Showing papers in "Zeitschrift Fur Kristallographie-new Crystal Structures in 2001"

Crystal structure of sodium gallium (monohydrogenmonophosphate- dihydrogenmonoborate-monophosphate), NaGa(BP2O7(OH)3)

Abstract: BGaH3NaO10P2, monoclinic, C12/c1 (No. 15), a = 10.408(3) A, b = 8.094(2) A, c = 9.099(2) A, = 116.64(2)°, V = 685.2 A, Z = 4, Rgt(F) = 0.025, wRref(F ) = 0.068, T = 293 K. Source of material NaGa[BP2O7(OH)3] was synthesized under mild hydrothermal conditions. The reaction was carried out with mixtures of Ga metal (0.139 g) dissolved in 1ml of HCl (18%) with Na2HPO4·12H2O (1.075 g) and Na2B4O7·10H2O (0.4767 g) (molar ratio of Ga:P:B = 2:3:6) in aqueous solution. The mixture was sealed in glass tubes (after adding 1 ml H2O to achieve a degree of filling of 30%) with subsequent heating at 408 K for 60 days. The starting materials are all of analytical grade. Discussion With the increasing interest in microporous materials, synthesis of compounds like borophosphates with open framework structure have drawn much attention during the past few years and show a rich crystal chemistry [1]. Systems including a p-block metal have not been widely explored up to now besides one Al compound [2] reported only recently. The structure of the title compound is isotypic to the Fe [3] and Al analogues [2] and is characterized by isolated GaO4(OH)2 octahedra sharing common O-corners with phosphate and common O(OH)-corners with hydrogenborate groups from the ol igomeric uni ts [B2P2O7(OH)3]. The condensation of the borophosphate oligomers with Ga-coordination octahedra via common corners results in an overall three-dimensional framework which contains elliptical channels running along the [001] direction. The cross section of the channels is defined by eight-membered octahedral/tetrahedral rings (four Ga coordination octahedra, two phosphateand two borate-groups). Sodium ions are distributed within the open channels. The Ga—O bond distances are 1.925 and 1.965 A, while the Ga—OH value is increased to 1.995 A. The bond distances P—O and B—O in the oligomeric borophosphate groups correspond to respective values in the Feand Al-analogues [2,3]. Z. Kristallogr. NCS 216 (2001) 15–16 15 © by Oldenbourg Wissenschaftsverlag, Munchen Crystal: colorless, prism, size 0.15 × 0.2 × 0.3 mm Wavelength: Mo K radiation (0.71073 A) : 45.94 cm Diffractometer, scan mode: Enraf Nonius CAD4, non-profiled scans 2 max: 69.86° N(hkl)measured, N(hkl)unique: 850, 737 Criterion for Iobs, N(hkl)gt: Iobs > 2 (Iobs), 676 N(param)refined: 75 Program: SHELXS-97 [4] Table 1. Data collection and handling. H(1) 4c 1/4 –1/4 1/2 0.05 H(2) 8f 0.485(7) 0.163(6) 0.591(7) 0.05 Table 2. Atomic coordinates and displacement parameters (in A). Atom Site x y z Uiso

Refinement of the crystal structure of digallium trisulfide, Ga2S3

Abstract: Ga2S3, monoclinic, Clcl (No. 9), a = 11.107(2) A, b = 6.395(1) A, c = 7.021(1) Α, β = 121.17(3)°, V= 426.7 A, Ζ = 4, Rgi(F) = 0.035, wRni(F) = 0.084, T= 294 K. Source of material A pale, yellow crystal of Ga2S3 was selected from crystals grown by vapor deposition from Ga2S3 powder in an effusion cell [ 1 ]. The selected crystal had smooth, uniformly-reflecting facet surfaces. Experimental details The unit cell parameters and atomic coordinates from this determination agree with the previously published structure [2], but are systematically smaller, possibly because of a difference in the temperature. An extinction coefficient, 0.142, is reported here for the first time. Crystal: Wavelength: μ: Diffractometer, scan mode: 20max: Wi«)m 2 σ(labs), 432 47 SHEXTL [11], SHELXL-97 [12], PLATON [13] Table 2, Atomic coordinates and displacement parameters (in A). Atom Site X y ζ υ η t/22 ί/33 ί/|2 C/13 t/23 Ga(l) 4a 0.04213(8) 0.4023(2) 0.1251(1) 0.0068(7) 0.0130(6) 0.0096(7) 0.0007(4) 0.0042(5) 0.0005(4) Ga(2) 4a 0.20026(9) 0.9321(2) 0.1156(1) 0.0065(7) 0.0133(6) 0.0102(7) -0.0003(4) 0.0045(5) -0.0012(4) S(l) 4a -0.0050(3) 1.0861(4) -0.0162(6) 0.007(1) 0.016(1) 0.018(1) -0.0001(8) 0.004(1) -0.0048(9) S(2) 4a 0.3378(3) 0.9075(3) 0.4999(4) 0.004(1) 0.015(1) 0.010(2) -0.0009(8) 0.004(1) -0.0019(8) S(3) 4a 0.1741(3) 0.5840(3) 0.0084(4) 0.008(1) 0.012(1) 0.010(1) -0.0017(8) 0.006(1) -0.0010(8) Correspondence author (e-mail: jonescy@oml.gov) Unauthenticated Download Date | 12/23/16 6:02 AM 328 Digall ium trisulfide Acknowledgment. We thank the College of Arts and Sciences of the University of Toledo for use of the X-ray diffractometer and computer facilities in the Arts and Sciences Instrumentation Center.

Refinement of the crystal structure of iron dibromide, FeBr2

Abstract: Br2Fe, trigonal, P3m\\ (No. 164), a = 3.776(1) Ä, c = 6.227(1 ) Ä , V= 76.9 A 3 , Z = 1, RgiF) = 0.057, wR^F) = 0.155, Τ = 293 Κ. Source of material The title compound FeBr2 was synthesized from iron metal and ammonium bromide [1], Single crystals were obtained by sublimation o f the sample at 773 Κ in an argon atmosphere. Discussion X-ray powder diffraction data have been known since 1929 [2]. W e report on the first single crystal data of iron dibromide. The compound crystallizes in the Cdfc-type structure (Pearson symbol hPi) and is isostructural with the high pressure phase of F e C b [3]. In References 1. Löwig, C.: Das Brom und seine chemischen Verhältnisse, Winter. Heidelberg 1829, p. 130. 2. Fenari, Α.; Giorgi, F.: La struttura cristallina dei bromuri di metalli bivalenti. Atti Accad. Naz. Lin. 9 (1929) 1134-1140. 3. Vettier, C.; Yelon, W. B.: The structure of FeCb at high pressure. J. Phys. Chem. Solids 36 (1975) 401-405. 4. Gregory, N. W.: The crystal structure of ferric bromide. J. Am. Chem. Soc. 73(1951)472-473. 5. Sheldrick, G. M.: SHELXL-97, a program for refining crystal structures. University of Göttingen, Germany 1997. Table 2. Atomic coordinates and displacement parameters (in Ä). Atom Site * y ζ Uu f/22 U33 U\\2 Uu Uu Fe la 0 0 0 0.027(1) Uu 0.051(3) Uu/2 0 0 Br 2d 2/3 1/3 0.2381(5) 0.0291(9) Uu 0.046(2) Una 0 0 * Correspondence author (e-mail: borrmann@cpfs.mpg.de)

