The crystal structure of 1-azoniatricyclo[4.4.4.01,6]tetradecane and 1-azoniatricyclo[4.4.3.01,6]tridecane bromides

1982 ◽  
Vol 60 (9) ◽  
pp. 1073-1077 ◽  
Author(s):  
John M. McIntosh ◽  
Masood A. Khan ◽  
Louis T. J. Delbaere
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Nmr Spectra ◽  
Membered Ring ◽  
Unit Cell ◽  
Space Group ◽  
The One

The crystal structures of 1-azoniatricyclo[4.4.4.01,6]tetradecane bromide (1) and 1-azoniatricyclo[4.4.3.01,6]tridecane bromide (2) are reported. Compound 1, C13H24NBr, crystallizes in space group P63/mmc with a = 8.383(2) Å, c = 10.092 Å, γ = 120°, Z = 2. Compound 2, C12H22NBr, crystallizes in space group P63/mmc with a = 8.283(2) Å, c = 10.046(2) Å, γ = 120°, Z = 2. The crystal structures of 1 and 2 are statistically disordered with both enantiomers occurring in the unit cell. Compound 2 is further disordered with the one five-membered ring and the two six-membered rings of the cation being averaged over the same site in the unit cell.The structures confirm the previously reported conclusions based on the 400 MHz nmr spectra of 1.

Synthesen und Kristallstrukturen der Lithiumphosphide {Li(DME)[P(t-Bu)2]}2 und [Li(DME)PPh2]∞ / Syntheses and Crystal Structures of the Lithium Phosphides {Li(DME)[P(t-Bu)2]}2 and [Li(DME)PPh2]∞

1993 ◽  
Vol 48 (2) ◽  
pp. 156-160 ◽  
Author(s):  
Gudrun Stieglitz ◽  
Bernhard Neumüller ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Membered Ring ◽  
Space Group ◽  
Bond Lengths ◽  
Polymeric Chains ◽  
Structure Determinations ◽  
Centrosymmetric Dimers

AbstractThe title compounds have been prepared by the reaction of n-butyllithium with the corresponding diorganophosphanes HPR2 (R = t-Bu, Ph) in DME solutions. Both compounds were characterized by crystal structure determinations.{Li(DME)[P(t-Bu)2]}2: Space group P 1̄, Z = 1, 2027 observed unique reflections, R = 0.055. Lattice dimensions at -80 °C: a = 879.9(3), b = 986.3(1), c = 1064.0(2) pm, α = 70.69(1)°, β = 70.63(2)°, γ - 69.89(2)°. The compound forms centrosymmetric dimers of symmetry Ci with Li-P bond lengths of 260.0 and 257.3 pm for the Li2P2 four-membered ring.[Li(DME)PPh2]∞: Space group P21/n, Z = 4. 3437 observed unique reflections, R = 0.055. Lattice dimensions at - 80 °C: a = 1034.8(2), b = 812.48(9), c = 1978.4(3) pm, β = 103.30(2)°. The compound forms polymeric chains via LiP bridges with Li-P bond lengths o f 256.3 and 254.1 pm.

Molecular and Crystal Structure of Sildenafil Base

2012 ◽  
Vol 67 (5) ◽  
pp. 491-494 ◽  
Author(s):  
Dmitrijs Stepanovs ◽  
Anatoly Mishnev
Keyword(s):  
Crystal Structure ◽  
Erectile Dysfunction ◽  
Crystal Structures ◽  
Unit Cell ◽  
Sildenafil Citrate ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Sildenafil citrate monohydrate, well known as Viagra®, is a drug for the treatment of erectile dysfunction. Here we present the X-ray crystal structure of the sildenafil base, C22H30N6O4S. The compound crystallizes in the monoclinic system, space group P21/c with the unit cell parameters a = 17:273(1), b=17:0710(8), c=8:3171(4) Å , b =99:326(2), Z = 4, V = 2420:0(3) Å3. A comparison with the known crystal structures of sildenafil citrate monohydrate and sildenafil saccharinate is also presented.

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.

