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The reaction of Mo(0) complex [Mo(CO)_4(S_2CNEt_2)]~- with phenthiolate [Et_4N]SΦin acetonitrilo in the presence of small amount of air affords a new oxo-molybdenum com-plex [MoO(SΦ)_2(S_2CNEt_2)]~-,which crystallizes in two forms of crystals,[Et_4N][MoO(SΦ)_2(S_2CNEt_2)](1a) and [Et_4N][MoO(SΦ)_2(S_2CNEt_2)]·(CH_3)_2CHOH (1b).The structures of1a and 1b were determined from three-dimensional X-ray data.1a crystallizes in the mo-noclinie,space group C_c with a=12.321(4),b=15.245(4),c=16.087(9);β=98.44(4)°.V=2989~3,Z=4,D_c=1.35 g/cm~3 and R=0.031 for 2434 reflections [I>3(I)].1b crystallizes inthe monoclinic,space group P2_1/n with a=9.861(1),b=20.357(3),c=17.122(5)A;β=92.27(2)°,V=3434.3~3,Z=4;D_c=1.29 g/cm~3 and R=0.051 for 2852 independeut reflections [I>3σ(I)],The structures of 1a and 1b reveal that the anion [MoO(SΦ)_2(S_2CNEt_2)]~- contains asingle oxo ligand coordinating to a molybdenum(Ⅳ) and the geometry around Me(Ⅳ) atomis a distorted square pyramid.Interestingly,the solvate molecule isopropanol of 1b is linkedto oxo group by a hydrogen-bond of 1.928A,leading to the increase of Mo=O bond distance(1.718).Mo—S distances are 2.44 and 2,39.The electrochemical behavior of 1 wasdiscussed also.
The reaction of Mo (0) complex [Mo (CO) _4 (S_2CNEt_2)] with phenthiolate [Et_4N] SΦin acetonitrilo in the presence of small amount of air affords a new oxo-molybdenum com plex [MoO (SΦ) (S_2CNEt_2)] - which crystallizes in two forms of crystals [Et_4N] [MoO (SΦ) _2 (S_2CNEt_2)] (1a) and [Et_4N] [MoO (SΦ) _2 (S_2CNEt_2)] (1b). The structures of 1a and 1b were determined from three-dimensional X-ray data.1a crystallizes in the mo-noclinie, space group C_c with a = 12.321 (4), b = 15.245 (4), c = 16.087 Β = 98.44 (4) ° .V = 2989-3, Z = 4, D_c = 1.35 g / cm 3 and R = 0.031 for 2434 reflections [I> 3 (I)]. 1b crystallizes inthe monoclinic, Space group P2_1 / n with a = 9.861 (1), b = 20.357 (3), c = 17.122 (5) A; β = 92.27 (2) °, V = 3434.3-3, Z = 4; D_c = 1.29 g / cm ~ 3 and R = 0.051 for 2852 independeut reflections [I> 3σ (I)], The structures of 1a and 1b reveal that the anion [MoO (SΦ) _2 (S_2CNEt_2)] - contains asingle oxo ligand coordinating to a molybdenum (IV) and the geometry around Me (IV) atomis a distorted square pyramid.Interestingly, the solvate molecule isopropanol of 1b is linked to oxo group by a hydrogen-bond of 1.928A, leading to the increase of Mo = O bond distance (1.718). Mo-S distances are 2.44 and 2,39. The electrochemical behavior of 1 wasdiscussed also