Experimental
Data collection
Kuma KM-4 four-circle diffractometer Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008 ) Tmin = 0.968, Tmax = 0.982 3274 measured reflections 3065 independent reflections 1709 reflections with I > 2σ(I) Rint = 0.049 3 standard reflections every 200 reflections intensity decay: 2.9%
|
Ca1—O5 | 2.398 (2) | Ca1—O7 | 2.420 (2) | Ca1—O3i | 2.4361 (17) | Ca1—O1ii | 2.4823 (16) | Ca1—O6 | 2.502 (2) | Ca1—O1 | 2.5061 (17) | Ca1—N1 | 2.563 (2) | Ca1—N3i | 2.6133 (19) | Symmetry codes: (i) ; (ii) -x, -y, -z+1. | |
D—H⋯A | D—H | H⋯A | D⋯A | D—H⋯A | O7—H72⋯O2iii | 0.80 (6) | 2.34 (6) | 3.048 (3) | 149 (6) | O6—H61⋯O2ii | 0.85 (5) | 1.88 (5) | 2.698 (3) | 163 (5) | O8—H81⋯O3iv | 0.76 (4) | 2.04 (4) | 2.793 (3) | 170 (4) | O8—H82⋯O6v | 0.77 (5) | 2.09 (5) | 2.818 (3) | 157 (5) | O5—H52⋯O8vi | 0.87 (4) | 1.94 (4) | 2.798 (3) | 169 (4) | O6—H62⋯O4iii | 0.77 (4) | 1.96 (4) | 2.719 (2) | 167 (4) | O7—H71⋯O4vii | 0.79 (4) | 2.16 (4) | 2.902 (3) | 158 (3) | O5—H51⋯O8iv | 0.78 (4) | 2.04 (4) | 2.816 (3) | 176 (4) | Symmetry codes: (ii) -x, -y, -z+1; (iii) ; (iv) ; (v) ; (vi) ; (vii) -x, -y+1, -z+1. | |
Data collection: KM-4 Software (Kuma, 1996
); cell refinement: KM-4 Software; data reduction: DATAPROC (Kuma, 2001
); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008
); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008
); molecular graphics: SHELXTL (Sheldrick, 2008
); software used to prepare material for publication: SHELXTL.
Supporting information
An aqueous solution containing 1 mmol of calcium acetate hydrate and 1 mmol of pyrimidine-4,6-diarboxylic acid dihydrate was refluxed with constant stirring for 6 h. After cooling to room temperature, the solution was left to evaporate. Well formed single-crystal blocks appeared overnight at the bottom of the reaction pot. They were separated from the mother liquid, washed with cold water and dried in air.
Hydrogen atoms attached to water molecules were located in a difference map and refined isotropically, while two H atoms attached to pyrimidine C atoms were located at a calculated positions and treated as riding on the parent atoms with C—H=0.93 Å and
Data collection: KM-4 Software (Kuma, 1996); cell refinement: KM-4 Software (Kuma, 1996); data reduction: DATAPROC (Kuma, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).