Crystal structure of dibismuth selenium pentoxide, Bi2SeO5

Abstract: Bi205Se, orthorhombic, Abm2 (No. 39), a = 11.425(2) Ä, b = 16.244(3) Ä, c = 5.487(2)Ä, V= 1018.3 Ä 3 , Z = 8, RoJF) = 0.038, wÄrefiF) = 0.100, T= 293 K. Source of material Pure Bi2SeC>5 is obtained by sintering of stoichiometric mixtures of B12O3 and SeC>2 at 773 K. Single crystals can be prepared by chemical transport reactions with Br2 orSeOBr2 . Pure Bi2SeOs is sealed in evacuated quartz glass tubes with some mg of transport medium 100 Torr at transport temperature) and transported in a temperature gradient from 1023 Κ to 873 K. The transport rate in ampoules of 15 cm length and 1.5 cm diameter is about 0.10.2 mg/h. The crystals of Bi2Se05 are clear flat prisms of 1 to 2 mm length. We interpret the chemical transport corresponding to the thermal decomposition via: Bi2Se05.s + SeOBr2,g = 2BiSe03Brg (1) and Bi2Se05.s + Se02,g + Br2.g = 2BiSe03Brg + l/2C>2,g (2) analogue to the transport of Bi2Se3C>9, described before [1], Discussion The title compound is one of six at room temperature thermodynamically stable phases on the quasi binary section Bi203-Se02 . The structure of one of these phases Bi2Se309 we described recently [1]. The thermal decomposition of Bi2SeOs gives in the temperature region 873 Κ to 1073 Κ solid Bii6Se5C>34 and at temperatures higher than 1073 Κ solid BLtSeOe as well as in both cases gaseous SeC>2 [2], Bi2SeOs melts congruently at 1198 K, the decomposition pressure on this point reaches 2 atm. Bi2SeOs coexists in the oxygen-poorer region with Bii6Ses034/Bi202Se as well as Bi202Se/Sei and on the oxygen-richer side with Bi2Se309/Sei [2-4].The compound crystallizes in the acentric space group Abm2 (only the Bi and Se atoms are close to special positions of the corresponding centrosymmetric space group). Bi2SeC>5 is isotypic with Bi2TeOs [5]. The oxygen coordination spheres around the Bi cations are distorted tetragonal pyramids with Bi—Ο distances in the range of 2.06 Ä to 2.70 Ä. The crystal structure consists of layer packages, which lie parallel to the be plane. Table 1. Data collection and handling. Crystal: light yellow, flat prism. size 0.03 χ 0.11 χ 0.29 mm Wavelength: Mo Ka radiation (0.71073 Ä) μ: 761 cm\" Diffractometer, scan mode: Stoe-STADI4 CCD, φ/ω 28max: 58° /V(AW)measured, W>WJumque: 5863,1291 Criterion for I0bS, N(hkl)p. /„bs > 2 af/obsj, 1127 N(param)rer,ncd·· 79 Programs: SHELXS-97 [6], SHELXL-97 [7], DIAMOND [8] * Correspondence author (e-mail: otto.rademacher@chemie.tu-dresden.de) 30 Dibismuth selenium pentoxide Table 2. Atomic coordinates and displacement parameters (in A). Atom Site .t ν : U\\\\ V22 U}i V1: U U 2 ) Bid) 8 d 0.38938(5) 0.08543(3) 0.5090(2) 0.0126(3) 0.0123(3) 0.0134(5) -0.0013(2) -0.0004(5) 0.0022(3) Bi(2) 4c 0.12332(5) 1/4 0.5059(2) 0.0092(3) 0.0176(3) 0.0143(7) 0 -0.0032(5) 0 Bi(3) 4c 0.37888(6) 1/4 0.9701(2) 0.0101(4) 0.0115(3) 0.017(1) 0 0.0017(3) 0 Se(l) 8 d 0.1418(2) 0.08666(7) 0.0157(7) 0.0119(5) 0.0104(6) 0.014(1) 0.0001(4) 0.003(1) 0.0006(6) O(l) 8 d 0.2688(9) 0.0565(7) 0.890(2) 0.032(6) 0.035(5) 0.021(7) 0.013(5) 0.014(5) 0.007(5) 0(2) 4 b 1/2 0 0.719(3) 0.017(6) 0.012(5) 0.03( 1) 0.001(6) 0 0 0(3) 8 d 0.081(1) 0.1487(7) 0.804(3) 0.034(6) 0.034(6) 0.039(9) 0.001(5) 0.000(6) 0.027(6) 0(4) 4c 0.297(1) 1/4 0.607(3) 0.023(8) 0.033(7) 0.023(9) 0 -0.006(6) 0 0(5) 8 d 0.4877(8) 0.1619(4) 0.781(2) 0.016(5) 0.013(4) 0.011(5) 0.003(4) -0.004(4) -0.003(4) 0(6) 8d 0.195(1) 0.1550(7) 0.223(3) 0.026(6) 0.047(7) 0.030(8) -0.003(5) 0.003(6) -0.013(5) Acknowledgment. The authors thank H. Langhof, STOE & Cie Darmstadt for the re-measurement of the reflection data set with a Stoe-STADI4 CCD detector system and the indexing of the crystal faces for the numerical absorption correction.

Crystal structure of pyridine-2-carbaldehyde thiosemicarbazonium perchlorate, (C7H9N4s)(ClO4)

Abstract: C7H9CIN4O4S, triclinic, PI (No. 2), a = 7.556(1) A, b = 8.624(1) A, c = 8.966(1) Α, α = 104.836(3)°, β = 99.612(3)°, γ = 101.635(3)°, K= 538.2 A, Ζ = 2, RpfF) = 0.059, w/?ref(F\\) = 0.159, T = 110 Κ. Source of material To a solution of pyridine-2-carbaldehyde thiosemicarbazone ligand in methanol (10 ml) was added a aqueous solution of zinc nitrate and excess of sodium Perchlorate. The reaction mixture was stirred for 10 h at room temperature and left in room temperature for five days. The yellow crystals were filtered off, washed with cold methanol and ether and dried in vacuum over P4O10 (mp 488 K; yield 60%). Elemental analyses were consistent with the stiochiometry C7H9CIN4O4S. Melting points were measured on an Electrothermal 9100 apparatus and are uncorrected. Discussion The ligand of pyridine-2-carbaldehyde thiosemicarbazone possess a wide range of biological activity depending on the parent aldehyde or ketone. Heterocyclic thiosemicarbazones are important because of their possible beneficial biological activity. In the last twenty years, the metal complexes derived from this ligand have drawn some attention. In most of cases, the ligand is tridentate binding to the metal through the N-pyridine, N-azomethine and S atoms. The chemistry of complexes of this ligand markedly depends on the kind of transition metal ions. In the course of our studies of the syntheses and reactions of amidic and thioamidic derivatives ligands with zinc(II) salts [1,2], we have isolated an interesting adduct of pyridine-2-carbaldehyde thiosemicarbazone and perchloric acid. The adduct structurally characterized by X-ray crystallography. The C=S distance of 1.687(3) A agrees well with the values in the literature of 1.681(5) A, 1.679(4) A and 1 .678(3) A, being intermediate between the values of 1.82 A for a C—S single bond and 1.56 A for C=S double bond .The C—Ν distances of 1.365(3) A and 1.314(3) A are indicative for double-bond character. The bond angles N(3)-C( 1 )-S( 1) and N( 1 )-C( 1 )-S( 1) [ 124.5(2)° and 118.1(2)°, respectively] agree well with a participation of S in the hydrogen bond. The atom attached to amino Ν atom has the potential to act as a hydrogen donor. There are other numbers of hydrogen bonds that stabilize the crystal packing (see figure, lower part). In five of the seven hydrogen bonds the Perchlorate ion acts as the acceptor. Because of the high acidity of H7, it able to participate in hydrogen bonding. No π π ring stacking is observed within the crystals probably is as a result of the presence of Per-

Crystal structure of sodium iron(II) diaqua catena-[monoboro-diphosphate] monohydrate, NaFe(H2O)2[BP2O8] · H2O, and of potassium iron(II) diaqua catena-[monoboro-diphosphate] hemihydrate, KFe(H2O)2[BP2O8] · 0.5H2O

Abstract: BFeNaOi ιΡ2, hexagonal, P6,22 (No. 178), a = 9.467(2) Ä, c = 15.861(2) Ä, V= 1231.1 Ä, Ζ = 6, Rgt(F) = 0.049, wRrei(F ) = 0Λ\\2, Τ =293 Κ. BFeKOio.5P2, hexagonal, P6\\22 (No. 178), a = 9.523(1) Ä, c = 15.998( 1) Ä, V = 1256.5 A, Ζ = 6, R&(F) = 0.063, wRref(F) = 0.186, 7\" = 293 K. Source of material NaFe(H20)2[BP208]-H20 was prepared by hydrothermal treatment of mixtures of 0.29 g Na2B 4 O7l0H 2 O, 0.96 g NaH2P04 • 2H20, and 0.31 g FeCl2 · 4 H 2 0 (molar ratio 2:1:7). A concentrated aqueous solution of pH = 1 (1.5 ml 18% HCl) was held at 393 Κ for two weeks in a sealed glass ampoule (degree of filling 50%). KFe(H20)2[BP20g] 0 .5H 2 0 was prepared by hydrothermal treatment of mixtures of 0.12 g K2B4O7 ·4Η20,0.47 g NaH2P04, and 0.15 g FeCl2-4H20 (molar ratio 2:1:7). A concentrated aqueous solution of pH = 0.5 1 (1.5 ml 9% HCl) was held at 393 Κ for two weeks in a sealed glass ampoule (degree of filling 50%). Discussion The crystal structures of NaFe (H20)2 [BP20g]H20 and K F e ( H 2 0 ) 2 [ B P 2 0 g ] 0 . 5 H 2 0 b e l o n g to the f a m i l y of b o r o p h o s p h a t e h y d r a t e s wi th the g e n e r a l f o r m u l a Μ Μ\"(Η20)2[ΒΡ208]· xH 2 0 (M = Li, Na (χ = 1), Κ (x = 0.5); M n = Mg, Mn, Fe, Co, Ni, Zn) [1,2]. Both crystal structures differ mainly in the positions of the monovalent cations in the free threads of the helical i[BP20g~] ribbons and in the positions of water of crystallisation whithin the helical channels. Wheras the diameter of the Na helix (projection on the same z-value) is of nearly the same size to that of the Κ helix (6.40 Ä and 6.05 Ä, respectively), diameters for the water helices (0(6) whithin the channels) d i f f e r s igni f icant ly (Na-compound: 2 .43 Ä; K-compound: 1.87 Ä). 0(2) represents the aqua-ligands of the Fe04(H20)2 coordination octahedron. The 0(6) site in the potassium compound was found to be only half occupied [3]. Interatomic distances and angles within the tetrahedral helices are similar to known values for borophosphates [4,5]. 1. NaFe(H20)2[BP208] · HzO Table 1. Data collection and handling. Crystal: pale grey-purple, hexagonal bipyramid, size 0 .10x0 .10x0 .20 mm Wavelength: Mo Ka radiation (0.71069 Ä) μ: 23.35 cm\"' Diffractometer, scan mode: Phillips PW 1100, ω 26max: 44.86° Wf/lWjrneasurcd, N(hkl)miquc: 1780,540 Criterion for /<,bs, Nfftklfe: /obs > 2 a(/„bsX 470 N(param)„ r,ned: 75 Programs: SHELXS-97 [6], SHELXL-97 [7], DIAMOND [8] * Correspondence author (e-mail: kniep@cpfs.mpg.de ) 1 4 NaFe(H20)2[BP208] · H 2 0 and KFe(H20)2[BP208] · 0.5H20 Table 2. Atomic coordinates and displacement parameters (in A). Atom Site χ y c U\\\\ U22 U 33 U\\i U13 (/; 3 Na(l) 6 b 0.1950(6) 0.390(1) 1/4 0.109(6) 0.085(8) 0.054(6) t/22/2 0.008(5) 0 Fed) 6b 0.5508(1) 0.1016(2) 1/4 0.0112(9) 0.011(1) 0.008(1) U22/2 0.0019(8) 0 B(l) 6b 0.8478(9) 0.696(2) 1/4 0.012(7) 0.007(8) 0.009(9) U22/2 0.001(7) 0 P(l) 12 c 0.3891(3) 0.1674(3) 0.4154(2) 0.015(1) 0.012(1) 0.009(1) 0.005(1) 0.002( 1) 0.001(1) O(l) 12c 0.2158(8) 0.0203(7) 0.3998(4) 0.008(4) 0.006(3) 0.014(4) 0.001(3) -0.006(3) -0.003(3) 0(2) 12c 0.2949(8) 0.4909(8) 0.1120(4) 0.015(4) 0.018(4) 0.012(4) 0.006(3) -0.005(3) -0.006(3) 0(3) 12c 0.3884(9) 0.3148(8) 0.3807(4) 0.018(4) 0.009(4) 0.012(3) 0.006(3) 0.001(3) 0.000(3) 0(4) 12c 0.4201(7) 0.1820(7) 0.5122(4) 0.004(4) 0.008(4) 0.007(3) -0.001(3) 0.000(3) 0.001(3) 0(5) 12c 0.6199(8) 0.1355(8) 0.1219(4) 0.019(4) 0.012(4) 0.009(3) 0.011(3) 0.002(3) 0.002(3) 0(6) 6a 0.129(2) 0 0 0.09(1) 0.09(2) 0.25(3) U22P. 0.048(8) 2(7,3 2 . K F e ( H 2 0 ) 2 [ B P 2 0 8 ] · 0 . 5 H 2 0 Table 3. Data collection and handling.

