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51.
H.-J. Mai S. Wocadlo H.-C. Kang W. Massa K. Dehnicke C. Maichle-Mssmer J. Strhle D. Fenske 《无机化学与普通化学杂志》1995,621(5):705-712
Phosphanimine and Phosphoraneiminato Complexes of Iron. The Crystal Structures of [FeCl3(Me3SiNPEt3)], [FeCl2(Me3SiNPEt3)]2, [FeCl2(NPEt3)]2, and [Fe(O2C? CH3)2(NPEt3)]2 The phosphanimine complexes [FeCl3(Me3SiNPEt3)] (red-orange) and [FeCl2(Me3SiNPEt3)]2 (colourless) have been prepared by reactions of Me3SiNPEt3 with FeCl3 and FeCl2, respectively, in CH2Cl2 suspensions. Thermal decomposition of these donor-acceptor complexes in boiling toluene leads to the phosphoraneiminato complex [FeCl2(NPEt3)]2 (black), whereas [Fe(O2C? CH3)2(NPEt3)]2 (brown) is formed from iron(II) acetate and Me3SiNPEt3 in boiling acetonitrile. The complexes are characterized by IR spectroscopy and by crystal structure determinations. [FeCl3(Me3SiNPEt3)] (1) : Space group P21/c, Z = 8, structure determination with 4 673 unique reflections, R = 0.033. Lattice dimensions at ?15°C: a = 1 607.8, b = 1 602.0, c = 1 417.2 pm, β = 106.56°. 1 forms monomeric molecules with tetrahedrally coordinated iron atoms. Bond lengths in average: Fe? N = 196.9 pm, Fe? Cl = 219.7 pm. [FeCl2(Me3SiNPEt3)]2 (2) : Space group P21/c, Z = 4, structure determination with 4 992 unique reflections, R = 0.048. Lattice dimensions at 20°C: a = 1 457.9, b = 1 685.4, c = 1 507.3 pm, β = 116.74°. 2 forms dimeric molecules, which are associated by chloro bridges. The iron atoms are tetrahedrally coordinated with trans positions of the phosphanimine ligands. Both lengths in average: Fe? N = 202.2 pm, Fe? Clterminal = 224.7 pm, Fe? Cl bridge = 241.0 pm. [FeCl2(NPEt3)]2 (3): Space group P21/n, Z = 2, structure determination with 2763 unique reflections, R = 0.039. Lattice dimensions at ?70°C: a = 799.1, b = 1009.0, c = 1441.9 pm, β = 93.45°. 3 forms centrosymmetric dimeric molecules, in which the tetrahedrally coordinated iron atoms are associated by the nitrogen atoms of the phosphoraneiminato ligands. Bond lengths in average: Fe? N = 191.4 pm, Fe? Cl = 222.7 pm. [Fe(O2C? CH3)2(NPEt3]2 (4): Space group P21/n, Z = 2, structure determination with 3005 observed unique reflections, R = 0.034. Lattice dimensions at -65°C: a = 886.4, b = 1444.6 pm, β = 90.60°. 4 forms centrosymmetric dimeric molecules, in which the octahedrally coordinated iron atoms are associated by the nitrogen atoms of the phosphoraneiminato ligands with bond lengths Fe? N of 191.9 and 195.0 pm. The acetate groups are coordinated in a chelating fashion. 相似文献
52.
During attempts to synthesize rare‐earth nitride tellurides black and bead‐shaped single crystals of the title compound sodium praseodymium(III) ditelluride (NaPrTe2) were obtained as a by‐product by reacting a mixture of praseodymium, sodium azide (NaN3) and tellurium at 900 °C for seven days in evacuated torch‐sealed silica vessels. NaPrTe2 crystallizes cubic (space group: Fd3¯m, Z = 16; a = 1285.51(9) pm, Vm = 79.96(1) cm3/mol, R1 = 0.028 for 146 unique reflections) and exhibits the Na+ and Pr3+ cations in slightly distorted octahedra of six telluride anions (d(Na—Te) = 325 pm, d(Pr—Te) = 317 pm) each. The main characteristics of this new structure type for alkali‐metal rare‐earth(III) dichalcogenides can be derived from the rock‐salt type structure (NaCl, cubic closest‐packed Te2— arrangement, all octahedral voids occupied with Na+ and Pr3+) with alternating layers consisting of Na+ and Pr3+ cations in a ratio of 3:1 and 1:3, respectively, piled along the [111] direction. 相似文献
53.
