Literature DB >> 21581553

catena-Poly[[aqua-(1,10-phenanthroline)cadmium(II)]-μ-benzene-1,4-di-carboxyl-ato].

Hongping Hu1.   

Abstract

The title compound, [Cd(C(8)H(4)O(4))(C(12)H(8)N(2))(H(2)O)](n), is a new coordination polymer of benzene-1,4-dicarboxyl-ate with cadmium(II) and 1,10-phenanthroline. The Cd(II) ion is coordinated by two N atoms from the 1,10-phenanthroline mol-ecule, three O atoms from two crystallographically independent benzene-1,4-dicarboxyl-ate ligands and the O atom of a coordinated water mol-ecule, forming a heavily distorted octa-hedron. The 1,10-phenanthroline ligand is approximately planar within 0.073 (4) Å. The two different benzene-1,4-dicarboxyl-ate ligands each coordinate to two Cd(II) ions in bidentate and monodentate modes, forming an infinite zigzag chain. Adjacent chains are packed tightly by strong π-π inter-actions [centroid-centroid distances = 3.851 (2) and 3.859 (2) Å] between the aromatic rings of the benzene-1,4-dicarboxyl-ate ligand and the 1,10-phenanthroline of a neighboring chain, forming a sheet parallel to (011). Different sheets are linked together via O-H⋯O hydrogen bonds between the coordinated water mol-ecules and the O atoms of the carboxyl-ate groups, forming a three-dimensional network.

Entities:  

Year:  2008        PMID： 21581553      PMCID： PMC2967922          DOI： 10.1107/S1600536808041913

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


Related literature

For related literature, see: Go et al. (2004 ▶); Sun et al. (2001 ▶).

Experimental

Crystal data

[Cd(C8H4O4)(C12H8N2)(H2O)] M = 474.74 Triclinic, a = 9.1831 (5) Å b = 9.6550 (6) Å c = 11.3600 (7) Å α = 104.6310 (8)° β = 104.0390 (9)° γ = 101.8920 (7)° V = 906.28 (9) Å3 Z = 2 Mo Kα radiation μ = 1.24 mm−1 T = 298 (2) K 0.10 × 0.08 × 0.04 mm

Data collection

Bruker SMART CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.888, T max = 0.952 5387 measured reflections 3939 independent reflections 3428 reflections with I > 2σ(I) R int = 0.018

