Crystal structure of [Y₆(μ₆-O)(μ₃-OH)₈(H₂O)₂₄]I₈·8H₂O

The crystal structure of the title compound {systematic name: octa-μ₃-hydroxido-μ₆-oxido-hexa­kis­[tetra­aqua­yttrium(III)] octa­iodide octa­hydrate}, is characterized by the presence of the centrosymmetric mol­ecular entity [Y₆(μ₆-O)(μ₃-OH)₈(H₂O)₂₄]⁸⁺, in which the six Y³⁺ cations are arranged octa­hedrally around a μ₆-O atom at the centre of the cationic complex. Each of the eight faces of the Y₆ octa­hedron is capped by an μ₃-OH group in the form of a distorted cube. In the hexa­nuclear entity, the Y³⁺ cations are coordinated by the central μ₆-O atom, the O atoms of four μ₃-OH and of four water mol­ecules. The resulting coordination sphere of the metal ions is a capped square-anti­prism. The crystal packing is quite similar to that of the ortho­rhom­bic [Ln₆(μ₆-O)(μ₃-OH)₈(H₂O)₂₄]I₈·8H₂O structures with Ln = La—Nd, Eu—Tb, Dy, except that the title compound exhibits a slight monoclinic distortion. The proximity of the cationic complexes and the lattice water mol­ecules leads to the formation of a three-dimensional hydrogen-bonded network of medium strength.

1. Chemical context

Rare-earth-based oxido-hydroxido polynuclear complexes are of inter­est because of their unique luminescence (Chen et al., 2010; Le Natur et al., 2013; Petit et al., 2009), magnetic properties (Abbas et al., 2010; Xu et al., 2011) or structural characteristics (Zheng, 2001; Andrews et al., 2013). Actually, in this kind of complex, the spatial proximity between metal ions affords cooperative/synergetic effects or energy-transfer mechanisms workable in terms of optical properties. For more than a decade, our group has been involved in the synthesis and the characterization of such rare-earth-based hexa­nuclear complexes (Calvez et al., 2010). The hexa­nuclear complexes crystallize in different structures depending on the counter-anion (e.g. nitrate, perchlorate, iodide: Zak et al., 1994; Wang et al., 2000; Mudring et al., 2006), the number of lattice water mol­ecules and/or the radius of the involved lanthanide ion. Since the pioneering work of Zak et al. (1994), we have developed a systematic synthetic procedure for the nitrate counter-anion complex with most of the rare earth elements (Calvez et al., 2008, 2010). In this context, we have undertaken the study of a series of complexes based on the iodide counter-anion which have never been obtained with heavier rare earth ions. We report here the synthesis and crystal structure of the yttrium derivative.

2. Structural commentary

In contrast to the ortho­rhom­bic [Ln₆(μ₆-O)(μ₃-OH)₈(H₂O)₂₄]I₈·8H₂O structures with Ln = La—Nd, Eu—Tb, Dy (Mudring & Babai, 2005; Mudring et al., 2006; Rukk et al., 2009), the crystal structure of the yttrium member of this series has monoclinic symmetry, with the monoclinic angle close to 90° (Table 2). The asymmetric unit of [Y₆(μ₆-O)(μ₃-OH)₈(H₂O)₂₄]I₈·8H₂O contains half of the formula unit because the complete complex is situated on a centre of inversion. Three independent yttrium cations (Y1, Y2 and Y3), four oxygen atoms from μ₃-hydroxyl groups (O1, O2, O3, O4), twelve oxygen atoms of terminal aqua ligands coordin­ating to each yttrium cation (Y1: O5, O6, O7, O8; Y2: O9, O10, O11, O12; Y3: O13, O14, O15 O16), one μ₆-bridging O atom (O) lying on an inversion centre, four iodide anions (I1, I2, I3, I4) and four oxygen atoms of lattice water mol­ecules (OW1, OW2, OW3, OW4) are present in the crystal structure (Fig. 1). Calculations with the SHAPE software suite (Alvarez et al., 2005) indicate that each of the coordination polyhedra surrounding the Y³⁺ ions is best described as a spherical capped square-anti­prism (Ruiz-Martínez et al., 2010) with idealized C_4v symmetry. However, the true symmetry of this structural fragment in the title structure is C₁.