烟酸对酸性硫酸盐体系铜电沉积的影响 总被引:2,自引:0,他引:2
对溶液A: 0.8 mol•L-1硫酸铜,0.6 mol•L-1硫酸,5.0×10-5 mol•L-1氯离子,1.0×10-4 mol•L-1聚乙二醇的溶液,溶液B:在溶液A中加入2.0×10-2 mol•L-1烟酸,pH为0.5,运用循环伏安和计时安培法研究玻碳电极上铜的电沉积行为.结果表明,铜的电沉积过程经历了晶核形成过程,其电结晶按瞬时成核和三维生长方式进行.烟酸的加入对铜的电沉积具有阻化作用,但不改变铜的电结晶机理.沉积层的X射线衍射表明Cu为面心立方结构,在烟酸存在下沉积层出现(220)高择优取向,这可能是烟酸在Cu(220)晶面上发生强烈吸附作用的结果. 相似文献
54.
Single crystals of (NMe4)(HF2) were obtained during attempted recrystallization of NMe4F from fluoroolefin. X‐ray diffraction data show that (NMe4)(HF2) crystallizes in the orthorhombic space group Pmmn with unit cell dimensions a = 6.535(2), b = 8.688(3), and c = 5.333(2) Å. The symmetric and virtually linear HF2 anions exhibit a short F···F distance of 2.256(2) Å. The both crystal structures of (NMe4)(H2F3) (orthorhombic, Pbca, a = 8.509(1), b = 11.273(2), and c = 14.880(2) Å) and CsH2F3 (orthorhombic, P212121, a = 7.345(3), b = 9.126(4), and c = 11.444(4) Å) contain dihydrogentrifluoride anions, H2F3?, which have a bent shape and F···F distances of 2.30‐2.34Å. 相似文献
55.
本研究采用直接曝热技术,分别以氢气和甲烷为反应气,测定了10个血卟啉衍生物和13个金属血卟啉衍生物的正、负离子解吸化学电离质谱,探讨了各种化学电离质谱法在结构测定中的应用。 相似文献
56.
EVA-g-VC的结构和动态粘弹性 总被引:1,自引:0,他引:1
本文研究了聚乙烯-醋酸乙烯酯(EVA,VAc:14%)与氯乙烯(VC)接枝共聚物(EVA-g-VC)的相结构和分子结构。接枝物EVA-g-VC由游离EVA、均聚PVC和EVA-VC接枝高分子三者组成,EVA呈连续相,PVC呈分散微粒。EVA-g-VC中EVA的含量越高,PVC粒子体积越小。实验结果表明,接枝物中“凝胶”的EVA玻璃化温度,随投料比(VC/EVA)的减小而升高;另外随VC/EVA减小,凝胶中PVC的含量和PVC的分子量也减小。这些结果说明,VC/EVA较小时得到的接枝物中,EVA上VC接枝点的数目较多,而PVC接枝链的长度较短。EVA-VC是不相容两相——EVA和PVC的“粘着剂”,其作用表现在:VC/EVA越小,接枝物中EVA和PVC的玻璃化温度越靠近。 相似文献
57.
簇合物[Fe(DMF)6][W2S6]的合成,结构和性能研究 总被引:4,自引:0,他引:4
以(NH_4)_2WS_4、FeCl_3和NaS_2CNC_5H_(10)为原料,合成出[Fe(DMF)_6][W_2S_6]簇合物,用X射线衍射法测定了晶胞结构.其晶胞参数为a=0.8778(1)nm,b=0.9467(3)nm,c=1.1362(6)nm,α=71.506(1)°,β=74.775(2)°,γ=74.775(2)°,ν=0.84806nm~3,Z=1.晶体结构经块矩阵最小二乘法精修后,最终偏离因子R=0.0811.此外还进行了红外光谱、紫外可见光谱的测定. 相似文献
58.
