Poly[di-μ₄-1,4-benzene­dicarboxyl­ato-μ₆-succinato-didysprosium(III)]

A new three-dimensional coordination polymer, [Dy₂(C₄H₄O₄)(C₈H₄O₄)₂]_n, has been synthesized under hydro­thermal conditions. The coordination of the Dy atoms is distorted square anti­prismatic. The anti­prisms are bridged by the 1,4-benzene­dicarboxyl­ate and succinate ligands, forming a three-dimensional network. The succinate ion is located on an inversion center.

Key indicators

• Single-crystal X-ray study
• T = 291 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.021
• wR factor = 0.060
• Data-to-parameter ratio = 15.8

checkCIF/PLATON results

No syntax errors found



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

---

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[di-µ₄-1,4-benzenedicarboxylato-µ₆-succinato-didysprosium(III)]

Crystal data

[Dy2(C4H4O4)(C8H4O4)2]	F(000) = 1440
Mr = 769.30	Dx = 2.510 Mg m^−3
Orthorhombic, Pbca	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ac 2ab	Cell parameters from 147 reflections
a = 13.8042 (9) Å	θ = 3.3–26.7°
b = 6.7910 (4) Å	µ = 7.35 mm^−1
c = 21.7163 (13) Å	T = 291 K
V = 2035.8 (2) Å^3	Column, colorless
Z = 4	0.32 × 0.11 × 0.08 mm

Data collection

Bruker SMART APEXII CCD area-detector diffractometer	2453 independent reflections
Radiation source: fine-focus sealed tube	2290 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.028
φ and ω scans	θmax = 28.1°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −11→18
Tmin = 0.265, Tmax = 0.563	k = −8→7
10848 measured reflections	l = −28→28

