(MeOH)4]·8MeOH (2). A test tube (5 mL) containing a solution
of NiCl2·6H2O (13 mg, 0.054 mmol) in methanol (4 mL) was
placed inside a boiling tube (25 mL) containing a solution of 1
(60 mg, 0.054 mmol) in methanol (10 mL). The tubes were
slowly filled with methanol (ca. 10 mL) until the two solutions
are able to mix. Red block crystals suitable for X-ray determination
were obtained after standing the set-up for 2 weeks at
room temperature. Yield: 30%. Selected IR (KBr, cm−1): ν(N3)
2065. ESI/MS: m/z 640 {[Ru(sap)]2(μ-N)}+; (Anal. calcd(found) for C60H62Ni2N12O16Ru4: C, 41.68 (41.70); H, 3.61
(3.54); N, 9.72 (9.65).
of NiCl2·6H2O (13 mg, 0.054 mmol) in methanol (4 mL) was
placed inside a boiling tube (25 mL) containing a solution of 1
(60 mg, 0.054 mmol) in methanol (10 mL). The tubes were
slowly filled with methanol (ca. 10 mL) until the two solutions
are able to mix. Red block crystals suitable for X-ray determination
were obtained after standing the set-up for 2 weeks at
room temperature. Yield: 30%. Selected IR (KBr, cm−1): ν(N3)
2065. ESI/MS: m/z 640 {[Ru(sap)]2(μ-N)}+; (Anal. calcd(found) for C60H62Ni2N12O16Ru4: C, 41.68 (41.70); H, 3.61
(3.54); N, 9.72 (9.65).
