Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804032635/cf6390sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536804032635/cf6390Isup2.hkl |
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).
[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 |
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 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) |
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. |
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)* |
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 |
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. |
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. |
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