Cyclopalladation of trimesitylarsine. The X-ray crystal structure for

1988 ◽  
Vol 66 (12) ◽  
pp. 3162-3165 ◽  
Author(s):  
Elmer C. Alyea ◽  
George Ferguson ◽  
John Malito ◽  
Barbara L. Ruhl
Keyword(s):  
Crystal Structure ◽  
Cleavage Product ◽  
Phosphine Ligands ◽  
Monoclinic Space Group ◽  
Dimeric Complex ◽  
Tertiary Phosphine ◽  
X Ray ◽  
H Nmr ◽  
Square Planar ◽  
Cleavage Reactions

The bulky trimesitylarsine ligand, As(mes)3, undergoes facile cyclopalladation to yield the dimeric complex, [Formula: see text], characterized by microanalysis, IR and 1H NMR spectroscopy. This complex is very stable but readily undergoes bridge-cleavage reactions with tertiary phosphine ligands having ligand cone angles less than 170°. The crystal structure for the PPh3 bridge-cleavage product is reported. This complex, [Formula: see text] is monoclinic, space group P21/c with a = 20.469(2), b = 12.702(2), c = 15.401(4) Å, β = 98.46(1)°, V = 3961 Å3Z = 4, R = 0.0284 and Rw = 0.0305. The Pd geometry is distorted square-planar with principal dimensions, Pd—Cl 2.395(1), Pd—P 2.318(1), Pd—C 2.056(3), and Pd—As 2.437(1) Å; As—Pd—Cl 96.5(1), Cl—Pd—P 90.9(1), P—Pd—C 93.7(1), As—Pd—C 78.9(1), As—Pd—P 172.6(1), and Cl—Pd—C 171.7(1)°. The average C—P—C angle (104.3(1)°) is smaller than expected and is rationalized on the basis of steric effects operative within the complex.

Preparation and characterization of some ruthenium(II) porphyrins containing tertiary phosphine axial ligands, including the crystal structure of (octaethylporphinato)bis(triphenylphosphine)ruthenium(II)

1984 ◽  
Vol 62 (4) ◽  
pp. 755-762 ◽  
Author(s):  
Sara Ariel ◽  
David Dolphin ◽  
George Domazetis ◽  
Brian R. James ◽  
Tak W. Leung ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Phosphine Ligands ◽  
Tertiary Phosphine ◽  
X Ray ◽  
Porphyrin Complex ◽  
H Nmr ◽  
Axial Ligands ◽  
Nmr Data ◽  
Phosphine Complex

The ruthenium(II) porphyrin complex Ru(OEP)(PPh3)2 (OEP = the dianion of octaethylporphyrin) has been prepared from Ru(OEP)(CO)EtOH, and the X-ray crystal structure determined; as expected, the six-coordinate ruthenium is situated in the porphyrin plane and has two axial phosphine ligands. Synthesized also from the carbonyl(ethanol) precursors were the corresponding tris(p-methoxyphenyl)phosphine complex, and the Ru(TPP)L2 (TPP = the dianion of tetraphenylporphyrin, L = PPh3, P(p-CH3OC6H4)3, P″Bu3) and Ru(TPP)(CO)PPh3 complexes. Optical and 1H nmr data are presented for the complexes in solution. In some cases dissociation of a phosphine ligand to generate five-coordinate species occurs and this has been studied quantitatively in toluene at 20 °C for the Ru(OEP)L2 and Ru(TPP)L2 systems.

