Synthesis and Structure of (1,8-Diammonio-3,6,10,13,16,19-hexaazabicyclo[6.6.6]icosane)-nickel(II) Tetrachloride Monohydrate

1993 ◽  
Vol 46 (1) ◽  
pp. 127 ◽  
Author(s):  
LM Engelhardt ◽  
JM Harrowfield ◽  
AM Sargeson ◽  
AH White
Keyword(s):  
Hydrogen Bonding ◽  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Narrow Range ◽  
Crystal Packing ◽  
The Other ◽  
X Ray ◽  
The Mean

The synthesis and single-crystal X-ray structure determination of the title compound are described. Crystals are monoclinic, P 21, a 16.164(9), b 8.277(3), c 8.829(4) Ǻ, β 102.86(4)°, Z 2; 2666 independent 'observed' diffractometer data [I > 3σ(I)] were refined to a residual of 0.045. The cation is unusual amongst complexes of sarcophagine (3,6,10,13,16,19-hexaazabicyclo[6.6.6]icosane) cage amines in adopting a lel2ob conformation, seemingly in response to hydrogen bonding/crystal packing forces. In consequence, unlike the tetranitrate analogue in which Ni-N bond distances are dispersed over a narrow range (2.097(5)-2.119(5) Ǻ; mean 2.109 Ǻ], the coordination sphere is more distorted with one pair of Ni-N distances, cis to each other, being short at 2.081(5) and 2.086(5) Ǻ, while the other four are long, ranging from 2.116(5) to 2.135(5) Ǻ, the mean of this array being 2.111 Ǻ.

Approaches to the total synthesis of triterpenes. VIII. The ABC + D/E approach. Synthesis and X-ray structure determination of 1β,4a β-dimethyl-7-methoxy-1α- (7′,7′-ethyleneketal-6′,6′-dimethyl-3′-ketooctyl)-3,4,4a,9,10,10aα-hexahydro- 2(l-H)phenanthrone

1982 ◽  
Vol 60 (4) ◽  
pp. 509-513 ◽  
Author(s):  
John W. ApSimon ◽  
Rick P. Sequin ◽  
Carol P. Huber
Keyword(s):  
Total Synthesis ◽  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Trimethylsilyl Ether ◽  
Synthetic Route ◽  
X Ray ◽  
Pentacyclic Triterpenes ◽  
Ongoing Work

The title compound was made following a projected synthetic route to pentacyclic triterpenes. The key step in the route is the alkylative trapping of the enolate derived from the enol trimethylsilyl ether 8. The stereochemical consequence of this reaction is confirmed by a single crystal X-ray structure determination on 4, which although of no further utility in the projected synthesis, nevertheless served as a useful template for this determination. In this way, ongoing work in a parallel series of compounds rests on a firm stereochemical footing.

Lewis-Base Adducts of Lead(II) Compounds. III. Synthesis and Structural Characterization of Mononuclear (Nitrato-O,O′)bis(1,10-phenanthroline)-(thiocyanato-N)lead(II)

1989 ◽  
Vol 42 (2) ◽  
pp. 335 ◽  
Author(s):  
LM Engelhardt ◽  
JM Patrick ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Title Compound ◽  
Lone Pair ◽  
Lewis Base ◽  
Lead Atom ◽  
X Ray

The isolation and single-crystal X-ray structure determination of the title compound, [(phen)2Pb(NCS)(O2NO)] is described; crystals are triclinic, P1, a 15.554(7), b 9-670(4), c 8.429(3) α 72.53(3), β 81.90(3), γ 72.88(3)� Z = 2, yielding R 0.052 for 3405 independent 'observed' reflections. The lead atom is seven-coordinate [Pb-N 2.49(1)-2.60(1) (phen), 2.89(1) (NCS); Pb-O 2.75(1), 2.89(1) �] with a large vacancy in the coordination sphere, possibly indicative of a stereochemically active lone pair.

scholarly journals Synthese und Strukturanalyse des gemischten Alkalimetallorthonitrats Na3K3(NO4)2 / Synthesis and X-Ray Structure Determination of the Mixed Alkali Metal Orthonitrate Na3K3(NO4)2

1991 ◽  
Vol 46 (8) ◽  
pp. 1031-1034 ◽  
Author(s):  
Thomas Bremm ◽  
Martin Jansen
Keyword(s):  
Alkali Metal ◽  
Single Crystal ◽  
Vibrational Spectra ◽  
Structure Determination ◽  
Title Compound ◽  
Single Crystal Diffraction ◽  
Tetrahedral Geometry ◽  
X Ray ◽  
Mixed Alkali

The title compound has been characterized by X-ray powder and single crystal diffraction: Pbcn; a = 7.296(1), b = 15.997(4), c = 7.016(1) Å; Z = 4; 1514 diffractometer data, R = 0.04, Rw = 0.03. The vibrational spectra are compatible with a tetrahedral geometry of the anion.

Synthesis and Single Crystal Structure Determination of Bis(carbido)bis(μ-diphenylphosphido)heptadecacarbonyloctaruthenium-Dichloromethane (1/1), Ru8(μ6-C)(μ5-C)(μ-PPh2)2(CO)17.CH2Cl2

1993 ◽  
Vol 46 (11) ◽  
pp. 1811 ◽  
Author(s):  
CJ Adams ◽  
MI Bruce ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
Room Temperature ◽  
Single Crystal Structure ◽  
Crystal Structure Determination ◽  
Triangular Face ◽  
X Ray

The synthesis and room-temperature single-crystal X-ray structure determination of the title compound are recorded. Crystals are monoclinic, P 21/c, a 14.43(2), b 18.39(1), c 23.64(3) Ǻ, β 123.16(7)°, Z = 4, isostructural with the recently described Fe3Ru5 analogue; R was 0.048 for 6892 'observed' data [I > 3σ(I)]. The cluster is one of the few containing separated carbide ligands within a polyhedral metal skeleton, consisting of an Ru5C square pyramid and an Ru6C octahedron sharing a triangular face, with two PPh2 groups bridging opposite Ru-Ru vectors in each polyhedron.

