79Br, 127I NQR of Diammoniumalkyl Halides and Piperazinium Halides. Crystal Structure of Piperazinium Dibromide Monohydrate and Piperazinium Monoiodide

1989 ◽  
Vol 44 (1) ◽  
pp. 41-55 ◽  
Author(s):  
Jutta Hartmann ◽  
Shi-Qi Dou ◽  
Alarich Weiss
Keyword(s):  
Crystal Structure ◽  
Phase Transitions ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Temperature Range

Abstract The 79Br and 127I NQR spectra were investigated for 1,2-diammoniumethane dibromide, -diiodide, 1,3-diammoniumpropane dibromide, -diiodide, piperazinium dibromide monohydrate, and piperazinium monoiodide in the temperature range 77 ≦ T/K ≦ 420. Phase transitions could be observed for the three iodides. The temperatures for the phase transitions are: 400 K and 404 K for 1,2-diammoniumethane diiodide, 366 K for 1,3-diammoniumpropane diiodide, and 196 K for piperazinium monoiodide.The crystal structures were determined for the piperazinium compounds. Piperazinium dibromide monohydrate crystallizes monoclinic, space group C2/c, with a= 1148.7 pm, 0 = 590.5 pm, c= 1501.6pm, β = 118.18°, and Z = 4. For piperazinium monoiodide the orthorhombic space group Pmn 21 was found with a = 958.1 pm, b = 776.9 pm, c = 989.3 pm, Z = 4. Hydrogen bonds N - H ... X with X = Br, I were compared with literature data.

Mono- and difunctional furan-based 1,2,3,5-dithiadiazolyl radicals; preparation and solid state structures of 2,5-[(S2N2C)OC4H2(CN2S2)] and 2,5-[(S2N2C)OC4H2(CN)]

1992 ◽  
Vol 70 (3) ◽  
pp. 919-925 ◽  
Author(s):  
A. Wallace Cordes ◽  
Charles M. Chamchoumis ◽  
Robin G. Hicks ◽  
Richard T. Oakley ◽  
Kelly M. Young ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
The Mean ◽  
Solid State Structures ◽  
Solid State Characterization

The preparation and solid state characterization of the bifunctional radical furan-2,5-bis(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN2S2)] and the related monofunctional radical 2-cyanofuran-5-(1,2,3,5-dithiadiazolyl) 2,5-[(S2N2C)OC4H2(CN)] are described. The crystal structure of 2,5-[(S2N2C)OC4H2(CN2S2)] is orthorhombic, space group Pna21, and consists of interleaved arrays of dimers, for which the mean interannular [Formula: see text] contact is 3.137 Å. The crystal structure of the monofunctional radical 2,5-[(S2N2C)OC4H2(CN)] is monoclinic, space group P21/n, and consists of a ribbon-like network of dimers (mean interannular [Formula: see text] interconnected by close head-to-tail [Formula: see text] contacts. The dimer units form stacks parallel to z, with a mean interdimer [Formula: see text] separation of 3.956 Å. The similarities and differences between these two crystal structures and those of related benzene-substituted systems are discussed. Keywords: dithiadiazolyl radicals, furan-based diradicals, cyanofuran-based radicals, radical dimers, crystal structures.

Synthese und Kristallstrukturen von N-[ω-(Dimethylammonio)alkyl]- N´,N´,N´´,N´´-tetramethylguanidinium-chlorid-tetraphenylboraten / Synthesis and Crystal Structures of N-[ω-(Dimethylammonio)alkyl]-N´,N´,N´´,N´´- tetramethylguanidinium Chloride Tetraphenylborates

2010 ◽  
Vol 65 (7) ◽  
pp. 907-916 ◽  
Author(s):  
Ioannis Tiritiris ◽  
Falk Lissner ◽  
Thomas Schleid ◽  
Willi Kantlehner
Keyword(s):  
Crystal Structure ◽  
Low Temperature ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Room Temperature ◽  
Chloride Ions ◽  
Monoclinic Space Group ◽  
Temperature Structure ◽  
Space Group ◽  
Temperature Modification

