Buy article online - an online subscription or single-article purchase is required to access this article.
Download citation
Download citation
link to html
The title compound, {[Yb2(C4H4O4)3(H2O)4]·6H2O}n, is a two-dimensional open-framework built up from centrosymmetric binuclear units developed along [100] through the spacers of four extended ligands, and inter­connected along [101] by two twisted ligands, forming a layered coordination polymer in the (010) plane embedding six uncoordinated water mol­ecules. The water-coordinated YbIII atom completes a nine-coordination mode via seven O atoms from four carboxyl­ate ligands, in a monocapped square anti­prism. One independent succinate ligand, located on an inversion center, is in a bidentate coordination mode, exhibiting an anti conformation. The second independent succinate ligand, in a gauche conformation, is bidentate and bridging–chelating, involving one triply ligating O atom displaying the longest Yb—O bond [2.598 (2) Å]. In addition to inter­layer hydrogen bonds, intra­layer hydrogen bonds involve, as acceptors, carboxyl­ate O atoms which are in bidentate mode.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806036002/lh2170sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806036002/lh2170Isup2.hkl
Contains datablock I

CCDC reference: 624907

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.024
  • wR factor = 0.065
  • Data-to-parameter ratio = 27.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT417_ALERT_2_C Short Inter D-H..H-D H31 .. H41 .. 2.13 Ang.
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 1 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 0 ALERT type 3 Indicator that the structure quality may be low 0 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: KappaCCD Software (Nonius, 1999); cell refinement: DIRAX/LSQ (Duisenberg, 1992); data reduction: EVALCCD (Duisenberg et al., 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Poly[[tetraaquadi-µ4-succinato-µ5– succinato-diyterbium (III)] hexahydrate] top
Crystal data top
[Yb2(C4H4O4)3(H2O)4]·3H2OZ = 2
Mr = 437.23F(000) = 420
Triclinic, P1Dx = 2.389 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 6.457 (5) ÅCell parameters from 29166 reflections
b = 9.741 (5) Åθ = 2.7–35.0°
c = 10.384 (5) ŵ = 7.75 mm1
α = 79.959 (5)°T = 100 K
β = 89.571 (5)°Prism, colourless
γ = 71.133 (5)°0.46 × 0.17 × 0.05 mm
V = 607.7 (6) Å3
Data collection top
Nonius KappaCCD
diffractometer
5330 independent reflections
Radiation source: fine-focus sealed tube5008 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.059
