丙酮基三苯基磷和2-丁烯-1,4-双（三苯基磷）氯化物与硝酸的反应

IF 1 4区化学 Q4 CHEMISTRY, MULTIDISCIPLINARY Doklady Chemistry Pub Date : 2025-03-19 DOI:10.1134/S0012500825600063

V. V. Sharutin, D. P. Shevchenko, K. R. Khazhieva

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引用次数: 0

摘要

以丙酮-三苯基磷酸和反式-2-丁烯-1,4-双（三苯基磷酸）氯化物为原料，分别与硝酸反应合成了烷基三苯基硝酸磷[Ph3PCH2С(O)Me]NO3(1)和[Ph3PCH2CH=CHCH2PPh3][NO3]2·2H2O(2)。用红外光谱和单晶x射线衍射对化合物进行了表征。根据XRD数据，丙酮基三苯基硝酸磷(1)(C21H20NO4P, FW = 381.35；单斜，空间群С2/；= 14.301 (13), b = 12.756 (11) a, c = 21.40 (2);α= 90.00°,β= 90.66(3)°,γ= 90.00°,V = 3904 (8) A3, Z = 8;ρX = 1.298 g/cm3；偏差= 1.034；R = 0.0631)和反式-2-丁烯-1,4-双（三苯基膦）硝酸二水合物(2)(C40H40N2O8P2, FW = 738.68；三斜，空间群P-1；A = 9.259(7) Å， b = 9.514(6) Å， c = 12.247(9) Å；α= 68.43(4)°,β= 72.47(5)°,γ= 84.06(3)°,V = 956.7 (12) A3, Z = 1;ρX = 1.282 g/cm3；偏差= 1.029；R = 0.0493)具有离子结构，由有机三苯基磷离子组成，磷原子的四面体配位有些扭曲（CPC角在104.99（11）°~ 112.25（12）°和107.61（11）°~ 111.28（11）°之间变化）；P-C距离分别为1.792(3)-1.802 (3)Å和1.792（2)-1.815 (2)Å）和平面三角形硝酸阴离子（ONO角之和分别为359.5°和360°）。硝酸盐1和硝酸盐2的原子坐标、键长和键角的完整表格已存放在剑桥晶体学数据中心(CCDC 2155176 (1), 2335887 (2)；deposit@ccdc.cam.ac.uk;http://www.ccdc.cam.ac.uk)。

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Reactions of Acetonyltriphenylphosphonium and 2-Butene-1,4-bis(triphenylphosphonium) Chlorides with Nitric Acid

Alkyltriphenylphosphonium nitrates [Ph₃PCH₂С(O)Me]NO₃ (1) and [Ph₃PCH₂CH=CHCH₂PPh₃][NO₃]₂ · 2H₂O (2) have been synthesized by reacting, respectively, acetonyl-triphenylphosphonium and trans-2-butene-1,4-bis(triphenylphosphonium) chlorides with nitric acid. The compounds have been characterized by IR spectroscopy and single-crystal X-ray diffraction. According to XRD data, acetonyltriphenylphosphonium nitrate (1) (C₂₁H₂₀NO₄P, FW = 381.35; monoclinic, space group С2/с; a = 14.301(13) Å, b = 12.756(11) Å, c = 21.40(2) Å; α = 90.00°, β = 90.66(3)°, γ = 90.00°, V = 3904(8) Å³, Z = 8; ρ_X = 1.298 g/cm³; GOOF = 1.034; R = 0.0631) and trans-2-butene-1,4-bis(triphenylphosphonium) dinitrate dihydrate (2) (C₄₀H₄₀N₂O₈P₂, FW = 738.68; triclinic, space group P–1; a = 9.259(7) Å, b = 9.514(6) Å, c = 12.247(9) Å; α = 68.43(4)°, β = 72.47(5)°, γ = 84.06(3)°, V = 956.7(12) Å³, Z = 1; ρ_X = 1.282 g/cm³; GOOF = 1.029; R = 0.0493) have ionic structure and consists of organyltriphenylphosphonium cations with a somewhat distorted tetrahedral coordination of the phosphorus atom (the CPC angle vary within 104.99(11)°−112.25(12)° for 1 and 107.61(11)°−111.28(11)° for 2; the P–C distances are 1.792(3)–1.802(3) Å and 1.792(2)–1.815(2) Å, respectively) and planar trigonal nitrate anions (the sums of the ONO angles are 359.5° and 360°, respectively). Complete tables of atomic coordinates and bond lengths and angles of nitrates 1 and 2 have been deposited with the Cambridge Crystallographic Data Centre (CCDC 2155176 (1), 2335887 (2); deposit@ccdc.cam.ac.uk; http://www.ccdc.cam.ac.uk).

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来源期刊

Doklady Chemistry 化学-化学综合

CiteScore

1.20

自引率

12.50%

发文量

审稿时长

6-12 weeks

期刊介绍： Doklady Chemistry is a journal that publishes new research in chemistry and chemical engineering of great significance. Initially the journal was a forum of the Russian Academy of Science and published only best contributions from Russia in the form of short articles. Now the journal welcomes submissions from any country in the English or Russian language. Every manuscript must be recommended by Russian or foreign members of the Russian Academy of Sciences.