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Volumn 46, Issue 22, 2007, Pages 9033-9035

Structure and magnetic ordering of KxH1-xNi(OH 2)4[Ru2(CO3)4] ·zH2O

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EID: 35848931479 PISSN: 00201669 EISSN: None Source Type: Journal
DOI: 10.1021/ic701318q Document Type: Article

Times cited : (25)

References (21)

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- 1 was synthesized in ∼80% yield via 1.5:1 Ni(NO 3)2 (139.9 mg)/K3[Ru2(CO 3)4]·4H2O (200.6 mg) each dissolved in 20 mL of H2O. The anion was added to the stirring solution of Ni II at the rate of 19.8 mL/h using a syringe pump. The initial black precipitate was removed via centrifugation, and the desired product was precipitated with addition of MeOH, washed with MeOH, and dried in a vacuum desiccator with P2O5 overnight. IR (KBr, 1634 νH2O, 1492(s) νCO, 1344 νCO, 1266(s) νCO, 1065(s, 818, 769, and 715 cm-1. Anal. Calcd for HNi(OH2)3.35[Ru2(CO3)4, C4H7.6NiO15.35Ru2: C, 8.54; H, 1.38; N, 0.00; H2O, 10.70; Found: C, 8.34; H, 1.20; N, <0.2; H 2O 10.7% from the T
- 2: C, 8.31; H, 1.51; K, 4.51; Found: C, 8.34; H, 1.44; K, 4.28; N, <0.2.

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- A Si(111) channel-cut monochromator selected a highly collimated incident beam of 0.69667(1) Å on the X16C beamline at National Synchrotron Light Source, BNL. The diffracted X-rays were analyzed by a Ge(111) single-reflection crystal and detected using NaI scintillation counter. The capillary was rotated during data collection for better averaging of the data. TOPAS-Academic was used to index, assign the space group, and solve the structure by the simulated annealing method and subsequent Rietveld refinement. Rigid-body constraints were imported to describe the D4h, Ru dimer, but interatomic distances were refined. Solvent molecules necessary to explain the observed XRPD pattern were observed; we assumed water and oxygen atoms O13-15, however, occupancy and thermal parameter are refined freely; consequently, atom identifications are not meaningful, TOPAS V3: General profile and structure analysis software for powder diffraction data, User's Manual; Bro
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