Literature DB >> 22090910

Poly[(μ-2-acet-oxy-benzoato)(2-acet-oxy-benzoato)-μ-aqua-mercury(II)].

Abstract

In the title compound, [Hg(C(9)H(7)O(4))(2)(H(2)O)](n), the Hg(II) ion is five-coordinated by three acetylsalicylate anions and water leading to the formation of a coordination polymer extending parallel to (001). O-H⋯O and C-H⋯O hydrogen bonds are effective in the stabilization of the crystal structure.

Entities: Chemical Disease Species

Year: 2011 PMID： 22090910 PMCID： PMC3212253 DOI： 10.1107/S1600536811029278

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

Related literature

For general background to metal complexes with acetylsalicylate as a ligand, see: Manojlović-Muir (1973 ▶); Garcia et al. (2003 ▶); Greenaway et al. (1984 ▶); Fujimori et al. (2005 ▶); James et al. (1998 ▶); Vasquez-Arciga et al. (2004) ▶; Ma & Moulton (2007 ▶).

Experimental

Crystal data

[Hg(C9H7O4)2(H2O)] M = 1153.80 Triclinic, a = 6.1851 (9) Å b = 10.1359 (17) Å c = 15.453 (2) Å α = 100.308 (7)° β = 98.700 (8)° γ = 100.667 (7)° V = 919.5 (2) Å3 Z = 1 Mo Kα radiation μ = 8.42 mm−1 T = 120 K 0.21 × 0.17 × 0.02 mm

Data collection

Bruker Kappa APEXII diffractometer Absorption correction: analytical (De Meulenaer & Tompa, 1965 ▶) T min = 0.24, T max = 0.83 9510 measured reflections 5293 independent reflections 4404 reflections with I > 2σ(I) R int = 0.037

Refinement

R[F 2 > 2σ(F 2)] = 0.040 wR(F 2) = 0.092 S = 0.97 5293 reflections 253 parameters H-atom parameters constrained Δρmax = 1.88 e Å−3 Δρmin = −2.19 e Å−3 Data collection: APEX2 (Bruker, 2006 ▶); cell refinement: SAINT (Bruker, 2006 ▶); data reduction: SAINT; program(s) used to solve structure: SIR92 (Altomare et al., 1994 ▶); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003 ▶); molecular graphics: Mercury (Macrae et al., 2006 ▶); software used to prepare material for publication: CRYSTALS. Crystal structure: contains datablock(s) global, I. DOI: 10.1107/S1600536811029278/dn2701sup1.cif Structure factors: contains datablock(s) I. DOI: 10.1107/S1600536811029278/dn2701Isup2.hkl Additional supplementary materials: crystallographic information; 3D view; checkCIF report

[Hg(C₉H₇O₄)₂(H₂O)]	Z = 1
M_r = 1153.80	F(000) = 552
Triclinic, P1	D_x = 2.084 Mg m⁻³
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 6.1851 (9) Å	Cell parameters from 3872 reflections
b = 10.1359 (17) Å	θ = 3–30°
c = 15.453 (2) Å	µ = 8.42 mm⁻¹
α = 100.308 (7)°	T = 120 K
β = 98.700 (8)°	Plate, colorless
γ = 100.667 (7)°	0.21 × 0.17 × 0.02 mm
V = 919.5 (2) Å³

Bruker Kappa APEXII diffractometer	4404 reflections with I > 2σ(I)
graphite	R_int = 0.037
φ & ω scans	θ_max = 30.0°, θ_min = 2.2°
Absorption correction: analytical (De Meulenaer & Tompa, 1965)	h = −8→7
T_min = 0.24, T_max = 0.83	k = −14→13
9510 measured reflections	l = −21→21
5293 independent reflections

Refinement on F²	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F² > 2σ(F²)] = 0.040	H-atom parameters constrained
wR(F²) = 0.092	Method = Modified Sheldrick w = 1/[σ²(F²) + (0.04P)² + 6.15P], where P = [max(F_o²,0) + 2F_c²]/3
S = 0.97	(Δ/σ)_max = 0.001
5293 reflections	Δρ_max = 1.88 e Å⁻³
253 parameters	Δρ_min = −2.19 e Å⁻³
0 restraints

