Air stable liquid clathrates: Solid state structure and hydrocarbon solubility of organic cation triiodide salts

A series of air and water stable organic cation triiodide salts have been prepared and characterized. Almost all of the salts isolated sustain liquid clathrate phases in the presence of benzene or toluene, the compositions of which were determined via¹H NMR spectroscopy. Two of the salts were also characterized via X-ray crystallography in order to determine the nature of any solid state interionic interactions (1-ethylpyridinium triiodide, monoclinic,P2₁/c,a = 9.6031(7),b = 15.129(3),c = 8.8160(16) Å, = 104.192(11)°,Z = 4,R = 0.041 for 2463 independent observed reflections; 1,2,4-trimethylpyridinium triiodide, orthorhombic,Pbcm,a = 9.434(4), 20.176(4), 7.411(4) Å,Z = 4,R = 0.045 for 966 observed reflections).     

Tetracarbonyliron adducts of Cp2Cr2(CO)4(μ-η2-P2). Syntheses and crystal structures of Cp2Cr2(CO)4P2[Fe(CO)4] m (m=1 and 2)

Cp₂Cr₂(CO)₄( - ² - P₂), 1, reacts with one molar equivalent of Fe₂(CO)₉ in THF to yield the mono- and di-iron complexes, Cp₂Cr₂(CO)₄P₂[Fe(CO)₄], 2, (16.5% yield) and Cp₂Cr₂(CO)₄P₂[Fe(CO)₄]₂, 3, (16.9% yield), as dark magenta brown and dark greenish brown crystals, respectively. Both complexes were characterized by single-crystal X-ray diffraction analysis. Crystal data –2: space group =P2₁/c,a=17.024(1) Å,b=8.180(1) Å,c=30.891(2) Å, =100.953(5)°,V=4223.4(7)ų,Z=8, 3743 observed reflections,R _F=0.033; 3: space group P1,a=10.209(2) Å,b=10.212(2) Å,c=15.989(3) Å, =106.93(1)°, =91.87(1)°, =119.50(1)°,V=1356.5(4) ų,Z=2, 3489 observed reflections,R _F=0.029.     

The crystal and molecular structures of aqua(1,4,7,10,13-pentaazacyclopentadecane)nickel(II) nitrate perchlorate [Ni[15]aneN5·H H2O](NO3)(ClO4) and (1,5,9,13,17-pentaazacycloeicosane)-nikel(II) nitrate hydrate [Ni[20]aneN5](NO3)2·H2O

Summary The structures of Ni^II complexes of the macrocyclic ligands 1,4,7,10,13-pentaazacyclopentadecane, [15]aneN₅ and 1,5,9,13,17-pentaazacycloeicosane, [20]aneN₅ have been determined. [Ni(C₁₀H₂₅N₅)H₂O]-(NO₃)(ClO₄) monoclinic, space group P2₁/n,a=8.265(3)Å,b=6.201(6)Å,c=13.672(4)Å, =93.35(3)°· 2394 unique reflections were used in the structure determination and the refinement proceeded to an R value of 0.045. The ligand is coordinated to the metalvia all five nitrogens in theracemic conformation and a water molecule completes the coordination sphere of the metal ion. The complex cation shows considerable distortion from octahedral geometry which may rationalise the unusual spectroscopic properties and the low enthalpy of formation of the complex cation. [Ni(C₁₅H₃₅N₅)](NO₃)₂·H₂O monoclinic, space group P2₁/n,a=15.437(9)Å,b=9.573(6)Å,c=15.942(8)Å, =109.24(4)°. 2715 unique observed reflections were used in the structure refinement which proceeded to an R value of 0.035. The five nitrogens of the macrocycle are bound to Ni(II) in a distorted square pyramidal coordination geometry. The Ni^II lies 0.35Å above the basal plane of the four nitrogen atoms.     

X-ray Diffraction Structural Study of Acid Pyridinium Hexamolybdochromate(III)

Acid pyridinium hexamolybdochromate(III) (₅₅NH)H₂[CrMo₆O₁₈(OH)₆] · 6H₂O was synthesized and structurally characterized. The crystals are monoclinic, space group P2₁/c, a = 11.400(2) Å, b = 11.165(2) Å, c = 11.665(2) Å, = 104.39(3)°, Z = 2, _calcd = 2.789 g/cm³.     