Poly[[hexaaquabis(µ
3-pyrimidine-4,6-dicarboxylato)dicalcium] dihydrate]
top Crystal data top [Ca2(C6H2N2O4)2(H2O)6]·2H2O | F(000) = 576 |
Mr = 278.24 | Dx = 1.762 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 25 reflections |
a = 7.7053 (15) Å | θ = 6–15° |
b = 11.432 (2) Å | µ = 0.64 mm−1 |
c = 11.916 (2) Å | T = 293 K |
β = 92.16 (3)° | Blocks, colourless |
V = 1048.9 (4) Å3 | 0.10 × 0.04 × 0.03 mm |
Z = 4 | |
Data collection top Kuma KM-4 four-circle diffractometer | 1709 reflections with I > 2σ(I) |
Radiation source: fine-focus sealed tube | Rint = 0.049 |
Graphite monochromator | θmax = 30.1°, θmin = 2.5° |
profile data from ω/2θ scans | h = 0→10 |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008) | k = −16→0 |
Tmin = 0.968, Tmax = 0.982 | l = −16→16 |
3274 measured reflections | 3 standard reflections every 200 reflections |
3065 independent reflections | intensity decay: 2.9% |
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)] = 0.033 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.107 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | w = 1/[σ2(Fo2) + (0.0572P)2 + 0.0532P] where P = (Fo2 + 2Fc2)/3 |
3065 reflections | (Δ/σ)max = 0.001 |
186 parameters | Δρmax = 0.44 e Å−3 |
0 restraints | Δρmin = −0.59 e Å−3 |
Crystal data top [Ca2(C6H2N2O4)2(H2O)6]·2H2O | V = 1048.9 (4) Å3 |
Mr = 278.24 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 7.7053 (15) Å | µ = 0.64 mm−1 |
b = 11.432 (2) Å | T = 293 K |
c = 11.916 (2) Å | 0.10 × 0.04 × 0.03 mm |
β = 92.16 (3)° | |
Data collection top Kuma KM-4 four-circle diffractometer | 1709 reflections with I > 2σ(I) |
Absorption correction: analytical (CrysAlis RED; Oxford Diffraction, 2008) | Rint = 0.049 |
Tmin = 0.968, Tmax = 0.982 | 3 standard reflections every 200 reflections |
3274 measured reflections | intensity decay: 2.9% |
3065 independent reflections | |
Refinement top R[F2 > 2σ(F2)] = 0.033 | 0 restraints |
wR(F2) = 0.107 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | Δρmax = 0.44 e Å−3 |
3065 reflections | Δρmin = −0.59 e Å−3 |
186 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 | 0.03092 (6) | 0.05117 (4) | 0.65920 (3) | 0.01409 (11) | |
O1 | 0.0060 (2) | 0.12495 (14) | 0.46120 (13) | 0.0195 (3) | |
O2 | 0.0320 (3) | 0.27178 (16) | 0.33877 (13) | 0.0261 (4) | |
N1 | 0.1313 (3) | 0.26241 (16) | 0.63011 (14) | 0.0163 (4) | |
C6 | 0.1190 (3) | 0.30679 (18) | 0.52650 (17) | 0.0148 (4) | |
C5 | 0.1834 (3) | 0.41685 (18) | 0.50185 (18) | 0.0174 (4) | |
H5 | 0.1705 | 0.4487 | 0.4302 | 0.021* | |
C7 | 0.0438 (3) | 0.22887 (19) | 0.43434 (18) | 0.0165 (4) | |
O4 | 0.3231 (3) | 0.64500 (15) | 0.48018 (14) | 0.0313 (5) | |
O7 | −0.2529 (3) | 0.14194 (19) | 0.6459 (2) | 0.0342 (5) | |