Phosphanimin- und Phosphaniminato-Komplexe des Zinks. Kristallstrukturen von [ZnCl2(Me3SiNP(CH2)4CMe3)]2, [ZnI2(Me3SiNPEt3)]2, [ZnI2{Me2Si(NPEt3)2}] und [ZnBr(NPMe3)]4· CH2Cl2/ Phosphaneimine and Phosphoraneiminato Complexes of Zinc. Crystal Structures of [ZnCl2(Me3SiNP(CH2)4CMe3)]2, [ZnI2(Me3SiNPEt3)]2, [Znl2{Me2Si(NPEt3)2}], and [ZnBr(NPMe3)]4· CH2Cl2

1997 ◽  
Vol 52 (2) ◽  
pp. 243-250 ◽  
Author(s):  
Matthias Krieger ◽  
Klaus Harms ◽  
Jörg Magull ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ir Spectra ◽  
Crystal Structures ◽  
Structure Determination ◽  
Chelating Agent ◽  
Membered Ring ◽  
Space Group ◽  
Zinc Crystal ◽  
Donor Acceptor

Abstract The donor-acceptor complexes [ZnCl2(Me3SiNP(CH2)4CMe3)]2 (1)and [ZnI2(Me3SiNPEt3)]2 (2) have been prepared from the zinc dihalides and the corresponding silylated phosphaneimines in CH2Cl2. Thermolysis of 2 leads to the formation of [ZnI2(Me2Si(NPEt3)2)] (3). Znl2 and ZnBr2 react with the silylated phosphaneimines Me3SiNPR3(R = Me, Et) in the presence of NaF at elavated temperatures to give the phosphoraneiminato complexes [ZnI(NPEt3)]4 (4), [ZnBr(NPMe3)]4 (5) and [ZnBr(NPEt3)]4 (6), respectively, which according to the IR spectra and to a crystal structure determination of 5 form heterocubane structures. The corresponding reactions with the more bulky phosphaneimine Me3SiNP(CH2)4CMe3 do not lead to a phosphoraneiminato complex of zinc. 1: Space group P21/n, Z = 2; lattice dimensions at -60 °C: a = 903.3(2), b = 1217.9(3), c = 1591.6(2) pm, β = 93.94(1)°, R = 0.031. 2: Space group P21/n, Z = 2; lattice dimensions at -70°C: a = 947.9(2), b = 1219.2(2), c - 1527.1(2) pm, 0 = 91.17(1)°, β = 0.045. 1 and 2 form centrosymmetric dimeric molecules via Zn2X2 bridges (X = Cl, I); bond lengths Zn-N = 198.7(2) pm (1) and 199.0(6) pm (2). 3: Space group P412121 Z = 8; lattice dimensions at -90°C: a = b = 965.4(1), c = 2796.9(2) pm, R = 0.019.3 forms monomeric molecules with the Me2Si(NPEt3)2 ligand as chelating agent to give a planar ZnN2Si four-membered ring with Zn-N distances of 207.0(2) pm. 5: Space group P42/nmc, Z = 2; lattice dimensions at -70°C: a = b = 1146.9(6), c = 1437.9(7) pm, R = 0.060.

scholarly journals Crystal chemistry of natural layered double hydroxides. 5. Single-crystal structure refinement of hydrotalcite, [Mg6Al2(OH)16](CO3)(H2O)4

2018 ◽  
Vol 83 (02) ◽  
pp. 269-280 ◽  
Author(s):  
Elena S. Zhitova ◽  
Sergey V. Krivovichev ◽  
Igor Pekov ◽  
H. Christopher Greenwell
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Crystal Structures ◽  
Structure Refinement ◽  
Unit Cell ◽  
Single Crystal Structure ◽  
Unit Cell Parameters ◽  
Diagnostic Features ◽  
Space Group ◽  
Cell Parameters

