Showing papers in "Zeitschrift Fur Kristallographie-new Crystal Structures in 2005"

Crystal structure of taedol, C10H16O2, from Haplopappus taeda

Abstract: C10H16O2, monoclinic, P1211 (no. 4), I± = 8.974(2) …, b = 5.933(1) …, c = 8.994(2) …, I² = 96.29(3), V = 476.0 …3, Z = 2, Rgt(F) = 0.052, wRobs(F2) = 0.148, T = 293 K.

Crystal structure of (1,10-phenanthroline-N,N' )bis(2-fluorobenzoato)lead(II), Pb(FC6H4COO)2(C12H8N2)

Abstract: C26Hi6F2N204Pb, triclinic, PI (no. 2), a = 9.431(2) A, b = 10.950(2) A, c = 11.609(2) A, a = 80.90(3)°, β = 84.41(3)°, γ = 73.36(3)°, V= 1132.5 A \\ z = 2 , Rgt(F) = 0.035, wRnftF) = 0.098, Γ= 293 K. Source of material Freshly prepared PbCQj (0.13 g, 0.49 mmol), 1,1 O-phenanthroline (phen · H2O) (0.10 g, 0.51 mmol), 2-fluoro-benzoic acid (0.08 g, 0.52 mmol), 12 mL CH3OH/H2O (1:2 vA>) were mixed and stirred for ca. 3 h. Subsequently, the resulting suspension was heated in a 23 ml Teflon-lined stainless steel autoclave at 373 Κ for 7 day. After the autoclave was cooled to room temperature, the solid was filtered off. The resulting yellow filtrate was allowed to stand at room temperature and slow evaporation for a week afforded yellowish block crystals. Table 2. Atomic coordinates and displacement parameters (in Ä). Correspondence author (e-mail: zbs Jy@163.com) Atom Site X y ζ Uiso H(l) 2i 0.5337 0.3239 0.6786 0.065 H(2) 2 i 0.6473 0.1270 0.7914 0.065 H(3) 2/ 0.5785 -0.0501 0.7778 0.065 H(5) 2/ 0.4255 -0.1569 0.6821 0.065 H(6) 2i 0.2626 -0.1466 0.5510 0.065 H(8) 2 i 0.0947 -0.0159 0.3942 0.065 H(9) 2i 0.0003 0.1808 0.2816 0.065 H(10) 2i 0.0608 0.3599 0.3191 0.065 H(16) 2i 0.5109 0.2976 -0.0552 0.065 H(17) 2/ 0.7537 0.3011 -0.0966 0.065 H(18) 2i 0.8839 0.3491 0.0386 0.065 H(19) 2i 0.7778 0.4146 0.2327 0.065 H(22) 2i -0.0977 0.5927 0.1806 0.065 H(23) 2i -0.2340 0.6982 0.0234 0.065 H(24) 2 i -0.2644 0.9024 -0.0396 0.065 H(25) 2i -0.1632 1.0303 0.0615 0.065 76 Pb(FC6H4COO)2(Ci2HgN2) Table 3. Atomic coordinates and displacement parameters (in A). Atom Site X y J υ 11 t/22 t/33 U12 U13 Un Pb(l) 2i 0.24095(2) 0.48169(2) 0.49051(1) 0.0482(1) 0.0434(1) 0.0456(1) -0.01010(7) -0.00476(8) -0.00632(7) N(l) 2 ; 0.3982(5) 0.2592(4) 0.6013(4) 0.059(3) 0.045(2) 0.054(2) -0.009(2) -0.006(2) -0.010(2) N(2) 2i 0.1927(5) 0.2759(4) 0.4443(4) 0.053(2) 0.051(2) 0.062(3) -0.013(2) 0.000(2) -0.018(2) CKl) 2 i 0.3519(6) 0.4565(6) 0.3061(4) 0.078(3) 0.140(5) 0.069(3) -0.026(3) 0.011(2) -0.027(3) 0(2) 2 i 0.5547(7) 0.4243(6) 0.3853(4) 0.150(5) 0.106(4) 0.055(3) -0.055(4) -0.003(3) -0.028(3) CK3) 2 i 0.1349(6) 0.7263(5) 0.3545(5) 0.085(3) 0.079(3) 0.098(4) -0.039(3) -0.046(3) 0.019(3) CK4) 2 i 0.0178(4) 0.5750(4) 0.3708(3) 0.062(2) 0.057(2) 0.057(2) -0.015(2) -0.003(2) -0.001(2) F(l) 2/ 0.373(1) 0.329(1) 0.1325(8) 0.184(8) 0.26(1) 0.187(8) -0.091(7) -0.013(6) -0.096(7) F(2) 2 i -0.003(1) 0.9441(7) 0.2208(7) 0.24(1) 0.101(5) 0.167(7) -0.045(5) -0.083(7) 0.006(4) C(l) 2i 0.5045(8) 0.2509(6) 0.6730(6) 0.086(4) 0.050(3) 0.069(4) -0.009(3) -0.017(3) -0.011(3) C(2) 2i 0.5741(9) 0.1313(7) 0.7414(6) 0.093(5) 0.066(4) 0.066(4) 0.001(3) -0.031(4) -0.012(3) C(3) 2 i 0.5337(9) 0.0273(7) 0.7330(7) 0.088(5) 0.052(3) 0.066(4) -0.001(3) -0.010(3) 0.001(3) C(4) 2 i 0.4246(7) 0.0314(5) 0.6579(5) 0.073(4) 0.043(3) 0.061(3) -0.011(2) 0.010(3) -0.004(2) C(5) 2i 0.3832(9) -0.0780(6) 0.6386(7) 0.094(5) 0.042(3) 0.091(5) -0.020(3) 0.005(4) 0.001(3) C(6) 2i 0.2863(9) -0.0723(6) 0.5609(8) 0.087(5) 0.048(3) 0.102(6) -0.030(3) 0.015(4) -0.017(3) C(7) 2i 0.2181(7) 0.0472(6) 0.4921(6) 0.061(3) 0.053(3) 0.084(4) -0.023(2) 0.011(3) -0.021(3) C(8) 2i 0.1209(8) 0.0564(8) 0.4067(8) 0.071(4) 0.082(5) 0.116(6) -0.035(4) -0.002(4) -0.047(4) C(9) 2i 0.0635(8) 0.1736(7) 0.3405(7) 0.073(4) 0.078(4) 0.097(5) -0.021(3) -0.020(4) -0.033(4) C(10) 2i 0.1015(7) 0.2810(6) 0.3631(6) 0.068(4) 0.061(3) 0.082(4) -0.009(3) -0.022(3) -0.018(3) C(ll) 2i 0.2524(6) 0.1607(5) 0.5082(5) 0.050(3) 0.047(3) 0.061(3) -0.013(2) 0.009(2) -0.016(2) C(12) 2 i 0.3597(6) 0.1518(5) 0.5919(4) 0.055(3) 0.043(2) 0.050(3) -0.010(2) 0.009(2) -0.010(2) C(13) 2 i 0.4846(7) 0.4238(5) 0.3006(5) 0.080(4) 0.038(2) 0.054(3) -0.018(2) 0.011(3) -0.008(2) C(14) 2 i 0.5659(6) 0.3869(4) 0.1883(4) 0.061(3) 0.041(2) 0.044(2) -0.011(2) -0.002(2) -0.000(2) C(15) 2 i 0.4986(8) 0.3498(7) 0.1049(6) 0.069(4) 0.083(4) 0.063(4) -0.030(3) 0.007(3) -0.021(3) C(16) 2 i 0.563(1) 0.3190(8) -0.0012(6) 0.109(6) 0.110(6) 0.054(4) -0.027(5) -0.002(4) -0.032(4) C(17) 21 0.707(1) 0.321(1) -0.0250(7) 0.096(6) 0.105(6) 0.059(4) -0.005(5) 0.019(4) -0.011(4) C(18) 2/ 0.7850(9) 0.353(1) 0.0590(9) 0.068(5) 0.114(7) 0.112(7) -0.015(4) 0.034(5) -0.010(5) C(19) 2/ 0.727(1) 0.3923(8) 0.178(1) 0.127(7) 0.084(5) 0.161(9) 0.010(5) 0.105(7) 0.033(6) C(20) 2/ 0.0421(6) 0.6803(6) 0.3233(5) 0.055(3) 0.058(3) 0.050(3) -0.011(2) -0.007(2) 0.004(2) C(21) 2i -0.0467(6) 0.7503(6) 0.2197(5) 0.042(2) 0.073(3) 0.045(3) -0.015(2) 0.000(2) 0.001(2) C(22) 2i -0.1100(9) 0.680(1) 0.1580(7) 0.085(5) 0.18(1) 0.072(5) -0.070(6) -0.018(4) -0.002(5) C(23) 2 i -0.191(1) 0.745(2) 0.063(1) 0.128(9) 0.25(2) 0.099(8) -0.09(1) -0.059(7) 0.011(9) C(24) 2 i -0.210(1) 0.865(2) 0.026(1) 0.109(8) 0.27(2) 0.097(8) -0.05(1) -0.052(6) 0.07(1) C(25) 2 i -0.149(1) 0.943(1) 0.084(1) 0.101(7) 0.15(1) 0.113(8) 0.002(7) -0.017(6) 0.074(8) C(26) 2 i -0.0666(9) 0.8754(8) 0.1772(7) 0.080(4) 0.084(5) 0.080(5) -0.022(4) -0.022(4) 0.012(4) Acknowledgments. The authors gratefully acknowledge the financial support by Jinhua Municipal Science and Technology Commission (grant no. 03-1179). BSZ also gratefully acknowledges the guidance of Professor Y.-Q. Cheng, Institute of Solid State Chemistry, Ningbo University.

