Preparation of trans-RuH(η1-BH4)L (L = Me6[15]aneS4, Me8[16]aneS4) and oxidation in alcohols to give trans-{Ru(OR)2(anti-Me8[16]aneS4)}+ R = Me, Et). Crystal structures of the hydrido and ethoxo complexes of Me8[16]aneS4

1995 
Abstract Reaction of cis -RuCl 2 L (L = Me 8 [16]aneS 4 , Me 6 [15]aneS 4 ) with an excess of NaBH 4 in EtOH gave trans -RuH( η 1 -BH 4 )L(L = Me 8 [16]aneS 4 (1); Me 6 [15] ane S 4 (2)). The monodentate coordination of the BH 4 − ligand in 1 was confirmed by a single crystal X-ray diffraction study. It crystallizes in monoclinic space group P 2 1 / c , with Z = 4, a = 13.720(5), b = 17.975(6), c = 13.033(3) A , β = 113.86(3)°, R (R w ) = 0.070 (0.070) for 2258 reflections (| F O |⩾4 σ ( F o )) and 272 parameters. Reaction 1 with O 2 and subsequent treatment with alcohols produced trans -{ Ru ( OR ) 2 ( ani - Me 8 [16] aneS 4 )} + ( if (R = Me (3), Et (4)). The diethoxo complex was fully characterized by X-ray crystallography: monoclinic, space group C2/c, c = 16.627(5), b = 11.917(4), c = 18.418(9) A , β = 102.80(3)°, Z = 4, R ( R w = 0.036 (0.040) for 3491 reflections (| F o |⩾3 σ ( F O )) and 312 parameters.
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