Startseite Naturwissenschaften Crystal structure of bis(μ-benzeneselenolato)-(tetracarbonyl)-{μ-[N-(diphenylphosphanyl)-N-(3-ethynylphenyl)-P,P-diphenylphosphinous amide]} diiron, C48H35Fe2NO4P2Se2
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Crystal structure of bis(μ-benzeneselenolato)-(tetracarbonyl)-{μ-[N-(diphenylphosphanyl)-N-(3-ethynylphenyl)-P,P-diphenylphosphinous amide]} diiron, C48H35Fe2NO4P2Se2

  • Shuang Lü EMAIL logo und Qian-Li Li ORCID logo
Veröffentlicht/Copyright: 8. Juli 2024

Abstract

C48H35Fe2NO4P2Se2, monoclinic, P21/c, a = 20.3289(18) Å, b = 12.6909(11) Å, c = 17.6743(16) Å, β = 109.767(4), V = 4291.1(7) Å3, Z = 4, Rgt(F) = 0.0638, wRref(F2) = 0.1439, T = 298(2) K.

CCDC no.: 2349331

The molecular structure is shown in the figure. Table 1 contains crystallographic data and Table 2 contains the list of the atoms including atomic coordinates and displacement parameters.

Table 1:

Data collection and handling.

Crystal: Red block
Size: 0.38 × 0.26 × 0.20 mm
Wavelength:

μ:
Mo Kα radiation (0.71073 Å)

2.49 mm−1
Diffractometer, scan mode:

θmax, completeness:
Bruker SMART-1000, φ and ω

25.0°, 99 %
N(hkl)measured, N(hkl)unique, Rint: 19908, 7498, 0.100
Criterion for Iobs, N(hkl)gt: Iobs > 2 σ(Iobs), 4106
N(param)refined: 532
Programs: Bruker, 1 SHELX, 2 , 3 Olex2 4
Table 2:

