共查询到20条相似文献,搜索用时 15 毫秒
1.
Elena Bermejo Alfonso Castieiras Douglas X. West 《Journal of Molecular Structure》2003,650(1-3):93-97
Condensation of thiosemicarbazide or N(4)-ethylthiosemicarbazide with 1,2,8,9-tetraphenyl-3,7-diazanona-1,9-dione in the presence of copper(II) acetate in 96% ethanol leads to Δ6-5,6-diphenyl-5-methoxy-1,2,4-triazacyclohexene-3-thione, C16H15N3OS, or Δ6-4-methyl-5,6-diphenyl-5-ethoxy-1,2,4-triazacyclohexene-3-thione, C18H19N3OS. For C16H15N3OS the crystal data are monoclinic, P21/c, a=9.7780(7), b=8.5120(3), c=18.2210(13) Å, β=100.958(3)°, V=1488.89(16) Å3, and Z=4 in agreement with an earlier report. For C18H19N3OS the crystal data are orthorhombic, P212121, a=8.6940(3), b=12.9946(3), c=15.5139(5) Å, V=1752.68(9) Å3, and Z=4. 相似文献
2.
The structures of an isomeric pair: 1-[2-(2,6-dichlorophenoxy)-ethyl]-3-methylthio-5-amino-1H-1,2,4-triazole (IV) and 2-[2-(2,6-dichlorophenoxy)-ethyl]-3-methylthio-5-amino-2H-1,2,4-triazole (V) have been established by X-ray crystallography from diffractometer data. Crystals of IV are monoclinic, space group P21/c with a = 11.220(1), b = 10.005(3), c = 12.784(3) Å, β = 91.99(1)°, Z = 4, Dc = 1.478 g cm−3. Crystals of V are orthorhombic, space group Pbca with a = 7.618(2), b = 14.289(4), c = 26.494(7) Å, Z = 8, Dc = 1.470 g cm−3. The structures determined by direct methods were refined to R = 0.060 for 1931 reflections of IV and R = 0.061 for 1315 reflections of V. The X-ray analysis corroborated the structures assigned to the isomeric pair on the basis of proton coupled 13C-NMR spectra. The features (i.e. the sequence of the endocyclic bond angle magnitudes) of the planar s-triazole rings are governed by the same rules reported recently by Kálmán and Argay [J. Mol. Struct., 102 (1983) 391] discussing the structures of the related I, II and III compounds. In contrast to I, II, III and IV the S(6)---C(7) bond of V is almost perpendicular to the best plane of the s-triazole ring C(7)---S(6)---C(3)---N(4) = −79.0(7)°. This unusual orientation of the S-methyl bond is created by the steric hindrance of the very same vicinal 2-ethyl (C(9)H2---C(10)H2) moiety once within the molecule V and the second time as the part of a symmetry equivalent molecule at a distance of −a (7.618 Å). These molecules are fixed together by two infinite helices of hydrogen bonds formed around the screw axis 2, (X, 1/4, 1/2) via an intermediate V molecule at (x − 1/2, 1/2 − y, 1 − z). 相似文献
3.
Werner Kaminsky Diantha R. Kelman James M. Giesen Karen I. Goldberg Kacey A. Claborn Lisa F. Szczepura Douglas X. West 《Journal of Molecular Structure》2002,616(1-3):79-89
Structures of the following compounds have been obtained: N-(2-pyridyl)-N′-2-thiomethoxyphenylthiourea, PyTu2SMe, monoclinic, P21/c, a=11.905(3), b=4.7660(8), c=23,532(6) Å, β=95.993(8)°, V=1327.9(5) Å3 and Z=4; N-2-(3-picolyl)-N′-2-thiomethoxyphenyl-thiourea, 3PicTu2SeMe, monoclinic, C2/c, a=22.870(5), b=7.564(1), c=16.941(4) Å, β=98.300(6)°, V=2899.9(9) Å3 and Z=8; N-2-(4-picolyl)-N′-2-thiomethoxyphenylthiourea, 4PicTu2SMe, monoclinic P21/a, a=9.44(5), b=18.18(7), c=8.376(12) Å, β=91.62(5)°, V=1437(1) Å3 and Z=4; N-2-(5-picolyl)-N′-2-thiomethoxyphenylthiourea, 5PicTu2SMe, monoclinic, C2/c, a=21.807(2), b=7.5940(9), c=17.500(2) Å, β=93.267(6)°, V=2893.3(5) Å3 and Z=8; N-2-(6-picolyl)-N′-2-thiomethoxyphenylthiourea, 6PicTu2SMe, monoclinic, P21/c, a=8.499(4), b=7.819(2), c=22.291(8) Å, β=90.73(3)°, V=1481.2(9) Å3 and Z=4 and N-2-(4,6-lutidyl)-N′-2-thiomethoxyphenyl-thiourea, 4,6LutTu2SMe, monoclinic, P21/c, a=11.621(1), b=9.324(1), c=14.604(1) Å, β=96.378(4)°, V=1572.4(2) Å3 and Z=4. Comparisons with other N-2-pyridyl-N′-arylthioureas having substituents in the 2-position of the aryl ring are included. 相似文献
4.
