Poly[[tetra­aqua­bis[μ4-2,2′-(p-phenyl­ene­di­oxy)diacetato][μ2-2,2′-(p-phenyl­ene­di­oxy)diacetato]dierbium(III)] hexa­hydrate]

Wei, D.-Y.; Zhang, Y.-G.; Wang, M.-L.; Zhu, Z.-K.

doi:10.1107/S1600536809046613

Poly[[tetraaquabis[μ₄-2,2′-(p-phenylenedioxy)diacetato][μ₂-2,2′-(p-phenylenedioxy)diacetato]dierbium(III)] hexahydrate]

D.-Y. Wei, Y.-G. Zhang, M.-L. Wang and Z.-K. Zhu

The asymmetric unit of the title compound, [Er₂(C₁₀H₈O₆)₃(H₂O)₄]·6H₂O, comprises one Er³⁺ ion, one and a half 2,2′-(p-phenylenedioxy)diacetate (hqda) ligands, two coordinated water molecules and three uncoordinated water molecules. The Er³⁺ ion is nine-coordinated by seven O atoms from hqda ligands and two O atoms from water molecules. In the title compound, there are two types of crystallographically independent ligands: one with an inversion center in the middle of the ligand is chelating on both ends of the ligand towards each one Er center; the other hqda ligands are bridging-chelating on one side, and bridging on the other end of the ligand. Two adjacent Er³⁺ ions are thus chelated and bridged by –COO groups from hqda ligands in three coordination modes (briding–chelating, bridging and chelating). These building blocks are linked by OOC—CH₂O—C₆H₄—OCH₂—COO spacers, forming two-dimensional neutral layers. Adjacent layers are linked by O—H

O hydrogen-bonding interactions, forming a three-dimensional supermolecular network.

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Supporting information

	Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536809046613/zl2248sup1.cif Contains datablocks global, I
	Structure factor file (CIF format) https://doi.org/10.1107/S1600536809046613/zl2248Isup2.hkl Contains datablock I

CCDC reference: 758662

checkCIF report

Key indicators

Single-crystal X-ray study
T = 298 K
Mean (C-C) = 0.004 Å
R factor = 0.019
wR factor = 0.044
Data-to-parameter ratio = 16.2

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor       O14    -   H14D   ...          ?

Alert level C
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Er1    --  O7      ..       6.32 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Er1    --  O5_a    ..       9.24 su
PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X)  Er1    --  O6_a    ..       6.17 su
PLAT910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) .....          6
PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L=  0.600          3
PLAT041_ALERT_1_C Calc. and Reported SumFormula    Strings  Differ          ?
PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings  Differ          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       2.00 Ratio
PLAT774_ALERT_1_C Suspect X-Y Bond in CIF:   ER1    --  ER1     ..       3.85 Ang.
PLAT912_ALERT_4_C Missing # of FCF Reflections Above STh/L=  0.600         32

Alert level G
PLAT860_ALERT_3_G Note: Number of Least-Squares Restraints .......          1
PLAT154_ALERT_1_G The su's on the Cell Angles are Equal  (x 10000)       3000 Deg.
PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) .       1.27 Ratio

   0 ALERT level A = In general: serious problem
   1 ALERT level B = Potentially serious problem
  10 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   5 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   4 ALERT type 2 Indicator that the structure model may be wrong or deficient
   3 ALERT type 3 Indicator that the structure quality may be low
   2 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

Comment top

The investigation of the assembly of metal-organic frameworks (MOFs) has attracted great interest due to their versatile architecture and promising applications for ion exchange, gas storage, separation, and catalysis (Maji et al., 2005; Moulton & Zaworotko 2001; Rao et al., 2004; Sun et al., 2006; Zou et al., 2006). The selection of multifunctional bridging ligands is crucial to synthesize novel MOFS (Burrows et al., 2000; Huang et al., 2005). Among these, hydroquinone-O,O'-diacetic acid (H₂hqda) is a good ligand in the preparation various metal-organic coordination polymers. Recently, several lanthanide(III) hqda compounds with fascinating structures have been reported (Hong et al., 2006; Li et al., 2008). Herein, we report a new compound [Er₂(hqda)₃(H₂O)₄].6H₂O.