Table 2
Experimental details

Crystal data
Chemical formula	[Y6O(OH)8(H2O)24]I8·8H2O
Mr	2277.24
Crystal system, space group	Monoclinic, P21/n
Temperature (K)	293
a, b, c (Å)	12.9099 (2), 14.8050 (2), 14.7933 (3)
β (°)	90.821 (1)
V (Å^3)	2827.17 (8)
Z	2
Radiation type	Mo Kα
μ (mm^−1)	10.54
Crystal size (mm)	0.18 × 0.14 × 0.1
Data collection
Diffractometer	Nonius KappaCCD
Absorption correction	Gaussian (Coppens et al., 1965)
Tmin, Tmax	0.018, 0.091
No. of measured, independent and observed [I > 2σ(I)] reflections	35352, 6374, 5449
Rint	0.124
(sin θ/λ)max (Å^−1)	0.647
Refinement
R[F^2 > 2σ(F^2)], wR(F^2), S	0.067, 0.178, 1.11
No. of reflections	6374
No. of parameters	251
	w = 1/[σ^2(Fo^2) + (0.0487P)^2 + 43.8859P] where P = (Fo^2 + 2Fc^2)/3
Δρmax, Δρmin (e Å^−3)	2.62, −1.83
Computer programs: COLLECT (Nonius, 1998), EVALCCD (Duisenberg et al., 2003), SHELXS97 and SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 2006) and publCIF (Westrip, 2010).

Figure 1 The asymmetric unit of the title complex. Displacement ellipsoids are drawn at the 50% probability level.

Since the μ₆-O atom is located on an inversion centre and binds to six Y³⁺ cations, a slightly distorted anion-centred [OY₆] octa­hedron results (Fig. 2). The average of the Y⋯Y distances between adjacent cations in the octa­hedron is found to be 3.536 Å. The mean Y—(μ₆-O) distance is 2.537 Å, while the averaged Y—(μ₃-OH) is 2.34 Å. The hydroxide ions are situated above the eight faces of the OY₆ octa­hedron and form a distorted cube around the octa­hedron (Fig. 2).

Figure 2 The OY6 octa­hedron in the complex [Y6(μ6-O)(μ3-OH)8(H2O)24]^8+ cation. Y atoms are green and O atoms are red.

3. Supra­molecular features

The hexa­nuclear [Y₆(μ₆-O)(μ₃-OH)₈(H₂O)₂₄]⁸⁺ units are arranged in a body-centred fashion in the crystal structure. Each of these units is surrounded by twelve iodide anions, connecting the units to each other through Coulombic inter­actions. Although the hydrogen atoms of the water mol­ecules and hydroxide groups could not be located, the range of O⋯O distances between the cationic complex and the lattice water mol­ecules suggest the formation of medium-strength hydrogen bonds (Table 1). These inter­actions lead to the formation of a three-dimensional network in the structure (Fig. 3).

Table 1
Hydrogen-bond geometry (Å)

D⋯A	D⋯A
O7⋯OW2	2.646 (4)
O10⋯OW3	2.764 (1)
O13⋯OW4	2.803 (8)
O15⋯OW1	2.767 (2)
O16⋯OW4	2.836 (2)
O16⋯OW1	2.851 (6)

Figure 3 The crystal structure of [Y6(μ6-O)(μ3-OH)8(H2O)24]I8·8H2O in projections along [100], [010] and [001], respectively, from left to right. Y atoms are green, O atoms are red and I atoms are yellow.

4. Synthesis and crystallization

Yttrium oxide Y₂O₃ (2 g, Strem Chemicals 4M) was dissolved in fresh hydro­iodic acid (9 ml, 57wt%, unstabilized from Acros Organics) under gentle heating (323 K). If the acid used is not fresh, it should be distilled twice. The clear solution was exposed to air under isothermal conditions (6 weeks). At this stage, the pH of the solution remains acidic. Large pale-yellow polyhedral crystals were separated manually from the solution and were mounted into a glass capillary.

5. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2. The hydrogen atoms from the water mol­ecules or hydroxide could not be assigned reliably and thus were not included in the refinement. However, they were taken into account for the chemical formula sum, moiety, weight, as well as for the absorption coefficient and the number of electrons in the unit cell.

