Poly[μ-aqua-aqua-(μ-benzene-1,2,4,5-tetra-carboxyl-ato)gadolinate(III)potassium(I)].

In the title compound, [KGd(C(10)H(2)O(8))(H(2)O)(2)](n), the Gd(3+) ion is nine-coordinated by eight O atoms from five individual benzene-1,2,4,5-tetra-carboxyl-ate (btec) ligands and one water mol-ecule, and the K(+) ion is eight-coordinated by six O atoms from five individual btec ligands and two water mol-ecules. In the crystal, the btec half-mol-ecules are completed by crystallographic inversion symmetry. GdO(9) and KO(8) polyhedra are connected, forming layers in the ab plane, which are further inter-connected by μ(8)- or μ(12)-bridging btec ligands, forming a three-dimensional structure.

Related literature

For structures based on H4btec ligand, see: Huang et al. (2009 ▶); Lu et al. (2005 ▶); Wu et al. (2001 ▶); Zhang et al. (2005 ▶). For the isotypic neodymium(III) compound, see: Dai et al. (2008 ▶).

Experimental

Crystal data

[KGd(C10H2O8)(H2O)2]

M = 482.50

Monoclinic,

a = 8.9003 (1) Å

b = 7.7816 (1) Å

c = 17.5150 (3) Å

β = 91.857 (1)°

V = 1212.43 (3) Å3

Z = 4

Mo Kα radiation

μ = 5.87 mm−1

T = 296 K

0.20 × 0.10 × 0.10 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer

Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.386, T max = 0.591

14043 measured reflections

3002 independent reflections

2588 reflections with I > 2σ(I)

R int = 0.037

Refinement

R[F 2 > 2σ(F 2)] = 0.024

wR(F 2) = 0.051

S = 1.04

3002 reflections

199 parameters

H-atom parameters constrained

Δρmax = 0.91 e Å−3

Δρmin = −1.29 e Å−3

Data collection: APEX2 (Bruker, 2008 ▶); cell refinement: SAINT (Bruker, 2008 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: SHELXTL (Sheldrick, 2008 ▶); software used to prepare material for publication: SHELXL97.

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536811016254/si2351sup1.cif

Structure factors: contains datablocks I. DOI: 10.1107/S1600536811016254/si2351Isup2.hkl

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

[KGd(C10H2O8)(H2O)2]	F(000) = 916
Mr = 482.50	Dx = 2.643 Mg m−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 2537 reflections
a = 8.9003 (1) Å	θ = 2.3–25.1°
b = 7.7816 (1) Å	µ = 5.87 mm−1
c = 17.5150 (3) Å	T = 296 K
β = 91.857 (1)°	Prism, colourless
V = 1212.43 (3) Å3	0.20 × 0.10 × 0.10 mm
Z = 4

Bruker SMART APEXII CCD area-detector diffractometer	3002 independent reflections
Radiation source: fine-focus sealed tube	2588 reflections with I > 2σ(I)
graphite	Rint = 0.037
Detector resolution: 83.33 pixels mm-1	θmax = 28.3°, θmin = 2.3°
ω scans	h = −11→11
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	k = −10→9
Tmin = 0.386, Tmax = 0.591	l = −23→23
14043 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)] = 0.024	Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.051	H-atom parameters constrained
S = 1.04	w = 1/[σ2(Fo2) + (0.0208P)2 + 1.8584P] where P = (Fo2 + 2Fc2)/3
3002 reflections	(Δ/σ)max = 0.002
199 parameters	Δρmax = 0.91 e Å−3
0 restraints	Δρmin = −1.29 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
Gd1	0.21753 (2)	0.47536 (2)	0.699264 (9)	0.00997 (6)
K1	0.22962 (11)	0.97212 (11)	0.78942 (5)	0.02529 (19)
O1	0.4699 (3)	0.5723 (3)	0.66830 (15)	0.0226 (6)
H1A	0.5081	0.6065	0.7107	0.027*
H1B	0.4533	0.6604	0.6406	0.027*
C1	0.3791 (4)	0.5106 (4)	0.8437 (2)	0.0147 (7)
O2	0.3319 (3)	0.6478 (3)	0.81457 (14)	0.0183 (6)
C2	0.4485 (4)	0.5076 (4)	0.92329 (19)	0.0128 (7)
O3	0.3601 (3)	0.3676 (3)	0.81063 (14)	0.0210 (6)
C3	0.3828 (4)	0.3974 (4)	0.97488 (18)	0.0142 (7)
H3	0.3041	0.3270	0.9581	0.017*
O4	0.6594 (3)	0.6935 (3)	0.82750 (13)	0.0180 (6)
C4	0.5683 (4)	0.6106 (4)	0.94877 (18)	0.0128 (7)
O5	0.7106 (3)	0.8636 (3)	0.92519 (13)	0.0173 (6)
C5	0.6512 (4)	0.7290 (4)	0.89702 (19)	0.0139 (7)
O6	−0.0404 (3)	1.0020 (3)	0.70586 (14)	0.0163 (5)
C6	0.0794 (4)	0.7479 (4)	0.61673 (19)	0.0129 (7)
O7	0.0284 (3)	1.2656 (3)	0.67405 (14)	0.0168 (5)
C7	0.0324 (4)	0.8804 (4)	0.55820 (18)	0.0105 (7)
O8	0.1973 (3)	0.7726 (3)	0.65718 (14)	0.0189 (6)
C8	0.0245 (4)	0.8287 (4)	0.48207 (18)	0.0118 (7)
H8	0.0403	0.7138	0.4700	0.014*
O9	0.0079 (3)	0.6102 (3)	0.61982 (15)	0.0236 (6)
C9	0.0067 (4)	1.0533 (4)	0.57629 (19)	0.0121 (7)
C10	−0.0015 (4)	1.1124 (4)	0.65777 (18)	0.0107 (7)
H10A	0.3331	1.0155	0.9851	0.013*
H10B	0.4337	0.9339	0.9384	0.013*
O10	0.3392 (4)	0.9561 (4)	0.94345 (18)	0.0398 (8)

