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PubMed2002

Unsymmetrical tren-based ligands: synthesis and reactivity of rhenium complexes.

Reaction of bis(2-aminoethyl)(3-aminopropyl)amine with C(6)F(6) and K(2)CO(3) in DMSO yields unsymmetrical [(C(6)F(5))HNCH(2)CH(2)](2)NCH(2)CH(2)CH(2)NH(C(6)F(5)) ([N(3)N]H(3)). The tetraamine acts as a tridentate ligand in complexes of the type H[N(3)N]Re(O)X (X = Cl 1, Br 2) prepared by reacting Re(O)X(3)(PPh(3))(2) with [N(3)N]H(3) and an excess of NEt(3) in THF. Addition of 1 equiv of TaCH(CMe(2)Ph)Br(3)(THF)(2) to 1 gives the dimeric compound H[N(3)N]ClReOReBrCl[N(3)N]H (3) in quantitative yield that contains a Re(V)[double bond]O[bond]Re(IV) core with uncoordinated aminopropyl groups in each ligand. Addition of 2 equiv of TaCH(CMe(2)Ph)Cl(3)(THF)(2) to 1 leads to the chloro complex [N(3)N]ReCl (4) with all three amido groups coordinated to the metal, whereas by addition of 2 equiv of TaCH(CMe(2)Ph)Br(3)(THF)(2) to 2 the dibromo species H[N(3)N]ReBr(2) (5) with one uncoordinated amino group is isolated. Reduction of 4 under an atmosphere of dinitrogen with sodium amalgam gives the dinitrogen complex [N(3)N]Re(N(2)) (6). Single-crystal X-ray structure determinations have been carried out on complexes 1, 3, 5, and 6.

Journal Article↗
PubMed2005

New oxorhenium(V) compound for catalyzed oxygen atom transfer from picoline N-oxide to triarylphosphines.

The synthesis and characterization of a new oxorhenium(V) compound is reported; it is [MeReO(edt)(bpym)], 8, where edt = 1,2-ethanedithiolate and bpym = 2,2'-bipyrimidine. Compound 8 was characterized by NMR spectroscopy and single-crystal X-ray analysis. It exists as a six-coordinate Re(V) compound comparable to the previously known [MeReO(edt)(bpy)] and [MeReO(mtp)(bpy)]. Compound 8 catalyzes the oxygen-atom-transfer reaction PicO + PZ3 --> Pic + Z3PO, whereas the other two do not. The kinetics of this reaction with catalyst 8 follows the rate law -d[PicO]/dt = k[8][PicO]/(1 + c[PZ3]). With different phosphines, the rate law has the same k value, 4.17 L mol(-1) s(-1), but different c values. For tritolylphosphine, c = 67.5 L mol(-1) in benzene at 25 degrees C. A mechanism has been proposed to account for these findings. The data establish that an open coordination site on rhenium is necessary for oxygen-atom-transfer reactions.

Journal Article↗
PubMed2000

Diagnosis of human hydatidosis. Predictive value of a rural ultrasonographic survey in an apparently healthy population.

The usefulness of ultrasonography (US) in the early diagnosis of hydatidosis, applied in large-scale surveys to populations lacking clinical symptoms of the disease, has been amply documented. However, the rate of false positive and negative results is poorly described. Due to this, the present paper is aimed to evaluate the sensitivity, specificity and predictive value of a conventional rural ultrasonographic survey in comparison with higher imaging complexity. Accordingly, during 1997 and 1998 a total of 1054 children from 7 to 14 years of age were evaluated by means of US, in the town of Ingeniero Jacobacci, Province of Rio Negro, Argentina, employing a portable device for population studies. All detected cases were referred to a high complexity center specialized in imaging diagnosis for their re-evaluation with US, CT scanning and X-rays. A control group comprising 3 children negative by US for each positive case in the mass screening survey was selected and reexamined by US and X-rays and CT scanning in doubtful situations. Twenty-seven asymptomatic carriers were referred with images compatible with hydatid cysts, while 66 were classified as disease free. At reexamination, 24 of those diagnosed as carriers and the totality of those classified as healthy were confirmed. On the basis of our results, a sensitivity of 100%, a specificity of 95.6% and a global test value of 96.7% were estimated.

