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The water-coordinated Ca atom in the layer structure of the title compound, [Ca(C10H8O6)(H2O)2]n, is connected to a carboxyl O atom of one —O—CH2—CO2 arm of the dicarboxylate dianion; it is also linked to an O atom of a carboxylate group of this arm of an adjacent dianion, as well as to the O atoms of the other arm of two different dianions. The six-coordinate octahedral geometry is distorted, owing to a weak interaction with the ether O atom of one of the arms; the dianion functions in a μ4-bridging mode.
Supporting information
CCDC reference: 261034
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.009 Å
- R factor = 0.061
- wR factor = 0.203
- Data-to-parameter ratio = 12.4
checkCIF/PLATON results
No syntax errors found
Alert level C
ABSTM02_ALERT_3_C The ratio of expected to reported Tmax/Tmin(RR') is < 0.90
Tmin and Tmax reported: 0.638 0.923
Tmin' and Tmax expected: 0.806 0.922
RR' = 0.791
Please check that your absorption correction is appropriate.
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.79
PLAT127_ALERT_1_C Implicit Hall Symbol Inconsistent with Explicit -P 2yc
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for Ca1
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 9
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 4
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
8 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 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
3 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
poly[[diaquacalcium(II)]-µ
4-benzene-1,3-dioxyacetato]
top
Crystal data top
[Ca(C10H8O6)(H2O)2] | F(000) = 624 |
Mr = 300.28 | Dx = 1.623 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yc | Cell parameters from 9802 reflections |
a = 15.795 (3) Å | θ = 3.3–27.5° |
b = 7.917 (2) Å | µ = 0.54 mm−1 |
c = 9.829 (2) Å | T = 295 K |
β = 90.65 (3)° | Prism, colorless |
V = 1229.0 (4) Å3 | 0.39 × 0.26 × 0.15 mm |
Z = 4 | |
Data collection top
Rigaku R-AXIS-RAPID diffractometer | 2153 independent reflections |
Radiation source: fine-focus sealed tube | 1933 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.040 |
ω scans | θmax = 25.0°, θmin = 3.3° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −18→18 |
Tmin = 0.638, Tmax = 0.923 | k = −9→9 |
9687 measured reflections | l = −11→11 |
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)] = 0.061 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.203 | H-atom parameters constrained |
