The Stability and Conformation of the 1,3,6,8-Tetraazatricyclo[4.4.1.13,8]dodecane System: the Structure of the Condensation Product of 1,2-Diaminocyclohexane and Formaldehyde

1975 ◽  
Vol 53 (13) ◽  
pp. 1933-1935 ◽  
Author(s):  
P. Murray-Rust ◽  
F. G. Riddell
Keyword(s):  
Structure Analysis ◽  
Condensation Product ◽  
Optically Active ◽  
Starting Material ◽  
Analogous Reaction ◽  
X Ray ◽  
The Stability

The condensation of d,1-trans-1,2-diaminocyclohexane with formaldehyde gives a pentacyclic molecule based on the 1,3,6,8-tetraazatricyclo[4.4.1.13,8]dodecane nucleus. This was shown to have S4 symmetry by 1H n.m.r. and an X-ray analysis showed crystals to be orthorhombic, Fddd, a = 12.02, b = 19.25, c = 12.90 Å. The symmetry of the compound in the crystal was D2d due to a disordered arrangement and structure analysis was carried out to R = 0.166. When optically active diamine was used as starting material, the analogous reaction did not occur and this was attributed to strain in the tricyclic system. The conformation of the molecule is related to those of similar compounds as found by X-ray analysis.

scholarly journals Pyridinium Pentachloridooxomolybdate(V), (PyH)2[MoOCl5], Revisited: Single-Crystal X-ray Structure Determination

Molbank ◽  
10.3390/m1249 ◽  
2021 ◽  
Vol 2021 (3) ◽  
pp. M1249
Author(s):  
Jaka Šturm ◽  
Barbara Modec
Keyword(s):  
Coordination Chemistry ◽  
Single Crystal ◽  
Structure Analysis ◽  
Structure Determination ◽  
Structural Characteristics ◽  
Starting Material ◽  
X Ray

(PyH)2[MoOCl5] was obtained in the form of emerald green crystals unintentionally from (PyH)5[MoOCl4(H2O)]3Cl2 in acetonitrile. (PyH)2[MoOCl5] has been used as a starting material in molybdenum(V) coordination chemistry for decades, yet its true identity has not been known until now. The X-ray structure analysis has undoubtedly confirmed the existence of this compound. The [MoOCl5]2− ion displays the usual structural characteristics of the mononuclear MoO3+-containing compounds.

scholarly journals Synthesis and photophysical properties of novel benzophospholo[3,2-b]indole derivatives

2017 ◽  
Vol 13 ◽  
pp. 2304-2309 ◽  
Author(s):  
Mio Matsumura ◽  
Mizuki Yamada ◽  
Atsuya Muranaka ◽  
Misae Kanai ◽  
Naoki Kakusawa ◽  
...  
Keyword(s):  
Structure Analysis ◽  
Phosphine Oxide ◽  
Photophysical Properties ◽  
Starting Material ◽  
Indole Derivatives ◽  
X Ray

The parent benzophospholo[3,2-b]indole was prepared by the reaction of dichlorophenylphosphine with a dilithium intermediate, which was prepared in two steps from 2-ethynyl-N,N-dimethylaniline. Using the obtained benzophosphole-fused indole as a common starting material, simple modifications were carried out at the phosphorus center of the phosphole, synthesizing various functionalized analogs. The X-ray structure analysis of trivalent phosphole and phosphine oxide showed that the fused tetracyclic moieties are planar. The benzophosphole-fused indoles, such as phosphine oxide, phospholium salt, and borane complex, exhibited strong photoluminescence in dichloromethane (Φ = 67–75%).

Preparation and Characterisation of Iodo-functionalised Azobenzene Derivatives of the Type I–p-C6H4–N=N–p-C6H4–X

2008 ◽  
Vol 63 (12) ◽  
pp. 1395-1401 ◽  
Author(s):  
Ulrich Siemeling ◽  
Clemens Bruhn ◽  
Mario Meier ◽  
Christian Schirrmacher
Keyword(s):  
Single Crystal ◽  
Structure Analysis ◽  
General Type ◽  
Starting Material ◽  
Type I ◽  
X Ray Diffraction ◽  
Ferrocene Derivative ◽  
X Ray ◽  
Derivatives Of ◽  
Azobenzene Derivatives

A broad range of azobenzene derivates of the general type I-p-C6H4-N=N-p-C6H4-X (1) have been prepared. In the case of X = Ph (b), C≡C-Fc (e, Fc = ferrocenyl), OMe (g), Oi-Pr (i), and NMe2 (m), these compounds have been characterised by single-crystal X-ray structure analysis. In addition, the closely related 4-dimethylamino-1-(4-iodophenylazo)naphthalene 2 and 8-(4-iodophenylazo) quinoline 3 have also been prepared. Furthermore, the ferrocene derivative Fc-C≡C-p-C6H4- NH2 (4), which served as a starting material for the synthesis of I-p-C6H4-N=N-p-C6H4-p-C6H4- C≡C-Fc (1e), was prepared and structurally characterised by X-ray diffraction.

