Showing papers in "Zeitschrift Fur Kristallographie-new Crystal Structures in 2003"

Crystal structure of di[potassium([2.2.2]crypt)]tetrapotassium octadecagermanide(6-)–ethylenediamine solvate (1:6), [K(C18H36N2O6)]2K4(Ge9)2 · 6C2N2H8

Abstract: Abstract C24H60Ge9K3N8O6, triclinic, P1̅ (No. 2), a = 9.408(2) Å, b = 13.606(3) Å, c = 19.507(4) Å, α = 84.74(3)°, β = 81.35(3)°, γ = 80.18(3)°, V = 2426.8 Å3, Z = 2, Rgt(F) = 0.064, wRref(F2) = 0.192, T = 150 K.

Reinvestigation of the crystal structure of barium aluminum borate difluoride, BaAlBO3F2, a new nonlinear optical material

Abstract: AlBBaF 2 O 3 , hexagonal, P6 (No. 174), a = 4.8879(6) A, c = 9.403(1) A, V = 194.5 A 3 , Z = 2, R gt (F) = 0.024, wR obs (F 2 ) = 0.036, T = 296K.

Crystal structure of 4,7-dibromo-2,1,3-benzothiadiazole, C6H2Br2N2S

Abstract: C6H2Br2N2S, monoclinic, Plhkl (No. 14), a = 18.3670(9) Â, b = 3.9522(2)Á, c = 22.120(2)λ,β = 97.390(6)°, V= 1592.4Â, Z = 8, Rgi(F) = 0.045, wRrei(F) = 0.127, T= 296 K. Source of material The title compound was synthesized by bromination of 2,1,3benzothiadiazole in 47% HBr [1]. Pale yellow crystals suitable for X-ray analysis were grown from a dichloromethane solution. Discussion The title compound crystallizes with two crystallographically independent molecules in the asymmetric unit. The geometric parameters of the 1,2,5-thiadiazole rings are almost same with those of 3,4-diphenyl-l ,2,5-thiadiazole [2], The considerable shortenings of the CI— C6, C4—C5, C7—C12 and C10—Cl 1 bonds are observed. Such double bond fixation suggests the quinonoid character of the 2,1,3-benzothiadiazole ring. Short S—N and Br· Br intermolecular heteroatom contacts are found in the crystal. The S N [3.226(4) Â for S l N l (-x+1, -y+1, -ζ) and 3.238(4) À for S2-N4(-x+2, y+l/2, -z+1/2)] and the distances B r B r [3.542(1) ÂforBrl -Br3(-x+l , ;yl /2 , -z+1/2) and 3.662(1) Â for Br2-Br4(-x+2, y-l/2, -z+1/2)] are 3.4% 3.7% and 1.0% 4.3% shorter than the sum of the corresponding van der Waals radii [3], respectively. Although a planar I4 square cluster via the short intermolecular I—I contacts was formed in the crystal of 4,7-diiodo-2,l,3-benzothiadiazole [4], no Br4 square clusters exist in the structure of the title compound. Table 1. Data collection and handling. Crystal: pale yellow plate, size 0.05x0.10x0.60 mm Wavelength: Cu Ka radiation (1.54178 Â) μ· 147.99 cnT Diffractometer, scan mode: Em-af-Nonius CAD4, ω/2θ 2f/max: 148.44° N(hkl)measureà, N(hkl)unique: 3313,3219 Criterion for 70bs, N(hkl)gt: /obs > 2 ö(/obs), 2772 N(param)TefmtA'· 216 Programs: TeXsan [5], SHELXS-97 [6], SHELXL-97 [7], ORTEP-III [8] Table 2. Atomic coordinates and displacement parameters (in Â). Atom Site X y ζ fiso H(5) Ae 0.722(4) -0.36(2) 0.204(3) 0.10(2) H(6) 4e 0.615(4) -0.17(2) 0.224(3) 0.07(2) H(ll) 4e 0.891(4) -0.26(1) 0.472(3) 0.07(2) H(12) 4e 0.776(3) -0.11(1) 0.451(2) 0.05(1) * Correspondence author (e-mail: tomura@ims.ac.jp)

Crystal structure of Tutton′s salts,Rb2[Mn(H2O)6](SeO4)2,MnII=Mg,Co,Mn,Zn

Abstract: Hi2MgOi4Rb2Se2, monoclinic, P 1 2 i M (No. 14), a = 9.401(1) À, b = 12.658(2) Â, c = 6.339(1) λ,β= 105.25(1)°, V= 727.8 À , Z= 2, Rg,(F) = 0.020, wRTef(F) = 0.040, T= 293 K. CoHi2Oi4Rb2Se2, monoclinic, P 1 2 i M (No. 14), a = 9.363(1)Â, b= 12 .618(1)k ,c = 6 . 3 5 6 2 ( 7 ) Á , β = 105.238(9)°, V = 7 2 4 . 5 Â 3 , Z= 2, Rgl(F) = 0.018, wRKi(F) = 0.037, Γ = 293 Κ. Hi2MnOi4Rb2Se2, monoclinic, P12i /al (No. 14), a = 9.4496(8) Â, b= 12.760(1) A, c = 6.3794(7) λ,β= 105.189(7)°, V= 742.4 Â , Z= 2, RgfF) = 0.025, wRlei(F) = 0.056, Τ = 293 Κ. Hi20i4Rb2Se2Zn, monoclinic, P12 i / a l (No. 14), a = 9.352(1) À, b = 12.626(2) Â, c = 6.360(1) λ, β = 105.195(8)°, V = 724.7 Á , z = 2, Rgt(F) = 0.024, wRTei(F) = 0.048, 7 = 293 K. Source of material All compounds of the isomorphous series Rb 2 [M n (H 20)ô](Se04) 2 ( M n = Mg, Mn, Co, Zn) were prepared by dissolution of equimolar amounts of rubidium selenate Rb 2 Se04 and M-selenate-hydrate M n S e 0 4 · n H 2 0 in hot destilled water and ensuing evaporation of the solvent H 2 0 . The M-selenate-hydrates contained different amounts of crystal water. For the syntheses of the Tutton's salts with M n = Mg, Co, Zn, the M-selenate-hexahydrates, and for M n = Mn, the Mn(EI)-selenate-pentahydrate was used. Differently coloured, in most cases ideomorphous single crystals of dimensions up to 10 mm were obtained. Discussion The structure is characterized by irregular RbOs polyhedra (d(Rb-O) = 2.881(2) Â 3.384(4) À) and M n ( H 2 0 ) 6 octahedra (<¿(M-0) = 2.030(2) Â 2 . 2 0 3 ( 3 ) À), the latter being linked to SeC>4 tetrahedra by hydrogen bonds. Compared to the isotypic sulfates [1], and the own structure analyses of Tutton's salts of the same isomorphous series with M n = Ni, Cu, found in excellent agreement with [2], one finds: 1. The lattice constants increase, a and c by about 1.9%, b by about 1.5%, due to the larger volume of the (SeC>4)~ anion [3]. The ratio of the TO4 volumes (T = S, Se), V(Se04)/V(S04) = 1.37, is in perfect agreement with the ratio of the Se—O and S—O bond lengths, d(Se—0)/d(S—O) = 1.111. The angle β decreases for all compounds by about 0.8°. With respect to the exchange of M n , the linear correlations between the different lattice constants and the cation radii exhibit the same slope. 2. The volumes of the MC>6 coordination octahedra agree with those of the sulfates. 3. The volumes of the RbOs coordination polyhedra increase by 4.4%. 4. While, in agreement with chemical expectation, the selenate group is practically invariant against the M cation exchange in the hexahydrate complex, the volumes of both the MC>6 and RbOs coordination polyhedra increase as the cation radius R(M n ) [4] increases. However, for V(Rb08), the rate of increase is about three times smaller than for V(M n 0 6 ) . 5. a, b and V(RbOs) of the Mg compound are, as in the sulfate series and in [5] significantly larger than expected from the linear lattice constant correlations observed for the other structures. This finding can be attributed to the smaller electronegativitiy of Mg, causing a somewhat weaker electrostatic R b 0 interaction, as reflected by increased distances d(Rb—05) = 3.263(3) A and ¿ ( R b — 0 6 ) = 3.185(2) A. 6. For the individual selenate compounds, the respective distributions of the hydrogen bonds differ f rom those observed in the sulfates, but no significant differences are found for the mean distances ¿¿(0-Η···0). Correspondence author (e-mail: h.euler@uni-bonn.de)