Ethylenediamine-N,N"-Diacetate Ion (Edda2–) as a Tridentate Ligand: Synthesis and Structure of the [Co(Edda)(Dien)]ClO4 · H2O and [Co(Edda)(En)(CN)] · 2H2O Complexes

The cobalt(III) complexes with tridentate ethylenediamine-N,N"-diacetate ions (Edda^2–) and additional ligands, namely, diethylenetriamine (Dien) or ethylenediamine (En) and cyanide ions, were synthesized. As follows from X-ray diffraction analysis of [Co(Edda)(Dien)]ClO₄· H₂O (monoclinic crystals with a = 9.243 (2) Å, b = 14.167 (4) Å, c = 13.046 (3) Å, = 91.19 (2)°, Z = 4, space group P2₁/c), the secondary N atom of the Dien ligand occupies the trans-position relative to the N atom of the Edda^2– ligand, which contains a free acetate group. Two fac-isomers of [Co(Edda)(En)(CN)] with the CN^– ion in the cis- and trans-positions relative to the oxygen atom of the carboxyl group were isolated, and the structure of the trans-(O,CN)-[Co(Edda)(En)(CN)]· 2H₂O was determined: monoclinic crystals with a = 9.136 (3) Å, b = 15.484 (3) Å, c = 10.564 (3) Å, = 110.67 (5)°, Z = 4, space group P2₁/c.     

Crystal Structure Refinement for Potassium(2.2.2-cryptand)thiocyanate Monohydrate

The crystal structure of potassium(2.2.2-cryptand)thiocyanate monohydrate, [K⁺(2.2.2-Crypt)]·SCN^- ·H₂O, has been refined by XRD analysis: space group P2/c, a=11.290(2), b=8.308(2), c=14.360(2) , =109.97(2)°, Z=2; 3680 unique reflections, R=0.051. Using a different structural model with a twice shorter crystallographic a axis compared to the original work gave much more precise structural data.     

Complexation with diol host compounds. Part 1. Structures of the 1:2 molecular complexes oftrans-9, 10-dihydroxy-9,10-diphenyl-9,10-dihydroanthracene with acetophenone and with 3-methylcyclopentanone

The structures of the 1:2 molecular complexes of trans -9,10-dihydroxy-9,10-diphenyl-9,10-dihydroanthracene with acetophenone (1), (C₂₆H₂₀O₂·2 C₈H₈O) and with 3-methylcyclopentanone (2), (C₂₆H₂₀O₂·2C₆H₁₀O) have been determined by X-ray crystallography. The crystal data are as follows: Compound (1):P ,a =8.979(5) Å,b =9.316(3) Å,c = 11.12(1) Å, =94.40(6)°, = 106.53(6)°, = 109.92(5)°,V = 822.94 ų,Z = 1,R = 0.097 for 2549 unique reflections. Compound (2):P ,a = 8.958(7) Å,b =9.815(4) Å,c = 9.807(4) Å, = 96.88(3)°, = 109.21(8)°, = 103.33(7)°,V = 774.10 ų,Z = 1,R = 0.059 for 2494 unique reflections. The intermolecular arrangements in both structures are characterised by host-to-guest hydrogen bonding interactions. The thermal properties of compound (2) have been characterised by DTA and TGA thermograms.     

Ferrocene Compounds. XXVII. Synthesis and Structure of 2-(Ferrocenylmethyl)propane-1,3-diol

The title compound was obtained by reduction of diethyl (ferrocenylmethyl)malonate with lithium aluminium hydride in diethyl ether. The structure of this novel ferrocene derivative was assigned by means of elemental analysis, IR, [¹H]NMR, and [¹³C]NMR spectroscopy. The structure was also confirmed by a single crystal X-ray study. The compound crystallizes in monoclinic P2₁/a space group with unit cell dimensions: a = 9.7360(6), b = 27.040(5), c = 14.767(3) Å, = 103.835(6)°, V = 3774.8(11) ų, Z = 12. The asymmetric unit contains three crystallographically independent molecules. In the ferrocenyl moieties, the Fe–C bond distance values are in the range 2.006(5)—2.051(3) Å and C–C distances in the range 1.366(7)–1.425(4) Å. The cyclopentadienyl rings in each of the molecules are mutually twisted by about 13° from the eclipsed conformation. The hydroxyl groups are involved in the intermolecular O–H...O hydrogen bond formation with O-O distances in the range 2.686(3)–2.801(4) Å forming infinite two-dimensional network in a [0 0 1] plane. The crystal structure is additionally stabilized by C–H-O weak intermolecular hydrogen bonds.     

