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The title compound, {[Er2(C4H4O4)3(H2O)2]·H2O}n, is isostructural with other Ln–succinates of the same formula. The ErIII atom is nine-coordinated by O atoms.
Supporting information
CCDC reference: 640337
Key indicators
- Single-crystal X-ray study
- T = 273 K
- Mean (C-C) = 0.007 Å
- H-atom completeness 89%
- R factor = 0.024
- wR factor = 0.066
- Data-to-parameter ratio = 12.0
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O2W
| Author Response: The attached H atoms could not be located.
|
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ?
PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) . 20 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 2
PLAT731_ALERT_1_C Bond Calc 0.85(5), Rep 0.84(2) ...... 2.50 su-Ra
O1W -H1WB 1.555 1.555
PLAT764_ALERT_4_C Overcomplete CIF Bond List Detected (Rep/Expd) . 1.20 Ratio
Alert level G
FORMU01_ALERT_2_G There is a discrepancy between the atom counts in the
_chemical_formula_sum and the formula from the _atom_site* data.
Atom count from _chemical_formula_sum:C12 H18 Er2 O15
Atom count from the _atom_site data: C12 H16 Er2 O15
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
From the CIF: _cell_formula_units_Z 4
From the CIF: _chemical_formula_sum C12 H18 Er2 O15
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 48.00 48.00 0.00
H 72.00 64.00 8.00
Er 8.00 8.00 0.00
O 60.00 60.00 0.00
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
7 ALERT level C = Check and explain
3 ALERT level G = General alerts; check
7 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
2 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
2 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: SMART (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; 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: SHELXTL (Bruker, 2004).
Poly[[diaqua-µ
6-succinato-di-µ
5-succinato-dierbium(III)] monohydrate]
top
Crystal data top
[Er2(C4H4O4)3(H2O)2]·H2O | F(000) = 1384 |
Mr = 736.78 | Dx = 2.725 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 1696 reflections |
a = 19.8837 (2) Å | θ = 2.9–25.7° |
b = 7.6642 (2) Å | µ = 9.36 mm−1 |
c = 13.8194 (2) Å | T = 273 K |
β = 121.50 (1)° | Prism, pale red |
V = 1795.7 (2) Å3 | 0.55 × 0.24 × 0.14 mm |
Z = 4 | |
Data collection top
Bruker SMART CCD diffractometer | 1696 independent reflections |
Radiation source: fine-focus sealed tube | 1632 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.030 |
Detector resolution: none pixels mm-1 | θmax = 25.7°, θmin = 2.9° |
ω scans | h = −21→24 |
Absorption correction: multi-scan (SADABS; Bruker, 2004) | k = −9→9 |
Tmin = 0.076, Tmax = 0.272 | l = −16→11 |
4673 measured reflections | |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.025 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.066 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.08 | w = 1/[σ2(Fo2) + (0.0422P)2 + 9.2468P] where P = (Fo2 + 2Fc2)/3 |
