The title compound, {[Er(C4H4O4)(H2O)3]Cl·2H2O}n, crystallizes with an infinite polymeric structure, in which erbium(III) ions on twofold rotation axes are bridged by centrosymmetric succinate dianions. The carboxylate groups of the dicarboxylate coordinate in a tridentate-bridging manner to the otherwise water-coordinated ErIII ion. The structure is completed by Cl− anions and uncoordinated water molecules.
Supporting information
CCDC reference: 262268
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.005 Å
- R factor = 0.020
- wR factor = 0.051
- Data-to-parameter ratio = 14.7
checkCIF/PLATON results
No syntax errors found
Alert level A
DIFF022_ALERT_1_A _diffrn_standards_decay_% is missing
Percentage decrease in standards intensity.
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT199_ALERT_1_C Check the Reported cell_measurement_temperature 293
PLAT200_ALERT_1_C Check the Reported cell_ambient_temperature .... 293
PLAT731_ALERT_1_C Bond Calc 0.82(5), Rep 0.809(19) ...... 2.63 su-Rat
O2 -H3 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.82(7), Rep 0.81(2) ...... 3.50 su-Rat
O4 -H4 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.82(5), Rep 0.81(2) ...... 2.50 su-Rat
O4 -H5 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.82(5), Rep 0.809(19) ...... 2.63 su-Rat
O2 -H3 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.82(7), Rep 0.81(2) ...... 3.50 su-Rat
O4 -H4 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.82(5), Rep 0.81(2) ...... 2.50 su-Rat
O4 -H5 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 2.03(5), Rep 2.03(2) ...... 2.50 su-Rat
H3 -O4 1.555 8.556
PLAT736_ALERT_1_C H...A Calc 2.32(7), Rep 2.32(3) ...... 2.33 su-Rat
H4 -CL1 1.555 3.455
PLAT736_ALERT_1_C H...A Calc 2.31(6), Rep 2.31(2) ...... 3.00 su-Rat
H5 -CL1 1.555 7.646
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.23 Ratio
Alert level G
ABSTM02_ALERT_3_G The ratio of expected to reported Tmax/Tmin(RR) is > 1.10
Tmin and Tmax reported: 0.308 0.370
Tmin and Tmax expected: 0.261 0.461
RR = 1.472
Please check that your absorption correction is appropriate.
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
13 ALERT level C = Check and explain
1 ALERT level G = General alerts; check
13 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
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: IPDS program system (Stoe & Cie, 1996); cell refinement: IPDS program system; data reduction: IPDS program system; program(s) used to solve structure: SIR92 (Altomare et al., 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 1996); software used to prepare material for publication: CIF-Editor (Wieczorrek, 2004).
Poly[[[triaquaerbium(III)]-µ
3-succinato] chloride dihydrate]
top
Crystal data top
[Er(C4H4O4)(H2O)3]Cl·2H2O | F(000) = 780 |
Mr = 408.86 | Dx = 2.421 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 5000 reflections |
a = 13.047 (2) Å | θ = 2.4–28.0° |
b = 11.6893 (14) Å | µ = 7.75 mm−1 |
c = 7.8244 (12) Å | T = 293 K |
β = 109.954 (17)° | Block, light pink |
V = 1121.6 (3) Å3 | 0.2 × 0.15 × 0.1 mm |
Z = 4 | |
Data collection top
Stoe IPDS I diffractometer | 1348 independent reflections |
Radiation source: fine-focus sealed tube | 1234 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
φ scans | θmax = 28.0°, θmin = 2.4° |
Absorption correction: numerical [X-RED (Stoe & Cie, 2001); crystal shape optimized by X-SHAPE (Stoe &
Cie, 1999)] | h = −17→17 |
Tmin = 0.308, Tmax = 0.370 | k = −15→15 |
6684 measured reflections | l = −10→10 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.020 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.051 | w = 1/[σ2(Fo2) + (0.0329P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.12 | (Δ/σ)max = 0.001 |
1348 reflections | Δρmax = 1.08 e Å−3 |
92 parameters | Δρmin = −0.77 e Å−3 |
5 restraints | Extinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
Primary atom site location: structure-invariant direct methods | Extinction coefficient: 0.0022 (2) |
Special details top
Experimental. A suitable single-crystal was carefully selected under a polarizing microscope
and mounted in a glass capillary. The scattering intensities were collected on
an imaging plate diffractometer (IPDS I, Stoe & Cie) equipped with a
fine focus sealed tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at 50 kV and 40 mA. Intensity data for the title compound were collected at room
temperature by φ scans in 125 frames (0 < φ < 250°, Δφ = 2°, exposure
time of 4 min) in the 2 θ range 3.8 to 56.3°. Structure solution and
refinement were carried out using the programs SIR92 (Altomare et
al., 1993) and SHELXL97 (Sheldrick, 1997). A numerical absorption
correction (X-RED (Stoe & Cie, 2001) was applied after optimization of
the crystal shape (X-SHAPE (Stoe & Cie, 1999)). The last cycles of
refinement included atomic positions for all atoms, anisotropic parameters for
all non-H atoms and isotropic displacement parameters for all H atoms. The
final difference maps were free of any chemically significant features. The
refinement was based on F2 for ALL reflections. |
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 | x | y | z | Uiso*/Ueq | |
Er1 | 1.0000 | 0.055401 (19) | 0.7500 | 0.01014 (10) | |
C1 | 1.1357 (3) | −0.1338 (3) | 0.9504 (5) | 0.0117 (7) | |
O11 | 1.1311 (2) | −0.0985 (2) | 0.7967 (4) | 0.0190 (6) | |
O12 | 1.0729 (2) | −0.0890 (2) | 1.0270 (4) | 0.0168 (5) | |
C2 | 1.2164 (3) | −0.2242 (3) | 1.0525 (5) | 0.0161 (7) | |
H2A | 1.1768 | −0.2851 | 1.0869 | 0.042 (12)* | |
H2B | 1.2656 | −0.1905 | 1.1636 | 0.042 (12)* | |
O2 | 1.0000 | 0.2559 (4) | 0.7500 | 0.0296 (11) | |
O3 | 0.8403 (3) | 0.1303 (3) | 0.5313 (4) | 0.0209 (6) | |
O4 | 0.6308 (3) | 0.0783 (4) | 0.4887 (6) | 0.0393 (9) | |
Cl1 | 1.0000 | −0.37771 (16) | 0.7500 | 0.0386 (4) | |
H3 | 1.047 (3) | 0.298 (4) | 0.815 (6) | 0.019 (12)* | |
H4 | 0.605 (6) | 0.085 (6) | 0.570 (8) | 0.05 (2)* | |
H5 | 0.602 (6) | 0.021 (4) | 0.433 (10) | 0.06 (2)* | |
H6 | 0.831 (5) | 0.126 (6) | 0.423 (3) | 0.040 (18)* | |
H7 | 0.780 (2) | 0.116 (4) | 0.532 (7) | 0.018 (12)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Er1 | 0.01051 (13) | 0.01088 (13) | 0.01024 (14) | 0.000 | 0.00511 (8) | 0.000 |
C1 | 0.0109 (17) | 0.0129 (15) | 0.0122 (18) | 0.0037 (12) | 0.0050 (14) | 0.0001 (12) |
O11 | 0.0229 (15) | 0.0229 (13) | 0.0131 (14) | 0.0069 (11) | 0.0087 (11) | 0.0035 (11) |
O12 | 0.0162 (14) | 0.0175 (12) | 0.0189 (15) | 0.0059 (10) | 0.0088 (11) | 0.0001 (10) |
C2 | 0.0162 (18) | 0.0189 (17) | 0.0140 (19) | 0.0089 (14) | 0.0062 (15) | 0.0046 (14) |
O2 | 0.029 (2) | 0.018 (2) | 0.030 (3) | 0.000 | −0.005 (2) | 0.000 |
O3 | 0.0182 (15) | 0.0269 (14) | 0.0179 (16) | 0.0030 (12) | 0.0067 (12) | −0.0003 (11) |