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

Atom x y z Uiso*/Ueq
C1 0.1165 (4) 0.6876 (6) 0.4179 (5) 0.0353 (19)
C2 0.1956 (4) 0.7142 (6) 0.5663 (5) 0.040 (2)
C3 0.1732 (4) 0.6913 (6) 0.2873 (5) 0.0315 (18)
C4 0.3058 (4) 0.7366 (6) 0.3108 (4) 0.0320 (18)
C5 0.1252 (4) 0.4480 (6) 0.4607 (4) 0.045 (2)
C6 0.0846 (4) 0.4204 (6) 0.3840 (5) 0.079 (3)
H6 0.102708 0.438966 0.344036 0.095*
C7 0.0210 (4) 0.3694 (6) 0.3572 (7) 0.098 (3)
H7 −0.002887 0.355185 0.303202 0.118*
C8 −0.0038 (6) 0.3414 (8) 0.4179 (6) 0.110 (4)
H8 −0.045451 0.303837 0.404926 0.133*
C9 0.0306 (5) 0.3670 (8) 0.4968 (7) 0.120 (4)
H9 0.011824 0.350485 0.536543 0.144*
C10 0.0945 (5) 0.4182 (7) 0.5155 (6) 0.095 (3)
H10 0.118191 0.433590 0.569271 0.114*
C11 0.2524 (4) 0.4551 (6) 0.5840 (4) 0.0311 (17)
C12 0.2440 (5) 0.3531 (7) 0.6030 (5) 0.052 (2)
H12 0.216850 0.308764 0.562565 0.062*
C13 0.2733 (5) 0.3128 (7) 0.6784 (5) 0.064 (3)
H13 0.265575 0.243135 0.689391 0.077*
C14 0.3149 (5) 0.3780 (7) 0.7385 (5) 0.063 (3)
H14 0.335647 0.352283 0.790374 0.076*
C15 0.3253 (4) 0.4791 (6) 0.7214 (5) 0.048 (2)
H15 0.353902 0.522761 0.761276 0.057*
C16 0.2932 (4) 0.5177 (6) 0.6439 (4) 0.0382 (19)
H16 0.299817 0.587748 0.632916 0.046*
C17 0.2179 (4) 0.4713 (6) 0.2521 (4) 0.0355 (18)
C18 0.2374 (5) 0.5057 (7) 0.1889 (4) 0.054 (2)
H18 0.275255 0.551170 0.198565 0.065*
C19 0.2016 (5) 0.4735 (7) 0.1116 (5) 0.066 (3)
H19 0.216276 0.495419 0.069710 0.079*
C20 0.1444 (5) 0.4092 (7) 0.0961 (5) 0.067 (3)
H20 0.119054 0.390888 0.043312 0.081*
C21 0.1243 (5) 0.3718 (7) 0.1572 (5) 0.069 (3)
H21 0.085449 0.328349 0.147498 0.083*
C22 0.1640 (4) 0.4012 (6) 0.2337 (5) 0.058 (2)
H22 0.153343 0.371112 0.276106 0.070*
C23 0.3553 (4) 0.4770 (6) 0.3568 (4) 0.0319 (17)
C24 0.4129 (4) 0.5374 (6) 0.3864 (5) 0.040 (2)
H24 0.408910 0.603806 0.406719 0.048*
C25 0.4771 (4) 0.5033 (7) 0.3873 (5) 0.050 (2)
H25 0.516176 0.545769 0.409562 0.060*
C26 0.4843 (5) 0.4082 (7) 0.3559 (5) 0.053 (2)
H26 0.527529 0.386090 0.354574 0.063*
C27 0.4265 (5) 0.3456 (7) 0.3263 (5) 0.055 (2)
H27 0.430425 0.279480 0.305513 0.067*
C28 0.3643 (4) 0.3791 (6) 0.3271 (5) 0.0412 (19)
H28 0.325707 0.335090 0.306901 0.049*
C29 0.2761 (4) 0.3450 (6) 0.4435 (5) 0.0344 (17)
C30 0.2384 (4) 0.2564 (6) 0.4117 (5) 0.050 (2)
H30 0.194048 0.261394 0.373323 0.060*
C31 0.2682 (5) 0.1591 (7) 0.4382 (6) 0.066 (3)
H31 0.242963 0.098775 0.416301 0.079*
C32 0.3320 (5) 0.1479 (7) 0.4944 (6) 0.058 (2)
H32 0.350374 0.081200 0.510669 0.070*
C33 0.3699 (4) 0.2379 (6) 0.5277 (5) 0.044 (2)
C34 0.3413 (4) 0.3358 (6) 0.5008 (5) 0.0375 (18)
H34 0.366635 0.396373 0.521858 0.045*
C35 0.4349 (5) 0.2299 (7) 0.5912 (6) 0.056 (2)
C36 0.4864 (6) 0.2256 (8) 0.6440 (7) 0.083 (4)
H36 0.528225 0.222154 0.686987 0.100*
C37 0.3810 (4) 0.7880 (6) 0.5485 (5) 0.0354 (19)
C38 0.4333 (5) 0.8220 (7) 0.5236 (6) 0.057 (2)
H38 0.438641 0.793831 0.477481 0.069*
C39 0.4791 (5) 0.8991 (7) 0.5670 (6) 0.069 (3)
H39 0.515798 0.921552 0.550741 0.083*
C40 0.4700 (5) 0.9410 (8) 0.6323 (7) 0.071 (3)
H40 0.500915 0.992409 0.661325 0.085*
C41 0.4175 (5) 0.9107 (7) 0.6568 (6) 0.068 (3)
H41 0.411496 0.941638 0.701714 0.082*
C42 0.3724 (5) 0.8330 (7) 0.6147 (5) 0.053 (2)
H42 0.335869 0.811147 0.631546 0.063*
C43 0.1496 (4) 0.9239 (6) 0.3592 (5) 0.040 (2)
C44 0.0989 (5) 0.9523 (7) 0.3887 (6) 0.061 (2)
H44 0.098280 0.921984 0.436397 0.074*
C45 0.0482 (5) 1.0249 (8) 0.3502 (7) 0.077 (3)
H45 0.012487 1.041049 0.370073 0.092*
C46 0.0514 (6) 1.0718 (9) 0.2833 (7) 0.089 (3)
H46 0.018603 1.123116 0.258168 0.106*
C47 0.1012 (6) 1.0459 (9) 0.2518 (6) 0.090 (3)
H47 0.102424 1.079195 0.205449 0.108*
C48 0.1511 (5) 0.9689 (8) 0.2889 (6) 0.068 (3)
H48 0.184497 0.948631 0.266482 0.082*
Fe1 0.20562 (5) 0.68237 (8) 0.47512 (6) 0.0255 (3)
Fe2 0.25452 (5) 0.69126 (8) 0.36364 (6) 0.0251 (3)
N1 0.2471 (3) 0.4492 (4) 0.4220 (3) 0.0220 (14)
O1 0.0579 (3) 0.6945 (5) 0.3821 (3) 0.0553 (17)
O2 0.1879 (3) 0.7343 (5) 0.6260 (3) 0.0643 (19)
O3 0.1188 (3) 0.6887 (5) 0.2390 (3) 0.0532 (17)
O4 0.3394 (3) 0.7691 (5) 0.2734 (3) 0.0552 (17)
P1 0.20776 (10) 0.51040 (15) 0.48374 (11) 0.0262 (5)
P2 0.26847 (10) 0.52271 (15) 0.35160 (11) 0.0266 (5)
Se1 0.32723 (4) 0.66590 (6) 0.49919 (4) 0.0279 (2)
Se2 0.22984 (4) 0.84541 (6) 0.42415 (5) 0.0304 (2)

