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PubMed1996

Bis(ligand) Rhenium(V) and Technetium(V) Complexes of Two Naturally Occurring Binding Moieties (Oxazoline and Thiazoline).

Attempts to prepare tris(ligand) metal complexes of technetium in intermediate oxidation states with potentially bidentate oxazoline- and thiazoline-containing ligands were unsuccessful; when pertechnetate was reduced in the presence of excess ligand, TcO(2).xH(2)O was produced. Instead, by reaction with preformed M.O cores, a series of oxotechnetium(V) and oxorhenium(V) complexes of the formula MOXL(2) (M = Re, X = Br; M = Tc, X = Cl) and HL = 2-(2'-hydroxyphenyl)-2-oxazoline (Hoz), 2-(2'-hydroxy-3'-methylphenyl)-2-oxazoline (Hmoz), 2-(2'-hydroxyphenyl)-2-thiazoline (Hthoz), and 2-(2'-hydroxyphenyl)-2-benzoxazoline (Hhbo) have been prepared. These compounds have been characterized by a variety of techniques including single-crystal X-ray diffraction. Crystals of Hthoz (C(9)H(9)NOS) are monoclinic, with space group P2(1)/n, a = 7.5342(6) Å, b = 12.2187(6) Å, c = 9.3942(8) Å, beta = 94.233(7) degrees, and Z = 4; those of TcOCl(thoz)(2) (C(18)H(16)ClN(2)O(3)S(2)Tc) are monoclinic, with space group P2(1)/n, a = 16.506(1) Å, b = 7.664(1) Å, c = 16.3216(6) Å, beta = 111.154(4) degrees, and Z = 4; those of ReOBr(oz)(2) (C(18)H(16)BrN(2)O(5)Re) are orthorhombic, with space group Pbca, a = 12.864(2) Å, b = 25.369(2) Å, c = 11.025(2) Å, and Z = 8. The structures were solved by direct (Hthoz) or Patterson (metal complexes) methods and were refined by full-matrix least-squares procedures to R = 0.033, 0.032, and 0.028 for 1600, 3152, and 2651 reflections with I >/= 3sigma(I), respectively. In the two complexes, the geometry around the metals is distorted octahedral with the halide ligands in each bound cis, and one phenolate oxygen from one ligand in each bound trans to the metal-oxo linkage. In ReOBr(oz)(2), the two oxazoline nitrogens are coordinated trans to one another; in TcOCl(thoz)(2), the two thiazoline nitrogens are found cis to one another.

Journal Article↗
PubMed2001

[Intramedullary fixation of humerus shaft fractures. An analysis of complications of 2 implants with special reference to outcome after management with the unreamed humerus interlocking nail].

