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The title compound, {[Ce(C5H6O5)(H2O)4]Cl·2H2O}n, is a coordination polymer built up from binuclear units extending along [100] with the ligands as spacers. The complex polymers are held together by inter­layer hydrogen bonds involving the counter-ion and the solvent water mol­ecules embedded in the structure. The tetra­dentate glutarate dianion coordinates in a bridging–chelating mode, with one triply ligating O atom, and in a conventional carboxyl­ate bridge to the water-coordinated CeIII ion. In the centered cage assembly, two nine-coordinated CeIII ions are linked through six oxo bridges.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806030741/xu2099sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806030741/xu2099Isup2.hkl
Contains datablock I

CCDC reference: 621550

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.003 Å
  • R factor = 0.017
  • wR factor = 0.034
  • Data-to-parameter ratio = 24.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 1 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 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 0 ALERT type 5 Informative message, check

Computing details top

Data collection: DENZO (Otwinowski & Minor, 1997); cell refinement: DENZO; data reduction: DENZO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 (Farrugia, 1997); software used to prepare material for publication: WinGX (Farrugia, 1999).

Poly[[tetraaqua-µ4-glutarato-cerium(III)] chloride dihydrate] top
Crystal data top
[Ce(C5H6O4)(H2O)4]Cl·2H2OZ = 2
Mr = 413.76F(000) = 406
Triclinic, P1Dx = 2.096 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.932 (5) ÅCell parameters from 21564 reflections
b = 8.803 (5) Åθ = 3.5–30.0°
c = 10.509 (5) ŵ = 3.71 mm1
α = 110.500 (5)°T = 100 K
β = 95.531 (5)°Prism, colourless
γ = 103.439 (5)°0.60 × 0.30 × 0.20 mm
V = 655.7 (6) Å3
Data collection top
Nonius KappaCCD area-detector
diffractometer
3827 independent reflections
Radiation source: fine-focus sealed tube3561 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
ω scansθmax = 30.0°, θmin = 3.5°
Absorption correction: empirical (using intensity measurements)
(DIFABS; Walker & Stuart, 1983)
h = 1111
Tmin = 0.254, Tmax = 0.476k = 1212
21564 measured reflectionsl = 1411
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)] = 0.017Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.034H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0151P)2 + 0.3197P]
where P = (Fo2 + 2Fc2)/3
3827 reflections(Δ/σ)max = 0.001
154 parametersΔρmax = 1.83 e Å3
0 restraintsΔρmin = 0.99 e Å3
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
O10.68431 (16)0.59638 (15)0.50985 (12)0.0098 (2)