ω scansθmax = 35.0°, θmin = 2.7°
Absorption correction: numerical
(ABSORB; De Titta, 1988)
h = 1010
Tmin = 0.184, Tmax = 0.690k = 1515
29166 measured reflectionsl = 1616
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)] = 0.024H-atom parameters constrained
wR(F2) = 0.065 w = 1/[σ2(Fo2) + (0.0401P)2 + 1.5702P]
where P = (Fo2 + 2Fc2)/3
S = 1.06(Δ/σ)max = 0.002
5330 reflectionsΔρmax = 2.23 e Å3
194 parametersΔρmin = 3.31 e Å3
8 restraintsExtinction correction: SHELXL97, Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.0182 (9)
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 > 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 (Å2) top
xyzUiso*/Ueq
O10.4061 (3)0.4799 (2)0.65756 (19)0.0110 (3)
O20.0736 (3)0.6188 (2)0.68644 (19)0.0109 (3)
O30.0647 (3)0.8547 (2)0.8291 (2)0.0124 (3)
O40.0889 (3)0.6516 (2)0.96694 (19)0.0118 (3)
O50.4523 (3)0.6052 (2)1.05179 (19)0.0108 (3)
O60.4807 (4)0.7948 (2)0.8968 (2)0.0144 (3)
O1W0.7492 (3)0.5203 (2)0.80455 (19)0.0106 (3)
H110.82600.56230.76980.016*
H120.81120.46460.86920.016*
O2W0.4192 (3)0.7800 (2)0.63939 (19)0.0116 (3)
H210.51290.81930.63830.017*
H220.38420.77470.56510.017*
O3W0.7253 (4)0.9190 (2)0.6092 (2)0.0159 (4)
H310.69921.01490.62850.024*
H320.84790.86470.66640.024*
O4W0.3216 (4)0.7853 (2)0.3887 (2)0.0152 (4)
H420.39530.70000.36060.023*
H410.18890.80180.37120.023*
O5W0.1228 (4)0.8914 (2)0.3504 (2)0.0172 (4)
H510.14470.97060.30350.026*
H520.16570.90240.41750.026*
C10.2022 (4)0.5244 (3)0.6266 (2)0.0082 (4)
C20.1206 (4)0.4635 (3)0.5207 (3)0.0113 (4)
H2A0.14810.35680.55190.014*
H2B0.20760.47360.44290.014*
C30.0028 (4)0.7909 (3)0.9312 (2)0.0081 (3)
C40.1651 (4)0.8771 (3)1.0150 (3)0.0107 (4)
H4A0.27290.96150.95770.013*
H4B0.09070.91721.07480.013*
C50.2862 (4)0.7836 (3)1.0958 (2)0.0090 (4)
H5A0.17910.69981.15410.011*
H5B0.38860.84411.15150.011*
C60.4124 (4)0.7252 (3)1.0101 (2)0.0084 (4)
Yb10.374655 (14)0.625982 (10)0.822076 (9)0.00615 (4)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0074 (7)0.0148 (8)0.0115 (7)0.0025 (6)0.0004 (6)0.0065 (6)
O20.0085 (7)0.0146 (8)0.0110 (7)0.0037 (6)0.0008 (6)0.0059 (6)
O30.0159 (8)0.0096 (7)0.0131 (8)0.0062 (6)0.0049 (6)0.0020 (6)
O40.0101 (7)0.0118 (8)0.0101 (7)0.0002 (6)0.0030 (6)0.0001 (6)
O50.0123 (8)0.0100 (7)0.0123 (8)0.0061 (6)0.0031 (6)0.0031 (6)
O60.0187 (9)0.0129 (8)0.0117 (8)0.0064 (7)0.0057 (7)0.0000 (6)
O1W0.0078 (7)0.0134 (8)0.0091 (7)0.0032 (6)0.0001 (6)0.0010 (6)
O2W0.0131 (8)0.0154 (8)0.0080 (7)0.0075 (7)0.0007 (6)0.0008 (6)
O3W0.0146 (9)0.0149 (9)0.0172 (9)0.0062 (7)0.0039 (7)0.0027 (7)
O4W0.0149 (9)0.0150 (9)0.0150 (8)0.0022 (7)0.0007 (7)0.0061 (7)
O5W0.0189 (10)0.0128 (8)0.0189 (9)0.0037 (7)0.0024 (8)0.0028 (7)
C10.0087 (9)0.0103 (9)0.0068 (8)0.0042 (7)0.0002 (7)0.0025 (7)
C20.0104 (9)0.0141 (10)0.0113 (9)0.0042 (8)0.0015 (7)0.0064 (8)
C30.0063 (8)0.0108 (9)0.0086 (8)0.0045 (7)0.0003 (7)0.0025 (7)
C40.0111 (9)0.0112 (9)0.0125 (9)0.0059 (8)0.0047 (8)0.0050 (8)
C50.0078 (9)0.0132 (10)0.0085 (8)0.0055 (7)0.0012 (7)0.0043 (7)
C60.0059 (8)0.0085 (9)0.0120 (9)0.0026 (7)0.0003 (7)0.0047 (7)
Yb10.00535 (5)0.00769 (6)0.00600 (5)0.00274 (3)0.00011 (3)0.00163 (3)
Geometric parameters (Å, º) top
O1—C11.271 (3)C1—C21.508 (4)
O1—Yb12.375 (2)C2—C2i1.518 (5)
O2—C11.272 (3)C2—H2A0.9900
O2—Yb12.435 (2)C2—H2B0.9900
O3—C31.263 (3)C3—C41.513 (4)
O3—Yb12.479 (2)C4—C51.525 (4)
O4—C31.276 (3)C4—H4A0.9900
O4—Yb12.350 (2)C4—H4B0.9900
O1W—Yb12.322 (3)C5—C61.505 (3)
O1W—H110.7881C5—H5A0.9900
O1W—H120.8010C5—H5B0.9900
O2W—Yb12.283 (2)C6—O61.255 (3)
O2W—H210.8133C6—O51.279 (3)
O2W—H220.8200Yb1—O5ii2.300 (2)
O3W—H310.9516Yb1—O6iii2.372 (2)
O3W—H320.9412Yb1—O5iii2.589 (2)
O5W—H510.8072O4W—H420.9103
O5W—H520.7603O4W—H410.8344
C1—O1—Yb195.08 (15)O5ii—Yb1—O3129.75 (7)
C1—O2—Yb192.21 (15)O1W—Yb1—O3146.85 (7)
C3—O3—Yb189.93 (16)O4—Yb1—O353.90 (7)
C3—O4—Yb195.57 (15)O6iii—Yb1—O372.48 (9)
H11—O1W—H12110.1O1—Yb1—O3123.98 (7)
H21—O2W—H22111.2O2—Yb1—O373.17 (8)
H31—O3W—H32100.4O2W—Yb1—O5iii123.98 (7)
H51—O5W—H52109.7O5ii—Yb1—O5iii66.97 (8)
O1—C1—O2118.6 (2)O1W—Yb1—O5iii74.90 (7)
O1—C1—C2119.1 (2)O4—Yb1—O5iii73.61 (8)
O2—C1—C2122.3 (2)O6iii—Yb1—O5iii52.08 (7)
O1—C1—Yb157.95 (13)O1—Yb1—O5iii138.84 (7)
O2—C1—Yb160.69 (13)O2—Yb1—O5iii149.65 (6)
C2—C1—Yb1177.00 (18)O3—Yb1—O5iii96.15 (7)
C1—C2—C2i115.1 (3)O2W—Yb1—C3105.02 (8)
O3—C3—O4119.3 (2)O5ii—Yb1—C3102.88 (7)
O3—C3—C4121.4 (2)O1W—Yb1—C3154.83 (7)
O4—C3—C4119.3 (2)O4—Yb1—C327.17 (7)
O3—C3—Yb163.05 (14)O6iii—Yb1—C381.08 (9)
O4—C3—Yb157.26 (13)O1—Yb1—C3129.81 (7)
C4—C3—Yb1167.56 (17)O2—Yb1—C376.31 (8)
C3—C4—C5112.8 (2)O3—Yb1—C327.02 (7)
C3—C4—H4A109.0O5iii—Yb1—C381.79 (8)
C5—C4—H4A109.0O2W—Yb1—C178.95 (8)
C3—C4—H4B109.0O5ii—Yb1—C188.08 (8)
C5—C4—H4B109.0O1W—Yb1—C1102.00 (8)
H4A—C4—H4B107.8O4—Yb1—C199.46 (9)
C6—C5—C4111.7 (2)O6iii—Yb1—C1152.47 (7)
C6—C5—H5A109.3O1—Yb1—C126.97 (7)
C4—C5—H5A109.3O2—Yb1—C127.10 (7)
C6—C5—H5B109.3O3—Yb1—C198.79 (8)
C4—C5—H5B109.3O5iii—Yb1—C1154.99 (7)
H5A—C5—H5B107.9C3—Yb1—C1103.14 (8)
O6—C6—O5119.3 (2)O2W—Yb1—C6iii98.15 (8)
O6—C6—C5120.0 (2)O5ii—Yb1—C6iii92.61 (8)
O5—C6—C5120.7 (2)O1W—Yb1—C6iii73.16 (8)
O6—C6—Yb1iv54.78 (13)O4—Yb1—C6iii85.71 (9)
O5—C6—Yb1iv64.73 (13)O6iii—Yb1—C6iii25.61 (7)
C5—C6—Yb1iv173.23 (17)O1—Yb1—C6iii148.36 (7)