Crystal structure of Tutton's salts, Rb2[MII(H2O)6](SO4)2, MII = Mg, Mn, Fe, Co, Ni, Zn

Abstract: H12MgO14Se2Tl2, monoclinic, P121/a1 (no. 14), a = 9.434(2) Å, b = 12.634(2) Å, c = 6.292(1) Å, / = 105.72(2)°, V = 721.9 Å, Z = 2, Rgt(F) = 0.028, wRref(F ) = 0.047, T = 295 K. H12MnO14Se2Tl2, monoclinic, P121/a1 (no. 14), a = 9.490(1) Å, b = 12.734(2) Å, c = 6.332(1) Å, / = 105.57(1)°, V = 737.1 Å, Z = 2, Rgt(F) = 0.032, wRref(F ) = 0.068, T = 295 K. H12CoO14Se2Tl2, monoclinic, P121/a1 (no. 14), a = 9.387(2) Å, b = 12.600(2) Å, c = 6.308(2) Å, / = 105.70(2)°, V = 718.3 Å, Z = 2, Rgt(F) = 0.036, wRref(F ) = 0.082, T = 295 K. H12NiO14Se2Tl2, monoclinic, P121/a1 (no. 14), a = 9.334(1) Å, b = 12.572(2) Å, c = 6.298(1) Å, / = 105.70(1)°, V = 711.5 Å, Z = 2, Rgt(F) = 0.031, wRref(F ) = 0.051, T = 295 K. H12CuO14Se2Tl2, monoclinic, P121/a1 (no. 14), a = 9.400(2) Å, b = 12.539(2) Å, c = 6.315(1) Å, / = 105.01(2)°, V = 718.9 Å, Z = 2, Rgt(F) = 0.028, wRref(F ) = 0.055, T = 295 K. H12O14Se2TlZn2, monoclinic, P121/a1 (no. 14), a = 9.383(1) Å, b = 12.612(2) Å, c = 6.317(1) Å, / = 105.59(1)°, V = 720.1 Å, Z = 2, Rgt(F) = 0.027, wRref(F ) = 0.054, T = 295 K. Source of material The synthesis of all title compounds of the probably isomorphous series Tl2[M(H2O)6](SeO4)2 was performed by dissolution of equimolar amounts of thallium selenate Tl2SeO4 and M selenate hydrate MSeO4.·.nH2O in hot destilled water and ensuing evaporation of the solvent. The M selenate hydrates contained different amounts of crystal water. For the syntheses of the Tutton’s salts with M = Mg, Co, Ni, Cu, Zn, the M selenate hexahydrates were used, for M = Mn, the M selenate pentahydrate. Differently coloured, mostly ideomorphous single crystals of dimensions up to 10 mm were obtained. Experimental details To reduce errors introduced by insufficient corrections of absorption effects, it was attempted to grind a crystal sphere in order to apply a spherical absorption correction in the course of data processing. The grinding produced an ellipsoid, whose deviation from spherical is characterized by the given max, mid and min crystal dimensions. Discussion The so far unknown crystal structures of the compounds of the thallium selenates, constituting one more important series in our studies of crystal chemistry, metal-water interaction and hydrogen bonds in Tutton salts (Rb sulfates [1], Rb selenates [2], Cs sulfates [3], Cs selenates [4], K sulfates [5], K selenates [6], Tl sulfates [7]) by single crystal and powder X-ray diffraction experiments. As all other Tutton salts, they are isotypic. Due to scattering power of Tl and data errors introduced by insufficient correction for the large absorption, the hydrogen positions could not be determined by difference Fourier mapping, as done in [16]. Therefore, all hydrogen coordinates were calculated from the linear correlations x(H(i)), y(H(i)), z(H(i)), i = 1...6 vs the cation radius R(M) (M = K, Rb, Cs), derived for each of the 6 independend hydrogen bonds of the so far studied compounds. The evaluation of the O#H···O bond lengths and angles yielded resonable hydrogen coordinates. During the structure refinements, these predicted hydrogen coordinates were kept fixed, contrary to a common variable isotropic thermal displacement parameter, assigned to all hydrogens atoms. In all cases, the agreement indices were significantly lowered by introducing the H atoms into the model, for example R1(M = Mg) = 0.0284 to R1 (M = Mg) = 0.0302. The Tutton salt structure is characterized by irregular MO8 polyhedral (here with M = Tl), d(Tl—O) = 2.796(5) 3.362(5) Å, and M(H2O)6 octahedra, which are linked to the SeO4 groups by a system of hydrogen bonds. According to expectations, the most distorted M(H2O)6 octahedron is obtained for M = Cu (Jahn-Teller distortion) with 360 Z. Kristallogr. NCS 224 (2009) 360-364 / DOI 10.1524/ncrs.2009.0158 © by Oldenbourg Wissenschaftsverlag, München

Crystal structure of Tutton’s salts, Rb2[MII(H2O)6](SeO4)2, MII = Mg, Co, Mn, Zn

Abstract: Abstract H12MgO14Rb2Se2, monoclinic, P121/a1 (No. 14), a = 9.401(1) Å, b = 12.658(2) Å, c = 6.339(1) Å, β = 105.25(1)°, V = 727.8 Å3, Z = 2, Rgt(F) = 0.020, wRref(F2) = 0.040, T = 293 K. CoH12O14Rb2Se2, monoclinic, P121/a1 (No. 14), a = 9.363(1) Å, b = 12.618(1) Å, c = 6.3562(7) Å, β = 105.238(9)°, V = 724.5Å3, Z = 2, Rgt(F) = 0.018, wRref(F2) = 0.037, T = 293 K. H12MnO14Rb2Se2, monoclinic, P121/a1 (No. 14), a = 9.4496(8) Å, b = 12.760(1) Å, c = 6.3794(7) Å, β = 105.189(7)°, V = 742.4Å3, Z = 2, Rgt(F) = 0.025, wRref(F2) = 0.056, T = 293 K. H12O14Rb2Se2Zn, monoclinic, P121/a1 (No. 14), a = 9.352(1) Å, b = 12.626(2) Å, c = 6.360(1) Å, β = 105.195(8)°, V = 724.7 Å3, Z = 2, Rgt(F) = 0.024, wRref(F2) = 0.048, T = 293 K.

Crystal structure of cis-bis(N,N-dimethyl-N′-4-chlorobenzoylthioureato) palladium(II), Pd(C10H10ClN2OS)2

