Crystal Structures of (3S*,4S*,5S*,6S*)-3,4-Epoxy- 1,7-dioxaspiro[5.5]undecan-5-ol, (3R*,5S*,6S*)-1,7- Dioxaspiro[5.5]undecane-3,5-diyl Diacetate and (4S*,5S*,6S*)-1,7-Dioxaspiro[5.5]undecane-4,5-diol

1997 ◽  
Vol 50 (2) ◽  
pp. 123
Author(s):  
Margaret A. Brimble ◽  
Andrew Johnston ◽  
Trevor W. Hambley ◽  
Peter Turner
Keyword(s):  
Hydrogen Bonding ◽  
Hydroxy Group ◽  
Axial Position ◽  
Monoclinic Space Group ◽  
Equatorial Position ◽  
Intermolecular Hydrogen Bonding ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray Crystallography

The structures of (3S*,4S*,5S*,6S*)-3,4-epoxy-1,7-dioxaspiro[5.5]undecan-5-ol (2), (3R*,5S*,6S*)-1,7- dioxaspiro[5.5]undecane-3,5-diyl diacetate (4) and (4S*,5S*,6S*)-1,7-dioxaspiro[5.5]undecane-4,5-diol (5) have been determined by X-ray crystallography. The unsubstituted tetrahydropyran ring in (2) adopts an axial position with respect to the epoxy-substituted ring and the hydroxy group at C5 is syn to the epoxide group. Intermolecular hydrogen bonding is observed between the C5 hydroxy group and O1. The two six-membered rings in (4) adopt chair conformations and the two acetate groups adopt 1,3-diaxial positions. The C5 hydroxy group in (5) assumes an axial position anti to the C-O bond of the neighbouring ring whilst 4-OH occupies an equatorial position. Intermolecular hydrogen bonding is also observed between 4-OH and 5-OH. Compound (2), C9H14O4, M 186·21, crystallized in the monoclinic space group P 21/c with a 7·867(1), b 12·2060(9), c 9·3676(8) Å, b 102·744(8), V 877·4(1) Å 3 and No 1163 [I > 2·5s (I)], R 0·031, Rw 0·035. Compound (4), C13H20O6, M 272·30, crystallized in the triclinic space group P 1 with a 9·902(1), b 11·0024(9), c 6·9183(5)Å, a 104·078(8), b 96·769(9), g 101·980(8), V 703·8(1) Å 3 , No 1657 [I > 2·5s(I)], R 0·047, Rw 0·044. Compound (5), C9H16O4, M 188·22, crystallized in the orthorhombic space group Pbca with a 25·504(3), b 8·909(2), c 8·038(2) Å, V 1826·4(5) QA 3 , No 1096 [I > 2·5s(I)], R 0·030, Rw 0·030.

Electronic and Structural Properties of the Spin Crossover Systems Bis(2,6-bis(pyrazol-3-yl)pyridine)iron(II) Thiocyanate and Selenocyanate

2000 ◽  
Vol 53 (9) ◽  
pp. 755 ◽  
Author(s):  
Kristian H. Sugiyarto ◽  
Marcia L. Scudder ◽  
Donald C. Craig ◽  
Harold A. Goodwin
Keyword(s):  
Hydrogen Bonding ◽  
High Spin ◽  
Room Temperature ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Face To Face ◽  
Bright Yellow ◽  
Electronic And Structural Properties

