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Ge2H2NaOioSm3, monoclinic, C12/cl (No. 15), a = 18.323(3)Â, b = 5.2369(8)À, c = 12.108(2)Â,yS= 131.230(2)°, V = 873.8À, Ζ = 4, Rgi(F) = 0.037, wR^F 1 ) = 0.010, T= 153 Κ. Source of material Yellow crystals of NaSm3(Ge04)2(OH)2 were obtained from a hydrothermal reaction of0.035 g (0.10 mmol) S1112O3 and 0.020 g (0.20 mmol) Ge02 in 0.4 mL of NaOH (10.5 M) solution sealed in a silver tube that was heated at 797 Κ for 3 days. Discussion Hydrothermal methods have been used successfully to synthesize many compounds [ 1,2]. The title compound was first synthesized in [3,4]., and the structure was described in the noncentrosymmetric space group Cc. However, we believed that the space group determination was not right based on the position of the atoms. In addition, a review article by Demianets gives the space group as Illa for the same compound, but they did not give any explanation or new characterization [5]. Table 3. Atomic coordinates and displacement parameters (in Â). Our X-ray single crystal structure determination of the compound was done with a final reliability factor R = 0.037 and space group was determined as Clic. The hydrogen atoms were not localized. This structure has an olivine type chain parallel to α-axis [6]. The cation polyhedral chain is made up with alternation Na and Sm polyhedra. There are two crystallographically independent Sm atoms. The Sm 1 is coordinated by eight oxygen atoms and Sm2 is coordinated by seven oxygen atoms in an irregular polyhedron. The Sm 1 —O distances range from 2.359(5) Â to 2.644(5) Â. The Sm2—O distances range from 2.353(5) Â to 2.507(5) À. The Ge atom has four coordinating oxygen atoms forming a distorted tetrahedron. The Ge—O distances range from 1.741(5) Â to 1.786(5) À. Table i . Data collection and handling. Crystal: yellow block, size 0.058 χ 0.118 χ 0.150 mm Wavelength: Mo Ka radiation (0.71073 Â) μ· 267.36 cm" 1 Diffractometer, scan mode: Broker SMARTCCD, Δω = 0.3° 20max* 57.62° WAWJmeasured, N(hkl)miqm· 3997, 1023 Criterion for /obs, N(hkl)gc. /obs > 2 a(Iobs), 970 N(param)K nn«j: 78 Programs: SHELXS-97 [7], SHELXL-97 [8] Table 2. Atomic coordinates and displacement parameters (in Â). Atom Site Occ. χ y ζ {/¡» Na(l) 8 / 0.23 0.247(3) 0.246(7) 0.509(4) 0.006(4) Na(2) 8 / 0.27 0.264(1) 0.295(3) 0.480(2) 0.006 Atom Site χ y ζ U\\ C/22 Í/33 Un t/13 C/23 Sm(l) 4e 0 0.29016(9) 1/4 0.0066(3) 0.0027(3) 0.0031(3) 0 0.0039(3) 0 Sm(2) 8 / 0.11829(2) 0.29557(7) 0.08559(4) 0.0070(3) 0.0047(3) 0.0029(3) 0.0013(1) 0.0035(2) 0.0000(1) Ge(l) 8 / 0.14042(5) 0.7395(1) 0.29168(8) 0.0077(4) 0.0028(4) 0.0045(4) -0.0004(2) 0.0048(4) -0.0005(2) 0(1) 8 / 0.1258(3) 0.0696(9) 0.2718(5) 0.008(2) 0.001(2) 0.004(2) -0.001(2) 0.003(2) -0.000(2) 0(2) 8 / 0.1503(3) 0.5952(9) 0.4316(5) 0.011(2) 0.006(2) 0.006(2) -0.002(2) 0.007(2) -0.002(2) 0(3) 8 / 0.2233(3) 0.615(1) 0.2779(5) 0.008(2) 0.006(2) 0.013(2) 0.001(2) 0.008(2) 0.001(2) 0(4) 8 / 0.0339(4) 0.5799(9) 0.1375(5) 0.009(2) 0.005(2) 0.003(2) -0.001(2) 0.004(2) -0.001(2) 0(5) 8 / 0.0876(4) -0.118(1) -0.0127(5) 0.015(2) 0.006(2) 0.006(2) -0.002(2) 0.007(2) -0.002(2) * (e-mail: emirdag@likya.iyte.edu.tr) 18 NaSm3(Ge04)2(OH)2 Acknowledgments. We gratefully acknowledge help from Clemson University and Dr. Joseph Kolis.

Redetermination of the crystal structure of sodium trisamarium digermanate dihydroxide, NaSm 3 (GeO 4 ) 2 (OH) 2