Re-refinement of dineodymium tris­[sulfate­(VI)] tetra­hydrate

Jiajaroen, S.; Theppitak, C.; Laksee, S.; Chainok, K.

doi:10.1107/S2414314626001756

inorganic compounds

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ISSN: 2414-3146

Volume 11| Part 2| February 2026| x260175

https://doi.org/10.1107/S2414314626001756

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Re-refinement of dineodymium tris[sulfate(VI)] tetrahydrate

Suwadee Jiajaroen,^a ^* Chatphorn Theppitak,^b Sakchai Laksee ^c and Kittipong Chainok ^d

^aDivision of Science and Mathematic, Faculty of Science and Technology, Rajamangala University of Technology Tawan-ok, Bangpra, Sriracha, Chonburi, 20110, Thailand, ^bChulabhorn Research Institute, Lak Si, Bangkok 10210, Thailand, ^cThailand Institute of Nuclear Technology (Public, Organization), Nakhon Nayok 26120, Thailand, and ^dThammasat University Research Unit in Multifunctional Crystalline Materials and Applications (TU-MCMA), Faculty of Science and Technology, Thammasat, University, Khlong Luang, Pathum Thani, 12121, Thailand
^*Correspondence e-mail: [email protected]

Edited by M. Weil, Vienna University of Technology, Austria (Received 5 February 2026; accepted 18 February 2026; online 27 February 2026)

The crystal structure of the title compound, poly[tetraaquatri-μ-sulfato-dineodymium], [Nd₂(SO₄)₃(H₂O)₄]_n, was re-refined from modern CCD-based single-crystal X-ray diffraction data. In comparison with the original report [Bede (1987 ). Jiegou Huaxue, 6, 70–74], the re-refinement shows improved precision and accuracy, with all hydrogen atoms being located. The crystal structure comprises two crystallographically independent Nd^III sites. One adopts a capped square-antiprismatic and the other a square-antiprismatic coordination environment. The cations are interconnected by bridging sulfato ligands into a framework structure that is reinforced by classical O—H⋯O hydrogen-bonding interactions of medium to weak strengths.

Keywords: crystal structure; neodymium(III) sulfate; redetermination.

CCDC reference: 2531694

Structure description

Coordination networks comprising lanthanide metal ions have attracted considerable interest in recent decades due to their structural complexity and functional properties in optical and magnetic materials, resulting from their unpaired electrons in f-orbitals (Patra & Pal, 2025 ; Mautner et al., 2021 ; Cui et al., 2012 ; Eliseeva & Bünzli, 2010 ). Since lanthanide ions favour hard donor atoms, a variety of organic ligands with oxygen atoms have been used extensively for the creation of different lanthanide coordination networks. Among them, polycarboxylic acids, particularly aromatic dicarboxylic acids like terephthalic acid (H₂bdc) and its derivatives, have been extensively used as bridging linkers in the formation of lanthanide coordination networks (He et al., 2020 ; Bai et al., 2016 ), demonstrating significant luminescent properties (Alexander et al., 2025 ). Furthermore, negatively charged polyatomic ions or oxyanions such as nitrate, sulfate, or carbonate are effective as linkers in the construction of neutral coordination networks (Yimklan et al., 2024 ; Guo et al., 2023 ). These networks display intriguing magnetic features attributable to the diverse coordination modes of oxyanions that connect the lanthanide cations in close proximity.

In the context given above, we reacted neodymium chloride with 1-(4-carboxyphenyl)-5-mercapto-1H-tetrazole (cmt) under solvothermal conditions. This reaction unexpectedly yielded crystals of the inorganic title compound [Nd₂(SO₄)₃(H₂O)₄] (Fig. 1). The sulfate anion was probably generated from the decomposition of cmt under the solvothermal conditions. A search of the Inorganic Crystal Structure Database (ICSD; Zagorac et al., 2019 ) revealed that the crystal structure of this compound has been determined previously (collection code 68006; Bede, 1987). Isotypic lanthanide (Ln) crystal structures are reported for Ln = Ce (240937; Xu, 2008 ; 417417; Casari & Langer, 2007 ), Ln = Pr (422431; Kazmierczak & Hoeppe, 2011 ), Ln = La (68005; Bede, 1987), and Ln = Eu (420715; Choi et al., 2010 ). The current re-refinement of [Nd₂(SO₄)₃(H₂O)₄] provides improved precision of atomic coordinates and displacement parameters and more accurate bond lengths and bond angles. All hydrogen-atom positions were located from difference-Fourier maps and refined, allowing a more reliable description of the hydrogen-bonding interactions between water molecules and sulfate anions (Table 1).

