Poly[diaquadi-μ₅-succinato-μ₆-succinato-didysprosium(III)]

The title compound, [Dy₂(C₄H₄O₄)₃(H₂O)₂], has been synthesized under hydro­thermal conditions. The asymmetric unit consists of two Dy³⁺ cations, three succinate anions and two aqua ligands. The succinate ligands exhibit gauche and anti conformations with different coordination modes. The Dy atoms are bridged into a three-dimensional network by succinate ligands.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C)= 0.007 Å
• R factor = 0.024
• wR factor = 0.061
• Data-to-parameter ratio = 13.4

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.

Poly[diaquadi-µ₅-succinato-µ₆-succinato-didysprosium(III)]

Crystal data

[Dy2(C4H4O4)3(H2O)2]	Z = 2
Mr = 709.25	F(000) = 664
Triclinic, P1	Dx = 2.846 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.646 (2) Å	Cell parameters from 256 reflections
b = 8.041 (2) Å	θ = 3.3–26.7°
c = 14.086 (4) Å	µ = 9.04 mm^−1
α = 96.915 (4)°	T = 295 K
β = 97.004 (4)°	Needle, colorless
γ = 103.057 (4)°	0.18 × 0.08 × 0.06 mm
V = 827.6 (4) Å^3

Data collection

Bruker SMART APEXII CCD area-detector diffractometer	3413 independent reflections
Radiation source: fine-focus sealed tube	2840 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.018
φ and ω scans	θmax = 26.9°, θmin = 1.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −9→10
Tmin = 0.425, Tmax = 0.586	k = −8→10
4877 measured reflections	l = −18→17

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)] = 0.024	H-atom parameters constrained
wR(F^2) = 0.061	w = 1/[σ^2(Fo^2) + (0.038P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.96	(Δ/σ)max = 0.001
3413 reflections	Δρmax = 1.19 e Å^−3
254 parameters	Δρmin = −1.49 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 (2)

