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The title compound, [Gd2(C8H4O4)3(H2O)]n, is a two-dimensional coordination polymer. The Gd atoms are eight- and nine-coordinated. This compound is isostructural with its dysprosium analog.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806011433/hb2010sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806011433/hb2010Isup2.hkl
Contains datablock I

CCDC reference: 608335

Key indicators

  • Single-crystal X-ray study
  • T = 290 K
  • Mean [sigma](C-C) = 0.010 Å
  • R factor = 0.043
  • wR factor = 0.111
  • Data-to-parameter ratio = 14.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.77 Ratio PLAT342_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 10
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 2 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 1 ALERT type 2 Indicator that the structure model may be wrong or deficient 1 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: CrystalClear (Rigaku, 2002); cell refinement: CrystalClear; data reduction: CrystalClear; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: PROG (ref, date); software used to prepare material for publication: SHELXL97.

Poly[aquabis(µ4-benzene-1,2-dicarboxylato)(µ3-benzene-1,2- dicarboxylato)digadolinium(III)] top
Crystal data top
[Gd2(C8H4O4)3(H2O)F(000) = 1560
Mr = 824.85Dx = 2.333 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 5932 reflections
a = 7.9786 (5) Åθ = 3.1–27.5°
b = 26.4255 (15) ŵ = 5.67 mm1
c = 11.6508 (8) ÅT = 290 K
β = 107.048 (3)°Rod, colorless
V = 2348.5 (3) Å30.60 × 0.11 × 0.10 mm
Z = 4
Data collection top
Rigaku Mercury CCD
diffractometer
5352 independent reflections
Radiation source: fine-focus sealed tube4551 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.056
Detector resolution: 14.631 pixels mm-1θmax = 27.5°, θmin = 3.1°
ω scansh = 1010
Absorption correction: multi-scan
(CrystalClear; Rigaku, 2002)
k = 3425
Tmin = 0.125, Tmax = 0.567l = 1514
17823 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.043Hydrogen site location: difmap and geom
wR(F2) = 0.111H atoms treated by a mixture of independent and constrained refinement
S = 1.06 w = 1/[σ2(Fo2) + (0.063P)2]
where P = (Fo2 + 2Fc2)/3
5352 reflections(Δ/σ)max = 0.001
358 parametersΔρmax = 2.33 e Å3
3 restraintsΔρmin = 2.45 e Å3
Special details top