Preparation and x-ray structure determination of penta-and tetracyano-oxomolybdenum(IV) anions. The influence of water on their reactivity

Summary Several penta-and tetracyanooxomolybdenum(IV) anions have been synthesized containing different numbers of H₂O molecules, either coordinated or present as crystallisation molecules. The influence of these molecules on the reactivity of the complex, especially towards O₂, is discussed. Three compounds were characterized by x-ray structure determination. [Mo(O)(CN)₅(H₂O)₂(MeCN)₂][PPh₄]₄Cl belongs to triclinic space group P-1 witha=13.146(3) Å,b=16.944(5) Å,c=21.761(6) Å, =84.72(2)°, =87.15(2)° and =85.25(2)°. The volume of the unit cell is 4678(6)ų withz=2. The structure was refined to R=6.5%. [Mo(O)(CN)₄(H₂O)·6H₂O][PPh₄]₂ belongs to monoclinic space group P2₁/n witha=15.313(2)Å,b=19.983(3)Å,c=17.006(2)Å, =100.51(2)°. The volume of the unit cell is 5117(3)ų withz=4. The structure was refined to R=8.7%. [Mo(O)(CN)₄(MeCN)](PH₃)₂N]₂ belongs to triclinic space group P-1 witha=13.770(4)Å,b=16.292(5)Å,c=16.889(5)Å, =73.23(2)°, =72.02(2)° and =71.57(2)°. The volume of the unit cell is 3342(3)ų withz=2. The structure was refined to R=7.2%.     

Inclusion complexes of the natural product gossypol. Clathrate type inclusion complexes of gossypol with carbonyl group containing guests

The crystal structures of 2:1 inclusion complexes of gossypol with methyl propionate (GPMEP) and ethyl acetoacetate (GPEAA) have been determined by X-ray structure analysis. The crystals of GPMEP, C₃₀H₃₀O₈l/2 C₄H₈O₂, are monoclinic, space groupC2/c,a=11.079(3),b = 30.724(7), c = 16.515(5) Å, = 90.46(2)°,V = 5621(3) Å,Z = 8,D _x = 1.33 g cm^–3. The structure has been refined to the finalR value of 0.059 for 1899 observed reflections. The crystals of GPEAA, C₃₀H₃₀O₈l/2 C₆H₁₀O₃, are monoclinic, space groupC2/c,a=11.095(2),b=30.604(9),c = 16.955(5) Å, = 88.27(2)°,V = 5754(3) Å,Z = 8,D _x = 1.35 g cm^–3. The structure has been refined to the finalR value of 0.056 for 2502 observed reflections.In contrast to previously investigated inclusion complexes of gossypol the host molecules do not form centrosymmetric dimersvia hydrogen bonds. In the crystal structures the racemic gossypol is separated into enantiomers forming alternating bimolecular layers. Nearly perpendicular to these chiral bilayers run elongated cavities enclosed on each side by layers of opposite chirality. The surface of these layers is hydrophobic, the polar groups are hidden inside the layer. Guest molecules which are hydrogen bonded to the host are included in cylindrically shaped cavities. Possible hydrogen bonds between host and guest are analysed for this isostructural class of complexes.     

Alternative methods of modifying the calixarene conformation. The synthesis and molecular structures oft-butylcalix[4]arene methyl ether complexed with aluminum alkyl species

The configurations of calix[4]arenes may be modified by the formation of donor-acceptor complexes which make use of the basicity of the oxygen atoms of the macrocycle. The complex [t-butylcalix[4]arene methyl ether][AlMe₃]₂,2, exhibits the previously unseen 1,2-alternate geometry, while [t-butylcalix[4]arene methyl ether][MeAlCl₂]₂,3, and [t-butylcalix[4]arene methyl ether][EtAlCl₂]₂,4, show the 1,3-alternate configuration.2 crystallizes in the triclinic space groupPl witha=11.14(1),b=11.60(1),c=12.02(1) Å, =77.32(8), =67.91(8), and =69.34(8)^o withD _c =1.06 g cm^–3 forZ=1. Refinement based on 1270 observed reflections led toR=0.106.3 as the benzene solvate belongs to the monoclinic space groupC2/c witha=12.116(2),b=21.557(7),c=23.470(6) Å, and =104.05(2)^o withD _c =1.13 g cm^–3 forZ=4. Refinement based on 2335 observed reflections led toR=0.075.4 crystallizes in the monoclinic space groupC2/c witha=12.062(4),b=21.175(6),c=21.596(5) Å, and =100.78(4)^o withD _c =1.18 g cm^–3 forZ=4. Refinement based on 2529 observed reflections gaveR=0.082. The Al-O lengths in all three complexes are normal for donor-acceptor interactions. Supplementary Data relating to this article are deposited with the British Library as Supplementary Publication No. SUP 82053 (45 pages).     

