Crystal structure of [Pd(NH3)4][Rh(NH3)(NO2)5]

Shusharina, E. A.; Rybinskaya, A. A.; Plyusnin, P. E.; Shubin, Yu. V.; Коренев, С. В.; Gromilov, S. A.

doi:10.1134/s0022476611030255

Cited by 6 publications

(6 citation statements)

References 5 publications

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“…In [9], for the corresponding anion, the following values were obtained: Pd-N(NO 2 ) 1.984 Å, Pd-N(NH 3 ) 2.034-2.053 Å; in the neutral trans-[Pd(NH 3 ) 3 (NO 2 )] complex, the lengths of these bonds are 2.010 Å and 2.045 Å [23] respectively. The same relation could be observed when comparing the characteristics of tetranitrite and tetrammine cations [see, e.g., 6,7,24,25]. The palladium atom is by 0.019 Å out of the plane of coordinating it nitrogen atoms; in [9], this value was 0.…”

Section: Results and Discussion Conclusionsupporting

confidence: 62%

“…The Rh-N(NO 2 ) values of 2.033(2)-2.045(2) Å are in good correlation, for example, with the data from[6] for [Pd(NH 3 ) 4 ][Rh(NH 3 )(NO 2 ) 5 ] being 2.020(4)-2.060(3) Å and 2.012(7)-2.034(7) Å [15, 16] for two fac-[Rh(NH 3 ) 3 (NO 2 ) 3 ] modifications. In the hexanitrite Na(NH 4 ) 2 [Rh(NO 2 ) 6 ] complex, this distance is somewhat longer being 2.051(2) Å [17].…”

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confidence: 55%

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Crystal structures of [Pd(NH3)3(NO2)][Rh(NH3)2(NO2)4] and [PdEn2][Rh(NH3)(NO2)5]·0.75H2O

2014

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Section: Results and Discussion Conclusionsupporting

confidence: 62%

supporting

confidence: 55%

Crystal structures of [Pd(NH3)3(NO2)][Rh(NH3)2(NO2)4] and [PdEn2][Rh(NH3)(NO2)5]·0.75H2O

2014

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“…[1][2][3][4] Its interactions with palladium(II) are prominent examples that have been investigated in the context of catalysis as well as in electrochemical processes, 2,[5][6][7][8] however, the majority of experimental investigations have been carried out only with ammonia-containing complexes. [9][10][11][12][13] The only experimental investigation in liquid ammonia was conducted by Rasmussen et al 14 reporting a dissociation rate of Pd(NH 3 ) 4 2+ as 7.8 × 10 −4 s −1 .…”

Section: Introductionmentioning

confidence: 99%

“…Thus, the respective structural properties of Pd 2+ in liquid ammonia remain ambiguous today. The vast majority of experimental investigations report a square-planar coordination geometry, [9][10][11]13,15,16 but a number of studies also highlight the presence of ligands in an axial position with respect to the plane [17][18][19] similar to the aqueous case. 20 Caminiti et al 21 performed EXAFS and LAXS measurements on (NH 4 ) 2 PdCl 4 in aqueous solutions and reported the presence of two axial water molecules at 2.77 Å coordinated to the [PdCl 4 ] 2− complex.…”

Section: Introductionmentioning

confidence: 99%

Palladium(ii) in liquid ammonia: an investigation of structural and dynamical properties by applying quantum mechanical charge field molecular dynamics (QMCF-MD)

Muhammad

Hofer

2017

Dalton Trans.

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The structural and dynamical properties of Pd in liquid ammonia have been investigated via quantum mechanical charge field molecular dynamics. Similar to the case of aqueous Pd, a six-fold coordination polyhedron in the form of a tetrahedrally elongated octahedron is observed with two ligands in axial positions forming an extended first shell. To highlight the difference in solvation between the aqueous and ammonia case a selection based on the angular-radial distribution with respect to the well-known square planar motif was applied also providing a detailed understanding of ligand exchange between the extended first and second shells. All structural properties resulting from this investigation compare well with the available solid-state data of various N-containing complexes. From the dynamical perspective, Pd in liquid ammonia forms a more flexible complex with a higher rate of ligand exchange than that of its aqueous counterpart.