X-ray reflection anomalous fine structure analysis of the stability of permalloy/copper multilayers

2001 ◽  
Vol 226-230 ◽  
pp. 1728-1729 ◽  
Author(s):  
G.M Luo ◽  
Z.H Mai ◽  
T.P.A Hase ◽  
B.D Fulthorpe ◽  
B.K Tanner ◽  
...  
Keyword(s):  
Fine Structure ◽  
Structure Analysis ◽  
X Ray ◽  
Fine Structure Analysis ◽  
The Stability

scholarly journals Hybrid Layered Crystal Comprising Polyoxometalate and Surfactant Synthesized from Reduced Mo-Blue Species

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Keisuke Mikurube ◽  
Kimiko Hasegawa ◽  
Haruo Naruke ◽  
Takeru Ito
Keyword(s):  
Structure Analysis ◽  
Single Phase ◽  
Proton Conductor ◽  
Starting Material ◽  
Layered Crystal ◽  
Two Dimensional ◽  
X Ray ◽  
New Class ◽  
Layered Crystals ◽  
Inorganic Layers

A hybrid layered crystal containing polyoxomolybdate was successfully synthesized from reduced Mo-blue species as starting material. The hybrid crystal, [C5H5N(C16H33)]2[β-H2Mo8O26]·2C2H5OH (C16py-H2Mo8), was obtained as a single phase by the gradual oxidation of hexadecylpyridinium-Mo-blue (C16py-Mo-blue) hybrid. The X-ray structure analysis revealed that C16py-H2Mo8comprisedβ-type octamolybdate anion with two protons (β-H2Mo8). Theβ-H2Mo8anions and ethanol molecules of crystallization formed two-dimensional anionic layers. The pyridine rings of C16py did not attend to form the two-dimensional inorganic layers, and the interdigitated C16py bilayers were sandwiched by theβ-H2Mo8anionic layers with periodicity of 18.2 Å. These C16py-H2Mo8hybrid layered crystals possibly work as a new class of proton conductor.

An efficient synthesis of an optically active (-)-(3R, 4R, 5R)-4-(1-hydroxyl-isopropyl)-3-acetyloxyl-butyrolactone

2005 ◽  
Vol 2005 (10) ◽  
pp. 665-668 ◽  
Author(s):  
JinXin Wang ◽  
ChaoXin Zhang ◽  
Ying Li ◽  
QiDong You
Keyword(s):  
Crystal Structure ◽  
Optically Active ◽  
Reductive Cleavage ◽  
Starting Material ◽  
Asymmetric Epoxidation ◽  
Efficient Synthesis ◽  
Cleavage Reaction ◽  
X Ray ◽  
Key Steps ◽  
Sharpless Asymmetric Epoxidation

An optically active β-hydroxyl–γ-butyrolactone was synthesised from nonchiral starting material by employing reductive cleavage reaction, Sharpless asymmetric epoxidation and dihydroxylation as key steps. This strategy can be used to prepare many chiral β-hydroxyl–γ-butyrolactone analogues. The crystal structure of 10 was determined by X-ray crystallographs.

Crystal packing of amides: X-ray structure analysis of optically active dilactylamide

1973 ◽  
Vol 29 (12) ◽  
pp. 2699-2702
Author(s):  
L. Mazzarella ◽  
C. Pedone ◽  
R. Puliti
Keyword(s):  
Structure Analysis ◽  
Crystal Packing ◽  
Optically Active ◽  
X Ray

Isolated versus Condensed Anion Structure VII: X-ray Structure Analysis of 1,3-Propanediammonium Dibromodichlorocadmate(II), [H3N(CH2)3NH3]CdBr2Cl2, and Estimation of Stability of Five-coordinated Halide Anions, MX53-(M = Cd, Zn; X = Cl, Br) by Means of Ab-initio MO Calculations

