Synthesis, crystal structure, and Hirshfeld surface analysis of undeca­carbon­yl{tris­[4-(methyl­sulfan­yl)phen­yl]arsine}-triangulo-triosmium(0)

Sirat, S.S.; Rosli, M.M.; Tan, S.L.; Razak, I.A.; Shawkataly, O. bin

doi:10.1107/S2056989025006541

research communications

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ISSN: 2056-9890

Volume 81| Part 8| August 2025| Pages 765-769

https://doi.org/10.1107/S2056989025006541

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Synthesis, crystal structure, and Hirshfeld surface analysis of undecacarbonyl{tris[4-(methylsulfanyl)phenyl]arsine}-triangulo-triosmium(0)

Siti Syaida Sirat,^a,^b ^* Mohd Mustaqim Rosli,^c Sang Loon Tan,^d Ibrahim Abdul Razak ^c and Omar bin Shawkataly ^e

^aFaculty of Applied Sciences, Universiti Teknologi MARA, Cawangan Negeri Sembilan, Kampus Kuala Pilah, 72000 Kuala Pilah, Negeri Sembilan, Malaysia, ^bAtta-ur-Rahman Institute for Natural Product Discovery (AuRIns), Universiti Teknologi MARA, Kampus Puncak Alam, 42300 Bandar Puncak Alam, Selangor, Malaysia, ^cX-ray Crystallography Unit, School of Physics, Universiti Sains Malaysia, 11800 USM, Penang, Malaysia, ^dSunway Biofunctional Molecules Discovery Centre, Faculty of Medical and Life Sciences, Sunway University, 47500 Sunway City, Malaysia, and ^eDepartment of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 Skudai, Johor Bahru, Malaysia
^*Correspondence e-mail: [email protected]

Edited by B. Therrien, University of Neuchâtel, Switzerland (Received 26 June 2025; accepted 21 July 2025; online 29 July 2025)

The title compound, [Os₃(C₂₁H₂₁AsS₃)(CO)₁₁] or [Os₃{As(C₆H₄SCH₃)₃}(CO)₁₁], comprises a triangle of Os atoms, two of which are bonded to four carbonyl ligands. The third Os atom is bound to three carbonyl ligands, and the arsine ligand [As(C₆H₄SCH₃)₃] occupies the equatorial position. In the crystal, the molecules are linked by C—H⋯O hydrogen bonds. To further analyse the intermolecular interactions, a Hirshfeld surface analysis was performed. Two out of the three methylsulfanyl groups are disordered over two sites with final refinement occupancy ratios of 0.612 (12):0.388 (12) and 0.620 (9):0.380 (9).

Keywords: osmium; crystal-structure; cluster; Hirshfeld surface analysis.

CCDC reference: 2474325

1. Chemical context

The chemistry of triosmium carbonyl clusters with group 15 ligands has been extensively studied (Raithby, 2024 ). The majority of reported structures have focused on tertiary phosphine ligands (PR₃) with R = alkyl or aryl groups, with fewer examples involving tertiary arsine ligands (AsPR₃) (webCSD, accessed May 2025; Groom et al., 2016 ). These ligands stabilize low oxidation states of metal centres and can be used to modify both the electronic and steric properties of resulting coordination compounds (Honaker et al., 2007 ). Numerous triosmium carbonyl clusters containing one, two, or three PR₃ have been synthesized and fully characterised (Bruce et al., 1988a ,b ; Biradha et al., 2000 ). Os₃(CO)₁₁(PR₃) is the most reported crystal structure among derivatives in this series, the earlier ones being Os₃(CO)₁₁(PPh₃), and Os₃(CO)₁₁{PPh(OMe)₂}, which were prepared in refluxing toluene for more than 10 h (Bruce et al., 1988a). Biradha and co-workers reported a series of Os₃(CO)₁₁(PR₃) with R = F, OPh, Et, p-C₆H₄Me, o-C₆H₄Me, p-C₆H₄(CF₃) and C₆H₁₁ (Biradha et al., 2000) by reacting Os₃(CO)₁₁(CH₃CN) with PR₃ in dichloromethane for 15 min (Hansen et al., 1998 ). According to these structures, the steric and electronic effects of PR₃ often result in variations of the Os—Os bond that is cis to PR₃ and the Os—P bond length (Biradha et al., 2000). However, there are not many reactions conducted on Os₃(CO)₁₂ with AsPR₃. Os₃(CO)₁₁(AsPh₃) is the only reported structure in this series (Oh et al., 2015 ). Thus, we are currently exploring the reaction between Os₃(CO)₁₂ and the AsPR₃ ligand, focusing on how such ligands influence structural parameters within the triangular osmium cluster. We anticipate that the resulting compound will serve as a representative example contributing to the broader understanding of this structural series Os₃(CO)₁₁(P/AsR₃). Herein, we report the synthesis of Os₃(CO)₁₁{As(C₆H₄SCH₃)₃}, 1, and its examination using single-crystal X-ray diffraction and Hirshfeld surface analysis.

2. Structural commentary

The molecular structure of 1 is shown in Fig. 1. The molecule comprises an Os₃ triangle with one Os centre being equatorially coordinated by the tris{4-(methylsulfanyl)phenyl}arsine ligand [As(C₆H₄SCH₃)₃]. The Os—Os bond lengths in the Os₃ triangle are not equivalent, with the Os1—Os2 bond [2.9150 (3) Å] being longer than the Os1—Os3 and Os2—Os3 bonds, at 2.8611 (3) and 2.8817 (4) Å, respectively. The longest Os—Os bond is cis to As(C₆H₄SCH₃)₃ and comparable with a similar Os—Os bond [2.9148 (7) Å] in Os₃(CO)₁₁AsPh₃ (Oh et al., 2015). These observations are attributed to the steric and electronic effects of the arsine ligand on the Os—Os bonds. The Os—As bond length in 1 is 2.4603 (5) Å and almost similar to the related bond in Os₃(CO)₁₁(AsPh₃) 2.4670 (9) Å (Oh et al., 2015). The Os—C(CO) bond lengths are in the range 1.872 (6)–1.951 (7) Å. The equatorial Os—C≡O bond angles range from 175.7 (5) to 178.4 (5)°, whereas the axial Os—C≡O bond angles range from 174.3 (6) to 177.2 (5)°.

