Crystal and molecular structure of 8-acetamido-2,4,4,8-tetramethyl-3-azaniumbicyclo[3.3.1]non-2-ene perchlorate

1987 ◽  
Vol 65 (9) ◽  
pp. 2000-2003 ◽  
Author(s):  
H. R. Viturro ◽  
B. E. Rivero ◽  
O. E. Piro ◽  
J. A. Caram ◽  
M. E. Martins ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Crystal And Molecular Structure ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Iminium Salt ◽  
Carbonium Ion ◽  
Single Crystal Analysis

X-ray single crystal analysis sheds further light on the structure of this new iminium salt. ATABNEP crystallizes in the monoclinic system, space group P21 and shows a very short value for the C—N distance in the iminium group, thus suggesting that the contribution of the carbonium ion form in this particular case is much lower than usual, a fact that can be considered a rationale for the reluctance of ATABNEP to undergo hydrolysis.

Dodecamethyl Bisimidotriphosphoramide (TRIPA), Part III [1, 2] The Crystal and Molecular Structure of TRIPA · H2O

1980 ◽  
Vol 35 (10) ◽  
pp. 1203-1206 ◽  
Author(s):  
Johannes C. P. M. Lapidaire ◽  
Anthoni J. De Kok
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Crystal And Molecular Structure ◽  
Van Der Waals ◽  
Water Molecules ◽  
X Ray Diffraction ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray

Abstract The crystal and molecular structure of dodecamethyl bisimidotriphosphoramide mono-hydrate (TRIPA • H2O, C12H38N7O4P3) has been determined by single crystal X-ray diffraction techniques. The compound crystallises in the monoclinic system, space group P2i/n with a = 9.236(3), b = 14.016(4), c = 17.534(5) A, β = 97.32(4)°, Z = 4. The building units are dimers of TRIPA • H2O. These units are separated by normal van der Waals distances. The two molecules in the dimer are connected by four hydrogen bridges involving two water molecules. The nitrogen atoms display a nearly planar hybridisation.

5-Allyl-9-oxobenzomorphans. Part 2. The Crystal and Molecular Structure of an Unusual Product of Dequaternization of 5-Allyl-9-oxobenzomorphan Methobromide

1975 ◽  
Vol 53 (21) ◽  
pp. 3276-3284 ◽  
Author(s):  
Farid R. Ahmed ◽  
Michel Saucier ◽  
Ivo Monković
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Heavy Atom ◽  
Methoxy Derivative ◽  
X Ray ◽  
Unusual Product ◽  
Single Crystal Analysis

The synthesis of 5-allyl-2'-methoxy-9-oxo-6,7-benzomorphan (5b) is described. The 10-hydroxy-2-methyl-1,11-propano-9H-indeno-1,2,10,11-tetrahydro[2,1-c]pyridine (7a) and the corresponding 6-methoxy derivative (7b) are unexpected products of pyrolysis of 5-allyl-2-methyl-9-oxobenzomorphan methobromide (4a) and 5-allyl-2′-methoxy-2-methyl-9-oxobenzomorphan methobromide (4b) respectively. The molecular structure of 7a (C16H19NO) has been determined from spectral and microanalytical data, and confirmed by X-ray single crystal analysis on its hydrobromide salt using the heavy atom technique. The crystals of [C16H20NO]+Br− are monoclinic, P21/a, with a = 13.724(2), b = 14.022(3), c = 7.495(2) Å, β = 97.33(5)°, and Z = 4. The crystal structure has been refined by block-diagonal least-squares calculations to R and Rw = 0.036 for the 2197 observed reflections. The N atom has planar trigonal coordination, and forms one double and two single C—N bonds of lengths 1.273(4), 1.465(4), and 1.474(4) Å, respectively. The Br is hydrogen-bonded to O. The N and O atoms are trans.

The Crystal and Molecular Structure of Chloro-mer-Tris(dimethylphenylphosphine)-cis-dihydridoiridium(III) by X-Ray and Neutron Diffraction

1988 ◽  
Vol 41 (5) ◽  
pp. 641 ◽  
Author(s):  
GB Robertson ◽  
PA Tucker
Keyword(s):  
Molecular Structure ◽  
Neutron Diffraction ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Neutron Data ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The structure of mer-(Pme2Ph)3Cl-cis-H2IrIII (1) has been determined by single-crystal X-ray and neutron diffraction analyses. Crystals are monoclinic, space group P21, with a 11.476(4), b 14.069(5), c 8.286(3)Ǻ, β 92.45(1)° and Z 2. Full-matrix least-squares analyses converged 0.022 for 7773 X-ray data and R(F2) = 0.062 for 1538 neutron data. Ir -H [1.557(11)Ǻ trans to Cl, 1.603(10) Ǻ trans to P] and Ir -P distances [2.292(1)Ǻ trans to P, 2.328(1)Ǻ trans to H] both exhibit trans lengthening effects. Consistent with the increased hydride content the Ir -P distances in (1) are c. 0.04 Ǻ shorter than for the corresponding bonds in its dichloro monohydrido analogues and c. 0.08 Ǻ shorter than those in the trichloride . In contrast Ir-Cl [2.505(1)Ǻ] is not significantly different to the corresponding distance (2.504 Ǻ av.) in mer -(PMe2Ph)3-cis-Cl2HIrIII.