Crystal structure of sodium nickel diaqua catena-[monoboro-diphosphate] monohydrate, NaNi(H2O)2[BP2O8] · H2O, at 293 K and 198 K

Abstract: BNaNiOi 1P2, hexagonal, P6i22 (No. 178), a = 9.377(1) Ä, c= 15.848(1) Ä, V= 1206.8 A, Ζ = 6, Rsl(F) = 0.028, wRref(F) = 0.074, T= 293 K. BNaNiOi 1P2, hexagonal, P6i22 (No. 178), a = 9.358(1) Ä, c = 15.833(1) k , V = 1200.7 Ä, Z = 6, R ^ F ) = 0.026, wRKf(F) = 0.070, Τ = 198 Κ. Source of material NaNi(H20)2[BP208] H 2 0 was prepared by hydrothermal treatment of mixtures of 0.29 g Na2B4O7 l0H2O, 0.96 g * Correspondence author (e-mail: kniep@cpfs.mpg.de) 12 N a N i ( H 2 0 ) 2 [ B P 2 0 8 ] · H 2 0 at 293 Κ and 198 Κ Table 2. Atomic coordinates and displacement parameters (in A). Atom Site χ ν ; U\\\\ U22 t/33 U\\i U\\\\ U2i Na(l) 6 b 0.1947(2) 2x 1/4 0.060(1) 0.049(2) 0.036(1) V i l l i 0.006(1) 0 Ni(l) 6b 0.55421(3) 2x 1/4 0.0127(2) 0.0130(2) 0.0120(2) U22/2 0.0007(2) 0 B(l) 6b 0.8477(2) I x 1/4 0.011(1) 0.012(2) 0.009(2) U22/2 0.000( 1) 0 PCD 12 c 0.39041(8) 0.17057(8) 0.41480(4) 0.0128(3) 0.0119(3) 0.0105(3) 0.0058(2) 0.0007(2) -0.0001(2) 0(1) 12c 0.2148(2) 0.0220(2) 0.4001(1) 0.0144(9) 0.0093(8) 0.0167(9) 0.0040(7) -0.0024(7) 0.0002(7) 0(2) 12c 0.2923(3) 0.4927(3) 0.1108(1) 0.0157(9) 0.021(1) 0.0177(8) 0.0087(8) -0.0013(7) -0.0023(8) 0(3) 12c 0.3875(3) 0.3194(3) 0.3806(1) 0.024(1) 0.0121(9) 0.0145(8) 0.0101(8) 0.0017(8) 0.0014(7) 0 (4 ) 12c 0.4192(2) 0.1835(2) 0.5126(1) 0.0127(8) 0.0164(9) 0.0086(7) 0.0060(7) 0.0005(6) -0.0014(6) 0(5) 12c 0.6193(2) 0.1374(3) 0.1233(1) 0.0148(9) 0.020(1) 0.0126(8) 0.0088(8) 0.0034(7) 0.0008(7) 0(6) 6a 0.1359(7) 0 0 0.051(3) 0.072(4) 0.182(8) U22/2 0.031(3) 2 U , 3 2. NaNi(H20)2[BP208] · HzO, Τ = 198 Κ Table 3. Data collection and handling.

Refinement of the crystal structure of gallium trifluoride, GaF3

Abstract: F 3 G a , trigonal, R3c (No . 167), a = 5 . 0 1 2 ( 4 ) A , c = 12 .99 (1 ) Ä , V= 2 8 2 . 6 Ä 3 , Z = 6, R&(F) = 0 . 0 2 2 , w R n f i F 2 ) = 0 .053 , T = 2 9 3 K. Source of material G a F 3 m a y be obtained through the reaction o f ga l l ium metal (Ventron 4 N ) with NH4F (Merck, 9 9 , 8 %, recrystal l ized from C H 3 O H to remove traces o f water) in the molar ratio o f 1:3 in a sea led M o n e l container. T h e reaction temperature is 7 4 8 Κ with a crystal l izat ion t ime o f s ix weeks . Colour less square shaped nearly cub ic crystals are obtained [1]. Table 2. Atomic coordinates and displacement parameters (in Ä). References 1. Roos, M.: Aufbau und Abbau komplexer Ammoniumfluorometallate der Elemente Aluminium, Gallium und Indium unter Ammoniakatmosphäre. Dissertation, Universität zu Köln, Germany 1999. 2. Brewer, F. Μ.; Garton, G.; Goodgame, D. M. L.: The preparation and crystal structure of gallium trifluoride. J. Inorg. Nucl. Chem. 9 (1959) 56. 3. Sheldrick, G. M.: SHELXS-97-2, Program for the Solution of Crystal Structures. University of Göttingen, Germany 1997. 4. Sheldrick, G. M.: SHELXL-97-2, Program for Crystal Structure Refinement. University of Göttingen, Germany 1997. 5. Brandenburg, K.: Diamond (Version 2.1 a). Crystal Impact GbR, Germany 1996-1999. Atom Site X ίΖ Un U22 t/33 U η t / n Uli Ga 6b 0 ο 0 0.0033(4) U η 0.0030(5) 0.0016(2) 0 0 F 18e 0.0591(3) jc-1/3 1/12 0.0090(7) U ι. 0.0083(7) 0.0057(7) -0.0020(3) -Uli * Correspondence author (e-mail: gerd.meyer@uni-koeln.de)

Crystal structure of 2,6-diaminopyridinum bis(2,6-pyridinedicarboxylato) chromium(III) 2,6-pyridinedicarboxylic acid hemihydrate, C26H18CrN6O12 · 0.5H2O

Abstract: C26H2oCrN6012.50, monoclinic, P\\2\\lc\\ (No. 14), a = 15.233(4) A,b = 25.208(6) Ä, c = 14.685(3) Ä, β = 103.893(5)°, V = 5474.0 Ä, Z = 8, Rgl(F) = 0.057, wRM(F) = Q.\\5\\,T = 110 K. Source of material The title compound was synthesized by the reaction between ligand LH2, [H2pyda][pydc]~, (pyda = 2,6-pyridinediamine and H2pydc = 2,6-pyridinedicarboxylic acid) that is a new se l f -assembl ing sys tem [1], and chromium(I I I ) chlor ide hexahydrate in water. The resulting violet solution was left to slow concentration at room temperature. After five days, dark red block shaped crystals were isolated.

Crystal structure of 4-methylphenylboronic acid, C7H9BO2

Abstract: C7H9BO2, orthorhombic, I b a l (No. 45), a = 17.016(5) A, £>= 19.164(5) A , c = 9.722(5) A, V= 3170.3 A 3 , Z = 16, R g t ( F ) = 0.064, w R t e r f F 2 ) = 0.204, T = 293 K. Source of material The Grignard reagent, p-bromotoluene, was reacted with tri-methoxy-borane, B(OMe)3 in anhydrous THF in a modified literature procedure [1-3], and the resulting product alter work up was made anhydrous by azeotropic removal of the water to collect colorless crystalline solid in 71% yield.

Crystal structure of trisodium holmium(III) hexachloride, Na3HoCl6

Abstract: Cl6HoNa3, monoclinic, P\\2\\ln\\ (No. 14), a = 6.8683(9) Ä, b = 7.274( 1) Ä, c = 10.167( 1) Ä, β = 90.79(2)°, V = 507.9 Ä, Ζ = 2, RRt(F) = 0.017, wRKf(F) = 0.044, 7 = 293 K. Source of material Single crystals of Na3HoCl6 were obtained during numerous attempts to reduce H0CI3 with sodium metal (HoCb:Na =1:1 ; tantalum container, 873 K) [1,2], Discussion Na3HoCl6 crystallizes with the cryolite type of structure (Na3AlF6 [3]). Isotypic are a number of analogous ternary chlorides, Na3MCl6 (M = Dy-Lu, Y, Sc) [4], Table 1. Data collection and handling.

