Literature DB >> 21583430

Poly[μ-aqua-di-μ-benzoato-lead(II)].

Abstract

The reaction of lead(II) nitrate and benzoic acid in aqueous solution yields the title polymer, [Pb(C(7)H(5)O(2))(2)(H(2)O)](n). The asymmetric unit contains one Pb(II) ion, two benzoate ligands and one water mol-ecule. The Pb-O bond distances are in the range 2.494 (4)-2.735 (4) Å. The Pb⋯Pb distance is 4.0683 (4) Å, indicating an insignificant metal-metal inter-action. The Pb(II) atom has a distorted penta-gonal-bipyramidal geometry chelated by two carboxyl-ate O atoms. The Pb atoms are bridged through a coordinating water mol-ecule and two carboxyl-ate O atoms from another two benzoate ligands, giving an infinite three-dimensional supra-molecular structure. O-H⋯O hydrogen-bonding inter-actions involved the coordinating water and carboxyl-ate O atoms enhance the stability of the supra-molecular arrangement.

Entities: Chemical Disease Gene Species

Year: 2009 PMID： 21583430 PMCID： PMC2977498 DOI： 10.1107/S1600536809028542

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

Related literature

For general background to lead(II) compounds, see: Shi et al. (2007 ▶); Fan & Zhu (2006 ▶); Wang et al. (2006 ▶); Kim et al. (2001 ▶). For related structures, see: Shi et al. (2007 ▶).

Experimental

Crystal data

[Pb(C7H5O2)2(H2O)] M = 467.43 Monoclinic, a = 15.4118 (12) Å b = 7.5122 (6) Å c = 11.4856 (9) Å β = 91.2930 (10)° V = 1329.42 (18) Å3 Z = 4 Mo Kα radiation μ = 12.71 mm−1 T = 295 K 0.40 × 0.10 × 0.08 mm

Data collection

Bruker APEXII CCD area-detector diffractometer Absorption correction: multi-scan (SADABS; Bruker, 2007 ▶) T min = 0.1, T max = 0.247 (expected range = 0.146–0.362) 13406 measured reflections 2664 independent reflections 2315 reflections with I > 2σ(I) R int = 0.057

Refinement

R[F 2 > 2σ(F 2)] = 0.034 wR(F 2) = 0.087 S = 1.09 2664 reflections 181 parameters H-atom parameters constrained Δρmax = 3.35 e Å−3 Δρmin = −1.31 e Å−3 Data collection: APEX2 (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. Crystal structure: contains datablocks global, I. DOI: 10.1107/S1600536809028542/fj2238sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536809028542/fj2238Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Pb(C₇H₅O₂)₂(H₂O)]	F(000) = 872
M_r = 467.43	D_x = 2.335 Mg m⁻³
Monoclinic, P2₁/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 4827 reflections
a = 15.4118 (12) Å	θ = 2.6–28.5°
b = 7.5122 (6) Å	µ = 12.71 mm⁻¹
c = 11.4856 (9) Å	T = 295 K
β = 91.293 (1)°	Block, colorless
V = 1329.42 (18) Å³	0.4 × 0.1 × 0.08 mm
Z = 4

Bruker APEXII CCD area-detector diffractometer	2664 independent reflections
Radiation source: fine-focus sealed tube	2315 reflections with I > 2σ(I)
graphite	R_int = 0.057
φ and ω scans	θ_max = 26.2°, θ_min = 3.2°
Absorption correction: multi-scan (SADABS; Bruker, 2007)	h = −19→18
T_min = 0.1, T_max = 0.247	k = −9→9
13406 measured reflections	l = −14→14

Refinement on F²	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.034	H-atom parameters constrained
wR(F²) = 0.087	w = 1/[σ²(F_o²) + (0.047P)²] where P = (F_o² + 2F_c²)/3
S = 1.09	(Δ/σ)_max < 0.001
2664 reflections	Δρ_max = 3.35 e Å⁻³
181 parameters	Δρ_min = −1.31 e Å⁻³
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 2008)
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.082

	x	y	z	U_iso*/U_eq
Pb1	0.478855 (16)	0.52214 (3)	0.311202 (19)	0.02834 (12)
O1	0.6082 (3)	0.3213 (6)	0.3120 (4)	0.0390 (11)
O2	0.5947 (4)	0.4879 (5)	0.4674 (4)	0.0401 (12)
O3	0.5875 (3)	0.6929 (5)	0.1986 (4)	0.0372 (11)
O4	0.6356 (4)	0.5476 (7)	0.0428 (4)	0.0453 (13)
O5	0.4960 (3)	0.3455 (6)	0.1048 (3)	0.0349 (10)
H5A	0.4562	0.3648	0.0539	0.052*
H5B	0.5374	0.3865	0.0651	0.052*
C1	0.6397 (4)	0.3861 (8)	0.4045 (5)	0.0310 (14)
C2	0.7318 (4)	0.3531 (8)	0.4365 (5)	0.0286 (13)
C3	0.7840 (5)	0.2548 (9)	0.3639 (5)	0.0370 (15)
H3A	0.7596	0.1994	0.2986	0.044*
C4	0.8716 (5)	0.2383 (10)	0.3876 (6)	0.0469 (18)
H4A	0.9062	0.1732	0.3378	0.056*
C5	0.9082 (5)	0.3177 (10)	0.4847 (6)	0.0495 (19)
H5C	0.9675	0.3082	0.4996	0.059*
C6	0.8567 (5)	0.4114 (10)	0.5599 (6)	0.0470 (18)
H6A	0.8810	0.4624	0.6268	0.056*
C7	0.7695 (5)	0.4291 (9)	0.5356 (6)	0.0405 (16)
H7A	0.7351	0.4930	0.5863	0.049*
C8	0.6480 (4)	0.6270 (8)	0.1387 (5)	0.0309 (14)
C9	0.7395 (4)	0.6483 (7)	0.1816 (5)	0.0270 (13)
C10	0.8062 (4)	0.5691 (9)	0.1224 (5)	0.0346 (14)
H10A	0.7938	0.5033	0.0554	0.042*
C11	0.8914 (5)	0.5869 (11)	0.1619 (6)	0.0462 (17)
H11A	0.9361	0.5359	0.1203	0.055*
C12	0.9098 (5)	0.6794 (11)	0.2623 (6)	0.0503 (19)
H12A	0.9668	0.6896	0.2898	0.060*
C13	0.8433 (5)	0.7573 (10)	0.3222 (6)	0.050 (2)
H13A	0.8560	0.8209	0.3899	0.060*
C14	0.7587 (5)	0.7427 (9)	0.2838 (6)	0.0408 (17)
H14A	0.7144	0.7952	0.3254	0.049*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.02962 (19)	0.02363 (16)	0.03171 (17)	0.00173 (9)	−0.00073 (11)	0.00129 (8)
O1	0.030 (3)	0.042 (3)	0.044 (3)	0.001 (2)	−0.010 (2)	−0.004 (2)
O2	0.039 (3)	0.041 (3)	0.041 (3)	0.015 (2)	0.005 (2)	0.0009 (19)
O3	0.036 (3)	0.027 (2)	0.049 (3)	0.0032 (19)	0.011 (2)	0.0011 (19)
O4	0.037 (3)	0.056 (3)	0.043 (3)	−0.001 (2)	−0.004 (2)	−0.006 (2)
O5	0.043 (3)	0.033 (2)	0.028 (2)	−0.005 (2)	−0.0034 (19)	0.0054 (17)
C1	0.035 (4)	0.030 (3)	0.028 (3)	−0.003 (3)	−0.001 (3)	0.009 (2)
C2	0.027 (4)	0.026 (3)	0.032 (3)	0.004 (2)	−0.002 (3)	0.003 (2)
C3	0.039 (4)	0.041 (4)	0.031 (3)	0.001 (3)	−0.005 (3)	−0.003 (3)
C4	0.037 (5)	0.053 (5)	0.051 (4)	0.005 (3)	0.008 (3)	0.003 (3)
C5	0.034 (4)	0.057 (5)	0.057 (5)	−0.003 (4)	−0.006 (4)	0.012 (4)
C6	0.052 (5)	0.045 (4)	0.044 (4)	−0.006 (4)	−0.011 (4)	−0.002 (3)
C7	0.048 (5)	0.038 (4)	0.035 (4)	0.005 (3)	−0.010 (3)	−0.008 (3)
C8	0.037 (4)	0.021 (3)	0.035 (3)	0.002 (3)	0.001 (3)	0.006 (2)
C9	0.031 (4)	0.022 (3)	0.028 (3)	−0.006 (2)	0.000 (2)	0.006 (2)
C10	0.029 (4)	0.041 (4)	0.034 (3)	−0.003 (3)	0.002 (3)	−0.003 (3)
C11	0.033 (4)	0.055 (5)	0.051 (4)	0.003 (4)	0.006 (3)	−0.004 (4)
C12	0.039 (5)	0.060 (5)	0.052 (4)	−0.004 (4)	−0.012 (4)	0.002 (4)
C13	0.057 (6)	0.053 (5)	0.039 (4)	−0.008 (4)	−0.012 (4)	−0.007 (3)
C14	0.048 (5)	0.033 (4)	0.041 (4)	−0.004 (3)	0.008 (3)	−0.005 (3)

Pb1—O3	2.494 (4)	C4—C5	1.374 (10)
Pb1—O1	2.499 (4)	C4—H4A	0.9300
Pb1—O2	2.515 (5)	C5—C6	1.379 (10)
Pb1—O5ⁱ	2.639 (4)	C5—H5C	0.9300
Pb1—O3ⁱⁱ	2.677 (4)	C6—C7	1.374 (10)
Pb1—O5	2.735 (4)	C6—H6A	0.9300
Pb1—C1	2.867 (6)	C7—H7A	0.9300
O1—C1	1.256 (7)	C8—C9	1.493 (8)
O2—C1	1.269 (8)	C9—C10	1.379 (9)
O3—C8	1.271 (7)	C9—C14	1.397 (8)
O3—Pb1ⁱ	2.677 (4)	C10—C11	1.386 (10)
O4—C8	1.264 (7)	C10—H10A	0.9300
O5—Pb1ⁱⁱ	2.639 (4)	C11—C12	1.370 (10)
O5—H5A	0.8500	C11—H11A	0.9300
O5—H5B	0.8500	C12—C13	1.378 (10)
C1—C2	1.479 (8)	C12—H12A	0.9300
C2—C3	1.385 (8)	C13—C14	1.371 (10)
C2—C7	1.389 (8)	C13—H13A	0.9300
C3—C4	1.377 (10)	C14—H14A	0.9300
C3—H3A	0.9300

O3—Pb1—O1	76.58 (15)	C3—C2—C1	120.5 (5)
O3—Pb1—O2	87.06 (16)	C7—C2—C1	121.1 (6)
O1—Pb1—O2	51.87 (14)	C4—C3—C2	120.6 (6)
O3—Pb1—O5ⁱ	67.76 (13)	C4—C3—H3A	119.7
O1—Pb1—O5ⁱ	116.34 (14)	C2—C3—H3A	119.7
O2—Pb1—O5ⁱ	74.78 (13)	C5—C4—C3	120.2 (7)
O3—Pb1—O3ⁱⁱ	135.53 (10)	C5—C4—H4A	119.9
O1—Pb1—O3ⁱⁱ	75.30 (14)	C3—C4—H4A	119.9
O2—Pb1—O3ⁱⁱ	101.51 (14)	C4—C5—C6	119.9 (7)
O5ⁱ—Pb1—O3ⁱⁱ	156.67 (12)	C4—C5—H5C	120.0
O3—Pb1—O5	73.78 (13)	C6—C5—H5C	120.0
O1—Pb1—O5	67.52 (13)	C7—C6—C5	119.7 (7)
O2—Pb1—O5	119.18 (14)	C7—C6—H6A	120.1
O5ⁱ—Pb1—O5	138.36 (11)	C5—C6—H6A	120.1
O3ⁱⁱ—Pb1—O5	63.89 (12)	C6—C7—C2	121.1 (7)
O3—Pb1—C1	78.02 (15)	C6—C7—H7A	119.5
O1—Pb1—C1	25.93 (15)	C2—C7—H7A	119.5
O2—Pb1—C1	26.25 (15)	O4—C8—O3	123.8 (6)
O5ⁱ—Pb1—C1	94.18 (15)	O4—C8—C9	117.5 (6)
O3ⁱⁱ—Pb1—C1	90.71 (16)	O3—C8—C9	118.7 (5)
O5—Pb1—C1	92.94 (15)	C10—C9—C14	119.2 (6)
C1—O1—Pb1	93.6 (4)	C10—C9—C8	120.0 (5)
C1—O2—Pb1	92.5 (4)	C14—C9—C8	120.8 (6)
C8—O3—Pb1	126.1 (4)	C9—C10—C11	120.5 (6)
C8—O3—Pb1ⁱ	128.4 (4)	C9—C10—H10A	119.8
Pb1—O3—Pb1ⁱ	103.70 (15)	C11—C10—H10A	119.8
Pb1ⁱⁱ—O5—Pb1	98.38 (12)	C12—C11—C10	120.1 (7)
Pb1ⁱⁱ—O5—H5A	120.4	C12—C11—H11A	119.9
Pb1—O5—H5A	115.5	C10—C11—H11A	119.9
Pb1ⁱⁱ—O5—H5B	115.0	C11—C12—C13	119.5 (7)
Pb1—O5—H5B	112.2	C11—C12—H12A	120.3
H5A—O5—H5B	96.3	C13—C12—H12A	120.3
O1—C1—O2	120.6 (6)	C14—C13—C12	121.2 (7)
O1—C1—C2	119.7 (6)	C14—C13—H13A	119.4
O2—C1—C2	119.5 (6)	C12—C13—H13A	119.4
O1—C1—Pb1	60.5 (3)	C13—C14—C9	119.5 (7)
O2—C1—Pb1	61.2 (4)	C13—C14—H14A	120.3
C2—C1—Pb1	165.8 (4)	C9—C14—H14A	120.3
C3—C2—C7	118.3 (6)

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5A···O4ⁱⁱⁱ	0.85	1.90	2.734 (7)	168
O5—H5B···O4	0.85	1.96	2.740 (7)	152

Table 1

Selected bond lengths (Å)

Pb1—O3	2.494 (4)
Pb1—O1	2.499 (4)
Pb1—O2	2.515 (5)
Pb1—O5ⁱ	2.639 (4)
Pb1—O3ⁱⁱ	2.677 (4)
Pb1—O5	2.735 (4)
Pb1—C1ⁱⁱ	2.867 (6)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5A⋯O4ⁱⁱⁱ	0.85	1.90	2.734 (7)	168
O5—H5B⋯O4	0.85	1.96	2.740 (7)	152

Symmetry code: (iii) .

3 in total

1. Influence of the reaction conditions on the self-assembly of lead(II) 5-sulfosalicylate coordination polymers with chelating amine ligands.

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Journal: Inorg Chem Date: 2006-09-18 Impact factor: 5.165

2. A short history of SHELX.

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

3. Assembly of metal-organic frameworks from large organic and inorganic secondary building units: new examples and simplifying principles for complex structures.

Authors: J Kim; B Chen; T M Reineke; H Li; M Eddaoudi; D B Moler; M O'Keeffe; O M Yaghi
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3 in total