AbstractHydrotalcite, ideally [Mg6Al2(OH)16](CO3)(H2O)4, was studied in samples from Dypingdal, Snarum, Norway (3R and 2H), Zelentsovskaya pit (2H) and Praskovie–Evgenievskaya pit (2H) (both Southern Urals, Russia), Talnakh, Siberia, Russia (3R), Khibiny, Kola, Russia (3R), and St. Lawrence, New York, USA (3R and 2H). Two polytypes, 3R and 2H (both ‘classical’), were confirmed on the basis of single-crystal and powder X-ray diffraction data. Their chemical composition was studied by electron-microprobe analysis, infrared spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. The crystal structure of hydrotalcite-3R was solved by direct methods in the space group R$ {\bar 3} $m on three crystals (two data collections at 290 K and one at 120 K). The unit-cell parameters are as follows (290/290/120 K): a = 3.0728(9)/3.0626(3)/3.0617(4), c = 23.326(9)/23.313(3)/23.203(3) Å and V = 190.7(1)/189.37(4)/188.36(4) Å3. The crystal structures were refined on the basis of 304/150/101 reflections to R1 = 0.075/0.041/0.038. Hydrotalcite-2H crystallises in the P63/mmc space group; unit-cell parameters for two crystals are (data collection at 290 K and 93 K): a = 3.046(1)/3.0521(9), c = 15.447(6)/15.439(4) Å, V = 124.39(8)/124.55(8) Å3. The crystal structures were refined on the basis of 160/142 reflections to R1 = 0.077/0.059. This paper reports the first single-crystal structure data on hydrotalcite. Hydrotalcite distribution in Nature, diagnostic features, polytypism, interlayer topology and localisation of M2+–M3+ cations within metal hydroxide layers are discussed.

Addukte Aromat/Chlorwasserstoff bei tiefen Temperaturen: Beiträge zu Bildung und Kristallstruktur [1] / Adducts Arene/Hydrogen Chloride at Low Temperatures: Contributions to Formation and Crystal Structure [1]

1993 ◽  
Vol 48 (5) ◽  
pp. 571-576 ◽  
Author(s):  
Axel Deeg ◽  
Dietrich Mootz
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Hydrogen Chloride ◽  
Low Temperatures ◽  
Unit Cell ◽  
Aromatic System ◽  
Space Group ◽  
Weak Hydrogen Bonds

The melting diagrams of the systems benzene-HCl, toluene-HCl and mesitylene-HCl have been established and the crystal structures of two adducts determined. The adduct toluene · 2 HCl, melting incongruently at -115°C, is monoclinic with space group C2/c and Ζ = 4 formula units per unit cell; the adduct mesitylene · HCl, m. p. -64°C, is orthorhombic with space group Pbca and Ζ = 8. The HCl molecules are situated on both sides and one side, respectively, of the plane of the aromatic system and are linked to it by weak hydrogen bonds of the type Cl-H···π.

Preparation of Cr2(CO)8(NO)2 and X-ray crystal structures of Cr2(CO)8(NO)2 and Cr2(CO)9NO−. Stereochemical comparisons to Cr2(CO)102−

1991 ◽  
Vol 69 (12) ◽  
pp. 2136-2141 ◽  
Author(s):  
A. P. Masters ◽  
M. Parvez ◽  
T. S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Bond Length ◽  
Key Words ◽  
Crystal Structures ◽  
Quantitative Yield ◽  
Space Group ◽  
X Ray ◽  
Metal Metal ◽  
Chromium Carbonyl ◽  
The One

Cr2(CO)8(NO)2 (1) has been prepared and characterized, and the crystal structure determined, along with that of the related salt Cr2(CO)9NO− monoanion (2) as the CH2Cl2-solvated PPN+ salt (where PPN+ denotes the (PPh3)2N+ monocation). Both 1 and 2 possess a metal–metal bonded structure analogous to that of Mn2(CO)10 and the electronically equivalent Cr2(CO)102− dianion. Although Cr2(CO)8(NO)2 (1) is slowly formed in poor yield from Cr(CO)4NO− and Cr(CO)4NOBr, it can be prepared in an almost quantitative yield by the one-electron oxidation of the monoanion with trityl hexafluorophosphate. The slowness of the former reaction makes Cr(CO)4NO− useful as a two-electron reductant of organohalide bonds. Triclinic crystals of 1 incorporate two distinct molecules in die [Formula: see text] space group, although the geometries of each are almost identical. Triclinic crystals of monoanion (2) also belong to the [Formula: see text] space group. The Cr—Cr bond length is 3.00–3.02 Å in 1 and 2.995 Å in 2, compared to 2.904 Å for the central Mn—Mn bond in Mn2(CO)10. Key words: chromium nitrosyl, chromium carbonyl, X-ray crystal structure, metalate anion, metal–metal dimer.