Crystal structure of 4-hydroxy-3-methoxybenzaldehyde-4-nitrophenyl-hydrazone, C14H13N3O4

Abstract: C14H13N3O4, monoclinic, P\\2\\ln\\ (No. 14), a = 12.593(2) Ä, b = 6.9910(9) Kc= 15.765(2) Ä, β = 107.661(6)°, V = 1322.5 Ä, Ζ = 4, RpfF) = 0.043, wR^F) = 0.096, 7=291 K. Source of material The title compound was synthesized by condensation of equimolar ratio of 4-hydroxy-3-methoxybenzaldehyde and 4-nitrophenylhydrazine in ethanol solution. Some drops of acetic acid were added as a catalyst according to known procedure [1]. Both starting materials are commercially available. The orange crystals are obtained from the dark red ethanol solution by cooling. The product was isolated and recrystallized from glacial acetic acid (mp 505 Κ 506 Κ). The crystals were grown by slow evaporation from glacial acetic acid within two days. Experimental details For the methyl group, hydrogen atoms were placed in calculated positions with UtSo constrained to be 1.5x£/eq of the carrier atom, and for the remaining hydrogen atoms 1.2 χί/eq of the corresponding carrier atom. Discussion In the course of our investigations on organic nonlinear optical (NLO) materials we now determined the crystal structure of the title compound. The asymmetric unit of the crystal contains one formula unit C14H13N3O4. The molecule is nearly planar with distances and angles in the normal range. The molecules are linked by Ο—Η· Ο, N—HO and C — H 0 hydrogen bonds (d(02—H2 0 4 ) = 2.892(2) Ä, Z O H O = 162°; d(N2—H2A· 0 3 ) = 3.105(3) Ä, Z N H O = 166°; rf(C10—H10· 02) = 3.372(3) Ä, Z C H O = 160°). Table 1. Data collection and handling. Crystal: orange plate, size 0.2 χ 0.4 χ 0.5 mm Wavelength: Mo Ka radiation (0.71073 A) μ: 1.08 cm\" Diffractometer, scan mode: Nonius KappaCCD, 208 frames, Δω = 1°

Crystal structure of tris(acetylacetonato)iron(III), C15H21O6Fe, at 20 K

Abstract: CisHiiOeFe,, Pbca (No. 61), a = 16.561(3) A, b = 15.434(4) A, c = 13.578(3) A, V= 3470.6 A, Z = 8, Rgi(F) =0 .053 , wRdbs(F) = 0.059, Τ = 20 Κ. Source of material 3 mmol imidazole was dissolved in 10 mL water, and 1 mmol (NH4)2Fe(SC>4)2 · H2O was also dissolved in 10 mL water. The two solitions were mixed to give green precipitate, then 10 mL acetylacetone was added into above mixture with stirring at room temperaure. When the precipitate had entirely dissolved, the solution clanged its color from green to deep red, and the reaction mixture was filtered. The filtrate stood for six days until the red single cystals were obtained. Experinental details The stricture was solved by Patterson method followed by Fourier synheses. Η atoms were located in a difference Fourier map, and ther coordinates and thermal parameters were fixed during structuD refinement. Discusson Ferric aid ferrous ions exist broadly in various organisms, and play imjortant roles in bewildering array of proteins [ 1 ]. They relate closely to many functions such as O2 storage in yoglobin, O2 transport in hemoglobin, oxidation of inactivated carbonhydrogm bonds in cytochrome P450, oxygen reduction in cytochromeC oxidase and so on [2,3]. Consequently, much interest has beei focused on their complexes [4]. What is more, the ß-dion« find a variety of laboratory uses and many industrial application and have contributed a lot to the present understanding of sterii pressure and conformers, prototropy and tautomerism, chelate brmation, and intramolecular bonding [5]. So we use ferric ion andacetylacetonato anion as center ion and ligand respectively to synthesize the title complex and report its crystal structure herein. The molecular structure of the title complex with the atom numbering scheme is illustrated in the figure (left, 50% probability displacement elipsoids). In a molecule of the title complex, six oxygen atoms from three bidentate acac anions coordinate to a ferric ion to complete the coordination geometry of a six-coordinated octahedron around the ferric ion. It is worthy to take a look at the distances and angles around ferric ion in this complex. The bond angles of 0 ( l ) -Fe -0 (4 ) , 0(3)-Fe-0(6) , 0(2)-Fe-0(5) , are 176.4(1)°, 175.0(1)°, 173.5(1)°, respectively, which are all smaller than 180°. On the other hand, the bond distances of all the Fe—O, namely Fe—0(1) [2.004(3) A], Fe—0(2) [1.996(3) A], Fe—0(3) [1.995(3) A], Fe—0(4) [1.977(3) A], Fe—0(5) [1.985(3) A], Fe—0(6) [1.992(3) A ], are not equal to each other. Therefore, the coordination geometry formed by six oxygen atoms is a distorted octahedron. A ß-diketonate anion coordinate usually to a metal cation in a chelate fashion [6]. The bond distances of O(l)—C(2), 0(2)—C(4), C(2)—C(3) and C(3)—C(4) are 1.274(6) A, 1.258(6) A, 1.381(7)Aand 1.390(7) A, respectively, which are in range between the single and double bond distances. It shows that there exists conjugated structure in each coordinated ß-diketonate anion acac, which leads to the delocalization of electron density of the coordinated ß-diketonate structure. Whereas, the annular and exocyclic C—C distances are on average 1.385 A and 1.504 A, respectively, which are the main deviations from those observed at room temperature (1.377 A and 1.530 A, respectively) [7]. The mean values of annular and exocyclic O C C angle for the title compound at 20 Κ are 124.2° and 115.6 , respectively, and those observed previously [7] at room temperature are 125.0° and 114.9 , respectively. The other bond lengths and angles are almost the same in spite of the temperature difference. All in all, three acac coordinates concurrently to a ferric ion to result a distorted octahedron of the title complex with three six-membered rings. The plane through 0 ( 1), 0(2) and Fe joints to the plane through 0(3), 0(4) and Fe at an angle of 86.49°, to the plane through 0(5), 0(6) and Fe at an angle of 78.91°. In the molecular packing, separate molecules insert with each other by the ramose six-membered ring. Table 1. Data collection and handling. * Grrespondence author (e-mail: zhimin-j@163.net) Crystal: red prismatic, size 0.20 χ 0.20 χ 0.30 mm Wavelength: Mo Ka radiation (0.7107 A) μ: 89.13 cm" 1 Diffiractometer, scan mode: Rigaku AFC7R, ω/2θ 26rT1ax • 54.98° N(hkl)mcasuKd, WlA/)unique: 3944,3744 Criterion for lobs, N(hkl)p: U s > 2.5 σί/obsA 1920 N(param)nfiaai· 200 Programs: SHELXS-86 [8], teXsan [9]

The crystal structure of 1,2-bis(diphenylphosphino)ethane at 173 K, [Ph2PCH2CH2PPh2]

Abstract: C26H24P2, monoclinic, P\\2\\ln\\ (No. 14), a = 13.077(4) A, b = 5.476(2)Ä, c = 16.137(2)Ä, β = 110.96(2)°, V= 1079.1 Ä, Ζ = 2, Rgi 3 of/obs), 1846 N(param)rcrmed'· 175 Programs: TEXSAN [2], DIRDIF92 PATTY [3], PLATON [4] Table 2. Atomic coordinates and displacement parameters (in A). Atom Site X y ζ i/iso H(l) 4e 0.1139(9) -0.045(2) 0.5520(8) 0.034(3) H(2) 4e 0.0483(9) -0.184(2) 0.4649(7) 0.029(3) H(12) 4e 0.239(1) -0.219(3) 0.493(1) 0.067(5) H(13) 4e 0.396(1) -0.355(3) 0.472(1) 0.093(6) H(14) 4e 0.463(1) -0.122(3) 0.377(1) 0.078(6) H(15) 4e 0.370(1) 0.225(3) 0.305(1) 0.103(7) H(16) 4e 0.214(1) 0.358(3) 0.329(1) 0.072(5) H(22) 4e 0.037(1) -0.149(2) 0.2891(8) 0.040(4) H(23) 4e -0.100(1) -0.191(3) 0.1469(9) 0.056(4) H(24) 4e -0.236(1) 0.121(3) 0.0996(9) 0.057(4) H(25) 4e -0.235(1) 0.453(3) 0.1892(9) 0.066(5) H(26) 4e -0.094(1) 0.490(2) 0.3280(8) 0.044(4) Atom Site U11 U22 i/33 U12 U is ί / 2 3 P(l) 4e 0.09255(2) 0.21364(6) 0.43222(2) 0.0279(2) 0.0342(2) 0.0235(1) -0.0037(1) 0.0077(1) -0.0010(1) C(1) 4e 0.05361(9) -0.0312(2) 0.49365(8) 0.0281(6) 0.0351(7) 0.0221(6) 0.0004(6) 0.0081(5) 0.0012(5) C( l l ) 4e 0.21171(9) 0.0823(2) 0.41417(8) 0.0250(6) 0.0443(8) 0.0249(6) -0.0071(6) 0.0078(5) -0.0057(6) C( 12) 4e 0.2661(1) -0.1261(3) 0.4539(1) 0.0369(8) 0.061(1) 0.0483(9) 0.0072(7) 0.0192(7) 0.0049(8) C(13) 4e 0.3595(1) -0.2038(4) 0.4393(1) 0.0389(9) 0.081(1) 0.068(1) 0.0137(9) 0.0185(8) -0.004(1) * Correspondence author (e-mail: edward.tiekink@adelaide.edu.au) 70 l ,2-Bis(diphenylphosphino)ethane Table 3. Continued Atom Site X V c t'll Ο22 f/33 U\\2 Ud Ui) C(14) 4i 0.3987(1) -0.0743(4) 0.3849(1) 0.0350(9) 0.106(2) 0.069( 1) -0.006( 1) 0.0263(9) -0.029(1) C(15) 4e 0.3454(2) 0.1303(5) 0.3445(1) 0.061(1) 0.110(2) 0.080(1) -0.016(1) 0.050(1) 0.002(1) C(16) 4e 0.2530(1) 0.2119(3) 0.3592(1) 0.0496(9) 0.070( 1) 0.064( 1) -0.0042(9) 0.0322(8) 0.013(1) C(21) 4e -0.01363(9) 0.1745(2) 0.32198(7) 0.0269(6) 0.0324(7) 0.0224(5) -0.0029(5) 0.0078(5) 0.0041(5) C(22) 4e -0.0170(1) -0.0250(3) 0.26785(8) 0.0318(7) 0.0427(8) 0.0299(7) 0.0036(6) 0.0078(5) -0.0020(6) C(23) 4e -0.0985(1) -0.0466(3) 0.18474(9) 0.0419(8) 0.0531(9) 0.0289(7) -0.0025(7) 0.0088(6) -0.0060(7) C(24) 4e -0.1781(1) 0.1308(3) 0.15575(9) 0.0413(8) 0.060( 1) 0.0284(7) -0.0053(8) -0.0015(6) 0.0077(7) C(25) 4e -0.1774(1) 0.3271(3) 0.2093(1) 0.0472(9) 0.046( 1) 0.0463(9) 0.0102(8) -0.0037(7) 0.0096(8) C(26) 4e -0.0949(1) 0.3488(3) 0.29203(9) 0.0435(8) 0.0332(8) 0.0392(8) 0.0036(6) 0.0051(6) 0.0012(6) Acknowledgment. The Australian Research Council is thanked for support. References 1. Pel izzi , C.; Pel izzi , G.: Crystal s t ructure of two forms of l,2-bis(diphenylphosphino)ethane. Acta Crystallogr. B3S (1979) 17851790. 2. teXsan: Single Crystal Structure Analysis Software. Version 1.04. Molecular Structure Corporation. The Woodlands, TX, USA 1997. 3. Beurskens. P. T.; Admiraal, G.; Beurskens. G.: Bosman. W. P.; Garcia-Granda, S.: Gould. R. O.; Smits. J. Μ. M.; Smykalla. C.: The DIRDIF program system. Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands 1992. 4. Spek, A. L.: PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands 2000; http://www.cryst. chem.uu.nl/platon/.