	U11	U22	U33	U12	U13	U23
Gd1	0.01314 (10)	0.00955 (8)	0.00718 (8)	0.00160 (7)	−0.00007 (6)	−0.00017 (6)
K1	0.0245 (5)	0.0240 (4)	0.0270 (5)	−0.0026 (4)	−0.0061 (4)	0.0027 (3)
O1	0.0190 (15)	0.0213 (13)	0.0278 (15)	−0.0025 (11)	0.0022 (12)	−0.0034 (11)
C1	0.0161 (19)	0.0175 (17)	0.0104 (16)	0.0008 (14)	0.0006 (14)	0.0011 (13)
O2	0.0226 (15)	0.0168 (13)	0.0153 (13)	−0.0012 (11)	−0.0046 (11)	0.0045 (10)
C2	0.0161 (19)	0.0125 (16)	0.0096 (16)	0.0008 (13)	−0.0010 (13)	0.0008 (12)
O3	0.0335 (17)	0.0156 (12)	0.0133 (13)	0.0060 (11)	−0.0071 (12)	−0.0033 (10)
C3	0.0158 (19)	0.0157 (17)	0.0111 (16)	−0.0033 (14)	−0.0003 (14)	0.0000 (13)
O4	0.0225 (15)	0.0206 (13)	0.0109 (12)	−0.0066 (11)	0.0026 (11)	0.0019 (10)
C4	0.0151 (19)	0.0140 (17)	0.0092 (16)	0.0013 (14)	0.0001 (14)	0.0018 (13)
O5	0.0225 (15)	0.0175 (12)	0.0121 (12)	−0.0048 (11)	0.0011 (11)	0.0015 (10)
C5	0.0122 (18)	0.0161 (17)	0.0134 (17)	0.0005 (14)	0.0003 (14)	0.0050 (13)
O6	0.0220 (14)	0.0159 (13)	0.0111 (12)	0.0023 (10)	0.0044 (10)	0.0046 (9)
C6	0.020 (2)	0.0116 (16)	0.0075 (15)	0.0030 (14)	0.0051 (14)	−0.0011 (12)
O7	0.0199 (15)	0.0144 (12)	0.0161 (13)	−0.0036 (10)	0.0023 (11)	−0.0040 (10)
C7	0.0137 (18)	0.0095 (15)	0.0083 (15)	−0.0020 (13)	0.0009 (13)	0.0015 (12)
O8	0.0193 (15)	0.0172 (13)	0.0199 (14)	0.0003 (11)	−0.0055 (11)	0.0045 (10)
C8	0.0151 (19)	0.0109 (16)	0.0096 (16)	0.0013 (13)	0.0026 (13)	−0.0005 (12)
O9	0.0280 (17)	0.0165 (13)	0.0255 (15)	−0.0050 (11)	−0.0090 (12)	0.0082 (11)
C9	0.0133 (18)	0.0117 (16)	0.0112 (16)	−0.0010 (13)	−0.0001 (13)	0.0004 (12)
C10	0.0106 (18)	0.0124 (16)	0.0090 (15)	0.0034 (13)	0.0008 (13)	0.0010 (12)
O10	0.045 (2)	0.046 (2)	0.0290 (17)	−0.0029 (16)	0.0128 (15)	−0.0107 (14)

