Showing papers in "Zeitschrift Fur Kristallographie-new Crystal Structures in 2014"

The twinned crystal structure of bis((4-aminopyridin-1-ium) iodide triiodide, C20H28I8N8

Abstract: C20H28I8N8, C2/c (no. 15), a = 17.2334(2) Å, b = 13.95310(10) Å, c = 29.3522(3) Å, & = 91.0960(10)°, V = 7056.7 Å, Z = 8, Rgt(F) = 0.0458, wRref(F ) = 0.1195, T = 290 K.

Refinement of cesium diaquatrichloromanganate(II), CsMnCl3·2(H2O) by neutron diffraction, Cl3CsH4MnO2

Abstract: Cl3CsH4MnO2, orthorhombic, Pcca (no. 54), a = 9.1197(11) Å, b = 7.3240(5) Å, c = 11.533(7) Å, V = 770.3 Å, Z = 4, Rgt(F) = 0.0694, wRref(F ) = 0.1703, T = 300 K.

Crystal structure of N-(methoxy)methanethioylbenzamide, C9H9NO2S

Abstract: C9H9NO2S, orthorhombic, Pna21 (no. 33), a =9 .6168(2) A, b =9 .0206(2) A, c =1 1.0006(2) A, V =9 54.3 A 3 , Z =4 , Rgt(F) =0 .0242, wRref(F 2 ) =0 .0659, T =2 00 K. Source of material Th et itle compound was obtained upon reacting benzoyl chloride with ammonium thiocyanate in acetone and, subsequently, with boiling methanol. Crystals suitable for the Xray analysis were obtained upon storage of the oily residue at room temperature for one week. Experimental details Carbon-bound Ha toms were placed in calculated positions (C–H 0.95 Af or aromatic carbon atoms) and were included in the refinement in the riding model approximation, with Uiso(H) se tt o 1.2Ueq(C). The Ha toms of the methyl group were allowed to rotate with af ixed angle around the C–C bond to best fit the experimenta le lectron density (HFIX 137 in the SHELX program suite [5]), with Uiso(H) se tt o1 .5Ueq(C). The nitrogen-bound Ha tom was placed in ac alculated position (N–H 0.88 A) and was included in the refinement in the riding model approximation, with Uiso(H) se tt o1 .2Ueq(N).

Crystal structure of Scheelite-type potassium cerium bis(tetraoxomolybdate( VI)), KCe(MoO4)2

Abstract: Abstract CeKMo2O8, tetragonal, I41/a (no. 88), a = 5.420(1) Å, c = 12.119(3) Å, V = 356.0 Å3, Z = 2, Rgt(F) = 0.0752, wRref(F2) = 0.1639, T = 293 K.

Crystal structure of 2-nor-1,2-secolycoserone, C24H32O4

Abstract: C24H32O4 ,o rthorhombic, P212121 (no. 19), a =7 .0809(3) A, b =1 5.0684(6) A, c =2 0.6315(10) A, V =2 201.3 A 3 , Z =4 , Rgt(F) =0 .0304, wRref(F 2 ) =0 .0753, T =1 73 K.

Crystal structure of 3-aminium-pyridin-1-ium bis(triiodide) dihydrate, C5H12I6N2O2

Abstract: C5H12I6N2O2, orthorhombic, Cmc21 (no. 36), a = 11.58920(14) A, b = 8.53178(11) A, c = 17.4355(2) A, V = 1724.0 A, Z = 4, Rgt(F) = 0.0155, wRref(F ) = 0.0342, T = 293 K.

Crystal structure of lappaconitine-ium nitrate monohydrate, C32H47N3O12

Abstract: C32H47N3O12, monoclinic, P21 (no. 4), a = 10.5829(4) Å, b = 12.4835(5) Å, c = 12.3115(5) Å, $ = 91.699(2)°, V = 1625.8 Å, Z = 2, Rgt(F) = 0.0415, wRref(F ) = 0.1016, T = 294 K.