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O13—H13A⋯O4ⁱ	0.82 (2)	2.10 (4)	2.838 (4)	149 (5)
O13—H13B⋯O11ⁱⁱ	0.82 (2)	2.01 (3)	2.776 (4)	156 (6)
O14—H14A⋯O8ⁱⁱⁱ	0.83 (2)	2.52 (6)	3.038 (4)	121 (6)
O14—H14A⋯O12	0.83 (2)	2.36 (6)	2.933 (4)	127 (6)
O14—H14B⋯O5^iv	0.84 (2)	1.96 (2)	2.785 (4)	166 (5)
O15—H15A⋯O10^v	0.84 (2)	2.03 (3)	2.798 (4)	151 (6)
O15—H15B⋯O5^vi	0.84 (2)	2.54 (6)	3.141 (4)	130 (7)
O15—H15B⋯O13^vi	0.84 (2)	2.47 (5)	3.194 (4)	145 (7)
O16—H16A⋯O4^v	0.82 (2)	2.02 (3)	2.799 (4)	157 (6)
O16—H16B⋯O10^v	0.84 (2)	1.87 (2)	2.676 (4)	162 (5)
Symmetry codes: (i) $[-x+{\script{1\over 2}}, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) $[-x+{\script{1\over 2}}, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (iii) $[x-{\script{1\over 2}}, -y+{\script{1\over 2}}, z+{\script{1\over 2}}]$ ; (iv) ; (v) $[x+{\script{1\over 2}}, -y+{\script{3\over 2}}, z-{\script{1\over 2}}]$ ; (vi) .

Figure 1
The asymmetric unit of [Nd₂(SO₄)₃(H₂O)₄] expanded to show the full coordination spheres of the Nd atoms. Displacement ellipsoids are drawn at the 50% probability level; hydrogen-bonding interactions are shown as dashed lines. [Symmetry codes: (i) −x + 1, −y + 1, −z + 1; (ii) x, y − 1, z; (iii) −x + $[{3\over 2}]$ , y + $[{1\over 2}]$ , −z + $[{1\over 2}]$ ; (iv) −x + $[{1\over 2}]$ , y + $[{1\over 2}]$ , −z + $[{1\over 2}]$ ; (v) x + $[{1\over 2}]$ , −y + $[{1\over 2}]$ , z − $[{1\over 2}]$ .]

The asymmetric unit comprises two Nd^III cations (Nd1 and Nd2), three sulfate anions (S1–S3), and four coordinating water molecules (O13–O16) (Fig.1). The shapes of the coordination polyhedra around the Nd^III cations were calculated using the SHAPE program (Llunell et al., 2013 ). The Nd1 site exhibits a distorted capped square-antiprismatic (CSAPR-9) [NdO₉] coordination environment, comprising seven oxygen atoms from six different sulfate anions and two oxygen atoms from the coordinating water molecules. The Nd2 site has a distorted square-antiprismatic (SAPR-8) [NdO₈] coordination environment defined by six oxygen atoms from five distinct sulfate anions and two oxygen atoms from the coordinating water molecules. The Nd—O bond lengths range from 2.318 (3) to 2.676 (3) Å, while the O—Nd—O bond angles vary from 53.94 (8) to 150.36 (8)°. Bond lengths of the tetrahedral sulfate groups are in typical ranges [1.446 (3)–1.503 (2) Å].

Each Nd1 site is connected through μ₄-κ²O,O′:κO:κO′:κO′′ bridging sulfato ligands, forming a double chain parallel to [010]. Nd1 and Nd2 sites are interlinked to generate a sheet structure extending parallel (100) through μ₄-κ²O,O′:κO:κO′:κO′′ and μ₄-κO:κO′:κO′′:κO′′′ bridging sulfato ligands (Fig. 2). These sheets are interconnected via another sulfato ligand in a μ₃-κ²O,O′:κO:κO' bridging mode along [001] (Fig. 3). Hydrogen-bonding interactions of medium to weak strengths between water molecules and sulfate O atoms, including two bifurcated hydrogen bonds (Table 1), consolidate the packing.

Figure 2
The (100) sheet in the title compound in a view along [101]. Water molecules are omitted for clarity.

Figure 3
The crystal structure of the title compound in a viewe along [001].

Fig. 4 shows the infrared spectrum of the title compound. The broad absorption bands observed at around 3016 and 3502 cm⁻¹ correspond to O—H stretching vibrations of coordinating water molecules. The strong bands in the 972–1074 cm⁻¹ region signify the vibration modes of the sulfate groups.

