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The crystal structure of calcium tartrate esahydrate, CaC4H4O6·6H2O, has been solved by the charge-flipping method from single-crystal X-ray diffraction data and refined to R = 0.021, based on 1700 unique observed diffractions. Salient crystallographic data are: a = 7.7390 (1), b = 12.8030 (2), c = 5.8290 (1) Å, Z = 2, and space group P21212. During the refinement step it was possible to locate all H atoms by difference Fourier synthesis. The tartrate molecule has a (-)-gauche conformation and is coordinated to two calcium ions to form infinite chains along the a axis which alternate Ca polyhedra with tartrate molecules. The chains are interlinked by a three-dimensional network of hydrogen bonds from four water molecules surrounding the Ca ion, reinforced by hydrogen bonds from one interstitial water molecule. Micro-Raman and FT-IR spectroscopic data are provided.
Supporting information
CCDC reference: 1039889
Crystal data, data collection and structure refinement details are summarized
in Table 1.
S2. Results and discussion
top
Program(s) used to refine structure: SHELXL2013 (Sheldrick, 2013).
Crystal data top
C4H16CaO12 | Z = 2 |
Mr = 296.25 | F(000) = 312 |
Orthorhombic, P21212 | Dx = 1.704 Mg m−3 |
a = 7.7390 (1) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 12.8030 (2) Å | µ = 0.60 mm−1 |
c = 5.8290 (1) Å | T = 293 K |
V = 577.55 (2) Å3 | 0.22 × 0.20 × 0.07 mm |
Data collection top
Bruker APEXII diffractometer | θmax = 30.5°, θmin = 3.1° |
8303 measured reflections | h = −10→11 |
1759 independent reflections | k = −17→18 |
1700 reflections with I > 2σ(I) | l = −8→6 |
Rint = 0.025 | |
Refinement top
Refinement on F2 | Hydrogen site location: difference Fourier map |
Least-squares matrix: full | Only H-atom coordinates refined |
R[F2 > 2σ(F2)] = 0.021 | w = 1/[σ2(Fo2) + (0.1P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.075 | (Δ/σ)max < 0.001 |
S = 0.68 | Δρmax = 0.29 e Å−3 |
1759 reflections | Δρmin = −0.19 e Å−3 |
102 parameters | Absolute structure: Flack x determined using 679 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61). |
8 restraints | Absolute structure parameter: −0.173 (15) |
Crystal data top
C4H16CaO12 | V = 577.55 (2) Å3 |
Mr = 296.25 | Z = 2 |
Orthorhombic, P21212 | Mo Kα radiation |
a = 7.7390 (1) Å | µ = 0.60 mm−1 |
b = 12.8030 (2) Å | T = 293 K |
c = 5.8290 (1) Å | 0.22 × 0.20 × 0.07 mm |
Data collection top
Bruker APEXII diffractometer | 1700 reflections with I > 2σ(I) |
8303 measured reflections | Rint = 0.025 |
1759 independent reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.021 | Only H-atom coordinates refined |
wR(F2) = 0.075 | Δρmax = 0.29 e Å−3 |
S = 0.68 | Δρmin = −0.19 e Å−3 |