Dicationic N,N´,N´,N´´,N´´-pentasubstituted guanidinium dichlorides 4a, b are obtained from the chloroformamidinium salt 2 and diamines 3a, b. N-[2-(Dimethylammonio)ethyl]-N´,N´,N´´,N´´-tetramethylguanidinium chloride tetraphenylborate (5a) and N-[3-(dimethylammonio)propyl]-N´,N´,N´´,N´´-tetramethylguanidinium chloride tetraphenylborate (5b) were synthesized from 4a, b by anion metathesis with one equivalent of sodium tetraphenylborate. The thermal properties of the salts 5a, b were studied by means of DSC methods, and their crystal structures were determined by single-crystal X-ray diffraction analysis. For 5a a solid-solid phase transition is observed at −156 ◦C to a low-temperature structure. The room-temperature modification (α-5a) crystallizes in the centrosymmetric orthorhombic space group Pbca (a = 13.1844(4), b = 13.8007(4), c = 34.7537(11) A° ).The guanidinium ions are interconnected via chloride ions through bridging N-H· · ·Cl hydrogen bonds, providing isolated units. The tetraphenylborate ions show some dynamic disordering in the crystal structure. The low-temperature modification (β -5a) also crystallizes orthorhombically, but in the non-centrosymmetric space group Pna21 (a = 13.1099(4), b = 69.1810(11), c = 13.5847(5) A° ) and consists of four crystallographically independent cations and anions in the unit cell. Compared with the room-temperature structure, a similar N-H· · ·Cl hydrogen bond pattern is observed in the β -phase, but the tetraphenylborate ions are now completely ordered. 5b crystallizes in the monoclinic space group P21/c (a = 10.8010(3), b = 14.1502(5), c = 20.9867(9) A° , β = 94.322(1)◦). In the crystal structure the guanidinium ions are linked via chloride ions through N-H· · ·Cl hydrogen bonds, but in contrast to 5a two infinite strands are formed along the a axis with the tetraphenylborate ions interspersed between them for charge compensation.

Halogen NQR and Crystal Structure of Ammonium Halides (R-NH3)+X- and (X–) (+H3NR´­NH3+) (X–). R = (HOCH2)3C, R´ = CH2C(CH3)2CH2; X = I,Br

1994 ◽  
Vol 49 (1-2) ◽  
pp. 174-184
Author(s):  
Shi-qi Dou ◽  
Hartmut Fuess ◽  
Helmut Paulus ◽  
Alarich Weiss
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Unit Cell ◽  
Space Group ◽  
Temperature Range ◽  
Ammonium Halides

AbstractThe 127I-NQR of(HOCH2)3CNH3+ I- was determined in the range 77 ≤ T/K ≤ 310. At T = 310 K the NQR signal fades out (Tm = 463 K). The 127I spectrum ( T =77 K.): v1 =29.195 MHz, v2 = 14.597 MHz, η(121l)=0, e QΦzz h-1 (127I) = 97.315 MHz, is in agreement with the crystal structure. The 127I NQR spectrum of 1,3-diammonium-2,2-dimethylpropane diiodide, (H3NCH2C(CH3)2CH2NH3)2+ ·2I- , is a quartet within the whole temperature range investigated, and the lines correspond to two crystallographically independent iodines: Space group P21/c, Z = 4, a = 731.2(3) pm, b = 689.0(3) pm, c = 2255.1(8) pm, β = 104.90(1)°. At 7 = 7 7 K the 127I NQR quartet is (MHz): v1 = 34.145, v2 = 32.805, v3 = 22.113, v4 = 16.787; at 295 K (same order, MHz): 30.559, 29.729, 19.810, 15.651. There are two combinations of the NQR frequencies. Considering the coordination of I-, the hydrogen bonds N -H ··· I, eQΦzzQ h-1 and η, we choose for I(1) v1 and v3, for I(2) v2 and v4. At 77 K eQΦzzQ h-1 (I(1))= 118.86 MHz,η (127I(1)) = 0.498, eQΦzzQ h-1 (I(2)) = 109.75 MHz, η(127I(2)) = 0.135 follow for the two iodine atoms. Both, eQΦzzQ h-1 (I(1)) and e eΦzzQ h-1(I(2)) decrease smoothly with increasing T: η I(2)) increases with increasing T whereas η(127I(1)) is almost constant within 77 ≤ T /K ≤ 4 0 6 . The 79,81Br NQR spectrum of l,3-diamino-2,2-dimethylpropane dihydrobromide is also a quartet, showing two crystallographic inequivalent Br atoms in the unit cell. The frequencies are (T =273 K, MHz): v1 (79Br)= 14.303, v2 (79Br)= 12.884, (81Br)= 11.951, v2(81Br) = 10.781; space group C2/c, Z = 8 , a = 2136.4(6) pm, b = 854.6(3) pm, c = 1125.8(3) pm, β = 93.23(1)°. Crystal structures and NQR results are discussed.