The crystal and molecular structure of aqua-bis(ethylenediamine)cupric-tris(cyano)-selenocyanatodicuprate

1982 ◽  
Vol 47 (10) ◽  
pp. 2623-2632 ◽  
Author(s):  
Viktor Vrábel ◽  
Jan Lokaj ◽  
Ján Garaj ◽  
František Pavelčík
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structural Analysis ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Triclinic System

The crystal structure of [Cu(H2O)(en)2][Cu2(CN)3(SeCN)] was solved by single crystal X-ray structural analysis in the triclinic system with a space group of P1 and in the monoclinic system with a space group of C2. In the triclinic system the unit cell has dimensions of a = 0.8445(3), b = 0.7903(3), c = 0.8444(3) nm, α = 119.58(2), β = 118.59(2) and γ = 93.63(3)° and, in the monoclinic system, a = 1.3331(4), b = 0.8670(2), c = 0.8267(3), β = 122.60(2)°. The structure was refined by the least squares method to final value of R = 5.5% in the triclinic system and R = 7.8% in the monoclinic system. The coordination sphere around the Cu(II) atom is square pyramidal, formed of two ethylenediamine molecules and one water molecule. The Cu(I) atoms are tetrahedrally coordinated by bridging SeCN and CN ligands to form infinite three-dimensional chains. The SeCN group is bonded to the Cu(I) atoms through the Se atom at distances of 0.2731(3) and 0.2745(3) nm.

Adiponitrile at 100 K

2017 ◽  
Vol 73 (11) ◽  
pp. 937-940 ◽  
Author(s):  
Rüdiger W. Seidel ◽  
Richard Goddard ◽  
Nils Nöthling ◽  
Christian W. Lehmann
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Low Temperature ◽  
Single Crystal ◽  
Large Scale ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Intermolecular Contacts

Adiponitrile, C6H8N2, is a key intermediate in the synthesis of the polyamide Nylon 66 and is produced industrially on a large scale. We have determined the crystal and molecular structure of adiponitrile by single-crystal X-ray analysis at 100 K, a suitable crystal (m.p. 275 K) having been grown from the melt at low temperature. The compound crystallizes in the monoclinic space group P21/c with Z = 2. In the crystal structure, the molecule adopts an exact C i-symmetric gauche–anti–gauche conformation of the C—C—C—C skeleton about an inversion centre. The molecules are densely packed, with short intermolecular contacts between the α-H and nitrile N atoms.

Investigation of Isomer Formation of Triorganotin(IV) Complexes Involving Diorganophosphino-N-Phenyl(Thioformamide) Ligands: The Crystal and Molecular-Structure of [Diphenylphosphino-N-Phenyl(Thioformamido)]Triphenyltin, Ph3Sn[Ph2PC(S) NPh ]

1988 ◽  
Vol 41 (2) ◽  
pp. 195 ◽  
Author(s):  
D Dakternieks ◽  
BF Hoskins ◽  
CL Rolls
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Sulfur Atom ◽  
Crystal And Molecular Structure ◽  
Steric Effects ◽  
X Ray Diffraction ◽  
Similar Compound ◽  
Space Group ◽  
X Ray ◽  
Tetrahedral Environment

The isomer of Ph3Sn[Ph2PC(S) NPh] formed depends on the method of preparation. The crystal and molecular structure of the tin(IV) complex Ph3Sn[Ph2PC(S) NPh ] has been established by single-crystal X-ray diffraction techniques. The crystals are monolinic, space group P21/n, a 12.620(2), b 10.541(2), c 24.292(4)Ǻ, β 96.90(1) with Z 4; R and Rw were 0.031 and 0.034 respectively for 5632 unique reflections with I > 3σ(I). The crystals consist of discrete Ph3Sn[Ph2PC(S) NPh ] molecules. There is a tetrahedral environment about the tin atom formed by the three phenylic carbons and a sulfur atom of the [Ph2PC(S) NPh ]- ligand . Comparisons are made with the structurally similar compound Ph3Sn[(c-C6H11)2PC(S) NPh ]. On the basis of these comparisons and on earlier n.m.r . data, a favoured four-centered mechanism for insertion of dipolar PhNCS into the tin-phosphorus bond of Ph3SnPPh2 is inferred. Differences in reactivity of Ph2PC(S)N(H)Ph and (c-C6H11)2PC(S)N(H)Ph appear to result from electronic rather than steric effects.

