Nanoporous Copper Silicates with One‐Dimensional 12‐Ring Channel Systems

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We use the general notation MSH‐nA (Metal Silicate Houston n is the framework type and A is the nonframework cation) to designate this series of compounds. Thus CuSH‐n is used for the copper silicate family.

Elemental analyses (Galbraith Lab. Knoxville TN USA) calcd (%) for CuSH‐1Cs (Na4[Cu2Si12O27(OH)2][(CsOH)(NaOH)(H2O)6]): Cs 10.07 Na 8.71 Cu 9.63 Si 25.53; found: Cs 10.37 Na 8.78 Cu 9.66 Si 25.62. Calcd for CuSH‐1Na (Na4[Cu2Si12O27(OH)2] [(NaOH)2(H2O)6]): H 1.32 Na 11.40 Cu 10.50 Si 27.85; found: H 1.31 Na 11.13 Cu 10.38 Si 27.46

X‐ray single‐crystal analysis for CuSH‐1Na: pale‐blue plate 0.26×0.08×0.01 mm space groupCmcm a=25.578(4) b=13.098(2) c=9.890(1) Å V=3313.4(8) Å3 Z=4. Final R indices (I>2σ(I)):R1=0.0687 wR2=0.1678. For CuSH‐1K: pale‐blue plate 0.24×0.12×0.01 mm space groupCmcm a=25.474(2) b=13.1346(8) c=9.8537(6) Å V=3297.0(3) Å3 Z=4.R1=0.0528 wR2=0.1249. For CuSH‐1Rb: pale‐blue plate 0.30×0.12×0.01 mm space groupCmcm a=25.425(2) b=13.135(1) c=9.9068(7) Å V=3308.4(4) Å3 Z=4.R1=0.0323 wR2=0.0824. For CuSH‐1Cs: pale‐blue plate 0.29×0.11×0.01 mm space groupCmcm a=25.639(7) b=13.142(4) c=9.960(3) Å V=3356(2) Å3 Z=4.R1=0.0410 wR2=0.1059. Intensities were measured on a SMART platform diffractometer equipped with a 1 K CCD area detector using graphite‐monochromated MoKαradiation at 293 K for CuSH‐1Na and at 243 K for the other three phases. The structures were solved by direct methods and refined using the SHELXTL program. All ordered non‐hydrogen atom positions were refined anisotropically in the final refinements. The disordered water oxygen atoms were forced to have an equal but variable displacement parameter in order to refine their relative occupancies. The total amount of observed water is consistent with that measured from TGA measurements and was fixed to the formula based on the TGA data. Further details on the crystal structure investigation may be obtained from the Fachinformationszentrum Karlsruhe 76344 Eggenstein‐Leopoldshafen Germany (fax: (+49) 7247‐808‐666; e‐mail: crysdata@fiz‐karlsruhe.de) on quoting the depository numbers CSD‐412966 ‐412967 ‐412968 ‐412969.

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