Tris(dimethylphenylphosphine)ruthenium(0) Complexes of n4-Coordinated Polycyclic Aromatic Hydrocarbons

2000 ◽  
Vol 53 (6) ◽  
pp. 507 ◽  
Author(s):  
Martin A. Bennett ◽  
Mark Bown ◽  
David C. R. Hockless
Keyword(s):  
Coordination Geometry ◽  
Crystal Data ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Tertiary Phosphine ◽  
X Ray ◽  
Tertiary Phosphines ◽  
Polycyclic Aromatic ◽  
R Value ◽  
Axial Site

From the reaction of [Ru2Cl3(PMe2Ph)6] Cl with the appropriate radical anions, yellow complexes of general formula [Ru(PMe2Ph)3(η4-arene)] [arene = naphthalene (C10H8) (1), anthracene (C14H10) (2), and triphenylene (C18H12) (3)] have been isolated in poor yield and characterized by elemental analysis, n.m.r. (1H, 13C, 31P) spectroscopy and single-crystal X-ray diffraction. Crystal data: (1), monoclinic, C2/c, a 31.096(8), b 12.012(4), c 17.078(8) Å, β 104.41(3)˚, V 6178(4) Å3, ? 8, refined to final R value of 0.032 with use of 3641 reflections [I > 3σ(I)]; (2), monoclinic, C2/c, a 55.909(4), b 14.348(5), c 17.573(5) Å, β 105.41(1)˚, V 13590(6) Å3, Z 16 (two molecules per asymmetric unit), refined to final R value of 0.049 with use of 7770 reflections [I > 3σ(I)]; (3), mono-clinic, Pn, a 9.377(3), b 12.229(3), c 15.975(3) Å, β 103.51(2)˚, V 1781.2 (7) Å3, Z 2, refined to final R value of 0.026 with use of 2830 reflections [I > 3σ(I)]. In each case, coordination of the zerovalent metal fragment Ru(PMe2Ph)3 to the diene section of one of the terminal rings causes the aromatic molecule to be folded by c. 40˚ at the outer carbon atoms of the diene. The coordination geometry about ruthenium is approximately square pyramidal, with the diene and two tertiary phosphines in the equatorial plane and the remaining tertiary phosphine in the axial site.

scholarly journals The Isomorphous Structures of Ammonium trans-Diiodobis(ethanedial-dioximato-(1–)-N,N′)cobaltate(III) and Ammonium trans-Diiodobis(ethanedial-dioximato-(1–)-N,N′)rhodate(III): Extended Metaloximate Chains with a Novel ···I–M–I···I–M–I··· Zigzagged Structure

1990 ◽  
Vol 45 (11) ◽  
pp. 1508-1512 ◽  
Author(s):  
Michel Mégnamisi-Bélombé ◽  
Bernhard Nuber
Keyword(s):  
Room Temperature ◽  
Ammonium Salts ◽  
Monoclinic Space Group ◽  
Hydroxyl Groups ◽  
Coordination Geometry ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Anionic Complexes ◽  
Complex Anions

The ammonium salts of the complex anions trans-diiodobis(ethanedial-dioximato)-cobaltate(III), [Col2(GH)2]-, and trans-diiodobis(ethanedial-dioximato)rhodate(III), [RhI2(GH)2]- (GH- = ethanedial dioximate or glyoximate), have been synthesized and their structures determined from single crystal X-ray diffraction data at room temperature. The crystals of the two salts are monoclinic, space group C2/c. NH4[CoI2(GH)2] (I) crystallizes as dark-brown prisms with a greenish reflectance; its crystal data are: C4H10Col2N5O4, Mr = 504.90; a = 8.910(6), b = 11.700(9), c = 11.691(6) Å; β = 93.55(5)°; V = 1216.4 Å3; Z = 4; Dc = 2.78 Mg m-3. NH4[RhI2(GH)2] (II) crystallizes as yellow-brown blocks with crystal data: C4H10I2N5O4Rh, Mr = 548.88; a = 9.038(4), b = 11.949(5), c = 11.770(3) Å; β = 95.54(3)°; V = 1265.16 A3; Z = 4; Dc = 2.87 Mg m-3. The two structures were refined to a final RW = 0.045 for 1209 observed independent reflections and 95 parameters for I, and to a final RW = 0.040 for 1922 observed independent reflections and 87 parameters for II. The coordination geometry around Co or Rh in the anionic complexes is a distorted (4 + 2) octahedron of four equatorial chelating N atoms and two apical iodides. The H atoms of the hydroxyl groups are involved, as usual, in intramolecular O—H—O bridges with uniform Ο···Ο separations of 2.582 Å for I, and 2.713 Å for II. The rectilinear I—Co—I or I—Rh—I triads form “infinite” zigzag chains extending parallel to the ab plane, with a weak I—I contact of 3.988 Å for I, and 4.010 Å for II.

