Home Crystal structure of [(4-bromobenzyl)triphenylphosphonium] tetrabromoantimony(III), [C25H21BrP]+[SbBr4]−
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Crystal structure of [(4-bromobenzyl)triphenylphosphonium] tetrabromoantimony(III), [C25H21BrP]+[SbBr4]

  • Xue Li and Guangyao Wang ORCID logo EMAIL logo
Published/Copyright: February 17, 2025

Abstract

C25H21Br5PSb, monoclinic, P21/c (no. 14), a = 10.5893(1) Å, b = 14.7743(2) Å, c = 18.9737(3) Å, β = 102.279(1)°, V = 2900.52(7) Å3, Z = 4, Rgt(F) = 0.0481, wRref(F2) = 0.1362, T = 293(2) K.

CCDC no.: 2416000

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: Clear light colourless block
Size: 0.12 × 0.10 × 0.08 mm
Wavelength: CuKα radiation (1.54184 Å)
μ: 16.2 mm−1
Diffractometer, scan mode: Rigaku Synergy, ω scans
θmax, completeness: 73.9°, 100 %
N(hkl)measured, N(hkl)unique, Rint: 30343, 5811, 0.076
Criterion for Iobs, N(hkl)gt: Iobs > 2σ(Iobs), 4,967
N(param)refined: 300
Programs: Rigaku, 1 Olex2, 2 SHELX 3 , 4
Table 2:

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

x y z Uiso*/Ueq
Sb1 −0.29059 (3) 0.84883 (2) 0.61408 (2) 0.04832 (15)
Br1 −0.52310 (6) 0.80475 (6) 0.57658 (4) 0.0773 (2)
Br2 −0.23436 (8) 0.95849 (5) 0.52650 (4) 0.0758 (2)
Br3 −0.25289 (8) 0.91717 (5) 0.73554 (3) 0.0752 (2)
Br4 −0.16391 (8) 0.70512 (6) 0.62217 (5) 0.0826 (3)
P1 0.70586 (10) 0.33212 (7) 0.64386 (6) 0.0360 (2)
C1 0.7686 (4) 0.3940 (3) 0.7248 (3) 0.0422 (9)
C2 0.7511 (6) 0.3662 (4) 0.7919 (3) 0.0573 (13)
H2 0.697104 0.317688 0.795848 0.069*
C3 0.8154 (8) 0.4119 (5) 0.8532 (3) 0.0737 (18)
H3 0.803794 0.393974 0.898415 0.088*
C4 0.8956 (7) 0.4829 (6) 0.8475 (4) 0.081 (2)
H4 0.939077 0.512660 0.888774 0.097*
C5 0.9116 (8) 0.5102 (6) 0.7811 (5) 0.089 (3)
H5 0.966613 0.558230 0.777518 0.106*
C6 0.8473 (7) 0.4673 (5) 0.7195 (4) 0.0678 (16)
H6 0.856627 0.487497 0.674471 0.081*
C7 0.8430 (4) 0.2854 (3) 0.6157 (3) 0.0412 (9)
C8 0.9525 (6) 0.2650 (5) 0.6677 (4) 0.0722 (19)
H8 0.953366 0.274859 0.716199 0.087*
C9 1.0595 (7) 0.2302 (6) 0.6476 (5) 0.093 (3)
H9 1.131290 0.214138 0.682814 0.112*
C10 1.0622 (6) 0.2187 (4) 0.5761 (4) 0.0693 (17)
H10 1.137125 0.198598 0.562927 0.083*
C11 0.9548 (7) 0.2368 (5) 0.5247 (4) 0.0707 (17)
H11 0.954814 0.225696 0.476488 0.085*
C12 0.8446 (6) 0.2718 (5) 0.5437 (3) 0.0633 (15)
H12 0.772379 0.286030 0.508178 0.076*
C13 0.5970 (4) 0.2456 (3) 0.6587 (3) 0.0407 (9)
C14 0.4996 (5) 0.2658 (4) 0.6955 (3) 0.0514 (11)
H14 0.491927 0.324137 0.712575 0.062*
C15 0.4146 (6) 0.1989 (5) 0.7067 (4) 0.0676 (16)
H15 0.351912 0.211398 0.733004 0.081*
C16 0.4230 (6) 0.1136 (5) 0.6787 (5) 0.0746 (19)
H16 0.365881 0.068520 0.686095 0.089*
C17 0.5161 (6) 0.0949 (4) 0.6395 (5) 0.0741 (19)
H17 0.519059 0.037831 0.619165 0.089*
C18 0.6045 (6) 0.1598 (4) 0.6303 (4) 0.0551 (13)
H18 0.668634 0.146268 0.605310 0.066*
C19 0.6244 (5) 0.4067 (4) 0.5723 (3) 0.0510 (12)
H19A 0.682592 0.455704 0.567025 0.061*
H19B 0.606327 0.373060 0.527426 0.061*
C20 0.3836 (6) 0.4053 (4) 0.5547 (3) 0.0578 (13)
H20 0.383660 0.351870 0.528786 0.069*
C21 0.2663 (6) 0.4425 (5) 0.5632 (4) 0.0696 (18)
H21 0.188224 0.414163 0.543748 0.084*
C22 0.2697 (6) 0.5218 (5) 0.6009 (4) 0.0677 (19)
C23 0.3810 (7) 0.5637 (5) 0.6302 (4) 0.0699 (18)
H23 0.380220 0.617203 0.655916 0.084*
C24 0.4978 (6) 0.5261 (4) 0.6218 (3) 0.0562 (13)
H24 0.575179 0.555042 0.641764 0.067*
C25 0.4993 (5) 0.4470 (3) 0.5843 (2) 0.0420 (10)
Br5 0.0966 (3) 0.5578 (3) 0.6001 (2) 0.0779 (7)
Br5A 0.1234 (3) 0.5898 (3) 0.6211 (2) 0.0784 (7)a
  1. aOccupancy: 0.534 (7).

