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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768109013688/kd5029sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108768109013688/kd5029sup2.hkl
Contains datablock I

rtv

Rietveld powder data file (CIF format) https://doi.org/10.1107/S0108768109013688/kd5029sup3.rtv
Contains datablock I

pdf

Portable Document Format (PDF) file https://doi.org/10.1107/S0108768109013688/kd5029sup4.pdf
Tables of coordinates, displacement parameters and powder data, and extra figures

CCDC reference: 742424

Computing details top

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).

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
Calcium tartrate tetrahydrate top
Crystal data top
C4H12CaO10Z = 2
Mr = 260.22F(000) = 272
Triclinic, P1Dx = 1.797 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71069 Å
a = 6.241 (2) ÅCell parameters from 27 reflections
b = 8.214 (3) Åθ = 2–27.6°
c = 10.411 (5) ŵ = 0.69 mm1
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 tubeθmax = 27.6°, θmin = 2.1°
Graphite monochromatorh = 87
2θ/ω scansk = 1010
2222 measured reflectionsl = 013
2222 independent reflections3 standard reflections every 120 min
1495 reflections with I > 2σ(I) intensity decay: 15%
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.065H 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 reflectionsΔρmax = 0.97 e Å3
174 parametersΔρmin = 0.56 e Å3
16 restraints
Crystal data top
C4H12CaO10γ = 107.55 (3)°
Mr = 260.22V = 480.8 (4) Å3
Triclinic, P1Z = 2
a = 6.241 (2) ÅMo Kα radiation
b = 8.214 (3) ŵ = 0.69 mm1
c = 10.411 (5) ÅT = 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 reflections3 standard reflections every 120 min
2222 independent reflections intensity decay: 15%
1495 reflections with I > 2σ(I)
Refinement top
R[F2 > 2σ(F2)] = 0.06516 restraints
wR(F2) = 0.187H atoms treated by a mixture of independent and constrained refinement
S = 1.06Δρmax = 0.97 e Å3
2144 reflectionsΔρmin = 0.56 e Å3
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
xyzUiso*/Ueq
Ca10.34040 (16)0.19006 (12)0.27379 (10)0.0191 (3)
O10.3163 (6)0.0233 (4)0.0927 (3)0.0232 (7)
O21.1726 (6)0.0267 (5)0.3928 (4)0.0273 (8)
O30.9111 (6)0.0269 (4)0.1676 (3)0.0223 (7)
O40.6207 (6)0.0217 (4)0.3327 (3)0.0217 (7)
O50.9267 (7)0.2925 (5)0.3736 (4)0.0301 (8)
O60.2977 (6)0.2968 (5)0.0343 (4)0.0260 (8)
C10.9834 (8)0.1508 (6)0.3352 (5)0.0186 (9)
C20.3817 (8)0.1506 (6)0.1127 (5)0.0194 (9)
C30.8071 (8)0.1289 (6)0.2081 (4)0.0166 (9)
C40.5809 (8)0.1332 (6)0.2429 (5)0.0182 (9)
OW10.6007 (6)0.3134 (5)0.5045 (4)0.0312 (9)
OW20.1417 (6)0.3464 (5)0.3836 (4)0.0285 (8)
OW30.6889 (7)0.3761 (5)0.2295 (4)0.0296 (8)
OW40.1896 (7)0.3524 (5)0.1016 (4)0.0350 (9)
H1W10.686 (12)0.424 (4)0.540 (8)0.074 (10)*
H2W10.683 (12)0.244 (8)0.498 (9)0.074 (10)*
H1W20.118 (13)0.307 (11)0.458 (5)0.074 (10)*
H2W20.006 (9)0.327 (11)0.317 (5)0.074 (10)*
H1W30.679 (15)0.347 (9)0.143 (4)0.074 (10)*
H2W30.758 (13)0.494 (4)0.255 (7)0.074 (10)*
H1W40.033 (5)0.332 (10)0.068 (8)0.074 (10)*
H2W40.268 (11)0.462 (5)0.095 (9)0.074 (10)*
HC30.781 (8)0.210 (5)0.135 (4)0.036 (6)*
HC40.534 (8)0.210 (5)0.293 (4)0.036 (6)*
HO40.669 (8)0.003 (6)0.414 (3)0.036 (6)*
HO30.822 (7)0.015 (6)0.084 (3)0.036 (6)*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0153 (4)0.0188 (5)0.0208 (5)0.0052 (3)0.0030 (3)0.0036 (3)
O10.0248 (17)0.0240 (17)0.0187 (17)0.0131 (14)0.0011 (13)0.0025 (13)