Thiocarbonyl Complexes of Rhenium. Part I.

1993 ◽  
Vol 48 (6) ◽  
pp. 771-777 ◽  
Author(s):  
Ulrich Abram ◽  
Bernd Lorenz
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Rhenium Atom ◽  
Space Group ◽  
X Ray ◽  
Monomeric Complex ◽  
Structure Solution ◽  
R Value

Novel rhenium complexes with terminal thiocarbonyl groups have been synthesized from ReCl3(Me2PhP)3 and sodium diethyldithiocarbamate. mer-(Diethyldithiocarbamato)tris-(dimethylphenylphosphine)(thiocarbonyl)rhenium(I), mer-[Re(CS)(Me2PhP)3(Et2dtc)], and tris(diethyldithiocarbamato)(thiocarbonyl)rhenium(III), [Re(CS)(Et2dtc)3] have been studied by infrared and NMR spectroscopy, mass spectrometry and X-ray diffraction.mer-[Re(CS)(Me2PhP)3(Et2dtc)] crystallizes orthorhombic in the space group Pna21 with a = 1516.1(2), b = 2189.8(2) and c = 1035.6(1) pm. Structure solution and refinement converged at R = 0.042. The coordination geometry is a distorted octahedron. The Re—C bond length is found to be 184(2) pm.[Re(CS)(Et2dtc)3] crystallizes monoclinic in the space group P21/c with a = 962.2(6), b = 1744.0(2), c = 1537.4(6) pm and β = 96.21(1)°. The final R value is 0.028. In the monomeric complex the rhenium atom is seven-coordinate with an approximate pentagonal-bipyramidal coordination sphere and a rhenium-carbon distance of 181(1) pm.

Ideal and Real Structure of Ti5O4(PO4)4: X-ray and HRTEM Investigations

1998 ◽  
Vol 54 (6) ◽  
pp. 722-731 ◽  
Author(s):  
F. Reinauer ◽  
R. Glaum
Keyword(s):  
Crystal Structure ◽  
Electron Microscopy ◽  
Structure Refinement ◽  
Ideal Structure ◽  
Crystal Data ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
The Ideal

The crystal structure of pentatitanium tetraoxide tetrakis(phosphate), Ti5O4(PO4)4, has been determined and refined from X-ray diffraction single-crystal data [P212121 (No. 19), Z = 4, a = 12.8417 (12), b = 14.4195 (13), c = 7.4622 (9) Å (from Guinier photographs); conventional residual R 1 = 0.042 for 2556 Fo > 4σ(Fo ), R 1 = 0.057 for all 3276 independent reflections; 282 parameters; 29 atoms in the asymmetric unit of the ideal structure]. The structure is closely related to those of β-Fe2O(PO4)-type phosphates and synthetic lipscombite, Fe3(PO4)4(OH). While these consist of infinite chains of face-sharing MO6 octahedra, in pentatitanium tetraoxide tetrakis(phosphate) only five-eighths of the octahedral voids are occupied according to □3Ti5O4(PO4)4. Four of the five independent Ti4+O6 show high radial distortion [1.72 ≤ d(Ti−O) ≤ 2.39 Å] and a typical 1 + 4 + 1 distance distribution. The fifth Ti4+O6 is an almost regular octahedron [1.91 ≤ d(Ti−O) ≤ 1.98 Å]. Partial disorder of Ti4+ over the available octahedral voids is revealed by the X-ray structure refinement. High-resolution transmission electron microscopy (HRTEM) investigations confirm this result.

