; CH3OH:hexane = 90:10). The corresponding SiCl-containing mixtures were successfully separated only after reductin of the SiCl groups by means of LiAlH4 (CH3OH: C6H6 + H2O = 92.5:7.5 + 4 - 8%). A model separation of the silylphosphanes Me3SiPH2, (Me3Si)2PH and (Me3Si)3P using the same material but acetonitrile: toluene = 85:15 is also reported.
    Notes: Testgemische Si-methylierter Carbosilane werden mit reversed-phase HPLC getrennt (Nucleosil 5-C18; CH3OH:Hexan = 90:10). Die Auftrennung entsprechender SiCl-haltiger Verbindungen gelingt nach Reduktion der SiCl-Gruppen mit LiAlH4 (CH3OH: C6H6 + H2O = 92,5: 7,5 + 4 - 8%). Über die Modelltrennung der Silylphosphane Me3SiPH2, ((Me3Si)2)2PH und (Me3Si)3P unter Verwendung des gleichen Säulenmaterials, jedoch mit dem Eluens Acetonitril: Toluol = 85:15, wird ebenfalls berichtet.
    Additional Material: 5 Ill.
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    Zur Reaktivität von intramolekular basenstabilisierten Zinn(II)-Verbindungen mit Halogenen, Zinntetrachlorid und Chloroform (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 512 (1984), S. 177-180 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactivity of Intramolecular Basestabilized Tin(II) Compounds with Halogens, Tin Tetrachloride, and TrichloromethaneIntramolecular basestabilized tin(II) compounds of the type RN(CH2CH2Y)2Sn (Y = O, S and R = Me, t-Bu) react with halogens, tin tetrachloride, and trichloromethan at room temperature by oxydative addition reaction to tin(IV) derivatives. These compounds are characterized by n.m.r. investigations and by Mössbauer studies.
    Notes: Intramolekular basenstabilisierte Zinn(II)-Verbindungen des Typs RN(CH2CH2Y)2Sn (Y = O, S und R = Me, t-Bu) reagieren bei Raumtemperatur mit Halogenen, Zinntetrachlorid und Chloroform im Sinne von oxydativen Additionsreaktionen zu Zinn(IV)-Derivaten. Diese Derivate werden durch NMR-Untersuchungen und durch Mößbauerstudien charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19845120519
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    Über Chalkogenolate. 137. Isothiocyano-, Isothiocyanomonothio- und Isothiocyanodithio- ameisensäurealkylester (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 512 (1984), S. 231-239 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 137. Alkyl Esters of Isothiocyanoformic, Isothiocyanomonothioformic and Isothiocyanodithioformic AcidsThe esters RO—CO—NCS, where R = CH3, C2H5, as well as RS—CO—NCS and RS—CS—NCS with R = C2H5, nC3H7 have been prepared by three different methods. The reaction between the corresponding chloro compound and KSCN in the presence of the phase transfer catalyst 18-crown-6 gives the highest yields.The electron absorption, infrared, nuclear magnetic resonance, and mass spectra of these compounds are reported.
    Notes: Die Ester RO—CO—NCS mit R = CH3, C2H5 sowie RS—CO—NCS und RS—CS—NCS mit R = C2H5, nC3H7 wurden nach drei verschiedenen Verfahren hergestellt, wobei die Umsetzung der entsprechenden Chloroverbindung mit KSCN in Gegenwart des Phasentransferkatalysators 18-Krone-6 die besten Ausbeuten erbringt.Die Elektronenabsorptions-, Infrarot-, kernmagnetische Resonanz- und Massenspektren der Verbindungen werden mitgeteilt.
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    Komplexbildung und Extraktion von Molybdän(VI) mit zweizähnigen Liganden (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 191-196 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Coordination and Extraction of Molybdenum(VI) with Bidentate LigandsA series of bidentate ligands as well as their thio derivatives from the groups of 8-quinolinols, β-diketones, acylpyrazolones, and N-acyl-phenylhydroxylamines was studied for the ability to extract molybdenum(VI) from heptamolybdate. The extraction principally runs only in acidic medium, sulfur-containing extractants having no advantage. The composition of the complexes was determined by the isolation of compounds in the solid state and also by the interpretation of distribution data.
    Notes: Eine Reihe zweizähniger Liganden sowie entsprechende Thioderivate aus den Gruppen der 8-Hydroxychinoline, β-Diketone, Acylpyrazolone und N-Acyl-phenylhydroxylamine wurde auf ihr Extraktionsvermögen für Molybdän aus Heptamolybdat geprüft. Die Extraktion ist grundsätzlich nur im sauren Bereich möglich, schwefelhaltige Extraktionsmittel bringen keine Vorteile. Die Komplexzusammensetzung wurde durch Isolierung von Komplexen in Substanz und durch Auswertung der Verteilungsdaten ermittelt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845080127
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    Beiträge zur Chemie der Silicium-Schwefel-Verbindungen. XXIX. 29Si-NMR-Untersuchungen (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 201-207 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Silicon-Sulphur Compounds. XXIX. 29Si-N.M.R. InvestigationsThree series of silicon-sulphur compounds (RO)3SiSR′ (I), (i-PrO)4-nSi(SEt)n (II) and cyclic Si—S compounds (III) were prepared, some of them at the first time and their 29Si-N.M.R. spectra were measured. In the series of trialkoxysilylthio derivatives (I) were the steric and inductive effects of the RO and R'S groups evaluated. In the series II were the 29Si-N.M.R. chemical shifts related to the relative paramagnetic screening constants σ* and netto charge at the silicon atom q(Si) using the EN-quantum-chemical model discussed. In the series III were the shift contribution of the (SiS)2 and 1-sila-2,5-dithiacyclopentan rings determined.
    Notes: Drei Reihen von Silicium-Schwefel-Verbindungen: (RO)3SiSR'(I), (i-PrO)4-nSi(SEt)n (II) und cyclische Si—S-Verbindungen (III) wurden dargestellt, davon einige erstmalig, und ihre 29Si-NMR-Spektren vermessen. In der Reihe der Trialkoxysilylthio-Derivate (I) wurden die sterischen und induktiven Wirkungen der RO- und R'S-Gruppen abgeschätzt. In der Reihe II wurden die 29Si-NMR-chemischen Verschiebungen in Abhängigkeit von den relativen paramagnetischen Abschirmungskonstanten σ* und der Nettoladung am Silicium q(Si) im Rahmen des EN-quantenchemischen Modells diskutiert. In der Reihe III wurden die Beiträge des (SiS)2-und 1-sila-2,5-dithia-cyclopentan-Rings zur chemischen Verschiebung ermittelt.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845080129
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    Über Chalkogenolate. 134. Untersuchungen über Ester von Halogenoameisensäuren 2. Darstellung und Eigenschaften von Se-Alkylestern der Chloromonothiomonoselenoameisensäure [1] (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 61-66 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 134. Studies on Esters of Haloformic Acids 2. Synthesis and Properties of Se-Alkyl Esters of Chloromonothiomonoselenoformic AcidThe hitherto unknown esters RSe—CS—Cl with R = C2H5 and nC3H7 have been prepared by reaction of thiophosgene with the corresponding alkane selenol. The compounds have been characterized with electron absorption, nuclear magnetic resonance (1H, 13C, and 77Se), infrared, and mass spectra.
    Notes: Die bisher nicht bekannten Ester RSe—CS—Cl mit R = C2H5 und nC3H7 wurden durch Umsetzung von Thiophosgen mit dem entsprechenden Alkanselenol hergestellt. Die Verbindungen wurden mit Elektronenabsorptions-, 1H-, 13C- und 77Se-NMR-, Infrarot- und Massenspektren charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19845090206
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    Beiträge zur Chemie des Siliciums und Germaniums. XXXIV. Ein weiterer Beitrag zur Darstellung von Kaliumsilyl (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 95-100 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Silicon and Germanium. XXXIV. A Further Contribution to the Preparation of Potassium SilylThe reaction time for the preparation of potassium silyl from monosilane in glyme is abridged considerably by the use of dispersed Na/K alloy. The preparation is simplyfied by the use of pure dispersed potassium instead of the dispersed alloy. In this case a further abridgement of the reaction time is observed and the filtration of the residue after the end of the reaction is easier because there is no sodium in the residue. Crystalline potassium silyl, free of potassium hydride and glyme, is obtained by recrystallisation followed by slow crystallisation from a glyme/benzene mixture. During a storage of 30 month the crystals turned out to be stable.
    Notes: Die Reaktionszeit für die Darstellung von Kaliumsilyl aus Monosilan in Monoglyme verkürzt sich bei Verwendung von dispergierter Na/K-Legierung erheblich. Die Darstellung vereinfacht sich, wenn statt der dispergierten Na/K-Legierung reines dispergiertes Kalium eingesetzt wird. Hierbei wird eine weitere Verkürzung der Reaktionszeit festgestellt, und die Filtration des Rückstandes nach Ende der Reaktion ist durch das Fehlen des Natriums einfacher. Kaliumsilylkristalle, in denen weder Kaliumhydrid noch Monoglyme nachweisbar sind, werden durch Umkristallisieren und nachfolgende langsame Kristallisation aus einem Monoglyme/Benzol-Gemisch erhalten. Die Kristalle erwiesen sich bei einer 30monatigen Lagerung als stabil.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845090210
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    Über Oxothorate der Alkalimetalle. Zur Kenntnis von K3NaTh2O6 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 127-137 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Oxothorates of the Alkaline Metals: K3NaTh2O6For a first time single crystals of a (in addition: new) oxothorate were prepared starting with the binary oxides [1 200°C, 4d, then 1 300°C, 5d, Ni-bomb; powder: 650°C, 10d, Ag-bomb]. The colourless, transparent single crystals are monoclinic, C2/c, a = 629.64 pm, b = 1 089.93 pm, c = 1 259.75 pm, β = 99.66°, z = 4, Dx = 5.458 g cm-3 and Dpyc = 5.456 gcm-3. It is an ordered variant of the NaCl-type; MoKα, fourcircle diffractometer data (PW 1100), R = 7.67 and Rw = 7.35% for 1 083 of 1 236 I0 (hkl). The Madelung Part of Lattice Energy, MAPLE, is calculated and discussed.
    Notes: Erstmals wurden Einkristalle eines zudem neuen Oxothorates, K3NaTh2O6, aus den binären Komponenten dargestellt [1 200°C, 4d, dann 1 300°C, 5d, Ni-Bömbchen; Pulver analog: 650°C, 10d, Ag-Bömbchen]. Die farblosen, durchsichtigen Einkristalle kristallisieren monoklin, C2/c, a = 629,64 pm, b = 1 089,93 pm, c = 1 259,75 pm, β = 99,66°, Z = 4, drö = 5,458 g cm-3 und dpyk = 5,456 g cm-3. Es liegt eine geordnete NaCl-Variante vor; MoKα, Vierkreisdiffraktometerdaten (PW 1100), R = 7,67 und Rw = 7,35% für 1 083 von 1 236 I0(hkl). Der Madelunganteil der Gitterenergie, MAPLE, wird berechnet und diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19845090213
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    Nitrat-, Thiosulfat-, Sulfat- und Sulfid-Cancrinit (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 509 (1984), S. 153-160 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Nitrate-, Thiosulphate-, Sulphate-, and Sulphide Cancrinite1For the synthesis of the compounds to a solution of sodium aluminate there is added in excess sodium nitrate, or sodium thiosulphate, or sodium sulphite, or sodium sulphide. After heating a solution of sodium silicate is added, and the suspension is hold at 110°C for a long time, the precipatite is filtered, washed, and dried.2The white compounds are characterized in composition and crystal structure by chemical and X-ray analysis and densities.3The unimolecular hexagonal cell of the compounds has the cancrinite structure (lattice constants and densities see „Inhaltsübersicht“).4By heating of thiosulphate cancrinite at 1 000°C in air there is produced a nice deep blue coloured pigment.
    Notes: 1Zur Darstellung der Verbindungen wird zu einer Natriumaluminatlösung Natriumnitrat oder Natriumthiosulfat oder Natriumsulfat oder Natriumsulfid bei Zimmer-temperatur im Überschuß gegeben. Nach Aufheizen wird eine Wasserglaslösung zugetropft, die Suspension längere Zeit bei 110°C gehalten, der Niederschlag abfiltriert, gewaschen und getrocknet.2Die weißen Verbindungen werden in Zusammensetzung und Kristallstruktur durch chemische und röntgenographische Analyse sowie Dichten charakterisiert.3Mit 1 Molekel/Zelle kristallisieren die Verbindungen im hexagonalen Cancrinitgitter mit den Konstanten und Dichten: TextVerbindungGitterkonstanten in ÅDichten in g/ml a0c0RöntgenPyknometerNa8[Al6Si6O24](NO3)2 · 4 H0O12,68 ± 0,025,18 ± 0,012,522,30Na8[Al6Si6O24](S2O3) · 3 H2O12,73 ± 0,025,02 ± 0,032,512,28Na8[Al6Si6O24](SO4) · 3 H2O12,674 ± 0,0045,173 ± 0,0032,422,37Na8[Al6Si6O24](S) · 4 H2O12,669 ± 0,0075,187 ± 0,0032,312,244Durch Glühen des Thiosulfat-Cancrinits bei 1 000°C an Luft erhält man ein schönes tiefblaues Pigment.