Tristram Chivers Robert W. Hilts Masood Parvez
Dusan Ristic-Petrovic
Kenneth Hoffman 《Journal of organometallic chemistry》1994,480(1-2):c4-c6The reaction of Ru(CO)4(C2H4) or Ru(CO)5 with 1,5-Ph4P2N4S2 in CH2Cl2/hexane at 23°C produces the dimer [Ru(CO)2(Ph4 P2N4S2)]2 (2), which was shown by X-ray crystallography to have a centrosymmetric structure in which the P2N4S2 ring is attached to one ruthenium atom through two (geminal) nitrogen atoms and the remote sulfur atom and serves as a bridge to the other ruthenium atom via the second sulfur atom. Crystals of 2 ·2(CH2Cl2) are triclinic, space group P
(No. 2), a = 12.901(1) Å, b = 13.072(1) Å, c = 10.123(1) Å, = 100.88(1)°, β = 98.90(1)°, γ = 67.50(1)°, V = 1542.4(3) Å, Z = 1 with final R and Rw values of 0.040 and 0.027, respectively. 相似文献
5.
Reaction of the optically active primary amine (S)-(—)--methylbenzylamine with trimethylaluminium in heptane affords the crystalline organoaluminium dimer (S)-(—)-(S)-(—)-[(C6H5)CH(CH3)NHA1(CH3)2]2. Isolated as large, colourless, extremely air-sensitive prismatic crystals, the title compound crystallizes in the orthorhombic space group P212121 with unit cell parameters a = 8.406(3), b = 15.505(4), c = 17.547(5) Å, V = 2287 Å3 and p = 1.03 g cm−3 for Z = 4. Least-squares refinement based on 1477 observed reflections converged at R = 0.056, Rw = 0.058. Methane was eliminated during the course of the reaction due to cleavage of A1---C and N---H bonds resulting in an asymmetric A12N2 fragment at the core of the organoaluminium dimer. The mean A1---C bond distance in the dimethylaluminium units is 1.930(8), while the mean A1---N bond distance is 1.950(5) Å. Specific rotation ([]D25 in CH2C12)of the dimer is determined to be - 20.6°. 相似文献
6.
A number of isomeric N-benzylbenzalimine palladium(II) complexes of the type [P
·CH2Ph]2 (with C=N endo to the palladocycle) and [P
=C(CH3Ph]2 (with C=N exo to the palladocycle), have been prepared and charcterised by 1H and 13C NMR methods. The crystal structures of two analogous monomeric acac complexes, synthesized independently by oxidative addition of o-BrC6H4CH2N=CH · Ph to Ph to Pd(dibenzylideneacetone)2 have also been determined. These are [P
· CH2Ph)] (15a) and [P
=CHPh)] (20a). Crystals of 15a are monoclinic, space group P21/a with Z = 4 in a cell of dimensions a 10.286(2), b 11.902(3), c 13.895(5) Å, β 93.52(2)° while 20a is monoclinic, space group P21/c with Z = 8 and a 10.353(3), b 20.600(5), c 16.545(7) Å, β 92.14(3)°. The structures 15a and 20a were refined to residuals R = 0.041 and 0.055 for 1661 and 2525 observed reflections respectively. 相似文献
7.