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
Dy1	0.87103 (3)	0.93180 (3)	0.709780 (14)	0.01426 (8)
Dy2	0.40950 (3)	1.01236 (3)	0.795775 (14)	0.01380 (8)
O1	0.6567 (4)	0.8480 (4)	0.8130 (2)	0.0199 (7)
O2	0.4411 (4)	0.7974 (5)	0.8997 (2)	0.0224 (8)
C1	0.5890 (6)	0.7715 (6)	0.8789 (3)	0.0161 (9)
C2	0.6792 (6)	0.6481 (6)	0.9264 (3)	0.0191 (10)
H2A	0.6825	0.5536	0.8774	0.023*
H2B	0.6058	0.5998	0.9726	0.023*
C3	0.8731 (6)	0.7297 (6)	0.9789 (3)	0.0168 (10)
H3A	0.9300	0.6385	0.9954	0.020*
H3B	0.9427	0.7914	0.9353	0.020*
C4	0.8805 (6)	0.8531 (6)	1.0703 (3)	0.0156 (9)
O3	0.7439 (4)	0.9104 (5)	1.0800 (2)	0.0245 (8)
O4	1.0243 (4)	0.8923 (5)	1.1312 (2)	0.0215 (7)
O5	0.3553 (5)	0.8420 (5)	0.6402 (2)	0.0241 (8)
O6	0.6108 (4)	0.7798 (5)	0.6032 (2)	0.0261 (8)
C5	0.4431 (6)	0.7649 (6)	0.5872 (3)	0.0155 (9)
C6	0.3405 (6)	0.6428 (6)	0.4972 (3)	0.0149 (9)
H6A	0.2117	0.6369	0.4936	0.018*
H6B	0.3577	0.5279	0.5014	0.018*
C7	0.4052 (6)	0.7017 (6)	0.4055 (3)	0.0169 (10)
H7A	0.5333	0.7594	0.4205	0.020*
H7B	0.3920	0.6008	0.3575	0.020*
C8	0.3041 (6)	0.8215 (6)	0.3628 (3)	0.0175 (10)
O9	1.1186 (4)	0.8080 (4)	0.7730 (2)	0.0190 (7)
O10	0.8565 (5)	0.6290 (5)	0.7203 (3)	0.0297 (8)
C9	1.0183 (6)	0.6540 (6)	0.7582 (3)	0.0173 (10)
C10	1.0892 (7)	0.5036 (6)	0.7872 (3)	0.0225 (11)
H10A	0.9900	0.4154	0.8009	0.027*
H10B	1.1783	0.5422	0.8455	0.027*
C11	1.1761 (7)	0.4284 (7)	0.7058 (4)	0.0251 (11)
H11A	1.0859	0.3860	0.6482	0.030*
H11B	1.2723	0.5177	0.6905	0.030*
C12	1.2534 (7)	0.2819 (6)	0.7360 (3)	0.0190 (10)
O11	1.4014 (5)	0.3141 (5)	0.7892 (3)	0.0298 (8)
O12	1.1658 (4)	0.1229 (4)	0.7055 (2)	0.0212 (7)
O13	0.9919 (5)	0.8307 (6)	0.5685 (3)	0.0355 (10)
O14	0.6475 (4)	1.1793 (5)	0.9178 (2)	0.0225 (8)
O8	0.1859 (5)	0.8726 (5)	0.4035 (3)	0.0317 (9)
O7	0.3384 (4)	0.8725 (4)	0.2829 (2)	0.0194 (7)
H13B	0.8827	0.8174	0.5788	0.050*
H13A	1.1024	0.8303	0.5853	0.050*
H14B	0.6225	1.1783	0.9749	0.050*
H14A	0.7379	1.1406	0.9045	0.050*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Dy1	0.00938 (13)	0.01928 (14)	0.01527 (13)	0.00598 (9)	0.00142 (8)	0.00287 (9)
