Tetra­ammonium μ-ethyl­enedi­amine­tetra­acetato-1κ3O,N,O′:2κ3O′′,N′,O′′′-bis­[trioxidotungstate(VI)] tetra­hydrate

Yaffa, L.; Pouye, S.F.; Ndoye, D.; Diallo, W.; Diop, M.; Sidibe, M.; Diop, C.A.K.

doi:10.1107/S2414314621009822

metal-organic compounds

IUCrDATA

ISSN: 2414-3146

Volume 6| Part 9| September 2021| x210982

https://doi.org/10.1107/S2414314621009822

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Tetraammonium μ-ethylenediaminetetraacetato-1κ³O,N,O′:2κ³O′′,N′,O′′′-bis[trioxidotungstate(VI)] tetrahydrate

Lamine Yaffa,^a ^* Sérigne Fallou Pouye,^a Daouda Ndoye,^a Waly Diallo,^a Mayoro Diop,^a Mamadou Sidibe ^a and Cheikh Abdoul Khadir Diop ^a

^aLaboratoire de Chimie Minérale et Analytique (LACHIMIA), Département de Chimie, Faculté des Sciences et Techniques, Université Cheikh Anta Diop, Dakar, Senegal
^*Correspondence e-mail: lamine.yaffa@ucad.edu.sn

Edited by W. Imhof, University Koblenz-Landau, Germany (Received 25 August 2021; accepted 21 September 2021; online 28 September 2021)

The title compound, (NH₄)₄[W₂(C₁₀H₁₂N₂O₈)O₆]·4H₂O, was obtained from a mixture of tungstic acid, ammonia and ethylenediaminetetraacetic acid (H₄edta) in a 2:4:1 ratio. The anion of the complex contains two WO₃ units and one bridging edta⁴⁻ ligand. Each central metal atom is tridentately coordinated by nitrogen and two carboxylate groups of the edta⁴⁻ ligand, together with the three oxido ligands, producing a distorted octahedral coordination environment around each tungsten atom. The center of the carbon–carbon bond of the ethylene bridge represents a crystallographic inversion center. The crystal structure consists of a three-dimensional supramolecular framework built up by the dinuclear cations, the ammonium counter-ions and the solvent water molecules via hydrogen bonds of the N—H⋯O and O—H⋯O type.

Keywords: crystal structure; ethylenediaminetetraacetate; tungstic acid; binuclear complex.

CCDC reference: 2112632

Structure description

Research on inorganic–organic framework materials is one of the fastest growing areas in materials chemistry because of their unique hybrid nature, which enables the combination of properties from both inorganic and organic materials (Cheetham & Rao, 2007 ). As organic ligands, polycarboxylates are multidentate chelating agents that are widespread in nature and industry because of their ability to coordinate with various transition metals in different ratios (Nicolau & Guy, 1995 ; Langer, 2000 ).

As a part of this field, molybdenum polycarboxylate complexes have thus been thoroughly investigated over the past three decades (Lee & Holm, 2004 ). Some well-characterized mono-, bi- and polynuclear molybdenum and tungsten complexes have been reported, for example Mo₂(O₂CCH₂OH)₄, M₂[MoO₃(C₂O₄)] (M = Na, K, Rb, Cs), Na₂[MO₂(C₆H₆O₇)₂]·3H₂O (M = Mo, W) (Cotton et al., 2002 ; Cindríc et al., 2000 ; Zhou et al., 1999 ). Structural analyses of W^VI–edta complexes are rare in the literature. Together with the structure of Na₂K₂[Mo₂O₆(edta)]·10H₂O, the structure of Na₄[W₂O₆(edta)]·8H₂O has been published (Lin et al., 2006 ).

Nevertheless, tungsten has been reported to incorporate into several enzymes (Johnson et al., 1996 ). In fact, tungsten could be a useful probe for the active site of molybdenum enzymes. As a consequence, more effort has been put into tungsten chemistry by inorganic and bioinorganic chemists (Bagno & Bonchio, 2000 ; Enemark et al., 2004 ; Sung & Holm, 2001 ; Zhou et al., 2004 ).