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    URL: http://dx.doi.org/10.1002/zaac.19845090216
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    Masthead (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845100301
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    Benzylnickel(II)-Komplexe und ihre Reaktionen (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 11-15 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Benzyl Nickel(II) Complexes and their ReactionsBy the oxydative addition of p-substituted benzyl chlorides to (Ph3P)2Ni(C2H4) at -20°C the violet nickel(II) complexes (Ph3P)2Ni(p-CH2C6H4R)Cl (R = CN, COOH, CH3, Cl) are, formed. In water containing solutions the carbonic acid (Ph3P)2Ni(p-CH2C6H4COOH)Cl is rearranged to the corresponding p-methylbenzoate.With carbon dioxide the complexes (Ph3P)2Ni(p—CH2C6H4R)Cl react like Grignard compounds. Diphenyl ethine and butadien-1,3 are inserted in the Ni - C bond at room temperature. Substituted nickel-σ-vinyl or π-allyl complexes are obtained. The reactivity of the nickel-σ-benzyl compounds is compared with that of other nickel(II)-alkyl compounds.
    Notes: Die oxydative Addition von p-substituierten Benzylchloriden an (Ph3P)2—Ni(C2H4) bei -20°C ergibt die violetten Nickel(II)-Komplexe (Ph3P)2Ni(p—CH2C6H4R)Cl (R = CN, COOH, CH3, Cl). Die Carbonsäure (Ph3P)2Ni(p—CH2C6H4COOH)Cl lagert sich in Gegenwart von Wasser in das entsprechende p-Methylbenzoat ein.Die Verbindungen des Typs (Ph3P)2Ni(p—CH2C6H4R)Cl reagieren mit Kohlendioxid grignardanalog. Diphenylethin und Butadien-1,3 werden bei normaler Temperatur in die Ni - C-Bindung eingeschoben. Dabei entstehen substituierte Nickel-σ-vinyl- bzw. π-allyl-Komplexe. Das Reaktionsverhalten der Nickel-σ-benzylverbindungen wird mit dem anderer Nickel(II)-alkylverbindungen verglichen.
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    URL: http://dx.doi.org/10.1002/zaac.19845100303
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    Preparation and Crystal Structure of La3ReO8 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 46-50 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Darstellung und Kristallstrukturbestimmung von La3ReO8La3ReO8 wurde bei 1425°C dargestellt, die Strukturbestimmung ergab abweichende Resultate von einer Darstellung, die bei 900°C erfolgte (BAUD u. Mitarb. 1979). Die Hochtemperaturmodifikation kristallisiert in der monoklinen Raumgruppe P21/m mit a = 7,757(1), b = 7,777(1), c = 5,928(1) Å, γ = 111,1°, Z = 2. Die Struktur wurde durch Patterson und Fouriersynthesen gelöst und bis R(F) = 0,073 verfeinert. Die Struktur besteht aus isolierten, verzerrten ReO6-Oktaedern und Doppelketten von kantenverknüpften La4O-Tetraedern.
    Notes: The crystal structure of La3ReO8, prepared at 1425°C, is reported to be different from a previous result on a preparation at 900°C (BAUD et al., 1979). The high temperature modification crystallizes in the monoclinic space group P21/m with a = 7.757(1), b = 7.777(1), c = 5.928(1) Å, γ = 111.1°, Z = 2. The structure was solved by Patterson and Fourier methods from single crystal diffractometer data and refined to final R(F) = 0,073. The structure consists of isolated, distorted ReO6 octahedra and double chains of edge-shared La4O tetrahedra.
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    URL: http://dx.doi.org/10.1002/zaac.19845100308
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    Resonanzramanspektrum und Struktur von matrixisoliertem Te3 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 72-78 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Resonance Raman Spectrum and Structure of Matrixisolated Te3By condensing a mixture of 76% Te atoms and 24% Te2 molecules in a nitrogen matrix at 15 K followed by annealing to nearly 25 K we obtained Te3 molecules by a matrix reaction. The resonance Raman spectrum of Te3 contains 8 overtones of the symmetric stretching vibration. The following values for ω1 and x11 have been calculated for the isotopically pure species 126Te3: ω1 = 206.33 ± 0.15 cm-1; x11 = 0.24 ± 0.03 cm-1 and 130Te3: ω1 = 203.1 ± 0.2 cm-1; x11 = 0.22 ± 0.05 cm-1. Using a 1:1 ratio of 126Te and 130Te in the synthesis of Te3 the band shape of the envelopes of the superimposed spectra of all possible Te3 species could only be explained assuming a bent structure (120° ± 10°). The value of the force constant fr + frr of 210 ± 10 Nm-1 reflects multiple bonding in this molecule. The proposed structure also agrees with thermodynamical considerations.
    Notes: Wird eine Gasmischung aus 76% Te-Atomen und 24% Te2-Molekeln mit einem Überschuß Stickstoff bei 15 K abgeschreckt und anschließend kurz auf 25 K erwärmt, so entstehen durch eine Matrixreaktion Te3-Molekeln. Im Resonanzramanspektrum dieser Spezies werden 8 Obertöne der symmetrischen Streckschwingung beobachtet. Für zwei verschiedene Te-Isotope erhält man folgende Werte für ω1 und x11: 126Te3: 206,33 ± 0,15 cm-1, 0,24 ± 0,03 cm-1; 130Te3: 203,1 ± 0,20 cm-1, 0,22 ± 0,05 cm-1. Die Verwendung von Proben, die je 50% der beiden Isotopen enthalten führt zu einem Bandenmuster, bei dem die Intensität der einzelnen Banden und ihre Frequenzverschiebung für eine gewinkeltes Te3-Molekel sprechen (120° ± 10°). Der Wert der Kraftkonstante fr + frr von 210 ± 10 Nm-1 zeigt Mehrfachbindungsanteile an. Eine thermodynamische Betrachtung liefert zusätzliche Anhaltspunkte für eine offene (nicht ringförmige) Struktur vom Te3.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845100311
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    Trialkylbismutine als Liganden in Carbonylkomplexen des Eisens und der VIa-Elemente (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 104-108 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Trialkylbismutines as Ligands in Carbonyl Complexes of Iron and Group VIa ElementsThe complexes (CO)4FeBiR3 (R = Et, Pr, Bu) are synthesized by reaction of Fe2(CO)9 and the corresponding bismutines. Complexes of the type Bu3BiM(CO)5 (M = Cr, Mo, W) are formed by irradiation of the hexacarbonyls of group VIa elements in tetrahydrofuran and subsequent addition of Bu3Bi. The novel compounds are obtained in 40 - 90% yield. They are stable in an inert atmosphere above 25°C. Their 1H-n. m. r., i. r., and m. s. data are discussed.
    Notes: Die Komplexe (CO)4FeBiR3 (R = Et, Pr, Bu) werden durch Umsetzung von Fe2(CO)9 mit den entsprechenden Bismutinen synthetisiert. Komplexe des Typs Bu3BiM(CO)5 (M = Cr, Mo, W) entstehen durch Bestrahlung der Hexacarbonyle der VIa-Elemente in Tetrahydrofuran und nachfolgende Umsetzung mit Bu3Bi. Die neuen Verbindungen werden in 40 - 90% Ausbeute erhalten. Sie sind bei Luftausschluß auch oberhalb von 25°C stabil. Ihre 1H-NMR-, IR- und EI-MS-Daten werden diskutiert.
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19845100315
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    Die Kristallstruktur von Ag2Ge2O5: Eine neuartige Gerüststruktur von Ge2O52- (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 143-151 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Crystal Structure of Ag2Ge2O5: A New Ge2O52- Network StructureAg2Ge2O5 was prepared from the binary oxides at high O2 pressures. Single crystal X-ray diffraction work indicated monoclinic symmetry (P21/c; a = 1101.3(2); b = 1006.3(1); c = 1221.9(3) pm; ß = 94.6(1)°). The structure was determined by direct methods (3372 independent structure factors) and refined to a conventional R value of 0.084. A new Ge2O52- network structure was found with germanium coordinated octahedrally (­d(Ge - O) = 188,7 pm) and tetrahedrally (­d(Ge - O) = 175,9 pm), in equal proportions, by oxygen. The polyhedra share vertices and edges, thus forming a three dimensional channel system, which is occupied by Ag+ ions. The shortest Ag - Ag distance of 284 pm, like the pale yellow colour of the compound, indicates Ag+ - Ag+ interaction.
    Notes: Durch Sauerstoffhochdrucksynthese wurde Ag2Ge2O5 aus den binären Komponenten dargestellt. Nach Einkristalluntersuchungen liegt monokline Symmetrie vor (P21/c; a = 1101,3(2); b = 1006,3(1); c = 1221,9(3) pm; ß = 94,6°(1); Z = 12). Die Struktur wurde mittels direkter Methoden (Ag-Positionen) und Fourier-Synthesen gelöst (3372 unabhängige Strukturfaktoren); der R-Wert konvergierte bei 8,4%. Das Anion Ge2O52- bildet eine neuartige Raumnetzstruktur, wobei die Germaniumatome jeweils zur Hälfte oktaedrisch [­d(Ge - O) = 188,7 pm] und tetraedrisch [­d(Ge - O) = 175,9 pm] von Sauerstoff koordiniert sind. Die Polyeder sind in der Weise über gemeinsame Ecken und Kanten verknüpft, daß dreidimensional vernetzte, kanalartige Hohlräume entstehen, die von den Gegenkationen (Ag+) ausgefüllt werden. Der kürzeste Ag - Ag-Abstand beträgt 284 pm und gibt, wie die blaßgelbe Eigenfarbe der Substanz, einen Hinweis auf bindende Ag+ - Ag+-Wechselwirkungen.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845100320
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    Synthese von Bis- und Tris(trimethylsilyl)methyl-aminofluorsilanen (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 510 (1984), S. 175-179 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis of Bis- and Tris(trimethylsilyl)-methyl-aminofluorosilanesLithium-tris(trimethylsilyl)methane reacts with fluoro-silanes to give (Me3Si)3C - SiF2R (1 - 3, R = F, C6H5, CMe3). 1 and 2 react with lithiated amines to aminofluorosilanes 4 a, 5 a, 6 a, and with a 1, 3-migration of a silyl group to the structure isomeric trimethylsilylaminofluorsilanes 4 b, 5 b, 6 b, 7, 8. The disubstituted NH-compound 9 is obtained in the reaction of 1 with LiNH2.
    Notes: Lithium-tris(trimethylsilyl)-methan reagiert mit Fluorsilanen unter Substitution zu (Me3Si)3CSiF2R (1 - 3, R = F, C6H5, CMe3). Mit lithiierten Aminen reagieren 1 und 2 zu den Aminofluorsilanen 4a, 5a, 6a, und unter 1, 3-Silylgruppenwanderung zu den strukturisomeren Trimethylsilylaminofluorsilanen 4 b, 5 b, 6 b, 7, 8. In der Reaktion von 1 mit LiNH2 wird die disubstituierte NH-Verbindung 9 erhalten.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845100324
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    Das Tris-trimethylsilyl-tert.butyl-cyclotetraphosphan (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 514 (1984), S. 69-71 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tris-trimethylsilyl-tert.butyl-cyclotetraphosphaneP4(SiMe3)3CMe3 1, which was previously unknown in the series of the cyclotetraphosphanes P4(SiMe3)nCMe34-n, n = 0-4, could be obtained by the reaction of P3(SiMe3)5 with Me3CPCl2. 1 froms intensely coloured yellow crystals, melting point 143 ± 2°C. The 31P- and 1H-NMR data of 1 are given.
    Notes: Das in der Reihe der Cyclotetraphosphane P4(SiMe3)n(CMe3)4-n, n = 0-4, bisher noch unbekannte P4(SiMe3)CMe3 1 konnte durch Umsetzung von P3(SiMe3)5 mit Me3CPCl2 dargestellt werden. 1 bildet intensiv gelbe Kristalle, Schmp. 143 ± 2°C. Die 31P- und 1H-NMR-Daten von 1 werden angegeben.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19845140708
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    [PPh3Cl]⊕[ReCl4(N2S2)]⊖ Synthese, IR-Spektrum und Kristallstruktur (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 514 (1984), S. 72-78 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [PPh3Cl]⊕[ReCl4(N2S2)]⊖; Synthese, IR-Spektrum und Kristall StruktureThe title compound is prepared by the reaction of [ReCl3(NSCl)2(POCl3)] with triphenylphosphane; it formes black crystals. The crystal structure determination was solved with X-ray methods (2861 observed independent reflexions, R = 0.038). The compound crystallizes monoclinic in the space group P21/n with four formula units per unit cell. The structure consists of [PPh3Cl]⊕ cations and [ReCl4(N2S2)]⊖ anions, in which the rhenium atom is surrounded octahedrally by four chlorine ligands and the N atoms of a ReN2S2-five-membered ring in cis-position (symmetry C2v). The Re—N bond lengths (181 pm) and the NS bond lengths (152 pm) are in the range of double bonds; the S—S distance is very long (253 pm). The i.r. spectrum is reported.
