Literature DB >> 21588208

catena-Poly[[(1,10-phenanthroline)lead(II)]bis-(μ-5-chloro-2-hy-droxy-benzoato)].

Lei Yang, Bing Li, Qing Xue, Yu Huo, Gaopeng Wang.   

Abstract

In the title polymer, [Pb(C(7)H(4)ClO(3))(2)(C(12)H(8)N(2))](n), the Pb(II) ion displays a distorted pseudo-octa-hedral coordination geometry. The metal center is coordinated by six O atoms from four 5-chloro-salicylate ligands and two N atoms from a chelating phenanthroline ligand. The polymeric structure is built up from bridging carboxyl-ate O atoms, forming chains along [100]. The crystal structure is stabilized by π-π inter-actions between the 1,10-phenanthroline and 5-chloro-salicylate ligands, the shortest centroid-centroid separation between neighbouring aromatic rings being 3.652 (1) Å.

Entities:  

Year:  2010        PMID: 21588208      PMCID: PMC3007493          DOI: 10.1107/S1600536810023561

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


Related literature

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

Experimental

Crystal data

[Pb(C7H4ClO3)2(C12H8N2)] M = 730.51 Triclinic, 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 ▶) T min = 0.156, T max = 0.181 21579 measured reflections 5987 independent reflections 5339 reflections with I > 2σ(I) R int = 0.029

Refinement

R[F 2 > 2σ(F 2)] = 0.025 wR(F 2) = 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 ▶); cell refinement: SAINT (Bruker, 2001 ▶); 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. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810023561/bh2289sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810023561/bh2289Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report
[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
Bruker APEXII CCD diffractometer5987 independent reflections
Radiation source: fine-focus sealed tube5339 reflections with I > 2σ(I)
graphiteRint = 0.029
φ and ω scansθmax = 28.2°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Bruker, 2001)h = −11→11
Tmin = 0.156, Tmax = 0.181k = −14→14
21579 measured reflectionsl = −18→17
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 = 1.05w = 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
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)
Cl2−0.2949 (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)
H3B0.3326−0.24360.30430.132*
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)
H8A0.6005−0.3804−0.31480.074*
O60.0401 (4)0.3062 (3)0.2185 (3)0.0704 (9)
H6B0.08090.27560.17020.106*
C21−0.0455 (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)
H1A0.1000−0.24650.14460.061*
C22−0.0349 (5)0.2293 (5)0.2767 (3)0.0512 (10)
C190.7579 (5)−0.2452 (4)0.2740 (3)0.0449 (8)
H19A0.8040−0.21070.21600.054*
C200.0289 (4)0.0873 (4)0.1522 (3)0.0447 (9)
C90.5890 (6)−0.2234 (5)−0.2688 (4)0.0634 (12)
H9A0.6523−0.1946−0.31910.076*
C20.1143 (6)−0.4148 (5)0.1118 (4)0.0590 (11)
H2A0.0533−0.43960.16550.071*
C100.5239 (5)−0.1554 (5)−0.1941 (3)0.0551 (10)
H10A0.5475−0.0814−0.19520.066*
C26−0.1257 (5)0.0475 (4)0.3101 (3)0.0510 (9)
H26A−0.1347−0.02360.29160.061*
C30.1744 (6)−0.4899 (4)0.0450 (4)0.0616 (12)
H3A0.1529−0.56600.05170.074*
C50.3351 (6)−0.5275 (5)−0.1086 (4)0.0664 (13)
H5A0.3147−0.6033−0.10540.080*
C60.4259 (6)−0.4894 (5)−0.1825 (4)0.0660 (13)
H6A0.4673−0.5396−0.22970.079*
C25−0.1914 (6)0.0793 (5)0.3981 (3)0.0638 (12)
C24−0.1821 (6)0.1881 (6)0.4256 (4)0.0740 (15)
H24A−0.22850.20990.48510.089*
C23−0.1051 (6)0.2610 (6)0.3650 (4)0.0688 (13)
H23A−0.09930.33350.38300.083*
C180.8483 (5)−0.3069 (5)0.3622 (3)0.0616 (12)
C170.7827 (7)−0.3620 (7)0.4485 (4)0.0867 (19)
H17A0.8447−0.40350.50850.104*
C160.6277 (7)−0.3553 (7)0.4453 (4)0.090 (2)
H16A0.5853−0.39560.50250.108*
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)
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)
  2 in total

1.  A short history of SHELX.

Authors:  George M Sheldrick
Journal:  Acta Crystallogr A       Date:  2007-12-21       Impact factor: 2.290

2.  Bis(5-chloro-salicylato-κO)bis-(1,10-phenanthroline-κN,N')cadmium(II).

Authors:  Decai Wen; Jing Xie; Xiurong Jiang
Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2008-06-07
  2 in total
  1 in total

1.  Bis(benzoato-κO,O')(1,10-phenanthroline-κN,N')lead(II) benzoic acid mono-solvate.

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Journal:  Acta Crystallogr Sect E Struct Rep Online       Date:  2010-11-27
  1 in total

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