X-Ray Structure, Electrochemical and Electronic Spectroscopic Examination of Cobaloximatic Acid: Hydro-trans-diiodobis(ethanedioximato(1-)-N,N′)cobaltate(III). Extended Intermolecular O-H-O Bridging in the Solid

1993 ◽  
Vol 48 (10) ◽  
pp. 1360-1364
Author(s):  
Michel Mégnamisi-Bélombé ◽  
Irene Jokwi ◽  
Emmanuel Ngameni ◽  
Robert Roux ◽  
Bernhard Nuber
Keyword(s):  
Room Temperature ◽  
Strong Acid ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
Crystal Data ◽  
X Ray Diffraction ◽  
X Ray ◽  
Acidic Proton ◽  
Spectroscopic Examination

The structure of the cobaloximatic acid, hydro-trans-diiodobis(ethanedioximato(1-)-N,N′)cobaltate(III), has been determined by X-ray diffraction. Crystal data: C4H7CoI2N4O4, Mr = 487.87; monoclinic space group P21/a (C2h5 ); a = 10.795(7), b = 9.003(7), c = 11.881(6) Å; β = 97.29(6)°; V = 1145.35 Å3; Z = 4; dc = 2.83 Mg m-3. Rw (R) = 3.6 (3.9)% for 3064 observed independent reflections and 148 parameters. The coordination geometry around CoIII is a distorted (4 + 2) octahedron of four chelating equatorial N atoms and two apical iodides. The compound is most adequately formulated as a monovalent strong acid: H(Co(GH)2I2) (GH- = ethanedioximate or glyoximate). The H atoms of the oxime groups are involved in the usual intramolecular, as well as in much stronger intermolecular O-H-O bridgings (O ••• Ointramol = 2.613-2.631, O ••• Ointramol = 2.454 A). The “acidic” H atom of each molecule participates in the intermolecular bridging which extends throughout the structure, and propagates nearly parallel to the [101] crystallographic direction. The redox properties of the present compound were examined by cyclic voltammetry in acetonitrile solution at room temperature. Redox waves attributed to the reduction of CoIII and to the oxidation of I- were observed, along with a wave which may be linked to the reduction of the “acidic” proton

The Preparation, Spectroscopic Characterization and X-Ray Structure of the Salt [Pt(η1 -C6H9)(Cy2PCH2CH2PCy2)(PPh3)]HCO3·3H2O Containing the Discrete, Uncoordinated, Hydrogen-Bonded Dimeric Bicarbonate Dianion [(HCO3)(H2O)3]22-

1999 ◽  
Vol 52 (10) ◽  
pp. 949 ◽  
Author(s):  
Martin A. Bennett ◽  
Glen B. Robertson ◽  
Pramesh N. Kapoor
Keyword(s):  
Low Temperature ◽  
Spectroscopic Characterization ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Triclinic Space Group ◽  
X Ray ◽  
Cell Dimensions ◽  
R Value ◽  
Unit Cell Dimensions ◽  
Hydrogen Bonded

Reaction of the cyclohexyne–platinum(0) complex [Pt(η2-C6H8)(Cy2PCH2CH2PCy2)]* with water and CO2 in the presence of triphenylphosphine gives the bicarbonate salt of the (η1-cyclohexenyl)platinum(II) cation, [Pt(η1-C6H9)(Cy2PCH2CH2 PCy2)(PPh3)] [HCO3] · 3H2O, which has been characterized by n.m.r. spectroscopy and single-crystal X-ray diffraction at low temperature. Crystals are triclinic, space group P1– with unit cell dimensions a 20.315(2), b 12.782(1), c 10.694(1) Å, α 66.61(1), β 104.73(1), γ 102.11(1)˚, and Z 2. The structure was refined to a final R value of 0.036 with use of 7553 reflections [I > 3σ(I)]. The cation has the expected, somewhat distorted planar coordination geometry; the anion consists of discrete, hydrogen-bonded dimers [(HCO3)(H2O)3]22-.