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“…DCS with the stoichiometry [Pd(NH 3 ) 4 ] [Rh(NH 3 )(NO 2 ) 5 ] (IV) was synthesized previously, and its structure was reported in [8]. The work does not mention that the anion is disordered.…”

mentioning

confidence: 99%

Structural study of complex [Rh(NH3)5(NO2)](NO3)2·H2O, [Rh(NH3)5(NO2)][Pd(NO2)4], and K2[Rh(NH3)(NO2)5]·H2O salts

2014

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Original Russian Text © 2014 I. A. Baidina, A. I. Smolentsev, A. V. Belyaev. STRUCTURAL STUDY OF COMPLEX [Rh(NH 3 ) 5 (NO 2 )](NO 3 ) 2 ⋅H 2 O, [Rh(NH 3 ) 5 (NO 2 )][Pd(NO 2 ) 4 ], AND K 2 [Rh(NH 3 )(NO 2 ) 5 ]⋅H 2 O SALTS I. A. Baidina, A. I. Smolentsev, and A. V. Belyaev UDC 546.97′32′36′57:541.486-163.2 Compounds [Rh(NH 3 ) 5 (NO 2 )](NO 3 ) 2 ⋅H 2 O (I) with a = 7.6230(3) Å, b = 7.6230(3) Å, c = 10.3584(4) Å, space group I-42m, Z = 2, d calc = 2.026 g/cm 3 , V = 601.93(4) Å 3 , Rh-NH 3 eq = 2.074 Å, Rh-NH 3 ax (NO 2 ) = 2.048 Å; [Rh(NH 3 ) 5 (NO 2 )][Pd(NO 2 ) 4 ] (II) with a = 8.095(3) Å, b = 22.422(8) Å, c = 7.887(3) Å, β = 98.559 (17)°, space group Cc, Z = 4, d calc = 2.461 g/cm 3 , V = 1415.6(9) Å 3 , Rh-NH 3 eq = 2.069 Å, (14) Å 3 , Rh-NH 3 ax (NO 2 ) = 2.094 Å, Rh-NO 2 eq = 2.030 Å are synthesized and studied using single crystal X-ray diffraction.Some complexes of a series [Rh(NH 3 ) 6-x (NO 2 ) x ] (3+÷3-) were synthesized as long as in the 20th century, but the structural study of the compounds of this series have been started fairly recently [1-3]. Due to their low solubility, the ammino nitrite complexes can be used to yield the target products in the rhodium refining processes. In the class of compounds under consideration, the bonding isomers can form in the synthesis. There is no information on the isomeric composition of the complexes in the literature.The work was devoted to the preparation and structural study of compounds of the series [Rh(NH 3 ) 6-x (NO 2 ) x ] (3+÷3-) with x = 1 and 5. EXPERIMENTAL In order to produce the crystals of [Rh(NH 3 ) 5 (NO 2 )](NO 3 ) 2 ⋅H 2 O (I), to an aqueous solution of [Rh(NH 3 ) 5 (H 2 O)](NO 2 ) 3 obtained using the technique described in [4], a portion of sodium nitrite (molar ratio Rh:NaNO 2 = 1:12) was added; then the solution was concentrated at 70 °C until the crystals began to form. After cooling the system to room temperature, the crystals were filtered off, rinsed with water, then with ethanol, and dried in the air. IR spectrum, cm -1 : ν(N-H) two components 3301÷3228, δ(N-H) 1625, ν(N-O) three components 1410÷1308, δ(N-O) 590, ρ(-NO 2 ), (NH 3 ) 854, 824, ν(Rh-NH 3 ) 475, ν(O-H) 3664. Chemical shifts (CSs, δ) in the 14 N NMR spectra of the saturated aqueous solution, ppm: K 2 NO − 83; 3 NO − 0.56; NH 3 eq 409; NH 3 ax 417.

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Crystal structure of [Pd(NH3)4][Rh(NH3)(NO2)5]

Cited by 6 publications

References 5 publications

Crystal structures of [Pd(NH3)3(NO2)][Rh(NH3)2(NO2)4] and [PdEn2][Rh(NH3)(NO2)5]·0.75H2O

Crystal structures of [Pd(NH3)3(NO2)][Rh(NH3)2(NO2)4] and [PdEn2][Rh(NH3)(NO2)5]·0.75H2O

Palladium(ii) in liquid ammonia: an investigation of structural and dynamical properties by applying quantum mechanical charge field molecular dynamics (QMCF-MD)

Structural study of complex [Rh(NH3)5(NO2)](NO3)2·H2O, [Rh(NH3)5(NO2)][Pd(NO2)4], and K2[Rh(NH3)(NO2)5]·H2O salts

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