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The title lanthanide–bdc complex, {[Lu2(C8H4O4)3(H2O)8]·2H2O}n (bdc is benzene-1,4-dicarboxyl­ate), was synthesized under hydro­thermal conditions. In this complex, the LuIII centers are eight-coordinated by four O atoms from three benzene-1,4-dicarboxyl­ate ligands and four from water mol­ecules. LuIII ions are bridged by benzene-1,4-dicarboxyl­ate anions in two modes, forming polymeric chains. These chains are further assembled into a three-dimensional supramol­ecular network by O—H...O hydrogen-bonding inter­actions.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806000225/ww6475sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806000225/ww6475Isup2.hkl
Contains datablock I

CCDC reference: 298578

Key indicators

  • Single-crystal X-ray study
  • T = 292 K
  • Mean [sigma](C-C) = 0.006 Å
  • R factor = 0.027
  • wR factor = 0.065
  • Data-to-parameter ratio = 19.8

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 top

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[[[µ-benzene-1,4-dicarboxylato-bis[tetraaqualutetium(III)]- di-µ-benzene-1,4-dicarboxylato] dihydrate] top
Crystal data top
[Lu2(C8H4O4)3(H2O)8]·2H2OZ = 1
Mr = 1022.44F(000) = 494
Triclinic, P1Dx = 2.171 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.5264 (4) ÅCell parameters from 156 reflections
b = 10.0492 (6) Åθ = 3.3–26.7°
c = 10.4543 (5) ŵ = 6.37 mm1
α = 87.806 (4)°T = 292 K
β = 82.513 (3)°Block, colorless
γ = 86.215 (3)°0.09 × 0.07 × 0.05 mm
V = 781.90 (7) Å3
Data collection top
Bruker SMART APEXII CCD area-detector
diffractometer
4327 independent reflections
Radiation source: fine-focus sealed tube3777 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.087
φ and ω scansθmax = 29.8°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Sheldrick, 1996)
h = 1010
Tmin = 0.586, Tmax = 0.725k = 1413
10175 measured reflectionsl = 1414
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.065 w = 1/[σ2(Fo2) + (0.0181P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.97(Δ/σ)max = 0.002
4327 reflectionsΔρmax = 1.81 e Å3
218 parametersΔρmin = 1.35 e Å3
0 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0012 (3)
Special details top

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 > 2σ(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 (Å2) top
xyzUiso*/Ueq
Lu0.22057 (2)0.264446 (15)0.547240 (16)0.01782 (6)
O10.2223 (4)0.2431 (3)0.3245 (3)0.0272 (7)
O20.2636 (4)0.4468 (3)0.3769 (3)0.0250 (6)
C10.2439 (5)0.3665 (4)0.2916 (4)0.0223 (8)
C20.2450 (5)0.4078 (4)0.1533 (4)0.0210 (8)
C30.2705 (6)0.5392 (4)0.1114 (4)0.0288 (10)
H30.29000.60270.16960.035*
C40.2666 (6)0.5747 (4)0.0180 (4)0.0278 (10)
H40.28570.66220.04590.033*
C50.2350 (5)0.4827 (4)0.1067 (4)0.0202 (8)
C60.2298 (5)0.5198 (4)0.2464 (4)0.0209 (8)
C70.2097 (7)0.3517 (4)0.0635 (4)0.0306 (10)
H70.18890.28840.12160.037*
C80.2153 (7)0.3148 (4)0.0647 (4)0.0309 (10)
H80.19900.22670.09190.037*
O30.2108 (5)0.4298 (3)0.3228 (3)0.0327 (7)
O40.2382 (5)0.6404 (3)0.2820 (3)0.0330 (8)
O50.3594 (4)0.1474 (3)0.7030 (3)0.0277 (7)
O60.6562 (4)0.1476 (3)0.6806 (3)0.0327 (7)
C90.5077 (5)0.1225 (4)0.7447 (4)0.0214 (8)
C100.5056 (5)0.0586 (4)0.8764 (4)0.0200 (8)
C110.3546 (5)0.0050 (4)0.9319 (4)0.0274 (9)
H110.25650.00860.88670.033*
C120.6497 (6)0.0632 (4)0.9455 (4)0.0255 (9)
H120.75100.10590.90910.031*
O70.5171 (4)0.2686 (3)0.4829 (3)0.0318 (9)
O80.2015 (5)0.0435 (3)0.5028 (3)0.0272 (8)
O90.0691 (4)0.3410 (3)0.5129 (3)0.0260 (6)
O100.0077 (4)0.1785 (3)0.7120 (3)0.0264 (7)
O110.0707 (4)0.8968 (3)0.7239 (4)0.0372 (8)
H7A0.57010.22960.53840.050*
H7B0.57850.31410.42980.050*
H8A0.17430.00310.56760.050*
H8B0.25960.00070.44450.050*
H9A0.10720.38120.57870.050*
H9B0.09970.35510.44090.050*
H10A0.04570.10250.72920.050*
H10B0.10030.17650.70850.050*
H11A0.12310.82590.74220.050*
H11B0.02370.86090.72220.050*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Lu0.01908 (9)0.02268 (10)0.01513 (9)0.00093 (6)0.00528 (6)0.00460 (6)
O10.0313 (18)0.0260 (15)0.0311 (16)0.0058 (13)0.0076 (13)0.0063 (12)
O20.0346 (17)0.0278 (14)0.0341 (16)0.0001 (12)0.0090 (12)0.0000 (12)
C10.0227 (19)0.031 (2)0.019 (2)0.0007 (16)0.0063 (15)0.0052 (16)
C20.027 (2)0.026 (2)0.0202 (19)0.0005 (16)0.0028 (15)0.0053 (15)
C30.025 (3)0.027 (2)0.020 (2)0.0073 (19)0.0085 (19)0.0009 (17)
C40.036 (3)0.020 (2)0.031 (2)0.0061 (18)0.0077 (19)0.0052 (17)
C50.026 (2)0.0223 (19)0.021 (2)0.0029 (16)0.0044 (15)0.0057 (15)
C60.024 (2)0.028 (2)0.0211 (19)0.0010 (16)0.0022 (15)0.0054 (16)
C70.026 (3)0.025 (2)0.022 (2)0.013 (2)0.006 (2)0.0010 (17)
C80.0355 (3)0.024 (2)0.0322 (2)0.0112 (19)0.005 (2)0.0051 (17)
O30.032 (2)0.0317 (16)0.0288 (17)0.0110 (14)0.0073 (15)0.0010 (13)
O40.034 (2)0.0256 (15)0.0310 (18)0.0008 (14)0.0026 (15)0.0082 (12)
O50.0198 (14)0.0404 (16)0.0169 (18)0.0001 (12)0.0035 (12)0.0139 (14)
O60.0209 (15)0.0517 (18)0.0185 (19)0.0052 (13)0.0052 (13)0.0167 (15)
C90.0226 (19)0.0239 (19)0.0202 (2)0.0014 (16)0.0057 (16)0.0071 (16)
C100.0198 (18)0.0230 (19)0.017 (2)0.0010 (15)0.0065 (15)0.0064 (15)
C110.026 (2)0.043 (2)0.021 (2)0.0053 (18)0.0097 (17)0.0104 (19)
C120.023 (2)0.036 (2)0.021 (2)0.0086 (17)0.0042 (16)0.0100 (18)
O70.0312 (16)0.077 (2)0.029 (2)0.0016 (15)0.0030 (14)0.0306 (18)
O80.031 (2)0.0260 (15)0.0276 (19)0.0017 (15)0.0005 (16)0.0065 (13)