The asymmetric unit of the title compound comprises one Er³⁺ ion, one and a half 2,2'-(p-phenylenedioxy)diacetate anions (hqda), two coordinated water molecules and three lattice water molecules. The Er³⁺ ion is nine coordinated by seven oxygen atoms of hqda ligands and two oxygen atoms of aqua ligands (Fig 1). The Er—O (carboxylate) distances fall in the range 2.341 (2)–2.529 (2) Å, and those of the Er—O (water) bonds are 2.317 (2) Å and 2.368 (2) Å, respectively. The coordination environment of the Er³⁺ ion may be described as a distorted tricapped trigonal prism. In the title compound, there are two types of crystallographically independent ligands. One type with an inversion center in the middle of the ligand is chelating on both ends of the ligand towards each one Er center. The other type is bridging-chelating on one side, and bridging on the other, thus connecting each two Er centers with each other. Two adjacent Er³⁺ ions are thus chelated and briged by –COO groups from hqda ligands in three coordination modes (briding-chelating, bridging and chelating modes) to form [Er₂(hqda)₃(H₂O)₄].6H₂O building blocks. These building blocks are linked by the OOC–CH₂O–C₆H₄–OCH₂COO (hqda) spacers to form two-dimensional neutral layers perpendicular to the [100] direction (Fig 2). The lattice water molecules are sandwiched between these two-dimensional layers and hydrogen bonded with them. The adjacent two-dimensional layers are further interlinked by these hydrogen bonds to form a three-dimensional supermolecular network.

Related literature top

For general background on metal-organic frameworks (MOFs), see: Maji et al. (2005); Moulton & Zaworotko (2001); Rao et al. (2004); Sun et al. (2006); Zou et al. (2006); Burrows et al. (2000); Huang et al. (2005). For related stuctures, see: Hong et al. (2006); Li et al. (2008).

Experimental top

All commercially available chemicals were of reagent grade and used without further purification. Er(NO₃)₃.6H₂O (0.0922 g, 0.2 mmol) and H₂hqda (0.0452 g, 0.2 mmol) were added to a stirred solution of 20 ml dimethyl formamide/H₂O to form a clear solution, which was mixed with 5 ml ethanol and 0.15 ml triethylamine. The resulting solution was kept at room temperature and pink, block-like crystals grew after ca. 20 days.

Computing details top

Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO (Rigaku, 1998); data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. ORTEP view of complex molecule of the title compound. Displacement ellipsoids are drawn at the 45% probability level. H atoms and lattice water molecules were omitted for clarity. (Symmetry codes: ii = -x + 1, -y + 1, -z; iii = x, y, z-1; iv = x - 1, y, z; v = -x + 2, -y + 2, -z).
	Fig. 2. Two-dimensional layer in the title compond perpendicular to the [100] direction with H-atoms and lattice water molecules omitted.

Poly[[tetraaquabis[µ₄-2,2'-(p-phenylenedioxy)diacetato][µ₂- 2,2'-(p-phenylenedioxy)diacetato]dierbium(III)] hexahydrate] top

Crystal data top

[Er₂(C₁₀H₈O₆)₃(H₂O)₄]·6H₂O	Z = 1
M_r = 1187.17	F(000) = 584
Triclinic, P1	D_x = 2.032 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 8.5993 (17) Å	Cell parameters from 8985 reflections
b = 9.6356 (19) Å	θ = 3.2–27.5°
c = 12.689 (3) Å	µ = 4.40 mm⁻¹
α = 102.46 (3)°	T = 298 K
β = 95.28 (3)°	Block, pink
γ = 106.69 (3)°	0.43 × 0.29 × 0.15 mm
V = 970.0 (4) Å³

Data collection top

Rigaku R-AXIS RAPID diffractometer	4403 independent reflections
Radiation source: fine-focus sealed tube	4219 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.030
Detector resolution: 0 pixels mm^-1	θ_max = 27.5°, θ_min = 3.2°
ω scans	h = −9→11
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −12→12
T_min = 0.312, T_max = 0.535	l = −16→16
9659 measured reflections

Refinement top

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.019	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.044	H-atom parameters constrained
S = 1.17	w = 1/[σ²(F_o²) + (0.0129P)² + 0.5344P] where P = (F_o² + 2F_c²)/3
4403 reflections	(Δ/σ)_max = 0.001
271 parameters	Δρ_max = 0.46 e Å⁻³
1 restraint	Δρ_min = −1.08 e Å⁻³

