Home Crystal structure of tris(hexafluoroacetylacetonato-κ2O,O′) bis(triphenylphosphine oxide-κ1O)samarium(III), C51H33F18O8P2Sm
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Crystal structure of tris(hexafluoroacetylacetonato-κ2O,O′) bis(triphenylphosphine oxide-κ1O)samarium(III), C51H33F18O8P2Sm

  • Wanbin Li , Jinke Jiang , Xin Wang and Qiang Liu ORCID logo EMAIL logo
Published/Copyright: June 18, 2024

Abstract

C51H33F18O8P2Sm, monoclinic, P21/c (no. 14), a = 12.8193(9) Å, b = 13.4721(8) Å, c = 30.280(2) Å, β = 91.227(3)°, V = 5,228.2(6) Å3, Z = 4, R gt (F) = 0.0370, wR ref (F 2) = 0.1025, T = 100.0 K.

CCDC no.: 2351578

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: Colourless block
Size: 0.40 × 0.30 × 0.25 mm
Wavelength: Mo Kα radiation (0.71073 Å)
μ: 1.30 mm−1
Diffractometer, scan mode: Bruker APEX-II CCD, φ and ω
θ max, completeness: 27.5°, >99 %
N(hkl)measured, N(hkl)unique, R int: 172,838, 11,988, 0.089
Criterion for I obs, N(hkl)gt: I obs > 2σ(I obs), 9,105
N(param)refined: 751
Programs: Bruker, 1 SHELX, 2 , 4 Olex2 3
Table 2:

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

Atom x y z U iso */U eq
C1 −0.0390 (3) 0.2574 (3) 0.68588 (14) 0.0271 (9)
C2 0.0215 (3) 0.2907 (3) 0.64508 (12) 0.0208 (8)
C3 −0.0380 (3) 0.3073 (3) 0.60621 (13) 0.0244 (8)
H3 −0.1108 0.2938 0.6058 0.029*
C4 0.0086 (3) 0.3432 (3) 0.56846 (13) 0.0218 (8)
C5 −0.0636 (3) 0.3635 (4) 0.52794 (14) 0.0308 (9)
C6 0.3593 (3) 0.6359 (3) 0.54033 (14) 0.0300 (9)
C7 0.3322 (3) 0.5256 (3) 0.53772 (13) 0.0209 (8)
C8 0.3374 (3) 0.4777 (3) 0.49681 (13) 0.0240 (8)
H8 0.3558 0.5140 0.4712 0.029*
C9 0.3155 (3) 0.3767 (3) 0.49372 (12) 0.0215 (8)
C10 0.3009 (3) 0.3319 (3) 0.44761 (13) 0.0271 (8)
C11 0.6309 (4) 0.3244 (5) 0.62619 (16) 0.0463 (14)
C12 0.5189 (3) 0.2878 (3) 0.63363 (14) 0.0284 (9)
C13 0.5044 (3) 0.2214 (4) 0.66784 (14) 0.0325 (10)
H13 0.5627 0.2008 0.6854 0.039*
C14 0.4055 (3) 0.1842 (3) 0.67698 (12) 0.0218 (8)
C15 0.3961 (3) 0.1033 (3) 0.71196 (13) 0.0256 (8)
C16 0.2521 (3) 0.4608 (3) 0.74992 (12) 0.0203 (7)
C17 0.2337 (3) 0.3592 (3) 0.75557 (14) 0.0270 (9)
H17 0.2237 0.3174 0.7306 0.032*
C18 0.2302 (3) 0.3201 (3) 0.79784 (14) 0.0304 (9)
H18 0.2182 0.2511 0.8017 0.036*
C19 0.2441 (4) 0.3807 (3) 0.83450 (14) 0.0327 (10)
H19 0.2405 0.3534 0.8633 0.039*
C20 0.2632 (3) 0.4807 (3) 0.82910 (13) 0.0308 (9)
H20 0.2735 0.5221 0.8542 0.037*
C21 0.2673 (3) 0.5212 (3) 0.78678 (13) 0.0249 (8)
H21 0.2806 0.5901 0.7831 0.030*
C22 0.1194 (3) 0.5398 (3) 0.67927 (13) 0.0214 (8)
C23 0.0936 (3) 0.5531 (3) 0.63445 (13) 0.0238 (8)
H23 0.1460 0.5476 0.6129 0.029*
C24 −0.0086 (3) 0.5742 (3) 0.62157 (14) 0.0272 (9)
H24 −0.0262 0.5822 0.5911 0.033*
C25 −0.0852 (3) 0.5836 (3) 0.65299 (14) 0.0304 (9)
H25 −0.1553 0.5971 0.6441 0.037*
C26 −0.0593 (3) 0.5732 (4) 0.69747 (15) 0.0384 (11)
H26 −0.1112 0.5813 0.7191 0.046*
C27 0.0429 (3) 0.5510 (4) 0.71037 (14) 0.0329 (10)
H27 0.0602 0.5435 0.7408 0.040*
C28 0.3280 (3) 0.6190 (3) 0.69280 (12) 0.0207 (8)
C29 0.2923 (3) 0.7065 (3) 0.71240 (14) 0.0283 (9)
H29 0.2253 0.7081 0.7252 0.034*
C30 0.3542 (4) 0.7904 (3) 0.71315 (16) 0.0369 (11)
H30 0.3300 0.8496 0.7265 0.044*
C31 0.4525 (4) 0.7881 (3) 0.69419 (15) 0.0361 (11)
H31 0.4956 0.8454 0.6951 0.043*
C32 0.4873 (4) 0.7022 (3) 0.67402 (15) 0.0348 (10)
H32 0.5536 0.7012 0.6606 0.042*
C33 0.4251 (3) 0.6175 (3) 0.67338 (14) 0.0270 (9)
H33 0.4491 0.5586 0.6597 0.032*
C34 0.1652 (3) −0.0167 (3) 0.61110 (13) 0.0223 (8)
C35 0.1315 (3) 0.0299 (3) 0.64927 (14) 0.0287 (9)
H35 0.1418 0.0992 0.6531 0.034*
C36 0.0829 (4) −0.0246 (4) 0.68168 (16) 0.0409 (12)
H36 0.0614 0.0073 0.7080 0.049*
C37 0.0656 (4) −0.1251 (4) 0.67605 (16) 0.0391 (11)
H37 0.0307 −0.1618 0.6981 0.047*
C38 0.0988 (4) −0.1722 (3) 0.63858 (17) 0.0368 (11)
H38 0.0880 −0.2415 0.6351 0.044*
C39 0.1485 (3) −0.1182 (3) 0.60565 (15) 0.0294 (9)
H39 0.1707 −0.1507 0.5796 0.035*
C40 0.3647 (3) 0.0297 (3) 0.57120 (13) 0.0224 (8)
C41 0.4061 (3) −0.0538 (3) 0.59245 (14) 0.0267 (9)
H41 0.3619 −0.0968 0.6085 0.032*
C42 0.5119 (3) −0.0740 (3) 0.59010 (15) 0.0319 (10)
H42 0.5399 −0.1313 0.6043 0.038*
C43 0.5770 (3) −0.0114 (3) 0.56728 (14) 0.0281 (9)
H43 0.6493 −0.0262 0.5656 0.034*
C44 0.5369 (3) 0.0731 (3) 0.54681 (14) 0.0295 (9)
H44 0.5820 0.1168 0.5317 0.035*
C45 0.4307 (3) 0.0937 (3) 0.54850 (14) 0.0252 (8)
H45 0.4031 0.1511 0.5343 0.030*
C46 0.1785 (3) 0.0315 (3) 0.51598 (12) 0.0218 (8)
C47 0.1257 (3) 0.1066 (4) 0.49337 (14) 0.0339 (10)
H47 0.1148 0.1690 0.5072 0.041*
C48 0.0890 (4) 0.0901 (5) 0.45038 (16) 0.0471 (13)
H48 0.0537 0.1416 0.4347 0.056*
C49 0.1034 (4) 0.0001 (5) 0.43058 (15) 0.0476 (14)
H49 0.0771 −0.0108 0.4014 0.057*
C50 0.1563 (4) −0.0753 (4) 0.45277 (16) 0.0421 (13)
H50 0.1661 −0.1375 0.4387 0.051*
C51 0.1952 (3) −0.0601 (3) 0.49568 (14) 0.0307 (9)
H51 0.2325 −0.1113 0.5108 0.037*
F1 0.0243 (2) 0.2248 (3) 0.71790 (10) 0.0567 (9)
F2 −0.1038 (3) 0.1829 (2) 0.67658 (10) 0.0541 (9)
F3 −0.0955 (3) 0.3290 (2) 0.70225 (10) 0.0568 (9)
F4 −0.0206 (2) 0.3335 (2) 0.49080 (8) 0.0447 (7)
F5 −0.0828 (2) 0.4606 (2) 0.52377 (10) 0.0469 (7)
F6 −0.1566 (2) 0.3199 (3) 0.53083 (10) 0.0549 (9)
F7 0.4439 (2) 0.6498 (2) 0.56637 (10) 0.0479 (8)
F8 0.2814 (2) 0.68766 (19) 0.55757 (10) 0.0470 (7)
F9 0.3794 (2) 0.6778 (2) 0.50152 (9) 0.0434 (7)
F10 0.3363 (2) 0.3879 (2) 0.41476 (8) 0.0407 (7)
F11 0.1983 (2) 0.3177 (2) 0.43881 (8) 0.0393 (6)
F12 0.3468 (2) 0.2432 (2) 0.44438 (8) 0.0394 (6)
F13a 0.6353 (6) 0.4154 (8) 0.6114 (7) 0.079 (6)
F14b 0.6733 (11) 0.273 (2) 0.5933 (8) 0.097 (9)
F15c 0.6943 (5) 0.3174 (13) 0.6608 (3) 0.078 (5)
F16 0.4865 (2) 0.0764 (2) 0.73089 (10) 0.0474 (8)
F17 0.3549 (3) 0.0219 (2) 0.69421 (10) 0.0533 (9)
F18 0.3338 (2) 0.1306 (2) 0.74416 (9) 0.0468 (7)
O1 0.1177 (2) 0.30045 (19) 0.65074 (8) 0.0204 (5)
O2 0.1025 (2) 0.3647 (2) 0.56262 (9) 0.0218 (6)
O3 0.3066 (2) 0.48902 (19) 0.57424 (9) 0.0221 (6)
O4 0.3022 (2) 0.31569 (19) 0.52426 (8) 0.0211 (5)
O5 0.4524 (2) 0.3217 (2) 0.60646 (9) 0.0224 (6)
O6 0.3204 (2) 0.2090 (2) 0.65909 (9) 0.0228 (6)
O7 0.2948 (2) 0.43052 (19) 0.66324 (8) 0.0196 (5)
O8 0.2093 (2) 0.16784 (19) 0.58018 (8) 0.0201 (5)
P1 0.25195 (8) 0.50705 (7) 0.69407 (3) 0.01806 (19)
P2 0.22798 (7) 0.05981 (7) 0.57076 (3) 0.01752 (19)
Sm1 0.26477 (2) 0.32591 (2) 0.60233 (2) 0.01607 (6)
F14Ad 0.6552 (10) 0.339 (3) 0.5862 (5) 0.071 (11)
F13Ae 0.6393 (12) 0.4152 (15) 0.6436 (11) 0.114 (9)
F15Af 0.6994 (10) 0.253 (2) 0.6405 (11) 0.064 (8)
  1. aOccupancy: 0.58(3), boccupancy: 0.64(5), coccupancy: 0.72(3), doccupancy: 0.36(5), eoccupancy: 0.42(3), foccupancy: 0.28(3).

