Literature DB >> 22969488

Triaqua[2,2'-(propane-1,3-diyl)bis(5-carboxy-1H-imidazole-4-carboxylato-κ(2)N(3),O(4))]calcium(II) tetrahydrate.

Ling-Zhi Du1, Xia Li.   

Abstract

In the title compound, [Ca(C(13)H(10)N(4)O(8))(n class="Chemical">H(2)O)(3)]·4H(2)O, the Ca(II) ion is hepta-coordinated by two N atoms and two O atoms from a tetra-dentate 1,3-bis-(1H-imidazole-4,5-dicarb-oxy-l-ate) propane dianion and three water O atoms, giving a distorted penta-gonal-bipyramidal coordination environment. The Ca-O bond lengths are in the range 2.354 (3)-2.453 (2) Å, while the Ca-N bond lengths are in the range 2.523 (2)-2.548 (2) Å. An intra-molecular O-H⋯O hydrogen bond between the carb-oxy and carboxyl-ate groups stabilizes the mol-ecular configuration. A three-dimensional network of N-H⋯O and O-H⋯O hydrogen bonds help to stabilize the crystal packing.

Entities:  

Year:  2012        PMID： 22969488      PMCID： PMC3435615          DOI： 10.1107/S1600536812035544

Source DB:  PubMed          Journal:  Acta Crystallogr Sect E Struct Rep Online        ISSN： 1600-5368


Related literature

For complexes based on 4,5-imidazole­din class="Chemical">carb­oxy­lic acid, see: Zhu et al. (2010 ▶); Lu et al. (2010 ▶). For complexes based on 2-methyl-1H-imidazole-4,5-dicarb­oxy­lic acid, see: Song et al. (2010 ▶). For complexes based on 2-ethyl-1H-imidazole-4,5-dicarb­oxy­lic acid, see: Zhang et al. (2010 ▶); Wang et al. (2008 ▶). For complexes based on 2-propyl-1H-imidazole-4,5-dicarb­oxy­lic acid, see: Feng et al. (2010 ▶); Liu et al. (2010 ▶). For complexes based on 2-(hy­droxy­meth­yl)-1H-imidazole-4,5-dicarb­oxy­lic acid, see: Zheng et al. (2011 ▶). For complexes based on 2-phenyl-1H-imidazole-4,5-dicarb­oxy­lic acid, see: Zhu et al. (2011 ▶). For complexes based on 2-pyridyl-1H-imidazole-4,5-dicarb­oxy­lic acid, see: Li et al. (2009 ▶, 2010 ▶).

Experimental

Crystal data

[Ca(C13H10N4O8)(n class="Chemical">H2O3)3]·4H2O M = 516.44 Triclinic, a = 6.7794 (12) Å b = 12.172 (2) Å c = 13.718 (2) Å α = 98.776 (2)° β = 102.420 (2)° γ = 90.444 (2)° V = 1091.6 (3) Å3 Z = 2 Mo Kα radiation μ = 0.37 mm−1 T = 296 K 0.16 × 0.16 × 0.14 mm

Data collection

Bruker SMART CCD diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 2001 ▶) T min = 0.943, T max = 0.950 8318 measured reflections 4031 independent reflections 2595 reflections with I > 2σ(I) R int = 0.040

