Literature DB >> 21580222

catena-Poly[[[aqua-[(2-hydroxy-phen-yl)acetato-κO,O']lead(II)]-μ(3)-[(2-hydroxy-phen-yl)acetato-κO:O,O':O']] monohydrate].

Abstract

In the title complex, {[Pb(C(8)H(7)O(3))(2)(H(2)O)]·H(2)O}(n), the Pb(II) atom is seven-coordinated by six carboxyl-ate O atoms from four different 2-hydroxy-phenyl-acetate (2-dph) ligands and one water mol-ecule, displaying a hemidirected irregular geometry, with the empty side of the metal ion capped by a benzene ring forming a Pb⋯π contact [Pb⋯centroid distance = 3.342 (2) Å]. One 2-dph ligand functions in a bridging mode and connects Pb ions into a linear chain. The crystal packing is governed by intra- and inter-molecular O-H⋯O hydrogen bonds.

Entities: CellLine Chemical Disease Gene Species

Year: 2010 PMID： 21580222 PMCID： PMC2983550 DOI： 10.1107/S1600536810004162

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

Related literature

For general background to hydroxyphenylacetate complexes, see: Liwporncharoenvong et al. (2002 ▶); Nie & Li (2009 ▶). For general background to hemi- and holodirected geometries of lead(II) complexes, see: Shimoni-Livny et al. (1998 ▶).

Experimental

Crystal data

[Pb(C8H7O3)2(H2O)]·H2O M = 545.50 Triclinic, a = 7.4610 (15) Å b = 10.721 (2) Å c = 11.701 (2) Å α = 109.72 (3)° β = 90.10 (3)° γ = 102.92 (3)° V = 855.7 (3) Å3 Z = 2 Mo Kα radiation μ = 9.90 mm−1 T = 293 K 0.30 × 0.26 × 0.22 mm

Data collection

Rigaku/MSC Mercury CCD diffractometer Absorption correction: multi-scan (REQAB; Jacobson, 1998 ▶) T min = 0.075, T max = 0.126 6821 measured reflections 3076 independent reflections 2951 reflections with I > 2σ(I) R int = 0.056

Refinement

R[F 2 > 2σ(F 2)] = 0.036 wR(F 2) = 0.084 S = 1.05 3076 reflections 228 parameters 6 restraints H-atom parameters constrained Δρmax = 2.77 e Å−3 Δρmin = −1.58 e Å−3 Data collection: CrystalStructure (Rigaku/MSC, 2002 ▶); cell refinement: CrystalStructure; data reduction: CrystalStructure; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ▶); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008 ▶); molecular graphics: ORTEPII (Johnson, 1976 ▶) and DIAMOND (Brandenburg, 1999 ▶); software used to prepare material for publication: SHELXL97. Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536810004162/hy2276sup1.cif Structure factors: contains datablocks I. DOI: 10.1107/S1600536810004162/hy2276Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Pb(C₈H₇O₃)₂(H₂O)]·H₂O	Z = 2
M_r = 545.50	F(000) = 520
Triclinic, P1	D_x = 2.117 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 7.4610 (15) Å	Cell parameters from 2895 reflections
b = 10.721 (2) Å	θ = 2.4–27.9°
c = 11.701 (2) Å	µ = 9.90 mm⁻¹
α = 109.72 (3)°	T = 293 K
β = 90.10 (3)°	Block, colorless
γ = 102.92 (3)°	0.30 × 0.26 × 0.22 mm
V = 855.7 (3) Å³

Rigaku/MSC Mercury CCD diffractometer	3076 independent reflections
Radiation source: fine-focus sealed tube	2951 reflections with I > 2σ(I)
graphite	R_int = 0.056
ω scans	θ_max = 25.2°, θ_min = 3.1°
Absorption correction: multi-scan (REQAB; Jacobson, 1998)	h = −8→8
T_min = 0.075, T_max = 0.126	k = −12→12
6821 measured reflections	l = −14→14

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F² > 2σ(F²)] = 0.036	Hydrogen site location: inferred from neighbouring sites
wR(F²) = 0.084	H-atom parameters constrained
S = 1.05	w = 1/[σ²(F_o²) + (0.0431P)²] where P = (F_o² + 2F_c²)/3
3076 reflections	(Δ/σ)_max = 0.003
228 parameters	Δρ_max = 2.77 e Å⁻³
6 restraints	Δρ_min = −1.58 e Å⁻³