《Journal of Molecular Structure》1997,416(1-3):209-220
The crystal structures of pharmaceutical product mesalazine (marketed also under different proprietary names as Salofalk, Asacol, Asacolitin, and Claversal) and its hydrochloride are reported. In the crystal mesalazine is in zwitterion form as 5-ammoniosalicylate (1) whereas mesalazine hydrochloride crystallizes in an ionized form as 5-ammoniosalicylium chloride (2). Compound 1 (C7H7O3N) crystallizes in the monoclinic space group P21/n with a = 3.769(1) Å, b = 7.353(2) Å, c = 23.475(5) Å, β = 94.38(2)°, V = 648.7(8) Å3, Z = 4, Dc = 1.568 g cm−3 and μ(MoK) = 1.2 cm−1. Compound 2 (C7H8O3NCl) crystallizes in the triclinic space group P
with a = 4.4839(2) Å, b = 5.7936(2) Å, c = 15.6819(5) Å, = 81.329(3)°, β = 88.026(3)°, γ = 79.317(4)°, V = 395.74(3) Å3, Z = 2, Dc = 1.591 g cm−3 and μ(CuK) = 40.8 cm−1. The crystal structures were solved by direct methods and refined to R = 0.041 for 1 and 0.028 for 2, using 607 and 1374 observed reflections, respectively. The configuration of both molecules, with the ortho hydroxyl to a carboxyl group, favours the intramolecular hydrogen bonds. Very complex systems of intermolecular hydrogen bonds were observed in both crystal packings. They are discussed in terms of graph-set notation. The mesalazine crystal structure is characterized by two-dimensional network of hydrogen bonds in the ab plane. The crystal structure pattern of mesalazine hydrochloride is a three-dimensional network significantly supported by N+---HCl− interactions. 相似文献
8.
J. M. Varela A. Mací as J. S. Casas J. Sordo 《Journal of organometallic chemistry》1993,450(1-2):41-45
The compounds [HgR(L)] (R = Me or Ph; L = 4-amino-5-mercapto-3-methyl-1,2,4-triazolate) have been prepared and the crystal structure of the methylmercury(II) compound determined. This compound crystallizes in the monoclinic space group P21/n with a = 5.087(1), b = 10.102(1), c = 16.167(2) Å, β = 98.56(1)°, Z = 4 (R = 0.027; Rw = 0.030). It is formed of molecules in which the triazolate anion is bound to mercury strongly via the S atom and weakly via the amine N; there is also a weak intermolecular interaction between the endocyclic N and the Hg atom of a neighbouring unit. 相似文献
9.
N-(2-hydroxyphenyl)-4-amino-3-penten-2-on (C11H13NO2) has been studied by X-ray analysis. It crystallizes the orthorhombic space group P212121 with a=8.834(1), b=10.508(2), c=11.212(2) Å, V=1040.8(3) Å3, Z=4, Dc=1.22 g cm−3 and μ(MoK)=0.084 mm−1. The structure was solved by direct methods and refined to R=0.038 for 1373 reflections (I>2σ(I)). The title compound is photochromic and the molecule is not planar. Intramolecular hydrogen bonds occur between the pairs of atoms N(1) and O(1) [2.631(2) Å], and N(1) and O(2) [2.641(2) Å], the H atom essentially being bonded to the N atom. There is also a strong intermolecular O–HO hydrogen bonding [2.647(2) Å] between neighbouring molecules. Tautomeric properties and conformations of the title compound were investigated by semi-empirical quantum mechanical AM1 calculations and the results are compared with the X-ray results. 相似文献
10.
James M. Boncella Shu-Yu S. Wang Daniel D. Vanderlende R. Leigh Huff Khalil A. Abboud William M. Vaughn 《Journal of organometallic chemistry》1997,530(1-2):59-70
The complex W(NPh)Cl2[o-(NSiMe3)2C6H4] 3 was synthesized from PhN = WCl4 · OEt2 and N,N′-(Li2[o-(NSiMe3)2C6H4] and reacts with Lewis bases to form the adducts W(NPh)Cl2[o-(NSiMe3)2C6H4](L) (L = PMe3, THF, 3-picoline, tBuNC, MeCN) 4a–e. Crystals of 4a are triclinic, space group P1¯, with a = 9.562(1), b = 10.277(1), c = 14.920(2) Å, = 82.15(1), β = 80.18(1), γ = 80.41(1)°, and Z = 2. The structure was solved by the heavy atom method and refined to R = 0.0408 for 4224 observed (I > 2σ(I)) reflections. The dialkyl complexes W(NPh)R2[o-(NSiMe3)2C6H4] (R = Me, Et, CH2Ph, CH2CMe3, CH2CMe2Ph) 5–9 are formed through subsequent reactions of 3 with the corresponding Grignard reagent. Crystals of complex 5 are monoclinic, space group P2(1)/n, with a = 10.3545(2), b = 17.9669(1), c = 13.3168(1) Å, β = 103.826(1)°, and Z = 4. The structure of complex 5 was solved by direct methods in SHELXTL5 and refined to R = 0.0247 for 4572 observed reflections. Compound 5 has a square pyramidal geometry in which the imido ligand occupies the apical position and reacts with PMe3 to form the adduct W(NPh)Me2[o-(NSiMe3)2C6H4](PMe3) 5a. Crystals of complex 5a are monoclinic, space group C2/m, with a = 13.5336(1), b = 14.4291(1), c = 15.3785(1) Å, β = 110.365(1)°, and Z = 4. The structure of compound 5a was solved by direct methods in shelxtl5 and refined to R = 0.0272 for 3057 observed reflections. Crystals of the bis-neopentyl complex 8 are monoclinic, space group P2(1)/n, with a = 10.6992(4), b = 18.3144(7), c = 16.0726(6) Å, β = 92.042(1)°, and Z = 4. The structure of 8 was solved by direct methods in shelxtl5 and refined to R = 0.0261 for 5881 observed reflections. Complex 8 has a trigonal bipyramidal geometry with both neopentyl groups and one amido nitrogen in the equatorial plane. 相似文献
11.
