The title compound, [Ca(C4H4O6)]·4H2O, calcium tartrate tetrahydrate, is a new triclinic centrosymmetric form identified in rat kidney calculus. The crystal structure was determined from powder and single-crystal X-ray diffraction. The four water molecules belong to one square face of the Ca-atom coordination (a square antiprism), the four O atoms of the second square face coming from two tartrate anions, building infinite chains alternating Ca atom polyhedra and tartrate anions along a, with the chains cross-linked by a network of hydrogen bonds.
Supporting information
CCDC reference: 742424
Data collection: Stadi4 (Stoe, 1998); cell refinement: Stadi4; data reduction: X-RED32 (Stoe, 1998); program(s) used to solve structure: ESPOIR (Le Bail, 2001); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2001); software used to prepare material for publication: enCIFer (Allen et al. (2004).
Calcium tartrate tetrahydrate
top
Crystal data top
C4H12CaO10 | Z = 2 |
Mr = 260.22 | F(000) = 272 |
Triclinic, P1 | Dx = 1.797 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 6.241 (2) Å | Cell parameters from 27 reflections |
b = 8.214 (3) Å | θ = 2–27.6° |
c = 10.411 (5) Å | µ = 0.69 mm−1 |
α = 94.92 (4)° | T = 293 K |
β = 106.00 (5)° | Parallelepiped, white |
γ = 107.55 (3)° | 0.12 × 0.10 × 0.03 mm |
V = 480.8 (4) Å3 | |
Data collection top
Siemens AED2 diffractometer | Rint = 0.023 |
Radiation source: fine-focus sealed tube | θmax = 27.6°, θmin = 2.1° |
Graphite monochromator | h = −8→7 |
2θ/ω scans | k = −10→10 |
2222 measured reflections | l = 0→13 |
2222 independent reflections | 3 standard reflections every 120 min |
1495 reflections with I > 2σ(I) | intensity decay: 15% |
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)] = 0.065 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.187 | w = 1/[σ2(Fo2) + (0.0918P)2 + 1.4964P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
2144 reflections | Δρmax = 0.97 e Å−3 |
174 parameters | Δρmin = −0.56 e Å−3 |
16 restraints | |
Crystal data top
C4H12CaO10 | γ = 107.55 (3)° |
Mr = 260.22 | V = 480.8 (4) Å3 |
Triclinic, P1 | Z = 2 |
a = 6.241 (2) Å | Mo Kα radiation |
b = 8.214 (3) Å | µ = 0.69 mm−1 |
c = 10.411 (5) Å | T = 293 K |
α = 94.92 (4)° | 0.12 × 0.10 × 0.03 mm |
β = 106.00 (5)° | |
Data collection top
Siemens AED2 diffractometer | Rint = 0.023 |
2222 measured reflections | 3 standard reflections every 120 min |
2222 independent reflections | intensity decay: 15% |
1495 reflections with I > 2σ(I) | |
Refinement top
R[F2 > 2σ(F2)] = 0.065 | 16 restraints |