Crystal structure of the inorganic-organic hybrid material tris(N,Nʹ- dimethylethylenediammonium) bis(hexachloridorhodate(III)) dihydrate, C6H23Cl6N3ORh

Abstract: Abstract C6H23Cl6N3ORh, triclinic, P1¯ (no. 2), a = 6.9907(2) Å, b = 7.7437(3) Å, c = 15.8733(5) Å, α = 78.590(3)°, β = 89.035(2)°, γ = 85.304(2)°, V = 839.5 Å3, Z = 2, Rgt(F) = 0.0292, wRref(F2) = 0.0585, T = 295 K.

Redetermination of the crystal structure of di-2-pyridylketone 2- aminobenzoylhydrazone, at 200 K – Localisation of hydrogen atoms, C18H15N5O

Abstract: C18H15N5O, monoclinic, P21/c (no. 14), a = 11.4450(4) Å, b = 8.5980(3) Å, c = 15.5640(6) Å, $ = 92.678(1)°, V = 1529.9 Å, Z = 4, Rgt(F) = 0.0381, wRref(F ) = 0.1054, T = 200 K.

Crystal structure of 3-bromo-N-[4-chloro-2-methyl-6-[(methylamino)- carbonyl]phenyl]-1-(3-chloro-2-pyridinyl)-1H-pyrazole-5-carboxamide, C18H14BrCl2N5O2

Abstract: C18H14BrCl2N5O2, monoclinic, P21/n (no. 14), a = 8.945(3) Å, b = 17.742(5) Å, c = 13.187(4) Å, $ = 107.520(3)°, V = 1995.7 Å, Z = 4, Rgt(F) = 0.0572, wRref(F ) = 0.1612, T = 296 K.

Crystal structure of poly[bis-μ3-[(2-(1,2,4-triazol-1-yl)acetato-κ3 O:O':N)]- cobalt(II), [Co(C4H4N3O2)2]n, C8H8CoN6O4

Abstract: C8H8CoN6O4, monoclinic, P21/n (no. 14), a = 8.464(1) Å, b = 4.8374(5) Å, c = 11.976(2) Å, \" = 91.415(4)°, V = 490.2 Å, Z = 2, Rgt(F) = 0.0361, wRref(F ) = 0.0872, T = 223 K.

The crystal structure of N-(1-(dimethyl-l4-azanylidene)ethyl)propan-2- amine, a Z'1 structure, C8H18N2

Abstract: C8H18N2, monoclinic, P21/n (no. 14), a = 9.708(9) Å, b = 14.988(17) Å, c = 13.207(12) Å, \" = 95.92(3)°, V = 1911.4 Å, Z = 8, Rgt(F) = 0.0369, wRref(F ) = 0.0937, T = 100 K.

Crystal structure of the trinuclear complex hexachlorido-1κ3Cl,3κ3Cl-bis(µ2-dimethylphosphorylmethanamine-1:2κ2N:O,3:2κ2N:O)- bis(dimethylphosphorylmethanamine-2κ2N,O)trizinc(II), C12H40Cl6N4O4P4Zn3

