Literature DB >> 23125619

Poly[[diaqua-(μ-4,4'-bipyridine N,N'-di-oxide-κ(2)O:O')(μ-terephthalato-κ(2)O(1):O(4))cobalt(II)] 4,4'-bipyridine N,N'-dioxide monosolvate].

Xin Ge1, Shu-Yan Song.   

Abstract

In the title compound, {[Co(C(8)H(4)O(4))(C(10)H(8)N(2)O(2))(H(2)O)(2)]·C(10)H(8)N(2)O(2)}(n), the Co(II) atom, lying on an inversion center, is hexa-coordinated in a distorted octa-hedral geometry defined by two O atoms from two terephthalate (tp) ligands, two O atoms from two 4,4'-bipyridine N,N'-dioxide (bpydo) ligands and two water mol-ecules. The coordinated tp and bpydo ligands and uncoordinated bpydo mol-ecule all have an inversion center. The Co(II) atoms are connected by the tp and bpydo ligands into a layer parallel to (111). In the crystal, O-H⋯O hydrogen bonds link the uncoordinated bpydo mol-ecules and the layers into a three-dimensional supra-molecular structure. Intra-layer O-H⋯O hydrogen bonds and π-π inter-actions [centroid-to-centroid distances = 3.6643 (13) and 3.8048 (13) Å] are also observed.

Entities:  

Year:  2012        PMID： 23125619      PMCID： PMC3470175          DOI： 10.1107/S1600536812040056

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


Related literature

For the design of supra­molecular structures containing metal ions and organic ligands, see: Liao et al. (2008 ▶); Wang et al. (2008 ▶). For a related structure, see: Su et al. (2009 ▶).

Experimental

Crystal data

[Co(C8H4O4)(C10H8N2O2)(H2O)2]·C10H8N2O2 M = 635.44 Triclinic, a = 7.3883 (10) Å b = 9.1788 (13) Å c = 9.8054 (13) Å α = 81.312 (2)° β = 82.200 (2)° γ = 79.301 (2)° V = 641.92 (15) Å3 Z = 1 Mo Kα radiation μ = 0.74 mm−1 T = 293 K 0.27 × 0.24 × 0.20 mm

Data collection

Bruker APEXII CCD diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2001 ▶) T min = 0.825, T max = 0.866 3574 measured reflections 2516 independent reflections 2340 reflections with I > 2σ(I) R int = 0.017