Crystal structure of palladium selenide, PdSe

Abstract: PdSe, tetragonal, PA-Jmbc (No. 135), a = 11.5646(6) Ä, c = 6.9978(6) Ä, V= 935.9 Ä, Ζ = 24, R&(F) = 0.034, wRref(F) = 0.093, T= 153 K. Source of material Single crystals of PdSe were obtained in the reaction of Bi (0.0819 g, Alfa, 99.9%), Pd (0.1252 g, Johnson Matthey, 99.95%), and Se (0.0929 g, Alfa, 99.5%). The elements were thoroughly mixed and sealed in a carbon-coated fused-silica tube that was then evacuated to 5-10 -5 Torr. A computer-controlled furnace was used to heat the sample from 300 Κ to 923 Κ in 48 h. This temperature was maintained for 72 h and then the sample was quenched to room temperature in water. Black block-like single crystals of PdSe were found. Qualitative energy dispersive spectroscopy (EDS) analysis indicated the presence of Pd and Se but not of Bi. Discussion X-ray powder diffraction studies of PdSe [ 1,2] led to a tetragonal structure of the PdS type. The structure of PdS was reinvestigated and found to crystallize in the tetragonal space group Pb-Jm [3]. The study of PdS ι -xSex mixed phases (0 < χ < 1) [4] showed that the PdS-type mixed crystals are stable only in the ranges 0.0 < χ < 0.2 and 0.9 < χ < 1; for 0.2 < χ < 0.9 PdSi-xSex crystallizes in the space group PA^mbc. Here we report the first single-crystal study of the title compound, PdSe. This binary compound crystallizes in space group PA^mbc and consequently is not isostructural with PdS. A perspective view of PdSe along [001] is shown in the figure. There are three crystallographically unique Pd atoms. Each of these sits in a slightly distorted square-planar environment. Each of the two crystallographically independent Se atoms is coordinated by a distorted tetrahedron of Pd atoms. The Pd Se distances range from 2.4039(7) Ä to 2.4683(8) Ä, and are consistent with those observed in square-planar PdSe4 environments. Table 1. Data collection and handling. Crystal: Wavelength: μ: Diffractometer, scan mode: 2Θπμ*: W(AM)measured, N(hkl)anique: Criterion for /<>bs, N(hkl)gC N(param)nr,txA'. Program: black block, size 0.130 χ 0.178 χ 0.250 mm Mo Ka radiation (0.71073 Ä) 345.43 cm\" Broker SMART CCD, Δω = 0.3° 57.58° 7424,639 U s > 2 a(lobs), 629 33 SHELXTL [5] Table 2. Atomic coordinates and displacement parameters (in A). Atom S i t e X y ζ Uu U22 t/33 U12 1 / 1 3 U23 P d ( I ) 8/i 0.04507(6) 0.13065(5) 0 0.0076(4) 0.0090(4) 0.0029(4) 0.0006(2) 0 0 Pd(2) 8ft 0.23178(6) 0.35785(6) 0 0.0075(4) 0.0089(4) 0.0032(4) 0.0006(2) 0 0 Pd(3) 8« 0.11259(4) ;c+l/2 1/4 0.0072(3) Uu 0.0061(4) -0.0002(2) -0.0002(2) -Uu Se(!) 16/ 0.17697(5) 0.11009(5) 0.27523(9) 0.0076(4) 0.0079(4) 0.0032(4) 0.0003(2) 0.0000(2) 0.0001(2) Se(2) 8 g 0.59667(6) jc+1/2 1/4 0.0078(3) Uu 0.0046(5) -0.0002(3) 0.0001(2) -Un * Correspondence author (e-mail: ibers@chem.northwestern.edu) 486 Palladium selenide Acknowledgments. This research was supported by NSF Grant DMR0096676. Use was made of the Central Facilities supported by the MRSEC program of the National Science Foundation (DMR0O-76O97) at the Materials Research Center of Northwestern University.

Crystal structure of tetrarubidium dichloride monooxide, Rb4(Cl2O)

Abstract: Cl2ORb4, cubic, /43d (No. 220), a = 9.521(3) Ä, V= 863.1 Ä, Ζ = 4, Rgi(F) = 0.077, wRKi(F) = 0.155, T= 293 K. lower symmetryjndicate no ordering in the anionic partial structure, as e.g. in I42d where the Th-position is split in two positions (2:1 ratio). The same features have been reported for several other compounds as CdRE2X4 (RE = La, Ce, Pr, Nd, Sm; X = S, Se, Te) [1], CaYb2S4 [2], E114X2Y (X = P, As, Y = S, Se), Eu4X2Te (X = As, Sb, Bi) and M4Bi2Te (M = Sm, Yb, Ca) [3], In Rb4Cl20, Rb is surrounded by an octahedron of anions (Cl/O), which is slightly distorted by the influence of the nearest Rb cations located above three of the triangular polyhedral faces. For Cl/O a 4 + 4 coordination by Rb cations i s found which can be best described by a distorted dodecahedron. Table 1. Data collection and handling. Crystal: Wavelength: μ: Diffractometer, scan mode: 2ömax: WAdmeasured, WlM/unique: Criterion for /obs, N(hkl)p. N(param)n fined: Programs: pale yellow, irregular, size 0.09 χ 0.08 χ 0.06 mm Mo Ka radiation (0.71070 A) 233.89 cm\" Broker SMART, ω 39.5° 1762,65 /obs > 2 o ( W , 58 7 SHELXL-97 [4], DIAMOND [5] Source of material Single-phase, pale yellow Rb 4Cl 20 is obtained by reacting a homogenous mixture of the appropriate amounts of R b 2 0 and RbCl in a sealed silver crucible under argon atmosphere at 673 Κ within a few hours (thermoanalytic investigation show an onset for the reaction at 660±10 K). The basic compound decomposes in air immediately under formation of carbonates and hydroxides. Experimental details The relative large / lvalues are a consequence of the poor quality of the crystal studied and of a low signal/noise ratio. Discussion Rb4Cl20 crystallizes in the anti-Th3P4 type of structure where both anions, chlorine and oxygen, share the thorium position (12a) in a ratio of 2:1. Structure refinements in space groups of Acknowledgment. Dr. Jürgen Nuss is gratefully acknowledged for collecting the single crystal data. References 1. Aliev, Ο. M.; Agaev, A. B.; Azadaliev, R. Α.: Synthesis and properties of CdLn2X4 (X = S, Se, Te) and CdLruS? chalcogenides. Inorg. Mat. USSR 33(1997) 1123-1127. 2. Li, R.-Y.; Lange, Κ. G.; Andratschke, M.; Range, K.-J.: Crystal structure of calcium ytterbium sulphide (1/2/4), high pressure modification, CaYbiS. Z. Kristallogr. 211 (1996) 814. 3. Hulliger, F.: New ternary anti-Th3P4 europium compounds. Mat. Res. Bull. 14 (1979) 259-262. 4. Sheldrick, G. M.: SHELXS-97. Program for solving and refining crystal structures, University of Göttingen, Germany 1997. 5. Brandenburg, K.: Diamond Version 2.0f. Crystal Impact GbR, Bonn, Germany 1998. Table 2. Atomic coordinates and displacement parameters (in A). Atom Site U π 1/22 1/33 U12 U ,3 Uli Rb 16c 0.0656(4) * .r 0.115(4) Uu U11 0.000(3) U12 i/12 E° 12a 3/8 0 1/4 0.10(2) 0.042(7) U22 0 0 0 a: Ε = 2/3CI + 1/30 * Correspondence author (e-mail: mudring@web.de)