Figure 1
The molecular structure of 1 with 30% displacement ellipsoids.

3. Supramolecular features

In the crystal, C5—H5A⋯O10 intermolecular interactions (Table 1, Fig. 2) lead to the formation of an inversion dimer between two molecules. This dimer is further consolidated by a short S3⋯O10 contact [3.21 (2) Å, symmetry code: $[{1\over 2}]$ + x, $[{3\over 2}]$ − y, $[{1\over 2}]$ + z].

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
C5—H5A⋯O10ⁱ	0.93	2.55	3.41 (1)	154
Symmetry code: (i) .

Figure 2
The crystal structure of the title compound viewed along the c axis. H atoms not involved in hydrogen bonds (dashed lines) have been omitted for clarity.

4. Hirshfeld surface analysis

The major and minor components of the disorder in 1 were subjected to Hirshfeld surface analysis using CrystalExplorer21 (Spackman et al., 2021 ). This is based on the procedures described in the literature (Tan et al., 2019 ) to better understand the nature of the intermolecular interactions that exist in the crystal.

The d_norm mapping reveals a relatively simple landscape of molecular interactions, with only a few red spots being observed on the Hirshfeld surfaces. For the major component, the red spots originated from H5A, O10, H21B, C20, S3, O7, H20A, and C21 (Fig. 3a), corresponding to the close contacts for C5—H5A⋯O10, C21—H21B⋯C20, S3⋯O10, O7⋯O7, and C20—H20A⋯C21 (Table 2). The respective deviations of these contacts from the sum of the van der Waals radii are 0.20, 0.15, 0.11, 0.09 and 0.04 Å, reflecting the intensity of the corresponding red spots. For the minor component, red spots are detected on the disorder fragments of S3X and H21D, corresponding to S3X⋯O10 and C21X—H21D⋯O1 in addition to the intrinsic C5—H5A⋯O10 and O7⋯O7 close contacts for 1 (Fig. 3b). The deviations between the d_norm contact distance and the sum of the van der Waals radii for S3X⋯O10 and H21D⋯O1 are 0.19 and 0.06 Å, respectively (Table 3).

Table 2
The d_norm contact distances (Å, adjusted to neutron values) for all identified interactions present in the major and minor components of 1 with respect to the corresponding sum of van der Waals radii of the relevant contact atoms

Contact	d_norm Distance	ΣvdW radii	Δ(ΣvdW – d_norm distance)	Symmetry operation
Major
C5–H5A⋯O10	2.41	2.61	0.20	1 − x, 2 − y, 2 − z
C20–H20A⋯C21	2.57	2.61	0.04	− $[{1\over 2}]$ + x, $[{1\over 2}]$ − y, − $[{1\over 2}]$ + z
C21–H21B⋯C20	2.64	2.79	0.15	$[{1\over 2}]$ + x, $[{1\over 2}]$ − y, $[{1\over 2}]$ + z
S3⋯O10	3.21	3.32	0.11	$[{1\over 2}]$ + x, $[{3\over 2}]$ − y, $[{1\over 2}]$ + z
O7⋯O7	2.95	3.04	0.09	2 − x, 2 − y, 2 − z
Minor
C5–H5A⋯O10	2.41	2.61	0.20	1 − x, 2 − y, 2 − z
S3X⋯O10	3.13	3.32	0.19	$[{1\over 2}]$ + x, $[{3\over 2}]$ − y, $[{1\over 2}]$ + z
O7⋯O7	2.95	3.04	0.09	2 − x, 2 − y, 2 − z
C21X–H21D⋯O1	2.55	2.61	0.06	2 − x, 1 − y, 2 − z

Table 3
Experimental details

Crystal data
Chemical formula	[Os₃(C₂₁H₂₁AsS₃)(CO)₁₁]
M_r	1323.19
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	297
a, b, c (Å)	14.5019 (15), 15.3759 (16), 17.8575 (19)
β (°)	107.870 (2)
V (Å³)	3789.8 (7)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	11.12
Crystal size (mm)	0.41 × 0.15 × 0.09

Data collection
Diffractometer	Bruker APEX Duo CCD area detector
Absorption correction	Multi-scan (SADABS; Krause et al., 2015 )
T_min, T_max	0.024, 0.076
No. of measured, independent and observed [I > 2σ(I)] reflections	52142, 13246, 8766
R_int	0.054
(sin θ/λ)_max (Å⁻¹)	0.749

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.033, 0.081, 0.97
No. of reflections	13246
No. of parameters	482
No. of restraints	64
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.46, −1.46
Computer programs: APEX2 and SAINT (Bruker, 2012 ), SHELXT (Sheldrick, 2015a ), SHELXL2014/7 (Sheldrick, 2015b ), SHELXTL (Sheldrick, 2015a) and PLATON (Spek, 2020).

Figure 3
Two views of the d_norm map showing the atoms with close contacts, as indicated by the corresponding red spots, with varying intensities for (a) the major component and (b) the minor component of 1.

Apart from the close contacts indicated by red spots, another significant feature emerges from the shape-index mapping on the Hirshfeld surface. This mapping highlights a complementary intermolecular stacking interaction between C32—O11 and the C7–C12 ring (symmetry code: $[{3\over 2}]$ − x, $[{1\over 2}]$ + y, $[{3\over 2}]$ − z), providing evidence of a lone pair⋯π interaction (Fig. 4). This finding aligns with the analysis from PLATON (Spek, 2020 ), which identified a contact distance of 3.867 (5) Å between O11 and the aromatic π-ring, along with a C≡O⋯π angle of 94.0 (4)°. Studies suggested that such interactions typically occur within a distance range of 3.0–4.5 Å, with angles varying between 60 and 160° (Caracelli et al., 2016 ; Chen et al., 2024 ), depending on the specific lone-pair donor and π-acceptor involved.

