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ABSTRACT: Two dicobalt compounds containing Co–Co bonds with DAniF ligands (DAniF=N,N′-di-p-anisylformamidinate) were synthesized and characterized by X-ray crystallography. One has a typical tetragonal paddlewheel
structure, Co2(DAniF)4 (1), while the other one has a rare trigonal paddlewheel structure with three formamidinate ligands spanning a low oxidation
state in the Co23+ unit in Co2(DAniF)3 (2). The singly bonded Co–Co distance in the Co24+ unit in 1 is 2.3580(16)Å while the Co–Co bond distance in 2 is 2.3773(5)Å. The average torsion angles are 10.46° and 2.34° for 1 and 2, respectively. Compound 1 is diamagnetic but 2 is paramagnetic as shown by the 1H NMR spectra.
Journal of Cluster Science 05/2012; 19(1):89-97. · 0.92 Impact Factor
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ABSTRACT: Oxidation of α-[Mo2(cis-DAniF)2]3(μ-F)6 with an excess of FeCp2BF4 produces the triply oxidized species {β-[Mo2(cis-DAniF)2]3(μ-F)6}(BF4)3. During the oxidation process, the conformation in the α triangular species changes from an arrangement in which two dimetal
units are parallel and the third one essentially orthogonal to a structure in which all three dimetal units are parallel.
Furthermore, upon removal of three electrons, the Mo–Mo distances increase by about 0.05–0.06Å and the Mo–F bond distances
decrease by 0.04Å. The structural data, as well as EPR, are consistent with an electronically localized system and a decrease
in bond order from 4 to 3.5 for each dimetal unit.
KeywordsMetal–metal bonds-Crystal structures-EPR-Electronic communication-Interconversion of isomers-Molecular triangles
Journal of Cluster Science 04/2012; 21(3):301-312. · 0.92 Impact Factor
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ABSTRACT: Three rare compounds have been synthesized and structurally characterized; these species have paddlewheel structures and Re(2)(7+) cores surrounded by four bicyclic guanidinates and two axial ligands along the Re-Re axis. Each possesses a formal bond order of 3.5 and a σ(2)π(4)δ(1) electronic configuration that entails the presence of one unpaired electron for each compound. The guanidinate ligands characterized by having CH(2) entities and a central C(N)(3) unit that joins two cyclic units--one having two fused 6-membered rings (hpp) and the other having a 5- and a 6-membered ring fused together (tbn)--allowed the isolation of [Re(2)(tbn)(4)Cl(2)]PF(6), 1, [Re(2)(tbn)(4)Cl(2)]Cl, 2, and [Re(2)(hpp)(4)(O(3)SCF(3))(2)](O(3)SCF(3)), 3. Because of the larger bite angle of the tbn relative to the hpp ligand, the Re-Re bond distances in 1 and 2 (2.2691(14) and 2.2589(14) Å, respectively) are much longer than that in 3 (2.1804(8) Å). Importantly, electron paramagnetic resonance (EPR) studies at both X-band (~9.4 GHz) and W-band (112 GHz) in the solid and in frozen solution show unusually low g-values (~1.75) and the absence of zero-field splitting, providing direct evidence for the presence of one metal-based unpaired electron for both 1 and 3. These spectroscopic data suggest that the unsymmetrical 5-/6-membered ligand leads to the formation of isomers, as shown by significantly broader EPR signals for 1 than for 3, even though both compounds possess what appears to be similar ideal crystallographic axial symmetry on the X-ray time scale.
Inorganic Chemistry 04/2012; 51(9):5257-63. · 4.60 Impact Factor
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ABSTRACT: A long-sought metal-metal bonded species with an M(2)(8+) core has been structurally characterized. The diamagnetic compound {[Re(2)(hpp)(3)(OH)(O(3)SCF(3))](2)(μ-O)(2)}(O(3)SCF(3))(2), 2, has two σ(2)π(4) electron-poor triple-bonded Re(2)(8+) units embraced by three bicyclic guanidinate ligands (hpp) and axial OH and triflate groups; the two dimetal units are held together by bridging oxo-groups.