1 Source of materials

1 mmol of (4-bromobenzyl)triphenylphosphonium bromide and 1 mmol of SbBr3 were dissolved in a 14 mL mixture of ethanol/dichloromethane in a 2:5 (v/v) ratio, and 0.5 mL of HBr solution was added. The resulting mixture was subjected to ultrasonic treatment for 10 min, ensuring the formation of a clear, homogeneous solution. The solution was kept at room temperature for several days, block-shaped single crystals were obtained.

2 Experimental details

The crystal data were collected on a Rigaku diffractometer. 1 The structure was determined using the SHELXT program within the Olex2 and subsequently refined with SHELXL. 2 , 3 , 4 The structural model was visualized using Diamond. 5

3 Comment

This study reports a antimony(III)-based salt compound, comprising a (4-bromobenzyl)triphenylphosphonium (4BBTP) cation, and a [SbBr4] anion. The 4BBTP cation carries a positive charge, with the tetrahedron [SbBr4] anion serving as the counterion. The bond lengths of Sb–Br within the anion as well as the geometric parameters of the phosphonium cation are in agreement with values reported in the literatures. 6 , 7 , 8 , 9

Interionic Br⃛Br distances < 3.5 Å are observed beween one bromido ligand of the tetrabromido antimonate anion and the bromo substituent of the cation indicating weak halogen–halogen interactions.


Corresponding author: Guangyao Wang, School of Agriculture, Jilin Agricultural Science and Technology University, 132101 Jilin, Jilin, China, 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: This work was funded by the Scientific and Technologic Development Program of Jilin Province (20220202101NC).

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

References

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Received: 2025-01-10
Accepted: 2025-02-05
Published Online: 2025-02-17
Published in Print: 2025-06-26

© 2025 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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