New uranyl complex with imidazolidine-2-one [UO<Subscript>2</Subscript>(Imon)<Subscript>4</Subscript>(H<Subscript>2</Subscript>O)](ClO<Subscript>4</Subscript>)<Subscript>2</Subscript>: Structure and some properties

A complex of uranyl perchlorate with imidazolidine-2-one as the molecular ligand, [UO₂(Imon)₄(H₂O)](ClO₄)₂ (I), was synthesized and structurally characterized by X-ray diffraction analysis. The coordination number of the uranium atom is 7. The nearest environment of the uranyl ion includes four O atoms of the imidazolidine-2-one molecules and one O atom of the water molecule. The perchlorate anions are outer-sphere ligands. The crystals are monoclinic: space group P2₁/c; a = 16.294(3) Å, b = 16.135(3) Å, c = 9.987(2) Å, = 97.69 (3)°, V = 2603.0 (9) ų, (calcd) = 2.117 g/cm³, Z = 4. The IR and luminescence spectra of the complex were recorded.Translated from Koordinatsionnaya Khimiya, Vol. 30, No. 12, 2004, pp. 919–924.Original Russian Text Copyright © 2004 by Andreev, Antipin, Budantseva, Tuchina, Serezhkina, Fedoseev, Yusov.     

Acetylene as a ligand on clusters: An accurate determination of the crystal and molecular structure of (Cp)2Ni2Fe(CO)3(μ3−C2H2) and of (CP)2Ni2Fe2(CO)6(μ4−C2H2)

Abstarct The Cp)₂Ni₂Fe(CO)₃(µ₃-C₂H₂) and Cp)₂Ni₂Fe(CO)₃(µ₃-C₂H₂) (B) complexes have been synthesized and spectroscopically characterized. An accurate X-ray study and a comparison with related structures shows that the substituents of the alkyne ligands exert considerable effects on the bonding parameters.Crystal data for complex A, monoclinic space group P2₁/n,a = 8.418(1),b = 15.779(2),c = 14,493(1) Å, = 91.64(1)°,Z = 4, 2753 observed reflections,R = 0.022; crystal data for complex B, monoclinic space group C2/c,a = 16.2189(7),b = 7.445(3),c = 25.745(5) Å, = 103.74(3),Z=8, 1853 observed reflections,R = 0.051.     

The preparation,crystal and molecular structure of [MoCl2(NH)O(EtPh2PO)2] the preparation,crystal and molecular structure of [MoCl2(NH)O(EtPh2PO)2]. An example of terminal,nonlinear-imido-coordination

Summary Reaction of MoOCl₃ with Me₃SiN₃ m THF followed by addition of tertiary phosphine oxides, RPO₃(R₃=Ph₃, Ph₂Et, Ph₂Me), gives [MoCl₂(NH)O(OPR₃)₂]. The crystal and molecular structure of the compound has been determined by x-ray diffraction methods. The complex crystallises in the monoclinic space group P2₁ /a with four molecules in a unit cell having dimensions a=15.667(8) Å, b=20.135(9) Å, c=9.726(7) Å and =95.01(1) Å. A total of 3510 reflections were collected by counter techniques using MoK radiation. The structure was refined on 2597 reflections with I > 2.58 (I) by full matrix least squares, using anisotropic temperature factors for all nonhydrogen atoms, to give a final R factor of 0.082. The overall configuration of the distorted octahedral complex istrans-dichloro-cis-bis[ethyl(diphenyl)phosphineoxide]cis-(oxo) imido with the molybdenum formally in the oxidation state (VI). The imido hydrogen has been located, and the Mo-N-H system is nonlinear.     

Antimony(III) Oxofluorides α-Sb3O2F5 and β-Sb3O2F5: Synthesis and Crystal Structures

The conditions for the synthesis of two polymorphous forms of antimony(III) oxofluoride Sb₃O₂F₅ from aqueous solutions are established. The crystal structure of a new polymorphous modification -Sb₃O₂F₅ is determined (monoclinic crystals with a = 6.9548(6) Å, b = 9.1043(7) Å, c = 20.336(2) Å, = 94.167(2)°, V = 1284.2(2) ų, Z = 8, (calcd) = 5.092 g/cm³, F(000) = 1712, space group P2₁/n) and the structure of -Sb₃O₂F₅ is refined. The geometric characteristics of crystal structures of antimony(III) oxofluorides SbOF (L- and -forms) are compared with those of Sb₃O₂F₅ (- and -forms).     