O4 | 0.0268 (19) | 0.047 (2) | 0.044 (2) | −0.0086 (16) | 0.0120 (17) | −0.0029 (18) |
Cl1 | 0.0345 (9) | 0.0371 (9) | 0.0430 (11) | 0.000 | 0.0117 (8) | 0.000 |
Geometric parameters (Å, º) top
Er1—O12i | 2.289 (3) | C1—O12 | 1.280 (4) |
Er1—O12ii | 2.289 (3) | C1—C2 | 1.513 (5) |
Er1—O2 | 2.344 (4) | O12—Er1ii | 2.289 (3) |
Er1—O3iii | 2.367 (3) | C2—C2iv | 1.518 (7) |
Er1—O3 | 2.367 (3) | C2—H2A | 0.970 |
Er1—O11iii | 2.423 (3) | C2—H2B | 0.970 |
Er1—O11 | 2.423 (3) | O2—H3 | 0.809 (19) |
Er1—O12iii | 2.654 (3) | O3—H6 | 0.82 (2) |
Er1—O12 | 2.654 (3) | O3—H7 | 0.80 (2) |
Er1—C1iii | 2.931 (3) | O4—H4 | 0.81 (2) |
Er1—C1 | 2.931 (3) | O4—H5 | 0.81 (2) |
C1—O11 | 1.254 (5) | | |
| | | |
O12i—Er1—O12ii | 160.26 (14) | O2—Er1—C1iii | 139.00 (7) |
O12i—Er1—O2 | 80.13 (7) | O3iii—Er1—C1iii | 152.60 (10) |
O12ii—Er1—O2 | 80.13 (7) | O3—Er1—C1iii | 70.76 (11) |
O12i—Er1—O3iii | 89.73 (10) | O11iii—Er1—C1iii | 24.84 (10) |
O12ii—Er1—O3iii | 82.99 (11) | O11—Er1—C1iii | 77.69 (10) |
O2—Er1—O3iii | 68.29 (8) | O12iii—Er1—C1iii | 25.89 (9) |
O12i—Er1—O3 | 82.99 (10) | O12—Er1—C1iii | 86.55 (10) |
O12ii—Er1—O3 | 89.73 (10) | O12i—Er1—C1 | 101.83 (10) |
O2—Er1—O3 | 68.29 (8) | O12ii—Er1—C1 | 93.08 (10) |
O3iii—Er1—O3 | 136.58 (15) | O2—Er1—C1 | 139.00 (7) |
O12i—Er1—O11iii | 117.92 (9) | O3iii—Er1—C1 | 70.76 (11) |
O12ii—Er1—O11iii | 77.66 (10) | O3—Er1—C1 | 152.60 (10) |
O2—Er1—O11iii | 137.94 (7) | O11iii—Er1—C1 | 77.69 (10) |
O3iii—Er1—O11iii | 141.80 (10) | O11—Er1—C1 | 24.84 (10) |
O3—Er1—O11iii | 76.32 (11) | O12iii—Er1—C1 | 86.55 (10) |
O12i—Er1—O11 | 77.66 (10) | O12—Er1—C1 | 25.89 (9) |
O12ii—Er1—O11 | 117.92 (9) | C1iii—Er1—C1 | 82.00 (14) |
O2—Er1—O11 | 137.94 (7) | O11—C1—O12 | 119.1 (3) |
O3iii—Er1—O11 | 76.32 (11) | O11—C1—C2 | 122.2 (3) |
O3—Er1—O11 | 141.80 (10) | O12—C1—C2 | 118.7 (3) |
O11iii—Er1—O11 | 84.12 (15) | O11—C1—Er1 | 54.27 (18) |
O12i—Er1—O12iii | 67.22 (10) | O12—C1—Er1 | 64.87 (19) |
O12ii—Er1—O12iii | 127.24 (10) | C2—C1—Er1 | 173.7 (3) |
O2—Er1—O12iii | 129.49 (6) | C1—O11—Er1 | 100.9 (2) |
O3iii—Er1—O12iii | 143.85 (10) | C1—O12—Er1ii | 157.8 (3) |
O3—Er1—O12iii | 70.31 (10) | C1—O12—Er1 | 89.2 (2) |
O11iii—Er1—O12iii | 50.71 (9) | Er1ii—O12—Er1 | 112.78 (10) |
O11—Er1—O12iii | 71.88 (10) | C1—C2—C2iv | 114.8 (4) |
O12i—Er1—O12 | 127.24 (10) | C1—C2—H2A | 108.6 |
O12ii—Er1—O12 | 67.22 (10) | C2iv—C2—H2A | 108.6 |
O2—Er1—O12 | 129.49 (6) | C1—C2—H2B | 108.6 |
O3iii—Er1—O12 | 70.31 (10) | C2iv—C2—H2B | 108.6 |
O3—Er1—O12 | 143.85 (10) | H2A—C2—H2B | 107.6 |
O11iii—Er1—O12 | 71.88 (10) | Er1—O2—H3 | 127 (4) |
O11—Er1—O12 | 50.71 (9) | Er1—O3—H6 | 121 (5) |
O12iii—Er1—O12 | 101.03 (12) | Er1—O3—H7 | 123 (4) |
O12i—Er1—C1iii | 93.08 (10) | H6—O3—H7 | 101 (6) |
O12ii—Er1—C1iii | 101.83 (10) | H4—O4—H5 | 105 (8) |
Symmetry codes: (i) x, −y, z−1/2; (ii) −x+2, −y, −z+2; (iii) −x+2, y, −z+3/2; (iv) −x+5/2, −y−1/2, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O2—H3···O4v | 0.81 (2) | 2.03 (2) | 2.825 (5) | 165 (5) |
O4—H4···Cl1vi | 0.81 (2) | 2.32 (3) | 3.120 (4) | 167 (8) |
O4—H5···Cl1vii | 0.81 (2) | 2.31 (2) | 3.118 (4) | 171 (8) |
O3—H6···O11viii | 0.82 (2) | 1.97 (3) | 2.742 (4) | 157 (7) |
O3—H7···O4 | 0.80 (2) | 1.91 (2) | 2.707 (5) | 170 (5) |
Symmetry codes: (v) x+1/2, −y+1/2, z+1/2; (vi) x−1/2, y+1/2, z; (vii) −x+3/2, −y−1/2, −z+1; (viii) −x+2, −y, −z+1. |