Synthesis and properties of trans-di(fluoro)phthalocyaninato(2-)rhenate(III); Crystal structure of the linear-bis(triphenylphosphine)iminium double salt (l)(PNP)(trans)[Re(F)(2)pc(2-)].0.33(l)(PNP)F.2H(2)O [German]

Goldner M.; Homborg H.; Huckstadt H.

首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >Synthesis and properties of trans-di(fluoro)phthalocyaninato(2-)rhenate(III); Crystal structure of the linear-bis(triphenylphosphine)iminium double salt (l)(PNP)(trans)[Re(F)(2)pc(2-)].0.33(l)(PNP)F.2H(2)O [German]

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Synthesis and properties of trans-di(fluoro)phthalocyaninato(2-)rhenate(III); Crystal structure of the linear-bis(triphenylphosphine)iminium double salt (l)(PNP)(trans)[Re(F)(2)pc(2-)].0.33(l)(PNP)F.2H(2)O [German]

机译：反式-二（氟）邻苯二甲酰氰基（2-）苯甲酸酯（III）的合成及性能线性双（三苯基膦）亚胺复盐（l）（PNP）（反式）[Re（F）（2）pc（2-）]。0.33（l）（PNP）F.2H（2）的晶体结构O [德语]

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trans-Bis(triphenylphosphine)phthalocyanato (2-)rhenium(II) reacts with ((Bu4N)-Bu-n)F . 3H(2)O in acetone on air yielding trans-di(fluoro)phthalocyaninato(2-)rhenate(III), (trans)[Re(F)(2)pc(2-)](-). The complex anion is precipitated as tetra(n-butyl)ammonium ((Bu4N)-Bu-n), or after addition of (PNP)HSO4 as linear-bis(triphenylphosphine)iminium ((l)(PNP)) salt. The latter crystallizes as a double salt of formula (l)(PNP)(trans)[Re(F)(2)pc(2-)]. 0.33(l)(PNP)F . 2H(2)O in the cubic space group I23 (no.197) with the cell parameter a = 21.836(2) Angstrom; V = 10412(2) Angstrom(3); Z = 6. The Re atom is located in the centre of the (N-iso)(4) plane (N-iso: isoindole-N atom) and coordinates axially two fluorine atoms in a mutual trans position. The Re-N and Re-F distance is 2.035(6) and 1.798(7) Angstrom, respectively. According to the short Re-F distance the asymmetric Re-F stretching vibration is observed in the MIR spectrum at 746 cm(-1). Obviously due to a large spin-orbit coupling, the complex salt with an electronic low-spin d(4) ground state of Re-III (S = 1) is diamagnetic. Hence a sharp signal is observed at -126.1 ppm in the (FNMR)-F-19 spectrum. The UV-VIS-NIR spectrum shows the typical pi-pi* transitions at 15000 (B), 29500 (Q) and 36900 cm(-1) (N) and trip-multiplet transitions at 9500/10500 cm(-1) and 13200/14100 cm(-1). [References: 32]

机译：反式-双（三苯基膦）酞菁（2-）r（II）与（（Bu4N）-Bu-n）F反应。在空气中的丙酮中形成3H（2）O，生成反式-二（氟）邻苯二甲酰氰基（2-）-苯甲酸酯（III），（反式）[Re（F）（2）pc（2-）]（-）。络合阴离子以四（正丁基）铵（（Bu4N）-Bu-n）沉淀，或以线性双（三苯基膦）亚胺（（I）（PNP））盐形式添加（PNP）HSO4后沉淀。后者结晶为式（1）（PNP）（反式）[Re（F）（2）pc（2-）]的复盐。 0.33（l）（PNP）F。单元参数a = 21.836（2）埃的立方空间群I23（编号197）中的2H（2）O; V = 10412（2）埃（3）; Z =6。Re原子位于（N-iso）（4）平面的中心（N-iso：异吲哚-N原子），并在相互反位的位置轴向配位两个氟原子。 Re-N和Re-F距离分别为2.035（6）和1.798（7）埃。根据较短的Re-F距离，在MIR光谱中746 cm（-1）处观察到不对称的Re-F拉伸振动。显然由于大的自旋轨道耦合，具有Re-III（S = 1）的电子低自旋d（4）基态的复合盐是反磁性的。因此，在（FNMR）-F-19光谱中在-126.1ppm处观察到清晰的信号。 UV-VIS-NIR光谱显示在15000（B），29500（Q）和36900 cm（-1）（N）处的典型pi-pi *跃迁以及在9500/10500 cm（-1）和13200/14100厘米（-1）。 [参考：32]

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《Zeitschrift fur Anorganische und Allgemeine Chemie》 |1998年第5期|共5页
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Goldner M.; Homborg H.; Huckstadt H.;
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1. Synthesis and properties of trans-di(fluoro)phthalocyaninato(2-)rhenate(III); Crystal structure of the linear-bis(triphenylphosphine)iminium double salt (l)(PNP)(trans)[Re(F)(2)pc(2-)].0.33(l)(PNP)F.2H(2)O [German] [J] . Goldner M., Homborg H., Huckstadt H. Zeitschrift fur Anorganische und Allgemeine Chemie . 1998,第5期

机译：反式-二（氟）邻苯二甲酰氰基（2-）苯甲酸酯（III）的合成及性能线性双（三苯基膦）亚胺复盐（l）（PNP）（反式）[Re（F）（2）pc（2-）]。0.33（l）（PNP）F.2H（2）的晶体结构O [德语]
2. HIGH INTENSITY TRIP-MULTIPLET TRANSITIONS, A REALITY - SYNTHESIS, PROPERTIES, AND CRYSTAL STRUCTURE OF L-BIS(TRIPHENYLPHOSPHINE)IMINIUM TRANS-DIBROMOPHTHALOCYANINATO(2-)MOLYBDATE(III) [J] . Gorsch M., Huckstadt H., Homborg H., Zeitschrift fur Anorganische und Allgemeine Chemie . 1997,第9期

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6. The Solution Properties of Bis(triphenylphosphine)iminium Salts. III. Osmotic and Activity Coefficients of PNP-salts in Aqueous Solution. [O] . Terje Palmesen, Harald Høiland, Jon Songstad, 1981

机译：双（三苯基膦）亚胺盐的溶液性质。 III。水溶液中PNP -Salts的渗透和活性系数。

Synthesis and properties of trans-di(fluoro)phthalocyaninato(2-)rhenate(III); Crystal structure of the linear-bis(triphenylphosphine)iminium double salt (l)(PNP)(trans)[Re(F)(2)pc(2-)].0.33(l)(PNP)F.2H(2)O [German]

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