On the crystal chemistry of three copper(II)-arsenates: Cu3(AsO4)2-III,Na4Cu(AsO4)2, and KCu4(AsO4)3

The three copper(II)-arsenates were synthesized under hydrothermal conditions; their crystal structures were determined by single-crystal X-ray diffraction methods:Cu₃(AsO₄)₂-III:a=5.046(2) Å,b=5.417(2) Å,c=6.354(2) Å, =70.61(2)°, =86.52(2)°, =68.43(2)°,Z=1, space group ,R=0.035 for 1674 reflections with sin / 0.90 Å^–1.Na₄Cu(AsO₄)₂:a=4.882(2) Å,b=5.870(2) Å,c=6.958(3) Å, =98.51(2)°, =90.76(2)°, =105.97(2)°,Z=1, space group ,R=0.028 for 2157 reflections with sin / 0.90 Å^–1.KCu₄(AsO₄)₃:a=12.234(5) Å,b=12.438(5) Å,c=7.307(3) Å, =118.17(2)°,Z=4, space group C2/c,R=0.029 for 1896 reflections with sin / 0.80 Å^–1.Within these three compounds the Cu atoms are square planar [4], tetragonal pyramidal [4+1], and tetragonal bipyramidal [4+2] coordinated by O atoms; an exception is the Cu(2)^[4+1] atom in Cu₃(AsO₄)₂-III: the coordination polyhedron is a representative for the transition from a tetragonal pyramid towards a trigonal bipyramid. In KCu₄(AsO₄)₃ the Cu(1)^[4]O₄ square and the As(1)O₄ tetrahedron share a common O—O edge of 2.428(5) Å, resulting in distortions of both the CuO₄ square and the AsO₄ tetrahedron. The two Na atoms in Na₄Cu(AsO₄)₂ are [6] coordinated, the K atom in KCu₄(AsO₄)₃ is [8] coordinated by O atoms.Die drei Kupfer(II)-Arsenate wurden unter Hydrothermalbedingungen gezüchtet und ihre Kristallstrukturen mittels Einkristall-Röntgenbeugungsmethoden ermittelt:Cu₃(AsO₄)₂-III:a = 5.046(2) Å,b = 5.417(2) Å,c = 6.354(2) Å, = 70.61 (2)°, = 86.52(2)°, = 68.43(2)°,Z = 1, Raumgruppe ,R = 0.035 für 1674 Reflexe mit sin / 0.90 Å^–1.Na₄Cu(AsO₄)₂:a = 4.882(2) Å,b = 5.870(2) Å,c = 6.958(3) Å, = 98.51(2)°, = 90.76(2)°, = 105.97(2)°,Z = 1, Raumgruppe ,R = 0.028 für 2157 Reflexe mit sin / 0.90 Å^–1.KCu₄(AsO₄)₃:a = 12.234(5) Å,b = 12.438(5) Å,c = 7.307(3) Å, = 118.17(2)°,Z = 4, Raumgruppe C2/c,R = 0.029 für 1896 Reflexe mit sin / 0.80 Å^–1.Die Cu-Atome in diesen drei Verbindungen sind durch O-Atome quadratisch planar [4], tetragonal pyramidal [4 + 1] und tetragonal dipyramidal [4 + 2]-koordiniert; eine Ausnahme ist das Cu(2)^{[4 + 1]}-Atom in Cu₃(AsO₄)₂-III: Das Koordinationspolyeder stellt einen Vertreter des Übergangs von einer tetragonalen Pyramide zu einer trigonalen Dipyramide dar. In KCu₄(AsO₄)₃ haben das Cu(1)^[4]O₄-Quadrat und das As(1)O₄-Tetraeder eine gemeinsame O—O-Kante von 2.428(5) Å, was eine Verzerrung der beiden Koordinationsfiguren CuO₄-Quadrat und AsO₄-Tetraeder bedingt. Die zwei Na-Atome in Na₄Cu(AsO₄)₃ sind durch O-Atome [6]-koordiniert, das K-Atom in KCu₄(AsO₄)₃ ist [8]-koordiniert.