Crystal structure of piperazine bis(aquapentafluorotitanate), (C4H12N2)[TiF5(H2O)]2

Abstract: Two types of novel framework materials, including six organically templated silicogermanates and five hybrid fluorotitanates, have been synthesized, and their structures have been determined by single crystal X-ray diffraction. Their structures and the interactions between the organic and inorganic species are discussed in some detail.The frameworks of the six silicogermanates, SU-9, SU-10, SU-11, SU-12, SU-14 and SU-21, are built up from either tetrahedra exclusively, or from mixed polyhedra. SU-9, SU-10 and SU-11 consist only of tetrahedra, and SU-12, SU-14 and SU-21 are built up from mixed polyhedra. In all silicogermanates, Si and Ge share the tetrahedrally coordinated positions, and only Ge occupies the 5- and 6-coordinated positions.The frameworks of SU-9, SU-10 and SU-11 belong to zeolite frameworks. SU-9 and SU-10 are built up from the same periodic building units (PBUs) that are formed by 4/4-4 units, and they adopt the known zeolite framework types AST and ASV, respectively. SU-11 is built up from 5-1 units and adopts the known zeolite framework type MFI. This is the first time that the frameworks of AST, ASV and MFI have been prepared in silicogermanate form.The 3-D frameworks of SU-12 and SU-14 contain (Ge,Si)7 composite building units that form one-dimensional 24-ring channels along the c axis. Their structures contain intersecting channels. SU-12 contains 8-, 10- 12- and 24-ring channels; while SU-14 has 9-, 10-, 12- and 24-ring channels. SU-21 is a two-dimensional framework structure containing 10-ring channels. It is the first silicogermanate with the template covalently bonded to Ge.All silicogermanates were synthesized by using organic amines as templates. The templates play a very important role in directing the structure of the inorganic framework.The obtained five hybrid fluorotitanates are SUF-1, SUF-2, SUF-3, SUF-4 and SUF-5. Their hybrid frameworks are built up from fluorotitanate anions, N-containing cations and crystal water/oxonium cations. Zero-dimensional fluorotitanate clusters are normally obtained when cyclic organic amines such as 1,4-diazabicyclo[2,2,2]octane (DABCO) and piperazine are used. Increasing the pH value of the starting solutions led to more condensed fluorotitanate anions, from isolated octahedra to pairs and eventually chains of octahedra. The formation of the hybrid frameworks of fluorotitanates is strongly dependent on hydrogen bonds between the fluorotitanate anions, N-containing organic cations and water molecules/oxonium ions.

Crystal structure of lithium zinc diaqua catena-[monoboro-diphosphate]- monohydrate, LiZn(H2O)2[BP2O8] · H2O

Abstract: BLiOnP2Zn, hexagonal, Ρ6ι (No. 169), a = 9.469(2) Ä , c = 15.667(2) Ä , V = 1216.6 Ä 3 , Z = 6, Rgl(F) = 0.031, wRref(F2) = 0.086, Γ = 2 9 3 Κ. Source of material LiZn(H20)2[BP2C>8]-H20 was prepared by hydrothermal treatment of mixtures of 1.30 g L12B4O7,6.40 g L1H2PO4, and 0.63 g ZnO (molar ratio 1:8:1). A concentrated aqueous solution of pH = 1 1 . 5 (H3PO4) was held at 443 Κ for two weeks in a teflon autoclave (20 ml, degree of filling: 50%) Discussion The crystal structure of LiZn(H20)2[BP208j H20 contains infinite one-dimensional anionic partial structures. The condensation of BO4 and PO4 tetrahedra through common vertices leads to tetrahedral ribbons i[BP2083 _], which are arranged around 61 screw axes to from helical arrangements. The spiral ribbons are built up from four-membered rings in which BO4 and PO4 groups alternate. Each BO4 tetrahedron belongs to the adjacent four-ring of tetrahedra along the ribbon in such a way that all vertices of the BO4 groups participate in bridging functions with PO4 tetrahedra. The phosphate groups occupy the borders of the ribbons with two terminal oxygen atoms. Bond lengths and angles within the anionic partial structure are consistent with related borophosphates (see [1,2] and refs. herein). The free loop of the borophosphate helix is occupied by Li + in a tetrahedral coordination by oxygen atoms from adjacent phosphate groups and water molecules (0(3)h20, 0(10)h2o). The double helix {Li[BP208]2~} is completed forming a central channel running along the 61 screw axis, and which is filled with water of crystallization (0(3)h2o) resulting in the formula LiZn(H20)[BP20e]-2H20. The water molecules form hydrogen bonds (0(3)h20 · · · 0(3)h20 = 3.04 Ä) with each other along the spiral. Zn 2 + is in an octahedral coordination ( Z n — Ο = 2.050(5) 2 . 3 4 1 ( 3 ) Ä ; see also [3]) by oxygen functions of P O 4 groups and water molecules ( 0 ( 1 0 ) h 2 0 and

Crystal structure of silver chloride chromate (VI), Ag3ClCrO4

Abstract: Ag3ClCr04, tetragonal, PAInmm (No. 129), a = 7.3889(5) Ä, c = 5.3065(3) Ä , V = 289.7 Ä 3 , Ζ = 2, Rgt(F) = 0.042, wRrefiF2) = 0.097, T= 293 K. Source of material Single crystals of AgjCrCUCl have been prepared by solid state reaction of a mixture of A g 2 0 and elemental Cr (molar ratio 3 : 2 ) under an elevated oxygen pressure. The mixture was annealed for 30 h in silver crucibles placed in stainless-steel autoclaves [1] using 2 ml of 3% HCIO4 as an accelerator. The reaction temperature and oxygen pressure were 753 Κ and 100 MPa, respectively. Discussion AgjCrCUCl was first obtained as a by-product of different syntheses aiming at ternary silver oxides in steel autoclaves with per-chloric acid as an accelerator. The crystal structure can be described as an anti-perowskite with CrCU-tetrahedra at Ca-sites, CI at Ti-sites and A g at O-sites showing a close structural relationship to Cd j0 (S i04 ) [2], which crystallizes in the same space group, and the C S 3 C K C 0 C I 4 ) type [3,4]. The CI atom is displaced from the center of its surrounding Ag6 octahedron along [001 ] resulting in a 5 + 1 coordination of the chlorine atom. Table 1. Data collection and handling. Crystal: red cube, size 0.05 χ 0.08 χ 0.10 mm Wavelength: Mo Ka radiation (0.71069 A ) μ: 121.97 cm\" 1 Diffractometer, scan mode: Bniker AXS, ω/2θ 20max: 69.96° Admeasured, N(hkl)unique: 2887, 390 Criterion for /obs, N(hkl)g\\. lobs > 2 af/obs), 382 N(param)rci,„cd'. 20 Programs: SHELXL-97 [51, DIAMOND [6] References 1. Linke, C.; Jansen, Μ.: Über AgiSnOi, das erste Silberstannat. Ζ. Anorg. Allg. Chem. 623 (1997) 1441-1446. 2. Eysel, W.: Kristallchemie von Oxoverbindungen, Α3θ(Βθ4). Neue Jahrbücher der Mineralogie, Monatshefte 1970 (1970) 534-547. 3. Powell, Η. M.; Wells, A. F.: The Structure of Cesium Cobalt Chloride (CS3C0CI5). J. Chem. Soc. 1935 (1935) 359-369. 4. Mansmann, M.: Die Kristallstruktur von Tribariumpentaoxometallaten ( IV) und isotyper Verbindungen. Ζ. Anorg. Allg. Chem. 339 (1965) 52-56. 5. Sheldrick, G. M.: SHELXL-97. Program for refining crystal structures. University of Göttingen, Germany 1997. 6. Brandenburg, K.: Diamond Version 2.1a. Crystal Impact GbR, Bonn, Germany 1999. Table 2. Atomic coordinates and displacement parameters (in A2). Atom Site X y Ζ t/n U22 t/33 t/12 f/|3 Uu A g ( l ) 2c 0 1/2 0.1010(1) 0.0310(3) Uu 0.0232(3) 0 0 0 Ag(2) 4e 1/4 1/4 1/2 0.0438(3) Uu 0.0486(4) 0.0181(2) -0.0050(1) u 13 Cr ( l ) 2a 0 0 0 0.0174(3) Uu 0.0246(6) 0 0 0 O ( l ) 81 0 0.1793(5) 0.1849(8) 0.063(2) 0.023(1) 0.043(2) 0 0 -0.006(1) C l ( l ) 2c 0 1/2 0.6267(3) 0.0375(6) Uu 0.0200(7) 0 0 0 * Correspondence author (e-mail: martin@jansen.mpi-stuttgart.mpg.de)

Crystal structure of diaqua-bis[N-(2-pyridyl)carbonylaniline]zinc(II) diperchlorate, Zn(C12H16N2O)2(H2O)2(ClO4)2