O6 | −0.1678 (3) | −0.08219 (17) | 0.76038 (16) | 0.0267 (4) | |
N3 | 0.2839 (3) | 0.43217 (16) | 0.69222 (14) | 0.0169 (4) | |
O5 | 0.3228 (3) | 0.0407 (2) | 0.59679 (18) | 0.0348 (5) | |
C2 | 0.2132 (3) | 0.32771 (19) | 0.70832 (18) | 0.0180 (4) | |
H2 | 0.2216 | 0.2974 | 0.7807 | 0.022* | |
C4 | 0.2679 (3) | 0.47703 (19) | 0.58880 (17) | 0.0152 (4) | |
C8 | 0.3517 (3) | 0.59611 (18) | 0.57191 (18) | 0.0170 (4) | |
O8 | 0.9331 (3) | 0.35726 (19) | 0.89833 (19) | 0.0303 (4) | |
H51 | 0.390 (5) | −0.010 (4) | 0.601 (3) | 0.047 (11)* | |
O3 | 0.4436 (2) | 0.63449 (14) | 0.65273 (13) | 0.0199 (3) | |
H71 | −0.285 (4) | 0.187 (3) | 0.600 (3) | 0.031 (9)* | |
H62 | −0.174 (5) | −0.090 (3) | 0.824 (3) | 0.038 (10)* | |
H52 | 0.358 (5) | 0.081 (4) | 0.540 (3) | 0.055 (12)* | |
H82 | 0.882 (6) | 0.384 (5) | 0.847 (4) | 0.076 (16)* | |
H81 | 0.957 (5) | 0.293 (3) | 0.888 (3) | 0.036 (9)* | |
H61 | −0.120 (6) | −0.146 (4) | 0.743 (4) | 0.081 (16)* | |
H72 | −0.324 (8) | 0.138 (5) | 0.693 (5) | 0.10 (2)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca1 | 0.0198 (2) | 0.01036 (17) | 0.01203 (17) | −0.00052 (18) | −0.00070 (13) | −0.00012 (16) |
O1 | 0.0290 (9) | 0.0126 (7) | 0.0168 (7) | −0.0043 (6) | −0.0002 (6) | −0.0028 (6) |
O2 | 0.0448 (10) | 0.0193 (8) | 0.0135 (7) | −0.0052 (8) | −0.0076 (7) | 0.0006 (6) |
N1 | 0.0223 (9) | 0.0135 (8) | 0.0131 (8) | −0.0017 (7) | −0.0013 (7) | −0.0006 (7) |
C6 | 0.0180 (10) | 0.0128 (9) | 0.0135 (9) | −0.0005 (8) | −0.0010 (8) | −0.0012 (7) |
C5 | 0.0266 (11) | 0.0124 (9) | 0.0130 (8) | −0.0024 (8) | −0.0019 (8) | 0.0011 (7) |
C7 | 0.0205 (10) | 0.0135 (9) | 0.0155 (9) | −0.0016 (8) | −0.0009 (8) | −0.0038 (8) |
O4 | 0.0595 (14) | 0.0183 (8) | 0.0154 (8) | −0.0108 (9) | −0.0070 (8) | 0.0064 (6) |
O7 | 0.0323 (11) | 0.0327 (11) | 0.0378 (11) | 0.0116 (9) | 0.0063 (9) | 0.0124 (9) |
O6 | 0.0394 (11) | 0.0236 (9) | 0.0172 (8) | −0.0052 (8) | 0.0030 (8) | 0.0011 (7) |
N3 | 0.0241 (9) | 0.0149 (9) | 0.0117 (7) | −0.0054 (7) | 0.0003 (7) | 0.0005 (6) |
O5 | 0.0301 (10) | 0.0360 (12) | 0.0389 (11) | 0.0114 (9) | 0.0109 (8) | 0.0158 (9) |
C2 | 0.0264 (12) | 0.0164 (10) | 0.0112 (8) | −0.0030 (9) | −0.0013 (8) | 0.0013 (8) |
C4 | 0.0206 (10) | 0.0123 (9) | 0.0125 (9) | −0.0006 (8) | 0.0001 (8) | −0.0001 (7) |
C8 | 0.0257 (12) | 0.0116 (9) | 0.0136 (9) | −0.0029 (9) | 0.0013 (8) | −0.0012 (7) |
O8 | 0.0296 (10) | 0.0219 (10) | 0.0392 (11) | 0.0042 (8) | 0.0005 (8) | −0.0076 (8) |
O3 | 0.0298 (9) | 0.0132 (7) | 0.0164 (7) | −0.0064 (7) | −0.0026 (6) | −0.0015 (6) |
Geometric parameters (Å, º) top Ca1—O5 | 2.398 (2) | C5—H5 | 0.9300 |
Ca1—O7 | 2.420 (2) | O4—C8 | 1.240 (3) |
Ca1—O3i | 2.4361 (17) | O7—H71 | 0.79 (4) |
