Literature DB >> 21588863

catena-Poly[[(1,10-phenanthroline-κN,N')cadmium(II)]-μ-oxalato-κO,O:O,O].

Yao-Kang Lv1, Li-Hua Gan, Yong-Jie Cao, Biao-Feng Gao, Liu-Hua Chen.   

Abstract

In the title complex, [Cd(C(2)O(4))(C(12)H(8)N(2))](n), the Cd(II) atom has a distorted octa-hedral coordination, defined by four O atoms from two symmetry-related oxalate ligands and by two N atoms from a bidentate 1,10-phenanthroline ligand. Each oxalate ligand bridges two Cd(II) atoms, generating a zigzag chain structure propagating along [100]. The packing of the structure is consolidated by non-classical C-H⋯O hydrogen-bonding inter-actions.

Entities:  

Year:  2010        PMID： 21588863      PMCID： PMC3009255          DOI： 10.1107/S1600536810040341

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


Related literature

For general background to the rational design and synthesis of metal-organic polymers, see: Kondrashev et al. (1985 ▶); Orioli et al. (2002 ▶); Athar et al. (2008 ▶); Lv et al. (2010 ▶). Wu et al. (2003 ▶). For related structures, see: Cao et al. (2009 ▶); Jeanneau et al. (2001 ▶).

Experimental

Crystal data

[Cd(C2O4)(C12H8N2)] M = 380.62 Orthorhombic, a = 9.7199 (2) Å b = 10.3338 (2) Å c = 13.1638 (2) Å V = 1322.22 (4) Å3 Z = 4 Mo Kα radiation μ = 1.67 mm−1 T = 296 K 0.29 × 0.14 × 0.10 mm

Data collection

Bruker APEXII area-detector diffractometer Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ▶) T min = 0.76, T max = 0.85 11056 measured reflections 2892 independent reflections 2386 reflections with I > 2σ(I) R int = 0.034

