metal-organic compounds
Poly[aqua-μ-bromido-(μ2-5-methylpyrazine-2-carboxylato-κ4N1,O2:O2,O2′)lead(II)]
aTianjin Key Laboratory of Structure and Performance of Functional Molecules, Tianjin Normal University, Tianjin 300071, People's Republic of China
*Correspondence e-mail: qsdingbin@yahoo.com.cn
In the title coordination polymer, [PbBr(C6H5N2O2)(H2O)]n, the PbII atom is coordinated by one pyrazine N atom, two bridging Br atoms, a water molecule and three carboxylate O atoms. Bridging by the two anions generates a layer structure parallel to (001); the layers are linked by O—H⋯N and O—H⋯Br hydrogen bonds, forming a three-dimensional network. The lone pair is stereochemically active, resulting in a Ψ-dodecahedral coordination environment for PbII.
Experimental
Crystal data
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Refinement
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Data collection: APEX2 (Bruker, 2007); cell 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: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).
Supporting information
10.1107/S1600536812033776/ng5284sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: 10.1107/S1600536812033776/ng5284Isup2.hkl
Lead(II) bromide (73.4 mg, 0.2 mmol), 5-pyrazine-2-carboxylic acid (27.6 mg, 0.2 mmol) and water (15 ml) were sealed in a 25 ml Teflon-lined steel vessel. The mixture was heated heated to 393 K for 5 days . The autoclave was cooled to room temperature at a rate of 10 K h-1. Yellow block-shaped crystals were obtained in 60% yield based on Pb.
H atoms were placed in calculated positions as riding atoms attached to non-riding atoms with O—H es of 0.85 Å and C–H 0.93 to 0.96 Å, and with Uiso(H) = 1.2 to 1.5Ueq(O,C). The final difference Fourier map had a peak in the vicinity of Pb and a hole in the vicinty of the same atom.
Data collection: APEX2 (Bruker, 2007); cell
SAINT (Bruker, 2007); data reduction: SAINT (Bruker, 2007); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).[PbBr(C6H5N2O2)(H2O)] | F(000) = 792 |
Mr = 442.24 | Dx = 3.018 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 3510 reflections |
a = 7.5493 (10) Å | θ = 3.3–28.2° |
b = 6.6775 (9) Å | µ = 21.41 mm−1 |
c = 19.335 (3) Å | T = 296 K |
β = 92.884 (2)° | Block, colourless |
V = 973.5 (2) Å3 | 0.15 × 0.14 × 0.13 mm |
Z = 4 |
Bruker SMART APEX CCD area-detector diffractometer | 1904 independent reflections |
Radiation source: fine-focus sealed tube | 1747 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.039 |
phi and ω scans | θmax = 26.0°, θmin = 3.2° |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | h = −9→5 |
