The addition of diethylcyanamide to a tetrahydrofuran solution of lithium dialkylamide LiN(CH(3))(2) or Li NCH(2)CH(2)CH(2) CH(2), Li(PYR), results in the corresponding lithium 1,1,3,3-tetraalkylguanidinate, Li(TAG). The subsequent metathesis reaction of Li(TAG) with CuCl generates hexanuclear copper(I) complexes with the general formula [Cu(mu-TAG)](6), where TAG = DEDMG (1) and DEPYRG (2).
Diethylcyanamide is added to a hexanes solution of lithium diethylamide [LiN(CH(2)CH(3))(2)] resulting in the formation of lithium 1,1,3,3-tetraethylguanidinate, [Li(mu-TEG)](6) (1). Upon successful isolation of 1, the metathesis reaction of MX(2) (MX(2) = MnBr(2), FeBr(2), CoBr(2), and ZnCl(2)) with [Li(mu-TEG)](6) and lithium bistrimethylsilylamide, LiN(SiMe(3))(2), was performed to generate dinuclear tetraethylguanidinate (TEG) complexes with the general formula [M(mu-TEG){N(SiMe(3))(2)}](2) {M = Mn (2), Fe (3), Co (4), Zn (5)}. Further reaction of 2 with 2 equiv of ethanol (EtOH) and 2 equiv of 2,6-ditert-butylphenol (H-DBP) results in the formation of the manganese alkoxide, [Mn(mu-OEt)(DBP)(H-TEG)](2) (6). Elemental analysis, FT-IR spectroscopy, UV-vis spectroscopy, and single crystal X-ray diffraction were utilized to characterize the six compounds.
Background: Shoulder impingement syndrome is one of the most common causes of shoulder pain, accounting for approximately 30% of all shoulder pain. Approximately 35% of patients with shoulder impingement syndrome are refractory to conservative treatment. For patients who fail conservative treatment, there is no established treatment to successfully treat their chronic pain. Prior randomized control trials have demonstrated efficacy for the use of a single lead intramuscular peripheral nerve stimulation of the axillary nerve at the motor points of the deltoid muscle for treatment of hemiplegic shoulder pain. This is the first controlled trial to utilize the same novel technology to treat shoulder impingement syndrome outside of the stroke population. Methods: This is a dual-site, placebo-controlled, double-blinded, randomized control trial. Participants will be randomized to two treatment groups. The intervention group will be treated with active peripheral nerve stimulation of the axillary nerve of the affected shoulder and the control group will be treated with sham peripheral nerve stimulation of the axillary nerve of the affected shoulder. Both groups will receive a standardized exercise therapy program directed by a licensed therapist.Discussion: This study protocol will allow the investigators to determine if this novel, non-pharmacologic treatment of shoulder pain can demonstrate the same benefit in musculoskeletal patients which has been previously demonstrated in the stroke population.
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