Poly[μ3-acetato-di-μ3-isonicotinato-μ2-isonicotinato-samarium(III)silver(I)]

Zhu, L.-C.

doi:10.1107/S1600536809048430

metal-organic compounds

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ISSN: 2056-9890

Volume 65| Part 12| December 2009| Page m1616

doi:10.1107/S1600536809048430

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Poly[μ₃-acetato-di-μ₃-isonicotinato-μ₂-isonicotinato-samarium(III)silver(I)]

Li-Cai Zhu ^a ^*

^aSchool of Chemistry and Environment, South China Normal University, Guangzhou 510631, People's Republic of China
^*Correspondence e-mail: licaizhu1977@yahoo.com.cn

(Received 6 November 2009; accepted 14 November 2009; online 21 November 2009)

In the title homochiral three-dimensional heterometallic complex, [AgSm(C₆H₄NO₂)₃(C₂H₃O₂)]_n, the eight-coordinate Sm^III ion displays a bicapped trigonal-prismatic geometry, being coordinated by two O atoms from one acetate ligand, four O atoms from four bridging isonicotinate ligands and two O atoms from two terminal isonicotinate ligands. The four-coordinate Ag^I ion adopts a tetrahedral geometry, being bonded to two N atoms from two bridging isonicotinate ligands and two O atoms from two acetate ligands. These metal coordination units are connected by bridging isonicotinate and acetate ligands, generating a three-dimensional network.

Related literature

For the applications of lanthanide–transition metal heterometallic complexes with bridging multifunctional organic ligands in ion exchange, magnetism, bimetallic catalysis and as luminescent probes, see: Cheng et al. (2006 ); Gu & Xue (2006 ); Peng et al. (2008 ); Zhu et al. (2009 ).

Experimental

Crystal data

[AgSm(C₆H₄NO₂)₃(C₂H₃O₂)]
M_r = 683.58
Hexagonal, P 6₁ 22
a = 11.8184 (5) Å
c = 27.340 (2) Å
V = 3307.0 (3) Å³
Z = 6
Mo Kα radiation
μ = 3.58 mm⁻¹
T = 296 K
0.23 × 0.20 × 0.19 mm

Data collection

Bruker APEXII area-detector diffractometer
Absorption correction: multi-scan (SADABS; Sheldrick, 1996 ) T_min = 0.444, T_max = 0.507
17136 measured reflections
1992 independent reflections
1928 reflections with I > 2σ(I)
R_int = 0.046

Refinement

R[F² > 2σ(F²)] = 0.020
wR(F²) = 0.049
S = 1.06
1992 reflections
154 parameters
H-atom parameters constrained
Δρ_max = 0.65 e Å⁻³
Δρ_min = −0.45 e Å⁻³
Absolute structure: Flack (1983 ), 739 Friedel pairs
Flack parameter: 0.006 (15)

Data collection: APEX2 (Bruker, 2004 ); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 2008 ); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97.

Supporting information

Crystal structure: contains datablocks I, global. DOI: 10.1107/S1600536809048430/pv2235sup1.cif

Structure factors: contains datablock I. DOI: 10.1107/S1600536809048430/pv2235Isup2.hkl

checkCIF report

Comment top

In the past few years, lanthanide-transition metal heterometallic complexs with bridging multifunctionnal organic ligands are of increasing interest, not only because of their impressive topological structures, but also due to their versatile applications in ion exchange, magnetism, bimetallic catalysis and luminescent probe (Cheng et al., 2006; Peng et al., 2008; Zhu et al., 2009). However, because of complicated interactions among the organic moiety and two types of metal centers, the construction of a homochiral Ln—M heterometallic coordination framework is one of the most challenging issues in synthetic chemistry and materials science(Gu & Xue, 2006). As an extension of this research, the structure of the title compound, a new homochiral heterometallic coordination polymer, (I), has been determined which is presented in this article.