INTRODUCTION: Operative treatment of humeral shaft fractures has gained a new impetus with the development of intramedullary interlocking systems for the humerus. Because of the anatomical structure of the humeral marrow cavity, a regular jamming of nail into bone is not to be expected, so that the stability of these systems needs to be achieved through an interlocking mechanism. Among the commercially available interlocking nailing systems the unreamed humeral nail (UHN) and the Seidel-nail (SHN) can be regarded as the standard implants. DESIGN: In a retrospective study comparing two groups of patients, each treated with one of the two systems, problems and advantages, as well as disadvantages were analyzed, and the complications inherent in the systems examined. PATIENTS: Between 1988-1992, 47 patients with humeral shaft fractures were treated with a Seidel interlocking nail: 25 acute and 18 pathological fractures as well as 4 non-unions (Group 1). Between 1997-1999, 34 patients with humeral shaft fractures were treated with the unreamed humeral nail (UHN). A total of thirty-five (n = 35) nailings (30 acute and 4 pathological fractures, as well as one re-osteosynthesis after emergence of a non-union) were carried out. Three primary palsies of the radial nerve ensued: two with loss of sensitivity, and one complete paralysis (Group 2). METHODS: Based on pre- and postoperative X-rays and follow-up examinations, the healing process and complications inherent in each of the systems were evaluated. RESULTS: Intra-operative complications of Seidel-nailing (Group 1) were seen in 5 cases: failure of the proximal target device in 2 (4.2%) cases; the breaking of the long screwdriver during the distal locking in 1 (2.1%) case; blockade of nail-insertion due to the spreading distal lamellas in 1 (2.1%) case; in 1 (2.1%) case it was impossible to find the imbus of the distal locking screw with the screwdriver. Incorrect surgical technique resulting in further fragmentation of the shaft required revisions in 2 (4.2%) cases. In 3 cases (6.4%), the insertion of the nail was insufficient, so that an impingement resulted. In 12 cases, postoperative complications after Seidel-nailing resulted: 3 (6.4%) radial nerve palsies, of which 2 (4.2%) were transitory; 3 (6.4%) infections; in 3 (6.4%) cases, loosening of the locking bolt inserted in the frontal plane; in 1 (2.1%) case, loosening of the distal spreading screw. The system failed in treating 2 (of 4) non-unions, whereas successful ossification and repair occurred in all acute fractures. In Group 2 (UHN) the acute fractures of 33 cases healed without complications. Intra-operative complications of the unreamed nail: in 2 cases (5.6%), failure of the target devices resulted in malpositoning of interlocking screws. The following intra-operative complications of the retrograde technique were observed: burst of a fragment at the insertion site in 1 case (2.8%); intra-articular positioning of the most proximal interlocking screw in another case (2.8%). Postoperative complications of the unreamed nail: breaking of a proximal and a distal interlocking screw in 1 case (2.8%), which had no influence on the healing progress. In 1 case (2.8%) both proximal interlocking screws came loose and a non-union ensued. After re-osteosynthesis with the same technique, bony repair was achieved. CONCLUSION: The possibilities of operative methods in treatment of humeral shaft fractures are enhanced by intramedullary interlocking systems. Comparing with the Seidel nail, the unreamed humeral nail (UHN) has two advantages: it can be inserted anterogradely as well as retrogradely, and it provides the possibility of compressing the fracture, resulting in a high rotational stability. Due to these results, the application of the UHN is recommended.

Adult↗
PubMed2002

Synthesis, characterization, photophysical properties, and biological labeling studies of a series of luminescent rhenium(I) polypyridine maleimide complexes.

We report the synthesis, characterization, and photophysical properties of a series of rhenium(I) polypyridine maleimide complexes [Re(N-N)(CO)(3)(py-3-mal)](CF(3)SO(3)) [N-N = 1,10-phenanthroline, phen (1), 2,9-dimethyl-1,10-phenanthroline, 2,9-Me(2)-phen (2), 3,4,7,8-tetramethyl-1,10-phenanthroline, 3,4,7,8-Me(4)-phen (3), 4,7-diphenyl-1,10-phenanthroline, 4,7-Ph(2)-phen (4), 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline, 2,9-Me(2)-4,7-Ph(2)-phen (5), 2,2'-biquinonine, biq (6); py-3-mal = N-(3-pyridyl)maleimide]. The X-ray crystal structure of complex 2 has been investigated. Upon excitation, the complexes exhibit intense and long-lived photoluminescence in fluid solutions at 298 K. The emission wavelengths range from 514 to 654 nm, and the emission lifetimes fall in the microsecond time scale. The luminescence is assigned to originate from a metal-to-ligand charge-transfer MLCT [dpi(Re) --> pi*(diimine)] triplet excited state. As the maleimide group can react with the sulfhydryl group to form a stable thioether moiety, these complexes have been used as thiol-specific luminescent labels for a thiolated oligonucleotide, glutathione, and bovine serum albumin and human serum albumin. The photoluminescence properties of the labeled biological species have also been investigated.

Animals↗
PubMed1998

Synthesis and Characterization of Rhenium(VI) cis-Dioxo Complexes and Examination of Their Redox Chemistry.

