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The crystal structure of Hexakis(diethylamido)dimolybdenum, Mo2(NEt2)6

  • Tobias Brauner , Christoph Wagner ORCID logo and Kurt Merzweiler ORCID logo EMAIL logo
Published/Copyright: May 18, 2021
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Zeitschrift für Kristallographie - New Crystal Structures
From the journal Zeitschrift für Kristallographie - New Crystal Structures Volume 236 Issue 4

Abstract

C24H60Mo2N6, trigonal, R3‾ (no. 148), a = 16.7680(8) Å, c = 9.7523(4) Å, V = 2374.7(2) Å3, Z = 3, Rgt(F) = 0.0205, wRref(F2) = 0.0517, T = 213 K.

CCDC no.: 2080037

The molecular structure is shown in the figure (Hydrogen atoms were omitted for clarity).

Table 1:

Data collection and handling.

Crystal:Yellow needle
Size:0.56 × 0.07 × 0.07 mm
Wavelength:Mo Kα radiation (0.71073 Å)
μ:0.81 mm−1
Diffractometer, scan mode:STOE IPDS 2, ω-scan
θmax, completeness:26.0°, >99%
N(hkl)measured, N(hkl)unique, Rint:7139, 1039, 0.062
Criterion for Iobs, N(hkl)gt:Iobs > 2 σ(Iobs), 1007
N(param)refined:49
Programs:SHELX [11], [12], Olex2 [13], Diamond [14], X-Area [15]
Table 2:

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2).

AtomxyzUiso*/Ueq
Mo0.66670.33330.44755 (2)0.02368 (11)
N0.73519 (10)0.46460 (10)0.49924 (15)0.0315 (3)
C10.76858 (15)0.48126 (14)0.6415 (2)0.0414 (4)
H10.72920.42630.69610.050*
H20.76240.53220.67890.050*
C20.86725 (17)0.50409 (19)0.6573 (3)0.0597 (6)
H30.88430.51410.75340.072*
H40.87380.45340.62290.072*
H50.90710.55940.60560.072*
C30.76863 (14)0.54991 (13)0.4211 (2)0.0401 (4)
H60.75270.53440.32440.048*
H70.83590.58540.42770.048*
C40.72989 (19)0.61003 (16)0.4690 (3)0.0585 (6)
H80.75490.66510.41280.070*
H90.66330.57610.46050.070*
H100.74670.62720.56400.070*

Source of material

Mo2(NEt2)6 was synthesized from LiNEt2 and MoCl3(THF)3 [1] by a slightly modified method according to Chisholm et al. [2]. Yellow single crystals of Mo2(NEt2)6 were obtained by sublimation at 150 °C and 10-5 mbar.

1H-NMR (400 MHz, C6D6): δ [ppm] = 1.11 (t, 36H, CH33J(HH) = 7.0 Hz); 3.50 (q, 24H, CH23J(HH) = 7.0 Hz), 13C-NMR (100 MHz, C6D6): δ [ppm] = 15.5 (s, 12 C, CH3); 51.9 (s; 12 C; CH2).

Experimental details

Details of the crystal structure determination are collected in Table 1 and the results of structure calculation are listed in Table 2 with atomic coordinates.

The hydrogen atoms were placed on calculated positions and refined with a riding model. Their Uiso values were set to 1.2 Ueq for CH2 groups and 1.5 for CH3 groups of the parent carbon atoms.

Comment

Since the first synthesis of Mo2(CH2SiMe3)6 around five decades ago [3], a large number of Mo2R6 compounds comprising Mo–Mo triple bonds were synthesized and characterized by X-ray diffraction methods [4]. However, in the case of dialkylamide derivatives Mo2(NR2)6 X-ray structure determinations apart from that of the parent compound Mo2(NMe2)6 [5] are still rare. Some more structural data are available from complexes with μ2-bridging bis-amido ligands like Mo2(R′NCH2CH2NR′)3 (R′ = Me [6], R′ = i–Pr [7]), and mixed organyl/dialkylamide ligands, e.g. Mo2R′2(NMe2)4 (R′ = benzyl, o-tolyl, p-tolyl [8], ethyl [9]).

The preparation of the title compound Mo2(NEt2)6 was reported in 1976 [2]. Pale yellow single crystals suitable for X-ray diffraction were grown by sublimation in high vacuum.