---

Zur Kristallchemie dreier Kupfer (II)-Arsenate: Cu₃(AsO₄)₂-III, Na₄Cu(AsO₄)₂ und KCu₄(AsO₄)₃

     

Organically Templated Vanadium Oxide Phases: Synthesis and Structures of [H3NCH2CH2NH3][V2O6] and [HN(CH2CH2)3NH][VV2VIV4O14]·H2O

The synthesis and crystal structures of [H₃NCH₂CH₂NH₃][V₂O₆] (1) and [HN(CH₂CH₂)₃NH][V^V ₂V^IV ₄O₁₄]·H₂O (2) are described. The structure of the oxidized compound 1 consists of parallel stacks of vanadium oxide chains of corner sharing {VO₄} tetrahedra. The chains are stabilized by extensive hydrogen bonding involving oxide ligands of the chains and ethylenediammonium ions which fill the space between the stacks of chains. The structure of compound 2 consists of vanadium oxide layers separated by doubly protonated 1,4-diazabicyclo[2.2.2]octane and lattice water. The vanadium oxide layers, containing mixed-valence vanadium (V^V and V^IV) centers, are composed of zigzag ribbons of edge-sharing {VO₅} square pyramids interconnected by {VO₄} tetrahedra. Crystal data. C₂H₁₀N₂O₆V₂ , 1: monoclinic, space group P2₁/c (No. 14), a=5.5359(5), b=12.9430(12), c=5.6856(5) Å, =90, =97.460(2), =90°, V=403.93(6) ų, Z=2. A total of 2506 reflections ( _max=27.89°) was collected, of which 954 were used to resolve the structure. The structure was solved by direct methods and least-squares refinement converged at R=0.0592. C₆H₁₆N₂O₁₅V₆, 2: monoclinic, space group C2 (No. 5), a=19.303(4), b=6.667(2), c=7.579(2) Å, =90, =111.31(2), =90°, V=908.4(4) ų, Z=2. A total of 1779 reflections was collected, of which 1591 unique reflections were used for structural elucidation. The structure was solved by direct methods and least-squares refinement converged at R=0.0314.     

The x-ray crystal structure,resolution and absolute configuration of thecis-α-dichloro(1, 8-diamino-3, 6-diazaoctane)-ruthenium(III) cation

Summary Acis- configuration for the [RuCl₂(trien)]Cl·2H₂O (trien=1, 8-diamino-3, 6-diazaoctane) complex has been confirmed by an x-ray crystal structure determination. Crystals are monoclinic, space group P2₁/c witha=7.336 (1),b=8.477 (2),c=23.181 (4) Å, =103.3 (1)°, U=1403 (1) Å.³ Z=4 and M=389.7, D_c=1.84 g cm^–3. The structure was refined by full matrix least squares methods to final residual values of R=0.025 and R_w=0.033 on the basis of 3882 unique reflections. The complex has been resolved into its optical isomers using the (+)1, 2-diaminoethanebis(oxalato)cobaltate(III) anion and the absolute configuration assigned.     

Novel cage-like cavity accommodating a pair of guest molecules in the structure ofcatena-[dl-1,2-diaminopropanecadmium(II) tetra-μ-cyanocadmate(II)]-(1,2-dichloroethane)(1/1)

The title clathrate Cd(dl-pn)Cd(CN)₄·CH₂CICH₂CI (pn=dl-1,2-diaminopropane=dl-propy-lenediamine) crystallizes in the monoclinic space groupP2 ,a = 8.278(2),b = 14.904(2),c = 14.477(1) Å, = 91.24(1)°,V = 1785.7(1) ų,Z = 4,R = 0.068 for 4993 independent reflections. A novel three-dimensional host is built of the alternate array of the pn-chelated octahedral Cd and the tetrahedral Cd(CN)₄ linked at every N atom to the former Cd to provide a cage-like cavity for a pair of 1,2-dichloroethane guest molecules.     

Crystal structure of tris(2-pyridylthio-2-pyridinium)pentaisothiocyanato-dioxouranate(VI)

Summary The crystal structure of [DPSH] ₃ ⁺ [UO₂[NCS)₅]^3– (DPSH = 2 pyridylthio-2-pyridinium) has been determined by standard methods using diffractometer data. Crystals are monoclinic, space groupP2₁/a, witha=33.16 (3),b=16.68(2),c=7.85(1) Å, and=97.3(1); D_c=1.65 g · cm^–3 for Z=4. The structure has been refined to R=5.8% by least squares methods. Five thiocyanate groups are equatorially bonded to the linear uranyl group. The mean of the five U-N, N-C, and C-S bond distances are 2.45, 1.17, and 1.59 Å respectively. The protonated DPS molecules have the N,N-inside conformations.