Abstract: C24H24CI2N4O12Z11, monoclinic, P12|/nl (No. 14), a = 8.262( 1) Ä, b = 11.847(2) Ä, c = 14.885(2) Ä, β = 103.368(6)°, V= 1417.4 Ä, Z = 2, RpfF) = 0.062, wRref(F) = 0.169, Τ110 K. Source of material yV-(2-pyridyl)carbonylaniline was synthesized in accordance with published procedure [1]. The colorless crystals of the title compound were obtained from the reaction of hydrated Zn(NC>3)2 with yV-(2-pyridyl)carbonylaniline ligand in excess of NaClCU and in a molar ratio of 1:2 in water solution. The resulting colorless solution was heated and stirred for about an hour. Then, it was left to evaporate at room temperature and, after a few days, colorless crystals were isolated, mp 673 K. Yield: 50%. Elemental analyses were consistent with the formula C24H24Cl2N40i2Zn (found: C, 40.8%; H, 3.3%; N, 8.19%. calc.: C, 41.3%; H, 3.4%; N, 8.04%). Discussion As a ligand with potential Ο and Ν donors, N-(2-pyridyl)carbonylaniline is interesting not only because of the structural chemistry of its multifunction coordination modes (the presence of a pyridyl nitrogen at the adjacent position of the amide linkage helps the ligand to bind to metal ion in a bidentate fashion forming a five membered chelate ring either through N-bonding or through O-bonding from the amide linkage), but also because of the formation of complexes similar to metal-peptide [2,3]. We have initiated an investigation of zinc(II) complex with A-(2-pyridyl)carbonylaniline and have been successful in obtaining [Zn(Ci2Hi6N20)2(H20)2] · 2[C104]\", and now report the crystal structure of it. The structure of the title compound consists of a cation [Zn(Ci2Hi6N20)2(H20)2] and two Perchlorate anions, which are joined together by intermolecular hydrogen bonding. As the molecule of the complex occupies a special position in the crystallographic inversion center only half of the molecule is actually independent. The cation of the complex contains a distorted octahedrally coordinated zinc(II) ion, which is chelated by two bidentate JV-(2-pyridyl)carbonylaniline ligands through their Ο and Ν atoms and two water molecules. Two oxygen atoms from amide and two nitrogen atoms from pyridyl are in trans positions (the angles 0(amide)-Zn-0(amide) and N(pyridyl)-Zn-N(pyridyl) are 180°), and also the two coordinated water molecules are trans (the angle 0(water)-Zn-0(water) is 180°). The Zn—O(amide), Zn—0(water) and Zn—Ν distances show no remarkable features [2.078(2) Ä, 2.154(3) Ä and 2.086(3) A, respectively], and the greatest deviation from octahedral geometry was found for the 08-Znl -Nl and 08A-Znl-Nl angles [78.8(1)° and 101.2(1)°, respectively]. It is very interesting that hydrogen bonding plays an important role in the crystal packing. Both, the coordinated water molecule and the uncoordinated amide NH group of the N-(2-pyridyl)carbonylaniline ligands are involved in hydrogen bonding acting as hydrogen-bond donors with two and three Ο atoms of Perchlorate as potential hydrogen-bond acceptors. The Η ISA atom of the coordinated water molecule from intermolecular hydrogen bonds with 01, and the other oxygen atoms of Perchlorate ions form an intermolecular hydrogen bond with Η-atom of adjacent molecules so the two Perchlorate anions bridge two [Zn(Ci2HiöN20)2(H20)2]2 cations and assembles the molecules into a one-dimensional chain. Table 1. Data collection and handling. Crystal: colorless prism, size 0.3 χ 0.4 χ 0.5 mm Wavelength: Mo Ka radiation (0.71073 Ä) μ: 11.25 cm\" Diffractometer, scan mode: Bruker SMART CCD, φ /ω 29max: 57.96° Wl̂ measured, N(hkl)umqUe: 11968, 3437 Criterion for /0bs, N(hkl)g): Us > 2 a(Iobs), 3033 N(param)Kf\ tä'· 244 Programs: SHELXTL-plus [4], SHELXL-97 [5], SADABS [6] * Correspondence author (e-mail: a-ramazani@mail.znu.ac.ir) 606 Zn(C 1 2 H i6N20)2(H20)2(C104)2 Table 2. Atomic coordinates and displacement parameters (in Ä). Atom Site Table 2. Continued.

Crystal structure of bis[bis(diethylether)lithium (trimethylsilyl)methyl-cyanocuprate], [(C4H10O)2Li(C3H9)SiCH2CuCN]2

Abstract: C26H62Cu2Li2N204Si2, monoclinic, P12i/cl (No. 14), a = 10.0080(8) Ä, b = 11.1636(6) Ä, c = 18.029(2) Ä, β = 106.091(9)°, V= 1935.4 Ä, Ζ = 2, Rgl(F) = 0.031, wRref(F) = 0.074, T= 193 K.

Crystal structure of sodium scandium borate, NaScB2O5

Abstract: B2Na05Sc, mor.oclinic, P\\2\\k\\ (No. 14), a = 7.2339(6) Ä, b = 9.7966(6) Ä, c = 5.9233(5) Ä, β = 71.483(8)°, V = 398.0 Ä, Z= 4, R#(F) = 0.018, wRnf(F) = 0.055, 7 = 293 K. Source of material The title compound was prepared in the course of crystal chemical investigations of borates. It was grown at temperatures between 1520 Κ and 1470 Κ from a melt with molar composition of SC2O3 : Na2B4C>7 of 1 : 6 to colorless, prismatic crystals. Table 1. Data collection and handling.

Crystal structure of 1,4-diaminobutane tetrafluorooxotitanate, (C4N2H14)[TiF4O]

Abstract: Two types of novel framework materials, including six organically templated silicogermanates and five hybrid fluorotitanates, have been synthesized, and their structures have been determined by single crystal X-ray diffraction. Their structures and the interactions between the organic and inorganic species are discussed in some detail.The frameworks of the six silicogermanates, SU-9, SU-10, SU-11, SU-12, SU-14 and SU-21, are built up from either tetrahedra exclusively, or from mixed polyhedra. SU-9, SU-10 and SU-11 consist only of tetrahedra, and SU-12, SU-14 and SU-21 are built up from mixed polyhedra. In all silicogermanates, Si and Ge share the tetrahedrally coordinated positions, and only Ge occupies the 5- and 6-coordinated positions.The frameworks of SU-9, SU-10 and SU-11 belong to zeolite frameworks. SU-9 and SU-10 are built up from the same periodic building units (PBUs) that are formed by 4/4-4 units, and they adopt the known zeolite framework types AST and ASV, respectively. SU-11 is built up from 5-1 units and adopts the known zeolite framework type MFI. This is the first time that the frameworks of AST, ASV and MFI have been prepared in silicogermanate form.The 3-D frameworks of SU-12 and SU-14 contain (Ge,Si)7 composite building units that form one-dimensional 24-ring channels along the c axis. Their structures contain intersecting channels. SU-12 contains 8-, 10- 12- and 24-ring channels; while SU-14 has 9-, 10-, 12- and 24-ring channels. SU-21 is a two-dimensional framework structure containing 10-ring channels. It is the first silicogermanate with the template covalently bonded to Ge.All silicogermanates were synthesized by using organic amines as templates. The templates play a very important role in directing the structure of the inorganic framework.The obtained five hybrid fluorotitanates are SUF-1, SUF-2, SUF-3, SUF-4 and SUF-5. Their hybrid frameworks are built up from fluorotitanate anions, N-containing cations and crystal water/oxonium cations. Zero-dimensional fluorotitanate clusters are normally obtained when cyclic organic amines such as 1,4-diazabicyclo[2,2,2]octane (DABCO) and piperazine are used. Increasing the pH value of the starting solutions led to more condensed fluorotitanate anions, from isolated octahedra to pairs and eventually chains of octahedra. The formation of the hybrid frameworks of fluorotitanates is strongly dependent on hydrogen bonds between the fluorotitanate anions, N-containing organic cations and water molecules/oxonium ions.

Crystal structure of bis(4-nitrobenzoate)tetraaquamanganese(II)dihy-drate,[Mn(p-No2C6H4COO)2(H2O)4]·2H2O,andofbis(4-nitrobenzo-ate)tetraaquanickel(II)dihydrate,[Ni(p-NO2C6H4COO]·2H2O