Abstract: C20H20CI2N4O2PCIS2, monoclinic, P12i /c l (No. 14), a= 12.323(4) Á, b = 8.629(3) Â, c = 21.212(7) k,ß = 97.170(6)°, V = 2238.0 Â, Z = 4, Rgt(F) = 0.045, wRKf(F) = 0.133, 7 = 193 K. Source of material The title compound was prepared according to the method described in the literature [1], The metallic solution was added dropwise to the ligand in a 1:2 ratio with a small excess of ligand. The solid complex was filtered and recrystallized from a ethanol/dichloromethane mixture (1:1). Discussion We have worked on the preparation, structure characterization and properties of new thiourea derivatives. In this study, we have crystallized the c/.s'-bis(A,Af-dimethyl-./V'-4-chlorobenzoylthioureato)palladium(II) complex and its structural analysis has been undertaken. The title compound is a m-complex with slightly distorted square planar coordination of the central Pd atom by 2 O and 2 S atoms. The Pd—S (2.240(1) À & 2.243(1) Â) bond distances are equal within experimental error as are the Pd—O bonds. The distance of Pd from the best plane through the coordination sphere is 0.008(1) À. The chelate ring systems, P d O C N C S , are nearly planar as well with the largest deviations from the best plane being 0.139(2) Â for SI . Accordingly; the dihedral angle between these chelate planes is 3.4(1)°. The molecular structure is very close to the related 1,1-diethyl Ni complex [2] and shows similar short C — Ν and C—S bonds indicating the known j r -bonding character in the chelate r ings ( d ( C l — O l ) = 1.269(4) Á, d(C8—SI) = 1.734(4) Á). The bond lengths and angles in the thiourea moiety are typical for compound. Table 1. Data collection and handling. Crystal: Wavelength: μ: Diffractometer, scan mode: 2Ömax: N(hkl)measuKä, N(hkl)unique: Criterion for 70bs, N(hkl)gύ N(param) refined: Program: brown prism, size 0.24 χ 0.41 χ 0.48 mm Mo Ka radiation (0.71073 Â) 12.81 cm\" Bruker CCD, ω 50.2° 13547,3891 U s > 2 ff(/obs), 3532 288 SHELXTL [3] Table 2. Atomic coordinates and displacement parameters (in Â\"). Atom Site X y ζ t/iso H(2) 4e 0.3852 -0.3451 -0.3723 0.032 H(3) 4e 0.4900 -0.3751 -0.2728 0.035 H(5) 4e 0.6134 -0.7789 -0.3336 0.031 H(6) 4e 0.5077 -0.7507 -0.4314 0.029 H(9A) 4e 0.4899 -0.8357 -0.5540 0.060 H(9B) 4e 0.4521 -0.9601 -0.6060 0.060 H(9C) 4e 0.3988 -0.9555 -0.5427 0.060 H(10A) 4e 0.2175 -0.8528 -0.6652 0.053 H(10B) 4e 0.3298 -0.9132 -0.6829 0.053 H(10C) 4e 0.2967 -0.7393 -0.6948 0.053 H(12) 4e 0.0427 0.2666 -0.5166 0.035 H(13) 4e 0.0524 0.4522 -0.4355 0.035 H(15) 4e 0.2985 0.2083 -0.3339 0.032 H(16) 4e 0.2864 0.0198 -0.4146 0.030 H(19A) 4e -0.0122 -0.0452 -0.7601 0.045 H(19B) 4e -0.1318 -0.0417 -0.7422 0.045 H(19C) 4e -0.0555 -0.1834 -0.7223 0.045 H(20A) 4e -0.1119 0.1489 -0.6249 0.044 H(20B) 4e -0.1078 0.1914 -0.6964 0.044 H(20C) 4e -0.0077 0.2290 -0.6456 0.044 * Correspondence author (e-mail: arslanh@mersin.edu.tr) 480 Pd(CioHioClN2OS)2 Table 3. Atomic coordinates and displacement parameters (in À). Atom Site X >> ζ Un Un ί/33 Un U13 U2Ì Pd(l) 4e 0.21837(2) -0.31933(3) -0.55932(1) 0.0223(2) 0.0200(2) 0.0207(2) 0.0033(1) -0.0026(2) 0.0009(1) S(l) 4e 0.21450(8) -0.5463(1) -0.61080(5) 0.0290(5) 0.0227(5) 0.0240(5) 0.0025(4) -0.0081(4) -0.0013(4) Cl(2) 4e 0.18157(9) 0.4814(1) -0.31719(5) 0.0404(6) 0.0320(5) 0.0347(6) 0.0051(4) 0.0040(5) -0.0103(4) S(2) 4e 0.12227(8) -0.2245(1) -0.64767(5) 0.0315(5) 0.0283(5) 0.0219(5) 0.0091(4) -0.0035(4) -0.0005(4) Cl(l) 4e 0.64213(9) -0.5978(1) -0.22207(5) 0.0399(6) 0.0380(6) 0.0282(6) -0.0059(4) -0.0156(4) 0.0047(4) 0(1) 4e 0.3144(2) -0.3991(3) -0.4817(1) 0.033(2) 0.022(1) 0.025(1) 0.009(1) -0.009(1) -0.002(1) 0(2) 4e 0.2150(2) -0.1172(3) -0.5104(1) 0.037(2) 0.027(2) 0.028(2) 0.009(1) -0.011(1) -0.006(1) N(l) 4e 0.3762(3) -0.6404(4) -0.5149(2) 0.024(2) 0.021(2) 0.020(2) 0.003(1) -0.001(1) 0.002(1) N(3) 4e 0.0810(3) 0.0300(4) -0.5730(2) 0.021(2) 0.023(2) 0.024(2) -0.000(1) -0.001(1) 0.001(1) N(4) 4e -0.0186(3) 0.0040(4) -0.6686(2) 0.024(2) 0.026(2) 0.024(2) 0.003(1) -0.003(1) 0.001(1) N(2) 4e 0.3447(3) -0.7867(4) -0.6034(2) 0.036(2) 0.026(2) 0.023(2) 0.006(2) -0.004(2) -0.004(1) C(l) 4e 0.4357(3) -0.5437(4) -0.4117(2) 0.017(2) 0.022(2) 0.024(2) -0.002(1) 0.002(1) 0.004(2) C(2) 4e 0.4316(3) -0.4341(4) -0.3643(2) 0.029(2) 0.022(2) 0.026(2) 0.002(2) -0.002(2) 0.003(2) C(3) 4e 0.4934(3) -0.4510(5) -0.3056(2) 0.034(2) 0.028(2) 0.024(2) 0.000(2) 0.001(2) -0.001(2) C(4) 4e 0.5598(3) -0.5787(5) -0.2952(2) 0.024(2) 0.031(2) 0.019(2) -0.008(2) -0.007(2) 0.003(2) C(5) 4e 0.5662(3) -0.6908(4) -0.3418(2) 0.027(2) 0.025(2) 0.027(2) 0.003(1) 0.000(2) 0.005(2) C(6) 4e 0.5044(3) -0.6735(4) -0.3991(2) 0.023(2) 0.023(2) 0.025(2) 0.001(1) -0.000(2) -0.003(1) C(7) 4e 0.3683(3) -0.5246(4) -0.4749(2) 0.020(2) 0.021(2) 0.021(2) 0.000(1) 0.000(1) 0.002(1) C(8) 4e 0.3192(3) -0.6586(4) -0.5723(2) 0.027(2) 0.022(2) 0.024(2) -0.002(2) 0.004(2) 0.003(2) C(9) 4e 0.4286(4) -0.8937(5) -0.5740(2) 0.057(3) 0.029(2) 0.034(2) 0.015(2) 0.002(2) -0.004(2) C(10) 4e 0.2927(4) -0.8264(5) -0.6670(2) 0.047(3) 0.029(2) 0.028(2) 0.001(2) -0.006(2) -0.008(2) C ( l l ) 4e 0.1633(3) 0.1223(4) -0.4727(2) 0.024(2) 0.022(2) 0.023(2) 0.000(2) 0.002(2) 0.005(2) C(12) 4e 0.0941(3) 0.2539(5) -0.4790(2) 0.029(2) 0.027(2) 0.030(2) 0.003(2) 0.001(2) 0.004(2) C(13) 4e 0.1001(3) 0.3638(5) -0.4315(2) 0.030(2) 0.026(2) 0.032(2) 0.007(2) 0.004(2) 0.001(2) C(14) 4e 0.1760(3) 0.3452(4) -0.3780(2) 0.025(2) 0.022(2) 0.026(2) -0.004(2) 0.007(2) -0.002(2) C(15) 4e 0.2459(3) 0.2190(5) -0.3711(2) 0.025(2) 0.029(2) 0.025(2) 0.002(2) -0.001(2) 0.003(2) C(16) 4e 0.2385(3) 0.1079(4) -0.4190(2) 0.026(2) 0.022(2) 0.026(2) 0.003(2) 0.001(2) 0.003(2) C(17) 4e 0.1539(3) 0.0002(4) -0.5230(2) 0.023(2) 0.021(2) 0.024(2) -0.003(2) 0.005(2) -0.001(2) C(18) 4e 0.0594(3) -0.0551(4) -0.6258(2) 0.019(2) 0.022(2) 0.021(2) 0.001(1) 0.000(1) 0.008(1) C(19) 4e -0.0579(3) -0.0732(5) -0.7284(2) 0.027(2) 0.037(2) 0.024(2) 0.000(2) -0.004(2) 0.001(2) C(20) 4e -0.0655(3) 0.1565(5) -0.6580(2) 0.028(2) 0.023(2) 0.034(2) 0.005(2) -0.005(2) 0.004(2) Acknowledgment. This work was supported by Mersin University Research Fund (Project No: FEF.K.HA.99.1).

Crystal structure of dicaesium hexachlorotungstate(IV), Cs2[WCl6]

Abstract: Cl 6 Cs 2 W, cubic, Fm3m (No. 225), a = 10.245(1) A, V= 1075.3 A 3 , Z = 4, R gt (F) = 0.060, wR ref (F 2 ) = 0.139, T = 293K.

