Poly[[aqua­tri-μ3-hydroxido-(μ4-2-phos­phon­ato­ethane­sulfonato)­dierbium(III)] monohydrate]

Sonnauer, A.; Stock, N.

doi:10.1107/S1600536808033230

metal-organic compounds

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ISSN: 2056-9890

Volume 64| Part 11| November 2008| Page m1433

doi:10.1107/S1600536808033230

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Poly[[aquatri-μ₃-hydroxido-(μ₄-2-phosphonatoethanesulfonato)dierbium(III)] monohydrate]

Andreas Sonnauer ^a and Norbert Stock ^a ^*

^aInstitute of Inorganic Chemistry, Christian-Albrechts-University, Max-Eyth-Strasse 2, D 24118 Kiel, Germany
^*Correspondence e-mail: stock@ac.uni-kiel.de

(Received 29 September 2008; accepted 13 October 2008; online 18 October 2008)

The crystal structure of the title compound, {[Er₂(C₂H₄O₆PS)(OH)₃(H₂O)]·H₂O}_n, consists of two Er³⁺ ions, one (C₂H₄O₆PS)³⁻ ion, three OH⁻ ions, and two water molecule. The Er³⁺ ions form ErO₈ polyhedra., which are connected by μ- and μ₃-O atoms. Thus, inorganic Er–O–Er layers of edge- and face-sharing polyhedra are observed. Whereas most often in metal phosphonosulfonates the organic linker bridges adjacent layers, in the title compound, the (O₃PC₂H₄SO₃)³⁻ anion is only connected to one Er–O–Er layer. Short interatomic O⋯O distances [2.898 (8), 2.997 (14) and 2.768 (10) Å] indicate hydrogen bonding between the layers. The noncoordinated water molecules are located between the layers.

Related literature

For related structures, see: Sonnauer et al. (2007 ); Sonnauer & Stock (2008a ,b ); Benedetto et al. (1997 ); Adani et al. (1998 ); Du et al. (2006a ,b ); Du, Li et al. (2007 ); Du, Prosvirin & Mao (2007 ); Du, Xu et al. (2007 ).

Experimental

Crystal data

[Er₂(C₂H₄O₆PS)(OH)₃(H₂O)]·H₂O
M_r = 608.65
Triclinic, $[P \overline 1]$
a = 5.8621 (6) Å
b = 9.0443 (9) Å
c = 11.6240 (11) Å
α = 105.543 (12)°
β = 101.713 (11)°
γ = 101.885 (11)°
V = 558.81 (10) Å³
Z = 2
Mo Kα radiation
μ = 15.29 mm⁻¹
T = 293 (2) K
0.08 × 0.07 × 0.06 mm

Data collection

Stoe IPDS-1 diffractometer
Absorption correction: ψ scan (X-RED and X-SHAPE; Stoe & Cie, 1999 ) T_min = 0.293, T_max = 0.399
4731 measured reflections
2664 independent reflections
2207 reflections with I > 2σ(I)
R_int = 0.041

Refinement

R[F² > 2σ(F²)] = 0.031
wR(F²) = 0.082
S = 0.97
2664 reflections
155 parameters
H-atom parameters constrained
Δρ_max = 1.61 e Å⁻³
Δρ_min = −2.07 e Å⁻³

Data collection: IPDS Program Package (Stoe & Cie, 1998 ); cell refinement: IPDS Program Package; data reduction: IPDS Program Package; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 1999 ); software used to prepare material for publication: publCIF (Westrip, 2008 ).

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536808033230/bt2804sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536808033230/bt2804Isup2.hkl

