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In the title complex, [Ca(H2IDC)2(H2O)4]·H2O, (H2IDC is 4-carboxy-1H-imidazole-5-carboxyl­ate, C5H3N2O4), the CaII atom is located on a twofold rotation axis and is trans-coordinated by two N,O bidentate H2IDC 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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804028132/hb6121sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804028132/hb6121Isup2.hkl
Contains datablock I

CCDC reference: 258647

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](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

Computing details top

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-1H-imidazole-5-carboxylato-κ2N,O)calcium(II) monohydrate top
Crystal data top
[Ca(C5H3N2O4)2(H2O)4]·H2OF(000) = 912
Mr = 440.35Dx = 1.738 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 7559 reflections
a = 8.2685 (17) Åθ = 3.1–27.5°
b = 11.949 (2) ŵ = 0.46 mm1
c = 17.525 (4) ÅT = 293 K
β = 103.64 (3)°Prism, colorless
V = 1682.6 (6) Å30.31 × 0.24 × 0.18 mm
Z = 4
Data collection top
Rigaku R-AXIS RAPID
diffractometer
1935 independent reflections
Radiation source: fine-focus sealed tube1712 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.027
Detector resolution: 10 pixels mm-1θmax = 27.5°, θmin = 3.1°
ω scansh = 1010
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
k = 1514
Tmin = 0.872, Tmax = 0.922l = 2222
8019 measured reflections
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.035Hydrogen site location: difmap (O-H) and geom (C-H and N-H)
wR(F2) = 0.097H 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 parametersΔρmax = 0.41 e Å3
10 restraintsΔρmin = 0.35 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Ca10.50000.72390 (4)0.75000.02287 (15)
O1W0.70875 (18)0.59434 (11)0.81017 (8)0.0369 (3)
H1W10.794 (2)0.5838 (19)0.7924 (14)0.055*
H1W20.695 (3)0.5391 (15)0.8383 (12)0.055*
O2W0.74671 (16)0.83225 (12)0.75453 (7)0.0343 (3)
H2W10.780 (3)0.844 (2)0.7133 (8)0.051*
H2W20.827 (2)0.815 (2)0.7922 (9)0.051*
O3W1.00000.6155 (2)0.75000.0468 (5)
H3W10.976 (4)0.6579 (11)0.7090 (3)0.070*
O10.41826 (17)0.82972 (11)0.62113 (7)0.0338 (3)
O20.39812 (18)0.85077 (11)0.49440 (7)0.0356 (3)
H30.421 (3)0.819 (2)0.4548 (10)0.053*
O30.50706 (17)0.75023 (11)0.39001 (7)0.0352 (3)