The Crystal and Molecular structure of trans-Dichlorobis(1,3-Diaminopropan-2-ol)cobalt(III) Chloride

1987 ◽  
Vol 40 (10) ◽  
pp. 1763
Author(s):  
R Kivekas ◽  
MR Sundberg
Keyword(s):  
Molecular Structure ◽  
Hydrogen Bonding ◽  
Coordination Sphere ◽  
Structure Determination ◽  
Title Compound ◽  
Crystal And Molecular Structure ◽  
Chloride Ions ◽  
X Ray ◽  
R Value

A single-crystal X-ray structure determination of the title compound is reported. The compound crystallizes in the space group P1 with a 7.273(1), b 8.525(2), c 12.358(3) �, α 80.03(3),β 75.38(2), γ 65.06(2)� and Z 2. The final R value for 3318 reflections was 0.041. The structure consists of two independent trans- dichlorobis (l,3-diaminopropan-2-ol)cobalt(III) cations and chloride ions interconnected by a hydrogen bonding network. The axial Co-Cl bonds in the pseudo-octahedral coordination sphere are shorter than those in the coordination sphere of the copper(II) analogue. The compression is clearly related to the simultaneous flattening of the rings.

Coordination Chemistry of the Calixarenes. II. Europium(III) and p-t-Butyl Calix[6]arene

1988 ◽  
Vol 41 (9) ◽  
pp. 1465 ◽  
Author(s):  
LM Engelhardt ◽  
BM Furphy ◽  
JM Harrowfield ◽  
DL Kepert ◽  
AH White ◽  
...  
Keyword(s):  
Coordination Chemistry ◽  
Single Crystal ◽  
Structure Determination ◽  
The Other ◽  
Arene Complexes ◽  
X Ray ◽  
Ligand Ratio ◽  
Lanthanide Elements ◽  
Europium Atom

The possible nature of p-t-butyl-calix [6] arene complexes of lanthanide elements has been explored by determination of the single-crystal X-ray structure of a complex with a 1:2 europium/ ligand ratio, obtained from dimethylformamide (dmf ≡ Me2NCHO) solution. This complex is formulated as [ Eu (LH4)(Me2NCHO)6(OH)].LH6.~4Me2NCHO (LH6 = p-t-butyl-calix [6] arene) on the basis of the structure determination. Crystals are monoclinic, P21/n, a 36.11(3), b 23.35(2), c 21.85(2)Ǻ, β 97.46(6)°, Z = 4 formula units; R was 0.11 for 8488 'observed' reflections. The complex is remarkable in that the only interaction of either of the two calixarene ligands (one presumably doubly or triply deprotonated ) with the eight-coordinate europium atom is by way of one behaving as monodentate, the other having no interaction. Eu -O( calix ) is 2.35(1) Ǻ; Eu -O( dmf )6 range from 2.38(2) to 2.49(2)Ǻ, and Eu -O(H ½?) is 2.49(2)Ǻ.

Synthesis and X-Ray Structural Characterization of the 1:1 Adduct of Bismuth(III) With the 'saltren' Anion ['saltren' ≡ N(CH2CH2N=CHC6H4OH)3]: A Novel Seven-Coordinate Bismuth(III) Complex

1994 ◽  
Vol 47 (9) ◽  
pp. 1799 ◽  
Author(s):  
PK Bharadwaj ◽  
AM Lee ◽  
S Mandal ◽  
BW Skelton ◽  
AH White
Keyword(s):  
Single Crystal ◽  
Structural Characterization ◽  
Structure Determination ◽  
Title Compound ◽  
X Ray

The synthesis and single-crystal X-ray structure determination of the title compound are recorded; crystals are monoclinic, P 21/c, a 10.309(8), b 18.817(7), c 15.542(6) Ǻ, β 121.80(5)°, Z 4; R was 0.038 for 2894 independent, 'observed' [I > 3σ(I)] reflections. The molecule has quasi-3 symmetry, with seven-coordinate bismuth [Bi-N(apical), 2.82(1); Bi-N, 2.512(8)-2.563(9); Bi-O, 2.197(8)-2.300(8)Ǻ].

Crystal structure of panduratin A: (1'RS,2'SR,6'RS)-(2,6-Dihydroxy-4-methoxyphenyl)[3''-methyl-2'-(3'-methylbut-2'-enyl)-6'-phenylcyclohex-3'-enyl]methanone

1984 ◽  
Vol 37 (12) ◽  
pp. 2589 ◽  
Author(s):  
O Pancharoen ◽  
V Reutrakul ◽  
BW Skelton ◽  
WC Taylor ◽  
P Tuntiwachwuttikul ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Structure Determination ◽  
Title Compound ◽  
X Ray ◽  
Panduratin A

Single-crystal X-ray structure determination of the title compound, C26H30O4, confirms the stoichiometry, connectivity and stereochemistry recently assigned spectroscopically. Crystals are monoclinic, P21/n, a 10.140(5), b 24.85(1), c 9.4134) � β 90.69(4)�,Z 4; the structure was refined to a residual of 0.055 for 1701 'observed' independent reflections.

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