Ternary Lithium Rare Earth Nitrates with Lonesome Nitrate Ions: Li3[M(NO3)5](NO3) (M = Gd? Lu, Y). The Crystal Structure of Li3Er(NO3)6 Single crystals of the ternary nitrate Li3Er(NO3)6 are obtained from a solution of “Er(NO3)3” in the melt of LiNO3. In Li3Er(NO3)6 (monoclinic, P21/n, Z = 4; a = 776.0(1); b = 748.86(8); c = 2 396(1) pm; β = 90.76(3)°; R1 = 0.0490; wR2 = 0.0792), Er3+ is surrounded by five bidentate nitrate ligands yielding the anionic units [Er(NO3)5]2?. These are arranged in the direction of the 21 screw axis. Two lonesome NO3? ions are in the middle of such a “helix” and are connected by Li+ with the anions [Er(NO3)5]2?. The helices are moved against each other by about half of the lattice constant a and are connected by further Li+ ions. 相似文献
59.
D. Rosmann K. -W. Klinkhammer A. Schmidt 《Monatshefte für Chemie / Chemical Monthly》1996,127(5):461-468
Zusammenfassung Arsen-tris(2,2-dimethylpropionat) (1) kristallisiert monoklin in der Raumgruppe P21/n mita=926.2,b=2158.6,c=983.7 pm, =94.92° undZ=4. As hat gegenüber O die Koordinationszahl 3+3. Antimontripropionat (2) kristallisiert monoklin in der Raumgruppe P21/c mita=930.2,b=863.0,c=1575.2 pm, =90.27 undZ=4. Die Moleküle sind intermolekular zu Ketten verknüpft, wodurch Sb die Koordinationszahl 3+3 (+3) erreicht.
Structure of arsen(III) and antimony(III) carboxylates
Summary Arsen-tris(2,2-dimethylpropionate) (1) crystallizes monoclinic in the space group P21/n witha=926.2,b=2158.6,c=983.7 pm, =94.92°, andZ=4. As has a coordination number of 3+3. Antimony tripropionate (2) crystallizes monoclinic in the space group P21/c witha=930.2,b=863.0,c=1575.2 pm, =90.27, andZ=4. The molecules are bridged to chains; therefore, Sb reaches the coordination number 3+3 (+3).相似文献
60.
Edith Gößnitzer Ales Krbavcic Winfried Wendelin Marija Krbavcic 《Monatshefte für Chemie / Chemical Monthly》2002,133(9):1177-1185
Summary. Novel N-(3-oxobutyl)-hydroxy- and acetoxypyrido[2,3-d]pyridazinones were synthesized and tested in vivo for their sedative and anticonvulsant activity. The Michael-type reaction of quinolinic acid hydrazide and methyl vinyl ketone afforded a mixture of two isomers, 5-hydroxy-N
7-(3-oxobutyl)-pyrido[2,3-d]pyridazin-8(7H)-one and 8-hydroxy-N
6-(3-oxobutyl)-pyrido[2,3,-d]pyridazin-5-(6H)-one, in a ratio of 2:1 which were separated by crystallization. Subsequent acetylation of both isomers yielded the corresponding
5- and 8-acetoxy compounds. The structures of the compounds were proven and completely assigned on the basis of 1H, 13C, 15N NMR, and 1D NOE difference spectra as well as 2D C,H-correlation experiments. Preliminary pharmacological tests showed low
acute toxicity with a LD
50 > 1000 mg/kg in the mouse and sedative activity for the title compounds. 5-Acetoxy-N
7- (3-oxobutyl)-pyrido[2,3-d]pyridazin-8(7H)-one displayed a borderline anticonvulsant activity in the metrazole test model.
Corresponding author. E-mail: edith.goessnitzer@uni-graz.at
Received March 20, 2002; accepted April 3, 2002 相似文献