Synthesis and X-ray structural characterization of the ruthenium β-diketonato complexes: Ru(hfac)3, cis-Ru(hfac)2(MeCN)2, and cis-Ru(hfac)(acac)(MeCN)2

1999 ◽  
Vol 77 (11) ◽  
pp. 1821-1833 ◽  
Author(s):  
Ian R Baird ◽  
Steven J Rettig ◽  
Brian R James ◽  
Kirsten A Skov
Keyword(s):  
Cyclic Voltammetry ◽  
Elemental Analysis ◽  
Structural Characterization ◽  
Subsequent Treatment ◽  
Peroxide Oxidation ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Etoh Solution

Ru(hfac)3 (2) was synthesized via peroxide oxidation of the Ru(II) species [Na][Ru(hfac)3] (1) (hfac = 1,1,1,5,5,5-hexafluoroacetylacetonate). Treatment of either 1 or 2 with CF3SO3H in MeCN generated cis-Ru(hfac)2(MeCN)2 (3). Ru(acac)2(hfac) (4) (acac = acetylacetonate) was generated by addition of hfac to an EtOH solution of cis-[Ru(acac)2(MeCN)2][CF3SO3]. Subsequent treatment of 4 with CF3SO3H in MeCN yielded cis-Ru(acac)(hfac)(MeCN)2 (7). Syntheses of [Na][Ru(hfac)2(acac)] (5) and Ru(hfac)2(acac) (6) are also reported. The complexes were characterized generally by elemental analysis, cyclic voltammetry, UV-vis, NMR, and IR spectroscopies. The structures of 2, 3, and 7 were established by X-ray crystallographic analyses. Crystals of 2 are monoclinic with a = 8.7781(4), b = 13.0760(11), c = 19.1857(5) Å, β = 92.2275(5)°, Z = 4, and space group P21/n; those of 3 are monoclinic with a = 25.731(4), b = 8.8332(13), c = 18.1955(4) Å, β = 93.3395(6)°, Z = 8, and space group C2/c; and those of 7 are triclinic with a = 7.6812(9), b = 10.680(2), c = 12.578(2) Å, α = 88.062(6)°, β = 83.874(3)°, γ = 69.5898(15)°, Z = 2, and space group Pbar over 1. The structures were solved by Patterson methods and refined by full-matrix least-squares procedures to R(F) = 0.036, 0.035, and 0.068 (Rw(F2) = 0.061,Rw(F) = 0.052, and Rw(F) = 0.089), respectively.Key words: ruthenium, β-diketonato complexes, acetylacetonate, 1,1,1,5,5,5-hexafluoroacetylacetonate, acetonitrile complexes.

Synthesis and characterization of homoleptic ruthenium(II) imidazole complexes, and a carbonyl species derived by CO abstraction from DMF

1998 ◽  
Vol 76 (10) ◽  
pp. 1379-1388 ◽  
Author(s):  
Ian R Baird ◽  
Steven J Rettig ◽  
Brian R James ◽  
Kirsten A Skov
Keyword(s):  
Ambient Temperature ◽  
Least Squares ◽  
Key Words ◽  
Elemental Analysis ◽  
Synthesis And Characterization ◽  
Full Matrix ◽  
Space Group ◽  
X Ray ◽  
Imidazole Complexes