Two lithium tricyanomethanide compounds: syntheses and single-crystal structure determination of LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO

2015 ◽  
Vol 70 (3) ◽  
pp. 191-196 ◽  
Author(s):  
Olaf Reckeweg ◽  
Francis J. DiSalvo
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Single Crystals ◽  
Structure Determination ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
New Compounds

AbstractThe new compounds LiK[C(CN)3]2 and Li[C(CN)3]·½ (H3C)2CO were synthesized and their crystal structures were determined. Li[C(CN)3]·½ (H3C)2CO crystallizes in the orthorhombic space group Ima2 (no. 46) with the cell parameters a=794.97(14), b=1165.1(2) and c=1485.4(3) pm, while LiK[C(CN)3]2 adopts the monoclinic space group P21/c (no. 14) with the cell parameters a=1265.7(2), b=1068.0(2) and c=778.36(12) pm and the angle β=95.775(7)°. Single crystals of K[C(CN)3] were also acquired, and the crystal structure was refined more precisely than before corroborating earlier results.

The Dichloroplatinum(II) and Dichloropalladium(II) Complexes of 1,4-Diazacycloheptane: Preparative, Structural and Conformational Studies

1996 ◽  
Vol 49 (12) ◽  
pp. 1301 ◽  
Author(s):  
GW Allen ◽  
ECH Ling ◽  
LV Krippner ◽  
TW Hambley
Keyword(s):  
Crystal Structures ◽  
Chelate Ring ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Membered Chelate Ring ◽  
Alternative Conformation

The preparation and purification of [Pt( hpip )Cl2] and [Pd( hpip )Cl2] ( hpip = homopiperazine = 1,4-diazacycloheptane) are described. Crystal structures of [Pt( hpip )Cl2] and [Pd( hpip )Cl2] have been determined by X-ray diffraction methods and refined to R values of 0.023 (932 F) and 0.023 (948 F). The crystals of [Pt( hpip )Cl2] are orthorhombic, space group Pbcm , a 7.7019(8), b 9.8080(12), c 12.1944(14) Ǻ, and those of [Pd( hpip )Cl2] are monoclinic, space group P21/m, a 6.1001(9), b 11.527(2), c 6.458(I) Ǻ, β 106.30(2)°. The seven- membered rings of the ligands in both complexes adopt boat-like conformations in which the five- membered chelate ring has an eclipsed N-C-C-N group and the six- membered chelate ring adopts a chair conformation. Molecular mechanics methods were used to investigate whether this conformation was a crystallographic artefact but it was found to be real. An alternative conformation in which the six-membered chelate ring adopts a skew-boat conformation was also investigated. It was found to be less stable than the conformation observed in the crystal structures, but to a degree that depends on whether non-bonded interactions involving the metal atom were included or not.