Mo2(NEt2)6 crystallizes in the trigonal system, space group R3‾ with three formula units per unit cell. The crystal structure consists of discrete molecules Mo2(NEt2)6 without any unusual short intermolecular contacts. The Mo2(NEt2)6 units are situated around a crystallographic center of inversion (Wyckoff site 3a). The asymmetric unit comprises one third of the molecule with the Mo atom situated on the 3‾ axis and the remaining atoms at general positions. Thus, the Mo2(NEt2)6 unit exhibits crystallographically imposed S6 point symmetry, which implies a staggered conformation of the Mo(NEt2)3 fragments. Generally, the staggered conformation is preferred for Mo2R6 compounds with terminally binding ligands R [4]. In the case of μ2-bridging ligands steric strain usually forces eclipsed arrangements, i.e. Mo2(RNCH2CH2NR)3 [10] (R = Me [5], i–Pr [6]).

Mo2(NEt2)6 exhibits a Mo–Mo distance of 2.2277(4) Å which is close to that in Mo2(NMe2)6 (2.21(2) Å) [1]. Comparable distances are found in the dimolybdenum hexaalkoxides Mo2(OR)6 R = CH2tBu [9] with 2.222(2) Å and R = C(CF3)2CH3 [10] with 2.2263(4) Å. Furthermore, the Mo–N distances (1.9723(1) Å) and the N–Mo–N angles (113.70(4)°) are in accordance with the observations in Mo2(NMe2)6 (1.97(2)–2.00(1) Å and (113.5(2)–115.2(2)°). Like in the case of the NMe2 derivative, the nitrogen atoms adopt a nearly planar coordination (sum of the angles around N: 359.6°). The dihedral angle between the Mo2N plane and NC2 plane is 16° and thus markedly larger than in case of Mo2(NMe2)6 (0.3–3.6°). Obviously, this is a result of increased steric crowding in the NEt2 derivative. The orientation of the ethyl groups with respect to the Mo–Mo triple bonds allows for a differentiation into proximal and distal groups. In the case of the proximal ethyl groups the Mo–N–C angles (133.1(1)°) are significantly larger than in the distal case (114.0(1)°). Similar disparities were observed for Mo2(NMe2)6 (132° and 116°, resp.) [2].

Corresponding author: Kurt Merzweiler, Naturwissenschaftliche Fakultät II, Institut für Chemie, Martin-Luther-Universität Halle Wittenberg, Kurt-Mothes-Straße 2, 06120Halle (Saale),Germany, E-mail:

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: We acknowledge the financial support within the funding programme Open Access Publishing by the German Research Foundation (DFG).

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

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Received: 2021-04-12
Accepted: 2021-04-26
Published Online: 2021-05-18
Published in Print: 2021-07-27

© 2021 Tobias Brauner et al., published by De Gruyter, Berlin/Boston

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  1. Frontmatter
  2. New Crystal Structures
  3. Crystal structure of poly[(μ2-aqua-tetraaqua-(μ3-glutarato-κ4O,O′:O′:O′′)-(μ5-glutarato-κ6O:O,O′:O′:O′′:O′′′)distrontium(II)], C10H22O13Sr2
  4. The crystal structure of acetato-κ1O-{(2-(2-(2-aminophenoxy)ethoxy)phenyl)(4-oxo-4-phenylbut-2-en-2-yl)amido-κ2N,N′,O}copper(II), C26H26CuN2O5
  5. Crystal structure of dimethanolato-k2O:O-bis(1-((2-methyl-1H-benzo[d]imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-κN)-bis(thiocyanato-κN)dicopper(II), C34H32Cu2N12O2S2
  6. Crystal structure of poly[diaqua-bis(μ2-3-(pyrimidin-5-yl)benzoato-κ2N:O)cobalt(II)] dihydrate, [Co(C11H11O2N2)2(H2O)2]
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  8. Crystal structure of catena-poly[(μ2-methanolato-κ2O:O)-(μ2-1-((2-methyl-1H-benzo[d]imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-κ2N:N′)-(thiocyanato-κ1N)copper(II)] 0.25 hydrate, C17H16CuN6OS ⋅ 0.5H2O
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  10. The crystal structure of 3-amino-5-carboxypyridin-1-ium perchlorate monohydrate, C6H9ClN2O7
  11. Crystal structure of 7-hydroxy-2,4-dimethoxy-9,10-dihydrophenanthrene from Arundina graminifolia, C16H16O3
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  23. The crystal structure of Ba2Mn(SeO3)2Cl2 containing 1∞[Mn(SeO3)2Cl2]4− chains
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  27. The crystal structure of ethyl 5-methyl-7-(4-(phenylthio)phenyl)-4,7-dihydrotetrazolo[1,5-a]pyrimidine-6-carboxylate, C20H19N5O2S
  28. Crystal structure of N′,N‴-((propane-2,2-diylbis(1H-pyrrole-5,2-diyl))bis(methaneylylidene))-di(isonicotinohydrazide)– water – dimethylformamide (1/4/2), C25H24N8O2·4H2O·2C3H7NO
  29. Synthesis and crystal structure of 4-(2,4-dinitrophenoxy)benzaldehyde, C13H8N2O6
  30. The crystal structure of 1-dodecylpyridin-1-ium bromide monohydrate, C17H32BrNO
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https://doi.org/10.1515/ncrs-2021-0138
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Articles in the same Issue