Refinement of the crystal structure of gallium oxide hydroxide, GaO(OH)

Abstract: GaHO 2 , orthorhombic, Pnma (No. 62), a = 9.7907(8) A, b = 2.9732(2) A, c = 4.5171(4) A, V = 131.5 A 3 , Z = 4, R gt (F) = 0.0403, wR ref (F 2 ) = 0.081, T= 293K.

Crystal structure of barium europium germanide, Ba6-xEuxGe25 (x = 0.6), a chiral clathrate

Abstract: Ba5.4oEuo.6oGe25, cubic, P4i32 (No. 213), a = 14.5271(2) Â, V= 3065.8Â, Ζ = 4, Rgt(F) = 0.055, wR^F) = 0.091, T= 295 K. Source of material The samples Ba6-.vEu.vGe25 (A = 0.1,0.2,0.4,0.5,0.6,0.8,2.0) were prepared by melting the elements in an open glassy carbon crucible (HF furnace, argon atmosphere) and annealing at 923 Κ (52 d). The materials are silvery metallic, brittle, and stable in air and moisture. The ICP-AES chemical analysis of the alloy with χ = 0.6 resulted in the composition Ba5.48(5)Euo.57(2)Ge24.9(2). Experimental details The lattice parameters of Bas.4Euo.6Ge25 were determined from the least-squares refinement of the 20 values of 140 reflections (powder data, 18°<26>< 100°, À(CuKai)= 1.540598 Â;LaB6 standard, a = 4.15695(6) Á). The rather large elongation of the displacement ellipsoid for the M2 site (Table 3) is typical for all members of the BaóIruGen family [1-10]. ForBa5.4Euo.6Ge25, the electron density distribution around the M2 position was additionally modelled using two split sites (M2' and M2\", Table 2). The lattice constant of Ba6-AEu.vGe25 alloys (x=0.1 to 2.0) depends on the composition and a phase range could be proven with the maximum solubility corresponding tox=0.6 [11]. Discussion Ba5.4Euo.öGe25 belongs to the Ba6ln4Ge2i structure type (Pearson symbol cP124) [ 1,2]. The structure is characterized by a 3D chiral framework of condensed Ge20 pentagondodecahedra (pdods) forming a 3D channel labyrinth (figure, top). Each pdod is centered by Ml . M2 and M3 are located in the cavities of the zeolite-like channels. The characteristic germanium environment around each of the metal sites is illustrated in the figure (bottom). The structure analysis indicates that Eu occupies partially the Ml and M3 sites. The refined Ba : Eu ratio at Ml (85.7(4) : 14.3) and at M3 (68.5(4) : 31.5) positions results in the chemical composition Ba5.40(4)Euo.6oGe25. The Ge—Ge bond lengths vary in the range 2.471(2) À to 2.565(3) Á [in particular d(Ge2—Ge2) = 2.494(5)  andí/(Gel—Gel) = 2.565(3) À], The Ge3 and Ge5 positions are three-fold bonded (3b), and the remaining Ge positions are four-fold bonded (4b). Magnetization and magnetic susceptibility measurements indicate an oxidation state for europium of 2+ [ 12]. In terms of the Zintl concept, the formula Bas.4Euo.6Ge25 might be written as [(Ba/Eu)]6[(3b)Gel8[(4b)Ge°]i7(4el. Thus, the title compound is a Zintl phase with few conduction electrons. This is confirmed by the electrical resistivity data, showing metall-like behavior above 230 K. The transport properties of Ba6-vEuAGe25 alloys are modified by europium insertion, and in comparison with BaéGe25, the two-step first-order phase transition at Tsi,s2 ~ 180 K, 220 Κ is quickly suppressed with increasing Eu content [11,12]. * Correspondence author (e-mail: carrillo@cpfs.mpg.de) 398 Ba6-.vEu.vGe25 (χ = 0.6) Table 1. Data collection and handling. silvery chunk, size 0.16 χ 0.23 χ 0.24 mm Ag Ka radiation (0.56087 Â) 168.65 cm\" Stoe IPDS, 268 exposures, Αφ = 0.6° 47.78° 31729, 1620 U s > 2 a(Iobs), 1386 56 SHELXL-97 [13], ATOMS [14] Table 3. Atomic coordinates and displacement parameters (in  ' ) .

Crystal structure of catena-poly{[tetra[μ-(benzoato-O,O′)]dicopper(II)]-μ-2-N,N′-(4,4″-bi-3,5-dimethylpyrazolate)} hydrate, [Cu2(O2CC6H5)4(C10N4H14)] · H2O

Abstract: Abstract C38H36Cu2N4O9, monoclinic, C12/c1 (No. 15), a = 18.336(4) Å, b = 19.494(4) Å, c = 11.389(2) Å, β = 113.76(1)°, V = 3725.9 Å3, Z = 4, Rgt(F) = 0.029, wRref(F2) = 0.073, T = 296 K.

Refinement of the crystal structure of the δ-modification of tris(8-hydroxyquinoline) aluminum(III), δ-Al(C9H6NO)3, the blue luminescent Alq3

Abstract: C27H18AIN3O3, triclinic, P I (No. 2), a = 6.181(1) Â, b = 13.268(3) Á, c = 14.430(3) À, a = 66.06(3)°, β = 88.56(3)°, y = 84.03(3)°, V= 1075.5 À , Z = 2, Rgt(F) = 0.108, wRlef(F) = 0.437, Γ = 2 9 3 K. Source of material Sublimed bright-yellow tris(8-hydroxyquinoline)aluminum(III) (Alq3, Eastman Kodak Company) was placed into a glass ampoule (cylindrical shaped bulb 3 cm χ 2.5 cm with a neck 7 cm long and 0.5 cm inside diameter). The ampoule was evacuated ( 10\" -10\" 6 Torr) and the end of the neck sealed. The ampoule was placed into a tube furnace and heated to 663 Κ over a period of 4 h at a rate of 100 K/h, and held at 663 Κ for 3.5 h. The heating source for the furnace was turned off and the ampoule (still in the furnace) was allowed to slowly cool to room temperature overnight. The ampoule was removed and the resulting Alq3 specimen was observed to be a dull yellow color and displayed blue luminescence when irradiated by 365 nm UV light. The neck of the ampoule was removed; an aliquot of the thermally processed Alq3 was analyzed by powder XRD, and the conversion to (5-Alq3 was found to be complete. Upon careful examination of the thermally processed sample, thin, plate-shaped <5-Alq3 crystals were observed to be present. Although thin, these crystals were found to be of acceptable quality for single-crystal data collection. To our knowledge, this is the first report of the generation of singlecrystals of <5-Alq3. * Correspondence author (e-mail: manju.rajeswaran@kodak.com) Experimental details The single-ciystal structure is of tremendous value, even though structure from powder data is available [1], because the data-to-parameter ratio is very high for single crystal data, i.e., 2830 reflections (560 with /obs > 2 o(Iobs) ) versus 357 reflections for powder data. Thus, the high data-to-parameter ratio leads to a more accurate structure. Also for structure determination using powder data, an idealized model is the starting point, which is then refined under constraints to closely match the powder pattern. This approach is in contrast to actually locating atomic positions in electron density maps for single-crystal data. Otherwise, the atomic positions were not refined anisotropically because of the relatively low quality data.

Crystal structure of sodium ytterbium(III) selenide, NaYbSe2

Abstract: NaSe 2 Yb, trigonal, R3m (No. 166), a = 4.0568(8) A, c = 20.772(6) A, V = 296.1 A 3 , Z = 3, R gt (F) = 0.051, wR ref (F 2 ) = 0.110, T = 298K.