    Notes: Die Titelverbindung entsteht in Form schwarzer Kristalle bei der Reaktion von [ReCl3(NSCl)2(POCl3)] mit Triphenylphosphan. Die Kristallstruktur wurde mit Hilfe von Röntgenbeugungsdaten ermittelt ermittelt (2861 beobachtete unabhängige Reflexe, R = 0,038). Die Verbindung kristallisiert monoklin in der Raumgruppe P21/n mit vier Formeleinheiten pro Elementarzelle. Die Struktur besteht aus [PPh3Cl]⊕-Kationen und Anionen [ReCl4(N2S2)]⊖, in denen das Rhenium oktaedrisch von vier Chlorliganden und den beiden cis-ständigen Stickstoffatomen eines ReN2S2-Fünfringes umgeben ist (Symmetrie C2v). Die ReN-Abstände (181 pm) und die NS-Abstände (152 pm) entsprechen etwa Doppelbindungen; die S—S-Bindungslänge ist mit 253 pm sehr lang. Das IR-Spektrum wird mitgeteilt.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845140709
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    Zur Kenntnis der Fluoride zweiwertiger Lanthanoide. II. Über die Synthese von MLnF3 aus MLnF4 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 514 (1984), S. 92-98 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Fluorides of Divalent Lanthanoids. II. Synthesis of MLnF3 from MLnF4CsEuF3, CsYbF3, and RbYbF3, which had already been prepared via reduction of the corresponding trifluorides with alkali metal, were also obtained by reducing MLnF4 with M (M = Cs, Rb, K; Ln = Eu, Yb). No additional alkali fluoroperovskites of lanthanoids were detected either by reduction of LnF3 or MLnF4 with metallic Cs, Rb, or K or by other reactions, e.g. 3CsF + 2SmF3 + Sm. It was shown that the reaction of CsF with EuF2 (350-850°C) produced only very little CsEuF3.
    Notes: CsEuF3, CsYbF3 und RbYbF3, zuvor nur durch Reduktion von EuF3 bzw. YbF3 mit met. Cs bzw. Rb erhalten, entstehen auch bei der Reduktion von MLnF4 mit M (M = Cs, Rb, K; Ln = Eu, Yb). Weitere unbekannte Perowskite wie CsSmF3 erhält man auf diesem Wege nicht. Tempern von innigen Gemengen der binären Fluoride (z.B. CsF + EuF2) führt nur zu sehr unvollständiger Umsetzung. Auch Synthesen durch Komproportionierung (z. B. 3CsF + 2SmF3 + Sm) sind ohne Erfolg. Durchgeführt wurden alle Reduktionen von LnF3 (Ln = Sm, Eu, Tm, Yb) mit M (M = Cs, Rb, K).
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19845140712
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    Über Chalkogenolate. 139. Untersuchungen über Dialkylester von Chalkogenokohlensäuren. 2. O,Se- und S, Se-Dialkylmonothiomonoselenocarbonate (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 514 (1984), S. 120-128 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 139. Studies on Dialkyl Esters of Chalcogenocarbonic Acids. 2. O,Se- and S, Se-Dialkyl MonothiomonoselenocarbonatesThe hitherto unknown esters RSe—CS—OR′, where R = C2H5, nC3H7 and R′ = C2H5, nC3H7, are formed by reaction of NaSeR with Cl—CS—OR′ and of RSe—CS—Cl with HOR′. At the first time, the esters RSe—CO—SR′ with R = R′ = C2H5, nC3H7 have been prepared by reaction between NaSeR and Cl—CO—SR′. The compounds have been characterized by means of diverse spectroscopic methods.
    Notes: Die bisher nicht bekannten Ester RSe—CS—OR′ mit R = C2H5, nC3H7 und R′ = C2H5, nC3H7 entstehen bei der Reaktion von NaSeR mit Cl—CS—OR′ und bei der von RSe—CS—Cl mit HOR′. Erstmals wurden die Ester RSe—CO—SR′ mit R = R′ = C2H5, nC3H7 durch Umsetzung von NaSeR mit Cl—CO—SR′ hergestellt. Die genannten Verbindungen wurden mit Hilfe verschiedener spektroskopischer Methoden charakterisiert.
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    URL: http://dx.doi.org/10.1002/zaac.19845140716
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    Metall-Schwefelstickstoff-Verbindungen. 16. Reaktionsprodukte von Blei- und Zinnsalzen mit S4N4 Die Strukturen von PbN2S2 · NH3, PbN2S2 und SnCl4 · 2S4N4 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 514 (1984), S. 107-114 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal Sulfur Nitrogen Compounds. 16. Products of the Reaction of Lead- and Tin Salts with S4N4. Structures of PbN2S2 · NH3, PbN2S2, and SnCl4 · 2S4N4PbN2S2 · NH3 is monoclinic, P21/a, a = 5.671, b = 16.123, c = 6.102 Å, β = 95.12°, Z = 4, PbN2S2, however, orthorhombic, P212121, a = 4.375, b = 7.654, c = 12.274 Å, Z = 4. The planar five-membered PbN2S2 rings in both compounds show no remarkable differences. In PbN2S2 · NH3, the NH3 molecule is bound to Pb perpendicularly to the plane of the ring.The structure of the long known addition compound SnCl4 · 2S4N4 was determined. It is orthorhombic, Pc21b, a = 11.467, b = 11.995, c = 12.374 Å, Z = 4. Sn shows sixfold coordination, the two S4N4 rings are attached to Sn trans to each other via a N atom.
    Notes: PbN2S2 · NH3 kristallisiert monoklin, Raumgruppe P21/a mit a = 5,671 Å, b = 16,123 Å; c = 6,102 Å, β = 95,12°, Z = 4, PbN2S2 dagegen orthorhombisch, Raumgruppe P212121 mit a = 4,375 Å, b = 7,654 Å, c = 12,274 Å, Z = 4. Die ebenen fünfgliedrigen PbN2S2-Ringe beider Verbindungen unterscheiden sich nur unwesentlich. Bei PbN2S2 · NH3 ist an Pb zusätzlich noch ein NH3-Molekül senkrecht zur Ringebene gebunden.Von der schon lange bekannten Additionsverbindung SnCl4 · 2S4N4 konnte ebenfalls die Struktur bestimmt werden: orthorhombisch, Raumgruppe Pc21b mit a = 11,467 Å, b = 11,995 Å, c = 12,374 Å, Z = 4. Sn ist 6fach koordiniert, die beiden S4N4-Ringe sind über je ein N-Atom in Transstellung an Sn gebunden.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845140714
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    Zum Aufbau schlecht geordneter Calciumhydrogensilicate. VI. Chemische, ESR- und Mößbauer-spektroskopische Untersuchungen zum Einbau von Fe3+-Ionen in C—S—H(Di, Poly) (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 514 (1984), S. 149-163 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Structure of Ill-crystallized Calcium Hydrogen Silicates. VI. Chemical, ESR, and Mössbauer-Spectroscopic Investigations on the Incorporation of Fe3+ into C—S—H(Di, Poly)C—S—H(Di, Poly), prepared by precipitation reactions from sodium silicate solutions in presence of Fe3+ ions, incorporates at least up to 0.09 Fe2O3/SiO2. Thereby the anion composition of the C—S—H(Di, Poly) ist not affected.The results of ESR and Mössbauer spectroscopic measurements show, that Fe is incorporated as Fe3+ at octahedral sites. Only less than 1% of the total amount of Fe3+ is situated at tetrahedral sites. In good accordance with that is the change of thermal stability of the silicate anions concerning condensation and degradation reactions.
    Notes: In C—S—H(Di, Poly), das bei 80°C (353 K) über Fällungsreaktionen aus Natriumsilicatlösungen in Gegenwart von Fe3+-Ionen synthetisiert wurde, lassen sich bis mindestens 0,09 Fe2O3/SiO2 einbauen. Der Anionenaufbau des C—S—H(Di, Poly) wird dadurch nicht verändert. Aus ESR- bzw. Mößbauer-spektroskopischen Befunden geht hervor, daß das Eisen als Fe3+ hauptsächlich auf Oktaederplätzen vorliegt, während Tetraederplätze nur von weniger als 1% der Gesamteisenmenge besetzt werden. Die Änderung der thermischen Stabilität der Silicatanionen gegenüber Kondensations- und Abbaureaktionen steht mit dem Einbau von Fe3+ auf Oktaederplätzen in guter Übereinstimmung.
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    URL: http://dx.doi.org/10.1002/zaac.19845140719
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    Chalkogenfluoride in niedrigen Oxydationsstufen. IX.Als Teil VIII gilt [6]; Teil VII siehe [4]. Darstellung und Charakterisierung von SF3SSFTeilweise vorgetragen auf der Chemiedozententagung in Dortmund (14.-18. 3. 1983) und dem 8. Europäischen Fluorsymposium in Jerusalem (21.-26. 8. 1983). (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 514 (1984), S. 171-178 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Lower Chalcogen Fluorides. IX. Preparation and Characterization of SF3SSFDuring cocondensation of SF2 and SSF2 the new compound 1,3-Difluorotrisulphane-1,1-difluoride is formed in low yield and can be isolated by means of low temperature fractionation. The compound was unequivocally characterized by 19F-n.m.r,i.r.,Raman, and mass spectra. The unstable compound ist a colourless, viscous liquid with an extrapolated boiling point of 94°C and a melting point of -62°C. It decomposes to SF4 and SSF2 in the gas phase.
    Notes: Bei der Cokondensation von SF2 und SSF2 entsteht in geringen Ausbeuten die neue Verbindung 1,3-Difluor-trisulfan-1,1-difluorid, SF3SSF, die mittels Tieftemperaturfraktionierung isoliert werden konnte. Durch 19F-NMR-, IR-, Raman- und Massenspektren wurde die Verbindung eindeutig charakterisiert. Das sehr zersetzliche SF3SSF ist eine farblose, viskose Flüssigkeit mit einem extrapolierten Siedepunkt von 94°C und einem Schmelzpunkt von -62°C. Es zerfällt in der Gasphase in SF4 und SSF2.
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    URL: http://dx.doi.org/10.1002/zaac.19845140721
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    Formation and decomposition of Lanthanum Monoxocarbonate (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 514 (1984), S. 205-212 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Bildung und Zersetzung von LanthanoxidcarbonatAmorphes Lanthancarbonat wird durch Hydrolyse von Lanthanisopropoxid mit wäßriger Ammoniaklösung an Luft dargestellt. Lanthanoxidcarbonat, La2O(CO3)2 · H2O, kristallisiert, wenn die amorphe Substanz mit heißem Wasser gewaschen wird. Die Kristallisation und das thermische Verhalten des kristallinen Materials werden röntgenographisch, thermoanalytisch und IR-spektroskopisch untersucht. Die Zersetzung des La2O(CO3)2 · H2O in das IA-(LaO)2CO3 wird bei 440 bis 540°C beobachtet. Die Zersetzungsisothermen können durch eine gebrochene rationale Funktion beschrieben werden; die Aktivierungsenergie beträgt 42,6 kcal · mol-1. IA-(LaO)2CO3 zersetzt sich dann zum A-La2O3 bei 750 bis 870°C. Die Kinetik wird ebenfalls durch eine gebrochene rationale Funktion interpretiert; die Aktivierungsenergie beträgt 58,3 kcal · mol-1.
    Notes: Amorphous lanthanum carbonate was prepared by hydrolysis of lanthanum isopropoxide using ammonia water in the atmosphere. Lanthanum monoxocarbonate, La2O(CO3)2 · H2O, crystallizes when this amorphous material was washed with hot water. The crystallization and thermal behavior of the crystalline material are studied by X-ray diffraction, thermal analysis, and infrared spectroscopy. The decomposition of La2O(CO3)2 · H2O into type-IA (LaO)2CO3 is observed at 440 to 540°C. Decomposition isotherms are described by the contracting cube equation, the activation energy being 42.6 kcal mol-1. Type-IA (LaO)2CO3 subsequently decomposes to A-type La2O3 at 750 to 870°C. The kinetics is also interpreted in terms of the contracting cube equation, the activation energy being 58.3 kcal mol-1.