  1. Frontmatter
  2. New Crystal Structures
  3. Crystal structure of poly[(μ2-aqua-tetraaqua-(μ3-glutarato-κ4O,O′:O′:O′′)-(μ5-glutarato-κ6O:O,O′:O′:O′′:O′′′)distrontium(II)], C10H22O13Sr2
  4. The crystal structure of acetato-κ1O-{(2-(2-(2-aminophenoxy)ethoxy)phenyl)(4-oxo-4-phenylbut-2-en-2-yl)amido-κ2N,N′,O}copper(II), C26H26CuN2O5
  5. Crystal structure of dimethanolato-k2O:O-bis(1-((2-methyl-1H-benzo[d]imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-κN)-bis(thiocyanato-κN)dicopper(II), C34H32Cu2N12O2S2
  6. Crystal structure of poly[diaqua-bis(μ2-3-(pyrimidin-5-yl)benzoato-κ2N:O)cobalt(II)] dihydrate, [Co(C11H11O2N2)2(H2O)2]
  7. Crystal structure of bis(3,3-dimethyl-1-phenylbut-1-en-2-yl)(trimethylsilyl)amido-k1N)zinc(II), Zn(C15H24NSi)2
  8. Crystal structure of catena-poly[(μ2-methanolato-κ2O:O)-(μ2-1-((2-methyl-1H-benzo[d]imidazol-1-yl)methyl)-1H-benzo[d][1,2,3]triazole-κ2N:N′)-(thiocyanato-κ1N)copper(II)] 0.25 hydrate, C17H16CuN6OS ⋅ 0.5H2O
  9. The crystal structure of 2-amino-5-nitroanilinium iodide monohydrate, C6H8IN3O2
  10. The crystal structure of 3-amino-5-carboxypyridin-1-ium perchlorate monohydrate, C6H9ClN2O7
  11. Crystal structure of 7-hydroxy-2,4-dimethoxy-9,10-dihydrophenanthrene from Arundina graminifolia, C16H16O3
  12. Crystal structure of 6,6′-((1E, 1′E)-(((1R, 2R)-1,2-diphenylethane-1,2-diyl) bis(azanylylidene))bis(methanylylidene))bis(2-ethylphenol), C32H32N2O2
  13. The crystal structure of 2-amino-5-carboxypyridin-1-ium iodide monohydrate, C6H9IN2O3
  14. The crystal structure of 2-(3,5-difluorophenyl)-2,3-dihydro-1H-naphtho[1,8-de][1,3,2]diazaborinine, C16H11BF2N2
  15. Crystal structure of bis{(2-pyridinyl)-1-phenyl-1-isopropylmethanolato-κ2N,O}nickel, C30H32N2NiO2
  16. Crystal structure of poly[(m3-3-carboxyadamantane-1-carboxylato-κ3O:O′:O″)-(phenanthroline-κ2N,N′)sodium(II)], C24H23N2NaO4
  17. Crystal structure of 2-phenylethynyl-1,3,6,8-tetramethylBOPHY (BOPHY = bis(difluoroboron)-1,2-bis((1H-pyrrol-2-yl)methylene)hydrazine), C22H20B2F4N4
  18. Crystal structure of 4-tert-butyl-2-N-(2-pyridylmethyl)aminophenol, C16H20N2O
  19. The crystal structure of (3Z,3′Z)-4,4′-((1,4-phenylenebis(methylene))bis(azanediyl))bis(pent-3-en-2-one), C18H24N2O2
  20. Crystal structure of (morpholine-1-carbodithioato-κ2-S,S′)bis(triphenylphosphine-κ-P)gold(I), C41H38AuNOP2S2
  21. Crystal structure of 1,4-bis(4-bromobenzyl)-4-(4-chlorophenyl)-1,4-dihydropyridine-3-carbonitrile, C26H19Br2ClN2
  22. The crystal structure of fac-tricarbonyl (N′-benzoyl-N,N-diphenylcarbamimidothioato-κ2S,O)-(pyrazole-κN)rhenium(I) — methanol (1/1) C26H23O4N4SRe
