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In the title complex, [Ca(H
2IDC)
2(H
2O)
4]·H
2O, (H
2IDC
− is 4-carboxy-1
H-imidazole-5-carboxylate, C
5H
3N
2O
4−), the Ca
II atom is located on a twofold rotation axis and is
trans-coordinated by two
N,O bidentate H
2IDC
− ligands and four water molecules, resulting in a distorted bicapped triangular prismatic configuration. The water molecule is also located on a twofold rotation axis. A three-dimensional network of N—H
O and O—H
O hydrogen bonds help to stabilize the crystal packing.
Supporting information
CCDC reference: 258647
Key indicators
- Single-crystal X-ray study
- T = 293 K
- Mean (C-C) = 0.002 Å
- R factor = 0.035
- wR factor = 0.097
- Data-to-parameter ratio = 13.3
checkCIF/PLATON results
No syntax errors found
Alert level C
PLAT417_ALERT_2_C Short Inter D-H..H-D H1W1 .. H3W1 .. 2.10 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 5
0 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
2 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
0 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
0 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.
Tetraaquabis(4-carboxy-1
H-imidazole-5-carboxylato-
κ2N,
O)calcium(II) monohydrate
top
Crystal data top
[Ca(C5H3N2O4)2(H2O)4]·H2O | F(000) = 912 |
Mr = 440.35 | Dx = 1.738 Mg m−3 |
Monoclinic, C2/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -C 2yc | Cell parameters from 7559 reflections |
a = 8.2685 (17) Å | θ = 3.1–27.5° |
b = 11.949 (2) Å | µ = 0.46 mm−1 |
c = 17.525 (4) Å | T = 293 K |
β = 103.64 (3)° | Prism, colorless |
V = 1682.6 (6) Å3 | 0.31 × 0.24 × 0.18 mm |
Z = 4 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 1935 independent reflections |
Radiation source: fine-focus sealed tube | 1712 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.027 |
Detector resolution: 10 pixels mm-1 | θmax = 27.5°, θmin = 3.1° |
ω scans | h = −10→10 |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | k = −15→14 |
Tmin = 0.872, Tmax = 0.922 | l = −22→22 |
8019 measured reflections | |
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)] = 0.035 | Hydrogen site location: difmap (O-H) and geom (C-H and N-H) |
wR(F2) = 0.097 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.057P)2 + 1.3396P] where P = (Fo2 + 2Fc2)/3 |
