Fe[S2CN(CHa)2] 3 has a temperature-dependent magnetic moment. Its crystal structure has been determined at 25 and 400 K from X-ray intensities collected with a diffractometer equipped with a Be-walled liquid He The main structural difference between the low-and high-spin complexes is the Fe-S distances: the average length is 2.302 (3) at 25 and 2.415 (4) A at 400 K. The 25 K low-spin complex is the least distorted. The average apparent decrease in bond lengths between non-H atoms in the planar ligands is only 0.011 (3) A when the temperature rises from 25 to 400 K. Preliminary ESCA studies indicate a charge redistribution in the complex: the low-spin Fe-S bond is more covalent than the high-spin bond.
Single-crystal neutron diffraction studies have been performed on natural fluorapophyllite at 295 and 373 K, and on partially dehydrated fluorapophyllite (PDFA), KCa4(Si802o)F.7-4H20, at 295 K. Space group P4/mnc, Z=2, a =8.970 (1)
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