checkCIF report

Comment top

Inorganic–organic hybrid materials based on metal carboxylates, sulfonates and phosphonates are intensively investigated due to their potential application i.e. in the field of gas separation, storage, as well as catalysis, or as sensor materials. We are interested in the use of organic ligands containing two or more different functional groups for the synthesis of functionalized hybrid compounds. Although a large number of metal phosphonates and metal sulfonates have been reported in the literature, compounds based on ligands containing simultaneously a phosphonic as well as a sulfonic acid group have only recently been investigated. These few studies are limited to the use of linker molecules based on rigid phosphonoarylsulfonic acids (Benedetto et al., 1997; Adani et al., 1998; Du et al., 2006a,b; Du, Li et al., 2007; Du, Prosvirin & Mao, 2007; Du, Xu et al., 2007). Our group has started a systematic investigation using the flexible linker 2-phosphonoethansulfonic acid, which has been recently reported in the literature (Sonnauer et al., 2007; Sonnauer & Stock, 2008a,b). Here we describe the crystal structure of the new rare earth phosphonatosulfonate [Er₂(O₃PC₂H₄SO₃)(OH)₃(H₂O)]H₂O, which was obtained during a high-throughput screening experiment.

The title compound consists of two crystallographic independent erbium ions, one fully deprotonated (O₃PC₂H₄SO₃)^3- anion, three hydroxide ions, as well as two water molecules (one is coordinated to a erbium ion) (Fig. 1). The erbium ions are coordinated eightfold by oxygen atoms and form ErO₈ polyhedra (Fig. 2), which are linked (edge- and face-sharing) to inorganic layers Er–O–Er in the ab-plane (Fig. 3). While most often in metal phosphonosulfonates the organic linker bridges adjacent layers, in [Er₂(O₃PC₂H₄SO₃)(OH)₃(H₂O)]H₂O the anion (O₃PC₂H₄SO₃)^3- is only connected to one Er–O–Er layer. These layers are further linked via hydrogen bonds into a three-dimensional structure (Fig. 4). The non-coordinating H₂O molecules are located in between the layers.

Related literature top

For related structures, see: Sonnauer et al. (2007); Sonnauer & Stock (2008a,b); Benedetto et al. (1997); Adani et al. (1998); Du et al. (2006a,b); Du, Li et al. (2007); Du, Prosvirin & Mao (2007); Du, Xu et al. (2007).

Experimental top

H₂O₃PC₂H₄SO₃H was synthesized as previously reported (Sonnauer & Stock, 2008b). All other reagents were of analytical grade (Aldrich and Fluka) and were used without furhter purification. For the synthesis a special high-throughput reactor system was used. 79 µl (0.016 mmol) of 0.2 M Er(CH₃CO₂)₃.4H₂O, 53.2 µl (0.032 mmol) of 0.5 M H₂O₃PC₂H₄SO₃H, 23.7 µl (0.048 mmol) of 2.0 M NaOH, and 54 µl H₂O were filled in a teflon reactor and heated to 160 °C for 48 h. After filtration the pink rod-shaped single crystals were isolated.

Computing details top

Data collection: IPDS Program Package (Stoe & Cie, 1998); cell refinement: IPDS Program Package (Stoe & Cie, 1998); data reduction: IPDS Program Package (Stoe & Cie, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg & Putz, 1999); software used to prepare material for publication: publCIF (Westrip, 2008).

Figures top

	Fig. 1. Asymmetric unit of the title compound. Displacement ellipsoides are drawn at 50% propability level.
	Fig. 2. First coordination sphere of the erbium ions.
	Fig. 3. Inorganic Er–O–Er layer in the ab-plane of edge- and face-sharing ErO₈polyhedra.
	Fig. 4. The anions (O₃PC₂H₄SO₃)^3- are connected to one Er–O–Er layer at a time. The layers are linked via hydrogen bonds between the sulfonate groups and the coordinating water molecules into a three-dimensional structure.

Poly[[aquatri-µ₃-hydroxido-(µ₄-2-phosphonatoethanesulfonato)dierbium(III)] monohydrate] top

Crystal data top

[Er₂(C₂H₄O₆PS)(OH)₃(H₂O)]·H₂O	Z = 2
M_r = 608.65	F(000) = 554
Triclinic, P1	D_x = 3.611 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 5.8621 (6) Å	Cell parameters from 4793 reflections
b = 9.0443 (9) Å	θ = 2.5–28°
c = 11.6240 (11) Å	µ = 15.29 mm⁻¹
α = 105.543 (12)°	T = 293 K
β = 101.713 (11)°	Rod, pink
γ = 101.885 (11)°	0.08 × 0.07 × 0.06 mm
V = 558.81 (10) Å³