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    URL: http://dx.doi.org/10.1002/zaac.19845140725
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    Neues zum chemischen Transport von CuO und Cu2O (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 514 (1984), S. 240-240 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845140729
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    Beiträge zur Strukturchemie phosphorhaltiger Ketten und Ringe. 11. Die Kristall- und Molekülstrukturen der beiden Konfigurationisomeren des Tetraphospha-silaspiro[2.2]pentans (PBut)2Si(PBut)2Die Ergebnisse dieser Untersuchung sind am 9. 8. 1983 auf dem “Eighth European Crystallographic Meeting” (ECM 8) in Lüttich kurz mitgeteilt worden [2]. (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 7-18 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Structural Chemistry of Phosphorus Containing Chains and Rings. 11. Crystal and Molecular Structures of the Two Stereoisomers of Tetraphospha-silaspiro[2.2]pentane (PBut)2Si(PBut)2The spirocyclic compound 1,2,4,5-tetra-tert-butyl-1,2,4,5-tetraphospha-3-silaspiro[2.2]pentane exists in tow diastereomers of point symmetry 4 and 2. The isomer with symmetry 4 even in the solid crystallizes tetragonally in I41/a with a = 1247.0, c = 1505.5 pm and Z = 4. The isomer of fairly exact symmetry 2 crystallizes triclinically in P1 with a = 612.8, b = 996.3, c = 1017.2 pm, α = 75.63, β = 72.38, γ = 88.71° and Z = 1. In this disordered structure the surroundings of Si is slightly distorted due to the influence of the substituents. The (average) bond lengths are (4, 2): d(Si—P) = 220.09(9), 221.5(5); d(P—P) = 225.5(2), 224.2(5); d(P—C) = 189.4(3), 190(2); d(C—C) = 151.4(4), 152(3) pm. The geometry of the substituents in both isomers is quite normal.
    Notes: Die Spiroverbindung 1,2,4,5-Tetra-tert-butyl-1,2,4,5-tetraphospha-3-silaspiro[2.2]pentan liegt in zwei Diastereomeren der Punktsymmetrie 4 und 2 vor. Das Isomer der auch im Festkörper exakten Symmetrie 4 kristallisiert tetragonal in der Raumgruppe I41/a mit a = 1247,0, c = 1505,5 pm und Z = 4. Das sterisch weniger günstige Isomer der im Festkörper nicht streng erfüllten Symmetrie 2 kristallisiert triklin in der Raumgruppe P1 mit a = 612,8, b = 996,3, c = 1017,2 pm, α = 75.63, β = 72,38, γ = 88,71° und Z = 1. In dieser nur fehlgeordnet beschreibbaren Struktur wird die Umgebung des Si durch Substituenteneinflüsse etwas verzerrt. Die (mittleren) Bindungslängen betragen (4, 2): d(Si—P) = 220,09(9), 221,5(5); d(P—P) = 225,5(2), 224,2(5); d(P—C) = 189,4(3), 190(2); d(C—C) = 151,4(4), 152(3) pm. Die Geometrie der Substituenten ist in beiden Isomeren normal.
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    Synthesen des Anions S3N3O2-, eines stabilen sechsgliedrigen Schwefel-Stickstoff-Ringes mit einem 8π-Elektronengerüst (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 51-60 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Syntheses of the Anion S3N3O2-, a Stable Six-membered Sulfur-Nitrogen Ring with an 8π-Electron SkeletonThe dark blue-violet cyclotrithiazene-dioxide anion S3N3O2-has been synthesized on different pathways: 1. reaction of S4N4O2 with alkali azides, 2. metathesis of (CH3)3ES3N3O2 (E = Si, Sn) with CsF, 3. addition of S4N4O2 and alkali bis(trimethylsilyl)-amides followed by cation exchange with tetraphenylarsonium chloride, and 4. reaction of S4N4O2 with trimethylsilyliminotriphenylphosphorane in a molar ratio of 1:1. Excess iminophosphorane leads to the formation of a covalent 1.5-disubstituted S4N4 derivative. Reaction mechanisms will be discussed and structures of trithiatriazine-anions will be compared.
    Notes: Das dunkelblauviolette Cyclotrithiatriazendioxid-Anion S3N3O2- konnte auf verschiedenen Wegen dargestellt werden: 1. Umsetzung von S4N4O2 mit Alkaliaziden, 2. Reaktion von (CH3)3ES3N3O2 (E = Si, Sn) mit CsF, 3. Addition von S4N4O2 und Alkali-bis(trimethylsilyl)-amiden mit anschließendem Kationenaustausch mit Tetraphenylarsoniumchlorid und 4. Umsetzung von S4N4O2 mit Trimethylsilyliminotriphenylphosphoran im Molverhältnis von 1:1. Ein überschuß des Iminophosphorans führt zur Bildung eines kovalenten 1,5-disubstituierten S4N4-Derivats. Reaktionsmechanismen werden diskutiert und Strukturvergleiche an Trithiatriazinanionen durchgeführt.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845150806
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    Die Reaktionen von Eisen(III)-chlorid mit Trithiazylchlorid. Die Kristallstruktur von [S4N4Cl]+[FeCl4]⊖ (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 69-80 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Reactions of Iron Trichloride with Trithyazyl Chloride. Crystal Structure of [S4N4Cl]+[FeCl4]-Iron trichloride reacts with (NSCl)3 yielding S4N4[FeCl4]2, S3N3Cl2[FeCl4] or S4N4Cl[FeCl4], depending on the reaction conditions. The i.r. spectra prove the presence of [FeCl4]⊖ ions for all three compounds. The 57Fe-Mössbauer spectra show a slight quadrupole splitting at 80 K for S3N3Cl2[FeCl4] (ΔEQ = 0.42 mm · s-1) and S4N4Cl[FeCl4] (ΔEQ = 0.23 mm · s-1), which indicates a slight deformation of the FeCl4⊖ tetrahedra. The crystal structure of S4N4Cl[FeCl4] was determined and refined with X-ray diffraction data (2549 independent reflexions, R = 0.026). S4N4Cl[FeCl4] crystallizes in the triclinic space group P1 with two formula units per unit cell. The lattice constants are a = 712, b = 911, c = 1006 pm, α = 76.5°, β = 83.8° and γ = 80.5°. The structure consists of the so far unknown [S4N4Cl]⊕ cations and slightly deformed FeCl4⊖ ions. The [S4N4Cl]⊕ ion consists of a S4N4 ring built up of two nearly planar S3N2 fragments having a dihedral angle of 136°. The average SN bond length is 157 pm, the SCI bond length 214 pm.
    Notes: Eisen(III)-chlorid reagiert mit (NSCl)3 je nach den angewandten Versuchsbedingungen unter Bildung von S4N4[FeCl4]2, S3N3Cl2[FeCl4] oder S4N4Cl[FeCl4]. Nach den IR-Spektren enthalten alle Verbindungen das FeCl4⊖-Anion. Die 57Fe-Mößbauer-Spektren lassen anhand der endlichen Beträge der Quadrupolaufspaltung bei 80 K für S3N3Cl2[FeCl4] (ΔEQ = 0,42 mm · s-1) und für S4N4Cl[FeCl4] (ΔEQ = 0,23 mm · s-1) leicht verzerrte FeCl4⊖-Tetraeder erkennen. Die Kristallstruktur von S4N4Cl[FeCl4] wurde mit Hilfe von Röntgenbeugungsdaten ermittelt und verfeinert (2549 unabhängige, beobachtete Reflexe, R = 2,6%). S4N4Cl[FeCl4] kristallisiert in der triklinen Raumgruppe P1 mit zwei Formeleinheiten pro Elementarzelle. Die Gitterkonstanten sind a = 712, b = 911, c = 1006 pm; α = 76,5°, β = 83,8°, γ = 80,5°. Die Struktur besteht aus dem bisher unbekannten [S4N4Cl]⊕-Kation und leicht verzerrten FeCl4⊖-Anionen. Das [S4N4Cl]⊕-Ion bildet einen S4N4-Achtring, der aus zwei zueinander gefalteten, nahezu ebenen Ringfragmenten S3N2 besteht mit einem Faltungswinkel von 136°. Der mittlere SN-Bindungsabstand beträgt 157 pm, die S—Cl-Bindungslänge 214 pm.
    Additional Material: 3 Ill.
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    Zur Kenntnis von Li2[CuO2] [1, 2] (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 95-100 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Li2[CuO2]At the first time single crystals of Li2[CuO2] are prepared by exchange reaction. The crystal structure (I mmm) with a = 365.4(0), b = 285.9(0), c = 937.4(0) pm, Z = 2, dx = 3.73 g/cm3, dpyk = 3.67 g/cm3 was refined (four-circle-diffractometer data PW 1100, 343 Io(hkl), MoKα, R = 0.046, Rw = 0.041). The characteristic structure element is the planar chain \documentclass{article}\pagestyle{empty}\begin{document}$ {}_\infty ^1 \left[{{\rm CuO}_{4/2}} \right]^{2 -} $\end{document}. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated.
    Notes: Einkristalle von Li2[CuO2] wurden erstmals durch „Austauschreaktion“ dargestellt und die Kristallstruktur (I mmm) mit a = 365,4(0), b = 285,9(0), c = 937,4(0) pm, Z = 2, drö = 3,73 g/cm3, dpyk = 3,67 g/cm3 aufgeklärt (Vierkreisdiffraktometerdaten, PW 1100, 343 Io(hkl), MoKα, R = 0,046, Rw = 0,041). Das charakteristische Strukturelement ist die planare Ketve \documentclass{article}\pagestyle{empty}\begin{document}$ {}_\infty ^1 \left[{{\rm CuO}_{4/2}} \right]^{2 -} $\end{document}. Der Madelunganteil der Gitterenergie, MAPLE, Effektive Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, werden berechnet.
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    Über Polygermane. X. Schwingungsspektren der Homocyclen (Ph2Ge)4, (Ph2Ge)5 und (Ph2Ge)6 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 141-146 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Polygermanes. X. Vibrational Spectra of the Homorings (Ph2Ge)4, (Ph2Ge)5, and (Ph2Ge)6IR and Raman transitions of the crystalline title compounds are given from 3100 to 100 cm-1. The spectra are nearly identical above 350 cm-1. The Gen ring vibrations range from 330 to 140 cm-1 and are unspecifically coupled with mass sensitive phenyl modes. The distribution of the individual values is discussed by means of the intracyclic bond angles determined by X-ray structure analysis.
    Notes: Für die kristallinen Titelverbindungen werden IR- und Raman-Übergänge im Bereich 3100-100 cm-1 angegeben. Oberhalb 350 cm-1 sind die Spektren weitgehend identisch. Die Gerüstschwingungen der Gen-Homocyclen liegen von 330-140 cm-1 und koppeln in unspezifischer Weise mit Phenylgruppenschwingungen. Die Verteilung der Einzelwerte wird an Hand von röntgeno-graphisch bestimmten intracyclischen Bindungswinkeln diskutiert.
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    Über Chalkogenolate. 141. Untersuchungen über Trimethylsilylxanthogensäure. 1. Darstellung und Eigenschaften von Trimethylsilylxanthaten (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 173-181 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Chalcogenolates. 141. Studies on Trimethylsilyl Xanthic Acid. 1. Synthesis and Properties of Trimethylsilyl XanthatesThe trimethylsilyl xanthates \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm M}\left[{{\rm S}_2 {\rm C} - {\rm OSi}\left({{\rm CH}_3} \right)_3} \right]\,{\rm mit\,M} = {\rm Li,Na,K},{\rm Rb},{\rm Cs} $$\end{document} have been prepared by reaction of the corresponding silanolate with carbon disulfide. The compounds were characterized by means of chemical and diverse spectroscopic methods.The existence of unstable trimethylsilyl xanthic acid has been demonstrated.
    Notes: Die Trimethylsilylxanthate \documentclass{article}\pagestyle{empty}\begin{document}$$ {\rm M}\left[{{\rm S}_2 {\rm C} - {\rm OSi}\left({{\rm CH}_3} \right)_3} \right]\,{\rm mit\,M} = {\rm Li,Na,K},{\rm Rb},{\rm Cs} $$\end{document} wurden durch Umsetzung des entsprechenden Silanolats mit Kohlenstoffdisulfid hergestellt und mit Hilfe chemischer und verschiedener spektroskopischer Methoden charakterisiert.Die Existenz der instabilen Trimethylsilylxanthogensäure konnte gesichert werden.