Strukturen der mehrkernigen nickelthiolato-komplexe [(μ-SMe)2(Ni(MeNHCS2))2] und cyclo-[(μ-SMe)2Ni]6 / Structures of Two Polynuclear Nickel-Thiolato-Complexes [(μ-SMe)2(Ni(MeNHCS2))2] and cyclo-[(μ-SMe)2Ni]6

1994 ◽  
Vol 49 (6) ◽  
pp. 770-772 ◽  
Author(s):  
Klaus Schulbert ◽  
Rainer Mattes
Keyword(s):  
Crystal Structures ◽  
Nickel Acetate ◽  
Monoclinic Space Group ◽  
Crystal Data ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Dithiocarbamic Acid ◽  
Coordination Spheres ◽  
Partial Degradation ◽  
Acid Esters

The reactions of N-substituted dithiocarbamic acid esters and nickel acetate yield, by partial degradation of the esters, the polynuclear nickel thiolato complexes cyclo-[(μ-SMe)2Ni]6, 1 and [(μ-SMe)2(Ni(MeNHCS2))2, 2. Their crystal structures have been determined. The Ni coordination spheres are comprised of four sulfur atoms in a planar arrangement. 1 is a second, highly symmetrical modification of the already known cyclic hexamer Ni6(SMe)12. In 2 two Ni(PhNHCS2) moieties are bridged to dimers by thiolato groups. Two of these dimers are connected to a tetramer by weak axial Ni-S interactions. Crystal data for 1: monoclinic, space group P21/n, a = 986.1(2), b = 1308.1(3), c = 1228.6(2) pm, β = 96.07(3)°, Z = 2, R = 0.072, Rw = 0.062, 3797 reflections. 2: orthorhombic, space group Pnma, a = 1790.0(4), b = 1806.7(4), c = 934.4(2) pm. Z = 4, R = 0.061, Rw = 0.051, 2079 reflections

scholarly journals Die Kristallstrukturen von (1,5-Ditolylpentaazadienido)(triphenylphosphan)gold(I) und 1,5-Ditolyl-3-methylpentaazadien / The Crystal Structures of (1,5-Ditolylpentaazadienido)(triphenylphosphane)gold(I) and 1,5-Ditolyl-3-methylpentaazadien

1988 ◽  
Vol 43 (10) ◽  
pp. 1219-1223 ◽  
Author(s):  
Johannes Beck
Keyword(s):  
Nitrogen Atom ◽  
Crystal Structures ◽  
Phosphorus Atom ◽  
Gold Atom ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Lattice Constants ◽  
Monomeric Complex ◽  
Single Bonds

PPh3Au(tolN5tol) is obtained by the reaction of PPh3Au+ClO4- with Tl(tolN5tol). It crystallizes in the monoclinic space group P21/c with the lattice parameters a = 1548.8(5), b = 1070.7(2), c = 1779.1(3) pm, β = 90.33(2)°, Z = 4. In the monomeric complex the gold atom is nearly linearcoordinated by the phosphorus atom of the PPh3 group and nitrogen atom N3 of the pentaazadienido ligand ( N3 - Au - P 178.4°). tolNN(NCH3)NNtol crystallizes in the orthorhombic space group Pccn with the lattice constants a = 2426.7(9), b = 469.3(2), c = 1195.3(4) pm. The unit cell contains four molecules, located on twofold axes. Due to the isolobality of the CH3 and the PPh3Au group, the two structures are closely related. Both contain the typical planar zig-zag chain of five nitrogen atoms with located double bonds N1-N2 and N4 - N5 (from 119.8 to 126.6 pm) and shortened single bonds N2 - N3 and N3 - N4 (132.7 to 140.0 pm).

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.