1935 reflections | (Δ/σ)max < 0.001 |
146 parameters | Δρmax = 0.41 e Å−3 |
10 restraints | Δρmin = −0.35 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Ca1 | 0.5000 | 0.72390 (4) | 0.7500 | 0.02287 (15) | |
O1W | 0.70875 (18) | 0.59434 (11) | 0.81017 (8) | 0.0369 (3) | |
H1W1 | 0.794 (2) | 0.5838 (19) | 0.7924 (14) | 0.055* | |
H1W2 | 0.695 (3) | 0.5391 (15) | 0.8383 (12) | 0.055* | |
O2W | 0.74671 (16) | 0.83225 (12) | 0.75453 (7) | 0.0343 (3) | |
H2W1 | 0.780 (3) | 0.844 (2) | 0.7133 (8) | 0.051* | |
H2W2 | 0.827 (2) | 0.815 (2) | 0.7922 (9) | 0.051* | |
O3W | 1.0000 | 0.6155 (2) | 0.7500 | 0.0468 (5) | |
H3W1 | 0.976 (4) | 0.6579 (11) | 0.7090 (3) | 0.070* | |
O1 | 0.41826 (17) | 0.82972 (11) | 0.62113 (7) | 0.0338 (3) | |
O2 | 0.39812 (18) | 0.85077 (11) | 0.49440 (7) | 0.0356 (3) | |
H3 | 0.421 (3) | 0.819 (2) | 0.4548 (10) | 0.053* | |
O3 | 0.50706 (17) | 0.75023 (11) | 0.39001 (7) | 0.0352 (3) | |
O4 | 0.67157 (19) | 0.60530 (11) | 0.38222 (7) | 0.0380 (3) | |
N1 | 0.60049 (17) | 0.63655 (11) | 0.63049 (8) | 0.0249 (3) | |
N2 | 0.69860 (17) | 0.55195 (11) | 0.53903 (8) | 0.0256 (3) | |
H2 | 0.7508 | 0.5040 | 0.5172 | 0.031* | |
C1 | 0.6890 (2) | 0.55164 (14) | 0.61455 (9) | 0.0268 (3) | |
H1 | 0.7388 | 0.4981 | 0.6511 | 0.032* | |
C2 | 0.4507 (2) | 0.79659 (14) | 0.56062 (9) | 0.0250 (3) | |
C3 | 0.55025 (19) | 0.69369 (13) | 0.56097 (9) | 0.0213 (3) | |
C4 | 0.61048 (19) | 0.64226 (13) | 0.50308 (9) | 0.0214 (3) | |
C5 | 0.5957 (2) | 0.66696 (14) | 0.41883 (9) | 0.0251 (3) | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Ca1 | 0.0286 (2) | 0.0235 (2) | 0.0184 (2) | 0.000 | 0.00944 (17) | 0.000 |
O1W | 0.0398 (7) | 0.0338 (7) | 0.0410 (8) | 0.0051 (6) | 0.0173 (6) | 0.0134 (6) |
O2W | 0.0395 (7) | 0.0400 (7) | 0.0260 (6) | −0.0069 (6) | 0.0131 (5) | 0.0033 (5) |
O3W | 0.0422 (11) | 0.0592 (13) | 0.0389 (11) | 0.000 | 0.0092 (9) | 0.000 |
O1 | 0.0467 (7) | 0.0335 (7) | 0.0252 (6) | 0.0144 (6) | 0.0165 (5) | 0.0014 (5) |
O2 | 0.0495 (8) | 0.0365 (7) | 0.0231 (6) | 0.0177 (6) | 0.0134 (6) | 0.0061 (5) |
O3 | 0.0422 (7) | 0.0433 (7) | 0.0207 (6) | 0.0088 (6) | 0.0085 (5) | 0.0059 (5) |
O4 | 0.0604 (9) | 0.0321 (7) | 0.0288 (7) | −0.0005 (6) | 0.0249 (6) | −0.0058 (5) |
