Synthesis, spectroscopic and single-crystal structural investigations of several lanthanide hexacyanoruthenate(II) tetrahydrates

Mullica, D. F.; Hayward, Paul K.; Sappenfield, E. L.

doi:10.1016/0020-1693(95)04777-8

Cited by 12 publications

(11 citation statements)

References 15 publications

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“…LaKRu(CN)6 ‚ 4H2O was prepared according to literature methods. 46 Powder X-ray diffraction measurements indicated that trace amounts of K4Ru(CN)6 ‚ 3H2O were present in the LaKRu(CN)6 ‚ 4H2O sample; however, the impurity did not interfere with the NMR analysis as their respective 99 Ru NMR chemical shifts are different.…”

Section: Methodsmentioning

confidence: 98%

Solid-State Ru-99 NMR Spectroscopy: A Useful Tool for Characterizing Prototypal Diamagnetic Ruthenium Compounds

Ooms

Wasylishen

2004

J. Am. Chem. Soc.

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The feasibility of (99)Ru NMR spectroscopy as a tool to characterize solid compounds is demonstrated. Results of the first solid-state (99)Ru NMR investigation of diamagnetic compounds are presented for Ru(NH(3))(6)Cl(2), K(4)Ru(CN)(6). xH(2)O (x = 0, 3), LaKRu(CN)(6), and Ru(3)(CO)(12). The sensitivity of the ruthenium magnetic shielding tensor to subtle changes in the local structure about the ruthenium nucleus is highlighted by comparing the (99)Ru isotropic chemical shift of Ru(NH(3))(6)Cl(2) in aqueous solutions and in the solid state. The narrow isotropic (99)Ru NMR peak observed for solid Ru(NH(3))(6)Cl(2) indicates that this compound is an ideal secondary reference sample for solid-state (99)Ru NMR studies. The isotropic (99)Ru chemical shift, (99)Ru nuclear quadrupolar coupling constant, C(Q), and quadrupolar asymmetry parameter of K(4)Ru(CN)(6). xH(2)O (x = 0, 3) are shown to be sensitive to x. For Ru(3)(CO)(12), the magnetic shielding tensors of each of the three nonequivalent Ru nuclei have spans of 1300-1400 ppm, and the (99)Ru C(Q) values are also similar, 1.36-1.85 MHz, and are surprisingly small given that (99)Ru has a moderate nuclear quadrupole moment. Information about the relative orientation of the Ru magnetic shielding and electric field gradient tensors has been determined for Ru(3)(CO)(12) from experimental (99)Ru NMR spectra as well as quantum chemical calculations.

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Section: Methodsmentioning

confidence: 98%

Solid-State Ru-99 NMR Spectroscopy: A Useful Tool for Characterizing Prototypal Diamagnetic Ruthenium Compounds

Ooms

Wasylishen

2004

J. Am. Chem. Soc.

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“…21,22 The coordinate bonds around the Ru atom are the same within experimental error and consistent with those found in other hexacyanoruthenate(II) containing structures. [24][25][26] A notable feature is the pronounced distortion of the C1a-N1a-Co angle (162.8(8)°) from its ideally linear value. Examination of the crystal packing (ESI Fig S1 †) illustrates that this distortion can be attributed to repulsion between the Co pentaamine fragment and the tetrahedrally coordinated Na atom (which is also coordinated to the cyano ligand through N4a).…”

Section: Physical Methodsmentioning

confidence: 99%

Tuning the metal-to-metal charge transfer energy of cyano-bridged dinuclear complexes

et al. 2004

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“…As a result, the occupancy factors for the zeolitic water molecule and the potassium ion are set at 0.5. The LnKRu(CN)6 series also display a phase transition from the hexagonal form (Mullica, Hayward & Sappenfield, 1996a) to the orthorhombic C-centered structure (Mullica, Hayward & Sappenfield, 1996b). In the orthorhombic lanthanide potassium hexacyanoruthenates, however, the potassium ion and zeolitic water molecules occupy specific crystallographic sites with no disorder.…”

mentioning

confidence: 99%

Gadolinium Potassium Hexacyanoferrate(II) Trihydrate

Mullica¹,

Ward²,

Sappenfield³

1996

Acta Crystallogr C

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Gadolinium potassium hexacyanoferrate(II) trihydrate, GdKFe(CN)6.3H20, crystallizes in the orthorhombic space group Pnma (No. 62). The structure consists of non-linear cyanide bridges linking octahedrally coordinated Fe atoms and eight-coordinate Gd atoms. Cavities within the structure are occupied by potassium and zeolitic water molecules which are within hydrogen-bonding distance of the water molecules bonded to the Gd atoms, GdN6(H20)2. ReferencesAbrahams, S. C., Lissalde, F. & Bernstein, J. L. (1978). J. Chem.Phys. 68, 1926-1935. © 1996 International Union of Crystallography Printed in Great Britain -all rights reserved CommentThe first ferrocyanide containing a lanthanide atom, CeKFe(CN)6, was described by Robinson (1909).

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Synthesis, spectroscopic and single-crystal structural investigations of several lanthanide hexacyanoruthenate(II) tetrahydrates

Cited by 12 publications

References 15 publications

Solid-State Ru-99 NMR Spectroscopy: A Useful Tool for Characterizing Prototypal Diamagnetic Ruthenium Compounds

Solid-State Ru-99 NMR Spectroscopy: A Useful Tool for Characterizing Prototypal Diamagnetic Ruthenium Compounds

Tuning the metal-to-metal charge transfer energy of cyano-bridged dinuclear complexes

Gadolinium Potassium Hexacyanoferrate(II) Trihydrate

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