Synthesis of complexes of the type cis-Pt(amine) (unsaturated ligand)Cl2 and crystal structure cis-Pt(methylaimne) (dimethylhexynediol)Cl2

1989 ◽  
Vol 67 (12) ◽  
pp. 2209-2212 ◽  
Author(s):  
F. D. Rochon ◽  
R. Melanson ◽  
Monique Doyon
Keyword(s):  
Crystal Structure ◽  
Platinum Complexes ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Methyl Derivative ◽  
Full Matrix ◽  
X Ray ◽  
H Nmr ◽  
R Factor ◽  
Square Planar

Complexes of the type cis-Pt(L)(un)Cl2 where L = primary amine or methyl derivative of pyridine and un = cyclopentene, cyclohexene, or dimethylhexynediol, have been synthesized from the reaction of K[Pt(L)Cl3] with the unsaturated ligand in water. The compounds were characterized and studied by 1H NMR and IR spectroscopy. The crystal structure of cis-Pt(CH3NH2)((CH3)2C(OH)—C≡C—C(OH)(CH3)2)Cl2 was determined by X-ray diffraction methods. The crystals are monoclinic, space group P21/c, with a = 6.544(2), b = 14.304(7), c = 15.508(7) Å, β = 109.39(2)°, and Z = 4. The coordinates and the anisotropic thermal factors were refined by full-matrix least-squares analysis to a R factor of 0.048 and wR = 0.047. The coordination around the platinum atom is square planar and the acetylenic ligand is perpendicular to the Pt plane. Keywords: platinum complexes, crystal structure, methylamine, dimethylhexynediol, synthesis.

scholarly journals Synthesis, Crystal Structure, and Biological Activity ofcis/transAmide Rotomers of (Z)-N′-(2-Oxoindolin-3-ylidene)formohydrazide

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Hatem A. Abdel-Aziz ◽  
Hazem A. Ghabbour ◽  
Wagdy M. Eldehna ◽  
Maha M. Qabeel ◽  
Hoong-Kun Fun
Keyword(s):  
Crystal Structure ◽  
Human Tumor ◽  
Cancer Cell Line ◽  
Monoclinic Space Group ◽  
Moderate Activity ◽  
Standard Drug ◽  
X Ray ◽  
H Nmr ◽  
Mcf 7

(Z)-N′-(2-Oxoindolin-3-ylidene)formohydrazide (2) was synthesized by the reaction of (Z)-3-hydrazonoindolin-2-one (1) with formic acid under reflux. The structure of2was characterized by IR, Mass,1H NMR, and X-ray crystal structure determination. Interestingly, compound2appeared in DMSO-d6ascisandtransamide rotomers in 25% and 75%, respectively. The X-ray analysis showed theZgeometrical isomer of2around –C=N– forcisandtransamide rotomers. The crystal of2belongs to monoclinic, space groupP21/c, witha=4.5206(1) Å,b=22.4747(7) Å,c=17.3637(5) Å,β=103.752(1)°,Z=8,V=1713.57(8) Å3,Dc=1.467 Mg m−3,μ=0.11 mm−1,F(000)=784,R=0.047, andwR=0.123for 3798 observed reflections withI>2σ(I). Compound2exhibited a moderate activity in its antimicrobial evaluation againstE. coliandP. aeruginosaand a good activity againstS. aureusclose to that of the standard drug ciprofloxacin. Thein vitroanticancer activity of2was evaluated against two human tumor cell lines, namely, HepG2 hepatocellular carcinoma and MCF-7 breast cancer. HepG2 cancer cell line was more susceptible to compound2than MCF-7.

Crystal Structure and Tautomerism of 1-[N-(4-Iodophenyl)]aminomethylidene-2(1H)naphthalenone

2001 ◽  
Vol 56 (10) ◽  
pp. 1003-1008 ◽  
Author(s):  
H. Ünver ◽  
M. Kabak ◽  
D. M. Zengin ◽  
T. N. Durlu
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Quantum Mechanical ◽  
Monoclinic Space Group ◽  
Quantum Mechanical Calculations ◽  
X Ray ◽  
H Nmr ◽  
Mechanical Methods ◽  
Intramolecular Hydrogen ◽  
Semi Empirical

1-[N-(4-Iodophenyl)]aminomethylidene-2(1H)naphthalenone (1) (C17H12NOI) has been studied by X-ray analysis, IR, 1H NMR, UV and AM1 semi-empirical quantum mechanical methods. It crystallises in the monoclinic space group P21/n with a = 4.844(3), b = 21.428(2), c = 13.726(2) Å, ß = 93.07(2)° (R1 =0.032 for 4132 reflections [I > 2σ(I)]). The title compound is not planar and an intramolecular hydrogen bond connects O1 and N1 [2.530(4) Å]. Complementary IR, 1H NMR and UV measurements out. Tautomerism and conformations of the title semi-empirical quantum mechanical calculations and the results are compared with the X-ray data.