Gd1—O6i	2.337 (3)	C2—C4	1.396 (5)
Gd1—O7ii	2.376 (2)	O3—K1ii	3.306 (3)
Gd1—O8	2.433 (2)	C3—C4vii	1.394 (4)
Gd1—O3	2.441 (2)	C3—H3	0.9300
Gd1—O1	2.447 (3)	O4—C5	1.253 (4)
Gd1—O5iii	2.451 (2)	O4—Gd1iv	2.503 (2)
Gd1—O4iii	2.503 (2)	O4—K1iii	2.875 (3)
Gd1—O9	2.520 (3)	C4—C3vii	1.394 (4)
Gd1—O2	2.604 (2)	C4—C5	1.502 (5)
Gd1—C6	2.825 (3)	O5—C5	1.266 (4)
Gd1—C5iii	2.831 (3)	O5—Gd1iv	2.451 (2)
Gd1—C1	2.882 (3)	C5—Gd1iv	2.831 (3)
K1—O2	2.714 (3)	O6—C10	1.259 (4)
K1—O6	2.783 (3)	O6—Gd1v	2.337 (3)
K1—O8	2.795 (3)	C6—O9	1.249 (4)
K1—O10	2.842 (3)	C6—O8	1.261 (4)
K1—O1iv	2.860 (3)	C6—C7	1.504 (4)
K1—O4iv	2.875 (3)	O7—C10	1.253 (4)
K1—O7i	2.891 (3)	O7—Gd1vi	2.376 (2)
K1—O9v	2.893 (3)	O7—K1v	2.891 (3)
K1—C10	3.230 (3)	C7—C8	1.392 (4)
K1—O3vi	3.306 (3)	C7—C9	1.402 (5)
K1—Gd1v	3.9912 (10)	C8—C9viii	1.396 (4)
O1—K1iii	2.860 (3)	C8—H8	0.9300
O1—H1A	0.8501	O9—K1i	2.893 (3)
O1—H1B	0.8500	C9—C8viii	1.396 (4)
C1—O2	1.250 (4)	C9—C10	1.503 (4)
C1—O3	1.263 (4)	O10—H10A	0.8671
C1—C2	1.506 (4)	O10—H10B	0.8656
C2—C3	1.388 (5)
O6i—Gd1—O7ii	72.72 (8)	O6—K1—O3vi	105.99 (7)
O6i—Gd1—O8	94.93 (9)	O8—K1—O3vi	129.52 (7)
O7ii—Gd1—O8	123.50 (8)	O10—K1—O3vi	79.96 (8)
O6i—Gd1—O3	78.90 (9)	O1iv—K1—O3vi	52.77 (7)
O7ii—Gd1—O3	105.04 (9)	O4iv—K1—O3vi	52.76 (7)
O8—Gd1—O3	126.89 (8)	O7i—K1—O3vi	140.46 (8)
O6i—Gd1—O1	140.86 (9)	O9v—K1—O3vi	81.54 (7)
O7ii—Gd1—O1	145.14 (9)	C10—K1—O3vi	88.80 (7)
O8—Gd1—O1	72.49 (9)	O2—K1—Gd1v	109.12 (6)
O3—Gd1—O1	79.97 (9)	O6—K1—Gd1v	34.92 (5)
O6i—Gd1—O5iii	149.95 (9)	O8—K1—Gd1v	88.21 (6)
O7ii—Gd1—O5iii	78.16 (8)	O10—K1—Gd1v	105.38 (8)
O8—Gd1—O5iii	94.98 (8)	O1iv—K1—Gd1v	155.64 (6)
O3—Gd1—O5iii	116.41 (8)	O4iv—K1—Gd1v	113.43 (6)
O1—Gd1—O5iii	69.16 (9)	O7i—K1—Gd1v	36.12 (5)
O6i—Gd1—O4iii	121.37 (8)	O9v—K1—Gd1v	38.99 (5)
O7ii—Gd1—O4iii	71.02 (8)	C10—K1—Gd1v	54.57 (6)
O8—Gd1—O4iii	143.63 (9)	O3vi—K1—Gd1v	109.62 (5)
O3—Gd1—O4iii	68.24 (8)	O2—K1—Gd1	37.34 (5)
O1—Gd1—O4iii	79.53 (9)	O6—K1—Gd1	82.38 (5)
