Preparation and characterization of Tl(1,2-C2H4Cl2)B(OTeF5)4: a metal complex of a least coordinating solvent and a least coordinating anion

1992 ◽  
Vol 70 (3) ◽  
pp. 726-731 ◽  
Author(s):  
Paul K. Hurlburt ◽  
Oren P. Anderson ◽  
Steven H. Strauss
Keyword(s):  
Metal Ion ◽  
Chelate Ring ◽  
Ion Solvation ◽  
Crystalline Compound ◽  
Triclinic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Solid Salt ◽  
Solvent Metal

Addition of B(OTeF5)3 to TIOTeF5 in the weakly coordinating solvents dichloromethane, 1,2-dichloroethane, and 1,1,2-trichlorotrifluoroethane produces solutions of M(solv)x+B(OTeF5)4−. When the solvent was 1,2-dichloroethane, the crystalline compound Tl(1,2-C2H4Cl2)B(OTeF5)4 was isolated and studied by X-ray crystallography: triclinic, space group [Formula: see text], a = 9.221 (4), b = 11.396(5), c = 12.538 (4) Å, α = 110.75 (3)°, β = 101.72(3)°, γ = 99.74 (3)°, Z = 2, T = −116 °C. The Tl(1,2-C2H4Cl2)+ cation contains a five-membered chelate ring with Tl—Cl distances of 3.138 (4) and 3.179 (3) Å. The metal ion is weakly bonded to four B(OTeF5)4− counterions, with nine Tl—F interactions that range from 2.950 (5) to 3.981 (8) Å. When the solvent is dichloromethane or 1,1,2-trichlorotrifluoroethane, only the unsolvated solid salt TlB(OTeF5)4 can be isolated by crystallization. This salt is thermally unstable, slowly forming TlOTeF5 and volatile B(OTeF5)3. Keywords: noncoordinating anion, noncoordinating solvent, metal ion solvation.

Synthesis and structural characterization of donor-stabilized disubstituted diphenyldithiophosphates of nickel(II)

2014 ◽  
Vol 70 (4) ◽  
pp. 761-767 ◽  
Author(s):  
Sandeep Kumar ◽  
Ruchi Khajuria ◽  
Amanpreet Kaur Jassal ◽  
Geeta Hundal ◽  
Maninder S. Hundal ◽  
...  
Keyword(s):  
Single Crystal ◽  
Chelate Ring ◽  
Donor Ligands ◽  
Monoclinic Space Group ◽  
Bidentate Ligands ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray

Donor-stabilized addition complexes of nickel(II) with disubstituted diphenyldithiophosphates, [{(ArO)2PS2}2NiL2] {Ar = 2,4-(CH3)2C6H3[(1), (5)], 2,5-(CH3)2C6H3[(2), (6)], 3,4-(CH3)2C6H3[(3), (7)] and 3,5-(CH3)2C6H3[(4), (8)];L= C5H5N [(1)–(4)] and C7H9N [(5)–(8)]}, were successfully isolated and characterized by elemental analysis, magnetic moment, IR spectroscopy and single-crystal X-ray analysis. Compound (4) crystallizes in the monoclinic space groupP21/nwhereas compounds (7) and (8) crystallize in the triclinic space group P\bar 1. The single-crystal X-ray diffraction analysis of (4), (7) and (8) reveals a six-coordinated octahedral geometry for the NiS4N2chromophore. Two diphenyldithiophosphate ions act as bidentate ligands with their S atoms coordinated to the Ni centre. Each of them forms a four-membered chelate ring in the equatorial plane. The N atoms from two donor ligands are axially coordinated to the Ni atom.