  23. The crystal structure of Ba2Mn(SeO3)2Cl2 containing 1∞[Mn(SeO3)2Cl2]4− chains
  24. Crystal structure of 3,3′,3″-((1E,1′E,1″E)-((nitrilotris(ethane-2,1-diyl))tris(azaneylylidene)) tris(methaneylylidene))tris(4-hydroxy-1-naphthaldehyde) monohydrate, C42H36N4O6·H2O
  25. The crystal structure of 4-(6-acetyl-5-methyl-4,7-dihydrotetrazolo[1,5-a]pyrimidin-7-yl)benzonitrile, C14H12N6O
  26. Crystal structure of benzo[d][1,3]dioxol-5-yl-2-(6-methoxynaphthalen-2-yl)propanoate, C21H18O5
  27. The crystal structure of ethyl 5-methyl-7-(4-(phenylthio)phenyl)-4,7-dihydrotetrazolo[1,5-a]pyrimidine-6-carboxylate, C20H19N5O2S
  28. Crystal structure of N′,N‴-((propane-2,2-diylbis(1H-pyrrole-5,2-diyl))bis(methaneylylidene))-di(isonicotinohydrazide)– water – dimethylformamide (1/4/2), C25H24N8O2·4H2O·2C3H7NO
  29. Synthesis and crystal structure of 4-(2,4-dinitrophenoxy)benzaldehyde, C13H8N2O6
  30. The crystal structure of 1-dodecylpyridin-1-ium bromide monohydrate, C17H32BrNO
  31. Crystal structure of (E)-amino(2-(4-(dimethylamino)benzylidene)hydrazineyl)methaniminium nitrate, C10H16N6O3
  32. Crystal structure of (E)-(2-((1H-pyrrol-2-yl)methylene)hydrazineyl)(amino)methaniminium nitrate monohydrate, C6H12N6O4
  33. The crystal structure of hexakis(1-propylimidazole-κ1N)copper(II) dichloride, C36H60Cl2CuN12
  34. The crystal structure of bis{(μ2-3,3-dimethyl-1-phenylbut-1-en-2-yl)((dimethylamino)dimethylsilyl)amido-κ3N,N′:N′}dilithium, C32H54Li2N4Si2
  35. The crystal structure of methyl 4-(1H-naphtho[1,8-de][1,3,2]diazaborinin-2(3H)-yl)benzoate, C18H15BN2O2
  36. Crystal structure of (E)-N-(1-((2-chlorothiazol-5-yl)methyl)pyridin-2(1H)-ylidene)-2,2,2-trifluoroacetamide, C11H7ClF3N3OS
  37. Crystal structure of N′, N‴-((propane-2,2-diylbis(1H-pyrrole-5,2-diyl))bis (methaneylylidene))di(picolinohydrazide) – water – methanol (1/1/1), C25H24N8O2·H2O·CH3OH
  38. Crystal structure of 3-(2-chloro-benzyl)-7-[4-(2-chloro-benzyl)-piperazin-1-yl]-5,6,8-trifluoro-3H-quinazolin-4-one, C26H21Cl2F3N4O
  39. Crystal structure of N1,N2-bis(2-fluorobenzyl)benzene-1,2-diamine,C20H18F2N2
  40. The crystal structure of 2-(benzo[d][1,3]dioxol-5-yl)-2,3-dihydro-1H-naphtho[1,8-de][1,3,2]diazaborinine, C17H13BN2O2
  41. The crystal structure of 6,6′-((1E,1′E)-hydrazine-1,2-diylidenebis(methaneylylidene)) bis(2-bromo-4-nitrophenol) — dimethylsulfoxide (1/2), C14H8Br2N4O6⋅2(C2H6OS)
  42. Selective biocatalytic synthesis and crystal structure of (2R,6R)-hydroxyketaminium chloride, C13H17Cl2NO2
