Crystal and molecular structure of [N(CH3)4]2[Mo2O2S2(S2)2]: a compound with two S22- ligands

Clegg, William; Mohan, N.; Mueller, A.; Neumann, Axel; Rittner, W.; Sheldrick, George M.

doi:10.1021/ic50209a046

Cited by 47 publications

(14 citation statements)

References 2 publications

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“…The distance for the sulfidic network found at 2.24 Å, is consistent with a mixture of short distances characteristic of terminal sulfido ligands (typically between 2.09 and 2.19 Å depending on the Mo oxidation state) and long distances around 2.28–2.35 Å associated to bridging sulfido ligands as encountered in (Mo 2 O 2 S 6 ) 2– moiety . In the case of sulfido bridging ligands, the mean Mo–Mo distance is found at 2.82 Å which is slightly longer than our refined Comp.2 distance (2.78 Å). We ascribe that the additional bridging by disulfido ligand of both Mo could be responsible for the Mo–Mo distance shortening.…”

Section: Discussionsupporting

confidence: 83%

“…The refined parameters for the oxidic network are fully consistent with Mo–ligand distances found in known hexavalent Mo-based compounds like (NH 4 ) 2 Mo 7 O 24 .4H 2 O with MoO t bond at 1.66 Å and oxo bridging ligand at 1.74 Å giving rise to Mo-Al and Mo-Mo distances at 3.06 and 3.42 Å. The distance for the sulfidic network found at 2.24 Å, is consistent with a mixture of short distances characteristic of terminal sulfido ligands (typically between 2.09 and 2.19 Å depending on the Mo oxidation state) and long distances around 2.28–2.35 Å associated to bridging sulfido ligands as encountered in (Mo 2 O 2 S 6 ) 2– moiety . In the case of sulfido bridging ligands, the mean Mo–Mo distance is found at 2.82 Å which is slightly longer than our refined Comp.2 distance (2.78 Å).…”

Section: Discussionsupporting

confidence: 80%

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Intermediate Species Revealed during Sulfidation of Bimetallic Hydrotreating Catalyst: A Multivariate Analysis of Combined Time-Resolved Spectroscopies

et al. 2017

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For the first time, the sulfidation process of a bimetallic NiMo catalyst supported on alumina has been followed by combining time-resolved laser Raman spectroscopy (LRS) and X-ray absorption spectroscopy (XAS) quasi simultaneously at both Ni and Mo K edges. Multivariate data analysis reveals that the thermal activation upon 15% H2S/H2 atmosphere of a dehydrated-calcined NiMo(VI) catalyst involves (i) a 5-stepped mechanism with oxysulfided or fully sulfided Mo intermediate species and (ii) a direct transformation of oxidic nickel species into NiS x and NiMoS ones. Complementary information extracted from LRS and Quick-XAS data permitted to identify at the early stage of the sulfidation the trimeric Mo(V/VI) oxysulfide species [Mo3(μ2O)4(μ2S)μ2{S2}(Ot)2(St)3] grafted to the support surface, which is quickly transformed into the Mo(IV) intermediate species [Mo3(μ3S)(μ2S)2μ2{S2}(Ot)2{S2}t]. Above 190 °C, the Mo(IV) second intermediate is transformed into Mo(IV)S3, itself transformed into the final Mo(IV)S2 at T > 220 °C. Thanks to the unambiguous comparison of sulfidation kinetics for both metals the incorporation of promoter into the extended sulfidic molybdenum-based phase has been unprecedentedly related to the formation of the MoS3 intermediate species.

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Section: Discussionsupporting

confidence: 83%

Section: Discussionsupporting

confidence: 80%

Intermediate Species Revealed during Sulfidation of Bimetallic Hydrotreating Catalyst: A Multivariate Analysis of Combined Time-Resolved Spectroscopies

et al. 2017

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“…The neutral-atom scattering factors were calculated from the analytical expression for the scattering factor curves. 16 The/'and/"components of anomalous dispersion were those of Cromer and Liberman17 and were included in the calculations for the Ru and P atoms. The agreement residuals are defined as R^= (|| 0| -|FC||)/2}|F0| and Ri…”

Section: Methodsmentioning

confidence: 99%

Studies of ruthenium(II) porphyrins containing tertiary diphosphine ligands, including the crystal structure of (5,10,15,20-tetraphenylporphinato)bis(bis(diphenylphosphino)methane)ruthenium(II)dichloromethane

Ball¹,

Domazetis²,

Dolphin³

et al. 1981

Inorg. Chem.