Chemical Communications 08/2011; 47(31):8940-2. · 6.17 Impact Factor
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ABSTRACT: Four Re(2)(6+) paddlewheel compounds with equatorial bicyclic guanidinate ligands and two monodentate anions in axial positions show a large change in the metal-metal distance that depends on the bite angle of the ligands and whether there are pi interactions between the dimetal unit and the axial ligands. These processes are accompanied by significant changes in the redox behavior. The two pairs of compounds that have been synthesized are Re(2)(tbn)(4)Cl(2), 1, and Re(2)(tbn)(4)(SO(3)CF(3))(2), 2, as well as Re(2)(tbo)(4)Cl(2), 3, and Re(2)(tbo)(4)(SO(3)CF(3))(2), 4, where tbn is the anion of a bicyclic guanidinate with six- and five-membered rings (1,5,7-triazabicyclo[4.3.0]non-6-ene) and tbo is an analogous species with two five-membered rings (the anion of 1,4,6-triazabicyclo[3.3.0]oct-4-ene). For both 1 and 2 as well as for 3 and 4, the metal-metal distances are shorter for the triflate species than for the chloride analogues because of the π interactions of the Cl with the π bonds of the triply bonded Re(2)(6+) cores compounded by a small but symmetry allowed interaction between the antisymmetric combination of the filled σp orbitals of the chlorine atom and the empty σ* orbital of the metal atoms. In addition there is a significant increase in the Re-Re distance from that in the six/five tbn-membered ring to the five/five-membered tbo species. Electrochemical measurements show two redox processes for each set of compounds corresponding to the uncommon Re(2)(6+) → Re(2)(7+) and Re(2)(7+) → Re(2)(8+) processes, which are strongly affected by the bite angle of the guanidinate ligand as well as the ability of the axial ligands to interact with the π orbitals of the dirhenium unit. For 1 and 3, the first redox couples are at 0.146 and 0.487 V, respectively, while for 2 and 4 these are at 0.430 and 0.698 V, respectively.
Inorganic Chemistry 02/2011; 50(4):1258-64. · 4.60 Impact Factor
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Ryan E Da Re,
Judith L Eglin,
Christin N Carlson,
Kevin D John,
David E Morris,
William H Woodruff,
James A Bailey,
Enrique Batista,
Richard L Martin,
F Albert Cotton,
Elizabeth A Hillard, Carlos A Murillo,
Alfred P Sattelberger,
Robert J Donohoe
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ABSTRACT: We report an investigation of complexes of the type M(2)(dmp)(4) (M = Mo, Cr; dmp = 2,6-dimethoxyphenyl) using resonance Raman (RR) spectroscopy, Cr isotopic substitution, and density functional theory (DFT) calculations. Assignment of the Mo-Mo stretching vibration in the Mo(2) species is straightforward, as evidenced by a single resonance-enhanced band at 424 cm(-1), consistent with an essentially unmixed metal-metal stretch, and overtones of this vibration. On the other hand, the Cr(2) congener has no obvious metal-metal stretching mode near 650-700 cm(-1), where empirical predictions based on the Cr-Cr distance as well as DFT calculations suggest that this vibration should appear if unmixed. Instead, three bands are observed at 345, 363, and 387 cm(-1) that (a) have relative RR intensities that are sensitive to the Raman excitation frequency, (b) exhibit overtones and combinations in the RR spectra, and (c) shift in frequency upon isotopic substitution ((50)Cr and (54)Cr). DFT calculations are used to model the vibrational data for the Mo(2) and Cr(2) systems. Both the DFT results and empirical predictions are in good agreement with experimental observations in the Mo(2) complex, but both, while mutually consistent, differ radically from experiment in the Cr(2) complex. Our experimental and theoretical results, especially the Cr isotope shifts, clearly demonstrate that the potential energy of the Cr-Cr stretching coordinate is distributed among several normal modes having both Cr-Cr and Cr-ligand character. The general significance of these results in interpreting spectroscopic observations in terms of the nature of metal-metal multiple bonding is discussed.