Reaction of rhenium(V)-oxo-halo-triflate complexes (HB(pz)(3))ReO(X)OTf (1, X = Cl, Br, I) with 1 equiv of pyridine N-oxide forms rare d(1) rhenium(VI) cis-dioxo compounds (HB(pz)(3))ReO(2)X (2, X = Cl, Br, I). This reaction likely occurs by initial formation of the d(0) rhenium(VII) dioxo cation (HB(pz)(3))ReO(2)X(+) by oxygen atom transfer, followed by a rapid one electron reduction. The chloride derivative 2a has been characterized by an X-ray crystal structure. The d(1) dioxo compounds are fairly stable, disproportionating slowly to (HB(pz)(3))ReO(3) and (HB(pz)(3))ReOX(2). Electrochemical oxidations of (HB(pz)(3))ReO(2)X to Re(VII) cations are reversible and are at remarkably high potentials (E(1/2) = 0.93 V vs Cp(2)Fe(+/0) in acetonitrile for 2a). When Me(2)SO is used as the oxidant instead of pyridine N-oxide, the Re(V) adducts [(HB(pz)(3))ReO(X)(OSMe(2))][OTf] (5) are formed by triflate displacement. These complexes reversibly lose SMe(2) (for 5a, k = 3.3(4) x 10(-)(6) s(-)(1) at 297 K in CD(2)Cl(2)), as shown by isotope exchange experiments. The intermediate Re(VII) cations (HB(pz)(3))ReO(2)X(+) oxidize Me(2)S much faster than Me(2)SO, indicating that they are highly electrophilic oxygen atom transfer reagents. Complexes 2, however, are relatively unreactive materials. Crystallographic data for 2a: C(9)H(10)BClN(6)O(2)Re; monoclinic, Cc; a = 14.716(3), b = 7.651(2), c = 13.232(3) Å; beta = 110.61(3) degrees; Z = 4.

Journal Article↗
PubMed2006

Very small and soft scorpionates: water stable technetium tricarbonyl complexes combining a bis-agostic (k(3)-H, H, S) binding motif with pendant and integrated bioactive molecules.

The novel trihydro(mercaptoazolyl)borates Na[H(3)B(tim(Me))] (L(1)) (tim(Me) = 2-mercapto-1-methylimidazolyl), Na[H(3)B(tim(Bupip))] (L(2)) (tim(Bupip) = 1-[4-((2-methoxyphenyl)-1-piperazinyl)butyl]-2-mercaptoimidazolyl), and Na[H(3)B(bzt)] (L(3)) (bzt = 2-mercaptobenzothiazolyl) were synthesized by reaction of NaBH(4) with the corresponding azole. Ligands L(1)-L(3) represent a new class of light and soft scorpionates that stabilizes the [M(CO)(3)](+) core (M = (99)Tc, Re) by formation of the complexes fac-[M{kappa(3)-H(mu-H)(2)B(tim(Me))}(CO)(3)] (M = (99)Tc (1), Re (2)), fac-[Re{kappa(3)-H(mu-H)(2)B(tim(Bupip))}(CO)(3)] (3), and fac-[Re{kappa(3)-H(mu-H)(2)B(bzt)}(CO)(3)] (4), respectively. The soft scorpionates are coordinated to the metal in unique (kappa(3)-H, H', S) fashion, as confirmed by X-ray crystallography of 1, 2, and 4. These complexes with bis-agostic hydride coordination are formed in aqueous solution with the two hydrides replacing two coordinating aquo ligands. The agostic hydrogen atoms were located directly, confirming an unprecedented donor atom set combining one sulfur and two hydrogen atoms. Preliminary studies have shown the possibility of preparing some of these complexes at the no carrier added level ((99m)Tc), under conditions as required in radiopharmaceutical preparation. Due to their lipophilicity, small-size, and easy functionalization with adequate biomolecules, the trihydro(mercaptoazolyl)borate technetium tricarbonyl complexes are suitable for the design of CNS receptor ligand radiopharmaceuticals as exemplified with 3, comprising a pendant serotonergic 5-HT(1A) ligand. The integrated design of radiopharmaceuticals involving a bis-agostic scorpionate ligand is demonstrated by the synthesis of 4, with an integrated benzothiazolyl fragment for the recognition of beta-amyloid plaques.