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Gd10.08447 (3)0.725781 (11)0.16147 (2)0.01568 (10)
Gd20.40324 (4)0.695017 (11)0.01144 (2)0.01719 (10)
O10.0827 (6)0.65425 (18)0.1484 (4)0.0267 (10)
O20.3697 (5)0.64166 (18)0.0742 (4)0.0265 (10)
O30.0659 (5)0.67768 (16)0.0287 (4)0.0207 (9)
O40.2408 (5)0.61594 (17)0.0493 (4)0.0265 (10)
O50.2605 (5)0.76746 (15)0.0456 (4)0.0186 (9)
O60.1940 (6)0.79896 (18)0.1368 (4)0.0288 (11)
O70.2379 (5)0.79779 (17)0.2683 (4)0.0226 (9)
O80.4840 (6)0.84035 (18)0.3174 (4)0.0285 (10)
O90.3389 (5)0.67518 (16)0.1753 (3)0.0190 (9)
O100.5797 (6)0.71996 (18)0.2356 (4)0.0301 (11)
O110.8887 (6)0.72640 (17)0.5174 (4)0.0262 (10)
O120.6120 (6)0.74871 (18)0.4843 (4)0.0296 (10)
O130.1103 (6)0.7644 (2)0.2597 (4)0.0290 (11)
H13B0.049 (7)0.779 (3)0.322 (4)0.044*
H13C0.208 (5)0.753 (3)0.259 (6)0.044*
C10.2143 (7)0.6330 (2)0.0771 (5)0.0176 (12)
C20.1857 (8)0.5927 (2)0.0063 (6)0.0242 (13)
C30.3072 (9)0.5533 (3)0.0315 (6)0.0316 (15)
H3A0.40140.55460.00020.038*
C40.2925 (10)0.5124 (3)0.1020 (7)0.0432 (19)
H4A0.37400.48630.11620.052*
C50.1549 (10)0.5111 (3)0.1510 (7)0.0385 (17)
H5A0.14350.48410.19910.046*
C60.0347 (9)0.5498 (3)0.1286 (6)0.0301 (15)
H6A0.05710.54850.16270.036*
C70.0457 (8)0.5909 (2)0.0567 (5)0.0218 (12)
C80.0938 (8)0.6310 (2)0.0420 (5)0.0188 (12)
C90.2163 (8)0.8043 (2)0.0273 (6)0.0212 (13)
C100.2006 (8)0.8556 (2)0.0206 (5)0.0227 (13)
C110.1312 (10)0.8939 (3)0.0622 (6)0.0336 (16)
H11A0.08610.88600.14320.040*
C120.1290 (12)0.9432 (3)0.0247 (8)0.046 (2)
H12A0.07910.96840.07990.055*
C130.2015 (12)0.9553 (3)0.0957 (7)0.046 (2)
H13A0.20330.98880.12060.056*
C140.2701 (10)0.9182 (3)0.1775 (6)0.0341 (16)
H14A0.31900.92660.25790.041*
C150.2675 (8)0.8679 (2)0.1417 (6)0.0229 (13)
C160.3397 (8)0.8317 (2)0.2452 (5)0.0210 (12)
C170.4906 (8)0.6840 (2)0.2523 (5)0.0222 (13)
C180.5523 (8)0.6483 (2)0.3545 (5)0.0227 (13)
C190.4945 (9)0.5985 (3)0.3373 (7)0.0346 (16)
H19A0.41560.58880.26470.041*
C200.5541 (11)0.5634 (3)0.4280 (7)0.0435 (19)
H20A0.51470.53010.41690.052*
C210.6716 (11)0.5778 (3)0.5345 (7)0.049 (2)
H21A0.70980.55410.59570.059*
C220.7341 (10)0.6265 (3)0.5526 (7)0.0365 (17)
H22A0.81600.63540.62470.044*
C230.6737 (8)0.6626 (2)0.4618 (5)0.0224 (13)
C240.7293 (8)0.7169 (2)0.4888 (5)0.0219 (13)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Gd10.00978 (16)0.02323 (17)0.01413 (17)0.00045 (10)0.00367 (12)0.00030 (10)