O20.37375 (17)0.68194 (15)0.40535 (12)0.0109 (2)
O30.17130 (16)0.22319 (16)0.28234 (12)0.0116 (2)
O40.56069 (16)0.21155 (15)0.36169 (12)0.0099 (2)
O1W0.76092 (17)0.39701 (16)0.20186 (14)0.0150 (3)
H110.78910.31490.16840.022*
H120.82910.46760.19010.022*
O2W0.61657 (17)0.66570 (16)0.21681 (14)0.0142 (3)
H210.54050.67840.16300.021*
H220.70560.69450.20410.021*
O3W0.23648 (18)0.46833 (16)0.13784 (13)0.0158 (3)
H310.18280.41730.05930.024*
H320.19900.54920.16750.024*
O4W0.39806 (17)0.18317 (16)0.05783 (12)0.0130 (3)
H410.45890.17530.00510.020*
H420.30780.09310.02100.020*
O5W0.56947 (17)0.12130 (15)0.83394 (13)0.0119 (2)
H510.66900.15160.83320.018*
H520.53220.02500.78290.018*
O6W0.12111 (17)0.88340 (16)0.93030 (13)0.0123 (2)
H610.08650.85350.98500.018*
H620.04390.86440.87290.018*
C50.3719 (2)0.7876 (2)0.52214 (17)0.0083 (3)
C40.2811 (2)0.9241 (2)0.52772 (17)0.0082 (3)
H4A0.23690.91210.43230.010*
H4B0.36761.03710.57590.010*
C30.1259 (2)0.9098 (2)0.60438 (17)0.0089 (3)
H3A0.16950.91950.69920.011*
H3B0.07321.00330.61200.011*
C20.9857 (2)0.7403 (2)0.52639 (18)0.0125 (3)
H2A0.94510.73290.43170.015*
H2B1.04230.64890.51720.015*
C10.8255 (2)0.7069 (2)0.59004 (17)0.0089 (3)
Cl10.99395 (5)0.27253 (5)0.84452 (4)0.01088 (8)
Ce10.474519 (13)0.428248 (12)0.289380 (10)0.00656 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0069 (6)0.0104 (6)0.0091 (6)0.0001 (5)0.0006 (5)0.0018 (5)
O20.0134 (6)0.0108 (6)0.0084 (6)0.0055 (5)0.0028 (5)0.0019 (5)
O30.0090 (6)0.0140 (6)0.0084 (6)0.0005 (5)0.0014 (5)0.0027 (5)
O40.0115 (6)0.0096 (6)0.0092 (6)0.0041 (5)0.0013 (5)0.0038 (5)
O1W0.0132 (6)0.0099 (6)0.0251 (7)0.0053 (5)0.0114 (6)0.0074 (5)
O2W0.0110 (6)0.0165 (6)0.0227 (7)0.0061 (5)0.0075 (5)0.0142 (6)
O3W0.0184 (7)0.0127 (6)0.0120 (6)0.0071 (5)0.0048 (5)0.0002 (5)
O4W0.0138 (6)0.0116 (6)0.0094 (6)0.0003 (5)0.0041 (5)0.0008 (5)
O5W0.0107 (6)0.0098 (6)0.0135 (6)0.0023 (5)0.0023 (5)0.0031 (5)
O6W0.0104 (6)0.0156 (6)0.0106 (6)0.0026 (5)0.0005 (5)0.0057 (5)
C50.0056 (7)0.0087 (7)0.0104 (7)0.0002 (6)0.0024 (6)0.0043 (6)
C40.0078 (8)0.0078 (7)0.0092 (7)0.0022 (6)0.0024 (6)0.0035 (6)
C30.0112 (8)0.0093 (8)0.0080 (7)0.0045 (6)0.0050 (6)0.0036 (6)
C20.0107 (8)0.0110 (8)0.0120 (8)0.0003 (7)0.0038 (7)0.0016 (6)
C10.0091 (8)0.0074 (7)0.0109 (8)0.0023 (6)0.0018 (6)0.0046 (6)
Cl10.00973 (19)0.01243 (19)0.01020 (18)0.00304 (15)0.00198 (15)0.00410 (15)
Ce10.00636 (5)0.00653 (4)0.00644 (4)0.00161 (3)0.00126 (3)0.00223 (3)
Geometric parameters (Å, º) top
O1—C11.284 (2)O3W—H310.8051
O1—Ce12.4572 (15)O3W—H320.8078
O1—Ce1i2.6061 (16)O4W—Ce12.5246 (15)
O2—C51.258 (2)O4W—H410.7647
O2—Ce12.4945 (16)O4W—H420.8714
O3—C1i1.259 (2)O5W—H510.7736
O3—Ce12.6273 (18)O5W—H520.7925