Synthesis and Structure of a Palladium(II) Chloride Complex with 2-(2-Methyl-3-phenyl-isoxazolidin-5-yl)-pyridine

2000 ◽  
Vol 55 (5) ◽  
pp. 373-376 ◽  
Author(s):  
Andrey B. Lysenko ◽  
Oleg V. Shishkin ◽  
Rostislav D. Lampeka
Keyword(s):  
Chelate Ring ◽  
Organic Ligand ◽  
Chloride Complex ◽  
Monoclinic Space Group ◽  
Equatorial Orientation ◽  
X Ray Diffraction ◽  
Methyl Group ◽  
X Ray ◽  
H Nmr ◽  
Square Planar

The 1:1 complex of palladium(II) chloride with 2-(2-methyl-3-phenyl-isoxazolidin-5-yl)- pyridine (L) has been prepared and studied by means of elemental analysis, 1H NMR spectroscopy and X-ray diffraction (monoclinic, space group P21/n with parameters: a = 8.141(2), b = 9.750(2),c = 20.691(6)Å ,β = 95.62(3)°,V = 1634.4(7)Å3 ,Z = 4 ;R1= 0.054 and wR2= 0.144 for 3352 unique reflections). A square-planar coordination polyhedron has been established for the palladium atom both in acetone solution and in the solid state. The organic ligand is coordinated toometal in a bidentate manner via nitrogen atoms of the pyridine substituent (Pd-N(2) 2.125(3) Å) and the isoxazolidine heterocycle (Pd-N(l) 2.102(3) Å). The other two coordination positions of palladium are occupied by chlorine atoms (Pd-Cl(l) 2.321(1) and Pd-Cl(2) 2.333(1) Å). The six-membered chelate ring formed by Pd, N(2), C(4), C(1), 0(1) and N (1) possesses a “twist-tub” conformation. The isoxazolidine cycle has an envelope conformation with an equatorial orientation of the methyl group.

Synthese, Struktur und Reaktivität labiler Rhodium(I)-Komplexe mit iPr2PC2H4NMe2 und iPr2PC2H4OMe als Phosphanliganden / Synthesis, Structure and Reactivity of Labile Rhodium(I) Complexes Containing iPr2PC2H4NMe2 and iPr2PC2H4OMe as Phosphine Ligands

1990 ◽  
Vol 45 (11) ◽  
pp. 1548-1558 ◽  
Author(s):  
Helmut Werner ◽  
Andreas Hampp ◽  
Karl Peters ◽  
Eva Maria Peters ◽  
Leonhard Walz ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Chelate Ring ◽  
Parent Compound ◽  
Phosphine Ligand ◽  
Phosphine Ligands ◽  
X Ray ◽  
Vinylidene Complexes ◽  
Square Planar

Square-planar rhodium(I) complexes [RhCl(iPr2PC2H4Y)2] (8, 9) containing one chelating and one P-bonded monodentate phosphine ligand are prepared from [RhCl(C8H14)2]2 (7) and the new functionalized phosphines iPr2PC2H4Y (5,6). Reaction of 9 (Y = NMe2) with CO and of 8 (Y = OMe) with CO, C2H4, C2H2, C2Ph2 and HC2Ph leads to opening of the chelate ring and formation of the complexes trans-[RhCl(L)(η1-P–iPr2PC2H4Y)2] (10-15). Treatment of 8 with H2 gives the dihydridorhodium(III) compound [RhH2Cl(iPr2PC2H4OMe)2] (16). The vinylidene complexes trans-[RhCl(=C=CHR)(η1-P– iPr2PC2H4OMe)2] (17, 18) are obtained by thermal or pyridine promoted rearrangement of 13 (L = C2H2) and 15 (L = HC2Ph). 13 and 15 have also been used as starting materials for the synthesis of the cyclopentadienyl alkyne and vinylidene complexes 19-21. The X-ray crystal structure of the parent compound 8 was determined.