O2W—Yb1—O5ii151.23 (7)O2—Yb1—C6iii157.34 (7)
O2W—Yb1—O1W80.97 (7)O3—Yb1—C6iii84.74 (8)
O5ii—Yb1—O1W76.75 (7)O5iii—Yb1—C6iii26.53 (7)
O2W—Yb1—O4131.32 (7)C3—Yb1—C6iii81.74 (8)
O5ii—Yb1—O475.85 (7)C1—Yb1—C6iii174.79 (7)
O1W—Yb1—O4144.33 (7)O2W—Yb1—H1295.9
O2W—Yb1—O6iii73.73 (8)O5ii—Yb1—H1264.0
O5ii—Yb1—O6iii117.86 (8)O1W—Yb1—H1215.5
O1W—Yb1—O6iii77.19 (8)O4—Yb1—H12129.0
O4—Yb1—O6iii96.04 (8)O6iii—Yb1—H1277.6
O2W—Yb1—O177.77 (8)O1—Yb1—H1282.2
O5ii—Yb1—O179.11 (8)O2—Yb1—H12135.7
O1W—Yb1—O175.21 (7)O3—Yb1—H12150.0
O4—Yb1—O1120.79 (8)O5iii—Yb1—H1262.7
O6iii—Yb1—O1142.85 (8)C3—Yb1—H12144.5
O2W—Yb1—O282.38 (8)C1—Yb1—H12108.9
O5ii—Yb1—O297.63 (7)C6iii—Yb1—H1266.9
O1W—Yb1—O2128.86 (8)H42—O4W—H41106.4
O4—Yb1—O277.35 (9)C6—O5—Yb1ii153.38 (17)
O6iii—Yb1—O2141.37 (7)C6—O5—Yb1iv88.74 (15)
O1—Yb1—O254.07 (7)Yb1ii—O5—Yb1iv113.03 (8)
O2W—Yb1—O378.02 (8)C6—O6—Yb1iv99.62 (16)
Yb1—O1—C1—O20.4 (2)O3—C3—Yb1—O2W1.66 (16)
Yb1—O1—C1—C2179.4 (2)O4—C3—Yb1—O2W166.99 (15)
Yb1—O2—C1—O10.4 (2)C4—C3—Yb1—O2W115.5 (8)
Yb1—O2—C1—C2179.4 (2)O3—C3—Yb1—O5ii174.58 (14)
O1—C1—C2—C2i172.9 (3)O4—C3—Yb1—O5ii5.93 (16)
O2—C1—C2—C2i7.3 (4)C4—C3—Yb1—O5ii71.5 (8)
Yb1—O3—C3—O410.9 (2)O3—C3—Yb1—O1W99.2 (2)
Yb1—O3—C3—C4166.7 (2)O4—C3—Yb1—O1W92.1 (2)
Yb1—O4—C3—O311.6 (2)C4—C3—Yb1—O1W14.7 (9)
Yb1—O4—C3—C4166.05 (18)O3—C3—Yb1—O4168.7 (2)
O3—C3—C4—C5156.0 (2)C4—C3—Yb1—O477.5 (8)
O4—C3—C4—C526.3 (3)O3—C3—Yb1—O6iii68.72 (15)
Yb1—C3—C4—C596.6 (8)O4—C3—Yb1—O6iii122.63 (16)
C3—C4—C5—C661.5 (3)C4—C3—Yb1—O6iii45.2 (8)
C4—C5—C6—O627.5 (3)O3—C3—Yb1—O188.11 (17)
C4—C5—C6—O5152.8 (2)O4—C3—Yb1—O180.54 (17)
C3—O4—Yb1—O2W16.83 (19)C4—C3—Yb1—O1158.0 (8)
C3—O4—Yb1—O5ii174.04 (16)O3—C3—Yb1—O279.73 (15)
C3—O4—Yb1—O1W133.21 (15)O4—C3—Yb1—O288.92 (16)
C3—O4—Yb1—O6iii56.79 (16)C4—C3—Yb1—O2166.4 (8)
C3—O4—Yb1—O1118.11 (15)O4—C3—Yb1—O3168.7 (2)
C3—O4—Yb1—O284.60 (15)C4—C3—Yb1—O3113.9 (8)
C3—O4—Yb1—O36.35 (14)O3—C3—Yb1—O5iii121.43 (15)
C3—O4—Yb1—O5iii104.31 (15)O4—C3—Yb1—O5iii69.92 (15)
C3—O4—Yb1—C1100.38 (15)C4—C3—Yb1—O5iii7.5 (8)
C3—O4—Yb1—C6iii80.25 (15)O3—C3—Yb1—C183.54 (15)
C1—O1—Yb1—O2W89.62 (16)O4—C3—Yb1—C185.11 (16)
C1—O1—Yb1—O5ii107.63 (16)C4—C3—Yb1—C1162.6 (8)
C1—O1—Yb1—O1W173.37 (17)O3—C3—Yb1—C6iii94.62 (15)
C1—O1—Yb1—O441.48 (18)O4—C3—Yb1—C6iii96.73 (16)
C1—O1—Yb1—O6iii130.09 (16)C4—C3—Yb1—C6iii19.3 (8)
C1—O1—Yb1—O20.22 (14)O1—C1—Yb1—O2W84.72 (16)
C1—O1—Yb1—O323.34 (18)O2—C1—Yb1—O2W94.88 (16)
C1—O1—Yb1—O5iii141.99 (14)O1—C1—Yb1—O5ii69.46 (16)
C1—O1—Yb1—C39.86 (19)O2—C1—Yb1—O5ii110.93 (16)
C1—O1—Yb1—C6iii175.30 (14)O1—C1—Yb1—O1W6.56 (16)
C1—O2—Yb1—O2W80.61 (16)O2—C1—Yb1—O1W173.05 (15)