Crystal data top

[Er₂(C₁₀H₈O₆)₃(H₂O)₄]·6H₂O	γ = 106.69 (3)°
M_r = 1187.17	V = 970.0 (4) Å³
Triclinic, P1	Z = 1
a = 8.5993 (17) Å	Mo Kα radiation
b = 9.6356 (19) Å	µ = 4.40 mm⁻¹
c = 12.689 (3) Å	T = 298 K
α = 102.46 (3)°	0.43 × 0.29 × 0.15 mm
β = 95.28 (3)°

Data collection top

Rigaku R-AXIS RAPID diffractometer	4403 independent reflections
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	4219 reflections with I > 2σ(I)
T_min = 0.312, T_max = 0.535	R_int = 0.030
9659 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.019	1 restraint
wR(F²) = 0.044	H-atom parameters constrained
S = 1.17	Δρ_max = 0.46 e Å⁻³
4403 reflections	Δρ_min = −1.08 e Å⁻³
271 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	0.869905 (13)	0.797688 (12)	−0.007667 (8)	0.01362 (4)
O1	0.7733 (2)	0.9698 (2)	0.10577 (15)	0.0238 (4)
O2	0.9134 (2)	1.2049 (2)	0.10636 (14)	0.0220 (4)
O3	0.5844 (2)	1.0620 (2)	0.24732 (14)	0.0230 (4)
O4	0.7484 (3)	0.8777 (2)	0.61490 (15)	0.0307 (5)
O5	0.8979 (2)	1.0035 (2)	0.90125 (13)	0.0189 (4)
O6	0.7683 (3)	0.7795 (2)	0.79481 (15)	0.0295 (5)
O7	1.0417 (2)	0.6690 (2)	0.07609 (14)	0.0224 (4)
O8	0.8399 (2)	0.7140 (2)	0.15645 (15)	0.0239 (4)
O9	0.9096 (3)	0.5949 (3)	0.32042 (15)	0.0267 (5)
O10	0.7747 (2)	0.5361 (2)	−0.08718 (17)	0.0293 (5)
H10D	0.8146	0.4726	−0.0746	0.044*
H10C	0.6899	0.4916	−0.1317	0.044*
O11	0.5849 (3)	0.7150 (3)	−0.03432 (19)	0.0386 (6)
H11D	0.5209	0.7517	−0.0033	0.058*
H11C	0.5269	0.6420	−0.0823	0.058*
C1	0.8034 (3)	1.1075 (3)	0.13378 (19)	0.0173 (5)
C2	0.6953 (4)	1.1713 (3)	0.2068 (2)	0.0235 (6)
H2B	0.7656	1.2496	0.2684	0.028*
H2A	0.6324	1.2167	0.1655	0.028*
C3	0.6421 (3)	1.0209 (3)	0.3382 (2)	0.0211 (6)
C4	0.5518 (4)	0.8850 (4)	0.3518 (2)	0.0339 (7)
H4A	0.4639	0.8225	0.2982	0.041*
C5	0.5904 (4)	0.8402 (4)	0.4447 (2)	0.0360 (7)
H5A	0.5279	0.7483	0.4534	0.043*
C6	0.7213 (4)	0.9312 (3)	0.5240 (2)	0.0241 (6)
C7	0.8153 (4)	1.0642 (4)	0.5093 (3)	0.0423 (9)
H7A	0.9059	1.1246	0.5616	0.051*
C8	0.7750 (4)	1.1096 (4)	0.4154 (3)	0.0430 (9)
H8A	0.8390	1.2002	0.4056	0.052*
C9	0.8428 (4)	0.9852 (3)	0.7110 (2)	0.0261 (6)
H9B	0.8012	1.0699	0.7253	0.031*
H9A	0.9565	1.0214	0.7010	0.031*
C10	0.8329 (3)	0.9155 (3)	0.8065 (2)	0.0190 (5)
C11	0.9563 (3)	0.6601 (3)	0.15137 (19)	0.0181 (5)
C12	1.0010 (4)	0.5810 (4)	0.2341 (2)	0.0243 (6)
H12B	0.9788	0.4759	0.1988	0.029*
H12A	1.1177	0.6239	0.2631	0.029*
C13	0.9586 (3)	0.5444 (3)	0.4075 (2)	0.0206 (5)
C14	0.8822 (3)	0.5722 (3)	0.4975 (2)	0.0232 (6)
H14A	0.8028	0.6202	0.4956	0.028*
C15	1.0760 (3)	0.4714 (3)	0.4092 (2)	0.0230 (6)
H15A	1.1263	0.4517	0.3484	0.028*
O12	0.4607 (3)	0.4588 (3)	−0.19590 (18)	0.0376 (5)
H12D	0.3720	0.3998	−0.1934	0.056*
H12C	0.4699	0.4849	−0.2530	0.056*
O13	0.3829 (3)	0.8206 (4)	0.0782 (2)	0.0567 (8)
H13D	0.2831	0.8057	0.0727	0.085*
H13C	0.4297	0.9046	0.1180	0.085*
O14	0.5142 (4)	0.5730 (4)	0.6226 (2)	0.0636 (8)
H14C	0.5877	0.6523	0.6493	0.095*
H14D	0.4202	0.5660	0.5976	0.095*