Gd20.01076 (16)0.02425 (18)0.01790 (17)0.00069 (10)0.00627 (12)0.00007 (11)
O10.019 (2)0.037 (3)0.025 (2)0.0074 (19)0.0078 (19)0.003 (2)
O20.012 (2)0.038 (3)0.029 (2)0.0066 (18)0.0069 (18)0.001 (2)
O30.018 (2)0.024 (2)0.019 (2)0.0005 (17)0.0034 (17)0.0001 (18)
O40.015 (2)0.030 (2)0.038 (3)0.0009 (18)0.0139 (19)0.007 (2)
O50.018 (2)0.023 (2)0.016 (2)0.0009 (16)0.0063 (17)0.0009 (17)
O60.031 (3)0.036 (3)0.019 (2)0.003 (2)0.006 (2)0.0029 (19)
O70.019 (2)0.029 (2)0.022 (2)0.0058 (17)0.0080 (18)0.0056 (18)
O80.020 (2)0.041 (3)0.024 (2)0.010 (2)0.0054 (19)0.002 (2)
O90.013 (2)0.029 (2)0.0139 (19)0.0013 (17)0.0022 (16)0.0020 (17)
O100.019 (2)0.034 (3)0.036 (3)0.0042 (19)0.008 (2)0.011 (2)
O110.014 (2)0.035 (3)0.028 (2)0.0064 (17)0.0023 (19)0.0064 (19)
O120.024 (2)0.028 (3)0.039 (3)0.0044 (19)0.013 (2)0.004 (2)
O130.012 (2)0.052 (3)0.025 (2)0.006 (2)0.0083 (19)0.008 (2)
C10.014 (3)0.014 (3)0.027 (3)0.001 (2)0.009 (2)0.004 (2)
C20.013 (3)0.030 (3)0.027 (3)0.001 (2)0.002 (2)0.002 (3)
C30.024 (3)0.030 (4)0.043 (4)0.007 (3)0.013 (3)0.007 (3)
C40.037 (4)0.039 (4)0.057 (5)0.018 (3)0.019 (4)0.015 (4)
C50.043 (5)0.033 (4)0.043 (4)0.008 (3)0.019 (4)0.017 (3)
C60.027 (4)0.031 (4)0.037 (4)0.006 (3)0.017 (3)0.010 (3)
C70.012 (3)0.027 (3)0.024 (3)0.003 (2)0.003 (2)0.001 (3)
C80.018 (3)0.025 (3)0.015 (3)0.000 (2)0.007 (2)0.000 (2)
C90.010 (3)0.035 (4)0.020 (3)0.001 (2)0.006 (2)0.003 (3)
C100.016 (3)0.030 (3)0.024 (3)0.003 (2)0.008 (2)0.002 (3)
C110.037 (4)0.037 (4)0.027 (4)0.006 (3)0.009 (3)0.005 (3)
C120.064 (6)0.028 (4)0.048 (5)0.017 (4)0.020 (4)0.012 (4)
C130.067 (6)0.027 (4)0.053 (5)0.007 (4)0.029 (5)0.006 (4)
C140.048 (5)0.029 (4)0.030 (4)0.003 (3)0.018 (3)0.005 (3)
C150.023 (3)0.022 (3)0.026 (3)0.006 (2)0.009 (3)0.002 (3)
C160.023 (3)0.027 (3)0.015 (3)0.004 (2)0.008 (2)0.005 (2)
C170.018 (3)0.030 (3)0.020 (3)0.005 (3)0.008 (2)0.003 (3)
C180.020 (3)0.025 (3)0.021 (3)0.003 (2)0.003 (2)0.002 (3)
C190.028 (4)0.035 (4)0.037 (4)0.006 (3)0.003 (3)0.000 (3)
C200.046 (5)0.026 (4)0.051 (5)0.006 (3)0.002 (4)0.009 (4)
C210.057 (5)0.034 (4)0.044 (5)0.000 (4)0.005 (4)0.020 (4)
C220.032 (4)0.034 (4)0.034 (4)0.001 (3)0.005 (3)0.009 (3)
C230.012 (3)0.030 (3)0.022 (3)0.000 (2)0.000 (2)0.006 (3)
C240.016 (3)0.032 (3)0.018 (3)0.004 (2)0.006 (2)0.000 (3)
Geometric parameters (Å, º) top
Gd1—O12.293 (4)C2—C71.407 (8)
Gd1—O11i2.306 (4)C3—C41.383 (10)
Gd1—O6ii2.348 (4)C3—H3A0.9300