Crystal structure of 1,3,5-tris(4-methoxyphenyl)-1H-1,2,4-triazole-2- oxide, C23H21N3O4

Abstract: C23H21N3O4, monoclinic, P\\2\\!c\\ (no. 14), a = 10.7855(7) A, b = 8.3439(6) Ä, c = 22.960(2) Ä, β = 101.620(6)°, V= 2023.9 Ä, Z= 4, R#(F) = 0.056, wR^F) = 0.185, T= 293 K. Source of material The title compound [1-4] was obtained as a by-product of an attempted 1,3-dipolar cycloaddition, when the nitrile oxide precursor, 4-methoxybenz-hydroximoyl chloride [5], and a rather unreactive dipolarophile [5-8] (a bi-cycüc isoxazolo-cyclopentenone) were heated under reflux in toluene for 16 h. Purification by column chromatography and crystallization from ethyl acetate and petroleum ether furnished the tide compound in the form of colorless crystals (m.p. 483-484 K) [9]. Discussion The anisyl moieties are showing a step-by-step deviation from the coplanar orientation in relation to the triazole core (figure, top) The anisyl group attached at the 1-position shows the strongest out-of-plane orientation, indicated by the torsion angle C3-N2-C6-C7 of -56.5°. This behavior is forced by the steric influence of the neighboring oxygen atom at the 2-position and another anisyl moiety at the 5-position. The anisyl group at the 3-position is only slightly influenced by the oxide at C2. Consequently, we found a nearly coplanar orientation indicated by the torsion angle N4-C5-C20-C21 of -6.4°. The torsion angle N4-C3-C13-C18 of-20.6° of the anisyl moiety at C5 characterizes a medium out-of-plane orientation. In the packing we observe hydrophobic layers in the a,b plane stacking along the c axis. The cell plot also shows hydrophobic channels along the b axis built up by a \"face-to-face\" and a \"side-by-side\" orientation of the anisyl groups (figure, bottom). Table 1. Data collection and handling.

Crystal structure of (diethyldithiocarbamato)(triethylphosphine)gold(I), Au[P(C2H5)3][S2CN(C2H5)2]

Abstract: C11H25A11NPS2, monoclinic, P12i/cl (no. 14), a = 11.1101(5) A, b= 13.5725(6) A, c = 21.945(1) Ä, β = 90.057(1)°, V = 3309.2 A, Ζ = 8, Rg(F) = 0.040, wRreffF) = 0.080, T= 223 K. Source of material The title compound was prepared as in the literature in the context of investigating the anti-tumor potential of this class of compound [1]. Crystals were obtained by layering ethanol over a dichloromethane solution of the compound. Experimental details Disorder was found in one of the two molecules comprising the asymmetric unit. Specifically, two sites were resolved for each methylene group bound to P2, as shown in the lower view of the figure, bottom, (H atoms for the phosphine ligand are omitted for clarity). Refinement showed the components of the disorder to be 0.67:0.33 (primed atoms); these atoms were refined isotropically. Discussion Two virtually identical molecules of Et3PAu(S2CNEt2) comprise the asymmetric unit. A linear environment is found for each of the Au atoms defined by S,

Crystal structure of (2,6-diisopropyl-phenyl)-(6-(2,6-dimethyl- phenyl)-pyridin-2-yl-methylene)-amine, C26H30N2

Abstract: C26H30N2, monoclinic, C12/cl (no. 15), a = 20.434(2) A, b = 8.551(1) A, c = 26.498(2) A,/? = 102.889(1)°, V= 4513.4 A, Z= 8, RpfF) = 0.062, wRnf(F) = 0.187, Τ =293 Κ. Source of material First, 2.0 g (10.7 mmol) of 6-bromopyridine-2-carbaldehyde and 2.03 mL (1.91 g, 10.7 mmol) of 2,6-diisopropylaniline were dissolved in 30 mL of ethanol and the mixture was heated at reflux for 2 h. The solvent was removed under reduced pressure and 3.59 g (97 %) of pale yellow crystalline material (I) was obtained and used without further purification. A solution of 1.39 mL (1.93 g, 10.4 mmol) of 2-bromo-m-xylene in 30 mL THF was added to 0.30 g (12.5 mmol) magnesium turnings and the resulting suspension stirred and activated using 0.2 mL of 1,2-bromoethane. An exothermic reaction took place and an ice bath was used to cool the reaction mixture when the reaction became too vigorous. The reaction mixture was stirred at room temperature for 2 h, then filtered and the filtrate (Π) directly used. To a solution of 3.0 g (8.69 mmol) I in 30 mL of dioxane was added a suspension of 0.11 g (0.87 mmol) FeCh in 10 mL of THF. The Grignard solution Π was then slowly added to the stirred suspension. The reaction mixture was heated to 70 °C for 48 h. 100 mL of water and 80 mL of diethyl ether were added and the resulting suspension transferred to a 500 mL separating funnel. The organic phase was collected and the inorganic phase washed with diethyl ether two times and extracted. The combined organic phases were washed with a saturated sodium chloride solution and dried with Na2S04. The organic phase was concentrated to dryness under vacuum resulting in a brown oily product. The oil was purified using silica chromatography (pentane) and then crystallized from pentane at -25 °C to afford pale yellow crystals suitable for X-ray crystal structure analysis (yield 1.16 g (39 %), m.p. 142.5 °C). Discussion As neutral metal complexes are required for selective oligomerization of ethylene or bis-alkoxycarbonylation of styrene, Bianchini and co-workers developed a series of substituted iminopyridine ligands [1-3]. The title compound, our search by SciFinder proceeded without any results, is a new sterically demanding member of this type of ligands. The bulky phenyl substituents in the 6-position of the pyridine and at the imino Ν atom are twisted with regard to the pyridine ring, and the dihedral angles are 118.6° and 98.1 respectively. Both phenyl rings form a dihedral angle of 68.8°. The significant shortening of the C6—N2 bond (1.25 A) indicates the imino function. In the uncoordinated ligand, the free electron pairs at the Npyndine and Njmino atoms are transoid. The C6-N2-C7 angle with 119.8° is much smaller than the C5-C6-N2 angle with 123.0°. Table 1. Data collection and handling. Crystal: Wavelength: μ· Diffractometer, scan mode: 20nux: WAUVasoitd. Nfhklhwpc: Criterion for /ote, Nfhkl)^: AYparamAefined·' Programs: pale yellow prism, size 0.4 χ 0.5 χ 0.6 mm Mo K„ radiation (0.71069 A) 0.63 cm Stoe IPDS Π, ω/φ 52.12° 31342,4468 /obs>2CTf/obs;, 3001 253 SIR97 [4], SHELXL-97 [5] Table 2. Atomic coordinates and displacement parameters (in A). * Correspondence author (e-mail: kempe@uni-bayreuth.de) Atom Site X y ζ Uiso H(2) 8/ -0.0275 -0.3555 0.3104 0.088 H(3) 8/ -0.0779 -0.2539 0.3733 0.098 H(4) 8/ -0.0126 -0.1203 0.4430 0.085 H(6) 8/ 0.1650 -0.0608 0.4627 0.074 H(9) 8/ 0.2317 0.0372 0.6549 0.092 H(10) 8/ 0.2624 0.2883 0.6421 0.102 H(ll) 8/ 0.2184 0.4149 0.5656 0.096 H(13) 8/ 0.1314 0.2503 0.4509 0.093 H(14A) 8/ 0.0399 0.4166 0.4461 0.203 H(14B) 8/ 0.0564 0.4292 0.5066 0.203 H(14C) 8/ 0.0339 0.2686 0.4797 0.203 H(15A) 8/ 0.2161 0.4401 0.4711 0.154 H(15B) 8/ 0.1690 0.5446 0.4963 0.154 H(15C) 8/ 0.1505 0.5113 0.4366 0.154 H(16) 8/ 0.1242 -0.2013 0.5611 0.102 H(17A) 8/ 0.0986 -0.2793 0.6390 0.286

Crystal structure of tetrakis[([2.2.2]crypt)potassium]tricarbonylmolybdenum(0) nonastannide ethylenediamine disolvate, [K(C18H36O6N2)]4[Mo(CO)3Sn9] . 2C2H8N2