scholarly journals Packing polymorphism in the structure oftrans-aqua[N,N′-bis(salicylidene)ethane-1,2-diamine-κ4O,N,N′,O′]chloridomanganese(III) monohydrate

2018 ◽  
Vol 74 (12) ◽  
pp. 1778-1782
Author(s):  
Juan Alberto Reyes Perea ◽  
Sylvain Bernès ◽  
Ma Guadalupe Quintero Téllez
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Unit Cell Parameter ◽  
Molecular Conformation ◽  
Cell Parameter ◽  
Title Complex ◽  
Unit Cell ◽  
Alternative Synthesis ◽  
Space Group ◽  
Structural Database

The crystal structure of the title complex (systematic name:trans-aquachlorido{2,2′[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato-κ4O,N,N′,O′}manganese(III) monohydrate), [Mn(C16H14N2O2)Cl(H2O)]·H2O has been reported previously in the space groupP21/n[Panjaet al.(2003).Polyhedron,22, 1191–1198]. We obtained the same hydrated complex through an alternative synthesis, and crystallized a new polymorph, in the space groupP21. The molecular conformation of the complex is virtually unmodified, but the absence of the glide plane in the new polymorph halves the unit-cell parameterc, affording a non-centrosymmetric crystal structure withZ= 2, while the previously reported crystal is centrosymmetric withZ= 4. Both phases represent a case of packing polymorphism, similar to other dimorphic crystal structures retrieved from the Cambridge Structural Database.

Notizen: Über die Kristallstruktur von β-SCl3+SbCl6- und interionischen Wechselwirkungen in SCl3+-Salzen/The Crystal Structure of β-SCl3+SbCl6- and Interionic Interactions in SCl3+ Salts

1992 ◽  
Vol 47 (4) ◽  
pp. 594-596 ◽  
Author(s):  
Rolf Minkwitz ◽  
Andreas Kornath ◽  
Hans Preut
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Unit Cell ◽  
Octahedral Coordination ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Distorted Octahedral Coordination ◽  
Distorted Octahedral ◽  
Interionic Interactions

Chlorosulfonium hexachloroantimonate crystallizes in the monoclinic space group C 2/m with a = 1405.5(3) pm, b = 1055.1(2) pm , c = 882.2(2) pm, β = 110.05(3)° at 169 K with 4 formula units per unit cell. A distorted octahedral coordination around sulphur is formed by three S - C l bonds and three interionic sulphur chlorine contacts. The interionic interactions in SCl3+ salts of known crystal structures are discussed.

A three-coordinate complex of mercury: crystal structure of bis(iodo-N,N-diethyldithiocarbamatomercury(II))

1977 ◽  
Vol 55 (1) ◽  
pp. 65-69 ◽  
Author(s):  
Chung Chieh
Keyword(s):  
Crystal Structure ◽  
Membered Ring ◽  
Unit Cell ◽  
Mercuric Iodide ◽  
Space Group ◽  
R Factor ◽  
Mercuric Ion

Reaction of mercuric iodide with N,N,N′,N′-tetraethylthiuramdisulfide (TETD), [Formula: see text] gave bis(iodo-N,N-diethyldithiocarbamatomercury(II)) and diiodo-N,N,N′,N′-tetraethylthiuramdisulfidemercury(II). The crystal of the former was mono-clinic with a = 7.645(3), b = 7.787(4), c = 18.005(7) Å and β = 102.08(4)°. The space group was P21/c, with two dimeric molecules per unit cell. Diffractometer measured intensities of 1727 observed reflections were used to determine the structure; the final R factor being 0.059. The mercuric ion was three-coordinated with two Hg—S distances of 2.422(4) and 2.644(4) Å and one Hg—I distance of 2.641(1) Å. The dimer had a centre of symmetry and formed an eight-membered ring.

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