[Ru(II)(L)6]2+ complexes were synthesized from [Ru(DMF)6][CF3SO3]3; DMF = dimethylformamide, L = imidazole (Im), N-methylimidazole (NMeIm) and 5-methylimidazole (5MeIm). The 2-methylimidazole complex trans-[Ru(CO)(DMF)(2MeIm)4][CF3SO3]2 (4) was also synthesized via a reaction involving abstraction of CO from DMF; 4 loses CO reversibly at ambient temperature to form [Ru(DMF)(2MeIm)4][CF3SO3]2 (5), and the DMF can be removed to generate a [Ru(CF3SO3)x(2MeIm)4][CF3SO3]y species (x = 2, y = 0, or x = 1 = y), containing coordinated triflate. The complexes were characterized by elemental analysis, conductivity, UV-vis, NMR, and IR spectroscopies. The structures of [Ru(Im)6][CF3SO3]2 (1), [Ru(NMeIm)6][CF3SO3]2 (2), and [Ru(5MeIm)6][CF3SO3]2 (3) were established by X-ray crystallographic analyses. Crystals of 1, are triclinic, a = 7.4010(6), b = 9.9846(15), c = 11.275(2) Å, α = 113.469(5), β = 92.419(2), γ = 94.737(2)°, Z = 1, space group P1 ; those of 2, are trigonal, a = 11.558(2), c = 8.109(3) Å, Z = 1, space group P3; and those of 3, are trigonal, a = 12.6547(4), c = 20.4078(12) Å, Z = 3, space group R3. The structures were solved by Patterson methods and refined by full-matrix least-squares procedures to R(F) = 0.029, 0.034, and 0.034 (R w (F2) = 0.055, R w (F) = 0.031, and R w (F2) = 0.058), respectively. Key words: hexakis(imidazole)ruthenium(II) triflates, crystal structures, CO abstraction.

Synthesis and Structural Characterization of Copper(I) and Copper(II) Complexes with an Ambivalent Phenanthroline-Type Ligand

1997 ◽  
Vol 50 (10) ◽  
pp. 951 ◽  
Author(s):  
Jean-Paul Collin ◽  
Pablo Gaviña ◽  
Jean-Pierre Sauvage ◽  
André De Cian ◽  
Jean Fischer
Keyword(s):  
Cyclic Voltammetry ◽  
Structural Characterization ◽  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Coordination Modes ◽  
X Ray Crystallography ◽  
Phenanthroline Ligand

The new phenanthroline ligand 2-(p-methoxyphenyl)-9-(5′-methylpyridin-2′-yl)-1,10-phenanthroline L has been synthesized and shown to form four-coordinate CuI(L)2 (1) and six-coordinate CuII(L)2 (2) complexes. Their structures have been determined by X-ray crystallography: (1) C50H38CuN6O2.BF4, triclinic, space group P -1, a12·924(3), b 14·567(4), c 12·649(3) Å , α 105·57(2), β 107·68(2), γ 104·00(2)°; (2) C50H38CuN6O2.2PF6, monoclinic, space group P 21/c, a 17·701(5), b 19·285(5), c 14·93(4) Å, β 98·20(2)°. In solution, cyclic voltammetry measurements indicate for the copper(I) and copper(II) complexes a very fast rearrangement of the pyridine substituent with the change of the oxidation state. Surprisingly, the X-ray data show two different coordination modes for the ligand around the copper(I) ion, the 1,10-phenanthroline nucleus being either mono- or bi-dentate. In solution, since the 1H n.m.r. spectra obtained even at several temperatures display only one set of signals, it is proposed that a fast equilibrium takes place between two coordination modes of the phenanthroline

Structural Systematics of Rare Earth Complexes. VII. Crystal Structure of Bis(2,2'/6',2␛-Terpyridinium) Octaaquaterbium(III) Heptachloride Hydrate

1994 ◽  
Vol 47 (2) ◽  
pp. 391 ◽  
Author(s):  
CJ Kepert ◽  
BW Skeleton ◽  
AH White
Keyword(s):  
Crystal Structure ◽  
Rare Earth ◽  
Single Crystal ◽  
Structural Characterization ◽  
Title Compound ◽  
Room Temperature ◽  
Chloride Ions ◽  
Full Matrix ◽  
X Ray

The room-temperature single-crystal X-ray structural characterization of the title compound (tpyH2)2[Tb(OH2)8]Cl7.~2⅓H2O is recorded. Crystals are triclinic, Pī , a 17.063(5), b 16.243(3), c 7.878(3) Ǻ, α 84.78(2), β 84.39(3), γ 87.81(2)°, Z = 2 formula units; 3167 'observed' diffractometer reflections were refined by full-matrix least-squares procedures to a residual of 0.057. Notable features of interest of the compound are the 'chelation' of chloride ions by the terpyridinium cations , and the existence of a free [Tb(OH2)8]2+ cation in the presence of an abundance of chloride ions.

scholarly journals Transition metal complexes with thiosemicarbazide-based ligands, Part 58. Synthesis, spectral and structural characterization of dioxovanadium(V) complexes with salicylaldehyde thiosemicarbazone

2011 ◽  
Vol 76 (6) ◽  
pp. 865-877 ◽  
Author(s):  
Ljiljana Vojinovic-Jesic ◽  
Vukadin Leovac ◽  
Mirjana Lalovic ◽  
Valerija Cesljevic ◽  
Ljiljana Jovanovic ◽  
...  
Keyword(s):  
Transition Metal ◽  
Metal Complexes ◽  
Transition Metal Complexes ◽  
Elemental Analysis ◽  
Structural Characterization ◽  
Ammoniacal Solution ◽  
X Ray ◽  
Vis Spectroscopy ◽  
Oxo Ligand

The first two complexes of dioxovanadium(V) with salicylaldehyde thiosemicarbazone (SALTSC), of the coordination formulas [VO2(SALTSC-H)]?H2O (1) and NH4[VO2(SALTSC-2H] (2), were synthesized and characterized by elemental analysis, conductometric measurements, IR and UV-vis spectroscopy and X-ray analysis. The complexes were obtained in the reaction of an aqueous ammoniacal solution of NH4VO3 and SALTSC. The results of the characterization showed that SALTSC was coordinated in the usual ONS tridentate mode as monoanion in complex 1 and dianion in complex 2. In both complexes, the vanadium atom is in a deformed square-pyramidal environment and is slightly shifted towards the apical oxo-ligand (? 0.52 ?).

scholarly journals Darstellung und Charakterisierung der μ3-Oxo-Cluster [Cp3Mo3(CO)4µ-Cl)(µ3-O)] und [Cp3Mo3(µ-CO)3(CO)3(µ3-O)]+ / Synthesis and Characterization of the µ3-Oxo Clusters [Cp3Mo3(CO)4μ-Cl)(μ3-O)] and [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+

1990 ◽  
Vol 45 (4) ◽  
pp. 508-514 ◽  
Author(s):  
B. Nuber ◽  
W. Schatz ◽  
M. L. Ziegler
Keyword(s):  
Structure Analysis ◽  
Elemental Analysis ◽  
Spectroscopic Data ◽  
Synthesis And Characterization ◽  
Monoclinic Space Group ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray

[CpMo(CO)3]2 (1) (Cp = cyclopentadienyl) reacts with InCl3 in diglyme to yield the oxo-cluster [Cp3Mo3(CO)4(μ-Cl)(μ3-O)] (2) and the cationic oxo-cluster [Cp3Mo3(μ-CO)3(CO)3(μ3-O)]+ as the salt [Cp3Mo3(μ-CO)3(CO)3(μ3-O)][CpMo(CO)3InCl3] (3). The compounds were characterized by elemental analysis, spectroscopic data and X-ray structure analysis. Compound 2 crystallizes in the orthorhombic space group P212121 with a = 1006.0(3), b = 1244.6(4) and c = 1600.8(5) pm, V = 2004.3 x 106 pm3, Z = 4. Compound 3 crystallizes in the monoclinic space group P 21/m with a = 874.4(8), b = 1407(1) and c = 1500(1) pm, β = 92.95(6) , V = 1843 × 106 pm3, Z = 2.

Structural Characterization of Cationic 16-Electron Pentamethylcyclopentadienyl Ruthenium(II) Complexes Containing the Binuclear [Cp*Ru(μ-Cl)3RuCp*]– Anion

2008 ◽  
Vol 63 (10) ◽  
pp. 1155-1159 ◽  
Author(s):  
Thomas Glöge ◽  
Dejan Petrovic ◽  
Cristian G. Hrib ◽  
Peter G. Jones ◽  
Matthias Tamm
Keyword(s):  
Crystal Structures ◽  
Structural Characterization ◽  
Complex Salt ◽  
Monoclinic Space Group ◽  
Chlorine Atoms ◽  
Space Group ◽  
X Ray ◽  
Diimine Ligand ◽  
Half Sandwich

AbstractThe reaction of the diimine ligand 1,2-bis(1,3-diisopropyl-4,5-dimethylimidazolin-2-imino)ethane (BLiPr) with tetrameric [Cp*RuCl]4 in a 1 : 0.75 ratio afforded the complex salt [1][2] containing the 16-electron half-sandwich cation [Cp*Ru(BLiPr)]+ (1) and the dinuclear anion [Cp*Ru(μ- Cl)3RuCp*]− (2). The X-ray crystal structures of [1][2]·31/2THF (monoclinic, space group P21/n, Z = 4) and of [1][2]·THF (monoclinic, space group C2/m, Z = 4) are reported, allowing the structural characterization of the unprecedented anion 2, in which two [(η5-C5Me5)Ru(II)] moieties are bridged by three μ2-chlorine atoms.

Synthesis and characterization of LMo(CO)3M(PPh3)x (where L = tridentate pyrazolyl-gallate or -borate ligand; M = Rh, x = 2; M = Cu, x = 1). X-ray crystal structures of [MeGapz3]Mo(CO)3Rh(PPh3)2 and [MeGapz3]Mo(CO)3Cu(PPh3) (where pz = pyrazolyl, N2C3H3)

1986 ◽  
Vol 64 (2) ◽  
pp. 373-386 ◽  
Author(s):  
Gregory A. Banta ◽  
Brenda M. Louie ◽  
Emmanuel Onyiriuka ◽  
Steven J. Rettig ◽  
Alan Storr
Keyword(s):  
Least Squares ◽  
Crystal Structures ◽  
Heavy Atom ◽  
Synthesis And Characterization ◽  
Octahedral Structure ◽  
Full Matrix ◽  
Space Group ◽  
X Ray

The reactions of the LMo(CO)3− ions (L = MeGapz3, HBpz3, Me2Gapz(OCH2CH2NMe2)) with [Cu(PPh3)Cl]4 and Rh(PPh3)3Cl have yielded complexes with Mo—Cu and Mo—Rh bonds. The X-ray crystal structures of two such complexes have been determined. Crystals of [MeGapz3]Mo(CO)3Cu(PPh3) are monoclinic, a = 17.071(2), b = 16.738(1), c = 23.641(3) Å, β = 104.899(6)°, Z = 8, space group P21/n, and those of [MeGapz3]Mo(CO)3Rh(PPh3)2, are triclinic, a = 12.519(3), b = 17.182(4), c = 12.071(2) Å, α = 105.02(1), β = 109.87(1), γ = 97.10(2)°, Z = 2, space group [Formula: see text]. Both structures were solved by conventional heavy atom methods and were refined by full-matrix least-squares procedures to R = 0.040 and Rw = 0.035 for 6296 reflections with I ≥ 2σ(I) and R = 0.036 and Rw = 0.037 for 5642 reflections with I ≥ 3σ(I), respectively. The former complex provides a rare example of a 3:3:1, or capped octahedral structure, with a short (mean) Mo—Cu distance of 2.513(9) Å. The latter compound displays one terminal and two bridging CO ligands and a Mo—Rh distance of 2.6066(5) Å.

Synthesis and structural characterization of a novel copper(II)/lead(II) heterometallic organic–inorganic hybrid

2015 ◽  
Vol 70 (9) ◽  
pp. 617-623 ◽  
Author(s):  
Gao-Feng Wang ◽  
Xiao Zhang ◽  
Shu-Wen Sun ◽  
Chen-Zhong Yao ◽  
Zhao-Rong Liu ◽  
...  
Keyword(s):  
Elemental Analysis ◽  
Structural Characterization ◽  
Building Blocks ◽  
Title Complex ◽  
X Ray Diffraction ◽  
Inorganic Hybrid ◽  
X Ray ◽  
Sheet Structure ◽  
Terpyridine Ligands

AbstractA new copper(II)/lead(II) complex [(terpy)3CuPb5Br12] (1) (terpy = 2,2′:6′,2″-terpyridine) has been synthesized and characterized by IR, elemental analysis, and single-crystal X-ray diffraction analysis. The copper(II) and lead(II) ions in the title complex are in distorted six- (Cu(II), Pb(II)) and eight-fold (Pb(II)) coordination environments, in which the donor atoms are provided by bromide anions and nitrogen atoms of the 2,2′:6′,2″-terpyridine ligands. Complex 1 contains [(terpy)4Pb9Br20]2– building blocks. These bromoplumbate(II) clusters are connected by (terpy)2Cu2Br4 units along the crystallographic b axis and by PbBr6 units along the a axis, thereby forming an extended sheet structure.

Synthesis and Structural Characterization of Metal Complexes of 2-Formylpyrrole 4N-Methylthiosemicarbazone (4ML1) and 2-Acetyl- pyrrole 4N-Methylthiosemicarbazone (4ML2). The X-Ray Crystal Structures of [Ni(4ML1-H)2], [Pd(4ML1-H)2] and [Cd(4ML2)2I2]

2001 ◽  
Vol 56 (3) ◽  
pp. 219-228 ◽  
Author(s):  
Ruben Alonso ◽  
Elena Bermejo ◽  
Rosa Carballo ◽  
Alfonso astiñeiras ◽  
Teresa Pérez
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Structural Characterization ◽  
X Ray ◽  
Group 12 ◽  
New Compounds ◽  
Group 10 Metals ◽  
C Nmr

Abstract Reaction of 4N-methyl-2-[1-(pyrrol-2-yl)methylidene]hydrazinecarbothioamide (4ML1 and 4N-methyl-2-[1-(pyrrol-2-yl)-ethylidene]hydrazine carbothioamide (4ML1) with zinc(II), cadmium(II) and mercury(II) halides afforded complexes with formulas [M(L)X2] [(L; M; X) =(4ML1; Cd; Cl) (4), (4ML1; Hg; Cl, Br, I) (7 - 9), (4ML2; Cd; Cl) (17), (4ML2; Hg; Cl, Br, I) (20 - 22)] or [M(L)2X2] [(L; M; X) = (4ML1; Zn; Cl, Br, I) (1 - 3), (4ML1; Cd; Br, I) (5, 6), (4ML2; Zn; Cl, Br, I) (14 - 16), (4ML2; Cd; Br, I) (18, 19)]. Reaction of 4ML1 with salts of copper(II), nickel(II), palladium(II) and platinum(II) afforded complexes of formula [M(4ML1-H)2] (10 -13). Crystals of 11, 12 and 19 were studied by X-ray diffractometry, and all new compounds were characterized by elemental analysis, mass spectrometry, and IR, electronic and 1H and 13C NMR spectroscopy and, when pertinent and allowed by the solubility of the compound, 113Cd or 199Hg NMR spectroscopy. In the complexes of Group 12 metals, both ligands are neutral and S-monodentate. In the complexes of copper or Group 10 metals, 4ML1 is monodeprotonated and S,N-bidentate.

Structural Characterization of a Calix[4]arene Constrained to a 1,3-Alternate Conformation by Polyether Bridging

1994 ◽  
Vol 47 (4) ◽  
pp. 757 ◽  
Author(s):  
Z Asfari ◽  
JM Harrowfield ◽  
AN Sobolev ◽  
J Vicens
Keyword(s):  
Alkali Metal ◽  
Metal Ions ◽  
Single Crystal ◽  
Structural Characterization ◽  
Room Temperature ◽  
Free Ligand ◽  
Tetraethylene Glycol ◽  
Space Group ◽  
X Ray

Despite evidence of coordinative interactions with alkali metal picrates in solution, attempts to crystallize Li+, Na+, K+, Rb+ or Cs+ complexes of a 'doubly crowned' calix [4] arene (obtained by reaction of tetraethylene glycol ditosylate with p-t- butylcalix [4] arene ) have resulted only in the deposition of crystals of the free ligand . A room-temperature single-crystal X-ray study has shown the crystals to be hexagonal, space group P6422, a (= b) 17.092(5), c 20.147(7) Ǻ, V 5097(5) Ǻ3, Z 3, conventional R (on |F|) 0.082 for 1397 'observed' reflections [I > 3σ(I)]. The highly symmetrical oblate-globular shape of this doublecrowncalix allows the enclosure of an extended narrow cavity possibly better suited to the binding of two small metal ions rather than one large.

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