Microdifferential thermal analysis (μ-DTA), X-ray diffraction (XRD) and infrared (IR) spectroscopy were used for the first time to investigate the liquidus and solidus relations in the KPO3–Y(PO3)3 system. The only compound observed within the system was KY(PO3)4 melting incongruently at 1033 K. An eutectic appears at 13.5 mol% Y(PO3)3 at 935 K, the peritectic occurs at 1033 K and the phase transition for potassium polyphosphate KPO3 was observed at 725 K. Three monoclinic allotropic phases of the single crystals were obtained. KY(PO3)4 polyphosphate has the P21 space group with lattice parameters: a=7.183(4) Å, b=8.351(6) Å, c=7.983(3) Å, β=91.75(3)° and Z=2 is isostructural with KNd(PO3)4. The second allotropic form of KY(PO3)4 belongs to the P21/n space group with lattice parameters: a=10.835(3) Å, b=9.003(2) Å, c=10.314(1) Å, β=106.09(7)° and Z=4 and is isostructural with TlNd(PO3)4. The IR absorption spectra of the two forms show a chain polyphosphates structure. The last modification of KYP4O12 crystallizes in the C2/c space group with lattice parameters: a=7.825(3) Å, b=12.537(4) Å, c=10.584(2) Å, β=110.22(7)° and Z=4 is isostructural with RbNdP4O12 and contains cyclic anions. The methods of chemical preparations, the determination of crystallographic data and IR spectra for these compounds are reported. 相似文献
12.
Don Solooki John D. Bradshaw Claire A. Tessier Wiley J. YoungsRonald F. See Melvyn ChurchillJoseph D. Ferrara 《Journal of organometallic chemistry》1994,470(1-2):231-236
1,2:5,6:9,10:13,14-Tetrabenzo-3,7,11,15-tetradehydro[16]annulene, or tetrabenzocyclyne (QBC) and 1,2:5,6:9,10:13,14:17,18:21,22-hexabenzo-3,7,11,15,19,23-hexadehydro[24]annulene (HBC) have been structurally characterized by X-ray. crystallography. QBC crystallizes in two different space groups; P21/c with a = 10.652(3) Å, b = 10.624(2) Å, c = 19.549(4) Å, β = 93.83(2)°, V = 2207.4(8) Å3, and Z = 4 and P41212 with a = 9.330(1) Å, c = 25.497(8) Å, V = 2219.6(12) Å, and Z = 4. HBC crystallizes in monoclinic P21/n with a = 14.763(3) Å, b = 10.296(2) Å, c = 22.057(4) Å, β = 108.61(3), V = 3177.4(11) Å3, T = 133 K, and Z = 4. Reaction of QBC with dicobaltoctacarbonyl has produced a tetracobalt complex which has been characterized by X-ray crystallography. This complex crystallizes in monoclinic P21/c with a = 14.699(3) Å, b = 17.188(3) Å, c = 17.254(3) Å, β = 112.63(3)°, V = 4023.5(13) Å3, and Z = 4. Only two of the four C---C triple bonds of QBC bind to dicobalthexacarbonyl moieties even when excess dicobaltoctacarbonyl is used. 相似文献
13.
