Literature DB >> 23284345

Poly[di-μ(3)-hy-droxy[μ(4)-5-(4-carb-oxy-phen-yl)pyridine-2-carboxyl-ato-κ(5)N,O(2):O(2'):O(4):O(4')]dicadmium].

Fan-Jin Meng1, Heng-Qing Jia, Ning-Hai Hu, Hua Zhou.   

Abstract

The asymmetric unit of the title polymeric complex, [Cd(2)(C(13)H(7)NO(4))(OH)(2)](n), consists of two independent Cd(II) atoms, one 5-(4-carb-oxy-phen-yl)pyridine-2-carboxyl-ate ligand and two hy-droxy groups. One Cd(II) atom is six-coordinated by two O atoms from two ligand mol-ecules and by four μ(3)-OH groups in a distorted trigonal-prismatic geometry. The other is five-coordinated by one N and two O atoms from two ligands and by two μ(3)-OH groups, forming a distorted square-pyramidal geometry. The two independent Cd(II) atoms are connected by the ligand mol-ecules and the OH groups into a three-dimensional framework. O-H⋯O hydrogen bonds between the OH groups and the carboxyl-ate O atoms are observed.

Entities:  

Year:  2012        PMID： 23284345      PMCID： PMC3515118          DOI： 10.1107/S1600536812042444

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


Related literature

For related structures and applications of metal complexes with N-heterocyclic multicarboxyl­ate ligands, see: Li et al. (2008 ▶); Mahata & Natarajan (2005 ▶); Sun et al. (2001 ▶); Wang et al. (2009 ▶). For the synthesis of the ligand, see: Ben & Gordon (1951 ▶); Liu et al. (2005 ▶).

Experimental

Crystal data

[Cd2(C13H7NO4)(OH)2] M = 500.03 Monoclinic, a = 15.4316 (17) Å b = 3.8261 (4) Å c = 21.586 (2) Å β = 102.114 (2)° V = 1246.1 (2) Å3 Z = 4 Mo Kα radiation μ = 3.44 mm−1 T = 293 K 0.27 × 0.21 × 0.14 mm

Data collection

Bruker APEX CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.457, T max = 0.644 6277 measured reflections 2448 independent reflections 2109 reflections with I > 2σ(I) R int = 0.052