1696 reflections | (Δ/σ)max = 0.001 |
141 parameters | Δρmax = 1.04 e Å−3 |
3 restraints | Δρmin = −1.89 e Å−3 |
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 | x | y | z | Uiso*/Ueq | |
Er1 | 0.268891 (11) | 0.71774 (2) | 0.229942 (15) | 0.01082 (11) | |
O1 | 0.18749 (18) | 0.9827 (4) | 0.1379 (3) | 0.0183 (7) | |
C1 | 0.1533 (2) | 0.9153 (6) | 0.0383 (3) | 0.0144 (8) | |
O2 | 0.1717 (2) | 0.7632 (4) | 0.0287 (3) | 0.0202 (7) | |
C2 | 0.0905 (2) | 1.0169 (6) | −0.0621 (4) | 0.0165 (9) | |
H2A | 0.0513 | 1.0566 | −0.0454 | 0.020* | |
H2B | 0.0644 | 0.9398 | −0.1272 | 0.020* | |
O3 | 0.1797 (2) | 0.9720 (4) | −0.1594 (3) | 0.0213 (7) | |
C3 | 0.1229 (3) | 1.1756 (6) | −0.0930 (4) | 0.0187 (9) | |
H3A | 0.0790 | 1.2493 | −0.1449 | 0.022* | |
H3B | 0.1561 | 1.2428 | −0.0246 | 0.022* | |
O4 | 0.1968 (2) | 1.2561 (5) | −0.1773 (3) | 0.0225 (8) | |
C4 | 0.1703 (2) | 1.1298 (6) | −0.1470 (4) | 0.0145 (8) | |
O5 | 0.32251 (17) | 0.9824 (4) | 0.3389 (2) | 0.0160 (6) | |
C5 | 0.3944 (2) | 0.9237 (6) | 0.3931 (4) | 0.0156 (9) | |
O6 | 0.4057 (2) | 0.7700 (4) | 0.3781 (3) | 0.0219 (7) | |
C6 | 0.4601 (3) | 1.0441 (6) | 0.4692 (4) | 0.0255 (10) | |
H6A | 0.4495 | 1.0930 | 0.5246 | 0.031* | |
H6B | 0.4615 | 1.1398 | 0.4243 | 0.031* | |
O1W | 0.3330 (2) | 0.8875 (4) | 0.1527 (3) | 0.0209 (7) | |
O2W | 0.5000 | 0.9747 (17) | 0.2500 | 0.116 (4) | |
H1WA | 0.322 (3) | 0.993 (3) | 0.140 (5) | 0.024 (15)* | |
H1WB | 0.329 (4) | 0.855 (9) | 0.091 (3) | 0.035 (17)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Er1 | 0.01238 (16) | 0.00863 (17) | 0.01225 (15) | −0.00043 (6) | 0.00699 (12) | −0.00013 (6) |
O1 | 0.0176 (15) | 0.0178 (16) | 0.0144 (14) | 0.0001 (12) | 0.0047 (13) | −0.0048 (12) |
C1 | 0.013 (2) | 0.020 (2) | 0.0132 (19) | −0.0040 (17) | 0.0089 (17) | 0.0005 (17) |
O2 | 0.0285 (19) | 0.0131 (14) | 0.0171 (17) | 0.0005 (13) | 0.0105 (15) | 0.0014 (13) |
C2 | 0.014 (2) | 0.024 (2) | 0.0131 (19) | 0.0006 (17) | 0.0085 (17) | 0.0016 (17) |
O3 | 0.0310 (18) | 0.0123 (15) | 0.0314 (18) | 0.0017 (13) | 0.0238 (16) | −0.0003 (13) |
C3 | 0.026 (2) | 0.0155 (19) | 0.022 (2) | 0.0045 (19) | 0.018 (2) | 0.0033 (19) |
O4 | 0.031 (2) | 0.0154 (14) | 0.034 (2) | −0.0011 (15) | 0.0264 (19) | −0.0001 (15) |
C4 | 0.015 (2) | 0.015 (2) | 0.015 (2) | 0.0012 (16) | 0.0082 (17) | 0.0007 (16) |
O5 | 0.0123 (14) | 0.0177 (15) | 0.0151 (14) | 0.0015 (12) | 0.0052 (12) | −0.0042 (12) |
C5 | 0.014 (2) | 0.019 (2) | 0.0129 (19) | 0.0023 (17) | 0.0057 (17) | 0.0045 (17) |
O6 | 0.0178 (17) | 0.0132 (16) | 0.0271 (19) | −0.0001 (12) | 0.0065 (15) | 0.0012 (13) |
C6 | 0.014 (2) | 0.018 (2) | 0.032 (3) | −0.0005 (19) | 0.004 (2) | −0.005 (2) |
O1W | 0.0307 (19) | 0.0169 (16) | 0.0231 (17) | −0.0026 (14) | 0.0197 (15) | −0.0025 (14) |
O2W | 0.108 (8) | 0.097 (8) | 0.149 (10) | 0.000 | 0.071 (8) | 0.000 |
Geometric parameters (Å, º) top
Er1—O3i | 2.270 (3) | C1—C2 | 1.510 (6) |
Er1—O5ii | 2.378 (3) | C2—C3 | 1.537 (6) |