Figure 4
IR spectrum of the title compound.

Synthesis and crystallization

All reagents were of analytical grade and were used as received without further purification. A mixture solution of NdCl₃·6H₂O (35.9 mg, 0.1 mmol) and cmt (22.2 mg, 0.1 mmol) in mixed EtOH (3 ml) and H₂O (2 ml) solution was added into a 15 ml Teflon lined reactor. The mixture solution was stirred at room temperature for 10 min, sealed in a stainless steel autoclave and heated in an oven at 428 K under autogenous pressure for 24 h. After cooling to room temperature and filtration, pink crystals were obtained in 45% yield (16.2 mg) based on NdCl₃·6H₂O.

An infrared (IR) spectrum was recorded on a Perkin-Elmer model Spectrum 100 spectrometer in the ATR mode, in the range of 650–4000 cm⁻¹.

Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2.

Table 2
Experimental details

Crystal data
Chemical formula	[Nd₂(SO₄)₃(H₂O)₄]
M_r	648.72
Crystal system, space group	Monoclinic, P2₁/n
Temperature (K)	296
a, b, c (Å)	13.0092 (6), 7.2033 (3), 13.2968 (6)
β (°)	92.388 (2)
V (Å³)	1244.95 (10)
Z	4
Radiation type	Mo Kα
μ (mm⁻¹)	8.84
Crystal size (mm)	0.20 × 0.08 × 0.08

Data collection
Diffractometer	Bruker D8 QUEST CMOS
Absorption correction	Multi-scan (SADABS; Krause et al., 2015 )
T_min, T_max	0.578, 0.746
No. of measured, independent and observed [I > 2σ(I)] reflections	24828, 3099, 2819
R_int	0.066
(sin θ/λ)_max (Å⁻¹)	0.668

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.023, 0.059, 1.09
No. of reflections	3099
No. of parameters	223
No. of restraints	8
H-atom treatment	All H-atom parameters refined
Δρ_max, Δρ_min (e Å⁻³)	1.19, −1.63
Computer programs: APEX4 and SAINT (Bruker, 2021 ), SHELXT (Sheldrick, 2015a ), SHELXL (Sheldrick, 2015b ), OLEX2 (Dolomanov et al., 2009 ) and publCIF (Westrip, 2010 ).

Structural data

CCDC reference: 2531694

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2414314626001756/wm5790sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314626001756/wm5790Isup3.hkl

checkCIF report

Computing details top

Poly[tetraaquatri-µ-sulfato-dineodymium] top

Crystal data top

[Nd₂(SO₄)₃(H₂O)₄]	F(000) = 1216
M_r = 648.72	D_x = 3.461 Mg m⁻³
Monoclinic, P2₁/n	Mo Kα radiation, λ = 0.71073 Å
a = 13.0092 (6) Å	Cell parameters from 9967 reflections
b = 7.2033 (3) Å	θ = 3.1–28.4°
c = 13.2968 (6) Å	µ = 8.84 mm⁻¹
β = 92.388 (2)°	T = 296 K
V = 1244.95 (10) Å³	Plate, pink
Z = 4	0.20 × 0.08 × 0.08 mm

Data collection top

Bruker D8 QUEST CMOS diffractometer	3099 independent reflections
Radiation source: sealed x-ray tube	2819 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.066
Detector resolution: 7.39 pixels mm^-1	θ_max = 28.4°, θ_min = 3.1°
φ and ω scans	h = −17→17
Absorption correction: multi-scan (SADABS; Krause et al., 2015)	k = −9→9
T_min = 0.578, T_max = 0.746	l = −17→17
24828 measured reflections

Refinement top

Refinement on F²	Hydrogen site location: difference Fourier map
Least-squares matrix: full	All H-atom parameters refined
R[F² > 2σ(F²)] = 0.023	w = 1/[σ²(F_o²) + (0.0257P)² + 2.3205P] where P = (F_o² + 2F_c²)/3
wR(F²) = 0.059	(Δ/σ)_max = 0.001
S = 1.09	Δρ_max = 1.19 e Å⁻³
3099 reflections	Δρ_min = −1.62 e Å⁻³
223 parameters	Extinction correction: SHELXL-2019/1 (Sheldrick, 2015b), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
8 restraints	Extinction coefficient: 0.00229 (13)

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.

Refinement. The H atoms bound to O atoms were located from difference Fourier maps and were refined with distance restraints of O—H = 0.84 ± 0.02 Å and with U_iso(H) = 1.5U_eq(O).

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

	x	y	z	U_iso*/U_eq
Nd1	0.41471 (2)	0.25908 (2)	0.46486 (2)	0.01048 (7)
Nd2	0.57353 (2)	0.73670 (2)	0.14948 (2)	0.01158 (7)
S1	0.40088 (6)	0.76256 (10)	0.36613 (6)	0.01053 (17)
S2	0.65392 (6)	0.39592 (11)	0.34841 (6)	0.01083 (16)
S3	0.13844 (6)	0.11067 (11)	0.45661 (6)	0.01159 (16)
O1	0.45540 (18)	0.5984 (3)	0.41346 (18)	0.0138 (5)
O2	0.4361 (2)	0.7922 (4)	0.26405 (19)	0.0179 (5)
O3	0.43662 (19)	0.9222 (3)	0.43036 (18)	0.0153 (5)
O4	0.2906 (2)	0.7380 (3)	0.3657 (2)	0.0187 (6)
O5	0.5769 (2)	0.2568 (3)	0.3787 (2)	0.0166 (6)
O6	0.6119 (2)	0.4962 (4)	0.26066 (18)	0.0205 (5)
O7	0.67762 (18)	0.5244 (4)	0.43216 (19)	0.0164 (5)
O8	0.74692 (19)	0.2962 (4)	0.3207 (2)	0.0177 (5)
O9	0.23938 (18)	0.1645 (4)	0.42137 (19)	0.0190 (5)
O10	0.0759 (2)	0.2808 (3)	0.4724 (2)	0.0175 (5)
O11	0.07797 (18)	0.0010 (3)	0.38166 (18)	0.0171 (5)
O12	0.15163 (19)	0.0109 (4)	0.55274 (18)	0.0187 (5)
O13	0.3728 (2)	0.2806 (5)	0.2807 (2)	0.0267 (7)
H13A	0.317 (3)	0.244 (7)	0.256 (4)	0.042 (18)*
H13B	0.389 (5)	0.369 (6)	0.246 (4)	0.062 (19)*
O14	0.3584 (2)	0.1111 (4)	0.6308 (2)	0.0214 (6)
H14A	0.297 (2)	0.126 (11)	0.644 (5)	0.08 (2)*
H14B	0.372 (4)	−0.003 (3)	0.637 (4)	0.039 (14)*
O15	0.5499 (2)	1.0738 (4)	0.1648 (2)	0.0247 (6)
H15A	0.549 (4)	1.152 (7)	0.117 (3)	0.052 (17)*
H15B	0.527 (6)	1.160 (8)	0.200 (5)	0.09 (3)*
O16	0.63068 (19)	0.8621 (4)	−0.01063 (19)	0.0177 (5)
H16A	0.677 (3)	0.805 (7)	−0.038 (4)	0.049 (17)*
H16B	0.628 (4)	0.978 (3)	−0.018 (4)	0.032 (13)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Nd1	0.00967 (11)	0.01244 (11)	0.00959 (10)	−0.00025 (6)	0.00351 (7)	−0.00079 (6)
Nd2	0.00989 (11)	0.01386 (11)	0.01126 (11)	0.00054 (6)	0.00388 (7)	0.00217 (6)
S1	0.0091 (4)	0.0129 (4)	0.0097 (4)	0.0001 (3)	0.0029 (3)	−0.0006 (3)
S2	0.0096 (4)	0.0135 (4)	0.0097 (4)	0.0012 (3)	0.0044 (3)	0.0012 (3)
S3	0.0092 (4)	0.0148 (4)	0.0111 (4)	−0.0004 (3)	0.0030 (3)	0.0006 (3)
O1	0.0142 (11)	0.0119 (11)	0.0155 (12)	0.0019 (9)	0.0029 (9)	0.0004 (9)
O2	0.0202 (13)	0.0238 (13)	0.0101 (12)	0.0023 (11)	0.0041 (10)	0.0014 (10)
O3	0.0185 (12)	0.0128 (11)	0.0149 (12)	0.0001 (9)	0.0035 (9)	−0.0026 (9)
O4	0.0110 (13)	0.0247 (14)	0.0205 (14)	−0.0014 (9)	0.0008 (10)	0.0004 (10)
O5	0.0161 (14)	0.0160 (13)	0.0184 (13)	−0.0021 (9)	0.0069 (10)	0.0003 (9)
O6	0.0239 (13)	0.0247 (13)	0.0131 (12)	0.0039 (11)	0.0017 (10)	0.0056 (10)
O7	0.0150 (12)	0.0191 (12)	0.0151 (11)	0.0016 (10)	0.0022 (9)	−0.0039 (10)
O8	0.0106 (12)	0.0228 (12)	0.0202 (13)	0.0033 (10)	0.0055 (10)	−0.0045 (11)
O9	0.0103 (11)	0.0267 (14)	0.0204 (13)	−0.0013 (10)	0.0064 (9)	0.0019 (11)
O10	0.0174 (13)	0.0160 (12)	0.0193 (13)	0.0037 (10)	0.0021 (10)	−0.0055 (10)
O11	0.0152 (12)	0.0187 (12)	0.0172 (12)	−0.0010 (10)	−0.0008 (9)	−0.0028 (10)
O12	0.0182 (12)	0.0251 (13)	0.0128 (11)	−0.0025 (10)	0.0006 (9)	0.0058 (10)
O13	0.0252 (16)	0.0401 (17)	0.0146 (14)	−0.0146 (13)	−0.0022 (12)	0.0111 (12)
O14	0.0161 (13)	0.0179 (13)	0.0308 (15)	0.0013 (10)	0.0073 (11)	0.0047 (12)
O15	0.0394 (17)	0.0172 (13)	0.0181 (14)	0.0021 (12)	0.0067 (12)	0.0023 (11)
O16	0.0168 (12)	0.0198 (13)	0.0171 (12)	0.0001 (10)	0.0078 (10)	0.0012 (11)