In the title compound (Fig. 1), there are half of Sm^III ion, half of Ag^I ion, half of acetate ligand, and one and half crystallogaphically unique isonicotinate ligands in the asymmetrical unit. Isonicotinate ligands have two types of distinctly different coordination modes: one acts as a bridging ligand to coordinate one Ag^I ion and two Sm^III ions, and the other acts as a terminal ligand to coordinate two Sm^III ions. Acetate ligand adopts chelating [Sm^III] and bridging [Ag^I] coordination modes. Each Sm^III ion is eight-coordinated by two O atoms from one acetate ligand, four O atoms from four bridging isonicotinate ligands, and two O atom from two terminal isonicotinate ligands. The Sm center can be described as having a bicapped trigonal prism coordination geometry. The four-coordinated Ag^I ion is bonded to two N atoms from two bridging isonicotinate ligand and two O atoms from two acetate ligands to furnish a tetrahedral geometry, (Table 1). These metal coordination units are connected by bridging isonicotinate and acetate ligands, generating a three-dimensional network (Fig. 2).

Related literature top

For the applications of lanthanide–transition metal heterometallic complexes with bridging multifunctional organic ligands in ion exchange, magnetism, bimetallic catalysis and as luminescent probes, see: Cheng et al. (2006); Gu & Xue (2006); Peng et al. (2008); Zhu et al. (2009).

Experimental top

A mixture of AgNO₃(0.057 g, 0.33 mmol), Sm₂O₃(0.116 g, 0.33 mmol), isonicotinic acid (0.164 g, 1.33 mmol), acetic acid (0.080 g, 1.33 mmol), and H₂O(7 ml) was sealed in a 20 ml Teflon-lined reaction vessel at 443 K for 6 days then slowly cooled to room temperature. The product was collected by filtration, washed with water and air-dried. Colorless block crystals suitable for X-ray analysis were obtained.

Computing details top

Data collection: APEX2 (Bruker, 2004); cell refinement: SAINT (Bruker, 2004); data reduction: SAINT (Bruker, 2004); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008); molecular graphics: XP in SHELXTL (Sheldrick, 2008); software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures top

	Fig. 1. The molecular structure showing the atomic-numbering scheme and displacement ellipsoids drawn at the 30% probability level. Symmetry codes: (A) x, 1 + x-y, 1/6 - z; (B) 1 + x-y, 2 - y, -z; (C) 1 + x-y, 1 - y, -z; (D) 1 + x, 1 + y, z; (E) 1 - y, 1 - x, -1/6 - z; (F) 1 + x-y, 1 + x, 1/6 + z.
	Fig. 2. A view of the three-dimensional structure of the title compound. Hydrogen atoms are omitted for clarity.

Poly[µ₃-acetato-di-µ₃-isonicotinato-µ₂-isonicotinato- samarium(III)silver(I)] top

Crystal data top

[AgSm(C₆H₄NO₂)₃(C₂H₃O₂)]	D_x = 2.059 Mg m⁻³
M_r = 683.58	Mo Kα radiation, λ = 0.71073 Å
Hexagonal, P6₁22	Cell parameters from 7353 reflections
Hall symbol: P 61 2 (0 0 -1)	θ = 2.5–27.4°
a = 11.8184 (5) Å	µ = 3.58 mm⁻¹
c = 27.340 (2) Å	T = 296 K
V = 3307.0 (3) Å³	Block, colorless
Z = 6	0.23 × 0.20 × 0.19 mm
F(000) = 1974

Data collection top

Bruker APEXII area-detector diffractometer	1992 independent reflections
Radiation source: fine-focus sealed tube	1928 reflections with I > 2σ(I)
Graphite monochromator	R_int = 0.046
ϕ and ω scan	θ_max = 25.2°, θ_min = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −13→14
T_min = 0.444, T_max = 0.507	k = −11→14
17136 measured reflections	l = −32→30