Refinement

R[F 2 > 2σ(F 2)] = 0.027 wR(F 2) = 0.066 S = 1.00 2892 reflections 191 parameters 1 restraint H-atom parameters constrained Δρmax = 0.37 e Å−3 Δρmin = −0.27 e Å−3 Absolute structure: Flack (1983 ▶), 1310 Friedel pairs Flack parameter: 0.33 (4) Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: DIAMOND (Brandenburg & Putz, 2004 ▶); software used to prepare material for publication: SHELXTL (Sheldrick, 2008 ▶). Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536810040341/wm2410sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810040341/wm2410Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cd(C2O4)(C12H8N2)]F(000) = 744
Mr = 380.62Dx = 1.912 Mg m−3
Orthorhombic, Pna21Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2c -2nCell parameters from 2979 reflections
a = 9.7199 (2) Åθ = 2.5–27.4°
b = 10.3338 (2) ŵ = 1.67 mm−1
c = 13.1638 (2) ÅT = 296 K
V = 1322.22 (4) Å3Block, colourless
Z = 40.29 × 0.14 × 0.10 mm
Bruker APEXII area-detector diffractometer2892 independent reflections
Radiation source: fine-focus sealed tube2386 reflections with I > 2σ(I)
graphiteRint = 0.034
ω scansθmax = 27.4°, θmin = 2.5°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)h = −12→12
Tmin = 0.76, Tmax = 0.85k = −13→13
11056 measured reflectionsl = −17→17
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.027H-atom parameters constrained
wR(F2) = 0.066w = 1/[σ2(Fo2) + (0.0359P)2] where P = (Fo2 + 2Fc2)/3
S = 1.00(Δ/σ)max = 0.001
2892 reflectionsΔρmax = 0.37 e Å−3
191 parametersΔρmin = −0.27 e Å−3
1 restraintAbsolute structure: Flack (1983), 1310 Friedel pairs
Primary atom site location: structure-invariant direct methodsFlack parameter: 0.33 (4)
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
Cd10.38159 (2)−0.09300 (2)0.33607 (7)0.04611 (10)
O10.5669 (3)−0.1452 (3)0.2410 (2)0.0499 (7)
O20.5193 (3)−0.2166 (3)0.4361 (2)0.0579 (8)
O30.7580 (3)−0.2606 (3)0.2421 (2)0.0558 (8)
O40.6953 (3)−0.3510 (3)0.4301 (2)0.0475 (7)
N10.4604 (4)0.1011 (3)0.4063 (3)0.0488 (9)
N20.2834 (4)0.0751 (3)0.2463 (3)0.0480 (8)
C10.6195 (3)−0.2664 (4)0.3923 (4)0.0395 (11)
C20.6499 (5)−0.2203 (4)0.2815 (4)0.0413 (11)
C30.1925 (5)0.0621 (5)0.1726 (3)0.0591 (12)
H3A0.1661−0.02100.15390.071*
C40.1343 (5)0.1662 (7)0.1214 (4)0.0689 (15)
H4A0.06950.15320.07040.083*
C50.1737 (6)0.2856 (6)0.1474 (4)0.0677 (15)
H5A0.13750.35630.11280.081*
C60.2686 (4)0.3061 (4)0.2260 (4)0.0537 (11)
C70.3150 (6)0.4299 (5)0.2568 (5)0.0691 (14)
H7A0.28270.50280.22310.083*
C80.4037 (5)0.4444 (4)0.3329 (9)0.0735 (13)
H8A0.43150.52730.35120.088*
C90.4585 (5)0.3335 (4)0.3883 (4)0.0566 (11)
C100.5520 (6)0.3424 (6)0.4680 (4)0.0738 (15)
H10A0.58410.42310.48860.089*
C110.5964 (6)0.2351 (7)0.5155 (5)0.0736 (18)
H11A0.65840.24080.56910.088*
C120.5478 (6)0.1150 (5)0.4831 (4)0.0666 (14)