Adolescent↗
PubMed2003

Cardiac herniation following intrapericardial pneumonectomy with partial pericardiectomy for advanced lung cancer.

We present in this paper a case of cardiac herniation following right intrapericardial pneumonectomy after induction chemotherapy. A 52-year-old man with advanced squamous cell carcinoma of the lung was admitted to our hospital suffering from a dry cough and chest pain. An intrapericardial pneumonectomy with partial pericardiectomy (4 x 4 cm) was performed. The pericardial defect was left open. Just prior to removal of the tracheal tube, cardiac herniation occurred with hypotension, arrhythmia and cardiac arrest. A chest X-ray revealed cardiac herniation into the right hemithorax. Re-thoracotomy was performed and the heart was returned to its normal position and the pericardial defect was immediately repaired with an expanded polytetrafluoroethylene (EPTFE) patch. The patient's postoperative course was uneventful. Unless prompt diagnosis and surgical treatment can be accomplished, cardiac herniation can be a fatal complication. We recommend that when pneumonectomy is performed, pericardial defects should be closed with a prosthetic patch, regardless of the defect's size.

Carcinoma, Squamous Cell↗
PubMed2006

[Right spontaneous pneumothorax which accompanied absence of right pulmonary artery].

A case had a checkup for dyspnea with a man of 70-year-old, and it was diagnosed as the recurrent right spontaneous pneumothorax. Bulla was found in the right lung with a chest computed tomography (CT), and absence of right pulmonary artery was suspected. Absence of right pulmonary artery was diagnosed by pulmonary arteriography. Re-examination of the patient's chest X-ray from the previous 11 years revealed a chronological decrease of right lung volume and an increase of the cardiothoracic ratio. We performed right bullectomy by thoracoscopic assistance. The postoperative course was uneventful.

Aged↗
PubMed1980

Clinical evaluation of a new device for the treatment of tension pneumothorax.

The two accepted major methods for decompression of a pneumothorax are needle aspiration in the second intercostal space and large bore chest tube insertion in the midaxillary line, sixth, seventh or eight intercostal space. Both of these devices have drawbacks in the emergency management of a tension pneumothorax. Relating to size, case of insertion, volume of air aspirated and cumbersomeness of associated equipment. This evaluation of its effectiveness is both in the prehospital phase and in the Emergency Department by studying 40 patients, 55% of which were prehospital. Sixty per cent were placed by EMT-Paramedic personnel. All of those patients that survived their multiple trauma long enough to allow x-rays to be made, had partial to total re-expansion of the pneumothorax. Of those patients undergoing autopsy or surgical exploration no indication could be identified of pulmonary injury secondary to the insertion of the device. The only complications were: intercostal artery laceration and a minor laceration of the dome of the diaphram. In summary this study of 40 patients demonstrates the effectiveness of the use of a device for the management of tension pneumothorax, both prehospital and in-hospital by physician and EMT-Paramedic personnel.

Catheterization↗
PubMed1980

Space-occupying lesions in the tail of the pancreas.

Most patients referred for an ERCP arrived with a large package of X-rays, the result of diverse routine investigations. On re-examination of these radiographs it was usually possible to make a diagnosis before performing the ERCP. In this article we analyze the value of several investigating methods used in 36 patients with a space-occupying lesion in the tail of the pancreas. Attention is paid to radiological changes suggestive of pathology in this area.

Abscess↗
PubMed1996

Synthesis and Characterization of Rhenium(V) Oxo Complexes with a New Thiol-Amide-Thiourea Ligand System. X-ray Crystal Structure of [1-Phenyl-3-[2-((2-thioacetyl)amino)ethyl]thioureato]oxorhenium(V).

