Poly[[bis­[penta­aqua­gadolinium(III)]-μ₄-benzene-1,2,3,4,5,6-hexa­carboxyl­ato] tetra­hydrate]

The title compound, {[Gd₂(C₁₂O₁₂)(H₂O)₁₀]·4H₂O}_n, consists of an extended network of Gd ions coordinated by the mellitate anions and water mol­ecules. In this complex, each Gd atom involves a dodeca­hedral coordination environment comprising five water mol­ecules and three O atoms from two separate mellitate anions. The center of mass of the hexa­anion [C₆(COO)₆]⁶⁻ coincides with a crystallographic inversion center.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C)= 0.007 Å
• R factor = 0.029
• wR factor = 0.083
• Data-to-parameter ratio = 14.8

checkCIF/PLATON results

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Computing details

Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2004); software used to prepare material for publication: SHELXTL.

catena-Poly[[bis[pentaaquagadolinium(III)]-µ-benzenehexacarboxylato] tetrahydrate]

Crystal data

[Gd2(C12O12)(H2O)10]·4H2O	F(000) = 872
Mr = 451.42	Dx = 2.345 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 156 reflections
a = 8.510 (1) Å	θ = 1.8–26.5°
b = 9.277 (1) Å	µ = 5.26 mm^−1
c = 16.464 (2) Å	T = 295 K
β = 100.337 (2)°	Column, colorless
V = 1278.7 (3) Å^3	0.21 × 0.12 × 0.08 mm
Z = 4

Data collection

Bruker SMART APEXII CCD area-detector diffractometer	2701 independent reflections
Radiation source: fine-focus sealed tube	2448 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.014
φ and ω scans	θmax = 26.8°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→10
Tmin = 0.479, Tmax = 0.663	k = −11→12
6721 measured reflections	l = −8→21

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.029	H-atom parameters constrained
wR(F^2) = 0.083	w = 1/[σ^2(Fo^2) + (0.0525P)^2 + 5.4257P] where P = (Fo^2 + 2Fc^2)/3
S = 1.02	(Δ/σ)max = 0.001
2701 reflections	Δρmax = 0.88 e Å^−3
182 parameters	Δρmin = −0.64 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0016 (4)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Gd	−0.05324 (2)	0.59001 (2)	0.667158 (12)	0.01995 (12)
O1	0.1852 (4)	0.5669 (4)	0.6178 (2)	0.0299 (8)
O2	0.4165 (5)	0.5717 (5)	0.7063 (2)	0.0382 (9)
C1	0.4206 (5)	0.5267 (5)	0.5654 (3)	0.0169 (8)
C2	0.3342 (5)	0.5584 (5)	0.6365 (3)	0.0207 (9)
O3	0.4905 (4)	0.8469 (4)	0.5994 (3)	0.0394 (9)
O4	0.7180 (4)	0.7444 (4)	0.6598 (2)	0.0259 (7)
C3	0.5467 (5)	0.6161 (5)	0.5529 (3)	0.0179 (8)
C4	0.5875 (5)	0.7462 (5)	0.6083 (3)	0.0211 (9)
O5	0.7522 (4)	0.7519 (4)	0.4075 (2)	0.0294 (8)
O6	0.8876 (4)	0.6851 (4)	0.5296 (2)	0.0256 (7)
C5	0.6271 (5)	0.5886 (4)	0.4872 (3)	0.0175 (8)
C6	0.7652 (5)	0.6827 (5)	0.4731 (3)	0.0192 (8)
O7	−0.0098 (7)	0.6526 (9)	0.8096 (3)	0.0224 (2)
O8	0.0840 (6)	0.3877 (7)	0.7411 (4)	0.0253 (2)
O9	0.0609 (5)	0.8275 (5)	0.6812 (3)	0.0255 (10)
O10	−0.2596 (4)	0.4643 (5)	0.7233 (2)	0.0261 (9)
O11	−0.1150 (5)	0.3868 (4)	0.5779 (2)	0.0232 (8)
O12	0.038 (3)	0.0217 (16)	0.5695 (8)	0.0248 (2)
O13	0.6993 (8)	0.1409 (8)	0.5667 (4)	0.0290 (11)
H7A	−0.0793	0.6303	0.8359	0.050*
H7B	0.0342	0.7299	0.8229	0.050*
H8A	0.0910	0.3116	0.7167	0.050*
H8B	0.0384	0.3699	0.7798	0.050*
H9A	0.1031	0.8729	0.7221	0.050*
H9B	0.1485	0.7932	0.6782	0.050*
H10A	−0.3426	0.5077	0.7254	0.050*
H10B	−0.2410	0.4019	0.7590	0.050*
H11A	−0.1722	0.3169	0.5818	0.050*
H11B	−0.0983	0.3895	0.5304	0.050*
H12A	0.0980	0.0913	0.5789	0.050*
H12B	0.0085	0.0306	0.6140	0.050*
H13A	0.6451	0.1400	0.5202	0.050*
H13B	0.7617	0.0794	0.5559	0.050*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Gd	0.01159 (15)	0.03111 (17)	0.01736 (16)	−0.00075 (8)	0.00315 (9)	0.00214 (8)
O1	0.0154 (16)	0.043 (2)	0.0335 (19)	0.0004 (14)	0.0121 (14)	−0.0032 (15)
O2	0.031 (2)	0.064 (3)	0.0192 (17)	−0.0048 (17)	0.0043 (15)	−0.0066 (16)
C1	0.0110 (18)	0.023 (2)	0.0175 (19)	0.0024 (15)	0.0030 (14)	0.0003 (16)
C2	0.018 (2)	0.022 (2)	0.022 (2)	−0.0028 (17)	0.0069 (17)	−0.0015 (17)
O3	0.032 (2)	0.034 (2)	0.046 (2)	0.0121 (16)	−0.0065 (16)	−0.0157 (18)
O4	0.0181 (15)	0.0292 (17)	0.0274 (16)	−0.0006 (12)	−0.0015 (12)	−0.0093 (13)
C3	0.0119 (18)	0.024 (2)	0.017 (2)	0.0016 (15)	0.0004 (15)	−0.0005 (16)
C4	0.018 (2)	0.025 (2)	0.021 (2)	0.0009 (17)	0.0058 (16)	−0.0034 (17)
O5	0.0229 (16)	0.0368 (19)	0.0268 (17)	−0.0047 (14)	0.0009 (13)	0.0098 (15)
O6	0.0165 (15)	0.0372 (18)	0.0218 (16)	−0.0098 (13)	−0.0008 (12)	0.0041 (13)
C5	0.0119 (19)	0.022 (2)	0.018 (2)	0.0000 (14)	0.0021 (16)	0.0017 (15)
C6	0.0141 (19)	0.024 (2)	0.020 (2)	−0.0013 (16)	0.0027 (16)	−0.0012 (16)
O7	0.0241 (3)	0.033 (7)	0.0237 (17)	0.0058 (4)	0.0004 (13)	−0.0052 (3)
O8	0.0237 (3)	0.024 (4)	0.021 (5)	0.011 (4)	0.006 (3)	−0.001 (4)
O9	0.036 (2)	0.045 (2)	0.059 (3)	−0.0135 (18)	0.0100 (19)	−0.024 (2)
O10	0.0190 (16)	0.048 (2)	0.042 (2)	−0.0006 (16)	0.0081 (15)	0.0226 (18)
O11	0.033 (2)	0.0345 (19)	0.035 (2)	−0.0052 (15)	0.0122 (16)	−0.0033 (15)
O12	0.0216 (5)	0.0214 (14)	0.0127 (12)	−0.0058 (12)	−0.0021 (2)	−0.0015 (11)
O13	0.0211 (16)	0.027 (4)	0.0217 (4)	−0.0091 (4)	0.0005 (3)	−0.0032 (4)

