metal-organic compounds\(\def\hfill{\hskip 5em}\def\hfil{\hskip 3em}\def\eqno#1{\hfil {#1}}\)

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890

catena-Poly[[(1,10-phenanthroline)lead(II)]bis­­(μ-5-chloro-2-hy­dr­oxy­benzoato)]

aDepartment of Physics–Chemistry, Henan Polytechnic University, Jiao Zuo, 454150, People's Republic of China, and bDepartment of Chemistry, Zhejiang Forestry University, Lin'an, 311300, People's Republic of China
*Correspondence e-mail: xcy78413@tom.com

(Received 27 May 2010; accepted 17 June 2010; online 21 July 2010)

In the title polymer, [Pb(C7H4ClO3)2(C12H8N2)]n, the Pb(II) ion displays a distorted pseudo-octa­hedral coordination geometry. The metal center is coordinated by six O atoms from four 5-chloro­salicylate ligands and two N atoms from a chelating phenanthroline ligand. The polymeric structure is built up from bridging carboxyl­ate O atoms, forming chains along [100]. The crystal structure is stabilized by ππ inter­actions between the 1,10-phenanthroline and 5-chloro­salicylate ligands, the shortest centroid–centroid separation between neighbouring aromatic rings being 3.652 (1) Å.

Related literature

For related non-polymeric complexes including 5-chloro­salicylate ligands, see: Wen & Ying (2007[Wen, D. & Ying, S. (2007). Acta Cryst. E63, m2407-m2408.]); Wen et al. (2008[Wen, D., Xie, J. & Jiang, X. (2008). Acta Cryst. E64, m851-m852.]).

[Scheme 1]

Experimental

Crystal data
  • [Pb(C7H4ClO3)2(C12H8N2)]

  • Mr = 730.51

  • Triclinic, [P \overline 1]

  • a = 8.9100 (1) Å

  • b = 11.2959 (1) Å

  • c = 13.5816 (1) Å

  • α = 75.508 (1)°

  • β = 86.302 (1)°

  • γ = 68.342 (1)°

  • V = 1229.43 (2) Å3

  • Z = 2

  • Mo Kα radiation

  • μ = 7.13 mm−1

  • T = 296 K

  • 0.28 × 0.25 × 0.24 mm

Data collection
  • Bruker APEXII CCD diffractometer

  • Absorption correction: multi-scan (SADABS; Bruker, 2001[Bruker (2001). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]) Tmin = 0.156, Tmax = 0.181

  • 21579 measured reflections

  • 5987 independent reflections

  • 5339 reflections with I > 2σ(I)

  • Rint = 0.029

Refinement
  • R[F2 > 2σ(F2)] = 0.025

  • wR(F2) = 0.064

  • S = 1.05

  • 5987 reflections

  • 334 parameters

  • H-atom parameters constrained

  • Δρmax = 1.18 e Å−3

  • Δρmin = −0.59 e Å−3

Data collection: APEX2 (Bruker, 2001[Bruker (2001). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); cell refinement: SAINT (Bruker, 2001[Bruker (2001). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.]); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); molecular graphics: SHELXTL (Sheldrick, 2008[Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.]); software used to prepare material for publication: SHELXTL.

Supporting information


Comment top

The Pb(II) ion in the asymmetric unit is pseudo-octahedrally coordinated (Fig. 1), with coordination to six O atoms from four 5-chlorosalicylate ligands, and two N atoms from a chelating phenanthroline (phen) ligand. Two related complexes, [Zn(C7H4ClO3)2(C12H8N2)(H2O)] and [Cd(C7H4ClO3)2(C12H8N2)2], were reported (Wen & Ying, 2007; Wen et al., 2008, respectively), both with 5-chlorosalicylate ions acting as monodentate ligands, while in the title polymer, 5-chlorosalicylate ions are bidentate ligands.

The Pb—O distances (Table 1) vary from 2.458 (3) to 2.887 (3) Å, which are close to those found in Pb2(PMIDA).1.5H2O [from 2.331 (9) to 2.876 (9) Å; H4PMIDA is N-(phosphonomethyl)iminodiacetic acid]. Each pair of adjacent Pb(II) ions is bridged by the O1 atom of 5-chlorosalicylate, which forms a SBU (secondary building units, Fig. 2) including two Pb polyhedron, six 5-chlorosalicylate and two phen. The Pb···Pb distance in the dimeric unit is 4.3587 (2) Å. The SBU is bridged by O5 atom of 5-chlorosalicylate, to give rise to a zigzag chain (Fig. 3). The excellent coordinating ability and large conjugated systems of phen and 5-chlorosalicylate allow to form π···π interactions. The chains are extended into the framework through π..π interactions between the ligands from adjacent chains.

Related literature top

For related non-polymeric complexes including 5-chlorosalicylate ligands, see: Wen & Ying (2007); Wen et al. (2008).

Experimental top

The pH value of a mixture of Pb(NO3)2 (0.5 mmol), phen (0.5 mmol) and 5-chlorosalicylic acid (0.5 mmol) in 8 ml of distilled water and 16 ml of ethanol was adjusted between 5 and 6 by addition of sodium hydroxide. The resultant solution was refluxed for 6 h. After cooling, yellow crystals were formed over 2 days, at room temperature.

Refinement top

H atoms were placed geometrically with bond lengths fixed to 0.82 (OH) and 0.93 Å (CH). Isotropic displacement parameters for H atoms were calculated as Uiso(H) = 1.2Ueq(carrier C) and Uiso(H) = 1.5Ueq(carrier O).

Computing details top

Data collection: APEX2 (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXS97 (Sheldrick, 2008); molecular graphics: SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXTL (Sheldrick, 2008).

Figures top
[Figure 1] Fig. 1. The Pb coordination geometry in the title compound, with thermal ellipsoids at the 50% probability level. Symmetry codes: A 1 - x, -y, -z; B: -x, -y, -z.
[Figure 2] Fig. 2. A section of the structure of the title complex showing SBU with shared corner O atoms.
[Figure 3] Fig. 3. The chain of the title polymer, viewed down the a axis.
catena-Poly[[(1,10-phenanthroline)lead(II)]bis(µ-5-chloro- 2-hydroxybenzoato)] top
Crystal data top
[Pb(C7H4ClO3)2(C12H8N2)]Z = 2
Mr = 730.51F(000) = 700
Triclinic, P1Dx = 1.973 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 8.9100 (1) ÅCell parameters from 5987 reflections
b = 11.2959 (1) Åθ = 2.8–26.9°
c = 13.5816 (1) ŵ = 7.13 mm1
α = 75.508 (1)°T = 296 K
β = 86.302 (1)°Block, yellow
γ = 68.342 (1)°0.28 × 0.25 × 0.24 mm
V = 1229.43 (2) Å3
Data collection top
Bruker APEXII CCD
diffractometer
5987 independent reflections
Radiation source: fine-focus sealed tube5339 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.029
ϕ and ω scansθmax = 28.2°, θmin = 2.0°
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
h = 1111
Tmin = 0.156, Tmax = 0.181k = 1414
21579 measured reflectionsl = 1817
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.025Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.064H-atom parameters constrained
S = 1.05 w = 1/[σ2(Fo2) + (0.0349P)2 + 0.472P]
where P = (Fo2 + 2Fc2)/3
5987 reflections(Δ/σ)max = 0.001
334 parametersΔρmax = 1.18 e Å3
0 restraintsΔρmin = 0.59 e Å3
0 constraints
Crystal data top
[Pb(C7H4ClO3)2(C12H8N2)]γ = 68.342 (1)°
Mr = 730.51V = 1229.43 (2) Å3
Triclinic, P1Z = 2
a = 8.9100 (1) ÅMo Kα radiation
b = 11.2959 (1) ŵ = 7.13 mm1
c = 13.5816 (1) ÅT = 296 K
α = 75.508 (1)°0.28 × 0.25 × 0.24 mm
β = 86.302 (1)°
Data collection top
Bruker APEXII CCD
diffractometer
5987 independent reflections
Absorption correction: multi-scan
(SADABS; Bruker, 2001)
5339 reflections with I > 2σ(I)
Tmin = 0.156, Tmax = 0.181Rint = 0.029
21579 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0250 restraints
wR(F2) = 0.064H-atom parameters constrained
S = 1.05Δρmax = 1.18 e Å3
5987 reflectionsΔρmin = 0.59 e Å3
334 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Pb10.258486 (14)0.038882 (12)0.001073 (10)0.03675 (5)
Cl11.04796 (14)0.31797 (16)0.36720 (10)0.0779 (4)
Cl20.2949 (2)0.0117 (2)0.47404 (14)0.1106 (6)
O50.0025 (3)0.0001 (3)0.1216 (2)0.0495 (6)
O10.5607 (4)0.1240 (3)0.0939 (2)0.0548 (7)
O20.3533 (3)0.1567 (3)0.1750 (2)0.0569 (7)
O40.1160 (4)0.1481 (3)0.1053 (2)0.0604 (8)
N10.2350 (4)0.2615 (3)0.0256 (2)0.0423 (7)
N20.4307 (4)0.1896 (3)0.1218 (3)0.0449 (7)
C120.2979 (4)0.3371 (3)0.0407 (3)0.0394 (8)
O30.3774 (4)0.2835 (5)0.3602 (3)0.0882 (13)
H3B0.33260.24360.30430.132*
C110.3981 (4)0.2980 (4)0.1197 (3)0.0409 (8)
C130.5001 (4)0.1665 (3)0.1727 (3)0.0417 (8)
C140.5973 (4)0.2334 (4)0.2701 (3)0.0421 (8)
C150.5322 (5)0.2888 (6)0.3575 (3)0.0609 (12)
C70.4610 (5)0.3747 (4)0.1912 (3)0.0509 (10)
C80.5574 (6)0.3329 (5)0.2661 (4)0.0615 (12)
H8A0.60050.38040.31480.074*
O60.0401 (4)0.3062 (3)0.2185 (3)0.0704 (9)
H6B0.08090.27560.17020.106*
C210.0455 (4)0.1217 (4)0.2486 (3)0.0419 (8)
C40.2689 (5)0.4538 (4)0.0344 (4)0.0496 (9)
C10.1447 (5)0.2992 (4)0.0995 (3)0.0506 (9)
H1A0.10000.24650.14460.061*
C220.0349 (5)0.2293 (5)0.2767 (3)0.0512 (10)
C190.7579 (5)0.2452 (4)0.2740 (3)0.0449 (8)
H19A0.80400.21070.21600.054*
C200.0289 (4)0.0873 (4)0.1522 (3)0.0447 (9)
C90.5890 (6)0.2234 (5)0.2688 (4)0.0634 (12)
H9A0.65230.19460.31910.076*
C20.1143 (6)0.4148 (5)0.1118 (4)0.0590 (11)
H2A0.05330.43960.16550.071*
C100.5239 (5)0.1554 (5)0.1941 (3)0.0551 (10)
H10A0.54750.08140.19520.066*
C260.1257 (5)0.0475 (4)0.3101 (3)0.0510 (9)
H26A0.13470.02360.29160.061*
C30.1744 (6)0.4899 (4)0.0450 (4)0.0616 (12)
H3A0.15290.56600.05170.074*
C50.3351 (6)0.5275 (5)0.1086 (4)0.0664 (13)
H5A0.31470.60330.10540.080*
C60.4259 (6)0.4894 (5)0.1825 (4)0.0660 (13)
H6A0.46730.53960.22970.079*
C250.1914 (6)0.0793 (5)0.3981 (3)0.0638 (12)
C240.1821 (6)0.1881 (6)0.4256 (4)0.0740 (15)
H24A0.22850.20990.48510.089*
C230.1051 (6)0.2610 (6)0.3650 (4)0.0688 (13)
H23A0.09930.33350.38300.083*
C180.8483 (5)0.3069 (5)0.3622 (3)0.0616 (12)
C170.7827 (7)0.3620 (7)0.4485 (4)0.0867 (19)
H17A0.84470.40350.50850.104*
C160.6277 (7)0.3553 (7)0.4453 (4)0.090 (2)
H16A0.58530.39560.50250.108*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Pb10.03379 (8)0.04199 (8)0.03692 (8)0.01778 (5)0.00344 (5)0.00846 (5)
Cl10.0494 (6)0.1113 (10)0.0641 (8)0.0373 (7)0.0139 (5)0.0104 (7)
Cl20.1064 (12)0.1390 (15)0.0809 (10)0.0634 (11)0.0396 (9)0.0020 (10)
O50.0489 (15)0.0541 (15)0.0449 (16)0.0154 (13)0.0012 (12)0.0156 (13)
O10.0612 (18)0.0596 (17)0.0402 (16)0.0272 (15)0.0072 (13)0.0037 (13)
O20.0420 (15)0.0743 (19)0.0543 (18)0.0233 (14)0.0065 (13)0.0106 (15)
O40.0583 (18)0.072 (2)0.0588 (19)0.0311 (16)0.0224 (15)0.0228 (16)
N10.0386 (16)0.0421 (15)0.0465 (18)0.0169 (13)0.0001 (13)0.0076 (13)
N20.0396 (16)0.0503 (18)0.0479 (19)0.0189 (14)0.0051 (14)0.0144 (15)
C120.0337 (17)0.0355 (17)0.044 (2)0.0068 (14)0.0094 (15)0.0072 (14)
O30.054 (2)0.168 (4)0.055 (2)0.063 (2)0.0100 (16)0.016 (2)
C110.0334 (17)0.0426 (18)0.043 (2)0.0090 (15)0.0082 (15)0.0089 (15)
C130.0431 (19)0.0386 (18)0.046 (2)0.0132 (15)0.0020 (16)0.0157 (16)
C140.0409 (19)0.051 (2)0.038 (2)0.0194 (16)0.0004 (15)0.0123 (16)
C150.052 (2)0.097 (4)0.042 (2)0.037 (2)0.0066 (19)0.017 (2)
C70.047 (2)0.049 (2)0.048 (2)0.0041 (17)0.0109 (18)0.0144 (18)
C80.059 (3)0.073 (3)0.045 (2)0.010 (2)0.003 (2)0.023 (2)
O60.068 (2)0.075 (2)0.085 (3)0.0421 (18)0.0217 (18)0.0284 (19)
C210.0324 (17)0.054 (2)0.0364 (19)0.0137 (16)0.0002 (14)0.0095 (16)
C40.050 (2)0.0374 (19)0.058 (2)0.0137 (17)0.0157 (19)0.0045 (17)
C10.050 (2)0.051 (2)0.050 (2)0.0226 (18)0.0022 (18)0.0045 (18)
C220.038 (2)0.065 (3)0.052 (2)0.0196 (19)0.0005 (17)0.016 (2)
C190.0416 (19)0.052 (2)0.039 (2)0.0193 (17)0.0012 (16)0.0035 (16)
C200.0338 (18)0.055 (2)0.040 (2)0.0095 (16)0.0021 (15)0.0103 (17)
C90.053 (3)0.079 (3)0.055 (3)0.020 (2)0.010 (2)0.017 (2)
C20.054 (2)0.058 (3)0.061 (3)0.029 (2)0.000 (2)0.005 (2)
C100.050 (2)0.064 (3)0.056 (3)0.026 (2)0.014 (2)0.018 (2)
C260.044 (2)0.061 (2)0.046 (2)0.0218 (19)0.0014 (17)0.0048 (18)
C30.061 (3)0.046 (2)0.078 (3)0.027 (2)0.011 (2)0.003 (2)
C50.072 (3)0.045 (2)0.085 (4)0.019 (2)0.014 (3)0.021 (2)
C60.073 (3)0.054 (2)0.069 (3)0.010 (2)0.007 (3)0.029 (2)
C250.052 (2)0.088 (3)0.043 (2)0.028 (2)0.0101 (19)0.000 (2)
C240.061 (3)0.111 (4)0.047 (3)0.022 (3)0.012 (2)0.030 (3)
C230.065 (3)0.087 (3)0.063 (3)0.028 (3)0.011 (2)0.036 (3)
C180.049 (2)0.090 (3)0.044 (2)0.033 (2)0.0051 (19)0.001 (2)
C170.068 (3)0.146 (6)0.042 (3)0.053 (4)0.011 (2)0.010 (3)
C160.078 (4)0.157 (6)0.040 (3)0.067 (4)0.001 (2)0.006 (3)
Geometric parameters (Å, º) top
Pb1—O22.458 (3)C8—H8A0.9300
Pb1—O52.703 (3)O6—C221.358 (6)
Pb1—O42.734 (3)O6—H6B0.8200
Pb1—O5i2.768 (3)C21—C261.388 (6)
Pb1—O12.785 (3)C21—C221.399 (6)
Pb1—O1ii2.887 (3)C21—C201.502 (5)
Pb1—N12.534 (3)C4—C31.398 (7)
Pb1—N22.662 (3)C4—C51.426 (7)
Cl1—C181.742 (4)C1—C21.397 (6)
Cl2—C251.737 (5)C1—H1A0.9300
O5—C201.259 (5)C22—C231.382 (6)
O5—Pb1i2.768 (3)C19—C181.364 (6)
O1—C131.235 (5)C19—H19A0.9300
O1—Pb1ii2.887 (3)C9—C101.393 (7)
O2—C131.270 (5)C9—H9A0.9300
O4—C201.261 (5)C2—C31.348 (7)
N1—C11.331 (5)C2—H2A0.9300
N1—C121.350 (5)C10—H10A0.9300
N2—C101.321 (5)C26—C251.366 (6)
N2—C111.353 (5)C26—H26A0.9300
C12—C41.416 (5)C3—H3A0.9300
C12—C111.439 (5)C5—C61.336 (8)
O3—C151.357 (5)C5—H5A0.9300
O3—H3B0.8200C6—H6A0.9300
C11—C71.415 (5)C25—C241.402 (8)
C13—C141.495 (5)C24—C231.354 (8)
C14—C191.390 (5)C24—H24A0.9300
C14—C151.395 (6)C23—H23A0.9300
C15—C161.386 (7)C18—C171.385 (7)
C7—C81.394 (7)C17—C161.358 (7)
C7—C61.417 (7)C17—H17A0.9300
C8—C91.358 (7)C16—H16A0.9300
O2—Pb1—N174.00 (10)O2—C13—C14116.7 (4)
O2—Pb1—N2107.51 (10)O1—C13—Pb168.5 (2)
N1—Pb1—N263.52 (10)O2—C13—Pb153.5 (2)
O2—Pb1—O570.89 (9)C14—C13—Pb1170.2 (3)
N1—Pb1—O581.85 (9)C19—C14—C15118.5 (4)
N2—Pb1—O5143.50 (9)C19—C14—C13120.0 (3)
O2—Pb1—O476.94 (10)C15—C14—C13121.5 (3)
N1—Pb1—O4128.10 (10)O3—C15—C16117.5 (4)
N2—Pb1—O4168.25 (9)O3—C15—C14122.5 (4)