General methods for preparing Re(V)O complexes with a novel series of thiol-amide-thiourea (TATU) ligands, a new class of N(2)S(2) chelates, were developed. The TATU ligands, the first multidentate systems designed with a bidentate thiourea moiety, have been used to prepare the first high-valent transition metal complexes with bidentate thiourea coordination. Direct reaction of N-(2-aminoethyl)-2-((triphenylmethyl)thio)acetamide (1) with phenyl, 4-methoxyphenyl, 4-chlorophenyl, and methyl isothiocyanate afforded ready access to the corresponding S-protected TATU ligands in one step. A two-step preparation of the N,N-dimethylthiourea TATU ligand derived from 1 was also developed. Deprotection of thiols in trifluoroacetic acid with triethylsilane followed by a ligand exchange reaction with Re(V)O precursors yielded neutral ReO(TATU) complexes. The structure of [1-phenyl-3-[2-((2-thioacetyl)amino)ethyl]thioureato]oxorhenium(V) (6a) was determined by X-ray diffraction methods. Crystal data for 6a: C(11)H(12)N(3)O(2)ReS(2), fw 468.6, orthorhombic, Pca2(1); a = 22.605(5) Å, b = 13.029(3) Å, c= 9.698(2) Å; V = 2856.3(11) Å(3); Z = 8. The coordination environment of 6a was pseudo-square-pyramidal with a deprotonated thiol S, deprotonated amide N, deprotonated thiourea N, and thiocarbonyl S coordinated in the basal plane and the oxo ligand in the apical position. The thiourea function forms a four-membered chelate ring in the multidentate TATU ligands. The two N-C and the S-C bond distances within the monodeprotonated thiourea moiety were typical of bonds with multiple-bond character. Solution (1)H NMR data for all five complexes were consistent with the solid-state structure of 6a. A broad singlet attributable to the uncoordinated NH group of thiourea was observed for the monosubstituted thiourea complexes but was not present for the N,N-dimethylthiourea derivative. Instead, two singlets of equal intensity were observed for the two methyl groups, indicating that there is restricted rotation around the C-N(CH(3))(2) bond and an extended pi system in the thiourea moiety. The four-membered ring might cause difficulty because the M-S distance would be relatively long in an undistorted ligand. This may be the reason such chelate ligands have not been previously investigated. However, the N-C-S angle narrows to approximately 105 degrees, permitting a Re-S bond with a typical bond length to be formed. We conclude that such a ring represents a versatile new building block to create multidentate ligands.

Journal Article↗
PubMed1997

Rhenium(V) and Technetium(V) Oxo Complexes of an N(2)N'S Peptidic Chelator: Evidence of Interconversion between the Syn and Anti Conformations.

Neutral Re(V) and Tc(V) oxo complexes of the peptide dimethylglycyl-L-seryl-L-cysteinylglycinamide (RP294) were prepared and characterized by HPLC, spectroscopic techniques, and X-ray crystallographic analysis. The peptide was prepared as a single peptide chain using solid phase methods and characterized by HPLC and various spectroscopic techniques. The water-soluble Re(V) oxo complex of dimethylglycyl-L-seryl-L-cysteinylglycinamide [ReO(RP294)] was prepared from the reaction of the peptide with either [ReO(2)(en)(2)]Cl or ReOCl(3)(PPh(3))(2) in the presence of base. The complex exists as two isomers, the serine CH(2)OH group being in the syn oranti conformation with respect to the Re-oxo bond. The ratio of the isomers at room temperature is 1:1.1. The isomers were separated by reverse-phase HPLC, but the isolation of each isomer was complicated by their rapid interconversion in aqueous solution at room temperature. The molecular structure of the syn isomer of the Re complex was determined by X-ray crystallography. Crystals of syn-[ReO(RP294)] (C(12)H(20)N(6)O(5)ReS) are orthorhombic, of space group P2(1)2(1)2(1), with a = 6.954(1) Å, b = 8.0472(1) Å, c = 32.9183(4) Å, and Z = 4. The structure was solved by direct methods and was refined by full-matrix least-squares procedures to R = 0.0327 (R(w) = 0.0838) for 10 447 reflections with I > 2sigma(I). The Re metal was coordinated in a distorted square pyramidal geometry with the oxo moiety in the apical position. The peptide coordinated to ReO(3+) via the N(amine) atom of dimethylglycine, the S(thiolate) atom of cysteine, and the two N(amide) atoms of serine and cysteine (an N(2)N'S donor atom set). The Re atom lies approximately 0.74 Å above the distorted plane formed by the N(2)N'S donor atom set. Variable-pH (1)H NMR spectral data showed the Re complex was stable from pH 5 to 8.5. The reaction of (99)TcO(4)(-) with SnCl(2), sodium gluconate, and RP294 produced the (99)Tc(V) oxo RP294 complex, [(99)TcO(RP294)]. Like the [ReO(RP294)] complex, [(99)TcO(RP294)] also exists in the syn and anti conformations in a ratio of approximately 1:1. The (99m)Tc complex of RP294 was prepared at the tracer level from the reaction of Na[(99m)TcO(4)] with excess SnCl(2), sodium gluconate, and RP294. The (99m)Tc and Re RP294 complexes behaved similarly under identical HPLC conditions.