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“…The Mo(1)–Mo(2) bond distance is 2.8285(5) Å, or similar to those seen for [Mo 2 O 2 (μ-S) 2 (cys) 2 ] 2– and [Mo 2 O 2 (μ-S) 2 (citrate) 2 ] 6– . The dihedral angle of the [Mo 2 O 2 (μ-S) 2 ] 2+ core was calculated as 173°, or quite a bit wider than those in [Mo 2 O 2 (μ-S) 2 (DMF) 6 ](I) 2 , [Mo 2 O 2 (μ-S) 2 (S 2 )(DMF) 3 ], and (Me 4 N) 2 [Mo 2 O 2 (μ-S) 2 (S 2 ) 2 ] that fall between 150° and 160°.…”

Section: Resultsmentioning

confidence: 99%

Water-Soluble α-Amino Acid Complexes of Molybdenum as Potential Antidotes for Cyanide Poisoning: Synthesis and Catalytic Studies of Threonine, Methionine, Serine, and Leucine Complexes

et al. 2020

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Water-soluble complexes are desirable for the aqueous detoxification of cyanide. Molybdenum complexes with α-amino acid and disulfide ligands with the formula K[(L)Mo2O2(μ-S)2(S2)] (L = leu (1), met (2), thr (3), and ser (4)) were synthesized in a reaction of [(DMF)3MoO(μ-S)2(S2)] with deprotonated α-amino acids; leu, met, thr, and ser are the carboxylate anions of l-leucine, l-methionine, l-threonine, and l-serine, respectively. Potassium salts of α-amino acids (leu (1a), met (2a), thr (3a), and ser (4a)) were prepared as precursors for complexes 1–4, respectively, by employing a nonaqueous synthesis route. The ligand exchange reaction of [Mo2O2(μ-S)2(DMF)6](I)2 with deprotonated α-amino acids afforded bis-α-amino acid complexes, [(L)2Mo2O2(μ-S)2] (6–8). A tris-α-amino acid complex, [(leu)2Mo2O2(μ-S)2(μ-leu + H)] (5; leu + H is the carboxylate anion of l-leucine with the amine protonated), formed in the reaction with leucine. 5 crystallized from methanol with a third weakly bonded leucine as a bridging bidentate carboxylate. An adduct of 8 with SCN coordinated, 9, crystallized and was structurally characterized. Complexes 1–4 are air stable and highly water-soluble chiral molecules. Cytotoxicity studies in the A549 cell line gave IC50 values that range from 80 to 400 μM. Cyclic voltammetry traces of 1–8 show solvent-dependent irreversible electrochemical behavior. Complexes 1–4 demonstrated the ability to catalyze the reaction of thiosulfate and cyanide in vitro to exhaustively transform cyanide to thiocyanate in less than 1 h.

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Crystal and molecular structure of [N(CH3)4]2[Mo2O2S2(S2)2]: a compound with two S22- ligands

Cited by 47 publications

References 2 publications

Intermediate Species Revealed during Sulfidation of Bimetallic Hydrotreating Catalyst: A Multivariate Analysis of Combined Time-Resolved Spectroscopies

Intermediate Species Revealed during Sulfidation of Bimetallic Hydrotreating Catalyst: A Multivariate Analysis of Combined Time-Resolved Spectroscopies

Studies of ruthenium(II) porphyrins containing tertiary diphosphine ligands, including the crystal structure of (5,10,15,20-tetraphenylporphinato)bis(bis(diphenylphosphino)methane)ruthenium(II)dichloromethane

Water-Soluble α-Amino Acid Complexes of Molybdenum as Potential Antidotes for Cyanide Poisoning: Synthesis and Catalytic Studies of Threonine, Methionine, Serine, and Leucine Complexes

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