Refinement top

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)] = 0.020	H-atom parameters constrained
wR(F²) = 0.049	w = 1/[σ²(F_o²) + (0.0242P)² + 2.1731P] where P = (F_o² + 2F_c²)/3
S = 1.06	(Δ/σ)_max = 0.001
1992 reflections	Δρ_max = 0.65 e Å⁻³
154 parameters	Δρ_min = −0.45 e Å⁻³
0 restraints	Absolute structure: Flack (1983), 739 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.006 (15)

Crystal data top

[AgSm(C₆H₄NO₂)₃(C₂H₃O₂)]	Z = 6
M_r = 683.58	Mo Kα radiation
Hexagonal, P6₁22	µ = 3.58 mm⁻¹
a = 11.8184 (5) Å	T = 296 K
c = 27.340 (2) Å	0.23 × 0.20 × 0.19 mm
V = 3307.0 (3) Å³

Data collection top

Bruker APEXII area-detector diffractometer	1992 independent reflections
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	1928 reflections with I > 2σ(I)
T_min = 0.444, T_max = 0.507	R_int = 0.046
17136 measured reflections

Refinement top

R[F² > 2σ(F²)] = 0.020	H-atom parameters constrained
wR(F²) = 0.049	Δρ_max = 0.65 e Å⁻³
S = 1.06	Δρ_min = −0.45 e Å⁻³
1992 reflections	Absolute structure: Flack (1983), 739 Friedel pairs
154 parameters	Absolute structure parameter: 0.006 (15)
0 restraints

Special details top

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å²) top

	x	y	z	U_iso*/U_eq	Occ. (<1)
Sm1	0.86531 (2)	1.0000	0.0000	0.02353 (8)
Ag2	0.51785 (4)	0.75893 (2)	0.0833	0.03675 (12)
O1	0.1435 (3)	0.2764 (3)	−0.10025 (9)	0.0409 (7)
O2	−0.0057 (3)	0.1970 (3)	−0.04112 (10)	0.0401 (7)
O3	0.6346 (3)	0.9170 (3)	0.02435 (11)	0.0401 (7)
O4	1.0601 (3)	1.0664 (3)	0.04589 (11)	0.0495 (8)
C1	0.1062 (4)	0.2765 (4)	−0.05754 (14)	0.0312 (10)
C2	0.1996 (4)	0.3805 (4)	−0.02321 (13)	0.0328 (9)
C3	0.1670 (4)	0.3897 (4)	0.02451 (15)	0.0410 (12)
H4	0.0847	0.3306	0.0366	0.049*
C4	0.2570 (5)	0.4864 (5)	0.05370 (16)	0.0460 (11)
H2	0.2328	0.4914	0.0856	0.055*
C5	0.4073 (6)	0.5645 (7)	−0.0058 (2)	0.101 (3)
H3	0.4902	0.6253	−0.0169	0.121*
C6	0.3228 (6)	0.4690 (6)	−0.03802 (19)	0.083 (3)
H5	0.3500	0.4655	−0.0696	0.100*
C7	0.6215 (5)	1.0000	0.0000	0.0345 (13)
C8	0.4962 (7)	1.0000	0.0000	0.089 (3)
H11A	0.5133	1.0884	−0.0010	0.133*	0.50
H11B	0.4481	0.9581	0.0292	0.133*	0.50
H11C	0.4458	0.9535	−0.0282	0.133*	0.50
C9	1.1136 (5)	1.0568 (3)	0.0833	0.0345 (13)
C10	1.2622 (6)	1.1311 (3)	0.0833	0.0375 (13)
C11	1.3318 (5)	1.2039 (6)	0.04352 (19)	0.0576 (15)
H13	1.2889	1.2083	0.0157	0.069*
C12	1.4659 (6)	1.2700 (8)	0.0456 (3)	0.082 (2)
H14	1.5112	1.3200	0.0186	0.099*
N1	0.3766 (4)	0.5734 (4)	0.03960 (13)	0.0508 (11)
N2	1.5358 (7)	1.2679 (4)	0.0833	0.093 (3)