1 Source of material

A mixture of [Fe2(CO)6(μ–SeC6H5)2] (118 mg, 0.2 mmol) and (Ph2P)2NC6H4-3–CCH (97 mg, 0.2 mmol) was dissolved in 15 mL of xylene. The reaction mixture was stirred at reflux for 1 h. After removing the solvent under vacuum, the residue was subjected to preparative TLC separation using dichloromethane/pentane (1:1, v/v) as eluent. The title complex was obtained as a deep-red solid (yield 38 %) from the main band. Single crystals were obtained by diffusing the dichloromethane solution into a hexane solution at room temperature.

2 Experimental details

The structure was solved by Direct Methods with the SHELXS program. Hydrogen atoms were positioned geometrically (C–H = 0.93–0.98 Å). Their Uiso values were set to 1.2 Ueq or 1.5 Ueq of the parent atoms.

3 Comment

Hydrogenase is considered a highly promising catalyst capable of catalyzing hydrogen production under mild conditions. 5 In recent years, hydrogenase model compounds containing the 2Fe2Se unit have garnered considerable attention as synthetic catalysts. The unique structure and activity of these model compounds make them powerful tools for understanding the catalytic mechanisms of natural hydrogenase and for designing novel catalysts. 6 , 7 They share similarities in structure with the active center of natural hydrogenase but offer greater flexibility in synthesis and regulation. A series of mono- and di-phosphine substituted Fe/Se model compounds have been reported. 8 12 Herein, we carried out the CO substitution reaction of [Fe2(CO)6(μ–SeC6H5)2] with a disphosphine ligand (Ph2P)2NC6H4-3–CCH, and obtained the title complex. The title complex comprises a 2Fe2Se cluster with four carbonyls and one diphosphine ligand. The Se1 and Se2 atoms are linked to the two phenyl substituents through axial Se1–C37 and Se2–C43 equatorial bonds. The two phosphorus atoms of diphosphine ligand are positioned at the cisoid dibasal site, symmetrically connecting the two Fe atoms, resembling the previously reported analogues. 13 , 14 The bond length Fe1–Fe2 [2.4916(14) Å] is slightly longer than that of sulfur analogues, and the average Se–Fe–Se angles in the title complex are more open than those in sulfur analogues. 15 19


Corresponding author: Shuang Lü, State Key Laboratory for Macromolecule Drugs and Large-scale Manufacturing, School of Pharmaceutical Sciences, Liaocheng University, Liaocheng 252059, P.R. China, E-mail:

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

  2. Competing interests: The authors declare no conflicts of interest regarding this article.

  3. Research funding: This research was supported by Shandong Provincial Natural Science Foundation under Grant ZR2020MB019.