Journal of the American Chemical Society 02/2010; 132(6):1839-47. · 9.91 Impact Factor
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ABSTRACT: Syntheses and characterization of two Ru(2)(6+) paddlewheel compounds having very different magnetic behavior are reported. The compounds Ru(2)(tbn)(4)Cl(2), 1, and Ru(2)(tbo)(4)Cl(2), 2 (where tbn = the anion of 1,5,7-triazabicyclo[4.3.0]non-6-ene and tbo = the anion of 1,4,6-triazabicyclo[3.3.0]oct-4-ene), have four equatorial bicyclic guanidinate ligands and two chloride ions in axial positions. They show large disparity in Ru-Ru distances of about 0.11 A (2.389(3) and 2.499(3) A at 30 K for 1 and 2, respectively) that is attributed to the divergence in the bite angle of the ligand. Variable temperature structural data show no significant changes in the Ru-Ru distances between 30 and 213 K suggesting that the electronic structure remains unchanged in this temperature range for both compounds. Magnetic studies of 1 indicate there are two unpaired electrons at room temperature but the compound behaves as essentially diamagnetic at approximately 2 K. Compound 2 is non-magnetic across all temperatures in the range of 2 to 300 K. Density functional theory calculations suggest a pi(4)pi*(4)delta(2) electronic configuration for 2, while the magnetic behavior and structural data for 1 are consistent with a sigma(2)pi(4)delta(2)pi*(2) electronic configuration. This shows the importance of the ligand bite angle in determining the electronic configuration of the diruthenium unit and a way to tune magnetic behavior.
Inorganic Chemistry 02/2010; 49(6):3051-6. · 4.60 Impact Factor
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ABSTRACT: Variable temperature structural and EPR studies are reported on the paddlewheel compound [Os(2)(hpp)(4)Cl(2)]PF(6), 1, (hpp = the anion of the bicyclic guanidine 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidine) that contains a rare M(2)(7+) species, with the goal of determining whether the unpaired electron resides in a metal- or ligand-based molecular orbital. Crystallographic studies show that the Os-Os distance in 1 remains essentially unchanged from 213 to 30 K, which is consistent with no changes in electronic structure in this range of temperature. It is noteworthy that the metal-metal distance in 1 is about 0.05 A shorter than that in the precursor Os(2)(hpp)(4)Cl(2), which is consistent with the loss of an electron in a delta* orbital. EPR spectra of 1 were measured in dilute frozen solution, powder, and single crystals. The spectra were observable only below about 50 K, with an exceptionally large line width, approximately 3,750 gauss, for a powdered sample, due to dipolar interactions and to short relaxation times. There is a very small average g value of approximately 0.750 and a cylindrical symmetry about the Os-Os bond. These data are consistent with the unpaired electron orbital having a large L value, such as that of a delta* orbital. The combination of X-ray structural data, the short relaxation time, and the magnetic data provide strong evidence that the unpaired electron in this nine-electron Os(2)(7+) species is localized in a metal-based orbital with this electron residing predominantly in a delta* orbital rather than in a pi* orbital and, thus, having an electronic configuration of sigma(2)pi(4)delta(2)delta*.
Inorganic Chemistry 11/2009; 49(1):319-24. · 4.60 Impact Factor
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ABSTRACT: Depending on conditions the reactions of [Mo(2)(cis-DAniF)(2)(NCCH(3))(4)](BF(4))(2) (DAniF = N,N'-di-p-anisylformamidinate) with solutions containing thiocyanate anions lead to two compounds: a quadruple-bonded dinuclear species 1, (Bu(n)(4)N)(2)[Mo(2)(cis-DAniF)(2)(NCS)(4)], and a molecular pair 3, [Mo(2)(cis-DAniF)(2)](2)(mu(1,3)-NCS)(4). The latter has a cuboidal structure having two (cis-DAniF)(2)Mo(2)(2+) units, [Mo(2)], with four thiocyanate groups bridging two [Mo(2)] units in an end-to-end fashion in which the N and S atoms serve as the bridging units. On the contrary, the structure of the cyanate isomer, [Mo(2)(cis-DAniF)(2)](2)(mu(1,1)-NCO)(4) (2), shows an end-on binding of the cyanate linkers. Various physical measurements of 2 and its oxidized species 2.PF(6) indicate that there is strong electronic communication between the two dimetal cores. For 1, two reversible oxidation processes were observed in the cyclic voltammogram corresponding to the successive oxidation to 1(+) and an uncommon 1(2+) species that has a triple-bonded Mo(2)(6+) core. DFT calculations indicate that the antibonding character between the Mo-Mo delta orbitals and thiocyanate p orbitals plays a very important role in elevating the HOMO delta orbital energy that allows formation of the dication. A selenium isomer of 3 was also studied. In both the thiocyanate and selenocyanate bridged dimers of dimers, in which the pseudohalide bridges bind the two dimetal units in an end-to-end fashion, long separations between the dimetal units are observed, and these generate very weak electronic interactions.