	x	y	z	U_iso*/U_eq
Hg1	0.89515 (4)	0.65817 (2)	0.467447 (16)	0.0168
O1	0.8495 (8)	0.5346 (4)	0.3440 (3)	0.0248
O2	0.4800 (8)	0.5246 (5)	0.3271 (3)	0.0285
O3	0.2895 (7)	0.4772 (4)	0.1441 (3)	0.0215
O4	0.5203 (8)	0.6855 (4)	0.1796 (4)	0.0281
O5	0.6204 (8)	0.7673 (5)	0.5843 (3)	0.0270
O6	0.9879 (7)	0.7872 (4)	0.5911 (3)	0.0222
O7	1.2498 (7)	1.0048 (4)	0.7117 (3)	0.0174
O8	1.0778 (8)	1.1274 (5)	0.6272 (3)	0.0268
O9	1.2672 (7)	0.5721 (4)	0.4763 (3)	0.0198
C1	0.6439 (11)	0.4964 (6)	0.2984 (4)	0.0198
C2	0.6323 (10)	0.4156 (6)	0.2068 (4)	0.0165
C3	0.7982 (11)	0.3423 (6)	0.1913 (4)	0.0205
C4	0.7977 (11)	0.2696 (6)	0.1066 (5)	0.0231
C5	0.6320 (11)	0.2710 (6)	0.0339 (5)	0.0249
C6	0.4648 (11)	0.3435 (6)	0.0472 (4)	0.0216
C7	0.4668 (10)	0.4133 (6)	0.1336 (4)	0.0178
C8	0.3385 (11)	0.6172 (6)	0.1734 (4)	0.0207
C9	0.1367 (13)	0.6643 (7)	0.1952 (6)	0.0365
C10	0.8163 (11)	0.8122 (6)	0.6245 (4)	0.0195
C11	0.8677 (10)	0.8985 (5)	0.7175 (4)	0.0171
C12	0.7009 (11)	0.8886 (6)	0.7696 (5)	0.0223
C13	0.7399 (12)	0.9606 (6)	0.8567 (4)	0.0238
C14	0.9507 (11)	1.0455 (6)	0.8963 (4)	0.0227
C15	1.1151 (11)	1.0597 (6)	0.8456 (4)	0.0204
C16	1.0744 (10)	0.9876 (6)	0.7573 (4)	0.0174
C17	1.2367 (11)	1.0780 (6)	0.6470 (4)	0.0224
C18	1.4387 (13)	1.0861 (8)	0.6063 (5)	0.0333
H31	0.9129	0.3424	0.2398	0.0255*
H41	0.9097	0.2185	0.0975	0.0281*
H51	0.6341	0.2225	−0.0244	0.0287*
H61	0.3524	0.3452	−0.0016	0.0251*
H91	0.1725	0.7613	0.2154	0.0468*
H92	0.0862	0.6224	0.2410	0.0468*
H93	0.0218	0.6394	0.1432	0.0468*
H121	0.5576	0.8309	0.7441	0.0281*
H131	0.6235	0.9526	0.8904	0.0321*
H141	0.9795	1.0926	0.9572	0.0282*
H151	1.2569	1.1192	0.8710	0.0242*
H181	1.4269	1.1379	0.5610	0.0441*
H182	1.5677	1.1294	0.6511	0.0441*
H183	1.4512	0.9960	0.5807	0.0441*
H2	1.3284	0.5582	0.4330	0.0237*
H1	1.3720	0.6302	0.5086	0.0237*