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    URL: http://dx.doi.org/10.1002/zaac.19845150820
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    Über die Trithiocyanatoargentate Rb2Ag(SCN)3 und Cs2Ag(SCN)3 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 199-206 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Trithiocyanatoargentates Rb2Ag(SCN)3 and Cs2Ag(SCN)3The trithiocyanatoargentates Rb2Ag(SCN)3 and CsAg(SCN)3 are obtained by crystallization from highly concentrated aqueous solutions. In the crystal structures the Ag atoms are surrounded tetrahedrally by the S atoms of 4 SCN groups. These Ag(SCN)4 tetrahedra are connected by common corners to polymer \documentclass{article}\pagestyle{empty}\begin{document}$ {}_\infty ^1 \left[{{\rm Ag}\left({{\rm SCN}} \right)_2 \left({{\rm SCN}_{2/2}} \right)} \right] $\end{document}1[Ag(SCN)2(SCN)2/2] anion in Rb2Ag(SCN)3, whereas dimeric Ag2(SCN)6 anions were found in the Cs compound.
    Notes: Die Trithiocyanatoargentate Rb2Ag(SCN)3 und Cs2Ag(SCN)3 können durch Kristallisation aus hochkonzentrierten wäßrigen Lösungen erhalten werden. In den Kristallstrukturen sind die Ag-Atome tetraedrisch durch die S-Atome von vier SCN-Gruppen umgeben. Diese Ag(SCN)4-Tetraeder sind in der Rb-Verbindung über zwei Ecken zu einem polymeren \documentclass{article}\pagestyle{empty}\begin{document}$ {}_\infty ^1 \left[{{\rm Ag}\left({{\rm SCN}} \right)_2 \left({{\rm SCN}_{2/2}} \right)} \right] $\end{document}1[Ag(SCN)2(SCN)2/2]-Anion verknüpft, während bei der Cs-Verbindung zweikernige Ag2(SCN)6-Anionen gebildet werden.
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    URL: http://dx.doi.org/10.1002/zaac.19845150823
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    Dichte, Leitfähigkeit und Elektrolyse flüssiger Phasen in wasserfreien Systemen vom Typ MCl/AlCl3/SO2 (M = Li, Na) (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 187-198 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Density, Conductivity, and Electrolysis of Liquid Phases in Nonaqueous Systems of the Type MCl/AlCl3/SO2 (M = Li, Na)The temperature dependence of the density and specific conductivity was determined at liquid phases of the composition MAlCl4 · nSO2 + mAlCl3 (M = Li, n = 3-5.5, m = 0.266; M = Na, n = 1.36-4.56, m = 0.01-0.1). The investigated range was between -30°C and +45°C. For different compositions it was limited by the liquidus point and by the point, where the SO2-equilibrium pressure surpassed 1 bar. The densities are between 1.63 and 1.76 g/cm3, the specific conductivities between 0.03 and 0.07 Ω-1 · cm-1.In diluted solutions below -10°C NaAlCl4 behaves as a strong electrolyte in which dissociation in Na+ and AlCl4-is prevailing. By electrolysis of the liquid phases at room temperature reversible galvanic cells of the type M/MAlCl4 · nSO2/Cl2, C(M = Li, Na) are generated, which have an open circuit potential between 4.12 and 4.18 volts. The alkali metal deposits are stable in contact with the electrolyte up to 60°C in the case of lithium and 35°C with sodium.
    Notes: Die Temperaturabhängigkeit der Dichte und der Leitfähigkeit flüssiger Phasen der Zusammensetzung MAlCl4 · nSO2 + mAlCl3 (M = Li, n = 3-5,5, m = 0,266; M = Na, n = 1,36-4,56, m = 0,01-0,1) wurde gemessen im Bereich zwischen der Liquidustemperatur und der Temperatur, bei der der SO2-Gleichgewichtsbruck 1 bar erreicht (-30°C bis +45°C). Die Dichten liegen zwischen 1,63 bis 1,76 g/cm3 und die spezifischen Leitfähigkeiten zwischen 0,03 bis 0,07 Ω-1 · cm-1 · NaAlCl4 verhält sich in verdünnten SO2-Lösungen bei -10°C bis -20°C als starker Elektroyt, der überwiegend in Na+ und AlCl4- dissoziiert vorliegt. Bei der Elektrolyse entstehen reversible Galvanische Zellen vom Typ M/MAlCl4 · nSO2/Cl2, C (M = Li, Na), deren EMK 4,12 bis 4,18 V beträgt. Die Alkalimetallabscheidung ist im Kontakt mit dem Elektrolyten im Falle des Lithiums bis +60°C beim Natrium bis +35°C stabil. An Graphit-Pulveranoden entstehen neben gelöstem Chlor Cl(AlCl3)3-Intercalate.
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    URL: http://dx.doi.org/10.1002/zaac.19845150822
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    The CaO—MgO—P2O5 System at 1000°C for P2O5 ≤ 33.3 mole % (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 213-224 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Das CaO—MgO—P2O5-System bei 1000°C für P2O5 ≤ 33,3 Mol-%Das quasiternäre Phasendiagramm CaO—MgO—P2O5 bei 1000°C für P2O5 ≤ 33,3 Mol-% wurde bestimmt durch Erhitzen von 140 Mischungen unter Verwendung von vier Ausgangsmaterialien (CaHPO4, CaCO3, MgO und MgHPO4 · 3 H2O). Die Produkte wurden röntgenographisch untersucht und die Temperung fortgeführt bis keine Änderung in der Phasenzusammensetzung und der Peakposition der Röntgendiagramme beobachtet wurde, was gegebenenfalls zu Temperzeiten von über 1000 Stunden führte.Es existieren drei bevorzugte Bereiche für feste Lösungen: die Whitlockit-Phase und bei den ternären Verbindungen im Gebiet der Pyro- und Orthophosphatphase. Der Bereich der festen Lösung der ternären Pyrophosphat-Verbindung wurde durch die Änderung in der Peakposition der Röntgendiagramme mit der Zusammensetzung bestimmt und wurde zu 15,9 bis 27,5 Mol-% MgO gefunden.Die Zwei- und Dreiphasengebiete wurden aus der Änderung der Peakposition der Whitlockit und ternären Pyrophosphat-Verbindung bestimmt. Die Experimente wurden in Luft ausgeführt. Zusätzliche Versuche in CO2-Atmosphäre zeigten keine Änderungen in den Röntgendiagrammen, besonders in jenen in denen Apatit enthalten war. Die Apatitphase baute keine bestimmbare Menge von Mg ein, weder beim Tempern in Luft noch in CO2-Atmosphäre.
    Notes: The quasi ternary phase diagram CaO-MgO-P2O5 at 1000°C for P2O5 ≤ 33.3 mole-% is determined by heating some 140 compositions prepared from the appropriate ones of 4 starting chemicals (reagent grade CaHPO4, CaCO3, MgO, and MgHPO4 · 3 aq.). Products were investigated with X-ray diffraction and heating was continued until no more changes in phase composition and peak positions in the X-ray diffraction pattern were observed, leading occasionally to heating times of over 1000 hours.There are three major regions of solid solution: for the whitlockite phase, and for the ternary compounds on the pyro- and the ortho-phosphate join. The extent of solid solution of the ternary pyrophosphate compound was determined by the change in peak position in the X-ray diffraction pattern with composition and was found to be 15.9-27.5 mole-% MgO.Two and three phase areas were determined using the change in peak position data for the whitlockite and ternary pyrophosphate compound. The experiments were carried out in air. However additional experiments in a CO2 atmosphere revealed no changes in the X-ray diffraction patterns, apart from those in which apatite was involved. The apatite phase did not incorporate detectable amounts of Mg, not on heating in air nor on heating in a carbondioxide atmosphere.
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    Zur Existenz und Struktur der sekundären Dithizonate (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 230-240 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Existence and Structure of Secondary DithizonatesOn example of complexation with copper and palladium proved, that dithizone by double deprotonation forming neutral “secondary” dithiozonates, which have been characterized by elemental analyses, electronic, i.r., ESCA, and EPR spectra and magnetic measurements. Dithizone reacts about ligator atoms N,N′,S. Secondary dithizonates probable are present dimeric.
    Notes: Am Beispiel der Komplexbildung mit Kupfer und Palladium wird nachgewiesen, daß Dithizon unter zweifacher Deprotonierung neutrale, „sekundäre“ Dithizonate bildet, die durch Elementaranalyse, VIS-, IR-, EPR- und Photoelektronen-Spektren sowie magnetische Messungen charakterisiert werden. Dithizon wirkt über die Ligatoratome N,N′,S. Die sekundären Dithizonate liegen wahrscheinlich dimer vor.
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    Beiträge zur Chemie des Phosphors. 142. P6(t-Bu)5H - das erste Cyclotetraphosphan mit P2-SeitenketteProfessor Walter Rüdorff zum 75. Geburtstage am 3. Oktober 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 516 (1984), S. 7-12 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Phosphorus. 142. P6(t-Bu)5H - the First Cyclotetraphosphane with a P2 Side ChainThe thermolysis of 1, 2-di-tert-butyldiphosphane, H(t-Bu)P—P(t-Bu)H, leads to formation of the hitherto unknown hexaphosphane P6(t-Bu)5H (1). In the first instance the iso-P5H5 derivative P5(t-Bu)4H [3] is formed, which reacts further with H2(t-BuP)2 or H2(t-BuP)3 yielding 1. Compound 1 has been isolated in the pure state and structurally characterized as 1-(1,2-di-tert-butyldiphosphino)-2, 3, 4-tri-tert-butyl-cyclotetraphosphane, i. e. as a four-membered ring compound with a P2 side chain. Due to the chirality of the P atoms in the side chain, 1 exists as a mixture of two configurational isomers, the threo-and the erythro-form.
    Notes: Bei der Thermolyse von 1, 2-Di-tert-butyldiphosphan, H(t-Bu) P—P(t-Bu) H, entsteht aus dem zunächst gebildeten iso-P5H5-Derivat P5(t-Bu)4H [3] durch Weiterreaktion mit H2(t-BuP)2 oder H2(t-BuP)3 das bislang unbekannte Hexaphosphan P6(t-Bu)5H (1). Verbindung 1 wurde in reiner Form isoliert und strukturell als 1-(1, 2-Di-tert-butyldiphosphino)-2, 3, 4-tri-tert-butyl-cyclotetraphosphan, d. h. als Vierring-Verbindung mit P2-Seitenkette, charakterisiert. Wegen der Chiralität der P-Atome in der Seitenkette liegt 1 als Gemisch aus zwei Konfigurationsisomeren, der threo- und erythro-Form, vor.
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    Polymere Thiolatokomplexe [M(SPh)3]∞ der Metalle Molybdän, Wolfram, Eisen und Ruthenium mit linearen Metallketten. Synthese und Struktur von (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3 · 2(CH3)2COProfessor Walter Rüdorff zum 75. Geburtstage am 3. Oktober 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 516 (1984), S. 19-29 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Polymeric Thiolato Complexes [M(SPh)3]∞ of the Metals Mo, W, Fe, and Ru with Linear Metal Chains. Synthesis and Crystal Structure of (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3 · 2(CH3)2COAt high temperature the reaction of the metal carbonyls Mo(CO)6, W(CO)6 and Fe(CO)5 with S2Ph2 (Ph = C6H5) yields the polymeric complexes [M(SPh)3]∞. Similarly [Ru(SPh)3]∞ can be obtained from ruthenium(III) acetylacetonate and HSPh. At room temperature under UV-irradiation Fe(CO)5 reacts with S2Ph2 to form the oligomeric complex (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3.The polymeric complexes [M(SPh)3]∞ (M = Mo, W, Fe, Ru) are composed of linear chains with bridging SPh-ligands between the metal atoms. Of these complexes [Fe(SPh)3]∞ is paramagnetic, whereas the others exhibit antiferromagnetic behaviour. The spin coupling is presumably connected with the formation of metal pairs, resulting in alternating shortened and extended distances in the metal chain. The oligomeric complex (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3 crystallizes triclinic in the space group P1 with z = 2. It has almost the symmetry D3d with a linear arrangement of the Fe atoms. The paramagnetism of Fe3(CO)6(SPh)6 can be explained by a d6 high spin configuration of the central atom and low spin behaviour of the two other Fe atoms, which are bonded to CO.
    Notes: Bei höherer Temperatur reagieren die Metallcarbonyle Mo(CO)6, W(CO)6 und Fe(CO)5 mit S2Ph2 (Ph = C6H5) unter Bildung der polymeren Komplexe [M(SPh)3]∞. Aufähnliche Weise kann [Ru(SPh)3]∞ aus Ruthenium (III)-acetylacetonat und HSPh erhalten werden. Bei Raumtemperatur unter UV-Bestrahlung führt die Reaktion von Fe(CO)5 mit S2Ph2 zum oligomeren Komplex (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3. Die polymeren Komplexe [M(SPh)3]∞ bestehen aus linearen Ketten, in denen die Metallatome durch SPh-Brücken verknüpft sind. [Fe(SPh)3]∞ ist paramagnetisch mit μ = 5,2 B.M., während die Komplexe des Mo, W und Ru antiferromagnetisches Verhalten zeigen. Die Spinkopplung ist vermutlich mit der Ausbildung von Metallpaaren verbunden, die alternierend lange Abstände in der Metallkette bewirken. Der oligomere Komplex (OC)3Fe(SPh)3Fe(SPh)3Fe(CO)3 kristallisiert triklin in der Raumgruppe P1 mit z = 2. Er hat nahezu die Symmetrie D3d, wobei die Fe-Atome eine lineare Anordnung bilden. Der Paramagnetismus von Fe3(CO)6(SPh)6 (μ = 6,15 B.M.) kann mit einer d6 high spin Konfiguration des Zentralatoms und low spin Verhalten der endständigen Fe-Atome erklärt werden.