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)] = 0.021	H-atom parameters constrained
wR(F^2) = 0.060	w = 1/[σ^2(Fo^2) + (0.0378P)^2 + 2.3787P] where P = (Fo^2 + 2Fc^2)/3
S = 1.01	(Δ/σ)max = 0.001
2453 reflections	Δρmax = 0.85 e Å^−3
155 parameters	Δρmin = −0.99 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: 0.00269 (12)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Dy	0.169168 (10)	0.01688 (2)	0.445231 (6)	0.01308 (8)
O1	0.1372 (2)	0.0378 (3)	0.54864 (8)	0.0209 (5)
O2	−0.01061 (14)	−0.0721 (3)	0.56733 (8)	0.0210 (4)
C1	0.0746 (2)	−0.0328 (4)	0.58392 (11)	0.0152 (5)
C2	0.10153 (19)	−0.0742 (4)	0.64940 (11)	0.0177 (5)
C3	0.0351 (2)	−0.1567 (5)	0.68975 (11)	0.0259 (6)
H3A	−0.0270	−0.1867	0.6760	0.031*
C4	0.0603 (2)	−0.1949 (5)	0.75024 (12)	0.0270 (6)
H4A	0.0155	−0.2511	0.7770	0.032*
C5	0.1528 (2)	−0.1488 (4)	0.77090 (11)	0.0213 (6)
C6	0.1810 (2)	−0.1971 (4)	0.83627 (11)	0.0219 (6)
C7	0.2195 (2)	−0.0663 (5)	0.73096 (12)	0.0267 (6)
H7A	0.2816	−0.0362	0.7447	0.032*
C8	0.1937 (3)	−0.0287 (5)	0.67054 (14)	0.0254 (6)
H8A	0.2385	0.0275	0.6438	0.030*
O3	0.26033 (15)	−0.1329 (3)	0.85588 (8)	0.0270 (5)
O4	0.12364 (15)	−0.3007 (3)	0.86707 (8)	0.0282 (5)
O5	0.33330 (13)	−0.1295 (4)	0.45301 (10)	0.0233 (5)
O6	0.32407 (13)	0.1752 (3)	0.48311 (9)	0.0211 (4)
C9	0.3745 (2)	0.0284 (4)	0.46824 (15)	0.0246 (6)
C10	0.4838 (3)	0.0410 (5)	0.46880 (16)	0.0305 (7)
H10A	0.5048	0.1765	0.4641	0.037*
H10B	0.5111	−0.0364	0.4355	0.037*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Dy	0.01281 (12)	0.01609 (11)	0.01035 (11)	0.00038 (4)	0.00008 (4)	−0.00129 (3)
O1	0.0224 (13)	0.0279 (11)	0.0123 (9)	−0.0028 (10)	−0.0006 (8)	0.0002 (7)
O2	0.0171 (10)	0.0311 (11)	0.0149 (8)	0.0014 (9)	−0.0035 (7)	0.0004 (8)
C1	0.0153 (13)	0.0184 (12)	0.0118 (11)	0.0027 (10)	0.0001 (10)	−0.0002 (9)
C2	0.0185 (13)	0.0226 (13)	0.0119 (10)	0.0002 (11)	−0.0023 (9)	0.0019 (9)
C3	0.0209 (14)	0.0401 (17)	0.0168 (12)	−0.0060 (13)	−0.0037 (10)	0.0075 (11)
C4	0.0280 (15)	0.0347 (17)	0.0183 (12)	−0.0048 (13)	−0.0004 (11)	0.0077 (11)
C5	0.0286 (14)	0.0226 (14)	0.0128 (11)	−0.0011 (12)	−0.0058 (10)	0.0034 (10)
C6	0.0305 (15)	0.0205 (14)	0.0147 (12)	0.0033 (11)	−0.0057 (10)	0.0020 (10)
C7	0.0263 (16)	0.0359 (16)	0.0179 (12)	−0.0103 (14)	−0.0093 (11)	0.0061 (12)
C8	0.0241 (16)	0.0344 (17)	0.0175 (14)	−0.0091 (13)	−0.0033 (13)	0.0084 (11)
O3	0.0280 (11)	0.0378 (12)	0.0151 (8)	−0.0011 (10)	−0.0060 (8)	−0.0012 (8)
O4	0.0366 (12)	0.0296 (11)	0.0185 (9)	−0.0011 (10)	−0.0047 (8)	0.0088 (8)
O5	0.0167 (11)	0.0179 (11)	0.0355 (11)	−0.0005 (8)	−0.0072 (8)	−0.0016 (9)
O6	0.0205 (10)	0.0186 (10)	0.0243 (9)	0.0014 (8)	−0.0022 (7)	−0.0029 (8)
C9	0.0232 (17)	0.0210 (14)	0.0297 (16)	0.0000 (11)	−0.0081 (13)	0.0002 (11)
C10	0.033 (2)	0.0248 (15)	0.0334 (18)	−0.0020 (14)	−0.0028 (14)	0.0038 (13)

Geometric parameters (Å, º)