Ca1—O1ii | 2.4823 (16) | O7—H72 | 0.80 (6) |
Ca1—O6 | 2.502 (2) | O6—H62 | 0.77 (4) |
Ca1—O1 | 2.5061 (17) | O6—H61 | 0.85 (5) |
Ca1—N1 | 2.563 (2) | N3—C2 | 1.330 (3) |
Ca1—N3i | 2.6133 (19) | N3—C4 | 1.336 (3) |
Ca1—Ca1ii | 3.9817 (11) | N3—Ca1iii | 2.6133 (19) |
Ca1—H61 | 2.74 (5) | O5—H51 | 0.78 (4) |
O1—C7 | 1.267 (3) | O5—H52 | 0.87 (4) |
O1—Ca1ii | 2.4823 (16) | C2—H2 | 0.9300 |
O2—C7 | 1.240 (3) | C4—C8 | 1.523 (3) |
N1—C2 | 1.334 (3) | C8—O3 | 1.253 (3) |
N1—C6 | 1.335 (3) | O8—H82 | 0.77 (5) |
C6—C5 | 1.388 (3) | O8—H81 | 0.76 (4) |
C6—C7 | 1.512 (3) | O3—Ca1iii | 2.4361 (17) |
C5—C4 | 1.385 (3) | | |
| | | |
O5—Ca1—O7 | 148.95 (7) | N1—Ca1—H61 | 163.4 (11) |
O5—Ca1—O3i | 105.11 (8) | N3i—Ca1—H61 | 63.5 (11) |
O7—Ca1—O3i | 86.21 (7) | Ca1ii—Ca1—H61 | 93.9 (11) |
O5—Ca1—O1ii | 82.45 (7) | C7—O1—Ca1ii | 129.56 (14) |
O7—Ca1—O1ii | 103.09 (7) | C7—O1—Ca1 | 122.89 (13) |
O3i—Ca1—O1ii | 148.46 (6) | Ca1ii—O1—Ca1 | 105.91 (6) |
O5—Ca1—O6 | 135.80 (7) | C2—N1—C6 | 116.67 (19) |
O7—Ca1—O6 | 74.03 (7) | C2—N1—Ca1 | 124.75 (14) |
O3i—Ca1—O6 | 79.90 (6) | C6—N1—Ca1 | 118.15 (14) |
O1ii—Ca1—O6 | 74.06 (6) | N1—C6—C5 | 121.77 (19) |
O5—Ca1—O1 | 76.37 (7) | N1—C6—C7 | 117.37 (19) |
O7—Ca1—O1 | 75.95 (7) | C5—C6—C7 | 120.70 (19) |
O3i—Ca1—O1 | 137.32 (5) | C4—C5—C6 | 116.97 (19) |
O1ii—Ca1—O1 | 74.09 (6) | C4—C5—H5 | 121.5 |
O6—Ca1—O1 | 129.21 (6) | C6—C5—H5 | 121.5 |
O5—Ca1—N1 | 73.37 (7) | O2—C7—O1 | 126.4 (2) |
O7—Ca1—N1 | 82.17 (7) | O2—C7—C6 | 116.52 (19) |
O3i—Ca1—N1 | 75.03 (6) | O1—C7—C6 | 117.02 (19) |
O1ii—Ca1—N1 | 135.61 (6) | Ca1—O7—H71 | 126 (2) |
O6—Ca1—N1 | 146.35 (7) | Ca1—O7—H72 | 125 (4) |
O1—Ca1—N1 | 64.43 (5) | H71—O7—H72 | 109 (5) |
O5—Ca1—N3i | 71.93 (7) | Ca1—O6—H62 | 127 (3) |
O7—Ca1—N3i | 137.41 (7) | Ca1—O6—H61 | 97 (3) |
O3i—Ca1—N3i | 63.72 (6) | H62—O6—H61 | 101 (4) |
O1ii—Ca1—N3i | 90.98 (6) | C2—N3—C4 | 116.97 (18) |
O6—Ca1—N3i | 71.62 (7) | C2—N3—Ca1iii | 125.87 (14) |
O1—Ca1—N3i | 146.45 (6) | C4—N3—Ca1iii | 117.02 (14) |
N1—Ca1—N3i | 114.97 (6) | Ca1—O5—H51 | 131 (3) |
O5—Ca1—Ca1ii | 76.69 (6) | Ca1—O5—H52 | 122 (3) |
O7—Ca1—Ca1ii | 89.33 (6) | H51—O5—H52 | 103 (4) |
O3i—Ca1—Ca1ii | 173.73 (4) | N3—C2—N1 | 126.0 (2) |
O1ii—Ca1—Ca1ii | 37.25 (4) | N3—C2—H2 | 117.0 |
O6—Ca1—Ca1ii | 103.10 (5) | N1—C2—H2 | 117.0 |
O1—Ca1—Ca1ii | 36.84 (4) | N3—C4—C5 | 121.6 (2) |
N1—Ca1—Ca1ii | 100.01 (4) | N3—C4—C8 | 116.09 (18) |
N3i—Ca1—Ca1ii | 122.36 (5) | C5—C4—C8 | 122.31 (18) |
O5—Ca1—H61 | 119.2 (10) | O4—C8—O3 | 126.6 (2) |
O7—Ca1—H61 | 88.9 (10) | O4—C8—C4 | 117.21 (19) |
O3i—Ca1—H61 | 90.5 (11) | O3—C8—C4 | 116.20 (18) |
O1ii—Ca1—H61 | 60.1 (11) | H82—O8—H81 | 112 (4) |
O6—Ca1—H61 | 17.9 (10) | C8—O3—Ca1iii | 126.43 (14) |
O1—Ca1—H61 | 126.9 (11) | | |