Abstract: C79Hi6oK4MoNi2027Sn9, triclinic, P I (no. 2), a = 15.4208(1)Ä, b = 16.2851(1) Ä, c = 25.9400(2) Ä, a = 80.2284(3)°, β = 79.1115(3)°, γ = 63.2406(2)°, V= 5685.1 Ä 3 , Z = 2, Rgt(F) = 0.027, wRrtffF) = 0.067, T= 120 K. * Correspondence author (e-mail: thomas.faessler@liz.tum.de) Source of material All experiments were carried out under argon atmosphere using a glove-box or Schlenk technique. Toluene (Merck) and ethylenediamine (en; Merck) were dried over K/CaH2 (Fluka), freshly distilled and degassed. The binary alloy of the formal composition K4Sn9 was prepared by high-temperature reaction (350 °C) from the elements Κ and Sn in the ratio of 4:9. Tricarbonylmesitylenemolybdenum(O) was prepared by heating Mo(CO)6 (Alfa Inorganics) in an excess of mesitylene under reflux in a nitrogen atmosphere. K4Sn9 (100 mg, 0.082 mmol) and [2.2.2]ciypt (123 mg, 0.33 mmol) were dissolved in en(ca. 1 ml) in an Schlenk tube and stirred for 5 min to yield a dark red solution. Then the solution of MesMo(CO)3 (25 mg, 0.082 mmol) in toluene (ca. 1 ml) was added dropwise at room temperature. The resulting mixture was stirred for another 2 hours at room temperature to yield a reddish-brown solution. After filtration the filtrate was layered with toluene (2 ml). After 48 hours, dark brown crystals of [K([2.2.2]crypt)MSn9Mo(CO)3] precipitated with the yield of 45 mg (ca. 39% with respect to K4Sn9). Discussion One research interest concerning group 14 E/-Sn9Mo(CO)3] · 2en with an explicit new unit cell (see figure). Though the crystal structure of [^-SngMoiCOh]" ion as [K([2.2.2]ciypt)]4 salt has been reported earlier [2] (a = 16.187(3) k,b=25.832(4) A, c=29.855(5) Ä, a = 111.46(1)°,/J = 102.84(2)°,y=92.87(2)°), the quality of the reported crystal was not very satisfactory (Rg(F)=0.098, wRg<(F) = 0.276). In the title compound four [K[2.2.2]crypt] cations are present per nonastannide cluster in addition of two en solvent molecules (figure, top). This clearly indicates a charge allocation of 4 for 54 [K(Ci8H3606N2)]4[Mo(CO)3Sn9] · 2C2H8N2 the cluster polyanion. Though there are four [K([2.2.2]crypt)] Table 2. Continued. units surround the Sng cluster, all of them are quite far away from the polyanion and do not show any coordination to the cluster ion. Atom Site χ > As shown in the bottom figure (thermal ellipsoids shown at 95 % probability), the Mo(CO)3 fragment occupies the capping posiH(22B) H(23A) 2i 2 i 0.1066 0.0855 1.0093 1.1496 0.5963 0.6238 0.047 0.043 tion and the [Sn9] Zintl ion, which binds to the Mo atom in an η H(23B) 2 i 0.1877 1.1382 0.5896 0.043 coordinative fashion. The [Sn9] cluster is still quite regular in H(24A) 2 i 0.1144 1.2757 0.5358 0.038 shape. Similar to the reported complexes [η -Sn9Cr(CO)3] [5] H(24B) 2i 0.0150 1.2914 0.5744 0.038 and [>7-Sn9W(CO)3] [4], the Sn—Sn bond length within the bottom square plane (Sn2, Sn3, Sn4, SnS) is approximately 0.1 A H(25A) H(25B) H(26A) 2i

Crystal structure of 2-(2,6-di(methylethyl)phenylamino)pyridine, C17H22N2

Abstract: C17H22N2, monoclinic, CY2Jc\ (no. 15), a = 10.705(2) Ä, b = 14.654(3) Ä , c = 19.558(4) Ä, β = 94.74(3)°, V= 3057.6 A 3 , Ζ = 8, Rgt(F) = 0.079, wRjeffF) = 0.196, T= 173 K. Source of material The title compound was obtained in a one-step procedure [1,2]. 2Chloropyridine and 2,6-di(methylethyl)aniline hydrochloride were heated at 180 °C for 9 0 minutes. The hydrochlorous raw product was suspended to aqueous sodium carbonate and then extracted with dichloromethane. The dichloromethane solution was dried over anhydrous sodium sulfate, then filtered and the solvent was removed. Recrystallization from diethylether/heptane yielded large colorless mosaic crystals. Discussion The crystal structure reported here is similar to 2-(2,6-dimethylphenylamino)pyridine [3]. 2-(2,6-Di(methylethyl)phenylamino)pyridine crystallizes with two similar Ν 7 Η 7 Ν Γ interactions Table 3. Atomic coordinates and displacement parameters (in Ä). that form dimeric structure. The Ν 7 Η 7 Ν Γ angle is 167 (2)°, where the N 1 H 7 ' distance is 2 .13(3) Ä and this results in a donor-acceptor distance o f 2 .998(3) Ä. Table 1. Data collection and handling. Crystal: Wavelength: MDifiractometer, scan mode: 20ΤΏΛΧNthkllmsani. N(hklhm Criterion for /<*», N(hkl)gi: N(paramhrBoeA· Programs: colorless plate, size 0.20 χ 0.25 χ 0.35 mm Mo Ka radiation (0.71073 A) 0.65 cm 1 Nonius 95 mm KappaCCD, ω 53° 26983, 3161 > 2 a(Iobs), 2470 175 SHELXS-97 [4], S H E L X L ^ [5], SHELXTL[6] Table 2. Atomic coordinates and displacement parameters (in A). Atom Site X y ζ t/i«. H(3A) 8 / 0.3908 0.1666 0.2536 0.044 H(4A) 8/ 0.4432 0.1692 0.1416 0.052 H(5A) 8/ 0.2848 0.1705 0.0518 0.049 H(6A) 8/ 0.0803 0.1660 0.0789 0.045 H(7) 8/ 0.082(3) 0.175(2) 0.298(1) 0.036 H(10) 8/ 0.4078 0.3364 0.4419 0.044 H( l l ) 8/ 0.4563 0.2144 0.5138 0.046 H(12) 8/ 0.3739 0.0717 0.4880 0.043 H(14) 8/ 0.2512 0.3251 0.2763 0.047 H(15A) 8/ 0.0764 0.3463 0.3388 0.122 H(15B) 8/ 0.1169 0.4394 0.3079 0.122 H(15C) 8/ 0.1505 0.4181 0.3857 0.122 H(16A) 8/ 0.4430 0.3917 0.3108 0.118 H(16B) 8/ 0.3807 0.4468 0.3677 0.118 H(16C) 8 / 0.3426 0.4667 0.2900 0.118 H(17) 8 / 0.1605 0.0164 0.3434 0.045 H(18A) 8/ 0.0827 0.0199 0.4517 0.089 H(18B) 8/ 0.2037 -0.0296 0.4836 0.089 H(18C) 8/ 0.1103 -0.0810 0.4309 0.089 H(19A) 8/ 0.3654 -0.0337 0.3312 0.110 H(19B) 8/ 0.2836 -0.1140 0.3562 0.110 H(19C) 8/ 0.3791 -0.0637 0.4084 0.110 Atom Site X y ζ Un U22 I/33 Un Un U23 N(l) 8/ 0.1090(2) 0.1666(1) 0.17886(9) 0.0247(9) 0.031(1) 0.036(1) 0.0000(8) -0.0021(7) 0.0004(7) C(2) 8/ 0.2002(2) 0.1674(1) 0.2305(1) 0.023(1) 0.025(1) 0.033(1) -0.0004(8) 0.0003(8) -0.0002(8) C(3) 8/ 0.3285(2) 0.1674(2) 0.2175(1) 0.021(1) 0.051(2) 0.038(1) -0.004(1) 0.0012(8) -0.005(1) * Correspondence author (e-mail: mika.polamo@helsinki.fi)

Crystal structure of aqua(2,2'-bipyridine-N,N')bis(2-fluoro-benzoato)cadmium(II),Cd(H2O)(C10H8N2)(C7H4FO2)2