Crystal structure of potassium antimony hexathiodiphosphate, KSbP2S6

Abstract: KSbP2S6, monoclinic, P1211 (No. 4), a = 6.605(1) A, b = 7.651(2) A, c = 9.754(2) A, = 92.11(3)°, V = 492.6 A, Z = 2, Rgt(F) = 0.018, wRref(F) = 0.044, T = 293 K. Source of material For the synthesis of KSbP2S6, the corresponding high purity element powders (99.99%) supplied by Aldrich were mixed in the stoichiometric amounts, sealed in evacuated quartz tubes, and heated at 1023 K for two weeks. After the reaction was completed, the sample was slowly cooled to room temperature. All manipulations were carried out under Ar atmosphere Discussion In the course of our work on chalcogen phosphates [1,2], we have preparated the quaternary antimony hexathiodiphosphate KSbP2S6. This compound is isostructural to KBiP2S6 [3]. As expected, the Sb—S bonds in KSbP2S6 are shorter that the Bi—S bonds in KBiP2S6. Also, the smaller radius of Sb results in a decreased coordination number. Thus, each Sb is coordinated by five S atoms compared with the six-coordinated Bi ions in the isostructural compound. In the title compound, each Sb ion is tri-coordinated by one ethane-like [P2S6] ligand and mono-coordinated by two [P2S6] groups forming chains, while a sixth S atom connect the Sb to a neighboring chain, through a Sb–S contact of 3.4187(9) A, to form a layer in the bc plane. The layer are separated by the K ions. The bond lengths d(Sb—S) range from 2.545(1) A to 3.1471(5) A. The compounds KMP2S6 (M = Sb, Bi) are structurally related to Na0.16Bi1.28P2S6 [4] and -KMP2Se6 [5]. Z. Kristallogr. NCS 218 (2003) 403–404 403 © by Oldenbourg Wissenschaftsverlag, Munchen Sb 2a 0.81740(3) 0.76783(2) 0.98199(2) 0.0247(1) 0.0193(1) 0.0235(1) –0.0014(1) –0.00049(9) –0.0024(1) K 2a 0.6955(1) 1.0534(1) 0.50699(9) 0.0300(5) 0.0380(5) 0.0314(5) –0.0002(4) –0.0020(4) –0.0003(4) P(1) 2a 0.6923(1) 0.3492(1) 0.82655(9) 0.0176(5) 0.0174(4) 0.0167(4) –0.0019(4) –0.0007(3) 0.0009(4) P(2) 2a 0.7957(1) 0.5678(1) 0.69610(9) 0.0191(4) 0.0199(4) 0.0172(4) –0.0019(4) –0.0001(3) 0.0016(4) S(1) 2a 0.6716(1) 0.4642(1) 1.01839(8) 0.0297(5) 0.0219(4) 0.0174(5) –0.0062(4) 0.0032(4) –0.0019(4) S(2) 2a 0.9110(1) 0.1592(1) 0.8275(1) 0.0230(5) 0.0213(4) 0.0247(5) 0.0034(4) –0.0038(4) –0.0015(4) S(3) 2a 0.4285(1) 0.2626(2) 0.74772(8) 0.0194(4) 0.0263(4) 0.0233(4) –0.0057(5) –0.0035(3) 0.0011(5) S(4) 2a 1.0547(1) 0.6438(1) 0.8062(1) 0.0180(4) 0.0297(4) 0.0232(5) –0.0036(4) 0.0002(4) –0.0025(4) S(5) 2a 0.5878(1) 0.7546(2) 0.73068(9) 0.0251(4) 0.0226(4) 0.0268(4) 0.0045(5) –0.0041(3) –0.0007(5) S(6) 2a 0.8271(2) 0.4844(2) 0.5078(1) 0.0308(6) 0.0367(6) 0.0184(5) –0.0037(5) 0.0023(4) –0.0030(4) Table 2. Atomic coordinates and displacement parameters (in A). Atom Site x y z U11 U22 U33 U12 U13 U23 Crystal: yellow block, size 0.089 × 0.104 × 0.224 mm Wavelength: Mo K radiation (0.71073 A) : 47.43 cm Diffractometer, scan mode: Bruker AXS SMART CCD, / 2 max: 55.84° N(hkl)measured, N(hkl)unique: 4075, 2078 Criterion for Iobs, N(hkl)gt: Iobs > 2 (Iobs), 2037 N(param)refined: 91 Programs: SHELXL-97 [6], DIAMOND [7] Table 1. Data collection and handling.

Crystal structure of potassium bismuth hexathiodiphosphate, KBiP2S6

Abstract: BiKP2S6, monoclinic, P12 i l (No. 4), a = 6.6200(6) À, b = 7.4058(7) Á, c = 9.9002(9) À, β = 92.108(1)°, V = 485.0 Â, Ζ = 2, Rgl(F) = 0.027, wRref(F) = 0.060, Τ = 293 Κ. Source of material All manipulations were carried out under Ar atmosphere. For the synthesis of KBÌP2S6 stoichiometric amounts of the corresponding high purity (99.99%) elements, supplied by Aldrich, were mixed an sealed in quartz tubes after evacuation. The mixture was them heated at 1123 Κ for two weeks. The reacted matter was slowly cooled (0.4 K/min) to room temperature. Experimental details The absolute configuration was tested and the wR(F) values for the two possible orientations were 0.0586 and 0.1907. The first one represents the absolute structure of the crystal studied. The corresponding Flack parameter is 0.012(7). Discussion In the course of our work on chalcophosphate [1,2] we have prepara ted the qua te rnary b i smuth hexa th iod iphospha te KBÌP2S6. The title compound has a complicated layered structure, which contains the ethane-like [P2S6] ligand. KB1P2S6 is structurally related to Nao.i6Bii.2sP2S6 [3] and KBiP2Se6 [4], The structure is characterized by layers of condensed S6 distorted octahedra alternately centered by P2 pairs and Bi atoms. The staircase layers of [B1P2S6]groups in the a-b plane are held together by a single layer of K ions. The bond lengths in the hexathiodiphosphate [P2S6]\" are d(P—P) = 2.219(3) Â and d(P—S) in the range from 1.962(3) À to 2.058(3) À. The ethane-like [P2S6]\" ligand chelates to 4 Bi atoms, the bond lengths d(Bi—S) range from 2.706(2) Â to 3.143(2) Â. Table 1. Data collection and handling. Crystal: Wavelength: μ· Diffractometer, scan mode: 20max : N(hkl)measured, N(hkl)unique: Criterion for I0bs, N(hkl)gt: N(param) refined: Programs: red dark prism, size 0.075 χ 0.075 χ 0.2 mm Mo Ka radiation (0.71073 Â) 201.48 cnT Siemens SMART CCD, φ/ω 56° 3908,2071 /obs>2CT(7obs), 1901 91 SHELXL-97 [5], ATOMS [6] Table 2. Atomic coordinates and displacement parameters (in Â).

Crystal structure of di[potassium(18-crown-6)]dipotassium nonastannide(4–)—diethylenediamine solvate (1:1.5), [K(C12H24O6)]2K2[Sn9] · 1.5C2N2H8

Abstract: Abstract C27H60K4N3O12Sn9, monoclinic, P121/n1(No. 14), a = 10.410(2) Å, b = 25.659(5) Å, c = 20.636(4) Å, β = 102.56(3)°, V = 5380.2 Å3, Z = 4, Rgt(F) = 0.030, wRref(F2) = 0.072, T = 150 K.

Crystal structure of potassium ytterbium(III) selenide, KYbSe2

Abstract: KSe 2 Yb, trigonal, R3m (No. 166), a = 4.111(2) A, c = 22.70(1) A, V= 332.2 A 3 , Z = 3, R gt (F) = 0.043, wR ref (F 2 ) = 0.113, T = 293K.

