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Structural and Magnetic Diversity in Tetraalkylammonium Salts of Anionic M[N(CN)2]3- (M = Mn and Ni) Three-Dimensional Coordination Polymers
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    Structural and Magnetic Diversity in Tetraalkylammonium Salts of Anionic M[N(CN)2]3- (M = Mn and Ni) Three-Dimensional Coordination Polymers
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    Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439-4831, and Department of Chemistry and Biochemistry, Eastern Washington University, Cheney, Washington 99004
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    Inorganic Chemistry

    Cite this: Inorg. Chem. 2005, 44, 9, 3194–3202
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    https://doi.org/10.1021/ic0484598
    Published April 2, 2005
    Copyright © 2005 American Chemical Society

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    Tetraalkylammonium cations, (NR4)+ (R = C3H7, C4H9, and C5H11), have been used as templates to form a new family of [M(dca)3]- [M = Mn and Ni; dca = dicyanamide or N(CN)2-] salts. The tetrapropylammonium (TPrA) salts possess a perovskite-type anion structure. (TPrA)[Mn(dca)3] (1) crystallizes in the tetragonal space group P4̄21c, with a = 16.2945(8) Å, c = 17.4321(8) Å, and V = 4628.4(6) Å3 at T = 298 K. At room temperature, (TPrA)[Ni(dca)3] (2) crystallizes in the orthorhombic space group Pnna, with a = 17.171(2) Å, b = 22.992(2) Å, c = 22.750(2) Å, and V = 8981(2) Å3, but undergoes a first-order phase transition within the temperature range 150−220 K to the tetragonal space group P4̄21c, with a = 16.0985(7) Å, c = 17.0287(8) Å, and V = 4413.2(5) Å3 at T = 160 K. At 110 K, 2 returns to the Pnna space group with a = 17.116(2) Å, b = 22.800(3) Å, c = 22.641(3) Å, and V = 8835(3) Å3. The tetrabutylammonium (TBA) salts possess a triple rutile structure. (TBA)[Mn(dca)3] (3) crystallizes in the orthorhombic space group P21212, with a = 16.0107(6) Å, b = 16.0114(6), c = 21.5577(8) Å, and V = 5526.4(5) Å3. (TBA)[Ni(dca)3] (4) also crystallizes in the orthorhombic space group P21212, with a = 15.6842(5) Å, b = 15.6841(6) Å, c = 21.1551(8) Å, and V = 5204.0(5) Å3. The tetrapentylammonium (TPnA) salts crystallize with a LiSbO3 structure type, space group Pnna. Lattice parameters for (TPnA)[Mn(dca)3] (5) are a = 13.2236(6) Å, b = 11.6300(6) Å, c = 20.3176(9) Å, and V = 3124.6(4) Å3, and for (TPnA)[Ni(dca)3] (6), a = 12.9380(4) Å, b = 11.6233(4) Å, c = 19.8038(7) Å, and V = 2978.1(2) Å3. Long-range antiferromagnetic ordering has been observed in the manganese salts below 2.1 K, as indicated by alternating current susceptibility measurements. Magnetic susceptibility data for the nickel salts do not show evidence for long-range magnetic ordering but can be described using an S = 1 zero-field splitting model with the exchange Hamiltonian ℋ = −JSiSi+1 + D∑( )2 + gμβBSi, giving |D|/kB values that range between 1.98(1) K and 3.20(2) K.

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     Author to whom correspondence should be addressed. E-mail:  [email protected].

     Argonne National Laboratory.

     Eastern Washington University.

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    X-ray crystallographic details, including selected bond lengths and angles, in CIF format, thermal ellipsoid plots with atom labeling for compounds 16, a plot of the unit cell parameters for 1 as a function of temperature, and infrared spectroscopy data. This material is available free of charge via the Internet at http://pubs.acs.org.

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    Inorganic Chemistry

    Cite this: Inorg. Chem. 2005, 44, 9, 3194–3202
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    https://doi.org/10.1021/ic0484598
    Published April 2, 2005
    Copyright © 2005 American Chemical Society

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