Poly[[tetra-aqua-bis[μ(4)-2,2'-(p-phenyl-ene-di-oxy)diacetato][μ(2)-2,2'-(p-phenyl-ene-di-oxy)diacetato]dierbium(III)] hexa-hydrate].

The asymmetric unit of the title compound, [Er(2)(C(10)H(8)O(6))(3)(H(2)O)(4)]·6H(2)O, comprises one Er(3+) ion, one and a half 2,2'-(p-phenyl-enedi-oxy)diacetate (hqda) ligands, two coordinated water mol-ecules and three uncoordinated water mol-ecules. The Er(3+) ion is nine-coordinated by seven O atoms from hqda ligands and two O atoms from water mol-ecules. 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 Er(3+) 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-CH(2)O-C(6)H(4)-OCH(2)-COO spacers, forming two-dimensional neutral layers. Adjacent layers are linked by O-H⋯O hydrogen-bonding inter-actions, forming a three-dimensional supermolecular network.

Related literature

For general background to metal-organic frameworks, 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

Crystal data

[Er2(C10H8O6)3(H2O)4]·6H2O

M = 1187.17

Triclinic,

a = 8.5993 (17) Å

b = 9.6356 (19) Å

c = 12.689 (3) Å

α = 102.46 (3)°

β = 95.28 (3)°

γ = 106.69 (3)°

V = 970.0 (4) Å3

Z = 1

Mo Kα radiation

μ = 4.40 mm−1

T = 298 K

0.43 × 0.29 × 0.15 mm

Data collection

Rigaku R-AXIS RAPID diffractometer

Absorption correction: multi-scan (ABSCOR; Higashi, 1995 ▶) T min = 0.312, T max = 0.535

9659 measured reflections

4403 independent reflections

4219 reflections with I > 2σ(I)

R int = 0.030

Refinement

R[F 2 > 2σ(F 2)] = 0.019

wR(F 2) = 0.044

S = 1.17

4403 reflections

271 parameters

1 restraint

H-atom parameters constrained

Δρmax = 0.46 e Å−3

Δρmin = −1.08 e Å−3

Data collection: RAPID-AUTO (Rigaku, 1998 ▶); cell refinement: RAPID-AUTO; 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.

Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809046613/zl2248sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536809046613/zl2248Isup2.hkl

Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Er2(C10H8O6)3(H2O)4]·6H2O	Z = 1
Mr = 1187.17	F(000) = 584
Triclinic, P1	Dx = 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

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

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(Fo2) + (0.0129P)2 + 0.5344P] where P = (Fo2 + 2Fc2)/3
4403 reflections	(Δ/σ)max = 0.001
271 parameters	Δρmax = 0.46 e Å−3
1 restraint	Δρmin = −1.08 e Å−3

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.

	x	y	z	Uiso*/Ueq
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*

	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)

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—Er1iv	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—Er1iv	2.4684 (19)	C13—C15	1.388 (4)
O6—C10	1.237 (4)	C14—C15v	1.388 (3)
O6—Er1iv	2.529 (2)	C14—H14A	0.9300
O7—C11	1.260 (3)	C15—C14v	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—Er1iv	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—Er1iv	62.09 (14)
O1—Er1—C10iii	94.05 (7)	O5—C10—Er1iv	59.45 (13)
O10—Er1—C10iii	102.16 (8)	C9—C10—Er1iv	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—C15v	120.2 (2)
C10iii—Er1—Er1i	61.18 (7)	C13—C14—H14A	119.9
C1—O1—Er1	137.57 (17)	C15v—C14—H14A	119.9
C1—O2—Er1i	135.37 (17)	C13—C15—C14v	119.5 (2)
C3—O3—C2	119.0 (2)	C13—C15—H15A	120.2
C6—O4—C9	116.5 (2)	C14v—C15—H15A	120.2
C10—O5—Er1ii	146.22 (17)	H12D—O12—H12C	116.6
C10—O5—Er1iv	93.99 (16)	H13D—O13—H13C	108.2
Er1ii—O5—Er1iv	105.10 (7)	H14C—O14—H14D	124.5

D—H···A	D—H	H···A	D···A	D—H···A
O10—H10D···O7vi	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···O8vii	0.82	2.00	2.798 (4)	167
O12—H12C···O14iii	0.82	1.97	2.780 (4)	172
O13—H13D···O7viii	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

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O10—H10D⋯O7i	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⋯O8ii	0.82	2.00	2.798 (4)	167
O12—H12C⋯O14iii	0.82	1.97	2.780 (4)	172
O13—H13D⋯O7iv	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: (i) ; (ii) ; (iii) ; (iv) .