Refinement

R[F 2 > 2σ(F 2)] = 0.037 wR(F 2) = 0.087 S = 1.04 2448 reflections 205 parameters 2 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 1.82 e Å−3 Δρmin = −1.36 e Å−3 Data collection: SMART (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; 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. Click here for additional data file. Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812042444/is5190sup1.cif Click here for additional data file. Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812042444/is5190Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Cd2(C13H7NO4)(OH)2]F(000) = 952
Mr = 500.03Dx = 2.665 Mg m−3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 2448 reflections
a = 15.4316 (17) Åθ = 2.1–26.0°
b = 3.8261 (4) ŵ = 3.44 mm−1
c = 21.586 (2) ÅT = 293 K
β = 102.114 (2)°Block, colourless
V = 1246.1 (2) Å30.27 × 0.21 × 0.14 mm
Z = 4
Bruker APEX CCD diffractometer2448 independent reflections
Radiation source: fine-focus sealed tube2109 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.052
φ and ω scansθmax = 26.0°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −19→14
Tmin = 0.457, Tmax = 0.644k = −3→4
6277 measured reflectionsl = −26→26
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.037Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.087H atoms treated by a mixture of independent and constrained refinement
S = 1.04w = 1/[σ2(Fo2) + (0.0384P)2 + 3.8222P] where P = (Fo2 + 2Fc2)/3
2448 reflections(Δ/σ)max = 0.001
205 parametersΔρmax = 1.82 e Å−3
2 restraintsΔρmin = −1.36 e Å−3
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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
Cd10.54015 (3)0.60259 (12)0.317372 (18)0.02773 (14)
Cd20.63702 (3)1.00568 (11)0.464037 (18)0.02162 (14)
C10.6046 (4)1.0297 (15)0.6045 (3)0.0230 (12)
C20.6959 (3)0.8660 (15)0.6131 (3)0.0197 (11)
C30.7430 (3)0.7675 (16)0.6720 (3)0.0226 (12)
H30.71810.78370.70750.027*
C40.8292 (4)0.6427 (16)0.6769 (3)0.0251 (13)
H40.86290.58040.71630.030*
C50.8646 (3)0.6115 (14)0.6239 (3)0.0185 (11)
C60.8105 (3)0.7034 (16)0.5659 (3)0.0231 (12)
H60.83270.67580.52930.028*
C70.9584 (3)0.5045 (14)0.6255 (3)0.0185 (11)
C81.0268 (3)0.6001 (15)0.6757 (2)0.0216 (12)
H81.01390.71860.71030.026*
C91.1138 (3)0.5190 (15)0.6742 (3)0.0216 (12)
H91.15890.58830.70760.026*
C101.1350 (3)0.3358 (15)0.6238 (3)0.0216 (12)
C111.2310 (4)0.2519 (16)0.6218 (3)0.0241 (12)
C121.0658 (3)0.2371 (15)0.5748 (2)0.0224 (12)
H121.07820.10980.54100.027*
C130.9795 (4)0.3229 (16)0.5751 (3)0.0238 (13)
H130.93470.25830.54120.029*
N10.7283 (3)0.8293 (13)0.5604 (2)0.0224 (10)
O10.5713 (3)1.1503 (12)0.55044 (18)0.0330 (10)
O20.5712 (3)1.0362 (13)0.6518 (2)0.0408 (12)
O31.2893 (3)0.3539 (12)0.66625 (19)0.0342 (10)
O41.2417 (3)0.0784 (12)0.57409 (19)0.0324 (10)
O50.5786 (2)0.5013 (10)0.42462 (18)0.0197 (8)
H5A0.5284 (17)0.528 (16)0.430 (3)0.030*
O60.5682 (2)1.1069 (11)0.27639 (19)0.0238 (8)
H6A0.6206 (13)1.093 (18)0.275 (3)0.036*