Atomic displacement parameters (Å²) top

	U¹¹	U²²	U³³	U¹²	U¹³	U²³
Sm1	0.02697 (12)	0.02447 (15)	0.01831 (13)	0.01224 (7)	0.00126 (6)	0.00253 (11)
Ag2	0.0309 (2)	0.0440 (2)	0.0310 (2)	0.01544 (12)	0.000	−0.00131 (18)
O1	0.0433 (18)	0.0454 (18)	0.0227 (14)	0.0137 (15)	−0.0043 (13)	−0.0073 (12)
O2	0.0395 (17)	0.0320 (16)	0.0298 (15)	0.0036 (14)	−0.0050 (13)	0.0045 (12)
O3	0.0345 (16)	0.0457 (18)	0.0413 (17)	0.0210 (14)	0.0125 (13)	0.0158 (14)
O4	0.0354 (17)	0.070 (2)	0.0403 (17)	0.0244 (15)	−0.0079 (14)	0.0031 (15)
C1	0.038 (2)	0.024 (2)	0.024 (2)	0.0092 (18)	−0.0050 (17)	0.0024 (16)
C2	0.038 (2)	0.028 (2)	0.023 (2)	0.009 (2)	−0.0038 (18)	0.0002 (17)
C3	0.040 (3)	0.033 (2)	0.031 (2)	0.004 (2)	0.0042 (18)	−0.0024 (19)
C4	0.048 (3)	0.042 (3)	0.028 (2)	0.008 (2)	0.002 (2)	−0.008 (2)
C5	0.061 (4)	0.095 (5)	0.045 (3)	−0.037 (3)	0.022 (3)	−0.033 (3)
C6	0.066 (4)	0.075 (4)	0.031 (3)	−0.023 (3)	0.017 (3)	−0.020 (3)
C7	0.031 (2)	0.046 (3)	0.031 (3)	0.0231 (17)	−0.0010 (15)	−0.002 (3)
C8	0.062 (3)	0.129 (9)	0.098 (7)	0.064 (4)	0.021 (3)	0.042 (7)
C9	0.031 (3)	0.034 (2)	0.037 (3)	0.0156 (16)	0.000	0.000 (2)
C10	0.035 (3)	0.042 (3)	0.034 (3)	0.0174 (16)	0.000	0.004 (3)
C11	0.041 (3)	0.080 (4)	0.051 (3)	0.029 (3)	0.011 (2)	0.025 (3)
C12	0.055 (4)	0.102 (6)	0.075 (4)	0.028 (4)	0.026 (3)	0.027 (4)
N1	0.042 (2)	0.046 (2)	0.033 (2)	−0.0024 (19)	−0.0019 (18)	−0.0115 (17)
N2	0.049 (4)	0.120 (6)	0.086 (6)	0.025 (2)	0.000	0.009 (5)

Geometric parameters (Å, º) top

Sm1—O2ⁱ	2.336 (3)	C3—H4	0.9300
Sm1—O2ⁱⁱ	2.336 (3)	C4—N1	1.323 (6)
Sm1—O4	2.384 (3)	C4—H2	0.9300
Sm1—O4ⁱⁱⁱ	2.384 (3)	C5—N1	1.311 (6)
Sm1—O1^iv	2.478 (3)	C5—C6	1.386 (7)
Sm1—O1^v	2.478 (3)	C5—H3	0.9300
Sm1—O3	2.483 (3)	C6—H5	0.9300
Sm1—O3ⁱⁱⁱ	2.483 (3)	C7—O3ⁱⁱⁱ	1.257 (4)
Ag2—N1	2.316 (4)	C7—C8	1.482 (9)
Ag2—N1^vi	2.316 (4)	C8—H11A	0.9600
Ag2—O3	2.328 (3)	C8—H11B	0.9600
Ag2—O3^vi	2.328 (3)	C8—H11C	0.9600
O1—C1	1.248 (5)	C9—O4^vi	1.238 (4)
O1—Sm1^vii	2.478 (3)	C9—C10	1.521 (8)
O2—C1	1.261 (5)	C10—C11	1.376 (6)
O2—Sm1^viii	2.336 (3)	C10—C11^vi	1.376 (6)
O3—C7	1.257 (4)	C11—C12	1.374 (8)
O4—C9	1.238 (4)	C11—H13	0.9300
C1—C2	1.501 (5)	C12—N2	1.329 (8)
C2—C6	1.362 (7)	C12—H14	0.9300
C2—C3	1.380 (6)	N2—C12^vi	1.329 (8)
C3—C4	1.363 (6)