O5—Pb1—O448.05 (9)C16—C15—C14120.0 (4)
O2—Pb1—O5i135.16 (9)C8—C7—C11117.1 (4)
N1—Pb1—O5i73.83 (9)C8—C7—C6123.7 (4)
N2—Pb1—O5i84.71 (9)C11—C7—C6119.2 (4)
O5—Pb1—O5i74.36 (9)C9—C8—C7120.6 (4)
O4—Pb1—O5i99.85 (9)C9—C8—H8A119.7
O2—Pb1—O148.91 (9)C7—C8—H8A119.7
N1—Pb1—O197.78 (9)C22—O6—H6B109.5
N2—Pb1—O181.42 (10)C26—C21—C22119.5 (4)
O5—Pb1—O1116.23 (9)C26—C21—C20120.4 (4)
O4—Pb1—O194.20 (10)C22—C21—C20120.1 (4)
O5i—Pb1—O1165.95 (9)C3—C4—C12117.3 (4)
O2—Pb1—O1ii111.66 (9)C3—C4—C5123.5 (4)
N1—Pb1—O1ii145.69 (10)C12—C4—C5119.2 (4)
N2—Pb1—O1ii83.09 (9)N1—C1—C2122.6 (4)
O5—Pb1—O1ii132.42 (9)N1—C1—H1A118.7
O4—Pb1—O1ii85.17 (9)C2—C1—H1A118.7
O5i—Pb1—O1ii112.58 (8)O6—C22—C23118.4 (4)
O1—Pb1—O1ii68.01 (9)O6—C22—C21121.9 (4)
O2—Pb1—C1324.55 (10)C23—C22—C21119.7 (4)
N1—Pb1—C1385.87 (10)C18—C19—C14120.6 (4)
N2—Pb1—C1394.97 (10)C18—C19—H19A119.7
O5—Pb1—C1393.59 (10)C14—C19—H19A119.7
O4—Pb1—C1384.95 (10)O5—C20—O4122.8 (4)
O5i—Pb1—C13157.51 (10)O5—C20—C21119.4 (4)
O1—Pb1—C1324.36 (9)O4—C20—C21117.8 (4)
O1ii—Pb1—C1389.63 (10)O5—C20—Pb162.0 (2)
O2—Pb1—C2068.44 (10)O4—C20—Pb163.4 (2)
N1—Pb1—C20103.98 (11)C21—C20—Pb1163.5 (2)
N2—Pb1—C20167.39 (11)C8—C9—C10118.2 (5)
O5—Pb1—C2024.29 (10)C8—C9—H9A120.9
O4—Pb1—C2024.36 (10)C10—C9—H9A120.9
O5i—Pb1—C2090.21 (9)C3—C2—C1119.2 (4)
O1—Pb1—C20102.90 (9)C3—C2—H2A120.4
O1ii—Pb1—C20109.53 (11)C1—C2—H2A120.4
C13—Pb1—C2085.33 (10)N2—C10—C9124.0 (5)
O2—Pb1—Pb1i104.32 (7)N2—C10—H10A118.0
N1—Pb1—Pb1i74.65 (7)C9—C10—H10A118.0
N2—Pb1—Pb1i116.10 (7)C25—C26—C21119.7 (4)
O5—Pb1—Pb1i37.70 (6)C25—C26—H26A120.1
O4—Pb1—Pb1i72.18 (7)C21—C26—H26A120.1
O5i—Pb1—Pb1i36.66 (6)C2—C3—C4120.3 (4)
O1—Pb1—Pb1i152.88 (6)C2—C3—H3A119.8
O1ii—Pb1—Pb1i131.46 (6)C4—C3—H3A119.8
C13—Pb1—Pb1i128.72 (8)C6—C5—C4121.2 (4)
C20—Pb1—Pb1i55.75 (7)C6—C5—H5A119.4
C20—O5—Pb193.7 (2)C4—C5—H5A119.4
C20—O5—Pb1i126.0 (2)C5—C6—C7121.9 (4)
Pb1—O5—Pb1i105.64 (9)C5—C6—H6A119.0
C13—O1—Pb187.2 (2)C7—C6—H6A119.0
C13—O1—Pb1ii145.9 (3)C26—C25—C24120.7 (4)
Pb1—O1—Pb1ii111.99 (9)C26—C25—Cl2119.8 (4)
C13—O2—Pb1101.9 (3)C24—C25—Cl2119.5 (4)
C20—O4—Pb192.2 (2)C23—C24—C25119.5 (4)
C1—N1—C12118.6 (3)C23—C24—H24A120.3
C1—N1—Pb1119.9 (3)C25—C24—H24A120.3
C12—N1—Pb1121.1 (2)C24—C23—C22120.9 (5)
C10—N2—C11117.9 (4)C24—C23—H23A119.6
C10—N2—Pb1124.7 (3)C22—C23—H23A119.6
C11—N2—Pb1116.5 (2)C19—C18—C17120.4 (4)
N1—C12—C4121.9 (4)C19—C18—Cl1120.3 (3)
N1—C12—C11118.9 (3)C17—C18—Cl1119.3 (4)
C4—C12—C11119.2 (4)C16—C17—C18119.9 (5)
C15—O3—H3B109.5C16—C17—H17A120.1
N2—C11—C7122.2 (4)C18—C17—H17A120.1
N2—C11—C12118.5 (3)C17—C16—C15120.5 (5)
C7—C11—C12119.3 (4)C17—C16—H16A119.8
O1—C13—O2122.0 (4)C15—C16—H16A119.8
O1—C13—C14121.3 (3)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z.