Abstract: C24Hi8CdF2N205, orthorhombic, Ρ2χ2χ2ι (no. 19), a = 9.8316(2) A, b = 10.0682(2) A, c = 22.5002(5) A, V = 2227.2 A, Ζ = 4, R^F) = 0.027, wR^F) = 0.069, 7 = 2 9 3 K. Source of material Freshly prepared CdCCk (0.26 g, 1.51 mmol), 2,2'-bipyridine (CioHgN2) (0.04 g, 0.26 mmol), 2-fluorobenzoic acid (0.05 g, 0.36 mmol), 12 mL CH3OH/H2O (1:2 v/v) were mixed and stirred for ca. 4.5 h. Subsequently, the resulting suspension was heated in a 23 ml Teflon-lined stainless steel autoclave at 393 Κ for 8 day. After the autoclave was cooled to room temperature, the solid was filtered off. The resulting yellowish filtrate was allowed to stand at room temperature and slow evaporation for two months afforded yellow flake-like crystals. Discussion In the complex molecule of the title compound (figure, top), the Cd atom is coordinated by two Ν atoms from one bidentate chelating 2,2-bipyridine ligand and five Ο atoms from two 2-fluorobenzoic acid anions and one aqua ligand to complete a distorted CdN2Os pentagonal bipyramid with d(Cd—N) = 2.355(2) A, 2.366(2) A, d(Cd—O) = 2.321(2) A 2.441(3) A. The coordinated water molecule (figure, bottom) shows hydrogen-bonding to the carboxylate Ο atoms of the 2-fluorobenzoate anions with d(05-H5A—Ol') = 2.704 A and (1(05-Ά5Β· 03) = 2.815 A, Z.O-H •O= 139.7°-158.8° (i: -x+1 ,y-Vi,-z+Vi). The complex molecules are connected via these Η bonds to chains parallel [010] figure, bottom). Moreover, the F and Ο atoms show weak hydrogen interactions with bs, N(hkl)gt: N(param)nSmA'· Programs: yellow flake, size 0.09 χ 0.31 χ 0.38 mm Mo Ka radiation (0.71073 A) 10.37 cm\" Bruker SMART APEX CCD Π, φ/ω 61.3° 13071,6540 /obs > 2 a(Iobs), 4895 316 SHELXS-97 [3], SHELXL-97 [4] Table 2. Atomic coordinates and displacement parameters (in Ä). Correspondence author (e-mail: zbs_jy@163.com) Atom Site X y ζ Uiso H(5A) 4a 0.5761 0.3771 0.2235 0.083 H(5B) 4a 0.5422 0.4115 0.2750 0.083 H(l) 4a 0.1368 0.7926 0.2065 0.083 H(2) 4a -0.0808 0.8433 0.1821 0.083 H(3) 4a -0.2296 0.6729 0.1570 0.083 H(4) 4a -0.1506 0.4556 0.1553 0.083 H(7) 4a -0.0586 0.2659 0.1438 0.083 H(8) 4a 0.0401 0.0606 0.1430 0.083 H(9) 4a 0.2607 0.0347 0.1775 0.083 H(10) 4a 0.3771 0.2224 0.2091 0.083 142 Cd(H20)(CioH8N2)(C7H4F02)2 Table 2. Continued. Table 2. Continued. Atom Site X y ζ t/Uo Atom Site X y : l/iso H(13) 4a 0.3815 0.8214 0.4074 0.068 H(20) 4a 0.6184 0.5876 0.0430 0.083 H(14) 4a 0.3403 0.8731 0.5047 0.083 H(21) 4a 0.6917 0.6840 -0.0435 0.083 H(15) 4a 0.2002 0.7400 0.5622 0.083 H(22) 4a 0.6304 0.8935 -0.0679 0.083 H(16) 4a 0.1141 0.5468 0.5224 0.083 H(23) 4a 0.4981 1.0171 -0.0034 0.083 Table 3. Atomic coordinates and displacement parameters (in A). Atom Site X y Ζ Ui ι U22 f/33 t/12 U13 1/23 Cd(l) 4a 0.34992(2) 0.54478(2) 0.22465(1) 0.04174(8) 0.03908(8) 0.0385(1) -0.00511(6) -0.00062(8) -0.00078(9) N(l) 4a 0.1265(2) 0.5992(2) 0.1942(1) 0.052(1) 0.046(1) 0.039(2) 0.0076(8) 0.000(1) 0.003(1) N(2) 4a 0.2328(2) 0.3520(2) 0.1949(1) 0.0404(9) 0.041(1) 0.040(2) -0.0014(8) -0.0019(8) 0.000(1) 0(1) 4a 0.4231(4) 0.7355(3) 0.1716(2) 0.135(2) 0.108(2) 0.050(2) -0.071(2) 0.033(2) -0.027(2) 0(2) 4a 0.4585(3) 0.5473(3) 0.1276(1) 0.100(2) 0.076(2) 0.069(3) -0.013(2) 0.009(2) 0.023(2)

Crystal structure of dibarium mononitride, Ba2N, an alkaline earth metal subnitride

Abstract: Abstract Ba2N, trigonal, R3m (no. 166), a = 4.0290(6) Å, c = 22.425(4) Å, V = 315.3 Å3, Z = 3, Rgt(F) = 0.026, wRref(F2) = 0.063, T = 293 K.

Crystal structure of trimagnesium monopalladium, Mg3Pd

Abstract: MgjPd, hexagonal, P03cm (no. 185), a = 7.987(1) A, c = 8.422(1) A, V= 465.3 Ä, Z= 6, Rgi(F) = 0.023, wRteffF) = 0.045, T = 293 K. Source of material Samples of the nominal composition Mg»Pdi_* with χ = 0.74, 0.75,0.76 and 0.78 were prepared by induction melting mixtures of the elements (Pd, 99.99 %; Mg, 99.99 %) in argon filled and weld-sealed tantalum ampoules. Subsequently, the ampoules were encapsulated in fused silica tubes and annealed at 773(5) Κ for three weeks. Finally, the ampoules were quenched in water. A single crystal of Mg3Pd with metallic lustre was obtained from the sample at the nominal composition Mgo.78Pdo.22Chemical analyses on impurities of Ο, N, C, Η and Ta were performed using the carrier gas hot extraction, the combustion technique and ICP-MS spectroscopy, respectively. All impurities were below their respective limit of detection: Ο < 750 ppm, Ν < 150 ppm, C < 1000 ppm, Η < 32 ppm, Ta < 600 ppm. The microstructures of the samples were analyzed via microscopic examination in combination with EDXS to determine the number of phases and their composition. At 78.0 at-% and 76.0 at-% Mg the samples revealed two phases, Mg3Pd and the complex metallic alloy phase (CMA) Mg78.sPd2i.5 [ 1 ]. The sample at 75.0 at-% Mg is nearly single phase (CMA < 1%), whereas the sample at 74.0 at-% Mg consists of MgjPd and MgsPd2. Experimental details The unit cell parameters of Mg3Pd either in equilibrium with the CMA or the MgsPd2 phase were obtained from least-squares fittings of reflections taken from Guinier powder patterns (Huber, Ge monochromator, CuKai radiation, λ = 1.5405929 A, Si powder SRM 640c as internal standard, a = 5.431195(9) Ä). They are equal within the e.s.ds. The title compound exhibits no perceptible homogeneity range and undergoes a peritectic reaction at 898(3) Κ into MgsPd2 and the liquid phase according to DTA measurements. Mg8

Crystal structure of pentacarbonyl[(ethoxycarbonyl)- (N-diphenylmethylenamino)methylene]chromium(0), Cr(CO)5[C(COOC2H5){NC(C6H5)2}]

Abstract: C22Hi5CrNC>7, monocLinie, P\\2\\ln\\ (no. 14), a = 9.7086(9) A, b = 21.743(2) A, c = 10.801(1) A, β = 109.594(1)°, V= 2148.1 A, Z = 4, R^F) = 0.038, wRrttfF) = 0.098, T= 183 K. Source of material The title complex was prepared by metathesis of the diphenylmethylene Schiff base of dehydroalanine ethyl ester with the Fischer carbene complex (OC)sCr=C(Ph)(OMe) [1], Orange-red plate-like crystals were obtained from a solution in n-hexane at 4 °C. Experimental details The unusual CI—C2 single-bond distance of 1.35 A and slightly enlarged displacement parameters of the carbon atoms involved are caused by the disorder of the ethoxy group. Discussion In the molecule (0C)sCr=C(C02Et)(N=CPh2) the bond lengths within the Cr-C(C02Et)-N=C group are of interest. The distance Nl—C4 of 1.260(3) A is even shorter than the C=N bond of the imino group (d(Nl =C5) = 1.276(3) A). The angle C5-N1-C4 is 167.2(2)°. In the tungsten complex (0C)5W=C(C02EtKN=CPh2) the corresponding data were found to be 1.253(7) A, 1.283(7) A and 167.3(6)° [1]. These findings point to a dominant nitrile ylide character Cr~-C(R)=N=C (heteroallene structure) in the carbene complex. The negative partial charge at the metal atom results in an elongated metal caibene bond (d(Cr—C4) = 2.084(2) A, d(W—C) = 2.208(6) A) and this leads to a stronger back donation in the frans-metal-CO bond as was found for the tungsten complex (d(W—C) = 2.017(7) A [1]). A high contribution of a zwitter ionic form was also observed in Fischer amino carbene complexes [2]. Table 1. Data collection and handling. Crystal: orange-red prism, size 0.3 χ 0.3 χ 0.4 mm Wavelength: Mo Ka radiation (0.71073 A) M5.75 cm\" Diffiractometer, scan mode: Siemens SMART CCD, ω/φ 20nuu' 56.1° N(hkl)mcasmA, AffAJUJumque: 10933,3754 Criterion for /obs, N(hkl)gc. /obs > 4 CT(/obsj, 2481 N(param)nBsisi'· 281 Programs: SHELXS-97 [3], SHELXL-97 [4] Table 2. Atomic coordinates and displacement parameters (in A). Atom Site X y ζ Ujso H(1A) 4e 0.4135 0.2593 0.3485 0.155 H(1B) 4e 0.2730 0.2199 0.3309 0.155 H(1C) 4e 0.2654 0.2769 0.2399 0.155 H(2A) 4e 0.3880 0.2326 0.1385 0.116 H(2B) 4e 0.2729 0.1841 0.1487 0.116 H(7A) 4e 0.5850 -0.1200 0.1500 0.041 H(8A) 4e 0.4943 -0.1915 0.2617 0.052 H(9A) 4e 0.4883 -0.1692 0.4685 0.058 H(10A) 4e 0.5755 -0.0764 0.5660 0.057 H(11A) 4e 0.6618 -0.0038 0.4547 0.047 H(13A) 4e 0.6392 0.0513 -0.0091 0.052 H(14A) 4e 0.7303 0.0303 -0.1769 0.072 H(15A) 4e 0.8831 -0.0531 -0.1595 0.081 H(16A) 4e 0.9435 -0.1160 0.0229 0.067 H(17A) 4e 0.8468 -0.0970 0.1871 0.050 * Correspondence author (e-mail: wbe@cup.uni-muenchen.de) 500 Cr