O5iii—Gd1—O4iii	52.70 (8)	O8—K1—Gd1	34.09 (5)
O6i—Gd1—O9	81.44 (9)	O10—K1—Gd1	108.80 (7)
O7ii—Gd1—O9	71.09 (8)	O1iv—K1—Gd1	111.26 (6)
O8—Gd1—O9	52.45 (8)	O4iv—K1—Gd1	106.89 (5)
O3—Gd1—O9	160.19 (9)	O7i—K1—Gd1	63.78 (5)
O1—Gd1—O9	114.70 (9)	O9v—K1—Gd1	122.78 (6)
O5iii—Gd1—O9	82.34 (9)	C10—K1—Gd1	92.00 (6)
O4iii—Gd1—O9	125.60 (8)	O3vi—K1—Gd1	155.35 (6)
O6i—Gd1—O2	70.03 (8)	Gd1v—K1—Gd1	90.638 (18)
O7ii—Gd1—O2	139.01 (8)	Gd1—O1—K1iii	135.72 (11)
O8—Gd1—O2	76.60 (8)	Gd1—O1—H1A	104.3
O3—Gd1—O2	51.49 (8)	K1iii—O1—H1A	61.0
O1—Gd1—O2	71.01 (9)	Gd1—O1—H1B	103.4
O5iii—Gd1—O2	139.97 (9)	K1iii—O1—H1B	120.7
O4iii—Gd1—O2	115.76 (8)	H1A—O1—H1B	107.7
O9—Gd1—O2	118.52 (8)	O2—C1—O3	121.8 (3)
O6i—Gd1—C6	90.28 (9)	O2—C1—C2	120.9 (3)
O7ii—Gd1—C6	97.28 (10)	O3—C1—C2	117.1 (3)
O8—Gd1—C6	26.43 (9)	O2—C1—Gd1	64.62 (18)
O3—Gd1—C6	150.81 (9)	O3—C1—Gd1	57.19 (17)
O1—Gd1—C6	92.43 (10)	C2—C1—Gd1	171.3 (2)
O5iii—Gd1—C6	86.17 (9)	C1—O2—Gd1	89.7 (2)
O4iii—Gd1—C6	138.40 (8)	C1—O2—K1	165.2 (2)
O9—Gd1—C6	26.23 (9)	Gd1—O2—K1	103.46 (8)
O2—Gd1—C6	99.35 (8)	C3—C2—C4	118.7 (3)
O6i—Gd1—C5iii	141.71 (9)	C3—C2—C1	116.3 (3)
O7ii—Gd1—C5iii	74.19 (9)	C4—C2—C1	125.0 (3)
O8—Gd1—C5iii	119.44 (10)	C1—O3—Gd1	97.0 (2)
O3—Gd1—C5iii	91.69 (9)	C1—O3—K1ii	155.9 (2)
O1—Gd1—C5iii	71.17 (9)	Gd1—O3—K1ii	93.34 (8)
O5iii—Gd1—C5iii	26.51 (9)	C2—C3—C4vii	121.8 (3)
O4iii—Gd1—C5iii	26.26 (9)	C2—C3—H3	119.1
O9—Gd1—C5iii	105.40 (9)	C4vii—C3—H3	119.1
O2—Gd1—C5iii	130.73 (9)	C5—O4—Gd1iv	91.6 (2)
C6—Gd1—C5iii	112.63 (10)	C5—O4—K1iii	148.9 (2)
O6i—Gd1—C1	72.32 (10)	Gd1iv—O4—K1iii	103.25 (9)
O7ii—Gd1—C1	123.98 (9)	C3vii—C4—C2	119.5 (3)
O8—Gd1—C1	101.85 (9)	C3vii—C4—C5	117.5 (3)
O3—Gd1—C1	25.79 (9)	C2—C4—C5	123.0 (3)
O1—Gd1—C1	74.32 (10)	C5—O5—Gd1iv	93.7 (2)
O5iii—Gd1—C1	132.62 (10)	O4—C5—O5	121.6 (3)
O4iii—Gd1—C1	92.23 (9)	O4—C5—C4	119.8 (3)
O9—Gd1—C1	141.67 (9)	O5—C5—C4	118.6 (3)
O2—Gd1—C1	25.71 (8)	O4—C5—Gd1iv	62.10 (18)
C6—Gd1—C1	125.03 (10)	O5—C5—Gd1iv	59.77 (18)