Tmin = 0.142, Tmax = 0.167 | k = −8→8 |
5123 measured reflections | l = −23→22 |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.033 | w = 1/[σ2(Fo2) + (0.0596P)2] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.091 | (Δ/σ)max = 0.032 |
S = 1.05 | Δρmax = 2.26 e Å−3 |
1904 reflections | Δρmin = −2.20 e Å−3 |
120 parameters |
[PbBr(C6H5N2O2)(H2O)] | V = 973.5 (2) Å3 |
Mr = 442.24 | Z = 4 |
Monoclinic, P21/c | Mo Kα radiation |
a = 7.5493 (10) Å | µ = 21.41 mm−1 |
b = 6.6775 (9) Å | T = 296 K |
c = 19.335 (3) Å | 0.15 × 0.14 × 0.13 mm |
β = 92.884 (2)° |
Bruker SMART APEX CCD area-detector diffractometer | 1904 independent reflections |
Absorption correction: multi-scan (SADABS; Sheldrick, 1996) | 1747 reflections with I > 2σ(I) |
Tmin = 0.142, Tmax = 0.167 | Rint = 0.039 |
5123 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | 0 restraints |
wR(F2) = 0.091 | H-atom parameters constrained |
S = 1.05 | Δρmax = 2.26 e Å−3 |
1904 reflections | Δρmin = −2.20 e Å−3 |
120 parameters |
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. |
x | y | z | Uiso*/Ueq | ||
Pb1 | 0.29327 (3) | −0.20899 (3) | 0.782606 (12) | 0.02328 (17) | |
Br1 | 0.00888 (10) | 0.08548 (11) | 0.80760 (4) | 0.0386 (2) | |
O1 | 0.5113 (7) | 0.0867 (8) | 0.7933 (3) | 0.0351 (12) | |
O2 | 0.4664 (8) | −0.0254 (8) | 0.8984 (3) | 0.0427 (13) | |
O3 | 0.2211 (10) | −0.5006 (9) | 0.8682 (3) | 0.067 (2) | |
H3A | 0.2481 | −0.4963 | 0.9114 | 0.100* | |
H3B | 0.1828 | −0.6189 | 0.8608 | 0.100* | |
N1 | 0.6818 (7) | 0.4165 (8) | 0.8455 (3) | 0.0274 (12) | |
N2 | 0.7181 (8) | 0.4728 (9) | 0.9872 (3) | 0.0322 (13) | |
C1 | 0.6189 (9) | 0.2822 (9) | 0.8890 (4) | 0.0245 (15) | |
C2 | 0.6373 (10) | 0.3105 (10) | 0.9598 (4) | 0.0302 (16) | |
H2 | 0.5925 | 0.2146 | 0.9891 | 0.036* | |
C3 | 0.7783 (9) | 0.6113 (9) | 0.9431 (4) | 0.0298 (15) | |
C4 | 0.7588 (9) | 0.5805 (9) | 0.8721 (4) | 0.0285 (15) | |
H4 | 0.8006 | 0.6771 | 0.8423 | 0.034* | |
C5 | 0.5250 (9) | 0.0994 (10) | 0.8587 (4) | 0.0280 (15) | |
C6 | 0.8627 (14) | 0.7958 (11) | 0.9749 (6) | 0.049 (2) | |
H6A | 0.7859 | 0.8517 | 1.0079 | 0.073* | |
H6B | 0.8818 | 0.8924 | 0.9392 | 0.073* | |
H6C | 0.9743 | 0.7609 | 0.9977 | 0.073* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Pb1 | 0.0230 (2) | 0.0234 (2) | 0.0233 (2) | −0.00092 (7) | 0.00028 (12) | 0.00041 (8) |
Br1 | 0.0362 (4) | 0.0338 (4) | 0.0451 (5) | 0.0095 (3) | −0.0054 (3) | 0.0001 (3) |
O1 | 0.036 (3) | 0.042 (3) | 0.027 (3) | −0.017 (2) | −0.005 (2) | −0.004 (2) |
O2 | 0.056 (4) | 0.038 (3) | 0.034 (3) | −0.015 (2) | −0.002 (2) | 0.009 (2) |