Crystal structure of 3,3,4,4,5,5-hexafluoro-{1-[2-methyl-5-(4-formylphenyl)-thien-3-yl]-2-[2-methyl-5 -(4-(1,3-dioxolan- 2-yl)phenyl) -thien-3-yl]}-cyclopent-1-ene, C31H22F6O3S2

Abstract: C 3 1 H 2 2 F 6 O 3 S 2 , monoclinic, P\\2\\lc\\ (no. 14), a = 27.16(1) A, b = 9.334(2) A, c = 10.929(3) k,ß = 92.10(3)°, V= 2768.4 A, Ζ = 4, Rg^F) = 0.128, wRieffF) = 0.199, T= 293 K. Source of material The title compound was derived originally from 2-methylthiophene. First, 3,5-dibromo-2-methylthiophene was afforded in 87 % yield by bromization 2-methylthiophene in acetic acid. The next step was that one bromine was substituted by B(OH)2 in 76 % yield by borating with B(OBu)3 at -78°C using n-BuLi. Thirdly, 3-bromo-2-methyl-5-(4-formylphenyl)thiophene was prepared in 94 % yield by reacting of borate derivative with 1bromo-4-formylbenzene in presence of Pd(PPh3)4 and Na2CC>3 in tetrahydrofuran for refluxing 16 hours. The fourth step was that the carbonyl groups of 3-bromo-2-methyl-5-(4-formylphenyl)thiophene were protected as the 1,3-dioxolane groups using glycol and l-sulfonic-4-methylbenzene at Dean-Stark condition. Then, one symmetrical diarylethene compound with 1,3-dioxolane groups was prepared in 47 % yield by coupling with perfluorocyclopentene, n-BuLi and the above product in die fourth step at -78 °C under nitrogen atmosphere. Finally, the tide compound was obtained in 18 % yield by hydrolyzing in part of the symmetrical diarylethene with 1,3-dioxolane groups. Colorless crystals of the title compound were obtained by slow vapor diffusion of chloroform (m.p.: 185-186 °C). 'H NMR and MS data are available in the CIF file. Experimental details The very low ratio of Ngt/Npaam and the large R values are caused by the poor quality of the crystals obtained after several tries of preparation and by the absence of two-dimensional detector or low-temperature device. However, generally larger/? values have been observed for the structures of hexafluorodiarylethenes. Correspondence author (e-mail: pushouzhi@tsinghua.org.cn) Discussion Photochromism is referred to a reversible photo-induced transformation of a molecule between two isomers whose absorption spectra are distinguishably different [1]. Photochromic compounds have attracted much attention because of their most promising for optical storage, photo switches and display devices [2,3]. Among all photochromic compounds, diaiylethenes with heterocyclic aryl rings are the most promising for the optoelectronic devices because of their good thermal stability in both isomers, fatigue resistant character, high sensitivity and rapid response [47]. Although many diarylethenes have been so far reported, they are mainly limited to symmetrical and amorphous diarylethenes [8-14]. Unsymmetrical crystalline diarylethenes are very rare. In this paper, the structure of a novel unsymmetrical photochromic diarylethene is presented. In the perfluorocyclopentene ring of the title compound, the distances of CI—C2, C2—C3, C3—C4, C4—C5 and CI—C5 are 1.291(5) A, 1.535(5) A, 1.527(5) A, 1.557(5)Aand 1.559(5) A,respectively. These data indicate clearly that the CI =C2 bond is a double bond. There are six planar rings in the title molecule, including two benzene rings, two thiophene rings, and one perfluorocyclopentene ring and one 1,2-dioxolane ring. Therefore, these six rings can form five dihedral angles every between two adjacent rings. At the left side of the title molecule, the dihedral angle between the perfluoropentene ring (C1-C2-C3-C4-C5) and the thiophene (C6-C7-C8-C9-S1) ring is 40.5(5)°, and that between the thiophene ring and the benzene ring (CI 1-C12-C13C14-C15-C16) is 21.7(5)°. At the right side of this molecule, the dihedral angle between the perfluorocyclopentene ring and the other thiophene ring (C17-C18-C19-C20-S2) is 41.0(5)°, and that between this thiophene and the other benzene ring (C22-C23C24-C25-C26-C27) is 19.9(6)°, and that between this benzene ring and the 1,3-dioxolane ring (C28-01-C29-C30-02) is 46.1(5)°. The distance of C6—C17, the two reactive carbon atoms, is 3.60(1) A. It is short enough theoretically for the reaction to take place in the crystalline phase [15]. 2 5 6 C 3 1 H 2 2 F 6 O 3 S 2 Table 1. Data collection and handling. Crystal: blue plate, size 0.04 χ 0.2 χ 0.3 mm Wavelength: Mo Ka radiation (0.71073 A) M2.66 cm\"1 Diffractometer, scan mode: Broker P4, ω 20ma*: 50.06° Nthklhaasurcd, N(hki}aiqoe·. 6422,4865 Criterion for lobs., N(hkl)p: U s > 2 a(l^), 1257 N(param)tc6aeä· 380 Program: SHELXTL [16] Table 2. Atomic coordinates and displacement parameters (in A2).

Crystal structure of L-tryptophanium phosphite, (C11H13N2O2)[H2PO3]

Abstract: Abstract C11H15N2O5P, orthorhombic, P212121 (no. 19), a = 5.5442(6) Å, b = 8.3603(4) Å, c = 27.427(3) Å, V = 1271.3 Å3, Z = 4, Rgt(F) = 0.053, wRref(F2) = 0.146, T = 293 K.

Refinement of the crystal structure of ytterbium nickel tetraboride, YbNiB4

Abstract: B4NiYb, orthorhombic, Pbam (no. 55), a = 5.8645(2) A, b= 11.3680(5) A, c = 3.3850(2) A, V = 225.7 A3, Z = 4, RgtfF) = 0.025, wRKf{F) = 0.026, T = 295 K. Source of material A mixture of ytterbium filings (99.95 %), nickel powder (99.98 %) and crystalline boron (99.98 %) with nominal composition YbNiB4 was compacted into a pellet and sealed into Ta tube. The primary reaction was performed at 800 °C during three days. The homogenization annealing was carried out at 1100 °C for four days. Single crystals were separated from the annealed sample by mechanical fragmentation.

Crystal structure of germanium tetrabromide, β-GeBr4, low temperature modification

Abstract: Abstract Br4Ge, monoclinic, P121/c1 (no. 14), a = 10.183(2) Å, b = 6.779(1) Å, c = 10.292(2) Å, β = 102.53(3)°, V = 693.5 Å3, Z = 4, Rgt(F) = 0.061, wRref(F2) = 0.138, T = 93 K.

Crystal structure of terf-butylammonium trifluoroacetyl-N-(terf-butylamino) dioxophosphate acetonitrile solvate hydrate (1:0.333:0.333), (C4H9NH3)[(F3C2ONH)(C4H9NH)PO2)] · 0.333 CH3CN · 0.333 H2O