In this study, the reaction of H₄edta with tungstic acid has been investigated and a new binuclear 2:1 W–edta complex, (NH₄)₄[W₂(C₁₀H₁₂N₂O₈)O₆]·4H₂O, was isolated and structurally characterized.

As shown in Fig. 1, the dinuclear anion of the title compound shows one edta⁴⁻ ligand bonded to two tungstate WO₃ units. Each W atom is six-coordinate in a distorted octahedral environment built up by the tridentate facial coordination of one N and two O atoms of the edta⁴⁻ ligand as well as by three oxido ligands. The edta⁴⁻ ligand itself therefore acts as a bridge between the two WO₃ units, with the central carbon–carbon bond also representing a crystallographic center of inversion. The anion is accompanied by four ammonium cations and four solvent water molecules.

Figure 1
Molecular structure of the title compound. Displacement ellipsoids are drawn at the 50% probability level.

The three terminal oxido ligands bonded to the metal, i.e. W=Ot (Ot = O3, O6, O8) show bond lengths in a range 1.753 (2) to 1.759 (2) Å. The resulting Ot—W—Ot bond angles [105.05 (9), 105.14 (9), 103.12 (10)°] are considerably larger than 90° expected for a regular octahedron. Bond distances of the oxygen atoms of edta⁴⁻ to W are 2.135 (2) and 2.159 (2) Å, respectively and therefore significantly longer than the W=Ot bonds.

In the crystal structure, the complex anion, ammonium cations and solvent water molecules interact through medium–strong classical hydrogen bonds (Table 1). Two neighboring complexes are connected via hydrogen bonds of the N—H⋯Ow—H⋯O, N—H⋯O and Ow—H⋯O types. These interactions lead to the supramolacular structure shown in Fig. 2.

Table 1
Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O2—H2A⋯O3	0.87	1.88	2.743 (3)	171
O2—H2B⋯O5ⁱ	0.87	1.90	2.763 (3)	170
O1—H1A⋯O7	0.87	2.72	3.468 (3)	145
O1—H1A⋯O4	0.87	2.06	2.900 (3)	161
O1—H1B⋯O2ⁱⁱ	0.87	2.49	3.177 (3)	137
N10—H10A⋯O6	0.95 (4)	1.78 (4)	2.727 (3)	175 (3)
N10—H10B⋯O4ⁱⁱⁱ	0.81 (4)	2.20 (4)	2.996 (3)	168 (3)
N10—H10C⋯O7^iv	0.90 (4)	2.01 (4)	2.876 (3)	160 (3)
N10—H10D⋯O8^v	0.87 (4)	1.87 (4)	2.736 (3)	175 (4)
N11—H11A⋯O8	0.87 (5)	2.13 (5)	2.947 (3)	156 (4)
N11—H11B⋯O3^vi	0.84 (5)	2.31 (5)	3.109 (3)	160 (4)
N11—H11C⋯O1^vi	0.83 (4)	2.25 (4)	2.979 (4)	147 (4)
N11—H11D⋯O2^vii	0.92 (4)	1.93 (4)	2.846 (4)	173 (4)
Symmetry codes: (i) $[-x+1, y+{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (ii) ; (iii) ; (iv) ; (v) ; (vi) $[-x+1, y-{\script{1\over 2}}, -z+{\script{1\over 2}}]$ ; (vii) .

Figure 2
Supramolecular arrangement of the title compound established by classical hydrogen-bonding interactions (dashed lines).

Synthesis and crystallization

Tungstic acid (4 mmol, 0.999 g) and ammonia solution (8 mmol, 1.001 g) were mixed in 30 ml of water to solubilize the W^VI source. To this mixture was slowly added ethylenediammine-tetraacetic acid (H₄edta) (2 mmol, 0.584 g) under vigorous stirring. The solution was then stirred for two h at room temperature. The colorless solution thus obtained was left at room temperature for slow evaporation of water. After two weeks, colorless crystals (yield 11.6% based on W) were obtained from the solution.

The FT–infrared spectra of the title compound shows well-resolved absorption bands for the carboxylate of the coordinating edta⁴⁻ at 1651 cm⁻¹ and 1402 cm⁻¹, which are attributed to the antisymmetric and symmetric stretching vibrations ν(COO–). The bands at 926, 857 and 666 cm⁻¹ can be attributed to symmetric and asymmetric W=Ot stretching vibrations (Lin et al., 2006; Li et al., 2007 ). The range of 3500–2800 cm⁻¹ shows many bands ascribed to O—H stretching of water molecules, as well as N—H stretching vibrations of ammonium cations (Yaffa et al., 2020 ).