Supporting information

S1. Chemical context

Rare-earth-based oxido-hydroxido polynuclear complexes are of inter­est because of their unique luminescence (Chen et al., 2010; Le Natur et al., 2013; Petit et al., 2009), magnetic properties (Abbas et al., 2010; Xu et al., 2011) or structural characteristics (Zheng, 2001; Andrews et al., 2013). Actually, in this kind of complex, the spatial proximity between metal ions affords cooperative/synergetic effects or energy-transfer mechanisms workable in terms of optical properties. For more than a decade, our group has been involved in the synthesis and the characterization of such rare-earth-based hexanuclear complexes (Calvez et al., 2010). The hexanuclear complexes crystallize in different structures depending on the counter-anion (e.g. nitrate, perchlorate, iodide: Zak et al., 1994; Wang et al., 2000; Mudring et al., 2006), the number of lattice water molecules and/or the radius of the involved lanthanide ion. Since the pioneering work of Zak et al. (1994), we have developed a systematic synthetic procedure for the nitrate counter-anion complex with most of the rare earth elements (Calvez et al., 2008, 2010). In this context, we have undertaken the study of a series of complexes based on the iodide counter-anion which have never been obtained with heavier rare earth ions. We report here the synthesis and crystal structure of the yttrium derivative.

S2. Structural commentary

In contrast to the orthorhombic [Ln₆(µ₆-O)(µ₃-OH)₈(H₂O)₂₄]I₈·8H₂O structures with Ln = La—Nd, Eu—Tb, Dy (Mudring & Babai, 2005; Mudring et al., 2006; Rukk et al., 2009), the crystal structure of the yttrium member of this series has monoclinic symmetry, with the monoclinic angle close to 90°. The asymmetric unit of [Y₆(µ₆-O)(µ₃-OH)₈(H₂O)₂₄]I₈·8H₂O contains half of the formula unit because the complete complex is situated on a centre of inversion. Three independent yttrium cations (Y1, Y2 and Y3), four oxygen atoms from µ₃-hydroxyl groups (O1, O2, O3, O4), twelve oxygen atoms of terminal aqua ligands coordinating to each yttrium cation (Y1: O5, O6, O7, O8; Y2: O9, O10, O11, O12; Y3: O13, O14, O15 O16), one µ₆-bridging O atom (O) lying on an inversion centre, four iodide anions (I1, I2, I3, I4) and four oxygen atoms of lattice water molecules (OW1, OW2, OW3, OW4) are present in the crystal structure (Fig. 1). Calculations with the SHAPE software suite (Alvarez et al., 2005) indicate that each of the coordination polyhedra surrounding the Y³⁺ ions is best described as a spherical capped square-anti­prism (Ruiz-Martínez et al., 2010) with idealized C_4v symmetry. However, the true symmetry of this structural fragment in the title structure is C₁.

Since the µ₆-O atom is located on an inversion centre and binds to six Y³⁺ cations, a slightly distorted anion-centred [OY₆] o­cta­hedron results (Fig. 2). The average of the Y···Y distances between adjacent cations in the o­cta­hedron is found to be 3.536 Å. The mean Y—(µ₆-O) distance is 2.537 Å, while the averaged Y—(µ₃-OH) is 2.34 Å. The hydroxide ions are situated above the eight faces of the OY₆ o­cta­hedron and form a distorted cube around the o­cta­hedron (Fig. 2).

S3. Supra­molecular features

The hexanuclear [Y₆(µ₆-O)(µ₃-OH)₈(H₂O)₂₄]⁸⁺ units are arranged in a body-centred fashion in the crystal structure. Each of these units is surrounded by twelve iodide anions, connecting the units to each other through Coulombic inter­actions. Although the hydrogen atoms of the water molecules and hydroxide groups could not be located, the range of O···O distances between the cationic complex and the lattice water molecules suggest the formation of medium-strength hydrogen bonds (Table 1). These inter­actions lead to the formation of a three-dimensional network in the structure (Fig. 3).

S4. Synthesis and crystallization

Yttrium oxide Y₂O₃ (2 g, Strem Chemicals 4M) was dissolved in fresh hydro­iodic acid (9 ml, 57wt%, unstabilized from Acros Organics) under gentle heating (323 K). If the acid used is not fresh, it should be distilled twice. The clear solution was exposed to air under isothermal conditions (6 weeks). At this stage, the pH of the solution remains acidic. Large pale-yellow polyhedral crystals were separated manually from the solution and were mounted into a glass capillary.

S5. Refinement

Crystal data, data collection and structure refinement details are summarized in Table 2. The hydrogen atoms from the water molecules or hydroxide could not be assigned reliably and thus were not included in the refinement. However, they were taken into account for the chemical formula sum, moiety, weight, as well as for the absorption coefficient and the number of electrons in the unit cell.

Related literature

For related literature, see: Abbas et al. (2010); Alvarez et al. (2005); Andrews et al. (2013); Calvez et al. (2008, 2010); Chen et al. (2010); Le Natur, Calvez, Daiguebonne, Guillou, Bernot, Ledoux, Le Pollès & Roiland (2013); Mudring & Babai (2005); Mudring et al. (2006); Petit et al. (2009); Ruiz-Martínez, Casanova & Alvarez (2010); Rukk et al. (2009); Wang et al. (2000); Xu et al. (2011); Zak et al. (1994); Zheng (2001).

Computing details

Data collection: COLLECT (Nonius, 1998); cell refinement: COLLECT (Nonius, 1998); data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 2006); software used to prepare material for publication: publCIF (Westrip, 2010).

Figures

The asymmetric unit of the title complex. Displacement ellipsoids are drawn at the 50% probability level.

The OY₆ octahedron in the complex [Y₆(µ₆-O)(µ₃-OH)₈(H₂O)₂₄]⁸⁺ cation. Y atoms are green and O atoms are red.

The crystal structure of [Y₆(µ₆-O)(µ₃-OH)₈(H₂O)₂₄]I₈·8H₂O in projections along [100], [010] and [001], respectively, from left to right. Y atoms are green, O atoms are red and I atoms are yellow.

Octa-µ₃-hydroxido-µ₆-oxido-hexakis[tetraaquayttrium(III)] octaiodide octahydrate

Crystal data

[Y6O(OH)8(H2O)24]I8·8H2O	F(000) = 2116
Mr = 2277.24	Dx = 2.675 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 62388 reflections
a = 12.9099 (2) Å	θ = 2.9–27.5°
b = 14.8050 (2) Å	µ = 10.54 mm^−1
c = 14.7933 (3) Å	T = 293 K
β = 90.821 (1)°	Block, colorless
V = 2827.17 (8) Å^3	0.18 × 0.14 × 0.1 mm
Z = 2

Data collection

Nonius KappaCCD diffractometer	6374 independent reflections
Radiation source: fine-focus sealed tube	5449 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.124
CCD rotation images, thick slices scans	θmax = 27.4°, θmin = 3.1°
Absorption correction: gaussian (Coppens et al., 1965)	h = −16→16
Tmin = 0.018, Tmax = 0.091	k = −19→18
35352 measured reflections	l = −19→19

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.067	w = 1/[σ^2(Fo^2) + (0.0487P)^2 + 43.8859P] where P = (Fo^2 + 2Fc^2)/3
wR(F^2) = 0.178	(Δ/σ)max = 0.001
S = 1.11	Δρmax = 2.62 e Å^−3
6374 reflections	Δρmin = −1.83 e Å^−3
251 parameters	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
0 restraints	Extinction coefficient: 0.00258 (19)

Special details

Experimental. 6336 sampling points

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

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Y1	0.50083 (7)	1.00150 (6)	1.16560 (6)	0.0335 (2)
Y2	0.46090 (7)	1.16586 (6)	0.99794 (6)	0.0317 (2)
Y3	0.30677 (7)	0.96613 (6)	0.99944 (6)	0.0323 (2)
I1	0.49148 (9)	0.82346 (8)	0.49868 (6)	0.0707 (3)
I2	0.28137 (7)	0.72379 (7)	0.24171 (7)	0.0650 (3)
I3	0.48625 (14)	0.50289 (7)	0.14980 (8)	0.0932 (4)
I4	0.78359 (8)	0.78678 (8)	0.26729 (8)	0.0792 (4)
O	0.5000	1.0000	1.0000	0.0293 (17)
O1	0.3633 (5)	1.0806 (4)	1.0999 (4)	0.0328 (13)
O2	0.4097 (5)	0.8826 (4)	1.1002 (4)	0.0313 (13)
O3	0.3622 (5)	1.0773 (4)	0.8978 (4)	0.0321 (13)
O4	0.4081 (5)	0.8803 (4)	0.9008 (4)	0.0335 (13)
O5	0.6563 (13)	1.0251 (17)	1.2721 (11)	0.150 (8)
O6	0.5306 (14)	0.8859 (13)	1.2758 (10)	0.136 (7)
O7	0.3511 (12)	0.9672 (11)	1.2711 (9)	0.106 (5)
O8	0.4775 (9)	1.1210 (7)	1.2708 (6)	0.069 (3)
O9	0.4402 (8)	1.2676 (6)	1.1305 (7)	0.064 (2)
O10	0.2918 (7)	1.2392 (6)	0.9958 (7)	0.065 (2)
O11	0.4402 (7)	1.2644 (6)	0.8649 (7)	0.060 (2)
O12	0.5819 (8)	1.2981 (6)	0.9988 (7)	0.066 (2)
O13	0.1968 (6)	0.9524 (7)	1.1339 (6)	0.058 (2)
O14	0.2216 (8)	0.8163 (7)	1.0027 (8)	0.075 (3)
O15	0.1950 (6)	0.9452 (7)	0.8664 (6)	0.059 (2)
O16	0.1578 (7)	1.0700 (7)	0.9987 (7)	0.063 (2)
OW1	−0.0079 (7)	0.8851 (8)	0.8689 (7)	0.070 (3)
OW2	0.2083 (19)	0.5431 (17)	0.0762 (13)	0.164 (8)
OW3	0.7261 (18)	0.5806 (14)	0.051 (2)	0.216 (13)
OW4	0.9948 (7)	0.8828 (8)	0.1328 (7)	0.069 (3)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Y1	0.0380 (5)	0.0307 (5)	0.0318 (4)	0.0014 (3)	−0.0006 (3)	0.0000 (3)
Y2	0.0313 (4)	0.0271 (4)	0.0367 (5)	−0.0001 (3)	−0.0010 (3)	0.0003 (3)
Y3	0.0297 (4)	0.0292 (4)	0.0381 (5)	−0.0001 (3)	−0.0011 (3)	0.0003 (3)
I1	0.0799 (7)	0.0740 (7)	0.0580 (5)	0.0010 (5)	−0.0028 (4)	−0.0014 (4)
I2	0.0624 (5)	0.0599 (5)	0.0731 (6)	−0.0069 (4)	0.0146 (4)	0.0202 (4)
I3	0.1624 (13)	0.0473 (5)	0.0701 (7)	−0.0080 (6)	0.0074 (7)	0.0003 (4)
I4	0.0647 (6)	0.0771 (7)	0.0950 (8)	0.0062 (5)	−0.0237 (5)	0.0377 (6)
O	0.035 (4)	0.021 (4)	0.032 (4)	0.001 (3)	−0.002 (3)	0.002 (3)
O1	0.032 (3)	0.028 (3)	0.039 (3)	−0.001 (2)	0.001 (3)	−0.003 (3)
O2	0.029 (3)	0.023 (3)	0.042 (3)	0.001 (2)	0.000 (3)	0.005 (3)
O3	0.029 (3)	0.033 (3)	0.034 (3)	−0.002 (2)	−0.003 (2)	0.003 (3)
O4	0.029 (3)	0.033 (3)	0.038 (3)	0.000 (2)	−0.006 (3)	0.000 (3)
O5	0.099 (11)	0.26 (3)	0.090 (11)	0.009 (13)	−0.001 (9)	−0.023 (13)
O6	0.157 (15)	0.171 (17)	0.080 (9)	0.027 (12)	0.002 (9)	0.065 (10)
O7	0.127 (11)	0.120 (11)	0.070 (7)	−0.043 (9)	0.026 (7)	−0.005 (7)
O8	0.101 (8)	0.057 (6)	0.050 (5)	0.002 (5)	0.000 (5)	−0.018 (4)
O9	0.064 (6)	0.051 (5)	0.078 (6)	−0.003 (4)	0.004 (5)	−0.020 (5)
O10	0.054 (5)	0.052 (5)	0.089 (7)	0.018 (4)	−0.004 (5)	0.006 (5)
O11	0.058 (5)	0.047 (5)	0.075 (6)	0.001 (4)	−0.006 (4)	0.020 (4)
O12	0.067 (6)	0.048 (5)	0.082 (7)	−0.007 (4)	−0.004 (5)	0.007 (5)
O13	0.041 (4)	0.073 (6)	0.061 (5)	0.000 (4)	0.005 (4)	0.010 (4)
O14	0.062 (6)	0.065 (6)	0.098 (8)	−0.027 (5)	−0.003 (5)	0.002 (6)
O15	0.045 (4)	0.075 (6)	0.058 (5)	−0.004 (4)	−0.018 (4)	−0.005 (4)
O16	0.041 (4)	0.079 (6)	0.071 (6)	0.023 (4)	0.002 (4)	−0.006 (5)
OW1	0.051 (5)	0.086 (7)	0.072 (6)	−0.006 (5)	−0.004 (4)	−0.009 (5)
OW2	0.19 (2)	0.19 (2)	0.114 (14)	0.012 (17)	0.028 (13)	−0.005 (14)
OW3	0.158 (19)	0.091 (13)	0.40 (4)	0.027 (13)	0.09 (2)	0.004 (19)
OW4	0.052 (5)	0.086 (7)	0.068 (6)	−0.010 (5)	−0.006 (4)	0.010 (5)