C5iii—Gd1—C1	112.55 (10)	C4—C5—Gd1iv	174.2 (2)
O2—K1—O6	116.27 (8)	C10—O6—Gd1v	138.0 (2)
O2—K1—O8	69.09 (7)	C10—O6—K1	99.1 (2)
O6—K1—O8	63.05 (8)	Gd1v—O6—K1	102.10 (9)
O2—K1—O10	72.67 (9)	O9—C6—O8	121.5 (3)
O6—K1—O10	140.08 (10)	O9—C6—C7	119.1 (3)
O8—K1—O10	141.74 (9)	O8—C6—C7	119.1 (3)
O2—K1—O1iv	84.58 (8)	O9—C6—Gd1	63.11 (18)
O6—K1—O1iv	153.86 (8)	O8—C6—Gd1	59.14 (17)
O8—K1—O1iv	115.86 (9)	C7—C6—Gd1	166.0 (2)
O10—K1—O1iv	58.46 (9)	C10—O7—Gd1vi	147.2 (2)
O2—K1—O4iv	123.48 (8)	C10—O7—K1v	114.5 (2)
O6—K1—O4iv	83.45 (7)	Gd1vi—O7—K1v	98.05 (8)
O8—K1—O4iv	76.77 (7)	C8—C7—C9	119.4 (3)
O10—K1—O4iv	125.96 (9)	C8—C7—C6	117.3 (3)
O1iv—K1—O4iv	71.42 (8)	C9—C7—C6	123.2 (3)
O2—K1—O7i	73.25 (8)	C6—O8—Gd1	94.4 (2)
O6—K1—O7i	58.96 (7)	C6—O8—K1	127.7 (2)
O8—K1—O7i	79.25 (8)	Gd1—O8—K1	105.81 (9)
O10—K1—O7i	90.92 (9)	C7—C8—C9viii	120.9 (3)
O1iv—K1—O7i	146.80 (8)	C7—C8—H8	119.5
O4iv—K1—O7i	141.64 (7)	C9viii—C8—H8	119.5
O2—K1—O9v	120.23 (8)	C6—O9—Gd1	90.7 (2)
O6—K1—O9v	67.91 (7)	C6—O9—K1i	136.5 (2)
O8—K1—O9v	127.17 (8)	Gd1—O9—K1i	94.77 (8)
O10—K1—O9v	74.28 (9)	C8viii—C9—C7	119.7 (3)
O1iv—K1—O9v	116.76 (8)	C8viii—C9—C10	118.6 (3)
O4iv—K1—O9v	116.29 (8)	C7—C9—C10	121.4 (3)
O7i—K1—O9v	59.01 (7)	O7—C10—O6	123.9 (3)
O2—K1—C10	129.24 (8)	O7—C10—C9	119.4 (3)
O6—K1—C10	22.64 (8)	O6—C10—C9	116.7 (3)
O8—K1—C10	63.26 (8)	O7—C10—K1	91.9 (2)
O10—K1—C10	152.09 (10)	O6—C10—K1	58.30 (18)
O1iv—K1—C10	131.40 (9)	C9—C10—K1	121.7 (2)
O4iv—K1—C10	60.96 (8)	K1—O10—H10A	138.3
O7i—K1—C10	81.59 (8)	K1—O10—H10B	102.5
O9v—K1—C10	78.87 (8)	H10A—O10—H10B	106.3
O2—K1—O3vi	137.10 (8)

Table 1

Selected bond lengths (Å)

Gd1—O6i	2.337 (3)
Gd1—O7ii	2.376 (2)
Gd1—O8	2.433 (2)
Gd1—O3	2.441 (2)
Gd1—O1	2.447 (3)
Gd1—O5iii	2.451 (2)
Gd1—O4iii	2.503 (2)
Gd1—O9	2.520 (3)
Gd1—O2	2.604 (2)
K1—O2	2.714 (3)
K1—O6	2.783 (3)
K1—O8	2.795 (3)
K1—O10	2.842 (3)
K1—O1iv	2.860 (3)
K1—O4iv	2.875 (3)
K1—O7i	2.891 (3)
K1—O9v	2.893 (3)

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .