Mössbauer study of the vibrational anisotropy and of the light-induced population of metastable states in single-crystalline guanidinium nitroprusside

Rusanov, V.; Winkler, H.; Ober, C.; Trautwein, Alfred X.

doi:10.1007/s100510050995

Cited by 13 publications

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“…The Mo È ssbauer spectrum shows the expected doublet ( Figure 2). Guanidinium nitroprusside (GNP) was prepared from sodium nitroprusside by twofold cation exchange via the silver nitroprusside [11]. Upon addition of silver nitrate to a solution of sodium nitroprusside, the colorless silver nitroprusside precipitates and, thus, can easily be separated from the soluble sodium nitrate byproduct (eq.…”

Section: Resultsmentioning

confidence: 99%

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Synthesis of Isotope Enriched (CN ₃ H ₆ ) ₂ [ ⁵⁷ Fe(CN) ₅ NO] starting from ⁵⁷ Fe

Janiak

Dorn

Paulsen

et al. 2001

Z. anorg. allg. Chem.

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A high-yield, mmolar-scale synthesis of pure guanidinium nitroprusside, (CN 3 H 6 ) 2 [ (57) Fe(CN) 5 NO] (GNP) from iron metal is described. The iron metal contained pieces of 95.3% 57 Fe together with normal iron so that an isotope enrichment in 57 Fe of 25% was achieved. Single-crystals of GNP could be grown in cubic shape and dimensions of about 3´4´4 mm 3 . The purity of the GNP product and the intermediates K 4 [ (57) Fe(CN) 6 ]´3 H 2 O and Na 2 [ (57) Fe-(CN) 5 NO]´2 H 2 O was ascertained by 57 Fe Mo È ssbauer spectroscopy as well as 13 C, 14 N and 57 Fe NMR spectroscopy. The 57 Fe NMR chemical shift for [ (57) Fe(CN) 5 NO] 2± in GNP was detected at +2004.0 ppm [vs Fe(CO) 5 ]. Synthese von Isotopen-angereichertem (CN 3 H 6 ) 2 [ 57 Fe(CN) 5 NO] ausgehend von 57 Fe Inhaltsu È bersicht. Es wird eine Synthese mit hoher Ausbeute und im mmol-Bereich von reinem Guanidiniumnitroprussiat, (CN 3 H 6 ) 2 [ (57) Fe(CN) 5 NO] (GNP) ausgehend von Eisenmetall beschrieben. Das Eisenmetall enthielt Stu È cke von 95.3%-igem 57 Fe und normales Eisen, so dass eine Isotopenanreicherung in 57 Fe von 25% erreicht wurde. Einkristalle von GNP konnten als Quader mit Abmessungen von etwa 3´4´4 mm 3 gezu È chtet werden. Die Reinheit des GNP-Produktes und der Zwischenprodukte K 4 [ (57) Fe(CN) 6 ]´3 H 2 O und Na 2 [ (57) Fe(CN) 5 NO]´2 H 2 O wurde mittels 57 Fe Mo È ssbauer Spektroskopie und fu È r K 4 [ (57) Fe(CN) 6 ]´3 H 2 O auch mit 13 C, 14 N and 57 Fe NMR Spektroskopie u È berpru È ft. Die 57 Fe NMR chemische Verschiebung fu È r [ (57) Fe(CN) 5 NO] 2± in GNP wurde bei +2004.0 ppm [vs Fe(CO) 5 ] detektiert.

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Section: Resultsmentioning

confidence: 99%

“…GNP is a standard material for such investigations [9]. GNP offers the advantage over other nitrosyl complexes that all Fe±N±O axes are oriented nearly parallel in its crystalline state [10,11].…”

Section: Introductionmentioning

confidence: 99%

Synthesis of Isotope Enriched (CN ₃ H ₆ ) ₂ [ ⁵⁷ Fe(CN) ₅ NO] starting from ⁵⁷ Fe

Janiak

Dorn

Paulsen

et al. 2001

Z. anorg. allg. Chem.

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“…In a guanidinium nitroprusside monocrystal the symmetry axes of all nitroprusside anions are approximately parallel. This allowed to be gained information about the anisotropy of the molecular vibrations [48]. For the comparison of measured and simulated NIS spectra, the normalized probability density of absorption S(E,k) defined in equation ( 3) has been plotted (Fig.…”