1759 reflections | Absolute structure: Flack x determined using 679 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61). |
102 parameters | Absolute structure parameter: −0.173 (15) |
8 restraints | |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca1 | 0.0000 | 0.5000 | 0.31079 (6) | 0.01632 (12) | |
O1 | −0.01771 (16) | 0.37975 (10) | −0.00915 (19) | 0.0242 (2) | |
O2 | 0.18578 (15) | 0.53433 (11) | 0.6286 (2) | 0.0263 (3) | |
O3 | 0.42004 (16) | 0.60400 (11) | 0.7860 (2) | 0.0287 (3) | |
O4 | 0.31487 (15) | 0.53668 (11) | 0.2164 (2) | 0.0267 (3) | |
O5 | 0.1153 (3) | 0.32751 (12) | 0.4185 (3) | 0.0450 (4) | |
O6 | 0.22163 (16) | 0.79013 (10) | 0.1646 (3) | 0.0325 (3) | |
C1 | 0.34089 (18) | 0.56254 (11) | 0.6220 (2) | 0.0177 (3) | |
C2 | 0.43903 (19) | 0.54806 (11) | 0.3954 (2) | 0.0178 (2) | |
H1 | 0.079 (3) | 0.3486 (18) | −0.059 (5) | 0.029* | |
H2 | −0.065 (3) | 0.4106 (17) | −0.129 (4) | 0.029* | |
H3 | 0.166 (4) | 0.311 (3) | 0.551 (5) | 0.054* | |
H4 | 0.141 (4) | 0.275 (2) | 0.323 (6) | 0.054* | |
H5 | 0.132 (3) | 0.833 (2) | 0.165 (6) | 0.039* | |
H6 | 0.188 (4) | 0.7346 (19) | 0.092 (5) | 0.039* | |
H7 | 0.508 (3) | 0.6119 (16) | 0.376 (4) | 0.021* | |
H8 | 0.359 (3) | 0.560 (2) | 0.085 (4) | 0.032* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca1 | 0.01416 (17) | 0.02106 (19) | 0.01374 (18) | −0.00108 (12) | 0.000 | 0.000 |
O1 | 0.0233 (5) | 0.0320 (5) | 0.0173 (5) | 0.0057 (4) | −0.0001 (4) | 0.0006 (4) |
O2 | 0.0159 (4) | 0.0431 (6) | 0.0198 (5) | −0.0054 (5) | 0.0036 (4) | −0.0066 (4) |
O3 | 0.0235 (5) | 0.0429 (6) | 0.0198 (5) | −0.0088 (5) | −0.0012 (4) | −0.0071 (5) |
O4 | 0.0165 (4) | 0.0488 (7) | 0.0149 (4) | 0.0020 (5) | −0.0017 (4) | 0.0060 (5) |
O5 | 0.0694 (11) | 0.0289 (6) | 0.0368 (8) | 0.0064 (7) | −0.0244 (8) | −0.0017 (6) |
O6 | 0.0222 (5) | 0.0302 (6) | 0.0452 (8) | −0.0029 (4) | −0.0006 (5) | −0.0055 (6) |
C1 | 0.0160 (6) | 0.0219 (6) | 0.0152 (5) | 0.0009 (4) | 0.0009 (4) | −0.0014 (5) |
C2 | 0.0135 (5) | 0.0255 (6) | 0.0144 (5) | 0.0009 (5) | −0.0001 (4) | 0.0010 (5) |
Geometric parameters (Å, º) top
Ca1—O1 | 2.4222 (12) | Ca1—O4 | 2.5419 (12) |
Ca1—O1i | 2.4222 (12) | O2—C1 | 1.2541 (18) |
Ca1—O2 | 2.3858 (12) | O3—C1 | 1.2535 (18) |
Ca1—O2i | 2.3858 (12) | O4—C2 | 1.4259 (18) |
Ca1—O5 | 2.4631 (15) | C1—C2 | 1.535 (2) |
Ca1—O5i | 2.4631 (15) | C2—C2ii | 1.551 (3) |
Ca1—O4i | 2.5419 (12) | | |
| | | |
O1—Ca1—O1i | 79.30 (6) | O2i—Ca1—O4i | 63.66 (4) |
O1—Ca1—O2 | 138.50 (4) | O5—Ca1—O4i | 103.70 (5) |
O1i—Ca1—O2 | 116.53 (4) | O5i—Ca1—O4i | 82.74 (6) |
O1—Ca1—O2i | 116.53 (4) | O1—Ca1—O4 | 90.29 (4) |
O1i—Ca1—O2i | 138.50 (4) | O1i—Ca1—O4 | 70.22 (4) |
O2—Ca1—O2i | 78.13 (6) | O2—Ca1—O4 | 63.66 (4) |
O1—Ca1—O5 | 69.32 (5) | O2i—Ca1—O4 | 141.25 (4) |
O1i—Ca1—O5 | 138.21 (6) | O5—Ca1—O4 | 82.74 (6) |