Geometric parameters (Å, º)

Y1—O2	2.321 (6)	Y2—O11	2.462 (9)
Y1—O3^i	2.326 (6)	Y2—O9	2.490 (9)
Y1—O1	2.328 (7)	Y2—O12	2.506 (9)
Y1—O4^i	2.332 (7)	Y2—O	2.5070 (9)
Y1—O8	2.378 (9)	Y3—O2	2.336 (6)
Y1—O6	2.390 (14)	Y3—O3	2.347 (6)
Y1—O	2.4497 (9)	Y3—O4	2.348 (7)
Y1—O7	2.553 (13)	Y3—O1	2.362 (6)
Y1—O5	2.557 (18)	Y3—O15	2.443 (8)
Y2—O2^i	2.341 (6)	Y3—O16	2.462 (8)
Y2—O3	2.341 (6)	Y3—O13	2.469 (8)
Y2—O4^i	2.344 (6)	Y3—O14	2.477 (10)
Y2—O1	2.347 (6)	Y3—O	2.5444 (9)
Y2—O10	2.438 (9)
O2—Y1—O3^i	80.5 (2)	O10—Y2—O	128.0 (2)
O2—Y1—O1	80.1 (2)	O11—Y2—O	127.6 (2)
O3^i—Y1—O1	131.5 (2)	O9—Y2—O	127.3 (3)
O2—Y1—O4^i	130.4 (2)	O12—Y2—O	129.8 (2)
O3^i—Y1—O4^i	79.4 (2)	O2—Y3—O3	127.1 (2)
O1—Y1—O4^i	80.4 (2)	O2—Y3—O4	78.1 (2)
O2—Y1—O8	140.2 (3)	O3—Y3—O4	78.7 (2)
O3^i—Y1—O8	137.8 (3)	O2—Y3—O1	79.1 (2)
O1—Y1—O8	78.2 (3)	O3—Y3—O1	78.8 (2)
O4^i—Y1—O8	77.7 (3)	O4—Y3—O1	127.5 (2)
O2—Y1—O6	79.4 (5)	O2—Y3—O15	140.4 (3)
O3^i—Y1—O6	78.5 (5)	O3—Y3—O15	75.8 (3)
O1—Y1—O6	139.4 (5)	O4—Y3—O15	76.0 (3)
O4^i—Y1—O6	138.4 (5)	O1—Y3—O15	140.5 (3)
O8—Y1—O6	96.2 (6)	O2—Y3—O16	140.4 (3)
O2—Y1—O	65.23 (16)	O3—Y3—O16	78.7 (3)
O3^i—Y1—O	65.46 (16)	O4—Y3—O16	141.0 (3)
O1—Y1—O	66.07 (16)	O1—Y3—O16	77.8 (3)
O4^i—Y1—O	65.21 (16)	O15—Y3—O16	67.9 (3)
O8—Y1—O	131.5 (3)	O2—Y3—O13	76.8 (3)
O6—Y1—O	132.4 (5)	O3—Y3—O13	139.3 (3)
O2—Y1—O7	73.7 (4)	O4—Y3—O13	142.0 (3)
O3^i—Y1—O7	137.2 (4)	O1—Y3—O13	74.2 (3)
O1—Y1—O7	77.0 (4)	O15—Y3—O13	107.4 (3)
O4^i—Y1—O7	142.9 (4)	O16—Y3—O13	66.2 (3)
O8—Y1—O7	69.2 (4)	O2—Y3—O14	76.3 (3)
O6—Y1—O7	63.7 (6)	O3—Y3—O14	141.2 (3)
O—Y1—O7	128.1 (3)	O4—Y3—O14	77.2 (3)
O2—Y1—O5	138.5 (6)	O1—Y3—O14	139.8 (3)
O3^i—Y1—O5	73.9 (4)	O15—Y3—O14	69.2 (4)