Figure 4
The partial Hirshfeld surface mapped with shape-index for C32–O11 (top) and the C7–C12 ring (bottom; $[{3\over 2}]$ − x, $[{1\over 2}]$ + y, $[{3\over 2}]$ − z), showing the shape complementarity between the intermolecular stacking fragments of 1. The remaining parts of the molecules were omitted for clarity.

The major and minor components of 1 were subjected to 2D fingerprint plot analysis to quantitatively assess close contacts within the structure. Both exhibit distinct shield- and paw-like fingerprint profiles, which, upon decomposition, reveal symmetrical H⋯O/O⋯H, H⋯H, H⋯C/C⋯H, O⋯S/S⋯O, O⋯O, and O⋯C/C⋯O interactions (Fig. 5), indicating homogeneous reciprocal contacts between internal-X⋯Y-external and external-X⋯Y-internal interfaces.

Figure 5
The comparison of the overall and prominent decomposed fingerprint print plots (> 5%) delineated into H⋯O/O⋯H, H⋯H, H⋯C/C⋯H, O⋯S/S⋯O, O⋯O, and O⋯C/C⋯O close contacts for the major (top) and minor (bottom) components of 1.

Slight deviations are observed in the decomposed fingerprint plots of H⋯H and O⋯S/S⋯O. The major component features a distinct H⋯H peak at a d_i + d_e of approximately 1.80 Å (H20A⋯H21A), whereas the minor component exhibits a broader profile with a larger d_i + d_e of about 2.30 Å (H21F⋯H19B). In the pincer-like decomposed fingerprint plots of O⋯S/S⋯O, the reciprocal contacts correspond to O10⋯S3 (d_i + d_e ≃ 3.21 Å) in the major component and O10⋯S3X (d_i + d_e ≃ 3.12 Å) in the minor component. Other fingerprint plots remain consistent across both components, with close contact distributions being as follows: H⋯O/O⋯H (34.3% vs 38.6%), H⋯H (20.5% vs 17.5%), H⋯C/C⋯H (10.0% vs 12.2%), O⋯S/S⋯O (9.2% vs 8.0%), O⋯O (9.1% vs 7.7%), and O⋯C/C⋯O (8.4% vs 7.7%), while the remaining less prominent contacts contribute to approximately 4.1% to 4.2% (Fig. 6).

Figure 6
The percentage contributions of different close contacts to the Hirshfeld surfaces of the major and minor components of 1.

5. Database survey

A search of the Cambridge Structural Database (webCSD accessed May 2025; Groom et al., 2016) for the title compound returned no relevant hits. However, a search with generalized tertiary arsine ligand (AsR₃) returned one hit [Os₃(CO)₁₁(AsPh₃)] [CSD refcode YUCXEB; Oh et al., 2015). The structure of the title compound is very similar to that of Ru₃(CO)₁₁{As(C₆H₄SCH₃)₃} (SUXQEI; Shawkataly et al., 2010 ), in which tris{4-(methylsulfanyl)phenyl}arsine [As(C₆H₄SCH₃)₃] is equatorially bonded to the metal centre. The structure is consistent with literature precedents for complexes with the general formula Os₃(CO)₁₁PR₃ [HIYVUG (Hansen et al., 1998), MASPEB, MASPIF and MASPUR (Biradha et al., 2000), VADYEE (Bruce et al., 1988a, VAWWUL (Ang et al., 1989 ), YEDZOW and YEFCAN (Adams et al., 1994 )].

6. Synthesis and crystallization

A solution of Os₃(CO)₁₁(CH₃CN) (Nicholls et al., 1990 ; Hansen et al., 1998) (80 mg, 0.087 mmol) and As(C₆H₄SCH₃)₃ (60 mg, 0.13 mmol) in CH₂Cl₂ (25 ml) was stirred at room temperature for 60 min. The reaction was carried out under nitrogen-free oxygen using standard Schlenk techniques. The solution was dried in vacuo, and the residue was chromatographed by preparative thin-layer chromatography on silica gel with C₆H₁₄/CH₂Cl₂ (3:2) as the eluent. Chromatographic separation afforded two bands: the first yellow band was identified as the starting material Os₃(CO)₁₂. The desired product Os₃(CO)₁₁{As(C₆H₄SCH₃)₃} was isolated as the second yellow band in 50% yield and recrystallized from CH₂Cl₂/CH₃OH (1:3). IR (ATR): ν(CO) 2107 s, 2051 m, 2006 w, 1974 m, 1942 w cm⁻¹.

7. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 3. All H atoms were positioned geometrically and refined using a riding model with C—H distances of 0.93 or 0.96 Å (for methyl groups) and U_iso(H) = 1.2U_eq(C) or 1.5U_eq(C-methyl). Two out of the three methylsulfanyl groups were disordered over two sites with a final refinement occupancy ratios of 0.612 (12):0.388 (12) and 0.620 (9):0.380 (9). Anisotropic displacement parameters and rigid-body restraints were applied to the disordered components. Due to poor agreement, reflections 020, $[\overline{4}]$ 33, 680, $[\overline{3}]$ 07, and 379 were omitted from the final cycles of refinement. Maximum and minimum residual electron densities of 1.46 and −1.46 e Å⁻³ were observed at 0.83 Å from Os1 and 0.70 Å from Os3, respectively.