wR(F2) = 0.187 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.06 | Δρmax = 0.97 e Å−3 |
2144 reflections | Δρmin = −0.56 e Å−3 |
174 parameters | |
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 | |
Ca1 | 0.34040 (16) | 0.19006 (12) | 0.27379 (10) | 0.0191 (3) | |
O1 | 0.3163 (6) | −0.0233 (4) | 0.0927 (3) | 0.0232 (7) | |
O2 | 1.1726 (6) | −0.0267 (5) | 0.3928 (4) | 0.0273 (8) | |
O3 | 0.9111 (6) | 0.0269 (4) | 0.1676 (3) | 0.0223 (7) | |
O4 | 0.6207 (6) | 0.0217 (4) | 0.3327 (3) | 0.0217 (7) | |
O5 | 0.9267 (7) | −0.2925 (5) | 0.3736 (4) | 0.0301 (8) | |
O6 | 0.2977 (6) | −0.2968 (5) | 0.0343 (4) | 0.0260 (8) | |
C1 | 0.9834 (8) | −0.1508 (6) | 0.3352 (5) | 0.0186 (9) | |
C2 | 0.3817 (8) | −0.1506 (6) | 0.1127 (5) | 0.0194 (9) | |
C3 | 0.8071 (8) | −0.1289 (6) | 0.2081 (4) | 0.0166 (9) | |
C4 | 0.5809 (8) | −0.1332 (6) | 0.2429 (5) | 0.0182 (9) | |
OW1 | 0.6007 (6) | 0.3134 (5) | 0.5045 (4) | 0.0312 (9) | |
OW2 | 0.1417 (6) | 0.3464 (5) | 0.3836 (4) | 0.0285 (8) | |
OW3 | 0.6889 (7) | 0.3761 (5) | 0.2295 (4) | 0.0296 (8) | |
OW4 | 0.1896 (7) | 0.3524 (5) | 0.1016 (4) | 0.0350 (9) | |
H1W1 | 0.686 (12) | 0.424 (4) | 0.540 (8) | 0.074 (10)* | |
H2W1 | 0.683 (12) | 0.244 (8) | 0.498 (9) | 0.074 (10)* | |
H1W2 | 0.118 (13) | 0.307 (11) | 0.458 (5) | 0.074 (10)* | |
H2W2 | 0.006 (9) | 0.327 (11) | 0.317 (5) | 0.074 (10)* | |
H1W3 | 0.679 (15) | 0.347 (9) | 0.143 (4) | 0.074 (10)* | |
H2W3 | 0.758 (13) | 0.494 (4) | 0.255 (7) | 0.074 (10)* | |
H1W4 | 0.033 (5) | 0.332 (10) | 0.068 (8) | 0.074 (10)* | |
H2W4 | 0.268 (11) | 0.462 (5) | 0.095 (9) | 0.074 (10)* | |
HC3 | 0.781 (8) | −0.210 (5) | 0.135 (4) | 0.036 (6)* | |
HC4 | 0.534 (8) | −0.210 (5) | 0.293 (4) | 0.036 (6)* | |
HO4 | 0.669 (8) | −0.003 (6) | 0.414 (3) | 0.036 (6)* | |
HO3 | 0.822 (7) | 0.015 (6) | 0.084 (3) | 0.036 (6)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca1 | 0.0153 (4) | 0.0188 (5) | 0.0208 (5) | 0.0052 (3) | 0.0030 (3) | 0.0036 (3) |
O1 | 0.0248 (17) | 0.0240 (17) | 0.0187 (17) | 0.0131 (14) | −0.0011 (13) | 0.0025 (13) |
O2 | 0.0172 (17) | 0.0295 (19) | 0.0267 (19) | 0.0019 (14) | −0.0011 (14) | 0.0113 (15) |
O3 | 0.0155 (16) | 0.0246 (17) | 0.0221 (18) | 0.0019 (13) | 0.0020 (13) | 0.0120 (14) |
O4 | 0.0228 (17) | 0.0256 (17) | 0.0179 (17) | 0.0123 (14) | 0.0043 (14) | 0.0018 (14) |
O5 | 0.033 (2) | 0.0243 (18) | 0.031 (2) | 0.0114 (15) | 0.0042 (16) | 0.0095 (15) |
O6 | 0.0213 (17) | 0.0220 (17) | 0.0255 (19) | 0.0037 (14) | −0.0003 (14) | −0.0043 (14) |
C1 | 0.016 (2) | 0.024 (2) | 0.016 (2) | 0.0100 (17) | 0.0026 (17) | 0.0011 (18) |