S = 1.11 | w = 1/[σ2(Fo2) + (0.1067P)2 + 4.6656P] where P = (Fo2 + 2Fc2)/3 |
2153 reflections | (Δ/σ)max = 0.001 |
173 parameters | Δρmax = 0.38 e Å−3 |
0 restraints | Δρmin = −0.96 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca1 | 0.6398 (1) | 0.4604 (1) | 0.315 (1) | 0.0279 (4) | |
O1 | 0.6002 (3) | 0.6325 (6) | 0.4971 (5) | 0.043 (1) | |
O2 | 0.6221 (3) | 0.8152 (6) | 0.6611 (6) | 0.047 (1) | |
O3 | 0.7458 (3) | 0.7036 (6) | 0.3826 (5) | 0.041 (1) | |
O4 | 0.8931 (3) | 1.1001 (6) | 0.0910 (5) | 0.037 (1) | |
O5 | 0.6951 (3) | 1.3101 (6) | 0.1307 (5) | 0.038 (1) | |
O6 | 0.7447 (3) | 1.1687 (6) | −0.0463 (5) | 0.043 (1) | |
O1w | 0.5671 (3) | 0.2318 (6) | 0.4330 (6) | 0.040 (1) | |
O2w | 0.4985 (4) | 0.4383 (8) | 0.2220 (7) | 0.059 (2) | |
C1 | 0.6406 (4) | 0.7506 (8) | 0.5503 (7) | 0.031 (1) | |
C2 | 0.7146 (4) | 0.8237 (8) | 0.4755 (7) | 0.037 (2) | |
C3 | 0.8124 (4) | 0.7531 (8) | 0.3015 (7) | 0.033 (1) | |
C4 | 0.8728 (4) | 0.6315 (8) | 0.2781 (7) | 0.037 (2) | |
C5 | 0.9380 (4) | 0.6689 (8) | 0.1874 (8) | 0.040 (2) | |
C6 | 0.9426 (4) | 0.8253 (8) | 0.1263 (7) | 0.036 (2) | |
C7 | 0.8824 (4) | 0.9469 (8) | 0.1557 (7) | 0.032 (2) | |
C8 | 0.8161 (4) | 0.9121 (9) | 0.2433 (8) | 0.037 (2) | |
C9 | 0.8408 (4) | 1.2363 (8) | 0.1334 (7) | 0.034 (1) | |
C10 | 0.7529 (4) | 1.2358 (8) | 0.0674 (7) | 0.031 (1) | |
H1w1 | 0.5192 | 0.2674 | 0.4599 | 0.048* | |
H1w2 | 0.5972 | 0.2034 | 0.5017 | 0.048* | |
H2w1 | 0.4620 | 0.4020 | 0.2775 | 0.070* | |
H2w2 | 0.4804 | 0.5268 | 0.1828 | 0.070* | |
H2a | 0.6971 | 0.9248 | 0.4271 | 0.045* | |
H2b | 0.7590 | 0.8545 | 0.5399 | 0.045* | |
H4 | 0.8704 | 0.5272 | 0.3214 | 0.044* | |
H5 | 0.9786 | 0.5874 | 0.1683 | 0.049* | |
H6 | 0.9859 | 0.8490 | 0.0658 | 0.043* | |
H8 | 0.7754 | 0.9934 | 0.2623 | 0.044* | |
H9a | 0.8688 | 1.3419 | 0.1118 | 0.041* | |
H9b | 0.8348 | 1.2310 | 0.2314 | 0.041* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca1 | 0.0276 (6) | 0.0221 (6) | 0.0340 (6) | 0.0008 (5) | 0.0046 (6) | 0.0006 (5) |
O1 | 0.038 (3) | 0.043 (3) | 0.048 (3) | −0.012 (2) | 0.018 (2) | −0.016 (2) |
O2 | 0.042 (3) | 0.043 (3) | 0.056 (3) | −0.008 (2) | 0.014 (2) | −0.020 (2) |
O3 | 0.041 (3) | 0.026 (2) | 0.058 (3) | −0.004 (2) | 0.022 (2) | −0.004 (2) |
O4 | 0.028 (2) | 0.028 (2) | 0.055 (3) | 0.000 (2) | 0.009 (2) | 0.007 (2) |
O5 | 0.035 (2) | 0.039 (3) | 0.041 (3) | 0.010 (2) | 0.007 (2) | −0.005 (2) |
O6 | 0.035 (2) | 0.051 (3) | 0.043 (3) | 0.004 (2) | 0.000 (2) | −0.018 (2) |
O1w | 0.030 (2) | 0.039 (3) | 0.049 (3) | −0.009 (2) | −0.001 (2) | 0.007 (2) |