O4—C5i1.282 (2)O6W—H610.7604
O4—Ce12.4910 (16)O6W—H620.7601
O1W—Ce12.5687 (18)C4—H4A0.9900
O1W—H110.7803C4—H4B0.9900
O1W—H120.7779C3—H3A0.9900
O2W—Ce12.5314 (16)C3—H3B0.9900
O2W—H210.8400C2—H2A0.9900
O2W—H220.7346C2—H2B0.9900
O3W—Ce12.5198 (16)
C1—O1—Ce1156.05 (11)O1—Ce1—O3W137.71 (5)
C1—O1—Ce1i94.85 (10)O4—Ce1—O3W142.53 (4)
Ce1—O1—Ce1i108.33 (6)O2—Ce1—O3W65.61 (5)
C5—O2—Ce1142.98 (11)O1—Ce1—O4W147.98 (4)
C1i—O3—Ce194.48 (10)O4—Ce1—O4W80.12 (6)
C5i—O4—Ce1133.80 (11)O2—Ce1—O4W137.96 (5)
Ce1—O1W—H11128.8O3W—Ce1—O4W72.40 (5)
Ce1—O1W—H12124.9O1—Ce1—O2W84.69 (5)
H11—O1W—H12105.3O4—Ce1—O2W138.56 (5)
Ce1—O2W—H21109.5O2—Ce1—O2W70.05 (6)
Ce1—O2W—H22132.2O3W—Ce1—O2W72.26 (5)
H21—O2W—H22110.8O4W—Ce1—O2W99.48 (6)
Ce1—O3W—H31134.9O1—Ce1—O1W81.73 (6)
Ce1—O3W—H32120.1O4—Ce1—O1W73.83 (4)
H31—O3W—H32105.0O2—Ce1—O1W131.93 (4)
Ce1—O4W—H41122.6O3W—Ce1—O1W118.49 (6)
Ce1—O4W—H42131.5O4W—Ce1—O1W71.07 (5)
H41—O4W—H42105.9O2W—Ce1—O1W67.18 (5)
H51—O5W—H52108.3O3W—Ce1—O1i100.89 (6)
H61—O6W—H62108.9O4W—Ce1—O1i120.38 (5)
C5—C4—H4A109.5O2W—Ce1—O1i135.90 (4)
C3—C4—H4A109.5O1W—Ce1—O1i140.28 (4)
C5—C4—H4B109.5O3W—Ce1—O371.99 (6)
C3—C4—H4B109.5O4W—Ce1—O373.26 (5)
H4A—C4—H4B108.1O2W—Ce1—O3144.03 (4)
C2ii—C3—H3A109.6O1W—Ce1—O3136.38 (5)
C4—C3—H3A109.6O1i—Ce1—O349.75 (4)
C2ii—C3—H3B109.6O3W—Ce1—C1i84.13 (6)
C4—C3—H3B109.6O4W—Ce1—C1i97.39 (5)
H3A—C3—H3B108.1O2W—Ce1—C1i145.03 (4)
C1—C2—H2A108.2O1W—Ce1—C1i147.73 (5)
C3iii—C2—H2A108.2O3W—Ce1—Ce1i124.24 (4)
C1—C2—H2B108.2O4W—Ce1—Ce1i145.94 (3)
C3iii—C2—H2B108.2O2W—Ce1—Ce1i113.60 (4)
H2A—C2—H2B107.3O1W—Ce1—Ce1i113.72 (4)
Ce1—O2—C5—O4i0.0 (3)Ce1—O1—C1—Ce1i165.6 (3)
Ce1—O2—C5—C4179.16 (12)C3iii—C2—C1—O3i25.0 (2)
O2—C5—C4—C3118.84 (17)C3iii—C2—C1—O1158.32 (15)
O4i—C5—C4—C360.4 (2)C3iii—C2—C1—Ce1i127.5 (5)
C5—C4—C3—C2ii62.67 (18)C1—O1—Ce1—O4120.3 (3)
Ce1—O1—C1—O3i155.20 (19)Ce1i—O1—Ce1—O474.83 (5)
Ce1i—O1—C1—O3i10.37 (16)C1—O1—Ce1—O293.3 (3)
Ce1—O1—C1—C228.0 (4)Ce1i—O1—Ce1—O271.50 (6)
Ce1i—O1—C1—C2166.40 (13)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x1, y, z; (iii) x+1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H11···O6Wi0.782.022.797 (3)173
O1W—H12···Cl1iv0.782.553.321 (3)169
O2W—H21···O5Wi0.842.132.795 (3)135
O2W—H22···Cl1iv0.742.463.179 (2)167
O3W—H31···Cl1v0.812.333.125 (2)172
O3W—H32···Cl1i0.812.463.207 (3)155
O4W—H41···O5Wvi0.772.032.783 (3)167
O4W—H42···O6Wvii0.871.932.801 (3)175
O5W—H51···Cl10.772.523.296 (3)176
O5W—H52···O4viii0.792.012.801 (3)175
O6W—H61···Cl1ix0.762.483.229 (2)171
O6W—H62···O3x0.762.042.788 (3)171
Symmetry codes: (i) x+1, y+1, z+1; (iv) x+2, y+1, z+1; (v) x1, y, z1; (vi) x, y, z1; (vii) x, y1, z1; (viii) x+1, y, z+1; (ix) x+1, y+1, z+2; (x) x, y+1, z+1.
 

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