Refinement

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

Table 2
Experimental details

Crystal data
Chemical formula	(NH₄)₄[W₂(C₁₀H₁₂N₂O₈)O₆]·4H₂O
M_r	896.15
Crystal system, space group	Monoclinic, P2₁/c
Temperature (K)	150
a, b, c (Å)	6.8017 (5), 7.7194 (5), 23.9807 (19)
β (°)	95.345 (3)
V (Å³)	1253.63 (16)
Z	2
Radiation type	Mo Kα
μ (mm⁻¹)	9.26
Crystal size (mm)	0.18 × 0.18 × 0.14

Data collection
Diffractometer	Bruker APEXII CCD
Absorption correction	Multi-scan (SADABS; Bruker, 2016 )
T_min, T_max	0.444, 0.746
No. of measured, independent and observed [I > 2σ(I)] reflections	55419, 2890, 2703
R_int	0.053
(sin θ/λ)_max (Å⁻¹)	0.652

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.014, 0.034, 1.07
No. of reflections	2890
No. of parameters	201
H-atom treatment	H atoms treated by a mixture of independent and constrained refinement
Δρ_max, Δρ_min (e Å⁻³)	0.71, −0.85
Computer programs: APEX2 and SAINT (Bruker, 2016), SHELXS (Sheldrick, 2008 ), SHELXL2014/6 (Sheldrick, 2015 ) and OLEX2 (Dolomanov et al., 2009 ).

Structural data

CCDC reference: 2112632

Crystal structure: contains datablock I. DOI: https://doi.org/10.1107/S2414314621009822/im4013sup1.cif

Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314621009822/im4013Isup2.hkl

checkCIF report

Computing details top

Data collection: APEX2 (Bruker, 2016); cell refinement: SAINT (Bruker, 2016); data reduction: SAINT (Bruker, 2016); program(s) used to solve structure: SHELXS (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014/6 (Sheldrick, 2015); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: OLEX2 (Dolomanov et al., 2009).

Tetraammonium µ-ethylenediaminetetraacetato-1κ³O,N,O':2κ³O'',N',O'''-bis[trioxidotungstate(VI)] tetrahydrate top

Crystal data top

(NH₄)₄[W₂(C₁₀H₁₂N₂O₈)O₆]·4H₂O	F(000) = 860
M_r = 896.15	D_x = 2.374 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
a = 6.8017 (5) Å	Cell parameters from 9817 reflections
b = 7.7194 (5) Å	θ = 2.8–27.6°
c = 23.9807 (19) Å	µ = 9.26 mm⁻¹
β = 95.345 (3)°	T = 150 K
V = 1253.63 (16) Å³	Block, colourless
Z = 2	0.18 × 0.18 × 0.14 mm

Data collection top

Bruker APEXII CCD diffractometer	2703 reflections with I > 2σ(I)
φ and ω scans	R_int = 0.053
Absorption correction: multi-scan (SADABS; Bruker, 2016)	θ_max = 27.6°, θ_min = 2.8°
T_min = 0.444, T_max = 0.746	h = −8→8
55419 measured reflections	k = −10→10
2890 independent reflections	l = −31→31

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: mixed
R[F² > 2σ(F²)] = 0.014	H atoms treated by a mixture of independent and constrained refinement
wR(F²) = 0.034	w = 1/[σ²(F_o²) + (0.0138P)² + 1.4846P] where P = (F_o² + 2F_c²)/3
S = 1.07	(Δ/σ)_max = 0.002
2890 reflections	Δρ_max = 0.71 e Å⁻³
201 parameters	Δρ_min = −0.85 e Å⁻³
0 restraints

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. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms bonded to carbon and oxygen were placed in idealized positions and refined using a riding model with isotropic displacement parameters calculated as U_iso(H) = 1.2U_eq(C) for ethylene and methylene hydrogen atoms and U_iso(H) = 1.5U_eq(O) for solvent water molecules. Hydrogen atoms of the ammonium cations were located in the difference-Fourier map and refined isotropically.