Gd1—O92.397 (4)C4—C51.378 (10)
Gd1—O72.403 (4)C4—H4A0.9300
Gd1—O132.410 (4)C5—C61.374 (10)
Gd1—O52.474 (4)C5—H5A0.9300
Gd1—O32.521 (4)C6—C71.390 (9)
Gd1—Gd23.7673 (4)C6—H6A0.9300
Gd2—O12iii2.244 (4)C7—C81.511 (8)
Gd2—O2iv2.282 (4)C9—C101.483 (9)
Gd2—O52.418 (4)C10—C151.394 (9)
Gd2—O42.430 (4)C10—C111.396 (9)
Gd2—O92.434 (4)C11—C121.376 (10)
Gd2—O8iii2.453 (4)C11—H11A0.9300
Gd2—O7iii2.525 (4)C12—C131.389 (11)
Gd2—O32.679 (4)C12—H12A0.9300
Gd2—O102.885 (5)C13—C141.366 (11)
C1—O11.263 (7)C13—H13A0.9300
C1—O21.251 (7)C14—C151.391 (9)
C8—O31.270 (7)C14—H14A0.9300
C8—O41.265 (7)C15—C161.515 (9)
C9—O51.273 (7)C17—C181.485 (9)
C9—O61.243 (7)C18—C191.389 (9)
C16—O71.289 (7)C18—C231.391 (9)
C16—O81.232 (7)C19—C201.381 (10)
C17—O91.299 (7)C19—H19A0.9300
C17—O101.236 (8)C20—C211.372 (11)
C24—O111.242 (7)C20—H20A0.9300
C24—O121.248 (7)C21—C221.372 (11)
O13—H13B0.84 (5)C21—H21A0.9300
O13—H13C0.84 (5)C22—C231.402 (9)
C1—C21.504 (8)C22—H22A0.9300
C2—C31.394 (9)C23—C241.507 (9)
O1—Gd1—O11i98.44 (17)Gd1—O13—H13B108 (5)
O1—Gd1—O6ii82.85 (16)Gd1—O13—H13C125 (5)
O11i—Gd1—O6ii148.81 (16)H13B—O13—H13C119 (5)
O1—Gd1—O990.53 (15)O2—C1—O1124.3 (6)
O11i—Gd1—O9137.23 (14)O2—C1—C2116.6 (5)
O6ii—Gd1—O973.63 (15)O1—C1—C2119.0 (5)
O1—Gd1—O7152.29 (14)C3—C2—C7118.4 (6)
O11i—Gd1—O794.40 (16)C3—C2—C1115.9 (5)
O6ii—Gd1—O773.64 (16)C7—C2—C1125.6 (5)
O9—Gd1—O796.56 (14)C4—C3—C2122.2 (6)
O1—Gd1—O1386.39 (16)C4—C3—H3A118.9
O11i—Gd1—O1373.76 (16)C2—C3—H3A118.9
O6ii—Gd1—O1375.23 (17)C5—C4—C3118.9 (7)
O9—Gd1—O13148.85 (15)C5—C4—H4A120.6
O7—Gd1—O1373.76 (15)C3—C4—H4A120.6
O1—Gd1—O5137.99 (14)C6—C5—C4120.0 (7)
O11i—Gd1—O574.36 (15)C6—C5—H5A120.0
O6ii—Gd1—O5124.48 (15)C4—C5—H5A120.0
O9—Gd1—O571.31 (14)C5—C6—C7122.1 (6)
O7—Gd1—O569.25 (14)C5—C6—H6A118.9
O13—Gd1—O5128.25 (16)C7—C6—H6A118.9
O1—Gd1—O369.05 (14)C6—C7—C2118.4 (6)
O11i—Gd1—O377.50 (15)C6—C7—C8116.2 (5)
O6ii—Gd1—O3130.41 (15)C2—C7—C8125.3 (6)
O9—Gd1—O366.92 (13)O4—C8—O3120.9 (5)
O7—Gd1—O3138.11 (14)O4—C8—C7116.0 (5)
O13—Gd1—O3138.66 (14)O3—C8—C7123.0 (5)
O5—Gd1—O368.99 (13)O4—C8—Gd254.9 (3)
O12iii—Gd2—O2iv85.41 (17)O3—C8—Gd266.2 (3)
O12iii—Gd2—O583.91 (15)C7—C8—Gd2170.7 (4)
O2iv—Gd2—O5138.30 (15)O6—C9—O5121.7 (6)
O12iii—Gd2—O4157.74 (16)O6—C9—C10119.2 (6)
O2iv—Gd2—O482.00 (16)O5—C9—C10119.0 (5)
O5—Gd2—O4117.49 (14)C15—C10—C11119.1 (6)
O12iii—Gd2—O9120.99 (16)C15—C10—C9123.0 (6)
O2iv—Gd2—O979.89 (14)C11—C10—C9117.6 (6)