Abstract: C12H40Cl6N4O4P4Zn3, monoclinic, C2/c (no. 15), a = 16.8933(5) Å, b = 9.1740(4) Å, c = 21.5013(7) Å, \" = 97.627(3)°, V = 3302.8 Å, Z = 4, Rgt(F) = 0.0317, wRref(F ) = 0.0784, T = 290 K. Source of material 0.78 g (7.17 mmol) (Dimethylphosphoryl)methanamine (dpma) was dissolved in basic ethanol (p.a., adjusted to pH 8-9 by an ammonium hydroxide solution (20%), 1,5 ml). To get a molar ratio of 3:4 zinc(II)chloride : dpma, 0.73 g (5.38 mmol) zinc(II)chloride was added to the solution. The reaction mixture was heated to 50 °C and stirred for 2 h. Cooling to room temperature yielded in a viscose liquid. Recrystallization from ethanol by slow evaporation at 60 °C – gave needle shaped colourless crystals. The Raman spectrum was measured using a neodymium doted yttrium-aluminum-garnet-laser (Nd:YAG) on a MultiRam spectrometer from Bruker, 4000-60 cm: 3282(w), 3254(m), 3224(w, sh), 3176(m), 3121(w), 2983(s), 2953(m), 2945(m), 2914(vs), 2826(w), 2814(w), 2793(w), 2587(vw), 1414(s), 1370(w), 1170(m), 1156(m), 1127(s), 1082(w), 1047(vw), 1020(w), 922(vw), 898(vw), 859(vw), 806(vw), 773(m, sh), 766(m), 740(m), 731(m, sh), 675(s), 593(w), 494(vw), 466(w), 399(m), 373(m), 363(m, sh), 324(m, sh), 310(m, sh), 279(s), 206(m), 175(m, sh), 119(s), 108(s, sh), 83(m, sh), 68(m). The Raman bands at 310 cm and 292 cm can be assigned to Zn–Cl stretching frequencies whereas the broad signal at 279 cm can be assigned to the Zn–N stretching frequencies [1, 2]. IR spectroscopic data were collected on a Digilab FT3400 spectrometer using a MIRacle ATR unit (Pike Technologies) 4000560 cm: 3274(s), 3250(s, sh), 3223(vs), 3173(m), 3121(m), 2983(w), 2913(w), 1611(m), 1589(w), 1425(m, sh), 1415(m), 1401(w, sh), 1362(w), 1315(m, sh), 1311(m, sh), 1299(s), 1272(w), 1147(s), 1122(vs), 1078(s), 1020(m), 943(s), 891(s), 859(m), 804(w), 791(w), 765(m), 739(w), 730(w), 686(m), 670(w), 593(w). Experimental details Nitrogen bound hydrogen atoms were refined freely with individual Uiso values. Carbon bound hydrogen atoms were included in 440 Z. Kristallogr. NCS 229 (2014) 440-442 / DOI 10.1515/ncrs-2014-9047 © 2014 by Walter de Gruyter Berlin/Boston Crystal: colourless block (cut from a needle), size 0.32!0.28!0.25 mm Wavelength: Mo K% radiation (0.71073 Å) $: 28.65 cm Diffractometer, scan mode: Xcalibur, Eos, # 2$max: 55° N(hkl)measured, N(hkl)unique: 13600, 3746 Criterion for Iobs, N(hkl)gt: Iobs > 2 !(Iobs), 3126 N(param)refined: 170 Programs: CrysalisPRO, SHELX, DIAMOND [3–5] Table 1. Data collection and handling.

Redetermination of the crystal structure of 1,4-dithiane, at 200 K – Analysis of intermolecular forces, C4H8S2

Abstract: C4H8S2, monoclinic, P2/c (no. 14), a = 6.7630(3) Å, b = 5.4100(2) Å, c = 10.0272(4) Å, $ = 129.660(2)°, V = 282.4 Å, Z = 2, Rgt(F) = 0.0182, wRref(F ) = 0.0510, T = 200 K.

Crystal structure of 8-(2-methylphenyl)-11-[(E)-(2-methylphenyl)- methylidene]-14-hydroxy-3,13-diazaheptacyclo- [13.7.1.9,13.02,9.02,14.03,7.019,23]tetracosa-1(22),15,17,19(23),20-pentaen-10- one methanol monosolvate, C37H34N2O2-CH3OH, C38H38N2O3

Abstract: Abstract C38H38N2O3, monoclinic, P21/c (no. 14), a = 11.3562(2) Å, b = 17.0817(4) Å, c = 15.2368(3) Å, β = 93.539(1)°, V = 2950.1 Å3, Z = 4, Rgt(F) = 0.0498, wRref(F2) = 0.1133, T = 293 K.