Experimental details

Crystal data
Chemical formula[Pb(C7H4ClO3)2(C12H8N2)]
Mr730.51
Crystal system, space groupTriclinic, P1
Temperature (K)296
a, b, c (Å)8.9100 (1), 11.2959 (1), 13.5816 (1)
α, β, γ (°)75.508 (1), 86.302 (1), 68.342 (1)
V3)1229.43 (2)
Z2
Radiation typeMo Kα
µ (mm1)7.13
Crystal size (mm)0.28 × 0.25 × 0.24
Data collection
DiffractometerBruker APEXII CCD
diffractometer
Absorption correctionMulti-scan
(SADABS; Bruker, 2001)
Tmin, Tmax0.156, 0.181
No. of measured, independent and
observed [I > 2σ(I)] reflections
21579, 5987, 5339
Rint0.029
(sin θ/λ)max1)0.664
Refinement
R[F2 > 2σ(F2)], wR(F2), S 0.025, 0.064, 1.05
No. of reflections5987
No. of parameters334
H-atom treatmentH-atom parameters constrained
Δρmax, Δρmin (e Å3)1.18, 0.59

Computer programs: APEX2 (Bruker, 2001), SAINT (Bruker, 2001), SHELXS97 (Sheldrick, 2008), SHELXTL (Sheldrick, 2008).

 

Acknowledgements

The authors are grateful for financial support from the Foundation of Zhejiang Educational Committee (No. Y200908533), the Open Fund for Zhejiang Provincial Key of Biological and Chemical Utilization of Forest Resources (No. 200907) and the Fund of Zhejiang Forestry University (No. 235100998).

References

First citationBruker (2001). APEX2, SAINT and SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.
First citationSheldrick, G. M. (2008). Acta Cryst. A64, 112–122.  Web of Science CrossRef CAS IUCr Journals
First citationWen, D., Xie, J. & Jiang, X. (2008). Acta Cryst. E64, m851–m852.  Web of Science CSD CrossRef IUCr Journals
First citationWen, D. & Ying, S. (2007). Acta Cryst. E63, m2407–m2408.  Web of Science CSD CrossRef IUCr Journals

This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.

Journal logoCRYSTALLOGRAPHIC
COMMUNICATIONS
ISSN: 2056-9890
Follow Acta Cryst. E
Sign up for e-alerts
Follow Acta Cryst. on Twitter
Follow us on facebook
Sign up for RSS feeds