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    Schwingungsspektren des käfigstrukturierten PAs3S3Professor Walter Rüdorff zum 75. Geburtstage am 3. Oktober 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 516 (1984), S. 42-48 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Vibrational Spectra of the Cage Compound PAs3S3The vibrational spectrum of crystalline PAs3S3 and the raman spectrum of the molten title compound have been recorded. The assignment of the frequencies is proposed mainly based on polarization data of a PAs3S3 solution in white phosphorus. In the molten state a partial decomposition takes place according to 2 PAs3S3 ⇌ P2As2S3 + α-As4S3.
    Notes: Das Schwingungsspektrum des kristallinen PAs3S3 und das Raman-Spektrum der geschmolzenen Titelverbindung wurden aufgenommen. Die Zuordnung der Schwingungsfrequenzen wird, vor allem basierend auf Polarisationsdaten einer PAs3S3-Lösung in weißem Phosphor, vorgeschlagen. Im geschmolzenen Zustand findet ein partieller Zerfall gemäß 2 PAs3S3 ⇌ P2As2S3 + α-As4S3 statt.
    Additional Material: 4 Ill.
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    Photoelektronenspektroskopie an NiobiodidenProfessor Walter Rüdorff zum 75. Geburtstage am 3. Oktober 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 516 (1984), S. 55-66 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Photoelectron Spectroscopy on Niobium IodidesThe photoelectron spectra (AlKα, HeI) of NbI5, NbI4, Nb3I8, Nb6I11, HNb6I11, Nb6I8(CH3NH2)6, Nb6I8(C3H7NH2)6, and Nb are measured and discussed. It is shown that the binding energy of the niobium core levels depends linearly on the oxidation number n (n = I/Nb). The relation BE = 201.8 + 1.07 · n holds for the Nb 3d5/2 level. Using this relation the hydridic character of the hydrogen in HNb6I11 becomes plausible and the increased electron concentration of the Nb6I8 cluster in the compounds Nb6I8(CH3NH2)6 and Nb6I8(C3H7NH2)6 is verified. Energy gaps Eg = 0.40 (0.45) eV are found for Nb6I11(HNb6I11) and for the amines the top of the valence band is 0.70 (CH3NH2) and 0.68 eV (C3H7NH2), resp. below the Fermi level.
    Notes: Es werden die Photoelektronenspektren (AlKα, HeI) von NbI5, NbI4, Nb3I8, Nb6I11, HNb6I11, Nb6I8(CH3NH2)6, Nb6I8(C3H7NH2)6 und Nb gemessen und diskutiert. Es läßt sich zeigen, daß die Bindungsenergie BE der Niob-Rumpfniveaus linear von der Oxydationszahl n (n = I/Nb) abhängt; für das Nb 3d5/2-Niveau ergibt sich die Beziehung BE = 201,8 + 1,07 · n. Durch Anwendung dieser Beziehung wird der hydridartige Charakter des Wasserstoffs in HNb6I11 wahrscheinlich gemacht sowie die Zunahme der Elektronenkonzentration im Nb6I8-Cluster der Verbindungen Nb6I8(CH3NH2)6 und Nb6I8(C3H7NH2)6 belegt. Für Nb6I11(HNb6I11) ergibt sich eine verbotene Zone Eg = 0,40 (0,45) eV, für die Amine ist der Abstand der Oberkante des Valenzbandes zur Fermi-Kante 0,70 (CH3NH2) bzw. 0,68 eV (C3H7NH2).
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845160909
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    Hydroxidmonohydrate des Kaliums und Rubidiums; Verbindungen, deren Atomanordnungen die Schreibweise K(H2O)OH bzw. Rb(H2O)OH nahelegenProfessor Walter Rüdorff zum 75. Geburtstage am 3. Oktober 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 516 (1984), S. 67-78 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Hydroxide Monohydrates of Potassium and Rubidium; Compounds with Atomic Arrangements which Suggest the Formula K(H2O)OH and Rb(H2O)OHSingle crystals for x-ray structure investigations of the monohydrates of potassium and rubidium hydroxides were obtained by recrystallization of microcrystalline sampels in supercritical ammonia as solvent. The structure determination on both structurally closely related compounds was successful up to the localization of the hydrogen positions. Besides the monohydrates were characterized by IR spectra and thermochemical data.The atomic arrangement of the compounds is discussed in comparison to the one of substances as PbFCl, γ-AlOOH etc. In addition to the chemical bonds in the stated compounds both monohydrates show one-dimensional infinite hydrogen bridges between the H atoms of the water molecules and the hydroxide ions; furthermore weak H bonds connect the OH- ions. Because the hydroxide ions are involved in two bridge-bindung systems water molecules are the nearest neigh-bours of the cations.
    Notes: Für die röntgenographische Strukturbestimmung geeignete Kristalle der Monohydrate des Kalium- und Rubidiumhydroxids wurden durch Rekristallisation der pulverförmigen Substanzen in überkritischem Ammoniak als Lösungsmittel erhalten. Die Strukturbestimmung an beiden, strukturell eng verwandten Verbindungen gelang einschließlich der Lagebestimmung der Wasserstoffatome. Außerdem wurden beide Monohydrate durch die IR-Spektren und durch thermochemische Daten charakterisiert.Der Aufbau der Verbindungen wird in Zusammenhang mit dem anderer Stoffe wie PbFCl, γ-AlOOH etc. diskutiert. Zusätzlich zu den Bindungsverhältnissen in den angegebenen Substanzen treten in beiden Monohydraten starke, eindimensional unendliche Wasserstoffbrückenbindungen zwischen den H-Atomen der Wassermoleküle und den Hydroxidionen auf; außerdem liegen schwache Brückenbindungen zwischen den Hydroxidionen vor. Die Einbindung der OH--Ionen in die Brückenbindungssysteme bedingt, daß Wassermoleküle zu nächsten Nachbarn der Kationen werden.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845160910
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    Züchtung und Untersuchung von Einkristallen in den pseudobinären Systemen ABS2—SnS2 (A = Cu, Ag; B = Al, Cr)Professor Walter Rüdorff zum 75. Geburtstage am 3. Oktober 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 516 (1984), S. 102-106 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Characterization of Single Crystals in the Pseudo-binary Systems ABS2—SnS2 (A = Cu, Ag; B = Al, Cr)In the pseudo-binary systems ABS2—SnS2 (A = Cu, Ag; B = Al, Cr) single crystals were grown by chemical transport using AlCl3/I3 mixtures as transporting agents. Characterization of the crystals was done by electron microprobe analyses and X-ray methods. The composition A1-x□x[B1-xSb1+x]S4 was found for the non-stoichiometric phases. The compounds are normal spinels, the space group is Fd3m. The results of least squares refinement using single crystal X-ray data are reported.
    Notes: In den pseudobinären Systemen ABS2—SnS2 (A = Cu, Ag; B = Al, Cr) wurden durch chemische Transportreaktionen mit AlCl3/I2-Gemischen als Transportmittel Einkristalle gezüchtet. Die Charakterisierung der Kristalle erfolgte mit der Elektronenstrahlmikrosonde und mit Röntgenmethoden. Nichtstöchiometrische Phasen der Zusammensetzung A1-x□x[B1-xSn1+x]S4 wurden gefunden. Die Verbindungen sind normale Spinelle, die Raumgruppe ist Fd3m. Die Ergebnisse der Strukturverfeinerung, ermittelt aus Einkristall-Röntgendaten, werden angegeben.
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    URL: http://dx.doi.org/10.1002/zaac.19845160914
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    27Al-MAS-NMR- und IR-spektroskopische Untersuchungen zur Aluminium-Koordination in röntgenamorphen SiO2 —Al2O3-Festkörpern (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 517 (1984), S. 167-176 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 27Al MAS N.M.R. and I.R. Investigations on the Aluminium Coordination in Amorphous Silica-Alumina GelsAmorphous silica-alumina of different Si/Al ratios have been investigated by 27Al magic-angle spinning n.m.r. (MAS n.m.r.) and i.r. spectroscopy. Aluminosilicate framework structures were found for the Na+- and NH4+-exchanged forms of the investigated gels. The thermal deammoniation of the NH4+-exchanged gels, producing the H+ forms, causes an irreversible damage of the aluminosilicate framework. This process is accompanied by a change of the coordination state of a part of the aluminium, converting AlO4 into AlO6 units. The progress of the solid-state reaction upon further thermal treatment of the H+ forms is reflected by a considerable broadening of the n.m.r. spectra and a decrease of the intensity. The possibility that well-known results, including those of nonframework aluminium, obtained for comparable zeolitic systems may also be valid for amorphous solids, is discussed.
    Notes: Es wurden röntgenamorphe SiO2—Al2O3-Festkörper unterschiedlicher Si/Al-Verhältnisse mit der 27Al-NMR-Spektroskopie unter Verwendung der schnellen Probenrotation um den Magischen Winkel (MAS) untersucht und IR-spektroskopisch charakterisiert. Die Na- und NH4-Formen dieser Substanzen besitzen Alumosilicatstruktur. Die zu den H-Formen führende thermische Deammonisierung der NH4-Formen bewirkt eine irreversible strukturelle Schädigung des Alumosilicatgerüsts. Dabei wird ein Teil der AlO4-Einheiten unter Koordinationszahlwechsel in AlO6-Einheiten umgewandelt. Das Fortschreiten der Festkörperreaktion mit weiterer thermischer Behandlung der H-Formen zeigt sich in einer starken Verbreiterung der NMR-Signale und in einer Verringerung der Nachweisintensität. Die Übertragbarkeit entsprechender Beobachtungen an vergleichbaren Zeolithen einschließlich des Auftretens von „Extragitter“-Aluminium auf amorphe Analoga wird diskutiert.
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    URL: http://dx.doi.org/10.1002/zaac.19845171016
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    Darstellung und Struktur der Verbindung Ca14AlSb11 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 519 (1984), S. 183-188 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Preparation and Structure of Ca14AlSb11The new compound Ca14AlSb11 crystallizes in the tetragonal system, space group I41/acd (No. 142) with lattice constants s. „Inhaltsübersicht“. In the structure there are Sb3- ions and complex tetrahedral AlSb49- and linear Sb37- anions. The compound can be interpreted as valence compound.
    Notes: Die neue Verbindung Ca14AlSb11 kristallisiert tetragonal in der Raumgruppe I41/acd (Nr. 142) mit den Gitterkonstanten a = 1667,6(5) pm, c = 2242,3(7) pm, c/a = 1,345.In der Struktur liegen neben Sb3--Ionen komplexe tetraedrische AlSb49-- und lineare Sb37--Anionen vor. Die Verbindung läßt sich dementsprechend als Valenzverbindung deuten.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845191219
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    Bildung siliciumorganischer Verbindungen. 105. Reaktionen des (Cl3Si)2C=PMe2Cl mit SilylphosphanenProfessor Kurt Issleib zum 65. Geburtstage am 19. November 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 518 (1984), S. 14-20 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Formation of Organosilicon Compounds. 105. Reactions of (Cl3Si)2C=PMe2Cl with SilylphosphanesThe reaction of (Cl3Si)2C=PMe2Cl 1 with MeP(SiMe3)2 proceeds at 130°C (15 hrs.), by cleavage of all Si—P bonds to compounds 2, 3, 4, 5. The course of this reaction incorporates a number of stages of which the compounds (Cl3Si)2C—PMe2—P(Me)SiMe3, (Cl3Si)2C=PMe2—PMe—P(Me)SiMe3 and ClP(Me)SiMe3 are important and are yet to be isolated.The reaction of (Cl3Si)2C=PMe2Cl with LiP(SiMe2)2 produces compound 2 as well as p2(SiMe3)4 and P(SiMe3)3. The formation of 2 can be explained by the initial formation of the intermediate (Cl3Si)2C=PMe2—P(SiMe2)2 with reacts with 1 to produce 2 and (ClP(SiMe)3)2. The formation of P2(SiMe3)4 is also explained by the reaction of ClP(SiMe3)2 with LiP(SiMe3)4.The reaction of (Cl3Si)2C=PMe2C(H)PMe2 at 130°C/15-20 hrs. is related to the formation of (Me3Si)2C(H)Pme2 from corresponding Si-methylated phosphorylides with the exception that, at 0°C, this reaction goes to completion within a few minutes.