scholarly journals A New 3D Coordination Polymer of Bismuth with Nicotinic AcidN-Oxide

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Farzin Marandi ◽  
Ingo Pantenburg ◽  
Gerd Meyer
Keyword(s):  
Crystal Structure ◽  
Thermal Stability ◽  
Coordination Polymer ◽  
Three Dimensional ◽  
Water Molecules ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Thermal Stability Of

The new three-dimensional coordination polymer {[Bi(NNO)2(NO3)]·1.5H2O}n(1, NNO−= nicotinateN-oxide) was synthesized and characterized by elemental analysis, IR and1H-NMR spectroscopy, as well as single-crystal X-ray diffraction analysis.1crystallizes in the monoclinic space group C2/c. The crystal structure consists of a rectangular-shaped grid constructed with NNO linkers. Cavities of a diameter of 7.9–8.3 Å2are filled with disordered water molecules. The thermal stability of the compound was evaluated by thermogravimetric analysis.

Synthesis of aminoalcohol compounds of platinum and crystal structure of trans-[Pt(2-amino-2-methyl-1-propanol)2Cl2]

1984 ◽  
Vol 62 (12) ◽  
pp. 2657-2660 ◽  
Author(s):  
F. D. Rochon ◽  
P. C. Kong ◽  
R. Melanson
Keyword(s):  
Crystal Structure ◽  
Organic Ligand ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Full Matrix ◽  
X Ray ◽  
R Factor ◽  
Bonding System ◽  
Square Planar ◽  
Hydrogen Bonding System

Three types of complexes, trans-[Pt(LH)2Cl2], [Pt(L)2], and [Pt(LH)2(SR)2] where LH = NH2—C(CH3)2(CH2OH) and NH2—C(CH2OH)3 and L are the deprotonated ligands, have been synthesized.The crystal structure of trans-[Pt(NH2—C(CH3)2CH2OH)2Cl2] has been determined by X-ray diffraction methods. The crystals are monoclinic, space group P21/c, with a = 6,282(3), b = 20,901(13), c = 10,769(10) Å, β = 92,64(6)°, and Z = 4. The structure was refined by full-matrix least-squares analysis to a conventional R factor of 0.049 and Rw = 0.042. The coordination around the platinum atom is square planar. The Pt—Cl distances are 2.306(2) and 2.309(3) Å and the Pt—N bonds are 2.060(8) and 2.071 (7) Å. The hydroxyl oxygen atoms are disordered; the disorder is different for each organic ligand. The structure is stabilized by an extensive hydrogen bonding system.

Reactions of "cyclen-" and "cyclam-phosphorane" with [Pt2Cl4(PEt3)2]. Monodentate and bidentate complexes and the crystal and molecular structure of [PtCl(PEt3)(cyclamPH)]Cl•CH2Cl2

1989 ◽  
Vol 67 (1) ◽  
pp. 48-53 ◽  
Author(s):  
David Eric Berry ◽  
Jane Browning ◽  
Gordon William Bushnell ◽  
Keith Roger Dixon ◽  
Alan Pidcock
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Simple Formula ◽  
Crystal And Molecular Structure ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
Nmr Studies ◽  
X Ray ◽  
Square Planar ◽  
Coordination Plane