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Hg1	0.01839 (11)	0.01710 (10)	0.01515 (12)	0.00792 (7)	0.00211 (8)	0.00097 (7)
O1	0.028 (2)	0.025 (2)	0.021 (2)	0.0116 (18)	0.0052 (19)	−0.0016 (18)
O2	0.027 (3)	0.042 (3)	0.022 (2)	0.018 (2)	0.007 (2)	0.005 (2)
O3	0.015 (2)	0.022 (2)	0.028 (3)	0.0090 (16)	0.0011 (18)	0.0050 (18)
O4	0.026 (2)	0.021 (2)	0.040 (3)	0.0077 (18)	0.012 (2)	0.009 (2)
O5	0.024 (2)	0.029 (2)	0.026 (3)	0.0072 (18)	−0.002 (2)	0.0028 (19)
O6	0.022 (2)	0.025 (2)	0.017 (2)	0.0076 (17)	0.0018 (18)	−0.0020 (17)
O7	0.020 (2)	0.0172 (18)	0.019 (2)	0.0097 (15)	0.0057 (17)	0.0068 (16)
O8	0.032 (3)	0.029 (2)	0.027 (3)	0.0148 (19)	0.008 (2)	0.015 (2)
O9	0.021 (2)	0.023 (2)	0.014 (2)	0.0036 (16)	0.0030 (17)	0.0014 (16)
C1	0.025 (3)	0.020 (3)	0.017 (3)	0.007 (2)	0.005 (2)	0.008 (2)
C2	0.014 (3)	0.019 (3)	0.018 (3)	0.005 (2)	0.002 (2)	0.006 (2)
C3	0.026 (3)	0.020 (3)	0.018 (3)	0.009 (2)	0.004 (3)	0.007 (2)
C4	0.024 (3)	0.020 (3)	0.026 (4)	0.008 (2)	0.009 (3)	0.002 (2)
C5	0.029 (3)	0.024 (3)	0.020 (3)	0.004 (2)	0.005 (3)	−0.001 (2)
C6	0.022 (3)	0.022 (3)	0.019 (3)	0.005 (2)	−0.001 (2)	0.003 (2)
C7	0.016 (3)	0.015 (2)	0.022 (3)	0.003 (2)	0.002 (2)	0.004 (2)
C8	0.025 (3)	0.019 (3)	0.022 (3)	0.009 (2)	0.006 (3)	0.012 (2)
C9	0.031 (4)	0.029 (3)	0.056 (5)	0.015 (3)	0.013 (4)	0.016 (3)
C10	0.025 (3)	0.015 (2)	0.021 (3)	0.008 (2)	0.005 (2)	0.005 (2)
C11	0.017 (3)	0.012 (2)	0.021 (3)	0.006 (2)	−0.001 (2)	0.001 (2)
C12	0.021 (3)	0.022 (3)	0.027 (4)	0.006 (2)	0.008 (3)	0.009 (3)
C13	0.034 (4)	0.026 (3)	0.020 (3)	0.015 (3)	0.014 (3)	0.013 (3)
C14	0.032 (4)	0.023 (3)	0.016 (3)	0.013 (3)	0.003 (3)	0.004 (2)
C15	0.024 (3)	0.016 (2)	0.021 (3)	0.005 (2)	0.002 (2)	0.003 (2)
C16	0.019 (3)	0.018 (2)	0.019 (3)	0.011 (2)	0.003 (2)	0.005 (2)
C17	0.028 (3)	0.018 (3)	0.023 (3)	0.007 (2)	0.003 (3)	0.007 (2)
C18	0.036 (4)	0.041 (4)	0.034 (4)	0.013 (3)	0.019 (3)	0.020 (3)

Hg1—O9ⁱ	2.708 (4)	C5—C6	1.394 (9)
Hg1—O8ⁱⁱ	2.823 (4)	C5—H51	0.950
Hg1—O1	2.034 (4)	C6—C7	1.393 (9)
Hg1—O6	2.046 (4)	C6—H61	0.950
Hg1—O9	2.601 (4)	C8—C9	1.479 (10)
O1—C1	1.309 (8)	C9—H91	0.950
O2—C1	1.226 (8)	C9—H92	0.950
O3—C7	1.388 (7)	C9—H93	0.950
O3—C8	1.372 (7)	C10—C11	1.497 (8)
O4—C8	1.187 (8)	C11—C12	1.402 (9)
O5—C10	1.236 (8)	C11—C16	1.401 (8)
O6—C10	1.295 (7)	C12—C13	1.373 (9)
O7—C16	1.382 (7)	C12—H121	0.950
O7—C17	1.348 (8)	C13—C14	1.403 (9)
O8—C17	1.207 (8)	C13—H131	0.950
O9—H2	0.820	C14—C15	1.377 (9)
O9—H1	0.820	C14—H141	0.950
C1—C2	1.488 (9)	C15—C16	1.389 (9)
C2—C3	1.398 (8)	C15—H151	0.950
C2—C7	1.400 (8)	C17—C18	1.477 (10)
C3—C4	1.382 (9)	C18—H181	0.950
C3—H31	0.950	C18—H182	0.950
C4—C5	1.406 (10)	C18—H183	0.950
C4—H41	0.950