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Received: 2024-04-18
Accepted: 2024-06-02
Published Online: 2024-07-08
Published in Print: 2024-10-28

© 2024 the author(s), published by De Gruyter, Berlin/Boston

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

Artikel in diesem Heft

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  39. The cocrystal of 2,2′-(hydrazine-1,1-diyl)bis(1H-imidazole-4,5-dicarbonitrile)– methanol (2/3)
  40. Crystal structure of (1′R,2′S,4′R,6′S)-4,6-dihydroxy-1′,8′,8′-trimethyl-3-(3-methylbutanoyl)-4′,8′,6′,1′,7,2′-hexahydro-1H-4′,6′-methanoxanthene-8-carbaldehyde, C23H30O5
  41. Crystal structure of (3,6-di(2-pyridyl)-4-methylphenyl pyridazine-k 2 N,N′)-bis(1-phenyl-pyrazole-κ 2 C,N) iridium(III) hexafluorophosphate, C39H29F6IrN8P
  42. Crystal structure of 1,5-bis[(E)-1-(2-hydroxyphenyl)ethylidene]thiocarbonohydrazide dimethyl sulfoxide monosolvate, C17H18N4O2S·C2H6OS
  43. Crystal structure of (S)-4-(2-(4-(2-acetyl-5-chlorophenyl)-3-methoxy-6-oxopyridazin-1(6H)-yl)-3-phenylpropanamido)benzoic acid monohydrate, C29H26ClN3O7
  44. The crystal structure of 1,3-bis(2,4-dinitro-1H-imidazol-1-yl)propane
  45. Crystal structure of 4-chlorobenzyl (S)-2-(6-methoxynaphthalen-2-yl)propanoate, C21H19ClO3
  46. Crystal structure of 1-(5-(benzo[d][1,3]dioxol-5-yl)-4-benzyl-1-(4-bromophenyl)-4,5-dihydro-1H-1,2,4-triazol-3-yl)ethan-1-one, C24H20BrN3O3
  47. The crystal structure of (Z)-3′-(2-(1-(3,4-dimethyl-phenyl)-3-methyl-5-oxo-1,5-dihydro-4H-pyrazol-4-ylidene)hydrazinyl)-2′-hydroxy-[1,1′-biphenyl]-3-carboxylicacid ─ methanol (1/1), C26H26N4O5
  48. Crystal structure of (S)-1-phenylpropan-1-aminium (S)-(1-phenylpropyl)carbamate C19H26N2O2
  49. Synthesis and crystal structure of methyl 2-((5-bromo-4-(4-cyclopropylnaphthalen-1-yl)-4H-1,2,4-triazol-3-yl)thio)acetate, C18H16BrN3O2S
  50. The crystal structure of trichlorobis(pyridine-2,6-dithio-κS-carbomethylamido)antimony(III), [SbCl3(C9H11N3S2)2]
  51. Crystal structure of 1,8-dihydroxy-3-{[(triphenylstannyl)oxy]carbonyl} anthracene-9,10-dione, C33H22O6Sn
  52. The crystal structure of (E)-4-(2-(pyridin-4-ylmethylene)hydrazine-1-carbonyl)pyridin-1-ium-2-olate dihydrate, C12H14N4O4
  53. The crystal structure of 6-amino-pyridinium-2-carboxylate, C6H6N2O2
  54. The crystal structure of catena-poly[aqua-nitrato-κ3O,O:O′′-(1,10-phenanthroline-κ2N,N)sodium(I)], C24H18N6O7Na2
  55. Retractions
  56. Retraction of: Crystal structure of bis[diaquaisonicotinatosamarium(III)]-µ-isonicotinato-[diisonicotinatocopper(II)], CuSm2(C6H4NO2)8(H2O)4
  57. Retraction of: Crystal structure of aqua(2,2-bipyridine-k 2 N:N′)(nitrato)-(4-aminobenzoato)cadmium(II) nitrate, [Cd(H2O)(NO3)(C10H8N2)(C7H7NO2)][NO3]
Heruntergeladen am 10.1.2026 von https://www.degruyterbrill.com/document/doi/10.1515/ncrs-2024-0176/html
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