N1 | 0.0321 (7) | 0.0247 (7) | 0.0191 (6) | 0.0037 (5) | 0.0087 (5) | 0.0025 (5) |
N2 | 0.0302 (7) | 0.0216 (6) | 0.0269 (7) | 0.0028 (5) | 0.0108 (5) | −0.0025 (5) |
C1 | 0.0338 (9) | 0.0237 (8) | 0.0232 (8) | 0.0033 (6) | 0.0073 (6) | 0.0041 (6) |
C2 | 0.0287 (8) | 0.0262 (8) | 0.0222 (7) | 0.0042 (6) | 0.0101 (6) | 0.0020 (6) |
C3 | 0.0251 (7) | 0.0219 (7) | 0.0178 (7) | 0.0006 (6) | 0.0070 (6) | 0.0001 (6) |
C4 | 0.0233 (7) | 0.0214 (7) | 0.0203 (7) | −0.0007 (6) | 0.0068 (6) | −0.0007 (6) |
C5 | 0.0298 (8) | 0.0274 (8) | 0.0200 (7) | −0.0064 (6) | 0.0093 (6) | −0.0036 (6) |
Geometric parameters (Å, º) top
Ca1—O1W | 2.3726 (14) | N2—C1 | 1.344 (2) |
Ca1—O1 | 2.5370 (13) | N2—C4 | 1.370 (2) |
Ca1—N1 | 2.6434 (14) | N2—H2 | 0.8600 |
Ca1—O2W | 2.4015 (14) | O1W—H1W1 | 0.85 (2) |
Ca1—O1Wi | 2.3726 (14) | O1W—H1W2 | 0.85 (2) |
Ca1—O1i | 2.5370 (13) | O2—H3 | 0.85 (2) |
Ca1—N1i | 2.6434 (14) | O2W—H2W1 | 0.84 (2) |
Ca1—O2Wi | 2.4015 (14) | O2W—H2W2 | 0.84 (2) |
C2—O1 | 1.2194 (19) | O3W—H3W1 | 0.86 (1) |
C2—O2 | 1.310 (2) | C1—H1 | 0.9300 |
C5—O3 | 1.268 (2) | C2—C3 | 1.479 (2) |
C5—O4 | 1.240 (2) | C3—C4 | 1.376 (2) |
N1—C1 | 1.319 (2) | C4—C5 | 1.482 (2) |
N1—C3 | 1.373 (2) | | |
| | | |
N1i—Ca1—N1 | 133.49 (6) | O1—C2—O2 | 120.99 (15) |
O1i—Ca1—N1 | 146.58 (4) | O1—C2—C3 | 120.17 (14) |
O1—Ca1—N1 | 63.83 (4) | O1Wi—Ca1—N1i | 76.28 (5) |
O1i—Ca1—O1 | 120.21 (6) | O1W—Ca1—N1i | 73.85 (5) |
O1Wi—Ca1—N1 | 73.85 (5) | O1Wi—Ca1—O1i | 137.22 (4) |
O1W—Ca1—N1 | 76.28 (5) | O1W—Ca1—O1i | 85.20 (5) |
O1Wi—Ca1—O1 | 85.20 (5) | O1Wi—Ca1—O2Wi | 79.27 (5) |
O1W—Ca1—O1 | 137.22 (4) | O1W—Ca1—O2Wi | 152.84 (4) |
O1Wi—Ca1—O1W | 98.54 (8) | O2—C2—C3 | 118.84 (13) |
O1Wi—Ca1—O2W | 152.84 (4) | O2W—Ca1—N1i | 127.59 (5) |
O1W—Ca1—O2W | 79.27 (5) | O2Wi—Ca1—N1i | 79.38 (5) |
O2W—Ca1—O2Wi | 114.75 (7) | O2W—Ca1—O1i | 69.88 (5) |
O2W—Ca1—N1 | 79.38 (5) | O2Wi—Ca1—O1i | 78.85 (5) |
O2Wi—Ca1—N1 | 127.59 (5) | O3—C5—C4 | 117.19 (14) |
O2W—Ca1—O1 | 78.85 (5) | O4—C5—O3 | 125.14 (15) |
O2Wi—Ca1—O1 | 69.88 (5) | O4—C5—C4 | 117.67 (15) |
Ca1—O1W—H1W1 | 121.2 (15) | C1—N1—Ca1 | 139.94 (11) |
Ca1—O1W—H1W2 | 125.6 (15) | C1—N1—C3 | 105.16 (13) |
Ca1—O2W—H2W1 | 120.6 (16) | C1—N2—C4 | 107.86 (13) |
Ca1—O2W—H2W2 | 113.4 (17) | C1—N2—H2 | 126.1 |
N1—C1—N2 | 111.77 (14) | C2—O1—Ca1 | 123.04 (11) |