Section: Spin Crossover Complexesmentioning

confidence: 99%

Mössbauer studies of coordination compounds using synchrotron radiation

Paulsen¹,

Schünemann²,

Trautwein³

et al. 2005

Coordination Chemistry Reviews

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“…(1) Woike geometry, the vibrational frequencies, and the electric field gradient (efg) at the nuclear positions for the ground state (GS), MS 1 , and MS 2 could be retrieved and compared with experimental data gained by Mo ¨ssbauer spectroscopy, 1,2 IR and Raman spectroscopy, 1 and X-ray diffraction. 3,7 Additional information has been gained by investigating experimentally and theoretically the shift of vibrational frequencies upon isotope substitution ( 15 NO, 54 Fe, 18 O). 11,12 In general, there is good agreement between the calculated and the measured quantities.…”

Section: Introductionmentioning

confidence: 99%

“…This allows information to be gained about the anisotropy of the molecular vibrations. 16,18 (ii) It has been demonstrated in a conventional Mo ¨ssbauer experiment that due to the alignment of the molecular axes a population of metastable states up to 26% could be achieved by using light emitting diodes (LEDs) instead of a laser, 18 which considerably simplifies the experimental setup at the synchrotron beamline.…”

Section: Introductionmentioning

confidence: 99%

Metastable Isonitrosyl Structure of the Nitroprusside Anion Confirmed by Nuclear Inelastic Scattering

et al. 2002

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Nuclear inelastic scattering (NIS) measurements were performed on a guanidium nitroprusside ((CN(3)H(6))(2)[Fe(CN)(5)NO], GNP) monocrystal at 77 K after the sample was illuminated with blue light (450 nm) at 50 K to populate the two metastable states, MS(1) and MS(2), of the nitroprusside anion. A second measurement was performed at 77 K after warming up the illuminated crystal to 250 K where the metastable states decay to the groundstate. The measured spectra were compared with simulated NIS spectra that were calculated by using density functional methods. Comparison of measured and simulated spectra provides strong evidence for the isonitrosyl structure of the metastable MS(1) state proposed by Carducci et al. (Carducci, M. D.; Pressprich, M. R.; Coppens, P. J. Am. Chem. Soc. 1997, 119, 2669-2678).

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Mössbauer study of the vibrational anisotropy and of the light-induced population of metastable states in single-crystalline guanidinium nitroprusside

Cited by 13 publications

References 0 publications

Synthesis of Isotope Enriched (CN ₃ H ₆ ) ₂ [ ⁵⁷ Fe(CN) ₅ NO] starting from ⁵⁷ Fe

Synthesis of Isotope Enriched (CN ₃ H ₆ ) ₂ [ ⁵⁷ Fe(CN) ₅ NO] starting from ⁵⁷ Fe

Mössbauer studies of coordination compounds using synchrotron radiation

Metastable Isonitrosyl Structure of the Nitroprusside Anion Confirmed by Nuclear Inelastic Scattering

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Mössbauer study of the vibrational anisotropy and of the light-induced population of metastable states in single-crystalline guanidinium nitroprusside

Cited by 13 publications

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Synthesis of Isotope Enriched (CN 3 H 6 ) 2 [ 57 Fe(CN) 5 NO] starting from 57 Fe

Synthesis of Isotope Enriched (CN 3 H 6 ) 2 [ 57 Fe(CN) 5 NO] starting from 57 Fe

Mössbauer studies of coordination compounds using synchrotron radiation

Metastable Isonitrosyl Structure of the Nitroprusside Anion Confirmed by Nuclear Inelastic Scattering

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Synthesis of Isotope Enriched (CN ₃ H ₆ ) ₂ [ ⁵⁷ Fe(CN) ₅ NO] starting from ⁵⁷ Fe

Synthesis of Isotope Enriched (CN ₃ H ₆ ) ₂ [ ⁵⁷ Fe(CN) ₅ NO] starting from ⁵⁷ Fe