Novel 1-D Coordination Polymers Containing μ-[N(CN)₂]- Bridging Ligands. Structure and Magnetic Properties of Mn[N(CN)₂]₂L (L = 2,2′-Bipyridine, 4,4′-Bipyridine)

References

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• (a) Mn[N(CN)2]2(2,2′-bipy), 1. A 5-mL, aqueous solution of MnCl2·4H2O (1.36 mmol, 0.2686 g) was added slowly to a stirring 15 mL H2O/EtOH solvent mixture containing Na[N(CN)2] (2.71 mmol, 0.2413 g) and 2,2′-bipyridine (1.35 mmol, 0.2115 g). A yellow microcrystalline powder precipitated immediately and was collected via vacuum filtration and dried in vacuo over P2O5 (0.4187 g, 89 %). μCN (Nujol): 2414 w, 2304 m, 2232 m, 2205 s, and 2169 S cm−1. Anal. Calc'd for C14H8N8Mn: C, 48.99; H, 2.34; N, 32.65. Found: C, 48.90; H, 2.31; N, 32.73. (b) Mn[N(CN)2]2(4,4′-bipy)·3/2H2O, 2. A 5 mL aqueous solution of MnCl2·4H2O (1.42 mmol, 0.2818 g) was added slowly to a stirring 10 mL H2O/Me2CO solvent mixture containing Na[N(CN)2] (2.87 mmol, 0.2558 g) and 4,4′-bipyridine (1.43 mmol, 0.2226 g). A pale peach microcrystalline powder precipitated immediately and was collected via vacuum filtration and dried in vacuo over P2O5 (0.4577 g, 94 %). μCN (Nujol): 2415 w, 2303 m, 2242 m, and 2178 S cm−1. Anal. Calc'd for C28H22N16O3Mn2: C, 45.42; H, 2.99; N, 30.27. Found: C, 45.40; H, 2.98; N, 30.18.
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• (a) Crystal Data for C14H8MnN8 1: M = 343.22, monoclinic C2/c a= 6.6769(3) Å, b= 17.2008(2) Å, c= 13.0142(4) Å, β= 90.110 (2)[ddot], U = 1494.65(8) Å3, Z = 4, D c = 1.525 Mg/m3, μ(Mo-Kα) = 0.895 mm−1 T= 173 (2) K. The data was collected on a standard Siemens P4/CCD diffractometer. Of 3096 data (4 < 2θ < ltm 52[ddot]), 1343 were independent (Rint = 0.0364), and 692 were observed [I > 2σ(I)]. The structure was solved by direct methods and refined using the Siemens SHELXTL© (Version 5.0) Software Package. All nonhydrogen atoms were refined anisotropically and hydrogen atoms were treated as idealized contributions, R(F) = 0.0514, R(wF) = 0.1218, GOF= 1.742. The X-ray data was deposited with the Cambridge Crystallographic Data Centre as supplementary publication no, CCDC-102608. Copies of the data can be obtained free of charge upon application to CCDC, 12 Union Road, Cambridge CB2 1EZ [fax: (+44) 1223–336–033; email [email protected]]. (b) Crystal Data for C28H22N16O3Mn2, 2: M = 740.50, orthorhombic Iba2, a = 22.378(6) Å, b = 22.517(5) Å, c= 13.519(5) Å, U = 6812(3) Å3, Z= 8, D c = 1.444 Mg/m3, μ(Mo-Kα) = 0.797 mm−1, T= 291 (2) K. The data was collected on a standard Enraf-Nonius CAD4 automated diffractometer. Of 3135 data (5 < 2θ < 50[ddot]), 3135 were independent (Rint = 0.0000), and 3008 were observed [I > 2σ(I)]. The structure was solved by direct methods and refined using the Siemens SHELXTL97© Software Package. Disordered water molecules with O(1), 0(2), O(1)′ and O(2)′ atoms were refined as 0.5 occupancy each. All nonhydrogen atoms were refined anisotropically and hydrogen atoms were treated as idealized contributions, R(F) = 0.0384, R(wF) = 0.0861, GOF = 1.033. All illustrations were drawn with Crystal Maker©.
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