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

	x	y	z	U_iso*/U_eq
W1	0.40177 (2)	0.69956 (2)	0.10889 (2)	0.01546 (4)
O6	0.4717 (3)	0.7513 (3)	0.04235 (8)	0.0290 (4)
O3	0.5793 (3)	0.7989 (2)	0.15614 (9)	0.0270 (4)
O9	0.2095 (3)	0.6721 (2)	0.17381 (8)	0.0237 (4)
N4	0.0791 (3)	0.6278 (2)	0.06743 (8)	0.0143 (4)
O8	0.4519 (3)	0.4764 (2)	0.11461 (8)	0.0276 (4)
O5	−0.0230 (3)	0.5116 (3)	0.20717 (8)	0.0351 (5)
C7	−0.0056 (4)	0.5133 (3)	0.10897 (10)	0.0192 (5)
H7A	0.0366	0.3924	0.1033	0.023*
H7B	−0.1515	0.5173	0.1031	0.023*
C11	0.0609 (4)	0.5690 (3)	0.16809 (11)	0.0200 (5)
C12	0.0980 (4)	0.5353 (3)	0.01373 (11)	0.0190 (5)
H12A	0.1915	0.4378	0.0208	0.023*
H12B	0.1546	0.6157	−0.0127	0.023*
O7	−0.0275 (3)	1.0904 (2)	0.07169 (9)	0.0280 (4)
O4	0.2366 (3)	0.9388 (2)	0.10315 (9)	0.0253 (4)
C1	0.0597 (4)	0.9519 (3)	0.07921 (11)	0.0183 (5)
C8	−0.0402 (4)	0.7886 (3)	0.05795 (12)	0.0219 (5)
H8A	−0.1639	0.7748	0.0762	0.026*
H8B	−0.0769	0.8012	0.0172	0.026*
N10	0.4415 (4)	0.8304 (3)	−0.06894 (11)	0.0225 (5)
O2	0.7912 (3)	1.0837 (3)	0.19478 (9)	0.0357 (5)
H2A	0.7148	0.9966	0.1847	0.054*
H2B	0.8584	1.0492	0.2254	0.054*
O1	0.2481 (3)	1.1729 (3)	0.19796 (10)	0.0367 (5)
H1A	0.2243	1.1196	0.1661	0.055*
H1B	0.1322	1.2036	0.2070	0.055*
N11	0.5898 (4)	0.3808 (4)	0.23069 (12)	0.0262 (5)
H10A	0.456 (5)	0.808 (4)	−0.0300 (16)	0.032 (9)*
H10B	0.521 (5)	0.904 (5)	−0.0757 (14)	0.034 (9)*
H10C	0.316 (6)	0.864 (5)	−0.0785 (16)	0.045 (10)*
H10D	0.471 (6)	0.735 (5)	−0.0853 (17)	0.046 (11)*
H11A	0.515 (6)	0.409 (6)	0.2004 (19)	0.060 (13)*
H11B	0.517 (7)	0.355 (6)	0.256 (2)	0.069 (14)*
H11C	0.662 (6)	0.466 (6)	0.2389 (17)	0.054 (12)*
H11D	0.663 (6)	0.288 (5)	0.2208 (17)	0.047 (11)*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
W1	0.01185 (5)	0.01695 (6)	0.01687 (6)	−0.00047 (3)	−0.00242 (4)	0.00027 (4)
O6	0.0201 (10)	0.0457 (11)	0.0211 (10)	−0.0102 (9)	0.0011 (8)	0.0012 (9)
O3	0.0216 (10)	0.0330 (11)	0.0253 (10)	−0.0030 (8)	−0.0044 (8)	−0.0031 (8)
O9	0.0244 (10)	0.0285 (10)	0.0182 (9)	−0.0082 (8)	0.0019 (8)	−0.0016 (7)
N4	0.0136 (9)	0.0125 (9)	0.0161 (10)	−0.0008 (7)	−0.0026 (8)	0.0005 (8)
O8	0.0255 (10)	0.0208 (9)	0.0344 (11)	0.0069 (8)	−0.0087 (8)	−0.0021 (8)
O5	0.0297 (11)	0.0522 (13)	0.0233 (10)	−0.0139 (10)	0.0015 (8)	0.0115 (10)
C7	0.0173 (12)	0.0174 (12)	0.0225 (13)	−0.0051 (9)	−0.0006 (10)	0.0026 (10)
C11	0.0174 (12)	0.0193 (12)	0.0227 (13)	0.0011 (9)	−0.0011 (10)	0.0044 (10)
C12	0.0165 (12)	0.0215 (12)	0.0186 (12)	−0.0022 (9)	−0.0010 (10)	−0.0051 (10)
O7	0.0256 (10)	0.0166 (9)	0.0411 (12)	0.0055 (8)	−0.0012 (8)	0.0011 (8)
O4	0.0190 (9)	0.0153 (9)	0.0396 (12)	−0.0016 (7)	−0.0083 (8)	−0.0005 (8)
C1	0.0169 (12)	0.0176 (12)	0.0202 (13)	0.0004 (9)	0.0013 (9)	0.0015 (9)
C8	0.0177 (12)	0.0142 (12)	0.0320 (15)	0.0019 (9)	−0.0070 (11)	0.0018 (10)
N10	0.0215 (12)	0.0178 (11)	0.0279 (14)	−0.0025 (9)	0.0010 (10)	0.0034 (10)
O2	0.0462 (13)	0.0282 (11)	0.0316 (12)	−0.0025 (10)	−0.0022 (10)	−0.0008 (9)
O1	0.0333 (12)	0.0386 (12)	0.0377 (13)	−0.0046 (10)	0.0013 (10)	−0.0024 (10)
N11	0.0272 (13)	0.0256 (13)	0.0254 (13)	−0.0032 (11)	0.0000 (11)	0.0033 (11)