O90.0262 (15)0.0340 (15)0.0202 (16)0.0028 (12)0.0082 (12)0.0058 (12)
O100.0390 (14)0.0364 (16)0.0333 (18)0.0000 (12)0.0055 (12)0.0106 (13)
O110.0323 (19)0.0257 (15)0.301 (2)0.0058 (13)0.0157 (17)0.0089 (14)
Geometric parameters (Å, º) top
Lu—O3i2.178 (3)C7—C81.382 (6)
Lu—O72.248 (3)C7—H70.9300
Lu—O52.294 (3)C8—H80.9300
Lu—O82.304 (3)O5—C91.257 (5)
Lu—O92.331 (3)O6—C91.261 (5)
Lu—O12.345 (3)C9—C101.495 (6)
Lu—O102.373 (3)C10—C121.383 (6)
Lu—O22.512 (3)C10—C111.391 (6)
O1—C11.290 (5)C11—C12ii1.386 (6)
O2—C11.255 (5)C11—H110.9300
C1—C21.487 (6)C12—H120.9300
C2—C81.389 (6)O7—H7A0.8200
C2—C31.393 (6)O7—H7B0.8200
C3—C41.390 (6)O8—H8A0.8199
C3—H30.9300O8—H8B0.8200
C4—C51.386 (6)O9—H9A0.8201
C4—H40.9300O9—H9B0.8199
C5—C71.392 (5)O10—H10A0.8200
C5—C61.499 (6)O10—H10B0.8199
C6—O31.256 (5)O11—H11A0.8199
C6—O41.256 (4)O11—H11B0.8201
O3i—Lu—O794.71 (14)C3—C2—C1121.1 (4)
O3i—Lu—O584.11 (11)C4—C3—C2119.5 (4)
O7—Lu—O573.88 (11)C4—C3—H3120.2
O3i—Lu—O8153.31 (13)C2—C3—H3120.2
O7—Lu—O895.48 (13)C5—C4—C3121.6 (4)
O5—Lu—O875.17 (12)C5—C4—H4119.2
O3i—Lu—O986.12 (11)C3—C4—H4119.2
O7—Lu—O9147.47 (11)C4—C5—C7118.3 (4)
O5—Lu—O9138.28 (10)C4—C5—C6122.1 (4)
O8—Lu—O998.15 (12)C7—C5—C6119.6 (4)
O3i—Lu—O1135.66 (10)O3—C6—O4122.4 (4)
O7—Lu—O180.42 (12)O3—C6—C5118.7 (3)
O5—Lu—O1134.43 (10)O4—C6—C5118.8 (4)
O8—Lu—O170.52 (11)C8—C7—C5120.7 (4)
O9—Lu—O176.58 (10)C8—C7—H7119.7
O3i—Lu—O1083.16 (11)C5—C7—H7119.7
O7—Lu—O10142.58 (10)C7—C8—C2120.7 (4)
O5—Lu—O1068.73 (10)C7—C8—H8119.7
O8—Lu—O1073.82 (11)C2—C8—H8119.7
O9—Lu—O1069.88 (9)C6—O3—Luiii171.2 (3)
O1—Lu—O10126.02 (10)C9—O5—Lu143.8 (3)
O3i—Lu—O282.80 (10)O5—C9—O6123.3 (4)
O7—Lu—O272.79 (10)O5—C9—C10117.6 (4)
O5—Lu—O2142.88 (10)O6—C9—C10119.1 (3)
O8—Lu—O2123.81 (10)C12—C10—C11119.0 (4)
O9—Lu—O275.07 (10)C12—C10—C9121.5 (4)
O1—Lu—O253.49 (9)C11—C10—C9119.5 (4)
O10—Lu—O2142.93 (9)C12ii—C11—C10120.0 (4)
O3i—Lu—C1108.89 (12)C12ii—C11—H11120.0
O7—Lu—C175.73 (12)C10—C11—H11120.0
O5—Lu—C1147.79 (11)C10—C12—C11ii121.0 (4)
O8—Lu—C197.52 (12)C10—C12—H12119.5
O9—Lu—C173.30 (11)C11ii—C12—H12119.5
O1—Lu—C127.04 (10)Lu—O7—H7A108.1
O10—Lu—C1140.28 (11)Lu—O7—H7B133.9
O2—Lu—C126.48 (10)H7A—O7—H7B115.8
C1—O1—Lu97.2 (2)Lu—O8—H8A113.0
C1—O2—Lu90.3 (2)Lu—O8—H8B127.8
O2—C1—O1118.9 (4)H8A—O8—H8B112.2
O2—C1—C2122.7 (4)Lu—O9—H9A103.6
O1—C1—C2118.4 (4)Lu—O9—H9B123.3
O2—C1—Lu63.2 (2)H9A—O9—H9B126.8
O1—C1—Lu55.7 (2)Lu—O10—H10A106.3
C2—C1—Lu173.7 (3)Lu—O10—H10B125.5
C8—C2—C3119.2 (4)H10A—O10—H10B107.5
C8—C2—C1119.6 (4)H11A—O11—H11B91.9
Symmetry codes: (i) x, y, z+1; (ii) x+1, y, z+2; (iii) x, y, z1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O7—H7A···O60.821.842.655 (4)171
O7—H7B···O4iv0.821.992.776 (5)159
O8—H8A···O11v0.821.982.797 (5)171
O8—H8B···O6vi0.822.042.826 (4)162
O9—H9A···O2vii0.822.062.712 (4)136
O9—H9B···O4viii0.822.072.866 (5)164
O10—H10A···O11v0.822.072.840 (4)158
O10—H10B···O6ix0.821.942.747 (4)170
O11—H11A···O4i0.822.012.792 (4)158
O11—H11B···O1vii0.822.002.802 (4)166
Symmetry codes: (i) x, y, z+1; (iv) x+1, y+1, z; (v) x, y1, z; (vi) x+1, y, z+1; (vii) x, y+1, z+1; (viii) x, y+1, z; (ix) x1, y, z.
 

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