Geometric parameters (Å, º) top

Nd1—O1	2.598 (2)	S1—O3	1.495 (3)
Nd1—O1ⁱ	2.510 (2)	S1—O4	1.446 (3)
Nd1—O3ⁱⁱ	2.489 (2)	S2—O5	1.484 (3)
Nd1—O3ⁱ	2.676 (3)	S2—O6	1.459 (3)
Nd1—O5	2.443 (3)	S2—O7	1.471 (3)
Nd1—O7ⁱ	2.427 (2)	S2—O8	1.467 (2)
Nd1—O9	2.427 (2)	S3—O9	1.465 (2)
Nd1—O13	2.491 (3)	S3—O10	1.490 (3)
Nd1—O14	2.584 (3)	S3—O11	1.473 (3)
Nd2—O2	2.430 (2)	S3—O12	1.470 (3)
Nd2—O6	2.318 (3)	O13—H13A	0.82 (2)
Nd2—O8ⁱⁱⁱ	2.392 (2)	O13—H13B	0.82 (2)
Nd2—O10^iv	2.499 (3)	O14—H14A	0.83 (2)
Nd2—O11^iv	2.621 (2)	O14—H14B	0.84 (2)
Nd2—O12^v	2.445 (2)	O15—H15A	0.84 (2)
Nd2—O15	2.457 (3)	O15—H15B	0.84 (2)
Nd2—O16	2.456 (2)	O16—H16A	0.82 (2)
S1—O1	1.503 (2)	O16—H16B	0.837 (19)
S1—O2	1.466 (3)