O1—Y1—O5	140.9 (6)	O16—Y3—O14	102.3 (4)
O4^i—Y1—O5	76.2 (5)	O13—Y3—O14	69.5 (4)
O8—Y1—O5	66.5 (5)	O2—Y3—O	63.48 (15)
O6—Y1—O5	64.0 (7)	O3—Y3—O	63.63 (15)
O—Y1—O5	127.5 (4)	O4—Y3—O	63.47 (15)
O7—Y1—O5	104.2 (5)	O1—Y3—O	64.06 (15)
O2^i—Y2—O3	79.8 (2)	O15—Y3—O	126.5 (2)
O2^i—Y2—O4^i	78.0 (2)	O16—Y3—O	130.0 (3)
O3—Y2—O4^i	128.4 (2)	O13—Y3—O	126.1 (2)
O2^i—Y2—O1	128.9 (2)	O14—Y3—O	127.7 (3)
O3—Y2—O1	79.2 (2)	Y1^i—O—Y1	180.0
O4^i—Y2—O1	79.7 (2)	Y1^i—O—Y2^i	90.07 (3)
O2^i—Y2—O10	140.8 (3)	Y1—O—Y2^i	89.93 (3)
O3—Y2—O10	76.2 (3)	Y1^i—O—Y2	89.93 (3)
O4^i—Y2—O10	140.9 (3)	Y1—O—Y2	90.07 (3)
O1—Y2—O10	76.1 (3)	Y2^i—O—Y2	180.0
O2^i—Y2—O11	75.9 (3)	Y1^i—O—Y3^i	89.73 (3)
O3—Y2—O11	77.0 (3)	Y1—O—Y3^i	90.27 (3)
O4^i—Y2—O11	138.8 (3)	Y2^i—O—Y3^i	89.76 (3)
O1—Y2—O11	141.2 (3)	Y2—O—Y3^i	90.24 (3)
O10—Y2—O11	68.8 (3)	Y1^i—O—Y3	90.27 (3)
O2^i—Y2—O9	139.4 (3)	Y1—O—Y3	89.73 (3)
O3—Y2—O9	140.6 (3)	Y2^i—O—Y3	90.24 (3)
O4^i—Y2—O9	76.0 (3)	Y2—O—Y3	89.76 (3)
O1—Y2—O9	75.8 (3)	Y3^i—O—Y3	180.0
O10—Y2—O9	68.6 (3)	Y1—O1—Y2	97.2 (2)
O11—Y2—O9	105.1 (4)	Y1—O1—Y3	97.4 (2)
O2^i—Y2—O12	78.0 (3)	Y2—O1—Y3	98.4 (2)
O3—Y2—O12	140.8 (3)	Y1—O2—Y3	98.3 (2)
O4^i—Y2—O12	77.3 (3)	Y1—O2—Y2^i	97.4 (2)
O1—Y2—O12	139.3 (3)	Y3—O2—Y2^i	99.9 (2)
O10—Y2—O12	102.2 (3)	Y1^i—O3—Y2	97.3 (2)
O11—Y2—O12	66.5 (3)	Y1^i—O3—Y3	98.5 (2)
O9—Y2—O12	66.3 (3)	Y2—O3—Y3	99.0 (2)
O2^i—Y2—O	64.02 (15)	Y1^i—O4—Y2^i	97.2 (2)
O3—Y2—O	64.31 (16)	Y1^i—O4—Y3	98.3 (2)
O4^i—Y2—O	64.12 (16)	Y2^i—O4—Y3	99.4 (2)
O1—Y2—O	64.86 (16)

Symmetry code: (i) −x+1, −y+2, −z+2.

Hydrogen-bond geometry (Å)

D—H···A	D···A
O7···OW2	2.646 (4)
O10···OW3	2.764 (1)
O13···OW4	2.803 (8)
O15···OW1	2.767 (2)
O16···OW4	2.836 (2)
O16···OW1	2.851 (6)