1 Source of material

The hexafluoroacetylacetone (6 FAAT) (0.312 g, 1.5 mmol) was dissolved in 10 ml ethanol, and 1 ml aqueous solution of samarium acetate monohydrate (0.164 g, 0.5 mmol) was added dropwise into the solution. The mixtures were stirred for 2 h at room temperature, and then add 10 ml of ethanol solution of triphenylphosphine oxide (TPPO) (0.279 g, 1.0 mmol). After stirring overnight and heating to concentrate the solution, a crystalline precipitate is formed. The complexes were dissolved in ethyl acetate/ethanol (1:1) and stilled several days. Crystals were obtained in the form of single crystals which are suitable for X-ray measurements.

2 Experimental details

The data were collected using Bruker, 1 the structure of crystal was solved by SHELXT 2 program within Olex2 3 and refined by SHELXL. 4

3 Comment

Rare earth organic complexes have extensive application value in fields such as fluorescence, biology, and magnetic materials, and have received increasing attention. 5 8 The title compound consists of three FAAT anions, two TPPOs, and one metal samarium(III) ion. The action of TPPO is to saturate the remaining coordination number of samarium ions. 9


Corresponding author: Qiang Liu, College of Biology and Pharmaceutical Engineering, Jilin Agricultural Science and Technology University, 132101 Jilin, China, E-mail:

Acknowledgment

This work was supported by the Jilin Agricultural Science and Technology University Students Science and Technology Innovation Training Program Project (GJ202211439019) and the Key Discipline of Biology.

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

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

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Received: 2024-05-04
Accepted: 2024-05-23
Published Online: 2024-06-18
Published in Print: 2024-08-27

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

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

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  52. The crystal structure of 1-(2-chlorophenyl)-3-(p-tolyl)urea, C14H13ClN2O
  53. The crystal structure of 1-cyclohexyl-3-(p-tolyl)urea, C14H20N2O
  54. Crystal structure of ((benzyl(hydroxy)-amino)(4-chlorophenyl)methyl)-diphenylphosphine oxide, C26H23ClNO2P
  55. The crystal structure of ethyl 3-(1-methyl-1H-indole-2-carbonyl)-2-phenylquinoline-4-carboxylate, C28H22N2O3
  56. The crystal structure of 1,4-bis(1H-imidazol-3-ium-1-yl)benzene dinitrate, C12H12N4 2+·2(NO3 )
  57. Crystal structure of tris(hexafluoroacetylacetonato-κ2O,O′) bis(triphenylphosphine oxide-κ1O)samarium(III), C51H33F18O8P2Sm
  58. Crystal structure of 1-(4-(dimethylamino)phenyl)-2,3-bis(diphenylphosphoryl)propan-1-one, C35H33NO3P2
  59. Crystal structure of diaqua[bis(μ 2-pyridine 2,6-dicarboxylato) bismuth(III) potassium(I)], C14H10BiKN2O10
  60. Crystal structure of (R)-N, N -dimethyl-[1, 1′-binaphthalene]-2, 2′-diamine, C22H20N2
  61. Crystal structure of 1-phenyl-4-(2-furoyl)-3-furyl-1H-pyrazol-5-ol, C18H12N2O4
  62. Crystal structure of bis(14,34-dimethyl[11,21:23,31-terphenyl]-22-yl)diselane, C40H34Se2
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