Inorganic Chemistry 11/2009; 48(24):11755-66. · 4.60 Impact Factor
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ABSTRACT: A dimer of dimers containing two quadruply bonded [Mo(2)(DAniF)(3)](+) units (DAniF = N,N'-di(p-anisyl)formamidinate) linked by the S-donor linker, dimethyldithiooxamidate was synthesized, structurally characterized, and electronic communication was probed. The core of [Mo(2)(DAniF)(3)](2)(C(2)S(2)N(2)Me(2)), 1, formed by the Mo(2)NSC(2)SNMo(2) atoms shows two fused but non planar six-membered rings, which differs from that of the beta form of dimethyloxamidate analogue that has a heteronaphthalene-type structure (Cotton, F. A.; Liu, C. Y.; Murillo, C. A.; Villagran, D.; Wang, X. J. Am. Chem. Soc. 2004, 126, 14822). For these two analogous compounds electronic coupling between the two [Mo(2)] units, as determined by electrochemical measurements, diminishes considerably upon replacement of O-donor by S-donor atoms (DeltaE(1/2) = 531 mV and 440 mV, respectively). This suggests that the non planar conformation of the linker in 1 hampers a pathway leading to pi conjugation. Density functional theory (DFT) calculations show that the highest occupied molecular orbitals HOMO-HOMO-1 energy gap of 0.12 eV for 1 is much smaller than that of 0.61 eV for the O-donor analogue, which is consistent with the electrochemical data.
Inorganic Chemistry 11/2009; 48(24):11847-52. · 4.60 Impact Factor
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ABSTRACT: Oxidation of the molybdate-linked pair having two quadruply bonded Mo(2)(4+) units, [Mo(2)(DAniF)(3)](2)(micro(2)-MoO(4)), (DAniF = N,N'-di-(p-anisyl)formamidinate) leads to the formation of a species consisting of three oxidized Mo(2)(5+) units connected by two micro(3)-MoO(4)(2-) dianions, {[Mo(2)(DAniF)(3)](3)(micro(3)-MoO(4))(2)}(2+). This cation displays overall D(3) point group symmetry due to a slight twisting of the three Mo(2)(5+) units about the threefold symmetry axis. This distortion removes all mirror symmetry but preserves all C(2) axes orthogonal to the unique C(3) axis. Cyclic voltammetry of {[Mo(2)(DAniF)(3)](3)(micro(3)-MoO(4))(2)}(2+) in CH(2)Cl(2) reveals three reversible one-electron redox processes, corresponding to successive reduction of each of the three Mo(2)(5+) units, with DeltaE(1/2) separations of 0.36 V and 0.41 V.
Dalton Transactions 04/2008; · 3.84 Impact Factor
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ABSTRACT: Two neutral compounds having [Mo2] units linked by squarate dianions, [Mo2(DAniF)3]2(mu4-C4O4) (DAniF = N,N'-di(p-anisyl)formamidinate) (1) and [Mo2(DmCF3F)3]2(mu4-C4O4) (DmCF3F = N,N'-di(m-trifluoromethylphenyl)formamidinate) (2), as well as the singly oxidized compound {[Mo2(DmCF3F)3]2(mu4-C4O4)}SbF6 (3) and the doubly oxidized species {[Mo2(DAniF)3]2(mu4-C4O4)}(TFPB)2 (TFPB = [B(3,5-(CF3)2C6H3)4]-) (4), were synthesized and structurally characterized. Electrochemical measurements of the two neutral species showed only very weak electronic interactions between the two dimolybdenum units linked by the squarate anion in contrast to what was observed in dioxolene analogues having C6 instead of C4 rings (J. Am. Chem. Soc. 2006, 128, 3281) which led to differences in comproportionation constants of over 108. In the squarate species, the pi electrons are localized within the carbonyl and dimetal units in the heterometallic six-membered Mo2O2C2 rings to minimize the antiaromaticity in the central C4 square. The oxidized species 3 and 4 are electronically localized in the time scale of the physical measurements. Calculations at the DFT level suggested that the energy mismatch of the frontier orbitals of the linker and dimetal units contributes to the weak communication between the Mo2 units. For the doubly oxidized complex 4, DFT calculations gave a J value of -130 cm(-1) which suggests that the two unpaired electrons are only weakly antiferromagnetically coupled, as shown by magnetic studies (J = -121 cm(-1)).
Inorganic Chemistry 02/2008; 47(1):219-29. · 4.60 Impact Factor
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ABSTRACT: Ligands derived from N-CH(3) substituted benzoquinonemonoimines are exceedingly good facilitators of electronic communication between two quadruply bonded dimolybdenum units and provide record values for comproportionation constants.
Chemical Communications 02/2008; · 6.17 Impact Factor
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ABSTRACT: An extended metal atom chain (EMAC) compound with an unsymmetrical trinickel core and the formula [Ni3(dpa)4(CH3CN)](PF6)2·2CH2Cl2 (1·2CH2Cl2, dpa is the anion of 2,2′-dipyridylamine) has the central Ni atom in an essentially square-planar configuration. Besides having four equatorial nitrogen atoms, the two terminal metal centers have axial interactions that are notably different with one having a strongly bound acetonitrile molecule with a Ni(3)–N(3) distance of 2.108(5) Å while the other unit has a very weak interaction with an axial PF6 anion [Ni(1)···F(1) separation of 2.690 Å]. In these outer units, the Ni(3) atom is pulled out of the idealized plane of the four equatorial nitrogen atoms by 0.239 Å, while in the one with an axial PF6 anion the metal atom is pulled from the plane of the equatorial nitrogen atoms by only 0.097 Å. In 1 there are two unpaired electrons and an S = 1 state prevails from ca. 25 to 300 K. This magnetic behavior differs considerably from that of symmetrical trinickel EMACs with two strongly pyramidal terminal nickel atoms. A discussion of the effect of various axial ligands on the geometry of the terminal nickel atoms is provided. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008)
European Journal of Inorganic Chemistry. 01/2008; 2008:5257–5262.
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ABSTRACT: A tetranuclear cluster containing two quadruply bonded cis-Mo2(DAniF)2 units (DAniF = N,N'-di-p-anisylformamidinate) linked by four hydroxide groups (1) was obtained by hydrolysis of [Mo2(cis-DAniF)2](mu-OCH3)4. Analogous compounds linked by two bidentate bridges (o-O2C6H4 for 2, o-O2C10H6 for 3, and o-S2C6H4 for 4) were synthesized by direct assembly of the corner species precursor [Mo2(cis-DAniF)2(NCCH3)4](BF4)2 and the respective protonated ligands. All four compounds were characterized by X-ray crystallography. Cyclic voltammograms of the O-linked compound 2 and the S analogue 4 show two reversible one-electron-oxidation processes with potential separations (DeltaE(1/2)) of 474 and 776 mV, respectively. The large increase of about 300 mV in DeltaE(1/2) for the S analogue relative to that of the O compound is consistent with a large increase in electronic communication. This enhancement occurs despite the increase of ca. 0.45 A in nonbonding separation between the midpoints of the Mo2 units, which changes from 3.266 A in 2 to 3.72 A in 4, and the increase of ca. 0.4 A in M-E distances as E changes from O to S. Density functional theory calculations show that the increase in electronic communication between the metal centers in 4 is due to a superexchange pathway involving d and p orbitals in the linker E atoms that is less important in 2.
Inorganic Chemistry 11/2007; 46(22):9294-302. · 4.60 Impact Factor
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Journal of the American Chemical Society 11/2007; 129(42):12666-7. · 9.91 Impact Factor
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ABSTRACT: Six very soluble paddlewheel compounds containing Mo2n+ units, n = 4, 5, 6, and two alkyl-substituted bicyclic guanidinate ligands have been synthesized. The quadruply bonded complexes with n = 4, Mo2(TMhpp)4 and Mo2(TEhpp)4, (TMhpp = the anion of 3,3,9,9-tetramethyl-1,5,7-triazabicyclo[4.4.0]dec-4-ene and TEhpp = the anion of 3,3,9,9-tetraethyl-1,5,7-triazabicyclo[4.4.0]dec-4-ene) are easily oxidized. The electrode potentials in THF are -1.08 and -1.17 V vs. Ag/AgCl, respectively, for the Mo(2)(5+/4+) couple. These potentials are in accord with the low ionization potentials for the quadruply bonded compounds. Because of the high solubility of the Mo(2)(4+) compounds in most common organic solvents they are attractive candidates for use as strong reducing agents in homogeneous systems.
Dalton Transactions 10/2007; · 3.84 Impact Factor
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ABSTRACT: Structures of compounds having two dimolybdenum units Mo2(DAniF)3+ (DAniF = N,N'-di-p-anisylformamidinate) connected by unsubstituted oxamidate (1) and dithiooxamidate (2) linkers are isomorphous, and the cores of the molecules are planar because of two intramolecular hydrogen bonds within the linkers. Molecular mechanics calculations show a barrier of rotation along the C-C bond of approximately 10 kcal x mol(-1), which suggests that planar conformations are also expected in solution. Changing the two oxygen atoms in the linker of 1 to sulfur atoms results in a significant enhancement of the electronic coupling between the dimetal units (Delta(E1/2) = 204 mV for 1 and 407 mV for 2). The electronic spectrum of 2 shows an intense low energy (600 nm) metal-to-ligand charge transfer (MLCT) band, whereas that for 1 shows only a weak absorption band at 460 nm. DFT calculations on models 1' and 2', in which the anisyl groups were replaced by hydrogen atoms, show that the energy of the pi* orbital of the linker is much lower for 2'. This allows dpi-ddelta interactions from the electrons in the delta orbitals of the Mo2 unit to the sulfur atom that in turn facilitates an electron hopping pathway.
Inorganic Chemistry 10/2007; 46(19):7840-7. · 4.60 Impact Factor
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ABSTRACT: Hydride anions, H-, have been found to cause the assembly of dimolybdenum units [Mo2(cis-DAniF)2]2+, DAniF = N,N'-di(p-anisyl)formamidinate, forming a tetranuclear complex [Mo2(cis-DAniF)2]2(mu-H)4 (1) with an Mo4H4 core that may be described as an elongated tetrahedron in which the H atoms are along the four long edges of such tetrahedron and the Mo2 units are along the short edges. The two quadruply bonded dimolybdenum units, separated by only 2.718 A, are essentially orthogonal. This gives the shortest [Mo2]...[Mo2] distance known for complexes with multiple dimolybdenum units. DFT calculations indicate that the energy of a cuboidal isomer is only 3.8 kcal/mol above that of 1, but such an isomer has not been observed.
Inorganic Chemistry 09/2007; 46(17):6858-63. · 4.60 Impact Factor
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ABSTRACT: Two compounds with quadruply bonded Mo2(4+) species having isonicotinate ligands bound through the carboxylate group have been designed to act as anglers by luring metal-containing Lewis acids to bind to the N-pyridyl group. The corner pieces are Mo2(DAniF)3(O2CC5H4N) and cis-Mo2(DAniF)2(O2CC5H4N)2, DAniF=N,N'-di(p-anisyl)formamidinate. The heterometallic molecular rods -Ni(acac)2-and-Rh2(O2CCH3)4- were made by reaction of with Ni(acac)2 and the metal-metal bonded species Rh2(O2CCH3)4, respectively. In these compounds either a mononuclear or a dinuclear species are sandwiched between two molecules of . The cisoid compound has been employed for the synthesis of a molecular rhombus, [-Zn(Cl2)]2. The successful syntheses and isolation of show that the use of corner pieces with angler groups is an excellent approach for making heterometallic supramolecular compounds having a combination of metal-metal bonded units and other metal species.
Dalton Transactions 07/2007; · 3.84 Impact Factor