Refinement

R[F 2 > 2σ(F 2)] = 0.031 wR(F 2) = 0.081 S = 1.05 2516 reflections 202 parameters 2 restraints H atoms treated by a mixture of independent and constrained refinement Δρmax = 0.48 e Å−3 Δρmin = −0.33 e Å−3 Data collection: APEX2 (Bruker, 2007 ▶); cell refinement: SAINT (Bruker, 2007 ▶); data reduction: SAINT; program(s) used to solve structure: SHELXTL (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXTL; molecular graphics: XP in SHELXTL; software used to prepare material for publication: SHELXTL. Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536812040056/hy2589sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536812040056/hy2589Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[Co(C8H4O4)(C10H8N2O2)(H2O)2]·C10H8N2O2Z = 1
Mr = 635.44F(000) = 327
Triclinic, P1Dx = 1.644 Mg m−3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 7.3883 (10) ÅCell parameters from 2899 reflections
b = 9.1788 (13) Åθ = 2.3–26.1°
c = 9.8054 (13) ŵ = 0.74 mm−1
α = 81.312 (2)°T = 293 K
β = 82.200 (2)°Block, pink
γ = 79.301 (2)°0.27 × 0.24 × 0.20 mm
V = 641.92 (15) Å3
Bruker APEXII CCD diffractometer2516 independent reflections
Radiation source: fine-focus sealed tube2340 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.017
φ and ω scansθmax = 26.1°, θmin = 2.1°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −8→9
Tmin = 0.825, Tmax = 0.866k = −10→11
3574 measured reflectionsl = −8→12
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.031Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.081H atoms treated by a mixture of independent and constrained refinement
S = 1.05w = 1/[σ2(Fo2) + (0.0389P)2 + 0.3924P] where P = (Fo2 + 2Fc2)/3
2516 reflections(Δ/σ)max < 0.001
202 parametersΔρmax = 0.48 e Å−3
2 restraintsΔρmin = −0.33 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
Co10.50000.50000.50000.01630 (11)
C10.3852 (3)0.7380 (2)0.2083 (2)0.0221 (4)
H10.35280.64390.21420.027*
C20.4275 (3)0.8156 (2)0.08038 (19)0.0209 (4)
H20.42490.77270.00070.025*
C30.4745 (2)0.9580 (2)0.06822 (18)0.0186 (4)
C40.4684 (3)1.0181 (2)0.1918 (2)0.0233 (4)
H40.49251.11450.18870.028*
C50.4271 (3)0.9365 (2)0.3176 (2)0.0242 (4)
H50.42460.97810.39880.029*
C60.8804 (3)0.7935 (2)0.2615 (2)0.0270 (4)
H60.85340.69800.29090.032*
C70.9285 (3)0.8359 (2)0.1234 (2)0.0264 (4)
H70.93130.76890.06060.032*
C80.9735 (3)0.9770 (2)0.0743 (2)0.0217 (4)
C90.9655 (3)1.0700 (2)0.1762 (2)0.0317 (5)
H90.99581.16490.14960.038*
C100.9150 (3)1.0265 (2)0.3131 (2)0.0344 (5)
H100.91021.09200.37770.041*
C110.6942 (2)0.44694 (19)0.21107 (18)0.0164 (4)
C120.8539 (2)0.47312 (19)0.10187 (18)0.0162 (3)