O5—Gd2—O971.65 (14)C12—C11—C10120.5 (7)
O4—Gd2—O974.70 (14)C12—C11—H11A119.8
O12iii—Gd2—O8iii82.01 (17)C10—C11—H11A119.8
O2iv—Gd2—O8iii75.87 (15)C11—C12—C13119.9 (7)
O5—Gd2—O8iii141.46 (14)C11—C12—H12A120.0
O4—Gd2—O8iii77.17 (15)C13—C12—H12A120.0
O9—Gd2—O8iii144.96 (15)C14—C13—C12120.1 (7)
O12iii—Gd2—O7iii95.60 (16)C14—C13—H13A119.9
O2iv—Gd2—O7iii127.02 (15)C12—C13—H13A119.9
O5—Gd2—O7iii94.13 (14)C13—C14—C15120.7 (7)
O4—Gd2—O7iii77.77 (15)C13—C14—H14A119.7
O9—Gd2—O7iii137.75 (13)C15—C14—H14A119.7
O8iii—Gd2—O7iii52.13 (14)C14—C15—C10119.6 (6)
O12iii—Gd2—O3147.94 (15)C14—C15—C16113.4 (6)
O2iv—Gd2—O3125.35 (14)C10—C15—C16127.0 (6)
O5—Gd2—O367.19 (13)O8—C16—O7120.4 (6)
O4—Gd2—O350.85 (13)O8—C16—C15119.1 (6)
O9—Gd2—O363.89 (13)O7—C16—C15119.3 (5)
O8iii—Gd2—O3111.79 (14)O8—C16—Gd2ii60.2 (3)
O7iii—Gd2—O373.89 (13)O7—C16—Gd2ii63.5 (3)
O12iii—Gd2—O1073.90 (15)C15—C16—Gd2ii150.7 (4)
O2iv—Gd2—O1067.19 (15)O10—C17—O9119.4 (6)
O5—Gd2—O1071.11 (14)O10—C17—C18123.0 (6)
O4—Gd2—O10117.12 (14)O9—C17—C18117.6 (6)
O9—Gd2—O1047.68 (13)O10—C17—Gd274.4 (4)
O8iii—Gd2—O10136.91 (14)O9—C17—Gd254.0 (3)
O7iii—Gd2—O10162.42 (14)C18—C17—Gd2144.8 (4)
O3—Gd2—O10107.43 (12)C19—C18—C23120.1 (6)
C1—O1—Gd1139.9 (4)C19—C18—C17117.9 (6)
C1—O2—Gd2v141.1 (4)C23—C18—C17121.8 (6)
C8—O3—Gd1129.0 (4)C20—C19—C18120.0 (7)
C8—O3—Gd288.1 (3)C20—C19—H19A120.0
Gd1—O3—Gd292.80 (13)C18—C19—H19A120.0
C8—O4—Gd299.9 (4)C21—C20—C19119.8 (7)
C9—O5—Gd2118.9 (4)C21—C20—H20A120.1
C9—O5—Gd1127.9 (4)C19—C20—H20A120.1
Gd2—O5—Gd1100.72 (15)C20—C21—C22121.3 (7)
C9—O6—Gd1iii163.4 (4)C20—C21—H21A119.3
C16—O7—Gd1134.2 (4)C22—C21—H21A119.3
C16—O7—Gd2ii89.2 (3)C21—C22—C23119.6 (7)
Gd1—O7—Gd2ii128.39 (18)C21—C22—H22A120.2
C16—O8—Gd2ii94.0 (3)C23—C22—H22A120.2
C17—O9—Gd1123.1 (4)C18—C23—C22119.2 (6)
C17—O9—Gd2100.4 (3)C18—C23—C24122.1 (5)
Gd1—O9—Gd2102.49 (15)C22—C23—C24118.5 (6)
C17—O10—Gd281.2 (4)O11—C24—O12124.9 (6)
C24—O11—Gd1vi136.7 (4)O11—C24—C23117.6 (5)
C24—O12—Gd2ii176.4 (4)O12—C24—C23117.5 (6)
Symmetry codes: (i) x1, y+3/2, z1/2; (ii) x, y+3/2, z+1/2; (iii) x, y+3/2, z1/2; (iv) x+1, y, z; (v) x1, y, z; (vi) x+1, y+3/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O13—H13B···O3ii0.84 (5)2.06 (6)2.893 (6)171 (8)
O13—H13C···O10v0.84 (5)1.85 (6)2.677 (6)170 (6)
Symmetry codes: (ii) x, y+3/2, z+1/2; (v) x1, y, z.
 

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