Crystal structure of desvenlafaxinium 3,5-dinitrobenzoate 3,5-dinitrobenzoic acid monohydrate, C30H35N5O15

Abstract: In the crystal, a mol. of H2O is present next to 1 addnl. mol. of the non-dissocd. carboxylic acid. While the least-squares planes defined by the atoms of the nitro groups of the deprotonated carboxylic acid enclose angles of 5.8(2) and 9.8(2)° with the plane defined by the C atoms of the arom. system they are bonded to, the least-squares plane defined by the atoms of the carboxylate group intersect with the aromat's plane at an angle of 13.88(14)°. The resp. values for the co-crystd. carboxylic acid are found at 4.9(2) and 7.25( 16)° for the nitro groups and 11.12( 16)° for the least-squares plane defined by the non-H atoms of the carboxylic acid group on the 1 hand and the plane defined by the C atoms of the arom. system they are bonded to on the other hand. According to a puckering anal., the satd. 6-membered ring adopts a 4C1 conformation (C24CC21). In the crystal, H bonds of the N-H···O as well as the O-H···O type are obsd. In total, the different moieties of the title compd. are connected to a 3-dimensional network. The shortest intercentroid distance between two centers of gravity was measured at 4.2942(8) A… and is apparent between the arom. system of the cation as well as the Ph ring of the deprotonated carboxylic acid. Crystallog. data are given.

Crystal structure of the inorganic-organic hybrid material bis(N,Ndimethyl- 1,3-diammoniopropane) hexachloridorhodate(III) chloride, [(CH3)2NH(CH2)3NH3]2[RhCl6]Cl, C10H32Cl7N4Rh

Abstract: C10H32Cl7N4Rh, monoclinic, P21/c (no. 14), a = 10.6247(1) Å, b = 11.2582(1) Å, c = 19.0137(2) Å, \" = 104.100(1)°, V = 2205.8 Å, Z = 4, Rgt(F) = 0.0306, wRref(F ) = 0.0889, T = 295 K.

Crystal structure of 1-(5-acetyl-3,4-dimethyl-thieno[2,3-b]thiophen-2-yl)- ethanone, C12H12O2S2

Abstract: C12H12O2S2, orthorhombic, Pbcn (no. 60), a = 11.867(2) Å, b = 13.357(2) Å, c = 7.368(1) Å, V = 1167.9 Å, Z = 4, Rgt(F) = 0.0411, wRref(F ) = 0.1128, T = 273 K.

Crystal structure of 3,4-dihydro-2-methylquinazoline hydrochloride hemihydrate, C18H24Cl2N4O

Abstract: C18H24Cl2N4O, triclinic, P1 (no. 2), a = 7.5152(3) Å, b = 7.5571(3) Å, c = 17.2245(7) Å, ' = 89.873(1)°, % = 80.854(1)°, ! = 89.782(1)°, V = 965.8 Å, Z = 2, Rgt(F) = 0.0312, wRref(F ) = 0.0875, T = 200 K.

Crystal structure of bis(4,5-diaza-fluoren-9-one-κ2N,N) dioxo-μ2- oxodirhenium(V)- acetonitrile (1:2), C26H18Cl4N6O5Re2

Abstract: C26H18Cl4N6O5Re2, monoclinic, P21/c (no. 14), a = 10.0110(4) Å, b = 14.1829(6) Å, c = 10.7113(4) Å, % = 96.265(2)°, V = 1511.8 Å, Z = 2, R(F) = 0.0230, wRref(F ) = 0.0542, T = 200 K.

Crystal structure of (Z)-methyl N'-(5,7-dibromo-1-(2-morpholinoethyl)-2- oxoindolin-3-ylidene)hydrazinecarbodithioate, C16H18Br2N4O2S2

Abstract: C16H18Br2N4O2S2, monoclinic, P21/c (no. 14), a = 7.8158(3) Å, b = 27.890(1) Å, c = 9.5004(4) Å, & = 105.135(2)°, V = 1999.1 Å, Z = 4, Rgt(F) = 0.0316, wRref(F ) = 0.0709, T = 296 K.

Crystal structure of (E)-3-(1-iodoethylidene)-2,3-dihydro-[1,4]thiazino- [2,3,4-ij]quinolin-4-ium triiodide, C13H11I4NS

Abstract: We thank financial support from Spanish Ministerio de Economia y Competitividad (MAT2010-15094, FPUgrant AP2008-03942 to A.D.) and EDRF. This work was supported by the Russian Ministry for Education and Science.

Crystal structure of (E)-methyl-N'-(3,5-dimethoxy-4-hydroxybenzylidene) hydrazinecarboxylate, C11H14N2O5

Abstract: C11H14N2O5, trigonal, R3c (no. 161), a = 25.868(8) Å, c = 10.074(4) Å, V = 5838.0 Å, Z = 18, Rgt(F) = 0.0397, wRref(F ) = 0.1013, T = 223 K. Source of material Methyl hydrazinecarboxylate (0.9 g, 10 mmol) and 3,4dimethoxy-5-hydroxybenzaldehyde (1.22 g, 10 mmol) were dissolved in stirred methanol (30 ml). The reaction mixture was refluxed for 3-4 h with TLC (thin layer chromatography) monitoring (ethyl acetate:hexane = v:v = 7:3). The resulting solid was filtered off and recrystallized from ethanol to give the title compound. Experimental details The H atoms attached to the N atom was located from the difference Fourier map, and refined freely. All other H atoms were positioned geometrically (O–H = 0.82 Å and C–H = 0.93 or 0.96 Å) and refined using a riding model, with Uiso(H) = 1.2 Ueq(C,N) and 1.5Ueq(Cmethyl).

The layered crystal structure of piperazine-1,4-diium diiodide – diiodine (1:1), C4H12I4N2

Abstract: C4H12I4N2, triclinic, P1 (no. 2), a = 6.4800(6) Å, b = 7.4090(7) Å, c = 8.0824(8) Å, ( = 63.939(10)°, ' = 67.290(10)°, ! = 69.471(9)°, V = 313.8 Å, Z = 1, Rgt(F) = 0.0201, wRref(F ) = 0.0507, T = 100 K. Source of material 86.1 mg (1 mmol) piperazine, 253.8 mg (1 mmol) I2 and 0.15 mL hydroiodic acid (58%; 2 mmol) were sealed in a thick-walled borosilicate glass tubing. Heating up to 130 °C and slow cooling (10 °C/h) to room temperature gave orange-red crystals of the title compound in almost quantitative yield. The Raman spectrum (Bruker MULTIRAM spectrometer (Nd:YAG-Laser at 1064 nm; RT-InGaAs-detector; back scattering geometry)) shows only one very strong signal at 169 cm whereas all other signals are weak. Experimental details The hydrogen atoms attached to the carbon atoms were included in the latest stages of the refinement using a riding model with their Uiso values set to 1.2Ueq(C). For the positions of the hydrogen atoms of the NH2 + group the AFIX 24 option of the SHELX system [2] was used which allows a change of the N–H distance during the refinement. One common Uiso value was refined for these two hydrogen atoms. The highest difference electron density peak (1.04 e!Å) is 0.88 Å apart from I1. Discussion Polyiodides, built from I, I2 and I3 – subunits, fulfill the general formula I m n n 2 $ \" (n = 1–4, m = integer) [4–8] and are connected via halogen bonds. The halogen bonding received much attention because of its influence on the functionality of biological systems and its role in the crystal engineering of new materials for various applications [9, 10]. Because of their potential use as Agent Defeat Weapons (ADW) [11] there is a general interest in iodinerich compounds. Furthermore, it has been proved that diaminium and pyridinium iodides and corresponding polyiodides influence the redox chemistry in dye-sensitized solar cells [12, 13]. Several new polyiodides have been synthesized and structurally characterized in the (,)-diamonioalkane iodide / diiodine system [14–18]. In these cases the lengths of the stick-shaped cations excellently fit with the topologies of the corresponding polyiodides. This synthetic protocol is known as dimensional caging [19]. This contribution is part of our ongoing interest on the synthesis of new polyiodides using nitrogen containing cyclic cations [20–22]. The asymmetric unit of the title structure contains one half of a piperazine-1,4-diium dication (pipH2 ) and one half of a diiodine molecule, both located around inversion centers. Whereas the iodide anion is placed in a general position. The geometric parameters of the pipH2 2+ cation exhibiting an all-chair conformation are all in the expected ranges (C–C: 1.505(7) Å; C–N: 1.485(6) and 1.498(6) Å). All moieties are connected by hydrogen and halogen bonds, respectively (Figure, upper part; ' = 1–x, 1–y, 1–z; '' = 2–x, –y, –z) [23]. Each dication is connected to four iodide anZ. Kristallogr. NCS 229 (2014) 423-424 / DOI 10.1515/ncrs-2014-9031 423 © 2014 by Walter de Gruyter Berlin/Boston Crystal: orange-red blocks, size 0.163$0.305$0.5395 mm Wavelength: Mo K\" radiation (0.71073 Å) &: 98.83 cm Diffractometer, scan mode: Xcalibur, Eos, ) 2%max: 50.95° N(hkl)measured, N(hkl)unique: 4047, 1157 Criterion for Iobs, N(hkl)gt: Iobs > 2 #(Iobs), 1127 N(param)refined: 49 Programs: CrysalisPRO, SHELX, DIAMOND [1–3] Table 1. Data collection and handling.