Geometric parameters (Å, º) top

W1—O6	1.7529 (19)	O7—C1	1.228 (3)
W1—O3	1.7534 (19)	O4—C1	1.288 (3)
W1—O9	2.1350 (19)	C1—C8	1.499 (3)
W1—N4	2.3884 (19)	C8—H8A	0.9900
W1—O8	1.7590 (19)	C8—H8B	0.9900
W1—O4	2.1590 (17)	N10—H10A	0.95 (4)
O9—C11	1.284 (3)	N10—H10B	0.81 (4)
N4—C7	1.487 (3)	N10—H10C	0.90 (4)
N4—C12	1.488 (3)	N10—H10D	0.87 (4)
N4—C8	1.489 (3)	O2—H2A	0.8701
O5—C11	1.225 (3)	O2—H2B	0.8698
C7—H7A	0.9900	O1—H1A	0.8701
C7—H7B	0.9900	O1—H1B	0.8698
C7—C11	1.510 (4)	N11—H11A	0.87 (5)
C12—C12ⁱ	1.531 (5)	N11—H11B	0.84 (5)
C12—H12A	0.9900	N11—H11C	0.83 (4)
C12—H12B	0.9900	N11—H11D	0.92 (4)

O6—W1—O3	105.05 (9)	N4—C12—C12ⁱ	113.7 (3)
O6—W1—O9	157.36 (9)	N4—C12—H12A	108.8
O6—W1—N4	89.46 (8)	N4—C12—H12B	108.8
O6—W1—O8	103.12 (10)	C12ⁱ—C12—H12A	108.8
O6—W1—O4	86.03 (9)	C12ⁱ—C12—H12B	108.8
O3—W1—O9	90.22 (8)	H12A—C12—H12B	107.7
O3—W1—N4	157.08 (8)	C1—O4—W1	123.67 (15)
O3—W1—O8	105.14 (9)	O7—C1—O4	123.5 (2)
O3—W1—O4	89.42 (8)	O7—C1—C8	119.0 (2)
O9—W1—N4	71.28 (7)	O4—C1—C8	117.4 (2)
O9—W1—O4	77.36 (8)	N4—C8—C1	115.2 (2)
O8—W1—O9	88.46 (8)	N4—C8—H8A	108.5
O8—W1—N4	88.23 (8)	N4—C8—H8B	108.5
O8—W1—O4	159.79 (8)	C1—C8—H8A	108.5
O4—W1—N4	73.71 (7)	C1—C8—H8B	108.5
C11—O9—W1	120.89 (17)	H8A—C8—H8B	107.5
C7—N4—W1	104.91 (14)	H10A—N10—H10B	108 (3)
C7—N4—C12	111.36 (19)	H10A—N10—H10C	108 (3)
C7—N4—C8	110.97 (19)	H10A—N10—H10D	106 (3)
C12—N4—W1	108.76 (14)	H10B—N10—H10C	112 (3)
C12—N4—C8	110.94 (19)	H10B—N10—H10D	108 (4)
C8—N4—W1	109.70 (14)	H10C—N10—H10D	113 (4)
N4—C7—H7A	109.4	H2A—O2—H2B	104.5
N4—C7—H7B	109.4	H1A—O1—H1B	104.5
N4—C7—C11	111.03 (19)	H11A—N11—H11B	109 (4)
H7A—C7—H7B	108.0	H11A—N11—H11C	106 (4)
C11—C7—H7A	109.4	H11A—N11—H11D	106 (4)
C11—C7—H7B	109.4	H11B—N11—H11C	113 (4)
O9—C11—C7	116.1 (2)	H11B—N11—H11D	112 (4)