Refinement

R[F 2 > 2σ(F 2)] = 0.033 wR(F 2) = 0.081 S = 1.07 3939 reflections 261 parameters H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.44 e Å−3 Δρmin = −0.49 e Å−3 Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT-Plus (Bruker, 2007 ▶); data reduction: SAINT-Plus; 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 datablocks global, I. DOI: 10.1107/S1600536808041913/ez2152sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536808041913/ez2152Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cd(C8H4O4)(C12H8N2)(H2O)]Z = 2
Mr = 474.74F(000) = 472
Triclinic, P1Dx = 1.74 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 9.1831 (5) ÅCell parameters from 2096 reflections
b = 9.6550 (6) Åθ = 2.6–26.7°
c = 11.3600 (7) ŵ = 1.24 mm−1
α = 104.6310 (8)°T = 298 K
β = 104.0390 (9)°Plate, colourless
γ = 101.8920 (7)°0.10 × 0.08 × 0.04 mm
V = 906.28 (9) Å3
Bruker SMART CCD area-detector diffractometer3939 independent reflections
Radiation source: fine-focus sealed tube3428 reflections with I > 2σ(I)
graphiteRint = 0.018
φ and ω scansθmax = 27.5°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −8→11
Tmin = 0.888, Tmax = 0.952k = −11→12
5387 measured reflectionsl = −14→13
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.033Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H atoms treated by a mixture of independent and constrained refinement
S = 1.07w = 1/[σ2(Fo2) + (0.0384P)2 + 0.2384P] where P = (Fo2 + 2Fc2)/3
3939 reflections(Δ/σ)max < 0.001
261 parametersΔρmax = 0.44 e Å−3
0 restraintsΔρmin = −0.49 e Å−3
Experimental. all of H atoms on water molecules were located on intermediate difference Fourier map
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
Cd10.95793 (3)0.18405 (3)0.35302 (2)0.02519 (9)
O11.0863 (3)−0.0176 (3)0.3642 (3)0.0414 (6)
O21.2261 (3)0.2183 (3)0.4339 (3)0.0405 (6)
O30.9956 (3)0.2355 (3)0.1778 (2)0.0359 (6)
O41.0395 (3)0.4563 (3)0.3186 (2)0.0391 (6)
O50.9890 (4)0.2639 (4)0.5669 (3)0.0405 (7)
N10.7280 (3)0.2663 (3)0.3305 (3)0.0303 (6)
N20.7334 (3)−0.0205 (3)0.2344 (3)0.0325 (7)
C11.2161 (4)0.0827 (4)0.4162 (3)0.0309 (8)
C21.3631 (4)0.0395 (4)0.4593 (3)0.0301 (7)
C31.4937 (4)0.1431 (4)0.5520 (4)0.0380 (9)
H31.49030.23990.58710.046*
C41.3706 (4)−0.1043 (4)0.4069 (4)0.0374 (9)
H41.2838−0.17490.34390.045*
C51.0181 (4)0.3738 (4)0.2075 (3)0.0300 (7)
C61.0122 (4)0.4413 (4)0.1011 (3)0.0291 (7)
C71.0364 (5)0.3674 (4)−0.0097 (3)0.0373 (9)
H71.06090.2775−0.01700.045*
C80.9751 (5)0.5750 (4)0.1105 (4)0.0398 (9)
H80.95800.62620.18470.048*
C90.7232 (5)0.4041 (4)0.3839 (4)0.0401 (9)
H90.81580.47530.43790.048*
C100.5850 (5)0.4462 (5)0.3622 (4)0.0499 (11)
H100.58590.54310.40270.060*
C110.4501 (5)0.3451 (5)0.2821 (4)0.0499 (11)