Journal Article↗
PubMedDate not supplied

Balloon catheter re-expansion of atelectatic lung.

Selective re-inflation of the lung with lobar atelectasis was carried out in four patients who were receiving mechanical ventilation. The increased pressure and volume were delivered mainly to the atelectatic lung by momentary obstruction of mainstem bronchus of the uninvolved lung with a balloon-tipped catheter. Blood gases and chest x-rays following the procedure showed improvement in oxygenation with prompt re-expansion of the atelectatic lung. The described procedure is recommended in atelectasis involving major portions of the lung with severe hypoxemia not responding to aggressive conventional treatment.

Adult↗
PubMed2002

Solid-state reaction study of the trans-to-cis isomerization of (eta-C(5)H(4)Me)Re(CO)[P(OPh)(3)]Br(2): a new mechanism for the isomerization reaction.

Single-crystal X-ray structures have been determined at intermediate stages in the single-crystal to single-crystal trans-to-cis thermal isomerization of (eta(5)-C(5)H(4)Me)Re(CO)[P(OPh)(3)]Br(2) at 150 degrees C. Unit cell parameters and site occupancy factors linked to the induced disorder were monitored and found to follow first-order kinetics in the initial (fast component) stage of the reaction. A rate constant of 30 x 10(-6) s(-1) (0.11 h(-1)) was obtained to first-order approximation for the reaction. The irreversibility of the isomerization from single crystals of the cis form was also confirmed. Fourier and difference Fourier maps suggest a novel 2-fold rotation mechanism for the trans-to-cis isomerization reaction. This mechanism entails a unidirectional anticlockwise movement of the CO ligand and only one Br atom.

Journal Article↗
PubMed2000

[Clinical experience with rhenium-188 HEDP therapy for metastatic bone pain].

Rhenium-188 hydroxyethylidene diphosphonate (Re-188 HEDP) is a new radiopharmaceutical for treatment of metastatic bone pain. Re-188 is a generator-produced radionuclide emitting high energy beta and gamma rays and having a relative short physical half-life makes it of especially interesting for therapeutic purpose. Seven patients (pts) with multiple painful bone metastases were treated with Re-188 HEDP. Five pts with prostate cancer and 2 pts with breast cancer received a fixed activity of 3000 MBq of Re-188 HEDP intravenously in two steps. Complete blood counts were determined, blood chemistry examinations and urine-analysis were performed before and 1, 2, 3, 4, 6, 8, 12 weeks following the treatment. A visual analogue score, a verbal rating scale, the Spitzer index and the Karnofsky score were used to assess pain and performance status. Three hours after Re-188 HEDP administration at 1 m from the anterior mid-trunk of the pts gamma and at the patient body surface beta-radiation dose measurements were made, together with urine radioactivity measurements. Three pts become pain-free, 2 pts exhibited partial pain improvement and 1 patient gave no response to the Re-188 HEDP therapy. In 1 patient due to central nervous system metastasis the modification of the pain intensity could not be evaluated. Three pts displayed a flare reaction within 1 week after the treatment. Transient decreases in platelet and white blood cell counts were observed. There were no significant changes in the liver and renal functions. Radiation dose rate values of 6.3 +/- 1.0 microSv/h for gamma, and of 183 +/- 40 s-1 for beta-radiation were found. 25-32% of the administered dose was eliminated via the urinary tract in the first three hours. The preliminary data suggests that Re-188 HEDP is an effective radiopharmaceutical in treatment for metastatic bone pain. An administered activity of 3000 MBq can bring about a pain reduction without causing any clinically significant bone marrow toxicity.

Alkaline Phosphatase↗
PubMed2002

Insertion of unsaturated organic electrophiles into molybdenumbond-alkoxide and rheniumbond-alkoxide bonds of neutral, stable carbonyl complexes.