O5—C11—O9	124.1 (3)	H11C—N11—H11D	111 (4)
O5—C11—C7	119.7 (2)

W1—O9—C11—O5	159.8 (2)	C7—N4—C12—C12ⁱ	58.5 (3)
W1—O9—C11—C7	−18.0 (3)	C7—N4—C8—C1	111.6 (2)
W1—N4—C7—C11	35.7 (2)	C12—N4—C7—C11	153.2 (2)
W1—N4—C12—C12ⁱ	173.6 (2)	C12—N4—C8—C1	−124.0 (2)
W1—N4—C8—C1	−3.8 (3)	O7—C1—C8—N4	178.2 (2)
W1—O4—C1—O7	−173.4 (2)	O4—C1—C8—N4	0.2 (4)
W1—O4—C1—C8	4.4 (3)	C8—N4—C7—C11	−82.7 (2)
N4—C7—C11—O9	−16.0 (3)	C8—N4—C12—C12ⁱ	−65.6 (3)
N4—C7—C11—O5	166.0 (2)

Symmetry code: (i) −x, −y+1, −z.

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
C7—H7A···O7ⁱⁱ	0.99	2.48	3.384 (3)	152
C12—H12B···O7ⁱⁱⁱ	0.99	2.77	3.548 (3)	136
C8—H8A···O6^iv	0.99	2.54	3.319 (3)	135
C8—H8B···O7ⁱⁱⁱ	0.99	2.46	3.319 (4)	145
O2—H2A···O3	0.87	1.88	2.743 (3)	171
O2—H2B···O5^v	0.87	1.90	2.763 (3)	170
O1—H1A···O7	0.87	2.72	3.468 (3)	145
O1—H1A···O4	0.87	2.06	2.900 (3)	161
O1—H1B···O2^iv	0.87	2.49	3.177 (3)	137
N10—H10A···O6	0.95 (4)	1.78 (4)	2.727 (3)	175 (3)
N10—H10B···O4^vi	0.81 (4)	2.20 (4)	2.996 (3)	168 (3)
N10—H10C···O7ⁱⁱⁱ	0.90 (4)	2.01 (4)	2.876 (3)	160 (3)
N10—H10D···O8^vii	0.87 (4)	1.87 (4)	2.736 (3)	175 (4)
N11—H11A···O8	0.87 (5)	2.13 (5)	2.947 (3)	156 (4)
N11—H11B···O3^viii	0.84 (5)	2.31 (5)	3.109 (3)	160 (4)
N11—H11C···O1^viii	0.83 (4)	2.25 (4)	2.979 (4)	147 (4)
N11—H11D···O2ⁱⁱ	0.92 (4)	1.93 (4)	2.846 (4)	173 (4)

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

Acknowledgements

The authors acknowledge the Cheikh Anta Diop University of Dakar (Senegal), the Institute of Inorganic Chemistry I, Ulm University and the Helmholtz Institute Ulm (HIU) for Electrochemical Energy Storage, Albert-Einstein-Allee 11, 89081 Ulm, Germany, for financial support and instrumentation use.

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