H110.35790.37280.26630.060*
C120.4487 (4)0.1981 (4)0.2224 (4)0.0362 (8)
C130.3116 (4)0.0852 (5)0.1363 (4)0.0475 (10)
H130.21740.10880.11610.057*
C140.3154 (4)−0.0539 (5)0.0839 (4)0.0476 (10)
H140.2250−0.12470.02580.057*
C150.4574 (4)−0.0949 (4)0.1162 (4)0.0418 (9)
C160.4649 (5)−0.2426 (5)0.0711 (5)0.0592 (13)
H160.3758−0.31780.01620.071*
C170.6024 (6)−0.2744 (5)0.1081 (6)0.0740 (17)
H170.6083−0.37160.07950.089*
C180.7343 (5)−0.1603 (4)0.1893 (4)0.0507 (11)
H180.8282−0.18350.21310.061*
C190.5959 (4)0.0121 (4)0.1992 (3)0.0295 (7)
C200.5924 (4)0.1633 (4)0.2516 (3)0.0274 (7)
H5A0.958 (5)0.200 (4)0.596 (4)0.032 (11)*
H5B0.960 (5)0.327 (4)0.596 (4)0.035 (13)*
U11U22U33U12U13U23
Cd10.02248 (13)0.02768 (14)0.02752 (14)0.01040 (9)0.00638 (9)0.01107 (10)
O10.0258 (13)0.0428 (15)0.0577 (17)0.0128 (12)0.0060 (12)0.0240 (13)
O20.0316 (14)0.0378 (15)0.0560 (17)0.0191 (12)0.0097 (12)0.0180 (13)
O30.0457 (15)0.0339 (14)0.0333 (13)0.0135 (12)0.0120 (12)0.0178 (11)
O40.0536 (17)0.0383 (14)0.0279 (13)0.0153 (13)0.0120 (12)0.0136 (11)
O50.0595 (19)0.0346 (16)0.0337 (15)0.0177 (15)0.0206 (14)0.0124 (13)
N10.0245 (15)0.0288 (15)0.0336 (15)0.0099 (12)0.0050 (12)0.0054 (13)
N20.0275 (15)0.0264 (15)0.0388 (16)0.0091 (12)0.0055 (13)0.0058 (13)
C10.0243 (17)0.045 (2)0.0348 (18)0.0181 (16)0.0120 (15)0.0218 (16)
C20.0251 (17)0.0342 (19)0.0364 (19)0.0156 (15)0.0090 (15)0.0151 (15)
C30.0314 (19)0.0314 (19)0.049 (2)0.0189 (16)0.0052 (17)0.0081 (17)
C40.0283 (19)0.0334 (19)0.043 (2)0.0106 (16)0.0010 (16)0.0080 (16)
C50.0274 (17)0.0364 (19)0.0305 (18)0.0120 (15)0.0090 (14)0.0154 (15)
C60.0308 (18)0.0300 (18)0.0267 (17)0.0109 (15)0.0066 (14)0.0102 (14)
C70.056 (2)0.0310 (19)0.0315 (19)0.0223 (18)0.0147 (17)0.0124 (15)
C80.057 (3)0.041 (2)0.0315 (19)0.0259 (19)0.0199 (18)0.0137 (16)
C90.035 (2)0.0285 (19)0.050 (2)0.0104 (16)0.0091 (18)0.0039 (17)
C100.047 (2)0.034 (2)0.070 (3)0.0220 (19)0.019 (2)0.010 (2)
C110.035 (2)0.051 (3)0.069 (3)0.024 (2)0.015 (2)0.019 (2)
C120.0273 (18)0.040 (2)0.042 (2)0.0138 (16)0.0068 (16)0.0136 (17)
C130.0243 (19)0.059 (3)0.052 (2)0.0127 (19)0.0004 (18)0.017 (2)
C140.0206 (18)0.053 (3)0.049 (2)−0.0023 (17)−0.0048 (17)0.009 (2)
C150.032 (2)0.043 (2)0.041 (2)0.0043 (17)0.0055 (17)0.0069 (18)
C160.041 (2)0.040 (2)0.067 (3)−0.002 (2)−0.002 (2)−0.005 (2)
C170.058 (3)0.030 (2)0.101 (4)0.011 (2)−0.003 (3)−0.008 (2)
C180.039 (2)0.034 (2)0.067 (3)0.0129 (18)0.004 (2)0.005 (2)
C190.0256 (17)0.0290 (18)0.0283 (17)0.0054 (14)0.0030 (14)0.0071 (14)
C200.0234 (16)0.0320 (18)0.0273 (17)0.0091 (14)0.0065 (13)0.0104 (14)
Cd1—O32.256 (2)C6—C81.387 (5)
Cd1—O52.281 (3)C7—C8ii1.385 (5)
Cd1—O22.330 (2)C7—H70.9300
Cd1—N22.366 (3)C8—C7ii1.386 (5)
Cd1—N12.384 (3)C8—H80.9300
Cd1—O12.489 (2)C9—C101.396 (5)
O1—C11.265 (4)C9—H90.9300
O2—C11.253 (4)C10—C111.349 (6)
O3—C51.251 (4)C10—H100.9300
O4—C51.255 (4)C11—C121.406 (5)
O5—H5A0.81 (4)C11—H110.9300
O5—H5B0.75 (4)C12—C201.411 (5)
N1—C91.330 (4)C12—C131.424 (5)
N1—C201.357 (4)C13—C141.336 (6)
N2—C181.320 (5)C13—H130.9300
N2—C191.354 (4)C14—C151.430 (5)
C1—C21.501 (4)C14—H140.9300
C2—C31.382 (5)C15—C191.400 (5)
C2—C41.389 (5)C15—C161.410 (6)
C3—C4i1.382 (5)C16—C171.354 (6)
C3—H30.9300C16—H160.9300
C4—C3i1.382 (5)C17—C181.388 (6)
C4—H40.9300C17—H170.9300
C5—C61.507 (5)C18—H180.9300
C6—C71.374 (5)C19—C201.441 (5)
O3—Cd1—O5149.20 (11)C8—C6—C5120.8 (3)
O3—Cd1—O289.18 (9)C6—C7—C8ii121.0 (3)
O5—Cd1—O280.46 (10)C6—C7—H7119.5
O3—Cd1—N293.93 (10)C8ii—C7—H7119.5
O5—Cd1—N2113.58 (11)C7ii—C8—C6120.1 (3)
O2—Cd1—N2136.37 (9)C7ii—C8—H8119.9
O3—Cd1—N192.49 (10)C6—C8—H8119.9
O5—Cd1—N184.71 (10)N1—C9—C10122.7 (4)
O2—Cd1—N1153.45 (10)N1—C9—H9118.6
N2—Cd1—N169.96 (9)C10—C9—H9118.6
O3—Cd1—O1102.64 (9)C11—C10—C9119.5 (4)
O5—Cd1—O194.69 (10)C11—C10—H10120.3
O2—Cd1—O154.27 (9)C9—C10—H10120.3
N2—Cd1—O182.74 (9)C10—C11—C12120.2 (4)
N1—Cd1—O1149.65 (9)C10—C11—H11119.9
C1—O1—Cd188.0 (2)C12—C11—H11119.9
C1—O2—Cd195.7 (2)C11—C12—C20117.0 (3)
C5—O3—Cd1103.3 (2)C11—C12—C13123.6 (3)
Cd1—O5—H5A116 (3)C20—C12—C13119.4 (3)
Cd1—O5—H5B122 (3)C14—C13—C12121.4 (4)
H5A—O5—H5B104 (4)C14—C13—H13119.3
C9—N1—C20118.2 (3)C12—C13—H13119.3
C9—N1—Cd1125.8 (2)C13—C14—C15120.6 (4)
C20—N1—Cd1116.0 (2)C13—C14—H14119.7
C18—N2—C19117.8 (3)C15—C14—H14119.7
C18—N2—Cd1125.2 (3)C19—C15—C16116.9 (4)
C19—N2—Cd1116.6 (2)C19—C15—C14120.3 (4)
O2—C1—O1122.0 (3)C16—C15—C14122.8 (4)
O2—C1—C2118.5 (3)C17—C16—C15119.8 (4)
O1—C1—C2119.5 (3)C17—C16—H16120.1
C3—C2—C4118.9 (3)C15—C16—H16120.1
C3—C2—C1120.2 (3)C16—C17—C18119.2 (4)
C4—C2—C1120.9 (3)C16—C17—H17120.4
C2—C3—C4i120.7 (3)C18—C17—H17120.4
C2—C3—H3119.6N2—C18—C17123.4 (4)
C4i—C3—H3119.6N2—C18—H18118.3
C3i—C4—C2120.3 (3)C17—C18—H18118.3
C3i—C4—H4119.8N2—C19—C15122.9 (3)
C2—C4—H4119.8N2—C19—C20118.2 (3)
O3—C5—O4123.6 (3)C15—C19—C20118.9 (3)
O3—C5—C6117.0 (3)N1—C20—C12122.4 (3)
O4—C5—C6119.3 (3)N1—C20—C19118.2 (3)
C7—C6—C8118.9 (3)C12—C20—C19119.3 (3)
C7—C6—C5120.3 (3)
O3—Cd1—O1—C180.9 (2)Cd1—C1—C2—C3−7(3)
O5—Cd1—O1—C1−73.5 (2)O2—C1—C2—C4−158.3 (4)
O2—Cd1—O1—C11.20 (19)O1—C1—C2—C422.1 (5)
N2—Cd1—O1—C1173.3 (2)Cd1—C1—C2—C4173 (3)
N1—Cd1—O1—C1−161.0 (2)C4—C2—C3—C4i−0.6 (6)
O3—Cd1—O2—C1−107.5 (2)C1—C2—C3—C4i179.6 (3)
O5—Cd1—O2—C1101.7 (2)C3—C2—C4—C3i0.6 (6)
N2—Cd1—O2—C1−12.6 (3)C1—C2—C4—C3i−179.6 (3)
N1—Cd1—O2—C1158.6 (2)Cd1—O3—C5—O410.6 (4)
O1—Cd1—O2—C1−1.2 (2)Cd1—O3—C5—C6−166.9 (2)
O5—Cd1—O3—C5−20.9 (3)O3—C5—C6—C7−22.1 (5)
O2—Cd1—O3—C5−90.5 (2)O4—C5—C6—C7160.3 (3)
N2—Cd1—O3—C5133.0 (2)O3—C5—C6—C8154.9 (4)
N1—Cd1—O3—C562.9 (2)O4—C5—C6—C8−22.7 (5)
O1—Cd1—O3—C5−143.6 (2)C8—C6—C7—C8ii0.2 (7)
C1—Cd1—O3—C5−116.4 (2)C5—C6—C7—C8ii177.3 (4)
O3—Cd1—N1—C9−91.3 (3)C7—C6—C8—C7ii−0.2 (7)
O5—Cd1—N1—C957.9 (3)C5—C6—C8—C7ii−177.2 (3)
O2—Cd1—N1—C91.8 (4)C20—N1—C9—C100.2 (6)
N2—Cd1—N1—C9175.4 (3)Cd1—N1—C9—C10177.2 (3)
O1—Cd1—N1—C9148.2 (3)N1—C9—C10—C11−1.3 (7)
C1—Cd1—N1—C984.5 (7)C9—C10—C11—C120.9 (7)
O3—Cd1—N1—C2085.8 (2)C10—C11—C12—C200.6 (6)
O5—Cd1—N1—C20−125.0 (2)C10—C11—C12—C13−179.7 (4)
O2—Cd1—N1—C20178.9 (2)C11—C12—C13—C14−178.6 (4)
N2—Cd1—N1—C20−7.5 (2)C20—C12—C13—C141.0 (6)
O1—Cd1—N1—C20−34.7 (3)C12—C13—C14—C152.0 (7)
C1—Cd1—N1—C20−98.4 (6)C13—C14—C15—C19−2.7 (7)
O3—Cd1—N2—C1890.0 (3)C13—C14—C15—C16175.1 (5)
O5—Cd1—N2—C18−104.2 (3)C19—C15—C16—C17−0.4 (7)
O2—Cd1—N2—C18−2.9 (4)C14—C15—C16—C17−178.3 (5)
N1—Cd1—N2—C18−178.7 (4)C15—C16—C17—C18−0.6 (9)
O1—Cd1—N2—C18−12.2 (3)C19—N2—C18—C170.1 (7)
C1—Cd1—N2—C18−8.9 (4)Cd1—N2—C18—C17−172.5 (4)
O3—Cd1—N2—C19−82.7 (3)C16—C17—C18—N20.8 (9)
O5—Cd1—N2—C1983.1 (3)C18—N2—C19—C15−1.2 (6)
O2—Cd1—N2—C19−175.6 (2)Cd1—N2—C19—C15172.1 (3)
N1—Cd1—N2—C198.6 (2)C18—N2—C19—C20177.8 (4)
O1—Cd1—N2—C19175.1 (3)Cd1—N2—C19—C20−9.0 (4)
C1—Cd1—N2—C19178.4 (2)C16—C15—C19—N21.3 (6)
Cd1—O2—C1—O12.3 (4)C14—C15—C19—N2179.2 (4)
Cd1—O2—C1—C2−177.3 (3)C16—C15—C19—C20−177.6 (4)
Cd1—O1—C1—O2−2.1 (3)C14—C15—C19—C200.3 (6)
Cd1—O1—C1—C2177.5 (3)C9—N1—C20—C121.5 (5)
O3—Cd1—C1—O274.0 (2)Cd1—N1—C20—C12−175.9 (3)
O5—Cd1—C1—O2−75.3 (2)C9—N1—C20—C19−176.7 (3)
N2—Cd1—C1—O2170.8 (2)Cd1—N1—C20—C196.0 (4)
N1—Cd1—C1—O2−101.9 (6)C11—C12—C20—N1−1.9 (5)
O1—Cd1—C1—O2177.8 (3)C13—C12—C20—N1178.5 (3)
O3—Cd1—C1—O1−103.9 (2)C11—C12—C20—C19176.3 (3)
O5—Cd1—C1—O1106.8 (2)C13—C12—C20—C19−3.4 (5)
O2—Cd1—C1—O1−177.8 (3)N2—C19—C20—N11.9 (5)
N2—Cd1—C1—O1−7.1 (2)C15—C19—C20—N1−179.1 (3)
N1—Cd1—C1—O180.3 (6)N2—C19—C20—C12−176.3 (3)
O2—C1—C2—C321.6 (5)C15—C19—C20—C122.7 (5)
O1—C1—C2—C3−158.0 (4)
D—H···AD—HH···AD···AD—H···A
O5—H5A···O1iii0.81 (4)1.91 (4)2.697 (4)163 (4)
O5—H5B···O4iv0.75 (4)2.07 (4)2.782 (4)159 (4)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
O5—H5A⋯O1i0.81 (4)1.91 (4)2.697 (4)163 (4)
O5—H5B⋯O4ii0.75 (4)2.07 (4)2.782 (4)159 (4)

Symmetry codes: (i) ; (ii) .

  2 in total

1.  A short history of SHELX.

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

2.  A chain of changes: influence of noncovalent interactions on the one-dimensional structures of nickel(II) dicarboxylate coordination polymers with chelating aromatic amine ligands.

Authors:  YongBok Go; Xiqu Wang; Ekaterina V Anokhina; Allan J Jacobson
Journal:  Inorg Chem       Date:  2004-08-23       Impact factor: 5.165
  2 in total

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