C2 | 0.0121 (19) | 0.023 (2) | 0.020 (2) | 0.0024 (17) | 0.0027 (17) | 0.0050 (18) |
C3 | 0.017 (2) | 0.019 (2) | 0.011 (2) | 0.0061 (17) | 0.0004 (16) | −0.0001 (16) |
C4 | 0.015 (2) | 0.018 (2) | 0.021 (2) | 0.0061 (17) | 0.0031 (17) | 0.0055 (18) |
OW1 | 0.0249 (19) | 0.033 (2) | 0.029 (2) | 0.0126 (16) | −0.0040 (15) | −0.0030 (17) |
OW2 | 0.0233 (18) | 0.034 (2) | 0.028 (2) | 0.0133 (16) | 0.0037 (15) | 0.0079 (16) |
OW3 | 0.0300 (19) | 0.0250 (18) | 0.027 (2) | 0.0018 (15) | 0.0077 (16) | 0.0016 (15) |
OW4 | 0.0238 (19) | 0.035 (2) | 0.040 (2) | 0.0067 (16) | 0.0005 (17) | 0.0178 (18) |
Geometric parameters (Å, º) top
Ca1—O1 | 2.401 (4) | O3—C3 | 1.407 (6) |
Ca1—O2i | 2.403 (4) | O3—HO3 | 0.87 (3) |
Ca1—OW1 | 2.424 (4) | O4—C4 | 1.426 (6) |
Ca1—OW3 | 2.439 (4) | O4—HO4 | 0.88 (3) |
Ca1—OW2 | 2.447 (4) | O5—C1 | 1.245 (6) |
Ca1—OW4 | 2.472 (4) | O6—C2 | 1.265 (6) |
Ca1—O3i | 2.479 (4) | C1—C3 | 1.533 (6) |
Ca1—O4 | 2.522 (3) | C2—C4 | 1.527 (6) |
O1—C2 | 1.245 (6) | C3—C4 | 1.542 (6) |
O1—O6 | 2.236 (5) | C3—HC3 | 0.91 (3) |
O2—C1 | 1.254 (6) | C4—HC4 | 0.88 (3) |
O2—O5 | 2.213 (5) | | |
| | | |
O1—Ca1—O2i | 92.85 (14) | OW1—Ca1—O4 | 72.32 (13) |
O1—Ca1—OW1 | 135.84 (13) | OW3—Ca1—O4 | 78.46 (13) |
O2i—Ca1—OW1 | 79.50 (14) | OW2—Ca1—O4 | 139.80 (12) |
O1—Ca1—OW3 | 86.36 (14) | OW4—Ca1—O4 | 142.46 (14) |
O2i—Ca1—OW3 | 149.10 (13) | O3i—Ca1—O4 | 118.64 (12) |
OW1—Ca1—OW3 | 79.72 (15) | O5—C1—O2 | 124.7 (4) |
O1—Ca1—OW2 | 148.98 (13) | O5—C1—C3 | 116.9 (4) |
O2i—Ca1—OW2 | 80.60 (14) | O2—C1—C3 | 118.5 (4) |
OW1—Ca1—OW2 | 73.07 (13) | O1—C2—O6 | 125.9 (4) |
OW3—Ca1—OW2 | 114.51 (14) | O1—C2—C4 | 118.6 (4) |
O1—Ca1—OW4 | 88.75 (14) | O6—C2—C4 | 115.5 (4) |
O2i—Ca1—OW4 | 136.45 (13) | O3—C3—C1 | 109.6 (4) |
OW1—Ca1—OW4 | 126.24 (15) | O3—C3—C4 | 112.6 (4) |
OW3—Ca1—OW4 | 74.44 (14) | C1—C3—C4 | 107.7 (4) |
OW2—Ca1—OW4 | 76.18 (15) | O3—C3—HC3 | 102 (3) |
O1—Ca1—O3i | 75.02 (13) | C1—C3—HC3 | 111 (3) |
O2i—Ca1—O3i | 64.86 (12) | C4—C3—HC3 | 114 (3) |
OW1—Ca1—O3i | 135.03 (14) | O4—C4—C2 | 108.7 (4) |
OW3—Ca1—O3i | 143.17 (13) | O4—C4—C3 | 111.0 (4) |
OW2—Ca1—O3i | 74.77 (13) | C2—C4—C3 | 109.7 (4) |
OW4—Ca1—O3i | 73.68 (13) | O4—C4—HC4 | 99 (3) |
O1—Ca1—O4 | 63.86 (12) | C2—C4—HC4 | 112 (3) |
O2i—Ca1—O4 | 73.58 (12) | C3—C4—HC4 | 116 (3) |
Symmetry code: (i) x−1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW1—H1W1···OW2ii | 0.89 (4) | 1.84 (5) | 2.729 (6) | 178 |
OW1—H2W1···O4 | 0.89 (8) | 2.26 (8) | 2.919 (5) | 131 (7) |
OW2—H1W2···O5iii | 0.90 (7) | 1.86 (6) | 2.728 (6) | 163 |
OW2—H2W2···OW3i | 0.89 (6) | 2.11 (6) | 2.933 (5) | 152 |
OW3—H1W3···O6iv | 0.89 (5) | 1.91 (5) | 2.798 (6) | 173 |
OW3—H2W3···O5v | 0.91 (4) | 1.87 (5) | 2.738 (6) | 157 |
OW4—H1W4···O6vi | 0.90 (5) | 1.96 (6) | 2.853 (5) | 170 |
OW4—H2W4···O6v | 0.90 (5) | 2.10 (5) | 2.947 (5) | 155 |
O4—HO4···O2vii | 0.88 (3) | 1.94 (3) | 2.783 (5) | 160 |
O3—HO3···O1iv | 0.87 (3) | 1.82 (3) | 2.683 (5) | 169 |
Symmetry codes: (i) x−1, y, z; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y, −z+1; (iv) −x+1, −y, −z; (v) x, y+1, z; (vi) −x, −y, −z; (vii) −x+2, −y, −z+1. |
Experimental details
Crystal data |
Chemical formula | C4H12CaO10 |
Mr | 260.22 |
Crystal system, space group | Triclinic, P1 |
Temperature (K) | 293 |
a, b, c (Å) | 6.241 (2), 8.214 (3), 10.411 (5) |
α, β, γ (°) | 94.92 (4), 106.00 (5), 107.55 (3) |
V (Å3) | 480.8 (4) |
Z | 2 |
Radiation type | Mo Kα |
µ (mm−1) | 0.69 |
Crystal size (mm) | 0.12 × 0.10 × 0.03 |
|
Data collection |
Diffractometer | Siemens AED2 diffractometer |
Absorption correction | – |
No. of measured, independent and observed [I > 2σ(I)] reflections | 2222, 2222, 1495 |
Rint | 0.023 |
(sin θ/λ)max (Å−1) | 0.651 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.065, 0.187, 1.06 |
No. of reflections | 2144 |
No. of parameters | 174 |
No. of restraints | 16 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.97, −0.56 |
Selected bond lengths (Å) topCa1—O1 | 2.401 (4) | O2—C1 | 1.254 (6) |
Ca1—O2i | 2.403 (4) | O2—O5 | 2.213 (5) |
Ca1—OW1 | 2.424 (4) | O3—C3 | 1.407 (6) |
Ca1—OW3 | 2.439 (4) | O4—C4 | 1.426 (6) |
Ca1—OW2 | 2.447 (4) | O5—C1 | 1.245 (6) |
Ca1—OW4 | 2.472 (4) | O6—C2 | 1.265 (6) |
Ca1—O3i | 2.479 (4) | C1—C3 | 1.533 (6) |
Ca1—O4 | 2.522 (3) | C2—C4 | 1.527 (6) |
O1—C2 | 1.245 (6) | C3—C4 | 1.542 (6) |
O1—O6 | 2.236 (5) | | |
Symmetry code: (i) x−1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
OW1—H1W1···OW2ii | 0.89 (4) | 1.84 (5) | 2.729 (6) | 178 |
OW1—H2W1···O4 | 0.89 (8) | 2.26 (8) | 2.919 (5) | 131 (7) |
OW2—H1W2···O5iii | 0.90 (7) | 1.86 (6) | 2.728 (6) | 163 |
OW2—H2W2···OW3i | 0.89 (6) | 2.11 (6) | 2.933 (5) | 152 |
OW3—H1W3···O6iv | 0.89 (5) | 1.91 (5) | 2.798 (6) | 173 |
OW3—H2W3···O5v | 0.91 (4) | 1.87 (5) | 2.738 (6) | 157 |
OW4—H1W4···O6vi | 0.90 (5) | 1.96 (6) | 2.853 (5) | 170 |
OW4—H2W4···O6v | 0.90 (5) | 2.10 (5) | 2.947 (5) | 155 |
O4—HO4···O2vii | 0.88 (3) | 1.94 (3) | 2.783 (5) | 160 |
O3—HO3···O1iv | 0.87 (3) | 1.82 (3) | 2.683 (5) | 169 |
Symmetry codes: (i) x−1, y, z; (ii) −x+1, −y+1, −z+1; (iii) −x+1, −y, −z+1; (iv) −x+1, −y, −z; (v) x, y+1, z; (vi) −x, −y, −z; (vii) −x+2, −y, −z+1. |