O1ⁱ—Nd1—O1	69.25 (9)	O15—Nd2—O10^iv	80.31 (9)
O1ⁱ—Nd1—O3ⁱ	53.94 (8)	O15—Nd2—O11^iv	123.88 (9)
O1—Nd1—O3ⁱ	116.43 (7)	O16—Nd2—O10^iv	69.32 (8)
O1ⁱ—Nd1—O14	79.94 (8)	O16—Nd2—O11^iv	110.74 (8)
O3ⁱⁱ—Nd1—O1ⁱ	116.01 (8)	O16—Nd2—O15	75.62 (9)
O3ⁱⁱ—Nd1—O1	147.43 (8)	O1—S1—Nd1ⁱ	49.11 (10)
O3ⁱⁱ—Nd1—O3ⁱ	62.25 (10)	O2—S1—Nd1ⁱ	113.62 (11)
O3ⁱⁱ—Nd1—O13	84.36 (10)	O2—S1—O1	110.01 (14)
O3ⁱⁱ—Nd1—O14	78.11 (8)	O2—S1—O3	108.37 (15)
O5—Nd1—O1ⁱ	74.56 (9)	O3—S1—Nd1ⁱ	55.51 (10)
O5—Nd1—O1	72.16 (7)	O3—S1—O1	103.63 (15)
O5—Nd1—O3ⁱⁱ	78.41 (8)	O4—S1—Nd1ⁱ	134.98 (12)
O5—Nd1—O3ⁱ	67.75 (8)	O4—S1—O1	110.87 (14)
O5—Nd1—O13	72.38 (10)	O4—S1—O2	111.26 (17)
O5—Nd1—O14	132.77 (9)	O4—S1—O3	112.42 (15)
O7ⁱ—Nd1—O1	69.80 (8)	O6—S2—O5	108.43 (17)
O7ⁱ—Nd1—O1ⁱ	73.09 (8)	O6—S2—O7	110.72 (16)
O7ⁱ—Nd1—O3ⁱ	112.57 (8)	O6—S2—O8	109.10 (15)
O7ⁱ—Nd1—O3ⁱⁱ	142.58 (8)	O7—S2—O5	110.01 (15)
O7ⁱ—Nd1—O5	136.61 (8)	O8—S2—O5	108.09 (15)
O7ⁱ—Nd1—O9	80.36 (8)	O8—S2—O7	110.42 (15)
O7ⁱ—Nd1—O13	114.92 (10)	O9—S3—Nd2^vi	123.73 (11)
O7ⁱ—Nd1—O14	67.57 (8)	O9—S3—O10	109.19 (16)
O9—Nd1—O1ⁱ	150.36 (8)	O9—S3—O11	112.71 (15)
O9—Nd1—O1	113.64 (8)	O9—S3—O12	109.51 (15)
O9—Nd1—O3ⁱ	129.70 (8)	O10—S3—Nd2^vi	50.12 (11)
O9—Nd1—O3ⁱⁱ	78.24 (9)	O11—S3—Nd2^vi	54.81 (10)
O9—Nd1—O5	135.06 (9)	O11—S3—O10	104.88 (15)
O9—Nd1—O13	67.55 (9)	O12—S3—Nd2^vi	126.40 (10)
O9—Nd1—O14	77.92 (9)	O12—S3—O10	108.93 (16)
O13—Nd1—O1ⁱ	136.23 (9)	O12—S3—O11	111.46 (15)
O13—Nd1—O1	73.83 (9)	Nd1ⁱ—O1—Nd1	110.75 (9)
O13—Nd1—O3ⁱ	131.76 (9)	S1—O1—Nd1ⁱ	103.97 (12)
O13—Nd1—O14	143.79 (9)	S1—O1—Nd1	138.78 (14)
O14—Nd1—O1	132.89 (8)	S1—O2—Nd2	145.36 (17)
O14—Nd1—O3ⁱ	65.08 (8)	Nd1^vii—O3—Nd1ⁱ	117.75 (10)
O2—Nd2—O10^iv	79.18 (9)	S1—O3—Nd1^vii	145.10 (15)
O2—Nd2—O11^iv	68.74 (8)	S1—O3—Nd1ⁱ	97.07 (12)
O2—Nd2—O12^v	141.50 (9)	S2—O5—Nd1	136.75 (14)
O2—Nd2—O15	71.81 (9)	S2—O6—Nd2	160.63 (18)
O2—Nd2—O16	137.73 (9)	S2—O7—Nd1ⁱ	137.62 (14)
O6—Nd2—O2	82.39 (9)	S2—O8—Nd2^viii	148.89 (17)
O6—Nd2—O8ⁱⁱⁱ	81.12 (9)	S3—O9—Nd1	147.58 (16)
O6—Nd2—O10^iv	130.49 (9)	S3—O10—Nd2^vi	102.64 (13)
O6—Nd2—O11^iv	75.94 (9)	S3—O11—Nd2^vi	97.84 (12)
O6—Nd2—O12^v	72.98 (9)	S3—O12—Nd2^ix	141.08 (16)
O6—Nd2—O15	135.23 (9)	Nd1—O13—H13A	121 (4)
O6—Nd2—O16	139.71 (9)	Nd1—O13—H13B	124 (5)
O8ⁱⁱⁱ—Nd2—O2	127.28 (9)	H13A—O13—H13B	105 (6)
O8ⁱⁱⁱ—Nd2—O10^iv	144.39 (8)	Nd1—O14—H14A	116 (5)
O8ⁱⁱⁱ—Nd2—O11^iv	149.90 (9)	Nd1—O14—H14B	115 (3)
O8ⁱⁱⁱ—Nd2—O12^v	78.09 (9)	H14A—O14—H14B	108 (6)
O8ⁱⁱⁱ—Nd2—O15	86.19 (10)	Nd2—O15—H15A	126 (4)
O8ⁱⁱⁱ—Nd2—O16	75.46 (9)	Nd2—O15—H15B	146 (6)
O10^iv—Nd2—O11^iv	54.56 (8)	H15A—O15—H15B	86 (6)
O12^v—Nd2—O10^iv	94.64 (9)	Nd2—O16—H16A	117 (4)
O12^v—Nd2—O11^iv	76.73 (8)	Nd2—O16—H16B	116 (3)
O12^v—Nd2—O15	145.15 (9)	H16A—O16—H16B	119 (5)
O12^v—Nd2—O16	70.43 (9)