C131.0328 (2)0.46045 (19)0.13839 (18)0.0175 (4)
H131.05490.43450.23080.021*
C141.1778 (2)0.4865 (2)0.03689 (18)0.0179 (4)
H141.29700.47700.06170.021*
N10.3901 (2)0.79675 (17)0.32562 (16)0.0206 (3)
N20.8716 (2)0.88841 (18)0.35576 (18)0.0254 (4)
O10.3567 (2)0.71908 (15)0.44822 (14)0.0266 (3)
O20.8186 (2)0.84874 (17)0.48725 (15)0.0350 (4)
O30.57776 (18)0.37620 (15)0.18300 (14)0.0232 (3)
O40.68909 (17)0.50355 (14)0.32145 (12)0.0194 (3)
O50.67652 (19)0.59404 (15)0.59885 (14)0.0225 (3)
H5A0.719 (3)0.6689 (19)0.555 (2)0.034*
H5B0.605 (3)0.626 (3)0.6676 (17)0.034*
U11U22U33U12U13U23
Co10.01820 (19)0.02037 (19)0.01144 (18)−0.00652 (13)0.00000 (13)−0.00296 (13)
C10.0249 (9)0.0193 (9)0.0237 (10)−0.0039 (7)−0.0069 (8)−0.0034 (7)
C20.0255 (9)0.0216 (9)0.0175 (9)−0.0037 (7)−0.0071 (7)−0.0046 (7)
C30.0171 (8)0.0206 (9)0.0179 (9)−0.0003 (7)−0.0048 (7)−0.0026 (7)
C40.0280 (10)0.0213 (9)0.0218 (10)−0.0048 (7)−0.0024 (8)−0.0057 (7)
C50.0301 (10)0.0250 (10)0.0188 (9)−0.0041 (8)−0.0018 (8)−0.0081 (8)
C60.0300 (10)0.0204 (9)0.0310 (11)−0.0082 (8)0.0042 (8)−0.0062 (8)
C70.0288 (10)0.0210 (9)0.0302 (11)−0.0063 (8)0.0028 (8)−0.0086 (8)
C80.0179 (9)0.0185 (9)0.0289 (11)−0.0020 (7)−0.0020 (7)−0.0048 (7)
C90.0451 (13)0.0205 (10)0.0318 (12)−0.0132 (9)−0.0024 (10)−0.0026 (8)
C100.0504 (14)0.0267 (11)0.0304 (12)−0.0155 (10)−0.0029 (10)−0.0080 (9)
C110.0182 (8)0.0164 (8)0.0137 (8)−0.0020 (6)−0.0012 (7)−0.0008 (7)
C120.0190 (8)0.0162 (8)0.0141 (9)−0.0044 (6)0.0011 (7)−0.0055 (7)
C130.0218 (9)0.0200 (8)0.0113 (8)−0.0042 (7)−0.0021 (7)−0.0028 (7)
C140.0166 (8)0.0217 (9)0.0167 (9)−0.0039 (7)−0.0026 (7)−0.0051 (7)
N10.0212 (8)0.0229 (8)0.0159 (8)−0.0011 (6)−0.0012 (6)−0.0009 (6)
N20.0265 (8)0.0251 (8)0.0252 (9)−0.0074 (7)0.0007 (7)−0.0043 (7)
O10.0343 (8)0.0249 (7)0.0168 (7)−0.0022 (6)0.0022 (6)0.0016 (5)
O20.0473 (9)0.0337 (8)0.0253 (8)−0.0170 (7)0.0073 (7)−0.0058 (6)
O30.0241 (7)0.0301 (7)0.0195 (7)−0.0133 (6)0.0022 (5)−0.0095 (5)
O40.0221 (6)0.0259 (7)0.0123 (6)−0.0093 (5)0.0018 (5)−0.0055 (5)
O50.0234 (7)0.0282 (7)0.0181 (7)−0.0109 (6)0.0008 (5)−0.0048 (6)
Co1—O4i2.0865 (12)C7—H70.9300
Co1—O42.0865 (12)C8—C91.398 (3)
Co1—O52.0975 (13)C8—C8iii1.475 (4)
Co1—O5i2.0976 (13)C9—C101.364 (3)
Co1—O1i2.1141 (13)C9—H90.9300
Co1—O12.1141 (13)C10—N21.356 (3)
C1—N11.350 (2)C10—H100.9300
C1—C21.373 (3)C11—O31.250 (2)
C1—H10.9300C11—O41.263 (2)
C2—C31.397 (3)C11—C121.510 (2)
C2—H20.9300C12—C14iv1.395 (2)
C3—C41.398 (3)C12—C131.396 (2)
C3—C3ii1.479 (4)C13—C141.389 (3)
C4—C51.371 (3)C13—H130.9300
C4—H40.9300C14—C12iv1.395 (2)
C5—N11.349 (3)C14—H140.9300
C5—H50.9300N1—O11.319 (2)