O40.67157 (19)0.60530 (11)0.38222 (7)0.0380 (3)
N10.60049 (17)0.63655 (11)0.63049 (8)0.0249 (3)
N20.69860 (17)0.55195 (11)0.53903 (8)0.0256 (3)
H20.75080.50400.51720.031*
C10.6890 (2)0.55164 (14)0.61455 (9)0.0268 (3)
H10.73880.49810.65110.032*
C20.4507 (2)0.79659 (14)0.56062 (9)0.0250 (3)
C30.55025 (19)0.69369 (13)0.56097 (9)0.0213 (3)
C40.61048 (19)0.64226 (13)0.50308 (9)0.0214 (3)
C50.5957 (2)0.66696 (14)0.41883 (9)0.0251 (3)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ca10.0286 (2)0.0235 (2)0.0184 (2)0.0000.00944 (17)0.000
O1W0.0398 (7)0.0338 (7)0.0410 (8)0.0051 (6)0.0173 (6)0.0134 (6)
O2W0.0395 (7)0.0400 (7)0.0260 (6)0.0069 (6)0.0131 (5)0.0033 (5)
O3W0.0422 (11)0.0592 (13)0.0389 (11)0.0000.0092 (9)0.000
O10.0467 (7)0.0335 (7)0.0252 (6)0.0144 (6)0.0165 (5)0.0014 (5)
O20.0495 (8)0.0365 (7)0.0231 (6)0.0177 (6)0.0134 (6)0.0061 (5)
O30.0422 (7)0.0433 (7)0.0207 (6)0.0088 (6)0.0085 (5)0.0059 (5)
O40.0604 (9)0.0321 (7)0.0288 (7)0.0005 (6)0.0249 (6)0.0058 (5)
N10.0321 (7)0.0247 (7)0.0191 (6)0.0037 (5)0.0087 (5)0.0025 (5)
N20.0302 (7)0.0216 (6)0.0269 (7)0.0028 (5)0.0108 (5)0.0025 (5)
C10.0338 (9)0.0237 (8)0.0232 (8)0.0033 (6)0.0073 (6)0.0041 (6)
C20.0287 (8)0.0262 (8)0.0222 (7)0.0042 (6)0.0101 (6)0.0020 (6)
C30.0251 (7)0.0219 (7)0.0178 (7)0.0006 (6)0.0070 (6)0.0001 (6)
C40.0233 (7)0.0214 (7)0.0203 (7)0.0007 (6)0.0068 (6)0.0007 (6)
C50.0298 (8)0.0274 (8)0.0200 (7)0.0064 (6)0.0093 (6)0.0036 (6)
Geometric parameters (Å, º) top
Ca1—O1W2.3726 (14)N2—C11.344 (2)
Ca1—O12.5370 (13)N2—C41.370 (2)
Ca1—N12.6434 (14)N2—H20.8600
Ca1—O2W2.4015 (14)O1W—H1W10.85 (2)
Ca1—O1Wi2.3726 (14)O1W—H1W20.85 (2)
Ca1—O1i2.5370 (13)O2—H30.85 (2)
Ca1—N1i2.6434 (14)O2W—H2W10.84 (2)
Ca1—O2Wi2.4015 (14)O2W—H2W20.84 (2)
C2—O11.2194 (19)O3W—H3W10.86 (1)
C2—O21.310 (2)C1—H10.9300
C5—O31.268 (2)C2—C31.479 (2)
C5—O41.240 (2)C3—C41.376 (2)
N1—C11.319 (2)C4—C51.482 (2)
N1—C31.373 (2)
N1i—Ca1—N1133.49 (6)O1—C2—O2120.99 (15)
O1i—Ca1—N1146.58 (4)O1—C2—C3120.17 (14)
O1—Ca1—N163.83 (4)O1Wi—Ca1—N1i76.28 (5)
O1i—Ca1—O1120.21 (6)O1W—Ca1—N1i73.85 (5)
O1Wi—Ca1—N173.85 (5)O1Wi—Ca1—O1i137.22 (4)
O1W—Ca1—N176.28 (5)O1W—Ca1—O1i85.20 (5)
O1Wi—Ca1—O185.20 (5)O1Wi—Ca1—O2Wi79.27 (5)
O1W—Ca1—O1137.22 (4)O1W—Ca1—O2Wi152.84 (4)
O1Wi—Ca1—O1W98.54 (8)O2—C2—C3118.84 (13)