Data collection top

Stoe IPDS-1 diffractometer	2664 independent reflections
Radiation source: fine-focus sealed tube	2207 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.041
ϕ scans	θ_max = 28.1°, θ_min = 2.4°
Absorption correction: ψ scan (X-RED and X-SHAPE; Stoe & Cie, 1999)	h = −7→7
T_min = 0.293, T_max = 0.399	k = −11→11
4731 measured reflections	l = −15→15

Refinement top

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.031	H-atom parameters constrained
wR(F²) = 0.082	w = 1/[σ²(F_o²) + (0.0577P)²] where P = (F_o² + 2F_c²)/3
S = 0.97	(Δ/σ)_max = 0.001
2664 reflections	Δρ_max = 1.61 e Å⁻³
155 parameters	Δρ_min = −2.07 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008), Fc^*=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0044 (5)

Crystal data top

[Er₂(C₂H₄O₆PS)(OH)₃(H₂O)]·H₂O	γ = 101.885 (11)°
M_r = 608.65	V = 558.81 (10) Å³
Triclinic, P1	Z = 2
a = 5.8621 (6) Å	Mo Kα radiation
b = 9.0443 (9) Å	µ = 15.29 mm⁻¹
c = 11.6240 (11) Å	T = 293 K
α = 105.543 (12)°	0.08 × 0.07 × 0.06 mm
β = 101.713 (11)°

Data collection top

Stoe IPDS-1 diffractometer	2664 independent reflections
Absorption correction: ψ scan (X-RED and X-SHAPE; Stoe & Cie, 1999)	2207 reflections with I > 2σ(I)
T_min = 0.293, T_max = 0.399	R_int = 0.041
4731 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.031	0 restraints
wR(F²) = 0.082	H-atom parameters constrained
S = 0.97	Δρ_max = 1.61 e Å⁻³
2664 reflections	Δρ_min = −2.07 e Å⁻³
155 parameters

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'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 > σ(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 (Å²) top

	x	y	z	U_iso*/U_eq
Er1	0.21965 (5)	0.71416 (3)	0.57132 (3)	0.00796 (12)
Er2	0.27992 (5)	1.10732 (3)	0.55352 (3)	0.00839 (12)
S1	0.6239 (4)	0.2840 (2)	0.86984 (18)	0.0197 (4)
P1	0.6867 (3)	0.5153 (2)	0.65414 (16)	0.0080 (3)
O1	0.5161 (10)	0.6197 (6)	0.6590 (5)	0.0150 (10)
O2	0.5556 (9)	0.3377 (5)	0.5872 (5)	0.0106 (9)
O3	0.8809 (9)	0.5494 (6)	0.5852 (5)	0.0129 (10)
O4	0.5879 (13)	0.2641 (8)	0.9845 (6)	0.0324 (15)
O5	0.3963 (11)	0.2164 (7)	0.7714 (5)	0.0214 (12)
O6	0.8156 (13)	0.2224 (8)	0.8314 (7)	0.0323 (15)
O7	−0.0251 (9)	1.0829 (6)	0.3821 (5)	0.0110 (9)
O8	0.0459 (10)	0.7988 (6)	0.4152 (5)	0.0170 (11)
O9	0.5197 (9)	0.9454 (5)	0.6002 (5)	0.0100 (9)
O10	0.3173 (12)	0.8253 (7)	0.7926 (6)	0.0255 (13)
C1	0.8513 (15)	0.5462 (9)	0.8095 (7)	0.0185 (15)
H1A	0.9760	0.4907	0.8057	0.022*
H1B	0.9328	0.6592	0.8479	0.022*
C2	0.7080 (16)	0.4931 (10)	0.8961 (7)	0.0217 (16)
H2A	0.5621	0.5287	0.8864	0.026*
H2B	0.8053	0.5464	0.9813	0.026*
O11	0.093 (2)	1.0351 (13)	0.9079 (12)	0.078 (4)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Er1	0.00654 (18)	0.00560 (17)	0.01466 (18)	0.00295 (11)	0.00471 (12)	0.00566 (12)
Er2	0.00577 (18)	0.00797 (17)	0.01466 (18)	0.00329 (12)	0.00454 (12)	0.00646 (12)
S1	0.0221 (10)	0.0209 (9)	0.0176 (9)	0.0061 (8)	0.0051 (8)	0.0086 (7)
P1	0.0070 (8)	0.0064 (7)	0.0131 (8)	0.0029 (6)	0.0043 (6)	0.0053 (6)
O1	0.015 (3)	0.015 (2)	0.022 (3)	0.012 (2)	0.008 (2)	0.009 (2)
O2	0.010 (2)	0.009 (2)	0.015 (2)	0.0000 (18)	0.0045 (19)	0.0069 (18)
O3	0.010 (3)	0.017 (2)	0.016 (2)	0.004 (2)	0.008 (2)	0.009 (2)
O4	0.043 (4)	0.037 (4)	0.018 (3)	0.006 (3)	0.006 (3)	0.016 (3)
O5	0.019 (3)	0.025 (3)	0.012 (2)	0.000 (2)	−0.001 (2)	0.001 (2)
O6	0.032 (4)	0.035 (4)	0.039 (4)	0.019 (3)	0.015 (3)	0.014 (3)
O7	0.004 (2)	0.012 (2)	0.016 (2)	0.0030 (18)	0.0005 (19)	0.0030 (18)
O8	0.020 (3)	0.024 (3)	0.018 (3)	0.019 (2)	0.009 (2)	0.012 (2)
O9	0.007 (2)	0.009 (2)	0.015 (2)	0.0002 (18)	0.0050 (19)	0.0058 (18)
O10	0.032 (4)	0.027 (3)	0.022 (3)	0.015 (3)	0.009 (3)	0.009 (2)
C1	0.015 (4)	0.018 (4)	0.020 (4)	−0.001 (3)	0.003 (3)	0.006 (3)
C2	0.023 (4)	0.025 (4)	0.018 (4)	0.003 (3)	0.006 (3)	0.012 (3)
O11	0.108 (9)	0.093 (7)	0.119 (9)	0.082 (7)	0.093 (8)	0.086 (7)