O2ⁱ—Sm1—O2ⁱⁱ	162.24 (16)	C9—O4—Sm1	149.2 (3)
O2ⁱ—Sm1—O4	83.32 (11)	O1—C1—O2	124.9 (4)
O2ⁱⁱ—Sm1—O4	82.47 (11)	O1—C1—C2	118.0 (4)
O2ⁱ—Sm1—O4ⁱⁱⁱ	82.47 (11)	O2—C1—C2	117.1 (3)
O2ⁱⁱ—Sm1—O4ⁱⁱⁱ	83.32 (11)	C6—C2—C3	117.0 (4)
O4—Sm1—O4ⁱⁱⁱ	73.52 (16)	C6—C2—C1	120.6 (4)
O2ⁱ—Sm1—O1^iv	102.15 (10)	C3—C2—C1	122.4 (4)
O2ⁱⁱ—Sm1—O1^iv	83.83 (10)	C4—C3—C2	119.2 (4)
O4—Sm1—O1^iv	145.28 (11)	C4—C3—H4	120.4
O4ⁱⁱⁱ—Sm1—O1^iv	73.30 (11)	C2—C3—H4	120.4
O2ⁱ—Sm1—O1^v	83.83 (10)	N1—C4—C3	124.3 (4)
O2ⁱⁱ—Sm1—O1^v	102.15 (10)	N1—C4—H2	117.9
O4—Sm1—O1^v	73.30 (11)	C3—C4—H2	117.9
O4ⁱⁱⁱ—Sm1—O1^v	145.28 (11)	N1—C5—C6	123.5 (5)
O1^iv—Sm1—O1^v	141.02 (16)	N1—C5—H3	118.3
O2ⁱ—Sm1—O3	124.27 (10)	C6—C5—H3	118.3
O2ⁱⁱ—Sm1—O3	73.44 (10)	C2—C6—C5	119.6 (5)
O4—Sm1—O3	132.68 (10)	C2—C6—H5	120.2
O4ⁱⁱⁱ—Sm1—O3	139.93 (12)	C5—C6—H5	120.2
O1^iv—Sm1—O3	72.14 (10)	O3ⁱⁱⁱ—C7—O3	118.3 (5)
O1^v—Sm1—O3	72.89 (11)	O3ⁱⁱⁱ—C7—C8	120.9 (3)
O2ⁱ—Sm1—O3ⁱⁱⁱ	73.44 (10)	O3—C7—C8	120.9 (3)
O2ⁱⁱ—Sm1—O3ⁱⁱⁱ	124.27 (10)	O3ⁱⁱⁱ—C7—Sm1	59.1 (3)
O4—Sm1—O3ⁱⁱⁱ	139.93 (12)	O3—C7—Sm1	59.1 (3)
O4ⁱⁱⁱ—Sm1—O3ⁱⁱⁱ	132.68 (10)	C8—C7—Sm1	180.000 (1)
O1^iv—Sm1—O3ⁱⁱⁱ	72.89 (11)	C7—C8—H11A	109.5
O1^v—Sm1—O3ⁱⁱⁱ	72.14 (10)	C7—C8—H11B	109.5
O3—Sm1—O3ⁱⁱⁱ	51.51 (13)	H11A—C8—H11B	109.5
O2ⁱ—Sm1—C7	98.88 (8)	C7—C8—H11C	109.5
O2ⁱⁱ—Sm1—C7	98.88 (8)	H11A—C8—H11C	109.5
O4—Sm1—C7	143.24 (8)	H11B—C8—H11C	109.5
O4ⁱⁱⁱ—Sm1—C7	143.24 (8)	O4—C9—O4^vi	127.5 (6)
O1^iv—Sm1—C7	70.51 (8)	O4—C9—C10	116.3 (3)
O1^v—Sm1—C7	70.51 (8)	O4^vi—C9—C10	116.3 (3)
O3—Sm1—C7	25.76 (7)	C11—C10—C11^vi	117.6 (6)
O3ⁱⁱⁱ—Sm1—C7	25.76 (7)	C11—C10—C9	121.2 (3)
N1—Ag2—N1^vi	102.7 (2)	C11^vi—C10—C9	121.2 (3)
N1—Ag2—O3	105.05 (13)	C10—C11—C12	118.8 (5)
N1^vi—Ag2—O3	112.42 (14)	C10—C11—H13	120.6
N1—Ag2—O3^vi	112.42 (14)	C12—C11—H13	120.6
N1^vi—Ag2—O3^vi	105.05 (13)	N2—C12—C11	125.0 (6)
O3—Ag2—O3^vi	118.21 (15)	N2—C12—H14	117.5
C1—O1—Sm1^vii	124.3 (3)	C11—C12—H14	117.5
C1—O2—Sm1^viii	146.4 (3)	C5—N1—C4	116.4 (4)
C7—O3—Ag2	137.6 (3)	C5—N1—Ag2	117.8 (3)
C7—O3—Sm1	95.1 (3)	C4—N1—Ag2	124.7 (3)
Ag2—O3—Sm1	126.58 (12)	C12—N2—C12^vi	114.9 (7)