Journal Article↗
PubMed2002

Experimental and theoretical insights regarding the cycloaddition reaction of carbohydrate-based 1,2-diaza-1,3-butadienes and acrylonitrile. A model case for the behavior of chiral azoalkenes and unsymmetric olefins.

A series of carbohydrate-based tetrahydropyridazines are prepared by the hetero-Diels-Alder reaction of the chiral 1,2-diaza-1,3-butadienes 1 and 2 with acrylonitrile. Reactions are regiospecific, and the observed diastereoselection is consistent with a preferred attack to the Re face of the heterodiene unit, as the chiral sugar placed at C4 does largely protect the opposite Si face. The stereochemistry of the major cycloadduct 4 has been firmly established by an X-ray crystallographic study that, in addition, reveals a conformation placing the cyano group in axial orientation. Cycloadducts such as 9 and 11, in which the axial cyano group and the carbohydrate moiety exhibit a cis relationship, undergo a facile E2 elimination that relieves the steric congestion. A detailed computational study is reported to provide better insight into the factors that influence this asymmetric cycloaddition. A DFT study (B3LYP/6-31G) on a reduced model does correctly predict the regiochemistry observed experimentally, while the facial diastereoselection is modeled at a semiempirical (PM3) level on the parent reagents, thereby accounting for the steric factor provided by the chiral substituent. The calculations also indicate that the axial orientation of the cyano group can be rationalized in terms of a stabilizing anomeric effect.

Journal Article↗
PubMed2004

Computational redesign of protein-protein interaction specificity.

We developed a 'computational second-site suppressor' strategy to redesign specificity at a protein-protein interface and applied it to create new specifically interacting DNase-inhibitor protein pairs. We demonstrate that the designed switch in specificity holds in in vitro binding and functional assays. We also show that the designed interfaces are specific in the natural functional context in living cells, and present the first high-resolution X-ray crystallographic analysis of a computer-redesigned functional protein-protein interface with altered specificity. The approach should be applicable to the design of interacting protein pairs with novel specificities for delineating and re-engineering protein interaction networks in living cells.

Bacterial Proteins↗
PubMed1989

[Relationship between pocket reduction and plaque control in initial treatment].

It has been suggested that plaque control is important in periodontal treatment. This study used O'Leary's plaque control record (PCR) to investigate the influence of plaque control in initial treatment. Thirty patients (18 men and 12 women, mean age 46.7 years) were selected for this study. The results were as follows: The mean pocket depth was reduced from 3.19 mm (at the first examination) to 2.11 mm (at re-evaluation). Mean pocket depth of 3 mm or more at the first examination was reduced from 4.09 mm to 2.43 mm. The mean number of times plaque control instruction was given to reduce the PCR 10% or less was 3.8. The quantity of pocket reduction was significantly greater in the group that underwent instructions to reduce the PCR 10% or less 4 times or less compared with the group that underwent instructions 5 times or more. The group whose mean PCR was 10% or less from the time 10% or less at the first time to re-evaluation, had significantly greater pocket reduction than the group with 20% or more. There was no correlation between pocket reduction and PCR at the first examination and bone loss scores obtained from X-ray films.

Dental Plaque↗
PubMed1999

[The effect of pedicle screw instrumentation on posterolateral spinal fusion. A prospective, randomized study with a two-year follow-up].

The aim was to evaluate the effect of supplementary pedicle screw fixation (Cotrel-Dubousset [CD]) in posterolateral lumbar spinal fusion. The study comprises 130 patients undergoing lumbar or lumbosacral fusion for spondyloisthesis grades I-II or degenerative segmental instability conditions. The patients were randomly allocated for no instrumentation (n = 66) or CD instrumentation (n = 64) in posterolateral lumbar fusion. A 97.7% follow-up was achieved. There were no significant differences between the two groups concerning fusion rates assessed by X-ray or functional outcomes assessed by Dallas Pain Questionnaire. The global patient satisfaction was 82% in the instrumented group versus 74% in the noninstrumented group. Instrumentation increased both operation time, blood loss, and early re-operation rates significantly. A high patient satisfaction was found in both groups. However, the results from this study do not justify the general use of pedicle screw fixation alone as an adjunct to posterolateral lumbar fusion.