O2—Ca1—O5 | 75.46 (5) | O5i—Ca1—O4 | 103.70 (5) |
O2i—Ca1—O5 | 81.68 (6) | O4i—Ca1—O4 | 154.99 (5) |
O1—Ca1—O5i | 138.21 (6) | C1—O2—Ca1 | 127.30 (10) |
O1i—Ca1—O5i | 69.32 (5) | C2—O4—Ca1 | 120.43 (9) |
O2—Ca1—O5i | 81.68 (6) | O2—C1—O3 | 124.49 (14) |
O2i—Ca1—O5i | 75.46 (5) | O2—C1—C2 | 117.73 (13) |
O5—Ca1—O5i | 150.47 (9) | O3—C1—C2 | 117.76 (13) |
O1—Ca1—O4i | 70.22 (4) | O4—C2—C1 | 107.98 (12) |
O1i—Ca1—O4i | 90.29 (4) | O4—C2—C2ii | 109.20 (11) |
O2—Ca1—O4i | 141.25 (4) | C1—C2—C2ii | 113.39 (9) |
Symmetry codes: (i) −x, −y+1, z; (ii) −x+1, −y+1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O6iii | 0.90 (2) | 1.82 (2) | 2.7180 (17) | 178 (2) |
O1—H2···O2iv | 0.88 (2) | 1.83 (2) | 2.7131 (16) | 173 (3) |
O4—H8···O3v | 0.89 (2) | 1.89 (2) | 2.7746 (18) | 171 (2) |
O5—H3···O6vi | 0.89 (2) | 1.89 (2) | 2.780 (2) | 174 (3) |
O5—H4···O3vi | 0.90 (2) | 2.33 (3) | 3.112 (2) | 146 (3) |
O6—H5···O3vii | 0.88 (2) | 1.85 (2) | 2.7143 (18) | 165 (3) |
O6—H6···O1i | 0.87 (2) | 2.06 (2) | 2.8717 (18) | 156 (3) |
Symmetry codes: (i) −x, −y+1, z; (iii) −x+1/2, y−1/2, −z; (iv) −x, −y+1, z−1; (v) x, y, z−1; (vi) −x+1/2, y−1/2, −z+1; (vii) x−1/2, −y+3/2, −z+1. |
Experimental details
Crystal data |
Chemical formula | C4H16CaO12 |
Mr | 296.25 |
Crystal system, space group | Orthorhombic, P21212 |
Temperature (K) | 293 |
a, b, c (Å) | 7.7390 (1), 12.8030 (2), 5.8290 (1) |
V (Å3) | 577.55 (2) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.60 |
Crystal size (mm) | 0.22 × 0.20 × 0.07 |
|
Data collection |
Diffractometer | Bruker APEXII diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 8303, 1759, 1700 |
Rint | 0.025 |
(sin θ/λ)max (Å−1) | 0.715 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.021, 0.075, 0.68 |
No. of reflections | 1759 |
No. of parameters | 102 |
No. of restraints | 8 |
H-atom treatment | Only H-atom coordinates refined |
Δρmax, Δρmin (e Å−3) | 0.29, −0.19 |
Absolute structure | Flack x determined using 679 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61). |
Absolute structure parameter | −0.173 (15) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1···O6i | 0.90 (2) | 1.82 (2) | 2.7180 (17) | 178 (2) |
O1—H2···O2ii | 0.883 (19) | 1.834 (19) | 2.7131 (16) | 173 (3) |
O4—H8···O3iii | 0.89 (2) | 1.89 (2) | 2.7746 (18) | 171 (2) |
O5—H3···O6iv | 0.89 (2) | 1.89 (2) | 2.780 (2) | 174 (3) |
O5—H4···O3iv | 0.90 (2) | 2.33 (3) | 3.112 (2) | 146 (3) |
O6—H5···O3v | 0.88 (2) | 1.85 (2) | 2.7143 (18) | 165 (3) |
O6—H6···O1vi | 0.87 (2) | 2.06 (2) | 2.8717 (18) | 156 (3) |
Symmetry codes: (i) −x+1/2, y−1/2, −z; (ii) −x, −y+1, z−1; (iii) x, y, z−1; (iv) −x+1/2, y−1/2, −z+1; (v) x−1/2, −y+3/2, −z+1; (vi) −x, −y+1, z. |
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