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Er1	0.01580 (6)	0.01211 (7)	0.01281 (6)	0.00315 (5)	0.00181 (4)	0.00477 (4)
O1	0.0278 (10)	0.0177 (11)	0.0276 (10)	0.0072 (9)	0.0128 (8)	0.0058 (8)
O2	0.0267 (10)	0.0182 (11)	0.0226 (9)	0.0063 (9)	0.0097 (8)	0.0070 (8)
O3	0.0216 (9)	0.0332 (12)	0.0170 (8)	0.0080 (9)	0.0051 (8)	0.0121 (9)
O4	0.0492 (13)	0.0192 (11)	0.0153 (9)	0.0017 (10)	−0.0075 (9)	0.0049 (8)
O5	0.0204 (9)	0.0196 (10)	0.0136 (8)	0.0039 (8)	−0.0023 (7)	0.0033 (7)
O6	0.0401 (12)	0.0184 (11)	0.0222 (9)	−0.0010 (10)	−0.0054 (9)	0.0071 (9)
O7	0.0259 (10)	0.0254 (11)	0.0203 (9)	0.0089 (9)	0.0066 (8)	0.0128 (8)
O8	0.0283 (10)	0.0270 (12)	0.0234 (9)	0.0126 (9)	0.0078 (8)	0.0140 (9)
O9	0.0357 (11)	0.0370 (13)	0.0191 (9)	0.0213 (11)	0.0086 (8)	0.0164 (9)
O10	0.0248 (10)	0.0174 (11)	0.0422 (11)	0.0076 (9)	−0.0026 (9)	0.0024 (9)
O11	0.0191 (10)	0.0379 (15)	0.0471 (13)	0.0097 (11)	−0.0015 (10)	−0.0118 (11)
C1	0.0199 (12)	0.0210 (15)	0.0123 (11)	0.0076 (11)	0.0018 (10)	0.0057 (10)
C2	0.0336 (15)	0.0248 (16)	0.0195 (12)	0.0145 (14)	0.0110 (12)	0.0110 (12)
C3	0.0233 (13)	0.0291 (16)	0.0135 (11)	0.0096 (13)	0.0060 (10)	0.0079 (11)
C4	0.0394 (18)	0.0275 (18)	0.0242 (14)	−0.0007 (15)	−0.0117 (13)	0.0069 (13)
C5	0.050 (2)	0.0211 (17)	0.0260 (14)	−0.0022 (15)	−0.0099 (14)	0.0078 (13)
C6	0.0339 (15)	0.0229 (16)	0.0145 (11)	0.0078 (13)	0.0009 (11)	0.0059 (11)
C7	0.0423 (19)	0.042 (2)	0.0264 (15)	−0.0108 (17)	−0.0125 (14)	0.0158 (15)
C8	0.0414 (19)	0.041 (2)	0.0341 (17)	−0.0128 (17)	−0.0065 (15)	0.0236 (17)
C9	0.0363 (16)	0.0221 (16)	0.0147 (12)	0.0023 (13)	−0.0018 (11)	0.0056 (11)
C10	0.0196 (13)	0.0215 (15)	0.0164 (11)	0.0066 (12)	0.0010 (10)	0.0060 (11)
C11	0.0234 (13)	0.0131 (13)	0.0145 (11)	0.0014 (11)	−0.0009 (10)	0.0039 (10)
C12	0.0328 (15)	0.0282 (17)	0.0199 (12)	0.0147 (14)	0.0086 (12)	0.0139 (12)
C13	0.0277 (14)	0.0196 (15)	0.0165 (12)	0.0080 (12)	0.0024 (10)	0.0087 (11)
C14	0.0261 (14)	0.0264 (16)	0.0232 (13)	0.0142 (13)	0.0056 (11)	0.0106 (12)
C15	0.0299 (15)	0.0252 (16)	0.0186 (12)	0.0124 (13)	0.0076 (11)	0.0090 (12)
O12	0.0275 (11)	0.0397 (15)	0.0333 (11)	−0.0039 (11)	−0.0022 (9)	0.0064 (11)
O13	0.0216 (12)	0.067 (2)	0.0594 (16)	0.0098 (13)	−0.0010 (11)	−0.0214 (15)
O14	0.0631 (19)	0.052 (2)	0.0439 (15)	−0.0218 (16)	−0.0011 (13)	0.0059 (14)

Geometric parameters (Å, º) top

Er1—O11	2.317 (2)	C1—C2	1.531 (3)
Er1—O2ⁱ	2.3415 (18)	C2—H2B	0.9700
Er1—O1	2.3437 (19)	C2—H2A	0.9700
Er1—O10	2.368 (2)	C3—C8	1.366 (4)
Er1—O5ⁱⁱ	2.381 (2)	C3—C4	1.373 (4)
Er1—O8	2.3996 (18)	C4—C5	1.383 (4)
Er1—O5ⁱⁱⁱ	2.4684 (19)	C4—H4A	0.9300
Er1—O7	2.4864 (19)	C5—C6	1.376 (4)
Er1—O6ⁱⁱⁱ	2.529 (2)	C5—H5A	0.9300
Er1—C11	2.798 (2)	C6—C7	1.366 (5)
Er1—C10ⁱⁱⁱ	2.859 (3)	C7—C8	1.403 (4)
Er1—Er1ⁱ	3.8505 (13)	C7—H7A	0.9300
O1—C1	1.240 (3)	C8—H8A	0.9300
O2—C1	1.260 (3)	C9—C10	1.505 (3)
O2—Er1ⁱ	2.3415 (18)	C9—H9B	0.9700
O3—C3	1.392 (3)	C9—H9A	0.9700
O3—C2	1.425 (3)	C10—Er1^iv	2.859 (3)
O4—C6	1.388 (3)	C11—C12	1.506 (3)
O4—C9	1.417 (3)	C12—H12B	0.9700
O5—C10	1.281 (3)	C12—H12A	0.9700
O5—Er1ⁱⁱ	2.381 (2)	C13—C14	1.384 (4)
O5—Er1^iv	2.4684 (19)	C13—C15	1.388 (4)
O6—C10	1.237 (4)	C14—C15^v	1.388 (3)
O6—Er1^iv	2.529 (2)	C14—H14A	0.9300
O7—C11	1.260 (3)	C15—C14^v	1.388 (3)
O8—C11	1.254 (3)	C15—H15A	0.9300
O9—C13	1.378 (3)	O12—H12D	0.8176
O9—C12	1.411 (3)	O12—H12C	0.8196
O10—H10D	0.8194	O13—H13D	0.8221
O10—H10C	0.8213	O13—H13C	0.8190
O11—H11D	0.8212	O14—H14C	0.8180
O11—H11C	0.8194	O14—H14D	0.8188

O11—Er1—O2ⁱ	140.01 (8)	C10—O6—Er1^iv	92.30 (16)
O11—Er1—O1	69.84 (8)	C11—O7—Er1	90.52 (15)
O2ⁱ—Er1—O1	139.47 (7)	C11—O8—Er1	94.74 (14)
O11—Er1—O10	71.00 (8)	C13—O9—C12	114.6 (2)
O2ⁱ—Er1—O10	84.46 (8)	Er1—O10—H10D	128.3
O1—Er1—O10	135.94 (7)	Er1—O10—H10C	124.8
O11—Er1—O5ⁱⁱ	141.78 (7)	H10D—O10—H10C	106.9
O2ⁱ—Er1—O5ⁱⁱ	74.46 (7)	Er1—O11—H11D	130.0
O1—Er1—O5ⁱⁱ	71.96 (7)	Er1—O11—H11C	124.3
O10—Er1—O5ⁱⁱ	142.81 (7)	H11D—O11—H11C	105.6
O11—Er1—O8	82.71 (8)	O1—C1—O2	127.0 (2)
O2ⁱ—Er1—O8	125.12 (6)	O1—C1—C2	118.6 (2)
O1—Er1—O8	74.50 (7)	O2—C1—C2	114.3 (2)
O10—Er1—O8	81.33 (8)	O3—C2—C1	113.5 (2)
O5ⁱⁱ—Er1—O8	86.19 (7)	O3—C2—H2B	108.9
O11—Er1—O5ⁱⁱⁱ	96.38 (8)	C1—C2—H2B	108.9
O2ⁱ—Er1—O5ⁱⁱⁱ	74.53 (6)	O3—C2—H2A	108.9
O1—Er1—O5ⁱⁱⁱ	75.37 (6)	C1—C2—H2A	108.9
O10—Er1—O5ⁱⁱⁱ	128.65 (7)	H2B—C2—H2A	107.7
O5ⁱⁱ—Er1—O5ⁱⁱⁱ	74.90 (7)	C8—C3—C4	119.4 (2)
O8—Er1—O5ⁱⁱⁱ	148.16 (7)	C8—C3—O3	124.3 (3)
O11—Er1—O7	123.14 (8)	C4—C3—O3	116.3 (3)
O2ⁱ—Er1—O7	72.14 (6)	C3—C4—C5	120.6 (3)
O1—Er1—O7	119.42 (7)	C3—C4—H4A	119.7
O10—Er1—O7	68.62 (7)	C5—C4—H4A	119.7
O5ⁱⁱ—Er1—O7	75.81 (7)	C6—C5—C4	120.1 (3)
O8—Er1—O7	53.28 (6)	C6—C5—H5A	120.0
O5ⁱⁱⁱ—Er1—O7	140.25 (6)	C4—C5—H5A	120.0
O11—Er1—O6ⁱⁱⁱ	72.43 (8)	C7—C6—C5	119.6 (3)
O2ⁱ—Er1—O6ⁱⁱⁱ	71.57 (7)	C7—C6—O4	124.5 (3)
O1—Er1—O6ⁱⁱⁱ	108.94 (7)	C5—C6—O4	115.8 (3)
O10—Er1—O6ⁱⁱⁱ	77.05 (8)	C6—C7—C8	120.0 (3)
O5ⁱⁱ—Er1—O6ⁱⁱⁱ	122.41 (7)	C6—C7—H7A	120.0
O8—Er1—O6ⁱⁱⁱ	151.20 (7)	C8—C7—H7A	120.0
O5ⁱⁱⁱ—Er1—O6ⁱⁱⁱ	52.04 (7)	C3—C8—C7	120.2 (3)
O7—Er1—O6ⁱⁱⁱ	131.64 (7)	C3—C8—H8A	119.9
O11—Er1—C11	103.21 (9)	C7—C8—H8A	119.9
O2ⁱ—Er1—C11	98.81 (7)	O4—C9—C10	109.7 (2)
O1—Er1—C11	97.32 (7)	O4—C9—H9B	109.7
O10—Er1—C11	72.86 (8)	C10—C9—H9B	109.7
O5ⁱⁱ—Er1—C11	80.41 (7)	O4—C9—H9A	109.7
O8—Er1—C11	26.52 (7)	C10—C9—H9A	109.7
O5ⁱⁱⁱ—Er1—C11	155.31 (7)	H9B—C9—H9A	108.2
O7—Er1—C11	26.77 (7)	O6—C10—O5	121.1 (2)
O6ⁱⁱⁱ—Er1—C11	149.19 (7)	O6—C10—C9	122.2 (2)
O11—Er1—C10ⁱⁱⁱ	85.37 (9)	O5—C10—C9	116.7 (3)
O2ⁱ—Er1—C10ⁱⁱⁱ	69.14 (7)	O6—C10—Er1^iv	62.09 (14)
O1—Er1—C10ⁱⁱⁱ	94.05 (7)	O5—C10—Er1^iv	59.45 (13)
O10—Er1—C10ⁱⁱⁱ	102.16 (8)	C9—C10—Er1^iv	170.90 (19)
O5ⁱⁱ—Er1—C10ⁱⁱⁱ	98.49 (8)	O8—C11—O7	121.4 (2)
O8—Er1—C10ⁱⁱⁱ	165.74 (7)	O8—C11—C12	122.0 (2)
O5ⁱⁱⁱ—Er1—C10ⁱⁱⁱ	26.56 (7)	O7—C11—C12	116.5 (2)
O7—Er1—C10ⁱⁱⁱ	140.92 (7)	O8—C11—Er1	58.74 (12)
O6ⁱⁱⁱ—Er1—C10ⁱⁱⁱ	25.61 (7)	O7—C11—Er1	62.71 (12)
C11—Er1—C10ⁱⁱⁱ	167.59 (7)	C12—C11—Er1	178.07 (19)
O11—Er1—Er1ⁱ	123.86 (7)	O9—C12—C11	110.6 (2)
O2ⁱ—Er1—Er1ⁱ	70.32 (5)	O9—C12—H12B	109.5
O1—Er1—Er1ⁱ	69.30 (5)	C11—C12—H12B	109.5
O10—Er1—Er1ⁱ	153.26 (5)	O9—C12—H12A	109.5
O5ⁱⁱ—Er1—Er1ⁱ	38.24 (4)	C11—C12—H12A	109.5
O8—Er1—Er1ⁱ	120.23 (6)	H12B—C12—H12A	108.1
O5ⁱⁱⁱ—Er1—Er1ⁱ	36.66 (5)	O9—C13—C14	115.1 (2)
O7—Er1—Er1ⁱ	109.95 (5)	O9—C13—C15	124.5 (2)
O6ⁱⁱⁱ—Er1—Er1ⁱ	86.39 (6)	C14—C13—C15	120.3 (2)
C11—Er1—Er1ⁱ	118.65 (6)	C13—C14—C15^v	120.2 (2)
C10ⁱⁱⁱ—Er1—Er1ⁱ	61.18 (7)	C13—C14—H14A	119.9
C1—O1—Er1	137.57 (17)	C15^v—C14—H14A	119.9
C1—O2—Er1ⁱ	135.37 (17)	C13—C15—C14^v	119.5 (2)
C3—O3—C2	119.0 (2)	C13—C15—H15A	120.2
C6—O4—C9	116.5 (2)	C14^v—C15—H15A	120.2
C10—O5—Er1ⁱⁱ	146.22 (17)	H12D—O12—H12C	116.6
C10—O5—Er1^iv	93.99 (16)	H13D—O13—H13C	108.2
Er1ⁱⁱ—O5—Er1^iv	105.10 (7)	H14C—O14—H14D	124.5

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

Hydrogen-bond geometry (Å, º) top

D—H···A	D—H	H···A	D···A	D—H···A
O10—H10D···O7^vi	0.82	2.09	2.880 (4)	163
O10—H10C···O12	0.82	1.97	2.732 (4)	154
O11—H11D···O13	0.82	1.82	2.634 (4)	173
O11—H11C···O12	0.82	1.92	2.709 (4)	161
O12—H12D···O8^vii	0.82	2.00	2.798 (4)	167
O12—H12C···O14ⁱⁱⁱ	0.82	1.97	2.780 (4)	172
O13—H13D···O7^viii	0.82	2.12	2.872 (4)	151
O13—H13C···O3	0.82	2.03	2.804 (4)	157
O14—H14C···O6	0.82	2.17	2.874 (4)	144

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

Experimental details

Crystal data
Chemical formula	[Er₂(C₁₀H₈O₆)₃(H₂O)₄]·6H₂O
M_r	1187.17
Crystal system, space group	Triclinic, P1
Temperature (K)	298
a, b, c (Å)	8.5993 (17), 9.6356 (19), 12.689 (3)
α, β, γ (°)	102.46 (3), 95.28 (3), 106.69 (3)
V (Å³)	970.0 (4)
Z	1
Radiation type	Mo Kα
µ (mm⁻¹)	4.40
Crystal size (mm)	0.43 × 0.29 × 0.15

Data collection
Diffractometer	Rigaku R-AXIS RAPID diffractometer
Absorption correction	Multi-scan (ABSCOR; Higashi, 1995)
T_min, T_max	0.312, 0.535
No. of measured, independent and observed [I > 2σ(I)] reflections	9659, 4403, 4219
R_int	0.030
(sin θ/λ)_max (Å⁻¹)	0.649

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.019, 0.044, 1.17
No. of reflections	4403
No. of parameters	271
No. of restraints	1
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.46, −1.08

Computer programs: RAPID-AUTO (Rigaku, 1998), CrystalStructure (Rigaku/MSC, 2002), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), ORTEPII (Johnson, 1976).