Adult↗
PubMed2006

Analysis of the cell cycle of fibroblasts derived from the LEC rat after X-irradiation.

The LEC rat is reported to exhibit hypersensitivity to X-irradiation, deficiency in DNA double-strand break repair, and radio-resistant DNA synthesis. This character of the LEC rat has been thought to be due to abnormal G1 arrest in cells after X-irradiation. In this report, we re-investigated the effect of X-irradiation on the cell cycle in primary-cultured fibroblasts. Primary-cultured fibroblasts derived from LEC and BN rats were exposed to 4 Gy of X-ray and their cell cycle analysis was performed with a flow cytometer. Fibroblasts derived from both rats showed normal response of the cell cycle, indicating the arrest at both G1--and G2/M-phase and no difference in the cell cycle population between fibroblasts derived from both rats. In contrast, when the same analysis was performed using the cell line, L7 and W8, which had been established from the lung fibroblasts of LEC and control WKAH rats, respectively, by immortalizing with SV40 T-antigen, L7 cells but not W8 cells showed impaired G1 arrest and abnormal cell cycle. These results suggest that fibroblasts derived from LEC rats possess the normal cell cycle response after X-irradiation, if they are kept naive as not immortalized with SV40 T-antigen.

Animals↗
PubMed2007

Thymic carcinoma.

This is a case of thymic carcinoma-a rare and highly aggressive type of tumor found in the anterior mediastinum. During a routine chest X-ray, a 66-yr-old male pilot was found to have a mediastinal mass. After diagnosis, he underwent chemotherapy, surgery, and radiation therapy and 1 yr after completion of these therapies he was re-issued a third-class medical certificate to fly.

Aged↗
PubMed1996

[A case of hamartoma originated from the chest wall].

Hamartoma originated from the chest wall is rare. All reported cases are infant's ones. A 16-year-old man was admitted to our hospital because of chest pain and abnormal shadow in routine chest X-ray film. Thoracotomy was performed under the diagnosis of pulmonary sequestration in the left apical region. However, the operation revealed a tumor originated from the chest wall, which was diagnosed hamartoma by histological examination. Re-operation was required because of hemothorax caused by residual tumor. Second and third ribs were resected with residual tumor. There is no evidence of recurrence one year after the second operation.

Adolescent↗
PubMed2004

A new method to determine the structure of the metal environment in metalloproteins: investigation of the prion protein octapeptide repeat Cu(2+) complex.

Since high-intensity synchrotron radiation is available, "extended X-ray absorption fine structure" spectroscopy (EXAFS) is used for detailed structural analysis of metal ion environments in proteins. However, the information acquired is often insufficient to obtain an unambiguous picture. ENDOR spectroscopy allows the determination of hydrogen positions around a metal ion. However, again the structural information is limited. In the present study, a method is proposed which combines computations with spectroscopic data from EXAFS, EPR, electron nuclear double resonance (ENDOR) and electron spin echo envelope modulation (ESEEM). From EXAFS a first picture of the nearest coordination shell is derived which has to be compatible with EPR data. Computations are used to select sterically possible structures, from which in turn structures with correct H and N positions are selected by ENDOR and ESEEM measurements. Finally, EXAFS spectra are re-calculated and compared with the experimental data. This procedure was successfully applied for structure determination of the Cu(2+) complex of the octapeptide repeat of the human prion protein. The structure of this octarepeat complex is rather similar to a pentapeptide complex which was determined by X-ray structure analysis. However, the tryptophan residue has a different orientation: the axial water is on the other side of the Cu.

Algorithms↗