Crystal structure of dilanthanum pentaiodide, La2l5

Abstract: I5La2,monoclinic, P12i /ml (No. 11), a = 8.618(2)À, 6 = 4.4038(9)À, c = 14.580(3) Α, β = 90.20(3)° , V = 553 .3 Á 3 , Z = 2, flgt(F) = 0.026, wRKf(F) = 0 .059, 7 = 2 9 3 K. Source of material Reaction of L a metal and Lal3 in T a capsules in A r a tmosphere for 12d at 1225 Κ leads to s ingle crystals of La2l5Discuss ion La 2 I 5 is isotypic wi th Pr 2 l5 [1], L a 2 B r 5 [2], and P r 2 X 5 (X = Br, I) [3]. T h e L a a toms are coord ina ted b y seven iodine a toms fo r L a ( l ) and eight fo r La(2) t r igonal pr ismat ica l ly inc luding posit ions above the rec tangular p r i sm faces . Table 1. Data collection and handling. Crystal: bronze, needle, size 0 .024 χ 0.024 χ 0.190 m m Wavelength: Mo Ka radiation (0.71073 Â) μ: 2 1 4 . 8 8 c m \" 1 Diffractometer, scan mode: Stoe IPDSn, φ 20ma\\'· 5 8 ° N(hkl)measured, N(hkl)unique· 10418 , 1 6 4 2 Criterion for 70bs, N(hkl)gC. 7obs>2CT(/obsJ, 1 4 7 5 N(param)K f lned: 4 4 Programs: SHELXL-97 [4], DIAMOND [5] References 1. Warkentin, E.: Zur Strukturchemie des Systems Pr-Prl3, Dissertation, Universität Karlsruhe 1977. 2. Krämer, Κ.; Schleid, T.; Schulze, M.; Urland, W.; Meyer, G.: Three Bromides of Lanthanum: LaBr2, La2Br6, and LaBr3. Z. Anorg. Allg. Chem. 575(1989)61-70. 3. Krämer, Κ.; Meyer, G.; Fischer, P.; Hewat, A. W.; Giidel, H. U.: Neutron Diffraction Investigation of Magnetic Phase Transitions to Longe-Range Antiferromagnetic Ordering in the 'Free-Electron' Praseodymium Halides Pr2X5 (X = Br, I). J. Solid State Chem. 95 (1991) 1-13. 4. Sheldrick, G. M.: SHELXL-97. Program for Refining Crystal Structures. University of Göttingen, Germany 1997. 5. Brandenburg, K.: DIAMOND Visual Crystal Structure Information System. Crystal Impact, Germany 2000. 1 able 2. Atomic coordinates and displacement parameters (in À). La(l) La(2) KD 1(2) 1(3) 1(4) 1(5) Site X y ζ Un U22 ί/33 Un t/13 U23 2e 0.42084(5) 1/4 0.65836(3) 0.0233(2) 0.0225(2) 0.0202(2) 0 0.0038(2) 0 2e 0.91707(6) 1/4 0.15865(3) 0.0403(3) 0.0178(2) 0.0239(2) 0 0.0085(2) 0 2e 0.69529(6) 1/4 0.49188(3) 0.0266(2) 0.0228(3) 0.0209(2) 0 0.0041(2) 0 2e 0.04689(6) 1/4 0.67838(3) 0.0238(2) 0.0261(3) 0.0233(2) 0 0.0030(2) 0 2e 0.35660(6) 1/4 0.87902(3) 0.0299(3) 0.0278(3) 0.0234(2) 0 0.0051(2) 0 2e 0.84783(6) 1/4 0.92992(3) 0.0298(3) 0.0238(3) 0.0210(2) 0 0.0041(2) 0 2e 0.33452(6) 1/4 0.27313(4) 0.0294(2) 0.0213(3) 0.0308(3) 0 0.0006(2) 0 Correspondence author (e-mail: Hj.Mattausch@fkf.mpg.de)

Crystal structure of digadolinium(III) oxide disulfide, Gd2OS2

Abstract: Gd2OS2, monoclinic, P121/c1 (No. 14), a = 8.3365(6) A, b = 6.9872(5) A, c = 6.9231(5) A, = 99.463(6)°, V = 397.8 A, Z = 4, Rgt(F) = 0.022, wRref(F) = 0.047, T = 293 K. Source of material The new oxysulfide Gd2OS2 was obtained by reacting a mixture of Gd2O3, S and Gd (molar ratio 1:9:6) at 1123 K for seven days in an evacuated sealed silica ampoule when an excess of CsCl is added as flux. Apart from the large, colourless, square brick-shaped single crystals of Gd2OS2, which turned out to be airand water-resistant, traces of Gd2S3 were also present as by-product. Discussion Since 1990, rare-earth oxysulfides of the general formula M2OS2 are already known with M = Sm, Tb, Dy and Y obtained at lower temperature under normal pressure [1–5]. They were also accessible with M = Er, Tm and Yb by using high-pressure/hightemperature techniques [6]. However, the isotypic gadolinium compound was to date unknown. The title compound Gd2OS2 contains two crystallographically different Gd cations, each in sevenfold coordination. The anionic coordination polyhedron about Gd1 can be described as a distorted monocapped trigonal prism [(Gd1)O3(S1)2+1(S2)], while one O and six S anions build a more perfect monocapped trigonal prism [(Gd2)O(S1)2(S2)4] around Gd2 where the cap is formed by the single oxygen above the rectangular (S1,S1,S2,S2) face. The O coordination sphere actually consists of four Gd cations arranged as [OGd4] tetrahedron with O—Gd distances of 227 pm, 229 pm, 230 pm and 232 pm. Two [O(Gd1)3(Gd2)] tetrahedra are bridged by a common Gd1—Gd1 edge (d(Gd1—Gd1) = 361 pm) to form cationic dimers [O2Gd6] surrounded by sixteen S and six O anions. Further connectivity of these dimers occurs via oxygen and terminal Gd1 atoms so that the latter become part of the bridging edge of the next dimers (see figure). When all Gd1 termini are connected, two-dimensional infinite layers stacked along [001] and described as 2 [O(Gd1)3/3(Gd2)1/1] appear within the structural framework. Different layers are held together by two crystallographically independent S anions occupying free edges and faces of the O centred (Gd)4 tetrahedra. Finally, the crystal structure shows two different S anions that exhibit a vicinity of four plus one (S1) or five Gd cations (S2) in the shape of distorted tetragonal pyramids (d(S—Gd) = 277 pm – 295 pm, 314 pm). Z. Kristallogr. NCS 218 (2003) 285–286 285 © by Oldenbourg Wissenschaftsverlag, Munchen Crystal: colourless, brick-shaped, size 0.06 × 0.08 × 0.09 mm Wavelength: Mo K radiation (0.71069 A) : 338.85 cm−1 Diffractometer, scan mode: Nonius Kappa-CCD, / 2 max: 55.02° N(hkl)measured, N(hkl)unique: 7293, 911 Criterion for Iobs, N(hkl)gt: Iobs > 2 (Iobs), 868 N(param)refined: 47 Programs: SHELXL-97 [7], DIAMOND [8] Table 1. Data collection and handling.

Crystal structure of di[K(18-crown-6)]dirubidium nonagermanide(4–) diethylenediamine, [K(C12H26N2O4)]2Rb2[Ge9] · 2C2N2H8

Abstract: Abstract C28H68Ge9K2N8O8Rb2, monoclinic, P121/c1 (No. 14), a = 16.864(3) Å, b = 12.091(2) Å, c = 26.466(5) Å, β = 97.28(3)°, V = 5353.0Å3, Z = 4, Rgt(F) = 0.058, wRref(F2) = 0.176, T = 153 K.

Crystal structure of rubidium gallium Catena-[monohydrogen-monoborate-bis(monophosphate)] RbGa[BP2O8(OH)], From a twinned crystal

Abstract: BGaHO9P2Rb, monoclinic, P121/c1 (No. 14), a = 9.3207(8) A, b = 8.3686(7) A, c = 9.5371(9) A, = 102.527(3)°, V = 726.2 A 3 , Z =4 ,Rgt(F) = 0.050, wRref(F 2 ) = 0.147, T = 295 K.

Crystal structure of ethylenediaminesilver(I) di(3,5-dinitrobenzoato)- silver(I) dihydrate, Ag2(C2H8N2)(C7H3N2O6)2 · 2H2O