Er1—O4iii | 2.378 (4) | C2—H2A | 0.9700 |
Er1—O1ii | 2.383 (3) | C2—H2B | 0.9700 |
Er1—O5 | 2.417 (3) | O3—Er1i | 2.270 (3) |
Er1—O1W | 2.425 (3) | C3—C4 | 1.518 (6) |
Er1—O6 | 2.436 (4) | C3—H3A | 0.9700 |
Er1—O2 | 2.444 (3) | C3—H3B | 0.9700 |
Er1—O1 | 2.492 (3) | O4—Er1v | 2.378 (4) |
C1—O1 | 1.282 (5) | O5—Er1iv | 2.378 (3) |
C1—O2 | 1.250 (6) | C5—C6 | 1.493 (6) |
C4—O3 | 1.249 (5) | C6—C6vi | 1.514 (9) |
C4—O4 | 1.274 (6) | C6—H6A | 0.9700 |
C5—O5 | 1.299 (5) | C6—H6B | 0.9700 |
C5—O6 | 1.237 (6) | O1W—H1WA | 0.83 (2) |
O1—Er1iv | 2.383 (3) | O1W—H1WB | 0.84 (2) |
| | | |
O3i—Er1—O5ii | 76.35 (11) | Er1iv—O1—Er1 | 110.20 (11) |
O3i—Er1—O4iii | 144.99 (12) | O2—C1—O1 | 118.0 (4) |
O5ii—Er1—O4iii | 74.32 (12) | O2—C1—C2 | 122.1 (4) |
O3i—Er1—O1ii | 77.29 (11) | O1—C1—C2 | 119.9 (4) |
O5ii—Er1—O1ii | 68.24 (11) | C1—O2—Er1 | 96.5 (3) |
O4iii—Er1—O1ii | 74.39 (12) | C1—C2—C3 | 113.5 (4) |
O3i—Er1—O5 | 130.86 (11) | C1—C2—H2A | 108.9 |
O5ii—Er1—O5 | 151.89 (3) | C3—C2—H2A | 108.9 |
O4iii—Er1—O5 | 77.72 (12) | C1—C2—H2B | 108.9 |
O1ii—Er1—O5 | 106.95 (11) | C3—C2—H2B | 108.9 |
O3i—Er1—O1W | 72.31 (12) | H2A—C2—H2B | 107.7 |
O5ii—Er1—O1W | 134.32 (11) | C4—O3—Er1i | 144.3 (3) |
O4iii—Er1—O1W | 142.70 (12) | C4—C3—C2 | 114.3 (4) |
O1ii—Er1—O1W | 132.74 (11) | C4—C3—H3A | 108.7 |
O5—Er1—O1W | 70.22 (11) | C2—C3—H3A | 108.7 |
O3i—Er1—O6 | 84.87 (12) | C4—C3—H3B | 108.7 |
O5ii—Er1—O6 | 138.20 (10) | C2—C3—H3B | 108.7 |
O4iii—Er1—O6 | 104.83 (14) | H3A—C3—H3B | 107.6 |
O1ii—Er1—O6 | 71.37 (11) | C4—O4—Er1v | 135.3 (3) |
O5—Er1—O6 | 53.34 (10) | O3—C4—O4 | 125.0 (4) |
O1W—Er1—O6 | 70.65 (12) | O3—C4—C3 | 117.9 (4) |
O3i—Er1—O2 | 82.43 (12) | O4—C4—C3 | 117.1 (4) |
O5ii—Er1—O2 | 70.63 (11) | C5—O5—Er1iv | 150.9 (3) |
O4iii—Er1—O2 | 105.09 (13) | C5—O5—Er1 | 93.6 (3) |
O1ii—Er1—O2 | 137.29 (11) | Er1iv—O5—Er1 | 113.04 (11) |
O5—Er1—O2 | 114.73 (10) | O6—C5—O5 | 118.4 (4) |
O1W—Er1—O2 | 73.00 (12) | O6—C5—C6 | 122.5 (4) |
O6—Er1—O2 | 143.60 (12) | O5—C5—C6 | 119.1 (4) |
O3i—Er1—O1 | 128.37 (11) | C5—O6—Er1 | 94.4 (3) |
O5ii—Er1—O1 | 104.90 (10) | C5—C6—C6vi | 113.2 (5) |
O4iii—Er1—O1 | 78.06 (12) | C5—C6—H6A | 108.9 |
O1ii—Er1—O1 | 152.44 (3) | C6vi—C6—H6A | 108.9 |
O5—Er1—O1 | 65.89 (10) | C5—C6—H6B | 108.9 |
O1W—Er1—O1 | 71.85 (11) | C6vi—C6—H6B | 108.9 |
O6—Er1—O1 | 115.93 (10) | H6A—C6—H6B | 107.7 |
O2—Er1—O1 | 52.15 (10) | Er1—O1W—H1WA | 118 (4) |
C1—O1—Er1iv | 154.6 (3) | Er1—O1W—H1WB | 119 (5) |
C1—O1—Er1 | 93.4 (3) | H1WA—O1W—H1WB | 101 (6) |
Symmetry codes: (i) −x+1/2, −y+3/2, −z; (ii) −x+1/2, y−1/2, −z+1/2; (iii) x, −y+2, z+1/2; (iv) −x+1/2, y+1/2, −z+1/2; (v) x, −y+2, z−1/2; (vi) −x+1, −y+2, −z+1. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1W—H1WA···O4vii | 0.83 (3) | 2.08 (3) | 2.853 (5) | 156 (6) |
O1W—H1WB···O2i | 0.85 (5) | 1.88 (6) | 2.717 (5) | 168 (6) |
Symmetry codes: (i) −x+1/2, −y+3/2, −z; (vii) −x+1/2, −y+5/2, −z. |
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