Crystal-Structure of Bis(2,2'-6',2'-terpyridine)manganese(II) Bis(triiodide) [Mn(terpy)2](I3)2

1991 ◽  
Vol 44 (2) ◽  
pp. 303 ◽  
Author(s):  
R Bhula ◽  
DC Weatherburn
Keyword(s):  
Crystal Structure ◽  
Transition Metal ◽  
Metal Ions ◽  
Coordination Sphere ◽  
Metal Ion ◽  
Transition Metal Ions ◽  
Triclinic Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
Distorted Octahedral

The crystal structure of [ Mn ( terpy )2](I3)2( terpy = 2,2°:6°,2°-terpyridene) has been determined by X-ray crystallography. The crystals are triclinic, space group Pī , a 9.357(4), b 8.600(2), c 24.531(8) Ǻ, α 93.64(2), B 95.58(3), γ 91.52(2)°, Z 2, V 1960(1)Ǻ3. The structure has been refined to a residual R of 0.065 (Rw 0.070). The coordination sphere of the metal ion is distorted octahedral with each terpy ligand coordinated in a meridional fashion. The structure is compared with those of other M( terpy )2n+ complexes formed by first-row transition metal ions.

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

Supramoleküle aus Kronenethern und geminalen Sulfonen: Synthese von vier binären Komplexen und Kristallstruktur von (CH2CH2O)4·2H 2C(SO2C2H5)2/Supramolecules of Crown Ethers with Geminal Sulfones: Synthesis of Four Binary Complexes and Crystal Structure of (CH2CH2O )4·2H2C(SO2C2H5)2

1995 ◽  
Vol 50 (7) ◽  
pp. 1018-1024 ◽  
Author(s):  
Axel Michalides ◽  
Dagmar Henschel ◽  
Armand Blaschette ◽  
Peter G. Jones
Keyword(s):  
Monoclinic Space Group ◽  
Triclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
X Ray Crystallography ◽  
H Nmr ◽  
Binary Complexes ◽  
Cyclic Polyethers ◽  
Adjacent Unit ◽  
Methylene Group

In a systematic search for supramolecular complexes involving all combinations of the cyclic polyethers 12-crown-4 (12C4), 15-crown-5 (15C 5), 18-crown-6 (18C 6) and dibenzo- 18-crown-6 (DB -18C6), and the geminal di- or trisulfones H2C(SO 2Me)2, H2C (SO2Et)2 and HC (SO2Me)3-n (SO2Et)n (n = 0 -3 ) , only the following four complexes could be isolated and unequivocally characterized by elemental analysis and 1H NMR spectroscopy: [(12C4){H2C (SO2Et)2}2] (3), [(18C6){H2C (S O2Me)2}] (4), [(DB -18C 6){H2C (SO2Et)2}] (5) and [(D B -18C 6)2{HC (SO2Me )(SO2Et)2}3] (6). The structure of 3 (triclinic, space group P1̄) consists of crystallographically centrosymmetric formula units, in which the disulfone molecules are bonded on each side of the ring by two C -H ··· O(crown) interactions originating from the central methylene group (H···O 213 pm) and from the methylene group of one EtSO2 moiety ( H ··· O 237 pm). Formula units related by translation are connected into parallel strands by a third type of reciprocal C -H ···O bond (H ···O 232 pm) between the second H atom of the central methylene group and a sulfonyl oxygen atom of the adjacent unit. The structure of 4 (monoclinic, space group C2/c) showed severe disorder of the crown ether and could not be refined satisfactorily. Compounds 5 and 6 crystallized as long and extremely thin fibres, indicative of linear-polymeric supramolecular structures; single crystals for X-ray crystallography were not available.

scholarly journals Structural Characterization of Heterodinuclear ZnII-LnIII Complexes (Ln = Pr, Nd) with a Ring-Contracted H2valdien-Derived Schiff Base Ligand

2021 ◽  
Author(s):  
Shabana Noor ◽  
Richard Goddard ◽  
Fehmeeda Khatoon ◽  
Sarvendra Kumar ◽  
Rüdiger W. Seidel
Keyword(s):  
Molecular Structure ◽  
Schiff Base ◽  
Structural Characterization ◽  
Schiff Base Ligand ◽  
Crystal And Molecular Structure ◽  
X Ray ◽  
X Ray Crystallography ◽  
Imidazoline Ring

AbstractSynthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes with the formula [ZnLn(HL)(µ-OAc)(NO3)2(H2O)x(MeOH)1-x]NO3 · n H2O · n MeOH [Ln = Pr (1), Nd (2)] and the crystal and molecular structure of [ZnNd(HL)(µ-OAc)(NO3)2(H2O)] [ZnNd(HL)(OAc)(NO3)2(H2O)](NO3)2 · n H2O · n MeOH (3) are reported. The asymmetrical compartmental ligand (E)-2-(1-(2-((2-hydroxy-3-methoxybenzylidene)amino)-ethyl)imidazolidin-2-yl)-6-methoxyphenol (H2L) is formed from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation, resulting in a peripheral imidazoline ring. The structures of 1–3 were revealed by X-ray crystallography. The smaller ZnII ion occupies the inner N2O2 compartment of the ligand, whereas the larger and more oxophilic LnIII ions are found in the outer O2O2’ site. Graphic Abstract Synthesis and structural characterization of two heterodinuclear ZnII-LnIII complexes (Ln = Pr, Nd) bearing an asymmetrical compartmental ligand formed in situ from N1,N3-bis(3-methoxysalicylidene)diethylenetriamine (H2valdien) through intramolecular aminal formation are reported.

scholarly journals Characterization of Aptamer-Protein Complexes by X-ray Crystallography and Alternative Approaches

2012 ◽  
Vol 13 (8) ◽  
pp. 10537-10552 ◽  
Author(s):  
Vincent J. B. Ruigrok ◽  
Mark Levisson ◽  
Johan Hekelaar ◽  
Hauke Smidt ◽  
Bauke W. Dijkstra ◽  
...  
Keyword(s):  
Protein Complexes ◽  
X Ray ◽  
X Ray Crystallography ◽  
Alternative Approaches

Structural determination and characterization of copper and zinc bis-glycinates with X-ray crystallography and mass spectrometry

2010 ◽  
Vol 63 (19) ◽  
pp. 3335-3347 ◽  
Author(s):  
Sanjit Konar ◽  
Kevin Gagnon ◽  
Abraham Clearfield ◽  
Charles Thompson ◽  
Jennifer Hartle ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Structural Determination ◽  
X Ray ◽  
X Ray Crystallography ◽  
Copper And Zinc

Synthesis and structural characterization of a magnesium phthalocyanine(3–) anion

2012 ◽  
Vol 16 (01) ◽  
pp. 154-162 ◽  
Author(s):  
Edwin W.Y. Wong ◽  
Daniel B. Leznoff
Keyword(s):  
Absorption Spectrum ◽  
Solid State ◽  
Single Crystal ◽  
Structural Characterization ◽  
Heterometallic Complex ◽  
State Structure ◽  
Solid State Structure ◽  
X Ray ◽  
X Ray Crystallography

The reduction of magnesium phthalocyanine (MgPc) with 2.2 equivalents of potassium graphite in 1,2-dimethoxyethane (DME) gives [K2(DME)4]PcMg(OH)(1) in 67% yield. Compound 1 was structurally characterized using single crystal X-ray crystallography and was found to be a monomeric, heterometallic complex consisting of a μ3-OH ligand that bridges a [MgIIPc3-]- anion to two potassium cations solvated by four DME molecules. An absorption spectrum of 1 confirms the Pc ligand is singly reduced and has a 3–charge. The solid-state structure of 1 does not indicate breaking of the aromaticity of the Pc ligand. Compound 1 is only the second Pc3- complex and the first reduced MgPc to be isolated and structurally characterized.

The direct electrochemical synthesis of some metal derivatives of lapachol

1997 ◽  
Vol 75 (5) ◽  
pp. 499-506 ◽  
Author(s):  
E.H. De Oliveira ◽  
G.E.A. Medeiros ◽  
C. Peppe ◽  
Martyn A. Brown ◽  
Dennis G. Tuck
Keyword(s):  
Electrochemical Oxidation ◽  
Copper Atom ◽  
Electrochemical Synthesis ◽  
Acetonitrile Solution ◽  
Triclinic Space Group ◽  
X Ray ◽  
Metal Anode ◽  
X Ray Crystallography ◽  
Metal Derivatives ◽  
Derivatives Of

The electrochemical oxidation of a sacrificial metal anode (M = Zn, Cd, Cu) in an acetonitrile solution of 2-hydroxy-3-(3-methyl-2-butenyl)-1,4-naphthoquinone, lapachol, C15H14O3 (=HL) gives ML2. The results are in keeping with earlier work on direct electrochemical synthesis in related systems. Adducts with 2,2′-bipyridine (bpy) and N,N,N′,N′-tetramethylethanediamine (tmen) have also been prepared. The structure of the 2,2′-bipyridine adduct of Cu(lapacholate)2 has been established by X-ray crystallography. The parameters are triclinic, space group [Formula: see text], a = 12.748(59) Å, b = 13.859(49) Å, c = 11.770(59) Å, α = 108.30(4)°, β = 108.08(3)°, γ = 68.94(3)°, Z = 2, R = 0.059 for 2256 unique reflections. The copper atom is in a distorted CuN2O2O2′ environment. The mechanism of the formation of this Cu(lapacholate)2 is discussed. Keywords: electrochemical synthesis, lapachol, X-ray crystallography, copper(II) complex.

Preparation and characterization of a new series of Cr(II) hydroborates

1995 ◽  
Vol 73 (7) ◽  
pp. 1126-1134 ◽  
Author(s):  
Michel Dionne ◽  
Shoukang Hao ◽  
Sandro Gambarotta
Keyword(s):  
Trinuclear Complex ◽  
Synthesis And Characterization ◽  
Crystal Data ◽  
X Ray ◽  
X Ray Crystallography ◽  
Quadruple Bond ◽  
Quadruple Bonds ◽  
Reaction Proceeds

The synthesis and characterization of a new series of mono-, di-, and trinuclear Cr(II) borohydride compounds is described. The reaction of CrCl2(TMEDA) with two equivalents of NaBH4 afforded the thermally unstable (TMEDA)Cr(BH4)2 (1), which was converted by treatment with pyridine into the octahedral monomeric (Py)4Cr(BH4)2 (2). The reaction proceeds via formation of an intermediate trinuclear complex {[(TMEDA)(Py)Cr(η2-BH4)]2[(Py)2Cr(η2-BH4)2]}(µ,η1-BH4)2 (3), which was isolated and characterized by X-ray crystallography. Reaction of 1 and 2 with both CO2 and RN=C=NR (R = Cy, iPr) afforded hydride insertion and formation of the corresponding diamagnetic lantern-type Cr(II) formate (HCO2)4Cr2Py2 (4) and formamidinate compounds [RNC(H)NR]2Cr2(µ-BH)4 (R = Cy (5a), iPr (5b)), respectively, with supershort Cr—Cr quadruple bonds. The structures of 1, 2, 3, and 5b were elucidated by X-ray analysis. Crystal data are as follows. 1: C6H24N2B2Cr, monoclinic, Cc, a = 8.517(2) Å, b = 15.921(5) Å, c = 9.624(2) Å, β = 115.59(1)°, Z = 4, R = 0.022, Rw = 0.029; 2: C28H44N4B2O2Cr, monoclinic, P21/n, a = 12.021(1) Å, b = 15.555(1) Å, c = 15.723(1) Å, β = 90.13(2)°, Z = 4, R = 0.074, Rw = 0.086; 3: C32H76N8B6Cr3, monoclinic, P21/n, a = 8.515(1) Å, b = 14.525(1) Å, c = 18.286(2) Å, β = 91.38(1)°, Z = 2, R = 0.051, Rw = 0.060; 5b: C21H49N6BCr2, monoclinic, C2/c, a = 17.000(1) Å, b = 9.033(1) Å, c = 19.160(1) Å, β = 105.579(9)°, Z = 4, R = 0.069, Rw = 0.078. Keywords: divalent chromium, borohydride, Cr—Cr quadruple bond.

Sign in / Sign up

Export Citation Format

Share Document