H12A0.57800.04120.51690.080*
C130.4163 (4)0.2091 (4)0.3576 (3)0.0436 (11)
C140.3214 (4)0.1959 (4)0.2760 (3)0.0424 (9)
U11U22U33U12U13U23
Cd10.04105 (14)0.04202 (14)0.05528 (16)0.00004 (11)−0.0025 (2)0.0066 (2)
O10.0474 (16)0.0561 (17)0.0462 (17)0.0046 (15)0.0020 (14)0.0163 (16)
O20.0529 (18)0.070 (2)0.0505 (17)0.0190 (16)0.0150 (16)0.0229 (17)
O30.0573 (19)0.0592 (17)0.0508 (17)0.0164 (15)0.0141 (15)0.0105 (15)
O40.0469 (15)0.0471 (15)0.0484 (16)0.0047 (13)0.0033 (13)0.0097 (14)
N10.0444 (19)0.056 (2)0.0457 (19)−0.0024 (16)−0.0074 (15)0.0050 (18)
N20.0466 (19)0.051 (2)0.0460 (19)0.0014 (15)−0.0064 (16)0.0079 (17)
C10.042 (3)0.038 (2)0.039 (2)−0.0019 (18)−0.0002 (18)0.001 (2)
C20.044 (2)0.032 (2)0.049 (3)−0.0045 (19)0.006 (2)0.006 (2)
C30.057 (3)0.069 (3)0.051 (3)−0.002 (2)−0.011 (2)0.006 (2)
C40.063 (3)0.089 (4)0.054 (3)0.001 (3)−0.013 (2)0.018 (3)
C50.061 (3)0.074 (4)0.068 (4)0.020 (3)0.002 (3)0.031 (3)
C60.047 (2)0.050 (2)0.064 (3)0.0105 (19)0.013 (2)0.015 (2)
C70.070 (3)0.049 (3)0.088 (4)0.013 (2)0.009 (3)0.010 (3)
C80.082 (3)0.0364 (19)0.102 (4)−0.0012 (19)0.031 (5)−0.002 (5)
C90.051 (3)0.049 (3)0.070 (3)−0.013 (2)0.013 (2)−0.010 (2)
C100.074 (4)0.074 (4)0.074 (4)−0.020 (3)0.012 (3)−0.015 (3)
C110.072 (4)0.100 (5)0.049 (3)−0.026 (3)−0.011 (3)−0.008 (3)
C120.066 (3)0.074 (3)0.060 (3)−0.014 (3)−0.018 (3)0.012 (3)
C130.0400 (18)0.045 (2)0.046 (3)−0.0005 (15)0.0091 (18)0.004 (2)
C140.043 (2)0.041 (2)0.043 (2)0.0026 (17)0.0074 (18)0.0054 (18)
Cd1—O12.258 (3)C4—C51.336 (9)
Cd1—O4i2.269 (3)C4—H4A0.9300
Cd1—O22.271 (3)C5—C61.402 (7)
Cd1—O3i2.294 (3)C5—H5A0.9300
Cd1—N22.307 (3)C6—C141.411 (5)
Cd1—N12.338 (3)C6—C71.416 (7)
O1—C21.240 (5)C7—C81.330 (11)
O2—C11.242 (5)C7—H7A0.9300
O3—C21.244 (5)C8—C91.459 (9)
O3—Cd1ii2.294 (3)C8—H8A0.9300
O4—C11.247 (5)C9—C101.392 (7)
O4—Cd1ii2.269 (3)C9—C131.409 (6)
N1—C121.329 (6)C10—C111.344 (9)
N1—C131.356 (5)C10—H10A0.9300
N2—C31.319 (6)C11—C121.394 (8)
N2—C141.359 (5)C11—H11A0.9300
C1—C21.563 (5)C12—H12A0.9300
C3—C41.391 (7)C13—C141.422 (6)
C3—H3A0.9300
O1—Cd1—O4i151.38 (10)C5—C4—C3118.3 (5)
O1—Cd1—O273.54 (9)C5—C4—H4A120.9
O4i—Cd1—O290.60 (10)C3—C4—H4A120.9
O1—Cd1—O3i87.77 (11)C4—C5—C6121.1 (5)
O4i—Cd1—O3i73.03 (10)C4—C5—H5A119.5
O2—Cd1—O3i104.50 (12)C6—C5—H5A119.5
O1—Cd1—N2103.06 (12)C5—C6—C14117.5 (4)
O4i—Cd1—N298.14 (12)C5—C6—C7123.9 (5)
O2—Cd1—N2164.61 (13)C14—C6—C7118.6 (5)
O3i—Cd1—N290.22 (13)C8—C7—C6121.6 (5)
O1—Cd1—N199.37 (13)C8—C7—H7A119.2
O4i—Cd1—N1105.35 (12)C6—C7—H7A119.2
O2—Cd1—N193.45 (13)C7—C8—C9121.7 (5)
O3i—Cd1—N1161.94 (12)C7—C8—H8A119.2
N2—Cd1—N172.07 (12)C9—C8—H8A119.2
C2—O1—Cd1115.5 (3)C10—C9—C13117.9 (5)
C1—O2—Cd1115.2 (3)C10—C9—C8124.3 (5)
C2—O3—Cd1ii116.0 (3)C13—C9—C8117.8 (5)
C1—O4—Cd1ii115.6 (3)C11—C10—C9120.4 (5)
C12—N1—C13118.3 (4)C11—C10—H10A119.8