C1—O2—Yb1—O5ii70.36 (16)O1—C1—Yb1—O4144.77 (16)
C1—O2—Yb1—O1W8.74 (18)O2—C1—Yb1—O435.62 (16)
C1—O2—Yb1—O4143.93 (16)O1—C1—Yb1—O6iii91.8 (2)
C1—O2—Yb1—O6iii132.28 (16)O2—C1—Yb1—O6iii87.8 (2)
C1—O2—Yb1—O10.22 (14)O2—C1—Yb1—O1179.6 (3)
C1—O2—Yb1—O3160.33 (16)O1—C1—Yb1—O2179.6 (3)
C1—O2—Yb1—O5iii126.83 (16)O1—C1—Yb1—O3160.58 (15)
C1—O2—Yb1—C3171.83 (16)O2—C1—Yb1—O319.02 (16)
C1—O2—Yb1—C6iii173.51 (16)O1—C1—Yb1—O5iii73.4 (2)
C3—O3—Yb1—O2W178.36 (16)O2—C1—Yb1—O5iii107.0 (2)
C3—O3—Yb1—O5ii6.88 (18)O1—C1—Yb1—C3172.24 (15)
C3—O3—Yb1—O1W129.84 (15)O2—C1—Yb1—C38.15 (16)
C3—O3—Yb1—O46.39 (14)O6—C6—O5—Yb1ii151.0 (3)
C3—O3—Yb1—O6iii105.13 (16)C5—C6—O5—Yb1ii29.4 (5)
C3—O3—Yb1—O1112.20 (15)Yb1iv—C6—O5—Yb1ii146.1 (4)
C3—O3—Yb1—O292.80 (15)O6—C6—O5—Yb1iv5.0 (2)
C3—O3—Yb1—O5iii58.15 (15)C5—C6—O5—Yb1iv175.4 (2)
C3—O3—Yb1—C1101.73 (15)O5—C6—O6—Yb1iv5.5 (3)
C3—O3—Yb1—C6iii82.14 (15)C5—C6—O6—Yb1iv174.87 (18)
Symmetry codes: (i) x, y+1, z+1; (ii) x, y+1, z+2; (iii) x+1, y, z; (iv) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H11···O2iii0.791.9972.768 (4)165
O1W—H12···O4v0.801.8612.654 (3)170
O2W—H21···O3W0.811.9152.722 (4)172
O2W—H22···O4W0.821.8572.671 (4)171
O3W—H31···O4Wvi0.951.8832.801 (3)161
O3W—H32···O3iii0.942.1713.017 (4)149
O3W—H32···O2iii0.942.3413.035 (4)130
O4W—H42···O1vii0.911.8462.735 (3)164
O4W—H41···O5W0.831.9142.723 (4)163
O5W—H51···O3viii0.802.1912.952 (4)157
O5W—H52···O3Wiv0.762.1212.880 (4)176
Symmetry codes: (iii) x+1, y, z; (iv) x1, y, z; (v) x+1, y+1, z+2; (vi) x+1, y+2, z+1; (vii) x+1, y+1, z+1; (viii) x, y+2, z+1.
 

Subscribe to Acta Crystallographica Section E: Crystallographic Communications

The full text of this article is available to subscribers to the journal.

If you have already registered and are using a computer listed in your registration details, please email support@iucr.org for assistance.

Buy online

You may purchase this article in PDF and/or HTML formats. For purchasers in the European Community who do not have a VAT number, VAT will be added at the local rate. Payments to the IUCr are handled by WorldPay, who will accept payment by credit card in several currencies. To purchase the article, please complete the form below (fields marked * are required), and then click on `Continue'.
E-mail address* 
Repeat e-mail address* 
(for error checking) 

Format*   PDF (US $40)
   HTML (US $40)
   PDF+HTML (US $50)
In order for VAT to be shown for your country javascript needs to be enabled.

VAT number 
(non-UK EC countries only) 
Country* 
 

Terms and conditions of use
Contact us

Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds