Poly[bis(μ₄-1,4-benzene­dicarboxyl­ato)(μ₆-succinato)digadolinium(III)]

A new three-dimensional coordination polymer with the formula [Gd₂(C₈H₄O₄)₂(C₄H₄O₄)]_n has been synthesized by hydro­thermal synthesis. The coordination polyhedron around each Gd atom is a distorted square antiprism; the antiprisms are bridged into a three-dimensional network by the 1,4-benzene­dicarboxyl­ate and succinate ligands. The succinate ion is located on a centre of inversion.

Key indicators

• Single-crystal X-ray study
• T = 291 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.017
• wR factor = 0.044
• Data-to-parameter ratio = 16.1

checkCIF/PLATON results

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Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............       2.00 Ratio

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

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

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Computing details

Data collection: SMART (Bruker, 1998); cell refinement: SMART; data reduction: SAINT (Bruker, 1998); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 1998); software used to prepare material for publication: SHELXTL.

Poly[(µ₆-1,4-benzenedicarboxylato)hemi(µ₆-succinato)gadolinium(III)]

Crystal data

[Gd2(C8H4O4)2(C4H4O4)]	F(000) = 1424
Mr = 758.80	Dx = 2.425 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 128 reflections
a = 13.9094 (9) Å	θ = 3.3–26.7°
b = 6.8497 (5) Å	µ = 6.40 mm^−1
c = 21.8148 (14) Å	T = 291 K
V = 2078.4 (2) Å^3	Column, colourless
Z = 4	0.17 × 0.15 × 0.08 mm

Data collection

Bruker SMART CCD area-detector diffractometer	2491 independent reflections
Radiation source: fine-focus sealed tube	2303 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.024
φ and ω scans	θmax = 28.0°, θmin = 1.9°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→18
Tmin = 0.344, Tmax = 0.605	k = −9→9
11172 measured reflections	l = −28→27

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)] = 0.017	H-atom parameters constrained
wR(F^2) = 0.044	w = 1/[σ^2(Fo^2) + (0.0233P)^2 + 2.0093P] where P = (Fo^2 + 2Fc^2)/3
S = 1.06	(Δ/σ)max = 0.004
2491 reflections	Δρmax = 0.83 e Å^−3
155 parameters	Δρmin = −1.29 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: 0.00185 (9)

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	0.668579 (7)	1.018944 (17)	0.445098 (5)	0.01219 (6)
O1	0.63763 (14)	1.0395 (3)	0.54989 (7)	0.0203 (4)
O2	0.49125 (11)	0.9254 (3)	0.56752 (7)	0.0210 (3)
C1	0.57532 (16)	0.9673 (3)	0.58438 (9)	0.0146 (4)
C2	0.60219 (16)	0.9255 (3)	0.64988 (9)	0.0181 (4)
C3	0.6938 (2)	0.9715 (4)	0.67113 (12)	0.0259 (5)
H3A	0.7385	1.0279	0.6448	0.031*
C4	0.71870 (19)	0.9335 (4)	0.73139 (11)	0.0275 (5)
H4A	0.7799	0.9647	0.7455	0.033*
C5	0.65238 (17)	0.8490 (4)	0.77075 (10)	0.0215 (5)
C6	0.68016 (17)	0.7996 (3)	0.83575 (10)	0.0219 (5)
C7	0.56094 (19)	0.8020 (4)	0.74966 (11)	0.0277 (5)
H7A	0.5166	0.7448	0.7760	0.033*
C8	0.53602 (18)	0.8402 (4)	0.68954 (10)	0.0262 (5)
H8A	0.4748	0.8087	0.6755	0.031*
O3	0.75919 (13)	0.8626 (3)	0.85568 (7)	0.0285 (4)
O4	0.62256 (13)	0.6967 (3)	0.86624 (7)	0.0292 (4)
O5	0.83402 (11)	0.8733 (3)	0.45344 (8)	0.0226 (4)
O6	0.82508 (11)	1.1769 (2)	0.48268 (8)	0.0201 (3)
C9	0.87523 (18)	1.0307 (3)	0.46824 (12)	0.0209 (5)
C10	0.98359 (19)	1.0427 (4)	0.46936 (12)	0.0261 (5)
H10A	1.0043	1.1774	0.4657	0.031*
H10B	1.0107	0.9687	0.4356	0.031*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Gd	0.01210 (8)	0.01453 (8)	0.00995 (8)	0.00041 (3)	0.00000 (3)	−0.00111 (3)
O1	0.0212 (9)	0.0291 (10)	0.0107 (8)	−0.0027 (7)	0.0011 (6)	0.0004 (6)
O2	0.0155 (8)	0.0322 (9)	0.0152 (7)	0.0019 (7)	−0.0037 (6)	0.0013 (7)
C1	0.0157 (10)	0.0159 (10)	0.0123 (10)	0.0031 (8)	−0.0008 (8)	−0.0012 (7)
C2	0.0210 (11)	0.0208 (10)	0.0124 (9)	−0.0005 (9)	−0.0026 (8)	0.0023 (8)
C3	0.0244 (13)	0.0341 (14)	0.0192 (12)	−0.0092 (10)	−0.0043 (11)	0.0072 (9)
C4	0.0261 (13)	0.0369 (14)	0.0196 (11)	−0.0090 (11)	−0.0106 (10)	0.0043 (10)
C5	0.0288 (12)	0.0228 (11)	0.0129 (10)	−0.0006 (9)	−0.0065 (9)	0.0037 (8)
C6	0.0300 (12)	0.0211 (11)	0.0145 (11)	0.0044 (9)	−0.0064 (9)	0.0012 (8)
C7	0.0273 (12)	0.0382 (15)	0.0176 (11)	−0.0052 (11)	−0.0027 (9)	0.0097 (10)
C8	0.0217 (11)	0.0395 (15)	0.0175 (11)	−0.0066 (10)	−0.0037 (9)	0.0083 (10)
O3	0.0316 (10)	0.0388 (11)	0.0150 (7)	0.0003 (8)	−0.0078 (7)	−0.0027 (7)
O4	0.0385 (10)	0.0309 (10)	0.0184 (8)	−0.0029 (8)	−0.0066 (7)	0.0102 (7)
O5	0.0177 (9)	0.0155 (8)	0.0346 (10)	−0.0005 (6)	−0.0062 (7)	−0.0014 (7)
O6	0.0197 (8)	0.0171 (8)	0.0234 (8)	0.0011 (6)	−0.0017 (6)	−0.0015 (6)
C9	0.0192 (12)	0.0189 (11)	0.0248 (13)	0.0005 (9)	−0.0055 (10)	0.0008 (8)
C10	0.0230 (13)	0.0261 (12)	0.0290 (14)	−0.0031 (10)	−0.0029 (10)	0.0037 (10)

Geometric parameters (Å, º)

Gd—O2^i	2.2723 (16)	C4—C5	1.387 (3)
Gd—O1	2.3305 (15)	C4—H4A	0.9300
Gd—O3^ii	2.3394 (16)	C5—C7	1.390 (3)
Gd—O4^iii	2.3560 (16)	C5—C6	1.508 (3)
Gd—O5^iv	2.4341 (19)	C6—O4	1.257 (3)
Gd—O6^v	2.4837 (17)	C6—O3	1.258 (3)
Gd—O5	2.5148 (16)	C7—C8	1.382 (3)
Gd—O6	2.5654 (16)	C7—H7A	0.9300
Gd—C9	2.920 (3)	C8—H8A	0.9300
O1—C1	1.250 (3)	O5—C9	1.263 (3)
O2—C1	1.259 (3)	O6—C9	1.260 (3)
C1—C2	1.504 (3)	C9—C10	1.510 (4)
C2—C8	1.392 (3)	C10—C10^vi	1.529 (5)
C2—C3	1.393 (3)	C10—H10A	0.9700
C3—C4	1.384 (3)	C10—H10B	0.9700
C3—H3A	0.9300
O2^i—Gd—O1	85.87 (6)	C8—C2—C3	119.6 (2)
O2^i—Gd—O3^ii	105.13 (6)	C8—C2—C1	120.4 (2)
O1—Gd—O3^ii	151.20 (7)	C3—C2—C1	120.0 (2)
O2^i—Gd—O4^iii	75.58 (6)	C4—C3—C2	120.2 (2)
O1—Gd—O4^iii	134.74 (7)	C4—C3—H3A	119.9
O3^ii—Gd—O4^iii	74.06 (7)	C2—C3—H3A	119.9
O2^i—Gd—O5^iv	80.04 (6)	C3—C4—C5	120.0 (2)
O1—Gd—O5^iv	82.17 (6)	C3—C4—H4A	120.0
O3^ii—Gd—O5^iv	73.91 (6)	C5—C4—H4A	120.0
O4^iii—Gd—O5^iv	132.50 (6)	C4—C5—C7	120.0 (2)
O2^i—Gd—O6^v	103.48 (6)	C4—C5—C6	120.4 (2)
O1—Gd—O6^v	74.91 (6)	C7—C5—C6	119.6 (2)
O3^ii—Gd—O6^v	125.95 (6)	O4—C6—O3	124.5 (2)
O4^iii—Gd—O6^v	70.08 (6)	O4—C6—C5	117.4 (2)
O5^iv—Gd—O6^v	156.41 (5)	O3—C6—C5	118.1 (2)
O2^i—Gd—O5	166.08 (6)	C8—C7—C5	120.0 (2)
O1—Gd—O5	97.00 (6)	C8—C7—H7A	120.0
O3^ii—Gd—O5	78.75 (6)	C5—C7—H7A	120.0
O4^iii—Gd—O5	93.02 (6)	C7—C8—C2	120.2 (2)
O5^iv—Gd—O5	113.82 (5)	C7—C8—H8A	119.9
O6^v—Gd—O5	64.49 (5)	C2—C8—H8A	119.9
O2^i—Gd—O6	142.94 (6)	C6—O3—Gd^vii	141.46 (15)
O1—Gd—O6	79.50 (6)	C6—O4—Gd^viii	124.38 (15)
O3^ii—Gd—O6	75.86 (6)	C9—O5—Gd^v	151.29 (16)
O4^iii—Gd—O6	136.74 (6)	C9—O5—Gd	95.45 (15)
O5^iv—Gd—O6	64.42 (5)	Gd^v—O5—Gd	112.13 (6)
O6^v—Gd—O6	105.20 (5)	C9—O6—Gd^iv	130.34 (15)
O5—Gd—O6	50.79 (6)	C9—O6—Gd	93.13 (14)
O2^i—Gd—C9	168.39 (6)	Gd^iv—O6—Gd	108.81 (6)
O1—Gd—C9	90.61 (7)	O6—C9—O5	119.4 (2)
O3^ii—Gd—C9	73.25 (7)	O6—C9—C10	120.4 (2)
O4^iii—Gd—C9	114.27 (7)	O5—C9—C10	120.2 (2)
O5^iv—Gd—C9	88.52 (6)	O6—C9—Gd	61.33 (12)
O6^v—Gd—C9	86.22 (6)	O5—C9—Gd	59.03 (12)
O5—Gd—C9	25.51 (6)	C10—C9—Gd	170.85 (18)
O6—Gd—C9	25.54 (6)	C9—C10—C10^vi	106.9 (3)
C1—O1—Gd	134.01 (15)	C9—C10—H10A	110.3
C1—O2—Gd^i	154.92 (16)	C10^vi—C10—H10A	110.3
O1—C1—O2	124.0 (2)	C9—C10—H10B	110.3
O1—C1—C2	118.3 (2)	C10^vi—C10—H10B	110.3
O2—C1—C2	117.70 (19)	H10A—C10—H10B	108.6

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