U11U22U33U12U13U23
Cd10.0398 (3)0.0251 (3)0.0162 (2)0.00757 (19)0.00127 (18)−0.00045 (18)
Cd20.0247 (2)0.0217 (2)0.0182 (2)0.00551 (16)0.00379 (16)−0.00076 (16)
C10.020 (3)0.025 (3)0.025 (3)0.006 (2)0.006 (2)−0.001 (2)
C20.017 (3)0.021 (3)0.023 (3)−0.001 (2)0.008 (2)−0.002 (2)
C30.021 (3)0.031 (3)0.018 (3)0.003 (2)0.009 (2)0.003 (2)
C40.025 (3)0.029 (3)0.020 (3)0.005 (2)0.002 (2)0.000 (3)
C50.016 (3)0.016 (3)0.024 (3)−0.001 (2)0.005 (2)0.000 (2)
C60.019 (3)0.033 (3)0.018 (3)0.004 (2)0.005 (2)0.000 (3)
C70.014 (2)0.022 (3)0.021 (3)−0.001 (2)0.007 (2)0.000 (2)
C80.022 (3)0.030 (3)0.015 (2)0.001 (2)0.007 (2)0.000 (2)
C90.018 (3)0.027 (3)0.019 (3)0.003 (2)0.001 (2)0.004 (2)
C100.020 (3)0.021 (3)0.026 (3)0.001 (2)0.010 (2)0.007 (2)
C110.023 (3)0.027 (3)0.024 (3)0.003 (2)0.008 (2)0.008 (3)
C120.023 (3)0.029 (3)0.018 (3)0.001 (2)0.008 (2)−0.006 (3)
C130.020 (3)0.028 (3)0.022 (3)−0.001 (2)−0.001 (2)0.001 (2)
N10.018 (2)0.028 (3)0.022 (2)0.0040 (19)0.0048 (19)−0.002 (2)
O10.027 (2)0.053 (3)0.020 (2)0.022 (2)0.0073 (17)0.008 (2)
O20.035 (2)0.064 (3)0.027 (2)0.025 (2)0.015 (2)0.010 (2)
O30.022 (2)0.049 (3)0.031 (2)0.006 (2)0.0018 (18)−0.003 (2)
O40.028 (2)0.046 (3)0.026 (2)0.006 (2)0.0105 (18)−0.004 (2)
O50.0139 (17)0.025 (2)0.0215 (19)0.0029 (15)0.0058 (15)0.0022 (16)
O60.0217 (19)0.023 (2)0.028 (2)0.0027 (17)0.0088 (17)−0.0046 (18)
Cd1—O6i2.174 (4)C6—H60.9300
Cd1—O62.203 (4)C7—C131.384 (8)
Cd1—O52.299 (4)C7—C81.393 (7)
Cd1—O6ii2.339 (4)C8—C91.385 (7)
Cd1—O2iii2.405 (4)C8—H80.9300
Cd1—O3iv2.586 (4)C9—C101.391 (8)
Cd2—O5v2.193 (4)C9—H90.9300
Cd2—O4iv2.221 (4)C10—C121.388 (7)
Cd2—O52.222 (4)C10—C111.525 (7)
Cd2—N12.354 (4)C11—O31.233 (7)
Cd2—O12.368 (4)C11—O41.264 (7)
C1—O21.237 (7)C12—C131.373 (7)
C1—O11.261 (7)C12—H120.9300
C1—C21.517 (7)C13—H130.9300
C2—N11.342 (7)O2—Cd1iii2.405 (4)
C2—C31.377 (7)O3—Cd1iv2.586 (4)
C3—C41.396 (7)O4—Cd2iv2.221 (4)
C3—H30.9300O5—Cd2i2.193 (4)
C4—C51.372 (8)O5—H5A0.814 (10)
C4—H40.9300O6—Cd1v2.174 (4)
C5—C61.396 (7)O6—Cd1vi2.339 (4)
C5—C71.498 (7)O6—H6A0.817 (10)
C6—N11.339 (7)
O6i—Cd1—O6121.88 (18)C5—C6—H6118.4
O6i—Cd1—O5103.38 (14)C13—C7—C8118.5 (5)
O6—Cd1—O5121.41 (14)C13—C7—C5120.3 (5)
O6i—Cd1—O6ii79.70 (13)C8—C7—C5121.1 (5)
O6—Cd1—O6ii79.12 (13)C9—C8—C7120.2 (5)
O5—Cd1—O6ii149.21 (13)C9—C8—H8119.9
O6i—Cd1—O2iii145.94 (16)C7—C8—H8119.9
O6—Cd1—O2iii79.60 (15)C8—C9—C10121.3 (5)
O5—Cd1—O2iii82.34 (13)C8—C9—H9119.4
O6ii—Cd1—O2iii79.22 (14)C10—C9—H9119.4
O6i—Cd1—O3iv80.11 (14)C12—C10—C9117.6 (5)
O6—Cd1—O3iv73.66 (14)C12—C10—C11121.2 (5)
O5—Cd1—O3iv80.39 (13)C9—C10—C11121.2 (5)
O6ii—Cd1—O3iv129.78 (13)O3—C11—O4127.0 (5)
O2iii—Cd1—O3iv133.69 (16)O3—C11—C10117.7 (5)
O5v—Cd2—O4iv106.95 (15)O4—C11—C10115.3 (5)
O5v—Cd2—O5120.10 (16)C13—C12—C10121.5 (5)
O4iv—Cd2—O592.19 (15)C13—C12—H12119.2
O5v—Cd2—N1135.39 (16)C10—C12—H12119.2
O4iv—Cd2—N183.77 (15)C12—C13—C7120.8 (5)
O5—Cd2—N1102.06 (15)C12—C13—H13119.6
O5v—Cd2—O183.94 (14)C7—C13—H13119.6
O4iv—Cd2—O1149.23 (14)C6—N1—C2118.5 (5)
O5—Cd2—O1107.35 (16)C6—N1—Cd2124.1 (4)
N1—Cd2—O169.28 (14)C2—N1—Cd2117.3 (3)
O2—C1—O1126.7 (5)C1—O1—Cd2119.1 (3)
O2—C1—C2116.5 (5)C1—O2—Cd1iii133.3 (4)
O1—C1—C2116.8 (5)C11—O3—Cd1iv133.0 (4)
N1—C2—C3122.3 (5)C11—O4—Cd2iv129.9 (4)
N1—C2—C1116.2 (5)Cd2i—O5—Cd2120.10 (16)
C3—C2—C1121.5 (5)Cd2i—O5—Cd1122.32 (17)
C2—C3—C4118.3 (5)Cd2—O5—Cd1103.73 (15)
C2—C3—H3120.9Cd2i—O5—H5A112 (5)
C4—C3—H3120.9Cd2—O5—H5A99 (5)
C5—C4—C3120.4 (5)Cd1—O5—H5A94 (4)
C5—C4—H4119.8Cd1v—O6—Cd1121.87 (18)
C3—C4—H4119.8Cd1v—O6—Cd1vi101.02 (15)
C4—C5—C6117.2 (5)Cd1—O6—Cd1vi100.16 (15)
C4—C5—C7123.8 (5)Cd1v—O6—H6A111 (5)
C6—C5—C7118.8 (5)Cd1—O6—H6A104 (5)
N1—C6—C5123.1 (5)Cd1vi—O6—H6A120 (5)
N1—C6—H6118.4
O2—C1—C2—N1173.9 (6)O1—Cd2—N1—C25.9 (4)
O1—C1—C2—N1−7.3 (8)O2—C1—O1—Cd2−168.3 (5)
O2—C1—C2—C3−7.3 (8)C2—C1—O1—Cd213.0 (7)
O1—C1—C2—C3171.5 (6)O5v—Cd2—O1—C1−154.0 (5)
N1—C2—C3—C43.5 (9)O4iv—Cd2—O1—C1−40.8 (6)
C1—C2—C3—C4−175.3 (5)O5—Cd2—O1—C186.3 (5)
C2—C3—C4—C5−1.7 (9)N1—Cd2—O1—C1−10.4 (4)
C3—C4—C5—C6−1.1 (9)O1—C1—O2—Cd1iii−22.3 (10)
C3—C4—C5—C7175.5 (5)C2—C1—O2—Cd1iii156.4 (4)
C4—C5—C6—N12.3 (9)O4—C11—O3—Cd1iv13.6 (10)
C7—C5—C6—N1−174.4 (5)C10—C11—O3—Cd1iv−167.4 (4)
C4—C5—C7—C13149.3 (6)O3—C11—O4—Cd2iv−17.1 (9)
C6—C5—C7—C13−34.2 (8)C10—C11—O4—Cd2iv163.9 (4)
C4—C5—C7—C8−34.0 (8)O5v—Cd2—O5—Cd2i−179.992 (1)
C6—C5—C7—C8142.5 (6)O4iv—Cd2—O5—Cd2i69.0 (2)
C13—C7—C8—C91.1 (8)N1—Cd2—O5—Cd2i−15.1 (2)
C5—C7—C8—C9−175.6 (5)O1—Cd2—O5—Cd2i−86.94 (19)
C7—C8—C9—C10−1.3 (9)O5v—Cd2—O5—Cd139.0 (3)
C8—C9—C10—C120.0 (8)O4iv—Cd2—O5—Cd1−72.10 (16)
C8—C9—C10—C11179.0 (5)N1—Cd2—O5—Cd1−156.20 (15)
C12—C10—C11—O3178.5 (6)O1—Cd2—O5—Cd1132.00 (14)
C9—C10—C11—O3−0.4 (8)O6i—Cd1—O5—Cd2i3.5 (2)
C12—C10—C11—O4−2.4 (8)O6—Cd1—O5—Cd2i−137.88 (18)
C9—C10—C11—O4178.7 (5)O6ii—Cd1—O5—Cd2i95.8 (3)
C9—C10—C12—C131.4 (9)O2iii—Cd1—O5—Cd2i149.3 (2)
C11—C10—C12—C13−177.6 (5)O3iv—Cd1—O5—Cd2i−73.8 (2)
C10—C12—C13—C7−1.6 (9)O6i—Cd1—O5—Cd2143.42 (15)
C8—C7—C13—C120.3 (9)O6—Cd1—O5—Cd22.1 (2)
C5—C7—C13—C12177.1 (5)O6ii—Cd1—O5—Cd2−124.3 (2)
C5—C6—N1—C2−0.7 (9)O2iii—Cd1—O5—Cd2−70.76 (17)
C5—C6—N1—Cd2177.7 (4)O3iv—Cd1—O5—Cd266.10 (15)
C3—C2—N1—C6−2.3 (9)O6i—Cd1—O6—Cd1v180.0
C1—C2—N1—C6176.5 (5)O5—Cd1—O6—Cd1v−45.7 (2)
C3—C2—N1—Cd2179.2 (4)O6ii—Cd1—O6—Cd1v109.5 (2)
C1—C2—N1—Cd2−2.0 (6)O2iii—Cd1—O6—Cd1v28.6 (2)
O5v—Cd2—N1—C6−115.5 (5)O3iv—Cd1—O6—Cd1v−113.2 (2)
O4iv—Cd2—N1—C6−7.7 (5)O6i—Cd1—O6—Cd1vi70.1 (2)
O5—Cd2—N1—C683.3 (5)O5—Cd1—O6—Cd1vi−155.55 (12)
O1—Cd2—N1—C6−172.6 (5)O6ii—Cd1—O6—Cd1vi−0.37 (9)
O5v—Cd2—N1—C262.9 (5)O2iii—Cd1—O6—Cd1vi−81.26 (15)
O4iv—Cd2—N1—C2170.8 (4)O3iv—Cd1—O6—Cd1vi136.96 (17)
O5—Cd2—N1—C2−98.3 (4)
D—H···AD—HH···AD···AD—H···A
O5—H5A···O1iii0.81 (3)2.08 (4)2.818 (6)150 (6)
O6—H6A···O3iv0.82 (2)2.39 (4)2.887 (6)120 (6)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O5—H5A⋯O1i 0.81 (3)2.08 (4)2.818 (6)150 (6)
O6—H6A⋯O3ii 0.82 (2)2.39 (4)2.887 (6)120 (6)

Symmetry codes: (i) ; (ii) .

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