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19944406698
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note
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2 (1:1.2 molar ratio) were mixed under argon atmosphere, sealed in a quartz ampule, and heated to 600 °C for 3 days. The green MnNCN compound is rather inert in air and can be washed using ordinary water. Suitable crystals for single-crystal diffraction were obtained by the same reaction but using 2.0 g of LiBr as a solvent at 650 °C. According to atomic absorption spectroscopy, crystalline samples still exhibit very small Zn contaminations (with Zn presumably replacing Mn), and this is in accord with precise magnetic measurements (see text). The product is entirely free of Li and Br. The powder X-ray diffraction diagram is single-phase, and all reflections perfectly coincide with the single-crystal result.
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33
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note
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2 = 0.059 using anisotropic displacement parameters for all atoms; Mn on 3a, C on 3b, N on 6c with z = 0.5855(3). Additional structural details may be obtained from FIZ Karlsruhe, 76344 Eggenstein-Leopoldshafen (Germany), on quoting the depository number CSD-415019.
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36
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note
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The minute elongation of the central C atom (see Figure 2) is due to a regular atomic vibration but not a split position below and above the 3b site, in full accord with the infrared data. The corresponding (but less stable) split refinement results in a z coordinate of 0.495(8) instead of the correct 1/2 and is characterized by significantly worse residual values.
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