Nd1ⁱ—S1—O1—Nd1	146.9 (2)	O5—S2—O8—Nd2^viii	−118.4 (3)
Nd1ⁱ—S1—O2—Nd2	31.0 (3)	O6—S2—O5—Nd1	−75.7 (3)
Nd1ⁱ—S1—O3—Nd1^vii	176.3 (3)	O6—S2—O7—Nd1ⁱ	60.9 (3)
Nd2^vi—S3—O9—Nd1	141.0 (2)	O6—S2—O8—Nd2^viii	123.9 (3)
Nd2^vi—S3—O12—Nd2^ix	39.3 (3)	O7—S2—O5—Nd1	45.6 (3)
O1—S1—O2—Nd2	−22.0 (3)	O7—S2—O6—Nd2	21.7 (5)
O1—S1—O3—Nd1^vii	−173.3 (2)	O7—S2—O8—Nd2^viii	2.0 (4)
O1—S1—O3—Nd1ⁱ	10.33 (13)	O8—S2—O5—Nd1	166.2 (2)
O2—S1—O1—Nd1	−108.7 (2)	O8—S2—O6—Nd2	−100.1 (5)
O2—S1—O1—Nd1ⁱ	104.40 (15)	O8—S2—O7—Nd1ⁱ	−178.1 (2)
O2—S1—O3—Nd1^vii	69.8 (3)	O9—S3—O10—Nd2^vi	118.38 (14)
O2—S1—O3—Nd1ⁱ	−106.50 (13)	O9—S3—O11—Nd2^vi	−116.20 (14)
O3—S1—O1—Nd1	135.65 (19)	O9—S3—O12—Nd2^ix	−147.5 (2)
O3—S1—O1—Nd1ⁱ	−11.28 (14)	O10—S3—O9—Nd1	86.7 (3)
O3—S1—O2—Nd2	90.6 (3)	O10—S3—O11—Nd2^vi	2.48 (15)
O4—S1—O1—Nd1ⁱ	−132.11 (14)	O10—S3—O12—Nd2^ix	93.1 (3)
O4—S1—O1—Nd1	14.8 (3)	O11—S3—O9—Nd1	−157.1 (3)
O4—S1—O2—Nd2	−145.3 (3)	O11—S3—O10—Nd2^vi	−2.64 (16)
O4—S1—O3—Nd1ⁱ	130.11 (13)	O11—S3—O12—Nd2^ix	−22.1 (3)
O4—S1—O3—Nd1^vii	−53.6 (3)	O12—S3—O9—Nd1	−32.5 (4)
O5—S2—O6—Nd2	142.4 (5)	O12—S3—O10—Nd2^vi	−122.07 (14)
O5—S2—O7—Nd1ⁱ	−58.9 (3)	O12—S3—O11—Nd2^vi	120.19 (13)

Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x, y−1, z; (iii) −x+3/2, y+1/2, −z+1/2; (iv) −x+1/2, y+1/2, −z+1/2; (v) x+1/2, −y+1/2, z−1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) x, y+1, z; (viii) −x+3/2, y−1/2, −z+1/2; (ix) x−1/2, −y+1/2, z+1/2.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O13—H13A···O4^vi	0.82 (2)	2.10 (4)	2.838 (4)	149 (5)
O13—H13B···O11^iv	0.82 (2)	2.01 (3)	2.776 (4)	156 (6)
O14—H14A···O8^ix	0.83 (2)	2.52 (6)	3.038 (4)	121 (6)
O14—H14A···O12	0.83 (2)	2.36 (6)	2.933 (4)	127 (6)
O14—H14B···O5^x	0.84 (2)	1.96 (2)	2.785 (4)	166 (5)
O15—H15A···O10^xi	0.84 (2)	2.03 (3)	2.798 (4)	151 (6)
O15—H15B···O5^vii	0.84 (2)	2.54 (6)	3.141 (4)	130 (7)
O15—H15B···O13^vii	0.84 (2)	2.47 (5)	3.194 (4)	145 (7)
O16—H16A···O4^xi	0.82 (2)	2.02 (3)	2.799 (4)	157 (6)
O16—H16B···O10^xi	0.84 (2)	1.87 (2)	2.676 (4)	162 (5)

Symmetry codes: (iv) −x+1/2, y+1/2, −z+1/2; (vi) −x+1/2, y−1/2, −z+1/2; (vii) x, y+1, z; (ix) x−1/2, −y+1/2, z+1/2; (x) −x+1, −y, −z+1; (xi) x+1/2, −y+3/2, z−1/2.