  43. Crystal structure of bis{tetraaqua-[μ3-1-(4-carboxylatophenyl)-5-methyl-1H-pyrazole-3-carboxylate-κ4N,O,O′,O″] [μ2-1-methyl-1H-pyrazole-3,5-dicarboxylate-κ3N,O:O]dicobalt(II)} dihydrate, C36H44Co4N8O26
  44. Crystal structure of diethyl-2,2′-naphthalene-2,3-diylbis(oxy)diacetate, C18H20O6
  45. Synthesis and crystal structure of poly[(μ3-2-(2-carboxylatophenyl)-1H-benzo[d]imidazole-5-carboxylato-κO,O′:O′;:O″, O″′)-(μ2-1-(4-(1Himidazol-1-yl)phenyl)-1H-imidazole-κ2N:N′)cadmium(II)], C27H18CdN6O4
  46. The crystal structure of catena-poly[diaqua-bis(μ2-2-((2-(2-phenylacetyl)hydrazineylidene)methyl)benzoato-κ2O:O')zinc(II)], C32H30N4O8Zn
  47. The crystal structure of 2-(3,4-dimethoxyphenyl)-2,3-dihydro-1H-naphtho [1,8-de][1,3,2]diazaborinine, C18H17BN2O2
  48. The crystal structure of hexakis(1-ethylimidazole-κ1N)nickel(II) dichloride – 1-ethylimidazole (1/2), C40H64Cl2NiN16
  49. Crystal structure of diaqua-bis(2,4-dinitrophenolato-κ2O,O′)copper(II) 1.5 hydrate, C12H13CuN4O13.5
  50. Crystal structure of N′,N‴-((1E,1′E)-((decane-1,10-diylbis(oxy))bis(2,1-phenylene)) bis(methaneylylidene))di(isonicotinohydrazide), C36H40N6O4
  51. The crystal structure of 2-[(R)-1-(naphthalen-1-yl)ethyl]-2,3,7,7a-tetrahydro-3a,6-epoxyisoindol-1(6H)-one, C19H20NO2
  52. Synthesis and crystal structure of (1E,2E)-3-(anthracen-9-yl)-1-(4-methoxyphenyl)prop-2-en-1-one oxime, C24H19NO2
  53. Synthesis and crystal structure of (2E,2′E)-3,3′-(1,3-phenylene)bis(1-(3-bromophenyl)prop-2-en-1-one), C24H16Br2O2
  54. The crystal structure of catena-poly[bis(µ2-1,2-bis((1H-imidazol-1-yl)methyl)benzene- κ2N:N′)-bis(nitrato-κO)copper(II)], C28H28N10O6Cu
  55. Synthesis and crystal structure of the novel chiral acetyl-3-thiophene-5-(9-anthryl)-2-pyrazoline, C23H18N2OS
  56. Crystal structure of (E)-3-(dimethylamino)-1-(thiophen-3-yl)prop-2-en-1-one, C9H11NOS
  57. Crystal structure of catena-poly[aqua-(4-iodopyridine-2,6-dicarboxylato-κ3N,O,O′)-(μ2-4-amino-4H-1,2,4-triazole-κ2N:N′) copper(II)], C9H8N5O5CuI
  58. Crystal structure of cyclopropane-1,2,3-triyltris(phenylmethanone), C24H18O3
  59. Crystal structure of bis(amino(thioureido)methaniminium) terephthalate, C12H18N8O4S2
  60. A three-dimensional Eu(III) framework in the crystal structure of dimethylaminium poly[dimethylformamide-κ1N)bis(μ4-terephthalato-κ4O:O′:O′′:O′′′)europium(III)] monohydrate, C21H25EuN2O10
  61. Crystal structure of 2-methoxyphenyl 2-(6-methoxynaphthalen-2-yl)propanoate, C21H20O4
  62. The crystal structure of Hexakis(diethylamido)dimolybdenum, Mo2(NEt2)6
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