Symmetry codes: (i) x+1, y+1, z; (ii) x−y+1, −y+1, −z; (iii) x−y+1, −y+2, −z; (iv) −y+1, −x+1, −z−1/6; (v) x−y+1, x+1, z+1/6; (vi) x, x−y+1, −z+1/6; (vii) y−1, −x+y, z−1/6; (viii) x−1, y−1, z.

Experimental details

Crystal data
Chemical formula	[AgSm(C₆H₄NO₂)₃(C₂H₃O₂)]
M_r	683.58
Crystal system, space group	Hexagonal, P6₁22
Temperature (K)	296
a, c (Å)	11.8184 (5), 27.340 (2)
V (Å³)	3307.0 (3)
Z	6
Radiation type	Mo Kα
µ (mm⁻¹)	3.58
Crystal size (mm)	0.23 × 0.20 × 0.19

Data collection
Diffractometer	Bruker APEXII area-detector diffractometer
Absorption correction	Multi-scan (SADABS; Sheldrick, 1996)
T_min, T_max	0.444, 0.507
No. of measured, independent and observed [I > 2σ(I)] reflections	17136, 1992, 1928
R_int	0.046
(sin θ/λ)_max (Å⁻¹)	0.599

Refinement
R[F² > 2σ(F²)], wR(F²), S	0.020, 0.049, 1.06
No. of reflections	1992
No. of parameters	154
H-atom treatment	H-atom parameters constrained
Δρ_max, Δρ_min (e Å⁻³)	0.65, −0.45
Absolute structure	Flack (1983), 739 Friedel pairs
Absolute structure parameter	0.006 (15)

Computer programs: APEX2 (Bruker, 2004), SAINT (Bruker, 2004), SHELXS97 (Sheldrick, 2008), SHELXL97 (Sheldrick, 2008), XP in SHELXTL (Sheldrick, 2008).

Acknowledgements

The author acknowledges South China Normal University for supporting this work.

References

Bruker (2004). APEX2 and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Google Scholar
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