Abstract: C10.667H24.667F3N3.333O3.333P, triclinic, PI (no. 2), a = 10.523(3) A, b = 16.082(5) A, c = 17.382(5) A, a = 65.120(5)°,/? = 86.867(5)°,γ = 78.073(5)°, V= 2609.2 A, Ζ = 6, Rgi(F) = 0.062, wR^F) = 0.149, T= 120 K. Source of material The title compound was synthesized by the reaction of N-trifluoroacetyl phosphoramidic dichloride (1 mmol) with terf-butylamine (4 mmol) in C H 3 C N under 4 hours stirring at 0 °C. TTie solvent was removed and the residue was washed with distilled water. Single crystals of product were obtained from a mixture of methanol and acetonitrile after slow evaporation at room temperature. Experimental details Because of the strong correlation, it was impossible to refine both thermal parameters (Ueq) and site occupancy factor (s.o.f.) simultaneously for the disordered atoms. Therefore, the refinement was done step by step: first thermal parameters, then s.o.f., then again thermal parameters and so on. Final refinement was carried out with fixed site occupancy factor. The refinement with restrained C—C bond distances revealed that the s.o.f. values are 0.63 and 0.37. The ί/eq values for C atoms are 0.062 A -0.078 A for the major part and 0.076 A 0.072 A for the minor part. Discussion In a previous study, we have reported the crystal structure of (CIOH2ONH2)PC12C>2 which consists of two symmetrically independent dichlorophosphate anions as well as cyclohexyl-tertbutylammonium cations linked by four different kinds of intermolecular hydrogen bonds [1]. The crystal structure of the title compound is composed of three symmetrically independent trifluoroacetyl-JV-(terT-butylamino)phosphate anions and three independent cations of tert-butylammonium, labeled with A, Β and C. The anion labeled with \"C indicates disorder in the tert-C4H9 moiety (see C4C, C4C', C5C, C5C', C6C and C6C' (figure, top). The PI Α—ΟΙ A, P1B—OIB and PIC—OIC bond lengths (1.477(2) A, 1.480(2) A and 1.480(2) A) are slightly longer than the P = 0 double bond length (1.45 A) [2]. The P—N(amine) bond lengths of 1.626(3) A, 1.628(3) A and 1.624(3) A for PIA—N2A, P1B—N2B and PIC—N2C, respectively, are shorter than the Ρ—Ν single bond length (1.77 A) [2] and P—N(amide) bond lengths (due to the resonance interaction of N(amide) with the C=0-n system). The phosphorus atom has slightly distorted tetrahedral configuration. The bond angles around PIA, P1B and PIC are in the range of 102.4(1)°-120.4(1)°, 102.9(1)°-119.0(1)° and 102.8(1)°-118.3(2)°, respectively. The maximum and minimnm values in each conformer are corresponding for the 02-P1 0 1 and02-Pl-Nl angles. The environments of the nitrogen atoms are practically planar. The bond angles C1A-^1A-4>1A, C3A-^I2A-P1A, C1B-J>I1B-P1B, C3B-N2B-P1B, C1C-N1C-P1C and C3C-N2C-P1C are 124.8(2)°, 126.6(2)°, 125.6(2)°, 128.7(2)°, 124.7(2)° and 129.8(2)°, respectively. These results are in agreement with the sp hybridization for nitrogen atoms, although some angles differ from the ideal values. In the network of the title structure, the organo-phosphate anions, fert-C4H9NH3 cations, H2O and CH3CN molecules produce fifteen types of hydrogen bonds leading to infinite chains running along [011]. Table 1. Data collection and handling. Crystal: colorless prism, size 0.10 χ 0.15 χ 0.45 mm Wavelength: Mo Ka radiation (0.71073 A) μ· 2.01 cm 1 Diffractometer, scan mode: Broker SMART 1000 CCD, φ/ω 2dmax: 52.24° N(hkl)measured, N(Md}umqae'· 21211,10129 Criterion for /ot», N(hkl)g: / o b s > 2 t f ( W , 5713 N(param)n fined: 604 Program: SHELXTL [3] * Correspondence author (e-mail: gholi_kh@modares.ac.ir) 388 (C4H9NH3)[(F3C20NH)(C4H9NH)P02)] · 0.333CH3CN · O.333H2O Table 2. Atomic coordinates and displacement parameters (in A). Table 2. Continued. Atom Site Occ. χ y ζ Uiw Atom Site Occ. χ y ζ Un H(1AA) 2» 0.5372 0.2304 -0.0049 0.037 H(3AA) 2 i 0.3328 0.6408 -0.0793 0.046 H(2AA) 2f 0.7234 0.0252 0.2035 0.037 H(3AB) 2 i 0.4346 0.5671 -0.0892 0.046 H(4AA) 2i 0.8115 -0.0922 0.1507 0.061 H(3AC) 2i 0.3664 0.5463 -0.0080 0.046 H(4AB) 2i 0.9132 -0.0862 0.2124 0.061 H(8AA) 2i 0.3387 0.5818 -0.2145 0.064 H(4AC) 2i 0.9591 -0.0891 0.1241 0.061 H(8AB) 21 0.2287 0.6650 -0.2106 0.064 H(5AA) 2i 0.9386 0.1499 0.0936 0.060 H(8AC) 2i 0.1886 0.5775 -0.2173 0.064 H(5AB) 2i 1.0383 0.0645 0.0854 0.060 H(9AA) 2i 0.1365 0.5436 0.0004 0.065 H(5AC) 2i 0.9924 0.0573 0.1769 0.060 H(9AB) 2i 0.0608 0.5511 -0.0805 0.065 H(6AA) 2i 0.7903 0.1383 -0.0108 0.062 H(9AC) 2i 0.1047 0.6412 -0.0817 0.065 H(6AB) 2i 0.7414 0.0428 0.0137 0.062 H(10A) 2i 0.3836 0.4275 -0.0900 0.063 H(6AC) 21 0.8892 0.0482 -0.0108 0.062 H(10B) 2i 0.2345 0.4192 -0.0891 0.063 K(1BA) 2i 0.44 il 0.4957 0.2832 0.039 H(10C) 2i 0.303! 0.4!2i -Ö.0C60 0.06: H(2BA) 2i 0.2032 0.6280 0.0763 0.040 H(3BA) 2i 0.4114 0.2338 0.2243 0.047 H(4BA) 2i -0.0237 0.6882 0.0553 0.083 H(3BB) 2i 0.3676 0.2179 0.3112 0.047 H(4BB) 2i 0.0482 0.7587 0.0706 0.083 H(3BC) 2i 0.3237 0.3104 0.2392 0.047 H(4BC) 2i -0.0812 0.7330 0.11% 0.083 H(8BA) 2i 0.2729 0.2458 0.1149 0.069 H(5BA) 2i 0.1674 0.6083 0.2814 0.089 H(8BB) 2i 0.1779 0.3310 0.1265 0.069 H(SBB) 2i 0.0353 0.6855 0.2562 0.089 H(8BC) 2i 0.1227 0.2430 0.1325 0.069 H(5BC) 2i 0.1650 0.7102 0.2071 0.089 H(9BA) 2i 0.1394 0.2119 0.3490 0.070 H(6BA) 2i -0.0191 0.5313 0.1670 0.074 H(9BB) 2i 0.0383 0.2306 0.2752 0.070 H(6BB) 2i -0.0777 0.5764 0.2310 0.074 H(9BC) 2i 0.1056 0.3129 0.2712 0.070 H(6BC) 21 0.0537 0.4986 0.2566 0.074 H(10D) 2i 0.3391 0.0950 0.2387 0.067 H(1CA) 2i 0.5984 0.2115 0.5450 0.043 H(10E) 2i 0.1903 0.0886 0.2588 0.067 H(2CA) 2i 0.2676 0.3060 0.4023 0.045 H(10F) 2i 0.2863 0.0819 0.3303 0.067 H(4CA) 2i 0.63 0.0770 0.4014 0.4120 0.117 H(3CA) 2i 0.4268 -0.0834 0.6081 0.050 H(4CB) 2i 0.63 0.0364 0.4022 0.5018 0.117 H(3CB) 2i 0.3743 -0.0795 0.6879 0.050 H(4CC) 2i 0.63 0.0531 0.3075 0.4892 0.117 H(3CC) 2i 0.3815 0.0085 0.6121 0.050 H(5CA) 2i 0.63 0.2698 0.4631 0.4099 0.113 H(8CA) 2i 0.1473 -0.0043 0.4839 0.070 H(5CB) 2i 0.63 0.3694 0.4148 0.4902 0.113 H(8CB) 2 i 0.2957 -0.0572 0.4913 0.070 H(5CC) 2i 0.63 0.2276 0.4704 0.4970 0.113 H(8CC) 2i 0.2617 0.0486 0.4812 0.070 H(6CA) 2i 0.63 0.3402 0.2752 0.6100 0.093 H(9CA) 2i 0.1444 -0.0015 0.6890 0.083 H(6CB) 2i 0.63 0.2132 0.2327 0.6166 0.093 H(9CB) 2i 0.0501 0.0234 0.6098 0.083 H(6CC) 2 i 0.63 0.2015 0.3310 0.6218 0.093 H(9CC) 2 i 0.1596 0.0827 0.5997 0.083 H(4CD) 2 i 0.37 0.1718 0.4673 0.3993 0.114 H(10G) 2 i 0.2052 -0.1630 0.7059 0.082 H(4CE) 2i 0.37 0.0680 0.4486 0.4724 0.114 H(10H) 2 i 0.2763 -0.1870 0.6318 0.082 H(4CF) 2i 0.37 0.0776 0.3968 0.4106 0.114 H(10I) 2i 0.1233 -0.1452 0.6236 0.082 H(5CD) 2i 0.37 0.3645 0.4054 0.5157 0.107 H(1SA) 21 0.4643 0.0331 0.7835 0.073 H(5CE) 2i 0.37 0.3685 0.3040 0.5912 0.107 H(1SB) 2i 0.4310 0.0862 0.6827 0.073 H(5CF) 2i 0.37 0.2576 0.3907 0.5868 0.107 H(2SA) 2/ 0.6705 0.1638 0.8260 0.070 H(6CD) 2i 0.37 0.0801 0.2642 0.5315 0.114 H(2SB) 2i 0.8109 0.0989 0.8336 0.070 H(6CE) 2 i 0.37 0.0918 0.3109 0.5952 0.114 H(2SC) 2 i 0.6842 0.0538 0.8547 0.070 H(6CF) 2i 0.37 0.1957 0.2199 0.6020 0.114 Table 3. Atomic coordinates and displacement parameters (in A). Atom Site Occ. X y ζ Un Un I/33 Un 1 / 1 3 t/23 P(1A) 21 0.64659(8) 0.17137(6) 0.12316(5) 0.0291(5) 0.0258(5) 0.0304(5) -0.0057(4) -0.0016(4) -0.0101(4) F(1A) 2 i 0.2654(2) 0.1179(2) 0.0011(1) 0.051(1) 0.055(2) 0.055(1) -0.028(1) -0.014(1) -0.004(1) F(2A) 2i 0.4344(2) 0.1079(2) -0.0689(2) 0.067(2) 0.079(2) 0.057(2) 0.010(1) -0.018(1) -0.044(1) F(3A) 2i 0.3419(2) 0.2386(2) -0.0706(1) 0.050(1) 0.038(1) 0.052(1) -0.014(1) -0.020(1) 0.001(1) 0(1A) 2 i 0.5666(2) 0.1730(2) 0.1952(1) 0.033(1) 0.035(1) 0.033(1) -0.004(1) -0.003(1) -0.013(1) CK2A) 2 i 0.7182(2) 0.2465(2) 0.0768(1) 0.031(1) 0.027(1) 0.040(1) -0.006(1) -0.003(1) -0.011(1) 0(3A) 2i 0.4462(2) 0.0588(2) 0.1199(1) 0.047(2) 0.033(1) 0.032(1) -0.016(1) -0.001(1) -0.006(1) N(1A) 2i 0.5385(3) 0.1831(2) 0.0451(2) 0.032(2) 0.026(2) 0.029(1) -0.007(1) -0.002(1) -0.006(1) N(2A) 2i 0.7406(3) 0.0683(2) 0.1546(2) 0.035(2) 0.026(2) 0.024(1) -0.004(1) -0.001(1) -0.004(1) C(1A) 2i 0.4585(3) 0.1264(2) 0.0554(2) 0.031(2) 0.026(2) 0.036(2) -0.005(2) 0.001(2) -0.013(2) C(2A) 2/ 0.3740(3) 0.1480(2) -0.0217(2) 0.035(2) 0.031(2) 0.036(2) -0.008(2) -0.005(2) -0.010(2) C(3A) 2 i 0.8517(3) 0.0396(2) 0.1096(2) 0.036(2) 0.030(2) 0.033(2) -0.004(2) 0.003(2) -0.011(2) C(4A) 2i 0.8870(4) -0.0663(2) 0.1530(2) 0.042(2) 0.032(2) 0.042(2) -0.001(2) -0.001(2) -0.012(2) C(5A) 2 i 0.9654(3) 0.0816(3) 0.1170(2) 0.036(2) 0.038(2) 0.042(2) -0.006(2) 0.002(2) -0.012(2) C(6A) 2i 0.8149(4) 0.0699(3) 0.0173(2) 0.043(2) 0.044(2) 0.033(2) -0.002(2) 0.003(2) -0.016(2) P(1B) 2 i 0.31583(8) 0.50589(6) 0.17606(5) 0.0283(5) 0.0272(5) 0.0340(5) -0.0058(4) -0.0024(4) -0.0106(4) F(1B) 2i 0.5228(3) 0.7154(2) 0.2552(2) 0.105(2) 0.039(1) 0.090(2) -0.005(1) -0.051(2) -0.028(1) F(2B) 2 i 0.6587(2) 0.5999(2) 0.2550(2) 0.040(1) 0.088(2) 0.076(2) -0.010(1) -0.012(1) -0.041(2) F(3B) 2 i 0.5148(3) 0.5790(2) 0.3460(1) 0.093(2) 0.091(2) 0.039(1) -0.054(2) -0.002(1) -0.020(1) 0(1B) 2 i 0.3965(2) 0.4914(2) 0.1086(1) 0.031(1) 0.032(1) 0.036(1) -0.002(1) -0.006(1) -0.011(1) 0(2B) 2 i 0.2712(2) 0.4255(2) 0.2429(1) 0.034(1) 0.026(1) 0.043(1) -0.010(1) 0.002(1) -0.009(1) (C4H9NH3)[(F3C20NH)(C4H9NH)P02)] · 0.333 CH3CN · 0.333 H 20 389