Essentially high-spin [Fe(bpp)2][NCS]2·2H2O and [Fe(bpp)2][NCSe]2 (bpp = 2,6-bis(pyrazol-3-yl)pyridine) were isolated from an aqueous reaction mixture. Both salts undergo an abrupt transition to low spin below room temperature, that for the thiocyanate occurring in two steps and the high-spin Æ low-spin Æ high-spin cycle being accompanied by hysteresis in both steps. Recrystallization of the salts from nitromethane yielded a mixture from which bright yellow crystals were separated for structure determination. In addition, from the recrystallized selenocyanate, deep red-brown crystals of composition [Fe(bpp)2][NCSe]2·H2O·0.25 CH3NO2 were obtained. Recrystallized [Fe(bpp)2][NCS]2·2H2O and [Fe(bpp)2][NCSe]2 were identified as high spin with average Fe–N distances of 2.16 and 2.17 Å, respectively. In the unit cell of [Fe(bpp)2][NCSe]2·H2O·0.25 CH3NO2, there are four independent iron atoms, three identified as low spin and the fourth as high spin. All salts crystallize in a layer-type array involving edge-to-face and face-to-face aryl–aryl-type interactions. Hydrogen bonding between pyrazole >NH groups, anions and solvate molecules is observed. The structure of the uncoordinated ligand was also determined, the molecule being found in a planar arrangement with thecis–cis configuration for the pyrazolyl groups relative to the central pyridyl and the >NH group being at the N 2 atom. Hydrogen bonding involving the >NH groups leads to stepped stacks of molecules. The principal difference in the geometry of coordinated and free bpp molecules is a contraction in the angles about the interannular bridges in the chelate rings. [Fe(bpp)2][NCS]2·2H2O: triclinic, space group P1–, a 8.302(6), b 8.446(6), c 21.531(13) Å, a 78.78(5), b 82.80(5), g 89.85(4)˚, Z 2. [Fe(bpp)2][NCSe]2: triclinic, space group P1–, a 8.354(4), b 8.409(4), c 19.918(9) Å, a 87.02(3), b 83.15(3), g 88.86(3)˚, Z 2. [Fe(bpp)2][NCSe]2·H2O·0.25 CH3NO2: monoclinic, space group Pn, a 16.425(12), b 20.774(9), c 16.933(14) Å, b 90.91(4)˚, Z 8. Uncoordinated bpp: orthorhombic, space group Pna21, a 8.075(3), b 22.479(9), c 5.525(1) Å, b Z 4.

1-Aminocyclohexene-2,4-dicarbonitrile derivatives. Syntheses and structural study

1995 ◽  
Vol 73 (9) ◽  
pp. 1546-1555 ◽  
Author(s):  
Antonio Lorente ◽  
Carmen Galan ◽  
Isabel Fonseca ◽  
Juliana Sanz-Aparicio
Keyword(s):  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
Benzyl Cyanide ◽  
X Ray Crystallography ◽  
Conformational Preferences ◽  
Cell Dimensions ◽  
Substituted 1

Substituted 1-aminocyclohexene-2,4-dicarbonitriles were obtained by reaction of α,β-unsaturated nitriles (two equivalents) with benzyl cyanide. By recrystallization from ethanol one diastereomeric racemate was isolated in each case. The cyclohexene structures were established from spectroscopic data (IR, MS, and one- and two-dimensional NMR). Relative stereochemical configurations and conformational preferences in the solid state of cyclohexenes 2 and 3 and propanedicarbonitrile 1 were established from X-ray crystallography. Crystals of 1 (C17H14N2) belong to the orthorhombic space group Pbca. Cell dimensions are a = 17.168(7), b = 21.612(5), c = 7.508(2) Å, V = 2785(7) Å3. Final R = 0.078 and Rw = 0.091; 1363 reflections were observed. The compound 2 (C26H21N3) crystallizes in the monoclinic space group P21/n with Z = 4. The crystal data for 2 are a = 7.743(1), b = 24.420(1), c = 11.164(1) Å, β = 102.65(1)°, V = 2059.7(3) Å3. Final R = 0.046 and Rw = 0.059; 2701 reflections were observed. Crystals of 3 (C16H17N3) belong to the triclinic space group [Formula: see text] Cell dimensions are a = 14.582(1), b = 7.283(1), c = 7.116(1) Å, α = 110.84(0)°, β = 85.92(0)°, γ = 97.81(1)°, V = 696.9(2) Å3. Final R = 0.047 and Rw = 0.052; 2227 reflections were observed. The cyclohexene ring in 2 and 3 exists as a sofa rather then as a half-chair conformation. Keywords: 1-aminocyclohexenes, α,β-unsaturated nitriles, benzyl cyanide.