Structural Studies of Technetium Complexes. XI. The Crystal Structure of Bis(tetraphenylarsonium) Bis(1,2-dicyanoethenedithiolato)nitridotechnetate(V)

1989 ◽  
Vol 42 (6) ◽  
pp. 875 ◽  
Author(s):  
GA Williams ◽  
J Baldas
Keyword(s):  
Crystal Structure ◽  
Monoclinic Space Group ◽  
Coordination Geometry ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Apical Position ◽  
Full Matrix ◽  
X Ray ◽  
R Value ◽  
Centrosymmetric Structure

The crystal structure of [AsPh4]2 [ TcN(mnt)2] ( mnt = 1,2-dicyanoethenedithiolate) has been determined by single-crystal X-ray diffraction methods at 21 � 1 C. Crystals are monoclinic, space group Pn , with a 11 369(2), b 15.530(2), c 14.421(3) � , P 97.58(2)�, and Z 2. Full-matrix least-squares refinement gave a final R value of 0.057 for 4232 independent reflections. The technetium atom in the [TcN( mnt )2]2- anion has square-pyramidal coordination geometry with the nitrido ligand in the apical position, Tc =N 1.59(1) � , and four Tc -S bonds with distances varying between 2.367(4) and 2.419(4) �. The Tc =N core is disordered about a pseudo-inversion centre, but unequal occupancies of the disordered sites preclude a centrosymmetric structure.

Experimental Charge Density and Electrostatic Potential of Triglycine

1998 ◽  
Vol 54 (4) ◽  
pp. 485-493 ◽  
Author(s):  
V. Pichon-Pesme ◽  
C. Lecomte
Keyword(s):  
Electrostatic Potential ◽  
Electron Density Distribution ◽  
Crystal Data ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
A Charge ◽  
Net Charges ◽  
Experimental Electron Density ◽  
Experimental Charge Density

The experimental electron density distribution in triglycine has been determined using single-crystal X-ray diffraction data at 123 K to a resolution of (sin θ/λ)max = 1.1 Å−1. Several multipolar pseudo-atom density refinements were performed against the 7238 observed data in order to estimate the net charges on the atoms. The electrostatic potential around the two molecules is calculated from the parameters derived from these refinements. A charge transfer between the two triglycine molecules of the asymmetric unit is discussed. Crystal data: C6H11N3O4, Mr = 189.2, triclinic, P1¯, Z = 4 (two molecules in the asymmetric unit), T = 123 K, a = 11.585 (1), b = 14.603 (2), c = 4.800 (4) Å, α = 89.28 (3), β = 95.55 (2), γ = 104.484 (8)°, V = 782.5 (7) Å3, Dx = 1.61 g cm−3, μ = 1.5 cm−1 for λMo = 0.7107 Å.

A three-dimensional ZnIIcoordination framework: poly[[μ2-(E)-1,2-bis(pyridin-4-yl)ethene][μ4-(E)-2,2′-(diazene-1,2-diyl)dibenzoato][μ2-(E)-2,2′-(diazene-1,2-diyl)dibenzoato]dizinc(II)]

2014 ◽  
Vol 70 (3) ◽  
pp. 277-280 ◽  
Author(s):  
Cai-Xia Yu ◽  
Feng Zhao ◽  
Min Zhou ◽  
Dan-Feng Zhi ◽  
Lei-Lei Liu
Keyword(s):  
Solid State ◽  
Coordination Polymer ◽  
Three Dimensional ◽  
Coordination Geometry ◽  
Two Dimensional ◽  
Tetrahedral Coordination ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Groups