Dy2	0.00943 (13)	0.01743 (14)	0.01510 (13)	0.00512 (9)	0.00137 (8)	0.00172 (9)
O1	0.0203 (18)	0.0198 (18)	0.0210 (17)	0.0058 (14)	0.0046 (14)	0.0057 (14)
O2	0.0153 (17)	0.033 (2)	0.0218 (17)	0.0092 (15)	0.0055 (14)	0.0084 (15)
C1	0.011 (2)	0.021 (3)	0.014 (2)	0.0006 (18)	−0.0004 (17)	0.0021 (18)
C2	0.017 (2)	0.019 (3)	0.021 (2)	0.0032 (19)	0.0004 (19)	0.004 (2)
C3	0.013 (2)	0.019 (3)	0.019 (2)	0.0058 (19)	0.0014 (18)	0.0029 (19)
C4	0.015 (2)	0.018 (2)	0.015 (2)	0.0028 (18)	0.0042 (18)	0.0057 (18)
O3	0.0149 (17)	0.038 (2)	0.0211 (17)	0.0124 (16)	0.0018 (14)	−0.0037 (16)
O4	0.0132 (17)	0.031 (2)	0.0189 (17)	0.0056 (15)	0.0004 (13)	0.0000 (15)
O5	0.0182 (18)	0.030 (2)	0.0217 (17)	0.0061 (15)	0.0039 (14)	−0.0067 (15)
O6	0.0149 (18)	0.036 (2)	0.0245 (18)	0.0092 (15)	−0.0025 (14)	−0.0061 (16)
C5	0.013 (2)	0.018 (2)	0.015 (2)	0.0020 (18)	0.0006 (18)	0.0035 (19)
C6	0.010 (2)	0.020 (2)	0.014 (2)	0.0019 (18)	0.0014 (17)	0.0027 (18)
C7	0.012 (2)	0.019 (3)	0.018 (2)	0.0036 (19)	−0.0004 (18)	−0.0004 (19)
C8	0.010 (2)	0.021 (3)	0.021 (2)	0.0018 (19)	0.0017 (18)	0.006 (2)
O9	0.0165 (17)	0.0166 (18)	0.0258 (17)	0.0071 (14)	0.0020 (14)	0.0055 (14)
O10	0.0158 (18)	0.0188 (19)	0.051 (2)	0.0042 (15)	−0.0054 (16)	0.0029 (17)
C9	0.015 (2)	0.014 (2)	0.020 (2)	0.0028 (19)	−0.0001 (19)	−0.0008 (19)
C10	0.026 (3)	0.016 (3)	0.026 (3)	0.006 (2)	0.002 (2)	0.004 (2)
C11	0.031 (3)	0.022 (3)	0.029 (3)	0.015 (2)	0.009 (2)	0.009 (2)
C12	0.021 (3)	0.018 (3)	0.022 (2)	0.009 (2)	0.010 (2)	0.004 (2)
O11	0.0207 (19)	0.024 (2)	0.042 (2)	0.0056 (15)	−0.0047 (16)	0.0028 (17)
O12	0.0192 (18)	0.0192 (19)	0.0279 (18)	0.0092 (14)	0.0046 (14)	0.0050 (15)
O13	0.0135 (19)	0.060 (3)	0.032 (2)	0.0087 (18)	0.0097 (16)	−0.0038 (19)
O14	0.0159 (17)	0.031 (2)	0.0196 (16)	0.0079 (15)	0.0012 (14)	−0.0004 (15)
O8	0.029 (2)	0.048 (3)	0.034 (2)	0.0241 (19)	0.0163 (17)	0.0263 (19)
O7	0.0216 (18)	0.0218 (19)	0.0174 (16)	0.0078 (14)	0.0051 (14)	0.0062 (14)