Supramoleküle aus Kronenethern und geminalen Sulfonen: Synthese von vier binären Komplexen und Kristallstruktur von (CH2CH2O)4·2H 2C(SO2C2H5)2/Supramolecules of Crown Ethers with Geminal Sulfones: Synthesis of Four Binary Complexes and Crystal Structure of (CH2CH2O )4·2H2C(SO2C2H5)2

1995 ◽  
Vol 50 (7) ◽  
pp. 1018-1024 ◽  
Author(s):  
Axel Michalides ◽  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Binary Complexes ◽  
Cyclic Polyethers ◽  
Adjacent Unit ◽  
Methylene Group

In a systematic search for supramolecular complexes involving all combinations of the cyclic polyethers 12-crown-4 (12C4), 15-crown-5 (15C 5), 18-crown-6 (18C 6) and dibenzo- 18-crown-6 (DB -18C6), and the geminal di- or trisulfones H2C(SO 2Me)2, H2C (SO2Et)2 and HC (SO2Me)3-n (SO2Et)n (n = 0 -3 ) , only the following four complexes could be isolated and unequivocally characterized by elemental analysis and 1H NMR spectroscopy: [(12C4){H2C (SO2Et)2}2] (3), [(18C6){H2C (S O2Me)2}] (4), [(DB -18C 6){H2C (SO2Et)2}] (5) and [(D B -18C 6)2{HC (SO2Me )(SO2Et)2}3] (6). The structure of 3 (triclinic, space group P1̄) consists of crystallographically centrosymmetric formula units, in which the disulfone molecules are bonded on each side of the ring by two C -H ··· O(crown) interactions originating from the central methylene group (H···O 213 pm) and from the methylene group of one EtSO2 moiety ( H ··· O 237 pm). Formula units related by translation are connected into parallel strands by a third type of reciprocal C -H ···O bond (H ···O 232 pm) between the second H atom of the central methylene group and a sulfonyl oxygen atom of the adjacent unit. The structure of 4 (monoclinic, space group C2/c) showed severe disorder of the crown ether and could not be refined satisfactorily. Compounds 5 and 6 crystallized as long and extremely thin fibres, indicative of linear-polymeric supramolecular structures; single crystals for X-ray crystallography were not available.

Untersuchungen an Polyhalogeniden, XXXVI. Zur Kenntnis des Oktaiodid-Ions I82-: Darstellung und Kristallstruktur des [(Crypt-2.2.2)H2]l8, des [Ni(phen)3]I8 · 2CHCl3 und der Bis(N-alkylurotropinium) oktaiodide (UrR)2I8 mit R = Methyl und Ethyl / Studies on Polyhalides, XXXVI. On the Octaiodide Ion I82-: Preparation and Crystal Structure of [(Crypt-2.2.2)H2]I8, of [Ni(phen)3]I8-2CHCl3 and of the Bis(N-alkylurotropinium)octaiodides (UrR)2I8 with R = methyl and ethyl

1998 ◽  
Vol 53 (7) ◽  
pp. 641-652 ◽  
Author(s):  
Arista Gräfe-Kavoosian ◽  
Shida Nafepour ◽  
Klaus Nagel ◽  
Karl-Friedrich Tebbe
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Iodine Molecule ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group

Abstract The new compound [(Crypt-2.2.2)H2]I8 has been prepared by the reaction of [(Crypt-2.2.2)H2](I3)2 with iodine in methanol. It crystallizes in the orthorhombic space group Pbcn with a = 11.476 (2), b = 13.589 (2), c = 22.888 (2) Å and Z = 4. The crystal structure has been refined to RF = 0.031 for 1618 reflections. It may be described as a layerlike packing of octaiodide anions I82-and diprotonated 2.2.2-Crypt as cations. The non planar octaiodide anion is built up from two triiodide groups and a bridging iodine molecule.Tris(1, 10-phenanthroline)nickel(II) octaiodide bis(chloroform) crystallizes in the monoclinic space group P21/n with a = 11.683 (8), b = 21.717 (8), c = 20.752 (5) Å, β = 95.03 (5)° and Z = 4 formula units. The crystal structure has been refined to RF = 0.058 for 3894 reflections. The structure consists of two chloroform molecules, octahedrally coordinated complex cations [Ni(phen)3]2+ and nonplanar octaiodide anions I82- each composed of two asymmetric triiodide units I3- weakly associated with an elongated bridging iodine molecule I2.The already known structure of bis(N-methylurotropinium) octaiodide, (UrMe)2I8, has been verified and more accurate crystal data have been collected. The crystal structure has been refined to RF = 0.045 for 1908 reflections. The compound crystallizes in the monoclinic space group P21/c with a = 11.302 (2), b = 9.850 (2), c = 14.188 (2) Å , β = 92.59 (1)° and Z = 2. The anion has the shape of a stretched Z.The structure of bis(N-ethylurotropinium) octaiodide (UrEt)2I8 has been determined and a new configuration (I3-, I5-) for octaiodide ions between Z (I3- · I2 ·I3-) and a “broken” configuration (I3-, I5-) has been observed. The compound crystallizes in the triclinic space group P1̄ with a = 9.741 (3), b = 11.815 (3), c = 15.426 (3) Å, α = 91.80 (2), β = 107.14 (2), γ = 90.04 (2)° and Z = 2. The crystal structure has been refined to RF = 0.037 for 3657 reflections.