Dy—O2^i	2.237 (2)	C4—C5	1.388 (4)
Dy—O1	2.2931 (19)	C4—H4A	0.9300
Dy—O3^ii	2.3093 (18)	C5—C7	1.384 (4)
Dy—O4^iii	2.3305 (19)	C5—C6	1.508 (3)
Dy—O5^iv	2.408 (3)	C6—O4	1.253 (3)
Dy—O6^v	2.463 (2)	C6—O3	1.253 (3)
Dy—O5	2.480 (2)	C7—C8	1.383 (4)
Dy—O6	2.5308 (19)	C7—H7A	0.9300
Dy—C9	2.880 (3)	C8—H8A	0.9300
O1—C1	1.251 (4)	O5—C9	1.258 (4)
O2—C1	1.258 (3)	O6—C9	1.259 (4)
C1—C2	1.496 (3)	C9—C10	1.511 (5)
C2—C3	1.387 (4)	C10—C10^vi	1.532 (7)
C2—C8	1.388 (4)	C10—H10A	0.9700
C3—C4	1.383 (3)	C10—H10B	0.9700
C3—H3A	0.9300
O2^i—Dy—O1	85.45 (8)	C3—C2—C8	119.2 (2)
O2^i—Dy—O3^ii	104.64 (7)	C3—C2—C1	120.8 (2)
O1—Dy—O3^ii	151.99 (8)	C8—C2—C1	120.0 (2)
O2^i—Dy—O4^iii	75.70 (7)	C4—C3—C2	120.6 (3)
O1—Dy—O4^iii	134.46 (8)	C4—C3—H3A	119.7
O3^ii—Dy—O4^iii	73.54 (8)	C2—C3—H3A	119.7
O2^i—Dy—O5^iv	80.07 (7)	C3—C4—C5	119.7 (3)
O1—Dy—O5^iv	82.34 (7)	C3—C4—H4A	120.1
O3^ii—Dy—O5^iv	74.02 (7)	C5—C4—H4A	120.1
O4^iii—Dy—O5^iv	132.50 (7)	C7—C5—C4	120.0 (2)
O2^i—Dy—O6^v	103.63 (7)	C7—C5—C6	120.4 (2)
O1—Dy—O6^v	74.85 (7)	C4—C5—C6	119.5 (2)
O3^ii—Dy—O6^v	125.87 (7)	O4—C6—O3	124.5 (2)
O4^iii—Dy—O6^v	70.13 (7)	O4—C6—C5	117.5 (2)
O5^iv—Dy—O6^v	156.42 (6)	O3—C6—C5	118.0 (2)
O2^i—Dy—O5	165.76 (8)	C8—C7—C5	119.8 (3)
O1—Dy—O5	97.70 (8)	C8—C7—H7A	120.1
O3^ii—Dy—O5	78.99 (7)	C5—C7—H7A	120.1
O4^iii—Dy—O5	92.49 (7)	C7—C8—C2	120.6 (3)
O5^iv—Dy—O5	114.08 (6)	C7—C8—H8A	119.7
O6^v—Dy—O5	64.22 (7)	C2—C8—H8A	119.7
O2^i—Dy—O6	142.65 (7)	C6—O3—Dy^vii	140.58 (17)
O1—Dy—O6	79.52 (8)	C6—O4—Dy^viii	124.91 (18)
O3^ii—Dy—O6	76.82 (7)	C9—O5—Dy^v	151.0 (2)
O4^iii—Dy—O6	137.07 (7)	C9—O5—Dy	95.15 (19)
O5^iv—Dy—O6	64.24 (7)	Dy^v—O5—Dy	112.46 (8)
O6^v—Dy—O6	105.05 (6)	C9—O6—Dy^iv	129.76 (19)
O5—Dy—O6	51.41 (7)	C9—O6—Dy	92.74 (18)
O2^i—Dy—C9	168.43 (8)	Dy^iv—O6—Dy	108.89 (7)
O1—Dy—C9	91.03 (10)	O5—C9—O6	119.5 (3)
O3^ii—Dy—C9	73.84 (8)	O5—C9—C10	120.1 (3)
O4^iii—Dy—C9	114.14 (8)	O6—C9—C10	120.4 (3)
O5^iv—Dy—C9	88.55 (7)	O5—C9—Dy	59.05 (16)
O6^v—Dy—C9	86.00 (7)	O6—C9—Dy	61.38 (16)
O5—Dy—C9	25.79 (8)	C10—C9—Dy	170.3 (2)
O6—Dy—C9	25.89 (7)	C9—C10—C10^vi	106.1 (4)
C1—O1—Dy	135.18 (19)	C9—C10—H10A	110.5
C1—O2—Dy^i	155.99 (19)	C10^vi—C10—H10A	110.5
O1—C1—O2	123.5 (2)	C9—C10—H10B	110.5
O1—C1—C2	118.8 (3)	C10^vi—C10—H10B	110.5
O2—C1—C2	117.7 (2)	H10A—C10—H10B	108.7

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