Abstract: Ci6H18Ag2N60i4, triclinio, PI (No. 2), a = 6.978(2) Á, b= 12.919(5)Á, c = 15.029(5)Â, a = 84.320(6)°, = 76.810(5)°, y = 79.612(6)°, V= 1295.1 Â 3 , Z = 2, Rgt(F) = 0.065, wRitífF) = 0.091, T = 298 K. Source of material AgiO (0.5 mmol, 116 mg) and 3,5-dinitrobenzoic acid (1 mmol, 212 mg) were dissolved in ammonium solution (10 ml), stirring for ca. 10 min and ethylenediamine (1 mmol, 60 mg) was added to obtain a clear solution. After standing in air for two days with the ammonium gas escaping, large colorless prismatic crystals were crystallized, isolated, washed with water for three times, and dried m a vacuum desiccator under drying CaCh (yield 73%). Elemental analysis: found C, 26.45%; H, 2.55%; N, 11.26%; calc. for Ci6H18Ag2N60i4 C, 26.18%; H, 2.47%; N, 11.45%. Experimental details All the H atoms were added on calculated positions. Due to a little disorder, the t/y values of C1 and C2 atoms are quite large, we do not try to split them. Discussion The coordination chemistry of the coinage metals has been the subject of investigation for decades [1]. Historically, the interest in this area grew out of the diverse structural motifs displayed by these superficially similar monovalent cations. More recently, the interest has been renewed by practical concerns. Such coinage metal complexes can be used as potential precursors to metal films via CVD (chemical vapor deposition) processes [2,3]. An alternative method for separating olefins and paraffins is chemical adsorption using silver(I) compounds [4], which form complexes with unsaturated compounds such as olefins and acetylenes but not with saturated compounds such as paraffins [5]. We are interested in the investigation on silver(I) complexes with various organic ligands containing Ν and/or O atoms. Reported here is a silver (I) carboxylato complex with ethylenediamine. The title complex crystallizes with the asymmetric unit consisting of two Ag ions, two 3,5-dinitrobenzoate anions, one ethylenediamine molecule, and two crystal water molecules. The Ag(l) ion has a linear coordination, being coordinated by two nitrogen atoms from two amine. The Ag—Ν distances are 2.148(5) À and 2.166(5) À and the N-Ag-N angle is 175.7(2)°. The Ag(2) ion also has a linear coordination, being coordinated by two oxygen atoms from two dnbc. The Ag—O distances are 2.146(5) Á and 2.097(6)Â and the O-Ag-O angle is 174.5(3)°. Ag(l) and Ag(2) form ligand-unsupported Ag---Ag interaction with a distance of 3.177(5) A. The amine ligands bridge Ag(l) ions to form a coordination polymer chain with Ag(dnbc)2 (where dnbc is 3,5-dinitrobenzoate anion) coordination fragment attached via Ag-'-Ag interaction. In addition, there are a variety of 0 H --0 and C-H-0 hydrogen bonds [¿(013---014) = 2.729(4) Á; ¿ (013-014)= 2.775(4) Â, ¿/(014-0Q3), 2.775(4), ¿ (C2-07) = 2.980(4) Â; d(C9---02) = 2.826(4) Â] which extend the two-dimensional layer into three-dimensional supramolecular array. Table 1. Data collection and handling. Crystal: colorless prism, size 0.08 χ 0.13 χ 0.26 mm Wavelength: Mo Ka radiation (0.71073 A) μ: 15.89 cm\" Diffractometer, scan mode: Bruker SMART CCD, φ/ω 20 max: 52.98° N(hkl)measured, N(hkl)amque: 6823, 4780 Criterion for/0bs, N(hkl)gt· U s > 2 af/obs), 1816 N(param)rei]ned'· 343 Programs: SHELXTL [6], SHELXTL-plus [7] Correspondence author (e-mail: hlzhu@wist.edu.cn) 306 A g 2 ( C 2 H 8 N 2 ) ( C 7 H 3 N 2 0 6 ) 2 · 2 H 2 0 Table 2. Atomic coordinates and displacement parameters (in Â). Table 2. Continued. Atom Site X y ζ UisO Atom Site X y ζ fiso H(1A) 2 i 0.4410 0.6461 0.7127 0.044 H(1D) 2 i 0.3717 0.8487 0.7210 0.080 H(1B) 2 i 0.4618 0.7189 0.6327 0.044 H(2C) 2 i -0.4753 0.8030 0.7154 0.080 H(2A) li -0.2403 0.7045 0.6328 0.043 H(2D) 2 i -0.3271 0.8157 0.7764 0.080 H(2B) 2 i -0.2601 0.6516 0.7235 0.043 H(5) 2 i 0.0622 0.4133 0.8676 0.050 H(l) 2 i 0.3876 0.0554 0.6562 0.080 H(7) 2 i 0.1552 0.1496 1.0232 0.077 H(2) 2 i 0.4221 0.0499 0.5563 0.080 H(9) 2 i 0.3487 0.1561 0.7561 0.062 H(3) 2 i 0.8304 0.0656 0.4822 0.080 H(12) 2 i 0.0756 0.8809 0.3784 0.050 H(4) 2 i 0.8091 -0.0447 0.5112 0.080 H(14) 2 i 0.2133 0.8690 0.1057 0.048 H(1C) 2 i 0.5560 0.7741 0.7477 0.080 H(16) 2 i 0.3451 0.6081 0.2649 0.043 Table 3. Atomic coordinates and displacement parameters (in Â). Atom Site X y ζ Un U22 í/33 U12 C/13 U23 Ag(l) 2 i 0.08760(8) 0.70971(5) 0.68482(4) 0.0297(4) 0.0560(5) 0.0597(5) -0.0053(3) -0.0132(3) -0.0059(4) Ag(2) 2 i 0.2149(1) 0.50890(6) 0.56557(5) 0.0873(6) 0.0553(5) 0.0472(5) -0.0112(4) -0.0181(4) 0.0134(4) N(l) 2 i 0.3920(8) 0.7102(5) 0.6904(4) 0.024(3) 0.037(4) 0.045(4) -0.005(3) -0.004(3) 0.006(3) N(2) 2 i -0.2245(8) 0.7094(5) 0.6899(4) 0.033(4) 0.045(4) 0.034(4) -0.009(3) -0.016(3) 0.002(3) N(3) 2 i -0.016(1) 0.347(1) 1.0416(6) 0.077(7) 0.13(1) 0.037(6) -0.025(7) -0.006(5) -0.015(7) N(4) 2 i 0.369(2) 0.0254(7) 0.8965(7) 0.096(7) 0.045(6) 0.069(7) -0.011(5) -0.019(6) 0.018(5) N(5) 2 i 0.043(1) 1.0002(7) 0.2336(7) 0.065(5) 0.043(6) 0.077(7) -0.012(5) -0.022(5) 0.013(5) N(6) 2 i 0.390(1) 0.6688(8) 0.0937(6) 0.048(5) 0.074(7) 0.047(5) -0.007(5) -0.004(4) -0.003(5) 0(1) 2 i 0.1683(9) 0.4467(5) 0.7052(4) 0.088(5) 0.042(4) 0.056(4) -0.018(4) -0.016(3) 0.010(3) 0(2) 2 i 0.295(1) 0.3009(5) 0.6357(4) 0.098(5) 0.074(5) 0.026(4) -0.014(4) -0.007(3) 0.011(3) 0(3) 2 i 0.242(1) 0.5825(5) 0.4340(4) 0.119(6) 0.043(4) 0.057(4) -0.024(4) -0.037(4) 0.013(3) 0(4) 2 i 0.1638(9) 0.7387(5) 0.4975(4) 0.095(5) 0.071(5) 0.044(4) -0.002(4) -0.011(4) 0.009(4) 0(5) 2 i -0.132(1) 0.4282(7) 1.0331(5) 0.115(7) 0.081(6) 0.094(6) -0.008(5) 0.018(5) -0.015(5) 0(6) 2 i 0.017(1) 0.3048(7) 1.1135(5) 0.173(9) 0.146(8) 0.041(5) 0.013(6) -0.020(5) -0.015(5) 0(7) 2 i 0.480(1) -0.0085(6) 0.8330(6) 0.099(6) 0.056(5) 0.101(7) -0.004(4) 0.012(5) 0.002(5) 0(8) 2 i 0.312(2) -0.0245(7) 0.9691(6) 0.213(9) 0.096(7) 0.092(6) -0.027(6) -0.016(6) 0.055(5) 0(9) 2 i 0.010(1) 1.0510(5) 0.2992(6) 0.102(6) 0.025(4) 0.111(7) 0.004(4) -0.037(5) -0.009(4) O(10) 2 i 0.007(1) 1.0343(6) 0.1604(6) 0.126(7) 0.080(6) 0.094(6) -0.003(5) -0.026(5) 0.043(5) 0(11) 2 i 0.395(1) 0.7197(6) 0.0184(5) 0.120(6) 0.086(5) 0.044(4) -0.026(4) -0.003(4) 0.001(4) 0(12) 2 i 0.450(1) 0.5745(7) 0.1033(5) 0.144(8) 0.058(5) 0.092(6) 0.043(5) -0.030(5) -0.011(4) 0(13) 2 i 0.391(1) 0.0861(6) 0.6033(5) 0.138(7) 0.093(6) 0.073(5) -0.017(5) -0.025(5) -0.014(4) 0(14) 2 i 0.761(1) 0.0206(7) 0.5115(5) 0.127(7) 0.119(7) 0.116(6) -0.020(5) -0.027(5) 0.013(6) C(l) 2 i 0.416(3) 0.782(2) 0.750(2) 0.10(2) 0.37(4) 0.75(6) 0.01(2) -0.15(2) -0.34(4) C(2) 2 i -0.340(2) 0.809(1) 0.715(2) 0.06(1) 0.20(2) 0.49(4) 0.02(1) -0.09(2) -0.10(2) C(3) 2 i 0.225(1) 0.3480(8) 0.7017(7) 0.040(5) 0.046(7) 0.070(7) -0.019(5) -0.033(5) 0.022(5) C(4) 2 i 0.211(1) 0.2930(8) 0.7970(5) 0.036(5) 0.053(6) 0.035(5) -0.005(4) 0.001(4) 0.002(5) C(5) 2 i 0.116(1) 0.3422(7) 0.8726(6) 0.041(5) 0.036(5) 0.048(6) -0.010(4) -0.007(4) -0.001(4) C(6) 2 i 0.096(1) 0.2882(8) 0.9617(6) 0.053(6) 0.050(7) 0.045(6) -0.012(5) -0.003(4) 0.002(5) C(7) 2 i 0.173(1) 0.1863(9) 0.9663(6) 0.075(7) 0.074(8) 0.047(6) -0.041(6) -0.005(5) 0.015(6) C(8) 2 i 0.276(1) 0.1328(8) 0.8919(6) 0.055(6) 0.059(7) 0.029(5) -0.019(5) 0.000(4) 0.018(5) C(9) 2 i 0.285(1) 0.1913(8) 0.8085(5) 0.040(5) 0.084(8) 0.041(5) -0.022(5) -0.022(4) 0.004(5) C(10) 2 i 0.202(1) 0.6837(9) 0.4317(6) 0.060(6) 0.066(8) 0.029(5) -0.007(6) -0.003(4) 0.002(5) C(l l ) 2 i 0.207(1) 0.7378(7) 0.3368(5) 0.034(5) 0.047(6) 0.042(5) -0.003(4) -0.006(4) 0.003(4) C(12) 2 i 0.129(1) 0.8416(6) 0.3273(5) 0.061(6) 0.033(5) 0.032(5) -0.021(4) -0.005(4) -0.003(4) C(13) 2 i 0.132(1) 0.8859(6) 0.2405(7) 0.067(6) 0.022(5) 0.063(7) -0.019(5) -0.021(5) 0.012(5) C(14) 2 i 0.211(1) 0.8363(7) 0.1618(6) 0.027(4) 0.033(5) 0.060(6) -0.008(4) -0.011(4) 0.002(5) C(15) 2 i 0.289(1) 0.7340(7) 0.1749(5) 0.038(5) 0.065(7) 0.030(5) -0.015(5) -0.010(4) -0.009(5) C(16) 2 i 0.291(1) 0.6792(6) 0.2600(5) 0.026(4) 0.035(5) 0.047(5) 0.003(4) -0.014(4) -0.002(4) Acbiowledgments. The authors thank the Education Office of Hubei Province, P. R. China, for the research grant No. 2002B29002 and the Natural Science Foundation of Hubei Province, P. R. China, for the research grant No. 2003ABB010.

Crystal structure of bis(2,6-diaminopyridinum) tetrachloropalladate(II), (C5H8N3)2 · PdCl4

Abstract: C 10 H 16 Cl 4 N 6 Pd, triclinic, P1 (No. 2), a = 6.900(3) A, b = 7.898(3) A, c = 8.025(3) A, α = 103.30(1)°, β = 104.07(1)°, γ = 92.42(1)°, V = 410.6 A 3 , Z = 1, R gt (F) = 0.060, wR ref (F 2 ) = 0.152, T = 110K.

Crystal structure of dilithium ethylenediammonium bis[sulfate], (C2N2H10)Li2(SO4)2

Abstract: C 2 H 10 Li 2 N 2 O 8 S 2 , monoclinic, C12/c1 (No. 15), a = 18.590(1)A, b = 4.9035(4)A, c = 10.1666(4)A, β = 99.599(4)°, V = 913.8A 3 , Z = 4, R gt (F) = 0.031, wR ref (F 2 ) = 0.087, T = 293K.

Crystal structure of trans-bisbenzimidazo[2,1-b:1',2'-j]benzo[lmn][3,8]- phenanthroline-6,9-dione, C26H12N4O2

Abstract: C 26 H 12 N 4 O 2 , monoclinic, P12 1 /c1 (No. 14), a = 11.199(1) A, b = 4.8120(6) A, c = 16.091(2) A, β = 96.816(9)°, V = 861.0 A 3 , Z = 2, R gt (F) = 0.041, wR ref (F 2 ) = 0.141, T = 93K.

Crystal structure of iron nickel phosphide, Fe1.8Ni1.2P, a Schreibersite extracted from Orange River meteorite

Abstract: Fe1.8Ni1.2P8, tetragonal, I4 (No. 82), a = 9.085(5) A, c = 4.481(3) A, V = 369.8 A 3 , Z =8 ,Rgt(F) = 0.037, wRref(F 2 ) = 0.086, T = 293 K. Source of material Single crystals of the phosphides from “Orange River” were obtained by using a solution with HNO3 (3%) and methanol. After dissolving the meteorite samples only sulphides, carbides, oxides, phosphides and other crystals remained. The solution with the crystals was filtered and the phosphides were picked up from thefiltermaterial.Theywerepreparedandfixedonglasfibresfor X-ray experiments. The chemical composition was determined by electron microprobe analysis (Cameca SX 100). The crystals are homogeneous and don’t show zonations, twinnings or intergrowth sections. Discussion The (Fe,Ni)3P single crystals (xenomorph variant named Schreibersite) from the “Orange River” meteorite with a Fe:Ni-ratioof1.5:1(Fe1.8Ni1.2P)showabodycenteredtetragonal crystal structure with the well known space group I4 typical for meteoritic phosphides. The distribution of Fe and Ni on the three symmetryindependentmetalpositionswasdeterminedearlieron Rhabdites from “North Chile” meteorite using a Co-tube with a wavelength near by the Fe absorption edge. This result showed thatNipreferstheM2andM3sitesavoidingM1[1](cf.also[2]). Additional measurements with synchrotron radiation (HASYLAB at DESY, Hamburg) near the Fe absorption edge in order to separate Fe and Ni using the anomalous dispersion and thedeltasynthesis[3,4]showedthesameordering:Feprefersthe M1 and M2 sites whereas Ni prefers the M2 and M3 sites. Considering this fact, the site occupancy factors of the Fe and Ni atomswerefixedduringrefinement[5].ThebestR-valueisevoked by a distribution with Fe on M1, Fe/Ni on M2 and Ni on M3.

Crystal structure of the antibiotic SY-1 (20-deoxy-salinomycin): sodium 2-(6-[2- (5-ethyl-5-hydroxy-6-methyl-tetrahydro-pyran-2-yl)-2,10,12-trimethyl- 1,6,8-trioxa-dispiro[4.1.5.3]pentadec-13-en-9-yl]-2-hydroxy-1,3-dimethyl-4-oxo-heptyl-5-methyl-tetrahydro-pyran-2-yl)-butyrate—methanol solvate (1:0.69), C42H69NaO10 · 0.69CH3OH

Abstract: Abstract C42.693H71.772NaO10.693, orthorhombic, P212121 (No. 19), a = 11.295(1) Å, b = 18.628(1) Å, c = 21.823(1) Å, V = 4591.6 Å3, Z = 4, Rgt(F) = 0.037, wRref(F2) = 0.099, T = 293 K.

Crystal structure of aqua-bis(4-nitrobenzoato)disilver(I), Ag2(C7H4NO4)2(H2O)

Abstract: Source of material AgjO (0.5 mmol, 116 mg) and4-nitrobenzoic acid (1 mmol, 167 mg) were dissolved in ammonium solution (10 ml) and stirred for ca. 10 min to obtain a clear solution. After standing still the solution in air for two days with the ammonium gas escaping, large colorless prism crystals were crystallized, isolated, washed with water for three times, and dried in a vacuum desiccator under drying CaCl2 (yield 41%). Elemental analysis: found C, 30.10%; H, 1.81%; N, 5.00%; calc.forC7H5AgNO4.5-C, 29.71%; H, 1.78%; N, 4.95%.