scholarly journals P1 or P\bar 1? Corrigendum

2000 ◽  
Vol 56 (4) ◽  
pp. 744-744 ◽  
Author(s):  
Richard E. Marsh
Keyword(s):  
Nauk Sssr ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Acta Cryst ◽  
Triclinic Space Group ◽  
Space Group ◽  
Akad Nauk Sssr

The structure of bis((phenyl-O,N,N-azoxy)oxy)methane, C_{13}H_{12}N_4O_4, originally reported as triclinic, space group P1 [Zyuzin et al. (1997). Isz. Akad. Nauk SSSR Ser. Khim. pp. 1486–1492; CSD refcode NIXQAM] was recently revised to monoclinic, space group C2 [Marsh (1999). Acta Cryst. B55, 931–936]. It is properly described as orthorhombic, space group Fdd2.

Three polymorphs of 3-(3-phenyl-1H-1,2,4-triazol-5-yl)-2H-1-benzopyran-2-one formed from different solvents

2019 ◽  
Vol 75 (6) ◽  
pp. 822-832 ◽  
Author(s):  
Svitlana V. Shishkina ◽  
Irina S. Konovalova ◽  
Pavlo V. Trostianko ◽  
Anna O. Geleverya ◽  
Sergiy M. Kovalenko ◽  
...  
Keyword(s):  
Hydrogen Bonds ◽  
Pairwise Interaction ◽  
Structural Motif ◽  
Monoclinic Space Group ◽  
Interaction Energies ◽  
Orthorhombic Space Group ◽  
Structure Packing ◽  
Triclinic Space Group ◽  
Space Group ◽  
Polymorphic Modifications

The polymorphic study of 3-(3-phenyl-1H-1,2,4-triazol-5-yl)-2H-1-benzopyran-2-one, C17H11N3O2, was performed due to its potential biological activity and revealed three polymorphic modifications in the triclinic space group P\overline{1}, the monoclinic space group P21 and the orthorhombic space group Pbca. These polymorphs have a one-column layered type of crystal organization. The strongest interactions between the molecules of the studied structures is stacking between π-systems, while N—H...N and C—H...O hydrogen bonds link stacked columns forming layers as a secondary basic structural motif. C—H...π hydrogen bonds were observed between neighbouring layers and their role is the least significant in the formation of the crystal structure. Packing differences between the polymorphic modifications are minor and can be identified only using an analysis based on a comparison of the pairwise interaction energies.

Metal-selenolate chemistry: stereochemistry of adamantane-type clusters of formula [(μ-SePh)6(MSePh)4]2− (M = Zn and Cd)

1992 ◽  
Vol 70 (3) ◽  
pp. 792-801 ◽  
Author(s):  
Jagadese J. Vittal ◽  
Philip A. W. Dean ◽  
Nicholas C. Payne
Keyword(s):  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Bridging Ligands ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Space Groups ◽  
X Ray Crystallography ◽  
Cell Dimensions ◽  
Minimum Number