    Notes: Die Umsetzung von (Cl3Si)2C=PMe2Cl 1 mit MeP(SiMe3)2 führt bei 130°C (15 h) unter Spaltung aller Si—P-Bindungen zu den Verbindungen 2, 3, 4, 5 Bei der über mehrere Stufen verlaufenden Reaktion sind die Verbindungen (Cl3Si)2C=PMe2-P(Me)SiMe3, (Cl3Si)2C=PMe2-PMe—P(Me)SiMe3 und ClP(Me)SiMe3 wichtige Zwischenglieder, die jedoch nicht zu isolieren waren.Die Umsetzung von (Cl3Si)2C=PMe2Cl mit LiP(SiMe3)2 führt ebenfalls zu Verbindung 2 neben P2(SiMe3)4 und P(SiMe3)3. Die Bildung von 2 ist über die Zwischenstufe (Cl3Si)2C=PMe2-P(SiMe3)2 zu erklären, die mit 1 zu Verbindung 2 und ClP(SiMe3)2 reagiert, die sich mit LiP(SiMe3)2 zu P2(SiMe3)4 umsetzt.Die Reaktion von (Cl3Si)2C=PMe2Cl 1 mit Me3SiPH2 unter Bildung von (Cl3Si)2C(H)PMe2 bei 130°C/15 - 20 h entspricht der Bildung von (Me3Si)2C(H)PMe2 aus entsprechenden Si-methylierten Phosphoryliden, die aber schon bei 0°C innerhalb weniger Minuten abläuft.
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    Neue Borate der Alkalimetalle: KNa2[BO3]Professor Kurt Issleib zum 65. Geburtstage am 19. November 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 518 (1984), S. 55-64 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: New Borates of Alkali Metals: KNa2[BO3]We prepared hittherto unknown KNa2[BO3] in the shape of orthorhombic, colourlesstransparent and columnar single crystals [a = 603.9(2) pm, b = 560.2(3) pm, c = 556.8(2) pm, Z = 2, dx = 2.54 g/cm3, dpyk = 2.50 g/cm3]. The crystal structure was solved by four-cycle-diffractometer [PW 1100, MoKα, R = 3.73%, Rw = 2.88%, 386 I0(hkl)]. KNa2[BO3] is very sensitiv against atmospheric moisture, and hydrolysis takes place.Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, and the Madelung-Part of Lattice Energy, MAPLE, are calculated and discussed.
    Notes: Neu dargestellt wurde KNa2[BO3] in Form orthorhombischer, farblosdurchsichtiger, säulenförmiger Einkristalle [a = 603,9(2) pm, b = 560,2(3) pm, c = 556,8(2) pm, Z = 2, dx = 2,54 g/cm3, dpyk = 2,50 g/cm3]. Die Kristallstruktur wurde über Vierkreisdiffraktometerdaten [PW 1100, MoK\documentclass{article}\pagestyle{empty}\begin{document}$ \bar \alpha $\end{document}, R = 3,73%, Rw = 2,88% für 386 I0(hkl)] aufgeklärt. KNa2[BO3] ist gegen Luftfeuchtigkeit sehr empfindlich; es tritt Hydrolyse ein.Effektive Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, sowie der Madelunganteil der Gitterenergie, MAPLE, werden berechnet und diskutiert.
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    Zur Kristallstruktur von Li8PbO6 [1] (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 81-86 
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    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Structure of Li8PbO6For the first time single crystals of Li8PbO6 have been prepared by heating of mixtures of Na2PbO3 and Li2O [Ag-cylinders, 650°C, 150 d]. The structure [382 I0(hkl), four circle diffractometer PW 1100, ω/2Θ-scan, MoKα, R = 3.07%, Rw = 3.00%, space group R3; a = 555.09(4), c = 1564.13(17) pm, Dx = 4.28 g · cm-3, Dpyk = 4.24 g · cm-3, Z = 3] is characterized by the motive of a hexagonal-closed O2- packing. Half of the octahedral sites are occupied by Pb4+ and Li+ and half of the tetrahedral sites only by Li+. The Madelung Part of Lattice Energy, MAPLE, and the Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated.
    Notes: Erstmals wurden farblose Einkristalle von Li8PbO6 durch Tempern inniger Gemenge von Na2PbO3 und Li2O [Ag-Bömbchen, 650°C, 150 d] dargestellt und die Struktur bestimmt [382 I0(hkl), Vierkreisdiffraktometer PW 1100, ω/2Θ-scan, MoKα, R = 3,07%, Rw = 3,00% in R3; a = 555,09(4), c = 1564,13(17) pm, drö = 4,28 g · cm-3, dpyk = 4,24 g · cm-3, Z = 3]. Die Struktur ist charakterisiert durch das Motiv einer hexagonal dichtesten O2--Packung, bei der die Hälfte aller Oktaederlücken mit Pb4+ und Li+ und die Hälfte aller Tetraederlücken nur mit Li+ besetzt sind. Der Madelunganteil der Gitterenergie, MAPLE, sowie die Effektiven Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, werden berechnet.
    Additional Material: 7 Tab.
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    URL: http://dx.doi.org/10.1002/zaac.19845150809
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  • 89
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    Das erste Oxocuprat(I) mit hantelförmigem Anion: KNa2[CuO2] (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 87-94 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The First Oxocuprate(I) with Dumb-bell-like Anion: KNa2[CuO2]For the first time KNa2[CuO2] was prepared in transparent, dark yellow single crystals from KO0.48 NaO0.50 and Cu2O (sealed cu-cylinders, 680°C, 30 d). The crystal structure, I 4mm, with a = 432.7(3), c = 1089.1(5) pm, Z = 2, Dx = 2.94 g/cm3, Dpyk = 2.89 g/cm3 was solved (four-circle-diffractometer PW 1100, 347 I0 (hkl), MoKα; R = 0.073, Rx = 0.069). The structure of KNa2[CuO2] may be regarded as a “stuffed derivative” of XeF2 with dumb-bell-like [CuO2] units. The C.N. of the two crystallographically independent O2- are 6 and 9, respectively. The Madelung Part of Lattice Energy, MAPLE, Effective Coordination Numbers, ECoN, these via Mean Fictive Ionic Radii, MEFIR, are calculated.
    Notes: Erstmals dargestellt wurde KNa2[CuO2] in Form transparenter, dunkelgelber Einkristalle aus KO0,48 NaO0,50 und Cu2O (geschlossene Cu-Bombe, 680°C, 30 d) und die Kristallstruktur, I 4mm, mit a = 432,7(3), c = 1089,1(5) pm, Z = 2, drö = 2,94 g/cm3, dpyk = 2,89 g/cm3 aufgeklärt (Vierkreisdiffraktometerdaten PW 1100, 347 I0 (hkl), MoKα; R = 0,073, Rw = 0,069). Es liegt eine „aufgefüllte“ XeF2-Struktur mit hantelförmigen [CuO2]-Einheiten vor. Von den zwei kristallographisch verschiedenen O2- hat eines C.N. 6 und das andere C.N. 9. Der Madelunganteil der Gitterenergie, MAPLE, Effektive Koordinationszahlen, ECoN, diese über Mittlere Fiktive Ionenradien, MEFIR, werden berechnet.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845150810
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  • 90
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    Synproportionierung am metallischen Substrat: CsCu2Cl3 und CsCu2Br3 (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 127-132 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: CsCu2Cl3 and CsCu2Br3 by Synproportionation at the Metallic SubstrateCsCu2Cl3 and CsCu2Br3 are obtained as single crystals via a dry route by synproportionation of mixtures of CsX/2 CuX (X = Cl, Br) and CsCuCl3, respectively, with the copper of the surface of a closed copper cylinder as the metallic substrate. Lattice constants of CsCu2Cl3 (CsCu2Br3) are: a = 950.75(9) (987.3(1)), b = 1189.8(2) (1235.5(2)), c = 559.92(6) (581.80(9)) pm, orthorhombic, Cmcm, Z = 4. Details of the Cs—X polyhedra (X = Cl, Br, I) and the double chains of tetrahedra [Cu2X3]- in CsCu2Cl3, CsCu2Br3, and CsCu2I3 are compared.
    Notes: CsCu2Cl3 und CsCu2Br3 wurden auf trockenem Wege durch Synproportionierung von Gemengen CsX/2 CuX (X = Cl, Br) bzw. CsCuCl3 mit der Gefäßwand eines Cu-Bömbchens als metallischem Substrat in Form von Einkristallen erhalten. Es ist für CsCu2Cl3 (CsCu2Br3): a = 950,75(9) (987,3(1)), b = 1189,8(2) (1235,5(2)), c = 559,92(6) (581,80(9)) pm, orthorhombisch, Cmcm, Z = 4. Einzelheiten der Polyeder Cs—X (X = Cl, Br, I) bzw. der Tetraeder-Doppelketten [Cu2X3]-werden für CsCu2Cl3, CsCu2Br3 und CsCu2I3 miteinander verglichen.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845150814
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  • 91
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    Über Oxostannate(II). V. Na4[SnO3] - das erste Oxostannat(II) mit „Inselstruktur“ (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 515 (1984), S. 114-126 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On Oxostannates(II). V. Na4[SnO3] - The First Oxostannate (II) with Island StructureThe new oxid Na4SnO3 (yellow, transparant single crystals) has been prepared by heating of mixtures of: 1. NaO0.45 and SnO (Na:Sn2+ = 4.1:1; Ag-cylinders; 600-730°C, 7-66 d); 2. NaO0.45′ SnO2 and Sn±0 (Na:Sn4+:Sn±0 = 8.2:1:1; Ag-cylinders; 650-680°C, 2-66 d); 3. NaO0.45′ Na2SnO3 and Sn±0 (Na:Na2SnO3:Sn±0 = 6.1:1:1; Ag-cylinders; 650-670°C, 5 d). Na4SnO3:804 I0(hkl); four circle diffractometer PW 1100; ω-scan; MoKα; R = 5.14%; Rw = 4.64%; monoclin, Cc—Cs4; a = 582.77(11), b = 1667.44(24), c = 589.42(10) pm, β = 110.187(13)°; dx = 3.20 g/cm3; dpyk = 3.19 g/cm3; Z = 4; parameter look for text. It is a NaCl-variant with systemathical blanks of the anion part and “isolated” groups of [SnO3]. \documentclass{article}\pagestyle{empty}\begin{document}$ {\rm N}\mathop {\rm a}\limits^{\rm 1} $\end{document} has the uncommon coordination number 2. The Effective Coordination Numbers, ECoN, the Mean Fictive Ionic Radii, MEFIR, and the Madelung Part of Lattice Energy, MAPLE, are calculated. The structure is described using „Erweiterte Schlegeldiagramme“.
    Notes: Das neue Oxid Na4SnO3 (hellgelbe, klare Einkristalle) aus: 1. NaO0,45 und SnO (Na:Sn2+ = 4,1:1; Ag-Bömbchen; 600 bis 730°C, 7 bis 66 d); 2. NaO0,45, SnO2 und Sn±0(Na:Sn4+: Sn±0 = 8,2:1:1; Ag-Bömbchen; 650 bis 680°C, 2 bis 66 d); 3. NaO0,45, Na2SnO3 und Sn±0 (Na: Na2SnO3: Sn±0 = 6,1:1:1; Ag-Bömbchen; 650 bis 670°C, 5 d) kristallisiert monoklin, Cc—Cs4; a = 582,77(11), b = 1667,44(24), c = 589,42(10) pm, β = 110,187(13)°; dx = 3,20 g/cm3; dpyk = 3,19 g/cm3; Z = 4; 804 I0(hkl); Vierkreisdiffraktometer PW 1100; ω-scan; MoKα; R = 5,14%; Rw = 4,64%; Parameter siehe Text. Es liegt eine NaCl-Variante mit systematischen Lücken im Anionenteil und „isolierte“ Baugruppen [SnO3] vor. \documentclass{article}\pagestyle{empty}\begin{document}$ {\rm N}\mathop {\rm a}\limits^{\rm 1} $\end{document} besitzt die ungewöhnliche Koordinationszahl 2. Die Effektiven Koodinationszahlen, ECoN, die Mittleren Fiktiven Ionenradien, MEFIR, und der Madelunganteil der Gitterenergie, MAPLE, werden berechnet, die Struktur über „Erweiterte Schlegeldiagramme“ beschrieben.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845150813
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  • 92
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    Masthead (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 517 (1984) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845171001
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  • 93
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    Zur Konstitution von Ba2WO3F4 und Ba2MoO3F4Professor Robert Juza zum 80. Geburtstage am 8. Dezember 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 518 (1984), S. 149-160 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: On the Structure of Ba2Wo3F4 and Ba2MoO3F4Ba2[WO2/2O2F2]F2 has been prepared for the first time as colourless single crystals (from powder, Au-tube, 680°C, 90 d). It crystallizes in the monoclinic (C c) crystal system with a = 1151.1, b = 938.2, c = 718.8 pm, ß = 126.17°, Z = 4. dx = 6.17, dpyk = 6.13 g · cm-3. (Fourcirclediffractometer PW 1100, Fa. Philips, MoKα-, ω-2Θ-scan, 1832 I0(hkl) R = 8.3, Rw = 7.4%). Parameters see in the text. The isotypic Ba2MoO3F4 has been prepared as powder (a = 1147.5, b = 937.0, c = 725.1 pm, ß = 126.42°). The structure shows chains of (WO2/2O2F2) groups along [001]. To establish O2- and F- on the positions IR and Raman Spectra are employed. The Madelung Part of Lattice Energy, MAPLE, is calculated and discussed.