O1Wi—Ca1—O2W152.84 (4)O2W—Ca1—N1i127.59 (5)
O1W—Ca1—O2W79.27 (5)O2Wi—Ca1—N1i79.38 (5)
O2W—Ca1—O2Wi114.75 (7)O2W—Ca1—O1i69.88 (5)
O2W—Ca1—N179.38 (5)O2Wi—Ca1—O1i78.85 (5)
O2Wi—Ca1—N1127.59 (5)O3—C5—C4117.19 (14)
O2W—Ca1—O178.85 (5)O4—C5—O3125.14 (15)
O2Wi—Ca1—O169.88 (5)O4—C5—C4117.67 (15)
Ca1—O1W—H1W1121.2 (15)C1—N1—Ca1139.94 (11)
Ca1—O1W—H1W2125.6 (15)C1—N1—C3105.16 (13)
Ca1—O2W—H2W1120.6 (16)C1—N2—C4107.86 (13)
Ca1—O2W—H2W2113.4 (17)C1—N2—H2126.1
N1—C1—N2111.77 (14)C2—O1—Ca1123.04 (11)
N1—C1—H1124.1C2—O2—H3114.1 (18)
N1—C3—C4110.24 (14)C3—N1—Ca1114.90 (10)
N1—C3—C2117.95 (13)C3—C4—C5133.36 (15)
N2—C1—H1124.1C4—N2—H2126.1
N2—C4—C3104.98 (13)C4—C3—C2131.77 (14)
N2—C4—C5121.67 (14)H1W1—O1W—H1W2109.7 (14)
O1i—Ca1—N1i63.83 (4)H2W1—O2W—H2W2110.9 (15)
O1—Ca1—N1i146.58 (4)
Ca1—N1—C1—N2179.10 (12)O1Wi—Ca1—N1—C390.72 (12)
Ca1—O1—C2—O2176.21 (12)O1W—Ca1—N1—C3165.99 (12)
Ca1—O1—C2—C33.6 (2)O1Wi—Ca1—O1—C271.38 (14)
Ca1—N1—C3—C4179.31 (10)O1W—Ca1—O1—C226.02 (17)
Ca1—N1—C3—C21.16 (18)O2—C2—C3—N1178.35 (15)
N1i—Ca1—N1—C137.84 (17)O2—C2—C3—C44.0 (3)
N1i—Ca1—N1—C3142.77 (12)O2W—Ca1—N1—C194.81 (18)
N1i—Ca1—O1—C2127.38 (13)O2Wi—Ca1—N1—C1152.03 (17)
N1—Ca1—O1—C22.97 (13)O2W—Ca1—N1—C384.57 (11)
N1—C3—C4—N20.14 (18)O2Wi—Ca1—N1—C328.59 (13)
N1—C3—C4—C5179.92 (16)O2W—Ca1—O1—C286.52 (14)
N2—C4—C5—O3177.71 (15)O2Wi—Ca1—O1—C2151.70 (15)
N2—C4—C5—O42.7 (2)C1—N1—C3—C2178.43 (15)
O1i—Ca1—N1—C171.6 (2)C1—N1—C3—C40.28 (18)
O1—Ca1—N1—C1177.51 (19)C1—N2—C4—C30.06 (17)
O1i—Ca1—N1—C3107.74 (12)C1—N2—C4—C5179.89 (14)
O1—Ca1—N1—C31.88 (10)C2—C3—C4—N2177.95 (17)
O1i—Ca1—O1—C2145.15 (15)C2—C3—C4—C52.1 (3)
O1—C2—C3—N11.5 (2)C3—N1—C1—N20.33 (19)
O1—C2—C3—C4176.19 (17)C3—C4—C5—O32.2 (3)
O1Wi—Ca1—N1—C189.89 (18)C3—C4—C5—O4177.35 (17)
O1W—Ca1—N1—C113.39 (17)C4—N2—C1—N10.25 (19)
Symmetry code: (i) x+1, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N2—H2···O2ii0.862.293.118 (2)163
O2W—H2W1···O4iii0.84 (2)1.91 (2)2.742 (2)169 (2)
O1W—H1W1···O3W0.85 (2)2.05 (2)2.859 (2)161 (2)
O1W—H1W2···O4iv0.85 (2)1.92 (2)2.750 (2)167 (2)
O2W—H2W2···O3v0.84 (2)2.13 (2)2.972 (2)171 (2)
O2—H3···O30.85 (2)1.69 (2)2.526 (2)167 (3)
O3W—H3W1···O3iii0.86 (1)2.09 (2)2.921 (2)162 (3)
Symmetry codes: (ii) x+1/2, y1/2, 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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