O9—Hg1—O8	107.12 (11)	O4—C8—O3	121.8 (5)
O9—Hg1—O6	94.68 (16)	O4—C8—C9	127.9 (5)
O1—Hg1—O6	171.97 (18)	O3—C8—C9	110.3 (5)
O1—Hg1—O9	78.28 (14)	O5—C10—C11	121.1 (5)
C1—O1—Hg1	116.6 (3)	O6—C10—C11	116.1 (5)
C8—O3—C7	118.1 (4)	C12—C11—C16	117.2 (5)
C17—O7—C16	117.7 (4)	C12—C11—C10	118.4 (5)
O2—C1—O1	124.4 (5)	C16—C11—C10	124.4 (5)
O2—C1—C2	123.5 (5)	C13—C12—C11	121.9 (5)
O1—C1—C2	112.1 (5)	C12—C13—C14	120.1 (5)
C3—C2—C7	117.5 (5)	C15—C14—C13	118.9 (5)
C3—C2—C1	119.1 (5)	C16—C15—C14	120.2 (5)
C7—C2—C1	123.4 (5)	C15—C16—O7	116.4 (5)
C4—C3—C2	121.0 (5)	C15—C16—C11	121.6 (5)
C5—C4—C3	120.1 (5)	O7—C16—C11	122.0 (5)
C4—C5—C6	120.4 (5)	O8—C17—O7	123.1 (5)
C7—C6—C5	118.6 (5)	O8—C17—C18	126.5 (6)
C6—C7—O3	116.2 (5)	O7—C17—C18	110.4 (5)
C6—C7—C2	122.4 (5)	H181—C18—H183	110.00
O3—C7—C2	121.3 (5)	H182—C18—H183	109.00

O9—Hg1—O1—C1	163.5 (4)	C7—O3—C8—O4	9.0 (8)
O9—Hg1—O6—C10	−156.3 (3)	C7—O3—C8—C9	−170.8 (5)
Hg1—O1—C1—O2	−3.7 (7)	Hg1—O6—C10—O5	−3.0 (6)
Hg1—O1—C1—C2	175.2 (3)	Hg1—O6—C10—C11	176.3 (3)
O2—C1—C2—C3	−154.5 (5)	O5—C10—C11—C12	22.0 (8)
O1—C1—C2—C3	26.5 (7)	O6—C10—C11—C12	−157.4 (5)
O2—C1—C2—C7	27.9 (8)	O5—C10—C11—C16	−159.3 (5)
O1—C1—C2—C7	−151.1 (5)	O6—C10—C11—C16	21.3 (7)
C7—C2—C3—C4	−0.3 (8)	C16—C11—C12—C13	−1.9 (8)
C1—C2—C3—C4	−178.0 (5)	C10—C11—C12—C13	176.9 (5)
C2—C3—C4—C5	1.1 (8)	C11—C12—C13—C14	−0.3 (8)
C3—C4—C5—C6	−0.6 (8)	C12—C13—C14—C15	2.8 (8)
C4—C5—C6—C7	−0.5 (8)	C14—C15—C16—O7	−177.9 (5)
C5—C6—C7—O3	−176.4 (4)	C17—O7—C16—C15	−108.1 (5)
C5—C6—C7—C2	1.3 (8)	C17—O7—C16—C11	73.3 (6)
C8—O3—C7—C6	−118.6 (5)	C12—C11—C16—C15	1.8 (7)
C8—O3—C7—C2	63.6 (7)	C10—C11—C16—C15	−177.0 (5)
C3—C2—C7—C6	−0.9 (8)	C12—C11—C16—O7	−179.7 (4)
C1—C2—C7—C6	176.7 (5)	C10—C11—C16—O7	1.5 (7)
C3—C2—C7—O3	176.7 (4)	C16—O7—C17—O8	−0.4 (7)
C1—C2—C7—O3	−5.7 (8)	C16—O7—C17—C18	180.0 (4)

D—H···A	D—H	H···A	D···A	D—H···A
O9—H2···O2ⁱⁱⁱ	0.82	2.01	2.835 (7)	180.(1)
O9—H1···O5ⁱⁱⁱ	0.82	1.93	2.758 (5)	179.(1)
C9—H92···O1^iv	0.95	2.49	3.409 (9)	163
C15—H151···O4ⁱⁱ	0.95	2.51	3.221 (8)	132
C18—H181···O5ⁱⁱ	0.95	2.59	3.530 (9)	169

Table 1

Hydrogen-bond geometry (Å, °)

D—H⋯A	D—H	H⋯A	D⋯A	D—H⋯A
O9—H2⋯O2ⁱ	0.82	2.01	2.835 (7)	180 (1)
O9—H1⋯O5ⁱ	0.82	1.93	2.758 (5)	179 (1)
C9—H92⋯O1ⁱⁱ	0.95	2.49	3.409 (9)	163
C15—H151⋯O4ⁱⁱⁱ	0.95	2.51	3.221 (8)	132
C18—H181⋯O5ⁱⁱⁱ	0.95	2.59	3.530 (9)	169

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

1 in total

1. Orally active antioxidative copper(II) aspirinate: synthesis, structure characterization, superoxide scavenging activity, and in vitro and in vivo antioxidative evaluations.

Authors: T Fujimori; S Yamada; H Yasui; H Sakurai; Y In; T Ishida
Journal: J Biol Inorg Chem Date: 2005-10-28 Impact factor: 3.358

1 in total