Acknowledgements

This project was partially supported by the Thammasat University Research Unit in Multifunctional Crystalline Materials and Applications (TU-McMa).

Funding information

Funding for this research was provided by: Thailand Institute of Nuclear Technology (Public Organization), Thailand, through its program of TINT to University (grant to Suwadee Jiajaroen).

References

Alexander, C., Guo, Z., Glover, P. B., Faulkner, S. & Pikramenou, Z. (2025). Chem. Rev. 125, 2269–2370. CrossRef CAS PubMed Google Scholar
Bai, Y., Dou, Y., Xie, L.-H., Rutledge, W., Li, J.-R. & Zhou, H.-C. (2016). Chem. Soc. Rev. 45, 2327–2367. CrossRef CAS PubMed Google Scholar
Bede, S. (1987). Jiegou Huaxue 6, 70–74. Google Scholar
Bruker (2021). APEX4 and SAINT. Bruker AXS Inc.,Madison, Wisconsin, USA. Google Scholar
Casari, B. M. & Langer, V. (2007). Z. Anorg. Allge Chem. 633, 1074–1081. CrossRef CAS Google Scholar
Choi, M.-H., Kim, M.-K., Jo, V., Lee, D.-W., Shim, I.-W. & Ok, K.-M. (2010). Bull. Korean Chem. Soc. 31, 1077–1080. CrossRef CAS Google Scholar
Cui, Y., Yue, Y., Qian, G. & Chen, B. (2012). Chem. Rev. 112, 1126–1162. Web of Science CrossRef CAS PubMed Google Scholar
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann, H. (2009). J. Appl. Cryst. 42, 339–341. Web of Science CrossRef CAS IUCr Journals Google Scholar
Eliseeva, S. V. & Bünzli, J. G. (2010). Chem. Soc. Rev. 39, 189–227. Web of Science CrossRef CAS PubMed Google Scholar
Guo, Y. Y., Wang, R. D., Wei, W. M., Fang, F., Zhao, X. H., Zhang, S. S., Shen, T. Z., Zhang, J., Zhao, Q. H. & Wang, J. (2023). Dalton Trans. 52, 15940–15949. CrossRef CAS PubMed Google Scholar
He, Y.-P., Tan, Y.-X. & Zhang, J. (2020). Coord. Chem. Rev. 420, 213354. CrossRef Google Scholar
Kazmierczak, K. & Höppe, H. A. (2011). J. Solid State Chem. 184, 1221–1226. CrossRef CAS Google Scholar
Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015). J. Appl. Cryst. 48, 3–10. Web of Science CSD CrossRef ICSD CAS IUCr Journals Google Scholar
Llunell, M., Casanova, D., Cirera, A., Alemany, A. & Alvarez, S. (2013). SHAPE. University of Barcelona, Barcelona, Spain. Google Scholar
Mautner, F. A., Bierbaumer, F., Fischer, R. C., Torvisco, A., Vicente, R., Font-Bardía, M., Tubau, À., Speed, S. & Massoud, S. S. (2021). Inorganics 9, 74–88. CrossRef CAS Google Scholar
Patra, K. & Pal, H. (2025). RSC Sustainability 3, 629–660. Web of Science CrossRef CAS Google Scholar
Sheldrick, G. M. (2015a). Acta Cryst. A71, 3–8. Web of Science CrossRef IUCr Journals Google Scholar
Sheldrick, G. M. (2015b). Acta Cryst. C71, 3–8. Web of Science CrossRef IUCr Journals Google Scholar
Westrip, S. P. (2010). J. Appl. Cryst. 43, 920–925. Web of Science CrossRef CAS IUCr Journals Google Scholar
Xu, X. (2008). Acta Cryst. E64, i1. Web of Science CrossRef ICSD IUCr Journals Google Scholar
Yimklan, S., Kaeosamut, N., Sammawipawekul, N., Wongngam, S., Ngamsomrit, S., Rujiwatra, A. & Chimupala, Y. (2024). ACS Omega 9, 3988–3996. CAS PubMed Google Scholar
Zagorac, D., Müller, H., Ruehl, S., Zagorac, J. & Rehme, S. (2019). J. Appl. Cryst. 52, 918–925. Web of Science CrossRef CAS IUCr Journals Google Scholar