Geometric parameters (Å, º) top

Er1—O1	2.269 (5)	S1—O4	1.442 (6)
Er1—O3ⁱ	2.287 (5)	S1—O6	1.449 (7)
Er1—O8	2.287 (5)	S1—O5	1.460 (6)
Er1—O9	2.334 (5)	S1—C2	1.777 (8)
Er1—O7ⁱⁱ	2.354 (5)	P1—O1	1.509 (5)
Er1—O10	2.394 (6)	P1—O2	1.535 (5)
Er1—O3ⁱⁱⁱ	2.450 (5)	P1—O3	1.547 (5)
Er1—O2ⁱⁱⁱ	2.475 (5)	P1—C1	1.784 (8)
Er1—P1ⁱⁱⁱ	3.1010 (18)	P1—Er1ⁱⁱⁱ	3.1010 (18)
Er1—Er2	3.5662 (5)	O2—Er2^vi	2.242 (4)
Er1—Er2^iv	3.7884 (6)	O2—Er1ⁱⁱⁱ	2.475 (5)
Er1—Er2ⁱⁱ	3.8428 (6)	O3—Er1^vii	2.287 (5)
Er2—O2^v	2.242 (5)	O3—Er1ⁱⁱⁱ	2.450 (5)
Er2—O8ⁱⁱ	2.299 (5)	O5—Er2^vi	2.353 (5)
Er2—O7	2.317 (5)	O7—Er1ⁱⁱ	2.354 (5)
Er2—O9	2.319 (5)	O7—Er2ⁱⁱ	2.416 (5)
Er2—O9^iv	2.329 (5)	O8—Er2ⁱⁱ	2.299 (5)
Er2—O5^v	2.353 (5)	O9—Er2^iv	2.329 (5)
Er2—O7ⁱⁱ	2.416 (5)	C1—C2	1.544 (10)
Er2—O8	2.716 (6)	C1—H1A	0.9700
Er2—Er2ⁱⁱ	3.2420 (8)	C1—H1B	0.9700
Er2—Er2^iv	3.7479 (7)	C2—H2A	0.9700
Er2—Er1^iv	3.7884 (6)	C2—H2B	0.9700

O1—Er1—O3ⁱ	101.48 (18)	O7—Er2—O8	67.01 (16)
O1—Er1—O8	150.13 (18)	O9—Er2—O8	70.88 (16)
O3ⁱ—Er1—O8	99.53 (19)	O9^iv—Er2—O8	76.51 (16)
O1—Er1—O9	87.87 (18)	O5^v—Er2—O8	126.96 (17)
O3ⁱ—Er1—O9	160.71 (18)	O7ⁱⁱ—Er2—O8	54.15 (16)
O8—Er1—O9	78.90 (19)	O2^v—Er2—Er2ⁱⁱ	148.76 (13)
O1—Er1—O7ⁱⁱ	141.65 (18)	O8ⁱⁱ—Er2—Er2ⁱⁱ	55.60 (15)
O3ⁱ—Er1—O7ⁱⁱ	85.63 (17)	O7—Er2—Er2ⁱⁱ	48.05 (12)
O8—Er1—O7ⁱⁱ	60.84 (17)	O9—Er2—Er2ⁱⁱ	108.32 (12)
O9—Er1—O7ⁱⁱ	76.79 (17)	O9^iv—Er2—Er2ⁱⁱ	109.66 (12)
O1—Er1—O10	70.82 (19)	O5^v—Er2—Er2ⁱⁱ	112.02 (14)
O3ⁱ—Er1—O10	86.1 (2)	O7ⁱⁱ—Er2—Er2ⁱⁱ	45.52 (12)
O8—Er1—O10	131.87 (19)	O8—Er2—Er2ⁱⁱ	44.30 (11)
O9—Er1—O10	81.02 (19)	O2^v—Er2—Er1	142.54 (13)
O7ⁱⁱ—Er1—O10	72.17 (18)	O8ⁱⁱ—Er2—Er1	112.98 (13)
O1—Er1—O3ⁱⁱⁱ	80.62 (18)	O7—Er2—Er1	105.98 (12)
O3ⁱ—Er1—O3ⁱⁱⁱ	69.78 (19)	O9—Er2—Er1	40.13 (11)
O8—Er1—O3ⁱⁱⁱ	87.03 (18)	O9^iv—Er2—Er1	90.81 (11)
O9—Er1—O3ⁱⁱⁱ	128.90 (16)	O5^v—Er2—Er1	90.97 (14)
O7ⁱⁱ—Er1—O3ⁱⁱⁱ	135.88 (18)	O7ⁱⁱ—Er2—Er1	40.96 (11)
O10—Er1—O3ⁱⁱⁱ	137.99 (18)	O8—Er2—Er1	39.89 (10)
O1—Er1—O2ⁱⁱⁱ	76.65 (17)	Er2ⁱⁱ—Er2—Er1	68.536 (15)
O3ⁱ—Er1—O2ⁱⁱⁱ	128.23 (17)	O2^v—Er2—Er2^iv	88.10 (13)
O8—Er1—O2ⁱⁱⁱ	73.69 (17)	O8ⁱⁱ—Er2—Er2^iv	168.52 (15)
O9—Er1—O2ⁱⁱⁱ	70.13 (16)	O7—Er2—Er2^iv	108.96 (12)
O7ⁱⁱ—Er1—O2ⁱⁱⁱ	127.72 (16)	O9—Er2—Er2^iv	36.36 (11)
O10—Er1—O2ⁱⁱⁱ	136.9 (2)	O9^iv—Er2—Er2^iv	36.18 (12)
O3ⁱⁱⁱ—Er1—O2ⁱⁱⁱ	58.77 (15)	O5^v—Er2—Er2^iv	110.34 (15)
O1—Er1—P1ⁱⁱⁱ	76.23 (14)	O7ⁱⁱ—Er2—Er2^iv	103.29 (11)
O3ⁱ—Er1—P1ⁱⁱⁱ	99.19 (13)	O8—Er2—Er2^iv	69.65 (11)
O8—Er1—P1ⁱⁱⁱ	79.66 (13)	Er2ⁱⁱ—Er2—Er2^iv	113.801 (19)
O9—Er1—P1ⁱⁱⁱ	99.42 (12)	Er1—Er2—Er2^iv	62.333 (12)
O7ⁱⁱ—Er1—P1ⁱⁱⁱ	140.41 (12)	O2^v—Er2—Er1^iv	38.73 (13)
O10—Er1—P1ⁱⁱⁱ	147.01 (15)	O8ⁱⁱ—Er2—Er1^iv	127.02 (12)
O3ⁱⁱⁱ—Er1—P1ⁱⁱⁱ	29.49 (11)	O7—Er2—Er1^iv	93.57 (12)
O2ⁱⁱⁱ—Er1—P1ⁱⁱⁱ	29.30 (11)	O9—Er2—Er1^iv	85.59 (11)
O1—Er1—Er2	126.95 (13)	O9^iv—Er2—Er1^iv	35.72 (12)
O3ⁱ—Er1—Er2	126.08 (13)	O5^v—Er2—Er1^iv	109.15 (14)
O8—Er1—Er2	49.59 (14)	O7ⁱⁱ—Er2—Er1^iv	159.77 (11)
O9—Er1—Er2	39.82 (12)	O8—Er2—Er1^iv	112.23 (11)
O7ⁱⁱ—Er1—Er2	42.28 (11)	Er2ⁱⁱ—Er2—Er1^iv	138.048 (15)
O10—Er1—Er2	88.68 (14)	Er1—Er2—Er1^iv	118.815 (12)
O3ⁱⁱⁱ—Er1—Er2	133.33 (11)	Er2^iv—Er2—Er1^iv	56.483 (10)
O2ⁱⁱⁱ—Er1—Er2	88.92 (10)	O4—S1—O6	114.3 (4)
P1ⁱⁱⁱ—Er1—Er2	112.89 (3)	O4—S1—O5	110.4 (4)
O1—Er1—Er2^iv	81.22 (13)	O6—S1—O5	111.1 (4)
O3ⁱ—Er1—Er2^iv	161.90 (13)	O4—S1—C2	106.3 (4)
O8—Er1—Er2^iv	72.40 (14)	O6—S1—C2	107.4 (4)
O9—Er1—Er2^iv	35.63 (12)	O5—S1—C2	106.9 (4)
O7ⁱⁱ—Er1—Er2^iv	103.46 (11)	O1—P1—O2	112.9 (3)
O10—Er1—Er2^iv	111.42 (16)	O1—P1—O3	116.1 (3)
O3ⁱⁱⁱ—Er1—Er2^iv	93.28 (11)	O2—P1—O3	103.3 (3)
O2ⁱⁱⁱ—Er1—Er2^iv	34.51 (11)	O1—P1—C1	108.1 (4)
P1ⁱⁱⁱ—Er1—Er2^iv	63.81 (3)	O2—P1—C1	110.6 (3)
Er2—Er1—Er2^iv	61.185 (12)	O3—P1—C1	105.5 (3)
O1—Er1—Er2ⁱⁱ	175.89 (14)	O1—P1—Er1ⁱⁱⁱ	130.4 (2)
O3ⁱ—Er1—Er2ⁱⁱ	78.19 (13)	O2—P1—Er1ⁱⁱⁱ	52.12 (18)
O8—Er1—Er2ⁱⁱ	33.17 (13)	O3—P1—Er1ⁱⁱⁱ	51.2 (2)
O9—Er1—Er2ⁱⁱ	91.27 (12)	C1—P1—Er1ⁱⁱⁱ	121.5 (3)
O7ⁱⁱ—Er1—Er2ⁱⁱ	34.35 (12)	P1—O1—Er1	153.3 (3)
O10—Er1—Er2ⁱⁱ	105.08 (14)	P1—O2—Er2^vi	154.7 (3)
O3ⁱⁱⁱ—Er1—Er2ⁱⁱ	103.01 (12)	P1—O2—Er1ⁱⁱⁱ	98.6 (2)
O2ⁱⁱⁱ—Er1—Er2ⁱⁱ	106.83 (11)	Er2^vi—O2—Er1ⁱⁱⁱ	106.76 (19)
P1ⁱⁱⁱ—Er1—Er2ⁱⁱ	107.88 (4)	P1—O3—Er1^vii	150.2 (3)
Er2—Er1—Er2ⁱⁱ	51.734 (13)	P1—O3—Er1ⁱⁱⁱ	99.3 (2)
Er2^iv—Er1—Er2ⁱⁱ	100.378 (12)	Er1^vii—O3—Er1ⁱⁱⁱ	110.22 (19)
O2^v—Er2—O8ⁱⁱ	100.04 (19)	S1—O5—Er2^vi	136.5 (3)
O2^v—Er2—O7	105.14 (17)	Er2—O7—Er1ⁱⁱ	110.7 (2)
O8ⁱⁱ—Er2—O7	61.23 (18)	Er2—O7—Er2ⁱⁱ	86.43 (16)
O2^v—Er2—O9	102.46 (17)	Er1ⁱⁱ—O7—Er2ⁱⁱ	96.76 (17)
O8ⁱⁱ—Er2—O9	146.13 (16)	Er1—O8—Er2ⁱⁱ	113.9 (2)
O7—Er2—O9	133.96 (17)	Er1—O8—Er2	90.51 (19)
O2^v—Er2—O9^iv	74.44 (17)	Er2ⁱⁱ—O8—Er2	80.09 (15)
O8ⁱⁱ—Er2—O9^iv	138.60 (17)	Er2—O9—Er2^iv	107.46 (18)
O7—Er2—O9^iv	80.31 (17)	Er2—O9—Er1	100.05 (18)
O9—Er2—O9^iv	72.54 (18)	Er2^iv—O9—Er1	108.64 (19)
O2^v—Er2—O5^v	77.68 (19)	C2—C1—P1	117.8 (6)
O8ⁱⁱ—Er2—O5^v	79.5 (2)	C2—C1—H1A	107.9
O7—Er2—O5^v	140.67 (19)	P1—C1—H1A	107.9
O9—Er2—O5^v	80.92 (19)	C2—C1—H1B	107.9
O9^iv—Er2—O5^v	135.8 (2)	P1—C1—H1B	107.9
O2^v—Er2—O7ⁱⁱ	153.74 (18)	H1A—C1—H1B	107.2
O8ⁱⁱ—Er2—O7ⁱⁱ	72.76 (17)	C1—C2—S1	115.0 (6)
O7—Er2—O7ⁱⁱ	93.57 (16)	C1—C2—H2A	108.5
O9—Er2—O7ⁱⁱ	75.87 (16)	S1—C2—H2A	108.5
O9^iv—Er2—O7ⁱⁱ	127.80 (16)	C1—C2—H2B	108.5
O5^v—Er2—O7ⁱⁱ	76.18 (18)	S1—C2—H2B	108.5
O2^v—Er2—O8	150.83 (16)	H2A—C2—H2B	107.5
O8ⁱⁱ—Er2—O8	99.91 (16)

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

Experimental details

Crystal data
Chemical formula	[Er₂(C₂H₄O₆PS)(OH)₃(H₂O)]·H₂O
M_r	608.65
Crystal system, space group	Triclinic, P1
Temperature (K)	293
a, b, c (Å)	5.8621 (6), 9.0443 (9), 11.6240 (11)
α, β, γ (°)	105.543 (12), 101.713 (11), 101.885 (11)
V (Å³)	558.81 (10)
Z	2
Radiation type	Mo Kα
µ (mm⁻¹)	15.29
Crystal size (mm)	0.08 × 0.07 × 0.06

Data collection
Diffractometer	Stoe IPDS1 diffractometer
Absorption correction	ψ scan (X-RED and X-SHAPE; Stoe & Cie, 1999)
T_min, T_max	0.293, 0.399
No. of measured, independent and observed [I > 2σ(I)] reflections	4731, 2664, 2207
R_int	0.041
(sin θ/λ)_max (Å⁻¹)	0.662

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.031, 0.082, 0.97
No. of reflections	2664
No. of parameters	155
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	1.61, −2.07

Computer programs: IPDS Program Package (Stoe & Cie, 1998), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg & Putz, 1999), publCIF (Westrip, 2008).

Acknowledgements

The authors thank PD Dr Christian Näther for the acquisition of the single-crystal data. This work was supported by the DFG-Project STO 643/2-2.

References

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