Geometric parameters (Å, º)

Gd—O1	2.327 (3)	O6—C6	1.267 (5)
Gd—O4^i	2.402 (3)	C5—C1^ii	1.391 (6)
Gd—O6^i	2.398 (3)	C5—C6	1.515 (6)
Gd—O7	2.380 (5)	O7—H7A	0.820
Gd—O8	2.421 (5)	O7—H7B	0.820
Gd—O9	2.402 (4)	O8—H8A	0.820
Gd—O10	2.425 (3)	O8—H8B	0.820
Gd—O11	2.391 (4)	O9—H9A	0.820
O1—C2	1.252 (6)	O9—H9B	0.820
O2—C2	1.240 (6)	O10—H10B	0.820
C1—C5^ii	1.391 (6)	O10—H10A	0.820
C1—C3	1.400 (6)	O11—H11B	0.820
C1—C2	1.519 (6)	O11—H11A	0.820
O3—C4	1.238 (6)	O12—H12A	0.820
O4—C4	1.270 (5)	O12—H12B	0.820
C3—C5	1.403 (6)	O13—H13B	0.820
C3—C4	1.515 (6)	O13—H13A	0.820
O5—C6	1.243 (5)
O1—Gd—O7	112.05 (16)	C5^ii—C1—C2	120.1 (4)
O1—Gd—O11	79.75 (13)	C3—C1—C2	119.2 (4)
O7—Gd—O11	140.9 (2)	O2—C2—O1	126.9 (4)
O1—Gd—O6^i	75.69 (12)	O2—C2—C1	117.5 (4)
O7—Gd—O6^i	144.1 (2)	O1—C2—C1	115.6 (4)
O11—Gd—O6^i	73.95 (13)	C4—O4—Gd^iii	130.2 (3)
O1—Gd—O9	75.83 (14)	C1—C3—C5	119.9 (4)
O7—Gd—O9	72.1 (2)	C1—C3—C4	118.9 (4)
O11—Gd—O9	145.40 (14)	C5—C3—C4	121.2 (4)
O6^i—Gd—O9	76.51 (14)	O3—C4—O4	125.0 (4)
O1—Gd—O4^i	141.90 (12)	O3—C4—C3	117.0 (4)
O7—Gd—O4^i	83.4 (2)	O4—C4—C3	118.0 (4)
O11—Gd—O4^i	110.63 (12)	C6—O6—Gd^iii	133.9 (3)
O6^i—Gd—O4^i	72.67 (12)	C1^ii—C5—C3	119.5 (4)
O9—Gd—O4^i	76.61 (13)	C1^ii—C5—C6	119.7 (4)
O1—Gd—O8	74.44 (17)	C3—C5—C6	120.9 (4)
O7—Gd—O8	73.6 (3)	O5—C6—O6	124.2 (4)
O11—Gd—O8	74.4 (2)	O5—C6—C5	118.7 (4)
O6^i—Gd—O8	139.5 (2)	O6—C6—C5	117.1 (4)
O9—Gd—O8	120.81 (19)	Gd—O7—H7A	117.4
O4^i—Gd—O8	143.25 (17)	Gd—O7—H7B	117.3
O1—Gd—O10	145.60 (13)	H7A—O7—H7B	114.7
O7—Gd—O10	74.76 (16)	Gd—O8—H8A	119.5
O11—Gd—O10	76.14 (14)	Gd—O8—H8B	107.1
O6^i—Gd—O10	119.53 (11)	H8A—O8—H8B	107.1
O9—Gd—O10	135.44 (15)	Gd—O9—H9A	131.4
O4^i—Gd—O10	70.75 (12)	Gd—O9—H9B	89.8
O8—Gd—O10	75.67 (15)	H9A—O9—H9B	88.8
O1—Gd—H9B	58.1	Gd—O10—H10B	123.6
O7—Gd—H9B	76.4	Gd—O10—H10A	117.9
O11—Gd—H9B	134.6	H10B—O10—H10A	111.9
C2—O1—Gd	145.9 (3)	Gd—O11—H11B	120.3
C5^ii—C1—C3	120.7 (4)	Gd—O11—H11A	130.0
O7—Gd—O1—C2	11.7 (6)	Gd^iii—O4—C4—O3	−164.5 (4)
O11—Gd—O1—C2	−129.4 (6)	Gd^iii—O4—C4—C3	15.2 (6)
O6^i—Gd—O1—C2	154.7 (6)	C1—C3—C4—O3	−70.0 (6)
O9—Gd—O1—C2	75.3 (6)	C5—C3—C4—O3	106.6 (5)
O4^i—Gd—O1—C2	120.2 (5)	C1—C3—C4—O4	110.4 (5)
O8—Gd—O1—C2	−52.9 (6)	C5—C3—C4—O4	−73.1 (6)
O10—Gd—O1—C2	−83.4 (6)	C1—C3—C5—C1^ii	0.6 (7)
Gd—O1—C2—O2	−5.7 (9)	C4—C3—C5—C1^ii	−175.9 (4)
Gd—O1—C2—C1	173.4 (4)	C1—C3—C5—C6	−179.3 (4)
C5^ii—C1—C2—O2	128.3 (5)	C4—C3—C5—C6	4.2 (6)
C3—C1—C2—O2	−52.7 (6)	Gd^iii—O6—C6—O5	172.3 (3)
C5^ii—C1—C2—O1	−51.0 (6)	Gd^iii—O6—C6—C5	−7.8 (6)
C3—C1—C2—O1	128.0 (4)	C1^ii—C5—C6—O5	62.5 (6)
C5^ii—C1—C3—C5	−0.6 (7)	C3—C5—C6—O5	−117.6 (5)
C2—C1—C3—C5	−179.6 (4)	C1^ii—C5—C6—O6	−117.4 (5)
C5^ii—C1—C3—C4	176.0 (4)	C3—C5—C6—O6	62.5 (6)
C2—C1—C3—C4	−3.0 (6)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O7—H7A···O13^iv	0.82	2.05	2.818 (8)	155
O8—H8B···O3^v	0.82	2.06	2.835 (4)	158
O9—H9A···O2^iv	0.82	2.21	2.911 (3)	143
O10—H10A···O2^i	0.82	2.10	2.897 (3)	163
O10—H10B···O4^v	0.82	1.97	2.783 (5)	174
O11—H11A···O13^i	0.82	1.96	2.762 (7)	167
O11—H11B···O1^vi	0.82	2.45	3.199 (5)	152
O12—H12A···O5^ii	0.82	1.92	2.74 (1)	175
O13—H13A···O3^ii	0.82	2.10	2.919 (4)	176
O13—H13B···O12^iii	0.82	2.38	3.08 (2)	143

Symmetry codes: (i) x−1, y, z; (ii) −x+1, −y+1, −z+1; (iii) x+1, y, z; (iv) −x+1/2, y+1/2, −z+3/2; (v) −x+1/2, y−1/2, −z+3/2; (vi) −x, −y+1, −z+1.