Crystal structure of barium selenate, BaSeO4

Abstract: BaC^Se, orthorhombic, Prima (no. 62), a = 8.993(8) A, b = 5.675(6) Ä, c = 7.349(4) Ä, V = 375.1 Ä, Ζ = 4, Rgt(F) = 0.042, wRnftF) = 0.116, T= 293 K. Source of material Crystallization of BaSeC>4 single crystals was carried out in a double-diffusion system where parent aqueous solutions of two reagents are separated by a column of silica hydrogel. Crystal growth in gels is in fact solution growth, although nucleation and growth conditions are quite different from those in conventional solution growth methods. The gel is a porous medium that suppresses convection and advection, only allowing diffusion of reacting ions, which eventually meet in the gel column where precipitation occurs. This method has been used extensively as a way of growing crystals of sparingly soluble salts from aqueous solutions [ 1 ]. In the present experiments, the two parent solutions (0.5 Μ BaCh and 0.5 Μ Na2SeC>4) were separated by a 28 cm column of silica hydrogel in a U-shaped tube. The gel was prepared by acidification of a sodium silicate solution with 1 Μ HCl to the desired pH of 5.5. The acidified solution was poured into the Utube, where it polymerized to form a solid gel. In all the aqueous solutions reagent grade chemicals (Merck) were used. During the experiment the temperature was maintained to 25.0±0.1 °C. Experimental details Hie high main residual electron density, ca. 4 eÄ , located near Ba and the odd thermal parameters for 01 and 02 reflect the low quality of the only available barium selenate crystals. Discussion Selenate is the predominant form of Se in soils and water. Selenate and sulfate ions have similar chemical properties and structures and, when both are present, compete in many processes such are sorption on mineral surfaces, absorption by plants and incorporation into plant and animal tissues [2-4]. Because of selenate* s toxicity and its mobility the relationship between selenate and sulfates in soils has been the subject of attention by researchers, mainly in the context of agricultural sciences [5,6]. However, the relationship between selenate and common sulfates mineral crystal structures are not always clear. The crystal structure studies of BaSeC>4 in the literature indicate that is isomorphous with barite, the corresponding sulfate [7]. The sulfate and selenate anions are both tetrahedral and even though the selenate anion is larger, the structures of many selenates are isomorphous with those of the corresponding sulfates [8,9]. These studies are limited to the determination of the cell parameters and space group, but the determination and refinement of the structure of BaSeÖ4 have not been completed until now. BaSe04 crystallizes orthorhombically and its structure is isomorphous with barite 0-BaSC>4). The structure consists of isolated SeC>4 tetrahedra joined by barium atoms coordinated to twelve oxygen atoms forming irregular BaOi2 polyhedra. The structure is easier to visualize by considering the six closest oxygen atoms to each barium. These atoms form chains of distorted BaOe octahedra parallel die α-axis, in the direction that those are linked by Se04 tetrahedra. Table 1. Data collection and handling.

Crystal structure of iodoferrocene, Fe(C5H4I)(C5H5)

Abstract: CioHgFel, monoclinic, Plcl (no. 7), a = 6.3676(2) A, b = 9.8475(4) A , c = 15.2298(6) k,ß = 93.015(2)°, V = 953.7 A, Ζ = 4, R f f f F ) = 0.018, wR^F) = 0.038,

Crystal structure of 5-chloro-2-methylanilinium chloride hydrate, (ClC7H6NH3)Cl · H2O

Abstract: H(l) 2a 0.0412 0.4851 0.1320 0.059 H(2) 2a 0.1675 0.3395 0.1240 0.059 H(3) 2a 0.2294 0.5261 0.1345 0.059 H(7) 2a 0.5339 0.3477 0.6358 0.057 H(8) 2a 0.3123 0.3899 0.7725 0.059 H(9) 2a -0.0504 0.4937 0.3624 0.048 H(4) 2a 0.4851 0.2833 0.2425 0.074 H(5) 2a 0.6324 0.3128 0.4009 0.074 H(6) 2a 0.5596 0.4780 0.2912 0.074 H(10) 2a -0.4659 0.1646 0.9596 0.098 H(ll) 2a -0.3295 0.2956 0.9651 0.098

Crystal structure of diytterbium pentadecanickel nonaboride, Yb2Ni15B9?