Refinement

R[F 2 > 2σ(F 2)] = 0.048 wR(F 2) = 0.098 S = 1.01 4031 reflections 344 parameters 14 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.24 e Å−3 Δρmin = −0.32 e Å−3 Data collection: SMART (Bruker, 2001 ▶); cell refinement: SAINT (Bruker, 2001 ▶); data reduction: SAIn class="Chemical">NT; 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. Crystal structure: contains datablock(s) I, global. DOI: 10.1107/S1600536812035544/ff2078sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812035544/ff2078Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Ca(C13H10N4O8)(H2O3)3]·4H2OZ = 2
Mr = 516.44F(000) = 540
Triclinic, P1Dx = 1.571 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 6.7794 (12) ÅCell parameters from 1354 reflections
b = 12.172 (2) Åθ = 2.5–23.1°
c = 13.718 (2) ŵ = 0.37 mm−1
α = 98.776 (2)°T = 296 K
β = 102.420 (2)°Block, colourless
γ = 90.444 (2)°0.16 × 0.16 × 0.14 mm
V = 1091.6 (3) Å3
Bruker SMART CCD diffractometer4031 independent reflections
Radiation source: X-ray tube2595 reflections with I > 2σ(I)
Phi and omega scans monochromatorRint = 0.040
φ and ω scansθmax = 25.5°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)h = −8→8
Tmin = 0.943, Tmax = 0.950k = −14→14
8318 measured reflectionsl = −16→16
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.048Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.098H atoms treated by a mixture of independent and constrained refinement
S = 1.01w = 1/[σ2(Fo2) + (0.0327P)2 + 0.2508P] where P = (Fo2 + 2Fc2)/3
4031 reflections(Δ/σ)max < 0.001
344 parametersΔρmax = 0.24 e Å−3
14 restraintsΔρmin = −0.32 e Å−3
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.
xyzUiso*/Ueq
Ca10.34365 (10)0.10418 (5)0.30772 (5)0.02902 (18)
O10.4347 (3)0.17772 (16)0.48632 (15)0.0339 (5)
O20.4429 (3)0.31736 (17)0.61241 (15)0.0404 (6)
O30.3556 (3)0.51623 (17)0.63708 (15)0.0381 (6)
H30.38140.45020.63090.046*
O40.2140 (3)0.63567 (16)0.53912 (16)0.0375 (6)
O50.2380 (4)0.07270 (19)−0.21218 (17)0.0498 (7)
O60.1955 (4)−0.08158 (19)−0.14977 (16)0.0489 (7)
H60.1955−0.0984−0.09410.059*
O70.2100 (3)−0.14045 (16)0.01549 (16)0.0406 (6)
O80.2447 (3)−0.05781 (16)0.17484 (16)0.0379 (6)
O90.0695 (4)0.03304 (19)0.36754 (17)0.0414 (6)
O100.5458 (4)−0.0399 (2)0.36928 (19)0.0464 (6)
O110.6575 (4)0.1900 (2)0.31047 (19)0.0432 (6)
O120.9370 (5)0.1553 (2)0.5324 (2)0.0604 (8)
O130.3808 (5)0.3595 (3)0.8695 (2)0.0670 (8)
O14−0.0383 (4)0.6606 (2)0.2953 (2)0.0514 (7)
O150.2804 (4)0.7234 (2)0.21968 (19)0.0511 (7)
N10.2148 (4)0.29607 (19)0.34785 (17)0.0282 (6)
N20.1366 (4)0.47230 (19)0.36829 (18)0.0278 (6)
H20.09020.53490.35420.033*
N30.2951 (4)0.14885 (19)0.12881 (17)0.0296 (6)
N40.2984 (4)0.1999 (2)−0.01827 (18)0.0322 (6)
H40.30660.2417−0.06260.039*
C10.2844 (4)0.3426 (2)0.4475 (2)0.0246 (7)
C20.2362 (4)0.4526 (2)0.4611 (2)0.0248 (7)
C30.1233 (5)0.3772 (2)0.3025 (2)0.0281 (7)
C40.3947 (5)0.2746 (2)0.5201 (2)0.0288 (7)
C50.2698 (4)0.5412 (2)0.5491 (2)0.0282 (7)
C60.0236 (5)0.3679 (3)0.1933 (2)0.0382 (9)
H6A−0.10090.40760.18720.046*
H6B−0.01160.29020.16610.046*
C70.1548 (6)0.4140 (3)0.1298 (2)0.0471 (10)
H7A0.18730.49220.15600.056*
H7B0.07750.40870.06090.056*
C80.3519 (5)0.3533 (2)0.1291 (2)0.0421 (9)
H8A0.43240.39090.09260.050*
H8B0.42840.35740.19810.050*
C90.3172 (5)0.2347 (2)0.0816 (2)0.0311 (8)
C100.2618 (4)0.0566 (2)0.0547 (2)0.0271 (7)
C110.2642 (4)0.0872 (2)−0.0371 (2)0.0300 (7)
C120.2371 (4)−0.0524 (2)0.0845 (2)0.0305 (7)
C130.2322 (5)0.0231 (3)−0.1405 (3)0.0376 (8)
H5W0.720 (5)0.247 (2)0.350 (2)0.083 (15)*
H6W0.726 (5)0.167 (3)0.266 (2)0.080 (15)*
H4W0.542 (5)−0.083 (2)0.4128 (19)0.054 (12)*
H3W0.612 (5)−0.067 (3)0.325 (2)0.070 (14)*
H13W0.370 (5)0.728 (4)0.276 (2)0.106*
H12W0.062 (5)0.683 (4)0.273 (3)0.106*
H2W−0.032 (4)0.000 (3)0.324 (3)0.106*
H14W0.269 (7)0.7895 (16)0.205 (3)0.106*
H11W−0.052 (7)0.709 (3)0.346 (2)0.106*
H9W0.498 (3)0.345 (4)0.858 (4)0.106*
H7W0.904 (7)0.102 (3)0.560 (3)0.106*
H10W0.280 (5)0.360 (4)0.820 (2)0.106*
H1W0.026 (6)0.074 (3)0.415 (2)0.106*
H8W0.844 (5)0.197 (3)0.509 (3)0.106*
U11U22U33U12U13U23
Ca10.0426 (4)0.0223 (3)0.0218 (4)0.0014 (3)0.0072 (3)0.0021 (3)
O10.0529 (15)0.0228 (11)0.0259 (13)0.0087 (10)0.0080 (11)0.0040 (9)
O20.0593 (16)0.0390 (13)0.0192 (12)0.0103 (11)0.0017 (11)0.0028 (10)
O30.0533 (15)0.0305 (12)0.0266 (13)0.0024 (11)0.0052 (11)−0.0029 (10)
O40.0464 (14)0.0253 (12)0.0377 (14)0.0017 (11)0.0076 (11)−0.0020 (10)
O50.0657 (18)0.0576 (16)0.0262 (14)−0.0151 (13)0.0167 (12)−0.0011 (12)
O60.0706 (18)0.0461 (15)0.0284 (14)−0.0049 (13)0.0158 (12)−0.0062 (11)
O70.0509 (15)0.0258 (12)0.0396 (14)0.0010 (11)0.0072 (12)−0.0082 (10)
O80.0527 (15)0.0292 (12)0.0305 (14)0.0000 (11)0.0054 (11)0.0054 (10)
O90.0456 (16)0.0444 (15)0.0321 (15)−0.0064 (12)0.0074 (12)0.0017 (11)
O100.0652 (18)0.0437 (15)0.0390 (16)0.0190 (13)0.0217 (14)0.0182 (13)
O110.0504 (17)0.0382 (14)0.0371 (16)−0.0096 (12)0.0149 (13)−0.0127 (12)
O120.087 (2)0.0513 (18)0.0465 (17)0.0267 (15)0.0146 (15)0.0186 (13)
O130.075 (2)0.075 (2)0.058 (2)−0.0009 (19)0.0211 (17)0.0238 (16)
O140.0622 (18)0.0382 (15)0.0601 (19)0.0109 (14)0.0211 (15)0.0165 (12)
O150.0573 (18)0.0431 (15)0.0495 (17)−0.0013 (14)−0.0018 (13)0.0165 (13)
N10.0368 (16)0.0250 (13)0.0210 (14)0.0012 (12)0.0037 (12)0.0015 (11)
N20.0352 (16)0.0204 (13)0.0263 (15)0.0020 (11)0.0053 (12)0.0015 (11)
N30.0404 (17)0.0260 (14)0.0195 (14)−0.0014 (12)0.0030 (12)−0.0004 (11)
N40.0396 (17)0.0356 (15)0.0225 (15)−0.0009 (13)0.0082 (12)0.0063 (12)
C10.0309 (18)0.0224 (16)0.0207 (17)0.0006 (13)0.0073 (14)0.0015 (13)
C20.0263 (17)0.0258 (16)0.0215 (16)0.0012 (13)0.0061 (14)0.0004 (13)
C30.0319 (19)0.0247 (16)0.0279 (18)0.0013 (14)0.0057 (15)0.0057 (14)
C40.0320 (19)0.0275 (17)0.0275 (19)−0.0011 (14)0.0081 (15)0.0045 (14)
C50.0250 (18)0.0281 (18)0.0306 (19)−0.0040 (14)0.0071 (15)0.0005 (14)
C60.050 (2)0.0294 (18)0.0276 (19)0.0061 (16)−0.0030 (16)−0.0017 (15)
C70.086 (3)0.0274 (18)0.0260 (19)0.0087 (19)0.0066 (19)0.0060 (15)
C80.066 (3)0.0328 (19)0.0253 (19)−0.0139 (18)0.0116 (18)−0.0024 (15)
C90.042 (2)0.0301 (17)0.0214 (18)−0.0005 (15)0.0074 (15)0.0034 (14)
C100.0255 (17)0.0289 (16)0.0253 (18)0.0015 (14)0.0050 (14)0.0001 (14)
C110.0282 (18)0.0314 (18)0.0276 (19)−0.0001 (14)0.0074 (15)−0.0058 (14)
C120.0256 (18)0.0288 (17)0.034 (2)0.0036 (14)0.0026 (15)0.0004 (15)
C130.035 (2)0.046 (2)0.030 (2)−0.0069 (17)0.0116 (16)−0.0051 (17)
Ca1—O112.354 (3)O14—H11W0.860 (10)
Ca1—O102.379 (3)O15—H13W0.864 (10)
Ca1—O92.393 (3)O15—H14W0.859 (10)
Ca1—O12.420 (2)N1—C31.333 (3)
Ca1—O82.453 (2)N1—C11.377 (3)
Ca1—N12.523 (2)N2—C31.345 (3)
Ca1—N32.548 (2)N2—C21.364 (3)
Ca1—H3W2.78 (3)N2—H20.8600
O1—C41.253 (3)N3—C91.333 (4)
O2—C41.265 (3)N3—C101.376 (3)
O3—C51.304 (3)N4—C91.349 (3)
O3—H30.8200N4—C111.366 (4)
O4—C51.232 (3)N4—H40.8600
O5—C131.237 (4)C1—C21.375 (4)
O6—C131.279 (4)C1—C41.475 (4)
O6—H60.8200C2—C51.467 (4)
O7—C121.301 (3)C3—C61.492 (4)
O8—C121.242 (3)C6—C71.529 (5)
O9—H2W0.861 (10)C6—H6A0.9700
O9—H1W0.859 (10)C6—H6B0.9700
O10—H4W0.859 (10)C7—C81.533 (5)
O10—H3W0.855 (10)C7—H7A0.9700
O11—H5W0.855 (10)C7—H7B0.9700
O11—H6W0.858 (10)C8—C91.486 (4)
O12—H7W0.858 (10)C8—H8A0.9700
O12—H8W0.852 (10)C8—H8B0.9700
O13—H9W0.856 (10)C10—C111.370 (4)
O13—H10W0.856 (10)C10—C121.465 (4)
O14—H12W0.862 (10)C11—C131.482 (4)
O11—Ca1—O1083.73 (10)C10—N3—Ca1114.06 (19)
O11—Ca1—O9159.80 (9)C9—N4—C11108.4 (2)
O10—Ca1—O989.24 (9)C9—N4—H4125.8
O11—Ca1—O181.93 (8)C11—N4—H4125.8
O10—Ca1—O179.49 (8)C2—C1—N1109.7 (3)
O9—Ca1—O178.17 (8)C2—C1—C4130.5 (3)
O11—Ca1—O8114.31 (8)N1—C1—C4119.9 (2)
O10—Ca1—O875.75 (8)N2—C2—C1105.6 (2)
O9—Ca1—O881.96 (8)N2—C2—C5120.8 (3)
O1—Ca1—O8148.28 (7)C1—C2—C5133.6 (3)
O11—Ca1—N187.84 (8)N1—C3—N2110.8 (3)
O10—Ca1—N1146.79 (9)N1—C3—C6126.0 (3)
O9—Ca1—N187.76 (8)N2—C3—C6123.1 (3)
O1—Ca1—N167.53 (7)O1—C4—O2124.0 (3)
O8—Ca1—N1136.25 (8)O1—C4—C1117.8 (3)
O11—Ca1—N377.65 (9)O2—C4—C1118.2 (3)
O10—Ca1—N3124.49 (9)O4—C5—O3121.7 (3)
O9—Ca1—N3121.47 (8)O4—C5—C2120.1 (3)
O1—Ca1—N3145.79 (7)O3—C5—C2118.3 (3)
O8—Ca1—N365.91 (7)C3—C6—C7113.7 (3)
N1—Ca1—N384.44 (8)C3—C6—H6A108.8
O11—Ca1—H3W76.2 (7)C7—C6—H6A108.8
O10—Ca1—H3W16.9 (5)C3—C6—H6B108.8
O9—Ca1—H3W101.5 (6)C7—C6—H6B108.8
O1—Ca1—H3W93.4 (6)H6A—C6—H6B107.7
O8—Ca1—H3W66.6 (7)C6—C7—C8113.6 (3)
N1—Ca1—H3W156.9 (8)C6—C7—H7A108.9
N3—Ca1—H3W107.8 (5)C8—C7—H7A108.9
C4—O1—Ca1121.77 (19)C6—C7—H7B108.9
C5—O3—H3109.5C8—C7—H7B108.9
C13—O6—H6109.5H7A—C7—H7B107.7
C12—O8—Ca1121.90 (19)C9—C8—C7112.8 (3)
Ca1—O9—H2W118 (3)C9—C8—H8A109.0
Ca1—O9—H1W119 (3)C7—C8—H8A109.0
H2W—O9—H1W109 (4)C9—C8—H8B109.0
Ca1—O10—H4W136 (2)C7—C8—H8B109.0
Ca1—O10—H3W109 (3)H8A—C8—H8B107.8
H4W—O10—H3W112 (4)N3—C9—N4110.5 (2)
Ca1—O11—H5W130 (3)N3—C9—C8126.2 (3)
Ca1—O11—H6W121 (3)N4—C9—C8123.3 (3)
H5W—O11—H6W109 (4)C11—C10—N3110.0 (3)
H7W—O12—H8W118 (5)C11—C10—C12131.7 (3)
H9W—O13—H10W120 (5)N3—C10—C12118.3 (3)
H12W—O14—H11W108 (4)N4—C11—C10105.5 (3)
H13W—O15—H14W106 (4)N4—C11—C13122.0 (3)
C3—N1—C1105.5 (2)C10—C11—C13132.5 (3)
C3—N1—Ca1141.1 (2)O8—C12—O7122.1 (3)
C1—N1—Ca1112.41 (17)O8—C12—C10119.0 (3)
C3—N2—C2108.4 (2)O7—C12—C10118.9 (3)
C3—N2—H2125.8O5—C13—O6124.0 (3)
C2—N2—H2125.8O5—C13—C11119.3 (3)
C9—N3—C10105.6 (2)O6—C13—C11116.7 (3)
C9—N3—Ca1139.60 (19)
O11—Ca1—O1—C486.6 (2)Ca1—N1—C3—N2−165.8 (2)
O10—Ca1—O1—C4171.7 (2)C1—N1—C3—C6179.7 (3)
O9—Ca1—O1—C4−96.9 (2)Ca1—N1—C3—C612.4 (5)
O8—Ca1—O1—C4−149.2 (2)C2—N2—C3—N1−1.6 (3)
N1—Ca1—O1—C4−4.4 (2)C2—N2—C3—C6−179.9 (3)
N3—Ca1—O1—C433.0 (3)Ca1—O1—C4—O2−178.5 (2)
O11—Ca1—O8—C12−54.5 (2)Ca1—O1—C4—C11.6 (4)
O10—Ca1—O8—C12−130.7 (2)C2—C1—C4—O1−173.7 (3)
O9—Ca1—O8—C12138.0 (2)N1—C1—C4—O15.3 (4)
O1—Ca1—O8—C12−170.5 (2)C2—C1—C4—O26.3 (5)
N1—Ca1—O8—C1259.8 (3)N1—C1—C4—O2−174.7 (3)
N3—Ca1—O8—C128.2 (2)N2—C2—C5—O4−2.5 (4)
O11—Ca1—N1—C390.9 (3)C1—C2—C5—O4177.9 (3)
O10—Ca1—N1—C3166.0 (3)N2—C2—C5—O3176.2 (3)
O9—Ca1—N1—C3−108.8 (3)C1—C2—C5—O3−3.4 (5)
O1—Ca1—N1—C3173.1 (3)N1—C3—C6—C7−99.3 (4)
O8—Ca1—N1—C3−32.8 (4)N2—C3—C6—C778.7 (4)
N3—Ca1—N1—C313.2 (3)C3—C6—C7—C861.5 (3)
O11—Ca1—N1—C1−75.75 (19)C6—C7—C8—C963.7 (4)
O10—Ca1—N1—C1−0.7 (3)C10—N3—C9—N40.2 (3)
O9—Ca1—N1—C184.53 (19)Ca1—N3—C9—N4169.1 (2)
O1—Ca1—N1—C16.41 (18)C10—N3—C9—C8178.6 (3)
O8—Ca1—N1—C1160.45 (17)Ca1—N3—C9—C8−12.6 (5)
N3—Ca1—N1—C1−153.55 (19)C11—N4—C9—N3−0.4 (4)
O11—Ca1—N3—C9−51.1 (3)C11—N4—C9—C8−178.8 (3)
O10—Ca1—N3—C9−124.4 (3)C7—C8—C9—N3−89.7 (4)
O9—Ca1—N3—C9121.9 (3)C7—C8—C9—N488.5 (4)
O1—Ca1—N3—C93.7 (4)C9—N3—C10—C110.0 (3)
O8—Ca1—N3—C9−175.1 (3)Ca1—N3—C10—C11−172.1 (2)
N1—Ca1—N3—C937.9 (3)C9—N3—C10—C12178.3 (3)
O11—Ca1—N3—C10117.1 (2)Ca1—N3—C10—C126.3 (3)
O10—Ca1—N3—C1043.8 (2)C9—N4—C11—C100.4 (3)
O9—Ca1—N3—C10−69.9 (2)C9—N4—C11—C13178.7 (3)
O1—Ca1—N3—C10171.85 (18)N3—C10—C11—N4−0.3 (3)
O8—Ca1—N3—C10−6.88 (19)C12—C10—C11—N4−178.3 (3)
N1—Ca1—N3—C10−153.9 (2)N3—C10—C11—C13−178.3 (3)
C3—N1—C1—C2−0.8 (3)C12—C10—C11—C133.7 (6)
Ca1—N1—C1—C2170.56 (19)Ca1—O8—C12—O7171.1 (2)
C3—N1—C1—C4180.0 (3)Ca1—O8—C12—C10−8.2 (4)
Ca1—N1—C1—C4−8.6 (3)C11—C10—C12—O8178.6 (3)
C3—N2—C2—C11.0 (3)N3—C10—C12—O80.8 (4)
C3—N2—C2—C5−178.7 (3)C11—C10—C12—O7−0.6 (5)
N1—C1—C2—N2−0.1 (3)N3—C10—C12—O7−178.5 (3)
C4—C1—C2—N2179.0 (3)N4—C11—C13—O50.5 (5)
N1—C1—C2—C5179.5 (3)C10—C11—C13—O5178.2 (3)
C4—C1—C2—C5−1.4 (6)N4—C11—C13—O6−178.0 (3)
C1—N1—C3—N21.5 (3)C10—C11—C13—O6−0.3 (5)
D—H···AD—HH···AD···AD—H···A
N4—H4···O13i0.861.942.778 (4)164
O10—H3W···O5ii0.86 (1)2.03 (2)2.839 (3)159 (4)
O10—H4W···O1iii0.86 (1)1.91 (1)2.768 (3)174 (3)
O9—H2W···O5iv0.86 (1)1.93 (1)2.784 (3)172 (4)
O9—H1W···O12v0.86 (1)1.97 (1)2.829 (4)174 (5)
O14—H11W···O12vi0.86 (1)2.17 (2)2.957 (4)152 (4)
O15—H13W···O2vi0.86 (1)1.93 (2)2.752 (3)159 (4)
O15—H14W···O8vii0.86 (1)1.97 (1)2.824 (3)179 (4)
O13—H9W···O15vi0.86 (1)2.13 (2)2.943 (4)158 (4)
O13—H10W···O14viii0.86 (1)2.00 (1)2.851 (4)173 (5)
O11—H6W···O6ii0.86 (1)1.94 (2)2.770 (3)161 (4)
O11—H5W···O4vi0.86 (1)1.90 (2)2.717 (3)160 (4)
O12—H7W···O9iii0.86 (1)2.03 (2)2.851 (3)160 (5)
N2—H2···O140.861.962.809 (3)169
O14—H12W···O150.86 (1)1.88 (1)2.740 (4)177 (5)
O6—H6···O70.821.642.462 (3)175
O3—H3···O20.821.672.487 (3)176
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
N4—H4⋯O13i 0.861.942.778 (4)164
O10—H3W⋯O5ii 0.86 (1)2.03 (2)2.839 (3)159 (4)
O10—H4W⋯O1iii 0.86 (1)1.91 (1)2.768 (3)174 (3)
O9—H2W⋯O5iv 0.86 (1)1.93 (1)2.784 (3)172 (4)
O9—H1W⋯O12v 0.86 (1)1.97 (1)2.829 (4)174 (5)
O14—H11W⋯O12vi 0.86 (1)2.17 (2)2.957 (4)152 (4)
O15—H13W⋯O2vi 0.86 (1)1.93 (2)2.752 (3)159 (4)
O15—H14W⋯O8vii 0.86 (1)1.97 (1)2.824 (3)179 (4)
O13—H9W⋯O15vi 0.86 (1)2.13 (2)2.943 (4)158 (4)
O13—H10W⋯O14viii 0.86 (1)2.00 (1)2.851 (4)173 (5)
O11—H6W⋯O6ii 0.86 (1)1.94 (2)2.770 (3)161 (4)
O11—H5W⋯O4vi 0.86 (1)1.90 (2)2.717 (3)160 (4)
O12—H7W⋯O9iii 0.86 (1)2.03 (2)2.851 (3)160 (5)
N2—H2⋯O140.861.962.809 (3)169
O14—H12W⋯O150.86 (1)1.88 (1)2.740 (4)177 (5)
O6—H6⋯O70.821.642.462 (3)175
O3—H3⋯O20.821.672.487 (3)176

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) ; (vi) ; (vii) ; (viii) .

  3 in total

1.  Four novel frameworks built by imidazole-based dicarboxylate ligands: hydro(solvo)thermal synthesis, crystal structures, and properties.

Authors:  Fuwei Zhang; Zifeng Li; Tiezhu Ge; Hongchang Yao; Gang Li; Huijie Lu; Yanyan Zhu
Journal:  Inorg Chem       Date:  2010-04-19       Impact factor: 5.165

2.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

3.  Hierarchical assembly of extended coordination networks constructed by novel metallacalix[4]arenes building blocks.

Authors:  Xia Li; Benlai Wu; Ruiying Wang; Hongyun Zhang; Caoyuan Niu; Yunyin Niu; Hongwei Hou
Journal:  Inorg Chem       Date:  2010-03-15       Impact factor: 5.165
  3 in total

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