Da-Ming Du Wen-Ting Hua Ling-Ping Zhou Jian-Wu Wang Xiang-Lin Jin 《Journal of Molecular Structure》2001,560(1-3):23-28
The new host 1,4,11,14-tetramethoxy-dibenzo[b,n]tetraphenylene forms a 1:1 inclusion compound with pyridine, in which a pair of centrosymmetrically-related guest species are enclosed in the cage surrounded by six host molecules. C36H28O4·C5H5N, FW=603.68, triclinic, space group P-1, a=11.796(2), b=16.075(3), c=9.004(2) Å; =98.39(3)°, β=90.01(3)°, γ=108.19(3)°, V=1602.8(5) Å3, Z=2, F(000)=636, Dc=1.251 g/cm3, μ=0.080 mm−1. The final R indices [I>2σ(I)] R1=0.0759, wR2=0.1970 for 5623 MoK observed data. 相似文献
14.
Darryl P. Klein N. Quir s M ndez Jeffery W. Seyler Atta M. Arif J. A. Gladysz 《Journal of organometallic chemistry》1993,450(1-2):157-164
The crystal structures of propionaldehyde complex (RS,SR)-(η5-C5H5)Re(NO)(PPh3)(η2-O=CHCH2CH3)]+ PF6− (1b+ PF6s−; monoclinic, P21/c (No. 14), a = 10.166 (1) Å, b = 18.316(1) Å, c = 14.872(2) Å, β = 100.51(1)°, Z = 4) and butyraldehyde complex (RS,SR)-[(η5-C5H5)Re(NO)(PPh3)(η2-O=CHCH2CH2CH3)]+ PF6− (1c+PF6−; monoclinic, P21/a (No. 14), a = 14.851(1) Å, b = 18.623(3) Å, c = 10.026(2) Å, β = 102.95(1)°, Z = 4) have been determined at 22°C and −125°C, respectively. These exhibit C
O bond lengths (1.35(1), 1.338(5) Å) that are intermediate between those of propionaldehyde (1.209(4) Å) and 1-propanol (1.41 Å). Other geometric features are analyzed. Reaction of [(η5-C5H5)Re(NO)(PPh3)(ClCH2Cl)]+ BF4− and pivalaldehyde gives [(η5-C5H5)Re(NO)(PPh3)(η2-O=CHC(CH3)3)]+BF4− (81%), the spectroscopic properties of which establish a π C
O binding mode. 相似文献
15.
Jos Elguero Enrique Gutierrez-Puebla Angeles Monge Carmen Parco Mar Ramos 《Tetrahedron》1993,49(48):11305-11320
Reaction of N-vinylindazolium tetrafluoroborates with aqueous potassium carbonate or sodium borohydride affords 2,3-dihydroquinazolines which evolve to 1,2,3,4-tetrahydroquinazolines by intra or intermolecular nucleophilic attack. The X-ray structure of one tetrahydroquinazoline, the tricyclic compound 17a, was determined (C14H16N2O5, P21/n, a=6.001(4)Å, b=13.601(8)Å, c=17.452(6)Å, β=94.93(3)°, V=1419(1)Å3, Z=4, R=0.078 for 1541 observed reflexions). Only open-chain compounds are obtained when these salts react with methanol. 2-Vinylindazolium and 3-vinylbenzotriazolium tetrafluoroborates react with aqueous potassium carbonate and with sodium borohydride yielding the corresponding neutral benzazoles by cleavage of the azole-vinyl bond. They add methanol to the exocyclic double bond and, in the case of indazole derivative, an expansion to a 1,2-dihydroquinazoline is observed in basic medium.A general mechanism is proposed for the reaction of vinylpyrazolium and indazolium salts with nucleophiles. 相似文献
16.
William J. Evans Roy A. Keyer Joseph W. Ziller 《Journal of organometallic chemistry》1993,450(1-2):115-120
The effects of cyclopentadienyl ring size on the geometry of bimetallic organosamarium complexes have been studied by comparing the X-ray crystal structure of [(C5H4Me)2(THF)Sm(μ-Cl)]2, prepared from KC5H4Me and SmCl3 in THF, with C5Me5 analogs. The complex crystallizes from THF at −30°C in space group Pbcn with a = 20.312(5), b = 9.626(2), c = 16.225(3) Å, V = 3172.5(12) Å3 and Dcalc = 1.74 g cm−3 for Z = 4. Least-squares refinement of the model based on 1759 reflections [|Fo| > 2.0σ(|Fo|)] converged to a final RF = 5.0%. The complex adopts a geometry which has a molecular two-fold rotation axis perpendicular to the Sm2Cl2 plane and a crystallographic inversion center. Hence, both methyl groups of each (C5H4Me)2Sm unit are located on the side opposite of the THF ligands, which are trans to each other, and the four C5H4Me ring centroids define a square plane. The Sm---Cl distances are 2.759(3) and 2.819(3) Å. 相似文献
17.