Abstract: B9Nii5Yb2, orthorhombic, Cmca (no. 64), a = 15.925(2) A, b= 11.590(1) A ,c= 11.232(1) A, V=2073.1 A \ z = 8 , Rgl(F) = 0.033, wRniF) = 0.054, T= 293 K. Source of material The title compound was obtained by systematic investigation of the Yb-Ni-B system. The samples were melted in the arc furnace (purified argon atmosphere) from compact Yb (99.5 wt. %) and powders of Ni (99.98 wt. %) and Β (99.4 wt. %), which were previously mixed and pressed. Each alloy was wrapped in Mo-foil and annealed at 1070 Κ for 700 h in the evacuated quartz tube. Single needle-like crystals with metallic luster were extracted from the compact alloy with nominal composition Yb2Nii5B9. Discussion The existence of Yb2NiisB9 (structure type H02N115B9 [1]) was established in [2], but only unit cell parameters were determined, the atomic coordinates were not specified. The ΖΛ2Ν115Β9 (Ln = Y, Tb, Dy, Er, Tm, Lu) borides belong also to Ho2NiisB9-structure type [2], but crystal structure was fully examined only for H02N115B9. The single crystal investigation of Yb2NiisB9 showed lattice parameters in good agreement with the results of X-ray powder diffraction method [2], Metal atoms in the Yb2Nii5B9 structure are characterized by high coordination numbers (CN): the Yb atoms have CN = 20 and 18, the Ni atoms -16, 14 and 13. Coordination spheres of the boron atoms are distorted Archimedean cubes which are connected with one another by square faces (B2-B3 and B4-B6). The Β1 atoms center a trigonal prism composed of the metal atoms. The B5 atoms are also situated in a trigonal prism, in which one of the apices is occupied by a B5 atom. As a result, the boron atoms in Yb2NiisB9 are either isolated (Β 1) or form pairs (other boron atoms). Thus, according to the common tendency, the increase in boron content in a boride leads to substitution of isolated boron atoms (structure types Ti3Co5B2, TiNiSi, CeCo3B2) by B2 pairs (structure types Z1C03B2, CeCo4B4, NdCo4B4>, B„ chains (structure types W3C0B3, Μ02ΙΓΒ2), Bn zigzag chains (structure types NdCoB2, CrB, FeB) or layers (structure types AIB2, YCrBi, Y2ReBe) [3]. The minimal interatomic distances for Yb atoms are well correlated with the distances in the other boride structures. Specifically, d(Ybl—Ni3) and

Crystal structure of disamarium undecaoxotetratellurate(IV), Sm2Te4O11

Abstract: 0.0267(4) 0.0911(9) 0.0995(3) 0.007(2) 0.012(2) 0.011(2) -0.004(2) 0.001(2) -0.006(2) 0(2) 8/ 0.2061(4) 0.0410(9) 0.4435(3) 0.013(3) 0.011(2) 0.011(2) -0.006(2) 0.005(2) -0.008(2) 0(3) 8/ 0.2502(4) 0.0646(8) 0.1293(3) 0.010(2) 0.011(2) 0.011(2) -0.005(2) 0.003(2) -0.003(2) 0(4) 8/ 0.3520(4) 0.0551(9) 0.3290(3) 0.018(3) 0.011(2) 0.007(2) 0.004(2) 0.004(2) 0.000(2) 0(5) 8/ 0.4283(4) 0.1185(9) 0.0460(3) 0.009(2) 0.011(2) 0.014(2) -0.002(2) 0.002(2) -0.005(2) 0(6) 4e

Crystal structure of naphthalen-1-yl-(4-nitro-benzylidene)-amine, C17H12N2O2

Abstract: C17H12N2O2, orthorhombic, P2\\2\\2\\ (no. 19), a = 7.2528(8) A, b = 12.301(1) A, c = 15.208(1) A, V = 1356.8 A, Ζ = 4, Rgf(F) = 0.046, w R ^ F ) = 0.107, Γ= 273 Κ. Source of material 1-Naphthylamine (0.1 mmol, 14.3 mg) and 4-nitrobenzaldehyde (0.1 mmol, 15.1 mg) were dissolved in methanol (10 ml). The mixture was stirred for 60 min at room temperature to give a clear yellow solution. After allowing the resulting solution to stand in air for 10 d, yellow prismatic crystals were formed at the bottom of the vessel by slow evaporation of the solvent. The crystals were isolated by filtration, washed with methanol and dried in a vacuum desiccator using anhydrous CaCk (yield 86 %). Elemental analysis: found C, 73.8 %; H, 4.4 %; N, 10.2 %; calc. for C17H12N2O2 C, 73.9 %; H, 4.4 %; N, 10.1 %. Discussion Schiff base compounds play an important role in the development of coordination chemistry related to catalysis and enzymatic reaction, magnetism and molecular architectures [1,2]. The crystal structure of the title compound is built up by only the C17H12N2O2 molecules, within which all the bond lengths are in Table 3. Atomic coordinates and displacement parameters (in A). normal ranges [3]. The dihedral angle between the CI C6 phenyl ring and the C8 C17 naphthalene system is 33.8(4)°, and the torsion angles are 178.1(2)° for C2-C3-C4-C7 and -177.7(3)° for C7-C4-C5-C6. As expected, the molecule adopts a trans configuration about the C7=N2 bond. Hie C7=N2 bond length of 1.267(3) A conforms to the value for a normal C=N double bond. Because of conjugation through the imino double bond C7=N2, the C1 C6 phenyl ring and the C8 C17 naphthalene system show a weak distortion. The C7—C4 bond length of 1.469(3) A is shorter than C-C(=C) of 1.51 A [4], Table 1. Data collection and handling. Crystal: Wavelength: μDiffractometer, scan mode: 20max: N(hJU)mcaamA, N(hkl)uniqpe'· Criterion for W Nfhklfo: Nfparam^Bncd·· Program: yellow prism, size 0.14 χ 0.32 χ 0.34 mm Mo Ka radiation (0.71073 A) 0.91 cm\"' Broker SMART CCD, ω 50.06° 6115,2385 labs > 2 σ( lobs), 1604 191 SHELXTL [5] Table 2. Atomic coordinates and displacement parameters (in A). Atom Site X y ζ Uiso H(2) 4a 0.0277 0.3641 0.7409 0.064 H(3) 4a 0.0367 0.2416 0.6257 0.059 H(5) 4a 0.2154 0.4778 0.4656 0.067 H(6) 4a 0.2098 0.5998 0.5814 0.067 H(7) 4a 0.1853 0.2953 0.4064 0.061 H(9) 4a 0.0339 0.2088 0.3002 0.068 H(10) 4a 0.0463 0.0881 0.1820 0.078 H(l l ) 4a 0.1363 -0.0866 0.2035 0.075 H(13) 4a 0.2283 -0.2359 0.3041 0.082 H(14) 4a 0.2843 -0.2976 0.4418 0.094 H(15) 4a 0.2520 -0.1819 0.5626 0.092 H(16) 4a 0.1757 -0.0040 0.5423 0.073 Atom Site X y ζ Un t/22 i/33 Un Un t/23 C(l) 4a 0.1199(3) 0.4921(2) 0.6703(2) 0.046(2) 0.052(2) 0.049(1) 0.008(1) -0.004(1) -0.011(1) C(2) 4a 0.0665(3) 0.3861(2) 0.6854(2) 0.052(2) 0.061(2) 0.046(1) 0.001(1) 0.001(1) 0.005(1) C(3) 4a 0.0718(3) 0.3135(2) 0.6167(2) 0.052(2) 0.041(1) 0.054(1) 0.000(1) -0.001(1) 0.001(1) C(4) 4a 0.1291(4) 0.3471(2) 0.5341(1) 0.044(1) 0.042(1) 0.048(1) 0.000(1) 0.001(1) -0.001(1) C(5) 4a 0.1790(4) 0.4547(2) 0.5212(2) 0.071(2) 0.044(1) 0.053(1) -0.002(1) 0.004(1) 0.004(1) * e-mail: wenpuhong0903@163.com 398 C 1 7 H 1 2 N 2 O 2

Crystal structures of 1,4-di(1-imidazolyl)butane dihydrochloride, (C10H16N4)Cl2, and 1,4-di( 1-imidazolyl)butane dihydrate, C10H14N4 · 2H2O

Abstract: C10H16CI2N4, monoclinic, C12/cl (no. 15), a = 15.915(3) A, b = 8.230(2) A, c = 10.189(2) A, β = 103.98(3)°, V= 1295.0 A3, Z = 4, Rgt(F) = 0.038, wRieffF2) = 0.113, T = 293 K. crystallographic data obtained for the salt (DIBHC1) and the neu- tral molecule l,4-di(l-imidazolyl)butane have been compared. It was found that protonation of the nitrogen atoms of imidazole ring causes very significant changes in conformation of DIBHC1 molecule (figure, top) in comparison to DIB one (figure, bottom). In the neutral DIB molecule the imidazole rings have trans-(ap)- position in respect to C7—C7' bond (ZC6-C7-C7-C6' = 180.0°). However, after protonation the rings in question have gauche-(sc)-coafoTmauon (Z.C6-C7-C7-C6' = 79.9(3)°)due to strong interactions between N-H* of the imidazolium ions and chloride anions, d(N3-Cl) = 3.035(3) A and Z.N3-H3-C1 = 169.21(3)° (figure, top). The molecules of DIBHC1 as well as DIB lie in special positions, but possess in the center of the mole- cule a two-fold rotation axis and a centre of symmetry, re- spectively. Contrary to DIBHC1, the DIB crystallizes with two molecules of water, which in the crystal lattice create chains joined by hydrogen bonds, parallel to the ύ-axis (d(0 ~0) = 2.892(3) A and ZO-HIW-O(-χ+3Λ,γ+X,ζ) = 165.91(3)°). There are also intermolecular hydrogen bonds between water and nitrogens from imidazole ring with