The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) ?, β = 114.581(3)o, V = 1336.7(3) ?3 , Z = 4, Dc = 1.254 g/...The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) ?, β = 114.581(3)o, V = 1336.7(3) ?3 , Z = 4, Dc = 1.254 g/cm3, μ(MoKa) = 0.081 cm-1 and F(000) = 536.00. The final R and wR are 0.0527 and 0.1285, respectively for 3058 observed reflections (I > 2σ(I)). In the title molecule, two phenyl rings are rotated oppositely with respect to the central part C(1)–C(2)=C(3)– C(4) (plane 3) and the dihedral angle between them is 14.8o. The phenone O(1) atom deviates from plane 3 by 0.291 ?. In the crystal the molecules form H-bond chains of R2 (6) and R2 (5) types 1 1 along [001]. The molecule chains interacted through three cooperative C–H…O H-bonds (R3 (11)) 1 in the ‘bay area’ (Fig. 3), extending along [010] and forming layer (100). Between the layers, there exist C–H/π interactions along [101]. Studies on the cooperative C–H…O H-bonds R3 (11) in the 1 similar crystals are also presented.展开更多
The reactions of dilithium salt of trans-1,2-bis（trimethylsilylamino）cyclohexane with anhydrous lanthanide trichlorides LnCl3 （Ln = Yb, Nd） in THF afforded the dianionic binuclear tricycles of lanthanide chlorides...The reactions of dilithium salt of trans-1,2-bis（trimethylsilylamino）cyclohexane with anhydrous lanthanide trichlorides LnCl3 （Ln = Yb, Nd） in THF afforded the dianionic binuclear tricycles of lanthanide chlorides {Li（THF）3[LnCl（μ2-trans-1,2-（NSiMe3）2C6H10）（μ2-Cl）]}2·2THF （Ln=Yb 1, Nd 2） in moderate yields. Both of the bridged complexes were characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. Crystal structural analysis shows that the two complexes are the analogues which have a tricyclic framework built by two bridged lanthanide metals, four nitrogens and four carbons from two diamide ligands. Each lanthanide metal coordinates to three nitrogen atoms and two chlorines to form a distorted trigonal bipyramid and connects with a lithium by a bridging chlorine.展开更多
The reaction of anhydrous YbCl3 with 1 equiv, of Li2Me2Si（NPh）2 in THF, after workup, yielded a ytterbium（Ⅲ） chloride [{Me2Si（NPh）2Yb}（μ2-CI）（TMEDA）]2·3PhMe （1） （TMEDA=tetramethylethanediamine）. T...The reaction of anhydrous YbCl3 with 1 equiv, of Li2Me2Si（NPh）2 in THF, after workup, yielded a ytterbium（Ⅲ） chloride [{Me2Si（NPh）2Yb}（μ2-CI）（TMEDA）]2·3PhMe （1） （TMEDA=tetramethylethanediamine）. The same reaction followed by treatment with Na-K alloy afforded a new ytterbium（H） complex supported by a bridged diamide with four coordinated LiC1 molecules, [{Me2Si（NPh）2Yb（THF）2}（μ3-CI）（μ4-CI）{Li（THF）}2]2·2THF （2） in high yield. Both complexes were structurally characterized by X-ray analysis to be dimers. Complex 1 was a chlorine-bridged dimer with ytterbium in a distorted octahedral geometry. In complex 2 two [Me2Si（NPh）2Yb（THF）2]- （μ3-CI）[Li（THF）]2 moieties were connected with each other by two μ4-CI bridges to form a ＂chair-form＂ framework.展开更多
基金This research was supported by the Key Subject Foundation of Jiangsu Province(S1109001)
文摘The title compound (C17H16O2, Mr = 252.30) crystallizes in the monoclinic system, space group P21/c with a = 11.5763(14), b = 11.0321(11), c = 11.5094(13) ?, β = 114.581(3)o, V = 1336.7(3) ?3 , Z = 4, Dc = 1.254 g/cm3, μ(MoKa) = 0.081 cm-1 and F(000) = 536.00. The final R and wR are 0.0527 and 0.1285, respectively for 3058 observed reflections (I > 2σ(I)). In the title molecule, two phenyl rings are rotated oppositely with respect to the central part C(1)–C(2)=C(3)– C(4) (plane 3) and the dihedral angle between them is 14.8o. The phenone O(1) atom deviates from plane 3 by 0.291 ?. In the crystal the molecules form H-bond chains of R2 (6) and R2 (5) types 1 1 along [001]. The molecule chains interacted through three cooperative C–H…O H-bonds (R3 (11)) 1 in the ‘bay area’ (Fig. 3), extending along [010] and forming layer (100). Between the layers, there exist C–H/π interactions along [101]. Studies on the cooperative C–H…O H-bonds R3 (11) in the 1 similar crystals are also presented.
基金Project supported by the National Natural Science Foundation of China （No. 20472063）.
文摘The reactions of dilithium salt of trans-1,2-bis（trimethylsilylamino）cyclohexane with anhydrous lanthanide trichlorides LnCl3 （Ln = Yb, Nd） in THF afforded the dianionic binuclear tricycles of lanthanide chlorides {Li（THF）3[LnCl（μ2-trans-1,2-（NSiMe3）2C6H10）（μ2-Cl）]}2·2THF （Ln=Yb 1, Nd 2） in moderate yields. Both of the bridged complexes were characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. Crystal structural analysis shows that the two complexes are the analogues which have a tricyclic framework built by two bridged lanthanide metals, four nitrogens and four carbons from two diamide ligands. Each lanthanide metal coordinates to three nitrogen atoms and two chlorines to form a distorted trigonal bipyramid and connects with a lithium by a bridging chlorine.
基金Project-supported by the National Natural Science Foundation of China （No. 20472063）.
文摘The reaction of anhydrous YbCl3 with 1 equiv, of Li2Me2Si（NPh）2 in THF, after workup, yielded a ytterbium（Ⅲ） chloride [{Me2Si（NPh）2Yb}（μ2-CI）（TMEDA）]2·3PhMe （1） （TMEDA=tetramethylethanediamine）. The same reaction followed by treatment with Na-K alloy afforded a new ytterbium（H） complex supported by a bridged diamide with four coordinated LiC1 molecules, [{Me2Si（NPh）2Yb（THF）2}（μ3-CI）（μ4-CI）{Li（THF）}2]2·2THF （2） in high yield. Both complexes were structurally characterized by X-ray analysis to be dimers. Complex 1 was a chlorine-bridged dimer with ytterbium in a distorted octahedral geometry. In complex 2 two [Me2Si（NPh）2Yb（THF）2]- （μ3-CI）[Li（THF）]2 moieties were connected with each other by two μ4-CI bridges to form a ＂chair-form＂ framework.