The Constituents of Marine Sponges. IX New Norditerpenoids from Aplysilla pallida

1997 ◽  
Vol 50 (9) ◽  
pp. 903 ◽  
Author(s):  
Trevor W. Hambley ◽  
Walter C. Taylor ◽  
Stephen Toth
Keyword(s):  
Crystal Structures ◽  
Spectroscopic Studies ◽  
Marine Sponges ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

Four novel norditerpenoids were isolated from a new encrusting sponge, conveniently labelled Aplysilla pallida. The structures of aplypallidenone (1), aplypallidoxone (2), aplypallidione (3) and aplypallidioxone (4) were elucidated by spectroscopic studies and the crystal structures of aplypallidenone and aplypallidoxone have been determined by X-ray diffraction methods. The structure of (1) was refined to a residual of 0·040 for 1665 independent observed reflections and the structure of (2) was refined to a residual of 0·031 for 1699 independent observed reflections. The crystals of (1) are orthorhombic, space group P212121, a 7·728(2), b 10·838(4), c 24·880(5) Å, Z 4. Those of (2) are monoclinic, space group C 2, a 23·927(7), b 6·674(2), c 14·033(3) Å, Z 4.

Organoamido- and Aryloxo-lanthanoids. XII. The Coordination Chemistry of Bis(2-phenylindol-1-yl)ytterbium(II), and the X-Ray Crystal Structures of Yb(pin)2(diglyme)(thf) and [Yb(pin)2(dme)]2 (pin = 2-Phenylindol-1-yl, diglyme = Bis(2-methoxyethyl) Ether, thf Equals Tetrahydrofuran, dme = 1,2-Dimethoxyethane)

1995 ◽  
Vol 48 (12) ◽  
pp. 1933 ◽  
Author(s):  
CT Abrahams ◽  
GB Deacon ◽  
CM Forsyth ◽  
WC Patalinghug ◽  
BW Skelton ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Coordination Chemistry ◽  
Crystal Structures ◽  
Coordination Polyhedron ◽  
Basal Plane ◽  
Monoclinic Space Group ◽  
Coordinate Structure ◽  
Space Group ◽  
X Ray ◽  
Nitrogen Donor

With the facile displacement being utilized of thf from Yb(pin)2(thf)4 (pin = 2-phenylindol-1-yl, thf = tetrahydrofuran) in toluene solution, the complexes Yb(pin)2(dme)2 (dme = 1,2- dimethoxyethane), Yb(pin)2 (tmen)(tmen = N,N,N′,N′-tetramethylethane-1,2-diamine) and Yb(pin)2(diglyme)(thf) (diglyme = bis(2-methoxyethyl) ether) have been prepared from the respective ligands and Yb(pin)2(thf)4. Yb(pin)2 (diglyme) (thf) [monoclinic, space group P 21 /c, a 15.35(1), b 16.179(5), c 14.45(2) Ǻ, β 107.51(8)°, Z 4, R 0.044 for 2956 (I > 3σ(I)) 'observed' reflections] has a monomeric six-coordinate structure with transoid nitrogen donor atoms, N-Yb-N 143.6(4)° and an irregular coordination polyhedron described as either a distorted trigonal prism or a monocapped square pyramid. Attempted crystallization of Yb(pin)2 (thf) by partial desolvation of Yb(pin)2(thf)4 in hot toluene, containing a trace of dme, gave a mixture of red Yb(pin)2(thf) and orange [Yb(pin)2(dme)]2. The latter was independently synthesized by partial desolvation of Yb(pin)2(dme)2 in toluene. An X-ray crystal structure showed [Yb(pin)2(dme)]2 [monoclinic, space group P 21/c, a 11 .614(2), b 15.945(7), c 15.327(4) Ǻ, β 110.19(2)°, Z 2 dimers, R 0.070 for 2314 (I ≥ 3σ(I)) 'observed' reflections] to be a dimer with two bridging pin ligands, coordinated through nitrogen only. There is an approximately square pyramidal five-coordinate ytterbium environment with an apical dme oxygen, and with two bridging nitrogens, a terminal nitrogen, and a dme oxygen in the basal plane.

Sign in / Sign up

Export Citation Format

Share Document