三(对氟苄基)氯化锡和三(对氟苄基)锡N,N-(1,4-亚丁基)氨荒酸酯的合成及晶体结构

合成了三(对氟苄基)氯化锡(1)和三(对氟苄基)锡N,N-(1,4-亚丁基)氨荒酸酯(2).通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征.用X射线单晶衍射测定了这两个化合物的晶体结构.化合物1为单斜晶系,空间群P21, a=0.8403(3) nm, b=0.5958(2) nm, c=2.0016(8) nm, β=97.052(6)°, Z=2, V=0.9945(7) nm3, Dc=1.608 g/cm3, μ=1.447 mm-1, R1=0.0397, wR2=0.0813.化合物2为单斜晶系,空间群P21/n, a=0.8786(9) nm, b=1.993(2) nm, c=1.5039(15) nm, β=103.548(15)°, Z=4, V=2.560(4) nm3, Dc=1.537 g/cm3, μ=1.197 mm-1, R1=0.0363, wR2=0.0796. 在1的晶体中,锡原子呈四配位畸变四面体构型;2的晶体中,锡原子则是五配位畸变三角双锥构型.     

有机锡化合物四对氰苄基锡(p-NCC6H4CH2)4Sn的合成、表征和晶体结构

The organotin(Ⅳ) compound (p-NCC₆H₄CH₂)₄Sn was synthesized by the reaction of p-cyanobenzyl chloride with tin. The compound was characterized by elemental analysis, IR, ¹H NMR, and the crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic, space group P1 with a=0.894 1(4) nm, b=0.977 9(4) nm, c=1.796 8(8) nm, V=1.386 9(11) nm³, Z=2, D_c=1.397 Mg·m^-3, μ(Mo Kα)=0.948 mm^-1, F(000)=588, R₁=0.046 9, wR₂=0.101 4. The tin atom adopts a distorted tetrahedral coordination geometry. CCDC: 272939.     

μ-氧-双[三(邻溴苄基)锡]的合成和结构研究

The tri(o-bromobenzyl)tin bromide was treated with aqueous solution of NaOH to formed the μ-oxygen-bis[tri(o-bromobenzyl)tin]. The crystal structures of compound was determined by X-ray diffraction. The crystal belongs to triclinic, space group with a=1.0544(4) nm, b=1.1029 (4) nm, c=1.1309 (4) nm, α =117.031(5) °, β=107.685 (6) °, γ=98.523(6) °, V=1.0506(6)nm³, Z=1, D_x=2.013g·cm^-3, μ(MoKα)=69.25cm^-1, F(000)=606, R₁=0.0524, wR₂=0.1196. In the struture the tin atom has a distorted tetrahedral geometry. CCDC: 220514.     

手性酒石酸二酰胺配体的合成及其锡络合物与苯甲醛的不对称加成

通过酒石酸乙酯和不同胺的酰胺化, 相应地合成到(+)N,N'-二苯基酒石酸二酰胺(2), (+)N,N'-二苄基酒石酸二酰胺(3),(+)N,N'-二环己基酒石酸二酰胺(4)和(+)N,N'-二正辛基酒石酸二酰胺(5).氯化亚锡与2当量的酒石酸二酰胺反应, 再加入烯丙基溴可制得手性锡络合物6, 锡络合物与苯甲醛反应,得到光学活性的高烯丙基化合物, 产率42～64％ , e.e.值24～62％.     

IR-spektroskopische Untersuchungen der Phasengleichgewichte im System Ru/Sn/O

Infrared Spectroscopic Investigations on Phase Equilibria in the System Ru/Sn/O Infrared spectroscopic investigations give evidence for the existence of new phases and their phase relations in the system Ru/Sn/O. The obtained results coincide well with X-ray diffraction investigation. The composition of two phases was found to correspond to the formula: RuSn₃O₄ and RuSn₅O₄. Evidence is given for the existence of a third phase, the composition should correspond to RuSn₉O₈.     

含锡介孔分子筛MCM-48的合成、表征及催化性能

自M41S问世以来[1],其在吸附、催化及催化剂载体等领域的应用成为人们研究的热点。但纯硅M41S本身不具有催化活性中心,不能直接应用于催化反应中,将具有催化活性的金属掺杂在分子筛骨架中是赋予M41S系列介孔分子筛催化性能的重要手段。文献[2,3]已报道了一些金属掺杂在MCM-41中     

New transparent conductors with the M7O12 ordered oxygen-deficient fluorite structure: from In4Sn3O12 to In5.5Sb1.5O12

A new transparent conductor, containing pentavalent antimony, In_4+xSn_3−2xSb_xO₁₂, has been synthesized for 0?x?1.5. The latter exhibits an ordered oxygen-deficient fluorite structure with an ordered distribution of Sb⁵⁺ and In³⁺/Sn⁴⁺ species in the octahedral and seven-fold coordinated sites, respectively. More importantly, it is shown that the electronic conductivity of this transparent conducting oxide (TCO) at room temperature, is one order of magnitude larger for x=1 (In₅SnSbO₁₂) than for x=0 (In₄Sn₃O₁₂) and it turns to a semi-metallic behavior in contrast to In₄Sn₃O₁₂ which is a semi-conductor. The potential of this new material, as TCO, is also shown by its reflectance spectra, similar to In₄Sn₃O₁₂, involving only a small increase of the optical bandgap, by 0.15 eV.     

二(对氯苄基)锡双吗啉氨荒酸酯和二(对氯苄基)氯化锡N,N-二乙基氨荒酸酯的合成、表征及晶体结构

利用二(对氯苄基)二氯化锡和吗啉氨荒酸钠、N, N-二乙基氨荒酸钠反应, 合成了二(对氯苄基)锡双吗啉氨荒酸酯C24H28Cl2N2O2S4Sn (Mr = 694.31) 1和二(对氯苄基)氯化锡N, N-二乙基氨荒酸酯C19H22Cl3N2S4Sn (Mr = 553.54) 2。用X-射线单晶衍射测定了这2个化合物的晶体结构, 测试结果表明:化合物1的晶体为单斜晶系, 空间群C2/c, a = 21.998(9), b = 6.469(3), c = 20.204(8) ,β= 94.444(6)o, Z = 4, V = 2866.3(19) 3, Dc = 1.609 g/cm3, m(MoKa) = 1.394 mm-1, F(000) = 1400, S = 0.955, (D/s)max = 0.000, R = 0.0389, wR = 0.0817。化合物2的晶体为单斜晶系, 空间群P21/c, a = 13.088(10), b = 9.304(7), c = 19.593(14) ,β=107.158(10)o, Z = 4, V = 2280(3) 3, Dc = 1.613 g/cm3, m(MoKa) = 1.660 mm-1, F(000) = 1104, S = 1.010, (D/s)max = 0.001, R = 0.0290, wR = 0.0651。在化合物1中, 锡原子呈六配位畸变八面体构型, 化合物2的锡原子则是五配位畸变三角双锥构型。