Crystal structure of diaqua-(2,4-dihydroxybenzoato-κ2O,O')-(2,9- dimethyl-1,10-phenanthroline-κ2N,N') nickel(II) 2,4-dihydroxybenzoate, C28H26N2NiO10

Abstract: C28H26N2NiO10, monoclinic, P21/n (no. 14), a = 9.4921(9) Å, b = 24.194(2) Å, c = 11.526(1) Å, $ = 98.607(1)°, V = 2617.1 Å, Z = 4, Rgt(F) = 0.0308, wRref(F ) = 0.0822, T = 296 K.

Crystal structure of (E,E)-4-hydroxy-3-methoxybenzaldehyde azine – a second polymorph, C16H16N2O4

Abstract: C16H16N2O4, monoclinic, C2/c (no. 15), a = 21.0239(4) Å, b = 21.0149(4) Å, c = 14.8104(3) Å, $ = 107.607(1)°, V = 6236.9 Å, Z = 16, Rgt(F) = 0.0388, wRref(F ) = 0.1079, T = 200 K.

Crystal structure of N-dichloroacetyl-3-methyl-6,8-dichloro-3,4-dihydro- 2H-1,4-benzoxazine, C11H9Cl4NO2

Abstract: C11H9Cl4NO2, monoclinic, P21/c (no. 14), a = 11.995(2) Å, b = 11.831(2) Å, c = 9.798(2) Å, \" = 108.65(3)°, V = 1317.5 Å, Z = 4, Rgt(F) = 0.0374, wRref(F ) = 0.1050, T = 293 K.

Crystal structure of di(potassium 2-(2-ethoxy-2-oxoethoxy)-5-(7-(2-ethoxy- 2-oxoethoxy)-4-oxo-4H-chromen-3-yl)benzenesulfonate), C23H21KO11S

Abstract: C23H21KO11S, triclinic, P1 (no. 2), a = 8.907(5) Å, b = 15.814(8) Å, c = 18.114(9) Å, ( = 109.786(6)°, ' = 96.732(7)°, $ = 99.446(6)°, V = 2327 Å, Z = 4, Rgt(F) = 0.0517, wRref(F ) = 0.1579, T = 296 K.

Crystal structure of iron(II)-benzenedisulfonate-triaqua-bis(Nmethylpyrrolidone), Fe(BDS)(H2O)3(NMP)2, C16H28FeN2O11S2

Abstract: Abstract C16H28FeN2O11S2, monoclinic, Pc (no. 7), a = 14.6849(5) Å, b = 7.7856(2) Å, c = 20.1174(7) Å, β = 98.020(2)°, V = 2277.6 Å3, Z = 4, Rgt(F) = 0.0346, wRref(F2) = 0.0675, T = 120 K.