    Notes: Erstmals wurden farblose Einkristalle von Ba2[WO2/2O2F2]F2 (aus Pulver, Au-Rohr, 680°C, 90 d) dargestellt, die monoklin, C c, mit a = 11,511, b = 9,382, c = 7,188 Å, ß = 126,17°, Z = 4, dx = 6,17 und dpyk = 6,13 g · cm-3 kristallisieren. (Vierkreisdiffraktometer PW 1100, Fa. Philips, MoKα-, ω-2Theta;-scan, 1832 I0(hkl) R = 8,3% und Rw = 7,4%). Parameter s. Text. Isotyp ist Ba2MoO3F4 mit a = 11,475, b = 9,370, c = 7,251 Å, ß = 126,42°, als Pulver erhalten. Charakteristisches Strukturelement ist die Kette (WO2/2O2F2) längs [001]. Der Madelunganteil der Gitterenergie, MAPLE sowie IR- und Raman-Spektren werden zur Festlegung der Verteilung von O2- und F- auf den Anionenpositionen herangezogen und diskutiert.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845181115
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  • 94
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    Magnetische Eigenschaften der Verbindungsreihe EuBX mit B = Element der ersten Neben- und X = Element der fünften HauptgruppeProfessor Robert Juza zum 80. Geburtstage am 8. Dezember 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 518 (1984), S. 161-167 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Magnetic Properties of the Compound Series EuBX with B = Element of the First Subgroup and X = Element of the Fifth Main GroupThe magnetic properties of the compounds EuBX (B = Cu, Ag, Au; X = P, As, Sb, Bi) in the temperature range between 3.8 and 300 K are reported. These compounds crystallize in a modified Ni2In-type structure. The compounds EuCuP, EuAgP, EuAuP, and EuAuAs show at low temperatures ferromagnetic behaviour, EuCuAs and EuAgAs are metamagnetic. According to our measurements this seems to be the same with EuCuSb, EuAgSb, EuAuSb, and EuAuBi whereas EuCuBi and EuAgBi show antiferromagnetic interaction.
    Notes: Es wird über die magnetischen Eigenschaften der Verbindungsreihe EuBX (B = Cu, Ag, Au; X = P, As, Sb, Bi) im Temperaturbereich zwischen 3,8 und 300 K berichtet. Die Verbindungen kristallisieren in einer Variante des Ni2In-Typs. EuCuP, EuAgP, EuAuP und EuAuAs verhalten sich bei tiefen Temperaturen ferromagnetisch, EuCuAs und EuAgAs sind metamagnetisch, was aufgrund der Ergebnisse auch für EuCuSb, EuAgSb, EuAuSb, EuAuBi zutreffen dürfte. EuCuBi bzw. EuAgBi zeigen antiferromagnetische Eigenschaften.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845181116
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  • 95
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    Metallextraktion und Komplexbildung mit α-Aminoximen (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 518 (1984), S. 187-196 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Metal Extraction and Complex Formation by α-Amino OximesCyclic secondary α-amino oximes (RNHR′NOH) in toluene as a diluent extract copper(II) from weakly acid solutions. The distribution ratio DCu amounts to 80. The extraction process is connected with the elimination of two protons (formation of [Cu(RNHR′NOH)2—H]NO3). Apart from this 1,2-complex 1,1-complexes Cu(RNHR′NOH)X2 (X = Cl, Br) are obtained. A blue and a black isomer of Cu(RNHDodNOH)Cl2 are described. According to x-ray structure analysis, the latter isomer is square-planar with the amino oxime in the E-configuration. Basing on the i.r. spectrum, for the blue isomer a monodentate coordination of the Z-isomer of RNHDodNOH is discussed.In the case of nickel(II) only the 1,2-chelates [Ni(RNHR′NOH)2—H]Y (Y = NO3, ClO4, I), in the case of palladium(II) only the 1,1-chelates Pd(RNHR′NOH)Cl2 were isolated.
    Notes: Cyclische sekundäre α-Aminoxime (RNHR′NOH) im Verdünnungsmittel Toluen extrahieren Kupfer(II) aus schwach saurer Lösung. Das Verteilungsverhältnis DCu kann bis auf 80 ansteigen. Der Extraktionsprozeß ist mit der Abspaltung von zwei Protonen verbunden (bevorzugte Bildung von [Cu(RNHR′NOH)2—H]NO3 (A)).Neben den 1,2-Komplexen A bildet Kupfer(II) noch die 1,1-Komplexe Cu(RNHR′NOH)X2 (X = Cl, Br). Von Cu(RNHDodNOH)Cl2 existieren ein blaues und ein schwarzes Isomer. Das letztere ist nach den Kristallstrukturanalyse planar-quadratisch und enthält das α-Aminoxim in der E-Konfiguration. Das IR-Spektrum der blauen Form läßt den Schluß auf eine einzählige Koordination von RNHDodNOH als Z-Isomer zu.Bei Nickel(II) und Palladium(II) konnte mit [Ni(RNHR′NOH)2—H] (Y = NO3, ClO4 I) bzw. Pd(RNHR′NOH)Cl2 jeweils nur ein Komplextyp isoliert werden.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845181119
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  • 96
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    Das Löslichkeitsdiagramm des Systems ZnSeO4—H2SeO4—H2O und einige Eigenschaften der erhaltenen Verbindungen (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 517 (1984), S. 223-230 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Isotherms of Solubility in the System ZnSeO4—H2SeO4—H2O and Some Properties of the Compounds ObtainedThe isotherms of solubility in the system ZnSeO4—H2SeO4—H2O were studied at 25 and 100°C. Some properties of the compounds obtained were investigated.
    Notes: Untersucht wird die Löslichkeitsisotherme des Systems ZnSeO4—H2SeO4—H2O bei 25 und 100°C. Einige Eigenschaften der erhaltenen Verbindungen werden erforscht.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845171023
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  • 97
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    Masthead (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 518 (1984) 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845181101
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  • 98
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    A Potentiometric Study of the AgI Complexes of Some Sulphur Containing Amino Acids (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 517 (1984), S. 235-240 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Potentiometrische Untersuchungen über Silber (I)-Komplexe einiger schwefelhaltiger AminosäurenDie Komplexbildung von Silber(I) mit einer Reihe von schwefelhaltigen Aminosäuren wurde durch simultane pH- und pM-Messungen bei 25°C in 0,5 M(K)NO3 Lösung untersucht. In saurem Milieu findet die Koordination mit der Thioether-Gruppe statt; die Carboxylat-Gruppe ist nicht beteiligt. In alkalischem Milieu sind die Liganden über S und N dem Ag1-Ion zugeordnet, und zwar sowohl in den tetraedrischen AgL- und AgL2--Chelat-Komplexen als auch in dem linearen dinuclearen Ag2L2-Komplex.
    Notes: The complex formation of silver(I) with some sulphur-containing amino acids was studied in aqueous solution by simultaneous pH and pM measurements at 25°C and at an ionic strength of 0.5M (K)NO3. In acid medium complex formation occurs only through the thioether group and the carboxylate group is not involved. In alkaline medium both the thioether and the amino group are bound in either the tetrahedral AgL and AgL2- chelates or the linear dinuclear Ag2L2 species.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845171025
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  • 99
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    Acyl- und Alkylidenphosphane. XXIV. (N,N-Dimethylthiocarbamoyl)trimethylsilylphosphane und 1,2-Di(tert-butyl)-3-dimethylamino-1-thio-4-trimethylsilylsulfano-1λ5,2λ3-diphosphet-3-enProfessor Kurt Issleib zum 65. Geburtstage am 19. November 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 518 (1984), S. 21-35 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Acyl- and Alkylidenephosphines. XXIV. (N,N-Dimethylthiocarbamoyl)trimethylsilyl-phosphines and 1.2-Di(tert-butyl)-3-dimethylamino-1-thio-4-trimethylsilylsulfano-1λ5, 2λ3-diphosphet-3-eneIn contrast to bis(trimethylsilyl)phosphines R—P[—Si(CH3)3]2 1 {R = H3C a; (H3C)3C b; H5H6 c; H11C9 d; (H3C)3Si e}, the more nucleophilic lithium trimethylsilylphosphides 4 react with N,N-dimethylthiocarbamoyl chloride already at -78°C to give (N,N-dimethylthiocarbamoyl)trimethylsilylphosphines 2. Working up the reaction, a dismutation of the mesityl derivative 2d is observed, whereas the tert-butyl compound 2b dissolved in toluene, eliminates dimethyl(trimethylsilyl)amine to form 1,2-di(tert-butyl)-3-dimethylamino-1-thio-4-trimethylsilyl-sulfano- 1λ5, 2λ3-diphosphet-3-ene 6b, nearly quantitatively within several days at +20°C.
    Notes: Im Gegensatz zu den Bis(trimethylsilyl)phosphanen R—P[—Si(CH3)3]2 1 {R = H3C a; (H3C)3C b; H5C6 c; H11C9 d; (H3C)3Si e} reagieren die nukleophileren Lithium-trimethylsilylphosphide 4 mit N,N-Dimethylthiocarbamoylchlorid bereits bei -78°C zu den (N,N-Dimethylthiocarbamoyl)trimethylsilylphosphanen 2. Während das Mesityl-Derivat 2d beim Aufarbeiten dismutiert, bildet sich aus der in Toluol gelösten tert-Butyl-Verbindung 2b bei + 20°C im Laufe von Tagen unter Abspaltung von Dimethyl(trimethylsilyl)amin 1,2-Di(tert-butyl)-3-dimethyl-amino-1-thio-4-trimethylsilylsulfano-1λ5,2λ3-diphosphet-3-en 6 b.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/zaac.19845181104
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  • 100
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    Perfluormethyl-Element-Liganden. XXVIII. Koordinatives Verhalten von Organoelement-Element-Liganden R2EE′R und R2EER′2(R,R′ = CH3, CF3; E = P, As; E′ = S, Se, Te)Professor Kurt Issleib zum 65. Geburtstage am 19. November 1984 gewidmet (1984)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 518 (1984), S. 36-54 
    Details
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Perfluoromethyl Element Ligands. XXVIII. Coordinating Properties of Organoelement Element Ligands R2EE′R and R2EER′2(R, R′ = CH3, CF3; E = P, As; E′ = S, Se, Te)The coordinating properties of organoelement-element compounds of the type R2EE′R and R2EER′2 (R,R′ = CH3, CF3; E = P, As; E′ = S, Se, Te) in VIB metal carbonyls are studied and comprehensively discussed. Results of i.r. and n.m.r. (1H, 19F, 31P, 13C) spectroscopic investigations of fifty M(CO)5L derivatives (M = Cr, Mo, W) support the description of the M—E bond as a combination of σ-donor and π-acceptor effects. Steric influences on the spectroscopic data are not significant in this series of compounds. The donor/acceptor ratio decreases in the order EMe3 〉 Me2EE(CF3)2, Me2EE′CF3 〉 (CF3)2EE′Me 〉 E(CF3)3.
    Notes: Die Koordinationsfähigkeit von Organoelement-Element-Verbindungen des Types R2EE′R und R2EER′2 (R, R′ = CH3, CF3; E = P, As; E′ = S, Se, Te) in Carbonylen der VI B-Metalle wird zusammenfassend diskutiert. Die Ergebnisse IR- und NMR (1H, 19F, 31P, 13C)-spektroskopischer Untersuchungen von fünfzig M(CO)5L-Komplexen (M = Cr, Mo, W) stützen das σ-Donor/π-Akzeptor-Bindungsmodell für die M—E-Verknüpfung. Sterische Einflüsse spielen in dieser Verbindungsreihe nur eine untergeordnete Rolle. Das Verhältnis aus σ-Donor- und π-Akzeptorstärke nimmt in der Reihe EMe3 〉 Me2EE(CF3)2, Me2EE′CF3 〉 (CF3)2EE′Me 〉 E(CF3)3 ab.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19845181105
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