Abstract: Ci4H2oMnN2Oi4, triclinic, P\\ (No. 2), a = 7.3302(6) A, b = 7.3884(6) A, c = 10.6470(9) Α, α = 92.707(1)°, β = 91.985(2)°,γ= 119.100(1)° V=502.2Ä 3 ,Z = 1, Rgl(F) = 0.028, wRKdF) = 0.066, T= 295 K. C14H20N2N1O14, triclinic, P\\ (No. 2), a = 7.2279(7) A, b = 7.3401(7) A, c = 10.600(1) Α, α = 91.114(2)°, β = 92.357(2)°, γ = 119.140(1)°, V= 490.3 Α 3 , Ζ = 1, Rgt(F) = 0.027, wRref(F) = 0.062, 7 = 2 9 5 Κ. Source of material Mixtures of Mn(N03)2 orNi(N03>2 (2 mmol) and NH4C7H4NO4 (4.2 mmol) in water were stirred while boiling. The solutions were allowed to cool slowly to room temperature which afforded X-ray quality crystals. The chosen crystals were coated with a hydrocarbon oil and mounted in a glass capillary. Discussion We wish to present in this contribution the crystal structures of [Mn(p-N02C6H4C00)2(H20)4] · 2H2O (1) and the isostructural [Ni(p-NO2C6H4CO0)2(H2O)4] • 2H20 (2) and briefly discuss the crystal organization in terms of hydrogen bonds and aromatic π-π interactions. Tetraaquabis(4-nitrobenzoato)manganese(II) in (1) has the Mn atom on a twofold axis and display a pseudo-octahedral coordination. The Mn—Ol and Mn—02 distances are 2.180(1) A and 2.195( 1) A, respectively. Thep-nitrobenzoate ligands are coordinating in a monodentate-frans mode with a Mn—04 distance of 2.184(1) A and an Mn-04-Cl angle of 127.09(9)°. The torsion angle Mn-04-C 1-C2 is 162.85(9)°. The C6H4N02 moiety is planar with an average deviation from the plane defined by the nine non-H atoms of 0.015(2) A whereas the dihedral angle between this plane and the plane defined by C2-C1-04 -05 is 8.04(21)°. The two aromatic planes are perfectly coplanar. The CI—C2 bond is significantly lengthened upon coordination with the Mn ion to 1.5158( 19) A as compared with 1.486(2) A for uncoordinated P-NO2C6H4COOH, and the CI—04 bond shortened to 1.272(2) A as compared with 1.302(2) A [1], Compound (2) is isostructural with the Mn analogue with Ni—Ol and Ni—02 distances of 2.058(2) A and 2.063(1) A whereas the Ni—04 distance has a value of 2.077( 1) A. In the related compound bis((p-ni t robenzoato)( l ,3-propane diamine))-nickel(II) a similar coordination mode of the p-nitrobenzoate ligands is observed with a Ni—Ο distance of 2.129(1)A [2], A third representative of compounds isostructural with (1) and (2) is [C0(p-N02C6H4C00)2(H20)4] · 2H20 with a comparable set of intraand intermolecular interactions [3], In contrast, the related [Zn(p-N02C6H4C00)2 · 2H20] has a distorted tetrahedral geometry where the angle O-Zn-O for the p-aminobenzoate ligands is 102.6(1)° [4], The crystal is assembled by alternating domains with hydrophobic and hydrophilic character, respectively. The hydrophobic domain is dominated by aromatic rings stacked into columns, with an interplanar distance of 3.421 (3) A, a distance that suggests that aromatic π -π interactions have an appreciable role for the non-bonded crystal organization [5-8]. The successive molecular planes are translated in a 1,2,3,1,2,3,... fashion, resembling a β stacking mode in the nomenclature introduced for polycyclic aro-. matic compounds [9]. The offset distances, in an orthogonal pro·! jection to the aromatic planes, between the aromatic ring centroids in adjacent planes are 1.368(3) A and 1.715(3) A , values that can be compared to an average value of 1.39 A, ranging from 0 A to 3.90 A, calculated for 32 nitrobenzene derivatives * Correspondence author (e-mail: olof.kristiansson@kemi.slu.se) [Mn0?-NO2C6H 4 COO)2(H2O)4] · 2 H 2 0 and [ N i ( p N 0 2 C 6 H 4 C 0 0 ) 2 ( H 2 0 ) 4 ] · 2 H 2 0 87 Crystall izing in h o m o g e n o u s s tacks [ 1 0 ] . T u r n i n g to the m i n i m a l inode l o f a romat ic interact ions , the b e n z e n e d imer , a paral le l disp l a c e d geometry with an o f f s e t d is tance o f 1.8 A is, b e s i d e s the T s h a p e d g e o m e t r y , the e n e r g e t i c a l l y preferred a r r a n g e m e n t as s h o w n by ab init io c a l c u l a t i o n s [ 1 1 ] . T h e h y d r o p h i l i c d o m a i n is charac ter ized by an e x t e n s i v e array o f h y d r o g e n b o n d s . W i t h i n the unit is 0 2 l inked by a s trong h y d r o g e n b o n d to 0 6 1 wi th an Ο — Η — Ο dis tance o f 2 . 6 2 1 ( 2 ) A . E a c h s o l v a t e w a t e r m o l e c u l e a c t s l i k e an e f f i c i e n t m o l e c u l a r \" g l u e \" b y l i n k i n g f o u r M n ( p N 0 2 C e H 4 C 0 0 ) 2 units by a c c e p t i n g t w o and donat ing three hydrogen bonds with Ο — Η — Ο b o n d lengths r a n g i n g f r o m 2 . 7 1 8 ( 2 ) A to 2 . 9 6 8 ( 2 ) A . F i n a l l y , O l is l inked to 0 7 ' ( s y m m e t r y Code: ( ; ) χ 1 , ν, ζ 1 ) with a re la t ive ly w e a k h y d r o g e n b o n d with an Ο — H 0 d is tance o f 2 . 9 8 1 ( 2 ) Ä . 1. Bis(4-nitrobenzoate)tetraaquamanganese(II) dihydrate, [Mn(p-N02C6H4C00)2(H20)4] (H 2 0) 2 Table 1. Data collection and handling. Crystal: colorless plate, size 0.10 χ 0.40 χ 0.50 mm Wavelength: Mo Ka radiation (0.71073 A) μ: 7.34 cm\"1 Diffractometer, scan mode: Bruker SMART CCD. ω 2Qmax'· 55.94° AYWr/Jmeasured, A/f/lW;unique: 3989,2211 Criterion for 70bs. N(hkl)iX: /obs > 2 af/obsJ. 1819 N(param)„ fined: 168 Program: SHELXTL-97 [12] Table 2. Atomic coordinates and displacement parameters (in A 2) . Atom Site f/ i s Table 2. Continued.

Crystal structure of hexacesium hexaselenidodigermanate(III), Cs6Ge2Se6

Abstract: Source of material The title compound was prepared starting from an inhomogeneous sample obtained by thermal decomposition of CsN3 mixed with GeSe2 (molar ratio 6:2). The reaction was carried out at 630 Κ in a quartz glass ampule. Together with additional Se (molar composition 6 Cs: 2 Ge: 6 Se), the raw product was heated to 1273 K. After quenching in icewater, homogenization and subsequent annealing at 953 Κ for two weeks the reaction yielded air sensitive, transparent, orange single crystals of Cs6Ge2Se6.

Crystal structure of N-methylpyrrolidone-2-one-N-methylpyrrolidine-2- onium perbromide, C10H19Br3N2O2

Abstract: CioHi9Br3N202, monoclinic, P\2\!n\ (No. 14), a = 7.680(2) Ä, b = 10.621(1) Ä, c = 9.975(2) Ä, β = 107.42(1)°, V= 776.3 Ä, Ζ = 2, pm = 1.860 g em, Rn(F) = 0.053, wR^F) = 0.176, Γ =293 Κ. Source of material The title compound was prepared as found in literature [ 1 ]. Anhydrous hydrogen bromide was passed into a Dresche) bottle containing 75 mL of methanol cooled at 273 Κ until 40.5 g (0.5 mole) was absorbed. To this was added 26 mL (0.5 mole) of bromine. This was then transferred to a 600 mL baker and cooled in an ice bath. Addition of 99 mL (1.0 mole) of 1 -methyl-pyrrolidin-2-one was begun. The resulting mixture rapidly deposited orange crystals. It was necessary to add 225 mL of methanol to complete the addition. The final product was recrystallised from methanol to yield 191.6 g of orange translucent crystals. Discussion Pyrrolidine-2-one gave a crystalline complex with bromine; the red brick solid was identified as a mixture of (C4H?NO)2 · Br2 and C4H7NO · HBr [2]. A similar complex was prepared from l-methyl-pyrrolidine-2-one (N-methylpyrrolidone) and bromine, constitution of which was not further investigated [3], More recently, by attemps to prepare the same entities, it was noted that a change of the structure of the lactam conferred a different requirement for stability upon these complexes: the molecular ratio for lactam-hydrogen bromide and bromine was 3-1-1 for pyrrolidine-2-one and 2-1-1 for the N-methyl derivative [1], They thought that stability might be due to the formation of [Bo] species, as it was observed since a long time in many other complexes of halogen and hydrohalides with organic compounds. The [Br3]~ species would interact with lactam derivatives to form stable unified complexes; no evidence for the exact structure was given. In the course of our research concerning various lactam complexes, we wanted to dispose of the title compound which could serve as a model. The crystal structure is built up from [N-methylpyrrolidoneN-methylpyrrolidonium] cations and [Br3]~ anions. Two N-methylpyrrolidone molecules are linked together by one strong hydrogen bond formed with the oxygen atoms 0 2 and 02 ' of the carbonyl groups; the hydrogen atom H2 occupies two statistic disordered positions relieved by the symmetry center (02—H2—02' or 02-H2 '—02 ' : 2.415(5) Ä, 153(29)°, i : 1-jc, -y, 1-z). The stereochemistry of this cation is in very good agreement with those determined in the (/V-methylpyrrolidone)2 · HI3 complex [4]. Since Brl is located at inversion center, the [Br2-Brl-Br2"r anion (ii: 1 x, l->>, 1-z) is linear with bond length Brl—Br2 : 2.531(1) Ä in good agreement with the values reported for [(CH3)3NH]2Br3~Br~. The crystal packing is characterized by the presence of layers parallel to (010) plane, consisting of [Br3]~ anions with a height of b/2. [CioHi9N202] cations are placed in sandwich in equal distance between these layers. Table 1. Data collection and handling. Crystal: orange, parallelepipedic, size 0.20 χ 0.25 χ 0.35 mm Wavelength: Cu Ka radiation (1.54180 A) μ: 96.00 cm" Diffractometer, scan mode: Enraf-Nonius CAD4, ω/2θ 26max: 129.92° WAWJmeasured, N(hkl)unique: 1309, 1309 Criterion for /0bs, N(hkl)p./obS > 2 σ(/οίκλ 1032 N(param)K rln«i: 80 Programs: SIR92 [5], SHELXL-97 [6], CAMERON [7], WinGX [8] * Correspondence author (e-mail: Alain.Danan@cep.u-psud.fr) 458 A/-Methylpyrrolidone-2-one-A'-methylpyrrolidine-2-onium perbromide Table 2. Atomic coordinates and displacement parameters (in A). Atom Site Occ. χ Table 2. Continued.