C12—N1—Cd1127.1 (3)C9—C10—H10A119.8
C13—N1—Cd1114.5 (3)C10—C11—C12119.0 (5)
C3—N2—C14119.1 (4)C10—C11—H11A120.5
C3—N2—Cd1125.3 (3)C12—C11—H11A120.5
C14—N2—Cd1115.6 (3)N1—C12—C11123.0 (5)
O2—C1—O4124.6 (5)N1—C12—H12A118.5
O2—C1—C2117.1 (4)C11—C12—H12A118.5
O4—C1—C2118.3 (4)N1—C13—C9121.5 (4)
O1—C2—O3125.5 (5)N1—C13—C14118.9 (4)
O1—C2—C1117.9 (4)C9—C13—C14119.5 (4)
O3—C2—C1116.6 (4)N2—C14—C6120.5 (4)
N2—C3—C4123.4 (5)N2—C14—C13118.7 (3)
N2—C3—H3A118.3C6—C14—C13120.7 (4)
C4—C3—H3A118.3
O4i—Cd1—O1—C2−54.2 (5)O2—C1—C2—O3172.9 (5)
O2—Cd1—O1—C24.5 (3)O4—C1—C2—O3−8.0 (5)
O3i—Cd1—O1—C2−101.3 (4)C14—N2—C3—C41.2 (7)
N2—Cd1—O1—C2169.0 (3)Cd1—N2—C3—C4179.0 (4)
N1—Cd1—O1—C295.4 (3)N2—C3—C4—C50.9 (8)
O1—Cd1—O2—C1−7.7 (3)C3—C4—C5—C6−1.6 (8)
O4i—Cd1—O2—C1148.1 (3)C4—C5—C6—C140.4 (7)
O3i—Cd1—O2—C175.5 (3)C4—C5—C6—C7179.7 (5)
N2—Cd1—O2—C1−87.0 (6)C5—C6—C7—C8179.0 (6)
N1—Cd1—O2—C1−106.5 (3)C14—C6—C7—C8−1.8 (8)
O1—Cd1—N1—C12−78.2 (4)C6—C7—C8—C90.3 (10)
O4i—Cd1—N1—C1287.2 (4)C7—C8—C9—C10179.6 (6)
O2—Cd1—N1—C12−4.4 (4)C7—C8—C9—C131.1 (9)
O3i—Cd1—N1—C12169.5 (4)C13—C9—C10—C11−2.0 (7)
N2—Cd1—N1—C12−179.0 (4)C8—C9—C10—C11179.4 (6)
O1—Cd1—N1—C1397.6 (3)C9—C10—C11—C120.4 (9)
O4i—Cd1—N1—C13−96.9 (3)C13—N1—C12—C11−0.3 (8)
O2—Cd1—N1—C13171.5 (3)Cd1—N1—C12—C11175.5 (4)
O3i—Cd1—N1—C13−14.6 (6)C10—C11—C12—N10.8 (9)
N2—Cd1—N1—C13−3.2 (3)C12—N1—C13—C9−1.5 (6)
O1—Cd1—N2—C388.0 (4)Cd1—N1—C13—C9−177.7 (3)
O4i—Cd1—N2—C3−72.7 (4)C12—N1—C13—C14−179.2 (4)
O2—Cd1—N2—C3163.3 (4)Cd1—N1—C13—C144.5 (5)
O3i—Cd1—N2—C30.2 (4)C10—C9—C13—N12.6 (6)
N1—Cd1—N2—C3−176.3 (4)C8—C9—C13—N1−178.7 (5)
O1—Cd1—N2—C14−94.2 (3)C10—C9—C13—C14−179.6 (4)
O4i—Cd1—N2—C14105.1 (3)C8—C9—C13—C14−1.0 (6)
O2—Cd1—N2—C14−18.9 (6)C3—N2—C14—C6−2.5 (6)
O3i—Cd1—N2—C14178.0 (3)Cd1—N2—C14—C6179.5 (3)
N1—Cd1—N2—C141.6 (3)C3—N2—C14—C13178.1 (4)
Cd1—O2—C1—O4−169.5 (3)Cd1—N2—C14—C130.1 (5)
Cd1—O2—C1—C29.5 (4)C5—C6—C14—N21.7 (6)
Cd1ii—O4—C1—O2−174.2 (3)C7—C6—C14—N2−177.6 (4)
Cd1ii—O4—C1—C26.8 (4)C5—C6—C14—C13−178.9 (4)
Cd1—O1—C2—O3−179.9 (4)C7—C6—C14—C131.8 (6)
Cd1—O1—C2—C1−1.5 (5)N1—C13—C14—N2−3.2 (6)
Cd1ii—O3—C2—O1−176.9 (4)C9—C13—C14—N2179.0 (4)
Cd1ii—O3—C2—C14.6 (4)N1—C13—C14—C6177.4 (4)
O2—C1—C2—O1−5.6 (5)C9—C13—C14—C6−0.4 (6)
O4—C1—C2—O1173.4 (5)
D—H···AD—HH···AD···AD—H···A
C4—H4A···O2iii0.932.383.106 (6)134
C7—H7A···O1iv0.932.573.289 (6)134
C11—H11A···O3v0.932.423.302 (7)159
Table 1

Selected bond lengths (Å)

Cd1—O12.258 (3)
Cd1—O4i2.269 (3)
Cd1—O22.271 (3)
Cd1—O3i2.294 (3)
Cd1—N22.307 (3)
Cd1—N12.338 (3)

Symmetry code: (i) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯AD—HH⋯AD⋯AD—H⋯A
C4—H4A⋯O2ii0.932.383.106 (6)134
C7—H7A⋯O1iii0.932.573.289 (6)134
C11—H11A⋯O3iv0.932.423.302 (7)159

Symmetry codes: (ii) ; (iii) ; (iv) .

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