O3 | 0.119 (7) | 0.049 (4) | 0.031 (3) | −0.039 (4) | −0.019 (3) | 0.008 (3) |
N1 | 0.028 (3) | 0.026 (3) | 0.028 (3) | −0.001 (2) | −0.001 (2) | −0.002 (2) |
N2 | 0.040 (4) | 0.030 (3) | 0.026 (3) | −0.004 (2) | −0.001 (2) | −0.005 (2) |
C1 | 0.021 (3) | 0.026 (4) | 0.027 (4) | 0.000 (2) | −0.002 (3) | 0.000 (3) |
C2 | 0.031 (4) | 0.031 (4) | 0.029 (4) | −0.001 (3) | 0.003 (3) | 0.001 (3) |
C3 | 0.030 (4) | 0.024 (3) | 0.035 (4) | 0.000 (3) | −0.003 (3) | −0.003 (3) |
C4 | 0.031 (4) | 0.023 (3) | 0.031 (4) | −0.002 (3) | 0.001 (3) | −0.001 (3) |
C5 | 0.025 (3) | 0.030 (3) | 0.029 (4) | −0.006 (3) | 0.003 (3) | −0.003 (3) |
C6 | 0.059 (6) | 0.033 (5) | 0.055 (6) | −0.011 (3) | 0.004 (5) | −0.008 (4) |
Pb1—O1i | 2.531 (5) | N1—C1 | 1.334 (8) |
Pb1—O1 | 2.572 (5) | N1—Pb1iv | 2.631 (5) |
Pb1—N1i | 2.631 (6) | N2—C2 | 1.340 (9) |
Pb1—O3 | 2.631 (6) | N2—C3 | 1.353 (9) |
Pb1—Br1 | 2.9688 (8) | C1—C2 | 1.381 (11) |
Pb1—Br1ii | 3.1190 (9) | C1—C5 | 1.514 (9) |
Br1—Pb1iii | 3.1190 (9) | C2—H2 | 0.9300 |
O1—C5 | 1.268 (8) | C3—C4 | 1.388 (10) |
O1—Pb1iv | 2.531 (5) | C3—C6 | 1.504 (10) |
O2—C5 | 1.230 (8) | C4—H4 | 0.9300 |
O3—H3A | 0.8501 | C6—H6A | 0.9600 |
O3—H3B | 0.8510 | C6—H6B | 0.9600 |
N1—C4 | 1.331 (9) | C6—H6C | 0.9600 |
O1i—Pb1—O1 | 94.06 (8) | C1—N1—Pb1iv | 115.1 (4) |
O1i—Pb1—N1i | 63.56 (16) | C2—N2—C3 | 117.6 (6) |
O1—Pb1—N1i | 75.81 (17) | N1—C1—C2 | 120.8 (6) |
O1i—Pb1—O3 | 96.4 (2) | N1—C1—C5 | 118.2 (6) |
O1—Pb1—O3 | 132.06 (18) | C2—C1—C5 | 121.0 (6) |
N1i—Pb1—O3 | 148.79 (18) | N2—C2—C1 | 121.6 (6) |
O1i—Pb1—Br1 | 153.98 (12) | N2—C2—H2 | 119.2 |
O1—Pb1—Br1 | 86.76 (12) | C1—C2—H2 | 119.2 |
N1i—Pb1—Br1 | 91.65 (12) | N2—C3—C4 | 120.0 (6) |
O3—Pb1—Br1 | 102.33 (18) | N2—C3—C6 | 116.8 (7) |
O1i—Pb1—Br1ii | 82.54 (13) | C4—C3—C6 | 123.2 (7) |
O1—Pb1—Br1ii | 146.05 (12) | N1—C4—C3 | 121.8 (6) |
N1i—Pb1—Br1ii | 72.46 (13) | N1—C4—H4 | 119.1 |
O3—Pb1—Br1ii | 81.80 (15) | C3—C4—H4 | 119.1 |
Br1—Pb1—Br1ii | 82.410 (17) | O2—C5—O1 | 124.3 (6) |
Pb1—Br1—Pb1iii | 135.64 (3) | O2—C5—C1 | 118.7 (6) |
C5—O1—Pb1iv | 121.4 (4) | O1—C5—C1 | 117.0 (5) |
C5—O1—Pb1 | 98.7 (4) | C3—C6—H6A | 109.5 |
Pb1iv—O1—Pb1 | 139.2 (2) | C3—C6—H6B | 109.5 |
Pb1—O3—H3A | 123.1 | H6A—C6—H6B | 109.5 |
Pb1—O3—H3B | 131.3 | C3—C6—H6C | 109.5 |
H3A—O3—H3B | 105.1 | H6A—C6—H6C | 109.5 |
C4—N1—C1 | 118.2 (6) | H6B—C6—H6C | 109.5 |
C4—N1—Pb1iv | 125.1 (4) | ||
O1i—Pb1—Br1—Pb1iii | 13.5 (3) | Pb1iv—N1—C1—C5 | −15.9 (7) |
O1—Pb1—Br1—Pb1iii | 106.16 (12) | C3—N2—C2—C1 | 1.4 (10) |
N1i—Pb1—Br1—Pb1iii | 30.47 (13) | N1—C1—C2—N2 | 0.1 (11) |
O3—Pb1—Br1—Pb1iii | −121.43 (15) | C5—C1—C2—N2 | −179.1 (6) |
Br1ii—Pb1—Br1—Pb1iii | −41.59 (4) | C2—N2—C3—C4 | −1.4 (10) |
O1i—Pb1—O1—C5 | −126.3 (4) | C2—N2—C3—C6 | 177.8 (7) |
N1i—Pb1—O1—C5 | 172.3 (4) | C1—N1—C4—C3 | 1.6 (10) |
O3—Pb1—O1—C5 | −23.9 (5) | Pb1iv—N1—C4—C3 | −163.3 (5) |
Br1—Pb1—O1—C5 | 79.8 (4) | N2—C3—C4—N1 | −0.1 (10) |
Br1ii—Pb1—O1—C5 | 151.1 (3) | C6—C3—C4—N1 | −179.3 (7) |
O1i—Pb1—O1—Pb1iv | 43.5 (3) | Pb1iv—O1—C5—O2 | −162.2 (6) |
N1i—Pb1—O1—Pb1iv | −17.9 (3) | Pb1—O1—C5—O2 | 10.0 (8) |
O3—Pb1—O1—Pb1iv | 145.9 (4) | Pb1iv—O1—C5—C1 | 18.3 (8) |
Br1—Pb1—O1—Pb1iv | −110.4 (3) | Pb1—O1—C5—C1 | −169.5 (5) |
Br1ii—Pb1—O1—Pb1iv | −39.1 (5) | N1—C1—C5—O2 | −179.9 (6) |
C4—N1—C1—C2 | −1.5 (9) | C2—C1—C5—O2 | −0.7 (10) |
Pb1iv—N1—C1—C2 | 164.8 (5) | N1—C1—C5—O1 | −0.4 (9) |
C4—N1—C1—C5 | 177.7 (6) | C2—C1—C5—O1 | 178.8 (6) |
Symmetry codes: (i) −x+1, y−1/2, −z+3/2; (ii) −x, y−1/2, −z+3/2; (iii) −x, y+1/2, −z+3/2; (iv) −x+1, y+1/2, −z+3/2. |
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3A···N2v | 0.85 | 1.97 | 2.816 (9) | 173 |
O3—H3B···Br1vi | 0.85 | 2.56 | 3.378 (6) | 161 |
Symmetry codes: (v) −x+1, −y, −z+2; (vi) x, y−1, z. |
Experimental details
Crystal data | |
Chemical formula | [PbBr(C6H5N2O2)(H2O)] |
Mr | 442.24 |
Crystal system, space group | Monoclinic, P21/c |
Temperature (K) | 296 |
a, b, c (Å) | 7.5493 (10), 6.6775 (9), 19.335 (3) |
β (°) | 92.884 (2) |
V (Å3) | 973.5 (2) |
Z | 4 |
Radiation type | Mo Kα |
µ (mm−1) | 21.41 |
Crystal size (mm) | 0.15 × 0.14 × 0.13 |
Data collection | |
Diffractometer | Bruker SMART APEX CCD area-detector diffractometer |
Absorption correction | Multi-scan (SADABS; Sheldrick, 1996) |
Tmin, Tmax | 0.142, 0.167 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 5123, 1904, 1747 |
Rint | 0.039 |
(sin θ/λ)max (Å−1) | 0.617 |
Refinement | |
R[F2 > 2σ(F2)], wR(F2), S | 0.033, 0.091, 1.05 |
No. of reflections | 1904 |
No. of parameters | 120 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.26, −2.20 |
Computer programs: APEX2 (Bruker, 2007), SAINT (Bruker, 2007), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), DIAMOND (Brandenburg, 1999), publCIF (Westrip, 2010).
D—H···A | D—H | H···A | D···A | D—H···A |
O3—H3A···N2i | 0.85 | 1.97 | 2.816 (9) | 173.1 |
O3—H3B···Br1ii | 0.85 | 2.56 | 3.378 (6) | 161.3 |
Symmetry codes: (i) −x+1, −y, −z+2; (ii) x, y−1, z. |
Acknowledgements
This present work was supported by the Tianjin Educational Committee (20090504) and Tianjin Normal University (1E0402B).
References
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