The crystal and molecular structure of (±)-('E')-N-Acetylpiperidine-2-carboxylic acid

1980 ◽  
Vol 33 (1) ◽  
pp. 215 ◽  
Author(s):  
ID Rae ◽  
CL Raston ◽  
AH White
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Carboxylic Acid ◽  
Single Crystal ◽  
Least Squares ◽  
Crystal And Molecular Structure ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

The crystal structure of N-acetylpiperidine-2-carboxylic acid has been determined by single-crystal X-ray diffraction methods at 295(1) K and refined by least squares to a residual of 0.039 for 846 'observed' reflections. Crystals are orthorhombic, with space group Pbca, a 13.684(6), b 11.602(4), c 11.171(4)Ǻ, Z 8. The ring is a chair structure in which, contrary to an earlier proposal based on 1H n.m.r. studies, there is almost perfect staggering about the C(2)-C(3) bond.

Diazadien-Nickel-Komplexe, I: Bis(diazadien)-nickel(O) und Bromo-diazadien-nickel(I) / Diazadiene Nickel Complexes, I: Bis(diazadiene) Nickel(O) and Bromo-diazadiene Nickel(I)

1978 ◽  
Vol 33 (12) ◽  
pp. 1381-1385 ◽  
Author(s):  
Heindirk tom Dieck ◽  
Michael Svoboda ◽  
Jürgen Kopf
Keyword(s):  
Molecular Structure ◽  
Single Crystal ◽  
Crystal And Molecular Structure ◽  
Nickel Complexes ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray

Abstract Reduction of anhydrous nickel(II) compounds in the presence of diazadienes RN=CR'-CR' = NR, |(DAD), yields (DAD)2Ni(0). This complex 1 with R = CH(i-C3H7)2 is especially reactive and comproportionates with DADNiBr2 (2) to yield the bromobridged dimeric nickel(I) species (DADNiBr)2 (3). The crystal and molecular structure of 3 has been determined by single crystal X-ray diffraction: Space group Pbca with a = 1225.8(12), b = 1474.8(14) and c = 2167.4(22) pm; Ra = 0.076, 1034 reflections. Catalytic tetramerisation of substituted alkynes with 1 is discussed in view of the very easy formation of dimers 3.

Synthesis and molecular structure of tetraphenylarsonium Tetrakis(benzenethiolato)-oxorhenate(V)-Acetonitrile (1/1)

1983 ◽  
Vol 36 (2) ◽  
pp. 253 ◽  
Author(s):  
AC McDonell ◽  
TW Hambley ◽  
MR Snow ◽  
AG Wedd
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Crystal Data ◽  
Rhenium Atom ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography

The salts Ph4As [ReO(SPh)4].MeCN and Ph4As [ReO(SePh)4] have been synthesized and characterized. The crystal and molecular structure of the thiolate compound has been determined by X-ray crystallography which reveals a square-pyramidal arrangement of ligand atoms around the central rhenium atom of the [ReO(SPh)4]- anion. Crystal data: a 9.756(4), b 18.171(3), c 25.684(4) �, space group P212121, Z 4.

Crystal Structure of (NH4)2[Mo3S(S2)6] Containing the Novel Isolated Cluster [MO3S13]2-

1979 ◽  
Vol 34 (3) ◽  
pp. 434-436 ◽  
Author(s):  
A. Müller ◽  
S. Pohl ◽  
M. Dartmann ◽  
J. P. Cohen ◽  
J. M. Bennett ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Aqueous Solutions ◽  
Single Crystal ◽  
Ammonium Salt ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
The Novel ◽  
Mean Values ◽  
X Ray

Abstract The novel tri-nuclear metal-sulfur cluster [Mo3S(S2)6]2- can be obtained as its ammonium salt by the reaction of a Moiv containing aqueous solutions with polysulfide. Its crystal and molecular structure has been determined by a single crystal X-ray study. The crystals are monoclinic (space group Cm, with a = 11.577(6) Å, b = 16.448(7) Å, c = 5.716(2) Å, β = 117.30(3)°, V = 967.2 Å3 , Z = 2, dexptl. = 2.54(2) g/cm3 , dcal = 2.54 g/cm3). The structure consists of isolated [Mo3S(S2)6]2- units, with three Mo atoms at the vertices of a triangle. There are bridging as well as terminal S22--ligands lying above and below the Mo3-plane (bond distances: Mo-Mo = 2.722 Å, Mo-S(terminal) = 2.435, Mo-S(bridging) = 2.452, Mo3-S = 2.353(4) Å and S-S = 2.04 Å (mean values)).

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