Supporting information

CCDC reference: 2474325

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2056989025006541/tx2100sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2056989025006541/tx2100Isup2.hkl

checkCIF report

Computing details top

Undecacarbonyl{tris[4-(methylsulfanyl)phenyl]arsine}-triangulo-triosmium(0) top

Crystal data top

[Os₃(C₂₁H₂₁AsS₃)(CO)₁₁]	F(000) = 2440
M_r = 1323.19	D_x = 2.319 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 14.5019 (15) Å	Cell parameters from 9975 reflections
b = 15.3759 (16) Å	θ = 2.7–27.7°
c = 17.8575 (19) Å	µ = 11.12 mm⁻¹
β = 107.870 (2)°	T = 297 K
V = 3789.8 (7) Å³	Plate, yellow
Z = 4	0.41 × 0.15 × 0.09 mm

Data collection top

Bruker APEX Duo CCD area detector diffractometer	8766 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	R_int = 0.054
φ and ω scans	θ_max = 32.2°, θ_min = 2.7°
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	h = −20→21
T_min = 0.024, T_max = 0.076	k = −22→23
52142 measured reflections	l = −25→26
13246 independent reflections

Refinement top

Refinement on F²	64 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.033	H-atom parameters constrained
wR(F²) = 0.081	w = 1/[σ²(F_o²) + (0.0331P)²] where P = (F_o² + 2F_c²)/3
S = 0.97	(Δ/σ)_max = 0.003
13246 reflections	Δρ_max = 1.46 e Å⁻³
482 parameters	Δρ_min = −1.46 e Å⁻³

Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes.