The structures of three tetramethylammonium salts containing anions of formula [(μ-SePh)6(MSePh)4]2− (M = Zn and Cd) were determined by single crystal X-ray diffraction techniques. The Zn salt crystallizes in different space groups depending upon the solvent combination used in the synthesis. Thus crystals of (Me4N)2[Zn4(SePh)10], 1, grown from a mixture of methanol, acetonitrile, and acetone are triclinic, space group [Formula: see text] with cell dimensions a = 13.214(2), b = 23.859(2), c = 13.072(1) Å, α = 91.134(8), β = 113.350(8), γ = 79.865(9)°, and Z = 2. In the absence of acetone, a solvated crystal (Me4N)2[Zn4(SePh)10]•CH3CN, 2, is formed, which belongs to the monoclinic space group P21/n with a = 14.248(1), b = 39.722(2), c = 13.408(1) Å, β = 97.132(5)°, and Z = 4. The Cd salt (Me4N)2[Cd4(SePh)10], 3, crystallizes in the monoclinic space group P21/c, with a = 20.830(2), b = 14.282(1), c = 25.872(1) Å, β = 99.626(6)°, and Z = 4. These three salts are the first examples of homoleptic, tetranuclear selenolatometal(II) anions with (μ-Se)6M4 cages of adamantane-type stereochemistry. In each case the phenyl substituents of the bridging ligands adopt the configuration [aae, aae, aee, aee], which has the minimum number of two 1,3-axial–axial non-bonding substituent interactions. Keywords: selenolate complexes, synthesis, X-ray crystallography, isomerism, adamantane stereochemistry.

Quinoxaline-1,2,3-dithiazolyls — Synthesis, EPR characterization, and redox chemistry

2001 ◽  
Vol 79 (9) ◽  
pp. 1352-1359
Author(s):  
A Wallace Cordes ◽  
James R Mingie ◽  
Richard T Oakley ◽  
Robert W Reed ◽  
Hongzhou Zhang
Keyword(s):  
Epr Spectroscopy ◽  
Ring Closure ◽  
Coupling Constants ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Molecular Conductors ◽  
Vacuum Sublimation ◽  
Space Group ◽  
X Ray Crystallography ◽  
Sulfenyl Chlorides

Oxidation of quinoxalineaminothiol with SCl2 or S2Cl2/Cl2 affords a series of compounds based on the quinoxaline-1,2,3-dithiazole framework QDTA. Under highly oxidizing conditions, the 1,2,3-dithiazolyl ring is opened to afford the acyclic dichlorosulfimino-sulfenyl chlorides Clx-QDTA-Cl3 (x = 0, 1, 2). Reduction of these "trichloro" compounds leads to ring closure. For x = 2, reduction using S2Cl2 affords the dithiazolylium chloride [Cl2-QDTA][Cl]. For all values of x, reduction with iodide ion (3 mol equiv) affords the corresponding dithiazolyl radical [Clx-QDTA]. The radicals can be isolated in good yield in crude form, but attempts to purify them by vacuum sublimation lead to thermal degradation. The radicals have nonetheless been fully characterized by EPR spectroscopy, and the assignments of the observed hyperfine coupling constants cross-matched with those obtained by computation at the B3LYP/6-31G** level. The structures of the trichloro compounds Clx-QDTA-Cl3 (x = 1, 2) have been confirmed by X-ray crystallography. Crystal data: Cl-QDTA-Cl3, monoclinic, space group C2/c, a = 30.561(5) Å, b = 4.9764(9) Å, c = 22.247(4) Å, β = 131.822(14)°, V = 2521.4(8) Å3, Z = 8, R(F) = 0.043, and Rw(F) [I [Formula: see text] σ (I)] = 0.049; Cl2-QDTA-Cl3, orthorhombic, space group Pnma, a = 18.627(12) Å, b = 6.848(4) Å, c = 10.926(7) Å, V = 1393.7(15) Å3, Z = 4, R(F) = 0.047, and Rw(F) [I [Formula: see text] 3σ(I)] = 0.060.Key words: thiazyl radicals, molecular conductors, EPR spectroscopy, quinoxaline, DFT calculations.

