Phenylimido complexes of tungsten(VI) and tungsten(V). The crystal and molecular structure of Trichloro(phenylimido)bis(trimethylphosphine)tungsten(V)

1983 ◽  
Vol 36 (2) ◽  
pp. 243 ◽  
Author(s):  
AJ Nielson ◽  
JM Waters

Tetrachloro(phenylimido)tungsten(VI) is reduced by trimethylphosphine in tetrahydrofuran solution to give the tungsten(V) complex PhNWCl3(Pme3)2 in which the phenylimido multiple bond remains intact. The complex reacts with oxygen to form the phosphine oxide complex PhNWCl3 (OPMe3)2. Pyridine and alkyl cyanides do not reduce tetrachloro(phenylimido)tungsten(V1) but give the adducts PhNWCl4.L (L = py, MeCN, EtCN). The crystal and molecular structure of the title complex has been determined from single-crystal X-ray diffractometer data. The crystals are monoclinic with a 14.903, b 10.221, c 14.380Š β 116.05�, space group P21/c, Z 4. The structure has been solved by Patterson and Fourier methods and refined to R 0.030 for the 1566 observed data. Distorted octahedral coordination geometry is found with two trans trimethylphosphine and two trans chloride ligands; a third chloride is trans to the phenylimido group. The W-N(imido) bond length is 1.731 �.


1991 ◽  
Vol 69 (3) ◽  
pp. 391-396 ◽  
Author(s):  
H. Willner ◽  
S. J. Rettig ◽  
J. Trotter ◽  
F. Aubke

Single crystals of gold(III) tris(fluorosulfate) are obtained by recrystallization from bis(fluorosulfuryl) peroxide, S2O6F2, under O2 pressure. The crystals of [Au(SO3F)3]2 are monoclinic, a = 9.700(4), b = 9.222(2), c = 10.810(4)Å, β = 94.43(3)°, Z = 2, space group P21/a. The structure was solved by heavy atom methods and was refined by full-matrix least-squares procedures, R(F) = 0.038 and Rw(F) = 0.050 for 1491 reflections with I ≥ 3σ(I). The structure consists of centrosymmetric [Au(SO3F)3]2 dimers containing two bidentate, symmetrically bridging and four monodentate, terminal SO3F ligands. The Au(III) ions have square-planar coordination geometry with bridging Au—O = 2.020(7) and 2.016(6) Å, and terminal Au—O = 1.959(7) and 1.956(9) Å. The dimeric [Au(SO3F)3]2 units are linked in the solid state by weak Au—O interactions (2.757(8) and 2.960(7) Å), resulting in a distorted octahedral coordination geometry about each gold atom. Key words: gold(III) tris(fluorosulfate), crystal structure.



1978 ◽  
Vol 56 (3) ◽  
pp. 267-272 ◽  
Author(s):  
Ei-Ichiro Ochiai ◽  
Steven J. Rettig ◽  
James Trotter

Crystals of bis(perchlorato) (γ-C-meso-5,5,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane)copper(II) are monoclinic, a = 14.061(1), b = 8.908(1), c = 19.710(1) Å, β = 90.912(5)°, Z = 4, space group P21/c. The structure was solved by Patterson and Fourier syntheses and was refined by full-matrix least-squares procedures to a final R of 0.054 and Rw of 0.069 for 2945 reflections with I ≥ 3σ(I). The copper(II) ion has tetragonally distorted octahedral coordination geometry. The four nitrogen atoms of the macrocyclic ligand occupy the equatorial sites and two perchlorate oxygen atoms are in the axial positions. Bond lengths (corrected for libration) are: Cu—N, 2.024(4)–2.051(4), Cu—O, 2.657(5) and 2.697(5), Cl—O, 1.420(4)–1.473(6), N—C, 1.463(6)–1.508(6), and C—C, 1.498(8)–1.542(8) Å.



1982 ◽  
Vol 35 (6) ◽  
pp. 1105 ◽  
Author(s):  
KR Morgan ◽  
GJ Gainsford ◽  
NF Curtis

The diperchlorate salts of the mono(β-amino ketone) 10-amino-4,4-dimethyl-5,8-diazadecan-2-one and of the bis(β-amino ketone) 4,4,12,12-tetramethyl-5,8,11-triazapentadecane-2,14-dione, ttp, have been prepared by reaction of the diperchlorate of 3-azapentane-1,5-diamine with acetone. The salt [ttpH2] (ClO4)2 has been used to prepare the six-coordinate complexes [Cu(ttp)(H2O)] (ClO4)2,1.5H2O and [Ni(ttp)(H2O)] (ClO4)2,H2O, and the five-coordinate [Cu(ttp)] (CIO,),. The complex [Cu(ttp)] (ClO4), reacts with ammonia, methylamine and ethylamine to form complexes of pentadentate β-amino ketone β-amino imine ligands. The structure of [Co(ttp)(H2O)] (ClO4)2,1.5H2O has been determined by X-ray diffractometry [space group P21/c, Z 4, a 797.5(2), b 1632.8(3), c 2236.4(3) pm, β 97.504(2)�, R 0.0749, Rw 0.0765 for 1678 reflections]. The complex cation has the bis(β-amino ketone) ttp acting as a pentadentate ligand, with the three nitrogen and one carbonyl oxygen atoms coplanar, and with oxygen of a water molecule completing distorted octahedral coordination about the cobalt(II) ion.