O20.0172 (17)0.0295 (19)0.0267 (19)0.0019 (14)0.0011 (14)0.0113 (15)
O30.0155 (16)0.0246 (17)0.0221 (18)0.0019 (13)0.0020 (13)0.0120 (14)
O40.0228 (17)0.0256 (17)0.0179 (17)0.0123 (14)0.0043 (14)0.0018 (14)
O50.033 (2)0.0243 (18)0.031 (2)0.0114 (15)0.0042 (16)0.0095 (15)
O60.0213 (17)0.0220 (17)0.0255 (19)0.0037 (14)0.0003 (14)0.0043 (14)
C10.016 (2)0.024 (2)0.016 (2)0.0100 (17)0.0026 (17)0.0011 (18)
C20.0121 (19)0.023 (2)0.020 (2)0.0024 (17)0.0027 (17)0.0050 (18)
C30.017 (2)0.019 (2)0.011 (2)0.0061 (17)0.0004 (16)0.0001 (16)
C40.015 (2)0.018 (2)0.021 (2)0.0061 (17)0.0031 (17)0.0055 (18)
OW10.0249 (19)0.033 (2)0.029 (2)0.0126 (16)0.0040 (15)0.0030 (17)
OW20.0233 (18)0.034 (2)0.028 (2)0.0133 (16)0.0037 (15)0.0079 (16)
OW30.0300 (19)0.0250 (18)0.027 (2)0.0018 (15)0.0077 (16)0.0016 (15)
OW40.0238 (19)0.035 (2)0.040 (2)0.0067 (16)0.0005 (17)0.0178 (18)
Geometric parameters (Å, º) top
Ca1—O12.401 (4)O3—C31.407 (6)
Ca1—O2i2.403 (4)O3—HO30.87 (3)
Ca1—OW12.424 (4)O4—C41.426 (6)
Ca1—OW32.439 (4)O4—HO40.88 (3)
Ca1—OW22.447 (4)O5—C11.245 (6)
Ca1—OW42.472 (4)O6—C21.265 (6)
Ca1—O3i2.479 (4)C1—C31.533 (6)
Ca1—O42.522 (3)C2—C41.527 (6)
O1—C21.245 (6)C3—C41.542 (6)
O1—O62.236 (5)C3—HC30.91 (3)
O2—C11.254 (6)C4—HC40.88 (3)
O2—O52.213 (5)
O1—Ca1—O2i92.85 (14)OW1—Ca1—O472.32 (13)
O1—Ca1—OW1135.84 (13)OW3—Ca1—O478.46 (13)
O2i—Ca1—OW179.50 (14)OW2—Ca1—O4139.80 (12)
O1—Ca1—OW386.36 (14)OW4—Ca1—O4142.46 (14)
O2i—Ca1—OW3149.10 (13)O3i—Ca1—O4118.64 (12)
OW1—Ca1—OW379.72 (15)O5—C1—O2124.7 (4)
O1—Ca1—OW2148.98 (13)O5—C1—C3116.9 (4)
O2i—Ca1—OW280.60 (14)O2—C1—C3118.5 (4)
OW1—Ca1—OW273.07 (13)O1—C2—O6125.9 (4)
OW3—Ca1—OW2114.51 (14)O1—C2—C4118.6 (4)
O1—Ca1—OW488.75 (14)O6—C2—C4115.5 (4)
O2i—Ca1—OW4136.45 (13)O3—C3—C1109.6 (4)
OW1—Ca1—OW4126.24 (15)O3—C3—C4112.6 (4)
OW3—Ca1—OW474.44 (14)C1—C3—C4107.7 (4)
OW2—Ca1—OW476.18 (15)O3—C3—HC3102 (3)
O1—Ca1—O3i75.02 (13)C1—C3—HC3111 (3)
O2i—Ca1—O3i64.86 (12)C4—C3—HC3114 (3)
OW1—Ca1—O3i135.03 (14)O4—C4—C2108.7 (4)
OW3—Ca1—O3i143.17 (13)O4—C4—C3111.0 (4)
OW2—Ca1—O3i74.77 (13)C2—C4—C3109.7 (4)
OW4—Ca1—O3i73.68 (13)O4—C4—HC499 (3)
O1—Ca1—O463.86 (12)C2—C4—HC4112 (3)
O2i—Ca1—O473.58 (12)C3—C4—HC4116 (3)
Symmetry code: (i) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
OW1—H1W1···OW2ii0.89 (4)1.84 (5)2.729 (6)178
OW1—H2W1···O40.89 (8)2.26 (8)2.919 (5)131 (7)
OW2—H1W2···O5iii0.90 (7)1.86 (6)2.728 (6)163
OW2—H2W2···OW3i0.89 (6)2.11 (6)2.933 (5)152
OW3—H1W3···O6iv0.89 (5)1.91 (5)2.798 (6)173
OW3—H2W3···O5v0.91 (4)1.87 (5)2.738 (6)157
OW4—H1W4···O6vi0.90 (5)1.96 (6)2.853 (5)170
OW4—H2W4···O6v0.90 (5)2.10 (5)2.947 (5)155
O4—HO4···O2vii0.88 (3)1.94 (3)2.783 (5)160
O3—HO3···O1iv0.87 (3)1.82 (3)2.683 (5)169
Symmetry codes: (i) x1, 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 formulaC4H12CaO10
Mr260.22
Crystal system, space groupTriclinic, 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)
V3)480.8 (4)
Z2
Radiation typeMo Kα
µ (mm1)0.69
Crystal size (mm)0.12 × 0.10 × 0.03
Data collection
DiffractometerSiemens AED2
diffractometer
Absorption correction
No. of measured, independent and
observed [I > 2σ(I)] reflections
2222, 2222, 1495
Rint0.023
(sin θ/λ)max1)0.651
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.065, 0.187, 1.06
No. of reflections2144
No. of parameters174
No. of restraints16
H-atom treatmentH atoms treated by a mixture of independent and constrained refinement
Δρmax, Δρmin (e Å3)0.97, 0.56