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

	x	y	z	U_iso*/U_eq	Occ. (<1)
Os1	0.64030 (2)	0.79000 (2)	0.83741 (2)	0.04272 (5)
Os2	0.77751 (2)	0.87250 (2)	0.97335 (2)	0.05053 (6)
Os3	0.75404 (2)	0.93459 (2)	0.81633 (2)	0.05645 (6)
As1	0.58467 (3)	0.66988 (3)	0.90375 (2)	0.04018 (9)
S1	0.26975 (11)	0.78176 (13)	1.07849 (11)	0.0909 (6)
S2	0.3328 (6)	0.3694 (4)	0.6797 (4)	0.098 (2)	0.612 (12)
C20	0.3547 (12)	0.2721 (10)	0.7360 (9)	0.126 (4)	0.612 (12)
H20A	0.3099	0.2281	0.7089	0.189*	0.612 (12)
H20B	0.3465	0.2829	0.7865	0.189*	0.612 (12)
H20C	0.4197	0.2528	0.7429	0.189*	0.612 (12)
S2X	0.3528 (7)	0.3392 (6)	0.7063 (7)	0.089 (3)	0.388 (12)
C20X	0.252 (2)	0.3784 (14)	0.6533 (15)	0.126 (4)	0.388 (12)
H20D	0.2008	0.3392	0.6530	0.189*	0.388 (12)
H20E	0.2544	0.3862	0.6005	0.189*	0.388 (12)
H20F	0.2414	0.4336	0.6743	0.189*	0.388 (12)
S3	0.9056 (13)	0.4559 (13)	1.1746 (11)	0.102 (4)	0.620 (9)
C21	0.8517 (8)	0.4338 (9)	1.2521 (7)	0.104 (3)	0.620 (9)
H21A	0.8994	0.4082	1.2963	0.156*	0.620 (9)
H21B	0.7984	0.3943	1.2329	0.156*	0.620 (9)
H21C	0.8289	0.4872	1.2680	0.156*	0.620 (9)
S3X	0.905 (2)	0.4698 (19)	1.1841 (16)	0.083 (4)	0.380 (9)
C21X	0.9804 (14)	0.4194 (15)	1.1371 (12)	0.104 (3)	0.380 (9)
H21D	1.0389	0.4004	1.1757	0.156*	0.380 (9)
H21E	0.9960	0.4598	1.1019	0.156*	0.380 (9)
H21F	0.9474	0.3701	1.1079	0.156*	0.380 (9)
O1	0.7863 (3)	0.6672 (3)	0.7993 (2)	0.0725 (10)
O2	0.5161 (3)	0.7732 (3)	0.6676 (2)	0.0875 (13)
O3	0.4744 (3)	0.9005 (3)	0.8608 (3)	0.0838 (12)
O4	0.9236 (3)	0.7338 (4)	0.9578 (3)	0.1041 (16)
O5	0.7750 (4)	0.7808 (3)	1.1233 (3)	0.0938 (14)
O6	0.6178 (4)	0.9914 (3)	0.9960 (3)	0.0998 (15)
O7	0.9269 (3)	1.0144 (3)	1.0409 (3)	0.0917 (14)
O8	0.9216 (5)	0.8158 (4)	0.8063 (4)	0.136 (2)
O9	0.6690 (7)	0.9423 (4)	0.6384 (3)	0.152 (3)
O10	0.5906 (3)	1.0542 (3)	0.8289 (2)	0.0752 (11)
O11	0.8903 (3)	1.0898 (3)	0.8460 (3)	0.0991 (15)
C1	0.4875 (3)	0.6994 (3)	0.9544 (3)	0.0444 (9)
C2	0.4001 (3)	0.6577 (3)	0.9364 (3)	0.0555 (12)
H2A	0.3860	0.6135	0.8992	0.067*
C3	0.3318 (3)	0.6811 (4)	0.9734 (3)	0.0598 (12)
H3A	0.2727	0.6520	0.9605	0.072*
C4	0.3507 (3)	0.7467 (3)	1.0290 (3)	0.0520 (11)
C5	0.4391 (3)	0.7880 (3)	1.0464 (3)	0.0583 (12)
H5A	0.4534	0.8322	1.0838	0.070*
C6	0.5069 (3)	0.7657 (3)	1.0100 (3)	0.0538 (11)
H6A	0.5658	0.7951	1.0226	0.065*
C7	0.5209 (3)	0.5744 (3)	0.8363 (2)	0.0442 (9)
C8	0.5417 (4)	0.4876 (3)	0.8579 (3)	0.0527 (10)
H8A	0.5917	0.4744	0.9034	0.063*
C9	0.4893 (4)	0.4213 (4)	0.8128 (3)	0.0666 (14)
H9A	0.5053	0.3638	0.8272	0.080*
C10	0.4135 (4)	0.4392 (4)	0.7466 (3)	0.0651 (14)
C11	0.3932 (4)	0.5262 (4)	0.7243 (3)	0.0690 (14)
H11A	0.3424	0.5395	0.6794	0.083*
C12	0.4478 (4)	0.5918 (4)	0.7684 (3)	0.0582 (12)
H12A	0.4350	0.6492	0.7520	0.070*
C13	0.6804 (3)	0.6093 (3)	0.9873 (2)	0.0421 (9)
C14	0.7659 (4)	0.5830 (4)	0.9766 (3)	0.0617 (13)
H14A	0.7786	0.5965	0.9299	0.074*
C15	0.8332 (4)	0.5369 (4)	1.0342 (3)	0.0682 (14)
H15A	0.8899	0.5181	1.0252	0.082*
C16	0.8178 (3)	0.5182 (4)	1.1049 (3)	0.0589 (12)
C17	0.7331 (4)	0.5453 (3)	1.1170 (3)	0.0615 (13)
H17A	0.7214	0.5336	1.1644	0.074*
C18	0.6649 (4)	0.5903 (3)	1.0575 (3)	0.0559 (11)
H18A	0.6074	0.6080	1.0657	0.067*
C19	0.1568 (4)	0.7396 (5)	1.0225 (4)	0.090 (2)
H19A	0.1085	0.7550	1.0468	0.135*
H19B	0.1610	0.6774	1.0198	0.135*
H19C	0.1394	0.7634	0.9703	0.135*
C22	0.7360 (4)	0.7139 (3)	0.8156 (3)	0.0518 (10)
C23	0.5636 (4)	0.7775 (3)	0.7325 (3)	0.0603 (12)
C24	0.5387 (4)	0.8629 (3)	0.8546 (3)	0.0536 (11)
C25	0.8686 (4)	0.7860 (4)	0.9595 (3)	0.0687 (15)
C26	0.7747 (4)	0.8120 (4)	1.0660 (4)	0.0670 (14)
C27	0.6752 (4)	0.9480 (4)	0.9840 (3)	0.0648 (13)
C28	0.8726 (4)	0.9610 (4)	1.0160 (3)	0.0653 (13)
C29	0.8587 (6)	0.8578 (4)	0.8105 (5)	0.094 (2)
C30	0.7036 (7)	0.9381 (4)	0.7049 (4)	0.095 (2)
C31	0.6500 (4)	1.0078 (3)	0.8269 (3)	0.0557 (11)
C32	0.8418 (4)	1.0322 (4)	0.8361 (4)	0.0701 (15)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Os1	0.04402 (9)	0.04182 (9)	0.04327 (10)	0.00121 (7)	0.01478 (7)	0.00311 (6)
Os2	0.04408 (9)	0.05623 (11)	0.05050 (11)	−0.00492 (8)	0.01333 (7)	−0.00148 (8)
Os3	0.06879 (12)	0.04738 (10)	0.06249 (13)	−0.00426 (9)	0.03387 (10)	0.00544 (8)
As1	0.0409 (2)	0.0400 (2)	0.0403 (2)	0.00060 (16)	0.01330 (17)	−0.00004 (16)
S1	0.0575 (8)	0.1229 (15)	0.1047 (13)	−0.0127 (8)	0.0434 (8)	−0.0478 (11)
S2	0.127 (5)	0.084 (4)	0.081 (3)	−0.049 (4)	0.029 (3)	−0.031 (2)
C20	0.144 (9)	0.087 (7)	0.124 (9)	−0.049 (7)	0.006 (8)	−0.023 (6)
S2X	0.094 (4)	0.058 (5)	0.114 (7)	−0.028 (3)	0.028 (4)	−0.025 (3)
C20X	0.144 (9)	0.087 (7)	0.124 (9)	−0.049 (7)	0.006 (8)	−0.023 (6)
S3	0.070 (4)	0.142 (10)	0.075 (5)	0.025 (5)	−0.007 (3)	0.036 (5)
C21	0.074 (5)	0.134 (9)	0.090 (7)	0.001 (5)	0.005 (4)	0.032 (6)
S3X	0.079 (7)	0.097 (5)	0.066 (6)	0.032 (4)	0.014 (5)	0.027 (5)
C21X	0.074 (5)	0.134 (9)	0.090 (7)	0.001 (5)	0.005 (4)	0.032 (6)
O1	0.076 (2)	0.069 (2)	0.081 (3)	0.018 (2)	0.037 (2)	−0.0059 (19)
O2	0.089 (3)	0.111 (4)	0.047 (2)	0.008 (3)	−0.001 (2)	0.008 (2)
O3	0.067 (2)	0.075 (3)	0.117 (4)	0.022 (2)	0.040 (2)	0.009 (2)
O4	0.065 (2)	0.116 (4)	0.117 (4)	0.026 (3)	0.007 (3)	−0.020 (3)
O5	0.107 (3)	0.103 (3)	0.062 (3)	−0.028 (3)	0.013 (2)	0.019 (2)
O6	0.098 (3)	0.112 (4)	0.095 (3)	0.033 (3)	0.038 (3)	−0.018 (3)
O7	0.086 (3)	0.099 (3)	0.097 (3)	−0.044 (3)	0.038 (2)	−0.028 (3)
O8	0.134 (4)	0.092 (4)	0.239 (7)	0.029 (3)	0.141 (5)	0.042 (4)
O9	0.286 (9)	0.112 (4)	0.062 (4)	−0.028 (5)	0.059 (5)	−0.002 (3)
O10	0.065 (2)	0.065 (2)	0.083 (3)	0.003 (2)	0.005 (2)	−0.0114 (19)
O11	0.090 (3)	0.070 (3)	0.143 (4)	−0.025 (2)	0.043 (3)	0.016 (3)
C1	0.045 (2)	0.041 (2)	0.049 (2)	0.0043 (17)	0.0162 (18)	−0.0003 (17)
C2	0.048 (2)	0.059 (3)	0.061 (3)	−0.012 (2)	0.019 (2)	−0.019 (2)
C3	0.044 (2)	0.068 (3)	0.072 (3)	−0.018 (2)	0.024 (2)	−0.017 (2)
C4	0.042 (2)	0.060 (3)	0.057 (3)	0.003 (2)	0.019 (2)	−0.004 (2)
C5	0.052 (2)	0.063 (3)	0.067 (3)	−0.010 (2)	0.027 (2)	−0.022 (2)
C6	0.043 (2)	0.062 (3)	0.060 (3)	−0.012 (2)	0.020 (2)	−0.015 (2)
C7	0.047 (2)	0.048 (2)	0.038 (2)	0.0006 (18)	0.0132 (17)	−0.0042 (16)
C8	0.062 (3)	0.044 (2)	0.054 (3)	−0.001 (2)	0.021 (2)	−0.0018 (19)
C9	0.084 (4)	0.053 (3)	0.070 (4)	−0.008 (3)	0.036 (3)	−0.013 (2)
C10	0.069 (3)	0.067 (3)	0.067 (4)	−0.020 (3)	0.032 (3)	−0.028 (3)
C11	0.065 (3)	0.087 (4)	0.050 (3)	−0.010 (3)	0.010 (2)	−0.018 (3)
C12	0.067 (3)	0.058 (3)	0.047 (3)	−0.001 (2)	0.012 (2)	−0.001 (2)
C13	0.043 (2)	0.041 (2)	0.042 (2)	−0.0020 (16)	0.0122 (17)	−0.0006 (16)
C14	0.057 (3)	0.077 (4)	0.057 (3)	0.014 (2)	0.027 (2)	0.014 (2)
C15	0.052 (3)	0.083 (4)	0.074 (4)	0.019 (3)	0.025 (3)	0.017 (3)
C16	0.046 (2)	0.068 (3)	0.052 (3)	0.002 (2)	−0.001 (2)	0.005 (2)
C17	0.069 (3)	0.069 (3)	0.042 (3)	0.001 (3)	0.010 (2)	0.008 (2)
C18	0.057 (3)	0.065 (3)	0.049 (3)	0.012 (2)	0.021 (2)	0.010 (2)
C19	0.049 (3)	0.130 (6)	0.100 (5)	−0.005 (3)	0.037 (3)	−0.012 (4)
C22	0.056 (2)	0.055 (3)	0.047 (3)	0.000 (2)	0.020 (2)	−0.0001 (19)
C23	0.064 (3)	0.058 (3)	0.061 (3)	0.006 (2)	0.022 (3)	0.012 (2)
C24	0.052 (2)	0.047 (3)	0.064 (3)	0.002 (2)	0.020 (2)	0.004 (2)
C25	0.044 (2)	0.080 (4)	0.076 (4)	0.001 (3)	0.009 (2)	−0.012 (3)
C26	0.057 (3)	0.073 (4)	0.065 (4)	−0.017 (3)	0.010 (3)	0.001 (3)
C27	0.071 (3)	0.073 (4)	0.051 (3)	0.000 (3)	0.019 (3)	−0.003 (2)
C28	0.058 (3)	0.075 (4)	0.065 (3)	−0.015 (3)	0.022 (3)	−0.011 (3)
C29	0.106 (5)	0.061 (4)	0.152 (7)	0.002 (3)	0.094 (5)	0.016 (4)
C30	0.162 (7)	0.064 (4)	0.072 (5)	−0.015 (4)	0.054 (5)	−0.001 (3)
C31	0.059 (3)	0.050 (3)	0.054 (3)	−0.007 (2)	0.012 (2)	−0.002 (2)
C32	0.068 (3)	0.063 (3)	0.084 (4)	−0.003 (3)	0.029 (3)	0.016 (3)

