螺[1-溴-4-(1R,2S,5R)-l-孟氧基-5-氧杂-6-氧代双环[3.1.0]己烷-2,2'-(3'-α-膦酸二乙酯基-(S)-苯甲氧基-4'-l-(1R,2S,5R)-孟氧基丁内酯)]的晶体结构

Crystal Structure of Spiro[1-bromo(S)-4-l-(1R,2S,5R)-menthyloxy-5- oxa-6-oxo-bicyclo[3.1.0]hexane-2,2'(3'diethyl-α-(R)-benzyloxy- phosphonyl-4'-l-(1R,2S,5R)-menthyloxybutyrolactone )]

报道了标题化合物合成和晶体结构。X-射线结构分析表明,该化合物的分子式为C39H58BrO10P,Mr = 797.74,晶体属于单斜晶系,空间群为P21,晶胞参数a = 12.858(3), b = 25.130(5), c = 14.125(3) ? = 105.15(3), V = 4405(2) ?, Z = 4, Dc = 1.203 g/cm3, ?= 1.019 mm-1, F(000) = 1688,R = 0.0726, wR = 0.1201,共收集到9691个独立衍射点,其中可观测点5638个(I≥2s(I))。每个分子中有6个环,13个手性中心,2个五员环呈信封式构象,并分别与三员环组合成[2.4]螺环和[3.1.0]桥环化合物,4个新生成的手性中心的绝对构型为C(6)(S), C(7)(S), C(3)(R), C(2)(R),新引入的磷酸酯官能团C(9)为S构型。

The crystal structure of the title compound 3a (C39H58BrO10P, Mr = 797.74) was determined by single- crystal X-ray diffraction. It belongs to monoclinic, space group P21 with a = 12.858(3), b = 25.130(5), c = 14.125(3) ? = 105.15(3), V = 4405(2) ?, Z = 4, Dc = 1.203 g/cm3, = 1.019 mm-1, F(000) = 1688, the final R = 0.0726 and wR = 0.1201 for 5638 observed reflections with I≥2s(I). The molecule has 6 cycles, of which the two six-membered rings of the menthyloxyl are shown as chair conformation and the two lactones are in envelope conformation. Meanwhile, the lactones fuse with cyclopropane to form the compound with spiro[4.2] and bicyclo[3.1.0] skeletons, respectively. In addition, there exist 13 chiral centers in the molecule. The 4 stereogenic centers are C(6)(S), C(7)(S), C(3)(R) and C(2)(R), and the chiral center C(9) maintains original S-configuration of diethyl-a-(S)-benzyloxy-phosphonyl building block.