Computer programs: Stadi4 (Stoe, 1998), Stadi4, X-RED32 (Stoe, 1998), ESPOIR (Le Bail, 2001), SHELXL97 (Sheldrick, 1997), DIAMOND (Brandenburg, 2001), enCIFer (Allen et al. (2004).

Selected bond lengths (Å) top
Ca1—O12.401 (4)O2—C11.254 (6)
Ca1—O2i2.403 (4)O2—O52.213 (5)
Ca1—OW12.424 (4)O3—C31.407 (6)
Ca1—OW32.439 (4)O4—C41.426 (6)
Ca1—OW22.447 (4)O5—C11.245 (6)
Ca1—OW42.472 (4)O6—C21.265 (6)
Ca1—O3i2.479 (4)C1—C31.533 (6)
Ca1—O42.522 (3)C2—C41.527 (6)
O1—C21.245 (6)C3—C41.542 (6)
O1—O62.236 (5)
Symmetry code: (i) x1, y, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
OW1—H1W1···OW2ii0.89 (4)1.84 (5)2.729 (6)178
OW1—H2W1···O40.89 (8)2.26 (8)2.919 (5)131 (7)
OW2—H1W2···O5iii0.90 (7)1.86 (6)2.728 (6)163
OW2—H2W2···OW3i0.89 (6)2.11 (6)2.933 (5)152
OW3—H1W3···O6iv0.89 (5)1.91 (5)2.798 (6)173
OW3—H2W3···O5v0.91 (4)1.87 (5)2.738 (6)157
OW4—H1W4···O6vi0.90 (5)1.96 (6)2.853 (5)170
OW4—H2W4···O6v0.90 (5)2.10 (5)2.947 (5)155
O4—HO4···O2vii0.88 (3)1.94 (3)2.783 (5)160
O3—HO3···O1iv0.87 (3)1.82 (3)2.683 (5)169
Symmetry codes: (i) x1, 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.
 

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