O2w | 0.036 (3) | 0.063 (4) | 0.076 (5) | −0.008 (3) | −0.001 (3) | 0.030 (3) |
C1 | 0.026 (3) | 0.024 (3) | 0.041 (3) | 0.003 (3) | 0.005 (3) | −0.007 (3) |
C2 | 0.038 (3) | 0.030 (3) | 0.044 (4) | −0.005 (3) | 0.010 (3) | −0.007 (3) |
C3 | 0.031 (3) | 0.027 (3) | 0.043 (4) | −0.003 (3) | 0.011 (3) | 0.000 (3) |
C4 | 0.036 (3) | 0.026 (3) | 0.048 (4) | 0.000 (3) | 0.006 (3) | 0.002 (3) |
C5 | 0.028 (3) | 0.032 (3) | 0.061 (4) | 0.008 (3) | 0.004 (3) | −0.007 (3) |
C6 | 0.025 (3) | 0.033 (3) | 0.050 (4) | 0.001 (3) | 0.010 (3) | 0.000 (3) |
C7 | 0.025 (3) | 0.030 (3) | 0.041 (4) | −0.005 (2) | 0.004 (3) | 0.000 (3) |
C8 | 0.029 (3) | 0.030 (3) | 0.052 (4) | 0.004 (3) | 0.011 (3) | −0.002 (3) |
C9 | 0.033 (3) | 0.026 (3) | 0.043 (3) | −0.004 (3) | −0.001 (3) | −0.002 (3) |
C10 | 0.029 (3) | 0.022 (3) | 0.041 (3) | −0.002 (3) | 0.000 (3) | −0.001 (3) |
Geometric parameters (Å, º) top
Ca1—O1 | 2.340 (5) | C4—C5 | 1.40 (1) |
Ca1—O2i | 2.347 (5) | C5—C6 | 1.38 (1) |
Ca1—O3 | 2.631 (5) | C6—C7 | 1.386 (9) |
Ca1—O6ii | 2.365 (5) | C7—C8 | 1.392 (9) |
Ca1—O5iii | 2.344 (5) | C9—C10 | 1.526 (9) |
Ca1—O1w | 2.443 (5) | O1w—H1w1 | 0.85 |
Ca1—O2w | 2.409 (6) | O1w—H1w2 | 0.85 |
O1—C1 | 1.244 (8) | O2w—H2w1 | 0.85 |
O2—C1 | 1.241 (8) | O2w—H2w2 | 0.85 |
O3—C3 | 1.384 (8) | C2—H2a | 0.97 |
O3—C2 | 1.410 (8) | C2—H2b | 0.97 |
O4—C7 | 1.381 (8) | C4—H4 | 0.93 |
O4—C9 | 1.423 (8) | C5—H5 | 0.93 |
O5—C10 | 1.257 (8) | C6—H6 | 0.93 |
O6—C10 | 1.243 (9) | C8—H8 | 0.93 |
C1—C2 | 1.504 (9) | C9—H9a | 0.97 |
C3—C4 | 1.377 (9) | C9—H9b | 0.97 |
C3—C8 | 1.384 (9) | | |
| | | |
O1—Ca1—O2i | 91.2 (2) | C3—C4—C5 | 118.3 (6) |
O1—Ca1—O3 | 63.6 (2) | C6—C5—C4 | 120.7 (6) |
O1—Ca1—O5iii | 172.6 (2) | C5—C6—C7 | 119.6 (6) |
O1—Ca1—O6ii | 90.1 (2) | O4—C7—C6 | 115.3 (5) |
O1—Ca1—O1w | 86.4 (2) | O4—C7—C8 | 123.7 (6) |
O1—Ca1—O2w | 94.5 (2) | C6—C7—C8 | 121.0 (6) |
O2i—Ca1—O3 | 71.3 (2) | C3—C8—C7 | 118.1 (6) |
O2i—Ca1—O5iii | 85.9 (2) | O4—C9—C10 | 113.7 (5) |
O2i—Ca1—O6ii | 140.9 (2) | O6—C10—O5 | 125.1 (6) |
O2i—Ca1—O1w | 144.4 (2) | O6—C10—C9 | 118.0 (6) |
O2i—Ca1—O2w | 73.0 (2) | O5—C10—C9 | 116.8 (6) |
O3—Ca1—O5iii | 109.0 (2) | Ca1—O1w—H1w1 | 109.0 |
O3—Ca1—O6ii | 74.4 (2) | Ca1—O1w—H1w2 | 108.1 |
O3—Ca1—O1w | 136.3 (2) | H1w1—O1w—H1w2 | 109.3 |
O3—Ca1—O2w | 137.1 (2) | Ca1—O2w—H2w1 | 114.5 |
O5iii—Ca1—O6ii | 87.8 (2) | Ca1—O2w—H2w2 | 114.8 |
O5iii—Ca1—O1w | 99.9 (2) | H2w1—O2w—H2w2 | 110.1 |
O5iii—Ca1—O2w | 91.2 (2) | O3—C2—H2a | 109.7 |
O6ii—Ca1—O1w | 74.7 (2) | C1—C2—H2a | 109.7 |