In the title coordination polymer, [Zn2(C14H8N2O4)2(C12H10N2)]n, the asymmetric unit contains one ZnIIcation, two halves of 2,2′-(diazene-1,2-diyl)dibenzoate anions (denotedL2−) and half of a 1,2-bis(pyridin-4-yl)ethene ligand (denoted bpe). The three ligands lie across crystallographic inversion centres. Each ZnIIcentre is four-coordinated by three O atoms of bridging carboxylate groups from threeL2−ligands and by one N atom from a bpe ligand, forming a tetrahedral coordination geometry. Two ZnIIatoms are bridged by two carboxylate groups ofL2−ligands, generating a [Zn2(CO2)2] ring. Each loop serves as a fourfold node, which links its four equivalent nodesviathe sharing of fourL2−ligands to form a two-dimensional [Zn2L4]nnet. These nets are separated by bpe ligands acting as spacers, producing a three-dimensional framework with a 4664topology. Powder X-ray diffraction and solid-state photoluminescence were also measured.

Preparation and Structure of Dibromobis(N,N-diethyldithiocarbamato)-thionitrosyltechnetium(III)

1991 ◽  
Vol 44 (8) ◽  
pp. 1125 ◽  
Author(s):  
J Baldas ◽  
SF Colmanet ◽  
GA Williams
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Title Compound ◽  
Coordination Geometry ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
Trans Influence ◽  
R Value

The title compound, [Tc (NS)(S2CNEt2)2Br2], has been prepared by the reaction of [ TcN (S2CNEt2)2] with SOBr2, and its crystal structure has been determined by single-crystal X-ray diffraction methods at 23�1°C. Crystals are orthorhombic, space group Pnma , with a 14.864(7), b 15.857(7), c 8.938(4)Ǻ, and Z 4. Full-matrix least-squares refinement gave a final R value of 0.047 for 1685 independent reflections. The technetium atom is seven-coordinate with a distorted pentagonal- bipyramidal coordination geometry. The thionitrosyl ligand and a bromo ligand occupy the axial positions, with the thionitrosyl group exerting a small trans influence with Tc-Brtrans 2.595(1) and Tc-Brcis 2.564(1)Ǻ. The coordination of the thionitrosyl group is essentially linear with Tc -N=S 177.2(7)°, Tc -N 1.754(9), and N=S 1.504(9)Ǻ.

A new potential NLO compound with a supramolecular layered structure: aqua(hexamethylenetetramine-κN)(iminodiacetato-κ3O,N,O′)copper(II)

2012 ◽  
Vol 68 (8) ◽  
pp. m206-m208 ◽  
Author(s):  
Jiao-Jiao He ◽  
Wen-Xiang Chai ◽  
Li Song ◽  
Feng Niu ◽  
Xiao-Bin Fang
Keyword(s):  
Coordination Geometry ◽  
Two Dimensional ◽  
Asymmetric Unit ◽  
X Ray Diffraction ◽  
Absorption Properties ◽  
X Ray ◽  
Bond Forming ◽  
Dimensional Network ◽  
Powder Samples ◽  
Coordinated Water

In the noncentrosymmetric title compound, [Cu(C4H5NO4)(C6H12N4)(H2O)] or [Cu(IDA)(HMTA)(H2O)], where IDA is iminodiacetate and HMTA is hexamethylenetetramine, the asymmetric unit consists of a whole mononuclear neutral molecule, where the CuIIcation is coordinated by two carboxylate O atoms and one N atom from the IDA ligand, by one N atom from the HMTA ligand and by the O atom of the coordinated water molecule, giving rise to a CuN2O3distorted square-pyramidal coordination geometry. The IDA and HTMA ligands adopt terminal tri- and monocoordinated modes, respectively. All adjacent molecules within theacplane are connected to each otherviatwo pairs of O—H...O and one N—H...O hydrogen bond, forming a (4,4) supramolecular two-dimensional network. In the unit cell, these layers stack alternately in an …ABABAB… sequence along thebaxis. The optical absorption properties of this compound have been studied on powder samples, which had previously been examined by powder X-ray diffraction.

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