	x	y	z	U_iso*/U_eq
Pb1	0.76187 (2)	0.029805 (17)	0.601979 (13)	0.02638 (11)
O1	0.6798 (6)	0.2761 (5)	0.6889 (4)	0.0433 (10)
O2	0.9615 (6)	0.2666 (4)	0.6423 (4)	0.0439 (10)
O6	0.7995 (6)	−0.2407 (5)	0.1437 (5)	0.0487 (11)
H6	0.8311	−0.3082	0.1465	0.073*
O5	1.1923 (6)	0.5007 (4)	0.8890 (3)	0.0413 (9)
H5	1.2721	0.5388	0.9460	0.062*
C1	0.8449 (8)	0.3338 (6)	0.6845 (5)	0.0320 (12)
C2	0.9012 (8)	0.4889 (6)	0.7318 (6)	0.0435 (14)
H2A	0.8219	0.5223	0.6892	0.052*
H2B	0.8802	0.5217	0.8175	0.052*
C3	1.0981 (8)	0.5484 (5)	0.7178 (5)	0.0392 (13)
C4	1.1459 (10)	0.6010 (6)	0.6257 (6)	0.0471 (15)
H4	1.0530	0.6059	0.5753	0.056*
C5	1.3273 (10)	0.6461 (7)	0.6070 (6)	0.0512 (17)
H5A	1.3558	0.6801	0.5442	0.061*
C6	1.4641 (10)	0.6410 (7)	0.6797 (6)	0.0531 (17)
H6A	1.5865	0.6687	0.6652	0.064*
C7	1.4221 (9)	0.5938 (6)	0.7770 (6)	0.0443 (14)
H7	1.5162	0.5935	0.8289	0.053*
C8	1.2403 (8)	0.5481 (5)	0.7949 (5)	0.0340 (12)
C9	0.7658 (7)	0.0291 (5)	0.3582 (5)	0.0269 (11)
C10	0.7743 (8)	0.0257 (7)	0.2278 (5)	0.0324 (12)
H10A	0.6655	−0.0388	0.1794	0.039*
H10B	0.7718	0.1151	0.2260	0.039*
C11	0.9411 (7)	−0.0131 (6)	0.1715 (4)	0.0296 (12)
C12	0.9491 (7)	−0.1495 (6)	0.1294 (4)	0.0300 (12)
C13	1.1053 (8)	−0.1886 (7)	0.0786 (5)	0.0407 (14)
H13	1.1097	−0.2799	0.0523	0.049*
C14	1.2530 (9)	−0.0917 (8)	0.0675 (6)	0.0448 (16)
H14	1.3572	−0.1176	0.0332	0.054*
C15	1.2474 (9)	0.0435 (7)	0.1069 (5)	0.0478 (18)
H15	1.3478	0.1088	0.0996	0.057*
C16	1.0910 (9)	0.0828 (6)	0.1580 (5)	0.0390 (14)
H16	1.0871	0.1741	0.1833	0.047*
O3	0.9083 (5)	0.0283 (4)	0.4142 (3)	0.0339 (9)
O4	0.6204 (5)	0.0363 (4)	0.4101 (3)	0.0366 (9)
O1W	0.6888 (6)	−0.2332 (5)	0.4561 (4)	0.0531 (12)
H2W	0.7696	−0.2339	0.4061	0.080*
H1W	0.5860	−0.2720	0.4161	0.080*
O2W	0.4261 (6)	0.6318 (6)	0.0817 (4)	0.0617 (14)
H3W	0.3977	0.6548	0.1537	0.093*
H4W	0.5291	0.6783	0.0746	0.093*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Pb1	0.01845 (15)	0.03419 (16)	0.02621 (15)	0.00640 (11)	0.00500 (9)	0.00999 (11)
O1	0.029 (2)	0.046 (2)	0.049 (2)	0.005 (2)	0.0044 (18)	0.013 (2)
O2	0.031 (2)	0.034 (2)	0.063 (3)	0.0088 (19)	0.017 (2)	0.012 (2)
O6	0.031 (2)	0.041 (2)	0.075 (3)	0.006 (2)	0.004 (2)	0.022 (2)
O5	0.041 (2)	0.042 (2)	0.041 (2)	0.006 (2)	0.0043 (17)	0.0162 (19)
C1	0.026 (3)	0.038 (3)	0.030 (3)	0.006 (3)	0.002 (2)	0.010 (2)
C2	0.029 (3)	0.035 (3)	0.063 (4)	0.008 (3)	0.005 (3)	0.014 (3)
C3	0.034 (3)	0.025 (3)	0.055 (3)	0.005 (3)	0.003 (3)	0.010 (3)
C4	0.061 (4)	0.035 (3)	0.047 (3)	0.013 (3)	0.003 (3)	0.015 (3)
C5	0.055 (4)	0.043 (3)	0.055 (4)	0.002 (3)	0.010 (3)	0.023 (3)
C6	0.043 (4)	0.047 (4)	0.064 (4)	0.002 (3)	0.022 (3)	0.018 (3)
C7	0.031 (3)	0.044 (3)	0.056 (4)	0.005 (3)	0.002 (3)	0.018 (3)
C8	0.029 (3)	0.030 (3)	0.040 (3)	0.006 (2)	0.004 (2)	0.009 (2)
C9	0.022 (3)	0.028 (2)	0.029 (2)	0.006 (2)	0.003 (2)	0.009 (2)
C10	0.027 (3)	0.052 (3)	0.025 (3)	0.018 (3)	0.010 (2)	0.016 (2)
C11	0.029 (3)	0.040 (3)	0.017 (2)	0.014 (3)	0.0021 (19)	0.003 (2)
C12	0.026 (3)	0.036 (3)	0.022 (2)	0.006 (2)	0.0002 (19)	0.003 (2)
C13	0.039 (3)	0.048 (3)	0.039 (3)	0.021 (3)	0.008 (3)	0.013 (3)
C14	0.035 (3)	0.068 (4)	0.038 (3)	0.025 (3)	0.016 (3)	0.018 (3)
C15	0.033 (4)	0.061 (5)	0.048 (4)	0.000 (4)	0.007 (3)	0.024 (4)
C16	0.047 (4)	0.038 (3)	0.026 (2)	0.004 (3)	0.005 (2)	0.008 (2)
O3	0.0205 (19)	0.057 (2)	0.0277 (17)	0.0135 (18)	0.0076 (14)	0.0173 (17)
O4	0.0182 (19)	0.052 (2)	0.044 (2)	0.0106 (18)	0.0099 (16)	0.0217 (19)
O1W	0.046 (3)	0.045 (2)	0.057 (3)	0.000 (2)	0.019 (2)	0.011 (2)
O2W	0.036 (3)	0.092 (4)	0.044 (2)	0.018 (3)	0.007 (2)	0.005 (3)

Pb1—O1	2.701 (5)	C6—H6A	0.9300
Pb1—O2	2.527 (4)	C7—C8	1.377 (8)
Pb1—O3	2.453 (3)	C7—H7	0.9300
Pb1—O3ⁱ	2.662 (4)	C9—O3	1.251 (6)
Pb1—O4	2.508 (4)	C9—O4	1.249 (6)
Pb1—O4ⁱⁱ	2.772 (4)	C9—C10	1.515 (7)
Pb1—O1W	2.687 (4)	C10—C11	1.485 (7)
O1—C1	1.259 (7)	C10—H10A	0.9700
O2—C1	1.249 (7)	C10—H10B	0.9700
O6—C12	1.362 (7)	C11—C12	1.392 (8)
O6—H6	0.8200	C11—C16	1.388 (8)
O5—C8	1.377 (7)	C12—C13	1.393 (8)
O5—H5	0.8200	C13—C14	1.375 (9)
C1—C2	1.521 (8)	C13—H13	0.9300
C2—C3	1.499 (8)	C14—C15	1.375 (9)
C2—H2A	0.9700	C14—H14	0.9300
C2—H2B	0.9700	C15—C16	1.396 (9)
C3—C4	1.389 (9)	C15—H15	0.9300
C3—C8	1.393 (8)	C16—H16	0.9300
C4—C5	1.376 (10)	O1W—H2W	0.8401
C4—H4	0.9300	O1W—H1W	0.8400
C5—C6	1.349 (10)	O2W—H3W	0.8365
C5—H5A	0.9300	O2W—H4W	0.8383
C6—C7	1.403 (9)

O3—Pb1—O4	51.86 (12)	C5—C6—C7	120.2 (6)
O3—Pb1—O2	72.89 (14)	C5—C6—H6A	119.9
O4—Pb1—O2	89.65 (15)	C7—C6—H6A	119.9
O3—Pb1—O3ⁱ	64.41 (14)	C8—C7—C6	119.5 (6)
O4—Pb1—O3ⁱ	115.37 (11)	C8—C7—H7	120.2
O2—Pb1—O3ⁱ	80.89 (13)	C6—C7—H7	120.2
O3—Pb1—O1W	74.25 (14)	O5—C8—C7	121.6 (6)
O4—Pb1—O1W	77.54 (15)	O5—C8—C3	117.7 (5)
O2—Pb1—O1W	145.72 (13)	C7—C8—C3	120.7 (6)
O3ⁱ—Pb1—O1W	76.41 (14)	O3—C9—O4	120.4 (5)
O3—Pb1—O1	104.29 (14)	O3—C9—C10	118.9 (4)
O4—Pb1—O1	80.18 (14)	O4—C9—C10	120.6 (5)
O2—Pb1—O1	49.36 (13)	C11—C10—C9	113.5 (4)
O3ⁱ—Pb1—O1	128.80 (13)	C11—C10—H10A	108.9
O1—Pb1—O4ⁱⁱ	76.94 (13)	C9—C10—H10A	108.9
O2—Pb1—O4ⁱⁱ	125.05 (14)	C11—C10—H10B	108.9
O3—Pb1—O4ⁱⁱ	117.78 (12)	C9—C10—H10B	108.9
O3ⁱ—Pb1—O4ⁱⁱ	154.01 (12)	H10A—C10—H10B	107.7
O4—Pb1—O4ⁱⁱ	67.94 (11)	C12—C11—C16	118.2 (5)
O1W—Pb1—O4ⁱⁱ	79.49 (13)	C12—C11—C10	119.8 (5)
O1W—Pb1—O1	152.25 (15)	C16—C11—C10	122.1 (5)
C1—O1—Pb1	90.2 (4)	O6—C12—C11	116.6 (5)
C1—O2—Pb1	98.8 (3)	O6—C12—C13	122.3 (5)
C12—O6—H6	109.5	C11—C12—C13	121.1 (5)
C8—O5—H5	109.5	C14—C13—C12	119.7 (6)
O2—C1—O1	121.5 (5)	C14—C13—H13	120.1
O2—C1—C2	120.0 (5)	C12—C13—H13	120.1
O1—C1—C2	118.5 (5)	C15—C14—C13	120.3 (6)
C3—C2—C1	114.7 (5)	C15—C14—H14	119.9
C3—C2—H2A	108.6	C13—C14—H14	119.9
C1—C2—H2A	108.6	C14—C15—C16	120.0 (6)
C3—C2—H2B	108.6	C14—C15—H15	120.0
C1—C2—H2B	108.6	C16—C15—H15	120.0
H2A—C2—H2B	107.6	C11—C16—C15	120.7 (6)
C4—C3—C8	117.8 (6)	C11—C16—H16	119.6
C4—C3—C2	121.6 (6)	C15—C16—H16	119.6
C8—C3—C2	120.6 (6)	C9—O3—Pb1	95.1 (3)
C5—C4—C3	121.5 (7)	C9—O3—Pb1ⁱ	146.8 (3)
C5—C4—H4	119.2	Pb1—O3—Pb1ⁱ	115.59 (14)
C3—C4—H4	119.2	C9—O4—Pb1	92.5 (3)
C6—C5—C4	120.1 (6)	H2W—O1W—H1W	107.6
C6—C5—H5A	119.9	H3W—O2W—H4W	112.2
C4—C5—H5A	119.9

D—H···A	D—H	H···A	D···A	D—H···A
O5—H5···O2Wⁱⁱⁱ	0.82	1.80	2.618 (6)	173
O6—H6···O5ⁱ	0.82	1.93	2.698 (6)	156
O1W—H1W···O1ⁱⁱ	0.84	2.31	3.089 (6)	154
O1W—H2W···O2ⁱ	0.84	2.16	2.900 (6)	147
O2W—H3W···O1^iv	0.84	1.88	2.715 (6)	172
O2W—H4W···O6^v	0.84	2.05	2.788 (7)	146

Table 1

Selected bond lengths (Å)

Pb1—O1	2.701 (5)
Pb1—O2	2.527 (4)
Pb1—O3	2.453 (3)
Pb1—O3ⁱ	2.662 (4)
Pb1—O4	2.508 (4)
Pb1—O4ⁱⁱ	2.772 (4)
Pb1—O1W	2.687 (4)

Symmetry codes: (i) ; (ii) .

Table 2

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O5—H5⋯O2Wⁱⁱⁱ	0.82	1.80	2.618 (6)	173
O6—H6⋯O5ⁱ	0.82	1.93	2.698 (6)	156
O1W—H1W⋯O1ⁱⁱ	0.84	2.31	3.089 (6)	154
O1W—H2W⋯O2ⁱ	0.84	2.16	2.900 (6)	147
O2W—H3W⋯O1^iv	0.84	1.88	2.715 (6)	172
O2W—H4W⋯O6^v	0.84	2.05	2.788 (7)	146

Symmetry codes: (i) ; (ii) ; (iii) ; (iv) ; (v) .

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(3-hydroxy-phenyl-acetato-κO,O')bis-(1H-imidazole-κN)nickel(II).

Authors: Xiao-Yan Nie; Qian-Zhu Li
Journal: Acta Crystallogr Sect E Struct Rep Online Date: 2009-02-28

2 in total