O6ii—Ca1—O2w | 145.8 (2) | O3—C2—H2b | 109.7 |
O1w—Ca1—O2w | 71.8 (2) | C1—C2—H2b | 109.7 |
C1—O1—Ca1 | 128.3 (4) | H2a—C2—H2b | 108.2 |
C1—O2—Ca1ii | 148.2 (5) | C3—C4—H4 | 120.9 |
C3—O3—C2 | 117.1 (5) | C5—C4—H4 | 120.9 |
C3—O3—Ca1 | 123.2 (4) | C6—C5—H5 | 119.7 |
C2—O3—Ca1 | 115.6 (4) | C4—C5—H5 | 119.7 |
C7—O4—C9 | 117.1 (5) | C5—C6—H6 | 120.2 |
C10—O5—Ca1iv | 154.0 (4) | C7—C6—H6 | 120.2 |
C10—O6—Ca1i | 140.2 (4) | C3—C8—H8 | 120.9 |
O2—C1—O1 | 123.7 (6) | C7—C8—H8 | 120.9 |
O2—C1—C2 | 117.6 (6) | O4—C9—H9a | 108.8 |
O1—C1—C2 | 118.8 (6) | C10—C9—H9a | 108.8 |
O3—C2—C1 | 109.6 (5) | O4—C9—H9b | 108.8 |
C4—C3—C8 | 122.3 (6) | C10—C9—H9b | 108.8 |
C4—C3—O3 | 115.5 (6) | H9a—C9—H9b | 107.7 |
C8—C3—O3 | 122.1 (6) | | |
| | | |
O2i—Ca1—O1—C1 | −71.1 (6) | O1—C1—C2—O3 | −23.0 (9) |
O6ii—Ca1—O1—C1 | 69.8 (6) | C2—O3—C3—C4 | 141.7 (6) |
O2w—Ca1—O1—C1 | −144.1 (6) | Ca1—O3—C3—C4 | −62.4 (8) |
O1w—Ca1—O1—C1 | 144.5 (6) | C2—O3—C3—C8 | −41 (1) |
O3—Ca1—O1—C1 | −2.7 (5) | Ca1—O3—C3—C8 | 115.0 (6) |
O1—Ca1—O3—C3 | −167.0 (5) | C8—C3—C4—C5 | −3 (1) |
O5iii—Ca1—O3—C3 | 12.8 (5) | O3—C3—C4—C5 | 174.6 (6) |
O2i—Ca1—O3—C3 | −65.9 (5) | C3—C4—C5—C6 | 2 (1) |
O6ii—Ca1—O3—C3 | 94.9 (5) | C4—C5—C6—C7 | 0 (1) |
O2w—Ca1—O3—C3 | −101.0 (5) | C9—O4—C7—C6 | −170.7 (6) |
O1w—Ca1—O3—C3 | 141.4 (5) | C9—O4—C7—C8 | 10.1 (9) |
O1—Ca1—O3—C2 | −10.7 (4) | C5—C6—C7—O4 | 179.1 (7) |
O5iii—Ca1—O3—C2 | 169.1 (4) | C5—C6—C7—C8 | −2 (1) |
O2i—Ca1—O3—C2 | 90.4 (5) | C4—C3—C8—C7 | 2 (1) |
O6ii—Ca1—O3—C2 | −108.8 (5) | O3—C3—C8—C7 | −175.6 (6) |
O2w—Ca1—O3—C2 | 55.3 (6) | O4—C7—C8—C3 | 179.8 (6) |
O1w—Ca1—O3—C2 | −62.4 (5) | C6—C7—C8—C3 | 1 (1) |
Ca1ii—O2—C1—O1 | −165.9 (6) | C7—O4—C9—C10 | −82.6 (7) |
Ca1ii—O2—C1—C2 | 12.4 (13) | Ca1i—O6—C10—O5 | −28 (1) |
Ca1—O1—C1—O2 | −166.5 (5) | Ca1i—O6—C10—C9 | 155.3 (5) |
Ca1—O1—C1—C2 | 15.3 (9) | Ca1iv—O5—C10—O6 | −179.7 (6) |
C3—O3—C2—C1 | 177.7 (6) | Ca1iv—O5—C10—C9 | −3 (1) |
Ca1—O3—C2—C1 | 20.0 (7) | O4—C9—C10—O6 | −27.0 (9) |
O2—C1—C2—O3 | 158.7 (6) | O4—C9—C10—O5 | 155.8 (6) |
Symmetry codes: (i) x, −y+3/2, z−1/2; (ii) x, −y+3/2, z+1/2; (iii) x, y−1, z; (iv) x, y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w1···O1v | 0.85 | 2.09 | 2.942 (7) | 173 |
O1w—H1w2···O5ii | 0.85 | 1.99 | 2.807 (7) | 160 |
O2w—H2w1···O2v | 0.85 | 2.26 | 3.004 (7) | 147 |
O2w—H2w2···O1wvi | 0.85 | 2.12 | 2.960 (8) | 174 |
Symmetry codes: (ii) x, −y+3/2, z+1/2; (v) −x+1, −y+1, −z+1; (vi) −x+1, y+1/2, −z+1/2. |
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