Kristallstrukturen der iodierten closo-Hexaborate trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P)2[B6H2I4] · 2 CH3CN und (CH2Py2)[B6HI5]/Crystal Structures of the Iodized closo-Hexaborates trans-(Ph4P)2[B6H4I2], mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2, trans-(Ph4P )2[B6H2I4] · 2 CH3CN and (CH2Py2)[B6HI5]

1998 ◽  
Vol 53 (2) ◽  
pp. 206-210 ◽  
Author(s):  
D. Sonnak ◽  
W. Preetz
Keyword(s):  
Single Crystals ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Structure Determinations

Abstract X-ray structure determinations have been performed on single crystals of trans-(Ph4P)2-[B6H4I2] (1) (triclinic, space group P1̄, a = 9.9680(12), b = 10.9690(11), c = 11.0470(14) Å,α = 88.167(9), β = 80.466(12), γ = 68.839(11)°, Z = 1), mer-(Ph4P)2[B6H3I3] · 2 CH2Cl2 (2)(triclinic, space group P1̄, a = 11.8694(11), b = 15.1699(13), c = 17.051(2) Å, α = 75.118(9), β = 71.953(10), γ = 69.331(8)°, Z = 2), trans-(Ph4P )2[B6H2I4] · 2 CH3CN (3) (monoclinic, space group P21/n, a = 14.9665(10), b = 7.6783(10), c = 23.385(3) Å, β = 95.78(9)°, Z = 2), and (CH2Py2)[B6HI5] (4) (orthorhombic, space group Pnma, a = 13.660(2), b = 11.8711(13), c = 13.839(2) Å, Z = 4). The B6 octahedra are compressed in the direction of the B-I bonds, resulting in shortened diagonal B ··· B distances with average values of the groups I-B ··· B-I = 2.37 and I-B ··· B-H = 2.43 Å as compared with H-B ··· B-H = 2.49 Å.

Syntheses and Crystal Structures of the Two New Polychalcogenides [Mn(C6H14N2)3]Se6 and [Mn(C6H14N2)3]2[C6H16N2](TeSe2)2Se

2004 ◽  
Vol 59 (6) ◽  
pp. 629-634 ◽  
Author(s):  
Frank Wendland ◽  
Christian Näther ◽  
Wolfgang Bensch
Keyword(s):  
Hydrogen Bonding ◽  
Single Step ◽  
Lattice Parameters ◽  
Solvothermal Reaction ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Layer Arrangement ◽  
Weak Hydrogen Bonding ◽  
Dark Blue

The solvothermal reaction of MnCl2·4 H2O, K2Se3 and Se in trans-cyclohexane-1,2-diamine (chxn) at 433 K yields dark blue crystals of [Mn(chxn)3]Se6 (1), and the reaction of MnCl2 ・4 H2O, K2Se3 and Te under similar conditions gives dark blue crystals of [Mn(chxn)3]2[H2chxn](TeSe2)2Se (2). While compound (1) crystallises in the orthorhombic space group Pbcn with the lattice parameters a = 13.7017(9), b = 19.9073(8) and c = 10.8058(5)Å , compound (2) crystallises in the monoclinic space group P21 with the lattice parameters a = 9.4396(6), b = 24.2450(2), c = 12.8170(8) Å and β =91.6(1)◦. In both structures discrete complex cations and polychalcogenide anions are found. In (1) the Se62− anions form a pseudo-layer arrangement with nearly rectangular pores. The complex cations are encapsulated by the arrangement of the Se62− anions. Some short distances between the amino groups of the ligands and the anions indicate weak hydrogen bonding. In compound (2) two independent [Mn(chxn)3]2+ and one unique H2chxn dications, two unique TeSe22− as well as one Se2− dianion coexist. The two complex cations exhibit different conformations. One of the two TeSe22− anions has the di-protonated chxn molecule in the neighbourhood and short Se···H separations indicate weak hydrogen bonding. The isolated Se2− ion is located above the ring of the di-protonated trans-cyclohexane-1,2-diamine molecule and again a short Se···H separation may be due to a weak hydrogen bond. Compound (1) decomposes in a single step when heated in an Ar atmosphere. In contrast, the thermal decomposition of compound (2) is complex and at least five different steps can be identified.

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