M. N. Bochkarev I. L. Fedushkin
H. Schumann
J. Loebel 《Journal of organometallic chemistry》1991,410(3):321-326Naphthaleneytterbium, C10H8Yb(THF)3, reacts with Cp2Cr, Cp2Co, Cp2Ni, and Cp2V in THF to give Cp2Yb. In the case of the reaction of C10H8Yb(THF)3 with Cp2V, vanadium-containing intermediates could be isolated. One of them, CpVC10H8VCp, has been characterized by X-ray diffraction. The crystals are monoclinic, space group P21/n, with a 907.0(5), b 798.8(3), c 1080.8(5) pm, β 105.21(4)°; Z = 2. The structure was refined to R = 0.0288 for 1131 observed reflections (Fo > 4σ(Fo)). 相似文献
18.
X-ray studies indicate that indanone-1 crystals belong to a monoclinic system, space group P21/c (C52h), with the following parameters: a = 7.90±0.01 Å; b = 12.38±0.01 Å; c = 7.39±0.01 Å; β = 99°±30' and Z = 4. A vibrational assignment of fundamental bands observed in the polarized infrared spectrum between 4000 cm−1 and 250 cm−1 is proposed. The band fine structure analysis at 77 °K shows a doublet structure, which agrees with X-ray data. 相似文献
19.
A series of new 2D-layered structural rare-earth coordination polymers with the general formal [Ln(C8H4O5)(H2O)5]·(H2O)·(C8H4O5)1/2 (Ln=Eu for (1); Gd for (2); Tb for (3); Dy for (4); and Er for (5)) have been yielded by hydrothermal synthesis. The coordination polymers crystallize in monoclinic space group C/2c with a=19.838(16), b=10.529(8), c=17.752(14) Å, β=107.503(14)° for (1), with a=19.823(7), b=10.552(4), c=17.762(6) Å, β=107.443(6)° for (2), with a=19.770(4), b=10.519(2), c=17.698(4) Å, β=107.52(3)° for (3), with a=19.632(2), b=10.492(2), c=17.617(3) Å, β=107.470(12)° for (4), with a=19.648(7), b=10.480(3), c=17.598(6) Å, β=107.502(6)° for (5), respectively. And the metal ions (Ln3+) are located in nine-member coordination environment. The carboxyl groups from 5-hydroxyisophthalate chelate the metal ions to form 1D helical cation chains. It is interesting that these helical cation chains are arranged to form 2D anion–cation layers by the uncoordinated ligands' anions as template. And the luminescence properties of the rare-earth ions are studied in the paper. 相似文献
20.
Barbara A. Fir Hlne P. A. Mercier Jeremy C. P. Sanders David A. Dixon Gary J. Schrobilgen 《Journal of fluorine chemistry》2001,110(2):89-107
The XeOSeF5+ cation has been synthesized for the first time and characterized in solution by 19F, 77Se and 129Xe NMR spectroscopy and in the solid state by X-ray crystallography and Raman spectroscopy with AsF6− as its counter anion. The X-ray crystal structures of the tellurium analogue and of the Xe(OChF5)2 derivatives have also been determined: [XeOChF5][AsF6] crystallize in tetragonal systems, P4/n, a=6.1356(1) Å, c=13.8232(2) Å, V=520.383(14) Å3, Z=2 and R1=0.0453 at −60°C (Te) and a=6.1195(7) Å, c=13.0315(2) Å, V=488.01(8) Å3, Z=2 and R1=0.0730 at −113°C (Se); Xe(OTeF5)2 crystallizes in a monoclinic system, P21/c, a=10.289(2) Å, b=9.605(2) Å, c=10.478(2) Å, β=106.599(4)°, V=992.3(3) Å3, Z=4 and R1=0.0680 at −127°C; Xe(OSeF5)2 crystallizes in a triclinic system,
, a=8.3859(6) Å, c=12.0355(13) Å, V=732.98(11) Å3, Z=3 and R1=0.0504 at −45°C. The energy minimized geometries and vibrational frequencies of the XeOChF5+ cations and Xe(OChF5)2 were calculated using density functional theory, allowing for definitive assignments of their experimental vibrational spectra. 相似文献