N1—C1—H1 | 124.1 | C2—O2—H3 | 114.1 (18) |
N1—C3—C4 | 110.24 (14) | C3—N1—Ca1 | 114.90 (10) |
N1—C3—C2 | 117.95 (13) | C3—C4—C5 | 133.36 (15) |
N2—C1—H1 | 124.1 | C4—N2—H2 | 126.1 |
N2—C4—C3 | 104.98 (13) | C4—C3—C2 | 131.77 (14) |
N2—C4—C5 | 121.67 (14) | H1W1—O1W—H1W2 | 109.7 (14) |
O1i—Ca1—N1i | 63.83 (4) | H2W1—O2W—H2W2 | 110.9 (15) |
O1—Ca1—N1i | 146.58 (4) | | |
| | | |
Ca1—N1—C1—N2 | −179.10 (12) | O1Wi—Ca1—N1—C3 | 90.72 (12) |
Ca1—O1—C2—O2 | 176.21 (12) | O1W—Ca1—N1—C3 | −165.99 (12) |
Ca1—O1—C2—C3 | −3.6 (2) | O1Wi—Ca1—O1—C2 | −71.38 (14) |
Ca1—N1—C3—C4 | 179.31 (10) | O1W—Ca1—O1—C2 | 26.02 (17) |
Ca1—N1—C3—C2 | 1.16 (18) | O2—C2—C3—N1 | −178.35 (15) |
N1i—Ca1—N1—C1 | −37.84 (17) | O2—C2—C3—C4 | 4.0 (3) |
N1i—Ca1—N1—C3 | 142.77 (12) | O2W—Ca1—N1—C1 | 94.81 (18) |
N1i—Ca1—O1—C2 | −127.38 (13) | O2Wi—Ca1—N1—C1 | −152.03 (17) |
N1—Ca1—O1—C2 | 2.97 (13) | O2W—Ca1—N1—C3 | −84.57 (11) |
N1—C3—C4—N2 | 0.14 (18) | O2Wi—Ca1—N1—C3 | 28.59 (13) |
N1—C3—C4—C5 | −179.92 (16) | O2W—Ca1—O1—C2 | 86.52 (14) |
N2—C4—C5—O3 | 177.71 (15) | O2Wi—Ca1—O1—C2 | −151.70 (15) |
N2—C4—C5—O4 | −2.7 (2) | C1—N1—C3—C2 | −178.43 (15) |
O1i—Ca1—N1—C1 | 71.6 (2) | C1—N1—C3—C4 | −0.28 (18) |
O1—Ca1—N1—C1 | 177.51 (19) | C1—N2—C4—C3 | 0.06 (17) |
O1i—Ca1—N1—C3 | −107.74 (12) | C1—N2—C4—C5 | −179.89 (14) |
O1—Ca1—N1—C3 | −1.88 (10) | C2—C3—C4—N2 | 177.95 (17) |
O1i—Ca1—O1—C2 | 145.15 (15) | C2—C3—C4—C5 | −2.1 (3) |
O1—C2—C3—N1 | 1.5 (2) | C3—N1—C1—N2 | 0.33 (19) |
O1—C2—C3—C4 | −176.19 (17) | C3—C4—C5—O3 | −2.2 (3) |
O1Wi—Ca1—N1—C1 | −89.89 (18) | C3—C4—C5—O4 | 177.35 (17) |
O1W—Ca1—N1—C1 | 13.39 (17) | C4—N2—C1—N1 | −0.25 (19) |
Symmetry code: (i) −x+1, y, −z+3/2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2—H2···O2ii | 0.86 | 2.29 | 3.118 (2) | 163 |
O2W—H2W1···O4iii | 0.84 (2) | 1.91 (2) | 2.742 (2) | 169 (2) |
O1W—H1W1···O3W | 0.85 (2) | 2.05 (2) | 2.859 (2) | 161 (2) |
O1W—H1W2···O4iv | 0.85 (2) | 1.92 (2) | 2.750 (2) | 167 (2) |
O2W—H2W2···O3v | 0.84 (2) | 2.13 (2) | 2.972 (2) | 171 (2) |
O2—H3···O3 | 0.85 (2) | 1.69 (2) | 2.526 (2) | 167 (3) |
O3W—H3W1···O3iii | 0.86 (1) | 2.09 (2) | 2.921 (2) | 162 (3) |
Symmetry codes: (ii) x+1/2, y−1/2, z; (iii) −x+3/2, −y+3/2, −z+1; (iv) x, −y+1, z+1/2; (v) x+1/2, −y+3/2, z+1/2. |
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