SUBSTITUENT AND SOLVENT EFFECTS ON ELECTROCHEMICAL PROPERTIES OF TETRA-MU-CARBOXYLATO-DIRHODIUM(II)
SUBSTITUENT AND SOLVENT EFFECTS ON ELECTROCHEMICAL PROPERTIES OF TETRA-MU-CARBOXYLATO-DIRHODIUM(II)
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DOI：
10.1021/ic50182a027
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发表时间：
1978-01-01
影响因子：
4.6
通讯作者：
BEAR, JL
中科院分区：
文献类型：
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作者：
DAS, K;KADISH, KM;BEAR, JL
铁、10.15。发现：C， 47.81；3.13;N, 12.51;铁、9.93。Fe (salen)(pico), C22H18N3Fe04: C, 59.47；4.09;N, 9.46;铁、12.57。发现：C， 58.16；4.13;N, 9.47;铁、12.08。三氯乙酸和苦味酸与[Fe (TPP)] 20的反应遵循类似的程序。将[Fe (TPP)] 20溶解于氯仿中，使溶液回流。将大量过量的三氯乙酸（水）或苦味酸（95%乙醇）搅拌加入到溶液中。溶液回流搅拌15-30分钟，蒸发至原体积的一半左右。用几个15ml等分的水洗涤氯仿溶液。然后将溶液蒸发以得到所需的化合物。分析的。Fe (TPP)(tea), C46H28N4Fe02Cl3: C, 66.48；3.40;N, 6.74;铁、6.72。发现：C， 64.79；H, 3.46;N, 6.44;铁、6.45。Fe (TPP)(pic), C50H28NvFeO7: C, 67.12；3.16;N, 10.96;铁、6.24。发现：C， 65.74；H, 3.64;N, 10.59;铁、5.99。物理测量。红外光谱记录在珀金-埃尔默467型分光光度计上。样品制备成13mm的KBr微球。低温红外光谱使用Cryogenics Technology， Inc.的“Spectrim”闭式循环氦气制冷机获得，该制冷机配有KBr窗口（50 X4 mm）。采用PAR 150A型振动样品磁强计获得了4.2 ~ 269 K的变温磁化率数据。温度监测与GaAs温度敏感二极管结合CuSo4-5H20标准。电子顺磁共振波谱通过Varían e线谱仪获得。（10公斤）磁铁x波段测量和El 10微波桥与12英寸。（25kg）磁铁用于q波段测量。使用Varían液氮x波段腔插入器在90±10 K下获得测量结果，使用Air Products Heli-tran x波段液氦冷却系统在8±2 K下获得测量结果。x波段测量温度由欧姆特碳电阻（2.7±10% kfi, 1/g W）确定。低温q波段测量值估计在~ 100k，是通过用玻璃杜瓦瓶包围腔体，并通过液氮冷却的气态氮来获得的
Fe, 10.15. Found: C, 47.81;, 3.13; N, 12.51; Fe, 9.93. Caled for Fe (salen)(pico), C22H18N3Fe04: C, 59.47;, 4.09; N, 9.46; Fe, 12.57. Found: C, 58.16;, 4.13; N, 9.47; Fe, 12.08. The reactions of trichloroacetic acid and picric acid with [Fe (TPP)] 20 followed similar procedures.[Fe (TPP)] 20 was dissolved in chloroform and the solution brought to reflux. A large excess of trichloroacetic acid in water or picric acid in 95% ethanol was added to the solution with stirring. The solution was stirred at reflux for 15-30 min and then evaporated to about half of the original volume. Several 15-mL aliquots of H20 were used to wash the chloroform solution. The solution was then evaporated to give the desired compound. Anal. Caled for Fe (TPP)(tea), C46H28N4Fe02Cl3: C, 66.48;, 3.40; N, 6.74; Fe, 6.72. Found: C, 64.79; H, 3.46; N, 6.44; Fe, 6.45. Caled for Fe (TPP)(pic), C50H28NvFeO7: C, 67.12;, 3.16; N, 10.96; Fe, 6.24. Found: C, 65.74; H, 3.64; N, 10.59; Fe, 5.99. Physical Measurements. Infrared spectra were recorded on a Perkin-Elmer Model 467 spectrophotometer. Samples were prepared as 13-mm KBr pellets. Low-temperatureIR spectra were obtained using a Cryogenics Technology, Inc.,“Spectrim" closed-cycle helium gas refrigerator with the cryocooling head equipped with KBr windows (50 X4 mm).Variable-tempera ture (4.2-269 K) magnetic susceptibility data were obtained with a PAR Model 150A vibrating-sample magnetometer. The temperature was monitored with a GaAs temperature-sensitive diode in conjunction with a CuSo4-5H20 standard. Electron paramagnetic resonance spectra were obtained with Varían E-line spectrometers using an E101 microwave bridge with a 6-in.(10 kG) magnet for X-band measurements and an El 10 microwave bridge with a 12-in.(25 kG) magnet for Q-band measurements. A Varían liquid-nitrogen X-band cavity insert was used toobtain measurements at 90±10 K and an Air Products Heli-tran X-band liquid-helium coolingsystem to obtain measurements at 8±2 K. Temperatures for the X-band measurements were determined by employing an Ohmite carbon resistor (2.7±10% kfi, 1/g W). The low-temperature Q-band measurements were estimated to be at~ 100 K and were obtained by surrounding the cavity with a glass Dewar and passing liquid-nitrogen-cooled, gaseous nitrogen through the