Geometric parameters (Å, º)

Dy1—O1	2.361 (3)	C3—H3B	0.9700
Dy1—O4^i	2.439 (3)	C4—O3	1.248 (5)
Dy1—O6	2.332 (3)	C4—O4	1.262 (5)
Dy1—O7^ii	2.488 (3)	O5—C5	1.262 (5)
Dy1—O8^ii	2.440 (3)	O6—C5	1.250 (5)
Dy1—O9	2.454 (3)	C5—C6	1.515 (6)
Dy1—O10	2.435 (4)	C6—C7	1.527 (6)
Dy1—O12^iii	2.436 (3)	C6—H6A	0.9700
Dy1—O13	2.423 (3)	C6—H6B	0.9700
Dy2—O1	2.544 (3)	C7—C8	1.500 (6)
Dy2—O2	2.430 (3)	C7—H7A	0.9700
Dy2—O3^iv	2.323 (3)	C7—H7B	0.9700
Dy2—O5	2.377 (3)	C8—O8	1.245 (6)
Dy2—O7^ii	2.400 (3)	C8—O7	1.280 (5)
Dy2—O9^v	2.408 (3)	O9—C9	1.278 (6)
Dy2—O11^vi	2.453 (4)	O10—C9	1.247 (6)
Dy2—O12^vi	2.515 (3)	C9—C10	1.512 (6)
Dy2—O14	2.376 (3)	C10—C11	1.525 (7)
Dy1—C8^ii	2.851 (5)	C10—H10A	0.9700
Dy1—C9	2.835 (5)	C10—H10B	0.9700
Dy2—C12^vi	2.862 (5)	C11—C12	1.514 (6)
Dy2—C1	2.892 (5)	C11—H11A	0.9700
O1—C1	1.272 (5)	C11—H11B	0.9700
O2—C1	1.257 (5)	C12—O11	1.235 (6)
C1—C2	1.505 (6)	C12—O12	1.295 (6)
C2—C3	1.533 (6)	O13—H13B	0.8502
C2—H2A	0.9700	O13—H13A	0.8499
C2—H2B	0.9700	O14—H14B	0.8505
C3—C4	1.515 (6)	O14—H14A	0.8513
C3—H3A	0.9700
O6—Dy1—O1	76.42 (12)	O5—Dy2—C12^vi	96.10 (13)
O6—Dy1—O13	76.94 (12)	O7^ii—Dy2—C12^vi	86.95 (12)
O1—Dy1—O13	143.53 (13)	O9^v—Dy2—C12^vi	92.89 (12)
O6—Dy1—O10	75.24 (12)	O2—Dy2—C12^vi	152.57 (12)
O1—Dy1—O10	73.76 (12)	O11^vi—Dy2—C12^vi	25.40 (13)
O13—Dy1—O10	75.70 (14)	O12^vi—Dy2—C12^vi	26.89 (13)
O6—Dy1—O12^iii	139.08 (11)	O1—Dy2—C12^vi	154.53 (12)
O1—Dy1—O12^iii	142.97 (11)	O3^iv—Dy2—C1	100.94 (12)
O13—Dy1—O12^iii	70.58 (12)	O14—Dy2—C1	73.48 (13)
O10—Dy1—O12^iii	118.26 (11)	O5—Dy2—C1	91.08 (13)
O6—Dy1—O4^i	143.16 (11)	O7^ii—Dy2—C1	93.04 (12)
O1—Dy1—O4^i	70.96 (11)	O9^v—Dy2—C1	91.50 (12)
O13—Dy1—O4^i	139.83 (12)	O2—Dy2—C1	25.48 (11)
O10—Dy1—O4^i	110.47 (12)	O11^vi—Dy2—C1	147.91 (13)
O12^iii—Dy1—O4^i	72.07 (11)	O12^vi—Dy2—C1	159.31 (13)
O6—Dy1—O8^ii	74.63 (14)	O1—Dy2—C1	26.07 (11)
O1—Dy1—O8^ii	119.05 (11)	C12^vi—Dy2—C1	172.52 (13)
O13—Dy1—O8^ii	76.50 (13)	O2—C1—O1	117.6 (4)
O10—Dy1—O8^ii	142.71 (13)	O2—C1—C2	121.6 (4)
O12^iii—Dy1—O8^ii	74.13 (12)	O1—C1—C2	120.7 (4)
O4^i—Dy1—O8^ii	106.82 (13)	O2—C1—Dy2	56.3 (2)
O6—Dy1—O9	125.19 (12)	O1—C1—Dy2	61.5 (2)
O1—Dy1—O9	101.24 (11)	C2—C1—Dy2	177.4 (3)
O13—Dy1—O9	74.87 (12)	C1—C2—C3	114.3 (4)
O10—Dy1—O9	52.73 (11)	C1—C2—H2A	108.7
O12^iii—Dy1—O9	69.13 (11)	C3—C2—H2A	108.7
O4^i—Dy1—O9	78.54 (11)	C1—C2—H2B	108.7
O8^ii—Dy1—O9	139.09 (11)	C3—C2—H2B	108.7
O6—Dy1—O7^ii	75.99 (12)	H2A—C2—H2B	107.6
O1—Dy1—O7^ii	69.15 (11)	C4—C3—C2	113.3 (4)
O13—Dy1—O7^ii	126.67 (12)	C4—C3—H3A	108.9
O10—Dy1—O7^ii	137.21 (11)	C2—C3—H3A	108.9
O12^iii—Dy1—O7^ii	104.23 (11)	C4—C3—H3B	108.9
O4^i—Dy1—O7^ii	76.78 (11)	C2—C3—H3B	108.9
O8^ii—Dy1—O7^ii	52.36 (10)	H3A—C3—H3B	107.7
O9—Dy1—O7^ii	155.27 (11)	O3—C4—O4	124.3 (4)
O6—Dy1—C9	100.09 (13)	O3—C4—C3	117.6 (4)
O1—Dy1—C9	86.76 (12)	O4—C4—C3	118.0 (4)