Symmetry codes: (i) −x+1/2, y−1/2, −z+3/2; (ii) −x, −y, −z+1; (iii) −x+1/2, y+1/2, −z+3/2. |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
O7—H72···O2iv | 0.80 (6) | 2.34 (6) | 3.048 (3) | 149 (6) |
O6—H61···O2ii | 0.85 (5) | 1.88 (5) | 2.698 (3) | 163 (5) |
O8—H81···O3v | 0.76 (4) | 2.04 (4) | 2.793 (3) | 170 (4) |
O8—H82···O6iii | 0.77 (5) | 2.09 (5) | 2.818 (3) | 157 (5) |
O5—H52···O8vi | 0.87 (4) | 1.94 (4) | 2.798 (3) | 169 (4) |
O6—H62···O4iv | 0.77 (4) | 1.96 (4) | 2.719 (2) | 167 (4) |
O7—H71···O4vii | 0.79 (4) | 2.16 (4) | 2.902 (3) | 158 (3) |
O5—H51···O8v | 0.78 (4) | 2.04 (4) | 2.816 (3) | 176 (4) |
Symmetry codes: (ii) −x, −y, −z+1; (iii) −x+1/2, y+1/2, −z+3/2; (iv) x−1/2, −y+1/2, z+1/2; (v) −x+3/2, y−1/2, −z+3/2; (vi) x−1/2, −y+1/2, z−1/2; (vii) −x, −y+1, −z+1. |
Experimental details
Crystal data |
Chemical formula | [Ca2(C6H2N2O4)2(H2O)6]·2H2O |
Mr | 278.24 |
Crystal system, space group | Monoclinic, P21/n |
Temperature (K) | 293 |
a, b, c (Å) | 7.7053 (15), 11.432 (2), 11.916 (2) |
β (°) | 92.16 (3) |
V (Å3) | 1048.9 (4) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 0.64 |
Crystal size (mm) | 0.10 × 0.04 × 0.03 |
|
Data collection |
Diffractometer | Kuma KM-4 four-circle diffractometer |
Absorption correction | Analytical (CrysAlis RED; Oxford Diffraction, 2008) |
Tmin, Tmax | 0.968, 0.982 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 3274, 3065, 1709 |
Rint | 0.049 |
(sin θ/λ)max (Å−1) | 0.705 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.107, 1.01 |
No. of reflections | 3065 |
No. of parameters | 186 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.44, −0.59 |
Selected bond lengths (Å) topCa1—O5 | 2.398 (2) | Ca1—O6 | 2.502 (2) |
Ca1—O7 | 2.420 (2) | Ca1—O1 | 2.5061 (17) |
Ca1—O3i | 2.4361 (17) | Ca1—N1 | 2.563 (2) |
Ca1—O1ii | 2.4823 (16) | Ca1—N3i | 2.6133 (19) |
Symmetry codes: (i) −x+1/2, y−1/2, −z+3/2; (ii) −x, −y, −z+1. |
Hydrogen-bond geometry (Å, º) top D—H···A | D—H | H···A | D···A | D—H···A |
O7—H72···O2iii | 0.80 (6) | 2.34 (6) | 3.048 (3) | 149 (6) |
O6—H61···O2ii | 0.85 (5) | 1.88 (5) | 2.698 (3) | 163 (5) |
O8—H81···O3iv | 0.76 (4) | 2.04 (4) | 2.793 (3) | 170 (4) |
O8—H82···O6v | 0.77 (5) | 2.09 (5) | 2.818 (3) | 157 (5) |
O5—H52···O8vi | 0.87 (4) | 1.94 (4) | 2.798 (3) | 169 (4) |
O6—H62···O4iii | 0.77 (4) | 1.96 (4) | 2.719 (2) | 167 (4) |
O7—H71···O4vii | 0.79 (4) | 2.16 (4) | 2.902 (3) | 158 (3) |
O5—H51···O8iv | 0.78 (4) | 2.04 (4) | 2.816 (3) | 176 (4) |
Symmetry codes: (ii) −x, −y, −z+1; (iii) x−1/2, −y+1/2, z+1/2; (iv) −x+3/2, y−1/2, −z+3/2; (v) −x+1/2, y+1/2, −z+3/2; (vi) x−1/2, −y+1/2, z−1/2; (vii) −x, −y+1, −z+1. |
References