Geometric parameters (Å, º) top

Os1—C23	1.872 (6)	O3—C24	1.131 (6)
Os1—C22	1.944 (5)	O4—C25	1.139 (7)
Os1—C24	1.950 (5)	O5—C26	1.129 (7)
Os1—As1	2.4603 (5)	O6—C27	1.137 (7)
Os1—Os3	2.8611 (3)	O7—C28	1.130 (6)
Os1—Os2	2.9150 (3)	O8—C29	1.139 (7)
Os2—C26	1.910 (6)	O9—C30	1.142 (8)
Os2—C28	1.921 (6)	O10—C31	1.128 (6)
Os2—C27	1.939 (6)	O11—C32	1.112 (7)
Os2—C25	1.943 (6)	C1—C2	1.368 (6)
Os2—Os3	2.8817 (4)	C1—C6	1.389 (6)
Os3—C30	1.898 (8)	C2—C3	1.396 (7)
Os3—C32	1.929 (6)	C2—H2A	0.9300
Os3—C31	1.938 (6)	C3—C4	1.383 (7)
Os3—C29	1.951 (7)	C3—H3A	0.9300
As1—C13	1.936 (4)	C4—C5	1.377 (6)
As1—C7	1.943 (4)	C5—C6	1.379 (6)
As1—C1	1.948 (4)	C5—H5A	0.9300
S1—C4	1.757 (5)	C6—H6A	0.9300
S1—C19	1.760 (6)	C7—C12	1.369 (6)
S2—C10	1.759 (8)	C7—C8	1.397 (6)
S2—C20	1.775 (17)	C8—C9	1.376 (7)
C20—H20A	0.9600	C8—H8A	0.9300
C20—H20B	0.9600	C9—C10	1.372 (8)
C20—H20C	0.9600	C9—H9A	0.9300
S2X—C20X	1.59 (3)	C10—C11	1.400 (8)
S2X—C10	1.809 (10)	C11—C12	1.373 (7)
C20X—H20D	0.9600	C11—H11A	0.9300
C20X—H20E	0.9600	C12—H12A	0.9300
C20X—H20F	0.9600	C13—C14	1.372 (6)
S3—C16	1.765 (16)	C13—C18	1.372 (6)
S3—C21	1.82 (2)	C14—C15	1.377 (7)
C21—H21A	0.9600	C14—H14A	0.9300
C21—H21B	0.9600	C15—C16	1.380 (7)
C21—H21C	0.9600	C15—H15A	0.9300
S3X—C21X	1.75 (4)	C16—C17	1.375 (8)
S3X—C16	1.75 (3)	C17—C18	1.393 (7)
C21X—H21D	0.9600	C17—H17A	0.9300
C21X—H21E	0.9600	C18—H18A	0.9300
C21X—H21F	0.9600	C19—H19A	0.9600
O1—C22	1.124 (6)	C19—H19B	0.9600
O2—C23	1.155 (6)	C19—H19C	0.9600