Reaction of "cyclamphosphorane" (cyclamPH) with [Pt2Cl4(PEt3)2] yields [PtCl(PEt3)(cyclamPH)]Cl. The complex crystallizes as a dichloromethane solvate in the monoclinic space group P21/n, with a = 13.877(3), b = 23.231(7), c = 8.295(2)Å, β = 91.86(4)°, and an X-ray diffraction study shows square planar platinum coordination in which the labile proton of cyclamPH has transferred from phosphorus to nitrogen and the ligand is attached via simple [Formula: see text] chelation. The phosphorus is trans to chlorine in the platinum coordination plane.The corresponding product, trans-[PtCl2(PEt3)(cyclenPH2)]Cl, derived from reaction of "cyclenphosphorane" (cyclenPH) with [Pt2Cl4(PEt3)2], is shown by NMR studies to have a quite different structure in which the ligand is protonated at two nitrogen sites but not at phosphorus. The phosphorus is pentacoordinate with four attachments to nitrogen atoms and one to platinum. The two chlorine atoms are mutually trans in the platinum coordination plane. Keywords: crystal structure, cyclenphosphorane reaction, cyclamphosphorane reaction, X-ray diffraction.

Organomercury Compounds. XXXI. Preparations and 199Hg N.M.R. Spectra of Organomercury Derivatives of 2-Phenylpyridine, Benzo[h]quinoline, 1-Phenylpyrazole and 3,4,5-Trimethyl-1-phenylpyrazole, and the X-Ray Crystal Structure of Bis[2-(pyridin-2'-yl)phenyl]mercury

1993 ◽  
Vol 46 (9) ◽  
pp. 1323 ◽  
Author(s):  
DS Black ◽  
GB Deacon ◽  
GL Edwards ◽  
BM Gatehouse
Keyword(s):  
Crystal Structure ◽  
Chemical Shifts ◽  
Monoclinic Space Group ◽  
Initial Product ◽  
X Ray ◽  
Square Planar ◽  
Phenyl Rings ◽  
Organomercury Compounds ◽  
Phenylmercuric Chloride ◽  
Phenyl Mercury

2-(Pyridin-2'-yl) phenylmercuric acetate has been prepared by mercuration of 2-phenylpyridine. Symmetrization of the corresponding chloride by alkaline sodium stannite gave bis [2-(pyridin-2'-yl)phenyl]mercury, which was also prepared from 2-(2'-aminophenyl)pyridine by the diazo method and treatment of the initial product with copper powder and aqueous ammonia. Mercuration of benzo [h] quinoline and 3,4,5-trimethyl-1-phenylpyrazole with mercuric acetate followed by treatment with lithium chloride yielded benzo [h]quinolin-10-ylmercuric chloride and 2-(3',4',5'-trimethylpyrazol-1'-yl) phenylmercuric chloride respectively. Treatment of the former product with tribromide ions gave 10-bromobenzo[h] quinoline. The exchange Grignard reaction between 1-phenylpyrazole and ethylmagnesium bromide to give 2-(pyrazol-1'-yl) phenylmagnesium bromide has been monitored by reactions with benzonitrile and D2O to establish optimum conditions for reaction with mercuric bromide giving bis [2-(pyrazol-1'-yl)phenyl]mercury. The 199Hg n.m.r. chemical shifts of the majority of mercurials are shifted substantially downfield relative to the corresponding simple phenylmercurials consistent with weak intramolecular coordination by the heterocyclic nitrogen donor atoms, but a small upfield shift is observed for bis [2-(pyrazol-1'-yl)phenyl]mercury. The X-ray crystal structure of bis [2-(pyridin-2′-yl)phenyl]mercury [monoclinic, space group P21/n, a 12.746(2), b 11.660(2), c 5.698(1) Ǻ, β 92.81(1)′, V 845.8 Ǻ3] shows a centrosymmetric molecule with strong linear two coordination [Hg-C 2.098(8) Ǻ; C-Hg-C 180.0°] and significant but much weaker Hg-N interactions [Hg-N 2.798(7) Ǻ; N-Hg-N 180.0°] giving overall distorted square planar stereochemistry. The phenyl rings are mutually coplanar, whilst the two pyridin-2'-yl rings are parallel and inclined at 10.8° to the phenyl groups.

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