Beobide, G., Castillo, O., Luque, A., Garcia-Couceiro, U., Garcia-Teran, J. P. & Roman, P. (2007). Dalton Trans. pp. 2668–2680. Google Scholar
Kuma (1996). KM-4 Software. Kuma Diffraction Ltd, Wrocław, Poland. Google Scholar
Kuma (2001). DATAPROC. Kuma Diffraction Ltd, Wrocław, Poland. Google Scholar
Oxford Diffraction (2008). CrysAlis RED. Oxford Diffraction Ltd, Yarnton, England. Google Scholar
Sheldrick, G. M. (2008). Acta Cryst. A64, 112–122. Web of Science CrossRef CAS IUCr Journals Google Scholar
Starosta, W., Ptasiewicz-Bąk, H. & Leciejewicz, J. (2003). J. Coord. Chem. 56, 677–682. Web of Science CSD CrossRef CAS Google Scholar
Starosta, W., Ptasiewicz-Bąk, H. & Leciejewicz, J. (2004). J. Coord. Chem. 57, 167–173. Web of Science CSD CrossRef CAS Google Scholar
This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.
 | CRYSTALLOGRAPHIC COMMUNICATIONS |
ISSN: 2056-9890
Open

access
The asymmetric unit of the title compound contains one CaII ion, one fully deprotonated pyrimidine-4,6-diarboxylate ligand molecule, three water molecules coordinated to the metal ion and one solvation water molecule. The ligand molecule acts in µ3 mode and bridges Ca II ions using monodentate N and O atoms and another O atom which is bidentate. One of the O atoms in the carboxylate groups remains uncoordinated. Ca1 and Ca1ii ions are related by an inversion centre and bridged by bidentate carboxylato O1 and O1ii atoms to form a dimeric moiety (Fig.1). Due to the bridging action of the ligands the dimers are the nodes of a cross-linked two dimensional molecular network. The structure of the title compound can be thus visualized as built of molecular layers parallel to the crystal (101) plane (Fig.2). Solvation water molecules are located between adjacent layers. The CaII ion has a distorted eight coordinate geometry. The observed Ca—N and Ca—O bond distances are typical (Table 1). The pyrimidine ring is planar with an r.m.s. of 0.0079 (2) Å; carboxylate groups C7/O1/O2 and C8/O3/O4 make dihedral angles with the plane of 9.7 (1)° and 8.9 (1)°, respectively. Bond distances and bond angles within the pyrimidine ring do not differ from those reported for the parent acid (Beobide, et al., 2007). In a system of hydrogen bonds, which is responsible for structure stability, solvation and coordinated water molecules act as donors and as acceptors and coordination inactive carboxylato O atoms act as acceptors (Table 2). Centro-symmetric dimeric units in which two CaIIions are bridged by ligand bidentate carboxylato O atoms have been also observed in the structures of complexes with pyrazine-2,6-dicarboxylate and water ligands. In all, dimeric units bridged by pairs of coordinated aqua O atoms form "ladder" type molecular ribbons (Starosta, et al., 2003, 2004).