C6—N21.350 (3)N2—O21.312 (2)
C6—C71.368 (3)O5—H5A0.84 (2)
C6—H60.9300O5—H5B0.85 (2)
C7—C81.395 (3)
O4i—Co1—O4180.0C6—C7—H7119.1
O4i—Co1—O590.46 (5)C8—C7—H7119.1
O4—Co1—O589.54 (5)C7—C8—C9115.04 (18)
O4i—Co1—O5i89.54 (5)C7—C8—C8iii122.1 (2)
O4—Co1—O5i90.46 (5)C9—C8—C8iii122.9 (2)
O5—Co1—O5i180.00 (6)C10—C9—C8122.32 (19)
O4i—Co1—O1i95.05 (5)C10—C9—H9118.8
O4—Co1—O1i84.95 (5)C8—C9—H9118.8
O5—Co1—O1i92.31 (6)N2—C10—C9120.4 (2)
O5i—Co1—O1i87.69 (6)N2—C10—H10119.8
O4i—Co1—O184.95 (5)C9—C10—H10119.8
O4—Co1—O195.05 (5)O3—C11—O4126.25 (16)
O5—Co1—O187.69 (6)O3—C11—C12117.81 (15)
O5i—Co1—O192.31 (6)O4—C11—C12115.90 (15)
O1i—Co1—O1180.0C14iv—C12—C13119.39 (16)
N1—C1—C2120.77 (17)C14iv—C12—C11119.82 (15)
N1—C1—H1119.6C13—C12—C11120.77 (15)
C2—C1—H1119.6C14—C13—C12120.09 (16)
C1—C2—C3120.92 (17)C14—C13—H13120.0
C1—C2—H2119.5C12—C13—H13120.0
C3—C2—H2119.5C13—C14—C12iv120.52 (16)
C2—C3—C4116.56 (17)C13—C14—H14119.7
C2—C3—C3ii121.9 (2)C12iv—C14—H14119.7
C4—C3—C3ii121.5 (2)O1—N1—C5119.74 (16)
C5—C4—C3120.68 (18)O1—N1—C1120.43 (16)
C5—C4—H4119.7C5—N1—C1119.82 (16)
C3—C4—H4119.7O2—N2—C6120.49 (16)
N1—C5—C4121.11 (17)O2—N2—C10120.07 (17)
N1—C5—H5119.4C6—N2—C10119.44 (18)
C4—C5—H5119.4N1—O1—Co1121.82 (11)
N2—C6—C7120.93 (18)C11—O4—Co1130.60 (11)
N2—C6—H6119.5Co1—O5—H5A117.3 (17)
C7—C6—H6119.5Co1—O5—H5B102.4 (17)
C6—C7—C8121.82 (19)H5A—O5—H5B106 (2)
N1—C1—C2—C3−0.8 (3)C4—C5—N1—C1−3.0 (3)
C1—C2—C3—C4−2.5 (3)C2—C1—N1—O1−177.21 (16)
C1—C2—C3—C3ii178.3 (2)C2—C1—N1—C53.6 (3)
C2—C3—C4—C53.1 (3)C7—C6—N2—O2177.42 (19)
C3ii—C3—C4—C5−177.7 (2)C7—C6—N2—C10−1.4 (3)
C3—C4—C5—N1−0.5 (3)C9—C10—N2—O2−178.3 (2)
N2—C6—C7—C81.1 (3)C9—C10—N2—C60.5 (3)
C6—C7—C8—C90.0 (3)C5—N1—O1—Co1−128.29 (15)
C6—C7—C8—C8iii179.6 (2)C1—N1—O1—Co152.5 (2)
C7—C8—C9—C10−0.9 (3)O4i—Co1—O1—N1−171.81 (14)
C8iii—C8—C9—C10179.5 (2)O4—Co1—O1—N18.19 (14)
C8—C9—C10—N20.6 (4)O5—Co1—O1—N197.52 (14)
O3—C11—C12—C14iv42.0 (2)O5i—Co1—O1—N1−82.48 (14)
O4—C11—C12—C14iv−135.93 (17)O3—C11—O4—Co12.1 (3)
O3—C11—C12—C13−139.35 (17)C12—C11—O4—Co1179.77 (11)
O4—C11—C12—C1342.7 (2)O5—Co1—O4—C11170.87 (15)
C14iv—C12—C13—C14−0.6 (3)O5i—Co1—O4—C11−9.13 (15)
C11—C12—C13—C14−179.28 (16)O1i—Co1—O4—C1178.51 (15)
C12—C13—C14—C12iv0.6 (3)O1—Co1—O4—C11−101.49 (15)
C4—C5—N1—O1177.84 (17)
D—H···AD—HH···AD···AD—H···A
O5—H5A···O20.84 (2)1.92 (2)2.755 (2)170 (2)
O5—H5B···O3i0.85 (2)1.85 (2)2.660 (2)158 (3)
Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A D—HH⋯A D⋯A D—H⋯A
O5—H5A⋯O20.84 (2)1.92 (2)2.755 (2)170 (2)
O5—H5B⋯O3i 0.85 (2)1.85 (2)2.660 (2)158 (3)

Symmetry code: (i) .

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