C23—Os1—C22	88.8 (2)	H21D—C21X—H21F	109.5
C23—Os1—C24	88.3 (2)	H21E—C21X—H21F	109.5
C22—Os1—C24	176.7 (2)	C2—C1—C6	118.8 (4)
C23—Os1—As1	102.89 (16)	C2—C1—As1	122.1 (3)
C22—Os1—As1	90.24 (14)	C6—C1—As1	119.1 (3)
C24—Os1—As1	88.87 (14)	C1—C2—C3	120.6 (4)
C23—Os1—Os3	97.90 (16)	C1—C2—H2A	119.7
C22—Os1—Os3	88.04 (14)	C3—C2—H2A	119.7
C24—Os1—Os3	93.91 (14)	C4—C3—C2	120.9 (4)
As1—Os1—Os3	159.100 (13)	C4—C3—H3A	119.5
C23—Os1—Os2	157.23 (16)	C2—C3—H3A	119.5
C22—Os1—Os2	94.70 (14)	C5—C4—C3	117.7 (4)
C24—Os1—Os2	88.54 (15)	C5—C4—S1	117.7 (4)
As1—Os1—Os2	99.586 (13)	C3—C4—S1	124.7 (4)
Os3—Os1—Os2	59.847 (8)	C4—C5—C6	121.9 (4)
C26—Os2—C28	101.9 (2)	C4—C5—H5A	119.1
C26—Os2—C27	89.2 (2)	C6—C5—H5A	119.1
C28—Os2—C27	90.9 (2)	C5—C6—C1	120.1 (4)
C26—Os2—C25	88.5 (3)	C5—C6—H6A	120.0
C28—Os2—C25	95.8 (2)	C1—C6—H6A	120.0
C27—Os2—C25	173.2 (2)	C12—C7—C8	118.3 (4)
C26—Os2—Os3	167.70 (16)	C12—C7—As1	119.5 (3)
C28—Os2—Os3	90.40 (17)	C8—C7—As1	121.9 (3)
C27—Os2—Os3	91.81 (16)	C9—C8—C7	120.8 (5)
C25—Os2—Os3	89.11 (19)	C9—C8—H8A	119.6
C26—Os2—Os1	108.61 (16)	C7—C8—H8A	119.6
C28—Os2—Os1	149.54 (17)	C10—C9—C8	120.6 (5)
C27—Os2—Os1	89.70 (16)	C10—C9—H9A	119.7
C25—Os2—Os1	85.01 (16)	C8—C9—H9A	119.7
Os3—Os2—Os1	59.148 (8)	C9—C10—C11	118.7 (5)
C30—Os3—C32	101.0 (3)	C9—C10—S2	130.7 (5)
C30—Os3—C31	91.4 (3)	C11—C10—S2	110.6 (5)
C32—Os3—C31	91.2 (2)	C9—C10—S2X	109.6 (5)
C30—Os3—C29	91.0 (4)	C11—C10—S2X	131.7 (6)
C32—Os3—C29	90.0 (3)	C12—C11—C10	120.3 (5)
C31—Os3—C29	177.1 (3)	C12—C11—H11A	119.9
C30—Os3—Os1	96.2 (2)	C10—C11—H11A	119.9
C32—Os3—Os1	162.78 (18)	C7—C12—C11	121.2 (5)
C31—Os3—Os1	86.62 (15)	C7—C12—H12A	119.4
C29—Os3—Os1	91.50 (18)	C11—C12—H12A	119.4
C30—Os3—Os2	157.2 (2)	C14—C13—C18	118.2 (4)
C32—Os3—Os2	101.86 (18)	C14—C13—As1	120.0 (3)
C31—Os3—Os2	87.73 (15)	C18—C13—As1	121.8 (3)
C29—Os3—Os2	89.4 (2)	C13—C14—C15	120.8 (5)
Os1—Os3—Os2	61.005 (6)	C13—C14—H14A	119.6
C13—As1—C7	101.94 (18)	C15—C14—H14A	119.6
C13—As1—C1	101.79 (18)	C14—C15—C16	120.9 (5)
C7—As1—C1	100.94 (18)	C14—C15—H15A	119.5
C13—As1—Os1	117.92 (12)	C16—C15—H15A	119.5
C7—As1—Os1	115.62 (13)	C17—C16—C15	119.0 (4)
C1—As1—Os1	116.07 (12)	C17—C16—S3X	117.6 (10)
C4—S1—C19	104.5 (3)	C15—C16—S3X	123.1 (10)
C10—S2—C20	99.4 (6)	C17—C16—S3	122.7 (7)
S2—C20—H20A	109.5	C15—C16—S3	118.2 (7)
S2—C20—H20B	109.5	C16—C17—C18	119.3 (5)
H20A—C20—H20B	109.5	C16—C17—H17A	120.3
S2—C20—H20C	109.5	C18—C17—H17A	120.3
H20A—C20—H20C	109.5	C13—C18—C17	121.7 (5)
H20B—C20—H20C	109.5	C13—C18—H18A	119.1
C20X—S2X—C10	99.1 (9)	C17—C18—H18A	119.1
S2X—C20X—H20D	109.5	S1—C19—H19A	109.5
S2X—C20X—H20E	109.5	S1—C19—H19B	109.5
H20D—C20X—H20E	109.5	H19A—C19—H19B	109.5
S2X—C20X—H20F	109.5	S1—C19—H19C	109.5
H20D—C20X—H20F	109.5	H19A—C19—H19C	109.5
H20E—C20X—H20F	109.5	H19B—C19—H19C	109.5
C16—S3—C21	104.6 (10)	O1—C22—Os1	175.3 (4)
S3—C21—H21A	109.5	O2—C23—Os1	177.4 (5)
S3—C21—H21B	109.5	O3—C24—Os1	174.4 (5)
H21A—C21—H21B	109.5	O4—C25—Os2	174.3 (6)
S3—C21—H21C	109.5	O5—C26—Os2	175.7 (5)
H21A—C21—H21C	109.5	O6—C27—Os2	175.0 (5)
H21B—C21—H21C	109.5	O7—C28—Os2	178.4 (5)
C21X—S3X—C16	101.8 (16)	O8—C29—Os3	177.2 (5)
S3X—C21X—H21D	109.5	O9—C30—Os3	176.4 (8)
S3X—C21X—H21E	109.5	O10—C31—Os3	174.9 (5)
H21D—C21X—H21E	109.5	O11—C32—Os3	177.9 (6)
S3X—C21X—H21F	109.5