2013 ◽  
Vol 69 (11) ◽  
pp. m590-m590
Author(s):  
Kaijun Luo ◽  
Chenyang Zhang ◽  
Juan Jia ◽  
Daibing Luo

The title compound, [Ir(C10H5F2N2)2(C5H7O2)], has a distorted octahedral coordination geometry around the IrIIIatom, retaining thecis-C,C/trans-N,Nchelate disposition in two 2,6-difluoro-3-(pyridin-2-yl-κN)pyridin-4-yl ligands which are nearly mutually perpendicular [dihedral angle = 82.75 (15)°]. The molecular structure is stabilized by weak C—H...O and C—H...F hydrogen-bond interactions. The crystal structure is stabilized by π–π stacking interactions (centroid–centroid distance = 3.951 Å).



2009 ◽  
Vol 2009 ◽  
pp. 1-5 ◽  
Author(s):  
Awni Khatib ◽  
Fathi Aqra ◽  
David Deamer ◽  
Allen Oliver

The title complex, [Ni, has been prepared from nickel(II) chloride in aqueous solution by adding L-alanine and potassium hydroxide. It has been crystallized from aqueous solution, and its structure was determined by X-ray structure analysis. The nickel(II) ion adopts distorted octahedral coordination geometry with two bidentate L-alanine molecules and two water molecules. The complex is neutral and dihydrated. The crystal structure shows the hydrogen bonding between water and amide hydrogens within the lattice, and each fragment of the complex contains two water molecules as hydrated water. The L-alaninato ligand skeleton of the compound adopts the most stable trans-III configuration in the solid state. The alternating two five-membered chelate rings are in the stable gauche conformation.



Author(s):  
Khatib Awni ◽  
Fatbi Aqrn ◽  
David Deamer ◽  
Allen Oliver

The title complex of formula [Ni(NH2CH3CHCOO)2(H20)2].2H2O has been prepared from nickel(II) chloride in an aqueous solution by adding D-alanine and potassium hydroxide. It has beett crystallized from an aqueous solution and its structure was determined by X-ray structure analysis. The nickel(II) atom adopts distorted octahedral coordination geometry with two bidentate alanine molecules and two water molecules. The complex is neutral and dihydrated. The network crystal structure shows hydrogen bonding between water and amide hydrogens within the lattice, and each fragment of the complex contains two water molecules as hydrated water.



2015 ◽  
Vol 71 (9) ◽  
pp. m162-m163
Author(s):  
Siddhartha S. Baisya ◽  
Baidyanath Ghosh ◽  
Parag S. Roy

In the title compound, [Zn(C8H5N5O3)(C12H8N2)(H2O)]·3H2O, a tridentate 2-amino-7-methyl-4-oxidopteridine-6-carboxylate ligand, a bidentate ancillary 1,10-phenanthroline (phen) ligand and a water molecule complete a distorted octahedral coordination geometry around the ZnIIatom. The pterin ligand forms two chelate rings. The phen and pterin ring systems are nearly perpendicular [dihedral angle = 85.16 (5)°]. Classical N—H...O, O—H...N and O—H...O hydrogen bonds and weak C—H...O hydrogen bonds link the complex molecules and lattice water molecules into a three-dimensional network. π–π stacking contacts are observed as well, with centroid-to-centroid distances of 3.5679 (14), 3.7004 (14), 3.6641 (15), 3.6974 (13) and 3.3412 (12) Å.



2007 ◽  
Vol 63 (11) ◽  
pp. m2722-m2722 ◽  
Author(s):  
Ying Liu ◽  
Jianmin Dou ◽  
Dacheng Li ◽  
Xianxi Zhang

The dinuclear FeIII complex in the title compound, [Fe2Cl2O(C18H18N4)2](PF6)2, lies on a center of inversion. The FeIII atom is chelated by a tetradentate tris(2-pyridylmethyl)amine ligand via four N atoms and further coordinated by one chloride ion and one bridging oxide O atom, giving a distorted octahedral coordination geometry.



2007 ◽  
Vol 63 (3) ◽  
pp. m845-m846 ◽  
Author(s):  
Ying-Ju Fan ◽  
Le Wang ◽  
Jian-Ping Ma ◽  
Zhong-Xi Sun

Reaction of indium(III) chloride with (E)-1-[1-(2-pyridyl)ethylidene]thiosemicarbazide afforded the title complex, [In(C8H9N4S)Cl2(C2H5OH)]. The ligand is in the enol form coordinating to the InIII atom through one S atom and two N atoms. The InIII atom is further coordinated by two Cl atoms and an ethanol molecule to complete a distorted octahedral coordination geometry.



2007 ◽  
Vol 63 (3) ◽  
pp. m856-m856 ◽  
Author(s):  
William Clegg ◽  
Nicola C. Martin

The title compound, [CoCl2(C6H7N)2(C2H6O)2], was obtained unintentionally as the product of an attempted synthesis of a polycarboxylate-bridged network complex of cobalt(II) using aniline as a base to deprotonate the organic acid. The molecule is centrosymmetric, so pairs of equivalent ligands lie trans to each other in a slightly distorted octahedral coordination geometry. Molecules are linked by O—H...Cl and N—H...Cl hydrogen bonds involving all the potential donors, generating sheets parallel to (001). The phenyl rings protrude on both sides of these sheets and have normal hydrophobic contacts with each other, involving no intercalation or stacking interactions.



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