首页> 外文期刊>Zeitschrift fur Naturforschung, B. A Journal of Chemical Sciences >Darstellung und spektroskopische Charakterisierung von Methylnitro-closo-hexaboraten sowie Kristallstrukturen von cis-(Ph_4As)_2(B_6H_4(CH_3)(NO_2)), fac-(Ph_4As)_2(B_6H_3(CH_3)(NO_2)_2)CH_3CN und mer-(Ph_4P)_2(B_6H_3(CH_3)(NO_2)_2~c)
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Darstellung und spektroskopische Charakterisierung von Methylnitro-closo-hexaboraten sowie Kristallstrukturen von cis-(Ph_4As)_2(B_6H_4(CH_3)(NO_2)), fac-(Ph_4As)_2(B_6H_3(CH_3)(NO_2)_2)CH_3CN und mer-(Ph_4P)_2(B_6H_3(CH_3)(NO_2)_2~c)

机译:甲基硝基-氯-六硼酸盐的表征和光谱表征以及顺式(Ph_4As)_2(B_6H_4(CH_3)(NO_2)),fac-(Ph_4As)_2(B_6H_3(CH_3)(NO_2)_2)CH_3CN和mer-( Ph_4P)_2(B_6H_3(CH_3)(NO_2)_2〜c)

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摘要

By electrochemical oxidation of (n-Bu_4N)[B_6H_6(CH_3)] in the presence of nitrite ions and of the base DBU in dichloromethane solution cis- and trans-[B_6H_4(CH_3)(NO_2)]~(2-), fac-[B_6H_4(CH_3)(NO_2)_2]~(2-) and mer-[B_6H_3(CH_3)(NO_2)_2~c]~(2-) are formed. X-ray diffraction analyses have been performed on single crystals of cis-(Ph_4As)_2 [B_6H_4(CH_3)(NO_2)] (1) (mono-clinic, space group P2~1/a, a = 20.063 (2), b = 10.858 (1), c = 21.384 (2) A, #beta# = 105.818 (9) deg, Z = 4), fac-(ph_4As)_2[B_6H_3(CH_3)(NO_2)_2] centre dot CH_3CN (2) (triclinic, space group P1, a = 10.333 (3), b = 10.695 (3), c = 22.833, (6), A, #alpha# = 93.91 (3), #beta# = 96.79 (3), #gamma#=104.56 (2) deg, Z = 2), and mer-(Ph_4P)_2 [B_6H_3(CH_3)(NO_2)_2~c] (3) (triclinic, space group P1, a = 10.100 (1), b = 10.402 (3), c = 22.923 (3), A, #alpha# = 96.328 (18), #beta# = 89.928 (12), #gamma# = 107.963 (16) deg, Z = 2). The ~(11)B NMR spectra and the vibrational spectra of the methylnitro compounds are discussed and compared with those of the monomethyl- and mononitro-closo-hexaborates.
机译:通过在亚硝酸根离子存在下对(n-Bu_4N)[B_6H_6(CH_3)]和碱DBU在二氯甲烷溶液中的顺式和反式[B_6H_4(CH_3)(NO_2)]〜(2-)进行电化学氧化形成-[B_6H_4(CH_3)(NO_2)_2]〜(2-)和mer- [B_6H_3(CH_3)(NO_2)_2〜c]〜(2-)。对cis-(Ph_4As)_2 [B_6H_4(CH_3)(NO_2)](1)(单斜晶系,空间群P2〜1 / a,a = 20.063(2), b = 10.858(1),c = 21.384(2)A,#beta#= 105.818(9)度,Z = 4),fac-(ph_4As)_2 [B_6H_3(CH_3)(NO_2)_2]中心点CH_3CN( 2)(三斜线,空间群P1,a = 10.333(3),b = 10.695(3),c = 22.833,(6),A,#alpha#= 93.91(3),#beta#= 96.79(3) ,#gamma#= 104.56(2)度,Z = 2)和mer-(Ph_4P)_2 [B_6H_3(CH_3)(NO_2)_2〜c](3)(三斜线,空间群P1,a = 10.100(1 ),b = 10.402(3),c = 22.923(3),A,#alpha#= 96.328(18),#beta#= 89.928(12),#gamma#= 107.963(16)度,Z = 2) 。对甲基硝基化合物的〜(11)B NMR光谱和振动光谱进行了讨论,并将其与单甲基-和单硝基-氯-六硼酸盐的振动光谱进行了比较。

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