Alkoxo complexes [Re(OR)(CO)(3)(N-N)] (R=Me, Et, tBu; N-N=2,2'-bipyridine (bipy), 4,4'-dimethyl-2,2'bipyridine (bipy'), 1,10-phenanthroline (phen)) and [M(OMe)(eta(3)-allyl)(CO)(2)(phen)] (M=Mo, W) have been synthesized in good yields and using mild conditions by the reaction of sodium alkoxides with [Re(OTf)(CO)(3)(N-N)] and [MCl(eta(3)-allyl)(CO)(2)(phen)] precursors. These have been characterized by IR and NMR spectroscopy as well as by X-ray diffraction for [W(OMe)(eta(3)-allyl)(CO)(2)(phen)] (10). The reactions of the molybdenum and rhenium alkoxo complexes with isocyanates, R'NCO, yield [L(n)M[N(R')C(O)OR]] complexes; the carbamate ligand, which results from an R'NCO insertion into the Mbond;OR bond, is monodentate through the nitrogen atom. The solid-state structures of Mo and Re examples have been determined by X-ray diffraction. The geometry around the carbamate nitrogen of these compounds is planar, and the distances indicate delocalization of the nitrogen lone pair involving mainly the carbonyl groups. Experiments carried out with the Re complexes showed that aryl isocyanates are more reactive than their alkyl counterparts, and that bulky R' groups led to slow rates of insertion. Insertion reactions were also observed with isothiocyanates, although here it is the Sbond;C bond that inserts into the Mbond;OR bond, and the resulting ligand is bound to the metal by sulfur. Competition experiments with the Re compounds indicate that isocyanates are more reactive than isothiocyanates towards the Rebond;OR bonds. Tetracyanoethylene inserts into the Rebond;OMe bond of [Re(OMe)(CO)(3)(bipy')], forming a complex with a 2-methoxytetracyanoethyl ligand; the structure of which was determined by X-ray diffraction. The formation of the xanthato complex [Re(SC(S)OtBu)(CO)(3)(bipy)] (20) by reaction of [Re(OTf)(CO)(3)(bipy)] with CS(2) and NaOtBu, but not by the reaction of CS(2) and [Re(OtBu)(CO)(3)(bipy)] (5 a), suggests that the insertion reactions do not take place by ionization of the alkoxo complexes to give the free alkoxide ion.

Journal Article↗
PubMed2006

[Re-expansion pulmonary oedema in a patient after treatment of pneumothorax].

In a 32-year-old man with left-sided pneumothorax, dyspnoea and tachypnoea with a drop in blood pressure and severe hypoxaemia recurred during drainage. The chest X-ray revealed an alveolar infiltrate in the middle and lower segments of the left lung that was interpreted as re-expansion pulmonary oedema. The patient was respirated and given extra fluids. Extubation was possible after four days. Re-expansion pulmonary oedema is a rare, potentially lethal complication after treatment of a collapsed lung due to a hydro- or pneumothorax. The oedema usually occurs in the re-expanded lung and must be considered when there is a sudden respiratory or haemodynamic deterioration after drainage of X fluid or air. The diagnosis is made by clinical examination and chest X-ray. Predisposing factors are a large hydro- or pneumothorax, long-term collapse, young age and rapid re-expansion. This complication can be prevented by low negative suction pressures and by aspirating a maximum of 1000 to 1500 ml of pleural fluid. The pathophysiology of re-expansion pulmonary oedema is not completely understood and is probably multifactorial. The treatment is merely supportive: oxygen, intravenous fluid substitution and if necessary artificial ventilation. The use of diuretics should be avoided in patients with hypotension.

Adult↗
PubMed2000

Measurements of activation induced by environmental neutrons using ultra low-level gamma-ray spectrometry.

The flux of environmental neutrons is being studied by activation of metal discs of selected elements. Near the earth's surface the total neutron flux is in the order of 10(-2) cm(-2)s(-1), which gives induced activities of a few mBq in the discs. Initial results from this technique, involving activation at ground level for several materials (W, Au, Ta, In, Re, Sm, Dy and Mn) and ultra low-level gamma-ray spectrometry in an underground laboratory located at 500 m.w.e., are presented. Diffusion of environmental neutrons in water is also measured by activation of gold at different depths.

Actinium↗