C6—C1—C2—C3	−0.3 (8)	C9—C10—C11—C12	−0.6 (8)
As1—C1—C2—C3	−179.5 (4)	S2—C10—C11—C12	−179.9 (5)
C1—C2—C3—C4	0.1 (9)	S2X—C10—C11—C12	175.7 (7)
C2—C3—C4—C5	0.0 (8)	C8—C7—C12—C11	2.9 (7)
C2—C3—C4—S1	179.5 (4)	As1—C7—C12—C11	−171.9 (4)
C19—S1—C4—C5	163.2 (5)	C10—C11—C12—C7	−2.2 (8)
C19—S1—C4—C3	−16.3 (6)	C18—C13—C14—C15	1.6 (8)
C3—C4—C5—C6	0.3 (8)	As1—C13—C14—C15	−177.4 (5)
S1—C4—C5—C6	−179.3 (4)	C13—C14—C15—C16	−2.0 (9)
C4—C5—C6—C1	−0.5 (8)	C14—C15—C16—C17	1.0 (9)
C2—C1—C6—C5	0.6 (8)	C14—C15—C16—S3X	−173.2 (14)
As1—C1—C6—C5	179.7 (4)	C14—C15—C16—S3	178.0 (9)
C12—C7—C8—C9	−0.9 (7)	C21X—S3X—C16—C17	163.8 (12)
As1—C7—C8—C9	173.8 (4)	C21X—S3X—C16—C15	−22 (2)
C7—C8—C9—C10	−1.9 (8)	C21—S3—C16—C17	4.3 (15)
C8—C9—C10—C11	2.6 (8)	C21—S3—C16—C15	−172.7 (8)
C8—C9—C10—S2	−178.3 (5)	C15—C16—C17—C18	0.3 (8)
C8—C9—C10—S2X	−174.5 (6)	S3X—C16—C17—C18	174.9 (13)
C20—S2—C10—C9	15.4 (10)	S3—C16—C17—C18	−176.6 (9)
C20—S2—C10—C11	−165.3 (8)	C14—C13—C18—C17	−0.3 (7)
C20X—S2X—C10—C9	161.1 (12)	As1—C13—C18—C17	178.7 (4)
C20X—S2X—C10—C11	−15.4 (15)	C16—C17—C18—C13	−0.7 (8)

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C5—H5A···O10ⁱ	0.93	2.55	3.41 (1)	154

Symmetry code: (i) −x+1, −y+2, −z+2.

The d_norm contact distances (Å, adjusted to neutron values) for all identified interactions present in the major and minor components of 1 with respect to the corresponding sum of van der Waals radii of the relevant contact atoms top

Contact	d_norm Distance	ΣvdW radii	Δ(ΣvdW – d_norm distance)	Symmetry operation
Major
C5–H5A···O10	2.41	2.61	0.20	1 - x, 2 - y, 2 - z
C20–H20A···C21	2.57	2.61	0.04	-1/2 + x, 1/2 - y, -1/2 + z
C21–H21B···C20	2.64	2.79	0.15	1/2 + x, 1/2 - y, 1/2 + z
S3···O10	3.21	3.32	0.11	1/2 + x, 3/2 - y, 1/2 + z
O7···O7	2.95	3.04	0.09	2 - x, 2 - y, 2 - z
Minor
C5–H5A···O10	2.41	2.61	0.20	1 - x, 2 - y, 2 - z
S3X···O10	3.13	3.32	0.19	1/2 + x, 3/2 - y, 1/2 + z
O7···O7	2.95	3.04	0.09	2 - x, 2 - y, 2 - z
C21X–H21D···O1	2.55	2.61	0.06	2 - x, 1 - y, 2 - z

Acknowledgements

The authors are grateful to Dr Imthyaz Ahmed Khan for his contribution to the synthesis of the title compound. SSS thanks Universiti Teknologi MARA (UiTM) for providing the research facilities.

References

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