2001 ◽  
Vol 56 (9-10) ◽  
pp. 641-646 ◽  
Author(s):  
Hideta Ishihara ◽  
Toshiya Okajima ◽  
Keizo Horiuchi ◽  
Ingrid Svoboda ◽  
Hartmut Fuess
Keyword(s):  
Ab Initio Calculations ◽  
Ab Initio ◽  
Structure Analysis ◽  
Metal Cation ◽  
The Other ◽  
Mo Calculations ◽  
X Ray ◽  
Ab Initio Mo Calculations ◽  
The Stability ◽  
Positively Charged

Abstract The coordination capability of Cl and Br in halogenocadmate(II) complexes is estimated by a solution of the structure of 1,3-propanediammonium dibromodichlorocadmate(II). The compound crystallizes as a layered anion structure with Cl bridges and Br terminals at 293 K: Imma, a = 741.56(7), b = 1869.5(5), and c -771.55(8) pm, Z = 4. In order to explain the stronger tendency of halogenocadmate(II) complexes to form layered structures as compared to halogenozincate(II), ab-initio calculations were performed. The stability of MX53-(M = Cd, Zn; X = Cl, Br) is compared. Isolated ZnX53- and CdBr53- ions are not stable. On the other hand a trigonal bipyramid CdCl53- ion is considered to be subtly stable in the crystal mainly due to Coulomb attractive interactions between the positively charged metal cation Cd2+ in a CdCl3- fragment and two Cl- ions.

Reaktive E=C(p-p)π-Systeme, XLIII [1] Darstellung und Charakterisierung P-Phosphino- oder P-Arsino-substituierter Fluorphosphaalkene des Typs R2E-P=C(F)NEt2 (R = Me, CF3, Me2N; E = P, As) / Reactive E=C(p-p)-π Systems XLIII [1] Synthesis and Characterization of P-Phosphino or P-Arsino Substituted Fluorophosphaalkenes of the Type R2E-P=C(F)NEt2 (R= Me, CF3, Me2N; E = P As)

1996 ◽  
Vol 51 (6) ◽  
pp. 778-784 ◽  
Author(s):  
Joseph Grobe ◽  
Duc Le Van ◽  
Jost Winnemöller ◽  
Bernt Krebs ◽  
Mechtild Läge
Keyword(s):  
Lone Pair ◽  
Molar Ratio ◽  
Analogous Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Nitrogen Lone Pair ◽  
Type Interaction ◽  
The Stability ◽  
High Yields

Abstract The easily accessible phosphaalkene HP=C(F)NEt2 (lb) reacts with halophosphanes or -arsanes R2EX (X = Cl, I) in the presence of NEt3 to give P-phosphino- or -P-arsino substituted fluorophosphaalkenes of the type RiE-P=C(F)NEti (2 - 6) in high yields (60 - 85 %) [R2E: (CF3)2P (2), Me2N(CF3)P (3), Me2P (4), (CF3)2As (5), Me2As (6)]. The analogous reaction of ib with CF3PI2 (molar ratio 1:2) unexpectedly leads to the triphosphetene Et2N - C=P-PCF3-PCF3 (7). The stability of compounds 2 - 6 as a function of R2E decreases from As to P and from CF3 to Me, respectively. Compounds 2 - 6 generally show the Z-configuration and have been characterized by thorough spectroscopic investigations (MS,IR; 1H, 19F, 11C, 31PNMR). A single crystal X-ray diffraction study of 2 proves the π-type interaction of the nitrogen lone pair with the P=C bond thus enhancing the stability of the system and the PP bond order

Carcinogenicity of lactones. II. x-Ray crystal structure analyses of ± 3-benzylamino-4-hydroxypentanoic acid lactone hydrochloride and hydrobromide

1968 ◽  
Vol 46 (5) ◽  
pp. 813-814 ◽  
Author(s):  
J. Bryan Jones ◽  
Chung Hoe Koo ◽  
Ian P. Mellor ◽  
S. C. Nyburg ◽  
John M. Young
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Structure Analysis ◽  
Crystal Structure Analysis ◽  
Optically Active ◽  
Spontaneous Resolution ◽  
X Ray ◽  
Acid Lactone

X-Ray crystal structure analysis of the hydrochloride of ± 3-benzylamino-4-hydroxypentanoic acid lactone shows the methyl and benzylamino groups to be trans-oriented.The hydrobromide is not isomorphous with the hydrochloride and its crystals are optically active owing to spontaneous resolution during crystallization. Refinement of both crystal structures is in progress.

Sign in / Sign up

Export Citation Format

Share Document