O13—Dy1—C9	73.93 (14)	O6—C5—O5	125.0 (4)
O10—Dy1—C9	25.99 (12)	O6—C5—C6	116.3 (4)
O12^iii—Dy1—C9	94.24 (12)	O5—C5—C6	118.6 (4)
O4^i—Dy1—C9	94.77 (12)	C5—C6—C7	111.5 (4)
O8^ii—Dy1—C9	150.38 (12)	C5—C6—H6A	109.3
O9—Dy1—C9	26.75 (12)	C7—C6—H6A	109.3
O7^ii—Dy1—C9	155.88 (12)	C5—C6—H6B	109.3
O6—Dy1—C8^ii	72.39 (13)	C7—C6—H6B	109.3
O1—Dy1—C8^ii	94.22 (12)	H6A—C6—H6B	108.0
O13—Dy1—C8^ii	100.94 (13)	C8—C7—C6	113.8 (4)
O10—Dy1—C8^ii	147.32 (13)	C8—C7—H7A	108.8
O12^iii—Dy1—C8^ii	89.81 (12)	C6—C7—H7A	108.8
O4^i—Dy1—C8^ii	93.15 (13)	C8—C7—H7B	108.8
O8^ii—Dy1—C8^ii	25.76 (12)	C6—C7—H7B	108.8
O9—Dy1—C8^ii	158.82 (13)	H7A—C7—H7B	107.7
O7^ii—Dy1—C8^ii	26.65 (11)	O8—C8—O7	118.9 (4)
C9—Dy1—C8^ii	171.89 (13)	O8—C8—C7	121.2 (4)
O3^iv—Dy2—O14	76.87 (12)	O7—C8—C7	119.9 (4)
O3^iv—Dy2—O5	140.79 (12)	Dy2^vii—O9—Dy1	111.92 (12)
O14—Dy2—O5	142.16 (11)	C9—O10—Dy1	95.2 (3)
O3^iv—Dy2—O7^ii	141.01 (12)	O10—C9—O9	118.5 (4)
O14—Dy2—O7^ii	72.55 (11)	O10—C9—C10	119.5 (4)
O5—Dy2—O7^ii	74.09 (12)	O9—C9—C10	121.9 (4)
O3^iv—Dy2—O9^v	72.28 (12)	O10—C9—Dy1	58.8 (2)
O14—Dy2—O9^v	142.30 (11)	O9—C9—Dy1	59.7 (2)
O5—Dy2—O9^v	70.21 (12)	C10—C9—Dy1	177.0 (3)
O7^ii—Dy2—O9^v	144.07 (11)	C9—C10—C11	109.9 (4)
O3^iv—Dy2—O2	78.49 (12)	C9—C10—H10A	109.7
O14—Dy2—O2	79.84 (12)	C11—C10—H10A	109.7
O5—Dy2—O2	101.02 (12)	C9—C10—H10B	109.7
O7^ii—Dy2—O2	118.25 (11)	C11—C10—H10B	109.7
O9^v—Dy2—O2	73.28 (11)	H10A—C10—H10B	108.2
O3^iv—Dy2—O11^vi	74.06 (13)	C12—C11—C10	110.1 (4)
O14—Dy2—O11^vi	74.53 (12)	C12—C11—H11A	109.6
O5—Dy2—O11^vi	113.07 (13)	C10—C11—H11A	109.6
O7^ii—Dy2—O11^vi	74.91 (12)	C12—C11—H11B	109.6
O9^v—Dy2—O11^vi	115.85 (11)	C10—C11—H11B	109.6
O2—Dy2—O11^vi	145.87 (12)	H11A—C11—H11B	108.2
O3^iv—Dy2—O12^vi	78.82 (11)	O11—C12—O12	119.9 (4)
O14—Dy2—O12^vi	125.74 (11)	O11—C12—C11	119.8 (5)
O5—Dy2—O12^vi	77.33 (12)	O12—C12—C11	120.3 (4)
O7^ii—Dy2—O12^vi	100.01 (11)	O11—C12—Dy2^viii	58.4 (3)
O9^v—Dy2—O12^vi	68.56 (11)	O12—C12—Dy2^viii	61.4 (2)
O2—Dy2—O12^vi	139.95 (11)	C11—C12—Dy2^viii	178.3 (4)
O11^vi—Dy2—O12^vi	52.29 (11)	C12—O11—Dy2^viii	96.2 (3)
O3^iv—Dy2—O1	124.38 (11)	C12—O12—Dy1^ix	139.0 (3)
O14—Dy2—O1	72.32 (11)	C12—O12—Dy2^viii	91.7 (3)
O5—Dy2—O1	78.89 (11)	Dy1^ix—O12—Dy2^viii	108.90 (12)
O7^ii—Dy2—O1	67.62 (11)	Dy1—O13—H13B	49.6
O9^v—Dy2—O1	108.42 (11)	Dy1—O13—H13A	109.0
O2—Dy2—O1	51.51 (10)	H13B—O13—H13A	152.2
O11^vi—Dy2—O1	135.65 (12)	Dy2—O14—H14B	113.9
O12^vi—Dy2—O1	155.51 (10)	Dy2—O14—H14A	102.2
O3^iv—Dy2—C12^vi	74.71 (12)	H14B—O14—H14A	117.5
O14—Dy2—C12^vi	99.43 (13)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O13—H13A···O5^vii	0.85	1.97	2.816 (6)	173
O13—H13B···O6	0.85	2.11	2.959 (6)	179
O14—H14A···O4^i	0.85	2.01	2.843 (5)	166
O14—H14B···O2^iv	0.85	1.89	2.733 (4)	173

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